#------------------------------------------------------------------------------ #$Date: 2019-03-21 05:32:57 +0200 (Thu, 21 Mar 2019) $ #$Revision: 214247 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/10/83/2108386.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2108386 loop_ _publ_author_name 'Han, Yang' 'Fu, Qiang' 'Zhang, Peng' 'Guan, Hongyu' 'Guo, Fang' _publ_section_title ; Acid--ammonium heterodimer and N~(ammonium)~--H···N~(pyridine)~ synthon preference in three salts of nicotinic acid with (1R,2R)-1,2-diphenylethylenediamine ; _journal_coeditor_code AW5017SUP1 _journal_issue 2 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first ; ; _journal_paper_doi 10.1107/S2052520619000477 _journal_volume 75 _journal_year 2019 _chemical_absolute_configuration ad _chemical_formula_moiety '2(C6 H4 N O2), 2(C7 H9 N), C4 H8 O2' _chemical_formula_sum 'C30 H34 N4 O6' _chemical_formula_weight 546.61 _space_group_crystal_system monoclinic _space_group_IT_number 5 _space_group_name_Hall 'C 2y' _space_group_name_H-M_alt 'C 1 2 1' _symmetry_space_group_name_Hall 'C 2y' _symmetry_space_group_name_H-M 'C 1 2 1' _atom_sites_solution_hydrogens mixed _audit_creation_date 2018-11-06 _audit_creation_method ; Olex2 1.2-beta (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 118.613(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 22.9673(11) _cell_length_b 8.8676(4) _cell_length_c 16.7749(8) _cell_measurement_reflns_used 9833 _cell_measurement_temperature 273(2) _cell_measurement_theta_max 28.275 _cell_measurement_theta_min 3.091 _cell_volume 2999.2(3) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _diffrn_ambient_temperature 273.0 _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_device_type 'CCD area detector' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71076 _diffrn_reflns_av_R_equivalents 0.0225 _diffrn_reflns_av_unetI/netI 0.0217 _diffrn_reflns_Laue_measured_fraction_full 0.984 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 25955 _diffrn_reflns_point_group_measured_fraction_full 0.985 _diffrn_reflns_point_group_measured_fraction_max 0.986 _diffrn_reflns_theta_full 25.243 _diffrn_reflns_theta_max 28.333 _diffrn_reflns_theta_min 3.090 _exptl_absorpt_coefficient_mu 0.085 _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.211 _exptl_crystal_description needle _exptl_crystal_F_000 1160 _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.09 _refine_diff_density_max 0.552 _refine_diff_density_min -0.348 _refine_diff_density_rms 0.036 _refine_ls_abs_structure_details ; Flack x determined using 2721 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.27(18) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 387 _refine_ls_number_reflns 7385 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.060 _refine_ls_R_factor_all 0.0602 _refine_ls_R_factor_gt 0.0516 _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^)+(0.0861P)^2^+0.8946P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1426 _refine_ls_wR_factor_ref 0.1518 _reflns_Friedel_coverage 0.879 _reflns_Friedel_fraction_full 0.985 _reflns_Friedel_fraction_max 0.985 _reflns_number_gt 6427 _reflns_number_total 7385 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file aw5017sup1.cif _cod_data_source_block DPEN1-NA2-EA1 _cod_original_cell_volume 2999.2(2) _cod_database_code 2108386 _shelx_shelxl_version_number 2014/7 _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 0.992 _shelx_estimated_absorpt_t_min 0.981 _olex2_refinement_description ; 1. 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 2.a Ternary CH refined with riding coordinates: C14(H14), C7(H7) 2.b Secondary CH2 refined with riding coordinates: C28(H28A,H28B) 2.c Aromatic/amide H refined with riding coordinates: C25(H25), C5(H5), C19(H19), C15(H15), C12(H12), C17(H17), C1(H1), C23(H23), C4(H4), C21(H21), C8(H8), C11(H11), C16(H16), C22(H22), C3(H3), C10(H10), C2(H2), C9(H9) 2.d Idealised Me refined as rotating group: C30(H30A,H30B,H30C), C27(H27A,H27B,H27C) ; _shelx_res_file ; 20161216a_0m.res created by SHELXL-2014/7 TITL 20161216a_0m_a.res in C2 REM Old TITL 20161216A_0m in C2/n #15 REM SHELXT solution in C2 REM R1 0.157, Rweak 0.024, Alpha 0.007, Orientation as input REM Flack x = -0.209 ( 0.169 ) from Parsons' quotients REM Formula found by SHELXT: C27 N4 O7 CELL 0.71076 22.9673 8.8676 16.7749 90 118.613 90 ZERR 4 0.0011 0.0004 0.0008 0 0.002 0 LATT -7 SYMM -X,+Y,-Z SFAC C H N O UNIT 120 136 16 24 L.S. 20 PLAN 20 SIZE 0.23 0.17 0.09 TEMP -0.15 BOND $H list 4 fmap 2 acta REM REM REM WGHT 0.086100 0.894600 FVAR 0.91063 O4 4 0.548611 0.404116 0.182846 11.00000 0.06875 0.05916 = 0.05776 -0.01360 0.03333 -0.01762 O1 4 0.464068 0.522427 0.347316 11.00000 0.05284 0.07336 = 0.06008 -0.02158 0.02198 -0.00700 O3 4 0.594921 0.508635 0.105661 11.00000 0.07289 0.06924 = 0.05119 -0.01210 0.03783 -0.00822 O2 4 0.371760 0.593704 0.349383 11.00000 0.07025 0.08642 = 0.05651 -0.02238 0.03215 0.00707 N2 3 0.450817 0.294057 0.027230 11.00000 0.04133 0.04921 = 0.04284 0.00363 0.02939 0.00421 N1 3 0.552927 0.696960 0.478645 11.00000 0.04641 0.04977 = 0.04095 -0.00114 0.02751 -0.00215 N3 3 0.358855 0.312097 0.099449 11.00000 0.05129 0.07413 = 0.05054 -0.01308 0.03372 -0.00744 N4 3 0.628684 0.721260 0.384899 11.00000 0.06378 0.06019 = 0.05116 -0.00799 0.03726 -0.00833 C14 1 0.514760 0.838749 0.467037 11.00000 0.04252 0.04739 = 0.03296 0.00261 0.01833 0.00069 AFIX 13 H14 2 0.477909 0.841055 0.404800 11.00000 -1.20000 AFIX 0 C7 1 0.464900 0.147205 -0.004034 11.00000 0.03172 0.04854 = 0.03184 -0.00229 0.01739 -0.00033 AFIX 13 H7 2 0.432073 0.132302 -0.067914 11.00000 -1.20000 AFIX 0 C25 1 0.603512 0.619358 0.318608 11.00000 0.05102 0.04710 = 0.05106 0.00012 0.03187 -0.00504 AFIX 43 H25 2 0.575255 0.546389 0.320871 11.00000 -1.20000 AFIX 0 C20 1 0.402449 0.526640 0.314963 11.00000 0.05494 0.04439 = 0.04438 -0.00411 0.02632 0.00019 C6 1 0.459642 0.017183 0.050894 11.00000 0.03441 0.04614 = 0.04183 -0.00014 0.02260 0.00023 C24 1 0.616968 0.615600 0.246254 11.00000 0.04128 0.04103 = 0.04125 0.00201 0.02192 0.00327 C5 1 0.488196 0.026346 0.144902 11.00000 0.06312 0.05239 = 0.04201 0.00324 0.02876 -0.00075 AFIX 43 H5 2 0.509188 0.114767 0.174548 11.00000 -1.20000 AFIX 0 C19 1 0.391823 0.382211 0.179569 11.00000 0.04047 0.05727 = 0.04894 -0.00742 0.02755 -0.00424 AFIX 43 H19 2 0.437775 0.387592 0.205829 11.00000 -1.20000 AFIX 0 O5 4 0.247090 0.876750 0.253824 11.00000 0.08090 0.10757 = 0.06994 -0.01945 0.02715 -0.00417 C18 1 0.362052 0.447076 0.225775 11.00000 0.04408 0.04819 = 0.04491 -0.00219 0.02598 -0.00127 C26 1 0.584089 0.499684 0.172098 11.00000 0.04582 0.04808 = 0.04436 -0.00286 0.02251 0.00350 C13 1 0.557167 0.977208 0.480897 11.00000 0.05159 0.04904 = 0.04690 0.00456 0.02817 0.00024 C15 1 0.293478 0.305466 0.063234 11.00000 0.05616 0.09824 = 0.04897 -0.02046 0.02702 -0.01601 AFIX 43 H15 2 0.269671 0.255700 0.008093 11.00000 -1.20000 AFIX 0 C12 1 0.531893 1.099065 0.422513 11.00000 0.06344 0.06171 = 0.07258 0.01790 0.03245 0.00585 AFIX 43 H12 2 0.489481 1.094474 0.373045 11.00000 -1.20000 AFIX 0 C17 1 0.293604 0.439876 0.185663 11.00000 0.04880 0.09169 = 0.06551 -0.01731 0.03702 -0.00006 AFIX 43 H17 2 0.271249 0.482515 0.213941 11.00000 -1.20000 AFIX 0 C1 1 0.428903 -0.115239 0.008295 11.00000 0.04714 0.06151 = 0.06159 -0.01221 0.02843 -0.01158 AFIX 43 H1 2 0.409565 -0.122730 -0.054561 11.00000 -1.20000 AFIX 0 O6 4 0.184497 0.671916 0.195203 11.00000 0.07823 0.10969 = 0.14231 -0.04908 0.01958 0.00760 C23 1 0.659078 0.724099 0.244133 11.00000 0.06198 0.05168 = 0.05461 0.00316 0.04007 -0.00008 AFIX 43 H23 2 0.669240 0.726127 0.196728 11.00000 -1.20000 AFIX 0 C4 1 0.485506 -0.095635 0.194571 11.00000 0.08336 0.06953 = 0.05846 0.01952 0.04250 0.01352 AFIX 43 H4 2 0.505156 -0.088975 0.257489 11.00000 -1.20000 AFIX 0 C21 1 0.669250 0.825477 0.381227 11.00000 0.07335 0.05366 = 0.06191 -0.01573 0.03982 -0.01444 AFIX 43 H21 2 0.686805 0.898029 0.426758 11.00000 -1.20000 AFIX 0 C8 1 0.620669 0.985859 0.553723 11.00000 0.05652 0.05740 = 0.06180 0.00500 0.01943 -0.00952 AFIX 43 H8 2 0.637983 0.904877 0.593500 11.00000 -1.20000 AFIX 0 C11 1 0.570003 1.227679 0.438083 11.00000 0.10254 0.05450 = 0.12717 0.03345 0.06119 0.00453 AFIX 43 H11 2 0.552874 1.309956 0.399319 11.00000 -1.20000 AFIX 0 C16 1 0.259136 0.368235 0.102909 11.00000 0.04095 0.12573 = 0.06818 -0.02168 0.02593 -0.00598 AFIX 43 H16 2 0.213098 0.362622 0.074379 11.00000 -1.20000 AFIX 0 C22 1 0.686205 0.830135 0.312923 11.00000 0.07835 0.05038 = 0.07604 -0.00891 0.05193 -0.01858 AFIX 43 H22 2 0.715317 0.903091 0.312986 11.00000 -1.20000 AFIX 0 C3 1 0.453961 -0.226754 0.151534 11.00000 0.07511 0.05443 = 0.09532 0.02074 0.05363 0.00743 AFIX 43 H3 2 0.451171 -0.307332 0.185031 11.00000 -1.20000 AFIX 0 C10 1 0.632294 1.234461 0.509666 11.00000 0.08993 0.06304 = 0.13963 0.00149 0.05042 -0.02432 AFIX 43 H10 2 0.657508 1.321382 0.519574 11.00000 -1.20000 AFIX 0 C2 1 0.426606 -0.237798 0.058694 11.00000 0.06254 0.04838 = 0.10832 -0.00805 0.04760 -0.01087 AFIX 43 H2 2 0.406542 -0.327236 0.029518 11.00000 -1.20000 AFIX 0 C9 1 0.658269 1.113837 0.567478 11.00000 0.06773 0.07591 = 0.09638 -0.00088 0.02219 -0.02173 AFIX 43 H9 2 0.701169 1.118587 0.615819 11.00000 -1.20000 AFIX 0 C29 1 0.210968 0.760135 0.257363 11.00000 0.05818 0.08104 = 0.10279 -0.02610 0.01522 0.01773 C30 1 0.208858 0.756222 0.342991 11.00000 0.12798 0.08061 = 0.13689 0.01393 0.07072 0.01245 AFIX 137 H30A 2 0.250583 0.720537 0.390452 11.00000 -1.50000 H30B 2 0.174063 0.689717 0.337212 11.00000 -1.50000 H30C 2 0.200540 0.855841 0.357587 11.00000 -1.50000 AFIX 0 C28 1 0.254015 0.890994 0.173501 11.00000 0.11094 0.24794 = 0.07886 -0.02271 0.04794 0.00906 AFIX 23 H28A 2 0.247214 0.793024 0.144655 11.00000 -1.20000 H28B 2 0.219861 0.958250 0.131245 11.00000 -1.20000 AFIX 0 C27 1 0.316339 0.946580 0.191445 11.00000 0.12656 0.22279 = 0.14059 0.05798 0.06724 -0.00633 AFIX 137 H27A 2 0.320224 0.942704 0.136992 11.00000 -1.50000 H27B 2 0.350539 0.886017 0.237540 11.00000 -1.50000 H27C 2 0.320882 1.049041 0.212077 11.00000 -1.50000 AFIX 0 H2A 2 0.435053 0.367813 -0.023927 11.00000 0.04598 H1A 2 0.576453 0.714381 0.455056 11.00000 0.05166 H1B 2 0.579105 0.660581 0.538416 11.00000 0.04187 H2B 2 0.419540 0.282297 0.042525 11.00000 0.05878 H1C 2 0.522663 0.621590 0.443942 11.00000 0.06102 H2C 2 0.490371 0.331128 0.084674 11.00000 0.07460 HKLF 4 REM 20161216a_0m_a.res in C2 REM R1 = 0.0516 for 6427 Fo > 4sig(Fo) and 0.0602 for all 7385 data REM 387 parameters refined using 1 restraints END WGHT 0.0861 0.8946 REM Highest difference peak 0.552, deepest hole -0.348, 1-sigma level 0.036 Q1 1 0.1929 0.7340 0.1312 11.00000 0.05 0.55 Q2 1 0.2638 1.0009 0.1704 11.00000 0.05 0.21 Q3 1 0.2191 0.8122 0.2012 11.00000 0.05 0.19 Q4 1 0.3807 0.4831 0.2683 11.00000 0.05 0.19 Q5 1 0.6057 0.5585 0.2157 11.00000 0.05 0.17 Q6 1 0.2786 0.3521 0.1554 11.00000 0.05 0.17 Q7 1 0.4540 0.0783 0.0206 11.00000 0.05 0.15 Q8 1 0.4149 -0.2323 0.1193 11.00000 0.05 0.14 Q9 1 0.5612 1.1465 0.4242 11.00000 0.05 0.14 Q10 1 0.4471 -0.1399 0.1655 11.00000 0.05 0.14 Q11 1 0.3756 0.4454 0.1966 11.00000 0.05 0.13 Q12 1 0.4578 0.2269 0.0117 11.00000 0.05 0.13 Q13 1 0.4044 -0.1479 0.0296 11.00000 0.05 0.12 Q14 1 0.6600 0.7451 0.3912 11.00000 0.05 0.12 Q15 1 0.5946 0.7701 0.4024 11.00000 0.05 0.12 Q16 1 0.4608 0.3941 0.0259 11.00000 0.05 0.12 Q17 1 0.2848 0.3766 0.0888 11.00000 0.05 0.12 Q18 1 0.1402 0.7737 0.2538 11.00000 0.05 0.12 Q19 1 0.4231 -0.0380 0.0283 11.00000 0.05 0.12 Q20 1 0.6269 0.5794 0.2942 11.00000 0.05 0.12 ; _shelx_res_checksum 4507 _shelx_hkl_file ; 4 0 0 242.33 5.46 -4 0 0 235.47 5.36 -4 0 0 248.88 5.47 -4 0 0 246.02 5.48 -4 0 0 252.27 5.51 -4 0 0 268.53 5.28 4 0 0 245.54 5.39 4 0 0 244.19 5.44 4 0 0 236.89 5.51 6 0 0 1354.06 27.30 -6 0 0 1314.14 27.08 -6 0 0 1269.61 27.39 6 0 0 1327.33 27.37 6 0 0 1275.69 27.37 6 0 0 1267.12 27.48 -6 0 0 1359.22 27.44 -6 0 0 1333.65 27.46 -8 0 0 288.42 6.36 8 0 0 280.64 6.57 8 0 0 282.02 6.78 8 0 0 280.80 6.95 -8 0 0 295.41 6.92 8 0 0 305.55 6.67 -8 0 0 283.83 6.87 -10 0 0 1685.74 35.37 -10 0 0 1649.84 34.68 -10 0 0 1715.86 35.32 10 0 0 1651.16 34.92 10 0 0 1728.99 35.04 10 0 0 1642.83 35.46 12 0 0 2126.98 44.79 12 0 0 2233.72 44.95 -12 0 0 2157.98 45.42 -12 0 0 2120.27 44.52 12 0 0 2151.79 45.54 14 0 0 433.11 10.05 14 0 0 427.21 9.87 14 0 0 438.48 11.75 -14 0 0 419.11 10.33 16 0 0 54.67 3.06 -16 0 0 52.55 3.63 16 0 0 44.45 4.12 -16 0 0 51.87 2.44 -16 0 0 49.17 4.14 16 0 0 49.93 2.82 -18 0 0 17.12 3.70 18 0 0 15.11 2.68 -18 0 0 11.79 2.38 -20 0 0 77.75 6.01 20 0 0 76.40 6.06 -20 0 0 79.73 5.19 22 0 0 -4.43 3.16 -22 0 0 1.74 3.15 -22 0 0 0.22 2.21 -24 0 0 70.43 5.30 24 0 0 63.40 8.30 -24 0 0 66.18 7.98 -26 0 0 6.15 7.63 -26 0 0 3.44 2.92 26 0 0 -3.66 7.64 7 -1 0 3323.05 69.65 7 -1 0 3291.34 69.44 -7 -1 0 3442.55 69.40 -7 -1 0 3264.12 69.55 -7 -1 0 3419.31 69.68 7 1 0 3429.36 69.53 7 1 0 3500.26 69.13 -7 1 0 3397.99 69.40 -7 1 0 3375.51 69.56 7 1 0 3494.94 69.29 7 1 0 3284.80 69.47 -7 1 0 3407.06 69.54 7 1 0 3287.82 69.61 -9 -1 0 2437.16 51.74 -9 -1 0 2588.79 51.76 -9 -1 0 2512.09 51.57 9 -1 0 2509.98 51.60 9 -1 0 2446.06 51.96 9 -1 0 2403.19 51.40 9 1 0 2553.30 51.25 9 1 0 2483.77 51.86 9 1 0 2536.51 51.78 -9 1 0 2472.51 51.70 9 1 0 2490.93 51.42 -9 1 0 2520.85 51.81 -9 1 0 2479.38 51.86 11 -1 0 1668.00 35.65 11 -1 0 1752.89 35.96 -11 -1 0 1658.12 36.14 -11 -1 0 1773.59 36.29 -11 -1 0 1718.09 35.84 11 -1 0 1709.41 36.43 -11 1 0 1731.21 35.57 11 1 0 1736.02 36.12 11 1 0 1703.19 36.28 11 1 0 1744.81 35.46 -11 1 0 1689.45 36.28 11 1 0 1712.59 35.85 -11 1 0 1670.70 36.01 -13 -1 0 117.52 4.68 13 -1 0 118.54 4.77 13 -1 0 120.02 4.11 -13 -1 0 120.41 3.91 13 -1 0 117.91 3.72 13 1 0 119.00 4.37 13 1 0 116.82 3.67 13 1 0 119.93 4.72 -13 1 0 117.03 4.25 -13 1 0 119.34 3.61 -13 1 0 110.83 4.65 15 -1 0 52.86 2.76 15 -1 0 53.66 4.05 -15 -1 0 48.95 3.88 15 1 0 52.33 2.97 15 1 0 56.33 2.74 -15 1 0 52.25 3.89 15 1 0 48.30 3.75 15 1 0 44.62 3.38 -15 1 0 50.88 3.39 -15 1 0 50.51 2.61 -17 -1 0 377.21 10.47 17 -1 0 384.95 9.03 17 -1 0 375.87 10.71 17 1 0 373.51 9.60 17 1 0 381.26 10.56 -17 1 0 377.61 8.87 17 1 0 368.01 9.16 -17 1 0 373.24 9.80 -17 1 0 388.23 10.64 -19 -1 0 49.30 4.35 -19 -1 0 44.37 5.29 19 -1 0 49.25 3.11 19 -1 0 45.23 5.61 19 1 0 45.34 5.35 -19 1 0 49.57 5.17 -19 1 0 51.17 2.92 -19 1 0 40.05 5.26 -21 -1 0 134.52 7.39 21 -1 0 134.84 7.81 -21 -1 0 132.44 6.31 21 1 0 134.01 7.60 -21 1 0 137.08 6.00 -21 1 0 135.31 7.52 -23 -1 0 4.69 3.21 23 -1 0 -0.74 3.75 -23 -1 0 1.61 2.39 -23 1 0 1.58 2.38 -23 1 0 3.18 3.46 23 1 0 2.23 3.46 -25 -1 0 -0.30 2.40 25 -1 0 1.46 4.46 -25 -1 0 0.91 3.94 -25 1 0 -1.43 2.55 -25 1 0 7.17 4.17 25 1 0 0.11 4.25 6 -2 0 1659.50 34.63 -6 -2 0 1705.49 34.97 6 -2 0 1659.41 35.03 -6 -2 0 1702.15 34.79 6 -2 0 1703.95 34.89 6 -2 0 1614.30 34.61 -6 -2 0 1616.09 34.70 -6 -2 0 1715.59 34.80 -6 2 0 1702.33 34.77 -6 2 0 1616.08 34.81 -6 2 0 1705.19 34.85 6 2 0 1686.47 34.89 -6 2 0 1639.71 34.87 6 2 0 1624.84 34.82 6 2 0 1712.22 34.77 6 2 0 1670.04 34.89 8 -2 0 1867.02 40.42 -8 -2 0 1901.29 40.66 8 -2 0 1955.85 41.02 -8 -2 0 1994.47 40.69 8 -2 0 1904.43 40.54 -8 -2 0 1987.10 40.69 8 2 0 2028.13 40.46 -8 2 0 1965.40 40.68 -8 2 0 1899.68 40.82 8 2 0 1898.39 40.75 8 2 0 2072.94 40.34 -8 2 0 1941.42 40.73 8 2 0 1969.41 40.80 10 -2 0 939.48 20.14 10 -2 0 941.93 20.90 -10 -2 0 960.65 20.47 -10 -2 0 952.76 20.61 -10 -2 0 926.35 20.51 -10 2 0 922.22 20.41 -10 2 0 932.37 20.73 10 2 0 964.69 20.66 10 2 0 925.64 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176.98 5.56 -1 5 0 186.87 5.55 1 5 0 186.05 5.47 3 -5 0 104.81 4.04 -3 -5 0 116.11 4.45 3 -5 0 112.43 3.61 -3 -5 0 117.56 3.66 3 -5 0 106.39 4.29 -3 -5 0 100.07 4.19 3 5 0 114.58 4.11 -3 5 0 104.64 4.31 -3 5 0 113.37 3.94 3 5 0 100.30 4.30 5 -5 0 485.87 11.07 5 -5 0 483.84 11.96 -5 -5 0 492.29 11.19 5 -5 0 502.50 11.57 -5 -5 0 489.06 12.35 -5 5 0 501.09 11.60 5 5 0 490.82 11.51 5 5 0 477.20 12.18 -5 5 0 488.65 11.82 -7 -5 0 46.28 3.68 -7 -5 0 60.69 3.07 7 -5 0 57.20 3.97 7 -5 0 61.46 3.03 7 -5 0 56.49 3.40 -7 5 0 57.55 3.52 -7 5 0 58.87 3.78 7 5 0 59.36 3.74 7 5 0 60.12 3.29 -9 -5 0 313.20 8.05 -9 -5 0 310.65 8.58 9 -5 0 318.13 8.26 9 -5 0 313.51 9.11 -9 5 0 305.49 10.71 9 5 0 317.51 8.33 -9 5 0 321.99 8.74 9 5 0 313.71 8.69 -11 -5 0 22.64 3.81 -11 -5 0 25.00 3.88 11 5 0 18.59 4.04 -11 5 0 24.43 4.03 -11 5 0 27.51 3.76 13 -5 0 304.27 9.78 -13 -5 0 351.26 9.69 -13 -5 0 351.65 9.19 13 -5 0 310.54 10.54 -13 5 0 333.86 9.51 13 5 0 317.59 10.00 -13 5 0 326.60 10.07 13 5 0 334.48 9.36 -15 -5 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-20 1.85 3.29 -13 1 20 -2.53 3.55 13 1 -20 1.96 3.02 13 1 -20 -0.49 4.44 -11 -1 20 36.62 7.49 -11 -1 20 36.71 5.83 11 -1 -20 29.69 5.09 11 -1 -20 43.02 7.62 11 1 -20 40.62 6.22 11 1 -20 45.42 5.37 -11 1 20 47.90 7.38 11 1 -20 35.82 5.55 -11 1 20 31.23 4.88 9 -1 -20 16.04 4.59 9 -1 -20 18.41 4.66 -9 -1 20 16.00 4.44 9 -1 -20 16.33 4.28 -9 -1 20 14.60 3.42 -9 1 20 15.63 4.21 9 1 -20 15.95 3.73 9 1 -20 12.30 5.18 9 1 -20 17.64 3.05 -9 1 20 16.56 3.56 7 -1 -20 7.17 4.66 7 -1 -20 5.78 3.90 7 -1 -20 9.46 4.71 -7 -1 20 8.58 4.74 7 1 -20 -1.05 3.74 -7 1 20 7.66 4.03 7 1 -20 7.14 5.46 5 -1 -20 3.67 3.82 -5 -1 20 -0.60 4.44 -5 -1 20 -2.04 3.60 5 -1 -20 6.97 4.84 -5 1 20 3.62 4.01 5 1 -20 3.15 4.17 5 1 -20 1.78 5.72 3 -1 -20 20.46 5.15 -3 -1 20 20.46 6.37 -3 -1 20 10.67 3.87 3 -1 -20 15.98 5.84 -3 1 20 18.60 6.35 -3 1 20 14.12 4.51 3 1 -20 22.17 5.42 3 1 -20 26.81 6.94 -24 -2 20 4.00 5.37 24 -2 -20 3.04 4.93 -24 2 20 1.65 6.24 24 2 -20 1.03 4.86 -24 2 20 -3.79 3.45 24 2 -20 2.74 3.83 22 -2 -20 14.22 5.20 -22 -2 20 11.91 4.82 -22 2 20 3.08 3.41 22 2 -20 3.42 3.88 -22 2 20 8.25 3.81 -22 2 20 9.67 3.59 22 2 -20 8.59 4.38 20 -2 -20 21.66 3.91 -20 -2 20 20.89 3.81 20 -2 -20 24.25 5.32 -20 -2 20 25.65 5.28 -20 2 20 17.94 3.80 20 2 -20 31.26 6.27 20 2 -20 39.43 8.22 -20 2 20 24.86 5.09 20 2 -20 25.46 4.69 18 -2 -20 15.50 4.65 -18 -2 20 18.83 3.58 18 -2 -20 21.74 3.99 -18 -2 20 15.08 4.84 -18 -2 20 29.65 6.12 18 2 -20 21.02 3.31 -18 2 20 18.26 3.80 -18 2 20 20.58 3.73 18 2 -20 21.90 4.28 -16 -2 20 43.39 6.38 -16 -2 20 41.68 5.99 16 -2 -20 39.82 6.93 16 2 -20 43.51 7.11 -16 2 20 51.08 5.73 16 2 -20 49.10 5.64 -16 2 20 54.95 6.97 -16 2 20 42.03 8.65 -14 -2 20 45.28 5.71 14 -2 -20 42.69 7.27 14 -2 -20 45.85 7.35 -14 -2 20 55.88 6.85 -14 2 20 51.24 5.63 14 2 -20 54.76 6.01 14 2 -20 51.39 9.57 -14 2 20 47.87 9.08 14 2 -20 53.09 7.09 -12 -2 20 80.72 6.31 -12 -2 20 87.17 7.83 12 -2 -20 93.91 8.47 12 -2 -20 83.45 8.14 12 2 -20 86.48 6.86 12 2 -20 84.13 10.55 12 2 -20 86.75 7.49 -12 2 20 84.08 5.78 -10 -2 20 6.59 3.26 10 -2 -20 11.42 4.09 -10 -2 20 7.55 4.02 10 -2 -20 10.02 4.41 -10 2 20 13.38 6.72 -10 2 20 8.46 2.72 10 2 -20 10.69 3.11 10 2 -20 8.25 3.76 10 2 -20 6.11 5.03 8 -2 -20 5.13 4.29 -8 -2 20 2.75 4.10 8 -2 -20 2.79 4.30 8 2 -20 -0.45 3.86 8 2 -20 3.46 2.67 -8 2 20 2.50 5.00 8 2 -20 6.20 5.00 6 -2 -20 23.10 5.16 6 -2 -20 20.29 5.72 -6 -2 20 22.30 4.91 6 2 -20 25.22 4.83 -6 2 20 22.74 7.15 6 2 -20 14.93 5.73 -4 -2 20 3.95 7.33 4 -2 -20 -3.71 7.79 4 -2 -20 7.47 5.74 4 2 -20 4.25 9.55 4 2 -20 7.74 7.75 -2 -2 20 60.63 10.56 2 -2 -20 69.18 11.47 2 -2 -20 62.85 10.48 2 2 -20 54.93 12.85 2 2 -20 53.80 8.64 23 -3 -20 9.58 5.50 -23 3 20 16.81 8.26 23 3 -20 16.75 5.43 21 -3 -20 21.80 5.58 -21 -3 20 30.01 7.03 21 -3 -20 30.29 6.19 -21 -3 20 19.77 4.09 21 3 -20 36.97 5.28 -21 3 20 35.68 7.50 19 -3 -20 36.03 5.92 -19 -3 20 28.69 5.80 19 -3 -20 27.31 4.38 -19 -3 20 25.21 5.50 -19 3 20 31.39 6.55 19 3 -20 44.04 8.49 -19 3 20 23.77 3.88 17 -3 -20 27.79 5.25 -17 -3 20 23.16 5.39 -17 -3 20 27.30 4.03 17 -3 -20 23.88 4.32 17 3 -20 34.00 4.02 17 3 -20 27.36 4.49 -17 3 20 22.05 3.91 -17 3 20 33.24 6.02 15 -3 -20 34.04 7.40 -15 -3 20 22.27 3.99 15 3 -20 26.73 3.98 -15 3 20 32.65 6.57 15 3 -20 34.92 6.81 -15 3 20 21.16 3.59 15 3 -20 19.44 5.52 -15 3 20 17.11 4.91 13 -3 -20 88.74 9.99 -13 -3 20 85.51 9.88 13 -3 -20 71.15 7.20 -13 3 20 72.77 6.26 13 3 -20 84.38 11.22 -13 3 20 82.87 9.23 13 3 -20 85.84 7.42 13 3 -20 81.31 6.69 -11 -3 20 15.63 4.53 11 -3 -20 10.93 3.98 11 -3 -20 21.80 4.73 -11 3 20 18.32 3.18 11 3 -20 20.61 5.76 11 3 -20 17.81 3.90 -11 3 20 15.85 4.81 11 3 -20 17.89 3.71 -9 -3 20 67.02 8.66 9 -3 -20 64.03 9.45 9 -3 -20 58.92 7.92 9 3 -20 64.90 7.13 9 3 -20 65.82 6.33 -9 3 20 72.38 9.69 7 -3 -20 29.77 6.11 7 -3 -20 27.09 4.98 -7 -3 20 31.88 5.52 7 3 -20 30.38 7.15 7 3 -20 24.33 4.97 7 3 -20 38.44 5.76 -7 3 20 27.07 5.57 5 -3 -20 10.06 5.78 -5 -3 20 8.93 5.55 5 -3 -20 19.15 5.23 5 3 -20 10.14 6.66 -5 3 20 15.72 5.33 5 3 -20 26.37 10.23 20 -4 -20 16.04 4.64 -20 -4 20 11.39 5.58 20 4 -20 16.67 3.51 -20 4 20 13.47 4.45 20 4 -20 16.00 6.26 -18 -4 20 5.72 8.17 18 -4 -20 15.45 4.26 18 -4 -20 6.75 5.26 -18 4 20 11.51 3.86 18 4 -20 14.68 4.69 18 4 -20 15.95 3.60 -16 -4 20 42.94 9.38 -16 -4 20 38.95 6.84 16 -4 -20 44.28 7.88 -16 4 20 40.39 6.63 -16 4 20 33.50 6.01 16 4 -20 32.53 4.26 16 4 -20 46.56 8.50 -14 -4 20 20.51 4.13 14 -4 -20 24.73 4.73 14 4 -20 29.58 4.40 14 4 -20 25.79 5.09 14 4 -20 30.84 7.62 -14 4 20 22.25 3.69 -14 4 20 24.27 5.56 12 -4 -20 18.12 3.82 12 -4 -20 25.66 5.50 -12 -4 20 21.91 4.54 12 4 -20 27.43 7.66 -12 4 20 24.25 5.60 12 4 -20 19.50 4.19 -12 4 20 21.27 3.57 12 4 -20 27.04 4.49 10 -4 -20 0.59 3.68 10 -4 -20 6.65 5.04 -10 -4 20 4.55 4.49 10 4 -20 5.25 3.53 -10 4 20 1.56 5.17 10 4 -20 6.21 3.65 8 -4 -20 34.95 10.05 -8 -4 20 38.17 6.84 8 -4 -20 40.28 7.52 -8 4 20 39.33 6.59 8 4 -20 46.97 6.44 8 4 -20 40.81 8.23 8 4 -20 27.39 4.68 6 -4 -20 4.87 4.19 -6 -4 20 4.70 5.25 6 -4 -20 9.23 5.57 6 4 -20 11.73 6.60 6 4 -20 8.00 4.61 17 -5 -20 96.68 9.66 17 5 -20 80.97 7.14 17 5 -20 96.89 9.71 -17 5 20 91.96 8.12 -15 -5 20 34.78 6.75 -15 -5 20 20.43 4.53 -15 5 20 32.97 6.34 15 5 -20 24.52 4.16 -15 5 20 23.05 3.99 -13 -5 20 20.39 4.96 -13 5 20 8.80 6.65 13 5 -20 17.04 4.01 -13 5 20 24.08 4.01 13 5 -20 21.28 4.49 13 5 -20 19.50 6.29 11 -5 -20 32.86 11.22 -11 -5 20 15.99 4.67 11 5 -20 25.21 6.79 11 5 -20 23.54 4.42 11 5 -20 22.64 4.54 -11 5 20 21.02 5.99 9 -5 -20 2.25 4.95 9 5 -20 2.63 4.86 -22 0 21 0.81 4.08 22 0 -21 0.61 4.23 -20 0 21 -0.51 3.23 20 0 -21 4.13 4.00 -20 0 21 -1.97 3.91 -18 0 21 8.46 5.03 -18 0 21 8.10 3.73 -18 0 21 3.86 4.19 -16 0 21 45.48 7.20 -16 0 21 37.67 7.18 14 0 -21 2.25 4.49 14 0 -21 2.37 3.18 -14 0 21 6.56 3.73 -14 0 21 4.92 5.18 12 0 -21 19.50 5.14 -12 0 21 24.18 4.30 -12 0 21 17.82 4.65 12 0 -21 23.72 4.20 -10 0 21 59.80 8.00 -10 0 21 72.41 9.40 10 0 -21 60.83 7.10 10 0 -21 64.82 10.25 8 0 -21 -1.05 5.14 8 0 -21 4.48 3.87 -8 0 21 2.00 3.82 -8 0 21 2.62 4.70 6 0 -21 1.82 5.70 -6 0 21 -5.15 3.86 6 0 -21 6.55 5.59 -6 0 21 -2.44 5.69 -21 -1 21 13.52 3.75 -21 -1 21 16.57 6.09 21 -1 -21 18.55 4.80 21 1 -21 10.26 3.95 -21 1 21 9.62 7.29 -21 1 21 15.88 3.98 21 1 -21 11.23 4.28 -21 1 21 12.32 4.15 19 -1 -21 26.88 4.88 -19 -1 21 32.62 6.37 -19 -1 21 27.46 5.93 -19 -1 21 38.07 7.16 -19 1 21 21.55 4.42 -19 1 21 27.02 4.46 -19 1 21 20.46 4.15 19 1 -21 23.61 3.61 19 1 -21 25.74 4.36 -17 -1 21 47.03 9.17 -17 -1 21 30.30 6.51 -17 -1 21 43.75 8.66 17 1 -21 30.50 5.62 -17 1 21 41.31 7.36 17 1 -21 36.98 7.00 -17 1 21 31.21 4.82 -17 1 21 41.13 7.73 -17 1 21 26.23 4.29 15 -1 -21 35.09 8.20 -15 -1 21 41.79 7.19 -15 -1 21 40.78 6.71 -15 1 21 53.14 7.67 15 1 -21 36.30 5.80 15 1 -21 38.74 6.69 -15 1 21 39.85 7.60 15 1 -21 44.65 5.98 -15 1 21 38.98 6.15 13 -1 -21 8.72 4.25 -13 -1 21 19.82 5.11 -13 -1 21 13.77 3.85 13 1 -21 13.19 3.61 13 1 -21 13.38 3.39 -13 1 21 12.09 3.76 -13 1 21 16.95 4.31 -13 1 21 12.23 4.17 13 1 -21 12.75 4.94 11 -1 -21 25.36 5.23 -11 -1 21 24.01 4.88 -11 -1 21 23.65 4.00 -11 1 21 25.76 5.19 -11 1 21 28.65 4.80 11 1 -21 32.89 5.88 11 1 -21 28.69 4.40 11 1 -21 26.07 6.07 -9 -1 21 7.00 4.50 -9 -1 21 7.42 3.71 9 -1 -21 4.17 4.41 -9 1 21 7.45 4.33 9 1 -21 8.90 5.55 -9 1 21 7.78 4.85 9 1 -21 4.14 4.11 -7 -1 21 5.26 3.82 7 -1 -21 4.80 5.15 7 1 -21 9.03 7.15 7 1 -21 4.59 5.37 -7 1 21 10.41 4.37 5 -1 -21 15.73 6.14 -5 -1 21 12.99 5.51 5 -1 -21 14.50 4.92 -5 1 21 12.77 5.64 5 1 -21 10.23 10.81 5 1 -21 17.33 4.62 -5 1 21 7.72 4.60 -20 -2 21 8.02 4.95 -20 -2 21 7.35 3.51 20 -2 -21 4.81 4.78 -20 2 21 11.06 3.69 20 2 -21 8.90 3.14 -20 2 21 9.34 3.87 20 2 -21 7.93 4.19 18 -2 -21 10.72 4.00 -18 -2 21 13.69 4.01 -18 -2 21 10.96 5.04 18 2 -21 11.66 3.40 18 2 -21 7.49 4.07 -18 2 21 5.77 3.69 -18 2 21 12.94 4.74 -18 2 21 8.76 3.44 16 -2 -21 31.63 7.22 -16 -2 21 22.87 4.23 -16 2 21 26.80 5.19 16 2 -21 27.62 5.72 16 2 -21 34.44 6.02 -16 2 21 23.96 3.99 16 2 -21 30.69 4.60 -16 2 21 36.79 7.11 -14 -2 21 17.04 4.56 14 -2 -21 14.91 4.25 14 -2 -21 16.31 4.32 14 2 -21 16.83 3.71 -14 2 21 14.35 4.63 14 2 -21 14.00 5.35 14 2 -21 21.22 4.05 -14 2 21 15.90 3.62 -12 -2 21 16.29 4.79 12 -2 -21 20.55 4.58 12 -2 -21 17.06 5.16 12 2 -21 19.06 4.18 12 2 -21 16.06 5.98 -12 2 21 14.65 4.67 -12 2 21 11.31 3.23 12 2 -21 16.87 3.62 10 -2 -21 8.42 4.50 -10 -2 21 4.37 4.36 10 -2 -21 1.98 4.41 10 2 -21 4.75 3.72 10 2 -21 5.85 6.05 -10 2 21 10.65 4.54 10 2 -21 11.73 3.36 8 -2 -21 46.21 10.23 -8 -2 21 54.94 8.90 8 -2 -21 56.27 9.60 8 2 -21 53.45 9.63 8 2 -21 52.89 7.38 -8 2 21 54.53 9.96 6 -2 -21 15.00 5.54 -6 -2 21 12.40 5.21 6 -2 -21 17.18 5.62 6 2 -21 17.27 4.96 -6 2 21 13.88 5.14 6 2 -21 19.77 6.86 19 -3 -21 56.41 10.36 -19 -3 21 63.32 14.88 19 -3 -21 55.72 7.74 -19 -3 21 61.10 6.70 19 3 -21 62.41 9.25 -19 3 21 61.90 7.27 -17 -3 21 8.04 3.79 17 -3 -21 18.58 4.75 -17 -3 21 10.51 9.18 17 3 -21 12.72 4.23 -17 3 21 10.77 5.09 -17 3 21 13.62 3.64 -17 3 21 11.66 4.12 17 3 -21 14.67 3.60 15 -3 -21 9.91 4.63 -15 -3 21 6.86 3.85 15 3 -21 6.90 3.83 15 3 -21 9.74 4.27 -15 3 21 6.49 4.79 15 3 -21 -0.72 8.84 -15 3 21 8.93 3.33 -15 3 21 12.28 3.89 -13 -3 21 9.81 6.42 13 -3 -21 9.76 3.87 13 -3 -21 13.64 4.74 -13 3 21 7.82 3.21 13 3 -21 13.95 3.89 13 3 -21 9.37 8.69 13 3 -21 11.24 3.71 -13 3 21 17.32 4.92 11 -3 -21 16.79 4.34 -11 -3 21 17.59 4.81 11 -3 -21 24.15 5.81 -11 3 21 27.99 5.57 11 3 -21 29.16 6.31 11 3 -21 23.29 4.39 -9 -3 21 -7.79 6.66 9 -3 -21 1.99 4.24 9 -3 -21 -1.58 8.60 9 3 -21 -4.38 5.71 9 3 -21 3.31 3.08 9 3 -21 1.01 6.85 -9 3 21 3.06 5.26 14 -4 -21 9.00 4.73 -14 -4 21 7.13 3.88 14 4 -21 11.78 4.00 -14 4 21 2.61 8.01 14 4 -21 10.67 5.98 -14 4 21 10.22 3.52 14 4 -21 11.34 4.30 12 4 -21 26.18 4.88 -18 0 22 91.86 9.95 -18 0 22 75.09 9.26 -18 0 22 70.21 8.60 16 0 -22 194.87 11.97 -16 0 22 202.07 10.26 -16 0 22 199.70 10.50 -16 0 22 188.03 8.87 -14 0 22 5.09 3.31 -14 0 22 1.90 4.26 -14 0 22 -1.74 3.78 14 0 -22 2.52 4.76 14 0 -22 -2.65 3.42 12 0 -22 20.91 5.76 12 0 -22 19.46 3.99 -12 0 22 9.43 5.04 -12 0 22 12.63 4.47 10 0 -22 59.48 11.42 -10 0 22 58.18 8.77 -10 0 22 33.45 9.65 10 0 -22 37.19 8.16 -17 -1 22 -1.38 3.91 -17 -1 22 5.43 3.99 -17 1 22 -0.32 4.20 17 1 -22 7.18 3.72 -17 1 22 7.48 4.41 -17 1 22 1.47 3.52 -17 1 22 6.86 4.75 17 1 -22 4.86 3.77 -15 -1 22 12.64 4.28 15 -1 -22 8.26 5.34 -15 -1 22 16.31 4.14 -15 1 22 16.10 4.58 15 1 -22 16.06 3.82 -15 1 22 14.54 3.54 15 1 -22 17.40 4.20 15 1 -22 11.78 5.12 -15 1 22 18.74 4.76 13 -1 -22 9.18 4.96 -13 -1 22 14.09 4.16 -13 -1 22 15.81 6.36 13 1 -22 16.89 3.71 13 1 -22 11.73 5.53 -13 1 22 18.34 5.16 -13 1 22 13.79 3.70 -13 1 22 17.25 4.66 13 1 -22 14.61 3.87 11 -1 -22 63.44 10.59 -11 -1 22 57.06 9.82 -11 -1 22 71.89 14.58 -11 1 22 66.17 9.99 11 1 -22 63.83 9.45 11 1 -22 68.13 12.45 -11 1 22 52.76 10.14 16 -2 -22 12.24 4.49 16 2 -22 9.51 4.02 16 2 -22 9.80 3.91 -14 -2 22 22.53 5.03 14 -2 -22 18.99 4.87 14 -2 -22 20.67 4.65 14 2 -22 24.95 4.14 14 2 -22 25.29 4.46 -14 2 22 25.95 5.55 14 2 -22 23.72 10.52 -14 2 22 20.70 3.72 0 0 0 0.00 0.00 _exptl_absorpt_process_details 'SADABS 2014/5' _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6873 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71076 22.976 8.872 16.772 89.999 118.543 90.000 ) _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 27368 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -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 O4 O 0.54861(12) 0.4041(3) 0.18285(15) 0.0606(5) Uani 1 1 d . O1 O 0.46407(11) 0.5224(3) 0.34732(15) 0.0642(6) Uani 1 1 d . O3 O 0.59492(11) 0.5086(3) 0.10566(14) 0.0611(5) Uani 1 1 d . O2 O 0.37176(12) 0.5937(3) 0.34938(16) 0.0703(7) Uani 1 1 d . N2 N 0.45082(11) 0.2941(3) 0.02723(14) 0.0406(4) Uani 1 1 d . N1 N 0.55293(12) 0.6970(3) 0.47865(15) 0.0430(5) Uani 1 1 d . N3 N 0.35886(12) 0.3121(3) 0.09945(16) 0.0548(6) Uani 1 1 d . N4 N 0.62868(13) 0.7213(3) 0.38490(16) 0.0543(6) Uani 1 1 d . C14 C 0.51476(12) 0.8387(3) 0.46704(15) 0.0408(5) Uani 1 1 d . H14 H 0.4779 0.8411 0.4048 0.049 Uiso 1 1 calc R C7 C 0.46490(10) 0.1472(3) -0.00403(14) 0.0365(5) Uani 1 1 d . H7 H 0.4321 0.1323 -0.0679 0.044 Uiso 1 1 calc R C25 C 0.60351(14) 0.6194(3) 0.31861(18) 0.0466(5) Uani 1 1 d . H25 H 0.5753 0.5464 0.3209 0.056 Uiso 1 1 calc R C20 C 0.40245(14) 0.5266(3) 0.31496(17) 0.0469(5) Uani 1 1 d . C6 C 0.45964(11) 0.0172(3) 0.05089(16) 0.0390(5) Uani 1 1 d . C24 C 0.61697(12) 0.6156(3) 0.24625(16) 0.0403(5) Uani 1 1 d . C5 C 0.48820(15) 0.0263(4) 0.14490(18) 0.0510(6) Uani 1 1 d . H5 H 0.5092 0.1148 0.1745 0.061 Uiso 1 1 calc R C19 C 0.39182(12) 0.3822(3) 0.17957(18) 0.0463(6) Uani 1 1 d . H19 H 0.4378 0.3876 0.2058 0.056 Uiso 1 1 calc R O5 O 0.24709(16) 0.8768(4) 0.2538(2) 0.0899(9) Uani 1 1 d . C18 C 0.36205(13) 0.4471(3) 0.22577(17) 0.0438(5) Uani 1 1 d . C26 C 0.58409(13) 0.4997(3) 0.17210(17) 0.0457(5) Uani 1 1 d . C13 C 0.55717(14) 0.9772(3) 0.48090(19) 0.0473(6) Uani 1 1 d . C15 C 0.29348(16) 0.3055(5) 0.0632(2) 0.0670(9) Uani 1 1 d . H15 H 0.2697 0.2557 0.0081 0.080 Uiso 1 1 calc R C12 C 0.53189(18) 1.0991(4) 0.4225(3) 0.0660(8) Uani 1 1 d . H12 H 0.4895 1.0945 0.3730 0.079 Uiso 1 1 calc R C17 C 0.29360(16) 0.4399(5) 0.1857(2) 0.0647(9) Uani 1 1 d . H17 H 0.2712 0.4825 0.2139 0.078 Uiso 1 1 calc R C1 C 0.42890(15) -0.1152(4) 0.0083(2) 0.0558(7) Uani 1 1 d . H1 H 0.4096 -0.1227 -0.0546 0.067 Uiso 1 1 calc R O6 O 0.18450(18) 0.6719(5) 0.1952(3) 0.1238(16) Uani 1 1 d . C23 C 0.65908(15) 0.7241(3) 0.2441(2) 0.0511(6) Uani 1 1 d . H23 H 0.6692 0.7261 0.1967 0.061 Uiso 1 1 calc R C4 C 0.4855(2) -0.0956(4) 0.1946(2) 0.0669(9) Uani 1 1 d . H4 H 0.5052 -0.0890 0.2575 0.080 Uiso 1 1 calc R C21 C 0.66925(17) 0.8255(4) 0.3812(2) 0.0599(7) Uani 1 1 d . H21 H 0.6868 0.8980 0.4268 0.072 Uiso 1 1 calc R C8 C 0.62067(16) 0.9859(4) 0.5537(2) 0.0623(8) Uani 1 1 d . H8 H 0.6380 0.9049 0.5935 0.075 Uiso 1 1 calc R C11 C 0.5700(3) 1.2277(5) 0.4381(4) 0.0922(14) Uani 1 1 d . H11 H 0.5529 1.3100 0.3993 0.111 Uiso 1 1 calc R C16 C 0.25914(16) 0.3682(6) 0.1029(3) 0.0784(12) Uani 1 1 d . H16 H 0.2131 0.3626 0.0744 0.094 Uiso 1 1 calc R C22 C 0.68621(19) 0.8301(4) 0.3129(2) 0.0621(8) Uani 1 1 d . H22 H 0.7153 0.9031 0.3130 0.074 Uiso 1 1 calc R C3 C 0.4540(2) -0.2268(4) 0.1515(3) 0.0696(9) Uani 1 1 d . H3 H 0.4512 -0.3073 0.1850 0.084 Uiso 1 1 calc R C10 C 0.6323(3) 1.2345(5) 0.5097(4) 0.0994(16) Uani 1 1 d . H10 H 0.6575 1.3214 0.5196 0.119 Uiso 1 1 calc R C2 C 0.42661(18) -0.2378(4) 0.0587(3) 0.0703(9) Uani 1 1 d . H2 H 0.4065 -0.3272 0.0295 0.084 Uiso 1 1 calc R C9 C 0.6583(2) 1.1138(5) 0.5675(3) 0.0871(12) Uani 1 1 d . H9 H 0.7012 1.1186 0.6158 0.105 Uiso 1 1 calc R C29 C 0.2110(2) 0.7601(6) 0.2574(4) 0.0903(14) Uani 1 1 d . C30 C 0.2089(3) 0.7562(7) 0.3430(5) 0.1121(18) Uani 1 1 d . H30A H 0.2506 0.7205 0.3905 0.168 Uiso 1 1 calc GR H30B H 0.1741 0.6897 0.3372 0.168 Uiso 1 1 calc GR H30C H 0.2005 0.8558 0.3576 0.168 Uiso 1 1 calc GR C28 C 0.2540(3) 0.8910(13) 0.1735(4) 0.145(3) Uani 1 1 d . H28A H 0.2472 0.7930 0.1447 0.174 Uiso 1 1 calc R H28B H 0.2199 0.9583 0.1312 0.174 Uiso 1 1 calc R C27 C 0.3163(4) 0.9466(14) 0.1914(6) 0.162(4) Uani 1 1 d . H27A H 0.3202 0.9427 0.1370 0.243 Uiso 1 1 calc GR H27B H 0.3505 0.8860 0.2375 0.243 Uiso 1 1 calc GR H27C H 0.3209 1.0490 0.2121 0.243 Uiso 1 1 calc GR H2A H 0.4351(15) 0.368(4) -0.024(2) 0.046(8) Uiso 1 1 d . H1A H 0.5765(18) 0.714(4) 0.455(2) 0.052(8) Uiso 1 1 d . H1B H 0.5791(15) 0.661(4) 0.538(2) 0.042(7) Uiso 1 1 d . H2B H 0.4195(19) 0.282(4) 0.043(2) 0.059(9) Uiso 1 1 d . H1C H 0.523(2) 0.622(5) 0.444(3) 0.061(10) Uiso 1 1 d . H2C H 0.490(2) 0.331(5) 0.085(3) 0.075(11) 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 O4 0.0688(13) 0.0592(12) 0.0578(11) -0.0136(10) 0.0333(10) -0.0176(10) O1 0.0528(11) 0.0734(14) 0.0601(12) -0.0216(11) 0.0220(9) -0.0070(11) O3 0.0729(13) 0.0692(14) 0.0512(10) -0.0121(10) 0.0378(10) -0.0082(11) O2 0.0702(14) 0.0864(17) 0.0565(12) -0.0224(12) 0.0321(11) 0.0071(12) N2 0.0413(10) 0.0492(12) 0.0428(10) 0.0036(9) 0.0294(9) 0.0042(8) N1 0.0464(11) 0.0498(12) 0.0409(10) -0.0011(9) 0.0275(9) -0.0021(9) N3 0.0513(12) 0.0741(17) 0.0505(12) -0.0131(11) 0.0337(10) -0.0074(11) N4 0.0638(14) 0.0602(14) 0.0512(12) -0.0080(11) 0.0373(11) -0.0083(12) C14 0.0425(11) 0.0474(13) 0.0330(10) 0.0026(9) 0.0183(9) 0.0007(10) C7 0.0317(10) 0.0485(13) 0.0318(9) -0.0023(9) 0.0174(8) -0.0003(9) C25 0.0510(13) 0.0471(13) 0.0511(13) 0.0001(11) 0.0319(11) -0.0050(11) C20 0.0549(14) 0.0444(13) 0.0444(12) -0.0041(10) 0.0263(11) 0.0002(11) C6 0.0344(10) 0.0461(12) 0.0418(11) -0.0001(10) 0.0226(9) 0.0002(9) C24 0.0413(11) 0.0410(12) 0.0412(11) 0.0020(9) 0.0219(9) 0.0033(9) C5 0.0631(15) 0.0524(15) 0.0420(12) 0.0032(11) 0.0288(11) -0.0008(13) C19 0.0405(11) 0.0573(15) 0.0489(13) -0.0074(11) 0.0276(10) -0.0042(11) O5 0.0809(17) 0.108(2) 0.0699(16) -0.0195(16) 0.0271(13) -0.0042(18) C18 0.0441(12) 0.0482(13) 0.0449(12) -0.0022(10) 0.0260(10) -0.0013(10) C26 0.0458(12) 0.0481(14) 0.0444(12) -0.0029(10) 0.0225(10) 0.0035(11) C13 0.0516(13) 0.0490(14) 0.0469(13) 0.0046(11) 0.0282(11) 0.0002(11) C15 0.0562(16) 0.098(3) 0.0490(14) -0.0205(16) 0.0270(13) -0.0160(17) C12 0.0634(18) 0.0617(18) 0.073(2) 0.0179(16) 0.0325(16) 0.0058(15) C17 0.0488(15) 0.092(2) 0.0655(18) -0.0173(17) 0.0370(14) -0.0001(15) C1 0.0471(13) 0.0615(17) 0.0616(16) -0.0122(14) 0.0284(12) -0.0116(12) O6 0.078(2) 0.110(3) 0.142(3) -0.049(3) 0.020(2) 0.0076(19) C23 0.0620(16) 0.0517(15) 0.0546(14) 0.0032(12) 0.0401(13) -0.0001(12) C4 0.083(2) 0.070(2) 0.0585(17) 0.0195(16) 0.0425(17) 0.0135(18) C21 0.0733(19) 0.0537(16) 0.0619(16) -0.0157(14) 0.0398(15) -0.0144(14) C8 0.0565(16) 0.0574(18) 0.0618(17) 0.0050(14) 0.0194(14) -0.0095(14) C11 0.103(3) 0.054(2) 0.127(4) 0.033(2) 0.061(3) 0.005(2) C16 0.0409(14) 0.126(4) 0.0682(19) -0.022(2) 0.0259(14) -0.0060(19) C22 0.078(2) 0.0504(16) 0.0760(19) -0.0089(15) 0.0519(17) -0.0186(15) C3 0.075(2) 0.0544(17) 0.095(3) 0.0207(18) 0.054(2) 0.0074(16) C10 0.090(3) 0.063(2) 0.140(4) 0.001(3) 0.050(3) -0.024(2) C2 0.0625(18) 0.0484(16) 0.108(3) -0.0080(18) 0.048(2) -0.0109(14) C9 0.068(2) 0.076(3) 0.096(3) -0.001(2) 0.022(2) -0.022(2) C29 0.058(2) 0.081(3) 0.103(3) -0.026(2) 0.015(2) 0.018(2) C30 0.128(5) 0.081(3) 0.137(5) 0.014(3) 0.071(4) 0.012(3) C28 0.111(4) 0.248(10) 0.079(3) -0.023(5) 0.048(3) 0.009(6) C27 0.127(5) 0.223(10) 0.141(6) 0.058(7) 0.067(5) -0.006(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C7 N2 H2A 108.6(19) . . C7 N2 H2B 110(3) . . C7 N2 H2C 112(3) . . H2A N2 H2B 109(3) . . H2A N2 H2C 113(3) . . H2B N2 H2C 104(3) . . C14 N1 H1A 105(3) . . C14 N1 H1B 117.5(19) . . C14 N1 H1C 108(2) . . H1A N1 H1B 110(3) . . H1A N1 H1C 107(3) . . H1B N1 H1C 109(3) . . C15 N3 C19 117.0(2) . . C25 N4 C21 117.7(2) . . N1 C14 C14 109.73(14) . 2_656 N1 C14 H14 108.1 . . N1 C14 C13 111.6(2) . . C14 C14 H14 108.1 2_656 . C13 C14 C14 111.07(16) . 2_656 C13 C14 H14 108.1 . . N2 C7 C7 111.06(14) . 2_655 N2 C7 H7 108.6 . . N2 C7 C6 110.81(18) . . C7 C7 H7 108.6 2_655 . C6 C7 C7 109.19(16) . 2_655 C6 C7 H7 108.6 . . N4 C25 H25 118.1 . . N4 C25 C24 123.8(2) . . C24 C25 H25 118.1 . . O1 C20 O2 125.7(3) . . O1 C20 C18 116.6(2) . . O2 C20 C18 117.7(2) . . C5 C6 C7 120.9(2) . . C1 C6 C7 120.1(2) . . C1 C6 C5 118.9(3) . . C25 C24 C26 120.3(2) . . C23 C24 C25 117.3(2) . . C23 C24 C26 122.4(2) . . C6 C5 H5 119.9 . . C4 C5 C6 120.3(3) . . C4 C5 H5 119.9 . . N3 C19 H19 117.9 . . N3 C19 C18 124.3(2) . . C18 C19 H19 117.9 . . C29 O5 C28 117.2(5) . . C19 C18 C20 121.2(2) . . C19 C18 C17 117.4(2) . . C17 C18 C20 121.4(2) . . O4 C26 O3 126.3(3) . . O4 C26 C24 116.6(2) . . O3 C26 C24 117.1(2) . . C12 C13 C14 120.2(3) . . C8 C13 C14 120.6(3) . . C8 C13 C12 119.2(3) . . N3 C15 H15 118.3 . . N3 C15 C16 123.3(3) . . C16 C15 H15 118.3 . . C13 C12 H12 120.1 . . C11 C12 C13 119.8(4) . . C11 C12 H12 120.1 . . C18 C17 H17 120.6 . . C16 C17 C18 118.8(3) . . C16 C17 H17 120.6 . . C6 C1 H1 119.7 . . C6 C1 C2 120.5(3) . . C2 C1 H1 119.7 . . C24 C23 H23 120.2 . . C24 C23 C22 119.6(2) . . C22 C23 H23 120.2 . . C5 C4 H4 119.7 . . C3 C4 C5 120.5(3) . . C3 C4 H4 119.7 . . N4 C21 H21 118.6 . . N4 C21 C22 122.8(3) . . C22 C21 H21 118.6 . . C13 C8 H8 119.9 . . C9 C8 C13 120.3(3) . . C9 C8 H8 119.9 . . C12 C11 H11 119.8 . . C10 C11 C12 120.4(4) . . C10 C11 H11 119.8 . . C15 C16 C17 119.3(3) . . C15 C16 H16 120.4 . . C17 C16 H16 120.4 . . C23 C22 H22 120.7 . . C21 C22 C23 118.7(3) . . C21 C22 H22 120.7 . . C4 C3 H3 120.2 . . C2 C3 C4 119.6(3) . . C2 C3 H3 120.2 . . C11 C10 H10 119.8 . . C11 C10 C9 120.5(4) . . C9 C10 H10 119.8 . . C1 C2 H2 119.9 . . C3 C2 C1 120.1(3) . . C3 C2 H2 119.9 . . C8 C9 H9 120.1 . . C10 C9 C8 119.9(4) . . C10 C9 H9 120.1 . . O5 C29 C30 111.9(4) . . O6 C29 O5 121.7(6) . . O6 C29 C30 126.4(6) . . C29 C30 H30A 109.5 . . C29 C30 H30B 109.5 . . C29 C30 H30C 109.5 . . H30A C30 H30B 109.5 . . H30A C30 H30C 109.5 . . H30B C30 H30C 109.5 . . O5 C28 H28A 109.0 . . O5 C28 H28B 109.0 . . H28A C28 H28B 107.8 . . C27 C28 O5 112.9(6) . . C27 C28 H28A 109.0 . . C27 C28 H28B 109.0 . . C28 C27 H27A 109.5 . . C28 C27 H27B 109.5 . . C28 C27 H27C 109.5 . . H27A C27 H27B 109.5 . . H27A C27 H27C 109.5 . . H27B C27 H27C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 O4 C26 1.247(4) . O1 C20 1.250(3) . O3 C26 1.255(3) . O2 C20 1.254(3) . N2 C7 1.496(3) . N2 H2A 1.00(3) . N2 H2B 0.88(4) . N2 H2C 1.01(4) . N1 C14 1.491(3) . N1 H1A 0.82(4) . N1 H1B 0.95(3) . N1 H1C 0.94(4) . N3 C19 1.338(4) . N3 C15 1.324(4) . N4 C25 1.331(4) . N4 C21 1.335(4) . C14 C14 1.549(4) 2_656 C14 H14 0.9800 . C14 C13 1.514(4) . C7 C7 1.552(4) 2_655 C7 H7 0.9800 . C7 C6 1.516(3) . C25 H25 0.9300 . C25 C24 1.389(3) . C20 C18 1.506(4) . C6 C5 1.390(3) . C6 C1 1.380(4) . C24 C26 1.508(4) . C24 C23 1.377(4) . C5 H5 0.9300 . C5 C4 1.385(4) . C19 H19 0.9300 . C19 C18 1.381(3) . O5 C29 1.345(6) . O5 C28 1.436(6) . C18 C17 1.384(4) . C13 C12 1.385(4) . C13 C8 1.385(4) . C15 H15 0.9300 . C15 C16 1.370(5) . C12 H12 0.9300 . C12 C11 1.384(6) . C17 H17 0.9300 . C17 C16 1.380(5) . C1 H1 0.9300 . C1 C2 1.393(5) . O6 C29 1.209(6) . C23 H23 0.9300 . C23 C22 1.384(4) . C4 H4 0.9300 . C4 C3 1.377(6) . C21 H21 0.9300 . C21 C22 1.376(4) . C8 H8 0.9300 . C8 C9 1.377(5) . C11 H11 0.9300 . C11 C10 1.359(8) . C16 H16 0.9300 . C22 H22 0.9300 . C3 H3 0.9300 . C3 C2 1.376(6) . C10 H10 0.9300 . C10 C9 1.373(7) . C2 H2 0.9300 . C9 H9 0.9300 . C29 C30 1.461(8) . C30 H30A 0.9600 . C30 H30B 0.9600 . C30 H30C 0.9600 . C28 H28A 0.9700 . C28 H28B 0.9700 . C28 C27 1.404(11) . C27 H27A 0.9600 . C27 H27B 0.9600 . C27 H27C 0.9600 . _cod_database_fobs_code 2108386