# 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 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H34 Co2 N2 O12' _chemical_formula_weight 912.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.763(3) _cell_length_b 21.535(2) _cell_length_c 26.471(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.687(2) _cell_angle_gamma 90.00 _cell_volume 13424(2) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6930 _cell_measurement_theta_min 2.217 _cell_measurement_theta_max 27.349 _exptl_crystal_description cubic _exptl_crystal_colour purple _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.903 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3744 _exptl_absorpt_coefficient_mu 0.536 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9004 _exptl_absorpt_correction_T_max 0.9097 _exptl_absorpt_process_details SADABS;Bruker,2000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 39055 _diffrn_reflns_av_R_equivalents 0.0618 _diffrn_reflns_av_sigmaI/netI 0.0833 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 25.50 _reflns_number_total 12505 _reflns_number_gt 6007 _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. ; _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^)+(0.0312P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12505 _refine_ls_number_parameters 584 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0955 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1168 _refine_ls_wR_factor_gt 0.1092 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.37042(16) 0.17654(19) 0.42286(13) 0.0602(10) Uani 1 1 d . . . C2 C 0.33090(14) 0.13431(17) 0.39045(13) 0.0584(9) Uani 1 1 d . . . C3 C 0.34576(16) 0.07412(19) 0.38064(14) 0.0759(12) Uani 1 1 d . . . H3 H 0.3814 0.0594 0.3941 0.091 Uiso 1 1 calc R . . C4 C 0.30823(17) 0.03509(18) 0.35093(15) 0.0810(12) Uani 1 1 d . . . H4 H 0.3186 -0.0055 0.3446 0.097 Uiso 1 1 calc R . . C5 C 0.25581(16) 0.0569(2) 0.33100(14) 0.0691(11) Uani 1 1 d . . . C6 C 0.24088(16) 0.1161(2) 0.34189(15) 0.0839(13) Uani 1 1 d . . . H6 H 0.2048 0.1306 0.3294 0.101 Uiso 1 1 calc R . . C7 C 0.27797(16) 0.15448(19) 0.37088(15) 0.0779(12) Uani 1 1 d . . . H7 H 0.2670 0.1949 0.3774 0.093 Uiso 1 1 calc R . . C8 C 0.23251(15) -0.02799(19) 0.27629(14) 0.082 Uani 1 1 d . . . H8A H 0.2396 -0.0628 0.2996 0.099 Uiso 1 1 calc R . . H8B H 0.2676 -0.0181 0.2630 0.099 Uiso 1 1 calc R . . C9 C 0.18691(14) -0.04531(16) 0.23269(13) 0.0605(9) Uani 1 1 d . . . C10 C 0.20942(15) -0.09965(17) 0.20081(14) 0.0713(11) Uani 1 1 d . . . H10A H 0.2164 -0.1368 0.2214 0.086 Uiso 1 1 calc R . . H10B H 0.1822 -0.1093 0.1712 0.086 Uiso 1 1 calc R . . C11 C 0.28896(18) -0.1131(2) 0.15637(15) 0.0752(11) Uani 1 1 d . . . C12 C 0.33901(17) -0.08664(19) 0.14810(15) 0.0839(12) Uani 1 1 d . . . H12 H 0.3504 -0.0489 0.1632 0.101 Uiso 1 1 calc R . . C13 C 0.37264(15) -0.11675(18) 0.11694(14) 0.0730(11) Uani 1 1 d . . . H13 H 0.4070 -0.0990 0.1115 0.088 Uiso 1 1 calc R . . C14 C 0.35644(14) -0.17194(16) 0.09410(12) 0.0567(9) Uani 1 1 d . . . C15 C 0.30645(15) -0.19791(17) 0.10366(14) 0.0716(11) Uani 1 1 d . . . H15 H 0.2949 -0.2357 0.0887 0.086 Uiso 1 1 calc R . . C16 C 0.27232(15) -0.1685(2) 0.13563(14) 0.0733(11) Uani 1 1 d . . . H16 H 0.2387 -0.1869 0.1425 0.088 Uiso 1 1 calc R . . C17 C 0.39046(14) -0.20073(18) 0.05660(12) 0.0543(9) Uani 1 1 d . . . C18 C 0.13103(14) -0.06536(18) 0.25409(13) 0.0693(11) Uani 1 1 d . . . H18A H 0.1177 -0.0317 0.2738 0.083 Uiso 1 1 calc R . . H18B H 0.1016 -0.0749 0.2261 0.083 Uiso 1 1 calc R . . C19 C 0.09893(18) -0.1345(2) 0.31207(15) 0.0798(12) Uani 1 1 d . . . C20 C 0.11367(18) -0.1842(2) 0.34272(17) 0.1035(16) Uani 1 1 d . . . H20 H 0.1494 -0.2023 0.3441 0.124 Uiso 1 1 calc R . . C21 C 0.07453(17) -0.2069(2) 0.37131(15) 0.0940(14) Uani 1 1 d . . . H21 H 0.0835 -0.2421 0.3910 0.113 Uiso 1 1 calc R . . C22 C 0.02170(15) -0.17925(18) 0.37203(13) 0.0650(10) Uani 1 1 d . . . C23 C 0.00907(15) -0.12745(19) 0.34266(13) 0.0705(11) Uani 1 1 d . . . H23 H -0.0254 -0.1072 0.3433 0.085 Uiso 1 1 calc R . . C24 C 0.04822(17) -0.10473(18) 0.31135(13) 0.0746(11) Uani 1 1 d . . . H24 H 0.0395 -0.0702 0.2907 0.090 Uiso 1 1 calc R . . C25 C -0.01747(16) -0.20284(19) 0.40752(13) 0.0641(10) Uani 1 1 d . . . C26 C 0.17228(15) 0.01153(18) 0.19756(14) 0.079 Uani 1 1 d . . . H26A H 0.1587 0.0453 0.2170 0.095 Uiso 1 1 calc R . . H26B H 0.2061 0.0256 0.1841 0.095 Uiso 1 1 calc R . . C27 C 0.10324(18) 0.0425(2) 0.12921(14) 0.0706(11) Uani 1 1 d . . . C28 C 0.12089(17) 0.1031(2) 0.13179(15) 0.0853(13) Uani 1 1 d . . . H28 H 0.1532 0.1147 0.1535 0.102 Uiso 1 1 calc R . . C29 C 0.08878(17) 0.14761(19) 0.10070(15) 0.0827(12) Uani 1 1 d . . . H29 H 0.1013 0.1885 0.1008 0.099 Uiso 1 1 calc R . . C30 C 0.04007(15) 0.13140(19) 0.07083(13) 0.0618(10) Uani 1 1 d . . . C31 C 0.02379(16) 0.0707(2) 0.06977(15) 0.0793(12) Uani 1 1 d . . . H31 H -0.0096 0.0591 0.0496 0.095 Uiso 1 1 calc R . . C32 C 0.05592(18) 0.02601(19) 0.09813(16) 0.0808(12) Uani 1 1 d . . . H32 H 0.0448 -0.0154 0.0957 0.097 Uiso 1 1 calc R . . C33 C 0.00426(16) 0.1792(2) 0.04073(14) 0.0632(10) Uani 1 1 d . . . C34 C 0.29277(15) 0.35327(18) 0.49730(14) 0.0815(13) Uani 1 1 d . . . H34 H 0.2905 0.3163 0.5151 0.098 Uiso 1 1 calc R . . C35 C 0.25075(16) 0.3968(2) 0.49888(15) 0.0893(14) Uani 1 1 d . . . H35 H 0.2210 0.3887 0.5175 0.107 Uiso 1 1 calc R . . C36 C 0.25216(15) 0.45235(18) 0.47328(14) 0.0691(11) Uani 1 1 d . . . C37 C 0.29607(15) 0.45974(18) 0.44590(14) 0.0763(12) Uani 1 1 d . . . H37 H 0.2984 0.4957 0.4268 0.092 Uiso 1 1 calc R . . C38 C 0.33787(14) 0.41381(17) 0.44609(13) 0.0644(10) Uani 1 1 d . . . H38 H 0.3679 0.4206 0.4275 0.077 Uiso 1 1 calc R . . C39 C 0.20848(18) 0.49964(19) 0.47325(15) 0.0886(14) Uani 1 1 d . . . H39 H 0.2141 0.5360 0.4557 0.106 Uiso 1 1 calc R . . C40 C 0.16430(18) 0.4972(2) 0.49395(16) 0.0974(15) Uani 1 1 d . . . H40 H 0.1592 0.4612 0.5121 0.117 Uiso 1 1 calc R . . C41 C 0.1193(2) 0.5444(2) 0.4932(2) 0.0838(14) Uani 1 1 d . . . C42 C 0.0648(4) 0.5304(4) 0.5020(4) 0.108(3) Uani 0.712(9) 1 d P . 1 H42 H 0.0541 0.4892 0.5048 0.130 Uiso 0.712(9) 1 calc PR . 1 C43 C 0.0265(4) 0.5767(5) 0.5067(4) 0.105(3) Uani 0.712(9) 1 d P . 1 H43 H -0.0079 0.5672 0.5181 0.126 Uiso 0.712(9) 1 calc PR . 1 C44 C 0.0902(3) 0.6496(3) 0.4912(3) 0.094(3) Uani 0.712(9) 1 d P . 1 H44 H 0.1002 0.6914 0.4905 0.113 Uiso 0.712(9) 1 calc PR . 1 C45 C 0.1319(3) 0.6045(4) 0.4879(4) 0.102(3) Uani 0.712(9) 1 d P . 1 H45 H 0.1682 0.6161 0.4821 0.123 Uiso 0.712(9) 1 calc PR . 1 N1 N 0.038(5) 0.635(6) 0.495(3) 0.063(6) Uani 0.712(9) 1 d P . 1 C43' C 0.0562(8) 0.6192(8) 0.4541(8) 0.084(6) Uani 0.288(9) 1 d P . 2 H43' H 0.0418 0.6353 0.4224 0.101 Uiso 0.288(9) 1 calc PR . 2 C45' C 0.0977(8) 0.5619(9) 0.5350(8) 0.095(7) Uani 0.288(9) 1 d P . 2 H45' H 0.1097 0.5418 0.5656 0.114 Uiso 0.288(9) 1 calc PR . 2 C42' C 0.1001(8) 0.5753(10) 0.4546(8) 0.091(6) Uani 0.288(9) 1 d P . 2 H42' H 0.1158 0.5688 0.4247 0.109 Uiso 0.288(9) 1 calc PR . 2 C44' C 0.0576(8) 0.6094(11) 0.5342(9) 0.086(6) Uani 0.288(9) 1 d P . 2 H44' H 0.0469 0.6205 0.5655 0.104 Uiso 0.288(9) 1 calc PR . 2 N1' N 0.033(12) 0.640(15) 0.494(9) 0.08(5) Uani 0.288(9) 1 d P . 2 Co1 Co 0.475783(17) 0.20300(2) 0.493489(16) 0.05185(15) Uani 1 1 d . . . Co2 Co 0.398137(16) 0.29568(2) 0.470334(16) 0.04954(14) Uani 1 1 d . . . N2 N 0.33639(10) 0.36152(13) 0.47147(10) 0.0520(7) Uani 1 1 d . . . O1 O 0.41703(10) 0.15421(11) 0.44381(8) 0.0685(7) Uani 1 1 d . . . O2 O 0.35435(9) 0.23146(12) 0.42720(9) 0.0696(7) Uani 1 1 d . . . O3 O 0.21455(11) 0.02307(13) 0.30198(10) 0.0891(8) Uani 1 1 d . . . O4 O 0.25945(11) -0.07703(13) 0.18638(10) 0.0868(8) Uani 1 1 d . . . O5 O 0.43594(9) -0.17292(11) 0.05014(8) 0.0681(7) Uani 1 1 d . . . O6 O 0.37246(9) -0.24867(11) 0.03368(8) 0.0653(7) Uani 1 1 d . . . O7 O 0.14248(11) -0.11648(14) 0.28424(11) 0.0928(9) Uani 1 1 d . . . O8 O -0.06218(10) -0.17298(12) 0.41167(9) 0.0741(7) Uani 1 1 d . . . O9 O -0.00152(10) -0.25089(12) 0.43308(9) 0.0757(7) Uani 1 1 d . . . O10 O 0.13072(10) -0.00475(12) 0.15770(9) 0.0816(8) Uani 1 1 d . . . O11 O 0.02218(10) 0.23360(12) 0.03862(9) 0.0706(7) Uani 1 1 d . . . O12 O -0.04276(10) 0.16008(11) 0.01799(9) 0.0711(7) 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 0.059(3) 0.066(3) 0.059(3) -0.006(2) 0.0209(19) 0.002(2) C2 0.053(2) 0.060(3) 0.063(2) -0.007(2) 0.0130(18) 0.007(2) C3 0.063(3) 0.074(3) 0.087(3) -0.018(2) -0.002(2) 0.014(2) C4 0.077(3) 0.071(3) 0.094(3) -0.027(2) 0.006(2) 0.014(2) C5 0.060(3) 0.081(3) 0.065(3) -0.018(2) 0.0015(19) -0.001(2) C6 0.066(3) 0.085(3) 0.096(3) -0.020(3) -0.004(2) 0.013(3) C7 0.063(3) 0.072(3) 0.097(3) -0.015(2) 0.003(2) 0.012(2) C8 0.078 0.083 0.084 0.002 0.002 0.001 C9 0.059(2) 0.066(3) 0.057(2) 0.000(2) 0.0093(17) -0.004(2) C10 0.067(3) 0.074(3) 0.075(3) 0.004(2) 0.017(2) -0.005(2) C11 0.077(3) 0.077(3) 0.077(3) -0.012(2) 0.028(2) -0.002(3) C12 0.080(3) 0.081(3) 0.095(3) -0.034(2) 0.031(2) -0.013(3) C13 0.062(2) 0.076(3) 0.085(3) -0.030(2) 0.025(2) -0.022(2) C14 0.051(2) 0.060(3) 0.063(2) -0.0096(19) 0.0209(17) -0.0154(19) C15 0.075(3) 0.060(3) 0.088(3) -0.014(2) 0.042(2) -0.021(2) C16 0.070(3) 0.079(3) 0.079(3) -0.002(2) 0.041(2) -0.012(2) C17 0.048(2) 0.064(3) 0.054(2) -0.004(2) 0.0163(16) -0.016(2) C18 0.070(3) 0.072(3) 0.065(3) 0.000(2) 0.0067(19) -0.001(2) C19 0.069(3) 0.108(4) 0.069(3) 0.007(3) 0.036(2) 0.002(3) C20 0.090(3) 0.121(4) 0.111(4) 0.042(3) 0.052(3) 0.027(3) C21 0.089(3) 0.099(4) 0.106(3) 0.037(3) 0.056(3) 0.032(3) C22 0.061(2) 0.078(3) 0.062(3) 0.014(2) 0.0325(18) 0.012(2) C23 0.062(3) 0.087(3) 0.066(3) 0.009(2) 0.0176(19) 0.007(2) C24 0.078(3) 0.088(3) 0.058(3) 0.022(2) 0.008(2) 0.005(2) C25 0.062(3) 0.068(3) 0.068(3) 0.004(2) 0.0289(19) 0.005(2) C26 0.064 0.086 0.087 0.002 0.009 0.001 C27 0.085(3) 0.070(3) 0.059(3) -0.003(2) 0.019(2) 0.003(3) C28 0.088(3) 0.082(4) 0.080(3) -0.002(3) -0.011(2) -0.004(3) C29 0.083(3) 0.071(3) 0.090(3) 0.008(2) -0.007(2) -0.006(2) C30 0.059(3) 0.064(3) 0.063(3) 0.007(2) 0.0118(19) -0.008(2) C31 0.066(3) 0.081(3) 0.089(3) 0.016(3) 0.007(2) -0.010(3) C32 0.081(3) 0.072(3) 0.090(3) 0.009(3) 0.013(2) -0.009(3) C33 0.055(3) 0.072(3) 0.065(3) 0.001(2) 0.016(2) 0.000(2) C34 0.073(3) 0.079(3) 0.104(3) 0.041(2) 0.051(2) 0.041(2) C35 0.077(3) 0.098(4) 0.105(3) 0.042(3) 0.057(2) 0.049(3) C36 0.065(3) 0.069(3) 0.079(3) 0.018(2) 0.026(2) 0.041(2) C37 0.075(3) 0.064(3) 0.096(3) 0.027(2) 0.033(2) 0.034(2) C38 0.056(2) 0.063(3) 0.079(3) 0.016(2) 0.0252(18) 0.020(2) C39 0.086(3) 0.079(3) 0.109(4) 0.020(2) 0.042(3) 0.046(3) C40 0.095(3) 0.087(4) 0.117(4) 0.017(3) 0.041(3) 0.053(3) C41 0.071(3) 0.081(4) 0.103(4) 0.004(3) 0.027(3) 0.045(3) C42 0.085(6) 0.083(6) 0.159(8) 0.011(5) 0.024(5) 0.040(5) C43 0.079(6) 0.089(7) 0.153(8) 0.011(6) 0.034(6) 0.034(5) C44 0.074(6) 0.079(5) 0.131(7) 0.000(5) 0.022(5) 0.027(4) C45 0.066(5) 0.096(7) 0.149(8) 0.001(6) 0.025(5) 0.036(5) N1 0.050(10) 0.063(14) 0.080(17) 0.007(9) 0.021(8) 0.028(12) C43' 0.078(12) 0.083(13) 0.093(14) -0.002(10) 0.014(11) 0.040(10) C45' 0.089(14) 0.092(14) 0.108(15) 0.006(11) 0.024(12) 0.053(12) C42' 0.082(13) 0.097(14) 0.097(15) -0.003(12) 0.021(10) 0.049(12) C44' 0.078(14) 0.080(14) 0.105(16) 0.004(13) 0.025(11) 0.043(13) N1' 0.06(6) 0.07(7) 0.10(5) 0.01(3) 0.02(3) 0.02(4) Co1 0.0422(3) 0.0507(3) 0.0651(3) 0.0033(2) 0.0163(2) 0.0178(2) Co2 0.0396(3) 0.0481(3) 0.0634(3) 0.0010(2) 0.0160(2) 0.0153(2) N2 0.0479(17) 0.053(2) 0.0589(19) 0.0137(15) 0.0191(13) 0.0210(14) O1 0.0617(16) 0.0703(18) 0.0724(17) -0.0084(13) 0.0049(13) 0.0072(14) O2 0.0628(16) 0.0562(17) 0.0905(19) -0.0143(14) 0.0127(13) 0.0084(14) O3 0.0786(19) 0.091(2) 0.101(2) -0.0419(17) 0.0229(15) -0.0046(16) O4 0.081(2) 0.090(2) 0.096(2) -0.0092(16) 0.0362(16) -0.0058(17) O5 0.0578(15) 0.0775(19) 0.0745(17) -0.0164(13) 0.0293(12) -0.0210(13) O6 0.0641(16) 0.0657(18) 0.0718(17) -0.0218(14) 0.0302(12) -0.0186(14) O7 0.082(2) 0.104(2) 0.099(2) 0.0257(18) 0.0373(16) 0.0167(17) O8 0.0613(16) 0.085(2) 0.0840(18) 0.0138(14) 0.0372(13) 0.0193(14) O9 0.0809(18) 0.072(2) 0.0815(19) 0.0192(15) 0.0389(13) 0.0190(15) O10 0.0851(19) 0.084(2) 0.0732(18) -0.0060(15) 0.0000(14) 0.0110(16) O11 0.0650(17) 0.0630(18) 0.0830(19) 0.0054(14) 0.0071(12) -0.0133(14) O12 0.0545(16) 0.0686(18) 0.0900(19) 0.0097(14) 0.0091(13) -0.0052(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.253(4) . ? C1 O1 1.265(4) . ? C1 C2 1.493(4) . ? C2 C7 1.365(4) . ? C2 C3 1.377(4) . ? C3 C4 1.390(4) . ? C3 H3 0.9300 . ? C4 C5 1.369(4) . ? C4 H4 0.9300 . ? C5 C6 1.364(5) . ? C5 O3 1.372(4) . ? C6 C7 1.366(5) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 O3 1.390(4) . ? C8 C9 1.520(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C26 1.548(4) . ? C9 C18 1.572(4) . ? C9 C10 1.578(5) . ? C10 O4 1.385(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C16 1.351(5) . ? C11 C12 1.362(5) . ? C11 O4 1.369(4) . ? C12 C13 1.384(5) . ? C12 H12 0.9300 . ? C13 C14 1.365(4) . ? C13 H13 0.9300 . ? C14 C15 1.367(4) . ? C14 C17 1.496(4) . ? C15 C16 1.399(4) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 O6 1.244(4) . ? C17 O5 1.267(3) . ? C18 O7 1.366(4) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.361(5) . ? C19 C24 1.363(5) . ? C19 O7 1.403(4) . ? C20 C21 1.366(5) . ? C20 H20 0.9300 . ? C21 C22 1.392(4) . ? C21 H21 0.9300 . ? C22 C23 1.370(4) . ? C22 C25 1.497(4) . ? C23 C24 1.413(5) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 O8 1.259(4) . ? C25 O9 1.266(4) . ? C26 O10 1.390(4) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C32 1.349(5) . ? C27 C28 1.369(5) . ? C27 O10 1.378(4) . ? C28 C29 1.419(5) . ? C28 H28 0.9300 . ? C29 C30 1.357(4) . ? C29 H29 0.9300 . ? C30 C31 1.362(5) . ? C30 C33 1.495(5) . ? C31 C32 1.386(5) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 O11 1.251(4) . ? C33 O12 1.265(4) . ? C34 N2 1.328(4) . ? C34 C35 1.374(4) . ? C34 H34 0.9300 . ? C35 C36 1.377(5) . ? C35 H35 0.9300 . ? C36 C37 1.357(4) . ? C36 C39 1.454(4) . ? C37 C38 1.401(4) . ? C37 H37 0.9300 . ? C38 N2 1.314(4) . ? C38 H38 0.9300 . ? C39 C40 1.249(5) . ? C39 H39 0.9300 . ? C40 C41 1.474(5) . ? C40 H40 0.9300 . ? C41 C42' 1.252(18) . ? C41 C45' 1.334(18) . ? C41 C45 1.340(9) . ? C41 C42 1.378(9) . ? C42 C43 1.366(9) . ? C42 H42 0.9300 . ? C43 N1 1.32(12) . ? C43 H43 0.9300 . ? C44 N1 1.31(10) . ? C44 C45 1.399(8) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? N1 Co1 2.07(13) 3_455 ? C43' N1' 1.3(2) . ? C43' C42' 1.41(2) . ? C43' H43' 0.9300 . ? C45' C44' 1.39(2) . ? C45' H45' 0.9300 . ? C42' H42' 0.9300 . ? C44' N1' 1.3(3) . ? C44' H44' 0.9300 . ? N1' Co1 1.9(3) 3_455 ? Co1 N1' 1.9(3) 3_545 ? Co1 O5 1.986(2) 6_556 ? Co1 O9 2.016(2) 3 ? Co1 O11 2.038(2) 8_556 ? Co1 N1 2.07(13) 3_545 ? Co1 O1 2.072(2) . ? Co1 Co2 2.7313(6) . ? Co2 O2 1.995(2) . ? Co2 O12 2.000(2) 8_556 ? Co2 O8 2.037(2) 3 ? Co2 N2 2.044(2) . ? Co2 O6 2.117(2) 6_556 ? O5 Co1 1.986(2) 6 ? O6 Co2 2.117(2) 6 ? O8 Co2 2.037(2) 3_445 ? O9 Co1 2.016(2) 3_445 ? O11 Co1 2.038(2) 8_455 ? O12 Co2 2.000(2) 8_455 ? 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 125.3(3) . . ? O2 C1 C2 116.9(3) . . ? O1 C1 C2 117.8(4) . . ? C7 C2 C3 118.3(3) . . ? C7 C2 C1 120.1(4) . . ? C3 C2 C1 121.6(3) . . ? C2 C3 C4 121.0(3) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C5 C4 C3 119.4(4) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C6 C5 C4 119.2(4) . . ? C6 C5 O3 115.4(3) . . ? C4 C5 O3 125.3(4) . . ? C5 C6 C7 121.1(4) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C2 C7 C6 120.9(4) . . ? C2 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? O3 C8 C9 109.3(3) . . ? O3 C8 H8A 109.8 . . ? C9 C8 H8A 109.8 . . ? O3 C8 H8B 109.8 . . ? C9 C8 H8B 109.8 . . ? H8A C8 H8B 108.3 . . ? C8 C9 C26 110.0(3) . . ? C8 C9 C18 110.1(3) . . ? C26 C9 C18 107.5(3) . . ? C8 C9 C10 109.3(3) . . ? C26 C9 C10 109.3(3) . . ? C18 C9 C10 110.6(3) . . ? O4 C10 C9 104.6(3) . . ? O4 C10 H10A 110.8 . . ? C9 C10 H10A 110.8 . . ? O4 C10 H10B 110.8 . . ? C9 C10 H10B 110.8 . . ? H10A C10 H10B 108.9 . . ? C16 C11 C12 121.2(4) . . ? C16 C11 O4 126.3(4) . . ? C12 C11 O4 112.5(4) . . ? C11 C12 C13 119.1(4) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? C14 C13 C12 121.4(4) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C13 C14 C15 118.4(3) . . ? C13 C14 C17 120.6(3) . . ? C15 C14 C17 120.9(3) . . ? C14 C15 C16 121.0(3) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C11 C16 C15 118.9(4) . . ? C11 C16 H16 120.5 . . ? C15 C16 H16 120.5 . . ? O6 C17 O5 124.8(3) . . ? O6 C17 C14 119.1(3) . . ? O5 C17 C14 116.1(3) . . ? O7 C18 C9 108.7(3) . . ? O7 C18 H18A 110.0 . . ? C9 C18 H18A 110.0 . . ? O7 C18 H18B 110.0 . . ? C9 C18 H18B 110.0 . . ? H18A C18 H18B 108.3 . . ? C20 C19 C24 122.3(4) . . ? C20 C19 O7 112.4(4) . . ? C24 C19 O7 125.2(4) . . ? C19 C20 C21 118.1(4) . . ? C19 C20 H20 120.9 . . ? C21 C20 H20 120.9 . . ? C20 C21 C22 122.5(4) . . ? C20 C21 H21 118.7 . . ? C22 C21 H21 118.8 . . ? C23 C22 C21 118.0(3) . . ? C23 C22 C25 121.7(3) . . ? C21 C22 C25 120.1(4) . . ? C22 C23 C24 120.2(4) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C19 C24 C23 118.6(4) . . ? C19 C24 H24 120.7 . . ? C23 C24 H24 120.7 . . ? O8 C25 O9 124.5(3) . . ? O8 C25 C22 119.0(4) . . ? O9 C25 C22 116.5(3) . . ? O10 C26 C9 109.6(3) . . ? O10 C26 H26A 109.7 . . ? C9 C26 H26A 109.7 . . ? O10 C26 H26B 109.7 . . ? C9 C26 H26B 109.7 . . ? H26A C26 H26B 108.2 . . ? C32 C27 C28 120.4(4) . . ? C32 C27 O10 115.8(4) . . ? C28 C27 O10 123.8(4) . . ? C27 C28 C29 118.5(4) . . ? C27 C28 H28 120.7 . . ? C29 C28 H28 120.7 . . ? C30 C29 C28 121.0(4) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C29 C30 C31 118.5(4) . . ? C29 C30 C33 120.9(4) . . ? C31 C30 C33 120.6(4) . . ? C30 C31 C32 121.4(4) . . ? C30 C31 H31 119.3 . . ? C32 C31 H31 119.3 . . ? C27 C32 C31 120.1(4) . . ? C27 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? O11 C33 O12 124.6(4) . . ? O11 C33 C30 119.7(3) . . ? O12 C33 C30 115.7(4) . . ? N2 C34 C35 123.0(3) . . ? N2 C34 H34 118.5 . . ? C35 C34 H34 118.5 . . ? C34 C35 C36 120.8(3) . . ? C34 C35 H35 119.6 . . ? C36 C35 H35 119.6 . . ? C37 C36 C35 115.8(3) . . ? C37 C36 C39 121.2(4) . . ? C35 C36 C39 123.0(4) . . ? C36 C37 C38 120.7(3) . . ? C36 C37 H37 119.7 . . ? C38 C37 H37 119.7 . . ? N2 C38 C37 122.6(3) . . ? N2 C38 H38 118.7 . . ? C37 C38 H38 118.7 . . ? C40 C39 C36 127.8(4) . . ? C40 C39 H39 116.1 . . ? C36 C39 H39 116.1 . . ? C39 C40 C41 128.1(5) . . ? C39 C40 H40 115.9 . . ? C41 C40 H40 115.9 . . ? C42' C41 C45' 112.9(11) . . ? C42' C41 C45 57.6(9) . . ? C45' C41 C45 86.1(10) . . ? C42' C41 C42 90.4(10) . . ? C45' C41 C42 56.5(8) . . ? C45 C41 C42 117.3(5) . . ? C42' C41 C40 124.1(9) . . ? C45' C41 C40 122.9(8) . . ? C45 C41 C40 119.6(5) . . ? C42 C41 C40 122.9(6) . . ? C43 C42 C41 120.5(7) . . ? C43 C42 H42 119.7 . . ? C41 C42 H42 119.7 . . ? N1 C43 C42 121(5) . . ? N1 C43 H43 119.5 . . ? C42 C43 H43 119.5 . . ? N1 C44 C45 122(6) . . ? N1 C44 H44 119.1 . . ? C45 C44 H44 119.1 . . ? C41 C45 C44 119.5(6) . . ? C41 C45 H45 120.2 . . ? C44 C45 H45 120.2 . . ? C44 N1 C43 118(10) . . ? C44 N1 Co1 120(8) . 3_455 ? C43 N1 Co1 121(6) . 3_455 ? N1' C43' C42' 127(10) . . ? N1' C43' H43' 116.2 . . ? C42' C43' H43' 116.3 . . ? C41 C45' C44' 122.1(16) . . ? C41 C45' H45' 118.9 . . ? C44' C45' H45' 118.9 . . ? C41 C42' C43' 123.6(15) . . ? C41 C42' H42' 118.2 . . ? C43' C42' H42' 118.2 . . ? N1' C44' C45' 127(10) . . ? N1' C44' H44' 116.4 . . ? C45' C44' H44' 116.4 . . ? C43' N1' C44' 106(10) . . ? C43' N1' Co1 128(10) . 3_455 ? C44' N1' Co1 126(10) . 3_455 ? N1' Co1 O5 100(7) 3_545 6_556 ? N1' Co1 O9 95(7) 3_545 3 ? O5 Co1 O9 164.71(10) 6_556 3 ? N1' Co1 O11 98(9) 3_545 8_556 ? O5 Co1 O11 92.92(10) 6_556 8_556 ? O9 Co1 O11 87.36(10) 3 8_556 ? N1' Co1 N1 1(9) 3_545 3_545 ? O5 Co1 N1 99(2) 6_556 3_545 ? O9 Co1 N1 96(2) 3 3_545 ? O11 Co1 N1 98(3) 8_556 3_545 ? N1' Co1 O1 94(9) 3_545 . ? O5 Co1 O1 87.99(10) 6_556 . ? O9 Co1 O1 88.59(10) 3 . ? O11 Co1 O1 167.85(10) 8_556 . ? N1 Co1 O1 94(3) 3_545 . ? N1' Co1 Co2 167(7) 3_545 . ? O5 Co1 Co2 91.82(7) 6_556 . ? O9 Co1 Co2 72.93(7) 3 . ? O11 Co1 Co2 86.46(7) 8_556 . ? N1 Co1 Co2 168(2) 3_545 . ? O1 Co1 Co2 81.40(7) . . ? O2 Co2 O12 163.72(10) . 8_556 ? O2 Co2 O8 93.02(10) . 3 ? O12 Co2 O8 88.01(10) 8_556 3 ? O2 Co2 N2 99.73(10) . . ? O12 Co2 N2 96.03(10) 8_556 . ? O8 Co2 N2 100.82(10) 3 . ? O2 Co2 O6 86.47(10) . 6_556 ? O12 Co2 O6 88.89(9) 8_556 6_556 ? O8 Co2 O6 166.96(9) 3 6_556 ? N2 Co2 O6 92.10(10) . 6_556 ? O2 Co2 Co1 84.66(7) . . ? O12 Co2 Co1 79.06(7) 8_556 . ? O8 Co2 Co1 92.61(7) 3 . ? N2 Co2 Co1 165.58(8) . . ? O6 Co2 Co1 74.37(6) 6_556 . ? C38 N2 C34 117.0(3) . . ? C38 N2 Co2 121.2(2) . . ? C34 N2 Co2 121.7(2) . . ? C1 O1 Co1 124.2(2) . . ? C1 O2 Co2 124.4(2) . . ? C5 O3 C8 116.8(3) . . ? C11 O4 C10 119.1(3) . . ? C17 O5 Co1 116.7(2) . 6 ? C17 O6 Co2 131.8(2) . 6 ? C18 O7 C19 115.2(3) . . ? C25 O8 Co2 112.3(2) . 3_445 ? C25 O9 Co1 137.2(2) . 3_445 ? C27 O10 C26 117.8(3) . . ? C33 O11 Co1 119.5(2) . 8_455 ? C33 O12 Co2 130.3(2) . 8_455 ? 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 -5.8(5) . . . . ? O1 C1 C2 C7 173.9(3) . . . . ? O2 C1 C2 C3 176.1(3) . . . . ? O1 C1 C2 C3 -4.2(5) . . . . ? C7 C2 C3 C4 1.0(6) . . . . ? C1 C2 C3 C4 179.2(4) . . . . ? C2 C3 C4 C5 0.2(6) . . . . ? C3 C4 C5 C6 -1.8(6) . . . . ? C3 C4 C5 O3 -178.7(4) . . . . ? C4 C5 C6 C7 2.2(6) . . . . ? O3 C5 C6 C7 179.4(4) . . . . ? C3 C2 C7 C6 -0.6(6) . . . . ? C1 C2 C7 C6 -178.8(4) . . . . ? C5 C6 C7 C2 -1.0(7) . . . . ? O3 C8 C9 C26 55.4(4) . . . . ? O3 C8 C9 C18 -63.0(4) . . . . ? O3 C8 C9 C10 175.3(3) . . . . ? C8 C9 C10 O4 -56.0(4) . . . . ? C26 C9 C10 O4 64.4(3) . . . . ? C18 C9 C10 O4 -177.4(3) . . . . ? C16 C11 C12 C13 1.4(6) . . . . ? O4 C11 C12 C13 -177.8(3) . . . . ? C11 C12 C13 C14 0.6(6) . . . . ? C12 C13 C14 C15 -1.5(6) . . . . ? C12 C13 C14 C17 174.0(3) . . . . ? C13 C14 C15 C16 0.6(6) . . . . ? C17 C14 C15 C16 -174.9(3) . . . . ? C12 C11 C16 C15 -2.3(6) . . . . ? O4 C11 C16 C15 176.8(4) . . . . ? C14 C15 C16 C11 1.3(6) . . . . ? C13 C14 C17 O6 -174.9(3) . . . . ? C15 C14 C17 O6 0.6(5) . . . . ? C13 C14 C17 O5 4.1(5) . . . . ? C15 C14 C17 O5 179.5(3) . . . . ? C8 C9 C18 O7 -61.7(4) . . . . ? C26 C9 C18 O7 178.5(3) . . . . ? C10 C9 C18 O7 59.2(4) . . . . ? C24 C19 C20 C21 3.9(7) . . . . ? O7 C19 C20 C21 -179.0(4) . . . . ? C19 C20 C21 C22 -3.2(7) . . . . ? C20 C21 C22 C23 0.2(7) . . . . ? C20 C21 C22 C25 -174.7(4) . . . . ? C21 C22 C23 C24 2.3(6) . . . . ? C25 C22 C23 C24 177.0(3) . . . . ? C20 C19 C24 C23 -1.6(6) . . . . ? O7 C19 C24 C23 -178.2(4) . . . . ? C22 C23 C24 C19 -1.6(6) . . . . ? C23 C22 C25 O8 -2.5(6) . . . . ? C21 C22 C25 O8 172.2(4) . . . . ? C23 C22 C25 O9 -179.6(3) . . . . ? C21 C22 C25 O9 -5.0(6) . . . . ? C8 C9 C26 O10 179.8(3) . . . . ? C18 C9 C26 O10 -60.3(4) . . . . ? C10 C9 C26 O10 59.8(4) . . . . ? C32 C27 C28 C29 -0.8(6) . . . . ? O10 C27 C28 C29 -179.7(4) . . . . ? C27 C28 C29 C30 3.2(6) . . . . ? C28 C29 C30 C31 -2.6(6) . . . . ? C28 C29 C30 C33 175.9(4) . . . . ? C29 C30 C31 C32 -0.3(6) . . . . ? C33 C30 C31 C32 -178.8(4) . . . . ? C28 C27 C32 C31 -2.1(6) . . . . ? O10 C27 C32 C31 176.9(3) . . . . ? C30 C31 C32 C27 2.7(6) . . . . ? C29 C30 C33 O11 7.7(6) . . . . ? C31 C30 C33 O11 -173.8(4) . . . . ? C29 C30 C33 O12 -173.7(3) . . . . ? C31 C30 C33 O12 4.8(5) . . . . ? N2 C34 C35 C36 -0.2(7) . . . . ? C34 C35 C36 C37 1.9(6) . . . . ? C34 C35 C36 C39 179.3(4) . . . . ? C35 C36 C37 C38 -2.4(6) . . . . ? C39 C36 C37 C38 -179.9(4) . . . . ? C36 C37 C38 N2 1.3(6) . . . . ? C37 C36 C39 C40 175.2(5) . . . . ? C35 C36 C39 C40 -2.1(7) . . . . ? C36 C39 C40 C41 -178.6(4) . . . . ? C39 C40 C41 C42' 41.1(17) . . . . ? C39 C40 C41 C45' -133.7(14) . . . . ? C39 C40 C41 C45 -27.8(10) . . . . ? C39 C40 C41 C42 157.8(7) . . . . ? C42' C41 C42 C43 -55.3(13) . . . . ? C45' C41 C42 C43 62.2(12) . . . . ? C45 C41 C42 C43 -2.0(13) . . . . ? C40 C41 C42 C43 172.5(7) . . . . ? C41 C42 C43 N1 10(5) . . . . ? C42' C41 C45 C44 71.2(11) . . . . ? C45' C41 C45 C44 -49.1(12) . . . . ? C42 C41 C45 C44 -0.3(13) . . . . ? C40 C41 C45 C44 -175.0(6) . . . . ? N1 C44 C45 C41 -6(5) . . . . ? C45 C44 N1 C43 14(9) . . . . ? C45 C44 N1 Co1 -174(3) . . . 3_455 ? C42 C43 N1 C44 -16(9) . . . . ? C42 C43 N1 Co1 172(3) . . . 3_455 ? C42' C41 C45' C44' 1(3) . . . . ? C45 C41 C45' C44' 53(2) . . . . ? C42 C41 C45' C44' -74(2) . . . . ? C40 C41 C45' C44' 175.9(16) . . . . ? C45' C41 C42' C43' -6(3) . . . . ? C45 C41 C42' C43' -75(2) . . . . ? C42 C41 C42' C43' 47(2) . . . . ? C40 C41 C42' C43' 178.5(14) . . . . ? N1' C43' C42' C41 9(17) . . . . ? C41 C45' C44' N1' 4(17) . . . . ? C42' C43' N1' C44' -3(27) . . . . ? C42' C43' N1' Co1 177(11) . . . 3_455 ? C45' C44' N1' C43' -3(27) . . . . ? C45' C44' N1' Co1 177(10) . . . 3_455 ? N1' Co1 Co2 O2 70(38) 3_545 . . . ? O5 Co1 Co2 O2 -86.78(10) 6_556 . . . ? O9 Co1 Co2 O2 92.08(10) 3 . . . ? O11 Co1 Co2 O2 -179.60(10) 8_556 . . . ? N1 Co1 Co2 O2 69(14) 3_545 . . . ? O1 Co1 Co2 O2 0.91(10) . . . . ? N1' Co1 Co2 O12 -111(38) 3_545 . . 8_556 ? O5 Co1 Co2 O12 92.96(10) 6_556 . . 8_556 ? O9 Co1 Co2 O12 -88.18(10) 3 . . 8_556 ? O11 Co1 Co2 O12 0.14(10) 8_556 . . 8_556 ? N1 Co1 Co2 O12 -111(14) 3_545 . . 8_556 ? O1 Co1 Co2 O12 -179.35(10) . . . 8_556 ? N1' Co1 Co2 O8 -23(38) 3_545 . . 3 ? O5 Co1 Co2 O8 -179.57(10) 6_556 . . 3 ? O9 Co1 Co2 O8 -0.71(10) 3 . . 3 ? O11 Co1 Co2 O8 87.61(10) 8_556 . . 3 ? N1 Co1 Co2 O8 -24(14) 3_545 . . 3 ? O1 Co1 Co2 O8 -91.88(10) . . . 3 ? N1' Co1 Co2 N2 178(38) 3_545 . . . ? O5 Co1 Co2 N2 21.7(3) 6_556 . . . ? O9 Co1 Co2 N2 -159.4(3) 3 . . . ? O11 Co1 Co2 N2 -71.1(3) 8_556 . . . ? N1 Co1 Co2 N2 178(14) 3_545 . . . ? O1 Co1 Co2 N2 109.4(3) . . . . ? N1' Co1 Co2 O6 158(38) 3_545 . . 6_556 ? O5 Co1 Co2 O6 1.03(9) 6_556 . . 6_556 ? O9 Co1 Co2 O6 179.89(10) 3 . . 6_556 ? O11 Co1 Co2 O6 -91.79(10) 8_556 . . 6_556 ? N1 Co1 Co2 O6 157(14) 3_545 . . 6_556 ? O1 Co1 Co2 O6 88.73(9) . . . 6_556 ? C37 C38 N2 C34 0.4(5) . . . . ? C37 C38 N2 Co2 179.7(3) . . . . ? C35 C34 N2 C38 -0.9(6) . . . . ? C35 C34 N2 Co2 179.8(3) . . . . ? O2 Co2 N2 C38 -108.1(3) . . . . ? O12 Co2 N2 C38 76.1(3) 8_556 . . . ? O8 Co2 N2 C38 -13.1(3) 3 . . . ? O6 Co2 N2 C38 165.2(3) 6_556 . . . ? Co1 Co2 N2 C38 145.2(3) . . . . ? O2 Co2 N2 C34 71.2(3) . . . . ? O12 Co2 N2 C34 -104.7(3) 8_556 . . . ? O8 Co2 N2 C34 166.2(3) 3 . . . ? O6 Co2 N2 C34 -15.6(3) 6_556 . . . ? Co1 Co2 N2 C34 -35.5(5) . . . . ? O2 C1 O1 Co1 3.4(5) . . . . ? C2 C1 O1 Co1 -176.3(2) . . . . ? N1' Co1 O1 C1 -170(7) 3_545 . . . ? O5 Co1 O1 C1 89.8(3) 6_556 . . . ? O9 Co1 O1 C1 -75.3(3) 3 . . . ? O11 Co1 O1 C1 -4.8(6) 8_556 . . . ? N1 Co1 O1 C1 -171(2) 3_545 . . . ? Co2 Co1 O1 C1 -2.4(3) . . . . ? O1 C1 O2 Co2 -2.0(5) . . . . ? C2 C1 O2 Co2 177.6(2) . . . . ? O12 Co2 O2 C1 -0.8(5) 8_556 . . . ? O8 Co2 O2 C1 92.5(3) 3 . . . ? N2 Co2 O2 C1 -166.0(3) . . . . ? O6 Co2 O2 C1 -74.5(3) 6_556 . . . ? Co1 Co2 O2 C1 0.1(3) . . . . ? C6 C5 O3 C8 159.4(4) . . . . ? C4 C5 O3 C8 -23.6(6) . . . . ? C9 C8 O3 C5 -159.7(3) . . . . ? C16 C11 O4 C10 4.9(6) . . . . ? C12 C11 O4 C10 -175.9(3) . . . . ? C9 C10 O4 C11 -178.0(3) . . . . ? O6 C17 O5 Co1 7.6(5) . . . 6 ? C14 C17 O5 Co1 -171.3(2) . . . 6 ? O5 C17 O6 Co2 -10.5(5) . . . 6 ? C14 C17 O6 Co2 168.4(2) . . . 6 ? C9 C18 O7 C19 171.1(3) . . . . ? C20 C19 O7 C18 -177.8(4) . . . . ? C24 C19 O7 C18 -0.8(6) . . . . ? O9 C25 O8 Co2 6.8(5) . . . 3_445 ? C22 C25 O8 Co2 -170.1(3) . . . 3_445 ? O8 C25 O9 Co1 -10.0(6) . . . 3_445 ? C22 C25 O9 Co1 166.9(2) . . . 3_445 ? C32 C27 O10 C26 -166.9(3) . . . . ? C28 C27 O10 C26 12.0(5) . . . . ? C9 C26 O10 C27 165.8(3) . . . . ? O12 C33 O11 Co1 -2.9(5) . . . 8_455 ? C30 C33 O11 Co1 175.6(2) . . . 8_455 ? O11 C33 O12 Co2 3.0(6) . . . 8_455 ? C30 C33 O12 Co2 -175.6(2) . . . 8_455 ? # 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 0.820 -0.098 0.039 6830 1885 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.452 _refine_diff_density_min -0.282 _refine_diff_density_rms 0.048 _database_code_depnum_ccdc_archive 'CCDC 928863' ####################################################################### # # 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 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H34 N2 O12 Zn2' _chemical_formula_weight 925.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.763(3) _cell_length_b 21.535(2) _cell_length_c 26.471(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.687(2) _cell_angle_gamma 90.00 _cell_volume 13424(2) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3347 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 21.98 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.916 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3792 _exptl_absorpt_coefficient_mu 0.756 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8635 _exptl_absorpt_correction_T_max 0.8759 _exptl_absorpt_process_details SADABS;Bruker,2000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 32063 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0861 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 25.10 _reflns_number_total 11614 _reflns_number_gt 5294 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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. ; _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^)+(0.0982P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11614 _refine_ls_number_parameters 536 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1332 _refine_ls_R_factor_gt 0.0743 _refine_ls_wR_factor_ref 0.2146 _refine_ls_wR_factor_gt 0.1969 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3727(3) 0.1769(3) 0.4225(3) 0.0655(18) Uani 1 1 d . . . C2 C 0.3327(3) 0.1364(3) 0.3894(2) 0.0618(16) Uani 1 1 d . . . C3 C 0.3476(3) 0.0758(3) 0.3802(3) 0.081(2) Uani 1 1 d . . . H3 H 0.3832 0.0609 0.3938 0.097 Uiso 1 1 calc R . . C4 C 0.3103(3) 0.0379(3) 0.3513(3) 0.090(2) Uani 1 1 d . . . H4 H 0.3209 -0.0025 0.3445 0.108 Uiso 1 1 calc R . . C5 C 0.2567(3) 0.0591(3) 0.3321(3) 0.0758(19) Uani 1 1 d . . . C6 C 0.2419(3) 0.1176(3) 0.3428(3) 0.089(2) Uani 1 1 d . . . H6 H 0.2059 0.1321 0.3302 0.107 Uiso 1 1 calc R . . C7 C 0.2793(3) 0.1561(3) 0.3718(3) 0.081(2) Uani 1 1 d . . . H7 H 0.2680 0.1959 0.3796 0.098 Uiso 1 1 calc R . . C8 C 0.2346(3) -0.0248(3) 0.2765(3) 0.082 Uani 1 1 d . . . H8A H 0.2425 -0.0600 0.2992 0.099 Uiso 1 1 calc R . . H8B H 0.2692 -0.0139 0.2628 0.099 Uiso 1 1 calc R . . C9 C 0.1872(3) -0.0413(3) 0.2328(3) 0.0697(18) Uani 1 1 d . . . C10 C 0.2101(3) -0.0958(3) 0.2015(3) 0.080(2) Uani 1 1 d . . . H10A H 0.2180 -0.1322 0.2227 0.096 Uiso 1 1 calc R . . H10B H 0.1823 -0.1067 0.1725 0.096 Uiso 1 1 calc R . . C11 C 0.2875(3) -0.1103(3) 0.1550(3) 0.076(2) Uani 1 1 d . . . C12 C 0.3393(3) -0.0856(3) 0.1462(3) 0.090(2) Uani 1 1 d . . . H12 H 0.3516 -0.0480 0.1611 0.108 Uiso 1 1 calc R . . C13 C 0.3727(3) -0.1166(3) 0.1153(3) 0.079(2) Uani 1 1 d . . . H13 H 0.4074 -0.0999 0.1098 0.095 Uiso 1 1 calc R . . C14 C 0.3553(2) -0.1706(2) 0.0933(3) 0.0627(17) Uani 1 1 d . . . C15 C 0.3055(3) -0.1965(3) 0.1046(3) 0.076(2) Uani 1 1 d . . . H15 H 0.2945 -0.2352 0.0911 0.091 Uiso 1 1 calc R . . C16 C 0.2711(3) -0.1666(3) 0.1355(3) 0.078(2) Uani 1 1 d . . . H16 H 0.2376 -0.1849 0.1427 0.094 Uiso 1 1 calc R . . C17 C 0.3902(2) -0.2010(3) 0.0562(2) 0.0561(15) Uani 1 1 d . . . C18 C 0.1306(3) -0.0608(3) 0.2568(3) 0.085(2) Uani 1 1 d . . . H18A H 0.1186 -0.0272 0.2773 0.102 Uiso 1 1 calc R . . H18B H 0.1000 -0.0703 0.2299 0.102 Uiso 1 1 calc R . . C19 C 0.1008(3) -0.1322(4) 0.3142(3) 0.082(2) Uani 1 1 d . . . C20 C 0.1136(3) -0.1814(4) 0.3426(3) 0.105(3) Uani 1 1 d . . . H20 H 0.1485 -0.2007 0.3420 0.126 Uiso 1 1 calc R . . C21 C 0.0765(3) -0.2048(3) 0.3730(3) 0.091(2) Uani 1 1 d . . . H21 H 0.0871 -0.2387 0.3939 0.109 Uiso 1 1 calc R . . C22 C 0.0231(3) -0.1785(3) 0.3730(2) 0.0649(17) Uani 1 1 d . . . C23 C 0.0102(3) -0.1284(3) 0.3440(2) 0.0730(19) Uani 1 1 d . . . H23 H -0.0251 -0.1096 0.3440 0.088 Uiso 1 1 calc R . . C24 C 0.0490(3) -0.1031(3) 0.3130(2) 0.080(2) Uani 1 1 d . . . H24 H 0.0397 -0.0683 0.2927 0.097 Uiso 1 1 calc R . . C25 C -0.0151(3) -0.2029(3) 0.4079(3) 0.0687(18) Uani 1 1 d . . . C26 C 0.1722(3) 0.0151(3) 0.1974(3) 0.079 Uani 1 1 d . . . H26A H 0.1594 0.0493 0.2169 0.095 Uiso 1 1 calc R . . H26B H 0.2057 0.0286 0.1831 0.095 Uiso 1 1 calc R . . C27 C 0.1038(3) 0.0464(3) 0.1306(3) 0.078(2) Uani 1 1 d . . . C28 C 0.1230(3) 0.1055(3) 0.1313(3) 0.088(2) Uani 1 1 d . . . H28 H 0.1570 0.1167 0.1508 0.105 Uiso 1 1 calc R . . C29 C 0.0904(3) 0.1491(3) 0.1018(3) 0.090(2) Uani 1 1 d . . . H29 H 0.1030 0.1900 0.1019 0.109 Uiso 1 1 calc R . . C30 C 0.0403(3) 0.1339(3) 0.0725(2) 0.0666(17) Uani 1 1 d . . . C31 C 0.0240(3) 0.0740(3) 0.0720(3) 0.085(2) Uani 1 1 d . . . H31 H -0.0097 0.0627 0.0520 0.102 Uiso 1 1 calc R . . C32 C 0.0553(3) 0.0288(3) 0.0999(3) 0.096(2) Uani 1 1 d . . . H32 H 0.0438 -0.0125 0.0981 0.115 Uiso 1 1 calc R . . C33 C 0.0040(3) 0.1808(3) 0.0425(3) 0.0646(17) Uani 1 1 d . . . C34 C 0.2918(2) 0.3546(3) 0.4982(3) 0.086(2) Uani 1 1 d . . . H34 H 0.2895 0.3178 0.5162 0.103 Uiso 1 1 calc R . . C35 C 0.2501(3) 0.3977(3) 0.4992(3) 0.085(2) Uani 1 1 d . . . H35 H 0.2203 0.3903 0.5179 0.103 Uiso 1 1 calc R . . C36 C 0.2522(2) 0.4519(3) 0.4728(2) 0.0667(18) Uani 1 1 d . . . C37 C 0.2979(3) 0.4603(3) 0.4451(3) 0.0730(19) Uani 1 1 d . . . H37 H 0.3004 0.4962 0.4260 0.088 Uiso 1 1 calc R . . C38 C 0.3396(3) 0.4147(3) 0.4464(2) 0.0694(19) Uani 1 1 d . . . H38 H 0.3703 0.4209 0.4287 0.083 Uiso 1 1 calc R . . C39 C 0.2102(3) 0.5002(3) 0.4731(3) 0.083(2) Uani 1 1 d . . . H39 H 0.2157 0.5367 0.4557 0.099 Uiso 1 1 calc R . . C40 C 0.1657(3) 0.4966(3) 0.4956(3) 0.087(2) Uani 1 1 d . . . H40 H 0.1614 0.4604 0.5139 0.105 Uiso 1 1 calc R . . C41 C 0.1204(4) 0.5438(4) 0.4954(4) 0.131(4) Uani 1 1 d . . . C42 C 0.1314(4) 0.6034(4) 0.4791(4) 0.131(4) Uani 1 1 d . . . H42 H 0.1659 0.6122 0.4677 0.158 Uiso 1 1 calc R . . C43 C 0.0909(3) 0.6498(4) 0.4799(3) 0.121(3) Uani 1 1 d . . . H43 H 0.0982 0.6897 0.4690 0.145 Uiso 1 1 calc R . . C44 C 0.0283(3) 0.5771(4) 0.5132(3) 0.121(3) Uani 1 1 d . . . H44 H -0.0062 0.5682 0.5246 0.145 Uiso 1 1 calc R . . C45 C 0.06884(17) 0.5306(2) 0.51246(19) 0.121(3) Uani 1 1 d . . . H45 H 0.0615 0.4908 0.5233 0.145 Uiso 1 1 calc R . . N1 N 0.03932(17) 0.6366(2) 0.49691(19) 0.0786(17) Uani 1 1 d . . . N2 N 0.33611(18) 0.36294(19) 0.47222(17) 0.0516(12) Uani 1 1 d . . . O1 O 0.41876(18) 0.1554(2) 0.44312(18) 0.0825(14) Uani 1 1 d . . . O2 O 0.35691(17) 0.2318(2) 0.42819(17) 0.0762(13) Uani 1 1 d . . . O3 O 0.2158(2) 0.0252(2) 0.3028(2) 0.1014(16) Uani 1 1 d . . . O4 O 0.2590(2) -0.0738(2) 0.1853(2) 0.1055(17) Uani 1 1 d . . . O5 O 0.43562(16) -0.17552(19) 0.04981(17) 0.0772(13) Uani 1 1 d . . . O6 O 0.37150(17) -0.24906(19) 0.03463(16) 0.0743(13) Uani 1 1 d . . . O7 O 0.1441(2) -0.1114(2) 0.2860(2) 0.1002(16) Uani 1 1 d . . . O8 O -0.06110(17) -0.1749(2) 0.41273(17) 0.0781(13) Uani 1 1 d . . . O9 O 0.00021(18) -0.2516(2) 0.43197(18) 0.0857(14) Uani 1 1 d . . . O10 O 0.1304(2) -0.0008(2) 0.15902(19) 0.0889(14) Uani 1 1 d . . . O11 O 0.02256(18) 0.2348(2) 0.03913(17) 0.0820(13) Uani 1 1 d . . . O12 O -0.04245(18) 0.16207(19) 0.01956(18) 0.0787(13) Uani 1 1 d . . . Zn1 Zn 0.47908(2) 0.20098(3) 0.49331(3) 0.0573(2) Uani 1 1 d . . . Zn2 Zn 0.39624(2) 0.29741(3) 0.47211(3) 0.0535(2) 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 0.059(4) 0.060(4) 0.084(5) -0.003(4) 0.030(4) 0.005(3) C2 0.055(4) 0.059(4) 0.072(4) -0.012(3) 0.010(3) -0.001(3) C3 0.057(4) 0.084(5) 0.098(5) -0.008(4) -0.001(4) 0.012(4) C4 0.076(5) 0.058(4) 0.134(7) -0.038(4) 0.005(5) 0.006(4) C5 0.060(4) 0.083(5) 0.084(5) -0.026(4) 0.005(4) -0.007(4) C6 0.066(5) 0.085(5) 0.117(6) -0.023(5) 0.014(4) 0.006(4) C7 0.068(5) 0.056(4) 0.118(6) -0.019(4) 0.008(4) 0.015(4) C8 0.078 0.083 0.084 0.002 0.002 0.001 C9 0.065(4) 0.051(4) 0.092(5) 0.020(4) 0.009(4) -0.035(3) C10 0.070(5) 0.060(4) 0.109(6) 0.022(4) 0.008(4) -0.022(4) C11 0.081(5) 0.065(4) 0.090(5) -0.014(4) 0.046(4) 0.004(4) C12 0.077(5) 0.076(5) 0.125(7) -0.039(4) 0.046(5) -0.015(4) C13 0.061(4) 0.067(4) 0.114(6) -0.029(4) 0.028(4) -0.012(3) C14 0.059(4) 0.038(3) 0.098(5) -0.015(3) 0.035(4) -0.010(3) C15 0.064(4) 0.048(4) 0.123(6) -0.022(4) 0.041(4) -0.017(3) C16 0.058(4) 0.075(5) 0.110(6) -0.005(4) 0.042(4) -0.001(4) C17 0.040(3) 0.050(3) 0.079(4) -0.007(3) 0.009(3) -0.014(3) C18 0.077(5) 0.061(4) 0.115(6) 0.020(4) 0.008(4) -0.030(4) C19 0.049(4) 0.110(6) 0.095(6) -0.011(5) 0.039(4) -0.006(4) C20 0.087(6) 0.111(7) 0.126(7) 0.035(6) 0.048(5) 0.030(5) C21 0.062(4) 0.104(6) 0.117(6) 0.030(5) 0.050(4) 0.020(4) C22 0.059(4) 0.083(5) 0.058(4) 0.012(4) 0.028(3) 0.018(3) C23 0.049(4) 0.094(5) 0.077(5) 0.016(4) 0.010(4) 0.013(4) C24 0.082(5) 0.086(5) 0.074(5) 0.029(4) 0.011(4) -0.009(4) C25 0.054(4) 0.060(4) 0.100(5) 0.003(4) 0.041(4) 0.007(3) C26 0.064 0.086 0.087 0.002 0.009 0.001 C27 0.092(6) 0.059(5) 0.089(6) 0.014(4) 0.039(5) 0.021(4) C28 0.073(5) 0.077(5) 0.106(6) 0.005(5) -0.013(4) 0.011(4) C29 0.074(5) 0.061(4) 0.131(7) -0.014(5) -0.001(5) -0.010(4) C30 0.068(4) 0.061(4) 0.074(5) -0.002(4) 0.019(4) -0.009(4) C31 0.064(4) 0.066(5) 0.124(6) 0.015(5) 0.013(4) -0.009(4) C32 0.075(5) 0.062(5) 0.147(7) 0.014(5) 0.003(5) 0.000(4) C33 0.055(4) 0.061(4) 0.078(5) -0.002(4) 0.011(4) 0.005(4) C34 0.062(4) 0.058(4) 0.148(7) 0.045(4) 0.058(4) 0.037(3) C35 0.073(4) 0.072(4) 0.127(6) 0.039(4) 0.067(4) 0.039(4) C36 0.056(4) 0.062(4) 0.084(5) 0.010(3) 0.018(3) 0.045(3) C37 0.067(4) 0.054(4) 0.104(5) 0.028(4) 0.032(4) 0.037(3) C38 0.069(4) 0.052(4) 0.095(5) 0.013(4) 0.039(4) 0.030(3) C39 0.078(5) 0.080(5) 0.096(5) 0.017(4) 0.033(4) 0.046(4) C40 0.084(5) 0.065(4) 0.116(6) 0.020(4) 0.028(5) 0.050(4) C41 0.106(7) 0.087(6) 0.217(10) 0.042(6) 0.083(7) 0.057(5) C42 0.106(7) 0.087(6) 0.217(10) 0.042(6) 0.083(7) 0.057(5) C43 0.106(6) 0.097(6) 0.177(9) 0.046(6) 0.087(6) 0.059(5) C44 0.106(6) 0.097(6) 0.177(9) 0.046(6) 0.087(6) 0.059(5) C45 0.106(6) 0.097(6) 0.177(9) 0.046(6) 0.087(6) 0.059(5) N1 0.047(3) 0.060(3) 0.136(5) -0.004(3) 0.036(3) 0.022(3) N2 0.043(3) 0.038(3) 0.074(3) 0.015(2) 0.011(2) 0.018(2) O1 0.060(3) 0.073(3) 0.111(4) -0.013(3) -0.001(3) 0.006(2) O2 0.055(3) 0.061(3) 0.113(4) -0.015(3) 0.014(2) -0.003(2) O3 0.077(3) 0.096(4) 0.135(4) -0.049(3) 0.027(3) -0.005(3) O4 0.089(4) 0.096(4) 0.142(5) -0.014(3) 0.055(4) -0.013(3) O5 0.051(3) 0.082(3) 0.106(4) -0.024(3) 0.038(2) -0.027(2) O6 0.063(3) 0.066(3) 0.102(4) -0.017(3) 0.040(2) -0.014(2) O7 0.080(3) 0.112(4) 0.117(4) 0.028(3) 0.042(3) 0.026(3) O8 0.053(3) 0.078(3) 0.110(4) 0.009(3) 0.034(3) 0.012(2) O9 0.078(3) 0.067(3) 0.119(4) 0.020(3) 0.039(3) 0.018(3) O10 0.090(3) 0.078(3) 0.098(4) -0.013(3) 0.009(3) 0.006(3) O11 0.069(3) 0.067(3) 0.110(4) 0.006(3) 0.012(3) 0.002(2) O12 0.059(3) 0.065(3) 0.112(4) 0.015(3) 0.011(3) -0.002(2) Zn1 0.0384(4) 0.0476(4) 0.0892(6) 0.0037(4) 0.0205(3) 0.0179(3) Zn2 0.0366(4) 0.0428(4) 0.0843(5) 0.0014(4) 0.0204(3) 0.0144(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.244(7) . ? C1 O2 1.255(7) . ? C1 C2 1.487(8) . ? C2 C7 1.361(8) . ? C2 C3 1.381(8) . ? C3 C4 1.363(8) . ? C3 H3 0.9300 . ? C4 C5 1.384(8) . ? C4 H4 0.9300 . ? C5 C6 1.346(9) . ? C5 O3 1.371(7) . ? C6 C7 1.373(8) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 O3 1.386(7) . ? C8 C9 1.544(8) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C26 1.547(8) . ? C9 C10 1.575(9) . ? C9 C18 1.617(8) . ? C10 O4 1.377(7) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C16 1.354(8) . ? C11 O4 1.365(7) . ? C11 C12 1.389(8) . ? C12 C13 1.385(8) . ? C12 H12 0.9300 . ? C13 C14 1.340(7) . ? C13 H13 0.9300 . ? C14 C15 1.377(7) . ? C14 C17 1.517(8) . ? C15 C16 1.389(8) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 O6 1.236(6) . ? C17 O5 1.242(6) . ? C18 O7 1.348(7) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.311(9) . ? C19 C24 1.379(9) . ? C19 O7 1.421(7) . ? C20 C21 1.369(9) . ? C20 H20 0.9300 . ? C21 C22 1.390(8) . ? C21 H21 0.9300 . ? C22 C23 1.337(8) . ? C22 C25 1.477(8) . ? C23 C24 1.421(8) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 O9 1.255(7) . ? C25 O8 1.269(6) . ? C26 O10 1.367(7) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.353(9) . ? C27 O10 1.369(7) . ? C27 C32 1.371(9) . ? C28 C29 1.388(9) . ? C28 H28 0.9300 . ? C29 C30 1.373(8) . ? C29 H29 0.9300 . ? C30 C31 1.345(8) . ? C30 C33 1.486(8) . ? C31 C32 1.379(9) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 O11 1.252(7) . ? C33 O12 1.254(7) . ? C34 N2 1.345(7) . ? C34 C35 1.359(7) . ? C34 H34 0.9300 . ? C35 C36 1.365(8) . ? C35 H35 0.9300 . ? C36 C37 1.401(8) . ? C36 C39 1.442(7) . ? C37 C38 1.391(7) . ? C37 H37 0.9300 . ? C38 N2 1.316(7) . ? C38 H38 0.9300 . ? C39 C40 1.283(9) . ? C39 H39 0.9300 . ? C40 C41 1.481(8) . ? C40 H40 0.9300 . ? C41 C45 1.390(9) . ? C41 C42 1.390(10) . ? C42 C43 1.390(9) . ? C42 H42 0.9300 . ? C43 N1 1.390(8) . ? C43 H43 0.9300 . ? C44 C45 1.390(7) . ? C44 N1 1.390(8) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? N1 Zn1 1.985(4) 3_455 ? N2 Zn2 2.008(4) . ? O1 Zn1 2.067(4) . ? O2 Zn2 1.982(4) . ? O5 Zn1 2.004(4) 6 ? O6 Zn2 2.104(4) 6 ? O8 Zn2 2.069(4) 3_445 ? O9 Zn1 2.037(5) 3_445 ? O11 Zn1 2.028(4) 8_455 ? O12 Zn2 1.993(4) 8_455 ? Zn1 N1 1.985(4) 3_545 ? Zn1 O5 2.004(4) 6_556 ? Zn1 O11 2.028(4) 8_556 ? Zn1 O9 2.037(5) 3 ? Zn1 Zn2 2.8648(8) . ? Zn2 O12 1.993(4) 8_556 ? Zn2 O8 2.069(4) 3 ? Zn2 O6 2.104(4) 6_556 ? 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 123.9(7) . . ? O1 C1 C2 119.6(6) . . ? O2 C1 C2 116.4(6) . . ? C7 C2 C3 118.9(6) . . ? C7 C2 C1 120.8(6) . . ? C3 C2 C1 120.0(6) . . ? C4 C3 C2 120.1(6) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 120.5(6) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 O3 115.6(7) . . ? C6 C5 C4 118.9(7) . . ? O3 C5 C4 125.4(6) . . ? C5 C6 C7 121.0(7) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C2 C7 C6 120.5(6) . . ? C2 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? O3 C8 C9 107.6(6) . . ? O3 C8 H8A 110.2 . . ? C9 C8 H8A 110.2 . . ? O3 C8 H8B 110.2 . . ? C9 C8 H8B 110.2 . . ? H8A C8 H8B 108.5 . . ? C8 C9 C26 111.0(5) . . ? C8 C9 C10 107.4(5) . . ? C26 C9 C10 109.5(5) . . ? C8 C9 C18 109.1(6) . . ? C26 C9 C18 107.8(5) . . ? C10 C9 C18 112.1(5) . . ? O4 C10 C9 105.9(5) . . ? O4 C10 H10A 110.6 . . ? C9 C10 H10A 110.6 . . ? O4 C10 H10B 110.6 . . ? C9 C10 H10B 110.6 . . ? H10A C10 H10B 108.7 . . ? C16 C11 O4 126.8(6) . . ? C16 C11 C12 119.8(6) . . ? O4 C11 C12 113.4(6) . . ? C13 C12 C11 120.2(6) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C14 C13 C12 120.6(6) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C15 118.7(6) . . ? C13 C14 C17 119.5(5) . . ? C15 C14 C17 121.7(5) . . ? C14 C15 C16 122.1(6) . . ? C14 C15 H15 119.0 . . ? C16 C15 H15 119.0 . . ? C11 C16 C15 118.5(6) . . ? C11 C16 H16 120.8 . . ? C15 C16 H16 120.8 . . ? O6 C17 O5 124.9(6) . . ? O6 C17 C14 117.8(5) . . ? O5 C17 C14 117.2(5) . . ? O7 C18 C9 106.8(5) . . ? O7 C18 H18A 110.4 . . ? C9 C18 H18A 110.4 . . ? O7 C18 H18B 110.4 . . ? C9 C18 H18B 110.4 . . ? H18A C18 H18B 108.6 . . ? C20 C19 C24 121.2(7) . . ? C20 C19 O7 115.3(7) . . ? C24 C19 O7 123.5(8) . . ? C19 C20 C21 121.1(7) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C20 C21 C22 120.7(7) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C23 C22 C21 118.0(6) . . ? C23 C22 C25 122.3(6) . . ? C21 C22 C25 119.5(6) . . ? C22 C23 C24 121.6(6) . . ? C22 C23 H23 119.2 . . ? C24 C23 H23 119.2 . . ? C19 C24 C23 117.4(6) . . ? C19 C24 H24 121.3 . . ? C23 C24 H24 121.3 . . ? O9 C25 O8 122.8(6) . . ? O9 C25 C22 117.0(5) . . ? O8 C25 C22 120.2(6) . . ? O10 C26 C9 109.8(6) . . ? O10 C26 H26A 109.7 . . ? C9 C26 H26A 109.7 . . ? O10 C26 H26B 109.7 . . ? C9 C26 H26B 109.7 . . ? H26A C26 H26B 108.2 . . ? C28 C27 O10 124.2(8) . . ? C28 C27 C32 121.6(7) . . ? O10 C27 C32 114.2(7) . . ? C27 C28 C29 117.8(7) . . ? C27 C28 H28 121.1 . . ? C29 C28 H28 121.1 . . ? C30 C29 C28 122.3(7) . . ? C30 C29 H29 118.9 . . ? C28 C29 H29 118.9 . . ? C31 C30 C29 117.5(7) . . ? C31 C30 C33 120.0(6) . . ? C29 C30 C33 122.5(6) . . ? C30 C31 C32 122.5(7) . . ? C30 C31 H31 118.8 . . ? C32 C31 H31 118.8 . . ? C27 C32 C31 118.3(7) . . ? C27 C32 H32 120.9 . . ? C31 C32 H32 120.9 . . ? O11 C33 O12 124.1(6) . . ? O11 C33 C30 119.1(6) . . ? O12 C33 C30 116.7(6) . . ? N2 C34 C35 122.7(6) . . ? N2 C34 H34 118.6 . . ? C35 C34 H34 118.6 . . ? C34 C35 C36 119.9(6) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C35 C36 C37 117.5(5) . . ? C35 C36 C39 122.8(6) . . ? C37 C36 C39 119.7(6) . . ? C38 C37 C36 119.7(5) . . ? C38 C37 H37 120.2 . . ? C36 C37 H37 120.2 . . ? N2 C38 C37 121.1(6) . . ? N2 C38 H38 119.4 . . ? C37 C38 H38 119.4 . . ? C40 C39 C36 125.0(7) . . ? C40 C39 H39 117.5 . . ? C36 C39 H39 117.5 . . ? C39 C40 C41 126.9(7) . . ? C39 C40 H40 116.5 . . ? C41 C40 H40 116.5 . . ? C45 C41 C42 120.0(6) . . ? C45 C41 C40 122.0(7) . . ? C42 C41 C40 117.9(7) . . ? C43 C42 C41 120.0(8) . . ? C43 C42 H42 120.0 . . ? C41 C42 H42 120.0 . . ? N1 C43 C42 120.0(7) . . ? N1 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C45 C44 N1 120.0(6) . . ? C45 C44 H44 120.0 . . ? N1 C44 H44 120.0 . . ? C44 C45 C41 120.0(5) . . ? C44 C45 H45 120.0 . . ? C41 C45 H45 120.0 . . ? C43 N1 C44 120.0(5) . . ? C43 N1 Zn1 120.2(4) . 3_455 ? C44 N1 Zn1 119.7(4) . 3_455 ? C38 N2 C34 119.1(5) . . ? C38 N2 Zn2 120.1(4) . . ? C34 N2 Zn2 120.9(4) . . ? C1 O1 Zn1 126.7(4) . . ? C1 O2 Zn2 128.0(5) . . ? C5 O3 C8 116.5(5) . . ? C11 O4 C10 119.4(6) . . ? C17 O5 Zn1 121.6(4) . 6 ? C17 O6 Zn2 131.0(4) . 6 ? C18 O7 C19 115.0(6) . . ? C25 O8 Zn2 117.1(4) . 3_445 ? C25 O9 Zn1 137.5(4) . 3_445 ? C26 O10 C27 117.3(6) . . ? C33 O11 Zn1 121.3(4) . 8_455 ? C33 O12 Zn2 133.4(4) . 8_455 ? N1 Zn1 O5 102.33(18) 3_545 6_556 ? N1 Zn1 O11 98.07(19) 3_545 8_556 ? O5 Zn1 O11 90.71(19) 6_556 8_556 ? N1 Zn1 O9 97.76(19) 3_545 3 ? O5 Zn1 O9 159.79(16) 6_556 3 ? O11 Zn1 O9 88.56(19) 8_556 3 ? N1 Zn1 O1 97.66(18) 3_545 . ? O5 Zn1 O1 88.14(19) 6_556 . ? O11 Zn1 O1 164.10(18) 8_556 . ? O9 Zn1 O1 87.09(19) 3 . ? N1 Zn1 Zn2 170.91(15) 3_545 . ? O5 Zn1 Zn2 86.29(11) 6_556 . ? O11 Zn1 Zn2 84.54(13) 8_556 . ? O9 Zn1 Zn2 73.54(12) 3 . ? O1 Zn1 Zn2 79.56(12) . . ? O2 Zn2 O12 158.31(18) . 8_556 ? O2 Zn2 N2 102.81(18) . . ? O12 Zn2 N2 98.73(18) 8_556 . ? O2 Zn2 O8 90.01(18) . 3 ? O12 Zn2 O8 87.79(18) 8_556 3 ? N2 Zn2 O8 102.69(17) . 3 ? O2 Zn2 O6 87.10(18) . 6_556 ? O12 Zn2 O6 88.77(18) 8_556 6_556 ? N2 Zn2 O6 94.18(17) . 6_556 ? O8 Zn2 O6 163.11(16) 3 6_556 ? O2 Zn2 Zn1 81.73(12) . . ? O12 Zn2 Zn1 76.63(12) 8_556 . ? N2 Zn2 Zn1 168.34(14) . . ? O8 Zn2 Zn1 87.93(11) 3 . ? O6 Zn2 Zn1 75.18(11) 6_556 . ? 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 C7 171.4(6) . . . . ? O2 C1 C2 C7 -8.0(9) . . . . ? O1 C1 C2 C3 -2.2(9) . . . . ? O2 C1 C2 C3 178.4(6) . . . . ? C7 C2 C3 C4 4.0(11) . . . . ? C1 C2 C3 C4 177.7(6) . . . . ? C2 C3 C4 C5 -1.7(12) . . . . ? C3 C4 C5 C6 -0.6(12) . . . . ? C3 C4 C5 O3 -179.9(7) . . . . ? O3 C5 C6 C7 180.0(6) . . . . ? C4 C5 C6 C7 0.5(12) . . . . ? C3 C2 C7 C6 -4.0(11) . . . . ? C1 C2 C7 C6 -177.7(6) . . . . ? C5 C6 C7 C2 1.8(12) . . . . ? O3 C8 C9 C26 57.5(7) . . . . ? O3 C8 C9 C10 177.1(5) . . . . ? O3 C8 C9 C18 -61.1(7) . . . . ? C8 C9 C10 O4 -57.7(7) . . . . ? C26 C9 C10 O4 62.9(7) . . . . ? C18 C9 C10 O4 -177.5(5) . . . . ? C16 C11 C12 C13 3.5(12) . . . . ? O4 C11 C12 C13 -178.7(7) . . . . ? C11 C12 C13 C14 0.5(12) . . . . ? C12 C13 C14 C15 -4.2(11) . . . . ? C12 C13 C14 C17 175.0(6) . . . . ? C13 C14 C15 C16 4.0(11) . . . . ? C17 C14 C15 C16 -175.1(6) . . . . ? O4 C11 C16 C15 178.9(7) . . . . ? C12 C11 C16 C15 -3.7(11) . . . . ? C14 C15 C16 C11 -0.1(11) . . . . ? C13 C14 C17 O6 -176.4(6) . . . . ? C15 C14 C17 O6 2.7(9) . . . . ? C13 C14 C17 O5 3.5(9) . . . . ? C15 C14 C17 O5 -177.4(6) . . . . ? C8 C9 C18 O7 -61.6(7) . . . . ? C26 C9 C18 O7 177.8(5) . . . . ? C10 C9 C18 O7 57.2(7) . . . . ? C24 C19 C20 C21 -1.6(13) . . . . ? O7 C19 C20 C21 177.6(7) . . . . ? C19 C20 C21 C22 2.8(13) . . . . ? C20 C21 C22 C23 -2.6(11) . . . . ? C20 C21 C22 C25 -177.2(7) . . . . ? C21 C22 C23 C24 1.4(10) . . . . ? C25 C22 C23 C24 175.9(6) . . . . ? C20 C19 C24 C23 0.4(11) . . . . ? O7 C19 C24 C23 -178.8(6) . . . . ? C22 C23 C24 C19 -0.3(10) . . . . ? C23 C22 C25 O9 177.3(6) . . . . ? C21 C22 C25 O9 -8.2(10) . . . . ? C23 C22 C25 O8 -2.7(10) . . . . ? C21 C22 C25 O8 171.7(7) . . . . ? C8 C9 C26 O10 179.7(5) . . . . ? C10 C9 C26 O10 61.4(7) . . . . ? C18 C9 C26 O10 -60.8(7) . . . . ? O10 C27 C28 C29 -177.7(6) . . . . ? C32 C27 C28 C29 3.3(11) . . . . ? C27 C28 C29 C30 -0.2(11) . . . . ? C28 C29 C30 C31 -1.9(11) . . . . ? C28 C29 C30 C33 177.5(6) . . . . ? C29 C30 C31 C32 0.8(11) . . . . ? C33 C30 C31 C32 -178.5(7) . . . . ? C28 C27 C32 C31 -4.3(11) . . . . ? O10 C27 C32 C31 176.6(6) . . . . ? C30 C31 C32 C27 2.2(12) . . . . ? C31 C30 C33 O11 -172.6(6) . . . . ? C29 C30 C33 O11 8.1(10) . . . . ? C31 C30 C33 O12 3.4(9) . . . . ? C29 C30 C33 O12 -175.9(6) . . . . ? N2 C34 C35 C36 0.5(12) . . . . ? C34 C35 C36 C37 0.4(11) . . . . ? C34 C35 C36 C39 -178.6(7) . . . . ? C35 C36 C37 C38 -1.5(10) . . . . ? C39 C36 C37 C38 177.6(6) . . . . ? C36 C37 C38 N2 1.7(10) . . . . ? C35 C36 C39 C40 -3.5(12) . . . . ? C37 C36 C39 C40 177.4(7) . . . . ? C36 C39 C40 C41 -177.6(8) . . . . ? C39 C40 C41 C45 167.1(8) . . . . ? C39 C40 C41 C42 -15.0(15) . . . . ? C45 C41 C42 C43 0.0(16) . . . . ? C40 C41 C42 C43 -177.9(9) . . . . ? C41 C42 C43 N1 0.0(15) . . . . ? N1 C44 C45 C41 0.0(13) . . . . ? C42 C41 C45 C44 0.0(14) . . . . ? C40 C41 C45 C44 177.8(8) . . . . ? C42 C43 N1 C44 0.0(13) . . . . ? C42 C43 N1 Zn1 -175.5(7) . . . 3_455 ? C45 C44 N1 C43 0.0(13) . . . . ? C45 C44 N1 Zn1 175.5(5) . . . 3_455 ? C37 C38 N2 C34 -0.7(10) . . . . ? C37 C38 N2 Zn2 178.8(5) . . . . ? C35 C34 N2 C38 -0.4(11) . . . . ? C35 C34 N2 Zn2 -179.9(6) . . . . ? O2 C1 O1 Zn1 2.8(10) . . . . ? C2 C1 O1 Zn1 -176.7(4) . . . . ? O1 C1 O2 Zn2 -3.2(9) . . . . ? C2 C1 O2 Zn2 176.2(4) . . . . ? C6 C5 O3 C8 157.9(7) . . . . ? C4 C5 O3 C8 -22.8(11) . . . . ? C9 C8 O3 C5 -160.2(6) . . . . ? C16 C11 O4 C10 4.4(11) . . . . ? C12 C11 O4 C10 -173.2(6) . . . . ? C9 C10 O4 C11 -177.4(6) . . . . ? O6 C17 O5 Zn1 11.1(9) . . . 6 ? C14 C17 O5 Zn1 -168.7(4) . . . 6 ? O5 C17 O6 Zn2 -12.4(10) . . . 6 ? C14 C17 O6 Zn2 167.4(4) . . . 6 ? C9 C18 O7 C19 174.5(5) . . . . ? C20 C19 O7 C18 179.9(7) . . . . ? C24 C19 O7 C18 -0.9(10) . . . . ? O9 C25 O8 Zn2 11.4(9) . . . 3_445 ? C22 C25 O8 Zn2 -168.6(5) . . . 3_445 ? O8 C25 O9 Zn1 -15.2(11) . . . 3_445 ? C22 C25 O9 Zn1 164.7(5) . . . 3_445 ? C9 C26 O10 C27 166.7(5) . . . . ? C28 C27 O10 C26 13.4(10) . . . . ? C32 C27 O10 C26 -167.5(6) . . . . ? O12 C33 O11 Zn1 -1.8(9) . . . 8_455 ? C30 C33 O11 Zn1 173.9(4) . . . 8_455 ? O11 C33 O12 Zn2 -0.2(10) . . . 8_455 ? C30 C33 O12 Zn2 -176.0(4) . . . 8_455 ? C1 O1 Zn1 N1 -172.3(5) . . . 3_545 ? C1 O1 Zn1 O5 85.5(5) . . . 6_556 ? C1 O1 Zn1 O11 -0.6(11) . . . 8_556 ? C1 O1 Zn1 O9 -74.9(5) . . . 3 ? C1 O1 Zn1 Zn2 -1.1(5) . . . . ? C1 O2 Zn2 O12 5.7(9) . . . 8_556 ? C1 O2 Zn2 N2 -167.3(5) . . . . ? C1 O2 Zn2 O8 89.7(5) . . . 3 ? C1 O2 Zn2 O6 -73.7(5) . . . 6_556 ? C1 O2 Zn2 Zn1 1.8(5) . . . . ? C38 N2 Zn2 O2 -106.9(5) . . . . ? C34 N2 Zn2 O2 72.7(5) . . . . ? C38 N2 Zn2 O12 75.8(5) . . . 8_556 ? C34 N2 Zn2 O12 -104.7(5) . . . 8_556 ? C38 N2 Zn2 O8 -13.9(5) . . . 3 ? C34 N2 Zn2 O8 165.6(5) . . . 3 ? C38 N2 Zn2 O6 165.2(5) . . . 6_556 ? C34 N2 Zn2 O6 -15.3(5) . . . 6_556 ? C38 N2 Zn2 Zn1 141.3(5) . . . . ? C34 N2 Zn2 Zn1 -39.2(10) . . . . ? N1 Zn1 Zn2 O2 72.7(9) 3_545 . . . ? O5 Zn1 Zn2 O2 -89.07(19) 6_556 . . . ? O11 Zn1 Zn2 O2 179.87(18) 8_556 . . . ? O9 Zn1 Zn2 O2 89.76(19) 3 . . . ? O1 Zn1 Zn2 O2 -0.27(19) . . . . ? N1 Zn1 Zn2 O12 -105.9(9) 3_545 . . 8_556 ? O5 Zn1 Zn2 O12 92.40(19) 6_556 . . 8_556 ? O11 Zn1 Zn2 O12 1.34(19) 8_556 . . 8_556 ? O9 Zn1 Zn2 O12 -88.8(2) 3 . . 8_556 ? O1 Zn1 Zn2 O12 -178.80(19) . . . 8_556 ? N1 Zn1 Zn2 N2 -173.5(11) 3_545 . . . ? O5 Zn1 Zn2 N2 24.8(7) 6_556 . . . ? O11 Zn1 Zn2 N2 -66.3(7) 8_556 . . . ? O9 Zn1 Zn2 N2 -156.4(7) 3 . . . ? O1 Zn1 Zn2 N2 113.6(7) . . . . ? N1 Zn1 Zn2 O8 -17.6(9) 3_545 . . 3 ? O5 Zn1 Zn2 O8 -179.37(18) 6_556 . . 3 ? O11 Zn1 Zn2 O8 89.56(18) 8_556 . . 3 ? O9 Zn1 Zn2 O8 -0.55(18) 3 . . 3 ? O1 Zn1 Zn2 O8 -90.58(19) . . . 3 ? N1 Zn1 Zn2 O6 161.8(9) 3_545 . . 6_556 ? O5 Zn1 Zn2 O6 0.11(18) 6_556 . . 6_556 ? O11 Zn1 Zn2 O6 -90.96(18) 8_556 . . 6_556 ? O9 Zn1 Zn2 O6 178.94(18) 3 . . 6_556 ? O1 Zn1 Zn2 O6 88.90(18) . . . 6_556 ? # 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 0.821 -0.098 0.039 6815 1810 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.730 _refine_diff_density_min -0.958 _refine_diff_density_rms 0.082 _database_code_depnum_ccdc_archive 'CCDC 928864' ####################################################################### # # 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 'C33 H26.50 Cd O12.25' _chemical_formula_weight 731.44 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.390(2) _cell_length_b 19.0868(16) _cell_length_c 27.639(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.4780(10) _cell_angle_gamma 90.00 _cell_volume 13858.0(19) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5741 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 19.86 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.701 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2964 _exptl_absorpt_coefficient_mu 0.345 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9311 _exptl_absorpt_correction_T_max 0.9374 _exptl_absorpt_process_details SADABS;Bruker,2000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 41663 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_sigmaI/netI 0.0743 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 26.02 _reflns_number_total 13648 _reflns_number_gt 5654 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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. ; _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^)+(0.1006P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13648 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1195 _refine_ls_R_factor_gt 0.0696 _refine_ls_wR_factor_ref 0.2228 _refine_ls_wR_factor_gt 0.2096 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.050 _refine_ls_shift/su_mean 0.003 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 0.4153(3) 0.7578(3) 1.1038(2) 0.1104(18) Uani 1 1 d . . . C2 C 0.4327(2) 0.7766(3) 1.0565(2) 0.1049(16) Uani 1 1 d . . . C3 C 0.4817(2) 0.7924(3) 1.0512(2) 0.1082(17) Uani 1 1 d . . . H3 H 0.5047 0.7926 1.0789 0.130 Uiso 1 1 calc R . . C4 C 0.4999(2) 0.8085(3) 1.0071(2) 0.1131(18) Uani 1 1 d . . . H4 H 0.5340 0.8190 1.0052 0.136 Uiso 1 1 calc R . . C5 C 0.4653(3) 0.8084(3) 0.9660(2) 0.1146(18) Uani 1 1 d . . . C6 C 0.4136(2) 0.7952(4) 0.9700(2) 0.136(2) Uani 1 1 d . . . H6 H 0.3900 0.7974 0.9427 0.163 Uiso 1 1 calc R . . C7 C 0.3982(3) 0.7787(3) 1.0152(3) 0.124(2) Uani 1 1 d . . . H7 H 0.3640 0.7689 1.0180 0.149 Uiso 1 1 calc R . . C8 C 0.52844(19) 0.8332(3) 0.91095(18) 0.1009(15) Uani 1 1 d . . . H8A H 0.5506 0.7994 0.9286 0.121 Uiso 1 1 calc R . . H8B H 0.5385 0.8798 0.9219 0.121 Uiso 1 1 calc R . . C9 C 0.5318(2) 0.8262(3) 0.85703(18) 0.0946(14) Uani 1 1 d . . . C10 C 0.4937(2) 0.8733(3) 0.82889(18) 0.1018(15) Uani 1 1 d . . . H10A H 0.4967 0.8690 0.7943 0.122 Uiso 1 1 calc R . . H10B H 0.4594 0.8603 0.8351 0.122 Uiso 1 1 calc R . . C11 C 0.4783(2) 0.9974(3) 0.8200(2) 0.0996(15) Uani 1 1 d . . . C12 C 0.4379(2) 0.9878(3) 0.7836(2) 0.1052(16) Uani 1 1 d . . . H12 H 0.4258 0.9430 0.7759 0.126 Uiso 1 1 calc R . . C13 C 0.4170(2) 1.0440(3) 0.7601(2) 0.1097(16) Uani 1 1 d . . . H13 H 0.3917 1.0375 0.7348 0.132 Uiso 1 1 calc R . . C14 C 0.4327(2) 1.1123(3) 0.7731(2) 0.0982(15) Uani 1 1 d . . . C15 C 0.4717(2) 1.1209(3) 0.8094(2) 0.1057(16) Uani 1 1 d . . . H15 H 0.4831 1.1657 0.8181 0.127 Uiso 1 1 calc R . . C16 C 0.4939(2) 1.0636(3) 0.8326(2) 0.1072(16) Uani 1 1 d . . . H16 H 0.5199 1.0699 0.8574 0.129 Uiso 1 1 calc R . . C17 C 0.4104(3) 1.1744(4) 0.7442(2) 0.1058(17) Uani 1 1 d . . . C18 C 0.5192(2) 0.7511(3) 0.8408(2) 0.1133(17) Uani 1 1 d . . . H18A H 0.4851 0.7388 0.8482 0.136 Uiso 1 1 calc R . . H18B H 0.5209 0.7464 0.8061 0.136 Uiso 1 1 calc R . . C19 C 0.5598(3) 0.6387(4) 0.8530(3) 0.133(2) Uani 1 1 d . . . C20 C 0.5293(3) 0.6042(4) 0.8199(3) 0.153(3) Uani 1 1 d . . . H20 H 0.5012 0.6258 0.8034 0.183 Uiso 1 1 calc R . . C21 C 0.5414(4) 0.5336(4) 0.8108(3) 0.154(3) Uani 1 1 d . . . H21 H 0.5202 0.5087 0.7881 0.185 Uiso 1 1 calc R . . C22 C 0.5822(3) 0.5005(4) 0.8334(3) 0.132(2) Uani 1 1 d . . . C23 C 0.6129(3) 0.5343(4) 0.8665(3) 0.133(2) Uani 1 1 d . . . H23 H 0.6411 0.5121 0.8826 0.159 Uiso 1 1 calc R . . C24 C 0.6014(3) 0.6060(4) 0.8770(3) 0.158(3) Uani 1 1 d . . . H24 H 0.6223 0.6305 0.9001 0.190 Uiso 1 1 calc R . . C25 C 0.5910(4) 0.4269(5) 0.8195(3) 0.142(3) Uani 1 1 d . . . C26 C 0.5859(2) 0.8455(3) 0.84735(18) 0.1112(18) Uani 1 1 d . . . H26A H 0.5925 0.8946 0.8543 0.133 Uiso 1 1 calc R . . H26B H 0.6104 0.8175 0.8674 0.133 Uiso 1 1 calc R . . C27 C 0.6383(3) 0.8276(4) 0.7812(3) 0.126(2) Uani 1 1 d . . . C28 C 0.6389(3) 0.7969(4) 0.7345(2) 0.149(3) Uani 1 1 d . . . H28 H 0.6089 0.7809 0.7177 0.179 Uiso 1 1 calc R . . C29 C 0.6846(3) 0.7914(4) 0.7146(3) 0.155(3) Uani 1 1 d . . . H29 H 0.6861 0.7720 0.6839 0.186 Uiso 1 1 calc R . . C30 C 0.7284(3) 0.8150(4) 0.7412(3) 0.142(3) Uani 1 1 d . . . C31 C 0.7284(3) 0.8441(4) 0.7887(3) 0.150(3) Uani 1 1 d . . . H31 H 0.7582 0.8583 0.8067 0.180 Uiso 1 1 calc R . . C32 C 0.6795(3) 0.8500(4) 0.8072(3) 0.142(2) Uani 1 1 d . . . H32 H 0.6770 0.8697 0.8376 0.170 Uiso 1 1 calc R . . C33 C 0.7818(3) 0.8057(4) 0.7221(3) 0.132(2) Uani 1 1 d . . . Cd1 Cd 0.375437(15) 0.71329(2) 1.189039(14) 0.0981(2) Uani 1 1 d . . . O1 O 0.36804(18) 0.7534(3) 1.10781(14) 0.1285(13) Uani 1 1 d . . . O2 O 0.44806(19) 0.7442(2) 1.13869(16) 0.1242(13) Uani 1 1 d . . . O3 O 0.47653(14) 0.8202(2) 0.91899(13) 0.1283(13) Uani 1 1 d . . . O4 O 0.50419(14) 0.9432(2) 0.84434(13) 0.1133(11) Uani 1 1 d . . . O5 O 0.42848(16) 1.2336(2) 0.75357(14) 0.1121(12) Uani 1 1 d . . . O6 O 0.37512(15) 1.16376(17) 0.71038(15) 0.0984(10) Uani 1 1 d . . . H6C H 0.3463 1.1548 0.7242 0.148 Uiso 1 1 d R . . O7 O 0.5553(2) 0.7073(2) 0.86633(17) 0.1477(17) Uani 1 1 d . . . O8 O 0.62939(16) 0.3984(2) 0.84610(14) 0.1107(11) Uani 1 1 d . . . H8C H 0.6590 0.4073 0.8356 0.166 Uiso 1 1 d R . . O9 O 0.56752(16) 0.3942(2) 0.78954(15) 0.1107(12) Uani 1 1 d . . . O10 O 0.58920(15) 0.8307(3) 0.79566(13) 0.1366(15) Uani 1 1 d . . . O11 O 0.8197(2) 0.8217(3) 0.7490(2) 0.1489(17) Uani 1 1 d . . . O12 O 0.78259(18) 0.7815(3) 0.6804(2) 0.1489(17) Uani 1 1 d . . . O13 O 0.4968(6) 0.3106(9) 0.7729(5) 0.136(6) Uani 0.25 1 d P . . H13A H 0.4762 0.2765 0.7685 0.204 Uiso 0.25 1 d PR . . H13B H 0.4943 0.3367 0.7478 0.204 Uiso 0.25 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.149(6) 0.092(4) 0.098(4) -0.007(3) 0.056(4) -0.013(4) C2 0.105(4) 0.117(5) 0.098(4) 0.000(3) 0.041(4) -0.006(3) C3 0.123(5) 0.122(5) 0.082(3) 0.006(3) 0.027(3) 0.008(3) C4 0.114(4) 0.126(5) 0.104(4) -0.001(3) 0.034(4) -0.010(3) C5 0.120(5) 0.122(5) 0.108(5) 0.010(3) 0.042(4) 0.004(3) C6 0.104(4) 0.217(8) 0.090(4) 0.005(4) 0.019(3) -0.008(4) C7 0.109(4) 0.150(6) 0.120(5) 0.010(4) 0.045(4) -0.001(4) C8 0.113(4) 0.102(4) 0.094(4) 0.005(3) 0.042(3) 0.009(3) C9 0.123(4) 0.080(3) 0.086(3) 0.005(3) 0.039(3) 0.022(3) C10 0.135(4) 0.088(4) 0.087(3) 0.000(3) 0.037(3) 0.018(3) C11 0.114(4) 0.096(5) 0.093(4) 0.005(3) 0.028(3) 0.025(3) C12 0.126(5) 0.088(4) 0.106(4) 0.008(3) 0.031(4) 0.014(3) C13 0.125(4) 0.106(5) 0.101(4) -0.001(4) 0.022(3) 0.009(4) C14 0.105(4) 0.098(4) 0.095(4) 0.012(3) 0.032(3) 0.017(3) C15 0.118(4) 0.101(4) 0.100(4) -0.004(3) 0.022(4) 0.012(3) C16 0.124(4) 0.102(5) 0.096(4) 0.000(3) 0.013(3) 0.021(4) C17 0.115(5) 0.108(5) 0.101(4) 0.009(4) 0.045(4) 0.014(4) C18 0.137(5) 0.095(4) 0.107(4) 0.004(4) 0.011(4) 0.028(4) C19 0.164(6) 0.107(5) 0.124(5) -0.013(4) -0.006(5) 0.020(5) C20 0.189(7) 0.095(5) 0.164(7) -0.011(5) -0.032(6) 0.016(5) C21 0.199(8) 0.119(6) 0.140(6) -0.028(5) -0.010(6) 0.004(6) C22 0.163(7) 0.110(6) 0.127(6) -0.017(5) 0.036(5) -0.005(5) C23 0.164(6) 0.111(5) 0.128(5) -0.016(4) 0.035(5) -0.004(5) C24 0.184(7) 0.129(6) 0.155(6) -0.021(5) -0.018(6) 0.017(5) C25 0.167(8) 0.119(7) 0.148(7) -0.007(5) 0.049(6) 0.000(6) C26 0.134(4) 0.116(4) 0.092(4) 0.005(3) 0.053(3) 0.032(3) C27 0.129(5) 0.147(6) 0.112(5) 0.022(4) 0.053(4) 0.054(5) C28 0.123(5) 0.226(8) 0.105(5) -0.014(5) 0.044(4) 0.044(5) C29 0.143(6) 0.218(9) 0.114(5) 0.018(5) 0.058(5) 0.057(6) C30 0.155(6) 0.154(6) 0.132(6) 0.023(5) 0.089(5) 0.042(5) C31 0.141(5) 0.172(7) 0.148(6) -0.023(5) 0.070(5) 0.001(5) C32 0.136(6) 0.167(7) 0.131(6) -0.011(5) 0.051(5) 0.026(5) C33 0.128(6) 0.139(6) 0.137(7) 0.022(5) 0.046(5) 0.017(5) Cd1 0.1136(3) 0.0880(3) 0.0992(3) -0.0077(2) 0.0431(2) -0.0057(2) O1 0.136(3) 0.145(3) 0.113(3) -0.004(3) 0.058(3) -0.017(3) O2 0.163(4) 0.122(3) 0.095(3) -0.001(2) 0.053(3) -0.016(3) O3 0.118(3) 0.187(4) 0.086(2) 0.016(2) 0.042(2) -0.001(3) O4 0.137(3) 0.096(3) 0.108(3) -0.002(2) 0.015(2) 0.020(2) O5 0.136(3) 0.094(3) 0.109(3) 0.007(2) 0.024(2) 0.014(2) O6 0.114(3) 0.088(2) 0.099(2) -0.008(2) 0.043(2) -0.006(2) O7 0.212(5) 0.090(3) 0.135(3) -0.012(2) -0.014(3) 0.039(3) O8 0.124(3) 0.108(3) 0.110(3) -0.010(2) 0.063(2) -0.010(2) O9 0.124(3) 0.108(3) 0.110(3) -0.010(2) 0.063(2) -0.010(2) O10 0.132(3) 0.187(4) 0.099(3) 0.019(3) 0.052(2) 0.057(3) O11 0.137(4) 0.164(4) 0.157(4) 0.009(3) 0.074(3) 0.012(3) O12 0.137(4) 0.164(5) 0.157(4) 0.009(3) 0.074(3) 0.013(3) O13 0.132(11) 0.186(16) 0.098(10) 0.018(9) 0.052(10) 0.056(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 O2 1.260(7) . ? C1 O1 1.265(7) . ? C1 C2 1.470(8) . ? C2 C3 1.350(8) . ? C2 C7 1.391(8) . ? C3 C4 1.386(7) . ? C3 H3 0.9300 . ? C4 C5 1.387(8) . ? C4 H4 0.9300 . ? C5 O3 1.379(7) . ? C5 C6 1.404(8) . ? C6 C7 1.387(8) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 O3 1.430(6) . ? C8 C9 1.507(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.509(7) . ? C9 C26 1.522(7) . ? C9 C18 1.529(8) . ? C10 O4 1.421(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C16 1.363(7) . ? C11 O4 1.379(6) . ? C11 C12 1.405(7) . ? C12 C13 1.345(7) . ? C12 H12 0.9300 . ? C13 C14 1.405(7) . ? C13 H13 0.9300 . ? C14 C15 1.375(7) . ? C14 C17 1.516(8) . ? C15 C16 1.372(7) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 O5 1.244(7) . ? C17 O6 1.271(7) . ? C17 Cd1 2.740(6) 6_575 ? C18 O7 1.405(6) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.334(9) . ? C19 O7 1.368(7) . ? C19 C24 1.376(9) . ? C20 C21 1.413(9) . ? C20 H20 0.9300 . ? C21 C22 1.348(9) . ? C21 H21 0.9300 . ? C22 C23 1.331(8) . ? C22 C25 1.481(10) . ? C23 C24 1.437(9) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 O9 1.167(9) . ? C25 O8 1.311(9) . ? C26 O10 1.467(6) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C32 1.316(9) . ? C27 O10 1.395(7) . ? C27 C28 1.417(9) . ? C28 C29 1.379(9) . ? C28 H28 0.9300 . ? C29 C30 1.383(10) . ? C29 H29 0.9300 . ? C30 C31 1.426(10) . ? C30 C33 1.561(10) . ? C31 C32 1.436(8) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 O11 1.228(8) . ? C33 O12 1.245(9) . ? C33 Cd1 2.741(8) 8_565 ? Cd1 O8 2.341(4) 5_667 ? Cd1 O1 2.362(4) . ? Cd1 O5 2.386(4) 6_576 ? Cd1 O11 2.412(4) 8_466 ? Cd1 O6 2.420(3) 6_576 ? Cd1 O12 2.441(5) 8_466 ? Cd1 O2 2.543(4) . ? Cd1 O9 2.580(4) 5_667 ? Cd1 C17 2.740(6) 6_576 ? Cd1 C33 2.741(8) 8_466 ? O5 Cd1 2.386(4) 6_575 ? O6 Cd1 2.420(3) 6_575 ? O6 H6C 0.8992 . ? O8 Cd1 2.341(4) 5_667 ? O8 H8C 0.8755 . ? O9 Cd1 2.580(4) 5_667 ? O11 Cd1 2.412(4) 8_565 ? O12 Cd1 2.441(5) 8_565 ? O13 O13 1.29(3) 2_656 ? O13 H13A 0.8501 . ? O13 H13B 0.8500 . ? 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 122.0(6) . . ? O2 C1 C2 118.7(6) . . ? O1 C1 C2 119.3(7) . . ? C3 C2 C7 117.6(5) . . ? C3 C2 C1 122.3(6) . . ? C7 C2 C1 120.1(6) . . ? C2 C3 C4 124.1(6) . . ? C2 C3 H3 118.0 . . ? C4 C3 H3 118.0 . . ? C3 C4 C5 117.7(6) . . ? C3 C4 H4 121.2 . . ? C5 C4 H4 121.2 . . ? O3 C5 C4 126.1(5) . . ? O3 C5 C6 113.6(6) . . ? C4 C5 C6 120.3(6) . . ? C7 C6 C5 118.8(6) . . ? C7 C6 H6 120.6 . . ? C5 C6 H6 120.6 . . ? C6 C7 C2 121.4(6) . . ? C6 C7 H7 119.3 . . ? C2 C7 H7 119.3 . . ? O3 C8 C9 106.7(4) . . ? O3 C8 H8A 110.4 . . ? C9 C8 H8A 110.4 . . ? O3 C8 H8B 110.4 . . ? C9 C8 H8B 110.4 . . ? H8A C8 H8B 108.6 . . ? C8 C9 C10 111.0(4) . . ? C8 C9 C26 107.3(4) . . ? C10 C9 C26 110.8(4) . . ? C8 C9 C18 109.9(4) . . ? C10 C9 C18 106.9(5) . . ? C26 C9 C18 110.9(4) . . ? O4 C10 C9 107.7(4) . . ? O4 C10 H10A 110.2 . . ? C9 C10 H10A 110.2 . . ? O4 C10 H10B 110.2 . . ? C9 C10 H10B 110.2 . . ? H10A C10 H10B 108.5 . . ? C16 C11 O4 116.5(6) . . ? C16 C11 C12 119.7(5) . . ? O4 C11 C12 123.9(6) . . ? C13 C12 C11 119.2(6) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C12 C13 C14 121.3(6) . . ? C12 C13 H13 119.3 . . ? C14 C13 H13 119.3 . . ? C15 C14 C13 118.6(5) . . ? C15 C14 C17 121.1(6) . . ? C13 C14 C17 120.0(6) . . ? C16 C15 C14 120.2(6) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C11 C16 C15 120.9(6) . . ? C11 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? O5 C17 O6 122.5(6) . . ? O5 C17 C14 118.5(7) . . ? O6 C17 C14 118.9(7) . . ? O5 C17 Cd1 60.5(3) . 6_575 ? O6 C17 Cd1 62.0(3) . 6_575 ? C14 C17 Cd1 176.5(4) . 6_575 ? O7 C18 C9 107.0(5) . . ? O7 C18 H18A 110.3 . . ? C9 C18 H18A 110.3 . . ? O7 C18 H18B 110.3 . . ? C9 C18 H18B 110.3 . . ? H18A C18 H18B 108.6 . . ? C20 C19 O7 126.5(7) . . ? C20 C19 C24 120.4(7) . . ? O7 C19 C24 113.1(7) . . ? C19 C20 C21 117.6(7) . . ? C19 C20 H20 121.2 . . ? C21 C20 H20 121.2 . . ? C22 C21 C20 123.2(7) . . ? C22 C21 H21 118.4 . . ? C20 C21 H21 118.4 . . ? C23 C22 C21 119.9(8) . . ? C23 C22 C25 122.5(9) . . ? C21 C22 C25 117.6(9) . . ? C22 C23 C24 118.2(7) . . ? C22 C23 H23 120.9 . . ? C24 C23 H23 120.9 . . ? C19 C24 C23 120.7(7) . . ? C19 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? O9 C25 O8 120.4(8) . . ? O9 C25 C22 127.2(10) . . ? O8 C25 C22 112.4(9) . . ? O10 C26 C9 105.6(5) . . ? O10 C26 H26A 110.6 . . ? C9 C26 H26A 110.6 . . ? O10 C26 H26B 110.6 . . ? C9 C26 H26B 110.6 . . ? H26A C26 H26B 108.8 . . ? C32 C27 O10 124.8(6) . . ? C32 C27 C28 123.5(6) . . ? O10 C27 C28 111.7(7) . . ? C29 C28 C27 118.7(8) . . ? C29 C28 H28 120.7 . . ? C27 C28 H28 120.7 . . ? C28 C29 C30 118.8(7) . . ? C28 C29 H29 120.6 . . ? C30 C29 H29 120.6 . . ? C29 C30 C31 122.9(6) . . ? C29 C30 C33 121.2(7) . . ? C31 C30 C33 115.7(8) . . ? C30 C31 C32 115.9(7) . . ? C30 C31 H31 122.0 . . ? C32 C31 H31 122.0 . . ? C27 C32 C31 120.1(7) . . ? C27 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? O11 C33 O12 124.6(8) . . ? O11 C33 C30 118.6(8) . . ? O12 C33 C30 116.8(8) . . ? O11 C33 Cd1 61.6(4) . 8_565 ? O12 C33 Cd1 63.0(4) . 8_565 ? C30 C33 Cd1 178.9(5) . 8_565 ? O8 Cd1 O1 84.52(15) 5_667 . ? O8 Cd1 O5 134.58(16) 5_667 6_576 ? O1 Cd1 O5 124.20(15) . 6_576 ? O8 Cd1 O11 91.14(15) 5_667 8_466 ? O1 Cd1 O11 137.9(2) . 8_466 ? O5 Cd1 O11 87.52(18) 6_576 8_466 ? O8 Cd1 O6 169.38(15) 5_667 6_576 ? O1 Cd1 O6 85.15(15) . 6_576 ? O5 Cd1 O6 54.63(14) 6_576 6_576 ? O11 Cd1 O6 94.87(15) 8_466 6_576 ? O8 Cd1 O12 88.95(16) 5_667 8_466 ? O1 Cd1 O12 84.39(18) . 8_466 ? O5 Cd1 O12 124.62(17) 6_576 8_466 ? O11 Cd1 O12 53.64(19) 8_466 8_466 ? O6 Cd1 O12 87.59(15) 6_576 8_466 ? O8 Cd1 O2 89.90(13) 5_667 . ? O1 Cd1 O2 53.34(15) . . ? O5 Cd1 O2 83.77(15) 6_576 . ? O11 Cd1 O2 168.7(2) 8_466 . ? O6 Cd1 O2 85.91(13) 6_576 . ? O12 Cd1 O2 137.61(19) 8_466 . ? O8 Cd1 O9 51.57(14) 5_667 5_667 ? O1 Cd1 O9 117.99(14) . 5_667 ? O5 Cd1 O9 83.03(16) 6_576 5_667 ? O11 Cd1 O9 90.13(16) 8_466 5_667 ? O6 Cd1 O9 136.96(16) 6_576 5_667 ? O12 Cd1 O9 127.80(15) 8_466 5_667 ? O2 Cd1 O9 81.75(14) . 5_667 ? O8 Cd1 C17 161.0(2) 5_667 6_576 ? O1 Cd1 C17 105.55(19) . 6_576 ? O5 Cd1 C17 26.99(17) 6_576 6_576 ? O11 Cd1 C17 91.71(17) 8_466 6_576 ? O6 Cd1 C17 27.65(15) 6_576 6_576 ? O12 Cd1 C17 107.75(19) 8_466 6_576 ? O2 Cd1 C17 83.76(15) . 6_576 ? O9 Cd1 C17 109.7(2) 5_667 6_576 ? O8 Cd1 C33 90.16(18) 5_667 8_466 ? O1 Cd1 C33 111.4(3) . 8_466 ? O5 Cd1 C33 106.9(2) 6_576 8_466 ? O11 Cd1 C33 26.6(2) 8_466 8_466 ? O6 Cd1 C33 91.31(18) 6_576 8_466 ? O12 Cd1 C33 27.0(2) 8_466 8_466 ? O2 Cd1 C33 164.6(3) . 8_466 ? O9 Cd1 C33 110.1(2) 5_667 8_466 ? C17 Cd1 C33 100.65(19) 6_576 8_466 ? C1 O1 Cd1 96.5(4) . . ? C1 O2 Cd1 88.2(4) . . ? C5 O3 C8 118.0(5) . . ? C11 O4 C10 119.0(4) . . ? C17 O5 Cd1 92.6(4) . 6_575 ? C17 O6 Cd1 90.3(3) . 6_575 ? C17 O6 H6C 107.9 . . ? Cd1 O6 H6C 108.1 6_575 . ? C19 O7 C18 120.5(5) . . ? C25 O8 Cd1 97.9(5) . 5_667 ? C25 O8 H8C 113.5 . . ? Cd1 O8 H8C 93.1 5_667 . ? C25 O9 Cd1 90.2(6) . 5_667 ? C27 O10 C26 115.6(5) . . ? C33 O11 Cd1 91.8(5) . 8_565 ? C33 O12 Cd1 90.0(5) . 8_565 ? O13 O13 H13A 90.0 2_656 . ? O13 O13 H13B 37.8 2_656 . ? H13A O13 H13B 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C3 -12.7(9) . . . . ? O1 C1 C2 C3 169.9(6) . . . . ? O2 C1 C2 C7 167.6(6) . . . . ? O1 C1 C2 C7 -9.8(9) . . . . ? C7 C2 C3 C4 -2.1(9) . . . . ? C1 C2 C3 C4 178.2(5) . . . . ? C2 C3 C4 C5 0.2(9) . . . . ? C3 C4 C5 O3 -177.3(6) . . . . ? C3 C4 C5 C6 2.6(9) . . . . ? O3 C5 C6 C7 176.5(6) . . . . ? C4 C5 C6 C7 -3.4(10) . . . . ? C5 C6 C7 C2 1.4(10) . . . . ? C3 C2 C7 C6 1.2(9) . . . . ? C1 C2 C7 C6 -179.0(6) . . . . ? O3 C8 C9 C10 54.4(6) . . . . ? O3 C8 C9 C26 175.6(4) . . . . ? O3 C8 C9 C18 -63.7(5) . . . . ? C8 C9 C10 O4 58.8(6) . . . . ? C26 C9 C10 O4 -60.3(5) . . . . ? C18 C9 C10 O4 178.7(4) . . . . ? C16 C11 C12 C13 3.3(8) . . . . ? O4 C11 C12 C13 -176.3(5) . . . . ? C11 C12 C13 C14 -3.7(8) . . . . ? C12 C13 C14 C15 2.7(8) . . . . ? C12 C13 C14 C17 176.7(5) . . . . ? C13 C14 C15 C16 -1.1(8) . . . . ? C17 C14 C15 C16 -175.1(5) . . . . ? O4 C11 C16 C15 177.7(5) . . . . ? C12 C11 C16 C15 -1.9(8) . . . . ? C14 C15 C16 C11 0.8(8) . . . . ? C15 C14 C17 O5 0.6(7) . . . . ? C13 C14 C17 O5 -173.3(5) . . . . ? C15 C14 C17 O6 178.6(5) . . . . ? C13 C14 C17 O6 4.7(7) . . . . ? C15 C14 C17 Cd1 73(10) . . . 6_575 ? C13 C14 C17 Cd1 -101(10) . . . 6_575 ? C8 C9 C18 O7 -60.6(6) . . . . ? C10 C9 C18 O7 178.9(4) . . . . ? C26 C9 C18 O7 57.9(6) . . . . ? O7 C19 C20 C21 178.7(7) . . . . ? C24 C19 C20 C21 0.1(12) . . . . ? C19 C20 C21 C22 -0.9(13) . . . . ? C20 C21 C22 C23 1.0(13) . . . . ? C20 C21 C22 C25 -178.7(7) . . . . ? C21 C22 C23 C24 -0.4(11) . . . . ? C25 C22 C23 C24 179.3(7) . . . . ? C20 C19 C24 C23 0.5(12) . . . . ? O7 C19 C24 C23 -178.3(7) . . . . ? C22 C23 C24 C19 -0.3(11) . . . . ? C23 C22 C25 O9 -176.4(7) . . . . ? C21 C22 C25 O9 3.2(12) . . . . ? C23 C22 C25 O8 4.9(10) . . . . ? C21 C22 C25 O8 -175.4(7) . . . . ? C8 C9 C26 O10 174.0(4) . . . . ? C10 C9 C26 O10 -64.7(5) . . . . ? C18 C9 C26 O10 53.9(5) . . . . ? C32 C27 C28 C29 -1.4(12) . . . . ? O10 C27 C28 C29 178.7(6) . . . . ? C27 C28 C29 C30 0.9(11) . . . . ? C28 C29 C30 C31 1.0(12) . . . . ? C28 C29 C30 C33 175.9(6) . . . . ? C29 C30 C31 C32 -2.3(12) . . . . ? C33 C30 C31 C32 -177.5(6) . . . . ? O10 C27 C32 C31 179.9(6) . . . . ? C28 C27 C32 C31 0.0(12) . . . . ? C30 C31 C32 C27 1.8(11) . . . . ? C29 C30 C33 O11 -173.4(8) . . . . ? C31 C30 C33 O11 1.9(11) . . . . ? C29 C30 C33 O12 5.9(11) . . . . ? C31 C30 C33 O12 -178.8(7) . . . . ? C29 C30 C33 Cd1 -72(39) . . . 8_565 ? C31 C30 C33 Cd1 104(39) . . . 8_565 ? O2 C1 O1 Cd1 -2.0(7) . . . . ? C2 C1 O1 Cd1 175.4(5) . . . . ? O8 Cd1 O1 C1 -92.9(4) 5_667 . . . ? O5 Cd1 O1 C1 49.0(4) 6_576 . . . ? O11 Cd1 O1 C1 -178.5(3) 8_466 . . . ? O6 Cd1 O1 C1 89.6(4) 6_576 . . . ? O12 Cd1 O1 C1 177.6(4) 8_466 . . . ? O2 Cd1 O1 C1 1.0(3) . . . . ? O9 Cd1 O1 C1 -52.2(4) 5_667 . . . ? C17 Cd1 O1 C1 70.7(4) 6_576 . . . ? C33 Cd1 O1 C1 179.1(4) 8_466 . . . ? O1 C1 O2 Cd1 1.8(6) . . . . ? C2 C1 O2 Cd1 -175.5(5) . . . . ? O8 Cd1 O2 C1 82.2(4) 5_667 . . . ? O1 Cd1 O2 C1 -1.0(3) . . . . ? O5 Cd1 O2 C1 -142.9(4) 6_576 . . . ? O11 Cd1 O2 C1 177.6(7) 8_466 . . . ? O6 Cd1 O2 C1 -88.0(4) 6_576 . . . ? O12 Cd1 O2 C1 -6.1(5) 8_466 . . . ? O9 Cd1 O2 C1 133.3(4) 5_667 . . . ? C17 Cd1 O2 C1 -115.7(4) 6_576 . . . ? C33 Cd1 O2 C1 -8.1(9) 8_466 . . . ? C4 C5 O3 C8 0.8(9) . . . . ? C6 C5 O3 C8 -179.1(5) . . . . ? C9 C8 O3 C5 166.1(5) . . . . ? C16 C11 O4 C10 -172.7(5) . . . . ? C12 C11 O4 C10 6.9(7) . . . . ? C9 C10 O4 C11 172.6(4) . . . . ? O6 C17 O5 Cd1 -1.7(5) . . . 6_575 ? C14 C17 O5 Cd1 176.2(4) . . . 6_575 ? O5 C17 O6 Cd1 1.7(5) . . . 6_575 ? C14 C17 O6 Cd1 -176.2(4) . . . 6_575 ? C20 C19 O7 C18 -7.4(12) . . . . ? C24 C19 O7 C18 171.3(6) . . . . ? C9 C18 O7 C19 -167.6(6) . . . . ? O9 C25 O8 Cd1 0.1(8) . . . 5_667 ? C22 C25 O8 Cd1 178.8(5) . . . 5_667 ? O8 C25 O9 Cd1 -0.1(7) . . . 5_667 ? C22 C25 O9 Cd1 -178.6(7) . . . 5_667 ? C32 C27 O10 C26 -14.1(10) . . . . ? C28 C27 O10 C26 165.7(5) . . . . ? C9 C26 O10 C27 -164.5(5) . . . . ? O12 C33 O11 Cd1 -0.4(9) . . . 8_565 ? C30 C33 O11 Cd1 178.8(6) . . . 8_565 ? O11 C33 O12 Cd1 0.4(9) . . . 8_565 ? C30 C33 O12 Cd1 -178.8(6) . . . 8_565 ? # 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 -0.004 -0.001 0.004 8806 2187 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.878 _refine_diff_density_min -1.392 _refine_diff_density_rms 0.057 #===END _database_code_depnum_ccdc_archive 'CCDC 928865'