#------------------------------------------------------------------------------ #$Date: 2017-09-15 05:38:12 +0300 (Fri, 15 Sep 2017) $ #$Revision: 200914 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/42/7044230.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_7044230 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 H120 Cu3 I4 N8 O24 P4' _chemical_formula_weight 2568.07 _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 95.549(3) _cell_angle_beta 99.530(6) _cell_angle_gamma 111.171(8) _cell_formula_units_Z 1 _cell_length_a 10.331(4) _cell_length_b 13.970(6) _cell_length_c 19.644(8) _cell_measurement_reflns_used 5650 _cell_measurement_temperature 130(2) _cell_measurement_theta_max 31.40 _cell_measurement_theta_min 2.90 _cell_volume 2569.2(18) _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 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 130(2) _diffrn_measured_fraction_theta_full 0.978 _diffrn_measured_fraction_theta_max 0.978 _diffrn_measurement_device_type 'Rigaku Saturn724' _diffrn_measurement_method \W _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0628 _diffrn_reflns_av_unetI/netI 0.0582 _diffrn_reflns_Laue_measured_fraction_full 0.978 _diffrn_reflns_Laue_measured_fraction_max 0.978 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 18037 _diffrn_reflns_point_group_measured_fraction_full 0.978 _diffrn_reflns_point_group_measured_fraction_max 0.978 _diffrn_reflns_theta_full 24.999 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_min 3.068 _exptl_absorpt_coefficient_mu 1.954 _exptl_absorpt_correction_T_max 0.647 _exptl_absorpt_correction_T_min 0.58 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.660 _exptl_crystal_description needles _exptl_crystal_F_000 1291 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _refine_diff_density_max 2.194 _refine_diff_density_min -2.330 _refine_diff_density_rms 0.204 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 628 _refine_ls_number_reflns 8863 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.074 _refine_ls_R_factor_all 0.0805 _refine_ls_R_factor_gt 0.0781 _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^)+(0.0914P)^2^+44.5591P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2174 _refine_ls_wR_factor_ref 0.2189 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8447 _reflns_number_total 8863 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt02763j2.cif _cod_data_source_block 5 _cod_database_code 7044230 _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 0.696 _shelx_estimated_absorpt_t_max 0.696 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL gb-598 CELL 0.71075 10.3310 13.9700 19.6440 95.549 99.530 111.171 ZERR 1.00 0.0040 0.0060 0.0080 0.003 0.006 0.008 LATT 1 SFAC C H CU I N O P UNIT 94 120 3 4 8 24 4 MERG 2 OMIT -4.00 50.00 OMIT -4 1 1 OMIT -5 4 1 OMIT -1 -8 6 OMIT -4 -2 3 OMIT -3 -5 4 OMIT -1 -9 4 MORE -1 HTAB C1 O7 EQIV $1 -x+2, -y+1, -z+1 HTAB C4 O11_$1 HTAB C7 O11_$1 EQIV $2 x+1, y, z HTAB C9 O10_$2 HTAB C12 O3_$2 EQIV $3 -x+2, -y, -z HTAB C14 I2_$3 HTAB C18 O10_$2 HTAB O10 O3 HTAB O9 O7 HTAB C46 O7 HTAB O11 O3 EQIV $4 -x+1, -y, -z+1 HTAB O12 O9_$4 HTAB O12 O7 FMAP 2 SIZE 0.200 0.200 0.200 ACTA HTAB 2.00000 BOND $H CONF LIST 4 WPDB -2 L.S. 30 TEMP -143.00 WGHT 0.091400 44.559097 FVAR 0.76248 I1 4 0.935548 0.710232 0.002085 11.00000 0.04649 0.03916 = 0.03856 0.02082 0.00653 0.01947 I2 4 0.792915 -0.031975 -0.005921 11.00000 0.05471 0.04231 = 0.02708 0.00055 0.00948 0.01557 CU1 3 1.035501 0.279913 0.353324 11.00000 0.01401 0.00985 = 0.00733 -0.00212 -0.00086 0.00233 CU2 3 1.000000 0.000000 0.500000 10.50000 0.01595 0.01062 = 0.00928 0.00133 -0.00617 0.00097 P1 7 0.804050 0.335527 0.244177 11.00000 0.01692 0.01331 = 0.01286 0.00294 -0.00008 0.00587 P2 7 0.827056 0.052333 0.366005 11.00000 0.01191 0.00879 = 0.00910 -0.00053 -0.00330 0.00196 O1 6 0.858108 0.344653 0.171546 11.00000 0.02183 0.01213 = 0.01260 0.00106 0.00188 0.00744 O2 6 0.930022 0.371389 0.305079 11.00000 0.02104 0.00911 = 0.01232 0.00049 -0.00195 0.00460 O3 6 0.699479 0.386575 0.247171 11.00000 0.02298 0.03061 = 0.02619 0.01006 0.00461 0.01695 O4 6 0.724875 0.213060 0.233903 11.00000 0.01950 0.01162 = 0.02185 0.00332 -0.00571 -0.00128 O5 6 0.754270 -0.050307 0.305561 11.00000 0.02134 0.01326 = 0.00816 -0.00409 -0.00559 0.00412 O6 6 0.876252 0.145677 0.327128 11.00000 0.01775 0.01232 = 0.00938 0.00152 -0.00319 0.00293 O7 6 0.713331 0.052774 0.405163 11.00000 0.01759 0.02069 = 0.01210 0.00099 0.00177 0.00462 O8 6 0.953938 0.040471 0.410063 11.00000 0.01639 0.01612 = 0.01418 0.00590 -0.00127 0.00636 N1 5 1.023475 0.331740 0.452728 11.00000 0.01782 0.01517 = 0.01438 0.00123 0.00087 0.00682 N2 5 1.222122 0.393412 0.383913 11.00000 0.01594 0.01214 = 0.00888 -0.00187 -0.00226 0.00317 N3 5 1.126189 0.263704 0.270166 11.00000 0.01824 0.00986 = 0.01174 -0.00041 -0.00151 0.00487 N4 5 0.836941 -0.142275 0.474481 11.00000 0.01323 0.01132 = 0.01581 -0.00006 -0.00354 0.00284 C1 1 0.919560 0.293446 0.486086 11.00000 0.02119 0.01080 = 0.01798 0.00022 0.00339 0.00101 AFIX 43 H1 2 0.841184 0.231170 0.464012 11.00000 -1.20000 AFIX 0 C1AA 1 0.431256 -0.142869 0.222936 11.00000 0.02408 0.02246 = 0.04572 0.00303 0.00368 0.00518 AFIX 33 H1AA 2 0.347334 -0.140801 0.239075 11.00000 -1.20000 H1AB 2 0.401088 -0.190344 0.178072 11.00000 -1.20000 H1AC 2 0.485915 -0.167503 0.257644 11.00000 -1.20000 AFIX 0 C2 1 0.919919 0.340174 0.551880 11.00000 0.02922 0.01844 = 0.02027 -0.00173 0.01266 0.00344 AFIX 43 H2 2 0.843837 0.309672 0.574306 11.00000 -1.20000 AFIX 0 C3 1 1.030909 0.430461 0.583942 11.00000 0.02951 0.02226 = 0.00951 -0.00706 0.00508 0.00465 AFIX 43 H3 2 1.031815 0.464618 0.628355 11.00000 -1.20000 AFIX 0 C4 1 1.144058 0.472216 0.550189 11.00000 0.01509 0.01656 = 0.01413 -0.00093 0.00000 0.00298 AFIX 43 H4 2 1.224077 0.533759 0.571785 11.00000 -1.20000 AFIX 0 C5 1 1.135169 0.421056 0.484842 11.00000 0.01398 0.01298 = 0.01150 0.00225 -0.00017 0.00461 C6 1 1.247701 0.457574 0.444254 11.00000 0.01598 0.01271 = 0.01031 0.00145 0.00134 0.00551 C7 1 1.369848 0.548378 0.463301 11.00000 0.01656 0.01233 = 0.00840 -0.00408 -0.00416 0.00428 AFIX 43 H7 2 1.385641 0.595361 0.504988 11.00000 -1.20000 AFIX 0 C8 1 1.469064 0.569959 0.420700 11.00000 0.00990 0.01279 = 0.01592 0.00353 -0.00258 0.00501 C9 1 1.440720 0.499923 0.358741 11.00000 0.01508 0.00980 = 0.01942 0.00202 0.00241 0.00700 AFIX 43 H9 2 1.506578 0.512116 0.328926 11.00000 -1.20000 AFIX 0 C10 1 1.314025 0.412040 0.341723 11.00000 0.01324 0.01248 = 0.01217 0.00052 -0.00356 0.00759 C11 1 1.260855 0.331742 0.277016 11.00000 0.02088 0.00947 = 0.01199 0.00118 -0.00168 0.00419 C12 1 1.339658 0.329782 0.225911 11.00000 0.01556 0.01862 = 0.01840 0.00002 0.00288 0.00641 AFIX 43 H12 2 1.435140 0.377711 0.232373 11.00000 -1.20000 AFIX 0 C13 1 1.273926 0.255172 0.164894 11.00000 0.02519 0.02396 = 0.01552 -0.00515 0.00597 0.01019 AFIX 43 H13 2 1.324841 0.250029 0.129549 11.00000 -1.20000 AFIX 0 C14 1 1.133356 0.189092 0.157101 11.00000 0.03183 0.01624 = 0.01147 -0.00330 0.00042 0.00393 AFIX 43 H14 2 1.085384 0.140459 0.115042 11.00000 -1.20000 AFIX 0 C15 1 1.062625 0.193797 0.210515 11.00000 0.01563 0.01638 = 0.01217 -0.00269 -0.00315 0.00345 AFIX 43 H15 2 0.966995 0.146653 0.205038 11.00000 -1.20000 AFIX 0 C47 1 1.599483 0.667906 0.439149 11.00000 0.01571 0.01328 = 0.01000 -0.00415 -0.00669 0.00827 C17 1 1.640245 0.729641 0.506077 11.00000 0.01866 0.02105 = 0.00665 -0.00390 -0.00313 0.00819 AFIX 43 H17 2 1.587937 0.707544 0.541042 11.00000 -1.20000 AFIX 0 C18 1 1.685158 0.703318 0.392031 11.00000 0.02122 0.01650 = 0.01058 -0.00301 0.00138 0.00410 AFIX 43 H18 2 1.663913 0.663479 0.346687 11.00000 -1.20000 AFIX 0 C19 1 0.756922 -0.177472 0.520311 11.00000 0.01466 0.01744 = 0.01261 -0.00408 -0.00527 0.00447 AFIX 43 H19 2 0.781627 -0.136224 0.565419 11.00000 -1.20000 AFIX 0 C20 1 0.802299 -0.202602 0.411455 11.00000 0.02192 0.01771 = 0.01132 0.00352 0.00221 0.00537 AFIX 43 H20 2 0.860278 -0.180080 0.378698 11.00000 -1.20000 AFIX 0 C21 1 0.765942 -0.050698 0.234754 11.00000 0.01687 0.00729 = 0.01021 -0.00278 -0.00595 0.00392 C22 1 0.877820 -0.068457 0.213357 11.00000 0.01767 0.00930 = 0.02133 -0.00205 -0.00194 0.00329 C23 1 0.881791 -0.068265 0.142323 11.00000 0.02611 0.01442 = 0.02283 -0.00536 0.00914 0.00465 AFIX 43 H23 2 0.954313 -0.082940 0.124916 11.00000 -1.20000 AFIX 0 C24 1 0.782005 -0.047097 0.097506 11.00000 0.03005 0.02096 = 0.01333 -0.00269 -0.00300 0.01005 C25 1 0.665631 -0.034134 0.119659 11.00000 0.02234 0.02135 = 0.01320 -0.00155 -0.00099 0.00606 AFIX 43 H25 2 0.595288 -0.023049 0.087348 11.00000 -1.20000 AFIX 0 C26 1 0.654063 -0.037586 0.188523 11.00000 0.01566 0.00965 = 0.01692 -0.00479 -0.00711 0.00177 C27 1 0.523918 -0.033668 0.213606 11.00000 0.02119 0.01737 = 0.02147 -0.00030 0.00076 0.00616 AFIX 13 H27 2 0.557331 0.012485 0.260419 11.00000 -1.20000 AFIX 0 C28 1 0.437402 0.010610 0.164160 11.00000 0.02077 0.03619 = 0.02923 0.00152 -0.00655 0.01563 AFIX 33 H28A 2 0.355282 0.011381 0.182687 11.00000 -1.20000 H28B 2 0.497268 0.081776 0.160510 11.00000 -1.20000 H28C 2 0.404383 -0.033038 0.117692 11.00000 -1.20000 AFIX 0 C29 1 0.990506 -0.087851 0.264909 11.00000 0.02481 0.02199 = 0.02547 0.00459 0.00388 0.01198 AFIX 13 H29 2 0.966537 -0.082130 0.312019 11.00000 -1.20000 AFIX 0 C30 1 0.988711 -0.196759 0.247271 11.00000 0.10494 0.05089 = 0.07157 -0.01719 -0.03590 0.05807 AFIX 33 H30A 2 1.062325 -0.205523 0.281549 11.00000 -1.20000 H30B 2 0.895391 -0.248414 0.248607 11.00000 -1.20000 H30C 2 1.007258 -0.206554 0.200286 11.00000 -1.20000 AFIX 0 C31 1 1.139309 -0.003485 0.271021 11.00000 0.02103 0.09614 = 0.06069 0.05157 -0.00491 0.01324 AFIX 33 H31A 2 1.136528 0.065515 0.282396 11.00000 -1.20000 H31B 2 1.207251 -0.013111 0.308151 11.00000 -1.20000 H31C 2 1.168880 -0.009149 0.226406 11.00000 -1.20000 AFIX 0 C32 1 0.874612 0.427785 0.134376 11.00000 0.02757 0.01719 = 0.00667 0.00411 0.00156 0.01563 C33 1 1.004186 0.512231 0.149555 11.00000 0.02470 0.01629 = 0.01262 0.00123 0.00160 0.01119 C34 1 1.020826 0.592984 0.110087 11.00000 0.01965 0.01804 = 0.02145 0.00510 0.00042 0.00575 AFIX 43 H34 2 1.107494 0.652352 0.119719 11.00000 -1.20000 AFIX 0 C35 1 0.909505 0.584747 0.057193 11.00000 0.03292 0.02106 = 0.02468 0.01008 0.01018 0.01466 C36 1 0.784034 0.498766 0.039656 11.00000 0.02039 0.02738 = 0.01575 0.00650 -0.00125 0.01153 AFIX 43 H36 2 0.711771 0.494304 0.001197 11.00000 -1.20000 AFIX 0 C37 1 0.763106 0.417753 0.078694 11.00000 0.01730 0.01943 = 0.00433 -0.00203 -0.00371 0.00333 C38 1 0.627967 0.319153 0.061083 11.00000 0.01756 0.02177 = 0.01953 -0.00134 -0.00214 0.00130 AFIX 13 H38 2 0.599309 0.301707 0.105958 11.00000 -1.20000 AFIX 0 C39 1 0.655158 0.227111 0.025870 11.00000 0.02770 0.02755 = 0.04254 -0.00912 -0.00088 0.00691 AFIX 33 H39A 2 0.567175 0.164622 0.014996 11.00000 -1.20000 H39B 2 0.686770 0.243457 -0.017496 11.00000 -1.20000 H39C 2 0.728862 0.214587 0.057667 11.00000 -1.20000 AFIX 0 C40 1 0.502397 0.333244 0.013338 11.00000 0.02448 0.03443 = 0.04054 0.00948 -0.00498 -0.00144 AFIX 33 H40A 2 0.418322 0.268044 0.003527 11.00000 -1.20000 H40B 2 0.481094 0.388949 0.037160 11.00000 -1.20000 H40C 2 0.528649 0.351620 -0.030761 11.00000 -1.20000 AFIX 0 C41 1 1.130310 0.520425 0.206774 11.00000 0.01636 0.01829 = 0.01659 0.00263 -0.00399 0.00589 AFIX 13 H41 2 1.105193 0.453043 0.224942 11.00000 -1.20000 AFIX 0 C42 1 1.158789 0.607102 0.267578 11.00000 0.03222 0.03084 = 0.01347 0.00239 -0.00584 0.01366 AFIX 33 H42A 2 1.239505 0.611158 0.303527 11.00000 -1.20000 H42B 2 1.180847 0.673658 0.250564 11.00000 -1.20000 H42C 2 1.074312 0.592185 0.287713 11.00000 -1.20000 AFIX 0 C43 1 1.264781 0.538452 0.176765 11.00000 0.02163 0.02661 = 0.02852 0.00253 0.00020 0.01115 AFIX 33 H43A 2 1.244485 0.482090 0.137817 11.00000 -1.20000 H43B 2 1.292911 0.605252 0.159925 11.00000 -1.20000 H43C 2 1.342225 0.539445 0.213521 11.00000 -1.20000 AFIX 0 O10 6 0.646478 0.561011 0.242203 11.00000 0.04083 0.02749 = 0.03088 0.00467 0.01421 0.01945 AFIX 147 H10 2 0.682912 0.516141 0.241039 11.00000 -1.50000 AFIX 0 C44 1 0.629283 0.591864 0.174562 11.00000 0.04483 0.05378 = 0.02290 0.00052 0.00786 0.02659 AFIX 137 H44A 2 0.548106 0.536987 0.142175 11.00000 -1.50000 H44B 2 0.715656 0.602991 0.156559 11.00000 -1.50000 H44C 2 0.612375 0.656624 0.178888 11.00000 -1.50000 AFIX 0 O9 6 0.427962 -0.044094 0.397573 11.00000 0.02376 0.03333 = 0.04643 0.01170 0.00621 0.01094 AFIX 147 H9A 2 0.506129 -0.004742 0.390446 11.00000 -1.50000 AFIX 0 C46 1 0.439497 -0.136578 0.416483 11.00000 0.03539 0.03532 = 0.09041 0.02358 0.02291 0.01231 AFIX 137 H46A 2 0.367648 -0.197042 0.383840 11.00000 -1.50000 H46B 2 0.424355 -0.141734 0.464164 11.00000 -1.50000 H46C 2 0.534459 -0.134872 0.414512 11.00000 -1.50000 AFIX 0 O11 6 0.571325 0.318010 0.362868 11.00000 0.02722 0.01810 = 0.03046 -0.00351 0.00565 0.00760 AFIX 147 H11 2 0.608624 0.340848 0.329828 11.00000 -1.50000 AFIX 0 C45 1 0.517447 0.205466 0.350078 11.00000 0.05633 0.02550 = 0.04616 0.00200 0.02059 0.01728 AFIX 137 H45A 2 0.459587 0.179043 0.302360 11.00000 -1.50000 H45B 2 0.458965 0.178424 0.383729 11.00000 -1.50000 H45C 2 0.597266 0.182642 0.355474 11.00000 -1.50000 AFIX 6 O12 6 0.823039 0.066241 0.545239 11.00000 0.03456 0.02732 = 0.02250 0.00078 -0.00012 0.01464 H12A 2 0.768767 0.056260 0.575519 11.00000 -1.50000 H12B 2 0.770531 0.047877 0.503039 11.00000 -1.50000 AFIX 0 HKLF 4 REM gb-598 REM R1 = 0.0781 for 8447 Fo > 4sig(Fo) and 0.0805 for all 8863 data REM 628 parameters refined using 0 restraints END WGHT 0.0914 44.5498 REM Instructions for potential hydrogen bonds HTAB C1 O7 HTAB C4 O11_$1 HTAB C7 O11_$1 HTAB C9 O10_$2 HTAB C12 O3_$2 HTAB C14 I2_$3 HTAB C18 O10_$2 HTAB O10 O3 HTAB O9 O7 HTAB C46 O7 HTAB O11 O3 HTAB O12 O9_$4 HTAB O12 O7 REM Highest difference peak 2.194, deepest hole -2.330, 1-sigma level 0.204 Q1 1 0.8120 -0.0138 0.0547 11.00000 0.05 2.19 Q2 1 0.9646 0.7297 0.0625 11.00000 0.05 2.03 Q3 1 0.9038 0.6887 -0.0590 11.00000 0.05 1.96 Q4 1 0.7630 -0.0530 -0.0652 11.00000 0.05 1.94 Q5 1 1.0589 0.2924 0.3945 11.00000 0.05 0.96 Q6 1 0.8640 0.0127 0.1275 11.00000 0.05 0.96 Q7 1 0.2651 0.0630 0.1208 11.00000 0.05 0.93 Q8 1 0.9914 -0.2450 0.1238 11.00000 0.05 0.82 Q9 1 0.8671 0.3580 0.2701 11.00000 0.05 0.81 Q10 1 0.9843 -0.0306 -0.0212 11.00000 0.05 0.80 Q11 1 0.8351 0.2106 -0.0256 11.00000 0.05 0.78 Q12 1 1.1301 0.3328 0.1203 11.00000 0.05 0.78 Q13 1 0.5644 -0.0961 0.0492 11.00000 0.05 0.73 Q14 1 1.2792 0.3839 0.3723 11.00000 0.05 0.71 Q15 1 0.3031 0.3526 -0.0463 11.00000 0.05 0.71 Q16 1 0.9209 0.2668 0.4023 11.00000 0.05 0.70 Q17 1 1.6258 0.6871 0.4717 11.00000 0.05 0.70 Q18 1 0.7807 0.1979 0.2690 11.00000 0.05 0.70 Q19 1 0.9620 -0.0559 0.0434 11.00000 0.05 0.69 Q20 1 1.2801 0.4268 0.4326 11.00000 0.05 0.68 ; _shelx_res_checksum 18534 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 I1 I 0.93555(8) 0.71023(5) 0.00208(4) 0.0398(2) Uani 1 1 d . . . I2 I 0.79291(8) -0.03198(6) -0.00592(4) 0.0426(2) Uani 1 1 d . . . Cu1 Cu 1.03550(9) 0.27991(7) 0.35332(4) 0.0117(2) Uani 1 1 d . . . Cu2 Cu 1.0000 0.0000 0.5000 0.0143(3) Uani 1 2 d S . P P1 P 0.8041(2) 0.33553(15) 0.24418(10) 0.0147(4) Uani 1 1 d . . . P2 P 0.8271(2) 0.05233(14) 0.36601(10) 0.0114(4) Uani 1 1 d . . . O1 O 0.8581(6) 0.3447(4) 0.1715(3) 0.0156(11) Uani 1 1 d . . . O2 O 0.9300(6) 0.3714(4) 0.3051(3) 0.0153(11) Uani 1 1 d . . . O3 O 0.6995(6) 0.3866(5) 0.2472(3) 0.0244(13) Uani 1 1 d . . . O4 O 0.7249(6) 0.2131(4) 0.2339(3) 0.0210(12) Uani 1 1 d . . . O5 O 0.7543(6) -0.0503(4) 0.3056(3) 0.0165(11) Uani 1 1 d . . . O6 O 0.8763(6) 0.1457(4) 0.3271(3) 0.0148(11) Uani 1 1 d . . . O7 O 0.7133(6) 0.0528(4) 0.4052(3) 0.0179(11) Uani 1 1 d . . . O8 O 0.9539(6) 0.0405(4) 0.4101(3) 0.0159(11) Uani 1 1 d . . . N1 N 1.0235(7) 0.3317(5) 0.4527(3) 0.0161(13) Uani 1 1 d . . . N2 N 1.2221(7) 0.3934(5) 0.3839(3) 0.0138(13) Uani 1 1 d . . . N3 N 1.1262(7) 0.2637(5) 0.2702(3) 0.0142(13) Uani 1 1 d . . . N4 N 0.8369(7) -0.1423(5) 0.4745(3) 0.0150(13) Uani 1 1 d . . . C1 C 0.9196(9) 0.2934(6) 0.4861(4) 0.0184(16) Uani 1 1 d . . . H1 H 0.8412 0.2312 0.4640 0.022 Uiso 1 1 calc R U . C1AA C 0.4313(10) -0.1429(7) 0.2229(6) 0.033(2) Uani 1 1 d . . . H1AA H 0.3473 -0.1408 0.2391 0.039 Uiso 1 1 calc R U . H1AB H 0.4011 -0.1903 0.1781 0.039 Uiso 1 1 calc R U . H1AC H 0.4859 -0.1675 0.2576 0.039 Uiso 1 1 calc R U . C2 C 0.9199(10) 0.3402(7) 0.5519(4) 0.0237(18) Uani 1 1 d . . . H2 H 0.8438 0.3097 0.5743 0.028 Uiso 1 1 calc R U . C3 C 1.0309(9) 0.4305(7) 0.5839(4) 0.0225(18) Uani 1 1 d . . . H3 H 1.0318 0.4646 0.6284 0.027 Uiso 1 1 calc R U . C4 C 1.1441(8) 0.4722(6) 0.5502(4) 0.0168(16) Uani 1 1 d . . . H4 H 1.2241 0.5338 0.5718 0.020 Uiso 1 1 calc R U . C5 C 1.1352(8) 0.4211(6) 0.4848(4) 0.0133(15) Uani 1 1 d . . . C6 C 1.2477(8) 0.4576(6) 0.4443(4) 0.0132(15) Uani 1 1 d . . . C7 C 1.3698(8) 0.5484(6) 0.4633(4) 0.0141(15) Uani 1 1 d . . . H7 H 1.3856 0.5954 0.5050 0.017 Uiso 1 1 calc R U . C8 C 1.4691(8) 0.5700(6) 0.4207(4) 0.0133(15) Uani 1 1 d . . . C9 C 1.4407(8) 0.4999(6) 0.3587(4) 0.0143(15) Uani 1 1 d . . . H9 H 1.5066 0.5121 0.3289 0.017 Uiso 1 1 calc R U . C10 C 1.3140(8) 0.4120(6) 0.3417(4) 0.0128(15) Uani 1 1 d . . . C11 C 1.2609(8) 0.3317(6) 0.2770(4) 0.0153(15) Uani 1 1 d . . . C12 C 1.3397(8) 0.3298(6) 0.2259(4) 0.0179(16) Uani 1 1 d . . . H12 H 1.4351 0.3777 0.2324 0.021 Uiso 1 1 calc R U . C13 C 1.2739(9) 0.2552(7) 0.1649(4) 0.0218(18) Uani 1 1 d . . . H13 H 1.3248 0.2500 0.1295 0.026 Uiso 1 1 calc R U . C14 C 1.1334(10) 0.1891(6) 0.1571(4) 0.0223(18) Uani 1 1 d . . . H14 H 1.0854 0.1405 0.1150 0.027 Uiso 1 1 calc R U . C15 C 1.0626(8) 0.1938(6) 0.2105(4) 0.0166(16) Uani 1 1 d . . . H15 H 0.9670 0.1467 0.2050 0.020 Uiso 1 1 calc R U . C47 C 1.5995(8) 0.6679(6) 0.4391(4) 0.0138(15) Uani 1 1 d . . . C17 C 1.6402(8) 0.7296(6) 0.5061(4) 0.0165(16) Uani 1 1 d . . . H17 H 1.5879 0.7075 0.5410 0.020 Uiso 1 1 calc R U . C18 C 1.6852(9) 0.7033(6) 0.3920(4) 0.0176(16) Uani 1 1 d . . . H18 H 1.6639 0.6635 0.3467 0.021 Uiso 1 1 calc R U . C19 C 0.7569(8) -0.1775(6) 0.5203(4) 0.0169(16) Uani 1 1 d . . . H19 H 0.7816 -0.1362 0.5654 0.020 Uiso 1 1 calc R U . C20 C 0.8023(9) -0.2026(6) 0.4115(4) 0.0177(16) Uani 1 1 d . . . H20 H 0.8603 -0.1801 0.3787 0.021 Uiso 1 1 calc R U . C21 C 0.7659(8) -0.0507(5) 0.2348(4) 0.0131(15) Uani 1 1 d . . . C22 C 0.8778(8) -0.0685(6) 0.2134(4) 0.0177(16) Uani 1 1 d . . . C23 C 0.8818(9) -0.0683(6) 0.1423(4) 0.0222(18) Uani 1 1 d . . . H23 H 0.9543 -0.0829 0.1249 0.027 Uiso 1 1 calc R U . C24 C 0.7820(10) -0.0471(7) 0.0975(4) 0.0227(18) Uani 1 1 d . . . C25 C 0.6656(9) -0.0341(6) 0.1197(4) 0.0206(17) Uani 1 1 d . . . H25 H 0.5953 -0.0230 0.0873 0.025 Uiso 1 1 calc R U . C26 C 0.6541(8) -0.0376(6) 0.1885(4) 0.0168(16) Uani 1 1 d . . . C27 C 0.5239(9) -0.0337(6) 0.2136(4) 0.0211(17) Uani 1 1 d . . . H27 H 0.5573 0.0125 0.2604 0.025 Uiso 1 1 calc R U . C28 C 0.4374(10) 0.0106(8) 0.1642(5) 0.029(2) Uani 1 1 d . . . H28A H 0.3553 0.0114 0.1827 0.035 Uiso 1 1 calc R U . H28B H 0.4973 0.0818 0.1605 0.035 Uiso 1 1 calc R U . H28C H 0.4044 -0.0330 0.1177 0.035 Uiso 1 1 calc R U . C29 C 0.9905(9) -0.0879(7) 0.2649(5) 0.0234(18) Uani 1 1 d . . . H29 H 0.9665 -0.0821 0.3120 0.028 Uiso 1 1 calc R U . C30 C 0.9887(19) -0.1968(11) 0.2473(8) 0.077(5) Uani 1 1 d . . . H30A H 1.0623 -0.2055 0.2815 0.092 Uiso 1 1 calc R U . H30B H 0.8954 -0.2484 0.2486 0.092 Uiso 1 1 calc R U . H30C H 1.0073 -0.2066 0.2003 0.092 Uiso 1 1 calc R U . C31 C 1.1393(11) -0.0035(12) 0.2710(7) 0.061(4) Uani 1 1 d . . . H31A H 1.1365 0.0655 0.2824 0.073 Uiso 1 1 calc R U . H31B H 1.2073 -0.0131 0.3082 0.073 Uiso 1 1 calc R U . H31C H 1.1689 -0.0091 0.2264 0.073 Uiso 1 1 calc R U . C32 C 0.8746(9) 0.4278(6) 0.1344(4) 0.0152(15) Uani 1 1 d . . . C33 C 1.0042(9) 0.5122(6) 0.1496(4) 0.0173(16) Uani 1 1 d . . . C34 C 1.0208(9) 0.5930(6) 0.1101(4) 0.0205(17) Uani 1 1 d . . . H34 H 1.1075 0.6524 0.1197 0.025 Uiso 1 1 calc R U . C35 C 0.9095(10) 0.5847(7) 0.0572(5) 0.0240(18) Uani 1 1 d . . . C36 C 0.7840(9) 0.4988(7) 0.0397(4) 0.0209(17) Uani 1 1 d . . . H36 H 0.7118 0.4943 0.0012 0.025 Uiso 1 1 calc R U . C37 C 0.7631(8) 0.4178(6) 0.0787(4) 0.0158(16) Uani 1 1 d . . . C38 C 0.6280(9) 0.3192(7) 0.0611(4) 0.0225(18) Uani 1 1 d . . . H38 H 0.5993 0.3017 0.1060 0.027 Uiso 1 1 calc R U . C39 C 0.6552(11) 0.2271(8) 0.0259(6) 0.036(2) Uani 1 1 d . . . H39A H 0.5672 0.1646 0.0150 0.043 Uiso 1 1 calc R U . H39B H 0.6868 0.2435 -0.0175 0.043 Uiso 1 1 calc R U . H39C H 0.7289 0.2146 0.0577 0.043 Uiso 1 1 calc R U . C40 C 0.5024(10) 0.3332(8) 0.0133(6) 0.038(2) Uani 1 1 d . . . H40A H 0.4183 0.2680 0.0035 0.046 Uiso 1 1 calc R U . H40B H 0.4811 0.3889 0.0372 0.046 Uiso 1 1 calc R U . H40C H 0.5286 0.3516 -0.0308 0.046 Uiso 1 1 calc R U . C41 C 1.1303(8) 0.5204(6) 0.2068(4) 0.0183(16) Uani 1 1 d . . . H41 H 1.1052 0.4530 0.2249 0.022 Uiso 1 1 calc R U . C42 C 1.1588(10) 0.6071(7) 0.2676(4) 0.0265(19) Uani 1 1 d . . . H42A H 1.2395 0.6112 0.3035 0.032 Uiso 1 1 calc R U . H42B H 1.1808 0.6737 0.2506 0.032 Uiso 1 1 calc R U . H42C H 1.0743 0.5922 0.2877 0.032 Uiso 1 1 calc R U . C43 C 1.2648(9) 0.5385(7) 0.1768(5) 0.0259(19) Uani 1 1 d . . . H43A H 1.2445 0.4821 0.1378 0.031 Uiso 1 1 calc R U . H43B H 1.2929 0.6053 0.1599 0.031 Uiso 1 1 calc R U . H43C H 1.3422 0.5394 0.2135 0.031 Uiso 1 1 calc R U . O10 O 0.6465(8) 0.5610(5) 0.2422(3) 0.0305(15) Uani 1 1 d . . . H10 H 0.6829 0.5161 0.2410 0.046 Uiso 1 1 calc R U . C44 C 0.6293(12) 0.5919(9) 0.1746(5) 0.039(2) Uani 1 1 d . . . H44A H 0.5481 0.5370 0.1422 0.058 Uiso 1 1 calc R U . H44B H 0.7157 0.6030 0.1566 0.058 Uiso 1 1 calc R U . H44C H 0.6124 0.6566 0.1789 0.058 Uiso 1 1 calc R U . O9 O 0.4280(7) -0.0441(5) 0.3976(4) 0.0343(16) Uani 1 1 d . . . H9A H 0.5061 -0.0047 0.3904 0.051 Uiso 1 1 calc R U . C46 C 0.4395(12) -0.1366(9) 0.4165(8) 0.052(3) Uani 1 1 d . . . H46A H 0.3676 -0.1970 0.3838 0.078 Uiso 1 1 calc R U . H46B H 0.4244 -0.1417 0.4642 0.078 Uiso 1 1 calc R U . H46C H 0.5345 -0.1349 0.4145 0.078 Uiso 1 1 calc R U . O11 O 0.5713(7) 0.3180(5) 0.3629(3) 0.0262(13) Uani 1 1 d . . . H11 H 0.6086 0.3408 0.3298 0.039 Uiso 1 1 calc R U . C45 C 0.5174(13) 0.2055(8) 0.3501(6) 0.041(3) Uani 1 1 d . . . H45A H 0.4596 0.1790 0.3024 0.062 Uiso 1 1 calc R U . H45B H 0.4590 0.1784 0.3837 0.062 Uiso 1 1 calc R U . H45C H 0.5973 0.1826 0.3555 0.062 Uiso 1 1 calc R U . O12 O 0.8230(7) 0.0662(5) 0.5452(3) 0.0284(14) Uani 1 1 d G . . H12A H 0.7688 0.0563 0.5755 0.043 Uiso 1 1 d G U . H12B H 0.7705 0.0479 0.5030 0.043 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 I1 0.0465(4) 0.0392(4) 0.0386(4) 0.0208(3) 0.0065(3) 0.0195(3) I2 0.0547(5) 0.0423(4) 0.0271(4) 0.0006(3) 0.0095(3) 0.0156(3) Cu1 0.0140(5) 0.0098(4) 0.0073(4) -0.0021(3) -0.0009(3) 0.0023(4) Cu2 0.0159(7) 0.0106(6) 0.0093(6) 0.0013(5) -0.0062(5) 0.0010(5) P1 0.0169(10) 0.0133(10) 0.0129(10) 0.0029(7) -0.0001(8) 0.0059(8) P2 0.0119(9) 0.0088(9) 0.0091(9) -0.0005(7) -0.0033(7) 0.0020(7) O1 0.022(3) 0.012(3) 0.013(3) 0.001(2) 0.002(2) 0.007(2) O2 0.021(3) 0.009(2) 0.012(3) 0.000(2) -0.002(2) 0.005(2) O3 0.023(3) 0.031(3) 0.026(3) 0.010(3) 0.005(2) 0.017(3) O4 0.020(3) 0.012(3) 0.022(3) 0.003(2) -0.006(2) -0.001(2) O5 0.021(3) 0.013(3) 0.008(3) -0.004(2) -0.006(2) 0.004(2) O6 0.018(3) 0.012(3) 0.009(3) 0.002(2) -0.003(2) 0.003(2) O7 0.018(3) 0.021(3) 0.012(3) 0.001(2) 0.002(2) 0.005(2) O8 0.016(3) 0.016(3) 0.014(3) 0.006(2) -0.001(2) 0.006(2) N1 0.018(3) 0.015(3) 0.014(3) 0.001(3) 0.001(3) 0.007(3) N2 0.016(3) 0.012(3) 0.009(3) -0.002(2) -0.002(2) 0.003(3) N3 0.018(3) 0.010(3) 0.012(3) 0.000(2) -0.002(3) 0.005(3) N4 0.013(3) 0.011(3) 0.016(3) 0.000(2) -0.004(3) 0.003(3) C1 0.021(4) 0.011(4) 0.018(4) 0.000(3) 0.003(3) 0.001(3) C1AA 0.024(5) 0.022(5) 0.046(6) 0.003(4) 0.004(4) 0.005(4) C2 0.029(5) 0.018(4) 0.020(4) -0.002(3) 0.013(4) 0.003(4) C3 0.030(5) 0.022(4) 0.010(4) -0.007(3) 0.005(3) 0.005(4) C4 0.015(4) 0.017(4) 0.014(4) -0.001(3) 0.000(3) 0.003(3) C5 0.014(4) 0.013(4) 0.011(4) 0.002(3) 0.000(3) 0.005(3) C6 0.016(4) 0.013(4) 0.010(4) 0.001(3) 0.001(3) 0.006(3) C7 0.017(4) 0.012(4) 0.008(4) -0.004(3) -0.004(3) 0.004(3) C8 0.010(3) 0.013(4) 0.016(4) 0.004(3) -0.003(3) 0.005(3) C9 0.015(4) 0.010(3) 0.019(4) 0.002(3) 0.002(3) 0.007(3) C10 0.013(4) 0.012(4) 0.012(4) 0.001(3) -0.004(3) 0.008(3) C11 0.021(4) 0.009(3) 0.012(4) 0.001(3) -0.002(3) 0.004(3) C12 0.016(4) 0.019(4) 0.018(4) 0.000(3) 0.003(3) 0.006(3) C13 0.025(4) 0.024(4) 0.016(4) -0.005(3) 0.006(3) 0.010(4) C14 0.032(5) 0.016(4) 0.011(4) -0.003(3) 0.000(3) 0.004(4) C15 0.016(4) 0.016(4) 0.012(4) -0.003(3) -0.003(3) 0.003(3) C47 0.016(4) 0.013(4) 0.010(4) -0.004(3) -0.007(3) 0.008(3) C17 0.019(4) 0.021(4) 0.007(4) -0.004(3) -0.003(3) 0.008(3) C18 0.021(4) 0.016(4) 0.011(4) -0.003(3) 0.001(3) 0.004(3) C19 0.015(4) 0.017(4) 0.013(4) -0.004(3) -0.005(3) 0.004(3) C20 0.022(4) 0.018(4) 0.011(4) 0.004(3) 0.002(3) 0.005(3) C21 0.017(4) 0.007(3) 0.010(4) -0.003(3) -0.006(3) 0.004(3) C22 0.018(4) 0.009(4) 0.021(4) -0.002(3) -0.002(3) 0.003(3) C23 0.026(4) 0.014(4) 0.023(4) -0.005(3) 0.009(3) 0.005(3) C24 0.030(5) 0.021(4) 0.013(4) -0.003(3) -0.003(3) 0.010(4) C25 0.022(4) 0.021(4) 0.013(4) -0.002(3) -0.001(3) 0.006(3) C26 0.016(4) 0.010(4) 0.017(4) -0.005(3) -0.007(3) 0.002(3) C27 0.021(4) 0.017(4) 0.021(4) 0.000(3) 0.001(3) 0.006(3) C28 0.021(4) 0.036(5) 0.029(5) 0.002(4) -0.007(4) 0.016(4) C29 0.025(4) 0.022(4) 0.025(5) 0.005(3) 0.004(4) 0.012(4) C30 0.105(12) 0.051(8) 0.072(10) -0.017(7) -0.036(9) 0.058(9) C31 0.021(5) 0.096(10) 0.061(8) 0.052(8) -0.005(5) 0.013(6) C32 0.028(4) 0.017(4) 0.007(3) 0.004(3) 0.002(3) 0.016(3) C33 0.025(4) 0.016(4) 0.013(4) 0.001(3) 0.002(3) 0.011(3) C34 0.020(4) 0.018(4) 0.021(4) 0.005(3) 0.000(3) 0.006(3) C35 0.033(5) 0.021(4) 0.025(5) 0.010(3) 0.010(4) 0.015(4) C36 0.020(4) 0.027(4) 0.016(4) 0.006(3) -0.001(3) 0.012(4) C37 0.017(4) 0.019(4) 0.004(3) -0.002(3) -0.004(3) 0.003(3) C38 0.018(4) 0.022(4) 0.020(4) -0.001(3) -0.002(3) 0.001(3) C39 0.028(5) 0.028(5) 0.043(6) -0.009(4) -0.001(4) 0.007(4) C40 0.024(5) 0.034(5) 0.041(6) 0.009(4) -0.005(4) -0.001(4) C41 0.016(4) 0.018(4) 0.017(4) 0.003(3) -0.004(3) 0.006(3) C42 0.032(5) 0.031(5) 0.013(4) 0.002(3) -0.006(3) 0.014(4) C43 0.022(4) 0.027(5) 0.029(5) 0.003(4) 0.000(4) 0.011(4) O10 0.041(4) 0.027(3) 0.031(4) 0.005(3) 0.014(3) 0.019(3) C44 0.045(6) 0.054(7) 0.023(5) 0.001(4) 0.008(4) 0.027(5) O9 0.024(3) 0.033(4) 0.046(4) 0.012(3) 0.006(3) 0.011(3) C46 0.035(6) 0.035(6) 0.090(10) 0.024(6) 0.023(6) 0.012(5) O11 0.027(3) 0.018(3) 0.030(4) -0.004(2) 0.006(3) 0.008(3) C45 0.056(7) 0.025(5) 0.046(6) 0.002(4) 0.021(5) 0.017(5) O12 0.035(4) 0.027(3) 0.023(3) 0.001(3) 0.000(3) 0.015(3) 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 O6 Cu1 N2 166.0(3) . . O6 Cu1 N3 96.5(2) . . N2 Cu1 N3 78.8(3) . . O6 Cu1 N1 103.0(2) . . N2 Cu1 N1 80.0(3) . . N3 Cu1 N1 158.2(3) . . O6 Cu1 O2 97.6(2) . . N2 Cu1 O2 95.9(2) . . N3 Cu1 O2 93.3(2) . . N1 Cu1 O2 93.8(2) . . O8 Cu2 O8 180.00(14) 2_756 . O8 Cu2 N4 94.0(2) 2_756 2_756 O8 Cu2 N4 86.0(2) . 2_756 O8 Cu2 N4 86.0(2) 2_756 . O8 Cu2 N4 94.0(2) . . N4 Cu2 N4 180.0(3) 2_756 . O3 P1 O2 116.3(3) . . O3 P1 O4 109.9(3) . . O2 P1 O4 109.5(3) . . O3 P1 O1 110.6(3) . . O2 P1 O1 109.8(3) . . O4 P1 O1 99.3(3) . . O7 P2 O8 114.1(3) . . O7 P2 O6 113.6(3) . . O8 P2 O6 110.6(3) . . O7 P2 O5 106.0(3) . . O8 P2 O5 105.9(3) . . O6 P2 O5 105.7(3) . . C32 O1 P1 125.6(5) . . P1 O2 Cu1 128.1(3) . . C21 O5 P2 124.1(5) . . P2 O6 Cu1 131.9(3) . . P2 O8 Cu2 137.3(3) . . C1 N1 C5 118.0(7) . . C1 N1 Cu1 128.6(5) . . C5 N1 Cu1 113.3(5) . . C10 N2 C6 121.6(7) . . C10 N2 Cu1 120.0(5) . . C6 N2 Cu1 118.0(5) . . C11 N3 C15 118.9(7) . . C11 N3 Cu1 115.1(5) . . C15 N3 Cu1 126.0(5) . . C19 N4 C20 117.3(7) . . C19 N4 Cu2 120.0(5) . . C20 N4 Cu2 122.6(5) . . N1 C1 C2 123.0(7) . . N1 C1 H1 118.5 . . C2 C1 H1 118.5 . . C27 C1AA H1AA 109.5 . . C27 C1AA H1AB 109.5 . . H1AA C1AA H1AB 109.5 . . C27 C1AA H1AC 109.5 . . H1AA C1AA H1AC 109.5 . . H1AB C1AA H1AC 109.5 . . C3 C2 C1 119.2(8) . . C3 C2 H2 120.4 . . C1 C2 H2 120.4 . . C2 C3 C4 119.0(7) . . C2 C3 H3 120.5 . . C4 C3 H3 120.5 . . C5 C4 C3 118.0(7) . . C5 C4 H4 121.0 . . C3 C4 H4 121.0 . . N1 C5 C4 122.7(7) . . N1 C5 C6 114.4(6) . . C4 C5 C6 122.9(7) . . N2 C6 C7 120.3(7) . . N2 C6 C5 113.3(7) . . C7 C6 C5 126.3(7) . . C6 C7 C8 119.5(7) . . C6 C7 H7 120.2 . . C8 C7 H7 120.2 . . C7 C8 C9 118.6(7) . . C7 C8 C47 120.6(7) . . C9 C8 C47 120.7(7) . . C10 C9 C8 118.8(7) . . C10 C9 H9 120.6 . . C8 C9 H9 120.6 . . N2 C10 C9 121.0(7) . . N2 C10 C11 111.9(7) . . C9 C10 C11 127.1(7) . . N3 C11 C12 122.5(7) . . N3 C11 C10 113.9(7) . . C12 C11 C10 123.6(7) . . C11 C12 C13 118.1(7) . . C11 C12 H12 120.9 . . C13 C12 H12 120.9 . . C14 C13 C12 118.7(7) . . C14 C13 H13 120.6 . . C12 C13 H13 120.6 . . C15 C14 C13 120.1(7) . . C15 C14 H14 120.0 . . C13 C14 H14 120.0 . . N3 C15 C14 121.6(7) . . N3 C15 H15 119.2 . . C14 C15 H15 119.2 . . C18 C47 C17 116.8(7) . . C18 C47 C8 122.5(7) . . C17 C47 C8 120.7(7) . . C19 C17 C47 119.3(7) 1_665 . C19 C17 H17 120.3 1_665 . C47 C17 H17 120.3 . . C47 C18 C20 119.8(7) . 1_665 C47 C18 H18 120.1 . . C20 C18 H18 120.1 1_665 . N4 C19 C17 123.8(7) . 1_445 N4 C19 H19 118.1 . . C17 C19 H19 118.1 1_445 . N4 C20 C18 122.9(7) . 1_445 N4 C20 H20 118.6 . . C18 C20 H20 118.6 1_445 . C22 C21 O5 119.9(7) . . C22 C21 C26 123.8(7) . . O5 C21 C26 116.1(7) . . C21 C22 C23 116.6(7) . . C21 C22 C29 121.4(7) . . C23 C22 C29 122.0(8) . . C24 C23 C22 120.9(8) . . C24 C23 H23 119.6 . . C22 C23 H23 119.6 . . C23 C24 C25 121.3(8) . . C23 C24 I2 122.7(7) . . C25 C24 I2 116.0(6) . . C26 C25 C24 119.8(8) . . C26 C25 H25 120.1 . . C24 C25 H25 120.1 . . C25 C26 C21 117.2(8) . . C25 C26 C27 121.8(7) . . C21 C26 C27 120.9(7) . . C26 C27 C1AA 109.1(7) . . C26 C27 C28 112.8(7) . . C1AA C27 C28 110.6(7) . . C26 C27 H27 108.0 . . C1AA C27 H27 108.0 . . C28 C27 H27 108.0 . . 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 . . C30 C29 C22 112.4(8) . . C30 C29 C31 111.7(11) . . C22 C29 C31 111.2(7) . . C30 C29 H29 107.1 . . C22 C29 H29 107.1 . . C31 C29 H29 107.1 . . C29 C30 H30A 109.5 . . C29 C30 H30B 109.5 . . H30A C30 H30B 109.5 . . C29 C30 H30C 109.5 . . H30A C30 H30C 109.5 . . H30B C30 H30C 109.5 . . C29 C31 H31A 109.5 . . C29 C31 H31B 109.5 . . H31A C31 H31B 109.5 . . C29 C31 H31C 109.5 . . H31A C31 H31C 109.5 . . H31B C31 H31C 109.5 . . C33 C32 O1 119.1(7) . . C33 C32 C37 122.4(7) . . O1 C32 C37 118.3(7) . . C32 C33 C34 118.4(7) . . C32 C33 C41 122.9(7) . . C34 C33 C41 118.7(7) . . C35 C34 C33 119.0(8) . . C35 C34 H34 120.5 . . C33 C34 H34 120.5 . . C36 C35 C34 122.6(8) . . C36 C35 I1 119.6(6) . . C34 C35 I1 117.8(6) . . C35 C36 C37 119.8(7) . . C35 C36 H36 120.1 . . C37 C36 H36 120.1 . . C36 C37 C32 117.7(7) . . C36 C37 C38 122.5(7) . . C32 C37 C38 119.8(7) . . C37 C38 C39 110.8(7) . . C37 C38 C40 112.5(7) . . C39 C38 C40 109.5(8) . . C37 C38 H38 108.0 . . C39 C38 H38 108.0 . . C40 C38 H38 108.0 . . C38 C39 H39A 109.5 . . C38 C39 H39B 109.5 . . H39A C39 H39B 109.5 . . C38 C39 H39C 109.5 . . H39A C39 H39C 109.5 . . H39B C39 H39C 109.5 . . C38 C40 H40A 109.5 . . C38 C40 H40B 109.5 . . H40A C40 H40B 109.5 . . C38 C40 H40C 109.5 . . H40A C40 H40C 109.5 . . H40B C40 H40C 109.5 . . C42 C41 C33 110.6(7) . . C42 C41 C43 110.6(7) . . C33 C41 C43 110.9(7) . . C42 C41 H41 108.2 . . C33 C41 H41 108.2 . . C43 C41 H41 108.2 . . C41 C42 H42A 109.5 . . C41 C42 H42B 109.5 . . H42A C42 H42B 109.5 . . C41 C42 H42C 109.5 . . H42A C42 H42C 109.5 . . H42B C42 H42C 109.5 . . C41 C43 H43A 109.5 . . C41 C43 H43B 109.5 . . H43A C43 H43B 109.5 . . C41 C43 H43C 109.5 . . H43A C43 H43C 109.5 . . H43B C43 H43C 109.5 . . C44 O10 H10 109.5 . . O10 C44 H44A 109.5 . . O10 C44 H44B 109.5 . . H44A C44 H44B 109.5 . . O10 C44 H44C 109.5 . . H44A C44 H44C 109.5 . . H44B C44 H44C 109.5 . . C46 O9 H9A 109.5 . . O9 C46 H46A 109.5 . . O9 C46 H46B 109.5 . . H46A C46 H46B 109.5 . . O9 C46 H46C 109.5 . . H46A C46 H46C 109.5 . . H46B C46 H46C 109.5 . . C45 O11 H11 109.5 . . O11 C45 H45A 109.5 . . O11 C45 H45B 109.5 . . H45A C45 H45B 109.5 . . O11 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 I1 C35 2.107(8) . I2 C24 2.080(9) . Cu1 O6 1.947(5) . Cu1 N2 1.954(6) . Cu1 N3 2.046(7) . Cu1 N1 2.055(7) . Cu1 O2 2.149(5) . Cu2 O8 1.943(5) 2_756 Cu2 O8 1.943(5) . Cu2 N4 2.037(6) 2_756 Cu2 N4 2.037(6) . P1 O3 1.500(6) . P1 O2 1.508(6) . P1 O4 1.583(6) . P1 O1 1.616(6) . P2 O7 1.509(6) . P2 O8 1.518(5) . P2 O6 1.544(5) . P2 O5 1.621(5) . O1 C32 1.405(9) . O5 C21 1.416(9) . N1 C1 1.324(11) . N1 C5 1.361(10) . N2 C10 1.334(10) . N2 C6 1.341(10) . N3 C11 1.347(10) . N3 C15 1.349(10) . N4 C19 1.332(11) . N4 C20 1.343(10) . C1 C2 1.389(11) . C1 H1 0.9500 . C1AA C27 1.528(12) . C1AA H1AA 0.9800 . C1AA H1AB 0.9800 . C1AA H1AC 0.9800 . C2 C3 1.366(12) . C2 H2 0.9500 . C3 C4 1.409(12) . C3 H3 0.9500 . C4 C5 1.380(11) . C4 H4 0.9500 . C5 C6 1.485(10) . C6 C7 1.392(11) . C7 C8 1.397(11) . C7 H7 0.9500 . C8 C9 1.403(11) . C8 C47 1.493(10) . C9 C10 1.395(11) . C9 H9 0.9500 . C10 C11 1.491(10) . C11 C12 1.397(11) . C12 C13 1.401(11) . C12 H12 0.9500 . C13 C14 1.384(12) . C13 H13 0.9500 . C14 C15 1.384(12) . C14 H14 0.9500 . C15 H15 0.9500 . C47 C18 1.389(11) . C47 C17 1.409(10) . C17 C19 1.380(11) 1_665 C17 H17 0.9500 . C18 C20 1.392(11) 1_665 C18 H18 0.9500 . C19 C17 1.380(11) 1_445 C19 H19 0.9500 . C20 C18 1.392(11) 1_445 C20 H20 0.9500 . C21 C22 1.386(11) . C21 C26 1.425(11) . C22 C23 1.403(12) . C22 C29 1.531(11) . C23 C24 1.377(13) . C23 H23 0.9500 . C24 C25 1.408(12) . C25 C26 1.382(12) . C25 H25 0.9500 . C26 C27 1.523(12) . C27 C28 1.534(12) . C27 H27 1.0000 . C28 H28A 0.9800 . C28 H28B 0.9800 . C28 H28C 0.9800 . C29 C30 1.520(14) . C29 C31 1.539(14) . C29 H29 1.0000 . C30 H30A 0.9800 . C30 H30B 0.9800 . C30 H30C 0.9800 . C31 H31A 0.9800 . C31 H31B 0.9800 . C31 H31C 0.9800 . C32 C33 1.390(12) . C32 C37 1.407(11) . C33 C34 1.406(11) . C33 C41 1.535(11) . C34 C35 1.379(12) . C34 H34 0.9500 . C35 C36 1.374(13) . C36 C37 1.401(12) . C36 H36 0.9500 . C37 C38 1.525(11) . C38 C39 1.538(13) . C38 C40 1.555(13) . C38 H38 1.0000 . C39 H39A 0.9800 . C39 H39B 0.9800 . C39 H39C 0.9800 . C40 H40A 0.9800 . C40 H40B 0.9800 . C40 H40C 0.9800 . C41 C42 1.525(11) . C41 C43 1.545(12) . C41 H41 1.0000 . C42 H42A 0.9800 . C42 H42B 0.9800 . C42 H42C 0.9800 . C43 H43A 0.9800 . C43 H43B 0.9800 . C43 H43C 0.9800 . O10 C44 1.439(12) . O10 H10 0.8400 . C44 H44A 0.9800 . C44 H44B 0.9800 . C44 H44C 0.9800 . O9 C46 1.418(13) . O9 H9A 0.8400 . C46 H46A 0.9800 . C46 H46B 0.9800 . C46 H46C 0.9800 . O11 C45 1.446(11) . O11 H11 0.8400 . C45 H45A 0.9800 . C45 H45B 0.9800 . C45 H45C 0.9800 . O12 H12A 0.8704 . O12 H12B 0.8699 . 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 C1 H1 O7 0.95 2.42 3.323(9) 158.9 . C4 H4 O11 0.95 2.41 3.361(10) 174.2 2_766 C7 H7 O11 0.95 2.65 3.574(10) 164.4 2_766 C9 H9 O10 0.95 2.41 3.342(10) 168.6 1_655 C12 H12 O3 0.95 2.65 3.452(10) 141.9 1_655 C14 H14 I2 0.95 3.18 3.862(8) 130.2 2_755 C18 H18 O10 0.95 2.33 3.268(10) 170.4 1_655 O10 H10 O3 0.84 1.89 2.691(9) 158.4 . O9 H9A O7 0.84 1.95 2.735(9) 154.1 . C46 H46C O7 0.98 2.65 3.157(12) 112.4 . O11 H11 O3 0.84 2.05 2.887(9) 176.1 . O12 H12A O9 0.87 2.14 2.921(10) 149.8 2_656 O12 H12B O7 0.87 1.93 2.758(8) 158.2 . 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_4 O3 P1 O1 C32 32.5(7) . O2 P1 O1 C32 -97.2(6) . O4 P1 O1 C32 148.0(6) . O3 P1 O2 Cu1 143.6(4) . O4 P1 O2 Cu1 18.2(5) . O1 P1 O2 Cu1 -89.8(4) . O7 P2 O5 C21 133.5(6) . O8 P2 O5 C21 -105.0(6) . O6 P2 O5 C21 12.5(6) . O7 P2 O6 Cu1 95.6(5) . O8 P2 O6 Cu1 -34.3(5) . O5 P2 O6 Cu1 -148.6(4) . O7 P2 O8 Cu2 14.3(6) . O6 P2 O8 Cu2 144.0(4) . O5 P2 O8 Cu2 -101.9(5) . C5 N1 C1 C2 -0.1(12) . Cu1 N1 C1 C2 -175.4(6) . N1 C1 C2 C3 0.8(14) . C1 C2 C3 C4 -1.7(14) . C2 C3 C4 C5 1.9(13) . C1 N1 C5 C4 0.2(11) . Cu1 N1 C5 C4 176.3(6) . C1 N1 C5 C6 179.1(7) . Cu1 N1 C5 C6 -4.8(8) . C3 C4 C5 N1 -1.2(12) . C3 C4 C5 C6 -180.0(7) . C10 N2 C6 C7 2.4(11) . Cu1 N2 C6 C7 -170.3(6) . C10 N2 C6 C5 -177.8(7) . Cu1 N2 C6 C5 9.4(9) . N1 C5 C6 N2 -2.6(10) . C4 C5 C6 N2 176.3(7) . N1 C5 C6 C7 177.1(7) . C4 C5 C6 C7 -4.0(12) . N2 C6 C7 C8 -2.9(11) . C5 C6 C7 C8 177.4(7) . C6 C7 C8 C9 1.4(11) . C6 C7 C8 C47 178.7(7) . C7 C8 C9 C10 0.6(11) . C47 C8 C9 C10 -176.7(7) . C6 N2 C10 C9 -0.4(11) . Cu1 N2 C10 C9 172.2(5) . C6 N2 C10 C11 -178.4(7) . Cu1 N2 C10 C11 -5.8(8) . C8 C9 C10 N2 -1.2(11) . C8 C9 C10 C11 176.6(7) . C15 N3 C11 C12 -2.9(11) . Cu1 N3 C11 C12 178.3(6) . C15 N3 C11 C10 173.9(7) . Cu1 N3 C11 C10 -4.9(8) . N2 C10 C11 N3 6.8(9) . C9 C10 C11 N3 -171.1(7) . N2 C10 C11 C12 -176.5(7) . C9 C10 C11 C12 5.6(12) . N3 C11 C12 C13 1.3(12) . C10 C11 C12 C13 -175.1(7) . C11 C12 C13 C14 1.8(12) . C12 C13 C14 C15 -3.3(13) . C11 N3 C15 C14 1.3(12) . Cu1 N3 C15 C14 180.0(6) . C13 C14 C15 N3 1.8(13) . C7 C8 C47 C18 -166.2(8) . C9 C8 C47 C18 11.1(11) . C7 C8 C47 C17 13.1(11) . C9 C8 C47 C17 -169.6(7) . C18 C47 C17 C19 2.8(11) 1_665 C8 C47 C17 C19 -176.5(7) 1_665 C17 C47 C18 C20 -1.9(11) 1_665 C8 C47 C18 C20 177.5(7) 1_665 C20 N4 C19 C17 -1.4(12) 1_445 Cu2 N4 C19 C17 176.6(6) 1_445 C19 N4 C20 C18 2.4(12) 1_445 Cu2 N4 C20 C18 -175.5(6) 1_445 P2 O5 C21 C22 89.1(8) . P2 O5 C21 C26 -94.0(7) . O5 C21 C22 C23 179.6(6) . C26 C21 C22 C23 3.1(11) . O5 C21 C22 C29 0.0(11) . C26 C21 C22 C29 -176.6(7) . C21 C22 C23 C24 2.6(11) . C29 C22 C23 C24 -177.8(8) . C22 C23 C24 C25 -5.7(13) . C22 C23 C24 I2 174.1(6) . C23 C24 C25 C26 3.2(13) . I2 C24 C25 C26 -176.7(6) . C24 C25 C26 C21 2.2(11) . C24 C25 C26 C27 -174.5(7) . C22 C21 C26 C25 -5.5(11) . O5 C21 C26 C25 177.8(6) . C22 C21 C26 C27 171.3(7) . O5 C21 C26 C27 -5.4(10) . C25 C26 C27 C1AA 103.9(9) . C21 C26 C27 C1AA -72.7(9) . C25 C26 C27 C28 -19.5(11) . C21 C26 C27 C28 163.9(7) . C21 C22 C29 C30 115.3(11) . C23 C22 C29 C30 -64.3(13) . C21 C22 C29 C31 -118.6(10) . C23 C22 C29 C31 61.8(12) . P1 O1 C32 C33 89.5(8) . P1 O1 C32 C37 -96.3(8) . O1 C32 C33 C34 177.6(7) . C37 C32 C33 C34 3.6(12) . O1 C32 C33 C41 -1.5(11) . C37 C32 C33 C41 -175.6(7) . C32 C33 C34 C35 -1.1(12) . C41 C33 C34 C35 178.1(7) . C33 C34 C35 C36 -2.4(13) . C33 C34 C35 I1 177.5(6) . C34 C35 C36 C37 3.5(13) . I1 C35 C36 C37 -176.4(6) . C35 C36 C37 C32 -1.0(12) . C35 C36 C37 C38 -178.6(8) . C33 C32 C37 C36 -2.5(12) . O1 C32 C37 C36 -176.6(7) . C33 C32 C37 C38 175.1(7) . O1 C32 C37 C38 1.0(11) . C36 C37 C38 C39 104.6(10) . C32 C37 C38 C39 -72.9(10) . C36 C37 C38 C40 -18.4(12) . C32 C37 C38 C40 164.1(8) . C32 C33 C41 C42 -111.5(9) . C34 C33 C41 C42 69.3(10) . C32 C33 C41 C43 125.3(8) . C34 C33 C41 C43 -53.9(10) .