# 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_rz96_no_w _database_code_depnum_ccdc_archive 'CCDC 894676' #TrackingRef 'web_deposit_cif_file_0_ZhiLin_1343932406.Rupam CEC compound 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H12 Co N2 O5' _chemical_formula_weight 395.23 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 ? _symmetry_space_group_name_H-M pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 17.5123(17) _cell_length_b 13.6834(15) _cell_length_c 15.2911(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3664.2(6) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 0.966 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6985 _exptl_absorpt_correction_T_max 0.9716 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 19261 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 29.12 _reflns_number_total 4911 _reflns_number_gt 3427 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1137P)^2^+4.5667P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4911 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0963 _refine_ls_R_factor_gt 0.0645 _refine_ls_wR_factor_ref 0.2272 _refine_ls_wR_factor_gt 0.2052 _refine_ls_goodness_of_fit_ref 1.130 _refine_ls_restrained_S_all 1.130 _refine_ls_shift/su_max 0.049 _refine_ls_shift/su_mean 0.010 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.44282(3) 0.47752(4) 0.11997(3) 0.0270(2) Uani 1 1 d . . . O3 O 0.55799(15) 0.4867(2) 0.1428(2) 0.0372(7) Uani 1 1 d . . . C2 C 0.6023(2) 0.5129(3) 0.0830(3) 0.0288(8) Uani 1 1 d . . . C3 C 0.6832(2) 0.5293(3) 0.1022(3) 0.0328(9) Uani 1 1 d . . . O4 O 0.70987(14) 0.5191(2) 0.18623(17) 0.0315(6) Uani 1 1 d . . . C5 C 0.7870(2) 0.5350(3) 0.1822(3) 0.0358(9) Uani 1 1 d . . . C6 C 0.8089(2) 0.5541(5) 0.0990(3) 0.0528(14) Uani 1 1 d . . . H6 H 0.8591 0.5681 0.0793 0.063 Uiso 1 1 calc R . . C7 C 0.7417(2) 0.5492(4) 0.0474(3) 0.0494(13) Uani 1 1 d . . . H7 H 0.7384 0.5581 -0.0141 0.059 Uiso 1 1 calc R . . O1 O 0.41605(18) 0.4716(3) -0.0059(2) 0.0507(9) Uani 1 1 d . . . O2 O 0.40340(17) 0.4665(2) 0.2462(2) 0.0449(8) Uani 1 1 d . . . O5 O 0.3003(2) 0.4781(2) 0.1639(2) 0.0475(8) Uani 1 1 d . . . C11 C 0.3316(2) 0.4710(3) 0.2358(3) 0.0367(9) Uani 1 1 d . . . N2 N 0.4305(2) 0.6333(3) 0.1200(2) 0.0376(8) Uani 1 1 d . . . C13 C 0.4825(3) 0.6939(3) 0.1556(3) 0.0440(10) Uani 1 1 d . . . H13 H 0.5269 0.6662 0.1812 0.053 Uiso 1 1 calc R . . C14 C 0.4745(3) 0.7944(3) 0.1567(3) 0.0469(11) Uani 1 1 d . . . H14 H 0.5130 0.8340 0.1824 0.056 Uiso 1 1 calc R . . C15 C 0.4103(3) 0.8371(3) 0.1203(3) 0.0426(10) Uani 1 1 d . . . C16 C 0.3561(3) 0.7750(3) 0.0840(4) 0.0584(15) Uani 1 1 d . . . H16 H 0.3108 0.8009 0.0588 0.070 Uiso 1 1 calc R . . C17 C 0.3686(3) 0.6749(3) 0.0849(4) 0.0512(13) Uani 1 1 d . . . H17 H 0.3312 0.6337 0.0592 0.061 Uiso 1 1 calc R . . C18 C 0.3982(3) 0.9436(3) 0.1183(3) 0.0477(11) Uani 1 1 d . . . H18 H 0.3474 0.9678 0.1165 0.057 Uiso 1 1 calc R . . C19 C 0.4550(3) 1.0065(3) 0.1191(3) 0.0443(11) Uani 1 1 d . . . H19 H 0.5052 0.9801 0.1211 0.053 Uiso 1 1 calc R . . C20 C 0.4486(3) 1.1135(3) 0.1171(3) 0.0400(10) Uani 1 1 d . . . C21 C 0.5140(3) 1.1697(4) 0.1052(4) 0.0647(16) Uani 1 1 d . . . H21 H 0.5619 1.1384 0.0970 0.078 Uiso 1 1 calc R . . C22 C 0.3814(3) 1.1649(4) 0.1272(4) 0.0545(14) Uani 1 1 d . . . H22 H 0.3345 1.1307 0.1340 0.065 Uiso 1 1 calc R . . N1 N 0.4452(2) 0.3192(3) 0.1159(2) 0.0408(9) Uani 1 1 d . . . C24 C 0.5100(3) 0.2693(4) 0.1051(4) 0.0583(14) Uani 1 1 d . . . H24 H 0.5559 0.3051 0.0968 0.070 Uiso 1 1 calc R . . C25 C 0.3821(3) 0.2656(4) 0.1274(4) 0.0589(15) Uani 1 1 d . . . H25 H 0.3351 0.2988 0.1361 0.071 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0294(3) 0.0245(3) 0.0271(3) 0.0012(2) -0.00039(19) -0.0013(2) O3 0.0257(13) 0.0416(17) 0.0444(16) 0.0058(14) 0.0026(11) -0.0041(12) C2 0.0233(16) 0.0293(18) 0.034(2) -0.0036(16) -0.0024(15) 0.0002(15) C3 0.0272(18) 0.044(2) 0.0273(18) 0.0023(17) -0.0047(14) -0.0035(17) O4 0.0252(12) 0.0423(16) 0.0270(13) 0.0018(12) -0.0038(10) -0.0039(12) C5 0.0248(17) 0.047(2) 0.036(2) -0.0019(19) -0.0053(16) -0.0015(17) C6 0.0258(19) 0.094(4) 0.039(2) 0.008(3) -0.0031(17) -0.009(2) C7 0.0298(19) 0.088(4) 0.030(2) 0.009(2) -0.0019(16) -0.013(2) O1 0.0370(16) 0.078(3) 0.0367(17) -0.0030(17) -0.0115(13) -0.0053(17) O2 0.0332(15) 0.0500(18) 0.0514(18) 0.0028(16) 0.0181(14) 0.0023(13) O5 0.059(2) 0.054(2) 0.0296(15) 0.0011(14) 0.0081(15) 0.0002(16) C11 0.039(2) 0.032(2) 0.039(2) 0.0003(18) 0.0141(18) 0.0004(18) N2 0.0388(18) 0.0255(16) 0.049(2) 0.0030(15) -0.0004(15) -0.0003(14) C13 0.048(2) 0.032(2) 0.052(3) 0.001(2) -0.014(2) 0.001(2) C14 0.055(3) 0.028(2) 0.057(3) -0.005(2) -0.015(2) -0.002(2) C15 0.045(2) 0.0255(19) 0.057(3) 0.0039(19) 0.001(2) 0.0000(18) C16 0.039(2) 0.028(2) 0.109(5) 0.009(3) -0.017(3) 0.0018(18) C17 0.037(2) 0.027(2) 0.089(4) 0.001(2) -0.012(2) -0.0026(18) C18 0.045(2) 0.032(2) 0.066(3) 0.000(2) -0.006(2) 0.004(2) C19 0.045(2) 0.028(2) 0.060(3) -0.003(2) -0.001(2) 0.0062(18) C20 0.045(2) 0.0270(19) 0.048(2) -0.0010(18) -0.0016(19) 0.0017(18) C21 0.049(3) 0.032(2) 0.112(5) -0.005(3) 0.023(3) 0.003(2) C22 0.041(2) 0.031(2) 0.092(4) -0.003(2) -0.006(2) -0.001(2) N1 0.049(2) 0.0272(17) 0.047(2) -0.0029(16) 0.0009(17) -0.0014(16) C24 0.051(3) 0.029(2) 0.095(4) -0.003(3) 0.023(3) -0.003(2) C25 0.041(3) 0.032(2) 0.104(5) -0.009(3) -0.009(3) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 1.982(3) . ? Co1 O3 2.051(3) . ? Co1 O2 2.055(3) . ? Co1 N2 2.143(4) . ? Co1 N1 2.167(4) . ? O3 C2 1.252(5) . ? C2 O1 1.240(5) 5_665 ? C2 C3 1.465(5) . ? C3 C7 1.351(6) . ? C3 O4 1.373(4) . ? O4 C5 1.369(4) . ? C5 C6 1.354(6) . ? C5 C11 1.480(5) 4_565 ? C6 C7 1.419(6) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? O1 C2 1.240(5) 5_665 ? O2 C11 1.270(5) . ? O5 C11 1.232(5) . ? C11 C5 1.480(5) 4_465 ? N2 C17 1.337(6) . ? N2 C13 1.346(6) . ? C13 C14 1.382(6) . ? C13 H13 0.9500 . ? C14 C15 1.385(6) . ? C14 H14 0.9500 . ? C15 C16 1.389(7) . ? C15 C18 1.472(6) . ? C16 C17 1.387(6) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.316(7) . ? C18 H18 0.9500 . ? C19 C20 1.468(6) . ? C19 H19 0.9500 . ? C20 C22 1.380(6) . ? C20 C21 1.391(7) . ? C21 C24 1.365(7) 1_565 ? C21 H21 0.9500 . ? C22 C25 1.378(7) 1_565 ? C22 H22 0.9500 . ? N1 C24 1.336(6) . ? N1 C25 1.338(6) . ? C24 C21 1.365(7) 1_545 ? C24 H24 0.9500 . ? C25 C22 1.378(7) 1_545 ? C25 H25 0.9500 . ? 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 Co1 O3 113.59(14) . . ? O1 Co1 O2 146.01(14) . . ? O3 Co1 O2 100.09(13) . . ? O1 Co1 N2 90.97(15) . . ? O3 Co1 N2 92.19(13) . . ? O2 Co1 N2 92.21(13) . . ? O1 Co1 N1 86.35(15) . . ? O3 Co1 N1 92.71(13) . . ? O2 Co1 N1 87.71(13) . . ? N2 Co1 N1 175.04(14) . . ? C2 O3 Co1 120.2(3) . . ? O1 C2 O3 125.7(4) 5_665 . ? O1 C2 C3 114.6(3) 5_665 . ? O3 C2 C3 119.8(4) . . ? C7 C3 O4 110.1(3) . . ? C7 C3 C2 129.7(4) . . ? O4 C3 C2 120.1(3) . . ? C5 O4 C3 106.1(3) . . ? C6 C5 O4 110.6(3) . . ? C6 C5 C11 131.1(4) . 4_565 ? O4 C5 C11 118.3(4) . 4_565 ? C5 C6 C7 106.2(4) . . ? C5 C6 H6 126.9 . . ? C7 C6 H6 126.9 . . ? C3 C7 C6 107.0(4) . . ? C3 C7 H7 126.5 . . ? C6 C7 H7 126.5 . . ? C2 O1 Co1 167.8(3) 5_665 . ? C11 O2 Co1 102.2(3) . . ? O5 C11 O2 123.8(4) . . ? O5 C11 C5 121.7(4) . 4_465 ? O2 C11 C5 114.5(4) . 4_465 ? C17 N2 C13 116.6(4) . . ? C17 N2 Co1 120.4(3) . . ? C13 N2 Co1 123.0(3) . . ? N2 C13 C14 123.3(4) . . ? N2 C13 H13 118.3 . . ? C14 C13 H13 118.3 . . ? C13 C14 C15 119.8(4) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C14 C15 C16 117.2(4) . . ? C14 C15 C18 122.9(4) . . ? C16 C15 C18 119.9(4) . . ? C17 C16 C15 119.5(4) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? N2 C17 C16 123.6(4) . . ? N2 C17 H17 118.2 . . ? C16 C17 H17 118.2 . . ? C19 C18 C15 122.6(5) . . ? C19 C18 H18 118.7 . . ? C15 C18 H18 118.7 . . ? C18 C19 C20 126.5(5) . . ? C18 C19 H19 116.8 . . ? C20 C19 H19 116.8 . . ? C22 C20 C21 115.8(4) . . ? C22 C20 C19 124.8(4) . . ? C21 C20 C19 119.4(4) . . ? C24 C21 C20 120.7(5) 1_565 . ? C24 C21 H21 119.6 1_565 . ? C20 C21 H21 119.6 . . ? C25 C22 C20 120.2(5) 1_565 . ? C25 C22 H22 119.9 1_565 . ? C20 C22 H22 119.9 . . ? C24 N1 C25 116.0(4) . . ? C24 N1 Co1 122.1(3) . . ? C25 N1 Co1 121.9(3) . . ? N1 C24 C21 123.6(5) . 1_545 ? N1 C24 H24 118.2 . . ? C21 C24 H24 118.2 1_545 . ? N1 C25 C22 123.8(5) . 1_545 ? N1 C25 H25 118.1 . . ? C22 C25 H25 118.1 1_545 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 29.12 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.250 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.123 data_rz97_no_w _database_code_depnum_ccdc_archive 'CCDC 894677' #TrackingRef 'web_deposit_cif_file_1_ZhiLin_1343932406.Rupam CEC compound 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H12 N2 Ni O5' _chemical_formula_weight 395.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 17.1691(4) _cell_length_b 13.5523(4) _cell_length_c 15.4503(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3594.99(18) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 1.110 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6069 _exptl_absorpt_correction_T_max 0.9570 _exptl_absorpt_process_details SADABS _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 17127 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 27.11 _reflns_number_total 3966 _reflns_number_gt 3153 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1183P)^2^+8.2227P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3966 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0729 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.2263 _refine_ls_wR_factor_gt 0.2131 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.157 _refine_ls_shift/su_max 0.027 _refine_ls_shift/su_mean 0.005 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.43593(3) 0.02523(4) 0.12260(4) 0.0264(2) Uani 1 1 d . . . O4 O 0.55348(18) 0.0157(3) 0.1400(2) 0.0338(7) Uani 1 1 d . . . C2 C 0.5981(2) -0.0139(3) 0.0813(3) 0.0282(9) Uani 1 1 d . . . C3 C 0.6815(3) -0.0304(4) 0.1017(3) 0.0327(10) Uani 1 1 d . . . O5 O 0.70922(17) -0.0180(2) 0.1841(2) 0.0305(7) Uani 1 1 d . . . C5 C 0.7881(3) -0.0344(4) 0.1795(3) 0.0357(11) Uani 1 1 d . . . C6 C 0.8094(3) -0.0553(6) 0.0969(4) 0.0547(16) Uani 1 1 d . . . H6 H 0.8595 -0.0683 0.0770 0.066 Uiso 1 1 calc R . . C7 C 0.7401(3) -0.0534(5) 0.0470(3) 0.0508(15) Uani 1 1 d . . . H7 H 0.7358 -0.0656 -0.0120 0.061 Uiso 1 1 calc R . . O3 O 0.4199(2) 0.0343(3) -0.0063(2) 0.0508(10) Uani 1 1 d . . . O1 O 0.40838(19) 0.0286(3) 0.2528(2) 0.0389(8) Uani 1 1 d . . . O2 O 0.30519(19) 0.0248(2) 0.1675(2) 0.0360(7) Uani 1 1 d . . . C11 C 0.3351(3) 0.0286(3) 0.2408(3) 0.0334(10) Uani 1 1 d . . . N2 N 0.4373(2) 0.1801(3) 0.1204(3) 0.0367(9) Uani 1 1 d . . . C13 C 0.5022(3) 0.2297(4) 0.1045(5) 0.0643(19) Uani 1 1 d . . . H13 H 0.5473 0.1937 0.0935 0.077 Uiso 1 1 calc R . . C14 C 0.5073(4) 0.3298(5) 0.1033(5) 0.069(2) Uani 1 1 d . . . H14 H 0.5551 0.3596 0.0923 0.083 Uiso 1 1 calc R . . C15 C 0.4428(3) 0.3876(4) 0.1179(3) 0.0401(12) Uani 1 1 d . . . C16 C 0.3744(3) 0.3373(4) 0.1339(4) 0.0551(16) Uani 1 1 d . . . H16 H 0.3284 0.3720 0.1432 0.066 Uiso 1 1 calc R . . C17 C 0.3744(3) 0.2356(4) 0.1363(5) 0.0567(17) Uani 1 1 d . . . H17 H 0.3280 0.2037 0.1498 0.068 Uiso 1 1 calc R . . C18 C 0.4504(3) 0.4957(4) 0.1182(4) 0.0455(13) Uani 1 1 d . . . H18 H 0.5007 0.5211 0.1202 0.055 Uiso 1 1 calc R . . C19 C 0.3936(3) 0.5594(4) 0.1160(4) 0.0495(14) Uani 1 1 d . . . H19 H 0.3428 0.5357 0.1131 0.059 Uiso 1 1 calc R . . C20 C 0.4055(3) 0.6659(4) 0.1177(4) 0.0451(13) Uani 1 1 d . . . C21 C 0.4692(3) 0.7106(4) 0.1591(4) 0.0473(13) Uani 1 1 d . . . H21 H 0.5065 0.6720 0.1867 0.057 Uiso 1 1 calc R . . C22 C 0.3535(3) 0.7292(4) 0.0760(5) 0.0604(18) Uani 1 1 d . . . H22 H 0.3108 0.7038 0.0465 0.072 Uiso 1 1 calc R . . N1 N 0.4257(2) -0.1275(3) 0.1196(3) 0.0349(9) Uani 1 1 d . . . C24 C 0.4763(3) -0.1878(4) 0.1586(4) 0.0445(12) Uani 1 1 d . . . H24 H 0.5187 -0.1598 0.1870 0.053 Uiso 1 1 calc R . . C25 C 0.3661(3) -0.1700(4) 0.0787(4) 0.0510(14) Uani 1 1 d . . . H25 H 0.3307 -0.1294 0.0503 0.061 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0222(3) 0.0270(4) 0.0302(4) -0.0020(2) 0.00014(19) 0.0011(2) O4 0.0231(15) 0.0397(19) 0.0386(17) -0.0079(14) -0.0005(13) 0.0027(13) C2 0.022(2) 0.030(2) 0.032(2) 0.0025(18) -0.0014(16) -0.0005(16) C3 0.024(2) 0.047(3) 0.027(2) -0.0002(19) -0.0044(17) 0.0034(18) O5 0.0209(14) 0.0404(17) 0.0302(16) -0.0012(13) -0.0022(12) 0.0026(12) C5 0.021(2) 0.046(3) 0.040(3) 0.001(2) -0.0040(18) 0.0049(18) C6 0.026(2) 0.101(5) 0.037(3) -0.006(3) -0.001(2) 0.012(3) C7 0.030(3) 0.088(4) 0.034(3) -0.010(3) -0.002(2) 0.014(3) O3 0.0362(19) 0.084(3) 0.0323(19) -0.0041(18) -0.0105(15) 0.0095(19) O1 0.0232(15) 0.054(2) 0.0399(18) -0.0018(16) 0.0068(14) -0.0013(14) O2 0.0314(16) 0.0429(19) 0.0337(17) -0.0003(14) 0.0030(13) 0.0029(14) C11 0.028(2) 0.035(2) 0.037(2) 0.003(2) 0.0057(18) -0.0004(18) N2 0.037(2) 0.0267(19) 0.046(2) 0.0013(17) 0.0027(17) 0.0005(16) C13 0.044(3) 0.033(3) 0.116(6) 0.002(3) 0.030(3) 0.001(2) C14 0.044(3) 0.036(3) 0.127(6) 0.007(4) 0.026(4) -0.002(2) C15 0.045(3) 0.029(2) 0.046(3) 0.003(2) -0.003(2) -0.003(2) C16 0.036(3) 0.033(3) 0.096(5) 0.002(3) -0.002(3) 0.005(2) C17 0.032(3) 0.035(3) 0.103(5) 0.012(3) 0.001(3) 0.001(2) C18 0.041(3) 0.031(2) 0.065(4) 0.001(2) -0.004(2) -0.004(2) C19 0.042(3) 0.036(3) 0.071(4) -0.001(3) -0.011(3) 0.000(2) C20 0.042(3) 0.030(2) 0.063(4) -0.007(2) -0.002(2) 0.000(2) C21 0.046(3) 0.029(2) 0.067(4) 0.003(2) -0.016(3) 0.003(2) C22 0.045(3) 0.033(3) 0.103(5) -0.010(3) -0.026(3) -0.002(2) N1 0.034(2) 0.0221(18) 0.049(2) -0.0030(16) -0.0035(16) 0.0009(15) C24 0.044(3) 0.033(3) 0.056(3) -0.002(2) -0.014(2) -0.003(2) C25 0.040(3) 0.032(3) 0.081(4) -0.002(3) -0.018(3) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O3 2.014(4) . ? Ni1 O4 2.040(3) . ? Ni1 O1 2.067(4) . ? Ni1 N1 2.077(4) . ? Ni1 N2 2.099(4) . ? Ni1 O2 2.350(3) . ? Ni1 C11 2.516(5) . ? O4 C2 1.253(5) . ? C2 O3 1.232(6) 5_655 ? C2 C3 1.484(6) . ? C3 C7 1.350(7) . ? C3 O5 1.370(5) . ? O5 C5 1.374(5) . ? C5 C6 1.358(7) . ? C5 C11 1.475(6) 4 ? C6 C7 1.418(7) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? O3 C2 1.232(6) 5_655 ? O1 C11 1.271(6) . ? O2 C11 1.244(6) . ? C11 C5 1.475(6) 4_455 ? N2 C13 1.325(7) . ? N2 C17 1.339(7) . ? C13 C14 1.359(8) . ? C13 H13 0.9300 . ? C14 C15 1.375(8) . ? C14 H14 0.9300 . ? C15 C16 1.380(7) . ? C15 C18 1.471(7) . ? C16 C17 1.379(8) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.303(8) . ? C18 H18 0.9300 . ? C19 C20 1.459(8) . ? C19 H19 0.9300 . ? C20 C22 1.396(8) . ? C20 C21 1.405(7) . ? C21 C24 1.382(7) 1_565 ? C21 H21 0.9300 . ? C22 C25 1.383(8) 1_565 ? C22 H22 0.9300 . ? N1 C25 1.334(6) . ? N1 C24 1.337(6) . ? C24 C21 1.382(7) 1_545 ? C24 H24 0.9300 . ? C25 C22 1.383(8) 1_545 ? C25 H25 0.9300 . ? 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 O3 Ni1 O4 105.62(15) . . ? O3 Ni1 O1 158.38(15) . . ? O4 Ni1 O1 95.71(14) . . ? O3 Ni1 N1 91.59(17) . . ? O4 Ni1 N1 91.37(14) . . ? O1 Ni1 N1 91.38(15) . . ? O3 Ni1 N2 85.64(17) . . ? O4 Ni1 N2 93.12(14) . . ? O1 Ni1 N2 89.79(15) . . ? N1 Ni1 N2 175.22(16) . . ? O3 Ni1 O2 99.32(14) . . ? O4 Ni1 O2 154.96(13) . . ? O1 Ni1 O2 59.59(12) . . ? N1 Ni1 O2 85.59(14) . . ? N2 Ni1 O2 91.01(13) . . ? O3 Ni1 C11 128.51(16) . . ? O4 Ni1 C11 125.86(15) . . ? O1 Ni1 C11 30.22(15) . . ? N1 Ni1 C11 88.61(15) . . ? N2 Ni1 C11 90.07(15) . . ? O2 Ni1 C11 29.38(14) . . ? C2 O4 Ni1 122.0(3) . . ? O3 C2 O4 126.8(4) 5_655 . ? O3 C2 C3 114.1(4) 5_655 . ? O4 C2 C3 119.0(4) . . ? C7 C3 O5 110.6(4) . . ? C7 C3 C2 128.4(4) . . ? O5 C3 C2 120.9(4) . . ? C3 O5 C5 105.9(4) . . ? C6 C5 O5 110.4(4) . . ? C6 C5 C11 130.4(4) . 4 ? O5 C5 C11 119.2(4) . 4 ? C5 C6 C7 106.3(4) . . ? C5 C6 H6 126.8 . . ? C7 C6 H6 126.8 . . ? C3 C7 C6 106.8(5) . . ? C3 C7 H7 126.6 . . ? C6 C7 H7 126.6 . . ? C2 O3 Ni1 162.1(4) 5_655 . ? C11 O1 Ni1 94.9(3) . . ? C11 O2 Ni1 82.7(3) . . ? O2 C11 O1 122.8(4) . . ? O2 C11 C5 122.4(4) . 4_455 ? O1 C11 C5 114.9(4) . 4_455 ? O2 C11 Ni1 67.9(3) . . ? O1 C11 Ni1 54.9(2) . . ? C5 C11 Ni1 169.6(3) 4_455 . ? C13 N2 C17 115.3(5) . . ? C13 N2 Ni1 121.3(4) . . ? C17 N2 Ni1 123.4(3) . . ? N2 C13 C14 124.2(6) . . ? N2 C13 H13 117.9 . . ? C14 C13 H13 117.9 . . ? C13 C14 C15 121.0(6) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C14 C15 C16 115.7(5) . . ? C14 C15 C18 119.8(5) . . ? C16 C15 C18 124.5(5) . . ? C17 C16 C15 119.9(5) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? N2 C17 C16 123.8(5) . . ? N2 C17 H17 118.1 . . ? C16 C17 H17 118.1 . . ? C19 C18 C15 126.4(6) . . ? C19 C18 H18 116.8 . . ? C15 C18 H18 116.8 . . ? C18 C19 C20 123.3(5) . . ? C18 C19 H19 118.3 . . ? C20 C19 H19 118.3 . . ? C22 C20 C21 116.3(5) . . ? C22 C20 C19 120.7(5) . . ? C21 C20 C19 123.0(5) . . ? C24 C21 C20 119.8(5) 1_565 . ? C24 C21 H21 120.1 1_565 . ? C20 C21 H21 120.1 . . ? C25 C22 C20 119.6(5) 1_565 . ? C25 C22 H22 120.2 1_565 . ? C20 C22 H22 120.2 . . ? C25 N1 C24 116.6(4) . . ? C25 N1 Ni1 120.4(3) . . ? C24 N1 Ni1 122.9(3) . . ? N1 C24 C21 123.6(5) . 1_545 ? N1 C24 H24 118.2 . . ? C21 C24 H24 118.2 1_545 . ? N1 C25 C22 124.1(5) . 1_545 ? N1 C25 H25 118.0 . . ? C22 C25 H25 118.0 1_545 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.11 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.451 _refine_diff_density_min -0.283 _refine_diff_density_rms 0.136 data_rz202 _database_code_depnum_ccdc_archive 'CCDC 894678' #TrackingRef 'web_deposit_cif_file_2_ZhiLin_1343932406.Rupam CEC compound 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H26 Co2 N4 O10' _chemical_formula_weight 792.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P21/C loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.6268(5) _cell_length_b 16.8885(6) _cell_length_c 15.9853(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.269(2) _cell_angle_gamma 90.00 _cell_volume 3672.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 0.964 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8016 _exptl_absorpt_correction_T_max 0.9624 _exptl_absorpt_process_details SADABS _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 32888 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0420 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 27.90 _reflns_number_total 8751 _reflns_number_gt 6244 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1095P)^2^+5.5570P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8751 _refine_ls_number_parameters 470 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0804 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.2073 _refine_ls_wR_factor_gt 0.1862 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.017 _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 CoA Co 0.02156(4) 0.06609(3) 0.12080(3) 0.02414(16) Uani 1 1 d . . . O1A O 0.0429(2) 0.09176(17) 0.24842(18) 0.0382(7) Uani 1 1 d . . . O2A O 0.0228(2) 0.19979(18) 0.17218(17) 0.0371(7) Uani 1 1 d . . . C3A C 0.0350(3) 0.1654(2) 0.2414(2) 0.0320(8) Uani 1 1 d . . . O4A O 0.0027(3) 0.08897(19) -0.00117(18) 0.0478(8) Uani 1 1 d . . . O5A O 0.0163(2) -0.05506(16) 0.13539(17) 0.0322(6) Uani 1 1 d . . . C6A C -0.0038(3) -0.1036(2) 0.0774(2) 0.0259(8) Uani 1 1 d . . . C7A C -0.0286(3) -0.1857(2) 0.0980(2) 0.0312(8) Uani 1 1 d . . . O8A O -0.0193(2) -0.21039(15) 0.17965(15) 0.0291(6) Uani 1 1 d . . . C9A C -0.0429(3) -0.2893(2) 0.1787(2) 0.0338(9) Uani 1 1 d . . . C10A C -0.0668(4) -0.3133(3) 0.0995(3) 0.0525(13) Uani 1 1 d . . . H10A H -0.0862 -0.3639 0.0826 0.063 Uiso 1 1 calc R . . C11A C -0.0564(4) -0.2462(3) 0.0473(3) 0.0510(13) Uani 1 1 d . . . H11A H -0.0667 -0.2444 -0.0107 0.061 Uiso 1 1 calc R . . \~N1A N 0.1788(3) 0.0692(2) 0.1113(2) 0.0371(8) Uani 1 1 d . . . C13A C 0.2367(3) 0.1272(3) 0.1406(4) 0.0513(13) Uani 1 1 d . . . H13A H 0.2072 0.1706 0.1648 0.062 Uiso 1 1 calc R . . N2A N -0.1340(2) 0.0734(2) 0.1286(2) 0.0312(7) Uani 1 1 d . . . C15A C -0.1838(3) 0.1350(3) 0.0959(3) 0.0476(12) Uani 1 1 d . . . H15A H -0.1495 0.1721 0.0660 0.057 Uiso 1 1 calc R . . C16A C -0.2845(4) 0.1473(3) 0.1038(4) 0.0529(13) Uani 1 1 d . . . C17A C -0.3369(3) 0.0938(3) 0.1491(3) 0.0392(10) Uani 1 1 d . . . C18A C -0.2856(3) 0.0278(3) 0.1808(3) 0.0439(11) Uani 1 1 d . . . H18A H -0.3183 -0.0114 0.2092 0.053 Uiso 1 1 calc R . . C19A C -0.1864(3) 0.0207(3) 0.1698(3) 0.0393(10) Uani 1 1 d . . . H19A H -0.1539 -0.0235 0.1924 0.047 Uiso 1 1 calc R . . C20A C -0.4443(3) 0.1045(3) 0.1610(3) 0.0457(11) Uani 1 1 d . . . H20A H -0.4588 0.0873 0.2168 0.055 Uiso 1 1 calc R . . H20B H -0.4610 0.1602 0.1558 0.055 Uiso 1 1 calc R . . C21A C -0.5052(3) 0.0584(3) 0.0979(3) 0.0483(12) Uani 1 1 d . . . H21A H -0.4867 0.0031 0.1031 0.058 Uiso 1 1 calc R . . H21B H -0.4891 0.0758 0.0425 0.058 Uiso 1 1 calc R . . C22A C -0.6157(3) 0.0644(3) 0.1038(3) 0.0380(10) Uani 1 1 d . . . C23A C -0.6627(3) 0.1275(3) 0.1376(4) 0.0511(13) Uani 1 1 d . . . H23A H -0.6265 0.1706 0.1584 0.061 Uiso 1 1 calc R . . C24A C -0.7760(4) 0.0083(4) 0.0768(4) 0.0671(18) Uani 1 1 d . . . C25A C -0.6758(4) 0.0040(4) 0.0730(4) 0.0704(19) Uani 1 1 d . . . H25A H -0.6478 -0.0403 0.0493 0.085 Uiso 1 1 calc R . . CoB Co 0.47187(4) 0.43910(3) 0.11730(3) 0.02322(16) Uani 1 1 d . . . O1B O 0.4667(2) 0.41397(17) 0.24627(19) 0.0371(7) Uani 1 1 d . . . O2B O 0.4745(2) 0.30461(18) 0.17097(17) 0.0373(7) Uani 1 1 d . . . C3B C 0.4680(3) 0.3393(2) 0.2395(2) 0.0307(8) Uani 1 1 d . . . O4B O 0.4823(2) 0.56074(15) 0.12937(17) 0.0316(6) Uani 1 1 d . . . O5B O 0.4589(2) 0.41166(17) -0.00493(16) 0.0365(7) Uani 1 1 d . . . C6B C 0.4809(3) 0.3938(2) -0.0770(2) 0.0259(8) Uani 1 1 d . . . C7B C 0.4621(3) 0.3102(2) -0.1007(2) 0.0300(8) Uani 1 1 d . . . O8B O 0.4789(2) 0.28478(15) -0.17988(15) 0.0284(6) Uani 1 1 d . . . C9B C 0.4577(3) 0.2056(2) -0.1817(2) 0.0316(9) Uani 1 1 d . . . C10B C 0.4292(4) 0.1816(3) -0.1065(3) 0.0525(13) Uani 1 1 d . . . H10B H 0.4116 0.1304 -0.0917 0.063 Uiso 1 1 calc R . . C11B C 0.4314(4) 0.2496(3) -0.0538(3) 0.0517(13) Uani 1 1 d . . . H11B H 0.4149 0.2519 0.0018 0.062 Uiso 1 1 calc R . . N2B N 0.6272(2) 0.42693(19) 0.1223(2) 0.0290(7) Uani 1 1 d . . . C13B C 0.6855(3) 0.4729(3) 0.1707(3) 0.0466(11) Uani 1 1 d . . . H13B H 0.6566 0.5131 0.2006 0.056 Uiso 1 1 calc R . . C14B C 0.7861(4) 0.4645(3) 0.1794(4) 0.0576(14) Uani 1 1 d . . . H14B H 0.8233 0.4988 0.2140 0.069 Uiso 1 1 calc R . . C15B C 0.8315(3) 0.4051(3) 0.1365(4) 0.0494(13) Uani 1 1 d . . . C16B C 0.7719(3) 0.3588(3) 0.0840(3) 0.0495(12) Uani 1 1 d . . . H16B H 0.7992 0.3196 0.0519 0.059 Uiso 1 1 calc R . . C17B C 0.6708(3) 0.3708(3) 0.0792(3) 0.0399(10) Uani 1 1 d . . . H17B H 0.6319 0.3381 0.0443 0.048 Uiso 1 1 calc R . . N1B N 0.3132(2) 0.4409(2) 0.1130(2) 0.0324(7) Uani 1 1 d . . . C19B C 0.2636(3) 0.5077(3) 0.0990(4) 0.0526(13) Uani 1 1 d . . . H19B H 0.2988 0.5537 0.0894 0.063 Uiso 1 1 calc R . . C20B C 0.1628(4) 0.5123(3) 0.0978(4) 0.0580(15) Uani 1 1 d . . . H20C H 0.1319 0.5607 0.0878 0.070 Uiso 1 1 calc R . . C21B C 0.1071(3) 0.4460(3) 0.1113(3) 0.0403(10) Uani 1 1 d . . . C22B C 0.1588(3) 0.3765(3) 0.1276(3) 0.0480(12) Uani 1 1 d . . . H22B H 0.1255 0.3299 0.1385 0.058 Uiso 1 1 calc R . . C23B C 0.2594(3) 0.3770(3) 0.1275(3) 0.0480(12) Uani 1 1 d . . . H23B H 0.2924 0.3296 0.1383 0.058 Uiso 1 1 calc R . . C24B C -0.0040(4) 0.4528(4) 0.1069(5) 0.0691(18) Uani 1 1 d . . . H24A H -0.0208 0.5035 0.1309 0.083 Uiso 1 1 calc R . . H24B H -0.0266 0.4540 0.0483 0.083 Uiso 1 1 calc R . . C25B C -0.0588(4) 0.3926(4) 0.1474(5) 0.0722(19) Uani 1 1 d . . . H25B H -0.0394 0.3921 0.2067 0.087 Uiso 1 1 calc R . . H25C H -0.0426 0.3413 0.1245 0.087 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 CoA 0.0225(3) 0.0252(3) 0.0248(3) 0.00094(19) 0.00180(19) -0.0027(2) O1A 0.0477(18) 0.0257(15) 0.0407(15) -0.0098(12) -0.0021(13) 0.0073(13) O2A 0.0426(17) 0.0377(17) 0.0307(14) -0.0057(12) -0.0002(12) 0.0020(13) C3A 0.0271(19) 0.032(2) 0.037(2) -0.0093(16) 0.0009(15) 0.0029(17) O4A 0.080(3) 0.0348(17) 0.0286(14) 0.0094(12) 0.0043(15) -0.0021(16) O5A 0.0386(16) 0.0229(14) 0.0353(14) -0.0006(11) 0.0035(12) -0.0016(12) C6A 0.0266(18) 0.0238(19) 0.0278(17) 0.0031(14) 0.0055(14) 0.0037(15) C7A 0.044(2) 0.027(2) 0.0229(16) 0.0021(15) 0.0006(15) -0.0014(17) O8A 0.0390(15) 0.0246(14) 0.0235(12) 0.0049(10) -0.0001(11) -0.0032(11) C9A 0.046(2) 0.0217(19) 0.0333(19) 0.0044(15) -0.0001(17) -0.0041(17) C10A 0.089(4) 0.028(2) 0.039(2) 0.0024(19) -0.012(2) -0.013(2) C11A 0.093(4) 0.031(2) 0.028(2) 0.0026(17) -0.009(2) -0.011(2) \~N1A 0.0255(17) 0.043(2) 0.044(2) -0.0044(16) 0.0084(15) -0.0050(15) C13A 0.028(2) 0.035(3) 0.092(4) -0.017(2) 0.011(2) -0.0021(19) N2A 0.0208(16) 0.0329(19) 0.0399(18) 0.0027(14) 0.0008(13) -0.0012(14) C15A 0.029(2) 0.036(3) 0.078(3) 0.018(2) 0.006(2) 0.0007(19) C16A 0.032(2) 0.039(3) 0.087(4) 0.009(3) 0.005(2) 0.002(2) C17A 0.024(2) 0.046(3) 0.048(2) -0.011(2) -0.0008(17) -0.0016(19) C18A 0.032(2) 0.051(3) 0.050(3) 0.009(2) 0.0081(19) -0.005(2) C19A 0.029(2) 0.043(3) 0.046(2) 0.0128(19) 0.0050(18) 0.0002(19) C20A 0.025(2) 0.054(3) 0.058(3) -0.015(2) 0.0080(19) 0.002(2) C21A 0.027(2) 0.061(3) 0.057(3) -0.020(2) 0.008(2) 0.001(2) C22A 0.027(2) 0.048(3) 0.039(2) -0.0071(19) 0.0061(17) -0.0015(19) C23A 0.030(2) 0.038(3) 0.085(4) -0.016(2) 0.002(2) -0.005(2) C24A 0.037(3) 0.073(4) 0.094(4) -0.048(3) 0.024(3) -0.015(3) C25A 0.035(3) 0.074(4) 0.104(5) -0.056(4) 0.022(3) -0.009(3) CoB 0.0201(3) 0.0246(3) 0.0252(3) -0.00217(18) 0.00333(18) -0.00149(19) O1B 0.0436(17) 0.0245(15) 0.0440(16) 0.0111(12) 0.0083(13) 0.0048(13) O2B 0.0424(17) 0.0386(17) 0.0311(14) 0.0053(12) 0.0041(12) -0.0020(13) C3B 0.0258(19) 0.034(2) 0.0322(19) 0.0086(16) 0.0023(15) 0.0008(17) O4B 0.0348(15) 0.0234(14) 0.0374(14) -0.0019(11) 0.0089(12) -0.0041(11) O5B 0.0486(18) 0.0340(16) 0.0273(13) -0.0087(11) 0.0044(12) -0.0035(14) C6B 0.0224(17) 0.0250(19) 0.0296(18) -0.0043(14) -0.0035(14) -0.0005(15) C7B 0.041(2) 0.027(2) 0.0233(16) -0.0038(14) 0.0068(15) -0.0001(17) O8B 0.0382(15) 0.0220(13) 0.0257(12) -0.0024(10) 0.0067(11) -0.0018(11) C9B 0.044(2) 0.0190(18) 0.0321(19) -0.0045(15) 0.0063(17) -0.0027(17) C10B 0.094(4) 0.024(2) 0.042(2) -0.0009(18) 0.020(2) -0.013(2) C11B 0.092(4) 0.030(2) 0.036(2) -0.0027(18) 0.025(2) -0.011(2) N2B 0.0177(15) 0.0324(18) 0.0369(17) -0.0013(13) 0.0025(12) -0.0004(13) C13B 0.030(2) 0.049(3) 0.060(3) -0.021(2) 0.000(2) -0.003(2) C14B 0.028(2) 0.059(3) 0.085(4) -0.014(3) -0.008(2) -0.006(2) C15B 0.023(2) 0.041(3) 0.085(4) 0.016(3) 0.006(2) 0.0000(19) C16B 0.033(2) 0.042(3) 0.075(3) -0.001(2) 0.014(2) 0.010(2) C17B 0.029(2) 0.037(2) 0.054(3) -0.006(2) 0.0036(18) 0.0020(18) N1B 0.0186(15) 0.041(2) 0.0372(17) -0.0009(15) 0.0010(13) -0.0023(14) C19B 0.026(2) 0.051(3) 0.080(4) 0.025(3) -0.002(2) -0.005(2) C20B 0.029(2) 0.048(3) 0.096(4) 0.024(3) -0.001(3) 0.002(2) C21B 0.022(2) 0.046(3) 0.052(3) 0.002(2) 0.0015(18) -0.0003(18) C22B 0.027(2) 0.036(3) 0.081(3) -0.004(2) 0.005(2) -0.0071(19) C23B 0.027(2) 0.035(3) 0.082(4) -0.005(2) 0.002(2) 0.0023(19) C24B 0.027(2) 0.067(4) 0.114(5) 0.029(4) 0.007(3) 0.002(3) C25B 0.025(2) 0.065(4) 0.127(6) 0.033(4) 0.009(3) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag CoA O4A 1.990(3) . ? CoA O5A 2.061(3) . ? CoA O1A 2.090(3) . ? CoA N2A 2.135(3) . ? CoA \~N1A 2.157(3) . ? CoA O2A 2.403(3) . ? O1A C3A 1.252(5) . ? O2A C3A 1.253(5) . ? C3A C9A 1.486(5) 2 ? O4A C6A 1.244(4) 3 ? O5A C6A 1.256(5) . ? C6A O4A 1.244(4) 3 ? C6A C7A 1.469(5) . ? C7A C11A 1.345(6) . ? C7A O8A 1.369(4) . ? O8A C9A 1.371(5) . ? C9A C10A 1.351(6) . ? C9A C3A 1.486(5) 2_545 ? C10A C11A 1.420(6) . ? C10A H10A 0.9300 . ? C11A H11A 0.9300 . ? \~N1A C13A 1.326(6) . ? \~N1A C24A 1.334(6) 1_655 ? C13A C23A 1.375(6) 1_655 ? C13A H13A 0.9300 . ? N2A C15A 1.332(5) . ? N2A C19A 1.338(5) . ? C15A C16A 1.401(6) . ? C15A H15A 0.9300 . ? C16A C17A 1.383(7) . ? C17A C18A 1.396(7) . ? C17A C20A 1.498(6) . ? C18A C19A 1.379(6) . ? C18A H18A 0.9300 . ? C19A H19A 0.9300 . ? C20A C21A 1.488(6) . ? C20A H20A 0.9700 . ? C20A H20B 0.9700 . ? C21A C22A 1.517(6) . ? C21A H21A 0.9700 . ? C21A H21B 0.9700 . ? C22A C23A 1.369(6) . ? C22A C25A 1.381(7) . ? C23A C13A 1.375(6) 1_455 ? C23A H23A 0.9300 . ? C24A \~N1A 1.334(6) 1_455 ? C24A C25A 1.373(7) . ? C25A H25A 0.9300 . ? CoB O5B 2.006(3) . ? CoB O4B 2.068(3) . ? CoB O1B 2.110(3) . ? CoB N2B 2.123(3) . ? CoB N1B 2.159(3) . ? O1B C3B 1.266(5) . ? O2B C3B 1.249(5) . ? C3B C9B 1.483(5) 4_566 ? O4B C6B 1.261(4) 3_665 ? O5B C6B 1.243(4) . ? C6B O4B 1.261(4) 3_665 ? C6B C7B 1.480(5) . ? C7B C11B 1.349(6) . ? C7B O8B 1.368(4) . ? O8B C9B 1.368(4) . ? C9B C10B 1.347(6) . ? C9B C3B 1.483(5) 4_565 ? C10B C11B 1.424(6) . ? C10B H10B 0.9300 . ? C11B H11B 0.9300 . ? N2B C13B 1.327(5) . ? N2B C17B 1.332(5) . ? C13B C14B 1.378(6) . ? C13B H13B 0.9300 . ? C14B C15B 1.382(7) . ? C14B H14B 0.9300 . ? C15B C16B 1.377(7) . ? C15B C25B 1.510(6) 1_655 ? C16B C17B 1.390(6) . ? C16B H16B 0.9300 . ? C17B H17B 0.9300 . ? N1B C19B 1.327(6) . ? N1B C23B 1.332(6) . ? C19B C20B 1.375(6) . ? C19B H19B 0.9300 . ? C20B C21B 1.376(6) . ? C20B H20C 0.9300 . ? C21B C22B 1.387(6) . ? C21B C24B 1.516(7) . ? C22B C23B 1.372(6) . ? C22B H22B 0.9300 . ? C23B H23B 0.9300 . ? C24B C25B 1.437(7) . ? C24B H24A 0.9700 . ? C24B H24B 0.9700 . ? C25B C15B 1.510(6) 1_455 ? C25B H25B 0.9700 . ? C25B H25C 0.9700 . ? 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 O4A CoA O5A 107.47(12) . . ? O4A CoA O1A 156.82(13) . . ? O5A CoA O1A 95.70(11) . . ? O4A CoA N2A 88.46(14) . . ? O5A CoA N2A 90.55(12) . . ? O1A CoA N2A 90.79(13) . . ? O4A CoA \~N1A 89.96(15) . . ? O5A CoA \~N1A 94.24(13) . . ? O1A CoA \~N1A 88.89(13) . . ? N2A CoA \~N1A 175.21(13) . . ? O4A CoA O2A 98.65(12) . . ? O5A CoA O2A 153.38(10) . . ? O1A CoA O2A 58.22(11) . . ? N2A CoA O2A 85.03(12) . . ? \~N1A CoA O2A 90.75(12) . . ? C3A O1A CoA 96.5(2) . . ? C3A O2A CoA 82.2(2) . . ? O1A C3A O2A 123.1(4) . . ? O1A C3A C9A 115.6(4) . 2 ? O2A C3A C9A 121.3(4) . 2 ? C6A O4A CoA 171.9(3) 3 . ? C6A O5A CoA 124.9(2) . . ? O4A C6A O5A 125.3(4) 3 . ? O4A C6A C7A 115.1(3) 3 . ? O5A C6A C7A 119.6(3) . . ? C11A C7A O8A 110.6(3) . . ? C11A C7A C6A 129.9(4) . . ? O8A C7A C6A 119.4(3) . . ? C7A O8A C9A 106.1(3) . . ? C10A C9A O8A 110.2(3) . . ? C10A C9A C3A 130.7(4) . 2_545 ? O8A C9A C3A 119.0(3) . 2_545 ? C9A C10A C11A 106.6(4) . . ? C9A C10A H10A 126.7 . . ? C11A C10A H10A 126.7 . . ? C7A C11A C10A 106.6(4) . . ? C7A C11A H11A 126.7 . . ? C10A C11A H11A 126.7 . . ? C13A \~N1A C24A 115.9(4) . 1_655 ? C13A \~N1A CoA 124.5(3) . . ? C24A \~N1A CoA 119.6(3) 1_655 . ? \~N1A C13A C23A 124.4(4) . 1_655 ? \~N1A C13A H13A 117.8 . . ? C23A C13A H13A 117.8 1_655 . ? C15A N2A C19A 116.1(4) . . ? C15A N2A CoA 120.5(3) . . ? C19A N2A CoA 123.4(3) . . ? N2A C15A C16A 124.0(4) . . ? N2A C15A H15A 118.0 . . ? C16A C15A H15A 118.0 . . ? C17A C16A C15A 119.3(4) . . ? C16A C17A C18A 116.7(4) . . ? C16A C17A C20A 121.7(4) . . ? C18A C17A C20A 121.6(4) . . ? C19A C18A C17A 119.8(4) . . ? C19A C18A H18A 120.1 . . ? C17A C18A H18A 120.1 . . ? N2A C19A C18A 124.0(4) . . ? N2A C19A H19A 118.0 . . ? C18A C19A H19A 118.0 . . ? C21A C20A C17A 111.3(4) . . ? C21A C20A H20A 109.4 . . ? C17A C20A H20A 109.4 . . ? C21A C20A H20B 109.4 . . ? C17A C20A H20B 109.4 . . ? H20A C20A H20B 108.0 . . ? C20A C21A C22A 116.1(4) . . ? C20A C21A H21A 108.3 . . ? C22A C21A H21A 108.3 . . ? C20A C21A H21B 108.3 . . ? C22A C21A H21B 108.3 . . ? H21A C21A H21B 107.4 . . ? C23A C22A C25A 115.8(4) . . ? C23A C22A C21A 124.4(4) . . ? C25A C22A C21A 119.9(4) . . ? C22A C23A C13A 120.0(4) . 1_455 ? C22A C23A H23A 120.0 . . ? C13A C23A H23A 120.0 1_455 . ? \~N1A C24A C25A 122.8(5) 1_455 . ? C24A C25A C22A 121.1(5) . . ? C24A C25A H25A 119.5 . . ? C22A C25A H25A 119.5 . . ? O5B CoB O4B 108.79(12) . . ? O5B CoB O1B 154.05(12) . . ? O4B CoB O1B 96.59(11) . . ? O5B CoB N2B 92.64(13) . . ? O4B CoB N2B 91.69(12) . . ? O1B CoB N2B 91.89(12) . . ? O5B CoB N1B 86.56(13) . . ? O4B CoB N1B 92.99(12) . . ? O1B CoB N1B 86.83(12) . . ? N2B CoB N1B 175.26(13) . . ? C3B O1B CoB 96.6(2) . . ? O2B C3B O1B 122.9(4) . . ? O2B C3B C9B 121.3(4) . 4_566 ? O1B C3B C9B 115.7(4) . 4_566 ? C6B O4B CoB 124.8(2) 3_665 . ? C6B O5B CoB 161.0(3) . . ? O5B C6B O4B 126.4(4) . 3_665 ? O5B C6B C7B 114.9(3) . . ? O4B C6B C7B 118.7(3) 3_665 . ? C11B C7B O8B 110.4(3) . . ? C11B C7B C6B 129.5(4) . . ? O8B C7B C6B 120.1(3) . . ? C9B O8B C7B 106.3(3) . . ? C10B C9B O8B 110.3(3) . . ? C10B C9B C3B 130.6(4) . 4_565 ? O8B C9B C3B 119.2(3) . 4_565 ? C9B C10B C11B 106.7(4) . . ? C9B C10B H10B 126.7 . . ? C11B C10B H10B 126.7 . . ? C7B C11B C10B 106.3(4) . . ? C7B C11B H11B 126.8 . . ? C10B C11B H11B 126.8 . . ? C13B N2B C17B 116.6(4) . . ? C13B N2B CoB 121.8(3) . . ? C17B N2B CoB 121.5(3) . . ? N2B C13B C14B 123.9(4) . . ? N2B C13B H13B 118.0 . . ? C14B C13B H13B 118.0 . . ? C13B C14B C15B 119.7(5) . . ? C13B C14B H14B 120.2 . . ? C15B C14B H14B 120.2 . . ? C16B C15B C14B 116.7(4) . . ? C16B C15B C25B 122.5(5) . 1_655 ? C14B C15B C25B 120.8(5) . 1_655 ? C15B C16B C17B 120.0(4) . . ? C15B C16B H16B 120.0 . . ? C17B C16B H16B 120.0 . . ? N2B C17B C16B 123.0(4) . . ? N2B C17B H17B 118.5 . . ? C16B C17B H17B 118.5 . . ? C19B N1B C23B 115.9(4) . . ? C19B N1B CoB 121.2(3) . . ? C23B N1B CoB 122.8(3) . . ? N1B C19B C20B 123.3(4) . . ? N1B C19B H19B 118.3 . . ? C20B C19B H19B 118.3 . . ? C19B C20B C21B 120.8(5) . . ? C19B C20B H20C 119.6 . . ? C21B C20B H20C 119.6 . . ? C20B C21B C22B 116.1(4) . . ? C20B C21B C24B 119.3(4) . . ? C22B C21B C24B 124.6(4) . . ? C23B C22B C21B 119.4(4) . . ? C23B C22B H22B 120.3 . . ? C21B C22B H22B 120.3 . . ? N1B C23B C22B 124.5(5) . . ? N1B C23B H23B 117.8 . . ? C22B C23B H23B 117.8 . . ? C25B C24B C21B 118.0(5) . . ? C25B C24B H24A 107.8 . . ? C21B C24B H24A 107.8 . . ? C25B C24B H24B 107.8 . . ? C21B C24B H24B 107.8 . . ? H24A C24B H24B 107.2 . . ? C24B C25B C15B 112.6(5) . 1_455 ? C24B C25B H25B 109.1 . . ? C15B C25B H25B 109.1 1_455 . ? C24B C25B H25C 109.1 . . ? C15B C25B H25C 109.1 1_455 . ? H25B C25B H25C 107.8 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.90 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.558 _refine_diff_density_min -0.501 _refine_diff_density_rms 0.133 data_rz97_no_w _database_code_depnum_ccdc_archive 'CCDC 894679' #TrackingRef 'web_deposit_cif_file_1_ZhiLin_1343932406.Rupam CEC compound 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H12 N2 Ni O5' _chemical_formula_weight 395.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 17.1691(4) _cell_length_b 13.5523(4) _cell_length_c 15.4503(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3594.99(18) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 1.110 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6069 _exptl_absorpt_correction_T_max 0.9570 _exptl_absorpt_process_details SADABS _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 17127 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 27.11 _reflns_number_total 3966 _reflns_number_gt 3153 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1183P)^2^+8.2227P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3966 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0729 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.2263 _refine_ls_wR_factor_gt 0.2131 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.157 _refine_ls_shift/su_max 0.027 _refine_ls_shift/su_mean 0.005 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.43593(3) 0.02523(4) 0.12260(4) 0.0264(2) Uani 1 1 d . . . O4 O 0.55348(18) 0.0157(3) 0.1400(2) 0.0338(7) Uani 1 1 d . . . C2 C 0.5981(2) -0.0139(3) 0.0813(3) 0.0282(9) Uani 1 1 d . . . C3 C 0.6815(3) -0.0304(4) 0.1017(3) 0.0327(10) Uani 1 1 d . . . O5 O 0.70922(17) -0.0180(2) 0.1841(2) 0.0305(7) Uani 1 1 d . . . C5 C 0.7881(3) -0.0344(4) 0.1795(3) 0.0357(11) Uani 1 1 d . . . C6 C 0.8094(3) -0.0553(6) 0.0969(4) 0.0547(16) Uani 1 1 d . . . H6 H 0.8595 -0.0683 0.0770 0.066 Uiso 1 1 calc R . . C7 C 0.7401(3) -0.0534(5) 0.0470(3) 0.0508(15) Uani 1 1 d . . . H7 H 0.7358 -0.0656 -0.0120 0.061 Uiso 1 1 calc R . . O3 O 0.4199(2) 0.0343(3) -0.0063(2) 0.0508(10) Uani 1 1 d . . . O1 O 0.40838(19) 0.0286(3) 0.2528(2) 0.0389(8) Uani 1 1 d . . . O2 O 0.30519(19) 0.0248(2) 0.1675(2) 0.0360(7) Uani 1 1 d . . . C11 C 0.3351(3) 0.0286(3) 0.2408(3) 0.0334(10) Uani 1 1 d . . . N2 N 0.4373(2) 0.1801(3) 0.1204(3) 0.0367(9) Uani 1 1 d . . . C13 C 0.5022(3) 0.2297(4) 0.1045(5) 0.0643(19) Uani 1 1 d . . . H13 H 0.5473 0.1937 0.0935 0.077 Uiso 1 1 calc R . . C14 C 0.5073(4) 0.3298(5) 0.1033(5) 0.069(2) Uani 1 1 d . . . H14 H 0.5551 0.3596 0.0923 0.083 Uiso 1 1 calc R . . C15 C 0.4428(3) 0.3876(4) 0.1179(3) 0.0401(12) Uani 1 1 d . . . C16 C 0.3744(3) 0.3373(4) 0.1339(4) 0.0551(16) Uani 1 1 d . . . H16 H 0.3284 0.3720 0.1432 0.066 Uiso 1 1 calc R . . C17 C 0.3744(3) 0.2356(4) 0.1363(5) 0.0567(17) Uani 1 1 d . . . H17 H 0.3280 0.2037 0.1498 0.068 Uiso 1 1 calc R . . C18 C 0.4504(3) 0.4957(4) 0.1182(4) 0.0455(13) Uani 1 1 d . . . H18 H 0.5007 0.5211 0.1202 0.055 Uiso 1 1 calc R . . C19 C 0.3936(3) 0.5594(4) 0.1160(4) 0.0495(14) Uani 1 1 d . . . H19 H 0.3428 0.5357 0.1131 0.059 Uiso 1 1 calc R . . C20 C 0.4055(3) 0.6659(4) 0.1177(4) 0.0451(13) Uani 1 1 d . . . C21 C 0.4692(3) 0.7106(4) 0.1591(4) 0.0473(13) Uani 1 1 d . . . H21 H 0.5065 0.6720 0.1867 0.057 Uiso 1 1 calc R . . C22 C 0.3535(3) 0.7292(4) 0.0760(5) 0.0604(18) Uani 1 1 d . . . H22 H 0.3108 0.7038 0.0465 0.072 Uiso 1 1 calc R . . N1 N 0.4257(2) -0.1275(3) 0.1196(3) 0.0349(9) Uani 1 1 d . . . C24 C 0.4763(3) -0.1878(4) 0.1586(4) 0.0445(12) Uani 1 1 d . . . H24 H 0.5187 -0.1598 0.1870 0.053 Uiso 1 1 calc R . . C25 C 0.3661(3) -0.1700(4) 0.0787(4) 0.0510(14) Uani 1 1 d . . . H25 H 0.3307 -0.1294 0.0503 0.061 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0222(3) 0.0270(4) 0.0302(4) -0.0020(2) 0.00014(19) 0.0011(2) O4 0.0231(15) 0.0397(19) 0.0386(17) -0.0079(14) -0.0005(13) 0.0027(13) C2 0.022(2) 0.030(2) 0.032(2) 0.0025(18) -0.0014(16) -0.0005(16) C3 0.024(2) 0.047(3) 0.027(2) -0.0002(19) -0.0044(17) 0.0034(18) O5 0.0209(14) 0.0404(17) 0.0302(16) -0.0012(13) -0.0022(12) 0.0026(12) C5 0.021(2) 0.046(3) 0.040(3) 0.001(2) -0.0040(18) 0.0049(18) C6 0.026(2) 0.101(5) 0.037(3) -0.006(3) -0.001(2) 0.012(3) C7 0.030(3) 0.088(4) 0.034(3) -0.010(3) -0.002(2) 0.014(3) O3 0.0362(19) 0.084(3) 0.0323(19) -0.0041(18) -0.0105(15) 0.0095(19) O1 0.0232(15) 0.054(2) 0.0399(18) -0.0018(16) 0.0068(14) -0.0013(14) O2 0.0314(16) 0.0429(19) 0.0337(17) -0.0003(14) 0.0030(13) 0.0029(14) C11 0.028(2) 0.035(2) 0.037(2) 0.003(2) 0.0057(18) -0.0004(18) N2 0.037(2) 0.0267(19) 0.046(2) 0.0013(17) 0.0027(17) 0.0005(16) C13 0.044(3) 0.033(3) 0.116(6) 0.002(3) 0.030(3) 0.001(2) C14 0.044(3) 0.036(3) 0.127(6) 0.007(4) 0.026(4) -0.002(2) C15 0.045(3) 0.029(2) 0.046(3) 0.003(2) -0.003(2) -0.003(2) C16 0.036(3) 0.033(3) 0.096(5) 0.002(3) -0.002(3) 0.005(2) C17 0.032(3) 0.035(3) 0.103(5) 0.012(3) 0.001(3) 0.001(2) C18 0.041(3) 0.031(2) 0.065(4) 0.001(2) -0.004(2) -0.004(2) C19 0.042(3) 0.036(3) 0.071(4) -0.001(3) -0.011(3) 0.000(2) C20 0.042(3) 0.030(2) 0.063(4) -0.007(2) -0.002(2) 0.000(2) C21 0.046(3) 0.029(2) 0.067(4) 0.003(2) -0.016(3) 0.003(2) C22 0.045(3) 0.033(3) 0.103(5) -0.010(3) -0.026(3) -0.002(2) N1 0.034(2) 0.0221(18) 0.049(2) -0.0030(16) -0.0035(16) 0.0009(15) C24 0.044(3) 0.033(3) 0.056(3) -0.002(2) -0.014(2) -0.003(2) C25 0.040(3) 0.032(3) 0.081(4) -0.002(3) -0.018(3) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O3 2.014(4) . ? Ni1 O4 2.040(3) . ? Ni1 O1 2.067(4) . ? Ni1 N1 2.077(4) . ? Ni1 N2 2.099(4) . ? Ni1 O2 2.350(3) . ? Ni1 C11 2.516(5) . ? O4 C2 1.253(5) . ? C2 O3 1.232(6) 5_655 ? C2 C3 1.484(6) . ? C3 C7 1.350(7) . ? C3 O5 1.370(5) . ? O5 C5 1.374(5) . ? C5 C6 1.358(7) . ? C5 C11 1.475(6) 4 ? C6 C7 1.418(7) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? O3 C2 1.232(6) 5_655 ? O1 C11 1.271(6) . ? O2 C11 1.244(6) . ? C11 C5 1.475(6) 4_455 ? N2 C13 1.325(7) . ? N2 C17 1.339(7) . ? C13 C14 1.359(8) . ? C13 H13 0.9300 . ? C14 C15 1.375(8) . ? C14 H14 0.9300 . ? C15 C16 1.380(7) . ? C15 C18 1.471(7) . ? C16 C17 1.379(8) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.303(8) . ? C18 H18 0.9300 . ? C19 C20 1.459(8) . ? C19 H19 0.9300 . ? C20 C22 1.396(8) . ? C20 C21 1.405(7) . ? C21 C24 1.382(7) 1_565 ? C21 H21 0.9300 . ? C22 C25 1.383(8) 1_565 ? C22 H22 0.9300 . ? N1 C25 1.334(6) . ? N1 C24 1.337(6) . ? C24 C21 1.382(7) 1_545 ? C24 H24 0.9300 . ? C25 C22 1.383(8) 1_545 ? C25 H25 0.9300 . ? 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 O3 Ni1 O4 105.62(15) . . ? O3 Ni1 O1 158.38(15) . . ? O4 Ni1 O1 95.71(14) . . ? O3 Ni1 N1 91.59(17) . . ? O4 Ni1 N1 91.37(14) . . ? O1 Ni1 N1 91.38(15) . . ? O3 Ni1 N2 85.64(17) . . ? O4 Ni1 N2 93.12(14) . . ? O1 Ni1 N2 89.79(15) . . ? N1 Ni1 N2 175.22(16) . . ? O3 Ni1 O2 99.32(14) . . ? O4 Ni1 O2 154.96(13) . . ? O1 Ni1 O2 59.59(12) . . ? N1 Ni1 O2 85.59(14) . . ? N2 Ni1 O2 91.01(13) . . ? O3 Ni1 C11 128.51(16) . . ? O4 Ni1 C11 125.86(15) . . ? O1 Ni1 C11 30.22(15) . . ? N1 Ni1 C11 88.61(15) . . ? N2 Ni1 C11 90.07(15) . . ? O2 Ni1 C11 29.38(14) . . ? C2 O4 Ni1 122.0(3) . . ? O3 C2 O4 126.8(4) 5_655 . ? O3 C2 C3 114.1(4) 5_655 . ? O4 C2 C3 119.0(4) . . ? C7 C3 O5 110.6(4) . . ? C7 C3 C2 128.4(4) . . ? O5 C3 C2 120.9(4) . . ? C3 O5 C5 105.9(4) . . ? C6 C5 O5 110.4(4) . . ? C6 C5 C11 130.4(4) . 4 ? O5 C5 C11 119.2(4) . 4 ? C5 C6 C7 106.3(4) . . ? C5 C6 H6 126.8 . . ? C7 C6 H6 126.8 . . ? C3 C7 C6 106.8(5) . . ? C3 C7 H7 126.6 . . ? C6 C7 H7 126.6 . . ? C2 O3 Ni1 162.1(4) 5_655 . ? C11 O1 Ni1 94.9(3) . . ? C11 O2 Ni1 82.7(3) . . ? O2 C11 O1 122.8(4) . . ? O2 C11 C5 122.4(4) . 4_455 ? O1 C11 C5 114.9(4) . 4_455 ? O2 C11 Ni1 67.9(3) . . ? O1 C11 Ni1 54.9(2) . . ? C5 C11 Ni1 169.6(3) 4_455 . ? C13 N2 C17 115.3(5) . . ? C13 N2 Ni1 121.3(4) . . ? C17 N2 Ni1 123.4(3) . . ? N2 C13 C14 124.2(6) . . ? N2 C13 H13 117.9 . . ? C14 C13 H13 117.9 . . ? C13 C14 C15 121.0(6) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C14 C15 C16 115.7(5) . . ? C14 C15 C18 119.8(5) . . ? C16 C15 C18 124.5(5) . . ? C17 C16 C15 119.9(5) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? N2 C17 C16 123.8(5) . . ? N2 C17 H17 118.1 . . ? C16 C17 H17 118.1 . . ? C19 C18 C15 126.4(6) . . ? C19 C18 H18 116.8 . . ? C15 C18 H18 116.8 . . ? C18 C19 C20 123.3(5) . . ? C18 C19 H19 118.3 . . ? C20 C19 H19 118.3 . . ? C22 C20 C21 116.3(5) . . ? C22 C20 C19 120.7(5) . . ? C21 C20 C19 123.0(5) . . ? C24 C21 C20 119.8(5) 1_565 . ? C24 C21 H21 120.1 1_565 . ? C20 C21 H21 120.1 . . ? C25 C22 C20 119.6(5) 1_565 . ? C25 C22 H22 120.2 1_565 . ? C20 C22 H22 120.2 . . ? C25 N1 C24 116.6(4) . . ? C25 N1 Ni1 120.4(3) . . ? C24 N1 Ni1 122.9(3) . . ? N1 C24 C21 123.6(5) . 1_545 ? N1 C24 H24 118.2 . . ? C21 C24 H24 118.2 1_545 . ? N1 C25 C22 124.1(5) . 1_545 ? N1 C25 H25 118.0 . . ? C22 C25 H25 118.0 1_545 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.11 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.451 _refine_diff_density_min -0.283 _refine_diff_density_rms 0.136 data_rz97_no_w _database_code_depnum_ccdc_archive 'CCDC 894680' #TrackingRef 'web_deposit_cif_file_1_ZhiLin_1343932406.Rupam CEC compound 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H12 N2 Ni O5' _chemical_formula_weight 395.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 17.1691(4) _cell_length_b 13.5523(4) _cell_length_c 15.4503(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3594.99(18) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 1.110 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6069 _exptl_absorpt_correction_T_max 0.9570 _exptl_absorpt_process_details SADABS _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 17127 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 27.11 _reflns_number_total 3966 _reflns_number_gt 3153 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1183P)^2^+8.2227P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3966 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0729 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.2263 _refine_ls_wR_factor_gt 0.2131 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.157 _refine_ls_shift/su_max 0.027 _refine_ls_shift/su_mean 0.005 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.43593(3) 0.02523(4) 0.12260(4) 0.0264(2) Uani 1 1 d . . . O4 O 0.55348(18) 0.0157(3) 0.1400(2) 0.0338(7) Uani 1 1 d . . . C2 C 0.5981(2) -0.0139(3) 0.0813(3) 0.0282(9) Uani 1 1 d . . . C3 C 0.6815(3) -0.0304(4) 0.1017(3) 0.0327(10) Uani 1 1 d . . . O5 O 0.70922(17) -0.0180(2) 0.1841(2) 0.0305(7) Uani 1 1 d . . . C5 C 0.7881(3) -0.0344(4) 0.1795(3) 0.0357(11) Uani 1 1 d . . . C6 C 0.8094(3) -0.0553(6) 0.0969(4) 0.0547(16) Uani 1 1 d . . . H6 H 0.8595 -0.0683 0.0770 0.066 Uiso 1 1 calc R . . C7 C 0.7401(3) -0.0534(5) 0.0470(3) 0.0508(15) Uani 1 1 d . . . H7 H 0.7358 -0.0656 -0.0120 0.061 Uiso 1 1 calc R . . O3 O 0.4199(2) 0.0343(3) -0.0063(2) 0.0508(10) Uani 1 1 d . . . O1 O 0.40838(19) 0.0286(3) 0.2528(2) 0.0389(8) Uani 1 1 d . . . O2 O 0.30519(19) 0.0248(2) 0.1675(2) 0.0360(7) Uani 1 1 d . . . C11 C 0.3351(3) 0.0286(3) 0.2408(3) 0.0334(10) Uani 1 1 d . . . N2 N 0.4373(2) 0.1801(3) 0.1204(3) 0.0367(9) Uani 1 1 d . . . C13 C 0.5022(3) 0.2297(4) 0.1045(5) 0.0643(19) Uani 1 1 d . . . H13 H 0.5473 0.1937 0.0935 0.077 Uiso 1 1 calc R . . C14 C 0.5073(4) 0.3298(5) 0.1033(5) 0.069(2) Uani 1 1 d . . . H14 H 0.5551 0.3596 0.0923 0.083 Uiso 1 1 calc R . . C15 C 0.4428(3) 0.3876(4) 0.1179(3) 0.0401(12) Uani 1 1 d . . . C16 C 0.3744(3) 0.3373(4) 0.1339(4) 0.0551(16) Uani 1 1 d . . . H16 H 0.3284 0.3720 0.1432 0.066 Uiso 1 1 calc R . . C17 C 0.3744(3) 0.2356(4) 0.1363(5) 0.0567(17) Uani 1 1 d . . . H17 H 0.3280 0.2037 0.1498 0.068 Uiso 1 1 calc R . . C18 C 0.4504(3) 0.4957(4) 0.1182(4) 0.0455(13) Uani 1 1 d . . . H18 H 0.5007 0.5211 0.1202 0.055 Uiso 1 1 calc R . . C19 C 0.3936(3) 0.5594(4) 0.1160(4) 0.0495(14) Uani 1 1 d . . . H19 H 0.3428 0.5357 0.1131 0.059 Uiso 1 1 calc R . . C20 C 0.4055(3) 0.6659(4) 0.1177(4) 0.0451(13) Uani 1 1 d . . . C21 C 0.4692(3) 0.7106(4) 0.1591(4) 0.0473(13) Uani 1 1 d . . . H21 H 0.5065 0.6720 0.1867 0.057 Uiso 1 1 calc R . . C22 C 0.3535(3) 0.7292(4) 0.0760(5) 0.0604(18) Uani 1 1 d . . . H22 H 0.3108 0.7038 0.0465 0.072 Uiso 1 1 calc R . . N1 N 0.4257(2) -0.1275(3) 0.1196(3) 0.0349(9) Uani 1 1 d . . . C24 C 0.4763(3) -0.1878(4) 0.1586(4) 0.0445(12) Uani 1 1 d . . . H24 H 0.5187 -0.1598 0.1870 0.053 Uiso 1 1 calc R . . C25 C 0.3661(3) -0.1700(4) 0.0787(4) 0.0510(14) Uani 1 1 d . . . H25 H 0.3307 -0.1294 0.0503 0.061 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0222(3) 0.0270(4) 0.0302(4) -0.0020(2) 0.00014(19) 0.0011(2) O4 0.0231(15) 0.0397(19) 0.0386(17) -0.0079(14) -0.0005(13) 0.0027(13) C2 0.022(2) 0.030(2) 0.032(2) 0.0025(18) -0.0014(16) -0.0005(16) C3 0.024(2) 0.047(3) 0.027(2) -0.0002(19) -0.0044(17) 0.0034(18) O5 0.0209(14) 0.0404(17) 0.0302(16) -0.0012(13) -0.0022(12) 0.0026(12) C5 0.021(2) 0.046(3) 0.040(3) 0.001(2) -0.0040(18) 0.0049(18) C6 0.026(2) 0.101(5) 0.037(3) -0.006(3) -0.001(2) 0.012(3) C7 0.030(3) 0.088(4) 0.034(3) -0.010(3) -0.002(2) 0.014(3) O3 0.0362(19) 0.084(3) 0.0323(19) -0.0041(18) -0.0105(15) 0.0095(19) O1 0.0232(15) 0.054(2) 0.0399(18) -0.0018(16) 0.0068(14) -0.0013(14) O2 0.0314(16) 0.0429(19) 0.0337(17) -0.0003(14) 0.0030(13) 0.0029(14) C11 0.028(2) 0.035(2) 0.037(2) 0.003(2) 0.0057(18) -0.0004(18) N2 0.037(2) 0.0267(19) 0.046(2) 0.0013(17) 0.0027(17) 0.0005(16) C13 0.044(3) 0.033(3) 0.116(6) 0.002(3) 0.030(3) 0.001(2) C14 0.044(3) 0.036(3) 0.127(6) 0.007(4) 0.026(4) -0.002(2) C15 0.045(3) 0.029(2) 0.046(3) 0.003(2) -0.003(2) -0.003(2) C16 0.036(3) 0.033(3) 0.096(5) 0.002(3) -0.002(3) 0.005(2) C17 0.032(3) 0.035(3) 0.103(5) 0.012(3) 0.001(3) 0.001(2) C18 0.041(3) 0.031(2) 0.065(4) 0.001(2) -0.004(2) -0.004(2) C19 0.042(3) 0.036(3) 0.071(4) -0.001(3) -0.011(3) 0.000(2) C20 0.042(3) 0.030(2) 0.063(4) -0.007(2) -0.002(2) 0.000(2) C21 0.046(3) 0.029(2) 0.067(4) 0.003(2) -0.016(3) 0.003(2) C22 0.045(3) 0.033(3) 0.103(5) -0.010(3) -0.026(3) -0.002(2) N1 0.034(2) 0.0221(18) 0.049(2) -0.0030(16) -0.0035(16) 0.0009(15) C24 0.044(3) 0.033(3) 0.056(3) -0.002(2) -0.014(2) -0.003(2) C25 0.040(3) 0.032(3) 0.081(4) -0.002(3) -0.018(3) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O3 2.014(4) . ? Ni1 O4 2.040(3) . ? Ni1 O1 2.067(4) . ? Ni1 N1 2.077(4) . ? Ni1 N2 2.099(4) . ? Ni1 O2 2.350(3) . ? Ni1 C11 2.516(5) . ? O4 C2 1.253(5) . ? C2 O3 1.232(6) 5_655 ? C2 C3 1.484(6) . ? C3 C7 1.350(7) . ? C3 O5 1.370(5) . ? O5 C5 1.374(5) . ? C5 C6 1.358(7) . ? C5 C11 1.475(6) 4 ? C6 C7 1.418(7) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? O3 C2 1.232(6) 5_655 ? O1 C11 1.271(6) . ? O2 C11 1.244(6) . ? C11 C5 1.475(6) 4_455 ? N2 C13 1.325(7) . ? N2 C17 1.339(7) . ? C13 C14 1.359(8) . ? C13 H13 0.9300 . ? C14 C15 1.375(8) . ? C14 H14 0.9300 . ? C15 C16 1.380(7) . ? C15 C18 1.471(7) . ? C16 C17 1.379(8) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.303(8) . ? C18 H18 0.9300 . ? C19 C20 1.459(8) . ? C19 H19 0.9300 . ? C20 C22 1.396(8) . ? C20 C21 1.405(7) . ? C21 C24 1.382(7) 1_565 ? C21 H21 0.9300 . ? C22 C25 1.383(8) 1_565 ? C22 H22 0.9300 . ? N1 C25 1.334(6) . ? N1 C24 1.337(6) . ? C24 C21 1.382(7) 1_545 ? C24 H24 0.9300 . ? C25 C22 1.383(8) 1_545 ? C25 H25 0.9300 . ? 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 O3 Ni1 O4 105.62(15) . . ? O3 Ni1 O1 158.38(15) . . ? O4 Ni1 O1 95.71(14) . . ? O3 Ni1 N1 91.59(17) . . ? O4 Ni1 N1 91.37(14) . . ? O1 Ni1 N1 91.38(15) . . ? O3 Ni1 N2 85.64(17) . . ? O4 Ni1 N2 93.12(14) . . ? O1 Ni1 N2 89.79(15) . . ? N1 Ni1 N2 175.22(16) . . ? O3 Ni1 O2 99.32(14) . . ? O4 Ni1 O2 154.96(13) . . ? O1 Ni1 O2 59.59(12) . . ? N1 Ni1 O2 85.59(14) . . ? N2 Ni1 O2 91.01(13) . . ? O3 Ni1 C11 128.51(16) . . ? O4 Ni1 C11 125.86(15) . . ? O1 Ni1 C11 30.22(15) . . ? N1 Ni1 C11 88.61(15) . . ? N2 Ni1 C11 90.07(15) . . ? O2 Ni1 C11 29.38(14) . . ? C2 O4 Ni1 122.0(3) . . ? O3 C2 O4 126.8(4) 5_655 . ? O3 C2 C3 114.1(4) 5_655 . ? O4 C2 C3 119.0(4) . . ? C7 C3 O5 110.6(4) . . ? C7 C3 C2 128.4(4) . . ? O5 C3 C2 120.9(4) . . ? C3 O5 C5 105.9(4) . . ? C6 C5 O5 110.4(4) . . ? C6 C5 C11 130.4(4) . 4 ? O5 C5 C11 119.2(4) . 4 ? C5 C6 C7 106.3(4) . . ? C5 C6 H6 126.8 . . ? C7 C6 H6 126.8 . . ? C3 C7 C6 106.8(5) . . ? C3 C7 H7 126.6 . . ? C6 C7 H7 126.6 . . ? C2 O3 Ni1 162.1(4) 5_655 . ? C11 O1 Ni1 94.9(3) . . ? C11 O2 Ni1 82.7(3) . . ? O2 C11 O1 122.8(4) . . ? O2 C11 C5 122.4(4) . 4_455 ? O1 C11 C5 114.9(4) . 4_455 ? O2 C11 Ni1 67.9(3) . . ? O1 C11 Ni1 54.9(2) . . ? C5 C11 Ni1 169.6(3) 4_455 . ? C13 N2 C17 115.3(5) . . ? C13 N2 Ni1 121.3(4) . . ? C17 N2 Ni1 123.4(3) . . ? N2 C13 C14 124.2(6) . . ? N2 C13 H13 117.9 . . ? C14 C13 H13 117.9 . . ? C13 C14 C15 121.0(6) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C14 C15 C16 115.7(5) . . ? C14 C15 C18 119.8(5) . . ? C16 C15 C18 124.5(5) . . ? C17 C16 C15 119.9(5) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? N2 C17 C16 123.8(5) . . ? N2 C17 H17 118.1 . . ? C16 C17 H17 118.1 . . ? C19 C18 C15 126.4(6) . . ? C19 C18 H18 116.8 . . ? C15 C18 H18 116.8 . . ? C18 C19 C20 123.3(5) . . ? C18 C19 H19 118.3 . . ? C20 C19 H19 118.3 . . ? C22 C20 C21 116.3(5) . . ? C22 C20 C19 120.7(5) . . ? C21 C20 C19 123.0(5) . . ? C24 C21 C20 119.8(5) 1_565 . ? C24 C21 H21 120.1 1_565 . ? C20 C21 H21 120.1 . . ? C25 C22 C20 119.6(5) 1_565 . ? C25 C22 H22 120.2 1_565 . ? C20 C22 H22 120.2 . . ? C25 N1 C24 116.6(4) . . ? C25 N1 Ni1 120.4(3) . . ? C24 N1 Ni1 122.9(3) . . ? N1 C24 C21 123.6(5) . 1_545 ? N1 C24 H24 118.2 . . ? C21 C24 H24 118.2 1_545 . ? N1 C25 C22 124.1(5) . 1_545 ? N1 C25 H25 118.0 . . ? C22 C25 H25 118.0 1_545 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.11 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.451 _refine_diff_density_min -0.283 _refine_diff_density_rms 0.136 data_f2 _database_code_depnum_ccdc_archive 'CCDC 894681' #TrackingRef 'web_deposit_cif_file_5_ZhiLin_1343932406.Rupam CEC compound 6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H63 O64 Zn8' _chemical_formula_weight 2186.94 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Pn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 22.1775(5) _cell_length_b 7.3566(2) _cell_length_c 22.1781(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.0890(10) _cell_angle_gamma 90.00 _cell_volume 3609.17(15) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour Colouless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.012 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2206 _exptl_absorpt_coefficient_mu 2.746 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4930 _exptl_absorpt_correction_T_max 0.6097 _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 CCD _diffrn_measurement_method 'Omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count 0.5 _diffrn_standards_interval_time 10 _diffrn_standards_decay_% ? _diffrn_reflns_number 64279 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0300 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 27.98 _reflns_number_total 16121 _reflns_number_gt 13803 _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 'Platon (Speck, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0903P)^2^+22.5499P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00162(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(11) _refine_ls_number_reflns 16121 _refine_ls_number_parameters 1093 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0762 _refine_ls_R_factor_gt 0.0680 _refine_ls_wR_factor_ref 0.2035 _refine_ls_wR_factor_gt 0.1953 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.044 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.34538(4) 0.0227(2) -0.02112(4) 0.0257(3) Uani 1 d . . . Zn2 Zn 0.16793(4) 0.04320(11) 0.05184(4) 0.0193(2) Uani 1 d . . . Zn3 Zn 0.09465(4) 0.04250(12) 0.22897(4) 0.0233(3) Uani 1 d . . . Zn4 Zn -0.08203(4) 0.0091(3) 0.30194(4) 0.0263(2) Uani 1 d . . . O1 O 0.3578(3) 0.2956(9) -0.0160(3) 0.0394(15) Uani 1 d . . . O2 O 0.3406(4) -0.2575(8) -0.0204(3) 0.0398(16) Uani 1 d . . . O3 O 0.3494(4) 0.0121(11) 0.0705(4) 0.0459(18) Uani 1 d . . . O4 O 0.2781(3) 0.0420(8) -0.0930(3) 0.0252(13) Uani 1 d . . . O5 O 0.2307(3) 0.0443(11) -0.0107(3) 0.0418(16) Uani 1 d . . . C6 C 0.2313(4) 0.0420(10) -0.0661(4) 0.0256(15) Uani 1 d . . . C7 C 0.1721(4) 0.0478(12) -0.1047(4) 0.0343(19) Uani 1 d . . . O8 O 0.1214(3) 0.0298(8) -0.0761(3) 0.0294(13) Uani 1 d . . . C9 C 0.0752(4) 0.0199(11) -0.1193(5) 0.0262(18) Uani 1 d . . . C10 C 0.0977(6) 0.0176(15) -0.1751(6) 0.047(3) Uani 1 d . . . H10 H 0.0757 0.0070 -0.2122 0.057 Uiso 1 calc R . . C11 C 0.1617(5) 0.0349(17) -0.1647(5) 0.052(3) Uani 1 d . . . H11 H 0.1901 0.0367 -0.1936 0.062 Uiso 1 calc R . . C12 C 0.0140(5) 0.0135(14) -0.1026(5) 0.035(2) Uani 1 d . . . O13 O -0.0294(4) 0.0113(14) -0.1417(4) 0.045(2) Uani 1 d . . . O14 O 0.0041(7) 0.099(4) -0.0497(6) 0.040(7) Uani 0.45(4) d P A 1 O14A O 0.0023(7) -0.040(6) -0.0503(8) 0.071(11) Uani 0.55(4) d P A 2 O15 O 0.1642(4) -0.2338(7) 0.0492(5) 0.056(2) Uani 1 d . . . O16 O 0.0767(3) 0.0386(9) 0.0478(3) 0.0351(14) Uani 1 d . . . O17 O 0.1657(3) 0.3196(8) 0.0467(5) 0.056(2) Uani 1 d . . . O18 O 0.2394(3) 0.0366(7) 0.1183(3) 0.0219(12) Uani 1 d . . . O19 O 0.1575(3) 0.0530(8) 0.1668(3) 0.0307(12) Uani 1 d . . . C20 C 0.2119(4) 0.0403(9) 0.1661(3) 0.0234(15) Uani 1 d . . . C21 C 0.2500(4) 0.0358(11) 0.2247(4) 0.0304(17) Uani 1 d . . . O22 O 0.2228(3) 0.0325(8) 0.2754(3) 0.0295(13) Uani 1 d . . . C23 C 0.2681(4) 0.0144(10) 0.3209(4) 0.0224(17) Uani 1 d . . . C24 C 0.3209(5) 0.0003(13) 0.2980(6) 0.040(2) Uani 1 d . . . H24 H 0.3581 -0.0150 0.3195 0.048 Uiso 1 calc R . . C25 C 0.3109(5) 0.0125(14) 0.2356(5) 0.043(2) Uani 1 d . . . H25 H 0.3396 0.0061 0.2071 0.051 Uiso 1 calc R . . C26 C 0.2500(6) 0.011(2) 0.3862(6) 0.063(4) Uani 1 d . . . O27 O 0.2903(4) -0.0196(18) 0.4267(4) 0.074(4) Uani 1 d . . . O28 O 0.1956(4) 0.0327(19) 0.3951(4) 0.097(5) Uani 1 d . . . O29 O 0.0979(3) 0.0585(10) 0.3201(3) 0.0374(14) Uani 1 d . . . O30 O 0.0940(4) 0.3194(9) 0.2301(3) 0.0485(17) Uani 1 d . . . O31 O 0.1043(4) -0.2359(7) 0.2347(3) 0.0420(17) Uani 1 d . . . O32 O 0.0273(3) 0.0218(11) 0.1562(3) 0.0394(18) Uani 1 d . . . O33 O -0.0199(3) 0.0330(9) 0.2395(3) 0.0355(14) Uani 1 d U . . C34 C -0.0192(4) 0.0217(13) 0.1835(4) 0.035(2) Uani 1 d . . . C35 C -0.0789(5) 0.016(2) 0.1444(5) 0.063(4) Uani 1 d . . . O36 O -0.1287(3) 0.0117(7) 0.1734(3) 0.0225(12) Uani 1 d . . . C37 C -0.1747(4) 0.0003(11) 0.1304(5) 0.0248(17) Uani 1 d . . . C38 C -0.1525(6) -0.0100(15) 0.0743(6) 0.047(3) Uani 1 d . . . H38 H -0.1747 -0.0171 0.0371 0.056 Uiso 1 calc R . . C39 C -0.0890(5) -0.0078(14) 0.0845(5) 0.044(2) Uani 1 d . . . H39 H -0.0604 -0.0201 0.0561 0.052 Uiso 1 calc R . . C40 C -0.2366(4) -0.0022(12) 0.1478(4) 0.0258(18) Uani 1 d . . . O41 O -0.2796(5) -0.0143(17) 0.1078(4) 0.091(4) Uani 1 d . . . O42 O -0.2481(4) 0.0164(13) 0.2005(4) 0.052(2) Uani 1 d . . . O43 O -0.0811(3) 0.2856(10) 0.3075(4) 0.0416(16) Uani 1 d . . . O44 O -0.0885(3) -0.2636(10) 0.2886(3) 0.0404(16) Uani 1 d . . . O45 O -0.1732(3) 0.0192(7) 0.2978(3) 0.0274(13) Uani 1 d . . . O46 O -0.0916(3) -0.0031(8) 0.4155(3) 0.0309(14) Uani 1 d . . . O47 O -0.0101(3) -0.0129(8) 0.3682(3) 0.0247(12) Uani 1 d . . . C48 C -0.0383(5) -0.0107(9) 0.4155(4) 0.030(2) Uani 1 d . . . C49 C 0.0005(5) -0.0203(13) 0.4744(5) 0.036(2) Uani 1 d . . . O50 O -0.0269(3) -0.0074(6) 0.5251(3) 0.0214(12) Uani 1 d . . . C51 C 0.0183(4) -0.0105(8) 0.5710(4) 0.0140(14) Uani 1 d . . . C52 C 0.0713(5) -0.0202(13) 0.5486(6) 0.039(2) Uani 1 d . . . H52 H 0.1086 -0.0222 0.5706 0.046 Uiso 1 calc R . . C53 C 0.0618(5) -0.0270(14) 0.4857(5) 0.045(2) Uani 1 d . . . H53 H 0.0908 -0.0345 0.4575 0.054 Uiso 1 calc R . . C54 C 0.0008(5) -0.0076(13) 0.6354(4) 0.0266(18) Uani 1 d . . . O55 O 0.0410(4) -0.0074(12) 0.6771(4) 0.048(2) Uani 1 d . . . O56 O -0.0539(4) 0.0102(16) 0.6448(4) 0.075(3) Uani 1 d . . . Zn5 Zn 0.88721(6) -0.4901(3) -0.06345(6) 0.0704(5) Uani 1 d . . . Zn6 Zn 0.71001(6) -0.5131(2) 0.00975(6) 0.0599(4) Uani 1 d . . . Zn7 Zn 0.63726(5) -0.49471(15) 0.18734(5) 0.0356(3) Uani 1 d . . . Zn8 Zn 0.45996(5) -0.50237(12) 0.25964(5) 0.0254(2) Uani 1 d . . . O57 O 0.8904(5) -0.7674(18) -0.0583(6) 0.106(4) Uani 1 d . . . O58 O 0.9774(5) -0.482(2) -0.0608(5) 0.128(6) Uani 1 d . . . O59 O 0.8911(5) -0.2093(17) -0.0609(5) 0.094(4) Uani 1 d . . . O60 O 0.8235(4) -0.4885(18) 0.0000(5) 0.100(4) Uani 1 d . . . O61 O 0.7746(4) -0.5073(13) 0.0802(5) 0.063(3) Uani 1 d . . . C62 C 0.8262(5) -0.5006(15) 0.0554(5) 0.047(3) Uani 1 d . . . C63 C 0.8807(3) -0.4941(8) 0.0933(4) 0.0162(14) Uani 1 d . . . O64 O 0.9350(4) -0.4706(12) 0.0646(4) 0.049(2) Uani 1 d . . . C65 C 0.9809(5) -0.4669(14) 0.1093(5) 0.035(2) Uani 1 d . . . C66 C 0.9571(6) -0.483(2) 0.1641(6) 0.057(4) Uani 1 d . . . H66 H 0.9788 -0.4848 0.2015 0.069 Uiso 1 calc R . . C67 C 0.8928(5) -0.4956(14) 0.1540(5) 0.041(2) Uani 1 d . . . H67 H 0.8649 -0.5034 0.1833 0.049 Uiso 1 calc R . . C68 C 1.0445(4) -0.4517(11) 0.0911(4) 0.0259(17) Uani 1 d . . . O69 O 1.0840(3) -0.4588(9) 0.1327(3) 0.0319(13) Uani 1 d . . . O70 O 1.0518(4) -0.438(2) 0.0374(4) 0.106(5) Uani 1 d . . . O71 O 0.7124(5) -0.7962(15) 0.0072(5) 0.089(3) Uani 1 d . . . O72 O 0.7007(5) -0.2359(15) 0.0056(4) 0.085(3) Uani 1 d . . . O73 O 0.7062(4) -0.5188(16) -0.0806(4) 0.087(4) Uani 1 d . . . O74 O 0.6475(4) -0.5203(12) 0.0724(4) 0.054(2) Uani 1 d . . . O75 O 0.5660(5) -0.4961(14) 0.1217(5) 0.069(3) Uani 1 d U . . C76 C 0.5906(5) -0.5046(15) 0.0708(5) 0.044(2) Uani 1 d U . . C77 C 0.5519(4) -0.4998(13) 0.0157(4) 0.034(2) Uani 1 d . . . O78 O 0.5819(3) -0.5260(12) -0.0381(3) 0.046(2) Uani 1 d . . . C79 C 0.5389(6) -0.517(2) -0.0847(6) 0.055(4) Uani 1 d . . . C80 C 0.4820(6) -0.491(2) -0.0613(6) 0.069(5) Uani 1 d . . . H80 H 0.4448 -0.4835 -0.0834 0.083 Uiso 1 calc R . . C81 C 0.4926(5) -0.4777(18) 0.0036(5) 0.056(3) Uani 1 d . . . H81 H 0.4638 -0.4577 0.0314 0.068 Uiso 1 calc R . . C82 C 0.5568(4) -0.5336(11) -0.1449(4) 0.0270(18) Uani 1 d . . . O83 O 0.5156(3) -0.5073(8) -0.1873(3) 0.0317(15) Uani 1 d . . . O84 O 0.6081(3) -0.5804(11) -0.1543(3) 0.0420(15) Uani 1 d . . . O85 O 0.6396(4) -0.2184(11) 0.1847(4) 0.063(2) Uani 1 d . . . O86 O 0.6414(4) -0.7737(11) 0.1969(4) 0.059(2) Uani 1 d . . . O87 O 0.7275(4) -0.4846(11) 0.1900(4) 0.0482(19) Uani 1 d . . . O88 O 0.5741(3) -0.4857(8) 0.2498(3) 0.0317(14) Uani 1 d . . . O89 O 0.5243(4) -0.5005(9) 0.3311(4) 0.0392(17) Uani 1 d . . . C90 C 0.5762(4) -0.4981(8) 0.3059(4) 0.0202(15) Uani 1 d . . . C91 C 0.6308(3) -0.5052(7) 0.3442(3) 0.0132(13) Uani 1 d . . . O92 O 0.6848(3) -0.4923(9) 0.3149(3) 0.0307(14) Uani 1 d . . . C93 C 0.7306(5) -0.5137(14) 0.3600(5) 0.036(2) Uani 1 d . . . C94 C 0.7075(6) -0.5353(17) 0.4148(5) 0.048(3) Uani 1 d . . . H94 H 0.7294 -0.5506 0.4518 0.058 Uiso 1 calc R . . C95 C 0.6432(5) -0.5297(14) 0.4046(4) 0.041(2) Uani 1 d . . . H95 H 0.6152 -0.5407 0.4337 0.049 Uiso 1 calc R . . C96 C 0.7943(5) -0.4862(16) 0.3419(5) 0.040(2) Uani 1 d . . . O97 O 0.8344(3) -0.5193(8) 0.3835(3) 0.0295(14) Uani 1 d . . . O98 O 0.8013(3) -0.4382(11) 0.2880(3) 0.0452(17) Uani 1 d . . . O99 O 0.4608(5) -0.7838(7) 0.2575(4) 0.061(2) Uani 1 d . . . O100 O 0.4529(4) -0.2237(8) 0.2558(3) 0.0511(19) Uani 1 d . . . O101 O 0.4570(4) -0.5068(11) 0.1695(3) 0.0460(19) Uani 1 d . . . O102 O 0.3972(3) -0.5116(9) 0.3216(3) 0.0385(16) Uani 1 d . . . O103 O 0.3153(4) -0.5078(13) 0.3715(4) 0.062(3) Uani 1 d . . . C104 C 0.3401(4) -0.5054(10) 0.3210(4) 0.0285(18) Uani 1 d . . . C105 C 0.3014(3) -0.4946(8) 0.2659(4) 0.0158(14) Uani 1 d . . . O106 O 0.3317(3) -0.4969(9) 0.2114(3) 0.0314(14) Uani 1 d . . . C107 C 0.2890(5) -0.4745(12) 0.1653(5) 0.031(2) Uani 1 d . . . C108 C 0.2318(5) -0.4651(13) 0.1888(5) 0.033(2) Uani 1 d . . . H108 H 0.1948 -0.4516 0.1668 0.040 Uiso 1 calc R . . C109 C 0.2415(4) -0.4801(13) 0.2534(4) 0.037(2) Uani 1 d . . . H109 H 0.2120 -0.4798 0.2811 0.044 Uiso 1 calc R . . C110 C 0.3065(4) -0.4805(9) 0.1047(4) 0.0214(17) Uani 1 d . . . O111 O 0.3592(4) -0.5215(14) 0.0949(4) 0.061(3) Uani 1 d . . . O112 O 0.2649(3) -0.4510(8) 0.0628(3) 0.0289(12) Uani 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 Zn1 0.0200(5) 0.0395(7) 0.0173(5) -0.0008(4) -0.0000(4) -0.0003(4) Zn2 0.0140(4) 0.0273(4) 0.0165(4) 0.0007(3) 0.0011(3) -0.0014(3) Zn3 0.0196(5) 0.0337(6) 0.0167(5) 0.0016(4) 0.0002(3) -0.0001(4) Zn4 0.0159(5) 0.0453(6) 0.0176(5) 0.0026(3) 0.0009(4) -0.0023(3) O1 0.050(4) 0.049(4) 0.018(3) -0.008(2) -0.000(2) -0.004(3) O2 0.069(5) 0.029(3) 0.022(3) 0.007(2) 0.004(3) 0.002(3) O3 0.024(4) 0.090(5) 0.024(4) 0.002(3) 0.004(3) 0.005(3) O4 0.008(3) 0.053(3) 0.015(3) 0.004(2) 0.001(2) 0.007(2) O5 0.022(3) 0.092(5) 0.013(3) -0.006(3) 0.009(2) 0.003(3) C6 0.023(4) 0.033(3) 0.021(4) -0.008(3) 0.002(3) -0.007(3) C7 0.023(4) 0.046(4) 0.035(5) -0.005(4) 0.003(3) 0.014(3) O8 0.018(3) 0.052(3) 0.019(3) 0.000(2) 0.003(2) -0.001(2) C9 0.010(4) 0.040(4) 0.029(5) -0.008(3) 0.003(3) 0.004(3) C10 0.027(6) 0.086(8) 0.028(6) -0.006(4) -0.001(4) -0.002(4) C11 0.017(5) 0.108(9) 0.031(6) -0.016(5) 0.003(4) 0.000(4) C12 0.016(4) 0.067(6) 0.022(5) 0.006(4) -0.005(4) -0.004(4) O13 0.021(4) 0.090(6) 0.023(4) -0.013(3) -0.005(3) 0.004(3) O14 0.016(7) 0.081(18) 0.024(7) -0.001(7) 0.003(5) -0.007(7) O14A 0.024(7) 0.15(3) 0.035(8) -0.007(10) 0.007(6) -0.040(10) O15 0.030(3) 0.020(2) 0.121(6) -0.016(4) 0.018(4) -0.009(3) O16 0.017(3) 0.068(4) 0.020(3) 0.012(3) -0.002(2) -0.002(2) O17 0.025(3) 0.039(3) 0.106(6) 0.028(4) 0.019(3) 0.009(3) O18 0.019(3) 0.041(3) 0.007(2) -0.0010(19) 0.005(2) -0.000(2) O19 0.015(3) 0.057(3) 0.021(3) 0.011(2) 0.004(2) -0.010(2) C20 0.030(4) 0.026(3) 0.016(3) 0.005(2) 0.011(3) 0.014(3) C21 0.024(4) 0.044(4) 0.024(4) -0.006(3) 0.007(3) 0.008(3) O22 0.019(3) 0.055(3) 0.015(3) 0.002(2) 0.001(2) -0.000(2) C23 0.020(4) 0.028(3) 0.018(4) 0.005(3) -0.006(3) -0.006(3) C24 0.024(5) 0.062(6) 0.033(6) 0.003(4) -0.005(4) 0.005(3) C25 0.043(7) 0.068(6) 0.018(5) -0.001(3) 0.007(4) 0.008(4) C26 0.027(6) 0.138(12) 0.024(6) 0.000(6) 0.003(5) -0.008(6) O27 0.024(4) 0.179(11) 0.017(4) 0.001(4) -0.001(3) 0.019(5) O28 0.033(5) 0.241(15) 0.018(4) -0.011(5) 0.000(3) 0.009(6) O29 0.021(3) 0.075(4) 0.016(3) -0.002(3) 0.003(2) -0.011(3) O30 0.074(5) 0.047(4) 0.025(3) 0.011(3) 0.010(3) 0.015(4) O31 0.083(5) 0.013(2) 0.031(3) 0.002(2) 0.010(3) -0.004(3) O32 0.009(3) 0.093(5) 0.016(3) 0.004(3) -0.000(2) 0.004(3) O33 0.023(3) 0.076(4) 0.010(3) 0.001(2) 0.011(2) -0.001(3) C34 0.022(5) 0.060(5) 0.024(5) -0.000(3) 0.010(4) -0.001(3) C35 0.019(5) 0.145(12) 0.025(6) 0.013(5) 0.006(4) 0.006(5) O36 0.015(3) 0.034(3) 0.018(3) -0.0009(18) 0.003(2) -0.0009(18) C37 0.013(4) 0.041(4) 0.021(4) 0.003(3) 0.003(3) 0.000(3) C38 0.025(6) 0.086(8) 0.029(6) -0.010(4) -0.000(4) 0.004(4) C39 0.019(5) 0.074(6) 0.039(6) -0.008(4) 0.007(4) 0.001(4) C40 0.018(4) 0.033(4) 0.026(5) 0.004(3) -0.003(3) 0.002(3) O41 0.025(4) 0.222(14) 0.024(4) -0.006(6) -0.006(3) -0.028(6) O42 0.023(4) 0.109(7) 0.024(4) -0.003(3) 0.004(3) 0.006(3) O43 0.019(3) 0.048(4) 0.058(4) 0.004(3) 0.003(3) 0.001(2) O44 0.022(3) 0.049(4) 0.051(4) 0.001(3) 0.001(3) -0.008(2) O45 0.018(3) 0.039(3) 0.025(3) 0.010(2) 0.000(2) -0.0006(19) O46 0.017(3) 0.046(3) 0.030(4) 0.004(2) 0.004(3) 0.002(2) O47 0.021(3) 0.043(3) 0.010(3) 0.004(2) 0.005(2) 0.001(2) C48 0.039(5) 0.024(3) 0.029(5) -0.003(3) 0.025(4) -0.006(3) C49 0.030(5) 0.056(5) 0.024(5) 0.005(3) 0.010(4) -0.009(4) O50 0.019(3) 0.027(2) 0.017(3) 0.0012(17) -0.001(2) 0.0021(17) C51 0.018(4) 0.015(3) 0.008(3) -0.001(2) -0.001(3) 0.000(2) C52 0.024(5) 0.058(5) 0.033(6) -0.006(4) -0.005(4) 0.000(3) C53 0.039(6) 0.072(6) 0.025(5) 0.000(4) 0.011(4) -0.001(4) C54 0.025(5) 0.039(4) 0.016(4) -0.006(3) 0.003(3) -0.001(3) O55 0.024(4) 0.105(6) 0.016(3) 0.002(3) -0.004(3) 0.021(4) O56 0.029(5) 0.171(11) 0.024(4) -0.009(4) -0.001(3) 0.003(5) Zn5 0.0224(7) 0.1627(17) 0.0261(8) -0.0021(7) 0.0016(6) -0.0049(7) Zn6 0.0253(7) 0.1322(13) 0.0222(6) -0.0035(6) 0.0028(5) -0.0040(7) Zn7 0.0250(6) 0.0550(6) 0.0268(6) -0.0020(4) 0.0010(5) -0.0024(4) Zn8 0.0252(5) 0.0289(4) 0.0221(5) -0.0004(3) 0.0017(4) 0.0006(3) O57 0.045(5) 0.155(11) 0.121(9) 0.055(8) 0.019(5) 0.014(6) O58 0.022(5) 0.33(2) 0.029(5) 0.001(6) 0.008(4) -0.000(6) O59 0.052(5) 0.152(10) 0.078(7) -0.051(7) 0.017(4) -0.025(6) O60 0.029(5) 0.230(14) 0.038(5) 0.009(6) -0.021(4) -0.018(5) O61 0.021(4) 0.128(8) 0.041(5) -0.002(4) 0.004(3) -0.007(3) C62 0.018(5) 0.093(8) 0.029(5) -0.003(4) -0.010(4) 0.000(4) C63 0.011(3) 0.021(3) 0.017(4) -0.008(2) -0.002(3) -0.002(2) O64 0.015(3) 0.111(6) 0.021(4) 0.003(3) 0.002(3) -0.008(3) C65 0.021(5) 0.067(6) 0.017(5) -0.001(4) -0.002(4) 0.002(4) C66 0.021(6) 0.132(11) 0.018(5) -0.001(5) 0.000(4) 0.006(5) C67 0.025(5) 0.080(6) 0.017(5) 0.010(4) 0.002(4) 0.006(4) C68 0.017(4) 0.036(4) 0.026(4) -0.005(3) 0.005(3) -0.013(3) O69 0.017(3) 0.052(3) 0.027(3) -0.005(3) 0.003(2) -0.001(2) O70 0.025(4) 0.269(15) 0.023(4) 0.024(7) 0.001(3) -0.018(7) O71 0.088(7) 0.127(8) 0.053(5) -0.018(6) 0.020(5) 0.010(7) O72 0.092(7) 0.126(8) 0.039(5) 0.001(5) 0.007(4) -0.003(6) O73 0.029(5) 0.214(12) 0.018(4) -0.001(5) 0.005(3) -0.024(5) O74 0.027(4) 0.106(6) 0.028(4) -0.008(3) -0.009(3) -0.001(3) O75 0.038(5) 0.136(7) 0.031(4) -0.005(4) -0.005(4) -0.000(4) C76 0.023(4) 0.084(6) 0.022(4) -0.001(4) -0.011(4) -0.010(3) C77 0.017(4) 0.072(6) 0.014(4) 0.002(3) -0.000(3) -0.003(3) O78 0.017(4) 0.105(6) 0.018(3) -0.008(3) 0.005(3) -0.004(3) C79 0.020(6) 0.123(11) 0.023(6) -0.002(5) 0.008(4) -0.001(5) C80 0.023(6) 0.167(14) 0.016(5) -0.004(6) 0.002(4) 0.014(6) C81 0.010(5) 0.128(10) 0.030(6) -0.008(5) -0.002(4) 0.015(5) C82 0.024(5) 0.034(4) 0.023(4) 0.001(3) -0.004(3) 0.005(3) O83 0.029(4) 0.042(3) 0.023(3) 0.002(2) -0.001(3) 0.004(2) O84 0.021(3) 0.083(5) 0.022(3) -0.006(3) 0.003(2) 0.008(3) O85 0.037(4) 0.068(5) 0.085(6) 0.026(4) 0.009(4) 0.003(3) O86 0.033(4) 0.066(4) 0.080(6) -0.026(4) 0.008(3) -0.001(3) O87 0.022(4) 0.094(6) 0.028(4) 0.005(3) 0.003(3) -0.004(3) O88 0.022(3) 0.045(3) 0.026(3) 0.003(2) -0.008(3) -0.003(2) O89 0.021(4) 0.061(4) 0.037(4) 0.002(3) 0.007(3) 0.001(2) C90 0.020(4) 0.021(3) 0.020(4) -0.006(2) -0.001(3) -0.001(2) C91 0.009(3) 0.018(3) 0.013(3) -0.0022(19) 0.001(2) 0.0001(18) O92 0.015(3) 0.055(3) 0.022(3) 0.003(2) 0.002(2) -0.002(2) C93 0.028(6) 0.059(5) 0.021(5) 0.002(4) -0.001(4) -0.002(4) C94 0.022(5) 0.106(9) 0.016(5) 0.009(5) -0.000(4) 0.002(5) C95 0.028(5) 0.084(7) 0.011(4) 0.010(4) 0.005(3) 0.001(4) C96 0.022(5) 0.074(6) 0.024(5) -0.005(4) 0.002(4) -0.015(4) O97 0.022(3) 0.034(3) 0.032(4) 0.014(2) -0.001(3) 0.002(2) O98 0.028(4) 0.084(5) 0.023(3) 0.011(3) 0.001(3) -0.010(3) O99 0.126(7) 0.015(2) 0.045(4) -0.002(3) 0.020(4) -0.013(3) O100 0.085(6) 0.034(3) 0.036(4) 0.005(3) 0.014(3) 0.015(3) O101 0.023(4) 0.098(6) 0.016(3) -0.001(3) 0.003(3) -0.002(3) O102 0.029(4) 0.057(4) 0.028(4) -0.006(3) -0.007(3) 0.010(3) O103 0.027(4) 0.130(8) 0.029(5) 0.008(4) -0.002(3) 0.007(4) C104 0.016(4) 0.046(4) 0.022(4) -0.001(3) -0.011(3) -0.002(3) C105 0.012(3) 0.020(3) 0.016(4) -0.000(2) -0.002(3) -0.001(2) O106 0.021(3) 0.056(3) 0.019(3) 0.001(2) 0.005(2) 0.001(2) C107 0.025(5) 0.034(4) 0.033(5) 0.015(3) 0.004(4) 0.004(3) C108 0.019(5) 0.061(6) 0.020(4) 0.004(3) 0.002(3) 0.012(3) C109 0.008(4) 0.077(6) 0.026(5) 0.004(4) 0.000(3) 0.016(3) C110 0.026(4) 0.016(3) 0.022(4) 0.001(2) -0.001(3) -0.002(2) O111 0.020(4) 0.129(8) 0.034(5) -0.021(4) 0.004(3) 0.004(4) O112 0.026(3) 0.041(3) 0.020(3) -0.001(2) -0.001(2) -0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 2.028(7) . ? Zn1 O3 2.028(8) . ? Zn1 O46 2.057(7) 2_554 ? Zn1 O2 2.064(6) . ? Zn1 O4 2.109(6) . ? Zn2 O16 2.019(7) . ? Zn2 O5 2.034(6) . ? Zn2 O17 2.037(6) . ? Zn2 O15 2.040(5) . ? Zn2 O18 2.086(7) . ? Zn3 O29 2.020(6) . ? Zn3 O19 2.031(6) . ? Zn3 O30 2.037(7) . ? Zn3 O31 2.062(5) . ? Zn3 O32 2.124(8) . ? Zn4 O45 2.019(7) . ? Zn4 O33 2.029(6) . ? Zn4 O44 2.032(7) . ? Zn4 O43 2.038(7) . ? Zn4 O47 2.096(7) . ? O4 C6 1.232(11) . ? O5 C6 1.230(10) . ? C6 C7 1.518(11) . ? C7 O8 1.336(12) . ? C7 C11 1.337(14) . ? O8 C9 1.355(12) . ? C9 C10 1.365(17) . ? C9 C12 1.432(14) . ? C10 C11 1.427(16) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 O13 1.249(13) . ? C12 O14A 1.27(2) . ? C12 O14 1.36(2) . ? O18 C20 1.260(10) . ? O19 C20 1.212(10) . ? C20 C21 1.499(12) . ? C21 O22 1.314(11) . ? C21 C25 1.365(15) . ? O22 C23 1.380(11) . ? C23 C24 1.313(16) . ? C23 C26 1.531(15) . ? C24 C25 1.388(15) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 O27 1.239(16) . ? C26 O28 1.248(17) . ? O32 C34 1.234(12) . ? O33 C34 1.245(11) . ? C34 C35 1.531(15) . ? C35 O36 1.318(13) . ? C35 C39 1.341(16) . ? O36 C37 1.351(12) . ? C37 C38 1.373(17) . ? C37 C40 1.452(14) . ? C38 C39 1.409(16) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 O42 1.222(13) . ? C40 O41 1.258(13) . ? O46 C48 1.183(12) . ? O46 Zn1 2.057(7) 2_455 ? O47 C48 1.258(11) . ? C48 C49 1.514(14) . ? C49 O50 1.319(12) . ? C49 C53 1.365(16) . ? O50 C51 1.378(10) . ? C51 C52 1.312(15) . ? C51 C54 1.507(12) . ? C52 C53 1.397(15) . ? C52 H52 0.9300 . ? C53 H53 0.9300 . ? C54 O55 1.238(13) . ? C54 O56 1.252(14) . ? Zn5 O58 1.997(10) . ? Zn5 O57 2.044(13) . ? Zn5 O60 2.064(12) . ? Zn5 O59 2.068(12) . ? Zn5 O103 2.072(9) 2_544 ? Zn6 O73 1.999(9) . ? Zn6 O74 2.031(9) . ? Zn6 O61 2.043(10) . ? Zn6 O72 2.052(11) . ? Zn6 O71 2.084(11) . ? Zn7 O87 1.999(8) . ? Zn7 O85 2.034(8) . ? Zn7 O88 2.041(8) . ? Zn7 O86 2.065(8) . ? Zn7 O75 2.071(10) . ? Zn8 O101 1.995(8) . ? Zn8 O102 2.025(8) . ? Zn8 O89 2.056(9) . ? Zn8 O100 2.058(6) . ? Zn8 O99 2.071(5) . ? O60 C62 1.228(15) . ? O61 C62 1.306(15) . ? C62 C63 1.423(12) . ? C63 C67 1.355(12) . ? C63 O64 1.411(11) . ? O64 C65 1.368(13) . ? C65 C66 1.365(17) . ? C65 C68 1.499(14) . ? C66 C67 1.430(17) . ? C66 H66 0.9300 . ? C67 H67 0.9300 . ? C68 O70 1.216(12) . ? C68 O69 1.229(12) . ? O74 C76 1.267(13) . ? O75 C76 1.287(15) . ? C76 C77 1.443(12) . ? C77 C81 1.333(13) . ? C77 O78 1.420(12) . ? O78 C79 1.357(15) . ? C79 C80 1.411(18) . ? C79 C82 1.425(15) . ? C80 C81 1.446(16) . ? C80 H80 0.9300 . ? C81 H81 0.9300 . ? C82 O84 1.221(11) . ? C82 O83 1.278(12) . ? O88 C90 1.244(11) . ? O89 C90 1.315(12) . ? C90 C91 1.429(10) . ? C91 C95 1.361(11) . ? C91 O92 1.405(10) . ? O92 C93 1.381(14) . ? C93 C94 1.361(17) . ? C93 C96 1.510(16) . ? C94 C95 1.429(16) . ? C94 H94 0.9300 . ? C95 H95 0.9300 . ? C96 O97 1.258(13) . ? C96 O98 1.268(13) . ? O102 C104 1.267(11) . ? O103 C104 1.284(14) . ? O103 Zn5 2.072(9) 2_445 ? C104 C105 1.445(10) . ? C105 C109 1.341(11) . ? C105 O106 1.425(11) . ? O106 C107 1.354(13) . ? C107 C108 1.406(15) . ? C107 C110 1.426(14) . ? C108 C109 1.437(14) . ? C108 H108 0.9300 . ? C109 H109 0.9300 . ? C110 O111 1.243(12) . ? C110 O112 1.279(11) . ? 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 Zn1 O3 89.2(3) . . ? O1 Zn1 O46 90.6(3) . 2_554 ? O3 Zn1 O46 134.3(3) . 2_554 ? O1 Zn1 O2 174.1(3) . . ? O3 Zn1 O2 87.3(3) . . ? O46 Zn1 O2 88.5(3) 2_554 . ? O1 Zn1 O4 93.5(2) . . ? O3 Zn1 O4 137.5(3) . . ? O46 Zn1 O4 88.1(3) 2_554 . ? O2 Zn1 O4 92.2(3) . . ? O16 Zn2 O5 134.6(3) . . ? O16 Zn2 O17 89.7(3) . . ? O5 Zn2 O17 88.4(3) . . ? O16 Zn2 O15 86.8(3) . . ? O5 Zn2 O15 90.7(3) . . ? O17 Zn2 O15 174.1(4) . . ? O16 Zn2 O18 137.7(3) . . ? O5 Zn2 O18 87.7(2) . . ? O17 Zn2 O18 94.4(3) . . ? O15 Zn2 O18 91.4(3) . . ? O29 Zn3 O19 134.4(3) . . ? O29 Zn3 O30 85.9(3) . . ? O19 Zn3 O30 88.7(3) . . ? O29 Zn3 O31 90.0(3) . . ? O19 Zn3 O31 90.3(3) . . ? O30 Zn3 O31 173.2(4) . . ? O29 Zn3 O32 137.5(3) . . ? O19 Zn3 O32 88.1(3) . . ? O30 Zn3 O32 94.4(3) . . ? O31 Zn3 O32 92.3(3) . . ? O45 Zn4 O33 133.8(3) . . ? O45 Zn4 O44 88.2(2) . . ? O33 Zn4 O44 91.8(3) . . ? O45 Zn4 O43 88.4(2) . . ? O33 Zn4 O43 87.2(3) . . ? O44 Zn4 O43 174.2(3) . . ? O45 Zn4 O47 138.1(3) . . ? O33 Zn4 O47 88.1(3) . . ? O44 Zn4 O47 93.9(2) . . ? O43 Zn4 O47 91.8(3) . . ? C6 O4 Zn1 102.0(5) . . ? C6 O5 Zn2 137.6(6) . . ? O5 C6 O4 123.6(8) . . ? O5 C6 C7 119.5(8) . . ? O4 C6 C7 116.9(7) . . ? O8 C7 C11 112.0(9) . . ? O8 C7 C6 116.9(8) . . ? C11 C7 C6 129.8(9) . . ? C7 O8 C9 106.8(8) . . ? O8 C9 C10 109.5(9) . . ? O8 C9 C12 120.1(9) . . ? C10 C9 C12 130.4(10) . . ? C9 C10 C11 106.1(10) . . ? C9 C10 H10 127.0 . . ? C11 C10 H10 127.0 . . ? C7 C11 C10 105.4(10) . . ? C7 C11 H11 127.3 . . ? C10 C11 H11 127.3 . . ? O13 C12 O14A 115.6(12) . . ? O13 C12 O14 116.1(11) . . ? O14A C12 O14 45.5(13) . . ? O13 C12 C9 121.2(10) . . ? O14A C12 C9 120.4(12) . . ? O14 C12 C9 114.9(11) . . ? C20 O18 Zn2 101.9(5) . . ? C20 O19 Zn3 137.6(5) . . ? O19 C20 O18 123.6(8) . . ? O19 C20 C21 119.4(7) . . ? O18 C20 C21 116.9(7) . . ? O22 C21 C25 110.8(9) . . ? O22 C21 C20 118.5(8) . . ? C25 C21 C20 130.2(8) . . ? C21 O22 C23 105.9(7) . . ? C24 C23 O22 110.3(9) . . ? C24 C23 C26 131.8(10) . . ? O22 C23 C26 117.9(9) . . ? C23 C24 C25 107.3(10) . . ? C23 C24 H24 126.4 . . ? C25 C24 H24 126.4 . . ? C21 C25 C24 105.7(10) . . ? C21 C25 H25 127.1 . . ? C24 C25 H25 127.1 . . ? O27 C26 O28 124.4(12) . . ? O27 C26 C23 117.7(11) . . ? O28 C26 C23 117.9(11) . . ? C34 O32 Zn3 101.3(7) . . ? C34 O33 Zn4 137.1(6) . . ? O32 C34 O33 124.0(10) . . ? O32 C34 C35 116.2(9) . . ? O33 C34 C35 119.7(9) . . ? O36 C35 C39 113.2(11) . . ? O36 C35 C34 116.3(9) . . ? C39 C35 C34 129.9(10) . . ? C35 O36 C37 105.8(8) . . ? O36 C37 C38 110.0(9) . . ? O36 C37 C40 119.6(9) . . ? C38 C37 C40 130.4(10) . . ? C37 C38 C39 105.8(11) . . ? C37 C38 H38 127.1 . . ? C39 C38 H38 127.1 . . ? C35 C39 C38 104.8(10) . . ? C35 C39 H39 127.6 . . ? C38 C39 H39 127.6 . . ? O42 C40 O41 118.8(10) . . ? O42 C40 C37 121.3(9) . . ? O41 C40 C37 119.8(10) . . ? C48 O46 Zn1 136.4(7) . 2_455 ? C48 O47 Zn4 100.7(6) . . ? O46 C48 O47 123.8(10) . . ? O46 C48 C49 120.5(8) . . ? O47 C48 C49 115.7(9) . . ? O50 C49 C53 111.1(9) . . ? O50 C49 C48 117.7(9) . . ? C53 C49 C48 131.0(9) . . ? C49 O50 C51 105.9(7) . . ? C52 C51 O50 110.2(8) . . ? C52 C51 C54 131.3(9) . . ? O50 C51 C54 118.5(7) . . ? C51 C52 C53 107.8(10) . . ? C51 C52 H52 126.1 . . ? C53 C52 H52 126.1 . . ? C49 C53 C52 105.1(10) . . ? C49 C53 H53 127.5 . . ? C52 C53 H53 127.5 . . ? O55 C54 O56 122.1(10) . . ? O55 C54 C51 119.2(9) . . ? O56 C54 C51 118.5(9) . . ? O58 Zn5 O57 89.9(5) . . ? O58 Zn5 O60 135.4(4) . . ? O57 Zn5 O60 89.4(5) . . ? O58 Zn5 O59 85.9(5) . . ? O57 Zn5 O59 173.7(5) . . ? O60 Zn5 O59 90.2(5) . . ? O58 Zn5 O103 137.7(4) . 2_544 ? O57 Zn5 O103 93.1(4) . 2_544 ? O60 Zn5 O103 86.8(4) . 2_544 ? O59 Zn5 O103 93.1(4) . 2_544 ? O73 Zn6 O74 134.6(4) . . ? O73 Zn6 O61 138.0(4) . . ? O74 Zn6 O61 87.3(3) . . ? O73 Zn6 O72 88.8(4) . . ? O74 Zn6 O72 89.1(4) . . ? O61 Zn6 O72 94.4(4) . . ? O73 Zn6 O71 87.2(5) . . ? O74 Zn6 O71 90.7(4) . . ? O61 Zn6 O71 91.4(4) . . ? O72 Zn6 O71 174.3(5) . . ? O87 Zn7 O85 86.3(3) . . ? O87 Zn7 O88 135.5(3) . . ? O85 Zn7 O88 90.5(3) . . ? O87 Zn7 O86 89.8(3) . . ? O85 Zn7 O86 174.4(4) . . ? O88 Zn7 O86 89.4(3) . . ? O87 Zn7 O75 137.1(4) . . ? O85 Zn7 O75 90.3(4) . . ? O88 Zn7 O75 87.2(3) . . ? O86 Zn7 O75 95.4(4) . . ? O101 Zn8 O102 134.7(3) . . ? O101 Zn8 O89 138.0(3) . . ? O102 Zn8 O89 87.1(3) . . ? O101 Zn8 O100 88.7(3) . . ? O102 Zn8 O100 90.4(3) . . ? O89 Zn8 O100 94.1(3) . . ? O101 Zn8 O99 87.7(3) . . ? O102 Zn8 O99 89.4(3) . . ? O89 Zn8 O99 91.0(3) . . ? O100 Zn8 O99 174.9(4) . . ? C62 O60 Zn5 134.0(8) . . ? C62 O61 Zn6 105.5(8) . . ? O60 C62 O61 116.3(10) . . ? O60 C62 C63 124.5(10) . . ? O61 C62 C63 119.1(10) . . ? C67 C63 O64 109.5(8) . . ? C67 C63 C62 133.3(9) . . ? O64 C63 C62 117.0(8) . . ? C65 O64 C63 106.9(8) . . ? C66 C65 O64 109.2(10) . . ? C66 C65 C68 132.7(10) . . ? O64 C65 C68 118.1(9) . . ? C65 C66 C67 108.1(11) . . ? C65 C66 H66 125.9 . . ? C67 C66 H66 125.9 . . ? C63 C67 C66 106.2(9) . . ? C63 C67 H67 126.9 . . ? C66 C67 H67 126.9 . . ? O70 C68 O69 126.9(9) . . ? O70 C68 C65 117.6(9) . . ? O69 C68 C65 115.4(8) . . ? C76 O74 Zn6 135.0(7) . . ? C76 O75 Zn7 105.5(8) . . ? O74 C76 O75 117.6(9) . . ? O74 C76 C77 123.8(10) . . ? O75 C76 C77 118.5(10) . . ? C81 C77 O78 111.3(9) . . ? C81 C77 C76 133.7(10) . . ? O78 C77 C76 115.0(9) . . ? C79 O78 C77 106.6(8) . . ? O78 C79 C80 109.0(11) . . ? O78 C79 C82 118.8(10) . . ? C80 C79 C82 132.2(12) . . ? C79 C80 C81 106.8(11) . . ? C79 C80 H80 126.6 . . ? C81 C80 H80 126.6 . . ? C77 C81 C80 106.2(10) . . ? C77 C81 H81 126.9 . . ? C80 C81 H81 126.9 . . ? O84 C82 O83 122.9(9) . . ? O84 C82 C79 120.6(9) . . ? O83 C82 C79 116.4(9) . . ? C90 O88 Zn7 134.2(6) . . ? C90 O89 Zn8 104.7(6) . . ? O88 C90 O89 116.9(8) . . ? O88 C90 C91 124.6(8) . . ? O89 C90 C91 118.5(8) . . ? C95 C91 O92 110.2(7) . . ? C95 C91 C90 133.8(8) . . ? O92 C91 C90 115.9(7) . . ? C93 O92 C91 105.3(8) . . ? C94 C93 O92 110.9(11) . . ? C94 C93 C96 132.1(11) . . ? O92 C93 C96 116.5(9) . . ? C93 C94 C95 106.9(10) . . ? C93 C94 H94 126.6 . . ? C95 C94 H94 126.6 . . ? C91 C95 C94 106.7(8) . . ? C91 C95 H95 126.6 . . ? C94 C95 H95 126.6 . . ? O97 C96 O98 128.2(10) . . ? O97 C96 C93 114.0(10) . . ? O98 C96 C93 117.8(10) . . ? C104 O102 Zn8 136.6(6) . . ? C104 O103 Zn5 104.5(7) . 2_445 ? O102 C104 O103 118.7(8) . . ? O102 C104 C105 123.0(8) . . ? O103 C104 C105 118.3(8) . . ? C109 C105 O106 110.2(8) . . ? C109 C105 C104 134.4(8) . . ? O106 C105 C104 115.4(7) . . ? C107 O106 C105 107.0(7) . . ? O106 C107 C108 109.0(9) . . ? O106 C107 C110 119.1(9) . . ? C108 C107 C110 131.6(10) . . ? C107 C108 C109 107.0(9) . . ? C107 C108 H108 126.5 . . ? C109 C108 H108 126.5 . . ? C105 C109 C108 106.7(8) . . ? C105 C109 H109 126.6 . . ? C108 C109 H109 126.6 . . ? O111 C110 O112 123.6(9) . . ? O111 C110 C107 119.7(9) . . ? O112 C110 C107 116.6(9) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.98 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.138 _refine_diff_density_min -3.550 _refine_diff_density_rms 0.153