#------------------------------------------------------------------------------ #$Date: 2017-09-15 05:38:12 +0300 (Fri, 15 Sep 2017) $ #$Revision: 200914 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/42/7044229.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_7044229 loop_ _publ_author_name 'Bhat, Gulzar A.' 'Maqbool, Raihana' 'Dar, Aijaz' 'Hussain, Mahboob Ul' 'Murugavel, Ramaswamy' _publ_section_title ; Selective formation of discrete versus polymeric copper organophosphates: DNA cleavage and cytotoxic activity ; _journal_name_full 'Dalton Trans.' _journal_paper_doi 10.1039/C7DT02763J _journal_year 2017 _chemical_formula_sum 'C94 H122 Cl4 Cu3 N8 O24 P4' _chemical_formula_weight 2204.29 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2017-07-27 deposited with the CCDC. 2017-09-14 downloaded from the CCDC. ; _cell_angle_alpha 94.80(3) _cell_angle_beta 99.73(3) _cell_angle_gamma 111.01(3) _cell_formula_units_Z 1 _cell_length_a 10.260(2) _cell_length_b 14.003(3) _cell_length_c 19.176(4) _cell_measurement_reflns_used 8791 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 24.999 _cell_measurement_theta_min 3.078 _cell_volume 2503.5(11) _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r4' _computing_data_collection 'CrystalClear-SM Expert 2.0 r4' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r4' _computing_molecular_graphics diamond _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Rigaku Saturn724' _diffrn_measurement_method \w _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0840 _diffrn_reflns_av_unetI/netI 0.0666 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 48382 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 24.999 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_min 3.078 _exptl_absorpt_coefficient_mu 0.878 _exptl_absorpt_correction_T_max 0.924 _exptl_absorpt_correction_T_min 0.854 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'NUMABS (Rigaku, 1999)' _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.462 _exptl_crystal_description needles _exptl_crystal_F_000 1149 _exptl_crystal_size_max 0.230 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.090 _refine_diff_density_max 0.595 _refine_diff_density_min -0.733 _refine_diff_density_rms 0.101 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 637 _refine_ls_number_reflns 8791 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.085 _refine_ls_R_factor_all 0.0644 _refine_ls_R_factor_gt 0.0499 _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^)+(0.0584P)^2^+1.3113P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1194 _refine_ls_wR_factor_ref 0.1312 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7374 _reflns_number_total 8791 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt02763j2.cif _cod_data_source_block 3 _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'Multi-scan' changed to 'multi-scan' according to /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas ; _cod_original_cell_volume 2503.5(10) _cod_database_code 7044229 _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_min 0.824 _shelx_estimated_absorpt_t_max 0.925 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL gb_a.res in P-1 CELL 0.71073 10.2600 14.0030 19.1760 94.799 99.726 111.014 ZERR 1.00 0.0021 0.0028 0.0038 0.030 0.030 0.030 LATT 1 SFAC C H CL CU N O P UNIT 94 122 4 3 8 24 4 MERG 2 OMIT -3.00 50.00 OMIT -2 3 10 OMIT 0 -2 4 OMIT -3 7 6 OMIT 1 -4 4 OMIT 0 -9 11 OMIT 0 1 8 MORE -1 HTAB O2 O5 HTAB O11 O3 HTAB O10 O3 HTAB O9 O6 EQIV $1 -x+1, -y+1, -z+1 HTAB C4 O10_$1 HTAB C7 O10_$1 HTAB C1 O6 EQIV $2 x+1, y, z HTAB C9 O11_$2 HTAB C12 O3_$2 HTAB C20 O10_$1 HTAB C17 O11_$2 EQIV $3 -x+1, -y, -z HTAB C14 Cl2_$3 HTAB C46 O6 EQIV $4 -x+1, -y, -z+1 HTAB O12 O6_$4 HTAB O12 O9_$2 FMAP 2 PLAN 20 SIZE 0.090 0.150 0.230 ACTA 52.00 HTAB 2.00000 BOND $H CONF LIST 6 L.S. 40 TEMP -173.15 WGHT 0.058400 1.311300 FVAR 0.29886 CU1 4 0.538329 0.281702 0.350993 11.00000 0.01402 0.01203 = 0.01201 -0.00160 0.00319 0.00080 CU2 4 0.500000 0.000000 0.500000 10.50000 0.01615 0.01188 = 0.01602 0.00149 -0.00319 -0.00232 P2 7 0.327445 0.054823 0.362350 11.00000 0.01196 0.01005 = 0.01297 -0.00092 0.00040 -0.00027 P1 7 0.307357 0.340755 0.241107 11.00000 0.01599 0.01319 = 0.01547 0.00238 0.00228 0.00257 CL2 3 0.307500 -0.049212 -0.001257 11.00000 0.03586 0.05685 = 0.01653 -0.00121 0.00964 0.01485 CL1 3 0.417468 0.690818 -0.000492 11.00000 0.04569 0.04655 = 0.05091 0.03475 0.00695 0.01514 O5 6 0.378994 0.149013 0.323446 11.00000 0.01819 0.01193 = 0.01471 -0.00025 0.00103 0.00047 O1 6 0.432199 0.374647 0.303385 11.00000 0.02055 0.01161 = 0.01705 0.00135 0.00190 0.00379 O8 6 0.454436 0.041280 0.407639 11.00000 0.01458 0.01864 = 0.01534 0.00105 -0.00070 0.00176 O7 6 0.254279 -0.044843 0.299016 11.00000 0.01585 0.01038 = 0.01550 -0.00072 0.00298 -0.00065 O6 6 0.213273 0.055046 0.401405 11.00000 0.01761 0.01969 = 0.01985 -0.00049 0.00486 0.00279 O4 6 0.366683 0.352818 0.168195 11.00000 0.02385 0.01442 = 0.01912 0.00379 0.00516 0.00642 O2 6 0.227863 0.219654 0.228997 11.00000 0.02224 0.01561 = 0.02353 0.00527 -0.00276 -0.00229 AFIX 147 H2 2 0.269911 0.194610 0.259345 11.00000 -1.50000 AFIX 0 O3 6 0.202255 0.391484 0.242894 11.00000 0.02151 0.02688 = 0.02452 0.00856 0.00830 0.01117 N2 5 0.723656 0.394738 0.381841 11.00000 0.01736 0.01151 = 0.01014 -0.00044 0.00291 0.00214 N3 5 0.629081 0.267924 0.265174 11.00000 0.01760 0.01033 = 0.01466 0.00071 0.00209 0.00339 N4 5 1.336723 0.858111 0.473312 11.00000 0.01441 0.01636 = 0.01609 0.00291 0.00222 0.00247 O11 6 0.156238 0.567906 0.239396 11.00000 0.05008 0.03266 = 0.02771 0.00250 0.01740 0.02199 AFIX 147 H11 2 0.176498 0.514889 0.236115 11.00000 -1.50000 AFIX 0 O10 6 0.070828 0.319479 0.361088 11.00000 0.02955 0.02305 = 0.03188 -0.00091 0.00940 0.00597 AFIX 147 H10 2 0.115447 0.344532 0.329795 11.00000 -1.50000 AFIX 0 N1 5 0.526067 0.331010 0.452460 11.00000 0.01605 0.01386 = 0.01470 -0.00160 0.00381 0.00161 C6 1 0.748567 0.458043 0.443374 11.00000 0.01639 0.01583 = 0.01200 0.00163 0.00143 0.00576 C5 1 0.636772 0.420807 0.485246 11.00000 0.01752 0.01404 = 0.01550 0.00287 0.00366 0.00538 C11 1 0.764351 0.336910 0.271505 11.00000 0.01675 0.01107 = 0.01551 0.00184 0.00179 0.00555 O9 6 -0.072815 -0.043017 0.395118 11.00000 0.02811 0.04697 = 0.06849 0.01704 0.01384 0.01129 AFIX 147 H9A 2 0.009396 0.002252 0.399142 11.00000 -1.50000 AFIX 0 C38 1 0.163039 -0.032229 0.178388 11.00000 0.01572 0.00960 = 0.01486 -0.00455 0.00146 -0.00210 C4 1 0.641987 0.470972 0.551285 11.00000 0.01984 0.01107 = 0.01879 -0.00127 0.00473 0.00072 AFIX 43 H4 2 0.720089 0.533435 0.572783 11.00000 -1.20000 AFIX 0 C35 1 0.394910 -0.066542 0.137040 11.00000 0.01813 0.02253 = 0.02635 -0.00468 0.00735 0.00455 AFIX 43 H35 2 0.470399 -0.080607 0.121661 11.00000 -1.20000 AFIX 0 C33 1 0.271131 -0.044849 0.228383 11.00000 0.01690 0.01071 = 0.01402 -0.00155 0.00218 -0.00003 C22 1 0.507334 0.520815 0.144446 11.00000 0.02188 0.01679 = 0.02132 0.00248 0.01083 0.00748 C16 1 1.099471 0.669193 0.437817 11.00000 0.01300 0.01294 = 0.01667 0.00385 0.00127 0.00406 C39 1 0.031523 -0.024845 0.201731 11.00000 0.01442 0.01854 = 0.02088 -0.00197 0.00173 0.00222 AFIX 13 H39 2 0.063882 0.021919 0.248878 11.00000 -1.20000 AFIX 0 C7 1 0.870091 0.548041 0.462657 11.00000 0.01472 0.01459 = 0.01165 0.00061 0.00331 0.00256 AFIX 43 H7 2 0.885854 0.593498 0.505585 11.00000 -1.20000 AFIX 0 C1 1 0.419440 0.291067 0.486625 11.00000 0.02001 0.01453 = 0.02125 -0.00386 0.00689 -0.00149 AFIX 43 H1 2 0.341492 0.228882 0.464432 11.00000 -1.20000 AFIX 0 C9 1 0.942271 0.503114 0.355113 11.00000 0.01375 0.01754 = 0.01448 0.00381 0.00289 0.00402 AFIX 43 H9 2 1.008148 0.516712 0.324343 11.00000 -1.20000 AFIX 0 C34 1 0.386261 -0.063243 0.208958 11.00000 0.01615 0.01161 = 0.02057 -0.00038 0.00288 0.00134 C12 1 0.841806 0.335618 0.219250 11.00000 0.01765 0.01999 = 0.01815 -0.00011 0.00392 0.00382 AFIX 43 H12 2 0.937764 0.383097 0.225642 11.00000 -1.20000 AFIX 0 C10 1 0.816503 0.414537 0.338036 11.00000 0.01595 0.01197 = 0.01544 -0.00070 0.00325 0.00490 C15 1 0.565164 0.199593 0.204521 11.00000 0.01875 0.01325 = 0.01816 0.00018 0.00329 0.00135 AFIX 43 H15 2 0.469243 0.152651 0.199323 11.00000 -1.20000 AFIX 0 C8 1 0.969867 0.571815 0.418514 11.00000 0.01300 0.01495 = 0.01450 0.00322 -0.00026 0.00332 C19 1 1.255488 0.821912 0.520833 11.00000 0.01444 0.02428 = 0.01635 -0.00407 -0.00180 0.00201 AFIX 43 H19 2 1.280130 0.861713 0.567113 11.00000 -1.20000 AFIX 0 C20 1 1.138781 0.730248 0.505588 11.00000 0.01775 0.01804 = 0.01607 0.00431 0.00526 0.00356 AFIX 43 H20 2 1.084569 0.708092 0.540890 11.00000 -1.20000 AFIX 0 C37 1 0.178366 -0.032664 0.108148 11.00000 0.01377 0.02198 = 0.01835 -0.00163 -0.00188 0.00091 AFIX 43 H37 2 0.109846 -0.021524 0.073299 11.00000 -1.20000 AFIX 0 C42 1 0.499633 -0.080258 0.263126 11.00000 0.02155 0.02138 = 0.02254 0.00186 0.00597 0.00983 AFIX 13 H42 2 0.475009 -0.072283 0.310985 11.00000 -1.20000 AFIX 0 C13 1 0.776268 0.263341 0.157129 11.00000 0.02622 0.02103 = 0.01944 0.00331 0.00953 0.00944 AFIX 43 H13 2 0.827240 0.260289 0.120543 11.00000 -1.20000 AFIX 0 C18 1 1.302060 0.798715 0.409370 11.00000 0.02334 0.01874 = 0.01841 0.00405 0.00808 0.00372 AFIX 43 H18 2 1.360115 0.822076 0.375757 11.00000 -1.20000 AFIX 0 C17 1 1.186656 0.705341 0.389425 11.00000 0.02344 0.02138 = 0.01225 -0.00051 0.00533 0.00230 AFIX 43 H17 2 1.166840 0.666169 0.343304 11.00000 -1.20000 AFIX 0 C21 1 0.378636 0.433812 0.129637 11.00000 0.02155 0.01919 = 0.01521 0.00071 0.00887 0.00483 C30 1 0.633569 0.530183 0.202185 11.00000 0.01884 0.02129 = 0.01807 0.00467 0.00402 0.00223 AFIX 13 H30 2 0.609114 0.463629 0.222020 11.00000 -1.20000 AFIX 0 C14 1 0.635663 0.195811 0.149251 11.00000 0.03251 0.01851 = 0.01404 -0.00193 0.00677 0.00912 AFIX 43 H14 2 0.588124 0.147510 0.106518 11.00000 -1.20000 AFIX 0 C3 1 0.530979 0.428391 0.585617 11.00000 0.03155 0.02159 = 0.01532 -0.00391 0.00909 0.00489 AFIX 43 H3 2 0.531938 0.461583 0.631090 11.00000 -1.20000 AFIX 0 C36 1 0.293405 -0.049300 0.088271 11.00000 0.02316 0.02385 = 0.01120 -0.00203 0.00576 0.00202 C23 1 0.516998 0.599615 0.103189 11.00000 0.02601 0.02221 = 0.02138 0.00740 0.00829 0.00476 AFIX 43 H23 2 0.601819 0.660254 0.112436 11.00000 -1.20000 AFIX 0 C2 1 0.419717 0.338033 0.553547 11.00000 0.02660 0.02294 = 0.02787 -0.00093 0.01788 -0.00154 AFIX 43 H2A 2 0.343469 0.307748 0.576812 11.00000 -1.20000 AFIX 0 C26 1 0.264538 0.422181 0.072889 11.00000 0.02282 0.02891 = 0.01657 0.00389 0.00581 0.00969 C31 1 0.767857 0.546928 0.171712 11.00000 0.02574 0.03225 = 0.02783 0.00612 0.00986 0.01137 AFIX 137 H31A 2 0.749606 0.487858 0.135060 11.00000 -1.50000 H31B 2 0.847652 0.553114 0.210359 11.00000 -1.50000 H31C 2 0.792015 0.610499 0.150268 11.00000 -1.50000 AFIX 0 C40 1 -0.065752 -0.133015 0.212254 11.00000 0.01947 0.02661 = 0.04113 0.00341 0.00742 0.00219 AFIX 137 H40A 2 -0.097450 -0.180333 0.166703 11.00000 -1.50000 H40B 2 -0.149173 -0.128622 0.228636 11.00000 -1.50000 H40C 2 -0.012609 -0.159004 0.248126 11.00000 -1.50000 AFIX 0 C27 1 0.132637 0.321322 0.055653 11.00000 0.02412 0.03150 = 0.01844 0.00471 0.00189 0.00219 AFIX 13 H27 2 0.105576 0.303244 0.101955 11.00000 -1.20000 AFIX 0 C32 1 0.663828 0.617189 0.263619 11.00000 0.03310 0.03151 = 0.02204 0.00148 0.00269 0.01370 AFIX 137 H32A 2 0.698065 0.684129 0.246708 11.00000 -1.50000 H32B 2 0.736944 0.615138 0.302953 11.00000 -1.50000 H32C 2 0.575886 0.608117 0.280607 11.00000 -1.50000 AFIX 0 C25 1 0.279142 0.501654 0.032824 11.00000 0.02617 0.03726 = 0.01882 0.00969 0.00245 0.01369 AFIX 43 H25 2 0.203879 0.495915 -0.005752 11.00000 -1.20000 AFIX 0 C24 1 0.403663 0.589631 0.049023 11.00000 0.03180 0.02836 = 0.02599 0.01514 0.00954 0.01337 C41 1 -0.052115 0.019021 0.148526 11.00000 0.01820 0.03312 = 0.02652 -0.00059 0.00195 0.00966 AFIX 137 H41A 2 0.012716 0.085043 0.138888 11.00000 -1.50000 H41B 2 -0.127866 0.030187 0.168887 11.00000 -1.50000 H41C 2 -0.094758 -0.030074 0.103732 11.00000 -1.50000 AFIX 0 C29 1 0.002246 0.329739 0.007099 11.00000 0.02695 0.05290 = 0.03173 0.01158 -0.00356 0.00170 AFIX 137 H29A 2 -0.018900 0.386764 0.029027 11.00000 -1.50000 H29B 2 -0.080657 0.264737 0.001349 11.00000 -1.50000 H29C 2 0.023486 0.343061 -0.039914 11.00000 -1.50000 AFIX 0 C47 1 0.139152 0.599379 0.171410 11.00000 0.04679 0.04630 = 0.03178 0.01155 0.01558 0.01822 AFIX 137 H47A 2 0.063054 0.542952 0.137294 11.00000 -1.50000 H47B 2 0.228870 0.616569 0.154763 11.00000 -1.50000 H47C 2 0.113689 0.660433 0.175048 11.00000 -1.50000 AFIX 0 C43 1 0.648649 0.002051 0.268667 11.00000 0.02121 0.05515 = 0.04982 0.02487 0.00079 0.00781 AFIX 137 H43A 2 0.673502 0.001451 0.221526 11.00000 -1.50000 H43B 2 0.718571 -0.012966 0.302825 11.00000 -1.50000 H43C 2 0.649380 0.070420 0.285200 11.00000 -1.50000 AFIX 0 C28 1 0.168535 0.233166 0.021786 11.00000 0.04304 0.03261 = 0.03809 -0.00902 0.00307 0.00037 AFIX 137 H28A 2 0.195298 0.248656 -0.023902 11.00000 -1.50000 H28B 2 0.084828 0.168155 0.013440 11.00000 -1.50000 H28C 2 0.248409 0.226379 0.054189 11.00000 -1.50000 AFIX 0 C46 1 0.018566 0.209898 0.346402 11.00000 0.06076 0.03469 = 0.05965 0.00565 0.03491 0.01614 AFIX 137 H46A 2 -0.019753 0.186872 0.294845 11.00000 -1.50000 H46B 2 -0.057325 0.180536 0.372426 11.00000 -1.50000 H46C 2 0.096633 0.186501 0.361778 11.00000 -1.50000 AFIX 0 C44 1 0.498570 -0.189331 0.249387 11.00000 0.07242 0.03207 = 0.05479 0.00043 -0.00427 0.03319 AFIX 137 H44A 2 0.403272 -0.240019 0.249191 11.00000 -1.50000 H44B 2 0.569013 -0.197647 0.287254 11.00000 -1.50000 H44C 2 0.522741 -0.200474 0.202879 11.00000 -1.50000 AFIX 0 C45 1 -0.061724 -0.136202 0.413155 11.00000 0.03970 0.03366 = 0.09553 0.02084 0.02162 0.00814 AFIX 137 H45A 2 -0.142977 -0.195420 0.384296 11.00000 -1.50000 H45B 2 -0.062055 -0.138204 0.464089 11.00000 -1.50000 H45C 2 0.027537 -0.139493 0.403566 11.00000 -1.50000 AFIX 6 O12 6 0.678218 -0.064740 0.455372 11.00000 0.03792 0.03859 = 0.02830 0.00760 0.00587 0.01471 H12A 2 0.714011 -0.064025 0.499991 11.00000 -1.50000 H12B 2 0.746295 -0.047763 0.431720 11.00000 -1.50000 AFIX 0 HKLF 4 REM gb_a.res in P-1 REM R1 = 0.0499 for 7374 Fo > 4sig(Fo) and 0.0644 for all 8791 data REM 637 parameters refined using 0 restraints END WGHT 0.0584 1.3113 REM Instructions for potential hydrogen bonds HTAB O2 O5 HTAB O11 O3 HTAB O10 O3 HTAB O9 O6 HTAB C4 O10_$1 HTAB C7 O10_$1 HTAB C1 O6 HTAB C9 O11_$2 HTAB C12 O3_$2 HTAB C20 O10_$1 HTAB C17 O11_$2 HTAB C14 Cl2_$3 HTAB C46 O6 HTAB O12 O6_$4 HTAB O12 O9_$2 REM Highest difference peak 0.595, deepest hole -0.733, 1-sigma level 0.101 Q1 1 0.5752 0.3018 0.3005 11.00000 0.05 0.59 Q2 1 0.5088 0.2779 0.4004 11.00000 0.05 0.57 Q3 1 0.8105 -0.0660 0.4632 11.00000 0.05 0.51 Q4 1 0.0010 0.1258 0.3947 11.00000 0.05 0.48 Q5 1 0.4170 -0.0180 0.4507 11.00000 0.05 0.46 Q6 1 0.3561 0.0868 0.3196 11.00000 0.05 0.44 Q7 1 0.5387 0.0224 0.4492 11.00000 0.05 0.44 Q8 1 0.3773 0.3491 0.2083 11.00000 0.05 0.42 Q9 1 0.5236 -0.0977 0.1081 11.00000 0.05 0.41 Q10 1 0.7787 0.0283 0.2474 11.00000 0.05 0.40 Q11 1 0.9212 0.5657 0.4382 11.00000 0.05 0.39 Q12 1 0.4779 0.0712 0.4970 11.00000 0.05 0.39 Q13 1 0.1105 0.2803 0.3818 11.00000 0.05 0.38 Q14 1 0.7637 0.4076 0.3549 11.00000 0.05 0.38 Q15 1 0.6395 0.2236 0.2704 11.00000 0.05 0.37 Q16 1 0.0929 -0.0310 0.1903 11.00000 0.05 0.37 Q17 1 0.1117 0.5261 0.2118 11.00000 0.05 0.37 Q18 1 0.3406 0.7063 0.0089 11.00000 0.05 0.37 Q19 1 0.7951 0.3762 0.3001 11.00000 0.05 0.37 Q20 1 0.3821 0.0390 0.3806 11.00000 0.05 0.37 ; _shelx_res_checksum 21741 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 Cu1 Cu 0.53833(4) 0.28170(3) 0.35099(2) 0.01403(12) Uani 1 1 d . . . Cu2 Cu 0.5000 0.0000 0.5000 0.01774(15) Uani 1 2 d S . P P2 P 0.32745(8) 0.05482(7) 0.36235(4) 0.01338(19) Uani 1 1 d . . . P1 P 0.30736(9) 0.34076(7) 0.24111(4) 0.0159(2) Uani 1 1 d . . . Cl2 Cl 0.30750(10) -0.04921(9) -0.00126(5) 0.0371(3) Uani 1 1 d . . . Cl1 Cl 0.41747(12) 0.69082(9) -0.00049(6) 0.0471(3) Uani 1 1 d . . . O5 O 0.3790(2) 0.14901(17) 0.32345(11) 0.0169(5) Uani 1 1 d . . . O1 O 0.4322(2) 0.37465(17) 0.30339(11) 0.0174(5) Uani 1 1 d . . . O8 O 0.4544(2) 0.04128(18) 0.40764(11) 0.0181(5) Uani 1 1 d . . . O7 O 0.2543(2) -0.04484(17) 0.29902(11) 0.0157(5) Uani 1 1 d . . . O6 O 0.2133(2) 0.05505(18) 0.40141(12) 0.0204(5) Uani 1 1 d . . . O4 O 0.3667(2) 0.35282(18) 0.16819(11) 0.0192(5) Uani 1 1 d . . . O2 O 0.2279(2) 0.21965(19) 0.22900(12) 0.0240(6) Uani 1 1 d . . . H2 H 0.2699 0.1946 0.2593 0.036 Uiso 1 1 calc R U . O3 O 0.2023(2) 0.39148(19) 0.24289(12) 0.0230(6) Uani 1 1 d . . . N2 N 0.7237(3) 0.3947(2) 0.38184(13) 0.0141(6) Uani 1 1 d . . . N3 N 0.6291(3) 0.2679(2) 0.26517(13) 0.0150(6) Uani 1 1 d . . . N4 N 1.3367(3) 0.8581(2) 0.47331(14) 0.0167(6) Uani 1 1 d . . . O11 O 0.1562(3) 0.5679(2) 0.23940(13) 0.0340(7) Uani 1 1 d . . . H11 H 0.1765 0.5149 0.2361 0.051 Uiso 1 1 calc R U . O10 O 0.0708(3) 0.3195(2) 0.36109(14) 0.0293(6) Uani 1 1 d . . . H10 H 0.1154 0.3445 0.3298 0.044 Uiso 1 1 calc R U . N1 N 0.5261(3) 0.3310(2) 0.45246(13) 0.0162(6) Uani 1 1 d . . . C6 C 0.7486(3) 0.4580(3) 0.44337(16) 0.0151(7) Uani 1 1 d . . . C5 C 0.6368(3) 0.4208(3) 0.48525(16) 0.0158(7) Uani 1 1 d . . . C11 C 0.7644(3) 0.3369(3) 0.27150(16) 0.0146(7) Uani 1 1 d . . . O9 O -0.0728(3) -0.0430(3) 0.39512(18) 0.0478(8) Uani 1 1 d . . . H9A H 0.0094 0.0023 0.3991 0.072 Uiso 1 1 calc R U . C38 C 0.1630(3) -0.0322(3) 0.17839(16) 0.0160(7) Uani 1 1 d . . . C4 C 0.6420(3) 0.4710(3) 0.55128(17) 0.0182(7) Uani 1 1 d . . . H4 H 0.7201 0.5334 0.5728 0.022 Uiso 1 1 calc R U . C35 C 0.3949(3) -0.0665(3) 0.13704(18) 0.0234(8) Uani 1 1 d . . . H35 H 0.4704 -0.0806 0.1217 0.028 Uiso 1 1 calc R U . C33 C 0.2711(3) -0.0448(3) 0.22838(16) 0.0157(7) Uani 1 1 d . . . C22 C 0.5073(3) 0.5208(3) 0.14445(17) 0.0192(7) Uani 1 1 d . . . C16 C 1.0995(3) 0.6692(3) 0.43782(16) 0.0146(7) Uani 1 1 d . . . C39 C 0.0315(3) -0.0248(3) 0.20173(18) 0.0197(8) Uani 1 1 d . . . H39 H 0.0639 0.0219 0.2489 0.024 Uiso 1 1 calc R U . C7 C 0.8701(3) 0.5480(3) 0.46266(16) 0.0145(7) Uani 1 1 d . . . H7 H 0.8859 0.5935 0.5056 0.017 Uiso 1 1 calc R U . C1 C 0.4194(3) 0.2911(3) 0.48662(17) 0.0210(8) Uani 1 1 d . . . H1 H 0.3415 0.2289 0.4644 0.025 Uiso 1 1 calc R U . C9 C 0.9423(3) 0.5031(3) 0.35511(16) 0.0157(7) Uani 1 1 d . . . H9 H 1.0081 0.5167 0.3243 0.019 Uiso 1 1 calc R U . C34 C 0.3863(3) -0.0632(3) 0.20896(17) 0.0175(7) Uani 1 1 d . . . C12 C 0.8418(3) 0.3356(3) 0.21925(17) 0.0197(8) Uani 1 1 d . . . H12 H 0.9378 0.3831 0.2256 0.024 Uiso 1 1 calc R U . C10 C 0.8165(3) 0.4145(3) 0.33804(16) 0.0148(7) Uani 1 1 d . . . C15 C 0.5652(3) 0.1996(3) 0.20452(16) 0.0183(7) Uani 1 1 d . . . H15 H 0.4692 0.1527 0.1993 0.022 Uiso 1 1 calc R U . C8 C 0.9699(3) 0.5718(3) 0.41851(16) 0.0151(7) Uani 1 1 d . . . C19 C 1.2555(3) 0.8219(3) 0.52083(17) 0.0210(8) Uani 1 1 d . . . H19 H 1.2801 0.8617 0.5671 0.025 Uiso 1 1 calc R U . C20 C 1.1388(3) 0.7302(3) 0.50559(17) 0.0179(7) Uani 1 1 d . . . H20 H 1.0846 0.7081 0.5409 0.021 Uiso 1 1 calc R U . C37 C 0.1784(3) -0.0327(3) 0.10815(17) 0.0207(8) Uani 1 1 d . . . H37 H 0.1098 -0.0215 0.0733 0.025 Uiso 1 1 calc R U . C42 C 0.4996(4) -0.0803(3) 0.26313(18) 0.0213(8) Uani 1 1 d . . . H42 H 0.4750 -0.0723 0.3110 0.026 Uiso 1 1 calc R U . C13 C 0.7763(4) 0.2633(3) 0.15713(18) 0.0215(8) Uani 1 1 d . . . H13 H 0.8272 0.2603 0.1205 0.026 Uiso 1 1 calc R U . C18 C 1.3021(4) 0.7987(3) 0.40937(17) 0.0208(8) Uani 1 1 d . . . H18 H 1.3601 0.8221 0.3758 0.025 Uiso 1 1 calc R U . C17 C 1.1867(3) 0.7053(3) 0.38942(17) 0.0208(8) Uani 1 1 d . . . H17 H 1.1668 0.6662 0.3433 0.025 Uiso 1 1 calc R U . C21 C 0.3786(3) 0.4338(3) 0.12964(17) 0.0190(7) Uani 1 1 d . . . C30 C 0.6336(3) 0.5302(3) 0.20219(17) 0.0208(8) Uani 1 1 d . . . H30 H 0.6091 0.4636 0.2220 0.025 Uiso 1 1 calc R U . C14 C 0.6357(4) 0.1958(3) 0.14925(17) 0.0219(8) Uani 1 1 d . . . H14 H 0.5881 0.1475 0.1065 0.026 Uiso 1 1 calc R U . C3 C 0.5310(4) 0.4284(3) 0.58562(17) 0.0242(8) Uani 1 1 d . . . H3 H 0.5319 0.4616 0.6311 0.029 Uiso 1 1 calc R U . C36 C 0.2934(4) -0.0493(3) 0.08827(17) 0.0214(8) Uani 1 1 d . . . C23 C 0.5170(4) 0.5996(3) 0.10319(18) 0.0238(8) Uani 1 1 d . . . H23 H 0.6018 0.6603 0.1124 0.029 Uiso 1 1 calc R U . C2 C 0.4197(4) 0.3380(3) 0.55355(19) 0.0277(9) Uani 1 1 d . . . H2A H 0.3435 0.3077 0.5768 0.033 Uiso 1 1 calc R U . C26 C 0.2645(4) 0.4222(3) 0.07289(17) 0.0226(8) Uani 1 1 d . . . C31 C 0.7679(4) 0.5469(3) 0.17171(19) 0.0279(9) Uani 1 1 d . . . H31A H 0.7496 0.4879 0.1351 0.042 Uiso 1 1 calc R U . H31B H 0.8477 0.5531 0.2104 0.042 Uiso 1 1 calc R U . H31C H 0.7920 0.6105 0.1503 0.042 Uiso 1 1 calc R U . C40 C -0.0658(4) -0.1330(3) 0.2123(2) 0.0309(9) Uani 1 1 d . . . H40A H -0.0974 -0.1803 0.1667 0.046 Uiso 1 1 calc R U . H40B H -0.1492 -0.1286 0.2286 0.046 Uiso 1 1 calc R U . H40C H -0.0126 -0.1590 0.2481 0.046 Uiso 1 1 calc R U . C27 C 0.1326(4) 0.3213(3) 0.05565(18) 0.0274(9) Uani 1 1 d . . . H27 H 0.1056 0.3032 0.1020 0.033 Uiso 1 1 calc R U . C32 C 0.6638(4) 0.6172(3) 0.26362(19) 0.0290(9) Uani 1 1 d . . . H32A H 0.6981 0.6841 0.2467 0.044 Uiso 1 1 calc R U . H32B H 0.7369 0.6151 0.3030 0.044 Uiso 1 1 calc R U . H32C H 0.5759 0.6081 0.2806 0.044 Uiso 1 1 calc R U . C25 C 0.2791(4) 0.5017(3) 0.03282(18) 0.0269(9) Uani 1 1 d . . . H25 H 0.2039 0.4959 -0.0058 0.032 Uiso 1 1 calc R U . C24 C 0.4037(4) 0.5896(3) 0.04902(19) 0.0271(9) Uani 1 1 d . . . C41 C -0.0521(4) 0.0190(3) 0.14853(19) 0.0267(9) Uani 1 1 d . . . H41A H 0.0127 0.0850 0.1389 0.040 Uiso 1 1 calc R U . H41B H -0.1279 0.0302 0.1689 0.040 Uiso 1 1 calc R U . H41C H -0.0948 -0.0301 0.1037 0.040 Uiso 1 1 calc R U . C29 C 0.0022(4) 0.3297(4) 0.0071(2) 0.0420(11) Uani 1 1 d . . . H29A H -0.0189 0.3868 0.0290 0.063 Uiso 1 1 calc R U . H29B H -0.0807 0.2647 0.0013 0.063 Uiso 1 1 calc R U . H29C H 0.0235 0.3431 -0.0399 0.063 Uiso 1 1 calc R U . C47 C 0.1392(5) 0.5994(4) 0.1714(2) 0.0402(11) Uani 1 1 d . . . H47A H 0.0631 0.5430 0.1373 0.060 Uiso 1 1 calc R U . H47B H 0.2289 0.6166 0.1548 0.060 Uiso 1 1 calc R U . H47C H 0.1137 0.6604 0.1750 0.060 Uiso 1 1 calc R U . C43 C 0.6486(4) 0.0021(4) 0.2687(2) 0.0438(12) Uani 1 1 d . . . H43A H 0.6735 0.0015 0.2215 0.066 Uiso 1 1 calc R U . H43B H 0.7186 -0.0130 0.3028 0.066 Uiso 1 1 calc R U . H43C H 0.6494 0.0704 0.2852 0.066 Uiso 1 1 calc R U . C28 C 0.1685(5) 0.2332(3) 0.0218(2) 0.0435(11) Uani 1 1 d . . . H28A H 0.1953 0.2487 -0.0239 0.065 Uiso 1 1 calc R U . H28B H 0.0848 0.1682 0.0134 0.065 Uiso 1 1 calc R U . H28C H 0.2484 0.2264 0.0542 0.065 Uiso 1 1 calc R U . C46 C 0.0186(5) 0.2099(3) 0.3464(3) 0.0496(12) Uani 1 1 d . . . H46A H -0.0198 0.1869 0.2948 0.074 Uiso 1 1 calc R U . H46B H -0.0573 0.1805 0.3724 0.074 Uiso 1 1 calc R U . H46C H 0.0966 0.1865 0.3618 0.074 Uiso 1 1 calc R U . C44 C 0.4986(6) -0.1893(4) 0.2494(3) 0.0520(13) Uani 1 1 d . . . H44A H 0.4033 -0.2400 0.2492 0.078 Uiso 1 1 calc R U . H44B H 0.5690 -0.1976 0.2873 0.078 Uiso 1 1 calc R U . H44C H 0.5227 -0.2005 0.2029 0.078 Uiso 1 1 calc R U . C45 C -0.0617(5) -0.1362(4) 0.4132(3) 0.0564(14) Uani 1 1 d . . . H45A H -0.1430 -0.1954 0.3843 0.085 Uiso 1 1 calc R U . H45B H -0.0621 -0.1382 0.4641 0.085 Uiso 1 1 calc R U . H45C H 0.0275 -0.1395 0.4036 0.085 Uiso 1 1 calc R U . O12 O 0.6782(3) -0.0647(2) 0.45537(14) 0.0349(7) Uani 1 1 d G . . H12A H 0.7140 -0.0640 0.5000 0.052 Uiso 1 1 d G U . H12B H 0.7463 -0.0478 0.4317 0.052 Uiso 1 1 d G U . 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 0.0140(2) 0.0120(2) 0.0120(2) -0.00160(16) 0.00319(15) 0.00080(17) Cu2 0.0161(3) 0.0119(3) 0.0160(3) 0.0015(2) -0.0032(2) -0.0023(2) P2 0.0120(4) 0.0100(4) 0.0130(4) -0.0009(3) 0.0004(3) -0.0003(3) P1 0.0160(4) 0.0132(5) 0.0155(4) 0.0024(4) 0.0023(3) 0.0026(4) Cl2 0.0359(5) 0.0568(7) 0.0165(4) -0.0012(4) 0.0096(4) 0.0148(5) Cl1 0.0457(6) 0.0465(7) 0.0509(7) 0.0347(6) 0.0070(5) 0.0151(6) O5 0.0182(11) 0.0119(13) 0.0147(11) -0.0002(9) 0.0010(9) 0.0005(10) O1 0.0205(12) 0.0116(12) 0.0171(11) 0.0014(10) 0.0019(9) 0.0038(10) O8 0.0146(11) 0.0186(13) 0.0153(11) 0.0010(10) -0.0007(9) 0.0018(10) O7 0.0158(11) 0.0104(12) 0.0155(11) -0.0007(9) 0.0030(9) -0.0007(9) O6 0.0176(12) 0.0197(14) 0.0199(12) -0.0005(10) 0.0049(9) 0.0028(10) O4 0.0238(12) 0.0144(13) 0.0191(12) 0.0038(10) 0.0052(10) 0.0064(11) O2 0.0222(12) 0.0156(14) 0.0235(13) 0.0053(11) -0.0028(10) -0.0023(11) O3 0.0215(12) 0.0269(15) 0.0245(13) 0.0086(11) 0.0083(10) 0.0112(11) N2 0.0174(13) 0.0115(15) 0.0101(13) -0.0004(11) 0.0029(10) 0.0021(12) N3 0.0176(14) 0.0103(15) 0.0147(13) 0.0007(11) 0.0021(11) 0.0034(12) N4 0.0144(13) 0.0164(16) 0.0161(14) 0.0029(12) 0.0022(11) 0.0025(12) O11 0.0501(17) 0.0327(18) 0.0277(14) 0.0025(13) 0.0174(12) 0.0220(15) O10 0.0296(14) 0.0231(15) 0.0319(15) -0.0009(12) 0.0094(11) 0.0060(12) N1 0.0161(13) 0.0139(15) 0.0147(13) -0.0016(12) 0.0038(11) 0.0016(12) C6 0.0164(16) 0.0158(18) 0.0120(15) 0.0016(14) 0.0014(12) 0.0058(14) C5 0.0175(16) 0.0140(18) 0.0155(16) 0.0029(14) 0.0037(13) 0.0054(14) C11 0.0168(16) 0.0111(17) 0.0155(16) 0.0018(13) 0.0018(12) 0.0055(14) O9 0.0281(15) 0.047(2) 0.068(2) 0.0170(18) 0.0138(15) 0.0113(15) C38 0.0157(16) 0.0096(17) 0.0149(16) -0.0046(13) 0.0015(13) -0.0021(13) C4 0.0198(17) 0.0111(18) 0.0188(17) -0.0013(14) 0.0047(13) 0.0007(14) C35 0.0181(17) 0.023(2) 0.0264(19) -0.0047(16) 0.0074(14) 0.0045(15) C33 0.0169(16) 0.0107(17) 0.0140(16) -0.0015(13) 0.0022(13) 0.0000(14) C22 0.0219(17) 0.0168(19) 0.0213(17) 0.0025(15) 0.0108(14) 0.0075(15) C16 0.0130(15) 0.0129(18) 0.0167(16) 0.0038(14) 0.0013(12) 0.0041(14) C39 0.0144(16) 0.019(2) 0.0209(17) -0.0020(15) 0.0017(13) 0.0022(14) C7 0.0147(15) 0.0146(18) 0.0117(15) 0.0006(13) 0.0033(12) 0.0026(14) C1 0.0200(17) 0.0145(19) 0.0213(18) -0.0039(15) 0.0069(14) -0.0015(15) C9 0.0138(15) 0.0175(19) 0.0145(16) 0.0038(14) 0.0029(12) 0.0040(14) C34 0.0162(16) 0.0116(18) 0.0206(17) -0.0004(14) 0.0029(13) 0.0013(14) C12 0.0176(16) 0.020(2) 0.0182(17) -0.0001(15) 0.0039(13) 0.0038(15) C10 0.0160(16) 0.0120(18) 0.0154(16) -0.0007(14) 0.0032(12) 0.0049(14) C15 0.0187(16) 0.0132(18) 0.0182(17) 0.0002(14) 0.0033(13) 0.0013(14) C8 0.0130(15) 0.0150(18) 0.0145(16) 0.0032(14) -0.0003(12) 0.0033(14) C19 0.0144(16) 0.024(2) 0.0164(17) -0.0041(15) -0.0018(13) 0.0020(15) C20 0.0177(16) 0.0180(19) 0.0161(17) 0.0043(14) 0.0053(13) 0.0036(15) C37 0.0138(16) 0.022(2) 0.0184(17) -0.0016(15) -0.0019(13) 0.0009(15) C42 0.0215(17) 0.021(2) 0.0225(18) 0.0019(15) 0.0060(14) 0.0098(16) C13 0.0262(18) 0.021(2) 0.0194(17) 0.0033(15) 0.0095(14) 0.0094(16) C18 0.0233(18) 0.019(2) 0.0184(17) 0.0040(15) 0.0081(14) 0.0037(15) C17 0.0234(17) 0.021(2) 0.0122(16) -0.0005(14) 0.0053(13) 0.0023(15) C21 0.0215(17) 0.019(2) 0.0152(16) 0.0007(14) 0.0089(13) 0.0048(15) C30 0.0188(17) 0.021(2) 0.0181(17) 0.0047(15) 0.0040(13) 0.0022(15) C14 0.0325(19) 0.019(2) 0.0140(17) -0.0019(15) 0.0068(14) 0.0091(16) C3 0.032(2) 0.022(2) 0.0153(17) -0.0039(15) 0.0091(15) 0.0049(17) C36 0.0232(17) 0.024(2) 0.0112(16) -0.0020(15) 0.0058(13) 0.0020(16) C23 0.0260(18) 0.022(2) 0.0214(18) 0.0074(16) 0.0083(14) 0.0048(16) C2 0.0266(19) 0.023(2) 0.0279(19) -0.0009(17) 0.0179(16) -0.0015(17) C26 0.0228(18) 0.029(2) 0.0166(17) 0.0039(16) 0.0058(14) 0.0097(16) C31 0.0257(19) 0.032(2) 0.028(2) 0.0061(17) 0.0099(16) 0.0114(18) C40 0.0195(18) 0.027(2) 0.041(2) 0.0034(18) 0.0074(16) 0.0022(17) C27 0.0241(18) 0.032(2) 0.0184(18) 0.0047(16) 0.0019(14) 0.0022(17) C32 0.033(2) 0.032(2) 0.0220(19) 0.0015(17) 0.0027(15) 0.0137(18) C25 0.0262(19) 0.037(2) 0.0188(18) 0.0097(17) 0.0025(14) 0.0137(18) C24 0.032(2) 0.028(2) 0.0260(19) 0.0151(17) 0.0095(16) 0.0134(18) C41 0.0182(17) 0.033(2) 0.0265(19) -0.0006(17) 0.0019(14) 0.0097(17) C29 0.027(2) 0.053(3) 0.032(2) 0.012(2) -0.0036(17) 0.002(2) C47 0.047(3) 0.046(3) 0.032(2) 0.012(2) 0.0156(19) 0.018(2) C43 0.021(2) 0.055(3) 0.050(3) 0.025(2) 0.0008(18) 0.008(2) C28 0.043(2) 0.033(3) 0.038(2) -0.009(2) 0.0031(19) 0.000(2) C46 0.061(3) 0.035(3) 0.060(3) 0.006(2) 0.035(2) 0.016(2) C44 0.072(3) 0.032(3) 0.055(3) 0.000(2) -0.004(2) 0.033(3) C45 0.040(3) 0.034(3) 0.096(4) 0.021(3) 0.022(3) 0.008(2) O12 0.0379(15) 0.0386(18) 0.0283(14) 0.0076(14) 0.0059(12) 0.0147(14) 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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' P P 0.1023 0.0942 '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 O5 Cu1 N2 166.76(10) . . O5 Cu1 N1 103.45(11) . . N2 Cu1 N1 79.86(11) . . O5 Cu1 N3 96.10(10) . . N2 Cu1 N3 79.04(11) . . N1 Cu1 N3 158.36(10) . . O5 Cu1 O1 97.63(9) . . N2 Cu1 O1 94.98(10) . . N1 Cu1 O1 93.04(10) . . N3 Cu1 O1 93.49(10) . . O8 Cu2 O8 180.00(13) . 2_656 O8 Cu2 N4 86.30(11) . 2_766 O8 Cu2 N4 93.70(11) 2_656 2_766 O8 Cu2 N4 93.70(11) . 1_445 O8 Cu2 N4 86.30(11) 2_656 1_445 N4 Cu2 N4 180.00(13) 2_766 1_445 O6 P2 O8 114.42(13) . . O6 P2 O5 113.50(14) . . O8 P2 O5 110.24(13) . . O6 P2 O7 106.20(12) . . O8 P2 O7 106.64(13) . . O5 P2 O7 105.07(12) . . O3 P1 O1 116.81(13) . . O3 P1 O2 109.93(14) . . O1 P1 O2 110.26(14) . . O3 P1 O4 110.65(13) . . O1 P1 O4 108.63(13) . . O2 P1 O4 99.12(13) . . P2 O5 Cu1 132.28(13) . . P1 O1 Cu1 127.54(14) . . P2 O8 Cu2 137.30(14) . . C33 O7 P2 125.2(2) . . C21 O4 P1 125.3(2) . . P1 O2 H2 109.5 . . C6 N2 C10 121.7(3) . . C6 N2 Cu1 118.2(2) . . C10 N2 Cu1 119.7(2) . . C15 N3 C11 119.0(3) . . C15 N3 Cu1 125.8(2) . . C11 N3 Cu1 115.2(2) . . C18 N4 C19 117.0(3) . . C18 N4 Cu2 123.4(2) . 1_665 C19 N4 Cu2 119.5(2) . 1_665 C47 O11 H11 109.5 . . C46 O10 H10 109.5 . . C1 N1 C5 118.0(3) . . C1 N1 Cu1 128.1(2) . . C5 N1 Cu1 113.6(2) . . N2 C6 C7 120.5(3) . . N2 C6 C5 113.5(3) . . C7 C6 C5 126.1(3) . . N1 C5 C4 122.4(3) . . N1 C5 C6 113.7(3) . . C4 C5 C6 123.8(3) . . N3 C11 C12 122.2(3) . . N3 C11 C10 113.3(3) . . C12 C11 C10 124.5(3) . . C45 O9 H9A 109.5 . . C37 C38 C33 117.4(3) . . C37 C38 C39 122.5(3) . . C33 C38 C39 120.1(3) . . C5 C4 C3 118.6(3) . . C5 C4 H4 120.7 . . C3 C4 H4 120.7 . . C36 C35 C34 119.8(3) . . C36 C35 H35 120.1 . . C34 C35 H35 120.1 . . O7 C33 C34 120.1(3) . . O7 C33 C38 116.9(3) . . C34 C33 C38 122.9(3) . . C23 C22 C21 117.7(3) . . C23 C22 C30 120.1(3) . . C21 C22 C30 122.2(3) . . C17 C16 C20 116.7(3) . . C17 C16 C8 122.0(3) . . C20 C16 C8 121.3(3) . . C38 C39 C41 113.0(3) . . C38 C39 C40 108.9(3) . . C41 C39 C40 110.1(3) . . C38 C39 H39 108.2 . . C41 C39 H39 108.2 . . C40 C39 H39 108.2 . . C6 C7 C8 119.7(3) . . C6 C7 H7 120.1 . . C8 C7 H7 120.1 . . N1 C1 C2 122.0(3) . . N1 C1 H1 119.0 . . C2 C1 H1 119.0 . . C10 C9 C8 119.0(3) . . C10 C9 H9 120.5 . . C8 C9 H9 120.5 . . C35 C34 C33 117.8(3) . . C35 C34 C42 119.9(3) . . C33 C34 C42 122.3(3) . . C11 C12 C13 118.6(3) . . C11 C12 H12 120.7 . . C13 C12 H12 120.7 . . N2 C10 C9 120.6(3) . . N2 C10 C11 112.5(3) . . C9 C10 C11 126.8(3) . . N3 C15 C14 121.7(3) . . N3 C15 H15 119.2 . . C14 C15 H15 119.2 . . C7 C8 C9 118.5(3) . . C7 C8 C16 120.3(3) . . C9 C8 C16 121.1(3) . . N4 C19 C20 123.1(3) . . N4 C19 H19 118.4 . . C20 C19 H19 118.4 . . C19 C20 C16 120.0(3) . . C19 C20 H20 120.0 . . C16 C20 H20 120.0 . . C38 C37 C36 120.3(3) . . C38 C37 H37 119.8 . . C36 C37 H37 119.8 . . C34 C42 C44 112.7(3) . . C34 C42 C43 112.1(3) . . C44 C42 C43 111.6(3) . . C34 C42 H42 106.7 . . C44 C42 H42 106.7 . . C43 C42 H42 106.7 . . C14 C13 C12 119.2(3) . . C14 C13 H13 120.4 . . C12 C13 H13 120.4 . . N4 C18 C17 123.8(3) . . N4 C18 H18 118.1 . . C17 C18 H18 118.1 . . C18 C17 C16 119.3(3) . . C18 C17 H17 120.4 . . C16 C17 H17 120.4 . . O4 C21 C22 119.3(3) . . O4 C21 C26 118.4(3) . . C22 C21 C26 122.1(3) . . C22 C30 C32 111.4(3) . . C22 C30 C31 111.4(3) . . C32 C30 C31 110.2(3) . . C22 C30 H30 107.9 . . C32 C30 H30 107.9 . . C31 C30 H30 107.9 . . C13 C14 C15 119.2(3) . . C13 C14 H14 120.4 . . C15 C14 H14 120.4 . . C2 C3 C4 119.6(3) . . C2 C3 H3 120.2 . . C4 C3 H3 120.2 . . C35 C36 C37 121.8(3) . . C35 C36 Cl2 119.8(3) . . C37 C36 Cl2 118.4(3) . . C24 C23 C22 120.1(3) . . C24 C23 H23 119.9 . . C22 C23 H23 119.9 . . C3 C2 C1 119.4(3) . . C3 C2 H2A 120.3 . . C1 C2 H2A 120.3 . . C25 C26 C21 118.2(3) . . C25 C26 C27 122.4(3) . . C21 C26 C27 119.3(3) . . C30 C31 H31A 109.5 . . C30 C31 H31B 109.5 . . H31A C31 H31B 109.5 . . C30 C31 H31C 109.5 . . H31A C31 H31C 109.5 . . H31B C31 H31C 109.5 . . C39 C40 H40A 109.5 . . C39 C40 H40B 109.5 . . H40A C40 H40B 109.5 . . C39 C40 H40C 109.5 . . H40A C40 H40C 109.5 . . H40B C40 H40C 109.5 . . C26 C27 C28 110.2(3) . . C26 C27 C29 113.4(3) . . C28 C27 C29 110.3(3) . . C26 C27 H27 107.6 . . C28 C27 H27 107.6 . . C29 C27 H27 107.6 . . C30 C32 H32A 109.5 . . C30 C32 H32B 109.5 . . H32A C32 H32B 109.5 . . C30 C32 H32C 109.5 . . H32A C32 H32C 109.5 . . H32B C32 H32C 109.5 . . C26 C25 C24 119.9(3) . . C26 C25 H25 120.0 . . C24 C25 H25 120.0 . . C23 C24 C25 121.8(4) . . C23 C24 Cl1 119.1(3) . . C25 C24 Cl1 119.1(3) . . C39 C41 H41A 109.5 . . C39 C41 H41B 109.5 . . H41A C41 H41B 109.5 . . C39 C41 H41C 109.5 . . H41A C41 H41C 109.5 . . H41B C41 H41C 109.5 . . C27 C29 H29A 109.5 . . C27 C29 H29B 109.5 . . H29A C29 H29B 109.5 . . C27 C29 H29C 109.5 . . H29A C29 H29C 109.5 . . H29B C29 H29C 109.5 . . O11 C47 H47A 109.5 . . O11 C47 H47B 109.5 . . H47A C47 H47B 109.5 . . O11 C47 H47C 109.5 . . H47A C47 H47C 109.5 . . H47B C47 H47C 109.5 . . C42 C43 H43A 109.5 . . C42 C43 H43B 109.5 . . H43A C43 H43B 109.5 . . C42 C43 H43C 109.5 . . H43A C43 H43C 109.5 . . H43B C43 H43C 109.5 . . C27 C28 H28A 109.5 . . C27 C28 H28B 109.5 . . H28A C28 H28B 109.5 . . C27 C28 H28C 109.5 . . H28A C28 H28C 109.5 . . H28B C28 H28C 109.5 . . O10 C46 H46A 109.5 . . O10 C46 H46B 109.5 . . H46A C46 H46B 109.5 . . O10 C46 H46C 109.5 . . H46A C46 H46C 109.5 . . H46B C46 H46C 109.5 . . C42 C44 H44A 109.5 . . C42 C44 H44B 109.5 . . H44A C44 H44B 109.5 . . C42 C44 H44C 109.5 . . H44A C44 H44C 109.5 . . H44B C44 H44C 109.5 . . O9 C45 H45A 109.5 . . O9 C45 H45B 109.5 . . H45A C45 H45B 109.5 . . O9 C45 H45C 109.5 . . H45A C45 H45C 109.5 . . H45B C45 H45C 109.5 . . H12A O12 H12B 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Cu1 O5 1.941(2) . Cu1 N2 1.943(3) . Cu1 N1 2.049(3) . Cu1 N3 2.051(3) . Cu1 O1 2.143(2) . Cu2 O8 1.943(2) . Cu2 O8 1.943(2) 2_656 Cu2 N4 2.042(3) 2_766 Cu2 N4 2.042(3) 1_445 P2 O6 1.494(2) . P2 O8 1.520(2) . P2 O5 1.541(2) . P2 O7 1.626(2) . P1 O3 1.492(2) . P1 O1 1.498(2) . P1 O2 1.573(3) . P1 O4 1.615(2) . Cl2 C36 1.747(3) . Cl1 C24 1.748(4) . O7 C33 1.394(4) . O4 C21 1.385(4) . O2 H2 0.8400 . N2 C6 1.343(4) . N2 C10 1.345(4) . N3 C15 1.343(4) . N3 C11 1.355(4) . N4 C18 1.339(4) . N4 C19 1.346(4) . N4 Cu2 2.042(3) 1_665 O11 C47 1.414(5) . O11 H11 0.8400 . O10 C46 1.417(5) . O10 H10 0.8400 . N1 C1 1.343(4) . N1 C5 1.367(4) . C6 C7 1.385(4) . C6 C5 1.478(4) . C5 C4 1.379(4) . C11 C12 1.383(4) . C11 C10 1.489(4) . O9 C45 1.416(5) . O9 H9A 0.8400 . C38 C37 1.382(5) . C38 C33 1.411(4) . C38 C39 1.526(4) . C4 C3 1.385(5) . C4 H4 0.9500 . C35 C36 1.381(5) . C35 C34 1.395(5) . C35 H35 0.9500 . C33 C34 1.397(4) . C22 C23 1.396(5) . C22 C21 1.404(5) . C22 C30 1.513(5) . C16 C17 1.397(5) . C16 C20 1.404(4) . C16 C8 1.488(4) . C39 C41 1.530(5) . C39 C40 1.538(5) . C39 H39 1.0000 . C7 C8 1.404(4) . C7 H7 0.9500 . C1 C2 1.391(5) . C1 H1 0.9500 . C9 C10 1.397(4) . C9 C8 1.406(4) . C9 H9 0.9500 . C34 C42 1.523(5) . C12 C13 1.391(5) . C12 H12 0.9500 . C15 C14 1.388(5) . C15 H15 0.9500 . C19 C20 1.372(5) . C19 H19 0.9500 . C20 H20 0.9500 . C37 C36 1.388(5) . C37 H37 0.9500 . C42 C44 1.524(5) . C42 C43 1.529(5) . C42 H42 1.0000 . C13 C14 1.386(5) . C13 H13 0.9500 . C18 C17 1.382(5) . C18 H18 0.9500 . C17 H17 0.9500 . C21 C26 1.409(5) . C30 C32 1.528(5) . C30 C31 1.536(5) . C30 H30 1.0000 . C14 H14 0.9500 . C3 C2 1.371(5) . C3 H3 0.9500 . C23 C24 1.379(5) . C23 H23 0.9500 . C2 H2A 0.9500 . C26 C25 1.383(5) . C26 C27 1.528(5) . C31 H31A 0.9800 . C31 H31B 0.9800 . C31 H31C 0.9800 . C40 H40A 0.9800 . C40 H40B 0.9800 . C40 H40C 0.9800 . C27 C28 1.534(6) . C27 C29 1.543(5) . C27 H27 1.0000 . C32 H32A 0.9800 . C32 H32B 0.9800 . C32 H32C 0.9800 . C25 C24 1.385(5) . C25 H25 0.9500 . C41 H41A 0.9800 . C41 H41B 0.9800 . C41 H41C 0.9800 . C29 H29A 0.9800 . C29 H29B 0.9800 . C29 H29C 0.9800 . C47 H47A 0.9800 . C47 H47B 0.9800 . C47 H47C 0.9800 . C43 H43A 0.9800 . C43 H43B 0.9800 . C43 H43C 0.9800 . C28 H28A 0.9800 . C28 H28B 0.9800 . C28 H28C 0.9800 . C46 H46A 0.9800 . C46 H46B 0.9800 . C46 H46C 0.9800 . C44 H44A 0.9800 . C44 H44B 0.9800 . C44 H44C 0.9800 . C45 H45A 0.9800 . C45 H45B 0.9800 . C45 H45C 0.9800 . O12 H12A 0.8699 . O12 H12B 0.8695 . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O5 0.84 1.83 2.667(3) 174.0 . O11 H11 O3 0.84 1.85 2.680(4) 168.9 . O10 H10 O3 0.84 2.07 2.900(4) 172.3 . O9 H9A O6 0.84 1.94 2.735(4) 156.4 . C4 H4 O10 0.95 2.43 3.379(4) 172.6 2_666 C7 H7 O10 0.95 2.63 3.562(4) 166.2 2_666 C1 H1 O6 0.95 2.41 3.314(4) 159.7 . C9 H9 O11 0.95 2.39 3.335(4) 171.1 1_655 C12 H12 O3 0.95 2.64 3.434(4) 141.9 1_655 C20 H20 O10 0.95 2.63 3.568(4) 169.2 2_666 C17 H17 O11 0.95 2.29 3.228(4) 169.8 1_655 C14 H14 Cl2 0.95 2.90 3.613(3) 132.2 2_655 C46 H46C O6 0.98 2.63 3.547(6) 156.3 . O12 H12A O6 0.87 1.89 2.756(3) 175.9 2_656 O12 H12B O9 0.87 2.07 2.907(4) 160.2 1_655 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 O6 P2 O5 Cu1 95.13(19) . O8 P2 O5 Cu1 -34.7(2) . O7 P2 O5 Cu1 -149.27(16) . O3 P1 O1 Cu1 145.28(15) . O2 P1 O1 Cu1 18.9(2) . O4 P1 O1 Cu1 -88.76(18) . O6 P2 O8 Cu2 13.5(3) . O5 P2 O8 Cu2 142.83(19) . O7 P2 O8 Cu2 -103.6(2) . O6 P2 O7 C33 135.8(2) . O8 P2 O7 C33 -101.8(2) . O5 P2 O7 C33 15.3(3) . O3 P1 O4 C21 28.9(3) . O1 P1 O4 C21 -100.6(3) . O2 P1 O4 C21 144.3(3) . C10 N2 C6 C7 1.8(5) . Cu1 N2 C6 C7 -170.7(2) . C10 N2 C6 C5 -177.8(3) . Cu1 N2 C6 C5 9.7(4) . C1 N1 C5 C4 -0.2(5) . Cu1 N1 C5 C4 174.6(3) . C1 N1 C5 C6 179.8(3) . Cu1 N1 C5 C6 -5.4(3) . N2 C6 C5 N1 -2.3(4) . C7 C6 C5 N1 178.1(3) . N2 C6 C5 C4 177.6(3) . C7 C6 C5 C4 -1.9(5) . C15 N3 C11 C12 -3.7(5) . Cu1 N3 C11 C12 177.9(3) . C15 N3 C11 C10 174.2(3) . Cu1 N3 C11 C10 -4.2(3) . N1 C5 C4 C3 0.2(5) . C6 C5 C4 C3 -179.8(3) . P2 O7 C33 C34 87.0(4) . P2 O7 C33 C38 -96.9(3) . C37 C38 C33 O7 -179.7(3) . C39 C38 C33 O7 -3.1(4) . C37 C38 C33 C34 -3.7(5) . C39 C38 C33 C34 172.9(3) . C37 C38 C39 C41 -20.1(5) . C33 C38 C39 C41 163.5(3) . C37 C38 C39 C40 102.6(4) . C33 C38 C39 C40 -73.8(4) . N2 C6 C7 C8 -1.7(5) . C5 C6 C7 C8 177.8(3) . C5 N1 C1 C2 -0.3(5) . Cu1 N1 C1 C2 -174.3(3) . C36 C35 C34 C33 1.6(5) . C36 C35 C34 C42 -178.9(3) . O7 C33 C34 C35 177.5(3) . C38 C33 C34 C35 1.6(5) . O7 C33 C34 C42 -2.1(5) . C38 C33 C34 C42 -177.9(3) . N3 C11 C12 C13 2.4(5) . C10 C11 C12 C13 -175.3(3) . C6 N2 C10 C9 -0.7(5) . Cu1 N2 C10 C9 171.7(2) . C6 N2 C10 C11 -177.4(3) . Cu1 N2 C10 C11 -5.0(4) . C8 C9 C10 N2 -0.5(5) . C8 C9 C10 C11 175.7(3) . N3 C11 C10 N2 5.8(4) . C12 C11 C10 N2 -176.3(3) . N3 C11 C10 C9 -170.6(3) . C12 C11 C10 C9 7.2(5) . C11 N3 C15 C14 2.0(5) . Cu1 N3 C15 C14 -179.7(3) . C6 C7 C8 C9 0.5(5) . C6 C7 C8 C16 178.8(3) . C10 C9 C8 C7 0.6(5) . C10 C9 C8 C16 -177.7(3) . C17 C16 C8 C7 -167.6(3) . C20 C16 C8 C7 11.3(5) . C17 C16 C8 C9 10.6(5) . C20 C16 C8 C9 -170.4(3) . C18 N4 C19 C20 -2.1(5) . Cu2 N4 C19 C20 176.1(3) 1_665 N4 C19 C20 C16 0.2(5) . C17 C16 C20 C19 1.8(5) . C8 C16 C20 C19 -177.3(3) . C33 C38 C37 C36 2.6(5) . C39 C38 C37 C36 -173.9(3) . C35 C34 C42 C44 -65.2(5) . C33 C34 C42 C44 114.4(4) . C35 C34 C42 C43 61.7(4) . C33 C34 C42 C43 -118.8(4) . C11 C12 C13 C14 0.6(5) . C19 N4 C18 C17 2.0(5) . Cu2 N4 C18 C17 -176.1(3) 1_665 N4 C18 C17 C16 0.0(5) . C20 C16 C17 C18 -1.9(5) . C8 C16 C17 C18 177.1(3) . P1 O4 C21 C22 91.7(3) . P1 O4 C21 C26 -93.3(3) . C23 C22 C21 O4 178.2(3) . C30 C22 C21 O4 -1.0(5) . C23 C22 C21 C26 3.4(5) . C30 C22 C21 C26 -175.8(3) . C23 C22 C30 C32 67.4(4) . C21 C22 C30 C32 -113.5(4) . C23 C22 C30 C31 -56.2(4) . C21 C22 C30 C31 123.0(3) . C12 C13 C14 C15 -2.1(5) . N3 C15 C14 C13 0.8(5) . C5 C4 C3 C2 0.2(5) . C34 C35 C36 C37 -2.6(6) . C34 C35 C36 Cl2 177.9(3) . C38 C37 C36 C35 0.5(6) . C38 C37 C36 Cl2 179.9(3) . C21 C22 C23 C24 -1.3(5) . C30 C22 C23 C24 177.9(3) . C4 C3 C2 C1 -0.6(6) . N1 C1 C2 C3 0.7(6) . O4 C21 C26 C25 -177.6(3) . C22 C21 C26 C25 -2.7(5) . O4 C21 C26 C27 -0.2(5) . C22 C21 C26 C27 174.7(3) . C25 C26 C27 C28 106.0(4) . C21 C26 C27 C28 -71.3(4) . C25 C26 C27 C29 -18.2(5) . C21 C26 C27 C29 164.6(3) . C21 C26 C25 C24 0.0(5) . C27 C26 C25 C24 -177.3(3) . C22 C23 C24 C25 -1.3(5) . C22 C23 C24 Cl1 178.6(3) . C26 C25 C24 C23 2.0(6) . C26 C25 C24 Cl1 -178.0(3) .