data_at320 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C73 H68 Co5 N4 O16, 8.5(C H4 O)' _chemical_formula_sum 'C81.50 H102 Co5 N4 O24.50' _chemical_formula_weight 1824.32 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' '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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.093(2) _cell_length_b 18.4290(14) _cell_length_c 29.824(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.442(11) _cell_angle_gamma 90.00 _cell_volume 8842.1(17) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 14439 _cell_measurement_theta_min 1.30 _cell_measurement_theta_max 22.59 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3800 _exptl_absorpt_coefficient_mu 0.992 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.909 _exptl_absorpt_correction_T_max 0.961 _exptl_absorpt_process_details 'XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate ( 34 cm diameter )' _diffrn_detector_type 'STOE' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41941 _diffrn_reflns_av_R_equivalents 0.1169 _diffrn_reflns_av_sigmaI/netI 0.1866 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 25.20 _reflns_number_total 15644 _reflns_number_gt 6434 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0500P)^2^] 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_number_reflns 15644 _refine_ls_number_parameters 1063 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2023 _refine_ls_R_factor_gt 0.0850 _refine_ls_wR_factor_ref 0.1884 _refine_ls_wR_factor_gt 0.1528 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.001 _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 Co1 Co 0.23135(8) 0.27126(7) 0.39292(4) 0.0527(3) Uani 1 1 d . A . Co3 Co 0.33350(8) 0.40354(7) 0.31353(4) 0.0527(3) Uani 1 1 d . . . Co5 Co 0.49774(7) 0.53775(7) 0.27551(4) 0.0504(3) Uani 1 1 d . . . Co2 Co 0.40357(8) 0.33097(7) 0.39154(4) 0.0542(4) Uani 1 1 d . A . Co4 Co 0.45267(8) 0.48510(7) 0.36622(4) 0.0531(4) Uani 1 1 d . A . O1 O 0.3045(3) 0.3010(3) 0.3462(2) 0.0519(16) Uani 1 1 d . A . O2 O 0.4560(4) 0.2259(4) 0.3855(2) 0.0666(19) Uani 1 1 d . A . H2 H 0.5068 0.2208 0.3920 0.100 Uiso 1 1 calc R . . O3 O 0.1637(4) 0.2383(4) 0.4398(2) 0.0613(17) Uani 1 1 d . . . O4 O 0.3451(4) 0.4351(3) 0.3821(2) 0.0500(16) Uani 1 1 d . A . O5 O 0.3171(4) 0.3015(3) 0.4348(2) 0.0553(16) Uani 1 1 d . . . O6 O 0.1489(4) 0.2413(3) 0.3502(2) 0.0543(17) Uani 1 1 d . . . O7 O 0.4547(3) 0.3769(3) 0.3372(2) 0.0530(16) Uani 1 1 d . A . O8 O 0.5512(3) 0.5129(3) 0.3306(2) 0.0550(16) Uani 1 1 d . A . O9 O 0.4438(4) 0.5632(3) 0.2208(2) 0.0549(17) Uani 1 1 d . A . O10 O 0.3938(3) 0.5072(3) 0.3017(2) 0.0524(16) Uani 1 1 d . A . O11 O 0.4229(4) 0.5899(4) 0.3888(2) 0.0600(17) Uani 1 1 d . A . H11 H 0.4686 0.6072 0.3980 0.090 Uiso 1 1 calc R . . O12 O 0.5998(4) 0.5724(3) 0.2537(2) 0.0556(17) Uani 1 1 d . A . O14 O 0.5182(4) 0.4705(4) 0.4249(2) 0.068(2) Uani 1 1 d . . . O15 O 0.4916(4) 0.3530(4) 0.4401(2) 0.0627(18) Uani 1 1 d . . . N1 N 0.2862(4) 0.1802(4) 0.3868(3) 0.0492(19) Uani 1 1 d . . . N2 N 0.1846(5) 0.3631(4) 0.3997(3) 0.051(2) Uani 1 1 d . . . N3 N 0.5266(4) 0.4448(4) 0.2565(3) 0.0454(18) Uani 1 1 d . A . N4 N 0.4702(5) 0.6280(4) 0.3004(3) 0.053(2) Uani 1 1 d . A . C1 C 0.3162(6) 0.2421(5) 0.3170(3) 0.058(3) Uani 1 1 d . . . H1A H 0.3627 0.2527 0.2968 0.070 Uiso 1 1 calc R A . H1B H 0.2653 0.2343 0.2983 0.070 Uiso 1 1 calc R . . C2 C 0.3364(6) 0.1718(6) 0.3454(4) 0.065(3) Uani 1 1 d . A . C3 C 0.4280(6) 0.1660(6) 0.3592(4) 0.064(3) Uani 1 1 d . . . H3A H 0.4369 0.1207 0.3765 0.077 Uiso 1 1 calc R A . H3B H 0.4617 0.1629 0.3319 0.077 Uiso 1 1 calc R . . C4 C 0.3099(6) 0.1058(5) 0.3186(4) 0.068(3) Uani 1 1 d . . . H4A H 0.2501 0.1085 0.3116 0.102 Uiso 1 1 calc R A . H4B H 0.3217 0.0619 0.3361 0.102 Uiso 1 1 calc R . . H4C H 0.3405 0.1041 0.2906 0.102 Uiso 1 1 calc R . . C5 C 0.2880(6) 0.1308(5) 0.4163(4) 0.059(3) Uani 1 1 d . A . H5A H 0.3223 0.0900 0.4107 0.071 Uiso 1 1 calc R . . C6 C 0.2429(7) 0.1303(5) 0.4580(4) 0.064(3) Uani 1 1 d . . . C7 C 0.1816(7) 0.1810(6) 0.4657(4) 0.069(3) Uani 1 1 d . A . C8 C 0.1259(7) 0.1699(7) 0.5023(4) 0.081(3) Uani 1 1 d . . . H8A H 0.0822 0.2036 0.5067 0.097 Uiso 1 1 calc R A . C9 C 0.1341(9) 0.1146(7) 0.5293(4) 0.095(4) Uani 1 1 d . A . H9A H 0.0959 0.1089 0.5528 0.114 Uiso 1 1 calc R . . C10 C 0.1974(10) 0.0638(7) 0.5247(4) 0.094(4) Uani 1 1 d . . . C11 C 0.2082(12) 0.0029(9) 0.5535(5) 0.137(6) Uani 1 1 d . A . H11A H 0.1687 -0.0045 0.5762 0.164 Uiso 1 1 calc R . . C12 C 0.2706(15) -0.0446(9) 0.5506(6) 0.160(9) Uani 1 1 d . . . H12A H 0.2759 -0.0837 0.5712 0.192 Uiso 1 1 calc R A . C13 C 0.3284(12) -0.0358(8) 0.5164(6) 0.138(6) Uani 1 1 d . A . H13A H 0.3729 -0.0692 0.5139 0.166 Uiso 1 1 calc R . . C14 C 0.3206(10) 0.0222(7) 0.4861(4) 0.108(5) Uani 1 1 d . . . H14A H 0.3599 0.0276 0.4631 0.129 Uiso 1 1 calc R A . C15 C 0.2557(8) 0.0722(6) 0.4892(4) 0.079(3) Uani 1 1 d . A . C16 C 0.2846(6) 0.3566(6) 0.4614(3) 0.060(3) Uani 1 1 d . A . H16A H 0.3309 0.3825 0.4769 0.072 Uiso 1 1 calc R . . H16B H 0.2493 0.3348 0.4845 0.072 Uiso 1 1 calc R . . C17 C 0.2325(6) 0.4114(5) 0.4335(3) 0.052(2) Uani 1 1 d . A . C18 C 0.2846(6) 0.4653(5) 0.4089(3) 0.056(3) Uani 1 1 d . . . H18A H 0.2473 0.4956 0.3898 0.067 Uiso 1 1 calc R A . H18B H 0.3122 0.4977 0.4311 0.067 Uiso 1 1 calc R . . C19 C 0.1741(6) 0.4505(6) 0.4649(3) 0.065(3) Uani 1 1 d . . . H19A H 0.1407 0.4147 0.4807 0.098 Uiso 1 1 calc R A . H19B H 0.1374 0.4827 0.4474 0.098 Uiso 1 1 calc R . . H19C H 0.2067 0.4791 0.4867 0.098 Uiso 1 1 calc R . . C20 C 0.1206(5) 0.3895(5) 0.3798(3) 0.051(2) Uani 1 1 d . A . H20A H 0.1059 0.4379 0.3870 0.061 Uiso 1 1 calc R . . C21 C 0.0680(5) 0.3520(5) 0.3471(3) 0.049(2) Uani 1 1 d . . . C22 C 0.0861(5) 0.2799(5) 0.3355(3) 0.048(2) Uani 1 1 d . A . C23 C 0.0299(6) 0.2416(6) 0.3056(3) 0.060(3) Uani 1 1 d . . . H23A H 0.0397 0.1922 0.2984 0.072 Uiso 1 1 calc R A . C24 C -0.0377(6) 0.2768(6) 0.2877(4) 0.063(3) Uani 1 1 d . A . H24 H -0.0739 0.2507 0.2678 0.075 Uiso 1 1 calc R . . C25 C -0.0569(5) 0.3503(5) 0.2971(4) 0.059(3) Uani 1 1 d . . . C26 C -0.1246(6) 0.3840(7) 0.2776(4) 0.088(4) Uani 1 1 d . A . H26A H -0.1590 0.3568 0.2574 0.106 Uiso 1 1 calc R . . C27 C -0.1452(7) 0.4544(7) 0.2856(5) 0.100(5) Uani 1 1 d . . . H27A H -0.1918 0.4768 0.2712 0.120 Uiso 1 1 calc R A . C28 C -0.0942(7) 0.4916(7) 0.3160(5) 0.105(5) Uani 1 1 d . A . H28A H -0.1070 0.5405 0.3229 0.126 Uiso 1 1 calc R . . C29 C -0.0245(6) 0.4593(6) 0.3368(4) 0.079(3) Uani 1 1 d . . . H29A H 0.0094 0.4869 0.3570 0.094 Uiso 1 1 calc R A . C30 C -0.0041(6) 0.3872(5) 0.3283(4) 0.059(3) Uani 1 1 d . A . C31 C 0.5177(6) 0.3466(5) 0.3120(3) 0.060(3) Uani 1 1 d . . . H31A H 0.4919 0.3161 0.2881 0.072 Uiso 1 1 calc R A . H31B H 0.5517 0.3143 0.3316 0.072 Uiso 1 1 calc R . . C32 C 0.5756(6) 0.4021(5) 0.2900(3) 0.056(3) Uani 1 1 d . A . C33 C 0.6100(5) 0.4571(6) 0.3230(3) 0.062(3) Uani 1 1 d . . . H33A H 0.6244 0.4327 0.3518 0.074 Uiso 1 1 calc R A . H33B H 0.6615 0.4786 0.3113 0.074 Uiso 1 1 calc R . . C34 C 0.6474(5) 0.3591(6) 0.2693(4) 0.066(3) Uani 1 1 d . . . H34A H 0.6297 0.3089 0.2639 0.100 Uiso 1 1 calc R A . H34B H 0.6957 0.3596 0.2899 0.100 Uiso 1 1 calc R . . H34C H 0.6624 0.3816 0.2408 0.100 Uiso 1 1 calc R . . C35 C 0.5087(5) 0.4173(5) 0.2170(3) 0.053(2) Uani 1 1 d . . . H35A H 0.5252 0.3684 0.2124 0.063 Uiso 1 1 calc R A . C36 C 0.4673(5) 0.4521(5) 0.1804(3) 0.045(2) Uani 1 1 d . A . C37 C 0.4391(5) 0.5254(5) 0.1844(3) 0.050(2) Uani 1 1 d . . . C38 C 0.4057(6) 0.5593(6) 0.1454(3) 0.060(3) Uani 1 1 d . A . H38A H 0.3891 0.6086 0.1476 0.072 Uiso 1 1 calc R . . C39 C 0.3962(6) 0.5263(5) 0.1055(3) 0.058(3) Uani 1 1 d . . . H39A H 0.3735 0.5525 0.0806 0.070 Uiso 1 1 calc R A . C40 C 0.4197(6) 0.4521(6) 0.1001(3) 0.057(3) Uani 1 1 d . A . C41 C 0.4054(6) 0.4164(6) 0.0587(4) 0.065(3) Uani 1 1 d . . . H41A H 0.3838 0.4422 0.0334 0.078 Uiso 1 1 calc R A . C42 C 0.4231(6) 0.3446(7) 0.0556(4) 0.081(4) Uani 1 1 d . A . H42A H 0.4114 0.3196 0.0283 0.097 Uiso 1 1 calc R . . C43 C 0.4584(6) 0.3071(6) 0.0923(4) 0.082(4) Uani 1 1 d . . . H43A H 0.4720 0.2572 0.0894 0.098 Uiso 1 1 calc R A . C44 C 0.4732(6) 0.3415(6) 0.1317(4) 0.070(3) Uani 1 1 d . A . H44A H 0.4964 0.3151 0.1564 0.084 Uiso 1 1 calc R . . C45 C 0.4550(5) 0.4152(5) 0.1370(3) 0.050(2) Uani 1 1 d . . . C46 C 0.3374(6) 0.5671(5) 0.2973(3) 0.057(3) Uani 1 1 d . . . H46A H 0.2878 0.5582 0.3156 0.068 Uiso 1 1 calc R A . H46B H 0.3188 0.5725 0.2656 0.068 Uiso 1 1 calc R . . C47 C 0.3811(6) 0.6362(5) 0.3132(3) 0.055(3) Uani 1 1 d . A . C48 C 0.3771(5) 0.6445(5) 0.3646(3) 0.057(3) Uani 1 1 d . . . H48A H 0.3992 0.6928 0.3732 0.068 Uiso 1 1 calc R A . H48B H 0.3182 0.6425 0.3734 0.068 Uiso 1 1 calc R . . C49 C 0.3379(5) 0.7015(5) 0.2913(4) 0.061(3) Uani 1 1 d . . . H49A H 0.3670 0.7461 0.3002 0.091 Uiso 1 1 calc R A . H49B H 0.2802 0.7038 0.3009 0.091 Uiso 1 1 calc R . . H49C H 0.3387 0.6964 0.2586 0.091 Uiso 1 1 calc R . . C50 C 0.5229(6) 0.6790(5) 0.3113(3) 0.055(3) Uani 1 1 d . . . H50A H 0.5018 0.7215 0.3250 0.066 Uiso 1 1 calc R A . C51 C 0.6094(6) 0.6754(6) 0.3042(3) 0.057(3) Uani 1 1 d . A . C52 C 0.6431(6) 0.6229(6) 0.2749(3) 0.059(3) Uani 1 1 d . . . C53 C 0.7293(6) 0.6238(6) 0.2665(4) 0.065(3) Uani 1 1 d . A . H53A H 0.7513 0.5892 0.2464 0.078 Uiso 1 1 calc R . . C54 C 0.7812(7) 0.6725(7) 0.2864(4) 0.075(3) Uani 1 1 d . . . H54A H 0.8390 0.6700 0.2811 0.090 Uiso 1 1 calc R A . C55 C 0.7504(7) 0.7274(7) 0.3150(4) 0.070(3) Uani 1 1 d . A . C56 C 0.8040(8) 0.7784(9) 0.3372(5) 0.107(5) Uani 1 1 d . . . H56A H 0.8618 0.7762 0.3315 0.129 Uiso 1 1 calc R A . C57 C 0.7781(11) 0.8282(10) 0.3649(6) 0.146(7) Uani 1 1 d . A . H57A H 0.8164 0.8611 0.3786 0.176 Uiso 1 1 calc R . . C58 C 0.6914(8) 0.8327(8) 0.3743(5) 0.107(5) Uani 1 1 d . . . H58A H 0.6714 0.8679 0.3947 0.129 Uiso 1 1 calc R A . C59 C 0.6366(7) 0.7839(7) 0.3528(4) 0.083(4) Uani 1 1 d . A . H59A H 0.5787 0.7877 0.3580 0.099 Uiso 1 1 calc R . . C60 C 0.6643(7) 0.7300(6) 0.3240(4) 0.063(3) Uani 1 1 d . . . C64 C 0.5285(6) 0.4145(8) 0.4475(3) 0.067(3) Uani 1 1 d . A . C65 C 0.5830(6) 0.4203(6) 0.4901(3) 0.072(3) Uani 1 1 d . . . H65A H 0.6182 0.3771 0.4930 0.108 Uiso 1 1 calc R A . H65B H 0.5476 0.4240 0.5163 0.108 Uiso 1 1 calc R . . H65C H 0.6181 0.4636 0.4884 0.108 Uiso 1 1 calc R . . O1A O 0.3216(8) 0.3686(8) 0.2525(6) 0.040(4) Uiso 0.50 1 d P A 1 O2A O 0.208(2) 0.443(3) 0.3042(13) 0.055(8) Uani 0.50 1 d P A 1 C11A C 0.1723(14) 0.4441(12) 0.2682(8) 0.048(6) Uiso 0.50 1 d P A 1 H11B H 0.1254 0.4754 0.2675 0.058 Uiso 0.50 1 calc PR A 1 C1A C 0.1858(14) 0.4091(12) 0.2269(9) 0.051(5) Uiso 0.50 1 d P A 1 C2A C 0.2677(15) 0.3775(11) 0.2205(6) 0.036(5) Uiso 0.50 1 d P A 1 C3A C 0.2827(12) 0.3530(11) 0.1770(7) 0.066(6) Uiso 0.50 1 d P A 1 H3A1 H 0.3342 0.3289 0.1730 0.079 Uiso 0.50 1 calc PR A 1 C4A C 0.2316(14) 0.3596(13) 0.1392(9) 0.054(7) Uiso 0.50 1 d P A 1 H4A1 H 0.2491 0.3460 0.1102 0.065 Uiso 0.50 1 calc PR A 1 C5A C 0.1426(16) 0.3914(12) 0.1477(9) 0.066(6) Uiso 0.50 1 d P A 1 C6A C 0.1278(16) 0.4165(13) 0.1909(9) 0.064(7) Uiso 0.50 1 d P A 1 C7A C 0.051(2) 0.442(2) 0.1940(14) 0.084(11) Uiso 0.50 1 d P A 1 H7A H 0.0333 0.4564 0.2230 0.100 Uiso 0.50 1 calc PR A 1 C8A C -0.0099(15) 0.4514(14) 0.1570(9) 0.088(7) Uiso 0.50 1 d P A 1 H8A1 H -0.0647 0.4686 0.1615 0.105 Uiso 0.50 1 calc PR A 1 C9A C 0.016(2) 0.4346(19) 0.1180(14) 0.119(12) Uiso 0.50 1 d P A 1 H9A1 H -0.0187 0.4483 0.0932 0.143 Uiso 0.50 1 calc PR A 1 C10A C 0.082(3) 0.402(3) 0.109(2) 0.110(16) Uiso 0.50 1 d P A 1 H10A H 0.0924 0.3849 0.0798 0.133 Uiso 0.50 1 calc PR A 1 O1B O 0.2299(18) 0.436(2) 0.2928(11) 0.047(7) Uani 0.50 1 d P A 2 O2B O 0.3593(9) 0.3564(8) 0.2511(4) 0.051(4) Uani 0.50 1 d P A 2 C11B C 0.3118(16) 0.3605(13) 0.2199(9) 0.068(7) Uiso 0.50 1 d P A 2 H11C H 0.3299 0.3385 0.1930 0.082 Uiso 0.50 1 calc PR A 2 C1B C 0.059(3) 0.450(2) 0.2100(14) 0.110(15) Uiso 0.50 1 d P A 2 H1B1 H 0.0034 0.4682 0.2076 0.132 Uiso 0.50 1 calc PR A 2 C2B C 0.1072(13) 0.4538(12) 0.2505(8) 0.072(6) Uiso 0.50 1 d P A 2 H2B H 0.0842 0.4745 0.2766 0.086 Uiso 0.50 1 calc PR A 2 C3B C 0.1920(15) 0.4261(14) 0.2521(11) 0.057(7) Uiso 0.50 1 d P A 2 C4B C 0.2278(16) 0.3955(11) 0.2169(6) 0.039(5) Uiso 0.50 1 d P A 2 C5B C 0.1814(13) 0.3945(12) 0.1731(8) 0.065(6) Uiso 0.50 1 d P A 2 C6B C 0.100(2) 0.4163(16) 0.1728(12) 0.086(9) Uiso 0.50 1 d P A 2 C7B C 0.055(3) 0.416(3) 0.1286(17) 0.131(17) Uiso 0.50 1 d P A 2 H7B H -0.0002 0.4326 0.1247 0.157 Uiso 0.50 1 calc PR A 2 C8B C 0.098(3) 0.392(3) 0.0962(16) 0.117(18) Uiso 0.50 1 d P A 2 H8B H 0.0666 0.3885 0.0689 0.141 Uiso 0.50 1 calc PR A 2 C9B C 0.166(2) 0.3721(18) 0.0923(12) 0.129(11) Uiso 0.50 1 d P A 2 H9B H 0.1917 0.3570 0.0654 0.154 Uiso 0.50 1 calc PR A 2 C10B C 0.205(2) 0.3755(15) 0.1358(11) 0.073(9) Uiso 0.50 1 d P A 2 H10B H 0.2609 0.3595 0.1362 0.087 Uiso 0.50 1 calc PR A 2 O1M O 0.4790(5) 0.2600(5) 0.5126(3) 0.109(3) Uani 1 1 d . . . H1M H 0.4914 0.2781 0.4878 0.163 Uiso 1 1 calc R . . C1M C 0.4311(9) 0.1976(8) 0.5053(5) 0.117(5) Uani 1 1 d . . . H1M1 H 0.3842 0.1977 0.5256 0.175 Uiso 1 1 calc R . . H1M2 H 0.4655 0.1545 0.5111 0.175 Uiso 1 1 calc R . . H1M3 H 0.4102 0.1968 0.4742 0.175 Uiso 1 1 calc R . . O2M O 0.5548(5) 0.6576(5) 0.4175(3) 0.093(3) Uani 1 1 d . . . H2M H 0.5478 0.6784 0.4422 0.140 Uiso 1 1 calc R . . C2M C 0.6379(8) 0.6205(8) 0.4183(4) 0.109(5) Uani 1 1 d . . . H2M1 H 0.6810 0.6550 0.4280 0.163 Uiso 1 1 calc R . . H2M2 H 0.6498 0.6028 0.3882 0.163 Uiso 1 1 calc R . . H2M3 H 0.6370 0.5795 0.4392 0.163 Uiso 1 1 calc R . . O3M O 0.6613(5) 0.5603(5) 0.1681(3) 0.092(3) Uani 1 1 d . . . H3M H 0.6246 0.5644 0.1875 0.138 Uiso 1 1 d R B . C3M1 C 0.6949(14) 0.4943(14) 0.1705(9) 0.088(7) Uiso 0.50 1 d P B 1 H3M1 H 0.6555 0.4587 0.1578 0.133 Uiso 0.50 1 calc PR B 1 H3M2 H 0.7077 0.4821 0.2019 0.133 Uiso 0.50 1 calc PR B 1 H3M3 H 0.7461 0.4934 0.1534 0.133 Uiso 0.50 1 calc PR B 1 C3M2 C 0.6195(18) 0.5963(19) 0.1397(12) 0.134(11) Uiso 0.50 1 d P B 2 H3M4 H 0.6008 0.6416 0.1534 0.202 Uiso 0.50 1 calc PR B 2 H3M5 H 0.5710 0.5678 0.1297 0.202 Uiso 0.50 1 calc PR B 2 H3M6 H 0.6539 0.6074 0.1140 0.202 Uiso 0.50 1 calc PR B 2 C4M C -0.1436(17) 0.3961(19) 0.4331(11) 0.130(11) Uiso 0.50 1 d P C 2 H4M1 H -0.1974 0.4163 0.4415 0.194 Uiso 0.25 1 calc PR C 2 H4M2 H -0.1496 0.3719 0.4039 0.194 Uiso 0.25 1 calc PR C 2 H4M3 H -0.1028 0.4353 0.4311 0.194 Uiso 0.25 1 calc PR C 2 H4M4 H -0.1755 0.4405 0.4382 0.194 Uiso 0.25 1 d PR C 1 H4M5 H -0.1811 0.3542 0.4332 0.194 Uiso 0.25 1 d PR C 1 H4M6 H -0.1168 0.3992 0.4040 0.194 Uiso 0.25 1 d PR C 1 O4M1 O -0.072(2) 0.395(2) 0.4727(14) 0.127(13) Uiso 0.25 1 d P D 1 H4M7 H -0.0771 0.3542 0.4851 0.190 Uiso 0.25 1 d PR D 1 O4M2 O -0.122(2) 0.3552(19) 0.4595(12) 0.093(10) Uiso 0.25 1 d P C 2 H4M8 H -0.0711 0.3456 0.4567 0.139 Uiso 0.25 1 d PR C 2 O5M O -0.1131(15) 0.3626(14) 0.5477(9) 0.169(9) Uiso 0.50 1 d P E 2 H5M H -0.1125 0.4013 0.5328 0.253 Uiso 0.50 1 calc PR E 2 C5M C -0.1845(15) 0.3425(15) 0.5517(9) 0.102(8) Uiso 0.50 1 d P E 2 H5M1 H -0.1871 0.3072 0.5762 0.153 Uiso 0.50 1 calc PR E 2 H5M2 H -0.2043 0.3198 0.5237 0.153 Uiso 0.50 1 calc PR E 2 H5M3 H -0.2197 0.3843 0.5584 0.153 Uiso 0.50 1 calc PR E 2 O6M O 0.0276(14) 0.3764(13) 0.6053(8) 0.145(8) Uiso 0.50 1 d P F 2 H6M H -0.0047 0.3951 0.5859 0.218 Uiso 0.50 1 calc PR F 2 C6M C 0.1107(14) 0.3675(15) 0.5862(9) 0.098(8) Uiso 0.50 1 d P F 2 H6M1 H 0.1145 0.3969 0.5589 0.148 Uiso 0.50 1 calc PR F 2 H6M2 H 0.1197 0.3163 0.5788 0.148 Uiso 0.50 1 calc PR F 2 H6M3 H 0.1532 0.3834 0.6082 0.148 Uiso 0.50 1 calc PR F 2 O6M1 O -0.0477(19) 0.3997(19) 0.5893(11) 0.096(10) Uiso 0.25 1 d P G 3 H6M4 H -0.0647 0.3568 0.5866 0.143 Uiso 0.25 1 calc PR G 3 C6M1 C 0.029(3) 0.407(3) 0.568(2) 0.099(16) Uiso 0.25 1 d P G 3 H6M5 H 0.0522 0.4553 0.5738 0.149 Uiso 0.25 1 calc PR G 3 H6M6 H 0.0212 0.4000 0.5356 0.149 Uiso 0.25 1 calc PR G 3 H6M7 H 0.0682 0.3701 0.5797 0.149 Uiso 0.25 1 calc PR G 3 O7M O 0.0020(7) 0.3168(7) 0.6864(5) 0.174(5) Uani 1 1 d . . . H7M H 0.0145 0.3494 0.6681 0.261 Uiso 1 1 calc R . . C7M C -0.0706(11) 0.3333(11) 0.7050(7) 0.210(11) Uani 1 1 d . . . H7M1 H -0.0611 0.3686 0.7292 0.315 Uiso 1 1 calc R . . H7M2 H -0.0955 0.2893 0.7173 0.315 Uiso 1 1 calc R . . H7M3 H -0.1084 0.3542 0.6822 0.315 Uiso 1 1 calc R . . O8M O -0.0059(11) 0.2666(11) 0.4415(6) 0.235(12) Uani 1 1 d . . . H8M H 0.0462 0.2632 0.4429 0.352 Uiso 1 1 calc R . . C8M C -0.0417(14) 0.199(2) 0.4224(9) 0.27(2) Uani 1 1 d . . . H8M1 H -0.0393 0.1604 0.4451 0.405 Uiso 1 1 calc R . . H8M2 H -0.0099 0.1840 0.3963 0.405 Uiso 1 1 calc R . . H8M3 H -0.0998 0.2073 0.4130 0.405 Uiso 1 1 calc R . . O9M O -0.3844(5) 0.1985(6) 0.4019(4) 0.140(4) Uani 1 1 d . . . H9M H -0.3546 0.1881 0.3801 0.209 Uiso 1 1 calc R . . C9M C -0.3286(15) 0.2400(12) 0.4401(12) 0.294(18) Uani 1 1 d . . . H9M1 H -0.2964 0.2787 0.4261 0.441 Uiso 1 1 calc R . . H9M2 H -0.2906 0.2053 0.4548 0.441 Uiso 1 1 calc R . . H9M3 H -0.3651 0.2611 0.4624 0.441 Uiso 1 1 calc R . . O10M O -0.2637(11) 0.1686(9) 0.3573(5) 0.106(6) Uani 0.50 1 d P H 1 H10M H -0.2334 0.1340 0.3494 0.159 Uiso 0.50 1 calc PR H 1 C10M C -0.2304(18) 0.2358(14) 0.3408(11) 0.130(11) Uani 0.50 1 d P H 1 H10C H -0.1718 0.2289 0.3335 0.195 Uiso 0.50 1 calc PR H 1 H10D H -0.2348 0.2734 0.3638 0.195 Uiso 0.50 1 calc PR H 1 H10E H -0.2618 0.2507 0.3137 0.195 Uiso 0.50 1 calc PR H 1 O11M O -0.3240(13) 0.1081(13) 0.3394(8) 0.047(6) Uiso 0.25 1 d P I 2 H11M H -0.2740 0.1014 0.3333 0.071 Uiso 0.25 1 calc PR I 2 C11M C -0.366(3) 0.058(3) 0.3253(17) 0.094(15) Uiso 0.25 1 d P I 2 H11D H -0.3990 0.0381 0.3495 0.141 Uiso 0.25 1 calc PR I 2 H11E H -0.3287 0.0195 0.3142 0.141 Uiso 0.25 1 calc PR I 2 H11F H -0.4023 0.0743 0.3007 0.141 Uiso 0.25 1 calc PR I 2 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 0.0740(8) 0.0404(8) 0.0435(8) 0.0008(7) 0.0024(6) 0.0006(6) Co3 0.0722(8) 0.0445(8) 0.0411(8) -0.0001(7) -0.0028(6) -0.0033(6) Co5 0.0640(8) 0.0436(8) 0.0435(8) -0.0025(7) 0.0013(6) -0.0039(6) Co2 0.0730(8) 0.0471(8) 0.0425(8) 0.0004(7) 0.0011(6) 0.0033(6) Co4 0.0686(8) 0.0471(8) 0.0435(8) -0.0019(7) -0.0007(6) -0.0020(6) O1 0.075(4) 0.041(4) 0.040(4) 0.002(3) 0.008(3) 0.001(3) O2 0.074(4) 0.052(4) 0.073(5) 0.007(4) 0.002(4) 0.012(4) O3 0.081(4) 0.052(4) 0.051(4) 0.013(4) 0.009(3) 0.000(3) O4 0.070(4) 0.042(4) 0.039(4) 0.002(3) 0.011(3) -0.002(3) O5 0.081(4) 0.056(4) 0.030(4) -0.004(3) 0.004(3) 0.005(3) O6 0.067(4) 0.045(4) 0.051(4) -0.013(3) -0.006(3) 0.000(3) O7 0.059(4) 0.049(4) 0.051(4) 0.000(3) 0.005(3) 0.002(3) O8 0.065(4) 0.059(4) 0.040(4) -0.007(3) 0.000(3) -0.005(3) O9 0.083(4) 0.044(4) 0.037(4) -0.005(3) -0.004(3) 0.004(3) O10 0.059(4) 0.050(4) 0.047(4) -0.007(3) 0.001(3) -0.003(3) O11 0.075(4) 0.060(4) 0.046(4) -0.006(4) 0.008(3) 0.000(3) O12 0.067(4) 0.045(4) 0.055(4) -0.008(3) 0.013(3) -0.010(3) O14 0.103(5) 0.055(5) 0.046(4) 0.002(4) -0.019(4) 0.001(4) O15 0.075(4) 0.062(5) 0.051(5) 0.000(4) -0.004(3) -0.006(4) N1 0.073(5) 0.036(5) 0.038(5) 0.009(4) 0.003(4) 0.017(4) N2 0.081(5) 0.030(4) 0.044(5) 0.001(4) 0.011(4) -0.001(4) N3 0.058(4) 0.033(4) 0.045(5) 0.000(4) 0.000(4) -0.001(3) N4 0.084(6) 0.032(4) 0.043(5) -0.001(4) 0.007(4) 0.007(4) C1 0.073(6) 0.042(6) 0.060(7) -0.019(6) 0.017(5) -0.016(5) C2 0.089(7) 0.050(7) 0.055(7) 0.003(6) -0.004(6) 0.006(5) C3 0.073(7) 0.051(7) 0.070(8) 0.000(6) 0.008(5) 0.000(5) C4 0.109(8) 0.037(6) 0.058(7) -0.012(6) 0.012(6) -0.003(5) C5 0.078(7) 0.040(6) 0.059(7) -0.008(6) -0.006(5) 0.008(5) C6 0.104(8) 0.034(6) 0.052(7) -0.001(6) -0.005(6) 0.001(6) C7 0.109(9) 0.053(7) 0.044(7) -0.001(6) 0.009(6) -0.024(6) C8 0.121(9) 0.075(9) 0.046(7) -0.011(7) 0.014(7) -0.015(7) C9 0.165(13) 0.056(9) 0.065(9) 0.006(8) 0.005(8) -0.008(8) C10 0.178(13) 0.062(9) 0.042(7) 0.020(7) 0.004(8) -0.011(9) C11 0.26(2) 0.092(12) 0.066(10) 0.041(9) 0.048(11) 0.007(12) C12 0.33(3) 0.079(12) 0.072(12) 0.022(10) -0.007(15) 0.067(15) C13 0.248(19) 0.078(11) 0.090(12) 0.031(10) 0.028(13) 0.040(11) C14 0.203(14) 0.054(8) 0.066(9) 0.012(7) -0.009(9) 0.019(9) C15 0.139(10) 0.043(7) 0.056(8) -0.005(6) -0.003(7) -0.003(7) C16 0.079(7) 0.064(7) 0.038(6) -0.005(6) 0.006(5) -0.005(5) C17 0.074(6) 0.036(5) 0.047(6) -0.005(5) -0.006(5) -0.006(5) C18 0.075(6) 0.042(6) 0.052(6) 0.001(5) 0.007(5) -0.008(5) C19 0.080(7) 0.059(7) 0.058(7) -0.007(6) 0.017(5) 0.000(5) C20 0.062(6) 0.036(6) 0.055(6) 0.003(5) 0.006(5) 0.013(5) C21 0.049(5) 0.040(6) 0.060(7) -0.011(5) 0.019(5) -0.002(4) C22 0.054(5) 0.054(6) 0.034(5) -0.007(5) 0.007(4) -0.005(5) C23 0.074(7) 0.046(6) 0.061(7) -0.005(6) 0.011(5) -0.013(5) C24 0.060(6) 0.059(7) 0.070(8) -0.019(6) 0.008(5) -0.006(5) C25 0.045(5) 0.052(6) 0.080(8) -0.009(6) 0.001(5) 0.006(5) C26 0.062(7) 0.084(10) 0.118(11) -0.030(8) -0.010(7) -0.001(6) C27 0.073(7) 0.068(9) 0.157(14) -0.035(9) -0.035(8) 0.017(6) C28 0.071(8) 0.081(9) 0.163(14) -0.037(10) -0.016(8) 0.029(7) C29 0.072(7) 0.050(7) 0.113(10) -0.028(7) -0.006(6) 0.002(6) C30 0.057(6) 0.042(6) 0.078(8) -0.012(6) 0.007(5) 0.001(5) C31 0.074(7) 0.057(7) 0.048(6) 0.010(5) 0.012(5) 0.006(5) C32 0.070(6) 0.047(6) 0.051(6) -0.013(5) -0.003(5) 0.012(5) C33 0.056(6) 0.071(7) 0.059(7) 0.006(6) 0.004(5) 0.013(5) C34 0.056(6) 0.079(8) 0.064(7) -0.006(6) -0.001(5) 0.013(5) C35 0.056(6) 0.042(6) 0.060(7) -0.011(5) 0.007(5) -0.005(4) C36 0.044(5) 0.049(6) 0.043(6) 0.008(5) 0.007(4) -0.005(4) C37 0.053(5) 0.053(7) 0.042(6) 0.002(5) 0.006(4) -0.006(5) C38 0.073(6) 0.052(7) 0.054(7) -0.003(6) 0.000(5) -0.001(5) C39 0.081(7) 0.048(7) 0.046(7) 0.005(6) -0.003(5) 0.007(5) C40 0.066(6) 0.061(7) 0.043(6) -0.001(6) 0.006(5) 0.005(5) C41 0.067(6) 0.074(8) 0.056(7) -0.004(6) 0.000(5) 0.005(6) C42 0.090(8) 0.075(9) 0.076(9) -0.035(7) -0.016(6) 0.021(7) C43 0.093(8) 0.069(8) 0.083(9) -0.032(7) -0.026(7) 0.030(6) C44 0.090(7) 0.066(8) 0.054(7) -0.015(6) -0.011(6) 0.026(6) C45 0.062(6) 0.042(6) 0.046(6) -0.011(5) -0.005(5) 0.003(4) C46 0.067(6) 0.056(7) 0.049(6) 0.002(5) 0.002(5) -0.003(5) C47 0.065(6) 0.048(6) 0.053(7) -0.015(5) 0.003(5) -0.003(5) C48 0.056(6) 0.052(6) 0.063(7) -0.006(6) 0.012(5) 0.002(5) C49 0.067(6) 0.042(6) 0.073(8) -0.006(6) 0.008(5) 0.002(5) C50 0.084(7) 0.040(6) 0.040(6) -0.001(5) 0.001(5) 0.005(5) C51 0.059(6) 0.055(7) 0.058(7) 0.006(6) -0.001(5) -0.002(5) C52 0.059(6) 0.064(7) 0.054(7) 0.020(6) -0.005(5) -0.006(5) C53 0.079(7) 0.059(7) 0.057(7) 0.012(6) 0.009(6) -0.003(6) C54 0.082(8) 0.082(9) 0.062(8) 0.003(7) 0.006(6) -0.013(7) C55 0.073(7) 0.087(9) 0.051(7) 0.014(7) 0.007(6) -0.028(6) C56 0.107(10) 0.130(13) 0.086(10) -0.031(10) 0.032(8) -0.060(9) C57 0.152(14) 0.176(18) 0.113(14) -0.071(13) 0.038(11) -0.100(13) C58 0.110(10) 0.123(12) 0.090(10) -0.037(10) 0.020(8) -0.039(9) C59 0.095(8) 0.067(8) 0.086(9) -0.014(7) -0.003(7) -0.034(7) C60 0.090(8) 0.049(7) 0.051(7) 0.013(6) 0.005(6) -0.017(6) C64 0.057(6) 0.106(11) 0.038(7) -0.010(7) 0.001(5) 0.016(7) C65 0.088(7) 0.069(8) 0.058(7) 0.000(6) -0.015(6) 0.006(6) O2A 0.06(2) 0.066(13) 0.041(13) 0.002(10) 0.024(11) 0.004(14) O1B 0.025(12) 0.052(13) 0.06(2) 0.019(15) 0.000(11) -0.002(9) O2B 0.049(9) 0.066(10) 0.039(8) -0.015(7) -0.007(7) 0.005(8) O1M 0.153(8) 0.111(8) 0.061(6) 0.013(6) -0.016(5) -0.019(6) C1M 0.171(13) 0.101(12) 0.077(10) 0.018(9) -0.011(9) -0.064(10) O2M 0.118(6) 0.089(6) 0.073(6) -0.010(5) 0.001(5) -0.036(5) C2M 0.127(11) 0.133(14) 0.066(9) -0.015(9) -0.008(8) -0.041(10) O3M 0.111(6) 0.103(7) 0.064(6) -0.002(5) 0.020(5) -0.007(5) O7M 0.157(9) 0.166(12) 0.202(13) -0.082(10) 0.064(9) -0.066(8) C7M 0.177(16) 0.22(2) 0.24(2) 0.022(19) 0.172(18) 0.030(16) O8M 0.223(19) 0.31(2) 0.174(18) 0.161(18) 0.122(14) 0.163(17) C8M 0.093(14) 0.59(8) 0.12(2) 0.04(3) 0.009(12) 0.07(3) O9M 0.093(6) 0.102(8) 0.223(13) -0.028(8) -0.011(7) 0.023(5) C9M 0.25(3) 0.13(2) 0.50(6) -0.10(3) 0.00(3) 0.064(18) O10M 0.178(16) 0.061(11) 0.080(12) 0.024(10) 0.054(11) 0.028(11) C10M 0.18(3) 0.067(19) 0.14(3) 0.06(2) 0.01(2) 0.002(18) _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 N2 1.865(7) . ? Co1 O3 1.893(6) . ? Co1 O6 1.898(6) . ? Co1 N1 1.907(7) . ? Co1 O5 1.921(6) . ? Co1 O1 1.925(6) . ? Co1 Co2 2.9832(18) . ? Co3 O1B 1.86(3) . ? Co3 O1A 1.937(17) . ? Co3 O2B 2.105(14) . ? Co3 O7 2.115(6) . ? Co3 O4 2.128(6) . ? Co3 O2A 2.16(4) . ? Co3 O10 2.175(6) . ? Co3 O1 2.183(6) . ? Co3 Co4 2.8731(18) . ? Co3 Co2 2.8880(18) . ? Co5 N3 1.867(7) . ? Co5 N4 1.878(7) . ? Co5 O9 1.887(6) . ? Co5 O8 1.891(6) . ? Co5 O12 1.893(6) . ? Co5 O10 1.948(6) . ? Co5 Co4 2.9809(19) . ? Co2 O5 1.996(6) . ? Co2 O7 2.021(6) . ? Co2 O15 2.042(7) . ? Co2 O1 2.137(6) . ? Co2 O4 2.152(6) . ? Co4 O8 1.997(6) . ? Co4 O4 2.027(6) . ? Co4 O14 2.038(7) . ? Co4 O10 2.162(6) . ? Co4 O7 2.174(6) . ? O1 C1 1.408(10) . ? O2 C3 1.421(11) . ? O2 H2 0.8400 . ? O3 C7 1.336(12) . ? O4 C18 1.393(10) . ? O5 C16 1.398(11) . ? O6 C22 1.303(10) . ? O7 C31 1.394(10) . ? O8 C33 1.419(10) . ? O9 C37 1.289(10) . ? O10 C46 1.433(10) . ? O11 C48 1.433(11) . ? O11 H11 0.8400 . ? O12 C52 1.317(11) . ? O14 C64 1.242(13) . ? O15 C64 1.296(13) . ? N1 C5 1.265(11) . ? N1 C2 1.503(12) . ? N2 C20 1.273(10) . ? N2 C17 1.539(11) . ? N3 C35 1.307(11) . ? N3 C32 1.483(11) . ? N4 C50 1.301(11) . ? N4 C47 1.503(11) . ? C1 C2 1.577(13) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C4 1.512(13) . ? C2 C3 1.524(12) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.455(14) . ? C5 H5A 0.9500 . ? C6 C7 1.382(14) . ? C6 C15 1.432(15) . ? C7 C8 1.445(14) . ? C8 C9 1.303(15) . ? C8 H8A 0.9500 . ? C9 C10 1.393(17) . ? C9 H9A 0.9500 . ? C10 C11 1.422(18) . ? C10 C15 1.439(17) . ? C11 C12 1.34(2) . ? C11 H11A 0.9500 . ? C12 C13 1.40(2) . ? C12 H12A 0.9500 . ? C13 C14 1.405(18) . ? C13 H13A 0.9500 . ? C14 C15 1.397(16) . ? C14 H14A 0.9500 . ? C16 C17 1.542(13) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.502(12) . ? C17 C19 1.523(13) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.450(12) . ? C20 H20A 0.9500 . ? C21 C22 1.406(12) . ? C21 C30 1.430(12) . ? C22 C23 1.439(12) . ? C23 C24 1.364(13) . ? C23 H23A 0.9500 . ? C24 C25 1.418(13) . ? C24 H24 0.9500 . ? C25 C26 1.371(13) . ? C25 C30 1.419(13) . ? C26 C27 1.361(15) . ? C26 H26A 0.9500 . ? C27 C28 1.388(15) . ? C27 H27A 0.9500 . ? C28 C29 1.402(14) . ? C28 H28A 0.9500 . ? C29 C30 1.392(13) . ? C29 H29A 0.9500 . ? C31 C32 1.541(13) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.508(13) . ? C32 C34 1.544(12) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.418(12) . ? C35 H35A 0.9500 . ? C36 C37 1.432(12) . ? C36 C45 1.471(12) . ? C37 C38 1.415(13) . ? C38 C39 1.343(13) . ? C38 H38A 0.9500 . ? C39 C40 1.429(13) . ? C39 H39A 0.9500 . ? C40 C45 1.401(13) . ? C40 C41 1.412(13) . ? C41 C42 1.357(14) . ? C41 H41A 0.9500 . ? C42 C43 1.403(15) . ? C42 H42A 0.9500 . ? C43 C44 1.351(14) . ? C43 H43A 0.9500 . ? C44 C45 1.400(13) . ? C44 H44A 0.9500 . ? C46 C47 1.525(12) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C49 1.528(13) . ? C47 C48 1.542(13) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C51 1.416(12) . ? C50 H50A 0.9500 . ? C51 C52 1.419(14) . ? C51 C60 1.456(14) . ? C52 C53 1.416(12) . ? C53 C54 1.351(14) . ? C53 H53A 0.9500 . ? C54 C55 1.422(15) . ? C54 H54A 0.9500 . ? C55 C60 1.418(13) . ? C55 C56 1.428(16) . ? C56 C57 1.310(19) . ? C56 H56A 0.9500 . ? C57 C58 1.432(18) . ? C57 H57A 0.9500 . ? C58 C59 1.404(15) . ? C58 H58A 0.9500 . ? C59 C60 1.392(15) . ? C59 H59A 0.9500 . ? C64 C65 1.529(13) . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? O1A C2A 1.28(3) . ? O2A C11A 1.20(5) . ? C11A C1A 1.41(4) . ? C11A H11B 0.9500 . ? C1A C6A 1.41(3) . ? C1A C2A 1.46(3) . ? C2A C3A 1.40(3) . ? C3A C4A 1.38(3) . ? C3A H3A1 0.9500 . ? C4A C5A 1.57(3) . ? C4A H4A1 0.9500 . ? C5A C6A 1.39(4) . ? C5A C10A 1.51(6) . ? C6A C7A 1.34(5) . ? C7A C8A 1.46(4) . ? C7A H7A 0.9500 . ? C8A C9A 1.28(4) . ? C8A H8A1 0.9500 . ? C9A C10A 1.25(6) . ? C9A H9A1 0.9500 . ? C10A H10A 0.9500 . ? O1B C3B 1.36(5) . ? O2B C11B 1.19(3) . ? C11B C4B 1.50(3) . ? C11B H11C 0.9500 . ? C1B C2B 1.42(4) . ? C1B C6B 1.45(6) . ? C1B H1B1 0.9500 . ? C2B C3B 1.46(3) . ? C2B H2B 0.9500 . ? C3B C4B 1.34(4) . ? C4B C5B 1.49(3) . ? C5B C10B 1.24(4) . ? C5B C6B 1.37(4) . ? C6B C7B 1.48(5) . ? C7B C8B 1.28(7) . ? C7B H7B 0.9500 . ? C8B C9B 1.17(5) . ? C8B H8B 0.9500 . ? C9B C10B 1.42(4) . ? C9B H9B 0.9500 . ? C10B H10B 0.9500 . ? O1M C1M 1.399(13) . ? O1M H1M 0.8400 . ? C1M H1M1 0.9800 . ? C1M H1M2 0.9800 . ? C1M H1M3 0.9800 . ? O2M C2M 1.501(14) . ? O2M H2M 0.8400 . ? C2M H2M1 0.9800 . ? C2M H2M2 0.9800 . ? C2M H2M3 0.9800 . ? O3M C3M2 1.26(3) . ? O3M C3M1 1.33(2) . ? O3M H3M 0.8400 . ? C3M1 H3M1 0.9800 . ? C3M1 H3M2 0.9800 . ? C3M1 H3M3 0.9800 . ? C3M2 H3M4 0.9800 . ? C3M2 H3M5 0.9800 . ? C3M2 H3M6 0.9800 . ? C4M O4M2 1.14(4) . ? C4M H4M1 0.9800 . ? C4M H4M2 0.9800 . ? C4M H4M3 0.9800 . ? C4M H4M4 0.9800 . ? C4M H4M5 0.9800 . ? C4M H4M6 0.9800 . ? O4M1 H4M7 0.8400 . ? O4M1 H4M8 1.0242 . ? O4M2 H4M5 1.2198 . ? O4M2 H4M7 1.0372 . ? O4M2 H4M8 0.8400 . ? O5M C5M 1.22(3) . ? O5M H5M 0.8400 . ? C5M H5M1 0.9800 . ? C5M H5M2 0.9800 . ? C5M H5M3 0.9800 . ? O6M C6M 1.48(3) . ? O6M H6M 0.8400 . ? C6M H6M1 0.9800 . ? C6M H6M2 0.9800 . ? C6M H6M3 0.9800 . ? O6M1 C6M1 1.41(5) . ? O6M1 H6M4 0.8400 . ? C6M1 H6M5 0.9800 . ? C6M1 H6M6 0.9800 . ? C6M1 H6M7 0.9800 . ? O7M C7M 1.341(14) . ? O7M H7M 0.8400 . ? C7M H7M1 0.9800 . ? C7M H7M2 0.9800 . ? C7M H7M3 0.9800 . ? O8M C8M 1.48(3) . ? O8M H8M 0.8400 . ? C8M H8M1 0.9800 . ? C8M H8M2 0.9800 . ? C8M H8M3 0.9800 . ? O9M C9M 1.62(3) . ? O9M H9M 0.8400 . ? C9M H9M1 0.9800 . ? C9M H9M2 0.9800 . ? C9M H9M3 0.9800 . ? O10M C10M 1.44(3) . ? O10M H10M 0.8400 . ? C10M H10C 0.9800 . ? C10M H10D 0.9800 . ? C10M H10E 0.9800 . ? O11M C11M 1.22(5) . ? O11M H11M 0.8400 . ? C11M H11D 0.9800 . ? C11M H11E 0.9800 . ? C11M H11F 0.9800 . ? 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 Co1 O3 88.3(3) . . ? N2 Co1 O6 93.4(3) . . ? O3 Co1 O6 89.8(3) . . ? N2 Co1 N1 176.2(3) . . ? O3 Co1 N1 93.6(3) . . ? O6 Co1 N1 89.9(3) . . ? N2 Co1 O5 87.2(3) . . ? O3 Co1 O5 91.7(3) . . ? O6 Co1 O5 178.4(3) . . ? N1 Co1 O5 89.5(3) . . ? N2 Co1 O1 94.3(3) . . ? O3 Co1 O1 177.0(3) . . ? O6 Co1 O1 91.6(3) . . ? N1 Co1 O1 83.6(3) . . ? O5 Co1 O1 86.9(3) . . ? N2 Co1 Co2 92.5(2) . . ? O3 Co1 Co2 132.9(2) . . ? O6 Co1 Co2 137.1(2) . . ? N1 Co1 Co2 83.8(2) . . ? O5 Co1 Co2 41.34(19) . . ? O1 Co1 Co2 45.57(18) . . ? O1B Co3 O1A 74.2(10) . . ? O1B Co3 O2B 91.9(10) . . ? O1A Co3 O2B 17.8(4) . . ? O1B Co3 O7 174.8(13) . . ? O1A Co3 O7 107.8(4) . . ? O2B Co3 O7 89.9(4) . . ? O1B Co3 O4 106.8(10) . . ? O1A Co3 O4 176.3(5) . . ? O2B Co3 O4 161.3(4) . . ? O7 Co3 O4 71.6(2) . . ? O1B Co3 O2A 12.0(16) . . ? O1A Co3 O2A 85.4(11) . . ? O2B Co3 O2A 103.2(11) . . ? O7 Co3 O2A 166.8(11) . . ? O4 Co3 O2A 95.3(10) . . ? O1B Co3 O10 93.7(13) . . ? O1A Co3 O10 100.0(5) . . ? O2B Co3 O10 96.9(4) . . ? O7 Co3 O10 81.2(2) . . ? O4 Co3 O10 83.5(2) . . ? O2A Co3 O10 96.1(13) . . ? O1B Co3 O1 103.0(12) . . ? O1A Co3 O1 96.6(5) . . ? O2B Co3 O1 95.0(4) . . ? O7 Co3 O1 81.7(2) . . ? O4 Co3 O1 79.7(2) . . ? O2A Co3 O1 97.8(12) . . ? O10 Co3 O1 159.1(2) . . ? O1B Co3 Co4 126.5(12) . . ? O1A Co3 Co4 137.5(4) . . ? O2B Co3 Co4 123.8(4) . . ? O7 Co3 Co4 48.83(17) . . ? O4 Co3 Co4 44.82(16) . . ? O2A Co3 Co4 120.4(12) . . ? O10 Co3 Co4 48.31(15) . . ? O1 Co3 Co4 110.85(16) . . ? O1B Co3 Co2 138.1(9) . . ? O1A Co3 Co2 129.1(4) . . ? O2B Co3 Co2 116.1(4) . . ? O7 Co3 Co2 44.39(17) . . ? O4 Co3 Co2 47.91(16) . . ? O2A Co3 Co2 127.2(10) . . ? O10 Co3 Co2 111.75(16) . . ? O1 Co3 Co2 47.36(16) . . ? Co4 Co3 Co2 63.89(5) . . ? N3 Co5 N4 174.4(3) . . ? N3 Co5 O9 94.5(3) . . ? N4 Co5 O9 90.8(3) . . ? N3 Co5 O8 86.0(3) . . ? N4 Co5 O8 88.8(3) . . ? O9 Co5 O8 179.5(3) . . ? N3 Co5 O12 88.8(3) . . ? N4 Co5 O12 93.0(3) . . ? O9 Co5 O12 90.2(3) . . ? O8 Co5 O12 90.1(3) . . ? N3 Co5 O10 94.6(3) . . ? N4 Co5 O10 83.4(3) . . ? O9 Co5 O10 92.2(3) . . ? O8 Co5 O10 87.6(3) . . ? O12 Co5 O10 175.7(3) . . ? N3 Co5 Co4 92.6(2) . . ? N4 Co5 Co4 82.2(2) . . ? O9 Co5 Co4 138.4(2) . . ? O8 Co5 Co4 41.28(18) . . ? O12 Co5 Co4 130.9(2) . . ? O10 Co5 Co4 46.41(17) . . ? O5 Co2 O7 159.4(2) . . ? O5 Co2 O15 94.5(3) . . ? O7 Co2 O15 101.3(3) . . ? O5 Co2 O1 79.5(2) . . ? O7 Co2 O1 85.1(2) . . ? O15 Co2 O1 173.6(3) . . ? O5 Co2 O4 91.0(2) . . ? O7 Co2 O4 72.9(2) . . ? O15 Co2 O4 102.1(3) . . ? O1 Co2 O4 80.2(2) . . ? O5 Co2 Co3 112.46(18) . . ? O7 Co2 Co3 47.07(16) . . ? O15 Co2 Co3 136.8(2) . . ? O1 Co2 Co3 48.72(16) . . ? O4 Co2 Co3 47.22(16) . . ? O5 Co2 Co1 39.47(17) . . ? O7 Co2 Co1 124.23(17) . . ? O15 Co2 Co1 133.8(2) . . ? O1 Co2 Co1 40.04(16) . . ? O4 Co2 Co1 85.85(16) . . ? Co3 Co2 Co1 80.67(5) . . ? O8 Co4 O4 159.1(2) . . ? O8 Co4 O14 95.2(3) . . ? O4 Co4 O14 99.6(3) . . ? O8 Co4 O10 79.3(2) . . ? O4 Co4 O10 86.3(2) . . ? O14 Co4 O10 174.1(3) . . ? O8 Co4 O7 90.2(2) . . ? O4 Co4 O7 72.4(2) . . ? O14 Co4 O7 102.0(3) . . ? O10 Co4 O7 80.2(2) . . ? O8 Co4 Co3 111.77(18) . . ? O4 Co4 Co3 47.74(17) . . ? O14 Co4 Co3 136.4(2) . . ? O10 Co4 Co3 48.70(16) . . ? O7 Co4 Co3 47.08(15) . . ? O8 Co4 Co5 38.67(17) . . ? O4 Co4 Co5 126.03(18) . . ? O14 Co4 Co5 133.6(2) . . ? O10 Co4 Co5 40.74(15) . . ? O7 Co4 Co5 86.05(17) . . ? Co3 Co4 Co5 81.27(5) . . ? C1 O1 Co1 108.8(5) . . ? C1 O1 Co2 118.8(5) . . ? Co1 O1 Co2 94.4(3) . . ? C1 O1 Co3 110.9(5) . . ? Co1 O1 Co3 135.4(3) . . ? Co2 O1 Co3 83.9(2) . . ? C3 O2 H2 109.5 . . ? C7 O3 Co1 124.1(6) . . ? C18 O4 Co4 124.5(5) . . ? C18 O4 Co3 127.9(6) . . ? Co4 O4 Co3 87.4(2) . . ? C18 O4 Co2 126.2(5) . . ? Co4 O4 Co2 93.6(2) . . ? Co3 O4 Co2 84.9(2) . . ? C16 O5 Co1 107.9(5) . . ? C16 O5 Co2 116.5(6) . . ? Co1 O5 Co2 99.2(3) . . ? C22 O6 Co1 126.2(6) . . ? C31 O7 Co2 125.6(5) . . ? C31 O7 Co3 126.1(6) . . ? Co2 O7 Co3 88.5(2) . . ? C31 O7 Co4 126.9(6) . . ? Co2 O7 Co4 93.1(3) . . ? Co3 O7 Co4 84.1(2) . . ? C33 O8 Co5 109.2(5) . . ? C33 O8 Co4 116.2(6) . . ? Co5 O8 Co4 100.1(3) . . ? C37 O9 Co5 127.5(6) . . ? C46 O10 Co5 106.8(5) . . ? C46 O10 Co4 119.2(5) . . ? Co5 O10 Co4 92.8(2) . . ? C46 O10 Co3 114.1(5) . . ? Co5 O10 Co3 135.3(3) . . ? Co4 O10 Co3 83.0(2) . . ? C48 O11 H11 109.5 . . ? C52 O12 Co5 121.7(6) . . ? C64 O14 Co4 129.5(7) . . ? C64 O15 Co2 127.0(7) . . ? C5 N1 C2 119.6(8) . . ? C5 N1 Co1 124.8(7) . . ? C2 N1 Co1 115.4(6) . . ? C20 N2 C17 118.1(8) . . ? C20 N2 Co1 128.3(7) . . ? C17 N2 Co1 113.5(6) . . ? C35 N3 C32 120.2(8) . . ? C35 N3 Co5 125.3(6) . . ? C32 N3 Co5 114.4(6) . . ? C50 N4 C47 118.8(8) . . ? C50 N4 Co5 125.5(7) . . ? C47 N4 Co5 115.2(6) . . ? O1 C1 C2 109.2(8) . . ? O1 C1 H1A 109.8 . . ? C2 C1 H1A 109.8 . . ? O1 C1 H1B 109.8 . . ? C2 C1 H1B 109.8 . . ? H1A C1 H1B 108.3 . . ? N1 C2 C4 111.5(8) . . ? N1 C2 C3 108.7(8) . . ? C4 C2 C3 110.2(9) . . ? N1 C2 C1 104.5(8) . . ? C4 C2 C1 109.0(8) . . ? C3 C2 C1 112.8(8) . . ? O2 C3 C2 112.7(8) . . ? O2 C3 H3A 109.1 . . ? C2 C3 H3A 109.1 . . ? O2 C3 H3B 109.1 . . ? C2 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 C6 126.4(9) . . ? N1 C5 H5A 116.8 . . ? C6 C5 H5A 116.8 . . ? C7 C6 C15 119.2(11) . . ? C7 C6 C5 120.8(9) . . ? C15 C6 C5 119.7(10) . . ? O3 C7 C6 125.7(10) . . ? O3 C7 C8 114.8(11) . . ? C6 C7 C8 119.3(11) . . ? C9 C8 C7 121.5(13) . . ? C9 C8 H8A 119.3 . . ? C7 C8 H8A 119.3 . . ? C8 C9 C10 121.8(13) . . ? C8 C9 H9A 119.1 . . ? C10 C9 H9A 119.1 . . ? C9 C10 C11 123.3(14) . . ? C9 C10 C15 119.5(12) . . ? C11 C10 C15 117.2(14) . . ? C12 C11 C10 123.9(16) . . ? C12 C11 H11A 118.0 . . ? C10 C11 H11A 118.0 . . ? C11 C12 C13 118.9(16) . . ? C11 C12 H12A 120.6 . . ? C13 C12 H12A 120.6 . . ? C14 C13 C12 120.4(16) . . ? C14 C13 H13A 119.8 . . ? C12 C13 H13A 119.8 . . ? C15 C14 C13 120.8(15) . . ? C15 C14 H14A 119.6 . . ? C13 C14 H14A 119.6 . . ? C14 C15 C6 122.9(12) . . ? C14 C15 C10 118.8(12) . . ? C6 C15 C10 118.3(12) . . ? O5 C16 C17 112.1(8) . . ? O5 C16 H16A 109.2 . . ? C17 C16 H16A 109.2 . . ? O5 C16 H16B 109.2 . . ? C17 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C18 C17 C19 110.4(8) . . ? C18 C17 N2 109.7(7) . . ? C19 C17 N2 111.7(7) . . ? C18 C17 C16 113.2(8) . . ? C19 C17 C16 108.3(8) . . ? N2 C17 C16 103.4(7) . . ? O4 C18 C17 115.1(8) . . ? O4 C18 H18A 108.5 . . ? C17 C18 H18A 108.5 . . ? O4 C18 H18B 108.5 . . ? C17 C18 H18B 108.5 . . ? H18A C18 H18B 107.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N2 C20 C21 125.7(8) . . ? N2 C20 H20A 117.1 . . ? C21 C20 H20A 117.1 . . ? C22 C21 C30 120.3(8) . . ? C22 C21 C20 119.6(8) . . ? C30 C21 C20 120.1(8) . . ? O6 C22 C21 126.7(8) . . ? O6 C22 C23 114.3(9) . . ? C21 C22 C23 119.0(9) . . ? C24 C23 C22 119.5(10) . . ? C24 C23 H23A 120.3 . . ? C22 C23 H23A 120.3 . . ? C23 C24 C25 123.5(9) . . ? C23 C24 H24 118.2 . . ? C25 C24 H24 118.2 . . ? C26 C25 C24 121.6(10) . . ? C26 C25 C30 121.1(10) . . ? C24 C25 C30 117.3(9) . . ? C27 C26 C25 123.5(11) . . ? C27 C26 H26A 118.2 . . ? C25 C26 H26A 118.2 . . ? C26 C27 C28 116.2(11) . . ? C26 C27 H27A 121.9 . . ? C28 C27 H27A 121.9 . . ? C27 C28 C29 122.3(11) . . ? C27 C28 H28A 118.9 . . ? C29 C28 H28A 118.9 . . ? C30 C29 C28 120.9(10) . . ? C30 C29 H29A 119.5 . . ? C28 C29 H29A 119.5 . . ? C29 C30 C25 115.9(9) . . ? C29 C30 C21 123.6(9) . . ? C25 C30 C21 120.4(8) . . ? O7 C31 C32 114.8(8) . . ? O7 C31 H31A 108.6 . . ? C32 C31 H31A 108.6 . . ? O7 C31 H31B 108.6 . . ? C32 C31 H31B 108.6 . . ? H31A C31 H31B 107.6 . . ? N3 C32 C33 105.4(8) . . ? N3 C32 C31 108.7(7) . . ? C33 C32 C31 112.7(8) . . ? N3 C32 C34 113.0(8) . . ? C33 C32 C34 109.9(8) . . ? C31 C32 C34 107.2(8) . . ? O8 C33 C32 110.7(7) . . ? O8 C33 H33A 109.5 . . ? C32 C33 H33A 109.5 . . ? O8 C33 H33B 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 108.1 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N3 C35 C36 127.4(9) . . ? N3 C35 H35A 116.3 . . ? C36 C35 H35A 116.3 . . ? C35 C36 C37 120.4(9) . . ? C35 C36 C45 121.3(9) . . ? C37 C36 C45 118.3(8) . . ? O9 C37 C38 117.8(9) . . ? O9 C37 C36 124.6(9) . . ? C38 C37 C36 117.5(9) . . ? C39 C38 C37 124.2(10) . . ? C39 C38 H38A 117.9 . . ? C37 C38 H38A 117.9 . . ? C38 C39 C40 120.6(10) . . ? C38 C39 H39A 119.7 . . ? C40 C39 H39A 119.7 . . ? C45 C40 C41 121.0(10) . . ? C45 C40 C39 118.6(9) . . ? C41 C40 C39 120.4(10) . . ? C42 C41 C40 118.9(11) . . ? C42 C41 H41A 120.5 . . ? C40 C41 H41A 120.5 . . ? C41 C42 C43 120.6(11) . . ? C41 C42 H42A 119.7 . . ? C43 C42 H42A 119.7 . . ? C44 C43 C42 120.4(11) . . ? C44 C43 H43A 119.8 . . ? C42 C43 H43A 119.8 . . ? C43 C44 C45 121.3(10) . . ? C43 C44 H44A 119.3 . . ? C45 C44 H44A 119.3 . . ? C44 C45 C40 117.7(9) . . ? C44 C45 C36 121.5(9) . . ? C40 C45 C36 120.7(8) . . ? O10 C46 C47 109.3(7) . . ? O10 C46 H46A 109.8 . . ? C47 C46 H46A 109.8 . . ? O10 C46 H46B 109.8 . . ? C47 C46 H46B 109.8 . . ? H46A C46 H46B 108.3 . . ? N4 C47 C46 105.8(7) . . ? N4 C47 C49 113.4(8) . . ? C46 C47 C49 108.8(8) . . ? N4 C47 C48 109.1(7) . . ? C46 C47 C48 111.2(8) . . ? C49 C47 C48 108.5(8) . . ? O11 C48 C47 113.4(7) . . ? O11 C48 H48A 108.9 . . ? C47 C48 H48A 108.9 . . ? O11 C48 H48B 108.9 . . ? C47 C48 H48B 108.9 . . ? H48A C48 H48B 107.7 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N4 C50 C51 124.4(9) . . ? N4 C50 H50A 117.8 . . ? C51 C50 H50A 117.8 . . ? C50 C51 C52 121.1(9) . . ? C50 C51 C60 119.7(10) . . ? C52 C51 C60 119.0(9) . . ? O12 C52 C53 115.6(10) . . ? O12 C52 C51 125.0(9) . . ? C53 C52 C51 119.5(9) . . ? C54 C53 C52 121.8(11) . . ? C54 C53 H53A 119.1 . . ? C52 C53 H53A 119.1 . . ? C53 C54 C55 121.0(11) . . ? C53 C54 H54A 119.5 . . ? C55 C54 H54A 119.5 . . ? C60 C55 C54 119.7(10) . . ? C60 C55 C56 118.1(12) . . ? C54 C55 C56 122.1(11) . . ? C57 C56 C55 123.7(13) . . ? C57 C56 H56A 118.2 . . ? C55 C56 H56A 118.2 . . ? C56 C57 C58 119.4(13) . . ? C56 C57 H57A 120.3 . . ? C58 C57 H57A 120.3 . . ? C59 C58 C57 118.5(13) . . ? C59 C58 H58A 120.7 . . ? C57 C58 H58A 120.7 . . ? C60 C59 C58 122.0(12) . . ? C60 C59 H59A 119.0 . . ? C58 C59 H59A 119.0 . . ? C59 C60 C55 118.1(10) . . ? C59 C60 C51 122.9(10) . . ? C55 C60 C51 119.0(10) . . ? O14 C64 O15 125.4(9) . . ? O14 C64 C65 117.4(11) . . ? O15 C64 C65 117.0(11) . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C2A O1A Co3 134.8(14) . . ? C11A O2A Co3 123(2) . . ? O2A C11A C1A 133(3) . . ? O2A C11A H11B 113.3 . . ? C1A C11A H11B 113.3 . . ? C6A C1A C11A 121(2) . . ? C6A C1A C2A 121(3) . . ? C11A C1A C2A 117(2) . . ? O1A C2A C3A 121(2) . . ? O1A C2A C1A 123.3(18) . . ? C3A C2A C1A 115(2) . . ? C4A C3A C2A 128(2) . . ? C4A C3A H3A1 116.1 . . ? C2A C3A H3A1 116.1 . . ? C3A C4A C5A 115(2) . . ? C3A C4A H4A1 122.4 . . ? C5A C4A H4A1 122.4 . . ? C6A C5A C10A 123(3) . . ? C6A C5A C4A 117(2) . . ? C10A C5A C4A 120(3) . . ? C7A C6A C5A 111(3) . . ? C7A C6A C1A 125(3) . . ? C5A C6A C1A 123(3) . . ? C6A C7A C8A 126(4) . . ? C6A C7A H7A 116.9 . . ? C8A C7A H7A 116.9 . . ? C9A C8A C7A 116(3) . . ? C9A C8A H8A1 122.2 . . ? C7A C8A H8A1 122.2 . . ? C10A C9A C8A 127(5) . . ? C10A C9A H9A1 116.5 . . ? C8A C9A H9A1 116.5 . . ? C9A C10A C5A 116(5) . . ? C9A C10A H10A 121.9 . . ? C5A C10A H10A 121.9 . . ? C3B O1B Co3 129(2) . . ? C11B O2B Co3 121.9(19) . . ? O2B C11B C4B 129(3) . . ? O2B C11B H11C 115.3 . . ? C4B C11B H11C 115.3 . . ? C2B C1B C6B 115(4) . . ? C2B C1B H1B1 122.7 . . ? C6B C1B H1B1 122.7 . . ? C1B C2B C3B 120(3) . . ? C1B C2B H2B 119.8 . . ? C3B C2B H2B 119.8 . . ? C4B C3B O1B 124(3) . . ? C4B C3B C2B 123(3) . . ? O1B C3B C2B 113(3) . . ? C3B C4B C5B 119(3) . . ? C3B C4B C11B 123(2) . . ? C5B C4B C11B 119(2) . . ? C10B C5B C6B 113(3) . . ? C10B C5B C4B 130(3) . . ? C6B C5B C4B 118(3) . . ? C5B C6B C1B 125(3) . . ? C5B C6B C7B 117(4) . . ? C1B C6B C7B 117(4) . . ? C8B C7B C6B 115(4) . . ? C8B C7B H7B 122.7 . . ? C6B C7B H7B 122.7 . . ? C9B C8B C7B 135(5) . . ? C9B C8B H8B 112.5 . . ? C7B C8B H8B 112.5 . . ? C8B C9B C10B 107(4) . . ? C8B C9B H9B 126.7 . . ? C10B C9B H9B 126.7 . . ? C5B C10B C9B 134(3) . . ? C5B C10B H10B 112.8 . . ? C9B C10B H10B 112.8 . . ? C1M O1M H1M 109.5 . . ? O1M C1M H1M1 109.5 . . ? O1M C1M H1M2 109.5 . . ? H1M1 C1M H1M2 109.5 . . ? O1M C1M H1M3 109.5 . . ? H1M1 C1M H1M3 109.5 . . ? H1M2 C1M H1M3 109.5 . . ? C2M O2M H2M 109.5 . . ? O2M C2M H2M1 109.5 . . ? O2M C2M H2M2 109.5 . . ? H2M1 C2M H2M2 109.5 . . ? O2M C2M H2M3 109.5 . . ? H2M1 C2M H2M3 109.5 . . ? H2M2 C2M H2M3 109.5 . . ? C3M2 O3M C3M1 137(2) . . ? C3M2 O3M H3M 92.4 . . ? C3M1 O3M H3M 109.6 . . ? O3M C3M1 H3M1 109.5 . . ? O3M C3M1 H3M2 109.5 . . ? H3M1 C3M1 H3M2 109.5 . . ? O3M C3M1 H3M3 109.5 . . ? H3M1 C3M1 H3M3 109.5 . . ? H3M2 C3M1 H3M3 109.5 . . ? O3M C3M2 H3M4 109.5 . . ? H3M C3M2 H3M4 87.2 . . ? O3M C3M2 H3M5 109.5 . . ? H3M C3M2 H3M5 95.9 . . ? H3M4 C3M2 H3M5 109.5 . . ? O3M C3M2 H3M6 109.5 . . ? H3M C3M2 H3M6 141.8 . . ? H3M4 C3M2 H3M6 109.5 . . ? H3M5 C3M2 H3M6 109.5 . . ? O4M2 C4M H4M1 109.5 . . ? O4M2 C4M H4M2 109.5 . . ? H4M1 C4M H4M2 109.5 . . ? O4M2 C4M H4M3 109.5 . . ? H4M1 C4M H4M3 109.5 . . ? H4M2 C4M H4M3 109.5 . . ? O4M2 C4M H4M4 126.8 . . ? H4M2 C4M H4M4 118.6 . . ? H4M3 C4M H4M5 174.5 . . ? H4M4 C4M H4M5 109.5 . . ? O4M2 C4M H4M6 121.0 . . ? H4M1 C4M H4M6 128.0 . . ? H4M4 C4M H4M6 109.5 . . ? H4M5 C4M H4M6 109.5 . . ? C4M O4M2 H4M7 136.0 . . ? H4M5 O4M2 H4M7 172.2 . . ? C4M O4M2 H4M8 110.9 . . ? H4M5 O4M2 H4M8 132.8 . . ? H4M7 O4M2 H4M8 53.9 . . ? C5M O5M H5M 109.5 . . ? O5M C5M H5M1 109.5 . . ? O5M C5M H5M2 109.5 . . ? H5M1 C5M H5M2 109.5 . . ? O5M C5M H5M3 109.5 . . ? H5M1 C5M H5M3 109.5 . . ? H5M2 C5M H5M3 109.5 . . ? C6M O6M H6M 109.5 . . ? O6M C6M H6M1 109.5 . . ? O6M C6M H6M2 109.5 . . ? H6M1 C6M H6M2 109.5 . . ? O6M C6M H6M3 109.5 . . ? H6M1 C6M H6M3 109.5 . . ? H6M2 C6M H6M3 109.5 . . ? C6M1 O6M1 H6M4 109.5 . . ? C7M O7M H7M 109.5 . . ? O7M C7M H7M1 109.5 . . ? O7M C7M H7M2 109.5 . . ? H7M1 C7M H7M2 109.5 . . ? O7M C7M H7M3 109.5 . . ? H7M1 C7M H7M3 109.5 . . ? H7M2 C7M H7M3 109.5 . . ? C8M O8M H8M 109.5 . . ? O8M C8M H8M1 109.5 . . ? O8M C8M H8M2 109.5 . . ? H8M1 C8M H8M2 109.5 . . ? O8M C8M H8M3 109.5 . . ? H8M1 C8M H8M3 109.5 . . ? H8M2 C8M H8M3 109.5 . . ? C9M O9M H9M 109.5 . . ? O9M C9M H9M1 109.5 . . ? O9M C9M H9M2 109.5 . . ? H9M1 C9M H9M2 109.5 . . ? O9M C9M H9M3 109.5 . . ? H9M1 C9M H9M3 109.5 . . ? H9M2 C9M H9M3 109.5 . . ? C10M O10M H10M 109.5 . . ? O10M C10M H10C 109.5 . . ? O10M C10M H10D 109.5 . . ? H10C C10M H10D 109.5 . . ? O10M C10M H10E 109.5 . . ? H10C C10M H10E 109.5 . . ? H10D C10M H10E 109.5 . . ? C11M O11M H11M 109.5 . . ? O11M C11M H11D 109.5 . . ? O11M C11M H11E 109.5 . . ? H11D C11M H11E 109.5 . . ? O11M C11M H11F 109.5 . . ? H11D C11M H11F 109.5 . . ? H11E C11M H11F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.624 _refine_diff_density_min -0.342 _refine_diff_density_rms 0.080 data_at328 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H38 N4 Ni O6' _chemical_formula_weight 657.39 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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7371(17) _cell_length_b 13.993(2) _cell_length_c 15.172(3) _cell_angle_alpha 110.521(13) _cell_angle_beta 103.869(15) _cell_angle_gamma 103.934(14) _cell_volume 1575.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 6313 _cell_measurement_theta_min 1.53 _cell_measurement_theta_max 25.50 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.386 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 692 _exptl_absorpt_coefficient_mu 0.668 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8509 _exptl_absorpt_correction_T_max 0.8893 _exptl_absorpt_process_details 'XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate ( 34 cm diameter )' _diffrn_detector_type 'STOE' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9682 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0983 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 25.63 _reflns_number_total 5891 _reflns_number_gt 3624 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0200P)^2^+0.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5891 _refine_ls_number_parameters 417 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0845 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.0813 _refine_ls_wR_factor_gt 0.0759 _refine_ls_goodness_of_fit_ref 0.953 _refine_ls_restrained_S_all 0.955 _refine_ls_shift/su_max 0.001 _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 0.88365(6) 0.23332(4) 0.98409(3) 0.03299(13) Uani 1 1 d . . . C1 C 0.6226(4) 0.0100(3) 0.8606(3) 0.0346(8) Uani 1 1 d . . . C2 C 0.5089(4) -0.0847(3) 0.8569(3) 0.0391(8) Uani 1 1 d . . . H2A H 0.4946 -0.0839 0.9173 0.047 Uiso 1 1 calc R . . C3 C 0.4208(4) -0.1759(3) 0.7693(3) 0.0414(8) Uani 1 1 d . . . H3A H 0.3476 -0.2377 0.7700 0.050 Uiso 1 1 calc R . . C4 C 0.4347(4) -0.1816(3) 0.6765(3) 0.0385(8) Uani 1 1 d . . . C5 C 0.3498(4) -0.2799(3) 0.5864(3) 0.0507(10) Uani 1 1 d . . . H5A H 0.2809 -0.3425 0.5884 0.061 Uiso 1 1 calc R . . C6 C 0.3645(5) -0.2868(3) 0.4974(3) 0.0565(11) Uani 1 1 d . . . H6A H 0.3061 -0.3531 0.4378 0.068 Uiso 1 1 calc R . . C7 C 0.4665(5) -0.1950(3) 0.4946(3) 0.0538(10) Uani 1 1 d . . . H7A H 0.4777 -0.1989 0.4328 0.065 Uiso 1 1 calc R . . C8 C 0.5509(4) -0.0989(3) 0.5811(3) 0.0448(9) Uani 1 1 d . . . H8A H 0.6195 -0.0376 0.5774 0.054 Uiso 1 1 calc R . . C9 C 0.5395(4) -0.0879(3) 0.6755(3) 0.0366(8) Uani 1 1 d . . . C10 C 0.6331(4) 0.0102(3) 0.7687(2) 0.0326(7) Uani 1 1 d . . . C11 C 0.7322(4) 0.1055(2) 0.7640(2) 0.0326(7) Uani 1 1 d . . . H11A H 0.7219 0.0994 0.6983 0.039 Uiso 1 1 calc R . . C12 C 0.9213(4) 0.2850(2) 0.8137(2) 0.0339(8) Uani 1 1 d . . . C13 C 1.0889(4) 0.3518(3) 0.9017(3) 0.0405(8) Uani 1 1 d . . . H13A H 1.1697 0.3136 0.8922 0.049 Uiso 1 1 calc R . . H13B H 1.1360 0.4236 0.9018 0.049 Uiso 1 1 calc R . . C14 C 0.8123(4) 0.3546(3) 0.8018(3) 0.0399(8) Uani 1 1 d . . . H14A H 0.8640 0.4043 0.7753 0.048 Uiso 1 1 calc R . . H14B H 0.6994 0.3053 0.7508 0.048 Uiso 1 1 calc R . . C15 C 0.9609(4) 0.2440(3) 0.7175(3) 0.0441(9) Uani 1 1 d . . . H15A H 0.8553 0.2005 0.6596 0.066 Uiso 1 1 calc R . . H15B H 1.0294 0.1987 0.7221 0.066 Uiso 1 1 calc R . . H15C H 1.0234 0.3065 0.7092 0.066 Uiso 1 1 calc R . . C16 C 0.7052(4) 0.3729(2) 1.0818(2) 0.0318(7) Uani 1 1 d . . . C17 C 0.5719(4) 0.4157(3) 1.0696(3) 0.0380(8) Uani 1 1 d . . . H17A H 0.4994 0.3965 1.0036 0.046 Uiso 1 1 calc R . . C18 C 0.5466(4) 0.4824(3) 1.1495(3) 0.0399(8) Uani 1 1 d . . . H18A H 0.4550 0.5074 1.1381 0.048 Uiso 1 1 calc R . . C19 C 0.6533(4) 0.5163(3) 1.2503(3) 0.0367(8) Uani 1 1 d . . . C20 C 0.6295(5) 0.5899(3) 1.3327(3) 0.0480(9) Uani 1 1 d . . . H20A H 0.5385 0.6152 1.3205 0.058 Uiso 1 1 calc R . . C21 C 0.7335(5) 0.6254(3) 1.4290(3) 0.0552(10) Uani 1 1 d . . . H21A H 0.7145 0.6740 1.4837 0.066 Uiso 1 1 calc R . . C22 C 0.8679(5) 0.5896(3) 1.4463(3) 0.0497(9) Uani 1 1 d . . . H22A H 0.9426 0.6151 1.5133 0.060 Uiso 1 1 calc R . . C23 C 0.8940(4) 0.5176(3) 1.3675(2) 0.0397(8) Uani 1 1 d . . . H23A H 0.9876 0.4951 1.3818 0.048 Uiso 1 1 calc R . . C24 C 0.7876(4) 0.4760(3) 1.2663(2) 0.0337(8) Uani 1 1 d . . . C25 C 0.8103(4) 0.4002(2) 1.1805(2) 0.0304(7) Uani 1 1 d . . . C26 C 0.9332(4) 0.3501(2) 1.1995(2) 0.0342(8) Uani 1 1 d . . . H26A H 0.9926 0.3700 1.2682 0.041 Uiso 1 1 calc R . . C27 C 1.0975(4) 0.2351(3) 1.1697(3) 0.0397(8) Uani 1 1 d . . . C28 C 1.1901(4) 0.2168(3) 1.0950(3) 0.0433(9) Uani 1 1 d . . . H28A H 1.2724 0.2879 1.1096 0.052 Uiso 1 1 calc R . . H28B H 1.2539 0.1694 1.1046 0.052 Uiso 1 1 calc R . . C29 C 1.0051(5) 0.1296(3) 1.1711(3) 0.0576(11) Uani 1 1 d . . . H29A H 1.0895 0.1091 1.2095 0.069 Uiso 1 1 calc R . . H29B H 0.9289 0.1442 1.2089 0.069 Uiso 1 1 calc R . . C30 C 1.2273(5) 0.3100(3) 1.2744(3) 0.0588(11) Uani 1 1 d . . . H30A H 1.1705 0.3222 1.3236 0.088 Uiso 1 1 calc R . . H30B H 1.2864 0.3800 1.2761 0.088 Uiso 1 1 calc R . . H30C H 1.3090 0.2760 1.2912 0.088 Uiso 1 1 calc R . . C31 C 0.3600(5) 0.1571(4) 0.7702(4) 0.0645(12) Uani 1 1 d . . . C32 C 0.3365(5) 0.1304(3) 0.8515(3) 0.0594(11) Uani 1 1 d . . . H32A H 0.4425 0.1674 0.9096 0.071 Uiso 1 1 calc R . . H32B H 0.3029 0.0512 0.8289 0.071 Uiso 1 1 calc R . . H32C H 0.2483 0.1547 0.8708 0.071 Uiso 1 1 calc R . . C33 C 0.0182(6) -0.0641(4) 0.6016(3) 0.0670(12) Uani 1 1 d . . . C34 C 0.0974(8) -0.1026(5) 0.5310(4) 0.109(2) Uani 1 1 d . . . H34A H 0.0526 -0.0906 0.4716 0.131 Uiso 1 1 calc R . . H34B H 0.0743 -0.1808 0.5105 0.131 Uiso 1 1 calc R . . H34C H 0.2195 -0.0627 0.5624 0.131 Uiso 1 1 calc R . . N1 N 0.8328(3) 0.1976(2) 0.8371(2) 0.0324(6) Uani 1 1 d . . . N2 N 0.9717(3) 0.2821(2) 1.13476(19) 0.0328(6) Uani 1 1 d . . . N3 N 0.3775(6) 0.1766(4) 0.7068(4) 0.1025(16) Uani 1 1 d . . . N4 N -0.0416(5) -0.0317(4) 0.6581(3) 0.0868(12) Uani 1 1 d . . . O1 O 0.7097(3) 0.09105(18) 0.94986(17) 0.0381(6) Uani 1 1 d . . . O2 O 1.0727(3) 0.36862(18) 0.99698(18) 0.0402(6) Uani 1 1 d D . . H21 H 1.102(4) 0.436(2) 1.037(2) 0.048 Uiso 1 1 d D . . O3 O 0.7910(3) 0.41835(18) 0.89121(18) 0.0427(6) Uani 1 1 d D . . H31 H 0.762(4) 0.381(3) 0.924(2) 0.051 Uiso 1 1 d D . . O4 O 0.7216(3) 0.31255(17) 0.99967(16) 0.0370(5) Uani 1 1 d . . . O5 O 1.0784(3) 0.16751(18) 0.99202(18) 0.0391(6) Uani 1 1 d D . . H51 H 1.055(4) 0.101(2) 0.970(3) 0.047 Uiso 1 1 d D . . O6 O 0.9111(4) 0.0409(2) 1.0799(2) 0.0714(8) Uani 1 1 d D . . H61 H 0.8112 0.0585 1.0392 0.086 Uiso 1 1 d RD . . 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 0.0376(3) 0.0265(2) 0.0355(2) 0.01268(19) 0.01430(19) 0.01227(19) C1 0.0324(19) 0.0279(19) 0.048(2) 0.0178(17) 0.0181(17) 0.0123(16) C2 0.037(2) 0.035(2) 0.053(2) 0.0244(18) 0.0200(17) 0.0132(17) C3 0.032(2) 0.030(2) 0.063(3) 0.0242(19) 0.0165(18) 0.0072(16) C4 0.0324(19) 0.0301(19) 0.049(2) 0.0156(17) 0.0098(16) 0.0104(16) C5 0.044(2) 0.032(2) 0.066(3) 0.0174(19) 0.015(2) 0.0071(17) C6 0.049(2) 0.038(2) 0.050(3) -0.0012(19) 0.006(2) 0.004(2) C7 0.048(2) 0.044(2) 0.045(2) 0.0050(19) 0.0117(19) 0.0050(19) C8 0.046(2) 0.034(2) 0.043(2) 0.0096(17) 0.0150(18) 0.0068(17) C9 0.0287(18) 0.0322(19) 0.045(2) 0.0143(16) 0.0112(16) 0.0098(15) C10 0.0305(18) 0.0284(18) 0.039(2) 0.0141(15) 0.0136(15) 0.0095(15) C11 0.0355(19) 0.0279(19) 0.0324(18) 0.0109(15) 0.0133(15) 0.0101(16) C12 0.038(2) 0.0258(18) 0.0371(19) 0.0146(15) 0.0170(16) 0.0053(15) C13 0.041(2) 0.034(2) 0.046(2) 0.0161(17) 0.0195(17) 0.0081(16) C14 0.051(2) 0.0281(19) 0.043(2) 0.0162(16) 0.0185(18) 0.0139(17) C15 0.048(2) 0.035(2) 0.051(2) 0.0181(17) 0.0248(18) 0.0120(17) C16 0.0341(19) 0.0249(18) 0.041(2) 0.0167(15) 0.0172(16) 0.0098(15) C17 0.0313(19) 0.039(2) 0.044(2) 0.0188(17) 0.0120(16) 0.0136(16) C18 0.031(2) 0.041(2) 0.055(2) 0.0242(18) 0.0188(18) 0.0170(17) C19 0.039(2) 0.0354(19) 0.046(2) 0.0214(17) 0.0217(17) 0.0171(16) C20 0.047(2) 0.053(2) 0.053(3) 0.024(2) 0.022(2) 0.030(2) C21 0.072(3) 0.057(3) 0.046(2) 0.0175(19) 0.030(2) 0.037(2) C22 0.062(3) 0.047(2) 0.043(2) 0.0173(19) 0.0195(19) 0.028(2) C23 0.045(2) 0.040(2) 0.040(2) 0.0185(17) 0.0156(17) 0.0213(17) C24 0.0342(19) 0.0291(18) 0.045(2) 0.0206(16) 0.0184(16) 0.0114(15) C25 0.0311(18) 0.0270(17) 0.0355(19) 0.0159(15) 0.0126(15) 0.0097(14) C26 0.037(2) 0.0324(19) 0.0338(19) 0.0163(16) 0.0118(16) 0.0119(16) C27 0.044(2) 0.043(2) 0.044(2) 0.0222(17) 0.0164(17) 0.0278(18) C28 0.044(2) 0.043(2) 0.051(2) 0.0219(18) 0.0192(19) 0.0228(18) C29 0.079(3) 0.049(3) 0.070(3) 0.033(2) 0.043(3) 0.037(2) C30 0.059(3) 0.073(3) 0.052(3) 0.024(2) 0.015(2) 0.045(2) C31 0.053(3) 0.061(3) 0.099(4) 0.043(3) 0.038(3) 0.030(2) C32 0.046(2) 0.054(3) 0.077(3) 0.024(2) 0.025(2) 0.021(2) C33 0.073(3) 0.076(3) 0.059(3) 0.030(2) 0.025(2) 0.037(3) C34 0.163(6) 0.111(5) 0.103(4) 0.052(4) 0.082(4) 0.085(4) N1 0.0339(16) 0.0259(15) 0.0384(16) 0.0134(13) 0.0150(13) 0.0107(13) N2 0.0341(16) 0.0312(15) 0.0400(16) 0.0177(13) 0.0149(13) 0.0178(13) N3 0.099(3) 0.129(4) 0.150(5) 0.105(4) 0.076(3) 0.059(3) N4 0.077(3) 0.105(3) 0.081(3) 0.033(3) 0.038(2) 0.037(3) O1 0.0454(14) 0.0286(13) 0.0378(14) 0.0126(11) 0.0170(12) 0.0093(11) O2 0.0404(14) 0.0287(13) 0.0408(15) 0.0098(11) 0.0110(12) 0.0064(12) O3 0.0577(16) 0.0289(14) 0.0452(15) 0.0155(11) 0.0233(13) 0.0171(12) O4 0.0402(14) 0.0346(13) 0.0368(14) 0.0139(11) 0.0144(11) 0.0161(11) O5 0.0462(15) 0.0308(13) 0.0447(15) 0.0155(12) 0.0217(12) 0.0170(12) O6 0.089(2) 0.0582(19) 0.077(2) 0.0333(17) 0.0363(18) 0.0302(17) _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 O1 1.996(2) . ? Ni1 O4 2.006(2) . ? Ni1 N1 2.015(3) . ? Ni1 N2 2.023(3) . ? Ni1 O2 2.105(2) . ? Ni1 O5 2.119(2) . ? C1 O1 1.309(4) . ? C1 C10 1.420(4) . ? C1 C2 1.426(4) . ? C2 C3 1.354(5) . ? C2 H2A 0.9500 . ? C3 C4 1.417(5) . ? C3 H3A 0.9500 . ? C4 C9 1.415(4) . ? C4 C5 1.420(5) . ? C5 C6 1.360(5) . ? C5 H5A 0.9500 . ? C6 C7 1.396(5) . ? C6 H6A 0.9500 . ? C7 C8 1.377(5) . ? C7 H7A 0.9500 . ? C8 C9 1.415(5) . ? C8 H8A 0.9500 . ? C9 C10 1.447(4) . ? C10 C11 1.441(4) . ? C11 N1 1.284(4) . ? C11 H11A 0.9500 . ? C12 N1 1.483(4) . ? C12 C15 1.525(4) . ? C12 C13 1.527(5) . ? C12 C14 1.542(4) . ? C13 O2 1.428(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 O3 1.422(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 O4 1.301(3) . ? C16 C25 1.415(4) . ? C16 C17 1.435(4) . ? C17 C18 1.350(4) . ? C17 H17A 0.9500 . ? C18 C19 1.423(5) . ? C18 H18A 0.9500 . ? C19 C20 1.412(5) . ? C19 C24 1.426(4) . ? C20 C21 1.358(5) . ? C20 H20A 0.9500 . ? C21 C22 1.388(5) . ? C21 H21A 0.9500 . ? C22 C23 1.377(4) . ? C22 H22A 0.9500 . ? C23 C24 1.410(5) . ? C23 H23A 0.9500 . ? C24 C25 1.455(4) . ? C25 C26 1.443(4) . ? C26 N2 1.281(4) . ? C26 H26A 0.9500 . ? C27 N2 1.495(4) . ? C27 C29 1.513(5) . ? C27 C30 1.518(5) . ? C27 C28 1.531(4) . ? C28 O5 1.435(4) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 O6 1.374(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 N3 1.122(5) . ? C31 C32 1.452(6) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 N4 1.127(5) . ? C33 C34 1.431(6) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? O2 H21 0.85(3) . ? O3 H31 0.88(3) . ? O5 H51 0.82(3) . ? O6 H61 1.0757 . ? 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 O1 Ni1 O4 92.49(9) . . ? O1 Ni1 N1 91.19(10) . . ? O4 Ni1 N1 94.64(9) . . ? O1 Ni1 N2 96.39(10) . . ? O4 Ni1 N2 89.68(9) . . ? N1 Ni1 N2 171.11(11) . . ? O1 Ni1 O2 170.14(9) . . ? O4 Ni1 O2 93.37(9) . . ? N1 Ni1 O2 80.44(10) . . ? N2 Ni1 O2 91.57(11) . . ? O1 Ni1 O5 92.24(9) . . ? O4 Ni1 O5 170.79(10) . . ? N1 Ni1 O5 93.15(9) . . ? N2 Ni1 O5 81.95(9) . . ? O2 Ni1 O5 83.10(9) . . ? O1 C1 C10 124.9(3) . . ? O1 C1 C2 116.6(3) . . ? C10 C1 C2 118.4(3) . . ? C3 C2 C1 121.5(3) . . ? C3 C2 H2A 119.2 . . ? C1 C2 H2A 119.2 . . ? C2 C3 C4 121.9(3) . . ? C2 C3 H3A 119.0 . . ? C4 C3 H3A 119.0 . . ? C9 C4 C3 118.7(3) . . ? C9 C4 C5 120.1(3) . . ? C3 C4 C5 121.2(3) . . ? C6 C5 C4 121.6(4) . . ? C6 C5 H5A 119.2 . . ? C4 C5 H5A 119.2 . . ? C5 C6 C7 119.2(4) . . ? C5 C6 H6A 120.4 . . ? C7 C6 H6A 120.4 . . ? C8 C7 C6 120.2(4) . . ? C8 C7 H7A 119.9 . . ? C6 C7 H7A 119.9 . . ? C7 C8 C9 122.6(4) . . ? C7 C8 H8A 118.7 . . ? C9 C8 H8A 118.7 . . ? C4 C9 C8 116.2(3) . . ? C4 C9 C10 119.7(3) . . ? C8 C9 C10 124.0(3) . . ? C1 C10 C11 122.4(3) . . ? C1 C10 C9 119.5(3) . . ? C11 C10 C9 118.1(3) . . ? N1 C11 C10 128.4(3) . . ? N1 C11 H11A 115.8 . . ? C10 C11 H11A 115.8 . . ? N1 C12 C15 114.6(3) . . ? N1 C12 C13 105.8(3) . . ? C15 C12 C13 107.6(3) . . ? N1 C12 C14 109.6(2) . . ? C15 C12 C14 107.2(3) . . ? C13 C12 C14 112.1(3) . . ? O2 C13 C12 112.8(3) . . ? O2 C13 H13A 109.0 . . ? C12 C13 H13A 109.0 . . ? O2 C13 H13B 109.0 . . ? C12 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? O3 C14 C12 115.5(3) . . ? O3 C14 H14A 108.4 . . ? C12 C14 H14A 108.4 . . ? O3 C14 H14B 108.4 . . ? C12 C14 H14B 108.4 . . ? H14A C14 H14B 107.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O4 C16 C25 124.8(3) . . ? O4 C16 C17 116.5(3) . . ? C25 C16 C17 118.7(3) . . ? C18 C17 C16 121.8(3) . . ? C18 C17 H17A 119.1 . . ? C16 C17 H17A 119.1 . . ? C17 C18 C19 121.8(3) . . ? C17 C18 H18A 119.1 . . ? C19 C18 H18A 119.1 . . ? C20 C19 C18 121.0(3) . . ? C20 C19 C24 120.4(3) . . ? C18 C19 C24 118.5(3) . . ? C21 C20 C19 121.6(3) . . ? C21 C20 H20A 119.2 . . ? C19 C20 H20A 119.2 . . ? C20 C21 C22 119.0(3) . . ? C20 C21 H21A 120.5 . . ? C22 C21 H21A 120.5 . . ? C23 C22 C21 120.7(3) . . ? C23 C22 H22A 119.6 . . ? C21 C22 H22A 119.6 . . ? C22 C23 C24 122.7(3) . . ? C22 C23 H23A 118.6 . . ? C24 C23 H23A 118.6 . . ? C23 C24 C19 115.5(3) . . ? C23 C24 C25 124.8(3) . . ? C19 C24 C25 119.7(3) . . ? C16 C25 C26 122.2(3) . . ? C16 C25 C24 119.4(3) . . ? C26 C25 C24 118.3(3) . . ? N2 C26 C25 127.8(3) . . ? N2 C26 H26A 116.1 . . ? C25 C26 H26A 116.1 . . ? N2 C27 C29 109.0(3) . . ? N2 C27 C30 113.7(3) . . ? C29 C27 C30 107.9(3) . . ? N2 C27 C28 106.1(3) . . ? C29 C27 C28 112.0(3) . . ? C30 C27 C28 108.2(3) . . ? O5 C28 C27 112.9(3) . . ? O5 C28 H28A 109.0 . . ? C27 C28 H28A 109.0 . . ? O5 C28 H28B 109.0 . . ? C27 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? O6 C29 C27 117.6(3) . . ? O6 C29 H29A 107.9 . . ? C27 C29 H29A 107.9 . . ? O6 C29 H29B 107.9 . . ? C27 C29 H29B 107.9 . . ? H29A C29 H29B 107.2 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N3 C31 C32 179.3(5) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N4 C33 C34 178.5(6) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C11 N1 C12 118.8(3) . . ? C11 N1 Ni1 124.8(2) . . ? C12 N1 Ni1 116.47(19) . . ? C26 N2 C27 119.6(3) . . ? C26 N2 Ni1 125.9(2) . . ? C27 N2 Ni1 114.43(18) . . ? C1 O1 Ni1 127.7(2) . . ? C13 O2 Ni1 110.96(19) . . ? C13 O2 H21 113(2) . . ? Ni1 O2 H21 129(2) . . ? C14 O3 H31 113(2) . . ? C16 O4 Ni1 128.8(2) . . ? C28 O5 Ni1 108.34(18) . . ? C28 O5 H51 108(2) . . ? Ni1 O5 H51 120(2) . . ? C29 O6 H61 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.192 _refine_diff_density_min -0.299 _refine_diff_density_rms 0.054 data_at228 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C102 H136 N6 Ni8 O34 S' _chemical_formula_weight 2491.91 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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.5108(11) _cell_length_b 24.3167(12) _cell_length_c 23.3917(11) _cell_angle_alpha 90.00 _cell_angle_beta 104.115(4) _cell_angle_gamma 90.00 _cell_volume 10762.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 37632 _cell_measurement_theta_min 1.36 _cell_measurement_theta_max 24.79 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5208 _exptl_absorpt_coefficient_mu 1.471 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6347 _exptl_absorpt_correction_T_max 0.7476 _exptl_absorpt_process_details 'XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate ( 34 cm diameter )' _diffrn_detector_type 'STOE' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32038 _diffrn_reflns_av_R_equivalents 0.0262 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 25.64 _reflns_number_total 10102 _reflns_number_gt 7633 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0309P)^2^+0.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10102 _refine_ls_number_parameters 707 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0669 _refine_ls_wR_factor_gt 0.0625 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.002 _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 0.686844(17) 0.930578(13) 0.554491(13) 0.04026(8) Uani 1 1 d . . . Ni2 Ni 0.846759(17) 0.911341(13) 0.575063(12) 0.03820(8) Uani 1 1 d . . . Ni3 Ni 0.785834(18) 1.027563(13) 0.554211(13) 0.04247(9) Uani 1 1 d . . . Ni4 Ni 0.757275(18) 0.944486(13) 0.452804(13) 0.04058(9) Uani 1 1 d . . . O1 O 0.79765(10) 1.09013(7) 0.50475(7) 0.0532(5) Uani 1 1 d . . . O2 O 0.78254(9) 0.96153(7) 0.60643(6) 0.0402(4) Uani 1 1 d . . . O3 O 0.93502(10) 0.94832(8) 0.62920(7) 0.0459(4) Uani 1 1 d D . . H31 H 0.9734(15) 0.9316(13) 0.6377(13) 0.069 Uiso 1 1 d D . . O4 O 0.62881(10) 0.97485(8) 0.59537(7) 0.0491(4) Uani 1 1 d . . . O5 O 0.75575(9) 0.88538(6) 0.52112(6) 0.0383(4) Uani 1 1 d . . . O6 O 0.84382(10) 0.85096(7) 0.63564(7) 0.0462(4) Uani 1 1 d D . . H61 H 0.8748(15) 0.8481(13) 0.6667(12) 0.069 Uiso 1 1 d D . . O7 O 0.67669(9) 0.91050(7) 0.39633(7) 0.0468(4) Uani 1 1 d . . . O8 O 0.84330(9) 0.97050(7) 0.51472(6) 0.0412(4) Uani 1 1 d . . . O9 O 0.90720(11) 0.86272(8) 0.53391(7) 0.0487(5) Uani 1 1 d D . . H91 H 0.9207(18) 0.8350(12) 0.5483(14) 0.073 Uiso 1 1 d D . . O10 O 0.70194(9) 0.99031(7) 0.49846(7) 0.0428(4) Uani 1 1 d . . . O11 O 0.60191(10) 0.90090(8) 0.48355(8) 0.0497(5) Uani 1 1 d D . . H111 H 0.6201(17) 0.9039(14) 0.4549(12) 0.075 Uiso 1 1 d D . . O12 O 0.76132(13) 1.01897(8) 0.40524(8) 0.0634(6) Uani 1 1 d D . . H121 H 0.775(2) 1.0466(13) 0.4272(14) 0.095 Uiso 1 1 d D . . O13 O 0.70699(11) 1.06607(8) 0.59104(9) 0.0582(5) Uani 1 1 d D . . H131 H 0.6766(18) 1.0426(14) 0.5958(15) 0.087 Uiso 1 1 d D . . C1 C 0.83559(16) 1.13393(11) 0.52317(11) 0.0492(7) Uani 1 1 d . . . C2 C 0.88243(15) 1.14072(11) 0.57936(11) 0.0472(6) Uani 1 1 d . . . C3 C 0.92403(15) 1.19088(11) 0.59207(12) 0.0527(7) Uani 1 1 d . . . C4 C 0.97477(16) 1.20062(13) 0.64583(14) 0.0642(8) Uani 1 1 d . . . H4A H 0.9823 1.1735 0.6759 0.077 Uiso 1 1 calc R . . C5 C 1.01332(18) 1.24843(15) 0.65535(18) 0.0772(10) Uani 1 1 d . . . H5A H 1.0470 1.2537 0.6918 0.093 Uiso 1 1 calc R . . C6 C 1.00410(19) 1.28907(15) 0.61287(19) 0.0778(10) Uani 1 1 d . . . H6A H 1.0312 1.3219 0.6200 0.093 Uiso 1 1 calc R . . C7 C 0.9559(2) 1.28152(14) 0.56088(17) 0.0760(10) Uani 1 1 d . . . H7A H 0.9493 1.3095 0.5317 0.091 Uiso 1 1 calc R . . C8 C 0.91545(17) 1.23301(12) 0.54936(13) 0.0608(8) Uani 1 1 d . . . C9 C 0.8658(2) 1.22535(13) 0.49466(14) 0.0735(10) Uani 1 1 d . . . H9A H 0.8586 1.2540 0.4662 0.088 Uiso 1 1 calc R . . C10 C 0.82858(19) 1.17840(12) 0.48217(13) 0.0655(9) Uani 1 1 d . . . H10A H 0.7964 1.1747 0.4447 0.079 Uiso 1 1 calc R . . C11 C 0.89030(14) 1.10009(11) 0.62584(11) 0.0471(6) Uani 1 1 d . . . H11A H 0.9216 1.1092 0.6625 0.057 Uiso 1 1 calc R . . C12 C 0.86997(14) 1.01621(11) 0.67468(10) 0.0448(6) Uani 1 1 d . . . C13 C 0.80421(14) 0.97888(11) 0.66563(10) 0.0435(6) Uani 1 1 d . . . H13A H 0.8154 0.9464 0.6917 0.052 Uiso 1 1 calc R . . H13B H 0.7653 0.9993 0.6764 0.052 Uiso 1 1 calc R . . C14 C 0.93695(14) 0.98200(11) 0.67971(10) 0.0456(6) Uani 1 1 d . . . H14A H 0.9780 1.0071 0.6855 0.055 Uiso 1 1 calc R . . H14B H 0.9439 0.9582 0.7150 0.055 Uiso 1 1 calc R . . C15 C 0.87753(16) 1.04669(12) 0.73325(11) 0.0539(7) Uani 1 1 d . . . H15A H 0.9191 1.0707 0.7403 0.081 Uiso 1 1 calc R . . H15B H 0.8831 1.0199 0.7654 0.081 Uiso 1 1 calc R . . H15C H 0.8352 1.0689 0.7315 0.081 Uiso 1 1 calc R . . C16 C 0.62062(14) 0.96294(11) 0.64828(11) 0.0483(7) Uani 1 1 d . . . C17 C 0.63575(14) 0.91160(11) 0.67672(11) 0.0452(6) Uani 1 1 d . . . C18 C 0.62026(15) 0.90417(12) 0.73430(11) 0.0518(7) Uani 1 1 d . . . C19 C 0.63028(18) 0.85402(13) 0.76549(12) 0.0602(8) Uani 1 1 d . . . H19A H 0.6479 0.8231 0.7487 0.072 Uiso 1 1 calc R . . C20 C 0.6151(2) 0.84883(14) 0.81977(13) 0.0713(9) Uani 1 1 d . . . H20A H 0.6226 0.8146 0.8399 0.086 Uiso 1 1 calc R . . C21 C 0.5890(2) 0.89328(15) 0.84552(13) 0.0727(10) Uani 1 1 d . . . H21A H 0.5783 0.8893 0.8828 0.087 Uiso 1 1 calc R . . C22 C 0.57890(19) 0.94207(15) 0.81709(13) 0.0688(9) Uani 1 1 d . . . H22A H 0.5610 0.9723 0.8347 0.083 Uiso 1 1 calc R . . C23 C 0.59461(17) 0.94888(13) 0.76155(12) 0.0590(8) Uani 1 1 d . . . C24 C 0.58480(18) 1.00052(13) 0.73290(13) 0.0664(9) Uani 1 1 d . . . H24A H 0.5698 1.0311 0.7520 0.080 Uiso 1 1 calc R . . C25 C 0.59656(17) 1.00677(13) 0.67848(13) 0.0610(8) Uani 1 1 d . . . H25A H 0.5884 1.0417 0.6599 0.073 Uiso 1 1 calc R . . C26 C 0.66848(14) 0.86639(11) 0.65351(10) 0.0449(6) Uani 1 1 d . . . H26A H 0.6769 0.8339 0.6768 0.054 Uiso 1 1 calc R . . C27 C 0.72533(14) 0.81698(10) 0.58815(10) 0.0420(6) Uani 1 1 d . . . C28 C 0.73795(14) 0.82944(10) 0.52622(10) 0.0413(6) Uani 1 1 d . . . H28A H 0.7766 0.8058 0.5196 0.050 Uiso 1 1 calc R . . H28B H 0.6946 0.8206 0.4955 0.050 Uiso 1 1 calc R . . C29 C 0.79541(14) 0.80672(11) 0.63285(10) 0.0449(6) Uani 1 1 d . . . H29A H 0.7864 0.8012 0.6723 0.054 Uiso 1 1 calc R . . H29B H 0.8169 0.7726 0.6221 0.054 Uiso 1 1 calc R . . C30 C 0.68035(15) 0.76491(11) 0.58427(11) 0.0496(7) Uani 1 1 d . . . H30A H 0.6733 0.7561 0.6233 0.074 Uiso 1 1 calc R . . H30B H 0.7045 0.7342 0.5703 0.074 Uiso 1 1 calc R . . H30C H 0.6344 0.7710 0.5567 0.074 Uiso 1 1 calc R . . C31 C 0.68120(14) 0.87815(10) 0.35275(10) 0.0433(6) Uani 1 1 d . . . C32 C 0.74463(14) 0.86312(10) 0.33735(10) 0.0415(6) Uani 1 1 d . . . C33 C 0.74089(15) 0.82868(10) 0.28592(10) 0.0455(6) Uani 1 1 d . . . C34 C 0.79995(16) 0.81469(11) 0.26367(11) 0.0503(7) Uani 1 1 d . . . H34A H 0.8451 0.8289 0.2829 0.060 Uiso 1 1 calc R . . C35 C 0.79434(18) 0.78132(12) 0.21537(11) 0.0585(8) Uani 1 1 d . . . H35A H 0.8349 0.7736 0.2012 0.070 Uiso 1 1 calc R . . C36 C 0.72857(18) 0.75865(13) 0.18694(12) 0.0628(8) Uani 1 1 d . . . H36A H 0.7249 0.7346 0.1543 0.075 Uiso 1 1 calc R . . C37 C 0.67077(18) 0.77130(12) 0.20626(12) 0.0601(8) Uani 1 1 d . . . H37A H 0.6265 0.7559 0.1868 0.072 Uiso 1 1 calc R . . C38 C 0.67443(16) 0.80687(11) 0.25478(11) 0.0506(7) Uani 1 1 d . . . C39 C 0.61295(16) 0.82160(12) 0.27286(11) 0.0546(7) Uani 1 1 d . . . H39A H 0.5686 0.8070 0.2523 0.065 Uiso 1 1 calc R . . C40 C 0.61570(15) 0.85606(12) 0.31870(11) 0.0515(7) Uani 1 1 d . . . H40A H 0.5730 0.8660 0.3287 0.062 Uiso 1 1 calc R . . C41 C 0.81398(14) 0.87836(10) 0.37170(10) 0.0428(6) Uani 1 1 d . . . H41A H 0.8532 0.8640 0.3592 0.051 Uiso 1 1 calc R . . C42 C 0.90286(13) 0.92181(10) 0.44834(10) 0.0417(6) Uani 1 1 d . . . C43 C 0.93718(14) 0.87293(11) 0.48495(10) 0.0446(6) Uani 1 1 d . . . H43A H 0.9314 0.8398 0.4596 0.053 Uiso 1 1 calc R . . H43B H 0.9884 0.8800 0.4996 0.053 Uiso 1 1 calc R . . C44 C 0.90040(14) 0.97292(11) 0.48783(10) 0.0448(6) Uani 1 1 d . . . H44A H 0.9452 0.9752 0.5187 0.054 Uiso 1 1 calc R . . H44B H 0.8962 1.0066 0.4635 0.054 Uiso 1 1 calc R . . C45 C 0.94793(14) 0.93630(12) 0.40522(10) 0.0489(6) Uani 1 1 d . . . H45A H 0.9475 0.9055 0.3782 0.073 Uiso 1 1 calc R . . H45B H 0.9966 0.9436 0.4273 0.073 Uiso 1 1 calc R . . H45C H 0.9285 0.9691 0.3827 0.073 Uiso 1 1 calc R . . C46 C 0.64374(16) 1.02339(12) 0.46823(12) 0.0561(7) Uani 1 1 d . . . H46A H 0.6234 1.0426 0.4971 0.084 Uiso 1 1 calc R . . H46B H 0.6077 0.9998 0.4434 0.084 Uiso 1 1 calc R . . H46C H 0.6602 1.0504 0.4435 0.084 Uiso 1 1 calc R . . C47 C 0.52994(16) 0.91752(14) 0.47503(14) 0.0667(8) Uani 1 1 d . . . H47A H 0.5010 0.8991 0.4402 0.100 Uiso 1 1 calc R . . H47B H 0.5264 0.9574 0.4693 0.100 Uiso 1 1 calc R . . H47C H 0.5130 0.9075 0.5097 0.100 Uiso 1 1 calc R . . C48 C 0.76272(18) 1.02752(14) 0.34617(11) 0.0634(8) Uani 1 1 d . . . H48A H 0.7630 1.0671 0.3383 0.095 Uiso 1 1 calc R . . H48B H 0.7208 1.0108 0.3203 0.095 Uiso 1 1 calc R . . H48C H 0.8054 1.0107 0.3388 0.095 Uiso 1 1 calc R . . C49 C 0.6882(2) 1.11914(16) 0.5976(3) 0.1229(18) Uani 1 1 d . . . H49A H 0.6496 1.1199 0.6178 0.184 Uiso 1 1 calc R . . H49B H 0.6724 1.1364 0.5588 0.184 Uiso 1 1 calc R . . H49C H 0.7289 1.1393 0.6211 0.184 Uiso 1 1 calc R . . N1 N 0.85954(12) 1.05320(9) 0.62278(8) 0.0443(5) Uani 1 1 d . . . N2 N 0.68747(11) 0.86553(8) 0.60446(8) 0.0409(5) Uani 1 1 d . . . N3 N 0.82801(11) 0.90950(8) 0.41752(8) 0.0409(5) Uani 1 1 d . . . S1 S 1.0000 0.81535(4) 0.7500 0.0491(2) Uani 1 2 d S . . O14 O 1.06578(11) 0.90805(9) 0.66295(8) 0.0577(5) Uani 1 1 d D . . H141 H 1.0660(19) 0.8894(14) 0.6953(13) 0.086 Uiso 1 1 d D . . O15 O 0.9460(2) 0.77050(11) 0.58660(9) 0.1120(12) Uani 1 1 d D . . H151 H 0.967(3) 0.772(2) 0.6237(15) 0.168 Uiso 1 1 d D . . O16 O 0.93637(10) 0.85114(8) 0.73816(7) 0.0572(5) Uani 1 1 d . . . O17 O 1.00182(12) 0.78146(9) 0.80141(8) 0.0672(6) Uani 1 1 d . . . C50 C 1.09657(19) 0.87442(14) 0.62619(14) 0.0693(9) Uani 1 1 d . . . H50A H 1.1026 0.8959 0.5923 0.104 Uiso 1 1 calc R . . H50B H 1.0656 0.8430 0.6122 0.104 Uiso 1 1 calc R . . H50C H 1.1427 0.8612 0.6487 0.104 Uiso 1 1 calc R . . C51 C 0.9720(2) 0.72424(15) 0.57262(14) 0.0834(11) Uani 1 1 d . . . H51A H 1.0223 0.7220 0.5925 0.125 Uiso 1 1 calc R . . H51B H 0.9663 0.7227 0.5299 0.125 Uiso 1 1 calc R . . H51C H 0.9468 0.6933 0.5850 0.125 Uiso 1 1 calc R . . 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 0.04022(19) 0.03748(18) 0.04148(16) 0.00055(13) 0.00689(13) 0.00005(15) Ni2 0.03968(18) 0.03776(17) 0.03482(15) -0.00006(12) 0.00459(13) -0.00055(14) Ni3 0.0475(2) 0.03579(17) 0.04075(16) -0.00007(13) 0.00422(14) -0.00196(16) Ni4 0.04353(19) 0.03942(18) 0.03595(15) 0.00068(13) 0.00424(13) -0.00277(15) O1 0.0651(13) 0.0411(10) 0.0476(9) 0.0017(8) 0.0026(9) -0.0066(9) O2 0.0445(10) 0.0389(9) 0.0348(8) -0.0029(7) 0.0050(7) -0.0016(8) O3 0.0445(11) 0.0490(11) 0.0407(9) -0.0057(8) 0.0036(8) 0.0005(9) O4 0.0502(11) 0.0475(11) 0.0489(10) 0.0012(8) 0.0109(8) 0.0038(9) O5 0.0423(10) 0.0339(9) 0.0376(8) -0.0006(7) 0.0076(7) -0.0034(8) O6 0.0481(11) 0.0476(10) 0.0378(9) 0.0049(8) 0.0004(8) -0.0034(9) O7 0.0455(11) 0.0497(11) 0.0415(9) -0.0019(8) 0.0035(8) -0.0024(9) O8 0.0454(10) 0.0399(9) 0.0374(8) -0.0015(7) 0.0080(7) -0.0050(8) O9 0.0564(12) 0.0460(11) 0.0455(10) 0.0059(8) 0.0155(9) 0.0076(9) O10 0.0438(10) 0.0392(10) 0.0406(8) 0.0023(7) 0.0008(7) 0.0023(8) O11 0.0420(11) 0.0527(11) 0.0516(10) -0.0023(9) 0.0058(8) -0.0003(9) O12 0.0963(17) 0.0472(12) 0.0425(10) 0.0049(8) 0.0090(10) -0.0059(12) O13 0.0625(14) 0.0411(11) 0.0735(12) -0.0063(10) 0.0212(10) 0.0013(10) C1 0.0602(19) 0.0381(15) 0.0511(15) 0.0000(12) 0.0168(13) -0.0026(13) C2 0.0491(17) 0.0394(14) 0.0532(14) -0.0044(12) 0.0128(12) -0.0052(13) C3 0.0509(18) 0.0438(16) 0.0675(17) -0.0092(13) 0.0227(14) -0.0050(14) C4 0.0531(19) 0.0507(18) 0.085(2) -0.0150(15) 0.0096(16) -0.0103(15) C5 0.056(2) 0.059(2) 0.111(3) -0.021(2) 0.0095(19) -0.0081(17) C6 0.060(2) 0.055(2) 0.125(3) -0.020(2) 0.036(2) -0.0181(17) C7 0.087(3) 0.056(2) 0.096(2) -0.0052(18) 0.044(2) -0.0188(19) C8 0.071(2) 0.0442(17) 0.0739(19) -0.0069(14) 0.0293(16) -0.0130(15) C9 0.107(3) 0.0463(18) 0.070(2) 0.0056(15) 0.0268(19) -0.0112(19) C10 0.090(3) 0.0502(18) 0.0558(16) 0.0047(14) 0.0180(16) -0.0084(17) C11 0.0454(16) 0.0475(16) 0.0459(14) -0.0045(11) 0.0062(12) 0.0002(13) C12 0.0516(16) 0.0436(15) 0.0350(12) -0.0014(11) 0.0029(11) -0.0007(13) C13 0.0453(15) 0.0444(15) 0.0385(12) -0.0001(11) 0.0061(11) 0.0005(12) C14 0.0489(16) 0.0482(16) 0.0359(12) -0.0030(11) 0.0031(11) -0.0002(13) C15 0.0590(19) 0.0572(18) 0.0423(14) -0.0091(12) 0.0060(12) -0.0033(14) C16 0.0428(16) 0.0512(17) 0.0492(15) -0.0096(12) 0.0081(12) -0.0014(13) C17 0.0430(15) 0.0456(15) 0.0468(13) -0.0079(12) 0.0105(11) -0.0065(13) C18 0.0527(18) 0.0539(17) 0.0475(14) -0.0106(13) 0.0094(12) -0.0105(14) C19 0.081(2) 0.0530(18) 0.0513(15) -0.0088(13) 0.0254(15) -0.0118(16) C20 0.101(3) 0.062(2) 0.0556(17) -0.0090(15) 0.0293(17) -0.0171(19) C21 0.093(3) 0.080(2) 0.0503(16) -0.0154(17) 0.0272(17) -0.013(2) C22 0.083(2) 0.075(2) 0.0497(16) -0.0164(16) 0.0180(15) 0.0031(19) C23 0.063(2) 0.064(2) 0.0495(15) -0.0136(14) 0.0124(14) 0.0007(16) C24 0.081(2) 0.061(2) 0.0585(18) -0.0156(15) 0.0194(16) 0.0092(18) C25 0.070(2) 0.0531(18) 0.0597(17) -0.0060(14) 0.0150(15) 0.0093(16) C26 0.0472(16) 0.0428(15) 0.0424(13) -0.0012(11) 0.0063(11) -0.0067(12) C27 0.0467(15) 0.0374(14) 0.0419(12) -0.0003(10) 0.0105(11) -0.0007(12) C28 0.0461(15) 0.0370(14) 0.0396(12) -0.0009(10) 0.0080(11) -0.0033(12) C29 0.0526(17) 0.0390(14) 0.0428(13) 0.0060(11) 0.0113(12) 0.0006(13) C30 0.0602(18) 0.0393(15) 0.0520(14) 0.0007(12) 0.0191(13) -0.0053(13) C31 0.0501(17) 0.0396(14) 0.0360(12) 0.0029(11) 0.0026(11) -0.0055(12) C32 0.0451(16) 0.0382(14) 0.0376(12) 0.0032(10) 0.0033(11) -0.0057(12) C33 0.0574(18) 0.0381(14) 0.0379(12) 0.0030(10) 0.0054(12) -0.0056(13) C34 0.0573(18) 0.0465(16) 0.0440(13) -0.0010(12) 0.0062(13) -0.0074(14) C35 0.072(2) 0.0536(18) 0.0487(15) -0.0072(13) 0.0123(14) -0.0016(16) C36 0.082(2) 0.0539(18) 0.0477(15) -0.0119(13) 0.0066(15) -0.0054(17) C37 0.071(2) 0.0533(18) 0.0490(15) -0.0080(13) 0.0002(15) -0.0099(16) C38 0.0566(18) 0.0460(16) 0.0429(13) 0.0007(12) 0.0000(12) -0.0075(14) C39 0.0540(19) 0.0537(17) 0.0498(15) -0.0034(13) 0.0007(13) -0.0115(14) C40 0.0449(17) 0.0558(17) 0.0502(14) -0.0006(13) 0.0044(12) -0.0057(14) C41 0.0480(16) 0.0392(14) 0.0404(13) 0.0001(11) 0.0091(11) -0.0067(12) C42 0.0410(15) 0.0448(15) 0.0371(12) -0.0030(10) 0.0053(10) -0.0076(12) C43 0.0444(16) 0.0487(15) 0.0405(13) -0.0019(11) 0.0101(11) -0.0006(13) C44 0.0471(16) 0.0454(15) 0.0406(12) -0.0014(11) 0.0082(11) -0.0071(13) C45 0.0470(16) 0.0561(17) 0.0436(13) -0.0044(12) 0.0109(12) -0.0094(14) C46 0.0576(18) 0.0458(16) 0.0567(15) 0.0050(13) -0.0018(13) 0.0089(14) C47 0.0462(18) 0.067(2) 0.081(2) -0.0085(16) 0.0047(15) 0.0013(16) C48 0.072(2) 0.069(2) 0.0489(15) 0.0093(14) 0.0145(14) -0.0052(17) C49 0.093(3) 0.049(2) 0.243(6) -0.025(3) 0.073(4) 0.000(2) N1 0.0507(14) 0.0399(12) 0.0411(11) 0.0001(9) 0.0093(9) 0.0011(11) N2 0.0417(13) 0.0392(12) 0.0405(11) -0.0035(9) 0.0076(9) -0.0042(10) N3 0.0451(13) 0.0394(11) 0.0364(10) 0.0020(9) 0.0064(9) -0.0071(10) S1 0.0517(6) 0.0478(5) 0.0420(5) 0.000 0.0002(4) 0.000 O14 0.0532(12) 0.0636(13) 0.0550(11) 0.0045(10) 0.0107(9) 0.0038(10) O15 0.211(3) 0.0708(16) 0.0494(12) 0.0046(12) 0.0215(16) 0.067(2) O16 0.0534(12) 0.0657(13) 0.0466(10) -0.0001(9) 0.0006(9) 0.0127(10) O17 0.0754(15) 0.0638(13) 0.0515(11) 0.0163(10) -0.0054(10) -0.0106(11) C50 0.073(2) 0.070(2) 0.0687(19) 0.0007(16) 0.0245(17) 0.0059(18) C51 0.119(3) 0.063(2) 0.0635(19) -0.0104(17) 0.0124(19) 0.006(2) _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 1.965(2) . ? Ni1 O4 1.9706(18) . ? Ni1 O10 2.0254(17) . ? Ni1 O5 2.0340(17) . ? Ni1 O2 2.1029(16) . ? Ni1 O11 2.1632(18) . ? Ni2 O8 2.0049(16) . ? Ni2 O2 2.0114(17) . ? Ni2 O5 2.0126(16) . ? Ni2 O6 2.0510(17) . ? Ni2 O9 2.0660(19) . ? Ni2 O3 2.0771(18) . ? Ni3 O1 1.9587(18) . ? Ni3 N1 1.976(2) . ? Ni3 O2 2.0281(16) . ? Ni3 O10 2.0395(17) . ? Ni3 O8 2.1309(17) . ? Ni3 O13 2.152(2) . ? Ni4 N3 1.966(2) . ? Ni4 O7 1.9715(17) . ? Ni4 O10 2.0274(17) . ? Ni4 O8 2.0320(16) . ? Ni4 O12 2.1371(19) . ? Ni4 O5 2.1549(15) . ? O1 C1 1.309(3) . ? O2 C13 1.410(3) . ? O3 C14 1.431(3) . ? O3 H31 0.83(3) . ? O4 C16 1.318(3) . ? O5 C28 1.416(3) . ? O6 C29 1.423(3) . ? O6 H61 0.83(2) . ? O7 C31 1.308(3) . ? O8 C44 1.408(3) . ? O9 C43 1.429(3) . ? O9 H91 0.77(3) . ? O10 C46 1.430(3) . ? O11 C47 1.428(4) . ? O11 H111 0.84(3) . ? O12 C48 1.404(3) . ? O12 H121 0.85(3) . ? O13 C49 1.361(4) . ? O13 H131 0.85(3) . ? C1 C2 1.416(4) . ? C1 C10 1.430(4) . ? C2 C11 1.449(4) . ? C2 C3 1.455(4) . ? C3 C8 1.412(4) . ? C3 C4 1.418(4) . ? C4 C5 1.373(4) . ? C4 H4A 0.9500 . ? C5 C6 1.382(5) . ? C5 H5A 0.9500 . ? C6 C7 1.356(5) . ? C6 H6A 0.9500 . ? C7 C8 1.409(4) . ? C7 H7A 0.9500 . ? C8 C9 1.416(4) . ? C9 C10 1.347(4) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 N1 1.282(3) . ? C11 H11A 0.9500 . ? C12 N1 1.484(3) . ? C12 C14 1.529(4) . ? C12 C15 1.533(3) . ? C12 C13 1.544(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.412(4) . ? C16 C25 1.420(4) . ? C17 C26 1.442(4) . ? C17 C18 1.462(4) . ? C18 C19 1.410(4) . ? C18 C23 1.412(4) . ? C19 C20 1.378(4) . ? C19 H19A 0.9500 . ? C20 C21 1.393(5) . ? C20 H20A 0.9500 . ? C21 C22 1.351(5) . ? C21 H21A 0.9500 . ? C22 C23 1.415(4) . ? C22 H22A 0.9500 . ? C23 C24 1.414(4) . ? C24 C25 1.356(4) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C26 N2 1.289(3) . ? C26 H26A 0.9500 . ? C27 N2 1.491(3) . ? C27 C29 1.526(4) . ? C27 C30 1.531(4) . ? C27 C28 1.557(3) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.418(4) . ? C31 C40 1.435(4) . ? C32 C41 1.443(3) . ? C32 C33 1.453(3) . ? C33 C34 1.417(4) . ? C33 C38 1.426(4) . ? C34 C35 1.373(4) . ? C34 H34A 0.9500 . ? C35 C36 1.406(4) . ? C35 H35A 0.9500 . ? C36 C37 1.349(4) . ? C36 H36A 0.9500 . ? C37 C38 1.415(4) . ? C37 H37A 0.9500 . ? C38 C39 1.412(4) . ? C39 C40 1.351(4) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? C41 N3 1.286(3) . ? C41 H41A 0.9500 . ? C42 N3 1.493(3) . ? C42 C43 1.521(3) . ? C42 C45 1.532(4) . ? C42 C44 1.556(3) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? S1 O17 1.4513(19) 2_756 ? S1 O17 1.4513(19) . ? S1 O16 1.486(2) 2_756 ? S1 O16 1.486(2) . ? O14 C50 1.422(4) . ? O14 H141 0.88(3) . ? O15 C51 1.308(4) . ? O15 H151 0.87(3) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? 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 O4 94.14(8) . . ? N2 Ni1 O10 168.91(8) . . ? O4 Ni1 O10 96.53(7) . . ? N2 Ni1 O5 83.36(8) . . ? O4 Ni1 O5 173.34(7) . . ? O10 Ni1 O5 85.71(7) . . ? N2 Ni1 O2 93.93(7) . . ? O4 Ni1 O2 93.35(7) . . ? O10 Ni1 O2 82.44(6) . . ? O5 Ni1 O2 80.69(6) . . ? N2 Ni1 O11 94.60(8) . . ? O4 Ni1 O11 97.54(8) . . ? O10 Ni1 O11 87.01(7) . . ? O5 Ni1 O11 88.84(7) . . ? O2 Ni1 O11 165.63(7) . . ? O8 Ni2 O2 84.52(7) . . ? O8 Ni2 O5 84.87(6) . . ? O2 Ni2 O5 83.47(6) . . ? O8 Ni2 O6 176.57(7) . . ? O2 Ni2 O6 93.29(7) . . ? O5 Ni2 O6 92.27(7) . . ? O8 Ni2 O9 90.44(7) . . ? O2 Ni2 O9 173.84(6) . . ? O5 Ni2 O9 92.57(7) . . ? O6 Ni2 O9 91.58(7) . . ? O8 Ni2 O3 89.95(7) . . ? O2 Ni2 O3 90.72(7) . . ? O5 Ni2 O3 172.55(7) . . ? O6 Ni2 O3 92.72(7) . . ? O9 Ni2 O3 92.82(8) . . ? O1 Ni3 N1 93.86(8) . . ? O1 Ni3 O2 175.11(8) . . ? N1 Ni3 O2 83.37(8) . . ? O1 Ni3 O10 99.15(7) . . ? N1 Ni3 O10 166.15(8) . . ? O2 Ni3 O10 83.98(6) . . ? O1 Ni3 O8 95.71(7) . . ? N1 Ni3 O8 101.63(8) . . ? O2 Ni3 O8 80.95(6) . . ? O10 Ni3 O8 81.88(7) . . ? O1 Ni3 O13 95.58(8) . . ? N1 Ni3 O13 89.29(9) . . ? O2 Ni3 O13 88.43(7) . . ? O10 Ni3 O13 84.76(8) . . ? O8 Ni3 O13 163.70(7) . . ? N3 Ni4 O7 93.67(8) . . ? N3 Ni4 O10 167.83(8) . . ? O7 Ni4 O10 98.23(7) . . ? N3 Ni4 O8 83.78(7) . . ? O7 Ni4 O8 173.29(7) . . ? O10 Ni4 O8 84.65(7) . . ? N3 Ni4 O12 91.68(9) . . ? O7 Ni4 O12 97.53(8) . . ? O10 Ni4 O12 84.29(8) . . ? O8 Ni4 O12 88.76(7) . . ? N3 Ni4 O5 99.25(7) . . ? O7 Ni4 O5 93.69(7) . . ? O10 Ni4 O5 82.56(6) . . ? O8 Ni4 O5 80.64(6) . . ? O12 Ni4 O5 163.80(7) . . ? C1 O1 Ni3 125.18(16) . . ? C13 O2 Ni2 118.39(15) . . ? C13 O2 Ni3 107.97(14) . . ? Ni2 O2 Ni3 98.43(7) . . ? C13 O2 Ni1 133.29(15) . . ? Ni2 O2 Ni1 96.69(6) . . ? Ni3 O2 Ni1 95.13(6) . . ? C14 O3 Ni2 127.04(16) . . ? C14 O3 H31 104(2) . . ? Ni2 O3 H31 120(2) . . ? C16 O4 Ni1 123.45(17) . . ? C28 O5 Ni2 116.46(14) . . ? C28 O5 Ni1 106.74(14) . . ? Ni2 O5 Ni1 98.89(6) . . ? C28 O5 Ni4 138.70(13) . . ? Ni2 O5 Ni4 94.94(7) . . ? Ni1 O5 Ni4 93.10(6) . . ? C29 O6 Ni2 129.77(14) . . ? C29 O6 H61 108(2) . . ? Ni2 O6 H61 122(2) . . ? C31 O7 Ni4 125.47(17) . . ? C44 O8 Ni2 116.75(15) . . ? C44 O8 Ni4 107.49(13) . . ? Ni2 O8 Ni4 99.13(7) . . ? C44 O8 Ni3 136.37(15) . . ? Ni2 O8 Ni3 95.34(7) . . ? Ni4 O8 Ni3 94.66(7) . . ? C43 O9 Ni2 131.73(16) . . ? C43 O9 H91 110(3) . . ? Ni2 O9 H91 118(3) . . ? C46 O10 Ni1 120.01(17) . . ? C46 O10 Ni4 120.62(15) . . ? Ni1 O10 Ni4 97.29(7) . . ? C46 O10 Ni3 118.89(15) . . ? Ni1 O10 Ni3 97.21(6) . . ? Ni4 O10 Ni3 97.67(8) . . ? C47 O11 Ni1 123.78(17) . . ? C47 O11 H111 117(2) . . ? Ni1 O11 H111 101(2) . . ? C48 O12 Ni4 130.54(19) . . ? C48 O12 H121 113(3) . . ? Ni4 O12 H121 114(3) . . ? C49 O13 Ni3 134.2(2) . . ? C49 O13 H131 114(3) . . ? Ni3 O13 H131 110(3) . . ? O1 C1 C2 125.9(2) . . ? O1 C1 C10 116.2(2) . . ? C2 C1 C10 118.0(3) . . ? C1 C2 C11 122.9(2) . . ? C1 C2 C3 119.3(2) . . ? C11 C2 C3 117.8(2) . . ? C8 C3 C4 116.3(3) . . ? C8 C3 C2 120.0(3) . . ? C4 C3 C2 123.7(3) . . ? C5 C4 C3 121.4(3) . . ? C5 C4 H4A 119.3 . . ? C3 C4 H4A 119.3 . . ? C4 C5 C6 121.3(3) . . ? C4 C5 H5A 119.4 . . ? C6 C5 H5A 119.4 . . ? C7 C6 C5 119.2(3) . . ? C7 C6 H6A 120.4 . . ? C5 C6 H6A 120.4 . . ? C6 C7 C8 121.2(3) . . ? C6 C7 H7A 119.4 . . ? C8 C7 H7A 119.4 . . ? C7 C8 C3 120.5(3) . . ? C7 C8 C9 120.7(3) . . ? C3 C8 C9 118.7(3) . . ? C10 C9 C8 121.4(3) . . ? C10 C9 H9A 119.3 . . ? C8 C9 H9A 119.3 . . ? C9 C10 C1 122.5(3) . . ? C9 C10 H10A 118.7 . . ? C1 C10 H10A 118.7 . . ? N1 C11 C2 127.0(2) . . ? N1 C11 H11A 116.5 . . ? C2 C11 H11A 116.5 . . ? N1 C12 C14 109.7(2) . . ? N1 C12 C15 113.7(2) . . ? C14 C12 C15 107.5(2) . . ? N1 C12 C13 107.49(19) . . ? C14 C12 C13 110.9(2) . . ? C15 C12 C13 107.6(2) . . ? O2 C13 C12 110.5(2) . . ? O2 C13 H13A 109.5 . . ? C12 C13 H13A 109.5 . . ? O2 C13 H13B 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? O3 C14 C12 113.45(19) . . ? O3 C14 H14A 108.9 . . ? C12 C14 H14A 108.9 . . ? O3 C14 H14B 108.9 . . ? C12 C14 H14B 108.9 . . ? H14A C14 H14B 107.7 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O4 C16 C17 125.3(2) . . ? O4 C16 C25 115.6(3) . . ? C17 C16 C25 119.1(2) . . ? C16 C17 C26 123.9(2) . . ? C16 C17 C18 118.5(2) . . ? C26 C17 C18 117.6(2) . . ? C19 C18 C23 116.9(3) . . ? C19 C18 C17 123.4(3) . . ? C23 C18 C17 119.8(3) . . ? C20 C19 C18 121.5(3) . . ? C20 C19 H19A 119.3 . . ? C18 C19 H19A 119.3 . . ? C19 C20 C21 120.7(3) . . ? C19 C20 H20A 119.6 . . ? C21 C20 H20A 119.6 . . ? C22 C21 C20 119.6(3) . . ? C22 C21 H21A 120.2 . . ? C20 C21 H21A 120.2 . . ? C21 C22 C23 121.1(3) . . ? C21 C22 H22A 119.5 . . ? C23 C22 H22A 119.5 . . ? C18 C23 C24 119.5(3) . . ? C18 C23 C22 120.3(3) . . ? C24 C23 C22 120.3(3) . . ? C25 C24 C23 120.7(3) . . ? C25 C24 H24A 119.7 . . ? C23 C24 H24A 119.7 . . ? C24 C25 C16 122.3(3) . . ? C24 C25 H25A 118.8 . . ? C16 C25 H25A 118.8 . . ? N2 C26 C17 126.7(2) . . ? N2 C26 H26A 116.7 . . ? C17 C26 H26A 116.7 . . ? N2 C27 C29 111.79(19) . . ? N2 C27 C30 111.0(2) . . ? C29 C27 C30 108.1(2) . . ? N2 C27 C28 106.54(19) . . ? C29 C27 C28 110.5(2) . . ? C30 C27 C28 108.92(19) . . ? O5 C28 C27 111.28(19) . . ? O5 C28 H28A 109.4 . . ? C27 C28 H28A 109.4 . . ? O5 C28 H28B 109.4 . . ? C27 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? O6 C29 C27 112.4(2) . . ? O6 C29 H29A 109.1 . . ? C27 C29 H29A 109.1 . . ? O6 C29 H29B 109.1 . . ? C27 C29 H29B 109.1 . . ? H29A C29 H29B 107.8 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O7 C31 C32 125.6(2) . . ? O7 C31 C40 116.0(2) . . ? C32 C31 C40 118.5(2) . . ? C31 C32 C41 123.4(2) . . ? C31 C32 C33 119.2(2) . . ? C41 C32 C33 117.4(2) . . ? C34 C33 C38 116.3(2) . . ? C34 C33 C32 124.2(2) . . ? C38 C33 C32 119.5(3) . . ? C35 C34 C33 122.4(3) . . ? C35 C34 H34A 118.8 . . ? C33 C34 H34A 118.8 . . ? C34 C35 C36 120.1(3) . . ? C34 C35 H35A 120.0 . . ? C36 C35 H35A 120.0 . . ? C37 C36 C35 119.6(3) . . ? C37 C36 H36A 120.2 . . ? C35 C36 H36A 120.2 . . ? C36 C37 C38 121.7(3) . . ? C36 C37 H37A 119.2 . . ? C38 C37 H37A 119.2 . . ? C39 C38 C37 121.0(3) . . ? C39 C38 C33 119.1(2) . . ? C37 C38 C33 119.9(3) . . ? C40 C39 C38 121.5(3) . . ? C40 C39 H39A 119.2 . . ? C38 C39 H39A 119.2 . . ? C39 C40 C31 122.0(3) . . ? C39 C40 H40A 119.0 . . ? C31 C40 H40A 119.0 . . ? N3 C41 C32 126.5(3) . . ? N3 C41 H41A 116.7 . . ? C32 C41 H41A 116.7 . . ? N3 C42 C43 111.1(2) . . ? N3 C42 C45 112.27(18) . . ? C43 C42 C45 107.8(2) . . ? N3 C42 C44 106.2(2) . . ? C43 C42 C44 111.28(19) . . ? C45 C42 C44 108.2(2) . . ? O9 C43 C42 112.1(2) . . ? O9 C43 H43A 109.2 . . ? C42 C43 H43A 109.2 . . ? O9 C43 H43B 109.2 . . ? C42 C43 H43B 109.2 . . ? H43A C43 H43B 107.9 . . ? O8 C44 C42 112.0(2) . . ? O8 C44 H44A 109.2 . . ? C42 C44 H44A 109.2 . . ? O8 C44 H44B 109.2 . . ? C42 C44 H44B 109.2 . . ? H44A C44 H44B 107.9 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O10 C46 H46A 109.5 . . ? O10 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? O10 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O11 C47 H47A 109.5 . . ? O11 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? O11 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? O12 C48 H48A 109.5 . . ? O12 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? O12 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O13 C49 H49A 109.5 . . ? O13 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? O13 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C11 N1 C12 121.6(2) . . ? C11 N1 Ni3 124.33(17) . . ? C12 N1 Ni3 113.59(16) . . ? C26 N2 C27 120.6(2) . . ? C26 N2 Ni1 123.70(18) . . ? C27 N2 Ni1 114.64(15) . . ? C41 N3 C42 120.3(2) . . ? C41 N3 Ni4 125.18(18) . . ? C42 N3 Ni4 114.49(15) . . ? O17 S1 O17 110.79(18) 2_756 . ? O17 S1 O16 109.73(12) 2_756 2_756 ? O17 S1 O16 109.13(10) . 2_756 ? O17 S1 O16 109.13(10) 2_756 . ? O17 S1 O16 109.73(12) . . ? O16 S1 O16 108.29(17) 2_756 . ? C50 O14 H141 108(2) . . ? C51 O15 H151 100(4) . . ? O14 C50 H50A 109.5 . . ? O14 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? O14 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? O15 C51 H51A 109.5 . . ? O15 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? O15 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H31 O14 0.83(3) 1.84(3) 2.666(3) 168(3) . O6 H61 O16 0.83(2) 1.81(3) 2.627(2) 171(3) . O9 H91 O15 0.77(3) 1.81(3) 2.582(3) 174(4) . O11 H111 O7 0.84(3) 1.96(3) 2.792(3) 171(3) . O12 H121 O1 0.85(3) 2.05(3) 2.848(3) 156(3) . O13 H131 O4 0.85(3) 1.89(3) 2.708(3) 161(4) . O14 H141 O16 0.88(3) 1.82(3) 2.705(3) 178(4) 2_756 O15 H151 O17 0.87(3) 1.72(3) 2.582(3) 171(6) 2_756 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.547 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.045 data_at229 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H60 Cu4 N4 O12' _chemical_formula_weight 1283.28 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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.720(2) _cell_length_b 14.6735(17) _cell_length_c 18.5807(17) _cell_angle_alpha 90.00 _cell_angle_beta 93.943(8) _cell_angle_gamma 90.00 _cell_volume 5363.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 5031 _cell_measurement_theta_min 1.73 _cell_measurement_theta_max 24.00 _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2640 _exptl_absorpt_coefficient_mu 1.634 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8280 _exptl_absorpt_correction_T_max 0.9526 _exptl_absorpt_process_details 'XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate ( 34 cm diameter )' _diffrn_detector_type 'STOE' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9755 _diffrn_reflns_av_R_equivalents 0.1232 _diffrn_reflns_av_sigmaI/netI 0.1516 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.64 _reflns_number_total 4951 _reflns_number_gt 2472 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0462P)^2^+0.0000P] 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_number_reflns 4951 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1368 _refine_ls_R_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.1572 _refine_ls_wR_factor_gt 0.1362 _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_restrained_S_all 0.949 _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 Cu1 Cu 0.91100(4) 0.45914(7) 0.76060(5) 0.0464(3) Uani 1 1 d . . . Cu2 Cu 0.97897(4) 0.31534(7) 0.64206(5) 0.0490(3) Uani 1 1 d . . . O1 O 0.8466(2) 0.4974(3) 0.6840(3) 0.0498(12) Uani 1 1 d . . . O2 O 0.9751(3) 0.4289(3) 0.8397(3) 0.0550(13) Uani 1 1 d . . . O3 O 0.8393(3) 0.5906(5) 0.9436(3) 0.0766(18) Uani 1 1 d . . . H3B H 0.8270 0.5987 0.9855 0.115 Uiso 1 1 calc R . . O4 O 1.0399(2) 0.2778(4) 0.5742(3) 0.0563(14) Uani 1 1 d . . . O5 O 0.9206(2) 0.3416(3) 0.7168(3) 0.0525(13) Uani 1 1 d . . . O6 O 0.8244(3) 0.3658(4) 0.5839(3) 0.0677(16) Uani 1 1 d . . . H6B H 0.8297 0.4018 0.6190 0.102 Uiso 1 1 calc R . . C1 C 0.8221(3) 0.5799(5) 0.6714(4) 0.0455(18) Uani 1 1 d . . . C2 C 0.7792(4) 0.5901(6) 0.6077(4) 0.056(2) Uani 1 1 d . . . H2A H 0.7708 0.5391 0.5769 0.067 Uiso 1 1 calc R . . C3 C 0.7496(4) 0.6722(6) 0.5897(4) 0.057(2) Uani 1 1 d . . . H3A H 0.7214 0.6771 0.5463 0.069 Uiso 1 1 calc R . . C4 C 0.7602(4) 0.7504(5) 0.6345(4) 0.0481(18) Uani 1 1 d . . . C5 C 0.7296(4) 0.8351(6) 0.6168(5) 0.060(2) Uani 1 1 d . . . H5A H 0.7004 0.8392 0.5740 0.072 Uiso 1 1 calc R . . C6 C 0.7395(4) 0.9095(6) 0.6570(5) 0.062(2) Uani 1 1 d . . . H6A H 0.7177 0.9653 0.6435 0.074 Uiso 1 1 calc R . . C7 C 0.7829(4) 0.9036(6) 0.7198(4) 0.054(2) Uani 1 1 d . . . H7A H 0.7907 0.9561 0.7491 0.065 Uiso 1 1 calc R . . C8 C 0.8147(4) 0.8223(5) 0.7400(4) 0.0495(18) Uani 1 1 d . . . H8A H 0.8447 0.8205 0.7822 0.059 Uiso 1 1 calc R . . C9 C 0.8033(3) 0.7428(5) 0.6991(4) 0.0452(18) Uani 1 1 d . . . C10 C 0.8328(3) 0.6542(5) 0.7178(4) 0.0434(17) Uani 1 1 d . . . C11 C 0.8695(3) 0.6450(6) 0.7853(4) 0.0486(18) Uani 1 1 d . . . H11A H 0.8701 0.6964 0.8165 0.058 Uiso 1 1 calc R . . C12 C 0.9419(3) 0.5773(5) 0.8816(4) 0.0475(18) Uani 1 1 d . . . C15 C 1.0102(4) 0.6261(7) 0.8675(5) 0.077(3) Uani 1 1 d . . . H15A H 1.0009 0.6893 0.8527 0.115 Uiso 1 1 calc R . . H15B H 1.0323 0.5941 0.8292 0.115 Uiso 1 1 calc R . . H15C H 1.0402 0.6256 0.9118 0.115 Uiso 1 1 calc R . . C13 C 0.9559(5) 0.4776(6) 0.9016(4) 0.068(2) Uani 1 1 d . . . H13A H 0.9929 0.4741 0.9404 0.081 Uiso 1 1 calc R . . H13B H 0.9146 0.4498 0.9197 0.081 Uiso 1 1 calc R . . C14 C 0.9076(4) 0.6295(6) 0.9380(5) 0.058(2) Uani 1 1 d . . . H14A H 0.9343 0.6247 0.9850 0.069 Uiso 1 1 calc R . . H14B H 0.9041 0.6947 0.9245 0.069 Uiso 1 1 calc R . . C16 C 1.0314(4) 0.2126(5) 0.5250(5) 0.0514(19) Uani 1 1 d . . . C17 C 1.0843(4) 0.2042(6) 0.4766(4) 0.053(2) Uani 1 1 d . . . H17A H 1.1240 0.2407 0.4836 0.064 Uiso 1 1 calc R . . C18 C 1.0784(4) 0.1451(6) 0.4212(4) 0.054(2) Uani 1 1 d . . . H18A H 1.1146 0.1409 0.3901 0.065 Uiso 1 1 calc R . . C19 C 1.0206(4) 0.0885(6) 0.4069(4) 0.056(2) Uani 1 1 d . . . C20 C 1.0160(4) 0.0264(6) 0.3471(5) 0.063(2) Uani 1 1 d . . . H20A H 1.0522 0.0228 0.3160 0.076 Uiso 1 1 calc R . . C21 C 0.9600(4) -0.0278(7) 0.3344(5) 0.067(2) Uani 1 1 d . . . H21A H 0.9571 -0.0680 0.2943 0.081 Uiso 1 1 calc R . . C22 C 0.9069(4) -0.0237(6) 0.3807(5) 0.066(2) Uani 1 1 d . . . H22A H 0.8687 -0.0626 0.3724 0.079 Uiso 1 1 calc R . . C23 C 0.9093(4) 0.0354(7) 0.4377(5) 0.070(2) Uani 1 1 d . . . H23A H 0.8719 0.0378 0.4673 0.084 Uiso 1 1 calc R . . C24 C 0.9669(4) 0.0942(6) 0.4542(4) 0.056(2) Uani 1 1 d . . . C25 C 0.9739(4) 0.1596(6) 0.5138(4) 0.054(2) Uani 1 1 d . . . C26 C 0.9189(4) 0.1642(6) 0.5612(5) 0.056(2) Uani 1 1 d . . . H26A H 0.8816 0.1240 0.5514 0.067 Uiso 1 1 calc R . . C27 C 0.8525(3) 0.2228(5) 0.6549(4) 0.0476(18) Uani 1 1 d . . . C28 C 0.8730(4) 0.2696(6) 0.7267(4) 0.055(2) Uani 1 1 d . . . H28A H 0.8321 0.2948 0.7475 0.066 Uiso 1 1 calc R . . H28B H 0.8937 0.2243 0.7611 0.066 Uiso 1 1 calc R . . C30 C 0.8212(4) 0.1309(5) 0.6695(5) 0.055(2) Uani 1 1 d . . . H30A H 0.8536 0.0940 0.6993 0.083 Uiso 1 1 calc R . . H30B H 0.8099 0.0995 0.6236 0.083 Uiso 1 1 calc R . . H30C H 0.7797 0.1396 0.6949 0.083 Uiso 1 1 calc R . . C29 C 0.8006(4) 0.2794(6) 0.6085(4) 0.057(2) Uani 1 1 d . . . H29A H 0.7851 0.2428 0.5657 0.068 Uiso 1 1 calc R . . H29B H 0.7606 0.2904 0.6367 0.068 Uiso 1 1 calc R . . N1 N 0.9026(3) 0.5735(4) 0.8090(3) 0.0411(14) Uani 1 1 d . . . N2 N 0.9161(3) 0.2183(4) 0.6158(4) 0.0537(17) Uani 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 0.0523(5) 0.0506(6) 0.0362(5) -0.0014(4) 0.0020(4) 0.0042(4) Cu2 0.0522(5) 0.0521(6) 0.0428(6) 0.0001(5) 0.0052(4) -0.0047(4) O1 0.059(3) 0.042(3) 0.048(3) 0.003(2) 0.001(2) 0.002(3) O2 0.076(3) 0.053(3) 0.034(3) -0.003(3) -0.008(2) 0.015(3) O3 0.064(4) 0.110(5) 0.057(4) -0.015(4) 0.009(3) 0.007(4) O4 0.055(3) 0.068(4) 0.047(3) -0.003(3) 0.011(2) -0.015(3) O5 0.053(3) 0.047(3) 0.058(4) 0.002(3) 0.011(2) -0.005(2) O6 0.102(4) 0.064(4) 0.037(3) -0.008(3) 0.006(3) -0.004(3) C1 0.045(4) 0.046(4) 0.046(5) -0.003(4) 0.007(3) 0.002(3) C2 0.070(5) 0.061(5) 0.037(5) -0.007(4) 0.010(4) 0.012(4) C3 0.070(5) 0.055(5) 0.047(5) -0.001(4) 0.004(4) -0.003(4) C4 0.054(4) 0.053(5) 0.039(4) 0.004(4) 0.011(3) 0.005(4) C5 0.061(5) 0.066(6) 0.054(5) 0.003(5) 0.012(4) 0.006(4) C6 0.069(5) 0.066(6) 0.051(5) 0.011(5) 0.014(4) 0.018(4) C7 0.062(5) 0.050(5) 0.052(5) -0.008(4) 0.011(4) -0.001(4) C8 0.051(4) 0.046(5) 0.053(5) 0.006(4) 0.015(3) 0.002(4) C9 0.042(4) 0.052(5) 0.042(4) 0.007(4) 0.005(3) 0.006(3) C10 0.046(4) 0.053(5) 0.031(4) -0.003(3) 0.005(3) 0.001(3) C11 0.047(4) 0.053(5) 0.046(5) 0.000(4) 0.008(3) 0.007(4) C12 0.046(4) 0.057(5) 0.037(4) -0.008(4) -0.011(3) -0.002(3) C15 0.059(5) 0.094(8) 0.076(7) -0.022(6) -0.003(4) 0.003(5) C13 0.094(6) 0.072(6) 0.036(5) -0.012(4) -0.003(4) 0.011(5) C14 0.064(5) 0.056(5) 0.051(5) -0.005(4) -0.011(4) 0.010(4) C16 0.048(4) 0.049(5) 0.058(5) 0.003(4) 0.010(4) -0.002(4) C17 0.060(5) 0.057(5) 0.046(5) 0.013(4) 0.018(4) 0.000(4) C18 0.041(4) 0.071(5) 0.053(5) 0.010(5) 0.017(3) 0.002(4) C19 0.053(4) 0.070(6) 0.044(5) 0.006(4) 0.006(4) 0.001(4) C20 0.069(5) 0.071(6) 0.051(5) 0.002(5) 0.010(4) 0.006(5) C21 0.071(5) 0.082(7) 0.049(5) 0.003(5) 0.008(4) -0.004(5) C22 0.074(5) 0.064(6) 0.062(6) -0.002(5) 0.015(4) -0.005(5) C23 0.077(6) 0.082(7) 0.051(5) -0.014(5) 0.010(4) -0.003(5) C24 0.063(5) 0.059(5) 0.045(5) 0.001(4) 0.012(4) 0.000(4) C25 0.058(5) 0.060(5) 0.045(5) -0.006(4) 0.009(4) 0.006(4) C26 0.057(5) 0.052(5) 0.059(6) 0.004(4) 0.005(4) 0.000(4) C27 0.043(4) 0.049(4) 0.052(5) 0.007(4) 0.008(3) -0.009(3) C28 0.064(5) 0.058(5) 0.043(5) 0.004(4) 0.011(4) -0.002(4) C30 0.072(5) 0.040(4) 0.055(5) -0.008(4) 0.019(4) -0.001(4) C29 0.073(5) 0.054(5) 0.045(5) -0.007(4) 0.017(4) 0.001(4) N1 0.049(3) 0.045(3) 0.029(3) 0.000(3) 0.002(2) -0.004(3) N2 0.051(3) 0.058(4) 0.055(4) -0.006(4) 0.020(3) -0.008(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 N1 1.917(6) . ? Cu1 O5 1.921(5) . ? Cu1 O1 1.924(5) . ? Cu1 O2 1.924(5) . ? Cu2 O4 1.882(5) . ? Cu2 O5 1.903(5) . ? Cu2 O2 1.915(5) 2_756 ? Cu2 N2 1.928(6) . ? O1 C1 1.319(8) . ? O2 C13 1.427(9) . ? O2 Cu2 1.915(5) 2_756 ? O3 C14 1.473(9) . ? O3 H3B 0.8400 . ? O4 C16 1.327(9) . ? O5 C28 1.433(9) . ? O6 C29 1.437(9) . ? O6 H6B 0.8400 . ? C1 C10 1.397(10) . ? C1 C2 1.414(11) . ? C2 C3 1.370(11) . ? C2 H2A 0.9500 . ? C3 C4 1.425(11) . ? C3 H3A 0.9500 . ? C4 C5 1.412(11) . ? C4 C9 1.426(10) . ? C5 C6 1.329(12) . ? C5 H5A 0.9500 . ? C6 C7 1.403(12) . ? C6 H6A 0.9500 . ? C7 C8 1.386(10) . ? C7 H7A 0.9500 . ? C8 C9 1.403(10) . ? C8 H8A 0.9500 . ? C9 C10 1.456(10) . ? C10 C11 1.412(10) . ? C11 N1 1.296(9) . ? C11 H11A 0.9500 . ? C12 C14 1.497(11) . ? C12 N1 1.509(9) . ? C12 C13 1.531(12) . ? C12 C15 1.564(11) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C16 C25 1.379(10) . ? C16 C17 1.429(10) . ? C17 C18 1.345(11) . ? C17 H17A 0.9500 . ? C18 C19 1.421(11) . ? C18 H18A 0.9500 . ? C19 C24 1.423(11) . ? C19 C20 1.436(12) . ? C20 C21 1.367(11) . ? C20 H20A 0.9500 . ? C21 C22 1.403(12) . ? C21 H21A 0.9500 . ? C22 C23 1.366(12) . ? C22 H22A 0.9500 . ? C23 C24 1.444(11) . ? C23 H23A 0.9500 . ? C24 C25 1.465(11) . ? C25 C26 1.445(11) . ? C26 N2 1.293(10) . ? C26 H26A 0.9500 . ? C27 N2 1.495(9) . ? C27 C30 1.516(10) . ? C27 C28 1.531(11) . ? C27 C29 1.537(11) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? 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 N1 Cu1 O5 177.0(2) . . ? N1 Cu1 O1 91.0(2) . . ? O5 Cu1 O1 91.6(2) . . ? N1 Cu1 O2 85.2(2) . . ? O5 Cu1 O2 92.2(2) . . ? O1 Cu1 O2 176.2(2) . . ? O4 Cu2 O5 173.6(2) . . ? O4 Cu2 O2 93.3(2) . 2_756 ? O5 Cu2 O2 89.8(2) . 2_756 ? O4 Cu2 N2 92.4(2) . . ? O5 Cu2 N2 85.7(2) . . ? O2 Cu2 N2 167.1(3) 2_756 . ? C1 O1 Cu1 128.0(5) . . ? C13 O2 Cu2 116.2(5) . 2_756 ? C13 O2 Cu1 107.7(4) . . ? Cu2 O2 Cu1 127.9(3) 2_756 . ? C14 O3 H3B 109.5 . . ? C16 O4 Cu2 128.2(4) . . ? C28 O5 Cu2 112.2(4) . . ? C28 O5 Cu1 121.5(4) . . ? Cu2 O5 Cu1 125.0(3) . . ? C29 O6 H6B 109.5 . . ? O1 C1 C10 124.6(7) . . ? O1 C1 C2 115.9(7) . . ? C10 C1 C2 119.3(7) . . ? C3 C2 C1 121.2(8) . . ? C3 C2 H2A 119.4 . . ? C1 C2 H2A 119.4 . . ? C2 C3 C4 121.5(8) . . ? C2 C3 H3A 119.3 . . ? C4 C3 H3A 119.3 . . ? C5 C4 C3 122.0(7) . . ? C5 C4 C9 119.1(8) . . ? C3 C4 C9 118.9(7) . . ? C6 C5 C4 123.2(8) . . ? C6 C5 H5A 118.4 . . ? C4 C5 H5A 118.4 . . ? C5 C6 C7 118.3(8) . . ? C5 C6 H6A 120.8 . . ? C7 C6 H6A 120.8 . . ? C8 C7 C6 121.1(8) . . ? C8 C7 H7A 119.4 . . ? C6 C7 H7A 119.4 . . ? C7 C8 C9 121.1(7) . . ? C7 C8 H8A 119.5 . . ? C9 C8 H8A 119.5 . . ? C8 C9 C4 117.1(7) . . ? C8 C9 C10 124.5(6) . . ? C4 C9 C10 118.4(7) . . ? C1 C10 C11 121.4(7) . . ? C1 C10 C9 120.5(6) . . ? C11 C10 C9 118.0(7) . . ? N1 C11 C10 126.5(7) . . ? N1 C11 H11A 116.8 . . ? C10 C11 H11A 116.8 . . ? C14 C12 N1 114.6(6) . . ? C14 C12 C13 113.6(7) . . ? N1 C12 C13 104.8(6) . . ? C14 C12 C15 108.6(7) . . ? N1 C12 C15 105.3(6) . . ? C13 C12 C15 109.6(7) . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O2 C13 C12 109.6(6) . . ? O2 C13 H13A 109.7 . . ? C12 C13 H13A 109.7 . . ? O2 C13 H13B 109.7 . . ? C12 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? O3 C14 C12 108.0(6) . . ? O3 C14 H14A 110.1 . . ? C12 C14 H14A 110.1 . . ? O3 C14 H14B 110.1 . . ? C12 C14 H14B 110.1 . . ? H14A C14 H14B 108.4 . . ? O4 C16 C25 125.0(7) . . ? O4 C16 C17 115.7(7) . . ? C25 C16 C17 119.0(8) . . ? C18 C17 C16 120.6(7) . . ? C18 C17 H17A 119.7 . . ? C16 C17 H17A 119.7 . . ? C17 C18 C19 123.0(7) . . ? C17 C18 H18A 118.5 . . ? C19 C18 H18A 118.5 . . ? C18 C19 C24 118.2(8) . . ? C18 C19 C20 121.5(7) . . ? C24 C19 C20 120.3(8) . . ? C21 C20 C19 120.6(8) . . ? C21 C20 H20A 119.7 . . ? C19 C20 H20A 119.7 . . ? C20 C21 C22 119.8(9) . . ? C20 C21 H21A 120.1 . . ? C22 C21 H21A 120.1 . . ? C23 C22 C21 121.0(9) . . ? C23 C22 H22A 119.5 . . ? C21 C22 H22A 119.5 . . ? C22 C23 C24 121.9(8) . . ? C22 C23 H23A 119.0 . . ? C24 C23 H23A 119.0 . . ? C19 C24 C23 116.2(7) . . ? C19 C24 C25 118.0(7) . . ? C23 C24 C25 125.8(7) . . ? C16 C25 C26 121.8(7) . . ? C16 C25 C24 121.1(7) . . ? C26 C25 C24 117.1(7) . . ? N2 C26 C25 125.5(7) . . ? N2 C26 H26A 117.3 . . ? C25 C26 H26A 117.3 . . ? N2 C27 C30 114.5(6) . . ? N2 C27 C28 105.3(6) . . ? C30 C27 C28 109.3(6) . . ? N2 C27 C29 107.4(6) . . ? C30 C27 C29 108.5(6) . . ? C28 C27 C29 111.9(6) . . ? O5 C28 C27 110.8(6) . . ? O5 C28 H28A 109.5 . . ? C27 C28 H28A 109.5 . . ? O5 C28 H28B 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 108.1 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O6 C29 C27 115.9(6) . . ? O6 C29 H29A 108.3 . . ? C27 C29 H29A 108.3 . . ? O6 C29 H29B 108.3 . . ? C27 C29 H29B 108.3 . . ? H29A C29 H29B 107.4 . . ? C11 N1 C12 119.3(6) . . ? C11 N1 Cu1 127.4(5) . . ? C12 N1 Cu1 113.3(5) . . ? C26 N2 C27 119.4(6) . . ? C26 N2 Cu2 126.3(5) . . ? C27 N2 Cu2 113.0(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3B O6 0.84 1.91 2.720(8) 163.2 6_566 O6 H6B O1 0.84 1.87 2.696(7) 169.1 . O6 H6B O5 0.84 2.62 3.031(8) 111.8 . _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.467 _refine_diff_density_min -0.692 _refine_diff_density_rms 0.101 data_at384 _audit_update_record ; 2012-08-08 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63.50 H78.50 Cu4 N4 O17.75' _chemical_formula_weight 1435.96 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.808(9) _cell_length_b 26.728(9) _cell_length_c 13.601(7) _cell_angle_alpha 90.00 _cell_angle_beta 93.89(4) _cell_angle_gamma 90.00 _cell_volume 7184(5) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 20576 _cell_measurement_theta_min 1.28 _cell_measurement_theta_max 23.39 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.328 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2982 _exptl_absorpt_coefficient_mu 1.234 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.769 _exptl_absorpt_correction_T_max 0.875 _exptl_absorpt_process_details ? _exptl_special_details ? _diffrn_ambient_temperature 180(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 '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate ( 34 cm diameter )' _diffrn_detector_type 'STOE' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61516 _diffrn_reflns_av_R_equivalents 0.2007 _diffrn_reflns_av_sigmaI/netI 0.1844 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 25.78 _reflns_number_total 13579 _reflns_number_gt 5209 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0830P)^2^] 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 0.0085(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 13579 _refine_ls_number_parameters 880 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1968 _refine_ls_R_factor_gt 0.0809 _refine_ls_wR_factor_ref 0.2188 _refine_ls_wR_factor_gt 0.1820 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.002 _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 0.31119(5) 0.51224(4) 0.25331(8) 0.0535(3) Uani 1 1 d . . . Cu2 Cu 0.23879(6) 0.58742(4) 0.09093(8) 0.0551(3) Uani 1 1 d . . . Cu3 Cu 0.19653(6) 0.47061(4) 0.06057(8) 0.0528(3) Uani 1 1 d . . . Cu4 Cu 0.15482(5) 0.51753(4) 0.25832(8) 0.0512(3) Uani 1 1 d . . . O11 O 0.3926(3) 0.5500(2) 0.2578(5) 0.0639(17) Uani 1 1 d . . . O21 O 0.2310(3) 0.4714(2) 0.2394(4) 0.0487(14) Uani 1 1 d . . . O31 O 0.3850(4) 0.3625(3) 0.1826(6) 0.101(3) Uani 1 1 d . . . H311 H 0.4078 0.3819 0.1494 0.152 Uiso 1 1 calc R . . N11 N 0.3572(4) 0.4525(3) 0.2976(5) 0.0493(18) Uani 1 1 d . . . C11 C 0.4670(5) 0.4902(4) 0.3417(7) 0.056(2) Uani 1 1 d . . . C21 C 0.4512(5) 0.5380(4) 0.3025(7) 0.058(2) Uani 1 1 d . . . C31 C 0.5005(5) 0.5751(4) 0.3090(8) 0.068(3) Uani 1 1 d . . . H31 H 0.4899 0.6071 0.2822 0.082 Uiso 1 1 calc R . . C41 C 0.5648(5) 0.5668(4) 0.3536(8) 0.069(3) Uani 1 1 d . . . H41 H 0.5973 0.5930 0.3562 0.082 Uiso 1 1 calc R . . C51 C 0.6470(5) 0.5115(4) 0.4430(8) 0.066(3) Uani 1 1 d . . . H51 H 0.6795 0.5377 0.4433 0.079 Uiso 1 1 calc R . . C61 C 0.6638(5) 0.4679(4) 0.4881(8) 0.070(3) Uani 1 1 d . . . H61 H 0.7071 0.4634 0.5215 0.084 Uiso 1 1 calc R . . C71 C 0.6161(5) 0.4299(4) 0.4843(8) 0.071(3) Uani 1 1 d . . . H71 H 0.6280 0.3988 0.5147 0.085 Uiso 1 1 calc R . . C81 C 0.5522(5) 0.4352(4) 0.4383(8) 0.066(3) Uani 1 1 d . . . H81 H 0.5209 0.4083 0.4386 0.079 Uiso 1 1 calc R . . C91 C 0.5331(5) 0.4811(4) 0.3903(7) 0.058(2) Uani 1 1 d . . . C101 C 0.5824(5) 0.5193(4) 0.3952(7) 0.063(3) Uani 1 1 d . . . C111 C 0.4193(5) 0.4498(4) 0.3337(7) 0.055(2) Uani 1 1 d . . . H111 H 0.4347 0.4180 0.3571 0.067 Uiso 1 1 calc R . . C121 C 0.3127(4) 0.4079(3) 0.2920(7) 0.055(2) Uani 1 1 d . . . C131 C 0.2410(4) 0.4278(3) 0.2982(7) 0.053(2) Uani 1 1 d . . . H131 H 0.2081 0.4017 0.2751 0.064 Uiso 1 1 calc R . . H132 H 0.2332 0.4357 0.3676 0.064 Uiso 1 1 calc R . . C141 C 0.3189(5) 0.3825(4) 0.1892(7) 0.066(3) Uani 1 1 d . . . H141 H 0.2850 0.3553 0.1802 0.079 Uiso 1 1 calc R . . H142 H 0.3095 0.4074 0.1362 0.079 Uiso 1 1 calc R . . C151 C 0.3274(5) 0.3692(4) 0.3752(7) 0.066(3) Uani 1 1 d . . . H151 H 0.3694 0.3513 0.3641 0.099 Uiso 1 1 calc R . . H152 H 0.2899 0.3453 0.3754 0.099 Uiso 1 1 calc R . . H153 H 0.3322 0.3865 0.4389 0.099 Uiso 1 1 calc R . . O12 O 0.2108(3) 0.6053(2) -0.0414(4) 0.0637(17) Uani 1 1 d . . . O22 O 0.2553(3) 0.5712(2) 0.2299(4) 0.0529(15) Uani 1 1 d . . . O32 O 0.3678(4) 0.6317(3) 0.1508(5) 0.0726(19) Uani 1 1 d . . . H321 H 0.3744 0.6057 0.1848 0.109 Uiso 1 1 calc R . . N12 N 0.2304(4) 0.6554(3) 0.1362(5) 0.056(2) Uani 1 1 d . . . C12 C 0.1653(5) 0.6867(4) -0.0068(7) 0.062(3) Uani 1 1 d . . . C22 C 0.1724(5) 0.6441(4) -0.0685(7) 0.060(3) Uani 1 1 d . . . C32 C 0.1394(5) 0.6425(4) -0.1639(7) 0.062(3) Uani 1 1 d . . . H32 H 0.1453 0.6141 -0.2044 0.074 Uiso 1 1 calc R . . C42 C 0.0995(5) 0.6808(4) -0.1987(7) 0.068(3) Uani 1 1 d . . . H42 H 0.0783 0.6787 -0.2634 0.082 Uiso 1 1 calc R . . C52 C 0.0454(5) 0.7647(4) -0.1749(8) 0.071(3) Uani 1 1 d . . . H52 H 0.0236 0.7628 -0.2392 0.086 Uiso 1 1 calc R . . C62 C 0.0352(6) 0.8053(4) -0.1179(9) 0.083(3) Uani 1 1 d . . . H62 H 0.0073 0.8318 -0.1432 0.100 Uiso 1 1 calc R . . C72 C 0.0655(6) 0.8085(4) -0.0219(9) 0.086(3) Uani 1 1 d . . . H72 H 0.0577 0.8368 0.0179 0.103 Uiso 1 1 calc R . . C82 C 0.1076(6) 0.7696(4) 0.0150(8) 0.074(3) Uani 1 1 d . . . H82 H 0.1280 0.7722 0.0801 0.089 Uiso 1 1 calc R . . C92 C 0.1203(5) 0.7271(4) -0.0414(8) 0.064(3) Uani 1 1 d . . . C102 C 0.0884(5) 0.7245(4) -0.1396(7) 0.063(3) Uani 1 1 d . . . C112 C 0.1996(5) 0.6920(4) 0.0879(7) 0.065(3) Uani 1 1 d . . . H112 H 0.2001 0.7241 0.1179 0.078 Uiso 1 1 calc R . . C122 C 0.2676(5) 0.6643(4) 0.2353(7) 0.061(3) Uani 1 1 d . . . C132 C 0.2560(5) 0.6142(3) 0.2908(7) 0.061(3) Uani 1 1 d . . . H133 H 0.2923 0.6102 0.3441 0.073 Uiso 1 1 calc R . . H134 H 0.2124 0.6162 0.3221 0.073 Uiso 1 1 calc R . . C142 C 0.3405(5) 0.6701(4) 0.2100(8) 0.074(3) Uani 1 1 d . . . H143 H 0.3447 0.7024 0.1753 0.089 Uiso 1 1 calc R . . H144 H 0.3690 0.6723 0.2725 0.089 Uiso 1 1 calc R . . C152 C 0.2448(6) 0.7073(4) 0.2933(8) 0.080(3) Uani 1 1 d . . . H154 H 0.2568 0.7386 0.2612 0.119 Uiso 1 1 calc R . . H155 H 0.2669 0.7061 0.3599 0.119 Uiso 1 1 calc R . . H156 H 0.1957 0.7057 0.2970 0.119 Uiso 1 1 calc R . . O13 O 0.1372(3) 0.4174(2) 0.0788(4) 0.0511(15) Uani 1 1 d . . . O23 O 0.2675(3) 0.5205(2) 0.0586(4) 0.0518(15) Uani 1 1 d . . . O33 O 0.1840(4) 0.5185(3) -0.1360(5) 0.076(2) Uani 1 1 d . . . H331 H 0.1937 0.5442 -0.1024 0.114 Uiso 1 1 calc R . . N13 N 0.2433(3) 0.4363(3) -0.0378(5) 0.0495(18) Uani 1 1 d . . . C13 C 0.1792(5) 0.3597(3) -0.0403(6) 0.050(2) Uani 1 1 d . . . C23 C 0.1365(5) 0.3727(3) 0.0327(7) 0.053(2) Uani 1 1 d . . . C33 C 0.0848(4) 0.3390(4) 0.0599(7) 0.058(2) Uani 1 1 d . . . H33 H 0.0556 0.3484 0.1092 0.070 Uiso 1 1 calc R . . C43 C 0.0774(5) 0.2954(4) 0.0176(8) 0.068(3) Uani 1 1 d . . . H43 H 0.0437 0.2734 0.0390 0.081 Uiso 1 1 calc R . . C53 C 0.1060(7) 0.2315(4) -0.1057(9) 0.084(3) Uani 1 1 d . . . H53 H 0.0720 0.2098 -0.0837 0.101 Uiso 1 1 calc R . . C63 C 0.1439(7) 0.2167(4) -0.1821(9) 0.085(3) Uani 1 1 d . . . H63 H 0.1348 0.1859 -0.2151 0.102 Uiso 1 1 calc R . . C73 C 0.1955(7) 0.2477(5) -0.2101(9) 0.096(4) Uani 1 1 d . . . H73 H 0.2237 0.2365 -0.2595 0.115 Uiso 1 1 calc R . . C83 C 0.2073(6) 0.2948(4) -0.1676(8) 0.082(3) Uani 1 1 d . . . H83 H 0.2413 0.3160 -0.1907 0.099 Uiso 1 1 calc R . . C93 C 0.1682(5) 0.3109(4) -0.0900(7) 0.060(3) Uani 1 1 d . . . C103 C 0.1176(5) 0.2792(4) -0.0592(7) 0.063(3) Uani 1 1 d . . . C113 C 0.2280(5) 0.3937(4) -0.0758(6) 0.052(2) Uani 1 1 d . . . H113 H 0.2509 0.3837 -0.1318 0.063 Uiso 1 1 calc R . . C123 C 0.2883(5) 0.4712(3) -0.0889(7) 0.055(2) Uani 1 1 d . . . C133 C 0.3170(4) 0.5080(3) -0.0097(7) 0.055(2) Uani 1 1 d . . . H135 H 0.3569 0.4929 0.0265 0.065 Uiso 1 1 calc R . . H136 H 0.3319 0.5390 -0.0419 0.065 Uiso 1 1 calc R . . C143 C 0.2435(5) 0.4976(4) -0.1691(7) 0.066(3) Uani 1 1 d . . . H145 H 0.2702 0.5245 -0.1982 0.079 Uiso 1 1 calc R . . H146 H 0.2310 0.4732 -0.2220 0.079 Uiso 1 1 calc R . . C153 C 0.3481(5) 0.4463(4) -0.1359(8) 0.080(3) Uani 1 1 d . . . H157 H 0.3713 0.4236 -0.0881 0.120 Uiso 1 1 calc R . . H158 H 0.3797 0.4720 -0.1554 0.120 Uiso 1 1 calc R . . H159 H 0.3313 0.4273 -0.1941 0.120 Uiso 1 1 calc R . . O14 O 0.1714(3) 0.5189(2) 0.3974(4) 0.0558(16) Uani 1 1 d . . . O24 O 0.1403(3) 0.5213(2) 0.1162(4) 0.0525(15) Uani 1 1 d . . . O34 O 0.0177(12) 0.6466(6) 0.1780(13) 0.086(6) Uani 0.379(4) 1 d P A 1 H34A H -0.0044 0.6643 0.1361 0.129 Uiso 0.379(4) 1 calc PR A 1 O341 O -0.0750(9) 0.5971(8) 0.2058(13) 0.091(8) Uani 0.410(19) 1 d P A 2 H341 H -0.0639 0.6263 0.1908 0.136 Uiso 0.410(19) 1 calc PR A 2 O342 O -0.0580(12) 0.5136(11) 0.174(2) 0.041(9) Uani 0.210(19) 1 d P A 3 H342 H -0.0686 0.4985 0.1206 0.062 Uiso 0.210(19) 1 calc PR A 3 N14 N 0.0683(4) 0.5495(3) 0.2596(5) 0.0503(18) Uani 1 1 d . A . C14 C 0.0632(4) 0.5516(3) 0.4386(6) 0.048(2) Uani 1 1 d . . . C24 C 0.1292(4) 0.5322(3) 0.4606(6) 0.050(2) Uani 1 1 d . . . C34 C 0.1515(5) 0.5240(4) 0.5618(7) 0.058(2) Uani 1 1 d . . . H34 H 0.1943 0.5088 0.5772 0.070 Uiso 1 1 calc R . . C44 C 0.1124(5) 0.5375(3) 0.6372(7) 0.056(2) Uani 1 1 d . . . H44 H 0.1298 0.5336 0.7036 0.067 Uiso 1 1 calc R . . C54 C 0.0056(5) 0.5695(4) 0.6948(7) 0.058(2) Uani 1 1 d . . . H54 H 0.0237 0.5651 0.7607 0.070 Uiso 1 1 calc R . . C64 C -0.0578(5) 0.5871(3) 0.6796(7) 0.060(2) Uani 1 1 d . . . H64 H -0.0844 0.5942 0.7335 0.072 Uiso 1 1 calc R . . C74 C -0.0840(5) 0.5946(4) 0.5818(7) 0.062(3) Uani 1 1 d . . . H74 H -0.1284 0.6076 0.5695 0.074 Uiso 1 1 calc R . . C84 C -0.0454(4) 0.5833(3) 0.5034(7) 0.054(2) Uani 1 1 d . . . H84 H -0.0642 0.5883 0.4381 0.064 Uiso 1 1 calc R . . C94 C 0.0205(4) 0.5646(3) 0.5181(7) 0.050(2) Uani 1 1 d . . . C104 C 0.0464(4) 0.5574(3) 0.6172(6) 0.050(2) Uani 1 1 d . . . C114 C 0.0375(5) 0.5595(3) 0.3380(7) 0.052(2) Uani 1 1 d . . . H114 H -0.0065 0.5735 0.3285 0.063 Uiso 1 1 calc R . . C124 C 0.0362(5) 0.5612(4) 0.1596(7) 0.057(2) Uani 1 1 d . . . C134 C 0.0696(4) 0.5244(4) 0.0913(6) 0.056(2) Uani 1 1 d . A . H13A H 0.0490 0.4909 0.0972 0.067 Uiso 1 1 calc R . . H13B H 0.0617 0.5356 0.0221 0.067 Uiso 1 1 calc R . . C144 C 0.0560(6) 0.6138(4) 0.1317(8) 0.074(3) Uani 1 1 d . A . H14A H 0.1044 0.6196 0.1512 0.088 Uiso 0.379(4) 1 calc PR A 1 H14B H 0.0490 0.6183 0.0595 0.088 Uiso 0.379(4) 1 calc PR A 1 H14C H 0.1053 0.6174 0.1401 0.111 Uiso 0.621(4) 1 calc PR A 2 H14D H 0.0346 0.6379 0.1742 0.111 Uiso 0.621(4) 1 calc PR A 2 H14E H 0.0408 0.6202 0.0628 0.111 Uiso 0.621(4) 1 calc PR A 2 C154 C -0.0348(19) 0.5576(18) 0.143(3) 0.039(12) Uiso 0.410(19) 1 d P A 2 H15A H -0.0492 0.5234 0.1596 0.047 Uiso 0.410(19) 1 calc PR A 2 H15B H -0.0472 0.5631 0.0719 0.047 Uiso 0.410(19) 1 calc PR A 2 C155 C -0.039(3) 0.569(2) 0.151(5) 0.03(2) Uiso 0.210(19) 1 d P A 3 H15C H -0.0564 0.5794 0.0841 0.041 Uiso 0.210(19) 1 calc PR A 3 H15D H -0.0549 0.5924 0.2007 0.041 Uiso 0.210(19) 1 calc PR A 3 C156 C -0.0469(16) 0.5438(19) 0.157(3) 0.043(9) Uiso 0.379(4) 1 d P A 1 H15E H -0.0500 0.5088 0.1777 0.064 Uiso 0.379(4) 1 calc PR A 1 H15F H -0.0677 0.5476 0.0902 0.064 Uiso 0.379(4) 1 calc PR A 1 H15G H -0.0706 0.5651 0.2024 0.064 Uiso 0.379(4) 1 calc PR A 1 O1M O 0.4684(6) 0.4142(6) 0.0690(9) 0.160(5) Uani 1 1 d . . . H1M H 0.4838 0.4004 0.0197 0.240 Uiso 1 1 calc R . . C1M C 0.5097(9) 0.4545(8) 0.0989(14) 0.170(8) Uani 1 1 d . . . H1M1 H 0.4823 0.4806 0.1271 0.255 Uiso 1 1 calc R . . H1M2 H 0.5315 0.4679 0.0419 0.255 Uiso 1 1 calc R . . H1M3 H 0.5445 0.4431 0.1486 0.255 Uiso 1 1 calc R . . O2M O 0.2751(11) 0.8136(6) 0.1185(16) 0.139(9) Uani 0.50 1 d P . . H2M H 0.3165 0.8196 0.1154 0.209 Uiso 0.50 1 calc PR . . C2M C 0.2411(12) 0.8520(9) 0.0916(17) 0.081(7) Uani 0.50 1 d P . . H2M1 H 0.1971 0.8510 0.1204 0.122 Uiso 0.50 1 calc PR . . H2M2 H 0.2343 0.8525 0.0196 0.122 Uiso 0.50 1 calc PR . . H2M3 H 0.2657 0.8822 0.1141 0.122 Uiso 0.50 1 calc PR . . O3M O 0.3246(11) 0.2843(9) 0.6164(17) 0.071(6) Uiso 0.30 1 d P B 1 H3M H 0.3478 0.2685 0.6601 0.107 Uiso 0.30 1 calc PR B 1 O3M1 O 0.309(3) 0.1992(19) 0.552(4) 0.126(16) Uiso 0.20 1 d P B 2 H3M1 H 0.3455 0.1916 0.5832 0.189 Uiso 0.20 1 calc PR B 2 C3M C 0.3026(19) 0.2535(9) 0.5472(17) 0.135(13) Uani 0.50 1 d P . . H3M2 H 0.2554 0.2614 0.5267 0.203 Uiso 0.30 1 calc PR B 1 H3M3 H 0.3055 0.2191 0.5722 0.203 Uiso 0.30 1 calc PR B 1 H3M4 H 0.3304 0.2568 0.4906 0.203 Uiso 0.30 1 calc PR B 1 H3M5 H 0.3212 0.2681 0.6094 0.203 Uiso 0.20 1 calc PR B 2 H3M6 H 0.2548 0.2625 0.5365 0.203 Uiso 0.20 1 calc PR B 2 H3M7 H 0.3276 0.2664 0.4928 0.203 Uiso 0.20 1 calc PR B 2 O4M O 0.2759(5) 0.3743(4) 0.6653(7) 0.111(3) Uani 1 1 d . . . H4M H 0.2931 0.3470 0.6494 0.166 Uiso 1 1 calc R . . C4M C 0.2093(7) 0.3779(7) 0.6214(12) 0.137(6) Uani 1 1 d . . . H4M1 H 0.1777 0.3833 0.6726 0.205 Uiso 1 1 calc R . . H4M2 H 0.1976 0.3469 0.5859 0.205 Uiso 1 1 calc R . . H4M3 H 0.2066 0.4061 0.5751 0.205 Uiso 1 1 calc R . . O5M O 0.3317(15) 0.6399(11) 0.829(2) 0.233(17) Uani 0.50 1 d P . . H5M H 0.2945 0.6306 0.8017 0.350 Uiso 0.50 1 calc PR . . C5M C 0.367(2) 0.6753(11) 0.759(3) 0.166(17) Uani 0.50 1 d P . . H5M1 H 0.4097 0.6876 0.7923 0.249 Uiso 0.50 1 calc PR . . H5M2 H 0.3378 0.7037 0.7413 0.249 Uiso 0.50 1 calc PR . . H5M3 H 0.3775 0.6570 0.6994 0.249 Uiso 0.50 1 calc PR . . O1W O 0.4304(15) 0.2693(9) 0.208(2) 0.200(12) Uani 0.50 1 d P . . O2W O 0.5651(19) 0.7031(13) 0.145(2) 0.230(15) Uani 0.50 1 d P . . O3W O 0.4667(10) 0.6555(6) 0.0395(14) 0.125(7) Uani 0.50 1 d P . . O4W O 0.6173(15) 0.2856(11) 0.505(2) 0.203(11) Uiso 0.50 1 d P . . O5W O 0.500(3) 0.299(2) 0.547(4) 0.19(2) Uiso 0.25 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 Cu1 0.0500(6) 0.0546(7) 0.0558(7) -0.0006(6) 0.0031(5) 0.0011(6) Cu2 0.0623(7) 0.0531(7) 0.0499(7) -0.0021(6) 0.0037(5) 0.0041(6) Cu3 0.0524(7) 0.0574(7) 0.0492(7) -0.0051(5) 0.0077(5) 0.0009(5) Cu4 0.0485(6) 0.0581(7) 0.0472(6) -0.0034(5) 0.0048(5) 0.0039(5) O11 0.053(4) 0.061(4) 0.077(5) 0.007(3) -0.003(3) -0.006(3) O21 0.051(3) 0.051(4) 0.043(3) 0.001(3) 0.002(3) 0.003(3) O31 0.097(6) 0.099(6) 0.112(7) -0.017(5) 0.039(5) 0.000(5) N11 0.046(4) 0.053(5) 0.049(4) -0.004(4) 0.002(4) 0.004(4) C11 0.054(6) 0.055(6) 0.058(6) -0.008(5) 0.003(5) 0.007(5) C21 0.048(6) 0.057(6) 0.068(6) -0.009(5) 0.002(5) -0.007(5) C31 0.063(7) 0.063(7) 0.080(7) 0.004(6) 0.007(6) 0.004(6) C41 0.060(7) 0.072(7) 0.076(7) -0.012(6) 0.014(6) -0.010(6) C51 0.053(6) 0.072(7) 0.074(7) -0.008(6) 0.011(5) 0.002(5) C61 0.049(6) 0.086(8) 0.076(7) -0.005(6) 0.002(5) 0.004(6) C71 0.059(7) 0.078(7) 0.075(7) 0.005(6) -0.002(6) 0.009(6) C81 0.058(6) 0.064(7) 0.075(7) -0.002(6) -0.002(5) 0.001(5) C91 0.057(6) 0.062(6) 0.054(6) -0.004(5) 0.004(5) 0.000(5) C101 0.052(6) 0.073(7) 0.065(6) -0.006(6) 0.006(5) -0.002(5) C111 0.049(6) 0.058(6) 0.061(6) -0.011(5) 0.010(5) 0.006(5) C121 0.052(5) 0.052(6) 0.059(6) 0.001(5) 0.003(5) 0.001(5) C131 0.047(5) 0.054(6) 0.059(6) -0.001(5) 0.006(4) 0.001(4) C141 0.058(6) 0.076(7) 0.063(7) -0.007(5) 0.006(5) 0.009(5) C151 0.082(7) 0.059(6) 0.056(6) 0.007(5) 0.003(5) -0.005(5) O12 0.076(4) 0.058(4) 0.057(4) 0.002(3) 0.004(3) 0.014(4) O22 0.058(4) 0.049(3) 0.051(4) -0.006(3) -0.002(3) 0.001(3) O32 0.071(5) 0.072(5) 0.076(5) 0.007(4) 0.010(4) 0.007(4) N12 0.062(5) 0.050(5) 0.056(5) -0.005(4) 0.000(4) 0.001(4) C12 0.079(7) 0.051(6) 0.057(6) 0.006(5) 0.009(5) 0.000(5) C22 0.072(7) 0.057(6) 0.052(6) 0.004(5) 0.004(5) -0.001(5) C32 0.069(7) 0.064(7) 0.052(6) 0.004(5) 0.004(5) 0.001(5) C42 0.089(8) 0.066(7) 0.050(6) 0.003(5) 0.005(6) 0.004(6) C52 0.072(7) 0.068(7) 0.074(7) 0.021(6) 0.006(6) 0.003(6) C62 0.101(9) 0.072(8) 0.078(8) 0.027(7) 0.008(7) 0.014(7) C72 0.112(10) 0.068(7) 0.080(9) 0.013(6) 0.016(7) 0.017(7) C82 0.096(8) 0.048(6) 0.078(7) 0.001(5) 0.002(6) 0.016(6) C92 0.075(7) 0.051(6) 0.068(7) 0.008(5) 0.008(6) -0.001(5) C102 0.062(6) 0.070(7) 0.059(6) 0.012(5) 0.015(5) 0.000(5) C112 0.082(7) 0.056(6) 0.057(6) -0.002(5) 0.006(6) 0.014(6) C122 0.048(5) 0.067(6) 0.065(6) 0.015(5) -0.013(5) -0.002(5) C132 0.065(6) 0.057(6) 0.058(6) -0.016(5) -0.009(5) 0.006(5) C142 0.069(7) 0.064(7) 0.088(8) -0.008(6) -0.004(6) -0.008(6) C152 0.098(9) 0.071(7) 0.069(7) -0.006(6) -0.003(6) 0.001(6) O13 0.044(3) 0.067(4) 0.043(3) -0.007(3) 0.007(3) -0.008(3) O23 0.065(4) 0.045(4) 0.047(3) -0.003(3) 0.012(3) 0.000(3) O33 0.083(5) 0.072(5) 0.071(5) -0.001(4) -0.008(4) 0.003(4) N13 0.047(4) 0.049(5) 0.054(5) 0.000(4) 0.015(4) 0.000(4) C13 0.055(5) 0.048(5) 0.048(5) 0.000(4) 0.009(4) 0.002(4) C23 0.061(6) 0.051(6) 0.048(5) -0.001(5) -0.002(5) -0.003(5) C33 0.049(6) 0.074(7) 0.052(6) 0.011(5) 0.012(5) -0.010(5) C43 0.067(7) 0.076(8) 0.062(7) 0.022(6) 0.012(6) -0.004(6) C53 0.122(10) 0.047(6) 0.083(8) 0.002(6) 0.008(8) -0.001(6) C63 0.118(10) 0.054(7) 0.085(8) -0.025(6) 0.024(8) -0.019(7) C73 0.121(10) 0.079(9) 0.093(9) -0.030(7) 0.038(8) -0.014(8) C83 0.117(9) 0.060(7) 0.073(7) -0.011(6) 0.032(7) -0.017(7) C93 0.066(6) 0.058(6) 0.055(6) 0.005(5) 0.005(5) -0.005(5) C103 0.074(7) 0.055(6) 0.060(6) 0.007(5) 0.006(6) -0.002(5) C113 0.060(6) 0.055(6) 0.044(5) 0.001(5) 0.007(4) 0.002(5) C123 0.055(6) 0.057(6) 0.054(6) -0.003(5) 0.010(5) -0.008(5) C133 0.052(5) 0.052(5) 0.060(6) -0.002(5) 0.008(5) -0.003(5) C143 0.073(7) 0.081(7) 0.045(5) 0.000(5) 0.010(5) -0.014(6) C153 0.075(7) 0.082(8) 0.088(8) -0.027(6) 0.040(6) -0.007(6) O14 0.047(3) 0.069(4) 0.052(4) -0.009(3) 0.008(3) 0.007(3) O24 0.044(3) 0.062(4) 0.051(3) -0.005(3) 0.000(3) 0.004(3) O34 0.147(19) 0.051(11) 0.058(11) -0.001(9) -0.002(12) 0.016(12) O341 0.075(13) 0.113(16) 0.085(14) -0.013(12) 0.017(10) 0.023(11) O342 0.034(15) 0.025(18) 0.065(19) 0.015(14) 0.003(12) -0.002(12) N14 0.056(4) 0.055(5) 0.039(4) -0.001(3) -0.002(4) 0.000(4) C14 0.048(5) 0.050(5) 0.046(5) -0.001(4) 0.009(4) 0.001(4) C24 0.053(5) 0.051(5) 0.046(5) -0.009(4) 0.010(5) -0.011(4) C34 0.052(5) 0.072(7) 0.051(6) 0.002(5) -0.002(5) -0.008(5) C44 0.052(6) 0.068(6) 0.046(5) 0.001(5) 0.004(5) 0.004(5) C54 0.068(7) 0.064(6) 0.043(5) 0.005(5) 0.007(5) 0.000(5) C64 0.057(6) 0.057(6) 0.066(7) -0.003(5) 0.011(5) 0.002(5) C74 0.051(6) 0.070(7) 0.068(7) 0.006(5) 0.021(5) 0.002(5) C84 0.051(5) 0.057(6) 0.053(6) 0.005(5) 0.004(5) -0.002(5) C94 0.047(5) 0.044(5) 0.060(6) 0.000(4) 0.008(4) -0.004(4) C104 0.054(6) 0.053(6) 0.045(5) 0.002(4) 0.016(5) -0.003(4) C114 0.054(5) 0.051(6) 0.052(6) 0.002(5) 0.006(5) -0.001(4) C124 0.054(6) 0.071(7) 0.046(5) -0.001(5) 0.003(5) 0.008(5) C134 0.048(5) 0.073(7) 0.046(5) -0.010(5) 0.000(4) 0.007(5) C144 0.080(7) 0.075(8) 0.066(7) 0.014(6) 0.004(6) 0.017(6) O1M 0.125(9) 0.242(15) 0.119(9) -0.014(9) 0.046(7) -0.027(10) C1M 0.129(14) 0.22(2) 0.168(18) -0.069(15) 0.032(12) -0.077(15) O2M 0.153(18) 0.063(11) 0.20(2) 0.070(13) -0.029(15) -0.044(12) C2M 0.092(16) 0.075(16) 0.080(15) 0.027(13) 0.021(13) -0.043(14) C3M 0.29(4) 0.065(16) 0.049(14) -0.020(12) 0.016(19) -0.03(2) O4M 0.106(7) 0.136(8) 0.089(6) 0.003(6) -0.007(5) -0.034(6) C4M 0.095(11) 0.183(16) 0.127(13) 0.037(11) -0.037(10) -0.020(11) O5M 0.20(3) 0.21(3) 0.28(4) 0.16(3) -0.03(3) -0.05(2) C5M 0.26(5) 0.09(2) 0.14(3) -0.01(2) -0.08(3) 0.01(3) O1W 0.25(3) 0.128(19) 0.23(3) 0.064(19) 0.07(2) 0.11(2) O2W 0.29(4) 0.25(4) 0.15(2) 0.00(2) 0.03(2) -0.08(3) O3W 0.165(17) 0.081(11) 0.145(15) -0.036(10) 0.132(14) -0.051(11) _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 O11 1.900(6) . ? Cu1 N11 1.915(7) . ? Cu1 O21 1.926(6) . ? Cu1 O22 1.939(6) . ? Cu2 O12 1.908(6) . ? Cu2 N12 1.930(7) . ? Cu2 O23 1.937(6) . ? Cu2 O22 1.945(6) . ? Cu3 O13 1.873(6) . ? Cu3 N13 1.912(7) . ? Cu3 O23 1.939(6) . ? Cu3 O24 1.940(6) . ? Cu4 O14 1.898(6) . ? Cu4 N14 1.917(7) . ? Cu4 O24 1.938(6) . ? Cu4 O21 1.978(6) . ? O11 C21 1.313(10) . ? O21 C131 1.422(10) . ? O31 C141 1.423(11) . ? O31 H311 0.8400 . ? N11 C111 1.294(10) . ? N11 C121 1.481(11) . ? C11 C21 1.409(13) . ? C11 C111 1.437(13) . ? C11 C91 1.447(12) . ? C21 C31 1.390(13) . ? C31 C41 1.391(13) . ? C31 H31 0.9500 . ? C41 C101 1.423(14) . ? C41 H41 0.9500 . ? C51 C61 1.348(14) . ? C51 C101 1.412(13) . ? C51 H51 0.9500 . ? C61 C71 1.385(14) . ? C61 H61 0.9500 . ? C71 C81 1.381(13) . ? C71 H71 0.9500 . ? C81 C91 1.429(13) . ? C81 H81 0.9500 . ? C91 C101 1.411(13) . ? C111 H111 0.9500 . ? C121 C131 1.523(12) . ? C121 C151 1.547(12) . ? C121 C141 1.566(13) . ? C131 H131 0.9900 . ? C131 H132 0.9900 . ? C141 H141 0.9900 . ? C141 H142 0.9900 . ? C151 H151 0.9800 . ? C151 H152 0.9800 . ? C151 H153 0.9800 . ? O12 C22 1.323(11) . ? O22 C132 1.417(10) . ? O32 C142 1.433(12) . ? O32 H321 0.8400 . ? N12 C112 1.306(11) . ? N12 C122 1.511(11) . ? C12 C112 1.422(13) . ? C12 C22 1.426(13) . ? C12 C92 1.458(13) . ? C22 C32 1.412(13) . ? C32 C42 1.358(13) . ? C32 H32 0.9500 . ? C42 C102 1.444(14) . ? C42 H42 0.9500 . ? C52 C62 1.357(15) . ? C52 C102 1.433(14) . ? C52 H52 0.9500 . ? C62 C72 1.402(15) . ? C62 H62 0.9500 . ? C72 C82 1.402(14) . ? C72 H72 0.9500 . ? C82 C92 1.404(14) . ? C82 H82 0.9500 . ? C92 C102 1.439(13) . ? C112 H112 0.9500 . ? C122 C152 1.481(14) . ? C122 C142 1.514(14) . ? C122 C132 1.564(13) . ? C132 H133 0.9900 . ? C132 H134 0.9900 . ? C142 H143 0.9900 . ? C142 H144 0.9900 . ? C152 H154 0.9800 . ? C152 H155 0.9800 . ? C152 H156 0.9800 . ? O13 C23 1.348(10) . ? O23 C133 1.434(10) . ? O33 C143 1.407(11) . ? O33 H331 0.8400 . ? N13 C113 1.280(11) . ? N13 C123 1.494(11) . ? C13 C23 1.392(12) . ? C13 C113 1.434(12) . ? C13 C93 1.479(13) . ? C23 C33 1.432(12) . ? C33 C43 1.303(13) . ? C33 H33 0.9500 . ? C43 C103 1.422(14) . ? C43 H43 0.9500 . ? C53 C63 1.381(15) . ? C53 C103 1.436(14) . ? C53 H53 0.9500 . ? C63 C73 1.388(15) . ? C63 H63 0.9500 . ? C73 C83 1.399(14) . ? C73 H73 0.9500 . ? C83 C93 1.416(14) . ? C83 H83 0.9500 . ? C93 C103 1.399(13) . ? C113 H113 0.9500 . ? C123 C143 1.530(13) . ? C123 C153 1.537(13) . ? C123 C133 1.539(12) . ? C133 H135 0.9900 . ? C133 H136 0.9900 . ? C143 H145 0.9900 . ? C143 H146 0.9900 . ? C153 H157 0.9800 . ? C153 H158 0.9800 . ? C153 H159 0.9800 . ? O14 C24 1.288(10) . ? O24 C134 1.420(9) . ? O34 C144 1.34(2) . ? O34 H34A 0.8400 . ? O341 C154 1.60(5) . ? O341 H341 0.8400 . ? O342 C155 1.56(6) . ? O342 H342 0.8400 . ? N14 C114 1.291(11) . ? N14 C124 1.494(11) . ? C14 C24 1.419(12) . ? C14 C114 1.443(12) . ? C14 C94 1.460(12) . ? C24 C34 1.434(12) . ? C34 C44 1.374(13) . ? C34 H34 0.9500 . ? C44 C104 1.421(12) . ? C44 H44 0.9500 . ? C54 C64 1.343(12) . ? C54 C104 1.410(12) . ? C54 H54 0.9500 . ? C64 C74 1.409(13) . ? C64 H64 0.9500 . ? C74 C84 1.387(12) . ? C74 H74 0.9500 . ? C84 C94 1.398(12) . ? C84 H84 0.9500 . ? C94 C104 1.422(12) . ? C114 H114 0.9500 . ? C124 C154 1.41(4) . ? C124 C155 1.51(6) . ? C124 C144 1.514(14) . ? C124 C134 1.534(12) . ? C124 C156 1.71(3) . ? C134 H13A 0.9900 . ? C134 H13B 0.9900 . ? C144 H14A 0.9900 . ? C144 H14B 0.9900 . ? C144 H14C 0.9800 . ? C144 H14D 0.9800 . ? C144 H14E 0.9800 . ? C154 H15A 0.9900 . ? C154 H15B 0.9900 . ? C155 H15C 0.9900 . ? C155 H15D 0.9900 . ? C156 H15E 0.9800 . ? C156 H15F 0.9800 . ? C156 H15G 0.9800 . ? O1M C1M 1.396(18) . ? O1M H1M 0.8400 . ? C1M H1M1 0.9800 . ? C1M H1M2 0.9800 . ? C1M H1M3 0.9800 . ? O2M C2M 1.27(3) . ? O2M H2M 0.8400 . ? C2M H2M1 0.9800 . ? C2M H2M2 0.9800 . ? C2M H2M3 0.9800 . ? O3M C3M 1.30(3) . ? O3M H3M 0.8400 . ? O3M1 C3M 1.46(5) . ? O3M1 H3M1 0.8400 . ? C3M H3M2 0.9800 . ? C3M H3M3 0.9800 . ? C3M H3M4 0.9800 . ? C3M H3M5 0.9800 . ? C3M H3M6 0.9800 . ? C3M H3M7 0.9800 . ? O4M C4M 1.414(14) . ? O4M H4M 0.8400 . ? C4M H4M1 0.9800 . ? C4M H4M2 0.9800 . ? C4M H4M3 0.9800 . ? O5M C5M 1.55(4) . ? O5M H5M 0.8400 . ? C5M H5M1 0.9800 . ? C5M H5M2 0.9800 . ? C5M H5M3 0.9800 . ? 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 O11 Cu1 N11 92.7(3) . . ? O11 Cu1 O21 175.4(3) . . ? N11 Cu1 O21 86.0(3) . . ? O11 Cu1 O22 92.8(3) . . ? N11 Cu1 O22 169.4(3) . . ? O21 Cu1 O22 89.1(2) . . ? O12 Cu2 N12 92.2(3) . . ? O12 Cu2 O23 95.1(3) . . ? N12 Cu2 O23 167.2(3) . . ? O12 Cu2 O22 172.5(3) . . ? N12 Cu2 O22 85.0(3) . . ? O23 Cu2 O22 88.9(2) . . ? O13 Cu3 N13 93.8(3) . . ? O13 Cu3 O23 170.5(2) . . ? N13 Cu3 O23 86.2(3) . . ? O13 Cu3 O24 95.6(3) . . ? N13 Cu3 O24 157.8(3) . . ? O23 Cu3 O24 87.8(2) . . ? O14 Cu4 N14 94.4(3) . . ? O14 Cu4 O24 175.6(3) . . ? N14 Cu4 O24 85.0(3) . . ? O14 Cu4 O21 93.5(2) . . ? N14 Cu4 O21 165.8(3) . . ? O24 Cu4 O21 88.0(2) . . ? C21 O11 Cu1 127.4(6) . . ? C131 O21 Cu1 109.1(5) . . ? C131 O21 Cu4 121.2(5) . . ? Cu1 O21 Cu4 105.4(3) . . ? C141 O31 H311 109.5 . . ? C111 N11 C121 121.4(8) . . ? C111 N11 Cu1 125.9(7) . . ? C121 N11 Cu1 112.7(5) . . ? C21 C11 C111 121.7(8) . . ? C21 C11 C91 119.8(9) . . ? C111 C11 C91 118.6(9) . . ? O11 C21 C31 116.8(9) . . ? O11 C21 C11 124.2(8) . . ? C31 C21 C11 119.0(9) . . ? C21 C31 C41 122.2(10) . . ? C21 C31 H31 118.9 . . ? C41 C31 H31 118.9 . . ? C31 C41 C101 120.4(10) . . ? C31 C41 H41 119.8 . . ? C101 C41 H41 119.8 . . ? C61 C51 C101 121.7(10) . . ? C61 C51 H51 119.2 . . ? C101 C51 H51 119.2 . . ? C51 C61 C71 118.1(10) . . ? C51 C61 H61 121.0 . . ? C71 C61 H61 121.0 . . ? C81 C71 C61 122.9(10) . . ? C81 C71 H71 118.5 . . ? C61 C71 H71 118.5 . . ? C71 C81 C91 120.0(10) . . ? C71 C81 H81 120.0 . . ? C91 C81 H81 120.0 . . ? C101 C91 C81 116.1(9) . . ? C101 C91 C11 120.0(9) . . ? C81 C91 C11 123.9(9) . . ? C91 C101 C51 121.2(10) . . ? C91 C101 C41 118.5(9) . . ? C51 C101 C41 120.3(10) . . ? N11 C111 C11 126.1(9) . . ? N11 C111 H111 116.9 . . ? C11 C111 H111 116.9 . . ? N11 C121 C131 105.7(7) . . ? N11 C121 C151 114.8(7) . . ? C131 C121 C151 108.8(8) . . ? N11 C121 C141 108.2(7) . . ? C131 C121 C141 109.3(7) . . ? C151 C121 C141 109.9(8) . . ? O21 C131 C121 110.5(7) . . ? O21 C131 H131 109.6 . . ? C121 C131 H131 109.6 . . ? O21 C131 H132 109.6 . . ? C121 C131 H132 109.6 . . ? H131 C131 H132 108.1 . . ? O31 C141 C121 110.3(8) . . ? O31 C141 H141 109.6 . . ? C121 C141 H141 109.6 . . ? O31 C141 H142 109.6 . . ? C121 C141 H142 109.6 . . ? H141 C141 H142 108.1 . . ? C121 C151 H151 109.5 . . ? C121 C151 H152 109.5 . . ? H151 C151 H152 109.5 . . ? C121 C151 H153 109.5 . . ? H151 C151 H153 109.5 . . ? H152 C151 H153 109.5 . . ? C22 O12 Cu2 125.8(6) . . ? C132 O22 Cu1 125.4(5) . . ? C132 O22 Cu2 112.4(5) . . ? Cu1 O22 Cu2 113.4(3) . . ? C142 O32 H321 109.5 . . ? C112 N12 C122 120.9(8) . . ? C112 N12 Cu2 126.3(6) . . ? C122 N12 Cu2 112.7(6) . . ? C112 C12 C22 123.6(9) . . ? C112 C12 C92 117.5(9) . . ? C22 C12 C92 118.9(9) . . ? O12 C22 C32 116.9(9) . . ? O12 C22 C12 122.6(8) . . ? C32 C22 C12 120.5(9) . . ? C42 C32 C22 121.3(10) . . ? C42 C32 H32 119.4 . . ? C22 C32 H32 119.4 . . ? C32 C42 C102 121.5(9) . . ? C32 C42 H42 119.3 . . ? C102 C42 H42 119.3 . . ? C62 C52 C102 121.1(10) . . ? C62 C52 H52 119.5 . . ? C102 C52 H52 119.5 . . ? C52 C62 C72 120.6(11) . . ? C52 C62 H62 119.7 . . ? C72 C62 H62 119.7 . . ? C62 C72 C82 119.7(11) . . ? C62 C72 H72 120.2 . . ? C82 C72 H72 120.2 . . ? C72 C82 C92 121.8(10) . . ? C72 C82 H82 119.1 . . ? C92 C82 H82 119.1 . . ? C82 C92 C102 117.6(9) . . ? C82 C92 C12 123.5(9) . . ? C102 C92 C12 118.9(9) . . ? C52 C102 C92 119.2(10) . . ? C52 C102 C42 122.0(10) . . ? C92 C102 C42 118.8(9) . . ? N12 C112 C12 124.0(9) . . ? N12 C112 H112 118.0 . . ? C12 C112 H112 118.0 . . ? C152 C122 N12 116.7(8) . . ? C152 C122 C142 111.8(9) . . ? N12 C122 C142 103.2(8) . . ? C152 C122 C132 110.4(9) . . ? N12 C122 C132 102.5(7) . . ? C142 C122 C132 111.8(8) . . ? O22 C132 C122 114.1(8) . . ? O22 C132 H133 108.7 . . ? C122 C132 H133 108.7 . . ? O22 C132 H134 108.7 . . ? C122 C132 H134 108.7 . . ? H133 C132 H134 107.6 . . ? O32 C142 C122 117.2(8) . . ? O32 C142 H143 108.0 . . ? C122 C142 H143 108.0 . . ? O32 C142 H144 108.0 . . ? C122 C142 H144 108.0 . . ? H143 C142 H144 107.2 . . ? C122 C152 H154 109.5 . . ? C122 C152 H155 109.5 . . ? H154 C152 H155 109.5 . . ? C122 C152 H156 109.5 . . ? H154 C152 H156 109.5 . . ? H155 C152 H156 109.5 . . ? C23 O13 Cu3 126.7(6) . . ? C133 O23 Cu2 125.8(5) . . ? C133 O23 Cu3 112.2(5) . . ? Cu2 O23 Cu3 114.0(3) . . ? C143 O33 H331 109.5 . . ? C113 N13 C123 120.0(7) . . ? C113 N13 Cu3 126.7(6) . . ? C123 N13 Cu3 111.0(6) . . ? C23 C13 C113 122.6(8) . . ? C23 C13 C93 118.0(8) . . ? C113 C13 C93 119.1(8) . . ? O13 C23 C13 124.4(8) . . ? O13 C23 C33 115.0(9) . . ? C13 C23 C33 120.5(9) . . ? C43 C33 C23 120.7(10) . . ? C43 C33 H33 119.7 . . ? C23 C33 H33 119.7 . . ? C33 C43 C103 123.0(10) . . ? C33 C43 H43 118.5 . . ? C103 C43 H43 118.5 . . ? C63 C53 C103 120.4(11) . . ? C63 C53 H53 119.8 . . ? C103 C53 H53 119.8 . . ? C53 C63 C73 119.0(10) . . ? C53 C63 H63 120.5 . . ? C73 C63 H63 120.5 . . ? C63 C73 C83 121.9(11) . . ? C63 C73 H73 119.1 . . ? C83 C73 H73 119.1 . . ? C73 C83 C93 119.8(11) . . ? C73 C83 H83 120.1 . . ? C93 C83 H83 120.1 . . ? C103 C93 C83 118.6(9) . . ? C103 C93 C13 118.9(9) . . ? C83 C93 C13 122.5(9) . . ? C93 C103 C43 119.0(9) . . ? C93 C103 C53 120.2(10) . . ? C43 C103 C53 120.8(10) . . ? N13 C113 C13 125.0(8) . . ? N13 C113 H113 117.5 . . ? C13 C113 H113 117.5 . . ? N13 C123 C143 106.5(7) . . ? N13 C123 C153 115.1(8) . . ? C143 C123 C153 109.2(8) . . ? N13 C123 C133 106.1(7) . . ? C143 C123 C133 111.9(8) . . ? C153 C123 C133 108.1(8) . . ? O23 C133 C123 111.4(7) . . ? O23 C133 H135 109.3 . . ? C123 C133 H135 109.3 . . ? O23 C133 H136 109.3 . . ? C123 C133 H136 109.3 . . ? H135 C133 H136 108.0 . . ? O33 C143 C123 114.3(8) . . ? O33 C143 H145 108.7 . . ? C123 C143 H145 108.7 . . ? O33 C143 H146 108.7 . . ? C123 C143 H146 108.7 . . ? H145 C143 H146 107.6 . . ? C123 C153 H157 109.5 . . ? C123 C153 H158 109.5 . . ? H157 C153 H158 109.5 . . ? C123 C153 H159 109.5 . . ? H157 C153 H159 109.5 . . ? H158 C153 H159 109.5 . . ? C24 O14 Cu4 126.5(5) . . ? C134 O24 Cu4 108.6(5) . . ? C134 O24 Cu3 122.0(5) . . ? Cu4 O24 Cu3 107.6(3) . . ? C144 O34 H34A 109.5 . . ? C154 O341 H341 109.5 . . ? C155 O342 H342 109.5 . . ? C114 N14 C124 120.9(7) . . ? C114 N14 Cu4 124.9(6) . . ? C124 N14 Cu4 114.2(6) . . ? C24 C14 C114 121.0(8) . . ? C24 C14 C94 120.2(8) . . ? C114 C14 C94 118.8(8) . . ? O14 C24 C14 126.1(8) . . ? O14 C24 C34 115.3(8) . . ? C14 C24 C34 118.5(8) . . ? C44 C34 C24 121.6(9) . . ? C44 C34 H34 119.2 . . ? C24 C34 H34 119.2 . . ? C34 C44 C104 120.8(9) . . ? C34 C44 H44 119.6 . . ? C104 C44 H44 119.6 . . ? C64 C54 C104 122.9(9) . . ? C64 C54 H54 118.5 . . ? C104 C54 H54 118.5 . . ? C54 C64 C74 118.3(9) . . ? C54 C64 H64 120.8 . . ? C74 C64 H64 120.8 . . ? C84 C74 C64 120.6(9) . . ? C84 C74 H74 119.7 . . ? C64 C74 H74 119.7 . . ? C74 C84 C94 121.8(9) . . ? C74 C84 H84 119.1 . . ? C94 C84 H84 119.1 . . ? C84 C94 C104 117.2(8) . . ? C84 C94 C14 124.2(8) . . ? C104 C94 C14 118.6(8) . . ? C54 C104 C44 120.6(8) . . ? C54 C104 C94 119.3(8) . . ? C44 C104 C94 120.1(8) . . ? N14 C114 C14 126.6(8) . . ? N14 C114 H114 116.7 . . ? C14 C114 H114 116.7 . . ? C154 C124 N14 119.2(19) . . ? N14 C124 C155 117(3) . . ? N14 C124 C144 108.8(8) . . ? C155 C124 C144 97(2) . . ? C154 C124 C134 108.9(19) . . ? N14 C124 C134 104.0(7) . . ? C155 C124 C134 120(3) . . ? C144 C124 C134 108.4(8) . . ? N14 C124 C156 108.0(14) . . ? C144 C124 C156 120.8(18) . . ? C134 C124 C156 105.6(15) . . ? O24 C134 C124 110.6(7) . . ? O24 C134 H13A 109.5 . . ? C124 C134 H13A 109.5 . . ? O24 C134 H13B 109.5 . . ? C124 C134 H13B 109.5 . . ? H13A C134 H13B 108.1 . . ? O34 C144 C124 109.0(12) . . ? O34 C144 H14A 109.9 . . ? C124 C144 H14A 109.9 . . ? O34 C144 H14B 109.9 . . ? C124 C144 H14B 109.9 . . ? H14A C144 H14B 108.3 . . ? O34 C144 H14C 118.1 . . ? C124 C144 H14C 109.5 . . ? H14B C144 H14C 100.1 . . ? C124 C144 H14D 109.5 . . ? H14A C144 H14D 100.9 . . ? H14B C144 H14D 117.9 . . ? H14C C144 H14D 109.5 . . ? O34 C144 H14E 100.8 . . ? C124 C144 H14E 109.5 . . ? H14A C144 H14E 117.2 . . ? H14C C144 H14E 109.5 . . ? H14D C144 H14E 109.5 . . ? C124 C154 O341 113(3) . . ? C124 C155 O342 96(3) . . ? C1M O1M H1M 109.5 . . ? O1M C1M H1M1 109.5 . . ? O1M C1M H1M2 109.5 . . ? H1M1 C1M H1M2 109.5 . . ? O1M C1M H1M3 109.5 . . ? H1M1 C1M H1M3 109.5 . . ? H1M2 C1M H1M3 109.5 . . ? C2M O2M H2M 109.5 . . ? O2M C2M H2M1 109.5 . . ? O2M C2M H2M2 109.5 . . ? H2M1 C2M H2M2 109.5 . . ? O2M C2M H2M3 109.5 . . ? H2M1 C2M H2M3 109.5 . . ? H2M2 C2M H2M3 109.5 . . ? C3M O3M H3M 109.5 . . ? C3M O3M1 H3M1 109.5 . . ? O3M C3M O3M1 125(3) . . ? O3M C3M H3M2 109.5 . . ? O3M1 C3M H3M2 107.8 . . ? O3M C3M H3M3 109.5 . . ? H3M2 C3M H3M3 109.5 . . ? O3M C3M H3M4 109.5 . . ? O3M1 C3M H3M4 93.9 . . ? H3M2 C3M H3M4 109.5 . . ? H3M3 C3M H3M4 109.5 . . ? O3M1 C3M H3M5 109.5 . . ? H3M2 C3M H3M5 117.0 . . ? H3M3 C3M H3M5 93.6 . . ? H3M4 C3M H3M5 116.4 . . ? O3M C3M H3M6 102.9 . . ? O3M1 C3M H3M6 109.5 . . ? H3M3 C3M H3M6 108.5 . . ? H3M4 C3M H3M6 116.8 . . ? H3M5 C3M H3M6 109.5 . . ? O3M C3M H3M7 99.4 . . ? O3M1 C3M H3M7 109.5 . . ? H3M2 C3M H3M7 103.3 . . ? H3M3 C3M H3M7 124.8 . . ? H3M5 C3M H3M7 109.5 . . ? H3M6 C3M H3M7 109.5 . . ? C4M O4M H4M 109.5 . . ? O4M C4M H4M1 109.5 . . ? O4M C4M H4M2 109.5 . . ? H4M1 C4M H4M2 109.5 . . ? O4M C4M H4M3 109.5 . . ? H4M1 C4M H4M3 109.5 . . ? H4M2 C4M H4M3 109.5 . . ? C5M O5M H5M 109.5 . . ? O5M C5M H5M1 109.5 . . ? O5M C5M H5M2 109.5 . . ? H5M1 C5M H5M2 109.5 . . ? O5M C5M H5M3 109.5 . . ? H5M1 C5M H5M3 109.5 . . ? H5M2 C5M H5M3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C111 C11 C21 O11 1.3(15) . . . . ? C91 C11 C21 O11 -179.6(9) . . . . ? C111 C11 C21 C31 -177.4(9) . . . . ? C91 C11 C21 C31 1.8(14) . . . . ? O11 C21 C31 C41 -179.2(9) . . . . ? C11 C21 C31 C41 -0.4(15) . . . . ? C21 C31 C41 C101 -0.4(16) . . . . ? C101 C51 C61 C71 1.7(15) . . . . ? C51 C61 C71 C81 -1.4(16) . . . . ? C61 C71 C81 C91 1.2(16) . . . . ? C71 C81 C91 C101 -1.2(14) . . . . ? C71 C81 C91 C11 -178.9(9) . . . . ? C21 C11 C91 C101 -2.3(14) . . . . ? C111 C11 C91 C101 176.9(9) . . . . ? C21 C11 C91 C81 175.4(9) . . . . ? C111 C11 C91 C81 -5.4(14) . . . . ? C81 C91 C101 C51 1.6(14) . . . . ? C11 C91 C101 C51 179.4(9) . . . . ? C81 C91 C101 C41 -176.4(9) . . . . ? C11 C91 C101 C41 1.4(14) . . . . ? C61 C51 C101 C91 -1.9(15) . . . . ? C61 C51 C101 C41 176.1(10) . . . . ? C31 C41 C101 C91 0.0(15) . . . . ? C31 C41 C101 C51 -178.1(9) . . . . ? C121 N11 C111 C11 179.2(8) . . . . ? Cu1 N11 C111 C11 -4.3(13) . . . . ? C21 C11 C111 N11 -4.9(15) . . . . ? C91 C11 C111 N11 175.9(8) . . . . ? C111 N11 C121 C131 151.5(8) . . . . ? Cu1 N11 C121 C131 -25.4(8) . . . . ? C111 N11 C121 C151 31.6(12) . . . . ? Cu1 N11 C121 C151 -145.2(7) . . . . ? C111 N11 C121 C141 -91.5(9) . . . . ? Cu1 N11 C121 C141 91.6(7) . . . . ? Cu1 O21 C131 C121 -40.0(8) . . . . ? Cu4 O21 C131 C121 -162.6(5) . . . . ? N11 C121 C131 O21 42.3(9) . . . . ? C151 C121 C131 O21 166.1(7) . . . . ? C141 C121 C131 O21 -74.0(9) . . . . ? N11 C121 C141 O31 66.9(10) . . . . ? C131 C121 C141 O31 -178.5(8) . . . . ? C151 C121 C141 O31 -59.2(11) . . . . ? C112 C12 C22 O12 1.4(16) . . . . ? C92 C12 C22 O12 -178.1(9) . . . . ? C112 C12 C22 C32 -176.8(9) . . . . ? C92 C12 C22 C32 3.7(14) . . . . ? O12 C22 C32 C42 -179.4(9) . . . . ? C12 C22 C32 C42 -1.1(15) . . . . ? C22 C32 C42 C102 -0.6(16) . . . . ? C102 C52 C62 C72 -1.4(17) . . . . ? C52 C62 C72 C82 0.9(18) . . . . ? C62 C72 C82 C92 -0.2(17) . . . . ? C72 C82 C92 C102 0.0(16) . . . . ? C72 C82 C92 C12 178.0(10) . . . . ? C112 C12 C92 C82 -2.2(15) . . . . ? C22 C12 C92 C82 177.3(10) . . . . ? C112 C12 C92 C102 175.8(9) . . . . ? C22 C12 C92 C102 -4.7(14) . . . . ? C62 C52 C102 C92 1.2(15) . . . . ? C62 C52 C102 C42 179.4(10) . . . . ? C82 C92 C102 C52 -0.4(14) . . . . ? C12 C92 C102 C52 -178.6(9) . . . . ? C82 C92 C102 C42 -178.7(10) . . . . ? C12 C92 C102 C42 3.1(14) . . . . ? C32 C42 C102 C52 -178.8(10) . . . . ? C32 C42 C102 C92 -0.5(15) . . . . ? C122 N12 C112 C12 178.1(9) . . . . ? Cu2 N12 C112 C12 1.7(15) . . . . ? C22 C12 C112 N12 -13.7(16) . . . . ? C92 C12 C112 N12 165.9(9) . . . . ? C112 N12 C122 C152 25.4(13) . . . . ? Cu2 N12 C122 C152 -157.8(7) . . . . ? C112 N12 C122 C142 -97.7(10) . . . . ? Cu2 N12 C122 C142 79.2(8) . . . . ? C112 N12 C122 C132 146.1(9) . . . . ? Cu2 N12 C122 C132 -37.1(8) . . . . ? Cu1 O22 C132 C122 126.1(7) . . . . ? Cu2 O22 C132 C122 -19.1(9) . . . . ? C152 C122 C132 O22 160.6(8) . . . . ? N12 C122 C132 O22 35.6(10) . . . . ? C142 C122 C132 O22 -74.3(10) . . . . ? C152 C122 C142 O32 -177.8(9) . . . . ? N12 C122 C142 O32 -51.6(11) . . . . ? C132 C122 C142 O32 57.9(12) . . . . ? C113 C13 C23 O13 -1.3(14) . . . . ? C93 C13 C23 O13 -174.8(8) . . . . ? C113 C13 C23 C33 174.8(8) . . . . ? C93 C13 C23 C33 1.4(13) . . . . ? O13 C23 C33 C43 177.4(8) . . . . ? C13 C23 C33 C43 0.9(14) . . . . ? C23 C33 C43 C103 -2.3(15) . . . . ? C103 C53 C63 C73 3.1(18) . . . . ? C53 C63 C73 C83 -4(2) . . . . ? C63 C73 C83 C93 3.5(19) . . . . ? C73 C83 C93 C103 -1.3(16) . . . . ? C73 C83 C93 C13 178.5(10) . . . . ? C23 C13 C93 C103 -2.4(13) . . . . ? C113 C13 C93 C103 -176.0(8) . . . . ? C23 C13 C93 C83 177.8(9) . . . . ? C113 C13 C93 C83 4.1(14) . . . . ? C83 C93 C103 C43 -179.0(10) . . . . ? C13 C93 C103 C43 1.1(14) . . . . ? C83 C93 C103 C53 0.2(15) . . . . ? C13 C93 C103 C53 -179.7(9) . . . . ? C33 C43 C103 C93 1.2(15) . . . . ? C33 C43 C103 C53 -178.0(10) . . . . ? C63 C53 C103 C93 -1.1(16) . . . . ? C63 C53 C103 C43 178.1(10) . . . . ? C123 N13 C113 C13 -172.0(8) . . . . ? Cu3 N13 C113 C13 -10.6(13) . . . . ? C23 C13 C113 N13 8.5(14) . . . . ? C93 C13 C113 N13 -178.2(8) . . . . ? C113 N13 C123 C143 81.0(10) . . . . ? Cu3 N13 C123 C143 -83.0(7) . . . . ? C113 N13 C123 C153 -40.2(11) . . . . ? Cu3 N13 C123 C153 155.8(7) . . . . ? C113 N13 C123 C133 -159.6(8) . . . . ? Cu3 N13 C123 C133 36.4(8) . . . . ? Cu2 O23 C133 C123 -125.2(7) . . . . ? Cu3 O23 C133 C123 21.6(9) . . . . ? N13 C123 C133 O23 -37.1(9) . . . . ? C143 C123 C133 O23 78.7(9) . . . . ? C153 C123 C133 O23 -161.0(8) . . . . ? N13 C123 C143 O33 50.3(10) . . . . ? C153 C123 C143 O33 175.2(8) . . . . ? C133 C123 C143 O33 -65.2(10) . . . . ? C114 C14 C24 O14 -1.6(14) . . . . ? C94 C14 C24 O14 179.4(8) . . . . ? C114 C14 C24 C34 -178.6(8) . . . . ? C94 C14 C24 C34 2.4(12) . . . . ? O14 C24 C34 C44 178.3(8) . . . . ? C14 C24 C34 C44 -4.4(13) . . . . ? C24 C34 C44 C104 4.0(14) . . . . ? C104 C54 C64 C74 -1.3(14) . . . . ? C54 C64 C74 C84 1.2(14) . . . . ? C64 C74 C84 C94 -0.7(14) . . . . ? C74 C84 C94 C104 0.3(13) . . . . ? C74 C84 C94 C14 179.4(9) . . . . ? C24 C14 C94 C84 -179.1(8) . . . . ? C114 C14 C94 C84 1.8(13) . . . . ? C24 C14 C94 C104 0.0(12) . . . . ? C114 C14 C94 C104 -179.1(8) . . . . ? C64 C54 C104 C44 -178.0(9) . . . . ? C64 C54 C104 C94 1.0(14) . . . . ? C34 C44 C104 C54 177.6(9) . . . . ? C34 C44 C104 C94 -1.4(14) . . . . ? C84 C94 C104 C54 -0.4(12) . . . . ? C14 C94 C104 C54 -179.6(8) . . . . ? C84 C94 C104 C44 178.6(8) . . . . ? C14 C94 C104 C44 -0.6(12) . . . . ? C124 N14 C114 C14 -178.0(8) . . . . ? Cu4 N14 C114 C14 4.0(13) . . . . ? C24 C14 C114 N14 1.8(14) . . . . ? C94 C14 C114 N14 -179.2(8) . . . . ? C114 N14 C124 C154 -34(3) . . . . ? Cu4 N14 C124 C154 145(2) . . . . ? C114 N14 C124 C155 -20(3) . . . . ? Cu4 N14 C124 C155 159(3) . . . . ? C114 N14 C124 C144 89.6(10) . . . . ? Cu4 N14 C124 C144 -92.3(8) . . . . ? C114 N14 C124 C134 -155.1(8) . . . . ? Cu4 N14 C124 C134 23.1(9) . . . . ? C114 N14 C124 C156 -43.2(19) . . . . ? C154 C124 C134 O24 -171(2) . . . . ? N14 C124 C134 O24 -43.0(10) . . . . ? C155 C124 C134 O24 -177(3) . . . . ? C144 C124 C134 O24 72.7(9) . . . . ? C156 C124 C134 O24 -156.5(16) . . . . ? C154 C124 C144 O34 51(2) . . . . ? C155 C124 C144 O34 43(3) . . . . ? C134 C124 C144 O34 168.8(11) . . . . ? C156 C124 C144 O34 47(2) . . . . ? N14 C124 C154 O341 65(3) . . . . ? C144 C124 C155 O342 177(3) . . . . ? C134 C124 C155 O342 60(4) . . . . ? C156 C124 C155 O342 4(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O31 H311 O1M 0.84 1.89 2.716(14) 169.0 . O32 H321 O11 0.84 1.81 2.653(9) 177.5 . O33 H331 O12 0.84 1.85 2.689(9) 173.0 . O1M H1M O3W 0.84 1.99 2.75(2) 150.3 3_665 O2M H2M O4W 0.84 2.35 2.90(4) 123.6 2_655 O3M H3M O1W 0.84 1.99 2.76(4) 151.9 4_566 O3M1 H3M1 O31 0.84 2.09 2.79(5) 140.2 4_566 O3M1 H3M1 O1W 0.84 2.53 3.21(6) 138.7 4_566 O4M H4M O3M 0.84 1.85 2.69(3) 175.4 . _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.78 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.223 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.146