#------------------------------------------------------------------------------ #$Date: 2021-06-03 22:11:15 +0300 (Thu, 03 Jun 2021) $ #$Revision: 265723 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/87/4518763.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4518763 loop_ _publ_author_name 'Britton, Luke' 'Skrodzki, Maciej' 'Nichol, Gary S.' 'Dominey, Andrew P.' 'Pawlu\'c, Piotr' 'Docherty, Jamie H.' 'Thomas, Stephen P.' _publ_section_title ; Manganese-Catalyzed C(sp2)--H Borylation of Furan and Thiophene Derivatives ; _journal_name_full 'ACS Catalysis' _journal_page_first 6857 _journal_page_last 6864 _journal_paper_doi 10.1021/acscatal.1c01563 _journal_year 2021 _chemical_formula_moiety 'C22 H42 B Mn N2 P4' _chemical_formula_sum 'C22 H42 B Mn N2 P4' _chemical_formula_weight 524.20 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2020-10-07 _audit_creation_method ; Olex2 1.3-beta (compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145) ; _cell_angle_alpha 67.787(2) _cell_angle_beta 86.307(2) _cell_angle_gamma 71.524(2) _cell_formula_units_Z 2 _cell_length_a 10.4506(3) _cell_length_b 11.3275(3) _cell_length_c 13.0799(4) _cell_measurement_reflns_used 13392 _cell_measurement_temperature 250.00(10) _cell_measurement_theta_max 75.6410 _cell_measurement_theta_min 4.4270 _cell_volume 1356.88(7) _computing_cell_refinement 'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 1.3-beta (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3-beta (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 250.0 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.1574 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -100.00 -15.00 1.00 5.00 -- -41.79 143.00-141.00 85 2 \w -88.00 -7.00 1.00 5.00 -- -41.79 127.00 48.00 81 3 \w -112.00 -65.00 1.00 5.00 -- -41.79-143.00 163.00 47 4 \w 29.00 98.00 1.00 5.00 -- 41.79-127.00 -26.00 69 5 \w 36.00 108.00 1.00 5.00 -- 41.79-143.00 163.00 72 6 \w 41.00 126.00 1.00 10.00 -- 111.00-143.00 163.00 85 7 \w 96.00 178.00 1.00 10.00 -- 111.00 127.00 48.00 82 8 \w 40.00 114.00 1.00 10.00 -- 111.00-127.00 -26.00 74 9 \w 87.00 171.00 1.00 10.00 -- 111.00 143.00-141.00 84 10 \w 3.00 30.00 1.00 5.00 -- 38.00 88.00-150.41 27 11 \w -114.00 -19.00 1.00 5.00 -- -41.79 -38.00 -90.00 95 12 \w -112.00 -15.00 1.00 5.00 -- -41.79 -57.00 30.00 97 13 \w -114.00 -19.00 1.00 5.00 -- -41.79 -38.00 150.00 95 14 \w 10.00 42.00 1.00 5.00 -- 41.79 79.00 -1.76 32 15 \w 10.00 42.00 1.00 5.00 -- 42.00 80.00 59.65 32 16 \w 13.00 42.00 1.00 5.00 -- 46.00 82.00-173.31 29 17 \w 14.00 42.00 1.00 5.00 -- 46.00 79.00 130.62 28 18 \w 14.00 42.00 1.00 5.00 -- 46.00 78.00 -64.78 28 19 \w 19.00 123.00 1.00 5.00 -- 50.00 74.00 -7.23 104 20 \w 27.00 131.00 1.00 5.00 -- 58.00 74.00-103.94 104 21 \w 28.00 130.00 1.00 5.00 -- 58.00 73.00 38.36 102 22 \w 27.00 131.00 1.00 5.00 -- 58.00 74.00 128.93 104 23 \w 31.00 135.00 1.00 5.00 -- 62.00 74.00 167.55 104 24 \w 32.00 134.00 1.00 5.00 -- 62.00 71.00 96.62 102 25 \w 32.00 134.00 1.00 5.00 -- 62.00 73.00-151.88 102 26 \w 36.00 138.00 1.00 5.00 -- 66.00 73.00 55.21 102 27 \w 36.00 138.00 1.00 5.00 -- 66.00 73.00 9.88 102 28 \w 41.00 141.00 1.00 5.00 -- 70.00 69.00 -31.33 100 29 \w 44.00 146.00 1.00 5.00 -- 74.00 72.00 132.47 102 30 \w 45.00 145.00 1.00 5.00 -- 74.00 66.00 -57.12 100 31 \w 47.00 151.00 1.00 10.00 -- 78.00 74.00-137.10 104 32 \w 52.00 154.00 1.00 10.00 -- 82.00 70.00 -28.57 102 33 \w 53.00 153.00 1.00 10.00 -- 82.00 68.00 76.20 100 34 \w 52.00 154.00 1.00 10.00 -- 82.00 71.00-100.33 102 35 \w 52.00 154.00 1.00 10.00 -- 82.00 71.00 100.20 102 36 \w 55.00 152.00 1.00 10.00 -- 82.00 59.00 63.88 97 37 \w 53.00 153.00 1.00 10.00 -- 82.00 66.00-170.32 100 38 \w 57.00 157.00 1.00 10.00 -- 86.00 68.00 140.27 100 39 \w 57.00 157.00 1.00 10.00 -- 86.00 69.00 -2.85 100 40 \w 61.00 161.00 1.00 10.00 -- 90.00 68.00 -77.43 100 41 \w 66.00 164.00 1.00 10.00 -- 94.00 61.00 161.67 98 42 \w 76.00 178.00 1.00 10.00 -- 106.00 72.00 119.52 102 43 \w 39.00 112.00 1.00 10.00 -- 111.00-125.00 -60.00 73 44 \w 30.00 107.00 1.00 10.00 -- 111.00 -94.00-120.00 77 45 \w 83.00 178.00 1.00 10.00 -- 111.00 61.00-120.00 95 46 \w 40.00 135.00 1.00 10.00 -- 111.00 -45.00 60.00 95 47 \w 85.00 178.00 1.00 10.00 -- 111.00 54.00-150.48 93 48 \w 83.00 178.00 1.00 10.00 -- 111.00 61.00 60.00 95 49 \w 83.00 178.00 1.00 10.00 -- 111.00 64.00 18.14 95 50 \w 83.00 178.00 1.00 10.00 -- 111.00 61.00 0.00 95 51 \w 80.00 178.00 1.00 10.00 -- 111.00 74.00 -61.83 98 52 \w 39.00 112.00 1.00 10.00 -- 111.00-125.00 90.00 73 53 \w 83.00 178.00 1.00 10.00 -- 111.00 61.00 -90.00 95 54 \w 81.00 178.00 1.00 10.00 -- 111.00 70.00 -25.25 97 55 \w 83.00 178.00 1.00 10.00 -- 111.00 61.00 120.00 95 56 \w 81.00 178.00 1.00 10.00 -- 111.00 72.00-152.69 97 57 \w 41.00 139.00 1.00 10.00 -- 111.00 -61.00 -30.00 98 58 \w 39.00 112.00 1.00 10.00 -- 111.00-125.00-180.00 73 59 \w 83.00 178.00 1.00 10.00 -- 111.00 61.00-180.00 95 60 \w 83.00 178.00 1.00 10.00 -- 111.00 61.00 -60.00 95 61 \w 83.00 178.00 1.00 10.00 -- 111.00 61.00 -30.00 95 62 \w 83.00 178.00 1.00 10.00 -- 111.00 61.00-150.00 95 63 \w 83.00 164.00 1.00 10.00 -- 111.00 61.00 90.00 81 64 \w 72.00 110.00 1.00 10.00 -- 111.00-125.00 30.00 38 65 \w 70.00 112.00 1.00 10.00 -- 111.00-125.00-150.00 42 66 \w 53.00 107.00 1.00 10.00 -- 111.00 -94.00-150.00 54 67 \w 87.00 132.00 1.00 10.00 -- 111.00 45.00 60.00 45 68 \w 41.00 97.00 1.00 10.00 -- 111.00-125.00 0.00 56 69 \w 83.00 178.00 1.00 10.00 -- 111.00 61.00 150.00 95 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Rigaku Oxford Diffraction SuperNova' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0204471000 _diffrn_orient_matrix_UB_12 -0.0853865000 _diffrn_orient_matrix_UB_13 0.1250200000 _diffrn_orient_matrix_UB_21 -0.0957419000 _diffrn_orient_matrix_UB_22 0.1205077000 _diffrn_orient_matrix_UB_23 0.0236196000 _diffrn_orient_matrix_UB_31 -0.1211144000 _diffrn_orient_matrix_UB_32 -0.0466168000 _diffrn_orient_matrix_UB_33 -0.0079058000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.1246 _diffrn_reflns_av_unetI/netI 0.0226 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 40247 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.076 _diffrn_reflns_theta_min 3.657 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 6.266 _exptl_absorpt_correction_T_max 0.56016 _exptl_absorpt_correction_T_min 0.52164 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019) Spherical absorption correction using equivalent radius and absorption coefficient. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.283 _exptl_crystal_description plate _exptl_crystal_F_000 556 _exptl_crystal_recrystallization_method 'The material was recrystallised from a mixture of d-benzene and hexane by slow evaporation' _exptl_crystal_size_max 0.253 _exptl_crystal_size_mid 0.186 _exptl_crystal_size_min 0.046 _refine_diff_density_max 0.599 _refine_diff_density_min -0.469 _refine_diff_density_rms 0.072 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 296 _refine_ls_number_reflns 9758 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.033 _refine_ls_R_factor_all 0.0655 _refine_ls_R_factor_gt 0.0576 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1064P)^2^+0.3340P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1495 _refine_ls_wR_factor_ref 0.1549 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8298 _reflns_number_total 9758 _reflns_threshold_expression 'I > 2\s(I)' _twin_special_details ; Component 2 rotated by 179.8958\% around [0.00 -0.00 1.00] (reciprocal) or [0.07 -0.42 0.91] (direct) ; _cod_data_source_file cs1c01563_si_002.cif _cod_data_source_block se20013 _cod_database_code 4518763 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula C22H42BMnN2P4 _chemical_oxdiff_usercomment '@ 120 K LAB145' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.761 _shelx_estimated_absorpt_t_min 0.300 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.4830(12) 0.5170(12) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 3. Restrained distances N2-H2 = N1-H1 0.84 with sigma of 0.02 4.a Secondary CH2 refined with riding coordinates: C11(H11A,H11B), C12(H12A,H12B), C17(H17A,H17B), C18(H18A,H18B) 4.b Aromatic/amide H refined with riding coordinates: C00K(H00K), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10) 4.c Idealised Me refined as rotating group: C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B, H16C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A, H22B,H22C) ; _shelx_res_file ; TITL se20013_a.res in P-1 se20013.res created by SHELXL-2018/3 at 10:01:34 on 07-Oct-2020 REM Old TITL SE200013_twin_refinalized_twin1_hklf4 in P-1 REM SHELXT solution in P-1: R1 0.134, Rweak 0.019, Alpha 0.065 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C22 N3 P4 Mn CELL 1.54184 10.4506 11.3275 13.0799 67.787 86.307 71.524 ZERR 2 0.0003 0.0003 0.0004 0.002 0.002 0.002 LATT 1 SFAC C H B N P Mn UNIT 44 84 2 4 8 2 DFIX 0.84 N2 H2 N1 H1 L.S. 16 PLAN 5 SIZE 0.046 0.186 0.253 TEMP -23.15 CONF FREE Mn1 B1 BOND list 4 fmap 2 53 MORE -1 BOND $H ACTA REM REM REM WGHT 0.106400 0.334000 BASF 0.51700 FVAR 6.57950 MN1 6 0.715814 0.640311 0.679522 11.00000 0.03050 0.03275 = 0.03187 -0.01188 0.00330 -0.00780 P1 5 0.658769 0.724191 0.810162 11.00000 0.04256 0.04357 = 0.04143 -0.02093 0.00451 -0.00768 P2 5 0.490860 0.694032 0.653080 11.00000 0.03231 0.04730 = 0.04231 -0.01410 0.00378 -0.01006 P3 5 0.739682 0.424787 0.770127 11.00000 0.04021 0.03581 = 0.04559 -0.01116 0.00396 -0.01067 P4 5 0.937794 0.572083 0.727447 11.00000 0.03341 0.04282 = 0.04546 -0.01977 0.00076 -0.00939 N1 4 0.850338 0.798827 0.466290 11.00000 0.03996 0.05171 = 0.04557 -0.01478 0.00240 -0.02068 H1 2 0.901620 0.809478 0.505719 11.00000 0.04087 N2 4 0.652906 0.763774 0.416795 11.00000 0.03912 0.05729 = 0.03965 -0.01286 0.00608 -0.02580 H2 2 0.597248 0.724287 0.431877 11.00000 0.03114 C00K 1 0.960514 0.937093 0.323836 11.00000 0.05487 0.04988 = 0.07499 -0.02517 0.01930 -0.02691 AFIX 43 H00K 2 1.016947 0.936545 0.377258 11.00000 -1.20000 AFIX 0 C2 1 0.865085 0.871607 0.356713 11.00000 0.04266 0.03716 = 0.05256 -0.01798 0.01430 -0.00947 C3 1 0.777292 0.876719 0.274407 11.00000 0.04360 0.03069 = 0.04243 -0.01231 0.00811 -0.00337 C4 1 0.673520 0.818481 0.306371 11.00000 0.04422 0.03703 = 0.03732 -0.01315 -0.00120 -0.00014 C5 1 0.593023 0.817569 0.225070 11.00000 0.05437 0.05199 = 0.04425 -0.01869 -0.00319 -0.00814 AFIX 43 H5 2 0.524959 0.776628 0.245708 11.00000 -1.20000 AFIX 0 C6 1 0.614278 0.877483 0.113754 11.00000 0.07265 0.04743 = 0.04374 -0.01797 -0.00830 -0.00029 AFIX 43 H6 2 0.560782 0.875152 0.059900 11.00000 -1.20000 AFIX 0 C7 1 0.710295 0.939193 0.080988 11.00000 0.08561 0.04613 = 0.03626 -0.01172 0.00342 0.00286 AFIX 43 H7 2 0.720881 0.980165 0.005071 11.00000 -1.20000 AFIX 0 C8 1 0.794762 0.942791 0.159428 11.00000 0.06025 0.03275 = 0.05166 -0.01218 0.02043 -0.00416 C9 1 0.893038 1.007315 0.130496 11.00000 0.08369 0.04155 = 0.05885 -0.01219 0.02954 -0.01510 AFIX 43 H9 2 0.904021 1.052942 0.055436 11.00000 -1.20000 AFIX 0 C10 1 0.973811 1.004852 0.210471 11.00000 0.06690 0.04461 = 0.09215 -0.02170 0.03858 -0.02653 AFIX 43 H10 2 1.039201 1.049166 0.189258 11.00000 -1.20000 AFIX 0 C11 1 0.474315 0.783343 0.821114 11.00000 0.04756 0.06276 = 0.05788 -0.03245 0.01507 -0.00824 AFIX 23 H11A 2 0.454441 0.769535 0.898273 11.00000 -1.20000 H11B 2 0.438026 0.879694 0.776451 11.00000 -1.20000 AFIX 0 C12 1 0.408071 0.706009 0.780500 11.00000 0.03652 0.06141 = 0.05754 -0.02353 0.01459 -0.01263 AFIX 23 H12A 2 0.310918 0.753360 0.764135 11.00000 -1.20000 H12B 2 0.420674 0.616033 0.837019 11.00000 -1.20000 AFIX 0 C13 1 0.695434 0.879358 0.791104 11.00000 0.07528 0.07051 = 0.10294 -0.05856 0.02256 -0.03156 AFIX 137 H13A 2 0.792362 0.860265 0.798837 11.00000 -1.50000 H13B 2 0.652106 0.913694 0.846518 11.00000 -1.50000 H13C 2 0.661173 0.945964 0.717904 11.00000 -1.50000 AFIX 0 C14 1 0.715361 0.628580 0.957352 11.00000 0.08262 0.08062 = 0.04443 -0.03336 -0.00539 0.00388 AFIX 137 H14A 2 0.684299 0.550635 0.985314 11.00000 -1.50000 H14B 2 0.678282 0.685321 0.999059 11.00000 -1.50000 H14C 2 0.813302 0.599438 0.965188 11.00000 -1.50000 AFIX 0 C15 1 0.401660 0.596606 0.617767 11.00000 0.04635 0.09363 = 0.08427 -0.04491 0.00484 -0.03289 AFIX 137 H15A 2 0.433047 0.586249 0.549286 11.00000 -1.50000 H15B 2 0.305215 0.643593 0.608724 11.00000 -1.50000 H15C 2 0.419747 0.508675 0.676696 11.00000 -1.50000 AFIX 0 C16 1 0.396044 0.863178 0.555128 11.00000 0.04443 0.06565 = 0.06362 -0.00579 0.00153 0.00216 AFIX 137 H16A 2 0.422430 0.930063 0.570172 11.00000 -1.50000 H16B 2 0.299915 0.878707 0.563612 11.00000 -1.50000 H16C 2 0.415900 0.869763 0.480060 11.00000 -1.50000 AFIX 0 C17 1 0.910427 0.325185 0.839111 11.00000 0.05083 0.04382 = 0.09674 -0.00040 -0.01343 -0.00864 AFIX 23 H17A 2 0.902583 0.259495 0.911934 11.00000 -1.20000 H17B 2 0.963480 0.275836 0.794928 11.00000 -1.20000 AFIX 0 C18 1 0.982246 0.415530 0.852652 11.00000 0.04466 0.05644 = 0.04965 -0.01273 -0.00980 -0.00440 AFIX 23 H18A 2 1.080246 0.371052 0.861068 11.00000 -1.20000 H18B 2 0.953689 0.435913 0.918609 11.00000 -1.20000 AFIX 0 C19 1 0.731501 0.328270 0.686059 11.00000 0.07355 0.05013 = 0.07798 -0.03339 0.01479 -0.02214 AFIX 137 H19A 2 0.639759 0.356972 0.655202 11.00000 -1.50000 H19B 2 0.758446 0.233238 0.732204 11.00000 -1.50000 H19C 2 0.791991 0.343767 0.626495 11.00000 -1.50000 AFIX 0 C20 1 0.635058 0.356838 0.880879 11.00000 0.07544 0.05111 = 0.05584 -0.00822 0.01734 -0.02799 AFIX 137 H20A 2 0.638758 0.387798 0.940039 11.00000 -1.50000 H20B 2 0.668881 0.259390 0.909425 11.00000 -1.50000 H20C 2 0.542274 0.387438 0.851670 11.00000 -1.50000 AFIX 0 C21 1 1.030186 0.665995 0.764374 11.00000 0.04603 0.07032 = 0.10289 -0.04911 -0.00507 -0.02145 AFIX 137 H21A 2 1.015654 0.753183 0.705082 11.00000 -1.50000 H21B 2 1.125991 0.616120 0.775473 11.00000 -1.50000 H21C 2 0.997538 0.678108 0.832001 11.00000 -1.50000 AFIX 0 C22 1 1.058583 0.510961 0.635307 11.00000 0.03798 0.06478 = 0.06537 -0.03212 0.00873 -0.00546 AFIX 137 H22A 2 1.029614 0.448761 0.615333 11.00000 -1.50000 H22B 2 1.147688 0.465477 0.673240 11.00000 -1.50000 H22C 2 1.061932 0.586522 0.568923 11.00000 -1.50000 AFIX 0 B1 3 0.742863 0.740516 0.510241 11.00000 0.03214 0.04081 = 0.04073 -0.01440 0.00611 -0.01410 H1A 2 0.760683 0.609674 0.576523 11.00000 0.04356 H1B 2 0.692551 0.791601 0.592653 11.00000 0.03570 HKLF 5 REM se20013_a.res in P-1 REM wR2 = 0.1549, GooF = S = 1.033, Restrained GooF = 1.033 for all data REM R1 = 0.0576 for 8298 Fo > 4sig(Fo) and 0.0655 for all 9758 data REM 296 parameters refined using 2 restraints END WGHT 0.1064 0.3340 REM Highest difference peak 0.599, deepest hole -0.469, 1-sigma level 0.072 Q1 1 0.7768 0.6769 0.6824 11.00000 0.05 0.60 Q2 1 0.6556 0.7326 0.6376 11.00000 0.05 0.57 Q3 1 0.7227 0.6646 0.6052 11.00000 0.05 0.53 Q4 1 0.6518 0.5962 0.6737 11.00000 0.05 0.53 Q5 1 0.7633 0.6084 0.6495 11.00000 0.05 0.49 ; _shelx_res_checksum 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297.845 -2 -11 -2 -7 2005.05 297.845 1 11 3 8 8038.83 297.596 -2 -11 -3 7 8038.83 297.596 1 11 3 7 3373.47 234.561 -2 -11 -3 6 3373.47 234.561 1 11 3 6 6879.85 429.826 -2 -11 -3 5 6879.85 429.826 1 -11 -3 -5 5487.88 267.115 -2 11 3 -4 5487.88 267.115 1 -11 -3 -4 3547.09 273.150 -2 11 3 -3 3547.09 273.150 1 11 3 3 1673.06 330.910 -2 -11 -3 2 1673.06 330.910 1 11 3 2 1228.63 258.553 -2 -11 -3 1 1228.63 258.553 1 11 3 1 475.072 206.589 -2 -11 -3 0 475.072 206.589 1 11 3 0 883.934 315.561 -2 -11 -3 -1 883.934 315.561 1 11 3 -1 1232.75 234.979 -2 -11 -3 -2 1232.75 234.979 1 11 3 -2 2707.44 299.440 -2 -11 -3 -3 2707.44 299.440 1 11 3 -3 3784.13 342.662 -2 -11 -3 -4 3784.13 342.662 1 11 3 -4 6897.56 334.450 -2 -11 -3 -5 6897.56 334.450 1 11 3 -5 7779.66 410.309 -2 -11 -3 -6 7779.66 410.309 1 11 3 -6 4146.31 353.397 -2 -11 -3 -7 4146.31 353.397 1 11 3 -7 8567.30 310.393 -2 -11 -3 -8 8567.30 310.393 1 11 4 9 9265.32 261.627 -2 -11 -4 7 9265.32 261.627 1 11 4 8 1140.16 290.746 -2 -11 -4 6 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13299.0 385.990 -2 -11 -6 1 13299.0 385.990 1 11 6 4 5666.43 383.787 -2 -11 -6 0 5666.43 383.787 1 11 6 3 12796.7 375.304 -2 -11 -6 -1 12796.7 375.304 1 11 6 2 10933.6 368.719 -2 -11 -6 -2 10933.6 368.719 1 11 6 1 12382.9 386.554 -2 -11 -6 -3 12382.9 386.554 1 11 6 0 6231.20 355.804 -2 -11 -6 -4 6231.20 355.804 1 11 6 -1 13901.9 412.256 -2 -11 -6 -5 13901.9 412.256 1 11 6 -2 170.948 354.110 -2 -11 -6 -6 170.948 354.110 1 11 6 -3 4328.43 408.643 -2 -11 -6 -7 4328.43 408.643 1 11 6 -4 2132.80 358.792 -2 -11 -6 -8 2132.80 358.792 1 -11 -6 -9 106.428 162.954 1 -11 -7 4 56.3510 202.659 1 -11 -7 3 40.9918 247.043 1 11 7 7 2160.24 358.113 -2 -11 -7 2 2160.24 358.113 1 11 7 6 8335.91 355.330 -2 -11 -7 1 8335.91 355.330 1 11 7 5 1870.49 365.144 -2 -11 -7 0 1870.49 365.144 1 11 7 4 19761.7 465.602 -2 -11 -7 -1 19761.7 465.602 1 11 7 3 7635.43 354.718 -2 -11 -7 -2 7635.43 354.718 1 11 7 2 7663.24 372.954 -2 -11 -7 -3 7663.24 372.954 1 11 7 1 22689.3 427.679 -2 -11 -7 -4 22689.3 427.679 1 11 7 0 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241.772 -2 12 0 0 1106.47 241.772 1 12 0 -3 2966.64 259.005 -2 -12 0 -1 2966.64 259.005 1 -12 0 -2 356.098 264.365 1 12 1 4 2555.47 379.843 -2 -12 -1 5 2555.47 379.843 1 12 1 3 379.409 245.315 -2 -12 -1 4 379.409 245.315 1 12 1 2 311.277 278.485 -2 -12 -1 3 311.277 278.485 1 12 1 1 1256.84 298.309 -2 -12 -1 2 1256.84 298.309 1 12 1 0 1521.47 305.388 -2 -12 -1 1 1521.47 305.388 1 12 1 -1 236.246 263.607 -2 -12 -1 0 236.246 263.607 1 12 1 -2 507.131 197.140 -2 -12 -1 -1 507.131 197.140 1 12 1 -3 303.931 166.949 -2 -12 -1 -2 303.931 166.949 1 12 1 -4 830.494 282.852 -2 -12 -1 -3 830.494 282.852 1 12 1 -5 2110.08 443.925 -2 -12 -1 -4 2110.08 443.925 1 12 2 5 392.171 268.397 -2 -12 -2 5 392.171 268.397 1 12 2 4 1555.51 223.335 -2 -12 -2 4 1555.51 223.335 1 12 2 3 3127.07 254.304 -2 -12 -2 3 3127.07 254.304 1 12 2 2 350.910 132.409 -2 -12 -2 2 350.910 132.409 1 12 2 1 506.698 233.147 -2 -12 -2 1 506.698 233.147 1 12 2 0 1286.57 481.113 -2 -12 -2 0 1286.57 481.113 1 12 2 -1 222.271 355.164 -2 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362.334 2 -1 3 -13 52.7485 146.689 2 1 0 -15 1484.18 143.735 2 1 0 -14 110.546 121.133 2 1 0 -13 4197.64 120.500 2 1 0 -12 3825.64 121.344 2 1 0 -11 1260.29 125.390 2 1 0 -10 3986.70 180.001 2 1 0 -9 30808.2 319.960 2 1 0 -8 1554.78 263.786 2 1 0 -6 620.270 917.236 2 1 0 -4 54878.3 200.566 2 1 0 -3 107651. 373.819 2 1 0 -2 478.732 125.754 2 -1 0 1 101379. 356.894 2 -1 0 0 18466.3 103.316 2 -1 0 -1 45969.9 566.952 2 -1 0 -2 17948.6 626.781 2 1 0 3 66340.2 275.067 2 1 0 4 622.228 98.9844 2 -1 0 -5 4862.99 410.480 2 -1 0 -6 15552.0 565.284 2 -1 0 -7 1639.04 541.437 2 -1 0 -8 18232.4 362.647 2 -1 0 -9 2582.50 205.575 2 -1 0 -10 12654.2 228.545 2 -1 0 -11 393.924 117.803 2 -1 0 -12 590.501 112.822 2 -1 0 -13 973.261 117.512 2 -1 0 -14 490.390 117.468 2 -1 0 -15 3351.84 162.709 2 1 1 -14 611.901 124.598 2 1 1 -13 90.0862 103.190 2 -1 -1 12 212.634 113.304 2 -1 -1 11 286.051 120.338 2 1 1 -10 9517.92 143.457 2 1 1 -9 5039.61 125.405 2 1 1 -8 43797.5 220.288 2 1 1 -7 84940.5 258.155 2 1 1 -6 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617.854 135.332 2 1 7 15 78.4619 133.790 2 1 7 16 349.419 143.146 2 -1 -8 8 10.4607 91.0182 2 -1 -8 7 257.427 121.714 2 -1 -8 6 534.282 140.755 2 -1 -8 5 529.446 222.529 2 -1 -8 4 2961.79 632.846 2 1 8 -1 3809.53 878.230 2 -1 -8 -7 71196.1 1094.35 2 1 8 8 1076.56 740.142 2 -1 -8 -11 11148.3 579.412 2 -1 -8 -12 5654.94 265.990 2 1 8 13 355.702 150.448 2 1 8 14 332.108 124.732 2 1 8 15 79.4140 125.255 2 1 8 16 1998.68 158.217 2 1 9 -7 365.253 224.899 2 -1 -13 -2 561.475 267.675 2 -2 12 10 441.703 224.211 2 2 -12 -9 4841.03 147.128 2 -2 12 8 218.164 192.158 2 -2 12 7 10879.9 360.051 2 -2 12 5 7944.86 402.189 2 2 -12 -3 327.200 250.252 2 2 -12 -2 862.518 200.755 2 2 -11 -12 1113.70 124.289 2 -2 11 11 209.209 132.712 2 2 -11 -10 133.155 126.494 2 2 -11 -9 824.371 144.951 2 2 -11 -8 1842.04 158.937 2 2 -11 -7 7478.85 178.050 2 -2 11 6 2130.49 231.806 2 -2 11 5 12624.3 212.661 2 -2 11 4 247.320 162.437 2 -2 11 3 6592.07 158.926 2 2 -11 -2 2426.42 157.048 2 2 -11 -1 56.9908 141.282 2 2 -11 0 2453.36 168.617 2 2 -11 1 916.162 132.331 2 2 -11 2-137.259 134.978 2 -2 10 13 672.939 130.008 2 -2 10 12 194.011 143.323 2 -2 10 11 235.575 137.172 2 -2 10 10 162.155 146.006 2 -2 10 9 233.649 134.696 2 -2 10 8 3051.30 153.095 2 2 -10 -7 2361.04 165.942 2 2 -10 -6 6999.09 166.721 2 2 -10 -5 6024.74 168.176 2 2 -10 -4 194.269 156.310 2 2 -10 -3 13340.7 196.611 2 2 -10 -2 3330.22 162.723 2 2 -10 -1 11331.2 184.926 2 2 -10 0 15407.9 194.451 2 2 -10 1 1355.57 159.653 2 2 -10 2 5813.00 183.969 2 -2 10 -3 173.789 153.488 2 2 -10 4 6.83337 137.040 2 -2 9 14 790.945 130.949 2 -2 9 13 1027.51 159.297 2 -2 9 12 1064.93 140.634 2 -2 9 11 927.238 156.548 2 -2 9 10 219.803 148.721 2 -2 9 9 6939.62 158.860 2 -2 9 8 1299.95 148.723 2 2 -9 -7 7946.79 184.781 2 2 -9 -6 384.506 163.178 2 2 -9 -5 112.876 162.137 2 -2 9 4 786.730 170.832 2 2 -9 -3 15444.7 216.694 2 2 -9 -2 249.007 151.660 2 2 -9 -1 31664.7 226.418 2 2 -9 0 837.681 166.691 2 2 -9 1 7010.25 154.268 2 2 -9 2 3302.53 146.474 2 2 -9 3-27.4790 129.778 2 2 -9 4 1730.89 132.613 2 2 -9 5 828.726 108.453 2 -2 8 15 2063.08 140.336 2 -2 8 14 930.206 147.826 2 -2 8 13 9694.67 164.057 2 -2 8 12 389.031 142.932 2 -2 8 11 862.491 158.895 2 -2 8 10 3937.95 163.865 2 -2 8 9 396.612 150.947 2 2 -8 -8 9464.56 187.689 2 2 -8 -7 326.035 162.542 2 2 -8 -6 10198.6 204.223 2 -2 8 5 3505.51 214.388 2 2 -8 -4 12555.6 264.275 2 -2 8 3 3082.64 266.566 2 2 -8 -2 10895.4 327.701 2 -2 8 1 15573.9 237.760 2 2 -8 0 4849.50 143.562 2 2 -8 1 22670.9 184.340 2 2 -8 2 495.591 135.073 2 2 -8 3 7800.28 152.355 2 2 -8 4 7278.52 161.633 2 2 -8 5 149.728 127.510 2 2 -8 6 2942.82 130.309 2 -2 8 -7 291.259 93.1538 2 -2 7 15 1666.17 113.530 2 -2 7 14 314.580 152.423 2 -2 7 13 1679.74 140.367 2 2 -7 -12 432.077 140.793 2 -2 7 11 899.317 148.525 2 -2 7 10 231.378 140.971 2 2 -7 -9 3336.02 163.740 2 2 -7 -8 2040.62 194.592 2 2 -7 -7-110.197 235.425 2 -2 7 6 852.543 331.289 2 -2 7 0 8919.35 456.380 2 -2 7 -1 348.794 203.072 2 2 -7 2 1446.17 158.750 2 2 -7 3 8790.59 168.610 2 2 -7 4 6772.03 154.260 2 2 -7 5 13517.6 168.389 2 2 -7 6 10587.7 160.426 2 2 -7 7 2307.18 132.727 2 2 -7 8 3216.57 108.738 2 -2 6 15 977.038 114.260 2 -2 6 14 655.244 133.893 2 2 -6 -13 671.690 140.549 2 2 -6 -12 2107.75 157.876 2 2 -6 -11 577.645 178.760 2 2 -6 -10 7868.52 677.525 2 -2 6 9 1211.28 515.601 2 -2 6 -2 17241.0 864.106 2 -2 6 -4 4288.86 711.271 2 -2 6 -5 21022.2 272.223 2 -2 6 -6 1493.16 160.013 2 2 -6 7 14566.4 167.290 2 2 -6 8 5317.14 124.769 2 2 -6 9-25.7985 122.556 2 2 -6 10 1128.65 89.2698 2 -2 5 16 267.761 195.791 2 -2 5 -11 403.768 106.573 2 2 -2 -15 2449.68 138.544 2 2 -2 -14 5817.19 136.164 2 2 -2 -13 1291.63 165.459 2 2 -2 -12 8793.04 278.327 2 -2 2 11 2968.11 1029.82 2 2 -2 -2 8257.61 174.172 2 2 -2 -1 60485.1 630.531 2 -2 2 -9 10625.2 790.765 2 2 -2 10 9669.23 293.019 2 2 -2 11 355.899 122.274 2 2 -2 12 3579.94 114.899 2 -2 2 -13 453.725 127.276 2 2 -1 -15 7483.26 154.043 2 2 -1 -14 147.261 116.053 2 2 -1 -13 11069.4 146.784 2 2 -1 -12 8031.66 146.262 2 2 -1 -11 2046.98 133.241 2 2 -1 -10 5089.36 139.050 2 2 -1 -9 505.466 123.762 2 2 -1 -8 336.798 135.253 2 2 -1 -7 4755.76 143.931 2 2 -1 -6 105.705 125.957 2 -2 1 5 10278.3 137.992 2 2 -1 -4 30155.0 186.723 2 2 -1 -3 47390.6 240.634 2 -2 1 2 27336.8 299.595 2 -2 1 1 112256. 651.272 2 -2 1 0 6943.04 130.004 2 -2 1 -1 663.380 125.111 2 -2 1 -2 181.281 118.605 2 -2 1 -3 856.618 124.840 2 -2 1 -4 3392.98 108.205 2 -2 1 -5 153.082 118.400 2 -2 1 -6 171.152 118.981 2 -2 1 -7 32041.6 194.041 2 2 -1 8 4492.80 116.827 2 2 -1 9 37504.0 174.531 2 2 -1 10 12816.0 141.087 2 2 -1 11 9114.13 136.997 2 -2 1 -12 2265.77 120.717 2 -2 1 -13 130.689 110.979 2 -2 1 -14 1043.52 166.061 2 2 0 -15 2151.49 141.161 2 2 0 -14 4532.53 119.361 2 2 0 -13 7048.58 118.716 2 2 0 -12 310.199 123.850 2 2 0 -11 8323.14 145.913 2 2 0 -10 10641.3 145.030 2 2 0 -9 2653.96 122.991 2 2 0 -8 40835.7 219.291 2 2 0 -7 23511.4 173.540 2 2 0 -6 4335.98 144.290 2 2 0 -5 73128.3 217.945 2 -2 0 4 37845.5 177.234 2 2 0 -3 3055.80 124.498 2 2 0 -2 8964.40 154.224 2 2 0 -1 8297.07 157.000 2 2 0 0 18231.6 146.153 2 -2 0 -1 3677.47 174.533 2 2 0 2 1194.48 145.580 2 -2 0 -3 9591.04 138.979 2 -2 0 -4 13737.5 143.522 2 -2 0 -5 3721.60 145.773 2 -2 0 -6 831.766 120.801 2 -2 0 -7 23330.4 184.666 2 -2 0 -8 2475.28 142.690 2 -2 0 -9 5447.02 116.248 2 -2 0 -10 4789.14 125.958 2 -2 0 -11 15712.5 158.902 2 -2 0 -12 856.648 120.038 2 -2 0 -13 1459.86 124.973 2 -2 0 -14 1464.50 119.161 2 2 1 -14 1919.48 129.105 2 2 1 -13 293.360 102.126 2 -2 -1 12 2482.46 112.001 2 2 1 -11 24329.5 183.831 2 2 1 -10 11918.3 148.713 2 2 1 -9 21508.9 156.959 2 2 1 -8 61573.1 270.069 2 2 1 -7 20046.7 166.873 2 2 1 -6 14919.7 153.045 2 2 1 -5 22780.1 198.066 2 -2 -1 4 6328.63 120.412 2 -2 -1 3 3629.80 106.853 2 2 1 -2 69429.2 195.265 2 2 1 -1 32210.6 219.704 2 2 1 0 11213.7 233.935 2 2 1 1 1177.39 215.971 2 2 1 2 8823.98 113.844 2 2 1 3 722.955 97.3854 2 -2 -1 -4 1112.02 101.417 2 -2 -1 -5 1701.64 116.436 2 -2 -1 -6 2417.29 120.186 2 -2 -1 -7 72.9526 119.123 2 -2 -1 -8 8886.24 154.280 2 2 1 9 12187.1 141.791 2 2 1 10 6714.69 132.606 2 -2 -1 -11 12711.8 142.837 2 -2 -1 -12 168.883 127.957 2 -2 -1 -13 2041.67 126.888 2 -2 -1 -14 6547.93 133.595 2 -2 -1 -15 1557.48 146.824 2 2 2 -14 78.1123 128.827 2 2 2 -13 347.337 128.763 2 -2 -2 12 1469.22 113.007 2 2 2 -11 840.502 124.897 2 2 2 -10 775.016 131.224 2 2 2 -9 25016.5 178.416 2 2 2 -8 8514.90 142.933 2 2 2 -7 64577.0 319.018 2 2 2 -6 45184.4 259.394 2 2 2 -5 20033.9 188.507 2 2 2 -4 16577.0 139.427 2 2 2 -3 10330.7 122.040 2 2 2 -2 426.933 88.4246 2 2 2 -1 8190.76 124.252 2 2 2 0 7938.75 224.831 2 2 2 1 8897.10 311.138 2 2 2 2 16924.6 180.006 2 2 2 3 8985.45 151.950 2 2 2 4 15434.4 139.731 2 2 2 5 981.690 101.803 2 2 2 6 573.679 112.343 2 -2 -2 -7 19672.0 159.940 2 -2 -2 -8 120.074 127.061 2 -2 -2 -9 1533.88 137.256 2 2 2 10 21752.4 163.259 2 2 2 11 737.732 122.373 2 2 2 12 2007.09 120.488 2 -2 -2 -13 6367.48 139.650 2 -2 -2 -14 921.826 119.082 2 -2 -2 -15 6920.65 129.137 2 2 3 -13 290.957 102.526 2 -2 -3 12 99.4462 112.485 2 -2 -3 11 242.338 113.844 2 2 3 -10 18220.5 168.234 2 2 3 -9 11790.1 155.889 2 2 3 -8 7346.23 146.872 2 2 3 -7 44384.4 208.429 2 2 3 -6 2888.86 163.580 2 2 3 -5 30291.6 233.211 2 2 3 -4 15506.5 173.521 2 2 3 -3 36230.8 202.769 2 2 3 -2 11039.7 175.903 2 2 3 -1 2304.68 116.871 2 -2 -3 0 59352.7 310.927 2 -2 -3 -1 68238.9 283.934 2 -2 -3 -2 1275.11 119.346 2 2 3 3 153.914 101.291 2 2 3 4 54250.8 225.440 2 -2 -3 -5 44636.6 222.710 2 -2 -3 -6 26081.9 162.786 2 -2 -3 -7 7467.22 155.269 2 -2 -3 -8 11374.6 156.897 2 -2 -3 -9 630.660 140.631 2 2 3 10 5105.81 143.327 2 2 3 11 259.938 133.035 2 2 3 12 2023.37 135.735 2 2 3 13 2954.98 126.433 2 2 3 14 551.644 119.276 2 -2 -3 -15 5452.22 130.067 2 -2 -4 12-64.2487 101.438 2 -2 -4 11 2335.22 123.530 2 -2 -4 10 716.441 115.824 2 2 4 -9 2317.32 128.586 2 2 4 -8 6849.06 155.389 2 2 4 -7 88.2264 132.115 2 2 4 -6 6060.93 155.725 2 2 4 -5 23235.1 218.414 2 2 4 -4 19684.0 219.312 2 2 4 -3 58666.9 263.763 2 2 4 -2 57359.3 240.639 2 2 4 -1 15954.7 186.690 2 2 4 0 127962. 520.673 2 -2 -4 -1 2420.06 154.686 2 -2 -4 -2 20000.9 188.983 2 -2 -4 -3 1430.42 107.683 2 -2 -4 -4 13194.7 153.811 2 -2 -4 -5 1401.50 106.599 2 -2 -4 -6 2339.98 114.848 2 -2 -4 -7 959.054 126.137 2 -2 -4 -8 3479.00 147.195 2 -2 -4 -9 182.540 132.371 2 2 4 10 4359.72 144.837 2 2 4 11 7107.02 166.070 2 2 4 12 688.524 144.058 2 2 4 13 263.312 138.812 2 -2 -4 -14 3281.69 117.888 2 2 4 15 246.674 138.243 2 -2 -4 -16 580.279 141.349 2 -2 -5 12 1158.71 125.261 2 -2 -5 11 1218.06 99.9589 2 -2 -5 10 1560.57 117.787 2 -2 -5 9 12062.4 146.329 2 2 5 -8 614.201 133.946 2 2 5 -7 4290.41 146.144 2 2 5 -6 493.224 144.271 2 2 5 -5 5486.61 148.903 2 2 5 -4 1233.22 150.669 2 2 5 -3 91358.0 354.754 2 2 5 -2 1619.16 127.051 2 2 5 -1 81676.7 344.901 2 -2 -5 0 6878.54 239.376 2 -2 -5 -1 25888.3 287.230 2 -2 -5 -2 30361.2 294.618 2 -2 -5 -3 14226.3 197.251 2 -2 -5 -4 10016.8 150.176 2 -2 -5 -5 11226.7 162.569 2 -2 -5 -6 18752.5 170.144 2 -2 -5 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2 2 11 -3 477.972 160.349 2 -2 -11 2 2899.32 192.891 2 -2 -11 -12 296.858 179.527 2 2 11 13 190.194 115.640 2 -2 -11 -14 748.756 181.924 2 -2 -12 2 357.157 129.507 2 -2 -12 1 66.8178 160.213 2 -2 -12 0 1268.97 169.600 2 2 12 1 323.116 169.835 2 -2 -12 -3 3692.86 647.573 2 -2 -12 -10 4781.99 235.748 2 -2 -12 -11 307.702 187.423 2 -2 -12 -12 713.283 142.979 2 -2 -12 -13 402.258 145.717 2 -2 -13 0 3354.98 213.288 2 -2 -13 -1 1304.52 202.114 2 -2 -13 -2 107.431 155.822 2 2 13 3 520.290 224.675 2 2 13 8 2926.56 366.462 2 -2 -13 -10 3746.22 147.165 2 -2 -13 -11 884.195 139.571 2 3 -12 -7 736.712 154.600 2 3 -12 -6 4186.15 151.974 2 3 -12 -5 994.763 119.990 2 -3 12 4 1071.41 245.020 2 -3 11 11 414.717 201.069 2 3 -11 -10 177.563 169.107 2 3 -11 -9 1648.24 144.255 2 3 -11 -8 5260.24 158.277 2 -3 11 7 2913.41 271.369 2 3 -11 -6 19381.4 633.442 2 3 -11 -5 337.098 293.936 2 3 -11 -4 3974.51 265.280 2 3 -11 -3 365.804 170.021 2 3 -11 -2 149.828 127.000 2 3 -11 -1 419.505 143.315 2 -3 11 0 424.241 143.217 2 -3 10 12 1042.66 134.780 2 -3 10 11 445.885 133.196 2 -3 10 10 2488.07 154.931 2 3 -10 -9 5620.54 160.516 2 3 -10 -8 329.308 172.907 2 3 -10 -3 71.8973 539.341 2 -3 10 2 2853.24 243.410 2 3 -10 -1 2281.79 173.082 2 3 -10 0 314.415 186.325 2 3 -10 1 633.524 189.173 2 -3 10 -2 119.394 193.447 2 3 -10 3-41.1494 142.958 2 -3 9 13 289.712 142.633 2 -3 9 12 885.707 136.267 2 -3 9 11 1223.69 150.682 2 3 -9 -10 9337.27 187.031 2 3 -9 -9 562.883 242.950 2 -3 9 0 16450.0 333.764 2 3 -9 1 6805.77 180.619 2 3 -9 2 1384.64 137.782 2 3 -9 3 206.511 127.552 2 3 -9 4 267.492 101.981 2 -3 9 -5 414.726 197.425 2 -3 8 14 310.854 130.328 2 -3 8 13 1014.57 167.023 2 3 -8 -12 2616.15 178.108 2 3 -8 -11 3060.43 804.384 2 3 -8 4 546.675 164.495 2 3 -8 5 408.253 120.463 2 3 -8 6 417.841 103.700 2 3 -7 -15 722.739 169.915 2 -3 7 -8 125.253 109.324 2 3 -4 -15 390.035 132.766 2 -3 4 14 267.059 167.960 2 3 -4 10-28.0264 144.275 2 -3 4 -11 4776.66 105.426 2 3 -3 -15 214.515 112.894 2 3 -3 -14 120.646 127.601 2 3 -3 -13 961.773 136.149 2 -3 3 12 1106.65 135.145 2 -3 3 11 1420.53 143.078 2 -3 3 10 2322.39 148.072 2 3 -3 -9 732.160 130.316 2 3 -3 -8 504.385 161.743 2 3 -3 -7 17766.1 228.265 2 3 -3 -6 2637.11 187.467 2 3 -3 -5 2142.07 192.720 2 3 -3 -4 5701.67 169.458 2 -3 3 3 376.011 175.257 2 -3 3 2 12896.5 269.674 2 -3 3 0 15163.3 377.043 2 -3 3 -1 28956.1 983.011 2 -3 3 -2 173264. 2260.80 2 -3 3 -3 14782.6 253.633 2 -3 3 -4 130889. 449.103 2 -3 3 -5 1953.19 145.454 2 3 -3 6 9917.51 152.838 2 3 -3 7 1366.33 140.003 2 3 -3 8 2216.67 130.974 2 3 -3 9 546.156 135.981 2 3 -3 10 4207.67 137.301 2 3 -3 11 1201.82 114.043 2 -3 3 -12 491.623 114.057 2 3 -2 -15 520.765 117.867 2 3 -2 -14 1270.66 124.963 2 3 -2 -13 5458.48 146.260 2 3 -2 -12 89.1893 147.126 2 3 -2 -11 1448.98 144.061 2 3 -2 -10 5436.44 149.626 2 3 -2 -9 673.351 140.011 2 3 -2 -8 5537.50 167.213 2 3 -2 -7 1341.66 149.086 2 3 -2 -6 7214.20 143.031 2 3 -2 -5 1608.58 115.900 2 3 -2 -4 2774.74 131.644 2 3 -2 -3 10168.2 148.085 2 3 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99.5626 135.851 2 3 -1 8 14823.6 159.639 2 3 -1 9 485.456 127.440 2 3 -1 10 5920.68 156.326 2 -3 1 -11 7672.07 161.313 2 -3 1 -12 997.862 121.837 2 -3 1 -13 545.464 141.951 2 3 0 -14 4767.26 113.814 2 3 0 -13 256.077 125.832 2 3 0 -12 8106.83 156.393 2 3 0 -11 4426.50 160.458 2 3 0 -10 3891.08 149.015 2 3 0 -9 1208.59 127.964 2 3 0 -8 4445.28 157.266 2 3 0 -7 2869.16 153.138 2 3 0 -6 25922.8 213.879 2 3 0 -5 2607.73 112.194 2 3 0 -4 5131.35 123.927 2 3 0 -3 512.859 116.888 2 -3 0 2 160.473 119.112 2 3 0 -1 109302. 265.028 2 -3 0 0 259126. 472.883 2 -3 0 -1 210374. 456.415 2 -3 0 -2 183574. 423.853 2 -3 0 -3 119.081 133.146 2 -3 0 -4 3853.17 132.420 2 3 0 5 362.338 111.114 2 -3 0 -6 4388.98 135.739 2 -3 0 -7 14193.9 181.075 2 -3 0 -8 74312.4 271.701 2 3 0 9 128.103 116.498 2 -3 0 -10 62266.3 236.625 2 -3 0 -11 2027.45 144.029 2 -3 0 -12 6901.16 151.867 2 -3 0 -13 1314.63 131.503 2 -3 0 -14 228.790 145.597 2 3 1 -14 873.200 118.197 2 3 1 -13 1619.35 114.222 2 3 1 -12 2232.25 133.018 2 3 1 -11 250.484 133.178 2 3 1 -10 2278.74 137.054 2 3 1 -9 1158.05 140.129 2 3 1 -8 18310.8 170.882 2 3 1 -7 5668.38 146.410 2 3 1 -6 28443.3 189.471 2 3 1 -5 2010.34 124.604 2 -3 -1 4 8333.79 135.230 2 3 1 -3 26493.2 189.403 2 -3 -1 2 397.139 107.417 2 3 1 -1 20049.0 226.240 2 3 1 0 1977.97 161.794 2 3 1 1 34165.9 229.895 2 3 1 2 37637.3 175.173 2 -3 -1 -3 34657.8 183.389 2 -3 -1 -4 2083.72 119.064 2 -3 -1 -5 6073.46 125.545 2 -3 -1 -6 1097.53 119.744 2 -3 -1 -7 31315.3 199.671 2 -3 -1 -8 254.857 130.246 2 3 1 9 10177.2 146.837 2 3 1 10 740.779 125.124 2 3 1 11 1948.38 139.506 2 -3 -1 -12 8585.30 155.421 2 -3 -1 -13 1608.84 139.679 2 -3 -1 -14 1183.25 124.910 2 -3 -1 -15 2003.82 194.365 2 3 2 -14 1261.74 127.007 2 -3 -2 13 387.771 112.537 2 -3 -2 12 555.465 109.299 2 3 2 -11 2110.36 137.642 2 3 2 -10 16442.9 171.357 2 3 2 -9 1113.83 134.608 2 3 2 -8 11328.5 174.034 2 3 2 -7 1748.74 165.038 2 3 2 -6 24749.4 215.677 2 3 2 -5 808.429 132.275 2 3 2 -4 12481.0 153.613 2 -3 -2 3 556.008 112.484 2 3 2 -2 2586.06 122.080 2 3 2 -1 2084.97 159.365 2 3 2 0 9850.82 199.450 2 3 2 1 542.005 292.591 2 3 2 2 898.996 112.093 2 3 2 3 3995.26 124.521 2 3 2 4 66065.6 227.369 2 3 2 5 4540.58 118.099 2 -3 -2 -6 11518.1 144.385 2 -3 -2 -7 298.868 126.275 2 -3 -2 -8 20311.1 196.499 2 3 2 9 19063.4 159.027 2 3 2 10 1686.69 124.101 2 3 2 11 17264.1 149.534 2 3 2 12 1840.72 120.753 2 -3 -2 -13 210.080 130.678 2 -3 -2 -14 7071.79 148.620 2 -3 -2 -15 3105.01 136.850 2 3 3 -13-26.7777 107.926 2 -3 -3 12 903.750 110.917 2 3 3 -11 2165.81 135.896 2 3 3 -10 769.869 130.947 2 3 3 -9 2455.14 136.889 2 3 3 -8 10963.4 156.353 2 3 3 -7 1111.36 141.981 2 3 3 -6 13872.8 204.892 2 3 3 -5 267.142 158.455 2 3 3 -4 15507.9 164.919 2 3 3 -3 6291.68 147.188 2 -3 -3 2 468.488 121.431 2 -3 -3 1 494.645 98.7916 2 3 3 0 22429.4 286.430 2 3 3 1 2274.21 282.909 2 3 3 2 22087.8 311.664 2 3 3 3 14872.2 149.972 2 3 3 4 1325.45 117.478 2 -3 -3 -5 540.876 105.086 2 -3 -3 -6 3680.59 121.978 2 -3 -3 -7 9867.43 170.933 2 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614.993 99.7428 2 -3 -5 10 7828.28 318.545 2 -3 -5 -14 13982.4 269.237 2 3 5 15 1994.23 107.441 2 -3 -5 -16 1365.87 171.066 2 -3 -8 9 88.5996 165.505 2 -3 -8 8 431.850 162.739 2 -3 -8 7 3186.27 337.609 2 -3 -8 -15 81.3125 217.196 2 -3 -9 7 1663.81 103.499 2 -3 -9 6 422.164 121.776 2 -3 -9 5 4921.54 147.909 2 -3 -9 4 12866.3 215.007 2 -3 -9 3 563.062 329.255 2 -3 -9 -11 4430.58 571.764 2 -3 -9 -12 233.716 203.178 2 -3 -9 -13 1188.79 156.217 2 3 9 14 386.957 161.692 2 3 9 15 161.034 120.857 2 3 10 -6 691.302 128.506 2 -3 -10 5 3211.47 141.020 2 -3 -10 4 1252.17 134.923 2 -3 -10 3 5161.03 172.250 2 -3 -10 2 109.689 167.597 2 -3 -10 1 479.532 178.939 2 -3 -10 0 17236.9 327.813 2 -3 -10 -1 6560.24 741.768 2 -3 -10 -5 5135.28 634.738 2 3 10 6 1841.23 299.644 2 -3 -10 -9 4015.02 276.007 2 3 10 10 88.8226 169.061 2 3 10 11 2208.92 171.974 2 3 10 12-165.444 155.330 2 3 10 13 250.338 134.724 2 3 10 14 304.092 122.727 2 3 10 15 332.311 128.336 2 3 11 -4 296.187 130.044 2 3 11 -3 799.131 166.411 2 3 11 -2 4504.16 163.194 2 -3 -11 1 883.677 157.909 2 -3 -11 0 9767.47 176.280 2 -3 -11 -1 334.706 155.554 2 -3 -11 -2 15404.9 323.688 2 -3 -11 -3 132.871 315.318 2 -3 -11 -4 10196.3 419.897 2 -3 -11 -5 404.547 367.928 2 -3 -11 -6 736.829 268.445 2 -3 -11 -7 150.044 389.971 2 -3 -11 -8 616.199 249.395 2 -3 -11 -9 156.277 157.859 2 -3 -11 -10 753.108 174.909 2 -3 -11 -11 61.7601 199.347 2 3 11 12 326.703 140.534 2 3 11 13 212.178 127.621 2 -3 -11 -14 825.221 147.331 2 -3 -12 2 1228.55 140.773 2 -3 -12 1 318.196 168.528 2 -3 -12 0 76.9146 163.226 2 -3 -12 -1 5612.16 179.261 2 -3 -12 -2 1894.48 168.157 2 -3 -12 -3 1596.79 175.235 2 -3 -12 -4 3295.33 218.152 2 -3 -12 -5 181.160 180.246 2 -3 -12 -6 3184.65 224.511 2 -3 -12 -7 4761.54 245.948 2 -3 -12 -8 135.593 158.604 2 -3 -12 -9 4673.88 171.680 2 -3 -12 -10 46.6770 158.849 2 -3 -12 -11 577.003 215.062 2 -3 -12 -12 431.761 144.436 2 -3 -12 -13 337.932 146.077 2 -3 -13 0 2098.72 184.192 2 -3 -13 -1 487.438 211.661 2 -3 -13 -2 1122.80 171.603 2 -3 -13 -3 1281.15 153.630 2 -3 -13 -4 914.371 154.785 2 -3 -13 -5 154.614 169.503 2 -3 -13 -6 6742.55 193.952 2 3 13 7 1674.49 162.676 2 -3 -13 -8 11838.7 207.186 2 -3 -13 -9 3200.42 165.274 2 -3 -13 -10 2735.57 165.763 2 -3 -13 -11 757.732 129.341 2 3 14 8 5198.31 290.205 2 4 -11 -3-175.867 244.986 2 4 -10 -11 3352.03 179.462 2 4 -10 1 640.105 242.774 2 4 -6 8 783.769 245.573 2 4 -5 -15 453.019 131.241 2 -4 5 14 963.297 123.013 2 -4 5 13 278.858 119.422 2 -4 5 12 4155.09 157.702 2 -4 5 11 2217.45 163.748 2 4 -5 -10 10360.4 291.904 2 4 -5 -9 1113.16 264.839 2 4 -5 -8 3215.29 370.364 2 4 -5 -7 186.721 311.852 2 -4 5 5 7934.25 547.477 2 -4 5 3 42638.9 782.788 2 -4 5 -4 158.254 283.862 2 -4 5 -5 6049.10 212.135 2 4 -5 6 4400.15 157.538 2 4 -5 7-138.359 141.297 2 4 -5 8 1643.31 132.014 2 -4 5 -9 1723.13 108.541 2 4 -4 -15 612.807 141.162 2 4 -4 -14 251.315 114.506 2 -4 4 13 290.479 130.288 2 -4 4 12 1855.92 160.922 2 -4 4 11 5066.90 186.570 2 -4 4 10 17010.9 204.117 2 -4 4 9-94.9208 155.784 2 -4 4 8 11487.5 183.210 2 -4 4 7 17733.2 177.424 2 4 -4 -6 1790.23 169.015 2 4 -4 -5 10088.2 192.814 2 4 -4 -4 53368.8 279.674 2 4 -4 -3 782.098 161.368 2 -4 4 2 71237.0 479.260 2 -4 4 1 33812.2 358.649 2 -4 4 0 3522.48 283.991 2 -4 4 -1 25597.6 309.406 2 -4 4 -2 989.455 142.324 2 4 -4 3 2867.22 134.412 2 4 -4 4 4550.41 154.005 2 -4 4 -5 233.476 143.136 2 4 -4 6 159.135 148.548 2 4 -4 7 7037.45 158.665 2 4 -4 8 48.5644 138.314 2 4 -4 9 5245.80 136.370 2 -4 4 -10 3090.19 107.280 2 4 -4 11 548.625 112.203 2 4 -3 -15 905.075 142.978 2 4 -3 -14 192.745 127.898 2 4 -3 -13 2748.59 139.846 2 -4 3 12 668.009 140.160 2 4 -3 -11 8168.40 164.940 2 -4 3 10 70.4308 154.699 2 4 -3 -9 9033.13 172.767 2 -4 3 8 5014.18 161.527 2 4 -3 -7 1602.04 176.219 2 4 -3 -6 4482.23 170.847 2 4 -3 -5 91649.1 320.280 2 4 -3 -4 5796.72 130.191 2 4 -3 -3 118637. 292.136 2 -4 3 2 25619.1 160.004 2 -4 3 1 566.036 100.945 2 -4 3 0 36759.2 191.681 2 -4 3 -1 89287.8 276.769 2 -4 3 -2 2889.22 143.398 2 -4 3 -3 50147.1 294.381 2 -4 3 -4 134.262 147.524 2 4 -3 5 10941.3 166.452 2 4 -3 6 1053.35 141.722 2 4 -3 7 1794.88 139.490 2 4 -3 8 255.763 127.702 2 4 -3 9 1311.88 131.003 2 4 -3 10 3234.35 127.757 2 4 -3 11 273.257 95.8011 2 4 -2 -14 174.169 124.152 2 4 -2 -13 4807.79 150.819 2 4 -2 -12 834.035 151.609 2 4 -2 -11 4345.68 155.385 2 4 -2 -10 4211.39 154.838 2 -4 2 9 1836.86 164.969 2 4 -2 -8 8516.48 165.260 2 4 -2 -7 951.207 157.256 2 4 -2 -6 107075. 345.523 2 4 -2 -5 42638.1 271.412 2 4 -2 -4 91570.0 295.245 2 4 -2 -3 65396.4 228.747 2 -4 2 2 10360.0 125.000 2 -4 2 1 1804.99 102.818 2 -4 2 0 4670.89 108.441 2 -4 2 -1 18932.7 150.098 2 -4 2 -2 34536.3 223.885 2 -4 2 -3 57301.7 261.081 2 -4 2 -4 16386.4 194.168 2 -4 2 -5 20344.9 203.953 2 4 -2 6 267.619 133.449 2 -4 2 -7 939.224 130.539 2 4 -2 8 4420.45 151.212 2 4 -2 9 241.323 136.556 2 4 -2 10 176.094 120.166 2 -4 2 -11 1009.04 110.550 2 -4 2 -12 513.674 110.532 2 4 -1 -14 446.747 101.451 2 4 -1 -13 8686.44 145.049 2 4 -1 -12 1069.57 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231.059 2 -4 -3 9 1221.99 655.672 2 -4 -3 0 40356.6 426.980 2 -4 -3 -2 6675.88 389.981 2 -4 -3 -11 5762.59 801.122 2 -4 -3 -12 779.346 407.399 2 -4 -3 -13 1118.74 137.003 2 -4 -3 -14 384.922 127.951 2 -4 -3 -15 3069.45 155.582 2 -4 -6 11 3224.93 133.401 2 -4 -6 10 2713.39 258.289 2 -4 -6 9 7530.51 380.484 2 -4 -6 -15 7374.15 252.958 2 -4 -7 10 3036.87 130.051 2 -4 -7 9 602.343 104.235 2 -4 -7 8 2016.13 134.949 2 -4 -7 7 3346.76 160.588 2 4 7 -6 199.790 146.393 2 -4 -7 5 8739.38 337.821 2 -4 -7 4 396.993 632.148 2 4 7 -2 516.453 546.683 2 -4 -7 -11 173.509 350.486 2 4 7 12 10310.2 200.153 2 -4 -7 -13 3135.60 166.526 2 4 7 14 4797.35 144.695 2 4 7 15 2995.01 108.267 2 -4 -8 8 1380.70 105.640 2 -4 -8 7 1770.76 138.234 2 -4 -8 6 373.741 117.751 2 -4 -8 5 4248.35 159.967 2 4 8 -4 11592.7 199.900 2 4 8 -3 4250.72 186.142 2 4 8 -2 530.059 189.762 2 -4 -8 1 17754.2 290.391 2 -4 -8 0 6737.59 405.261 2 -4 -8 -3 598.052 681.091 2 -4 -8 -4 6083.21 519.925 2 -4 -8 -7 73.3292 305.395 2 -4 -8 -8 2802.17 287.516 2 -4 -8 -9 1905.91 211.475 2 4 8 10 137.684 194.242 2 4 8 11 8413.18 205.628 2 -4 -8 -12 1131.74 178.831 2 4 8 13 2495.97 180.202 2 4 8 14 1871.73 161.576 2 4 8 15 204.213 101.586 2 -4 -9 7 608.636 115.464 2 -4 -9 6 2484.80 137.284 2 -4 -9 5 2085.79 128.497 2 -4 -9 4 8415.05 179.717 2 -4 -9 3 1753.58 160.925 2 -4 -9 2 6877.33 197.378 2 -4 -9 1 7625.81 180.149 2 -4 -9 0 461.553 164.390 2 -4 -9 -1 3304.13 299.344 2 -4 -9 -2 3285.42 283.100 2 -4 -9 -3 1244.64 255.013 2 -4 -9 -4 807.214 231.978 2 -4 -9 -5 1034.48 242.570 2 -4 -9 -6 99.6767 234.909 2 -4 -9 -7 90.2149 195.511 2 -4 -9 -8 1523.05 184.984 2 4 9 9 1668.05 180.505 2 4 9 10 2055.38 206.722 2 4 9 11 4838.40 206.494 2 4 9 12 1378.87 188.670 2 4 9 13 2664.91 165.394 2 4 9 14 94.6147 153.950 2 4 9 15 247.561 96.2818 2 -4 -10 6 1494.54 157.478 2 -4 -10 5 162.254 130.934 2 4 10 -4 3953.09 173.497 2 -4 -10 3 1907.09 158.095 2 -4 -10 2 160.791 160.464 2 -4 -10 1 1023.15 162.179 2 4 10 0 384.308 166.150 2 4 10 1 4332.14 196.816 2 4 10 2 2304.40 192.724 2 -4 -10 -3 3009.27 244.492 2 -4 -10 -4 1421.89 245.046 2 -4 -10 -5 1901.46 197.646 2 -4 -10 -6 232.222 222.682 2 -4 -10 -7 516.305 181.447 2 -4 -10 -8 1237.78 179.794 2 -4 -10 -9 1624.28 206.063 2 4 10 10 4461.28 186.008 2 4 10 11 394.242 180.087 2 4 10 12 4437.73 173.856 2 4 10 13 340.889 148.859 2 4 10 14 756.341 134.317 2 -4 -10 -15 580.227 123.516 2 -4 -11 4 249.447 147.423 2 4 11 -3 1728.02 177.115 2 4 11 -2 17.8308 161.739 2 4 11 -1-173.255 177.322 2 4 11 0 3.44147 164.149 2 -4 -11 -1 8396.60 200.028 2 -4 -11 -2 2403.81 185.062 2 -4 -11 -3 6920.73 184.438 2 -4 -11 -4 420.088 154.485 2 -4 -11 -5 4411.40 156.036 2 -4 -11 -6 1639.11 193.080 2 -4 -11 -7 196.961 186.076 2 -4 -11 -8 3682.24 186.417 2 -4 -11 -9 489.424 188.743 2 -4 -11 -10 1065.20 186.209 2 -4 -11 -11-67.4225 194.456 2 -4 -11 -12 605.689 200.228 2 4 11 13 723.824 138.691 2 -4 -11 -14 418.222 142.152 2 -4 -12 3 1218.89 175.341 2 4 12 -2 493.476 216.910 2 -4 -12 1 400.682 150.277 2 4 12 0 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19239.4 675.171 2 -8 -5 -3 10065.7 488.835 2 -8 -5 -4 166.367 235.709 2 -8 -5 -5 19786.0 240.792 2 -8 -5 -6 755.813 196.617 2 -8 -5 -7 6708.93 296.075 2 -8 -5 -8 1711.70 245.899 2 8 5 9 9141.74 288.252 2 8 5 10 47.6613 206.690 2 8 5 11 5765.29 266.889 2 -8 -5 -12 742.162 195.620 2 -8 -5 -13 315.008 144.469 2 8 6 -9 3361.52 155.062 2 -8 -6 8 3398.16 169.213 2 -8 -6 7 2605.86 227.125 2 8 6 -6 1365.01 339.930 2 8 6 -5 824.654 262.601 2 8 6 -4 22.7405 285.282 2 8 6 -3 279.798 514.561 2 8 6 -2 857.638 306.095 2 8 6 -1 5495.97 1403.92 2 8 6 0 17460.5 1757.00 2 -8 -6 -1 2112.77 530.413 2 -8 -6 -2 6534.13 825.118 2 -8 -6 -3 4695.30 865.056 2 -8 -6 -4 14580.5 1072.05 2 -8 -6 -5 461.786 498.461 2 -8 -6 -6 931.496 312.570 2 -8 -6 -7 82.4223 294.189 2 -8 -6 -8 2540.80 224.572 2 8 6 9 118.765 219.113 2 8 6 10 563.350 220.069 2 -8 -6 -11 1619.09 202.798 2 -8 -6 -12 447.495 159.080 2 -8 -6 -13 3108.86 171.026 2 8 7 -8 387.358 271.342 2 8 7 -7 8526.62 199.350 2 8 7 -6 987.113 239.994 2 -8 -7 5 219.889 282.749 2 -8 -7 -11 1232.46 201.278 2 -8 -7 -12 324.747 154.973 2 -8 -7 -13 4372.91 181.290 2 8 8 -6 489.959 330.647 2 8 11 -3 636.155 273.363 2 8 11 12 383.034 180.270 2 8 12 10-55.3918 211.378 2 8 13 2 539.388 345.932 2 8 13 3 3841.21 380.862 2 -9 3 -1 874.863 338.884 2 9 -2 -11 3525.02 253.961 2 9 -2 -10 4714.12 200.817 2 9 -2 -9 6947.78 154.889 2 -9 2 8 932.703 343.109 2 -9 2 -1 1149.15 637.169 2 -9 2 -5 3727.22 190.190 2 9 -2 6 326.242 113.071 2 9 -2 7 316.672 100.952 2 9 -1 -11 1822.11 262.201 2 9 -1 -10 478.615 156.766 2 9 -1 -9 251.572 173.336 2 9 -1 -8 1063.11 184.548 2 -9 1 7 2209.81 189.487 2 -9 1 6 4899.67 204.023 2 9 -1 -5 4019.26 255.093 2 -9 1 4 23671.8 353.300 2 -9 1 3 2183.87 254.178 2 -9 1 2 22235.4 809.814 2 -9 1 1-73.5278 340.579 2 -9 1 0 5545.96 347.377 2 -9 1 -1 8553.80 334.338 2 -9 1 -2 7372.49 264.745 2 -9 1 -3 325.320 182.607 2 9 -1 4 6986.95 154.339 2 -9 1 -5 425.472 126.057 2 -9 1 -6 3020.41 120.599 2 9 -1 7 841.438 136.340 2 9 -1 8 179.186 116.226 2 9 0 -11 1894.86 128.515 2 9 0 -10 998.345 213.264 2 9 0 -9 2548.75 186.280 2 9 0 -8 27.7435 205.606 2 9 0 -7 124.968 214.720 2 9 0 -6 193.899 194.802 2 9 0 -5 13648.2 246.153 2 9 0 -4 4972.07 215.850 2 9 0 -3 21053.6 243.011 2 -9 0 2 17719.7 274.274 2 -9 0 1 3069.51 240.447 2 9 0 0 18894.8 234.535 2 9 0 1 7564.84 278.031 2 9 0 2 91.5723 171.639 2 9 0 3 9598.37 189.279 2 9 0 4 1424.83 149.533 2 -9 0 -5 1251.51 143.417 2 -9 0 -6 1148.60 147.338 2 -9 0 -7 2217.15 145.742 2 9 0 8 15.8715 141.257 2 9 0 9 1568.59 119.624 2 9 1 -11 194.699 216.265 2 9 1 -10 5280.08 381.752 2 9 1 -9 231.820 167.473 2 9 1 -8 1560.48 168.742 2 9 1 -7-16.5716 206.874 2 -9 -1 6 481.376 222.851 2 9 1 -5 1565.45 211.405 2 9 1 -4 2389.86 238.768 2 9 1 -3 16029.2 238.915 2 9 1 -2 2990.65 192.143 2 9 1 -1 10949.1 193.785 2 9 1 0 22775.9 231.241 2 9 1 1 4547.76 203.513 2 9 1 2 52076.5 364.883 2 9 1 3 14460.5 193.165 2 9 1 4 4904.27 176.403 2 9 1 5 5144.85 200.582 2 9 1 6 116.509 159.412 2 -9 -1 -7-27.7209 166.552 2 9 1 8 129.089 149.960 2 9 1 9 1564.34 155.337 2 9 1 10 283.649 105.831 2 9 2 -10 617.439 152.355 2 9 2 -9 261.843 287.290 2 9 2 -8 96.5822 192.363 2 9 2 -7 827.321 246.682 2 9 2 -6 59.0539 212.710 2 9 2 -5 4552.34 264.758 2 9 2 -4 3837.14 268.342 2 9 2 -3 283.455 212.037 2 9 2 -2 271.559 215.761 2 9 2 -1 11119.0 208.273 2 9 2 0 13532.9 233.923 2 9 2 1 8466.33 206.104 2 9 2 2 31516.9 319.471 2 9 2 3 1620.90 192.787 2 -9 -2 -4 17506.6 243.021 2 -9 -2 -5 3052.18 193.023 2 9 2 6 2799.28 229.874 2 9 2 7 1364.44 215.800 2 -9 -2 -8 313.250 180.076 2 -9 -2 -9 228.581 138.782 2 9 2 10 865.215 149.897 2 9 2 11 448.007 138.866 2 9 3 -10 22.7981 253.535 2 9 3 -9 192.916 174.778 2 9 3 -8 437.108 232.205 2 9 3 -7 808.146 247.339 2 9 3 -6 3302.02 268.513 2 9 3 -5 6324.02 337.003 2 9 3 -4 1256.72 274.688 2 9 3 -3 14443.5 323.289 2 9 3 -2 2003.24 244.830 2 -9 -3 1 998.601 308.082 2 -9 -3 0 522.296 296.828 2 9 3 1 24683.1 524.850 2 9 3 2 1726.01 333.005 2 9 3 3 57350.3 561.525 2 -9 -3 -4 17507.8 296.941 2 -9 -3 -5 2730.61 207.966 2 -9 -3 -6 8767.34 285.867 2 9 3 7 2443.48 229.745 2 9 3 8 2880.13 226.228 2 9 3 9 1871.48 195.754 2 9 3 10 100.181 168.805 2 9 3 11 309.796 128.859 2 9 4 -9 119.438 207.212 2 9 4 -8 309.279 166.263 2 9 4 -7 972.350 190.556 2 -9 -4 6 361.232 231.001 2 -9 -4 5 761.386 395.237 2 9 4 -4 2285.86 391.449 2 9 4 -3 1356.77 551.957 2 -9 -4 1 1926.28 601.469 2 9 4 0 12596.6 1700.75 2 9 4 1 4416.37 385.182 2 9 4 2 169.847 497.192 2 -9 -4 -3 15165.4 702.471 2 -9 -4 -4 6123.12 552.117 2 -9 -4 -5 4262.22 349.674 2 -9 -4 -6 7912.42 362.510 2 9 4 7-97.0211 262.021 2 9 4 8 13351.7 307.370 2 9 4 9 4801.30 212.809 2 9 4 10 4415.01 177.876 2 9 4 11 2112.79 152.313 2 9 4 12 212.415 175.598 2 9 5 -8 732.738 235.191 2 9 5 -7 881.891 294.366 2 -9 -5 6 780.720 353.677 2 -9 -5 -8 13372.6 823.002 2 9 5 9 304.745 394.199 2 9 5 10 12262.3 214.816 2 9 5 11 1377.76 159.746 2 9 5 12 1283.09 207.341 2 9 9 12 1753.84 194.514 2 9 10 -4 3224.52 273.021 2 9 10 -3 81.9693 321.417 2 9 10 10 2131.92 296.881 2 9 10 11 500.529 224.364 2 9 11 -2 428.811 281.882 2 9 11 -1 300.315 273.337 2 9 11 0 1011.69 399.072 2 9 11 1 126.196 486.435 2 9 11 9 212.826 225.675 2 9 11 10 1443.78 196.804 2 9 12 1 104.120 253.457 2 9 12 2 587.669 387.547 2 9 12 8 753.651 314.321 2 9 12 9 190.611 310.969 2 10 -3 -8 4438.52 151.189 2 -10 3 7 5165.33 171.440 2 10 -3 -6 233.541 335.190 2 10 -3 2 471.139 241.209 2 -10 3 -3 286.411 173.653 2 10 -3 4 639.365 136.795 2 10 -2 -9 1512.14 158.561 2 10 -2 -8 5979.59 173.748 2 -10 2 7 2277.67 151.863 2 10 -2 -6 1143.24 142.712 2 10 -2 -5 3159.12 176.327 2 10 -2 -4 3443.44 213.071 2 -10 2 3 80.8083 230.398 2 -10 2 2 817.941 233.448 2 -10 2 1 8.85722 193.434 2 10 -2 0 955.743 194.925 2 10 -2 1 295.925 187.556 2 10 -2 2 421.480 155.230 2 10 -2 3 492.512 151.359 2 10 -2 4 723.585 163.285 2 -10 2 -5-6.40779 147.895 2 10 -1 -9 2148.93 171.409 2 10 -1 -8 4903.52 156.032 2 10 -1 -7 246.834 160.878 2 -10 1 6 3683.46 164.179 2 -10 1 5 9302.40 204.987 2 10 -1 -4 325.376 165.501 2 10 -1 -3 13426.1 247.995 2 10 -1 -2 812.604 191.848 2 10 -1 -1 1046.92 174.733 2 -10 1 0 1418.87 199.445 2 10 -1 1 116.108 196.596 2 10 -1 2 7223.00 180.041 2 10 -1 3 119.508 132.511 2 10 -1 4 958.145 143.545 2 10 -1 5-125.724 147.518 2 10 -1 6 524.594 139.089 2 -10 1 -7 96.4915 196.070 2 10 0 -9 2190.34 154.217 2 10 0 -8 31.6816 155.128 2 10 0 -7-117.440 154.900 2 10 0 -6 6755.10 200.030 2 10 0 -5 3378.68 193.892 2 10 0 -4 15602.6 277.385 2 10 0 -3 14273.5 248.140 2 10 0 -2 3342.66 225.416 2 10 0 -1 6902.43 233.418 2 10 0 0 33.3656 191.234 2 10 0 1 5511.81 208.700 2 10 0 2 644.206 178.893 2 -10 0 -3 80.7687 163.212 2 10 0 4-44.2330 128.633 2 -10 0 -5-31.8254 141.576 2 10 0 6-30.8126 171.171 2 10 0 7 129.802 157.636 2 10 0 8 219.093 112.445 2 10 1 -9 274.679 183.466 2 10 1 -8 339.475 155.662 2 10 1 -7 1575.63 188.034 2 10 1 -6 4775.67 253.318 2 10 1 -5 592.193 200.833 2 10 1 -4 15106.6 252.353 2 10 1 -3 670.727 544.813 2 -10 -1 2 11569.7 422.333 2 -10 -1 1 8720.57 256.240 2 -10 -1 0 381.418 384.424 2 -10 -1 -1 3523.10 257.953 2 10 1 2 4026.77 284.685 2 10 1 3 353.957 278.999 2 10 1 4-36.2815 192.745 2 10 1 5 1084.67 187.056 2 -10 -1 -6 1136.76 194.085 2 10 1 7 329.233 192.601 2 10 1 8 2793.02 164.013 2 10 1 9 61.5347 137.796 2 10 2 -9 538.701 299.087 2 10 2 -8 2942.37 237.057 2 10 2 -7-132.173 176.738 2 10 2 -6 3323.11 241.213 2 10 2 -5 9647.33 302.328 2 10 2 -4 1515.49 504.255 2 -10 -2 0 8544.99 644.132 2 -10 -2 -3 16966.9 462.580 2 -10 -2 -4 217.194 236.805 2 10 2 5 1143.11 221.626 2 10 2 6 664.254 211.607 2 -10 -2 -7 85.6700 187.425 2 10 2 8 1240.46 240.795 2 10 2 9 269.016 143.649 2 10 3 -9 411.975 259.202 2 10 3 -8 2196.35 268.015 2 10 3 -7 29.7136 251.876 2 -10 -3 6 10103.0 436.450 2 -10 -3 -7 529.511 267.906 2 -10 -3 -8 302.978 241.500 2 10 3 9 42.2319 212.929 2 10 3 10-3.83729 150.731 2 10 7 -6 2372.72 332.433 2 10 8 -5 270.262 276.846 2 10 8 -4-198.462 388.115 2 10 8 10 297.084 251.128 2 10 9 -4 260.940 264.319 2 10 9 -3 1369.37 255.314 2 10 9 -2 707.847 256.562 2 10 9 -1 1909.71 508.346 2 10 9 9 5555.52 342.476 2 10 9 10 77.4229 239.540 2 10 10 -2 118.257 300.576 2 10 10 -1 2837.66 239.979 2 10 10 0 942.818 365.240 2 10 10 1 2460.80 566.574 2 10 10 6 3781.12 400.456 2 10 10 7 934.694 266.866 2 10 10 8 5604.76 344.845 2 10 10 9 416.907 254.486 2 10 10 10 263.943 204.332 2 10 11 0 229.923 198.632 2 10 11 1 729.893 225.957 2 10 11 2 749.687 340.820 2 10 11 5 1617.39 304.721 2 10 11 6 1046.45 294.341 2 10 11 7 1112.73 223.538 2 10 11 8 427.838 241.447 2 10 11 9 12.5070 199.539 2 10 12 3 705.143 309.729 2 10 12 4 3716.11 262.364 2 10 12 5 193.520 316.923 2 10 12 6 4615.20 327.339 2 11 -3 -5 1904.78 409.859 2 -11 3 4 226.941 184.959 2 11 -3 -3 577.538 201.129 2 11 -3 -2 456.633 249.278 2 11 -3 -1 553.188 236.122 2 11 -3 0 6664.55 228.956 2 11 -3 1 77.9001 284.638 2 11 -2 -6 182.850 282.818 2 -11 2 5 641.132 136.466 2 11 -2 -4 281.677 189.976 2 11 -2 -3 471.491 269.442 2 11 -2 -2 17.5894 265.858 2 11 -2 -1 480.417 205.571 2 11 -2 0 217.343 198.202 2 11 -2 1 1939.32 148.856 2 -11 2 -2 216.452 185.231 2 -11 2 -3 958.884 160.426 2 11 -1 -7 2595.85 178.173 2 11 -1 -6 229.039 192.976 2 -11 1 5 758.436 147.236 2 11 -1 -4 2968.94 426.111 2 11 -1 -3 309.471 271.825 2 11 -1 0 5377.33 572.849 2 11 -1 1 708.811 342.192 2 11 -1 2 247.875 179.686 2 11 -1 3 2977.55 164.581 2 -11 1 -4 439.338 182.544 2 -11 1 -5 1181.57 186.792 2 11 0 -7 1602.52 180.046 2 11 0 -6 522.325 161.428 2 11 0 -5 1753.41 227.126 2 11 0 2 1726.26 508.559 2 11 0 3 4091.00 319.547 2 11 0 4 942.904 260.977 2 11 0 5 120.388 213.499 2 11 0 6 1152.12 223.131 2 11 1 -7-220.903 281.597 2 11 1 -5 8221.05 579.867 2 11 1 4 525.746 426.847 2 11 1 6 26.0595 206.740 2 11 1 7 201.432 153.713 2 11 2 8 375.034 193.078 2 11 5 -6 1579.28 393.441 2 11 6 -6 741.040 272.874 2 11 6 -5 119.833 269.431 2 11 6 -3 7531.46 498.808 2 11 6 8 2268.18 310.973 2 11 6 9 241.834 248.847 2 11 7 -5 285.415 289.381 2 11 7 -4 46.2986 352.270 2 11 7 -3-309.339 322.311 2 11 7 -2 2336.40 667.363 2 11 7 8 4.26305 165.429 2 11 7 9 689.100 249.318 2 11 8 -3 1134.00 375.909 2 11 8 -2 2172.60 268.099 2 11 8 -1 470.686 357.264 2 11 8 0 7025.83 687.314 2 11 8 7 331.126 247.196 2 11 8 8 3671.97 225.573 2 11 8 9 19.0406 214.157 2 11 9 -1 4636.53 342.885 2 11 9 0 1224.78 347.643 2 11 9 4 387.170 363.262 2 11 9 5 7534.88 422.815 2 11 9 6 2094.04 341.622 2 11 9 7 2833.85 320.915 2 11 9 8 791.577 256.720 2 11 10 1 6289.39 350.821 2 11 10 2 1897.96 410.516 2 11 10 3 1014.26 483.016 2 11 10 4 2837.67 474.695 2 11 10 6 706.488 290.372 2 11 10 7 4810.48 284.486 2 11 10 8 3.85076 209.357 2 12 0 2 494.132 343.750 2 12 4 4 510.158 313.531 2 12 5 -4 1640.01 264.592 2 12 5 7 945.059 256.557 2 12 6 -3 170.820 266.191 2 12 6 -2 1037.36 297.589 2 12 6 -1 913.933 266.096 2 12 6 2 3873.30 461.666 2 12 6 5 937.618 365.036 2 12 6 6 1913.56 333.491 2 12 6 7 440.629 262.441 2 12 7 -3 235.999 296.445 2 12 7 -2 1471.61 276.597 2 12 7 -1 764.594 290.884 2 12 7 0 7783.05 387.496 2 12 7 1 834.204 357.847 2 12 7 3 724.208 497.330 2 12 7 4 1534.15 444.126 2 12 7 6 314.384 321.256 2 12 7 7 243.735 258.231 2 12 8 5 349.266 338.495 2 12 8 6-171.864 296.410 2 13 5 0 238.189 369.683 2 13 5 2 476.165 352.807 2 13 6 1 746.879 345.422 2 13 6 2 916.470 333.638 2 ; _shelx_hkl_checksum 86939 _olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+' _olex2_exptl_crystal_mounting_method 'The crystal was mounted on a MITIGEN holder in Paratone oil' _olex2_submission_original_sample_id LAB145 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 3.922 _oxdiff_exptl_absorpt_empirical_full_min 0.512 _oxdiff_twin_integration_method simultaneous _oxdiff_twin_items 2 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.71581(5) 0.64031(5) 0.67952(4) 0.03244(16) Uani 1 1 d . . . . . P1 P 0.65877(10) 0.72419(10) 0.81016(8) 0.0426(2) Uani 1 1 d . . . . . P2 P 0.49086(10) 0.69403(10) 0.65308(8) 0.0422(2) Uani 1 1 d . . . . . P3 P 0.73968(10) 0.42479(10) 0.77013(8) 0.0423(2) Uani 1 1 d . . . . . P4 P 0.93779(10) 0.57208(10) 0.72745(8) 0.0402(2) Uani 1 1 d . . . . . N1 N 0.8503(4) 0.7988(4) 0.4663(3) 0.0453(8) Uani 1 1 d D . . . . H1 H 0.902(4) 0.809(4) 0.506(3) 0.041(12) Uiso 1 1 d D . . . . N2 N 0.6529(4) 0.7638(4) 0.4168(3) 0.0445(8) Uani 1 1 d D . . . . H2 H 0.597(3) 0.724(4) 0.432(3) 0.031(10) Uiso 1 1 d D . . . . C00K C 0.9605(5) 0.9371(5) 0.3238(4) 0.0575(11) Uani 1 1 d . . . . . H00K H 1.016947 0.936545 0.377258 0.069 Uiso 1 1 calc R U . . . C2 C 0.8651(4) 0.8716(4) 0.3567(3) 0.0452(9) Uani 1 1 d . . . . . C3 C 0.7773(4) 0.8767(4) 0.2744(3) 0.0418(8) Uani 1 1 d . . . . . C4 C 0.6735(4) 0.8185(4) 0.3064(3) 0.0429(9) Uani 1 1 d . . . . . C5 C 0.5930(5) 0.8176(4) 0.2251(3) 0.0519(10) Uani 1 1 d . . . . . H5 H 0.524959 0.776628 0.245708 0.062 Uiso 1 1 calc R U . . . C6 C 0.6143(5) 0.8775(5) 0.1138(4) 0.0585(12) Uani 1 1 d . . . . . H6 H 0.560782 0.875152 0.059900 0.070 Uiso 1 1 calc R U . . . C7 C 0.7103(6) 0.9392(5) 0.0810(3) 0.0632(14) Uani 1 1 d . . . . . H7 H 0.720881 0.980165 0.005071 0.076 Uiso 1 1 calc R U . . . C8 C 0.7948(5) 0.9428(4) 0.1594(4) 0.0529(11) Uani 1 1 d . . . . . C9 C 0.8930(6) 1.0073(5) 0.1305(4) 0.0659(15) Uani 1 1 d . . . . . H9 H 0.904021 1.052942 0.055436 0.079 Uiso 1 1 calc R U . . . C10 C 0.9738(6) 1.0049(5) 0.2105(5) 0.0686(15) Uani 1 1 d . . . . . H10 H 1.039201 1.049166 0.189258 0.082 Uiso 1 1 calc R U . . . C11 C 0.4743(5) 0.7833(5) 0.8211(4) 0.0560(11) Uani 1 1 d . . . . . H11A H 0.454441 0.769535 0.898273 0.067 Uiso 1 1 calc R U . . . H11B H 0.438026 0.879694 0.776451 0.067 Uiso 1 1 calc R U . . . C12 C 0.4081(4) 0.7060(5) 0.7805(4) 0.0528(10) Uani 1 1 d . . . . . H12A H 0.310918 0.753360 0.764135 0.063 Uiso 1 1 calc R U . . . H12B H 0.420674 0.616033 0.837019 0.063 Uiso 1 1 calc R U . . . C13 C 0.6954(6) 0.8794(6) 0.7911(5) 0.0736(15) Uani 1 1 d . . . . . H13A H 0.792362 0.860265 0.798837 0.110 Uiso 1 1 calc R U . . . H13B H 0.652106 0.913694 0.846518 0.110 Uiso 1 1 calc R U . . . H13C H 0.661173 0.945964 0.717904 0.110 Uiso 1 1 calc R U . . . C14 C 0.7154(6) 0.6286(6) 0.9574(4) 0.0733(16) Uani 1 1 d . . . . . H14A H 0.684299 0.550635 0.985314 0.110 Uiso 1 1 calc R U . . . H14B H 0.678282 0.685321 0.999059 0.110 Uiso 1 1 calc R U . . . H14C H 0.813302 0.599438 0.965188 0.110 Uiso 1 1 calc R U . . . C15 C 0.4017(5) 0.5966(6) 0.6178(5) 0.0685(14) Uani 1 1 d . . . . . H15A H 0.433047 0.586249 0.549286 0.103 Uiso 1 1 calc R U . . . H15B H 0.305215 0.643593 0.608724 0.103 Uiso 1 1 calc R U . . . H15C H 0.419747 0.508675 0.676696 0.103 Uiso 1 1 calc R U . . . C16 C 0.3960(5) 0.8632(5) 0.5551(4) 0.0686(14) Uani 1 1 d . . . . . H16A H 0.422430 0.930063 0.570172 0.103 Uiso 1 1 calc R U . . . H16B H 0.299915 0.878707 0.563612 0.103 Uiso 1 1 calc R U . . . H16C H 0.415900 0.869763 0.480060 0.103 Uiso 1 1 calc R U . . . C17 C 0.9104(5) 0.3252(5) 0.8391(5) 0.0726(16) Uani 1 1 d . . . . . H17A H 0.902583 0.259495 0.911934 0.087 Uiso 1 1 calc R U . . . H17B H 0.963480 0.275836 0.794928 0.087 Uiso 1 1 calc R U . . . C18 C 0.9822(5) 0.4155(5) 0.8527(4) 0.0548(11) Uani 1 1 d . . . . . H18A H 1.080246 0.371052 0.861068 0.066 Uiso 1 1 calc R U . . . H18B H 0.953689 0.435913 0.918609 0.066 Uiso 1 1 calc R U . . . C19 C 0.7315(5) 0.3283(5) 0.6861(4) 0.0642(12) Uani 1 1 d . . . . . H19A H 0.639759 0.356972 0.655202 0.096 Uiso 1 1 calc R U . . . H19B H 0.758446 0.233238 0.732204 0.096 Uiso 1 1 calc R U . . . H19C H 0.791991 0.343767 0.626495 0.096 Uiso 1 1 calc R U . . . C20 C 0.6351(6) 0.3568(5) 0.8809(4) 0.0631(12) Uani 1 1 d . . . . . H20A H 0.638758 0.387798 0.940039 0.095 Uiso 1 1 calc R U . . . H20B H 0.668881 0.259390 0.909425 0.095 Uiso 1 1 calc R U . . . H20C H 0.542274 0.387438 0.851670 0.095 Uiso 1 1 calc R U . . . C21 C 1.0302(5) 0.6660(5) 0.7644(5) 0.0667(13) Uani 1 1 d . . . . . H21A H 1.015654 0.753183 0.705082 0.100 Uiso 1 1 calc R U . . . H21B H 1.125991 0.616120 0.775473 0.100 Uiso 1 1 calc R U . . . H21C H 0.997538 0.678108 0.832001 0.100 Uiso 1 1 calc R U . . . C22 C 1.0586(4) 0.5110(5) 0.6353(4) 0.0567(11) Uani 1 1 d . . . . . H22A H 1.029614 0.448761 0.615333 0.085 Uiso 1 1 calc R U . . . H22B H 1.147688 0.465477 0.673240 0.085 Uiso 1 1 calc R U . . . H22C H 1.061932 0.586522 0.568923 0.085 Uiso 1 1 calc R U . . . B1 B 0.7429(4) 0.7405(4) 0.5102(3) 0.0377(9) Uani 1 1 d . . . . . H1A H 0.761(4) 0.610(4) 0.577(3) 0.044(11) Uiso 1 1 d . . . . . H1B H 0.693(4) 0.792(4) 0.593(3) 0.036(10) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0305(3) 0.0328(3) 0.0319(3) -0.0119(2) 0.0033(2) -0.0078(2) P1 0.0426(5) 0.0436(5) 0.0414(5) -0.0209(4) 0.0045(4) -0.0077(4) P2 0.0323(5) 0.0473(5) 0.0423(5) -0.0141(4) 0.0038(4) -0.0101(4) P3 0.0402(5) 0.0358(5) 0.0456(5) -0.0112(4) 0.0040(4) -0.0107(4) P4 0.0334(5) 0.0428(5) 0.0455(5) -0.0198(4) 0.0008(4) -0.0094(4) N1 0.0400(19) 0.0517(19) 0.0456(17) -0.0148(15) 0.0024(14) -0.0207(16) N2 0.0391(19) 0.057(2) 0.0396(16) -0.0129(14) 0.0061(13) -0.0258(16) C00K 0.055(3) 0.050(2) 0.075(3) -0.025(2) 0.019(2) -0.027(2) C2 0.043(2) 0.0372(19) 0.053(2) -0.0180(16) 0.0143(17) -0.0095(17) C3 0.044(2) 0.0307(17) 0.0424(18) -0.0123(14) 0.0081(16) -0.0034(15) C4 0.044(2) 0.0370(19) 0.0373(17) -0.0131(15) -0.0012(15) -0.0001(16) C5 0.054(3) 0.052(2) 0.044(2) -0.0187(18) -0.0032(18) -0.008(2) C6 0.073(3) 0.047(2) 0.044(2) -0.0180(18) -0.008(2) 0.000(2) C7 0.086(4) 0.046(2) 0.0363(19) -0.0117(17) 0.003(2) 0.003(2) C8 0.060(3) 0.0327(19) 0.052(2) -0.0122(17) 0.020(2) -0.0042(18) C9 0.084(4) 0.042(2) 0.059(3) -0.012(2) 0.030(3) -0.015(2) C10 0.067(3) 0.045(2) 0.092(4) -0.022(2) 0.039(3) -0.027(2) C11 0.048(2) 0.063(3) 0.058(2) -0.032(2) 0.0151(19) -0.008(2) C12 0.037(2) 0.061(3) 0.058(2) -0.024(2) 0.0146(17) -0.0126(19) C13 0.075(4) 0.071(3) 0.103(4) -0.059(3) 0.023(3) -0.032(3) C14 0.083(4) 0.081(3) 0.044(2) -0.033(2) -0.005(2) 0.004(3) C15 0.046(3) 0.094(4) 0.084(3) -0.045(3) 0.005(2) -0.033(3) C16 0.044(3) 0.066(3) 0.064(3) -0.006(2) 0.002(2) 0.002(2) C17 0.051(3) 0.044(2) 0.097(4) 0.000(2) -0.013(3) -0.009(2) C18 0.045(2) 0.056(3) 0.050(2) -0.0127(19) -0.0098(17) -0.004(2) C19 0.074(3) 0.050(2) 0.078(3) -0.033(2) 0.015(3) -0.022(2) C20 0.075(3) 0.051(2) 0.056(2) -0.008(2) 0.017(2) -0.028(2) C21 0.046(3) 0.070(3) 0.103(4) -0.049(3) -0.005(3) -0.021(2) C22 0.038(2) 0.065(3) 0.065(3) -0.032(2) 0.0087(18) -0.005(2) B1 0.032(2) 0.041(2) 0.0407(19) -0.0144(16) 0.0061(15) -0.0141(17) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.0197 -5 -6 -3 0.0824 1 -6 -5 0.0765 0 0 -1 0.0263 -2 6 5 0.0889 6 5 3 0.0939 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Mn1 P2 83.21(4) . . ? P1 Mn1 P4 92.81(4) . . ? P1 Mn1 H1A 168.3(16) . . ? P1 Mn1 H1B 87.6(14) . . ? P2 Mn1 P4 173.06(4) . . ? P2 Mn1 H1A 99.6(16) . . ? P2 Mn1 H1B 84.0(14) . . ? P3 Mn1 P1 102.68(4) . . ? P3 Mn1 P2 92.40(4) . . ? P3 Mn1 P4 82.90(4) . . ? P3 Mn1 H1A 88.6(16) . . ? P3 Mn1 H1B 168.7(14) . . ? P4 Mn1 H1A 85.5(16) . . ? P4 Mn1 H1B 101.5(14) . . ? H1A Mn1 H1B 81(2) . . ? C11 P1 Mn1 112.88(15) . . ? C13 P1 Mn1 117.72(18) . . ? C13 P1 C11 98.9(3) . . ? C13 P1 C14 99.2(3) . . ? C14 P1 Mn1 123.83(16) . . ? C14 P1 C11 100.3(2) . . ? C12 P2 Mn1 109.64(15) . . ? C15 P2 Mn1 126.28(18) . . ? C15 P2 C12 100.8(2) . . ? C15 P2 C16 98.7(3) . . ? C16 P2 Mn1 118.70(18) . . ? C16 P2 C12 98.0(2) . . ? C17 P3 Mn1 113.16(17) . . ? C19 P3 Mn1 116.62(17) . . ? C19 P3 C17 99.0(3) . . ? C20 P3 Mn1 125.63(17) . . ? C20 P3 C17 100.1(3) . . ? C20 P3 C19 97.9(2) . . ? C18 P4 Mn1 109.99(16) . . ? C21 P4 Mn1 126.90(17) . . ? C21 P4 C18 99.8(2) . . ? C21 P4 C22 99.0(2) . . ? C22 P4 Mn1 118.01(16) . . ? C22 P4 C18 98.3(2) . . ? C2 N1 H1 108(3) . . ? C2 N1 B1 127.2(4) . . ? B1 N1 H1 123(3) . . ? C4 N2 H2 116(3) . . ? C4 N2 B1 126.2(3) . . ? B1 N2 H2 116(3) . . ? C2 C00K H00K 119.8 . . ? C2 C00K C10 120.3(5) . . ? C10 C00K H00K 119.8 . . ? N1 C2 C3 117.6(4) . . ? C00K C2 N1 123.2(4) . . ? C00K C2 C3 119.1(4) . . ? C2 C3 C8 119.8(4) . . ? C4 C3 C2 120.0(3) . . ? C4 C3 C8 120.2(4) . . ? N2 C4 C3 119.2(4) . . ? N2 C4 C5 121.4(4) . . ? C5 C4 C3 119.5(4) . . ? C4 C5 H5 120.1 . . ? C6 C5 C4 119.8(5) . . ? C6 C5 H5 120.1 . . ? C5 C6 H6 119.2 . . ? C7 C6 C5 121.7(5) . . ? C7 C6 H6 119.2 . . ? C6 C7 H7 119.5 . . ? C6 C7 C8 121.0(4) . . ? C8 C7 H7 119.5 . . ? C7 C8 C3 117.8(4) . . ? C9 C8 C3 118.8(5) . . ? C9 C8 C7 123.5(4) . . ? C8 C9 H9 119.6 . . ? C10 C9 C8 120.7(4) . . ? C10 C9 H9 119.6 . . ? C00K C10 H10 119.4 . . ? C9 C10 C00K 121.2(5) . . ? C9 C10 H10 119.4 . . ? P1 C11 H11A 109.8 . . ? P1 C11 H11B 109.8 . . ? H11A C11 H11B 108.2 . . ? C12 C11 P1 109.5(3) . . ? C12 C11 H11A 109.8 . . ? C12 C11 H11B 109.8 . . ? P2 C12 H12A 110.4 . . ? P2 C12 H12B 110.4 . . ? C11 C12 P2 106.8(3) . . ? C11 C12 H12A 110.4 . . ? C11 C12 H12B 110.4 . . ? H12A C12 H12B 108.6 . . ? P1 C13 H13A 109.5 . . ? P1 C13 H13B 109.5 . . ? P1 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? P1 C14 H14A 109.5 . . ? P1 C14 H14B 109.5 . . ? P1 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? P2 C15 H15A 109.5 . . ? P2 C15 H15B 109.5 . . ? P2 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? P2 C16 H16A 109.5 . . ? P2 C16 H16B 109.5 . . ? P2 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? P3 C17 H17A 109.5 . . ? P3 C17 H17B 109.5 . . ? H17A C17 H17B 108.1 . . ? C18 C17 P3 110.8(3) . . ? C18 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? P4 C18 H18A 110.2 . . ? P4 C18 H18B 110.2 . . ? C17 C18 P4 107.7(3) . . ? C17 C18 H18A 110.2 . . ? C17 C18 H18B 110.2 . . ? H18A C18 H18B 108.5 . . ? P3 C19 H19A 109.5 . . ? P3 C19 H19B 109.5 . . ? P3 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? P3 C20 H20A 109.5 . . ? P3 C20 H20B 109.5 . . ? P3 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? P4 C21 H21A 109.5 . . ? P4 C21 H21B 109.5 . . ? P4 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? P4 C22 H22A 109.5 . . ? P4 C22 H22B 109.5 . . ? P4 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N1 B1 N2 108.9(3) . . ? N1 B1 H1A 125.8(18) . . ? N1 B1 H1B 103.8(17) . . ? N2 B1 H1A 103.3(18) . . ? N2 B1 H1B 120.9(16) . . ? H1A B1 H1B 95(2) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 P1 2.2171(10) . ? Mn1 P2 2.2485(11) . ? Mn1 P3 2.2116(11) . ? Mn1 P4 2.2487(11) . ? Mn1 H1A 1.52(4) . ? Mn1 H1B 1.61(4) . ? P1 C11 1.845(5) . ? P1 C13 1.839(5) . ? P1 C14 1.842(5) . ? P2 C12 1.859(4) . ? P2 C15 1.842(5) . ? P2 C16 1.844(5) . ? P3 C17 1.853(5) . ? P3 C19 1.842(5) . ? P3 C20 1.837(4) . ? P4 C18 1.850(4) . ? P4 C21 1.843(5) . ? P4 C22 1.846(4) . ? N1 H1 0.83(2) . ? N1 C2 1.384(5) . ? N1 B1 1.459(5) . ? N2 H2 0.81(2) . ? N2 C4 1.373(5) . ? N2 B1 1.481(5) . ? C00K H00K 0.9400 . ? C00K C2 1.379(6) . ? C00K C10 1.410(7) . ? C2 C3 1.432(6) . ? C3 C4 1.404(6) . ? C3 C8 1.434(5) . ? C4 C5 1.403(6) . ? C5 H5 0.9400 . ? C5 C6 1.392(6) . ? C6 H6 0.9400 . ? C6 C7 1.357(8) . ? C7 H7 0.9400 . ? C7 C8 1.416(7) . ? C8 C9 1.396(8) . ? C9 H9 0.9400 . ? C9 C10 1.373(8) . ? C10 H10 0.9400 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 C12 1.521(7) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 C18 1.511(7) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? B1 H1A 1.36(4) . ? B1 H1B 1.41(4) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Mn1 P1 C11 C12 26.5(4) . . . . ? Mn1 P2 C12 C11 44.0(3) . . . . ? Mn1 P3 C17 C18 19.3(5) . . . . ? Mn1 P4 C18 C17 42.9(4) . . . . ? P1 C11 C12 P2 -42.6(4) . . . . ? P3 C17 C18 P4 -37.6(5) . . . . ? N1 C2 C3 C4 5.1(5) . . . . ? N1 C2 C3 C8 -175.6(3) . . . . ? N2 C4 C5 C6 178.1(4) . . . . ? C00K C2 C3 C4 -175.7(4) . . . . ? C00K C2 C3 C8 3.6(6) . . . . ? C2 N1 B1 N2 3.6(6) . . . . ? C2 C00K C10 C9 -0.1(7) . . . . ? C2 C3 C4 N2 3.6(5) . . . . ? C2 C3 C4 C5 -176.5(4) . . . . ? C2 C3 C8 C7 176.7(4) . . . . ? C2 C3 C8 C9 -3.5(6) . . . . ? C3 C4 C5 C6 -1.8(6) . . . . ? C3 C8 C9 C10 1.6(7) . . . . ? C4 N2 B1 N1 6.2(6) . . . . ? C4 C3 C8 C7 -4.0(6) . . . . ? C4 C3 C8 C9 175.8(4) . . . . ? C4 C5 C6 C7 -1.0(7) . . . . ? C5 C6 C7 C8 1.2(7) . . . . ? C6 C7 C8 C3 1.3(6) . . . . ? C6 C7 C8 C9 -178.5(4) . . . . ? C7 C8 C9 C10 -178.6(4) . . . . ? C8 C3 C4 N2 -175.6(4) . . . . ? C8 C3 C4 C5 4.3(6) . . . . ? C8 C9 C10 C00K 0.2(7) . . . . ? C10 C00K C2 N1 177.4(4) . . . . ? C10 C00K C2 C3 -1.8(6) . . . . ? C13 P1 C11 C12 151.7(4) . . . . ? C14 P1 C11 C12 -107.2(4) . . . . ? C15 P2 C12 C11 179.0(3) . . . . ? C16 P2 C12 C11 -80.5(4) . . . . ? C19 P3 C17 C18 143.4(4) . . . . ? C20 P3 C17 C18 -116.8(4) . . . . ? C21 P4 C18 C17 178.2(4) . . . . ? C22 P4 C18 C17 -81.1(4) . . . . ? B1 N1 C2 C00K 171.8(4) . . . . ? B1 N1 C2 C3 -9.0(6) . . . . ? B1 N2 C4 C3 -9.9(6) . . . . ? B1 N2 C4 C5 170.3(4) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined _oxdiff_twin_reflns_isolated _oxdiff_twin_reflns_overlapped _twin_individual_twin_lattice_type _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 1 0.4830(12) 27118 24940 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 2 0.5170(12) 26999 24940 nmt -0.9996 -0.0024 0.0015 0.0019 -0.9994 -0.0017 0.1566 -0.9195 0.9991 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0.0011 -0.0021 0.9995 0.1252 0.0232 -0.0079 -5.2936 -6.0938 -3.3564 -0.0075 -0.3068 0.9517 1.3495 -6.2001 -4.6585 -0.0254 -0.9864 0.1624 -0.0011 0.0021 -0.9995 -0.1252 -0.0232 0.0079 -1.8754 5.8881 4.5337 0.0257 0.9962 -0.0832 6.0243 5.2198 2.5999 0.0025 0.1137 -0.9935