# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 # start Validation Reply Form _vrf_CHEMW03_1 ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE:The formula weight differs from that calculated due to unlocated solvent moieties - SQUEEZE used - see _platon_squeeze_details. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C75 H83 Cd3 N3 O25' _chemical_formula_weight 1763.7 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 14.7676(18) _cell_length_b 19.2240(14) _cell_length_c 19.7451(16) _cell_angle_alpha 65.774(2) _cell_angle_beta 87.413(3) _cell_angle_gamma 67.535(2) _cell_volume 4682.3(8) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 3580 _cell_measurement_theta_min 0.816 _cell_measurement_theta_max 0.852 _exptl_crystal_description rod _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.251 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1796 _exptl_absorpt_coefficient_mu 0.740 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8220 _exptl_absorpt_correction_T_max 0.8562 _exptl_absorpt_process_details SADABS;Bruker,2000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28581 _diffrn_reflns_av_R_equivalents 0.0148 _diffrn_reflns_av_sigmaI/netI 0.0753 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 26.00 _reflns_number_total 18313 _reflns_number_gt 9634 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. The hydrogen atoms on coordinated water cannot be located in the Fourier difference map and thus were not added in the final cycles of refinement. Those hydrogens are, however, included in the reported chemical formula and derived values (reported crystal-data formula, formula weight,Dx, Mu and F(000)). ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.001 -0.064 0.457 1892 120 ' ' _platon_squeeze_details ; Because of the highly disordered solvent molecules, the PLATON/SQUEEZE route was employed to calculate the diffraction contribution from the solvent molecules, and thereby to produce a set of solvent-free diffraction intensities used for refinement. The unit cell was found to contain a void of 1892 A^3 (40.1% of the unit cell volume), holding 120 electrons. These might correspond with the removal of ~3 DMF molecules from the unit cell, i.e. 1.5 DMF per asymmetric unit. Based on the elemental analysis and TG analysis, additional 1.5 DMF might be adsorbed in the sample and were thus included in the final molecular formula. Those solvents are included in the reported chemical formula and derived values (reported crystal-data formula, formula weight, Dx, Mu and F(000)).. ; _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^)+(0.0700P)^2^+1.9900P] 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 18313 _refine_ls_number_parameters 825 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1671 _refine_ls_wR_factor_gt 0.1665 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 C1 C 0.6800(4) -0.3308(3) 0.3150(3) 0.0514(14) Uani 1 1 d . . . C2 C 0.6544(4) -0.2399(3) 0.2651(3) 0.0454(13) Uani 1 1 d . . . C3 C 0.7117(4) -0.2136(3) 0.2074(3) 0.0564(15) Uani 1 1 d . . . H3 H 0.7673 -0.2525 0.1999 0.068 Uiso 1 1 calc R . . C4 C 0.6834(4) -0.1306(3) 0.1634(3) 0.0599(18) Uani 1 1 d . . . H4 H 0.7243 -0.1124 0.1296 0.072 Uiso 1 1 calc R . . C5 C 0.5961(4) -0.0741(3) 0.1683(3) 0.0468(13) Uani 1 1 d . . . C6 C 0.5377(4) -0.0966(3) 0.2208(3) 0.0520(14) Uani 1 1 d . . . H6 H 0.4793 -0.0571 0.2244 0.062 Uiso 1 1 calc R . . C7 C 0.5678(4) -0.1815(3) 0.2696(3) 0.0503(14) Uani 1 1 d . . . H7 H 0.5283 -0.1982 0.3055 0.060 Uiso 1 1 calc R . . C8 C 0.6345(4) 0.0375(3) 0.0861(3) 0.0570(15) Uani 1 1 d . . . H8A H 0.6564 0.0150 0.0496 0.068 Uiso 1 1 calc R . . H8B H 0.6911 0.0200 0.1213 0.068 Uiso 1 1 calc R . . C9 C 0.5810(3) 0.1350(3) 0.0466(3) 0.0392(12) Uani 1 1 d . . . C10 C 0.5591(4) 0.1784(3) -0.0319(3) 0.0484(14) Uani 1 1 d . . . C11 C 0.5305(4) 0.2658(3) -0.0646(3) 0.0477(13) Uani 1 1 d . . . C12 C 0.5179(4) 0.3102(3) -0.0173(3) 0.0460(13) Uani 1 1 d . . . C13 C 0.5364(3) 0.2637(3) 0.0586(3) 0.0399(12) Uani 1 1 d . . . C14 C 0.5693(4) 0.1787(3) 0.0901(3) 0.0418(13) Uani 1 1 d . . . C15 C 0.5593(4) 0.1388(4) -0.0848(4) 0.0610(16) Uani 1 1 d . . . H15C H 0.6134 0.1394 -0.1134 0.092 Uiso 1 1 d R . . H15B H 0.4985 0.1671 -0.1182 0.092 Uiso 1 1 d R . . H15A H 0.5682 0.0822 -0.0542 0.092 Uiso 1 1 d R . . C16 C 0.4915(4) 0.4042(3) -0.0556(3) 0.0576(16) Uani 1 1 d . . . H16A H 0.5034 0.4222 -0.0195 0.086 Uiso 1 1 calc R . . H16B H 0.4230 0.4330 -0.0764 0.086 Uiso 1 1 calc R . . H16C H 0.5316 0.4161 -0.0949 0.086 Uiso 1 1 calc R . . C17 C 0.5893(4) 0.1328(3) 0.1797(3) 0.0570(16) Uani 1 1 d . . . H17A H 0.6159 0.0736 0.1956 0.085 Uiso 1 1 calc R . . H17B H 0.5284 0.1497 0.1996 0.085 Uiso 1 1 calc R . . H17C H 0.6357 0.1474 0.1974 0.085 Uiso 1 1 calc R . . C18 C 0.5142(4) 0.3140(3) -0.1497(3) 0.0495(14) Uani 1 1 d . . . H18A H 0.4971 0.2852 -0.1741 0.059 Uiso 1 1 calc R . . H18B H 0.4631 0.3696 -0.1657 0.059 Uiso 1 1 calc R . . C19 C 0.6288(4) 0.3519(4) -0.2360(3) 0.069(2) Uani 1 1 d . . . C20 C 0.5626(4) 0.3728(4) -0.2984(3) 0.0632(18) Uani 1 1 d . . . H20 H 0.5030 0.3666 -0.2917 0.076 Uiso 1 1 calc R . . C21 C 0.5894(5) 0.4019(4) -0.3678(3) 0.0663(17) Uani 1 1 d . . . H21 H 0.5439 0.4198 -0.4087 0.080 Uiso 1 1 calc R . . C22 C 0.6801(5) 0.4065(4) -0.3816(4) 0.074(2) Uani 1 1 d . . . C23 C 0.7447(5) 0.3852(4) -0.3191(4) 0.076(2) Uani 1 1 d . . . H23 H 0.8060 0.3882 -0.3254 0.091 Uiso 1 1 calc R . . C24 C 0.7156(5) 0.3594(4) -0.2475(4) 0.080(2) Uani 1 1 d . . . H24 H 0.7576 0.3470 -0.2068 0.096 Uiso 1 1 calc R . . C25 C 0.7057(5) 0.4436(4) -0.4594(4) 0.0667(18) Uani 1 1 d . . . C26 C 0.5284(4) 0.3077(3) 0.1075(3) 0.0403(12) Uani 1 1 d . . . H26A H 0.4729 0.3613 0.0872 0.048 Uiso 1 1 calc R . . H26B H 0.5190 0.2749 0.1577 0.048 Uiso 1 1 calc R . . C27 C 0.6334(4) 0.3515(3) 0.1519(3) 0.0488(14) Uani 1 1 d . . . C28 C 0.7281(4) 0.3540(4) 0.1535(3) 0.0590(16) Uani 1 1 d . . . H28 H 0.7737 0.3332 0.1254 0.071 Uiso 1 1 calc R . . C29 C 0.7534(4) 0.3874(4) 0.1970(3) 0.0599(16) Uani 1 1 d . . . H29 H 0.8151 0.3898 0.1972 0.072 Uiso 1 1 calc R . . C30 C 0.6842(4) 0.4174(3) 0.2406(3) 0.0518(14) Uani 1 1 d . . . C31 C 0.5930(4) 0.4146(3) 0.2391(3) 0.0445(13) Uani 1 1 d . . . H31 H 0.5479 0.4348 0.2678 0.053 Uiso 1 1 calc R . . C32 C 0.5663(4) 0.3821(3) 0.1951(3) 0.0461(13) Uani 1 1 d . . . H32 H 0.5039 0.3810 0.1947 0.055 Uiso 1 1 calc R . . C33 C 0.7042(5) 0.4502(4) 0.2907(3) 0.0567(16) Uani 1 1 d . . . C34 C 1.1950(5) 0.1870(4) 0.5026(3) 0.0608(16) Uani 1 1 d . . . C35 C 1.1026(5) 0.1804(4) 0.5208(3) 0.0662(17) Uani 1 1 d . . . H35 H 1.0502 0.2005 0.4841 0.079 Uiso 1 1 calc R . . C36 C 1.0963(5) 0.1433(4) 0.5947(3) 0.0676(18) Uani 1 1 d . . . H36 H 1.0365 0.1410 0.6097 0.081 Uiso 1 1 calc R . . C37 C 1.1792(4) 0.1076(3) 0.6499(3) 0.0466(14) Uani 1 1 d . . . C38 C 1.2602(4) 0.1222(3) 0.6292(3) 0.0477(14) Uani 1 1 d . . . H38 H 1.3104 0.1074 0.6655 0.057 Uiso 1 1 calc R . . C39 C 1.2699(4) 0.1597(4) 0.5526(3) 0.0596(17) Uani 1 1 d . . . H39 H 1.3286 0.1650 0.5380 0.072 Uiso 1 1 calc R . . C40 C 1.2028(5) 0.2280(4) 0.4205(4) 0.071(2) Uani 1 1 d . . . C41 C 1.0723(4) 0.0733(4) 0.7445(3) 0.0555(16) Uani 1 1 d . . . H41A H 1.0514 0.0458 0.7205 0.067 Uiso 1 1 calc R . . H41B H 1.0225 0.1291 0.7308 0.067 Uiso 1 1 calc R . . C42 C 1.0995(3) 0.0201(3) 0.8334(3) 0.0458(14) Uani 1 1 d . . . C43 C 1.0901(4) 0.0642(3) 0.8765(3) 0.0474(14) Uani 1 1 d . . . C44 C 1.1104(3) 0.0187(3) 0.9554(3) 0.0446(13) Uani 1 1 d . . . C45 C 1.1427(3) -0.0657(3) 0.9903(3) 0.0350(11) Uani 1 1 d . . . C46 C 1.1541(4) -0.1079(3) 0.9450(3) 0.0475(14) Uani 1 1 d . . . C47 C 1.1309(4) -0.0653(3) 0.8642(3) 0.0516(14) Uani 1 1 d . . . C48 C 1.1373(5) -0.1188(4) 0.8218(4) 0.077(2) Uani 1 1 d . . . H48D H 1.1088 -0.0831 0.7706 0.115 Uiso 1 1 calc R . . H48E H 1.1018 -0.1535 0.8449 0.115 Uiso 1 1 calc R . . H48F H 1.2053 -0.1531 0.8238 0.115 Uiso 1 1 calc R . . C49 C 1.0615(4) 0.1587(3) 0.8473(3) 0.0567(16) Uani 1 1 d . . . H49A H 1.0558 0.1834 0.7936 0.085 Uiso 1 1 calc R . . H49B H 1.1116 0.1679 0.8674 0.085 Uiso 1 1 calc R . . H49C H 0.9994 0.1834 0.8628 0.085 Uiso 1 1 calc R . . C50 C 1.1708(4) -0.1153(4) 1.0737(3) 0.0501(14) Uani 1 1 d . . . H50A H 1.2367 -0.1231 1.0873 0.075 Uiso 1 1 calc R . . H50B H 1.1679 -0.1685 1.0882 0.075 Uiso 1 1 calc R . . H50C H 1.1257 -0.0859 1.0988 0.075 Uiso 1 1 calc R . . C51 C 1.0950(4) 0.0659(4) 1.0040(3) 0.0559(15) Uani 1 1 d . . . H51A H 1.0471 0.1227 0.9776 0.067 Uiso 1 1 calc R . . H51B H 1.0720 0.0389 1.0504 0.067 Uiso 1 1 calc R . . C52 C 1.1994(4) 0.0971(4) 1.0657(3) 0.0506(14) Uani 1 1 d . . . C53 C 1.1209(4) 0.1398(3) 1.0944(3) 0.0518(14) Uani 1 1 d . . . H53 H 1.0572 0.1461 1.0826 0.062 Uiso 1 1 calc R . . C54 C 1.1377(3) 0.1730(3) 1.1408(3) 0.0469(14) Uani 1 1 d . . . H54 H 1.0852 0.2016 1.1600 0.056 Uiso 1 1 calc R . . C55 C 1.2330(4) 0.1636(4) 1.1585(3) 0.0561(15) Uani 1 1 d . . . C56 C 1.3114(4) 0.1210(3) 1.1298(3) 0.0546(15) Uani 1 1 d . . . H56 H 1.3752 0.1147 1.1416 0.066 Uiso 1 1 calc R . . C57 C 1.2946(4) 0.0877(3) 1.0834(4) 0.0621(17) Uani 1 1 d . . . H57 H 1.3471 0.0592 1.0642 0.075 Uiso 1 1 calc R . . C58 C 1.2565(5) 0.2025(4) 1.2038(3) 0.0592(16) Uani 1 1 d . . . C59 C 1.2067(4) -0.2041(3) 0.9756(3) 0.0539(15) Uani 1 1 d . . . H59A H 1.2273 -0.2209 0.9354 0.065 Uiso 1 1 calc R . . H59B H 1.2639 -0.2260 1.0119 0.065 Uiso 1 1 calc R . . C60 C 1.1621(4) -0.3151(3) 1.0537(3) 0.0519(14) Uani 1 1 d . . . C61 C 1.2550(4) -0.3755(3) 1.0559(3) 0.0609(17) Uani 1 1 d . . . H61 H 1.2992 -0.3573 1.0261 0.073 Uiso 1 1 calc R . . C62 C 1.2837(4) -0.4563(3) 1.0972(3) 0.0512(14) Uani 1 1 d . . . H62 H 1.3444 -0.4937 1.0939 0.061 Uiso 1 1 calc R . . C63 C 1.2179(4) -0.4856(3) 1.1482(3) 0.0544(15) Uani 1 1 d . . . C64 C 1.1257(4) -0.4300(3) 1.1505(4) 0.0670(19) Uani 1 1 d . . . H64 H 1.0814 -0.4469 1.1812 0.080 Uiso 1 1 calc R . . C65 C 1.1033(4) -0.3425(4) 1.1009(4) 0.0690(19) Uani 1 1 d . . . H65 H 1.0433 -0.3030 1.1026 0.083 Uiso 1 1 calc R . . C66 C 1.2509(5) -0.5750(4) 1.2020(3) 0.0563(15) Uani 1 1 d . . . Cd1 Cd 0.73802(3) 0.50307(3) 0.39558(3) 0.05735(14) Uani 1 1 d . . . Cd2 Cd 0.96269(4) 0.34933(3) 0.33300(3) 0.07494(18) Uani 1 1 d . . . Cd3 Cd 1.31676(3) 0.26225(3) 0.29095(3) 0.06706(16) Uani 1 1 d . . . O4W O 1.4826(3) 0.1658(2) 0.3460(2) 0.0671(12) Uani 1 1 d . . . O1 O 0.7693(3) -0.3835(2) 0.3139(2) 0.0597(11) Uani 1 1 d . . . O2 O 0.6295(3) -0.3529(2) 0.3573(2) 0.0584(11) Uani 1 1 d . . . O3 O 0.5588(3) 0.0100(2) 0.1254(2) 0.0529(10) Uani 1 1 d . . . O4 O 0.6448(3) 0.4709(2) -0.5141(2) 0.0622(11) Uani 1 1 d . . . O5 O 0.7924(3) 0.4364(2) -0.4659(2) 0.0574(10) Uani 1 1 d . . . O6 O 0.6141(3) 0.3158(2) -0.1646(2) 0.0611(11) Uani 1 1 d . . . O7 O 0.7996(3) 0.4376(2) 0.2954(2) 0.0532(10) Uani 1 1 d . . . O8 O 0.6514(3) 0.4781(2) 0.3291(2) 0.0574(10) Uani 1 1 d . . . O9 O 0.6202(2) 0.3180(2) 0.1088(2) 0.0496(9) Uani 1 1 d . . . O10 O 1.1274(3) 0.2746(3) 0.3696(2) 0.0685(12) Uani 1 1 d . . . O11 O 1.2850(3) 0.2108(2) 0.4027(2) 0.0724(13) Uani 1 1 d . . . O12 O 1.1735(3) 0.0726(2) 0.72822(19) 0.0587(11) Uani 1 1 d . . . O13 O 1.1780(3) 0.2506(2) 1.2215(2) 0.0643(11) Uani 1 1 d . . . O14 O 1.3385(4) 0.1846(3) 1.2258(3) 0.0807(14) Uani 1 1 d . . . O15 O 1.1923(2) 0.0640(2) 1.0188(2) 0.0524(10) Uani 1 1 d . . . O16 O 1.3366(3) -0.6256(2) 1.1939(2) 0.0671(12) Uani 1 1 d . . . O17 O 1.1973(3) -0.5996(2) 1.2442(2) 0.0725(13) Uani 1 1 d . . . O18 O 1.1311(2) -0.2318(2) 1.0103(2) 0.0493(10) Uani 1 1 d . . . O1W O 0.9229(3) 0.4174(3) 0.4254(2) 0.0748(13) Uani 1 1 d . . . O2W O 0.9871(3) 0.4219(3) 0.2338(3) 0.0803(14) Uani 1 1 d . . . O3W O 0.9446(4) 0.2710(3) 0.2743(3) 0.0927(15) 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 C1 0.056(3) 0.050(3) 0.051(4) -0.022(3) 0.009(3) -0.024(3) C2 0.049(3) 0.045(3) 0.051(3) -0.023(3) 0.007(3) -0.026(2) C3 0.064(4) 0.043(3) 0.062(4) -0.022(3) 0.016(3) -0.021(3) C4 0.049(3) 0.039(3) 0.061(4) 0.001(3) 0.025(3) -0.013(2) C5 0.056(3) 0.047(3) 0.039(3) -0.018(3) 0.003(3) -0.023(3) C6 0.044(3) 0.055(3) 0.052(4) -0.016(3) -0.001(3) -0.022(3) C7 0.056(3) 0.048(3) 0.036(3) -0.013(3) 0.002(2) -0.013(3) C8 0.078(4) 0.050(3) 0.057(4) -0.031(3) 0.026(3) -0.033(3) C9 0.037(3) 0.035(3) 0.044(3) -0.013(2) 0.004(2) -0.017(2) C10 0.046(3) 0.050(3) 0.046(3) -0.017(3) 0.005(2) -0.018(2) C11 0.063(3) 0.054(3) 0.028(3) -0.015(3) 0.008(2) -0.027(3) C12 0.044(3) 0.038(3) 0.046(3) -0.014(3) 0.007(2) -0.009(2) C13 0.044(3) 0.046(3) 0.038(3) -0.025(2) 0.007(2) -0.018(2) C14 0.054(3) 0.040(3) 0.029(3) -0.016(2) 0.024(2) -0.018(2) C15 0.049(3) 0.074(4) 0.079(4) -0.053(4) 0.023(3) -0.023(3) C16 0.050(3) 0.051(3) 0.064(4) -0.015(3) -0.004(3) -0.020(3) C17 0.062(4) 0.052(3) 0.050(4) -0.016(3) -0.015(3) -0.020(3) C18 0.046(3) 0.053(3) 0.042(3) -0.011(3) -0.008(2) -0.020(2) C19 0.049(3) 0.061(4) 0.046(4) 0.020(3) -0.006(3) -0.017(3) C20 0.054(3) 0.065(4) 0.041(4) -0.003(3) 0.004(3) -0.014(3) C21 0.083(5) 0.078(4) 0.037(3) -0.022(3) 0.012(3) -0.034(4) C22 0.058(4) 0.076(4) 0.051(4) 0.005(3) 0.000(3) -0.023(3) C23 0.093(5) 0.084(5) 0.051(4) -0.015(4) 0.006(4) -0.049(4) C24 0.079(5) 0.092(5) 0.043(4) 0.006(3) -0.008(3) -0.045(4) C25 0.065(4) 0.089(5) 0.042(4) -0.014(3) 0.011(3) -0.042(4) C26 0.051(3) 0.038(3) 0.037(3) -0.027(2) 0.015(2) -0.013(2) C27 0.066(4) 0.045(3) 0.037(3) -0.022(3) 0.017(3) -0.021(3) C28 0.042(3) 0.084(4) 0.065(4) -0.047(4) 0.017(3) -0.023(3) C29 0.045(3) 0.076(4) 0.070(4) -0.044(4) 0.000(3) -0.022(3) C30 0.057(4) 0.059(3) 0.036(3) -0.017(3) -0.007(3) -0.020(3) C31 0.039(3) 0.046(3) 0.039(3) -0.017(2) 0.003(2) -0.009(2) C32 0.040(3) 0.048(3) 0.050(3) -0.023(3) 0.016(2) -0.016(2) C33 0.064(4) 0.057(4) 0.033(3) -0.010(3) -0.011(3) -0.016(3) C34 0.077(4) 0.061(4) 0.040(3) -0.024(3) 0.014(3) -0.021(3) C35 0.076(4) 0.074(4) 0.040(4) -0.022(3) 0.012(3) -0.024(3) C36 0.083(4) 0.076(4) 0.040(4) -0.005(3) -0.001(3) -0.049(4) C37 0.044(3) 0.052(3) 0.033(3) -0.012(2) 0.009(2) -0.015(2) C38 0.032(3) 0.070(4) 0.062(4) -0.044(3) 0.018(3) -0.025(2) C39 0.049(3) 0.065(4) 0.055(4) -0.015(3) 0.018(3) -0.026(3) C40 0.062(4) 0.061(4) 0.058(4) -0.001(3) 0.018(3) -0.019(3) C41 0.057(3) 0.066(4) 0.036(3) -0.012(3) 0.022(3) -0.030(3) C42 0.032(3) 0.051(3) 0.045(3) -0.015(3) 0.017(2) -0.014(2) C43 0.040(3) 0.046(3) 0.045(3) -0.005(3) 0.007(2) -0.021(2) C44 0.038(3) 0.049(3) 0.050(3) -0.026(3) 0.009(2) -0.015(2) C45 0.031(2) 0.045(3) 0.027(3) -0.009(2) 0.011(2) -0.021(2) C46 0.041(3) 0.043(3) 0.047(3) -0.011(3) 0.005(2) -0.014(2) C47 0.054(3) 0.053(3) 0.051(4) -0.020(3) 0.016(3) -0.028(3) C48 0.088(5) 0.076(4) 0.054(4) -0.042(4) 0.007(3) -0.005(4) C49 0.060(3) 0.050(3) 0.046(3) -0.004(3) 0.019(3) -0.027(3) C50 0.038(3) 0.072(4) 0.037(3) -0.031(3) 0.008(2) -0.011(2) C51 0.052(3) 0.056(3) 0.067(4) -0.038(3) 0.004(3) -0.016(3) C52 0.057(4) 0.063(3) 0.054(4) -0.036(3) 0.019(3) -0.035(3) C53 0.040(3) 0.066(4) 0.049(3) -0.026(3) 0.010(3) -0.020(3) C54 0.031(3) 0.052(3) 0.059(4) -0.024(3) 0.011(2) -0.018(2) C55 0.043(3) 0.074(4) 0.059(4) -0.043(3) 0.012(3) -0.016(3) C56 0.039(3) 0.061(3) 0.075(4) -0.038(3) 0.015(3) -0.022(3) C57 0.037(3) 0.058(3) 0.103(5) -0.045(4) 0.013(3) -0.020(3) C58 0.073(4) 0.071(4) 0.039(3) -0.023(3) 0.002(3) -0.034(4) C59 0.040(3) 0.047(3) 0.067(4) -0.016(3) 0.012(3) -0.019(2) C60 0.058(3) 0.045(3) 0.057(4) -0.024(3) 0.020(3) -0.025(3) C61 0.065(4) 0.046(3) 0.057(4) -0.007(3) 0.016(3) -0.023(3) C62 0.061(3) 0.043(3) 0.055(4) -0.019(3) 0.021(3) -0.029(3) C63 0.073(4) 0.042(3) 0.051(4) -0.023(3) 0.023(3) -0.025(3) C64 0.058(4) 0.040(3) 0.086(5) -0.018(3) 0.030(3) -0.015(3) C65 0.046(3) 0.058(4) 0.094(5) -0.025(4) 0.021(3) -0.022(3) C66 0.077(4) 0.062(4) 0.052(4) -0.032(3) 0.020(3) -0.042(3) Cd1 0.0649(3) 0.0501(2) 0.0576(3) -0.0182(2) 0.0102(2) -0.0288(2) Cd2 0.0689(3) 0.0511(3) 0.0771(4) -0.0127(2) 0.0125(3) -0.0123(2) Cd3 0.0633(3) 0.0587(3) 0.0597(3) -0.0178(2) 0.0126(2) -0.0134(2) O4W 0.063(2) 0.059(2) 0.060(3) -0.018(2) 0.013(2) -0.0134(19) O1 0.059(2) 0.0368(19) 0.064(3) -0.0075(18) 0.0061(19) -0.0144(17) O2 0.052(2) 0.056(2) 0.064(3) -0.017(2) 0.016(2) -0.0285(19) O3 0.056(2) 0.0358(19) 0.063(3) -0.0167(18) 0.0141(19) -0.0195(16) O4 0.061(2) 0.052(2) 0.054(3) -0.011(2) 0.015(2) -0.0164(19) O5 0.065(3) 0.050(2) 0.058(3) -0.0182(19) 0.010(2) -0.0288(19) O6 0.066(2) 0.068(2) 0.039(2) -0.0036(19) -0.0016(18) -0.036(2) O7 0.063(3) 0.053(2) 0.044(2) -0.0176(18) 0.0052(18) -0.0277(19) O8 0.065(3) 0.050(2) 0.058(3) -0.018(2) 0.010(2) -0.0288(19) O9 0.045(2) 0.066(2) 0.052(2) -0.039(2) 0.0152(17) -0.0223(17) O10 0.053(2) 0.074(3) 0.064(3) -0.016(2) 0.005(2) -0.025(2) O11 0.072(3) 0.059(3) 0.060(3) -0.004(2) 0.023(2) -0.025(2) O12 0.065(2) 0.068(2) 0.0241(19) -0.0020(18) 0.0059(17) -0.0278(19) O13 0.094(3) 0.062(3) 0.044(2) -0.029(2) 0.020(2) -0.032(2) O14 0.081(3) 0.068(3) 0.067(3) -0.015(2) -0.018(3) -0.014(2) O15 0.045(2) 0.057(2) 0.062(3) -0.034(2) 0.0154(18) -0.0182(17) O16 0.063(3) 0.059(2) 0.060(3) -0.018(2) 0.013(2) -0.013(2) O17 0.067(3) 0.053(2) 0.064(3) 0.003(2) 0.018(2) -0.022(2) O18 0.0300(17) 0.045(2) 0.068(3) -0.0207(19) 0.0161(17) -0.0145(15) O1W 0.059(2) 0.078(3) 0.063(3) -0.017(2) 0.008(2) -0.017(2) O2W 0.082(3) 0.078(3) 0.073(3) -0.024(3) 0.024(2) -0.034(2) O3W 0.091(3) 0.079(3) 0.085(4) -0.030(3) 0.016(3) -0.018(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. Because of disorder, the Hs of coordinated water were not located. ; 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 C1 O2 1.154(6) . ? C1 O1 1.327(6) . ? C1 C2 1.512(7) . ? C1 Cd1 2.707(5) 1_545 ? C2 C7 1.370(7) . ? C2 C3 1.426(7) . ? C3 C4 1.364(7) . ? C3 H3 0.9300 . ? C4 C5 1.364(7) . ? C4 H4 0.9300 . ? C5 C6 1.357(7) . ? C5 O3 1.368(6) . ? C6 C7 1.407(7) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 O3 1.471(6) . ? C8 C9 1.572(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C14 1.393(7) . ? C9 C10 1.408(7) . ? C10 C11 1.417(7) . ? C10 C15 1.525(8) . ? C11 C12 1.466(8) . ? C11 C18 1.526(7) . ? C12 C13 1.368(7) . ? C12 C16 1.534(7) . ? C13 C14 1.371(7) . ? C13 C26 1.499(7) . ? C14 C17 1.600(7) . ? C15 H15C 0.9598 . ? C15 H15B 0.9601 . ? C15 H15A 0.9604 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 O6 1.502(6) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 O6 1.342(7) . ? C19 C24 1.343(8) . ? C19 C20 1.427(8) . ? C20 C21 1.355(8) . ? C20 H20 0.9300 . ? C21 C22 1.384(8) . ? C21 H21 0.9300 . ? C22 C23 1.412(9) . ? C22 C25 1.505(8) . ? C23 C24 1.400(9) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 O4 1.229(7) . ? C25 O5 1.241(7) . ? C25 Cd1 2.709(6) 1_554 ? C26 O9 1.446(6) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 O9 1.316(6) . ? C27 C32 1.396(7) . ? C27 C28 1.419(8) . ? C28 C29 1.399(8) . ? C28 H28 0.9300 . ? C29 C30 1.411(8) . ? C29 H29 0.9300 . ? C30 C31 1.370(7) . ? C30 C33 1.465(8) . ? C31 C32 1.402(8) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 O8 1.198(7) . ? C33 O7 1.336(7) . ? C34 C39 1.305(8) . ? C34 C35 1.434(9) . ? C34 C40 1.507(8) . ? C35 C36 1.353(8) . ? C35 H35 0.9300 . ? C36 C37 1.423(8) . ? C36 H36 0.9300 . ? C37 C38 1.339(7) . ? C37 O12 1.424(6) . ? C38 C39 1.411(8) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 O11 1.206(7) . ? C40 O10 1.285(7) . ? C41 O12 1.512(6) . ? C41 C42 1.602(7) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C47 1.380(7) . ? C42 C43 1.398(8) . ? C43 C44 1.416(7) . ? C43 C49 1.545(7) . ? C44 C45 1.362(7) . ? C44 C51 1.526(8) . ? C45 C46 1.402(7) . ? C45 C50 1.505(6) . ? C46 C47 1.447(8) . ? C46 C59 1.555(7) . ? C47 C48 1.547(8) . ? C48 H48D 0.9600 . ? C48 H48E 0.9600 . ? C48 H48F 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 O15 1.464(6) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 O15 1.348(6) . ? C52 C53 1.390(7) . ? C52 C57 1.390(7) . ? C53 C54 1.390(8) . ? C53 H53 0.9300 . ? C54 C55 1.390(7) . ? C54 H54 0.9300 . ? C55 C56 1.390(7) . ? C55 C58 1.502(9) . ? C56 C57 1.390(8) . ? C56 H56 0.9300 . ? C57 H57 0.9300 . ? C58 O14 1.175(7) . ? C58 O13 1.315(7) . ? C58 Cd3 2.759(7) 1_556 ? C59 O18 1.444(6) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 C65 1.332(7) . ? C60 O18 1.362(6) . ? C60 C61 1.407(7) . ? C61 C62 1.321(7) . ? C61 H61 0.9300 . ? C62 C63 1.464(7) . ? C62 H62 0.9300 . ? C63 C64 1.386(7) . ? C63 C66 1.492(7) . ? C64 C65 1.467(8) . ? C64 H64 0.9300 . ? C65 H65 0.9300 . ? C66 O17 1.204(6) . ? C66 O16 1.318(7) . ? C66 Cd3 2.672(6) 1_546 ? Cd1 O8 2.175(4) . ? Cd1 O4 2.232(4) 1_556 ? Cd1 O1 2.321(3) 1_565 ? Cd1 O2 2.410(4) 1_565 ? Cd1 O5 2.511(4) 1_556 ? Cd1 O1W 2.536(4) . ? Cd1 C1 2.707(5) 1_565 ? Cd1 C25 2.710(6) 1_556 ? Cd2 O2W 1.998(4) . ? Cd2 O10 2.267(4) . ? Cd2 O7 2.287(4) . ? Cd2 O3W 2.333(6) . ? Cd2 O1W 2.581(5) . ? Cd3 O11 2.131(4) . ? Cd3 O14 2.271(5) 1_554 ? Cd3 O16 2.334(4) 1_564 ? Cd3 O17 2.361(4) 1_564 ? Cd3 O4W 2.394(4) . ? Cd3 O13 2.643(4) 1_554 ? Cd3 C66 2.672(6) 1_564 ? Cd3 C58 2.759(7) 1_554 ? O1 Cd1 2.321(3) 1_545 ? O2 Cd1 2.410(4) 1_545 ? O4 Cd1 2.232(4) 1_554 ? O5 Cd1 2.511(4) 1_554 ? O13 Cd3 2.643(4) 1_556 ? O14 Cd3 2.271(5) 1_556 ? O16 Cd3 2.334(4) 1_546 ? O17 Cd3 2.361(4) 1_546 ? 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 O2 C1 O1 121.1(5) . . ? O2 C1 C2 122.3(5) . . ? O1 C1 C2 116.2(5) . . ? O2 C1 Cd1 62.8(3) . 1_545 ? O1 C1 Cd1 59.0(2) . 1_545 ? C2 C1 Cd1 174.6(4) . 1_545 ? C7 C2 C3 118.7(5) . . ? C7 C2 C1 119.1(5) . . ? C3 C2 C1 121.8(5) . . ? C4 C3 C2 118.9(5) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C5 C4 C3 120.8(5) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C6 C5 C4 121.9(5) . . ? C6 C5 O3 112.2(5) . . ? C4 C5 O3 125.9(5) . . ? C5 C6 C7 118.2(5) . . ? C5 C6 H6 120.9 . . ? C7 C6 H6 120.9 . . ? C2 C7 C6 121.1(5) . . ? C2 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? O3 C8 C9 104.4(4) . . ? O3 C8 H8A 110.9 . . ? C9 C8 H8A 110.9 . . ? O3 C8 H8B 110.9 . . ? C9 C8 H8B 110.9 . . ? H8A C8 H8B 108.9 . . ? C14 C9 C10 119.7(4) . . ? C14 C9 C8 118.1(4) . . ? C10 C9 C8 121.4(5) . . ? C9 C10 C11 118.4(5) . . ? C9 C10 C15 124.5(5) . . ? C11 C10 C15 117.0(5) . . ? C10 C11 C12 120.6(5) . . ? C10 C11 C18 119.8(5) . . ? C12 C11 C18 119.6(5) . . ? C13 C12 C11 117.2(4) . . ? C13 C12 C16 124.3(5) . . ? C11 C12 C16 118.4(5) . . ? C12 C13 C14 122.2(5) . . ? C12 C13 C26 117.8(4) . . ? C14 C13 C26 119.8(5) . . ? C13 C14 C9 121.8(4) . . ? C13 C14 C17 116.4(5) . . ? C9 C14 C17 121.8(4) . . ? C10 C15 H15C 109.3 . . ? C10 C15 H15B 111.9 . . ? H15C C15 H15B 109.4 . . ? C10 C15 H15A 107.1 . . ? H15C C15 H15A 109.5 . . ? H15B C15 H15A 109.5 . . ? C12 C16 H16A 109.5 . . ? C12 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C12 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O6 C18 C11 101.3(4) . . ? O6 C18 H18A 111.5 . . ? C11 C18 H18A 111.5 . . ? O6 C18 H18B 111.5 . . ? C11 C18 H18B 111.5 . . ? H18A C18 H18B 109.3 . . ? O6 C19 C24 117.0(5) . . ? O6 C19 C20 123.2(5) . . ? C24 C19 C20 119.4(6) . . ? C21 C20 C19 118.1(6) . . ? C21 C20 H20 121.0 . . ? C19 C20 H20 121.0 . . ? C20 C21 C22 124.1(6) . . ? C20 C21 H21 118.0 . . ? C22 C21 H21 118.0 . . ? C21 C22 C23 116.8(6) . . ? C21 C22 C25 122.9(6) . . ? C23 C22 C25 119.7(6) . . ? C24 C23 C22 119.4(6) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C19 C24 C23 122.0(6) . . ? C19 C24 H24 119.0 . . ? C23 C24 H24 119.0 . . ? O4 C25 O5 121.8(6) . . ? O4 C25 C22 119.8(6) . . ? O5 C25 C22 117.8(6) . . ? O4 C25 Cd1 54.5(3) . 1_554 ? O5 C25 Cd1 67.5(3) . 1_554 ? C22 C25 Cd1 173.1(5) . 1_554 ? O9 C26 C13 106.3(4) . . ? O9 C26 H26A 110.5 . . ? C13 C26 H26A 110.5 . . ? O9 C26 H26B 110.5 . . ? C13 C26 H26B 110.5 . . ? H26A C26 H26B 108.7 . . ? O9 C27 C32 127.2(5) . . ? O9 C27 C28 114.0(5) . . ? C32 C27 C28 118.9(5) . . ? C29 C28 C27 120.7(5) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C28 C29 C30 119.2(5) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? C31 C30 C29 120.0(5) . . ? C31 C30 C33 116.0(6) . . ? C29 C30 C33 123.9(6) . . ? C30 C31 C32 121.4(5) . . ? C30 C31 H31 119.3 . . ? C32 C31 H31 119.3 . . ? C27 C32 C31 119.9(5) . . ? C27 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? O8 C33 O7 120.3(6) . . ? O8 C33 C30 129.7(6) . . ? O7 C33 C30 109.6(6) . . ? C39 C34 C35 123.7(6) . . ? C39 C34 C40 120.0(6) . . ? C35 C34 C40 116.3(6) . . ? C36 C35 C34 115.9(6) . . ? C36 C35 H35 122.1 . . ? C34 C35 H35 122.1 . . ? C35 C36 C37 121.4(6) . . ? C35 C36 H36 119.3 . . ? C37 C36 H36 119.3 . . ? C38 C37 C36 118.9(5) . . ? C38 C37 O12 116.9(5) . . ? C36 C37 O12 122.8(5) . . ? C37 C38 C39 120.5(5) . . ? C37 C38 H38 119.7 . . ? C39 C38 H38 119.7 . . ? C34 C39 C38 118.8(5) . . ? C34 C39 H39 120.6 . . ? C38 C39 H39 120.6 . . ? O11 C40 O10 119.8(6) . . ? O11 C40 C34 116.6(6) . . ? O10 C40 C34 123.3(6) . . ? O12 C41 C42 97.0(4) . . ? O12 C41 H41A 112.4 . . ? C42 C41 H41A 112.4 . . ? O12 C41 H41B 112.4 . . ? C42 C41 H41B 112.4 . . ? H41A C41 H41B 109.9 . . ? C47 C42 C43 122.9(5) . . ? C47 C42 C41 120.1(5) . . ? C43 C42 C41 117.0(5) . . ? C42 C43 C44 117.9(5) . . ? C42 C43 C49 126.8(5) . . ? C44 C43 C49 115.3(5) . . ? C45 C44 C43 122.9(5) . . ? C45 C44 C51 118.2(5) . . ? C43 C44 C51 118.9(5) . . ? C44 C45 C46 117.5(4) . . ? C44 C45 C50 123.5(5) . . ? C46 C45 C50 119.0(4) . . ? C45 C46 C47 122.7(5) . . ? C45 C46 C59 122.8(5) . . ? C47 C46 C59 113.9(5) . . ? C42 C47 C46 116.1(5) . . ? C42 C47 C48 126.6(5) . . ? C46 C47 C48 117.1(5) . . ? C47 C48 H48D 109.5 . . ? C47 C48 H48E 109.5 . . ? H48D C48 H48E 109.5 . . ? C47 C48 H48F 109.5 . . ? H48D C48 H48F 109.5 . . ? H48E C48 H48F 109.5 . . ? C43 C49 H49A 109.5 . . ? C43 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C43 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C45 C50 H50A 109.5 . . ? C45 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C45 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? O15 C51 C44 105.0(4) . . ? O15 C51 H51A 110.7 . . ? C44 C51 H51A 110.7 . . ? O15 C51 H51B 110.7 . . ? C44 C51 H51B 110.7 . . ? H51A C51 H51B 108.8 . . ? O15 C52 C53 125.6(5) . . ? O15 C52 C57 114.4(5) . . ? C53 C52 C57 120.0(6) . . ? C54 C53 C52 120.0(5) . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? C53 C54 C55 120.0(5) . . ? C53 C54 H54 120.0 . . ? C55 C54 H54 120.0 . . ? C56 C55 C54 120.0(6) . . ? C56 C55 C58 116.5(5) . . ? C54 C55 C58 123.3(5) . . ? C55 C56 C57 120.0(5) . . ? C55 C56 H56 120.0 . . ? C57 C56 H56 120.0 . . ? C56 C57 C52 120.0(6) . . ? C56 C57 H57 120.0 . . ? C52 C57 H57 120.0 . . ? O14 C58 O13 124.6(6) . . ? O14 C58 C55 121.2(6) . . ? O13 C58 C55 113.8(6) . . ? O14 C58 Cd3 53.7(4) . 1_556 ? O13 C58 Cd3 71.0(3) . 1_556 ? C55 C58 Cd3 174.7(5) . 1_556 ? O18 C59 C46 103.0(4) . . ? O18 C59 H59A 111.2 . . ? C46 C59 H59A 111.2 . . ? O18 C59 H59B 111.2 . . ? C46 C59 H59B 111.2 . . ? H59A C59 H59B 109.1 . . ? C65 C60 O18 118.7(5) . . ? C65 C60 C61 116.2(5) . . ? O18 C60 C61 125.0(5) . . ? C62 C61 C60 124.6(5) . . ? C62 C61 H61 117.7 . . ? C60 C61 H61 117.7 . . ? C61 C62 C63 118.5(5) . . ? C61 C62 H62 120.8 . . ? C63 C62 H62 120.8 . . ? C64 C63 C62 120.5(5) . . ? C64 C63 C66 118.6(5) . . ? C62 C63 C66 120.7(5) . . ? C63 C64 C65 114.9(5) . . ? C63 C64 H64 122.6 . . ? C65 C64 H64 122.6 . . ? C60 C65 C64 125.1(5) . . ? C60 C65 H65 117.4 . . ? C64 C65 H65 117.4 . . ? O17 C66 O16 122.7(5) . . ? O17 C66 C63 121.1(6) . . ? O16 C66 C63 115.7(5) . . ? O17 C66 Cd3 62.0(3) . 1_546 ? O16 C66 Cd3 60.9(3) . 1_546 ? C63 C66 Cd3 176.1(4) . 1_546 ? O8 Cd1 O4 87.28(16) . 1_556 ? O8 Cd1 O1 106.83(14) . 1_565 ? O4 Cd1 O1 140.10(14) 1_556 1_565 ? O8 Cd1 O2 95.99(14) . 1_565 ? O4 Cd1 O2 87.81(13) 1_556 1_565 ? O1 Cd1 O2 54.33(13) 1_565 1_565 ? O8 Cd1 O5 130.97(13) . 1_556 ? O4 Cd1 O5 53.78(14) 1_556 1_556 ? O1 Cd1 O5 122.09(14) 1_565 1_556 ? O2 Cd1 O5 109.19(13) 1_565 1_556 ? O8 Cd1 O1W 118.11(16) . . ? O4 Cd1 O1W 117.81(14) 1_556 . ? O1 Cd1 O1W 88.69(13) 1_565 . ? O2 Cd1 O1W 136.63(14) 1_565 . ? O5 Cd1 O1W 69.08(13) 1_556 . ? O8 Cd1 C1 99.95(15) . 1_565 ? O4 Cd1 C1 112.78(16) 1_556 1_565 ? O1 Cd1 C1 29.33(15) 1_565 1_565 ? O2 Cd1 C1 25.21(14) 1_565 1_565 ? O5 Cd1 C1 120.73(15) 1_556 1_565 ? O1W Cd1 C1 116.26(16) . 1_565 ? O8 Cd1 C25 110.26(18) . 1_556 ? O4 Cd1 C25 26.64(16) 1_556 1_556 ? O1 Cd1 C25 135.91(19) 1_565 1_556 ? O2 Cd1 C25 98.38(18) 1_565 1_556 ? O5 Cd1 C25 27.17(15) 1_556 1_556 ? O1W Cd1 C25 94.16(18) . 1_556 ? C1 Cd1 C25 119.2(2) 1_565 1_556 ? O2W Cd2 O10 91.02(16) . . ? O2W Cd2 O7 86.03(15) . . ? O10 Cd2 O7 173.40(15) . . ? O2W Cd2 O3W 86.62(19) . . ? O10 Cd2 O3W 95.18(17) . . ? O7 Cd2 O3W 90.54(15) . . ? O2W Cd2 O1W 113.05(17) . . ? O10 Cd2 O1W 99.40(15) . . ? O7 Cd2 O1W 76.43(13) . . ? O3W Cd2 O1W 155.09(16) . . ? O11 Cd3 O14 116.23(17) . 1_554 ? O11 Cd3 O16 147.52(17) . 1_564 ? O14 Cd3 O16 96.21(16) 1_554 1_564 ? O11 Cd3 O17 101.73(15) . 1_564 ? O14 Cd3 O17 120.98(16) 1_554 1_564 ? O16 Cd3 O17 56.26(13) 1_564 1_564 ? O11 Cd3 O4W 83.31(15) . . ? O14 Cd3 O4W 82.42(16) 1_554 . ? O16 Cd3 O4W 103.80(14) 1_564 . ? O17 Cd3 O4W 148.40(16) 1_564 . ? O11 Cd3 O13 98.68(15) . 1_554 ? O14 Cd3 O13 52.71(15) 1_554 1_554 ? O16 Cd3 O13 99.79(14) 1_564 1_554 ? O17 Cd3 O13 79.46(15) 1_564 1_554 ? O4W Cd3 O13 131.11(14) . 1_554 ? O11 Cd3 C66 124.49(18) . 1_564 ? O14 Cd3 C66 112.55(17) 1_554 1_564 ? O16 Cd3 C66 29.56(15) 1_564 1_564 ? O17 Cd3 C66 26.77(15) 1_564 1_564 ? O4W Cd3 C66 128.53(17) . 1_564 ? O13 Cd3 C66 90.34(15) 1_554 1_564 ? O11 Cd3 C58 110.89(18) . 1_554 ? O14 Cd3 C58 24.67(17) 1_554 1_554 ? O16 Cd3 C58 97.76(17) 1_564 1_554 ? O17 Cd3 C58 101.40(19) 1_564 1_554 ? O4W Cd3 C58 105.85(19) . 1_554 ? O13 Cd3 C58 28.08(16) 1_554 1_554 ? C66 Cd3 C58 102.35(18) 1_564 1_554 ? C1 O1 Cd1 91.7(3) . 1_545 ? C1 O2 Cd1 92.0(3) . 1_545 ? C5 O3 C8 112.0(4) . . ? C25 O4 Cd1 98.9(4) . 1_554 ? C25 O5 Cd1 85.3(4) . 1_554 ? C19 O6 C18 118.2(4) . . ? C33 O7 Cd2 150.3(3) . . ? C33 O8 Cd1 108.1(4) . . ? C27 O9 C26 118.0(4) . . ? C40 O10 Cd2 151.8(4) . . ? C40 O11 Cd3 124.1(4) . . ? C37 O12 C41 112.1(4) . . ? C58 O13 Cd3 80.9(4) . 1_556 ? C58 O14 Cd3 101.6(4) . 1_556 ? C52 O15 C51 116.2(4) . . ? C66 O16 Cd3 89.6(3) . 1_546 ? C66 O17 Cd3 91.2(4) . 1_546 ? C60 O18 C59 115.7(4) . . ? Cd1 O1W Cd2 104.66(16) . . ? 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 O2 C1 C2 C7 -0.4(9) . . . . ? O1 C1 C2 C7 -173.0(5) . . . . ? Cd1 C1 C2 C7 161(4) 1_545 . . . ? O2 C1 C2 C3 -173.0(6) . . . . ? O1 C1 C2 C3 14.4(8) . . . . ? Cd1 C1 C2 C3 -11(5) 1_545 . . . ? C7 C2 C3 C4 6.2(9) . . . . ? C1 C2 C3 C4 178.8(6) . . . . ? C2 C3 C4 C5 -7.5(10) . . . . ? C3 C4 C5 C6 5.5(10) . . . . ? C3 C4 C5 O3 -177.7(5) . . . . ? C4 C5 C6 C7 -2.0(9) . . . . ? O3 C5 C6 C7 -179.3(5) . . . . ? C3 C2 C7 C6 -2.9(8) . . . . ? C1 C2 C7 C6 -175.8(5) . . . . ? C5 C6 C7 C2 0.8(8) . . . . ? O3 C8 C9 C14 78.1(6) . . . . ? O3 C8 C9 C10 -111.9(5) . . . . ? C14 C9 C10 C11 3.2(7) . . . . ? C8 C9 C10 C11 -166.7(5) . . . . ? C14 C9 C10 C15 -173.8(5) . . . . ? C8 C9 C10 C15 16.3(8) . . . . ? C9 C10 C11 C12 -3.8(8) . . . . ? C15 C10 C11 C12 173.3(5) . . . . ? C9 C10 C11 C18 175.2(5) . . . . ? C15 C10 C11 C18 -7.7(7) . . . . ? C10 C11 C12 C13 1.0(7) . . . . ? C18 C11 C12 C13 -178.0(5) . . . . ? C10 C11 C12 C16 177.2(5) . . . . ? C18 C11 C12 C16 -1.8(7) . . . . ? C11 C12 C13 C14 2.6(7) . . . . ? C16 C12 C13 C14 -173.3(5) . . . . ? C11 C12 C13 C26 177.2(4) . . . . ? C16 C12 C13 C26 1.3(7) . . . . ? C12 C13 C14 C9 -3.4(8) . . . . ? C26 C13 C14 C9 -177.9(4) . . . . ? C12 C13 C14 C17 179.1(5) . . . . ? C26 C13 C14 C17 4.6(7) . . . . ? C10 C9 C14 C13 0.4(7) . . . . ? C8 C9 C14 C13 170.6(5) . . . . ? C10 C9 C14 C17 177.7(5) . . . . ? C8 C9 C14 C17 -12.0(7) . . . . ? C10 C11 C18 O6 -93.5(5) . . . . ? C12 C11 C18 O6 85.5(6) . . . . ? O6 C19 C20 C21 -174.0(6) . . . . ? C24 C19 C20 C21 -1.8(10) . . . . ? C19 C20 C21 C22 5.2(10) . . . . ? C20 C21 C22 C23 -4.9(11) . . . . ? C20 C21 C22 C25 -176.4(7) . . . . ? C21 C22 C23 C24 1.2(11) . . . . ? C25 C22 C23 C24 173.0(7) . . . . ? O6 C19 C24 C23 171.0(6) . . . . ? C20 C19 C24 C23 -1.6(11) . . . . ? C22 C23 C24 C19 1.9(11) . . . . ? C21 C22 C25 O4 -0.5(11) . . . . ? C23 C22 C25 O4 -171.8(7) . . . . ? C21 C22 C25 O5 -172.1(7) . . . . ? C23 C22 C25 O5 16.6(10) . . . . ? C21 C22 C25 Cd1 -34(5) . . . 1_554 ? C23 C22 C25 Cd1 155(4) . . . 1_554 ? C12 C13 C26 O9 -80.9(5) . . . . ? C14 C13 C26 O9 93.9(5) . . . . ? O9 C27 C28 C29 -179.7(5) . . . . ? C32 C27 C28 C29 -0.7(8) . . . . ? C27 C28 C29 C30 1.2(9) . . . . ? C28 C29 C30 C31 -0.9(8) . . . . ? C28 C29 C30 C33 177.2(5) . . . . ? C29 C30 C31 C32 0.3(8) . . . . ? C33 C30 C31 C32 -178.0(5) . . . . ? O9 C27 C32 C31 178.9(5) . . . . ? C28 C27 C32 C31 0.0(8) . . . . ? C30 C31 C32 C27 0.2(8) . . . . ? C31 C30 C33 O8 -3.1(9) . . . . ? C29 C30 C33 O8 178.8(6) . . . . ? C31 C30 C33 O7 170.6(4) . . . . ? C29 C30 C33 O7 -7.6(7) . . . . ? C39 C34 C35 C36 -0.2(10) . . . . ? C40 C34 C35 C36 179.8(6) . . . . ? C34 C35 C36 C37 -4.6(10) . . . . ? C35 C36 C37 C38 10.2(9) . . . . ? C35 C36 C37 O12 176.0(6) . . . . ? C36 C37 C38 C39 -10.9(8) . . . . ? O12 C37 C38 C39 -177.5(5) . . . . ? C35 C34 C39 C38 -0.6(10) . . . . ? C40 C34 C39 C38 179.5(6) . . . . ? C37 C38 C39 C34 6.3(9) . . . . ? C39 C34 C40 O11 23.4(10) . . . . ? C35 C34 C40 O11 -156.6(6) . . . . ? C39 C34 C40 O10 -161.5(7) . . . . ? C35 C34 C40 O10 18.5(10) . . . . ? O12 C41 C42 C47 -91.5(5) . . . . ? O12 C41 C42 C43 88.4(5) . . . . ? C47 C42 C43 C44 -2.4(7) . . . . ? C41 C42 C43 C44 177.7(4) . . . . ? C47 C42 C43 C49 176.2(5) . . . . ? C41 C42 C43 C49 -3.7(7) . . . . ? C42 C43 C44 C45 3.1(7) . . . . ? C49 C43 C44 C45 -175.7(4) . . . . ? C42 C43 C44 C51 -176.6(4) . . . . ? C49 C43 C44 C51 4.6(7) . . . . ? C43 C44 C45 C46 -1.3(7) . . . . ? C51 C44 C45 C46 178.5(4) . . . . ? C43 C44 C45 C50 175.9(5) . . . . ? C51 C44 C45 C50 -4.4(7) . . . . ? C44 C45 C46 C47 -1.3(7) . . . . ? C50 C45 C46 C47 -178.7(5) . . . . ? C44 C45 C46 C59 169.4(4) . . . . ? C50 C45 C46 C59 -7.9(7) . . . . ? C43 C42 C47 C46 0.0(7) . . . . ? C41 C42 C47 C46 179.8(4) . . . . ? C43 C42 C47 C48 175.8(5) . . . . ? C41 C42 C47 C48 -4.3(8) . . . . ? C45 C46 C47 C42 2.0(7) . . . . ? C59 C46 C47 C42 -169.5(4) . . . . ? C45 C46 C47 C48 -174.3(5) . . . . ? C59 C46 C47 C48 14.2(7) . . . . ? C45 C44 C51 O15 85.3(5) . . . . ? C43 C44 C51 O15 -95.0(5) . . . . ? O15 C52 C53 C54 -178.2(5) . . . . ? C57 C52 C53 C54 0.0(8) . . . . ? C52 C53 C54 C55 0.0(8) . . . . ? C53 C54 C55 C56 0.0(8) . . . . ? C53 C54 C55 C58 175.7(5) . . . . ? C54 C55 C56 C57 0.0(9) . . . . ? C58 C55 C56 C57 -176.0(5) . . . . ? C55 C56 C57 C52 0.0(9) . . . . ? O15 C52 C57 C56 178.4(5) . . . . ? C53 C52 C57 C56 0.0(9) . . . . ? C56 C55 C58 O14 -14.1(9) . . . . ? C54 C55 C58 O14 170.1(6) . . . . ? C56 C55 C58 O13 171.9(5) . . . . ? C54 C55 C58 O13 -3.9(8) . . . . ? C56 C55 C58 Cd3 -30(5) . . . 1_556 ? C54 C55 C58 Cd3 154(4) . . . 1_556 ? C45 C46 C59 O18 80.1(6) . . . . ? C47 C46 C59 O18 -108.4(5) . . . . ? C65 C60 C61 C62 4.7(10) . . . . ? O18 C60 C61 C62 -178.7(6) . . . . ? C60 C61 C62 C63 -4.2(10) . . . . ? C61 C62 C63 C64 2.8(9) . . . . ? C61 C62 C63 C66 -173.4(6) . . . . ? C62 C63 C64 C65 -2.1(10) . . . . ? C66 C63 C64 C65 174.2(6) . . . . ? O18 C60 C65 C64 179.2(6) . . . . ? C61 C60 C65 C64 -3.9(11) . . . . ? C63 C64 C65 C60 2.9(11) . . . . ? C64 C63 C66 O17 3.5(10) . . . . ? C62 C63 C66 O17 179.9(6) . . . . ? C64 C63 C66 O16 176.0(6) . . . . ? C62 C63 C66 O16 -7.7(8) . . . . ? C64 C63 C66 Cd3 147(6) . . . 1_546 ? C62 C63 C66 Cd3 -37(7) . . . 1_546 ? O2 C1 O1 Cd1 10.0(6) . . . 1_545 ? C2 C1 O1 Cd1 -177.3(4) . . . 1_545 ? O1 C1 O2 Cd1 -9.6(6) . . . 1_545 ? C2 C1 O2 Cd1 178.1(5) . . . 1_545 ? C6 C5 O3 C8 161.7(5) . . . . ? C4 C5 O3 C8 -15.4(8) . . . . ? C9 C8 O3 C5 -174.9(4) . . . . ? O5 C25 O4 Cd1 -4.2(7) . . . 1_554 ? C22 C25 O4 Cd1 -175.4(6) . . . 1_554 ? O4 C25 O5 Cd1 3.7(7) . . . 1_554 ? C22 C25 O5 Cd1 175.1(6) . . . 1_554 ? C24 C19 O6 C18 174.2(6) . . . . ? C20 C19 O6 C18 -13.5(9) . . . . ? C11 C18 O6 C19 177.7(5) . . . . ? O8 C33 O7 Cd2 106.6(8) . . . . ? C30 C33 O7 Cd2 -67.8(8) . . . . ? O2W Cd2 O7 C33 138.7(8) . . . . ? O10 Cd2 O7 C33 -157.8(12) . . . . ? O3W Cd2 O7 C33 52.1(8) . . . . ? O1W Cd2 O7 C33 -106.4(8) . . . . ? O7 C33 O8 Cd1 1.6(6) . . . . ? C30 C33 O8 Cd1 174.7(5) . . . . ? O4 Cd1 O8 C33 -146.9(4) 1_556 . . . ? O1 Cd1 O8 C33 71.1(4) 1_565 . . . ? O2 Cd1 O8 C33 125.5(4) 1_565 . . . ? O5 Cd1 O8 C33 -112.5(4) 1_556 . . . ? O1W Cd1 O8 C33 -26.7(4) . . . . ? C1 Cd1 O8 C33 100.4(4) 1_565 . . . ? C25 Cd1 O8 C33 -133.2(4) 1_556 . . . ? C32 C27 O9 C26 -3.0(7) . . . . ? C28 C27 O9 C26 175.9(4) . . . . ? C13 C26 O9 C27 -176.4(4) . . . . ? O11 C40 O10 Cd2 -172.7(6) . . . . ? C34 C40 O10 Cd2 12.4(14) . . . . ? O2W Cd2 O10 C40 154.1(10) . . . . ? O7 Cd2 O10 C40 90.8(15) . . . . ? O3W Cd2 O10 C40 -119.2(9) . . . . ? O1W Cd2 O10 C40 40.6(10) . . . . ? O10 C40 O11 Cd3 6.2(10) . . . . ? C34 C40 O11 Cd3 -178.5(4) . . . . ? O14 Cd3 O11 C40 -96.7(6) 1_554 . . . ? O16 Cd3 O11 C40 80.0(7) 1_564 . . . ? O17 Cd3 O11 C40 36.8(6) 1_564 . . . ? O4W Cd3 O11 C40 -174.8(6) . . . . ? O13 Cd3 O11 C40 -44.1(6) 1_554 . . . ? C66 Cd3 O11 C40 52.3(7) 1_564 . . . ? C58 Cd3 O11 C40 -70.3(6) 1_554 . . . ? C38 C37 O12 C41 169.7(5) . . . . ? C36 C37 O12 C41 3.7(7) . . . . ? C42 C41 O12 C37 172.8(4) . . . . ? O14 C58 O13 Cd3 4.1(6) . . . 1_556 ? C55 C58 O13 Cd3 177.9(5) . . . 1_556 ? O13 C58 O14 Cd3 -4.9(7) . . . 1_556 ? C55 C58 O14 Cd3 -178.2(5) . . . 1_556 ? C53 C52 O15 C51 -7.0(8) . . . . ? C57 C52 O15 C51 174.7(5) . . . . ? C44 C51 O15 C52 -175.4(4) . . . . ? O17 C66 O16 Cd3 -5.5(7) . . . 1_546 ? C63 C66 O16 Cd3 -177.8(5) . . . 1_546 ? O16 C66 O17 Cd3 5.4(6) . . . 1_546 ? C63 C66 O17 Cd3 177.3(5) . . . 1_546 ? C65 C60 O18 C59 164.4(6) . . . . ? C61 C60 O18 C59 -12.1(9) . . . . ? C46 C59 O18 C60 -168.8(5) . . . . ? O8 Cd1 O1W Cd2 15.8(2) . . . . ? O4 Cd1 O1W Cd2 118.57(17) 1_556 . . . ? O1 Cd1 O1W Cd2 -92.61(17) 1_565 . . . ? O2 Cd1 O1W Cd2 -121.7(2) 1_565 . . . ? O5 Cd1 O1W Cd2 142.10(18) 1_556 . . . ? C1 Cd1 O1W Cd2 -102.98(19) 1_565 . . . ? C25 Cd1 O1W Cd2 131.44(19) 1_556 . . . ? O2W Cd2 O1W Cd1 86.03(19) . . . . ? O10 Cd2 O1W Cd1 -178.81(15) . . . . ? O7 Cd2 O1W Cd1 6.41(13) . . . . ? O3W Cd2 O1W Cd1 -53.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.470 _refine_diff_density_min -1.045 _refine_diff_density_rms 0.104 _database_code_depnum_ccdc_archive 'CCDC 939259' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 # start Validation Reply Form _vrf_CHEMW03_2 ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE:The formula weight differs from that calculated due to unlocated solvent moieties - SQUEEZE used - see _platon_squeeze_details. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C81 H96 Mn3 N5 O26.5' _chemical_formula_weight 1728.46 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 16.1796(15) _cell_length_b 19.1505(17) _cell_length_c 19.5848(12) _cell_angle_alpha 112.451(2) _cell_angle_beta 93.548(3) _cell_angle_gamma 104.215(2) _cell_volume 5353.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 7098 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 22.33 _exptl_crystal_description rhombus _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.072 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1796 _exptl_absorpt_coefficient_mu 0.411 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9068 _exptl_absorpt_correction_T_max 0.9103 _exptl_absorpt_process_details SADABS;Bruker,2000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42686 _diffrn_reflns_av_R_equivalents 0.0079 _diffrn_reflns_av_sigmaI/netI 0.0738 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 26.00 _reflns_number_total 20816 _reflns_number_gt 13118 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. The hydrogen atoms on coordinated water cannot be located in the Fourier difference map and thus were not added in the final cycles of refinement. Those hydrogens are, however, included in the reported chemical formula and derived values (reported crystal-data formula, formula weight,Dx, Mu and F(000)). ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.006 -0.011 0.007 2260 113 ' ' _platon_squeeze_details ; Because of the highly disordered solvent molecules, the PLATON/SQUEEZE route was employed to calculate the diffraction contribution from the solvent molecules, and thereby to produce a set of solvent-free diffraction intensities used for refinement. The unit cell was found to contain a void of 2260 A^3 (42.2% of the unit cell volume), holding 113 electrons. These might correspond with the removal of 2 DMF and 3 H2O molecules from the unit cell, i.e. 1 DMF and 1.5 H2O per asymmetric unit. Based on the elemental analysis and TG analysis, additional 2 DMF might be adsorbed in the sample and were thus included in the final molecular formula. Those solvents are included in the reported chemical formula and derived values (reported crystal-data formula, formula weight, Dx, Mu and F(000)). ; _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^)+(0.0600P)^2^+1.8800P] 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 20816 _refine_ls_number_parameters 890 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0667 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1560 _refine_ls_wR_factor_gt 0.1545 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _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 C1 C 0.5724(2) 0.00059(19) 0.25756(19) 0.0449(8) Uani 1 1 d . . . C2 C 0.6308(2) 0.0839(2) 0.29073(19) 0.0490(9) Uani 1 1 d . . . C3 C 0.5965(2) 0.1460(2) 0.3131(2) 0.0521(9) Uani 1 1 d . . . H3 H 0.5368 0.1360 0.3087 0.062 Uiso 1 1 calc R . . C4 C 0.6496(2) 0.22435(18) 0.34261(18) 0.0447(8) Uani 1 1 d . . . H4 H 0.6253 0.2659 0.3582 0.054 Uiso 1 1 calc R . . C5 C 0.7376(2) 0.23910(18) 0.34824(18) 0.0425(8) Uani 1 1 d . . . C6 C 0.7738(2) 0.17822(19) 0.3308(2) 0.0514(9) Uani 1 1 d . . . H6 H 0.8337 0.1887 0.3385 0.062 Uiso 1 1 calc R . . C7 C 0.7194(2) 0.0986(2) 0.3006(2) 0.0519(9) Uani 1 1 d . . . H7 H 0.7436 0.0570 0.2878 0.062 Uiso 1 1 calc R . . C8 C 0.7577(2) 0.37930(18) 0.39439(17) 0.0406(7) Uani 1 1 d . . . H8A H 0.7229 0.3789 0.4329 0.049 Uiso 1 1 calc R . . H8B H 0.7204 0.3736 0.3507 0.049 Uiso 1 1 calc R . . C9 C 0.8282(2) 0.45578(17) 0.42245(17) 0.0374(7) Uani 1 1 d . . . C10 C 0.8531(2) 0.49220(18) 0.37408(16) 0.0388(7) Uani 1 1 d . . . C11 C 0.9069(2) 0.56939(18) 0.40331(17) 0.0390(7) Uani 1 1 d . . . C12 C 0.9452(2) 0.60868(18) 0.47954(17) 0.0423(8) Uani 1 1 d . . . C13 C 0.9267(2) 0.56944(19) 0.52661(17) 0.0429(8) Uani 1 1 d . . . C14 C 0.8681(2) 0.49296(19) 0.49940(16) 0.0414(7) Uani 1 1 d . . . C15 C 0.9297(2) 0.6105(2) 0.34986(19) 0.0459(8) Uani 1 1 d . . . H15A H 0.8895 0.5822 0.3027 0.055 Uiso 1 1 calc R . . H15B H 0.9261 0.6642 0.3721 0.055 Uiso 1 1 calc R . . C16 C 1.0545(2) 0.6496(2) 0.29623(19) 0.0460(8) Uani 1 1 d . . . C17 C 1.0111(2) 0.6767(2) 0.25379(19) 0.0466(8) Uani 1 1 d . . . H17 H 0.9519 0.6698 0.2519 0.056 Uiso 1 1 calc R . . C18 C 1.0572(2) 0.7148(2) 0.21360(19) 0.0497(8) Uani 1 1 d . . . H18 H 1.0274 0.7328 0.1849 0.060 Uiso 1 1 calc R . . C19 C 1.1444(2) 0.72683(19) 0.21462(18) 0.0454(8) Uani 1 1 d . . . C20 C 1.1876(2) 0.6995(2) 0.25801(19) 0.0499(9) Uani 1 1 d . . . H20 H 1.2468 0.7069 0.2601 0.060 Uiso 1 1 calc R . . C21 C 1.1433(2) 0.6615(2) 0.29826(19) 0.0483(8) Uani 1 1 d . . . H21 H 1.1733 0.6436 0.3271 0.058 Uiso 1 1 calc R . . C22 C 1.1951(2) 0.77206(19) 0.17396(18) 0.0436(8) Uani 1 1 d . . . C23 C 0.9762(2) 0.6055(2) 0.60528(16) 0.0431(8) Uani 1 1 d . . . H23A H 0.9791 0.5642 0.6218 0.052 Uiso 1 1 calc R . . H23B H 1.0348 0.6352 0.6070 0.052 Uiso 1 1 calc R . . C24 C 0.9726(2) 0.6981(2) 0.72833(17) 0.0487(9) Uani 1 1 d . . . C25 C 0.9327(3) 0.7478(2) 0.7774(2) 0.0688(12) Uani 1 1 d . . . H25 H 0.8790 0.7502 0.7601 0.083 Uiso 1 1 calc R . . C26 C 0.9702(3) 0.7929(2) 0.8500(2) 0.0672(12) Uani 1 1 d . . . H26 H 0.9454 0.8302 0.8799 0.081 Uiso 1 1 calc R . . C27 C 1.0459(2) 0.7845(2) 0.88095(18) 0.0507(9) Uani 1 1 d . . . C28 C 1.0836(2) 0.7358(2) 0.83244(18) 0.0493(9) Uani 1 1 d . . . H28 H 1.1342 0.7295 0.8511 0.059 Uiso 1 1 calc R . . C29 C 1.0509(2) 0.6945(2) 0.75602(18) 0.0507(9) Uani 1 1 d . . . H29 H 1.0816 0.6648 0.7241 0.061 Uiso 1 1 calc R . . C30 C 1.0867(3) 0.8297(2) 0.9633(2) 0.0549(9) Uani 1 1 d . . . C31 C 0.8200(2) 0.4471(2) 0.29094(17) 0.0473(8) Uani 1 1 d . . . H31A H 0.7765 0.4671 0.2761 0.071 Uiso 1 1 calc R . . H31B H 0.7955 0.3921 0.2797 0.071 Uiso 1 1 calc R . . H31C H 0.8670 0.4533 0.2641 0.071 Uiso 1 1 calc R . . C32 C 1.0046(2) 0.69323(19) 0.51106(19) 0.0493(8) Uani 1 1 d . . . H32A H 1.0566 0.6942 0.4899 0.074 Uiso 1 1 calc R . . H32B H 1.0189 0.7128 0.5646 0.074 Uiso 1 1 calc R . . H32C H 0.9756 0.7260 0.4985 0.074 Uiso 1 1 calc R . . C33 C 0.8464(2) 0.45045(19) 0.55097(17) 0.0436(8) Uani 1 1 d . . . H33A H 0.8949 0.4340 0.5627 0.065 Uiso 1 1 calc R . . H33B H 0.7969 0.4050 0.5262 0.065 Uiso 1 1 calc R . . H33C H 0.8337 0.4856 0.5964 0.065 Uiso 1 1 calc R . . C34 C 0.3957(2) -0.18018(19) 0.06724(17) 0.0406(7) Uani 1 1 d . . . C35 C 0.3980(2) -0.2269(2) -0.01320(17) 0.0467(8) Uani 1 1 d . . . C36 C 0.3497(2) -0.2187(2) -0.06978(18) 0.0475(8) Uani 1 1 d . . . H36 H 0.3167 -0.1835 -0.0575 0.057 Uiso 1 1 calc R . . C37 C 0.3511(2) -0.26260(19) -0.14299(17) 0.0452(8) Uani 1 1 d . . . H37 H 0.3186 -0.2570 -0.1804 0.054 Uiso 1 1 calc R . . C38 C 0.4002(2) -0.3160(2) -0.16344(17) 0.0442(8) Uani 1 1 d . . . C39 C 0.4506(2) -0.3218(2) -0.10814(17) 0.0467(8) Uani 1 1 d . . . H39 H 0.4858 -0.3550 -0.1208 0.056 Uiso 1 1 calc R . . C40 C 0.4493(2) -0.2780(2) -0.03293(18) 0.0465(8) Uani 1 1 d . . . H40 H 0.4828 -0.2829 0.0044 0.056 Uiso 1 1 calc R . . C41 C 0.4400(2) -0.42042(19) -0.26262(17) 0.0450(8) Uani 1 1 d . . . H41A H 0.4214 -0.4577 -0.2403 0.054 Uiso 1 1 calc R . . H41B H 0.5023 -0.3973 -0.2482 0.054 Uiso 1 1 calc R . . C42 C 0.4131(2) -0.46093(19) -0.34876(17) 0.0422(8) Uani 1 1 d . . . C43 C 0.4469(2) -0.41981(19) -0.39134(17) 0.0424(8) Uani 1 1 d . . . C44 C 0.4171(2) -0.45514(19) -0.46929(18) 0.0448(8) Uani 1 1 d . . . C45 C 0.3549(2) -0.5291(2) -0.50349(17) 0.0438(8) Uani 1 1 d . . . C46 C 0.3246(2) -0.57070(19) -0.46058(17) 0.0424(8) Uani 1 1 d . . . C47 C 0.3562(2) -0.53698(19) -0.38320(17) 0.0427(8) Uani 1 1 d . . . C48 C 0.2637(2) -0.65469(19) -0.4953(2) 0.0544(10) Uani 1 1 d . . . H48A H 0.2295 -0.6653 -0.4595 0.065 Uiso 1 1 calc R . . H48B H 0.2250 -0.6631 -0.5394 0.065 Uiso 1 1 calc R . . C49 C 0.29615(14) -0.77761(10) -0.57405(10) 0.0454(8) Uani 1 1 d G . . C50 C 0.21985(13) -0.80840(12) -0.62587(12) 0.0589(11) Uani 1 1 d G . . H50 H 0.1796 -0.7802 -0.6203 0.071 Uiso 1 1 calc R . . C51 C 0.20375(12) -0.88134(13) -0.68598(11) 0.0611(11) Uani 1 1 d G . . H51 H 0.1527 -0.9019 -0.7207 0.073 Uiso 1 1 calc R . . C52 C 0.26395(14) -0.92348(10) -0.69427(10) 0.0462(8) Uani 1 1 d G . . C53 C 0.34025(12) -0.89270(11) -0.64245(12) 0.0474(8) Uani 1 1 d G . . H53 H 0.3805 -0.9209 -0.6480 0.057 Uiso 1 1 calc R . . C54 C 0.35635(11) -0.81976(12) -0.58234(11) 0.0483(9) Uani 1 1 d G . . H54 H 0.4074 -0.7992 -0.5477 0.058 Uiso 1 1 calc R . . C55 C 0.2511(2) -1.0007(2) -0.76083(19) 0.0470(8) Uani 1 1 d . . . C56 C 0.4539(2) -0.4137(2) -0.51815(19) 0.0467(8) Uani 1 1 d . . . H56A H 0.5146 -0.3850 -0.4989 0.056 Uiso 1 1 calc R . . H56B H 0.4483 -0.4518 -0.5693 0.056 Uiso 1 1 calc R . . C57 C 0.4217(2) -0.3179(2) -0.55970(18) 0.0469(8) Uani 1 1 d . . . C58 C 0.4869(2) -0.3250(2) -0.60462(19) 0.0526(9) Uani 1 1 d . . . H58 H 0.5218 -0.3571 -0.6049 0.063 Uiso 1 1 calc R . . C59 C 0.4969(2) -0.2815(2) -0.64889(19) 0.0527(9) Uani 1 1 d . . . H59 H 0.5390 -0.2864 -0.6792 0.063 Uiso 1 1 calc R . . C60 C 0.4495(2) -0.2332(2) -0.65034(19) 0.0519(9) Uani 1 1 d . . . C61 C 0.3848(2) -0.2258(2) -0.6048(2) 0.0529(9) Uani 1 1 d . . . H61 H 0.3502 -0.1939 -0.6058 0.064 Uiso 1 1 calc R . . C62 C 0.3721(2) -0.2680(2) -0.55650(19) 0.0494(8) Uani 1 1 d . . . H62 H 0.3318 -0.2615 -0.5245 0.059 Uiso 1 1 calc R . . C63 C 0.4598(2) -0.1910(2) -0.7016(2) 0.0497(9) Uani 1 1 d . . . C64 C 0.5100(2) -0.3376(2) -0.3511(2) 0.0505(8) Uani 1 1 d . . . H64A H 0.5152 -0.3112 -0.3842 0.076 Uiso 1 1 calc R . . H64B H 0.5656 -0.3416 -0.3359 0.076 Uiso 1 1 calc R . . H64C H 0.4891 -0.3080 -0.3076 0.076 Uiso 1 1 calc R . . C65 C 0.3239(2) -0.5856(2) -0.33699(19) 0.0482(8) Uani 1 1 d . . . H65A H 0.3692 -0.5734 -0.2966 0.072 Uiso 1 1 calc R . . H65B H 0.3081 -0.6410 -0.3689 0.072 Uiso 1 1 calc R . . H65C H 0.2744 -0.5724 -0.3169 0.072 Uiso 1 1 calc R . . C66 C 0.3219(3) -0.5563(2) -0.58927(18) 0.0573(10) Uani 1 1 d . . . H66D H 0.3117 -0.5128 -0.5978 0.086 Uiso 1 1 calc R . . H66E H 0.2691 -0.5988 -0.6051 0.086 Uiso 1 1 calc R . . H66F H 0.3649 -0.5740 -0.6174 0.086 Uiso 1 1 calc R . . C67 C 0.6947(3) -0.0758(2) 0.1034(2) 0.0668(11) Uani 1 1 d . . . H67 H 0.7515 -0.0719 0.1197 0.080 Uiso 1 1 calc R . . C68 C 0.7518(3) 0.0654(2) 0.1200(2) 0.0725(12) Uani 1 1 d . . . H68A H 0.7638 0.0917 0.1738 0.109 Uiso 1 1 calc R . . H68B H 0.7352 0.0992 0.0995 0.109 Uiso 1 1 calc R . . H68C H 0.8028 0.0535 0.1021 0.109 Uiso 1 1 calc R . . C69 C 0.5937(3) -0.0072(2) 0.0712(2) 0.0657(11) Uani 1 1 d . . . H69A H 0.5771 -0.0385 0.0181 0.098 Uiso 1 1 calc R . . H69B H 0.5943 0.0462 0.0820 0.098 Uiso 1 1 calc R . . H69C H 0.5529 -0.0285 0.0969 0.098 Uiso 1 1 calc R . . C70 C 0.2683(3) 0.0465(2) 0.0857(2) 0.0633(10) Uani 1 1 d . . . H70 H 0.2137 0.0481 0.0698 0.076 Uiso 1 1 calc R . . C71 C 0.4197(3) 0.1255(3) 0.1603(2) 0.0712(12) Uani 1 1 d . . . H71A H 0.4167 0.0902 0.1847 0.107 Uiso 1 1 calc R . . H71B H 0.4478 0.1787 0.1958 0.107 Uiso 1 1 calc R . . H71C H 0.4521 0.1115 0.1202 0.107 Uiso 1 1 calc R . . C72 C 0.3096(3) 0.1940(2) 0.1509(2) 0.0704(11) Uani 1 1 d . . . H72A H 0.3036 0.2059 0.1078 0.106 Uiso 1 1 calc R . . H72B H 0.3547 0.2357 0.1892 0.106 Uiso 1 1 calc R . . H72C H 0.2560 0.1891 0.1697 0.106 Uiso 1 1 calc R . . Mn1 Mn 0.38596(3) -0.11289(3) 0.21689(2) 0.03531(12) Uani 1 1 d . . . Mn2 Mn 0.21415(3) -0.11855(3) 0.09345(2) 0.03525(12) Uani 1 1 d . . . Mn3 Mn 0.57313(3) -0.17709(3) 0.17399(3) 0.03999(13) Uani 1 1 d . . . N1 N 0.6807(2) -0.00860(19) 0.09653(18) 0.0668(9) Uani 1 1 d . . . N2 N 0.3316(2) 0.11950(19) 0.12969(18) 0.0624(8) Uani 1 1 d . . . O1 O 0.60701(15) -0.05383(14) 0.23939(13) 0.0532(6) Uani 1 1 d . . . O2 O 0.49126(13) -0.00986(11) 0.24959(11) 0.0358(5) Uani 1 1 d . . . O3 O 0.79519(14) 0.31344(12) 0.37459(12) 0.0443(5) Uani 1 1 d . . . O4 O 1.15438(13) 0.79746(12) 0.13695(11) 0.0380(5) Uani 1 1 d . . . O5 O 1.27643(13) 0.78190(11) 0.18183(11) 0.0361(5) Uani 1 1 d . . . O6 O 1.01728(14) 0.61082(14) 0.33718(13) 0.0489(6) Uani 1 1 d . . . O7 O 1.05460(18) 0.87632(17) 1.00664(14) 0.0722(8) Uani 1 1 d . . . O8 O 1.15229(16) 0.81665(14) 0.98273(13) 0.0578(7) Uani 1 1 d . . . O9 O 0.93198(14) 0.65795(13) 0.65461(12) 0.0527(6) Uani 1 1 d . . . O10 O 0.44464(14) -0.18275(13) 0.11778(11) 0.0433(5) Uani 1 1 d . . . O11 O 0.34416(14) -0.13871(13) 0.08426(11) 0.0441(5) Uani 1 1 d . . . O12 O 0.39516(14) -0.35876(13) -0.23960(11) 0.0494(6) Uani 1 1 d . . . O13 O 0.30129(14) -1.04052(12) -0.76280(11) 0.0392(5) Uani 1 1 d . . . O14 O 0.18736(17) -1.02375(14) -0.81222(13) 0.0617(7) Uani 1 1 d . . . O15 O 0.32058(15) -0.70468(13) -0.51529(12) 0.0566(7) Uani 1 1 d . . . O16 O 0.51063(17) -0.20999(15) -0.74903(14) 0.0634(7) Uani 1 1 d . . . O17 O 0.42007(13) -0.14288(12) -0.69396(11) 0.0366(5) Uani 1 1 d . . . O18 O 0.40335(15) -0.35913(14) -0.51567(12) 0.0475(6) Uani 1 1 d . . . O19 O 0.63589(14) -0.14363(12) 0.08918(11) 0.0400(5) Uani 1 1 d . . . O20 O 0.28022(16) -0.01793(15) 0.06727(14) 0.0560(6) Uani 1 1 d . . . O1W O 0.70226(17) -0.16942(16) 0.22635(14) 0.0658(7) Uani 1 1 d . . . O2W O 0.55931(15) -0.29901(13) 0.10808(12) 0.0468(6) 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 C1 0.044(2) 0.0305(17) 0.054(2) 0.0108(15) 0.0090(16) 0.0097(16) C2 0.045(2) 0.0372(19) 0.0496(19) 0.0127(16) 0.0126(16) -0.0068(16) C3 0.0348(18) 0.0394(19) 0.061(2) 0.0119(17) 0.0085(16) -0.0110(16) C4 0.0422(19) 0.0297(16) 0.0525(19) 0.0088(15) 0.0074(15) 0.0072(15) C5 0.0390(18) 0.0298(17) 0.0482(18) 0.0068(14) 0.0108(15) 0.0059(15) C6 0.0374(19) 0.0364(18) 0.068(2) 0.0099(17) 0.0112(17) 0.0069(16) C7 0.046(2) 0.0377(19) 0.062(2) 0.0076(17) 0.0122(17) 0.0141(16) C8 0.0357(17) 0.0374(17) 0.0386(16) 0.0088(14) 0.0095(14) 0.0038(14) C9 0.0360(17) 0.0291(16) 0.0401(16) 0.0090(13) 0.0104(13) 0.0049(13) C10 0.0387(18) 0.0363(17) 0.0333(15) 0.0091(13) 0.0084(13) 0.0048(14) C11 0.0363(17) 0.0389(17) 0.0362(16) 0.0104(14) 0.0117(13) 0.0081(14) C12 0.0405(18) 0.0352(17) 0.0397(17) 0.0061(14) 0.0070(14) 0.0067(15) C13 0.0394(18) 0.0437(19) 0.0356(16) 0.0080(14) 0.0074(14) 0.0077(15) C14 0.0421(19) 0.0402(18) 0.0341(16) 0.0065(14) 0.0087(14) 0.0123(15) C15 0.0407(19) 0.0446(19) 0.0469(18) 0.0135(16) 0.0121(15) 0.0105(16) C16 0.0440(19) 0.049(2) 0.0490(19) 0.0231(17) 0.0175(16) 0.0134(16) C17 0.0376(18) 0.051(2) 0.055(2) 0.0257(17) 0.0134(16) 0.0113(16) C18 0.044(2) 0.053(2) 0.0502(19) 0.0208(17) 0.0081(16) 0.0101(17) C19 0.044(2) 0.0387(18) 0.0409(17) 0.0087(15) 0.0075(15) 0.0035(15) C20 0.0393(19) 0.056(2) 0.054(2) 0.0218(18) 0.0183(16) 0.0119(17) C21 0.041(2) 0.055(2) 0.0512(19) 0.0235(17) 0.0119(16) 0.0151(17) C22 0.043(2) 0.0363(18) 0.0439(18) 0.0115(15) 0.0077(15) 0.0073(15) C23 0.0384(18) 0.0478(19) 0.0363(16) 0.0101(15) -0.0033(14) 0.0149(15) C24 0.047(2) 0.047(2) 0.0362(17) 0.0029(15) -0.0117(15) 0.0130(16) C25 0.055(2) 0.068(3) 0.050(2) -0.0142(19) -0.0105(18) 0.029(2) C26 0.060(2) 0.066(3) 0.047(2) -0.0125(19) 0.0049(18) 0.027(2) C27 0.053(2) 0.052(2) 0.0374(17) 0.0107(16) 0.0088(16) 0.0108(18) C28 0.0418(19) 0.053(2) 0.0400(17) 0.0116(16) -0.0115(15) 0.0086(17) C29 0.047(2) 0.052(2) 0.0371(17) 0.0033(16) -0.0112(15) 0.0169(17) C30 0.057(2) 0.048(2) 0.046(2) 0.0102(17) 0.0091(18) 0.0064(19) C31 0.046(2) 0.0466(19) 0.0384(17) 0.0081(15) 0.0102(15) 0.0088(16) C32 0.045(2) 0.0385(18) 0.0485(19) 0.0101(15) 0.0119(16) -0.0042(16) C33 0.0403(19) 0.0452(19) 0.0389(17) 0.0135(15) 0.0100(14) 0.0068(15) C34 0.0380(18) 0.0385(18) 0.0399(17) 0.0112(14) 0.0105(15) 0.0092(15) C35 0.047(2) 0.0438(19) 0.0378(17) 0.0055(15) 0.0090(15) 0.0124(16) C36 0.048(2) 0.049(2) 0.0420(18) 0.0132(16) 0.0133(15) 0.0157(17) C37 0.048(2) 0.0433(19) 0.0367(17) 0.0086(15) 0.0099(15) 0.0133(16) C38 0.047(2) 0.0436(19) 0.0346(16) 0.0068(14) 0.0092(14) 0.0156(16) C39 0.050(2) 0.0461(19) 0.0398(17) 0.0097(15) 0.0134(15) 0.0187(17) C40 0.053(2) 0.0454(19) 0.0366(17) 0.0106(15) 0.0096(15) 0.0169(17) C41 0.050(2) 0.0397(18) 0.0373(16) 0.0071(14) 0.0075(15) 0.0143(16) C42 0.0398(18) 0.0436(19) 0.0356(16) 0.0084(14) 0.0073(14) 0.0117(15) C43 0.0444(19) 0.0413(18) 0.0370(16) 0.0108(14) 0.0076(14) 0.0136(15) C44 0.047(2) 0.0410(19) 0.0444(18) 0.0128(15) 0.0159(16) 0.0149(16) C45 0.049(2) 0.0442(19) 0.0367(16) 0.0098(15) 0.0132(15) 0.0209(17) C46 0.0413(18) 0.0384(18) 0.0403(17) 0.0062(14) 0.0096(14) 0.0151(15) C47 0.047(2) 0.0391(18) 0.0383(16) 0.0115(14) 0.0140(15) 0.0124(16) C48 0.043(2) 0.0408(19) 0.051(2) -0.0124(16) 0.0023(16) 0.0152(16) C49 0.050(2) 0.0365(18) 0.0383(17) 0.0048(14) 0.0073(15) 0.0111(16) C50 0.048(2) 0.042(2) 0.056(2) -0.0126(17) -0.0139(17) 0.0185(17) C51 0.050(2) 0.056(2) 0.0447(19) -0.0147(17) -0.0058(16) 0.0216(19) C52 0.047(2) 0.0408(18) 0.0368(17) 0.0046(14) 0.0064(15) 0.0072(16) C53 0.044(2) 0.0397(18) 0.0509(19) 0.0122(16) 0.0057(16) 0.0098(16) C54 0.049(2) 0.0336(17) 0.0475(18) 0.0023(15) -0.0107(16) 0.0144(16) C55 0.052(2) 0.0369(18) 0.0465(19) 0.0090(15) 0.0128(17) 0.0159(17) C56 0.052(2) 0.049(2) 0.0445(18) 0.0188(16) 0.0185(16) 0.0225(17) C57 0.047(2) 0.056(2) 0.0383(17) 0.0188(16) 0.0100(15) 0.0158(17) C58 0.048(2) 0.059(2) 0.051(2) 0.0217(18) 0.0163(17) 0.0141(18) C59 0.046(2) 0.064(2) 0.0428(18) 0.0202(18) 0.0128(16) 0.0084(18) C60 0.052(2) 0.047(2) 0.0452(19) 0.0160(16) -0.0101(17) 0.0030(17) C61 0.054(2) 0.0409(19) 0.056(2) 0.0157(17) -0.0092(18) 0.0121(17) C62 0.049(2) 0.054(2) 0.0453(18) 0.0185(17) 0.0080(16) 0.0195(18) C63 0.047(2) 0.045(2) 0.0462(19) 0.0098(16) -0.0041(17) 0.0113(17) C64 0.043(2) 0.046(2) 0.054(2) 0.0171(17) 0.0093(16) 0.0043(16) C65 0.044(2) 0.0439(19) 0.054(2) 0.0174(16) 0.0138(16) 0.0116(16) C66 0.057(2) 0.070(3) 0.0395(18) 0.0102(18) 0.0098(16) 0.029(2) C67 0.054(2) 0.054(2) 0.067(2) 0.017(2) 0.011(2) -0.013(2) C68 0.072(3) 0.063(3) 0.062(2) 0.023(2) 0.012(2) -0.011(2) C69 0.067(3) 0.066(3) 0.063(2) 0.023(2) 0.021(2) 0.021(2) C70 0.056(2) 0.052(2) 0.070(3) 0.015(2) 0.010(2) 0.012(2) C71 0.061(3) 0.075(3) 0.067(2) 0.023(2) -0.006(2) 0.016(2) C72 0.078(3) 0.066(3) 0.067(3) 0.025(2) 0.015(2) 0.024(2) Mn1 0.0383(3) 0.0297(2) 0.0328(2) 0.00912(19) 0.00810(19) 0.0067(2) Mn2 0.0380(3) 0.0333(3) 0.0302(2) 0.00907(19) 0.00823(19) 0.0089(2) Mn3 0.0438(3) 0.0351(3) 0.0383(3) 0.0116(2) 0.0086(2) 0.0122(2) N1 0.054(2) 0.054(2) 0.067(2) 0.0174(17) 0.0114(16) -0.0130(16) N2 0.063(2) 0.057(2) 0.0596(19) 0.0145(16) 0.0160(16) 0.0171(17) O1 0.0505(15) 0.0389(13) 0.0585(14) 0.0086(11) 0.0125(12) 0.0109(12) O2 0.0383(12) 0.0300(11) 0.0340(10) 0.0097(9) 0.0080(9) 0.0063(9) O3 0.0378(12) 0.0345(12) 0.0500(13) 0.0093(10) 0.0049(10) 0.0059(10) O4 0.0409(12) 0.0365(12) 0.0333(10) 0.0116(9) 0.0080(9) 0.0096(10) O5 0.0389(12) 0.0306(11) 0.0340(10) 0.0098(9) 0.0088(9) 0.0068(9) O6 0.0420(13) 0.0562(15) 0.0511(13) 0.0255(12) 0.0126(11) 0.0119(11) O7 0.0679(18) 0.0687(18) 0.0523(15) -0.0067(14) 0.0147(14) 0.0227(15) O8 0.0518(16) 0.0516(15) 0.0462(13) 0.0130(12) -0.0154(12) -0.0085(12) O9 0.0420(13) 0.0473(14) 0.0392(12) -0.0095(10) -0.0097(10) 0.0106(11) O10 0.0410(13) 0.0421(13) 0.0355(11) 0.0035(10) 0.0095(10) 0.0123(10) O11 0.0438(13) 0.0477(13) 0.0357(11) 0.0121(10) 0.0115(10) 0.0116(11) O12 0.0463(14) 0.0437(13) 0.0348(11) -0.0095(10) 0.0047(10) 0.0154(11) O13 0.0389(12) 0.0326(11) 0.0400(11) 0.0095(9) 0.0124(9) 0.0074(10) O14 0.0618(17) 0.0462(14) 0.0447(13) -0.0155(11) 0.0091(12) 0.0158(13) O15 0.0464(14) 0.0433(13) 0.0489(13) -0.0111(11) -0.0101(11) 0.0132(11) O16 0.0607(17) 0.0606(16) 0.0534(14) 0.0237(13) 0.0112(13) -0.0098(13) O17 0.0396(12) 0.0311(11) 0.0335(10) 0.0096(9) 0.0077(9) 0.0065(10) O18 0.0504(14) 0.0538(14) 0.0452(12) 0.0222(11) 0.0168(11) 0.0218(12) O19 0.0438(13) 0.0351(12) 0.0383(11) 0.0116(9) 0.0086(10) 0.0122(10) O20 0.0603(16) 0.0443(15) 0.0611(15) 0.0216(12) 0.0179(13) 0.0096(12) O1W 0.0611(17) 0.0624(17) 0.0593(15) 0.0118(13) -0.0100(13) 0.0197(14) O2W 0.0545(14) 0.0414(13) 0.0420(12) 0.0124(10) 0.0074(10) 0.0178(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 C1 O1 1.246(4) . ? C1 O2 1.269(4) . ? C1 C2 1.501(4) . ? C2 C3 1.367(5) . ? C2 C7 1.377(5) . ? C3 C4 1.403(4) . ? C3 H3 0.9300 . ? C4 C5 1.370(5) . ? C4 H4 0.9300 . ? C5 C6 1.370(5) . ? C5 O3 1.375(4) . ? C6 C7 1.427(5) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 O3 1.463(4) . ? C8 C9 1.495(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.400(4) . ? C9 C14 1.425(4) . ? C10 C11 1.389(4) . ? C10 C31 1.508(4) . ? C11 C12 1.406(4) . ? C11 C15 1.544(4) . ? C12 C13 1.399(5) . ? C12 C32 1.525(4) . ? C13 C14 1.409(5) . ? C13 C23 1.502(4) . ? C14 C33 1.529(4) . ? C15 O6 1.452(4) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 O6 1.361(4) . ? C16 C17 1.374(5) . ? C16 C21 1.395(5) . ? C17 C18 1.397(5) . ? C17 H17 0.9300 . ? C18 C19 1.371(5) . ? C18 H18 0.9300 . ? C19 C20 1.388(5) . ? C19 C22 1.521(5) . ? C20 C21 1.384(5) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 O4 1.250(4) . ? C22 O5 1.274(4) . ? C23 O9 1.467(4) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C29 1.376(4) . ? C24 O9 1.376(4) . ? C24 C25 1.388(5) . ? C25 C26 1.354(5) . ? C25 H25 0.9300 . ? C26 C27 1.405(5) . ? C26 H26 0.9300 . ? C27 C28 1.348(5) . ? C27 C30 1.519(5) . ? C28 C29 1.392(4) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 O8 1.219(4) . ? C30 O7 1.221(4) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 O10 1.252(4) . ? C34 O11 1.263(4) . ? C34 C35 1.494(4) . ? C35 C40 1.394(5) . ? C35 C36 1.397(5) . ? C36 C37 1.362(4) . ? C36 H36 0.9300 . ? C37 C38 1.402(5) . ? C37 H37 0.9300 . ? C38 C39 1.370(5) . ? C38 O12 1.386(4) . ? C39 C40 1.394(4) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 O12 1.476(4) . ? C41 C42 1.543(4) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C47 1.392(5) . ? C42 C43 1.400(5) . ? C43 C44 1.407(4) . ? C43 C64 1.519(5) . ? C44 C45 1.400(5) . ? C44 C56 1.522(5) . ? C45 C46 1.397(5) . ? C45 C66 1.569(4) . ? C46 C47 1.403(4) . ? C46 C48 1.525(5) . ? C47 C65 1.556(5) . ? C48 O15 1.452(4) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 O15 1.370(2) . ? C49 C50 1.3900 . ? C49 C54 1.3900 . ? C50 C51 1.3900 . ? C50 H50 0.9300 . ? C51 C52 1.3900 . ? C51 H51 0.9300 . ? C52 C53 1.3900 . ? C52 C55 1.507(3) . ? C53 C54 1.3900 . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? C55 O13 1.236(4) . ? C55 O14 1.257(4) . ? C56 O18 1.466(4) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 O18 1.375(4) . ? C57 C62 1.377(5) . ? C57 C58 1.415(5) . ? C58 C59 1.405(5) . ? C58 H58 0.9300 . ? C59 C60 1.345(5) . ? C59 H59 0.9300 . ? C60 C61 1.415(5) . ? C60 C63 1.503(5) . ? C61 C62 1.455(5) . ? C61 H61 0.9300 . ? C62 H62 0.9300 . ? C63 O17 1.219(4) . ? C63 O16 1.287(4) . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? C66 H66D 0.9600 . ? C66 H66E 0.9600 . ? C66 H66F 0.9600 . ? C67 O19 1.325(4) . ? C67 N1 1.412(5) . ? C67 H67 0.9300 . ? C68 N1 1.477(5) . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C69 N1 1.474(5) . ? C69 H69A 0.9600 . ? C69 H69B 0.9600 . ? C69 H69C 0.9600 . ? C70 O20 1.214(4) . ? C70 N2 1.419(5) . ? C70 H70 0.9300 . ? C71 N2 1.471(5) . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? C72 N2 1.466(5) . ? C72 H72A 0.9600 . ? C72 H72B 0.9600 . ? C72 H72C 0.9600 . ? Mn1 O2 2.111(2) . ? Mn1 O17 2.118(2) 1_556 ? Mn1 O13 2.129(2) 1_566 ? Mn1 O5 2.170(2) 1_445 ? Mn1 O10 2.308(2) . ? Mn1 O11 2.467(2) . ? Mn2 O8 2.076(2) 1_444 ? Mn2 O4 2.152(2) 1_445 ? Mn2 O14 2.196(2) 1_566 ? Mn2 O20 2.220(2) . ? Mn2 O11 2.236(2) . ? Mn3 O16 2.072(3) 1_556 ? Mn3 O1 2.117(2) . ? Mn3 O2W 2.139(2) . ? Mn3 O19 2.214(2) . ? Mn3 O1W 2.215(2) . ? Mn3 O10 2.249(2) . ? O4 Mn2 2.152(2) 1_665 ? O5 Mn1 2.170(2) 1_665 ? O8 Mn2 2.076(2) 1_666 ? O13 Mn1 2.129(2) 1_544 ? O14 Mn2 2.196(2) 1_544 ? O16 Mn3 2.072(3) 1_554 ? O17 Mn1 2.118(2) 1_554 ? 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 C1 O2 124.3(3) . . ? O1 C1 C2 117.7(3) . . ? O2 C1 C2 118.0(3) . . ? C3 C2 C7 119.3(3) . . ? C3 C2 C1 120.2(3) . . ? C7 C2 C1 120.4(3) . . ? C2 C3 C4 121.4(3) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? C5 C4 C3 119.4(3) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C6 C5 C4 120.3(3) . . ? C6 C5 O3 115.5(3) . . ? C4 C5 O3 124.1(3) . . ? C5 C6 C7 119.8(3) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C2 C7 C6 119.6(3) . . ? C2 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? O3 C8 C9 109.9(2) . . ? O3 C8 H8A 109.7 . . ? C9 C8 H8A 109.7 . . ? O3 C8 H8B 109.7 . . ? C9 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C10 C9 C14 119.9(3) . . ? C10 C9 C8 120.3(3) . . ? C14 C9 C8 119.7(3) . . ? C11 C10 C9 119.7(3) . . ? C11 C10 C31 121.1(3) . . ? C9 C10 C31 119.2(3) . . ? C10 C11 C12 121.1(3) . . ? C10 C11 C15 119.2(3) . . ? C12 C11 C15 119.6(3) . . ? C13 C12 C11 118.9(3) . . ? C13 C12 C32 120.3(3) . . ? C11 C12 C32 120.8(3) . . ? C12 C13 C14 121.1(3) . . ? C12 C13 C23 119.8(3) . . ? C14 C13 C23 118.9(3) . . ? C13 C14 C9 118.7(3) . . ? C13 C14 C33 121.3(3) . . ? C9 C14 C33 120.1(3) . . ? O6 C15 C11 107.9(3) . . ? O6 C15 H15A 110.1 . . ? C11 C15 H15A 110.1 . . ? O6 C15 H15B 110.1 . . ? C11 C15 H15B 110.1 . . ? H15A C15 H15B 108.4 . . ? O6 C16 C17 125.0(3) . . ? O6 C16 C21 116.1(3) . . ? C17 C16 C21 119.0(3) . . ? C16 C17 C18 119.0(3) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? C19 C18 C17 123.0(3) . . ? C19 C18 H18 118.5 . . ? C17 C18 H18 118.5 . . ? C18 C19 C20 117.4(3) . . ? C18 C19 C22 122.7(3) . . ? C20 C19 C22 119.8(3) . . ? C21 C20 C19 120.7(3) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C20 C21 C16 120.9(3) . . ? C20 C21 H21 119.5 . . ? C16 C21 H21 119.5 . . ? O4 C22 O5 125.5(3) . . ? O4 C22 C19 118.0(3) . . ? O5 C22 C19 116.5(3) . . ? O9 C23 C13 108.7(2) . . ? O9 C23 H23A 110.0 . . ? C13 C23 H23A 110.0 . . ? O9 C23 H23B 110.0 . . ? C13 C23 H23B 110.0 . . ? H23A C23 H23B 108.3 . . ? C29 C24 O9 124.7(3) . . ? C29 C24 C25 118.0(3) . . ? O9 C24 C25 117.3(3) . . ? C26 C25 C24 121.4(3) . . ? C26 C25 H25 119.3 . . ? C24 C25 H25 119.3 . . ? C25 C26 C27 121.3(3) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? C28 C27 C26 116.0(3) . . ? C28 C27 C30 120.8(3) . . ? C26 C27 C30 123.1(3) . . ? C27 C28 C29 123.7(3) . . ? C27 C28 H28 118.2 . . ? C29 C28 H28 118.2 . . ? C24 C29 C28 119.0(3) . . ? C24 C29 H29 120.5 . . ? C28 C29 H29 120.5 . . ? O8 C30 O7 122.9(3) . . ? O8 C30 C27 116.3(3) . . ? O7 C30 C27 120.9(4) . . ? C10 C31 H31A 109.5 . . ? C10 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C10 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C12 C32 H32A 109.5 . . ? C12 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C12 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C14 C33 H33A 109.5 . . ? C14 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C14 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O10 C34 O11 120.1(3) . . ? O10 C34 C35 119.7(3) . . ? O11 C34 C35 120.2(3) . . ? C40 C35 C36 119.1(3) . . ? C40 C35 C34 120.8(3) . . ? C36 C35 C34 120.0(3) . . ? C37 C36 C35 119.5(3) . . ? C37 C36 H36 120.2 . . ? C35 C36 H36 120.2 . . ? C36 C37 C38 121.7(3) . . ? C36 C37 H37 119.1 . . ? C38 C37 H37 119.1 . . ? C39 C38 O12 124.4(3) . . ? C39 C38 C37 118.9(3) . . ? O12 C38 C37 116.7(3) . . ? C38 C39 C40 120.1(3) . . ? C38 C39 H39 119.9 . . ? C40 C39 H39 119.9 . . ? C39 C40 C35 120.5(3) . . ? C39 C40 H40 119.8 . . ? C35 C40 H40 119.8 . . ? O12 C41 C42 103.8(2) . . ? O12 C41 H41A 111.0 . . ? C42 C41 H41A 111.0 . . ? O12 C41 H41B 111.0 . . ? C42 C41 H41B 111.0 . . ? H41A C41 H41B 109.0 . . ? C47 C42 C43 120.9(3) . . ? C47 C42 C41 120.3(3) . . ? C43 C42 C41 118.8(3) . . ? C42 C43 C44 118.2(3) . . ? C42 C43 C64 118.7(3) . . ? C44 C43 C64 123.0(3) . . ? C45 C44 C43 121.1(3) . . ? C45 C44 C56 118.8(3) . . ? C43 C44 C56 120.1(3) . . ? C46 C45 C44 119.9(3) . . ? C46 C45 C66 125.4(3) . . ? C44 C45 C66 114.7(3) . . ? C45 C46 C47 119.3(3) . . ? C45 C46 C48 122.6(3) . . ? C47 C46 C48 117.9(3) . . ? C42 C47 C46 120.4(3) . . ? C42 C47 C65 121.2(3) . . ? C46 C47 C65 118.4(3) . . ? O15 C48 C46 104.6(3) . . ? O15 C48 H48A 110.8 . . ? C46 C48 H48A 110.8 . . ? O15 C48 H48B 110.8 . . ? C46 C48 H48B 110.8 . . ? H48A C48 H48B 108.9 . . ? O15 C49 C50 124.76(16) . . ? O15 C49 C54 115.14(16) . . ? C50 C49 C54 120.0 . . ? C49 C50 C51 120.0 . . ? C49 C50 H50 120.0 . . ? C51 C50 H50 120.0 . . ? C52 C51 C50 120.0 . . ? C52 C51 H51 120.0 . . ? C50 C51 H51 120.0 . . ? C51 C52 C53 120.0 . . ? C51 C52 C55 121.61(19) . . ? C53 C52 C55 118.31(19) . . ? C54 C53 C52 120.0 . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? C53 C54 C49 120.0 . . ? C53 C54 H54 120.0 . . ? C49 C54 H54 120.0 . . ? O13 C55 O14 121.8(3) . . ? O13 C55 C52 119.9(3) . . ? O14 C55 C52 118.3(3) . . ? O18 C56 C44 106.2(3) . . ? O18 C56 H56A 110.5 . . ? C44 C56 H56A 110.5 . . ? O18 C56 H56B 110.5 . . ? C44 C56 H56B 110.5 . . ? H56A C56 H56B 108.7 . . ? O18 C57 C62 115.0(3) . . ? O18 C57 C58 123.1(3) . . ? C62 C57 C58 121.9(3) . . ? C59 C58 C57 117.2(3) . . ? C59 C58 H58 121.4 . . ? C57 C58 H58 121.4 . . ? C60 C59 C58 124.3(4) . . ? C60 C59 H59 117.8 . . ? C58 C59 H59 117.8 . . ? C59 C60 C61 118.2(3) . . ? C59 C60 C63 122.2(4) . . ? C61 C60 C63 119.5(3) . . ? C60 C61 C62 120.3(3) . . ? C60 C61 H61 119.8 . . ? C62 C61 H61 119.8 . . ? C57 C62 C61 117.9(3) . . ? C57 C62 H62 121.1 . . ? C61 C62 H62 121.1 . . ? O17 C63 O16 126.9(4) . . ? O17 C63 C60 117.4(4) . . ? O16 C63 C60 115.7(3) . . ? C43 C64 H64A 109.5 . . ? C43 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C43 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C47 C65 H65A 109.5 . . ? C47 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C47 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C45 C66 H66D 109.5 . . ? C45 C66 H66E 109.5 . . ? H66D C66 H66E 109.5 . . ? C45 C66 H66F 109.5 . . ? H66D C66 H66F 109.5 . . ? H66E C66 H66F 109.5 . . ? O19 C67 N1 127.3(4) . . ? O19 C67 H67 116.4 . . ? N1 C67 H67 116.4 . . ? N1 C68 H68A 109.5 . . ? N1 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? N1 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? N1 C69 H69A 109.5 . . ? N1 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? N1 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? O20 C70 N2 124.8(4) . . ? O20 C70 H70 117.6 . . ? N2 C70 H70 117.6 . . ? N2 C71 H71A 109.5 . . ? N2 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? N2 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? N2 C72 H72A 109.5 . . ? N2 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? N2 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? O2 Mn1 O17 96.20(8) . 1_556 ? O2 Mn1 O13 88.56(8) . 1_566 ? O17 Mn1 O13 115.48(8) 1_556 1_566 ? O2 Mn1 O5 178.89(8) . 1_445 ? O17 Mn1 O5 84.86(8) 1_556 1_445 ? O13 Mn1 O5 90.72(8) 1_566 1_445 ? O2 Mn1 O10 92.46(8) . . ? O17 Mn1 O10 106.05(8) 1_556 . ? O13 Mn1 O10 138.09(8) 1_566 . ? O5 Mn1 O10 87.52(8) 1_445 . ? O2 Mn1 O11 99.71(8) . . ? O17 Mn1 O11 154.90(8) 1_556 . ? O13 Mn1 O11 84.34(8) 1_566 . ? O5 Mn1 O11 79.39(7) 1_445 . ? O10 Mn1 O11 54.19(8) . . ? O8 Mn2 O4 97.44(9) 1_444 1_445 ? O8 Mn2 O14 132.44(11) 1_444 1_566 ? O4 Mn2 O14 89.88(9) 1_445 1_566 ? O8 Mn2 O20 91.06(10) 1_444 . ? O4 Mn2 O20 170.94(8) 1_445 . ? O14 Mn2 O20 82.03(10) 1_566 . ? O8 Mn2 O11 100.22(10) 1_444 . ? O4 Mn2 O11 101.20(8) 1_445 . ? O14 Mn2 O11 124.38(9) 1_566 . ? O20 Mn2 O11 80.27(9) . . ? O16 Mn3 O1 96.04(10) 1_556 . ? O16 Mn3 O2W 88.57(10) 1_556 . ? O1 Mn3 O2W 171.38(9) . . ? O16 Mn3 O19 178.15(9) 1_556 . ? O1 Mn3 O19 84.77(9) . . ? O2W Mn3 O19 90.84(8) . . ? O16 Mn3 O1W 93.35(11) 1_556 . ? O1 Mn3 O1W 85.37(10) . . ? O2W Mn3 O1W 87.10(9) . . ? O19 Mn3 O1W 88.37(9) . . ? O16 Mn3 O10 88.95(10) 1_556 . ? O1 Mn3 O10 94.07(9) . . ? O2W Mn3 O10 93.28(8) . . ? O19 Mn3 O10 89.33(8) . . ? O1W Mn3 O10 177.67(10) . . ? C67 N1 C69 121.6(3) . . ? C67 N1 C68 121.2(4) . . ? C69 N1 C68 117.0(4) . . ? C70 N2 C72 120.4(3) . . ? C70 N2 C71 123.3(3) . . ? C72 N2 C71 116.2(3) . . ? C1 O1 Mn3 139.1(2) . . ? C1 O2 Mn1 131.6(2) . . ? C5 O3 C8 116.3(2) . . ? C22 O4 Mn2 124.4(2) . 1_665 ? C22 O5 Mn1 131.8(2) . 1_665 ? C16 O6 C15 118.7(3) . . ? C30 O8 Mn2 117.7(2) . 1_666 ? C24 O9 C23 115.1(2) . . ? C34 O10 Mn3 154.0(2) . . ? C34 O10 Mn1 96.48(19) . . ? Mn3 O10 Mn1 103.11(8) . . ? C34 O11 Mn2 155.0(2) . . ? C34 O11 Mn1 88.76(18) . . ? Mn2 O11 Mn1 96.86(8) . . ? C38 O12 C41 117.8(2) . . ? C55 O13 Mn1 171.7(2) . 1_544 ? C55 O14 Mn2 104.7(2) . 1_544 ? C49 O15 C48 122.7(2) . . ? C63 O16 Mn3 142.6(3) . 1_554 ? C63 O17 Mn1 121.8(2) . 1_554 ? C57 O18 C56 116.8(3) . . ? C67 O19 Mn3 125.4(2) . . ? C70 O20 Mn2 129.1(3) . . ? 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 O1 C1 C2 C3 -178.7(3) . . . . ? O2 C1 C2 C3 1.6(5) . . . . ? O1 C1 C2 C7 -0.3(5) . . . . ? O2 C1 C2 C7 180.0(3) . . . . ? C7 C2 C3 C4 3.2(5) . . . . ? C1 C2 C3 C4 -178.5(3) . . . . ? C2 C3 C4 C5 0.9(5) . . . . ? C3 C4 C5 C6 -5.1(5) . . . . ? C3 C4 C5 O3 178.4(3) . . . . ? C4 C5 C6 C7 5.2(5) . . . . ? O3 C5 C6 C7 -178.0(3) . . . . ? C3 C2 C7 C6 -3.0(5) . . . . ? C1 C2 C7 C6 178.6(3) . . . . ? C5 C6 C7 C2 -1.2(6) . . . . ? O3 C8 C9 C10 97.0(3) . . . . ? O3 C8 C9 C14 -85.1(3) . . . . ? C14 C9 C10 C11 -9.7(5) . . . . ? C8 C9 C10 C11 168.3(3) . . . . ? C14 C9 C10 C31 171.1(3) . . . . ? C8 C9 C10 C31 -10.9(5) . . . . ? C9 C10 C11 C12 7.6(5) . . . . ? C31 C10 C11 C12 -173.2(3) . . . . ? C9 C10 C11 C15 -176.6(3) . . . . ? C31 C10 C11 C15 2.6(5) . . . . ? C10 C11 C12 C13 -1.5(5) . . . . ? C15 C11 C12 C13 -177.3(3) . . . . ? C10 C11 C12 C32 179.6(3) . . . . ? C15 C11 C12 C32 3.8(5) . . . . ? C11 C12 C13 C14 -2.5(5) . . . . ? C32 C12 C13 C14 176.4(3) . . . . ? C11 C12 C13 C23 171.3(3) . . . . ? C32 C12 C13 C23 -9.8(5) . . . . ? C12 C13 C14 C9 0.4(5) . . . . ? C23 C13 C14 C9 -173.5(3) . . . . ? C12 C13 C14 C33 -178.8(3) . . . . ? C23 C13 C14 C33 7.3(5) . . . . ? C10 C9 C14 C13 5.7(5) . . . . ? C8 C9 C14 C13 -172.3(3) . . . . ? C10 C9 C14 C33 -175.1(3) . . . . ? C8 C9 C14 C33 6.9(4) . . . . ? C10 C11 C15 O6 -103.2(3) . . . . ? C12 C11 C15 O6 72.6(4) . . . . ? O6 C16 C17 C18 -179.2(3) . . . . ? C21 C16 C17 C18 0.5(5) . . . . ? C16 C17 C18 C19 -0.2(5) . . . . ? C17 C18 C19 C20 -0.1(5) . . . . ? C17 C18 C19 C22 -176.8(3) . . . . ? C18 C19 C20 C21 0.2(5) . . . . ? C22 C19 C20 C21 177.0(3) . . . . ? C19 C20 C21 C16 0.0(5) . . . . ? O6 C16 C21 C20 179.3(3) . . . . ? C17 C16 C21 C20 -0.4(5) . . . . ? C18 C19 C22 O4 -1.6(5) . . . . ? C20 C19 C22 O4 -178.2(3) . . . . ? C18 C19 C22 O5 177.2(3) . . . . ? C20 C19 C22 O5 0.6(4) . . . . ? C12 C13 C23 O9 88.2(4) . . . . ? C14 C13 C23 O9 -97.9(4) . . . . ? C29 C24 C25 C26 1.6(7) . . . . ? O9 C24 C25 C26 -176.3(4) . . . . ? C24 C25 C26 C27 -7.7(7) . . . . ? C25 C26 C27 C28 7.2(6) . . . . ? C25 C26 C27 C30 -175.6(4) . . . . ? C26 C27 C28 C29 -0.8(6) . . . . ? C30 C27 C28 C29 -178.1(4) . . . . ? O9 C24 C29 C28 -177.6(3) . . . . ? C25 C24 C29 C28 4.6(6) . . . . ? C27 C28 C29 C24 -5.1(6) . . . . ? C28 C27 C30 O8 -3.1(5) . . . . ? C26 C27 C30 O8 179.9(4) . . . . ? C28 C27 C30 O7 176.9(4) . . . . ? C26 C27 C30 O7 -0.2(6) . . . . ? O10 C34 C35 C40 4.8(5) . . . . ? O11 C34 C35 C40 -174.7(3) . . . . ? O10 C34 C35 C36 -174.1(3) . . . . ? O11 C34 C35 C36 6.5(5) . . . . ? C40 C35 C36 C37 2.3(5) . . . . ? C34 C35 C36 C37 -178.9(3) . . . . ? C35 C36 C37 C38 -0.2(5) . . . . ? C36 C37 C38 C39 -2.6(5) . . . . ? C36 C37 C38 O12 178.6(3) . . . . ? O12 C38 C39 C40 -178.1(3) . . . . ? C37 C38 C39 C40 3.2(5) . . . . ? C38 C39 C40 C35 -1.2(5) . . . . ? C36 C35 C40 C39 -1.6(5) . . . . ? C34 C35 C40 C39 179.6(3) . . . . ? O12 C41 C42 C47 -108.7(3) . . . . ? O12 C41 C42 C43 71.3(4) . . . . ? C47 C42 C43 C44 4.3(5) . . . . ? C41 C42 C43 C44 -175.6(3) . . . . ? C47 C42 C43 C64 -178.9(3) . . . . ? C41 C42 C43 C64 1.2(5) . . . . ? C42 C43 C44 C45 0.6(5) . . . . ? C64 C43 C44 C45 -176.1(3) . . . . ? C42 C43 C44 C56 -178.3(3) . . . . ? C64 C43 C44 C56 5.1(5) . . . . ? C43 C44 C45 C46 -3.2(5) . . . . ? C56 C44 C45 C46 175.6(3) . . . . ? C43 C44 C45 C66 174.1(3) . . . . ? C56 C44 C45 C66 -7.0(4) . . . . ? C44 C45 C46 C47 1.0(5) . . . . ? C66 C45 C46 C47 -176.0(3) . . . . ? C44 C45 C46 C48 -173.9(3) . . . . ? C66 C45 C46 C48 9.1(5) . . . . ? C43 C42 C47 C46 -6.6(5) . . . . ? C41 C42 C47 C46 173.3(3) . . . . ? C43 C42 C47 C65 175.3(3) . . . . ? C41 C42 C47 C65 -4.8(5) . . . . ? C45 C46 C47 C42 3.9(5) . . . . ? C48 C46 C47 C42 179.0(3) . . . . ? C45 C46 C47 C65 -178.0(3) . . . . ? C48 C46 C47 C65 -2.8(4) . . . . ? C45 C46 C48 O15 86.6(4) . . . . ? C47 C46 C48 O15 -88.4(4) . . . . ? O15 C49 C50 C51 176.3(3) . . . . ? C54 C49 C50 C51 0.0 . . . . ? C49 C50 C51 C52 0.0 . . . . ? C50 C51 C52 C53 0.0 . . . . ? C50 C51 C52 C55 -176.7(3) . . . . ? C51 C52 C53 C54 0.0 . . . . ? C55 C52 C53 C54 176.8(2) . . . . ? C52 C53 C54 C49 0.0 . . . . ? O15 C49 C54 C53 -176.6(2) . . . . ? C50 C49 C54 C53 0.0 . . . . ? C51 C52 C55 O13 -172.7(2) . . . . ? C53 C52 C55 O13 10.5(4) . . . . ? C51 C52 C55 O14 5.2(4) . . . . ? C53 C52 C55 O14 -171.5(3) . . . . ? C45 C44 C56 O18 95.9(3) . . . . ? C43 C44 C56 O18 -85.2(4) . . . . ? O18 C57 C58 C59 177.9(3) . . . . ? C62 C57 C58 C59 -2.8(5) . . . . ? C57 C58 C59 C60 1.0(5) . . . . ? C58 C59 C60 C61 -0.5(5) . . . . ? C58 C59 C60 C63 -176.9(3) . . . . ? C59 C60 C61 C62 1.6(5) . . . . ? C63 C60 C61 C62 178.2(3) . . . . ? O18 C57 C62 C61 -176.7(3) . . . . ? C58 C57 C62 C61 3.9(5) . . . . ? C60 C61 C62 C57 -3.3(5) . . . . ? C59 C60 C63 O17 -173.2(3) . . . . ? C61 C60 C63 O17 10.3(5) . . . . ? C59 C60 C63 O16 6.5(5) . . . . ? C61 C60 C63 O16 -169.9(3) . . . . ? O19 C67 N1 C69 -0.1(6) . . . . ? O19 C67 N1 C68 175.2(4) . . . . ? O20 C70 N2 C72 -177.9(4) . . . . ? O20 C70 N2 C71 -1.8(6) . . . . ? O2 C1 O1 Mn3 15.2(6) . . . . ? C2 C1 O1 Mn3 -164.6(2) . . . . ? O16 Mn3 O1 C1 -76.8(4) 1_556 . . . ? O2W Mn3 O1 C1 161.1(5) . . . . ? O19 Mn3 O1 C1 101.5(4) . . . . ? O1W Mn3 O1 C1 -169.7(4) . . . . ? O10 Mn3 O1 C1 12.6(4) . . . . ? O1 C1 O2 Mn1 7.4(5) . . . . ? C2 C1 O2 Mn1 -172.9(2) . . . . ? O17 Mn1 O2 C1 60.4(3) 1_556 . . . ? O13 Mn1 O2 C1 175.9(3) 1_566 . . . ? O5 Mn1 O2 C1 -135(4) 1_445 . . . ? O10 Mn1 O2 C1 -46.0(3) . . . . ? O11 Mn1 O2 C1 -100.1(3) . . . . ? C6 C5 O3 C8 -179.3(3) . . . . ? C4 C5 O3 C8 -2.6(5) . . . . ? C9 C8 O3 C5 179.6(3) . . . . ? O5 C22 O4 Mn2 -11.4(4) . . . 1_665 ? C19 C22 O4 Mn2 167.34(19) . . . 1_665 ? O4 C22 O5 Mn1 51.8(4) . . . 1_665 ? C19 C22 O5 Mn1 -127.0(2) . . . 1_665 ? C17 C16 O6 C15 -12.7(5) . . . . ? C21 C16 O6 C15 167.7(3) . . . . ? C11 C15 O6 C16 -174.9(3) . . . . ? O7 C30 O8 Mn2 -3.2(5) . . . 1_666 ? C27 C30 O8 Mn2 176.8(2) . . . 1_666 ? C29 C24 O9 C23 3.0(5) . . . . ? C25 C24 O9 C23 -179.2(3) . . . . ? C13 C23 O9 C24 -177.1(3) . . . . ? O11 C34 O10 Mn3 -131.8(4) . . . . ? C35 C34 O10 Mn3 48.8(6) . . . . ? O11 C34 O10 Mn1 7.2(3) . . . . ? C35 C34 O10 Mn1 -172.3(3) . . . . ? O16 Mn3 O10 C34 -174.0(5) 1_556 . . . ? O1 Mn3 O10 C34 90.0(5) . . . . ? O2W Mn3 O10 C34 -85.5(5) . . . . ? O19 Mn3 O10 C34 5.3(5) . . . . ? O1W Mn3 O10 C34 14(2) . . . . ? O16 Mn3 O10 Mn1 48.01(10) 1_556 . . . ? O1 Mn3 O10 Mn1 -47.97(10) . . . . ? O2W Mn3 O10 Mn1 136.52(9) . . . . ? O19 Mn3 O10 Mn1 -132.68(9) . . . . ? O1W Mn3 O10 Mn1 -124(2) . . . . ? O2 Mn1 O10 C34 -104.12(19) . . . . ? O17 Mn1 O10 C34 158.71(19) 1_556 . . . ? O13 Mn1 O10 C34 -13.5(2) 1_566 . . . ? O5 Mn1 O10 C34 74.78(19) 1_445 . . . ? O11 Mn1 O10 C34 -3.91(18) . . . . ? O2 Mn1 O10 Mn3 58.70(9) . . . . ? O17 Mn1 O10 Mn3 -38.47(10) 1_556 . . . ? O13 Mn1 O10 Mn3 149.29(9) 1_566 . . . ? O5 Mn1 O10 Mn3 -122.41(9) 1_445 . . . ? O11 Mn1 O10 Mn3 158.90(13) . . . . ? O10 C34 O11 Mn2 -110.4(5) . . . . ? C35 C34 O11 Mn2 69.1(6) . . . . ? O10 C34 O11 Mn1 -6.7(3) . . . . ? C35 C34 O11 Mn1 172.8(3) . . . . ? O8 Mn2 O11 C34 -54.7(5) 1_444 . . . ? O4 Mn2 O11 C34 45.0(5) 1_445 . . . ? O14 Mn2 O11 C34 142.7(5) 1_566 . . . ? O20 Mn2 O11 C34 -144.1(5) . . . . ? O8 Mn2 O11 Mn1 -156.66(9) 1_444 . . . ? O4 Mn2 O11 Mn1 -56.88(9) 1_445 . . . ? O14 Mn2 O11 Mn1 40.75(13) 1_566 . . . ? O20 Mn2 O11 Mn1 114.02(9) . . . . ? O2 Mn1 O11 C34 89.86(19) . . . . ? O17 Mn1 O11 C34 -38.7(3) 1_556 . . . ? O13 Mn1 O11 C34 177.42(19) 1_566 . . . ? O5 Mn1 O11 C34 -90.79(19) 1_445 . . . ? O10 Mn1 O11 C34 3.86(17) . . . . ? O2 Mn1 O11 Mn2 -114.57(9) . . . . ? O17 Mn1 O11 Mn2 116.86(17) 1_556 . . . ? O13 Mn1 O11 Mn2 -27.00(8) 1_566 . . . ? O5 Mn1 O11 Mn2 64.79(8) 1_445 . . . ? O10 Mn1 O11 Mn2 159.43(12) . . . . ? C39 C38 O12 C41 6.6(5) . . . . ? C37 C38 O12 C41 -174.7(3) . . . . ? C42 C41 O12 C38 174.2(3) . . . . ? O14 C55 O13 Mn1 40.1(18) . . . 1_544 ? C52 C55 O13 Mn1 -142.0(14) . . . 1_544 ? O13 C55 O14 Mn2 -16.2(4) . . . 1_544 ? C52 C55 O14 Mn2 165.9(2) . . . 1_544 ? C50 C49 O15 C48 7.6(4) . . . . ? C54 C49 O15 C48 -175.9(3) . . . . ? C46 C48 O15 C49 -150.7(3) . . . . ? O17 C63 O16 Mn3 10.3(6) . . . 1_554 ? C60 C63 O16 Mn3 -169.4(3) . . . 1_554 ? O16 C63 O17 Mn1 25.1(5) . . . 1_554 ? C60 C63 O17 Mn1 -155.1(2) . . . 1_554 ? C62 C57 O18 C56 179.2(3) . . . . ? C58 C57 O18 C56 -1.4(4) . . . . ? C44 C56 O18 C57 -176.3(3) . . . . ? N1 C67 O19 Mn3 -97.6(4) . . . . ? O16 Mn3 O19 C67 139(3) 1_556 . . . ? O1 Mn3 O19 C67 22.7(3) . . . . ? O2W Mn3 O19 C67 -149.9(3) . . . . ? O1W Mn3 O19 C67 -62.8(3) . . . . ? O10 Mn3 O19 C67 116.9(3) . . . . ? N2 C70 O20 Mn2 119.1(4) . . . . ? O8 Mn2 O20 C70 109.6(3) 1_444 . . . ? O4 Mn2 O20 C70 -50.1(7) 1_445 . . . ? O14 Mn2 O20 C70 -23.1(3) 1_566 . . . ? O11 Mn2 O20 C70 -150.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.842 _refine_diff_density_min -1.058 _refine_diff_density_rms 0.085 _database_code_depnum_ccdc_archive 'CCDC 939260' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C155 H167 Co7 N7 O51' _chemical_formula_weight 3356.53 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' 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' N N 0.0061 0.0033 '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 15.260(2) _cell_length_b 17.273(3) _cell_length_c 20.297(3) _cell_angle_alpha 99.832(2) _cell_angle_beta 104.423(3) _cell_angle_gamma 115.202(2) _cell_volume 4448.2(11) _cell_formula_units_Z 1 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 9278 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.46 _exptl_crystal_description rod _exptl_crystal_colour Purple _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.253 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1743 _exptl_absorpt_coefficient_mu 0.714 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8372 _exptl_absorpt_correction_T_max 0.8483 _exptl_absorpt_process_details SADABS;Bruker,2000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 34857 _diffrn_reflns_av_R_equivalents 0.0069 _diffrn_reflns_av_sigmaI/netI 0.0566 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 26.00 _reflns_number_total 17123 _reflns_number_gt 12326 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.087 0.000 0.500 707 50 ' ' 2 0.500 1.000 1.000 418 23 ' ' _platon_squeeze_details ; Because of the highly disordered solvent molecules, the PLATON/SQUEEZE route was employed to calculate the diffraction contribution from the solvent molecules, and thereby to produce a set of solvent-free diffraction intensities used for refinement. The unit cell was found to contain a void of 1125 A^3 (25.3% of the unit cell volume), holding 73 electrons. These might correspond with the removal of ~1 DMF and 4 H2O molecules from the unit cell. Based on the elemental analysis and TG analysis, 1 DMF and 4 H2O were directly included in the final molecular formula. Those solvents are included in the reported chemical formula and derived values (reported crystal-data formula, formula weight,Dx, Mu and F(000)). ; _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^)+(0.0900P)^2^+1.8800P] 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 17123 _refine_ls_number_parameters 964 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0682 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1594 _refine_ls_wR_factor_gt 0.1568 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 C1 C 1.5971(3) 0.6739(2) 1.04443(18) 0.0351(8) Uani 1 1 d . . . H1 H 1.5858 0.7192 1.0319 0.042 Uiso 1 1 calc R . . C2 C 1.6846(3) 0.6819(2) 0.95942(19) 0.0376(8) Uani 1 1 d . . . H2A H 1.6580 0.7213 0.9481 0.056 Uiso 1 1 calc R . . H2B H 1.6620 0.6340 0.9166 0.056 Uiso 1 1 calc R . . H2C H 1.7591 0.7154 0.9790 0.056 Uiso 1 1 calc R . . C3 C 1.6739(3) 0.5812(2) 1.03604(18) 0.0348(8) Uani 1 1 d . . . H3A H 1.7463 0.6125 1.0655 0.052 Uiso 1 1 calc R . . H3B H 1.6612 0.5352 0.9951 0.052 Uiso 1 1 calc R . . H3C H 1.6333 0.5540 1.0633 0.052 Uiso 1 1 calc R . . C4 C 1.3070(3) 0.6633(2) 0.98960(17) 0.0309(8) Uani 1 1 d . . . C5 C 1.2541(3) 0.6151(2) 0.91014(17) 0.0292(7) Uani 1 1 d . . . C6 C 1.1605(3) 0.6075(2) 0.87398(17) 0.0305(7) Uani 1 1 d . . . H6 H 1.1307 0.6334 0.8986 0.037 Uiso 1 1 calc R . . C7 C 1.1094(3) 0.5611(2) 0.80039(18) 0.0324(8) Uani 1 1 d . . . H7 H 1.0459 0.5556 0.7754 0.039 Uiso 1 1 calc R . . C8 C 1.1569(3) 0.5234(2) 0.76608(17) 0.0298(7) Uani 1 1 d . . . C9 C 1.2472(3) 0.5280(2) 0.80171(17) 0.0343(8) Uani 1 1 d . . . H9 H 1.2761 0.5006 0.7776 0.041 Uiso 1 1 calc R . . C10 C 1.2964(3) 0.5740(2) 0.87456(17) 0.0310(7) Uani 1 1 d . . . H10 H 1.3584 0.5771 0.8995 0.037 Uiso 1 1 calc R . . C11 C 1.1603(3) 0.4542(2) 0.65583(17) 0.0346(8) Uani 1 1 d . . . H11A H 1.1618 0.4013 0.6648 0.041 Uiso 1 1 calc R . . H11B H 1.2310 0.5027 0.6701 0.041 Uiso 1 1 calc R . . C12 C 1.0970(3) 0.4330(2) 0.57503(17) 0.0298(7) Uani 1 1 d . . . C13 C 1.1355(3) 0.4977(2) 0.54008(18) 0.0314(7) Uani 1 1 d . . . C14 C 1.0777(3) 0.4662(2) 0.46316(17) 0.0301(7) Uani 1 1 d . . . C15 C 0.9821(3) 0.3849(2) 0.42917(17) 0.0297(7) Uani 1 1 d . . . C16 C 0.9425(3) 0.3325(2) 0.46991(17) 0.0311(8) Uani 1 1 d . . . C17 C 0.9987(3) 0.3537(2) 0.54259(17) 0.0308(7) Uani 1 1 d . . . C18 C 0.9511(3) 0.2893(2) 0.58371(18) 0.0335(8) Uani 1 1 d . . . H18A H 0.8965 0.2971 0.5935 0.050 Uiso 1 1 calc R . . H18B H 1.0039 0.3027 0.6281 0.050 Uiso 1 1 calc R . . H18C H 0.9234 0.2280 0.5551 0.050 Uiso 1 1 calc R . . C19 C 1.2435(3) 0.5833(2) 0.56494(19) 0.0392(9) Uani 1 1 d . . . H19A H 1.2816 0.5947 0.6142 0.059 Uiso 1 1 calc R . . H19B H 1.2344 0.6340 0.5602 0.059 Uiso 1 1 calc R . . H19C H 1.2812 0.5741 0.5358 0.059 Uiso 1 1 calc R . . C20 C 0.9247(3) 0.3535(2) 0.34879(17) 0.0348(8) Uani 1 1 d . . . H20A H 0.8783 0.2896 0.3325 0.052 Uiso 1 1 calc R . . H20B H 0.9739 0.3670 0.3250 0.052 Uiso 1 1 calc R . . H20C H 0.8857 0.3840 0.3381 0.052 Uiso 1 1 calc R . . C21 C 0.8349(3) 0.2481(2) 0.43183(19) 0.0361(8) Uani 1 1 d . . . H21A H 0.7983 0.2347 0.4648 0.043 Uiso 1 1 calc R . . H21B H 0.7932 0.2564 0.3919 0.043 Uiso 1 1 calc R . . C22 C 0.7734(3) 0.1022(2) 0.35673(19) 0.0403(9) Uani 1 1 d . . . C23 C 0.7970(3) 0.0399(2) 0.3246(2) 0.0437(10) Uani 1 1 d . . . H23 H 0.8653 0.0511 0.3386 0.052 Uiso 1 1 calc R . . C24 C 0.7188(3) -0.0392(2) 0.2714(2) 0.0469(10) Uani 1 1 d . . . H24 H 0.7349 -0.0808 0.2499 0.056 Uiso 1 1 calc R . . C25 C 0.6166(3) -0.0568(2) 0.2502(2) 0.0414(9) Uani 1 1 d . . . C26 C 0.5934(3) 0.0063(2) 0.28247(19) 0.0377(9) Uani 1 1 d . . . H26 H 0.5252 -0.0047 0.2683 0.045 Uiso 1 1 calc R . . C27 C 0.6712(3) 0.0852(2) 0.33522(19) 0.0367(8) Uani 1 1 d . . . H27 H 0.6553 0.1271 0.3565 0.044 Uiso 1 1 calc R . . C28 C 0.5312(3) -0.1430(2) 0.1923(2) 0.0413(9) Uani 1 1 d . . . C29 C 1.1171(3) 0.5245(2) 0.41878(18) 0.0320(8) Uani 1 1 d . . . H29A H 1.0600 0.5234 0.3836 0.038 Uiso 1 1 calc R . . H29B H 1.1653 0.5864 0.4490 0.038 Uiso 1 1 calc R . . C30 C 1.2007(3) 0.5206(2) 0.33238(17) 0.0293(7) Uani 1 1 d . . . C31 C 1.1918(3) 0.5910(2) 0.31147(17) 0.0292(7) Uani 1 1 d . . . H31 H 1.1601 0.6188 0.3319 0.035 Uiso 1 1 calc R . . C32 C 1.2304(3) 0.6181(2) 0.26036(17) 0.0305(7) Uani 1 1 d . . . H32 H 1.2235 0.6641 0.2458 0.037 Uiso 1 1 calc R . . C33 C 1.2795(3) 0.5790(2) 0.22987(18) 0.0311(7) Uani 1 1 d . . . C34 C 1.2868(3) 0.5093(2) 0.24999(18) 0.0329(8) Uani 1 1 d . . . H34 H 1.3191 0.4822 0.2295 0.039 Uiso 1 1 calc R . . C35 C 1.2471(3) 0.4792(2) 0.29993(18) 0.0330(8) Uani 1 1 d . . . H35 H 1.2510 0.4310 0.3122 0.040 Uiso 1 1 calc R . . C36 C 1.3309(3) 0.6153(2) 0.18021(18) 0.0314(8) Uani 1 1 d . . . C37 C 1.2494(3) 0.8774(2) 1.22708(18) 0.0310(8) Uani 1 1 d . . . H37 H 1.2472 0.9064 1.1926 0.037 Uiso 1 1 calc R . . C38 C 1.1847(3) 0.9631(2) 1.28359(18) 0.0330(8) Uani 1 1 d . . . H38A H 1.2026 0.9963 1.2512 0.050 Uiso 1 1 calc R . . H38B H 1.2165 1.0040 1.3316 0.050 Uiso 1 1 calc R . . H38C H 1.1106 0.9320 1.2706 0.050 Uiso 1 1 calc R . . C39 C 1.2168(3) 0.8537(2) 1.33512(18) 0.0339(8) Uani 1 1 d . . . H39A H 1.1484 0.8032 1.3210 0.051 Uiso 1 1 calc R . . H39B H 1.2325 0.8954 1.3798 0.051 Uiso 1 1 calc R . . H39C H 1.2666 0.8330 1.3407 0.051 Uiso 1 1 calc R . . C40 C 1.0715(3) 0.6740(2) 1.02991(17) 0.0307(7) Uani 1 1 d . . . H40 H 1.0986 0.7143 1.0059 0.037 Uiso 1 1 calc R . . C41 C 0.9109(3) 0.6070(2) 0.93291(18) 0.0345(8) Uani 1 1 d . . . H41A H 0.9514 0.6550 0.9173 0.052 Uiso 1 1 calc R . . H41B H 0.8531 0.6129 0.9383 0.052 Uiso 1 1 calc R . . H41C H 0.8859 0.5501 0.8980 0.052 Uiso 1 1 calc R . . C42 C 0.9244(3) 0.5449(2) 1.03233(18) 0.0330(8) Uani 1 1 d . . . H42A H 0.9740 0.5557 1.0774 0.050 Uiso 1 1 calc R . . H42B H 0.8998 0.4857 1.0012 0.050 Uiso 1 1 calc R . . H42C H 0.8670 0.5495 1.0401 0.050 Uiso 1 1 calc R . . C43 C 1.3351(3) 0.9165(2) 1.05676(18) 0.0340(8) Uani 1 1 d . . . H43 H 1.3990 0.9185 1.0656 0.041 Uiso 1 1 calc R . . C44 C 1.0589(3) 0.8688(2) 0.90679(18) 0.0300(7) Uani 1 1 d . . . C45 C 1.0048(3) 0.8479(2) 0.82959(17) 0.0298(7) Uani 1 1 d . . . C46 C 0.9843(3) 0.7686(2) 0.78229(17) 0.0309(7) Uani 1 1 d . . . H46 H 1.0042 0.7303 0.8005 0.037 Uiso 1 1 calc R . . C47 C 0.9348(3) 0.7446(2) 0.70862(18) 0.0322(8) Uani 1 1 d . . . H47 H 0.9243 0.6923 0.6779 0.039 Uiso 1 1 calc R . . C48 C 0.9017(3) 0.7997(2) 0.68188(17) 0.0314(8) Uani 1 1 d . . . C49 C 0.9219(3) 0.8792(2) 0.72853(17) 0.0318(8) Uani 1 1 d . . . H49 H 0.9012 0.9172 0.7104 0.038 Uiso 1 1 calc R . . C50 C 0.9722(3) 0.9028(2) 0.80161(17) 0.0302(7) Uani 1 1 d . . . H50 H 0.9843 0.9560 0.8321 0.036 Uiso 1 1 calc R . . C51 C 0.8509(3) 0.7111(2) 0.56187(17) 0.0308(7) Uani 1 1 d . . . H51A H 0.8296 0.6579 0.5772 0.037 Uiso 1 1 calc R . . H51B H 0.9211 0.7312 0.5627 0.037 Uiso 1 1 calc R . . C52 C 0.7788(3) 0.6877(2) 0.48630(17) 0.0298(7) Uani 1 1 d . . . C53 C 0.6819(3) 0.6077(2) 0.45915(17) 0.0301(7) Uani 1 1 d . . . C54 C 0.6221(3) 0.5771(2) 0.38673(17) 0.0302(7) Uani 1 1 d . . . C55 C 0.6555(3) 0.6237(2) 0.34036(18) 0.0313(7) Uani 1 1 d . . . C56 C 0.7485(3) 0.7069(2) 0.36978(17) 0.0299(7) Uani 1 1 d . . . C57 C 0.8098(3) 0.7396(2) 0.44179(17) 0.0291(7) Uani 1 1 d . . . C58 C 0.9120(3) 0.8272(2) 0.47260(18) 0.0320(8) Uani 1 1 d . . . H58A H 0.9379 0.8403 0.4350 0.048 Uiso 1 1 calc R . . H58B H 0.9613 0.8217 0.5086 0.048 Uiso 1 1 calc R . . H58C H 0.9014 0.8752 0.4937 0.048 Uiso 1 1 calc R . . C59 C 0.6482(3) 0.5562(2) 0.50928(18) 0.0322(8) Uani 1 1 d . . . H59A H 0.5802 0.5050 0.4839 0.048 Uiso 1 1 calc R . . H59B H 0.6465 0.5947 0.5485 0.048 Uiso 1 1 calc R . . H59C H 0.6964 0.5362 0.5274 0.048 Uiso 1 1 calc R . . C60 C 0.5160(3) 0.4925(2) 0.35545(19) 0.0340(8) Uani 1 1 d . . . H60A H 0.4820 0.4872 0.3903 0.041 Uiso 1 1 calc R . . H60B H 0.4725 0.4954 0.3131 0.041 Uiso 1 1 calc R . . C61 C 0.4489(3) 0.3381(2) 0.28662(19) 0.0378(9) Uani 1 1 d . . . C62 C 0.3530(3) 0.3262(2) 0.25663(17) 0.0306(7) Uani 1 1 d . . . H62 H 0.3377 0.3715 0.2712 0.037 Uiso 1 1 calc R . . C63 C 0.2765(3) 0.2448(2) 0.20320(18) 0.0368(8) Uani 1 1 d . . . H63 H 0.2113 0.2379 0.1810 0.044 Uiso 1 1 calc R . . C64 C 0.2953(3) 0.1753(2) 0.18276(18) 0.0328(8) Uani 1 1 d . . . C65 C 0.3938(3) 0.1878(2) 0.21785(19) 0.0401(9) Uani 1 1 d . . . H65 H 0.4082 0.1412 0.2063 0.048 Uiso 1 1 calc R . . C66 C 0.4702(3) 0.2686(2) 0.26942(19) 0.0397(9) Uani 1 1 d . . . H66 H 0.5355 0.2762 0.2924 0.048 Uiso 1 1 calc R . . C67 C 0.2153(3) 0.0907(2) 0.12315(17) 0.0289(7) Uani 1 1 d . . . C68 C 0.5949(3) 0.5833(2) 0.26049(17) 0.0328(8) Uani 1 1 d . . . H68A H 0.5702 0.5196 0.2462 0.049 Uiso 1 1 calc R . . H68B H 0.6391 0.6108 0.2354 0.049 Uiso 1 1 calc R . . H68C H 0.5369 0.5939 0.2492 0.049 Uiso 1 1 calc R . . C69 C 0.7808(3) 0.7589(2) 0.31884(17) 0.0308(7) Uani 1 1 d . . . H69A H 0.7202 0.7504 0.2819 0.037 Uiso 1 1 calc R . . H69B H 0.8249 0.8228 0.3447 0.037 Uiso 1 1 calc R . . C70 C 0.8659(3) 0.7545(2) 0.23453(18) 0.0310(7) Uani 1 1 d . . . C71 C 0.9280(3) 0.7285(2) 0.21089(17) 0.0310(7) Uani 1 1 d . . . H71 H 0.9444 0.6885 0.2290 0.037 Uiso 1 1 calc R . . C72 C 0.9673(3) 0.7596(2) 0.16090(17) 0.0304(7) Uani 1 1 d . . . H72 H 1.0102 0.7413 0.1458 0.037 Uiso 1 1 calc R . . C73 C 0.8387(3) 0.8136(2) 0.20679(18) 0.0323(8) Uani 1 1 d . . . H73 H 0.7956 0.8315 0.2220 0.039 Uiso 1 1 calc R . . C74 C 0.8779(3) 0.8447(2) 0.15572(18) 0.0315(8) Uani 1 1 d . . . H74 H 0.8601 0.8836 0.1368 0.038 Uiso 1 1 calc R . . C75 C 0.9415(3) 0.8198(2) 0.13285(18) 0.0316(8) Uani 1 1 d . . . C76 C 0.9853(3) 0.8596(2) 0.08145(17) 0.0299(7) Uani 1 1 d . . . Co1 Co 1.0000 1.0000 1.0000 0.02895(16) Uani 1 2 d S . . Co2 Co 1.16397(4) 0.91287(3) 1.03486(2) 0.02959(12) Uani 1 1 d . . . Co3 Co 1.45933(4) 0.67451(3) 1.11762(2) 0.03094(13) Uani 1 1 d . . . Co4 Co 1.29079(4) 0.76849(3) 1.12272(2) 0.03056(13) Uani 1 1 d . . . N1 N 0.9734(2) 0.61144(18) 0.99946(15) 0.0309(6) Uani 1 1 d . . . N2 N 1.2210(2) 0.89894(18) 1.27968(15) 0.0327(7) Uani 1 1 d . . . N3 N 1.6456(2) 0.64373(19) 1.01256(15) 0.0351(7) Uani 1 1 d . . . O1 O 1.07762(18) 0.94118(14) 0.95161(12) 0.0302(5) Uani 1 1 d . . . O2 O 1.09153(18) 0.81966(15) 0.92848(11) 0.0304(5) Uani 1 1 d . . . O3 O 1.31399(19) 0.96288(15) 1.02159(12) 0.0336(5) Uani 1 1 d . . . O4 O 1.27038(18) 0.86671(15) 1.08047(12) 0.0304(5) Uani 1 1 d . . . O5 O 1.27946(18) 0.82075(15) 1.21975(12) 0.0324(5) Uani 1 1 d . . . O6 O 1.13135(18) 0.68304(15) 1.08962(12) 0.0322(5) Uani 1 1 d . . . O7 O 1.38359(19) 0.65416(15) 1.02024(12) 0.0319(5) Uani 1 1 d . . . O8 O 1.56319(19) 0.64417(15) 1.09302(12) 0.0330(5) Uani 1 1 d . . . O9 O 0.84887(18) 0.78137(15) 0.61053(12) 0.0334(5) Uani 1 1 d . . . O10 O 0.53139(19) 0.41606(15) 0.33711(13) 0.0399(6) Uani 1 1 d . . . O11 O 0.83599(18) 0.72432(15) 0.28771(12) 0.0310(5) Uani 1 1 d . . . O12 O 0.13944(18) 0.09190(14) 0.08168(12) 0.0305(5) Uani 1 1 d . . . O13 O 0.22992(18) 0.02383(14) 0.12003(12) 0.0311(5) Uani 1 1 d . . . O14 O 0.96310(18) 0.91319(15) 0.05932(11) 0.0301(5) Uani 1 1 d . . . O15 O 1.04888(18) 0.83744(14) 0.06674(12) 0.0307(5) Uani 1 1 d . . . O16 O 1.10288(18) 0.48110(15) 0.69333(12) 0.0307(5) Uani 1 1 d . . . O17 O 0.85641(19) 0.17688(14) 0.40701(12) 0.0363(6) Uani 1 1 d . . . O18 O 1.16888(18) 0.48789(15) 0.38351(12) 0.0314(5) Uani 1 1 d . . . O19 O 1.32558(18) 0.67763(15) 0.16097(12) 0.0323(5) Uani 1 1 d . . . O20 O 1.38557(18) 0.58394(15) 0.16167(12) 0.0320(5) Uani 1 1 d . . . O21 O 0.55410(18) -0.20483(15) 0.18202(12) 0.0309(5) Uani 1 1 d . . . O22 O 0.45002(19) -0.14347(15) 0.16325(12) 0.0336(6) Uani 1 1 d . . . O23 O 1.27491(18) 0.70850(15) 1.02012(12) 0.0309(5) 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 C1 0.033(2) 0.0360(19) 0.0295(18) 0.0117(15) 0.0101(16) 0.0116(16) C2 0.035(2) 0.0338(18) 0.037(2) 0.0117(15) 0.0135(16) 0.0106(16) C3 0.033(2) 0.0338(18) 0.0322(19) 0.0110(15) 0.0131(16) 0.0108(16) C4 0.030(2) 0.0272(17) 0.0276(17) 0.0079(14) 0.0077(15) 0.0097(15) C5 0.030(2) 0.0293(17) 0.0273(17) 0.0084(13) 0.0091(15) 0.0141(15) C6 0.032(2) 0.0292(17) 0.0289(17) 0.0102(14) 0.0116(15) 0.0135(15) C7 0.032(2) 0.0318(17) 0.0287(18) 0.0108(14) 0.0110(15) 0.0117(15) C8 0.031(2) 0.0289(17) 0.0237(17) 0.0061(13) 0.0088(15) 0.0115(15) C9 0.033(2) 0.0299(17) 0.0265(18) -0.0098(13) 0.0093(15) 0.0120(16) C10 0.0274(19) 0.0311(17) 0.0289(17) 0.0094(14) 0.0082(14) 0.0107(15) C11 0.031(2) 0.0318(18) 0.0278(18) -0.0056(14) 0.0089(15) 0.0109(16) C12 0.032(2) 0.0281(17) 0.0281(17) 0.0085(13) 0.0110(15) 0.0139(15) C13 0.031(2) 0.0306(17) 0.0305(18) 0.0110(14) 0.0107(15) 0.0125(15) C14 0.0286(19) 0.0304(17) 0.0261(17) 0.0089(13) 0.0075(14) 0.0114(15) C15 0.0291(19) 0.0286(17) 0.0286(17) 0.0089(13) 0.0105(14) 0.0118(15) C16 0.031(2) 0.0281(17) 0.0287(17) 0.0090(14) 0.0109(15) 0.0102(15) C17 0.031(2) 0.0272(16) 0.0289(17) 0.0076(13) 0.0109(15) 0.0101(15) C18 0.034(2) 0.0315(17) 0.0337(19) 0.0122(14) 0.0133(16) 0.0139(16) C19 0.030(2) 0.0315(18) 0.0284(18) -0.0118(14) -0.0111(15) 0.0108(16) C20 0.030(2) 0.0314(18) 0.0281(18) -0.0095(14) 0.0081(15) 0.0102(16) C21 0.0267(19) 0.0332(18) 0.0298(18) -0.0090(14) 0.0098(15) 0.0063(15) C22 0.029(2) 0.0310(18) 0.035(2) -0.0094(15) -0.0083(16) 0.0104(16) C23 0.035(2) 0.0297(18) 0.039(2) -0.0128(15) -0.0082(17) 0.0128(17) C24 0.034(2) 0.036(2) 0.040(2) -0.0126(16) -0.0125(17) 0.0139(18) C25 0.030(2) 0.0311(18) 0.036(2) -0.0098(15) -0.0095(16) 0.0107(16) C26 0.033(2) 0.0332(18) 0.0321(19) -0.0091(14) 0.0114(16) 0.0112(16) C27 0.031(2) 0.0301(18) 0.0352(19) -0.0096(14) 0.0107(16) 0.0114(16) C28 0.030(2) 0.0315(19) 0.034(2) -0.0116(15) -0.0113(16) 0.0117(17) C29 0.034(2) 0.0299(17) 0.0307(18) 0.0090(14) 0.0131(15) 0.0136(16) C30 0.0293(19) 0.0283(16) 0.0280(17) 0.0093(13) 0.0104(14) 0.0120(15) C31 0.0295(19) 0.0289(16) 0.0264(17) 0.0101(13) 0.0108(14) 0.0110(15) C32 0.031(2) 0.0296(17) 0.0284(17) 0.0097(14) 0.0099(15) 0.0132(15) C33 0.031(2) 0.0286(17) 0.0314(18) 0.0113(14) 0.0105(15) 0.0125(15) C34 0.032(2) 0.0331(18) 0.0339(18) 0.0141(15) 0.0140(15) 0.0142(16) C35 0.034(2) 0.0332(18) 0.0324(18) 0.0146(14) 0.0138(16) 0.0147(16) C36 0.030(2) 0.0281(17) 0.0312(18) 0.0109(14) 0.0102(15) 0.0100(15) C37 0.031(2) 0.0306(17) 0.0285(18) 0.0104(14) 0.0102(15) 0.0126(16) C38 0.031(2) 0.0305(17) 0.0312(18) 0.0087(14) 0.0109(15) 0.0107(15) C39 0.035(2) 0.0311(17) 0.0321(18) 0.0114(14) 0.0125(15) 0.0129(16) C40 0.033(2) 0.0274(17) 0.0283(18) 0.0084(13) 0.0102(15) 0.0123(15) C41 0.030(2) 0.0331(18) 0.0312(18) 0.0096(14) 0.0083(15) 0.0098(16) C42 0.033(2) 0.0301(17) 0.0305(18) 0.0089(14) 0.0096(15) 0.0118(15) C43 0.031(2) 0.0334(18) 0.0304(18) 0.0120(15) 0.0106(15) 0.0096(16) C44 0.0227(18) 0.0284(17) 0.0309(18) 0.0082(14) 0.0078(14) 0.0072(14) C45 0.031(2) 0.0299(17) 0.0246(17) 0.0089(13) 0.0093(14) 0.0123(15) C46 0.033(2) 0.0299(17) 0.0274(17) 0.0103(14) 0.0105(15) 0.0128(15) C47 0.030(2) 0.0315(17) 0.0290(18) 0.0095(14) 0.0084(15) 0.0117(15) C48 0.029(2) 0.0309(17) 0.0272(17) 0.0083(14) 0.0075(14) 0.0108(15) C49 0.033(2) 0.0314(17) 0.0300(18) 0.0109(14) 0.0106(15) 0.0148(16) C50 0.0288(19) 0.0312(17) 0.0254(17) 0.0087(13) 0.0079(14) 0.0114(15) C51 0.031(2) 0.0293(17) 0.0279(17) 0.0048(13) 0.0101(15) 0.0128(15) C52 0.0280(19) 0.0325(17) 0.0262(17) 0.0090(14) 0.0105(14) 0.0120(15) C53 0.0280(19) 0.0295(17) 0.0278(17) 0.0085(13) 0.0086(14) 0.0109(15) C54 0.0291(19) 0.0309(17) 0.0290(17) 0.0096(14) 0.0105(15) 0.0134(15) C55 0.0266(19) 0.0298(17) 0.0318(18) 0.0098(14) 0.0094(15) 0.0097(15) C56 0.0254(19) 0.0292(17) 0.0311(18) 0.0110(14) 0.0095(14) 0.0097(15) C57 0.0280(19) 0.0259(16) 0.0282(17) 0.0061(13) 0.0101(14) 0.0097(15) C58 0.031(2) 0.0288(17) 0.0291(18) 0.0075(14) 0.0091(15) 0.0096(15) C59 0.032(2) 0.0307(17) 0.0307(18) 0.0103(14) 0.0117(15) 0.0117(15) C60 0.0280(19) 0.0287(17) 0.0310(18) -0.0108(13) 0.0100(15) 0.0096(15) C61 0.030(2) 0.0272(17) 0.0318(19) -0.0090(14) -0.0088(15) 0.0110(16) C62 0.033(2) 0.0257(16) 0.0292(17) 0.0077(13) 0.0106(15) 0.0114(15) C63 0.029(2) 0.0298(18) 0.0286(18) -0.0074(14) -0.0084(15) 0.0109(16) C64 0.031(2) 0.0253(16) 0.0293(18) -0.0095(13) 0.0107(15) 0.0098(15) C65 0.030(2) 0.0307(18) 0.033(2) -0.0119(15) -0.0113(16) 0.0137(16) C66 0.029(2) 0.0287(18) 0.034(2) -0.0087(14) -0.0098(15) 0.0097(16) C67 0.028(2) 0.0276(17) 0.0261(17) 0.0084(13) 0.0071(15) 0.0105(15) C68 0.032(2) 0.0305(17) 0.0277(17) 0.0091(14) 0.0093(15) 0.0094(15) C69 0.031(2) 0.0281(17) 0.0281(17) 0.0093(13) 0.0095(15) 0.0106(15) C70 0.030(2) 0.0322(17) 0.0317(18) 0.0142(14) 0.0135(15) 0.0134(15) C71 0.031(2) 0.0297(17) 0.0286(17) 0.0113(14) 0.0106(15) 0.0115(15) C72 0.031(2) 0.0302(17) 0.0285(17) 0.0104(14) 0.0101(15) 0.0138(15) C73 0.033(2) 0.0336(18) 0.0322(18) 0.0150(14) 0.0145(15) 0.0147(16) C74 0.034(2) 0.0311(17) 0.0305(18) 0.0118(14) 0.0118(15) 0.0157(16) C75 0.031(2) 0.0294(17) 0.0299(18) 0.0096(14) 0.0104(15) 0.0107(15) C76 0.032(2) 0.0269(16) 0.0266(17) 0.0089(13) 0.0084(15) 0.0116(15) Co1 0.0289(4) 0.0276(3) 0.0261(3) 0.0086(3) 0.0091(3) 0.0106(3) Co2 0.0296(3) 0.0280(2) 0.0272(2) 0.00909(18) 0.0096(2) 0.0110(2) Co3 0.0292(3) 0.0298(2) 0.0282(2) 0.00893(19) 0.0088(2) 0.0106(2) Co4 0.0306(3) 0.0287(2) 0.0281(2) 0.00925(18) 0.0094(2) 0.0114(2) N1 0.0287(17) 0.0287(14) 0.0316(15) 0.0103(12) 0.0114(12) 0.0102(13) N2 0.0314(17) 0.0306(15) 0.0290(15) 0.0066(12) 0.0094(13) 0.0110(13) N3 0.0327(18) 0.0343(15) 0.0322(16) 0.0088(12) 0.0107(13) 0.0124(14) O1 0.0290(13) 0.0292(12) 0.0290(12) 0.0103(10) 0.0116(10) 0.0102(10) O2 0.0312(14) 0.0303(12) 0.0279(12) 0.0115(10) 0.0101(10) 0.0132(11) O3 0.0322(14) 0.0342(12) 0.0316(13) 0.0132(10) 0.0130(11) 0.0121(11) O4 0.0284(13) 0.0299(12) 0.0306(12) 0.0104(10) 0.0109(10) 0.0119(10) O5 0.0342(14) 0.0312(12) 0.0274(12) 0.0083(10) 0.0093(10) 0.0136(11) O6 0.0326(14) 0.0303(12) 0.0299(13) 0.0082(10) 0.0124(11) 0.0120(11) O7 0.0319(14) 0.0318(12) 0.0277(12) 0.0090(10) 0.0105(10) 0.0121(11) O8 0.0322(14) 0.0323(12) 0.0305(12) 0.0093(10) 0.0098(10) 0.0134(11) O9 0.0301(13) 0.0292(12) 0.0269(12) -0.0088(9) 0.0071(10) 0.0109(11) O10 0.0293(14) 0.0290(12) 0.0340(13) -0.0106(10) -0.0118(11) 0.0113(11) O11 0.0307(14) 0.0327(12) 0.0307(12) 0.0140(10) 0.0128(10) 0.0140(11) O12 0.0313(14) 0.0279(12) 0.0292(12) 0.0098(9) 0.0109(11) 0.0117(10) O13 0.0323(14) 0.0269(12) 0.0301(12) 0.0087(9) 0.0105(10) 0.0118(10) O14 0.0289(14) 0.0311(12) 0.0268(12) 0.0103(10) 0.0099(10) 0.0113(11) O15 0.0296(14) 0.0284(12) 0.0287(12) 0.0083(9) 0.0099(10) 0.0102(10) O16 0.0291(13) 0.0324(12) 0.0277(12) 0.0090(10) 0.0101(10) 0.0127(10) O17 0.0328(15) 0.0263(12) 0.0314(13) 0.0070(10) -0.0096(10) 0.0110(11) O18 0.0308(14) 0.0292(12) 0.0312(12) 0.0096(10) 0.0116(10) 0.0120(11) O19 0.0320(14) 0.0315(12) 0.0303(12) 0.0117(10) 0.0109(10) 0.0124(11) O20 0.0300(14) 0.0325(12) 0.0303(12) 0.0110(10) 0.0117(10) 0.0119(11) O21 0.0292(14) 0.0298(12) 0.0282(12) 0.0089(10) 0.0088(10) 0.0106(11) O22 0.0314(15) 0.0289(12) 0.0304(13) 0.0088(10) 0.0078(11) 0.0083(11) O23 0.0318(14) 0.0280(11) 0.0263(12) 0.0070(9) 0.0086(10) 0.0107(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 C1 N3 1.300(5) . ? C1 O8 1.305(4) . ? C1 H1 0.9300 . ? C2 N3 1.477(4) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 N3 1.432(4) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 O23 1.242(4) . ? C4 O7 1.268(4) . ? C4 C5 1.506(4) . ? C5 C6 1.372(5) . ? C5 C10 1.374(5) . ? C6 C7 1.400(5) . ? C6 H6 0.9300 . ? C7 C8 1.390(5) . ? C7 H7 0.9300 . ? C8 C9 1.348(5) . ? C8 O16 1.381(4) . ? C9 C10 1.385(5) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 O16 1.457(4) . ? C11 C12 1.569(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C17 1.418(5) . ? C12 C13 1.420(4) . ? C13 C14 1.458(5) . ? C13 C19 1.554(5) . ? C14 C15 1.414(5) . ? C14 C29 1.501(4) . ? C15 C16 1.381(4) . ? C15 C20 1.518(5) . ? C16 C17 1.401(5) . ? C16 C21 1.537(5) . ? C17 C18 1.547(4) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 O17 1.446(4) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 O17 1.351(4) . ? C22 C23 1.387(5) . ? C22 C27 1.391(5) . ? C23 C24 1.386(5) . ? C23 H23 0.9300 . ? C24 C25 1.387(6) . ? C24 H24 0.9300 . ? C25 C26 1.394(5) . ? C25 C28 1.512(4) . ? C26 C27 1.379(5) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 O22 1.229(4) . ? C28 O21 1.258(4) . ? C29 O18 1.445(4) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 O18 1.360(4) . ? C30 C35 1.396(5) . ? C30 C31 1.402(4) . ? C31 C32 1.371(4) . ? C31 H31 0.9300 . ? C32 C33 1.386(5) . ? C32 H32 0.9300 . ? C33 C34 1.375(5) . ? C33 C36 1.489(4) . ? C34 C35 1.372(4) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 O19 1.234(4) . ? C36 O20 1.266(4) . ? C37 O5 1.248(4) . ? C37 N2 1.303(4) . ? C37 H37 0.9300 . ? C38 N2 1.435(4) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 N2 1.475(4) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 O6 1.261(4) . ? C40 N1 1.314(4) . ? C40 H40 0.9300 . ? C41 N1 1.414(4) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 N1 1.450(4) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 O3 1.248(4) . ? C43 O4 1.265(4) . ? C43 Co2 2.509(4) . ? C43 H43 0.9300 . ? C44 O2 1.242(4) . ? C44 O1 1.284(4) . ? C44 C45 1.475(5) . ? C44 Co2 2.473(3) . ? C45 C50 1.383(5) . ? C45 C46 1.391(5) . ? C46 C47 1.392(5) . ? C46 H46 0.9300 . ? C47 C48 1.380(5) . ? C47 H47 0.9300 . ? C48 O9 1.376(4) . ? C48 C49 1.389(5) . ? C49 C50 1.384(5) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? C51 O9 1.444(4) . ? C51 C52 1.515(5) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C57 1.403(4) . ? C52 C53 1.412(5) . ? C53 C54 1.389(5) . ? C53 C59 1.507(4) . ? C54 C55 1.394(4) . ? C54 C60 1.522(5) . ? C55 C56 1.408(5) . ? C55 C68 1.513(5) . ? C56 C57 1.385(5) . ? C56 C69 1.521(4) . ? C57 C58 1.515(4) . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 O10 1.441(4) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 C62 1.347(5) . ? C61 O10 1.375(4) . ? C61 C66 1.383(5) . ? C62 C63 1.402(4) . ? C62 H62 0.9300 . ? C63 C64 1.371(5) . ? C63 H63 0.9300 . ? C64 C65 1.397(5) . ? C64 C67 1.493(4) . ? C65 C66 1.382(4) . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C67 O12 1.261(4) . ? C67 O13 1.261(4) . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C69 O11 1.425(4) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 C71 1.358(5) . ? C70 O11 1.371(4) . ? C70 C73 1.403(5) . ? C71 C72 1.376(4) . ? C71 H71 0.9300 . ? C72 C75 1.413(5) . ? C72 H72 0.9300 . ? C73 C74 1.396(4) . ? C73 H73 0.9300 . ? C74 C75 1.363(5) . ? C74 H74 0.9300 . ? C75 C76 1.486(4) . ? C76 O14 1.227(4) . ? C76 O15 1.265(4) . ? Co1 O14 2.062(2) 2_776 ? Co1 O14 2.062(2) 1_556 ? Co1 O12 2.065(2) 2_666 ? Co1 O12 2.065(2) 1_666 ? Co1 O1 2.160(2) . ? Co1 O1 2.160(2) 2_777 ? Co2 O13 2.008(2) 1_666 ? Co2 O15 2.026(2) 1_556 ? Co2 O1 2.134(2) . ? Co2 O2 2.141(2) . ? Co2 O4 2.176(2) . ? Co2 O3 2.182(2) . ? Co3 O7 1.909(2) . ? Co3 O21 1.925(2) 1_666 ? Co3 O20 1.998(2) 1_556 ? Co3 O8 2.012(2) . ? Co4 O23 2.066(2) . ? Co4 O19 2.066(2) 1_556 ? Co4 O22 2.079(3) 1_666 ? Co4 O6 2.083(2) . ? Co4 O5 2.102(2) . ? Co4 O4 2.127(2) . ? O12 Co1 2.065(2) 1_444 ? O13 Co2 2.008(2) 1_444 ? O14 Co1 2.062(2) 1_554 ? O15 Co2 2.026(2) 1_554 ? O19 Co4 2.066(2) 1_554 ? O20 Co3 1.998(2) 1_554 ? O21 Co3 1.925(2) 1_444 ? O22 Co4 2.079(2) 1_444 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 C1 O8 123.6(3) . . ? N3 C1 H1 118.2 . . ? O8 C1 H1 118.2 . . ? N3 C2 H2A 109.5 . . ? N3 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N3 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N3 C3 H3A 109.5 . . ? N3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O23 C4 O7 125.0(3) . . ? O23 C4 C5 119.8(3) . . ? O7 C4 C5 115.3(3) . . ? C6 C5 C10 119.9(3) . . ? C6 C5 C4 120.0(3) . . ? C10 C5 C4 120.0(3) . . ? C5 C6 C7 120.5(3) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C8 C7 C6 117.6(3) . . ? C8 C7 H7 121.2 . . ? C6 C7 H7 121.2 . . ? C9 C8 O16 124.0(3) . . ? C9 C8 C7 122.2(3) . . ? O16 C8 C7 113.8(3) . . ? C8 C9 C10 119.3(3) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C5 C10 C9 120.4(3) . . ? C5 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? O16 C11 C12 103.0(3) . . ? O16 C11 H11A 111.2 . . ? C12 C11 H11A 111.2 . . ? O16 C11 H11B 111.2 . . ? C12 C11 H11B 111.2 . . ? H11A C11 H11B 109.1 . . ? C17 C12 C13 123.0(3) . . ? C17 C12 C11 117.8(3) . . ? C13 C12 C11 118.9(3) . . ? C12 C13 C14 114.0(3) . . ? C12 C13 C19 129.7(3) . . ? C14 C13 C19 113.8(3) . . ? C15 C14 C13 122.4(3) . . ? C15 C14 C29 118.3(3) . . ? C13 C14 C29 119.2(3) . . ? C16 C15 C14 119.0(3) . . ? C16 C15 C20 120.0(3) . . ? C14 C15 C20 121.0(3) . . ? C15 C16 C17 121.7(3) . . ? C15 C16 C21 117.3(3) . . ? C17 C16 C21 121.0(3) . . ? C16 C17 C12 118.5(3) . . ? C16 C17 C18 118.6(3) . . ? C12 C17 C18 122.9(3) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C13 C19 H19A 109.5 . . ? C13 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C13 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O17 C21 C16 104.5(3) . . ? O17 C21 H21A 110.9 . . ? C16 C21 H21A 110.9 . . ? O17 C21 H21B 110.9 . . ? C16 C21 H21B 110.9 . . ? H21A C21 H21B 108.9 . . ? O17 C22 C23 114.3(3) . . ? O17 C22 C27 126.0(3) . . ? C23 C22 C27 119.8(3) . . ? C24 C23 C22 119.9(4) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C25 120.5(4) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C24 C25 C26 119.3(3) . . ? C24 C25 C28 120.6(3) . . ? C26 C25 C28 120.1(3) . . ? C27 C26 C25 120.3(4) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C22 120.2(3) . . ? C26 C27 H27 119.9 . . ? C22 C27 H27 119.9 . . ? O22 C28 O21 129.6(3) . . ? O22 C28 C25 116.3(3) . . ? O21 C28 C25 114.1(3) . . ? O18 C29 C14 106.5(3) . . ? O18 C29 H29A 110.4 . . ? C14 C29 H29A 110.4 . . ? O18 C29 H29B 110.4 . . ? C14 C29 H29B 110.4 . . ? H29A C29 H29B 108.6 . . ? O18 C30 C35 114.9(3) . . ? O18 C30 C31 125.8(3) . . ? C35 C30 C31 119.3(3) . . ? C32 C31 C30 118.9(3) . . ? C32 C31 H31 120.5 . . ? C30 C31 H31 120.5 . . ? C31 C32 C33 121.8(3) . . ? C31 C32 H32 119.1 . . ? C33 C32 H32 119.1 . . ? C34 C33 C32 119.0(3) . . ? C34 C33 C36 119.5(3) . . ? C32 C33 C36 121.3(3) . . ? C35 C34 C33 120.7(3) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? C34 C35 C30 120.3(3) . . ? C34 C35 H35 119.9 . . ? C30 C35 H35 119.9 . . ? O19 C36 O20 120.7(3) . . ? O19 C36 C33 121.2(3) . . ? O20 C36 C33 118.0(3) . . ? O5 C37 N2 124.7(3) . . ? O5 C37 H37 117.7 . . ? N2 C37 H37 117.7 . . ? N2 C38 H38A 109.5 . . ? N2 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N2 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N2 C39 H39A 109.5 . . ? N2 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N2 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O6 C40 N1 124.2(3) . . ? O6 C40 H40 117.9 . . ? N1 C40 H40 117.9 . . ? N1 C41 H41A 109.5 . . ? N1 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N1 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N1 C42 H42A 109.5 . . ? N1 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N1 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O3 C43 O4 120.5(3) . . ? O3 C43 Co2 60.42(19) . . ? O4 C43 Co2 60.14(19) . . ? O3 C43 H43 119.7 . . ? O4 C43 H43 119.7 . . ? Co2 C43 H43 179.1 . . ? O2 C44 O1 119.5(3) . . ? O2 C44 C45 120.6(3) . . ? O1 C44 C45 119.8(3) . . ? O2 C44 Co2 59.96(16) . . ? O1 C44 Co2 59.61(16) . . ? C45 C44 Co2 174.9(2) . . ? C50 C45 C46 118.0(3) . . ? C50 C45 C44 123.4(3) . . ? C46 C45 C44 118.6(3) . . ? C45 C46 C47 122.1(3) . . ? C45 C46 H46 119.0 . . ? C47 C46 H46 119.0 . . ? C48 C47 C46 119.0(3) . . ? C48 C47 H47 120.5 . . ? C46 C47 H47 120.5 . . ? O9 C48 C47 124.2(3) . . ? O9 C48 C49 116.4(3) . . ? C47 C48 C49 119.5(3) . . ? C50 C49 C48 121.0(3) . . ? C50 C49 H49 119.5 . . ? C48 C49 H49 119.5 . . ? C45 C50 C49 120.4(3) . . ? C45 C50 H50 119.8 . . ? C49 C50 H50 119.8 . . ? O9 C51 C52 110.4(3) . . ? O9 C51 H51A 109.6 . . ? C52 C51 H51A 109.6 . . ? O9 C51 H51B 109.6 . . ? C52 C51 H51B 109.6 . . ? H51A C51 H51B 108.1 . . ? C57 C52 C53 120.1(3) . . ? C57 C52 C51 121.4(3) . . ? C53 C52 C51 118.3(3) . . ? C54 C53 C52 119.2(3) . . ? C54 C53 C59 121.9(3) . . ? C52 C53 C59 118.9(3) . . ? C53 C54 C55 121.4(3) . . ? C53 C54 C60 121.1(3) . . ? C55 C54 C60 117.5(3) . . ? C54 C55 C56 118.1(3) . . ? C54 C55 C68 120.2(3) . . ? C56 C55 C68 121.6(3) . . ? C57 C56 C55 121.8(3) . . ? C57 C56 C69 120.9(3) . . ? C55 C56 C69 117.3(3) . . ? C56 C57 C52 118.9(3) . . ? C56 C57 C58 121.6(3) . . ? C52 C57 C58 119.4(3) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C53 C59 H59A 109.5 . . ? C53 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C53 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? O10 C60 C54 107.8(3) . . ? O10 C60 H60A 110.1 . . ? C54 C60 H60A 110.1 . . ? O10 C60 H60B 110.1 . . ? C54 C60 H60B 110.1 . . ? H60A C60 H60B 108.5 . . ? C62 C61 O10 124.6(3) . . ? C62 C61 C66 120.7(3) . . ? O10 C61 C66 114.6(3) . . ? C61 C62 C63 119.2(3) . . ? C61 C62 H62 120.4 . . ? C63 C62 H62 120.4 . . ? C64 C63 C62 121.8(3) . . ? C64 C63 H63 119.1 . . ? C62 C63 H63 119.1 . . ? C63 C64 C65 117.4(3) . . ? C63 C64 C67 121.5(3) . . ? C65 C64 C67 121.0(3) . . ? C66 C65 C64 121.0(3) . . ? C66 C65 H65 119.5 . . ? C64 C65 H65 119.5 . . ? C65 C66 C61 119.6(3) . . ? C65 C66 H66 120.2 . . ? C61 C66 H66 120.2 . . ? O12 C67 O13 126.2(3) . . ? O12 C67 C64 117.9(3) . . ? O13 C67 C64 115.9(3) . . ? C55 C68 H68A 109.5 . . ? C55 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C55 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? O11 C69 C56 106.6(3) . . ? O11 C69 H69A 110.4 . . ? C56 C69 H69A 110.4 . . ? O11 C69 H69B 110.4 . . ? C56 C69 H69B 110.4 . . ? H69A C69 H69B 108.6 . . ? C71 C70 O11 117.6(3) . . ? C71 C70 C73 119.8(3) . . ? O11 C70 C73 122.5(3) . . ? C70 C71 C72 122.0(3) . . ? C70 C71 H71 119.0 . . ? C72 C71 H71 119.0 . . ? C71 C72 C75 119.0(3) . . ? C71 C72 H72 120.5 . . ? C75 C72 H72 120.5 . . ? C74 C73 C70 118.3(3) . . ? C74 C73 H73 120.9 . . ? C70 C73 H73 120.9 . . ? C75 C74 C73 121.9(3) . . ? C75 C74 H74 119.1 . . ? C73 C74 H74 119.1 . . ? C74 C75 C72 119.0(3) . . ? C74 C75 C76 119.0(3) . . ? C72 C75 C76 122.0(3) . . ? O14 C76 O15 124.8(3) . . ? O14 C76 C75 120.3(3) . . ? O15 C76 C75 114.8(3) . . ? O14 Co1 O14 180.00(10) 2_776 1_556 ? O14 Co1 O12 92.03(9) 2_776 2_666 ? O14 Co1 O12 87.97(9) 1_556 2_666 ? O14 Co1 O12 87.97(9) 2_776 1_666 ? O14 Co1 O12 92.03(9) 1_556 1_666 ? O12 Co1 O12 180.000(1) 2_666 1_666 ? O14 Co1 O1 85.50(9) 2_776 . ? O14 Co1 O1 94.50(9) 1_556 . ? O12 Co1 O1 89.80(9) 2_666 . ? O12 Co1 O1 90.20(9) 1_666 . ? O14 Co1 O1 94.50(9) 2_776 2_777 ? O14 Co1 O1 85.50(9) 1_556 2_777 ? O12 Co1 O1 90.20(9) 2_666 2_777 ? O12 Co1 O1 89.80(9) 1_666 2_777 ? O1 Co1 O1 180.00(10) . 2_777 ? O13 Co2 O15 95.47(9) 1_666 1_556 ? O13 Co2 O1 104.11(9) 1_666 . ? O15 Co2 O1 99.83(9) 1_556 . ? O13 Co2 O2 164.30(9) 1_666 . ? O15 Co2 O2 93.22(9) 1_556 . ? O1 Co2 O2 61.41(9) . . ? O13 Co2 O4 93.61(9) 1_666 . ? O15 Co2 O4 96.15(9) 1_556 . ? O1 Co2 O4 154.75(9) . . ? O2 Co2 O4 98.44(9) . . ? O13 Co2 O3 87.77(9) 1_666 . ? O15 Co2 O3 156.22(9) 1_556 . ? O1 Co2 O3 102.20(9) . . ? O2 Co2 O3 89.54(9) . . ? O4 Co2 O3 60.10(9) . . ? O13 Co2 C44 135.03(10) 1_666 . ? O15 Co2 C44 98.09(10) 1_556 . ? O1 Co2 C44 31.28(10) . . ? O2 Co2 C44 30.14(10) . . ? O4 Co2 C44 126.95(10) . . ? O3 Co2 C44 96.11(10) . . ? O13 Co2 C43 90.47(11) 1_666 . ? O15 Co2 C43 126.43(10) 1_556 . ? O1 Co2 C43 130.05(10) . . ? O2 Co2 C43 94.86(10) . . ? O4 Co2 C43 30.29(9) . . ? O3 Co2 C43 29.82(9) . . ? C44 Co2 C43 114.25(11) . . ? O7 Co3 O21 120.69(10) . 1_666 ? O7 Co3 O20 115.22(10) . 1_556 ? O21 Co3 O20 115.93(9) 1_666 1_556 ? O7 Co3 O8 93.76(10) . . ? O21 Co3 O8 98.59(10) 1_666 . ? O20 Co3 O8 106.65(10) 1_556 . ? O23 Co4 O19 91.95(9) . 1_556 ? O23 Co4 O22 98.74(9) . 1_666 ? O19 Co4 O22 86.50(9) 1_556 1_666 ? O23 Co4 O6 85.39(9) . . ? O19 Co4 O6 92.86(9) 1_556 . ? O22 Co4 O6 175.84(9) 1_666 . ? O23 Co4 O5 170.23(10) . . ? O19 Co4 O5 91.56(9) 1_556 . ? O22 Co4 O5 90.58(9) 1_666 . ? O6 Co4 O5 85.33(9) . . ? O23 Co4 O4 85.05(9) . . ? O19 Co4 O4 173.54(9) 1_556 . ? O22 Co4 O4 88.30(9) 1_666 . ? O6 Co4 O4 92.61(9) . . ? O5 Co4 O4 92.32(9) . . ? C40 N1 C41 120.7(3) . . ? C40 N1 C42 122.0(3) . . ? C41 N1 C42 117.3(3) . . ? C37 N2 C38 121.6(3) . . ? C37 N2 C39 121.8(3) . . ? C38 N2 C39 116.4(3) . . ? C1 N3 C3 119.5(3) . . ? C1 N3 C2 121.0(3) . . ? C3 N3 C2 119.0(3) . . ? C44 O1 Co2 89.11(19) . . ? C44 O1 Co1 141.2(2) . . ? Co2 O1 Co1 105.73(9) . . ? C44 O2 Co2 89.90(19) . . ? C43 O3 Co2 89.8(2) . . ? C43 O4 Co4 121.4(2) . . ? C43 O4 Co2 89.6(2) . . ? Co4 O4 Co2 147.35(12) . . ? C37 O5 Co4 121.8(2) . . ? C40 O6 Co4 120.2(2) . . ? C4 O7 Co3 134.2(2) . . ? C1 O8 Co3 117.7(2) . . ? C48 O9 C51 114.9(3) . . ? C61 O10 C60 117.6(3) . . ? C70 O11 C69 118.4(2) . . ? C67 O12 Co1 137.4(2) . 1_444 ? C67 O13 Co2 126.4(2) . 1_444 ? C76 O14 Co1 142.2(2) . 1_554 ? C76 O15 Co2 124.7(2) . 1_554 ? C8 O16 C11 113.6(3) . . ? C22 O17 C21 114.2(3) . . ? C30 O18 C29 119.2(2) . . ? C36 O19 Co4 170.6(2) . 1_554 ? C36 O20 Co3 100.07(19) . 1_554 ? C28 O21 Co3 124.5(2) . 1_444 ? C28 O22 Co4 139.2(2) . 1_444 ? C4 O23 Co4 139.3(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O23 C4 C5 C6 -11.6(5) . . . . ? O7 C4 C5 C6 168.8(3) . . . . ? O23 C4 C5 C10 172.2(3) . . . . ? O7 C4 C5 C10 -7.3(4) . . . . ? C10 C5 C6 C7 -2.4(5) . . . . ? C4 C5 C6 C7 -178.6(3) . . . . ? C5 C6 C7 C8 0.1(5) . . . . ? C6 C7 C8 C9 2.2(5) . . . . ? C6 C7 C8 O16 -178.3(3) . . . . ? O16 C8 C9 C10 178.5(3) . . . . ? C7 C8 C9 C10 -2.0(5) . . . . ? C6 C5 C10 C9 2.6(5) . . . . ? C4 C5 C10 C9 178.8(3) . . . . ? C8 C9 C10 C5 -0.4(5) . . . . ? O16 C11 C12 C17 -71.9(4) . . . . ? O16 C11 C12 C13 102.0(3) . . . . ? C17 C12 C13 C14 -13.8(5) . . . . ? C11 C12 C13 C14 172.7(3) . . . . ? C17 C12 C13 C19 -174.6(3) . . . . ? C11 C12 C13 C19 11.8(5) . . . . ? C12 C13 C14 C15 10.2(5) . . . . ? C19 C13 C14 C15 174.2(3) . . . . ? C12 C13 C14 C29 -173.7(3) . . . . ? C19 C13 C14 C29 -9.7(5) . . . . ? C13 C14 C15 C16 -1.0(5) . . . . ? C29 C14 C15 C16 -177.2(3) . . . . ? C13 C14 C15 C20 -179.1(3) . . . . ? C29 C14 C15 C20 4.7(5) . . . . ? C14 C15 C16 C17 -5.6(5) . . . . ? C20 C15 C16 C17 172.5(3) . . . . ? C14 C15 C16 C21 175.8(3) . . . . ? C20 C15 C16 C21 -6.0(5) . . . . ? C15 C16 C17 C12 2.3(5) . . . . ? C21 C16 C17 C12 -179.2(3) . . . . ? C15 C16 C17 C18 -177.3(3) . . . . ? C21 C16 C17 C18 1.2(5) . . . . ? C13 C12 C17 C16 8.2(5) . . . . ? C11 C12 C17 C16 -178.2(3) . . . . ? C13 C12 C17 C18 -172.3(3) . . . . ? C11 C12 C17 C18 1.3(5) . . . . ? C15 C16 C21 O17 91.1(4) . . . . ? C17 C16 C21 O17 -87.5(4) . . . . ? O17 C22 C23 C24 -179.3(4) . . . . ? C27 C22 C23 C24 -0.3(6) . . . . ? C22 C23 C24 C25 -0.2(7) . . . . ? C23 C24 C25 C26 0.6(6) . . . . ? C23 C24 C25 C28 179.9(4) . . . . ? C24 C25 C26 C27 -0.4(6) . . . . ? C28 C25 C26 C27 -179.8(4) . . . . ? C25 C26 C27 C22 -0.1(6) . . . . ? O17 C22 C27 C26 179.3(4) . . . . ? C23 C22 C27 C26 0.5(6) . . . . ? C24 C25 C28 O22 -161.2(4) . . . . ? C26 C25 C28 O22 18.2(6) . . . . ? C24 C25 C28 O21 20.2(6) . . . . ? C26 C25 C28 O21 -160.5(4) . . . . ? C15 C14 C29 O18 -82.8(4) . . . . ? C13 C14 C29 O18 100.9(3) . . . . ? O18 C30 C31 C32 178.1(3) . . . . ? C35 C30 C31 C32 -1.0(5) . . . . ? C30 C31 C32 C33 -1.1(5) . . . . ? C31 C32 C33 C34 1.9(5) . . . . ? C31 C32 C33 C36 -173.5(3) . . . . ? C32 C33 C34 C35 -0.5(5) . . . . ? C36 C33 C34 C35 174.9(3) . . . . ? C33 C34 C35 C30 -1.6(5) . . . . ? O18 C30 C35 C34 -176.9(3) . . . . ? C31 C30 C35 C34 2.3(5) . . . . ? C34 C33 C36 O19 179.8(3) . . . . ? C32 C33 C36 O19 -4.8(5) . . . . ? C34 C33 C36 O20 -4.4(5) . . . . ? C32 C33 C36 O20 171.0(3) . . . . ? O2 C44 C45 C50 -175.9(3) . . . . ? O1 C44 C45 C50 0.1(5) . . . . ? Co2 C44 C45 C50 -81(3) . . . . ? O2 C44 C45 C46 4.8(5) . . . . ? O1 C44 C45 C46 -179.2(3) . . . . ? Co2 C44 C45 C46 99(3) . . . . ? C50 C45 C46 C47 1.5(5) . . . . ? C44 C45 C46 C47 -179.1(3) . . . . ? C45 C46 C47 C48 -2.4(5) . . . . ? C46 C47 C48 O9 -177.6(3) . . . . ? C46 C47 C48 C49 2.5(5) . . . . ? O9 C48 C49 C50 178.4(3) . . . . ? C47 C48 C49 C50 -1.8(5) . . . . ? C46 C45 C50 C49 -0.7(5) . . . . ? C44 C45 C50 C49 180.0(3) . . . . ? C48 C49 C50 C45 0.8(5) . . . . ? O9 C51 C52 C57 81.9(4) . . . . ? O9 C51 C52 C53 -103.3(3) . . . . ? C57 C52 C53 C54 5.5(5) . . . . ? C51 C52 C53 C54 -169.4(3) . . . . ? C57 C52 C53 C59 -176.7(3) . . . . ? C51 C52 C53 C59 8.4(5) . . . . ? C52 C53 C54 C55 -0.2(5) . . . . ? C59 C53 C54 C55 -177.9(3) . . . . ? C52 C53 C54 C60 -178.4(3) . . . . ? C59 C53 C54 C60 3.9(5) . . . . ? C53 C54 C55 C56 -4.7(5) . . . . ? C60 C54 C55 C56 173.6(3) . . . . ? C53 C54 C55 C68 173.0(3) . . . . ? C60 C54 C55 C68 -8.7(5) . . . . ? C54 C55 C56 C57 4.4(5) . . . . ? C68 C55 C56 C57 -173.2(3) . . . . ? C54 C55 C56 C69 -177.0(3) . . . . ? C68 C55 C56 C69 5.4(5) . . . . ? C55 C56 C57 C52 0.8(5) . . . . ? C69 C56 C57 C52 -177.8(3) . . . . ? C55 C56 C57 C58 177.5(3) . . . . ? C69 C56 C57 C58 -1.1(5) . . . . ? C53 C52 C57 C56 -5.7(5) . . . . ? C51 C52 C57 C56 168.9(3) . . . . ? C53 C52 C57 C58 177.5(3) . . . . ? C51 C52 C57 C58 -7.8(5) . . . . ? C53 C54 C60 O10 -86.2(4) . . . . ? C55 C54 C60 O10 95.5(4) . . . . ? O10 C61 C62 C63 177.1(3) . . . . ? C66 C61 C62 C63 -5.2(6) . . . . ? C61 C62 C63 C64 2.9(6) . . . . ? C62 C63 C64 C65 0.7(6) . . . . ? C62 C63 C64 C67 -176.7(3) . . . . ? C63 C64 C65 C66 -2.1(6) . . . . ? C67 C64 C65 C66 175.3(3) . . . . ? C64 C65 C66 C61 0.0(6) . . . . ? C62 C61 C66 C65 3.8(6) . . . . ? O10 C61 C66 C65 -178.3(4) . . . . ? C63 C64 C67 O12 15.4(5) . . . . ? C65 C64 C67 O12 -161.9(3) . . . . ? C63 C64 C67 O13 -163.5(3) . . . . ? C65 C64 C67 O13 19.2(5) . . . . ? C57 C56 C69 O11 93.5(4) . . . . ? C55 C56 C69 O11 -85.2(4) . . . . ? O11 C70 C71 C72 -176.0(3) . . . . ? C73 C70 C71 C72 1.2(5) . . . . ? C70 C71 C72 C75 -0.6(5) . . . . ? C71 C70 C73 C74 -0.7(5) . . . . ? O11 C70 C73 C74 176.3(3) . . . . ? C70 C73 C74 C75 -0.4(5) . . . . ? C73 C74 C75 C72 0.9(5) . . . . ? C73 C74 C75 C76 -176.5(3) . . . . ? C71 C72 C75 C74 -0.5(5) . . . . ? C71 C72 C75 C76 176.9(3) . . . . ? C74 C75 C76 O14 -1.0(5) . . . . ? C72 C75 C76 O14 -178.4(3) . . . . ? C74 C75 C76 O15 175.5(3) . . . . ? C72 C75 C76 O15 -1.9(5) . . . . ? O2 C44 Co2 O13 171.40(17) . . . 1_666 ? O1 C44 Co2 O13 -10.5(3) . . . 1_666 ? C45 C44 Co2 O13 74(3) . . . 1_666 ? O2 C44 Co2 O15 -82.43(19) . . . 1_556 ? O1 C44 Co2 O15 95.64(18) . . . 1_556 ? C45 C44 Co2 O15 -180(100) . . . 1_556 ? O2 C44 Co2 O1 -178.1(3) . . . . ? C45 C44 Co2 O1 84(3) . . . . ? O1 C44 Co2 O2 178.1(3) . . . . ? C45 C44 Co2 O2 -98(3) . . . . ? O2 C44 Co2 O4 21.6(2) . . . . ? O1 C44 Co2 O4 -160.34(16) . . . . ? C45 C44 Co2 O4 -76(3) . . . . ? O2 C44 Co2 O3 78.43(19) . . . . ? O1 C44 Co2 O3 -103.49(18) . . . . ? C45 C44 Co2 O3 -19(3) . . . . ? O2 C44 Co2 C43 53.8(2) . . . . ? O1 C44 Co2 C43 -128.15(18) . . . . ? C45 C44 Co2 C43 -44(3) . . . . ? O3 C43 Co2 O13 -84.69(19) . . . 1_666 ? O4 C43 Co2 O13 96.37(19) . . . 1_666 ? O3 C43 Co2 O15 178.16(17) . . . 1_556 ? O4 C43 Co2 O15 -0.8(2) . . . 1_556 ? O3 C43 Co2 O1 24.3(2) . . . . ? O4 C43 Co2 O1 -154.64(16) . . . . ? O3 C43 Co2 O2 80.52(19) . . . . ? O4 C43 Co2 O2 -98.42(18) . . . . ? O3 C43 Co2 O4 178.9(3) . . . . ? O4 C43 Co2 O3 -178.9(3) . . . . ? O3 C43 Co2 C44 56.5(2) . . . . ? O4 C43 Co2 C44 -122.40(18) . . . . ? O6 C40 N1 C41 178.8(3) . . . . ? O6 C40 N1 C42 -0.7(5) . . . . ? O5 C37 N2 C38 -178.3(3) . . . . ? O5 C37 N2 C39 -3.1(5) . . . . ? O8 C1 N3 C3 -6.7(5) . . . . ? O8 C1 N3 C2 -178.3(3) . . . . ? O2 C44 O1 Co2 1.9(3) . . . . ? C45 C44 O1 Co2 -174.1(3) . . . . ? O2 C44 O1 Co1 -112.5(4) . . . . ? C45 C44 O1 Co1 71.4(4) . . . . ? Co2 C44 O1 Co1 -114.4(3) . . . . ? O13 Co2 O1 C44 172.35(18) 1_666 . . . ? O15 Co2 O1 C44 -89.41(19) 1_556 . . . ? O2 Co2 O1 C44 -1.10(17) . . . . ? O4 Co2 O1 C44 39.1(3) . . . . ? O3 Co2 O1 C44 81.59(19) . . . . ? C43 Co2 O1 C44 69.5(2) . . . . ? O13 Co2 O1 Co1 -43.98(11) 1_666 . . . ? O15 Co2 O1 Co1 54.26(10) 1_556 . . . ? O2 Co2 O1 Co1 142.57(12) . . . . ? O4 Co2 O1 Co1 -177.26(15) . . . . ? O3 Co2 O1 Co1 -134.74(9) . . . . ? C44 Co2 O1 Co1 143.7(2) . . . . ? C43 Co2 O1 Co1 -146.83(11) . . . . ? O14 Co1 O1 C44 -111.4(3) 2_776 . . . ? O14 Co1 O1 C44 68.6(3) 1_556 . . . ? O12 Co1 O1 C44 -19.3(3) 2_666 . . . ? O12 Co1 O1 C44 160.7(3) 1_666 . . . ? O1 Co1 O1 C44 76(29) 2_777 . . . ? O14 Co1 O1 Co2 139.68(10) 2_776 . . . ? O14 Co1 O1 Co2 -40.32(10) 1_556 . . . ? O12 Co1 O1 Co2 -128.27(10) 2_666 . . . ? O12 Co1 O1 Co2 51.73(10) 1_666 . . . ? O1 Co1 O1 Co2 -33(29) 2_777 . . . ? O1 C44 O2 Co2 -1.9(3) . . . . ? C45 C44 O2 Co2 174.1(3) . . . . ? O13 Co2 O2 C44 -23.0(4) 1_666 . . . ? O15 Co2 O2 C44 100.58(19) 1_556 . . . ? O1 Co2 O2 C44 1.14(18) . . . . ? O4 Co2 O2 C44 -162.71(19) . . . . ? O3 Co2 O2 C44 -103.05(19) . . . . ? C43 Co2 O2 C44 -132.4(2) . . . . ? O4 C43 O3 Co2 1.1(3) . . . . ? O13 Co2 O3 C43 94.8(2) 1_666 . . . ? O15 Co2 O3 C43 -3.7(3) 1_556 . . . ? O1 Co2 O3 C43 -161.20(19) . . . . ? O2 Co2 O3 C43 -100.6(2) . . . . ? O4 Co2 O3 C43 -0.62(18) . . . . ? C44 Co2 O3 C43 -130.1(2) . . . . ? O3 C43 O4 Co4 168.1(2) . . . . ? Co2 C43 O4 Co4 169.1(2) . . . . ? O3 C43 O4 Co2 -1.1(3) . . . . ? O23 Co4 O4 C43 -63.8(2) . . . . ? O19 Co4 O4 C43 -1.2(9) 1_556 . . . ? O22 Co4 O4 C43 35.2(2) 1_666 . . . ? O6 Co4 O4 C43 -148.9(2) . . . . ? O5 Co4 O4 C43 125.7(2) . . . . ? O23 Co4 O4 Co2 95.8(2) . . . . ? O19 Co4 O4 Co2 158.3(7) 1_556 . . . ? O22 Co4 O4 Co2 -165.3(2) 1_666 . . . ? O6 Co4 O4 Co2 10.7(2) . . . . ? O5 Co4 O4 Co2 -74.8(2) . . . . ? O13 Co2 O4 C43 -84.73(19) 1_666 . . . ? O15 Co2 O4 C43 179.37(19) 1_556 . . . ? O1 Co2 O4 C43 50.2(3) . . . . ? O2 Co2 O4 C43 85.18(19) . . . . ? O3 Co2 O4 C43 0.61(18) . . . . ? C44 Co2 O4 C43 74.4(2) . . . . ? O13 Co2 O4 Co4 112.6(2) 1_666 . . . ? O15 Co2 O4 Co4 16.7(2) 1_556 . . . ? O1 Co2 O4 Co4 -112.4(2) . . . . ? O2 Co2 O4 Co4 -77.5(2) . . . . ? O3 Co2 O4 Co4 -162.0(2) . . . . ? C44 Co2 O4 Co4 -88.2(2) . . . . ? C43 Co2 O4 Co4 -162.6(3) . . . . ? N2 C37 O5 Co4 165.6(3) . . . . ? O23 Co4 O5 C37 -62.6(6) . . . . ? O19 Co4 O5 C37 -173.6(3) 1_556 . . . ? O22 Co4 O5 C37 99.8(3) 1_666 . . . ? O6 Co4 O5 C37 -80.9(3) . . . . ? O4 Co4 O5 C37 11.5(3) . . . . ? N1 C40 O6 Co4 168.3(3) . . . . ? O23 Co4 O6 C40 -45.8(2) . . . . ? O19 Co4 O6 C40 -137.5(2) 1_556 . . . ? O22 Co4 O6 C40 141.6(12) 1_666 . . . ? O5 Co4 O6 C40 131.2(2) . . . . ? O4 Co4 O6 C40 39.0(2) . . . . ? O23 C4 O7 Co3 16.8(5) . . . . ? C5 C4 O7 Co3 -163.7(2) . . . . ? O21 Co3 O7 C4 -73.5(3) 1_666 . . . ? O20 Co3 O7 C4 73.8(3) 1_556 . . . ? O8 Co3 O7 C4 -175.8(3) . . . . ? N3 C1 O8 Co3 -164.5(3) . . . . ? O7 Co3 O8 C1 41.0(2) . . . . ? O21 Co3 O8 C1 -80.8(2) 1_666 . . . ? O20 Co3 O8 C1 158.7(2) 1_556 . . . ? C47 C48 O9 C51 -14.1(5) . . . . ? C49 C48 O9 C51 165.7(3) . . . . ? C52 C51 O9 C48 172.2(3) . . . . ? C62 C61 O10 C60 -4.6(5) . . . . ? C66 C61 O10 C60 177.5(3) . . . . ? C54 C60 O10 C61 -157.7(3) . . . . ? C71 C70 O11 C69 173.0(3) . . . . ? C73 C70 O11 C69 -4.0(5) . . . . ? C56 C69 O11 C70 174.2(3) . . . . ? O13 C67 O12 Co1 7.4(5) . . . 1_444 ? C64 C67 O12 Co1 -171.4(2) . . . 1_444 ? O12 C67 O13 Co2 19.2(5) . . . 1_444 ? C64 C67 O13 Co2 -161.9(2) . . . 1_444 ? O15 C76 O14 Co1 -3.9(6) . . . 1_554 ? C75 C76 O14 Co1 172.2(2) . . . 1_554 ? O14 C76 O15 Co2 22.8(5) . . . 1_554 ? C75 C76 O15 Co2 -153.5(2) . . . 1_554 ? C9 C8 O16 C11 -9.5(4) . . . . ? C7 C8 O16 C11 170.9(3) . . . . ? C12 C11 O16 C8 -165.5(2) . . . . ? C23 C22 O17 C21 170.1(3) . . . . ? C27 C22 O17 C21 -8.7(5) . . . . ? C16 C21 O17 C22 -163.9(3) . . . . ? C35 C30 O18 C29 -178.2(3) . . . . ? C31 C30 O18 C29 2.7(5) . . . . ? C14 C29 O18 C30 171.6(3) . . . . ? O20 C36 O19 Co4 127.1(13) . . . 1_554 ? C33 C36 O19 Co4 -57.2(15) . . . 1_554 ? O19 C36 O20 Co3 8.8(4) . . . 1_554 ? C33 C36 O20 Co3 -167.0(3) . . . 1_554 ? O22 C28 O21 Co3 -3.5(6) . . . 1_444 ? C25 C28 O21 Co3 174.9(2) . . . 1_444 ? O21 C28 O22 Co4 35.7(7) . . . 1_444 ? C25 C28 O22 Co4 -142.7(3) . . . 1_444 ? O7 C4 O23 Co4 -14.7(6) . . . . ? C5 C4 O23 Co4 165.8(2) . . . . ? O19 Co4 O23 C4 -26.5(3) 1_556 . . . ? O22 Co4 O23 C4 60.3(3) 1_666 . . . ? O6 Co4 O23 C4 -119.2(3) . . . . ? O5 Co4 O23 C4 -137.5(5) . . . . ? O4 Co4 O23 C4 147.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.932 _refine_diff_density_min -0.994 _refine_diff_density_rms 0.095 _database_code_depnum_ccdc_archive 'CCDC 939261' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4 # start Validation Reply Form _vrf_CHEMW03_4 ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE:The formula weight differs from that calculated due to unlocated solvent moieties - SQUEEZE used - see _platon_squeeze_details. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H94 N4 O28 Zn3' _chemical_formula_weight 1726.39 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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' _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 14.692(2) _cell_length_b 18.436(3) _cell_length_c 19.8419(16) _cell_angle_alpha 115.514(2) _cell_angle_beta 96.834(3) _cell_angle_gamma 108.036(2) _cell_volume 4407.8(9) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 9910 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 27.51 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 0.886 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8113 _exptl_absorpt_correction_T_max 0.8379 _exptl_absorpt_process_details SADABS;Bruker,2000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35408 _diffrn_reflns_av_R_equivalents 0.0171 _diffrn_reflns_av_sigmaI/netI 0.0620 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 26.00 _reflns_number_total 17137 _reflns_number_gt 12773 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. The hydrogen atoms on coordinated water cannot be located in the Fourier difference map and thus were not added in the final cycles of refinement. Those hydrogens are, however, included in the reported chemical formula and derived values (reported crystal-data formula, formula weight,Dx, Mu and F(000)). ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.160 0.362 0.000 1212 59 ' ' 2 0.042 0.990 0.521 7 0 ' ' 3 0.952 0.012 0.476 6 0 ' ' _platon_squeeze_details ; Because of the highly disordered solvent molecules, the PLATON/SQUEEZE route was employed to calculate the diffraction contribution from the solvent molecules, and thereby to produce a set of solvent-free diffraction intensities used for refinement. The unit cell was found to contain a void of 1225 A^3 (28.8% of the unit cell volume), holding 59 electrons. These might correspond with the removal of ~6 H2O molecules from the unit cell, i.e. 3 H2O per asymmetric unit. Based on the elemental analysis and TG analysis, additional 2 DMF might be adsorbed in the sample and were thus included in the final molecular formula. Those solvents are included in the reported chemical formula and derived values (reported crystal-data formula, formula weight, Dx, Mu and F(000)). ; _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^)+(0.0600P)^2^+1.9900P] 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 17137 _refine_ls_number_parameters 911 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0584 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1383 _refine_ls_wR_factor_gt 0.1376 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 C1 C 0.3604(2) 0.10805(19) 0.21751(18) 0.0442(7) Uani 1 1 d . . . C2 C 0.4112(2) 0.20607(19) 0.25449(17) 0.0436(7) Uani 1 1 d . . . C3 C 0.4975(2) 0.25102(19) 0.31800(17) 0.0445(7) Uani 1 1 d . . . H3 H 0.5219 0.2197 0.3361 0.053 Uiso 1 1 calc R . . C4 C 0.5468(2) 0.34066(19) 0.35413(18) 0.0462(8) Uani 1 1 d . . . H4 H 0.6044 0.3692 0.3961 0.055 Uiso 1 1 calc R . . C5 C 0.5121(2) 0.38916(19) 0.32894(17) 0.0425(7) Uani 1 1 d . . . C6 C 0.4265(2) 0.34426(19) 0.26381(17) 0.0423(7) Uani 1 1 d . . . H6 H 0.4031 0.3753 0.2448 0.051 Uiso 1 1 calc R . . C7 C 0.3772(2) 0.25391(18) 0.22808(17) 0.0431(7) Uani 1 1 d . . . H7 H 0.3202 0.2249 0.1855 0.052 Uiso 1 1 calc R . . C8 C 0.6514(2) 0.52116(18) 0.41610(17) 0.0412(7) Uani 1 1 d . . . H8A H 0.6956 0.4999 0.3881 0.049 Uiso 1 1 calc R . . H8B H 0.6509 0.5063 0.4574 0.049 Uiso 1 1 calc R . . C9 C 0.6904(2) 0.61917(19) 0.45134(17) 0.0431(7) Uani 1 1 d . . . C10 C 0.7170(2) 0.65761(19) 0.40576(17) 0.0420(7) Uani 1 1 d . . . C11 C 0.6954(2) 0.59971(19) 0.31927(16) 0.0451(7) Uani 1 1 d . . . H11A H 0.6821 0.5406 0.3079 0.068 Uiso 1 1 calc R . . H11B H 0.7523 0.6208 0.3031 0.068 Uiso 1 1 calc R . . H11C H 0.6380 0.6008 0.2916 0.068 Uiso 1 1 calc R . . C12 C 0.7652(2) 0.74908(18) 0.44068(17) 0.0413(7) Uani 1 1 d . . . C13 C 0.7988(2) 0.78921(19) 0.39242(18) 0.0441(7) Uani 1 1 d . . . H13A H 0.7600 0.7501 0.3379 0.053 Uiso 1 1 calc R . . H13B H 0.7913 0.8444 0.4101 0.053 Uiso 1 1 calc R . . C14 C 0.7911(2) 0.80140(19) 0.52243(17) 0.0417(7) Uani 1 1 d . . . C15 C 0.8505(2) 0.89959(18) 0.56211(18) 0.0450(7) Uani 1 1 d . . . H15A H 0.8795 0.9142 0.5264 0.068 Uiso 1 1 calc R . . H15B H 0.9028 0.9178 0.6072 0.068 Uiso 1 1 calc R . . H15C H 0.8069 0.9291 0.5779 0.068 Uiso 1 1 calc R . . C16 C 0.7640(2) 0.76234(19) 0.56800(17) 0.0425(7) Uani 1 1 d . . . C17 C 0.8070(2) 0.81748(19) 0.65682(17) 0.0439(7) Uani 1 1 d . . . H17A H 0.8048 0.8748 0.6757 0.053 Uiso 1 1 calc R . . H17B H 0.7703 0.7883 0.6819 0.053 Uiso 1 1 calc R . . C18 C 0.7100(2) 0.67067(19) 0.53236(17) 0.0431(7) Uani 1 1 d . . . C19 C 0.6731(2) 0.62859(19) 0.57997(17) 0.0456(7) Uani 1 1 d . . . H19A H 0.7220 0.6105 0.5965 0.068 Uiso 1 1 calc R . . H19B H 0.6111 0.5783 0.5487 0.068 Uiso 1 1 calc R . . H19C H 0.6629 0.6702 0.6250 0.068 Uiso 1 1 calc R . . C20 C 0.9593(2) 0.84508(19) 0.74348(17) 0.0440(7) Uani 1 1 d . . . C21 C 0.9260(2) 0.87313(19) 0.80961(17) 0.0451(7) Uani 1 1 d . . . H21 H 0.8663 0.8809 0.8069 0.054 Uiso 1 1 calc R . . C22 C 0.9835(2) 0.88931(19) 0.87953(17) 0.0433(7) Uani 1 1 d . . . H22 H 0.9620 0.9086 0.9239 0.052 Uiso 1 1 calc R . . C23 C 1.0718(2) 0.87728(19) 0.88432(17) 0.0444(7) Uani 1 1 d . . . C24 C 1.1039(2) 0.84921(19) 0.81769(17) 0.0446(7) Uani 1 1 d . . . H24 H 1.1630 0.8404 0.8202 0.054 Uiso 1 1 calc R . . C25 C 1.0492(2) 0.83445(19) 0.74828(17) 0.0441(7) Uani 1 1 d . . . H25 H 1.0722 0.8174 0.7046 0.053 Uiso 1 1 calc R . . C26 C 1.1315(2) 0.89088(19) 0.95819(17) 0.0436(7) Uani 1 1 d . . . C27 C 0.9517(2) 0.83270(19) 0.35877(17) 0.0431(7) Uani 1 1 d . . . C28 C 1.0518(2) 0.84780(19) 0.37321(18) 0.0446(7) Uani 1 1 d . . . H28 H 1.0821 0.8391 0.4113 0.054 Uiso 1 1 calc R . . C29 C 1.1068(2) 0.87582(19) 0.33111(17) 0.0450(7) Uani 1 1 d . . . H29 H 1.1744 0.8862 0.3408 0.054 Uiso 1 1 calc R . . C30 C 1.0609(2) 0.88867(19) 0.27360(17) 0.0441(7) Uani 1 1 d . . . C31 C 0.9615(2) 0.87475(19) 0.26066(17) 0.0447(7) Uani 1 1 d . . . H31 H 0.9314 0.8842 0.2231 0.054 Uiso 1 1 calc R . . C32 C 0.9054(2) 0.84670(19) 0.30306(17) 0.0446(7) Uani 1 1 d . . . H32 H 0.8382 0.8375 0.2943 0.054 Uiso 1 1 calc R . . C33 C 1.1212(2) 0.91847(19) 0.22806(18) 0.0437(7) Uani 1 1 d . . . C34 C 0.4510(2) 0.7249(2) 0.31002(17) 0.0447(7) Uani 1 1 d . . . C35 C 0.4003(2) 0.68340(19) 0.35313(17) 0.0439(7) Uani 1 1 d . . . C36 C 0.3160(2) 0.69645(19) 0.37234(17) 0.0435(7) Uani 1 1 d . . . H36 H 0.2926 0.7310 0.3584 0.052 Uiso 1 1 calc R . . C37 C 0.2664(2) 0.65812(18) 0.41221(17) 0.0435(7) Uani 1 1 d . . . H37 H 0.2095 0.6662 0.4235 0.052 Uiso 1 1 calc R . . C38 C 0.3017(2) 0.60836(18) 0.43483(17) 0.0424(7) Uani 1 1 d . . . C39 C 0.3870(2) 0.59545(19) 0.41568(18) 0.0444(7) Uani 1 1 d . . . H39 H 0.4109 0.5614 0.4300 0.053 Uiso 1 1 calc R . . C40 C 0.4352(2) 0.63299(19) 0.37590(17) 0.0437(7) Uani 1 1 d . . . H40 H 0.4918 0.6245 0.3642 0.052 Uiso 1 1 calc R . . C41 C 0.1688(2) 0.57532(19) 0.49076(18) 0.0438(7) Uani 1 1 d . . . H41A H 0.1163 0.5481 0.4423 0.053 Uiso 1 1 calc R . . H41B H 0.1793 0.6365 0.5208 0.053 Uiso 1 1 calc R . . C42 C 0.1392(2) 0.52948(19) 0.53599(17) 0.0429(7) Uani 1 1 d . . . C43 C 0.0921(2) 0.43818(19) 0.49719(17) 0.0425(7) Uani 1 1 d . . . C44 C 0.0722(2) 0.38559(19) 0.41054(17) 0.0440(7) Uani 1 1 d . . . H44A H 0.0014 0.3587 0.3854 0.066 Uiso 1 1 calc R . . H44B H 0.0977 0.3409 0.3991 0.066 Uiso 1 1 calc R . . H44C H 0.1048 0.4236 0.3916 0.066 Uiso 1 1 calc R . . C45 C 0.0628(2) 0.39437(19) 0.53946(17) 0.0435(7) Uani 1 1 d . . . C46 C 0.0171(2) 0.29552(18) 0.49850(18) 0.0430(7) Uani 1 1 d . . . H46A H 0.0399 0.2717 0.4530 0.052 Uiso 1 1 calc R . . H46B H 0.0365 0.2753 0.5334 0.052 Uiso 1 1 calc R . . C47 C 0.0776(2) 0.44274(19) 0.62004(17) 0.0424(7) Uani 1 1 d . . . C48 C 0.0392(2) 0.39519(19) 0.66378(17) 0.0447(7) Uani 1 1 d . . . H48A H 0.0949 0.3994 0.6981 0.067 Uiso 1 1 calc R . . H48B H -0.0019 0.3345 0.6271 0.067 Uiso 1 1 calc R . . H48C H 0.0003 0.4216 0.6938 0.067 Uiso 1 1 calc R . . C49 C 0.1272(2) 0.53436(19) 0.65911(17) 0.0428(7) Uani 1 1 d . . . C50 C 0.1524(2) 0.5857(2) 0.74619(17) 0.0442(7) Uani 1 1 d . . . H50A H 0.1479 0.6419 0.7624 0.053 Uiso 1 1 calc R . . H50B H 0.1069 0.5537 0.7650 0.053 Uiso 1 1 calc R . . C51 C 0.1601(2) 0.57832(19) 0.61844(17) 0.0425(7) Uani 1 1 d . . . C52 C 0.2168(2) 0.67655(19) 0.66063(17) 0.0443(7) Uani 1 1 d . . . H52A H 0.1704 0.7042 0.6695 0.066 Uiso 1 1 calc R . . H52B H 0.2546 0.6929 0.6294 0.066 Uiso 1 1 calc R . . H52C H 0.2615 0.6952 0.7098 0.066 Uiso 1 1 calc R . . C53 C 0.2909(2) 0.62543(19) 0.85315(17) 0.0450(7) Uani 1 1 d . . . C54 C 0.3855(2) 0.62765(19) 0.87476(18) 0.0447(7) Uani 1 1 d . . . H54 H 0.4192 0.6116 0.8377 0.054 Uiso 1 1 calc R . . C55 C 0.4295(2) 0.65373(19) 0.95148(17) 0.0445(7) Uani 1 1 d . . . H55 H 0.4929 0.6550 0.9656 0.053 Uiso 1 1 calc R . . C56 C 0.3804(2) 0.67806(19) 1.00795(17) 0.0432(7) Uani 1 1 d . . . C57 C 0.2860(2) 0.67602(19) 0.98500(17) 0.0445(7) Uani 1 1 d . . . H57 H 0.2519 0.6916 1.0219 0.053 Uiso 1 1 calc R . . C58 C 0.2415(2) 0.65153(19) 0.90887(17) 0.0442(7) Uani 1 1 d . . . H58 H 0.1793 0.6525 0.8951 0.053 Uiso 1 1 calc R . . C59 C 0.4274(2) 0.70651(19) 1.09088(17) 0.0440(7) Uani 1 1 d . . . C60 C -0.1480(2) 0.17928(19) 0.43251(17) 0.0444(7) Uani 1 1 d . . . C61 C -0.2500(2) 0.15571(19) 0.40317(17) 0.0443(7) Uani 1 1 d . . . H61 H -0.2754 0.1987 0.4156 0.053 Uiso 1 1 calc R . . C62 C -0.3130(2) 0.06814(18) 0.35555(17) 0.0440(7) Uani 1 1 d . . . H62 H -0.3806 0.0525 0.3343 0.053 Uiso 1 1 calc R . . C63 C -0.2763(2) 0.00323(19) 0.33910(17) 0.0423(7) Uani 1 1 d . . . C64 C -0.1764(2) 0.02740(19) 0.37051(17) 0.0431(7) Uani 1 1 d . . . H64 H -0.1519 -0.0159 0.3604 0.052 Uiso 1 1 calc R . . C65 C -0.1112(2) 0.11462(18) 0.41682(17) 0.0425(7) Uani 1 1 d . . . H65 H -0.0435 0.1298 0.4372 0.051 Uiso 1 1 calc R . . C66 C -0.3470(2) -0.09016(19) 0.28794(17) 0.0423(7) Uani 1 1 d . . . C67 C 0.4082(2) 0.9663(2) 0.39815(17) 0.0454(7) Uani 1 1 d . . . H67 H 0.3837 0.9156 0.4018 0.054 Uiso 1 1 calc R . . C68 C 0.4354(2) 1.11751(19) 0.44600(18) 0.0480(8) Uani 1 1 d . . . H68A H 0.4964 1.1598 0.4870 0.072 Uiso 1 1 calc R . . H68B H 0.3849 1.1408 0.4518 0.072 Uiso 1 1 calc R . . H68C H 0.4468 1.1050 0.3963 0.072 Uiso 1 1 calc R . . C69 C 0.3646(2) 1.0398(2) 0.51547(18) 0.0480(8) Uani 1 1 d . . . H69A H 0.3361 0.9814 0.5078 0.072 Uiso 1 1 calc R . . H69B H 0.3142 1.0631 0.5185 0.072 Uiso 1 1 calc R . . H69C H 0.4187 1.0765 0.5632 0.072 Uiso 1 1 calc R . . C70 C 0.7151(2) 0.6803(2) 0.14119(19) 0.0504(8) Uani 1 1 d . . . H70 H 0.7091 0.7177 0.1228 0.061 Uiso 1 1 calc R . . C71 C 0.8628(2) 0.6735(2) 0.08939(19) 0.0521(8) Uani 1 1 d . . . H71A H 0.9277 0.6898 0.1218 0.078 Uiso 1 1 calc R . . H71B H 0.8595 0.7235 0.0869 0.078 Uiso 1 1 calc R . . H71C H 0.8517 0.6275 0.0377 0.078 Uiso 1 1 calc R . . C72 C 0.7885(2) 0.5793(2) 0.14072(18) 0.0482(8) Uani 1 1 d . . . H72A H 0.7863 0.5972 0.1934 0.072 Uiso 1 1 calc R . . H72B H 0.8494 0.5715 0.1357 0.072 Uiso 1 1 calc R . . H72C H 0.7322 0.5249 0.1056 0.072 Uiso 1 1 calc R . . N1 N 0.40212(19) 1.03743(16) 0.45038(14) 0.0464(6) Uani 1 1 d . . . N2 N 0.7850(2) 0.64209(17) 0.12294(15) 0.0506(7) Uani 1 1 d . . . O1 O 0.44514(15) 0.96303(13) 0.34376(12) 0.0453(5) Uani 1 1 d . . . O2 O 0.40423(15) 0.06892(13) 0.23404(12) 0.0451(5) Uani 1 1 d . . . O3 O 0.27259(15) 0.07344(13) 0.16993(11) 0.0443(5) Uani 1 1 d . . . O4 O 0.55227(15) 0.47902(13) 0.36367(12) 0.0454(5) Uani 1 1 d . . . O5 O 1.20184(15) 0.86491(13) 0.95515(12) 0.0467(5) Uani 1 1 d . . . O6 O 1.10586(15) 0.92634(13) 1.01938(12) 0.0451(5) Uani 1 1 d . . . O7 O 0.90906(15) 0.82522(13) 0.67147(12) 0.0454(5) Uani 1 1 d . . . O8 O 1.21147(15) 0.93146(13) 0.24051(12) 0.0444(5) Uani 1 1 d . . . O9 O 1.07816(15) 0.93045(13) 0.17614(12) 0.0449(5) Uani 1 1 d . . . O10 O 0.90259(14) 0.80337(13) 0.40231(11) 0.0428(5) Uani 1 1 d . . . O11 O 0.50643(15) 0.69118(13) 0.27400(12) 0.0450(5) Uani 1 1 d . . . O12 O 0.43899(15) 0.78973(13) 0.31285(12) 0.0457(5) Uani 1 1 d . . . O13 O 0.26042(14) 0.56911(12) 0.47448(11) 0.0430(5) Uani 1 1 d . . . O14 O 0.51030(15) 0.70249(13) 1.10690(12) 0.0450(5) Uani 1 1 d . . . O15 O 0.38177(15) 0.73226(13) 1.13988(11) 0.0444(5) Uani 1 1 d . . . O16 O 0.25413(15) 0.59811(13) 0.77610(11) 0.0448(5) Uani 1 1 d . . . O17 O -0.31596(15) -0.14951(13) 0.28132(11) 0.0446(5) Uani 1 1 d . . . O18 O -0.43160(15) -0.10831(13) 0.25065(11) 0.0442(5) Uani 1 1 d . . . O19 O -0.09100(14) 0.26704(12) 0.47504(11) 0.0434(5) Uani 1 1 d . . . O20 O 0.66221(15) 0.66497(13) 0.18073(12) 0.0461(5) Uani 1 1 d . . . O1W O 0.40238(15) 0.90846(13) 0.17870(12) 0.0451(5) Uani 1 1 d . . . O2W O 0.27051(15) 0.80747(13) 0.24105(12) 0.0460(5) Uani 1 1 d . . . O3W O 0.22063(15) -0.14898(12) 0.07978(12) 0.0423(5) Uani 1 1 d . . . Zn1 Zn 0.41790(3) 0.84537(2) 0.24384(2) 0.04288(11) Uani 1 1 d . . . Zn2 Zn 0.17969(3) -0.04744(2) 0.12279(2) 0.04306(11) Uani 1 1 d . . . Zn3 Zn 0.57526(3) 0.73383(2) 0.21218(2) 0.04290(11) 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 C1 0.0398(16) 0.0371(15) 0.0401(16) 0.0106(13) 0.0103(13) 0.0098(13) C2 0.0369(15) 0.0395(15) 0.0395(16) 0.0108(13) 0.0086(12) 0.0113(13) C3 0.0390(16) 0.0388(15) 0.0407(16) 0.0111(13) 0.0086(13) 0.0109(13) C4 0.0382(16) 0.0373(15) 0.0402(16) 0.0095(13) -0.0080(13) 0.0087(13) C5 0.0368(15) 0.0380(15) 0.0404(16) 0.0119(13) 0.0085(12) 0.0122(13) C6 0.0378(15) 0.0389(15) 0.0362(15) 0.0113(13) 0.0076(12) 0.0104(13) C7 0.0365(15) 0.0371(14) 0.0387(16) 0.0090(13) 0.0085(12) 0.0094(12) C8 0.0364(15) 0.0384(15) 0.0353(15) 0.0108(12) 0.0074(12) 0.0109(12) C9 0.0388(16) 0.0382(15) 0.0374(16) 0.0104(13) 0.0091(12) 0.0104(13) C10 0.0382(15) 0.0379(14) 0.0393(16) 0.0128(13) 0.0104(12) 0.0123(13) C11 0.0419(17) 0.0384(15) 0.0373(16) 0.0097(13) 0.0103(13) 0.0083(13) C12 0.0375(15) 0.0374(14) 0.0382(16) 0.0125(13) 0.0115(12) 0.0108(12) C13 0.0380(16) 0.0399(15) 0.0407(16) 0.0125(13) 0.0103(13) 0.0105(13) C14 0.0350(15) 0.0393(15) 0.0350(15) 0.0090(13) 0.0058(12) 0.0112(12) C15 0.0420(16) 0.0372(15) 0.0389(16) 0.0095(13) 0.0092(13) 0.0101(13) C16 0.0358(15) 0.0386(15) 0.0383(16) 0.0108(13) 0.0079(12) 0.0102(12) C17 0.0376(16) 0.0387(15) 0.0392(16) 0.0103(13) 0.0083(12) 0.0101(13) C18 0.0385(15) 0.0371(14) 0.0378(16) 0.0102(13) 0.0104(12) 0.0085(12) C19 0.0391(16) 0.0408(15) 0.0405(16) 0.0108(13) 0.0119(13) 0.0096(13) C20 0.0397(16) 0.0405(15) 0.0354(16) 0.0088(13) 0.0088(13) 0.0118(13) C21 0.0402(16) 0.0424(15) 0.0381(16) 0.0114(13) 0.0114(13) 0.0116(13) C22 0.0406(16) 0.0386(15) 0.0373(16) 0.0112(13) 0.0107(13) 0.0111(13) C23 0.0405(16) 0.0421(15) 0.0372(16) 0.0126(13) 0.0099(13) 0.0115(13) C24 0.0378(16) 0.0433(15) 0.0381(16) 0.0110(13) 0.0093(13) 0.0127(13) C25 0.0394(16) 0.0393(15) 0.0376(16) 0.0103(13) 0.0111(13) 0.0094(13) C26 0.0390(16) 0.0421(15) 0.0366(16) 0.0117(13) 0.0099(13) 0.0121(13) C27 0.0411(16) 0.0383(15) 0.0397(16) 0.0137(13) 0.0113(13) 0.0120(13) C28 0.0377(16) 0.0416(15) 0.0403(16) 0.0126(13) 0.0086(13) 0.0108(13) C29 0.0384(16) 0.0398(15) 0.0394(16) 0.0101(13) 0.0105(13) 0.0091(13) C30 0.0405(16) 0.0377(15) 0.0402(16) 0.0110(13) 0.0103(13) 0.0115(13) C31 0.0368(16) 0.0415(15) 0.0391(16) 0.0112(13) 0.0099(12) 0.0090(13) C32 0.0373(16) 0.0426(15) 0.0414(16) 0.0143(14) 0.0102(13) 0.0109(13) C33 0.0378(17) 0.0389(15) 0.0394(16) 0.0108(13) 0.0095(13) 0.0106(13) C34 0.0406(16) 0.0378(16) 0.0398(16) 0.0105(13) 0.0094(13) 0.0102(13) C35 0.0406(16) 0.0383(15) 0.0397(16) 0.0125(13) 0.0094(13) 0.0110(13) C36 0.0387(16) 0.0376(14) 0.0396(16) 0.0118(13) 0.0083(13) 0.0095(13) C37 0.0415(16) 0.0377(15) 0.0391(16) 0.0130(13) 0.0098(13) 0.0108(13) C38 0.0405(16) 0.0370(14) 0.0379(15) 0.0120(13) 0.0098(13) 0.0114(13) C39 0.0394(16) 0.0387(15) 0.0433(17) 0.0136(13) 0.0114(13) 0.0115(13) C40 0.0386(16) 0.0397(15) 0.0374(16) 0.0114(13) 0.0076(12) 0.0097(13) C41 0.0369(16) 0.0400(15) 0.0409(16) 0.0119(13) 0.0098(13) 0.0112(13) C42 0.0386(16) 0.0374(14) 0.0385(16) 0.0111(13) 0.0101(12) 0.0099(12) C43 0.0373(15) 0.0387(15) 0.0394(16) 0.0113(13) 0.0103(12) 0.0130(13) C44 0.0389(16) 0.0383(15) 0.0372(16) 0.0089(13) 0.0093(12) 0.0093(13) C45 0.0338(15) 0.0401(15) 0.0401(16) 0.0106(13) 0.0079(12) 0.0096(12) C46 0.0390(16) 0.0371(15) 0.0386(16) 0.0108(13) 0.0099(12) 0.0101(13) C47 0.0371(15) 0.0378(14) 0.0390(16) 0.0120(13) 0.0078(12) 0.0104(12) C48 0.0410(16) 0.0410(15) 0.0369(16) 0.0109(13) 0.0096(13) 0.0110(13) C49 0.0387(16) 0.0373(14) 0.0378(16) 0.0100(13) 0.0098(12) 0.0105(13) C50 0.0411(16) 0.0396(15) 0.0377(16) 0.0100(13) 0.0116(13) 0.0127(13) C51 0.0374(15) 0.0399(15) 0.0379(16) 0.0124(13) 0.0080(12) 0.0116(13) C52 0.0417(16) 0.0402(15) 0.0375(16) 0.0120(13) 0.0106(13) 0.0112(13) C53 0.0403(16) 0.0406(15) 0.0386(16) 0.0112(13) 0.0100(13) 0.0104(13) C54 0.0385(16) 0.0399(15) 0.0410(16) 0.0121(13) 0.0100(13) 0.0102(13) C55 0.0401(16) 0.0422(15) 0.0365(16) 0.0099(13) 0.0100(13) 0.0133(13) C56 0.0398(16) 0.0380(15) 0.0403(16) 0.0124(13) 0.0100(13) 0.0126(13) C57 0.0409(16) 0.0422(15) 0.0381(16) 0.0117(13) 0.0123(13) 0.0135(13) C58 0.0397(16) 0.0409(15) 0.0398(16) 0.0126(13) 0.0093(13) 0.0133(13) C59 0.0397(17) 0.0389(15) 0.0378(16) 0.0100(13) 0.0108(13) 0.0104(13) C60 0.0392(16) 0.0390(15) 0.0388(16) 0.0102(13) 0.0085(13) 0.0104(13) C61 0.0369(16) 0.0388(15) 0.0429(17) 0.0122(13) 0.0102(13) 0.0101(13) C62 0.0381(16) 0.0384(15) 0.0401(16) 0.0113(13) 0.0086(13) 0.0097(13) C63 0.0374(16) 0.0374(15) 0.0381(16) 0.0113(13) 0.0074(12) 0.0103(13) C64 0.0377(16) 0.0364(14) 0.0396(16) 0.0101(13) 0.0094(12) 0.0095(12) C65 0.0373(15) 0.0382(15) 0.0366(15) 0.0108(13) 0.0075(12) 0.0092(13) C66 0.0399(17) 0.0377(15) 0.0364(15) 0.0111(13) 0.0092(13) 0.0114(13) C67 0.0408(16) 0.0385(15) 0.0403(16) 0.0097(13) 0.0111(13) 0.0109(13) C68 0.0434(17) 0.0414(16) 0.0429(17) 0.0109(14) 0.0119(13) 0.0123(14) C69 0.0420(17) 0.0461(16) 0.0413(17) 0.0129(14) 0.0106(13) 0.0134(14) C70 0.0433(17) 0.0463(17) 0.0454(18) 0.0146(15) 0.0120(14) 0.0107(14) C71 0.0451(18) 0.0474(17) 0.0450(18) 0.0122(15) 0.0141(14) 0.0111(14) C72 0.0455(17) 0.0422(16) 0.0429(17) 0.0127(14) 0.0101(14) 0.0140(14) N1 0.0400(14) 0.0432(13) 0.0388(14) 0.0103(12) 0.0106(11) 0.0108(11) N2 0.0445(15) 0.0448(14) 0.0454(15) 0.0104(12) 0.0134(12) 0.0145(12) O1 0.0391(11) 0.0414(11) 0.0403(11) 0.0115(9) 0.0111(9) 0.0110(9) O2 0.0402(11) 0.0388(10) 0.0411(11) 0.0113(9) 0.0092(9) 0.0110(9) O3 0.0378(11) 0.0397(10) 0.0382(11) 0.0099(9) 0.0085(9) 0.0097(9) O4 0.0395(11) 0.0380(10) 0.0397(11) 0.0120(9) -0.0069(9) 0.0101(9) O5 0.0393(11) 0.0457(11) 0.0386(11) 0.0114(9) 0.0090(9) 0.0120(10) O6 0.0400(11) 0.0393(10) 0.0396(11) 0.0103(9) 0.0102(9) 0.0102(9) O7 0.0394(11) 0.0435(11) 0.0383(11) 0.0113(9) 0.0093(9) 0.0122(9) O8 0.0407(12) 0.0410(11) 0.0403(11) 0.0134(9) 0.0119(9) 0.0128(9) O9 0.0398(11) 0.0408(11) 0.0404(11) 0.0129(9) 0.0112(9) 0.0104(9) O10 0.0383(11) 0.0394(10) 0.0405(11) 0.0137(9) 0.0114(9) 0.0121(9) O11 0.0431(12) 0.0381(10) 0.0415(11) 0.0130(9) 0.0117(9) 0.0114(9) O12 0.0431(11) 0.0400(11) 0.0382(11) 0.0109(9) 0.0105(9) 0.0107(9) O13 0.0379(11) 0.0385(10) 0.0390(11) 0.0120(9) 0.0102(9) 0.0097(9) O14 0.0380(11) 0.0397(10) 0.0395(11) 0.0093(9) 0.0085(9) 0.0104(9) O15 0.0401(11) 0.0404(10) 0.0353(11) 0.0102(9) 0.0086(9) 0.0086(9) O16 0.0382(11) 0.0426(11) 0.0373(11) 0.0109(9) 0.0077(9) 0.0106(9) O17 0.0387(11) 0.0385(10) 0.0397(11) 0.0100(9) 0.0081(9) 0.0101(9) O18 0.0367(11) 0.0389(10) 0.0392(11) 0.0102(9) 0.0069(9) 0.0086(9) O19 0.0365(11) 0.0377(10) 0.0400(11) 0.0095(9) 0.0080(9) 0.0108(9) O20 0.0448(12) 0.0411(11) 0.0397(11) 0.0128(9) 0.0116(9) 0.0126(9) O1W 0.0421(11) 0.0385(10) 0.0413(11) 0.0117(9) 0.0125(9) 0.0117(9) O2W 0.0393(11) 0.0408(11) 0.0427(11) 0.0123(9) 0.0108(9) 0.0105(9) O3W 0.0388(11) 0.0317(9) 0.0426(11) 0.0113(9) 0.0103(9) 0.0087(8) Zn1 0.03882(19) 0.03855(18) 0.03762(19) 0.01123(15) 0.00948(14) 0.01088(15) Zn2 0.03791(19) 0.03876(18) 0.03783(19) 0.01097(15) 0.00926(14) 0.01004(15) Zn3 0.03881(19) 0.03825(18) 0.03724(19) 0.01075(15) 0.00916(14) 0.01044(15) _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 C1 O2 1.218(4) . ? C1 O3 1.282(4) . ? C1 C2 1.501(4) . ? C2 C7 1.382(4) . ? C2 C3 1.397(4) . ? C3 C4 1.373(4) . ? C3 H3 0.9300 . ? C4 C5 1.384(4) . ? C4 H4 0.9300 . ? C5 O4 1.372(3) . ? C5 C6 1.409(4) . ? C6 C7 1.384(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 O4 1.432(3) . ? C8 C9 1.502(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.392(4) . ? C9 C18 1.405(4) . ? C10 C12 1.401(4) . ? C10 C11 1.506(4) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C14 1.409(4) . ? C12 C13 1.485(4) . ? C13 O10 1.438(4) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C16 1.401(4) . ? C14 C15 1.513(4) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C18 1.412(4) . ? C16 C17 1.527(4) . ? C17 O7 1.442(4) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.510(4) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 O7 1.360(4) . ? C20 C25 1.392(4) . ? C20 C21 1.397(4) . ? C21 C22 1.391(4) . ? C21 H21 0.9300 . ? C22 C23 1.383(4) . ? C22 H22 0.9300 . ? C23 C24 1.396(4) . ? C23 C26 1.490(4) . ? C24 C25 1.377(4) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 O5 1.264(4) . ? C26 O6 1.273(4) . ? C27 O10 1.367(4) . ? C27 C28 1.378(4) . ? C27 C32 1.388(4) . ? C28 C29 1.375(4) . ? C28 H28 0.9300 . ? C29 C30 1.401(5) . ? C29 H29 0.9300 . ? C30 C31 1.373(4) . ? C30 C33 1.490(4) . ? C31 C32 1.389(4) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 O8 1.245(4) . ? C33 O9 1.280(4) . ? C33 Zn2 2.592(3) 1_665 ? C34 O12 1.240(4) . ? C34 O11 1.276(4) . ? C34 C35 1.496(5) . ? C35 C40 1.390(4) . ? C35 C36 1.398(4) . ? C36 C37 1.398(4) . ? C36 H36 0.9300 . ? C37 C38 1.381(4) . ? C37 H37 0.9300 . ? C38 O13 1.357(4) . ? C38 C39 1.411(4) . ? C39 C40 1.380(4) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 O13 1.447(4) . ? C41 C42 1.493(4) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.393(4) . ? C42 C51 1.422(4) . ? C43 C45 1.413(5) . ? C43 C44 1.500(4) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C47 1.402(4) . ? C45 C46 1.506(4) . ? C46 O19 1.453(3) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C49 1.400(4) . ? C47 C48 1.519(4) . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 C51 1.398(4) . ? C49 C50 1.497(4) . ? C50 O16 1.449(4) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.506(4) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 O16 1.362(4) . ? C53 C54 1.387(4) . ? C53 C58 1.390(4) . ? C54 C55 1.382(4) . ? C54 H54 0.9300 . ? C55 C56 1.392(4) . ? C55 H55 0.9300 . ? C56 C57 1.390(4) . ? C56 C59 1.490(4) . ? C57 C58 1.381(4) . ? C57 H57 0.9300 . ? C58 H58 0.9300 . ? C59 O14 1.255(4) . ? C59 O15 1.255(4) . ? C60 O19 1.359(3) . ? C60 C65 1.389(4) . ? C60 C61 1.394(4) . ? C61 C62 1.382(4) . ? C61 H61 0.9300 . ? C62 C63 1.390(4) . ? C62 H62 0.9300 . ? C63 C64 1.372(4) . ? C63 C66 1.486(4) . ? C64 C65 1.382(4) . ? C64 H64 0.9300 . ? C65 H65 0.9300 . ? C66 O18 1.230(4) . ? C66 O17 1.274(4) . ? C67 O1 1.251(4) . ? C67 N1 1.313(4) . ? C67 H67 0.9300 . ? C68 N1 1.449(4) . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C69 N1 1.452(4) . ? C69 H69A 0.9600 . ? C69 H69B 0.9600 . ? C69 H69C 0.9600 . ? C70 O20 1.224(4) . ? C70 N2 1.413(4) . ? C70 H70 0.9300 . ? C71 N2 1.479(4) . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? C72 N2 1.361(4) . ? C72 H72A 0.9600 . ? C72 H72B 0.9600 . ? C72 H72C 0.9600 . ? O1 Zn1 2.089(2) . ? O3 Zn2 1.9290(19) . ? O6 Zn2 1.978(2) 1_666 ? O9 Zn2 1.971(2) 1_665 ? O11 Zn3 1.944(2) . ? O12 Zn1 2.081(2) . ? O14 Zn3 1.937(2) 1_556 ? O15 Zn1 2.0575(19) 1_556 ? O17 Zn3 1.9672(19) 1_445 ? O18 Zn1 2.073(2) 1_445 ? O20 Zn3 2.036(2) . ? O1W Zn1 2.113(2) . ? O2W Zn1 2.045(2) . ? O3W Zn2 2.009(2) . ? Zn1 O15 2.0576(19) 1_554 ? Zn1 O18 2.073(2) 1_665 ? Zn2 O9 1.970(2) 1_445 ? Zn2 O6 1.978(2) 1_444 ? Zn2 C33 2.592(3) 1_445 ? Zn3 O14 1.937(2) 1_554 ? Zn3 O17 1.9672(19) 1_665 ? 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 O2 C1 O3 126.1(3) . . ? O2 C1 C2 119.1(3) . . ? O3 C1 C2 114.8(3) . . ? C7 C2 C3 118.4(3) . . ? C7 C2 C1 123.1(3) . . ? C3 C2 C1 118.5(3) . . ? C4 C3 C2 121.0(3) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 120.9(3) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? O4 C5 C4 125.5(3) . . ? O4 C5 C6 115.9(3) . . ? C4 C5 C6 118.5(3) . . ? C7 C6 C5 120.0(3) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C2 C7 C6 121.2(3) . . ? C2 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? O4 C8 C9 111.2(3) . . ? O4 C8 H8A 109.4 . . ? C9 C8 H8A 109.4 . . ? O4 C8 H8B 109.4 . . ? C9 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C10 C9 C18 121.1(3) . . ? C10 C9 C8 120.0(3) . . ? C18 C9 C8 118.4(3) . . ? C9 C10 C12 120.0(3) . . ? C9 C10 C11 119.2(3) . . ? C12 C10 C11 120.7(3) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 C14 119.6(3) . . ? C10 C12 C13 119.6(3) . . ? C14 C12 C13 120.4(3) . . ? O10 C13 C12 105.6(3) . . ? O10 C13 H13A 110.6 . . ? C12 C13 H13A 110.6 . . ? O10 C13 H13B 110.6 . . ? C12 C13 H13B 110.6 . . ? H13A C13 H13B 108.7 . . ? C16 C14 C12 120.0(3) . . ? C16 C14 C15 119.3(3) . . ? C12 C14 C15 120.6(3) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 C18 120.3(3) . . ? C14 C16 C17 119.1(3) . . ? C18 C16 C17 119.9(3) . . ? O7 C17 C16 104.0(2) . . ? O7 C17 H17A 111.0 . . ? C16 C17 H17A 111.0 . . ? O7 C17 H17B 111.0 . . ? C16 C17 H17B 111.0 . . ? H17A C17 H17B 109.0 . . ? C9 C18 C16 118.6(3) . . ? C9 C18 C19 120.5(3) . . ? C16 C18 C19 120.9(3) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O7 C20 C25 115.2(3) . . ? O7 C20 C21 124.7(3) . . ? C25 C20 C21 120.0(3) . . ? C22 C21 C20 119.0(3) . . ? C22 C21 H21 120.5 . . ? C20 C21 H21 120.5 . . ? C23 C22 C21 121.2(3) . . ? C23 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? C22 C23 C24 119.0(3) . . ? C22 C23 C26 121.4(3) . . ? C24 C23 C26 119.6(3) . . ? C25 C24 C23 120.7(3) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C20 120.0(3) . . ? C24 C25 H25 120.0 . . ? C20 C25 H25 120.0 . . ? O5 C26 O6 125.1(3) . . ? O5 C26 C23 117.9(3) . . ? O6 C26 C23 117.0(3) . . ? O10 C27 C28 115.8(3) . . ? O10 C27 C32 123.2(3) . . ? C28 C27 C32 121.1(3) . . ? C29 C28 C27 119.8(3) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C28 C29 C30 119.9(3) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C31 C30 C29 119.7(3) . . ? C31 C30 C33 121.0(3) . . ? C29 C30 C33 119.3(3) . . ? C30 C31 C32 120.8(3) . . ? C30 C31 H31 119.6 . . ? C32 C31 H31 119.6 . . ? C27 C32 C31 118.7(3) . . ? C27 C32 H32 120.7 . . ? C31 C32 H32 120.7 . . ? O8 C33 O9 121.0(3) . . ? O8 C33 C30 120.6(3) . . ? O9 C33 C30 118.5(3) . . ? O8 C33 Zn2 73.72(17) . 1_665 ? O9 C33 Zn2 47.60(14) . 1_665 ? C30 C33 Zn2 164.8(2) . 1_665 ? O12 C34 O11 124.7(3) . . ? O12 C34 C35 119.0(3) . . ? O11 C34 C35 116.3(3) . . ? C40 C35 C36 118.7(3) . . ? C40 C35 C34 122.0(3) . . ? C36 C35 C34 119.3(3) . . ? C35 C36 C37 120.8(3) . . ? C35 C36 H36 119.6 . . ? C37 C36 H36 119.6 . . ? C38 C37 C36 120.2(3) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? O13 C38 C37 125.2(3) . . ? O13 C38 C39 115.8(3) . . ? C37 C38 C39 119.0(3) . . ? C40 C39 C38 120.5(3) . . ? C40 C39 H39 119.7 . . ? C38 C39 H39 119.7 . . ? C39 C40 C35 120.8(3) . . ? C39 C40 H40 119.6 . . ? C35 C40 H40 119.6 . . ? O13 C41 C42 108.2(3) . . ? O13 C41 H41A 110.1 . . ? C42 C41 H41A 110.1 . . ? O13 C41 H41B 110.1 . . ? C42 C41 H41B 110.1 . . ? H41A C41 H41B 108.4 . . ? C43 C42 C51 119.9(3) . . ? C43 C42 C41 119.7(3) . . ? C51 C42 C41 120.4(3) . . ? C42 C43 C45 120.0(3) . . ? C42 C43 C44 120.5(3) . . ? C45 C43 C44 119.5(3) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C47 C45 C43 120.1(3) . . ? C47 C45 C46 119.7(3) . . ? C43 C45 C46 120.2(3) . . ? O19 C46 C45 107.5(2) . . ? O19 C46 H46A 110.2 . . ? C45 C46 H46A 110.2 . . ? O19 C46 H46B 110.2 . . ? C45 C46 H46B 110.2 . . ? H46A C46 H46B 108.5 . . ? C49 C47 C45 119.6(3) . . ? C49 C47 C48 120.8(3) . . ? C45 C47 C48 119.6(3) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C51 C49 C47 120.8(3) . . ? C51 C49 C50 119.2(3) . . ? C47 C49 C50 119.9(3) . . ? O16 C50 C49 105.6(2) . . ? O16 C50 H50A 110.6 . . ? C49 C50 H50A 110.6 . . ? O16 C50 H50B 110.6 . . ? C49 C50 H50B 110.6 . . ? H50A C50 H50B 108.7 . . ? C49 C51 C42 119.4(3) . . ? C49 C51 C52 121.0(3) . . ? C42 C51 C52 119.6(3) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O16 C53 C54 115.2(3) . . ? O16 C53 C58 124.7(3) . . ? C54 C53 C58 120.1(3) . . ? C55 C54 C53 119.9(3) . . ? C55 C54 H54 120.1 . . ? C53 C54 H54 120.1 . . ? C54 C55 C56 121.0(3) . . ? C54 C55 H55 119.5 . . ? C56 C55 H55 119.5 . . ? C57 C56 C55 118.0(3) . . ? C57 C56 C59 120.6(3) . . ? C55 C56 C59 121.4(3) . . ? C58 C57 C56 121.8(3) . . ? C58 C57 H57 119.1 . . ? C56 C57 H57 119.1 . . ? C57 C58 C53 119.1(3) . . ? C57 C58 H58 120.5 . . ? C53 C58 H58 120.5 . . ? O14 C59 O15 124.3(3) . . ? O14 C59 C56 117.4(3) . . ? O15 C59 C56 118.4(3) . . ? O19 C60 C65 124.7(3) . . ? O19 C60 C61 115.4(3) . . ? C65 C60 C61 119.9(3) . . ? C62 C61 C60 119.6(3) . . ? C62 C61 H61 120.2 . . ? C60 C61 H61 120.2 . . ? C61 C62 C63 120.6(3) . . ? C61 C62 H62 119.7 . . ? C63 C62 H62 119.7 . . ? C64 C63 C62 119.0(3) . . ? C64 C63 C66 122.2(3) . . ? C62 C63 C66 118.8(3) . . ? C63 C64 C65 121.6(3) . . ? C63 C64 H64 119.2 . . ? C65 C64 H64 119.2 . . ? C64 C65 C60 119.2(3) . . ? C64 C65 H65 120.4 . . ? C60 C65 H65 120.4 . . ? O18 C66 O17 121.7(3) . . ? O18 C66 C63 119.9(3) . . ? O17 C66 C63 118.3(3) . . ? O1 C67 N1 123.7(3) . . ? O1 C67 H67 118.2 . . ? N1 C67 H67 118.2 . . ? N1 C68 H68A 109.5 . . ? N1 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? N1 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? N1 C69 H69A 109.5 . . ? N1 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? N1 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? O20 C70 N2 121.3(3) . . ? O20 C70 H70 119.4 . . ? N2 C70 H70 119.4 . . ? N2 C71 H71A 109.5 . . ? N2 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? N2 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? N2 C72 H72A 109.5 . . ? N2 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? N2 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C67 N1 C68 120.7(3) . . ? C67 N1 C69 121.7(3) . . ? C68 N1 C69 117.5(3) . . ? C72 N2 C70 121.5(3) . . ? C72 N2 C71 116.8(3) . . ? C70 N2 C71 121.5(3) . . ? C67 O1 Zn1 123.12(19) . . ? C1 O3 Zn2 125.8(2) . . ? C5 O4 C8 114.3(2) . . ? C26 O6 Zn2 122.2(2) . 1_666 ? C20 O7 C17 119.2(2) . . ? C33 O9 Zn2 103.75(19) . 1_665 ? C27 O10 C13 118.9(2) . . ? C34 O11 Zn3 122.3(2) . . ? C34 O12 Zn1 141.8(2) . . ? C38 O13 C41 117.9(2) . . ? C59 O14 Zn3 120.58(19) . 1_556 ? C59 O15 Zn1 134.28(19) . 1_556 ? C53 O16 C50 119.4(2) . . ? C66 O17 Zn3 109.78(18) . 1_445 ? C66 O18 Zn1 144.2(2) . 1_445 ? C60 O19 C46 117.7(2) . . ? C70 O20 Zn3 117.2(2) . . ? O2W Zn1 O15 89.97(8) . 1_554 ? O2W Zn1 O18 176.50(8) . 1_665 ? O15 Zn1 O18 93.14(8) 1_554 1_665 ? O2W Zn1 O12 88.76(9) . . ? O15 Zn1 O12 94.52(8) 1_554 . ? O18 Zn1 O12 92.59(8) 1_665 . ? O2W Zn1 O1 87.17(8) . . ? O15 Zn1 O1 174.51(9) 1_554 . ? O18 Zn1 O1 89.59(8) 1_665 . ? O12 Zn1 O1 90.11(8) . . ? O2W Zn1 O1W 92.83(8) . . ? O15 Zn1 O1W 88.16(8) 1_554 . ? O18 Zn1 O1W 85.68(8) 1_665 . ? O12 Zn1 O1W 176.90(8) . . ? O1 Zn1 O1W 87.30(8) . . ? O3 Zn2 O9 115.07(8) . 1_445 ? O3 Zn2 O6 103.74(9) . 1_444 ? O9 Zn2 O6 106.16(9) 1_445 1_444 ? O3 Zn2 O3W 123.30(8) . . ? O9 Zn2 O3W 109.93(9) 1_445 . ? O6 Zn2 O3W 94.77(8) 1_444 . ? O3 Zn2 C33 110.56(9) . 1_445 ? O9 Zn2 C33 28.65(9) 1_445 1_445 ? O6 Zn2 C33 132.30(9) 1_444 1_445 ? O3W Zn2 C33 93.16(9) . 1_445 ? O14 Zn3 O11 123.36(9) 1_554 . ? O14 Zn3 O17 119.60(9) 1_554 1_665 ? O11 Zn3 O17 109.90(8) . 1_665 ? O14 Zn3 O20 95.53(9) 1_554 . ? O11 Zn3 O20 103.85(9) . . ? O17 Zn3 O20 97.59(9) 1_665 . ? 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 O2 C1 C2 C7 166.4(3) . . . . ? O3 C1 C2 C7 -13.3(4) . . . . ? O2 C1 C2 C3 -12.9(4) . . . . ? O3 C1 C2 C3 167.5(3) . . . . ? C7 C2 C3 C4 0.9(5) . . . . ? C1 C2 C3 C4 -179.9(3) . . . . ? C2 C3 C4 C5 0.4(5) . . . . ? C3 C4 C5 O4 176.0(3) . . . . ? C3 C4 C5 C6 -1.8(5) . . . . ? O4 C5 C6 C7 -175.9(3) . . . . ? C4 C5 C6 C7 2.0(5) . . . . ? C3 C2 C7 C6 -0.6(5) . . . . ? C1 C2 C7 C6 -179.8(3) . . . . ? C5 C6 C7 C2 -0.9(5) . . . . ? O4 C8 C9 C10 -71.8(4) . . . . ? O4 C8 C9 C18 115.4(3) . . . . ? C18 C9 C10 C12 0.7(5) . . . . ? C8 C9 C10 C12 -171.8(3) . . . . ? C18 C9 C10 C11 179.5(3) . . . . ? C8 C9 C10 C11 6.9(4) . . . . ? C9 C10 C12 C14 3.2(5) . . . . ? C11 C10 C12 C14 -175.5(3) . . . . ? C9 C10 C12 C13 176.3(3) . . . . ? C11 C10 C12 C13 -2.4(5) . . . . ? C10 C12 C13 O10 -95.8(3) . . . . ? C14 C12 C13 O10 77.2(3) . . . . ? C10 C12 C14 C16 -3.3(5) . . . . ? C13 C12 C14 C16 -176.4(3) . . . . ? C10 C12 C14 C15 175.1(3) . . . . ? C13 C12 C14 C15 2.0(5) . . . . ? C12 C14 C16 C18 -0.6(5) . . . . ? C15 C14 C16 C18 -179.0(3) . . . . ? C12 C14 C16 C17 170.1(3) . . . . ? C15 C14 C16 C17 -8.3(4) . . . . ? C14 C16 C17 O7 -75.2(3) . . . . ? C18 C16 C17 O7 95.4(3) . . . . ? C10 C9 C18 C16 -4.6(5) . . . . ? C8 C9 C18 C16 168.1(3) . . . . ? C10 C9 C18 C19 175.0(3) . . . . ? C8 C9 C18 C19 -12.4(4) . . . . ? C14 C16 C18 C9 4.5(5) . . . . ? C17 C16 C18 C9 -166.1(3) . . . . ? C14 C16 C18 C19 -175.1(3) . . . . ? C17 C16 C18 C19 14.3(5) . . . . ? O7 C20 C21 C22 178.4(3) . . . . ? C25 C20 C21 C22 -0.6(5) . . . . ? C20 C21 C22 C23 -0.6(5) . . . . ? C21 C22 C23 C24 0.6(5) . . . . ? C21 C22 C23 C26 -177.4(3) . . . . ? C22 C23 C24 C25 0.6(5) . . . . ? C26 C23 C24 C25 178.7(3) . . . . ? C23 C24 C25 C20 -1.9(5) . . . . ? O7 C20 C25 C24 -177.3(3) . . . . ? C21 C20 C25 C24 1.8(5) . . . . ? C22 C23 C26 O5 168.5(3) . . . . ? C24 C23 C26 O5 -9.5(4) . . . . ? C22 C23 C26 O6 -10.1(4) . . . . ? C24 C23 C26 O6 171.9(3) . . . . ? O10 C27 C28 C29 178.8(3) . . . . ? C32 C27 C28 C29 -1.1(4) . . . . ? C27 C28 C29 C30 -0.2(4) . . . . ? C28 C29 C30 C31 1.2(4) . . . . ? C28 C29 C30 C33 -179.6(3) . . . . ? C29 C30 C31 C32 -1.0(4) . . . . ? C33 C30 C31 C32 179.8(3) . . . . ? O10 C27 C32 C31 -178.6(3) . . . . ? C28 C27 C32 C31 1.2(4) . . . . ? C30 C31 C32 C27 -0.2(4) . . . . ? C31 C30 C33 O8 179.5(3) . . . . ? C29 C30 C33 O8 0.4(4) . . . . ? C31 C30 C33 O9 -0.4(4) . . . . ? C29 C30 C33 O9 -179.5(3) . . . . ? C31 C30 C33 Zn2 -22.1(10) . . . 1_665 ? C29 C30 C33 Zn2 158.7(7) . . . 1_665 ? O12 C34 C35 C40 -157.1(3) . . . . ? O11 C34 C35 C40 21.3(4) . . . . ? O12 C34 C35 C36 22.0(4) . . . . ? O11 C34 C35 C36 -159.7(3) . . . . ? C40 C35 C36 C37 -1.3(4) . . . . ? C34 C35 C36 C37 179.6(3) . . . . ? C35 C36 C37 C38 1.5(4) . . . . ? C36 C37 C38 O13 179.2(3) . . . . ? C36 C37 C38 C39 -1.3(4) . . . . ? O13 C38 C39 C40 -179.5(2) . . . . ? C37 C38 C39 C40 0.9(4) . . . . ? C38 C39 C40 C35 -0.7(4) . . . . ? C36 C35 C40 C39 0.9(4) . . . . ? C34 C35 C40 C39 180.0(3) . . . . ? O13 C41 C42 C43 -78.7(3) . . . . ? O13 C41 C42 C51 100.3(3) . . . . ? C51 C42 C43 C45 1.7(5) . . . . ? C41 C42 C43 C45 -179.3(3) . . . . ? C51 C42 C43 C44 -178.3(3) . . . . ? C41 C42 C43 C44 0.8(4) . . . . ? C42 C43 C45 C47 2.3(5) . . . . ? C44 C43 C45 C47 -177.7(3) . . . . ? C42 C43 C45 C46 -176.6(3) . . . . ? C44 C43 C45 C46 3.4(4) . . . . ? C47 C45 C46 O19 87.6(3) . . . . ? C43 C45 C46 O19 -93.5(3) . . . . ? C43 C45 C47 C49 -3.9(5) . . . . ? C46 C45 C47 C49 175.0(3) . . . . ? C43 C45 C47 C48 175.7(3) . . . . ? C46 C45 C47 C48 -5.4(4) . . . . ? C45 C47 C49 C51 1.4(5) . . . . ? C48 C47 C49 C51 -178.1(3) . . . . ? C45 C47 C49 C50 -173.9(3) . . . . ? C48 C47 C49 C50 6.5(5) . . . . ? C51 C49 C50 O16 -81.0(3) . . . . ? C47 C49 C50 O16 94.4(3) . . . . ? C47 C49 C51 C42 2.6(5) . . . . ? C50 C49 C51 C42 178.0(3) . . . . ? C47 C49 C51 C52 -177.7(3) . . . . ? C50 C49 C51 C52 -2.3(5) . . . . ? C43 C42 C51 C49 -4.1(5) . . . . ? C41 C42 C51 C49 176.9(3) . . . . ? C43 C42 C51 C52 176.1(3) . . . . ? C41 C42 C51 C52 -2.9(4) . . . . ? O16 C53 C54 C55 -179.5(3) . . . . ? C58 C53 C54 C55 1.7(5) . . . . ? C53 C54 C55 C56 0.0(5) . . . . ? C54 C55 C56 C57 -0.5(5) . . . . ? C54 C55 C56 C59 -179.8(3) . . . . ? C55 C56 C57 C58 -0.6(5) . . . . ? C59 C56 C57 C58 178.7(3) . . . . ? C56 C57 C58 C53 2.2(5) . . . . ? O16 C53 C58 C57 178.6(3) . . . . ? C54 C53 C58 C57 -2.7(5) . . . . ? C57 C56 C59 O14 176.4(3) . . . . ? C55 C56 C59 O14 -4.3(4) . . . . ? C57 C56 C59 O15 -3.2(4) . . . . ? C55 C56 C59 O15 176.1(3) . . . . ? O19 C60 C61 C62 176.4(3) . . . . ? C65 C60 C61 C62 -3.1(5) . . . . ? C60 C61 C62 C63 2.5(5) . . . . ? C61 C62 C63 C64 -0.4(5) . . . . ? C61 C62 C63 C66 179.7(3) . . . . ? C62 C63 C64 C65 -1.2(5) . . . . ? C66 C63 C64 C65 178.8(3) . . . . ? C63 C64 C65 C60 0.6(5) . . . . ? O19 C60 C65 C64 -177.8(3) . . . . ? C61 C60 C65 C64 1.5(5) . . . . ? C64 C63 C66 O18 -167.8(3) . . . . ? C62 C63 C66 O18 12.2(4) . . . . ? C64 C63 C66 O17 9.0(5) . . . . ? C62 C63 C66 O17 -171.0(3) . . . . ? O1 C67 N1 C68 2.4(5) . . . . ? O1 C67 N1 C69 -175.9(3) . . . . ? O20 C70 N2 C72 7.6(4) . . . . ? O20 C70 N2 C71 -167.4(3) . . . . ? N1 C67 O1 Zn1 -161.4(2) . . . . ? O2 C1 O3 Zn2 8.9(5) . . . . ? C2 C1 O3 Zn2 -171.49(19) . . . . ? C4 C5 O4 C8 17.0(4) . . . . ? C6 C5 O4 C8 -165.2(3) . . . . ? C9 C8 O4 C5 179.6(2) . . . . ? O5 C26 O6 Zn2 3.5(4) . . . 1_666 ? C23 C26 O6 Zn2 -177.98(19) . . . 1_666 ? C25 C20 O7 C17 168.0(3) . . . . ? C21 C20 O7 C17 -11.1(4) . . . . ? C16 C17 O7 C20 -158.9(2) . . . . ? O8 C33 O9 Zn2 7.7(3) . . . 1_665 ? C30 C33 O9 Zn2 -172.4(2) . . . 1_665 ? C28 C27 O10 C13 177.8(2) . . . . ? C32 C27 O10 C13 -2.4(4) . . . . ? C12 C13 O10 C27 174.1(2) . . . . ? O12 C34 O11 Zn3 -3.6(4) . . . . ? C35 C34 O11 Zn3 178.11(18) . . . . ? O11 C34 O12 Zn1 41.4(5) . . . . ? C35 C34 O12 Zn1 -140.4(3) . . . . ? C37 C38 O13 C41 3.7(4) . . . . ? C39 C38 O13 C41 -175.8(2) . . . . ? C42 C41 O13 C38 -178.7(2) . . . . ? O15 C59 O14 Zn3 1.8(4) . . . 1_556 ? C56 C59 O14 Zn3 -177.70(19) . . . 1_556 ? O14 C59 O15 Zn1 56.2(5) . . . 1_556 ? C56 C59 O15 Zn1 -124.3(3) . . . 1_556 ? C54 C53 O16 C50 174.4(3) . . . . ? C58 C53 O16 C50 -6.9(4) . . . . ? C49 C50 O16 C53 -165.5(2) . . . . ? O18 C66 O17 Zn3 -4.3(4) . . . 1_445 ? C63 C66 O17 Zn3 179.0(2) . . . 1_445 ? O17 C66 O18 Zn1 76.7(4) . . . 1_445 ? C63 C66 O18 Zn1 -106.6(4) . . . 1_445 ? C65 C60 O19 C46 7.1(4) . . . . ? C61 C60 O19 C46 -172.2(3) . . . . ? C45 C46 O19 C60 176.1(3) . . . . ? N2 C70 O20 Zn3 173.8(2) . . . . ? C34 O12 Zn1 O2W 105.2(3) . . . . ? C34 O12 Zn1 O15 15.3(3) . . . 1_554 ? C34 O12 Zn1 O18 -78.1(3) . . . 1_665 ? C34 O12 Zn1 O1 -167.7(3) . . . . ? C34 O12 Zn1 O1W -134.1(14) . . . . ? C67 O1 Zn1 O2W 44.5(2) . . . . ? C67 O1 Zn1 O15 103.2(9) . . . 1_554 ? C67 O1 Zn1 O18 -136.9(2) . . . 1_665 ? C67 O1 Zn1 O12 -44.3(2) . . . . ? C67 O1 Zn1 O1W 137.4(2) . . . . ? C1 O3 Zn2 O9 96.9(2) . . . 1_445 ? C1 O3 Zn2 O6 -147.6(2) . . . 1_444 ? C1 O3 Zn2 O3W -42.4(3) . . . . ? C1 O3 Zn2 C33 66.1(3) . . . 1_445 ? C34 O11 Zn3 O14 -79.9(2) . . . 1_554 ? C34 O11 Zn3 O17 70.2(2) . . . 1_665 ? C34 O11 Zn3 O20 173.7(2) . . . . ? C70 O20 Zn3 O14 54.3(2) . . . 1_554 ? C70 O20 Zn3 O11 -179.3(2) . . . . ? C70 O20 Zn3 O17 -66.6(2) . . . 1_665 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.708 _refine_diff_density_min -0.359 _refine_diff_density_rms 0.083 #===END _database_code_depnum_ccdc_archive 'CCDC 939262'