Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2001 data_global #=========================================================================== _journal_coden_Cambridge 186 # 1. SUBMISSION DETAILS _publ_contact_author ; Prof. Dr. R. van Eldik Institut f\"ur Anorganische Chemie Universit\"at Erlangen-N\"urnberg Egerlandstr. 1 D-91058 Erlangen Bundesrepublik Deutschland ; _publ_contact_author_phone '049 9131 852-27350' _publ_contact_author_fax '049 9131 852-27387' _publ_contact_author_email 'VANELDIK@ANORGANIK.CHEMIE.UNI-ERLANGEN.DE' _publ_requested_journal 'J. Chem. Soc. Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for data deposition. ; #=========================================================================== # 2. TITLE AND AUTHOR LIST _publ_section_title ; Complex-formation reactions of Cu(II) and Zn(II) 2,2'-bipyridine and, 1,10-phenathroline complexes with bicarbonate. Identification of different carbonate coordination modes ; loop_ _publ_author_name _publ_author_address 'Mao, Z.-W.' ; School of Chemistry and Chemical Engineering Zhongshan University 510275 Guangzhou P. R. China ; 'Heinemann, F. W.' ; Institut f\"ur Anorganische Chemie Universit\"at Erlangen-N\"urnberg Egerlandstr. 1 D-91058 Erlangen Bundesrepublik Deutschland ; 'Liehr, G.' ; Institut f\"ur Anorganische Chemie Universit\"at Erlangen-N\"urnberg Egerlandstr. 1 D-91058 Erlangen Bundesrepublik Deutschland ; 'van Eldik, R.' ; Institut f\"ur Anorganische Chemie Universit\"at Erlangen-N\"urnberg Egerlandstr. 1 D-91058 Erlangen Bundesrepublik Deutschland ; #=========================================================================== # 3. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_experimental ; source of material: see actual publication ; _publ_section_references ; ? ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #=========================================================================== # 4.1 RESULTS FOR 1 data_fh9811 _database_code_CSD 164327 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[Cu(phen)2(CO3)]*7H2O' _chemical_formula_analytical ? _chemical_formula_sum 'C25 H30 Cu N4 O10' _chemical_formula_weight 610.07 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 9.9010(10) _cell_length_b 26.277(3) _cell_length_c 10.510(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.93(2) _cell_angle_gamma 90.00 _cell_volume 2629.4(9) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 16.30 _exptl_crystal_description rhomb _exptl_crystal_colour turquoise _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method ? _exptl_crystal_F_000 1268 _exptl_absorpt_coefficient_mu 0.896 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.0531 _exptl_absorpt_correction_T_max 0.1750 _exptl_absorpt_process_details ; Parkin S, Moezzi B, Hope H, J. Appl. Cryst. 28 (1995), 53-56. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'Siemens P4' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.96 _diffrn_reflns_number 7033 _diffrn_reflns_av_R_equivalents 0.1726 _diffrn_reflns_av_sigmaI/netI 0.0905 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 27.00 _reflns_number_total 5739 _reflns_number_observed 4355 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'XSCAnS 2.20 (Siemens An. X-Ray Instr., 1996)' _computing_cell_refinement 'XSCAnS 2.20 (Siemens An. X-Ray Instr., 1996)' _computing_data_reduction 'XSCAnS 2.20 (Siemens An. X-Ray Instr., 1996)' _computing_structure_solution 'SHELXTL 5.03 (Siemens An. X-Ray Instr., 1995)' _computing_structure_refinement 'SHELXTL 5.03 (Siemens An. X-Ray Instr., 1995)' _computing_molecular_graphics 'SHELXTL 5.03 (Siemens An. X-Ray Instr., 1995)' _computing_publication_material 'SHELXTL 5.03 (Siemens An. X-Ray Instr., 1995)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 15 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0716P)^2^+1.6006P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5724 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0752 _refine_ls_R_factor_obs 0.0533 _refine_ls_wR_factor_all 0.1413 _refine_ls_wR_factor_obs 0.1275 _refine_ls_goodness_of_fit_all 1.016 _refine_ls_goodness_of_fit_obs 1.070 _refine_ls_restrained_S_all 1.022 _refine_ls_restrained_S_obs 1.070 _refine_ls_shift/esd_max 0.051 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.89723(3) 0.121298(14) 0.76295(4) 0.02087(13) Uani 1 d . . N1 N 0.7768(2) 0.16206(10) 0.6087(3) 0.0212(5) Uani 1 d . . C2 C 0.6997(3) 0.14286(14) 0.4948(3) 0.0262(7) Uani 1 d . . C3 C 0.6184(3) 0.17300(14) 0.3931(4) 0.0310(8) Uani 1 d . . C4 C 0.6209(3) 0.22511(15) 0.4074(4) 0.0313(8) Uani 1 d . . C5 C 0.7041(3) 0.24652(13) 0.5251(3) 0.0261(7) Uani 1 d . . C6 C 0.7165(4) 0.30052(14) 0.5486(4) 0.0335(8) Uani 1 d . . C7 C 0.8024(4) 0.31969(14) 0.6600(4) 0.0338(8) Uani 1 d . . C8 C 0.8808(3) 0.28743(13) 0.7625(4) 0.0283(7) Uani 1 d . . C9 C 0.9698(4) 0.30538(15) 0.8831(4) 0.0340(8) Uani 1 d . . C10 C 1.0365(4) 0.2718(2) 0.9775(4) 0.0367(9) Uani 1 d . . C11 C 1.0137(3) 0.21931(15) 0.9543(4) 0.0313(8) Uani 1 d . . N12 N 0.9322(2) 0.20074(10) 0.8434(3) 0.0239(6) Uani 1 d . . C13 C 0.8666(3) 0.23404(12) 0.7472(3) 0.0230(6) Uani 1 d . . C14 C 0.7805(3) 0.21368(12) 0.6253(3) 0.0214(6) Uani 1 d . . C15 C 1.0637(3) 0.08755(12) 0.6285(3) 0.0246(7) Uani 1 d . . N21 N 1.0006(3) 0.08669(10) 0.9348(3) 0.0242(6) Uani 1 d . . C22 C 1.1394(3) 0.08384(13) 0.9896(4) 0.0291(7) Uani 1 d . . C23 C 1.1967(4) 0.06372(15) 1.1156(4) 0.0358(8) Uani 1 d . . C24 C 1.1099(4) 0.04651(15) 1.1889(4) 0.0343(8) Uani 1 d . . C25 C 0.9632(3) 0.04928(12) 1.1347(4) 0.0275(7) Uani 1 d . . C26 C 0.8627(4) 0.03381(14) 1.2036(4) 0.0331(8) Uani 1 d . . C27 C 0.7236(4) 0.03873(14) 1.1453(4) 0.0330(8) Uani 1 d . . C28 C 0.6706(3) 0.05837(13) 1.0153(4) 0.0271(7) Uani 1 d . . C29 C 0.5259(3) 0.06390(14) 0.9472(4) 0.0336(8) Uani 1 d . . C30 C 0.4867(4) 0.08304(15) 0.8228(4) 0.0351(8) Uani 1 d . . C31 C 0.5893(3) 0.09816(14) 0.7610(4) 0.0302(8) Uani 1 d . . N32 N 0.7270(3) 0.09435(10) 0.8214(3) 0.0243(6) Uani 1 d . . C33 C 0.7659(3) 0.07405(11) 0.9446(3) 0.0217(6) Uani 1 d . . C34 C 0.9151(3) 0.06958(11) 1.0074(3) 0.0225(6) Uani 1 d . . O11 O 0.9565(2) 0.05934(10) 0.6165(3) 0.0429(7) Uani 1 d . . O12 O 1.0695(2) 0.12761(9) 0.7045(3) 0.0322(5) Uani 1 d . . O13 O 1.1631(3) 0.07853(11) 0.5796(4) 0.0548(9) Uani 1 d . . O1 O 0.7293(3) 0.00639(10) 0.4904(3) 0.0340(6) Uani 1 d . . O2 O 0.4542(3) 0.04246(11) 0.3750(3) 0.0416(7) Uani 1 d . . O3 O 0.3238(3) 0.12979(10) 0.4605(3) 0.0387(6) Uani 1 d . . O4 O 0.4460(3) 0.20502(11) 0.6425(3) 0.0373(6) Uani 1 d . . O5 O 0.2714(3) 0.19719(11) 0.8059(3) 0.0401(6) Uani 1 d . . O6 O 0.2295(3) 0.19628(13) 1.2441(3) 0.0463(7) Uani 1 d . . O7 O 0.4011(3) 0.19123(14) 1.0768(3) 0.0477(8) Uani 1 d . . H2 H 0.7061(52) 0.1057(23) 0.4848(60) 0.080 Uiso 1 d . . H3 H 0.5620(52) 0.1581(21) 0.3142(61) 0.080 Uiso 1 d . . H4 H 0.5674(52) 0.2467(21) 0.3485(60) 0.080 Uiso 1 d . . H6 H 0.6724(53) 0.3193(22) 0.4853(60) 0.080 Uiso 1 d . . H7 H 0.8013(51) 0.3567(23) 0.6752(59) 0.080 Uiso 1 d . . H9 H 0.9826(54) 0.3394(22) 0.8922(61) 0.080 Uiso 1 d . . H10 H 1.0881(52) 0.2820(22) 1.0597(60) 0.080 Uiso 1 d . . H11 H 1.0510(52) 0.1942(22) 1.0192(59) 0.080 Uiso 1 d . . H22 H 1.1992(52) 0.0960(22) 0.9278(61) 0.080 Uiso 1 d . . H23 H 1.2933(54) 0.0658(21) 1.1501(61) 0.080 Uiso 1 d . . H24 H 1.1481(54) 0.0350(21) 1.2723(61) 0.080 Uiso 1 d . . H26 H 0.8957(51) 0.0240(22) 1.2887(61) 0.080 Uiso 1 d . . H27 H 0.6692(52) 0.0271(21) 1.2008(61) 0.080 Uiso 1 d . . H29 H 0.4604(53) 0.0560(22) 0.9997(60) 0.080 Uiso 1 d . . H31 H 0.5680(55) 0.1134(21) 0.6813(67) 0.080 Uiso 1 d . . H30 H 0.3966(53) 0.0822(22) 0.7688(57) 0.080 Uiso 1 d . . H1A H 0.7578(61) -0.0117(25) 0.4686(70) 0.080 Uiso 1 d . . H1B H 0.8030(56) 0.0213(23) 0.5393(63) 0.080 Uiso 1 d . . H2A H 0.5330(59) 0.0325(22) 0.4037(62) 0.080 Uiso 1 d . . H2B H 0.4041(54) 0.0181(23) 0.4176(61) 0.080 Uiso 1 d . . H3A H 0.2720(60) 0.1165(23) 0.4954(67) 0.080 Uiso 1 d . . H3B H 0.3672(56) 0.1076(24) 0.4309(64) 0.080 Uiso 1 d . . H4A H 0.4065(55) 0.1840(22) 0.5772(62) 0.080 Uiso 1 d . . H4B H 0.4290(56) 0.2352(24) 0.6218(63) 0.080 Uiso 1 d . . H5A H 0.3335(59) 0.1925(22) 0.7658(61) 0.080 Uiso 1 d . . H5B H 0.1968(57) 0.1728(22) 0.7666(58) 0.080 Uiso 1 d . . H6A H 0.2513(61) 0.1780(24) 1.2948(66) 0.080 Uiso 1 d . . H6B H 0.2413(60) 0.2249(24) 1.2688(66) 0.080 Uiso 1 d . . H7A H 0.3427(60) 0.1864(22) 1.1225(65) 0.080 Uiso 1 d . . H7B H 0.3586(59) 0.1923(24) 1.0033(67) 0.080 Uiso 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0207(2) 0.0212(2) 0.0202(2) 0.0032(2) 0.00470(13) 0.00117(14) N1 0.0221(11) 0.0198(13) 0.0218(13) 0.0020(11) 0.0061(10) 0.0000(9) C2 0.0276(15) 0.028(2) 0.023(2) -0.0013(14) 0.0064(12) -0.0026(13) C3 0.027(2) 0.041(2) 0.023(2) 0.002(2) 0.0039(13) -0.0031(14) C4 0.0248(15) 0.043(2) 0.027(2) 0.015(2) 0.0084(13) 0.0085(14) C5 0.0238(14) 0.028(2) 0.030(2) 0.0071(14) 0.0132(12) 0.0034(12) C6 0.036(2) 0.025(2) 0.043(2) 0.014(2) 0.018(2) 0.0073(14) C7 0.041(2) 0.021(2) 0.047(2) 0.004(2) 0.025(2) 0.0037(14) C8 0.031(2) 0.023(2) 0.038(2) -0.0050(14) 0.0200(14) -0.0019(12) C9 0.035(2) 0.029(2) 0.044(2) -0.011(2) 0.021(2) -0.0089(14) C10 0.032(2) 0.048(2) 0.032(2) -0.017(2) 0.0116(15) -0.009(2) C11 0.026(2) 0.042(2) 0.027(2) -0.002(2) 0.0089(13) 0.0000(14) N12 0.0209(12) 0.0286(14) 0.0229(14) 0.0024(12) 0.0075(10) 0.0005(10) C13 0.0224(14) 0.023(2) 0.025(2) 0.0002(13) 0.0097(12) 0.0003(11) C14 0.0204(13) 0.0211(15) 0.026(2) 0.0011(13) 0.0115(12) 0.0005(11) C15 0.0281(15) 0.0204(15) 0.026(2) 0.0034(13) 0.0096(12) 0.0026(12) N21 0.0218(12) 0.0236(13) 0.0267(15) 0.0005(11) 0.0062(10) 0.0024(10) C22 0.0239(14) 0.032(2) 0.030(2) 0.0037(15) 0.0054(13) 0.0017(13) C23 0.027(2) 0.043(2) 0.034(2) 0.005(2) 0.0019(14) 0.0045(15) C24 0.037(2) 0.037(2) 0.025(2) 0.007(2) 0.0020(14) 0.0057(15) C25 0.036(2) 0.019(2) 0.028(2) 0.0019(14) 0.0087(13) 0.0025(12) C26 0.043(2) 0.028(2) 0.029(2) 0.006(2) 0.011(2) 0.0032(14) C27 0.042(2) 0.028(2) 0.034(2) 0.005(2) 0.019(2) -0.0023(14) C28 0.030(2) 0.022(2) 0.031(2) 0.0015(14) 0.0111(13) -0.0022(12) C29 0.028(2) 0.031(2) 0.046(2) 0.002(2) 0.0158(15) -0.0029(13) C30 0.025(2) 0.037(2) 0.042(2) 0.000(2) 0.0068(14) -0.0003(14) C31 0.026(2) 0.032(2) 0.029(2) -0.003(2) 0.0016(13) 0.0024(13) N32 0.0239(12) 0.0220(14) 0.0261(15) 0.0011(11) 0.0054(10) 0.0028(10) C33 0.0263(14) 0.0176(14) 0.022(2) 0.0017(12) 0.0076(12) 0.0022(11) C34 0.0252(14) 0.0163(14) 0.026(2) 0.0018(12) 0.0071(12) 0.0017(11) O11 0.0342(13) 0.0357(14) 0.054(2) 0.0009(13) 0.0036(12) -0.0095(11) O12 0.0397(12) 0.0242(12) 0.0299(14) -0.0030(10) 0.0050(10) -0.0028(10) O13 0.069(2) 0.037(2) 0.080(2) 0.003(2) 0.056(2) 0.0076(14) O1 0.0258(11) 0.0283(14) 0.046(2) -0.0013(12) 0.0067(10) 0.0018(10) O2 0.0351(13) 0.040(2) 0.046(2) 0.0144(13) 0.0058(12) 0.0048(11) O3 0.047(2) 0.0303(15) 0.041(2) 0.0020(12) 0.0165(12) -0.0019(11) O4 0.0377(13) 0.040(2) 0.035(2) -0.0042(13) 0.0111(11) -0.0037(12) O5 0.0421(14) 0.049(2) 0.0323(15) -0.0078(13) 0.0151(12) -0.0151(13) O6 0.048(2) 0.054(2) 0.038(2) 0.0113(15) 0.0145(13) 0.0047(15) O7 0.0384(15) 0.068(2) 0.037(2) -0.001(2) 0.0108(12) -0.0005(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O12 1.972(3) . ? Cu1 N21 2.030(3) . ? Cu1 N1 2.034(3) . ? Cu1 N32 2.071(3) . ? Cu1 N12 2.243(3) . ? Cu1 O11 2.421(3) . ? N1 C2 1.330(4) . ? N1 C14 1.367(4) . ? C2 C3 1.395(5) . ? C2 H2 0.99(6) . ? C3 C4 1.377(5) . ? C3 H3 0.95(6) . ? C4 C5 1.402(5) . ? C4 H4 0.90(6) . ? C5 C14 1.410(4) . ? C5 C6 1.440(5) . ? C6 C7 1.343(6) . ? C6 H6 0.85(6) . ? C7 C8 1.422(5) . ? C7 H7 0.99(6) . ? C8 C9 1.411(5) . ? C8 C13 1.415(4) . ? C9 C10 1.356(6) . ? C9 H9 0.90(6) . ? C10 C11 1.409(5) . ? C10 H10 0.92(6) . ? C11 N12 1.315(4) . ? C11 H11 0.95(6) . ? N12 C13 1.360(4) . ? C13 C14 1.434(4) . ? C15 O13 1.252(4) . ? C15 O11 1.272(4) . ? C15 O12 1.313(4) . ? N21 C22 1.338(4) . ? N21 C34 1.363(4) . ? C22 C23 1.394(5) . ? C22 H22 1.04(6) . ? C23 C24 1.378(6) . ? C23 H23 0.93(5) . ? C24 C25 1.409(5) . ? C24 H24 0.91(6) . ? C25 C34 1.397(5) . ? C25 C26 1.441(5) . ? C26 C27 1.351(5) . ? C26 H26 0.90(6) . ? C27 C28 1.419(5) . ? C27 H27 0.95(6) . ? C28 C33 1.413(5) . ? C28 C29 1.422(5) . ? C29 C30 1.354(6) . ? C29 H29 0.98(6) . ? C30 C31 1.405(5) . ? C30 H30 0.92(5) . ? C31 N32 1.341(4) . ? C31 H31 0.90(6) . ? N32 C33 1.355(4) . ? C33 C34 1.448(4) . ? O1 H1A 0.63(6) . ? O1 H1B 0.86(6) . ? O2 H2A 0.80(6) . ? O2 H2B 0.99(6) . ? O3 H3A 0.79(6) . ? O3 H3B 0.83(6) . ? O4 H4A 0.88(6) . ? O4 H4B 0.83(6) . ? O5 H5A 0.84(6) . ? O5 H5B 0.98(6) . ? O6 H6A 0.71(6) . ? O6 H6B 0.79(6) . ? O7 H7A 0.86(6) . ? O7 H7B 0.77(6) . ? 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 O12 Cu1 N21 92.67(11) . . ? O12 Cu1 N1 94.35(10) . . ? N21 Cu1 N1 170.80(11) . . ? O12 Cu1 N32 164.82(10) . . ? N21 Cu1 N32 80.55(10) . . ? N1 Cu1 N32 93.98(10) . . ? O12 Cu1 N12 88.98(9) . . ? N21 Cu1 N12 95.36(10) . . ? N1 Cu1 N12 78.84(10) . . ? N32 Cu1 N12 105.09(10) . . ? O12 Cu1 O11 58.47(9) . . ? N21 Cu1 O11 96.51(10) . . ? N1 Cu1 O11 92.23(10) . . ? N32 Cu1 O11 108.53(10) . . ? N12 Cu1 O11 145.72(9) . . ? C2 N1 C14 118.7(3) . . ? C2 N1 Cu1 125.7(2) . . ? C14 N1 Cu1 115.6(2) . . ? N1 C2 C3 122.8(3) . . ? N1 C2 H2 115.7(34) . . ? C3 C2 H2 121.4(34) . . ? C4 C3 C2 119.4(3) . . ? C4 C3 H3 119.6(34) . . ? C2 C3 H3 120.9(35) . . ? C3 C4 C5 118.9(3) . . ? C3 C4 H4 124.3(36) . . ? C5 C4 H4 116.6(36) . . ? C4 C5 C14 118.6(3) . . ? C4 C5 C6 123.2(3) . . ? C14 C5 C6 118.2(3) . . ? C7 C6 C5 121.5(3) . . ? C7 C6 H6 122.2(39) . . ? C5 C6 H6 116.0(40) . . ? C6 C7 C8 121.4(3) . . ? C6 C7 H7 118.6(33) . . ? C8 C7 H7 119.6(34) . . ? C9 C8 C13 116.8(3) . . ? C9 C8 C7 123.9(3) . . ? C13 C8 C7 119.3(3) . . ? C10 C9 C8 119.9(3) . . ? C10 C9 H9 122.6(38) . . ? C8 C9 H9 117.4(38) . . ? C9 C10 C11 119.2(3) . . ? C9 C10 H10 122.3(37) . . ? C11 C10 H10 118.2(37) . . ? N12 C11 C10 123.2(4) . . ? N12 C11 H11 113.8(35) . . ? C10 C11 H11 122.9(35) . . ? C11 N12 C13 118.1(3) . . ? C11 N12 Cu1 132.3(2) . . ? C13 N12 Cu1 109.0(2) . . ? N12 C13 C8 122.8(3) . . ? N12 C13 C14 118.0(3) . . ? C8 C13 C14 119.2(3) . . ? N1 C14 C5 121.5(3) . . ? N1 C14 C13 118.2(3) . . ? C5 C14 C13 120.3(3) . . ? O13 C15 O11 125.2(3) . . ? O13 C15 O12 119.6(3) . . ? O11 C15 O12 115.1(3) . . ? C22 N21 C34 117.6(3) . . ? C22 N21 Cu1 128.0(2) . . ? C34 N21 Cu1 114.0(2) . . ? N21 C22 C23 122.2(3) . . ? N21 C22 H22 114.0(30) . . ? C23 C22 H22 123.8(30) . . ? C24 C23 C22 120.1(3) . . ? C24 C23 H23 122.4(38) . . ? C22 C23 H23 117.1(37) . . ? C23 C24 C25 119.3(3) . . ? C23 C24 H24 119.4(33) . . ? C25 C24 H24 121.2(33) . . ? C34 C25 C24 116.7(3) . . ? C34 C25 C26 119.2(3) . . ? C24 C25 C26 124.1(3) . . ? C27 C26 C25 120.2(4) . . ? C27 C26 H26 121.6(33) . . ? C25 C26 H26 117.9(33) . . ? C26 C27 C28 122.2(3) . . ? C26 C27 H27 111.8(34) . . ? C28 C27 H27 126.0(34) . . ? C33 C28 C27 119.2(3) . . ? C33 C28 C29 115.5(3) . . ? C27 C28 C29 125.2(3) . . ? C30 C29 C28 120.4(3) . . ? C30 C29 H29 124.2(33) . . ? C28 C29 H29 115.2(33) . . ? C29 C30 C31 120.0(3) . . ? C29 C30 H30 124.2(36) . . ? C31 C30 H30 115.1(36) . . ? N32 C31 C30 122.0(4) . . ? N32 C31 H31 115.0(34) . . ? C30 C31 H31 122.8(34) . . ? C31 N32 C33 117.8(3) . . ? C31 N32 Cu1 129.7(3) . . ? C33 N32 Cu1 112.2(2) . . ? N32 C33 C28 124.2(3) . . ? N32 C33 C34 117.0(3) . . ? C28 C33 C34 118.8(3) . . ? N21 C34 C25 124.1(3) . . ? N21 C34 C33 115.5(3) . . ? C25 C34 C33 120.3(3) . . ? C15 O11 Cu1 83.5(2) . . ? C15 O12 Cu1 103.0(2) . . ? H1A O1 H1B 99.6(61) . . ? H2A O2 H2B 100.1(50) . . ? H3A O3 H3B 109.4(60) . . ? H4A O4 H4B 112.4(54) . . ? H5A O5 H5B 105.2(51) . . ? H6A O6 H6B 114.3(69) . . ? H7A O7 H7B 107.4(55) . . ? 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 O1 H1A O13 0.63(6) 2.04(6) 2.662(4) 169(8) 3_756 O1 H1B O11 0.86(6) 1.82(6) 2.668(4) 170(6) . O2 H2A O1 0.80(6) 2.03(6) 2.824(4) 175(6) . O2 H2B O1 0.99(6) 1.95(6) 2.891(4) 158(5) 3_656 O3 H3A O13 0.79(6) 1.86(6) 2.647(4) 174(6) 1_455 O3 H3B O2 0.84(6) 2.07(6) 2.894(4) 168(6) . O4 H4A O3 0.89(6) 1.91(6) 2.786(4) 170(6) . O4 H4B O7 0.83(6) 1.99(6) 2.817(5) 176(5) 4_565 O5 H5A O4 0.85(6) 1.95(6) 2.760(4) 159(6) . O5 H5B O12 0.97(6) 1.73(6) 2.703(4) 177(5) 1_455 O6 H6A O3 0.71(6) 2.11(6) 2.816(4) 174(7) 1_556 O6 H6B O5 0.79(6) 2.09(6) 2.878(5) 172(7) 4_566 O7 H7A O6 0.86(6) 1.94(7) 2.763(5) 162(6) . O7 H7B O5 0.77(6) 2.02(7) 2.788(4) 172(6) . _refine_diff_density_max 0.606 _refine_diff_density_min -1.454 _refine_diff_density_rms 0.101 #===END Of DATA FOR 1 # 4.2 RESULTS FOR 2 data_fh9813 _database_code_CSD 164328 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[Cu(CO3)(phen)2] * 11 H2O' _chemical_formula_analytical ? _chemical_formula_sum 'C25 H38 Cu N4 O14' _chemical_formula_weight 682.13 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.007(2) _cell_length_b 11.683(2) _cell_length_c 13.345(2) _cell_angle_alpha 78.180(10) _cell_angle_beta 75.83(2) _cell_angle_gamma 70.37(3) _cell_volume 1553.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 36 _cell_measurement_theta_min 3.20 _cell_measurement_theta_max 19.45 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.58 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method ? _exptl_crystal_F_000 714 _exptl_absorpt_coefficient_mu 0.776 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.4836 _exptl_absorpt_correction_T_max 0.5178 _exptl_absorpt_process_details ; North A C T, Phillips D C, Mathews F S, Acat Cryst. A24 (1968), 351-359. ; _exptl_special_details ; As the cyrstals underwent very rapid weathering when removed from the solvent leading to their destruction a suitable crystal was sealed in a capillary that was filled with the mother liquor. ; _diffrn_ambient_temperature 295(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 'Siemens P4' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.45 _diffrn_reflns_number 7840 _diffrn_reflns_av_R_equivalents 0.0113 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 27.01 _reflns_number_total 6759 _reflns_number_observed 5545 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'XSCAnS 2.20 (Siemens An. X-Ray Instr., 1996)' _computing_cell_refinement 'XSCAnS 2.20 (Siemens An. X-Ray Instr., 1996)' _computing_data_reduction 'XSCAnS 2.20 (Siemens An. X-Ray Instr., 1996)' _computing_structure_solution 'SHELXTL 5.03 (Siemens An. X-Ray Instr., 1995)' _computing_structure_refinement 'SHELXTL 5.03 (Siemens An. X-Ray Instr., 1995)' _computing_molecular_graphics 'SHELXTL 5.03 (Siemens An. X-Ray Instr., 1995)' _computing_publication_material 'SHELXTL 5.03 (Siemens An. X-Ray Instr., 1995)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The compound crystallizes with 11 molecules of H~2~O as a solvate. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+0.6511P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment 'refxyz except solvate H atoms noref' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0210(15) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6759 _refine_ls_number_parameters 446 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0585 _refine_ls_R_factor_obs 0.0447 _refine_ls_wR_factor_all 0.1219 _refine_ls_wR_factor_obs 0.1128 _refine_ls_goodness_of_fit_all 1.075 _refine_ls_goodness_of_fit_obs 1.105 _refine_ls_restrained_S_all 1.075 _refine_ls_restrained_S_obs 1.105 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 1.89455(3) -0.25976(3) 0.75316(2) 0.03633(12) Uani 1 d . . N1 N 2.0153(2) -0.1809(2) 0.6432(2) 0.0387(4) Uani 1 d . . C2 C 2.0849(3) -0.1159(3) 0.6612(2) 0.0473(6) Uani 1 d . . C3 C 2.1707(3) -0.0686(3) 0.5827(3) 0.0561(8) Uani 1 d . . C4 C 2.1845(3) -0.0875(3) 0.4824(3) 0.0548(7) Uani 1 d . . C5 C 2.1138(3) -0.1560(2) 0.4602(2) 0.0460(6) Uani 1 d . . C6 C 2.1228(3) -0.1804(3) 0.3575(2) 0.0583(8) Uani 1 d . . C7 C 2.0537(4) -0.2459(3) 0.3399(2) 0.0604(8) Uani 1 d . . C8 C 1.9677(3) -0.2962(3) 0.4231(2) 0.0477(6) Uani 1 d . . C9 C 1.8944(4) -0.3674(3) 0.4094(3) 0.0621(8) Uani 1 d . . C10 C 1.8192(3) -0.4138(3) 0.4930(3) 0.0622(8) Uani 1 d . . C11 C 1.8149(3) -0.3894(3) 0.5918(3) 0.0526(7) Uani 1 d . . N12 N 1.8814(2) -0.3219(2) 0.6084(2) 0.0419(5) Uani 1 d . . C13 C 1.9565(2) -0.2752(2) 0.5252(2) 0.0383(5) Uani 1 d . . C14 C 2.0302(2) -0.2024(2) 0.5441(2) 0.0379(5) Uani 1 d . . C15 C 1.7344(3) -0.0506(2) 0.8180(2) 0.0447(6) Uani 1 d . . N21 N 1.7954(2) -0.3571(2) 0.8645(2) 0.0397(5) Uani 1 d . . C22 C 1.6674(3) -0.3251(3) 0.9060(2) 0.0498(7) Uani 1 d . . C23 C 1.6115(3) -0.4042(3) 0.9815(3) 0.0599(8) Uani 1 d . . C24 C 1.6872(3) -0.5189(3) 1.0132(2) 0.0579(8) Uani 1 d . . C25 C 1.8228(3) -0.5564(3) 0.9704(2) 0.0462(6) Uani 1 d . . C26 C 1.9126(4) -0.6734(3) 0.9990(2) 0.0553(8) Uani 1 d . . C27 C 2.0409(4) -0.7013(3) 0.9571(2) 0.0537(7) Uani 1 d . . C28 C 2.0940(3) -0.6156(2) 0.8815(2) 0.0449(6) Uani 1 d . . C29 C 2.2272(3) -0.6384(3) 0.8338(3) 0.0545(7) Uani 1 d . . C30 C 2.2670(3) -0.5502(3) 0.7645(3) 0.0559(7) Uani 1 d . . C31 C 2.1764(3) -0.4371(3) 0.7409(2) 0.0484(6) Uani 1 d . . N32 N 2.0495(2) -0.4117(2) 0.7832(2) 0.0395(5) Uani 1 d . . C33 C 2.0085(3) -0.5001(2) 0.8526(2) 0.0374(5) Uani 1 d . . C34 C 1.8712(3) -0.4703(2) 0.8968(2) 0.0374(5) Uani 1 d . . O11 O 1.8300(3) -0.0874(2) 0.8650(2) 0.0731(7) Uani 1 d . . O12 O 1.7398(2) -0.1146(2) 0.74710(14) 0.0462(4) Uani 1 d . . O13 O 1.6380(2) 0.0440(2) 0.8356(2) 0.0727(7) Uani 1 d . . O21 O 1.9609(3) 0.0507(3) 0.9035(2) 0.0802(7) Uani 1 d . . O22 O 1.5759(3) -0.1194(3) 0.6218(2) 0.0847(8) Uani 1 d . . O23 O 1.6981(3) 0.2260(3) 0.9048(3) 0.0945(9) Uani 1 d . . O24 O 1.3833(3) 0.1080(3) 0.5990(2) 0.0915(9) Uani 1 d . . O25 O 1.5302(3) 0.2220(3) 0.6758(3) 0.0931(9) Uani 1 d . . O26 O 1.3745(3) 0.0431(4) 0.9148(2) 0.1168(13) Uani 1 d . . O27 O 0.2045(3) 0.0789(4) 0.7819(2) 0.1068(11) Uani 1 d . . O28 O 2.5967(4) -0.6148(4) 0.4900(4) 0.157(2) Uani 1 d . . O29 O 2.3831(4) -0.4327(3) 0.2528(3) 0.1269(13) Uani 1 d . . O30 O 2.6751(5) -0.8023(4) 0.1389(4) 0.168(2) Uani 1 d . . O31 O 2.5325(4) -0.6793(4) 0.3090(4) 0.145(2) Uani 1 d . . H2 H 2.0728(37) -0.0994(35) 0.7280(31) 0.080 Uiso 1 d . . H3 H 2.2160(37) -0.0247(36) 0.5982(30) 0.080 Uiso 1 d . . H4 H 2.2399(38) -0.0567(35) 0.4325(31) 0.080 Uiso 1 d . . H6 H 2.1763(38) -0.1553(36) 0.3089(31) 0.080 Uiso 1 d . . H7 H 2.0598(38) -0.2640(35) 0.2734(31) 0.080 Uiso 1 d . . H9 H 1.9019(36) -0.3849(34) 0.3396(30) 0.080 Uiso 1 d . . H10 H 1.7703(38) -0.4563(36) 0.4926(30) 0.080 Uiso 1 d . . H11 H 1.7680(38) -0.4161(36) 0.6440(31) 0.080 Uiso 1 d . . H22 H 1.6181(37) -0.2535(36) 0.8861(31) 0.080 Uiso 1 d . . H23 H 1.5266(39) -0.3777(35) 1.0056(30) 0.080 Uiso 1 d . . H24 H 1.6519(36) -0.5757(35) 1.0676(29) 0.080 Uiso 1 d . . H26 H 1.8835(37) -0.7276(35) 1.0519(30) 0.080 Uiso 1 d . . H27 H 2.1017(38) -0.7732(36) 0.9765(30) 0.080 Uiso 1 d . . H29 H 2.2858(38) -0.7106(36) 0.8520(30) 0.080 Uiso 1 d . . H30 H 2.3477(39) -0.5625(36) 0.7319(30) 0.080 Uiso 1 d . . H31 H 2.1991(37) -0.3830(36) 0.6899(30) 0.080 Uiso 1 d . . H21A H 1.9205 -0.0006 0.8882 0.080 Uiso 1 d . . H21B H 2.0033 0.0000 0.9576 0.080 Uiso 1 d . . H22A H 1.5195 -0.0728 0.6350 0.080 Uiso 1 d . . H22B H 1.6237 -0.1166 0.6627 0.080 Uiso 1 d . . H23A H 1.6528 0.2069 0.8889 0.080 Uiso 1 d . . H23B H 1.6646 0.2194 0.9772 0.080 Uiso 1 d . . H24A H 1.3276 0.1170 0.6455 0.080 Uiso 1 d . . H24B H 1.3819 0.1256 0.5437 0.080 Uiso 1 d . . H25A H 1.4790 0.1938 0.6586 0.080 Uiso 1 d . . H25B H 1.5629 0.1626 0.7230 0.080 Uiso 1 d . . H26A H 1.4496 0.0554 0.9075 0.080 Uiso 1 d . . H26B H 1.3592 0.0295 0.9796 0.080 Uiso 1 d . . H27A H 0.2553 0.0679 0.8268 0.080 Uiso 1 d . . H27B H 0.1486 0.0562 0.8040 0.080 Uiso 1 d . . H28A H 2.7029 -0.5988 0.4513 0.080 Uiso 1 d . . H28B H 2.5206 -0.6077 0.5194 0.080 Uiso 1 d . . H29A H 2.3170 -0.4391 0.2212 0.080 Uiso 1 d . . H29B H 2.4299 -0.3991 0.2095 0.080 Uiso 1 d . . H30A H 2.5918 -0.7761 0.2136 0.080 Uiso 1 d . . H30B H 2.6937 -0.8829 0.1664 0.080 Uiso 1 d . . H31A H 2.6006 -0.7166 0.2793 0.080 Uiso 1 d . . H31B H 2.4940 -0.6159 0.2892 0.080 Uiso 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0381(2) 0.0342(2) 0.0348(2) -0.00387(11) -0.00506(12) -0.01032(12) N1 0.0418(11) 0.0343(10) 0.0396(11) -0.0035(8) -0.0069(9) -0.0122(9) C2 0.051(2) 0.0416(14) 0.052(2) -0.0079(12) -0.0096(13) -0.0163(12) C3 0.050(2) 0.045(2) 0.076(2) -0.0087(14) -0.0070(15) -0.0208(13) C4 0.046(2) 0.0432(15) 0.065(2) -0.0007(13) 0.0027(14) -0.0135(13) C5 0.0410(14) 0.0386(13) 0.0469(14) -0.0014(11) -0.0020(11) -0.0043(11) C6 0.063(2) 0.057(2) 0.0389(15) -0.0010(13) 0.0050(14) -0.011(2) C7 0.071(2) 0.063(2) 0.0359(14) -0.0077(13) -0.0068(14) -0.008(2) C8 0.052(2) 0.0459(14) 0.0406(13) -0.0108(11) -0.0150(12) -0.0013(12) C9 0.072(2) 0.065(2) 0.054(2) -0.020(2) -0.023(2) -0.011(2) C10 0.061(2) 0.062(2) 0.076(2) -0.024(2) -0.024(2) -0.019(2) C11 0.051(2) 0.053(2) 0.059(2) -0.0144(14) -0.0088(14) -0.0192(13) N12 0.0424(11) 0.0399(11) 0.0450(12) -0.0090(9) -0.0078(9) -0.0128(9) C13 0.0404(13) 0.0332(11) 0.0371(12) -0.0070(9) -0.0084(10) -0.0035(10) C14 0.0399(13) 0.0323(11) 0.0356(12) -0.0030(9) -0.0062(10) -0.0049(10) C15 0.056(2) 0.0348(12) 0.0426(14) -0.0036(10) -0.0088(12) -0.0147(12) N21 0.0407(11) 0.0396(11) 0.0400(11) -0.0063(9) -0.0053(9) -0.0147(9) C22 0.045(2) 0.051(2) 0.053(2) -0.0083(13) -0.0026(13) -0.0170(13) C23 0.050(2) 0.073(2) 0.061(2) -0.014(2) 0.0038(15) -0.031(2) C24 0.071(2) 0.063(2) 0.050(2) -0.0015(14) -0.0053(15) -0.042(2) C25 0.063(2) 0.0464(14) 0.0390(13) -0.0048(11) -0.0124(12) -0.0276(13) C26 0.087(2) 0.0424(15) 0.044(2) 0.0028(12) -0.020(2) -0.030(2) C27 0.078(2) 0.0363(14) 0.050(2) -0.0011(12) -0.027(2) -0.0132(14) C28 0.059(2) 0.0366(13) 0.0441(14) -0.0104(10) -0.0222(12) -0.0086(12) C29 0.055(2) 0.045(2) 0.063(2) -0.0144(14) -0.0277(15) 0.0014(13) C30 0.0414(15) 0.056(2) 0.067(2) -0.0148(15) -0.0112(14) -0.0064(13) C31 0.0413(14) 0.048(2) 0.053(2) -0.0077(12) -0.0081(12) -0.0097(12) N32 0.0411(11) 0.0381(11) 0.0383(11) -0.0061(8) -0.0068(9) -0.0106(9) C33 0.0470(14) 0.0348(12) 0.0344(12) -0.0079(9) -0.0129(10) -0.0119(10) C34 0.0478(14) 0.0360(12) 0.0347(12) -0.0062(9) -0.0107(10) -0.0179(11) O11 0.106(2) 0.0486(12) 0.077(2) -0.0017(11) -0.0542(15) -0.0170(12) O12 0.0490(11) 0.0437(10) 0.0471(10) -0.0089(8) -0.0140(8) -0.0103(8) O13 0.0616(14) 0.0504(12) 0.100(2) -0.0317(12) 0.0005(13) -0.0073(11) O21 0.096(2) 0.096(2) 0.068(2) -0.0049(14) -0.0289(14) -0.047(2) O22 0.082(2) 0.080(2) 0.098(2) -0.0139(15) -0.050(2) -0.0062(14) O23 0.099(2) 0.084(2) 0.108(2) -0.047(2) 0.005(2) -0.033(2) O24 0.073(2) 0.108(2) 0.077(2) 0.000(2) -0.0170(14) -0.012(2) O25 0.084(2) 0.075(2) 0.107(2) -0.010(2) -0.016(2) -0.0093(15) O26 0.079(2) 0.203(4) 0.064(2) 0.017(2) -0.0195(15) -0.054(2) O27 0.084(2) 0.168(3) 0.085(2) -0.036(2) -0.007(2) -0.055(2) O28 0.086(2) 0.097(3) 0.236(5) 0.026(3) 0.002(3) -0.016(2) O29 0.096(2) 0.106(3) 0.156(3) -0.003(2) -0.010(2) -0.021(2) O30 0.193(5) 0.097(3) 0.160(4) 0.004(3) 0.048(3) -0.046(3) O31 0.110(3) 0.101(3) 0.197(4) -0.011(3) -0.017(3) -0.009(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 Cu1 O12 1.964(2) . ? Cu1 N21 2.010(2) . ? Cu1 N1 2.021(2) . ? Cu1 N32 2.056(2) . ? Cu1 N12 2.250(2) . ? N1 C2 1.333(3) . ? N1 C14 1.357(3) . ? C2 C3 1.387(4) . ? C2 H2 0.92(4) . ? C3 C4 1.365(5) . ? C3 H3 0.90(4) . ? C4 C5 1.401(4) . ? C4 H4 0.89(4) . ? C5 C14 1.405(4) . ? C5 C6 1.430(4) . ? C6 C7 1.331(5) . ? C6 H6 0.84(4) . ? C7 C8 1.437(4) . ? C7 H7 0.93(4) . ? C8 C9 1.401(5) . ? C8 C13 1.403(4) . ? C9 C10 1.351(5) . ? C9 H9 0.97(4) . ? C10 C11 1.390(5) . ? C10 H10 0.85(4) . ? C11 N12 1.321(4) . ? C11 H11 0.83(4) . ? N12 C13 1.348(3) . ? C13 C14 1.447(4) . ? C15 O11 1.262(4) . ? C15 O13 1.264(3) . ? C15 O12 1.300(3) . ? N21 C22 1.334(4) . ? N21 C34 1.353(3) . ? C22 C23 1.396(4) . ? C22 H22 0.86(4) . ? C23 C24 1.363(5) . ? C23 H23 0.88(4) . ? C24 C25 1.411(4) . ? C24 H24 0.98(4) . ? C25 C34 1.399(3) . ? C25 C26 1.433(4) . ? C26 C27 1.339(5) . ? C26 H26 0.92(4) . ? C27 C28 1.432(4) . ? C27 H27 0.92(4) . ? C28 C33 1.403(4) . ? C28 C29 1.405(4) . ? C29 C30 1.351(5) . ? C29 H29 0.90(4) . ? C30 C31 1.392(4) . ? C30 H30 0.87(4) . ? C31 N32 1.327(3) . ? C31 H31 0.88(4) . ? N32 C33 1.358(3) . ? C33 C34 1.431(4) . ? O21 H21A 0.934(3) . ? O21 H21B 0.945(3) . ? O22 H22A 0.686(3) . ? O22 H22B 0.857(2) . ? O23 H23A 0.699(3) . ? O23 H23B 0.944(3) . ? O24 H24A 0.754(3) . ? O24 H24B 0.726(3) . ? O25 H25A 0.835(3) . ? O25 H25B 0.878(3) . ? O26 H26A 0.864(3) . ? O26 H26B 0.832(3) . ? O27 H27A 0.879(3) . ? O27 H27B 0.724(3) . ? O28 H28A 1.217(4) . ? O28 H28B 0.817(4) . ? O29 H29A 0.955(4) . ? O29 H29B 0.807(4) . ? O30 H30A 1.191(4) . ? O30 H30B 0.911(4) . ? O31 H31A 0.784(4) . ? O31 H31B 0.750(4) . ? 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 O12 Cu1 N21 93.27(8) . . ? O12 Cu1 N1 94.22(8) . . ? N21 Cu1 N1 172.50(8) . . ? O12 Cu1 N32 171.43(8) . . ? N21 Cu1 N32 81.18(9) . . ? N1 Cu1 N32 91.33(8) . . ? O12 Cu1 N12 94.50(8) . . ? N21 Cu1 N12 101.15(8) . . ? N1 Cu1 N12 78.80(8) . . ? N32 Cu1 N12 92.99(8) . . ? C2 N1 C14 118.5(2) . . ? C2 N1 Cu1 125.4(2) . . ? C14 N1 Cu1 116.0(2) . . ? N1 C2 C3 122.7(3) . . ? N1 C2 H2 118.4(24) . . ? C3 C2 H2 118.9(24) . . ? C4 C3 C2 119.4(3) . . ? C4 C3 H3 120.6(25) . . ? C2 C3 H3 119.9(25) . . ? C3 C4 C5 119.7(3) . . ? C3 C4 H4 118.7(25) . . ? C5 C4 H4 121.5(25) . . ? C4 C5 C14 117.5(3) . . ? C4 C5 C6 123.3(3) . . ? C14 C5 C6 119.1(3) . . ? C7 C6 C5 121.4(3) . . ? C7 C6 H6 120.8(27) . . ? C5 C6 H6 117.7(28) . . ? C6 C7 C8 121.7(3) . . ? C6 C7 H7 122.4(25) . . ? C8 C7 H7 115.9(25) . . ? C9 C8 C13 117.0(3) . . ? C9 C8 C7 124.1(3) . . ? C13 C8 C7 118.9(3) . . ? C10 C9 C8 119.7(3) . . ? C10 C9 H9 121.6(23) . . ? C8 C9 H9 118.6(23) . . ? C9 C10 C11 119.5(3) . . ? C9 C10 H10 126.8(27) . . ? C11 C10 H10 113.7(27) . . ? N12 C11 C10 122.9(3) . . ? N12 C11 H11 116.3(28) . . ? C10 C11 H11 120.8(28) . . ? C11 N12 C13 117.9(2) . . ? C11 N12 Cu1 132.9(2) . . ? C13 N12 Cu1 109.2(2) . . ? N12 C13 C8 122.9(2) . . ? N12 C13 C14 117.7(2) . . ? C8 C13 C14 119.4(2) . . ? N1 C14 C5 122.2(2) . . ? N1 C14 C13 118.3(2) . . ? C5 C14 C13 119.6(2) . . ? O11 C15 O13 123.6(3) . . ? O11 C15 O12 116.4(2) . . ? O13 C15 O12 120.0(3) . . ? C22 N21 C34 118.2(2) . . ? C22 N21 Cu1 128.2(2) . . ? C34 N21 Cu1 113.5(2) . . ? N21 C22 C23 121.8(3) . . ? N21 C22 H22 119.2(26) . . ? C23 C22 H22 119.1(26) . . ? C24 C23 C22 120.1(3) . . ? C24 C23 H23 122.5(26) . . ? C22 C23 H23 117.4(26) . . ? C23 C24 C25 119.6(3) . . ? C23 C24 H24 122.3(22) . . ? C25 C24 H24 118.0(22) . . ? C34 C25 C24 116.4(3) . . ? C34 C25 C26 118.9(3) . . ? C24 C25 C26 124.7(3) . . ? C27 C26 C25 121.3(3) . . ? C27 C26 H26 118.8(24) . . ? C25 C26 H26 119.6(24) . . ? C26 C27 C28 121.4(3) . . ? C26 C27 H27 123.6(24) . . ? C28 C27 H27 114.9(24) . . ? C33 C28 C29 116.9(3) . . ? C33 C28 C27 118.5(3) . . ? C29 C28 C27 124.6(3) . . ? C30 C29 C28 119.7(3) . . ? C30 C29 H29 120.6(25) . . ? C28 C29 H29 119.7(25) . . ? C29 C30 C31 120.0(3) . . ? C29 C30 H30 121.9(27) . . ? C31 C30 H30 118.1(27) . . ? N32 C31 C30 122.5(3) . . ? N32 C31 H31 116.4(25) . . ? C30 C31 H31 120.5(26) . . ? C31 N32 C33 117.9(2) . . ? C31 N32 Cu1 130.2(2) . . ? C33 N32 Cu1 111.7(2) . . ? N32 C33 C28 123.0(2) . . ? N32 C33 C34 116.7(2) . . ? C28 C33 C34 120.3(2) . . ? N21 C34 C25 123.8(2) . . ? N21 C34 C33 116.5(2) . . ? C25 C34 C33 119.7(2) . . ? C15 O12 Cu1 107.2(2) . . ? H21A O21 H21B 101.2(3) . . ? H22A O22 H22B 101.9(3) . . ? H23A O23 H23B 99.0(3) . . ? H24A O24 H24B 129.8(4) . . ? H25A O25 H25B 101.3(3) . . ? H26A O26 H26B 97.3(3) . . ? H27A O27 H27B 112.7(4) . . ? H28A O28 H28B 165.2(5) . . ? H29A O29 H29B 108.6(5) . . ? H30A O30 H30B 90.0(3) . . ? H31A O31 H31B 124.3(6) . . ? 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 O21 H21A O11 0.93 1.75 2.686(3) 174.4 . O21 H21B O21 0.95 1.92 2.815(5) 156.8 2_957 O22 H22A O24 0.69 2.18 2.802(4) 151.3 . O22 H22B O12 0.86 1.91 2.763(3) 176.3 . O23 H23A O13 0.70 2.23 2.804(4) 140.2 . O23 H23B O30 0.94 2.15 3.030(6) 155.2 1_466 O24 H24A O27 0.75 2.05 2.775(4) 160.7 1_655 O24 H24B O22 0.73 2.15 2.852(4) 161.3 2_856 O25 H25A O24 0.84 2.05 2.873(5) 169.6 . O25 H25B O13 0.88 1.96 2.836(4) 173.7 . O26 H26A O13 0.86 2.03 2.836(4) 154.2 . O27 H27A O26 0.88 1.88 2.760(4) 175.8 1_455 O27 H27B O21 0.72 2.18 2.859(4) 156.9 1_355 _refine_diff_density_max 0.481 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.056 #===END OF DATA FOR 2 # 4.3 RESULTS FOR 3 data_fh9812 _database_code_CSD 164329 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ; [\m-CO~3~{Cu(phen)~2~}~2~](ClO~4~)2 * 4.25 H~2~O ; _chemical_formula_analytical ? _chemical_formula_sum 'C49 H40.50 Cl2 Cu2 N8 O15.25' _chemical_formula_weight 1183.37 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' .3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4880(10) _cell_length_b 12.8320(10) _cell_length_c 30.367(4) _cell_angle_alpha 90.050(10) _cell_angle_beta 91.930(10) _cell_angle_gamma 94.780(10) _cell_volume 4846.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 45 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 10.60 _exptl_crystal_description fragment _exptl_crystal_colour blue _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.622 _exptl_crystal_density_method ? _exptl_crystal_F_000 2418 _exptl_absorpt_coefficient_mu 1.069 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.5267 _exptl_absorpt_correction_T_max 0.6806 ; North A C T, Phillips D C, Mathews F S, Acta Cryst. A24 (1968), 351-359. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Siemens P4' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5.49 _diffrn_reflns_number 19647 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_sigmaI/netI 0.1576 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 25.00 _reflns_number_total 17065 _reflns_number_observed 7307 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'XSCAnS 2.20 (Siemens An. X-Ray Instr., 1996)' _computing_cell_refinement 'XSCAnS 2.20 (Siemens An. X-Ray Instr., 1996)' _computing_data_reduction 'XSCAnS 2.20 (Siemens An. X-Ray Instr., 1996)' _computing_structure_solution 'SHELXTL 5.03 (Siemens An. X-Ray Instr., 1995)' _computing_structure_refinement 'SHELXTL 5.03 (Siemens An. X-Ray Instr., 1995)' _computing_molecular_graphics 'SHELXTL 5.03 (Siemens An. X-Ray Instr., 1995)' _computing_publication_material 'SHELXTL 5.03 (Siemens An. X-Ray Instr., 1995)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The asymmetric unit contains 2 independent molecules. The compound crystallizes with 4.25 molecules H~2~O per formula unit. No H atoms have been included for the solvate water molecules. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0745P)^2^+6.7671P] 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 'riding on preceding C atom' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17063 _refine_ls_number_parameters 1378 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2095 _refine_ls_R_factor_obs 0.0882 _refine_ls_wR_factor_all 0.2367 _refine_ls_wR_factor_obs 0.1707 _refine_ls_goodness_of_fit_all 1.031 _refine_ls_goodness_of_fit_obs 1.190 _refine_ls_restrained_S_all 1.032 _refine_ls_restrained_S_obs 1.190 _refine_ls_shift/esd_max 0.059 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.75925(9) 0.85979(8) 0.40389(4) 0.0425(3) Uani 1 d . . Cu2 Cu 0.75185(9) 0.52500(8) 0.39228(4) 0.0455(3) Uani 1 d . . N1 N 0.9199(5) 0.8923(5) 0.4136(2) 0.038(2) Uani 1 d . . N12 N 0.7683(6) 1.0245(6) 0.4292(3) 0.046(2) Uani 1 d . . N21 N 0.5987(6) 0.8523(6) 0.3920(3) 0.049(2) Uani 1 d . . N32 N 0.7593(6) 0.8874(5) 0.3380(3) 0.045(2) Uani 1 d . . N41 N 0.5943(6) 0.5507(5) 0.3795(3) 0.044(2) Uani 1 d . . N52 N 0.7580(6) 0.5823(5) 0.3219(3) 0.047(2) Uani 1 d . . N61 N 0.7383(6) 0.3756(6) 0.3695(3) 0.048(2) Uani 1 d . . N72 N 0.9019(6) 0.4864(6) 0.4073(3) 0.047(2) Uani 1 d . . O11 O 0.7393(5) 0.7893(5) 0.4603(2) 0.049(2) Uani 1 d . . O12 O 0.7801(5) 0.6645(5) 0.4156(2) 0.054(2) Uani 1 d . . O13 O 0.7122(7) 0.6236(6) 0.4817(3) 0.088(3) Uani 1 d . . C2 C 0.9936(7) 0.8266(7) 0.4055(3) 0.041(2) Uani 1 d . . H2 H 0.9720(7) 0.7619(7) 0.3928(3) 0.062 Uiso 1 calc R . C3 C 1.1018(7) 0.8519(8) 0.4154(3) 0.054(3) Uani 1 d . . H3 H 1.1518(7) 0.8053(8) 0.4083(3) 0.081 Uiso 1 calc R . C4 C 1.1356(8) 0.9447(8) 0.4356(3) 0.054(3) Uani 1 d . . H4 H 1.2078(8) 0.9607(8) 0.4433(3) 0.082 Uiso 1 calc R . C5 C 1.0597(7) 1.0146(7) 0.4442(3) 0.044(2) Uani 1 d . . C6 C 1.0877(8) 1.1125(8) 0.4660(3) 0.055(3) Uani 1 d . . H6 H 1.1587(8) 1.1302(8) 0.4750(3) 0.082 Uiso 1 calc R . C7 C 1.0122(8) 1.1798(7) 0.4736(3) 0.053(3) Uani 1 d . . H7 H 1.0328(8) 1.2446(7) 0.4864(3) 0.080 Uiso 1 calc R . C8 C 0.9013(7) 1.1525(6) 0.4623(3) 0.042(2) Uani 1 d . . C9 C 0.8185(9) 1.2181(7) 0.4691(3) 0.060(3) Uani 1 d . . H9 H 0.8343(9) 1.2838(7) 0.4819(3) 0.091 Uiso 1 calc R . C10 C 0.7152(9) 1.1852(8) 0.4570(4) 0.066(3) Uani 1 d . . H10 H 0.6600(9) 1.2275(8) 0.4623(4) 0.099 Uiso 1 calc R . C11 C 0.6926(8) 1.0880(8) 0.4368(3) 0.058(3) Uani 1 d . . H11 H 0.6219(8) 1.0669(8) 0.4283(3) 0.087 Uiso 1 calc R . C13 C 0.8704(7) 1.0561(6) 0.4412(3) 0.040(2) Uani 1 d . . C14 C 0.9520(7) 0.9851(6) 0.4328(3) 0.038(2) Uani 1 d . . C15 C 0.7439(8) 0.6895(7) 0.4541(3) 0.048(2) Uani 1 d . . C22 C 0.5205(9) 0.8369(8) 0.4204(4) 0.068(3) Uani 1 d . . H22 H 0.5372(9) 0.8153(8) 0.4489(4) 0.102 Uiso 1 calc R . C23 C 0.4147(9) 0.8522(9) 0.4089(5) 0.081(4) Uani 1 d . . H23 H 0.3615(9) 0.8381(9) 0.4293(5) 0.121 Uiso 1 calc R . C24 C 0.3875(9) 0.8878(9) 0.3678(5) 0.084(4) Uani 1 d . . H24 H 0.3171(9) 0.9012(9) 0.3605(5) 0.126 Uiso 1 calc R . C25 C 0.4671(8) 0.9032(8) 0.3378(4) 0.063(3) Uani 1 d . . C26 C 0.4483(10) 0.9375(8) 0.2935(4) 0.081(4) Uani 1 d . . H26 H 0.3792(10) 0.9514(8) 0.2843(4) 0.122 Uiso 1 calc R . C27 C 0.5266(10) 0.9496(8) 0.2657(4) 0.074(4) Uani 1 d . . H27 H 0.5109(10) 0.9698(8) 0.2370(4) 0.111 Uiso 1 calc R . C28 C 0.6368(9) 0.9327(7) 0.2782(3) 0.059(3) Uani 1 d . . C29 C 0.7258(11) 0.9460(8) 0.2510(4) 0.073(4) Uani 1 d . . H29 H 0.7167(11) 0.9665(8) 0.2219(4) 0.110 Uiso 1 calc R . C30 C 0.8262(10) 0.9285(9) 0.2678(4) 0.077(4) Uani 1 d . . H30 H 0.8851(10) 0.9355(9) 0.2498(4) 0.115 Uiso 1 calc R . C31 C 0.8394(9) 0.9006(8) 0.3113(4) 0.062(3) Uani 1 d . . H31 H 0.9083(9) 0.8907(8) 0.3221(4) 0.094 Uiso 1 calc R . C33 C 0.6582(8) 0.9027(7) 0.3214(3) 0.052(3) Uani 1 d . . C34 C 0.5718(8) 0.8868(7) 0.3509(4) 0.052(3) Uani 1 d . . C42 C 0.5156(8) 0.5345(7) 0.4071(4) 0.054(3) Uani 1 d . . H42 H 0.5303(8) 0.5048(7) 0.4344(4) 0.081 Uiso 1 calc R . C43 C 0.4113(8) 0.5600(8) 0.3972(4) 0.066(3) Uani 1 d . . H43 H 0.3575(8) 0.5480(8) 0.4175(4) 0.099 Uiso 1 calc R . C44 C 0.3896(8) 0.6027(8) 0.3574(4) 0.067(3) Uani 1 d . . H44 H 0.3201(8) 0.6198(8) 0.3503(4) 0.101 Uiso 1 calc R . C45 C 0.4703(7) 0.6213(7) 0.3269(3) 0.047(2) Uani 1 d . . C46 C 0.4529(10) 0.6678(8) 0.2847(4) 0.069(3) Uani 1 d . . H46 H 0.3857(10) 0.6897(8) 0.2770(4) 0.104 Uiso 1 calc R . C47 C 0.5334(10) 0.6801(7) 0.2562(4) 0.067(3) Uani 1 d . . H47 H 0.5198(10) 0.7085(7) 0.2286(4) 0.100 Uiso 1 calc R . C48 C 0.6390(9) 0.6509(7) 0.2671(3) 0.056(3) Uani 1 d . . C49 C 0.7272(11) 0.6631(8) 0.2376(4) 0.078(4) Uani 1 d . . H49 H 0.7179(11) 0.6904(8) 0.2095(4) 0.117 Uiso 1 calc R . C50 C 0.8225(10) 0.6342(9) 0.2518(4) 0.076(4) Uani 1 d . . H50 H 0.8804(10) 0.6403(9) 0.2332(4) 0.114 Uiso 1 calc R . C51 C 0.8356(9) 0.5953(8) 0.2939(4) 0.066(3) Uani 1 d . . H51 H 0.9035(9) 0.5773(8) 0.3028(4) 0.098 Uiso 1 calc R . C53 C 0.6584(8) 0.6086(7) 0.3084(3) 0.050(3) Uani 1 d . . C54 C 0.5729(8) 0.5934(7) 0.3395(3) 0.046(2) Uani 1 d . . C62 C 0.6538(8) 0.3189(7) 0.3510(3) 0.054(3) Uani 1 d . . H62 H 0.5863(8) 0.3443(7) 0.3521(3) 0.081 Uiso 1 calc R . C63 C 0.6624(9) 0.2238(8) 0.3300(4) 0.066(3) Uani 1 d . . H63 H 0.6017(9) 0.1872(8) 0.3174(4) 0.099 Uiso 1 calc R . C64 C 0.7598(8) 0.1845(7) 0.3281(3) 0.054(3) Uani 1 d . . H64 H 0.7658(8) 0.1207(7) 0.3142(3) 0.081 Uiso 1 calc R . C65 C 0.8504(9) 0.2397(7) 0.3470(3) 0.053(3) Uani 1 d . . C66 C 0.9555(8) 0.2057(7) 0.3486(3) 0.056(3) Uani 1 d . . H66 H 0.9672(8) 0.1440(7) 0.3341(3) 0.083 Uiso 1 calc R . C67 C 1.0391(8) 0.2582(8) 0.3700(4) 0.060(3) Uani 1 d . . H67 H 1.1057(8) 0.2306(8) 0.3712(4) 0.090 Uiso 1 calc R . C68 C 1.0265(7) 0.3578(7) 0.3913(3) 0.051(3) Uani 1 d . . C69 C 1.1068(8) 0.4163(8) 0.4165(4) 0.065(3) Uani 1 d . . H69 H 1.1751(8) 0.3930(8) 0.4201(4) 0.097 Uiso 1 calc R . C70 C 1.0837(8) 0.5066(8) 0.4353(4) 0.069(3) Uani 1 d . . H70 H 1.1365(8) 0.5462(8) 0.4518(4) 0.103 Uiso 1 calc R . C71 C 0.9797(8) 0.5412(8) 0.4300(3) 0.058(3) Uani 1 d . . H71 H 0.9654(8) 0.6042(8) 0.4428(3) 0.088 Uiso 1 calc R . C73 C 0.9243(7) 0.3956(6) 0.3894(3) 0.039(2) Uani 1 d . . C74 C 0.8344(7) 0.3362(6) 0.3675(3) 0.042(2) Uani 1 d . . Cu3 Cu 0.15854(12) 0.18565(12) 0.08052(5) 0.0748(5) Uani 1 d . . Cu4 Cu 0.17402(11) 0.51724(11) 0.13476(5) 0.0637(4) Uani 1 d . . N81 N 0.0027(7) 0.1464(8) 0.0678(3) 0.072(3) Uani 1 d . . N92 N 0.1638(8) 0.0231(8) 0.0672(3) 0.070(3) Uani 1 d . . N101 N 0.3175(7) 0.2010(7) 0.0923(3) 0.071(3) Uani 1 d . . N112 N 0.1638(8) 0.1721(6) 0.1513(3) 0.066(3) Uani 1 d . . N121 N 0.1737(7) 0.4644(6) 0.2024(3) 0.061(2) Uani 1 d . . N132 N 0.3317(7) 0.4930(7) 0.1443(3) 0.065(3) Uani 1 d . . N141 N 0.1978(6) 0.6779(6) 0.1532(3) 0.055(2) Uani 1 d . . N152 N 0.0222(6) 0.5578(7) 0.1289(3) 0.062(2) Uani 1 d . . O21 O 0.1395(7) 0.3674(10) 0.1003(3) 0.140(5) Uani 1 d . . O22 O 0.1767(9) 0.3285(9) 0.0349(4) 0.147(5) Uani 1 d . . O23 O 0.1839(7) 0.4892(7) 0.0556(4) 0.113(4) Uani 1 d . . C82 C -0.0731(11) 0.2109(12) 0.0693(5) 0.101(5) Uani 1 d . . H82 H -0.0550(11) 0.2814(12) 0.0753(5) 0.152 Uiso 1 calc R . C83 C -0.1823(11) 0.1742(12) 0.0620(5) 0.103(5) Uani 1 d . . H83 H -0.2358(11) 0.2203(12) 0.0627(5) 0.154 Uiso 1 calc R . C84 C -0.2087(11) 0.0691(12) 0.0537(4) 0.096(5) Uani 1 d . . H84 H -0.2804(11) 0.0441(12) 0.0495(4) 0.145 Uiso 1 calc R . C85 C -0.1278(10) 0.0001(11) 0.0515(4) 0.076(4) Uani 1 d . . C86 C -0.1473(11) -0.1106(11) 0.0420(3) 0.085(4) Uani 1 d . . H86 H -0.2174(11) -0.1400(11) 0.0372(3) 0.127 Uiso 1 calc R . C87 C -0.0646(11) -0.1712(11) 0.0402(4) 0.091(4) Uani 1 d . . H87 H -0.0790(11) -0.2411(11) 0.0322(4) 0.137 Uiso 1 calc R . C88 C 0.0431(11) -0.1333(9) 0.0497(3) 0.071(3) Uani 1 d . . C89 C 0.1344(12) -0.1886(10) 0.0496(4) 0.089(4) Uani 1 d . . H89 H 0.1270(12) -0.2595(10) 0.0427(4) 0.133 Uiso 1 calc R . C90 C 0.2329(11) -0.1422(11) 0.0592(4) 0.091(4) Uani 1 d . . H90 H 0.2924(11) -0.1813(11) 0.0601(4) 0.136 Uiso 1 calc R . C91 C 0.2456(10) -0.0357(10) 0.0679(4) 0.081(4) Uani 1 d . . H91 H 0.3142(10) -0.0046(10) 0.0745(4) 0.121 Uiso 1 calc R . C93 C 0.0639(10) -0.0225(10) 0.0587(3) 0.069(3) Uani 1 d . . C94 C -0.0223(9) 0.0437(10) 0.0599(3) 0.066(3) Uani 1 d . . C95 C 0.1678(9) 0.3950(11) 0.0623(4) 0.075(4) Uani 1 d . . C102 C 0.3918(11) 0.2158(11) 0.0631(4) 0.094(4) Uani 1 d . . H102 H 0.3713(11) 0.2276(11) 0.0340(4) 0.141 Uiso 1 calc R . C103 C 0.5039(10) 0.2145(11) 0.0747(5) 0.106(5) Uani 1 d . . H103 H 0.5550(10) 0.2242(11) 0.0532(5) 0.159 Uiso 1 calc R . C104 C 0.5348(12) 0.1989(11) 0.1173(5) 0.107(5) Uani 1 d . . H104 H 0.6074(12) 0.1978(11) 0.1251(5) 0.161 Uiso 1 calc R . C105 C 0.4570(10) 0.1844(8) 0.1496(5) 0.079(4) Uani 1 d . . C106 C 0.4834(11) 0.1685(9) 0.1942(5) 0.085(4) Uani 1 d . . H106 H 0.5548(11) 0.1636(9) 0.2031(5) 0.127 Uiso 1 calc R . C107 C 0.4085(11) 0.1606(8) 0.2234(4) 0.078(4) Uani 1 d . . H107 H 0.4285(11) 0.1544(8) 0.2530(4) 0.118 Uiso 1 calc R . C108 C 0.2971(10) 0.1610(8) 0.2114(4) 0.067(3) Uani 1 d . . C109 C 0.2137(12) 0.1545(9) 0.2399(4) 0.083(4) Uani 1 d . . H109 H 0.2294(12) 0.1492(9) 0.2699(4) 0.125 Uiso 1 calc R . C110 C 0.1094(12) 0.1555(9) 0.2261(4) 0.089(4) Uani 1 d . . H110 H 0.0543(12) 0.1509(9) 0.2460(4) 0.133 Uiso 1 calc R . C111 C 0.0878(10) 0.1638(8) 0.1810(4) 0.078(4) Uani 1 d . . H111 H 0.0164(10) 0.1634(8) 0.1712(4) 0.116 Uiso 1 calc R . C113 C 0.2676(9) 0.1725(8) 0.1670(4) 0.061(3) Uani 1 d . . C114 C 0.3490(9) 0.1851(8) 0.1349(4) 0.062(3) Uani 1 d . . C122 C 0.0962(9) 0.4490(9) 0.2307(4) 0.075(4) Uani 1 d . . H122 H 0.0260(9) 0.4582(9) 0.2213(4) 0.112 Uiso 1 calc R . C123 C 0.1158(11) 0.4194(9) 0.2742(4) 0.081(4) Uani 1 d . . H123 H 0.0598(11) 0.4102(9) 0.2936(4) 0.122 Uiso 1 calc R . C124 C 0.2145(11) 0.4047(8) 0.2872(4) 0.080(4) Uani 1 d . . H124 H 0.2265(11) 0.3841(8) 0.3162(4) 0.120 Uiso 1 calc R . C125 C 0.3016(9) 0.4181(7) 0.2605(4) 0.061(3) Uani 1 d . . C126 C 0.4124(11) 0.4020(8) 0.2714(4) 0.075(4) Uani 1 d . . H126 H 0.4308(11) 0.3832(8) 0.3000(4) 0.112 Uiso 1 calc R . C127 C 0.4894(10) 0.4129(8) 0.2419(4) 0.070(3) Uani 1 d . . H127 H 0.5596(10) 0.4002(8) 0.2500(4) 0.105 Uiso 1 calc R . C128 C 0.4641(8) 0.4440(8) 0.1983(4) 0.060(3) Uani 1 d . . C129 C 0.5423(9) 0.4597(9) 0.1663(4) 0.076(4) Uani 1 d . . H129 H 0.6136(9) 0.4504(9) 0.1739(4) 0.114 Uiso 1 calc R . C130 C 0.5156(9) 0.4883(10) 0.1245(4) 0.089(4) Uani 1 d . . H130 H 0.5673(9) 0.4971(10) 0.1032(4) 0.133 Uiso 1 calc R . C131 C 0.4067(10) 0.5042(10) 0.1145(4) 0.081(4) Uani 1 d . . H131 H 0.3871(10) 0.5232(10) 0.0860(4) 0.121 Uiso 1 calc R . C133 C 0.3604(8) 0.4621(7) 0.1851(3) 0.056(3) Uani 1 d . . C134 C 0.2765(9) 0.4483(7) 0.2164(4) 0.056(3) Uani 1 d . . C142 C 0.2873(10) 0.7346(9) 0.1657(4) 0.078(4) Uani 1 d . . H142 H 0.3531(10) 0.7057(9) 0.1651(4) 0.118 Uiso 1 calc R . C143 C 0.2828(10) 0.8393(10) 0.1801(4) 0.085(4) Uani 1 d . . H143 H 0.3458(10) 0.8779(10) 0.1895(4) 0.127 Uiso 1 calc R . C144 C 0.1897(10) 0.8836(9) 0.1804(4) 0.082(4) Uani 1 d . . H144 H 0.1881(10) 0.9524(9) 0.1898(4) 0.124 Uiso 1 calc R . C145 C 0.0954(9) 0.8264(8) 0.1666(3) 0.060(3) Uani 1 d . . C146 C -0.0094(10) 0.8661(9) 0.1652(4) 0.073(3) Uani 1 d . . H146 H -0.0166(10) 0.9342(9) 0.1745(4) 0.110 Uiso 1 calc R . C147 C -0.0964(10) 0.8063(9) 0.1508(3) 0.069(3) Uani 1 d . . H147 H -0.1623(10) 0.8352(9) 0.1491(3) 0.103 Uiso 1 calc R . C148 C -0.0918(9) 0.6995(9) 0.1379(3) 0.064(3) Uani 1 d . . C149 C -0.1776(9) 0.6366(10) 0.1225(4) 0.075(4) Uani 1 d . . H149 H -0.2445(9) 0.6630(10) 0.1191(4) 0.113 Uiso 1 calc R . C150 C -0.1661(10) 0.5339(12) 0.1119(5) 0.101(5) Uani 1 d . . H150 H -0.2247(10) 0.4894(12) 0.1022(5) 0.152 Uiso 1 calc R . C151 C -0.0614(10) 0.4978(10) 0.1162(4) 0.086(4) Uani 1 d . . H151 H -0.0528(10) 0.4283(10) 0.1097(4) 0.130 Uiso 1 calc R . C153 C 0.0087(8) 0.6579(8) 0.1401(3) 0.056(3) Uani 1 d . . C154 C 0.1022(8) 0.7227(8) 0.1540(3) 0.052(3) Uani 1 d . . Cl3 Cl 0.1245(2) 0.7384(3) 0.29398(11) 0.0741(9) Uani 1 d . . O31 O 0.1070(10) 0.6769(10) 0.3322(3) 0.150(5) Uani 1 d . . O32 O 0.1356(16) 0.6791(9) 0.2587(4) 0.232(9) Uani 1 d . . O33 O 0.0473(11) 0.7949(13) 0.2873(5) 0.242(9) Uani 1 d . . O34 O 0.2164(9) 0.7942(13) 0.2997(6) 0.226(8) Uani 1 d . . Cl4 Cl 0.3650(2) 1.1885(2) 0.37808(9) 0.0584(7) Uani 1 d . . O41 O 0.4484(8) 1.1630(8) 0.4064(3) 0.127(4) Uani 1 d . . O42 O 0.3467(10) 1.2941(7) 0.3832(4) 0.146(5) Uani 1 d . . O43 O 0.2709(8) 1.1261(9) 0.3848(5) 0.161(5) Uani 1 d . . O44 O 0.3944(9) 1.1744(9) 0.3352(3) 0.136(4) Uani 1 d . . Cl5 Cl 0.5696(3) 0.8698(3) 0.12330(14) 0.1010(12) Uani 1 d . . O51 O 0.5644(17) 0.7865(15) 0.1466(8) 0.330(14) Uani 1 d . . O52 O 0.4939(15) 0.8795(18) 0.0960(7) 0.319(13) Uani 1 d . . O53 O 0.6485(15) 0.8696(22) 0.1033(10) 0.427(23) Uani 1 d . . O54 O 0.5663(34) 0.9451(17) 0.1462(8) 0.499(30) Uani 1 d . . Cl6 Cl 0.8064(3) 0.2850(3) 0.20993(15) 0.1049(13) Uani 1 d . . O61 O 0.7691(23) 0.1930(16) 0.2177(7) 0.358(17) Uani 1 d . . O62 O 0.8290(19) 0.3027(14) 0.1684(5) 0.291(12) Uani 1 d . . O63 O 0.7368(17) 0.3379(20) 0.2244(8) 0.352(16) Uani 1 d . . O64 O 0.8898(11) 0.2868(20) 0.2339(7) 0.313(13) Uani 1 d . . O1 O 0.5224(6) 0.6685(6) 0.5179(3) 0.084(3) Uani 1 d . . O2 O 0.6943(7) 0.4180(6) 0.4962(3) 0.108(3) Uani 1 d . . O3 O 0.4857(10) 0.6837(12) 0.0309(4) 0.188(6) Uani 1 d . . O4 O 0.1074(12) 1.0185(11) 0.3240(5) 0.197(6) Uani 1 d . . O5 O 0.3363(11) 0.4159(15) -0.0233(4) 0.227(8) Uani 1 d . . O6 O 0.6236(14) 0.9451(13) 0.5138(5) 0.233(8) Uani 1 d . . O7 O 0.3020(13) 0.6120(12) -0.0116(6) 0.236(8) Uani 1 d . . O8 O 0.0476(24) 0.5881(16) 0.0019(8) 0.389(16) Uani 1 d . . O9 O 0.8286(33) 0.0601(35) 0.1599(11) 0.290(20) Uani 0.50 d P . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0373(6) 0.0358(6) 0.0546(8) -0.0028(5) 0.0028(6) 0.0028(5) Cu2 0.0405(7) 0.0324(6) 0.0636(9) -0.0048(6) -0.0054(6) 0.0060(5) N1 0.029(4) 0.036(4) 0.048(5) 0.000(3) 0.002(3) 0.005(3) N12 0.040(5) 0.038(4) 0.060(6) -0.004(4) 0.008(4) 0.005(4) N21 0.046(5) 0.041(5) 0.060(6) -0.008(4) 0.007(4) 0.004(4) N32 0.044(5) 0.040(5) 0.051(5) -0.003(4) 0.000(4) 0.009(4) N41 0.043(5) 0.039(4) 0.052(5) -0.002(4) 0.008(4) 0.008(4) N52 0.046(5) 0.036(4) 0.057(6) 0.002(4) 0.003(4) -0.001(4) N61 0.045(5) 0.041(5) 0.058(6) -0.001(4) 0.000(4) 0.012(4) N72 0.041(5) 0.039(5) 0.062(6) -0.005(4) -0.004(4) 0.002(4) O11 0.046(4) 0.044(4) 0.055(4) -0.007(3) 0.003(3) -0.005(3) O12 0.047(4) 0.043(4) 0.072(5) -0.013(3) 0.002(4) 0.001(3) O13 0.102(7) 0.058(5) 0.104(7) 0.025(5) 0.009(5) -0.005(5) C2 0.042(5) 0.037(5) 0.046(6) -0.003(4) 0.005(4) 0.007(4) C3 0.039(6) 0.052(6) 0.074(8) 0.001(5) 0.011(5) 0.016(5) C4 0.037(5) 0.072(7) 0.054(7) 0.002(6) 0.005(5) 0.002(5) C5 0.049(6) 0.047(6) 0.035(6) 0.006(4) -0.001(5) -0.003(5) C6 0.060(7) 0.059(7) 0.040(6) 0.007(5) -0.009(5) -0.016(6) C7 0.070(7) 0.036(5) 0.050(7) -0.001(5) 0.010(6) -0.014(5) C8 0.052(6) 0.028(5) 0.044(6) 0.005(4) 0.008(5) -0.006(4) C9 0.092(9) 0.030(5) 0.060(7) -0.005(5) 0.018(6) 0.002(6) C10 0.077(8) 0.046(7) 0.077(9) -0.003(6) 0.021(7) 0.016(6) C11 0.047(6) 0.058(7) 0.072(8) -0.003(6) -0.001(5) 0.020(5) C13 0.050(6) 0.032(5) 0.039(6) 0.007(4) 0.008(5) -0.002(4) C14 0.043(5) 0.035(5) 0.036(5) 0.000(4) 0.007(4) 0.001(4) C15 0.051(6) 0.040(6) 0.051(7) 0.003(5) -0.008(5) 0.003(5) C22 0.064(8) 0.058(7) 0.082(9) -0.008(6) 0.017(7) -0.001(6) C23 0.041(7) 0.071(8) 0.132(13) 0.012(8) 0.023(8) 0.005(6) C24 0.038(7) 0.064(8) 0.152(14) 0.003(8) -0.001(8) 0.008(6) C25 0.046(7) 0.044(6) 0.096(10) 0.001(6) -0.009(7) 0.002(5) C26 0.070(9) 0.053(7) 0.118(13) 0.001(8) -0.033(9) 0.007(7) C27 0.079(9) 0.049(7) 0.090(10) 0.017(6) -0.037(8) 0.003(7) C28 0.088(9) 0.038(6) 0.051(7) -0.002(5) -0.009(7) 0.006(6) C29 0.127(12) 0.053(7) 0.041(7) 0.003(5) 0.006(8) 0.010(7) C30 0.086(10) 0.073(8) 0.074(10) -0.010(7) 0.013(8) 0.014(7) C31 0.074(8) 0.056(7) 0.056(8) -0.003(6) 0.002(7) 0.003(6) C33 0.052(6) 0.030(5) 0.072(8) -0.004(5) -0.008(6) -0.001(5) C34 0.042(6) 0.033(5) 0.082(8) -0.002(5) 0.004(6) -0.002(4) C42 0.054(7) 0.042(6) 0.067(8) -0.005(5) -0.007(6) 0.007(5) C43 0.051(7) 0.070(8) 0.077(9) -0.005(7) 0.016(6) 0.006(6) C44 0.045(6) 0.051(7) 0.107(11) -0.017(7) -0.005(7) 0.018(5) C45 0.040(6) 0.038(5) 0.064(7) -0.011(5) -0.009(5) 0.010(4) C46 0.079(9) 0.051(7) 0.080(9) 0.006(6) -0.018(7) 0.020(6) C47 0.096(10) 0.037(6) 0.066(8) 0.002(5) -0.026(7) 0.006(6) C48 0.085(8) 0.029(5) 0.053(7) 0.004(5) -0.016(6) -0.001(5) C49 0.106(11) 0.060(8) 0.064(9) 0.016(6) 0.011(8) -0.019(7) C50 0.077(9) 0.087(9) 0.065(9) 0.013(7) 0.023(7) 0.009(7) C51 0.063(8) 0.059(7) 0.075(9) 0.002(6) 0.021(7) 0.003(6) C53 0.057(7) 0.029(5) 0.064(7) -0.010(5) -0.005(6) 0.004(5) C54 0.053(6) 0.031(5) 0.054(7) -0.009(5) -0.003(5) -0.001(4) C62 0.043(6) 0.046(6) 0.072(8) -0.004(5) -0.002(5) 0.002(5) C63 0.066(8) 0.056(7) 0.074(8) -0.007(6) -0.020(6) -0.004(6) C64 0.058(7) 0.035(5) 0.067(8) -0.014(5) 0.004(6) -0.004(5) C65 0.073(7) 0.036(5) 0.051(7) 0.008(5) 0.017(6) 0.007(5) C66 0.070(7) 0.040(6) 0.060(7) -0.003(5) 0.023(6) 0.017(5) C67 0.055(7) 0.051(7) 0.078(8) 0.017(6) 0.020(6) 0.020(5) C68 0.043(6) 0.046(6) 0.063(7) 0.019(5) 0.008(5) 0.002(5) C69 0.039(6) 0.052(7) 0.102(10) 0.014(6) -0.003(6) 0.006(5) C70 0.047(7) 0.052(7) 0.104(10) 0.002(6) -0.025(6) -0.009(5) C71 0.052(6) 0.055(7) 0.068(8) -0.008(5) -0.014(6) 0.005(5) C73 0.041(5) 0.035(5) 0.041(6) 0.013(4) 0.003(4) 0.006(4) C74 0.047(6) 0.031(5) 0.049(6) 0.002(4) 0.003(5) 0.010(4) Cu3 0.0696(10) 0.0892(11) 0.0677(10) 0.0058(8) -0.0046(8) 0.0227(8) Cu4 0.0553(8) 0.0646(9) 0.0701(10) 0.0129(7) 0.0008(7) -0.0005(7) N81 0.068(7) 0.093(8) 0.058(7) -0.003(6) 0.012(5) 0.020(6) N92 0.073(7) 0.095(8) 0.047(6) -0.010(5) -0.006(5) 0.037(6) N101 0.062(6) 0.091(8) 0.064(7) 0.021(6) 0.015(5) 0.019(5) N112 0.080(7) 0.052(6) 0.068(7) -0.008(5) 0.010(6) 0.015(5) N121 0.062(6) 0.051(5) 0.071(7) 0.009(5) 0.017(5) 0.006(4) N132 0.052(6) 0.078(7) 0.068(7) 0.017(5) 0.012(5) 0.010(5) N141 0.051(5) 0.061(6) 0.050(6) 0.002(4) -0.006(4) -0.007(5) N152 0.046(5) 0.059(6) 0.080(7) -0.012(5) -0.001(5) -0.005(4) O21 0.067(6) 0.249(14) 0.110(9) 0.105(9) 0.024(6) 0.040(7) O22 0.121(9) 0.162(11) 0.159(12) -0.086(10) -0.039(8) 0.041(8) O23 0.080(7) 0.068(6) 0.189(12) 0.017(7) 0.004(7) 0.006(5) C82 0.083(11) 0.110(12) 0.116(13) -0.010(9) 0.005(9) 0.036(9) C83 0.087(11) 0.128(14) 0.101(12) 0.008(10) 0.020(9) 0.043(10) C84 0.077(10) 0.136(14) 0.078(10) 0.007(10) 0.022(8) 0.011(10) C85 0.071(9) 0.111(11) 0.046(8) 0.005(7) 0.001(6) 0.004(8) C86 0.101(11) 0.108(12) 0.041(7) 0.007(7) -0.003(7) -0.014(9) C87 0.098(11) 0.110(12) 0.067(10) 0.013(8) 0.002(8) 0.015(10) C88 0.101(11) 0.077(9) 0.036(7) -0.002(6) 0.008(7) 0.010(8) C89 0.122(13) 0.085(10) 0.062(9) -0.014(7) 0.013(9) 0.018(10) C90 0.096(11) 0.103(12) 0.078(10) -0.009(8) 0.015(8) 0.027(9) C91 0.086(10) 0.092(10) 0.066(9) -0.001(7) 0.006(7) 0.026(8) C93 0.082(9) 0.098(10) 0.029(6) 0.002(6) 0.008(6) 0.020(8) C94 0.061(8) 0.100(10) 0.039(7) 0.007(6) 0.005(6) 0.018(7) C95 0.046(7) 0.120(12) 0.057(9) 0.025(8) -0.014(6) 0.003(8) C102 0.092(11) 0.114(12) 0.078(10) 0.017(8) 0.004(9) 0.018(9) C103 0.060(9) 0.119(13) 0.140(15) 0.040(11) 0.026(9) 0.009(8) C104 0.079(11) 0.104(12) 0.140(16) 0.030(11) -0.005(11) 0.021(9) C105 0.078(9) 0.050(7) 0.106(12) -0.004(7) -0.022(9) 0.002(6) C106 0.084(10) 0.059(8) 0.110(13) -0.004(8) -0.029(9) 0.009(7) C107 0.097(11) 0.053(7) 0.083(10) -0.007(7) -0.026(9) -0.001(7) C108 0.107(11) 0.039(6) 0.057(8) -0.011(5) 0.009(8) 0.013(6) C109 0.123(13) 0.058(8) 0.068(9) -0.006(6) -0.023(9) 0.010(8) C110 0.131(14) 0.065(8) 0.074(10) -0.010(7) 0.030(10) 0.014(9) C111 0.076(9) 0.061(8) 0.097(11) -0.008(7) 0.017(8) 0.014(6) C113 0.081(9) 0.045(6) 0.059(8) 0.003(5) -0.012(7) 0.014(6) C114 0.077(8) 0.055(7) 0.056(8) 0.001(6) -0.015(7) 0.018(6) C122 0.063(8) 0.070(8) 0.092(10) 0.005(7) 0.025(7) 0.003(6) C123 0.103(11) 0.064(8) 0.078(10) 0.008(7) 0.040(9) 0.002(8) C124 0.111(12) 0.052(7) 0.078(10) 0.010(6) 0.026(9) -0.003(8) C125 0.078(8) 0.031(6) 0.075(9) -0.001(5) 0.005(7) -0.001(5) C126 0.117(12) 0.046(7) 0.061(8) 0.002(6) -0.014(8) 0.011(7) C127 0.086(9) 0.057(7) 0.069(9) -0.002(6) -0.010(7) 0.023(7) C128 0.053(7) 0.050(6) 0.077(9) -0.009(6) -0.005(6) 0.007(5) C129 0.053(7) 0.082(9) 0.096(11) 0.003(7) -0.005(7) 0.029(6) C130 0.047(7) 0.121(12) 0.098(11) 0.027(9) 0.008(7) 0.004(7) C131 0.072(9) 0.106(11) 0.064(9) 0.019(7) 0.001(7) 0.006(8) C133 0.059(7) 0.047(6) 0.061(8) 0.004(5) 0.000(6) 0.000(5) C134 0.068(7) 0.035(6) 0.065(8) -0.002(5) 0.003(6) 0.011(5) C142 0.075(9) 0.076(9) 0.082(10) 0.003(7) 0.002(7) -0.007(7) C143 0.080(10) 0.076(9) 0.095(11) -0.011(8) -0.007(8) -0.012(8) C144 0.094(10) 0.061(8) 0.090(10) -0.013(7) 0.004(8) -0.002(8) C145 0.080(8) 0.055(7) 0.040(6) 0.008(5) 0.000(6) -0.014(6) C146 0.085(9) 0.060(8) 0.078(9) -0.008(6) 0.007(7) 0.021(7) C147 0.075(8) 0.078(9) 0.056(8) 0.006(6) 0.012(6) 0.023(7) C148 0.063(8) 0.079(8) 0.053(7) 0.000(6) 0.005(6) 0.010(7) C149 0.054(7) 0.099(10) 0.074(9) -0.007(8) 0.007(6) 0.009(7) C150 0.049(8) 0.123(13) 0.130(14) -0.011(10) -0.007(8) -0.005(8) C151 0.067(9) 0.084(9) 0.107(11) -0.021(8) 0.008(8) -0.008(7) C153 0.059(7) 0.059(7) 0.048(7) -0.003(5) 0.005(5) -0.005(6) C154 0.066(7) 0.055(7) 0.036(6) 0.009(5) 0.009(5) 0.006(6) Cl3 0.052(2) 0.087(2) 0.084(2) -0.020(2) 0.004(2) 0.012(2) O31 0.201(13) 0.172(12) 0.078(8) 0.010(8) 0.037(8) 0.010(10) O32 0.502(29) 0.093(9) 0.104(10) -0.030(7) 0.104(14) -0.003(13) O33 0.174(14) 0.308(21) 0.275(19) 0.104(16) 0.067(13) 0.186(15) O34 0.086(9) 0.277(19) 0.297(20) 0.004(15) -0.032(11) -0.087(11) Cl4 0.053(2) 0.062(2) 0.062(2) 0.0043(14) 0.0039(14) 0.0096(13) O41 0.109(8) 0.145(10) 0.129(9) 0.033(7) -0.036(7) 0.046(7) O42 0.218(13) 0.069(7) 0.154(10) -0.022(6) -0.024(9) 0.057(8) O43 0.063(7) 0.127(9) 0.293(16) 0.067(10) 0.028(8) -0.014(6) O44 0.168(11) 0.165(11) 0.078(7) -0.014(7) 0.043(7) 0.012(8) Cl5 0.079(3) 0.118(3) 0.109(3) 0.007(3) 0.011(2) 0.028(2) O51 0.291(25) 0.238(22) 0.462(34) 0.232(23) 0.025(23) 0.015(18) O52 0.216(21) 0.448(36) 0.284(25) 0.053(23) -0.158(19) 0.044(20) O53 0.199(20) 0.522(45) 0.600(49) 0.296(40) 0.281(28) 0.152(25) O54 1.062(95) 0.199(22) 0.249(27) -0.099(20) -0.123(40) 0.188(37) Cl6 0.056(2) 0.120(3) 0.138(4) 0.038(3) 0.001(2) 0.005(2) O61 0.538(47) 0.193(20) 0.311(28) 0.018(19) 0.052(28) -0.164(27) O62 0.506(35) 0.253(20) 0.128(13) 0.098(13) 0.120(18) 0.064(20) O63 0.272(25) 0.417(38) 0.410(35) 0.074(27) 0.100(23) 0.243(27) O64 0.088(11) 0.527(40) 0.310(26) 0.049(24) -0.064(14) -0.025(17) O1 0.081(6) 0.081(6) 0.086(6) -0.005(5) 0.009(5) -0.023(5) O2 0.078(6) 0.054(5) 0.192(10) -0.047(6) -0.026(6) 0.023(4) O3 0.156(13) 0.259(17) 0.144(12) 0.010(11) 0.021(9) -0.021(11) O4 0.187(14) 0.158(13) 0.251(17) 0.017(11) 0.027(12) 0.026(11) O5 0.174(14) 0.394(25) 0.130(12) 0.033(13) 0.044(10) 0.105(15) O6 0.284(20) 0.217(17) 0.185(15) 0.025(12) 0.006(14) -0.061(15) O7 0.213(17) 0.200(17) 0.290(21) 0.080(14) 0.003(15) -0.007(13) O8 0.577(46) 0.242(22) 0.342(29) 0.027(22) -0.171(29) 0.071(27) O9 0.290(47) 0.397(60) 0.185(34) 0.080(36) -0.015(31) 0.048(42) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O11 1.951(6) . ? Cu1 N21 2.020(8) . ? Cu1 N1 2.027(7) . ? Cu1 N32 2.033(8) . ? Cu1 N12 2.241(7) . ? Cu2 O12 1.925(6) . ? Cu2 N72 2.016(7) . ? Cu2 N61 2.029(7) . ? Cu2 N41 2.047(7) . ? Cu2 N52 2.263(8) . ? N1 C2 1.327(10) . ? N1 C14 1.350(10) . ? N12 C11 1.323(11) . ? N12 C13 1.343(11) . ? N21 C22 1.327(12) . ? N21 C34 1.366(12) . ? N32 C31 1.309(12) . ? N32 C33 1.374(11) . ? N41 C42 1.316(12) . ? N41 C54 1.362(11) . ? N52 C51 1.311(12) . ? N52 C53 1.366(11) . ? N61 C62 1.339(11) . ? N61 C74 1.343(11) . ? N72 C71 1.324(11) . ? N72 C73 1.339(10) . ? O11 C15 1.300(10) . ? O12 C15 1.317(11) . ? O13 C15 1.241(11) . ? C2 C3 1.386(12) . ? C3 C4 1.368(13) . ? C4 C5 1.389(13) . ? C5 C14 1.397(12) . ? C5 C6 1.431(12) . ? C6 C7 1.356(13) . ? C7 C8 1.431(13) . ? C8 C9 1.408(13) . ? C8 C13 1.410(11) . ? C9 C10 1.362(14) . ? C10 C11 1.394(13) . ? C13 C14 1.451(12) . ? C22 C23 1.385(15) . ? C23 C24 1.37(2) . ? C24 C25 1.37(2) . ? C25 C34 1.388(13) . ? C25 C26 1.43(2) . ? C26 C27 1.31(2) . ? C27 C28 1.448(15) . ? C28 C33 1.389(14) . ? C28 C29 1.41(2) . ? C29 C30 1.37(2) . ? C30 C31 1.377(15) . ? C33 C34 1.428(14) . ? C42 C43 1.393(13) . ? C43 C44 1.356(15) . ? C44 C45 1.398(14) . ? C45 C54 1.401(12) . ? C45 C46 1.430(14) . ? C46 C47 1.35(2) . ? C47 C48 1.430(15) . ? C48 C53 1.390(13) . ? C48 C49 1.44(2) . ? C49 C50 1.33(2) . ? C50 C51 1.382(15) . ? C53 C54 1.448(13) . ? C62 C63 1.389(13) . ? C63 C64 1.358(14) . ? C64 C65 1.391(13) . ? C65 C66 1.417(13) . ? C65 C74 1.418(12) . ? C66 C67 1.342(14) . ? C67 C68 1.455(13) . ? C68 C73 1.402(12) . ? C68 C69 1.406(13) . ? C69 C70 1.348(14) . ? C70 C71 1.411(13) . ? C73 C74 1.446(12) . ? Cu3 N81 1.994(10) . ? Cu3 N101 1.999(10) . ? Cu3 N92 2.131(10) . ? Cu3 N112 2.156(10) . ? Cu3 O22 2.299(15) . ? Cu4 N152 2.010(9) . ? Cu4 N132 2.030(9) . ? Cu4 N141 2.130(8) . ? Cu4 N121 2.164(9) . ? Cu4 O21 2.192(14) . ? N81 C82 1.310(15) . ? N81 C94 1.349(14) . ? N92 C91 1.319(14) . ? N92 C93 1.350(14) . ? N101 C102 1.307(15) . ? N101 C114 1.359(13) . ? N112 C111 1.330(14) . ? N112 C113 1.364(13) . ? N121 C122 1.318(13) . ? N121 C134 1.371(13) . ? N132 C131 1.323(14) . ? N132 C133 1.347(13) . ? N141 C142 1.326(13) . ? N141 C154 1.368(12) . ? N152 C151 1.291(13) . ? N152 C153 1.354(12) . ? O21 C95 1.260(14) . ? O22 C95 1.21(2) . ? O23 C95 1.23(2) . ? C82 C83 1.42(2) . ? C83 C84 1.38(2) . ? C84 C85 1.40(2) . ? C85 C94 1.40(2) . ? C85 C86 1.45(2) . ? C86 C87 1.35(2) . ? C87 C88 1.41(2) . ? C88 C89 1.39(2) . ? C88 C93 1.45(2) . ? C89 C90 1.34(2) . ? C90 C91 1.39(2) . ? C93 C94 1.43(2) . ? C102 C103 1.43(2) . ? C103 C104 1.36(2) . ? C104 C105 1.41(2) . ? C105 C106 1.40(2) . ? C105 C114 1.41(2) . ? C106 C107 1.31(2) . ? C107 C108 1.43(2) . ? C108 C109 1.37(2) . ? C108 C113 1.397(15) . ? C109 C110 1.36(2) . ? C110 C111 1.39(2) . ? C113 C114 1.43(2) . ? C122 C123 1.39(2) . ? C123 C124 1.31(2) . ? C124 C125 1.38(2) . ? C125 C134 1.426(14) . ? C125 C126 1.44(2) . ? C126 C127 1.33(2) . ? C127 C128 1.418(15) . ? C128 C133 1.382(14) . ? C128 C129 1.40(2) . ? C129 C130 1.36(2) . ? C130 C131 1.42(2) . ? C133 C134 1.438(14) . ? C142 C143 1.42(2) . ? C143 C144 1.34(2) . ? C144 C145 1.386(15) . ? C145 C154 1.394(13) . ? C145 C146 1.44(2) . ? C146 C147 1.337(15) . ? C147 C148 1.431(15) . ? C148 C149 1.357(15) . ? C148 C153 1.404(14) . ? C149 C150 1.38(2) . ? C150 C151 1.42(2) . ? C153 C154 1.427(13) . ? Cl3 O33 1.264(11) . ? Cl3 O34 1.307(11) . ? Cl3 O32 1.333(10) . ? Cl3 O31 1.416(11) . ? Cl4 O44 1.382(9) . ? Cl4 O43 1.386(9) . ? Cl4 O41 1.389(9) . ? Cl4 O42 1.403(9) . ? Cl5 O53 1.17(2) . ? Cl5 O54 1.19(2) . ? Cl5 O52 1.250(14) . ? Cl5 O51 1.28(2) . ? Cl6 O63 1.24(2) . ? Cl6 O64 1.248(15) . ? Cl6 O61 1.26(2) . ? Cl6 O62 1.317(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Cu1 N21 91.1(3) . . ? O11 Cu1 N1 94.7(3) . . ? N21 Cu1 N1 170.7(3) . . ? O11 Cu1 N32 161.4(3) . . ? N21 Cu1 N32 81.5(3) . . ? N1 Cu1 N32 95.0(3) . . ? O11 Cu1 N12 97.6(3) . . ? N21 Cu1 N12 93.8(3) . . ? N1 Cu1 N12 78.3(3) . . ? N32 Cu1 N12 99.8(3) . . ? O12 Cu2 N72 93.2(3) . . ? O12 Cu2 N61 174.0(3) . . ? N72 Cu2 N61 80.7(3) . . ? O12 Cu2 N41 90.6(3) . . ? N72 Cu2 N41 174.5(3) . . ? N61 Cu2 N41 95.4(3) . . ? O12 Cu2 N52 92.3(3) . . ? N72 Cu2 N52 104.9(3) . . ? N61 Cu2 N52 89.2(3) . . ? N41 Cu2 N52 78.8(3) . . ? C2 N1 C14 118.5(7) . . ? C2 N1 Cu1 124.9(6) . . ? C14 N1 Cu1 116.4(5) . . ? C11 N12 C13 118.3(8) . . ? C11 N12 Cu1 131.7(7) . . ? C13 N12 Cu1 109.7(6) . . ? C22 N21 C34 117.5(9) . . ? C22 N21 Cu1 128.6(8) . . ? C34 N21 Cu1 112.7(7) . . ? C31 N32 C33 117.7(9) . . ? C31 N32 Cu1 130.4(7) . . ? C33 N32 Cu1 111.7(7) . . ? C42 N41 C54 118.9(9) . . ? C42 N41 Cu2 125.8(7) . . ? C54 N41 Cu2 115.3(6) . . ? C51 N52 C53 117.7(9) . . ? C51 N52 Cu2 133.2(8) . . ? C53 N52 Cu2 109.1(7) . . ? C62 N61 C74 116.9(8) . . ? C62 N61 Cu2 130.2(7) . . ? C74 N61 Cu2 112.0(6) . . ? C71 N72 C73 118.0(8) . . ? C71 N72 Cu2 128.4(7) . . ? C73 N72 Cu2 113.5(6) . . ? C15 O11 Cu1 108.3(6) . . ? C15 O12 Cu2 120.7(6) . . ? N1 C2 C3 121.7(8) . . ? C4 C3 C2 120.6(9) . . ? C3 C4 C5 118.4(9) . . ? C4 C5 C14 118.2(9) . . ? C4 C5 C6 122.2(9) . . ? C14 C5 C6 119.6(9) . . ? C7 C6 C5 121.0(9) . . ? C6 C7 C8 120.8(9) . . ? C9 C8 C13 116.1(9) . . ? C9 C8 C7 124.1(9) . . ? C13 C8 C7 119.7(9) . . ? C10 C9 C8 119.8(9) . . ? C9 C10 C11 119.7(10) . . ? N12 C11 C10 122.4(10) . . ? N12 C13 C8 123.6(8) . . ? N12 C13 C14 117.5(8) . . ? C8 C13 C14 118.9(8) . . ? N1 C14 C5 122.5(8) . . ? N1 C14 C13 117.7(8) . . ? C5 C14 C13 119.8(8) . . ? O13 C15 O11 122.3(10) . . ? O13 C15 O12 123.2(9) . . ? O11 C15 O12 114.5(9) . . ? N21 C22 C23 121.9(12) . . ? C24 C23 C22 120.8(12) . . ? C23 C24 C25 118.3(11) . . ? C24 C25 C34 118.7(12) . . ? C24 C25 C26 123.5(12) . . ? C34 C25 C26 117.8(12) . . ? C27 C26 C25 121.3(12) . . ? C26 C27 C28 122.4(12) . . ? C33 C28 C29 116.1(11) . . ? C33 C28 C27 117.7(11) . . ? C29 C28 C27 126.2(12) . . ? C30 C29 C28 119.6(11) . . ? C29 C30 C31 119.8(12) . . ? N32 C31 C30 123.0(11) . . ? N32 C33 C28 123.7(10) . . ? N32 C33 C34 116.8(10) . . ? C28 C33 C34 119.4(10) . . ? N21 C34 C25 122.8(10) . . ? N21 C34 C33 115.9(9) . . ? C25 C34 C33 121.4(11) . . ? N41 C42 C43 122.6(10) . . ? C44 C43 C42 118.8(11) . . ? C43 C44 C45 120.7(10) . . ? C44 C45 C54 116.9(10) . . ? C44 C45 C46 123.4(10) . . ? C54 C45 C46 119.8(10) . . ? C47 C46 C45 120.4(11) . . ? C46 C47 C48 122.0(11) . . ? C53 C48 C47 118.4(11) . . ? C53 C48 C49 117.9(11) . . ? C47 C48 C49 123.7(11) . . ? C50 C49 C48 118.2(11) . . ? C49 C50 C51 120.3(12) . . ? N52 C51 C50 124.0(11) . . ? N52 C53 C48 122.0(10) . . ? N52 C53 C54 117.4(9) . . ? C48 C53 C54 120.6(10) . . ? N41 C54 C45 122.1(9) . . ? N41 C54 C53 119.2(9) . . ? C45 C54 C53 118.7(10) . . ? N61 C62 C63 122.9(9) . . ? C64 C63 C62 119.8(10) . . ? C63 C64 C65 119.8(9) . . ? C64 C65 C66 125.4(9) . . ? C64 C65 C74 116.6(9) . . ? C66 C65 C74 118.0(9) . . ? C67 C66 C65 123.2(9) . . ? C66 C67 C68 120.6(9) . . ? C73 C68 C69 116.7(9) . . ? C73 C68 C67 117.9(9) . . ? C69 C68 C67 125.3(9) . . ? C70 C69 C68 119.2(9) . . ? C69 C70 C71 120.2(10) . . ? N72 C71 C70 121.8(10) . . ? N72 C73 C68 123.9(9) . . ? N72 C73 C74 115.4(8) . . ? C68 C73 C74 120.7(8) . . ? N61 C74 C65 123.9(9) . . ? N61 C74 C73 116.5(8) . . ? C65 C74 C73 119.5(8) . . ? N81 Cu3 N101 171.0(4) . . ? N81 Cu3 N92 80.3(4) . . ? N101 Cu3 N92 90.7(4) . . ? N81 Cu3 N112 100.1(4) . . ? N101 Cu3 N112 80.0(4) . . ? N92 Cu3 N112 96.1(3) . . ? N81 Cu3 O22 97.7(4) . . ? N101 Cu3 O22 88.8(4) . . ? N92 Cu3 O22 131.0(4) . . ? N112 Cu3 O22 131.8(4) . . ? N152 Cu4 N132 173.2(4) . . ? N152 Cu4 N141 79.8(3) . . ? N132 Cu4 N141 93.5(4) . . ? N152 Cu4 N121 99.1(4) . . ? N132 Cu4 N121 79.9(4) . . ? N141 Cu4 N121 93.1(3) . . ? N152 Cu4 O21 94.6(3) . . ? N132 Cu4 O21 92.2(4) . . ? N141 Cu4 O21 166.2(3) . . ? N121 Cu4 O21 100.2(3) . . ? C82 N81 C94 120.5(12) . . ? C82 N81 Cu3 124.9(11) . . ? C94 N81 Cu3 114.5(8) . . ? C91 N92 C93 118.8(11) . . ? C91 N92 Cu3 130.6(10) . . ? C93 N92 Cu3 110.6(8) . . ? C102 N101 C114 118.2(11) . . ? C102 N101 Cu3 126.8(10) . . ? C114 N101 Cu3 114.8(8) . . ? C111 N112 C113 116.7(11) . . ? C111 N112 Cu3 132.8(9) . . ? C113 N112 Cu3 110.5(8) . . ? C122 N121 C134 118.3(11) . . ? C122 N121 Cu4 132.2(9) . . ? C134 N121 Cu4 109.5(7) . . ? C131 N132 C133 118.3(10) . . ? C131 N132 Cu4 126.3(8) . . ? C133 N132 Cu4 115.5(7) . . ? C142 N141 C154 118.8(10) . . ? C142 N141 Cu4 129.8(8) . . ? C154 N141 Cu4 111.3(6) . . ? C151 N152 C153 118.5(10) . . ? C151 N152 Cu4 126.4(9) . . ? C153 N152 Cu4 115.2(7) . . ? C95 O21 Cu4 99.1(11) . . ? C95 O22 Cu3 97.8(11) . . ? N81 C82 C83 120.5(14) . . ? C84 C83 C82 119.5(14) . . ? C83 C84 C85 120.2(14) . . ? C84 C85 C94 116.1(14) . . ? C84 C85 C86 124.2(14) . . ? C94 C85 C86 119.7(13) . . ? C87 C86 C85 120.3(14) . . ? C86 C87 C88 122.9(15) . . ? C89 C88 C87 127.9(14) . . ? C89 C88 C93 114.8(13) . . ? C87 C88 C93 117.2(13) . . ? C90 C89 C88 121.7(14) . . ? C89 C90 C91 119.7(14) . . ? N92 C91 C90 122.4(13) . . ? N92 C93 C94 116.7(12) . . ? N92 C93 C88 122.5(12) . . ? C94 C93 C88 120.8(13) . . ? N81 C94 C85 123.3(12) . . ? N81 C94 C93 117.8(12) . . ? C85 C94 C93 119.0(13) . . ? O22 C95 O23 124.0(15) . . ? O22 C95 O21 118.9(17) . . ? O23 C95 O21 117.2(16) . . ? N101 C102 C103 122.1(14) . . ? C104 C103 C102 119.4(14) . . ? C103 C104 C105 119.9(15) . . ? C106 C105 C104 122.8(14) . . ? C106 C105 C114 120.7(14) . . ? C104 C105 C114 116.5(14) . . ? C107 C106 C105 120.6(14) . . ? C106 C107 C108 122.2(14) . . ? C109 C108 C113 115.3(13) . . ? C109 C108 C107 126.0(13) . . ? C113 C108 C107 118.7(13) . . ? C110 C109 C108 122.8(14) . . ? C109 C110 C111 117.6(14) . . ? N112 C111 C110 123.4(13) . . ? N112 C113 C108 124.1(12) . . ? N112 C113 C114 116.2(10) . . ? C108 C113 C114 119.6(12) . . ? N101 C114 C105 123.9(12) . . ? N101 C114 C113 118.0(11) . . ? C105 C114 C113 118.0(12) . . ? N121 C122 C123 122.3(12) . . ? C124 C123 C122 118.9(13) . . ? C123 C124 C125 123.7(14) . . ? C124 C125 C134 114.8(12) . . ? C124 C125 C126 128.0(13) . . ? C134 C125 C126 117.2(11) . . ? C127 C126 C125 122.6(12) . . ? C126 C127 C128 119.9(12) . . ? C133 C128 C129 116.2(11) . . ? C133 C128 C127 121.4(11) . . ? C129 C128 C127 122.4(11) . . ? C130 C129 C128 121.2(11) . . ? C129 C130 C131 117.8(12) . . ? N132 C131 C130 122.3(12) . . ? N132 C133 C128 124.1(11) . . ? N132 C133 C134 116.9(10) . . ? C128 C133 C134 119.0(11) . . ? N121 C134 C125 122.0(10) . . ? N121 C134 C133 118.1(10) . . ? C125 C134 C133 119.9(11) . . ? N141 C142 C143 120.1(12) . . ? C144 C143 C142 121.2(12) . . ? C143 C144 C145 119.7(12) . . ? C144 C145 C154 117.7(12) . . ? C144 C145 C146 124.5(11) . . ? C154 C145 C146 117.8(10) . . ? C147 C146 C145 120.9(11) . . ? C146 C147 C148 122.4(11) . . ? C149 C148 C153 117.7(11) . . ? C149 C148 C147 124.4(12) . . ? C153 C148 C147 117.9(11) . . ? C148 C149 C150 120.3(12) . . ? C149 C150 C151 117.9(12) . . ? N152 C151 C150 122.7(13) . . ? N152 C153 C148 122.8(10) . . ? N152 C153 C154 117.4(10) . . ? C148 C153 C154 119.8(10) . . ? N141 C154 C145 122.6(10) . . ? N141 C154 C153 116.2(9) . . ? C145 C154 C153 121.2(10) . . ? O33 Cl3 O34 112.1(12) . . ? O33 Cl3 O32 109.9(12) . . ? O34 Cl3 O32 105.5(11) . . ? O33 Cl3 O31 109.9(9) . . ? O34 Cl3 O31 107.9(9) . . ? O32 Cl3 O31 111.5(8) . . ? O44 Cl4 O43 108.3(8) . . ? O44 Cl4 O41 108.8(7) . . ? O43 Cl4 O41 112.0(7) . . ? O44 Cl4 O42 107.5(7) . . ? O43 Cl4 O42 109.9(7) . . ? O41 Cl4 O42 110.2(7) . . ? O53 Cl5 O54 113.8(24) . . ? O53 Cl5 O52 107.1(18) . . ? O54 Cl5 O52 102.4(19) . . ? O53 Cl5 O51 106.5(15) . . ? O54 Cl5 O51 110.4(19) . . ? O52 Cl5 O51 116.8(16) . . ? O63 Cl6 O64 113.8(17) . . ? O63 Cl6 O61 102.5(17) . . ? O64 Cl6 O61 98.6(17) . . ? O63 Cl6 O62 114.8(14) . . ? O64 Cl6 O62 111.4(14) . . ? O61 Cl6 O62 114.4(15) . . ? _refine_diff_density_max .507 _refine_diff_density_min -.556 _refine_diff_density_rms .085 #===END OF DATA FOR 3 # 4.4 RESULTS FOR 4 data_maon12 _database_code_CSD 164330 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H41 Cl2 Cu2 N9 O13' _chemical_formula_weight 1197.92 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 11.44(1) _cell_length_b 21.57(1) _cell_length_c 20.26(1) _cell_angle_alpha 90.0 _cell_angle_beta 91.4(1) _cell_angle_gamma 90.0 _cell_volume 4998(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'blue-green' _exptl_crystal_size_max 0.73 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2448 _exptl_absorpt_coefficient_mu 1.036 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 'Philips PW1100/10' _diffrn_measurement_method '\w/2\q-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17510 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_sigmaI/netI 0.0644 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 25.01 _reflns_number_total 8772 _reflns_number_gt 5826 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'PWCOM 6.6 (Gomm, 1993)' _computing_cell_refinement 'PWCOM 6.6 (Gomm, 1993)' _computing_data_reduction 'INREAD (Liehr, 1981)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXTL 5.1 (Bruker AXS, 1998)' _computing_molecular_graphics 'SHELXTL 5.1 (Bruker AXS, 1998)' _computing_publication_material 'SHELXTL 5.1 (Bruker AXS, 1998)' _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^)+(0.0407P)^2^+8.2031P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment 'refxyz except solvate DMF hydrogen atoms noref' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8772 _refine_ls_number_parameters 799 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0887 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1188 _refine_ls_wR_factor_gt 0.0968 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 Cu1 Cu 0.91575(4) 0.20368(2) 0.29280(2) 0.02360(14) Uani 1 1 d . . . Cu2 Cu 0.55845(4) 0.25376(2) 0.13038(3) 0.02573(14) Uani 1 1 d . . . N1 N 0.9635(3) 0.13764(16) 0.22869(17) 0.0285(8) Uani 1 1 d . . . N12 N 1.0929(3) 0.21556(17) 0.30038(18) 0.0305(9) Uani 1 1 d . . . N21 N 0.8893(3) 0.28615(16) 0.33929(16) 0.0222(8) Uani 1 1 d . . . N32 N 0.8981(3) 0.17269(16) 0.39631(17) 0.0271(8) Uani 1 1 d . . . N41 N 0.3617(3) 0.26149(16) 0.12481(18) 0.0288(8) Uani 1 1 d . . . N52 N 0.5312(3) 0.33769(16) 0.17330(18) 0.0280(8) Uani 1 1 d . . . N61 N 0.5721(3) 0.28445(17) 0.03623(18) 0.0296(8) Uani 1 1 d . . . N72 N 0.5768(3) 0.17070(16) 0.08466(18) 0.0286(8) Uani 1 1 d . . . O11 O 0.7506(2) 0.19041(13) 0.27593(14) 0.0273(7) Uani 1 1 d . . . O12 O 0.5950(2) 0.21686(13) 0.21560(14) 0.0268(7) Uani 1 1 d . . . O13 O 0.7711(2) 0.25490(13) 0.19048(14) 0.0277(7) Uani 1 1 d . . . C2 C 0.8964(5) 0.1002(2) 0.1921(2) 0.0365(12) Uani 1 1 d . . . C3 C 0.9432(6) 0.0601(2) 0.1455(3) 0.0467(15) Uani 1 1 d . . . C4 C 1.0609(6) 0.0575(2) 0.1379(3) 0.0474(15) Uani 1 1 d . . . C5 C 1.1358(5) 0.0932(2) 0.1785(2) 0.0392(12) Uani 1 1 d . . . C6 C 1.2615(6) 0.0915(3) 0.1786(3) 0.0566(18) Uani 1 1 d . . . C7 C 1.3270(6) 0.1280(3) 0.2175(3) 0.0594(17) Uani 1 1 d . . . C8 C 1.2735(4) 0.1727(3) 0.2598(3) 0.0449(13) Uani 1 1 d . . . C9 C 1.3371(4) 0.2165(3) 0.2984(3) 0.0529(16) Uani 1 1 d . . . C10 C 1.2789(4) 0.2567(3) 0.3366(3) 0.0507(14) Uani 1 1 d . . . C11 C 1.1560(4) 0.2552(3) 0.3368(2) 0.0400(12) Uani 1 1 d . . . C13 C 1.1517(4) 0.1747(2) 0.2628(2) 0.0323(10) Uani 1 1 d . . . C14 C 1.0813(4) 0.1336(2) 0.2224(2) 0.0310(10) Uani 1 1 d . . . C15 C 0.7075(3) 0.22228(18) 0.2261(2) 0.0228(9) Uani 1 1 d . . . C22 C 0.8875(4) 0.3412(2) 0.3104(2) 0.0283(10) Uani 1 1 d . . . C23 C 0.8844(4) 0.3967(2) 0.3463(3) 0.0380(12) Uani 1 1 d . . . C24 C 0.8798(4) 0.3943(2) 0.4136(2) 0.0359(12) Uani 1 1 d . . . C25 C 0.8781(3) 0.3367(2) 0.4452(2) 0.0271(10) Uani 1 1 d . . . C26 C 0.8687(4) 0.3296(3) 0.5156(2) 0.0350(11) Uani 1 1 d . . . C27 C 0.8650(4) 0.2732(3) 0.5438(2) 0.0377(13) Uani 1 1 d . . . C28 C 0.8752(4) 0.2176(2) 0.5053(2) 0.0334(11) Uani 1 1 d . . . C29 C 0.8738(4) 0.1575(3) 0.5318(3) 0.0452(14) Uani 1 1 d . . . C30 C 0.8834(5) 0.1074(3) 0.4909(3) 0.0476(14) Uani 1 1 d . . . C31 C 0.8960(4) 0.1170(2) 0.4233(3) 0.0404(13) Uani 1 1 d . . . C33 C 0.8857(3) 0.2227(2) 0.4365(2) 0.0255(9) Uani 1 1 d . . . C34 C 0.8845(3) 0.2832(2) 0.4064(2) 0.0246(9) Uani 1 1 d . . . C42 C 0.2788(4) 0.2269(2) 0.0959(2) 0.0338(11) Uani 1 1 d . . . C43 C 0.1597(4) 0.2383(2) 0.1036(3) 0.0399(12) Uani 1 1 d . . . C44 C 0.1249(4) 0.2852(2) 0.1439(3) 0.0407(13) Uani 1 1 d . . . C45 C 0.2092(4) 0.3238(2) 0.1747(2) 0.0339(11) Uani 1 1 d . . . C46 C 0.1837(5) 0.3757(2) 0.2160(3) 0.0439(13) Uani 1 1 d . . . C47 C 0.2684(5) 0.4128(2) 0.2408(3) 0.0430(13) Uani 1 1 d . . . C48 C 0.3887(4) 0.4023(2) 0.2271(2) 0.0365(11) Uani 1 1 d . . . C49 C 0.4804(5) 0.4425(2) 0.2475(3) 0.0441(13) Uani 1 1 d . . . C50 C 0.5928(5) 0.4297(2) 0.2310(3) 0.0426(13) Uani 1 1 d . . . C51 C 0.6158(4) 0.3761(2) 0.1941(3) 0.0364(12) Uani 1 1 d . . . C53 C 0.4182(4) 0.35067(19) 0.1890(2) 0.0275(10) Uani 1 1 d . . . C54 C 0.3280(4) 0.31050(19) 0.1624(2) 0.0280(10) Uani 1 1 d . . . C62 C 0.5754(4) 0.3422(2) 0.0132(3) 0.0383(12) Uani 1 1 d . . . C63 C 0.5837(4) 0.3561(3) -0.0540(3) 0.0433(13) Uani 1 1 d . . . C64 C 0.5865(4) 0.3085(3) -0.0985(3) 0.0424(13) Uani 1 1 d . . . C65 C 0.5804(4) 0.2467(2) -0.0766(2) 0.0326(10) Uani 1 1 d . . . C66 C 0.5835(4) 0.1935(3) -0.1193(3) 0.0401(13) Uani 1 1 d . . . C67 C 0.5840(4) 0.1362(3) -0.0945(3) 0.0422(13) Uani 1 1 d . . . C68 C 0.5844(4) 0.1246(2) -0.0245(2) 0.0339(11) Uani 1 1 d . . . C69 C 0.5966(4) 0.0662(2) 0.0048(3) 0.0382(12) Uani 1 1 d . . . C70 C 0.5987(4) 0.0612(2) 0.0725(3) 0.0383(12) Uani 1 1 d . . . C71 C 0.5876(4) 0.1143(2) 0.1111(2) 0.0308(11) Uani 1 1 d . . . C73 C 0.5767(3) 0.1760(2) 0.0178(2) 0.0278(10) Uani 1 1 d . . . C74 C 0.5745(3) 0.2375(2) -0.0085(2) 0.0268(10) Uani 1 1 d . . . Cl2 Cl 0.92230(12) 0.01630(6) 0.66669(6) 0.0428(3) Uani 1 1 d . . . O21 O 0.8909(4) 0.07936(19) 0.6754(2) 0.0715(13) Uani 1 1 d . . . O22 O 1.0173(4) 0.0000(2) 0.7093(2) 0.0793(14) Uani 1 1 d . . . O23 O 0.9536(7) 0.0083(3) 0.6018(2) 0.155(3) Uani 1 1 d . . . O24 O 0.8288(5) -0.0222(3) 0.6825(4) 0.142(3) Uani 1 1 d . . . Cl3 Cl 0.22215(10) 0.08661(5) -0.03383(6) 0.0382(3) Uani 1 1 d . . . O31 O 0.1430(4) 0.0368(2) -0.0234(2) 0.0758(13) Uani 1 1 d . . . O32 O 0.3119(3) 0.08438(18) 0.0166(2) 0.0653(12) Uani 1 1 d . . . O33 O 0.1635(4) 0.14469(19) -0.0302(2) 0.0700(13) Uani 1 1 d . . . O34 O 0.2722(5) 0.0785(2) -0.0966(2) 0.0898(16) Uani 1 1 d . . . N80 N 0.7226(7) 0.5582(4) -0.0102(5) 0.114(3) Uani 1 1 d . . . O80 O 0.6520(6) 0.4948(3) -0.0953(3) 0.121(2) Uani 1 1 d . . . C80 C 0.7135(9) 0.5365(6) -0.0714(7) 0.130(4) Uani 1 1 d . . . C81 C 0.7883(16) 0.6071(7) 0.0077(10) 0.334(15) Uani 1 1 d . . . C82 C 0.6551(6) 0.5265(5) 0.0407(5) 0.101(3) Uani 1 1 d . . . O1 O 0.6324(4) 0.07367(18) 0.2790(2) 0.0729(13) Uani 1 1 d . . . H2 H 0.820(5) 0.101(3) 0.199(3) 0.080 Uiso 1 1 d . . . H3 H 0.895(5) 0.040(3) 0.124(3) 0.080 Uiso 1 1 d . . . H4 H 1.099(5) 0.033(3) 0.103(3) 0.080 Uiso 1 1 d . . . H6 H 1.294(5) 0.064(3) 0.153(3) 0.080 Uiso 1 1 d . . . H7 H 1.404(5) 0.128(3) 0.216(3) 0.080 Uiso 1 1 d . . . H9 H 1.418(5) 0.216(3) 0.298(3) 0.080 Uiso 1 1 d . . . H10 H 1.314(5) 0.287(3) 0.364(3) 0.080 Uiso 1 1 d . . . H11 H 1.118(5) 0.281(3) 0.362(3) 0.080 Uiso 1 1 d . . . H22 H 0.889(5) 0.337(3) 0.264(3) 0.080 Uiso 1 1 d . . . H23 H 0.878(5) 0.432(3) 0.325(3) 0.080 Uiso 1 1 d . . . H24 H 0.882(5) 0.431(3) 0.440(3) 0.080 Uiso 1 1 d . . . H26 H 0.861(5) 0.368(3) 0.540(3) 0.080 Uiso 1 1 d . . . H27 H 0.857(5) 0.268(3) 0.584(3) 0.080 Uiso 1 1 d . . . H29 H 0.865(5) 0.157(3) 0.575(3) 0.080 Uiso 1 1 d . . . H30 H 0.875(5) 0.068(3) 0.505(3) 0.080 Uiso 1 1 d . . . H31 H 0.900(5) 0.087(3) 0.399(3) 0.080 Uiso 1 1 d . . . H42 H 0.308(5) 0.194(3) 0.068(3) 0.080 Uiso 1 1 d . . . H43 H 0.107(5) 0.214(3) 0.079(3) 0.080 Uiso 1 1 d . . . H44 H 0.051(5) 0.295(3) 0.154(3) 0.080 Uiso 1 1 d . . . H46 H 0.106(5) 0.379(3) 0.225(3) 0.080 Uiso 1 1 d . . . H47 H 0.248(5) 0.449(3) 0.269(3) 0.080 Uiso 1 1 d . . . H49 H 0.459(5) 0.474(3) 0.272(3) 0.080 Uiso 1 1 d . . . H50 H 0.654(5) 0.454(3) 0.242(3) 0.080 Uiso 1 1 d . . . H51 H 0.686(5) 0.367(3) 0.185(3) 0.080 Uiso 1 1 d . . . H62 H 0.572(5) 0.371(3) 0.047(3) 0.080 Uiso 1 1 d . . . H63 H 0.584(5) 0.396(3) -0.067(3) 0.080 Uiso 1 1 d . . . H64 H 0.588(5) 0.315(3) -0.139(3) 0.080 Uiso 1 1 d . . . H66 H 0.583(5) 0.200(3) -0.163(3) 0.080 Uiso 1 1 d . . . H67 H 0.590(5) 0.101(3) -0.119(3) 0.080 Uiso 1 1 d . . . H69 H 0.608(5) 0.030(3) -0.019(3) 0.080 Uiso 1 1 d . . . H70 H 0.610(5) 0.028(3) 0.093(3) 0.080 Uiso 1 1 d . . . H71 H 0.589(5) 0.114(3) 0.153(3) 0.080 Uiso 1 1 d . . . H1A H 0.6689 0.1053 0.2830 0.080 Uiso 1 1 d . . . H1B H 0.5812 0.0769 0.2633 0.080 Uiso 1 1 d . . . H80 H 0.7705 0.5613 -0.1020 0.080 Uiso 1 1 d . . . H81A H 0.7775 0.6366 -0.0130 0.080 Uiso 1 1 d . . . H81B H 0.8609 0.5897 0.0028 0.080 Uiso 1 1 d . . . H81C H 0.7861 0.6108 0.0538 0.080 Uiso 1 1 d . . . H82A H 0.6502 0.5528 0.0879 0.080 Uiso 1 1 d . . . H82B H 0.6792 0.4806 0.0425 0.080 Uiso 1 1 d . . . H82C H 0.5780 0.5204 0.0271 0.080 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 Cu1 0.0225(3) 0.0281(3) 0.0203(3) -0.0034(2) -0.0001(2) 0.0008(2) Cu2 0.0249(3) 0.0248(3) 0.0274(3) -0.0022(2) -0.0019(2) 0.0023(2) N1 0.036(2) 0.029(2) 0.0204(19) -0.0005(16) -0.0017(16) 0.0040(16) N12 0.0256(19) 0.041(2) 0.025(2) -0.0051(17) 0.0027(16) 0.0027(17) N21 0.0168(17) 0.029(2) 0.0211(19) -0.0036(16) 0.0003(14) 0.0003(14) N32 0.0252(19) 0.030(2) 0.026(2) 0.0067(17) 0.0001(15) 0.0036(16) N41 0.0285(19) 0.027(2) 0.030(2) -0.0015(17) -0.0043(16) 0.0023(16) N52 0.0282(19) 0.0271(19) 0.028(2) -0.0003(16) -0.0062(16) -0.0007(16) N61 0.0278(19) 0.031(2) 0.030(2) 0.0039(17) 0.0013(16) 0.0020(16) N72 0.0235(19) 0.030(2) 0.032(2) -0.0034(17) 0.0002(15) 0.0019(16) O11 0.0273(16) 0.0309(16) 0.0236(16) 0.0033(13) -0.0019(12) -0.0003(13) O12 0.0220(15) 0.0298(16) 0.0285(17) 0.0007(13) -0.0038(12) 0.0019(12) O13 0.0277(15) 0.0326(16) 0.0229(16) 0.0043(14) 0.0041(12) 0.0014(13) C2 0.054(3) 0.027(2) 0.028(3) 0.002(2) -0.008(2) 0.009(2) C3 0.088(5) 0.027(3) 0.025(3) -0.001(2) -0.013(3) 0.007(3) C4 0.087(5) 0.028(3) 0.028(3) 0.007(2) 0.021(3) 0.019(3) C5 0.066(3) 0.026(3) 0.027(3) 0.007(2) 0.017(2) 0.014(2) C6 0.071(4) 0.041(3) 0.060(4) 0.013(3) 0.042(3) 0.024(3) C7 0.044(3) 0.063(4) 0.072(4) 0.010(4) 0.025(3) 0.018(3) C8 0.029(3) 0.057(3) 0.049(3) 0.012(3) 0.016(2) 0.014(2) C9 0.021(2) 0.080(4) 0.057(4) 0.011(3) 0.000(2) 0.002(3) C10 0.032(3) 0.071(4) 0.049(4) -0.003(3) -0.003(2) -0.007(3) C11 0.030(3) 0.056(3) 0.034(3) -0.006(3) -0.002(2) -0.004(2) C13 0.031(2) 0.036(3) 0.030(3) 0.007(2) 0.005(2) 0.008(2) C14 0.043(3) 0.027(2) 0.023(2) 0.0072(19) 0.012(2) 0.010(2) C15 0.025(2) 0.023(2) 0.021(2) -0.0065(18) 0.0000(18) 0.0016(17) C22 0.031(2) 0.029(2) 0.025(2) 0.000(2) -0.0002(19) -0.0037(19) C23 0.046(3) 0.032(3) 0.036(3) 0.000(2) 0.001(2) -0.009(2) C24 0.040(3) 0.030(3) 0.038(3) -0.011(2) 0.001(2) -0.005(2) C25 0.021(2) 0.037(3) 0.024(2) -0.007(2) 0.0011(17) -0.0009(19) C26 0.024(2) 0.055(3) 0.026(3) -0.014(2) 0.0004(19) -0.003(2) C27 0.022(2) 0.074(4) 0.017(2) -0.004(3) -0.0027(19) -0.001(2) C28 0.019(2) 0.058(3) 0.023(2) 0.008(2) -0.0040(18) -0.001(2) C29 0.039(3) 0.068(4) 0.029(3) 0.019(3) -0.001(2) -0.003(3) C30 0.048(3) 0.050(3) 0.045(3) 0.028(3) -0.009(3) -0.001(3) C31 0.037(3) 0.037(3) 0.047(3) 0.009(2) -0.006(2) 0.010(2) C33 0.017(2) 0.040(3) 0.019(2) 0.0019(19) -0.0030(16) -0.0005(18) C34 0.0143(19) 0.039(3) 0.021(2) 0.0001(19) 0.0008(16) -0.0003(18) C42 0.029(2) 0.032(3) 0.040(3) -0.002(2) -0.006(2) -0.001(2) C43 0.026(2) 0.044(3) 0.049(3) 0.006(3) -0.009(2) -0.003(2) C44 0.025(2) 0.048(3) 0.049(3) 0.016(3) 0.000(2) 0.004(2) C45 0.030(2) 0.037(3) 0.035(3) 0.007(2) -0.001(2) 0.008(2) C46 0.040(3) 0.043(3) 0.050(3) 0.003(3) 0.012(3) 0.014(3) C47 0.048(3) 0.038(3) 0.043(3) -0.002(2) 0.009(2) 0.016(3) C48 0.043(3) 0.037(3) 0.029(3) -0.004(2) -0.004(2) 0.012(2) C49 0.061(4) 0.030(3) 0.041(3) -0.011(2) -0.011(3) 0.011(2) C50 0.053(3) 0.032(3) 0.043(3) -0.005(2) -0.017(3) 0.003(2) C51 0.033(3) 0.035(3) 0.041(3) -0.001(2) -0.007(2) 0.003(2) C53 0.030(2) 0.026(2) 0.027(2) -0.0029(19) -0.0023(18) 0.0055(19) C54 0.028(2) 0.026(2) 0.030(2) 0.0055(19) -0.0019(19) 0.0069(18) C62 0.043(3) 0.034(3) 0.038(3) 0.003(2) 0.004(2) 0.000(2) C63 0.044(3) 0.045(3) 0.041(3) 0.013(3) 0.006(2) 0.000(2) C64 0.033(3) 0.060(4) 0.034(3) 0.010(3) 0.004(2) 0.000(2) C65 0.020(2) 0.050(3) 0.028(3) 0.002(2) -0.0017(18) -0.004(2) C66 0.031(3) 0.061(4) 0.028(3) -0.008(3) -0.003(2) -0.002(2) C67 0.032(3) 0.054(3) 0.040(3) -0.022(3) -0.003(2) -0.002(2) C68 0.025(2) 0.041(3) 0.035(3) -0.014(2) -0.001(2) -0.002(2) C69 0.032(3) 0.036(3) 0.047(3) -0.012(2) -0.001(2) 0.000(2) C70 0.034(3) 0.029(3) 0.051(3) -0.003(2) 0.001(2) 0.001(2) C71 0.022(2) 0.032(3) 0.038(3) 0.002(2) 0.000(2) 0.0004(19) C73 0.016(2) 0.035(2) 0.032(3) -0.004(2) -0.0005(18) -0.0011(18) C74 0.019(2) 0.034(3) 0.027(2) -0.003(2) -0.0008(17) -0.0024(18) Cl2 0.0620(8) 0.0352(7) 0.0311(7) 0.0040(5) -0.0003(6) 0.0070(6) O21 0.095(3) 0.057(3) 0.062(3) -0.013(2) -0.005(2) 0.032(2) O22 0.076(3) 0.069(3) 0.091(4) 0.037(3) -0.038(3) -0.008(2) O23 0.294(9) 0.129(5) 0.043(3) 0.023(3) 0.043(4) 0.146(6) O24 0.105(4) 0.120(5) 0.197(7) 0.082(5) -0.074(4) -0.059(4) Cl3 0.0426(7) 0.0366(6) 0.0354(7) -0.0050(5) -0.0006(5) 0.0042(5) O31 0.089(3) 0.073(3) 0.066(3) -0.018(2) 0.007(2) -0.038(3) O32 0.057(2) 0.062(3) 0.075(3) -0.013(2) -0.030(2) 0.014(2) O33 0.069(3) 0.062(3) 0.078(3) -0.021(2) -0.021(2) 0.029(2) O34 0.140(4) 0.085(3) 0.047(3) 0.007(2) 0.040(3) 0.024(3) N80 0.088(5) 0.093(5) 0.159(8) 0.044(6) -0.061(6) -0.017(4) O80 0.164(6) 0.069(4) 0.130(6) 0.015(4) -0.011(5) -0.028(4) C80 0.110(8) 0.106(9) 0.172(12) 0.092(9) -0.026(8) -0.010(6) C81 0.34(2) 0.227(15) 0.42(3) 0.218(17) -0.31(2) -0.199(16) C82 0.054(4) 0.129(7) 0.120(7) -0.005(6) 0.008(4) 0.011(5) O1 0.086(3) 0.051(2) 0.082(3) -0.014(2) 0.009(2) -0.032(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 Cu1 O11 1.933(3) . ? Cu1 N1 2.013(4) . ? Cu1 N21 2.039(3) . ? Cu1 N12 2.045(4) . ? Cu1 N32 2.215(4) . ? Cu2 O12 1.938(3) . ? Cu2 N61 2.029(4) . ? Cu2 N72 2.030(4) . ? Cu2 N52 2.036(4) . ? Cu2 N41 2.258(4) . ? N1 C2 1.328(6) . ? N1 C14 1.359(6) . ? N12 C11 1.332(6) . ? N12 C13 1.354(6) . ? N21 C22 1.324(5) . ? N21 C34 1.363(5) . ? N32 C31 1.321(6) . ? N32 C33 1.361(5) . ? N41 C42 1.330(6) . ? N41 C54 1.364(5) . ? N52 C51 1.335(6) . ? N52 C53 1.367(5) . ? N61 C62 1.332(6) . ? N61 C74 1.359(5) . ? N72 C71 1.333(6) . ? N72 C73 1.359(6) . ? O11 C15 1.307(5) . ? O12 C15 1.305(5) . ? O13 C15 1.253(5) . ? C2 C3 1.397(7) . ? C2 H2 0.89(6) . ? C3 C4 1.360(8) . ? C3 H3 0.82(6) . ? C4 C5 1.402(8) . ? C4 H4 1.00(6) . ? C5 C14 1.403(6) . ? C5 C6 1.439(8) . ? C6 C7 1.331(9) . ? C6 H6 0.88(6) . ? C7 C8 1.437(8) . ? C7 H7 0.88(6) . ? C8 C13 1.397(6) . ? C8 C9 1.415(8) . ? C9 C10 1.349(8) . ? C9 H9 0.93(6) . ? C10 C11 1.406(7) . ? C10 H10 0.95(6) . ? C11 H11 0.88(6) . ? C13 C14 1.439(7) . ? C22 C23 1.402(7) . ? C22 H22 0.94(6) . ? C23 C24 1.366(7) . ? C23 H23 0.88(6) . ? C24 C25 1.399(6) . ? C24 H24 0.96(6) . ? C25 C34 1.399(6) . ? C25 C26 1.440(6) . ? C26 C27 1.345(7) . ? C26 H26 0.98(6) . ? C27 C28 1.436(7) . ? C27 H27 0.82(6) . ? C28 C29 1.404(7) . ? C28 C33 1.405(6) . ? C29 C30 1.366(8) . ? C29 H29 0.89(6) . ? C30 C31 1.397(8) . ? C30 H30 0.90(6) . ? C31 H31 0.81(6) . ? C33 C34 1.442(6) . ? C42 C43 1.397(7) . ? C42 H42 0.98(6) . ? C43 C44 1.366(7) . ? C43 H43 0.93(6) . ? C44 C45 1.407(7) . ? C44 H44 0.90(6) . ? C45 C54 1.417(6) . ? C45 C46 1.432(7) . ? C46 C47 1.345(8) . ? C46 H46 0.91(6) . ? C47 C48 1.429(7) . ? C47 H47 1.00(6) . ? C48 C53 1.401(6) . ? C48 C49 1.414(7) . ? C49 C50 1.365(8) . ? C49 H49 0.89(6) . ? C50 C51 1.406(7) . ? C50 H50 0.90(6) . ? C51 H51 0.85(6) . ? C53 C54 1.442(6) . ? C62 C63 1.400(7) . ? C62 H62 0.93(6) . ? C63 C64 1.366(8) . ? C63 H63 0.90(6) . ? C64 C65 1.407(7) . ? C64 H64 0.84(6) . ? C65 C74 1.399(6) . ? C65 C66 1.438(7) . ? C66 C67 1.334(8) . ? C66 H66 0.90(6) . ? C67 C68 1.441(7) . ? C67 H67 0.91(6) . ? C68 C69 1.398(7) . ? C68 C73 1.405(6) . ? C69 C70 1.374(7) . ? C69 H69 0.92(6) . ? C70 C71 1.396(7) . ? C70 H70 0.83(6) . ? C71 H71 0.85(6) . ? C73 C74 1.430(6) . ? Cl2 O23 1.382(5) . ? Cl2 O24 1.398(5) . ? Cl2 O22 1.416(4) . ? Cl2 O21 1.419(4) . ? Cl3 O34 1.417(4) . ? Cl3 O33 1.424(4) . ? Cl3 O31 1.424(4) . ? Cl3 O32 1.431(4) . ? N80 C80 1.326(15) . ? N80 C81 1.340(13) . ? N80 C82 1.472(11) . ? O80 C80 1.234(13) . ? C80 H80 1.0562 . ? C81 H81A 0.7699 . ? C81 H81B 0.9179 . ? C81 H81C 0.9392 . ? C82 H82A 1.1154 . ? C82 H82B 1.0291 . ? C82 H82C 0.9267 . ? O1 H1A 0.8026 . ? O1 H1B 0.6622 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Cu1 N1 93.49(15) . . ? O11 Cu1 N21 93.18(13) . . ? N1 Cu1 N21 164.04(14) . . ? O11 Cu1 N12 173.95(13) . . ? N1 Cu1 N12 81.53(16) . . ? N21 Cu1 N12 90.80(14) . . ? O11 Cu1 N32 90.65(15) . . ? N1 Cu1 N32 115.47(14) . . ? N21 Cu1 N32 78.92(14) . . ? N12 Cu1 N32 94.58(16) . . ? O12 Cu2 N61 162.18(13) . . ? O12 Cu2 N72 91.23(14) . . ? N61 Cu2 N72 81.24(15) . . ? O12 Cu2 N52 90.95(13) . . ? N61 Cu2 N52 97.33(15) . . ? N72 Cu2 N52 176.72(14) . . ? O12 Cu2 N41 105.56(15) . . ? N61 Cu2 N41 91.62(16) . . ? N72 Cu2 N41 99.01(14) . . ? N52 Cu2 N41 78.04(14) . . ? C2 N1 C14 118.0(4) . . ? C2 N1 Cu1 128.9(3) . . ? C14 N1 Cu1 113.1(3) . . ? C11 N12 C13 117.4(4) . . ? C11 N12 Cu1 130.2(3) . . ? C13 N12 Cu1 112.4(3) . . ? C22 N21 C34 118.8(4) . . ? C22 N21 Cu1 125.4(3) . . ? C34 N21 Cu1 115.5(3) . . ? C31 N32 C33 118.0(4) . . ? C31 N32 Cu1 132.0(3) . . ? C33 N32 Cu1 109.9(3) . . ? C42 N41 C54 118.2(4) . . ? C42 N41 Cu2 132.8(3) . . ? C54 N41 Cu2 108.9(3) . . ? C51 N52 C53 118.8(4) . . ? C51 N52 Cu2 124.7(3) . . ? C53 N52 Cu2 115.9(3) . . ? C62 N61 C74 117.5(4) . . ? C62 N61 Cu2 129.7(3) . . ? C74 N61 Cu2 112.7(3) . . ? C71 N72 C73 118.4(4) . . ? C71 N72 Cu2 129.1(3) . . ? C73 N72 Cu2 112.5(3) . . ? C15 O11 Cu1 114.0(3) . . ? C15 O12 Cu2 107.4(3) . . ? N1 C2 C3 121.9(5) . . ? N1 C2 H2 117(4) . . ? C3 C2 H2 121(4) . . ? C4 C3 C2 119.9(5) . . ? C4 C3 H3 125(5) . . ? C2 C3 H3 115(5) . . ? C3 C4 C5 120.3(5) . . ? C3 C4 H4 123(3) . . ? C5 C4 H4 116(3) . . ? C4 C5 C14 116.0(5) . . ? C4 C5 C6 125.7(5) . . ? C14 C5 C6 118.3(5) . . ? C7 C6 C5 122.3(5) . . ? C7 C6 H6 121(4) . . ? C5 C6 H6 117(4) . . ? C6 C7 C8 120.6(6) . . ? C6 C7 H7 123(4) . . ? C8 C7 H7 117(4) . . ? C13 C8 C9 117.1(5) . . ? C13 C8 C7 119.1(6) . . ? C9 C8 C7 123.8(5) . . ? C10 C9 C8 119.4(5) . . ? C10 C9 H9 122(4) . . ? C8 C9 H9 119(4) . . ? C9 C10 C11 119.7(5) . . ? C9 C10 H10 125(4) . . ? C11 C10 H10 115(4) . . ? N12 C11 C10 122.7(5) . . ? N12 C11 H11 117(4) . . ? C10 C11 H11 120(4) . . ? N12 C13 C8 123.6(5) . . ? N12 C13 C14 116.2(4) . . ? C8 C13 C14 120.1(4) . . ? N1 C14 C5 123.8(5) . . ? N1 C14 C13 116.7(4) . . ? C5 C14 C13 119.5(4) . . ? O13 C15 O12 122.7(4) . . ? O13 C15 O11 121.8(4) . . ? O12 C15 O11 115.5(4) . . ? N21 C22 C23 122.4(4) . . ? N21 C22 H22 111(4) . . ? C23 C22 H22 126(4) . . ? C24 C23 C22 119.3(5) . . ? C24 C23 H23 121(4) . . ? C22 C23 H23 119(4) . . ? C23 C24 C25 119.4(4) . . ? C23 C24 H24 122(4) . . ? C25 C24 H24 119(4) . . ? C34 C25 C24 118.2(4) . . ? C34 C25 C26 118.4(4) . . ? C24 C25 C26 123.4(4) . . ? C27 C26 C25 121.4(5) . . ? C27 C26 H26 123(4) . . ? C25 C26 H26 115(4) . . ? C26 C27 C28 121.3(4) . . ? C26 C27 H27 123(5) . . ? C28 C27 H27 115(5) . . ? C29 C28 C33 116.9(5) . . ? C29 C28 C27 124.2(4) . . ? C33 C28 C27 118.9(4) . . ? C30 C29 C28 119.8(5) . . ? C30 C29 H29 127(4) . . ? C28 C29 H29 113(4) . . ? C29 C30 C31 119.3(5) . . ? C29 C30 H30 123(4) . . ? C31 C30 H30 118(4) . . ? N32 C31 C30 122.9(5) . . ? N32 C31 H31 118(5) . . ? C30 C31 H31 119(5) . . ? N32 C33 C28 123.0(4) . . ? N32 C33 C34 117.7(4) . . ? C28 C33 C34 119.4(4) . . ? N21 C34 C25 121.8(4) . . ? N21 C34 C33 117.6(4) . . ? C25 C34 C33 120.5(4) . . ? N41 C42 C43 122.6(5) . . ? N41 C42 H42 114(3) . . ? C43 C42 H42 123(4) . . ? C44 C43 C42 119.7(5) . . ? C44 C43 H43 123(4) . . ? C42 C43 H43 117(4) . . ? C43 C44 C45 119.8(4) . . ? C43 C44 H44 126(4) . . ? C45 C44 H44 115(4) . . ? C44 C45 C54 116.9(4) . . ? C44 C45 C46 125.0(4) . . ? C54 C45 C46 118.1(4) . . ? C47 C46 C45 121.9(5) . . ? C47 C46 H46 125(4) . . ? C45 C46 H46 113(4) . . ? C46 C47 C48 121.5(5) . . ? C46 C47 H47 120(3) . . ? C48 C47 H47 119(3) . . ? C53 C48 C49 117.5(4) . . ? C53 C48 C47 118.6(5) . . ? C49 C48 C47 123.8(5) . . ? C50 C49 C48 120.1(5) . . ? C50 C49 H49 124(4) . . ? C48 C49 H49 116(4) . . ? C49 C50 C51 119.0(5) . . ? C49 C50 H50 124(4) . . ? C51 C50 H50 117(4) . . ? N52 C51 C50 122.4(5) . . ? N52 C51 H51 118(4) . . ? C50 C51 H51 120(4) . . ? N52 C53 C48 122.2(4) . . ? N52 C53 C54 117.6(4) . . ? C48 C53 C54 120.2(4) . . ? N41 C54 C45 122.7(4) . . ? N41 C54 C53 117.7(4) . . ? C45 C54 C53 119.6(4) . . ? N61 C62 C63 122.9(5) . . ? N61 C62 H62 112(4) . . ? C63 C62 H62 125(4) . . ? C64 C63 C62 119.0(5) . . ? C64 C63 H63 121(4) . . ? C62 C63 H63 120(4) . . ? C63 C64 C65 120.2(5) . . ? C63 C64 H64 122(5) . . ? C65 C64 H64 118(5) . . ? C74 C65 C64 116.7(4) . . ? C74 C65 C66 118.9(4) . . ? C64 C65 C66 124.5(5) . . ? C67 C66 C65 120.9(5) . . ? C67 C66 H66 121(4) . . ? C65 C66 H66 118(4) . . ? C66 C67 C68 122.1(5) . . ? C66 C67 H67 125(4) . . ? C68 C67 H67 113(4) . . ? C69 C68 C73 117.4(4) . . ? C69 C68 C67 124.9(5) . . ? C73 C68 C67 117.7(5) . . ? C70 C69 C68 119.5(5) . . ? C70 C69 H69 117(4) . . ? C68 C69 H69 123(4) . . ? C69 C70 C71 119.7(5) . . ? C69 C70 H70 124(5) . . ? C71 C70 H70 116(5) . . ? N72 C71 C70 122.1(5) . . ? N72 C71 H71 114(4) . . ? C70 C71 H71 124(4) . . ? N72 C73 C68 122.9(4) . . ? N72 C73 C74 116.6(4) . . ? C68 C73 C74 120.4(4) . . ? N61 C74 C65 123.7(4) . . ? N61 C74 C73 116.3(4) . . ? C65 C74 C73 119.9(4) . . ? O23 Cl2 O24 111.2(5) . . ? O23 Cl2 O22 109.6(4) . . ? O24 Cl2 O22 107.0(3) . . ? O23 Cl2 O21 108.1(3) . . ? O24 Cl2 O21 110.1(4) . . ? O22 Cl2 O21 110.8(3) . . ? O34 Cl3 O33 110.9(3) . . ? O34 Cl3 O31 108.2(3) . . ? O33 Cl3 O31 110.7(3) . . ? O34 Cl3 O32 109.7(3) . . ? O33 Cl3 O32 108.9(2) . . ? O31 Cl3 O32 108.4(3) . . ? C80 N80 C81 124.2(14) . . ? C80 N80 C82 117.4(8) . . ? C81 N80 C82 118.5(13) . . ? O80 C80 N80 131.0(11) . . ? O80 C80 H80 119.5 . . ? N80 C80 H80 109.5 . . ? N80 C81 H81A 115.0 . . ? N80 C81 H81B 98.8 . . ? H81A C81 H81B 114.3 . . ? N80 C81 H81C 107.9 . . ? H81A C81 H81C 117.5 . . ? H81B C81 H81C 100.9 . . ? N80 C82 H82A 113.8 . . ? N80 C82 H82B 109.1 . . ? H82A C82 H82B 118.5 . . ? N80 C82 H82C 111.7 . . ? H82A C82 H82C 105.0 . . ? H82B C82 H82C 97.3 . . ? H1A O1 H1B 114.3 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.688 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.082 #===END OF DATA FOR 4 # 4.5 RESULTS FOR 5 data_fh9804 _database_code_CSD 164331 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ; [\m2-CO3{Zn(bipy)2}Zn(bipy)2(H2O)}](NO3)2*7H2O ; _chemical_formula_analytical ? _chemical_formula_sum 'C41 H48 N10 O17 Zn2' _chemical_formula_weight 1083.63 _chemical_melting_point ? _chemical_compound_source ? 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 P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.976(2) _cell_length_b 14.009(2) _cell_length_c 16.347(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.840(10) _cell_angle_gamma 90.00 _cell_volume 2392.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 78 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 13.21 _exptl_crystal_description fragment _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method ? _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 1.084 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.3096 _exptl_absorpt_correction_T_max 0.3599 ; North A C T, Phillips D C, Mathews F S, Acta Cryst. A24 (1968), 351-359. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Siemens P4' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.00 _diffrn_reflns_number 6784 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0748 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 27.00 _reflns_number_total 5872 _reflns_number_observed 3551 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'XSCAnS 2.20 (Siemens An. X-Ray Instr.,1996)' _computing_cell_refinement 'XSCAnS 2.20 (Siemens An. X-Ray Instr.,1996)' _computing_data_reduction 'XSCAnS 2.20 (Siemens An. X-Ray Instr.,1996)' _computing_structure_solution 'SHELXTL 5.03 (Siemens An. X-Ray Instr.,1995)' _computing_structure_refinement 'SHELXTL 5.03 (Siemens An. X-Ray Instr.,1995)' _computing_molecular_graphics 'SHELXTL 5.03 (Siemens An. X-Ray Instr.,1995)' _computing_publication_material 'SHELXTL 5.03 (Siemens An. X-Ray Instr.,1995)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The crystal under study proved to be a racemic twin with twin components of 0.55(4) and 0.45(4) (see Flack parameter). The compound crystallizes with 7 molecules of solvent water. No H atoms have been included for the solvent water molecules as well as for the water molecule coordinated to Zn1 (O11). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0672P)^2^+0.3261P] 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 'riding on preceding C atom' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.45(4) _refine_ls_number_reflns 5872 _refine_ls_number_parameters 632 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1178 _refine_ls_R_factor_obs 0.0606 _refine_ls_wR_factor_all 0.1508 _refine_ls_wR_factor_obs 0.1220 _refine_ls_goodness_of_fit_all 1.052 _refine_ls_goodness_of_fit_obs 1.135 _refine_ls_restrained_S_all 1.052 _refine_ls_restrained_S_obs 1.134 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zn1 Zn 0.52453(10) 0.09166(7) 0.19156(6) 0.0438(3) Uani 1 d . . N11 N 0.6964(7) 0.0700(7) 0.2970(4) 0.046(2) Uani 1 d . . N12 N 0.4854(8) -0.0319(7) 0.2581(5) 0.049(2) Uani 1 d . . N21 N 0.5751(8) -0.0007(7) 0.0999(5) 0.047(2) Uani 1 d . . N22 N 0.3556(7) 0.0928(8) 0.0818(4) 0.051(2) Uani 1 d . . O11 O 0.5945(6) 0.2098(5) 0.1385(4) 0.051(2) Uani 1 d . . O12 O 0.4399(6) 0.1795(5) 0.2584(4) 0.049(2) Uani 1 d . . C1 C 0.4546(9) 0.2677(7) 0.2739(5) 0.046(2) Uani 1 d . . C10 C 0.7985(10) 0.1285(11) 0.3173(6) 0.070(4) Uani 1 d . . H10 H 0.7979(10) 0.1804(11) 0.2817(6) 0.105 Uiso 1 calc R . C11 C 0.9040(10) 0.1153(12) 0.3884(6) 0.073(4) Uani 1 d . . H11 H 0.9725(10) 0.1576(12) 0.4002(6) 0.110 Uiso 1 calc R . C12 C 0.9069(11) 0.0385(13) 0.4418(7) 0.081(5) Uani 1 d . . H12 H 0.9771(11) 0.0273(13) 0.4898(7) 0.121 Uiso 1 calc R . C13 C 0.8020(10) -0.0212(9) 0.4214(6) 0.062(3) Uani 1 d . . H13 H 0.8008(10) -0.0740(9) 0.4555(6) 0.093 Uiso 1 calc R . C14 C 0.6965(10) -0.0019(9) 0.3487(6) 0.055(3) Uani 1 d . . C15 C 0.5802(9) -0.0606(10) 0.3237(6) 0.053(3) Uani 1 d . . C16 C 0.5689(12) -0.1449(11) 0.3693(7) 0.078(4) Uani 1 d . . H16 H 0.6359(12) -0.1657(11) 0.4161(7) 0.117 Uiso 1 calc R . C17 C 0.4583(14) -0.1935(12) 0.3427(9) 0.092(4) Uani 1 d . . H17 H 0.4481(14) -0.2474(12) 0.3731(9) 0.138 Uiso 1 calc R . C18 C 0.3593(12) -0.1661(11) 0.2718(7) 0.072(4) Uani 1 d . . H18 H 0.2839(12) -0.2010(11) 0.2522(7) 0.108 Uiso 1 calc R . C19 C 0.3794(11) -0.0830(9) 0.2316(7) 0.063(3) Uani 1 d . . H19 H 0.3148(11) -0.0622(9) 0.1834(7) 0.094 Uiso 1 calc R . C20 C 0.6832(9) -0.0474(10) 0.1153(6) 0.055(3) Uani 1 d . . H20 H 0.7462(9) -0.0387(10) 0.1677(6) 0.083 Uiso 1 calc R . C21 C 0.7068(11) -0.1107(9) 0.0542(7) 0.058(3) Uani 1 d . . H21 H 0.7846(11) -0.1422(9) 0.0648(7) 0.086 Uiso 1 calc R . C22 C 0.6100(12) -0.1235(10) -0.0211(7) 0.068(3) Uani 1 d . . H22 H 0.6212(12) -0.1663(10) -0.0617(7) 0.102 Uiso 1 calc R . C23 C 0.4985(11) -0.0752(9) -0.0377(6) 0.061(3) Uani 1 d . . H23 H 0.4342(11) -0.0833(9) -0.0897(6) 0.092 Uiso 1 calc R . C24 C 0.4817(10) -0.0139(8) 0.0234(6) 0.048(3) Uani 1 d . . C25 C 0.3678(10) 0.0415(9) 0.0124(6) 0.051(3) Uani 1 d . . C26 C 0.2718(11) 0.0515(10) -0.0689(6) 0.068(4) Uani 1 d . . H26 H 0.2812(11) 0.0204(10) -0.1168(6) 0.103 Uiso 1 calc R . C27 C 0.1673(10) 0.1060(12) -0.0764(6) 0.077(4) Uani 1 d . . H27 H 0.1030(10) 0.1098(12) -0.1289(6) 0.116 Uiso 1 calc R . C28 C 0.1554(9) 0.1578(10) -0.0040(7) 0.064(3) Uani 1 d . . H28 H 0.0857(9) 0.1974(10) -0.0082(7) 0.096 Uiso 1 calc R . C29 C 0.2523(10) 0.1466(10) 0.0729(7) 0.063(3) Uani 1 d . . H29 H 0.2449(10) 0.1784(10) 0.1211(7) 0.095 Uiso 1 calc R . Zn2 Zn 0.45890(11) 0.44685(8) 0.29933(6) 0.0490(4) Uani 1 d . . N31 N 0.2832(8) 0.4644(8) 0.1965(5) 0.053(3) Uani 1 d . . N32 N 0.5016(9) 0.5642(7) 0.2304(5) 0.056(3) Uani 1 d . . N41 N 0.4097(8) 0.5279(7) 0.3950(5) 0.050(2) Uani 1 d . . N42 N 0.6320(7) 0.4423(9) 0.4054(5) 0.052(2) Uani 1 d . . O21 O 0.3993(6) 0.3094(5) 0.3248(4) 0.049(2) Uani 1 d . . O22 O 0.5170(7) 0.3252(5) 0.2377(4) 0.055(2) Uani 1 d . . C30 C 0.1826(11) 0.4087(10) 0.1792(7) 0.065(3) Uani 1 d . . H30 H 0.1820(11) 0.3607(10) 0.2183(7) 0.097 Uiso 1 calc R . C31 C 0.0787(13) 0.4164(13) 0.1077(8) 0.088(5) Uani 1 d . . H31 H 0.0078(13) 0.3769(13) 0.0996(8) 0.132 Uiso 1 calc R . C32 C 0.0826(14) 0.4853(13) 0.0475(9) 0.091(5) Uani 1 d . . H32 H 0.0157(14) 0.4906(13) -0.0035(9) 0.136 Uiso 1 calc R . C33 C 0.1828(13) 0.5438(11) 0.0633(7) 0.078(4) Uani 1 d . . H33 H 0.1853(13) 0.5903(11) 0.0232(7) 0.118 Uiso 1 calc R . C34 C 0.2851(10) 0.5359(9) 0.1403(6) 0.054(3) Uani 1 d . . C35 C 0.4031(11) 0.5947(10) 0.1622(6) 0.061(3) Uani 1 d . . C36 C 0.4141(15) 0.6744(11) 0.1135(9) 0.093(4) Uani 1 d . . H36 H 0.3470(15) 0.6919(11) 0.0655(9) 0.140 Uiso 1 calc R . C37 C 0.5235(16) 0.7256(13) 0.1373(11) 0.110(6) Uani 1 d . . H37 H 0.5303(16) 0.7818(13) 0.1087(11) 0.165 Uiso 1 calc R . C38 C 0.6246(15) 0.6938(11) 0.2043(10) 0.095(5) Uani 1 d . . H38 H 0.7019(15) 0.7266(11) 0.2185(10) 0.143 Uiso 1 calc R . C39 C 0.6128(12) 0.6120(10) 0.2519(7) 0.070(4) Uani 1 d . . H39 H 0.6814(12) 0.5914(10) 0.2976(7) 0.104 Uiso 1 calc R . C40 C 0.3005(10) 0.5763(9) 0.3840(6) 0.056(3) Uani 1 d . . H40 H 0.2324(10) 0.5650(9) 0.3346(6) 0.084 Uiso 1 calc R . C41 C 0.2849(11) 0.6418(11) 0.4423(7) 0.069(4) Uani 1 d . . H41 H 0.2094(11) 0.6765(11) 0.4320(7) 0.104 Uiso 1 calc R . C42 C 0.3855(11) 0.6544(10) 0.5173(6) 0.067(4) Uani 1 d . . H42 H 0.3773(11) 0.6967(10) 0.5592(6) 0.101 Uiso 1 calc R . C43 C 0.4975(11) 0.6041(11) 0.5296(6) 0.063(3) Uani 1 d . . H43 H 0.5661(11) 0.6136(11) 0.5790(6) 0.095 Uiso 1 calc R . C44 C 0.5076(10) 0.5398(8) 0.4684(6) 0.050(3) Uani 1 d . . C45 C 0.6254(10) 0.4805(8) 0.4788(6) 0.048(3) Uani 1 d . . C46 C 0.7192(11) 0.4697(10) 0.5537(6) 0.066(3) Uani 1 d . . H46 H 0.7153(11) 0.5005(10) 0.6032(6) 0.099 Uiso 1 calc R . C47 C 0.8200(13) 0.4124(10) 0.5549(8) 0.078(4) Uani 1 d . . H47 H 0.8825(13) 0.4006(10) 0.6070(8) 0.118 Uiso 1 calc R . C48 C 0.8320(13) 0.3715(13) 0.4814(9) 0.089(5) Uani 1 d . . H48 H 0.9017(13) 0.3337(13) 0.4815(9) 0.133 Uiso 1 calc R . C49 C 0.7347(10) 0.3901(10) 0.4084(7) 0.066(4) Uani 1 d . . H49 H 0.7403(10) 0.3648(10) 0.3571(7) 0.100 Uiso 1 calc R . N3 N 0.9466(13) 0.4038(13) 0.2863(8) 0.095(4) Uani 1 d . . O31 O 0.9719(11) 0.3191(10) 0.2758(7) 0.138(4) Uani 1 d . . O32 O 0.8472(13) 0.4285(16) 0.2398(8) 0.229(10) Uani 1 d . . O33 O 1.0220(14) 0.4452(16) 0.3407(9) 0.177(7) Uani 1 d . . N4 N 1.0207(15) 0.8043(15) 0.2045(10) 0.124(5) Uani 1 d . . O41 O 1.0734(14) 0.7217(11) 0.2218(10) 0.177(7) Uani 1 d . . O42 O 0.9489(14) 0.8286(18) 0.2405(9) 0.199(9) Uani 1 d . . O43 O 1.0353(12) 0.8544(13) 0.1468(8) 0.157(6) Uani 1 d . . O1 O 0.8399(8) 0.2176(8) 0.1206(5) 0.101(3) Uani 1 d . . O2 O 1.2076(7) 0.1299(7) 0.2844(4) 0.088(3) Uani 1 d . . O3 O 0.9946(9) 0.0597(9) 0.1633(6) 0.117(4) Uani 1 d . . O4 O 0.7879(12) 0.6652(12) 0.4555(7) 0.157(5) Uani 1 d . . O5 O 1.2001(18) 0.8338(15) 0.0365(11) 0.274(10) Uani 1 d . . O6 O 0.2222(9) 0.2919(9) 0.4127(5) 0.120(4) Uani 1 d . . O7 O 0.9491(11) 0.6509(16) 0.3553(7) 0.184(7) 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 0.0516(6) 0.0395(7) 0.0371(5) 0.0004(5) 0.0090(5) -0.0028(6) N11 0.046(4) 0.050(7) 0.040(4) -0.005(4) 0.008(3) -0.003(4) N12 0.053(5) 0.042(6) 0.053(4) 0.001(4) 0.017(4) -0.004(5) N21 0.046(5) 0.044(6) 0.045(4) -0.001(4) 0.007(4) -0.007(4) N22 0.060(5) 0.043(5) 0.044(4) 0.007(5) 0.007(4) -0.007(6) O11 0.065(4) 0.046(4) 0.044(3) 0.004(3) 0.021(3) -0.011(4) O12 0.065(4) 0.042(4) 0.043(3) -0.006(3) 0.022(3) -0.010(3) C1 0.057(6) 0.040(5) 0.036(4) 0.005(4) 0.004(4) -0.010(5) C10 0.069(7) 0.090(11) 0.048(5) -0.006(6) 0.012(5) -0.004(7) C11 0.044(6) 0.110(13) 0.056(6) -0.010(8) 0.002(5) -0.009(7) C12 0.056(7) 0.120(13) 0.051(6) -0.006(8) -0.005(6) 0.029(8) C13 0.070(7) 0.059(7) 0.052(5) -0.001(5) 0.011(5) 0.025(6) C14 0.069(7) 0.055(7) 0.040(5) 0.001(5) 0.015(5) 0.017(6) C15 0.067(6) 0.050(7) 0.045(5) 0.004(6) 0.021(5) 0.004(6) C16 0.089(9) 0.078(10) 0.065(7) 0.033(7) 0.022(7) -0.010(8) C17 0.123(12) 0.059(10) 0.101(10) 0.015(8) 0.047(10) 0.008(10) C18 0.093(8) 0.068(9) 0.069(7) -0.013(7) 0.045(7) -0.022(7) C19 0.071(7) 0.062(9) 0.057(6) 0.002(6) 0.022(5) -0.015(7) C20 0.063(6) 0.055(7) 0.046(5) -0.001(6) 0.014(5) -0.028(7) C21 0.071(7) 0.041(7) 0.072(7) -0.013(6) 0.038(6) -0.008(6) C22 0.088(9) 0.055(8) 0.067(7) -0.017(6) 0.033(7) -0.014(7) C23 0.085(8) 0.049(8) 0.049(6) -0.012(5) 0.021(6) -0.007(7) C24 0.056(6) 0.047(7) 0.044(5) 0.008(5) 0.021(5) -0.006(5) C25 0.063(7) 0.052(7) 0.034(4) 0.003(5) 0.008(5) -0.023(6) C26 0.070(7) 0.086(9) 0.036(5) 0.002(5) -0.003(5) -0.008(7) C27 0.055(6) 0.108(11) 0.055(6) 0.010(7) -0.004(5) -0.010(8) C28 0.040(6) 0.056(7) 0.088(8) 0.016(7) 0.007(5) 0.011(5) C29 0.051(6) 0.059(8) 0.073(7) 0.014(6) 0.009(6) 0.004(6) Zn2 0.0673(8) 0.0416(8) 0.0397(5) -0.0022(5) 0.0190(5) -0.0070(6) N31 0.058(5) 0.053(7) 0.046(4) 0.005(5) 0.016(4) -0.003(5) N32 0.089(7) 0.045(6) 0.049(4) -0.002(4) 0.042(5) -0.002(5) N41 0.071(6) 0.039(5) 0.047(4) -0.005(4) 0.027(4) -0.007(5) N42 0.051(5) 0.057(6) 0.054(4) -0.009(5) 0.024(4) -0.011(6) O21 0.073(4) 0.040(4) 0.044(3) -0.003(3) 0.031(3) -0.008(3) O22 0.076(5) 0.033(4) 0.059(4) -0.004(4) 0.027(4) -0.011(4) C30 0.074(7) 0.063(8) 0.056(6) 0.001(6) 0.017(6) -0.002(7) C31 0.081(9) 0.110(14) 0.071(8) -0.006(9) 0.018(7) 0.009(9) C32 0.084(9) 0.103(13) 0.082(8) -0.003(9) 0.021(8) 0.030(9) C33 0.091(9) 0.089(10) 0.054(6) 0.014(7) 0.022(6) 0.028(8) C34 0.075(7) 0.048(7) 0.049(5) 0.006(5) 0.033(5) 0.017(6) C35 0.095(8) 0.046(7) 0.055(5) 0.016(6) 0.044(5) 0.031(8) C36 0.131(12) 0.061(9) 0.110(10) 0.023(9) 0.071(10) 0.017(10) C37 0.120(12) 0.086(13) 0.146(14) 0.061(11) 0.072(11) 0.000(11) C38 0.120(11) 0.062(10) 0.144(13) 0.001(9) 0.101(11) -0.017(9) C39 0.088(8) 0.056(9) 0.080(7) -0.021(7) 0.048(7) -0.017(7) C40 0.065(6) 0.049(8) 0.059(6) -0.013(6) 0.026(5) 0.003(6) C41 0.070(8) 0.081(10) 0.062(7) -0.009(7) 0.029(6) -0.003(7) C42 0.092(9) 0.070(9) 0.050(6) -0.011(6) 0.037(6) -0.015(8) C43 0.075(7) 0.075(9) 0.040(5) 0.006(6) 0.018(5) -0.001(8) C44 0.068(7) 0.044(6) 0.044(5) -0.001(5) 0.028(5) -0.019(6) C45 0.066(6) 0.033(6) 0.043(5) 0.003(4) 0.015(5) -0.008(5) C46 0.075(7) 0.074(9) 0.044(5) 0.002(6) 0.011(5) 0.004(7) C47 0.092(9) 0.063(8) 0.066(7) 0.022(6) 0.002(7) -0.002(7) C48 0.073(8) 0.091(11) 0.093(9) 0.012(9) 0.011(7) -0.018(8) C49 0.051(7) 0.080(10) 0.065(7) -0.006(7) 0.014(6) -0.012(7) N3 0.097(10) 0.114(11) 0.084(9) 0.046(8) 0.043(7) 0.016(9) O31 0.140(10) 0.111(9) 0.140(9) 0.025(8) 0.010(7) -0.042(9) O32 0.170(12) 0.372(28) 0.153(11) 0.147(15) 0.063(9) 0.120(16) O33 0.162(12) 0.234(20) 0.146(11) -0.050(13) 0.064(10) -0.055(14) N4 0.087(10) 0.149(16) 0.101(12) 0.009(11) -0.023(8) -0.039(12) O41 0.151(11) 0.121(11) 0.204(14) 0.033(11) -0.029(10) -0.048(10) O42 0.140(11) 0.315(27) 0.125(11) -0.010(15) 0.018(9) 0.017(16) O43 0.139(11) 0.195(15) 0.127(9) 0.035(11) 0.025(9) -0.021(10) O1 0.094(6) 0.129(8) 0.089(5) 0.020(6) 0.041(5) -0.010(6) O2 0.090(5) 0.102(7) 0.067(4) -0.002(5) 0.017(4) -0.029(5) O3 0.100(6) 0.126(10) 0.103(6) -0.017(7) 0.000(6) -0.013(7) O4 0.187(11) 0.178(14) 0.117(8) -0.015(9) 0.063(8) -0.014(10) O5 0.306(20) 0.191(18) 0.247(17) -0.018(15) -0.031(15) 0.094(16) O6 0.121(7) 0.169(11) 0.091(6) 0.050(7) 0.062(5) 0.013(8) O7 0.149(10) 0.273(20) 0.142(9) 0.037(12) 0.063(8) 0.043(12) _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 O12 2.048(7) . ? Zn1 O11 2.119(7) . ? Zn1 N22 2.149(7) . ? Zn1 N11 2.152(7) . ? Zn1 N12 2.155(9) . ? Zn1 N21 2.176(9) . ? N11 C14 1.314(13) . ? N11 C10 1.346(14) . ? N12 C15 1.309(12) . ? N12 C19 1.322(13) . ? N21 C20 1.310(13) . ? N21 C24 1.365(11) . ? N22 C29 1.332(14) . ? N22 C25 1.382(14) . ? O12 C1 1.261(11) . ? C1 O21 1.310(11) . ? C1 O22 1.309(10) . ? C1 Zn2 2.542(10) . ? C10 C11 1.379(13) . ? C11 C12 1.38(2) . ? C12 C13 1.38(2) . ? C13 C14 1.408(12) . ? C14 C15 1.47(2) . ? C15 C16 1.42(2) . ? C16 C17 1.34(2) . ? C17 C18 1.38(2) . ? C18 C19 1.39(2) . ? C20 C21 1.418(15) . ? C21 C22 1.369(14) . ? C22 C23 1.35(2) . ? C23 C24 1.372(14) . ? C24 C25 1.44(2) . ? C25 C26 1.428(12) . ? C26 C27 1.35(2) . ? C27 C28 1.43(2) . ? C28 C29 1.384(13) . ? Zn2 O21 2.116(7) . ? Zn2 N32 2.125(9) . ? Zn2 N41 2.132(8) . ? Zn2 N42 2.145(7) . ? Zn2 N31 2.149(8) . ? Zn2 O22 2.172(7) . ? N31 C30 1.310(14) . ? N31 C34 1.363(13) . ? N32 C39 1.340(13) . ? N32 C35 1.362(12) . ? N41 C40 1.340(12) . ? N41 C44 1.352(11) . ? N42 C49 1.332(15) . ? N42 C45 1.334(12) . ? C30 C31 1.364(14) . ? C31 C32 1.39(2) . ? C32 C33 1.33(2) . ? C33 C34 1.411(15) . ? C34 C35 1.48(2) . ? C35 C36 1.40(2) . ? C36 C37 1.35(2) . ? C37 C38 1.37(2) . ? C38 C39 1.41(2) . ? C40 C41 1.37(2) . ? C41 C42 1.387(14) . ? C42 C43 1.38(2) . ? C43 C44 1.376(15) . ? C44 C45 1.50(2) . ? C45 C46 1.346(13) . ? C46 C47 1.36(2) . ? C47 C48 1.37(2) . ? C48 C49 1.36(2) . ? N3 O33 1.17(2) . ? N3 O32 1.174(15) . ? N3 O31 1.24(2) . ? N4 O42 1.17(2) . ? N4 O43 1.22(2) . ? N4 O41 1.29(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 O12 Zn1 O11 91.7(3) . . ? O12 Zn1 N22 91.4(3) . . ? O11 Zn1 N22 88.9(3) . . ? O12 Zn1 N11 95.0(3) . . ? O11 Zn1 N11 95.7(3) . . ? N22 Zn1 N11 172.0(4) . . ? O12 Zn1 N12 91.2(3) . . ? O11 Zn1 N12 170.6(3) . . ? N22 Zn1 N12 99.9(3) . . ? N11 Zn1 N12 75.2(3) . . ? O12 Zn1 N21 167.9(3) . . ? O11 Zn1 N21 89.0(3) . . ? N22 Zn1 N21 76.5(3) . . ? N11 Zn1 N21 97.0(3) . . ? N12 Zn1 N21 90.1(3) . . ? C14 N11 C10 118.2(9) . . ? C14 N11 Zn1 116.8(7) . . ? C10 N11 Zn1 124.8(8) . . ? C15 N12 C19 120.1(11) . . ? C15 N12 Zn1 115.4(8) . . ? C19 N12 Zn1 124.2(7) . . ? C20 N21 C24 119.3(9) . . ? C20 N21 Zn1 124.9(7) . . ? C24 N21 Zn1 115.6(7) . . ? C29 N22 C25 119.8(8) . . ? C29 N22 Zn1 125.7(8) . . ? C25 N22 Zn1 113.9(7) . . ? C1 O12 Zn1 130.1(7) . . ? O12 C1 O21 120.6(9) . . ? O12 C1 O22 124.4(10) . . ? O21 C1 O22 114.9(9) . . ? O12 C1 Zn2 174.0(7) . . ? O21 C1 Zn2 56.2(5) . . ? O22 C1 Zn2 58.7(5) . . ? N11 C10 C11 123.1(13) . . ? C10 C11 C12 119.3(12) . . ? C13 C12 C11 117.7(9) . . ? C12 C13 C14 119.9(12) . . ? N11 C14 C13 121.9(11) . . ? N11 C14 C15 114.9(8) . . ? C13 C14 C15 123.2(11) . . ? N12 C15 C16 120.7(11) . . ? N12 C15 C14 117.4(11) . . ? C16 C15 C14 121.9(9) . . ? C17 C16 C15 117.8(12) . . ? C16 C17 C18 122.2(15) . . ? C17 C18 C19 115.7(12) . . ? N12 C19 C18 123.5(11) . . ? N21 C20 C21 121.8(9) . . ? C22 C21 C20 117.2(11) . . ? C23 C22 C21 121.4(11) . . ? C22 C23 C24 118.8(10) . . ? N21 C24 C23 121.4(10) . . ? N21 C24 C25 115.0(10) . . ? C23 C24 C25 123.6(9) . . ? N22 C25 C26 118.9(11) . . ? N22 C25 C24 118.5(8) . . ? C26 C25 C24 122.4(10) . . ? C27 C26 C25 120.2(11) . . ? C26 C27 C28 120.1(9) . . ? C29 C28 C27 117.1(11) . . ? N22 C29 C28 123.7(12) . . ? O21 Zn2 N32 160.1(3) . . ? O21 Zn2 N41 100.2(3) . . ? N32 Zn2 N41 97.1(3) . . ? O21 Zn2 N42 93.7(3) . . ? N32 Zn2 N42 99.6(4) . . ? N41 Zn2 N42 77.5(3) . . ? O21 Zn2 N31 90.1(3) . . ? N32 Zn2 N31 77.7(4) . . ? N41 Zn2 N31 98.3(3) . . ? N42 Zn2 N31 174.8(5) . . ? O21 Zn2 O22 62.0(2) . . ? N32 Zn2 O22 102.6(3) . . ? N41 Zn2 O22 159.1(3) . . ? N42 Zn2 O22 92.2(3) . . ? N31 Zn2 O22 92.7(3) . . ? O21 Zn2 C1 31.0(3) . . ? N32 Zn2 C1 132.3(3) . . ? N41 Zn2 C1 130.5(3) . . ? N42 Zn2 C1 94.1(4) . . ? N31 Zn2 C1 91.0(3) . . ? O22 Zn2 C1 31.0(2) . . ? C30 N31 C34 118.6(9) . . ? C30 N31 Zn2 126.5(8) . . ? C34 N31 Zn2 114.6(7) . . ? C39 N32 C35 119.2(11) . . ? C39 N32 Zn2 125.3(8) . . ? C35 N32 Zn2 115.4(8) . . ? C40 N41 C44 119.5(9) . . ? C40 N41 Zn2 126.0(6) . . ? C44 N41 Zn2 113.9(7) . . ? C49 N42 C45 117.8(9) . . ? C49 N42 Zn2 125.1(8) . . ? C45 N42 Zn2 115.9(7) . . ? C1 O21 Zn2 92.8(5) . . ? C1 O22 Zn2 90.3(6) . . ? N31 C30 C31 124.5(13) . . ? C30 C31 C32 117.5(14) . . ? C33 C32 C31 119.6(13) . . ? C32 C33 C34 120.6(13) . . ? N31 C34 C33 119.1(11) . . ? N31 C34 C35 116.0(9) . . ? C33 C34 C35 124.7(11) . . ? N32 C35 C36 122.1(13) . . ? N32 C35 C34 116.0(11) . . ? C36 C35 C34 121.9(11) . . ? C37 C36 C35 119.0(14) . . ? C36 C37 C38 119.2(15) . . ? C37 C38 C39 120.9(13) . . ? N32 C39 C38 119.3(12) . . ? N41 C40 C41 122.8(10) . . ? C40 C41 C42 117.7(12) . . ? C43 C42 C41 119.8(11) . . ? C44 C43 C42 119.7(9) . . ? N41 C44 C43 120.4(10) . . ? N41 C44 C45 117.1(9) . . ? C43 C44 C45 122.5(9) . . ? N42 C45 C46 122.4(11) . . ? N42 C45 C44 113.7(8) . . ? C46 C45 C44 123.9(10) . . ? C45 C46 C47 118.1(11) . . ? C46 C47 C48 121.9(11) . . ? C49 C48 C47 115.3(15) . . ? N42 C49 C48 124.4(13) . . ? O33 N3 O32 130.5(22) . . ? O33 N3 O31 116.3(17) . . ? O32 N3 O31 113.2(20) . . ? O42 N4 O43 119.2(25) . . ? O42 N4 O41 118.5(24) . . ? O43 N4 O41 122.0(23) . . ? _refine_diff_density_max 0.344 _refine_diff_density_min -0.712 _refine_diff_density_rms 0.076 #===END OF ALL DATA