Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Wenbin Lin' _publ_contact_author_address ; Department of Chemistry University of North Carolina CB #3290,Chapel Hill Chapel Hill NC 27599 UNITED STATES OF AMERICA ; _publ_contact_author_email WLIN@UNC.EDU _publ_section_title ; Homochiral Porous Solids Based on 1D Coordination Polymers Built from 46-Membered Macrocycles ; loop_ _publ_author_name 'Wenbin Lin.' 'Chuan-De Wu.' # Attachment 'new1.cif' data_new1 _database_code_depnum_ccdc_archive 'CCDC 607389' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H90 Cl2 N4 Ni O11' _chemical_formula_weight 1437.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M P3(1)21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'y, x, -z' 'x-y, -y, -z+2/3' '-x, -x+y, -z+1/3' _cell_length_a 18.6823(8) _cell_length_b 18.6823(8) _cell_length_c 25.475(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 7700.1(8) _cell_formula_units_Z 3 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 20.49 _exptl_crystal_description Bloc _exptl_crystal_colour 'light green' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.930 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2280 _exptl_absorpt_coefficient_mu 0.287 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.6236 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 22247 _diffrn_reflns_av_R_equivalents 0.1377 _diffrn_reflns_av_sigmaI/netI 0.1156 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 20.49 _reflns_number_total 4999 _reflns_number_gt 2853 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1443P)^2^+10.5863P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0017(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.06(6) _refine_ls_number_reflns 4999 _refine_ls_number_parameters 402 _refine_ls_number_restraints 10 _refine_ls_R_factor_ref 0.1749 _refine_ls_R_factor_gt 0.1121 _refine_ls_wR_factor_ref 0.2933 _refine_ls_wR_factor_gt 0.2633 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 1.0000 2.02454(11) 2.1667 0.0693(8) Uani 1 2 d S . . Cl Cl 0.8690(2) 1.9631(2) 2.11848(11) 0.0930(12) Uani 1 1 d . . . O1 O 1.2867(13) 2.6367(12) 1.7526(5) 0.231(8) Uani 1 1 d . . . O2 O 1.4441(12) 2.7743(10) 1.8154(8) 0.243(8) Uani 1 1 d . . . N1 N 1.0453(9) 2.9666(8) 2.1153(3) 0.095(4) Uani 1 1 d . . . N2 N 1.0482(8) 2.1267(7) 2.1154(4) 0.077(3) Uani 1 1 d . . . C1 C 1.0232(9) 2.9530(8) 2.0633(4) 0.098(5) Uani 1 1 d . . . H1A H 0.9862 2.9699 2.0506 0.117 Uiso 1 1 calc R . . C2 C 1.0503(11) 2.9178(9) 2.0298(4) 0.112(6) Uani 1 1 d . . . H2A H 1.0329 2.9104 1.9942 0.134 Uiso 1 1 calc R . . C3 C 1.1061(13) 2.8906(10) 2.0475(5) 0.116(6) Uani 1 1 d . . . C4 C 1.1270(13) 2.9019(11) 2.1005(5) 0.124(6) Uani 1 1 d . . . H4A H 1.1640 2.8858 2.1145 0.149 Uiso 1 1 calc R . . C5 C 1.0943(12) 2.9355(11) 2.1311(5) 0.108(5) Uani 1 1 d . . . H5A H 1.1061 2.9383 2.1676 0.130 Uiso 1 1 calc R . . C6 C 1.1368(13) 2.8465(10) 2.0142(5) 0.144(8) Uani 1 1 d . . . H6A H 1.1769 2.8351 2.0285 0.172 Uiso 1 1 calc R . . C7 C 1.1108(12) 2.8217(10) 1.9642(5) 0.123(6) Uani 1 1 d . . . H7A H 1.0656 2.8260 1.9509 0.148 Uiso 1 1 calc R . . C8 C 1.1503(19) 2.7886(13) 1.9303(6) 0.172(10) Uani 1 1 d . . . C9 C 1.2189(18) 2.7748(10) 1.9491(7) 0.177(12) Uani 1 1 d . . . H9A H 1.2408 2.7926 1.9833 0.213 Uiso 1 1 calc R . . C10 C 1.2514(16) 2.7365(11) 1.9175(8) 0.182(11) Uani 1 1 d . . . H10A H 1.2888 2.7222 1.9330 0.219 Uiso 1 1 calc R . . C13 C 1.126(3) 2.7705(18) 1.8789(6) 0.28(2) Uani 1 1 d . . . H13A H 1.0812 2.7748 1.8647 0.340 Uiso 1 1 calc R . . C11 C 1.1780(17) 2.7422(16) 1.8456(5) 0.35(3) Uani 1 1 d G . . C12 C 1.2322(12) 2.7187(10) 1.8658(3) 0.215(14) Uani 1 1 d G . . C14 C 1.2648(12) 2.6823(11) 1.8333(4) 0.231(13) Uani 1 1 d GD . . C15 C 1.2431(16) 2.6695(13) 1.7805(4) 0.41(3) Uani 1 1 d G . . C16 C 1.1888(17) 2.6931(16) 1.7603(4) 0.270(19) Uani 1 1 d G . . H16A H 1.1740 2.6843 1.7242 0.324 Uiso 1 1 calc R . . C17 C 1.1563(17) 2.7294(18) 1.7928(5) 0.65(7) Uani 1 1 d G . . H17A H 1.1192 2.7455 1.7790 0.785 Uiso 1 1 calc R . . C18 C 1.2801(17) 2.6323(16) 1.6974(6) 0.198(10) Uani 1 1 d . . . H18A H 1.2214 2.6079 1.6871 0.237 Uiso 1 1 calc R . . H18B H 1.3111 2.6887 1.6824 0.237 Uiso 1 1 calc R . . C19 C 1.3118(19) 2.5838(16) 1.6772(7) 0.231(13) Uani 1 1 d . . . H19A H 1.3050 2.5798 1.6390 0.347 Uiso 1 1 calc R . . H19B H 1.2819 2.5284 1.6926 0.347 Uiso 1 1 calc R . . H19C H 1.3706 2.6094 1.6859 0.347 Uiso 1 1 calc R . . C20 C 1.517(4) 2.866(2) 1.7479(15) 0.52(5) Uani 1 1 d D . . H20A H 1.5622 2.8825 1.7224 0.774 Uiso 1 1 calc R . . H20B H 1.5305 2.9118 1.7719 0.774 Uiso 1 1 calc R . . H20C H 1.4657 2.8506 1.7293 0.774 Uiso 1 1 calc R . . C21 C 1.507(2) 2.7924(18) 1.7789(12) 0.48(5) Uani 1 1 d D . . H21A H 1.4920 2.7445 1.7555 0.580 Uiso 1 1 calc R . . H21B H 1.5595 2.8061 1.7971 0.580 Uiso 1 1 calc R . . C22 C 1.3228(12) 2.6512(10) 1.8545(6) 0.251(12) Uiso 1 1 d GD . . C23 C 1.4074(12) 2.6948(9) 1.8450(6) 0.204(9) Uiso 1 1 d G . . C24 C 1.4579(9) 2.6670(14) 1.8659(8) 0.270(15) Uiso 1 1 d G . . H24A H 1.5158 2.6968 1.8594 0.324 Uiso 1 1 calc R . . C25 C 1.4239(14) 2.5957(14) 1.8963(8) 0.263(15) Uiso 1 1 d G . . H25A H 1.4584 2.5768 1.9106 0.316 Uiso 1 1 calc R . . C26 C 1.3393(15) 2.5522(9) 1.9058(5) 0.226(16) Uani 1 1 d G . . C27 C 1.2888(10) 2.5799(9) 1.8849(6) 0.228(17) Uani 1 1 d G . . C28 C 1.315(2) 2.4883(15) 1.9326(7) 0.183(12) Uani 1 1 d . . . H28A H 1.3512 2.4684 1.9413 0.219 Uiso 1 1 calc R . . C29 C 1.237(2) 2.4486(11) 1.9487(6) 0.123(7) Uani 1 1 d . . . C30 C 1.1774(16) 2.4678(13) 1.9326(7) 0.139(7) Uani 1 1 d . . . H30A H 1.1220 2.4378 1.9449 0.167 Uiso 1 1 calc R . . C31 C 1.202(2) 2.5309(14) 1.8989(7) 0.210(14) Uani 1 1 d . . . H31A H 1.1630 2.5435 1.8842 0.251 Uiso 1 1 calc R . . C32 C 1.2017(14) 2.3714(10) 1.9869(6) 0.121(6) Uani 1 1 d . . . H32A H 1.2433 2.3588 1.9965 0.145 Uiso 1 1 calc R . . C33 C 1.1386(13) 2.3262(10) 2.0063(6) 0.122(7) Uani 1 1 d . . . H33A H 1.0965 2.3362 1.9938 0.147 Uiso 1 1 calc R . . C34 C 1.0023(10) 2.1592(9) 2.1026(5) 0.083(4) Uani 1 1 d . . . H34A H 0.9497 2.1390 2.1185 0.100 Uiso 1 1 calc R . . C35 C 1.0296(13) 2.2221(11) 2.0663(7) 0.109(5) Uani 1 1 d . . . H35A H 0.9927 2.2408 2.0563 0.130 Uiso 1 1 calc R . . C36 C 1.1051(14) 2.2591(10) 2.0439(6) 0.100(5) Uani 1 1 d . . . C37 C 1.1554(12) 2.2252(11) 2.0585(5) 0.116(6) Uani 1 1 d . . . H37A H 1.2093 2.2473 2.0441 0.140 Uiso 1 1 calc R . . C38 C 1.1247(9) 2.1569(9) 2.0955(5) 0.087(4) Uani 1 1 d . . . H38A H 1.1580 2.1339 2.1054 0.105 Uiso 1 1 calc R . . O3 O 1.036(4) 2.545(3) 1.370(2) 0.33(2) Uiso 0.50 1 d PD . . C39 C 1.052(3) 2.500(3) 1.3945(18) 0.174(16) Uiso 0.50 1 d PD . . C40 C 1.0958(19) 2.4519(19) 1.4042(11) 0.111(10) Uiso 0.50 1 d PD . . O4 O 1.127(3) 2.353(3) 1.8141(18) 0.28(2) Uiso 0.50 1 d PD . . H4B H 1.1703 2.3494 1.8143 0.427 Uiso 0.50 1 calc PR . . C41 C 1.074(3) 2.429(3) 1.7776(19) 0.21(2) Uiso 0.50 1 d PD . . H41A H 1.0945 2.4770 1.7544 0.309 Uiso 0.50 1 calc PR . . H41B H 1.0599 2.4426 1.8119 0.309 Uiso 0.50 1 calc PR . . H41C H 1.0248 2.3823 1.7621 0.309 Uiso 0.50 1 calc PR . . C42 C 1.136(4) 2.407(5) 1.784(4) 0.39(6) Uiso 0.50 1 d PD . . H42A H 1.1472 2.3925 1.7491 0.467 Uiso 0.50 1 calc PR . . H42B H 1.1869 2.4582 1.7952 0.467 Uiso 0.50 1 calc PR . . C44 C 1.742(3) 2.844(3) 1.982(2) 0.22(2) Uiso 0.50 1 d PD . . H44A H 1.7613 2.8181 2.0073 0.326 Uiso 0.50 1 calc PR . . H44B H 1.6927 2.8434 1.9953 0.326 Uiso 0.50 1 calc PR . . H44C H 1.7859 2.9016 1.9760 0.326 Uiso 0.50 1 calc PR . . O101 O 1.0033(16) 2.6184(16) 1.7022(10) 0.157(9) Uiso 0.50 1 d P . . O102 O 1.035(7) 2.468(6) 1.682(5) 0.53(6) Uiso 0.50 1 d P . . O103 O 1.408(4) 3.006(4) 1.7389(19) 0.39(3) Uiso 0.50 1 d PD . . O104 O 1.336(3) 2.936(3) 1.8302(15) 0.260(16) Uiso 0.50 1 d PD . . C43 C 1.722(4) 2.798(4) 1.931(2) 0.22(2) Uiso 0.50 1 d PD . . H43A H 1.7734 2.8030 1.9162 0.270 Uiso 0.50 1 calc PR . . H43B H 1.6831 2.7390 1.9378 0.270 Uiso 0.50 1 calc PR . . O5 O 1.692(3) 2.824(4) 1.899(2) 0.32(2) Uiso 0.50 1 d PD . . H5B H 1.6807 2.7966 1.8717 0.486 Uiso 0.50 1 calc PR . . 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 Ni1 0.0871(17) 0.0775(11) 0.0464(11) -0.0024(5) -0.0048(11) 0.0435(8) Cl 0.091(2) 0.100(3) 0.0578(18) 0.011(2) -0.0071(16) 0.025(2) O1 0.40(2) 0.297(19) 0.119(9) 0.012(11) 0.033(12) 0.269(19) O2 0.221(17) 0.146(12) 0.32(2) 0.058(14) 0.097(17) 0.057(12) N1 0.159(12) 0.113(9) 0.044(6) 0.011(6) -0.005(7) 0.090(8) N2 0.079(10) 0.097(8) 0.065(7) -0.009(5) -0.013(7) 0.052(9) C1 0.160(15) 0.112(11) 0.039(7) 0.000(7) -0.004(8) 0.080(11) C2 0.23(2) 0.109(12) 0.044(7) 0.014(8) 0.011(9) 0.121(14) C3 0.23(2) 0.095(12) 0.049(9) 0.018(8) 0.022(10) 0.100(14) C4 0.23(2) 0.138(14) 0.067(10) -0.010(10) 0.025(11) 0.140(14) C5 0.176(16) 0.123(13) 0.056(8) 0.019(10) -0.009(10) 0.098(12) C6 0.32(3) 0.115(13) 0.070(10) 0.028(10) 0.052(13) 0.164(18) C7 0.26(2) 0.133(13) 0.034(7) -0.011(8) -0.001(9) 0.138(14) C8 0.39(3) 0.152(17) 0.065(12) 0.036(11) 0.033(15) 0.20(2) C9 0.39(4) 0.094(13) 0.096(12) 0.041(10) 0.133(18) 0.156(19) C10 0.33(3) 0.134(16) 0.132(14) 0.093(13) 0.142(18) 0.15(2) C13 0.72(7) 0.31(3) 0.052(11) 0.001(14) -0.004(19) 0.43(4) C11 0.87(9) 0.42(5) 0.034(10) -0.002(17) -0.01(2) 0.54(6) C12 0.51(5) 0.186(19) 0.062(11) 0.081(12) 0.103(18) 0.26(3) C14 0.44(4) 0.27(3) 0.060(10) 0.070(14) 0.139(17) 0.24(3) C15 1.13(11) 0.41(4) 0.062(12) 0.009(17) 0.01(3) 0.66(7) C16 0.63(6) 0.33(3) 0.077(12) 0.007(16) 0.02(2) 0.41(4) C17 1.5(2) 1.11(14) 0.068(15) 0.08(4) 0.07(4) 1.24(16) C18 0.32(3) 0.23(2) 0.058(10) -0.013(12) 0.004(12) 0.16(2) C19 0.41(4) 0.24(2) 0.146(16) -0.064(16) 0.02(2) 0.23(3) C20 0.92(11) 0.23(3) 0.40(5) 0.26(4) 0.52(7) 0.29(5) C21 0.33(4) 0.39(6) 0.24(3) -0.04(4) 0.18(3) -0.20(4) C26 0.44(5) 0.097(16) 0.21(2) 0.102(17) 0.18(3) 0.19(2) C27 0.52(5) 0.087(13) 0.091(12) 0.082(10) 0.16(2) 0.16(2) C28 0.32(3) 0.108(17) 0.094(14) 0.027(12) 0.107(18) 0.083(19) C29 0.22(3) 0.082(12) 0.062(10) 0.006(9) 0.003(14) 0.076(16) C30 0.19(2) 0.113(17) 0.079(13) 0.001(11) -0.011(13) 0.046(15) C31 0.47(5) 0.108(17) 0.070(13) 0.034(11) 0.036(18) 0.16(2) C32 0.165(19) 0.083(12) 0.109(12) 0.011(10) 0.004(13) 0.058(13) C33 0.140(16) 0.069(11) 0.091(11) 0.018(9) 0.023(11) 0.003(11) C34 0.081(11) 0.069(10) 0.069(9) 0.008(8) 0.018(8) 0.015(9) C35 0.085(13) 0.088(13) 0.139(14) 0.017(11) -0.024(11) 0.033(10) C36 0.112(16) 0.091(12) 0.072(10) -0.012(9) -0.029(11) 0.033(13) C37 0.124(15) 0.130(16) 0.048(9) -0.011(9) 0.007(9) 0.029(13) C38 0.067(10) 0.131(13) 0.057(8) 0.011(8) 0.035(7) 0.044(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Ni1 N2 2.107(11) 6_769 ? Ni1 N2 2.107(11) . ? Ni1 N1 2.126(10) 6_759 ? Ni1 N1 2.126(10) 1_545 ? Ni1 Cl 2.450(3) 6_769 ? Ni1 Cl 2.450(3) . ? O1 C18 1.409(16) . ? O1 C15 1.429(17) . ? O2 C21 1.41(3) . ? O2 C23 1.49(2) . ? N1 C5 1.367(16) . ? N1 C1 1.371(13) . ? N1 Ni1 2.126(10) 1_565 ? N2 C34 1.317(17) . ? N2 C38 1.346(15) . ? C1 C2 1.322(16) . ? C2 C3 1.44(2) . ? C3 C4 1.393(19) . ? C3 C6 1.483(19) . ? C4 C5 1.327(17) . ? C6 C7 1.359(18) . ? C7 C8 1.46(2) . ? C8 C13 1.37(2) . ? C8 C9 1.50(3) . ? C9 C10 1.40(2) . ? C10 C12 1.36(2) . ? C13 C11 1.57(2) . ? C11 C12 1.3900 . ? C11 C17 1.3900 . ? C12 C14 1.3900 . ? C14 C15 1.3900 . ? C14 C22 1.561(15) . ? C15 C16 1.3900 . ? C16 C17 1.3900 . ? C18 C19 1.40(3) . ? C20 C21 1.51(2) . ? C22 C23 1.3900 . ? C22 C27 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C26 C28 1.25(2) . ? C26 C27 1.3900 . ? C27 C31 1.45(4) . ? C28 C29 1.33(3) . ? C29 C30 1.39(3) . ? C29 C32 1.58(2) . ? C30 C31 1.34(2) . ? C32 C33 1.16(2) . ? C33 C36 1.45(2) . ? C34 C35 1.38(2) . ? C35 C36 1.35(2) . ? C36 C37 1.42(2) . ? C37 C38 1.45(2) . ? O3 C39 1.21(2) . ? C39 C40 1.50(2) . ? O4 C42 1.21(2) . ? C41 C42 1.41(2) . ? C44 C43 1.49(2) . ? O101 O101 1.81(5) 6_768 ? O102 O102 1.4(2) 6_768 ? C43 O5 1.22(2) . ? 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 N2 Ni1 N2 92.4(7) 6_769 . ? N2 Ni1 N1 88.9(4) 6_769 6_759 ? N2 Ni1 N1 178.2(6) . 6_759 ? N2 Ni1 N1 178.2(6) 6_769 1_545 ? N2 Ni1 N1 88.9(4) . 1_545 ? N1 Ni1 N1 89.8(6) 6_759 1_545 ? N2 Ni1 Cl 89.3(4) 6_769 6_769 ? N2 Ni1 Cl 88.2(4) . 6_769 ? N1 Ni1 Cl 90.7(4) 6_759 6_769 ? N1 Ni1 Cl 91.9(4) 1_545 6_769 ? N2 Ni1 Cl 88.2(3) 6_769 . ? N2 Ni1 Cl 89.3(3) . . ? N1 Ni1 Cl 91.9(4) 6_759 . ? N1 Ni1 Cl 90.7(4) 1_545 . ? Cl Ni1 Cl 176.4(2) 6_769 . ? C18 O1 C15 118.0(16) . . ? C21 O2 C23 119(2) . . ? C5 N1 C1 114.2(11) . . ? C5 N1 Ni1 123.8(8) . 1_565 ? C1 N1 Ni1 121.9(9) . 1_565 ? C34 N2 C38 120.9(11) . . ? C34 N2 Ni1 119.3(10) . . ? C38 N2 Ni1 119.8(11) . . ? C2 C1 N1 124.1(14) . . ? C1 C2 C3 119.8(12) . . ? C4 C3 C2 116.6(13) . . ? C4 C3 C6 118.8(15) . . ? C2 C3 C6 124.4(13) . . ? C5 C4 C3 118.8(15) . . ? C4 C5 N1 126.3(12) . . ? C7 C6 C3 123.7(16) . . ? C6 C7 C8 121.9(16) . . ? C13 C8 C7 119(2) . . ? C13 C8 C9 118(2) . . ? C7 C8 C9 122.6(15) . . ? C10 C9 C8 122(2) . . ? C12 C10 C9 124(2) . . ? C8 C13 C11 114(2) . . ? C12 C11 C17 120.0 . . ? C12 C11 C13 125.4(12) . . ? C17 C11 C13 113.9(13) . . ? C10 C12 C14 124.8(13) . . ? C10 C12 C11 115.1(13) . . ? C14 C12 C11 120.0 . . ? C12 C14 C15 120.0 . . ? C12 C14 C22 122.0(10) . . ? C15 C14 C22 117.9(11) . . ? C16 C15 C14 120.0 . . ? C16 C15 O1 127.8(11) . . ? C14 C15 O1 112.0(12) . . ? C15 C16 C17 120.0 . . ? C16 C17 C11 120.0 . . ? C19 C18 O1 110.6(19) . . ? O2 C21 C20 106(2) . . ? C23 C22 C27 120.0 . . ? C23 C22 C14 121.3(14) . . ? C27 C22 C14 118.6(14) . . ? C24 C23 C22 120.0 . . ? C24 C23 O2 120.3(16) . . ? C22 C23 O2 119.5(16) . . ? C23 C24 C25 120.00(5) . . ? C26 C25 C24 120.0 . . ? C28 C26 C27 125(2) . . ? C28 C26 C25 115(2) . . ? C27 C26 C25 120.0 . . ? C26 C27 C22 120.00(5) . . ? C26 C27 C31 114.9(15) . . ? C22 C27 C31 125.1(15) . . ? C26 C28 C29 119(3) . . ? C28 C29 C30 124(2) . . ? C28 C29 C32 123(2) . . ? C30 C29 C32 113(2) . . ? C31 C30 C29 117(2) . . ? C30 C31 C27 120(3) . . ? C33 C32 C29 137(2) . . ? C32 C33 C36 139(2) . . ? N2 C34 C35 120.7(15) . . ? C36 C35 C34 124.6(16) . . ? C35 C36 C37 114.6(15) . . ? C35 C36 C33 128(2) . . ? C37 C36 C33 118(2) . . ? C36 C37 C38 120.2(16) . . ? N2 C38 C37 118.8(14) . . ? O3 C39 C40 155(5) . . ? O4 C42 C41 122(3) . . ? O5 C43 C44 112(6) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 20.49 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.494 _refine_diff_density_min -0.301 _refine_diff_density_rms 0.079 # Attachment 'new2.cif' data_new2 _database_code_depnum_ccdc_archive 'CCDC 607390' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C171 H189 Cl4 Cu2 N9 O36' _chemical_formula_weight 3215.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M C222(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 18.6113(8) _cell_length_b 32.2357(8) _cell_length_c 38.176(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 22903.8(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 20.50 _exptl_crystal_description Bloc _exptl_crystal_colour Brown _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.932 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6768 _exptl_absorpt_coefficient_mu 0.288 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.3420 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 37513 _diffrn_reflns_av_R_equivalents 0.1858 _diffrn_reflns_av_sigmaI/netI 0.1320 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 20.50 _reflns_number_total 11403 _reflns_number_gt 6633 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+197.5582P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(4) _refine_ls_number_reflns 11403 _refine_ls_number_parameters 990 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.2149 _refine_ls_R_factor_gt 0.1435 _refine_ls_wR_factor_ref 0.3087 _refine_ls_wR_factor_gt 0.2780 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 1.0000 -0.28477(12) 0.7500 0.1022(12) Uani 1 2 d S . . Cu2 Cu 1.36369(14) 0.5000 -0.5000 0.1066(11) Uani 1 2 d S . . O1 O 0.4800(4) -0.2078(5) 0.4571(2) 0.121(5) Uani 1 1 d . . . O2 O 0.5174(4) -0.2979(4) 0.4488(3) 0.115(5) Uani 1 1 d . . . O3 O 1.0000 -0.3561(7) 0.7500 0.139(7) Uani 1 2 d S . . O4 O 0.8394(7) 0.2412(6) -0.2972(4) 0.137(5) Uani 1 1 d . . . O5 O 0.8861(8) 0.3036(5) -0.2517(3) 0.158(6) Uani 1 1 d . . . N1 N 0.9226(7) -0.2823(6) 0.7126(3) 0.098(4) Uani 1 1 d . . . N2 N 0.0721(7) -0.2811(6) 0.7106(3) 0.097(4) Uani 1 1 d . . . N3 N 1.2913(7) 0.4746(4) -0.4704(4) 0.102(5) Uani 1 1 d . . . N4 N 0.4372(8) 0.4750(5) -0.4692(5) 0.128(6) Uani 1 1 d . . . C1 C 0.9172(10) -0.2496(6) 0.6910(5) 0.107(6) Uiso 1 1 d . . . H1A H 0.9502 -0.2271 0.6921 0.128 Uiso 1 1 calc R . . C2 C 0.8582(10) -0.2501(8) 0.6658(4) 0.112(7) Uani 1 1 d . . . H2A H 0.8529 -0.2282 0.6493 0.135 Uiso 1 1 calc R . . C3 C 0.8113(9) -0.2822(9) 0.6661(5) 0.114(8) Uani 1 1 d . . . C4 C 0.8170(12) -0.3130(8) 0.6886(5) 0.137(9) Uani 1 1 d . . . H4A H 0.7813 -0.3341 0.6886 0.164 Uiso 1 1 calc R . . C5 C 0.8714(10) -0.3157(8) 0.7115(3) 0.135(9) Uani 1 1 d . . . H5A H 0.8761 -0.3391 0.7265 0.162 Uiso 1 1 calc R . . C6 C 0.7542(9) -0.2819(9) 0.6339(6) 0.134(8) Uani 1 1 d . . . H6A H 0.7229 -0.3050 0.6316 0.161 Uiso 1 1 calc R . . C7 C 0.7486(9) -0.2519(8) 0.6109(5) 0.117(8) Uani 1 1 d . . . H7A H 0.7820 -0.2296 0.6124 0.141 Uiso 1 1 calc R . . C8 C 0.6920(8) -0.2502(8) 0.5820(6) 0.112(7) Uani 1 1 d . . . C9 C 0.6950(9) -0.2211(8) 0.5579(5) 0.130(8) Uani 1 1 d . . . H9A H 0.7340 -0.2022 0.5573 0.156 Uiso 1 1 calc R . . C10 C 0.6414(8) -0.2186(8) 0.5341(5) 0.105(6) Uani 1 1 d . . . C11 C 0.6456(9) -0.1839(8) 0.5098(5) 0.129(8) Uani 1 1 d . . . H11A H 0.6833 -0.1642 0.5114 0.154 Uiso 1 1 calc R . . C12 C 0.5919(9) -0.1806(7) 0.4838(4) 0.116(7) Uani 1 1 d . . . H12A H 0.5921 -0.1576 0.4682 0.139 Uiso 1 1 calc R . . C13 C 0.5331(10) -0.2139(7) 0.4804(5) 0.110(6) Uiso 1 1 d . . . C14 C 0.5297(7) -0.2447(7) 0.5024(4) 0.099(5) Uani 1 1 d . . . C15 C 0.5863(8) -0.2475(7) 0.5309(5) 0.097(6) Uani 1 1 d . . . C16 C 0.5850(8) -0.2834(8) 0.5555(4) 0.113(7) Uani 1 1 d . . . H16A H 0.5492 -0.3043 0.5541 0.136 Uiso 1 1 calc R . . C17 C 0.6378(9) -0.2844(7) 0.5801(4) 0.124(7) Uani 1 1 d . . . H17A H 0.6403 -0.3069 0.5961 0.148 Uiso 1 1 calc R . . C18 C 0.4964(14) -0.1790(9) 0.4271(4) 0.202(13) Uani 1 1 d . . . H18A H 0.5438 -0.1850 0.4165 0.243 Uiso 1 1 calc R . . H18B H 0.4942 -0.1495 0.4343 0.243 Uiso 1 1 calc R . . C19 C 0.4301(10) -0.1916(8) 0.4010(4) 0.164(10) Uani 1 1 d . . . H19A H 0.4318 -0.1742 0.3800 0.247 Uiso 1 1 calc R . . H19B H 0.3843 -0.1873 0.4131 0.247 Uiso 1 1 calc R . . H19C H 0.4346 -0.2208 0.3943 0.247 Uiso 1 1 calc R . . C20 C 0.5594(10) -0.2914(8) 0.3901(4) 0.154(9) Uani 1 1 d . . . H20A H 0.5510 -0.2995 0.3657 0.232 Uiso 1 1 calc R . . H20B H 0.6073 -0.3006 0.3974 0.232 Uiso 1 1 calc R . . H20C H 0.5564 -0.2611 0.3921 0.232 Uiso 1 1 calc R . . C21 C 0.5000(10) -0.3123(7) 0.4148(5) 0.133(7) Uani 1 1 d . . . H21A H 0.4511 -0.3035 0.4079 0.160 Uiso 1 1 calc R . . H21B H 0.5029 -0.3430 0.4136 0.160 Uiso 1 1 calc R . . C22 C 0.4677(8) -0.2748(5) 0.5031(4) 0.085(5) Uani 1 1 d . . . C23 C 0.4133(7) -0.2775(6) 0.5285(4) 0.083(5) Uani 1 1 d . . . C24 C 0.4129(9) -0.2505(7) 0.5601(4) 0.117(7) Uani 1 1 d . . . H24A H 0.4501 -0.2309 0.5641 0.140 Uiso 1 1 calc R . . C25 C 0.3600(9) -0.2547(6) 0.5822(4) 0.102(6) Uani 1 1 d . . . H25A H 0.3611 -0.2375 0.6024 0.122 Uiso 1 1 calc R . . C26 C 0.3032(9) -0.2810(8) 0.5792(4) 0.111(7) Uani 1 1 d . . . C27 C 0.3029(7) -0.3067(7) 0.5522(5) 0.106(7) Uani 1 1 d . . . H27A H 0.2657 -0.3268 0.5506 0.127 Uiso 1 1 calc R . . C28 C 0.3585(8) -0.3053(7) 0.5242(4) 0.097(6) Uani 1 1 d . . . C29 C 0.3534(7) -0.3320(6) 0.4959(4) 0.102(6) Uani 1 1 d . . . H29A H 0.3152 -0.3515 0.4946 0.122 Uiso 1 1 calc R . . C30 C 0.4070(8) -0.3302(7) 0.4681(4) 0.124(8) Uani 1 1 d . . . H30A H 0.4055 -0.3476 0.4480 0.149 Uiso 1 1 calc R . . C31 C 0.4608(8) -0.3005(8) 0.4737(4) 0.120(8) Uani 1 1 d . . . C32 C 0.2430(9) -0.2875(7) 0.6047(4) 0.113(7) Uani 1 1 d . . . H32A H 0.2090 -0.3089 0.6003 0.136 Uiso 1 1 calc R . . C33 C 0.2361(9) -0.2654(9) 0.6318(6) 0.155(10) Uani 1 1 d D . . H33A H 0.2684 -0.2431 0.6359 0.186 Uiso 1 1 calc R . . C34 C 0.0776(9) -0.3098(5) 0.6840(4) 0.091(5) Uiso 1 1 d . . . H34A H 0.0463 -0.3331 0.6844 0.109 Uiso 1 1 calc R . . C35 C 0.1263(9) -0.3067(7) 0.6567(4) 0.105(6) Uani 1 1 d . . . H35A H 0.1262 -0.3257 0.6378 0.126 Uiso 1 1 calc R . . C36 C 0.1747(9) -0.2745(8) 0.6585(4) 0.114(7) Uani 1 1 d D . . C37 C 0.1691(10) -0.2443(6) 0.6860(5) 0.114(6) Uiso 1 1 d . . . H37A H 0.2004 -0.2210 0.6861 0.137 Uiso 1 1 calc R . . C38 C 0.1193(9) -0.2486(7) 0.7122(4) 0.122(7) Uani 1 1 d . . . H38A H 0.1176 -0.2293 0.7310 0.146 Uiso 1 1 calc R . . C39 C 1.2391(11) 0.4949(8) -0.4574(6) 0.150(9) Uani 1 1 d D . . H39A H 1.2354 0.5239 -0.4618 0.180 Uiso 1 1 calc R . . C40 C 1.1820(11) 0.4734(10) -0.4345(4) 0.148(9) Uani 1 1 d D . . H40A H 1.1458 0.4903 -0.4243 0.178 Uiso 1 1 calc R . . C41 C 1.1796(18) 0.4344(7) -0.4283(9) 0.177(15) Uani 1 1 d . . . C42 C 1.2434(13) 0.4113(7) -0.4428(9) 0.205(15) Uani 1 1 d . . . H42A H 1.2508 0.3827 -0.4380 0.247 Uiso 1 1 calc R . . C43 C 1.2896(9) 0.4330(6) -0.4628(5) 0.125(8) Uani 1 1 d . . . H43A H 1.3267 0.4171 -0.4734 0.150 Uiso 1 1 calc R . . C44 C 1.1235(9) 0.4156(7) -0.4085(5) 0.102(6) Uani 1 1 d . . . H44A H 1.0904 0.4345 -0.3983 0.123 Uiso 1 1 calc R . . C45 C 1.1114(10) 0.3806(7) -0.4027(4) 0.100(6) Uani 1 1 d . . . H45A H 1.1429 0.3622 -0.4147 0.120 Uiso 1 1 calc R . . C46 C 1.0582(10) 0.3588(10) -0.3809(5) 0.116(8) Uani 1 1 d . . . C47 C 1.0516(10) 0.3140(10) -0.3781(5) 0.129(9) Uani 1 1 d . . . H47A H 1.0850 0.2968 -0.3902 0.155 Uiso 1 1 calc R . . C48 C 0.9995(10) 0.2961(7) -0.3589(4) 0.092(5) Uani 1 1 d . . . C49 C 0.9964(11) 0.2509(7) -0.3541(4) 0.099(5) Uani 1 1 d . . . H49A H 1.0323 0.2345 -0.3652 0.118 Uiso 1 1 calc R . . C50 C 0.9458(12) 0.2311(8) -0.3351(4) 0.121(8) Uani 1 1 d . . . H50A H 0.9457 0.2017 -0.3334 0.145 Uiso 1 1 calc R . . C51 C 0.8921(12) 0.2552(11) -0.3173(5) 0.124(9) Uani 1 1 d . . . C52 C 0.8957(10) 0.2970(10) -0.3213(5) 0.112(8) Uani 1 1 d . . . C53 C 0.9466(9) 0.3229(8) -0.3404(4) 0.094(6) Uani 1 1 d . . . C54 C 0.9532(10) 0.3656(7) -0.3442(4) 0.098(6) Uani 1 1 d . . . H54A H 0.9199 0.3834 -0.3327 0.117 Uiso 1 1 calc R . . C55 C 1.0081(11) 0.3830(8) -0.3647(4) 0.129(7) Uani 1 1 d . . . H55A H 1.0103 0.4123 -0.3674 0.154 Uiso 1 1 calc R . . C56 C 0.8444(12) 0.1987(9) -0.2916(6) 0.175(11) Uani 1 1 d . . . H56A H 0.8906 0.1923 -0.2799 0.210 Uiso 1 1 calc R . . H56B H 0.8437 0.1841 -0.3144 0.210 Uiso 1 1 calc R . . C57 C 0.7837(11) 0.1836(8) -0.2694(6) 0.178(10) Uani 1 1 d . . . H57A H 0.7902 0.1540 -0.2644 0.266 Uiso 1 1 calc R . . H57B H 0.7382 0.1878 -0.2819 0.266 Uiso 1 1 calc R . . H57C H 0.7829 0.1992 -0.2473 0.266 Uiso 1 1 calc R . . C58 C 0.8372(14) 0.2711(10) -0.1961(6) 0.220(18) Uani 1 1 d . . . H58A H 0.8386 0.2726 -0.1705 0.331 Uiso 1 1 calc R . . H58B H 0.8502 0.2431 -0.2038 0.331 Uiso 1 1 calc R . . H58C H 0.7886 0.2777 -0.2043 0.331 Uiso 1 1 calc R . . C59 C 0.8852(16) 0.2993(12) -0.2099(4) 0.241(19) Uani 1 1 d . . . H59A H 0.9341 0.2914 -0.2021 0.289 Uiso 1 1 calc R . . H59B H 0.8745 0.3269 -0.1998 0.289 Uiso 1 1 calc R . . C60 C 0.8281(11) 0.3240(9) -0.2657(4) 0.133(9) Uani 1 1 d . . . C61 C 0.7763(13) 0.3467(9) -0.2493(6) 0.147(9) Uani 1 1 d . . . H61A H 0.7767 0.3488 -0.2245 0.176 Uiso 1 1 calc R . . C62 C 0.7252(15) 0.3662(8) -0.2675(7) 0.165(10) Uani 1 1 d . . . H62A H 0.6887 0.3809 -0.2553 0.198 Uiso 1 1 calc R . . C63 C 0.7244(11) 0.3652(8) -0.3041(5) 0.141(9) Uani 1 1 d . . . C64 C 0.6704(9) 0.3849(7) -0.3218(4) 0.114(7) Uani 1 1 d . . . H64A H 0.6330 0.3980 -0.3091 0.137 Uiso 1 1 calc R . . C65 C 0.6694(10) 0.3859(6) -0.3599(5) 0.112(6) Uani 1 1 d . . . C66 C 0.7256(11) 0.3655(6) -0.3766(5) 0.116(6) Uani 1 1 d . . . H66A H 0.7270 0.3654 -0.4015 0.139 Uiso 1 1 calc R . . C67 C 0.7763(10) 0.3464(6) -0.3594(4) 0.112(7) Uani 1 1 d . . . H67A H 0.8131 0.3334 -0.3727 0.135 Uiso 1 1 calc R . . C68 C 0.7812(8) 0.3435(6) -0.3214(4) 0.096(6) Uani 1 1 d . . . C69 C 0.8372(9) 0.3225(7) -0.3024(5) 0.114(7) Uani 1 1 d . . . C70 C 0.6084(9) 0.4081(6) -0.3767(6) 0.114(7) Uani 1 1 d . . . H70A H 0.5721 0.4203 -0.3626 0.137 Uiso 1 1 calc R . . C71 C 0.6045(10) 0.4108(8) -0.4100(7) 0.157(10) Uani 1 1 d . . . H71A H 0.6433 0.3986 -0.4225 0.189 Uiso 1 1 calc R . . C72 C 0.4437(10) 0.4734(6) -0.4349(5) 0.118(7) Uani 1 1 d . . . H72A H 0.4081 0.4876 -0.4217 0.141 Uiso 1 1 calc R . . C73 C 0.4948(12) 0.4540(7) -0.4164(5) 0.132(7) Uani 1 1 d . . . H73A H 0.4951 0.4563 -0.3916 0.159 Uiso 1 1 calc R . . C74 C 0.5467(10) 0.4308(6) -0.4326(6) 0.109(6) Uani 1 1 d . . . C75 C 0.5472(12) 0.4345(8) -0.4688(5) 0.151(9) Uani 1 1 d . . . H75A H 0.5869 0.4237 -0.4815 0.181 Uiso 1 1 calc R . . C76 C 0.4958(11) 0.4520(6) -0.4857(5) 0.120(7) Uani 1 1 d . . . H76A H 0.4959 0.4499 -0.5105 0.144 Uiso 1 1 calc R . . O6 O 1.3648(14) 0.4426(8) -0.5347(7) 0.102(9) Uiso 0.50 1 d P . . C120 C 1.3649(15) 0.4318(9) -0.5494(8) 0.142(10) Uiso 1 1 d . . . N110 N 1.3805(12) 0.4061(8) -0.5818(7) 0.192(8) Uiso 1 1 d . . . C121 C 1.365(2) 0.3811(11) -0.6165(9) 0.281(17) Uiso 1 1 d . . . H12B H 1.3181 0.3898 -0.6260 0.422 Uiso 1 1 calc R . . H12C H 1.3633 0.3514 -0.6112 0.422 Uiso 1 1 calc R . . H12D H 1.4025 0.3866 -0.6337 0.422 Uiso 1 1 calc R . . C122 C 1.4480(19) 0.3781(10) -0.5799(9) 0.268(17) Uiso 1 1 d . . . H12E H 1.4768 0.3859 -0.5594 0.402 Uiso 1 1 calc R . . H12F H 1.4767 0.3816 -0.6012 0.402 Uiso 1 1 calc R . . H12G H 1.4331 0.3490 -0.5778 0.402 Uiso 1 1 calc R . . C89 C 0.576(3) -0.038(4) 0.076(3) 0.21(5) Uiso 0.25 1 d PD . . C90 C 0.647(4) -0.087(2) 0.1372(18) 0.10(2) Uiso 0.25 1 d P . . O11 O 0.702(4) -0.094(2) 0.1186(19) 0.20(3) Uiso 0.25 1 d P . . C91 C 0.627(17) -0.068(8) 0.073(5) 0.6(3) Uiso 0.25 1 d PD . . Cl1 Cl 0.1536(10) 0.1287(6) 0.1416(5) 0.320(6) Uiso 1 1 d . . . O18 O 0.084(2) 0.1392(12) 0.1561(10) 0.377(18) Uiso 1 1 d . . . O19 O 0.1582(18) 0.0851(11) 0.1311(8) 0.351(16) Uiso 1 1 d D . . O20 O 0.217(3) 0.1447(17) 0.1673(15) 0.51(3) Uiso 1 1 d . . . O21 O 0.1765(13) 0.1597(8) 0.1169(6) 0.260(10) Uiso 1 1 d . . . Cl2 Cl 0.3665(7) -0.0929(4) 0.0867(3) 0.306(5) Uiso 1 1 d D . . O31 O 0.388(2) -0.1286(9) 0.1022(10) 0.60(4) Uiso 1 1 d D . . O32 O 0.3239(15) -0.1017(11) 0.0578(7) 0.42(2) Uiso 1 1 d D . . O33 O 0.4246(14) -0.0695(11) 0.0754(9) 0.45(2) Uiso 1 1 d D . . O34 O 0.3302(17) -0.0672(10) 0.1097(8) 0.46(2) Uiso 1 1 d D . . O12 O 1.096(2) -0.1239(14) 0.3276(11) 0.182(18) Uiso 0.50 1 d P . . C92 C 1.029(3) -0.126(2) 0.3027(17) 0.22(3) Uiso 0.50 1 d PD . . C93 C 1.081(2) -0.1421(14) 0.3252(11) 0.100(14) Uiso 0.50 1 d P . . O13 O 1.004(5) -0.1031(13) 0.7600(16) 0.27(2) Uiso 0.50 1 d P . . C94 C 1.004(3) -0.1520(10) 0.7602(8) 0.105(11) Uiso 0.50 1 d P . . C95 C 1.0000 -0.1976(5) 0.7500 0.054(4) Uiso 1 2 d S . . C97 C 0.210(5) 0.026(2) 0.2624(11) 0.13(3) Uiso 0.25 1 d PD . . C96 C 0.215(4) 0.012(3) 0.3001(14) 0.15(3) Uiso 0.25 1 d PD . . O14 O 0.136(6) 0.030(3) 0.2531(19) 0.32(5) Uiso 0.25 1 d PD . . C99 C 0.039(3) -0.012(2) 0.1791(16) 0.22(3) Uiso 0.50 1 d PD . . C98 C 0.068(3) -0.0292(19) 0.1450(16) 0.21(2) Uiso 0.50 1 d PD . . O15 O -0.002(3) 0.0160(19) 0.1788(14) 0.30(2) Uiso 0.50 1 d PD . . O16 O 0.274(4) 0.025(2) 0.162(2) 0.21(3) Uiso 0.25 1 d PD . . C100 C 0.207(3) 0.012(2) 0.1843(11) 0.10(2) Uiso 0.25 1 d PD . . C101 C 0.220(3) 0.0015(13) 0.1461(11) 0.14(3) Uiso 0.25 1 d PD . . C116 C 0.857(7) -0.025(4) 0.102(2) 0.23(5) Uiso 0.25 1 d PD . . N11 N 0.611(7) -0.080(4) 0.105(4) 0.27(5) Uiso 0.25 1 d PD . . C103 C 0.915(4) -0.047(2) 0.1166(18) 0.10(2) Uiso 0.25 1 d P . . O22 O 1.2065(13) 0.2005(8) 0.4694(7) 0.135(9) Uiso 0.50 1 d P . . C104 C 1.2415(12) 0.1781(8) 0.4986(7) 0.065(7) Uiso 0.50 1 d PD . . C105 C 1.3036(14) 0.1947(9) 0.5158(7) 0.074(8) Uiso 0.50 1 d P . . O23 O 0.486(5) -0.008(3) 0.133(2) 0.26(5) Uiso 0.25 1 d PD . . C106 C 0.475(5) 0.003(3) 0.148(2) 0.11(2) Uiso 0.25 1 d P . . C107 C 0.431(4) 0.006(4) 0.165(3) 0.21(5) Uiso 0.25 1 d PD . . O24 O 0.978(3) 0.596(2) 0.244(2) 0.16(3) Uiso 0.25 1 d P . . C108 C 0.950(7) 0.569(4) 0.268(4) 0.21(5) Uiso 0.25 1 d P . . C109 C 1.032(6) 0.573(4) 0.263(3) 0.15(4) Uiso 0.25 1 d P . . O25 O 0.263(4) 0.014(2) 0.371(2) 0.21(3) Uiso 0.25 1 d P . . C110 C 0.276(3) 0.0157(18) 0.3267(14) 0.073(16) Uiso 0.25 1 d PD . . C111 C 0.318(4) 0.039(2) 0.337(2) 0.12(2) Uiso 0.25 1 d P . . O26 O 1.266(5) 0.443(3) 0.277(3) 0.27(4) Uiso 0.25 1 d P . . C112 C 1.161(4) 0.411(2) 0.2708(18) 0.26(3) Uiso 0.50 1 d PD . . C113 C 1.206(5) 0.432(3) 0.243(2) 0.16(3) Uiso 0.25 1 d PD . . O27 O 1.3792(18) 0.1329(10) 0.4388(9) 0.166(11) Uiso 0.50 1 d PD . . C114 C 1.465(2) 0.1018(16) 0.4772(12) 0.155(17) Uiso 0.50 1 d P . . C115 C 1.423(3) 0.134(2) 0.4630(15) 0.24(3) Uiso 0.50 1 d PD . . O101 O 1.0000 -0.064(3) 0.2500 0.27(6) Uiso 0.50 2 d SPD . . O102 O 0.324(2) 0.0325(14) 0.3026(12) 0.239(17) Uiso 0.50 1 d P . . O103 O 0.321(4) 0.027(2) 0.3831(19) 0.19(3) Uiso 0.25 1 d P . . O17 O 0.864(3) -0.0453(15) 0.0665(13) 0.259(19) Uiso 0.50 1 d PD . . O106 O 1.276(4) 0.0000 0.5000 0.26(3) Uiso 0.50 2 d SP . . O107 O 1.133(4) 0.121(2) 0.522(2) 0.29(4) Uiso 0.25 1 d PD . . 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 0.0498(14) 0.206(4) 0.0513(14) 0.000 0.0034(13) 0.000 Cu2 0.0772(18) 0.131(3) 0.112(2) 0.046(2) 0.000 0.000 O1 0.047(6) 0.255(15) 0.061(6) 0.006(8) -0.019(5) -0.015(7) O2 0.048(6) 0.240(15) 0.057(6) -0.014(8) 0.003(5) -0.002(7) O3 0.062(8) 0.29(3) 0.061(8) 0.000 -0.002(8) 0.000 O4 0.099(10) 0.193(16) 0.118(11) 0.068(11) -0.012(9) -0.050(10) O5 0.163(12) 0.239(17) 0.072(7) 0.019(10) 0.037(9) 0.026(11) N1 0.059(8) 0.155(14) 0.079(9) -0.004(10) -0.028(7) 0.000(9) N2 0.070(8) 0.162(14) 0.060(8) 0.011(10) 0.023(7) 0.011(10) N3 0.081(9) 0.066(10) 0.159(13) 0.077(10) 0.031(9) -0.004(8) N4 0.121(12) 0.131(13) 0.134(14) 0.096(12) -0.024(11) 0.032(11) C2 0.084(12) 0.21(2) 0.042(9) -0.016(11) -0.045(9) 0.029(15) C3 0.049(10) 0.20(2) 0.093(14) -0.041(16) -0.031(10) -0.002(13) C4 0.115(17) 0.20(3) 0.097(15) 0.049(17) 0.016(14) -0.018(16) C5 0.081(12) 0.30(3) 0.026(8) -0.028(13) -0.036(9) 0.019(17) C6 0.054(11) 0.20(3) 0.15(2) -0.065(19) -0.004(13) 0.038(14) C7 0.060(11) 0.19(2) 0.098(15) -0.007(15) -0.010(11) 0.031(13) C8 0.040(10) 0.20(2) 0.099(15) -0.031(15) 0.021(11) -0.011(12) C9 0.074(13) 0.24(3) 0.076(13) 0.021(17) 0.021(11) 0.028(15) C10 0.049(10) 0.20(2) 0.063(11) -0.036(13) 0.004(9) -0.029(13) C11 0.063(11) 0.23(3) 0.089(13) -0.004(16) 0.001(11) 0.029(13) C12 0.105(13) 0.20(2) 0.045(9) 0.005(11) 0.025(9) -0.023(14) C14 0.053(9) 0.166(17) 0.079(11) -0.012(13) -0.003(9) 0.021(10) C15 0.054(10) 0.150(17) 0.089(13) -0.014(13) -0.002(9) 0.027(12) C16 0.060(10) 0.21(2) 0.068(10) 0.004(14) -0.023(9) -0.017(12) C17 0.070(11) 0.25(2) 0.056(10) 0.024(13) 0.026(9) 0.024(16) C18 0.22(2) 0.30(3) 0.077(12) 0.071(17) -0.036(16) -0.17(3) C19 0.143(17) 0.28(3) 0.069(11) 0.023(16) -0.047(12) 0.024(19) C20 0.102(13) 0.27(3) 0.095(13) -0.036(17) 0.018(11) -0.016(17) C21 0.082(11) 0.20(2) 0.117(14) -0.021(15) 0.006(13) -0.004(15) C22 0.076(11) 0.106(13) 0.074(11) 0.003(11) -0.034(10) -0.021(9) C23 0.033(8) 0.130(15) 0.086(12) 0.023(11) 0.001(8) -0.007(9) C24 0.090(13) 0.21(2) 0.049(10) 0.006(13) -0.024(10) -0.013(13) C25 0.065(10) 0.190(19) 0.049(10) -0.001(11) 0.007(9) -0.017(13) C26 0.081(13) 0.22(2) 0.030(9) 0.000(12) 0.011(9) -0.002(15) C27 0.056(9) 0.18(2) 0.080(12) 0.041(13) 0.035(9) 0.024(10) C28 0.052(10) 0.190(19) 0.049(10) 0.014(11) -0.015(8) 0.021(12) C29 0.046(8) 0.208(19) 0.050(9) 0.013(12) 0.002(8) 0.006(10) C30 0.037(9) 0.28(3) 0.058(10) 0.013(13) -0.019(8) 0.002(12) C31 0.038(9) 0.26(3) 0.064(11) 0.016(14) -0.029(9) 0.020(12) C32 0.095(13) 0.20(2) 0.041(9) 0.015(12) -0.010(9) 0.046(14) C33 0.078(12) 0.26(3) 0.129(18) 0.03(2) 0.055(13) -0.006(15) C35 0.078(11) 0.19(2) 0.047(9) -0.015(11) 0.018(9) 0.005(13) C36 0.078(12) 0.18(2) 0.080(12) 0.019(13) 0.012(10) 0.007(14) C38 0.085(12) 0.22(2) 0.063(10) 0.014(13) 0.053(10) -0.047(14) C39 0.104(15) 0.17(2) 0.17(2) -0.04(2) 0.017(15) -0.047(18) C40 0.120(16) 0.26(3) 0.069(12) -0.003(17) 0.027(11) -0.013(19) C41 0.23(3) 0.060(15) 0.24(3) 0.031(18) -0.11(3) -0.04(2) C42 0.15(2) 0.077(17) 0.39(5) -0.03(2) 0.07(3) 0.046(17) C43 0.075(11) 0.113(18) 0.19(2) 0.081(15) 0.028(12) -0.028(11) C44 0.096(13) 0.085(15) 0.126(16) 0.017(13) 0.014(11) -0.038(12) C45 0.111(14) 0.130(19) 0.059(10) 0.035(12) 0.020(10) -0.028(13) C46 0.078(14) 0.19(2) 0.081(14) -0.051(17) -0.020(11) 0.040(17) C47 0.062(12) 0.23(3) 0.098(15) -0.067(18) -0.021(11) -0.012(16) C48 0.049(9) 0.16(2) 0.064(10) 0.012(12) -0.023(9) -0.007(13) C49 0.114(14) 0.126(17) 0.055(10) -0.019(11) -0.026(11) 0.005(14) C50 0.109(15) 0.19(2) 0.065(11) 0.040(14) 0.015(11) -0.022(16) C51 0.091(16) 0.21(3) 0.068(14) 0.063(18) -0.022(12) 0.046(19) C52 0.086(15) 0.20(3) 0.044(10) 0.002(15) -0.012(10) 0.057(17) C53 0.075(12) 0.16(2) 0.046(10) -0.007(13) -0.008(9) -0.001(14) C54 0.110(15) 0.117(17) 0.066(12) 0.019(12) 0.001(10) 0.015(13) C55 0.094(13) 0.22(2) 0.074(11) 0.000(14) 0.017(12) -0.005(17) C56 0.14(2) 0.19(3) 0.19(2) 0.06(2) 0.091(17) -0.050(19) C57 0.138(17) 0.24(3) 0.153(19) 0.05(2) -0.021(16) -0.066(19) C58 0.20(3) 0.34(4) 0.117(19) 0.09(2) 0.007(18) -0.15(3) C59 0.24(3) 0.44(6) 0.038(11) 0.06(2) -0.036(15) 0.10(3) C60 0.103(14) 0.26(3) 0.035(10) -0.012(14) -0.035(10) 0.034(17) C61 0.123(17) 0.24(3) 0.073(13) -0.030(18) -0.008(15) 0.015(18) C62 0.15(2) 0.21(3) 0.14(2) 0.03(2) 0.016(18) 0.02(2) C63 0.100(15) 0.26(3) 0.063(13) 0.012(15) -0.020(12) 0.026(16) C64 0.090(12) 0.20(2) 0.054(11) -0.007(12) -0.009(10) -0.021(13) C65 0.103(14) 0.122(17) 0.110(16) 0.019(13) 0.008(13) 0.002(12) C66 0.102(14) 0.137(18) 0.108(15) 0.029(13) 0.014(14) 0.015(13) C67 0.112(13) 0.18(2) 0.041(10) -0.011(11) -0.016(9) 0.059(14) C68 0.061(10) 0.137(16) 0.090(13) -0.006(12) 0.032(10) 0.003(10) C69 0.071(12) 0.18(2) 0.087(14) 0.033(14) -0.021(10) -0.003(12) C70 0.079(12) 0.136(17) 0.129(17) 0.023(14) -0.055(12) -0.004(11) C71 0.078(13) 0.20(3) 0.20(2) -0.03(2) -0.053(16) 0.065(14) C72 0.101(13) 0.155(18) 0.097(14) 0.084(14) -0.020(11) 0.006(12) C73 0.114(15) 0.17(2) 0.116(15) -0.016(15) -0.027(14) 0.042(16) C74 0.095(13) 0.107(15) 0.126(17) 0.023(13) 0.023(12) 0.036(11) C75 0.139(18) 0.24(3) 0.077(14) 0.035(16) 0.009(13) 0.056(18) C76 0.123(14) 0.136(16) 0.102(13) 0.035(12) -0.019(13) 0.085(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N2 2.018(11) 3_656 ? Cu1 N2 2.018(11) 1_655 ? Cu1 N1 2.030(11) 3_756 ? Cu1 N1 2.030(11) . ? Cu1 O3 2.30(2) . ? Cu2 N3 1.942(12) . ? Cu2 N3 1.942(12) 4_564 ? Cu2 N4 1.974(13) 1_655 ? Cu2 N4 1.974(13) 4_664 ? Cu2 O6 2.28(3) 4_564 ? Cu2 O6 2.28(3) . ? O1 C13 1.35(2) . ? O1 C18 1.503(19) . ? O2 C21 1.415(18) . ? O2 C31 1.421(17) . ? O4 C51 1.32(2) . ? O4 C56 1.39(3) . ? O5 C60 1.37(2) . ? O5 C59 1.60(2) . ? N1 C1 1.34(2) . ? N1 C5 1.44(2) . ? N2 C34 1.378(19) . ? N2 C38 1.37(2) . ? N2 Cu1 2.018(11) 1_455 ? N3 C39 1.27(2) . ? N3 C43 1.37(2) . ? N4 C72 1.32(2) . ? N4 C76 1.46(2) . ? N4 Cu2 1.974(13) 1_455 ? C1 C2 1.46(2) . ? C2 C3 1.35(3) . ? C3 C4 1.32(3) . ? C3 C6 1.62(3) . ? C4 C5 1.34(2) . ? C6 C7 1.31(3) . ? C7 C8 1.53(2) . ? C8 C9 1.31(3) . ? C8 C17 1.50(3) . ? C9 C10 1.35(2) . ? C10 C15 1.39(2) . ? C10 C11 1.46(3) . ? C11 C12 1.41(2) . ? C12 C13 1.54(2) . ? C13 C14 1.30(2) . ? C14 C15 1.52(2) . ? C14 C22 1.51(2) . ? C15 C16 1.49(2) . ? C16 C17 1.358(19) . ? C18 C19 1.64(2) . ? C20 C21 1.60(2) . ? C22 C31 1.40(2) . ? C22 C23 1.406(19) . ? C23 C28 1.37(2) . ? C23 C24 1.49(2) . ? C24 C25 1.30(2) . ? C25 C26 1.36(2) . ? C26 C27 1.32(2) . ? C26 C32 1.50(2) . ? C27 C28 1.487(19) . ? C28 C29 1.38(2) . ? C29 C30 1.457(18) . ? C30 C31 1.40(3) . ? C32 C33 1.27(3) . ? C33 C36 1.559(16) . ? C34 C35 1.38(2) . ? C35 C36 1.38(2) . ? C36 C37 1.44(2) . ? C37 C38 1.37(2) . ? C39 C40 1.540(17) . ? C40 C41 1.28(3) . ? C41 C44 1.43(3) . ? C41 C42 1.51(4) . ? C42 C43 1.35(3) . ? C44 C45 1.17(2) . ? C45 C46 1.47(3) . ? C46 C55 1.37(2) . ? C46 C47 1.45(3) . ? C47 C48 1.35(2) . ? C48 C49 1.47(2) . ? C48 C53 1.49(2) . ? C49 C50 1.35(2) . ? C50 C51 1.44(3) . ? C51 C52 1.36(3) . ? C52 C53 1.46(3) . ? C52 C69 1.54(2) . ? C53 C54 1.39(2) . ? C54 C55 1.40(2) . ? C56 C57 1.49(2) . ? C58 C59 1.38(4) . ? C60 C61 1.36(3) . ? C60 C69 1.41(2) . ? C61 C62 1.33(3) . ? C62 C63 1.40(3) . ? C63 C64 1.37(2) . ? C63 C68 1.43(2) . ? C64 C65 1.46(2) . ? C65 C66 1.39(2) . ? C65 C70 1.49(2) . ? C66 C67 1.31(2) . ? C67 C68 1.46(2) . ? C68 C69 1.44(2) . ? C70 C71 1.28(3) . ? C71 C74 1.52(3) . ? C72 C73 1.34(2) . ? C73 C74 1.37(2) . ? C74 C75 1.39(2) . ? C75 C76 1.29(2) . ? O6 C120 0.66(4) . ? C120 N110 1.52(3) . ? N110 C122 1.55(3) . ? N110 C121 1.58(4) . ? C89 C91 1.37(3) . ? C89 N11 1.85(17) . ? C90 O11 1.27(8) . ? C90 N11 1.43(13) . ? C91 N11 1.31(4) . ? Cl1 O21 1.44(2) . ? Cl1 O18 1.45(4) . ? Cl1 O19 1.46(3) . ? Cl1 O20 1.62(5) . ? Cl2 O31 1.354(17) . ? Cl2 O34 1.383(17) . ? Cl2 O32 1.387(16) . ? Cl2 O33 1.388(17) . ? O12 C93 0.66(6) . ? O12 C92 1.56(7) . ? C92 C93 1.39(7) . ? O13 O13 0.78(12) 3_756 ? O13 C94 1.58(4) . ? O13 C94 1.76(5) 3_756 ? C94 C94 0.80(6) 3_756 ? C94 C95 1.52(3) . ? C94 O13 1.76(5) 3_756 ? C95 C94 1.52(3) 3_756 ? C97 O14 1.42(12) . ? C97 C96 1.52(2) . ? C96 C110 1.52(2) . ? C99 O15 1.20(2) . ? C99 C98 1.51(2) . ? O16 C101 1.41(8) . ? O16 C100 1.56(8) . ? C100 C101 1.51(2) . ? C116 C103 1.41(13) . ? C116 O17 1.51(2) . ? O22 C104 1.48(3) . ? C104 C105 1.43(3) . ? O23 C106 0.71(12) . ? O23 C107 1.66(12) . ? C106 C107 1.05(11) . ? O24 O24 0.93(13) 3_755 ? O24 C109 0.82(11) 3_755 ? O24 C108 1.36(14) . ? O24 C108 1.68(15) 3_755 ? O24 C109 1.44(11) . ? C108 C109 1.24(14) 3_755 ? C108 O24 1.68(15) 3_755 ? C108 C109 1.54(14) . ? C109 O24 0.82(12) 3_755 ? C109 C108 1.24(14) 3_755 ? C109 C109 1.6(2) 3_755 ? O25 O103 1.25(9) . ? O25 C110 1.70(9) . ? O25 C111 1.81(10) . ? C110 C111 1.16(8) . ? C110 O102 1.39(6) . ? C111 O102 1.34(8) . ? C111 O103 1.78(10) . ? O26 C113 1.72(11) . ? C112 C113 1.51(2) . ? O27 C115 1.24(2) . ? C114 C115 1.41(7) . ? 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 N2 Cu1 N2 173.3(10) 3_656 1_655 ? N2 Cu1 N1 86.9(5) 3_656 3_756 ? N2 Cu1 N1 92.8(5) 1_655 3_756 ? N2 Cu1 N1 92.8(5) 3_656 . ? N2 Cu1 N1 86.9(5) 1_655 . ? N1 Cu1 N1 175.5(10) 3_756 . ? N2 Cu1 O3 93.3(5) 3_656 . ? N2 Cu1 O3 93.3(5) 1_655 . ? N1 Cu1 O3 92.2(5) 3_756 . ? N1 Cu1 O3 92.2(5) . . ? N3 Cu2 N3 92.1(8) . 4_564 ? N3 Cu2 N4 87.8(6) . 1_655 ? N3 Cu2 N4 178.9(8) 4_564 1_655 ? N3 Cu2 N4 178.9(8) . 4_664 ? N3 Cu2 N4 87.8(6) 4_564 4_664 ? N4 Cu2 N4 92.3(9) 1_655 4_664 ? N3 Cu2 O6 90.6(8) . 4_564 ? N3 Cu2 O6 90.1(8) 4_564 4_564 ? N4 Cu2 O6 88.8(9) 1_655 4_564 ? N4 Cu2 O6 90.5(9) 4_664 4_564 ? N3 Cu2 O6 90.1(8) . . ? N3 Cu2 O6 90.6(8) 4_564 . ? N4 Cu2 O6 90.5(9) 1_655 . ? N4 Cu2 O6 88.8(9) 4_664 . ? O6 Cu2 O6 179.0(13) 4_564 . ? C13 O1 C18 116.5(14) . . ? C21 O2 C31 115.2(12) . . ? C51 O4 C56 112(2) . . ? C60 O5 C59 115.0(15) . . ? C1 N1 C5 121.5(14) . . ? C1 N1 Cu1 121.0(14) . . ? C5 N1 Cu1 117.5(12) . . ? C34 N2 C38 119.9(14) . . ? C34 N2 Cu1 124.0(13) . 1_455 ? C38 N2 Cu1 116.1(11) . 1_455 ? C39 N3 C43 113.9(16) . . ? C39 N3 Cu2 122.6(14) . . ? C43 N3 Cu2 123.4(13) . . ? C72 N4 C76 109.9(14) . . ? C72 N4 Cu2 132.2(15) . 1_455 ? C76 N4 Cu2 117.9(13) . 1_455 ? N1 C1 C2 116.8(18) . . ? C3 C2 C1 119.3(19) . . ? C4 C3 C2 122.0(18) . . ? C4 C3 C6 123(2) . . ? C2 C3 C6 114(2) . . ? C3 C4 C5 122(2) . . ? C4 C5 N1 118(2) . . ? C7 C6 C3 124(2) . . ? C6 C7 C8 124(2) . . ? C9 C8 C17 121.3(19) . . ? C9 C8 C7 120(2) . . ? C17 C8 C7 118(2) . . ? C8 C9 C10 119(2) . . ? C9 C10 C15 124(2) . . ? C9 C10 C11 116(2) . . ? C15 C10 C11 119.8(17) . . ? C12 C11 C10 118.0(19) . . ? C11 C12 C13 120.4(19) . . ? C14 C13 O1 120.3(18) . . ? C14 C13 C12 120.9(19) . . ? O1 C13 C12 118.3(19) . . ? C13 C14 C15 118.3(19) . . ? C13 C14 C22 122.6(15) . . ? C15 C14 C22 118.8(17) . . ? C10 C15 C16 118.4(16) . . ? C10 C15 C14 122(2) . . ? C16 C15 C14 119.1(17) . . ? C17 C16 C15 116.2(18) . . ? C16 C17 C8 120.3(19) . . ? O1 C18 C19 99.1(14) . . ? O2 C21 C20 104.0(14) . . ? C31 C22 C23 116.8(15) . . ? C31 C22 C14 115.9(16) . . ? C23 C22 C14 127.0(16) . . ? C28 C23 C22 119.7(16) . . ? C28 C23 C24 118.5(14) . . ? C22 C23 C24 121.8(16) . . ? C25 C24 C23 117.9(17) . . ? C24 C25 C26 126.7(17) . . ? C27 C26 C25 117.3(15) . . ? C27 C26 C32 114.5(19) . . ? C25 C26 C32 128.0(19) . . ? C26 C27 C28 122.7(18) . . ? C23 C28 C29 123.5(15) . . ? C23 C28 C27 116.8(17) . . ? C29 C28 C27 119.7(17) . . ? C28 C29 C30 119.8(16) . . ? C31 C30 C29 113.9(17) . . ? C22 C31 C30 126.2(15) . . ? C22 C31 O2 115.7(17) . . ? C30 C31 O2 117.9(17) . . ? C33 C32 C26 122(2) . . ? C32 C33 C36 120(2) . . ? N2 C34 C35 123.6(16) . . ? C36 C35 C34 116.6(16) . . ? C35 C36 C37 120.0(15) . . ? C35 C36 C33 126(2) . . ? C37 C36 C33 114(2) . . ? C38 C37 C36 120.9(19) . . ? C37 C38 N2 118.7(18) . . ? N3 C39 C40 121(2) . . ? C41 C40 C39 125(3) . . ? C40 C41 C44 123(3) . . ? C40 C41 C42 113(3) . . ? C44 C41 C42 124(2) . . ? C43 C42 C41 117(2) . . ? C42 C43 N3 130.0(19) . . ? C45 C44 C41 131(2) . . ? C44 C45 C46 134(2) . . ? C55 C46 C47 118(2) . . ? C55 C46 C45 116(2) . . ? C47 C46 C45 125(2) . . ? C48 C47 C46 122(2) . . ? C47 C48 C49 121(2) . . ? C47 C48 C53 119(2) . . ? C49 C48 C53 119.4(19) . . ? C50 C49 C48 124(2) . . ? C49 C50 C51 119(2) . . ? O4 C51 C52 116(3) . . ? O4 C51 C50 127(3) . . ? C52 C51 C50 117(2) . . ? C51 C52 C53 131(2) . . ? C51 C52 C69 116(2) . . ? C53 C52 C69 113(2) . . ? C54 C53 C52 133(2) . . ? C54 C53 C48 117.9(19) . . ? C52 C53 C48 110(2) . . ? C53 C54 C55 121(2) . . ? C46 C55 C54 121(2) . . ? O4 C56 C57 111(2) . . ? C58 C59 O5 116(3) . . ? O5 C60 C61 129.3(18) . . ? O5 C60 C69 106.1(19) . . ? C61 C60 C69 124(2) . . ? C62 C61 C60 121(2) . . ? C61 C62 C63 121(2) . . ? C64 C63 C62 120(2) . . ? C64 C63 C68 122.9(18) . . ? C62 C63 C68 118(2) . . ? C63 C64 C65 121.0(18) . . ? C66 C65 C64 116.0(18) . . ? C66 C65 C70 127.2(19) . . ? C64 C65 C70 116.8(19) . . ? C67 C66 C65 122.4(19) . . ? C66 C67 C68 125.3(17) . . ? C69 C68 C63 122.3(16) . . ? C69 C68 C67 125.2(15) . . ? C63 C68 C67 112.4(16) . . ? C60 C69 C68 113.3(18) . . ? C60 C69 C52 124.6(17) . . ? C68 C69 C52 121.7(16) . . ? C71 C70 C65 120(2) . . ? C70 C71 C74 129(2) . . ? N4 C72 C73 127(2) . . ? C72 C73 C74 121.4(19) . . ? C73 C74 C75 114.0(18) . . ? C73 C74 C71 118.3(19) . . ? C75 C74 C71 126.6(19) . . ? C76 C75 C74 122.3(19) . . ? C75 C76 N4 124.2(17) . . ? C120 O6 Cu2 157(5) . . ? O6 C120 N110 169(5) . . ? C120 N110 C122 116(2) . . ? C120 N110 C121 158(3) . . ? C122 N110 C121 84(2) . . ? C91 C89 N11 45(5) . . ? O11 C90 N11 86(7) . . ? N11 C91 C89 87(10) . . ? O21 Cl1 O18 111(2) . . ? O21 Cl1 O19 118(2) . . ? O18 Cl1 O19 112(3) . . ? O21 Cl1 O20 88(2) . . ? O18 Cl1 O20 110(3) . . ? O19 Cl1 O20 115(3) . . ? O31 Cl2 O34 112.1(16) . . ? O31 Cl2 O32 109.8(16) . . ? O34 Cl2 O32 110.4(16) . . ? O31 Cl2 O33 111.7(17) . . ? O34 Cl2 O33 104.7(15) . . ? O32 Cl2 O33 108.0(15) . . ? C93 O12 C92 63(6) . . ? C93 C92 O12 25(3) . . ? O12 C93 C92 92(7) . . ? O13 O13 C94 90(3) 3_756 . ? O13 O13 C94 63(2) 3_756 3_756 ? C94 O13 C94 27(2) . 3_756 ? C94 C94 C95 74.8(12) 3_756 . ? C94 C94 O13 90(3) 3_756 . ? C95 C94 O13 164(3) . . ? C94 C94 O13 63(2) 3_756 3_756 ? C95 C94 O13 138(3) . 3_756 ? O13 C94 O13 26(4) . 3_756 ? C94 C95 C94 30(2) . 3_756 ? O14 C97 C96 109(6) . . ? C97 C96 C110 131(6) . . ? O15 C99 C98 120(7) . . ? C101 O16 C100 61(3) . . ? C101 C100 O16 54(3) . . ? O16 C101 C100 65(4) . . ? C103 C116 O17 94(7) . . ? C91 N11 C90 138(10) . . ? C91 N11 C89 47(5) . . ? C90 N11 C89 142(10) . . ? C105 C104 O22 121(2) . . ? C106 O23 C107 24(10) . . ? O23 C106 C107 139(10) . . ? C106 C107 O23 16(8) . . ? O24 O24 C109 111(10) 3_755 3_755 ? O24 O24 C108 92(10) 3_755 . ? C109 O24 C108 63(10) 3_755 . ? O24 O24 C108 54(8) 3_755 3_755 ? C109 O24 C108 66(10) 3_755 3_755 ? C108 O24 C108 98(10) . 3_755 ? O24 O24 C109 32(5) 3_755 . ? C109 O24 C109 82(10) 3_755 . ? C108 O24 C109 67(6) . . ? C108 O24 C109 46(5) 3_755 . ? C109 C108 O24 36(7) 3_755 . ? C109 C108 O24 57(9) 3_755 3_755 ? O24 C108 O24 33(6) . 3_755 ? C109 C108 C109 67(10) 3_755 . ? O24 C108 C109 59(8) . . ? O24 C108 C109 29(5) 3_755 . ? O24 C109 C108 81(10) 3_755 3_755 ? O24 C109 C108 85(10) 3_755 . ? C108 C109 C108 111(10) 3_755 . ? O24 C109 O24 37(8) 3_755 . ? C108 C109 O24 77(10) 3_755 . ? C108 C109 O24 54(6) . . ? O24 C109 C109 66(10) 3_755 3_755 ? C108 C109 C109 66(9) 3_755 3_755 ? C108 C109 C109 47(6) . 3_755 ? O24 C109 C109 31(5) . 3_755 ? O103 O25 C110 104(7) . . ? O103 O25 C111 69(6) . . ? C110 O25 C111 38(3) . . ? C111 C110 O102 63(5) . . ? C111 C110 C96 142(7) . . ? O102 C110 C96 94(5) . . ? C111 C110 O25 76(6) . . ? O102 C110 O25 138(5) . . ? C96 C110 O25 124(5) . . ? C110 C111 O102 67(5) . . ? C110 C111 O103 104(7) . . ? O102 C111 O103 159(7) . . ? C110 C111 O25 66(5) . . ? O102 C111 O25 133(7) . . ? O103 C111 O25 41(3) . . ? C112 C113 O26 86(6) . . ? O27 C115 C114 129(7) . . ? C110 O102 C111 50(4) . . ? O25 O103 C111 71(6) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 20.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.361 _refine_diff_density_min -0.505 _refine_diff_density_rms 0.061 # Attachment 'new3.cif' data_new3 _database_code_depnum_ccdc_archive 'CCDC 607391' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H102 Cu N8 O22' _chemical_formula_weight 1639.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 32.153(1) _cell_length_b 16.217(1) _cell_length_c 21.2146(9) _cell_angle_alpha 90.00 _cell_angle_beta 118.535(7) _cell_angle_gamma 90.00 _cell_volume 9718.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.01 _cell_measurement_theta_max 27.63 _exptl_crystal_description Bloc _exptl_crystal_colour Blue _exptl_crystal_size_max 1.20 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.120 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3468 _exptl_absorpt_coefficient_mu 0.291 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.6222 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 58989 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_sigmaI/netI 0.0632 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 27.63 _reflns_number_total 21571 _reflns_number_gt 15486 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0988P)^2^+59.9892P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_number_reflns 21571 _refine_ls_number_parameters 895 _refine_ls_number_restraints 5 _refine_ls_R_factor_ref 0.1306 _refine_ls_R_factor_gt 0.0976 _refine_ls_wR_factor_ref 0.2703 _refine_ls_wR_factor_gt 0.2461 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.24615(2) 0.79697(5) 0.26191(3) 0.03814(18) Uani 1 1 d . . . O1 O 0.31911(15) 0.6785(3) -0.3435(2) 0.0479(11) Uani 1 1 d . . . O2 O 0.39170(16) 0.8093(3) -0.3142(2) 0.0466(10) Uani 1 1 d . . . O3 O 0.63912(16) 0.3204(3) 0.8524(2) 0.0506(11) Uani 1 1 d . . . O4 O 0.67023(17) 0.4911(3) 0.8896(2) 0.0464(10) Uani 1 1 d . . . O5 O 0.20313(18) 0.6680(3) 0.2272(3) 0.0509(11) Uani 1 1 d . . . H5B H 0.2071 0.6457 0.1947 0.061 Uiso 1 1 calc R . . H5C H 0.1863 0.6513 0.2486 0.061 Uiso 1 1 d R . . N1 N 0.27157(17) 0.7850(3) 0.1910(2) 0.0381(11) Uani 1 1 d . . . N2 N 0.68873(17) 0.3575(3) 0.1872(3) 0.0382(11) Uani 1 1 d . . . N3 N 0.30371(19) 0.7387(3) 0.3375(3) 0.0416(12) Uani 1 1 d . . . N4 N 0.72396(18) 0.3217(3) 0.3350(3) 0.0414(12) Uani 1 1 d . . . C1 C 0.2825(2) 0.7113(4) 0.1753(3) 0.0388(13) Uani 1 1 d . . . H1A H 0.2781 0.6639 0.1976 0.047 Uiso 1 1 calc R . . C2 C 0.3002(2) 0.7013(4) 0.1278(4) 0.0427(14) Uani 1 1 d . . . H2A H 0.3081 0.6478 0.1188 0.051 Uiso 1 1 calc R . . C3 C 0.3063(2) 0.7700(4) 0.0930(3) 0.0399(14) Uani 1 1 d . . . C4 C 0.2961(2) 0.8467(4) 0.1114(3) 0.0388(13) Uani 1 1 d . . . H4A H 0.3016 0.8954 0.0917 0.047 Uiso 1 1 calc R . . C5 C 0.2780(2) 0.8515(4) 0.1580(3) 0.0409(14) Uani 1 1 d . . . H5A H 0.2694 0.9042 0.1676 0.049 Uiso 1 1 calc R . . C6 C 0.3249(2) 0.7568(4) 0.0420(3) 0.0432(15) Uani 1 1 d . . . H6A H 0.3320 0.7018 0.0350 0.052 Uiso 1 1 calc R . . C7 C 0.3324(2) 0.8166(4) 0.0049(3) 0.0434(15) Uani 1 1 d . . . H7A H 0.3275 0.8721 0.0144 0.052 Uiso 1 1 calc R . . C8 C 0.3477(2) 0.8022(4) -0.0497(3) 0.0418(13) Uani 1 1 d . . . C9 C 0.3508(2) 0.8654(4) -0.0888(4) 0.0417(14) Uani 1 1 d . . . H9A H 0.3452 0.9198 -0.0780 0.050 Uiso 1 1 calc R . . C10 C 0.3619(2) 0.8540(4) -0.1454(3) 0.0365(13) Uani 1 1 d . . . C11 C 0.3634(2) 0.9212(4) -0.1885(4) 0.0467(15) Uani 1 1 d . . . H11A H 0.3579 0.9759 -0.1783 0.056 Uiso 1 1 calc R . . C12 C 0.3728(3) 0.9070(4) -0.2436(4) 0.0458(16) Uani 1 1 d . . . H12A H 0.3734 0.9520 -0.2717 0.055 Uiso 1 1 calc R . . C13 C 0.3815(2) 0.8265(4) -0.2599(3) 0.0386(13) Uani 1 1 d . . . C14 C 0.3811(2) 0.7590(4) -0.2194(3) 0.0365(12) Uani 1 1 d . . . C15 C 0.3717(2) 0.7729(3) -0.1608(3) 0.0344(12) Uani 1 1 d . . . C16 C 0.3705(2) 0.7081(4) -0.1168(3) 0.0405(14) Uani 1 1 d . . . H16A H 0.3786 0.6538 -0.1240 0.049 Uiso 1 1 calc R . . C17 C 0.3581(3) 0.7214(4) -0.0647(4) 0.0477(17) Uani 1 1 d . . . H17A H 0.3563 0.6760 -0.0378 0.057 Uiso 1 1 calc R . . C18 C 0.2488(3) 0.7042(6) -0.4507(5) 0.087(3) Uani 1 1 d . . . H18A H 0.2255 0.6805 -0.4966 0.130 Uiso 1 1 calc R . . H18B H 0.2635 0.7527 -0.4596 0.130 Uiso 1 1 calc R . . H18C H 0.2330 0.7205 -0.4230 0.130 Uiso 1 1 calc R . . C19 C 0.2857(3) 0.6423(5) -0.4100(4) 0.065(2) Uani 1 1 d . . . H19A H 0.2713 0.5929 -0.4010 0.078 Uiso 1 1 calc R . . H19B H 0.3018 0.6253 -0.4378 0.078 Uiso 1 1 calc R . . C20 C 0.3741(4) 0.8177(6) -0.4350(4) 0.084(3) Uani 1 1 d . . . H20A H 0.3604 0.8530 -0.4777 0.126 Uiso 1 1 calc R . . H20B H 0.3565 0.7658 -0.4455 0.126 Uiso 1 1 calc R . . H20C H 0.4073 0.8063 -0.4212 0.126 Uiso 1 1 calc R . . C21 C 0.3715(3) 0.8607(6) -0.3748(4) 0.066(2) Uani 1 1 d . . . H21A H 0.3888 0.9136 -0.3641 0.079 Uiso 1 1 calc R . . H21B H 0.3380 0.8724 -0.3882 0.079 Uiso 1 1 calc R . . C22 C 0.3909(2) 0.6737(4) -0.2367(3) 0.0343(12) Uani 1 1 d . . . C23 C 0.3585(2) 0.6351(4) -0.2987(3) 0.0404(14) Uani 1 1 d . . . C24 C 0.3662(2) 0.5521(4) -0.3147(3) 0.0408(13) Uani 1 1 d . . . H24A H 0.3437 0.5262 -0.3578 0.049 Uiso 1 1 calc R . . C25 C 0.4050(2) 0.5115(4) -0.2685(3) 0.0425(14) Uani 1 1 d . . . H25A H 0.4094 0.4564 -0.2794 0.051 Uiso 1 1 calc R . . C26 C 0.4395(2) 0.5470(4) -0.2042(3) 0.0379(13) Uani 1 1 d . . . C27 C 0.4799(2) 0.5019(4) -0.1540(3) 0.0430(14) Uani 1 1 d . . . H27A H 0.4846 0.4473 -0.1655 0.052 Uiso 1 1 calc R . . C28 C 0.5123(2) 0.5355(4) -0.0892(3) 0.0420(14) Uani 1 1 d . . . C29 C 0.5068(2) 0.6205(4) -0.0757(3) 0.0420(14) Uani 1 1 d . . . H29A H 0.5303 0.6459 -0.0331 0.050 Uiso 1 1 calc R . . C30 C 0.4678(2) 0.6666(4) -0.1238(3) 0.0364(12) Uani 1 1 d . . . H30A H 0.4647 0.7225 -0.1132 0.044 Uiso 1 1 calc R . . C31 C 0.4330(2) 0.6307(4) -0.1880(3) 0.0335(12) Uani 1 1 d . . . C32 C 0.5491(3) 0.4832(5) -0.0370(4) 0.0520(17) Uani 1 1 d . . . H32A H 0.5561 0.4336 -0.0539 0.062 Uiso 1 1 calc R . . C33 C 0.5736(2) 0.4990(4) 0.0316(4) 0.0444(14) Uani 1 1 d . . . H33A H 0.5666 0.5486 0.0484 0.053 Uiso 1 1 calc R . . C34 C 0.6610(2) 0.3242(4) 0.1224(3) 0.0432(15) Uani 1 1 d . . . H34A H 0.6684 0.2711 0.1115 0.052 Uiso 1 1 calc R . . C35 C 0.6218(2) 0.3659(5) 0.0711(3) 0.0490(16) Uani 1 1 d . . . H35A H 0.6019 0.3404 0.0263 0.059 Uiso 1 1 calc R . . C36 C 0.6114(2) 0.4462(4) 0.0852(4) 0.0424(14) Uani 1 1 d . . . C37 C 0.6407(2) 0.4778(4) 0.1538(4) 0.0439(14) Uani 1 1 d . . . H37A H 0.6348 0.5306 0.1673 0.053 Uiso 1 1 calc R . . C38 C 0.6780(2) 0.4316(4) 0.2009(4) 0.0446(15) Uani 1 1 d . . . H38A H 0.6977 0.4542 0.2471 0.054 Uiso 1 1 calc R . . C39 C 0.2991(2) 0.6777(4) 0.3761(3) 0.0451(14) Uani 1 1 d . . . H39A H 0.2684 0.6610 0.3669 0.054 Uiso 1 1 calc R . . C40 C 0.3395(3) 0.6376(4) 0.4304(3) 0.0470(15) Uani 1 1 d . . . H40A H 0.3356 0.5929 0.4560 0.056 Uiso 1 1 calc R . . C41 C 0.3838(2) 0.6623(4) 0.4463(3) 0.0467(16) Uani 1 1 d . . . C42 C 0.3873(3) 0.7247(5) 0.4035(4) 0.0572(19) Uani 1 1 d . . . H42A H 0.4175 0.7428 0.4113 0.069 Uiso 1 1 calc R . . C43 C 0.3470(2) 0.7595(5) 0.3504(4) 0.0487(16) Uani 1 1 d . . . H43A H 0.3501 0.8008 0.3212 0.058 Uiso 1 1 calc R . . C44 C 0.4278(3) 0.6282(5) 0.5045(4) 0.0494(16) Uani 1 1 d . . . H44A H 0.4565 0.6546 0.5134 0.059 Uiso 1 1 calc R . . C45 C 0.4314(3) 0.5654(5) 0.5448(4) 0.0548(18) Uani 1 1 d . . . H45A H 0.4028 0.5393 0.5368 0.066 Uiso 1 1 calc R . . C46 C 0.4760(2) 0.5312(5) 0.6020(4) 0.0505(17) Uani 1 1 d . . . C47 C 0.4735(2) 0.4630(5) 0.6411(4) 0.0501(16) Uani 1 1 d . . . H47A H 0.4436 0.4408 0.6305 0.060 Uiso 1 1 calc R . . C48 C 0.5149(2) 0.4275(4) 0.6956(3) 0.0426(14) Uani 1 1 d . . . C49 C 0.5124(2) 0.3599(5) 0.7365(4) 0.0509(16) Uani 1 1 d . . . H49A H 0.4824 0.3390 0.7274 0.061 Uiso 1 1 calc R . . C50 C 0.5531(2) 0.3252(4) 0.7888(4) 0.0489(16) Uani 1 1 d . . . H50A H 0.5511 0.2804 0.8162 0.059 Uiso 1 1 calc R . . C51 C 0.5981(2) 0.3552(4) 0.8027(3) 0.0420(14) Uani 1 1 d . . . C52 C 0.6025(2) 0.4200(4) 0.7631(3) 0.0378(13) Uani 1 1 d . . . C53 C 0.5607(2) 0.4583(4) 0.7108(3) 0.0395(13) Uani 1 1 d . . . C54 C 0.5617(2) 0.5272(4) 0.6701(3) 0.0440(15) Uani 1 1 d . . . H54A H 0.5912 0.5501 0.6791 0.053 Uiso 1 1 calc R . . C55 C 0.5201(3) 0.5612(4) 0.6177(4) 0.0485(16) Uani 1 1 d . . . H55A H 0.5219 0.6072 0.5913 0.058 Uiso 1 1 calc R . . C56 C 0.6374(3) 0.2619(5) 0.9030(5) 0.066(2) Uani 1 1 d . . . H56A H 0.6221 0.2101 0.8781 0.079 Uiso 1 1 calc R . . H56B H 0.6187 0.2851 0.9248 0.079 Uiso 1 1 calc R . . C57 C 0.6871(3) 0.2450(5) 0.9602(4) 0.072(2) Uani 1 1 d . . . H57A H 0.6866 0.2056 0.9949 0.108 Uiso 1 1 calc R . . H57B H 0.7019 0.2965 0.9849 0.108 Uiso 1 1 calc R . . H57C H 0.7053 0.2218 0.9383 0.108 Uiso 1 1 calc R . . C58 C 0.6838(4) 0.4929(6) 1.0089(4) 0.076(3) Uani 1 1 d . . . H58A H 0.7083 0.4931 1.0594 0.115 Uiso 1 1 calc R . . H58B H 0.6639 0.4437 0.9993 0.115 Uiso 1 1 calc R . . H58C H 0.6642 0.5424 0.9988 0.115 Uiso 1 1 calc R . . C59 C 0.7063(3) 0.4920(5) 0.9632(4) 0.0572(18) Uani 1 1 d . . . H59A H 0.7265 0.5414 0.9727 0.069 Uiso 1 1 calc R . . H59B H 0.7266 0.4425 0.9737 0.069 Uiso 1 1 calc R . . C60 C 0.6502(2) 0.4447(3) 0.7741(3) 0.0342(12) Uani 1 1 d . . . C61 C 0.6836(2) 0.4768(4) 0.8378(3) 0.0375(13) Uani 1 1 d . . . C62 C 0.7296(2) 0.4966(4) 0.8500(3) 0.0418(14) Uani 1 1 d . . . H62A H 0.7529 0.5149 0.8961 0.050 Uiso 1 1 calc R . . C63 C 0.7405(2) 0.4895(4) 0.7961(4) 0.0417(14) Uani 1 1 d . . . H63A H 0.7712 0.5048 0.8044 0.050 Uiso 1 1 calc R . . C64 C 0.7074(2) 0.4601(4) 0.7277(3) 0.0382(13) Uani 1 1 d . . . C65 C 0.7183(2) 0.4511(4) 0.6711(4) 0.0436(14) Uani 1 1 d . . . H65A H 0.7489 0.4668 0.6787 0.052 Uiso 1 1 calc R . . C66 C 0.6862(2) 0.4204(4) 0.6051(3) 0.0451(15) Uani 1 1 d . . . C67 C 0.6426(2) 0.3928(5) 0.5972(3) 0.0464(16) Uani 1 1 d . . . H67A H 0.6208 0.3682 0.5529 0.056 Uiso 1 1 calc R . . C68 C 0.6300(2) 0.3994(4) 0.6496(3) 0.0420(14) Uani 1 1 d . . . H68A H 0.5998 0.3806 0.6411 0.050 Uiso 1 1 calc R . . C69 C 0.6617(2) 0.4342(4) 0.7171(3) 0.0367(12) Uani 1 1 d . . . C70 C 0.7002(3) 0.4129(4) 0.5490(4) 0.0463(15) Uani 1 1 d . . . H70A H 0.7303 0.4344 0.5595 0.056 Uiso 1 1 calc R . . C71 C 0.6746(3) 0.3787(5) 0.4846(3) 0.0483(16) Uani 1 1 d . . . H71A H 0.6429 0.3638 0.4711 0.058 Uiso 1 1 calc R . . C72 C 0.6812(2) 0.2987(5) 0.3244(3) 0.0464(13) Uani 1 1 d . . . H72A H 0.6614 0.2687 0.2820 0.056 Uiso 1 1 calc R . . C73 C 0.6643(2) 0.3157(4) 0.3711(3) 0.0488(17) Uani 1 1 d . . . H73A H 0.6341 0.2959 0.3618 0.059 Uiso 1 1 calc R . . C74 C 0.6919(2) 0.3626(4) 0.4332(3) 0.0465(16) Uani 1 1 d . . . C75 C 0.7356(2) 0.3894(5) 0.4425(3) 0.0482(16) Uani 1 1 d . . . H75A H 0.7552 0.4227 0.4827 0.058 Uiso 1 1 calc R . . C76 C 0.7506(2) 0.3677(4) 0.3933(3) 0.0456(15) Uani 1 1 d . . . H76A H 0.7808 0.3859 0.4012 0.055 Uiso 1 1 calc R . . O101 O -0.20615(18) 1.4318(3) -0.6994(3) 0.0585(13) Uiso 1 1 d . . . O102 O -0.2490(7) 1.5690(11) -0.7119(10) 0.254(8) Uiso 1 1 d D . . O103 O 0.1459(4) 0.6103(8) 0.0750(6) 0.150(4) Uiso 1 1 d . . . O104 O 0.5000 0.359(2) 0.5000 0.308(15) Uiso 1 2 d S . . O105 O 0.5000 0.806(2) 0.5000 0.289(13) Uiso 1 2 d S . . O106 O 0.5636(7) 0.1837(14) 0.3158(11) 0.260(8) Uiso 1 1 d . . . O107 O 0.3863(7) 0.9427(12) 0.3108(10) 0.125(6) Uiso 0.50 1 d P . . O108 O 0.5830(7) 0.2447(12) 0.4441(10) 0.245(8) Uiso 1 1 d . . . O109 O 0.4821(11) 0.107(2) 0.2264(17) 0.196(11) Uiso 0.50 1 d P . . N5 N -0.1767(4) 1.5775(6) -1.3626(5) 0.090(2) Uiso 1 1 d . . . O6 O -0.2177(8) 1.5684(14) -1.3891(11) 0.255(8) Uiso 1 1 d . . . O7 O -0.1498(6) 1.5740(10) -1.3863(9) 0.203(6) Uiso 1 1 d . . . O8 O -0.1567(5) 1.6037(9) -1.3006(8) 0.175(5) Uiso 1 1 d . . . N6 N 0.1668(6) 0.5333(12) -0.0596(12) 0.171(6) Uiso 1 1 d D . . O9 O 0.1753(5) 0.5313(9) -0.0036(8) 0.176(5) Uiso 1 1 d D . . O10 O 0.1168(8) 0.546(2) -0.0969(12) 0.364(15) Uiso 1 1 d D . . O11 O 0.1750(7) 0.5404(13) -0.1065(11) 0.238(8) Uiso 1 1 d . . . O12 O 0.0625(4) 1.3092(8) -0.3036(6) 0.149(4) Uiso 1 1 d . . . N7 N 0.0428(3) 1.2113(5) -0.2492(5) 0.081(2) Uiso 1 1 d . . . C77 C -0.0081(5) 1.2176(11) -0.2866(9) 0.135(5) Uiso 1 1 d . . . H77A H -0.0177 1.2602 -0.3237 0.203 Uiso 1 1 calc R . . H77B H -0.0193 1.2323 -0.2525 0.203 Uiso 1 1 calc R . . H77C H -0.0217 1.1645 -0.3090 0.203 Uiso 1 1 calc R . . C78 C 0.0629(5) 1.1524(9) -0.1938(8) 0.120(4) Uiso 1 1 d . . . H78A H 0.0975 1.1535 -0.1730 0.180 Uiso 1 1 calc R . . H78B H 0.0511 1.0974 -0.2134 0.180 Uiso 1 1 calc R . . H78C H 0.0542 1.1653 -0.1566 0.180 Uiso 1 1 calc R . . C79 C 0.0754(6) 1.2554(10) -0.2606(8) 0.121(4) Uiso 1 1 d . . . H79A H 0.1082 1.2426 -0.2339 0.145 Uiso 1 1 calc R . . O13 O 0.5624(7) 0.2080(12) 0.9810(10) 0.249(7) Uiso 1 1 d . . . N8 N 0.4792(6) 0.1836(11) 0.8921(9) 0.164(5) Uiso 1 1 d . . . C80 C 0.5281(13) 0.164(2) 0.9379(19) 0.275(14) Uiso 1 1 d D . . C81 C 0.4794(11) 0.268(2) 0.9010(17) 0.302(15) Uiso 1 1 d D . . H81A H 0.5116 0.2861 0.9343 0.453 Uiso 1 1 calc R . . H81B H 0.4581 0.2820 0.9204 0.453 Uiso 1 1 calc R . . H81C H 0.4686 0.2950 0.8545 0.453 Uiso 1 1 calc R . . C82 C 0.4580(9) 0.0969(17) 0.8643(13) 0.212(10) Uiso 1 1 d . . . H82A H 0.4826 0.0549 0.8877 0.318 Uiso 1 1 calc R . . H82B H 0.4458 0.0943 0.8123 0.318 Uiso 1 1 calc R . . H82C H 0.4321 0.0866 0.8753 0.318 Uiso 1 1 calc R . . O14 O -0.2348(3) 1.6908(6) -0.7783(5) 0.121(3) Uiso 1 1 d D . . C83 C -0.2291(7) 1.7595(14) -0.8121(11) 0.169(7) Uiso 1 1 d . . . O15 O 0.0204(7) 0.3832(12) -0.0063(12) 0.249(8) Uiso 1 1 d . . . C84 C 0.0020(7) 0.3837(12) -0.0765(11) 0.155(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0408(3) 0.0486(4) 0.0280(3) 0.0062(3) 0.0189(3) 0.0162(3) O1 0.039(2) 0.051(3) 0.043(2) 0.007(2) 0.011(2) 0.011(2) O2 0.062(3) 0.046(3) 0.043(2) 0.014(2) 0.035(2) 0.010(2) O3 0.049(2) 0.052(3) 0.046(2) 0.019(2) 0.018(2) 0.014(2) O4 0.059(3) 0.049(3) 0.039(2) 0.001(2) 0.030(2) 0.005(2) O5 0.060(3) 0.044(3) 0.055(3) -0.005(2) 0.033(2) 0.001(2) N1 0.039(2) 0.041(3) 0.033(2) 0.005(2) 0.017(2) 0.009(2) N2 0.037(3) 0.046(3) 0.034(3) 0.007(2) 0.019(2) 0.013(2) N3 0.047(3) 0.050(3) 0.030(3) 0.005(2) 0.021(2) 0.011(2) N4 0.043(3) 0.054(3) 0.029(2) 0.007(2) 0.019(2) 0.014(2) C1 0.056(4) 0.032(3) 0.042(3) 0.003(3) 0.034(3) 0.004(3) C2 0.055(4) 0.037(3) 0.047(3) 0.007(3) 0.033(3) 0.013(3) C3 0.049(3) 0.043(3) 0.035(3) 0.003(2) 0.026(3) 0.004(3) C4 0.049(4) 0.036(3) 0.036(3) 0.008(2) 0.024(3) 0.008(3) C5 0.051(4) 0.032(3) 0.037(3) 0.002(2) 0.018(3) 0.012(3) C6 0.058(4) 0.039(3) 0.044(3) 0.004(3) 0.034(3) 0.014(3) C7 0.051(3) 0.050(4) 0.040(3) 0.003(3) 0.031(3) 0.007(3) C8 0.053(3) 0.043(3) 0.042(3) 0.002(3) 0.034(3) 0.008(3) C9 0.046(3) 0.038(3) 0.052(4) 0.005(3) 0.033(3) 0.009(3) C10 0.040(3) 0.036(3) 0.039(3) 0.002(2) 0.024(3) 0.003(2) C11 0.055(4) 0.032(3) 0.063(4) 0.011(3) 0.037(3) 0.010(3) C12 0.061(4) 0.038(3) 0.048(4) 0.016(3) 0.034(3) 0.009(3) C13 0.041(3) 0.039(3) 0.040(3) 0.005(2) 0.023(3) 0.003(2) C14 0.038(3) 0.040(3) 0.037(3) 0.008(2) 0.021(3) 0.008(2) C15 0.040(3) 0.034(3) 0.036(3) 0.006(2) 0.024(3) 0.005(2) C16 0.052(4) 0.036(3) 0.046(4) 0.008(3) 0.033(3) 0.010(3) C17 0.072(5) 0.030(3) 0.063(4) 0.011(3) 0.050(4) 0.009(3) C18 0.075(6) 0.067(6) 0.070(6) 0.007(5) -0.005(5) 0.021(5) C19 0.055(4) 0.067(5) 0.044(4) 0.006(4) -0.001(3) 0.005(4) C20 0.125(8) 0.089(7) 0.046(4) 0.014(4) 0.048(5) 0.020(6) C21 0.084(6) 0.077(5) 0.048(4) 0.021(4) 0.042(4) 0.026(5) C22 0.041(3) 0.039(3) 0.029(3) 0.008(2) 0.022(3) 0.007(3) C23 0.044(3) 0.045(3) 0.034(3) 0.009(3) 0.019(3) 0.011(3) C24 0.041(3) 0.042(3) 0.037(3) -0.002(3) 0.017(3) 0.000(3) C25 0.055(4) 0.040(3) 0.040(3) 0.000(3) 0.028(3) 0.008(3) C26 0.044(3) 0.038(3) 0.038(3) 0.003(2) 0.024(3) 0.007(3) C27 0.053(4) 0.038(3) 0.043(3) 0.005(3) 0.026(3) 0.015(3) C28 0.046(4) 0.046(3) 0.038(3) 0.012(3) 0.023(3) 0.018(3) C29 0.047(4) 0.051(4) 0.029(3) 0.003(3) 0.019(3) 0.009(3) C30 0.039(3) 0.043(3) 0.031(3) 0.005(2) 0.020(2) 0.009(3) C31 0.037(3) 0.040(3) 0.031(3) 0.008(2) 0.022(2) 0.010(2) C32 0.051(4) 0.054(4) 0.048(4) 0.006(3) 0.022(3) 0.014(3) C33 0.043(3) 0.039(3) 0.052(4) -0.001(3) 0.024(3) 0.008(3) C34 0.048(3) 0.042(3) 0.035(3) 0.008(2) 0.016(3) 0.020(3) C35 0.050(4) 0.053(4) 0.034(3) -0.001(3) 0.011(3) 0.000(3) C36 0.041(3) 0.046(3) 0.048(4) 0.005(3) 0.028(3) 0.010(3) C37 0.051(4) 0.040(3) 0.045(4) 0.007(3) 0.027(3) 0.014(3) C38 0.046(4) 0.046(4) 0.042(3) -0.007(3) 0.021(3) -0.002(3) C39 0.049(4) 0.046(4) 0.039(3) 0.002(3) 0.020(3) 0.005(3) C40 0.059(4) 0.040(3) 0.038(3) 0.005(3) 0.020(3) 0.007(3) C41 0.051(4) 0.057(4) 0.035(3) 0.003(3) 0.023(3) 0.020(3) C42 0.043(4) 0.080(5) 0.051(4) 0.016(4) 0.025(3) 0.008(4) C43 0.044(4) 0.056(4) 0.049(4) 0.010(3) 0.024(3) 0.006(3) C44 0.046(4) 0.061(4) 0.040(3) 0.006(3) 0.020(3) 0.014(3) C45 0.046(4) 0.071(5) 0.046(4) 0.007(4) 0.021(3) 0.013(4) C46 0.038(3) 0.062(4) 0.050(4) 0.015(3) 0.020(3) 0.026(3) C47 0.043(3) 0.061(4) 0.050(4) 0.009(3) 0.025(3) 0.009(3) C48 0.041(3) 0.049(4) 0.042(3) 0.007(3) 0.023(3) 0.010(3) C49 0.044(4) 0.063(4) 0.047(4) 0.005(3) 0.024(3) -0.003(3) C50 0.053(4) 0.044(3) 0.059(4) 0.020(3) 0.034(3) 0.013(3) C51 0.047(3) 0.045(3) 0.036(3) 0.009(3) 0.022(3) 0.018(3) C52 0.039(3) 0.040(3) 0.040(3) 0.005(3) 0.023(3) 0.012(3) C53 0.043(3) 0.047(3) 0.034(3) 0.008(3) 0.023(3) 0.013(3) C54 0.047(4) 0.050(4) 0.043(3) 0.013(3) 0.027(3) 0.016(3) C55 0.056(4) 0.051(4) 0.047(4) 0.015(3) 0.032(3) 0.015(3) C56 0.063(5) 0.057(5) 0.066(5) 0.025(4) 0.021(4) 0.000(4) C57 0.074(5) 0.063(5) 0.050(4) 0.027(4) 0.006(4) -0.002(4) C58 0.109(7) 0.088(6) 0.046(4) 0.018(4) 0.049(5) 0.034(6) C59 0.072(5) 0.069(5) 0.033(3) 0.006(3) 0.026(3) 0.010(4) C60 0.042(3) 0.033(3) 0.034(3) 0.007(2) 0.023(3) 0.012(2) C61 0.046(3) 0.033(3) 0.035(3) 0.007(2) 0.020(3) 0.012(3) C62 0.056(4) 0.032(3) 0.036(3) 0.000(2) 0.021(3) 0.005(3) C63 0.041(3) 0.040(3) 0.050(4) 0.002(3) 0.027(3) 0.000(3) C64 0.047(3) 0.034(3) 0.040(3) 0.007(2) 0.026(3) 0.012(3) C65 0.049(4) 0.043(3) 0.047(4) 0.005(3) 0.030(3) 0.005(3) C66 0.056(4) 0.047(4) 0.041(3) 0.003(3) 0.030(3) 0.011(3) C67 0.045(4) 0.061(4) 0.034(3) -0.002(3) 0.020(3) 0.011(3) C68 0.049(4) 0.046(4) 0.034(3) 0.006(3) 0.022(3) 0.011(3) C69 0.042(3) 0.036(3) 0.035(3) 0.009(2) 0.021(3) 0.014(2) C70 0.053(4) 0.047(4) 0.045(4) 0.004(3) 0.028(3) 0.006(3) C71 0.054(4) 0.063(4) 0.038(3) 0.007(3) 0.029(3) 0.017(3) C72 0.045(3) 0.057(4) 0.039(3) 0.005(4) 0.021(2) 0.006(4) C73 0.045(3) 0.064(5) 0.044(3) -0.001(3) 0.026(3) 0.008(3) C74 0.052(4) 0.056(4) 0.036(3) 0.014(3) 0.025(3) 0.020(3) C75 0.050(4) 0.064(4) 0.036(3) -0.001(3) 0.025(3) 0.007(3) C76 0.045(3) 0.063(4) 0.031(3) 0.004(3) 0.019(3) 0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N3 2.014(5) . ? Cu1 N2 2.022(5) 3_455 ? Cu1 N4 2.031(5) 3_455 ? Cu1 N1 2.035(5) . ? Cu1 O5 2.420(5) . ? O1 C23 1.362(7) . ? O1 C19 1.429(9) . ? O2 C13 1.368(7) . ? O2 C21 1.403(8) . ? O3 C51 1.357(7) . ? O3 C56 1.454(8) . ? O4 C61 1.376(7) . ? O4 C59 1.434(8) . ? N1 C1 1.333(8) . ? N1 C5 1.353(8) . ? N2 C38 1.320(8) . ? N2 C34 1.345(8) . ? N2 Cu1 2.021(5) 3_545 ? N3 C43 1.327(9) . ? N3 C39 1.336(8) . ? N4 C72 1.336(8) . ? N4 C76 1.345(8) . ? N4 Cu1 2.031(5) 3_545 ? C1 C2 1.380(8) . ? C2 C3 1.403(9) . ? C3 C4 1.389(9) . ? C3 C6 1.479(8) . ? C4 C5 1.369(9) . ? C6 C7 1.342(9) . ? C7 C8 1.479(7) . ? C8 C9 1.350(9) . ? C8 C17 1.425(9) . ? C9 C10 1.420(9) . ? C10 C15 1.425(8) . ? C10 C11 1.437(8) . ? C11 C12 1.360(9) . ? C12 C13 1.413(9) . ? C13 C14 1.395(8) . ? C14 C15 1.432(8) . ? C14 C22 1.503(8) . ? C15 C16 1.419(8) . ? C16 C17 1.361(9) . ? C18 C19 1.477(11) . ? C20 C21 1.493(11) . ? C22 C23 1.377(9) . ? C22 C31 1.432(8) . ? C23 C24 1.438(9) . ? C24 C25 1.335(9) . ? C25 C26 1.406(9) . ? C26 C27 1.425(9) . ? C26 C31 1.440(8) . ? C27 C28 1.380(9) . ? C28 C29 1.436(9) . ? C28 C32 1.447(9) . ? C29 C30 1.397(8) . ? C30 C31 1.410(8) . ? C32 C33 1.307(10) . ? C33 C36 1.476(9) . ? C34 C35 1.385(9) . ? C35 C36 1.411(10) . ? C36 C37 1.401(9) . ? C37 C38 1.361(9) . ? C39 C40 1.418(9) . ? C40 C41 1.357(10) . ? C41 C42 1.400(10) . ? C41 C44 1.472(9) . ? C42 C43 1.369(10) . ? C44 C45 1.299(10) . ? C45 C46 1.475(9) . ? C46 C55 1.381(10) . ? C46 C47 1.407(10) . ? C47 C48 1.404(9) . ? C48 C49 1.423(9) . ? C48 C53 1.437(9) . ? C49 C50 1.369(10) . ? C50 C51 1.419(9) . ? C51 C52 1.396(9) . ? C52 C53 1.414(8) . ? C52 C60 1.490(8) . ? C53 C54 1.422(9) . ? C54 C55 1.381(9) . ? C56 C57 1.499(11) . ? C58 C59 1.460(11) . ? C60 C61 1.366(9) . ? C60 C69 1.433(8) . ? C61 C62 1.413(9) . ? C62 C63 1.351(9) . ? C63 C64 1.410(9) . ? C64 C65 1.411(8) . ? C64 C69 1.439(9) . ? C65 C66 1.376(9) . ? C66 C67 1.402(10) . ? C66 C70 1.466(9) . ? C67 C68 1.358(9) . ? C68 C69 1.419(9) . ? C70 C71 1.333(10) . ? C71 C74 1.465(9) . ? C72 C73 1.366(8) . ? C73 C74 1.409(10) . ? C74 C75 1.391(10) . ? C75 C76 1.389(9) . ? N5 O6 1.17(2) . ? N5 O7 1.190(17) . ? N5 O8 1.232(15) . ? N6 O9 1.09(2) . ? N6 O11 1.15(2) . ? N6 O10 1.430(16) . ? O12 C79 1.186(16) . ? N7 C79 1.383(16) . ? N7 C78 1.408(15) . ? N7 C77 1.441(16) . ? O13 C80 1.26(4) . ? N8 C81 1.38(3) . ? N8 C82 1.55(3) . ? N8 C80 1.43(3) . ? O14 C83 1.38(2) . ? O15 C84 1.31(2) . ? O15 O15 1.46(3) 2 ? 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 N3 Cu1 N2 178.8(2) . 3_455 ? N3 Cu1 N4 90.5(2) . 3_455 ? N2 Cu1 N4 88.85(19) 3_455 3_455 ? N3 Cu1 N1 90.2(2) . . ? N2 Cu1 N1 90.34(19) 3_455 . ? N4 Cu1 N1 173.6(2) 3_455 . ? N3 Cu1 O5 90.7(2) . . ? N2 Cu1 O5 90.3(2) 3_455 . ? N4 Cu1 O5 92.6(2) 3_455 . ? N1 Cu1 O5 93.76(19) . . ? C23 O1 C19 119.0(5) . . ? C13 O2 C21 117.2(5) . . ? C51 O3 C56 118.6(5) . . ? C61 O4 C59 118.3(5) . . ? C1 N1 C5 117.4(5) . . ? C1 N1 Cu1 121.2(4) . . ? C5 N1 Cu1 121.4(4) . . ? C38 N2 C34 118.4(5) . . ? C38 N2 Cu1 120.4(4) . 3_545 ? C34 N2 Cu1 121.2(4) . 3_545 ? C43 N3 C39 118.3(6) . . ? C43 N3 Cu1 121.3(4) . . ? C39 N3 Cu1 120.4(5) . . ? C72 N4 C76 117.5(5) . . ? C72 N4 Cu1 121.7(4) . 3_545 ? C76 N4 Cu1 120.6(4) . 3_545 ? N1 C1 C2 122.5(6) . . ? C1 C2 C3 120.1(6) . . ? C4 C3 C2 116.8(5) . . ? C4 C3 C6 124.6(5) . . ? C2 C3 C6 118.6(5) . . ? C5 C4 C3 119.6(6) . . ? N1 C5 C4 123.4(5) . . ? C7 C6 C3 125.0(6) . . ? C6 C7 C8 124.5(6) . . ? C9 C8 C17 117.9(5) . . ? C9 C8 C7 120.7(6) . . ? C17 C8 C7 121.3(6) . . ? C8 C9 C10 122.8(6) . . ? C9 C10 C15 119.1(5) . . ? C9 C10 C11 122.5(6) . . ? C15 C10 C11 118.4(5) . . ? C12 C11 C10 120.5(6) . . ? C11 C12 C13 121.3(6) . . ? O2 C13 C14 115.8(5) . . ? O2 C13 C12 123.3(5) . . ? C14 C13 C12 120.8(5) . . ? C13 C14 C15 118.6(5) . . ? C13 C14 C22 120.4(5) . . ? C15 C14 C22 120.9(5) . . ? C16 C15 C10 117.1(5) . . ? C16 C15 C14 122.5(5) . . ? C10 C15 C14 120.4(5) . . ? C17 C16 C15 121.8(6) . . ? C16 C17 C8 121.1(6) . . ? O1 C19 C18 108.2(7) . . ? O2 C21 C20 108.3(7) . . ? C23 C22 C31 119.5(6) . . ? C23 C22 C14 120.0(5) . . ? C31 C22 C14 120.5(5) . . ? O1 C23 C22 117.3(6) . . ? O1 C23 C24 121.8(6) . . ? C22 C23 C24 120.9(6) . . ? C25 C24 C23 119.6(6) . . ? C24 C25 C26 122.5(6) . . ? C25 C26 C27 121.9(6) . . ? C25 C26 C31 118.8(5) . . ? C27 C26 C31 119.3(6) . . ? C28 C27 C26 121.8(6) . . ? C27 C28 C29 118.1(6) . . ? C27 C28 C32 119.0(6) . . ? C29 C28 C32 122.8(6) . . ? C30 C29 C28 121.4(6) . . ? C29 C30 C31 120.4(6) . . ? C30 C31 C22 122.5(5) . . ? C30 C31 C26 118.8(5) . . ? C22 C31 C26 118.7(6) . . ? C33 C32 C28 125.1(7) . . ? C32 C33 C36 125.5(6) . . ? N2 C34 C35 121.1(6) . . ? C34 C35 C36 120.3(6) . . ? C37 C36 C35 116.5(6) . . ? C37 C36 C33 119.1(6) . . ? C35 C36 C33 124.3(6) . . ? C38 C37 C36 118.8(6) . . ? N2 C38 C37 124.8(6) . . ? N3 C39 C40 120.7(6) . . ? C41 C40 C39 120.8(6) . . ? C40 C41 C42 116.9(6) . . ? C40 C41 C44 124.9(7) . . ? C42 C41 C44 118.2(7) . . ? C43 C42 C41 119.6(7) . . ? N3 C43 C42 123.6(7) . . ? C45 C44 C41 126.4(7) . . ? C44 C45 C46 125.5(7) . . ? C55 C46 C47 118.4(6) . . ? C55 C46 C45 123.3(7) . . ? C47 C46 C45 118.3(7) . . ? C48 C47 C46 120.7(6) . . ? C47 C48 C49 120.6(6) . . ? C47 C48 C53 120.5(6) . . ? C49 C48 C53 118.8(6) . . ? C50 C49 C48 120.0(6) . . ? C49 C50 C51 120.9(6) . . ? O3 C51 C52 116.1(6) . . ? O3 C51 C50 122.4(6) . . ? C52 C51 C50 121.4(6) . . ? C51 C52 C53 118.1(6) . . ? C51 C52 C60 120.1(5) . . ? C53 C52 C60 121.8(5) . . ? C52 C53 C54 122.2(6) . . ? C52 C53 C48 120.8(6) . . ? C54 C53 C48 117.0(6) . . ? C55 C54 C53 120.7(6) . . ? C54 C55 C46 122.7(6) . . ? O3 C56 C57 108.4(6) . . ? O4 C59 C58 109.0(7) . . ? C61 C60 C69 118.8(6) . . ? C61 C60 C52 121.4(5) . . ? C69 C60 C52 119.8(5) . . ? C60 C61 O4 117.1(5) . . ? C60 C61 C62 121.9(5) . . ? O4 C61 C62 121.0(5) . . ? C63 C62 C61 119.8(6) . . ? C62 C63 C64 121.9(6) . . ? C63 C64 C65 122.6(6) . . ? C63 C64 C69 118.1(5) . . ? C65 C64 C69 119.2(6) . . ? C66 C65 C64 122.1(6) . . ? C65 C66 C67 117.4(6) . . ? C65 C66 C70 118.8(6) . . ? C67 C66 C70 123.6(6) . . ? C68 C67 C66 123.3(6) . . ? C67 C68 C69 120.4(6) . . ? C68 C69 C60 123.2(6) . . ? C68 C69 C64 117.5(5) . . ? C60 C69 C64 119.3(5) . . ? C71 C70 C66 126.1(7) . . ? C70 C71 C74 124.7(7) . . ? N4 C72 C73 123.8(6) . . ? C72 C73 C74 119.7(6) . . ? C75 C74 C73 116.3(6) . . ? C75 C74 C71 123.7(7) . . ? C73 C74 C71 120.0(6) . . ? C74 C75 C76 120.3(7) . . ? N4 C76 C75 122.3(6) . . ? O6 N5 O7 132.1(17) . . ? O6 N5 O8 116.6(16) . . ? O7 N5 O8 110.8(14) . . ? O9 N6 O11 155(2) . . ? O9 N6 O10 103.8(18) . . ? O11 N6 O10 100(2) . . ? C79 N7 C78 114.4(11) . . ? C79 N7 C77 128.5(12) . . ? C78 N7 C77 117.1(11) . . ? O12 C79 N7 120.0(15) . . ? C81 N8 C82 157(2) . . ? C81 N8 C80 101(2) . . ? C82 N8 C80 102(2) . . ? O13 C80 N8 132(3) . . ? C84 O15 O15 104(2) . 2 ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.63 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.305 _refine_diff_density_min -0.600 _refine_diff_density_rms 0.122 # Attachment 'new4.cif' data_new4 _database_code_depnum_ccdc_archive 'CCDC 607392' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C83.50 H90.50 Cd Cl2 N5.50 O18.50' _chemical_formula_weight 1650.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 42.00(13) _cell_length_b 12.93(3) _cell_length_c 19.36(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.80(6) _cell_angle_gamma 90.00 _cell_volume 10163(47) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.02 _cell_measurement_theta_max 23.27 _exptl_crystal_description Bloc _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.079 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3440 _exptl_absorpt_coefficient_mu 0.325 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.5181 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 27368 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0641 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 23.27 _reflns_number_total 13601 _reflns_number_gt 9319 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0824P)^2^+78.6893P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00036(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(5) _refine_ls_number_reflns 13601 _refine_ls_number_parameters 924 _refine_ls_number_restraints 36 _refine_ls_R_factor_ref 0.1396 _refine_ls_R_factor_gt 0.1055 _refine_ls_wR_factor_ref 0.2625 _refine_ls_wR_factor_gt 0.2420 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.63809(2) 0.37543(11) -0.10407(4) 0.0825(3) Uani 1 1 d . . . O1 O 0.4322(3) 0.9733(9) 0.3046(5) 0.118(4) Uani 1 1 d . . . O2 O 0.4839(4) 1.1198(9) 0.2919(6) 0.141(4) Uani 1 1 d . . . O3 O 0.8197(3) -0.3141(7) 0.4795(5) 0.114(3) Uani 1 1 d . . . O4 O 0.8646(2) -0.1347(12) 0.5442(5) 0.117(3) Uani 1 1 d . . . O5 O 0.5942(3) 0.2566(9) -0.1155(6) 0.123(4) Uani 1 1 d . . . O6 O 0.6832(3) 0.4948(9) -0.0905(6) 0.127(4) Uani 1 1 d D . . N1 N 0.6149(3) 0.4873(11) -0.0364(6) 0.097(4) Uani 1 1 d . . . N2 N 0.6100(3) 0.4623(9) 0.7928(6) 0.080(3) Uani 1 1 d . . . N3 N 0.6641(3) 0.2720(9) 0.8278(5) 0.081(3) Uani 1 1 d . . . N4 N 0.6662(3) 0.2928(11) -0.0005(5) 0.096(3) Uani 1 1 d . . . C1 C 0.5836(4) 0.4938(14) -0.0470(9) 0.115(5) Uani 1 1 d . . . H1A H 0.5701 0.4572 -0.0863 0.139 Uiso 1 1 calc R . . C2 C 0.5683(4) 0.5515(16) -0.0042(10) 0.124(6) Uani 1 1 d . . . H2A H 0.5451 0.5481 -0.0120 0.149 Uiso 1 1 calc R . . C3 C 0.5865(4) 0.6134(12) 0.0493(8) 0.098(4) Uani 1 1 d . . . C4 C 0.6203(5) 0.6080(18) 0.0580(11) 0.156(8) Uani 1 1 d . . . H4A H 0.6341 0.6480 0.0950 0.187 Uiso 1 1 calc R . . C5 C 0.6344(6) 0.550(2) 0.0178(15) 0.173(10) Uani 1 1 d . . . H5A H 0.6576 0.5508 0.0253 0.207 Uiso 1 1 calc R . . C6 C 0.5713(5) 0.6744(14) 0.0955(7) 0.109(5) Uani 1 1 d . . . H6A H 0.5859 0.7089 0.1342 0.131 Uiso 1 1 calc R . . C7 C 0.5403(5) 0.6871(13) 0.0899(7) 0.105(5) Uani 1 1 d . . . H7A H 0.5254 0.6510 0.0525 0.127 Uiso 1 1 calc R . . C8 C 0.5260(4) 0.7522(12) 0.1362(8) 0.098(4) Uani 1 1 d . . . C9 C 0.4925(5) 0.7565(13) 0.1224(7) 0.108(5) Uani 1 1 d . . . H9A H 0.4797 0.7219 0.0814 0.130 Uiso 1 1 calc R . . C10 C 0.4760(5) 0.8106(10) 0.1667(7) 0.095(4) Uani 1 1 d . . . C11 C 0.4408(5) 0.8185(12) 0.1500(9) 0.109(5) Uani 1 1 d . . . H11A H 0.4279 0.7894 0.1069 0.131 Uiso 1 1 calc R . . C12 C 0.4260(4) 0.8667(17) 0.1951(7) 0.114(5) Uani 1 1 d . . . H12A H 0.4026 0.8685 0.1856 0.137 Uiso 1 1 calc R . . C13 C 0.4455(4) 0.9138(11) 0.2560(8) 0.102(5) Uani 1 1 d . . . C14 C 0.4794(4) 0.9111(8) 0.2764(7) 0.080(4) Uani 1 1 d . . . C15 C 0.4957(4) 0.8638(17) 0.2295(7) 0.110(5) Uani 1 1 d . . . C16 C 0.5299(4) 0.8508(10) 0.2431(7) 0.089(4) Uani 1 1 d . . . H16A H 0.5432 0.8785 0.2863 0.107 Uiso 1 1 calc R . . C17 C 0.5451(4) 0.8016(12) 0.1988(8) 0.099(4) Uani 1 1 d . . . H17A H 0.5685 0.8001 0.2095 0.119 Uiso 1 1 calc R . . C18 C 0.4043(5) 1.0360(14) 0.2733(9) 0.125(6) Uani 1 1 d . . . H18A H 0.3841 0.9932 0.2605 0.150 Uiso 1 1 calc R . . H18B H 0.4072 1.0700 0.2295 0.150 Uiso 1 1 calc R . . C19 C 0.4017(5) 1.1125(17) 0.3258(12) 0.151(7) Uani 1 1 d . . . H19A H 0.3829 1.1579 0.3060 0.227 Uiso 1 1 calc R . . H19B H 0.4219 1.1538 0.3385 0.227 Uiso 1 1 calc R . . H19C H 0.3985 1.0779 0.3686 0.227 Uiso 1 1 calc R . . C20 C 0.4747(11) 1.262(4) 0.2189(16) 0.35(2) Uiso 1 1 d D . . H20A H 0.4713 1.3372 0.2193 0.526 Uiso 1 1 calc R . . H20B H 0.4534 1.2275 0.2018 0.526 Uiso 1 1 calc R . . H20C H 0.4888 1.2456 0.1871 0.526 Uiso 1 1 calc R . . C21 C 0.4904(9) 1.227(2) 0.2906(15) 0.265(19) Uani 1 1 d D . . H21A H 0.5144 1.2398 0.3020 0.318 Uiso 1 1 calc R . . H21B H 0.4812 1.2640 0.3260 0.318 Uiso 1 1 calc R . . C22 C 0.5000(4) 0.9600(11) 0.3446(7) 0.086(4) Uani 1 1 d . . . C23 C 0.5014(4) 1.0640(13) 0.3490(8) 0.108(5) Uani 1 1 d . . . C24 C 0.5196(4) 1.1138(13) 0.4127(10) 0.114(5) Uani 1 1 d . . . H24A H 0.5211 1.1871 0.4149 0.136 Uiso 1 1 calc R . . C25 C 0.5338(5) 1.0597(15) 0.4665(10) 0.114(6) Uani 1 1 d . . . H25A H 0.5442 1.0941 0.5097 0.136 Uiso 1 1 calc R . . C26 C 0.5349(4) 0.9481(12) 0.4645(8) 0.085(4) Uani 1 1 d . . . C27 C 0.5510(3) 0.8895(13) 0.5248(6) 0.087(4) Uani 1 1 d . . . H27A H 0.5627 0.9247 0.5666 0.104 Uiso 1 1 calc R . . C28 C 0.5503(4) 0.7835(14) 0.5251(7) 0.095(4) Uani 1 1 d . . . C29 C 0.5320(4) 0.7323(11) 0.4594(8) 0.078(4) Uani 1 1 d . . . H29A H 0.5318 0.6589 0.4570 0.094 Uiso 1 1 calc R . . C30 C 0.5151(3) 0.7889(12) 0.4007(7) 0.078(4) Uani 1 1 d . . . H30A H 0.5025 0.7549 0.3590 0.094 Uiso 1 1 calc R . . C31 C 0.5168(3) 0.8993(11) 0.4038(7) 0.079(4) Uani 1 1 d . . . C32 C 0.5655(4) 0.7241(13) 0.5888(6) 0.094(4) Uani 1 1 d . . . H32A H 0.5786 0.7630 0.6273 0.113 Uiso 1 1 calc R . . C33 C 0.5636(3) 0.6242(12) 0.6010(7) 0.087(4) Uani 1 1 d . . . H33A H 0.5511 0.5826 0.5634 0.104 Uiso 1 1 calc R . . C34 C 0.6113(4) 0.5658(12) 0.7886(6) 0.094(4) Uani 1 1 d . . . H34A H 0.6230 0.6029 0.8296 0.113 Uiso 1 1 calc R . . C35 C 0.5967(4) 0.6211(11) 0.7280(7) 0.091(4) Uani 1 1 d . . . H35A H 0.5988 0.6942 0.7286 0.110 Uiso 1 1 calc R . . C36 C 0.5793(3) 0.5737(11) 0.6671(6) 0.072(3) Uani 1 1 d . . . C37 C 0.5769(3) 0.4660(13) 0.6720(6) 0.088(4) Uani 1 1 d . . . H37A H 0.5641 0.4286 0.6322 0.106 Uiso 1 1 calc R . . C38 C 0.5927(3) 0.4121(10) 0.7335(6) 0.082(4) Uani 1 1 d . . . H38A H 0.5913 0.3388 0.7339 0.099 Uiso 1 1 calc R . . C39 C 0.6699(3) 0.1706(12) 0.8354(7) 0.092(4) Uani 1 1 d . . . H39A H 0.6621 0.1380 0.8720 0.111 Uiso 1 1 calc R . . C40 C 0.6854(3) 0.1072(12) 0.7977(8) 0.097(5) Uani 1 1 d . . . H40A H 0.6871 0.0346 0.8053 0.116 Uiso 1 1 calc R . . C41 C 0.6990(4) 0.1597(13) 0.7450(8) 0.096(4) Uani 1 1 d . . . C42 C 0.6924(4) 0.2676(14) 0.7359(8) 0.121(6) Uani 1 1 d . . . H42A H 0.6996 0.3046 0.7002 0.145 Uiso 1 1 calc R . . C43 C 0.6754(4) 0.3199(11) 0.7790(7) 0.100(4) Uani 1 1 d . . . H43A H 0.6720 0.3923 0.7728 0.120 Uiso 1 1 calc R . . C44 C 0.7184(5) 0.1105(15) 0.7017(13) 0.165(11) Uani 1 1 d . . . H44A H 0.7263 0.1570 0.6719 0.198 Uiso 1 1 calc R . . C45 C 0.7260(5) 0.026(2) 0.6970(10) 0.140(7) Uani 1 1 d . . . H45A H 0.7196 -0.0206 0.7291 0.168 Uiso 1 1 calc R . . C46 C 0.7450(4) -0.024(2) 0.6466(7) 0.124(7) Uani 1 1 d . . . C47 C 0.7488(5) -0.126(2) 0.6462(10) 0.156(8) Uani 1 1 d . . . H47A H 0.7390 -0.1681 0.6755 0.187 Uiso 1 1 calc R . . C48 C 0.7661(4) -0.1709(15) 0.6057(7) 0.113(6) Uani 1 1 d . . . C49 C 0.7707(8) -0.2796(19) 0.6058(13) 0.182(12) Uani 1 1 d . . . H49A H 0.7608 -0.3196 0.6357 0.218 Uiso 1 1 calc R . . C50 C 0.7884(6) -0.3318(14) 0.5661(10) 0.156(9) Uani 1 1 d . . . H50A H 0.7909 -0.4048 0.5683 0.187 Uiso 1 1 calc R . . C51 C 0.8025(4) -0.2697(13) 0.5221(7) 0.102(5) Uani 1 1 d . . . C52 C 0.7984(3) -0.1649(11) 0.5175(6) 0.082(4) Uani 1 1 d . . . C53 C 0.7808(3) -0.1097(15) 0.5592(6) 0.083(4) Uani 1 1 d . . . C54 C 0.7781(4) -0.0048(13) 0.5602(7) 0.093(4) Uani 1 1 d . . . H54A H 0.7887 0.0367 0.5322 0.111 Uiso 1 1 calc R . . C55 C 0.7599(5) 0.0410(16) 0.6019(9) 0.113(6) Uani 1 1 d . . . H55A H 0.7571 0.1140 0.6016 0.135 Uiso 1 1 calc R . . C56 C 0.8312(5) -0.4161(15) 0.4967(11) 0.139(6) Uani 1 1 d D . . H56A H 0.8354 -0.4264 0.5489 0.167 Uiso 1 1 calc R . . H56B H 0.8139 -0.4656 0.4729 0.167 Uiso 1 1 calc R . . C57 C 0.8598(7) -0.438(2) 0.4762(17) 0.231(15) Uani 1 1 d D . . H57A H 0.8665 -0.5095 0.4884 0.347 Uiso 1 1 calc R . . H57B H 0.8774 -0.3910 0.5011 0.347 Uiso 1 1 calc R . . H57C H 0.8559 -0.4280 0.4245 0.347 Uiso 1 1 calc R . . C58 C 0.9188(8) -0.184(3) 0.6188(17) 0.274(18) Uani 1 1 d . . . H58A H 0.9425 -0.1831 0.6221 0.411 Uiso 1 1 calc R . . H58B H 0.9114 -0.2564 0.6186 0.411 Uiso 1 1 calc R . . H58C H 0.9145 -0.1483 0.6600 0.411 Uiso 1 1 calc R . . C59 C 0.9015(5) -0.135(3) 0.5549(10) 0.180(9) Uani 1 1 d . . . H59A H 0.9067 -0.1699 0.5137 0.217 Uiso 1 1 calc R . . H59B H 0.9092 -0.0623 0.5555 0.217 Uiso 1 1 calc R . . C60 C 0.8140(3) -0.1042(11) 0.4674(5) 0.074(4) Uani 1 1 d . . . C61 C 0.7935(4) -0.0614(10) 0.4028(6) 0.079(3) Uani 1 1 d . . . C62 C 0.7597(4) -0.0727(10) 0.3814(7) 0.088(4) Uani 1 1 d . . . H62A H 0.7490 -0.1125 0.4099 0.106 Uiso 1 1 calc R . . C63 C 0.7415(4) -0.0282(13) 0.3203(8) 0.106(5) Uani 1 1 d . . . H63A H 0.7183 -0.0380 0.3056 0.128 Uiso 1 1 calc R . . C64 C 0.7584(7) 0.0354(13) 0.2777(7) 0.126(8) Uani 1 1 d . . . C65 C 0.7907(6) 0.0424(14) 0.2981(8) 0.124(7) Uani 1 1 d . . . H65A H 0.8016 0.0814 0.2694 0.149 Uiso 1 1 calc R . . C66 C 0.8091(5) -0.0032(10) 0.3577(7) 0.096(5) Uani 1 1 d . . . C67 C 0.8436(6) 0.0013(15) 0.3772(11) 0.124(6) Uani 1 1 d . . . H67A H 0.8542 0.0353 0.3458 0.148 Uiso 1 1 calc R . . C68 C 0.8623(5) -0.0387(15) 0.4367(9) 0.119(6) Uani 1 1 d . . . H68A H 0.8855 -0.0287 0.4488 0.143 Uiso 1 1 calc R . . C69 C 0.8473(4) -0.0970(15) 0.4825(7) 0.112(6) Uani 1 1 d . . . C70 C 0.7417(7) 0.1038(18) 0.2081(13) 0.173(11) Uani 1 1 d D . . H70A H 0.7548 0.1406 0.1828 0.207 Uiso 1 1 calc R . . C71 C 0.7119(6) 0.106(2) 0.1894(12) 0.163(10) Uani 1 1 d D . . H71A H 0.6968 0.0712 0.2103 0.195 Uiso 1 1 calc R . . C72 C 0.6510(5) 0.2389(13) 0.0395(8) 0.118(6) Uani 1 1 d . . . H72A H 0.6277 0.2356 0.0290 0.142 Uiso 1 1 calc R . . C73 C 0.6714(8) 0.1856(14) 0.0995(8) 0.149(9) Uani 1 1 d . . . H73A H 0.6601 0.1471 0.1275 0.179 Uiso 1 1 calc R . . C74 C 0.7033(7) 0.1826(17) 0.1210(10) 0.138(9) Uani 1 1 d . . . C75 C 0.7152(5) 0.230(2) 0.0776(10) 0.157(9) Uani 1 1 d . . . H75A H 0.7384 0.2281 0.0858 0.189 Uiso 1 1 calc R . . C76 C 0.6976(4) 0.2844(18) 0.0178(9) 0.152(8) Uani 1 1 d . . . H76A H 0.7097 0.3176 -0.0111 0.182 Uiso 1 1 calc R . . Cl1 Cl 0.5000 0.3915(5) 0.5000 0.169(3) Uani 1 2 d S . . O8 O 0.4720(4) 0.3282(12) 0.4702(8) 0.178(6) Uiso 1 1 d . . . O9 O 0.5101(5) 0.4516(17) 0.4489(11) 0.226(8) Uiso 1 1 d . . . N5 N 0.4805(5) 0.5304(14) 0.7646(11) 0.158(6) Uiso 1 1 d . . . O12 O 0.5022(5) 0.4714(15) 0.8760(11) 0.214(7) Uiso 1 1 d . . . C89 C 0.5111(6) 0.547(2) 0.7531(14) 0.190(10) Uiso 1 1 d . . . H89A H 0.5282 0.5251 0.7951 0.284 Uiso 1 1 calc R . . H89B H 0.5138 0.6214 0.7448 0.284 Uiso 1 1 calc R . . H89C H 0.5132 0.5080 0.7112 0.284 Uiso 1 1 calc R . . C90 C 0.4530(8) 0.557(2) 0.7042(16) 0.234(12) Uiso 1 1 d . . . H90A H 0.4322 0.5370 0.7147 0.351 Uiso 1 1 calc R . . H90B H 0.4553 0.5209 0.6613 0.351 Uiso 1 1 calc R . . H90C H 0.4529 0.6321 0.6960 0.351 Uiso 1 1 calc R . . C91 C 0.4785(6) 0.487(2) 0.8208(14) 0.172(8) Uiso 1 1 d . . . H91A H 0.4573 0.4642 0.8228 0.207 Uiso 1 1 calc R . . C81 C 0.7544(6) 0.458(4) -0.041(3) 0.204(19) Uiso 0.50 1 d PD . . C80 C 0.7529(19) 0.519(6) 0.024(3) 0.28(3) Uiso 0.50 1 d PD . . C79 C 0.8324(9) 0.307(3) 0.4529(18) 0.130(11) Uiso 0.50 1 d PD . . N6 N 0.8493(8) 0.289(3) 0.5328(18) 0.182(14) Uiso 0.50 1 d PD . . C78 C 0.8147(9) 0.297(3) 0.545(2) 0.148(13) Uiso 0.50 1 d PD . . O7 O 0.8423(13) 0.281(4) 0.395(2) 0.30(2) Uiso 0.50 1 d PD . . O13 O 0.6303(7) 0.978(2) 0.2240(15) 0.153(9) Uiso 0.50 1 d P . . O102 O 0.6438(15) 0.212(3) 0.274(3) 0.28(3) Uiso 0.50 1 d PD . . C85 C 0.6380(13) 0.894(5) 0.207(3) 0.207(19) Uiso 0.50 1 d PD . . O101 O 1.0000 0.850(4) 0.0000 0.326(17) Uiso 1 2 d S . . O103 O 0.5627(10) 0.269(4) 0.014(2) 0.238(17) Uiso 0.50 1 d P . . O10 O 0.7465(11) 0.402(4) -0.094(3) 0.27(2) Uiso 0.50 1 d PD . . C82 C 0.6505(16) 0.796(5) 0.233(3) 0.22(2) Uiso 0.50 1 d PD . . O19 O 0.6453(11) 0.433(3) 0.250(3) 0.28(2) Uiso 0.50 1 d PD . . C83 C 0.6206(13) 0.411(3) 0.199(3) 0.26(3) Uiso 0.50 1 d PD . . C84 C 0.5950(10) 0.339(3) 0.154(2) 0.160(15) Uiso 0.50 1 d PD . . Cl2 Cl 0.68186(19) 0.7908(5) 0.8322(8) 0.208(7) Uani 1 1 d D . . O15 O 0.6574(5) 0.8418(19) 0.8458(14) 0.208(12) Uiso 1 1 d D . . O16 O 0.6705(10) 0.765(3) 0.7574(12) 0.26(5) Uiso 1 1 d D . . O17 O 0.6897(8) 0.7021(18) 0.865(2) 0.25(2) Uiso 1 1 d D . . O18 O 0.7073(5) 0.8531(19) 0.8348(13) 0.202(11) Uiso 1 1 d D . . O24 O 0.8838(5) 0.5634(17) 0.0769(12) 0.125(7) Uiso 0.50 1 d PD . . O23 O 0.8711(13) 0.433(3) 0.000(2) 0.19(2) Uiso 0.50 1 d PD . . O22 O 0.9231(10) 0.471(11) 0.050(8) 0.17(6) Uiso 0.50 1 d PD . . O21 O 0.893(5) 0.577(6) -0.030(4) 0.27(8) Uiso 0.50 1 d PD . . Cl3 Cl 0.8927(11) 0.513(4) 0.025(3) 0.27(3) Uiso 0.50 1 d PD . . C77 C 0.8839(9) 0.307(3) 0.588(2) 0.192(18) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0928(6) 0.0947(6) 0.0606(5) 0.0099(6) 0.0205(4) 0.0118(7) O1 0.124(8) 0.160(10) 0.075(6) 0.040(6) 0.034(6) 0.072(7) O2 0.234(14) 0.080(7) 0.105(8) 0.024(6) 0.035(8) 0.037(8) O3 0.195(11) 0.069(6) 0.081(6) 0.010(5) 0.040(7) 0.019(7) O4 0.107(6) 0.158(9) 0.079(6) 0.009(8) 0.014(5) 0.040(9) O5 0.128(8) 0.128(9) 0.112(8) -0.003(7) 0.030(7) -0.022(7) O6 0.123(8) 0.113(8) 0.148(10) 0.018(7) 0.041(7) -0.005(7) N1 0.084(9) 0.129(11) 0.070(7) -0.012(7) 0.006(6) 0.022(7) N2 0.095(7) 0.074(8) 0.074(7) 0.020(6) 0.027(6) 0.012(6) N3 0.096(8) 0.087(8) 0.055(6) 0.019(5) 0.013(5) 0.006(6) N4 0.089(8) 0.137(10) 0.053(6) 0.024(7) 0.002(6) 0.013(7) C1 0.086(11) 0.143(15) 0.115(13) -0.026(11) 0.020(9) 0.006(10) C2 0.084(10) 0.161(17) 0.132(14) -0.033(13) 0.037(10) -0.007(11) C3 0.114(12) 0.100(11) 0.074(9) 0.002(8) 0.011(9) 0.004(9) C4 0.106(14) 0.20(2) 0.164(18) -0.089(16) 0.035(13) -0.014(14) C5 0.129(17) 0.21(3) 0.20(3) -0.05(2) 0.082(18) 0.010(17) C6 0.123(13) 0.141(14) 0.070(9) -0.017(9) 0.039(9) 0.012(11) C7 0.151(15) 0.115(12) 0.057(8) -0.005(8) 0.039(9) 0.025(11) C8 0.119(13) 0.109(12) 0.074(9) 0.010(8) 0.040(9) 0.014(10) C9 0.148(15) 0.119(13) 0.064(8) 0.002(8) 0.041(9) 0.020(11) C10 0.146(14) 0.075(9) 0.061(9) 0.014(7) 0.022(9) 0.022(9) C11 0.133(14) 0.102(11) 0.089(10) 0.017(8) 0.021(10) 0.042(10) C12 0.143(12) 0.130(13) 0.059(7) 0.019(11) 0.006(8) 0.052(14) C13 0.127(12) 0.112(13) 0.079(10) 0.043(8) 0.050(9) 0.051(9) C14 0.139(12) 0.047(8) 0.069(8) 0.016(5) 0.055(8) 0.025(7) C15 0.166(13) 0.104(12) 0.075(8) 0.048(11) 0.061(9) 0.040(14) C16 0.113(10) 0.082(11) 0.086(8) -0.006(7) 0.049(8) 0.000(8) C17 0.113(11) 0.109(11) 0.086(10) 0.005(9) 0.044(9) -0.012(9) C18 0.171(16) 0.109(13) 0.097(11) 0.019(10) 0.040(11) 0.054(12) C19 0.161(18) 0.131(17) 0.161(19) 0.031(15) 0.041(15) 0.039(14) C21 0.39(5) 0.17(3) 0.17(2) 0.09(2) -0.05(3) 0.09(3) C22 0.116(11) 0.072(10) 0.077(9) 0.005(7) 0.039(8) 0.018(8) C23 0.161(15) 0.089(12) 0.077(10) 0.009(9) 0.036(10) 0.014(10) C24 0.152(15) 0.082(11) 0.106(13) 0.021(10) 0.030(11) 0.020(10) C25 0.157(16) 0.106(14) 0.082(11) -0.010(10) 0.038(11) 0.024(12) C26 0.102(10) 0.076(10) 0.090(11) 0.001(9) 0.045(9) 0.014(8) C27 0.130(10) 0.072(11) 0.062(7) 0.004(8) 0.031(6) 0.000(10) C28 0.115(11) 0.108(12) 0.073(10) 0.010(9) 0.043(8) 0.027(9) C29 0.097(10) 0.060(9) 0.089(11) 0.007(8) 0.042(8) 0.008(8) C30 0.085(9) 0.102(11) 0.045(7) 0.011(7) 0.011(6) 0.016(8) C31 0.100(9) 0.082(12) 0.065(7) 0.017(8) 0.038(7) 0.030(8) C32 0.125(12) 0.108(12) 0.053(7) 0.013(8) 0.028(7) 0.038(9) C33 0.100(10) 0.095(11) 0.065(8) -0.001(7) 0.021(7) 0.017(8) C34 0.126(11) 0.101(12) 0.050(7) 0.002(7) 0.012(7) 0.014(9) C35 0.131(12) 0.067(9) 0.075(10) -0.002(7) 0.024(9) 0.006(8) C36 0.089(9) 0.076(10) 0.056(8) 0.023(7) 0.025(7) 0.034(7) C37 0.083(9) 0.117(13) 0.058(8) -0.011(8) 0.007(6) 0.003(8) C38 0.102(9) 0.079(10) 0.055(7) 0.001(6) 0.003(7) 0.012(7) C39 0.099(10) 0.098(11) 0.079(9) 0.046(8) 0.020(8) 0.010(8) C40 0.083(9) 0.101(11) 0.088(10) -0.034(9) -0.014(8) 0.040(8) C41 0.131(13) 0.089(11) 0.070(9) -0.017(8) 0.029(9) 0.023(10) C42 0.161(15) 0.126(15) 0.108(12) -0.002(10) 0.092(11) 0.032(12) C43 0.147(13) 0.075(9) 0.092(10) 0.015(7) 0.059(10) 0.015(8) C44 0.141(16) 0.076(12) 0.23(2) -0.057(14) -0.038(15) 0.058(12) C45 0.124(14) 0.17(2) 0.109(13) -0.040(13) -0.006(11) -0.009(14) C46 0.110(12) 0.23(2) 0.050(8) -0.030(11) 0.047(8) -0.002(13) C47 0.22(2) 0.133(16) 0.143(15) -0.045(17) 0.101(14) 0.02(2) C48 0.160(14) 0.136(16) 0.060(8) -0.014(8) 0.056(9) -0.011(11) C49 0.32(4) 0.115(18) 0.15(2) 0.019(15) 0.12(2) -0.06(2) C50 0.30(3) 0.087(12) 0.101(12) 0.010(10) 0.098(16) 0.036(15) C51 0.165(15) 0.087(11) 0.071(9) 0.012(8) 0.058(9) 0.010(10) C52 0.104(9) 0.091(12) 0.043(6) 0.005(6) 0.006(6) 0.013(7) C53 0.103(8) 0.100(12) 0.050(6) 0.016(9) 0.026(6) 0.008(11) C54 0.108(11) 0.098(12) 0.075(9) -0.013(8) 0.029(8) 0.011(9) C55 0.124(13) 0.128(14) 0.083(11) -0.020(10) 0.019(10) 0.026(11) C56 0.154(17) 0.118(16) 0.140(15) 0.010(12) 0.032(13) 0.027(13) C57 0.21(3) 0.15(2) 0.35(4) -0.02(2) 0.09(3) 0.06(2) C58 0.26(3) 0.30(4) 0.25(3) -0.01(3) 0.03(3) 0.12(3) C59 0.136(15) 0.27(3) 0.121(13) 0.05(2) 0.007(11) 0.02(2) C60 0.095(8) 0.080(10) 0.052(6) 0.003(6) 0.028(6) 0.023(8) C61 0.105(10) 0.077(8) 0.061(8) 0.004(6) 0.030(8) 0.010(7) C62 0.119(12) 0.083(9) 0.062(8) 0.002(6) 0.023(8) 0.020(8) C63 0.132(12) 0.114(12) 0.065(9) -0.027(9) 0.009(9) 0.032(10) C64 0.25(2) 0.095(11) 0.020(7) 0.015(7) 0.010(11) 0.076(14) C65 0.20(2) 0.120(14) 0.039(9) 0.020(8) -0.001(11) 0.030(14) C66 0.177(16) 0.057(8) 0.072(9) 0.005(7) 0.062(10) 0.001(9) C67 0.160(18) 0.131(15) 0.105(14) -0.008(12) 0.081(14) -0.022(13) C68 0.130(14) 0.160(16) 0.080(11) -0.009(11) 0.048(11) -0.012(12) C69 0.121(12) 0.156(19) 0.063(8) -0.001(9) 0.032(8) 0.020(12) C70 0.20(2) 0.17(2) 0.17(2) -0.121(19) 0.09(2) -0.061(19) C71 0.138(17) 0.24(3) 0.119(17) -0.072(18) 0.049(15) -0.021(19) C72 0.187(19) 0.102(12) 0.074(10) 0.016(9) 0.049(12) -0.008(12) C73 0.29(3) 0.093(12) 0.050(10) 0.016(8) 0.017(14) 0.032(16) C74 0.19(2) 0.130(16) 0.062(12) -0.018(11) -0.029(13) 0.068(16) C75 0.127(15) 0.25(3) 0.087(13) 0.059(15) 0.019(12) 0.013(15) C76 0.093(12) 0.23(2) 0.109(13) 0.072(14) -0.011(10) 0.004(13) Cl1 0.255(8) 0.056(4) 0.143(5) 0.000 -0.050(5) 0.000 Cl2 0.176(6) 0.097(4) 0.67(2) -0.059(8) 0.149(10) 0.005(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Cd1 N4 2.312(11) . ? Cd1 N1 2.327(12) . ? Cd1 N2 2.331(11) 1_554 ? Cd1 N3 2.336(11) 1_554 ? Cd1 O5 2.367(12) . ? Cd1 O6 2.406(12) . ? O1 C18 1.427(17) . ? O1 C13 1.434(16) . ? O2 C23 1.367(18) . ? O2 C21 1.41(3) . ? O3 C51 1.354(16) . ? O3 C56 1.41(2) . ? O4 C69 1.322(17) . ? O4 C59 1.51(2) . ? N1 C1 1.279(18) . ? N1 C5 1.41(3) . ? N2 C34 1.342(17) . ? N2 C38 1.358(15) . ? N2 Cd1 2.331(11) 1_556 ? N3 C43 1.316(15) . ? N3 C39 1.334(17) . ? N3 Cd1 2.336(11) 1_556 ? N4 C76 1.280(19) . ? N4 C72 1.322(18) . ? C1 C2 1.39(2) . ? C2 C3 1.38(2) . ? C3 C4 1.39(2) . ? C3 C6 1.45(2) . ? C4 C5 1.32(3) . ? C6 C7 1.29(2) . ? C7 C8 1.46(2) . ? C8 C9 1.37(2) . ? C8 C17 1.42(2) . ? C9 C10 1.41(2) . ? C10 C11 1.43(2) . ? C10 C15 1.46(2) . ? C11 C12 1.349(19) . ? C12 C13 1.39(2) . ? C13 C14 1.37(2) . ? C14 C15 1.411(19) . ? C14 C22 1.520(19) . ? C15 C16 1.400(19) . ? C16 C17 1.354(18) . ? C18 C19 1.44(2) . ? C20 C21 1.449(19) . ? C22 C23 1.347(19) . ? C22 C31 1.420(17) . ? C23 C24 1.43(2) . ? C24 C25 1.27(2) . ? C25 C26 1.44(2) . ? C26 C31 1.378(19) . ? C26 C27 1.410(19) . ? C27 C28 1.37(2) . ? C28 C32 1.455(18) . ? C28 C29 1.46(2) . ? C29 C30 1.385(19) . ? C30 C31 1.43(2) . ? C32 C33 1.318(19) . ? C33 C36 1.439(17) . ? C34 C35 1.377(18) . ? C35 C36 1.363(18) . ? C36 C37 1.401(19) . ? C37 C38 1.392(16) . ? C39 C40 1.368(18) . ? C40 C41 1.46(2) . ? C41 C42 1.43(2) . ? C41 C44 1.46(3) . ? C42 C43 1.401(18) . ? C44 C45 1.15(2) . ? C45 C46 1.55(2) . ? C46 C47 1.33(3) . ? C46 C55 1.46(3) . ? C47 C48 1.33(2) . ? C48 C49 1.42(3) . ? C48 C53 1.45(2) . ? C49 C50 1.37(3) . ? C50 C51 1.41(2) . ? C51 C52 1.365(18) . ? C52 C53 1.420(19) . ? C52 C60 1.519(17) . ? C53 C54 1.36(2) . ? C54 C55 1.38(2) . ? C56 C57 1.388(17) . ? C58 C59 1.42(3) . ? C60 C69 1.360(18) . ? C60 C61 1.437(17) . ? C61 C62 1.379(19) . ? C61 C66 1.432(18) . ? C62 C63 1.361(19) . ? C63 C64 1.47(3) . ? C64 C65 1.32(3) . ? C64 C70 1.61(3) . ? C65 C66 1.35(2) . ? C66 C67 1.40(2) . ? C67 C68 1.32(2) . ? C68 C69 1.43(2) . ? C70 C71 1.214(17) . ? C71 C74 1.61(3) . ? C72 C73 1.43(2) . ? C73 C74 1.30(3) . ? C74 C75 1.24(3) . ? C75 C76 1.40(2) . ? Cl1 O9 1.41(2) . ? Cl1 O9 1.41(2) 2_656 ? Cl1 O8 1.429(17) 2_656 ? Cl1 O8 1.429(17) . ? N5 C91 1.24(3) . ? N5 C89 1.38(3) . ? N5 C90 1.46(3) . ? O12 C91 1.28(3) . ? C81 O10 1.23(2) . ? C81 C80 1.49(2) . ? C79 O7 1.33(2) . ? C79 N6 1.547(19) . ? N6 C78 1.54(2) . ? N6 C77 1.585(19) . ? O13 C85 1.21(6) . ? C85 C82 1.41(2) . ? O19 C83 1.27(2) . ? C83 C84 1.51(2) . ? Cl2 O15 1.305(15) . ? Cl2 O17 1.309(16) . ? Cl2 O18 1.331(15) . ? Cl2 O16 1.443(17) . ? O24 Cl3 1.331(18) . ? O23 Cl3 1.376(18) . ? O22 Cl3 1.351(19) . ? O21 Cl3 1.347(18) . ? 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 N4 Cd1 N1 89.6(5) . . ? N4 Cd1 N2 178.7(5) . 1_554 ? N1 Cd1 N2 89.4(4) . 1_554 ? N4 Cd1 N3 90.9(4) . 1_554 ? N1 Cd1 N3 176.0(5) . 1_554 ? N2 Cd1 N3 90.0(4) 1_554 1_554 ? N4 Cd1 O5 89.7(4) . . ? N1 Cd1 O5 91.5(5) . . ? N2 Cd1 O5 91.2(4) 1_554 . ? N3 Cd1 O5 92.4(4) 1_554 . ? N4 Cd1 O6 89.3(4) . . ? N1 Cd1 O6 88.4(5) . . ? N2 Cd1 O6 89.8(4) 1_554 . ? N3 Cd1 O6 87.7(4) 1_554 . ? O5 Cd1 O6 179.0(4) . . ? C18 O1 C13 116.2(11) . . ? C23 O2 C21 117.8(16) . . ? C51 O3 C56 117.2(13) . . ? C69 O4 C59 115.6(13) . . ? C1 N1 C5 117.3(15) . . ? C1 N1 Cd1 120.8(11) . . ? C5 N1 Cd1 121.9(11) . . ? C34 N2 C38 116.4(11) . . ? C34 N2 Cd1 120.9(9) . 1_556 ? C38 N2 Cd1 122.7(9) . 1_556 ? C43 N3 C39 117.0(12) . . ? C43 N3 Cd1 116.3(9) . 1_556 ? C39 N3 Cd1 126.7(9) . 1_556 ? C76 N4 C72 114.3(14) . . ? C76 N4 Cd1 122.8(11) . . ? C72 N4 Cd1 122.4(11) . . ? N1 C1 C2 123.6(16) . . ? C3 C2 C1 120.6(15) . . ? C2 C3 C4 114.6(15) . . ? C2 C3 C6 122.1(16) . . ? C4 C3 C6 123.2(16) . . ? C5 C4 C3 123.7(19) . . ? C4 C5 N1 120.0(19) . . ? C7 C6 C3 127.5(16) . . ? C6 C7 C8 125.7(17) . . ? C9 C8 C17 118.4(14) . . ? C9 C8 C7 117.8(16) . . ? C17 C8 C7 123.4(16) . . ? C8 C9 C10 122.7(16) . . ? C9 C10 C11 122.2(15) . . ? C9 C10 C15 118.6(16) . . ? C11 C10 C15 119.1(14) . . ? C12 C11 C10 120.6(16) . . ? C11 C12 C13 118.6(15) . . ? C14 C13 C12 125.1(13) . . ? C14 C13 O1 111.9(14) . . ? C12 C13 O1 123.0(15) . . ? C13 C14 C15 117.7(14) . . ? C13 C14 C22 123.8(12) . . ? C15 C14 C22 118.5(15) . . ? C16 C15 C14 125.1(16) . . ? C16 C15 C10 115.9(15) . . ? C14 C15 C10 118.4(15) . . ? C17 C16 C15 124.4(15) . . ? C16 C17 C8 119.7(15) . . ? O1 C18 C19 107.0(15) . . ? O2 C21 C20 106(3) . . ? C23 C22 C31 119.7(14) . . ? C23 C22 C14 118.5(13) . . ? C31 C22 C14 121.8(12) . . ? C22 C23 O2 118.0(15) . . ? C22 C23 C24 120.7(15) . . ? O2 C23 C24 121.2(15) . . ? C25 C24 C23 119.7(17) . . ? C24 C25 C26 122.7(18) . . ? C31 C26 C27 120.1(13) . . ? C31 C26 C25 117.7(14) . . ? C27 C26 C25 121.8(16) . . ? C28 C27 C26 122.3(14) . . ? C27 C28 C32 121.7(15) . . ? C27 C28 C29 117.1(13) . . ? C32 C28 C29 121.1(15) . . ? C30 C29 C28 121.3(13) . . ? C29 C30 C31 118.8(14) . . ? C26 C31 C22 119.2(13) . . ? C26 C31 C30 120.3(12) . . ? C22 C31 C30 120.5(14) . . ? C33 C32 C28 129.4(15) . . ? C32 C33 C36 124.7(14) . . ? N2 C34 C35 123.6(13) . . ? C36 C35 C34 121.8(13) . . ? C35 C36 C37 114.9(11) . . ? C35 C36 C33 126.0(14) . . ? C37 C36 C33 119.1(13) . . ? C38 C37 C36 121.8(12) . . ? N2 C38 C37 121.4(12) . . ? N3 C39 C40 128.8(13) . . ? C39 C40 C41 114.9(14) . . ? C42 C41 C44 118.4(17) . . ? C42 C41 C40 116.3(12) . . ? C44 C41 C40 125.3(16) . . ? C43 C42 C41 120.7(14) . . ? N3 C43 C42 122.2(14) . . ? C45 C44 C41 132(3) . . ? C44 C45 C46 130(3) . . ? C47 C46 C55 120.1(16) . . ? C47 C46 C45 120.0(19) . . ? C55 C46 C45 120(2) . . ? C48 C47 C46 121(2) . . ? C47 C48 C49 122(2) . . ? C47 C48 C53 121(2) . . ? C49 C48 C53 117.5(16) . . ? C50 C49 C48 125.5(18) . . ? C49 C50 C51 115.4(17) . . ? O3 C51 C52 117.4(12) . . ? O3 C51 C50 119.9(15) . . ? C52 C51 C50 122.7(15) . . ? C51 C52 C53 122.5(13) . . ? C51 C52 C60 119.1(12) . . ? C53 C52 C60 118.5(12) . . ? C54 C53 C52 124.3(13) . . ? C54 C53 C48 119.1(14) . . ? C52 C53 C48 116.5(16) . . ? C53 C54 C55 119.7(16) . . ? C54 C55 C46 118.9(18) . . ? C57 C56 O3 112.9(18) . . ? C58 C59 O4 114(2) . . ? C69 C60 C61 121.0(12) . . ? C69 C60 C52 119.1(11) . . ? C61 C60 C52 119.7(11) . . ? C62 C61 C60 124.2(12) . . ? C62 C61 C66 117.9(13) . . ? C60 C61 C66 117.9(14) . . ? C63 C62 C61 121.6(15) . . ? C62 C63 C64 118.5(16) . . ? C65 C64 C63 118.6(14) . . ? C65 C64 C70 114(2) . . ? C63 C64 C70 127(2) . . ? C64 C65 C66 123.2(19) . . ? C65 C66 C67 122.6(17) . . ? C65 C66 C61 120.0(19) . . ? C67 C66 C61 117.3(14) . . ? C68 C67 C66 124.2(16) . . ? C67 C68 C69 119.3(17) . . ? O4 C69 C60 117.8(13) . . ? O4 C69 C68 122.0(16) . . ? C60 C69 C68 119.8(15) . . ? C71 C70 C64 117(3) . . ? C70 C71 C74 105(3) . . ? N4 C72 C73 117(2) . . ? C74 C73 C72 129(2) . . ? C75 C74 C73 109.1(19) . . ? C75 C74 C71 144(2) . . ? C73 C74 C71 106(2) . . ? C74 C75 C76 126(2) . . ? N4 C76 C75 124.2(17) . . ? O9 Cl1 O9 112.9(18) . 2_656 ? O9 Cl1 O8 103.6(10) . 2_656 ? O9 Cl1 O8 113.5(10) 2_656 2_656 ? O9 Cl1 O8 113.5(10) . . ? O9 Cl1 O8 103.6(10) 2_656 . ? O8 Cl1 O8 110.1(13) 2_656 . ? C91 N5 C89 119(2) . . ? C91 N5 C90 126(2) . . ? C89 N5 C90 114(2) . . ? N5 C91 O12 126(3) . . ? O10 C81 C80 161(5) . . ? O7 C79 N6 130(4) . . ? C78 N6 C79 86(3) . . ? C78 N6 C77 129(3) . . ? C79 N6 C77 139(3) . . ? O13 C85 C82 144(6) . . ? O19 C83 C84 154(3) . . ? O15 Cl2 O17 117.4(16) . . ? O15 Cl2 O18 110.8(13) . . ? O17 Cl2 O18 114.3(15) . . ? O15 Cl2 O16 104.2(15) . . ? O17 Cl2 O16 104.9(15) . . ? O18 Cl2 O16 103.6(16) . . ? O24 Cl3 O21 110.5(19) . . ? O24 Cl3 O22 110.4(19) . . ? O21 Cl3 O22 109.4(19) . . ? O24 Cl3 O23 110.2(18) . . ? O21 Cl3 O23 108.4(18) . . ? O22 Cl3 O23 107.9(18) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.739 _refine_diff_density_min -0.480 _refine_diff_density_rms 0.102 # Attachment 'new5.cif' data_new5 _database_code_depnum_ccdc_archive 'CCDC 607393' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84.50 H90.50 Cl2 Co N7.50 O18.50' _chemical_formula_weight 1636.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 42.576(1) _cell_length_b 12.605(1) _cell_length_c 19.2306(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.695(2) _cell_angle_gamma 90.00 _cell_volume 9983.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 21.50 _exptl_crystal_description Bloc _exptl_crystal_colour Pink _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.089 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3436 _exptl_absorpt_coefficient_mu 0.286 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.7464 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 34437 _diffrn_reflns_av_R_equivalents 0.0840 _diffrn_reflns_av_sigmaI/netI 0.1052 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 21.50 _reflns_number_total 11415 _reflns_number_gt 6379 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+116.8766P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(5) _refine_ls_number_reflns 11415 _refine_ls_number_parameters 887 _refine_ls_number_restraints 25 _refine_ls_R_factor_ref 0.1973 _refine_ls_R_factor_gt 0.1254 _refine_ls_wR_factor_ref 0.2922 _refine_ls_wR_factor_gt 0.2664 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.13841(5) 0.79774(18) 0.39361(9) 0.0721(6) Uani 1 1 d . . . O1 O -0.0665(3) 1.3869(9) 0.7993(5) 0.092(3) Uani 1 1 d . . . O2 O -0.0149(3) 1.5487(10) 0.7858(6) 0.112(4) Uani 1 1 d . . . O3 O 0.3656(2) 0.3002(11) 1.0429(5) 0.092(3) Uani 1 1 d . . . O4 O 0.3210(3) 0.1192(9) 0.9834(6) 0.098(4) Uani 1 1 d . . . O5 O 0.1781(3) 0.9053(8) 0.3993(5) 0.085(3) Uani 1 1 d . . . O6 O 0.1004(3) 0.6852(9) 0.3866(5) 0.096(4) Uani 1 1 d . . . N1 N 0.1182(3) 0.9055(10) 0.4583(6) 0.070(4) Uani 1 1 d . . . N2 N 0.1102(3) 0.8790(11) 1.2973(5) 0.075(4) Uani 1 1 d . . . N3 N 0.1663(3) 0.7215(11) 0.4912(7) 0.083(4) Uiso 1 1 d . . . N4 N 0.1595(3) 0.6984(10) 1.3304(6) 0.072(4) Uani 1 1 d . . . C1 C 0.1366(4) 0.9548(15) 0.5129(9) 0.088(5) Uani 1 1 d . . . H1A H 0.1595 0.9472 0.5223 0.106 Uiso 1 1 calc R . . C2 C 0.1237(5) 1.0190(14) 0.5584(8) 0.096(6) Uani 1 1 d . . . H2A H 0.1376 1.0547 0.5980 0.115 Uiso 1 1 calc R . . C3 C 0.0889(5) 1.0299(14) 0.5441(8) 0.085(5) Uani 1 1 d . . . C4 C 0.0696(4) 0.9743(14) 0.4897(7) 0.092(6) Uani 1 1 d . . . H4A H 0.0466 0.9730 0.4811 0.111 Uiso 1 1 calc R . . C5 C 0.0860(5) 0.9196(17) 0.4478(8) 0.110(7) Uani 1 1 d . . . H5A H 0.0727 0.8874 0.4058 0.132 Uiso 1 1 calc R . . C6 C 0.0755(5) 1.0927(14) 0.5926(8) 0.090(5) Uani 1 1 d . . . H6A H 0.0901 1.1295 0.6305 0.108 Uiso 1 1 calc R . . C7 C 0.0435(5) 1.1017(15) 0.5869(7) 0.096(6) Uani 1 1 d . . . H7A H 0.0290 1.0635 0.5497 0.116 Uiso 1 1 calc R . . C8 C 0.0295(4) 1.1695(15) 0.6364(7) 0.083(5) Uani 1 1 d . . . C9 C -0.0026(5) 1.1721(17) 0.6212(7) 0.109(7) Uani 1 1 d . . . H9A H -0.0144 1.1348 0.5799 0.130 Uiso 1 1 calc R . . C10 C -0.0212(5) 1.2296(13) 0.6649(8) 0.077(5) Uani 1 1 d . . . C11 C -0.0549(5) 1.2362(14) 0.6469(8) 0.097(6) Uani 1 1 d . . . H11A H -0.0670 1.2052 0.6033 0.117 Uiso 1 1 calc R . . C12 C -0.0709(4) 1.2857(14) 0.6900(8) 0.091(5) Uani 1 1 d . . . H12A H -0.0940 1.2879 0.6779 0.109 Uiso 1 1 calc R . . C13 C -0.0525(4) 1.3340(12) 0.7536(7) 0.073(5) Uani 1 1 d . . . C14 C -0.0186(4) 1.3291(11) 0.7719(6) 0.070(5) Uani 1 1 d . . . C15 C -0.0018(5) 1.2794(13) 0.7283(6) 0.074(5) Uani 1 1 d . . . C16 C 0.0319(4) 1.2705(12) 0.7436(7) 0.072(5) Uani 1 1 d . . . H16A H 0.0449 1.3006 0.7866 0.086 Uiso 1 1 calc R . . C17 C 0.0465(4) 1.2188(15) 0.6975(8) 0.094(5) Uani 1 1 d . . . H17A H 0.0696 1.2173 0.7086 0.112 Uiso 1 1 calc R . . C18 C -0.0947(5) 1.4516(15) 0.7710(9) 0.102(6) Uani 1 1 d . . . H18A H -0.0925 1.4887 0.7271 0.122 Uiso 1 1 calc R . . H18B H -0.1143 1.4066 0.7582 0.122 Uiso 1 1 calc R . . C19 C -0.0973(4) 1.5249(17) 0.8231(11) 0.113(6) Uani 1 1 d . . . H19A H -0.1170 1.5673 0.8055 0.170 Uiso 1 1 calc R . . H19B H -0.0783 1.5717 0.8334 0.170 Uiso 1 1 calc R . . H19C H -0.0984 1.4876 0.8670 0.170 Uiso 1 1 calc R . . C20 C -0.0290(9) 1.693(4) 0.7208(17) 0.35(2) Uiso 1 1 d D . . H20A H -0.0256 1.7685 0.7143 0.526 Uiso 1 1 calc R . . H20B H -0.0514 1.6806 0.7235 0.526 Uiso 1 1 calc R . . H20C H -0.0250 1.6531 0.6799 0.526 Uiso 1 1 calc R . . C21 C -0.0066(7) 1.6563(16) 0.7872(13) 0.199(15) Uani 1 1 d D . . H21A H -0.0105 1.6926 0.8298 0.238 Uiso 1 1 calc R . . H21B H 0.0163 1.6663 0.7861 0.238 Uiso 1 1 calc R . . C22 C 0.0000(3) 1.3800(13) 0.8419(8) 0.072(4) Uani 1 1 d . . . C23 C 0.0177(3) 1.3188(12) 0.9031(7) 0.066(4) Uani 1 1 d . . . C24 C 0.0166(3) 1.2032(12) 0.9033(7) 0.063(4) Uani 1 1 d . . . H24A H 0.0052 1.1674 0.8609 0.076 Uiso 1 1 calc R . . C25 C 0.0311(4) 1.1456(12) 0.9615(7) 0.066(4) Uani 1 1 d . . . H25A H 0.0300 1.0703 0.9613 0.079 Uiso 1 1 calc R . . C26 C 0.0483(4) 1.2043(17) 1.0246(7) 0.087(5) Uani 1 1 d . . . C27 C 0.0499(4) 1.3129(12) 1.0257(7) 0.069(4) Uani 1 1 d . . . H27A H 0.0616 1.3470 1.0685 0.083 Uiso 1 1 calc R . . C28 C 0.0348(4) 1.3758(16) 0.9666(8) 0.082(5) Uani 1 1 d . . . C29 C 0.0352(4) 1.4879(14) 0.9698(9) 0.081(5) Uani 1 1 d . . . H29A H 0.0467 1.5239 1.0120 0.098 Uiso 1 1 calc R . . C30 C 0.0193(5) 1.5410(13) 0.9129(10) 0.102(6) Uani 1 1 d . . . H30A H 0.0198 1.6164 0.9145 0.122 Uiso 1 1 calc R . . C31 C 0.0009(4) 1.4890(16) 0.8473(9) 0.093(5) Uani 1 1 d . . . C32 C 0.0639(4) 1.1414(15) 1.0917(7) 0.082(5) Uani 1 1 d . . . H32A H 0.0759 1.1822 1.1311 0.099 Uiso 1 1 calc R . . C33 C 0.0632(4) 1.0370(13) 1.1036(8) 0.077(5) Uani 1 1 d . . . H33A H 0.0521 0.9930 1.0650 0.092 Uiso 1 1 calc R . . C34 C 0.1091(4) 0.9835(12) 1.2916(8) 0.080(5) Uani 1 1 d . . . H34A H 0.1192 1.0230 1.3334 0.095 Uiso 1 1 calc R . . C35 C 0.0782(4) 0.8794(14) 1.1787(8) 0.081(5) Uani 1 1 d . . . H35A H 0.0677 0.8399 1.1373 0.097 Uiso 1 1 calc R . . C36 C 0.0921(4) 0.8208(14) 1.2401(6) 0.081(5) Uani 1 1 d . . . H36A H 0.0893 0.7462 1.2425 0.097 Uiso 1 1 calc R . . C37 C 0.0954(4) 1.0382(12) 1.2334(8) 0.076(5) Uani 1 1 d . . . H37A H 0.0973 1.1133 1.2339 0.091 Uiso 1 1 calc R . . C38 C 0.0781(3) 0.9871(11) 1.1711(6) 0.048(3) Uani 1 1 d . . . C39 C 0.1976(3) 0.6986(15) 0.5085(8) 0.088(5) Uani 1 1 d . . . H39A H 0.2097 0.7224 0.4761 0.106 Uiso 1 1 calc R . . C40 C 0.2138(5) 0.6468(15) 0.5652(8) 0.109(7) Uani 1 1 d . . . H40A H 0.2363 0.6345 0.5710 0.131 Uiso 1 1 calc R . . C41 C 0.2001(7) 0.6114(15) 0.6140(9) 0.114(7) Uani 1 1 d . . . C42 C 0.1674(5) 0.6248(15) 0.5980(8) 0.100(6) Uani 1 1 d . . . H42A H 0.1557 0.5941 0.6290 0.120 Uiso 1 1 calc R . . C43 C 0.1505(4) 0.6805(15) 0.5394(9) 0.096(6) Uani 1 1 d . . . H43A H 0.1277 0.6908 0.5318 0.115 Uiso 1 1 calc R . . C44 C 0.2139(5) 0.5470(18) 0.6844(9) 0.117(8) Uani 1 1 d . . . H44A H 0.2003 0.5146 0.7105 0.140 Uiso 1 1 calc R . . C45 C 0.2446(6) 0.5411(16) 0.7040(11) 0.112(7) Uani 1 1 d . . . H45A H 0.2577 0.5758 0.6777 0.135 Uiso 1 1 calc R . . C46 C 0.2607(5) 0.4731(17) 0.7749(8) 0.103(7) Uani 1 1 d . . . C47 C 0.2923(5) 0.4824(14) 0.7922(9) 0.091(5) Uiso 1 1 d . . . H47A H 0.3022 0.5232 0.7621 0.109 Uiso 1 1 calc R . . C48 C 0.3127(6) 0.4329(14) 0.8554(9) 0.100(6) Uani 1 1 d . . . C49 C 0.2961(5) 0.3729(14) 0.9021(8) 0.084(5) Uani 1 1 d . . . C50 C 0.2605(4) 0.3591(14) 0.8757(9) 0.094(5) Uani 1 1 d . . . H50A H 0.2490 0.3143 0.9003 0.112 Uiso 1 1 calc R . . C51 C 0.2439(4) 0.4147(14) 0.8121(8) 0.087(5) Uani 1 1 d . . . H51A H 0.2209 0.4105 0.7960 0.104 Uiso 1 1 calc R . . C52 C 0.3464(6) 0.4400(17) 0.8724(10) 0.120(7) Uani 1 1 d . . . H52A H 0.3568 0.4762 0.8412 0.144 Uiso 1 1 calc R . . C53 C 0.3641(5) 0.3955(17) 0.9330(12) 0.122(7) Uani 1 1 d . . . H53A H 0.3871 0.4007 0.9459 0.147 Uiso 1 1 calc R . . C54 C 0.3461(5) 0.3357(13) 0.9816(8) 0.083(5) Uani 1 1 d . . . C55 C 0.3153(3) 0.3287(11) 0.9646(6) 0.056(4) Uani 1 1 d . . . C56 C 0.3982(5) 0.297(2) 1.0546(10) 0.150(9) Uani 1 1 d . . . H56A H 0.4076 0.3680 1.0691 0.180 Uiso 1 1 calc R . . H56B H 0.4043 0.2751 1.0104 0.180 Uiso 1 1 calc R . . C57 C 0.4104(6) 0.218(3) 1.1139(16) 0.246(17) Uani 1 1 d . . . H57A H 0.4340 0.2104 1.1224 0.369 Uiso 1 1 calc R . . H57B H 0.4001 0.1488 1.0997 0.369 Uiso 1 1 calc R . . H57C H 0.4052 0.2421 1.1579 0.369 Uiso 1 1 calc R . . C58 C 0.3602(7) -0.002(2) 0.9716(13) 0.198(12) Uani 1 1 d . . . H58A H 0.3693 -0.0716 0.9873 0.296 Uiso 1 1 calc R . . H58B H 0.3774 0.0520 0.9843 0.296 Uiso 1 1 calc R . . H58C H 0.3511 -0.0019 0.9194 0.296 Uiso 1 1 calc R . . C59 C 0.3347(5) 0.023(2) 1.0070(12) 0.130(8) Uani 1 1 d . . . H59A H 0.3179 -0.0328 0.9964 0.156 Uiso 1 1 calc R . . H59B H 0.3439 0.0258 1.0597 0.156 Uiso 1 1 calc R . . C60 C 0.3001(3) 0.2721(13) 1.0145(6) 0.065(4) Uani 1 1 d . . . C61 C 0.3038(4) 0.1592(17) 1.0258(8) 0.091(6) Uani 1 1 d . . . C62 C 0.2878(6) 0.1052(14) 1.0708(10) 0.125(8) Uani 1 1 d . . . H62A H 0.2892 0.0302 1.0749 0.149 Uiso 1 1 calc R . . C63 C 0.2705(5) 0.161(2) 1.1082(10) 0.135(9) Uani 1 1 d . . . H63A H 0.2608 0.1241 1.1402 0.162 Uiso 1 1 calc R . . C64 C 0.2660(4) 0.2765(17) 1.1023(10) 0.100(6) Uiso 1 1 d . . . C65 C 0.2810(4) 0.3329(16) 1.0550(7) 0.079(5) Uani 1 1 d . . . C66 C 0.2774(4) 0.4387(15) 1.0518(8) 0.082(5) Uani 1 1 d . . . H66A H 0.2877 0.4808 1.0229 0.098 Uiso 1 1 calc R . . C67 C 0.2581(5) 0.4846(18) 1.0923(10) 0.117(7) Uani 1 1 d . . . H67A H 0.2537 0.5584 1.0861 0.140 Uiso 1 1 calc R . . C68 C 0.2448(5) 0.431(3) 1.1408(13) 0.151(14) Uani 1 1 d . . . C69 C 0.2486(5) 0.323(3) 1.1435(11) 0.137(10) Uani 1 1 d . . . H69A H 0.2391 0.2810 1.1739 0.164 Uiso 1 1 calc R . . C70 C 0.2244(4) 0.512(2) 1.1771(10) 0.153(11) Uani 1 1 d D . . H70A H 0.2249 0.5834 1.1623 0.183 Uiso 1 1 calc R . . C71 C 0.2084(6) 0.495(2) 1.2207(13) 0.169(11) Uiso 1 1 d D . . H71A H 0.2064 0.4242 1.2352 0.203 Uiso 1 1 calc R . . C72 C 0.1702(4) 0.7405(15) 1.2756(9) 0.098(5) Uiso 1 1 d . . . H72A H 0.1664 0.8141 1.2661 0.117 Uiso 1 1 calc R . . C73 C 0.1865(4) 0.6831(15) 1.2308(10) 0.101(6) Uiso 1 1 d . . . H73A H 0.1926 0.7150 1.1914 0.121 Uiso 1 1 calc R . . C74 C 0.1931(5) 0.5737(17) 1.2502(10) 0.111(6) Uiso 1 1 d D . . C75 C 0.1814(3) 0.5233(12) 1.3041(7) 0.073(4) Uiso 1 1 d . . . H75A H 0.1841 0.4497 1.3149 0.087 Uiso 1 1 calc R . . C76 C 0.1655(4) 0.5920(13) 1.3399(8) 0.086(5) Uiso 1 1 d . . . H76A H 0.1574 0.5603 1.3767 0.103 Uiso 1 1 calc R . . Cl1 Cl 0.0000 0.8100(6) 1.0000 0.126(3) Uani 1 2 d S . . O7 O 0.0099(5) 0.8703(14) 0.9473(9) 0.192(8) Uani 1 1 d . . . O8 O -0.0285(4) 0.7429(11) 0.9693(7) 0.151(6) Uani 1 1 d . . . C81 C 0.0459(7) -0.027(2) 0.7935(15) 0.177(10) Uiso 1 1 d . . . N5 N 0.0177(5) -0.0550(15) 0.7359(11) 0.147(6) Uiso 1 1 d . . . C82 C -0.0138(6) -0.0363(19) 0.7474(12) 0.144(8) Uiso 1 1 d . . . C85 C 0.2288(9) 0.951(3) -0.3860(19) 0.091(10) Uiso 0.50 1 d P . . N6 N 0.2416(9) 0.964(3) -0.440(2) 0.145(13) Uiso 0.50 1 d P . . C84 C 0.2089(10) 0.921(3) -0.354(2) 0.125(14) Uiso 0.50 1 d P . . H84A H 0.2202 0.8947 -0.3064 0.188 Uiso 0.50 1 calc PR . . H84B H 0.1957 0.8635 -0.3815 0.188 Uiso 0.50 1 calc PR . . H84C H 0.1948 0.9802 -0.3493 0.188 Uiso 0.50 1 calc PR . . Cl2 Cl 0.1354(4) 0.3868(15) 0.7392(10) 0.226(7) Uiso 0.50 1 d PD . . O14 O 0.1242(9) 0.438(3) 0.6758(16) 0.28(2) Uiso 0.50 1 d PD . . O15 O 0.1128(10) 0.401(4) 0.777(2) 0.27(3) Uiso 0.50 1 d PD . . O13 O 0.1385(9) 0.2836(18) 0.7241(18) 0.232(16) Uiso 0.50 1 d PD . . O12 O 0.1632(7) 0.426(3) 0.776(2) 0.22(2) Uiso 0.50 1 d PD . . Cl3 Cl 0.17799(19) 0.2087(6) 0.3615(4) 0.178(3) Uiso 1 1 d D . . O16 O 0.1513(6) 0.263(3) 0.3656(19) 0.25(2) Uiso 1 1 d D . . O17 O 0.1840(7) 0.1296(18) 0.4068(13) 0.232(15) Uiso 1 1 d D . . O18 O 0.2032(7) 0.277(3) 0.373(2) 0.23(3) Uiso 1 1 d D . . O19 O 0.1720(9) 0.183(3) 0.2907(9) 0.23(2) Uiso 1 1 d D . . C88 C 0.1615(13) 0.736(5) -0.218(3) 0.169(19) Uiso 0.50 1 d P . . C89 C 0.1087(13) 0.876(4) -0.290(3) 0.152(17) Uiso 0.50 1 d P . . C90 C 0.1667(10) 0.225(3) 1.065(2) 0.124(13) Uiso 0.50 1 d P . . C91 C 0.1763(10) 0.203(4) 1.007(2) 0.133(15) Uiso 0.50 1 d P . . N9 N 0.1871(10) 0.234(3) 0.940(2) 0.173(15) Uiso 0.50 1 d P . . C83 C 0.0227(9) -0.092(3) 0.675(2) 0.212(12) Uiso 1 1 d . . . O11 O -0.0034(6) -0.1108(19) 0.6235(13) 0.242(9) Uiso 1 1 d . . . O101 O 0.0000 -0.219(4) 0.5000 0.26(2) Uiso 1 2 d S . . O102 O 0.1144(5) 0.4829(18) 0.4343(12) 0.232(9) Uiso 1 1 d D . . O103 O 0.1229(12) 0.317(3) 0.529(2) 0.29(2) Uiso 0.50 1 d PD . . O104 O 0.1130(7) 0.186(3) 0.9107(16) 0.262(14) Uiso 1 1 d . . . C94 C 0.1492(16) 0.945(6) -0.224(3) 0.22(3) Uiso 0.50 1 d P . . N8 N 0.1431(16) 0.821(6) -0.249(3) 0.26(3) Uiso 0.50 1 d P . . O20 O 0.1004(12) 0.787(5) -0.328(3) 0.27(2) Uiso 0.50 1 d P . . N10 N 0.2783(12) 0.793(4) -0.598(2) 0.210(18) Uiso 0.50 1 d P . . C92 C 0.2395(8) 0.836(3) -0.5928(17) 0.070(10) Uiso 0.50 1 d P . . C93 C 0.2427(10) 0.798(4) -0.626(2) 0.115(12) Uiso 0.50 1 d P . . 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 Co1 0.0954(14) 0.0738(13) 0.0491(10) 0.0087(11) 0.0222(9) 0.0165(14) O1 0.117(9) 0.103(8) 0.062(6) 0.039(6) 0.034(6) 0.035(8) O2 0.145(11) 0.116(11) 0.067(7) 0.030(7) 0.014(7) -0.007(9) O3 0.057(7) 0.131(9) 0.079(7) 0.004(8) 0.003(6) 0.033(8) O4 0.144(11) 0.068(8) 0.085(8) -0.008(6) 0.036(8) 0.035(8) O5 0.109(8) 0.072(7) 0.081(7) 0.018(6) 0.037(6) 0.010(6) O6 0.113(9) 0.118(9) 0.060(6) 0.018(6) 0.028(6) 0.033(8) N1 0.075(10) 0.095(10) 0.034(7) -0.009(6) 0.002(6) 0.017(8) N2 0.084(9) 0.109(11) 0.036(6) 0.043(7) 0.022(6) 0.071(8) N4 0.083(9) 0.080(9) 0.062(7) 0.013(7) 0.034(7) 0.028(8) C1 0.065(11) 0.133(16) 0.067(11) -0.011(11) 0.018(9) -0.001(11) C2 0.115(16) 0.113(15) 0.060(10) -0.028(10) 0.022(10) -0.001(12) C3 0.103(15) 0.112(14) 0.042(9) -0.018(9) 0.021(9) -0.003(12) C4 0.111(14) 0.140(15) 0.037(8) -0.022(9) 0.037(10) 0.044(12) C5 0.086(15) 0.165(19) 0.054(10) -0.004(12) -0.028(10) -0.014(14) C6 0.083(13) 0.126(15) 0.060(10) -0.013(10) 0.019(9) 0.013(12) C7 0.118(16) 0.132(16) 0.030(8) -0.009(9) 0.005(9) 0.008(13) C8 0.076(13) 0.139(16) 0.035(9) 0.004(9) 0.016(9) -0.002(12) C9 0.123(17) 0.18(2) 0.032(8) 0.009(10) 0.029(10) -0.019(15) C10 0.097(14) 0.099(12) 0.048(10) -0.001(9) 0.043(10) -0.001(11) C11 0.140(18) 0.104(14) 0.047(9) -0.002(9) 0.021(11) -0.016(13) C12 0.128(14) 0.088(12) 0.064(10) 0.023(10) 0.038(11) 0.018(13) C13 0.089(13) 0.099(14) 0.036(8) 0.017(8) 0.029(9) 0.026(10) C14 0.111(14) 0.065(12) 0.026(7) 0.008(7) 0.002(8) 0.000(10) C15 0.131(15) 0.079(12) 0.025(7) 0.008(8) 0.047(9) 0.011(11) C16 0.070(11) 0.098(14) 0.055(9) -0.014(8) 0.030(8) 0.012(9) C17 0.110(14) 0.124(15) 0.049(9) -0.008(10) 0.024(10) -0.021(12) C18 0.132(17) 0.101(15) 0.073(11) 0.023(11) 0.029(11) 0.027(13) C19 0.091(14) 0.133(18) 0.123(16) -0.008(14) 0.040(12) 0.024(13) C21 0.24(3) 0.070(15) 0.20(2) 0.084(15) -0.11(2) -0.025(16) C22 0.062(10) 0.077(12) 0.091(12) 0.015(10) 0.046(9) 0.028(9) C23 0.086(11) 0.076(13) 0.037(7) 0.006(8) 0.020(7) 0.025(9) C24 0.088(11) 0.073(11) 0.031(8) -0.007(7) 0.020(7) 0.006(9) C25 0.104(12) 0.058(10) 0.030(8) -0.004(7) 0.007(8) -0.013(9) C26 0.079(12) 0.151(18) 0.037(9) 0.000(10) 0.025(8) 0.003(12) C27 0.124(13) 0.037(9) 0.054(8) 0.002(7) 0.037(8) 0.024(9) C28 0.088(12) 0.116(15) 0.053(10) 0.028(10) 0.038(9) 0.051(11) C29 0.109(14) 0.076(13) 0.069(11) 0.035(10) 0.041(10) 0.045(11) C30 0.157(18) 0.056(11) 0.096(13) -0.012(10) 0.039(13) 0.027(12) C31 0.114(15) 0.097(16) 0.077(12) 0.000(12) 0.043(11) -0.012(12) C32 0.108(14) 0.102(15) 0.049(9) 0.023(9) 0.044(9) 0.042(11) C33 0.106(13) 0.068(12) 0.062(10) -0.018(9) 0.032(9) 0.002(10) C34 0.118(14) 0.054(10) 0.063(10) 0.041(8) 0.017(9) 0.061(10) C35 0.083(12) 0.096(14) 0.063(10) -0.026(9) 0.018(9) 0.005(10) C36 0.115(12) 0.099(13) 0.014(6) -0.005(8) -0.012(7) 0.017(11) C37 0.112(13) 0.065(10) 0.072(11) 0.013(9) 0.061(10) 0.036(10) C38 0.064(10) 0.045(9) 0.035(8) 0.009(7) 0.013(7) 0.030(7) C39 0.050(10) 0.158(16) 0.065(10) -0.012(11) 0.029(8) 0.004(11) C40 0.129(16) 0.166(19) 0.028(8) 0.036(10) 0.012(10) 0.092(14) C41 0.19(2) 0.090(14) 0.042(12) -0.017(10) -0.002(14) 0.008(16) C42 0.129(17) 0.112(15) 0.036(9) 0.022(9) -0.020(11) -0.006(14) C43 0.081(12) 0.137(16) 0.080(12) -0.012(11) 0.040(10) -0.018(12) C44 0.098(15) 0.17(2) 0.074(13) -0.047(13) 0.009(12) 0.045(16) C45 0.131(18) 0.111(16) 0.118(16) -0.053(13) 0.071(15) -0.005(15) C46 0.131(18) 0.144(18) 0.032(9) 0.015(10) 0.019(10) 0.062(14) C48 0.131(18) 0.091(13) 0.071(11) -0.006(10) 0.015(12) 0.022(13) C49 0.114(15) 0.096(13) 0.055(9) -0.001(9) 0.046(10) 0.016(11) C50 0.074(13) 0.110(14) 0.096(13) -0.036(10) 0.020(10) 0.029(11) C51 0.080(12) 0.116(15) 0.047(9) -0.013(10) -0.015(9) 0.008(11) C52 0.125(19) 0.16(2) 0.075(13) 0.039(13) 0.020(13) 0.012(16) C53 0.097(15) 0.145(19) 0.129(17) -0.024(16) 0.037(14) -0.004(14) C54 0.085(14) 0.106(15) 0.058(9) 0.011(9) 0.015(10) 0.032(11) C55 0.033(8) 0.094(13) 0.038(7) 0.003(7) 0.002(6) 0.020(8) C56 0.095(17) 0.22(2) 0.103(14) 0.049(19) -0.032(12) 0.00(2) C57 0.14(2) 0.35(4) 0.23(3) -0.10(3) 0.03(2) 0.13(3) C58 0.23(3) 0.21(3) 0.15(2) -0.04(2) 0.04(2) 0.06(3) C59 0.114(17) 0.14(2) 0.149(19) -0.010(17) 0.062(15) 0.024(16) C60 0.079(10) 0.073(13) 0.042(8) -0.002(7) 0.017(7) 0.009(9) C61 0.094(14) 0.124(17) 0.059(10) -0.033(11) 0.025(9) 0.000(12) C62 0.26(3) 0.060(12) 0.099(14) 0.010(10) 0.121(17) -0.021(14) C63 0.138(18) 0.20(3) 0.078(13) 0.042(15) 0.051(13) -0.052(18) C65 0.058(10) 0.127(18) 0.049(8) 0.014(9) 0.010(7) 0.008(10) C66 0.100(13) 0.077(13) 0.065(10) 0.009(9) 0.014(9) 0.032(11) C67 0.127(17) 0.141(19) 0.073(13) -0.047(13) 0.009(13) 0.043(15) C68 0.059(13) 0.31(4) 0.092(16) -0.11(2) 0.032(11) 0.01(2) C69 0.109(16) 0.22(3) 0.094(13) -0.08(2) 0.053(12) -0.02(2) C70 0.055(12) 0.29(3) 0.103(15) -0.096(18) -0.001(11) -0.057(16) Cl1 0.208(9) 0.046(4) 0.096(5) 0.000 -0.013(5) 0.000 O7 0.25(2) 0.163(15) 0.147(13) 0.049(12) 0.010(13) -0.035(14) O8 0.197(15) 0.102(10) 0.114(10) 0.007(8) -0.036(10) -0.005(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Co1 N4 2.100(11) 1_554 ? Co1 O6 2.131(12) . ? Co1 O5 2.146(10) . ? Co1 N1 2.161(11) . ? Co1 N3 2.174(13) . ? Co1 N2 2.191(9) 1_554 ? O1 C13 1.356(15) . ? O1 C18 1.439(18) . ? O2 C21 1.40(2) . ? O2 C31 1.419(19) . ? O3 C54 1.337(16) . ? O3 C56 1.35(2) . ? O4 C61 1.327(17) . ? O4 C59 1.37(2) . ? N1 C1 1.298(18) . ? N1 C5 1.35(2) . ? N2 C34 1.322(18) . ? N2 C36 1.383(17) . ? N2 Co1 2.191(9) 1_556 ? N3 C39 1.319(16) . ? N3 C43 1.378(18) . ? N4 C72 1.356(18) . ? N4 C76 1.368(18) . ? N4 Co1 2.100(11) 1_556 ? C1 C2 1.41(2) . ? C2 C3 1.44(2) . ? C3 C4 1.35(2) . ? C3 C6 1.45(2) . ? C4 C5 1.38(2) . ? C6 C7 1.34(2) . ? C7 C8 1.51(2) . ? C8 C9 1.32(2) . ? C8 C17 1.36(2) . ? C9 C10 1.48(2) . ? C10 C11 1.39(2) . ? C10 C15 1.43(2) . ? C11 C12 1.35(2) . ? C12 C13 1.41(2) . ? C13 C14 1.40(2) . ? C14 C15 1.380(19) . ? C14 C22 1.52(2) . ? C15 C16 1.395(18) . ? C16 C17 1.373(19) . ? C18 C19 1.39(2) . ? C20 C21 1.461(19) . ? C22 C31 1.38(2) . ? C22 C23 1.447(18) . ? C23 C24 1.46(2) . ? C23 C28 1.44(2) . ? C24 C25 1.346(18) . ? C25 C26 1.451(19) . ? C26 C27 1.37(2) . ? C26 C32 1.52(2) . ? C27 C28 1.401(18) . ? C28 C29 1.41(2) . ? C29 C30 1.32(2) . ? C30 C31 1.46(2) . ? C32 C33 1.338(19) . ? C33 C38 1.437(19) . ? C34 C37 1.317(17) . ? C35 C38 1.366(19) . ? C35 C36 1.389(19) . ? C37 C38 1.394(19) . ? C39 C40 1.308(19) . ? C40 C41 1.30(2) . ? C41 C42 1.36(3) . ? C41 C44 1.56(3) . ? C42 C43 1.37(2) . ? C44 C45 1.27(2) . ? C45 C46 1.61(3) . ? C46 C47 1.31(2) . ? C46 C51 1.35(2) . ? C47 C48 1.44(2) . ? C48 C52 1.39(2) . ? C48 C49 1.48(2) . ? C49 C55 1.387(19) . ? C49 C50 1.48(2) . ? C50 C51 1.43(2) . ? C52 C53 1.34(2) . ? C53 C54 1.55(2) . ? C54 C55 1.270(19) . ? C55 C60 1.472(18) . ? C56 C57 1.51(3) . ? C58 C59 1.45(3) . ? C60 C61 1.44(2) . ? C60 C65 1.48(2) . ? C61 C62 1.40(2) . ? C62 C63 1.35(3) . ? C63 C64 1.46(3) . ? C64 C69 1.34(3) . ? C64 C65 1.43(2) . ? C65 C66 1.34(2) . ? C66 C67 1.39(2) . ? C67 C68 1.38(3) . ? C68 C69 1.37(4) . ? C68 C70 1.61(3) . ? C70 C71 1.225(17) . ? C71 C74 1.382(17) . ? C72 C73 1.43(2) . ? C73 C74 1.44(2) . ? C74 C75 1.41(2) . ? C75 C76 1.385(19) . ? Cl1 O7 1.414(17) . ? Cl1 O7 1.414(17) 2_557 ? Cl1 O8 1.475(15) . ? Cl1 O8 1.475(15) 2_557 ? C81 N5 1.46(3) . ? N5 C83 1.33(3) . ? N5 C82 1.44(3) . ? C85 C84 1.22(4) . ? C85 N6 1.29(4) . ? Cl2 O12 1.313(17) . ? Cl2 O13 1.346(17) . ? Cl2 O14 1.357(17) . ? Cl2 O15 1.353(17) . ? Cl3 O17 1.306(15) . ? Cl3 O16 1.348(16) . ? Cl3 O18 1.351(16) . ? Cl3 O19 1.360(16) . ? C88 N8 1.36(7) . ? C89 O20 1.34(6) . ? C89 N8 1.63(7) . ? C90 C91 1.31(5) . ? C91 N9 1.53(5) . ? C83 O11 1.31(3) . ? C94 N8 1.63(8) . ? N10 C93 1.48(5) . ? N10 C92 1.77(6) . ? C92 C93 0.83(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 N4 Co1 O6 89.8(4) 1_554 . ? N4 Co1 O5 87.7(4) 1_554 . ? O6 Co1 O5 177.3(4) . . ? N4 Co1 N1 177.4(5) 1_554 . ? O6 Co1 N1 92.8(5) . . ? O5 Co1 N1 89.8(5) . . ? N4 Co1 N3 90.9(5) 1_554 . ? O6 Co1 N3 90.0(4) . . ? O5 Co1 N3 89.1(4) . . ? N1 Co1 N3 89.5(5) . . ? N4 Co1 N2 90.8(4) 1_554 1_554 ? O6 Co1 N2 90.7(5) . 1_554 ? O5 Co1 N2 90.2(5) . 1_554 ? N1 Co1 N2 88.8(4) . 1_554 ? N3 Co1 N2 178.2(5) . 1_554 ? C13 O1 C18 119.6(12) . . ? C21 O2 C31 115.7(14) . . ? C54 O3 C56 122.8(14) . . ? C61 O4 C59 112.8(15) . . ? C1 N1 C5 116.1(14) . . ? C1 N1 Co1 121.4(11) . . ? C5 N1 Co1 122.4(12) . . ? C34 N2 C36 117.5(11) . . ? C34 N2 Co1 122.4(11) . 1_556 ? C36 N2 Co1 120.0(10) . 1_556 ? C39 N3 C43 112.6(14) . . ? C39 N3 Co1 127.6(11) . . ? C43 N3 Co1 119.5(12) . . ? C72 N4 C76 113.6(14) . . ? C72 N4 Co1 119.5(11) . 1_556 ? C76 N4 Co1 126.8(10) . 1_556 ? N1 C1 C2 121.9(15) . . ? C1 C2 C3 118.9(15) . . ? C4 C3 C6 121.3(17) . . ? C4 C3 C2 119.5(15) . . ? C6 C3 C2 118.9(15) . . ? C3 C4 C5 114.4(16) . . ? N1 C5 C4 128.8(15) . . ? C7 C6 C3 123.5(17) . . ? C6 C7 C8 123.4(16) . . ? C9 C8 C17 118.2(17) . . ? C9 C8 C7 115.2(16) . . ? C17 C8 C7 126.3(16) . . ? C8 C9 C10 123.9(17) . . ? C11 C10 C15 121.3(15) . . ? C11 C10 C9 123.7(17) . . ? C15 C10 C9 115.0(16) . . ? C12 C11 C10 121.6(16) . . ? C11 C12 C13 118.4(16) . . ? O1 C13 C14 117.0(14) . . ? O1 C13 C12 122.4(16) . . ? C14 C13 C12 120.7(14) . . ? C15 C14 C13 121.7(13) . . ? C15 C14 C22 119.8(15) . . ? C13 C14 C22 118.5(14) . . ? C14 C15 C16 124.7(14) . . ? C14 C15 C10 116.2(15) . . ? C16 C15 C10 119.0(14) . . ? C17 C16 C15 121.0(14) . . ? C8 C17 C16 122.9(16) . . ? C19 C18 O1 108.5(15) . . ? C20 C21 O2 100(3) . . ? C31 C22 C23 118.2(16) . . ? C31 C22 C14 119.0(14) . . ? C23 C22 C14 122.8(14) . . ? C22 C23 C24 121.6(14) . . ? C22 C23 C28 118.0(14) . . ? C24 C23 C28 120.3(13) . . ? C25 C24 C23 122.2(13) . . ? C24 C25 C26 116.6(14) . . ? C27 C26 C25 122.3(14) . . ? C27 C26 C32 119.9(14) . . ? C25 C26 C32 117.7(17) . . ? C26 C27 C28 122.8(15) . . ? C27 C28 C29 122.0(16) . . ? C27 C28 C23 115.8(16) . . ? C29 C28 C23 122.1(14) . . ? C30 C29 C28 118.3(18) . . ? C29 C30 C31 122.7(17) . . ? C22 C31 O2 117.9(16) . . ? C22 C31 C30 120.7(17) . . ? O2 C31 C30 121.3(17) . . ? C33 C32 C26 129.5(17) . . ? C32 C33 C38 124.1(14) . . ? C37 C34 N2 126.2(16) . . ? C38 C35 C36 127.5(14) . . ? N2 C36 C35 115.1(14) . . ? C34 C37 C38 120.8(15) . . ? C35 C38 C37 112.3(12) . . ? C35 C38 C33 121.4(14) . . ? C37 C38 C33 126.2(13) . . ? C40 C39 N3 127.1(16) . . ? C41 C40 C39 122.4(19) . . ? C40 C41 C42 114.5(18) . . ? C40 C41 C44 132(2) . . ? C42 C41 C44 113(2) . . ? C41 C42 C43 123.0(19) . . ? C42 C43 N3 120.1(16) . . ? C45 C44 C41 115(2) . . ? C44 C45 C46 118(2) . . ? C47 C46 C51 124.3(16) . . ? C47 C46 C45 111(2) . . ? C51 C46 C45 124.7(18) . . ? C46 C47 C48 122.4(19) . . ? C52 C48 C47 122(2) . . ? C52 C48 C49 120.7(17) . . ? C47 C48 C49 116.9(19) . . ? C55 C49 C50 125.4(15) . . ? C55 C49 C48 117.5(16) . . ? C50 C49 C48 117.0(16) . . ? C51 C50 C49 118.7(17) . . ? C46 C51 C50 120.2(16) . . ? C53 C52 C48 120(2) . . ? C52 C53 C54 118.3(18) . . ? C55 C54 O3 125.2(15) . . ? C55 C54 C53 121.0(15) . . ? O3 C54 C53 113.7(17) . . ? C54 C55 C49 122.7(15) . . ? C54 C55 C60 117.5(13) . . ? C49 C55 C60 119.9(13) . . ? O3 C56 C57 107(2) . . ? O4 C59 C58 110(2) . . ? C61 C60 C55 121.9(14) . . ? C61 C60 C65 119.1(14) . . ? C55 C60 C65 119.0(14) . . ? O4 C61 C62 128.6(19) . . ? O4 C61 C60 109.7(15) . . ? C62 C61 C60 121.4(16) . . ? C63 C62 C61 119.2(18) . . ? C62 C63 C64 123.8(17) . . ? C69 C64 C65 124(2) . . ? C69 C64 C63 118(2) . . ? C65 C64 C63 118.1(19) . . ? C66 C65 C64 117.4(17) . . ? C66 C65 C60 124.3(16) . . ? C64 C65 C60 118.3(17) . . ? C65 C66 C67 117.6(19) . . ? C68 C67 C66 125(2) . . ? C69 C68 C67 117(2) . . ? C69 C68 C70 133(3) . . ? C67 C68 C70 110(3) . . ? C64 C69 C68 119(3) . . ? C71 C70 C68 130(3) . . ? C70 C71 C74 124(3) . . ? N4 C72 C73 125.3(17) . . ? C74 C73 C72 114.9(18) . . ? C71 C74 C75 105.7(19) . . ? C71 C74 C73 131(2) . . ? C75 C74 C73 122.8(19) . . ? C76 C75 C74 113.0(16) . . ? N4 C76 C75 130.1(15) . . ? O7 Cl1 O7 114.9(17) . 2_557 ? O7 Cl1 O8 112.7(9) . . ? O7 Cl1 O8 103.3(10) 2_557 . ? O7 Cl1 O8 103.3(10) . 2_557 ? O7 Cl1 O8 112.7(9) 2_557 2_557 ? O8 Cl1 O8 110.1(12) . 2_557 ? C83 N5 C82 124(3) . . ? C83 N5 C81 118(3) . . ? C82 N5 C81 118(2) . . ? C84 C85 N6 157(4) . . ? O12 Cl2 O13 110.9(17) . . ? O12 Cl2 O14 112.0(18) . . ? O13 Cl2 O14 107.4(16) . . ? O12 Cl2 O15 109.0(17) . . ? O13 Cl2 O15 111.1(18) . . ? O14 Cl2 O15 106.4(17) . . ? O17 Cl3 O16 112.2(15) . . ? O17 Cl3 O18 111.4(15) . . ? O16 Cl3 O18 107.9(16) . . ? O17 Cl3 O19 116.1(15) . . ? O16 Cl3 O19 103.6(14) . . ? O18 Cl3 O19 105.0(15) . . ? O20 C89 N8 90(4) . . ? C90 C91 N9 153(5) . . ? O11 C83 N5 116(3) . . ? C88 N8 C89 152(6) . . ? C88 N8 C94 126(6) . . ? C89 N8 C94 78(5) . . ? C93 N10 C92 28(2) . . ? C93 C92 N10 56(4) . . ? C92 C93 N10 96(5) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 21.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.557 _refine_diff_density_min -0.483 _refine_diff_density_rms 0.089 # Attachment 'new6.cif' data_new6 _database_code_depnum_ccdc_archive 'CCDC 607394' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84.50 H90 Cl2 Mn N7 O18' _chemical_formula_weight 1617.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 41.7484(12) _cell_length_b 12.4528(4) _cell_length_c 19.8531(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.090(2) _cell_angle_gamma 90.00 _cell_volume 9917.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.94 _cell_measurement_theta_max 23.33 _exptl_crystal_description Bloc _exptl_crystal_colour 'Light pink' _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.083 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3396 _exptl_absorpt_coefficient_mu 0.247 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.6099 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 45100 _diffrn_reflns_av_R_equivalents 0.0784 _diffrn_reflns_av_sigmaI/netI 0.0886 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 23.33 _reflns_number_total 13790 _reflns_number_gt 7097 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0714P)^2^+86.8380P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(6) _refine_ls_number_reflns 13790 _refine_ls_number_parameters 943 _refine_ls_number_restraints 28 _refine_ls_R_factor_ref 0.2175 _refine_ls_R_factor_gt 0.1362 _refine_ls_wR_factor_ref 0.3294 _refine_ls_wR_factor_gt 0.2852 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.36313(6) 1.3305(2) 0.61089(10) 0.1013(7) Uani 1 1 d . . . O1 O 0.1773(3) 0.6610(8) 1.0253(5) 0.125(4) Uani 1 1 d . . . O2 O 0.1319(3) 0.8510(11) 0.9556(6) 0.136(4) Uani 1 1 d . . . O5 O 0.3219(2) 1.4498(8) 0.6006(4) 0.106(3) Uani 1 1 d . . . O3 O 0.5164(3) 2.0753(9) 1.2194(5) 0.131(4) Uani 1 1 d . . . O4 O 0.5697(3) 1.9120(9) 1.2026(5) 0.109(3) Uani 1 1 d . . . N1 N 0.3352(3) 1.2450(9) 1.5092(6) 0.097(3) Uani 1 1 d . . . N2 N 0.3375(3) 1.2329(9) 0.6732(5) 0.088(3) Uani 1 1 d . . . N3 N 0.3854(4) 1.4402(12) 1.5459(7) 0.120(4) Uani 1 1 d . . . N4 N 0.3925(4) 1.4164(12) 0.7072(6) 0.130(5) Uani 1 1 d . . . N5 N 0.4019(3) 1.2069(12) 0.6283(7) 0.139(6) Uani 1 1 d . . . C1 C 0.3529(4) 1.2035(16) 1.4637(7) 0.119(6) Uani 1 1 d . . . H1A H 0.3765 1.2080 1.4748 0.143 Uiso 1 1 calc R . . C2 C 0.3350(5) 1.1578(14) 1.4045(8) 0.123(6) Uani 1 1 d . . . H2A H 0.3466 1.1353 1.3720 0.148 Uiso 1 1 calc R . . C3 C 0.3012(4) 1.1407(11) 1.3868(8) 0.093(4) Uani 1 1 d . . . C4 C 0.2853(4) 1.1785(11) 1.4297(8) 0.092(4) Uani 1 1 d . . . H4A H 0.2618 1.1720 1.4191 0.111 Uiso 1 1 calc R . . C5 C 0.3039(4) 1.2302(12) 1.4936(8) 0.103(5) Uani 1 1 d . . . H5A H 0.2922 1.2543 1.5255 0.124 Uiso 1 1 calc R . . C6 C 0.2872(5) 1.0807(14) 1.3162(10) 0.123(6) Uani 1 1 d D . . H6A H 0.3016 1.0461 1.2934 0.148 Uiso 1 1 calc R . . C7 C 0.2568(5) 1.0797(15) 1.2908(10) 0.139(7) Uani 1 1 d D . . H7A H 0.2423 1.1172 1.3120 0.167 Uiso 1 1 calc R . . C8 C 0.2429(6) 1.0120(16) 1.2205(8) 0.171(14) Uani 1 1 d D . . C9 C 0.2113(7) 1.0288(16) 1.2009(10) 0.174(11) Uani 1 1 d D . . H9A H 0.2021 1.0739 1.2294 0.208 Uiso 1 1 calc R . . C10 C 0.1879(7) 0.9826(13) 1.1365(8) 0.136(7) Uani 1 1 d D . . C11 C 0.1520(8) 0.990(3) 1.1173(15) 0.211(12) Uani 1 1 d . . . H11A H 0.1411 1.0260 1.1469 0.253 Uiso 1 1 calc R . . C12 C 0.1325(5) 0.9411(18) 1.0514(14) 0.156(7) Uani 1 1 d . . . H12A H 0.1090 0.9484 1.0355 0.187 Uiso 1 1 calc R . . C13 C 0.1487(7) 0.8886(15) 1.0164(9) 0.134(7) Uani 1 1 d . . . C14 C 0.1836(5) 0.8790(10) 1.0311(6) 0.091(4) Uani 1 1 d . . . C15 C 0.2041(5) 0.9267(11) 1.0952(7) 0.102(5) Uani 1 1 d . . . C16 C 0.2378(5) 0.9026(12) 1.1220(8) 0.104(5) Uani 1 1 d . . . H16A H 0.2483 0.8539 1.0981 0.125 Uiso 1 1 calc R . . C17 C 0.2548(5) 0.9479(15) 1.1806(7) 0.129(7) Uani 1 1 d D . . H17A H 0.2780 0.9330 1.1957 0.155 Uiso 1 1 calc R . . C18 C 0.0977(7) 0.859(2) 0.9437(12) 0.191(11) Uani 1 1 d D . . H18A H 0.0905 0.9348 0.9369 0.229 Uiso 1 1 calc R . . H18B H 0.0909 0.8296 0.9840 0.229 Uiso 1 1 calc R . . C19 C 0.0821(11) 0.795(4) 0.8785(15) 0.42(3) Uani 1 1 d D . . H19A H 0.0580 0.7885 0.8722 0.635 Uiso 1 1 calc R . . H19B H 0.0920 0.7226 0.8831 0.635 Uiso 1 1 calc R . . H19C H 0.0861 0.8307 0.8377 0.635 Uiso 1 1 calc R . . C20 C 0.1381(8) 0.547(2) 1.027(3) 0.37(3) Uani 1 1 d . . . H20A H 0.1282 0.4757 1.0179 0.558 Uiso 1 1 calc R . . H20B H 0.1221 0.6012 1.0020 0.558 Uiso 1 1 calc R . . H20C H 0.1435 0.5620 1.0779 0.558 Uiso 1 1 calc R . . C21 C 0.1643(7) 0.5517(15) 1.0077(13) 0.180(10) Uani 1 1 d . . . H21A H 0.1592 0.5388 0.9566 0.216 Uiso 1 1 calc R . . H21B H 0.1807 0.4975 1.0326 0.216 Uiso 1 1 calc R . . C22 C 0.1944(4) 0.7008(13) 0.9817(8) 0.113(5) Uani 1 1 d . . . C23 C 0.2086(7) 0.6459(14) 0.9345(10) 0.159(9) Uani 1 1 d . . . H23A H 0.2036 0.5715 0.9284 0.191 Uiso 1 1 calc R . . C24 C 0.2267(6) 0.6830(18) 0.9001(11) 0.154(8) Uani 1 1 d . . . H24A H 0.2380 0.6375 0.8758 0.184 Uiso 1 1 calc R . . C25 C 0.2298(4) 0.7996(16) 0.8988(7) 0.115(6) Uani 1 1 d . . . C26 C 0.2454(5) 0.837(2) 0.8527(10) 0.154(7) Uani 1 1 d . . . H26A H 0.2516 0.7920 0.8197 0.185 Uiso 1 1 calc R . . C27 C 0.2521(6) 0.955(3) 0.8578(9) 0.147(9) Uani 1 1 d . . . C28 C 0.2419(6) 1.0120(13) 0.8982(12) 0.134(7) Uani 1 1 d . . . H28A H 0.2471 1.0865 0.9008 0.161 Uiso 1 1 calc R . . C29 C 0.2223(4) 0.9692(13) 0.9423(8) 0.113(5) Uani 1 1 d . . . H29A H 0.2128 1.0161 0.9693 0.136 Uiso 1 1 calc R . . C30 C 0.2178(4) 0.8634(11) 0.9443(7) 0.087(4) Uani 1 1 d . . . C31 C 0.1996(4) 0.8178(13) 0.9862(6) 0.097(4) Uani 1 1 d . . . C32 C 0.2701(6) 0.9925(18) 0.8052(11) 0.198(13) Uani 1 1 d D . . H32A H 0.2738 0.9432 0.7717 0.237 Uiso 1 1 calc R . . C33 C 0.2801(6) 1.0893(16) 0.8054(10) 0.162(10) Uani 1 1 d D . . H33A H 0.2742 1.1405 0.8354 0.194 Uiso 1 1 calc R . . C34 C 0.3304(3) 1.1265(10) 0.6670(7) 0.082(4) Uani 1 1 d . . . H34A H 0.3383 1.0876 0.6337 0.098 Uiso 1 1 calc R . . C35 C 0.3134(4) 1.0714(12) 0.7032(8) 0.097(5) Uani 1 1 d . . . H35A H 0.3086 0.9974 0.6939 0.116 Uiso 1 1 calc R . . C36 C 0.3025(4) 1.1257(14) 0.7564(9) 0.096(5) Uani 1 1 d . . . C37 C 0.3091(4) 1.2287(15) 0.7672(7) 0.116(5) Uani 1 1 d . . . H37A H 0.3034 1.2656 0.8041 0.139 Uiso 1 1 calc R . . C38 C 0.3247(5) 1.2822(12) 0.7236(9) 0.127(6) Uani 1 1 d . . . H38A H 0.3269 1.3579 0.7284 0.152 Uiso 1 1 calc R . . C39 C 0.4180(5) 1.4233(13) 1.5484(7) 0.117(5) Uani 1 1 d . . . H39A H 0.4303 1.3693 1.5784 0.140 Uiso 1 1 calc R . . C40 C 0.4352(5) 1.4900(16) 1.5036(9) 0.121(5) Uani 1 1 d . . . H40A H 0.4582 1.4836 1.5069 0.146 Uiso 1 1 calc R . . C41 C 0.4145(5) 1.5588(14) 1.4590(9) 0.106(5) Uani 1 1 d . . . C42 C 0.3826(6) 1.5652(18) 1.4581(9) 0.146(7) Uani 1 1 d . . . H42A H 0.3693 1.6148 1.4259 0.175 Uiso 1 1 calc R . . C43 C 0.3672(4) 1.5085(16) 1.4983(8) 0.131(7) Uani 1 1 d . . . H43A H 0.3440 1.5170 1.4928 0.158 Uiso 1 1 calc R . . C44 C 0.4276(5) 1.6311(18) 1.4086(9) 0.140(7) Uani 1 1 d . . . H44A H 0.4130 1.6776 1.3764 0.168 Uiso 1 1 calc R . . C45 C 0.4598(4) 1.6261(15) 1.4118(8) 0.120(6) Uani 1 1 d . . . H45A H 0.4739 1.5799 1.4451 0.144 Uiso 1 1 calc R . . C46 C 0.4742(5) 1.6912(14) 1.3645(7) 0.106(5) Uani 1 1 d . . . C47 C 0.5080(4) 1.6985(13) 1.3824(7) 0.106(5) Uani 1 1 d . . . H47A H 0.5209 1.6660 1.4245 0.127 Uiso 1 1 calc R . . C48 C 0.5245(4) 1.7552(13) 1.3381(6) 0.102(5) Uani 1 1 d . . . C49 C 0.5593(4) 1.7613(12) 1.3538(7) 0.099(4) Uani 1 1 d . . . H49A H 0.5726 1.7276 1.3950 0.118 Uiso 1 1 calc R . . C50 C 0.5742(4) 1.8144(13) 1.3112(7) 0.105(4) Uani 1 1 d . . . H50A H 0.5979 1.8193 1.3232 0.126 Uiso 1 1 calc R . . C51 C 0.5544(3) 1.8634(9) 1.2479(6) 0.073(3) Uani 1 1 d . . . C52 C 0.5209(4) 1.8580(10) 1.2307(6) 0.075(3) Uani 1 1 d . . . C53 C 0.5044(3) 1.8080(12) 1.2756(6) 0.088(4) Uani 1 1 d . . . C54 C 0.4707(3) 1.7988(13) 1.2610(7) 0.109(6) Uani 1 1 d . . . H54A H 0.4570 1.8335 1.2206 0.131 Uiso 1 1 calc R . . C55 C 0.4549(4) 1.7373(17) 1.3057(8) 0.130(6) Uani 1 1 d . . . H55A H 0.4314 1.7298 1.2934 0.156 Uiso 1 1 calc R . . C56 C 0.5972(5) 1.9761(17) 1.2258(9) 0.144(7) Uani 1 1 d . . . H56A H 0.5946 2.0224 1.2644 0.172 Uiso 1 1 calc R . . H56B H 0.6172 1.9307 1.2442 0.172 Uiso 1 1 calc R . . C57 C 0.6014(5) 2.0378(19) 1.1729(11) 0.168(9) Uani 1 1 d . . . H57A H 0.6209 2.0839 1.1903 0.252 Uiso 1 1 calc R . . H57B H 0.5815 2.0826 1.1548 0.252 Uiso 1 1 calc R . . H57C H 0.6046 1.9918 1.1353 0.252 Uiso 1 1 calc R . . C58 C 0.4784(8) 2.129(3) 1.2642(17) 0.32(2) Uani 1 1 d D . . H58A H 0.4669 2.1873 1.2814 0.475 Uiso 1 1 calc R . . H58B H 0.4864 2.0761 1.3015 0.475 Uiso 1 1 calc R . . H58C H 0.4629 2.0947 1.2238 0.475 Uiso 1 1 calc R . . C59 C 0.5085(6) 2.176(2) 1.2418(15) 0.204(11) Uani 1 1 d D . . H59A H 0.5019 2.2293 1.2035 0.245 Uiso 1 1 calc R . . H59B H 0.5262 2.2055 1.2816 0.245 Uiso 1 1 calc R . . C60 C 0.4985(4) 2.0175(14) 1.1610(9) 0.121(6) Uani 1 1 d . . . C61 C 0.4820(5) 2.0636(16) 1.0945(11) 0.147(7) Uani 1 1 d . . . H61A H 0.4825 2.1396 1.0906 0.176 Uiso 1 1 calc R . . C62 C 0.4667(5) 2.0106(14) 1.0399(8) 0.115(6) Uani 1 1 d . . . H62A H 0.4548 2.0474 0.9986 0.138 Uiso 1 1 calc R . . C63 C 0.4675(3) 1.9061(11) 1.0411(7) 0.081(4) Uani 1 1 d . . . C64 C 0.4519(3) 1.8436(13) 0.9806(6) 0.084(3) Uani 1 1 d . . . H64A H 0.4404 1.8800 0.9388 0.100 Uiso 1 1 calc R . . C65 C 0.4527(3) 1.7311(13) 0.9800(6) 0.084(4) Uani 1 1 d . . . C66 C 0.4691(3) 1.6761(11) 1.0454(6) 0.075(3) Uani 1 1 d . . . H66A H 0.4685 1.5999 1.0478 0.090 Uiso 1 1 calc R . . C67 C 0.4851(3) 1.7331(10) 1.1021(6) 0.067(3) Uani 1 1 d . . . H67A H 0.4977 1.6961 1.1427 0.080 Uiso 1 1 calc R . . C68 C 0.4837(3) 1.8494(11) 1.1033(5) 0.068(3) Uani 1 1 d . . . C69 C 0.5003(3) 1.9122(12) 1.1626(6) 0.081(4) Uani 1 1 d . . . C70 C 0.4378(3) 1.6754(13) 0.9150(7) 0.090(4) Uani 1 1 d . . . H70A H 0.4265 1.7181 0.8759 0.108 Uiso 1 1 calc R . . C71 C 0.4383(3) 1.5719(15) 0.9050(7) 0.103(5) Uani 1 1 d . . . H71A H 0.4475 1.5284 0.9450 0.123 Uiso 1 1 calc R . . C72 C 0.4091(5) 1.3528(17) 0.7681(11) 0.194(11) Uani 1 1 d . . . H72A H 0.4101 1.2768 0.7650 0.233 Uiso 1 1 calc R . . C73 C 0.4238(5) 1.4062(14) 0.8323(7) 0.149(8) Uani 1 1 d . . . H73A H 0.4326 1.3651 0.8736 0.179 Uiso 1 1 calc R . . C74 C 0.4256(4) 1.5156(13) 0.8359(8) 0.121(6) Uani 1 1 d . . . C75 C 0.4092(4) 1.5718(14) 0.7703(8) 0.118(6) Uani 1 1 d . . . H75A H 0.4086 1.6481 0.7696 0.142 Uiso 1 1 calc R . . C76 C 0.3955(4) 1.5192(14) 0.7139(7) 0.112(6) Uani 1 1 d . . . H76A H 0.3868 1.5606 0.6727 0.135 Uiso 1 1 calc R . . C77 C 0.4333(19) 1.121(5) 0.639(4) 0.54(5) Uiso 1 1 d D . . C78 C 0.4510(12) 1.040(4) 0.611(3) 0.39(3) Uiso 1 1 d D . . H78A H 0.4537 0.9751 0.6399 0.581 Uiso 1 1 calc R . . H78B H 0.4730 1.0672 0.6105 0.581 Uiso 1 1 calc R . . H78C H 0.4382 1.0220 0.5626 0.581 Uiso 1 1 calc R . . Cl1 Cl 0.18086(17) 1.2437(5) 0.3535(5) 0.164(2) Uani 1 1 d . . . O6 O 0.1624(5) 1.314(3) 0.356(3) 0.65(5) Uani 1 1 d . . . O7 O 0.1990(6) 1.2867(15) 0.3144(12) 0.270(11) Uani 1 1 d D . . Cl2 Cl 0.0000 1.8305(5) 1.0000 0.181(3) Uani 1 2 d S . . O8 O 0.1972(6) 1.1971(19) 0.4098(12) 0.290(12) Uani 1 1 d D . . O9 O 0.1714(10) 1.132(4) 0.3120(18) 0.35(2) Uiso 1 1 d D . . O10 O 0.0285(3) 1.7670(9) 1.0305(10) 0.194(7) Uani 1 1 d . . . O11 O -0.0118(4) 1.8968(15) 1.0489(8) 0.200(6) Uiso 1 1 d . . . Cl3 Cl 0.2513(4) 1.4756(13) 0.4575(8) 0.241 Uiso 0.50 1 d PD . . O12 O 0.2738(6) 1.5378(19) 0.4423(14) 0.201(12) Uiso 0.50 1 d PD . . O13 O 0.2594(6) 1.4383(19) 0.5241(9) 0.173(10) Uiso 0.50 1 d PD . . O14 O 0.2204(5) 1.512(2) 0.4361(14) 0.207 Uiso 0.50 1 d PD . . O15 O 0.2526(6) 1.3795(17) 0.4190(12) 0.207 Uiso 0.50 1 d PD . . O101 O 0.336(3) 1.384(10) 0.285(5) 0.22(5) Uiso 0.25 1 d P . . O102 O 0.0257(13) 0.449(4) 0.525(3) 0.167(18) Uiso 0.25 1 d P . . O103 O -0.0088(13) 0.783(4) 0.448(2) 0.21(2) Uiso 0.50 1 d P . . O104 O 0.2427(11) 1.295(3) 0.613(2) 0.21(2) Uiso 0.50 1 d PD . . N6 N 0.1373(16) 0.811(5) 0.744(3) 0.22(3) Uiso 0.50 1 d PD . . N7 N 0.1614(19) 1.315(7) 0.692(4) 0.28(4) Uiso 0.50 1 d P . . O18 O 0.3154(5) 0.7600(18) 0.0500(12) 0.266(9) Uiso 1 1 d . . . O16 O 0.3781(8) 0.978(3) 0.5572(16) 0.191(11) Uiso 0.50 1 d P . . O17 O 0.0083(8) 1.003(3) 0.7659(17) 0.256(14) Uiso 1 1 d D . . N8 N 0.3932(9) 0.858(4) 0.112(2) 0.196(14) Uiso 0.50 1 d P . . C81 C 0.1340(12) 0.618(4) 0.773(2) 0.185(17) Uiso 0.50 1 d PD . . C82 C 0.1240(11) 0.720(4) 0.732(2) 0.167(15) Uiso 0.50 1 d PD . . C83 C 0.1679(10) 1.233(4) 0.723(2) 0.157(15) Uiso 0.50 1 d PD . . C84 C 0.1995(17) 1.239(10) 0.705(4) 0.35(6) Uiso 0.50 1 d PD . . C85 C 0.3535(14) 0.891(5) 0.510(3) 0.21(2) Uiso 0.50 1 d P . . C86 C 0.0002(9) 0.945(3) 0.6983(19) 0.294(16) Uiso 1 1 d D . . C87 C 0.3230(9) 0.764(3) -0.022(2) 0.324(19) Uiso 1 1 d D . . C89 C 0.3897(10) 0.747(6) 0.084(3) 0.23(2) Uiso 0.50 1 d PD . . C88 C 0.3960(11) 0.649(4) 0.115(2) 0.173(16) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.1162(16) 0.0971(14) 0.0773(12) -0.0003(13) 0.0046(11) -0.0329(14) O1 0.196(11) 0.087(7) 0.110(8) 0.018(6) 0.072(8) -0.021(7) O2 0.119(9) 0.151(10) 0.132(10) -0.026(9) 0.027(7) 0.003(8) O5 0.120(7) 0.109(7) 0.084(6) -0.023(6) 0.022(5) -0.013(6) O3 0.195(12) 0.092(7) 0.095(7) -0.024(6) 0.024(7) 0.046(8) O4 0.116(8) 0.143(8) 0.064(6) -0.031(6) 0.017(6) -0.045(7) N1 0.116(10) 0.089(8) 0.072(7) -0.003(6) 0.000(7) -0.023(7) N2 0.125(9) 0.085(8) 0.053(6) -0.028(6) 0.021(6) -0.010(7) N3 0.101(10) 0.128(11) 0.126(11) -0.009(9) 0.026(9) -0.038(9) N4 0.165(12) 0.115(11) 0.087(9) 0.035(8) -0.006(8) -0.063(10) N5 0.094(8) 0.147(12) 0.138(11) 0.050(9) -0.031(8) -0.071(8) C1 0.124(12) 0.175(16) 0.058(9) 0.010(10) 0.025(9) -0.022(12) C2 0.157(17) 0.128(14) 0.079(11) -0.030(10) 0.024(11) -0.023(12) C3 0.107(12) 0.074(9) 0.090(11) 0.006(8) 0.015(10) 0.000(9) C4 0.079(9) 0.090(10) 0.100(11) 0.006(9) 0.014(9) 0.005(8) C5 0.087(10) 0.102(11) 0.104(11) -0.037(9) -0.003(9) -0.011(9) C6 0.116(13) 0.109(13) 0.144(17) 0.047(12) 0.035(13) 0.005(12) C7 0.163(18) 0.117(14) 0.130(16) 0.046(12) 0.027(14) -0.012(14) C8 0.28(3) 0.149(19) 0.034(9) 0.022(11) -0.047(14) -0.13(2) C9 0.32(4) 0.104(14) 0.084(15) -0.044(12) 0.031(18) -0.03(2) C10 0.23(2) 0.092(11) 0.067(10) -0.014(9) 0.016(13) 0.008(14) C11 0.18(2) 0.29(3) 0.17(2) -0.01(2) 0.07(2) 0.08(2) C12 0.142(17) 0.17(2) 0.162(19) -0.045(17) 0.055(16) 0.011(15) C13 0.18(2) 0.137(15) 0.083(12) -0.072(10) 0.031(13) -0.014(14) C14 0.148(14) 0.073(9) 0.049(8) -0.007(7) 0.024(9) -0.015(9) C15 0.205(18) 0.061(8) 0.047(8) -0.003(7) 0.046(11) -0.006(10) C16 0.143(14) 0.081(10) 0.080(11) 0.009(9) 0.018(10) 0.000(10) C17 0.186(17) 0.159(17) 0.035(8) -0.026(9) 0.017(10) -0.073(14) C18 0.19(2) 0.26(3) 0.155(18) -0.10(2) 0.090(17) -0.08(2) C19 0.50(8) 0.55(9) 0.34(5) 0.07(5) 0.30(6) -0.15(6) C20 0.27(4) 0.15(2) 0.79(9) -0.05(3) 0.31(5) -0.12(2) C21 0.25(3) 0.097(14) 0.24(2) -0.061(14) 0.14(2) -0.086(16) C22 0.148(14) 0.095(12) 0.083(10) 0.022(9) 0.012(10) -0.001(10) C23 0.30(3) 0.078(12) 0.147(17) -0.046(11) 0.141(19) 0.011(14) C24 0.22(2) 0.128(18) 0.150(18) -0.052(14) 0.111(17) 0.003(16) C25 0.157(14) 0.139(17) 0.071(9) 0.006(10) 0.069(9) -0.036(12) C26 0.191(18) 0.138(16) 0.167(18) -0.014(16) 0.105(15) -0.014(16) C27 0.186(19) 0.21(3) 0.052(10) 0.023(13) 0.049(11) -0.013(19) C28 0.20(2) 0.070(11) 0.122(16) 0.005(11) 0.033(15) -0.002(11) C29 0.164(15) 0.093(12) 0.086(10) 0.014(9) 0.042(10) -0.017(11) C30 0.117(11) 0.068(10) 0.089(10) 0.008(8) 0.048(9) -0.016(8) C31 0.133(11) 0.092(11) 0.055(7) -0.015(8) 0.009(8) -0.020(10) C32 0.25(3) 0.15(2) 0.129(19) -0.063(17) -0.053(18) 0.08(2) C33 0.24(2) 0.085(12) 0.111(15) -0.040(12) -0.030(15) 0.004(14) C34 0.092(9) 0.061(8) 0.074(8) -0.008(7) -0.007(7) -0.015(7) C35 0.118(12) 0.074(9) 0.076(10) 0.014(8) -0.010(9) -0.025(9) C36 0.095(10) 0.105(13) 0.093(12) 0.027(10) 0.033(9) -0.030(9) C37 0.164(15) 0.114(14) 0.080(10) -0.007(10) 0.052(10) -0.044(12) C38 0.184(17) 0.078(10) 0.107(12) 0.003(9) 0.023(12) -0.050(11) C39 0.144(15) 0.119(13) 0.086(10) 0.023(9) 0.029(11) -0.027(12) C40 0.119(13) 0.142(15) 0.102(12) -0.037(12) 0.028(11) -0.023(12) C41 0.082(11) 0.110(12) 0.103(12) -0.014(10) -0.015(10) -0.014(10) C42 0.137(17) 0.20(2) 0.089(12) 0.040(13) 0.004(11) -0.033(15) C43 0.105(12) 0.190(18) 0.094(11) 0.083(12) 0.019(10) -0.005(12) C44 0.114(14) 0.21(2) 0.096(12) -0.017(13) 0.024(11) -0.035(14) C45 0.095(12) 0.173(17) 0.078(10) -0.003(10) 0.001(9) -0.021(11) C46 0.119(13) 0.163(15) 0.048(8) 0.032(9) 0.042(9) 0.028(11) C47 0.121(13) 0.147(14) 0.053(8) 0.031(9) 0.029(9) 0.019(11) C48 0.110(12) 0.130(12) 0.053(8) -0.019(8) 0.000(8) 0.039(10) C49 0.099(11) 0.109(11) 0.069(9) 0.013(8) -0.008(8) 0.008(9) C50 0.097(10) 0.120(12) 0.086(9) -0.010(10) 0.004(8) -0.029(10) C51 0.079(9) 0.071(9) 0.054(7) -0.024(6) -0.008(7) 0.012(7) C52 0.101(10) 0.079(9) 0.050(7) -0.004(6) 0.029(7) 0.018(7) C53 0.091(9) 0.119(12) 0.056(7) -0.020(8) 0.023(7) 0.045(9) C54 0.081(9) 0.180(17) 0.080(8) 0.030(10) 0.043(8) 0.053(10) C55 0.104(11) 0.22(2) 0.079(10) -0.025(12) 0.050(9) 0.021(13) C56 0.136(15) 0.178(18) 0.095(12) -0.023(13) -0.004(11) -0.062(14) C57 0.126(15) 0.23(2) 0.139(17) 0.019(17) 0.016(13) -0.073(15) C58 0.38(5) 0.32(4) 0.35(4) -0.14(3) 0.25(4) -0.21(4) C59 0.19(2) 0.17(2) 0.30(3) 0.01(2) 0.14(2) -0.010(18) C60 0.152(15) 0.089(12) 0.105(13) -0.008(10) 0.008(11) 0.047(11) C61 0.179(18) 0.104(13) 0.134(16) 0.017(14) 0.006(15) 0.005(13) C62 0.193(18) 0.081(12) 0.065(10) 0.010(9) 0.024(11) 0.019(11) C63 0.097(10) 0.071(10) 0.086(10) 0.010(8) 0.045(8) 0.013(7) C64 0.084(8) 0.107(12) 0.063(8) 0.010(9) 0.027(6) -0.003(8) C65 0.066(8) 0.124(12) 0.071(9) 0.016(9) 0.034(7) -0.020(8) C66 0.064(8) 0.093(9) 0.063(8) 0.006(8) 0.009(6) 0.003(7) C67 0.065(7) 0.079(8) 0.053(7) 0.015(6) 0.009(6) 0.001(6) C68 0.067(7) 0.096(10) 0.045(6) 0.000(7) 0.024(5) 0.011(7) C69 0.097(9) 0.093(10) 0.063(8) 0.003(8) 0.038(7) 0.016(8) C70 0.080(9) 0.119(12) 0.065(8) -0.019(8) 0.011(7) -0.052(9) C71 0.091(10) 0.138(14) 0.061(8) 0.004(9) -0.008(7) -0.054(10) C72 0.22(2) 0.144(17) 0.160(17) 0.056(16) -0.048(15) -0.114(17) C73 0.22(2) 0.122(14) 0.059(9) 0.016(9) -0.035(11) -0.079(14) C74 0.113(11) 0.114(13) 0.092(11) 0.020(10) -0.046(9) -0.074(10) C75 0.128(12) 0.133(13) 0.084(10) 0.013(10) 0.012(9) -0.079(11) C76 0.120(12) 0.119(13) 0.068(9) 0.018(9) -0.025(8) -0.067(10) Cl1 0.132(4) 0.125(5) 0.222(7) 0.029(5) 0.029(4) 0.023(4) O6 0.162(16) 0.42(4) 1.41(12) 0.66(6) 0.27(4) 0.15(2) O7 0.36(3) 0.163(17) 0.33(3) 0.047(16) 0.17(2) 0.071(17) Cl2 0.177(7) 0.055(3) 0.331(11) 0.000 0.105(7) 0.000 O8 0.34(3) 0.28(2) 0.25(2) 0.13(2) 0.079(19) 0.13(2) O10 0.106(8) 0.093(8) 0.37(2) -0.076(11) 0.039(11) 0.015(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 N5 2.192(16) . ? Mn1 N2 2.212(11) . ? Mn1 N4 2.238(13) . ? Mn1 O5 2.241(10) . ? Mn1 N3 2.248(14) 1_554 ? Mn1 N1 2.293(11) 1_554 ? O1 C22 1.357(18) . ? O1 C21 1.470(18) . ? O2 C13 1.303(17) . ? O2 C18 1.38(2) . ? O3 C59 1.40(2) . ? O3 C60 1.393(18) . ? O4 C56 1.369(17) . ? O4 C51 1.379(15) . ? N1 C5 1.270(16) . ? N1 C1 1.413(18) . ? N1 Mn1 2.294(11) 1_556 ? N2 C34 1.355(15) . ? N2 C38 1.399(19) . ? N3 C43 1.341(18) . ? N3 C39 1.368(19) . ? N3 Mn1 2.247(14) 1_556 ? N4 C76 1.290(18) . ? N4 C72 1.45(2) . ? N5 C77 1.66(6) . ? C1 C2 1.332(19) . ? C2 C3 1.37(2) . ? C3 C4 1.304(18) . ? C3 C6 1.55(2) . ? C4 C5 1.442(17) . ? C6 C7 1.230(15) . ? C7 C8 1.60(3) . ? C8 C9 1.29(3) . ? C8 C17 1.317(18) . ? C9 C10 1.492(17) . ? C10 C15 1.39(2) . ? C10 C11 1.44(3) . ? C11 C12 1.47(3) . ? C12 C13 1.27(2) . ? C13 C14 1.41(2) . ? C14 C15 1.450(19) . ? C14 C31 1.467(19) . ? C15 C16 1.39(2) . ? C16 C17 1.311(19) . ? C18 C19 1.508(19) . ? C20 C21 1.26(3) . ? C22 C23 1.42(2) . ? C22 C31 1.47(2) . ? C23 C24 1.24(2) . ? C24 C25 1.46(2) . ? C25 C26 1.34(2) . ? C25 C30 1.398(19) . ? C26 C27 1.50(3) . ? C27 C28 1.23(2) . ? C27 C32 1.52(3) . ? C28 C29 1.46(2) . ? C29 C30 1.333(18) . ? C30 C31 1.392(18) . ? C32 C33 1.277(17) . ? C33 C36 1.59(3) . ? C34 C35 1.332(17) . ? C35 C36 1.43(2) . ? C36 C37 1.32(2) . ? C37 C38 1.389(19) . ? C39 C40 1.53(2) . ? C40 C41 1.36(2) . ? C41 C42 1.33(2) . ? C41 C44 1.55(2) . ? C42 C43 1.36(2) . ? C44 C45 1.33(2) . ? C45 C46 1.49(2) . ? C46 C47 1.361(18) . ? C46 C55 1.349(19) . ? C47 C48 1.44(2) . ? C48 C49 1.399(19) . ? C48 C53 1.449(17) . ? C49 C50 1.354(18) . ? C50 C51 1.436(17) . ? C51 C52 1.346(16) . ? C52 C53 1.415(17) . ? C52 C69 1.542(16) . ? C53 C54 1.360(17) . ? C54 C55 1.46(2) . ? C56 C57 1.35(2) . ? C58 C59 1.559(17) . ? C60 C69 1.313(18) . ? C60 C61 1.43(2) . ? C61 C62 1.28(2) . ? C62 C63 1.302(18) . ? C63 C68 1.421(16) . ? C63 C64 1.428(17) . ? C64 C65 1.401(19) . ? C65 C70 1.445(17) . ? C65 C66 1.461(16) . ? C66 C67 1.342(15) . ? C67 C68 1.450(17) . ? C68 C69 1.423(16) . ? C70 C71 1.306(19) . ? C71 C74 1.50(2) . ? C72 C73 1.42(2) . ? C73 C74 1.36(2) . ? C74 C75 1.470(19) . ? C75 C76 1.286(18) . ? C77 C78 1.45(2) . ? Cl1 O6 1.18(3) . ? Cl1 O8 1.276(18) . ? Cl1 O7 1.34(2) . ? Cl1 O9 1.61(4) . ? Cl2 O10 1.417(13) 2_557 ? Cl2 O10 1.417(12) . ? Cl2 O11 1.459(17) . ? Cl2 O11 1.460(17) 2_557 ? Cl3 O12 1.316(15) . ? Cl3 O14 1.318(15) . ? Cl3 O13 1.354(14) . ? Cl3 O15 1.428(15) . ? N6 C82 1.26(2) . ? N7 C83 1.19(9) . ? N7 C84 1.81(11) . ? O18 C87 1.55(4) . ? O16 C85 1.61(6) . ? O17 C86 1.482(19) . ? N8 C89 1.49(7) . ? C81 C82 1.51(2) . ? C83 C84 1.470(15) . ? C89 C88 1.35(6) . ? 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 N5 Mn1 N2 88.7(4) . . ? N5 Mn1 N4 89.8(5) . . ? N2 Mn1 N4 91.2(4) . . ? N5 Mn1 O5 174.9(4) . . ? N2 Mn1 O5 86.4(4) . . ? N4 Mn1 O5 89.2(5) . . ? N5 Mn1 N3 96.5(5) . 1_554 ? N2 Mn1 N3 174.8(6) . 1_554 ? N4 Mn1 N3 89.1(5) . 1_554 ? O5 Mn1 N3 88.5(5) . 1_554 ? N5 Mn1 N1 89.2(5) . 1_554 ? N2 Mn1 N1 91.8(4) . 1_554 ? N4 Mn1 N1 176.9(5) . 1_554 ? O5 Mn1 N1 92.1(4) . 1_554 ? N3 Mn1 N1 88.1(5) 1_554 1_554 ? C22 O1 C21 114.2(14) . . ? C13 O2 C18 113.5(17) . . ? C59 O3 C60 127.5(16) . . ? C56 O4 C51 122.3(12) . . ? C5 N1 C1 118.3(13) . . ? C5 N1 Mn1 121.3(11) . 1_556 ? C1 N1 Mn1 120.3(11) . 1_556 ? C34 N2 C38 112.2(12) . . ? C34 N2 Mn1 127.8(10) . . ? C38 N2 Mn1 119.9(9) . . ? C43 N3 C39 119.1(15) . . ? C43 N3 Mn1 123.2(12) . 1_556 ? C39 N3 Mn1 116.9(12) . 1_556 ? C76 N4 C72 116.4(14) . . ? C76 N4 Mn1 125.3(10) . . ? C72 N4 Mn1 118.2(11) . . ? C77 N5 Mn1 175(3) . . ? C2 C1 N1 117.1(16) . . ? C1 C2 C3 125.3(17) . . ? C4 C3 C2 116.6(16) . . ? C4 C3 C6 129.2(16) . . ? C2 C3 C6 114.2(16) . . ? C3 C4 C5 119.3(14) . . ? N1 C5 C4 123.2(15) . . ? C7 C6 C3 118(2) . . ? C6 C7 C8 117(2) . . ? C9 C8 C17 116.3(17) . . ? C9 C8 C7 106(2) . . ? C17 C8 C7 138(2) . . ? C8 C9 C10 125(2) . . ? C15 C10 C11 121.1(18) . . ? C15 C10 C9 113(2) . . ? C11 C10 C9 126(2) . . ? C10 C11 C12 119(2) . . ? C13 C12 C11 117(2) . . ? C12 C13 O2 117(3) . . ? C12 C13 C14 127.1(19) . . ? O2 C13 C14 114.9(17) . . ? C13 C14 C15 118.2(15) . . ? C13 C14 C31 122.5(13) . . ? C15 C14 C31 119.3(16) . . ? C10 C15 C16 119.4(15) . . ? C10 C15 C14 117.3(18) . . ? C16 C15 C14 122.3(16) . . ? C17 C16 C15 119.2(17) . . ? C8 C17 C16 126.4(19) . . ? O2 C18 C19 107(2) . . ? C20 C21 O1 105(2) . . ? O1 C22 C23 129.5(16) . . ? O1 C22 C31 114.7(15) . . ? C23 C22 C31 115.8(16) . . ? C24 C23 C22 128.0(18) . . ? C23 C24 C25 116.9(18) . . ? C26 C25 C30 125.0(18) . . ? C26 C25 C24 115(2) . . ? C30 C25 C24 120.2(14) . . ? C25 C26 C27 114.2(18) . . ? C28 C27 C32 127(3) . . ? C28 C27 C26 121.2(19) . . ? C32 C27 C26 112(2) . . ? C27 C28 C29 122.3(19) . . ? C30 C29 C28 119.2(16) . . ? C29 C30 C31 121.7(15) . . ? C29 C30 C25 117.6(14) . . ? C31 C30 C25 120.5(13) . . ? C30 C31 C14 124.5(14) . . ? C30 C31 C22 117.6(14) . . ? C14 C31 C22 117.8(14) . . ? C33 C32 C27 121(2) . . ? C32 C33 C36 121(2) . . ? C35 C34 N2 126.1(14) . . ? C34 C35 C36 118.8(13) . . ? C37 C36 C35 119.0(14) . . ? C37 C36 C33 108.1(17) . . ? C35 C36 C33 132.8(16) . . ? C36 C37 C38 118.7(16) . . ? C37 C38 N2 124.9(14) . . ? N3 C39 C40 121.2(16) . . ? C41 C40 C39 114.1(17) . . ? C42 C41 C40 119.9(19) . . ? C42 C41 C44 119.1(17) . . ? C40 C41 C44 121.0(17) . . ? C43 C42 C41 126.9(19) . . ? C42 C43 N3 118.5(17) . . ? C45 C44 C41 118.4(18) . . ? C44 C45 C46 121.7(17) . . ? C47 C46 C55 121.6(14) . . ? C47 C46 C45 116.4(14) . . ? C55 C46 C45 122.0(16) . . ? C46 C47 C48 120.7(13) . . ? C49 C48 C47 122.1(13) . . ? C49 C48 C53 119.1(15) . . ? C47 C48 C53 118.8(14) . . ? C50 C49 C48 121.0(14) . . ? C49 C50 C51 120.0(13) . . ? C52 C51 O4 119.5(11) . . ? C52 C51 C50 120.6(14) . . ? O4 C51 C50 119.8(12) . . ? C51 C52 C53 121.0(12) . . ? C51 C52 C69 119.3(12) . . ? C53 C52 C69 119.7(12) . . ? C54 C53 C52 124.0(12) . . ? C54 C53 C48 117.7(14) . . ? C52 C53 C48 118.1(12) . . ? C53 C54 C55 122.0(13) . . ? C46 C55 C54 119.2(14) . . ? C57 C56 O4 110.3(15) . . ? O3 C59 C58 92.0(19) . . ? C69 C60 O3 118.9(15) . . ? C69 C60 C61 115.6(16) . . ? O3 C60 C61 124.8(16) . . ? C62 C61 C60 125.1(18) . . ? C63 C62 C61 119.7(17) . . ? C62 C63 C68 121.1(15) . . ? C62 C63 C64 121.7(15) . . ? C68 C63 C64 117.2(12) . . ? C65 C64 C63 123.1(12) . . ? C64 C65 C70 118.8(13) . . ? C64 C65 C66 117.9(12) . . ? C70 C65 C66 123.3(14) . . ? C67 C66 C65 120.0(13) . . ? C66 C67 C68 121.9(11) . . ? C69 C68 C63 116.8(12) . . ? C69 C68 C67 123.4(11) . . ? C63 C68 C67 119.6(11) . . ? C60 C69 C68 121.2(13) . . ? C60 C69 C52 118.2(13) . . ? C68 C69 C52 120.6(12) . . ? C71 C70 C65 126.0(15) . . ? C70 C71 C74 125.7(14) . . ? C73 C72 N4 118.7(17) . . ? C74 C73 C72 121.3(15) . . ? C73 C74 C75 115.0(13) . . ? C73 C74 C71 121.0(14) . . ? C75 C74 C71 123.2(15) . . ? C76 C75 C74 121.0(16) . . ? C75 C76 N4 127.0(15) . . ? C78 C77 N5 150(6) . . ? O6 Cl1 O8 120(3) . . ? O6 Cl1 O7 102.4(15) . . ? O8 Cl1 O7 116.0(15) . . ? O6 Cl1 O9 126(2) . . ? O8 Cl1 O9 93.0(15) . . ? O7 Cl1 O9 98.4(18) . . ? O10 Cl2 O10 112.2(10) 2_557 . ? O10 Cl2 O11 101.7(9) 2_557 . ? O10 Cl2 O11 115.4(9) . . ? O10 Cl2 O11 115.4(9) 2_557 2_557 ? O10 Cl2 O11 101.7(9) . 2_557 ? O11 Cl2 O11 111.1(14) . 2_557 ? O12 Cl3 O14 114.9(16) . . ? O12 Cl3 O13 115.0(15) . . ? O14 Cl3 O13 113.0(15) . . ? O12 Cl3 O15 103.6(14) . . ? O14 Cl3 O15 107.0(15) . . ? O13 Cl3 O15 101.4(14) . . ? C83 N7 C84 54(4) . . ? N6 C82 C81 128(5) . . ? N7 C83 C84 85(6) . . ? C83 C84 N7 41(4) . . ? C88 C89 N8 133(4) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 23.33 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.631 _refine_diff_density_min -0.527 _refine_diff_density_rms 0.077