# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global #TrackingRef '- 1-5.cif' _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _publ_contact_author_name 'Hong Zhang' _publ_contact_author_address ; Department of Chemistry Northeast Normal University Changchun 130024 P.R.China ; _publ_contact_author_email zhangh@nenu.edu.cn _publ_contact_author_phone +86-431-85099370 _publ_contact_author_fax +86-431-85099372 _publ_section_title ; A series of complexes based on biphenyl-2,5,2',5'-tetracarboxylic acid: syntheses, crystal structures, luminescent and magnetic properties ; loop_ _publ_author_name 'Dan Tian' 'Yu Pang' 'Hong-Yan Zhou' 'Li Guan' 'Hong Zhang' data_complex-1 #TrackingRef '- 1-5.cif' _database_code_depnum_ccdc_archive 'CCDC 730693' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H40 Cu2 N0 O25' _chemical_formula_sum 'C16 H40 Cu2 N0 O25' _chemical_formula_weight 759.56 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' Cu Cu 0.3201 1.2651 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.1695(11) _cell_length_b 17.1480(11) _cell_length_c 14.6239(16) _cell_angle_alpha 90.00 _cell_angle_beta 107.9160(10) _cell_angle_gamma 90.00 _cell_volume 3142.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.01 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 1.449 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.608 _exptl_absorpt_correction_T_max 0.629 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'BRUKER SMART CCD Apex II' _diffrn_measurement_method 'omega and phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7477 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2701 _reflns_number_gt 2358 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SMART (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0667P)^2^+11.6804P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2701 _refine_ls_number_parameters 195 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1241 _refine_ls_wR_factor_gt 0.1202 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4396(3) 0.16153(18) 0.6417(2) 0.0213(7) Uani 1 1 d . . . C2 C 0.5123(2) 0.09349(17) 0.6451(2) 0.0185(6) Uani 1 1 d . . . C3 C 0.5669(3) 0.09214(19) 0.5775(2) 0.0250(7) Uani 1 1 d . . . H3 H 0.5625 0.1349 0.5374 0.030 Uiso 1 1 calc R . . C4 C 0.6276(3) 0.0286(2) 0.5689(3) 0.0284(8) Uani 1 1 d . . . H4 H 0.6650 0.0291 0.5244 0.034 Uiso 1 1 calc R . . C5 C 0.6323(3) -0.03615(19) 0.6272(2) 0.0237(7) Uani 1 1 d . . . C6 C 0.5820(3) -0.03394(18) 0.6975(2) 0.0218(7) Uani 1 1 d . . . H6 H 0.5876 -0.0768 0.7377 0.026 Uiso 1 1 calc R . . C7 C 0.5232(2) 0.03063(17) 0.7098(2) 0.0170(6) Uani 1 1 d . . . C8 C 0.6916(3) -0.1079(2) 0.6134(3) 0.0295(8) Uani 1 1 d . . . Cu1 Cu 0.25399(3) 0.23552(2) 0.65821(3) 0.02576(18) Uani 1 1 d . . . O1 O 0.35303(18) 0.14904(13) 0.66096(19) 0.0278(6) Uani 1 1 d . . . O2 O 0.4653(2) 0.22696(13) 0.6182(2) 0.0333(6) Uani 1 1 d . . . O3 O 0.6636(2) -0.17191(14) 0.6440(2) 0.0337(6) Uani 1 1 d . . . O4 O 0.7620(2) -0.10213(17) 0.5748(2) 0.0503(8) Uani 1 1 d . . . O1W O 0.1634(2) 0.19494(15) 0.53521(18) 0.0348(6) Uani 1 1 d . . . H1WB H 0.1306 0.2325 0.5006 0.052 Uiso 1 1 d R . . H1WA H 0.1966 0.1666 0.5061 0.052 Uiso 1 1 d R . . O3W O 0.1624(3) 0.1586(2) 0.7328(3) 0.0752(11) Uani 1 1 d . . . H3WA H 0.1754 0.1726 0.7888 0.113 Uiso 1 1 d R . . H3WB H 0.1175 0.1884 0.6993 0.113 Uiso 1 1 d R . . O2W O 0.3457(2) 0.28326(18) 0.7769(2) 0.0512(8) Uani 1 1 d D . . H2WB H 0.3073 0.3004 0.8098 0.077 Uiso 1 1 d RD . . H2WA H 0.3958 0.2578 0.8160 0.077 Uiso 1 1 d RD . . O4W O 0.7463(3) 0.1474(2) 0.3930(3) 0.0586(9) Uani 1 1 d . . . H4WB H 0.6834 0.1612 0.3906 0.088 Uiso 1 1 d R . . H4WA H 0.7822 0.1553 0.4516 0.088 Uiso 1 1 d R . . O5W O 0.8720(4) 0.1477(3) 0.5855(4) 0.0949(15) Uani 1 1 d D . . H5WA H 0.9060 0.1335 0.5501 0.142 Uiso 1 1 d RD . . H5WB H 0.8953 0.1256 0.6375 0.142 Uiso 1 1 d RD . . O6W O 0.9575(3) 0.2901(2) 0.6477(3) 0.0719(11) Uani 1 1 d D . . H6WA H 0.9337 0.2500 0.6128 0.108 Uiso 1 1 d RD . . H6WB H 1.0124 0.3023 0.6322 0.108 Uiso 1 1 d RD . . O7W O 0.5000 0.4120(5) 0.7500 0.138(3) Uani 1 2 d SD . . H7WA H 0.5245 0.3701 0.7397 0.207 Uiso 0.50 1 d PRD . . H7WB H 0.4505 0.4232 0.7021 0.207 Uiso 0.50 1 d PRD . . O8W O 0.4983(12) 0.5207(6) 0.8872(10) 0.310(8) Uani 1 1 d D . . H8WA H 0.4644 0.5137 0.9251 0.465 Uiso 1 1 d RD . . H8WB H 0.5566 0.4946 0.9099 0.465 Uiso 1 1 d RD . . O9W O 0.7879(5) -0.0110(3) 0.3943(4) 0.1143(19) Uani 1 1 d D . . H9WA H 0.7683 0.0345 0.3851 0.172 Uiso 1 1 d RD . . H9WB H 0.7417 -0.0352 0.4093 0.172 Uiso 1 1 d RD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0219(16) 0.0203(15) 0.0177(17) -0.0003(12) 0.0003(13) 0.0037(12) C2 0.0182(15) 0.0155(14) 0.0214(17) 0.0012(12) 0.0053(13) 0.0009(12) C3 0.0322(18) 0.0211(15) 0.0234(18) 0.0057(13) 0.0112(15) 0.0014(14) C4 0.0327(19) 0.0316(18) 0.027(2) 0.0004(14) 0.0176(16) 0.0031(15) C5 0.0227(17) 0.0222(16) 0.0264(19) -0.0036(13) 0.0079(14) 0.0039(13) C6 0.0270(17) 0.0153(14) 0.0239(18) 0.0021(12) 0.0090(14) 0.0022(12) C7 0.0157(14) 0.0158(14) 0.0195(16) -0.0007(12) 0.0054(13) 0.0000(11) C8 0.0266(18) 0.0293(18) 0.032(2) -0.0070(15) 0.0087(15) 0.0072(14) Cu1 0.0266(3) 0.0218(3) 0.0291(3) -0.00075(16) 0.00886(19) 0.00954(16) O1 0.0244(12) 0.0219(11) 0.0385(15) 0.0023(10) 0.0116(11) 0.0073(9) O2 0.0322(14) 0.0179(12) 0.0451(17) 0.0079(10) 0.0050(12) 0.0023(10) O3 0.0312(14) 0.0243(12) 0.0467(17) -0.0033(11) 0.0137(12) 0.0101(10) O4 0.0543(19) 0.0403(16) 0.073(2) -0.0078(15) 0.0441(18) 0.0109(14) O1W 0.0401(15) 0.0310(13) 0.0308(15) -0.0008(10) 0.0074(12) 0.0176(11) O3W 0.086(3) 0.085(3) 0.066(3) 0.015(2) 0.040(2) -0.006(2) O2W 0.0428(17) 0.0528(18) 0.0483(19) -0.0171(15) -0.0003(14) 0.0213(14) O4W 0.056(2) 0.062(2) 0.054(2) 0.0062(16) 0.0128(17) -0.0071(16) O5W 0.120(4) 0.094(3) 0.072(3) -0.012(2) 0.033(3) -0.015(3) O6W 0.060(2) 0.068(2) 0.095(3) -0.003(2) 0.034(2) -0.0083(19) O7W 0.103(6) 0.083(5) 0.236(11) 0.000 0.064(7) 0.000 O8W 0.415(18) 0.240(11) 0.388(17) -0.170(12) 0.292(16) -0.210(12) O9W 0.120(4) 0.055(3) 0.147(5) 0.011(3) 0.009(4) -0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.251(4) . ? C1 O1 1.273(4) . ? C1 C2 1.501(4) . ? C2 C3 1.390(5) . ? C2 C7 1.413(4) . ? C3 C4 1.379(5) . ? C3 H3 0.9300 . ? C4 C5 1.390(5) . ? C4 H4 0.9300 . ? C5 C6 1.384(5) . ? C5 C8 1.503(4) . ? C6 C7 1.394(4) . ? C6 H6 0.9300 . ? C7 C7 1.481(6) 2_656 ? C8 O4 1.228(5) . ? C8 O3 1.282(5) . ? Cu1 O1W 1.955(3) . ? Cu1 O3 1.957(2) 3_455 ? Cu1 O2W 1.962(3) . ? Cu1 O1 1.967(2) . ? Cu1 O3W 2.279(4) . ? O3 Cu1 1.957(2) 3_545 ? O1W H1WB 0.8499 . ? O1W H1WA 0.8500 . ? O3W H3WA 0.8199 . ? O3W H3WB 0.8200 . ? O2W H2WB 0.8500 . ? O2W H2WA 0.8500 . ? O4W H4WB 0.8520 . ? O4W H4WA 0.8520 . ? O5W H5WA 0.8190 . ? O5W H5WB 0.8200 . ? O6W H6WA 0.8569 . ? O6W H6WB 0.8475 . ? O7W H7WA 0.8200 . ? O7W H7WB 0.8200 . ? O8W H8WA 0.8211 . ? O8W H8WB 0.8619 . ? O9W H9WA 0.8199 . ? O9W H9WB 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 C1 O1 123.3(3) . . ? O2 C1 C2 118.8(3) . . ? O1 C1 C2 117.9(3) . . ? C3 C2 C7 119.7(3) . . ? C3 C2 C1 117.0(3) . . ? C7 C2 C1 123.2(3) . . ? C4 C3 C2 121.3(3) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 119.5(3) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C6 C5 C4 119.5(3) . . ? C6 C5 C8 120.6(3) . . ? C4 C5 C8 119.9(3) . . ? C5 C6 C7 122.0(3) . . ? C5 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C6 C7 C2 117.7(3) . . ? C6 C7 C7 118.9(2) . 2_656 ? C2 C7 C7 123.4(2) . 2_656 ? O4 C8 O3 124.6(3) . . ? O4 C8 C5 119.5(3) . . ? O3 C8 C5 115.9(3) . . ? O1W Cu1 O3 90.71(11) . 3_455 ? O1W Cu1 O2W 175.88(13) . . ? O3 Cu1 O2W 86.78(11) 3_455 . ? O1W Cu1 O1 87.90(10) . . ? O3 Cu1 O1 172.64(11) 3_455 . ? O2W Cu1 O1 94.17(11) . . ? O1W Cu1 O3W 88.36(14) . . ? O3 Cu1 O3W 97.24(13) 3_455 . ? O2W Cu1 O3W 95.19(16) . . ? O1 Cu1 O3W 89.94(13) . . ? C1 O1 Cu1 120.1(2) . . ? C8 O3 Cu1 120.1(2) . 3_545 ? Cu1 O1W H1WB 109.4 . . ? Cu1 O1W H1WA 113.7 . . ? H1WB O1W H1WA 112.4 . . ? Cu1 O3W H3WA 109.3 . . ? Cu1 O3W H3WB 75.2 . . ? H3WA O3W H3WB 107.7 . . ? Cu1 O2W H2WB 109.5 . . ? Cu1 O2W H2WA 121.4 . . ? H2WB O2W H2WA 105.7 . . ? H4WB O4W H4WA 103.2 . . ? H5WA O5W H5WB 109.2 . . ? H6WA O6W H6WB 103.0 . . ? H7WA O7W H7WB 107.7 . . ? H8WA O8W H8WB 105.5 . . ? H9WA O9W H9WB 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C3 -34.4(4) . . . . ? O1 C1 C2 C3 143.9(3) . . . . ? O2 C1 C2 C7 148.5(3) . . . . ? O1 C1 C2 C7 -33.2(5) . . . . ? C7 C2 C3 C4 3.4(5) . . . . ? C1 C2 C3 C4 -173.8(3) . . . . ? C2 C3 C4 C5 1.5(5) . . . . ? C3 C4 C5 C6 -4.3(5) . . . . ? C3 C4 C5 C8 175.5(3) . . . . ? C4 C5 C6 C7 2.2(5) . . . . ? C8 C5 C6 C7 -177.7(3) . . . . ? C5 C6 C7 C2 2.7(5) . . . . ? C5 C6 C7 C7 -176.5(3) . . . 2_656 ? C3 C2 C7 C6 -5.4(5) . . . . ? C1 C2 C7 C6 171.6(3) . . . . ? C3 C2 C7 C7 173.7(3) . . . 2_656 ? C1 C2 C7 C7 -9.3(5) . . . 2_656 ? C6 C5 C8 O4 -157.0(4) . . . . ? C4 C5 C8 O4 23.2(5) . . . . ? C6 C5 C8 O3 22.9(5) . . . . ? C4 C5 C8 O3 -157.0(3) . . . . ? O2 C1 O1 Cu1 -1.9(5) . . . . ? C2 C1 O1 Cu1 179.9(2) . . . . ? O1W Cu1 O1 C1 104.0(3) . . . . ? O3 Cu1 O1 C1 24.8(10) 3_455 . . . ? O2W Cu1 O1 C1 -72.4(3) . . . . ? O3W Cu1 O1 C1 -167.6(3) . . . . ? O4 C8 O3 Cu1 14.0(5) . . . 3_545 ? C5 C8 O3 Cu1 -165.9(2) . . . 3_545 ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.690 _refine_diff_density_min -0.601 _refine_diff_density_rms 0.087 #===========================end data_complex-4 #TrackingRef '- 1-5.cif' _database_code_depnum_ccdc_archive 'CCDC 732293' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H38 N4 Ni2 O16' _chemical_formula_sum 'C36 H38 N4 Ni2 O16' _chemical_formula_weight 900.08 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 monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall 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 14.223(2) _cell_length_b 19.095(3) _cell_length_c 15.143(2) _cell_angle_alpha 90.00 _cell_angle_beta 113.099(2) _cell_angle_gamma 90.00 _cell_volume 3783.0(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.56 _cell_measurement_theta_max 25.00 _exptl_crystal_description neddle _exptl_crystal_colour blue _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 1.076 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.846 _exptl_absorpt_correction_T_max 0.869 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'BRUKER SMART CCD Apex II' _diffrn_measurement_method 'omega and phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19000 _diffrn_reflns_av_R_equivalents 0.0770 _diffrn_reflns_av_sigmaI/netI 0.1016 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6629 _reflns_number_gt 3820 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SMART (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6629 _refine_ls_number_parameters 561 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1141 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1014 _refine_ls_wR_factor_gt 0.0882 _refine_ls_goodness_of_fit_ref 0.919 _refine_ls_restrained_S_all 0.918 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.1298(4) 0.1632(3) 0.5599(4) 0.0467(14) Uani 1 1 d . . . H1 H 1.0754 0.1322 0.5332 0.056 Uiso 1 1 calc R . . C2 C 1.2214(5) 0.1378(3) 0.6244(4) 0.0603(16) Uani 1 1 d . . . H2 H 1.2289 0.0905 0.6399 0.072 Uiso 1 1 calc R . . C3 C 1.3017(4) 0.1830(3) 0.6655(4) 0.0618(17) Uani 1 1 d . . . H3 H 1.3642 0.1669 0.7095 0.074 Uiso 1 1 calc R . . C4 C 1.2881(4) 0.2524(3) 0.6406(4) 0.0540(14) Uani 1 1 d . . . H4 H 1.3415 0.2839 0.6680 0.065 Uiso 1 1 calc R . . C5 C 1.1949(3) 0.2755(3) 0.5748(3) 0.0377(12) Uani 1 1 d . . . C6 C 1.1736(3) 0.3493(2) 0.5427(3) 0.0367(12) Uani 1 1 d . . . C7 C 1.2462(4) 0.4013(3) 0.5667(4) 0.0509(15) Uani 1 1 d . . . H7 H 1.3135 0.3919 0.6075 0.061 Uiso 1 1 calc R . . C8 C 1.2184(4) 0.4673(3) 0.5296(4) 0.0538(15) Uani 1 1 d . . . H8 H 1.2666 0.5031 0.5462 0.065 Uiso 1 1 calc R . . C9 C 1.1203(4) 0.4804(2) 0.4686(4) 0.0480(14) Uani 1 1 d . . . H9 H 1.1008 0.5246 0.4419 0.058 Uiso 1 1 calc R . . C10 C 1.0503(4) 0.4264(2) 0.4475(4) 0.0406(13) Uani 1 1 d . . . H10 H 0.9828 0.4352 0.4070 0.049 Uiso 1 1 calc R . . C11 C 0.7651(3) 0.32996(19) 0.3443(3) 0.0231(10) Uani 1 1 d . . . C12 C 0.6957(3) 0.39164(19) 0.3057(3) 0.0215(10) Uani 1 1 d . . . C13 C 0.6086(3) 0.3964(2) 0.3256(3) 0.0280(11) Uani 1 1 d . . . H13 H 0.5917 0.3590 0.3560 0.034 Uiso 1 1 calc R . . C14 C 0.5462(3) 0.4547(2) 0.3018(3) 0.0295(11) Uani 1 1 d . . . H14 H 0.4892 0.4567 0.3175 0.035 Uiso 1 1 calc R . . C15 C 0.5686(3) 0.5101(2) 0.2547(3) 0.0265(10) Uani 1 1 d . . . C16 C 0.5077(4) 0.5770(2) 0.2335(4) 0.0427(13) Uani 1 1 d . . . C17 C 0.6525(3) 0.5039(2) 0.2306(3) 0.0265(10) Uani 1 1 d . . . H17 H 0.6658 0.5401 0.1961 0.032 Uiso 1 1 calc R . . C18 C 0.7182(3) 0.44654(19) 0.2550(3) 0.0193(9) Uani 1 1 d . . . C19 C 0.8069(3) 0.4488(2) 0.2249(3) 0.0242(10) Uani 1 1 d . . . C20 C 0.8642(3) 0.5101(2) 0.2432(3) 0.0269(10) Uani 1 1 d . . . H20 H 0.8488 0.5458 0.2771 0.032 Uiso 1 1 calc R . . C21 C 0.9443(3) 0.5199(2) 0.2124(3) 0.0297(11) Uani 1 1 d . . . C22 C 0.9958(4) 0.5905(2) 0.2225(4) 0.0408(13) Uani 1 1 d . . . C23 C 0.9701(3) 0.4652(2) 0.1675(4) 0.0429(13) Uani 1 1 d . . . H23 H 1.0248 0.4699 0.1489 0.051 Uiso 1 1 calc R . . C24 C 0.9156(3) 0.4037(2) 0.1496(3) 0.0385(12) Uani 1 1 d . . . H24 H 0.9343 0.3670 0.1194 0.046 Uiso 1 1 calc R . . C25 C 0.8330(3) 0.39524(19) 0.1760(3) 0.0250(10) Uani 1 1 d . . . C26 C 0.7735(3) 0.3276(2) 0.1445(3) 0.0249(10) Uani 1 1 d . . . C27 C 0.4745(4) 0.3973(2) 0.0505(3) 0.0409(12) Uani 1 1 d . . . H27 H 0.5403 0.4113 0.0899 0.049 Uiso 1 1 calc R . . C28 C 0.3966(4) 0.4462(3) 0.0256(4) 0.0508(14) Uani 1 1 d . . . H28 H 0.4098 0.4917 0.0493 0.061 Uiso 1 1 calc R . . C29 C 0.3010(4) 0.4269(3) -0.0337(4) 0.0544(15) Uani 1 1 d . . . H29 H 0.2474 0.4589 -0.0508 0.065 Uiso 1 1 calc R . . C30 C 0.2840(4) 0.3598(3) -0.0681(4) 0.0509(14) Uani 1 1 d . . . H30 H 0.2193 0.3465 -0.1110 0.061 Uiso 1 1 calc R . . C31 C 0.3639(3) 0.3113(3) -0.0386(3) 0.0391(12) Uani 1 1 d . . . C32 C 0.3532(4) 0.2374(3) -0.0652(3) 0.0444(13) Uani 1 1 d . . . C33 C 0.2622(4) 0.2064(3) -0.1246(4) 0.0631(17) Uani 1 1 d . . . H33 H 0.2038 0.2337 -0.1527 0.076 Uiso 1 1 calc R . . C34 C 0.2577(5) 0.1356(4) -0.1421(4) 0.076(2) Uani 1 1 d . . . H34 H 0.1964 0.1146 -0.1812 0.092 Uiso 1 1 calc R . . C35 C 0.3454(5) 0.0958(3) -0.1008(4) 0.0697(19) Uani 1 1 d . . . H35 H 0.3445 0.0479 -0.1116 0.084 Uiso 1 1 calc R . . C36 C 0.4346(4) 0.1294(3) -0.0429(4) 0.0543(15) Uani 1 1 d . . . H36 H 0.4939 0.1030 -0.0152 0.065 Uiso 1 1 calc R . . N1 N 1.1157(3) 0.2307(2) 0.5342(3) 0.0371(10) Uani 1 1 d . . . N2 N 1.0759(3) 0.36234(18) 0.4828(3) 0.0334(9) Uani 1 1 d . . . N3 N 0.4593(3) 0.33111(19) 0.0206(3) 0.0331(9) Uani 1 1 d . . . N4 N 0.4390(3) 0.1979(2) -0.0253(3) 0.0408(10) Uani 1 1 d . . . Ni1 Ni 0.97934(4) 0.27802(3) 0.44828(4) 0.02796(16) Uani 1 1 d . . . Ni2 Ni 0.56969(4) 0.25564(3) 0.05047(4) 0.02912(16) Uani 1 1 d . . . O1 O 0.8592(2) 0.34035(13) 0.3717(2) 0.0309(7) Uani 1 1 d . . . O2 O 0.72491(19) 0.27129(13) 0.3481(2) 0.0289(7) Uani 1 1 d . . . O3 O 0.4558(3) 0.59044(18) 0.2785(3) 0.0897(16) Uani 1 1 d . . . O4 O 0.5208(4) 0.6175(2) 0.1783(4) 0.117(2) Uani 1 1 d . . . O7 O 0.9589(2) 0.64151(16) 0.2512(2) 0.0480(9) Uani 1 1 d . . . O8 O 1.0690(3) 0.59442(16) 0.1958(3) 0.0585(11) Uani 1 1 d . . . O5 O 0.6787(2) 0.32935(13) 0.1198(2) 0.0316(7) Uani 1 1 d . . . O6 O 0.8246(2) 0.27314(13) 0.1449(2) 0.0376(8) Uani 1 1 d . . . O1W O 0.9475(3) 0.29387(18) 0.5704(2) 0.0480(9) Uani 1 1 d D . . H1WA H 0.9872 0.3230 0.6052 0.072 Uiso 1 1 calc R . . O2W O 0.8917(2) 0.18841(15) 0.4212(3) 0.0373(8) Uani 1 1 d D . . H2WA H 0.8313 0.1986 0.3921 0.056 Uiso 1 1 calc R . . O3W O 1.0038(2) 0.26339(16) 0.3213(2) 0.0352(8) Uani 1 1 d D . . H3WA H 0.9515 0.2734 0.2749 0.053 Uiso 1 1 calc R . . O4W O 0.5600(3) 0.23057(15) 0.1809(2) 0.0402(8) Uani 1 1 d . . . H4WA H 0.5537 0.1881 0.1842 0.060 Uiso 1 1 calc R . . O5W O 0.6755(2) 0.17785(16) 0.0640(3) 0.0411(8) Uani 1 1 d D . . H5WA H 0.7334 0.1941 0.0893 0.062 Uiso 1 1 calc R . . O6W O 0.5840(3) 0.27802(18) -0.0773(2) 0.0473(9) Uani 1 1 d D . . H6WA H 0.5436 0.3091 -0.1057 0.071 Uiso 1 1 calc R . . O7W O 0.7198(4) 0.0643(2) 0.1869(4) 0.0745(12) Uani 1 1 d D . . O8W O 0.2386(12) 0.5544(7) 0.0866(9) 0.555(13) Uani 1 1 d . . . H1WB H 0.903(3) 0.2677(18) 0.581(3) 0.048(15) Uiso 1 1 d D . . H4WB H 0.614(4) 0.251(3) 0.238(4) 0.09(2) Uiso 1 1 d . . . H2WB H 0.907(5) 0.157(3) 0.383(4) 0.13(3) Uiso 1 1 d D . . H6WB H 0.625(4) 0.257(3) -0.101(4) 0.12(3) Uiso 1 1 d D . . H3WB H 1.009(4) 0.2193(13) 0.304(4) 0.08(2) Uiso 1 1 d D . . H5WB H 0.694(4) 0.143(2) 0.107(4) 0.11(3) Uiso 1 1 d D . . H7WB H 0.762(5) 0.042(4) 0.242(4) 0.20(5) Uiso 1 1 d D . . H7WA H 0.651(2) 0.063(4) 0.149(5) 0.16(4) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.047(3) 0.048(3) 0.050(4) 0.014(3) 0.024(3) 0.018(3) C2 0.067(4) 0.068(4) 0.053(4) 0.026(3) 0.031(4) 0.033(3) C3 0.040(4) 0.101(5) 0.043(4) 0.015(4) 0.015(3) 0.032(3) C4 0.034(3) 0.081(4) 0.041(4) 0.003(3) 0.008(3) 0.006(3) C5 0.028(3) 0.066(4) 0.019(3) 0.001(2) 0.008(2) 0.006(3) C6 0.025(3) 0.058(3) 0.025(3) -0.010(2) 0.007(2) -0.003(2) C7 0.026(3) 0.076(4) 0.041(4) -0.023(3) 0.002(3) -0.008(3) C8 0.042(4) 0.057(4) 0.060(4) -0.027(3) 0.017(3) -0.026(3) C9 0.054(4) 0.044(3) 0.046(4) -0.010(3) 0.020(3) -0.016(3) C10 0.031(3) 0.042(3) 0.047(4) -0.002(3) 0.013(3) -0.009(2) C11 0.025(3) 0.020(2) 0.027(3) -0.0050(19) 0.014(2) -0.0004(19) C12 0.022(2) 0.017(2) 0.025(3) -0.0023(18) 0.009(2) -0.0032(17) C13 0.031(3) 0.025(2) 0.033(3) 0.008(2) 0.017(2) 0.0011(19) C14 0.020(2) 0.034(3) 0.039(3) -0.001(2) 0.015(2) 0.0031(19) C15 0.029(3) 0.024(2) 0.026(3) -0.002(2) 0.011(2) 0.0047(19) C16 0.047(3) 0.043(3) 0.050(4) 0.015(3) 0.032(3) 0.016(2) C17 0.028(3) 0.021(2) 0.033(3) 0.001(2) 0.014(2) 0.0014(18) C18 0.020(2) 0.019(2) 0.019(2) -0.0019(18) 0.0079(19) -0.0007(17) C19 0.025(2) 0.021(2) 0.026(3) 0.0030(19) 0.009(2) -0.0015(18) C20 0.028(3) 0.024(2) 0.026(3) 0.002(2) 0.009(2) 0.0041(19) C21 0.024(3) 0.033(3) 0.032(3) 0.002(2) 0.010(2) -0.006(2) C22 0.035(3) 0.040(3) 0.040(3) 0.004(2) 0.006(3) -0.015(2) C23 0.035(3) 0.037(3) 0.066(4) 0.000(3) 0.030(3) -0.003(2) C24 0.037(3) 0.034(3) 0.053(4) -0.010(2) 0.027(3) -0.005(2) C25 0.024(3) 0.020(2) 0.032(3) 0.0006(19) 0.011(2) -0.0029(18) C26 0.029(3) 0.026(2) 0.021(3) 0.0008(19) 0.010(2) 0.001(2) C27 0.032(3) 0.053(3) 0.036(3) 0.000(3) 0.011(2) 0.002(2) C28 0.053(4) 0.057(4) 0.041(4) 0.012(3) 0.017(3) 0.022(3) C29 0.037(3) 0.088(5) 0.039(4) 0.018(3) 0.015(3) 0.024(3) C30 0.033(3) 0.088(4) 0.026(3) 0.010(3) 0.007(3) 0.006(3) C31 0.028(3) 0.064(4) 0.029(3) -0.001(3) 0.016(3) -0.004(3) C32 0.030(3) 0.078(4) 0.026(3) -0.009(3) 0.012(3) -0.016(3) C33 0.032(3) 0.121(5) 0.040(4) -0.023(4) 0.018(3) -0.031(3) C34 0.067(5) 0.125(6) 0.047(4) -0.041(4) 0.033(4) -0.064(4) C35 0.083(5) 0.083(5) 0.064(5) -0.041(4) 0.052(4) -0.050(4) C36 0.061(4) 0.055(4) 0.054(4) -0.024(3) 0.031(3) -0.026(3) N1 0.028(2) 0.049(3) 0.037(3) 0.005(2) 0.016(2) 0.0092(19) N2 0.029(2) 0.034(2) 0.033(3) -0.0021(19) 0.008(2) -0.0033(17) N3 0.027(2) 0.049(3) 0.023(2) -0.0042(19) 0.0096(19) -0.0030(18) N4 0.042(3) 0.052(3) 0.031(3) -0.015(2) 0.018(2) -0.015(2) Ni1 0.0237(3) 0.0291(3) 0.0303(4) 0.0014(3) 0.0097(3) 0.0018(2) Ni2 0.0265(3) 0.0319(3) 0.0285(4) -0.0042(3) 0.0103(3) -0.0042(3) O1 0.0181(17) 0.0277(16) 0.043(2) 0.0051(14) 0.0085(15) -0.0011(13) O2 0.0257(17) 0.0194(16) 0.041(2) 0.0031(13) 0.0124(15) -0.0032(12) O3 0.127(4) 0.061(3) 0.125(4) 0.034(2) 0.097(4) 0.054(2) O4 0.157(5) 0.097(3) 0.149(5) 0.087(3) 0.118(4) 0.091(3) O7 0.057(2) 0.0337(19) 0.057(3) -0.0106(18) 0.026(2) -0.0152(17) O8 0.043(2) 0.045(2) 0.094(3) 0.012(2) 0.035(2) -0.0124(17) O5 0.0198(17) 0.0306(17) 0.040(2) -0.0061(14) 0.0065(15) -0.0014(13) O6 0.0300(18) 0.0226(16) 0.062(2) -0.0072(15) 0.0204(17) 0.0027(13) O1W 0.046(2) 0.060(3) 0.048(3) -0.0102(18) 0.028(2) -0.0256(18) O2W 0.0336(19) 0.0287(18) 0.049(3) 0.0054(16) 0.0159(19) 0.0035(14) O3W 0.035(2) 0.035(2) 0.034(2) -0.0014(16) 0.0114(16) 0.0063(15) O4W 0.046(2) 0.041(2) 0.031(2) -0.0034(16) 0.0125(17) -0.0185(17) O5W 0.039(2) 0.035(2) 0.044(2) -0.0066(18) 0.0098(19) -0.0009(15) O6W 0.061(3) 0.053(2) 0.039(2) 0.0149(17) 0.031(2) 0.0296(18) O7W 0.075(4) 0.061(3) 0.088(4) 0.008(3) 0.032(3) 0.001(2) O8W 0.76(3) 0.490(19) 0.292(16) -0.054(13) 0.076(17) 0.45(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 C1 N1 1.340(5) . ? C1 C2 1.374(7) . ? C1 H1 0.9300 . ? C2 C3 1.370(7) . ? C2 H2 0.9300 . ? C3 C4 1.370(7) . ? C3 H3 0.9300 . ? C4 C5 1.381(6) . ? C4 H4 0.9300 . ? C5 N1 1.354(5) . ? C5 C6 1.482(6) . ? C6 N2 1.351(5) . ? C6 C7 1.376(6) . ? C7 C8 1.373(7) . ? C7 H7 0.9300 . ? C8 C9 1.361(7) . ? C8 H8 0.9300 . ? C9 C10 1.380(6) . ? C9 H9 0.9300 . ? C10 N2 1.328(5) . ? C10 H10 0.9300 . ? C11 O1 1.252(4) . ? C11 O2 1.269(4) . ? C11 C12 1.500(5) . ? C12 C13 1.388(5) . ? C12 C18 1.408(5) . ? C13 C14 1.381(5) . ? C13 H13 0.9300 . ? C14 C15 1.382(5) . ? C14 H14 0.9300 . ? C15 C17 1.383(5) . ? C15 C16 1.505(6) . ? C16 O4 1.205(5) . ? C16 O3 1.212(5) . ? C17 C18 1.392(5) . ? C17 H17 0.9300 . ? C18 C19 1.502(5) . ? C19 C20 1.391(5) . ? C19 C25 1.395(5) . ? C20 C21 1.403(5) . ? C20 H20 0.9300 . ? C21 C23 1.373(5) . ? C21 C22 1.513(5) . ? C22 O8 1.258(5) . ? C22 O7 1.261(5) . ? C23 C24 1.376(5) . ? C23 H23 0.9300 . ? C24 C25 1.390(5) . ? C24 H24 0.9300 . ? C25 C26 1.516(5) . ? C26 O5 1.251(4) . ? C26 O6 1.267(4) . ? C27 N3 1.332(5) . ? C27 C28 1.383(6) . ? C27 H27 0.9300 . ? C28 C29 1.355(7) . ? C28 H28 0.9300 . ? C29 C30 1.368(7) . ? C29 H29 0.9300 . ? C30 C31 1.396(6) . ? C30 H30 0.9300 . ? C31 N3 1.354(5) . ? C31 C32 1.460(6) . ? C32 N4 1.359(6) . ? C32 C33 1.386(6) . ? C33 C34 1.375(8) . ? C33 H33 0.9300 . ? C34 C35 1.382(8) . ? C34 H34 0.9300 . ? C35 C36 1.384(7) . ? C35 H35 0.9300 . ? C36 N4 1.332(5) . ? C36 H36 0.9300 . ? N1 Ni1 2.071(4) . ? N2 Ni1 2.047(3) . ? N3 Ni2 2.047(4) . ? N4 Ni2 2.077(4) . ? Ni1 O1 2.031(3) . ? Ni1 O2W 2.062(3) . ? Ni1 O1W 2.091(3) . ? Ni1 O3W 2.103(3) . ? Ni2 O5 2.052(3) . ? Ni2 O5W 2.067(3) . ? Ni2 O6W 2.068(3) . ? Ni2 O4W 2.089(3) . ? O1W H1WA 0.8200 . ? O1W H1WB 0.874(19) . ? O2W H2WA 0.8200 . ? O2W H2WB 0.92(2) . ? O3W H3WA 0.8200 . ? O3W H3WB 0.893(19) . ? O4W H4WA 0.8200 . ? O4W H4WB 0.99(6) . ? O5W H5WA 0.8200 . ? O5W H5WB 0.90(2) . ? O6W H6WA 0.8200 . ? O6W H6WB 0.88(2) . ? O7W H7WB 0.91(2) . ? O7W H7WA 0.92(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 122.5(5) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C3 C2 C1 119.4(5) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C4 C3 C2 118.8(5) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 C5 120.0(5) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? N1 C5 C4 121.2(5) . . ? N1 C5 C6 115.1(4) . . ? C4 C5 C6 123.7(5) . . ? N2 C6 C7 120.8(5) . . ? N2 C6 C5 114.8(4) . . ? C7 C6 C5 124.3(5) . . ? C8 C7 C6 119.3(5) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? C9 C8 C7 120.0(5) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 118.3(5) . . ? C8 C9 H9 120.8 . . ? C10 C9 H9 120.8 . . ? N2 C10 C9 122.4(5) . . ? N2 C10 H10 118.8 . . ? C9 C10 H10 118.8 . . ? O1 C11 O2 124.5(4) . . ? O1 C11 C12 117.3(3) . . ? O2 C11 C12 118.1(4) . . ? C13 C12 C18 118.9(3) . . ? C13 C12 C11 118.3(3) . . ? C18 C12 C11 122.8(3) . . ? C14 C13 C12 122.2(4) . . ? C14 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? C13 C14 C15 119.8(4) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C14 C15 C17 117.9(4) . . ? C14 C15 C16 122.0(4) . . ? C17 C15 C16 120.1(4) . . ? O4 C16 O3 123.2(5) . . ? O4 C16 C15 117.3(4) . . ? O3 C16 C15 119.1(4) . . ? C15 C17 C18 123.8(4) . . ? C15 C17 H17 118.1 . . ? C18 C17 H17 118.1 . . ? C17 C18 C12 117.2(4) . . ? C17 C18 C19 117.0(3) . . ? C12 C18 C19 125.8(3) . . ? C20 C19 C25 117.8(4) . . ? C20 C19 C18 117.3(3) . . ? C25 C19 C18 124.9(3) . . ? C19 C20 C21 122.3(4) . . ? C19 C20 H20 118.8 . . ? C21 C20 H20 118.8 . . ? C23 C21 C20 118.2(4) . . ? C23 C21 C22 121.0(4) . . ? C20 C21 C22 120.7(4) . . ? O8 C22 O7 125.1(4) . . ? O8 C22 C21 116.7(4) . . ? O7 C22 C21 118.1(4) . . ? C21 C23 C24 120.6(4) . . ? C21 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C23 C24 C25 121.1(4) . . ? C23 C24 H24 119.4 . . ? C25 C24 H24 119.4 . . ? C24 C25 C19 119.9(4) . . ? C24 C25 C26 116.0(4) . . ? C19 C25 C26 124.0(4) . . ? O5 C26 O6 125.0(4) . . ? O5 C26 C25 118.3(3) . . ? O6 C26 C25 116.7(4) . . ? N3 C27 C28 122.9(5) . . ? N3 C27 H27 118.6 . . ? C28 C27 H27 118.6 . . ? C29 C28 C27 119.0(5) . . ? C29 C28 H28 120.5 . . ? C27 C28 H28 120.5 . . ? C28 C29 C30 119.2(5) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? C29 C30 C31 120.0(5) . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? N3 C31 C30 120.3(5) . . ? N3 C31 C32 114.9(4) . . ? C30 C31 C32 124.7(5) . . ? N4 C32 C33 120.0(5) . . ? N4 C32 C31 115.8(4) . . ? C33 C32 C31 124.2(5) . . ? C34 C33 C32 120.4(6) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 119.2(6) . . ? C33 C34 H34 120.4 . . ? C35 C34 H34 120.4 . . ? C34 C35 C36 118.2(6) . . ? C34 C35 H35 120.9 . . ? C36 C35 H35 120.9 . . ? N4 C36 C35 122.7(6) . . ? N4 C36 H36 118.6 . . ? C35 C36 H36 118.6 . . ? C1 N1 C5 118.2(4) . . ? C1 N1 Ni1 126.7(3) . . ? C5 N1 Ni1 114.7(3) . . ? C10 N2 C6 119.2(4) . . ? C10 N2 Ni1 124.9(3) . . ? C6 N2 Ni1 115.9(3) . . ? C27 N3 C31 118.5(4) . . ? C27 N3 Ni2 125.8(3) . . ? C31 N3 Ni2 115.6(3) . . ? C36 N4 C32 119.5(4) . . ? C36 N4 Ni2 126.4(4) . . ? C32 N4 Ni2 113.9(3) . . ? O1 Ni1 N2 90.85(13) . . ? O1 Ni1 O2W 93.73(11) . . ? N2 Ni1 O2W 175.37(14) . . ? O1 Ni1 N1 169.96(13) . . ? N2 Ni1 N1 79.23(15) . . ? O2W Ni1 N1 96.17(14) . . ? O1 Ni1 O1W 89.68(13) . . ? N2 Ni1 O1W 90.95(13) . . ? O2W Ni1 O1W 88.37(13) . . ? N1 Ni1 O1W 88.98(14) . . ? O1 Ni1 O3W 87.69(12) . . ? N2 Ni1 O3W 90.18(13) . . ? O2W Ni1 O3W 90.70(13) . . ? N1 Ni1 O3W 93.80(13) . . ? O1W Ni1 O3W 177.15(14) . . ? N3 Ni2 O5 89.44(13) . . ? N3 Ni2 O5W 173.52(15) . . ? O5 Ni2 O5W 93.88(11) . . ? N3 Ni2 O6W 89.80(13) . . ? O5 Ni2 O6W 90.31(14) . . ? O5W Ni2 O6W 84.62(14) . . ? N3 Ni2 N4 78.99(16) . . ? O5 Ni2 N4 168.43(14) . . ? O5W Ni2 N4 97.61(15) . . ? O6W Ni2 N4 89.32(15) . . ? N3 Ni2 O4W 92.33(13) . . ? O5 Ni2 O4W 89.43(12) . . ? O5W Ni2 O4W 93.27(14) . . ? O6W Ni2 O4W 177.85(13) . . ? N4 Ni2 O4W 91.37(13) . . ? C11 O1 Ni1 130.3(2) . . ? C26 O5 Ni2 130.1(2) . . ? Ni1 O1W H1WA 109.5 . . ? Ni1 O1W H1WB 121(3) . . ? H1WA O1W H1WB 129.3 . . ? Ni1 O2W H2WA 109.5 . . ? Ni1 O2W H2WB 114(4) . . ? H2WA O2W H2WB 105.7 . . ? Ni1 O3W H3WA 109.5 . . ? Ni1 O3W H3WB 117(3) . . ? H3WA O3W H3WB 96.8 . . ? Ni2 O4W H4WA 109.5 . . ? Ni2 O4W H4WB 115(3) . . ? H4WA O4W H4WB 113.5 . . ? Ni2 O5W H5WA 109.5 . . ? Ni2 O5W H5WB 127(4) . . ? H5WA O5W H5WB 89.4 . . ? Ni2 O6W H6WA 109.5 . . ? Ni2 O6W H6WB 128(4) . . ? H6WA O6W H6WB 122.9 . . ? H7WB O7W H7WA 135(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 1.0(8) . . . . ? C1 C2 C3 C4 -0.3(8) . . . . ? C2 C3 C4 C5 -0.3(8) . . . . ? C3 C4 C5 N1 0.3(7) . . . . ? C3 C4 C5 C6 -179.2(4) . . . . ? N1 C5 C6 N2 4.7(6) . . . . ? C4 C5 C6 N2 -175.8(4) . . . . ? N1 C5 C6 C7 -172.4(4) . . . . ? C4 C5 C6 C7 7.1(7) . . . . ? N2 C6 C7 C8 0.6(7) . . . . ? C5 C6 C7 C8 177.5(4) . . . . ? C6 C7 C8 C9 -1.1(8) . . . . ? C7 C8 C9 C10 1.5(8) . . . . ? C8 C9 C10 N2 -1.4(7) . . . . ? O1 C11 C12 C13 -143.6(4) . . . . ? O2 C11 C12 C13 35.7(6) . . . . ? O1 C11 C12 C18 32.7(6) . . . . ? O2 C11 C12 C18 -148.1(4) . . . . ? C18 C12 C13 C14 -3.4(6) . . . . ? C11 C12 C13 C14 173.0(4) . . . . ? C12 C13 C14 C15 1.5(7) . . . . ? C13 C14 C15 C17 1.8(6) . . . . ? C13 C14 C15 C16 -175.5(4) . . . . ? C14 C15 C16 O4 -167.6(5) . . . . ? C17 C15 C16 O4 15.2(8) . . . . ? C14 C15 C16 O3 19.2(8) . . . . ? C17 C15 C16 O3 -158.0(5) . . . . ? C14 C15 C17 C18 -3.1(6) . . . . ? C16 C15 C17 C18 174.2(4) . . . . ? C15 C17 C18 C12 1.2(6) . . . . ? C15 C17 C18 C19 -178.9(4) . . . . ? C13 C12 C18 C17 2.0(6) . . . . ? C11 C12 C18 C17 -174.2(4) . . . . ? C13 C12 C18 C19 -177.9(4) . . . . ? C11 C12 C18 C19 5.9(6) . . . . ? C17 C18 C19 C20 47.2(5) . . . . ? C12 C18 C19 C20 -132.9(4) . . . . ? C17 C18 C19 C25 -129.6(4) . . . . ? C12 C18 C19 C25 50.3(6) . . . . ? C25 C19 C20 C21 1.5(6) . . . . ? C18 C19 C20 C21 -175.6(4) . . . . ? C19 C20 C21 C23 -3.7(6) . . . . ? C19 C20 C21 C22 172.1(4) . . . . ? C23 C21 C22 O8 -6.4(7) . . . . ? C20 C21 C22 O8 177.9(4) . . . . ? C23 C21 C22 O7 169.5(5) . . . . ? C20 C21 C22 O7 -6.2(7) . . . . ? C20 C21 C23 C24 2.7(7) . . . . ? C22 C21 C23 C24 -173.1(4) . . . . ? C21 C23 C24 C25 0.4(7) . . . . ? C23 C24 C25 C19 -2.6(7) . . . . ? C23 C24 C25 C26 174.7(4) . . . . ? C20 C19 C25 C24 1.7(6) . . . . ? C18 C19 C25 C24 178.5(4) . . . . ? C20 C19 C25 C26 -175.4(4) . . . . ? C18 C19 C25 C26 1.4(7) . . . . ? C24 C25 C26 O5 -143.6(4) . . . . ? C19 C25 C26 O5 33.6(6) . . . . ? C24 C25 C26 O6 36.2(6) . . . . ? C19 C25 C26 O6 -146.6(4) . . . . ? N3 C27 C28 C29 -1.7(8) . . . . ? C27 C28 C29 C30 -0.6(8) . . . . ? C28 C29 C30 C31 2.8(8) . . . . ? C29 C30 C31 N3 -2.9(7) . . . . ? C29 C30 C31 C32 175.5(4) . . . . ? N3 C31 C32 N4 1.7(6) . . . . ? C30 C31 C32 N4 -176.7(4) . . . . ? N3 C31 C32 C33 179.6(4) . . . . ? C30 C31 C32 C33 1.1(8) . . . . ? N4 C32 C33 C34 1.1(7) . . . . ? C31 C32 C33 C34 -176.7(5) . . . . ? C32 C33 C34 C35 -0.9(8) . . . . ? C33 C34 C35 C36 0.2(9) . . . . ? C34 C35 C36 N4 0.3(8) . . . . ? C2 C1 N1 C5 -1.1(7) . . . . ? C2 C1 N1 Ni1 -173.9(4) . . . . ? C4 C5 N1 C1 0.4(7) . . . . ? C6 C5 N1 C1 180.0(4) . . . . ? C4 C5 N1 Ni1 174.1(3) . . . . ? C6 C5 N1 Ni1 -6.4(5) . . . . ? C9 C10 N2 C6 0.9(7) . . . . ? C9 C10 N2 Ni1 -175.8(3) . . . . ? C7 C6 N2 C10 -0.4(7) . . . . ? C5 C6 N2 C10 -177.6(4) . . . . ? C7 C6 N2 Ni1 176.5(3) . . . . ? C5 C6 N2 Ni1 -0.6(5) . . . . ? C28 C27 N3 C31 1.7(7) . . . . ? C28 C27 N3 Ni2 178.3(3) . . . . ? C30 C31 N3 C27 0.6(6) . . . . ? C32 C31 N3 C27 -177.9(4) . . . . ? C30 C31 N3 Ni2 -176.3(3) . . . . ? C32 C31 N3 Ni2 5.1(5) . . . . ? C35 C36 N4 C32 -0.1(7) . . . . ? C35 C36 N4 Ni2 -174.5(4) . . . . ? C33 C32 N4 C36 -0.6(7) . . . . ? C31 C32 N4 C36 177.3(4) . . . . ? C33 C32 N4 Ni2 174.5(3) . . . . ? C31 C32 N4 Ni2 -7.5(5) . . . . ? C10 N2 Ni1 O1 -6.8(4) . . . . ? C6 N2 Ni1 O1 176.4(3) . . . . ? C10 N2 Ni1 O2W -178(61) . . . . ? C6 N2 Ni1 O2W 5.1(19) . . . . ? C10 N2 Ni1 N1 174.7(4) . . . . ? C6 N2 Ni1 N1 -2.1(3) . . . . ? C10 N2 Ni1 O1W -96.5(4) . . . . ? C6 N2 Ni1 O1W 86.7(3) . . . . ? C10 N2 Ni1 O3W 80.9(4) . . . . ? C6 N2 Ni1 O3W -95.9(3) . . . . ? C1 N1 Ni1 O1 168.9(6) . . . . ? C5 N1 Ni1 O1 -4.2(9) . . . . ? C1 N1 Ni1 N2 177.7(4) . . . . ? C5 N1 Ni1 N2 4.7(3) . . . . ? C1 N1 Ni1 O2W -1.7(4) . . . . ? C5 N1 Ni1 O2W -174.7(3) . . . . ? C1 N1 Ni1 O1W 86.6(4) . . . . ? C5 N1 Ni1 O1W -86.5(3) . . . . ? C1 N1 Ni1 O3W -92.8(4) . . . . ? C5 N1 Ni1 O3W 94.1(3) . . . . ? C27 N3 Ni2 O5 -4.1(4) . . . . ? C31 N3 Ni2 O5 172.6(3) . . . . ? C27 N3 Ni2 O5W -124.9(12) . . . . ? C31 N3 Ni2 O5W 51.8(13) . . . . ? C27 N3 Ni2 O6W -94.4(4) . . . . ? C31 N3 Ni2 O6W 82.3(3) . . . . ? C27 N3 Ni2 N4 176.3(4) . . . . ? C31 N3 Ni2 N4 -7.0(3) . . . . ? C27 N3 Ni2 O4W 85.3(4) . . . . ? C31 N3 Ni2 O4W -98.0(3) . . . . ? C36 N4 Ni2 N3 -177.5(4) . . . . ? C32 N4 Ni2 N3 7.8(3) . . . . ? C36 N4 Ni2 O5 -179.2(5) . . . . ? C32 N4 Ni2 O5 6.1(9) . . . . ? C36 N4 Ni2 O5W 8.1(4) . . . . ? C32 N4 Ni2 O5W -166.6(3) . . . . ? C36 N4 Ni2 O6W 92.6(4) . . . . ? C32 N4 Ni2 O6W -82.1(3) . . . . ? C36 N4 Ni2 O4W -85.3(4) . . . . ? C32 N4 Ni2 O4W 99.9(3) . . . . ? O2 C11 O1 Ni1 -11.0(6) . . . . ? C12 C11 O1 Ni1 168.2(3) . . . . ? N2 Ni1 O1 C11 -161.4(4) . . . . ? O2W Ni1 O1 C11 17.9(4) . . . . ? N1 Ni1 O1 C11 -152.8(7) . . . . ? O1W Ni1 O1 C11 -70.5(4) . . . . ? O3W Ni1 O1 C11 108.4(4) . . . . ? O6 C26 O5 Ni2 -12.4(6) . . . . ? C25 C26 O5 Ni2 167.3(3) . . . . ? N3 Ni2 O5 C26 -163.9(4) . . . . ? O5W Ni2 O5 C26 10.5(4) . . . . ? O6W Ni2 O5 C26 -74.1(4) . . . . ? N4 Ni2 O5 C26 -162.2(6) . . . . ? O4W Ni2 O5 C26 103.7(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6W H6WA O4 0.82 1.80 2.598(5) 165.9 3_665 O5W H5WA O6 0.82 1.95 2.696(4) 150.3 . O4W H4WA O3 0.82 1.97 2.774(5) 167.5 2_645 O3W H3WA O6 0.82 2.08 2.885(4) 165.2 . O2W H2WA O2 0.82 1.97 2.701(4) 148.6 . O1W H1WA O7 0.82 2.11 2.788(5) 139.4 3_766 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.480 _refine_diff_density_min -0.484 _refine_diff_density_rms 0.078 #===========================end data_complex-2 #TrackingRef '- 1-5.cif' _database_code_depnum_ccdc_archive 'CCDC 735924' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H40 Ni2 O25' _chemical_formula_sum 'C16 H40 Ni2 O25' _chemical_formula_weight 749.86 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.1584(5) _cell_length_b 17.1511(5) _cell_length_c 14.6293(5) _cell_angle_alpha 90.00 _cell_angle_beta 107.968(4) _cell_angle_gamma 90.00 _cell_volume 3140.53(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 4.35 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 1.293 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.642 _exptl_absorpt_correction_T_max 0.752 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'BRUKER SMART CCD Apex II' _diffrn_measurement_method 'omega and phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6052 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0632 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.35 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2754 _reflns_number_gt 1901 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SMART (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2754 _refine_ls_number_parameters 217 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0781 _refine_ls_wR_factor_gt 0.0751 _refine_ls_goodness_of_fit_ref 0.902 _refine_ls_restrained_S_all 0.935 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O3 O 0.66403(17) 0.82829(12) 0.14498(17) 0.0360(6) Uani 1 1 d . . . O7W O 0.5000 0.4108(3) 0.2500 0.133(2) Uani 1 2 d S . . Ni1 Ni 0.75399(3) 0.73556(2) 0.15827(3) 0.02400(14) Uani 1 1 d D . . O1 O 0.96485(17) 0.72684(12) 0.11768(17) 0.0358(6) Uani 1 1 d . . . C3 C 1.0231(2) 0.53114(15) 0.2098(2) 0.0192(6) Uani 1 1 d . . . C1 C 0.9397(2) 0.66167(17) 0.1422(2) 0.0243(7) Uani 1 1 d . . . C2 C 1.0121(2) 0.59345(16) 0.1451(2) 0.0204(7) Uani 1 1 d . . . C8 C 0.6918(3) 0.89232(18) 0.1138(2) 0.0292(8) Uani 1 1 d . . . C4 C 1.0814(2) 0.46641(17) 0.1971(2) 0.0241(7) Uani 1 1 d . . . H4 H 1.0863 0.4234 0.2370 0.029 Uiso 1 1 calc R . . C7 C 1.0665(2) 0.59205(17) 0.0780(2) 0.0277(7) Uani 1 1 d . . . H7 H 1.0620 0.6348 0.0379 0.033 Uiso 1 1 calc R . . C6 C 1.1275(2) 0.52866(18) 0.0692(2) 0.0301(8) Uani 1 1 d . . . H6 H 1.1651 0.5295 0.0248 0.036 Uiso 1 1 calc R . . O5W O 0.7531(2) 0.35235(16) 0.1059(2) 0.0611(8) Uani 1 1 d . . . O3W O 0.6625(4) 0.6604(3) 0.2311(3) 0.0833(14) Uani 1 1 d D . . C5 C 1.1323(2) 0.46383(16) 0.1268(2) 0.0237(7) Uani 1 1 d . . . O8W O 0.6269(3) 0.3524(2) 0.9145(3) 0.0994(12) Uani 1 1 d . . . O4W O 0.7133(4) 0.5113(2) 0.1056(3) 0.1207(16) Uani 1 1 d . . . O4 O 0.7619(2) 0.89762(14) 0.0746(2) 0.0524(7) Uani 1 1 d . . . O2W O 0.66287(19) 0.69543(13) 0.03494(17) 0.0383(6) Uani 1 1 d . . . H2WA H 0.6965 0.6637 0.0138 0.057 Uiso 1 1 calc R . . O1W O 0.8454(2) 0.78337(16) 0.2771(2) 0.0534(8) Uani 1 1 d . . . H1WA H 0.8887 0.7511 0.3076 0.080 Uiso 1 1 calc R . . O9W O 0.4985(9) 0.4785(5) 0.8897(8) 0.312(6) Uani 1 1 d . . . O6W O 0.9568(3) 0.2902(2) 0.1472(3) 0.0761(10) Uani 1 1 d . . . O2 O 0.85291(16) 0.64911(12) 0.16127(16) 0.0300(5) Uani 1 1 d . . . H2WB H 0.616(4) 0.729(3) -0.011(4) 0.11(2) Uiso 1 1 d . . . H1WB H 0.811(6) 0.805(4) 0.319(5) 0.17(3) Uiso 1 1 d . . . H6WB H 0.927(4) 0.240(3) 0.113(4) 0.088(16) Uiso 1 1 d . . . H6WA H 1.029(8) 0.288(5) 0.160(7) 0.24(5) Uiso 1 1 d . . . H3WA H 0.656(4) 0.653(3) 0.269(3) 0.046(16) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O3 0.0326(12) 0.0232(12) 0.0530(16) -0.0027(11) 0.0146(11) 0.0101(10) O7W 0.107(4) 0.084(4) 0.217(8) 0.000 0.062(5) 0.000 Ni1 0.0247(2) 0.0196(2) 0.0278(2) -0.00056(19) 0.00837(15) 0.00973(18) O1 0.0345(12) 0.0191(11) 0.0486(14) 0.0107(11) 0.0052(11) 0.0038(10) C3 0.0185(15) 0.0144(14) 0.0229(16) -0.0022(12) 0.0037(13) -0.0024(11) C1 0.0219(16) 0.0244(17) 0.0218(17) -0.0013(13) -0.0004(14) 0.0041(13) C2 0.0190(15) 0.0173(14) 0.0234(16) 0.0001(13) 0.0043(13) 0.0005(12) C8 0.0288(18) 0.0268(18) 0.0308(19) -0.0063(14) 0.0071(15) 0.0052(14) C4 0.0261(16) 0.0205(15) 0.0256(17) 0.0013(13) 0.0081(14) -0.0008(13) C7 0.0338(18) 0.0245(16) 0.0282(18) 0.0055(14) 0.0145(15) 0.0015(14) C6 0.0320(18) 0.0326(18) 0.0321(19) -0.0008(15) 0.0191(16) 0.0017(14) O5W 0.0640(18) 0.0608(18) 0.0576(19) 0.0085(14) 0.0177(15) -0.0063(14) O3W 0.100(3) 0.097(3) 0.071(3) 0.016(2) 0.052(2) -0.014(2) C5 0.0216(16) 0.0220(16) 0.0274(18) -0.0026(13) 0.0074(14) 0.0012(13) O8W 0.120(3) 0.093(3) 0.082(3) -0.015(2) 0.027(2) -0.015(2) O4W 0.134(3) 0.066(2) 0.144(4) 0.008(2) 0.016(3) -0.009(2) O4 0.0574(17) 0.0400(14) 0.078(2) -0.0061(13) 0.0475(16) 0.0087(12) O2W 0.0440(14) 0.0341(14) 0.0343(14) -0.0009(11) 0.0082(12) 0.0207(11) O1W 0.0465(16) 0.0523(18) 0.0502(17) -0.0177(13) -0.0012(13) 0.0212(13) O9W 0.402(12) 0.251(9) 0.390(12) 0.182(9) 0.281(11) 0.208(9) O6W 0.064(2) 0.068(2) 0.102(3) -0.0055(19) 0.033(2) -0.0023(18) O2 0.0262(12) 0.0257(12) 0.0393(14) 0.0040(10) 0.0117(11) 0.0105(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O3 C8 1.285(4) . ? O3 Ni1 1.956(2) . ? Ni1 O2W 1.958(2) . ? Ni1 O1W 1.963(2) . ? Ni1 O2 1.965(2) . ? Ni1 O3W 2.244(4) . ? O1 C1 1.249(4) . ? C3 C4 1.394(4) . ? C3 C2 1.405(4) . ? C3 C3 1.482(6) 2_755 ? C1 O2 1.275(4) . ? C1 C2 1.501(4) . ? C2 C7 1.382(4) . ? C8 O4 1.229(4) . ? C8 C5 1.499(4) 3_455 ? C4 C5 1.391(4) . ? C4 H4 0.9300 . ? C7 C6 1.380(4) . ? C7 H7 0.9300 . ? C6 C5 1.385(4) . ? C6 H6 0.9300 . ? O3W H3WA 0.60(5) . ? C5 C8 1.499(4) 3_545 ? O2W H2WA 0.8200 . ? O2W H2WB 0.95(6) . ? O1W H1WA 0.8200 . ? O1W H1WB 0.94(8) . ? O6W H6WB 1.01(5) . ? O6W H6WA 0.91(10) . ? 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 C8 O3 Ni1 120.0(2) . . ? O3 Ni1 O2W 90.83(10) . . ? O3 Ni1 O1W 86.28(10) . . ? O2W Ni1 O1W 175.68(12) . . ? O3 Ni1 O2 172.89(10) . . ? O2W Ni1 O2 88.19(9) . . ? O1W Ni1 O2 94.28(10) . . ? O3 Ni1 O3W 96.75(15) . . ? O2W Ni1 O3W 88.27(15) . . ? O1W Ni1 O3W 95.25(16) . . ? O2 Ni1 O3W 90.26(14) . . ? C4 C3 C2 117.6(3) . . ? C4 C3 C3 118.9(2) . 2_755 ? C2 C3 C3 123.6(2) . 2_755 ? O1 C1 O2 123.3(3) . . ? O1 C1 C2 118.9(3) . . ? O2 C1 C2 117.8(3) . . ? C7 C2 C3 119.8(3) . . ? C7 C2 C1 117.2(3) . . ? C3 C2 C1 123.0(3) . . ? O4 C8 O3 124.4(3) . . ? O4 C8 C5 119.7(3) . 3_455 ? O3 C8 C5 115.9(3) . 3_455 ? C5 C4 C3 122.3(3) . . ? C5 C4 H4 118.9 . . ? C3 C4 H4 118.9 . . ? C6 C7 C2 121.5(3) . . ? C6 C7 H7 119.2 . . ? C2 C7 H7 119.2 . . ? C7 C6 C5 119.7(3) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? Ni1 O3W H3WA 144(5) . . ? C6 C5 C4 118.8(3) . . ? C6 C5 C8 120.5(3) . 3_545 ? C4 C5 C8 120.7(3) . 3_545 ? Ni1 O2W H2WA 109.5 . . ? Ni1 O2W H2WB 121(3) . . ? H2WA O2W H2WB 115.8 . . ? Ni1 O1W H1WA 109.5 . . ? Ni1 O1W H1WB 117(4) . . ? H1WA O1W H1WB 108.1 . . ? H6WB O6W H6WA 107(6) . . ? C1 O2 Ni1 119.98(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C8 O3 Ni1 O2W -98.4(2) . . . . ? C8 O3 Ni1 O1W 78.4(2) . . . . ? C8 O3 Ni1 O2 -16.4(9) . . . . ? C8 O3 Ni1 O3W 173.3(3) . . . . ? C4 C3 C2 C7 -6.0(4) . . . . ? C3 C3 C2 C7 173.6(3) 2_755 . . . ? C4 C3 C2 C1 171.5(3) . . . . ? C3 C3 C2 C1 -8.9(5) 2_755 . . . ? O1 C1 C2 C7 -33.4(4) . . . . ? O2 C1 C2 C7 143.8(3) . . . . ? O1 C1 C2 C3 149.0(3) . . . . ? O2 C1 C2 C3 -33.8(4) . . . . ? Ni1 O3 C8 O4 13.7(4) . . . . ? Ni1 O3 C8 C5 -166.71(19) . . . 3_455 ? C2 C3 C4 C5 3.3(4) . . . . ? C3 C3 C4 C5 -176.2(3) 2_755 . . . ? C3 C2 C7 C6 3.5(4) . . . . ? C1 C2 C7 C6 -174.1(3) . . . . ? C2 C7 C6 C5 1.8(5) . . . . ? C7 C6 C5 C4 -4.4(4) . . . . ? C7 C6 C5 C8 175.8(3) . . . 3_545 ? C3 C4 C5 C6 1.8(4) . . . . ? C3 C4 C5 C8 -178.3(3) . . . 3_545 ? O1 C1 O2 Ni1 -2.7(4) . . . . ? C2 C1 O2 Ni1 -179.75(18) . . . . ? O3 Ni1 O2 C1 21.8(9) . . . . ? O2W Ni1 O2 C1 104.0(2) . . . . ? O1W Ni1 O2 C1 -72.5(2) . . . . ? O3W Ni1 O2 C1 -167.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.529 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.063 #===========================end data_complex-3 #TrackingRef '- 1-5.cif' _database_code_depnum_ccdc_archive 'CCDC 752213' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H22 Co N2 O11' _chemical_formula_sum 'C26 H22 Co N2 O11' _chemical_formula_weight 597.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2/n _symmetry_space_group_name_Hall P2/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 9.879(4) _cell_length_b 11.397(4) _cell_length_c 21.932(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.030(5) _cell_angle_gamma 90.00 _cell_volume 2465.9(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.01 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.604 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1220 _exptl_absorpt_coefficient_mu 0.765 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.766 _exptl_absorpt_correction_T_max 0.858 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'BRUKER SMART CCD Apex II' _diffrn_measurement_method 'omega and phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18633 _diffrn_reflns_av_R_equivalents 0.0452 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5593 _reflns_number_gt 4305 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SMART (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0384P)^2^+2.5826P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5593 _refine_ls_number_parameters 381 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0738 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1166 _refine_ls_wR_factor_gt 0.1058 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 1.2500 0.08537(4) 0.2500 0.02059(14) Uani 1 2 d S . . Co2 Co 0.7500 0.18245(5) 0.2500 0.02295(14) Uani 1 2 d S . . O7 O 0.63134(19) 0.19401(17) 0.33377(9) 0.0277(4) Uani 1 1 d . . . O1W O 1.4008(2) 0.0787(2) 0.31924(9) 0.0293(5) Uani 1 1 d . . . H1WA H 1.3672 0.0617 0.3515 0.044 Uiso 1 1 calc R . . O2 O 0.94062(19) 0.17820(17) 0.29238(9) 0.0263(4) Uani 1 1 d . . . O8 O 0.5249(2) 0.2700(2) 0.41200(10) 0.0374(5) Uani 1 1 d . . . C16 C 1.1009(4) 0.5427(4) 0.43363(16) 0.0516(10) Uani 1 1 d . . . C21 C 0.8511(4) 0.8083(3) 0.22525(19) 0.0515(11) Uani 1 1 d . . . H21 H 0.9228 0.7699 0.2080 0.062 Uiso 1 1 calc R . . O1 O 1.12257(18) 0.07487(17) 0.32307(9) 0.0279(4) Uani 1 1 d . . . O3 O 0.6884(3) -0.1748(2) 0.53116(12) 0.0508(7) Uani 1 1 d . . . H3 H 0.6276 -0.1919 0.5536 0.076 Uiso 1 1 calc R . . O4 O 0.6477(3) 0.0057(2) 0.56419(11) 0.0480(6) Uani 1 1 d . . . C17 C 0.8660(3) 0.4297(2) 0.25525(13) 0.0279(6) Uani 1 1 d . . . H17 H 0.9473 0.3886 0.2592 0.033 Uiso 1 1 calc R . . C27 C 1.2428(3) 0.8343(3) 0.30200(14) 0.0322(7) Uani 1 1 d . . . H27 H 1.2376 0.8753 0.3385 0.039 Uiso 1 1 calc R . . N3 N 0.7500 0.3688(3) 0.2500 0.0239(7) Uani 1 2 d S . . N1 N 1.2500 0.2734(3) 0.2500 0.0236(7) Uani 1 2 d S . . O6 O 1.0995(3) 0.6484(3) 0.42988(14) 0.0736(10) Uani 1 1 d . . . C15 C 0.6252(3) 0.2606(3) 0.37996(13) 0.0264(6) Uani 1 1 d . . . O5 O 1.2115(3) 0.4813(3) 0.44931(13) 0.0658(9) Uani 1 1 d . . . H5 H 1.2735 0.5263 0.4593 0.099 Uiso 1 1 calc R . . C23 C 1.2812(3) 0.4552(3) 0.30259(14) 0.0346(7) Uani 1 1 d . . . H23 H 1.3039 0.4935 0.3392 0.042 Uiso 1 1 calc R . . C8 C 0.7029(3) -0.0593(3) 0.52977(14) 0.0358(7) Uani 1 1 d . . . C26 C 1.2429(3) 0.7138(3) 0.30363(14) 0.0351(7) Uani 1 1 d . . . H26 H 1.2383 0.6750 0.3408 0.042 Uiso 1 1 calc R . . N2 N 1.2500 0.8954(3) 0.2500 0.0269(7) Uani 1 2 d S . . C13 C 0.7412(3) 0.4551(3) 0.39592(14) 0.0353(7) Uani 1 1 d . . . H13 H 0.6584 0.4922 0.3874 0.042 Uiso 1 1 calc R . . C9 C 0.8706(3) 0.2770(3) 0.41341(12) 0.0258(6) Uani 1 1 d . . . C7 C 0.8708(3) 0.1474(3) 0.42290(12) 0.0246(6) Uani 1 1 d . . . C18 C 0.8701(3) 0.5506(3) 0.25509(14) 0.0298(6) Uani 1 1 d . . . H18 H 0.9531 0.5893 0.2584 0.036 Uiso 1 1 calc R . . C2 C 0.9369(3) 0.0686(3) 0.38503(12) 0.0249(6) Uani 1 1 d . . . C1 C 1.0054(3) 0.1110(2) 0.32901(12) 0.0221(6) Uani 1 1 d . . . C6 C 0.8005(3) 0.1023(3) 0.47115(12) 0.0288(6) Uani 1 1 d . . . H6 H 0.7587 0.1536 0.4973 0.035 Uiso 1 1 calc R . . C20 C 0.7500 0.7445(3) 0.2500 0.0273(9) Uani 1 2 d S . . C24 C 1.2500 0.5204(3) 0.2500 0.0231(8) Uani 1 2 d S . . C14 C 0.7488(3) 0.3331(3) 0.39734(12) 0.0265(6) Uani 1 1 d . . . C19 C 0.7500 0.6150(3) 0.2500 0.0253(8) Uani 1 2 d S . . C11 C 0.9801(3) 0.4665(3) 0.42121(14) 0.0371(8) Uani 1 1 d . . . C3 C 0.9351(3) -0.0510(3) 0.39763(14) 0.0329(7) Uani 1 1 d . . . H3A H 0.9839 -0.1023 0.3742 0.040 Uiso 1 1 calc R . . C4 C 0.8614(3) -0.0945(3) 0.44481(14) 0.0350(7) Uani 1 1 d . . . H4 H 0.8588 -0.1748 0.4522 0.042 Uiso 1 1 calc R . . C5 C 0.7918(3) -0.0178(3) 0.48090(13) 0.0293(6) Uani 1 1 d . . . C22 C 1.2787(3) 0.3344(3) 0.30084(14) 0.0334(7) Uani 1 1 d . . . H22 H 1.2980 0.2934 0.3369 0.040 Uiso 1 1 calc R . . C10 C 0.9870(3) 0.3448(3) 0.42511(13) 0.0337(7) Uani 1 1 d . . . H10 H 1.0693 0.3084 0.4355 0.040 Uiso 1 1 calc R . . C25 C 1.2500 0.6495(3) 0.2500 0.0261(8) Uani 1 2 d S . . C12 C 0.8573(4) 0.5208(3) 0.40726(15) 0.0421(8) Uani 1 1 d . . . H12 H 0.8528 0.6022 0.4055 0.051 Uiso 1 1 calc R . . N4 N 0.7500 -0.0093(3) 0.2500 0.0263(7) Uani 1 2 d S . . O3W O 0.4345(4) 0.6038(4) 0.47904(18) 0.0909(13) Uani 1 1 d D . . C28 C 0.8471(4) -0.0710(3) 0.2259(2) 0.0522(10) Uani 1 1 d . . . H28 H 0.9168 -0.0304 0.2082 0.063 Uiso 1 1 calc R . . O2W O 0.5143(8) 0.7872(7) 0.4074(3) 0.223(3) Uani 1 1 d . . . H3WB H 0.445(7) 0.660(5) 0.510(2) 0.16(3) Uiso 1 1 d D . . H1WB H 1.471(5) 0.119(4) 0.320(2) 0.085(16) Uiso 1 1 d . . . H3WA H 0.499(16) 0.556(13) 0.469(7) 0.40(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0208(3) 0.0150(3) 0.0265(3) 0.000 0.00651(19) 0.000 Co2 0.0204(3) 0.0149(3) 0.0338(3) 0.000 0.0040(2) 0.000 O7 0.0270(10) 0.0276(12) 0.0289(10) -0.0036(8) 0.0053(8) -0.0050(9) O1W 0.0239(10) 0.0329(13) 0.0314(11) 0.0033(9) 0.0047(8) -0.0040(9) O2 0.0242(10) 0.0256(11) 0.0292(10) 0.0048(8) 0.0025(8) 0.0004(8) O8 0.0305(11) 0.0445(14) 0.0384(12) -0.0089(10) 0.0118(9) -0.0036(10) C16 0.053(2) 0.070(3) 0.0327(18) -0.0136(18) 0.0136(16) -0.030(2) C21 0.048(2) 0.0179(18) 0.092(3) -0.0032(17) 0.042(2) -0.0017(15) O1 0.0207(9) 0.0300(12) 0.0339(11) 0.0055(9) 0.0096(8) 0.0062(8) O3 0.0602(17) 0.0388(15) 0.0564(16) 0.0074(12) 0.0305(13) -0.0109(12) O4 0.0616(16) 0.0453(15) 0.0395(13) 0.0042(11) 0.0241(12) -0.0025(12) C17 0.0225(14) 0.0199(16) 0.0416(17) 0.0017(12) 0.0047(12) 0.0012(11) C27 0.0469(18) 0.0200(16) 0.0304(16) -0.0014(12) 0.0082(13) 0.0022(14) N3 0.0248(16) 0.0173(18) 0.0303(17) 0.000 0.0063(13) 0.000 N1 0.0261(17) 0.0166(18) 0.0286(17) 0.000 0.0056(13) 0.000 O6 0.099(2) 0.0544(19) 0.069(2) -0.0132(15) 0.0248(17) -0.0516(18) C15 0.0253(14) 0.0235(16) 0.0305(15) 0.0026(12) 0.0029(11) 0.0011(12) O5 0.0573(18) 0.088(2) 0.0522(16) -0.0156(15) 0.0063(13) -0.0447(17) C23 0.051(2) 0.0241(17) 0.0286(16) -0.0043(12) 0.0018(13) 0.0009(14) C8 0.0380(17) 0.036(2) 0.0339(17) 0.0076(14) 0.0061(13) -0.0036(15) C26 0.056(2) 0.0201(16) 0.0298(16) 0.0020(12) 0.0098(14) -0.0012(14) N2 0.0326(18) 0.0174(18) 0.0313(18) 0.000 0.0068(14) 0.000 C13 0.0419(18) 0.0258(17) 0.0389(17) -0.0025(13) 0.0078(14) -0.0010(14) C9 0.0282(14) 0.0271(16) 0.0229(13) -0.0020(11) 0.0079(11) -0.0040(12) C7 0.0213(13) 0.0304(17) 0.0222(13) 0.0003(11) 0.0034(10) -0.0020(12) C18 0.0236(14) 0.0202(16) 0.0461(18) -0.0014(13) 0.0065(12) -0.0042(12) C2 0.0199(13) 0.0299(17) 0.0253(13) 0.0032(12) 0.0047(10) -0.0007(11) C1 0.0233(13) 0.0196(15) 0.0238(13) -0.0019(11) 0.0053(10) -0.0023(11) C6 0.0285(15) 0.0350(18) 0.0235(14) 0.0007(12) 0.0080(11) 0.0006(13) C20 0.026(2) 0.017(2) 0.039(2) 0.000 0.0039(16) 0.000 C24 0.0264(19) 0.016(2) 0.028(2) 0.000 0.0085(15) 0.000 C14 0.0313(15) 0.0244(16) 0.0247(14) -0.0020(11) 0.0085(11) -0.0045(12) C19 0.0250(19) 0.021(2) 0.030(2) 0.000 0.0076(16) 0.000 C11 0.049(2) 0.034(2) 0.0291(16) -0.0077(13) 0.0126(13) -0.0182(15) C3 0.0330(16) 0.0303(18) 0.0368(16) 0.0039(13) 0.0136(13) 0.0057(13) C4 0.0429(18) 0.0255(17) 0.0376(17) 0.0079(13) 0.0100(14) 0.0020(14) C5 0.0295(14) 0.0314(18) 0.0277(15) 0.0074(12) 0.0067(11) -0.0024(13) C22 0.052(2) 0.0188(16) 0.0296(16) 0.0016(12) 0.0027(13) 0.0028(14) C10 0.0315(16) 0.045(2) 0.0248(14) -0.0039(13) 0.0063(12) -0.0085(14) C25 0.028(2) 0.018(2) 0.032(2) 0.000 0.0052(16) 0.000 C12 0.063(2) 0.0271(19) 0.0372(18) -0.0057(14) 0.0147(16) -0.0113(17) N4 0.0257(17) 0.0145(17) 0.0392(19) 0.000 0.0065(14) 0.000 O3W 0.059(2) 0.125(4) 0.090(3) -0.046(2) 0.0163(18) -0.040(2) C28 0.047(2) 0.0223(19) 0.092(3) 0.0003(18) 0.039(2) -0.0035(15) O2W 0.196(7) 0.310(10) 0.162(6) 0.040(6) 0.004(5) -0.010(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1W 2.071(2) . ? Co1 O1W 2.071(2) 2_755 ? Co1 O1 2.0929(19) 2_755 ? Co1 O1 2.0929(19) . ? Co1 N1 2.143(3) . ? Co1 N2 2.165(3) 1_545 ? Co2 O2 2.0560(19) . ? Co2 O2 2.0560(19) 2_655 ? Co2 N3 2.124(3) . ? Co2 N4 2.185(3) . ? Co2 O7 2.235(2) . ? Co2 O7 2.235(2) 2_655 ? O7 C15 1.270(3) . ? O2 C1 1.260(3) . ? O8 C15 1.250(3) . ? C16 O6 1.208(5) . ? C16 O5 1.327(5) . ? C16 C11 1.490(5) . ? C21 C20 1.371(4) . ? C21 C28 1.377(5) 1_565 ? O1 C1 1.242(3) . ? O3 C8 1.325(4) . ? O4 C8 1.208(4) . ? C17 N3 1.339(3) . ? C17 C18 1.379(4) . ? C27 N2 1.341(3) . ? C27 C26 1.375(4) . ? N3 C17 1.339(3) 2_655 ? N1 C22 1.332(3) . ? N1 C22 1.332(3) 2_755 ? C15 C14 1.506(4) . ? C23 C22 1.378(4) . ? C23 C24 1.393(4) . ? C8 C5 1.498(4) . ? C26 C25 1.390(4) . ? N2 C27 1.341(3) 2_755 ? N2 Co1 2.165(3) 1_565 ? C13 C12 1.381(5) . ? C13 C14 1.393(4) . ? C9 C14 1.392(4) . ? C9 C10 1.398(4) . ? C9 C7 1.491(4) . ? C7 C6 1.394(4) . ? C7 C2 1.407(4) . ? C18 C19 1.394(3) . ? C2 C3 1.390(4) . ? C2 C1 1.513(4) . ? C6 C5 1.389(4) . ? C20 C21 1.371(4) 2_655 ? C20 C19 1.476(6) . ? C24 C23 1.393(4) 2_755 ? C24 C25 1.471(6) . ? C19 C18 1.394(3) 2_655 ? C11 C12 1.381(5) . ? C11 C10 1.391(5) . ? C3 C4 1.388(4) . ? C4 C5 1.386(4) . ? C25 C26 1.390(4) 2_755 ? N4 C28 1.322(4) 2_655 ? N4 C28 1.322(4) . ? C28 C21 1.377(5) 1_545 ? 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 O1W Co1 O1W 175.78(13) . 2_755 ? O1W Co1 O1 96.95(8) . 2_755 ? O1W Co1 O1 82.81(8) 2_755 2_755 ? O1W Co1 O1 82.81(8) . . ? O1W Co1 O1 96.95(8) 2_755 . ? O1 Co1 O1 173.44(11) 2_755 . ? O1W Co1 N1 92.11(6) . . ? O1W Co1 N1 92.11(6) 2_755 . ? O1 Co1 N1 93.28(5) 2_755 . ? O1 Co1 N1 93.28(6) . . ? O1W Co1 N2 87.89(6) . 1_545 ? O1W Co1 N2 87.89(6) 2_755 1_545 ? O1 Co1 N2 86.72(6) 2_755 1_545 ? O1 Co1 N2 86.72(6) . 1_545 ? N1 Co1 N2 180.000(1) . 1_545 ? O2 Co2 O2 177.30(11) . 2_655 ? O2 Co2 N3 91.35(6) . . ? O2 Co2 N3 91.35(6) 2_655 . ? O2 Co2 N4 88.65(6) . . ? O2 Co2 N4 88.65(6) 2_655 . ? N3 Co2 N4 180.0 . . ? O2 Co2 O7 97.90(8) . . ? O2 Co2 O7 82.26(8) 2_655 . ? N3 Co2 O7 86.62(5) . . ? N4 Co2 O7 93.38(5) . . ? O2 Co2 O7 82.26(8) . 2_655 ? O2 Co2 O7 97.90(8) 2_655 2_655 ? N3 Co2 O7 86.62(5) . 2_655 ? N4 Co2 O7 93.38(5) . 2_655 ? O7 Co2 O7 173.24(10) . 2_655 ? C15 O7 Co2 137.73(18) . . ? C1 O2 Co2 136.43(18) . . ? O6 C16 O5 123.4(4) . . ? O6 C16 C11 124.3(4) . . ? O5 C16 C11 112.4(4) . . ? C20 C21 C28 120.3(3) . 1_565 ? C1 O1 Co1 131.53(18) . . ? N3 C17 C18 122.9(3) . . ? N2 C27 C26 122.8(3) . . ? C17 N3 C17 117.5(3) . 2_655 ? C17 N3 Co2 121.23(17) . . ? C17 N3 Co2 121.23(17) 2_655 . ? C22 N1 C22 117.1(4) . 2_755 ? C22 N1 Co1 121.47(17) . . ? C22 N1 Co1 121.47(18) 2_755 . ? O8 C15 O7 124.9(3) . . ? O8 C15 C14 117.9(3) . . ? O7 C15 C14 117.2(2) . . ? C22 C23 C24 120.5(3) . . ? O4 C8 O3 122.8(3) . . ? O4 C8 C5 123.7(3) . . ? O3 C8 C5 113.5(3) . . ? C27 C26 C25 120.3(3) . . ? C27 N2 C27 117.5(4) 2_755 . ? C27 N2 Co1 121.27(18) 2_755 1_565 ? C27 N2 Co1 121.27(18) . 1_565 ? C12 C13 C14 119.6(3) . . ? C14 C9 C10 118.9(3) . . ? C14 C9 C7 119.1(2) . . ? C10 C9 C7 121.8(3) . . ? C6 C7 C2 118.6(3) . . ? C6 C7 C9 118.3(3) . . ? C2 C7 C9 123.2(2) . . ? C17 C18 C19 120.1(3) . . ? C3 C2 C7 119.8(3) . . ? C3 C2 C1 119.0(3) . . ? C7 C2 C1 121.1(3) . . ? O1 C1 O2 125.4(2) . . ? O1 C1 C2 116.0(2) . . ? O2 C1 C2 118.6(2) . . ? C5 C6 C7 121.1(3) . . ? C21 C20 C21 115.9(4) . 2_655 ? C21 C20 C19 122.1(2) . . ? C21 C20 C19 122.1(2) 2_655 . ? C23 C24 C23 115.5(4) 2_755 . ? C23 C24 C25 122.26(18) 2_755 . ? C23 C24 C25 122.26(18) . . ? C9 C14 C13 120.6(3) . . ? C9 C14 C15 119.4(3) . . ? C13 C14 C15 120.0(3) . . ? C18 C19 C18 116.5(4) 2_655 . ? C18 C19 C20 121.74(18) 2_655 . ? C18 C19 C20 121.74(18) . . ? C12 C11 C10 120.0(3) . . ? C12 C11 C16 117.7(3) . . ? C10 C11 C16 122.3(3) . . ? C4 C3 C2 120.7(3) . . ? C5 C4 C3 119.8(3) . . ? C4 C5 C6 119.8(3) . . ? C4 C5 C8 122.5(3) . . ? C6 C5 C8 117.7(3) . . ? N1 C22 C23 123.2(3) . . ? C11 C10 C9 120.2(3) . . ? C26 C25 C26 116.5(4) . 2_755 ? C26 C25 C24 121.77(19) . . ? C26 C25 C24 121.77(19) 2_755 . ? C13 C12 C11 120.6(3) . . ? C28 N4 C28 115.7(4) 2_655 . ? C28 N4 Co2 122.13(19) 2_655 . ? C28 N4 Co2 122.13(19) . . ? N4 C28 C21 123.9(3) . 1_545 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.723 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.071 #===========================end data_complex-5 #TrackingRef '- 1-5.cif' _database_code_depnum_ccdc_archive 'CCDC 772718' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H40 N4 O17 Zn2' _chemical_formula_sum 'C36 H40 N4 O17 Zn2' _chemical_formula_weight 931.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall 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 14.264 _cell_length_b 19.306 _cell_length_c 15.435 _cell_angle_alpha 90.00 _cell_angle_beta 113.44 _cell_angle_gamma 90.00 _cell_volume 3899.7 _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.56 _cell_measurement_theta_max 25.04 _exptl_crystal_description neddle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.576 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 1.311 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.815 _exptl_absorpt_correction_T_max 0.843 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'BRUKER SMART CCD Apex II' _diffrn_measurement_method 'omega and phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19586 _diffrn_reflns_av_R_equivalents 0.0784 _diffrn_reflns_av_sigmaI/netI 0.1016 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.04 _reflns_number_total 6862 _reflns_number_gt 3838 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SMART (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0545P)^2^+0.2046P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6862 _refine_ls_number_parameters 568 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1214 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1314 _refine_ls_wR_factor_gt 0.1084 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.97536(5) 0.22476(3) 0.94890(5) 0.0374(2) Uani 1 1 d . . . Zn2 Zn 0.56666(5) 0.24262(3) 0.54970(5) 0.03464(19) Uani 1 1 d . . . O1 O 0.8558(3) 0.16052(16) 0.8738(3) 0.0369(9) Uani 1 1 d . . . O1W O 0.9981(3) 0.2429(2) 0.8187(3) 0.0582(12) Uani 1 1 d D . . H1WA H 0.9472 0.2309 0.7732 0.087 Uiso 1 1 d R . . O2 O 0.7209(2) 0.22872(15) 0.8467(3) 0.0350(9) Uani 1 1 d . . . O2W O 0.8877(4) 0.3144(2) 0.9173(4) 0.0697(14) Uani 1 1 d D . . O3 O 1.0687(4) -0.0920(2) 0.7051(4) 0.0782(16) Uani 1 1 d . . . O3W O 0.9463(3) 0.2096(3) 1.0735(3) 0.0645(13) Uani 1 1 d D . . H3WA H 0.9088 0.2349 1.0771 0.097 Uiso 1 1 d R . . O4 O 0.9607(4) -0.1366(2) 0.7585(4) 0.0904(18) Uani 1 1 d . . . O4W O 0.5586(3) 0.27190(19) 0.6802(3) 0.0472(10) Uani 1 1 d D . . H4WA H 0.5495 0.3136 0.6808 0.071 Uiso 1 1 d R . . O5 O 0.8196(3) 0.22662(16) 0.6482(3) 0.0432(10) Uani 1 1 d . . . O5W O 0.5824(3) 0.2202(2) 0.4206(3) 0.0563(12) Uani 1 1 d D . . H5WA H 0.5708 0.1811 0.4071 0.085 Uiso 1 1 d R . . O6 O 0.6758(3) 0.16919(16) 0.6217(3) 0.0367(9) Uani 1 1 d . . . O6W O 0.6715(3) 0.32121(19) 0.5592(3) 0.0466(10) Uani 1 1 d D . . H6WA H 0.7257 0.3133 0.6036 0.070 Uiso 1 1 d R . . O7 O 0.4516(5) -0.0888(2) 0.7750(4) 0.116(2) Uani 1 1 d . . . O8 O 0.5215(5) -0.1165(3) 0.6823(5) 0.123(2) Uani 1 1 d . . . N1 N 1.1190(3) 0.2714(2) 1.0373(3) 0.0433(12) Uani 1 1 d . . . N2 N 1.0768(3) 0.1402(2) 0.9843(3) 0.0389(11) Uani 1 1 d . . . N3 N 0.4528(3) 0.1646(2) 0.5173(3) 0.0391(12) Uani 1 1 d . . . N4 N 0.4279(4) 0.2982(3) 0.4697(3) 0.0467(13) Uani 1 1 d . . . C1 C 1.1350(5) 0.3378(3) 1.0631(4) 0.0514(17) Uani 1 1 d . . . H1 H 1.0813 0.3689 1.0368 0.062 Uiso 1 1 calc R . . C2 C 1.2280(6) 0.3626(4) 1.1272(5) 0.065(2) Uani 1 1 d . . . H2 H 1.2366 0.4093 1.1435 0.078 Uiso 1 1 calc R . . C3 C 1.3063(5) 0.3169(4) 1.1656(5) 0.071(2) Uani 1 1 d . . . H3 H 1.3697 0.3321 1.2084 0.086 Uiso 1 1 calc R . . C4 C 1.2911(5) 0.2476(4) 1.1408(5) 0.0638(19) Uani 1 1 d . . . H4 H 1.3437 0.2158 1.1674 0.077 Uiso 1 1 calc R . . C5 C 1.1967(4) 0.2262(3) 1.0759(4) 0.0420(15) Uani 1 1 d . . . C6 C 1.1739(4) 0.1534(3) 1.0431(4) 0.0404(14) Uani 1 1 d . . . C7 C 1.2482(5) 0.1014(3) 1.0680(4) 0.0554(18) Uani 1 1 d . . . H7 H 1.3153 0.1109 1.1084 0.067 Uiso 1 1 calc R . . C8 C 1.2204(5) 0.0361(4) 1.0319(5) 0.0621(19) Uani 1 1 d . . . H8 H 1.2691 0.0011 1.0477 0.075 Uiso 1 1 calc R . . C9 C 1.1219(5) 0.0222(3) 0.9730(5) 0.0561(17) Uani 1 1 d . . . H9 H 1.1021 -0.0221 0.9489 0.067 Uiso 1 1 calc R . . C10 C 1.0523(5) 0.0761(3) 0.9503(4) 0.0529(17) Uani 1 1 d . . . H10 H 0.9851 0.0673 0.9093 0.063 Uiso 1 1 calc R . . C11 C 0.7616(4) 0.1705(2) 0.8445(4) 0.0269(12) Uani 1 1 d . . . C12 C 0.6915(4) 0.1093(2) 0.8066(3) 0.0251(12) Uani 1 1 d . . . C13 C 0.6045(4) 0.1043(2) 0.8265(4) 0.0332(13) Uani 1 1 d . . . H13 H 0.5870 0.1409 0.8563 0.040 Uiso 1 1 calc R . . C14 C 0.5440(4) 0.0454(2) 0.8026(4) 0.0342(13) Uani 1 1 d . . . H14 H 0.4873 0.0426 0.8179 0.041 Uiso 1 1 calc R . . C15 C 0.5669(4) -0.0093(2) 0.7561(4) 0.0304(13) Uani 1 1 d . . . C16 C 0.5065(4) -0.0760(3) 0.7350(4) 0.0425(15) Uani 1 1 d . . . C17 C 0.6503(4) -0.0025(2) 0.7318(4) 0.0298(12) Uani 1 1 d . . . H17 H 0.6637 -0.0379 0.6974 0.036 Uiso 1 1 calc R . . C18 C 0.7146(3) 0.0547(2) 0.7564(3) 0.0250(12) Uani 1 1 d . . . C19 C 0.8045(4) 0.0531(2) 0.7296(4) 0.0271(12) Uani 1 1 d . . . C20 C 0.8626(4) -0.0077(2) 0.7479(4) 0.0349(14) Uani 1 1 d . . . H20 H 0.8460 -0.0436 0.7794 0.042 Uiso 1 1 calc R . . C21 C 0.9441(4) -0.0168(3) 0.7212(4) 0.0402(15) Uani 1 1 d . . . C22 C 0.9725(4) 0.0378(3) 0.6804(5) 0.0484(17) Uani 1 1 d . . . H22 H 1.0291 0.0337 0.6651 0.058 Uiso 1 1 calc R . . C23 C 0.9176(4) 0.0988(3) 0.6618(4) 0.0421(15) Uani 1 1 d . . . H23 H 0.9384 0.1355 0.6347 0.051 Uiso 1 1 calc R . . C24 C 0.8311(4) 0.1067(2) 0.6829(4) 0.0288(12) Uani 1 1 d . . . C25 C 0.9972(5) -0.0866(3) 0.7313(5) 0.059(2) Uani 1 1 d . . . C26 C 0.7712(4) 0.1728(2) 0.6487(4) 0.0290(12) Uani 1 1 d . . . C27 C 0.4703(4) 0.0993(3) 0.5480(4) 0.0476(16) Uani 1 1 d . . . H27 H 0.5366 0.0870 0.5875 0.057 Uiso 1 1 calc R . . C28 C 0.3954(5) 0.0493(3) 0.5245(5) 0.0566(18) Uani 1 1 d . . . H28 H 0.4101 0.0045 0.5484 0.068 Uiso 1 1 calc R . . C29 C 0.2978(5) 0.0678(4) 0.4642(4) 0.0571(18) Uani 1 1 d . . . H29 H 0.2450 0.0357 0.4472 0.069 Uiso 1 1 calc R . . C30 C 0.2794(5) 0.1336(4) 0.4298(4) 0.0573(18) Uani 1 1 d . . . H30 H 0.2143 0.1459 0.3871 0.069 Uiso 1 1 calc R . . C31 C 0.3572(4) 0.1827(3) 0.4581(4) 0.0434(15) Uani 1 1 d . . . C32 C 0.3446(5) 0.2562(4) 0.4302(4) 0.0517(17) Uani 1 1 d . . . C33 C 0.2517(5) 0.2847(4) 0.3708(5) 0.069(2) Uani 1 1 d . . . H33 H 0.1945 0.2565 0.3442 0.083 Uiso 1 1 calc R . . C34 C 0.2443(6) 0.3547(5) 0.3512(5) 0.084(3) Uani 1 1 d . . . H34 H 0.1821 0.3738 0.3118 0.101 Uiso 1 1 calc R . . C35 C 0.3307(6) 0.3968(4) 0.3910(5) 0.075(2) Uani 1 1 d . . . H35 H 0.3280 0.4441 0.3784 0.090 Uiso 1 1 calc R . . C36 C 0.4200(5) 0.3652(3) 0.4495(4) 0.0603(19) Uani 1 1 d . . . H36 H 0.4782 0.3925 0.4765 0.072 Uiso 1 1 calc R . . O7W O 0.7148(5) 0.4353(3) 0.6763(5) 0.0888(17) Uani 1 1 d D . . O9W O 0.0989(12) 0.9679(7) 0.5632(10) 0.392(9) Uani 1 1 d . . . O8W O 0.2650(8) 0.5775(7) 0.0711(10) 0.348(8) Uani 1 1 d . . . H5WB H 0.629(4) 0.236(3) 0.401(5) 0.10(3) Uiso 1 1 d D . . H4WB H 0.606(3) 0.252(3) 0.731(3) 0.060(19) Uiso 1 1 d D . . H1WB H 0.989(5) 0.2886(12) 0.819(6) 0.12(3) Uiso 1 1 d D . . H6WB H 0.689(5) 0.361(2) 0.594(4) 0.09(2) Uiso 1 1 d D . . H2WB H 0.868(3) 0.311(2) 0.966(2) 0.000(12) Uiso 1 1 d D . . H3WB H 0.974(7) 0.173(3) 1.110(6) 0.19(5) Uiso 1 1 d D . . H2WA H 0.820(3) 0.303(5) 0.892(8) 0.21(5) Uiso 1 1 d D . . H7WA H 0.742(7) 0.459(5) 0.733(4) 0.19(5) Uiso 1 1 d D . . H7WB H 0.645(2) 0.439(3) 0.626(3) 0.05(2) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0287(4) 0.0339(4) 0.0431(4) -0.0005(3) 0.0073(3) -0.0037(3) Zn2 0.0333(4) 0.0338(4) 0.0373(4) 0.0058(3) 0.0145(3) 0.0049(3) O1 0.024(2) 0.029(2) 0.052(3) -0.0043(17) 0.0094(19) 0.0003(15) O1W 0.051(3) 0.060(3) 0.050(3) 0.008(2) 0.005(2) -0.021(2) O2 0.032(2) 0.0215(19) 0.052(3) -0.0042(17) 0.0164(19) 0.0023(15) O2W 0.057(3) 0.048(3) 0.094(5) -0.013(3) 0.019(3) 0.003(2) O3 0.059(3) 0.053(3) 0.125(5) -0.011(3) 0.040(3) 0.021(2) O3W 0.062(3) 0.083(3) 0.059(3) 0.005(3) 0.036(3) 0.028(3) O4 0.073(4) 0.048(3) 0.151(5) 0.038(3) 0.045(4) 0.023(2) O4W 0.055(3) 0.047(2) 0.037(3) 0.005(2) 0.016(2) 0.024(2) O5 0.035(2) 0.024(2) 0.070(3) 0.0070(19) 0.021(2) -0.0030(16) O5W 0.077(3) 0.053(3) 0.058(3) -0.016(2) 0.047(3) -0.031(2) O6 0.031(2) 0.032(2) 0.047(3) 0.0078(17) 0.015(2) 0.0018(16) O6W 0.045(3) 0.037(2) 0.053(3) 0.004(2) 0.013(2) -0.0002(19) O7 0.170(6) 0.082(4) 0.164(6) -0.058(4) 0.138(5) -0.081(4) O8 0.155(6) 0.094(4) 0.168(6) -0.089(4) 0.116(5) -0.090(4) N1 0.037(3) 0.055(3) 0.036(3) -0.001(2) 0.012(2) -0.008(2) N2 0.036(3) 0.042(3) 0.035(3) -0.002(2) 0.010(2) 0.000(2) N3 0.030(3) 0.052(3) 0.034(3) 0.000(2) 0.011(2) -0.003(2) N4 0.047(3) 0.057(3) 0.043(3) 0.019(3) 0.025(3) 0.020(3) C1 0.054(4) 0.052(4) 0.048(4) -0.010(3) 0.020(4) -0.019(3) C2 0.071(5) 0.077(5) 0.046(5) -0.021(4) 0.024(4) -0.031(4) C3 0.051(5) 0.114(7) 0.044(5) -0.017(5) 0.014(4) -0.036(5) C4 0.033(4) 0.102(6) 0.050(5) -0.005(4) 0.009(3) -0.010(4) C5 0.033(3) 0.067(4) 0.028(4) -0.003(3) 0.014(3) -0.009(3) C6 0.030(3) 0.065(4) 0.026(4) 0.013(3) 0.010(3) 0.004(3) C7 0.037(4) 0.072(5) 0.051(5) 0.019(4) 0.010(3) 0.009(3) C8 0.058(5) 0.065(5) 0.059(5) 0.026(4) 0.020(4) 0.022(4) C9 0.061(5) 0.045(4) 0.059(5) 0.014(3) 0.020(4) 0.012(3) C10 0.045(4) 0.053(4) 0.051(4) 0.002(3) 0.010(3) 0.004(3) C11 0.030(3) 0.026(3) 0.028(3) 0.003(2) 0.015(3) -0.001(2) C12 0.026(3) 0.022(3) 0.025(3) 0.003(2) 0.008(2) 0.001(2) C13 0.034(3) 0.029(3) 0.041(4) -0.005(3) 0.019(3) -0.004(2) C14 0.027(3) 0.037(3) 0.042(4) -0.001(3) 0.017(3) -0.003(2) C15 0.035(3) 0.025(3) 0.032(3) 0.001(2) 0.014(3) -0.005(2) C16 0.046(4) 0.040(4) 0.051(4) -0.012(3) 0.029(3) -0.018(3) C17 0.036(3) 0.022(3) 0.033(3) -0.001(2) 0.015(3) -0.002(2) C18 0.024(3) 0.026(3) 0.023(3) 0.004(2) 0.008(2) 0.000(2) C19 0.030(3) 0.021(3) 0.030(3) 0.000(2) 0.011(3) -0.002(2) C20 0.035(3) 0.024(3) 0.045(4) 0.004(3) 0.015(3) -0.005(2) C21 0.034(3) 0.031(3) 0.050(4) 0.003(3) 0.010(3) 0.008(2) C22 0.032(3) 0.041(3) 0.081(5) 0.003(3) 0.033(4) 0.008(3) C23 0.037(4) 0.036(3) 0.061(4) 0.006(3) 0.028(3) 0.000(3) C24 0.026(3) 0.027(3) 0.036(3) -0.003(2) 0.016(3) -0.001(2) C25 0.036(4) 0.038(4) 0.096(6) 0.004(4) 0.017(4) 0.010(3) C26 0.035(3) 0.026(3) 0.027(3) 0.000(2) 0.013(3) -0.001(2) C27 0.042(4) 0.047(4) 0.055(4) 0.004(3) 0.020(3) -0.003(3) C28 0.062(5) 0.060(4) 0.054(5) -0.004(3) 0.029(4) -0.017(3) C29 0.060(5) 0.081(5) 0.038(4) -0.021(4) 0.027(4) -0.029(4) C30 0.033(4) 0.106(6) 0.034(4) -0.012(4) 0.015(3) -0.015(4) C31 0.037(4) 0.066(4) 0.031(4) 0.004(3) 0.018(3) 0.004(3) C32 0.041(4) 0.087(5) 0.031(4) 0.013(4) 0.019(3) 0.017(4) C33 0.050(5) 0.119(6) 0.040(4) 0.025(4) 0.021(4) 0.027(4) C34 0.064(6) 0.147(8) 0.055(5) 0.051(5) 0.037(5) 0.057(6) C35 0.094(6) 0.082(5) 0.076(6) 0.047(5) 0.063(5) 0.053(5) C36 0.069(5) 0.062(4) 0.055(5) 0.025(4) 0.030(4) 0.026(4) O7W 0.102(5) 0.064(3) 0.104(6) -0.010(4) 0.045(5) -0.003(3) O9W 0.47(2) 0.413(19) 0.37(2) -0.068(15) 0.252(18) 0.152(16) O8W 0.195(10) 0.368(16) 0.41(2) -0.173(14) 0.039(11) 0.067(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 2.054(3) . ? Zn1 O2W 2.077(5) . ? Zn1 N2 2.105(4) . ? Zn1 O3W 2.142(4) . ? Zn1 N1 2.156(4) . ? Zn1 O1W 2.188(4) . ? Zn2 O6 2.071(3) . ? Zn2 O6W 2.094(4) . ? Zn2 N3 2.123(4) . ? Zn2 O5W 2.136(4) . ? Zn2 O4W 2.139(4) . ? Zn2 N4 2.156(4) . ? O1 C11 1.250(5) . ? O1W H1WA 0.8183 . ? O1W H1WB 0.89(2) . ? O2 C11 1.271(5) . ? O2W H2WB 0.906(18) . ? O2W H2WA 0.91(2) . ? O3 C25 1.242(7) . ? O3W H3WA 0.7427 . ? O3W H3WB 0.90(2) . ? O4 C25 1.245(7) . ? O4W H4WA 0.8162 . ? O4W H4WB 0.89(2) . ? O5 C26 1.250(5) . ? O5W H5WA 0.7839 . ? O5W H5WB 0.88(2) . ? O6 C26 1.258(5) . ? O6W H6WA 0.8181 . ? O6W H6WB 0.91(2) . ? O7 C16 1.199(6) . ? O8 C16 1.206(6) . ? N1 C1 1.334(6) . ? N1 C5 1.349(7) . ? N2 C10 1.334(7) . ? N2 C6 1.344(6) . ? N3 C27 1.335(6) . ? N3 C31 1.351(7) . ? N4 C36 1.325(7) . ? N4 C32 1.365(7) . ? C1 C2 1.387(8) . ? C1 H1 0.9300 . ? C2 C3 1.361(9) . ? C2 H2 0.9300 . ? C3 C4 1.384(9) . ? C3 H3 0.9300 . ? C4 C5 1.383(8) . ? C4 H4 0.9300 . ? C5 C6 1.486(7) . ? C6 C7 1.398(7) . ? C7 C8 1.370(8) . ? C7 H7 0.9300 . ? C8 C9 1.362(8) . ? C8 H8 0.9300 . ? C9 C10 1.384(7) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.507(6) . ? C12 C13 1.396(6) . ? C12 C18 1.422(6) . ? C13 C14 1.385(6) . ? C13 H13 0.9300 . ? C14 C15 1.388(6) . ? C14 H14 0.9300 . ? C15 C17 1.389(6) . ? C15 C16 1.511(7) . ? C17 C18 1.389(6) . ? C17 H17 0.9300 . ? C18 C19 1.496(6) . ? C19 C20 1.398(6) . ? C19 C24 1.399(6) . ? C20 C21 1.390(7) . ? C20 H20 0.9300 . ? C21 C22 1.369(7) . ? C21 C25 1.523(7) . ? C22 C23 1.380(7) . ? C22 H22 0.9300 . ? C23 C24 1.405(6) . ? C23 H23 0.9300 . ? C24 C26 1.508(6) . ? C27 C28 1.378(7) . ? C27 H27 0.9300 . ? C28 C29 1.379(8) . ? C28 H28 0.9300 . ? C29 C30 1.362(8) . ? C29 H29 0.9300 . ? C30 C31 1.390(8) . ? C30 H30 0.9300 . ? C31 C32 1.475(8) . ? C32 C33 1.389(8) . ? C33 C34 1.380(9) . ? C33 H33 0.9300 . ? C34 C35 1.398(10) . ? C34 H34 0.9300 . ? C35 C36 1.376(9) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? O7W H7WA 0.93(2) . ? O7W H7WB 0.99(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O2W 94.80(17) . . ? O1 Zn1 N2 90.50(15) . . ? O2W Zn1 N2 174.39(19) . . ? O1 Zn1 O3W 90.58(17) . . ? O2W Zn1 O3W 90.6(2) . . ? N2 Zn1 O3W 91.14(17) . . ? O1 Zn1 N1 167.54(16) . . ? O2W Zn1 N1 97.58(19) . . ? N2 Zn1 N1 77.17(18) . . ? O3W Zn1 N1 87.93(17) . . ? O1 Zn1 O1W 88.38(15) . . ? O2W Zn1 O1W 86.9(2) . . ? N2 Zn1 O1W 91.41(17) . . ? O3W Zn1 O1W 177.26(17) . . ? N1 Zn1 O1W 93.63(16) . . ? O6 Zn2 O6W 95.46(14) . . ? O6 Zn2 N3 88.97(15) . . ? O6W Zn2 N3 171.21(17) . . ? O6 Zn2 O5W 91.54(16) . . ? O6W Zn2 O5W 82.80(15) . . ? N3 Zn2 O5W 89.50(16) . . ? O6 Zn2 O4W 89.20(14) . . ? O6W Zn2 O4W 92.71(16) . . ? N3 Zn2 O4W 94.95(16) . . ? O5W Zn2 O4W 175.50(15) . . ? O6 Zn2 N4 166.02(17) . . ? O6W Zn2 N4 98.44(17) . . ? N3 Zn2 N4 77.06(19) . . ? O5W Zn2 N4 88.81(17) . . ? O4W Zn2 N4 91.55(16) . . ? C11 O1 Zn1 130.0(3) . . ? Zn1 O1W H1WA 109.8 . . ? Zn1 O1W H1WB 94(5) . . ? H1WA O1W H1WB 101.6 . . ? Zn1 O2W H2WB 95(3) . . ? Zn1 O2W H2WA 109(7) . . ? H2WB O2W H2WA 73(8) . . ? Zn1 O3W H3WA 112.3 . . ? Zn1 O3W H3WB 119(6) . . ? H3WA O3W H3WB 128.5 . . ? Zn2 O4W H4WA 109.9 . . ? Zn2 O4W H4WB 114(4) . . ? H4WA O4W H4WB 118.8 . . ? Zn2 O5W H5WA 110.7 . . ? Zn2 O5W H5WB 128(5) . . ? H5WA O5W H5WB 110.7 . . ? C26 O6 Zn2 128.6(3) . . ? Zn2 O6W H6WA 109.4 . . ? Zn2 O6W H6WB 132(4) . . ? H6WA O6W H6WB 73.6 . . ? C1 N1 C5 118.5(5) . . ? C1 N1 Zn1 126.7(4) . . ? C5 N1 Zn1 114.5(4) . . ? C10 N2 C6 118.7(5) . . ? C10 N2 Zn1 124.8(4) . . ? C6 N2 Zn1 116.4(4) . . ? C27 N3 C31 118.6(5) . . ? C27 N3 Zn2 124.7(4) . . ? C31 N3 Zn2 116.7(4) . . ? C36 N4 C32 119.8(5) . . ? C36 N4 Zn2 126.4(4) . . ? C32 N4 Zn2 113.5(4) . . ? N1 C1 C2 123.1(6) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C3 C2 C1 118.2(7) . . ? C3 C2 H2 120.9 . . ? C1 C2 H2 120.9 . . ? C2 C3 C4 119.7(7) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C5 C4 C3 119.3(7) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? N1 C5 C4 121.2(6) . . ? N1 C5 C6 115.6(5) . . ? C4 C5 C6 123.2(6) . . ? N2 C6 C7 120.9(6) . . ? N2 C6 C5 115.9(5) . . ? C7 C6 C5 123.1(6) . . ? C8 C7 C6 118.9(6) . . ? C8 C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? C9 C8 C7 120.5(6) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 117.8(6) . . ? C8 C9 H9 121.1 . . ? C10 C9 H9 121.1 . . ? N2 C10 C9 123.2(6) . . ? N2 C10 H10 118.4 . . ? C9 C10 H10 118.4 . . ? O1 C11 O2 124.2(4) . . ? O1 C11 C12 118.1(4) . . ? O2 C11 C12 117.7(4) . . ? C13 C12 C18 119.1(4) . . ? C13 C12 C11 118.7(4) . . ? C18 C12 C11 122.1(4) . . ? C14 C13 C12 120.9(5) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 120.8(5) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C14 C15 C17 118.1(4) . . ? C14 C15 C16 122.0(5) . . ? C17 C15 C16 119.9(4) . . ? O7 C16 O8 122.8(6) . . ? O7 C16 C15 119.8(5) . . ? O8 C16 C15 117.3(5) . . ? C15 C17 C18 123.0(5) . . ? C15 C17 H17 118.5 . . ? C18 C17 H17 118.5 . . ? C17 C18 C12 117.9(4) . . ? C17 C18 C19 116.9(4) . . ? C12 C18 C19 125.2(4) . . ? C20 C19 C24 117.7(5) . . ? C20 C19 C18 117.8(4) . . ? C24 C19 C18 124.4(4) . . ? C21 C20 C19 123.0(5) . . ? C21 C20 H20 118.5 . . ? C19 C20 H20 118.5 . . ? C22 C21 C20 118.3(5) . . ? C22 C21 C25 120.1(5) . . ? C20 C21 C25 121.5(5) . . ? C21 C22 C23 120.3(5) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C22 C23 C24 121.6(5) . . ? C22 C23 H23 119.2 . . ? C24 C23 H23 119.2 . . ? C19 C24 C23 118.8(5) . . ? C19 C24 C26 125.1(4) . . ? C23 C24 C26 116.1(4) . . ? O3 C25 O4 123.5(6) . . ? O3 C25 C21 118.7(6) . . ? O4 C25 C21 117.5(6) . . ? O5 C26 O6 124.9(4) . . ? O5 C26 C24 117.9(5) . . ? O6 C26 C24 117.2(4) . . ? N3 C27 C28 123.6(6) . . ? N3 C27 H27 118.2 . . ? C28 C27 H27 118.2 . . ? C27 C28 C29 117.7(6) . . ? C27 C28 H28 121.2 . . ? C29 C28 H28 121.2 . . ? C30 C29 C28 119.5(6) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C29 C30 C31 120.4(6) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? N3 C31 C30 120.2(6) . . ? N3 C31 C32 114.7(5) . . ? C30 C31 C32 125.1(6) . . ? N4 C32 C33 119.5(7) . . ? N4 C32 C31 117.3(5) . . ? C33 C32 C31 123.1(7) . . ? C34 C33 C32 120.1(8) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 119.8(7) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C36 C35 C34 117.0(7) . . ? C36 C35 H35 121.5 . . ? C34 C35 H35 121.5 . . ? N4 C36 C35 123.8(7) . . ? N4 C36 H36 118.1 . . ? C35 C36 H36 118.1 . . ? H7WA O7W H7WB 128(7) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.618 _refine_diff_density_min -0.439 _refine_diff_density_rms 0.080