#------------------------------------------------------------------------------ #$Date: 2021-11-03 02:03:18 +0200 (Wed, 03 Nov 2021) $ #$Revision: 270220 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/86/7708688.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_7708688 loop_ _publ_author_name 'Meyer, Marco' 'Mardegan, Lorenzo' 'Tordera, Daniel' 'Prescimone, Alessandro' 'Sessolo, Michele' 'Bolink, Henk J.' 'Constable, Edwin C.' 'Housecroft, Catherine E.' _publ_section_title ; A counterion study of a series of [Cu(P^P)(N^N)][A] compounds with bis(phosphane) and 6-methyl and 6,6'-dimethyl-substituted 2,2'-bipyridine ligands for light-emitting electrochemical cells ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT03239A _journal_year 2021 _chemical_formula_moiety 'C50 H42 Cu N2 O P2, F6 P, 0.5(C H2 Cl2), C4 H10 O' _chemical_formula_sum 'C54.5 H53 Cl Cu F6 N2 O2 P3' _chemical_formula_weight 1073.89 _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 geom _atom_sites_solution_primary dual _audit_creation_date 2020-03-02 _audit_creation_method ; Olex2 1.2 (compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-05-01 deposited with the CCDC. 2021-11-02 downloaded from the CCDC. ; _cell_angle_alpha 109.125(2) _cell_angle_beta 96.617(2) _cell_angle_gamma 109.348(2) _cell_formula_units_Z 2 _cell_length_a 11.0667(8) _cell_length_b 15.0405(11) _cell_length_c 18.1887(14) _cell_measurement_reflns_used 8124 _cell_measurement_temperature 150 _cell_measurement_theta_max 70.231 _cell_measurement_theta_min 4.35 _cell_volume 2612.4(3) _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 150 _diffrn_measured_fraction_theta_full 0.974 _diffrn_measured_fraction_theta_max 0.944 _diffrn_measurement_device Area _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_method '\f & \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_unetI/netI 0.0216 _diffrn_reflns_Laue_measured_fraction_full 0.974 _diffrn_reflns_Laue_measured_fraction_max 0.944 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 33044 _diffrn_reflns_point_group_measured_fraction_full 0.974 _diffrn_reflns_point_group_measured_fraction_max 0.944 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 70.240 _diffrn_reflns_theta_min 3.389 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.467 _exptl_absorpt_correction_T_max 0.7533 _exptl_absorpt_correction_T_min 0.6394 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0742 before and 0.0396 after correction. The Ratio of minimum to maximum transmission is 0.8488. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.365 _exptl_crystal_description block _exptl_crystal_F_000 1110 _exptl_crystal_recrystallization_method 'The material was recrystallised from a mixture of DCM and Et2O by solvent layering' _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _refine_diff_density_max 1.634 _refine_diff_density_min -0.710 _refine_diff_density_rms 0.104 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 645 _refine_ls_number_reflns 9401 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.078 _refine_ls_R_factor_all 0.0573 _refine_ls_R_factor_gt 0.0569 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1092P)^2^+4.5727P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1806 _refine_ls_wR_factor_ref 0.1813 _reflns_Friedel_coverage 0.000 _reflns_number_gt 9314 _reflns_number_total 9401 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt03239a2.cif _cod_data_source_block mem040_150k_0m _cod_original_formula_sum 'C54.50 H53 Cl Cu F6 N2 O2 P3' _cod_database_code 7708688 _shelx_shelxl_version_number 2018/3 _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 0.665 _shelx_estimated_absorpt_t_min 0.601 _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. Others Fixed Sof: Cl2(0.5) Cl1(0.5) C55(0.5) H55A(0.5) H55B(0.5) 3.a Secondary CH2 refined with riding coordinates: C51(H51A,H51B), C55(H55A,H55B), C53(H53A,H53B) 3.b Aromatic/amide H refined with riding coordinates: C40(H40), C42(H42), C44(H44), C20(H20), C19(H19), C28(H28), C29(H29), C34(H34), C46(H46), C27(H27), C13(H13), C41(H41), C43(H43), C23(H23), C11(H11), C35(H35), C21(H21), C15(H15), C17(H17), C36(H36), C50(H50), C14(H14), C48(H48), C10(H10), C16(H16), C22(H22), C49(H49), C3(H3), C8(H8), C47(H47), C9(H9), C5(H5), C4(H4) 3.c Idealised Me refined as rotating group: C38(H38A,H38B,H38C), C37(H37A,H37B,H37C), C1(H1A,H1B,H1C), C54(H54A,H54B, H54C), C52(H52A,H52B,H52C) ; _shelx_res_file ; TITL mem040_150k_0m_a.res in P-1 mem040_150k_0m.res created by SHELXL-2018/3 at 11:55:33 on 02-Mar-2020 REM Old TITL MEM040_150K_0m in P-1 REM SHELXT solution in P-1: R1 0.130, Rweak 0.009, Alpha 0.065 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C55 N3 F9 P3 Cu CELL 1.54178 11.0667 15.0405 18.1887 109.125 96.617 109.348 ZERR 2 0.0008 0.0011 0.0014 0.002 0.002 0.002 LATT 1 SFAC C H Cl Cu F N O P UNIT 109 106 2 2 12 4 4 6 L.S. 10 PLAN 5 SIZE 0.18 0.22 0.23 TEMP -123.15 BOND list 4 fmap 2 53 acta OMIT 0 0 1 OMIT 1 -2 0 OMIT 0 2 1 OMIT 0 1 0 OMIT 1 0 0 OMIT -1 1 1 OMIT -1 0 1 OMIT -1 2 1 OMIT 1 1 0 OMIT 1 1 1 OMIT -1 2 0 OMIT 1 0 1 OMIT 0 1 2 OMIT 1 3 2 REM REM REM WGHT 0.109200 4.572700 FVAR 0.52926 CU1 4 0.685263 0.661237 0.335073 11.00000 0.02403 0.02051 = 0.02126 0.00898 0.00779 0.01088 P2 8 0.530143 0.684474 0.400178 11.00000 0.02285 0.01713 = 0.02068 0.00687 0.00786 0.00870 P1 8 0.613373 0.602061 0.199553 11.00000 0.02453 0.02149 = 0.01936 0.00953 0.00787 0.00977 P3 8 0.830118 1.141968 0.341972 11.00000 0.02583 0.02752 = 0.03958 0.01141 0.01293 0.01204 CL2 3 0.994334 0.922747 0.059683 10.50000 0.05718 0.04812 = 0.02802 0.01418 0.00380 -0.00758 CL1 3 1.020462 0.877993 0.202743 10.50000 0.06885 0.04110 = 0.02257 0.00691 -0.01106 0.00120 O1 7 0.376933 0.519436 0.248227 11.00000 0.03013 0.01773 = 0.02224 0.00921 0.01134 0.00894 F1 5 0.690916 1.094003 0.278112 11.00000 0.03613 0.04946 = 0.04762 0.00460 0.00465 0.01559 F2 5 0.970205 1.190782 0.405674 11.00000 0.02941 0.06017 = 0.05296 0.02224 0.01080 0.01757 F3 5 0.778406 1.214001 0.404239 11.00000 0.03944 0.06007 = 0.05034 0.00015 0.01393 0.02564 F4 5 0.883132 1.228483 0.307091 11.00000 0.05243 0.04750 = 0.07154 0.03521 0.02080 0.01989 F5 5 0.884207 1.072134 0.279553 11.00000 0.05881 0.05446 = 0.06475 0.00832 0.02452 0.03626 F6 5 0.778523 1.056427 0.376703 11.00000 0.05369 0.05547 = 0.09058 0.04705 0.02264 0.01104 N2 6 0.862942 0.783229 0.376791 11.00000 0.02867 0.02904 = 0.02391 0.00804 0.00955 0.00921 N1 6 0.805126 0.592623 0.367668 11.00000 0.04194 0.03354 = 0.01899 0.01137 0.01151 0.02517 C39 1 0.583857 0.757047 0.508638 11.00000 0.02707 0.01750 = 0.02165 0.00712 0.00873 0.00969 C18 1 0.530321 0.671277 0.161926 11.00000 0.02886 0.02493 = 0.01999 0.01083 0.00990 0.01299 C45 1 0.446789 0.756551 0.367082 11.00000 0.02533 0.02315 = 0.02466 0.01116 0.01100 0.01213 C25 1 0.386571 0.441322 0.185573 11.00000 0.03078 0.02051 = 0.02008 0.00855 0.00754 0.01286 C32 1 0.336761 0.491619 0.310329 11.00000 0.02648 0.02177 = 0.02425 0.01229 0.01176 0.01230 C40 1 0.497594 0.785007 0.553228 11.00000 0.02658 0.02579 = 0.02843 0.00869 0.00959 0.01306 AFIX 43 H40 2 0.408118 0.765638 0.526935 11.00000 -1.20000 AFIX 0 C42 1 0.672658 0.871028 0.673537 11.00000 0.03821 0.02314 = 0.02181 0.00671 0.00693 0.01226 AFIX 43 H42 2 0.703156 0.909693 0.729896 11.00000 -1.20000 AFIX 0 C26 1 0.294158 0.341452 0.160824 11.00000 0.03099 0.02242 = 0.02257 0.01032 0.00609 0.00936 C33 1 0.397647 0.565104 0.387855 11.00000 0.02611 0.01842 = 0.02727 0.01028 0.01153 0.01041 C44 1 0.715550 0.788000 0.547834 11.00000 0.02630 0.02251 = 0.02686 0.01170 0.01039 0.01226 AFIX 43 H44 2 0.774897 0.769728 0.518148 11.00000 -1.20000 AFIX 0 C20 1 0.351774 0.679531 0.079389 11.00000 0.03537 0.04672 = 0.03580 0.02027 0.01006 0.02300 AFIX 43 H20 2 0.268167 0.645767 0.041420 11.00000 -1.20000 AFIX 0 C24 1 0.493447 0.469378 0.152362 11.00000 0.02942 0.01990 = 0.02127 0.01054 0.00667 0.01001 C19 1 0.408653 0.623118 0.106676 11.00000 0.02906 0.02806 = 0.03139 0.01309 0.00892 0.01161 AFIX 43 H19 2 0.363769 0.550883 0.087299 11.00000 -1.20000 AFIX 0 C12 1 0.740707 0.600193 0.143790 11.00000 0.02513 0.02512 = 0.02114 0.00648 0.00764 0.00827 C31 1 0.242937 0.393778 0.291916 11.00000 0.02844 0.02081 = 0.02741 0.01028 0.00945 0.01022 C28 1 0.414988 0.291700 0.062927 11.00000 0.04486 0.02426 = 0.02437 0.00525 0.00987 0.01728 AFIX 43 H28 2 0.424210 0.239578 0.020124 11.00000 -1.20000 AFIX 0 C29 1 0.506407 0.392706 0.089603 11.00000 0.03697 0.02921 = 0.02233 0.01122 0.01179 0.01730 AFIX 43 H29 2 0.577303 0.409036 0.064951 11.00000 -1.20000 AFIX 0 C34 1 0.363902 0.536860 0.451069 11.00000 0.03691 0.02529 = 0.02420 0.01048 0.01249 0.01417 AFIX 43 H34 2 0.404263 0.584223 0.505118 11.00000 -1.20000 AFIX 0 C46 1 0.321010 0.713577 0.316518 11.00000 0.02798 0.02345 = 0.03856 0.00674 0.00359 0.01078 AFIX 43 H46 2 0.269347 0.642584 0.299887 11.00000 -1.20000 AFIX 0 C27 1 0.310778 0.266719 0.098344 11.00000 0.04105 0.01975 = 0.02514 0.00754 0.00530 0.00962 AFIX 43 H27 2 0.249908 0.197560 0.079633 11.00000 -1.20000 AFIX 0 C13 1 0.741903 0.626347 0.076788 11.00000 0.03011 0.03559 = 0.02697 0.01424 0.01066 0.01161 AFIX 43 H13 2 0.673878 0.644912 0.058121 11.00000 -1.20000 AFIX 0 C41 1 0.542653 0.841052 0.635894 11.00000 0.03569 0.02398 = 0.02863 0.00797 0.01358 0.01549 AFIX 43 H41 2 0.483528 0.858504 0.666175 11.00000 -1.20000 AFIX 0 C43 1 0.760459 0.845484 0.630163 11.00000 0.02770 0.02621 = 0.03087 0.01164 0.00581 0.01053 AFIX 43 H43 2 0.850498 0.867213 0.656681 11.00000 -1.20000 AFIX 0 C7 1 0.966913 0.763473 0.400096 11.00000 0.03378 0.03861 = 0.02181 0.00819 0.00957 0.01644 C30 1 0.181848 0.323427 0.202819 11.00000 0.03299 0.02251 = 0.02518 0.00959 0.00834 0.00651 C23 1 0.593068 0.777191 0.190398 11.00000 0.04458 0.02491 = 0.03314 0.01094 0.00148 0.00946 AFIX 43 H23 2 0.675921 0.811390 0.229113 11.00000 -1.20000 AFIX 0 C11 1 0.884382 0.878811 0.380499 11.00000 0.03208 0.02764 = 0.03310 0.01126 0.01002 0.00936 AFIX 43 H11 2 0.810680 0.893440 0.364709 11.00000 -1.20000 AFIX 0 C35 1 0.271020 0.439192 0.434846 11.00000 0.04170 0.02616 = 0.02781 0.01579 0.01711 0.01363 AFIX 43 H35 2 0.248611 0.420753 0.478184 11.00000 -1.20000 AFIX 0 C21 1 0.415997 0.784566 0.107106 11.00000 0.06174 0.04112 = 0.03793 0.02022 0.01500 0.03429 AFIX 43 H21 2 0.377316 0.822879 0.087660 11.00000 -1.20000 AFIX 0 C15 1 0.940442 0.598009 0.063725 11.00000 0.03396 0.04512 = 0.03955 0.00706 0.02021 0.01291 AFIX 43 H15 2 1.009050 0.597779 0.036807 11.00000 -1.20000 AFIX 0 C17 1 0.841001 0.572557 0.169409 11.00000 0.04051 0.04675 = 0.02853 0.01433 0.01133 0.02520 AFIX 43 H17 2 0.841716 0.554660 0.214886 11.00000 -1.20000 AFIX 0 C6 1 0.936929 0.657309 0.394154 11.00000 0.03600 0.04885 = 0.02305 0.01159 0.00849 0.02602 C36 1 0.210805 0.368505 0.356370 11.00000 0.03425 0.02010 = 0.03290 0.01324 0.01345 0.00889 AFIX 43 H36 2 0.147355 0.302548 0.346550 11.00000 -1.20000 AFIX 0 C50 1 0.519659 0.861194 0.390722 11.00000 0.02848 0.02639 = 0.04990 0.01780 0.00670 0.00887 AFIX 43 H50 2 0.606301 0.891884 0.425072 11.00000 -1.20000 AFIX 0 C38 1 0.115965 0.211166 0.190555 11.00000 0.04736 0.02237 = 0.02889 0.00787 0.01021 0.00242 AFIX 137 H38A 2 0.077035 0.169081 0.133102 11.00000 -1.50000 H38B 2 0.046372 0.202969 0.219576 11.00000 -1.50000 H38C 2 0.182212 0.189409 0.211117 11.00000 -1.50000 AFIX 0 C14 1 0.842055 0.625327 0.037362 11.00000 0.04171 0.04029 = 0.03311 0.01508 0.01997 0.01141 AFIX 43 H14 2 0.842543 0.643562 -0.007946 11.00000 -1.20000 AFIX 0 C2 1 0.769991 0.495217 0.359473 11.00000 0.05778 0.03475 = 0.02356 0.01252 0.01319 0.02888 C48 1 0.343074 0.876899 0.313974 11.00000 0.04535 0.04091 = 0.05133 0.02515 0.01471 0.02866 AFIX 43 H48 2 0.307545 0.917400 0.295413 11.00000 -1.20000 AFIX 0 C10 1 1.009745 0.956038 0.406450 11.00000 0.03975 0.03188 = 0.03792 0.01072 0.01029 0.00526 AFIX 43 H10 2 1.022360 1.022500 0.408459 11.00000 -1.20000 AFIX 0 C16 1 0.939681 0.570857 0.129384 11.00000 0.03693 0.05501 = 0.04445 0.01180 0.01201 0.02706 AFIX 43 H16 2 1.007030 0.551012 0.147016 11.00000 -1.20000 AFIX 0 C37 1 0.077540 0.357799 0.170011 11.00000 0.03056 0.04049 = 0.03443 0.01521 0.00633 0.01115 AFIX 137 H37A 2 0.120186 0.429572 0.177245 11.00000 -1.50000 H37B 2 0.008279 0.350487 0.199314 11.00000 -1.50000 H37C 2 0.038100 0.315106 0.112696 11.00000 -1.50000 AFIX 0 C1 1 0.627384 0.429091 0.330283 11.00000 0.06250 0.03132 = 0.03951 0.01935 0.01276 0.02388 AFIX 137 H1A 2 0.578358 0.462076 0.363357 11.00000 -1.50000 H1B 2 0.613083 0.362951 0.333930 11.00000 -1.50000 H1C 2 0.596114 0.418383 0.274197 11.00000 -1.50000 AFIX 0 C22 1 0.536088 0.833531 0.162928 11.00000 0.07042 0.02555 = 0.04234 0.01416 0.00826 0.02075 AFIX 43 H22 2 0.580005 0.905877 0.182669 11.00000 -1.20000 AFIX 0 C49 1 0.467656 0.921041 0.364890 11.00000 0.04045 0.02651 = 0.06567 0.02443 0.01544 0.01245 AFIX 43 H49 2 0.517872 0.992395 0.382281 11.00000 -1.20000 AFIX 0 C3 1 0.864714 0.457753 0.377801 11.00000 0.07185 0.04282 = 0.04476 0.01244 0.00884 0.04008 AFIX 43 H3 2 0.838764 0.388530 0.372202 11.00000 -1.20000 AFIX 0 C8 1 1.095707 0.839226 0.427179 11.00000 0.03005 0.05352 = 0.03840 0.01193 0.00821 0.01632 AFIX 43 H8 2 1.168634 0.824340 0.443974 11.00000 -1.20000 AFIX 0 C47 1 0.270173 0.773548 0.290081 11.00000 0.03619 0.03751 = 0.04657 0.01122 0.00086 0.02193 AFIX 43 H47 2 0.184096 0.743119 0.255088 11.00000 -1.20000 AFIX 0 C9 1 1.115064 0.933804 0.429146 11.00000 0.03002 0.04563 = 0.04031 0.00991 0.00720 0.00273 AFIX 43 H9 2 1.202223 0.985087 0.446373 11.00000 -1.20000 AFIX 0 O2 7 0.672500 0.096400 0.013015 11.00000 0.11472 0.08493 = 0.07191 0.03375 0.01997 0.05674 C5 1 1.033219 0.622961 0.412630 11.00000 0.04502 0.05182 = 0.05517 0.01389 0.00455 0.03023 AFIX 43 H5 2 1.123909 0.668110 0.431013 11.00000 -1.20000 AFIX 0 C4 1 0.996286 0.523217 0.404112 11.00000 0.06560 0.06308 = 0.06449 0.01846 0.00376 0.04758 AFIX 43 H4 2 1.061792 0.498844 0.416420 11.00000 -1.20000 AFIX 0 C51 1 0.663501 -0.003714 -0.024772 11.00000 0.11389 0.08370 = 0.09652 0.04994 0.04318 0.06490 AFIX 23 H51A 2 0.596093 -0.050761 -0.008637 11.00000 -1.20000 H51B 2 0.749626 -0.007449 -0.008562 11.00000 -1.20000 AFIX 0 C55 1 0.924725 0.901799 0.135713 10.50000 0.04358 0.02202 = 0.02849 0.00254 0.01789 0.01117 AFIX 23 H55A 2 0.838341 0.842816 0.111357 10.50000 -1.20000 H55B 2 0.907660 0.962568 0.165711 10.50000 -1.20000 AFIX 0 C53 1 0.719601 0.133966 0.097398 11.00000 0.08158 0.11354 = 0.07190 0.03486 0.00957 0.05413 AFIX 23 H53A 2 0.812664 0.141792 0.111709 11.00000 -1.20000 H53B 2 0.665572 0.085877 0.118655 11.00000 -1.20000 AFIX 0 C54 1 0.709480 0.236513 0.132506 11.00000 0.09108 0.10981 = 0.08469 0.01353 -0.00383 0.05939 AFIX 137 H54A 2 0.756850 0.270840 0.189489 11.00000 -1.50000 H54B 2 0.616206 0.226272 0.127165 11.00000 -1.50000 H54C 2 0.748822 0.278913 0.103626 11.00000 -1.50000 AFIX 0 C52 1 0.624776 -0.035189 -0.116069 11.00000 0.17122 0.07993 = 0.08459 0.03410 0.05077 0.06850 AFIX 137 H52A 2 0.543662 -0.025337 -0.131070 11.00000 -1.50000 H52B 2 0.609634 -0.107403 -0.143196 11.00000 -1.50000 H52C 2 0.696286 0.007058 -0.132283 11.00000 -1.50000 AFIX 0 HKLF 4 REM mem040_150k_0m_a.res in P-1 REM wR2 = 0.1813, GooF = S = 1.078, Restrained GooF = 1.078 for all data REM R1 = 0.0569 for 9314 Fo > 4sig(Fo) and 0.0573 for all 9401 data REM 645 parameters refined using 0 restraints END WGHT 0.1093 4.5639 REM Highest difference peak 1.634, deepest hole -0.710, 1-sigma level 0.104 Q1 1 1.0603 0.8655 0.1834 11.00000 0.05 1.63 Q2 1 0.9624 0.9339 0.0771 11.00000 0.05 1.57 Q3 1 1.0333 0.9008 0.0675 11.00000 0.05 1.50 Q4 1 1.0016 0.8935 0.1993 11.00000 0.05 1.39 Q5 1 0.8321 0.0446 -0.1201 11.00000 0.05 0.64 ; _shelx_res_checksum 49860 _shelx_hkl_file ; 1 0 0 599.24 29.20 1 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231.38 14.90 2 7 0 250.57 14.90 -3 -7 0 71.69 3.10 -3 -7 0 73.49 2.80 -3 -7 0 75.99 4.50 -3 -7 0 74.79 3.10 3 7 0 74.39 3.50 -4 -7 0 124.39 4.40 -4 -7 0 118.09 6.60 -4 -7 0 120.29 4.90 -4 -7 0 121.19 3.80 -5 -7 0 17.90 0.70 -5 -7 0 20.50 1.60 -5 -7 0 22.00 2.30 -5 -7 0 20.00 0.70 -6 -7 0 588.44 24.00 -6 -7 0 573.34 16.20 -6 -7 0 543.05 18.50 -7 -7 0 550.84 23.50 -7 -7 0 557.14 16.00 -7 -7 0 570.74 18.20 -8 -7 0 43.10 1.80 -8 -7 0 44.30 1.40 -9 -7 0 36.60 1.20 -13 8 0 115.99 3.80 -12 8 0 171.88 5.60 11 -8 0 3.20 0.50 -11 8 0 1.50 0.70 10 -8 0 31.00 1.30 10 -8 0 30.60 1.40 -10 8 0 28.70 1.50 9 -8 0 155.08 5.20 9 -8 0 160.88 5.70 8 -8 0 60.59 2.40 7 -8 0 633.84 23.50 7 -8 0 650.33 21.60 -7 8 0 607.24 22.60 6 -8 0 144.29 5.10 6 -8 0 140.29 5.90 -6 8 0 138.89 5.70 5 -8 0 330.57 12.20 5 -8 0 327.47 12.70 -5 8 0 339.97 12.40 -5 8 0 355.06 17.70 4 -8 0 453.55 16.30 4 -8 0 444.96 16.60 -4 8 0 453.05 25.10 -4 8 0 440.76 19.20 -4 8 0 468.85 16.30 -4 8 0 470.75 23.20 3 -8 0 257.17 9.50 3 -8 0 248.28 11.10 -3 8 0 274.07 13.80 -3 8 0 265.97 9.60 -3 8 0 271.17 15.00 -3 8 0 261.67 11.30 2 -8 0 675.43 24.60 2 -8 0 697.63 37.80 2 -8 0 681.73 27.80 -2 8 0 681.43 34.40 -2 8 0 713.23 40.40 -2 8 0 708.23 36.80 -2 8 0 694.83 28.60 1 -8 0 33.10 1.60 1 -8 0 37.50 3.60 1 -8 0 35.20 1.80 1 -8 0 32.70 1.40 1 -8 0 37.10 1.90 -1 8 0 36.00 2.70 -1 8 0 39.00 1.90 -1 8 0 38.80 2.90 0 -8 0 2.60 0.30 0 -8 0 3.60 0.60 0 -8 0 2.70 0.30 0 8 0 3.70 0.50 -1 -8 0 12.70 0.60 -1 -8 0 12.90 0.70 -1 -8 0 10.90 0.90 -1 -8 0 11.80 0.70 1 8 0 14.80 1.30 1 8 0 12.50 0.90 -2 -8 0 3.80 0.30 -2 -8 0 3.20 0.30 -2 -8 0 3.60 0.30 2 8 0 2.90 0.50 2 8 0 2.60 0.80 -3 -8 0 2.20 0.50 -3 -8 0 1.20 1.00 -3 -8 0 1.40 0.30 -4 -8 0 39.10 1.90 -4 -8 0 35.60 2.30 -4 -8 0 43.80 1.30 -4 -8 0 40.10 1.30 -5 -8 0 0.60 0.40 -5 -8 0 0.70 0.90 -6 -8 0 166.98 7.40 -6 -8 0 163.88 4.90 -7 -8 0 173.28 7.60 -7 -8 0 171.78 5.00 -8 -8 0 1.70 0.30 -13 9 0 3.40 0.40 12 -9 0 44.10 1.70 -12 9 0 46.70 1.80 11 -9 0 31.60 1.40 11 -9 0 32.10 1.40 -11 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5.90 -2 -10 0 145.59 6.60 -2 -10 0 139.89 4.20 -2 -10 0 147.09 4.50 -2 -10 0 149.88 5.40 -3 -10 0 43.80 1.40 -3 -10 0 45.10 1.50 -3 -10 0 42.60 2.00 -3 -10 0 45.70 2.50 -4 -10 0 25.50 0.90 -4 -10 0 24.40 0.90 -4 -10 0 26.20 1.90 -5 -10 0 22.10 1.50 -5 -10 0 23.70 0.90 -6 -10 0 27.60 0.90 -6 -10 0 28.40 1.60 -7 -10 0 89.89 2.60 12 -11 0 89.89 3.00 -12 11 0 90.39 3.10 11 -11 0 13.50 0.70 11 -11 0 13.40 0.80 10 -11 0 64.79 2.40 10 -11 0 67.89 2.60 -10 11 0 66.69 2.30 9 -11 0 192.18 6.00 9 -11 0 175.58 6.60 -9 11 0 182.78 6.00 8 -11 0 28.70 1.10 8 -11 0 27.60 1.40 8 -11 0 29.60 1.20 -8 11 0 27.30 1.30 7 -11 0 460.15 13.00 7 -11 0 462.75 14.40 7 -11 0 446.36 13.40 7 -11 0 451.65 15.80 -7 11 0 457.45 14.40 -7 11 0 461.65 14.40 6 -11 0 17.30 0.80 6 -11 0 17.20 0.70 6 -11 0 17.90 0.80 6 -11 0 16.30 1.00 6 -11 0 16.80 1.00 -6 11 0 17.00 0.90 -6 11 0 17.00 0.90 5 -11 0 158.28 4.60 5 -11 0 146.29 5.80 5 -11 0 149.59 5.50 5 -11 0 154.18 4.50 4 -11 0 442.96 16.30 4 -11 0 464.15 13.10 4 -11 0 450.65 15.60 3 -11 0 536.35 19.30 3 -11 0 543.45 15.60 2 -11 0 183.08 6.80 1 -11 0 3.70 0.40 1 -11 0 3.80 0.30 0 -11 0 744.73 31.50 0 -11 0 766.62 26.80 0 -11 0 755.92 21.40 0 -11 0 746.73 22.90 -1 -11 0 101.29 3.30 -1 -11 0 104.49 3.10 -1 -11 0 110.59 4.00 -1 -11 0 106.09 4.90 -2 -11 0 137.39 6.20 -2 -11 0 131.09 4.30 -2 -11 0 142.49 5.10 -2 -11 0 135.09 4.00 -3 -11 0 20.50 0.70 -3 -11 0 20.60 1.50 -3 -11 0 22.10 0.80 -4 -11 0 121.99 3.50 -4 -11 0 120.29 5.50 -4 -11 0 118.19 3.50 -5 -11 0 0.50 0.20 -5 -11 0 0.20 0.50 -6 -11 0 17.20 0.60 12 -12 0 4.60 0.30 11 -12 0 55.59 1.90 11 -12 0 57.79 2.20 11 -12 0 58.09 2.00 11 -12 0 54.09 1.80 10 -12 0 2.70 0.40 10 -12 0 3.20 0.60 10 -12 0 3.30 0.40 -10 12 0 3.10 0.50 9 -12 0 21.30 0.90 9 -12 0 20.70 1.10 9 -12 0 20.30 0.90 -9 12 0 19.50 1.00 8 -12 0 246.18 7.30 8 -12 0 253.57 7.30 8 -12 0 245.38 7.10 8 -12 0 242.98 7.80 8 -12 0 230.18 8.60 -8 12 0 252.77 7.90 7 -12 0 8.50 0.50 7 -12 0 8.90 0.60 7 -12 0 10.30 0.60 7 -12 0 8.00 0.70 7 -12 0 8.40 0.50 -7 12 0 8.50 0.80 6 -12 0 3.30 0.50 6 -12 0 3.40 0.40 6 -12 0 3.00 0.40 6 -12 0 2.50 0.40 6 -12 0 2.40 0.50 6 -12 0 2.20 0.30 6 -12 0 2.70 0.50 -6 12 0 2.80 0.70 -6 12 0 3.00 0.70 5 -12 0 706.43 20.10 5 -12 0 692.33 25.10 5 -12 0 678.43 24.00 5 -12 0 709.23 20.30 5 -12 0 724.63 19.90 4 -12 0 112.89 4.40 4 -12 0 112.59 3.40 4 -12 0 110.29 3.40 4 -12 0 108.69 3.30 4 -12 0 109.79 4.20 4 -12 0 117.79 3.60 3 -12 0 6.30 0.40 3 -12 0 5.60 0.60 3 -12 0 4.20 0.50 3 -12 0 5.50 0.50 2 -12 0 105.59 3.20 2 -12 0 104.79 3.20 2 -12 0 110.39 4.10 1 -12 0 4.50 0.30 1 -12 0 5.40 0.50 0 -12 0 34.10 1.50 0 -12 0 32.20 1.10 0 -12 0 29.50 1.90 -1 -12 0 182.68 5.20 -1 -12 0 173.68 7.90 -1 -12 0 177.88 6.50 -1 -12 0 174.28 5.50 -2 -12 0 135.39 4.30 -2 -12 0 134.79 4.00 -2 -12 0 139.29 6.20 -3 -12 0 139.99 6.30 -3 -12 0 141.99 4.10 -4 -12 0 14.80 1.10 -4 -12 0 14.80 0.60 -5 -12 0 1.70 0.20 11 -13 0 145.49 4.80 11 -13 0 149.39 4.50 11 -13 0 148.29 4.40 11 -13 0 151.58 4.50 10 -13 0 44.70 1.50 10 -13 0 45.90 1.60 10 -13 0 42.40 1.40 10 -13 0 42.80 1.80 -10 13 0 43.40 1.60 9 -13 0 56.29 1.80 9 -13 0 51.89 1.80 9 -13 0 55.89 2.20 9 -13 0 54.79 1.90 -9 13 0 53.99 2.00 8 -13 0 262.97 7.70 8 -13 0 258.57 8.30 8 -13 0 264.87 9.20 8 -13 0 256.77 7.60 8 -13 0 262.17 7.70 8 -13 0 262.47 7.70 -8 13 0 263.37 8.40 7 -13 0 151.98 5.10 7 -13 0 160.48 4.80 7 -13 0 160.38 4.80 7 -13 0 162.78 4.70 7 -13 0 157.38 5.80 -7 13 0 161.88 5.30 6 -13 0 13.60 0.70 6 -13 0 13.00 0.60 6 -13 0 12.50 0.90 6 -13 0 13.30 0.90 -6 13 0 14.20 0.90 5 -13 0 58.59 2.00 5 -13 0 59.79 2.60 5 -13 0 59.49 1.90 5 -13 0 59.59 1.90 4 -13 0 8.30 0.60 4 -13 0 8.20 0.60 4 -13 0 8.70 0.90 4 -13 0 9.10 0.60 3 -13 0 551.84 19.40 3 -13 0 519.75 15.30 3 -13 0 546.85 15.50 2 -13 0 78.39 3.10 2 -13 0 74.69 2.40 2 -13 0 77.99 2.40 1 -13 0 14.80 0.60 1 -13 0 14.60 0.60 1 -13 0 16.20 0.90 0 -13 0 96.09 2.80 0 -13 0 92.69 3.60 -1 -13 0 249.38 7.30 -1 -13 0 256.27 10.90 -2 -13 0 186.38 8.10 -2 -13 0 183.08 5.30 -3 -13 0 324.17 14.00 -3 -13 0 335.57 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5.80 8 -13 3 196.38 5.80 8 -13 3 196.68 5.80 8 -13 3 189.18 6.90 8 -13 3 194.58 6.30 -9 13 -3 72.09 2.50 9 -13 3 69.89 2.50 9 -13 3 74.39 2.30 9 -13 3 69.89 2.40 9 -13 3 69.99 2.40 9 -13 3 74.19 2.80 10 -13 3 165.48 5.80 10 -13 3 156.38 4.90 10 -13 3 166.68 5.30 -11 13 -3 9.20 0.70 11 -13 3 9.30 0.50 11 -13 3 8.60 0.60 -6 -12 3 2.40 0.20 -5 -12 3 85.69 4.00 -5 -12 3 87.39 2.60 -4 -12 3 208.38 6.20 -4 -12 3 218.88 9.30 -4 -12 3 214.88 6.20 -3 -12 3 48.60 2.60 -3 -12 3 49.00 1.60 -3 -12 3 48.50 1.60 -2 -12 3 103.59 3.20 -2 -12 3 102.19 4.90 -2 -12 3 108.69 3.20 -2 -12 3 107.79 4.10 -1 -12 3 13.10 1.10 -1 -12 3 13.40 0.80 -1 -12 3 12.70 0.60 -1 -12 3 13.30 0.60 0 -12 3 232.98 6.70 0 -12 3 241.18 8.60 0 -12 3 236.08 6.70 0 -12 3 222.08 10.10 0 -12 3 226.38 6.90 1 -12 3 10.90 0.60 1 -12 3 10.80 0.50 1 -12 3 11.00 0.50 1 -12 3 10.00 0.70 2 -12 3 33.60 1.20 2 -12 3 34.10 1.60 2 -12 3 33.30 1.10 3 -12 3 211.78 6.00 3 -12 3 191.38 7.60 3 -12 3 207.48 5.90 4 -12 3 18.80 0.80 4 -12 3 17.90 0.80 4 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5.60 -5 16 -4 1.50 0.50 5 -16 4 2.40 0.40 5 -16 4 1.10 0.30 -6 16 -4 299.97 9.60 6 -16 4 310.47 9.10 6 -16 4 297.97 8.70 -7 16 -4 298.87 9.30 7 -16 4 291.57 8.50 7 -16 4 294.37 8.90 -8 16 -4 154.48 4.90 8 -16 4 149.19 4.60 8 -16 4 146.79 4.40 -9 16 -4 1.00 0.40 9 -16 4 0.70 0.30 9 -16 4 0.80 0.20 -3 -15 4 1.60 0.20 -2 -15 4 18.80 1.20 -2 -15 4 21.00 0.70 -2 -15 4 20.50 0.70 -1 -15 4 27.60 1.60 -1 -15 4 27.70 0.90 -1 -15 4 28.80 0.90 0 -15 4 75.59 2.30 0 -15 4 73.69 2.30 1 -15 4 2.40 0.30 1 -15 4 2.80 0.30 2 -15 4 50.89 1.70 2 -15 4 55.19 1.70 3 -15 4 50.69 1.70 3 -15 4 51.19 2.30 3 -15 4 49.80 1.70 3 -15 4 51.39 1.70 -4 15 -4 296.17 9.40 4 -15 4 288.17 8.50 4 -15 4 302.57 9.00 -5 15 -4 534.25 16.40 5 -15 4 543.95 15.60 5 -15 4 499.25 15.10 5 -15 4 508.65 14.80 -6 15 -4 673.03 20.70 6 -15 4 659.43 18.70 6 -15 4 662.13 19.10 6 -15 4 658.43 19.20 6 -15 4 655.53 19.80 -7 15 -4 187.18 6.20 7 -15 4 192.68 5.60 7 -15 4 193.58 5.70 7 -15 4 191.68 6.00 7 -15 4 185.08 5.60 -8 15 -4 10.90 0.70 8 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-13 4 50.59 1.50 4 -13 4 46.10 1.70 4 -13 4 45.50 1.70 4 -13 4 48.00 1.60 4 -13 4 46.40 2.20 4 -13 4 48.80 1.60 4 -13 4 47.90 1.60 -5 13 -4 144.09 4.60 5 -13 4 140.59 4.20 5 -13 4 134.39 4.50 5 -13 4 138.39 4.20 5 -13 4 136.39 4.20 -6 13 -4 57.09 2.20 6 -13 4 58.39 2.00 6 -13 4 59.89 1.90 6 -13 4 55.89 2.40 6 -13 4 57.99 2.10 6 -13 4 58.29 1.90 -7 13 -4 285.07 8.90 7 -13 4 279.37 8.30 7 -13 4 276.67 8.30 7 -13 4 263.07 9.70 7 -13 4 275.67 8.30 7 -13 4 285.37 8.90 -8 13 -4 75.89 2.60 8 -13 4 72.99 2.90 8 -13 4 72.29 2.40 8 -13 4 74.39 2.40 8 -13 4 74.79 2.60 8 -13 4 71.89 2.40 -9 13 -4 20.20 1.00 9 -13 4 23.20 1.10 9 -13 4 21.00 0.90 9 -13 4 22.10 1.00 10 -13 4 108.59 3.60 10 -13 4 105.79 3.90 -11 13 -4 124.69 4.10 11 -13 4 121.29 3.80 11 -13 4 125.19 4.00 -6 -12 4 2.70 0.30 -5 -12 4 36.30 1.20 -5 -12 4 35.20 1.90 -4 -12 4 10.90 0.50 -4 -12 4 11.00 0.50 -4 -12 4 11.40 1.00 -3 -12 4 10.60 0.60 -3 -12 4 11.50 0.50 -3 -12 4 12.10 1.10 -2 -12 4 79.99 3.10 -2 -12 4 84.49 2.50 -2 -12 4 82.19 4.00 -2 -12 4 82.59 3.30 -2 -12 4 78.99 2.50 -1 -12 4 107.49 3.20 -1 -12 4 104.49 4.90 -1 -12 4 98.89 3.90 -1 -12 4 113.19 3.20 -1 -12 4 101.39 3.20 -1 -12 4 109.69 4.20 0 -12 4 643.44 18.70 0 -12 4 626.44 17.80 0 -12 4 640.74 17.90 0 -12 4 596.74 26.30 0 -12 4 631.04 22.50 1 -12 4 157.08 4.50 1 -12 4 153.68 5.80 1 -12 4 147.09 4.50 2 -12 4 148.69 4.50 2 -12 4 153.38 4.40 2 -12 4 146.19 5.70 3 -12 4 7.30 0.50 3 -12 4 7.10 0.50 3 -12 4 6.50 0.70 4 -12 4 1.00 0.40 4 -12 4 2.30 0.30 4 -12 4 1.90 0.40 4 -12 4 2.70 0.40 -5 12 -4 98.29 3.40 5 -12 4 96.99 3.30 5 -12 4 98.99 3.00 5 -12 4 97.79 3.10 5 -12 4 98.19 3.10 -6 12 -4 103.59 3.30 6 -12 4 96.89 3.30 6 -12 4 95.39 3.00 6 -12 4 91.49 3.00 6 -12 4 95.29 3.60 6 -12 4 93.29 3.00 6 -12 4 91.99 3.00 -7 12 -4 4.30 0.80 7 -12 4 3.10 0.60 7 -12 4 3.30 0.60 -8 12 -4 15.80 0.90 8 -12 4 17.80 1.00 8 -12 4 18.20 0.90 9 -12 4 1.40 0.50 9 -12 4 2.40 0.50 -10 12 -4 85.69 3.20 10 -12 4 94.79 3.40 10 -12 4 90.79 3.10 -11 12 -4 9.20 0.70 11 -12 4 11.20 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1 -4 8.80 0.70 -9 1 -4 8.80 0.70 -9 1 -4 9.40 1.00 -10 1 -4 3.30 0.50 -10 1 -4 3.10 0.40 -10 1 -4 3.00 0.70 -10 1 -4 3.10 0.50 10 -1 4 3.20 0.50 -11 1 -4 11.50 0.80 -11 1 -4 12.50 0.60 11 -1 4 12.40 0.60 12 0 -4 8.40 0.50 -12 0 4 8.60 0.60 -12 0 4 8.40 0.60 11 0 -4 10.00 0.60 -11 0 4 11.00 0.80 -11 0 4 9.70 0.60 -11 0 4 10.30 0.60 -11 0 4 10.40 0.80 10 0 -4 0.80 0.50 -10 0 4 1.70 0.40 -10 0 4 1.10 0.50 -10 0 4 1.70 0.60 -10 0 4 1.50 0.50 9 0 -4 115.59 3.70 9 0 -4 112.39 4.10 -9 0 4 112.09 4.00 -9 0 4 112.79 3.50 -9 0 4 100.99 6.10 -9 0 4 106.79 3.70 -9 0 4 109.59 3.50 8 0 -4 3.60 0.60 -8 0 4 2.90 0.60 -8 0 4 1.00 0.90 7 0 -4 2.90 0.40 -7 0 4 3.60 0.70 -6 0 4 105.09 4.40 -6 0 4 105.39 4.40 5 0 -4 741.53 27.40 5 0 -4 741.83 38.20 -5 0 4 772.32 28.40 4 0 -4 5730.33 203.88 4 0 -4 5687.93 281.67 4 0 -4 5539.95 294.67 4 0 -4 5621.54 231.98 -4 0 4 5760.72 212.28 3 0 -4 1437.76 77.99 3 0 -4 1513.65 74.59 3 0 -4 1524.15 61.69 3 0 -4 1548.15 54.19 -3 0 4 1494.25 61.49 2 0 -4 5976.70 307.17 2 0 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0 -4 5.90 0.90 -4 0 -4 5.00 0.60 -4 0 -4 3.80 0.50 4 0 4 3.80 0.60 4 0 4 3.20 0.80 -5 0 -4 57.99 2.90 -5 0 -4 60.39 3.40 5 0 4 60.39 3.20 5 0 4 63.19 4.50 -6 0 -4 445.86 19.60 -6 0 -4 457.75 18.20 6 0 4 432.36 19.00 -7 0 -4 84.39 3.10 -7 0 -4 82.09 2.50 -8 0 -4 215.08 7.50 -8 0 -4 221.48 6.50 -8 0 -4 223.78 6.70 -9 0 -4 203.78 5.90 -9 0 -4 205.98 6.10 -9 0 -4 193.18 5.90 -9 0 -4 197.68 6.80 -10 0 -4 14.40 1.00 -10 0 -4 14.00 0.70 -10 0 -4 13.80 0.70 10 0 4 13.00 0.70 -11 0 -4 13.80 0.80 -11 0 -4 14.20 0.60 11 0 4 14.30 0.60 12 -1 -4 93.09 3.00 -12 1 4 92.39 2.80 -12 1 4 85.49 2.90 11 -1 -4 441.46 13.90 -11 1 4 455.75 13.00 -11 1 4 432.26 13.00 -11 1 4 449.06 14.00 10 -1 -4 112.19 3.60 10 -1 -4 101.29 3.90 -10 1 4 105.49 3.40 -10 1 4 105.79 3.60 -10 1 4 104.29 3.40 9 -1 -4 4.80 0.70 9 -1 -4 3.20 0.50 -9 1 4 2.80 1.20 -9 1 4 5.80 0.80 -9 1 4 6.30 0.80 8 -1 -4 79.89 2.90 -8 1 4 71.89 3.50 -8 1 4 72.59 4.40 7 -1 -4 11.70 0.70 6 -1 -4 1432.26 51.69 -6 1 4 1432.16 53.79 5 -1 -4 895.81 32.50 -5 1 4 900.01 32.40 -5 1 4 891.31 33.70 4 -1 -4 93.79 3.80 4 -1 -4 93.19 5.50 -4 1 4 95.79 5.60 -4 1 4 90.39 3.70 -4 1 4 89.59 3.80 3 -1 -4 1701.13 83.59 3 -1 -4 1743.83 60.09 3 -1 -4 1559.94 87.09 3 -1 -4 1640.84 66.39 -3 1 4 1745.73 68.69 -3 1 4 1575.74 83.39 -3 1 4 1812.12 61.19 2 -1 -4 6384.06 250.87 2 -1 -4 6281.77 226.98 2 -1 -4 6894.31 250.87 -2 1 4 5570.54 313.67 -2 1 4 6371.46 226.98 -2 1 4 6542.05 314.47 -2 1 4 6614.54 365.06 -2 1 4 5709.33 326.87 -2 1 4 6719.23 259.57 1 -1 -4 30.60 1.70 1 -1 -4 31.70 1.40 1 -1 -4 32.70 1.60 -1 1 4 32.70 2.20 -1 1 4 28.20 2.20 -1 1 4 28.90 2.00 -1 1 4 33.80 1.60 0 -1 -4 182.58 7.50 0 -1 -4 195.48 7.50 0 1 4 177.18 9.90 -1 -1 -4 234.68 9.90 -1 -1 -4 221.18 9.10 -1 -1 -4 222.88 9.10 1 1 4 227.08 12.10 -2 -1 -4 120.99 5.10 -2 -1 -4 123.09 5.10 -2 -1 -4 129.69 5.80 2 1 4 126.79 6.90 -3 -1 -4 1947.11 75.89 -3 -1 -4 2027.20 80.29 -3 -1 -4 1876.11 74.19 -3 -1 -4 1905.01 75.89 -3 -1 -4 1927.11 74.29 3 1 4 1968.00 110.99 3 1 4 1812.52 110.89 3 1 4 1979.10 78.79 -4 -1 -4 753.32 30.80 -4 -1 -4 825.92 31.70 -4 -1 -4 817.42 33.80 -4 -1 -4 799.82 31.60 4 1 4 791.32 32.90 4 1 4 796.52 46.20 -5 -1 -4 578.44 23.00 -5 -1 -4 579.24 23.10 -5 -1 -4 578.94 24.80 5 1 4 555.34 33.70 5 1 4 574.94 24.00 -6 -1 -4 47.70 3.20 -7 -1 -4 84.69 3.20 -8 -1 -4 482.85 15.60 -8 -1 -4 473.65 14.20 -8 -1 -4 476.05 13.70 -9 -1 -4 108.99 4.10 -9 -1 -4 113.39 3.40 -9 -1 -4 117.09 3.50 -10 -1 -4 19.50 0.80 -10 -1 -4 19.60 1.10 -10 -1 -4 18.10 0.80 -13 2 4 35.90 1.30 12 -2 -4 215.88 6.80 -12 2 4 216.58 6.40 -12 2 4 215.08 6.80 11 -2 -4 5.70 0.50 -11 2 4 5.00 0.50 -11 2 4 3.80 0.60 -11 2 4 4.40 0.60 10 -2 -4 183.58 6.70 10 -2 -4 188.08 6.10 -10 2 4 197.48 6.20 -10 2 4 187.08 5.80 9 -2 -4 244.78 8.20 9 -2 -4 236.08 7.40 -9 2 4 231.08 7.60 -9 2 4 215.48 11.10 8 -2 -4 221.68 7.80 7 -2 -4 105.39 3.80 7 -2 -4 105.19 4.70 6 -2 -4 149.09 6.00 -6 2 4 142.09 5.90 5 -2 -4 111.99 4.60 -5 2 4 113.29 4.60 -5 2 4 112.19 4.50 4 -2 -4 247.68 9.70 -4 2 4 259.17 14.60 -4 2 4 253.67 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4 314.47 17.10 -3 3 4 311.17 13.00 2 -3 -4 573.04 22.80 2 -3 -4 577.94 22.90 2 -3 -4 592.84 20.50 -2 3 4 548.95 23.50 -2 3 4 601.14 28.90 -2 3 4 577.14 30.30 -2 3 4 536.95 33.10 1 -3 -4 22.10 1.00 1 -3 -4 24.40 1.00 1 -3 -4 22.00 1.20 1 -3 -4 22.80 1.20 -1 3 4 22.90 1.50 -1 3 4 24.50 1.10 -1 3 4 22.80 1.70 -1 3 4 22.40 1.10 0 -3 -4 1341.57 69.49 0 3 4 1288.37 67.59 -1 -3 -4 2355.56 123.69 -2 -3 -4 3.90 1.40 -2 -3 -4 2.50 0.80 -3 -3 -4 1337.97 68.99 -3 -3 -4 1259.97 54.29 -3 -3 -4 1276.97 49.70 -4 -3 -4 857.91 32.60 -4 -3 -4 822.72 36.10 4 3 4 815.52 48.80 4 3 4 880.91 34.80 -5 -3 -4 85.79 4.90 -5 -3 -4 87.09 2.70 5 3 4 84.79 5.90 -6 -3 -4 88.79 4.30 -6 -3 -4 91.69 3.30 -6 -3 -4 90.59 5.30 -7 -3 -4 194.48 6.60 -7 -3 -4 192.38 5.70 -8 -3 -4 6.30 0.50 -8 -3 -4 6.80 0.50 -8 -3 -4 7.10 0.80 -9 -3 -4 97.99 3.40 -9 -3 -4 95.69 2.80 -9 -3 -4 91.09 2.90 -10 -3 -4 31.30 1.00 -13 4 4 16.10 0.70 -13 4 4 17.40 0.70 -12 4 4 282.57 8.70 -12 4 4 274.87 8.20 -12 4 4 265.17 8.20 11 -4 -4 101.59 3.90 11 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2.10 -10 8 4 56.99 2.10 9 -8 -4 16.00 0.80 9 -8 -4 13.10 0.90 -9 8 4 15.00 0.90 8 -8 -4 38.90 1.60 8 -8 -4 40.30 1.70 -8 8 4 41.50 1.60 7 -8 -4 211.48 7.40 7 -8 -4 207.28 6.30 6 -8 -4 35.80 1.60 6 -8 -4 37.30 1.70 5 -8 -4 399.96 13.70 5 -8 -4 405.76 14.40 -5 8 4 386.46 17.10 4 -8 -4 712.03 28.50 4 -8 -4 724.73 25.00 -4 8 4 673.23 29.30 3 -8 -4 12.20 0.70 3 -8 -4 12.70 1.00 3 -8 -4 11.40 0.90 -3 8 4 11.30 1.00 2 -8 -4 5.40 0.50 2 -8 -4 4.90 0.70 2 -8 -4 6.30 0.40 -2 8 4 6.30 0.70 -2 8 4 3.50 1.00 1 -8 -4 433.56 15.90 1 -8 -4 443.16 16.90 1 -8 -4 420.86 15.40 -1 8 4 440.06 18.00 0 -8 -4 543.25 20.10 0 -8 -4 587.54 21.30 0 8 4 522.95 31.80 -1 -8 -4 236.68 9.00 -2 -8 -4 714.33 27.00 -2 -8 -4 774.82 31.20 -3 -8 -4 8.60 1.40 -4 -8 -4 170.78 8.00 -5 -8 -4 246.88 7.40 -5 -8 -4 259.07 11.30 -5 -8 -4 271.97 7.90 -6 -8 -4 16.00 0.60 -6 -8 -4 16.20 0.60 -6 -8 -4 17.00 1.20 -7 -8 -4 1.40 0.20 12 -9 -4 134.59 4.40 -12 9 4 132.39 4.40 11 -9 -4 131.99 4.70 11 -9 -4 125.89 4.30 10 -9 -4 38.70 1.50 10 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13 4 7.10 0.60 8 -13 -4 269.37 7.60 8 -13 -4 264.47 9.30 -8 13 4 259.37 8.40 7 -13 -4 9.10 0.50 7 -13 -4 9.90 0.50 -7 13 4 9.10 0.70 -7 13 4 9.00 0.70 6 -13 -4 8.70 0.50 6 -13 -4 9.90 0.50 5 -13 -4 60.69 2.00 5 -13 -4 62.59 2.00 5 -13 -4 63.89 2.60 4 -13 -4 104.79 3.10 4 -13 -4 100.79 3.10 3 -13 -4 157.98 4.60 2 -13 -4 338.47 9.70 1 -13 -4 65.39 1.90 1 -13 -4 62.39 2.10 0 -13 -4 21.30 0.80 0 -13 -4 21.30 0.70 10 -14 -4 65.79 2.00 -10 14 4 66.19 2.20 9 -14 -4 239.98 7.10 9 -14 -4 240.38 6.90 -9 14 4 237.48 7.60 8 -14 -4 247.78 7.10 -8 14 4 244.98 7.80 7 -14 -4 50.19 1.70 7 -14 -4 53.99 1.70 -7 14 4 52.69 1.90 6 -14 -4 5.20 0.40 6 -14 -4 5.70 0.40 5 -14 -4 66.89 2.20 5 -14 -4 74.29 2.20 4 -14 -4 182.78 5.20 4 -14 -4 178.38 5.30 3 -14 -4 15.30 0.60 2 -14 -4 12.40 0.50 1 -14 -4 3.00 0.20 8 -15 -4 2.50 0.30 -8 15 4 3.10 0.40 7 -15 -4 199.28 5.60 7 -15 -4 192.98 5.60 -7 15 4 188.98 6.20 6 -15 -4 2.20 0.30 6 -15 -4 2.10 0.30 5 -15 -4 12.60 0.50 5 -15 -4 13.50 0.50 4 -15 -4 1.20 0.20 3 -15 -4 14.10 0.50 2 -15 -4 35.70 1.10 -5 18 -5 7.80 0.50 -6 18 -5 93.29 3.10 1 -17 5 34.00 1.10 1 -17 5 34.50 1.10 2 -17 5 154.88 4.50 2 -17 5 155.88 4.50 -3 17 -5 81.09 2.70 3 -17 5 80.09 2.40 3 -17 5 77.79 2.40 -4 17 -5 4.60 0.60 4 -17 5 3.00 0.30 -5 17 -5 19.50 0.90 5 -17 5 20.00 0.80 -6 17 -5 303.67 9.70 6 -17 5 312.37 9.20 6 -17 5 307.27 8.80 -7 17 -5 203.58 6.50 7 -17 5 201.78 5.90 7 -17 5 208.98 6.20 -8 17 -5 12.30 0.60 8 -17 5 12.10 0.50 -1 -16 5 187.28 5.40 0 -16 5 49.99 1.60 0 -16 5 51.89 1.60 1 -16 5 2.80 0.30 1 -16 5 2.90 0.30 2 -16 5 56.59 1.80 2 -16 5 56.99 1.80 -3 16 -5 81.29 2.80 3 -16 5 86.99 2.60 3 -16 5 80.89 2.50 -4 16 -5 57.89 2.10 4 -16 5 58.39 1.90 4 -16 5 60.79 1.90 -5 16 -5 390.96 12.30 5 -16 5 382.26 11.20 5 -16 5 401.36 11.80 -6 16 -5 20.40 1.00 6 -16 5 19.30 0.80 6 -16 5 19.60 0.80 -7 16 -5 1.50 0.50 7 -16 5 1.70 0.30 7 -16 5 1.30 0.40 7 -16 5 1.00 0.30 -8 16 -5 0.70 0.50 8 -16 5 0.80 0.40 8 -16 5 0.60 0.30 8 -16 5 0.30 0.20 9 -16 5 1.00 0.20 9 -16 5 0.70 0.30 9 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119.09 3.80 -4 -14 5 56.49 2.70 -4 -14 5 58.09 1.70 -3 -14 5 5.10 0.70 -3 -14 5 5.30 0.30 -3 -14 5 4.60 0.30 -2 -14 5 61.29 3.00 -2 -14 5 60.99 1.90 -2 -14 5 58.79 1.90 -1 -14 5 11.40 1.10 -1 -14 5 12.70 0.60 -1 -14 5 11.50 0.60 0 -14 5 152.58 4.60 0 -14 5 157.48 4.60 0 -14 5 157.68 5.90 0 -14 5 151.38 6.90 1 -14 5 39.70 1.40 1 -14 5 40.20 1.40 1 -14 5 42.90 1.40 1 -14 5 41.90 1.90 2 -14 5 42.40 1.50 2 -14 5 42.70 2.10 2 -14 5 44.30 1.50 2 -14 5 43.90 1.60 -3 14 -5 49.20 2.00 3 -14 5 48.10 2.30 3 -14 5 49.00 1.70 3 -14 5 50.09 1.80 3 -14 5 51.69 1.70 3 -14 5 49.60 1.60 -4 14 -5 135.49 4.50 4 -14 5 131.99 4.00 4 -14 5 134.59 4.00 4 -14 5 130.09 4.20 4 -14 5 132.99 4.00 4 -14 5 133.69 5.20 -5 14 -5 84.19 2.90 5 -14 5 84.29 2.60 5 -14 5 82.19 2.60 5 -14 5 83.89 2.60 5 -14 5 85.99 2.60 5 -14 5 78.89 2.80 -6 14 -5 335.47 10.30 6 -14 5 329.87 9.60 6 -14 5 312.97 9.50 6 -14 5 315.97 10.20 6 -14 5 322.67 9.30 -7 14 -5 3.10 0.70 7 -14 5 3.70 0.50 7 -14 5 2.20 0.30 7 -14 5 3.70 0.50 -8 14 -5 7.70 0.60 8 -14 5 9.10 0.60 8 -14 5 8.50 0.50 8 -14 5 8.30 0.60 9 -14 5 3.20 0.50 9 -14 5 3.20 0.50 9 -14 5 2.30 0.40 10 -14 5 25.40 1.00 10 -14 5 27.70 1.10 10 -14 5 25.50 1.00 11 -14 5 16.40 0.60 11 -14 5 16.30 0.70 -5 -13 5 88.69 4.00 -5 -13 5 90.29 2.70 -4 -13 5 3.10 0.70 -4 -13 5 2.80 0.30 -3 -13 5 0.70 0.50 -3 -13 5 0.70 0.30 -3 -13 5 0.70 0.30 -2 -13 5 3.00 0.40 -2 -13 5 3.50 0.30 -2 -13 5 3.30 0.70 -1 -13 5 170.38 7.90 -1 -13 5 183.48 5.30 -1 -13 5 184.08 6.80 -1 -13 5 179.38 5.30 0 -13 5 228.98 8.30 0 -13 5 212.48 9.70 0 -13 5 226.58 6.70 0 -13 5 225.88 6.50 0 -13 5 219.78 6.50 1 -13 5 133.39 4.10 1 -13 5 134.79 5.10 1 -13 5 131.19 4.00 1 -13 5 130.59 4.00 2 -13 5 177.48 5.70 2 -13 5 184.58 6.90 2 -13 5 180.18 5.40 2 -13 5 181.78 5.30 2 -13 5 183.88 5.40 2 -13 5 184.78 5.40 -3 13 -5 17.80 1.20 3 -13 5 20.70 0.90 3 -13 5 18.70 0.70 3 -13 5 17.60 1.20 3 -13 5 18.80 0.80 3 -13 5 19.30 1.00 3 -13 5 19.20 0.80 3 -13 5 19.90 0.90 -4 13 -5 16.00 0.90 4 -13 5 17.70 0.70 4 -13 5 15.60 1.00 4 -13 5 17.90 0.80 4 -13 5 16.30 0.90 4 -13 5 18.10 0.80 4 -13 5 17.20 0.80 4 -13 5 17.50 0.70 -5 13 -5 39.60 1.60 5 -13 5 39.40 1.50 5 -13 5 40.20 1.40 5 -13 5 39.10 1.40 5 -13 5 41.20 1.40 -6 13 -5 502.25 15.20 6 -13 5 484.95 15.20 6 -13 5 476.45 13.80 6 -13 5 470.85 14.20 6 -13 5 479.05 14.10 -7 13 -5 13.10 0.80 7 -13 5 14.80 0.70 7 -13 5 13.30 0.70 7 -13 5 11.80 0.80 7 -13 5 13.90 0.80 7 -13 5 13.50 0.70 -8 13 -5 572.94 17.80 8 -13 5 585.44 17.80 8 -13 5 547.05 19.50 9 -13 5 116.59 3.90 9 -13 5 117.79 4.30 -10 13 -5 18.80 1.00 10 -13 5 22.90 1.00 -11 13 -5 99.19 3.40 11 -13 5 102.09 3.30 -6 -12 5 0.40 0.40 -6 -12 5 0.50 0.20 -5 -12 5 2.90 0.60 -5 -12 5 2.30 0.30 -4 -12 5 0.70 0.50 -4 -12 5 1.00 0.30 -4 -12 5 1.30 0.30 -3 -12 5 11.20 0.50 -3 -12 5 11.30 0.60 -3 -12 5 10.60 0.80 -3 -12 5 10.50 1.10 -2 -12 5 257.77 7.40 -2 -12 5 240.28 8.70 -2 -12 5 255.87 9.30 -2 -12 5 253.87 7.30 -2 -12 5 254.97 11.00 -1 -12 5 84.19 2.60 -1 -12 5 85.69 2.70 -1 -12 5 86.09 3.40 -1 -12 5 84.19 2.60 -1 -12 5 87.49 4.10 -1 -12 5 78.19 3.20 0 -12 5 100.89 3.20 0 -12 5 103.79 3.00 0 -12 5 94.29 4.60 0 -12 5 100.79 3.00 0 -12 5 98.29 3.90 1 -12 5 692.43 18.70 1 -12 5 634.54 23.70 1 -12 5 656.83 19.10 2 -12 5 53.39 1.70 2 -12 5 53.39 1.70 2 -12 5 49.99 2.30 3 -12 5 113.79 3.80 3 -12 5 115.09 3.60 3 -12 5 116.69 4.60 3 -12 5 119.39 3.50 4 -12 5 38.90 1.40 4 -12 5 35.90 1.40 4 -12 5 38.00 1.80 4 -12 5 35.80 1.30 -5 12 -5 44.20 1.70 5 -12 5 42.20 1.60 5 -12 5 43.90 1.50 5 -12 5 40.80 1.50 5 -12 5 42.40 1.80 -6 12 -5 73.09 2.60 6 -12 5 73.29 2.90 6 -12 5 73.39 2.60 -7 12 -5 308.27 9.80 7 -12 5 311.47 9.80 7 -12 5 300.17 10.70 -8 12 -5 9.10 0.70 8 -12 5 8.60 0.70 8 -12 5 8.90 0.70 9 -12 5 33.90 1.50 9 -12 5 37.10 1.50 -10 12 -5 10.70 0.80 10 -12 5 12.50 0.70 -11 12 -5 45.90 1.70 11 -12 5 45.90 1.70 -7 -11 5 0.70 0.20 -6 -11 5 1.60 0.30 -6 -11 5 0.50 0.50 -5 -11 5 93.79 2.80 -5 -11 5 88.29 4.30 -5 -11 5 91.69 3.40 -4 -11 5 12.80 1.20 -4 -11 5 13.60 0.70 -3 -11 5 17.90 1.30 -3 -11 5 17.20 0.70 -3 -11 5 17.00 0.70 -3 -11 5 17.10 1.10 -3 -11 5 16.30 0.60 -2 -11 5 3.40 0.60 -2 -11 5 2.70 0.30 -2 -11 5 3.20 0.40 -2 -11 5 2.60 0.50 -2 -11 5 3.10 0.40 -2 -11 5 2.40 0.70 -1 -11 5 21.70 0.90 -1 -11 5 20.80 1.20 -1 -11 5 21.90 1.40 -1 -11 5 21.60 1.10 -1 -11 5 22.20 0.70 0 11 -5 243.68 9.70 0 -11 5 252.27 7.30 0 -11 5 251.47 9.20 -1 11 -5 1416.06 50.59 1 -11 5 1470.05 51.09 -2 11 -5 160.48 6.70 2 -11 5 168.18 6.20 -3 11 -5 3.20 0.80 3 -11 5 2.80 0.50 -4 11 -5 211.28 8.60 4 -11 5 225.18 7.70 4 -11 5 211.88 8.50 -5 11 -5 51.49 3.00 5 -11 5 58.89 2.30 6 -11 5 275.47 9.60 6 -11 5 272.97 8.80 -7 11 -5 36.90 1.50 7 -11 5 36.60 1.50 7 -11 5 37.10 1.60 -8 11 -5 65.69 2.40 8 -11 5 68.39 2.40 8 -11 5 66.59 2.60 -9 11 -5 206.08 6.80 9 -11 5 206.58 6.70 -10 11 -5 53.99 2.00 10 -11 5 51.59 2.00 -11 11 -5 123.39 4.00 11 -11 5 116.19 4.00 -12 11 -5 1.20 0.40 -7 -10 5 74.99 3.50 -7 -10 5 76.29 2.30 -6 -10 5 212.48 7.20 -6 -10 5 207.18 6.10 -6 -10 5 201.48 9.00 -5 -10 5 22.60 1.40 -5 -10 5 26.30 1.00 -5 -10 5 26.50 1.90 -4 -10 5 23.80 1.70 -4 -10 5 21.90 1.30 -4 -10 5 23.30 0.90 -4 -10 5 23.90 0.90 -3 -10 5 2.80 0.80 -3 -10 5 3.00 0.30 -3 -10 5 3.80 0.50 -3 -10 5 3.00 0.50 -3 -10 5 2.70 0.30 -3 -10 5 2.60 0.60 2 10 -5 61.29 3.60 -2 -10 5 65.19 2.70 -2 -10 5 62.69 1.90 -2 -10 5 62.39 2.00 -2 -10 5 66.09 3.20 -2 -10 5 64.59 2.50 1 10 -5 580.24 20.90 -1 -10 5 557.24 19.10 -1 -10 5 587.04 20.60 0 10 -5 896.81 32.20 0 10 -5 876.51 37.80 0 -10 5 950.50 32.30 -1 10 -5 183.68 7.20 -1 10 -5 180.88 10.30 -1 10 -5 170.08 8.20 -1 10 -5 178.58 8.20 1 -10 5 189.78 6.70 -2 10 -5 2.90 0.70 -2 10 -5 2.50 0.90 2 -10 5 4.40 0.60 2 -10 5 4.30 0.50 -3 10 -5 216.38 8.60 3 -10 5 224.28 8.20 3 -10 5 215.48 8.60 3 -10 5 228.08 7.80 -4 10 -5 0.80 0.50 4 -10 5 0.60 0.40 4 -10 5 0.90 0.50 -5 10 -5 99.39 4.50 5 -10 5 102.99 3.70 5 -10 5 102.09 4.60 -6 10 -5 12.20 1.30 -6 10 -5 11.20 1.40 6 -10 5 12.20 0.70 7 -10 5 291.37 10.20 7 -10 5 291.67 9.30 -8 10 -5 0.10 0.60 8 -10 5 1.70 0.50 8 -10 5 0.50 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19.10 1 6 -9 50.99 3.40 1 6 -9 51.29 2.50 1 6 -9 48.40 2.60 -1 -6 9 48.90 2.50 -1 -6 9 46.90 2.30 0 6 -9 350.26 13.40 0 6 -9 340.47 12.80 0 6 -9 364.96 18.10 0 -6 9 347.57 13.60 0 -6 9 360.66 13.40 -1 6 -9 98.79 4.30 -1 6 -9 95.69 4.10 -1 6 -9 101.59 5.80 1 -6 9 102.59 4.50 1 -6 9 99.09 4.10 -2 6 -9 1733.13 63.29 -2 6 -9 1852.11 86.09 -2 6 -9 1693.03 60.99 2 -6 9 1727.33 66.09 2 -6 9 1810.72 63.59 -3 6 -9 1437.26 52.99 -3 6 -9 1521.45 74.69 -3 6 -9 1558.14 54.99 3 -6 9 1522.55 57.29 3 -6 9 1592.14 55.59 -4 6 -9 863.11 31.00 -4 6 -9 875.81 32.00 -4 6 -9 917.41 45.30 4 -6 9 855.11 33.20 -5 6 -9 11.20 1.00 5 -6 9 11.20 0.90 -6 6 -9 4.40 0.60 -6 6 -9 2.60 0.70 -6 6 -9 3.20 0.70 6 -6 9 1.50 0.50 -7 6 -9 273.47 8.00 -7 6 -9 266.47 8.60 -7 6 -9 255.67 10.20 -7 6 -9 277.57 9.00 -7 6 -9 277.47 7.90 7 -6 9 263.07 8.50 7 -6 9 267.47 10.70 -8 6 -9 173.18 5.90 -8 6 -9 167.68 5.10 -8 6 -9 160.68 5.40 -8 6 -9 170.28 5.10 8 -6 9 163.48 5.40 -9 6 -9 1.20 0.50 -9 6 -9 0.90 0.40 -9 6 -9 2.50 1.00 -9 6 -9 2.00 0.40 9 -6 9 1.80 0.50 -10 6 -9 40.30 1.40 -10 6 -9 42.80 1.70 -10 6 -9 39.30 1.50 10 -6 9 41.70 1.50 -11 6 -9 2.50 0.40 11 -6 9 2.60 0.30 10 5 -9 771.72 23.80 -10 -5 9 758.22 24.70 -10 -5 9 771.22 22.90 9 5 -9 167.58 5.50 9 5 -9 173.88 6.10 -9 -5 9 168.88 5.10 -9 -5 9 169.18 5.90 -9 -5 9 173.08 5.40 8 5 -9 90.89 3.60 8 5 -9 98.89 3.30 -8 -5 9 95.99 3.50 -8 -5 9 97.39 3.00 -8 -5 9 93.29 3.20 -8 -5 9 95.99 3.10 7 5 -9 45.10 1.90 7 5 -9 46.80 1.70 -7 -5 9 43.80 1.90 -7 -5 9 45.30 2.00 -7 -5 9 44.70 1.60 -7 -5 9 46.70 1.70 -7 -5 9 44.90 1.80 -7 -5 9 43.20 3.30 -7 -5 9 44.40 1.60 -7 -5 9 45.50 2.50 6 5 -9 202.28 7.00 -6 -5 9 203.48 8.00 -6 -5 9 190.48 6.30 -6 -5 9 199.78 6.80 -6 -5 9 183.78 5.90 -6 -5 9 181.48 9.50 5 5 -9 624.24 20.60 5 5 -9 584.54 21.80 -5 -5 9 573.94 22.20 -5 -5 9 591.94 26.10 -5 -5 9 615.24 23.00 -5 -5 9 603.24 20.00 4 5 -9 1475.65 53.99 4 5 -9 1662.43 76.49 4 5 -9 1560.44 52.49 -4 -5 9 1516.95 55.89 -4 -5 9 1524.35 58.19 3 5 -9 15.20 1.30 3 5 -9 16.20 1.40 3 5 -9 17.80 1.80 -3 -5 9 14.90 1.10 2 5 -9 59.99 3.90 2 5 -9 56.09 2.80 2 5 -9 61.39 2.90 -2 -5 9 56.99 2.60 -2 -5 9 58.99 2.90 1 5 -9 7.50 1.10 1 5 -9 6.70 0.80 1 5 -9 7.60 0.90 -1 -5 9 8.00 0.70 -1 -5 9 6.30 0.80 0 5 -9 377.26 18.20 0 5 -9 348.37 12.90 0 5 -9 356.16 13.40 0 -5 9 362.66 13.50 0 -5 9 337.17 13.70 -1 5 -9 664.43 24.20 -1 5 -9 627.84 23.20 -1 5 -9 678.03 32.80 1 -5 9 664.03 24.30 1 -5 9 663.73 25.00 -2 5 -9 2609.64 136.79 -2 5 -9 2737.33 130.39 -2 5 -9 2700.83 96.29 -2 5 -9 2631.84 92.49 2 -5 9 2739.53 101.09 -3 5 -9 49.40 2.40 -3 5 -9 51.19 3.10 3 -5 9 45.30 2.20 -4 5 -9 206.78 7.90 4 -5 9 199.78 8.10 -5 5 -9 290.47 11.30 -5 5 -9 308.67 11.30 5 -5 9 304.17 11.80 -6 5 -9 262.77 7.80 -6 5 -9 250.27 9.90 -6 5 -9 262.07 8.80 6 -5 9 274.07 10.40 -7 5 -9 1.60 1.10 -7 5 -9 2.10 0.80 -7 5 -9 1.40 0.50 -7 5 -9 2.00 0.60 -7 5 -9 2.00 0.50 7 -5 9 0.50 0.40 7 -5 9 3.20 0.50 -8 5 -9 17.90 0.90 -8 5 -9 19.90 1.40 -8 5 -9 19.60 0.80 -8 5 -9 19.20 0.90 8 -5 9 18.60 0.90 -9 5 -9 42.80 1.50 -9 5 -9 40.60 1.50 -9 5 -9 40.40 1.30 -9 5 -9 40.70 1.80 9 -5 9 40.80 1.50 -10 5 -9 70.19 2.60 -10 5 -9 66.59 2.20 -10 5 -9 67.19 2.20 10 -5 9 67.69 2.30 -11 5 -9 5.30 0.40 11 -5 9 6.70 0.40 11 4 -9 12.50 0.60 -11 -4 9 12.20 0.60 10 4 -9 120.69 4.60 10 4 -9 128.39 4.20 -10 -4 9 124.89 4.10 -10 -4 9 134.99 3.90 -10 -4 9 130.69 4.40 9 4 -9 169.78 6.10 9 4 -9 172.38 5.50 -9 -4 9 163.48 5.50 -9 -4 9 173.28 5.10 -9 -4 9 167.78 5.80 -9 -4 9 171.48 5.20 8 4 -9 220.68 6.90 8 4 -9 207.28 7.60 -8 -4 9 212.38 7.00 -8 -4 9 218.78 6.50 -8 -4 9 214.08 6.50 -8 -4 9 215.98 7.30 7 4 -9 49.00 1.80 7 4 -9 50.59 2.10 -7 -4 9 52.89 2.60 -7 -4 9 49.90 1.90 -7 -4 9 42.10 3.30 -7 -4 9 45.20 1.80 -7 -4 9 49.20 2.10 -7 -4 9 51.39 2.00 6 4 -9 25.40 1.90 6 4 -9 26.40 1.30 -6 -4 9 25.40 1.20 -6 -4 9 27.80 1.70 -6 -4 9 23.10 2.20 5 4 -9 21.70 1.10 5 4 -9 22.80 1.70 -5 -4 9 21.20 1.60 -5 -4 9 21.40 1.90 -5 -4 9 22.00 1.40 4 4 -9 55.49 2.90 4 4 -9 60.09 3.00 4 4 -9 56.89 3.90 -4 -4 9 56.39 2.70 -4 -4 9 58.99 2.90 3 4 -9 329.97 12.50 3 4 -9 342.87 13.10 3 4 -9 360.86 17.70 -3 -4 9 338.07 13.20 -3 -4 9 340.67 13.00 2 4 -9 264.67 10.40 2 4 -9 279.77 14.10 2 4 -9 259.67 10.00 -2 -4 9 271.57 10.40 -2 -4 9 277.97 10.50 1 4 -9 15.80 1.50 1 4 -9 13.60 1.00 1 4 -9 16.00 1.20 -1 -4 9 17.50 1.30 -1 -4 9 15.20 1.00 0 4 -9 130.69 7.00 0 4 -9 124.09 4.90 0 4 -9 127.79 5.20 0 -4 9 125.39 5.30 0 -4 9 125.49 5.10 -1 4 -9 596.14 29.20 -1 4 -9 579.14 30.40 -1 4 -9 584.24 21.50 1 -4 9 622.04 22.30 1 -4 9 552.54 24.70 -2 4 -9 64.29 2.90 -2 4 -9 65.29 3.80 2 -4 9 61.59 3.50 2 -4 9 68.09 2.80 -3 4 -9 297.47 10.50 -3 4 -9 286.57 10.60 3 -4 9 280.17 10.90 3 -4 9 259.87 12.40 -4 4 -9 257.47 9.60 -4 4 -9 264.67 9.60 4 -4 9 261.37 10.00 4 -4 9 237.58 11.50 -5 4 -9 714.83 25.80 5 -4 9 703.73 27.00 -6 4 -9 112.89 3.40 -6 4 -9 104.09 4.50 -6 4 -9 108.09 3.90 -6 4 -9 110.39 3.40 6 -4 9 111.79 4.70 -7 4 -9 189.48 5.70 -7 4 -9 199.98 5.80 -7 4 -9 191.88 5.70 -7 4 -9 197.78 6.00 -7 4 -9 193.18 6.60 7 -4 9 184.58 7.90 7 -4 9 191.28 6.20 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0.80 -2 -2 20 16.40 0.80 1 2 -20 12.50 0.60 -1 -2 20 8.30 0.70 0 2 -20 111.19 3.30 0 -2 20 108.89 3.60 -1 2 -20 2.40 0.30 1 -2 20 2.30 0.50 -6 -1 20 43.10 1.50 5 1 -20 46.30 1.50 -5 -1 20 48.20 1.70 4 1 -20 3.40 0.30 -4 -1 20 3.30 0.50 3 1 -20 12.70 0.60 -3 -1 20 13.00 0.70 2 1 -20 2.50 0.40 -2 -1 20 0.80 0.60 1 1 -20 59.89 1.90 -1 -1 20 60.59 2.10 0 1 -20 11.60 0.50 0 -1 20 12.50 0.80 -6 0 20 16.80 0.70 5 0 -20 24.90 0.90 -5 0 20 25.20 1.00 4 0 -20 128.69 3.80 -4 0 20 130.79 4.20 3 0 -20 1.50 0.20 -3 0 20 0.60 0.40 2 0 -20 27.70 0.90 -2 0 20 27.80 1.10 1 0 -20 2.40 0.20 -1 0 20 2.30 0.50 -5 1 20 135.79 4.30 4 -1 -20 12.60 0.50 -4 1 20 12.90 0.60 3 -1 -20 1.40 0.20 -3 1 20 2.30 0.50 2 -1 -20 9.10 0.40 -1 -10 21 6.80 0.60 -2 -9 21 2.40 0.50 1 9 -21 1.70 0.30 0 9 -21 38.10 1.20 -1 9 -21 11.70 0.50 -1 9 -21 12.10 0.50 -2 9 -21 21.70 0.80 2 8 -21 1.00 0.30 1 8 -21 31.30 1.10 0 8 -21 1.70 0.30 0 8 -21 1.30 0.30 -1 8 -21 1.00 0.30 1 -8 21 0.30 0.30 -2 8 -21 30.70 1.00 2 -8 21 28.70 1.10 3 7 -21 101.99 3.10 2 7 -21 5.90 0.40 1 7 -21 2.90 0.40 1 7 -21 2.80 0.30 -1 -7 21 2.30 0.30 0 7 -21 3.70 0.40 0 7 -21 3.00 0.20 0 -7 21 2.80 0.40 -1 7 -21 62.09 2.00 1 -7 21 60.69 2.10 -2 7 -21 2.90 0.20 2 -7 21 3.00 0.30 4 6 -21 42.30 1.40 3 6 -21 1.60 0.30 2 6 -21 52.29 1.60 2 6 -21 53.99 1.80 -2 -6 21 49.70 2.00 -2 -6 21 53.69 1.80 1 6 -21 5.80 0.30 1 6 -21 6.80 0.40 -1 -6 21 6.70 0.70 0 6 -21 48.60 1.60 0 -6 21 47.70 1.70 -1 6 -21 101.89 3.00 -1 6 -21 95.89 2.90 1 -6 21 99.69 3.20 2 -6 21 0.50 0.30 4 5 -21 113.99 3.40 3 5 -21 102.89 3.00 -3 -5 21 103.99 3.30 -3 -5 21 96.99 3.60 2 5 -21 61.79 1.90 2 5 -21 53.79 1.70 -2 -5 21 53.29 2.10 -2 -5 21 59.79 2.00 1 5 -21 76.59 2.40 1 5 -21 74.59 2.30 -1 -5 21 78.99 2.60 0 5 -21 54.19 1.70 0 5 -21 53.79 1.70 0 -5 21 56.89 2.00 -1 5 -21 212.38 6.20 1 -5 21 220.48 6.80 4 4 -21 185.38 5.40 -4 -4 21 185.78 5.90 -3 -4 21 65.79 2.50 -3 -4 21 71.39 2.30 2 4 -21 7.10 0.50 -2 -4 21 7.00 0.60 1 4 -21 1.40 0.30 -1 -4 21 1.70 0.50 0 4 -21 73.99 2.30 0 -4 21 78.19 2.60 1 -4 21 13.70 0.70 -4 -3 21 0.40 0.40 3 3 -21 2.20 0.30 -3 -3 21 1.90 0.50 2 3 -21 4.10 0.40 -2 -3 21 3.50 0.40 1 3 -21 15.10 0.70 -1 -3 21 14.70 0.80 0 3 -21 42.30 1.30 0 -3 21 36.50 1.40 -4 -2 21 5.20 0.40 3 2 -21 117.79 3.50 -3 -2 21 118.39 3.80 2 2 -21 17.50 0.70 -2 -2 21 14.10 0.70 1 2 -21 12.80 0.50 -4 -1 21 50.69 1.70 -3 -1 21 7.00 0.50 1 7 -22 7.20 0.40 0 7 -22 40.10 1.30 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 83798 _olex2_date_sample_data_collection 2020-02-29 _olex2_date_sample_submission 2020-01-25 _olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems' _olex2_exptl_crystal_mounting_method 'The crystal was mounted on a mylar loop in perfluoroether oil' _olex2_submission_original_sample_id MEM040_150K _olex2_submission_special_instructions 'No special instructions were received' 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 Cu1 Cu 0.68526(4) 0.66124(3) 0.33507(2) 0.02092(15) Uani 1 1 d . . . . . P2 P 0.53014(7) 0.68447(5) 0.40018(4) 0.01990(18) Uani 1 1 d . . . . . P1 P 0.61337(7) 0.60206(5) 0.19955(4) 0.02095(18) Uani 1 1 d . . . . . P3 P 0.83012(8) 1.14197(6) 0.34197(5) 0.0306(2) Uani 1 1 d . . . . . Cl2 Cl 0.9943(2) 0.92275(16) 0.05968(11) 0.0531(5) Uani 0.5 1 d . . P . . Cl1 Cl 1.0205(2) 0.87799(15) 0.20274(10) 0.0534(5) Uani 0.5 1 d . . P . . O1 O 0.3769(2) 0.51944(15) 0.24823(12) 0.0227(4) Uani 1 1 d . . . . . F1 F 0.6909(2) 1.09400(18) 0.27811(14) 0.0492(6) Uani 1 1 d . . . . . F2 F 0.9702(2) 1.19078(19) 0.40567(14) 0.0474(5) Uani 1 1 d . . . . . F3 F 0.7784(2) 1.2140(2) 0.40424(15) 0.0539(6) Uani 1 1 d . . . . . F4 F 0.8831(2) 1.22848(19) 0.30709(16) 0.0533(6) Uani 1 1 d . . . . . F5 F 0.8842(3) 1.0721(2) 0.27955(17) 0.0587(7) Uani 1 1 d . . . . . F6 F 0.7785(3) 1.0564(2) 0.37670(19) 0.0640(7) Uani 1 1 d . . . . . N2 N 0.8629(3) 0.7832(2) 0.37679(16) 0.0282(6) Uani 1 1 d . . . . . N1 N 0.8051(3) 0.5926(2) 0.36767(15) 0.0280(6) Uani 1 1 d . . . . . C39 C 0.5839(3) 0.7570(2) 0.50864(17) 0.0217(6) Uani 1 1 d . . . . . C18 C 0.5303(3) 0.6713(2) 0.16193(17) 0.0230(6) Uani 1 1 d . . . . . C45 C 0.4468(3) 0.7566(2) 0.36708(18) 0.0227(6) Uani 1 1 d . . . . . C25 C 0.3866(3) 0.4413(2) 0.18557(17) 0.0227(6) Uani 1 1 d . . . . . C32 C 0.3368(3) 0.4916(2) 0.31033(18) 0.0220(6) Uani 1 1 d . . . . . C40 C 0.4976(3) 0.7850(2) 0.55323(19) 0.0264(6) Uani 1 1 d . . . . . H40 H 0.408118 0.765638 0.526935 0.032 Uiso 1 1 calc R . . . . C42 C 0.6727(3) 0.8710(2) 0.67354(19) 0.0283(6) Uani 1 1 d . . . . . H42 H 0.703156 0.909693 0.729896 0.034 Uiso 1 1 calc R . . . . C26 C 0.2942(3) 0.3415(2) 0.16082(18) 0.0253(6) Uani 1 1 d . . . . . C33 C 0.3976(3) 0.5651(2) 0.38786(18) 0.0227(6) Uani 1 1 d . . . . . C44 C 0.7156(3) 0.7880(2) 0.54783(18) 0.0236(6) Uani 1 1 d . . . . . H44 H 0.774897 0.769728 0.518148 0.028 Uiso 1 1 calc R . . . . C20 C 0.3518(4) 0.6795(3) 0.0794(2) 0.0361(8) Uani 1 1 d . . . . . H20 H 0.268167 0.645767 0.041420 0.043 Uiso 1 1 calc R . . . . C24 C 0.4934(3) 0.4694(2) 0.15236(17) 0.0227(6) Uani 1 1 d . . . . . C19 C 0.4087(3) 0.6231(3) 0.1067(2) 0.0289(6) Uani 1 1 d . . . . . H19 H 0.363769 0.550883 0.087299 0.035 Uiso 1 1 calc R . . . . C12 C 0.7407(3) 0.6002(2) 0.14379(18) 0.0248(6) Uani 1 1 d . . . . . C31 C 0.2429(3) 0.3938(2) 0.29192(19) 0.0249(6) Uani 1 1 d . . . . . C28 C 0.4150(4) 0.2917(2) 0.06293(19) 0.0312(7) Uani 1 1 d . . . . . H28 H 0.424210 0.239578 0.020124 0.037 Uiso 1 1 calc R . . . . C29 C 0.5064(3) 0.3927(2) 0.08960(18) 0.0276(6) Uani 1 1 d . . . . . H29 H 0.577303 0.409036 0.064951 0.033 Uiso 1 1 calc R . . . . C34 C 0.3639(3) 0.5369(2) 0.45107(19) 0.0276(6) Uani 1 1 d . . . . . H34 H 0.404263 0.584223 0.505118 0.033 Uiso 1 1 calc R . . . . C46 C 0.3210(3) 0.7136(2) 0.3165(2) 0.0317(7) Uani 1 1 d . . . . . H46 H 0.269347 0.642584 0.299887 0.038 Uiso 1 1 calc R . . . . C27 C 0.3108(3) 0.2667(2) 0.09834(19) 0.0299(7) Uani 1 1 d . . . . . H27 H 0.249908 0.197560 0.079633 0.036 Uiso 1 1 calc R . . . . C13 C 0.7419(3) 0.6263(3) 0.07679(19) 0.0304(7) Uani 1 1 d . . . . . H13 H 0.673878 0.644912 0.058121 0.036 Uiso 1 1 calc R . . . . C41 C 0.5427(3) 0.8411(2) 0.63589(19) 0.0285(6) Uani 1 1 d . . . . . H41 H 0.483528 0.858504 0.666175 0.034 Uiso 1 1 calc R . . . . C43 C 0.7605(3) 0.8455(2) 0.6302(2) 0.0283(6) Uani 1 1 d . . . . . H43 H 0.850498 0.867213 0.656681 0.034 Uiso 1 1 calc R . . . . C7 C 0.9669(3) 0.7635(3) 0.40010(19) 0.0315(7) Uani 1 1 d . . . . . C30 C 0.1818(3) 0.3234(2) 0.20282(19) 0.0279(6) Uani 1 1 d . . . . . C23 C 0.5931(4) 0.7772(3) 0.1904(2) 0.0362(8) Uani 1 1 d . . . . . H23 H 0.675921 0.811390 0.229113 0.043 Uiso 1 1 calc R . . . . C11 C 0.8844(3) 0.8788(3) 0.3805(2) 0.0316(7) Uani 1 1 d . . . . . H11 H 0.810680 0.893440 0.364709 0.038 Uiso 1 1 calc R . . . . C35 C 0.2710(3) 0.4392(2) 0.4348(2) 0.0296(7) Uani 1 1 d . . . . . H35 H 0.248611 0.420753 0.478184 0.036 Uiso 1 1 calc R . . . . C21 C 0.4160(4) 0.7846(3) 0.1071(2) 0.0415(9) Uani 1 1 d . . . . . H21 H 0.377316 0.822879 0.087660 0.050 Uiso 1 1 calc R . . . . C15 C 0.9404(4) 0.5980(3) 0.0637(2) 0.0419(9) Uani 1 1 d . . . . . H15 H 1.009050 0.597779 0.036807 0.050 Uiso 1 1 calc R . . . . C17 C 0.8410(4) 0.5726(3) 0.1694(2) 0.0362(8) Uani 1 1 d . . . . . H17 H 0.841716 0.554660 0.214886 0.043 Uiso 1 1 calc R . . . . C6 C 0.9369(3) 0.6573(3) 0.39415(19) 0.0339(7) Uani 1 1 d . . . . . C36 C 0.2108(3) 0.3685(2) 0.3564(2) 0.0283(7) Uani 1 1 d . . . . . H36 H 0.147355 0.302548 0.346550 0.034 Uiso 1 1 calc R . . . . C50 C 0.5197(3) 0.8612(3) 0.3907(2) 0.0349(7) Uani 1 1 d . . . . . H50 H 0.606301 0.891884 0.425072 0.042 Uiso 1 1 calc R . . . . C38 C 0.1160(4) 0.2112(2) 0.1906(2) 0.0365(8) Uani 1 1 d . . . . . H38A H 0.077035 0.169081 0.133102 0.055 Uiso 1 1 calc GR . . . . H38B H 0.046372 0.202969 0.219576 0.055 Uiso 1 1 calc GR . . . . H38C H 0.182212 0.189409 0.211117 0.055 Uiso 1 1 calc GR . . . . C14 C 0.8421(4) 0.6253(3) 0.0374(2) 0.0385(8) Uani 1 1 d . . . . . H14 H 0.842543 0.643562 -0.007946 0.046 Uiso 1 1 calc R . . . . C2 C 0.7700(4) 0.4952(3) 0.35947(19) 0.0351(8) Uani 1 1 d . . . . . C48 C 0.3431(4) 0.8769(3) 0.3140(2) 0.0404(8) Uani 1 1 d . . . . . H48 H 0.307545 0.917400 0.295413 0.048 Uiso 1 1 calc R . . . . C10 C 1.0097(4) 0.9560(3) 0.4064(2) 0.0397(8) Uani 1 1 d . . . . . H10 H 1.022360 1.022500 0.408459 0.048 Uiso 1 1 calc R . . . . C16 C 0.9397(4) 0.5709(3) 0.1294(2) 0.0449(9) Uani 1 1 d . . . . . H16 H 1.007030 0.551012 0.147016 0.054 Uiso 1 1 calc R . . . . C37 C 0.0775(3) 0.3578(3) 0.1700(2) 0.0359(7) Uani 1 1 d . . . . . H37A H 0.120186 0.429572 0.177245 0.054 Uiso 1 1 calc GR . . . . H37B H 0.008279 0.350487 0.199314 0.054 Uiso 1 1 calc GR . . . . H37C H 0.038100 0.315106 0.112696 0.054 Uiso 1 1 calc GR . . . . C1 C 0.6274(4) 0.4291(3) 0.3303(2) 0.0414(8) Uani 1 1 d . . . . . H1A H 0.578358 0.462076 0.363357 0.062 Uiso 1 1 calc GR . . . . H1B H 0.613083 0.362951 0.333930 0.062 Uiso 1 1 calc GR . . . . H1C H 0.596114 0.418383 0.274197 0.062 Uiso 1 1 calc GR . . . . C22 C 0.5361(5) 0.8335(3) 0.1629(2) 0.0459(9) Uani 1 1 d . . . . . H22 H 0.580005 0.905877 0.182669 0.055 Uiso 1 1 calc R . . . . C49 C 0.4677(4) 0.9210(3) 0.3649(3) 0.0424(9) Uani 1 1 d . . . . . H49 H 0.517872 0.992395 0.382281 0.051 Uiso 1 1 calc R . . . . C3 C 0.8647(5) 0.4578(3) 0.3778(3) 0.0501(10) Uani 1 1 d . . . . . H3 H 0.838764 0.388530 0.372202 0.060 Uiso 1 1 calc R . . . . C8 C 1.0957(4) 0.8392(3) 0.4272(2) 0.0424(9) Uani 1 1 d . . . . . H8 H 1.168634 0.824340 0.443974 0.051 Uiso 1 1 calc R . . . . C47 C 0.2702(4) 0.7735(3) 0.2901(2) 0.0403(8) Uani 1 1 d . . . . . H47 H 0.184096 0.743119 0.255088 0.048 Uiso 1 1 calc R . . . . C9 C 1.1151(4) 0.9338(3) 0.4291(2) 0.0441(9) Uani 1 1 d . . . . . H9 H 1.202223 0.985087 0.446373 0.053 Uiso 1 1 calc R . . . . O2 O 0.6725(5) 0.0964(3) 0.0130(3) 0.0851(12) Uani 1 1 d . . . . . C5 C 1.0332(4) 0.6230(3) 0.4126(3) 0.0502(10) Uani 1 1 d . . . . . H5 H 1.123909 0.668110 0.431013 0.060 Uiso 1 1 calc R . . . . C4 C 0.9963(5) 0.5232(4) 0.4041(3) 0.0611(13) Uani 1 1 d . . . . . H4 H 1.061792 0.498844 0.416420 0.073 Uiso 1 1 calc R . . . . C51 C 0.6635(8) -0.0037(5) -0.0248(4) 0.0852(18) Uani 1 1 d . . . . . H51A H 0.596093 -0.050761 -0.008637 0.102 Uiso 1 1 calc R . . . . H51B H 0.749626 -0.007449 -0.008562 0.102 Uiso 1 1 calc R . . . . C55 C 0.9247(7) 0.9018(5) 0.1357(4) 0.0330(14) Uani 0.5 1 d . . P . . H55A H 0.838341 0.842816 0.111357 0.040 Uiso 0.5 1 calc R . P . . H55B H 0.907660 0.962568 0.165711 0.040 Uiso 0.5 1 calc R . P . . C53 C 0.7196(7) 0.1340(6) 0.0974(4) 0.0859(18) Uani 1 1 d . . . . . H53A H 0.812664 0.141792 0.111709 0.103 Uiso 1 1 calc R . . . . H53B H 0.665572 0.085877 0.118655 0.103 Uiso 1 1 calc R . . . . C54 C 0.7095(7) 0.2365(6) 0.1325(4) 0.099(2) Uani 1 1 d . . . . . H54A H 0.756850 0.270840 0.189489 0.148 Uiso 1 1 calc GR . . . . H54B H 0.616206 0.226272 0.127165 0.148 Uiso 1 1 calc GR . . . . H54C H 0.748822 0.278913 0.103626 0.148 Uiso 1 1 calc GR . . . . C52 C 0.6248(10) -0.0352(6) -0.1161(4) 0.104(3) Uani 1 1 d . . . . . H52A H 0.543662 -0.025337 -0.131070 0.156 Uiso 1 1 calc GR . . . . H52B H 0.609634 -0.107403 -0.143196 0.156 Uiso 1 1 calc GR . . . . H52C H 0.696286 0.007058 -0.132283 0.156 Uiso 1 1 calc GR . . . . 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 Cu1 0.0240(2) 0.0205(2) 0.0213(2) 0.00898(18) 0.00779(17) 0.01088(18) P2 0.0229(4) 0.0171(3) 0.0207(4) 0.0069(3) 0.0079(3) 0.0087(3) P1 0.0245(4) 0.0215(4) 0.0194(4) 0.0095(3) 0.0079(3) 0.0098(3) P3 0.0258(4) 0.0275(4) 0.0396(5) 0.0114(4) 0.0129(3) 0.0120(3) Cl2 0.0572(11) 0.0481(10) 0.0280(8) 0.0142(8) 0.0038(8) -0.0076(9) Cl1 0.0688(13) 0.0411(10) 0.0226(8) 0.0069(7) -0.0111(8) 0.0012(9) O1 0.0301(11) 0.0177(9) 0.0222(10) 0.0092(8) 0.0113(8) 0.0089(8) F1 0.0361(11) 0.0495(13) 0.0476(13) 0.0046(11) 0.0046(10) 0.0156(10) F2 0.0294(10) 0.0602(14) 0.0530(13) 0.0222(11) 0.0108(9) 0.0176(10) F3 0.0394(12) 0.0601(15) 0.0503(13) 0.0001(12) 0.0139(10) 0.0256(11) F4 0.0524(14) 0.0475(13) 0.0715(16) 0.0352(13) 0.0208(12) 0.0199(11) F5 0.0588(15) 0.0545(14) 0.0648(16) 0.0083(12) 0.0245(13) 0.0363(13) F6 0.0537(15) 0.0555(15) 0.091(2) 0.0470(15) 0.0226(14) 0.0110(12) N2 0.0287(13) 0.0290(14) 0.0239(13) 0.0080(11) 0.0095(10) 0.0092(11) N1 0.0419(15) 0.0335(14) 0.0190(12) 0.0114(11) 0.0115(11) 0.0252(12) C39 0.0271(14) 0.0175(13) 0.0217(14) 0.0071(11) 0.0087(12) 0.0097(11) C18 0.0289(15) 0.0249(14) 0.0200(13) 0.0108(12) 0.0099(12) 0.0130(12) C45 0.0253(14) 0.0232(14) 0.0247(14) 0.0112(12) 0.0110(12) 0.0121(12) C25 0.0308(15) 0.0205(14) 0.0201(13) 0.0086(11) 0.0075(11) 0.0129(12) C32 0.0265(14) 0.0218(14) 0.0242(14) 0.0123(12) 0.0118(12) 0.0123(12) C40 0.0266(15) 0.0258(15) 0.0284(15) 0.0087(13) 0.0096(12) 0.0131(12) C42 0.0382(17) 0.0231(15) 0.0218(14) 0.0067(12) 0.0069(13) 0.0123(13) C26 0.0310(15) 0.0224(15) 0.0226(14) 0.0103(12) 0.0061(12) 0.0094(12) C33 0.0261(14) 0.0184(13) 0.0273(15) 0.0103(12) 0.0115(12) 0.0104(12) C44 0.0263(14) 0.0225(14) 0.0269(15) 0.0117(12) 0.0104(12) 0.0123(12) C20 0.0354(18) 0.047(2) 0.0358(18) 0.0203(16) 0.0101(14) 0.0230(16) C24 0.0294(15) 0.0199(14) 0.0213(14) 0.0105(11) 0.0067(11) 0.0100(12) C19 0.0291(16) 0.0281(16) 0.0314(16) 0.0131(13) 0.0089(13) 0.0116(13) C12 0.0251(14) 0.0251(15) 0.0211(14) 0.0065(12) 0.0076(11) 0.0083(12) C31 0.0284(15) 0.0208(14) 0.0274(15) 0.0103(12) 0.0094(12) 0.0102(12) C28 0.0449(19) 0.0243(15) 0.0244(15) 0.0052(13) 0.0099(14) 0.0173(14) C29 0.0370(17) 0.0292(16) 0.0223(14) 0.0112(13) 0.0118(13) 0.0173(14) C34 0.0369(17) 0.0253(15) 0.0242(15) 0.0105(13) 0.0125(13) 0.0142(13) C46 0.0280(16) 0.0235(15) 0.0386(18) 0.0067(14) 0.0036(13) 0.0108(13) C27 0.0410(18) 0.0197(14) 0.0251(15) 0.0075(12) 0.0053(13) 0.0096(13) C13 0.0301(16) 0.0356(17) 0.0270(16) 0.0142(14) 0.0107(13) 0.0116(14) C41 0.0357(17) 0.0240(15) 0.0286(16) 0.0080(13) 0.0136(13) 0.0155(13) C43 0.0277(15) 0.0262(15) 0.0309(16) 0.0116(13) 0.0058(13) 0.0105(13) C7 0.0338(17) 0.0386(18) 0.0218(15) 0.0082(13) 0.0096(13) 0.0164(14) C30 0.0330(16) 0.0225(15) 0.0252(15) 0.0096(13) 0.0083(13) 0.0065(13) C23 0.0446(19) 0.0249(16) 0.0331(17) 0.0109(14) 0.0015(15) 0.0095(15) C11 0.0321(16) 0.0276(16) 0.0331(17) 0.0113(14) 0.0100(13) 0.0094(13) C35 0.0417(18) 0.0262(15) 0.0278(16) 0.0158(13) 0.0171(14) 0.0136(14) C21 0.062(2) 0.041(2) 0.0379(19) 0.0202(16) 0.0150(17) 0.0343(19) C15 0.0340(18) 0.045(2) 0.0395(19) 0.0071(17) 0.0202(16) 0.0129(16) C17 0.0405(19) 0.047(2) 0.0285(16) 0.0143(15) 0.0113(14) 0.0252(17) C6 0.0360(17) 0.049(2) 0.0230(15) 0.0116(14) 0.0085(13) 0.0260(16) C36 0.0342(16) 0.0201(14) 0.0329(16) 0.0132(13) 0.0135(13) 0.0089(13) C50 0.0285(16) 0.0264(16) 0.050(2) 0.0178(15) 0.0067(15) 0.0089(13) C38 0.047(2) 0.0224(16) 0.0289(16) 0.0079(13) 0.0102(15) 0.0024(14) C14 0.0417(19) 0.0403(19) 0.0331(18) 0.0151(15) 0.0200(15) 0.0114(16) C2 0.058(2) 0.0347(18) 0.0236(15) 0.0125(14) 0.0132(15) 0.0289(17) C48 0.045(2) 0.041(2) 0.051(2) 0.0251(18) 0.0147(17) 0.0287(17) C10 0.0398(19) 0.0319(18) 0.0379(19) 0.0107(15) 0.0103(15) 0.0053(15) C16 0.0369(19) 0.055(2) 0.044(2) 0.0118(18) 0.0120(16) 0.0271(18) C37 0.0306(17) 0.0405(19) 0.0344(18) 0.0152(15) 0.0063(14) 0.0111(15) C1 0.063(2) 0.0313(18) 0.0395(19) 0.0194(16) 0.0128(17) 0.0239(17) C22 0.070(3) 0.0256(17) 0.042(2) 0.0142(16) 0.0083(19) 0.0208(18) C49 0.040(2) 0.0265(17) 0.066(3) 0.0244(18) 0.0154(18) 0.0124(15) C3 0.072(3) 0.043(2) 0.045(2) 0.0124(18) 0.009(2) 0.040(2) C8 0.0300(17) 0.054(2) 0.0384(19) 0.0119(17) 0.0082(15) 0.0163(17) C47 0.0362(18) 0.0375(19) 0.047(2) 0.0112(16) 0.0009(16) 0.0219(16) C9 0.0300(18) 0.046(2) 0.040(2) 0.0099(17) 0.0072(15) 0.0027(16) O2 0.115(3) 0.085(3) 0.072(2) 0.034(2) 0.020(2) 0.057(3) C5 0.045(2) 0.052(2) 0.055(2) 0.014(2) 0.0046(19) 0.0302(19) C4 0.066(3) 0.063(3) 0.064(3) 0.018(2) 0.004(2) 0.048(3) C51 0.114(5) 0.084(4) 0.097(5) 0.050(4) 0.043(4) 0.065(4) C55 0.044(4) 0.022(3) 0.028(3) 0.003(3) 0.018(3) 0.011(3) C53 0.082(4) 0.114(5) 0.072(4) 0.035(4) 0.010(3) 0.054(4) C54 0.091(5) 0.110(5) 0.085(4) 0.014(4) -0.004(4) 0.059(4) C52 0.171(8) 0.080(4) 0.085(5) 0.034(4) 0.051(5) 0.069(5) 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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 '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' O O 0.0492 0.0322 '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' 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 P2 Cu1 P1 113.43(3) . . ? N2 Cu1 P2 114.95(8) . . ? N2 Cu1 P1 111.20(8) . . ? N2 Cu1 N1 80.75(11) . . ? N1 Cu1 P2 121.04(8) . . ? N1 Cu1 P1 111.30(7) . . ? C39 P2 Cu1 117.71(10) . . ? C39 P2 C45 101.53(13) . . ? C39 P2 C33 103.90(13) . . ? C45 P2 Cu1 113.28(9) . . ? C33 P2 Cu1 113.66(9) . . ? C33 P2 C45 105.27(14) . . ? C18 P1 Cu1 115.88(10) . . ? C24 P1 Cu1 114.41(9) . . ? C24 P1 C18 103.31(14) . . ? C24 P1 C12 102.27(14) . . ? C12 P1 Cu1 115.71(10) . . ? C12 P1 C18 103.48(14) . . ? F1 P3 F2 179.50(15) . . ? F1 P3 F4 89.78(14) . . ? F2 P3 F4 89.72(14) . . ? F3 P3 F1 89.88(13) . . ? F3 P3 F2 90.14(13) . . ? F3 P3 F4 89.65(15) . . ? F3 P3 F5 178.71(16) . . ? F5 P3 F1 90.63(14) . . ? F5 P3 F2 89.33(14) . . ? F5 P3 F4 89.17(15) . . ? F6 P3 F1 90.54(15) . . ? F6 P3 F2 89.96(14) . . ? F6 P3 F3 90.48(16) . . ? F6 P3 F4 179.66(16) . . ? F6 P3 F5 90.69(16) . . ? C25 O1 C32 114.2(2) . . ? C7 N2 Cu1 115.1(2) . . ? C7 N2 C11 118.5(3) . . ? C11 N2 Cu1 126.4(2) . . ? C6 N1 Cu1 112.4(2) . . ? C2 N1 Cu1 127.9(2) . . ? C2 N1 C6 119.5(3) . . ? C40 C39 P2 122.0(2) . . ? C44 C39 P2 118.8(2) . . ? C44 C39 C40 119.2(3) . . ? C19 C18 P1 123.1(2) . . ? C19 C18 C23 118.7(3) . . ? C23 C18 P1 118.2(2) . . ? C46 C45 P2 124.7(2) . . ? C46 C45 C50 118.3(3) . . ? C50 C45 P2 116.9(2) . . ? O1 C25 C26 119.8(3) . . ? O1 C25 C24 116.1(3) . . ? C26 C25 C24 124.0(3) . . ? C33 C32 O1 116.2(2) . . ? C33 C32 C31 124.4(3) . . ? C31 C32 O1 119.4(3) . . ? C41 C40 C39 120.2(3) . . ? C41 C42 C43 120.8(3) . . ? C25 C26 C30 117.6(3) . . ? C27 C26 C25 116.8(3) . . ? C27 C26 C30 125.6(3) . . ? C32 C33 P2 117.8(2) . . ? C32 C33 C34 117.0(3) . . ? C34 C33 P2 124.7(2) . . ? C43 C44 C39 120.3(3) . . ? C21 C20 C19 120.3(3) . . ? C25 C24 P1 117.5(2) . . ? C29 C24 P1 124.7(2) . . ? C29 C24 C25 117.6(3) . . ? C18 C19 C20 120.4(3) . . ? C13 C12 P1 122.6(2) . . ? C17 C12 P1 118.8(2) . . ? C17 C12 C13 118.6(3) . . ? C32 C31 C30 117.6(3) . . ? C32 C31 C36 117.0(3) . . ? C36 C31 C30 125.4(3) . . ? C27 C28 C29 120.7(3) . . ? C24 C29 C28 119.9(3) . . ? C35 C34 C33 120.1(3) . . ? C47 C46 C45 120.4(3) . . ? C28 C27 C26 121.0(3) . . ? C14 C13 C12 120.3(3) . . ? C42 C41 C40 119.9(3) . . ? C44 C43 C42 119.6(3) . . ? N2 C7 C6 115.8(3) . . ? N2 C7 C8 121.2(3) . . ? C8 C7 C6 123.0(3) . . ? C26 C30 C31 106.3(2) . . ? C26 C30 C37 109.3(3) . . ? C31 C30 C37 107.6(3) . . ? C38 C30 C26 111.8(3) . . ? C38 C30 C31 112.1(3) . . ? C38 C30 C37 109.6(3) . . ? C22 C23 C18 120.7(3) . . ? N2 C11 C10 122.5(3) . . ? C36 C35 C34 121.1(3) . . ? C22 C21 C20 119.8(3) . . ? C14 C15 C16 120.1(3) . . ? C16 C17 C12 120.7(3) . . ? N1 C6 C7 115.8(3) . . ? N1 C6 C5 120.9(4) . . ? C5 C6 C7 123.3(4) . . ? C35 C36 C31 120.4(3) . . ? C49 C50 C45 121.1(3) . . ? C15 C14 C13 120.2(3) . . ? N1 C2 C1 117.2(3) . . ? N1 C2 C3 121.2(4) . . ? C3 C2 C1 121.6(3) . . ? C49 C48 C47 119.6(3) . . ? C9 C10 C11 118.1(4) . . ? C15 C16 C17 120.1(4) . . ? C21 C22 C23 119.9(3) . . ? C48 C49 C50 119.9(3) . . ? C4 C3 C2 118.7(4) . . ? C9 C8 C7 119.3(4) . . ? C48 C47 C46 120.8(3) . . ? C8 C9 C10 120.4(4) . . ? C51 O2 C53 111.8(5) . . ? C4 C5 C6 119.2(4) . . ? C5 C4 C3 120.5(4) . . ? O2 C51 C52 108.7(5) . . ? Cl2 C55 Cl1 114.4(4) . . ? O2 C53 C54 107.3(5) . . ? 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 Cu1 P2 2.2508(8) . ? Cu1 P1 2.2677(8) . ? Cu1 N2 2.040(3) . ? Cu1 N1 2.074(3) . ? P2 C39 1.824(3) . ? P2 C45 1.830(3) . ? P2 C33 1.828(3) . ? P1 C18 1.831(3) . ? P1 C24 1.828(3) . ? P1 C12 1.831(3) . ? P3 F1 1.595(2) . ? P3 F2 1.600(2) . ? P3 F3 1.594(2) . ? P3 F4 1.600(2) . ? P3 F5 1.594(2) . ? P3 F6 1.584(3) . ? Cl2 C55 1.725(7) . ? Cl1 C55 1.725(8) . ? O1 C25 1.387(3) . ? O1 C32 1.397(3) . ? N2 C7 1.337(4) . ? N2 C11 1.354(4) . ? N1 C6 1.377(5) . ? N1 C2 1.336(4) . ? C39 C40 1.402(4) . ? C39 C44 1.394(4) . ? C18 C19 1.383(4) . ? C18 C23 1.390(5) . ? C45 C46 1.386(4) . ? C45 C50 1.396(4) . ? C25 C26 1.392(4) . ? C25 C24 1.394(4) . ? C32 C33 1.389(4) . ? C32 C31 1.393(4) . ? C40 C41 1.392(5) . ? C42 C41 1.372(5) . ? C42 C43 1.393(5) . ? C26 C27 1.392(4) . ? C26 C30 1.527(4) . ? C33 C34 1.398(4) . ? C44 C43 1.390(5) . ? C20 C19 1.386(5) . ? C20 C21 1.381(6) . ? C24 C29 1.392(4) . ? C12 C13 1.398(4) . ? C12 C17 1.391(5) . ? C31 C30 1.534(4) . ? C31 C36 1.394(4) . ? C28 C29 1.397(5) . ? C28 C27 1.389(5) . ? C34 C35 1.395(5) . ? C46 C47 1.385(5) . ? C13 C14 1.389(5) . ? C7 C6 1.483(5) . ? C7 C8 1.402(5) . ? C30 C38 1.527(4) . ? C30 C37 1.547(5) . ? C23 C22 1.387(5) . ? C11 C10 1.385(5) . ? C35 C36 1.389(5) . ? C21 C22 1.375(6) . ? C15 C14 1.375(6) . ? C15 C16 1.383(6) . ? C17 C16 1.383(5) . ? C6 C5 1.383(5) . ? C50 C49 1.386(5) . ? C2 C1 1.477(6) . ? C2 C3 1.401(5) . ? C48 C49 1.377(6) . ? C48 C47 1.379(6) . ? C10 C9 1.371(6) . ? C3 C4 1.378(7) . ? C8 C9 1.354(6) . ? O2 C51 1.399(7) . ? O2 C53 1.414(7) . ? C5 C4 1.367(7) . ? C51 C52 1.534(10) . ? C53 C54 1.512(10) . ?