# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name _publ_author_address 'Rui-Fang Jin' ; State Key Laboratory of Physical Chemistry of Solid Surface, and Department of Chemistry, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen 361005, China ; 'Shi-Yao Yang' ; State Key Laboratory of Physical Chemistry of Solid Surface, and Department of Chemistry, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen 361005, China ; 'Hui-Min Li' 'Li, Hui-Min' 'La-Sheng Long' . 'Rong-Bin Huang' ; State Key Laboratory of Physical Chemistry of Solid Surface, and Department of Chemistry, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen 361005, China ; 'Lansun Zheng' 'Huang, Rong-Bin' _publ_contact_author_name 'Dr Shi-Yao Yang' _publ_contact_author_address ; State Key Laboratory of Physical Chemistry of Solid Surface, and Department of Chemistry, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen 361005, China ; _publ_contact_author_email syyang@xmu.edu.cn _publ_contact_author_fax 86-592-2183047 _publ_contact_author_phone 86-592-2186175 _publ_contact_letter ; Please consider this CIFs for publication. I certify that this contibution is the original work of those listed as authors; that it has not been published before (in any language or medium) and is not being considered for publication elsewhere; that all authors concur with and are aware of the submission; that all workers involved in the study are listed as authors or given proper credit in the acknowledgements; that I have obtained permission for and acknowledged the source of any excerpts from other copyright works; and that to the best of my knowledge the paper contains no statements which are libellous, unlawful or in any way actionable. All coauthors have made significant scientific contributions to the work reported, including the ideas and their execution, and share responsibility and accountability for the results. ; _publ_section_title ; Effect of ionic radius on the assemblies of first row transition metal-5-tert-butylisophthalate-(2,2'-bipyridine/phenanthraline) coordination compounds ; _publ_section_abstract ; 18 coordination compounds have been synthesized. ; # Attachment '- revised cifs.cif' #============================================================================== data_MnBpy-[Mn3(tbip)3(bpy)2]n _database_code_depnum_ccdc_archive 'CCDC 835405' #TrackingRef '- revised cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H52 Mn3 N4 O12' _chemical_formula_sum 'C56 H52 Mn3 N4 O12' _chemical_formula_weight 1137.84 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 9.845(2) _cell_length_b 23.329(5) _cell_length_c 22.778(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.54(3) _cell_angle_gamma 90.00 _cell_volume 5125.5(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 18780 _cell_measurement_theta_min 6.04 _cell_measurement_theta_max 54.83 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.475 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2348 _exptl_absorpt_coefficient_mu 0.796 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7680 _exptl_absorpt_correction_T_max 0.8899 _exptl_absorpt_process_details 'Tompa_analytical (Rigaku Corporation, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Rigaku R-AXIS RAPID imaging plate' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41496 _diffrn_reflns_av_R_equivalents 0.0654 _diffrn_reflns_av_sigmaI/netI 0.0638 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.47 _reflns_number_total 11645 _reflns_number_gt 7455 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'PROCESS-AUTO (Rigaku Corporation,1998)' _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan (Molecular Structure Corporation & Rigaku Corporation, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. SADI is applied to the six C-C distances of the disordered tert-butyl. And ISOR is also applied to the six carbon atoms. ; _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^)+(0.0763P)^2^+2.9366P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11645 _refine_ls_number_parameters 715 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.0890 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1645 _refine_ls_wR_factor_gt 0.1121 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.105 _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 Mn1 Mn 0.15797(5) 0.35640(2) 0.25329(2) 0.01788(14) Uani 1 1 d . . . Mn2 Mn 0.22943(5) 0.25276(2) 0.35162(2) 0.01716(13) Uani 1 1 d . . . Mn3 Mn 0.30115(5) 0.14195(2) 0.44705(2) 0.01799(13) Uani 1 1 d . . . O1 O 0.1600(3) 0.28761(10) 0.19556(11) 0.0281(6) Uani 1 1 d . . . O2 O 0.2120(2) 0.21302(10) 0.25806(10) 0.0245(5) Uani 1 1 d . . . O3 O 0.2540(2) 0.21221(10) -0.05484(10) 0.0236(5) Uani 1 1 d . . . O4 O 0.3003(3) 0.28935(10) 0.00527(11) 0.0261(6) Uani 1 1 d . . . O5 O 0.0531(2) 0.31187(10) 0.32714(11) 0.0257(6) Uani 1 1 d . . . O6 O -0.0748(2) 0.36282(11) 0.25532(12) 0.0302(6) Uani 1 1 d . . . O7 O -0.5936(2) 0.37468(11) 0.25394(12) 0.0320(6) Uani 1 1 d . . . O8 O -0.6673(2) 0.32797(9) 0.32589(11) 0.0217(5) Uani 1 1 d . . . O9 O 0.4027(2) 0.19412(12) 0.37388(12) 0.0315(6) Uani 1 1 d . . . O10 O 0.5306(2) 0.14336(10) 0.44532(12) 0.0273(6) Uani 1 1 d . . . O11 O 1.0485(2) 0.13104(10) 0.44798(11) 0.0270(6) Uani 1 1 d . . . O12 O 1.1277(2) 0.17630(9) 0.37666(11) 0.0210(5) Uani 1 1 d . . . N1 N 0.1648(3) 0.44476(12) 0.29386(14) 0.0257(7) Uani 1 1 d . . . N2 N 0.1016(3) 0.41710(11) 0.17740(12) 0.0185(6) Uani 1 1 d . . . N4 N 0.2872(3) 0.05272(12) 0.40656(13) 0.0222(6) Uani 1 1 d . . . N13 N 0.3456(3) 0.08025(11) 0.52325(13) 0.0193(6) Uani 1 1 d . . . C1 C 0.2233(3) 0.20191(14) 0.15350(15) 0.0186(7) Uani 1 1 d . . . C2 C 0.2358(3) 0.23140(14) 0.10167(15) 0.0185(7) Uani 1 1 d . . . H2A H 0.2275 0.2720 0.1007 0.022 Uiso 1 1 calc R . . C3 C 0.2602(3) 0.20258(14) 0.05111(15) 0.0193(7) Uani 1 1 d . . . C4 C 0.2740(3) 0.14281(14) 0.05313(16) 0.0217(7) Uani 1 1 d . . . H4A H 0.2890 0.1229 0.0186 0.026 Uiso 1 1 calc R . . C5 C 0.2661(3) 0.11173(14) 0.10527(16) 0.0224(7) Uani 1 1 d . . . C6 C 0.2397(3) 0.14214(14) 0.15453(16) 0.0215(7) Uani 1 1 d . . . H6A H 0.2327 0.1217 0.1899 0.026 Uiso 1 1 calc R . . C7 C 0.1969(3) 0.23610(14) 0.20744(15) 0.0194(7) Uani 1 1 d . . . C8 C 0.2724(3) 0.23674(14) -0.00464(16) 0.0191(7) Uani 1 1 d . . . C9 C 0.2859(4) 0.04593(16) 0.10515(19) 0.0347(9) Uani 1 1 d . . . C10 C 0.1682(5) 0.01925(18) 0.0590(2) 0.0501(12) Uani 1 1 d . . . H10A H 0.0790 0.0288 0.0694 0.075 Uiso 1 1 calc R . . H10B H 0.1796 -0.0225 0.0589 0.075 Uiso 1 1 calc R . . H10C H 0.1708 0.0344 0.0191 0.075 Uiso 1 1 calc R . . C11 C 0.2846(6) 0.01916(17) 0.1663(2) 0.0504(13) Uani 1 1 d . . . H11A H 0.1950 0.0267 0.1774 0.076 Uiso 1 1 calc R . . H11B H 0.3590 0.0359 0.1965 0.076 Uiso 1 1 calc R . . H11C H 0.2987 -0.0223 0.1643 0.076 Uiso 1 1 calc R . . C12 C 0.4257(5) 0.03164(18) 0.0873(2) 0.0520(13) Uani 1 1 d . . . H12A H 0.5014 0.0501 0.1154 0.078 Uiso 1 1 calc R . . H12B H 0.4245 0.0457 0.0466 0.078 Uiso 1 1 calc R . . H12C H 0.4396 -0.0100 0.0885 0.078 Uiso 1 1 calc R . . C13 C -0.1778(3) 0.33608(13) 0.33806(16) 0.0188(7) Uani 1 1 d . . . C14 C -0.3114(3) 0.35031(14) 0.30814(16) 0.0207(7) Uani 1 1 d . . . H14A H -0.3266 0.3650 0.2685 0.025 Uiso 1 1 calc R . . C15 C -0.4225(3) 0.34278(14) 0.33684(15) 0.0183(7) Uani 1 1 d . . . C16 C -0.3975(3) 0.32661(14) 0.39718(16) 0.0220(7) Uani 1 1 d . . . H16A H -0.4736 0.3222 0.4167 0.026 Uiso 1 1 calc R . . C17 C -0.2627(3) 0.31680(15) 0.42955(15) 0.0212(7) Uani 1 1 d . A . C18 C -0.1546(3) 0.31993(14) 0.39787(16) 0.0215(7) Uani 1 1 d . . . H18A H -0.0630 0.3107 0.4179 0.026 Uiso 1 1 calc R . . C19 C -0.0610(3) 0.33720(14) 0.30482(16) 0.0203(7) Uani 1 1 d . . . C20 C -0.5685(3) 0.34935(14) 0.30268(16) 0.0210(7) Uani 1 1 d . . . C21 C -0.2359(4) 0.30552(16) 0.49667(17) 0.0299(8) Uani 1 1 d D . . C22 C -0.3464(15) 0.2655(5) 0.5129(8) 0.033(3) Uani 0.50 1 d PDU A 1 H22A H -0.4388 0.2798 0.4947 0.049 Uiso 0.50 1 calc PR A 1 H22B H -0.3367 0.2642 0.5565 0.049 Uiso 0.50 1 calc PR A 1 H22C H -0.3342 0.2269 0.4978 0.049 Uiso 0.50 1 calc PR A 1 C23 C -0.2553(13) 0.3659(4) 0.5244(5) 0.050(3) Uani 0.50 1 d PDU A 1 H23A H -0.3494 0.3799 0.5086 0.075 Uiso 0.50 1 calc PR A 1 H23B H -0.1878 0.3928 0.5137 0.075 Uiso 0.50 1 calc PR A 1 H23C H -0.2408 0.3626 0.5681 0.075 Uiso 0.50 1 calc PR A 1 C24 C -0.0911(9) 0.2848(5) 0.5219(5) 0.048(3) Uani 0.50 1 d PDU A 1 H24A H -0.0821 0.2765 0.5646 0.072 Uiso 0.50 1 calc PR A 1 H24B H -0.0243 0.3145 0.5166 0.072 Uiso 0.50 1 calc PR A 1 H24C H -0.0727 0.2499 0.5008 0.072 Uiso 0.50 1 calc PR A 1 C22' C -0.3635(14) 0.2835(6) 0.5177(8) 0.039(4) Uani 0.50 1 d PDU A 2 H22D H -0.4308 0.3147 0.5162 0.058 Uiso 0.50 1 calc PR A 2 H22E H -0.3366 0.2694 0.5589 0.058 Uiso 0.50 1 calc PR A 2 H22F H -0.4054 0.2522 0.4915 0.058 Uiso 0.50 1 calc PR A 2 C23' C -0.1779(14) 0.3585(5) 0.5303(6) 0.058(3) Uani 0.50 1 d PDU A 2 H23D H -0.2418 0.3906 0.5188 0.087 Uiso 0.50 1 calc PR A 2 H23E H -0.0878 0.3677 0.5206 0.087 Uiso 0.50 1 calc PR A 2 H23F H -0.1663 0.3516 0.5735 0.087 Uiso 0.50 1 calc PR A 2 C24' C -0.1252(10) 0.2562(4) 0.5139(5) 0.042(3) Uani 0.50 1 d PDU A 2 H24D H -0.1641 0.2200 0.4964 0.063 Uiso 0.50 1 calc PR A 2 H24E H -0.1006 0.2526 0.5576 0.063 Uiso 0.50 1 calc PR A 2 H24F H -0.0420 0.2656 0.4983 0.063 Uiso 0.50 1 calc PR A 2 C25 C 0.6374(3) 0.17614(13) 0.36559(16) 0.0192(7) Uani 1 1 d . . . C26 C 0.7711(3) 0.16307(14) 0.39615(16) 0.0214(7) Uani 1 1 d . . . H26A H 0.7865 0.1494 0.4362 0.026 Uiso 1 1 calc R . . C27 C 0.8813(3) 0.17027(13) 0.36732(16) 0.0194(7) Uani 1 1 d . . . C28 C 0.8577(3) 0.18777(14) 0.30736(16) 0.0208(7) Uani 1 1 d . . . H28A H 0.9343 0.1930 0.2884 0.025 Uiso 1 1 calc R . . C29 C 0.7240(3) 0.19772(14) 0.27497(16) 0.0212(7) Uani 1 1 d . . . C30 C 0.6145(3) 0.19341(14) 0.30608(17) 0.0244(8) Uani 1 1 d . . . H30A H 0.5230 0.2025 0.2859 0.029 Uiso 1 1 calc R . . C31 C 0.5169(3) 0.17124(14) 0.39700(17) 0.0220(7) Uani 1 1 d . . . C32 C 1.0272(3) 0.15878(14) 0.40024(16) 0.0201(7) Uani 1 1 d . . . C33 C 0.6937(4) 0.20886(16) 0.20709(16) 0.0279(8) Uani 1 1 d . . . C34 C 0.6197(4) 0.15501(17) 0.17752(18) 0.0347(9) Uani 1 1 d . . . H34A H 0.6765 0.1211 0.1907 0.052 Uiso 1 1 calc R . . H34B H 0.6058 0.1585 0.1339 0.052 Uiso 1 1 calc R . . H34C H 0.5296 0.1511 0.1892 0.052 Uiso 1 1 calc R . . C35 C 0.8281(4) 0.21912(19) 0.18443(18) 0.0367(10) Uani 1 1 d . . . H35A H 0.8865 0.1848 0.1916 0.055 Uiso 1 1 calc R . . H35B H 0.8778 0.2518 0.2058 0.055 Uiso 1 1 calc R . . H35C H 0.8059 0.2273 0.1414 0.055 Uiso 1 1 calc R . . C36 C 0.5980(4) 0.26097(18) 0.18963(18) 0.0372(10) Uani 1 1 d . . . H36A H 0.6492 0.2962 0.2027 0.056 Uiso 1 1 calc R . . H36B H 0.5179 0.2580 0.2090 0.056 Uiso 1 1 calc R . . H36C H 0.5660 0.2618 0.1460 0.056 Uiso 1 1 calc R . . C37 C 0.1865(4) 0.45510(16) 0.35241(16) 0.0305(9) Uani 1 1 d . . . H37A H 0.2216 0.4249 0.3791 0.037 Uiso 1 1 calc R . . C38 C 0.1607(4) 0.50733(17) 0.37643(19) 0.0388(10) Uani 1 1 d . . . H38A H 0.1780 0.5132 0.4185 0.047 Uiso 1 1 calc R . . C39 C 0.1088(5) 0.55093(17) 0.3371(2) 0.0426(11) Uani 1 1 d . . . H39A H 0.0878 0.5872 0.3521 0.051 Uiso 1 1 calc R . . C40 C 0.0875(4) 0.54182(15) 0.27597(19) 0.0335(9) Uani 1 1 d . . . H40A H 0.0529 0.5717 0.2487 0.040 Uiso 1 1 calc R . . C41 C 0.1178(3) 0.48777(14) 0.25502(17) 0.0244(8) Uani 1 1 d . . . C42 C 0.0961(3) 0.47331(14) 0.19046(16) 0.0218(7) Uani 1 1 d . . . C43 C 0.0692(4) 0.51434(15) 0.14533(17) 0.0273(8) Uani 1 1 d . . . H43A H 0.0696 0.5539 0.1551 0.033 Uiso 1 1 calc R . . C44 C 0.0417(4) 0.49699(16) 0.08588(17) 0.0284(8) Uani 1 1 d . . . H44A H 0.0218 0.5245 0.0546 0.034 Uiso 1 1 calc R . . C45 C 0.0438(3) 0.43896(15) 0.07270(17) 0.0261(8) Uani 1 1 d . . . H45A H 0.0240 0.4259 0.0324 0.031 Uiso 1 1 calc R . . C46 C 0.0754(3) 0.40043(15) 0.12007(15) 0.0219(7) Uani 1 1 d . . . H46A H 0.0786 0.3607 0.1114 0.026 Uiso 1 1 calc R . . C47 C 0.3761(3) 0.09664(16) 0.58092(16) 0.0243(8) Uani 1 1 d . . . H47A H 0.3817 0.1365 0.5897 0.029 Uiso 1 1 calc R . . C48 C 0.3998(4) 0.05811(16) 0.62839(17) 0.0286(8) Uani 1 1 d . . . H48A H 0.4211 0.0712 0.6687 0.034 Uiso 1 1 calc R . . C49 C 0.3915(4) -0.00005(16) 0.61517(18) 0.0316(9) Uani 1 1 d . . . H49A H 0.4071 -0.0276 0.6465 0.038 Uiso 1 1 calc R . . C50 C 0.3599(4) -0.01777(16) 0.55558(17) 0.0273(8) Uani 1 1 d . . . H50A H 0.3534 -0.0574 0.5458 0.033 Uiso 1 1 calc R . . C51 C 0.3383(3) 0.02358(14) 0.51071(16) 0.0208(7) Uani 1 1 d . . . C52 C 0.3060(3) 0.00812(14) 0.44575(17) 0.0221(7) Uani 1 1 d . . . C53 C 0.2940(4) -0.04864(16) 0.42546(19) 0.0308(9) Uani 1 1 d . . . H53A H 0.3072 -0.0795 0.4532 0.037 Uiso 1 1 calc R . . C54 C 0.2624(4) -0.05944(17) 0.36392(19) 0.0327(9) Uani 1 1 d . . . H54A H 0.2532 -0.0977 0.3493 0.039 Uiso 1 1 calc R . . C55 C 0.2448(4) -0.01391(18) 0.3249(2) 0.0359(10) Uani 1 1 d . . . H55A H 0.2232 -0.0201 0.2828 0.043 Uiso 1 1 calc R . . C56 C 0.2591(4) 0.04143(16) 0.34798(16) 0.0270(8) Uani 1 1 d . . . H56A H 0.2483 0.0727 0.3207 0.032 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0166(2) 0.0224(3) 0.0156(3) 0.0024(2) 0.0055(2) 0.0025(2) Mn2 0.0151(2) 0.0222(3) 0.0153(3) 0.0030(2) 0.00583(19) 0.00102(19) Mn3 0.0164(2) 0.0207(3) 0.0177(3) 0.0016(2) 0.0054(2) 0.00166(19) O1 0.0412(15) 0.0263(13) 0.0193(14) 0.0002(10) 0.0118(11) 0.0067(11) O2 0.0337(13) 0.0299(13) 0.0110(12) 0.0019(10) 0.0074(10) 0.0015(11) O3 0.0337(13) 0.0284(12) 0.0103(12) -0.0040(10) 0.0078(10) -0.0022(11) O4 0.0378(14) 0.0251(12) 0.0166(13) 0.0036(10) 0.0088(11) -0.0049(11) O5 0.0174(11) 0.0342(13) 0.0269(15) 0.0005(11) 0.0074(10) 0.0038(10) O6 0.0207(12) 0.0450(15) 0.0277(15) 0.0085(12) 0.0112(11) 0.0012(11) O7 0.0215(12) 0.0462(15) 0.0282(15) 0.0177(13) 0.0045(11) 0.0039(12) O8 0.0164(11) 0.0275(12) 0.0223(13) 0.0041(10) 0.0063(10) -0.0023(10) O9 0.0165(12) 0.0496(16) 0.0286(15) -0.0028(12) 0.0050(10) 0.0069(11) O10 0.0225(12) 0.0271(13) 0.0361(16) 0.0053(11) 0.0148(11) 0.0021(10) O11 0.0240(12) 0.0328(13) 0.0242(14) 0.0108(11) 0.0048(10) 0.0030(11) O12 0.0136(10) 0.0267(12) 0.0243(14) 0.0013(10) 0.0079(9) -0.0013(9) N1 0.0263(15) 0.0292(15) 0.0223(17) 0.0033(13) 0.0066(13) 0.0011(13) N2 0.0149(13) 0.0262(14) 0.0173(15) 0.0051(12) 0.0097(11) 0.0026(11) N4 0.0181(13) 0.0274(15) 0.0216(17) 0.0023(12) 0.0055(12) 0.0023(12) N13 0.0159(13) 0.0237(14) 0.0203(16) 0.0041(12) 0.0085(11) 0.0009(11) C1 0.0202(16) 0.0244(16) 0.0115(17) -0.0042(13) 0.0040(13) 0.0000(13) C2 0.0212(16) 0.0204(15) 0.0159(17) -0.0004(13) 0.0084(13) -0.0001(13) C3 0.0185(16) 0.0243(16) 0.0168(18) 0.0014(13) 0.0075(13) -0.0020(13) C4 0.0232(17) 0.0247(17) 0.0180(18) -0.0034(14) 0.0062(14) -0.0009(14) C5 0.0251(17) 0.0225(16) 0.0209(19) -0.0017(14) 0.0075(14) -0.0027(14) C6 0.0188(16) 0.0268(17) 0.0204(19) -0.0009(14) 0.0074(14) -0.0008(14) C7 0.0191(16) 0.0245(16) 0.0157(17) -0.0029(14) 0.0063(13) -0.0018(13) C8 0.0158(15) 0.0221(16) 0.0209(19) 0.0031(14) 0.0073(13) 0.0001(13) C9 0.047(2) 0.0261(19) 0.035(2) -0.0044(17) 0.0191(19) -0.0020(18) C10 0.071(3) 0.031(2) 0.050(3) -0.009(2) 0.018(3) -0.016(2) C11 0.089(4) 0.027(2) 0.039(3) 0.0041(19) 0.020(3) 0.009(2) C12 0.064(3) 0.029(2) 0.071(4) 0.001(2) 0.032(3) 0.013(2) C13 0.0154(15) 0.0200(15) 0.0218(19) 0.0005(14) 0.0053(13) -0.0014(13) C14 0.0174(15) 0.0252(17) 0.0204(19) 0.0032(14) 0.0057(13) -0.0016(13) C15 0.0134(14) 0.0225(16) 0.0194(18) -0.0005(14) 0.0043(13) 0.0005(13) C16 0.0180(16) 0.0272(17) 0.0233(19) 0.0008(15) 0.0100(14) -0.0025(14) C17 0.0196(16) 0.0302(17) 0.0136(17) -0.0013(14) 0.0027(13) -0.0028(14) C18 0.0139(15) 0.0277(17) 0.0228(19) 0.0006(14) 0.0033(13) -0.0013(14) C19 0.0175(16) 0.0256(17) 0.0191(18) 0.0018(14) 0.0069(13) -0.0004(14) C20 0.0166(15) 0.0253(17) 0.0226(19) 0.0017(14) 0.0074(14) 0.0004(13) C21 0.0267(18) 0.044(2) 0.019(2) -0.0007(17) 0.0039(15) -0.0080(17) C22 0.041(6) 0.031(5) 0.026(5) -0.001(5) 0.003(4) -0.015(5) C23 0.079(7) 0.048(5) 0.022(5) -0.001(4) 0.010(5) -0.023(5) C24 0.025(4) 0.098(7) 0.020(5) 0.020(5) 0.000(3) -0.005(5) C22' 0.032(5) 0.061(8) 0.023(6) 0.011(6) 0.004(4) -0.007(5) C23' 0.082(7) 0.056(6) 0.029(5) -0.008(4) -0.005(6) -0.022(6) C24' 0.042(5) 0.066(6) 0.017(4) -0.003(4) 0.003(4) 0.014(5) C25 0.0155(15) 0.0214(16) 0.0218(19) 0.0014(14) 0.0066(13) 0.0005(13) C26 0.0211(16) 0.0219(16) 0.0215(19) 0.0030(14) 0.0051(14) 0.0011(14) C27 0.0157(15) 0.0183(15) 0.0246(19) -0.0001(14) 0.0048(13) 0.0002(13) C28 0.0189(16) 0.0224(16) 0.0229(19) 0.0022(14) 0.0082(14) 0.0008(13) C29 0.0183(16) 0.0226(16) 0.0232(19) -0.0009(14) 0.0050(14) -0.0001(13) C30 0.0162(16) 0.0256(17) 0.030(2) -0.0027(15) 0.0017(14) -0.0018(14) C31 0.0176(16) 0.0219(16) 0.027(2) -0.0026(15) 0.0061(14) -0.0018(14) C32 0.0197(16) 0.0222(16) 0.0200(19) 0.0009(14) 0.0077(14) 0.0007(13) C33 0.0277(18) 0.038(2) 0.0175(19) -0.0024(16) 0.0027(15) 0.0003(16) C34 0.0293(19) 0.047(2) 0.027(2) -0.0109(18) 0.0048(17) -0.0025(18) C35 0.030(2) 0.062(3) 0.019(2) 0.0009(19) 0.0060(16) -0.0057(19) C36 0.042(2) 0.048(2) 0.020(2) 0.0010(18) 0.0015(17) 0.0126(19) C37 0.043(2) 0.037(2) 0.0106(18) -0.0043(15) 0.0033(16) -0.0004(18) C38 0.050(2) 0.042(2) 0.025(2) -0.0028(18) 0.0105(19) -0.010(2) C39 0.060(3) 0.033(2) 0.038(3) -0.0117(19) 0.017(2) -0.004(2) C40 0.047(2) 0.0240(18) 0.031(2) -0.0023(16) 0.0111(18) -0.0013(17) C41 0.0216(17) 0.0260(17) 0.028(2) -0.0006(15) 0.0096(15) -0.0031(14) C42 0.0199(16) 0.0222(16) 0.025(2) 0.0036(14) 0.0093(14) 0.0017(14) C43 0.0288(18) 0.0275(18) 0.028(2) 0.0052(16) 0.0118(16) 0.0030(15) C44 0.0288(19) 0.0340(19) 0.025(2) 0.0129(16) 0.0118(16) 0.0058(16) C45 0.0239(17) 0.037(2) 0.0184(19) 0.0079(15) 0.0077(14) 0.0084(15) C46 0.0257(17) 0.0281(17) 0.0132(17) -0.0012(14) 0.0072(14) 0.0024(14) C47 0.0206(16) 0.0326(18) 0.0210(19) -0.0025(15) 0.0077(14) 0.0030(15) C48 0.0257(18) 0.045(2) 0.0177(19) 0.0096(16) 0.0093(15) 0.0075(16) C49 0.0292(19) 0.036(2) 0.032(2) 0.0145(17) 0.0111(17) 0.0072(17) C50 0.0268(18) 0.0291(18) 0.029(2) 0.0037(16) 0.0116(16) 0.0041(15) C51 0.0142(15) 0.0211(16) 0.029(2) 0.0033(14) 0.0084(14) 0.0019(13) C52 0.0149(15) 0.0240(17) 0.029(2) -0.0016(15) 0.0082(14) -0.0003(13) C53 0.0235(18) 0.0309(19) 0.040(2) -0.0061(17) 0.0115(16) 0.0012(15) C54 0.0255(18) 0.036(2) 0.038(2) -0.0127(18) 0.0095(17) -0.0014(16) C55 0.0236(19) 0.049(2) 0.035(2) -0.011(2) 0.0051(17) 0.0031(18) C56 0.0277(18) 0.038(2) 0.0148(19) -0.0038(15) 0.0019(14) 0.0016(16) _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 Mn1 O1 2.077(2) . ? Mn1 N2 2.218(3) . ? Mn1 O8 2.235(2) 1_655 ? Mn1 N1 2.255(3) . ? Mn1 O6 2.306(2) . ? Mn1 O5 2.381(3) . ? Mn1 O7 2.480(3) 1_655 ? Mn2 O9 2.166(2) . ? Mn2 O8 2.167(2) 1_655 ? Mn2 O12 2.177(2) 1_455 ? Mn2 O5 2.200(2) . ? Mn2 O3 2.249(2) 4_566 ? Mn2 O2 2.299(2) . ? Mn3 O4 2.081(2) 4_566 ? Mn3 N13 2.230(3) . ? Mn3 O12 2.243(2) 1_455 ? Mn3 O10 2.268(2) . ? Mn3 N4 2.270(3) . ? Mn3 O9 2.434(3) . ? Mn3 O11 2.505(2) 1_455 ? O1 C7 1.269(4) . ? O2 C7 1.254(4) . ? O3 C8 1.259(4) . ? O3 Mn2 2.249(2) 4_565 ? O4 C8 1.268(4) . ? O4 Mn3 2.081(2) 4_565 ? O5 C19 1.281(4) . ? O6 C19 1.259(4) . ? O7 C20 1.238(4) . ? O7 Mn1 2.480(2) 1_455 ? O8 C20 1.296(4) . ? O8 Mn2 2.167(2) 1_455 ? O8 Mn1 2.235(2) 1_455 ? O9 C31 1.260(4) . ? O10 C31 1.262(4) . ? O11 C32 1.247(4) . ? O11 Mn3 2.505(2) 1_655 ? O12 C32 1.284(4) . ? O12 Mn2 2.177(2) 1_655 ? O12 Mn3 2.243(2) 1_655 ? N1 C37 1.330(5) . ? N1 C41 1.356(4) . ? N2 C46 1.337(4) . ? N2 C42 1.348(4) . ? N4 C56 1.334(4) . ? N4 C52 1.359(4) . ? N13 C47 1.343(4) . ? N13 C51 1.351(4) . ? C1 C2 1.393(5) . ? C1 C6 1.403(4) . ? C1 C7 1.530(5) . ? C2 C3 1.396(5) . ? C2 H2A 0.9500 . ? C3 C4 1.401(4) . ? C3 C8 1.524(5) . ? C4 C5 1.407(5) . ? C4 H4A 0.9500 . ? C5 C6 1.395(5) . ? C5 C9 1.547(5) . ? C6 H6A 0.9500 . ? C9 C11 1.530(6) . ? C9 C10 1.533(6) . ? C9 C12 1.547(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C18 1.388(5) . ? C13 C14 1.396(4) . ? C13 C19 1.498(5) . ? C14 C15 1.393(5) . ? C14 H14A 0.9500 . ? C15 C16 1.399(5) . ? C15 C20 1.499(4) . ? C16 C17 1.402(4) . ? C16 H16A 0.9500 . ? C17 C18 1.402(5) . ? C17 C21 1.521(5) . ? C18 H18A 0.9500 . ? C21 C24 1.506(9) . ? C21 C23' 1.504(9) . ? C21 C22' 1.521(11) . ? C21 C22 1.534(10) . ? C21 C23 1.570(10) . ? C21 C24' 1.579(9) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C22' H22D 0.9800 . ? C22' H22E 0.9800 . ? C22' H22F 0.9800 . ? C23' H23D 0.9800 . ? C23' H23E 0.9800 . ? C23' H23F 0.9800 . ? C24' H24D 0.9800 . ? C24' H24E 0.9800 . ? C24' H24F 0.9800 . ? C25 C30 1.389(5) . ? C25 C26 1.394(4) . ? C25 C31 1.508(5) . ? C26 C27 1.386(5) . ? C26 H26A 0.9500 . ? C27 C28 1.400(5) . ? C27 C32 1.506(4) . ? C28 C29 1.394(4) . ? C28 H28A 0.9500 . ? C29 C30 1.406(5) . ? C29 C33 1.537(5) . ? C30 H30A 0.9500 . ? C33 C35 1.532(5) . ? C33 C34 1.538(5) . ? C33 C36 1.541(5) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.380(5) . ? C37 H37A 0.9500 . ? C38 C39 1.384(6) . ? C38 H38A 0.9500 . ? C39 C40 1.382(6) . ? C39 H39A 0.9500 . ? C40 C41 1.401(5) . ? C40 H40A 0.9500 . ? C41 C42 1.482(5) . ? C42 C43 1.391(5) . ? C43 C44 1.387(5) . ? C43 H43A 0.9500 . ? C44 C45 1.388(5) . ? C44 H44A 0.9500 . ? C45 C46 1.391(5) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C47 C48 1.389(5) . ? C47 H47A 0.9500 . ? C48 C49 1.389(5) . ? C48 H48A 0.9500 . ? C49 C50 1.393(5) . ? C49 H49A 0.9500 . ? C50 C51 1.390(5) . ? C50 H50A 0.9500 . ? C51 C52 1.494(5) . ? C52 C53 1.400(5) . ? C53 C54 1.397(6) . ? C53 H53A 0.9500 . ? C54 C55 1.374(6) . ? C54 H54A 0.9500 . ? C55 C56 1.390(5) . ? C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 N2 91.87(10) . . ? O1 Mn1 O8 97.79(9) . 1_655 ? N2 Mn1 O8 143.30(9) . 1_655 ? O1 Mn1 N1 164.27(11) . . ? N2 Mn1 N1 73.61(11) . . ? O8 Mn1 N1 90.72(9) 1_655 . ? O1 Mn1 O6 101.45(10) . . ? N2 Mn1 O6 83.07(10) . . ? O8 Mn1 O6 128.70(9) 1_655 . ? N1 Mn1 O6 83.14(10) . . ? O1 Mn1 O5 99.83(9) . . ? N2 Mn1 O5 138.84(9) . . ? O8 Mn1 O5 74.11(8) 1_655 . ? N1 Mn1 O5 95.21(10) . . ? O6 Mn1 O5 56.02(9) . . ? O1 Mn1 O7 90.12(10) . 1_655 ? N2 Mn1 O7 89.29(9) . 1_655 ? O8 Mn1 O7 55.55(8) 1_655 1_655 ? N1 Mn1 O7 83.79(10) . 1_655 ? O6 Mn1 O7 166.30(9) . 1_655 ? O5 Mn1 O7 129.60(8) . 1_655 ? O9 Mn2 O8 100.63(9) . 1_655 ? O9 Mn2 O12 78.65(9) . 1_455 ? O8 Mn2 O12 179.03(9) 1_655 1_455 ? O9 Mn2 O5 178.87(10) . . ? O8 Mn2 O5 79.22(9) 1_655 . ? O12 Mn2 O5 101.48(9) 1_455 . ? O9 Mn2 O3 94.44(10) . 4_566 ? O8 Mn2 O3 89.70(9) 1_655 4_566 ? O12 Mn2 O3 91.00(9) 1_455 4_566 ? O5 Mn2 O3 86.68(9) . 4_566 ? O9 Mn2 O2 82.62(9) . . ? O8 Mn2 O2 91.60(9) 1_655 . ? O12 Mn2 O2 87.67(9) 1_455 . ? O5 Mn2 O2 96.26(9) . . ? O3 Mn2 O2 176.96(8) 4_566 . ? O4 Mn3 N13 91.51(10) 4_566 . ? O4 Mn3 O12 94.64(9) 4_566 1_455 ? N13 Mn3 O12 142.17(9) . 1_455 ? O4 Mn3 O10 97.51(10) 4_566 . ? N13 Mn3 O10 88.95(10) . . ? O12 Mn3 O10 126.93(9) 1_455 . ? O4 Mn3 N4 163.24(10) 4_566 . ? N13 Mn3 N4 73.19(10) . . ? O12 Mn3 N4 93.53(9) 1_455 . ? O10 Mn3 N4 89.19(9) . . ? O4 Mn3 O9 96.07(9) 4_566 . ? N13 Mn3 O9 144.30(9) . . ? O12 Mn3 O9 71.95(8) 1_455 . ? O10 Mn3 O9 55.51(9) . . ? N4 Mn3 O9 100.37(10) . . ? O4 Mn3 O11 86.70(9) 4_566 1_455 ? N13 Mn3 O11 88.20(9) . 1_455 ? O12 Mn3 O11 55.06(8) 1_455 1_455 ? O10 Mn3 O11 174.97(8) . 1_455 ? N4 Mn3 O11 86.02(9) . 1_455 ? O9 Mn3 O11 126.96(8) . 1_455 ? C7 O1 Mn1 129.4(2) . . ? C7 O2 Mn2 130.7(2) . . ? C8 O3 Mn2 131.6(2) . 4_565 ? C8 O4 Mn3 131.3(2) . 4_565 ? C19 O5 Mn2 167.1(2) . . ? C19 O5 Mn1 89.3(2) . . ? Mn2 O5 Mn1 91.19(9) . . ? C19 O6 Mn1 93.3(2) . . ? C20 O7 Mn1 86.7(2) . 1_455 ? C20 O8 Mn2 148.5(2) . 1_455 ? C20 O8 Mn1 96.5(2) . 1_455 ? Mn2 O8 Mn1 96.15(8) 1_455 1_455 ? C31 O9 Mn2 163.7(2) . . ? C31 O9 Mn3 87.5(2) . . ? Mn2 O9 Mn3 93.66(9) . . ? C31 O10 Mn3 95.1(2) . . ? C32 O11 Mn3 86.2(2) . 1_655 ? C32 O12 Mn2 143.5(2) . 1_655 ? C32 O12 Mn3 97.3(2) . 1_655 ? Mn2 O12 Mn3 98.97(8) 1_655 1_655 ? C37 N1 C41 119.0(3) . . ? C37 N1 Mn1 124.2(2) . . ? C41 N1 Mn1 115.5(2) . . ? C46 N2 C42 119.3(3) . . ? C46 N2 Mn1 123.0(2) . . ? C42 N2 Mn1 117.6(2) . . ? C56 N4 C52 118.7(3) . . ? C56 N4 Mn3 124.8(2) . . ? C52 N4 Mn3 116.5(2) . . ? C47 N13 C51 118.5(3) . . ? C47 N13 Mn3 123.2(2) . . ? C51 N13 Mn3 118.2(2) . . ? C2 C1 C6 118.4(3) . . ? C2 C1 C7 118.8(3) . . ? C6 C1 C7 122.8(3) . . ? C1 C2 C3 121.4(3) . . ? C1 C2 H2A 119.3 . . ? C3 C2 H2A 119.3 . . ? C2 C3 C4 118.9(3) . . ? C2 C3 C8 119.4(3) . . ? C4 C3 C8 121.7(3) . . ? C3 C4 C5 121.3(3) . . ? C3 C4 H4A 119.3 . . ? C5 C4 H4A 119.3 . . ? C6 C5 C4 117.9(3) . . ? C6 C5 C9 123.4(3) . . ? C4 C5 C9 118.8(3) . . ? C5 C6 C1 122.1(3) . . ? C5 C6 H6A 119.0 . . ? C1 C6 H6A 119.0 . . ? O2 C7 O1 125.4(3) . . ? O2 C7 C1 120.4(3) . . ? O1 C7 C1 114.2(3) . . ? O3 C8 O4 126.1(3) . . ? O3 C8 C3 119.9(3) . . ? O4 C8 C3 114.1(3) . . ? C11 C9 C10 108.4(4) . . ? C11 C9 C5 112.3(3) . . ? C10 C9 C5 109.0(3) . . ? C11 C9 C12 108.8(4) . . ? C10 C9 C12 108.8(4) . . ? C5 C9 C12 109.5(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 119.9(3) . . ? C18 C13 C19 120.6(3) . . ? C14 C13 C19 119.5(3) . . ? C15 C14 C13 119.5(3) . . ? C15 C14 H14A 120.2 . . ? C13 C14 H14A 120.2 . . ? C14 C15 C16 119.7(3) . . ? C14 C15 C20 120.3(3) . . ? C16 C15 C20 120.0(3) . . ? C15 C16 C17 121.5(3) . . ? C15 C16 H16A 119.3 . . ? C17 C16 H16A 119.3 . . ? C16 C17 C18 117.2(3) . . ? C16 C17 C21 120.8(3) . . ? C18 C17 C21 122.0(3) . . ? C13 C18 C17 121.8(3) . . ? C13 C18 H18A 119.1 . . ? C17 C18 H18A 119.1 . . ? O6 C19 O5 120.2(3) . . ? O6 C19 C13 120.3(3) . . ? O5 C19 C13 119.5(3) . . ? O7 C20 O8 121.2(3) . . ? O7 C20 C15 120.8(3) . . ? O8 C20 C15 118.0(3) . . ? C24 C21 C23' 80.5(7) . . ? C24 C21 C22' 123.4(8) . . ? C23' C21 C22' 111.7(9) . . ? C24 C21 C17 113.5(5) . . ? C23' C21 C17 110.0(6) . . ? C22' C21 C17 112.8(7) . . ? C24 C21 C22 112.0(8) . . ? C23' C21 C22 126.3(9) . . ? C17 C21 C22 111.0(8) . . ? C24 C21 C23 108.4(7) . . ? C22' C21 C23 90.1(7) . . ? C17 C21 C23 103.8(5) . . ? C22 C21 C23 107.5(7) . . ? C23' C21 C24' 107.3(7) . . ? C22' C21 C24' 104.4(8) . . ? C17 C21 C24' 110.3(5) . . ? C22 C21 C24' 89.1(7) . . ? C23 C21 C24' 133.4(6) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? C21 C22' H22D 109.5 . . ? C21 C22' H22E 109.5 . . ? H22D C22' H22E 109.5 . . ? C21 C22' H22F 109.5 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? C21 C23' H23D 109.5 . . ? C21 C23' H23E 109.5 . . ? H23D C23' H23E 109.5 . . ? C21 C23' H23F 109.5 . . ? H23D C23' H23F 109.5 . . ? H23E C23' H23F 109.5 . . ? C21 C24' H24D 109.5 . . ? C21 C24' H24E 109.5 . . ? H24D C24' H24E 109.5 . . ? C21 C24' H24F 109.5 . . ? H24D C24' H24F 109.5 . . ? H24E C24' H24F 109.5 . . ? C30 C25 C26 120.2(3) . . ? C30 C25 C31 119.7(3) . . ? C26 C25 C31 120.0(3) . . ? C27 C26 C25 119.1(3) . . ? C27 C26 H26A 120.4 . . ? C25 C26 H26A 120.4 . . ? C26 C27 C28 120.3(3) . . ? C26 C27 C32 120.1(3) . . ? C28 C27 C32 119.6(3) . . ? C29 C28 C27 121.3(3) . . ? C29 C28 H28A 119.3 . . ? C27 C28 H28A 119.3 . . ? C28 C29 C30 117.3(3) . . ? C28 C29 C33 122.2(3) . . ? C30 C29 C33 120.3(3) . . ? C25 C30 C29 121.4(3) . . ? C25 C30 H30A 119.3 . . ? C29 C30 H30A 119.3 . . ? O9 C31 O10 120.9(3) . . ? O9 C31 C25 119.3(3) . . ? O10 C31 C25 119.7(3) . . ? O11 C32 O12 121.4(3) . . ? O11 C32 C27 120.3(3) . . ? O12 C32 C27 118.3(3) . . ? C35 C33 C29 111.0(3) . . ? C35 C33 C34 110.2(3) . . ? C29 C33 C34 106.4(3) . . ? C35 C33 C36 108.3(3) . . ? C29 C33 C36 112.2(3) . . ? C34 C33 C36 108.6(3) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N1 C37 C38 123.5(4) . . ? N1 C37 H37A 118.2 . . ? C38 C37 H37A 118.2 . . ? C37 C38 C39 117.7(4) . . ? C37 C38 H38A 121.1 . . ? C39 C38 H38A 121.1 . . ? C40 C39 C38 120.1(4) . . ? C40 C39 H39A 120.0 . . ? C38 C39 H39A 120.0 . . ? C39 C40 C41 118.8(4) . . ? C39 C40 H40A 120.6 . . ? C41 C40 H40A 120.6 . . ? N1 C41 C40 120.8(4) . . ? N1 C41 C42 116.2(3) . . ? C40 C41 C42 123.0(3) . . ? N2 C42 C43 121.1(3) . . ? N2 C42 C41 115.9(3) . . ? C43 C42 C41 123.0(3) . . ? C44 C43 C42 119.5(3) . . ? C44 C43 H43A 120.3 . . ? C42 C43 H43A 120.3 . . ? C43 C44 C45 119.2(3) . . ? C43 C44 H44A 120.4 . . ? C45 C44 H44A 120.4 . . ? C44 C45 C46 118.2(3) . . ? C44 C45 H45A 120.9 . . ? C46 C45 H45A 120.9 . . ? N2 C46 C45 122.6(3) . . ? N2 C46 H46A 118.7 . . ? C45 C46 H46A 118.7 . . ? N13 C47 C48 123.1(3) . . ? N13 C47 H47A 118.4 . . ? C48 C47 H47A 118.4 . . ? C47 C48 C49 118.0(4) . . ? C47 C48 H48A 121.0 . . ? C49 C48 H48A 121.0 . . ? C48 C49 C50 119.6(3) . . ? C48 C49 H49A 120.2 . . ? C50 C49 H49A 120.2 . . ? C51 C50 C49 118.8(3) . . ? C51 C50 H50A 120.6 . . ? C49 C50 H50A 120.6 . . ? N13 C51 C50 122.0(3) . . ? N13 C51 C52 115.9(3) . . ? C50 C51 C52 122.1(3) . . ? N4 C52 C53 121.1(3) . . ? N4 C52 C51 116.1(3) . . ? C53 C52 C51 122.9(3) . . ? C54 C53 C52 119.3(4) . . ? C54 C53 H53A 120.4 . . ? C52 C53 H53A 120.4 . . ? C55 C54 C53 118.9(4) . . ? C55 C54 H54A 120.5 . . ? C53 C54 H54A 120.5 . . ? C54 C55 C56 118.9(4) . . ? C54 C55 H55A 120.6 . . ? C56 C55 H55A 120.6 . . ? N4 C56 C55 123.2(4) . . ? N4 C56 H56A 118.4 . . ? C55 C56 H56A 118.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Mn1 O1 C7 173.4(3) . . . . ? O8 Mn1 O1 C7 28.9(3) 1_655 . . . ? N1 Mn1 O1 C7 151.1(4) . . . . ? O6 Mn1 O1 C7 -103.3(3) . . . . ? O5 Mn1 O1 C7 -46.2(3) . . . . ? O7 Mn1 O1 C7 84.1(3) 1_655 . . . ? O9 Mn2 O2 C7 -133.0(3) . . . . ? O8 Mn2 O2 C7 -32.5(3) 1_655 . . . ? O12 Mn2 O2 C7 148.1(3) 1_455 . . . ? O5 Mn2 O2 C7 46.8(3) . . . . ? O8 Mn2 O5 C19 124.0(11) 1_655 . . . ? O12 Mn2 O5 C19 -55.3(11) 1_455 . . . ? O3 Mn2 O5 C19 -145.7(11) 4_566 . . . ? O2 Mn2 O5 C19 33.6(11) . . . . ? O8 Mn2 O5 Mn1 31.90(8) 1_655 . . . ? O12 Mn2 O5 Mn1 -147.43(8) 1_455 . . . ? O3 Mn2 O5 Mn1 122.23(9) 4_566 . . . ? O2 Mn2 O5 Mn1 -58.54(9) . . . . ? O1 Mn1 O5 C19 -103.3(2) . . . . ? N2 Mn1 O5 C19 1.1(3) . . . . ? O8 Mn1 O5 C19 161.4(2) 1_655 . . . ? N1 Mn1 O5 C19 72.1(2) . . . . ? O6 Mn1 O5 C19 -6.02(19) . . . . ? O7 Mn1 O5 C19 158.34(19) 1_655 . . . ? O1 Mn1 O5 Mn2 63.82(10) . . . . ? N2 Mn1 O5 Mn2 168.21(12) . . . . ? O8 Mn1 O5 Mn2 -31.55(8) 1_655 . . . ? N1 Mn1 O5 Mn2 -120.82(10) . . . . ? O6 Mn1 O5 Mn2 161.07(13) . . . . ? O7 Mn1 O5 Mn2 -34.57(14) 1_655 . . . ? O1 Mn1 O6 C19 100.3(2) . . . . ? N2 Mn1 O6 C19 -169.1(2) . . . . ? O8 Mn1 O6 C19 -9.5(3) 1_655 . . . ? N1 Mn1 O6 C19 -94.9(2) . . . . ? O5 Mn1 O6 C19 6.13(19) . . . . ? O7 Mn1 O6 C19 -112.6(4) 1_655 . . . ? O8 Mn2 O9 C31 57.4(9) 1_655 . . . ? O12 Mn2 O9 C31 -123.2(9) 1_455 . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.741 _refine_diff_density_min -0.995 _refine_diff_density_rms 0.121 #============================================================================== data_MnPhen-{[Mn(tbip)(phen)].2H2O}n _database_code_depnum_ccdc_archive 'CCDC 835406' #TrackingRef '- revised cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H20 Mn N2 O4, H2 O' _chemical_formula_sum 'C24 H22 Mn N2 O5' _chemical_formula_weight 473.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.7774(18) _cell_length_b 9.6971(6) _cell_length_c 18.9936(12) _cell_angle_alpha 90.00 _cell_angle_beta 125.855(1) _cell_angle_gamma 90.00 _cell_volume 4295.9(5) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3139 _cell_measurement_theta_min 2.2745 _cell_measurement_theta_max 22.6930 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960 _exptl_absorpt_coefficient_mu 0.654 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8914 _exptl_absorpt_correction_T_max 0.9198 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18365 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_sigmaI/netI 0.0665 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 28.77 _reflns_number_total 5143 _reflns_number_gt 4079 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0653P)^2^+8.8179P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5143 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0862 _refine_ls_R_factor_gt 0.0642 _refine_ls_wR_factor_ref 0.1493 _refine_ls_wR_factor_gt 0.1376 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.448887(19) 0.32433(5) 0.62205(3) 0.01689(14) Uani 1 1 d . . . O1 O 0.53145(10) 0.4073(3) 0.70742(15) 0.0305(6) Uani 1 1 d . . . O2 O 0.60032(9) 0.4398(2) 0.84681(14) 0.0242(5) Uani 1 1 d . . . O3 O 0.62821(10) 0.6936(2) 0.52090(14) 0.0300(5) Uani 1 1 d . . . O4 O 0.55519(10) 0.5621(2) 0.48228(14) 0.0294(5) Uani 1 1 d . . . N1 N 0.49793(11) 0.1439(3) 0.61732(17) 0.0228(6) Uani 1 1 d . . . N2 N 0.41709(11) 0.1275(3) 0.64685(17) 0.0223(6) Uani 1 1 d . . . C1 C 0.61754(12) 0.5076(3) 0.74341(19) 0.0178(6) Uani 1 1 d . . . C2 C 0.59484(12) 0.5258(3) 0.65617(19) 0.0178(6) Uani 1 1 d . . . H2A H 0.5567 0.4975 0.6123 0.021 Uiso 1 1 calc R . . C3 C 0.62812(13) 0.5854(3) 0.63352(19) 0.0184(6) Uani 1 1 d . . . C4 C 0.68419(13) 0.6264(3) 0.6981(2) 0.0203(6) Uani 1 1 d . . . H4A H 0.7062 0.6698 0.6818 0.024 Uiso 1 1 calc R . . C5 C 0.70862(13) 0.6053(3) 0.7856(2) 0.0205(6) Uani 1 1 d . . . C6 C 0.67407(13) 0.5459(3) 0.80676(19) 0.0196(6) Uani 1 1 d . . . H6A H 0.6896 0.5312 0.8662 0.023 Uiso 1 1 calc R . . C7 C 0.58048(13) 0.4469(3) 0.7676(2) 0.0197(6) Uani 1 1 d . . . C8 C 0.60251(13) 0.6136(3) 0.5399(2) 0.0214(6) Uani 1 1 d . . . C9 C 0.77077(13) 0.6441(3) 0.8577(2) 0.0249(7) Uani 1 1 d . . . C10 C 0.79977(15) 0.7185(4) 0.8224(3) 0.0404(9) Uani 1 1 d . . . H10A H 0.8390 0.7432 0.8706 0.061 Uiso 1 1 calc R . . H10B H 0.7782 0.8024 0.7919 0.061 Uiso 1 1 calc R . . H10C H 0.8007 0.6578 0.7820 0.061 Uiso 1 1 calc R . . C11 C 0.77240(16) 0.7401(5) 0.9233(3) 0.0528(12) Uani 1 1 d . . . H11A H 0.8123 0.7624 0.9701 0.079 Uiso 1 1 calc R . . H11B H 0.7544 0.6941 0.9476 0.079 Uiso 1 1 calc R . . H11C H 0.7515 0.8252 0.8940 0.079 Uiso 1 1 calc R . . C12 C 0.80399(15) 0.5121(4) 0.9045(2) 0.0380(9) Uani 1 1 d . . . H12A H 0.8434 0.5358 0.9526 0.057 Uiso 1 1 calc R . . H12B H 0.8044 0.4516 0.8636 0.057 Uiso 1 1 calc R . . H12C H 0.7854 0.4645 0.9273 0.057 Uiso 1 1 calc R . . C13 C 0.53915(15) 0.1524(4) 0.6059(2) 0.0302(8) Uani 1 1 d . . . H13A H 0.5511 0.2411 0.6013 0.036 Uiso 1 1 calc R . . C14 C 0.56567(16) 0.0370(4) 0.6005(3) 0.0405(9) Uani 1 1 d . . . H14A H 0.5956 0.0478 0.5936 0.049 Uiso 1 1 calc R . . C15 C 0.54856(16) -0.0908(4) 0.6050(3) 0.0428(10) Uani 1 1 d . . . H15A H 0.5661 -0.1700 0.6006 0.051 Uiso 1 1 calc R . . C16 C 0.50499(15) -0.1059(4) 0.6164(2) 0.0343(8) Uani 1 1 d . . . C17 C 0.48296(18) -0.2364(4) 0.6194(3) 0.0463(10) Uani 1 1 d . . . H17A H 0.4973 -0.3188 0.6117 0.056 Uiso 1 1 calc R . . C18 C 0.44204(18) -0.2435(4) 0.6331(3) 0.0455(10) Uani 1 1 d . . . H18A H 0.4283 -0.3314 0.6353 0.055 Uiso 1 1 calc R . . C19 C 0.41887(16) -0.1224(4) 0.6444(2) 0.0333(8) Uani 1 1 d . . . C20 C 0.37611(17) -0.1250(4) 0.6586(3) 0.0403(9) Uani 1 1 d . . . H20A H 0.3621 -0.2106 0.6632 0.048 Uiso 1 1 calc R . . C21 C 0.35518(17) -0.0062(4) 0.6655(3) 0.0418(10) Uani 1 1 d . . . H21A H 0.3262 -0.0073 0.6749 0.050 Uiso 1 1 calc R . . C22 C 0.37614(15) 0.1189(4) 0.6588(2) 0.0311(8) Uani 1 1 d . . . H22A H 0.3604 0.2020 0.6630 0.037 Uiso 1 1 calc R . . C23 C 0.43785(13) 0.0082(3) 0.6388(2) 0.0226(6) Uani 1 1 d . . . C24 C 0.48157(13) 0.0165(3) 0.6242(2) 0.0231(7) Uani 1 1 d . . . O1W O 0.7214(3) 0.6421(8) 0.5135(5) 0.072(2) Uani 0.60 1 d P . . H1WA H 0.6871 0.6520 0.4953 0.108 Uiso 0.60 1 calc PR . . H1WB H 0.7129 0.6965 0.4724 0.108 Uiso 0.60 1 d PR . . O2W O 0.7559(4) 0.8372(13) 0.4308(7) 0.077(3) Uani 0.40 1 d P . . H2WA H 0.7756 0.8082 0.4144 0.115 Uiso 0.40 1 calc PR . . H2WB H 0.7508 0.7900 0.4647 0.115 Uiso 0.40 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0205(2) 0.0171(2) 0.0175(2) -0.00147(18) 0.0136(2) -0.00205(18) O1 0.0277(12) 0.0403(14) 0.0270(12) -0.0092(11) 0.0179(11) -0.0158(11) O2 0.0315(12) 0.0266(12) 0.0215(11) 0.0015(9) 0.0195(10) -0.0037(10) O3 0.0297(12) 0.0404(14) 0.0219(12) 0.0061(10) 0.0163(10) -0.0075(11) O4 0.0310(13) 0.0344(13) 0.0185(11) 0.0022(10) 0.0122(10) -0.0091(10) N1 0.0219(13) 0.0203(13) 0.0244(14) -0.0045(10) 0.0126(12) -0.0031(10) N2 0.0244(14) 0.0220(13) 0.0218(13) -0.0015(11) 0.0142(12) -0.0038(11) C1 0.0211(15) 0.0140(14) 0.0207(15) 0.0007(11) 0.0136(13) 0.0006(11) C2 0.0155(14) 0.0167(14) 0.0203(15) 0.0000(11) 0.0100(12) 0.0010(11) C3 0.0215(15) 0.0171(14) 0.0191(14) 0.0003(11) 0.0132(13) 0.0031(12) C4 0.0212(15) 0.0188(14) 0.0265(16) -0.0002(12) 0.0171(14) -0.0006(12) C5 0.0201(15) 0.0199(15) 0.0233(15) -0.0004(12) 0.0136(13) 0.0024(12) C6 0.0234(15) 0.0209(15) 0.0160(14) 0.0024(11) 0.0124(13) 0.0030(12) C7 0.0260(16) 0.0145(14) 0.0225(15) -0.0030(12) 0.0163(14) -0.0027(12) C8 0.0248(16) 0.0203(15) 0.0223(15) -0.0003(12) 0.0155(14) 0.0047(13) C9 0.0181(15) 0.0305(18) 0.0249(16) -0.0019(13) 0.0120(14) -0.0002(13) C10 0.0209(17) 0.047(2) 0.041(2) 0.0095(18) 0.0113(17) -0.0070(16) C11 0.027(2) 0.073(3) 0.043(2) -0.031(2) 0.0122(19) -0.006(2) C12 0.0213(17) 0.046(2) 0.038(2) 0.0131(17) 0.0124(16) 0.0028(16) C13 0.0303(18) 0.0280(18) 0.039(2) -0.0077(15) 0.0240(17) -0.0043(14) C14 0.0275(19) 0.051(2) 0.045(2) -0.0109(19) 0.0226(18) 0.0005(17) C15 0.035(2) 0.036(2) 0.049(2) -0.0066(18) 0.021(2) 0.0138(18) C16 0.0296(18) 0.0291(19) 0.0326(19) -0.0006(15) 0.0118(16) 0.0064(15) C17 0.048(2) 0.0229(19) 0.053(3) 0.0008(18) 0.021(2) 0.0096(17) C18 0.054(3) 0.0175(18) 0.056(3) 0.0070(17) 0.027(2) 0.0017(17) C19 0.036(2) 0.0271(18) 0.0278(18) 0.0040(14) 0.0138(16) -0.0029(15) C20 0.046(2) 0.034(2) 0.040(2) 0.0023(17) 0.025(2) -0.0161(18) C21 0.041(2) 0.047(2) 0.049(2) -0.0040(19) 0.033(2) -0.0154(18) C22 0.0333(19) 0.0338(19) 0.0348(19) -0.0059(15) 0.0248(17) -0.0079(15) C23 0.0239(15) 0.0229(16) 0.0172(14) 0.0003(12) 0.0098(13) -0.0035(13) C24 0.0203(15) 0.0225(16) 0.0200(15) -0.0034(12) 0.0082(13) -0.0010(12) O1W 0.061(5) 0.097(5) 0.078(5) 0.000(5) 0.051(4) -0.010(4) O2W 0.049(6) 0.111(9) 0.073(7) 0.019(7) 0.037(6) 0.008(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O1 2.100(2) . ? Mn1 O2 2.142(2) 2_656 ? Mn1 O4 2.209(2) 5_666 ? Mn1 N2 2.282(3) . ? Mn1 N1 2.283(3) . ? Mn1 O3 2.295(2) 5_666 ? Mn1 C8 2.586(3) 5_666 ? O1 C7 1.247(4) . ? O2 C7 1.260(4) . ? O2 Mn1 2.142(2) 2_656 ? O3 C8 1.262(4) . ? O3 Mn1 2.295(2) 5_666 ? O4 C8 1.247(4) . ? O4 Mn1 2.209(2) 5_666 ? N1 C13 1.327(4) . ? N1 C24 1.356(4) . ? N2 C22 1.327(4) . ? N2 C23 1.350(4) . ? C1 C2 1.391(4) . ? C1 C6 1.392(4) . ? C1 C7 1.507(4) . ? C2 C3 1.385(4) . ? C2 H2A 0.9500 . ? C3 C4 1.395(4) . ? C3 C8 1.498(4) . ? C4 C5 1.390(4) . ? C4 H4A 0.9500 . ? C5 C6 1.396(4) . ? C5 C9 1.532(4) . ? C6 H6A 0.9500 . ? C8 Mn1 2.586(3) 5_666 ? C9 C10 1.523(5) . ? C9 C12 1.532(5) . ? C9 C11 1.534(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.392(5) . ? C13 H13A 0.9500 . ? C14 C15 1.355(6) . ? C14 H14A 0.9500 . ? C15 C16 1.398(5) . ? C15 H15A 0.9500 . ? C16 C24 1.415(5) . ? C16 C17 1.432(6) . ? C17 C18 1.348(6) . ? C17 H17A 0.9500 . ? C18 C19 1.428(5) . ? C18 H18A 0.9500 . ? C19 C20 1.405(5) . ? C19 C23 1.408(5) . ? C20 C21 1.342(6) . ? C20 H20A 0.9500 . ? C21 C22 1.393(5) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C24 1.440(5) . ? O1W O2W 0.882(10) 7_666 ? O1W H1WA 0.8400 . ? O1W H1WB 0.8501 . ? O2W O1W 0.882(10) 7_666 ? O2W H2WA 0.8400 . ? O2W H2WB 0.8698 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 O2 102.62(9) . 2_656 ? O1 Mn1 O4 86.75(9) . 5_666 ? O2 Mn1 O4 106.90(9) 2_656 5_666 ? O1 Mn1 N2 124.77(9) . . ? O2 Mn1 N2 88.31(9) 2_656 . ? O4 Mn1 N2 141.72(9) 5_666 . ? O1 Mn1 N1 83.00(9) . . ? O2 Mn1 N1 159.29(9) 2_656 . ? O4 Mn1 N1 93.21(9) 5_666 . ? N2 Mn1 N1 72.47(10) . . ? O1 Mn1 O3 144.60(9) . 5_666 ? O2 Mn1 O3 91.66(9) 2_656 5_666 ? O4 Mn1 O3 57.99(8) 5_666 5_666 ? N2 Mn1 O3 87.37(9) . 5_666 ? N1 Mn1 O3 94.98(9) . 5_666 ? O1 Mn1 C8 115.44(10) . 5_666 ? O2 Mn1 C8 101.36(9) 2_656 5_666 ? O4 Mn1 C8 28.81(9) 5_666 5_666 ? N2 Mn1 C8 114.91(10) . 5_666 ? N1 Mn1 C8 93.87(9) . 5_666 ? O3 Mn1 C8 29.20(9) 5_666 5_666 ? C7 O1 Mn1 170.7(2) . . ? C7 O2 Mn1 116.60(19) . 2_656 ? C8 O3 Mn1 88.26(18) . 5_666 ? C8 O4 Mn1 92.59(19) . 5_666 ? C13 N1 C24 117.8(3) . . ? C13 N1 Mn1 126.2(2) . . ? C24 N1 Mn1 115.9(2) . . ? C22 N2 C23 117.5(3) . . ? C22 N2 Mn1 126.2(2) . . ? C23 N2 Mn1 115.8(2) . . ? C2 C1 C6 119.4(3) . . ? C2 C1 C7 119.4(3) . . ? C6 C1 C7 121.2(3) . . ? C3 C2 C1 119.7(3) . . ? C3 C2 H2A 120.2 . . ? C1 C2 H2A 120.2 . . ? C2 C3 C4 120.0(3) . . ? C2 C3 C8 119.7(3) . . ? C4 C3 C8 120.2(3) . . ? C5 C4 C3 121.6(3) . . ? C5 C4 H4A 119.2 . . ? C3 C4 H4A 119.2 . . ? C4 C5 C6 117.3(3) . . ? C4 C5 C9 122.7(3) . . ? C6 C5 C9 120.0(3) . . ? C1 C6 C5 122.0(3) . . ? C1 C6 H6A 119.0 . . ? C5 C6 H6A 119.0 . . ? O1 C7 O2 123.7(3) . . ? O1 C7 C1 117.6(3) . . ? O2 C7 C1 118.6(3) . . ? O4 C8 O3 121.1(3) . . ? O4 C8 C3 119.6(3) . . ? O3 C8 C3 119.3(3) . . ? O4 C8 Mn1 58.60(16) . 5_666 ? O3 C8 Mn1 62.54(16) . 5_666 ? C3 C8 Mn1 174.7(2) . 5_666 ? C10 C9 C5 112.1(3) . . ? C10 C9 C12 109.6(3) . . ? C5 C9 C12 108.6(3) . . ? C10 C9 C11 107.8(3) . . ? C5 C9 C11 109.8(3) . . ? C12 C9 C11 108.9(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C14 122.9(3) . . ? N1 C13 H13A 118.5 . . ? C14 C13 H13A 118.5 . . ? C15 C14 C13 119.7(3) . . ? C15 C14 H14A 120.2 . . ? C13 C14 H14A 120.2 . . ? C14 C15 C16 119.8(3) . . ? C14 C15 H15A 120.1 . . ? C16 C15 H15A 120.1 . . ? C15 C16 C24 117.0(3) . . ? C15 C16 C17 123.8(4) . . ? C24 C16 C17 119.2(3) . . ? C18 C17 C16 120.7(4) . . ? C18 C17 H17A 119.6 . . ? C16 C17 H17A 119.6 . . ? C17 C18 C19 121.6(4) . . ? C17 C18 H18A 119.2 . . ? C19 C18 H18A 119.2 . . ? C20 C19 C23 116.9(3) . . ? C20 C19 C18 123.5(3) . . ? C23 C19 C18 119.5(3) . . ? C21 C20 C19 119.8(3) . . ? C21 C20 H20A 120.1 . . ? C19 C20 H20A 120.1 . . ? C20 C21 C22 119.7(3) . . ? C20 C21 H21A 120.2 . . ? C22 C21 H21A 120.2 . . ? N2 C22 C21 123.0(3) . . ? N2 C22 H22A 118.5 . . ? C21 C22 H22A 118.5 . . ? N2 C23 C19 123.0(3) . . ? N2 C23 C24 117.9(3) . . ? C19 C23 C24 119.1(3) . . ? N1 C24 C16 122.7(3) . . ? N1 C24 C23 117.5(3) . . ? C16 C24 C23 119.8(3) . . ? O2W O1W H1WA 109.5 7_666 . ? O2W O1W H1WB 125.0 7_666 . ? H1WA O1W H1WB 85.1 . . ? O1W O2W H2WA 109.5 7_666 . ? O1W O2W H2WB 63.8 7_666 . ? H2WA O2W H2WB 122.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Mn1 N1 C13 -47.5(3) . . . . ? O2 Mn1 N1 C13 -154.8(3) 2_656 . . . ? O4 Mn1 N1 C13 38.8(3) 5_666 . . . ? N2 Mn1 N1 C13 -177.4(3) . . . . ? O3 Mn1 N1 C13 97.0(3) 5_666 . . . ? C8 Mn1 N1 C13 67.7(3) 5_666 . . . ? O1 Mn1 N1 C24 134.7(2) . . . . ? O2 Mn1 N1 C24 27.4(4) 2_656 . . . ? O4 Mn1 N1 C24 -139.0(2) 5_666 . . . ? N2 Mn1 N1 C24 4.8(2) . . . . ? O3 Mn1 N1 C24 -80.9(2) 5_666 . . . ? C8 Mn1 N1 C24 -110.1(2) 5_666 . . . ? O1 Mn1 N2 C22 114.2(3) . . . . ? O2 Mn1 N2 C22 10.0(3) 2_656 . . . ? O4 Mn1 N2 C22 -105.6(3) 5_666 . . . ? N1 Mn1 N2 C22 -177.8(3) . . . . ? O3 Mn1 N2 C22 -81.8(3) 5_666 . . . ? C8 Mn1 N2 C22 -91.8(3) 5_666 . . . ? O1 Mn1 N2 C23 -73.6(2) . . . . ? O2 Mn1 N2 C23 -177.8(2) 2_656 . . . ? O4 Mn1 N2 C23 66.6(3) 5_666 . . . ? N1 Mn1 N2 C23 -5.6(2) . . . . ? O3 Mn1 N2 C23 90.4(2) 5_666 . . . ? C8 Mn1 N2 C23 80.4(2) 5_666 . . . ? C6 C1 C2 C3 -1.9(4) . . . . ? C7 C1 C2 C3 178.1(3) . . . . ? C1 C2 C3 C4 0.3(4) . . . . ? C1 C2 C3 C8 -176.0(3) . . . . ? C2 C3 C4 C5 1.9(5) . . . . ? C8 C3 C4 C5 178.1(3) . . . . ? C3 C4 C5 C6 -2.3(4) . . . . ? C3 C4 C5 C9 177.6(3) . . . . ? C2 C1 C6 C5 1.5(4) . . . . ? C7 C1 C6 C5 -178.5(3) . . . . ? C4 C5 C6 C1 0.6(4) . . . . ? C9 C5 C6 C1 -179.3(3) . . . . ? Mn1 O2 C7 O1 9.9(4) 2_656 . . . ? Mn1 O2 C7 C1 -170.67(19) 2_656 . . . ? C2 C1 C7 O1 4.3(4) . . . . ? C6 C1 C7 O1 -175.7(3) . . . . ? C2 C1 C7 O2 -175.2(3) . . . . ? C6 C1 C7 O2 4.8(4) . . . . ? Mn1 O4 C8 O3 -3.0(3) 5_666 . . . ? Mn1 O4 C8 C3 174.2(2) 5_666 . . . ? Mn1 O3 C8 O4 2.9(3) 5_666 . . . ? Mn1 O3 C8 C3 -174.3(2) 5_666 . . . ? C2 C3 C8 O4 -12.5(4) . . . . ? C4 C3 C8 O4 171.3(3) . . . . ? C2 C3 C8 O3 164.7(3) . . . . ? C4 C3 C8 O3 -11.5(4) . . . . ? C4 C5 C9 C10 5.0(4) . . . . ? C6 C5 C9 C10 -175.1(3) . . . . ? C4 C5 C9 C12 -116.2(3) . . . . ? C6 C5 C9 C12 63.7(4) . . . . ? C4 C5 C9 C11 124.9(4) . . . . ? C6 C5 C9 C11 -55.2(4) . . . . ? C24 N1 C13 C14 0.3(5) . . . . ? Mn1 N1 C13 C14 -177.5(3) . . . . ? N1 C13 C14 C15 1.4(6) . . . . ? C13 C14 C15 C16 -0.9(6) . . . . ? C14 C15 C16 C24 -1.2(6) . . . . ? C14 C15 C16 C17 178.1(4) . . . . ? C15 C16 C17 C18 178.0(4) . . . . ? C24 C16 C17 C18 -2.7(6) . . . . ? C16 C17 C18 C19 0.5(6) . . . . ? C17 C18 C19 C20 179.8(4) . . . . ? C17 C18 C19 C23 1.8(6) . . . . ? C23 C19 C20 C21 0.4(5) . . . . ? C18 C19 C20 C21 -177.6(4) . . . . ? C19 C20 C21 C22 -0.1(6) . . . . ? C23 N2 C22 C21 1.7(5) . . . . ? Mn1 N2 C22 C21 173.8(3) . . . . ? C20 C21 C22 N2 -1.0(6) . . . . ? C22 N2 C23 C19 -1.4(5) . . . . ? Mn1 N2 C23 C19 -174.3(2) . . . . ? C22 N2 C23 C24 178.9(3) . . . . ? Mn1 N2 C23 C24 6.0(4) . . . . ? C20 C19 C23 N2 0.4(5) . . . . ? C18 C19 C23 N2 178.5(3) . . . . ? C20 C19 C23 C24 -179.9(3) . . . . ? C18 C19 C23 C24 -1.8(5) . . . . ? C13 N1 C24 C16 -2.5(5) . . . . ? Mn1 N1 C24 C16 175.5(2) . . . . ? C13 N1 C24 C23 178.4(3) . . . . ? Mn1 N1 C24 C23 -3.6(4) . . . . ? C15 C16 C24 N1 3.0(5) . . . . ? C17 C16 C24 N1 -176.4(3) . . . . ? C15 C16 C24 C23 -178.0(3) . . . . ? C17 C16 C24 C23 2.7(5) . . . . ? N2 C23 C24 N1 -1.6(4) . . . . ? C19 C23 C24 N1 178.6(3) . . . . ? N2 C23 C24 C16 179.3(3) . . . . ? C19 C23 C24 C16 -0.4(5) . . . . ? 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 O1W H1WA O3 0.84 2.06 2.812(7) 149.2 . O1W H1WA O2 0.84 2.59 3.142(8) 124.0 6_565 O1W H1WB O2W 0.85 2.27 2.976(11) 140.2 . O1W H1WB O1W 0.85 2.35 2.887(14) 121.9 7_666 O2W H2WA O3 0.84 2.28 2.911(10) 132.5 7_666 O2W H2WB O1W 0.87 2.13 2.976(11) 163.2 . O2W H2WB O2W 0.87 2.44 3.31(2) 175.5 7_666 _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.569 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.087 #============================================================================== data_MnPhen1-[Mn(Htbip)2(phen)2] _database_code_depnum_ccdc_archive 'CCDC 835407' #TrackingRef '- revised cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H42 Mn N4 O8' _chemical_formula_sum 'C48 H42 Mn N4 O8' _chemical_formula_weight 857.80 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' Mn Mn 0.3368 0.7283 '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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5778(7) _cell_length_b 12.0330(7) _cell_length_c 15.8590(9) _cell_angle_alpha 90.307(1) _cell_angle_beta 94.863(1) _cell_angle_gamma 108.680(1) _cell_volume 2084.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3657 _cell_measurement_theta_min 2.2400 _cell_measurement_theta_max 27.1013 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.367 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 894 _exptl_absorpt_coefficient_mu 0.378 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8791 _exptl_absorpt_correction_T_max 0.9525 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16004 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0719 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 28.70 _reflns_number_total 9480 _reflns_number_gt 7159 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. DFIX (1.53 0.01) is applied to the six C-C distances of the disordered tert-butyl. EADP and ISOR (0.01) are also applied to the disorderd carbon atoms. ; _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^)+(0.0753P)^2^+0.1055P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9480 _refine_ls_number_parameters 563 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0804 _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.1511 _refine_ls_wR_factor_gt 0.1396 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.037 _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 Mn1 Mn 0.85055(3) 0.15077(3) 0.22470(2) 0.01888(12) Uani 1 1 d . . . O1 O 0.80190(19) -0.02481(16) 0.25035(12) 0.0348(5) Uani 1 1 d . . . O2 O 0.86443(16) -0.11787(16) 0.35604(11) 0.0275(4) Uani 1 1 d . . . O3 O 0.62453(18) -0.64073(17) 0.21281(13) 0.0347(5) Uani 1 1 d . . . H3A H 0.6481 -0.6981 0.2259 0.052 Uiso 1 1 calc R . . O4 O 0.75859(18) -0.55210(17) 0.32201(12) 0.0325(5) Uani 1 1 d . . . O5 O 0.67369(15) 0.16164(15) 0.23506(11) 0.0243(4) Uani 1 1 d . . . O6 O 0.52967(17) 0.00488(17) 0.17334(12) 0.0295(4) Uani 1 1 d . . . O7 O 0.11291(17) -0.11912(17) 0.28216(12) 0.0310(5) Uani 1 1 d . . . O8 O 0.08792(17) -0.00390(17) 0.38483(12) 0.0320(5) Uani 1 1 d . . . H8A H 0.0138 -0.0434 0.3739 0.048 Uiso 1 1 calc R . . N1 N 0.94190(19) 0.24347(19) 0.34671(13) 0.0223(5) Uani 1 1 d . . . N2 N 0.91201(18) 0.34905(18) 0.19913(13) 0.0212(5) Uani 1 1 d . . . N3 N 1.0535(2) 0.17938(19) 0.19005(13) 0.0229(5) Uani 1 1 d . . . N4 N 0.84203(19) 0.11268(19) 0.08629(13) 0.0220(5) Uani 1 1 d . . . C1 C 0.7166(2) -0.2301(2) 0.25149(15) 0.0202(5) Uani 1 1 d . . . C2 C 0.7386(2) -0.3331(2) 0.27303(16) 0.0220(5) Uani 1 1 d . . . H2A H 0.8070 -0.3311 0.3113 0.026 Uiso 1 1 calc R . . C3 C 0.6605(2) -0.4393(2) 0.23862(16) 0.0237(6) Uani 1 1 d . . . C4 C 0.5593(2) -0.4421(2) 0.18417(17) 0.0274(6) Uani 1 1 d . . . H4A H 0.5066 -0.5154 0.1607 0.033 Uiso 1 1 calc R . . C5 C 0.5332(2) -0.3405(2) 0.16310(16) 0.0252(6) Uani 1 1 d . . . C6 C 0.6155(2) -0.2342(2) 0.19637(16) 0.0228(5) Uani 1 1 d . . . H6A H 0.6019 -0.1629 0.1809 0.027 Uiso 1 1 calc R . . C7 C 0.8013(2) -0.1155(2) 0.28895(16) 0.0222(5) Uani 1 1 d . . . C8 C 0.6870(2) -0.5480(2) 0.26324(17) 0.0258(6) Uani 1 1 d . . . C9 C 0.4176(3) -0.3413(3) 0.1083(2) 0.0342(7) Uani 1 1 d . . . C10 C 0.3391(3) -0.2955(3) 0.1631(2) 0.0492(9) Uani 1 1 d . . . H10A H 0.2635 -0.2968 0.1296 0.074 Uiso 1 1 calc R . . H10B H 0.3846 -0.2148 0.1830 0.074 Uiso 1 1 calc R . . H10C H 0.3187 -0.3454 0.2119 0.074 Uiso 1 1 calc R . . C11 C 0.4519(3) -0.2605(3) 0.0350(2) 0.0468(9) Uani 1 1 d . . . H11A H 0.3773 -0.2587 0.0016 0.070 Uiso 1 1 calc R . . H11B H 0.5016 -0.2894 -0.0010 0.070 Uiso 1 1 calc R . . H11C H 0.4989 -0.1812 0.0569 0.070 Uiso 1 1 calc R . . C12 C 0.3416(4) -0.4637(3) 0.0751(3) 0.0804(15) Uani 1 1 d . . . H12A H 0.2647 -0.4612 0.0455 0.121 Uiso 1 1 calc R . . H12B H 0.3237 -0.5165 0.1225 0.121 Uiso 1 1 calc R . . H12C H 0.3873 -0.4925 0.0357 0.121 Uiso 1 1 calc R . . C13 C 0.4861(2) 0.0868(2) 0.29804(16) 0.0220(5) Uani 1 1 d . . . C14 C 0.3648(2) 0.0172(2) 0.28999(15) 0.0219(5) Uani 1 1 d . . . H14A H 0.3347 -0.0381 0.2439 0.026 Uiso 1 1 calc R . . C15 C 0.2872(2) 0.0277(2) 0.34882(16) 0.0230(6) Uani 1 1 d . . . C16 C 0.3329(2) 0.1055(3) 0.41841(16) 0.0287(6) Uani 1 1 d . . . H16A H 0.2792 0.1127 0.4586 0.034 Uiso 1 1 calc R . . C17 C 0.4554(3) 0.1723(3) 0.42959(17) 0.0307(6) Uani 1 1 d . A . C18 C 0.5303(2) 0.1628(2) 0.36793(16) 0.0271(6) Uani 1 1 d . . . H18A H 0.6142 0.2096 0.3738 0.033 Uiso 1 1 calc R . . C19 C 0.5676(2) 0.0812(2) 0.23031(16) 0.0229(5) Uani 1 1 d . . . C20 C 0.1547(2) -0.0408(2) 0.33533(16) 0.0232(6) Uani 1 1 d . . . C21 C 0.5093(3) 0.2526(3) 0.50817(18) 0.0484(9) Uani 1 1 d D . . C22 C 0.582(3) 0.3757(13) 0.482(2) 0.0498(17) Uani 0.556(13) 1 d PD A 1 H22A H 0.5302 0.4047 0.4416 0.075 Uiso 0.556(13) 1 calc PR A 1 H22B H 0.6542 0.3725 0.4552 0.075 Uiso 0.556(13) 1 calc PR A 1 H22C H 0.6080 0.4286 0.5321 0.075 Uiso 0.556(13) 1 calc PR A 1 C23 C 0.4189(9) 0.2377(12) 0.5738(6) 0.074(3) Uani 0.556(13) 1 d PDU A 1 H23A H 0.3921 0.1559 0.5909 0.110 Uiso 0.556(13) 1 calc PR A 1 H23B H 0.3479 0.2583 0.5498 0.110 Uiso 0.556(13) 1 calc PR A 1 H23C H 0.4579 0.2893 0.6233 0.110 Uiso 0.556(13) 1 calc PR A 1 C24 C 0.592(2) 0.202(3) 0.5638(14) 0.071(3) Uani 0.556(13) 1 d PDU A 1 H24A H 0.5468 0.1208 0.5771 0.106 Uiso 0.556(13) 1 calc PR A 1 H24B H 0.6210 0.2492 0.6164 0.106 Uiso 0.556(13) 1 calc PR A 1 H24C H 0.6630 0.2019 0.5336 0.106 Uiso 0.556(13) 1 calc PR A 1 C22' C 0.574(4) 0.3777(16) 0.482(3) 0.0498(17) Uani 0.444(13) 1 d PD A 2 H22D H 0.6625 0.3954 0.4916 0.075 Uiso 0.444(13) 1 calc PR A 2 H22E H 0.5484 0.4332 0.5153 0.075 Uiso 0.444(13) 1 calc PR A 2 H22F H 0.5513 0.3849 0.4215 0.075 Uiso 0.444(13) 1 calc PR A 2 C23' C 0.4047(9) 0.2917(13) 0.5451(8) 0.074(3) Uani 0.444(13) 1 d PDU A 2 H23D H 0.3511 0.2261 0.5742 0.110 Uiso 0.444(13) 1 calc PR A 2 H23E H 0.3567 0.3148 0.4986 0.110 Uiso 0.444(13) 1 calc PR A 2 H23F H 0.4417 0.3584 0.5852 0.110 Uiso 0.444(13) 1 calc PR A 2 C24' C 0.609(3) 0.206(3) 0.5496(19) 0.071(3) Uani 0.444(13) 1 d PDU A 2 H24D H 0.5715 0.1253 0.5675 0.106 Uiso 0.444(13) 1 calc PR A 2 H24E H 0.6519 0.2559 0.5991 0.106 Uiso 0.444(13) 1 calc PR A 2 H24F H 0.6682 0.2060 0.5086 0.106 Uiso 0.444(13) 1 calc PR A 2 C25 C 0.9599(3) 0.1924(3) 0.41823(17) 0.0295(6) Uani 1 1 d . . . H25A H 0.9216 0.1101 0.4213 0.035 Uiso 1 1 calc R . . C26 C 1.0318(3) 0.2533(3) 0.48893(18) 0.0378(7) Uani 1 1 d . . . H26A H 1.0438 0.2127 0.5384 0.045 Uiso 1 1 calc R . . C27 C 1.0849(3) 0.3714(3) 0.48659(18) 0.0354(7) Uani 1 1 d . . . H27A H 1.1343 0.4141 0.5345 0.042 Uiso 1 1 calc R . . C28 C 1.0664(2) 0.4298(2) 0.41318(17) 0.0278(6) Uani 1 1 d . . . C29 C 1.1155(3) 0.5543(3) 0.40666(19) 0.0349(7) Uani 1 1 d . . . H29A H 1.1630 0.6005 0.4539 0.042 Uiso 1 1 calc R . . C30 C 1.0959(3) 0.6069(3) 0.33516(19) 0.0350(7) Uani 1 1 d . . . H30A H 1.1285 0.6899 0.3329 0.042 Uiso 1 1 calc R . . C31 C 1.0272(2) 0.5406(2) 0.26263(17) 0.0260(6) Uani 1 1 d . . . C32 C 1.0024(3) 0.5927(3) 0.18741(19) 0.0335(7) Uani 1 1 d . . . H32A H 1.0324 0.6756 0.1829 0.040 Uiso 1 1 calc R . . C33 C 0.9351(3) 0.5235(3) 0.12086(19) 0.0363(7) Uani 1 1 d . . . H33A H 0.9173 0.5576 0.0695 0.044 Uiso 1 1 calc R . . C34 C 0.8927(3) 0.4024(3) 0.12879(17) 0.0307(6) Uani 1 1 d . . . H34A H 0.8473 0.3553 0.0813 0.037 Uiso 1 1 calc R . . C35 C 0.9779(2) 0.4184(2) 0.26579(16) 0.0220(5) Uani 1 1 d . . . C36 C 0.9955(2) 0.3613(2) 0.34335(16) 0.0231(5) Uani 1 1 d . . . C37 C 1.1565(2) 0.2112(2) 0.24010(17) 0.0277(6) Uani 1 1 d . . . H37A H 1.1516 0.2144 0.2995 0.033 Uiso 1 1 calc R . . C38 C 1.2720(3) 0.2403(3) 0.21053(19) 0.0319(7) Uani 1 1 d . . . H38A H 1.3436 0.2631 0.2490 0.038 Uiso 1 1 calc R . . C39 C 1.2807(3) 0.2356(3) 0.12632(19) 0.0338(7) Uani 1 1 d . . . H39A H 1.3588 0.2551 0.1051 0.041 Uiso 1 1 calc R . . C40 C 1.1741(3) 0.2018(2) 0.07002(18) 0.0281(6) Uani 1 1 d . . . C41 C 1.1745(3) 0.1912(3) -0.01974(19) 0.0362(7) Uani 1 1 d . . . H41A H 1.2506 0.2114 -0.0439 0.043 Uiso 1 1 calc R . . C42 C 1.0698(3) 0.1534(3) -0.07073(18) 0.0327(7) Uani 1 1 d . . . H42A H 1.0730 0.1457 -0.1301 0.039 Uiso 1 1 calc R . . C43 C 0.9537(3) 0.1245(2) -0.03670(16) 0.0253(6) Uani 1 1 d . . . C44 C 0.8421(3) 0.0833(3) -0.08665(17) 0.0311(6) Uani 1 1 d . . . H44A H 0.8413 0.0742 -0.1463 0.037 Uiso 1 1 calc R . . C45 C 0.7342(3) 0.0560(3) -0.05014(17) 0.0311(6) Uani 1 1 d . . . H45A H 0.6580 0.0261 -0.0835 0.037 Uiso 1 1 calc R . . C46 C 0.7387(2) 0.0733(2) 0.03738(16) 0.0259(6) Uani 1 1 d . . . H46A H 0.6637 0.0559 0.0628 0.031 Uiso 1 1 calc R . . C47 C 0.9497(2) 0.1374(2) 0.05102(16) 0.0232(6) Uani 1 1 d . . . C48 C 1.0611(2) 0.1738(2) 0.10526(16) 0.0225(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0192(2) 0.0166(2) 0.0210(2) 0.00104(15) 0.00193(14) 0.00587(16) O1 0.0413(12) 0.0138(10) 0.0430(12) 0.0067(8) -0.0087(9) 0.0034(9) O2 0.0224(10) 0.0264(11) 0.0287(10) 0.0047(8) -0.0017(8) 0.0017(8) O3 0.0376(12) 0.0184(10) 0.0486(12) -0.0017(9) -0.0033(10) 0.0113(9) O4 0.0323(11) 0.0264(11) 0.0419(11) 0.0039(9) 0.0004(9) 0.0146(9) O5 0.0159(9) 0.0188(9) 0.0388(10) -0.0023(8) 0.0059(8) 0.0056(7) O6 0.0267(10) 0.0263(11) 0.0347(10) -0.0068(8) 0.0074(8) 0.0062(8) O7 0.0268(10) 0.0275(11) 0.0321(10) -0.0071(9) 0.0049(8) -0.0008(9) O8 0.0188(10) 0.0335(12) 0.0392(11) -0.0093(9) 0.0043(8) 0.0019(8) N1 0.0246(11) 0.0206(12) 0.0228(11) 0.0002(9) 0.0012(9) 0.0091(9) N2 0.0168(10) 0.0196(11) 0.0261(11) 0.0008(9) 0.0001(8) 0.0049(9) N3 0.0248(11) 0.0210(12) 0.0250(11) 0.0041(9) 0.0038(9) 0.0099(9) N4 0.0249(11) 0.0218(12) 0.0204(10) 0.0000(9) 0.0030(9) 0.0087(9) C1 0.0217(13) 0.0185(13) 0.0218(12) 0.0025(10) 0.0048(10) 0.0079(10) C2 0.0204(13) 0.0218(14) 0.0247(13) 0.0020(10) 0.0036(10) 0.0078(11) C3 0.0237(13) 0.0211(14) 0.0289(13) 0.0007(11) 0.0059(11) 0.0098(11) C4 0.0237(14) 0.0203(14) 0.0363(15) -0.0033(11) -0.0003(11) 0.0053(11) C5 0.0237(14) 0.0224(14) 0.0295(14) 0.0005(11) 0.0009(11) 0.0077(11) C6 0.0231(13) 0.0203(14) 0.0268(13) 0.0048(11) 0.0036(10) 0.0089(11) C7 0.0180(12) 0.0230(14) 0.0263(13) 0.0006(11) 0.0065(10) 0.0063(11) C8 0.0231(14) 0.0212(14) 0.0349(15) 0.0016(12) 0.0068(11) 0.0084(11) C9 0.0259(15) 0.0234(15) 0.0499(18) 0.0002(13) -0.0131(13) 0.0073(12) C10 0.0274(17) 0.058(2) 0.064(2) 0.0180(18) 0.0045(15) 0.0152(16) C11 0.0378(18) 0.065(2) 0.0394(18) 0.0034(16) -0.0077(14) 0.0226(17) C12 0.071(3) 0.036(2) 0.122(4) -0.015(2) -0.064(3) 0.019(2) C13 0.0200(13) 0.0211(14) 0.0258(13) 0.0027(10) 0.0004(10) 0.0083(11) C14 0.0238(13) 0.0197(13) 0.0230(12) 0.0011(10) -0.0009(10) 0.0089(11) C15 0.0214(13) 0.0223(14) 0.0239(13) 0.0032(11) 0.0000(10) 0.0055(11) C16 0.0250(14) 0.0343(17) 0.0251(13) -0.0028(12) 0.0060(11) 0.0064(12) C17 0.0239(14) 0.0369(17) 0.0243(13) -0.0056(12) 0.0017(11) 0.0003(12) C18 0.0199(13) 0.0292(15) 0.0275(14) -0.0001(11) -0.0007(11) 0.0023(11) C19 0.0213(13) 0.0205(14) 0.0289(13) 0.0021(11) 0.0015(11) 0.0099(11) C20 0.0247(14) 0.0228(14) 0.0224(12) 0.0051(11) 0.0026(10) 0.0076(11) C21 0.0343(18) 0.067(3) 0.0277(16) -0.0141(15) 0.0078(13) -0.0067(17) C22 0.047(4) 0.049(2) 0.049(2) -0.0205(18) -0.004(2) 0.0114(19) C23 0.057(3) 0.094(6) 0.039(4) -0.036(3) 0.027(3) -0.023(4) C24 0.087(5) 0.057(3) 0.035(6) 0.012(4) -0.018(4) -0.017(4) C22' 0.047(4) 0.049(2) 0.049(2) -0.0205(18) -0.004(2) 0.0114(19) C23' 0.057(3) 0.094(6) 0.039(4) -0.036(3) 0.027(3) -0.023(4) C24' 0.087(5) 0.057(3) 0.035(6) 0.012(4) -0.018(4) -0.017(4) C25 0.0361(16) 0.0249(15) 0.0297(14) 0.0047(12) 0.0036(12) 0.0128(13) C26 0.0454(19) 0.0421(19) 0.0252(14) 0.0061(13) -0.0039(13) 0.0147(15) C27 0.0366(17) 0.0379(18) 0.0276(14) -0.0062(13) -0.0073(12) 0.0089(14) C28 0.0265(14) 0.0287(16) 0.0283(14) -0.0024(12) -0.0008(11) 0.0097(12) C29 0.0306(16) 0.0279(16) 0.0393(16) -0.0089(13) -0.0062(13) 0.0024(13) C30 0.0333(16) 0.0200(15) 0.0462(18) -0.0044(13) 0.0005(14) 0.0019(13) C31 0.0202(13) 0.0203(14) 0.0355(15) 0.0012(11) 0.0021(11) 0.0040(11) C32 0.0295(15) 0.0211(15) 0.0489(18) 0.0112(13) 0.0038(13) 0.0066(12) C33 0.0383(17) 0.0271(16) 0.0413(17) 0.0128(13) -0.0004(14) 0.0081(14) C34 0.0324(16) 0.0288(16) 0.0291(14) 0.0051(12) -0.0016(12) 0.0081(13) C35 0.0189(12) 0.0211(14) 0.0269(13) 0.0009(11) 0.0032(10) 0.0073(11) C36 0.0183(13) 0.0221(14) 0.0289(13) -0.0016(11) 0.0014(10) 0.0069(11) C37 0.0250(14) 0.0300(16) 0.0294(14) 0.0032(12) 0.0002(11) 0.0109(12) C38 0.0234(14) 0.0304(16) 0.0421(17) 0.0038(13) -0.0024(12) 0.0105(12) C39 0.0229(15) 0.0308(17) 0.0471(18) 0.0063(14) 0.0092(13) 0.0061(13) C40 0.0260(14) 0.0211(14) 0.0393(16) 0.0040(12) 0.0095(12) 0.0089(12) C41 0.0338(17) 0.0358(18) 0.0424(17) 0.0084(14) 0.0184(14) 0.0119(14) C42 0.0374(17) 0.0348(17) 0.0287(14) 0.0062(12) 0.0121(12) 0.0130(14) C43 0.0327(15) 0.0215(14) 0.0252(13) 0.0029(11) 0.0069(11) 0.0127(12) C44 0.0430(17) 0.0342(17) 0.0208(13) 0.0035(12) 0.0052(12) 0.0183(14) C45 0.0322(16) 0.0339(17) 0.0268(14) -0.0015(12) -0.0036(12) 0.0115(13) C46 0.0261(14) 0.0259(15) 0.0279(13) 0.0017(11) 0.0029(11) 0.0113(12) C47 0.0291(14) 0.0179(13) 0.0273(13) 0.0034(10) 0.0071(11) 0.0129(11) C48 0.0256(14) 0.0175(13) 0.0270(13) 0.0022(10) 0.0049(11) 0.0098(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O1 2.0573(18) . ? Mn1 O5 2.1132(17) . ? Mn1 N4 2.227(2) . ? Mn1 N1 2.232(2) . ? Mn1 N2 2.310(2) . ? Mn1 N3 2.376(2) . ? O1 C7 1.252(3) . ? O2 C7 1.245(3) . ? O3 C8 1.335(3) . ? O3 H3A 0.8400 . ? O4 C8 1.206(3) . ? O5 C19 1.293(3) . ? O6 C19 1.232(3) . ? O7 C20 1.209(3) . ? O8 C20 1.316(3) . ? O8 H8A 0.8400 . ? N1 C25 1.325(3) . ? N1 C36 1.357(3) . ? N2 C34 1.328(3) . ? N2 C35 1.357(3) . ? N3 C37 1.320(3) . ? N3 C48 1.358(3) . ? N4 C46 1.317(3) . ? N4 C47 1.356(3) . ? C1 C2 1.382(3) . ? C1 C6 1.388(3) . ? C1 C7 1.497(4) . ? C2 C3 1.384(4) . ? C2 H2A 0.9500 . ? C3 C4 1.386(4) . ? C3 C8 1.484(4) . ? C4 C5 1.386(4) . ? C4 H4A 0.9500 . ? C5 C6 1.396(4) . ? C5 C9 1.530(4) . ? C6 H6A 0.9500 . ? C9 C11 1.516(4) . ? C9 C12 1.518(4) . ? C9 C10 1.529(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.380(3) . ? C13 C18 1.386(4) . ? C13 C19 1.504(4) . ? C14 C15 1.382(4) . ? C14 H14A 0.9500 . ? C15 C16 1.396(4) . ? C15 C20 1.486(4) . ? C16 C17 1.384(4) . ? C16 H16A 0.9500 . ? C17 C18 1.389(4) . ? C17 C21 1.531(4) . ? C18 H18A 0.9500 . ? C21 C23' 1.585(8) . ? C21 C23 1.510(6) . ? C21 C22' 1.529(9) . ? C21 C24' 1.545(9) . ? C21 C24 1.524(8) . ? C21 C22 1.530(8) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C22' H22D 0.9800 . ? C22' H22E 0.9800 . ? C22' H22F 0.9800 . ? C23' H23D 0.9800 . ? C23' H23E 0.9800 . ? C23' H23F 0.9800 . ? C24' H24D 0.9800 . ? C24' H24E 0.9800 . ? C24' H24F 0.9800 . ? C25 C26 1.389(4) . ? C25 H25A 0.9500 . ? C26 C27 1.357(4) . ? C26 H26A 0.9500 . ? C27 C28 1.399(4) . ? C27 H27A 0.9500 . ? C28 C36 1.408(4) . ? C28 C29 1.430(4) . ? C29 C30 1.340(4) . ? C29 H29A 0.9500 . ? C30 C31 1.422(4) . ? C30 H30A 0.9500 . ? C31 C35 1.400(4) . ? C31 C32 1.401(4) . ? C32 C33 1.360(4) . ? C32 H32A 0.9500 . ? C33 C34 1.391(4) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? C35 C36 1.443(3) . ? C37 C38 1.392(4) . ? C37 H37A 0.9500 . ? C38 C39 1.350(4) . ? C38 H38A 0.9500 . ? C39 C40 1.405(4) . ? C39 H39A 0.9500 . ? C40 C48 1.408(4) . ? C40 C41 1.429(4) . ? C41 C42 1.345(4) . ? C41 H41A 0.9500 . ? C42 C43 1.430(4) . ? C42 H42A 0.9500 . ? C43 C44 1.398(4) . ? C43 C47 1.405(4) . ? C44 C45 1.366(4) . ? C44 H44A 0.9500 . ? C45 C46 1.397(4) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C47 C48 1.428(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 O1 Mn1 O5 94.46(8) . . ? O1 Mn1 N4 91.80(8) . . ? O5 Mn1 N4 100.94(7) . . ? O1 Mn1 N1 104.80(8) . . ? O5 Mn1 N1 98.48(7) . . ? N4 Mn1 N1 153.31(8) . . ? O1 Mn1 N2 177.82(7) . . ? O5 Mn1 N2 87.17(7) . . ? N4 Mn1 N2 89.31(8) . . ? N1 Mn1 N2 73.50(7) . . ? O1 Mn1 N3 98.67(8) . . ? O5 Mn1 N3 165.37(7) . . ? N4 Mn1 N3 72.32(7) . . ? N1 Mn1 N3 84.44(8) . . ? N2 Mn1 N3 79.89(7) . . ? C7 O1 Mn1 158.41(18) . . ? C8 O3 H3A 109.5 . . ? C19 O5 Mn1 131.12(16) . . ? C20 O8 H8A 109.5 . . ? C25 N1 C36 117.9(2) . . ? C25 N1 Mn1 125.72(19) . . ? C36 N1 Mn1 115.87(16) . . ? C34 N2 C35 117.0(2) . . ? C34 N2 Mn1 128.86(18) . . ? C35 N2 Mn1 114.14(16) . . ? C37 N3 C48 118.0(2) . . ? C37 N3 Mn1 129.04(18) . . ? C48 N3 Mn1 112.52(16) . . ? C46 N4 C47 119.2(2) . . ? C46 N4 Mn1 123.30(18) . . ? C47 N4 Mn1 117.42(17) . . ? C2 C1 C6 119.7(2) . . ? C2 C1 C7 119.5(2) . . ? C6 C1 C7 120.8(2) . . ? C3 C2 C1 119.7(2) . . ? C3 C2 H2A 120.1 . . ? C1 C2 H2A 120.1 . . ? C2 C3 C4 120.0(2) . . ? C2 C3 C8 118.2(2) . . ? C4 C3 C8 121.8(2) . . ? C5 C4 C3 121.6(3) . . ? C5 C4 H4A 119.2 . . ? C3 C4 H4A 119.2 . . ? C4 C5 C6 117.4(2) . . ? C4 C5 C9 122.9(2) . . ? C6 C5 C9 119.7(2) . . ? C1 C6 C5 121.6(2) . . ? C1 C6 H6A 119.2 . . ? C5 C6 H6A 119.2 . . ? O1 C7 O2 125.3(2) . . ? O1 C7 C1 117.1(2) . . ? O2 C7 C1 117.6(2) . . ? O4 C8 O3 123.4(2) . . ? O4 C8 C3 123.6(3) . . ? O3 C8 C3 113.0(2) . . ? C11 C9 C12 109.9(3) . . ? C11 C9 C10 108.6(3) . . ? C12 C9 C10 107.8(3) . . ? C11 C9 C5 109.9(2) . . ? C12 C9 C5 112.4(2) . . ? C10 C9 C5 108.0(2) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 119.3(2) . . ? C14 C13 C19 119.8(2) . . ? C18 C13 C19 120.9(2) . . ? C13 C14 C15 120.2(2) . . ? C13 C14 H14A 119.9 . . ? C15 C14 H14A 119.9 . . ? C14 C15 C16 119.7(2) . . ? C14 C15 C20 119.4(2) . . ? C16 C15 C20 120.8(2) . . ? C17 C16 C15 120.9(3) . . ? C17 C16 H16A 119.6 . . ? C15 C16 H16A 119.6 . . ? C16 C17 C18 118.0(2) . . ? C16 C17 C21 121.8(3) . . ? C18 C17 C21 120.1(2) . . ? C13 C18 C17 121.8(2) . . ? C13 C18 H18A 119.1 . . ? C17 C18 H18A 119.1 . . ? O6 C19 O5 124.3(2) . . ? O6 C19 C13 119.5(2) . . ? O5 C19 C13 116.2(2) . . ? O7 C20 O8 123.9(2) . . ? O7 C20 C15 123.2(2) . . ? O8 C20 C15 112.8(2) . . ? C17 C21 C23' 109.2(5) . . ? C17 C21 C23 112.4(4) . . ? C17 C21 C22' 110.0(17) . . ? C23' C21 C22' 91.2(18) . . ? C23 C21 C22' 117.0(18) . . ? C17 C21 C24' 104.5(14) . . ? C23' C21 C24' 132.9(14) . . ? C23 C21 C24' 104.7(14) . . ? C22' C21 C24' 107(2) . . ? C17 C21 C24 109.6(12) . . ? C23' C21 C24 122.0(12) . . ? C23 C21 C24 93.3(12) . . ? C22' C21 C24 113(2) . . ? C17 C21 C22 110.1(14) . . ? C23' C21 C22 94.9(15) . . ? C23 C21 C22 120.0(15) . . ? C24' C21 C22 103(2) . . ? C24 C21 C22 110.0(18) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C22' H22D 109.5 . . ? C21 C22' H22E 109.5 . . ? H22D C22' H22E 109.5 . . ? C21 C22' H22F 109.5 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? C21 C23' H23D 109.5 . . ? C21 C23' H23E 109.5 . . ? H23D C23' H23E 109.5 . . ? C21 C23' H23F 109.5 . . ? H23D C23' H23F 109.5 . . ? H23E C23' H23F 109.5 . . ? C21 C24' H24D 109.5 . . ? C21 C24' H24E 109.5 . . ? H24D C24' H24E 109.5 . . ? C21 C24' H24F 109.5 . . ? H24D C24' H24F 109.5 . . ? H24E C24' H24F 109.5 . . ? N1 C25 C26 123.2(3) . . ? N1 C25 H25A 118.4 . . ? C26 C25 H25A 118.4 . . ? C27 C26 C25 119.3(3) . . ? C27 C26 H26A 120.3 . . ? C25 C26 H26A 120.3 . . ? C26 C27 C28 119.6(3) . . ? C26 C27 H27A 120.2 . . ? C28 C27 H27A 120.2 . . ? C27 C28 C36 117.6(3) . . ? C27 C28 C29 123.0(3) . . ? C36 C28 C29 119.4(2) . . ? C30 C29 C28 121.2(3) . . ? C30 C29 H29A 119.4 . . ? C28 C29 H29A 119.4 . . ? C29 C30 C31 121.1(3) . . ? C29 C30 H30A 119.5 . . ? C31 C30 H30A 119.5 . . ? C35 C31 C32 117.5(2) . . ? C35 C31 C30 119.8(2) . . ? C32 C31 C30 122.7(3) . . ? C33 C32 C31 119.3(3) . . ? C33 C32 H32A 120.3 . . ? C31 C32 H32A 120.3 . . ? C32 C33 C34 119.3(3) . . ? C32 C33 H33A 120.4 . . ? C34 C33 H33A 120.4 . . ? N2 C34 C33 123.6(3) . . ? N2 C34 H34A 118.2 . . ? C33 C34 H34A 118.2 . . ? N2 C35 C31 123.2(2) . . ? N2 C35 C36 117.3(2) . . ? C31 C35 C36 119.5(2) . . ? N1 C36 C28 122.3(2) . . ? N1 C36 C35 118.8(2) . . ? C28 C36 C35 119.0(2) . . ? N3 C37 C38 123.5(3) . . ? N3 C37 H37A 118.2 . . ? C38 C37 H37A 118.2 . . ? C39 C38 C37 119.0(3) . . ? C39 C38 H38A 120.5 . . ? C37 C38 H38A 120.5 . . ? C38 C39 C40 120.0(3) . . ? C38 C39 H39A 120.0 . . ? C40 C39 H39A 120.0 . . ? C48 C40 C39 117.3(3) . . ? C48 C40 C41 118.9(3) . . ? C39 C40 C41 123.7(3) . . ? C42 C41 C40 121.5(3) . . ? C42 C41 H41A 119.2 . . ? C40 C41 H41A 119.2 . . ? C41 C42 C43 120.8(3) . . ? C41 C42 H42A 119.6 . . ? C43 C42 H42A 119.6 . . ? C44 C43 C47 117.6(2) . . ? C44 C43 C42 123.1(2) . . ? C47 C43 C42 119.3(3) . . ? C45 C44 C43 120.3(2) . . ? C45 C44 H44A 119.8 . . ? C43 C44 H44A 119.8 . . ? C44 C45 C46 118.4(3) . . ? C44 C45 H45A 120.8 . . ? C46 C45 H45A 120.8 . . ? N4 C46 C45 123.0(3) . . ? N4 C46 H46A 118.5 . . ? C45 C46 H46A 118.5 . . ? N4 C47 C43 121.6(2) . . ? N4 C47 C48 118.7(2) . . ? C43 C47 C48 119.7(2) . . ? N3 C48 C40 122.1(2) . . ? N3 C48 C47 118.1(2) . . ? C40 C48 C47 119.7(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Mn1 O1 C7 -117.2(5) . . . . ? N4 Mn1 O1 C7 141.6(5) . . . . ? N1 Mn1 O1 C7 -17.2(5) . . . . ? N3 Mn1 O1 C7 69.3(5) . . . . ? O1 Mn1 O5 C19 -20.1(2) . . . . ? N4 Mn1 O5 C19 72.6(2) . . . . ? N1 Mn1 O5 C19 -125.8(2) . . . . ? N2 Mn1 O5 C19 161.3(2) . . . . ? N3 Mn1 O5 C19 133.6(3) . . . . ? O1 Mn1 N1 C25 0.6(2) . . . . ? O5 Mn1 N1 C25 97.6(2) . . . . ? N4 Mn1 N1 C25 -126.1(2) . . . . ? N2 Mn1 N1 C25 -178.0(2) . . . . ? N3 Mn1 N1 C25 -96.9(2) . . . . ? O1 Mn1 N1 C36 172.51(17) . . . . ? O5 Mn1 N1 C36 -90.56(18) . . . . ? N4 Mn1 N1 C36 45.8(3) . . . . ? N2 Mn1 N1 C36 -6.08(17) . . . . ? N3 Mn1 N1 C36 74.99(18) . . . . ? O5 Mn1 N2 C34 -76.4(2) . . . . ? N4 Mn1 N2 C34 24.6(2) . . . . ? N1 Mn1 N2 C34 -176.1(2) . . . . ? N3 Mn1 N2 C34 96.7(2) . . . . ? O5 Mn1 N2 C35 104.42(17) . . . . ? N4 Mn1 N2 C35 -154.60(18) . . . . ? N1 Mn1 N2 C35 4.70(17) . . . . ? N3 Mn1 N2 C35 -82.44(17) . . . . ? O1 Mn1 N3 C37 -90.5(2) . . . . ? O5 Mn1 N3 C37 116.0(3) . . . . ? N4 Mn1 N3 C37 -179.6(2) . . . . ? N1 Mn1 N3 C37 13.7(2) . . . . ? N2 Mn1 N3 C37 87.8(2) . . . . ? O1 Mn1 N3 C48 97.41(17) . . . . ? O5 Mn1 N3 C48 -56.1(4) . . . . ? N4 Mn1 N3 C48 8.29(16) . . . . ? N1 Mn1 N3 C48 -158.42(18) . . . . ? N2 Mn1 N3 C48 -84.23(17) . . . . ? O1 Mn1 N4 C46 77.1(2) . . . . ? O5 Mn1 N4 C46 -17.8(2) . . . . ? N1 Mn1 N4 C46 -153.8(2) . . . . ? N2 Mn1 N4 C46 -104.8(2) . . . . ? N3 Mn1 N4 C46 175.6(2) . . . . ? O1 Mn1 N4 C47 -106.35(18) . . . . ? O5 Mn1 N4 C47 158.76(18) . . . . ? N1 Mn1 N4 C47 22.8(3) . . . . ? N2 Mn1 N4 C47 71.78(18) . . . . ? N3 Mn1 N4 C47 -7.82(17) . . . . ? C6 C1 C2 C3 0.8(4) . . . . ? C7 C1 C2 C3 180.0(2) . . . . ? C1 C2 C3 C4 -1.3(4) . . . . ? C1 C2 C3 C8 -180.0(2) . . . . ? C2 C3 C4 C5 -0.3(4) . . . . ? C8 C3 C4 C5 178.3(2) . . . . ? C3 C4 C5 C6 2.4(4) . . . . ? C3 C4 C5 C9 -175.6(3) . . . . ? C2 C1 C6 C5 1.3(4) . . . . ? C7 C1 C6 C5 -177.8(2) . . . . ? C4 C5 C6 C1 -2.9(4) . . . . ? C9 C5 C6 C1 175.1(2) . . . . ? Mn1 O1 C7 O2 0.4(7) . . . . ? Mn1 O1 C7 C1 179.8(4) . . . . ? C2 C1 C7 O1 158.9(2) . . . . ? C6 C1 C7 O1 -22.0(4) . . . . ? C2 C1 C7 O2 -21.7(3) . . . . ? C6 C1 C7 O2 157.4(2) . . . . ? C2 C3 C8 O4 13.6(4) . . . . ? C4 C3 C8 O4 -165.0(3) . . . . ? C2 C3 C8 O3 -165.5(2) . . . . ? C4 C3 C8 O3 15.9(4) . . . . ? C4 C5 C9 C11 -127.0(3) . . . . ? C6 C5 C9 C11 55.1(4) . . . . ? C4 C5 C9 C12 -4.2(4) . . . . ? C6 C5 C9 C12 177.9(3) . . . . ? C4 C5 C9 C10 114.6(3) . . . . ? C6 C5 C9 C10 -63.3(3) . . . . ? C18 C13 C14 C15 3.3(4) . . . . ? C19 C13 C14 C15 -175.4(2) . . . . ? C13 C14 C15 C16 -2.7(4) . . . . ? C13 C14 C15 C20 175.0(2) . . . . ? C14 C15 C16 C17 -0.2(4) . . . . ? C20 C15 C16 C17 -177.8(3) . . . . ? C15 C16 C17 C18 2.4(4) . . . . ? C15 C16 C17 C21 -176.2(3) . . . . ? C14 C13 C18 C17 -1.1(4) . . . . ? C19 C13 C18 C17 177.6(2) . . . . ? C16 C17 C18 C13 -1.7(4) . . . . ? C21 C17 C18 C13 176.8(3) . . . . ? Mn1 O5 C19 O6 -48.9(4) . . . . ? Mn1 O5 C19 C13 133.50(19) . . . . ? C14 C13 C19 O6 -8.5(4) . . . . ? C18 C13 C19 O6 172.7(2) . . . . ? C14 C13 C19 O5 169.2(2) . . . . ? C18 C13 C19 O5 -9.5(4) . . . . ? C14 C15 C20 O7 11.5(4) . . . . ? C16 C15 C20 O7 -170.9(3) . . . . ? C14 C15 C20 O8 -165.9(2) . . . . ? C16 C15 C20 O8 11.7(4) . . . . ? C16 C17 C21 C23' -26.5(8) . . . . ? C18 C17 C21 C23' 155.0(7) . . . . ? C16 C17 C21 C23 7.2(8) . . . . ? C18 C17 C21 C23 -171.3(7) . . . . ? C16 C17 C21 C22' -125.2(19) . . . . ? C18 C17 C21 C22' 56.3(19) . . . . ? C16 C17 C21 C24' 120.1(14) . . . . ? C18 C17 C21 C24' -58.4(14) . . . . ? C16 C17 C21 C24 109.5(11) . . . . ? C18 C17 C21 C24 -69.0(11) . . . . ? C16 C17 C21 C22 -129.5(15) . . . . ? C18 C17 C21 C22 52.1(15) . . . . ? C36 N1 C25 C26 -0.9(4) . . . . ? Mn1 N1 C25 C26 170.8(2) . . . . ? N1 C25 C26 C27 1.6(5) . . . . ? C25 C26 C27 C28 0.0(5) . . . . ? C26 C27 C28 C36 -2.0(4) . . . . ? C26 C27 C28 C29 177.8(3) . . . . ? C27 C28 C29 C30 179.9(3) . . . . ? C36 C28 C29 C30 -0.4(4) . . . . ? C28 C29 C30 C31 -1.1(5) . . . . ? C29 C30 C31 C35 0.6(4) . . . . ? C29 C30 C31 C32 178.5(3) . . . . ? C35 C31 C32 C33 -1.5(4) . . . . ? C30 C31 C32 C33 -179.5(3) . . . . ? C31 C32 C33 C34 -0.3(5) . . . . ? C35 N2 C34 C33 -0.5(4) . . . . ? Mn1 N2 C34 C33 -179.7(2) . . . . ? C32 C33 C34 N2 1.4(5) . . . . ? C34 N2 C35 C31 -1.4(4) . . . . ? Mn1 N2 C35 C31 177.86(19) . . . . ? C34 N2 C35 C36 177.8(2) . . . . ? Mn1 N2 C35 C36 -2.9(3) . . . . ? C32 C31 C35 N2 2.4(4) . . . . ? C30 C31 C35 N2 -179.6(3) . . . . ? C32 C31 C35 C36 -176.8(2) . . . . ? C30 C31 C35 C36 1.2(4) . . . . ? C25 N1 C36 C28 -1.3(4) . . . . ? Mn1 N1 C36 C28 -173.8(2) . . . . ? C25 N1 C36 C35 179.5(2) . . . . ? Mn1 N1 C36 C35 6.9(3) . . . . ? C27 C28 C36 N1 2.7(4) . . . . ? C29 C28 C36 N1 -177.1(2) . . . . ? C27 C28 C36 C35 -178.1(2) . . . . ? C29 C28 C36 C35 2.2(4) . . . . ? N2 C35 C36 N1 -2.6(4) . . . . ? C31 C35 C36 N1 176.7(2) . . . . ? N2 C35 C36 C28 178.1(2) . . . . ? C31 C35 C36 C28 -2.6(4) . . . . ? C48 N3 C37 C38 0.6(4) . . . . ? Mn1 N3 C37 C38 -171.1(2) . . . . ? N3 C37 C38 C39 -0.3(4) . . . . ? C37 C38 C39 C40 0.1(4) . . . . ? C38 C39 C40 C48 -0.1(4) . . . . ? C38 C39 C40 C41 -178.2(3) . . . . ? C48 C40 C41 C42 -1.2(4) . . . . ? C39 C40 C41 C42 176.9(3) . . . . ? C40 C41 C42 C43 1.3(5) . . . . ? C41 C42 C43 C44 -179.1(3) . . . . ? C41 C42 C43 C47 0.8(4) . . . . ? C47 C43 C44 C45 -0.6(4) . . . . ? C42 C43 C44 C45 179.3(3) . . . . ? C43 C44 C45 C46 1.7(4) . . . . ? C47 N4 C46 C45 -0.3(4) . . . . ? Mn1 N4 C46 C45 176.2(2) . . . . ? C44 C45 C46 N4 -1.2(4) . . . . ? C46 N4 C47 C43 1.4(4) . . . . ? Mn1 N4 C47 C43 -175.30(19) . . . . ? C46 N4 C47 C48 -176.6(2) . . . . ? Mn1 N4 C47 C48 6.7(3) . . . . ? C44 C43 C47 N4 -1.0(4) . . . . ? C42 C43 C47 N4 179.1(2) . . . . ? C44 C43 C47 C48 177.0(2) . . . . ? C42 C43 C47 C48 -2.9(4) . . . . ? C37 N3 C48 C40 -0.6(4) . . . . ? Mn1 N3 C48 C40 172.4(2) . . . . ? C37 N3 C48 C47 178.9(2) . . . . ? Mn1 N3 C48 C47 -8.1(3) . . . . ? C39 C40 C48 N3 0.4(4) . . . . ? C41 C40 C48 N3 178.6(2) . . . . ? C39 C40 C48 C47 -179.1(2) . . . . ? C41 C40 C48 C47 -0.9(4) . . . . ? N4 C47 C48 N3 1.5(4) . . . . ? C43 C47 C48 N3 -176.6(2) . . . . ? N4 C47 C48 C40 -179.0(2) . . . . ? C43 C47 C48 C40 3.0(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3A O5 0.84 1.81 2.635(3) 167.2 1_545 O8 H8A O2 0.84 1.67 2.511(3) 176.9 1_455 _diffrn_measured_fraction_theta_max 0.880 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.472 _refine_diff_density_min -0.334 _refine_diff_density_rms 0.071 #============================================================================== data_FePhen-[Fe(phen)3].2Htbip.3.5H2O _database_code_depnum_ccdc_archive 'CCDC 835408' #TrackingRef '- revised cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C36 H24 Fe N6), 2(C12 H13 O4), 3.5(H2 O)' _chemical_formula_sum 'C60 H57 Fe N6 O11.50' _chemical_formula_weight 1101.97 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C 2 2 21' _symmetry_space_group_name_Hall 'C 2c 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y, -z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z+1/2' _cell_length_a 14.4060(8) _cell_length_b 18.0665(10) _cell_length_c 20.6240(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5367.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5019 _cell_measurement_theta_min 2.4615 _cell_measurement_theta_max 26.0144 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.364 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2308 _exptl_absorpt_coefficient_mu 0.351 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8638 _exptl_absorpt_correction_T_max 0.9082 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31088 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 28.66 _reflns_number_total 6546 _reflns_number_gt 5903 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ISOR 0.01 is applied to one lattice water molecule. ; _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^)+(0.1043P)^2^+2.2582P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.38(2) _refine_ls_number_reflns 6546 _refine_ls_number_parameters 375 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0669 _refine_ls_R_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.1598 _refine_ls_wR_factor_gt 0.1556 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.64204(4) 0.5000 0.5000 0.03222(16) Uani 1 2 d S . . N1 N 0.73861(17) 0.54180(14) 0.44371(15) 0.0400(6) Uani 1 1 d . . . N2 N 0.6446(2) 0.60022(13) 0.53834(13) 0.0395(6) Uani 1 1 d . . . N3 N 0.54054(17) 0.53083(14) 0.44268(12) 0.0321(5) Uani 1 1 d . . . O1 O 0.68390(15) 0.61904(10) 0.27334(10) 0.0365(5) Uani 1 1 d . . . O2 O 0.7944(2) 0.66813(12) 0.21355(15) 0.0621(9) Uani 1 1 d . . . O3 O 0.85132(18) 0.93857(10) 0.22312(12) 0.0441(5) Uani 1 1 d . . . O4 O 0.74265(16) 1.00685(11) 0.26897(12) 0.0479(6) Uani 1 1 d . . . H4 H 0.7735 1.0412 0.2520 0.072 Uiso 1 1 calc R . . C1 C 0.7059(2) 0.74799(13) 0.27978(14) 0.0283(5) Uani 1 1 d . . . C2 C 0.7558(2) 0.80892(14) 0.25922(14) 0.0280(5) Uani 1 1 d . . . H2A H 0.8067 0.8031 0.2303 0.034 Uiso 1 1 calc R . . C3 C 0.7310(2) 0.87848(13) 0.28115(13) 0.0269(5) Uani 1 1 d . . . C4 C 0.6572(2) 0.88603(14) 0.32420(13) 0.0285(6) Uani 1 1 d . . . H4A H 0.6406 0.9339 0.3392 0.034 Uiso 1 1 calc R . . C5 C 0.6073(2) 0.82504(15) 0.34564(13) 0.0280(5) Uani 1 1 d . . . C6 C 0.6332(2) 0.75622(13) 0.32257(13) 0.0298(5) Uani 1 1 d . . . H6A H 0.6001 0.7136 0.3365 0.036 Uiso 1 1 calc R . . C7 C 0.7313(2) 0.67398(15) 0.25238(16) 0.0360(7) Uani 1 1 d . . . C8 C 0.7805(2) 0.94460(14) 0.25551(15) 0.0326(6) Uani 1 1 d . . . C9 C 0.5230(2) 0.83459(16) 0.38924(15) 0.0357(6) Uani 1 1 d . . . C10 C 0.4996(3) 0.7629(2) 0.4254(3) 0.0664(12) Uani 1 1 d . . . H10A H 0.4791 0.7253 0.3943 0.100 Uiso 1 1 calc R . . H10B H 0.4499 0.7724 0.4567 0.100 Uiso 1 1 calc R . . H10C H 0.5549 0.7451 0.4483 0.100 Uiso 1 1 calc R . . C11 C 0.4416(3) 0.8542(3) 0.3464(2) 0.0730(14) Uani 1 1 d . . . H11A H 0.4564 0.8987 0.3212 0.110 Uiso 1 1 calc R . . H11B H 0.3868 0.8636 0.3733 0.110 Uiso 1 1 calc R . . H11C H 0.4287 0.8130 0.3168 0.110 Uiso 1 1 calc R . . C12 C 0.5392(4) 0.8949(3) 0.4388(2) 0.0734(15) Uani 1 1 d . . . H12A H 0.5454 0.9426 0.4167 0.110 Uiso 1 1 calc R . . H12B H 0.5961 0.8843 0.4631 0.110 Uiso 1 1 calc R . . H12C H 0.4865 0.8969 0.4688 0.110 Uiso 1 1 calc R . . C13 C 0.7885(2) 0.5104(2) 0.3980(2) 0.0539(9) Uani 1 1 d . . . H13A H 0.7779 0.4597 0.3884 0.065 Uiso 1 1 calc R . . C14 C 0.8564(3) 0.5482(2) 0.3632(3) 0.0672(13) Uani 1 1 d . . . H14A H 0.8923 0.5228 0.3316 0.081 Uiso 1 1 calc R . . C15 C 0.8713(2) 0.6215(2) 0.3741(3) 0.0650(12) Uani 1 1 d . . . H15A H 0.9171 0.6477 0.3502 0.078 Uiso 1 1 calc R . . C16 C 0.8191(2) 0.6569(2) 0.4203(2) 0.0565(11) Uani 1 1 d . . . C17 C 0.8267(3) 0.7341(2) 0.4364(3) 0.0678(14) Uani 1 1 d . . . H17A H 0.8682 0.7645 0.4125 0.081 Uiso 1 1 calc R . . C18 C 0.7765(3) 0.7641(2) 0.4843(3) 0.0697(15) Uani 1 1 d . . . H18A H 0.7834 0.8154 0.4935 0.084 Uiso 1 1 calc R . . C19 C 0.7135(3) 0.72165(18) 0.5216(2) 0.0567(11) Uani 1 1 d . . . C20 C 0.6606(4) 0.7488(2) 0.5732(2) 0.0683(14) Uani 1 1 d . . . H20A H 0.6654 0.7992 0.5857 0.082 Uiso 1 1 calc R . . C21 C 0.6030(4) 0.7029(2) 0.6049(2) 0.0672(13) Uani 1 1 d . . . H21A H 0.5671 0.7209 0.6402 0.081 Uiso 1 1 calc R . . C22 C 0.5958(3) 0.62855(19) 0.58618(18) 0.0478(9) Uani 1 1 d . . . H22A H 0.5539 0.5973 0.6090 0.057 Uiso 1 1 calc R . . C23 C 0.7031(2) 0.64664(16) 0.50673(19) 0.0426(8) Uani 1 1 d . . . C24 C 0.7552(2) 0.61492(18) 0.45557(19) 0.0449(8) Uani 1 1 d . . . C25 C 0.5426(2) 0.55992(17) 0.38443(16) 0.0394(7) Uani 1 1 d . . . H25A H 0.6010 0.5688 0.3644 0.047 Uiso 1 1 calc R . . C26 C 0.4617(3) 0.5782(2) 0.35095(17) 0.0452(8) Uani 1 1 d . . . H26A H 0.4662 0.5991 0.3088 0.054 Uiso 1 1 calc R . . C27 C 0.3763(2) 0.56681(18) 0.37749(17) 0.0423(7) Uani 1 1 d . . . H27A H 0.3214 0.5809 0.3551 0.051 Uiso 1 1 calc R . . C28 C 0.3720(2) 0.53371(16) 0.43870(14) 0.0334(6) Uani 1 1 d . . . C29 C 0.2878(2) 0.51606(17) 0.47056(16) 0.0394(7) Uani 1 1 d . . . H29A H 0.2304 0.5271 0.4500 0.047 Uiso 1 1 calc R . . C30 C 0.45534(19) 0.51700(14) 0.46901(14) 0.0279(5) Uani 1 1 d . . . O1W O 1.0000 0.7054(2) 0.2500 0.0711(12) Uani 1 2 d S . . H1WA H 0.9529 0.7115 0.2734 0.107 Uiso 0.50 1 calc PR . . H1WB H 1.0239 0.6709 0.2726 0.107 Uiso 0.50 1 d PR . . O2W O 1.0054(6) 0.8526(3) 0.2292(3) 0.059(2) Uani 0.50 1 d P . . H2WA H 0.9730 0.8853 0.2113 0.089 Uiso 0.50 1 calc PR . . H2WB H 1.0057 0.8150 0.2540 0.089 Uiso 0.50 1 d PR . . O3W O 0.8935(4) 0.5786(4) 0.1276(4) 0.079(2) Uani 0.50 1 d P A 1 H3WA H 0.8674 0.6180 0.1393 0.118 Uiso 0.50 1 calc PR A 1 H3WB H 0.8628 0.5403 0.1382 0.118 Uiso 0.50 1 d PR A 1 O4W O 0.9361(7) 0.5701(6) 0.1925(7) 0.064(3) Uani 0.25 1 d PU B 2 H4WA H 0.8995 0.6015 0.2083 0.096 Uiso 0.25 1 calc PR B 2 H4WB H 0.9718 0.5710 0.2252 0.096 Uiso 0.25 1 d PR B 2 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 Fe1 0.0241(2) 0.0243(3) 0.0483(3) -0.0047(2) 0.000 0.000 N1 0.0223(11) 0.0281(12) 0.0694(18) 0.0014(12) 0.0013(11) 0.0003(9) N2 0.0388(13) 0.0283(12) 0.0513(15) -0.0071(10) -0.0179(12) 0.0039(11) N3 0.0299(12) 0.0305(12) 0.0361(13) -0.0017(10) 0.0025(10) -0.0032(9) O1 0.0469(12) 0.0136(8) 0.0489(12) 0.0003(8) 0.0194(10) -0.0039(8) O2 0.0828(19) 0.0179(9) 0.0857(19) -0.0134(11) 0.0552(16) -0.0135(11) O3 0.0455(12) 0.0193(9) 0.0675(14) 0.0030(9) 0.0202(12) 0.0016(9) O4 0.0551(13) 0.0115(8) 0.0773(16) 0.0067(9) 0.0265(12) 0.0039(9) C1 0.0368(14) 0.0145(10) 0.0337(13) -0.0007(9) 0.0038(11) -0.0006(10) C2 0.0304(13) 0.0190(12) 0.0347(13) 0.0000(10) 0.0065(11) -0.0016(10) C3 0.0346(14) 0.0145(11) 0.0316(13) 0.0001(9) -0.0012(11) 0.0006(10) C4 0.0344(14) 0.0173(11) 0.0338(13) -0.0032(9) -0.0013(11) 0.0036(10) C5 0.0319(13) 0.0223(12) 0.0298(13) -0.0005(10) 0.0011(10) 0.0034(10) C6 0.0374(15) 0.0169(11) 0.0349(13) 0.0014(9) 0.0057(12) -0.0029(10) C7 0.0468(18) 0.0160(11) 0.0452(16) -0.0046(11) 0.0156(14) -0.0056(11) C8 0.0349(14) 0.0191(12) 0.0437(15) 0.0014(11) 0.0051(12) 0.0005(11) C9 0.0384(15) 0.0305(14) 0.0381(15) -0.0059(12) 0.0094(13) 0.0023(12) C10 0.060(2) 0.048(2) 0.091(3) 0.012(2) 0.040(2) 0.0064(18) C11 0.045(2) 0.106(4) 0.069(3) -0.007(3) 0.0050(19) 0.035(2) C12 0.086(3) 0.068(3) 0.066(3) -0.034(2) 0.038(2) -0.018(2) C13 0.0328(15) 0.0381(18) 0.091(3) 0.0044(18) 0.0189(16) 0.0008(14) C14 0.0333(17) 0.052(2) 0.116(4) 0.021(2) 0.027(2) 0.0104(17) C15 0.0224(15) 0.052(2) 0.121(4) 0.030(2) 0.0102(19) -0.0007(14) C16 0.0289(16) 0.0390(18) 0.102(3) 0.0236(19) -0.0210(19) -0.0065(13) C17 0.046(2) 0.0384(19) 0.119(4) 0.023(2) -0.029(2) -0.0159(16) C18 0.068(3) 0.0285(16) 0.112(4) 0.004(2) -0.045(3) -0.0090(17) C19 0.061(2) 0.0282(15) 0.081(3) -0.0006(16) -0.039(2) -0.0013(15) C20 0.102(4) 0.0288(17) 0.074(3) -0.0103(18) -0.046(3) 0.013(2) C21 0.098(3) 0.043(2) 0.060(2) -0.0189(18) -0.035(2) 0.026(2) C22 0.055(2) 0.0378(18) 0.051(2) -0.0105(14) -0.0165(16) 0.0117(15) C23 0.0361(14) 0.0257(13) 0.066(2) -0.0021(14) -0.0228(16) 0.0018(11) C24 0.0258(14) 0.0318(15) 0.077(2) 0.0077(15) -0.0144(15) -0.0020(11) C25 0.0388(16) 0.0369(16) 0.0427(17) 0.0009(13) 0.0110(13) -0.0073(13) C26 0.055(2) 0.0415(17) 0.0392(17) 0.0095(14) 0.0016(15) -0.0051(15) C27 0.0428(18) 0.0399(17) 0.0442(17) 0.0057(13) -0.0055(14) 0.0027(14) C28 0.0347(15) 0.0305(13) 0.0349(13) 0.0002(11) -0.0019(12) 0.0011(11) C29 0.0252(13) 0.0448(19) 0.0481(16) 0.0052(13) -0.0032(12) -0.0001(11) C30 0.0282(13) 0.0236(13) 0.0319(13) -0.0023(10) 0.0016(10) -0.0027(9) O1W 0.080(3) 0.044(2) 0.089(3) 0.000 0.005(3) 0.000 O2W 0.047(3) 0.034(2) 0.098(6) 0.004(2) -0.016(5) 0.001(2) O3W 0.063(4) 0.052(3) 0.121(6) -0.039(4) 0.048(4) -0.023(3) O4W 0.027(4) 0.056(5) 0.110(7) -0.035(5) 0.043(5) -0.017(4) _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 Fe1 N3 1.961(3) . ? Fe1 N3 1.961(3) 3_566 ? Fe1 N1 1.963(3) 3_566 ? Fe1 N1 1.963(3) . ? Fe1 N2 1.976(2) 3_566 ? Fe1 N2 1.976(2) . ? N1 C13 1.314(5) . ? N1 C24 1.365(4) . ? N2 C22 1.316(5) . ? N2 C23 1.356(4) . ? N3 C25 1.312(4) . ? N3 C30 1.365(4) . ? O1 C7 1.280(3) . ? O2 C7 1.217(4) . ? O3 C8 1.225(4) . ? O4 C8 1.280(3) . ? O4 H4 0.8400 . ? C1 C6 1.378(4) . ? C1 C2 1.381(4) . ? C1 C7 1.497(4) . ? C2 C3 1.383(4) . ? C2 H2A 0.9500 . ? C3 C4 1.392(4) . ? C3 C8 1.488(4) . ? C4 C5 1.387(4) . ? C4 H4A 0.9500 . ? C5 C6 1.382(4) . ? C5 C9 1.521(4) . ? C6 H6A 0.9500 . ? C9 C11 1.511(6) . ? C9 C12 1.513(5) . ? C9 C10 1.533(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.393(5) . ? C13 H13A 0.9500 . ? C14 C15 1.360(6) . ? C14 H14A 0.9500 . ? C15 C16 1.371(7) . ? C15 H15A 0.9500 . ? C16 C24 1.397(5) . ? C16 C17 1.439(6) . ? C17 C18 1.338(7) . ? C17 H17A 0.9500 . ? C18 C19 1.417(7) . ? C18 H18A 0.9500 . ? C19 C20 1.397(7) . ? C19 C23 1.398(4) . ? C20 C21 1.343(8) . ? C20 H20A 0.9500 . ? C21 C22 1.401(5) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C24 1.416(5) . ? C25 C26 1.395(5) . ? C25 H25A 0.9500 . ? C26 C27 1.362(5) . ? C26 H26A 0.9500 . ? C27 C28 1.398(4) . ? C27 H27A 0.9500 . ? C28 C30 1.387(4) . ? C28 C29 1.416(4) . ? C29 C29 1.346(7) 3_566 ? C29 H29A 0.9500 . ? C30 C30 1.418(6) 3_566 ? O1W H1WA 0.8400 . ? O1W H1WB 0.8499 . ? O2W O2W 0.872(11) 4_755 ? O2W H2WA 0.8400 . ? O2W H2WB 0.8500 . ? O3W H3WA 0.8400 . ? O3W H3WB 0.8500 . ? O4W H4WA 0.8400 . ? O4W H4WB 0.8499 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Fe1 N3 83.58(14) . 3_566 ? N3 Fe1 N1 173.82(11) . 3_566 ? N3 Fe1 N1 93.59(10) 3_566 3_566 ? N3 Fe1 N1 93.59(10) . . ? N3 Fe1 N1 173.82(11) 3_566 . ? N1 Fe1 N1 89.74(16) 3_566 . ? N3 Fe1 N2 91.90(11) . 3_566 ? N3 Fe1 N2 89.72(10) 3_566 3_566 ? N1 Fe1 N2 82.57(12) 3_566 3_566 ? N1 Fe1 N2 95.88(11) . 3_566 ? N3 Fe1 N2 89.72(10) . . ? N3 Fe1 N2 91.90(11) 3_566 . ? N1 Fe1 N2 95.88(11) 3_566 . ? N1 Fe1 N2 82.57(12) . . ? N2 Fe1 N2 177.83(17) 3_566 . ? C13 N1 C24 116.8(3) . . ? C13 N1 Fe1 130.2(2) . . ? C24 N1 Fe1 113.0(2) . . ? C22 N2 C23 116.9(3) . . ? C22 N2 Fe1 130.3(3) . . ? C23 N2 Fe1 112.7(2) . . ? C25 N3 C30 117.3(3) . . ? C25 N3 Fe1 130.5(2) . . ? C30 N3 Fe1 112.24(19) . . ? C8 O4 H4 109.5 . . ? C6 C1 C2 120.4(2) . . ? C6 C1 C7 121.6(2) . . ? C2 C1 C7 118.0(2) . . ? C1 C2 C3 119.3(3) . . ? C1 C2 H2A 120.4 . . ? C3 C2 H2A 120.4 . . ? C2 C3 C4 119.7(2) . . ? C2 C3 C8 119.3(2) . . ? C4 C3 C8 120.9(2) . . ? C5 C4 C3 121.4(2) . . ? C5 C4 H4A 119.3 . . ? C3 C4 H4A 119.3 . . ? C6 C5 C4 117.7(2) . . ? C6 C5 C9 121.4(2) . . ? C4 C5 C9 120.8(2) . . ? C1 C6 C5 121.5(2) . . ? C1 C6 H6A 119.3 . . ? C5 C6 H6A 119.3 . . ? O2 C7 O1 123.6(3) . . ? O2 C7 C1 120.6(2) . . ? O1 C7 C1 115.8(3) . . ? O3 C8 O4 123.4(3) . . ? O3 C8 C3 121.4(2) . . ? O4 C8 C3 115.1(3) . . ? C11 C9 C12 110.3(4) . . ? C11 C9 C5 107.5(3) . . ? C12 C9 C5 111.0(3) . . ? C11 C9 C10 108.2(4) . . ? C12 C9 C10 108.3(3) . . ? C5 C9 C10 111.6(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C14 122.9(4) . . ? N1 C13 H13A 118.6 . . ? C14 C13 H13A 118.6 . . ? C15 C14 C13 120.2(4) . . ? C15 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? C14 C15 C16 118.8(4) . . ? C14 C15 H15A 120.6 . . ? C16 C15 H15A 120.6 . . ? C15 C16 C24 118.0(3) . . ? C15 C16 C17 124.8(4) . . ? C24 C16 C17 117.1(4) . . ? C18 C17 C16 121.5(4) . . ? C18 C17 H17A 119.3 . . ? C16 C17 H17A 119.3 . . ? C17 C18 C19 121.9(3) . . ? C17 C18 H18A 119.1 . . ? C19 C18 H18A 119.1 . . ? C20 C19 C23 116.7(4) . . ? C20 C19 C18 125.0(4) . . ? C23 C19 C18 118.3(4) . . ? C21 C20 C19 119.4(3) . . ? C21 C20 H20A 120.3 . . ? C19 C20 H20A 120.3 . . ? C20 C21 C22 120.2(4) . . ? C20 C21 H21A 119.9 . . ? C22 C21 H21A 119.9 . . ? N2 C22 C21 122.7(4) . . ? N2 C22 H22A 118.7 . . ? C21 C22 H22A 118.7 . . ? N2 C23 C19 124.1(4) . . ? N2 C23 C24 115.9(3) . . ? C19 C23 C24 120.0(4) . . ? N1 C24 C16 123.2(4) . . ? N1 C24 C23 115.6(3) . . ? C16 C24 C23 121.2(3) . . ? N3 C25 C26 122.0(3) . . ? N3 C25 H25A 119.0 . . ? C26 C25 H25A 119.0 . . ? C27 C26 C25 121.3(3) . . ? C27 C26 H26A 119.3 . . ? C25 C26 H26A 119.3 . . ? C26 C27 C28 117.9(3) . . ? C26 C27 H27A 121.1 . . ? C28 C27 H27A 121.1 . . ? C30 C28 C27 117.5(3) . . ? C30 C28 C29 118.9(3) . . ? C27 C28 C29 123.6(3) . . ? C29 C29 C28 121.05(17) 3_566 . ? C29 C29 H29A 119.5 3_566 . ? C28 C29 H29A 119.5 . . ? N3 C30 C28 124.0(3) . . ? N3 C30 C30 115.96(16) . 3_566 ? C28 C30 C30 120.04(16) . 3_566 ? H1WA O1W H1WB 96.2 . . ? O2W O2W H2WA 109.5 4_755 . ? O2W O2W H2WB 53.8 4_755 . ? H2WA O2W H2WB 146.1 . . ? H3WA O3W H3WB 112.6 . . ? H4WA O4W H4WB 93.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Fe1 N1 C13 80.4(3) 3_566 . . . ? N2 Fe1 N1 C13 -2.1(4) 3_566 . . . ? N2 Fe1 N1 C13 176.4(3) . . . . ? N1 Fe1 N1 C24 -99.0(3) 3_566 . . . ? N2 Fe1 N1 C24 178.5(2) 3_566 . . . ? N2 Fe1 N1 C24 -3.0(2) . . . . ? N3 Fe1 N2 C22 85.9(3) . . . . ? N3 Fe1 N2 C22 2.4(3) 3_566 . . . ? N1 Fe1 N2 C22 -91.4(3) 3_566 . . . ? N1 Fe1 N2 C22 179.6(3) . . . . ? N3 Fe1 N2 C23 -90.0(2) . . . . ? N3 Fe1 N2 C23 -173.5(2) 3_566 . . . ? N1 Fe1 N2 C23 92.6(2) 3_566 . . . ? N1 Fe1 N2 C23 3.7(2) . . . . ? N3 Fe1 N3 C25 -177.9(3) 3_566 . . . ? N1 Fe1 N3 C25 7.6(3) . . . . ? N2 Fe1 N3 C25 -88.4(3) 3_566 . . . ? N2 Fe1 N3 C25 90.2(3) . . . . ? N3 Fe1 N3 C30 0.24(13) 3_566 . . . ? N1 Fe1 N3 C30 -174.2(2) . . . . ? N2 Fe1 N3 C30 89.7(2) 3_566 . . . ? N2 Fe1 N3 C30 -91.7(2) . . . . ? C6 C1 C2 C3 -1.1(4) . . . . ? C7 C1 C2 C3 176.7(3) . . . . ? C1 C2 C3 C4 0.9(4) . . . . ? C1 C2 C3 C8 -175.8(3) . . . . ? C2 C3 C4 C5 -0.3(4) . . . . ? C8 C3 C4 C5 176.4(3) . . . . ? C3 C4 C5 C6 -0.2(4) . . . . ? C3 C4 C5 C9 -176.0(3) . . . . ? C2 C1 C6 C5 0.6(4) . . . . ? C7 C1 C6 C5 -177.1(3) . . . . ? C4 C5 C6 C1 0.0(4) . . . . ? C9 C5 C6 C1 175.8(3) . . . . ? C6 C1 C7 O2 178.4(3) . . . . ? C2 C1 C7 O2 0.5(5) . . . . ? C6 C1 C7 O1 -2.9(5) . . . . ? C2 C1 C7 O1 179.3(3) . . . . ? C2 C3 C8 O3 -11.0(5) . . . . ? C4 C3 C8 O3 172.2(3) . . . . ? C2 C3 C8 O4 167.8(3) . . . . ? C4 C3 C8 O4 -8.9(4) . . . . ? C6 C5 C9 C11 -94.4(4) . . . . ? C4 C5 C9 C11 81.3(4) . . . . ? C6 C5 C9 C12 144.9(4) . . . . ? C4 C5 C9 C12 -39.4(4) . . . . ? C6 C5 C9 C10 24.1(4) . . . . ? C4 C5 C9 C10 -160.3(3) . . . . ? C24 N1 C13 C14 0.8(6) . . . . ? Fe1 N1 C13 C14 -178.6(3) . . . . ? N1 C13 C14 C15 -2.3(7) . . . . ? C13 C14 C15 C16 0.6(7) . . . . ? C14 C15 C16 C24 2.3(6) . . . . ? C14 C15 C16 C17 -179.3(4) . . . . ? C15 C16 C17 C18 -176.7(4) . . . . ? C24 C16 C17 C18 1.7(6) . . . . ? C16 C17 C18 C19 0.0(6) . . . . ? C17 C18 C19 C20 178.4(4) . . . . ? C17 C18 C19 C23 -1.0(6) . . . . ? C23 C19 C20 C21 -0.6(5) . . . . ? C18 C19 C20 C21 179.9(4) . . . . ? C19 C20 C21 C22 -0.3(6) . . . . ? C23 N2 C22 C21 -0.5(5) . . . . ? Fe1 N2 C22 C21 -176.2(3) . . . . ? C20 C21 C22 N2 0.9(6) . . . . ? C22 N2 C23 C19 -0.6(5) . . . . ? Fe1 N2 C23 C19 176.0(3) . . . . ? C22 N2 C23 C24 179.8(3) . . . . ? Fe1 N2 C23 C24 -3.7(3) . . . . ? C20 C19 C23 N2 1.1(5) . . . . ? C18 C19 C23 N2 -179.4(3) . . . . ? C20 C19 C23 C24 -179.3(3) . . . . ? C18 C19 C23 C24 0.2(5) . . . . ? C13 N1 C24 C16 2.4(5) . . . . ? Fe1 N1 C24 C16 -178.2(3) . . . . ? C13 N1 C24 C23 -177.6(3) . . . . ? Fe1 N1 C24 C23 1.9(4) . . . . ? C15 C16 C24 N1 -3.9(5) . . . . ? C17 C16 C24 N1 177.5(3) . . . . ? C15 C16 C24 C23 176.0(3) . . . . ? C17 C16 C24 C23 -2.5(5) . . . . ? N2 C23 C24 N1 1.2(4) . . . . ? C19 C23 C24 N1 -178.5(3) . . . . ? N2 C23 C24 C16 -178.7(3) . . . . ? C19 C23 C24 C16 1.6(5) . . . . ? C30 N3 C25 C26 1.8(4) . . . . ? Fe1 N3 C25 C26 179.9(2) . . . . ? N3 C25 C26 C27 0.1(5) . . . . ? C25 C26 C27 C28 -2.1(5) . . . . ? C26 C27 C28 C30 2.0(4) . . . . ? C26 C27 C28 C29 -177.4(3) . . . . ? C30 C28 C29 C29 0.3(6) . . . 3_566 ? C27 C28 C29 C29 179.8(4) . . . 3_566 ? C25 N3 C30 C28 -1.9(4) . . . . ? Fe1 N3 C30 C28 179.7(2) . . . . ? C25 N3 C30 C30 177.7(3) . . . 3_566 ? Fe1 N3 C30 C30 -0.7(4) . . . 3_566 ? C27 C28 C30 N3 -0.1(4) . . . . ? C29 C28 C30 N3 179.4(3) . . . . ? C27 C28 C30 C30 -179.6(3) . . . 3_566 ? C29 C28 C30 C30 -0.2(5) . . . 3_566 ? 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 O4 H4 O1 0.84 1.62 2.447(3) 167.4 8_655 O1W H1WB O2 0.85 2.63 3.128(3) 118.5 4_755 O2W H2WA O3 0.84 2.01 2.713(8) 140.1 . O2W H2WB O1W 0.85 1.98 2.695(6) 140.5 . O3W H3WA O2 0.84 2.07 2.792(6) 144.1 . O3W H3WB O4 0.85 2.52 3.174(7) 134.8 8_645 O4W H4WA O2 0.84 1.94 2.736(11) 158.6 . _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.040 _refine_diff_density_min -0.293 _refine_diff_density_rms 0.083 #============================================================================== data_CoBpy1-[Co(bpy)(tbip)(H2O)]4 _database_code_depnum_ccdc_archive 'CCDC 835409' #TrackingRef '- revised cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C88 H88 Co4 N8 O20' _chemical_formula_sum 'C88 H88 Co4 N8 O20' _chemical_formula_weight 1813.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2581(6) _cell_length_b 13.0985(9) _cell_length_c 18.1773(12) _cell_angle_alpha 97.650(1) _cell_angle_beta 97.648(1) _cell_angle_gamma 107.288(1) _cell_volume 2051.0(2) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2710 _cell_measurement_theta_min 2.3433 _cell_measurement_theta_max 26.8798 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 940 _exptl_absorpt_coefficient_mu 0.873 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7796 _exptl_absorpt_correction_T_max 0.9177 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12847 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_sigmaI/netI 0.0941 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 28.85 _reflns_number_total 9265 _reflns_number_gt 6860 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. SADI 0.01 is applied to the twelve C-C distances of the disordered tert-butyl. EADP is also applied to the disorderd carbon atoms. ; _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^)+(0.0914P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9265 _refine_ls_number_parameters 548 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0928 _refine_ls_R_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.1836 _refine_ls_wR_factor_gt 0.1641 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.01870(6) 0.23739(4) 0.53508(3) 0.01673(15) Uani 1 1 d . . . Co2 Co 0.32720(6) 0.46239(4) 0.11641(3) 0.01944(15) Uani 1 1 d . . . O1 O 0.2050(3) 0.1979(2) 0.49588(15) 0.0241(6) Uani 1 1 d . . . O1W O -0.1320(3) 0.0787(2) 0.49280(15) 0.0221(6) Uani 1 1 d . . . H1WA H -0.1158 0.0380 0.5211 0.033 Uiso 1 1 calc R . . H1WB H -0.1017 0.0521 0.4548 0.033 Uiso 1 1 d R . . O2 O 0.0554(3) 0.2566(2) 0.41991(16) 0.0240(6) Uani 1 1 d . . . O2W O 0.4823(3) 0.4007(3) 0.06838(16) 0.0299(7) Uani 1 1 d . . . H2WB H 0.4793 0.3428 0.0817 0.045 Uiso 1 1 calc R . . H2WA H 0.4880 0.4029 0.0223 0.045 Uiso 1 1 d R . . O3 O 0.2953(3) 0.3547(2) 0.18778(16) 0.0247(6) Uani 1 1 d . . . O4 O 0.4010(4) 0.2382(3) 0.13431(18) 0.0416(9) Uani 1 1 d . . . O5 O 0.4953(3) 0.5888(2) 0.18654(16) 0.0305(7) Uani 1 1 d . . . O6 O 0.4484(3) 0.6248(2) 0.07393(15) 0.0253(7) Uani 1 1 d . . . O7 O 0.9646(3) 0.7988(2) 0.35955(15) 0.0221(6) Uani 1 1 d . . . O8 O 0.9908(3) 0.9760(2) 0.38414(15) 0.0244(6) Uani 1 1 d . . . N1 N 0.1516(4) 0.3978(3) 0.58886(17) 0.0177(7) Uani 1 1 d . . . N2 N -0.1438(3) 0.3183(3) 0.53849(17) 0.0173(7) Uani 1 1 d . . . N3 N 0.1514(4) 0.5164(3) 0.15621(18) 0.0221(7) Uani 1 1 d . . . N4 N 0.1316(4) 0.3806(3) 0.03295(18) 0.0222(7) Uani 1 1 d . . . C1 C 0.2452(4) 0.1908(3) 0.3693(2) 0.0181(8) Uani 1 1 d . . . C2 C 0.2475(4) 0.2423(3) 0.3076(2) 0.0211(8) Uani 1 1 d . . . H2A H 0.2003 0.2955 0.3043 0.025 Uiso 1 1 calc R . . C3 C 0.3221(4) 0.2131(3) 0.2501(2) 0.0197(8) Uani 1 1 d . . . C4 C 0.3845(4) 0.1304(3) 0.2544(2) 0.0200(8) Uani 1 1 d . . . H4A H 0.4297 0.1091 0.2148 0.024 Uiso 1 1 calc R . . C5 C 0.3822(4) 0.0773(3) 0.3161(2) 0.0213(8) Uani 1 1 d . . . C6 C 0.3135(4) 0.1113(3) 0.3739(2) 0.0211(8) Uani 1 1 d . . . H6A H 0.3137 0.0796 0.4167 0.025 Uiso 1 1 calc R . . C7 C 0.1633(4) 0.2173(3) 0.4313(2) 0.0194(8) Uani 1 1 d . . . C8 C 0.3402(5) 0.2724(3) 0.1851(2) 0.0231(9) Uani 1 1 d . . . C9 C 0.4539(6) -0.0120(4) 0.3179(2) 0.0314(10) Uani 1 1 d . . . C10 C 0.4275(8) -0.0685(5) 0.3850(3) 0.0548(16) Uani 1 1 d . . . H10A H 0.3190 -0.1019 0.3824 0.082 Uiso 1 1 calc R . . H10B H 0.4693 -0.0161 0.4310 0.082 Uiso 1 1 calc R . . H10C H 0.4773 -0.1232 0.3841 0.082 Uiso 1 1 calc R . . C11 C 0.3849(7) -0.0982(4) 0.2457(3) 0.0476(14) Uani 1 1 d . . . H11A H 0.2766 -0.1309 0.2439 0.071 Uiso 1 1 calc R . . H11B H 0.4342 -0.1532 0.2457 0.071 Uiso 1 1 calc R . . H11C H 0.4008 -0.0645 0.2024 0.071 Uiso 1 1 calc R . . C12 C 0.6276(6) 0.0375(5) 0.3229(3) 0.0501(15) Uani 1 1 d . . . H12A H 0.6679 0.0975 0.3645 0.075 Uiso 1 1 calc R . . H12B H 0.6477 0.0627 0.2769 0.075 Uiso 1 1 calc R . . H12C H 0.6761 -0.0166 0.3304 0.075 Uiso 1 1 calc R . . C13 C 0.6478(4) 0.7580(3) 0.1668(2) 0.0180(8) Uani 1 1 d . . . C14 C 0.7402(4) 0.7739(3) 0.2365(2) 0.0185(8) Uani 1 1 d . . . H14A H 0.7247 0.7186 0.2647 0.022 Uiso 1 1 calc R . . C15 C 0.8551(4) 0.8714(3) 0.2643(2) 0.0184(8) Uani 1 1 d . . . C16 C 0.8774(4) 0.9537(3) 0.2228(2) 0.0207(8) Uani 1 1 d . . . H16A H 0.9536 1.0199 0.2426 0.025 Uiso 1 1 calc R . . C17 C 0.7880(5) 0.9398(3) 0.1520(2) 0.0232(9) Uani 1 1 d . A . C18 C 0.6728(5) 0.8411(3) 0.1254(2) 0.0217(9) Uani 1 1 d . . . H18A H 0.6108 0.8303 0.0785 0.026 Uiso 1 1 calc R . . C19 C 0.5230(4) 0.6514(3) 0.1401(2) 0.0214(8) Uani 1 1 d . . . C20 C 0.9459(4) 0.8852(3) 0.3427(2) 0.0175(8) Uani 1 1 d . . . C21 C 0.8154(5) 1.0304(4) 0.1061(3) 0.0359(11) Uani 1 1 d D . . C22 C 0.9856(8) 1.0600(8) 0.0973(6) 0.0592(16) Uani 0.665(7) 1 d PD A 1 H22A H 1.0504 1.0904 0.1459 0.089 Uiso 0.665(7) 1 calc PR A 1 H22B H 1.0063 1.1123 0.0645 0.089 Uiso 0.665(7) 1 calc PR A 1 H22C H 1.0061 0.9958 0.0761 0.089 Uiso 0.665(7) 1 calc PR A 1 C23 C 0.7161(11) 1.0021(8) 0.0289(4) 0.0592(16) Uani 0.665(7) 1 d PD A 1 H23A H 0.6110 0.9918 0.0339 0.089 Uiso 0.665(7) 1 calc PR A 1 H23B H 0.7239 0.9363 0.0020 0.089 Uiso 0.665(7) 1 calc PR A 1 H23C H 0.7501 1.0601 0.0017 0.089 Uiso 0.665(7) 1 calc PR A 1 C24 C 0.8094(11) 1.1347(6) 0.1534(5) 0.0592(16) Uani 0.665(7) 1 d PD A 1 H24A H 0.8660 1.1449 0.2035 0.089 Uiso 0.665(7) 1 calc PR A 1 H24B H 0.7043 1.1287 0.1557 0.089 Uiso 0.665(7) 1 calc PR A 1 H24C H 0.8541 1.1958 0.1305 0.089 Uiso 0.665(7) 1 calc PR A 1 C22' C 0.6780(15) 1.0735(14) 0.1032(10) 0.0592(16) Uani 0.335(7) 1 d PD A 2 H22D H 0.6708 1.1022 0.1535 0.089 Uiso 0.335(7) 1 calc PR A 2 H22E H 0.5851 1.0152 0.0807 0.089 Uiso 0.335(7) 1 calc PR A 2 H22F H 0.6922 1.1299 0.0735 0.089 Uiso 0.335(7) 1 calc PR A 2 C23' C 0.9713(14) 1.1156(14) 0.1198(11) 0.0592(16) Uani 0.335(7) 1 d PD A 2 H23D H 0.9894 1.1601 0.1687 0.089 Uiso 0.335(7) 1 calc PR A 2 H23E H 0.9751 1.1601 0.0818 0.089 Uiso 0.335(7) 1 calc PR A 2 H23F H 1.0489 1.0809 0.1178 0.089 Uiso 0.335(7) 1 calc PR A 2 C24' C 0.782(2) 0.9791(14) 0.0218(5) 0.0592(16) Uani 0.335(7) 1 d PD A 2 H24D H 0.6867 0.9198 0.0109 0.089 Uiso 0.335(7) 1 calc PR A 2 H24E H 0.8637 0.9527 0.0103 0.089 Uiso 0.335(7) 1 calc PR A 2 H24F H 0.7731 1.0328 -0.0082 0.089 Uiso 0.335(7) 1 calc PR A 2 C25 C 0.3005(4) 0.4282(4) 0.6199(2) 0.0254(9) Uani 1 1 d . . . H25A H 0.3525 0.3775 0.6151 0.030 Uiso 1 1 calc R . . C26 C 0.3804(5) 0.5327(4) 0.6588(3) 0.0327(11) Uani 1 1 d . . . H26A H 0.4831 0.5514 0.6816 0.039 Uiso 1 1 calc R . . C27 C 0.3042(5) 0.6076(4) 0.6629(3) 0.0361(11) Uani 1 1 d . . . H27A H 0.3563 0.6791 0.6867 0.043 Uiso 1 1 calc R . . C28 C 0.1499(5) 0.5773(3) 0.6316(2) 0.0276(10) Uani 1 1 d . . . H28A H 0.0967 0.6274 0.6343 0.033 Uiso 1 1 calc R . . C29 C 0.0765(4) 0.4703(3) 0.5963(2) 0.0196(8) Uani 1 1 d . . . C30 C -0.0917(4) 0.4251(3) 0.5675(2) 0.0183(8) Uani 1 1 d . . . C31 C -0.1887(5) 0.4861(3) 0.5718(2) 0.0248(9) Uani 1 1 d . . . H31A H -0.1495 0.5604 0.5906 0.030 Uiso 1 1 calc R . . C32 C -0.3453(5) 0.4363(4) 0.5480(3) 0.0303(10) Uani 1 1 d . . . H32A H -0.4129 0.4761 0.5515 0.036 Uiso 1 1 calc R . . C33 C -0.3997(5) 0.3256(4) 0.5186(3) 0.0300(10) Uani 1 1 d . . . H33A H -0.5044 0.2898 0.5022 0.036 Uiso 1 1 calc R . . C34 C -0.2964(4) 0.2705(3) 0.5144(2) 0.0251(9) Uani 1 1 d . . . H34A H -0.3327 0.1966 0.4939 0.030 Uiso 1 1 calc R . . C35 C 0.1708(6) 0.5887(4) 0.2195(2) 0.0314(10) Uani 1 1 d . . . H35A H 0.2700 0.6229 0.2467 0.038 Uiso 1 1 calc R . . C36 C 0.0519(7) 0.6145(4) 0.2459(3) 0.0389(12) Uani 1 1 d . . . H36A H 0.0695 0.6664 0.2891 0.047 Uiso 1 1 calc R . . C37 C -0.0963(7) 0.5602(4) 0.2058(3) 0.0428(13) Uani 1 1 d . . . H37A H -0.1803 0.5739 0.2228 0.051 Uiso 1 1 calc R . . C38 C -0.1179(6) 0.4862(4) 0.1408(3) 0.0361(11) Uani 1 1 d . . . H38A H -0.2164 0.4496 0.1135 0.043 Uiso 1 1 calc R . . C39 C 0.0077(5) 0.4669(3) 0.1166(2) 0.0237(9) Uani 1 1 d . . . C40 C -0.0017(5) 0.3910(3) 0.0471(2) 0.0226(9) Uani 1 1 d . . . C41 C -0.1396(5) 0.3358(4) -0.0026(3) 0.0314(11) Uani 1 1 d . . . H41A H -0.2312 0.3457 0.0069 0.038 Uiso 1 1 calc R . . C42 C -0.1376(5) 0.2667(4) -0.0656(3) 0.0374(12) Uani 1 1 d . . . H42A H -0.2289 0.2278 -0.0988 0.045 Uiso 1 1 calc R . . C43 C -0.0023(6) 0.2550(4) -0.0795(2) 0.0360(11) Uani 1 1 d . . . H43A H 0.0008 0.2087 -0.1223 0.043 Uiso 1 1 calc R . . C44 C 0.1297(5) 0.3131(4) -0.0289(2) 0.0299(10) Uani 1 1 d . . . H44B H 0.2223 0.3049 -0.0383 0.036 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0182(3) 0.0144(3) 0.0165(3) 0.0001(2) 0.0017(2) 0.0054(2) Co2 0.0186(3) 0.0187(3) 0.0172(3) 0.0030(2) 0.0005(2) 0.0017(2) O1 0.0226(14) 0.0320(17) 0.0199(14) 0.0010(12) 0.0063(11) 0.0126(13) O1W 0.0252(14) 0.0158(14) 0.0226(14) -0.0006(11) 0.0020(11) 0.0055(12) O2 0.0301(15) 0.0211(15) 0.0263(15) 0.0070(12) 0.0096(12) 0.0133(13) O2W 0.0325(16) 0.0371(18) 0.0274(16) 0.0113(14) 0.0130(13) 0.0164(14) O3 0.0284(15) 0.0225(15) 0.0242(15) 0.0086(12) 0.0081(12) 0.0063(13) O4 0.069(2) 0.040(2) 0.0328(19) 0.0156(16) 0.0262(17) 0.0316(19) O5 0.0298(16) 0.0254(17) 0.0237(15) 0.0071(13) -0.0006(13) -0.0085(13) O6 0.0207(14) 0.0315(17) 0.0200(14) 0.0021(12) -0.0021(11) 0.0064(13) O7 0.0329(15) 0.0181(14) 0.0156(13) 0.0032(11) 0.0017(11) 0.0097(12) O8 0.0305(15) 0.0127(14) 0.0235(15) -0.0022(11) 0.0006(12) 0.0014(12) N1 0.0189(16) 0.0164(16) 0.0152(16) 0.0034(13) 0.0027(13) 0.0017(13) N2 0.0167(15) 0.0185(17) 0.0176(16) 0.0011(13) 0.0005(12) 0.0090(13) N3 0.0284(18) 0.0191(18) 0.0191(17) 0.0011(14) 0.0046(14) 0.0089(15) N4 0.0222(17) 0.0196(18) 0.0216(17) 0.0008(14) -0.0020(14) 0.0061(14) C1 0.0176(18) 0.0156(19) 0.0194(19) 0.0018(15) 0.0029(15) 0.0037(15) C2 0.0198(19) 0.017(2) 0.026(2) 0.0017(16) 0.0015(16) 0.0062(16) C3 0.0224(19) 0.0142(19) 0.0192(19) 0.0021(15) -0.0009(15) 0.0032(16) C4 0.0217(19) 0.021(2) 0.0167(19) 0.0012(15) 0.0059(15) 0.0051(16) C5 0.023(2) 0.019(2) 0.021(2) 0.0006(16) 0.0027(16) 0.0077(17) C6 0.0218(19) 0.019(2) 0.0195(19) 0.0029(16) 0.0018(16) 0.0028(16) C7 0.0197(18) 0.0116(19) 0.022(2) 0.0016(15) -0.0001(15) -0.0007(15) C8 0.0214(19) 0.024(2) 0.023(2) 0.0059(17) 0.0018(16) 0.0053(17) C9 0.047(3) 0.035(3) 0.023(2) 0.0073(19) 0.010(2) 0.027(2) C10 0.091(5) 0.059(4) 0.048(3) 0.032(3) 0.036(3) 0.054(4) C11 0.078(4) 0.032(3) 0.041(3) -0.001(2) 0.012(3) 0.032(3) C12 0.049(3) 0.078(4) 0.040(3) 0.015(3) 0.012(3) 0.044(3) C13 0.0174(18) 0.0146(19) 0.0211(19) 0.0023(15) 0.0041(15) 0.0041(15) C14 0.0214(19) 0.0148(19) 0.0203(19) 0.0029(15) 0.0023(15) 0.0078(16) C15 0.0185(18) 0.0157(19) 0.0196(19) -0.0006(15) 0.0015(15) 0.0060(15) C16 0.0206(19) 0.017(2) 0.024(2) 0.0016(16) 0.0064(16) 0.0051(16) C17 0.024(2) 0.021(2) 0.023(2) 0.0056(17) 0.0069(16) 0.0035(17) C18 0.023(2) 0.026(2) 0.0176(19) 0.0060(16) 0.0026(16) 0.0097(17) C19 0.0208(19) 0.024(2) 0.0185(19) 0.0049(16) 0.0040(15) 0.0054(17) C20 0.0175(18) 0.018(2) 0.0168(19) 0.0023(15) 0.0066(15) 0.0042(15) C21 0.044(3) 0.028(3) 0.038(3) 0.015(2) 0.013(2) 0.009(2) C22 0.068(3) 0.048(3) 0.059(3) 0.034(3) 0.005(3) 0.007(3) C23 0.068(3) 0.048(3) 0.059(3) 0.034(3) 0.005(3) 0.007(3) C24 0.068(3) 0.048(3) 0.059(3) 0.034(3) 0.005(3) 0.007(3) C22' 0.068(3) 0.048(3) 0.059(3) 0.034(3) 0.005(3) 0.007(3) C23' 0.068(3) 0.048(3) 0.059(3) 0.034(3) 0.005(3) 0.007(3) C24' 0.068(3) 0.048(3) 0.059(3) 0.034(3) 0.005(3) 0.007(3) C25 0.0177(19) 0.025(2) 0.027(2) 0.0030(18) -0.0007(17) 0.0008(17) C26 0.021(2) 0.035(3) 0.033(2) 0.003(2) -0.0049(18) 0.0017(19) C27 0.034(2) 0.022(2) 0.040(3) -0.002(2) -0.005(2) -0.001(2) C28 0.030(2) 0.017(2) 0.033(2) 0.0015(18) 0.0033(19) 0.0056(18) C29 0.025(2) 0.0149(19) 0.0194(19) 0.0042(15) 0.0051(16) 0.0054(16) C30 0.0229(19) 0.0150(19) 0.0180(19) 0.0059(15) 0.0056(15) 0.0053(16) C31 0.030(2) 0.018(2) 0.027(2) 0.0043(17) 0.0039(18) 0.0096(18) C32 0.027(2) 0.032(3) 0.038(3) 0.008(2) 0.0039(19) 0.019(2) C33 0.020(2) 0.028(2) 0.036(3) 0.002(2) -0.0037(18) 0.0038(18) C34 0.0209(19) 0.022(2) 0.023(2) 0.0008(17) -0.0048(16) -0.0009(17) C35 0.049(3) 0.023(2) 0.020(2) 0.0010(18) 0.005(2) 0.009(2) C36 0.070(4) 0.028(3) 0.029(3) 0.008(2) 0.023(2) 0.023(3) C37 0.060(3) 0.048(3) 0.048(3) 0.025(3) 0.031(3) 0.042(3) C38 0.036(3) 0.034(3) 0.044(3) 0.013(2) 0.015(2) 0.014(2) C39 0.024(2) 0.022(2) 0.030(2) 0.0101(18) 0.0071(17) 0.0112(17) C40 0.023(2) 0.017(2) 0.025(2) 0.0074(16) 0.0015(17) 0.0024(17) C41 0.022(2) 0.029(2) 0.039(3) 0.011(2) -0.0055(19) 0.0046(19) C42 0.033(3) 0.031(3) 0.033(3) 0.007(2) -0.013(2) -0.003(2) C43 0.051(3) 0.026(2) 0.021(2) -0.0064(19) -0.005(2) 0.008(2) C44 0.031(2) 0.034(3) 0.025(2) 0.0022(19) 0.0048(18) 0.012(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O7 2.030(3) 2_666 ? Co1 N2 2.085(3) . ? Co1 O1W 2.103(3) . ? Co1 N1 2.117(3) . ? Co1 O1 2.124(3) . ? Co1 O2 2.200(3) . ? Co1 C7 2.485(4) . ? Co2 O3 2.025(3) . ? Co2 O5 2.042(3) . ? Co2 O2W 2.077(3) . ? Co2 N4 2.100(3) . ? Co2 N3 2.129(4) . ? Co2 O6 2.373(3) . ? O1 C7 1.269(5) . ? O1W H1WA 0.8200 . ? O1W H1WB 0.8500 . ? O2 C7 1.259(5) . ? O2W H2WB 0.8200 . ? O2W H2WA 0.8499 . ? O3 C8 1.263(5) . ? O4 C8 1.244(5) . ? O5 C19 1.252(5) . ? O6 C19 1.252(4) . ? O7 C20 1.265(5) . ? O7 Co1 2.030(3) 2_666 ? O8 C20 1.241(5) . ? N1 C29 1.336(5) . ? N1 C25 1.336(5) . ? N2 C30 1.343(5) . ? N2 C34 1.347(5) . ? N3 C35 1.344(5) . ? N3 C39 1.348(5) . ? N4 C44 1.328(5) . ? N4 C40 1.336(5) . ? C1 C6 1.376(6) . ? C1 C2 1.383(5) . ? C1 C7 1.498(6) . ? C2 C3 1.399(6) . ? C2 H2A 0.9300 . ? C3 C4 1.377(6) . ? C3 C8 1.500(5) . ? C4 C5 1.395(5) . ? C4 H4A 0.9300 . ? C5 C6 1.389(6) . ? C5 C9 1.509(6) . ? C6 H6A 0.9300 . ? C9 C10 1.519(6) . ? C9 C12 1.530(7) . ? C9 C11 1.536(6) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.384(5) . ? C13 C18 1.386(5) . ? C13 C19 1.494(5) . ? C14 C15 1.376(5) . ? C14 H14A 0.9300 . ? C15 C16 1.378(5) . ? C15 C20 1.514(5) . ? C16 C17 1.392(5) . ? C16 H16A 0.9300 . ? C17 C18 1.385(5) . ? C17 C21 1.522(6) . ? C18 H18A 0.9300 . ? C21 C23' 1.504(8) . ? C21 C23 1.505(7) . ? C21 C24 1.534(7) . ? C21 C22' 1.535(8) . ? C21 C24' 1.538(8) . ? C21 C22 1.542(7) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C22' H22D 0.9600 . ? C22' H22E 0.9600 . ? C22' H22F 0.9600 . ? C23' H23D 0.9600 . ? C23' H23E 0.9600 . ? C23' H23F 0.9600 . ? C24' H24D 0.9600 . ? C24' H24E 0.9600 . ? C24' H24F 0.9600 . ? C25 C26 1.386(6) . ? C25 H25A 0.9300 . ? C26 C27 1.369(7) . ? C26 H26A 0.9300 . ? C27 C28 1.381(6) . ? C27 H27A 0.9300 . ? C28 C29 1.385(5) . ? C28 H28A 0.9300 . ? C29 C30 1.483(5) . ? C30 C31 1.371(6) . ? C31 C32 1.382(6) . ? C31 H31A 0.9300 . ? C32 C33 1.389(6) . ? C32 H32A 0.9300 . ? C33 C34 1.363(6) . ? C33 H33A 0.9300 . ? C34 H34A 0.9300 . ? C35 C36 1.370(7) . ? C35 H35A 0.9300 . ? C36 C37 1.391(7) . ? C36 H36A 0.9300 . ? C37 C38 1.375(7) . ? C37 H37A 0.9300 . ? C38 C39 1.374(6) . ? C38 H38A 0.9300 . ? C39 C40 1.475(6) . ? C40 C41 1.392(5) . ? C41 C42 1.367(7) . ? C41 H41A 0.9300 . ? C42 C43 1.359(7) . ? C42 H42A 0.9300 . ? C43 C44 1.371(6) . ? C43 H43A 0.9300 . ? C44 H44B 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Co1 N2 100.35(12) 2_666 . ? O7 Co1 O1W 89.35(11) 2_666 . ? N2 Co1 O1W 98.63(12) . . ? O7 Co1 N1 85.51(11) 2_666 . ? N2 Co1 N1 76.64(13) . . ? O1W Co1 N1 172.25(12) . . ? O7 Co1 O1 102.38(11) 2_666 . ? N2 Co1 O1 155.06(12) . . ? O1W Co1 O1 91.78(11) . . ? N1 Co1 O1 94.99(12) . . ? O7 Co1 O2 163.34(11) 2_666 . ? N2 Co1 O2 96.24(11) . . ? O1W Co1 O2 89.77(11) . . ? N1 Co1 O2 96.81(11) . . ? O1 Co1 O2 61.02(10) . . ? O3 Co2 O5 98.48(11) . . ? O3 Co2 O2W 92.61(12) . . ? O5 Co2 O2W 93.83(13) . . ? O3 Co2 N4 98.40(12) . . ? O5 Co2 N4 158.97(13) . . ? O2W Co2 N4 97.83(13) . . ? O3 Co2 N3 88.35(12) . . ? O5 Co2 N3 91.56(13) . . ? O2W Co2 N3 174.32(12) . . ? N4 Co2 N3 76.49(13) . . ? O3 Co2 O6 156.69(11) . . ? O5 Co2 O6 58.54(10) . . ? O2W Co2 O6 85.70(11) . . ? N4 Co2 O6 104.87(11) . . ? N3 Co2 O6 95.63(12) . . ? C7 O1 Co1 90.5(2) . . ? Co1 O1W H1WA 109.5 . . ? Co1 O1W H1WB 108.4 . . ? H1WA O1W H1WB 98.1 . . ? C7 O2 Co1 87.4(2) . . ? Co2 O2W H2WB 109.5 . . ? Co2 O2W H2WA 119.3 . . ? H2WB O2W H2WA 115.9 . . ? C8 O3 Co2 126.4(3) . . ? C19 O5 Co2 97.9(2) . . ? C19 O6 Co2 82.7(2) . . ? C20 O7 Co1 125.3(2) . 2_666 ? C29 N1 C25 118.9(4) . . ? C29 N1 Co1 116.6(2) . . ? C25 N1 Co1 124.3(3) . . ? C30 N2 C34 118.4(4) . . ? C30 N2 Co1 117.2(2) . . ? C34 N2 Co1 124.5(3) . . ? C35 N3 C39 118.4(4) . . ? C35 N3 Co2 125.5(3) . . ? C39 N3 Co2 115.9(3) . . ? C44 N4 C40 118.4(4) . . ? C44 N4 Co2 124.7(3) . . ? C40 N4 Co2 116.6(3) . . ? C6 C1 C2 120.7(4) . . ? C6 C1 C7 118.4(3) . . ? C2 C1 C7 120.8(4) . . ? C1 C2 C3 118.9(4) . . ? C1 C2 H2A 120.6 . . ? C3 C2 H2A 120.6 . . ? C4 C3 C2 119.5(4) . . ? C4 C3 C8 119.1(4) . . ? C2 C3 C8 121.4(4) . . ? C3 C4 C5 122.2(4) . . ? C3 C4 H4A 118.9 . . ? C5 C4 H4A 118.9 . . ? C6 C5 C4 117.1(4) . . ? C6 C5 C9 123.1(4) . . ? C4 C5 C9 119.8(4) . . ? C1 C6 C5 121.6(4) . . ? C1 C6 H6A 119.2 . . ? C5 C6 H6A 119.2 . . ? O2 C7 O1 120.7(4) . . ? O2 C7 C1 121.4(3) . . ? O1 C7 C1 117.9(4) . . ? O2 C7 Co1 62.2(2) . . ? O1 C7 Co1 58.7(2) . . ? C1 C7 Co1 173.0(3) . . ? O4 C8 O3 125.7(4) . . ? O4 C8 C3 117.6(4) . . ? O3 C8 C3 116.7(4) . . ? C5 C9 C10 112.9(4) . . ? C5 C9 C12 108.7(4) . . ? C10 C9 C12 108.0(4) . . ? C5 C9 C11 109.5(4) . . ? C10 C9 C11 107.9(4) . . ? C12 C9 C11 109.9(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 119.2(3) . . ? C14 C13 C19 118.0(3) . . ? C18 C13 C19 122.8(3) . . ? C15 C14 C13 120.3(4) . . ? C15 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? C14 C15 C16 119.9(3) . . ? C14 C15 C20 117.3(3) . . ? C16 C15 C20 122.7(3) . . ? C15 C16 C17 121.3(4) . . ? C15 C16 H16A 119.3 . . ? C17 C16 H16A 119.3 . . ? C18 C17 C16 117.7(4) . . ? C18 C17 C21 121.3(4) . . ? C16 C17 C21 120.9(4) . . ? C17 C18 C13 121.6(4) . . ? C17 C18 H18A 119.2 . . ? C13 C18 H18A 119.2 . . ? O5 C19 O6 120.8(4) . . ? O5 C19 C13 117.3(3) . . ? O6 C19 C13 121.9(3) . . ? O8 C20 O7 126.6(3) . . ? O8 C20 C15 119.0(4) . . ? O7 C20 C15 114.4(3) . . ? C23' C21 C23 119.3(9) . . ? C23' C21 C17 119.4(8) . . ? C23 C21 C17 115.2(5) . . ? C23' C21 C24 70.9(10) . . ? C23 C21 C24 113.0(6) . . ? C17 C21 C24 109.7(4) . . ? C23' C21 C22' 115.6(11) . . ? C23 C21 C22' 66.9(8) . . ? C17 C21 C22' 108.2(7) . . ? C24 C21 C22' 53.1(8) . . ? C23' C21 C24' 106.0(11) . . ? C17 C21 C24' 108.6(7) . . ? C24 C21 C24' 136.8(9) . . ? C22' C21 C24' 96.2(11) . . ? C23 C21 C22 108.9(6) . . ? C17 C21 C22 106.2(5) . . ? C24 C21 C22 102.8(6) . . ? C22' C21 C22 143.3(8) . . ? C24' C21 C22 84.7(9) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? C21 C22' H22D 109.5 . . ? C21 C22' H22E 109.5 . . ? H22D C22' H22E 109.5 . . ? C21 C22' H22F 109.5 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? C21 C23' H23D 109.5 . . ? C21 C23' H23E 109.5 . . ? H23D C23' H23E 109.5 . . ? C21 C23' H23F 109.5 . . ? H23D C23' H23F 109.5 . . ? H23E C23' H23F 109.5 . . ? C21 C24' H24D 109.5 . . ? C21 C24' H24E 109.5 . . ? H24D C24' H24E 109.5 . . ? C21 C24' H24F 109.5 . . ? H24D C24' H24F 109.5 . . ? H24E C24' H24F 109.5 . . ? N1 C25 C26 122.3(4) . . ? N1 C25 H25A 118.9 . . ? C26 C25 H25A 118.9 . . ? C27 C26 C25 118.3(4) . . ? C27 C26 H26A 120.9 . . ? C25 C26 H26A 120.9 . . ? C26 C27 C28 120.1(4) . . ? C26 C27 H27A 120.0 . . ? C28 C27 H27A 120.0 . . ? C27 C28 C29 118.2(4) . . ? C27 C28 H28A 120.9 . . ? C29 C28 H28A 120.9 . . ? N1 C29 C28 122.1(4) . . ? N1 C29 C30 114.6(3) . . ? C28 C29 C30 123.3(4) . . ? N2 C30 C31 121.8(4) . . ? N2 C30 C29 115.0(3) . . ? C31 C30 C29 123.2(4) . . ? C30 C31 C32 119.5(4) . . ? C30 C31 H31A 120.2 . . ? C32 C31 H31A 120.2 . . ? C31 C32 C33 118.7(4) . . ? C31 C32 H32A 120.6 . . ? C33 C32 H32A 120.6 . . ? C34 C33 C32 118.6(4) . . ? C34 C33 H33A 120.7 . . ? C32 C33 H33A 120.7 . . ? N2 C34 C33 122.9(4) . . ? N2 C34 H34A 118.6 . . ? C33 C34 H34A 118.6 . . ? N3 C35 C36 123.3(4) . . ? N3 C35 H35A 118.3 . . ? C36 C35 H35A 118.3 . . ? C35 C36 C37 117.6(5) . . ? C35 C36 H36A 121.2 . . ? C37 C36 H36A 121.2 . . ? C38 C37 C36 119.7(5) . . ? C38 C37 H37A 120.2 . . ? C36 C37 H37A 120.2 . . ? C39 C38 C37 119.3(5) . . ? C39 C38 H38A 120.3 . . ? C37 C38 H38A 120.3 . . ? N3 C39 C38 121.6(4) . . ? N3 C39 C40 114.5(4) . . ? C38 C39 C40 123.9(4) . . ? N4 C40 C41 121.3(4) . . ? N4 C40 C39 115.9(3) . . ? C41 C40 C39 122.7(4) . . ? C42 C41 C40 118.7(5) . . ? C42 C41 H41A 120.6 . . ? C40 C41 H41A 120.6 . . ? C43 C42 C41 119.9(4) . . ? C43 C42 H42A 120.0 . . ? C41 C42 H42A 120.0 . . ? C42 C43 C44 118.4(4) . . ? C42 C43 H43A 120.8 . . ? C44 C43 H43A 120.8 . . ? N4 C44 C43 123.2(4) . . ? N4 C44 H44B 118.4 . . ? C43 C44 H44B 118.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O7 Co1 O1 C7 174.9(2) 2_666 . . . ? N2 Co1 O1 C7 -29.9(4) . . . . ? O1W Co1 O1 C7 85.2(2) . . . . ? N1 Co1 O1 C7 -98.6(2) . . . . ? O2 Co1 O1 C7 -3.6(2) . . . . ? O7 Co1 O2 C7 -1.6(5) 2_666 . . . ? N2 Co1 O2 C7 172.8(2) . . . . ? O1W Co1 O2 C7 -88.6(2) . . . . ? N1 Co1 O2 C7 95.6(2) . . . . ? O1 Co1 O2 C7 3.6(2) . . . . ? O5 Co2 O3 C8 -105.5(3) . . . . ? O2W Co2 O3 C8 -11.2(3) . . . . ? N4 Co2 O3 C8 87.1(3) . . . . ? N3 Co2 O3 C8 163.2(3) . . . . ? O6 Co2 O3 C8 -96.4(4) . . . . ? O3 Co2 O5 C19 174.8(3) . . . . ? O2W Co2 O5 C19 81.6(3) . . . . ? N4 Co2 O5 C19 -42.1(5) . . . . ? N3 Co2 O5 C19 -96.6(3) . . . . ? O6 Co2 O5 C19 -1.0(2) . . . . ? O3 Co2 O6 C19 -9.6(4) . . . . ? O5 Co2 O6 C19 1.0(2) . . . . ? O2W Co2 O6 C19 -96.2(2) . . . . ? N4 Co2 O6 C19 166.8(2) . . . . ? N3 Co2 O6 C19 89.4(2) . . . . ? O7 Co1 N1 C29 -104.2(3) 2_666 . . . ? N2 Co1 N1 C29 -2.4(3) . . . . ? O7 Co1 N2 C30 85.4(3) 2_666 . . . ? O1W Co1 N2 C30 176.3(3) . . . . ? N1 Co1 N2 C30 2.5(3) . . . . ? O1 Co1 N2 C30 -70.1(4) . . . . ? O2 Co1 N2 C30 -93.0(3) . . . . ? C7 Co1 N2 C30 -88.5(3) . . . . ? O7 Co1 N2 C34 -94.0(3) 2_666 . . . ? O1W Co1 N2 C34 -3.0(3) . . . . ? N1 Co1 N2 C34 -176.8(3) . . . . ? O1 Co1 N2 C34 110.6(4) . . . . ? O2 Co1 N2 C34 87.7(3) . . . . ? C7 Co1 N2 C34 92.2(3) . . . . ? O3 Co2 N3 C35 82.7(3) . . . . ? O5 Co2 N3 C35 -15.8(3) . . . . ? N4 Co2 N3 C39 6.8(3) . . . . ? O6 Co2 N3 C39 110.7(3) . . . . ? O3 Co2 N4 C44 -94.4(3) . . . . ? O5 Co2 N4 C44 122.6(4) . . . . ? O2W Co2 N4 C44 -0.5(4) . . . . ? N3 Co2 N4 C44 179.4(4) . . . . ? O6 Co2 N4 C44 87.1(3) . . . . ? O3 Co2 N4 C40 79.8(3) . . . . ? O5 Co2 N4 C40 -63.3(5) . . . . ? O2W Co2 N4 C40 173.6(3) . . . . ? N3 Co2 N4 C40 -6.5(3) . . . . ? O6 Co2 N4 C40 -98.8(3) . . . . ? C6 C1 C2 C3 -0.7(6) . . . . ? C7 C1 C2 C3 -178.4(3) . . . . ? C1 C2 C3 C4 3.2(6) . . . . ? C1 C2 C3 C8 -174.7(3) . . . . ? C2 C3 C4 C5 -3.0(6) . . . . ? C8 C3 C4 C5 175.1(3) . . . . ? C3 C4 C5 C6 0.1(6) . . . . ? C3 C4 C5 C9 -179.4(4) . . . . ? C2 C1 C6 C5 -2.2(6) . . . . ? C7 C1 C6 C5 175.5(3) . . . . ? C4 C5 C6 C1 2.5(6) . . . . ? C9 C5 C6 C1 -178.0(4) . . . . ? Co1 O2 C7 O1 -6.2(4) . . . . ? Co1 O2 C7 C1 173.2(3) . . . . ? Co1 O1 C7 O2 6.4(4) . . . . ? Co1 O1 C7 C1 -173.0(3) . . . . ? C6 C1 C7 O2 -153.9(4) . . . . ? C2 C1 C7 O2 23.8(5) . . . . ? C6 C1 C7 O1 25.4(5) . . . . ? C2 C1 C7 O1 -156.8(4) . . . . ? O7 Co1 C7 O2 179.39(19) 2_666 . . . ? N2 Co1 C7 O2 -8.9(3) . . . . ? O1W Co1 C7 O2 91.1(2) . . . . ? N1 Co1 C7 O2 -88.7(2) . . . . ? O1 Co1 C7 O2 -173.8(4) . . . . ? O7 Co1 C7 O1 -6.8(3) 2_666 . . . ? N2 Co1 C7 O1 164.9(2) . . . . ? O1W Co1 C7 O1 -95.1(2) . . . . ? N1 Co1 C7 O1 85.1(2) . . . . ? O2 Co1 C7 O1 173.8(4) . . . . ? Co2 O3 C8 O4 -6.3(6) . . . . ? Co2 O3 C8 C3 171.9(2) . . . . ? C4 C3 C8 O4 5.5(6) . . . . ? C2 C3 C8 O4 -176.5(4) . . . . ? C4 C3 C8 O3 -172.8(3) . . . . ? C2 C3 C8 O3 5.2(5) . . . . ? C6 C5 C9 C10 6.3(6) . . . . ? C4 C5 C9 C10 -174.2(4) . . . . ? C6 C5 C9 C12 -113.5(5) . . . . ? C4 C5 C9 C12 66.0(5) . . . . ? C6 C5 C9 C11 126.5(4) . . . . ? C4 C5 C9 C11 -54.1(5) . . . . ? C18 C13 C14 C15 0.3(6) . . . . ? C19 C13 C14 C15 -178.9(4) . . . . ? C13 C14 C15 C16 0.5(6) . . . . ? C13 C14 C15 C20 176.7(4) . . . . ? C14 C15 C16 C17 -1.5(6) . . . . ? C20 C15 C16 C17 -177.6(4) . . . . ? C15 C16 C17 C18 1.7(6) . . . . ? C15 C16 C17 C21 -178.9(4) . . . . ? C16 C17 C18 C13 -0.8(6) . . . . ? C21 C17 C18 C13 179.7(4) . . . . ? C14 C13 C18 C17 -0.1(6) . . . . ? C19 C13 C18 C17 179.1(4) . . . . ? Co2 O5 C19 O6 1.9(5) . . . . ? Co2 O5 C19 C13 -178.2(3) . . . . ? Co2 O6 C19 O5 -1.6(4) . . . . ? Co2 O6 C19 C13 178.4(4) . . . . ? C14 C13 C19 O5 9.9(6) . . . . ? C18 C13 C19 O5 -169.2(4) . . . . ? C14 C13 C19 O6 -170.1(4) . . . . ? C18 C13 C19 O6 10.7(6) . . . . ? Co1 O7 C20 O8 29.6(6) 2_666 . . . ? Co1 O7 C20 C15 -148.6(3) 2_666 . . . ? C14 C15 C20 O8 -144.9(4) . . . . ? C16 C15 C20 O8 31.3(6) . . . . ? C14 C15 C20 O7 33.5(5) . . . . ? C16 C15 C20 O7 -150.4(4) . . . . ? C18 C17 C21 C23' -156.2(11) . . . . ? C16 C17 C21 C23' 24.4(12) . . . . ? C18 C17 C21 C23 -3.7(8) . . . . ? C16 C17 C21 C23 176.9(6) . . . . ? C18 C17 C21 C24 125.2(5) . . . . ? C16 C17 C21 C24 -54.3(6) . . . . ? C18 C17 C21 C22' 68.7(9) . . . . ? C16 C17 C21 C22' -110.7(9) . . . . ? C18 C17 C21 C24' -34.5(10) . . . . ? C16 C17 C21 C24' 146.0(9) . . . . ? C18 C17 C21 C22 -124.3(6) . . . . ? C16 C17 C21 C22 56.2(7) . . . . ? C29 N1 C25 C26 -0.7(6) . . . . ? Co1 N1 C25 C26 -175.7(3) . . . . ? N1 C25 C26 C27 -2.4(7) . . . . ? C25 C26 C27 C28 2.9(7) . . . . ? C26 C27 C28 C29 -0.3(7) . . . . ? C25 N1 C29 C28 3.5(6) . . . . ? Co1 N1 C29 C28 178.8(3) . . . . ? C25 N1 C29 C30 -173.4(3) . . . . ? Co1 N1 C29 C30 2.0(4) . . . . ? C27 C28 C29 N1 -3.0(6) . . . . ? C27 C28 C29 C30 173.6(4) . . . . ? C34 N2 C30 C31 -1.2(6) . . . . ? Co1 N2 C30 C31 179.5(3) . . . . ? C34 N2 C30 C29 177.0(3) . . . . ? Co1 N2 C30 C29 -2.3(4) . . . . ? N1 C29 C30 N2 0.2(5) . . . . ? C28 C29 C30 N2 -176.6(4) . . . . ? N1 C29 C30 C31 178.4(4) . . . . ? C28 C29 C30 C31 1.6(6) . . . . ? N2 C30 C31 C32 2.1(6) . . . . ? C29 C30 C31 C32 -175.9(4) . . . . ? C30 C31 C32 C33 -1.4(6) . . . . ? C31 C32 C33 C34 -0.1(7) . . . . ? C30 N2 C34 C33 -0.4(6) . . . . ? Co1 N2 C34 C33 178.9(3) . . . . ? C32 C33 C34 N2 1.1(7) . . . . ? C39 N3 C35 C36 0.2(6) . . . . ? Co2 N3 C35 C36 -174.7(3) . . . . ? N3 C35 C36 C37 1.8(7) . . . . ? C35 C36 C37 C38 -1.9(7) . . . . ? C36 C37 C38 C39 0.1(7) . . . . ? C35 N3 C39 C38 -2.1(6) . . . . ? Co2 N3 C39 C38 173.2(3) . . . . ? C35 N3 C39 C40 178.5(4) . . . . ? Co2 N3 C39 C40 -6.1(4) . . . . ? C37 C38 C39 N3 2.0(7) . . . . ? C37 C38 C39 C40 -178.8(4) . . . . ? C44 N4 C40 C41 -2.1(6) . . . . ? Co2 N4 C40 C41 -176.7(3) . . . . ? C44 N4 C40 C39 179.9(4) . . . . ? Co2 N4 C40 C39 5.3(5) . . . . ? N3 C39 C40 N4 0.6(5) . . . . ? C38 C39 C40 N4 -178.7(4) . . . . ? N3 C39 C40 C41 -177.4(4) . . . . ? C38 C39 C40 C41 3.3(7) . . . . ? N4 C40 C41 C42 2.4(6) . . . . ? C39 C40 C41 C42 -179.8(4) . . . . ? C40 C41 C42 C43 -1.5(7) . . . . ? C41 C42 C43 C44 0.5(7) . . . . ? C40 N4 C44 C43 1.1(7) . . . . ? Co2 N4 C44 C43 175.1(3) . . . . ? C42 C43 C44 N4 -0.3(7) . . . . ? 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 O2W H2WB O4 0.82 1.81 2.549(4) 150.0 . O1W H1WA O8 0.82 2.00 2.726(4) 146.5 2_666 O1W H1WB O8 0.85 1.96 2.793(4) 166.9 1_445 O2W H2WA O6 0.85 1.94 2.748(4) 158.0 2_665 _diffrn_measured_fraction_theta_max 0.859 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.907 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.111 #============================================================================== data_CoBpy2-{[Co3(bpy)2(tbip)3Co(bpy)(tbip)].5H2O}n _database_code_depnum_ccdc_archive 'CCDC 835410' #TrackingRef '- revised cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C39 H36 Co2 N3 O8), 5(H2 O)' _chemical_formula_sum 'C78 H82 Co4 N6 O21' _chemical_formula_weight 1675.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.7379(8) _cell_length_b 9.5391(2) _cell_length_c 28.4999(7) _cell_angle_alpha 90.00 _cell_angle_beta 116.1861(8) _cell_angle_gamma 90.00 _cell_volume 7742.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 297(2) _cell_measurement_reflns_used 26580 _cell_measurement_theta_min 6.05 _cell_measurement_theta_max 55.01 _exptl_crystal_description rod _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3472 _exptl_absorpt_coefficient_mu 0.919 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8520 _exptl_absorpt_correction_T_max 0.9219 _exptl_absorpt_process_details 'Tompa_analytical (Rigaku Corporation, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 297(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 'Rigaku R-AXIS RAPID imaging plate' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37164 _diffrn_reflns_av_R_equivalents 0.0386 _diffrn_reflns_av_sigmaI/netI 0.0309 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8865 _reflns_number_gt 7210 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'PROCESS-AUTO (Rigaku Corporation,1998)' _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan (Molecular Structure Corporation & Rigaku Corporation, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. DFIX 0.85 0.01 and DFIX 1.39 0.01 are applied to the three crystallographically independent lattice water molecules. DFIX 1.52 0.01 is applied to the C-C distances of the disordered tert-butyl. EADP is applied to three carbon atoms in the diordered tert-butyl. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+4.4860P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8865 _refine_ls_number_parameters 517 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0852 _refine_ls_wR_factor_gt 0.0789 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.046 _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 Co1 Co 0.164198(8) 0.21792(2) 0.045495(9) 0.02230(7) Uani 1 1 d . . . Co2 Co 0.2500 0.2500 0.0000 0.01965(8) Uani 1 2 d S . . Co3 Co 0.5000 0.51939(4) 0.2500 0.03252(10) Uani 1 2 d S . . O1 O 0.22495(5) 0.23369(14) 0.11088(5) 0.0331(3) Uani 1 1 d . . . O2 O 0.27858(5) 0.25908(16) 0.08021(5) 0.0365(3) Uani 1 1 d . . . O3 O 0.43993(6) 0.4015(2) 0.20139(6) 0.0521(4) Uani 1 1 d . . . O4 O 0.45570(5) 0.43966(19) 0.28273(6) 0.0466(4) Uani 1 1 d . . . O5 O 0.15749(5) 0.45791(13) 0.04023(6) 0.0356(3) Uani 1 1 d . . . O6 O 0.18551(4) 0.33706(11) -0.00473(5) 0.0255(3) Uani 1 1 d . . . O7 O 0.16974(5) 1.01066(13) 0.02833(6) 0.0321(3) Uani 1 1 d . . . O8 O 0.22033(5) 1.05732(13) -0.00449(6) 0.0377(3) Uani 1 1 d . . . N1 N 0.09400(6) 0.20907(16) -0.01474(6) 0.0297(3) Uani 1 1 d . . . N2 N 0.12412(6) 0.18143(16) 0.08652(6) 0.0295(3) Uani 1 1 d . . . N3 N 0.52421(7) 0.6924(2) 0.30080(8) 0.0463(5) Uani 1 1 d . . . O1W O 0.08102(8) 0.8719(2) 0.00772(13) 0.0931(8) Uani 1 1 d D . . H1C H 0.0842(12) 0.7840(14) 0.0154(16) 0.112 Uiso 1 1 d D . . H1D H 0.1079(6) 0.904(3) 0.0135(15) 0.112 Uiso 1 1 d D . . O2W O 0.07020(10) 0.5790(3) 0.01480(15) 0.1052(9) Uani 1 1 d D . . H2C H 0.0463(7) 0.526(3) 0.0039(18) 0.126 Uiso 1 1 d D . . H2D H 0.0951(7) 0.532(3) 0.0221(17) 0.126 Uiso 1 1 d D . . O3W O 0.0162(2) 0.4838(6) 0.0635(3) 0.128(2) Uani 0.50 1 d PD . . H3C H 0.0386 0.4871 0.0926 0.153 Uiso 0.50 1 calc PRD . . H3D H -0.0072 0.4947 0.0701 0.153 Uiso 0.50 1 d PRD . . C1 C 0.30477(6) 0.26011(18) 0.17090(7) 0.0257(4) Uani 1 1 d . . . C2 C 0.34797(7) 0.31264(18) 0.17895(7) 0.0271(4) Uani 1 1 d . . . H2 H 0.3531 0.3410 0.1507 0.033 Uiso 1 1 calc R . . C3 C 0.38375(7) 0.3228(2) 0.22962(7) 0.0297(4) Uani 1 1 d . . . C4 C 0.37646(7) 0.2718(2) 0.27104(8) 0.0364(4) Uani 1 1 d . . . H4 H 0.4006 0.2783 0.3048 0.044 Uiso 1 1 calc R . . C5 C 0.33405(8) 0.2111(2) 0.26363(8) 0.0357(4) Uani 1 1 d . A . C6 C 0.29802(7) 0.2108(2) 0.21312(8) 0.0317(4) Uani 1 1 d . . . H6 H 0.2687 0.1767 0.2073 0.038 Uiso 1 1 calc R . . C7 C 0.26618(6) 0.25083(17) 0.11607(7) 0.0255(4) Uani 1 1 d . . . C8 C 0.42897(7) 0.3905(2) 0.23867(8) 0.0337(4) Uani 1 1 d . . . C9 C 0.32881(9) 0.1471(3) 0.31020(9) 0.0515(6) Uani 1 1 d D . . C13 C 0.17774(6) 0.58530(17) -0.01925(7) 0.0241(4) Uani 1 1 d . . . C14 C 0.18047(6) 0.71603(17) 0.00412(7) 0.0251(4) Uani 1 1 d . . . H14A H 0.1785 0.7232 0.0356 0.030 Uiso 1 1 calc R . . C15 C 0.18620(6) 0.83496(17) -0.02058(7) 0.0251(4) Uani 1 1 d . . . C16 C 0.18649(7) 0.82364(18) -0.06897(8) 0.0286(4) Uani 1 1 d . . . H16A H 0.1907 0.9041 -0.0849 0.034 Uiso 1 1 calc R . . C17 C 0.18072(7) 0.69569(19) -0.09446(8) 0.0299(4) Uani 1 1 d . . . C18 C 0.17801(7) 0.57607(18) -0.06765(7) 0.0280(4) Uani 1 1 d . . . H18A H 0.1764 0.4883 -0.0826 0.034 Uiso 1 1 calc R . . C19 C 0.17381(6) 0.45465(17) 0.00753(7) 0.0244(4) Uani 1 1 d . . . C20 C 0.19291(6) 0.97881(17) 0.00355(7) 0.0248(4) Uani 1 1 d . . . C21 C 0.17995(9) 0.6832(2) -0.14839(8) 0.0389(5) Uani 1 1 d . . . C22 C 0.22626(9) 0.6181(3) -0.14136(10) 0.0506(6) Uani 1 1 d . . . H22A H 0.2517 0.6793 -0.1206 0.076 Uiso 1 1 calc R . . H22B H 0.2258 0.6050 -0.1750 0.076 Uiso 1 1 calc R . . H22C H 0.2304 0.5292 -0.1241 0.076 Uiso 1 1 calc R . . C23 C 0.13904(10) 0.5895(3) -0.18411(10) 0.0571(7) Uani 1 1 d . . . H23A H 0.1099 0.6313 -0.1889 0.086 Uiso 1 1 calc R . . H23B H 0.1421 0.4988 -0.1684 0.086 Uiso 1 1 calc R . . H23C H 0.1395 0.5799 -0.2174 0.086 Uiso 1 1 calc R . . C24 C 0.17428(15) 0.8265(3) -0.17479(11) 0.0803(11) Uani 1 1 d . . . H24A H 0.2003 0.8854 -0.1537 0.121 Uiso 1 1 calc R . . H24B H 0.1456 0.8693 -0.1785 0.121 Uiso 1 1 calc R . . H24C H 0.1733 0.8146 -0.2087 0.121 Uiso 1 1 calc R . . C25 C 0.08191(8) 0.2120(2) -0.06611(8) 0.0406(5) Uani 1 1 d . . . H25A H 0.1054 0.2243 -0.0769 0.049 Uiso 1 1 calc R . . C26 C 0.03639(9) 0.1976(3) -0.10349(10) 0.0527(6) Uani 1 1 d . . . H26A H 0.0292 0.1990 -0.1389 0.063 Uiso 1 1 calc R . . C27 C 0.00185(10) 0.1813(3) -0.08749(11) 0.0636(7) Uani 1 1 d . . . H27A H -0.0293 0.1728 -0.1121 0.076 Uiso 1 1 calc R . . C28 C 0.01342(8) 0.1774(3) -0.03501(11) 0.0566(7) Uani 1 1 d . . . H28A H -0.0098 0.1661 -0.0237 0.068 Uiso 1 1 calc R . . C29 C 0.06018(7) 0.1905(2) 0.00093(9) 0.0355(4) Uani 1 1 d . . . C30 C 0.07725(7) 0.1772(2) 0.05823(9) 0.0349(4) Uani 1 1 d . . . C31 C 0.04768(9) 0.1548(3) 0.08181(11) 0.0576(7) Uani 1 1 d . . . H31A H 0.0153 0.1544 0.0619 0.069 Uiso 1 1 calc R . . C32 C 0.06692(11) 0.1334(3) 0.13457(12) 0.0662(8) Uani 1 1 d . . . H32A H 0.0476 0.1181 0.1509 0.079 Uiso 1 1 calc R . . C33 C 0.11454(11) 0.1346(3) 0.16321(10) 0.0597(7) Uani 1 1 d . . . H33A H 0.1281 0.1181 0.1990 0.072 Uiso 1 1 calc R . . C34 C 0.14221(9) 0.1607(2) 0.13808(9) 0.0446(5) Uani 1 1 d . . . H34A H 0.1746 0.1640 0.1577 0.054 Uiso 1 1 calc R . . C35 C 0.51146(9) 0.8192(3) 0.27894(11) 0.0549(6) Uani 1 1 d . . . C36 C 0.51992(13) 0.9379(4) 0.31000(17) 0.0882(11) Uani 1 1 d . . . H36A H 0.5102 1.0257 0.2948 0.106 Uiso 1 1 calc R . . C37 C 0.54270(15) 0.9243(4) 0.36328(18) 0.0996(13) Uani 1 1 d . . . H37A H 0.5487 1.0033 0.3844 0.120 Uiso 1 1 calc R . . C38 C 0.55663(12) 0.7963(4) 0.38555(14) 0.0801(10) Uani 1 1 d . . . H38A H 0.5723 0.7863 0.4217 0.096 Uiso 1 1 calc R . . C39 C 0.54683(10) 0.6815(3) 0.35309(11) 0.0593(7) Uani 1 1 d . . . H39A H 0.5562 0.5933 0.3679 0.071 Uiso 1 1 calc R . . C10 C 0.3379(3) 0.2477(7) 0.3537(2) 0.0682(8) Uani 0.635(10) 1 d PD A 1 H10A H 0.3705 0.2733 0.3699 0.102 Uiso 0.635(10) 1 calc PR A 1 H10B H 0.3300 0.2045 0.3792 0.102 Uiso 0.635(10) 1 calc PR A 1 H10C H 0.3190 0.3301 0.3401 0.102 Uiso 0.635(10) 1 calc PR A 1 C11 C 0.2774(2) 0.1036(9) 0.29481(19) 0.0682(8) Uani 0.635(10) 1 d PD A 1 H11A H 0.2682 0.0319 0.2685 0.102 Uiso 0.635(10) 1 calc PR A 1 H11B H 0.2573 0.1835 0.2814 0.102 Uiso 0.635(10) 1 calc PR A 1 H11C H 0.2749 0.0682 0.3250 0.102 Uiso 0.635(10) 1 calc PR A 1 C12 C 0.3619(2) 0.0220(6) 0.3307(2) 0.0682(8) Uani 0.635(10) 1 d PD A 1 H12A H 0.3532 -0.0482 0.3039 0.102 Uiso 0.635(10) 1 calc PR A 1 H12B H 0.3598 -0.0165 0.3607 0.102 Uiso 0.635(10) 1 calc PR A 1 H12C H 0.3935 0.0520 0.3403 0.102 Uiso 0.635(10) 1 calc PR A 1 C10' C 0.3351(6) 0.2789(10) 0.3464(4) 0.0682(8) Uani 0.365(10) 1 d PD A 2 H10D H 0.3649 0.3222 0.3548 0.102 Uiso 0.365(10) 1 calc PR A 2 H10E H 0.3339 0.2496 0.3780 0.102 Uiso 0.365(10) 1 calc PR A 2 H10F H 0.3104 0.3450 0.3283 0.102 Uiso 0.365(10) 1 calc PR A 2 C11' C 0.2886(4) 0.0418(13) 0.2943(3) 0.0682(8) Uani 0.365(10) 1 d PD A 2 H11D H 0.2935 -0.0330 0.2747 0.102 Uiso 0.365(10) 1 calc PR A 2 H11E H 0.2594 0.0879 0.2731 0.102 Uiso 0.365(10) 1 calc PR A 2 H11F H 0.2876 0.0044 0.3250 0.102 Uiso 0.365(10) 1 calc PR A 2 C12' C 0.3739(3) 0.0588(11) 0.3431(4) 0.0682(8) Uani 0.365(10) 1 d PD A 2 H12D H 0.3793 -0.0063 0.3206 0.102 Uiso 0.365(10) 1 calc PR A 2 H12E H 0.3697 0.0083 0.3698 0.102 Uiso 0.365(10) 1 calc PR A 2 H12F H 0.4004 0.1203 0.3589 0.102 Uiso 0.365(10) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.02114(13) 0.02204(12) 0.02410(13) -0.00068(9) 0.01033(10) -0.00272(8) Co2 0.02007(17) 0.01879(15) 0.02031(16) -0.00075(11) 0.00911(14) -0.00301(11) Co3 0.01981(19) 0.0440(2) 0.0304(2) 0.000 0.00807(16) 0.000 O1 0.0226(7) 0.0450(8) 0.0275(7) -0.0011(6) 0.0073(6) -0.0043(6) O2 0.0279(8) 0.0579(9) 0.0213(7) -0.0035(6) 0.0087(6) -0.0052(6) O3 0.0333(9) 0.0901(13) 0.0335(8) -0.0072(8) 0.0153(7) -0.0203(8) O4 0.0293(8) 0.0737(11) 0.0322(8) -0.0118(7) 0.0092(7) -0.0169(7) O5 0.0473(9) 0.0267(6) 0.0439(8) 0.0053(6) 0.0302(8) 0.0030(6) O6 0.0256(7) 0.0187(6) 0.0327(7) 0.0018(5) 0.0134(6) 0.0006(5) O7 0.0360(8) 0.0242(6) 0.0420(8) -0.0060(5) 0.0225(7) -0.0028(5) O8 0.0408(9) 0.0215(6) 0.0581(10) -0.0046(6) 0.0286(8) -0.0080(6) N1 0.0270(9) 0.0297(8) 0.0301(8) 0.0007(6) 0.0104(7) -0.0017(6) N2 0.0317(9) 0.0314(8) 0.0283(8) -0.0006(6) 0.0159(7) -0.0042(6) N3 0.0343(11) 0.0527(11) 0.0480(12) -0.0078(9) 0.0147(9) -0.0068(8) O1W 0.0638(15) 0.0574(12) 0.172(3) 0.0017(15) 0.0651(18) -0.0026(10) O2W 0.0711(17) 0.0771(16) 0.168(3) 0.0104(17) 0.053(2) 0.0167(13) O3W 0.100(5) 0.108(4) 0.192(7) 0.003(4) 0.079(5) -0.001(3) C1 0.0234(9) 0.0287(9) 0.0225(9) -0.0017(7) 0.0080(8) -0.0011(7) C2 0.0261(10) 0.0316(9) 0.0223(9) 0.0013(7) 0.0095(8) -0.0018(7) C3 0.0235(10) 0.0374(10) 0.0254(9) -0.0021(7) 0.0082(8) -0.0027(7) C4 0.0285(11) 0.0530(12) 0.0210(9) -0.0006(8) 0.0048(8) -0.0041(9) C5 0.0368(12) 0.0452(11) 0.0261(10) -0.0004(8) 0.0148(9) -0.0046(9) C6 0.0266(10) 0.0404(10) 0.0280(10) -0.0027(8) 0.0120(8) -0.0056(8) C7 0.0238(9) 0.0247(8) 0.0242(9) -0.0022(7) 0.0073(8) -0.0019(7) C8 0.0226(10) 0.0444(11) 0.0302(10) 0.0005(8) 0.0079(9) -0.0012(8) C9 0.0564(16) 0.0718(16) 0.0298(12) 0.0049(11) 0.0222(12) -0.0118(12) C13 0.0214(9) 0.0195(8) 0.0310(9) 0.0011(7) 0.0111(8) -0.0005(6) C14 0.0245(9) 0.0220(8) 0.0297(9) 0.0002(7) 0.0128(8) -0.0008(6) C15 0.0221(9) 0.0193(8) 0.0333(10) -0.0005(7) 0.0116(8) -0.0003(6) C16 0.0367(11) 0.0202(8) 0.0346(10) 0.0040(7) 0.0209(9) 0.0010(7) C17 0.0348(11) 0.0267(9) 0.0296(10) 0.0034(7) 0.0155(9) 0.0047(7) C18 0.0322(10) 0.0191(8) 0.0325(10) -0.0014(7) 0.0141(9) 0.0001(7) C19 0.0213(9) 0.0205(8) 0.0298(9) 0.0023(7) 0.0098(8) -0.0007(6) C20 0.0237(9) 0.0189(8) 0.0292(9) 0.0016(7) 0.0092(8) 0.0007(6) C21 0.0577(15) 0.0317(10) 0.0325(11) 0.0035(8) 0.0247(11) 0.0077(9) C22 0.0555(16) 0.0570(14) 0.0500(14) -0.0052(11) 0.0332(13) 0.0009(11) C23 0.0549(17) 0.0748(17) 0.0365(13) -0.0087(12) 0.0156(12) 0.0093(13) C24 0.160(4) 0.0475(15) 0.0546(17) 0.0197(12) 0.067(2) 0.0247(18) C25 0.0428(13) 0.0428(11) 0.0311(11) -0.0002(9) 0.0117(10) -0.0039(9) C26 0.0533(16) 0.0539(14) 0.0342(12) 0.0009(10) 0.0040(11) -0.0030(11) C27 0.0335(14) 0.0807(19) 0.0501(16) 0.0055(14) -0.0059(12) -0.0047(13) C28 0.0256(12) 0.0768(18) 0.0610(17) 0.0030(13) 0.0133(12) -0.0044(11) C29 0.0271(11) 0.0358(10) 0.0416(12) 0.0010(8) 0.0132(9) -0.0005(8) C30 0.0308(11) 0.0361(10) 0.0437(12) 0.0006(9) 0.0218(10) -0.0020(8) C31 0.0401(14) 0.0818(18) 0.0637(17) 0.0039(14) 0.0346(14) -0.0049(13) C32 0.068(2) 0.089(2) 0.0659(19) 0.0014(15) 0.0522(17) -0.0123(16) C33 0.077(2) 0.0748(18) 0.0395(14) -0.0006(12) 0.0369(15) -0.0131(15) C34 0.0452(14) 0.0568(13) 0.0325(11) 0.0006(10) 0.0178(11) -0.0079(10) C35 0.0390(14) 0.0488(13) 0.0742(18) -0.0071(12) 0.0225(14) -0.0037(10) C36 0.086(3) 0.0566(18) 0.109(3) -0.0223(19) 0.031(2) 0.0002(16) C37 0.099(3) 0.081(2) 0.106(3) -0.051(2) 0.033(3) -0.010(2) C38 0.070(2) 0.096(3) 0.068(2) -0.0374(19) 0.0249(18) -0.0189(18) C39 0.0516(16) 0.0714(17) 0.0491(15) -0.0136(13) 0.0168(13) -0.0146(13) C10 0.0945(19) 0.073(2) 0.0479(13) 0.0071(12) 0.0417(14) -0.0128(15) C11 0.0945(19) 0.073(2) 0.0479(13) 0.0071(12) 0.0417(14) -0.0128(15) C12 0.0945(19) 0.073(2) 0.0479(13) 0.0071(12) 0.0417(14) -0.0128(15) C10' 0.0945(19) 0.073(2) 0.0479(13) 0.0071(12) 0.0417(14) -0.0128(15) C11' 0.0945(19) 0.073(2) 0.0479(13) 0.0071(12) 0.0417(14) -0.0128(15) C12' 0.0945(19) 0.073(2) 0.0479(13) 0.0071(12) 0.0417(14) -0.0128(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.0105(14) . ? Co1 O7 2.0628(12) 1_545 ? Co1 N2 2.1022(15) . ? Co1 N1 2.1312(17) . ? Co1 O6 2.1570(12) . ? Co1 O5 2.2980(13) . ? Co2 O8 2.0432(12) 1_545 ? Co2 O8 2.0432(12) 7_565 ? Co2 O2 2.0556(13) . ? Co2 O2 2.0556(13) 7 ? Co2 O6 2.1572(12) 7 ? Co2 O6 2.1572(12) . ? Co3 N3 2.104(2) . ? Co3 N3 2.104(2) 2_655 ? Co3 O3 2.1184(16) 2_655 ? Co3 O3 2.1185(16) . ? Co3 O4 2.1408(15) . ? Co3 O4 2.1408(15) 2_655 ? Co3 C8 2.461(2) . ? Co3 C8 2.461(2) 2_655 ? O1 C7 1.261(2) . ? O2 C7 1.249(2) . ? O3 C8 1.260(2) . ? O4 C8 1.256(2) . ? O5 C19 1.251(2) . ? O6 C19 1.278(2) . ? O7 C20 1.261(2) . ? O7 Co1 2.0628(12) 1_565 ? O8 C20 1.244(2) . ? O8 Co2 2.0432(12) 1_565 ? N1 C25 1.340(3) . ? N1 C29 1.344(3) . ? N2 C34 1.335(3) . ? N2 C30 1.344(3) . ? N3 C35 1.339(3) . ? N3 C39 1.343(3) . ? O1W H1C 0.86(3) . ? O1W H1D 0.85(3) . ? O2W H2C 0.85(3) . ? O2W H2D 0.85(3) . ? O3W H3C 0.820 . ? O3W H3D 0.850 . ? C1 C2 1.381(3) . ? C1 C6 1.394(3) . ? C1 C7 1.503(2) . ? C2 C3 1.392(3) . ? C2 H2 0.9300 . ? C3 C4 1.387(3) . ? C3 C8 1.489(3) . ? C4 C5 1.393(3) . ? C4 H4 0.9300 . ? C5 C6 1.388(3) . ? C5 C9 1.535(3) . ? C6 H6 0.9300 . ? C9 C10 1.493(6) . ? C9 C12 1.525(6) . ? C9 C11' 1.527(7) . ? C9 C11 1.547(5) . ? C9 C12' 1.566(8) . ? C9 C10' 1.582(8) . ? C13 C18 1.386(3) . ? C13 C14 1.398(2) . ? C13 C19 1.495(2) . ? C14 C15 1.389(2) . ? C14 H14A 0.9300 . ? C15 C16 1.387(3) . ? C15 C20 1.507(2) . ? C16 C17 1.391(3) . ? C16 H16A 0.9300 . ? C17 C18 1.397(2) . ? C17 C21 1.531(3) . ? C18 H18A 0.9300 . ? C21 C22 1.525(3) . ? C21 C24 1.532(3) . ? C21 C23 1.534(3) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.372(3) . ? C25 H25A 0.9300 . ? C26 C27 1.369(4) . ? C26 H26A 0.9300 . ? C27 C28 1.374(4) . ? C27 H27A 0.9300 . ? C28 C29 1.388(3) . ? C28 H28A 0.9300 . ? C29 C30 1.482(3) . ? C30 C31 1.391(3) . ? C31 C32 1.366(4) . ? C31 H31A 0.9300 . ? C32 C33 1.364(4) . ? C32 H32A 0.9300 . ? C33 C34 1.379(3) . ? C33 H33A 0.9300 . ? C34 H34A 0.9300 . ? C35 C36 1.389(4) . ? C35 C35 1.480(6) 2_655 ? C36 C37 1.370(5) . ? C36 H36A 0.9300 . ? C37 C38 1.357(5) . ? C37 H37A 0.9300 . ? C38 C39 1.377(4) . ? C38 H38A 0.9300 . ? C39 H39A 0.9300 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C10' H10D 0.9600 . ? C10' H10E 0.9600 . ? C10' H10F 0.9600 . ? C11' H11D 0.9600 . ? C11' H11E 0.9600 . ? C11' H11F 0.9600 . ? C12' H12D 0.9600 . ? C12' H12E 0.9600 . ? C12' H12F 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O7 98.29(6) . 1_545 ? O1 Co1 N2 93.73(6) . . ? O7 Co1 N2 96.27(6) 1_545 . ? O1 Co1 N1 169.63(6) . . ? O7 Co1 N1 86.52(6) 1_545 . ? N2 Co1 N1 76.55(6) . . ? O1 Co1 O6 97.02(5) . . ? O7 Co1 O6 105.25(5) 1_545 . ? N2 Co1 O6 154.20(6) . . ? N1 Co1 O6 90.51(5) . . ? O1 Co1 O5 90.53(6) . . ? O7 Co1 O5 162.65(5) 1_545 . ? N2 Co1 O5 98.05(5) . . ? N1 Co1 O5 87.31(6) . . ? O6 Co1 O5 58.59(4) . . ? O8 Co2 O8 180.00(9) 1_545 7_565 ? O8 Co2 O2 94.16(6) 1_545 . ? O8 Co2 O2 85.84(6) 7_565 . ? O8 Co2 O2 85.84(6) 1_545 7 ? O8 Co2 O2 94.16(6) 7_565 7 ? O2 Co2 O2 180.00(3) . 7 ? O8 Co2 O6 93.20(5) 1_545 7 ? O8 Co2 O6 86.80(5) 7_565 7 ? O2 Co2 O6 90.34(5) . 7 ? O2 Co2 O6 89.66(5) 7 7 ? O8 Co2 O6 86.80(5) 1_545 . ? O8 Co2 O6 93.20(5) 7_565 . ? O2 Co2 O6 89.66(5) . . ? O2 Co2 O6 90.34(5) 7 . ? O6 Co2 O6 180.00(6) 7 . ? N3 Co3 N3 76.70(12) . 2_655 ? N3 Co3 O3 90.94(8) . 2_655 ? N3 Co3 O3 144.72(7) 2_655 2_655 ? N3 Co3 O3 144.72(7) . . ? N3 Co3 O3 90.94(8) 2_655 . ? O3 Co3 O3 115.87(11) 2_655 . ? N3 Co3 O4 95.13(7) . . ? N3 Co3 O4 117.89(7) 2_655 . ? O3 Co3 O4 95.80(7) 2_655 . ? O3 Co3 O4 61.43(6) . . ? N3 Co3 O4 117.89(7) . 2_655 ? N3 Co3 O4 95.13(7) 2_655 2_655 ? O3 Co3 O4 61.43(6) 2_655 2_655 ? O3 Co3 O4 95.80(7) . 2_655 ? O4 Co3 O4 138.38(10) . 2_655 ? N3 Co3 C8 121.16(7) . . ? N3 Co3 C8 105.45(7) 2_655 . ? O3 Co3 C8 109.17(7) 2_655 . ? O3 Co3 C8 30.79(6) . . ? O4 Co3 C8 30.67(6) . . ? O4 Co3 C8 120.34(7) 2_655 . ? N3 Co3 C8 105.45(7) . 2_655 ? N3 Co3 C8 121.16(7) 2_655 2_655 ? O3 Co3 C8 30.79(6) 2_655 2_655 ? O3 Co3 C8 109.17(7) . 2_655 ? O4 Co3 C8 120.34(7) . 2_655 ? O4 Co3 C8 30.67(6) 2_655 2_655 ? C8 Co3 C8 120.04(10) . 2_655 ? C7 O1 Co1 129.77(12) . . ? C7 O2 Co2 139.77(13) . . ? C8 O3 Co3 89.79(12) . . ? C8 O4 Co3 88.89(12) . . ? C19 O5 Co1 88.11(10) . . ? C19 O6 Co1 93.84(10) . . ? C19 O6 Co2 134.67(11) . . ? Co1 O6 Co2 108.81(5) . . ? C20 O7 Co1 119.71(11) . 1_565 ? C20 O8 Co2 150.54(12) . 1_565 ? C25 N1 C29 118.68(19) . . ? C25 N1 Co1 124.95(14) . . ? C29 N1 Co1 116.23(14) . . ? C34 N2 C30 118.70(18) . . ? C34 N2 Co1 124.39(15) . . ? C30 N2 Co1 116.91(13) . . ? C35 N3 C39 119.3(2) . . ? C35 N3 Co3 116.41(17) . . ? C39 N3 Co3 123.86(18) . . ? H1C O1W H1D 107.8(16) . . ? H2C O2W H2D 111.0(17) . . ? H3C O3W H3D 102.9 . . ? C2 C1 C6 119.92(17) . . ? C2 C1 C7 119.20(16) . . ? C6 C1 C7 120.82(17) . . ? C1 C2 C3 119.56(17) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C4 C3 C2 119.49(18) . . ? C4 C3 C8 120.99(17) . . ? C2 C3 C8 119.51(17) . . ? C3 C4 C5 121.98(18) . . ? C3 C4 H4 119.0 . . ? C5 C4 H4 119.0 . . ? C6 C5 C4 117.20(18) . . ? C6 C5 C9 122.78(19) . . ? C4 C5 C9 120.02(19) . . ? C5 C6 C1 121.61(18) . . ? C5 C6 H6 119.2 . . ? C1 C6 H6 119.2 . . ? O2 C7 O1 126.68(17) . . ? O2 C7 C1 116.13(16) . . ? O1 C7 C1 117.18(16) . . ? O4 C8 O3 119.76(18) . . ? O4 C8 C3 120.62(18) . . ? O3 C8 C3 119.60(18) . . ? O4 C8 Co3 60.44(10) . . ? O3 C8 Co3 59.42(11) . . ? C3 C8 Co3 175.33(15) . . ? C10 C9 C12 109.7(4) . . ? C10 C9 C11' 120.0(6) . . ? C12 C9 C11' 86.8(5) . . ? C10 C9 C5 114.1(3) . . ? C12 C9 C5 108.8(3) . . ? C11' C9 C5 113.6(4) . . ? C10 C9 C11 101.6(5) . . ? C12 C9 C11 111.2(3) . . ? C5 C9 C11 111.4(2) . . ? C10 C9 C12' 93.4(5) . . ? C5 C9 C12' 108.2(4) . . ? C11 C9 C12' 126.6(4) . . ? C12 C9 C10' 120.3(6) . . ? C11' C9 C10' 124.4(8) . . ? C5 C9 C10' 102.5(4) . . ? C11 C9 C10' 102.3(7) . . ? C12' C9 C10' 102.6(7) . . ? C18 C13 C14 120.30(16) . . ? C18 C13 C19 119.58(15) . . ? C14 C13 C19 120.11(16) . . ? C15 C14 C13 118.78(17) . . ? C15 C14 H14A 120.6 . . ? C13 C14 H14A 120.6 . . ? C16 C15 C14 120.01(16) . . ? C16 C15 C20 117.58(15) . . ? C14 C15 C20 122.41(16) . . ? C15 C16 C17 122.05(16) . . ? C15 C16 H16A 119.0 . . ? C17 C16 H16A 119.0 . . ? C16 C17 C18 117.19(17) . . ? C16 C17 C21 122.20(17) . . ? C18 C17 C21 120.53(17) . . ? C13 C18 C17 121.43(16) . . ? C13 C18 H18A 119.3 . . ? C17 C18 H18A 119.3 . . ? O5 C19 O6 119.44(15) . . ? O5 C19 C13 121.00(15) . . ? O6 C19 C13 119.50(15) . . ? O8 C20 O7 125.91(16) . . ? O8 C20 C15 115.69(16) . . ? O7 C20 C15 118.36(15) . . ? C22 C21 C17 108.19(18) . . ? C22 C21 C24 109.0(2) . . ? C17 C21 C24 111.71(17) . . ? C22 C21 C23 109.55(19) . . ? C17 C21 C23 110.21(19) . . ? C24 C21 C23 108.2(2) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N1 C25 C26 122.8(2) . . ? N1 C25 H25A 118.6 . . ? C26 C25 H25A 118.6 . . ? C27 C26 C25 118.4(2) . . ? C27 C26 H26A 120.8 . . ? C25 C26 H26A 120.8 . . ? C26 C27 C28 119.8(2) . . ? C26 C27 H27A 120.1 . . ? C28 C27 H27A 120.1 . . ? C27 C28 C29 119.1(2) . . ? C27 C28 H28A 120.5 . . ? C29 C28 H28A 120.5 . . ? N1 C29 C28 121.2(2) . . ? N1 C29 C30 114.85(18) . . ? C28 C29 C30 123.9(2) . . ? N2 C30 C31 121.3(2) . . ? N2 C30 C29 115.35(17) . . ? C31 C30 C29 123.3(2) . . ? C32 C31 C30 119.1(2) . . ? C32 C31 H31A 120.5 . . ? C30 C31 H31A 120.5 . . ? C33 C32 C31 119.8(2) . . ? C33 C32 H32A 120.1 . . ? C31 C32 H32A 120.1 . . ? C32 C33 C34 118.8(2) . . ? C32 C33 H33A 120.6 . . ? C34 C33 H33A 120.6 . . ? N2 C34 C33 122.4(2) . . ? N2 C34 H34A 118.8 . . ? C33 C34 H34A 118.8 . . ? N3 C35 C36 120.4(3) . . ? N3 C35 C35 114.68(15) . 2_655 ? C36 C35 C35 124.9(2) . 2_655 ? C37 C36 C35 119.2(3) . . ? C37 C36 H36A 120.4 . . ? C35 C36 H36A 120.4 . . ? C38 C37 C36 120.5(3) . . ? C38 C37 H37A 119.7 . . ? C36 C37 H37A 119.7 . . ? C37 C38 C39 118.1(3) . . ? C37 C38 H38A 121.0 . . ? C39 C38 H38A 121.0 . . ? N3 C39 C38 122.4(3) . . ? N3 C39 H39A 118.8 . . ? C38 C39 H39A 118.8 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? C9 C10' H10D 109.5 . . ? C9 C10' H10E 109.5 . . ? H10D C10' H10E 109.5 . . ? C9 C10' H10F 109.5 . . ? H10D C10' H10F 109.5 . . ? H10E C10' H10F 109.5 . . ? C9 C11' H11D 109.5 . . ? C9 C11' H11E 109.5 . . ? H11D C11' H11E 109.5 . . ? C9 C11' H11F 109.5 . . ? H11D C11' H11F 109.5 . . ? H11E C11' H11F 109.5 . . ? C9 C12' H12D 109.5 . . ? C9 C12' H12E 109.5 . . ? H12D C12' H12E 109.5 . . ? C9 C12' H12F 109.5 . . ? H12D C12' H12F 109.5 . . ? H12E C12' H12F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O7 Co1 O1 C7 79.94(16) 1_545 . . . ? N2 Co1 O1 C7 176.83(16) . . . . ? N1 Co1 O1 C7 -163.0(3) . . . . ? O6 Co1 O1 C7 -26.67(16) . . . . ? O5 Co1 O1 C7 -85.07(16) . . . . ? O8 Co2 O2 C7 -55.6(2) 1_545 . . . ? O8 Co2 O2 C7 124.4(2) 7_565 . . . ? 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 O1W H1C O2W 0.86(3) 2.00(3) 2.833(3) 161(3) . O1W H1D O7 0.85(3) 2.08(3) 2.927(3) 172(3) . O2W H2C O3W 0.85(3) 2.32(4) 2.791(7) 115(4) . O2W H2D O5 0.85(3) 1.95(3) 2.786(3) 169(3) . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.425 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.053 #============================================================================== data_CoPhen1-[Co(tbip)(phen)(H2O)]n _database_code_depnum_ccdc_archive 'CCDC 835411' #TrackingRef '- revised cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H22 Co N2 O5' _chemical_formula_sum 'C24 H22 Co N2 O5' _chemical_formula_weight 477.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.3721(7) _cell_length_b 12.7909(6) _cell_length_c 12.5990(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.234(1) _cell_angle_gamma 90.00 _cell_volume 2297.66(19) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6189 _cell_measurement_theta_min 2.2783 _cell_measurement_theta_max 27.6926 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.380 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 988 _exptl_absorpt_coefficient_mu 0.784 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8465 _exptl_absorpt_correction_T_max 0.8527 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18582 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 28.46 _reflns_number_total 5354 _reflns_number_gt 4214 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0764P)^2^+0.3367P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5354 _refine_ls_number_parameters 292 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1309 _refine_ls_wR_factor_gt 0.1229 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 Co1 Co 0.14142(2) 0.43504(2) 0.63591(2) 0.02836(12) Uani 1 1 d . . . N1 N 0.10275(14) 0.30010(14) 0.54056(15) 0.0303(4) Uani 1 1 d . . . N2 N 0.20830(14) 0.31513(15) 0.72911(15) 0.0323(4) Uani 1 1 d . . . O1W O 0.00638(11) 0.44663(12) 0.67751(13) 0.0346(4) Uani 1 1 d . . . H1WA H 0.0027 0.4984 0.7152 0.052 Uiso 1 1 calc R . . H1WB H -0.0356 0.4495 0.6237 0.052 Uiso 1 1 d R . . O1 O 0.11646(12) 0.54468(13) 0.50851(14) 0.0361(4) Uani 1 1 d . . . O2 O 0.26097(12) 0.49479(13) 0.55627(15) 0.0402(4) Uani 1 1 d . . . O3 O 0.05763(12) 0.87693(14) 0.29075(15) 0.0418(4) Uani 1 1 d . . . O4 O 0.18515(13) 0.95936(14) 0.25071(16) 0.0449(5) Uani 1 1 d . . . C1 C 0.23673(16) 0.64148(17) 0.43858(18) 0.0296(5) Uani 1 1 d . . . C2 C 0.17542(16) 0.71863(17) 0.39644(18) 0.0298(5) Uani 1 1 d . . . H2A H 0.1134 0.7184 0.4104 0.036 Uiso 1 1 calc R . . C3 C 0.20716(16) 0.79618(18) 0.33335(19) 0.0321(5) Uani 1 1 d . . . C4 C 0.29912(18) 0.7935(2) 0.3107(2) 0.0423(6) Uani 1 1 d . . . H4A H 0.3196 0.8453 0.2673 0.051 Uiso 1 1 calc R . . C5 C 0.36201(17) 0.7156(2) 0.3508(2) 0.0421(6) Uani 1 1 d . . . C6 C 0.32932(16) 0.64128(19) 0.4175(2) 0.0352(5) Uani 1 1 d . . . H6A H 0.3702 0.5904 0.4486 0.042 Uiso 1 1 calc R . . C7 C 0.20391(17) 0.55537(17) 0.50539(19) 0.0314(5) Uani 1 1 d . . . C8 C 0.14351(17) 0.88311(18) 0.28805(18) 0.0324(5) Uani 1 1 d . . . C9 C 0.4616(2) 0.7134(3) 0.3193(3) 0.0671(10) Uani 1 1 d . . . C10 C 0.5221(3) 0.6276(4) 0.3800(5) 0.1111(18) Uani 1 1 d . . . H10A H 0.4994 0.5601 0.3555 0.167 Uiso 1 1 calc R . . H10B H 0.5185 0.6339 0.4553 0.167 Uiso 1 1 calc R . . H10C H 0.5861 0.6354 0.3669 0.167 Uiso 1 1 calc R . . C11 C 0.5109(3) 0.8167(4) 0.3544(6) 0.125(2) Uani 1 1 d . . . H11A H 0.4808 0.8733 0.3135 0.187 Uiso 1 1 calc R . . H11B H 0.5755 0.8130 0.3426 0.187 Uiso 1 1 calc R . . H11C H 0.5072 0.8282 0.4291 0.187 Uiso 1 1 calc R . . C12 C 0.4556(3) 0.6998(7) 0.2009(4) 0.158(3) Uani 1 1 d . . . H12A H 0.4272 0.6336 0.1809 0.237 Uiso 1 1 calc R . . H12B H 0.5174 0.7022 0.1799 0.237 Uiso 1 1 calc R . . H12C H 0.4182 0.7550 0.1658 0.237 Uiso 1 1 calc R . . C13 C 0.04992(18) 0.29342(19) 0.44691(19) 0.0365(5) Uani 1 1 d . . . H13A H 0.0252 0.3547 0.4151 0.044 Uiso 1 1 calc R . . C14 C 0.02953(19) 0.1990(2) 0.3935(2) 0.0420(6) Uani 1 1 d . . . H14A H -0.0074 0.1982 0.3274 0.050 Uiso 1 1 calc R . . C15 C 0.06415(19) 0.1081(2) 0.4390(2) 0.0416(6) Uani 1 1 d . . . H15A H 0.0509 0.0446 0.4044 0.050 Uiso 1 1 calc R . . C16 C 0.12008(18) 0.11161(18) 0.5387(2) 0.0366(6) Uani 1 1 d . . . C17 C 0.1599(2) 0.0211(2) 0.5936(3) 0.0504(7) Uani 1 1 d . . . H17A H 0.1498 -0.0443 0.5618 0.061 Uiso 1 1 calc R . . C18 C 0.2113(2) 0.0283(2) 0.6897(3) 0.0521(7) Uani 1 1 d . . . H18A H 0.2356 -0.0321 0.7238 0.062 Uiso 1 1 calc R . . C19 C 0.22945(18) 0.1275(2) 0.7407(2) 0.0399(6) Uani 1 1 d . . . C20 C 0.28139(19) 0.1418(2) 0.8421(2) 0.0484(7) Uani 1 1 d . . . H20A H 0.3064 0.0842 0.8808 0.058 Uiso 1 1 calc R . . C21 C 0.29502(19) 0.2393(2) 0.8834(2) 0.0477(7) Uani 1 1 d . . . H21A H 0.3287 0.2487 0.9507 0.057 Uiso 1 1 calc R . . C22 C 0.25821(18) 0.3249(2) 0.8245(2) 0.0404(6) Uani 1 1 d . . . H22A H 0.2690 0.3915 0.8530 0.049 Uiso 1 1 calc R . . C23 C 0.19317(16) 0.21815(18) 0.68825(19) 0.0308(5) Uani 1 1 d . . . C24 C 0.13712(16) 0.21025(17) 0.58594(19) 0.0292(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.03321(19) 0.02137(17) 0.02928(18) 0.00004(12) -0.00086(13) 0.00119(12) N1 0.0369(11) 0.0239(9) 0.0296(10) 0.0009(8) 0.0025(8) 0.0024(8) N2 0.0327(10) 0.0318(10) 0.0320(10) 0.0033(8) 0.0020(8) 0.0017(8) O1W 0.0356(9) 0.0335(9) 0.0337(9) 0.0018(7) 0.0000(7) -0.0008(7) O1 0.0319(9) 0.0349(9) 0.0403(10) 0.0100(7) 0.0003(7) -0.0038(7) O2 0.0407(10) 0.0316(9) 0.0481(11) 0.0113(8) 0.0042(8) 0.0095(7) O3 0.0356(10) 0.0364(10) 0.0532(11) 0.0098(8) 0.0051(8) 0.0040(7) O4 0.0409(10) 0.0368(10) 0.0538(12) 0.0201(8) -0.0068(9) -0.0058(8) C1 0.0305(12) 0.0253(11) 0.0324(12) 0.0002(9) 0.0012(9) -0.0011(9) C2 0.0278(11) 0.0259(11) 0.0357(12) 0.0008(9) 0.0042(9) 0.0000(9) C3 0.0344(12) 0.0272(11) 0.0338(12) 0.0025(9) 0.0011(10) -0.0003(9) C4 0.0372(14) 0.0428(14) 0.0476(15) 0.0137(12) 0.0088(11) -0.0054(11) C5 0.0310(13) 0.0440(15) 0.0517(16) 0.0067(12) 0.0071(11) -0.0010(11) C6 0.0311(12) 0.0314(12) 0.0419(14) 0.0021(10) -0.0003(10) 0.0033(10) C7 0.0367(13) 0.0240(11) 0.0327(12) -0.0030(9) 0.0005(10) -0.0002(9) C8 0.0406(14) 0.0264(12) 0.0285(12) 0.0004(9) -0.0021(10) -0.0020(10) C9 0.0331(16) 0.083(2) 0.089(3) 0.022(2) 0.0190(16) 0.0034(16) C10 0.041(2) 0.125(4) 0.171(5) 0.046(4) 0.031(3) 0.026(2) C11 0.049(2) 0.106(4) 0.223(7) 0.037(4) 0.026(3) -0.020(2) C12 0.068(3) 0.326(10) 0.087(4) 0.010(5) 0.043(3) 0.036(4) C13 0.0442(14) 0.0312(12) 0.0330(12) -0.0004(10) 0.0006(10) 0.0040(10) C14 0.0464(15) 0.0432(15) 0.0350(13) -0.0084(11) 0.0000(11) -0.0011(12) C15 0.0501(15) 0.0321(13) 0.0433(15) -0.0129(11) 0.0091(12) -0.0045(11) C16 0.0410(14) 0.0254(12) 0.0450(14) -0.0004(10) 0.0115(11) -0.0019(10) C17 0.0608(18) 0.0242(13) 0.066(2) 0.0006(13) 0.0080(15) 0.0021(12) C18 0.0587(18) 0.0286(13) 0.068(2) 0.0143(13) 0.0034(15) 0.0060(12) C19 0.0372(13) 0.0355(13) 0.0477(15) 0.0139(11) 0.0080(11) 0.0047(11) C20 0.0445(16) 0.0506(17) 0.0491(16) 0.0226(14) 0.0027(13) 0.0099(13) C21 0.0400(15) 0.0639(19) 0.0368(14) 0.0101(13) -0.0048(12) 0.0051(13) C22 0.0374(13) 0.0460(15) 0.0362(13) 0.0014(11) -0.0018(11) 0.0004(11) C23 0.0303(11) 0.0278(11) 0.0354(12) 0.0049(9) 0.0085(10) 0.0017(9) C24 0.0309(12) 0.0249(11) 0.0329(12) 0.0028(9) 0.0084(9) 0.0008(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O4 2.0205(17) 4_576 ? Co1 O1W 2.0784(17) . ? Co1 N2 2.0906(19) . ? Co1 O1 2.1277(16) . ? Co1 N1 2.1362(19) . ? Co1 O2 2.2310(18) . ? Co1 C7 2.500(2) . ? N1 C13 1.323(3) . ? N1 C24 1.349(3) . ? N2 C22 1.325(3) . ? N2 C23 1.350(3) . ? O1W H1WA 0.8200 . ? O1W H1WB 0.8499 . ? O1 C7 1.270(3) . ? O2 C7 1.246(3) . ? O3 C8 1.242(3) . ? O4 C8 1.265(3) . ? O4 Co1 2.0205(17) 4_575 ? C1 C2 1.384(3) . ? C1 C6 1.389(3) . ? C1 C7 1.498(3) . ? C2 C3 1.384(3) . ? C2 H2A 0.9300 . ? C3 C4 1.387(3) . ? C3 C8 1.506(3) . ? C4 C5 1.396(4) . ? C4 H4A 0.9300 . ? C5 C6 1.389(4) . ? C5 C9 1.533(4) . ? C6 H6A 0.9300 . ? C9 C12 1.493(6) . ? C9 C11 1.538(6) . ? C9 C10 1.542(5) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.395(3) . ? C13 H13A 0.9300 . ? C14 C15 1.362(4) . ? C14 H14A 0.9300 . ? C15 C16 1.404(4) . ? C15 H15A 0.9300 . ? C16 C24 1.403(3) . ? C16 C17 1.431(4) . ? C17 C18 1.340(4) . ? C17 H17A 0.9300 . ? C18 C19 1.431(4) . ? C18 H18A 0.9300 . ? C19 C23 1.402(3) . ? C19 C20 1.408(4) . ? C20 C21 1.356(4) . ? C20 H20A 0.9300 . ? C21 C22 1.390(4) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C24 1.435(3) . ? 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 O4 Co1 O1W 89.31(7) 4_576 . ? O4 Co1 N2 90.51(8) 4_576 . ? O1W Co1 N2 106.77(7) . . ? O4 Co1 O1 96.15(8) 4_576 . ? O1W Co1 O1 93.96(6) . . ? N2 Co1 O1 158.31(7) . . ? O4 Co1 N1 168.01(8) 4_576 . ? O1W Co1 N1 90.82(7) . . ? N2 Co1 N1 77.98(8) . . ? O1 Co1 N1 95.80(7) . . ? O4 Co1 O2 84.56(8) 4_576 . ? O1W Co1 O2 152.31(6) . . ? N2 Co1 O2 100.27(7) . . ? O1 Co1 O2 60.07(6) . . ? N1 Co1 O2 100.63(7) . . ? O4 Co1 C7 87.38(8) 4_576 . ? O1W Co1 C7 123.10(7) . . ? N2 Co1 C7 130.03(8) . . ? O1 Co1 C7 30.51(7) . . ? N1 Co1 C7 102.54(7) . . ? O2 Co1 C7 29.84(7) . . ? C13 N1 C24 117.5(2) . . ? C13 N1 Co1 129.29(16) . . ? C24 N1 Co1 113.23(15) . . ? C22 N2 C23 118.4(2) . . ? C22 N2 Co1 126.73(17) . . ? C23 N2 Co1 114.79(15) . . ? Co1 O1W H1WA 109.5 . . ? Co1 O1W H1WB 113.2 . . ? H1WA O1W H1WB 109.6 . . ? C7 O1 Co1 91.19(14) . . ? C7 O2 Co1 87.14(15) . . ? C8 O4 Co1 131.47(16) . 4_575 ? C2 C1 C6 120.5(2) . . ? C2 C1 C7 120.6(2) . . ? C6 C1 C7 118.9(2) . . ? C1 C2 C3 119.4(2) . . ? C1 C2 H2A 120.3 . . ? C3 C2 H2A 120.3 . . ? C2 C3 C4 119.5(2) . . ? C2 C3 C8 121.2(2) . . ? C4 C3 C8 119.3(2) . . ? C3 C4 C5 122.2(2) . . ? C3 C4 H4A 118.9 . . ? C5 C4 H4A 118.9 . . ? C6 C5 C4 117.0(2) . . ? C6 C5 C9 122.8(2) . . ? C4 C5 C9 120.2(2) . . ? C5 C6 C1 121.3(2) . . ? C5 C6 H6A 119.4 . . ? C1 C6 H6A 119.4 . . ? O2 C7 O1 120.5(2) . . ? O2 C7 C1 120.9(2) . . ? O1 C7 C1 118.6(2) . . ? O2 C7 Co1 63.03(13) . . ? O1 C7 Co1 58.30(12) . . ? C1 C7 Co1 170.66(16) . . ? O3 C8 O4 125.3(2) . . ? O3 C8 C3 120.1(2) . . ? O4 C8 C3 114.6(2) . . ? C12 C9 C5 108.8(3) . . ? C12 C9 C11 110.7(5) . . ? C5 C9 C11 108.7(3) . . ? C12 C9 C10 111.8(4) . . ? C5 C9 C10 111.8(3) . . ? C11 C9 C10 105.0(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C14 123.2(2) . . ? N1 C13 H13A 118.4 . . ? C14 C13 H13A 118.4 . . ? C15 C14 C13 119.5(2) . . ? C15 C14 H14A 120.2 . . ? C13 C14 H14A 120.2 . . ? C14 C15 C16 119.1(2) . . ? C14 C15 H15A 120.4 . . ? C16 C15 H15A 120.4 . . ? C24 C16 C15 117.2(2) . . ? C24 C16 C17 119.0(2) . . ? C15 C16 C17 123.8(2) . . ? C18 C17 C16 121.5(3) . . ? C18 C17 H17A 119.3 . . ? C16 C17 H17A 119.3 . . ? C17 C18 C19 121.0(3) . . ? C17 C18 H18A 119.5 . . ? C19 C18 H18A 119.5 . . ? C23 C19 C20 116.3(2) . . ? C23 C19 C18 119.1(2) . . ? C20 C19 C18 124.6(2) . . ? C21 C20 C19 120.2(2) . . ? C21 C20 H20A 119.9 . . ? C19 C20 H20A 119.9 . . ? C20 C21 C22 119.5(3) . . ? C20 C21 H21A 120.3 . . ? C22 C21 H21A 120.3 . . ? N2 C22 C21 122.4(3) . . ? N2 C22 H22A 118.8 . . ? C21 C22 H22A 118.8 . . ? N2 C23 C19 123.2(2) . . ? N2 C23 C24 116.9(2) . . ? C19 C23 C24 119.9(2) . . ? N1 C24 C16 123.4(2) . . ? N1 C24 C23 117.0(2) . . ? C16 C24 C23 119.5(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Co1 N1 C13 163.3(3) 4_576 . . . ? O1W Co1 N1 C13 72.8(2) . . . . ? N2 Co1 N1 C13 179.8(2) . . . . ? O1 Co1 N1 C13 -21.3(2) . . . . ? O2 Co1 N1 C13 -81.9(2) . . . . ? C7 Co1 N1 C13 -51.4(2) . . . . ? O4 Co1 N1 C24 -15.4(5) 4_576 . . . ? O1W Co1 N1 C24 -105.92(16) . . . . ? N2 Co1 N1 C24 1.06(16) . . . . ? O1 Co1 N1 C24 160.02(16) . . . . ? O2 Co1 N1 C24 99.43(16) . . . . ? C7 Co1 N1 C24 129.84(16) . . . . ? O4 Co1 N2 C22 -1.2(2) 4_576 . . . ? O1W Co1 N2 C22 -90.6(2) . . . . ? O1 Co1 N2 C22 107.0(3) . . . . ? N1 Co1 N2 C22 -177.8(2) . . . . ? O2 Co1 N2 C22 83.4(2) . . . . ? C7 Co1 N2 C22 85.8(2) . . . . ? O4 Co1 N2 C23 174.81(17) 4_576 . . . ? O1W Co1 N2 C23 85.38(17) . . . . ? O1 Co1 N2 C23 -77.0(3) . . . . ? N1 Co1 N2 C23 -1.82(16) . . . . ? O2 Co1 N2 C23 -100.62(17) . . . . ? C7 Co1 N2 C23 -98.19(17) . . . . ? O4 Co1 O1 C7 74.12(14) 4_576 . . . ? O1W Co1 O1 C7 163.86(14) . . . . ? N2 Co1 O1 C7 -33.0(3) . . . . ? N1 Co1 O1 C7 -104.91(14) . . . . ? O2 Co1 O1 C7 -5.97(13) . . . . ? O4 Co1 O2 C7 -94.22(14) 4_576 . . . ? O1W Co1 O2 C7 -16.2(2) . . . . ? N2 Co1 O2 C7 176.25(14) . . . . ? O1 Co1 O2 C7 6.09(13) . . . . ? N1 Co1 O2 C7 96.70(14) . . . . ? C6 C1 C2 C3 -0.3(3) . . . . ? C7 C1 C2 C3 -178.8(2) . . . . ? C1 C2 C3 C4 2.0(4) . . . . ? C1 C2 C3 C8 -178.5(2) . . . . ? C2 C3 C4 C5 -1.0(4) . . . . ? C8 C3 C4 C5 179.5(2) . . . . ? C3 C4 C5 C6 -1.6(4) . . . . ? C3 C4 C5 C9 177.2(3) . . . . ? C4 C5 C6 C1 3.3(4) . . . . ? C9 C5 C6 C1 -175.5(3) . . . . ? C2 C1 C6 C5 -2.4(4) . . . . ? C7 C1 C6 C5 176.1(2) . . . . ? Co1 O2 C7 O1 -10.3(2) . . . . ? Co1 O2 C7 C1 170.3(2) . . . . ? Co1 O1 C7 O2 10.8(2) . . . . ? Co1 O1 C7 C1 -169.78(18) . . . . ? C2 C1 C7 O2 -169.4(2) . . . . ? C6 C1 C7 O2 12.1(3) . . . . ? C2 C1 C7 O1 11.2(3) . . . . ? C6 C1 C7 O1 -167.3(2) . . . . ? O4 Co1 C7 O2 83.64(14) 4_576 . . . ? O1W Co1 C7 O2 171.10(12) . . . . ? N2 Co1 C7 O2 -4.82(18) . . . . ? O1 Co1 C7 O2 -169.6(2) . . . . ? N1 Co1 C7 O2 -89.55(14) . . . . ? O4 Co1 C7 O1 -106.80(14) 4_576 . . . ? O1W Co1 C7 O1 -19.34(16) . . . . ? N2 Co1 C7 O1 164.74(13) . . . . ? N1 Co1 C7 O1 80.01(14) . . . . ? O2 Co1 C7 O1 169.6(2) . . . . ? Co1 O4 C8 O3 -27.8(4) 4_575 . . . ? Co1 O4 C8 C3 153.26(18) 4_575 . . . ? C2 C3 C8 O3 -12.6(3) . . . . ? C4 C3 C8 O3 166.9(2) . . . . ? C2 C3 C8 O4 166.3(2) . . . . ? C4 C3 C8 O4 -14.1(3) . . . . ? C6 C5 C9 C12 117.6(5) . . . . ? C4 C5 C9 C12 -61.2(5) . . . . ? C6 C5 C9 C11 -121.8(4) . . . . ? C4 C5 C9 C11 59.4(4) . . . . ? C6 C5 C9 C10 -6.3(5) . . . . ? C4 C5 C9 C10 174.9(3) . . . . ? C24 N1 C13 C14 -0.7(4) . . . . ? Co1 N1 C13 C14 -179.41(19) . . . . ? N1 C13 C14 C15 0.7(4) . . . . ? C13 C14 C15 C16 -0.3(4) . . . . ? C14 C15 C16 C24 -0.1(4) . . . . ? C14 C15 C16 C17 180.0(3) . . . . ? C24 C16 C17 C18 1.3(4) . . . . ? C15 C16 C17 C18 -178.7(3) . . . . ? C16 C17 C18 C19 -0.8(5) . . . . ? C17 C18 C19 C23 -0.5(4) . . . . ? C17 C18 C19 C20 178.9(3) . . . . ? C23 C19 C20 C21 -0.8(4) . . . . ? C18 C19 C20 C21 179.7(3) . . . . ? C19 C20 C21 C22 -0.7(4) . . . . ? C23 N2 C22 C21 -0.2(4) . . . . ? Co1 N2 C22 C21 175.7(2) . . . . ? C20 C21 C22 N2 1.2(4) . . . . ? C22 N2 C23 C19 -1.5(3) . . . . ? Co1 N2 C23 C19 -177.85(18) . . . . ? C22 N2 C23 C24 178.7(2) . . . . ? Co1 N2 C23 C24 2.3(3) . . . . ? C20 C19 C23 N2 2.0(4) . . . . ? C18 C19 C23 N2 -178.6(2) . . . . ? C20 C19 C23 C24 -178.2(2) . . . . ? C18 C19 C23 C24 1.3(4) . . . . ? C13 N1 C24 C16 0.4(4) . . . . ? Co1 N1 C24 C16 179.27(19) . . . . ? C13 N1 C24 C23 -179.1(2) . . . . ? Co1 N1 C24 C23 -0.2(3) . . . . ? C15 C16 C24 N1 0.0(4) . . . . ? C17 C16 C24 N1 180.0(2) . . . . ? C15 C16 C24 C23 179.5(2) . . . . ? C17 C16 C24 C23 -0.5(4) . . . . ? N2 C23 C24 N1 -1.4(3) . . . . ? C19 C23 C24 N1 178.8(2) . . . . ? N2 C23 C24 C16 179.1(2) . . . . ? C19 C23 C24 C16 -0.7(3) . . . . ? 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 O1W H1WA O3 0.82 1.97 2.721(2) 151.9 4_576 O1W H1WB O1 0.85 1.91 2.753(2) 172.4 3_566 _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.565 _refine_diff_density_min -0.370 _refine_diff_density_rms 0.084 #============================================================================== data_CoPhen2-{[Co3(tbip)3(phen)2Co(tbip)(phen)].1.5H2O}n _database_code_depnum_ccdc_archive 'CCDC 835412' #TrackingRef '- revised cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C42 H36 Co2 N3 O8), 1.5(H2 O)' _chemical_formula_sum 'C84 H75 Co4 N6 O17.50' _chemical_formula_weight 1684.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 32.932(7) _cell_length_b 9.4843(19) _cell_length_c 27.667(6) _cell_angle_alpha 90.00 _cell_angle_beta 116.54(3) _cell_angle_gamma 90.00 _cell_volume 7731(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 17250 _cell_measurement_theta_min 6.22 _cell_measurement_theta_max 55.10 _exptl_crystal_description rod _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3476 _exptl_absorpt_coefficient_mu 0.918 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7897 _exptl_absorpt_correction_T_max 0.9138 _exptl_absorpt_process_details 'Tompa_analytical (Rigaku Corporation, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Rigaku R-AXIS RAPID imaging plate' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29056 _diffrn_reflns_av_R_equivalents 0.0766 _diffrn_reflns_av_sigmaI/netI 0.0851 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8307 _reflns_number_gt 4468 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'PROCESS-AUTO (Rigaku Corporation,1998)' _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan (Molecular Structure Corporation & Rigaku Corporation, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1344P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0015(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8307 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1328 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.2255 _refine_ls_wR_factor_gt 0.1645 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.16959(3) 0.22210(6) 0.55031(3) 0.0377(2) Uani 1 1 d . . . Co2 Co 0.2500 0.2500 0.5000 0.0404(3) Uani 1 2 d S . . Co3 Co 0.5000 0.48486(9) 0.7500 0.0456(3) Uani 1 2 d S . . O1 O 0.22979(15) 0.2359(3) 0.61765(14) 0.0456(10) Uani 1 1 d . . . O2 O 0.27901(15) 0.2743(4) 0.58291(15) 0.0530(11) Uani 1 1 d . . . O3 O 0.44008(15) 0.3651(3) 0.69991(16) 0.0519(10) Uani 1 1 d . . . O4 O 0.45961(13) 0.4100(4) 0.78563(16) 0.0527(10) Uani 1 1 d . . . O5 O 0.18700(13) 0.3348(3) 0.49356(13) 0.0404(9) Uani 1 1 d . . . O6 O 0.16363(13) 0.4562(3) 0.54379(13) 0.0441(9) Uani 1 1 d . . . O7 O 0.17284(13) 1.0149(3) 0.53165(13) 0.0433(9) Uani 1 1 d . . . O8 O 0.22464(14) 1.0564(3) 0.50174(15) 0.0515(10) Uani 1 1 d . . . N1 N 0.09961(17) 0.2169(4) 0.49061(16) 0.0421(11) Uani 1 1 d . . . N2 N 0.1348(2) 0.1762(4) 0.59706(17) 0.0513(14) Uani 1 1 d . . . N3 N 0.52851(17) 0.6572(4) 0.8023(2) 0.0479(12) Uani 1 1 d . . . C1 C 0.3085(2) 0.2561(4) 0.67680(18) 0.0364(12) Uani 1 1 d . . . C2 C 0.3501(2) 0.3007(4) 0.6823(2) 0.0386(12) Uani 1 1 d . . . H2A H 0.3535 0.3308 0.6516 0.046 Uiso 1 1 calc R . . C3 C 0.3873(2) 0.3013(4) 0.7335(2) 0.0413(13) Uani 1 1 d . . . C4 C 0.38216(18) 0.2502(5) 0.7769(2) 0.0385(12) Uani 1 1 d . . . H4A H 0.4077 0.2504 0.8114 0.046 Uiso 1 1 calc R . . C5 C 0.34167(19) 0.1990(5) 0.77259(19) 0.0388(12) Uani 1 1 d . . . C6 C 0.30408(19) 0.2062(4) 0.72151(19) 0.0366(11) Uani 1 1 d . . . H6A H 0.2752 0.1765 0.7174 0.044 Uiso 1 1 calc R . . C7 C 0.2691(2) 0.2563(4) 0.6213(2) 0.0405(13) Uani 1 1 d . . . C8 C 0.4308(2) 0.3610(5) 0.7396(2) 0.0449(13) Uani 1 1 d . . . C9 C 0.3382(2) 0.1357(6) 0.8218(2) 0.0461(13) Uani 1 1 d . . . C10 C 0.3764(3) 0.0321(7) 0.8498(3) 0.081(2) Uani 1 1 d . . . H10A H 0.3740 -0.0442 0.8248 0.121 Uiso 1 1 calc R . . H10B H 0.3744 -0.0072 0.8814 0.121 Uiso 1 1 calc R . . H10C H 0.4055 0.0805 0.8613 0.121 Uiso 1 1 calc R . . C11 C 0.2942(3) 0.0609(12) 0.8077(3) 0.134(4) Uani 1 1 d . . . H11A H 0.2921 -0.0222 0.7856 0.201 Uiso 1 1 calc R . . H11B H 0.2688 0.1247 0.7873 0.201 Uiso 1 1 calc R . . H11C H 0.2929 0.0313 0.8409 0.201 Uiso 1 1 calc R . . C12 C 0.3449(4) 0.2547(7) 0.8622(3) 0.103(3) Uani 1 1 d . . . H12A H 0.3500 0.2141 0.8970 0.155 Uiso 1 1 calc R . . H12B H 0.3179 0.3146 0.8484 0.155 Uiso 1 1 calc R . . H12C H 0.3714 0.3113 0.8669 0.155 Uiso 1 1 calc R . . C13 C 0.18116(19) 0.5859(4) 0.48146(18) 0.0396(13) Uani 1 1 d . . . C14 C 0.1831(2) 0.7154(4) 0.5057(2) 0.0421(13) Uani 1 1 d . . . H14A H 0.1802 0.7208 0.5383 0.051 Uiso 1 1 calc R . . C15 C 0.1893(2) 0.8370(4) 0.48189(19) 0.0416(13) Uani 1 1 d . . . C16 C 0.1912(2) 0.8280(4) 0.4327(2) 0.0424(13) Uani 1 1 d . . . H16A H 0.1961 0.9117 0.4172 0.051 Uiso 1 1 calc R . . C17 C 0.18609(19) 0.7015(4) 0.40552(18) 0.0381(12) Uani 1 1 d . . . C18 C 0.18200(19) 0.5793(4) 0.43200(19) 0.0425(13) Uani 1 1 d . . . H18A H 0.1798 0.4901 0.4154 0.051 Uiso 1 1 calc R . . C19 C 0.17775(19) 0.4534(4) 0.50876(19) 0.0385(13) Uani 1 1 d . . . C20 C 0.1960(2) 0.9804(4) 0.50774(19) 0.0412(13) Uani 1 1 d . . . C21 C 0.1863(2) 0.6920(5) 0.35104(19) 0.0413(13) Uani 1 1 d . . . C22 C 0.1441(2) 0.6147(6) 0.3105(2) 0.0578(17) Uani 1 1 d . . . H22A H 0.1424 0.5215 0.3248 0.087 Uiso 1 1 calc R . . H22B H 0.1459 0.6037 0.2762 0.087 Uiso 1 1 calc R . . H22C H 0.1169 0.6691 0.3044 0.087 Uiso 1 1 calc R . . C23 C 0.1877(3) 0.8395(5) 0.3278(2) 0.0636(19) Uani 1 1 d . . . H23A H 0.1598 0.8909 0.3207 0.095 Uiso 1 1 calc R . . H23B H 0.1904 0.8288 0.2941 0.095 Uiso 1 1 calc R . . H23C H 0.2139 0.8921 0.3540 0.095 Uiso 1 1 calc R . . C24 C 0.2287(2) 0.6121(5) 0.3575(2) 0.0482(14) Uani 1 1 d . . . H24A H 0.2290 0.5185 0.3727 0.072 Uiso 1 1 calc R . . H24B H 0.2558 0.6645 0.3818 0.072 Uiso 1 1 calc R . . H24C H 0.2284 0.6020 0.3221 0.072 Uiso 1 1 calc R . . C25 C 0.0830(2) 0.2238(5) 0.4371(2) 0.0516(15) Uani 1 1 d . . . H25A H 0.1038 0.2356 0.4222 0.062 Uiso 1 1 calc R . . C26 C 0.0366(3) 0.2146(6) 0.4015(3) 0.066(2) Uani 1 1 d . . . H26A H 0.0264 0.2164 0.3635 0.079 Uiso 1 1 calc R . . C27 C 0.0069(3) 0.2029(7) 0.4228(3) 0.080(2) Uani 1 1 d . . . H27A H -0.0248 0.2000 0.3998 0.096 Uiso 1 1 calc R . . C28 C 0.0232(3) 0.1952(7) 0.4794(3) 0.071(2) Uani 1 1 d . . . C29 C -0.0056(3) 0.1757(10) 0.5048(4) 0.099(3) Uani 1 1 d . . . H29A H -0.0376 0.1765 0.4833 0.118 Uiso 1 1 calc R . . C30 C 0.0107(4) 0.1565(9) 0.5573(4) 0.100(3) Uani 1 1 d . . . H30A H -0.0097 0.1459 0.5727 0.120 Uiso 1 1 calc R . . C31 C 0.0590(4) 0.1512(7) 0.5919(3) 0.079(3) Uani 1 1 d . . . C32 C 0.0798(4) 0.1157(8) 0.6465(4) 0.104(4) Uani 1 1 d . . . H32A H 0.0616 0.0949 0.6642 0.124 Uiso 1 1 calc R . . C33 C 0.1250(4) 0.1105(8) 0.6744(3) 0.104(4) Uani 1 1 d . . . H33A H 0.1385 0.0842 0.7114 0.125 Uiso 1 1 calc R . . C34 C 0.1531(3) 0.1439(6) 0.6491(2) 0.076(2) Uani 1 1 d . . . H34A H 0.1852 0.1431 0.6697 0.091 Uiso 1 1 calc R . . C35 C 0.0892(3) 0.1761(5) 0.5695(2) 0.0534(17) Uani 1 1 d . . . C36 C 0.0706(2) 0.1995(5) 0.5120(2) 0.0499(15) Uani 1 1 d . . . C37 C 0.5563(2) 0.6537(6) 0.8543(3) 0.0585(17) Uani 1 1 d . . . H37A H 0.5659 0.5645 0.8712 0.070 Uiso 1 1 calc R . . C38 C 0.5723(2) 0.7764(6) 0.8861(3) 0.0642(18) Uani 1 1 d . . . H38A H 0.5925 0.7702 0.9235 0.077 Uiso 1 1 calc R . . C39 C 0.5582(3) 0.9039(6) 0.8616(3) 0.075(2) Uani 1 1 d . . . H39A H 0.5682 0.9880 0.8823 0.090 Uiso 1 1 calc R . . C40 C 0.5289(3) 0.9117(6) 0.8058(3) 0.070(2) Uani 1 1 d . . . C41 C 0.5134(3) 1.0401(6) 0.7758(3) 0.090(3) Uani 1 1 d . . . H41A H 0.5230 1.1277 0.7941 0.109 Uiso 1 1 calc R . . C42 C 0.5144(2) 0.7830(5) 0.7779(2) 0.0519(15) Uani 1 1 d . . . O1W O 0.1004(6) 0.8693(16) 0.5128(9) 0.199(9) Uani 0.50 1 d P . . H1WD H 0.0834 0.9403 0.5047 0.299 Uiso 0.50 1 calc PR . . H1WA H 0.1235 0.9192 0.5204 0.299 Uiso 0.50 1 d PR . . O2W O 0.0814(11) 0.586(3) 0.5037(12) 0.165(14) Uani 0.25 1 d P . . H2WA H 0.1071 0.5604 0.5270 0.248 Uiso 0.25 1 calc PR . . H2WB H 0.0865 0.6746 0.5057 0.248 Uiso 0.25 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0568(5) 0.0241(3) 0.0321(4) 0.0002(2) 0.0196(3) 0.0040(3) Co2 0.0685(8) 0.0227(4) 0.0318(5) 0.0017(3) 0.0239(5) 0.0047(4) Co3 0.0526(8) 0.0302(5) 0.0664(7) 0.000 0.0376(6) 0.000 O1 0.066(3) 0.0323(17) 0.034(2) 0.0016(13) 0.0178(19) 0.0064(16) O2 0.073(3) 0.051(2) 0.039(2) -0.0003(15) 0.028(2) -0.0013(18) O3 0.063(3) 0.0422(19) 0.070(3) -0.0012(16) 0.048(2) -0.0099(17) O4 0.052(3) 0.050(2) 0.066(3) -0.0116(18) 0.035(2) -0.0105(17) O5 0.062(3) 0.0239(15) 0.0386(19) 0.0033(12) 0.0256(18) 0.0042(14) O6 0.069(3) 0.0313(16) 0.039(2) 0.0028(13) 0.0306(19) 0.0063(15) O7 0.064(3) 0.0280(16) 0.040(2) -0.0032(13) 0.0248(19) 0.0025(15) O8 0.073(3) 0.0265(17) 0.056(2) -0.0007(14) 0.029(2) 0.0052(17) N1 0.065(4) 0.0253(19) 0.041(3) 0.0049(15) 0.028(2) 0.0021(18) N2 0.098(5) 0.027(2) 0.033(3) -0.0056(15) 0.032(3) -0.012(2) N3 0.050(3) 0.034(2) 0.067(3) 0.0000(19) 0.033(3) 0.0002(19) C1 0.053(4) 0.024(2) 0.030(3) -0.0011(16) 0.017(2) 0.0032(19) C2 0.055(4) 0.031(2) 0.038(3) 0.0030(18) 0.028(3) 0.001(2) C3 0.054(4) 0.027(2) 0.048(3) -0.0002(19) 0.027(3) -0.003(2) C4 0.030(3) 0.051(3) 0.033(3) -0.0039(19) 0.013(2) -0.006(2) C5 0.042(3) 0.041(3) 0.037(3) 0.0028(19) 0.021(3) -0.003(2) C6 0.039(3) 0.039(2) 0.035(3) -0.0021(18) 0.019(2) -0.004(2) C7 0.059(4) 0.024(2) 0.044(3) -0.0002(17) 0.028(3) 0.002(2) C8 0.051(4) 0.035(3) 0.062(4) -0.002(2) 0.037(3) -0.008(2) C9 0.046(4) 0.062(3) 0.034(3) 0.005(2) 0.022(3) -0.005(3) C10 0.083(6) 0.089(5) 0.074(5) 0.040(4) 0.038(4) 0.016(4) C11 0.099(8) 0.225(11) 0.068(5) 0.048(6) 0.028(5) -0.072(7) C12 0.186(11) 0.088(5) 0.072(5) 0.001(4) 0.091(7) 0.014(5) C13 0.060(4) 0.027(2) 0.032(3) 0.0002(17) 0.021(2) 0.002(2) C14 0.067(4) 0.023(2) 0.038(3) -0.0008(17) 0.025(3) 0.003(2) C15 0.063(4) 0.026(2) 0.034(3) 0.0011(17) 0.021(3) 0.005(2) C16 0.061(4) 0.025(2) 0.041(3) 0.0057(18) 0.023(3) 0.004(2) C17 0.057(4) 0.027(2) 0.030(2) 0.0013(17) 0.019(2) 0.005(2) C18 0.061(4) 0.023(2) 0.037(3) -0.0006(17) 0.016(3) 0.007(2) C19 0.057(4) 0.022(2) 0.035(3) 0.0020(17) 0.019(3) 0.010(2) C20 0.060(4) 0.026(2) 0.029(3) 0.0043(17) 0.013(3) 0.000(2) C21 0.057(4) 0.031(2) 0.035(3) 0.0042(18) 0.020(3) 0.008(2) C22 0.073(5) 0.061(3) 0.039(3) -0.006(2) 0.024(3) 0.005(3) C23 0.112(6) 0.035(3) 0.057(4) 0.007(2) 0.050(4) 0.010(3) C24 0.060(4) 0.048(3) 0.037(3) -0.001(2) 0.022(3) 0.007(3) C25 0.066(5) 0.042(3) 0.053(4) 0.008(2) 0.032(3) 0.000(3) C26 0.069(5) 0.063(4) 0.051(4) 0.016(3) 0.012(4) -0.012(3) C27 0.071(6) 0.080(5) 0.078(5) 0.029(4) 0.024(4) -0.003(4) C28 0.082(6) 0.063(4) 0.092(6) 0.009(3) 0.061(5) -0.001(4) C29 0.089(8) 0.112(7) 0.118(8) 0.008(5) 0.067(6) -0.005(5) C30 0.119(9) 0.103(6) 0.116(8) -0.018(5) 0.086(7) -0.029(6) C31 0.144(9) 0.063(4) 0.062(5) -0.013(3) 0.074(5) -0.026(4) C32 0.176(11) 0.092(5) 0.083(6) -0.036(4) 0.094(7) -0.073(6) C33 0.192(11) 0.087(5) 0.044(4) -0.019(4) 0.062(6) -0.071(6) C34 0.132(7) 0.055(3) 0.037(3) -0.007(2) 0.036(4) -0.036(4) C35 0.089(6) 0.037(3) 0.047(4) -0.006(2) 0.042(4) -0.012(3) C36 0.057(4) 0.040(3) 0.063(4) -0.001(2) 0.035(3) -0.008(2) C37 0.059(4) 0.046(3) 0.080(5) -0.008(3) 0.039(4) -0.003(3) C38 0.057(5) 0.066(4) 0.080(5) -0.017(3) 0.040(4) -0.007(3) C39 0.090(6) 0.052(4) 0.110(6) -0.025(4) 0.070(5) -0.020(3) C40 0.100(6) 0.039(3) 0.095(5) -0.013(3) 0.065(5) -0.009(3) C41 0.152(9) 0.033(3) 0.115(6) -0.008(3) 0.085(7) -0.010(4) C42 0.056(4) 0.039(3) 0.078(4) -0.006(2) 0.046(3) -0.003(2) O1W 0.163(17) 0.125(12) 0.36(3) -0.088(14) 0.163(19) -0.055(11) O2W 0.20(3) 0.086(17) 0.16(3) -0.026(16) 0.04(2) 0.033(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.029(4) . ? Co1 O7 2.047(3) 1_545 ? Co1 N2 2.121(5) . ? Co1 N1 2.154(5) . ? Co1 O5 2.177(3) . ? Co1 O6 2.229(3) . ? Co2 O8 2.027(4) 1_545 ? Co2 O8 2.027(4) 7_566 ? Co2 O2 2.066(4) 7_556 ? Co2 O2 2.066(4) . ? Co2 O5 2.157(4) . ? Co2 O5 2.157(4) 7_556 ? Co3 O4 2.102(4) 2_656 ? Co3 O4 2.102(4) . ? Co3 N3 2.106(4) 2_656 ? Co3 N3 2.106(4) . ? Co3 O3 2.159(4) . ? Co3 O3 2.159(4) 2_656 ? Co3 C8 2.463(6) . ? Co3 C8 2.463(6) 2_656 ? O1 C7 1.266(7) . ? O2 C7 1.256(7) . ? O3 C8 1.264(6) . ? O4 C8 1.288(6) . ? O5 C19 1.284(5) . ? O6 C19 1.249(6) . ? O7 C20 1.256(6) . ? O7 Co1 2.047(3) 1_565 ? O8 C20 1.255(6) . ? O8 Co2 2.027(3) 1_565 ? N1 C25 1.330(7) . ? N1 C36 1.342(7) . ? N2 C34 1.324(7) . ? N2 C35 1.347(8) . ? N3 C37 1.315(8) . ? N3 C42 1.348(7) . ? C1 C2 1.374(8) . ? C1 C6 1.392(7) . ? C1 C7 1.504(8) . ? C2 C3 1.399(7) . ? C2 H2A 0.9500 . ? C3 C4 1.374(7) . ? C3 C8 1.479(8) . ? C4 C5 1.373(7) . ? C4 H4A 0.9500 . ? C5 C6 1.404(7) . ? C5 C9 1.539(7) . ? C6 H6A 0.9500 . ? C9 C11 1.499(9) . ? C9 C10 1.509(8) . ? C9 C12 1.533(8) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C18 1.383(7) . ? C13 C14 1.387(6) . ? C13 C19 1.496(6) . ? C14 C15 1.388(6) . ? C14 H14A 0.9500 . ? C15 C16 1.392(7) . ? C15 C20 1.506(6) . ? C16 C17 1.386(6) . ? C16 H16A 0.9500 . ? C17 C18 1.409(6) . ? C17 C21 1.513(7) . ? C18 H18A 0.9500 . ? C21 C24 1.527(8) . ? C21 C22 1.528(8) . ? C21 C23 1.549(7) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.402(9) . ? C25 H25A 0.9500 . ? C26 C27 1.355(10) . ? C26 H26A 0.9500 . ? C27 C28 1.412(10) . ? C27 H27A 0.9500 . ? C28 C36 1.412(10) . ? C28 C29 1.422(11) . ? C29 C30 1.315(12) . ? C29 H29A 0.9500 . ? C30 C31 1.444(13) . ? C30 H30A 0.9500 . ? C31 C32 1.391(11) . ? C31 C35 1.409(9) . ? C32 C33 1.337(13) . ? C32 H32A 0.9500 . ? C33 C34 1.423(11) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? C35 C36 1.443(8) . ? C37 C38 1.411(8) . ? C37 H37A 0.9500 . ? C38 C39 1.362(9) . ? C38 H38A 0.9500 . ? C39 C40 1.412(10) . ? C39 H39A 0.9500 . ? C40 C42 1.408(8) . ? C40 C41 1.434(9) . ? C41 C41 1.299(15) 2_656 ? C41 H41A 0.9500 . ? C42 C42 1.404(12) 2_656 ? O1W H1WD 0.8400 . ? O1W H1WA 0.8400 . ? O2W H2WA 0.8400 . ? O2W H2WB 0.8499 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O7 98.85(14) . 1_545 ? O1 Co1 N2 91.47(19) . . ? O7 Co1 N2 93.44(15) 1_545 . ? O1 Co1 N1 167.71(17) . . ? O7 Co1 N1 86.75(14) 1_545 . ? N2 Co1 N1 77.22(19) . . ? O1 Co1 O5 99.57(15) . . ? O7 Co1 O5 103.24(13) 1_545 . ? N2 Co1 O5 158.21(16) . . ? N1 Co1 O5 89.69(15) . . ? O1 Co1 O6 91.41(13) . . ? O7 Co1 O6 161.54(13) 1_545 . ? N2 Co1 O6 101.65(14) . . ? N1 Co1 O6 86.30(13) . . ? O5 Co1 O6 59.65(12) . . ? O8 Co2 O8 180.000(1) 1_545 7_566 ? O8 Co2 O2 86.23(14) 1_545 7_556 ? O8 Co2 O2 93.77(14) 7_566 7_556 ? O8 Co2 O2 93.77(14) 1_545 . ? O8 Co2 O2 86.23(14) 7_566 . ? O2 Co2 O2 180.000(1) 7_556 . ? O8 Co2 O5 87.03(14) 1_545 . ? O8 Co2 O5 92.97(14) 7_566 . ? O2 Co2 O5 89.97(15) 7_556 . ? O2 Co2 O5 90.03(15) . . ? O8 Co2 O5 92.97(14) 1_545 7_556 ? O8 Co2 O5 87.03(14) 7_566 7_556 ? O2 Co2 O5 90.03(15) 7_556 7_556 ? O2 Co2 O5 89.97(15) . 7_556 ? O5 Co2 O5 180.00(17) . 7_556 ? O4 Co3 O4 140.5(2) 2_656 . ? O4 Co3 N3 96.94(16) 2_656 2_656 ? O4 Co3 N3 113.81(17) . 2_656 ? O4 Co3 N3 113.81(17) 2_656 . ? O4 Co3 N3 96.94(16) . . ? N3 Co3 N3 78.2(3) 2_656 . ? O4 Co3 O3 96.29(15) 2_656 . ? O4 Co3 O3 62.28(14) . . ? N3 Co3 O3 88.18(16) 2_656 . ? N3 Co3 O3 148.05(17) . . ? O4 Co3 O3 62.28(14) 2_656 2_656 ? O4 Co3 O3 96.29(15) . 2_656 ? N3 Co3 O3 148.05(17) 2_656 2_656 ? N3 Co3 O3 88.18(16) . 2_656 ? O3 Co3 O3 116.5(2) . 2_656 ? O4 Co3 C8 122.01(17) 2_656 . ? O4 Co3 C8 31.54(16) . . ? N3 Co3 C8 100.64(19) 2_656 . ? N3 Co3 C8 123.75(18) . . ? O3 Co3 C8 30.85(15) . . ? O3 Co3 C8 110.90(16) 2_656 . ? O4 Co3 C8 31.54(16) 2_656 2_656 ? O4 Co3 C8 122.01(16) . 2_656 ? N3 Co3 C8 123.75(18) 2_656 2_656 ? N3 Co3 C8 100.64(19) . 2_656 ? O3 Co3 C8 110.90(16) . 2_656 ? O3 Co3 C8 30.85(15) 2_656 2_656 ? C8 Co3 C8 123.0(2) . 2_656 ? C7 O1 Co1 128.9(4) . . ? C7 O2 Co2 139.3(4) . . ? C8 O3 Co3 88.0(3) . . ? C8 O4 Co3 89.9(3) . . ? C19 O5 Co2 131.3(3) . . ? C19 O5 Co1 90.9(3) . . ? Co2 O5 Co1 108.12(13) . . ? C19 O6 Co1 89.5(2) . . ? C20 O7 Co1 119.7(3) . 1_565 ? C20 O8 Co2 149.9(4) . 1_565 ? C25 N1 C36 118.5(5) . . ? C25 N1 Co1 128.3(4) . . ? C36 N1 Co1 113.2(4) . . ? C34 N2 C35 117.7(6) . . ? C34 N2 Co1 127.1(5) . . ? C35 N2 Co1 115.1(3) . . ? C37 N3 C42 119.1(5) . . ? C37 N3 Co3 127.6(3) . . ? C42 N3 Co3 113.2(4) . . ? C2 C1 C6 120.1(5) . . ? C2 C1 C7 118.4(5) . . ? C6 C1 C7 121.4(5) . . ? C1 C2 C3 119.5(5) . . ? C1 C2 H2A 120.3 . . ? C3 C2 H2A 120.3 . . ? C4 C3 C2 119.3(5) . . ? C4 C3 C8 121.8(5) . . ? C2 C3 C8 118.9(5) . . ? C5 C4 C3 122.8(5) . . ? C5 C4 H4A 118.6 . . ? C3 C4 H4A 118.6 . . ? C4 C5 C6 117.1(5) . . ? C4 C5 C9 121.0(5) . . ? C6 C5 C9 121.9(5) . . ? C1 C6 C5 121.0(5) . . ? C1 C6 H6A 119.5 . . ? C5 C6 H6A 119.5 . . ? O2 C7 O1 126.6(6) . . ? O2 C7 C1 115.5(6) . . ? O1 C7 C1 117.9(5) . . ? O3 C8 O4 119.4(5) . . ? O3 C8 C3 120.7(5) . . ? O4 C8 C3 119.9(5) . . ? O3 C8 Co3 61.1(3) . . ? O4 C8 Co3 58.6(3) . . ? C3 C8 Co3 174.0(4) . . ? C11 C9 C10 108.2(6) . . ? C11 C9 C12 110.3(7) . . ? C10 C9 C12 106.8(6) . . ? C11 C9 C5 113.6(5) . . ? C10 C9 C5 109.4(5) . . ? C12 C9 C5 108.3(5) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 120.1(4) . . ? C18 C13 C19 120.1(4) . . ? C14 C13 C19 119.8(4) . . ? C13 C14 C15 119.4(5) . . ? C13 C14 H14A 120.3 . . ? C15 C14 H14A 120.3 . . ? C14 C15 C16 119.5(4) . . ? C14 C15 C20 123.2(4) . . ? C16 C15 C20 117.3(4) . . ? C17 C16 C15 122.4(4) . . ? C17 C16 H16A 118.8 . . ? C15 C16 H16A 118.8 . . ? C16 C17 C18 116.5(4) . . ? C16 C17 C21 122.6(4) . . ? C18 C17 C21 120.9(4) . . ? C13 C18 C17 121.8(4) . . ? C13 C18 H18A 119.1 . . ? C17 C18 H18A 119.1 . . ? O6 C19 O5 119.8(4) . . ? O6 C19 C13 120.8(4) . . ? O5 C19 C13 119.2(4) . . ? O8 C20 O7 126.1(4) . . ? O8 C20 C15 114.5(5) . . ? O7 C20 C15 119.3(5) . . ? C17 C21 C24 108.9(4) . . ? C17 C21 C22 110.7(5) . . ? C24 C21 C22 109.3(4) . . ? C17 C21 C23 112.0(4) . . ? C24 C21 C23 107.5(5) . . ? C22 C21 C23 108.4(4) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N1 C25 C26 123.8(6) . . ? N1 C25 H25A 118.1 . . ? C26 C25 H25A 118.1 . . ? C27 C26 C25 118.1(6) . . ? C27 C26 H26A 121.0 . . ? C25 C26 H26A 121.0 . . ? C26 C27 C28 119.8(7) . . ? C26 C27 H27A 120.1 . . ? C28 C27 H27A 120.1 . . ? C36 C28 C27 118.1(7) . . ? C36 C28 C29 118.6(8) . . ? C27 C28 C29 123.3(8) . . ? C30 C29 C28 121.9(9) . . ? C30 C29 H29A 119.0 . . ? C28 C29 H29A 119.0 . . ? C29 C30 C31 121.6(9) . . ? C29 C30 H30A 119.2 . . ? C31 C30 H30A 119.2 . . ? C32 C31 C35 114.6(9) . . ? C32 C31 C30 126.3(8) . . ? C35 C31 C30 119.1(7) . . ? C33 C32 C31 121.2(8) . . ? C33 C32 H32A 119.4 . . ? C31 C32 H32A 119.4 . . ? C32 C33 C34 120.5(7) . . ? C32 C33 H33A 119.7 . . ? C34 C33 H33A 119.7 . . ? N2 C34 C33 120.4(8) . . ? N2 C34 H34A 119.8 . . ? C33 C34 H34A 119.8 . . ? N2 C35 C31 125.4(6) . . ? N2 C35 C36 116.2(5) . . ? C31 C35 C36 118.3(7) . . ? N1 C36 C28 121.6(6) . . ? N1 C36 C35 118.0(6) . . ? C28 C36 C35 120.3(6) . . ? N3 C37 C38 123.0(6) . . ? N3 C37 H37A 118.5 . . ? C38 C37 H37A 118.5 . . ? C39 C38 C37 118.2(7) . . ? C39 C38 H38A 120.9 . . ? C37 C38 H38A 120.9 . . ? C38 C39 C40 120.3(6) . . ? C38 C39 H39A 119.8 . . ? C40 C39 H39A 119.8 . . ? C42 C40 C39 117.0(6) . . ? C42 C40 C41 118.2(7) . . ? C39 C40 C41 124.8(6) . . ? C41 C41 C40 121.8(4) 2_656 . ? C41 C41 H41A 119.1 2_656 . ? C40 C41 H41A 119.1 . . ? N3 C42 C42 117.6(3) . 2_656 ? N3 C42 C40 122.4(6) . . ? C42 C42 C40 120.0(4) 2_656 . ? H1WD O1W H1WA 92.1 . . ? H2WA O2W H2WB 98.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O7 Co1 O1 C7 82.8(4) 1_545 . . . ? N2 Co1 O1 C7 176.5(4) . . . . ? N1 Co1 O1 C7 -160.8(5) . . . . ? O5 Co1 O1 C7 -22.3(4) . . . . ? O6 Co1 O1 C7 -81.8(4) . . . . ? O8 Co2 O2 C7 -45.1(5) 1_545 . . . ? O8 Co2 O2 C7 134.9(5) 7_566 . . . ? O5 Co2 O2 C7 42.0(5) . . . . ? O5 Co2 O2 C7 -138.0(5) 7_556 . . . ? O4 Co3 O3 C8 148.8(3) 2_656 . . . ? O4 Co3 O3 C8 3.8(3) . . . . ? N3 Co3 O3 C8 -114.4(3) 2_656 . . . ? N3 Co3 O3 C8 -50.4(4) . . . . ? O3 Co3 O3 C8 86.7(3) 2_656 . . . ? C8 Co3 O3 C8 119.9(3) 2_656 . . . ? O4 Co3 O4 C8 -67.4(3) 2_656 . . . ? N3 Co3 O4 C8 70.5(3) 2_656 . . . ? N3 Co3 O4 C8 150.6(3) . . . . ? O3 Co3 O4 C8 -3.7(3) . . . . ? O3 Co3 O4 C8 -120.4(3) 2_656 . . . ? C8 Co3 O4 C8 -102.2(4) 2_656 . . . ? O8 Co2 O5 C19 151.4(4) 1_545 . . . ? O8 Co2 O5 C19 -28.6(4) 7_566 . . . ? O2 Co2 O5 C19 -122.3(4) 7_556 . . . ? O2 Co2 O5 C19 57.7(4) . . . . ? O8 Co2 O5 Co1 43.38(15) 1_545 . . . ? O8 Co2 O5 Co1 -136.62(15) 7_566 . . . ? O2 Co2 O5 Co1 129.60(15) 7_556 . . . ? O2 Co2 O5 Co1 -50.40(15) . . . . ? O1 Co1 O5 C19 -85.2(3) . . . . ? O7 Co1 O5 C19 173.3(3) 1_545 . . . ? N2 Co1 O5 C19 34.3(5) . . . . ? N1 Co1 O5 C19 86.7(3) . . . . ? O6 Co1 O5 C19 0.8(3) . . . . ? O1 Co1 O5 Co2 49.18(15) . . . . ? O7 Co1 O5 Co2 -52.35(17) 1_545 . . . ? N2 Co1 O5 Co2 168.6(3) . . . . ? N1 Co1 O5 Co2 -138.94(15) . . . . ? O6 Co1 O5 Co2 135.2(2) . . . . ? O1 Co1 O6 C19 99.5(3) . . . . ? O7 Co1 O6 C19 -24.5(7) 1_545 . . . ? N2 Co1 O6 C19 -168.8(3) . . . . ? N1 Co1 O6 C19 -92.6(3) . . . . ? O5 Co1 O6 C19 -0.8(3) . . . . ? O1 Co1 N1 C25 163.9(5) . . . . ? O7 Co1 N1 C25 -78.5(4) 1_545 . . . ? N2 Co1 N1 C25 -172.8(4) . . . . ? O5 Co1 N1 C25 24.8(4) . . . . ? O6 Co1 N1 C25 84.4(4) . . . . ? O1 Co1 N1 C36 -18.6(8) . . . . ? O7 Co1 N1 C36 99.0(3) 1_545 . . . ? N2 Co1 N1 C36 4.7(3) . . . . ? O5 Co1 N1 C36 -157.7(3) . . . . ? O6 Co1 N1 C36 -98.1(3) . . . . ? O1 Co1 N2 C34 -11.3(4) . . . . ? O7 Co1 N2 C34 87.6(4) 1_545 . . . ? N1 Co1 N2 C34 173.5(4) . . . . ? O5 Co1 N2 C34 -132.2(5) . . . . ? O6 Co1 N2 C34 -103.1(4) . . . . ? O1 Co1 N2 C35 170.9(3) . . . . ? O7 Co1 N2 C35 -90.1(3) 1_545 . . . ? N1 Co1 N2 C35 -4.3(3) . . . . ? O5 Co1 N2 C35 50.1(6) . . . . ? O6 Co1 N2 C35 79.2(3) . . . . ? O4 Co3 N3 C37 -88.5(5) 2_656 . . . ? O4 Co3 N3 C37 66.1(5) . . . . ? N3 Co3 N3 C37 179.0(6) 2_656 . . . ? O3 Co3 N3 C37 112.4(5) . . . . ? O3 Co3 N3 C37 -30.0(5) 2_656 . . . ? C8 Co3 N3 C37 84.0(5) . . . . ? C8 Co3 N3 C37 -58.4(5) 2_656 . . . ? O4 Co3 N3 C42 93.6(4) 2_656 . . . ? O4 Co3 N3 C42 -111.8(4) . . . . ? N3 Co3 N3 C42 1.2(3) 2_656 . . . ? O3 Co3 N3 C42 -65.4(5) . . . . ? O3 Co3 N3 C42 152.1(4) 2_656 . . . ? C8 Co3 N3 C42 -93.8(4) . . . . ? C8 Co3 N3 C42 123.7(4) 2_656 . . . ? 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 O1W H1WA O7 0.84 1.76 2.601(16) 174.6 . O2W H2WA O6 0.84 1.97 2.72(3) 148.1 . O2W H2WB O1W 0.85 1.89 2.74(3) 177.3 . _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 0.766 _refine_diff_density_min -1.023 _refine_diff_density_rms 0.123 #============================================================================== data_NiBpy-[Ni(bpy)(tbip)(H2O)]4 _database_code_depnum_ccdc_archive 'CCDC 835413' #TrackingRef '- revised cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C88 H88 N8 Ni4 O20' _chemical_formula_sum 'C88 H88 N8 Ni4 O20' _chemical_formula_weight 1812.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2982(5) _cell_length_b 13.1243(7) _cell_length_c 18.0169(10) _cell_angle_alpha 97.222(1) _cell_angle_beta 97.784(1) _cell_angle_gamma 107.232(1) _cell_volume 2048.41(19) _cell_formula_units_Z 1 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 3801 _cell_measurement_theta_min 2.3324 _cell_measurement_theta_max 28.1038 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 0.984 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6967 _exptl_absorpt_correction_T_max 0.8298 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12779 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0746 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 28.74 _reflns_number_total 9205 _reflns_number_gt 7395 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ISOR 0.01 is applied to three carbon atoms of the disordered tert-butyl. ; _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^)+(0.0583P)^2^+0.6002P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9205 _refine_ls_number_parameters 574 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1568 _refine_ls_wR_factor_gt 0.1460 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.02210(5) 0.24047(3) 0.53286(2) 0.02392(12) Uani 1 1 d . . . Ni2 Ni 0.32745(5) 0.46816(4) 0.11541(3) 0.02809(13) Uani 1 1 d . . . O1 O 0.2035(3) 0.1969(2) 0.49658(14) 0.0322(6) Uani 1 1 d . . . O1W O -0.1266(3) 0.08573(19) 0.49077(15) 0.0324(6) Uani 1 1 d . . . H1WA H -0.1050 0.0620 0.4509 0.049 Uiso 1 1 calc R . . H1WB H -0.0994 0.0571 0.5278 0.049 Uiso 1 1 d R . . O2 O 0.0605(3) 0.2610(2) 0.42062(14) 0.0312(6) Uani 1 1 d . . . O2W O 0.4851(3) 0.4096(2) 0.06815(17) 0.0445(7) Uani 1 1 d . . . H2WA H 0.4718 0.4095 0.0222 0.067 Uiso 1 1 calc R . . H2WB H 0.4712 0.3519 0.0869 0.067 Uiso 1 1 d R . . O3 O 0.2959(3) 0.3598(2) 0.18609(15) 0.0342(6) Uani 1 1 d . . . O4 O 0.4062(5) 0.2479(3) 0.1342(2) 0.0735(13) Uani 1 1 d . . . O5 O 0.5017(3) 0.5852(2) 0.18828(15) 0.0404(7) Uani 1 1 d . . . O6 O 0.4407(3) 0.6255(2) 0.07652(15) 0.0351(6) Uani 1 1 d . . . O7 O 0.9648(3) 0.79729(19) 0.36163(14) 0.0310(6) Uani 1 1 d . . . O8 O 0.9917(3) 0.97337(19) 0.38466(15) 0.0355(6) Uani 1 1 d . . . N1 N 0.1525(3) 0.3949(2) 0.58602(17) 0.0271(6) Uani 1 1 d . . . N2 N -0.1429(3) 0.3138(2) 0.53874(16) 0.0254(6) Uani 1 1 d . . . N3 N 0.1596(4) 0.5208(2) 0.15536(18) 0.0328(7) Uani 1 1 d . . . N4 N 0.1387(3) 0.3804(2) 0.03481(18) 0.0313(7) Uani 1 1 d . . . C1 C 0.2448(4) 0.1934(3) 0.3689(2) 0.0259(7) Uani 1 1 d . . . C2 C 0.2493(4) 0.2465(3) 0.3073(2) 0.0278(7) Uani 1 1 d . . . H2 H 0.2030 0.3001 0.3044 0.033 Uiso 1 1 calc R . . C3 C 0.3233(4) 0.2192(3) 0.2502(2) 0.0279(7) Uani 1 1 d . . . C4 C 0.3841(4) 0.1358(3) 0.2533(2) 0.0299(8) Uani 1 1 d . . . H4 H 0.4295 0.1158 0.2133 0.036 Uiso 1 1 calc R . . C5 C 0.3795(4) 0.0805(3) 0.3145(2) 0.0295(8) Uani 1 1 d . . . C6 C 0.3121(4) 0.1129(3) 0.3727(2) 0.0292(7) Uani 1 1 d . . . H6 H 0.3118 0.0799 0.4154 0.035 Uiso 1 1 calc R . . C7 C 0.1659(4) 0.2197(3) 0.4322(2) 0.0265(7) Uani 1 1 d . . . C8 C 0.3431(4) 0.2795(3) 0.1846(2) 0.0338(8) Uani 1 1 d . . . C9 C 0.4496(5) -0.0110(3) 0.3153(2) 0.0429(10) Uani 1 1 d . . . C10 C 0.3791(8) -0.0943(4) 0.2421(3) 0.0768(18) Uani 1 1 d . . . H10A H 0.2707 -0.1243 0.2397 0.115 Uiso 1 1 calc R . . H10B H 0.4244 -0.1512 0.2417 0.115 Uiso 1 1 calc R . . H10C H 0.3980 -0.0596 0.1989 0.115 Uiso 1 1 calc R . . C11 C 0.6206(6) 0.0360(5) 0.3195(3) 0.0696(16) Uani 1 1 d . . . H11A H 0.6401 0.0721 0.2770 0.104 Uiso 1 1 calc R . . H11B H 0.6654 -0.0213 0.3181 0.104 Uiso 1 1 calc R . . H11C H 0.6649 0.0869 0.3661 0.104 Uiso 1 1 calc R . . C12 C 0.4226(8) -0.0678(5) 0.3831(3) 0.082(2) Uani 1 1 d . . . H12A H 0.3145 -0.0991 0.3811 0.123 Uiso 1 1 calc R . . H12B H 0.4666 -0.0162 0.4294 0.123 Uiso 1 1 calc R . . H12C H 0.4695 -0.1238 0.3817 0.123 Uiso 1 1 calc R . . C13 C 0.6453(4) 0.7562(3) 0.1682(2) 0.0269(7) Uani 1 1 d . . . C14 C 0.7394(4) 0.7718(3) 0.23771(19) 0.0255(7) Uani 1 1 d . . . H14 H 0.7261 0.7160 0.2658 0.031 Uiso 1 1 calc R . . C15 C 0.8526(4) 0.8691(3) 0.2656(2) 0.0274(7) Uani 1 1 d . . . C16 C 0.8724(4) 0.9514(3) 0.2227(2) 0.0314(8) Uani 1 1 d . . . H16 H 0.9481 1.0175 0.2419 0.038 Uiso 1 1 calc R . . C17 C 0.7816(4) 0.9375(3) 0.1515(2) 0.0308(8) Uani 1 1 d . A . C18 C 0.6677(4) 0.8392(3) 0.1253(2) 0.0307(8) Uani 1 1 d . . . H18 H 0.6048 0.8282 0.0783 0.037 Uiso 1 1 calc R . . C19 C 0.5217(4) 0.6498(3) 0.1421(2) 0.0316(8) Uani 1 1 d . . . C20 C 0.9443(4) 0.8826(3) 0.3435(2) 0.0271(7) Uani 1 1 d . . . C21 C 0.8053(5) 1.0285(4) 0.1045(3) 0.0465(11) Uani 1 1 d . . . C22 C 0.9823(16) 1.0592(12) 0.0951(8) 0.077(4) Uani 0.50 1 d P A 1 H23A H 1.0010 0.9961 0.0708 0.116 Uiso 0.50 1 calc PR A 1 H23B H 1.0469 1.0848 0.1443 0.116 Uiso 0.50 1 calc PR A 1 H23C H 1.0044 1.1149 0.0645 0.116 Uiso 0.50 1 calc PR A 1 C22' C 0.786(2) 0.9741(12) 0.0173(8) 0.080(5) Uani 0.50 1 d P A 2 H22D H 0.6840 0.9240 0.0006 0.120 Uiso 0.50 1 calc PR A 2 H22E H 0.8589 0.9362 0.0128 0.120 Uiso 0.50 1 calc PR A 2 H22F H 0.8025 1.0294 -0.0137 0.120 Uiso 0.50 1 calc PR A 2 C23 C 0.7173(19) 1.0000(14) 0.0300(9) 0.088(5) Uani 0.50 1 d PU A 1 H22A H 0.6153 1.0014 0.0322 0.133 Uiso 0.50 1 calc PR A 1 H22B H 0.7135 0.9285 0.0080 0.133 Uiso 0.50 1 calc PR A 1 H22C H 0.7634 1.0508 -0.0007 0.133 Uiso 0.50 1 calc PR A 1 C23' C 0.9504(16) 1.1091(10) 0.1236(8) 0.073(4) Uani 0.50 1 d PU A 2 H23D H 0.9580 1.1533 0.1716 0.110 Uiso 0.50 1 calc PR A 2 H23E H 0.9627 1.1535 0.0850 0.110 Uiso 0.50 1 calc PR A 2 H23F H 1.0290 1.0753 0.1273 0.110 Uiso 0.50 1 calc PR A 2 C24 C 0.803(2) 1.1338(10) 0.1535(9) 0.093(4) Uani 0.50 1 d PU A 1 H24A H 0.7026 1.1243 0.1646 0.140 Uiso 0.50 1 calc PR A 1 H24B H 0.8307 1.1928 0.1260 0.140 Uiso 0.50 1 calc PR A 1 H24C H 0.8755 1.1497 0.2002 0.140 Uiso 0.50 1 calc PR A 1 C24' C 0.6695(15) 1.0741(11) 0.1038(8) 0.081(4) Uani 0.50 1 d P A 2 H24D H 0.5748 1.0155 0.0885 0.121 Uiso 0.50 1 calc PR A 2 H24E H 0.6760 1.1237 0.0686 0.121 Uiso 0.50 1 calc PR A 2 H24F H 0.6736 1.1112 0.1538 0.121 Uiso 0.50 1 calc PR A 2 C25 C 0.3005(4) 0.4256(3) 0.6169(2) 0.0364(9) Uani 1 1 d . . . H34A H 0.3532 0.3758 0.6111 0.044 Uiso 1 1 calc R . . C26 C 0.3777(5) 0.5273(4) 0.6567(3) 0.0478(11) Uani 1 1 d . . . H33A H 0.4805 0.5460 0.6787 0.057 Uiso 1 1 calc R . . C27 C 0.2999(5) 0.6017(4) 0.6636(3) 0.0550(12) Uani 1 1 d . . . H32A H 0.3505 0.6722 0.6890 0.066 Uiso 1 1 calc R . . C28 C 0.1479(5) 0.5708(3) 0.6327(3) 0.0429(10) Uani 1 1 d . . . H31A H 0.0941 0.6202 0.6365 0.051 Uiso 1 1 calc R . . C29 C 0.0746(4) 0.4654(3) 0.5956(2) 0.0292(7) Uani 1 1 d . . . C30 C -0.0913(4) 0.4205(3) 0.5674(2) 0.0270(7) Uani 1 1 d . . . C31 C -0.1898(5) 0.4810(3) 0.5718(2) 0.0385(9) Uani 1 1 d . . . H28A H -0.1525 0.5550 0.5907 0.046 Uiso 1 1 calc R . . C32 C -0.3437(5) 0.4293(4) 0.5475(3) 0.0485(11) Uani 1 1 d . . . H27A H -0.4122 0.4683 0.5503 0.058 Uiso 1 1 calc R . . C33 C -0.3968(5) 0.3211(4) 0.5193(3) 0.0471(11) Uani 1 1 d . . . H26A H -0.5012 0.2852 0.5036 0.057 Uiso 1 1 calc R . . C34 C -0.2925(4) 0.2661(3) 0.5146(2) 0.0354(8) Uani 1 1 d . . . H25A H -0.3279 0.1928 0.4937 0.042 Uiso 1 1 calc R . . C35 C 0.1811(6) 0.5937(3) 0.2177(2) 0.0455(10) Uani 1 1 d . . . H35A H 0.2802 0.6289 0.2442 0.055 Uiso 1 1 calc R . . C36 C 0.0611(7) 0.6189(4) 0.2442(3) 0.0600(15) Uani 1 1 d . . . H36A H 0.0788 0.6711 0.2873 0.072 Uiso 1 1 calc R . . C37 C -0.0840(7) 0.5655(5) 0.2056(3) 0.0662(16) Uani 1 1 d . . . H37A H -0.1669 0.5802 0.2228 0.079 Uiso 1 1 calc R . . C38 C -0.1073(6) 0.4904(4) 0.1418(3) 0.0536(12) Uani 1 1 d . . . H38A H -0.2059 0.4533 0.1152 0.064 Uiso 1 1 calc R . . C39 C 0.0183(4) 0.4704(3) 0.1173(2) 0.0338(8) Uani 1 1 d . . . C40 C 0.0054(4) 0.3924(3) 0.0483(2) 0.0328(8) Uani 1 1 d . . . C41 C -0.1300(5) 0.3351(4) -0.0005(3) 0.0470(11) Uani 1 1 d . . . H41A H -0.2215 0.3442 0.0093 0.056 Uiso 1 1 calc R . . C42 C -0.1301(6) 0.2650(4) -0.0632(3) 0.0553(13) Uani 1 1 d . . . H42A H -0.2212 0.2267 -0.0965 0.066 Uiso 1 1 calc R . . C43 C 0.0046(6) 0.2516(4) -0.0766(3) 0.0522(12) Uani 1 1 d . . . H43A H 0.0075 0.2036 -0.1186 0.063 Uiso 1 1 calc R . . C44 C 0.1359(5) 0.3113(3) -0.0260(2) 0.0433(10) Uani 1 1 d . . . H44A H 0.2281 0.3026 -0.0349 0.052 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0248(2) 0.0262(2) 0.0225(2) 0.00313(17) 0.00471(17) 0.01108(17) Ni2 0.0275(2) 0.0324(3) 0.0239(2) 0.00833(19) 0.00438(18) 0.00755(19) O1 0.0342(14) 0.0424(14) 0.0273(14) 0.0080(11) 0.0098(11) 0.0206(12) O1W 0.0359(14) 0.0300(13) 0.0303(14) 0.0014(11) 0.0018(11) 0.0122(11) O2 0.0348(14) 0.0352(13) 0.0315(14) 0.0086(11) 0.0116(11) 0.0192(11) O2W 0.0457(17) 0.0592(18) 0.0406(18) 0.0213(14) 0.0183(14) 0.0251(14) O3 0.0411(15) 0.0355(14) 0.0361(15) 0.0188(12) 0.0166(12) 0.0179(12) O4 0.136(4) 0.073(2) 0.058(2) 0.040(2) 0.067(3) 0.071(2) O5 0.0406(16) 0.0392(15) 0.0291(15) 0.0126(12) -0.0030(12) -0.0042(12) O6 0.0328(14) 0.0428(15) 0.0276(14) 0.0079(11) 0.0021(11) 0.0099(12) O7 0.0439(15) 0.0304(13) 0.0221(13) 0.0052(10) 0.0039(11) 0.0174(11) O8 0.0449(16) 0.0265(13) 0.0308(15) 0.0001(11) 0.0034(12) 0.0085(11) N1 0.0256(15) 0.0278(14) 0.0282(16) 0.0074(12) 0.0056(12) 0.0075(12) N2 0.0261(15) 0.0271(14) 0.0250(15) 0.0052(12) 0.0063(12) 0.0105(12) N3 0.0406(18) 0.0307(16) 0.0310(18) 0.0090(13) 0.0106(14) 0.0140(14) N4 0.0311(16) 0.0321(16) 0.0294(17) 0.0051(13) 0.0025(13) 0.0096(13) C1 0.0248(17) 0.0279(17) 0.0253(18) 0.0031(13) 0.0068(13) 0.0083(14) C2 0.0306(18) 0.0268(17) 0.0287(19) 0.0077(14) 0.0066(14) 0.0116(14) C3 0.0284(18) 0.0298(17) 0.0273(19) 0.0092(14) 0.0063(14) 0.0093(14) C4 0.0339(19) 0.0314(18) 0.0282(19) 0.0054(14) 0.0107(15) 0.0139(15) C5 0.036(2) 0.0255(17) 0.032(2) 0.0069(14) 0.0105(15) 0.0146(15) C6 0.0319(19) 0.0335(18) 0.0277(19) 0.0111(15) 0.0106(15) 0.0143(15) C7 0.0269(17) 0.0254(16) 0.0276(18) 0.0047(14) 0.0068(14) 0.0083(14) C8 0.038(2) 0.037(2) 0.027(2) 0.0069(15) 0.0070(16) 0.0124(16) C9 0.068(3) 0.049(2) 0.034(2) 0.0159(18) 0.021(2) 0.044(2) C10 0.115(5) 0.051(3) 0.071(4) -0.003(3) 0.010(4) 0.048(3) C11 0.067(4) 0.106(4) 0.064(4) 0.023(3) 0.018(3) 0.063(3) C12 0.144(6) 0.089(4) 0.074(4) 0.055(3) 0.062(4) 0.091(4) C13 0.0244(17) 0.0309(18) 0.0262(18) 0.0047(14) 0.0051(14) 0.0097(14) C14 0.0301(18) 0.0254(16) 0.0241(18) 0.0076(13) 0.0066(14) 0.0117(14) C15 0.0289(18) 0.0291(17) 0.0276(19) 0.0065(14) 0.0071(14) 0.0130(14) C16 0.0308(19) 0.0294(18) 0.035(2) 0.0079(15) 0.0093(16) 0.0090(15) C17 0.035(2) 0.0338(19) 0.031(2) 0.0167(15) 0.0144(16) 0.0147(16) C18 0.0297(19) 0.042(2) 0.0249(19) 0.0112(15) 0.0073(15) 0.0151(16) C19 0.0293(19) 0.040(2) 0.0239(18) 0.0059(15) 0.0030(14) 0.0090(16) C20 0.0270(18) 0.0265(17) 0.0295(19) 0.0050(14) 0.0091(14) 0.0095(14) C21 0.052(3) 0.045(2) 0.048(3) 0.029(2) 0.013(2) 0.014(2) C22 0.083(9) 0.090(10) 0.062(9) 0.044(8) 0.038(7) 0.009(8) C22' 0.134(15) 0.063(8) 0.044(7) 0.028(6) 0.038(9) 0.016(8) C23 0.094(8) 0.083(8) 0.074(8) 0.051(7) -0.011(6) 0.004(6) C23' 0.071(7) 0.063(7) 0.068(7) 0.036(5) -0.003(6) -0.009(5) C24 0.132(9) 0.068(6) 0.099(8) 0.045(6) 0.042(7) 0.039(6) C24' 0.097(9) 0.093(9) 0.104(11) 0.074(9) 0.055(8) 0.070(8) C25 0.031(2) 0.040(2) 0.041(2) 0.0100(17) 0.0094(17) 0.0128(16) C26 0.031(2) 0.047(2) 0.054(3) 0.006(2) -0.0033(19) 0.0025(18) C27 0.047(3) 0.038(2) 0.065(3) -0.005(2) 0.000(2) 0.002(2) C28 0.048(3) 0.0275(19) 0.050(3) -0.0006(17) 0.010(2) 0.0099(17) C29 0.0338(19) 0.0294(17) 0.0266(19) 0.0096(14) 0.0085(15) 0.0103(15) C30 0.0316(18) 0.0271(17) 0.0253(18) 0.0056(14) 0.0106(14) 0.0112(14) C31 0.042(2) 0.036(2) 0.045(2) 0.0095(17) 0.0100(18) 0.0214(18) C32 0.043(2) 0.050(3) 0.066(3) 0.017(2) 0.016(2) 0.030(2) C33 0.027(2) 0.055(3) 0.060(3) 0.012(2) 0.0026(19) 0.0161(19) C34 0.030(2) 0.0345(19) 0.039(2) 0.0038(16) 0.0033(16) 0.0091(15) C35 0.068(3) 0.040(2) 0.033(2) 0.0068(18) 0.013(2) 0.021(2) C36 0.109(5) 0.051(3) 0.044(3) 0.016(2) 0.038(3) 0.046(3) C37 0.086(4) 0.076(4) 0.072(4) 0.031(3) 0.050(3) 0.055(3) C38 0.050(3) 0.059(3) 0.066(3) 0.021(3) 0.024(2) 0.028(2) C39 0.035(2) 0.036(2) 0.038(2) 0.0149(17) 0.0139(17) 0.0167(16) C40 0.032(2) 0.0327(19) 0.038(2) 0.0151(16) 0.0044(16) 0.0135(16) C41 0.036(2) 0.050(3) 0.054(3) 0.024(2) 0.001(2) 0.0089(19) C42 0.055(3) 0.045(3) 0.049(3) 0.011(2) -0.015(2) 0.000(2) C43 0.069(3) 0.045(2) 0.033(2) -0.0011(19) -0.006(2) 0.015(2) C44 0.048(3) 0.045(2) 0.034(2) 0.0013(18) 0.0057(19) 0.0142(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O7 2.021(2) 2_666 ? Ni1 N2 2.046(3) . ? Ni1 N1 2.059(3) . ? Ni1 O1W 2.068(2) . ? Ni1 O1 2.092(2) . ? Ni1 O2 2.137(2) . ? Ni1 C7 2.429(3) . ? Ni2 O3 2.009(2) . ? Ni2 O5 2.037(3) . ? Ni2 N4 2.051(3) . ? Ni2 N3 2.061(3) . ? Ni2 O2W 2.075(3) . ? Ni2 O6 2.267(3) . ? Ni2 C19 2.470(4) . ? O1 C7 1.263(4) . ? O1W H1WA 0.8200 . ? O1W H1WB 0.8500 . ? O2 C7 1.259(4) . ? O2W H2WA 0.8200 . ? O2W H2WB 0.8500 . ? O3 C8 1.256(4) . ? O4 C8 1.239(4) . ? O5 C19 1.253(4) . ? O6 C19 1.260(4) . ? O7 C20 1.264(4) . ? O7 Ni1 2.021(2) 2_666 ? O8 C20 1.242(4) . ? N1 C25 1.332(5) . ? N1 C29 1.341(4) . ? N2 C34 1.329(5) . ? N2 C30 1.345(4) . ? N3 C39 1.328(5) . ? N3 C35 1.331(5) . ? N4 C44 1.323(5) . ? N4 C40 1.345(5) . ? C1 C2 1.381(5) . ? C1 C6 1.382(5) . ? C1 C7 1.496(4) . ? C2 C3 1.380(5) . ? C2 H2 0.9300 . ? C3 C4 1.377(5) . ? C3 C8 1.506(5) . ? C4 C5 1.394(5) . ? C4 H4 0.9300 . ? C5 C6 1.376(5) . ? C5 C9 1.527(5) . ? C6 H6 0.9300 . ? C9 C11 1.513(7) . ? C9 C12 1.520(6) . ? C9 C10 1.532(7) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.381(5) . ? C13 C18 1.396(5) . ? C13 C19 1.493(5) . ? C14 C15 1.375(5) . ? C14 H14 0.9300 . ? C15 C16 1.389(5) . ? C15 C20 1.500(5) . ? C16 C17 1.395(5) . ? C16 H16 0.9300 . ? C17 C18 1.383(5) . ? C17 C21 1.530(5) . ? C18 H18 0.9300 . ? C21 C23' 1.412(13) . ? C21 C23 1.416(16) . ? C21 C24' 1.548(11) . ? C21 C24 1.550(14) . ? C21 C22' 1.605(14) . ? C21 C22 1.612(13) . ? C22 H23A 0.9600 . ? C22 H23B 0.9600 . ? C22 H23C 0.9600 . ? C22' H22D 0.9600 . ? C22' H22E 0.9600 . ? C22' H22F 0.9600 . ? C23 H22A 0.9600 . ? C23 H22B 0.9600 . ? C23 H22C 0.9600 . ? C23' H23D 0.9600 . ? C23' H23E 0.9600 . ? C23' H23F 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C24' H24D 0.9600 . ? C24' H24E 0.9600 . ? C24' H24F 0.9600 . ? C25 C26 1.365(6) . ? C25 H34A 0.9300 . ? C26 C27 1.380(6) . ? C26 H33A 0.9300 . ? C27 C28 1.365(6) . ? C27 H32A 0.9300 . ? C28 C29 1.382(5) . ? C28 H31A 0.9300 . ? C29 C30 1.470(5) . ? C30 C31 1.382(5) . ? C31 C32 1.372(6) . ? C31 H28A 0.9300 . ? C32 C33 1.362(6) . ? C32 H27A 0.9300 . ? C33 C34 1.375(5) . ? C33 H26A 0.9300 . ? C34 H25A 0.9300 . ? C35 C36 1.381(6) . ? C35 H35A 0.9300 . ? C36 C37 1.363(8) . ? C36 H36A 0.9300 . ? C37 C38 1.364(7) . ? C37 H37A 0.9300 . ? C38 C39 1.386(5) . ? C38 H38A 0.9300 . ? C39 C40 1.474(5) . ? C40 C41 1.377(6) . ? C41 C42 1.363(7) . ? C41 H41A 0.9300 . ? C42 C43 1.364(7) . ? C42 H42A 0.9300 . ? C43 C44 1.375(6) . ? C43 H43A 0.9300 . ? C44 H44A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Ni1 N2 97.67(11) 2_666 . ? O7 Ni1 N1 85.64(11) 2_666 . ? N2 Ni1 N1 78.94(11) . . ? O7 Ni1 O1W 88.99(10) 2_666 . ? N2 Ni1 O1W 96.27(11) . . ? N1 Ni1 O1W 172.24(10) . . ? O7 Ni1 O1 101.10(10) 2_666 . ? N2 Ni1 O1 160.02(11) . . ? N1 Ni1 O1 95.66(11) . . ? O1W Ni1 O1 90.86(10) . . ? O7 Ni1 O2 163.52(10) 2_666 . ? N2 Ni1 O2 98.78(10) . . ? N1 Ni1 O2 96.54(11) . . ? O1W Ni1 O2 90.20(10) . . ? O1 Ni1 O2 62.46(9) . . ? O7 Ni1 C7 132.33(11) 2_666 . ? N2 Ni1 C7 129.86(12) . . ? N1 Ni1 C7 98.68(11) . . ? O1W Ni1 C7 89.07(11) . . ? O1 Ni1 C7 31.33(11) . . ? O2 Ni1 C7 31.19(10) . . ? O3 Ni2 O5 95.75(11) . . ? O3 Ni2 N4 95.10(12) . . ? O5 Ni2 N4 166.70(12) . . ? O3 Ni2 N3 88.47(11) . . ? O5 Ni2 N3 93.78(13) . . ? N4 Ni2 N3 78.83(13) . . ? O3 Ni2 O2W 92.58(11) . . ? O5 Ni2 O2W 90.05(12) . . ? N4 Ni2 O2W 97.13(12) . . ? N3 Ni2 O2W 175.91(13) . . ? O3 Ni2 O6 156.56(11) . . ? O5 Ni2 O6 60.87(10) . . ? N4 Ni2 O6 108.29(11) . . ? N3 Ni2 O6 94.39(11) . . ? O2W Ni2 O6 86.22(10) . . ? O3 Ni2 C19 126.13(12) . . ? O5 Ni2 C19 30.40(11) . . ? N4 Ni2 C19 138.32(12) . . ? N3 Ni2 C19 94.78(12) . . ? O2W Ni2 C19 87.80(12) . . ? O6 Ni2 C19 30.47(10) . . ? C7 O1 Ni1 89.2(2) . . ? Ni1 O1W H1WA 109.5 . . ? Ni1 O1W H1WB 96.2 . . ? H1WA O1W H1WB 112.5 . . ? C7 O2 Ni1 87.3(2) . . ? Ni2 O2W H2WA 109.5 . . ? Ni2 O2W H2WB 98.9 . . ? H2WA O2W H2WB 122.8 . . ? C8 O3 Ni2 127.0(2) . . ? C19 O5 Ni2 94.3(2) . . ? C19 O6 Ni2 83.7(2) . . ? C20 O7 Ni1 126.0(2) . 2_666 ? C25 N1 C29 119.1(3) . . ? C25 N1 Ni1 125.3(3) . . ? C29 N1 Ni1 115.2(2) . . ? C34 N2 C30 118.7(3) . . ? C34 N2 Ni1 125.7(2) . . ? C30 N2 Ni1 115.5(2) . . ? C39 N3 C35 119.1(4) . . ? C39 N3 Ni2 115.2(3) . . ? C35 N3 Ni2 125.5(3) . . ? C44 N4 C40 118.3(4) . . ? C44 N4 Ni2 126.4(3) . . ? C40 N4 Ni2 115.3(3) . . ? C2 C1 C6 120.3(3) . . ? C2 C1 C7 121.4(3) . . ? C6 C1 C7 118.3(3) . . ? C3 C2 C1 119.2(3) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C4 C3 C2 119.8(3) . . ? C4 C3 C8 118.1(3) . . ? C2 C3 C8 122.0(3) . . ? C3 C4 C5 121.8(3) . . ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 . . ? C6 C5 C4 117.4(3) . . ? C6 C5 C9 123.0(3) . . ? C4 C5 C9 119.7(3) . . ? C5 C6 C1 121.4(3) . . ? C5 C6 H6 119.3 . . ? C1 C6 H6 119.3 . . ? O2 C7 O1 120.7(3) . . ? O2 C7 C1 120.2(3) . . ? O1 C7 C1 119.0(3) . . ? O2 C7 Ni1 61.50(17) . . ? O1 C7 Ni1 59.45(17) . . ? C1 C7 Ni1 173.5(2) . . ? O4 C8 O3 125.0(3) . . ? O4 C8 C3 118.3(3) . . ? O3 C8 C3 116.7(3) . . ? C11 C9 C12 108.2(4) . . ? C11 C9 C5 108.8(4) . . ? C12 C9 C5 112.3(3) . . ? C11 C9 C10 109.6(4) . . ? C12 C9 C10 108.8(4) . . ? C5 C9 C10 109.1(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 119.6(3) . . ? C14 C13 C19 117.9(3) . . ? C18 C13 C19 122.4(3) . . ? C15 C14 C13 120.6(3) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 119.2(3) . . ? C14 C15 C20 117.6(3) . . ? C16 C15 C20 123.1(3) . . ? C15 C16 C17 121.8(3) . . ? C15 C16 H16 119.1 . . ? C17 C16 H16 119.1 . . ? C18 C17 C16 117.7(3) . . ? C18 C17 C21 121.0(4) . . ? C16 C17 C21 121.3(3) . . ? C17 C18 C13 121.1(3) . . ? C17 C18 H18 119.4 . . ? C13 C18 H18 119.4 . . ? O5 C19 O6 121.2(3) . . ? O5 C19 C13 117.1(3) . . ? O6 C19 C13 121.7(3) . . ? O5 C19 Ni2 55.34(18) . . ? O6 C19 Ni2 65.8(2) . . ? C13 C19 Ni2 172.5(3) . . ? O8 C20 O7 125.5(4) . . ? O8 C20 C15 119.1(3) . . ? O7 C20 C15 115.4(3) . . ? C23' C21 C23 122.6(9) . . ? C23' C21 C17 115.4(6) . . ? C23 C21 C17 115.5(7) . . ? C23' C21 C24' 113.8(9) . . ? C23 C21 C24' 71.3(9) . . ? C17 C21 C24' 109.1(5) . . ? C23' C21 C24 66.9(8) . . ? C23 C21 C24 116.6(9) . . ? C17 C21 C24 109.7(6) . . ? C24' C21 C24 53.0(7) . . ? C23' C21 C22' 107.1(9) . . ? C17 C21 C22' 107.4(6) . . ? C24' C21 C22' 103.1(9) . . ? C24 C21 C22' 140.9(8) . . ? C23 C21 C22 106.5(9) . . ? C17 C21 C22 105.1(6) . . ? C24' C21 C22 142.8(7) . . ? C24 C21 C22 101.7(8) . . ? C22' C21 C22 79.8(8) . . ? C21 C22 H23A 109.5 . . ? C21 C22 H23B 109.5 . . ? C21 C22 H23C 109.5 . . ? C21 C22' H22D 109.5 . . ? C21 C22' H22E 109.5 . . ? H22D C22' H22E 109.5 . . ? C21 C22' H22F 109.5 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? C21 C23 H22A 109.5 . . ? C21 C23 H22B 109.5 . . ? C21 C23 H22C 109.5 . . ? C21 C23' H23D 109.5 . . ? C21 C23' H23E 109.5 . . ? H23D C23' H23E 109.5 . . ? C21 C23' H23F 109.5 . . ? H23D C23' H23F 109.5 . . ? H23E C23' H23F 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? C21 C24' H24D 109.5 . . ? C21 C24' H24E 109.5 . . ? H24D C24' H24E 109.5 . . ? C21 C24' H24F 109.5 . . ? H24D C24' H24F 109.5 . . ? H24E C24' H24F 109.5 . . ? N1 C25 C26 122.5(4) . . ? N1 C25 H34A 118.7 . . ? C26 C25 H34A 118.7 . . ? C25 C26 C27 118.5(4) . . ? C25 C26 H33A 120.7 . . ? C27 C26 H33A 120.7 . . ? C28 C27 C26 119.4(4) . . ? C28 C27 H32A 120.3 . . ? C26 C27 H32A 120.3 . . ? C27 C28 C29 119.3(4) . . ? C27 C28 H31A 120.3 . . ? C29 C28 H31A 120.3 . . ? N1 C29 C28 121.0(4) . . ? N1 C29 C30 115.2(3) . . ? C28 C29 C30 123.8(3) . . ? N2 C30 C31 121.6(3) . . ? N2 C30 C29 115.0(3) . . ? C31 C30 C29 123.4(3) . . ? C32 C31 C30 118.4(4) . . ? C32 C31 H28A 120.8 . . ? C30 C31 H28A 120.8 . . ? C33 C32 C31 120.3(4) . . ? C33 C32 H27A 119.9 . . ? C31 C32 H27A 119.9 . . ? C32 C33 C34 118.4(4) . . ? C32 C33 H26A 120.8 . . ? C34 C33 H26A 120.8 . . ? N2 C34 C33 122.6(4) . . ? N2 C34 H25A 118.7 . . ? C33 C34 H25A 118.7 . . ? N3 C35 C36 122.2(5) . . ? N3 C35 H35A 118.9 . . ? C36 C35 H35A 118.9 . . ? C37 C36 C35 118.4(5) . . ? C37 C36 H36A 120.8 . . ? C35 C36 H36A 120.8 . . ? C36 C37 C38 119.9(5) . . ? C36 C37 H37A 120.1 . . ? C38 C37 H37A 120.1 . . ? C37 C38 C39 118.9(5) . . ? C37 C38 H38A 120.5 . . ? C39 C38 H38A 120.5 . . ? N3 C39 C38 121.5(4) . . ? N3 C39 C40 115.5(3) . . ? C38 C39 C40 123.1(4) . . ? N4 C40 C41 120.7(4) . . ? N4 C40 C39 114.9(3) . . ? C41 C40 C39 124.5(4) . . ? C42 C41 C40 120.1(4) . . ? C42 C41 H41A 119.9 . . ? C40 C41 H41A 119.9 . . ? C41 C42 C43 119.5(4) . . ? C41 C42 H42A 120.3 . . ? C43 C42 H42A 120.3 . . ? C42 C43 C44 117.7(4) . . ? C42 C43 H43A 121.1 . . ? C44 C43 H43A 121.1 . . ? N4 C44 C43 123.8(4) . . ? N4 C44 H44A 118.1 . . ? C43 C44 H44A 118.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O7 Ni1 O1 C7 175.9(2) 2_666 . . . ? N2 Ni1 O1 C7 -24.4(4) . . . . ? N1 Ni1 O1 C7 -97.4(2) . . . . ? O1W Ni1 O1 C7 86.8(2) . . . . ? O2 Ni1 O1 C7 -3.0(2) . . . . ? O7 Ni1 O2 C7 -0.8(5) 2_666 . . . ? N2 Ni1 O2 C7 175.7(2) . . . . ? N1 Ni1 O2 C7 96.0(2) . . . . ? O1W Ni1 O2 C7 -87.9(2) . . . . ? O1 Ni1 O2 C7 3.0(2) . . . . ? O5 Ni2 O3 C8 -100.7(3) . . . . ? N4 Ni2 O3 C8 87.0(3) . . . . ? N3 Ni2 O3 C8 165.7(3) . . . . ? O2W Ni2 O3 C8 -10.4(3) . . . . ? O6 Ni2 O3 C8 -96.8(4) . . . . ? C19 Ni2 O3 C8 -99.5(3) . . . . ? O3 Ni2 O5 C19 178.2(2) . . . . ? N4 Ni2 O5 C19 -37.3(6) . . . . ? N3 Ni2 O5 C19 -93.0(2) . . . . ? O2W Ni2 O5 C19 85.6(2) . . . . ? O6 Ni2 O5 C19 -0.1(2) . . . . ? O3 Ni2 O6 C19 -4.3(4) . . . . ? O5 Ni2 O6 C19 0.1(2) . . . . ? N4 Ni2 O6 C19 171.6(2) . . . . ? N3 Ni2 O6 C19 92.0(2) . . . . ? O2W Ni2 O6 C19 -92.1(2) . . . . ? O7 Ni1 N1 C25 72.2(3) 2_666 . . . ? N2 Ni1 N1 C25 170.9(3) . . . . ? 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 O2W H2WB O4 0.85 1.70 2.532(4) 164.4 . O1W H1WA O8 0.82 2.04 2.804(4) 155.5 1_445 O1W H1WB O8 0.85 1.90 2.732(4) 164.7 2_666 O2W H2WA O6 0.82 2.11 2.803(4) 142.4 2_665 _diffrn_measured_fraction_theta_max 0.865 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.617 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.085 #============================================================================== data_NiPhen-[Ni(tbip)(phen)(H2O)]n _database_code_depnum_ccdc_archive 'CCDC 835414' #TrackingRef '- revised cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H22 N2 Ni O5' _chemical_formula_sum 'C24 H22 N2 Ni O5' _chemical_formula_weight 477.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' 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 15.1908(11) _cell_length_b 10.2298(8) _cell_length_c 15.6092(12) _cell_angle_alpha 90.00 _cell_angle_beta 109.9490(10) _cell_angle_gamma 90.00 _cell_volume 2280.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2913 _cell_measurement_theta_min 2.4271 _cell_measurement_theta_max 23.7548 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 0.888 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8494 _exptl_absorpt_correction_T_max 0.9009 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22632 _diffrn_reflns_av_R_equivalents 0.0809 _diffrn_reflns_av_sigmaI/netI 0.1103 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 28.51 _reflns_number_total 5457 _reflns_number_gt 3944 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0271P)^2^+4.4833P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5457 _refine_ls_number_parameters 294 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0970 _refine_ls_R_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.1583 _refine_ls_wR_factor_gt 0.1428 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 Ni1 Ni 0.34314(3) 0.42083(4) 0.51073(3) 0.01748(15) Uani 1 1 d . . . O1W O 0.46748(17) 0.4080(3) 0.61634(16) 0.0230(6) Uani 1 1 d . . . H1 H 0.4718 0.4701 0.6527 0.055(16) Uiso 1 1 calc R . . H2 H 0.5176 0.4065 0.6052 0.024(11) Uiso 1 1 d R . . O1 O 0.37447(16) 0.5677(2) 0.42762(16) 0.0206(5) Uani 1 1 d . . . O2 O 0.23486(16) 0.4814(2) 0.39192(16) 0.0208(5) Uani 1 1 d . . . O3 O 0.29331(17) 0.9483(3) 0.07997(17) 0.0243(6) Uani 1 1 d . . . O4 O 0.42150(17) 0.8867(3) 0.19414(17) 0.0250(6) Uani 1 1 d . . . N1 N 0.3805(2) 0.2668(3) 0.4437(2) 0.0216(6) Uani 1 1 d . . . N2 N 0.2865(2) 0.2671(3) 0.5599(2) 0.0226(7) Uani 1 1 d . . . C1 C 0.2518(2) 0.6575(3) 0.2996(2) 0.0191(7) Uani 1 1 d . . . C2 C 0.3109(2) 0.7268(3) 0.2649(2) 0.0192(7) Uani 1 1 d . . . H2A H 0.3768 0.7165 0.2910 0.023 Uiso 1 1 calc R . . C3 C 0.2731(2) 0.8109(3) 0.1922(2) 0.0201(7) Uani 1 1 d . . . C4 C 0.1762(2) 0.8263(4) 0.1557(2) 0.0208(7) Uani 1 1 d . . . H4A H 0.1505 0.8834 0.1053 0.025 Uiso 1 1 calc R . . C5 C 0.1163(2) 0.7606(4) 0.1908(2) 0.0235(8) Uani 1 1 d . . . C6 C 0.1554(2) 0.6743(4) 0.2624(2) 0.0209(8) Uani 1 1 d . . . H6A H 0.1156 0.6260 0.2863 0.025 Uiso 1 1 calc R . . C7 C 0.2887(2) 0.5632(3) 0.3771(2) 0.0183(7) Uani 1 1 d . . . C8 C 0.3354(2) 0.8870(3) 0.1530(2) 0.0180(7) Uani 1 1 d . . . C9 C 0.0093(3) 0.7783(5) 0.1510(3) 0.0348(10) Uani 1 1 d . . . C10 C -0.0196(3) 0.8915(7) 0.0868(4) 0.076(2) Uani 1 1 d . . . H10A H 0.0101 0.9715 0.1180 0.114 Uiso 1 1 calc R . . H10B H -0.0879 0.9012 0.0664 0.114 Uiso 1 1 calc R . . H10C H -0.0001 0.8759 0.0340 0.114 Uiso 1 1 calc R . . C11 C -0.0303(4) 0.7976(9) 0.2256(4) 0.098(3) Uani 1 1 d . . . H11A H 0.0027 0.8693 0.2652 0.146 Uiso 1 1 calc R . . H11B H -0.0227 0.7172 0.2615 0.146 Uiso 1 1 calc R . . H11C H -0.0971 0.8191 0.1991 0.146 Uiso 1 1 calc R . . C12 C -0.0325(4) 0.6544(7) 0.1002(6) 0.106(3) Uani 1 1 d . . . H12A H -0.1009 0.6621 0.0761 0.159 Uiso 1 1 calc R . . H12B H -0.0148 0.5797 0.1420 0.159 Uiso 1 1 calc R . . H12C H -0.0088 0.6411 0.0498 0.159 Uiso 1 1 calc R . . C13 C 0.4264(3) 0.2683(4) 0.3845(3) 0.0313(9) Uani 1 1 d . . . H13A H 0.4444 0.3503 0.3672 0.038 Uiso 1 1 calc R . . C14 C 0.4491(3) 0.1560(4) 0.3473(3) 0.0356(10) Uani 1 1 d . . . H14A H 0.4815 0.1616 0.3050 0.043 Uiso 1 1 calc R . . C15 C 0.4242(3) 0.0369(4) 0.3719(3) 0.0315(9) Uani 1 1 d . . . H15A H 0.4399 -0.0411 0.3473 0.038 Uiso 1 1 calc R . . C16 C 0.3756(3) 0.0307(4) 0.4335(3) 0.0269(8) Uani 1 1 d . . . C17 C 0.3455(3) -0.0882(4) 0.4622(3) 0.0352(10) Uani 1 1 d . . . H17A H 0.3607 -0.1691 0.4408 0.042 Uiso 1 1 calc R . . C18 C 0.2958(3) -0.0882(4) 0.5190(3) 0.0374(10) Uani 1 1 d . . . H18A H 0.2754 -0.1688 0.5359 0.045 Uiso 1 1 calc R . . C19 C 0.2734(3) 0.0314(4) 0.5542(3) 0.0281(9) Uani 1 1 d . . . C20 C 0.2239(3) 0.0390(5) 0.6149(3) 0.0378(10) Uani 1 1 d . . . H20A H 0.2005 -0.0384 0.6330 0.045 Uiso 1 1 calc R . . C21 C 0.2091(3) 0.1563(5) 0.6481(3) 0.0418(12) Uani 1 1 d . . . H21A H 0.1776 0.1613 0.6912 0.050 Uiso 1 1 calc R . . C22 C 0.2407(3) 0.2695(4) 0.6184(3) 0.0334(10) Uani 1 1 d . . . H22A H 0.2290 0.3515 0.6409 0.040 Uiso 1 1 calc R . . C23 C 0.3037(2) 0.1491(4) 0.5290(2) 0.0228(8) Uani 1 1 d . . . C24 C 0.3546(3) 0.1496(4) 0.4669(2) 0.0222(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0171(2) 0.0176(2) 0.0200(2) 0.00053(19) 0.00921(17) 0.00040(19) O1W 0.0180(12) 0.0270(15) 0.0254(13) -0.0004(12) 0.0092(10) 0.0024(11) O1 0.0170(12) 0.0211(14) 0.0234(12) 0.0029(10) 0.0066(10) -0.0005(10) O2 0.0173(12) 0.0250(14) 0.0200(12) 0.0049(10) 0.0062(10) -0.0018(10) O3 0.0225(13) 0.0262(15) 0.0248(13) 0.0068(11) 0.0089(11) -0.0029(11) O4 0.0194(13) 0.0299(15) 0.0277(14) 0.0077(11) 0.0106(11) 0.0033(11) N1 0.0260(16) 0.0177(16) 0.0247(15) -0.0029(12) 0.0132(13) -0.0028(13) N2 0.0209(15) 0.0262(18) 0.0229(15) 0.0045(13) 0.0104(13) -0.0024(13) C1 0.0206(17) 0.0180(19) 0.0205(17) -0.0009(14) 0.0091(14) -0.0012(14) C2 0.0183(17) 0.0207(19) 0.0200(17) -0.0002(14) 0.0082(14) 0.0021(14) C3 0.0207(18) 0.0178(19) 0.0232(18) 0.0004(14) 0.0094(14) 0.0013(14) C4 0.0201(17) 0.0211(19) 0.0228(18) 0.0042(14) 0.0092(15) 0.0025(15) C5 0.0192(18) 0.026(2) 0.0267(19) -0.0006(16) 0.0092(15) 0.0008(15) C6 0.0183(17) 0.023(2) 0.0250(18) -0.0012(15) 0.0125(15) -0.0021(15) C7 0.0143(15) 0.0199(19) 0.0233(17) -0.0019(14) 0.0100(13) -0.0010(14) C8 0.0183(17) 0.0151(18) 0.0231(18) -0.0014(13) 0.0103(14) 0.0022(13) C9 0.0133(18) 0.048(3) 0.043(2) 0.019(2) 0.0101(17) 0.0056(17) C10 0.027(3) 0.102(5) 0.104(5) 0.064(4) 0.032(3) 0.026(3) C11 0.045(3) 0.188(9) 0.077(4) 0.063(5) 0.044(3) 0.060(4) C12 0.036(3) 0.090(6) 0.146(7) -0.002(5) -0.028(4) -0.008(3) C13 0.036(2) 0.029(2) 0.037(2) -0.0025(18) 0.0236(19) -0.0053(18) C14 0.041(2) 0.034(3) 0.041(2) -0.0079(19) 0.026(2) -0.004(2) C15 0.040(2) 0.026(2) 0.031(2) -0.0103(17) 0.0146(18) 0.0000(18) C16 0.028(2) 0.023(2) 0.026(2) -0.0026(16) 0.0048(16) 0.0007(16) C17 0.048(3) 0.020(2) 0.035(2) -0.0042(18) 0.011(2) -0.0022(19) C18 0.050(3) 0.022(2) 0.037(2) 0.0060(18) 0.010(2) -0.008(2) C19 0.029(2) 0.027(2) 0.027(2) 0.0085(16) 0.0071(16) -0.0055(17) C20 0.041(2) 0.035(3) 0.042(2) 0.016(2) 0.019(2) -0.004(2) C21 0.041(3) 0.054(3) 0.044(3) 0.010(2) 0.032(2) -0.003(2) C22 0.035(2) 0.038(3) 0.034(2) 0.0039(19) 0.0214(19) 0.0010(19) C23 0.0199(18) 0.024(2) 0.0232(18) 0.0048(15) 0.0057(15) -0.0013(15) C24 0.0220(18) 0.019(2) 0.0260(19) 0.0005(15) 0.0082(15) -0.0016(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O3 2.023(2) 4_576 ? Ni1 O1W 2.044(2) . ? Ni1 N2 2.063(3) . ? Ni1 N1 2.074(3) . ? Ni1 O2 2.109(2) . ? Ni1 O1 2.142(2) . ? Ni1 C7 2.445(4) . ? O1W H1 0.8400 . ? O1W H2 0.8368 . ? O1 C7 1.273(4) . ? O2 C7 1.246(4) . ? O3 C8 1.267(4) . ? O3 Ni1 2.023(2) 4_575 ? O4 C8 1.245(4) . ? N1 C13 1.335(4) . ? N1 C24 1.349(5) . ? N2 C22 1.322(5) . ? N2 C23 1.358(5) . ? C1 C6 1.389(5) . ? C1 C2 1.391(5) . ? C1 C7 1.499(5) . ? C2 C3 1.383(5) . ? C2 H2A 0.9500 . ? C3 C4 1.394(5) . ? C3 C8 1.507(5) . ? C4 C5 1.385(5) . ? C4 H4A 0.9500 . ? C5 C6 1.389(5) . ? C5 C9 1.540(5) . ? C6 H6A 0.9500 . ? C9 C11 1.496(7) . ? C9 C10 1.496(6) . ? C9 C12 1.515(8) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.383(6) . ? C13 H13A 0.9500 . ? C14 C15 1.369(6) . ? C14 H14A 0.9500 . ? C15 C16 1.400(5) . ? C15 H15A 0.9500 . ? C16 C24 1.403(5) . ? C16 C17 1.424(6) . ? C17 C18 1.346(6) . ? C17 H17A 0.9500 . ? C18 C19 1.430(6) . ? C18 H18A 0.9500 . ? C19 C23 1.393(5) . ? C19 C20 1.399(6) . ? C20 C21 1.356(7) . ? C20 H20A 0.9500 . ? C21 C22 1.392(6) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C24 1.431(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Ni1 O1W 91.32(10) 4_576 . ? O3 Ni1 N2 91.48(12) 4_576 . ? O1W Ni1 N2 92.23(11) . . ? O3 Ni1 N1 171.35(11) 4_576 . ? O1W Ni1 N1 91.22(11) . . ? N2 Ni1 N1 80.16(12) . . ? O3 Ni1 O2 87.35(10) 4_576 . ? O1W Ni1 O2 163.16(10) . . ? N2 Ni1 O2 104.58(11) . . ? N1 Ni1 O2 92.59(11) . . ? O3 Ni1 O1 93.46(10) 4_576 . ? O1W Ni1 O1 101.45(10) . . ? N2 Ni1 O1 165.33(11) . . ? N1 Ni1 O1 94.14(10) . . ? O2 Ni1 O1 61.92(9) . . ? O3 Ni1 C7 88.99(11) 4_576 . ? O1W Ni1 C7 132.61(11) . . ? N2 Ni1 C7 135.15(12) . . ? N1 Ni1 C7 95.36(12) . . ? O2 Ni1 C7 30.63(10) . . ? O1 Ni1 C7 31.34(10) . . ? Ni1 O1W H1 109.5 . . ? Ni1 O1W H2 119.3 . . ? H1 O1W H2 106.7 . . ? C7 O1 Ni1 87.6(2) . . ? C7 O2 Ni1 89.8(2) . . ? C8 O3 Ni1 130.0(2) . 4_575 ? C13 N1 C24 117.6(3) . . ? C13 N1 Ni1 129.7(3) . . ? C24 N1 Ni1 112.7(2) . . ? C22 N2 C23 118.2(3) . . ? C22 N2 Ni1 128.8(3) . . ? C23 N2 Ni1 112.9(2) . . ? C6 C1 C2 120.1(3) . . ? C6 C1 C7 117.9(3) . . ? C2 C1 C7 122.0(3) . . ? C3 C2 C1 119.6(3) . . ? C3 C2 H2A 120.2 . . ? C1 C2 H2A 120.2 . . ? C2 C3 C4 119.4(3) . . ? C2 C3 C8 120.7(3) . . ? C4 C3 C8 119.9(3) . . ? C5 C4 C3 121.9(3) . . ? C5 C4 H4A 119.1 . . ? C3 C4 H4A 119.1 . . ? C4 C5 C6 117.9(3) . . ? C4 C5 C9 121.9(3) . . ? C6 C5 C9 120.1(3) . . ? C5 C6 C1 121.0(3) . . ? C5 C6 H6A 119.5 . . ? C1 C6 H6A 119.5 . . ? O2 C7 O1 120.5(3) . . ? O2 C7 C1 119.6(3) . . ? O1 C7 C1 119.9(3) . . ? O2 C7 Ni1 59.60(18) . . ? O1 C7 Ni1 61.09(17) . . ? C1 C7 Ni1 175.3(2) . . ? O4 C8 O3 125.8(3) . . ? O4 C8 C3 119.0(3) . . ? O3 C8 C3 115.2(3) . . ? C11 C9 C10 108.3(5) . . ? C11 C9 C12 108.0(6) . . ? C10 C9 C12 108.8(5) . . ? C11 C9 C5 110.6(4) . . ? C10 C9 C5 112.9(4) . . ? C12 C9 C5 108.0(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C14 123.1(4) . . ? N1 C13 H13A 118.4 . . ? C14 C13 H13A 118.4 . . ? C15 C14 C13 119.3(4) . . ? C15 C14 H14A 120.4 . . ? C13 C14 H14A 120.4 . . ? C14 C15 C16 119.6(4) . . ? C14 C15 H15A 120.2 . . ? C16 C15 H15A 120.2 . . ? C15 C16 C24 117.2(4) . . ? C15 C16 C17 123.8(4) . . ? C24 C16 C17 119.1(4) . . ? C18 C17 C16 121.3(4) . . ? C18 C17 H17A 119.4 . . ? C16 C17 H17A 119.4 . . ? C17 C18 C19 121.0(4) . . ? C17 C18 H18A 119.5 . . ? C19 C18 H18A 119.5 . . ? C23 C19 C20 116.7(4) . . ? C23 C19 C18 119.1(4) . . ? C20 C19 C18 124.2(4) . . ? C21 C20 C19 120.4(4) . . ? C21 C20 H20A 119.8 . . ? C19 C20 H20A 119.8 . . ? C20 C21 C22 119.2(4) . . ? C20 C21 H21A 120.4 . . ? C22 C21 H21A 120.4 . . ? N2 C22 C21 122.5(4) . . ? N2 C22 H22A 118.8 . . ? C21 C22 H22A 118.8 . . ? N2 C23 C19 123.0(3) . . ? N2 C23 C24 116.9(3) . . ? C19 C23 C24 120.1(4) . . ? N1 C24 C16 123.2(3) . . ? N1 C24 C23 117.3(3) . . ? C16 C24 C23 119.5(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Ni1 O1 C7 -82.4(2) 4_576 . . . ? O1W Ni1 O1 C7 -174.40(19) . . . . ? N2 Ni1 O1 C7 27.1(5) . . . . ? N1 Ni1 O1 C7 93.5(2) . . . . ? O2 Ni1 O1 C7 2.78(18) . . . . ? O3 Ni1 O2 C7 92.5(2) 4_576 . . . ? O1W Ni1 O2 C7 6.7(4) . . . . ? N2 Ni1 O2 C7 -176.7(2) . . . . ? N1 Ni1 O2 C7 -96.1(2) . . . . ? O1 Ni1 O2 C7 -2.84(19) . . . . ? O1W Ni1 N1 C13 -89.1(3) . . . . ? N2 Ni1 N1 C13 178.8(4) . . . . ? O2 Ni1 N1 C13 74.5(3) . . . . ? O1 Ni1 N1 C13 12.5(3) . . . . ? C7 Ni1 N1 C13 43.9(4) . . . . ? O1W Ni1 N1 C24 89.5(3) . . . . ? N2 Ni1 N1 C24 -2.6(2) . . . . ? O2 Ni1 N1 C24 -106.9(3) . . . . ? O1 Ni1 N1 C24 -169.0(2) . . . . ? C7 Ni1 N1 C24 -137.5(3) . . . . ? O3 Ni1 N2 C22 -2.9(3) 4_576 . . . ? O1W Ni1 N2 C22 88.4(3) . . . . ? N1 Ni1 N2 C22 179.3(4) . . . . ? O2 Ni1 N2 C22 -90.6(3) . . . . ? O1 Ni1 N2 C22 -112.6(5) . . . . ? C7 Ni1 N2 C22 -93.0(4) . . . . ? O3 Ni1 N2 C23 -179.9(2) 4_576 . . . ? O1W Ni1 N2 C23 -88.6(2) . . . . ? N1 Ni1 N2 C23 2.3(2) . . . . ? O2 Ni1 N2 C23 92.4(2) . . . . ? O1 Ni1 N2 C23 70.4(5) . . . . ? C7 Ni1 N2 C23 90.0(3) . . . . ? C6 C1 C2 C3 -1.1(5) . . . . ? C7 C1 C2 C3 178.8(3) . . . . ? C1 C2 C3 C4 1.0(5) . . . . ? C1 C2 C3 C8 -179.9(3) . . . . ? C2 C3 C4 C5 0.7(5) . . . . ? C8 C3 C4 C5 -178.5(3) . . . . ? C3 C4 C5 C6 -2.2(6) . . . . ? C3 C4 C5 C9 179.6(4) . . . . ? C4 C5 C6 C1 2.0(5) . . . . ? C9 C5 C6 C1 -179.7(4) . . . . ? C2 C1 C6 C5 -0.4(5) . . . . ? C7 C1 C6 C5 179.6(3) . . . . ? Ni1 O2 C7 O1 4.9(3) . . . . ? Ni1 O2 C7 C1 -174.6(3) . . . . ? Ni1 O1 C7 O2 -4.8(3) . . . . ? Ni1 O1 C7 C1 174.7(3) . . . . ? C6 C1 C7 O2 16.9(5) . . . . ? C2 C1 C7 O2 -163.0(3) . . . . ? C6 C1 C7 O1 -162.6(3) . . . . ? C2 C1 C7 O1 17.5(5) . . . . ? O3 Ni1 C7 O2 -86.5(2) 4_576 . . . ? O1W Ni1 C7 O2 -177.35(18) . . . . ? N2 Ni1 C7 O2 4.6(3) . . . . ? N1 Ni1 C7 O2 86.0(2) . . . . ? O1 Ni1 C7 O2 175.2(3) . . . . ? O3 Ni1 C7 O1 98.32(19) 4_576 . . . ? O1W Ni1 C7 O1 7.5(3) . . . . ? N2 Ni1 C7 O1 -170.59(18) . . . . ? N1 Ni1 C7 O1 -89.2(2) . . . . ? O2 Ni1 C7 O1 -175.2(3) . . . . ? Ni1 O3 C8 O4 -7.1(5) 4_575 . . . ? Ni1 O3 C8 C3 171.8(2) 4_575 . . . ? C2 C3 C8 O4 -9.3(5) . . . . ? C4 C3 C8 O4 169.9(3) . . . . ? C2 C3 C8 O3 171.7(3) . . . . ? C4 C3 C8 O3 -9.2(5) . . . . ? C4 C5 C9 C11 -133.9(5) . . . . ? C6 C5 C9 C11 47.8(6) . . . . ? C4 C5 C9 C10 -12.4(6) . . . . ? C6 C5 C9 C10 169.4(4) . . . . ? C4 C5 C9 C12 108.0(5) . . . . ? C6 C5 C9 C12 -70.2(6) . . . . ? C24 N1 C13 C14 -0.6(6) . . . . ? Ni1 N1 C13 C14 177.9(3) . . . . ? N1 C13 C14 C15 -0.4(7) . . . . ? C13 C14 C15 C16 0.6(6) . . . . ? C14 C15 C16 C24 0.1(6) . . . . ? C14 C15 C16 C17 179.0(4) . . . . ? C15 C16 C17 C18 -177.4(4) . . . . ? C24 C16 C17 C18 1.4(6) . . . . ? C16 C17 C18 C19 -1.4(7) . . . . ? C17 C18 C19 C23 0.0(6) . . . . ? C17 C18 C19 C20 -178.6(4) . . . . ? C23 C19 C20 C21 -1.5(6) . . . . ? C18 C19 C20 C21 177.1(4) . . . . ? C19 C20 C21 C22 2.4(7) . . . . ? C23 N2 C22 C21 -0.7(6) . . . . ? Ni1 N2 C22 C21 -177.6(3) . . . . ? C20 C21 C22 N2 -1.3(7) . . . . ? C22 N2 C23 C19 1.7(5) . . . . ? Ni1 N2 C23 C19 179.1(3) . . . . ? C22 N2 C23 C24 -179.0(3) . . . . ? Ni1 N2 C23 C24 -1.7(4) . . . . ? C20 C19 C23 N2 -0.6(6) . . . . ? C18 C19 C23 N2 -179.3(4) . . . . ? C20 C19 C23 C24 -179.8(4) . . . . ? C18 C19 C23 C24 1.5(6) . . . . ? C13 N1 C24 C16 1.5(5) . . . . ? Ni1 N1 C24 C16 -177.3(3) . . . . ? C13 N1 C24 C23 -178.7(3) . . . . ? Ni1 N1 C24 C23 2.5(4) . . . . ? C15 C16 C24 N1 -1.2(6) . . . . ? C17 C16 C24 N1 179.9(4) . . . . ? C15 C16 C24 C23 179.0(3) . . . . ? C17 C16 C24 C23 0.1(6) . . . . ? N2 C23 C24 N1 -0.6(5) . . . . ? C19 C23 C24 N1 178.7(3) . . . . ? N2 C23 C24 C16 179.2(3) . . . . ? C19 C23 C24 C16 -1.5(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 O1W H1 O4 0.84 1.87 2.637(4) 151.9 4_576 O1W H2 O1 0.84 1.90 2.724(3) 170.3 3_666 _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.632 _refine_diff_density_min -0.598 _refine_diff_density_rms 0.105 #============================================================================== data_CuBpy1-[Cu(bpy)(tbip)]n _database_code_depnum_ccdc_archive 'CCDC 835415' #TrackingRef '- revised cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H40 Cu2 N4 O8' _chemical_formula_sum 'C44 H40 Cu2 N4 O8' _chemical_formula_weight 879.88 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 P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.7048(6) _cell_length_b 13.1186(5) _cell_length_c 26.8081(8) _cell_angle_alpha 90.00 _cell_angle_beta 131.266(1) _cell_angle_gamma 90.00 _cell_volume 3887.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 8148 _cell_measurement_theta_min 2.2312 _cell_measurement_theta_max 26.5424 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 1.156 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6679 _exptl_absorpt_correction_T_max 0.8190 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _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_type 'Bruker APEX area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32905 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 28.68 _reflns_number_total 9245 _reflns_number_gt 8009 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ISOR 0.02 is applied to one carbon atom (C12) of tert-butyl. ; _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^)+(0.0767P)^2^+4.9152P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9245 _refine_ls_number_parameters 526 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0821 _refine_ls_R_factor_gt 0.0701 _refine_ls_wR_factor_ref 0.1675 _refine_ls_wR_factor_gt 0.1598 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.113 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.45320(4) 0.08482(4) 0.70495(2) 0.02994(13) Uani 1 1 d . . . Cu2 Cu 0.19904(4) 0.47704(3) 0.34566(2) 0.02915(13) Uani 1 1 d . . . N1 N 0.4747(3) 0.1787(2) 0.77120(14) 0.0312(6) Uani 1 1 d . . . N2 N 0.2927(3) 0.0683(2) 0.67951(15) 0.0320(7) Uani 1 1 d . . . N3 N 0.1875(3) 0.5871(2) 0.28963(15) 0.0307(6) Uani 1 1 d . . . N4 N 0.3704(3) 0.4761(2) 0.38350(16) 0.0332(7) Uani 1 1 d . . . O1 O 0.6260(2) 0.0661(2) 0.75299(13) 0.0378(6) Uani 1 1 d . . . O2 O 0.5672(2) -0.0578(2) 0.78083(14) 0.0438(7) Uani 1 1 d . . . O3 O 1.0315(2) 0.0042(2) 0.81117(13) 0.0338(6) Uani 1 1 d . . . O4 O 1.1641(2) -0.0854(2) 0.90073(14) 0.0437(7) Uani 1 1 d . . . O5 O 0.3944(3) 0.0380(2) 0.61884(13) 0.0355(6) Uani 1 1 d . . . O6 O 0.4045(3) 0.2045(2) 0.61532(14) 0.0453(7) Uani 1 1 d . . . O7 O 0.2273(3) 0.3622(2) 0.39923(15) 0.0423(7) Uani 1 1 d . . . O8 O 0.1718(3) 0.2665(2) 0.31497(14) 0.0467(7) Uani 1 1 d . . . C1 C 0.7730(3) -0.0562(3) 0.83056(17) 0.0296(7) Uani 1 1 d . . . C2 C 0.8520(3) -0.0350(3) 0.82048(17) 0.0293(7) Uani 1 1 d . . . H2A H 0.8273 0.0047 0.7847 0.035 Uiso 1 1 calc R . . C3 C 0.9683(3) -0.0737(3) 0.86454(17) 0.0285(7) Uani 1 1 d . . . C4 C 1.0051(3) -0.1289(3) 0.91934(18) 0.0331(8) Uani 1 1 d . . . H4A H 1.0837 -0.1542 0.9488 0.040 Uiso 1 1 calc R . . C5 C 0.9291(3) -0.1477(3) 0.93165(17) 0.0313(7) Uani 1 1 d . . . C6 C 0.8107(3) -0.1131(3) 0.88502(18) 0.0325(8) Uani 1 1 d . . . H6A H 0.7558 -0.1284 0.8904 0.039 Uiso 1 1 calc R . . C7 C 0.6458(3) -0.0144(3) 0.78502(17) 0.0310(8) Uani 1 1 d . . . C8 C 1.0610(3) -0.0517(3) 0.85858(19) 0.0309(7) Uani 1 1 d . . . C9 C 0.9718(4) -0.2022(3) 0.99398(19) 0.0419(9) Uani 1 1 d . . . C10 C 0.9056(7) -0.3012(6) 0.9755(4) 0.119(3) Uani 1 1 d . . . H10A H 0.9436 -0.3520 0.9688 0.178 Uiso 1 1 calc R . . H10B H 0.8231 -0.2925 0.9352 0.178 Uiso 1 1 calc R . . H10C H 0.9076 -0.3224 1.0104 0.178 Uiso 1 1 calc R . . C11 C 0.9323(9) -0.1412(7) 1.0260(4) 0.128(4) Uani 1 1 d . . . H11A H 0.9480 -0.1805 1.0611 0.192 Uiso 1 1 calc R . . H11B H 0.8474 -0.1265 0.9931 0.192 Uiso 1 1 calc R . . H11C H 0.9770 -0.0785 1.0436 0.192 Uiso 1 1 calc R . . C12 C 1.1025(5) -0.2183(9) 1.0434(3) 0.132(4) Uani 1 1 d U . . H12A H 1.1269 -0.2611 1.0250 0.199 Uiso 1 1 calc R . . H12B H 1.1232 -0.2507 1.0818 0.199 Uiso 1 1 calc R . . H12C H 1.1432 -0.1539 1.0558 0.199 Uiso 1 1 calc R . . C13 C 0.5735(3) 0.2325(3) 0.8177(2) 0.0392(9) Uani 1 1 d . . . H13A H 0.6428 0.2226 0.8237 0.047 Uiso 1 1 calc R . . C14 C 0.5768(4) 0.3018(4) 0.8570(2) 0.0497(11) Uani 1 1 d . . . H14A H 0.6471 0.3382 0.8891 0.060 Uiso 1 1 calc R . . C15 C 0.4752(4) 0.3167(4) 0.8483(2) 0.0487(11) Uani 1 1 d . . . H15A H 0.4754 0.3641 0.8742 0.058 Uiso 1 1 calc R . . C16 C 0.3732(4) 0.2613(3) 0.8013(2) 0.0395(9) Uani 1 1 d . . . H16A H 0.3035 0.2702 0.7950 0.047 Uiso 1 1 calc R . . C17 C 0.3756(3) 0.1917(3) 0.76336(17) 0.0300(7) Uani 1 1 d . . . C18 C 0.2730(3) 0.1263(3) 0.71282(17) 0.0307(7) Uani 1 1 d . . . C19 C 0.1670(4) 0.1197(3) 0.7014(2) 0.0412(9) Uani 1 1 d . . . H19A H 0.1539 0.1616 0.7241 0.049 Uiso 1 1 calc R . . C20 C 0.0813(4) 0.0501(4) 0.6560(2) 0.0544(12) Uani 1 1 d . . . H20A H 0.0095 0.0435 0.6479 0.065 Uiso 1 1 calc R . . C21 C 0.1025(4) -0.0095(4) 0.6227(3) 0.0556(12) Uani 1 1 d . . . H21A H 0.0455 -0.0573 0.5920 0.067 Uiso 1 1 calc R . . C22 C 0.2073(4) 0.0016(4) 0.6348(2) 0.0463(10) Uani 1 1 d . . . H22A H 0.2202 -0.0384 0.6114 0.056 Uiso 1 1 calc R . . C23 C 0.3313(3) 0.1100(3) 0.51947(18) 0.0299(7) Uani 1 1 d . . . C24 C 0.2960(3) 0.1952(3) 0.48001(19) 0.0312(7) Uani 1 1 d . . . H24A H 0.3023 0.2596 0.4966 0.037 Uiso 1 1 calc R . . C25 C 0.2514(3) 0.1848(3) 0.41585(18) 0.0305(7) Uani 1 1 d . . . C26 C 0.2469(3) 0.0885(3) 0.39217(18) 0.0355(8) Uani 1 1 d . . . H26A H 0.2166 0.0819 0.3490 0.043 Uiso 1 1 calc R . . C27 C 0.2865(4) 0.0027(3) 0.43151(19) 0.0366(8) Uani 1 1 d . . . C28 C 0.3250(4) 0.0152(3) 0.49449(18) 0.0338(8) Uani 1 1 d . . . H28A H 0.3473 -0.0422 0.5208 0.041 Uiso 1 1 calc R . . C29 C 0.3804(3) 0.1204(3) 0.58914(17) 0.0304(7) Uani 1 1 d . . . C30 C 0.2125(3) 0.2767(3) 0.3719(2) 0.0351(8) Uani 1 1 d . . . C31 C 0.2912(5) -0.1011(3) 0.4072(2) 0.0500(11) Uani 1 1 d . . . C32 C 0.3851(7) -0.1705(5) 0.4635(3) 0.094(2) Uani 1 1 d . . . H32A H 0.3647 -0.1845 0.4902 0.142 Uiso 1 1 calc R . . H32B H 0.4629 -0.1381 0.4902 0.142 Uiso 1 1 calc R . . H32C H 0.3875 -0.2332 0.4459 0.142 Uiso 1 1 calc R . . C33 C 0.3365(6) -0.0853(5) 0.3689(3) 0.0773(18) Uani 1 1 d . . . H33A H 0.3399 -0.1500 0.3535 0.116 Uiso 1 1 calc R . . H33B H 0.4157 -0.0553 0.3980 0.116 Uiso 1 1 calc R . . H33C H 0.2817 -0.0411 0.3317 0.116 Uiso 1 1 calc R . . C34 C 0.1696(6) -0.1481(5) 0.3613(4) 0.112(3) Uani 1 1 d . . . H34A H 0.1402 -0.1582 0.3840 0.169 Uiso 1 1 calc R . . H34B H 0.1744 -0.2127 0.3463 0.169 Uiso 1 1 calc R . . H34C H 0.1153 -0.1041 0.3239 0.169 Uiso 1 1 calc R . . C35 C 0.0902(3) 0.6436(3) 0.2447(2) 0.0391(9) Uani 1 1 d . . . H35A H 0.0184 0.6295 0.2355 0.047 Uiso 1 1 calc R . . C36 C 0.0923(4) 0.7221(3) 0.2115(2) 0.0443(10) Uani 1 1 d . . . H36A H 0.0228 0.7598 0.1799 0.053 Uiso 1 1 calc R . . C37 C 0.1980(4) 0.7439(3) 0.2255(2) 0.0440(10) Uani 1 1 d . . . H37A H 0.2013 0.7968 0.2036 0.053 Uiso 1 1 calc R . . C38 C 0.2990(4) 0.6869(3) 0.2721(2) 0.0392(9) Uani 1 1 d . . . H38A H 0.3718 0.7009 0.2824 0.047 Uiso 1 1 calc R . . C39 C 0.2914(3) 0.6081(3) 0.30366(18) 0.0306(7) Uani 1 1 d . . . C40 C 0.3953(3) 0.5454(3) 0.35651(18) 0.0317(8) Uani 1 1 d . . . C41 C 0.5103(4) 0.5560(4) 0.3790(3) 0.0546(12) Uani 1 1 d . . . H41A H 0.5261 0.6030 0.3596 0.065 Uiso 1 1 calc R . . C42 C 0.6007(4) 0.4960(4) 0.4304(3) 0.0667(16) Uani 1 1 d . . . H42A H 0.6789 0.5017 0.4461 0.080 Uiso 1 1 calc R . . C43 C 0.5759(4) 0.4272(4) 0.4587(2) 0.0559(12) Uani 1 1 d . . . H43A H 0.6372 0.3873 0.4944 0.067 Uiso 1 1 calc R . . C44 C 0.4593(4) 0.4187(3) 0.4335(2) 0.0448(10) Uani 1 1 d . . . H44A H 0.4420 0.3711 0.4519 0.054 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0266(2) 0.0396(3) 0.0267(2) 0.00322(18) 0.01892(19) 0.00634(18) Cu2 0.0289(2) 0.0303(2) 0.0351(2) 0.00904(18) 0.0240(2) 0.00562(17) N1 0.0313(15) 0.0353(16) 0.0274(14) 0.0000(12) 0.0195(13) 0.0001(13) N2 0.0275(15) 0.0389(17) 0.0281(15) -0.0025(13) 0.0177(13) 0.0023(13) N3 0.0305(15) 0.0335(16) 0.0341(16) 0.0067(13) 0.0238(14) 0.0037(12) N4 0.0294(15) 0.0349(17) 0.0360(17) 0.0053(13) 0.0220(14) 0.0057(13) O1 0.0319(14) 0.0465(16) 0.0417(15) 0.0152(13) 0.0271(13) 0.0121(12) O2 0.0267(13) 0.0580(18) 0.0460(16) 0.0144(14) 0.0237(13) 0.0058(13) O3 0.0300(13) 0.0409(15) 0.0354(14) 0.0003(11) 0.0237(12) 0.0006(11) O4 0.0255(13) 0.0595(19) 0.0465(16) 0.0100(14) 0.0239(13) 0.0053(12) O5 0.0501(16) 0.0337(14) 0.0300(13) 0.0069(11) 0.0295(13) 0.0097(12) O6 0.0635(19) 0.0370(15) 0.0380(15) -0.0014(12) 0.0345(15) 0.0010(14) O7 0.0532(17) 0.0349(15) 0.0512(17) 0.0175(13) 0.0398(15) 0.0121(13) O8 0.0568(18) 0.0533(18) 0.0410(16) 0.0165(14) 0.0370(15) 0.0112(15) C1 0.0249(16) 0.0382(19) 0.0268(16) 0.0020(14) 0.0176(15) 0.0030(14) C2 0.0306(17) 0.0334(18) 0.0263(16) 0.0020(14) 0.0198(15) 0.0034(14) C3 0.0249(16) 0.0322(18) 0.0291(17) -0.0034(14) 0.0181(15) -0.0014(14) C4 0.0197(16) 0.037(2) 0.0322(18) 0.0012(15) 0.0125(15) 0.0019(14) C5 0.0266(17) 0.0338(19) 0.0269(17) 0.0023(14) 0.0148(15) -0.0016(14) C6 0.0285(17) 0.042(2) 0.0319(18) 0.0036(15) 0.0220(16) -0.0005(15) C7 0.0264(17) 0.041(2) 0.0256(17) 0.0030(15) 0.0172(15) 0.0059(15) C8 0.0275(17) 0.0324(18) 0.0372(19) -0.0039(15) 0.0233(16) -0.0024(14) C9 0.039(2) 0.046(2) 0.0309(19) 0.0078(17) 0.0186(18) -0.0018(18) C10 0.109(6) 0.084(5) 0.077(4) 0.036(4) 0.025(4) -0.027(4) C11 0.204(10) 0.132(7) 0.080(5) 0.046(5) 0.107(6) 0.068(7) C12 0.047(3) 0.252(10) 0.068(4) 0.085(5) 0.026(3) 0.008(5) C13 0.0272(18) 0.047(2) 0.0361(19) -0.0032(17) 0.0178(17) -0.0055(17) C14 0.047(2) 0.048(3) 0.043(2) -0.014(2) 0.025(2) -0.016(2) C15 0.055(3) 0.046(2) 0.049(2) -0.015(2) 0.036(2) -0.008(2) C16 0.045(2) 0.043(2) 0.042(2) -0.0053(18) 0.034(2) -0.0014(18) C17 0.0307(18) 0.0341(19) 0.0277(17) 0.0032(14) 0.0203(15) 0.0007(15) C18 0.0304(18) 0.0354(19) 0.0291(17) 0.0009(15) 0.0208(15) 0.0032(15) C19 0.034(2) 0.054(3) 0.046(2) -0.0066(19) 0.0307(19) -0.0012(18) C20 0.035(2) 0.067(3) 0.061(3) -0.008(2) 0.031(2) -0.009(2) C21 0.035(2) 0.061(3) 0.055(3) -0.021(2) 0.022(2) -0.015(2) C22 0.037(2) 0.051(3) 0.042(2) -0.0121(19) 0.022(2) 0.0000(19) C23 0.0350(18) 0.0291(17) 0.0333(18) 0.0063(14) 0.0259(16) 0.0083(14) C24 0.0380(19) 0.0277(17) 0.041(2) 0.0049(15) 0.0314(18) 0.0075(15) C25 0.0285(17) 0.0373(19) 0.0323(18) 0.0098(15) 0.0229(16) 0.0096(15) C26 0.038(2) 0.041(2) 0.0269(17) 0.0075(15) 0.0215(17) 0.0091(16) C27 0.044(2) 0.0333(19) 0.036(2) 0.0074(16) 0.0278(18) 0.0124(16) C28 0.044(2) 0.0287(18) 0.0316(18) 0.0079(15) 0.0259(17) 0.0083(16) C29 0.0311(18) 0.0357(19) 0.0284(17) 0.0043(15) 0.0213(15) 0.0091(15) C30 0.0323(19) 0.040(2) 0.046(2) 0.0154(17) 0.0314(18) 0.0095(16) C31 0.064(3) 0.038(2) 0.041(2) 0.0016(18) 0.032(2) 0.013(2) C32 0.154(7) 0.056(3) 0.071(4) 0.017(3) 0.073(4) 0.054(4) C33 0.111(5) 0.069(4) 0.081(4) 0.005(3) 0.075(4) 0.026(3) C34 0.088(5) 0.077(5) 0.166(8) -0.066(5) 0.081(6) -0.020(4) C35 0.0318(19) 0.045(2) 0.043(2) 0.0129(18) 0.0255(18) 0.0072(17) C36 0.044(2) 0.044(2) 0.044(2) 0.0140(19) 0.029(2) 0.0097(19) C37 0.056(3) 0.039(2) 0.041(2) 0.0086(18) 0.034(2) -0.0010(19) C38 0.040(2) 0.043(2) 0.044(2) 0.0035(18) 0.0315(19) -0.0053(17) C39 0.0328(18) 0.0314(18) 0.0330(18) -0.0021(15) 0.0240(16) -0.0020(15) C40 0.0280(17) 0.0324(19) 0.0346(18) -0.0012(15) 0.0206(16) 0.0007(14) C41 0.036(2) 0.057(3) 0.072(3) 0.014(2) 0.036(2) 0.001(2) C42 0.026(2) 0.068(3) 0.084(4) 0.010(3) 0.027(2) 0.001(2) C43 0.034(2) 0.053(3) 0.054(3) 0.009(2) 0.017(2) 0.012(2) C44 0.036(2) 0.044(2) 0.044(2) 0.0123(19) 0.0219(19) 0.0080(18) _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 O5 1.954(3) . ? Cu1 O1 1.965(3) . ? Cu1 N2 1.989(3) . ? Cu1 N1 2.008(3) . ? Cu1 O2 2.439(3) . ? Cu1 C7 2.511(4) . ? Cu2 O7 1.928(3) . ? Cu2 O3 1.995(3) 4_465 ? Cu2 N4 2.001(3) . ? Cu2 N3 2.008(3) . ? Cu2 O4 2.337(3) 4_465 ? Cu2 C8 2.475(4) 4_465 ? N1 C13 1.331(5) . ? N1 C17 1.339(5) . ? N2 C22 1.339(5) . ? N2 C18 1.342(5) . ? N3 C35 1.332(5) . ? N3 C39 1.339(5) . ? N4 C44 1.328(5) . ? N4 C40 1.354(5) . ? O1 C7 1.268(5) . ? O2 C7 1.226(4) . ? O3 C8 1.270(4) . ? O3 Cu2 1.995(2) 4_666 ? O4 C8 1.229(4) . ? O4 Cu2 2.337(3) 4_666 ? O5 C29 1.276(4) . ? O6 C29 1.228(5) . ? O7 C30 1.278(5) . ? O8 C30 1.226(5) . ? C1 C2 1.384(5) . ? C1 C6 1.389(5) . ? C1 C7 1.508(5) . ? C2 C3 1.384(5) . ? C2 H2A 0.9300 . ? C3 C4 1.389(5) . ? C3 C8 1.501(5) . ? C4 C5 1.381(5) . ? C4 H4A 0.9300 . ? C5 C6 1.388(5) . ? C5 C9 1.521(5) . ? C6 H6A 0.9300 . ? C8 Cu2 2.475(4) 4_666 ? C9 C12 1.461(7) . ? C9 C10 1.498(8) . ? C9 C11 1.539(8) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.368(6) . ? C13 H13A 0.9300 . ? C14 C15 1.367(6) . ? C14 H14A 0.9300 . ? C15 C16 1.368(6) . ? C15 H15A 0.9300 . ? C16 C17 1.385(5) . ? C16 H16A 0.9300 . ? C17 C18 1.467(5) . ? C18 C19 1.379(5) . ? C19 C20 1.371(6) . ? C19 H19A 0.9300 . ? C20 C21 1.367(7) . ? C20 H20A 0.9300 . ? C21 C22 1.357(6) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C24 1.383(5) . ? C23 C28 1.387(5) . ? C23 C29 1.500(5) . ? C24 C25 1.385(5) . ? C24 H24A 0.9300 . ? C25 C26 1.396(5) . ? C25 C30 1.509(5) . ? C26 C27 1.381(5) . ? C26 H26A 0.9300 . ? C27 C28 1.392(5) . ? C27 C31 1.530(6) . ? C28 H28A 0.9300 . ? C31 C34 1.480(8) . ? C31 C32 1.505(7) . ? C31 C33 1.562(7) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.375(6) . ? C35 H35A 0.9300 . ? C36 C37 1.366(6) . ? C36 H36A 0.9300 . ? C37 C38 1.371(6) . ? C37 H37A 0.9300 . ? C38 C39 1.386(5) . ? C38 H38A 0.9300 . ? C39 C40 1.470(5) . ? C40 C41 1.377(5) . ? C41 C42 1.367(7) . ? C41 H41A 0.9300 . ? C42 C43 1.374(7) . ? C42 H42A 0.9300 . ? C43 C44 1.371(6) . ? C43 H43A 0.9300 . ? C44 H44A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Cu1 O1 96.22(12) . . ? O5 Cu1 N2 93.45(12) . . ? O1 Cu1 N2 160.09(12) . . ? O5 Cu1 N1 157.86(12) . . ? O1 Cu1 N1 96.65(12) . . ? N2 Cu1 N1 80.17(12) . . ? O5 Cu1 O2 105.63(11) . . ? O1 Cu1 O2 58.49(10) . . ? N2 Cu1 O2 102.11(11) . . ? N1 Cu1 O2 96.45(12) . . ? O5 Cu1 C7 102.57(11) . . ? O1 Cu1 C7 29.86(12) . . ? N2 Cu1 C7 130.62(13) . . ? N1 Cu1 C7 97.54(12) . . ? O2 Cu1 C7 28.63(10) . . ? O7 Cu2 O3 92.03(12) . 4_465 ? O7 Cu2 N4 92.12(12) . . ? O3 Cu2 N4 172.99(12) 4_465 . ? O7 Cu2 N3 171.56(12) . . ? O3 Cu2 N3 95.47(11) 4_465 . ? N4 Cu2 N3 80.81(12) . . ? O7 Cu2 O4 91.95(12) . 4_465 ? O3 Cu2 O4 59.94(10) 4_465 4_465 ? N4 Cu2 O4 114.27(11) . 4_465 ? N3 Cu2 O4 95.16(12) . 4_465 ? O7 Cu2 C8 89.92(12) . 4_465 ? O3 Cu2 C8 30.68(11) 4_465 4_465 ? N4 Cu2 C8 143.69(13) . 4_465 ? N3 Cu2 C8 98.51(12) . 4_465 ? O4 Cu2 C8 29.43(11) 4_465 4_465 ? C13 N1 C17 118.8(3) . . ? C13 N1 Cu1 126.2(3) . . ? C17 N1 Cu1 114.8(2) . . ? C22 N2 C18 118.6(3) . . ? C22 N2 Cu1 125.3(3) . . ? C18 N2 Cu1 116.0(2) . . ? C35 N3 C39 119.1(3) . . ? C35 N3 Cu2 125.9(3) . . ? C39 N3 Cu2 114.8(2) . . ? C44 N4 C40 119.1(3) . . ? C44 N4 Cu2 126.0(3) . . ? C40 N4 Cu2 114.8(2) . . ? C7 O1 Cu1 99.7(2) . . ? C7 O2 Cu1 78.9(2) . . ? C8 O3 Cu2 96.0(2) . 4_666 ? C8 O4 Cu2 81.5(2) . 4_666 ? C29 O5 Cu1 103.6(2) . . ? C30 O7 Cu2 112.9(2) . . ? C2 C1 C6 120.6(3) . . ? C2 C1 C7 121.4(3) . . ? C6 C1 C7 118.0(3) . . ? C1 C2 C3 119.0(3) . . ? C1 C2 H2A 120.5 . . ? C3 C2 H2A 120.5 . . ? C2 C3 C4 119.6(3) . . ? C2 C3 C8 122.5(3) . . ? C4 C3 C8 117.7(3) . . ? C5 C4 C3 122.3(3) . . ? C5 C4 H4A 118.9 . . ? C3 C4 H4A 118.9 . . ? C4 C5 C6 117.3(3) . . ? C4 C5 C9 122.3(3) . . ? C6 C5 C9 120.4(3) . . ? C5 C6 C1 121.1(3) . . ? C5 C6 H6A 119.5 . . ? C1 C6 H6A 119.5 . . ? O2 C7 O1 122.9(3) . . ? O2 C7 C1 119.8(3) . . ? O1 C7 C1 117.3(3) . . ? O2 C7 Cu1 72.4(2) . . ? O1 C7 Cu1 50.46(17) . . ? C1 C7 Cu1 167.8(3) . . ? O4 C8 O3 121.9(3) . . ? O4 C8 C3 119.3(3) . . ? O3 C8 C3 118.8(3) . . ? O4 C8 Cu2 69.1(2) . 4_666 ? O3 C8 Cu2 53.31(17) . 4_666 ? C3 C8 Cu2 167.7(3) . 4_666 ? C12 C9 C10 110.7(6) . . ? C12 C9 C5 114.0(4) . . ? C10 C9 C5 109.6(4) . . ? C12 C9 C11 108.9(6) . . ? C10 C9 C11 103.5(6) . . ? C5 C9 C11 109.5(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C14 122.3(4) . . ? N1 C13 H13A 118.8 . . ? C14 C13 H13A 118.8 . . ? C15 C14 C13 119.1(4) . . ? C15 C14 H14A 120.5 . . ? C13 C14 H14A 120.5 . . ? C14 C15 C16 119.4(4) . . ? C14 C15 H15A 120.3 . . ? C16 C15 H15A 120.3 . . ? C15 C16 C17 118.9(4) . . ? C15 C16 H16A 120.6 . . ? C17 C16 H16A 120.6 . . ? N1 C17 C16 121.4(3) . . ? N1 C17 C18 114.8(3) . . ? C16 C17 C18 123.7(3) . . ? N2 C18 C19 121.6(4) . . ? N2 C18 C17 113.9(3) . . ? C19 C18 C17 124.4(3) . . ? C20 C19 C18 118.8(4) . . ? C20 C19 H19A 120.6 . . ? C18 C19 H19A 120.6 . . ? C21 C20 C19 119.2(4) . . ? C21 C20 H20A 120.4 . . ? C19 C20 H20A 120.4 . . ? C22 C21 C20 119.6(4) . . ? C22 C21 H21A 120.2 . . ? C20 C21 H21A 120.2 . . ? N2 C22 C21 122.1(4) . . ? N2 C22 H22A 119.0 . . ? C21 C22 H22A 119.0 . . ? C24 C23 C28 118.9(3) . . ? C24 C23 C29 120.6(3) . . ? C28 C23 C29 120.4(3) . . ? C23 C24 C25 120.1(3) . . ? C23 C24 H24A 120.0 . . ? C25 C24 H24A 120.0 . . ? C24 C25 C26 119.7(3) . . ? C24 C25 C30 121.0(3) . . ? C26 C25 C30 119.2(3) . . ? C27 C26 C25 121.4(3) . . ? C27 C26 H26A 119.3 . . ? C25 C26 H26A 119.3 . . ? C26 C27 C28 117.4(4) . . ? C26 C27 C31 121.0(4) . . ? C28 C27 C31 121.6(3) . . ? C23 C28 C27 122.4(3) . . ? C23 C28 H28A 118.8 . . ? C27 C28 H28A 118.8 . . ? O6 C29 O5 122.5(3) . . ? O6 C29 C23 120.9(3) . . ? O5 C29 C23 116.6(3) . . ? O8 C30 O7 124.6(4) . . ? O8 C30 C25 120.5(4) . . ? O7 C30 C25 114.9(3) . . ? C34 C31 C32 112.7(6) . . ? C34 C31 C27 110.8(4) . . ? C32 C31 C27 112.4(4) . . ? C34 C31 C33 108.3(5) . . ? C32 C31 C33 103.4(5) . . ? C27 C31 C33 108.7(4) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N3 C35 C36 122.1(4) . . ? N3 C35 H35A 118.9 . . ? C36 C35 H35A 118.9 . . ? C37 C36 C35 119.1(4) . . ? C37 C36 H36A 120.4 . . ? C35 C36 H36A 120.4 . . ? C36 C37 C38 119.2(4) . . ? C36 C37 H37A 120.4 . . ? C38 C37 H37A 120.4 . . ? C37 C38 C39 119.2(4) . . ? C37 C38 H38A 120.4 . . ? C39 C38 H38A 120.4 . . ? N3 C39 C38 121.3(3) . . ? N3 C39 C40 115.0(3) . . ? C38 C39 C40 123.6(3) . . ? N4 C40 C41 121.3(4) . . ? N4 C40 C39 114.5(3) . . ? C41 C40 C39 124.1(4) . . ? C42 C41 C40 118.7(4) . . ? C42 C41 H41A 120.6 . . ? C40 C41 H41A 120.6 . . ? C41 C42 C43 119.9(4) . . ? C41 C42 H42A 120.1 . . ? C43 C42 H42A 120.1 . . ? C44 C43 C42 118.8(4) . . ? C44 C43 H43A 120.6 . . ? C42 C43 H43A 120.6 . . ? N4 C44 C43 122.0(4) . . ? N4 C44 H44A 119.0 . . ? C43 C44 H44A 119.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Cu1 N1 C13 -106.0(4) . . . . ? O1 Cu1 N1 C13 19.1(3) . . . . ? N2 Cu1 N1 C13 179.3(3) . . . . ? O2 Cu1 N1 C13 78.0(3) . . . . ? C7 Cu1 N1 C13 49.2(3) . . . . ? O5 Cu1 N1 C17 69.2(4) . . . . ? O1 Cu1 N1 C17 -165.6(3) . . . . ? N2 Cu1 N1 C17 -5.5(3) . . . . ? O2 Cu1 N1 C17 -106.7(3) . . . . ? C7 Cu1 N1 C17 -135.6(3) . . . . ? O5 Cu1 N2 C22 27.9(4) . . . . ? O1 Cu1 N2 C22 -91.1(5) . . . . ? N1 Cu1 N2 C22 -173.5(4) . . . . ? O2 Cu1 N2 C22 -78.9(4) . . . . ? C7 Cu1 N2 C22 -81.9(4) . . . . ? O5 Cu1 N2 C18 -155.4(3) . . . . ? O1 Cu1 N2 C18 85.6(5) . . . . ? N1 Cu1 N2 C18 3.2(3) . . . . ? O2 Cu1 N2 C18 97.8(3) . . . . ? C7 Cu1 N2 C18 94.8(3) . . . . ? O5 Cu1 O1 C7 -104.5(2) . . . . ? N2 Cu1 O1 C7 14.1(5) . . . . ? N1 Cu1 O1 C7 93.6(2) . . . . ? O2 Cu1 O1 C7 0.1(2) . . . . ? O5 Cu1 O2 C7 87.7(2) . . . . ? O1 Cu1 O2 C7 -0.1(2) . . . . ? N2 Cu1 O2 C7 -175.2(2) . . . . ? N1 Cu1 O2 C7 -93.9(2) . . . . ? O1 Cu1 O5 C29 -95.7(2) . . . . ? N2 Cu1 O5 C29 101.7(2) . . . . ? N1 Cu1 O5 C29 29.5(4) . . . . ? O2 Cu1 O5 C29 -154.7(2) . . . . ? C7 Cu1 O5 C29 -125.3(2) . . . . ? C6 C1 C2 C3 1.8(6) . . . . ? C7 C1 C2 C3 178.8(3) . . . . ? C1 C2 C3 C4 -2.9(5) . . . . ? C1 C2 C3 C8 -178.0(3) . . . . ? C2 C3 C4 C5 0.4(6) . . . . ? C8 C3 C4 C5 175.8(3) . . . . ? C3 C4 C5 C6 3.0(6) . . . . ? C3 C4 C5 C9 -175.9(4) . . . . ? C4 C5 C6 C1 -4.1(6) . . . . ? C9 C5 C6 C1 174.8(4) . . . . ? C2 C1 C6 C5 1.8(6) . . . . ? C7 C1 C6 C5 -175.3(3) . . . . ? Cu1 O2 C7 O1 0.1(3) . . . . ? Cu1 O2 C7 C1 179.3(3) . . . . ? Cu1 O1 C7 O2 -0.1(4) . . . . ? Cu1 O1 C7 C1 -179.3(3) . . . . ? C2 C1 C7 O2 156.6(4) . . . . ? C6 C1 C7 O2 -26.3(5) . . . . ? C2 C1 C7 O1 -24.2(5) . . . . ? C6 C1 C7 O1 152.9(4) . . . . ? C2 C1 C7 Cu1 -26.6(14) . . . . ? C6 C1 C7 Cu1 150.5(11) . . . . ? O5 Cu1 C7 O2 -99.7(2) . . . . ? O1 Cu1 C7 O2 179.9(4) . . . . ? N2 Cu1 C7 O2 6.2(3) . . . . ? N1 Cu1 C7 O2 89.6(2) . . . . ? O5 Cu1 C7 O1 80.5(2) . . . . ? N2 Cu1 C7 O1 -173.7(2) . . . . ? N1 Cu1 C7 O1 -90.2(2) . . . . ? O2 Cu1 C7 O1 -179.9(4) . . . . ? O5 Cu1 C7 C1 83.3(12) . . . . ? O1 Cu1 C7 C1 2.8(11) . . . . ? N2 Cu1 C7 C1 -170.9(12) . . . . ? N1 Cu1 C7 C1 -87.4(12) . . . . ? O2 Cu1 C7 C1 -177.1(14) . . . . ? Cu2 O4 C8 O3 7.8(3) 4_666 . . . ? Cu2 O4 C8 C3 -169.9(3) 4_666 . . . ? Cu2 O3 C8 O4 -9.0(4) 4_666 . . . ? Cu2 O3 C8 C3 168.7(3) 4_666 . . . ? C2 C3 C8 O4 177.4(4) . . . . ? C4 C3 C8 O4 2.2(5) . . . . ? C2 C3 C8 O3 -0.4(5) . . . . ? C4 C3 C8 O3 -175.6(3) . . . . ? C2 C3 C8 Cu2 47.2(14) . . . 4_666 ? C4 C3 C8 Cu2 -128.1(12) . . . 4_666 ? C4 C5 C9 C12 8.9(8) . . . . ? C6 C5 C9 C12 -170.0(6) . . . . ? C4 C5 C9 C10 -115.9(6) . . . . ? C6 C5 C9 C10 65.2(6) . . . . ? C4 C5 C9 C11 131.2(6) . . . . ? C6 C5 C9 C11 -47.7(7) . . . . ? C17 N1 C13 C14 -1.1(6) . . . . ? Cu1 N1 C13 C14 173.9(3) . . . . ? N1 C13 C14 C15 0.0(7) . . . . ? C13 C14 C15 C16 0.8(7) . . . . ? C14 C15 C16 C17 -0.4(7) . . . . ? C13 N1 C17 C16 1.6(5) . . . . ? Cu1 N1 C17 C16 -174.0(3) . . . . ? C13 N1 C17 C18 -177.7(3) . . . . ? Cu1 N1 C17 C18 6.7(4) . . . . ? C15 C16 C17 N1 -0.8(6) . . . . ? C15 C16 C17 C18 178.3(4) . . . . ? C22 N2 C18 C19 -1.0(6) . . . . ? Cu1 N2 C18 C19 -177.9(3) . . . . ? C22 N2 C18 C17 176.3(4) . . . . ? Cu1 N2 C18 C17 -0.6(4) . . . . ? N1 C17 C18 N2 -4.1(5) . . . . ? C16 C17 C18 N2 176.7(4) . . . . ? N1 C17 C18 C19 173.1(4) . . . . ? C16 C17 C18 C19 -6.1(6) . . . . ? N2 C18 C19 C20 1.7(6) . . . . ? C17 C18 C19 C20 -175.3(4) . . . . ? C18 C19 C20 C21 -0.9(7) . . . . ? C19 C20 C21 C22 -0.5(8) . . . . ? C18 N2 C22 C21 -0.5(7) . . . . ? Cu1 N2 C22 C21 176.1(4) . . . . ? C20 C21 C22 N2 1.2(8) . . . . ? C28 C23 C24 C25 2.2(6) . . . . ? C29 C23 C24 C25 179.6(3) . . . . ? C23 C24 C25 C26 -2.6(5) . . . . ? C23 C24 C25 C30 -180.0(3) . . . . ? C24 C25 C26 C27 -0.3(6) . . . . ? C30 C25 C26 C27 177.1(4) . . . . ? C25 C26 C27 C28 3.4(6) . . . . ? C25 C26 C27 C31 -174.8(4) . . . . ? C24 C23 C28 C27 1.2(6) . . . . ? C29 C23 C28 C27 -176.3(4) . . . . ? C26 C27 C28 C23 -3.9(6) . . . . ? C31 C27 C28 C23 174.2(4) . . . . ? Cu1 O5 C29 O6 1.3(4) . . . . ? Cu1 O5 C29 C23 -178.1(2) . . . . ? C24 C23 C29 O6 -9.2(6) . . . . ? C28 C23 C29 O6 168.2(4) . . . . ? C24 C23 C29 O5 170.2(3) . . . . ? C28 C23 C29 O5 -12.4(5) . . . . ? Cu2 O7 C30 O8 -7.8(5) . . . . ? Cu2 O7 C30 C25 171.3(2) . . . . ? C24 C25 C30 O8 -179.1(3) . . . . ? C26 C25 C30 O8 3.6(5) . . . . ? C24 C25 C30 O7 1.8(5) . . . . ? C26 C25 C30 O7 -175.5(3) . . . . ? C26 C27 C31 C34 -79.4(6) . . . . ? C28 C27 C31 C34 102.5(6) . . . . ? C26 C27 C31 C32 153.4(5) . . . . ? C28 C27 C31 C32 -24.7(7) . . . . ? C26 C27 C31 C33 39.5(6) . . . . ? C28 C27 C31 C33 -138.6(5) . . . . ? C39 N3 C35 C36 0.9(6) . . . . ? Cu2 N3 C35 C36 175.6(3) . . . . ? N3 C35 C36 C37 -0.9(7) . . . . ? C35 C36 C37 C38 0.2(7) . . . . ? C36 C37 C38 C39 0.3(6) . . . . ? C35 N3 C39 C38 -0.3(6) . . . . ? Cu2 N3 C39 C38 -175.6(3) . . . . ? C35 N3 C39 C40 176.7(3) . . . . ? Cu2 N3 C39 C40 1.4(4) . . . . ? C37 C38 C39 N3 -0.3(6) . . . . ? C37 C38 C39 C40 -177.1(4) . . . . ? C44 N4 C40 C41 1.3(6) . . . . ? Cu2 N4 C40 C41 177.9(4) . . . . ? C44 N4 C40 C39 -177.3(4) . . . . ? Cu2 N4 C40 C39 -0.7(4) . . . . ? N3 C39 C40 N4 -0.5(5) . . . . ? C38 C39 C40 N4 176.5(4) . . . . ? N3 C39 C40 C41 -179.0(4) . . . . ? C38 C39 C40 C41 -2.1(6) . . . . ? N4 C40 C41 C42 -1.1(7) . . . . ? C39 C40 C41 C42 177.3(5) . . . . ? C40 C41 C42 C43 -0.3(9) . . . . ? C41 C42 C43 C44 1.6(9) . . . . ? C40 N4 C44 C43 0.0(7) . . . . ? Cu2 N4 C44 C43 -176.2(4) . . . . ? C42 C43 C44 N4 -1.5(8) . . . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.644 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.096 #============================================================================== data_CuPhen1a-[Cu(tbip)(phen)(H2O)]n _database_code_depnum_ccdc_archive 'CCDC 835416' #TrackingRef '- revised cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H22 Cu N2 O5' _chemical_formula_sum 'C24 H22 Cu N2 O5' _chemical_formula_weight 481.98 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 P21/c _symmetry_space_group_name_Hall '-P 2ybc' 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 15.0898(10) _cell_length_b 12.3402(8) _cell_length_c 12.2249(8) _cell_angle_alpha 90.00 _cell_angle_beta 107.505(1) _cell_angle_gamma 90.00 _cell_volume 2171.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3171 _cell_measurement_theta_min 2.1740 _cell_measurement_theta_max 26.3091 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.475 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 996 _exptl_absorpt_coefficient_mu 1.045 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8424 _exptl_absorpt_correction_T_max 0.9211 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12399 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0571 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 28.66 _reflns_number_total 4993 _reflns_number_gt 4058 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0644P)^2^+1.1038P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4993 _refine_ls_number_parameters 294 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0692 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1280 _refine_ls_wR_factor_gt 0.1207 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 0.36822(2) 0.42376(3) 0.57976(3) 0.01830(12) Uani 1 1 d . . . O1 O 0.36807(14) 0.53386(15) 0.45656(18) 0.0197(4) Uani 1 1 d . . . O1W O 0.51403(14) 0.45223(16) 0.68200(19) 0.0220(5) Uani 1 1 d . . . H1 H 0.5187 0.5136 0.7130 0.059(14) Uiso 1 1 calc R . . H2 H 0.5494 0.4571 0.6461 0.049(13) Uiso 1 1 d R . . O2 O 0.21908(15) 0.49726(17) 0.42682(19) 0.0274(5) Uani 1 1 d . . . O3 O 0.32646(14) 0.97186(16) 0.17048(18) 0.0231(5) Uani 1 1 d . . . O4 O 0.44808(14) 0.86943(16) 0.26250(18) 0.0227(5) Uani 1 1 d . . . N1 N 0.30009(16) 0.30689(18) 0.6389(2) 0.0184(5) Uani 1 1 d . . . N2 N 0.40415(17) 0.29595(18) 0.5014(2) 0.0175(5) Uani 1 1 d . . . C1 C 0.2558(2) 0.6459(2) 0.3262(3) 0.0187(6) Uani 1 1 d . . . C2 C 0.3217(2) 0.7195(2) 0.3148(3) 0.0186(6) Uani 1 1 d . . . H2A H 0.3847 0.7125 0.3603 0.022 Uiso 1 1 calc R . . C3 C 0.2949(2) 0.8037(2) 0.2360(3) 0.0182(6) Uani 1 1 d . . . C4 C 0.2034(2) 0.8120(2) 0.1690(3) 0.0237(7) Uani 1 1 d . . . H4A H 0.1860 0.8697 0.1154 0.028 Uiso 1 1 calc R . . C5 C 0.1360(2) 0.7384(3) 0.1777(3) 0.0247(7) Uani 1 1 d . . . C6 C 0.1643(2) 0.6565(2) 0.2593(3) 0.0207(6) Uani 1 1 d . . . H6A H 0.1195 0.6065 0.2693 0.025 Uiso 1 1 calc R . . C7 C 0.2809(2) 0.5522(2) 0.4091(3) 0.0195(6) Uani 1 1 d . . . C8 C 0.3637(2) 0.8863(2) 0.2225(2) 0.0188(6) Uani 1 1 d . . . C9 C 0.0365(2) 0.7508(3) 0.1003(3) 0.0392(9) Uani 1 1 d . . . C10 C -0.0257(3) 0.6579(4) 0.1154(4) 0.0502(11) Uani 1 1 d . . . H10A H -0.0005 0.5890 0.0983 0.075 Uiso 1 1 calc R . . H10B H -0.0885 0.6681 0.0630 0.075 Uiso 1 1 calc R . . H10C H -0.0279 0.6570 0.1947 0.075 Uiso 1 1 calc R . . C11 C 0.0366(3) 0.7540(6) -0.0241(4) 0.090(2) Uani 1 1 d . . . H11A H 0.0627 0.6862 -0.0429 0.136 Uiso 1 1 calc R . . H11B H 0.0743 0.8152 -0.0352 0.136 Uiso 1 1 calc R . . H11C H -0.0273 0.7624 -0.0743 0.136 Uiso 1 1 calc R . . C12 C -0.0035(3) 0.8569(4) 0.1314(5) 0.0694(16) Uani 1 1 d . . . H12A H -0.0018 0.8549 0.2121 0.104 Uiso 1 1 calc R . . H12B H -0.0679 0.8654 0.0829 0.104 Uiso 1 1 calc R . . H12C H 0.0336 0.9182 0.1189 0.104 Uiso 1 1 calc R . . C13 C 0.2488(2) 0.3165(2) 0.7089(3) 0.0228(6) Uani 1 1 d . . . H13A H 0.2412 0.3860 0.7383 0.027 Uiso 1 1 calc R . . C14 C 0.2058(2) 0.2276(3) 0.7406(3) 0.0275(7) Uani 1 1 d . . . H14A H 0.1702 0.2367 0.7922 0.033 Uiso 1 1 calc R . . C15 C 0.2143(2) 0.1276(3) 0.6981(3) 0.0279(7) Uani 1 1 d . . . H15A H 0.1841 0.0669 0.7190 0.033 Uiso 1 1 calc R . . C16 C 0.2679(2) 0.1148(2) 0.6234(3) 0.0226(6) Uani 1 1 d . . . C17 C 0.2829(2) 0.0138(2) 0.5739(3) 0.0285(7) Uani 1 1 d . . . H17A H 0.2544 -0.0501 0.5907 0.034 Uiso 1 1 calc R . . C18 C 0.3367(2) 0.0080(2) 0.5042(3) 0.0267(7) Uani 1 1 d . . . H18A H 0.3449 -0.0598 0.4717 0.032 Uiso 1 1 calc R . . C19 C 0.3820(2) 0.1025(2) 0.4780(3) 0.0203(6) Uani 1 1 d . . . C20 C 0.4414(2) 0.1023(2) 0.4088(3) 0.0226(7) Uani 1 1 d . . . H20A H 0.4547 0.0365 0.3767 0.027 Uiso 1 1 calc R . . C21 C 0.4797(2) 0.1971(2) 0.3880(3) 0.0228(6) Uani 1 1 d . . . H21A H 0.5199 0.1979 0.3412 0.027 Uiso 1 1 calc R . . C22 C 0.4596(2) 0.2929(2) 0.4361(3) 0.0210(6) Uani 1 1 d . . . H22A H 0.4868 0.3585 0.4213 0.025 Uiso 1 1 calc R . . C23 C 0.3666(2) 0.2018(2) 0.5232(2) 0.0176(6) Uani 1 1 d . . . C24 C 0.3099(2) 0.2074(2) 0.5972(2) 0.0182(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0235(2) 0.01182(17) 0.0214(2) -0.00140(14) 0.00956(15) -0.00137(14) O1 0.0203(11) 0.0162(9) 0.0237(12) 0.0050(8) 0.0085(9) 0.0028(8) O1W 0.0200(11) 0.0195(10) 0.0272(12) -0.0008(9) 0.0080(10) 0.0000(8) O2 0.0257(12) 0.0254(11) 0.0309(13) 0.0040(9) 0.0083(10) -0.0083(9) O3 0.0256(11) 0.0173(10) 0.0277(12) 0.0087(9) 0.0101(10) 0.0036(8) O4 0.0200(11) 0.0181(10) 0.0289(13) 0.0035(9) 0.0058(9) -0.0003(8) N1 0.0189(12) 0.0173(12) 0.0178(13) 0.0011(10) 0.0035(10) -0.0026(9) N2 0.0211(13) 0.0143(11) 0.0167(13) -0.0011(9) 0.0052(10) -0.0001(9) C1 0.0203(15) 0.0162(13) 0.0200(16) -0.0006(11) 0.0065(12) 0.0021(11) C2 0.0159(14) 0.0164(13) 0.0217(16) -0.0015(11) 0.0029(12) 0.0026(11) C3 0.0219(15) 0.0143(13) 0.0205(16) -0.0012(11) 0.0094(12) 0.0013(11) C4 0.0237(16) 0.0245(15) 0.0203(17) 0.0057(12) 0.0026(13) 0.0060(12) C5 0.0219(16) 0.0290(16) 0.0242(18) 0.0038(13) 0.0082(13) 0.0035(13) C6 0.0191(15) 0.0225(14) 0.0226(17) -0.0034(12) 0.0093(13) -0.0034(12) C7 0.0258(16) 0.0147(13) 0.0189(16) -0.0028(11) 0.0079(13) 0.0014(11) C8 0.0250(16) 0.0192(13) 0.0143(15) -0.0020(11) 0.0092(12) -0.0008(12) C9 0.0203(17) 0.059(2) 0.033(2) 0.0170(18) -0.0001(15) 0.0002(16) C10 0.0221(19) 0.062(3) 0.059(3) 0.005(2) 0.0011(19) -0.0092(18) C11 0.038(3) 0.193(7) 0.031(3) 0.028(3) -0.005(2) -0.030(3) C12 0.026(2) 0.060(3) 0.116(5) 0.036(3) 0.013(3) 0.017(2) C13 0.0198(15) 0.0246(15) 0.0238(17) -0.0021(12) 0.0064(13) 0.0005(12) C14 0.0211(16) 0.0366(18) 0.0277(18) 0.0020(14) 0.0117(14) -0.0002(13) C15 0.0272(17) 0.0265(16) 0.0286(19) 0.0087(14) 0.0066(14) -0.0032(13) C16 0.0215(16) 0.0203(14) 0.0225(17) 0.0040(12) 0.0014(13) -0.0040(12) C17 0.0315(18) 0.0159(14) 0.035(2) 0.0014(13) 0.0059(15) -0.0082(13) C18 0.0333(18) 0.0144(14) 0.0294(19) -0.0020(12) 0.0048(15) -0.0016(12) C19 0.0231(16) 0.0173(13) 0.0160(15) -0.0013(11) -0.0010(12) 0.0023(11) C20 0.0276(17) 0.0196(14) 0.0185(16) -0.0056(12) 0.0036(13) 0.0026(12) C21 0.0285(17) 0.0230(15) 0.0175(16) -0.0012(12) 0.0079(13) 0.0018(12) C22 0.0227(15) 0.0177(14) 0.0236(17) 0.0004(12) 0.0083(13) -0.0042(11) C23 0.0211(15) 0.0147(13) 0.0142(15) 0.0006(11) 0.0009(12) -0.0010(11) C24 0.0198(15) 0.0165(13) 0.0167(15) 0.0026(11) 0.0032(12) 0.0015(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O3 1.925(2) 4_576 ? Cu1 N2 2.003(2) . ? Cu1 N1 2.027(2) . ? Cu1 O1 2.028(2) . ? Cu1 O1W 2.207(2) . ? O1 C7 1.288(4) . ? O1W H1 0.8400 . ? O1W H2 0.7888 . ? O2 C7 1.224(4) . ? O3 C8 1.273(3) . ? O3 Cu1 1.925(2) 4_575 ? O4 C8 1.236(4) . ? N1 C13 1.320(4) . ? N1 C24 1.354(4) . ? N2 C22 1.319(4) . ? N2 C23 1.354(3) . ? C1 C6 1.382(4) . ? C1 C2 1.385(4) . ? C1 C7 1.509(4) . ? C2 C3 1.391(4) . ? C2 H2A 0.9500 . ? C3 C4 1.380(4) . ? C3 C8 1.500(4) . ? C4 C5 1.392(4) . ? C4 H4A 0.9500 . ? C5 C6 1.394(4) . ? C5 C9 1.522(4) . ? C6 H6A 0.9500 . ? C9 C11 1.521(5) . ? C9 C10 1.528(5) . ? C9 C12 1.537(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.388(4) . ? C13 H13A 0.9500 . ? C14 C15 1.360(5) . ? C14 H14A 0.9500 . ? C15 C16 1.399(4) . ? C15 H15A 0.9500 . ? C16 C24 1.390(4) . ? C16 C17 1.433(4) . ? C17 C18 1.345(5) . ? C17 H17A 0.9500 . ? C18 C19 1.436(4) . ? C18 H18A 0.9500 . ? C19 C23 1.392(4) . ? C19 C20 1.406(4) . ? C20 C21 1.362(4) . ? C20 H20A 0.9500 . ? C21 C22 1.394(4) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C24 1.422(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 O3 Cu1 N2 170.05(9) 4_576 . ? O3 Cu1 N1 88.94(9) 4_576 . ? N2 Cu1 N1 81.36(10) . . ? O3 Cu1 O1 92.99(9) 4_576 . ? N2 Cu1 O1 96.44(9) . . ? N1 Cu1 O1 148.70(9) . . ? O3 Cu1 O1W 90.60(9) 4_576 . ? N2 Cu1 O1W 91.66(9) . . ? N1 Cu1 O1W 115.94(9) . . ? O1 Cu1 O1W 95.29(8) . . ? C7 O1 Cu1 103.02(17) . . ? Cu1 O1W H1 109.5 . . ? Cu1 O1W H2 115.0 . . ? H1 O1W H2 101.7 . . ? C8 O3 Cu1 132.13(19) . 4_575 ? C13 N1 C24 118.5(2) . . ? C13 N1 Cu1 128.8(2) . . ? C24 N1 Cu1 112.74(19) . . ? C22 N2 C23 118.3(2) . . ? C22 N2 Cu1 128.63(19) . . ? C23 N2 Cu1 113.07(19) . . ? C6 C1 C2 119.9(3) . . ? C6 C1 C7 118.3(3) . . ? C2 C1 C7 121.8(3) . . ? C1 C2 C3 119.4(3) . . ? C1 C2 H2A 120.3 . . ? C3 C2 H2A 120.3 . . ? C4 C3 C2 119.8(3) . . ? C4 C3 C8 119.1(3) . . ? C2 C3 C8 121.1(3) . . ? C3 C4 C5 122.0(3) . . ? C3 C4 H4A 119.0 . . ? C5 C4 H4A 119.0 . . ? C4 C5 C6 117.0(3) . . ? C4 C5 C9 119.6(3) . . ? C6 C5 C9 123.4(3) . . ? C1 C6 C5 121.9(3) . . ? C1 C6 H6A 119.0 . . ? C5 C6 H6A 119.0 . . ? O2 C7 O1 123.5(3) . . ? O2 C7 C1 119.5(3) . . ? O1 C7 C1 117.0(3) . . ? O4 C8 O3 125.8(3) . . ? O4 C8 C3 120.4(3) . . ? O3 C8 C3 113.7(3) . . ? C11 C9 C5 109.1(3) . . ? C11 C9 C10 109.0(4) . . ? C5 C9 C10 112.1(3) . . ? C11 C9 C12 110.1(4) . . ? C5 C9 C12 108.6(3) . . ? C10 C9 C12 107.9(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C14 121.7(3) . . ? N1 C13 H13A 119.2 . . ? C14 C13 H13A 119.2 . . ? C15 C14 C13 120.3(3) . . ? C15 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? C14 C15 C16 119.4(3) . . ? C14 C15 H15A 120.3 . . ? C16 C15 H15A 120.3 . . ? C24 C16 C15 116.8(3) . . ? C24 C16 C17 118.5(3) . . ? C15 C16 C17 124.7(3) . . ? C18 C17 C16 121.1(3) . . ? C18 C17 H17A 119.5 . . ? C16 C17 H17A 119.5 . . ? C17 C18 C19 121.1(3) . . ? C17 C18 H18A 119.4 . . ? C19 C18 H18A 119.4 . . ? C23 C19 C20 116.9(3) . . ? C23 C19 C18 118.6(3) . . ? C20 C19 C18 124.4(3) . . ? C21 C20 C19 119.6(3) . . ? C21 C20 H20A 120.2 . . ? C19 C20 H20A 120.2 . . ? C20 C21 C22 119.4(3) . . ? C20 C21 H21A 120.3 . . ? C22 C21 H21A 120.3 . . ? N2 C22 C21 122.6(3) . . ? N2 C22 H22A 118.7 . . ? C21 C22 H22A 118.7 . . ? N2 C23 C19 123.2(3) . . ? N2 C23 C24 116.8(2) . . ? C19 C23 C24 120.0(3) . . ? N1 C24 C16 123.4(3) . . ? N1 C24 C23 116.0(2) . . ? C16 C24 C23 120.7(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Cu1 O1 C7 -69.78(18) 4_576 . . . ? N2 Cu1 O1 C7 107.06(18) . . . . ? N1 Cu1 O1 C7 23.1(3) . . . . ? O1W Cu1 O1 C7 -160.66(17) . . . . ? O3 Cu1 N1 C13 1.7(3) 4_576 . . . ? N2 Cu1 N1 C13 179.5(3) . . . . ? O1 Cu1 N1 C13 -92.3(3) . . . . ? O1W Cu1 N1 C13 91.9(3) . . . . ? O3 Cu1 N1 C24 -179.2(2) 4_576 . . . ? N2 Cu1 N1 C24 -1.37(19) . . . . ? O1 Cu1 N1 C24 86.8(3) . . . . ? O1W Cu1 N1 C24 -89.0(2) . . . . ? N1 Cu1 N2 C22 -177.2(3) . . . . ? O1 Cu1 N2 C22 34.3(3) . . . . ? O1W Cu1 N2 C22 -61.2(3) . . . . ? N1 Cu1 N2 C23 1.08(19) . . . . ? O1 Cu1 N2 C23 -147.4(2) . . . . ? O1W Cu1 N2 C23 117.1(2) . . . . ? C6 C1 C2 C3 0.2(4) . . . . ? C7 C1 C2 C3 179.3(3) . . . . ? C1 C2 C3 C4 -1.1(4) . . . . ? C1 C2 C3 C8 178.9(3) . . . . ? C2 C3 C4 C5 0.3(5) . . . . ? C8 C3 C4 C5 -179.6(3) . . . . ? C3 C4 C5 C6 1.3(5) . . . . ? C3 C4 C5 C9 -179.1(3) . . . . ? C2 C1 C6 C5 1.5(4) . . . . ? C7 C1 C6 C5 -177.6(3) . . . . ? C4 C5 C6 C1 -2.2(4) . . . . ? C9 C5 C6 C1 178.2(3) . . . . ? Cu1 O1 C7 O2 -11.3(3) . . . . ? Cu1 O1 C7 C1 169.6(2) . . . . ? C6 C1 C7 O2 -10.0(4) . . . . ? C2 C1 C7 O2 170.9(3) . . . . ? C6 C1 C7 O1 169.1(3) . . . . ? C2 C1 C7 O1 -10.0(4) . . . . ? Cu1 O3 C8 O4 28.5(5) 4_575 . . . ? Cu1 O3 C8 C3 -153.2(2) 4_575 . . . ? C4 C3 C8 O4 -164.9(3) . . . . ? C2 C3 C8 O4 15.2(4) . . . . ? C4 C3 C8 O3 16.7(4) . . . . ? C2 C3 C8 O3 -163.2(3) . . . . ? C4 C5 C9 C11 54.7(5) . . . . ? C6 C5 C9 C11 -125.8(4) . . . . ? C4 C5 C9 C10 175.5(3) . . . . ? C6 C5 C9 C10 -5.0(5) . . . . ? C4 C5 C9 C12 -65.4(4) . . . . ? C6 C5 C9 C12 114.2(4) . . . . ? C24 N1 C13 C14 0.4(4) . . . . ? Cu1 N1 C13 C14 179.4(2) . . . . ? N1 C13 C14 C15 -1.1(5) . . . . ? C13 C14 C15 C16 0.9(5) . . . . ? C14 C15 C16 C24 0.1(4) . . . . ? C14 C15 C16 C17 179.4(3) . . . . ? C24 C16 C17 C18 0.4(5) . . . . ? C15 C16 C17 C18 -178.9(3) . . . . ? C16 C17 C18 C19 0.8(5) . . . . ? C17 C18 C19 C23 -2.2(5) . . . . ? C17 C18 C19 C20 178.0(3) . . . . ? C23 C19 C20 C21 -0.8(4) . . . . ? C18 C19 C20 C21 179.1(3) . . . . ? C19 C20 C21 C22 0.2(5) . . . . ? C23 N2 C22 C21 0.8(4) . . . . ? Cu1 N2 C22 C21 179.0(2) . . . . ? C20 C21 C22 N2 -0.2(5) . . . . ? C22 N2 C23 C19 -1.5(4) . . . . ? Cu1 N2 C23 C19 -180.0(2) . . . . ? C22 N2 C23 C24 177.8(2) . . . . ? Cu1 N2 C23 C24 -0.6(3) . . . . ? C20 C19 C23 N2 1.5(4) . . . . ? C18 C19 C23 N2 -178.4(3) . . . . ? C20 C19 C23 C24 -177.8(3) . . . . ? C18 C19 C23 C24 2.3(4) . . . . ? C13 N1 C24 C16 0.6(4) . . . . ? Cu1 N1 C24 C16 -178.6(2) . . . . ? C13 N1 C24 C23 -179.4(3) . . . . ? Cu1 N1 C24 C23 1.4(3) . . . . ? C15 C16 C24 N1 -0.9(4) . . . . ? C17 C16 C24 N1 179.8(3) . . . . ? C15 C16 C24 C23 179.2(3) . . . . ? C17 C16 C24 C23 -0.2(4) . . . . ? N2 C23 C24 N1 -0.5(4) . . . . ? C19 C23 C24 N1 178.8(3) . . . . ? N2 C23 C24 C16 179.4(3) . . . . ? C19 C23 C24 C16 -1.2(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1 O4 0.84 1.99 2.719(3) 144.0 4_576 O1W H2 O1 0.79 2.02 2.807(3) 175.6 3_666 _diffrn_measured_fraction_theta_max 0.893 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.586 _refine_diff_density_min -0.378 _refine_diff_density_rms 0.090 #============================================================================== data_CuPhen1b-[Cu(Htbip)2(phen)]n _database_code_depnum_ccdc_archive 'CCDC 835417' #TrackingRef '- revised cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H34 Cu N2 O8' _chemical_formula_sum 'C36 H34 Cu N2 O8' _chemical_formula_weight 686.19 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 P21/c _symmetry_space_group_name_Hall '-P 2ybc' 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 10.036(2) _cell_length_b 12.322(3) _cell_length_c 25.767(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.06(3) _cell_angle_gamma 90.00 _cell_volume 3181.9(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 16337 _cell_measurement_theta_min 6.01 _cell_measurement_theta_max 54.98 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1428 _exptl_absorpt_coefficient_mu 0.744 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7654 _exptl_absorpt_correction_T_max 0.8359 _exptl_absorpt_process_details 'Tompa_analytical (Rigaku Corporation, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Rigaku R-AXIS RAPID imaging plate' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14071 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0357 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6949 _reflns_number_gt 5466 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'PROCESS-AUTO (Rigaku Corporation,1998)' _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan (Molecular Structure Corporation & Rigaku Corporation, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0996P)^2^+0.6911P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6949 _refine_ls_number_parameters 430 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.1574 _refine_ls_wR_factor_gt 0.1168 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _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 0.63143(3) 0.24546(2) 0.264452(11) 0.02026(12) Uani 1 1 d . . . O1 O 0.60751(18) 0.38445(15) 0.29948(7) 0.0278(4) Uani 1 1 d . . . O2 O 0.70077(19) 0.30390(16) 0.36966(8) 0.0358(5) Uani 1 1 d . . . O3 O 0.64128(18) 0.87245(15) 0.37429(7) 0.0282(4) Uani 1 1 d . . . H3A H 0.6150 0.9302 0.3598 0.042 Uiso 1 1 calc R . . O4 O 0.51476(19) 0.79698(17) 0.31001(7) 0.0317(4) Uani 1 1 d . . . O5 O 0.47398(17) 0.18500(14) 0.29468(7) 0.0245(4) Uani 1 1 d . . . O6 O 0.58984(16) 0.06462(14) 0.34366(7) 0.0246(4) Uani 1 1 d . . . O7 O -0.0929(2) 0.1760(2) 0.38866(9) 0.0538(7) Uani 1 1 d . . . H7A H -0.1549 0.2192 0.3799 0.081 Uiso 1 1 calc R . . O8 O -0.0151(2) 0.2281(2) 0.31360(9) 0.0429(5) Uani 1 1 d . . . N1 N 0.69581(19) 0.10821(17) 0.23139(8) 0.0219(4) Uani 1 1 d . . . N2 N 0.7911(2) 0.30781(19) 0.23037(8) 0.0249(5) Uani 1 1 d . . . C1 C 0.6474(2) 0.4908(2) 0.37485(10) 0.0227(5) Uani 1 1 d . . . C2 C 0.6109(2) 0.5873(2) 0.34978(9) 0.0214(5) Uani 1 1 d . . . H2A H 0.5831 0.5869 0.3140 0.026 Uiso 1 1 calc R . . C3 C 0.6155(2) 0.6844(2) 0.37744(10) 0.0221(5) Uani 1 1 d . . . C4 C 0.6538(2) 0.6852(2) 0.43031(10) 0.0234(5) Uani 1 1 d . . . H4A H 0.6571 0.7521 0.4486 0.028 Uiso 1 1 calc R . . C5 C 0.6876(2) 0.5885(2) 0.45688(10) 0.0227(5) Uani 1 1 d . . . C6 C 0.6847(2) 0.4924(2) 0.42808(10) 0.0232(5) Uani 1 1 d . . . H6A H 0.7088 0.4262 0.4450 0.028 Uiso 1 1 calc R . . C7 C 0.6531(2) 0.3847(2) 0.34654(10) 0.0235(5) Uani 1 1 d . . . C8 C 0.5845(2) 0.7887(2) 0.35002(10) 0.0229(5) Uani 1 1 d . . . C9 C 0.7293(3) 0.5919(2) 0.51487(10) 0.0287(6) Uani 1 1 d . . . C10 C 0.8728(3) 0.6366(3) 0.52049(13) 0.0477(8) Uani 1 1 d . . . H10A H 0.8744 0.7108 0.5068 0.071 Uiso 1 1 calc R . . H10B H 0.9320 0.5906 0.5009 0.071 Uiso 1 1 calc R . . H10C H 0.9032 0.6369 0.5573 0.071 Uiso 1 1 calc R . . C11 C 0.6363(3) 0.6648(3) 0.54452(11) 0.0395(7) Uani 1 1 d . . . H11A H 0.5439 0.6407 0.5380 0.059 Uiso 1 1 calc R . . H11B H 0.6450 0.7400 0.5327 0.059 Uiso 1 1 calc R . . H11C H 0.6604 0.6606 0.5818 0.059 Uiso 1 1 calc R . . C12 C 0.7265(4) 0.4779(3) 0.53913(12) 0.0481(9) Uani 1 1 d . . . H12A H 0.6373 0.4465 0.5331 0.072 Uiso 1 1 calc R . . H12B H 0.7482 0.4830 0.5766 0.072 Uiso 1 1 calc R . . H12C H 0.7922 0.4316 0.5231 0.072 Uiso 1 1 calc R . . C13 C 0.3588(2) 0.0910(2) 0.35863(9) 0.0213(5) Uani 1 1 d . . . C14 C 0.2390(2) 0.1428(2) 0.34371(9) 0.0222(5) Uani 1 1 d . . . H14A H 0.2344 0.1897 0.3144 0.027 Uiso 1 1 calc R . . C15 C 0.1269(2) 0.1254(2) 0.37177(10) 0.0237(5) Uani 1 1 d . . . C16 C 0.1315(2) 0.0544(2) 0.41387(10) 0.0242(5) Uani 1 1 d . . . H16A H 0.0542 0.0443 0.4330 0.029 Uiso 1 1 calc R . . C17 C 0.2487(2) -0.0025(2) 0.42836(9) 0.0225(5) Uani 1 1 d . . . C18 C 0.3615(2) 0.0188(2) 0.40041(9) 0.0229(5) Uani 1 1 d . . . H18A H 0.4428 -0.0170 0.4102 0.027 Uiso 1 1 calc R . . C19 C 0.4843(2) 0.1136(2) 0.33094(9) 0.0217(5) Uani 1 1 d . . . C20 C 0.0000(2) 0.1815(2) 0.35502(10) 0.0266(5) Uani 1 1 d . . . C21 C 0.2512(2) -0.0808(2) 0.47440(10) 0.0267(6) Uani 1 1 d . . . C22 C 0.3773(3) -0.1496(3) 0.47901(15) 0.0508(9) Uani 1 1 d . . . H22A H 0.3840 -0.1932 0.4474 0.076 Uiso 1 1 calc R . . H22B H 0.3737 -0.1979 0.5091 0.076 Uiso 1 1 calc R . . H22C H 0.4555 -0.1022 0.4834 0.076 Uiso 1 1 calc R . . C23 C 0.1311(3) -0.1572(3) 0.47007(12) 0.0394(7) Uani 1 1 d . . . H23A H 0.1350 -0.2009 0.4384 0.059 Uiso 1 1 calc R . . H23B H 0.0486 -0.1145 0.4686 0.059 Uiso 1 1 calc R . . H23C H 0.1329 -0.2052 0.5004 0.059 Uiso 1 1 calc R . . C24 C 0.2438(4) -0.0131(3) 0.52450(12) 0.0446(8) Uani 1 1 d . . . H24A H 0.3207 0.0359 0.5278 0.067 Uiso 1 1 calc R . . H24B H 0.2448 -0.0617 0.5546 0.067 Uiso 1 1 calc R . . H24C H 0.1612 0.0295 0.5229 0.067 Uiso 1 1 calc R . . C25 C 0.6459(2) 0.0083(2) 0.23273(10) 0.0237(5) Uani 1 1 d . . . H25A H 0.5677 -0.0036 0.2512 0.028 Uiso 1 1 calc R . . C26 C 0.7034(3) -0.0797(2) 0.20816(11) 0.0307(6) Uani 1 1 d . . . H26A H 0.6647 -0.1499 0.2100 0.037 Uiso 1 1 calc R . . C27 C 0.8159(3) -0.0639(2) 0.18141(11) 0.0339(6) Uani 1 1 d . . . H27A H 0.8565 -0.1233 0.1649 0.041 Uiso 1 1 calc R . . C28 C 0.8712(2) 0.0405(2) 0.17852(10) 0.0292(6) Uani 1 1 d . . . C29 C 0.9895(3) 0.0662(3) 0.15201(12) 0.0392(7) Uani 1 1 d . . . H29A H 1.0336 0.0105 0.1341 0.047 Uiso 1 1 calc R . . C30 C 1.0392(3) 0.1679(3) 0.15210(12) 0.0406(7) Uani 1 1 d . . . H30A H 1.1174 0.1824 0.1341 0.049 Uiso 1 1 calc R . . C31 C 0.9764(3) 0.2547(2) 0.17887(11) 0.0307(6) Uani 1 1 d . . . C32 C 1.0260(3) 0.3612(3) 0.18337(11) 0.0380(7) Uani 1 1 d . . . H32A H 1.1059 0.3805 0.1675 0.046 Uiso 1 1 calc R . . C33 C 0.9588(3) 0.4370(3) 0.21068(12) 0.0374(7) Uani 1 1 d . . . H33A H 0.9921 0.5090 0.2142 0.045 Uiso 1 1 calc R . . C34 C 0.8401(3) 0.4072(2) 0.23354(10) 0.0300(6) Uani 1 1 d . . . H34A H 0.7933 0.4606 0.2520 0.036 Uiso 1 1 calc R . . C35 C 0.8591(2) 0.2322(2) 0.20413(10) 0.0245(5) Uani 1 1 d . . . C36 C 0.8072(2) 0.1249(2) 0.20424(9) 0.0227(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02560(19) 0.01410(18) 0.02137(19) -0.00083(10) 0.00380(13) -0.00017(11) O1 0.0399(10) 0.0170(9) 0.0265(9) -0.0044(7) 0.0008(8) 0.0015(8) O2 0.0385(10) 0.0233(11) 0.0443(12) -0.0073(9) -0.0085(9) 0.0121(8) O3 0.0371(9) 0.0162(9) 0.0302(10) -0.0011(7) -0.0077(8) 0.0013(7) O4 0.0400(10) 0.0275(11) 0.0265(10) -0.0018(8) -0.0080(8) 0.0010(8) O5 0.0301(8) 0.0171(9) 0.0266(9) 0.0062(7) 0.0059(7) 0.0018(7) O6 0.0274(8) 0.0181(9) 0.0287(9) 0.0037(7) 0.0050(7) 0.0006(7) O7 0.0368(11) 0.0760(19) 0.0500(14) 0.0351(13) 0.0148(10) 0.0312(12) O8 0.0344(11) 0.0536(14) 0.0404(13) 0.0208(11) -0.0009(9) 0.0076(10) N1 0.0244(9) 0.0207(11) 0.0206(10) 0.0000(8) 0.0018(8) 0.0024(8) N2 0.0235(9) 0.0256(12) 0.0251(11) 0.0024(9) -0.0029(8) -0.0028(8) C1 0.0193(10) 0.0181(12) 0.0305(13) -0.0051(10) 0.0009(9) 0.0008(9) C2 0.0204(10) 0.0207(12) 0.0229(12) -0.0019(9) 0.0006(9) 0.0002(9) C3 0.0211(10) 0.0207(13) 0.0244(12) 0.0005(10) 0.0012(9) 0.0035(9) C4 0.0229(11) 0.0203(13) 0.0271(12) -0.0019(10) 0.0013(9) 0.0023(9) C5 0.0220(11) 0.0208(12) 0.0251(12) -0.0014(10) -0.0007(9) -0.0004(9) C6 0.0248(11) 0.0176(12) 0.0273(13) -0.0006(9) 0.0006(10) 0.0023(9) C7 0.0192(10) 0.0191(12) 0.0323(13) -0.0030(10) 0.0025(9) 0.0004(9) C8 0.0241(11) 0.0199(12) 0.0250(12) -0.0046(10) 0.0044(10) 0.0018(10) C9 0.0343(13) 0.0235(14) 0.0275(13) 0.0003(10) -0.0045(10) 0.0014(11) C10 0.0359(15) 0.057(2) 0.0482(19) -0.0106(16) -0.0136(14) -0.0021(15) C11 0.0484(16) 0.0444(19) 0.0254(14) -0.0038(12) -0.0005(12) 0.0098(14) C12 0.087(2) 0.0270(16) 0.0280(15) 0.0016(12) -0.0149(16) 0.0014(16) C13 0.0269(11) 0.0162(12) 0.0208(11) 0.0003(9) 0.0026(9) -0.0003(9) C14 0.0295(12) 0.0172(12) 0.0199(11) 0.0030(9) 0.0005(9) -0.0003(10) C15 0.0264(11) 0.0194(12) 0.0249(12) 0.0024(10) -0.0028(9) 0.0019(10) C16 0.0255(11) 0.0232(13) 0.0241(12) 0.0045(10) 0.0057(9) 0.0014(10) C17 0.0260(11) 0.0217(12) 0.0199(12) 0.0033(9) 0.0021(9) 0.0017(10) C18 0.0249(11) 0.0221(13) 0.0219(12) 0.0008(10) 0.0033(9) 0.0013(10) C19 0.0294(12) 0.0132(11) 0.0226(12) -0.0012(9) 0.0032(9) -0.0027(9) C20 0.0259(11) 0.0236(13) 0.0301(13) 0.0061(11) -0.0012(10) 0.0004(10) C21 0.0223(11) 0.0311(15) 0.0270(13) 0.0088(11) 0.0044(9) 0.0021(10) C22 0.0380(16) 0.055(2) 0.061(2) 0.0355(18) 0.0154(15) 0.0145(15) C23 0.0410(15) 0.0339(16) 0.0421(17) 0.0155(13) -0.0073(13) -0.0089(13) C24 0.0563(18) 0.050(2) 0.0277(15) 0.0081(13) 0.0006(13) -0.0067(16) C25 0.0287(12) 0.0200(12) 0.0226(12) -0.0027(9) 0.0011(10) -0.0029(10) C26 0.0342(13) 0.0231(13) 0.0344(14) -0.0066(11) -0.0025(11) 0.0021(11) C27 0.0372(14) 0.0293(15) 0.0350(15) -0.0077(12) 0.0015(12) 0.0130(12) C28 0.0248(12) 0.0342(15) 0.0284(13) -0.0036(11) -0.0006(10) 0.0072(11) C29 0.0268(13) 0.053(2) 0.0386(16) -0.0044(14) 0.0078(12) 0.0091(13) C30 0.0238(12) 0.059(2) 0.0399(17) 0.0033(15) 0.0101(12) 0.0010(13) C31 0.0265(13) 0.0390(17) 0.0263(14) 0.0067(11) -0.0009(11) -0.0042(11) C32 0.0285(13) 0.052(2) 0.0334(15) 0.0093(14) -0.0012(11) -0.0129(13) C33 0.0378(14) 0.0370(17) 0.0362(15) 0.0103(13) -0.0084(12) -0.0176(13) C34 0.0379(13) 0.0212(13) 0.0298(14) 0.0039(10) -0.0065(11) -0.0084(11) C35 0.0201(11) 0.0316(14) 0.0214(12) 0.0024(10) -0.0014(9) -0.0001(10) C36 0.0225(10) 0.0270(13) 0.0182(11) -0.0002(10) -0.0024(9) 0.0022(10) _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 O5 1.9469(18) . ? Cu1 O1 1.9567(18) . ? Cu1 N1 2.015(2) . ? Cu1 N2 2.020(2) . ? Cu1 O4 2.4364(19) 2_645 ? O1 C7 1.273(3) . ? O2 C7 1.243(3) . ? O3 C8 1.320(3) . ? O3 H3A 0.8400 . ? O4 C8 1.219(3) . ? O4 Cu1 2.4364(19) 2_655 ? O5 C19 1.284(3) . ? O6 C19 1.248(3) . ? O7 C20 1.309(3) . ? O7 H7A 0.8400 . ? O8 C20 1.214(3) . ? N1 C25 1.330(3) . ? N1 C36 1.366(3) . ? N2 C34 1.321(3) . ? N2 C35 1.357(4) . ? C1 C2 1.393(4) . ? C1 C6 1.403(3) . ? C1 C7 1.499(3) . ? C2 C3 1.392(4) . ? C2 H2A 0.9500 . ? C3 C4 1.396(3) . ? C3 C8 1.492(4) . ? C4 C5 1.407(4) . ? C4 H4A 0.9500 . ? C5 C6 1.397(4) . ? C5 C9 1.531(3) . ? C6 H6A 0.9500 . ? C9 C11 1.530(4) . ? C9 C12 1.538(4) . ? C9 C10 1.541(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C18 1.395(3) . ? C13 C14 1.396(3) . ? C13 C19 1.507(3) . ? C14 C15 1.386(3) . ? C14 H14A 0.9500 . ? C15 C16 1.393(4) . ? C15 C20 1.493(3) . ? C16 C17 1.402(3) . ? C16 H16A 0.9500 . ? C17 C18 1.399(3) . ? C17 C21 1.528(3) . ? C18 H18A 0.9500 . ? C21 C22 1.523(4) . ? C21 C23 1.529(4) . ? C21 C24 1.542(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.396(4) . ? C25 H25A 0.9500 . ? C26 C27 1.368(4) . ? C26 H26A 0.9500 . ? C27 C28 1.404(4) . ? C27 H27A 0.9500 . ? C28 C36 1.406(4) . ? C28 C29 1.436(4) . ? C29 C30 1.349(5) . ? C29 H29A 0.9500 . ? C30 C31 1.437(5) . ? C30 H30A 0.9500 . ? C31 C35 1.404(4) . ? C31 C32 1.406(4) . ? C32 C33 1.369(5) . ? C32 H32A 0.9500 . ? C33 C34 1.406(4) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? C35 C36 1.421(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 O5 Cu1 O1 91.62(8) . . ? O5 Cu1 N1 97.66(8) . . ? O1 Cu1 N1 168.36(8) . . ? O5 Cu1 N2 177.80(8) . . ? O1 Cu1 N2 89.28(9) . . ? N1 Cu1 N2 81.70(9) . . ? O5 Cu1 O4 86.98(7) . 2_645 ? O1 Cu1 O4 92.96(7) . 2_645 ? N1 Cu1 O4 94.53(8) . 2_645 ? N2 Cu1 O4 90.96(8) . 2_645 ? C7 O1 Cu1 113.26(16) . . ? C8 O3 H3A 109.5 . . ? C8 O4 Cu1 159.83(18) . 2_655 ? C19 O5 Cu1 121.20(16) . . ? C20 O7 H7A 109.5 . . ? C25 N1 C36 118.2(2) . . ? C25 N1 Cu1 129.48(17) . . ? C36 N1 Cu1 112.35(17) . . ? C34 N2 C35 118.2(2) . . ? C34 N2 Cu1 128.8(2) . . ? C35 N2 Cu1 112.77(18) . . ? C2 C1 C6 119.4(2) . . ? C2 C1 C7 122.3(2) . . ? C6 C1 C7 118.2(2) . . ? C3 C2 C1 119.7(2) . . ? C3 C2 H2A 120.1 . . ? C1 C2 H2A 120.1 . . ? C2 C3 C4 120.4(2) . . ? C2 C3 C8 119.9(2) . . ? C4 C3 C8 119.7(2) . . ? C3 C4 C5 121.0(2) . . ? C3 C4 H4A 119.5 . . ? C5 C4 H4A 119.5 . . ? C6 C5 C4 117.5(2) . . ? C6 C5 C9 122.6(2) . . ? C4 C5 C9 119.9(2) . . ? C5 C6 C1 121.9(2) . . ? C5 C6 H6A 119.0 . . ? C1 C6 H6A 119.0 . . ? O2 C7 O1 124.3(2) . . ? O2 C7 C1 119.3(2) . . ? O1 C7 C1 116.4(2) . . ? O4 C8 O3 123.3(2) . . ? O4 C8 C3 124.6(2) . . ? O3 C8 C3 112.0(2) . . ? C11 C9 C5 111.1(2) . . ? C11 C9 C12 108.0(3) . . ? C5 C9 C12 111.2(2) . . ? C11 C9 C10 109.5(3) . . ? C5 C9 C10 107.9(2) . . ? C12 C9 C10 109.0(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 119.0(2) . . ? C18 C13 C19 120.0(2) . . ? C14 C13 C19 120.9(2) . . ? C15 C14 C13 119.8(2) . . ? C15 C14 H14A 120.1 . . ? C13 C14 H14A 120.1 . . ? C14 C15 C16 120.6(2) . . ? C14 C15 C20 118.8(2) . . ? C16 C15 C20 120.6(2) . . ? C15 C16 C17 120.9(2) . . ? C15 C16 H16A 119.5 . . ? C17 C16 H16A 119.5 . . ? C18 C17 C16 117.3(2) . . ? C18 C17 C21 122.5(2) . . ? C16 C17 C21 120.1(2) . . ? C13 C18 C17 122.2(2) . . ? C13 C18 H18A 118.9 . . ? C17 C18 H18A 118.9 . . ? O6 C19 O5 123.9(2) . . ? O6 C19 C13 120.4(2) . . ? O5 C19 C13 115.8(2) . . ? O8 C20 O7 123.1(2) . . ? O8 C20 C15 122.6(2) . . ? O7 C20 C15 114.3(2) . . ? C22 C21 C17 113.1(2) . . ? C22 C21 C23 108.1(3) . . ? C17 C21 C23 110.6(2) . . ? C22 C21 C24 108.2(3) . . ? C17 C21 C24 108.0(2) . . ? C23 C21 C24 108.7(2) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N1 C25 C26 122.8(2) . . ? N1 C25 H25A 118.6 . . ? C26 C25 H25A 118.6 . . ? C27 C26 C25 119.3(3) . . ? C27 C26 H26A 120.3 . . ? C25 C26 H26A 120.3 . . ? C26 C27 C28 119.7(3) . . ? C26 C27 H27A 120.1 . . ? C28 C27 H27A 120.1 . . ? C27 C28 C36 117.4(2) . . ? C27 C28 C29 124.4(3) . . ? C36 C28 C29 118.1(3) . . ? C30 C29 C28 121.3(3) . . ? C30 C29 H29A 119.4 . . ? C28 C29 H29A 119.4 . . ? C29 C30 C31 121.4(3) . . ? C29 C30 H30A 119.3 . . ? C31 C30 H30A 119.3 . . ? C35 C31 C32 116.7(3) . . ? C35 C31 C30 118.4(3) . . ? C32 C31 C30 124.9(3) . . ? C33 C32 C31 119.9(3) . . ? C33 C32 H32A 120.1 . . ? C31 C32 H32A 120.1 . . ? C32 C33 C34 119.3(3) . . ? C32 C33 H33A 120.4 . . ? C34 C33 H33A 120.4 . . ? N2 C34 C33 122.5(3) . . ? N2 C34 H34A 118.7 . . ? C33 C34 H34A 118.7 . . ? N2 C35 C31 123.5(3) . . ? N2 C35 C36 116.4(2) . . ? C31 C35 C36 120.1(2) . . ? N1 C36 C28 122.5(2) . . ? N1 C36 C35 116.8(2) . . ? C28 C36 C35 120.7(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Cu1 O1 C7 81.66(17) . . . . ? N1 Cu1 O1 C7 -61.3(4) . . . . ? N2 Cu1 O1 C7 -100.36(17) . . . . ? O4 Cu1 O1 C7 168.71(17) 2_645 . . . ? O1 Cu1 O5 C19 -107.48(19) . . . . ? N1 Cu1 O5 C19 65.47(19) . . . . ? O4 Cu1 O5 C19 159.64(19) 2_645 . . . ? O5 Cu1 N1 C25 -2.4(2) . . . . ? O1 Cu1 N1 C25 140.2(4) . . . . ? N2 Cu1 N1 C25 179.7(2) . . . . ? O4 Cu1 N1 C25 -90.0(2) 2_645 . . . ? O5 Cu1 N1 C36 177.71(15) . . . . ? O1 Cu1 N1 C36 -39.7(5) . . . . ? N2 Cu1 N1 C36 -0.16(16) . . . . ? O4 Cu1 N1 C36 90.16(16) 2_645 . . . ? O1 Cu1 N2 C34 -2.7(2) . . . . ? N1 Cu1 N2 C34 -175.3(2) . . . . ? O4 Cu1 N2 C34 90.2(2) 2_645 . . . ? O1 Cu1 N2 C35 172.22(17) . . . . ? N1 Cu1 N2 C35 -0.40(17) . . . . ? O4 Cu1 N2 C35 -94.84(17) 2_645 . . . ? C6 C1 C2 C3 1.8(3) . . . . ? C7 C1 C2 C3 -176.0(2) . . . . ? C1 C2 C3 C4 -1.3(3) . . . . ? C1 C2 C3 C8 176.3(2) . . . . ? C2 C3 C4 C5 -0.4(4) . . . . ? C8 C3 C4 C5 -178.1(2) . . . . ? C3 C4 C5 C6 1.6(3) . . . . ? C3 C4 C5 C9 179.9(2) . . . . ? C4 C5 C6 C1 -1.2(4) . . . . ? C9 C5 C6 C1 -179.4(2) . . . . ? C2 C1 C6 C5 -0.5(4) . . . . ? C7 C1 C6 C5 177.3(2) . . . . ? Cu1 O1 C7 O2 -4.3(3) . . . . ? Cu1 O1 C7 C1 175.74(16) . . . . ? C2 C1 C7 O2 171.8(2) . . . . ? C6 C1 C7 O2 -5.9(3) . . . . ? C2 C1 C7 O1 -8.2(3) . . . . ? C6 C1 C7 O1 174.1(2) . . . . ? Cu1 O4 C8 O3 -176.8(4) 2_655 . . . ? Cu1 O4 C8 C3 3.0(7) 2_655 . . . ? C2 C3 C8 O4 25.1(4) . . . . ? C4 C3 C8 O4 -157.3(2) . . . . ? C2 C3 C8 O3 -155.1(2) . . . . ? C4 C3 C8 O3 22.6(3) . . . . ? C6 C5 C9 C11 -136.9(3) . . . . ? C4 C5 C9 C11 44.9(3) . . . . ? C6 C5 C9 C12 -16.5(4) . . . . ? C4 C5 C9 C12 165.3(3) . . . . ? C6 C5 C9 C10 103.0(3) . . . . ? C4 C5 C9 C10 -75.2(3) . . . . ? C18 C13 C14 C15 2.7(4) . . . . ? C19 C13 C14 C15 -176.2(2) . . . . ? C13 C14 C15 C16 -1.8(4) . . . . ? C13 C14 C15 C20 -179.9(2) . . . . ? C14 C15 C16 C17 -1.0(4) . . . . ? C20 C15 C16 C17 177.0(2) . . . . ? C15 C16 C17 C18 2.9(4) . . . . ? C15 C16 C17 C21 -179.5(2) . . . . ? C14 C13 C18 C17 -0.8(4) . . . . ? C19 C13 C18 C17 178.1(2) . . . . ? C16 C17 C18 C13 -2.0(4) . . . . ? C21 C17 C18 C13 -179.5(2) . . . . ? Cu1 O5 C19 O6 -12.2(3) . . . . ? Cu1 O5 C19 C13 167.54(15) . . . . ? C18 C13 C19 O6 3.1(4) . . . . ? C14 C13 C19 O6 -178.0(2) . . . . ? C18 C13 C19 O5 -176.7(2) . . . . ? C14 C13 C19 O5 2.2(3) . . . . ? C14 C15 C20 O8 11.6(4) . . . . ? C16 C15 C20 O8 -166.4(3) . . . . ? C14 C15 C20 O7 -168.4(3) . . . . ? C16 C15 C20 O7 13.5(4) . . . . ? C18 C17 C21 C22 -12.4(4) . . . . ? C16 C17 C21 C22 170.1(3) . . . . ? C18 C17 C21 C23 -133.8(3) . . . . ? C16 C17 C21 C23 48.8(3) . . . . ? C18 C17 C21 C24 107.4(3) . . . . ? C16 C17 C21 C24 -70.1(3) . . . . ? C36 N1 C25 C26 0.8(4) . . . . ? Cu1 N1 C25 C26 -179.11(19) . . . . ? N1 C25 C26 C27 0.0(4) . . . . ? C25 C26 C27 C28 -0.7(4) . . . . ? C26 C27 C28 C36 0.6(4) . . . . ? C26 C27 C28 C29 179.3(3) . . . . ? C27 C28 C29 C30 -178.0(3) . . . . ? C36 C28 C29 C30 0.7(4) . . . . ? C28 C29 C30 C31 0.3(5) . . . . ? C29 C30 C31 C35 -1.6(4) . . . . ? C29 C30 C31 C32 176.1(3) . . . . ? C35 C31 C32 C33 -1.0(4) . . . . ? C30 C31 C32 C33 -178.8(3) . . . . ? C31 C32 C33 C34 -0.5(4) . . . . ? C35 N2 C34 C33 0.3(4) . . . . ? Cu1 N2 C34 C33 174.97(19) . . . . ? C32 C33 C34 N2 1.0(4) . . . . ? C34 N2 C35 C31 -2.0(4) . . . . ? Cu1 N2 C35 C31 -177.5(2) . . . . ? C34 N2 C35 C36 176.4(2) . . . . ? Cu1 N2 C35 C36 0.9(3) . . . . ? C32 C31 C35 N2 2.4(4) . . . . ? C30 C31 C35 N2 -179.7(2) . . . . ? C32 C31 C35 C36 -176.0(2) . . . . ? C30 C31 C35 C36 1.9(4) . . . . ? C25 N1 C36 C28 -0.9(3) . . . . ? Cu1 N1 C36 C28 179.05(19) . . . . ? C25 N1 C36 C35 -179.2(2) . . . . ? Cu1 N1 C36 C35 0.7(3) . . . . ? C27 C28 C36 N1 0.2(4) . . . . ? C29 C28 C36 N1 -178.6(2) . . . . ? C27 C28 C36 C35 178.5(2) . . . . ? C29 C28 C36 C35 -0.3(4) . . . . ? N2 C35 C36 N1 -1.1(3) . . . . ? C31 C35 C36 N1 177.4(2) . . . . ? N2 C35 C36 C28 -179.5(2) . . . . ? C31 C35 C36 C28 -1.0(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3A O6 0.84 1.72 2.540(3) 163.8 1_565 O7 H7A O2 0.84 1.79 2.627(3) 171.4 1_455 _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.540 _refine_diff_density_min -0.819 _refine_diff_density_rms 0.103 #============================================================================== data_CuPhen1c-[Cu(tbip)(H2tbip)(phen)]n _database_code_depnum_ccdc_archive 'CCDC 835418' #TrackingRef '- revised cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H34 Cu N2 O8' _chemical_formula_sum 'C36 H34 Cu N2 O8' _chemical_formula_weight 686.19 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 P21 _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.988(2) _cell_length_b 14.253(3) _cell_length_c 11.358(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.93(3) _cell_angle_gamma 90.00 _cell_volume 1682.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11090 _cell_measurement_theta_min 6.28 _cell_measurement_theta_max 54.94 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 714 _exptl_absorpt_coefficient_mu 0.703 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7615 _exptl_absorpt_correction_T_max 0.8329 _exptl_absorpt_process_details 'Tompa_analytical (Rigaku Corporation, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Rigaku R-AXIS RAPID imaging plate' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16396 _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.0878 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7599 _reflns_number_gt 6200 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'PROCESS-AUTO (Rigaku Corporation,1998)' _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan (Molecular Structure Corporation & Rigaku Corporation, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.005(11) _refine_ls_number_reflns 7599 _refine_ls_number_parameters 430 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0593 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1102 _refine_ls_wR_factor_gt 0.0919 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.11872(3) 0.71205(3) 0.36524(3) 0.02395(10) Uani 1 1 d . . . O1 O 0.00734(18) 0.62492(16) 0.24442(19) 0.0278(5) Uani 1 1 d . . . O2 O 0.11978(19) 0.61831(18) 0.1104(2) 0.0322(5) Uani 1 1 d . . . O3 O 0.04875(19) 0.32435(18) -0.1194(2) 0.0376(6) Uani 1 1 d . . . O4 O -0.15110(19) 0.29989(16) -0.25035(19) 0.0283(5) Uani 1 1 d . . . O5 O 0.31842(19) 0.64499(17) 0.3969(2) 0.0321(5) Uani 1 1 d . . . O6 O 0.3523(2) 0.66321(19) 0.2146(2) 0.0404(6) Uani 1 1 d . . . H6B H 0.2744 0.6480 0.1860 0.061 Uiso 1 1 calc R . . O7 O 0.77957(19) 0.76276(18) 0.2083(2) 0.0357(6) Uani 1 1 d . . . H7A H 0.8353 0.7827 0.1784 0.053 Uiso 1 1 calc R . . O8 O 0.93276(18) 0.79200(18) 0.3899(2) 0.0324(5) Uani 1 1 d . . . N1 N 0.2022(2) 0.8071(2) 0.5037(2) 0.0271(6) Uani 1 1 d . . . N2 N 0.1048(2) 0.63783(19) 0.5118(2) 0.0260(6) Uani 1 1 d . . . C1 C -0.0780(3) 0.5406(2) 0.0532(3) 0.0254(7) Uani 1 1 d . . . C2 C -0.0355(3) 0.4716(2) -0.0090(3) 0.0261(7) Uani 1 1 d . . . H2A H 0.0542 0.4634 0.0070 0.031 Uiso 1 1 calc R . . C3 C -0.1222(3) 0.4138(2) -0.0950(3) 0.0257(7) Uani 1 1 d . . . C4 C -0.2522(3) 0.4280(2) -0.1199(3) 0.0257(7) Uani 1 1 d . . . H4A H -0.3113 0.3894 -0.1799 0.031 Uiso 1 1 calc R . . C5 C -0.3003(3) 0.4979(2) -0.0594(3) 0.0271(7) Uani 1 1 d . . . C6 C -0.2103(3) 0.5533(2) 0.0296(3) 0.0252(7) Uani 1 1 d . . . H6A H -0.2394 0.5997 0.0741 0.030 Uiso 1 1 calc R . . C7 C 0.0238(3) 0.6003(2) 0.1427(3) 0.0250(7) Uani 1 1 d . . . C8 C -0.0698(3) 0.3401(2) -0.1593(3) 0.0254(7) Uani 1 1 d . . . C9 C -0.4458(3) 0.5090(3) -0.0910(3) 0.0370(8) Uani 1 1 d . . . C10 C -0.4825(3) 0.5916(3) -0.0233(4) 0.0509(11) Uani 1 1 d . . . H10A H -0.4485 0.5810 0.0668 0.076 Uiso 1 1 calc R . . H10B H -0.5764 0.5971 -0.0492 0.076 Uiso 1 1 calc R . . H10C H -0.4460 0.6496 -0.0440 0.076 Uiso 1 1 calc R . . C11 C -0.5023(3) 0.4184(3) -0.0545(4) 0.0536(11) Uani 1 1 d . . . H11A H -0.4672 0.4095 0.0359 0.080 Uiso 1 1 calc R . . H11B H -0.4793 0.3645 -0.0965 0.080 Uiso 1 1 calc R . . H11C H -0.5962 0.4238 -0.0795 0.080 Uiso 1 1 calc R . . C12 C -0.5099(4) 0.5242(4) -0.2331(4) 0.0570(13) Uani 1 1 d . . . H12A H -0.4731 0.5800 -0.2590 0.085 Uiso 1 1 calc R . . H12B H -0.6028 0.5330 -0.2519 0.085 Uiso 1 1 calc R . . H12C H -0.4945 0.4693 -0.2781 0.085 Uiso 1 1 calc R . . C13 C 0.5162(2) 0.7079(3) 0.3956(3) 0.0280(6) Uani 1 1 d . . . C14 C 0.6028(2) 0.7210(3) 0.3309(3) 0.0282(7) Uani 1 1 d . . . H14A H 0.5797 0.7045 0.2454 0.034 Uiso 1 1 calc R . . C15 C 0.7224(3) 0.7581(2) 0.3920(3) 0.0292(7) Uani 1 1 d . . . C16 C 0.7559(3) 0.7835(3) 0.5170(3) 0.0324(8) Uani 1 1 d . . . H16A H 0.8396 0.8076 0.5579 0.039 Uiso 1 1 calc R . . C17 C 0.6707(3) 0.7748(3) 0.5836(3) 0.0313(7) Uani 1 1 d . . . C18 C 0.5503(3) 0.7350(2) 0.5202(3) 0.0323(8) Uani 1 1 d . . . H18A H 0.4902 0.7263 0.5634 0.039 Uiso 1 1 calc R . . C19 C 0.3869(3) 0.6688(2) 0.3366(3) 0.0308(7) Uani 1 1 d . . . C20 C 0.8224(3) 0.7719(2) 0.3304(3) 0.0296(7) Uani 1 1 d . . . C21 C 0.7085(3) 0.8096(3) 0.7190(3) 0.0398(9) Uani 1 1 d . . . C22 C 0.5959(4) 0.8071(5) 0.7678(4) 0.085(2) Uani 1 1 d . . . H22A H 0.6238 0.8289 0.8543 0.127 Uiso 1 1 calc R . . H22B H 0.5637 0.7426 0.7640 0.127 Uiso 1 1 calc R . . H22C H 0.5273 0.8479 0.7168 0.127 Uiso 1 1 calc R . . C23 C 0.7532(6) 0.9106(4) 0.7248(5) 0.093(2) Uani 1 1 d . . . H23A H 0.8413 0.9124 0.7219 0.140 Uiso 1 1 calc R . . H23B H 0.7509 0.9393 0.8024 0.140 Uiso 1 1 calc R . . H23C H 0.6962 0.9453 0.6538 0.140 Uiso 1 1 calc R . . C24 C 0.8139(5) 0.7477(5) 0.7995(4) 0.088(2) Uani 1 1 d . . . H24A H 0.8892 0.7517 0.7715 0.131 Uiso 1 1 calc R . . H24B H 0.7836 0.6826 0.7930 0.131 Uiso 1 1 calc R . . H24C H 0.8374 0.7684 0.8862 0.131 Uiso 1 1 calc R . . C25 C 0.2474(3) 0.8919(3) 0.4952(3) 0.0334(8) Uani 1 1 d . . . H25A H 0.2597 0.9096 0.4192 0.040 Uiso 1 1 calc R . . C26 C 0.2780(4) 0.9565(3) 0.5926(4) 0.0444(9) Uani 1 1 d . . . H26A H 0.3098 1.0169 0.5828 0.053 Uiso 1 1 calc R . . C27 C 0.2613(4) 0.9311(3) 0.7031(4) 0.0462(10) Uani 1 1 d . . . H27A H 0.2795 0.9748 0.7697 0.055 Uiso 1 1 calc R . . C28 C 0.2173(3) 0.8406(3) 0.7176(3) 0.0381(8) Uani 1 1 d . . . C29 C 0.2011(3) 0.8060(3) 0.8301(3) 0.0476(10) Uani 1 1 d . . . H29A H 0.2196 0.8460 0.9006 0.057 Uiso 1 1 calc R . . C30 C 0.1600(3) 0.7174(4) 0.8375(3) 0.0475(9) Uani 1 1 d . . . H30A H 0.1526 0.6953 0.9138 0.057 Uiso 1 1 calc R . . C31 C 0.1274(3) 0.6561(3) 0.7310(3) 0.0342(8) Uani 1 1 d . . . C32 C 0.0803(4) 0.5640(3) 0.7298(4) 0.0484(10) Uani 1 1 d . . . H32A H 0.0704 0.5379 0.8032 0.058 Uiso 1 1 calc R . . C33 C 0.0492(4) 0.5125(3) 0.6232(4) 0.0450(10) Uani 1 1 d . . . H33A H 0.0195 0.4498 0.6224 0.054 Uiso 1 1 calc R . . C34 C 0.0610(3) 0.5520(3) 0.5152(3) 0.0357(8) Uani 1 1 d . . . H34A H 0.0366 0.5157 0.4410 0.043 Uiso 1 1 calc R . . C35 C 0.1387(3) 0.6888(2) 0.6182(3) 0.0272(7) Uani 1 1 d . . . C36 C 0.1878(3) 0.7814(2) 0.6140(3) 0.0274(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02479(17) 0.02264(19) 0.02417(17) -0.00054(18) 0.00760(13) -0.00372(17) O1 0.0266(10) 0.0288(13) 0.0292(11) -0.0010(10) 0.0106(9) -0.0035(10) O2 0.0237(10) 0.0424(15) 0.0292(12) -0.0092(11) 0.0068(9) -0.0081(11) O3 0.0254(11) 0.0462(16) 0.0398(14) -0.0137(12) 0.0085(10) 0.0010(11) O4 0.0273(10) 0.0300(13) 0.0257(11) -0.0048(10) 0.0061(9) 0.0010(10) O5 0.0257(10) 0.0333(14) 0.0411(13) 0.0001(11) 0.0158(10) -0.0032(10) O6 0.0277(11) 0.0575(17) 0.0383(13) -0.0115(12) 0.0137(10) -0.0148(12) O7 0.0254(10) 0.0448(15) 0.0381(13) 0.0003(11) 0.0122(10) -0.0057(11) O8 0.0186(10) 0.0378(14) 0.0399(13) -0.0010(11) 0.0084(9) -0.0048(10) N1 0.0174(11) 0.0272(15) 0.0307(14) -0.0008(12) -0.0007(10) -0.0010(11) N2 0.0270(12) 0.0223(14) 0.0281(14) 0.0010(11) 0.0080(11) -0.0003(11) C1 0.0252(14) 0.0267(17) 0.0241(15) -0.0018(14) 0.0079(12) -0.0035(13) C2 0.0279(16) 0.0272(17) 0.0248(15) -0.0033(13) 0.0109(14) -0.0036(15) C3 0.0284(15) 0.0275(18) 0.0234(15) -0.0007(13) 0.0114(13) -0.0022(14) C4 0.0244(14) 0.0252(17) 0.0249(15) -0.0035(13) 0.0045(12) -0.0044(13) C5 0.0261(15) 0.0288(18) 0.0267(16) -0.0003(14) 0.0091(13) -0.0012(14) C6 0.0291(15) 0.0213(16) 0.0278(16) 0.0007(13) 0.0130(13) 0.0017(13) C7 0.0248(15) 0.0237(18) 0.0257(16) -0.0014(14) 0.0072(13) -0.0025(14) C8 0.0264(15) 0.0255(18) 0.0248(16) -0.0029(14) 0.0092(13) -0.0031(14) C9 0.0253(16) 0.042(2) 0.041(2) -0.0117(17) 0.0083(15) 0.0011(16) C10 0.0332(18) 0.059(3) 0.059(3) -0.018(2) 0.0127(17) 0.012(2) C11 0.0279(17) 0.062(3) 0.072(3) -0.012(2) 0.0175(19) -0.0110(19) C12 0.039(2) 0.076(3) 0.044(2) -0.010(2) -0.0035(18) 0.014(2) C13 0.0219(12) 0.0252(15) 0.0351(15) 0.0011(18) 0.0067(11) -0.0007(17) C14 0.0212(12) 0.0311(19) 0.0328(14) -0.0006(18) 0.0095(11) 0.0001(15) C15 0.0222(14) 0.0296(18) 0.0340(17) -0.0026(15) 0.0067(13) -0.0005(14) C16 0.0211(14) 0.032(2) 0.0403(19) -0.0016(15) 0.0044(13) -0.0047(14) C17 0.0270(14) 0.0320(19) 0.0326(17) -0.0061(15) 0.0066(13) -0.0013(14) C18 0.0266(14) 0.035(2) 0.0380(17) -0.0024(14) 0.0138(13) -0.0015(14) C19 0.0313(16) 0.0286(18) 0.0345(18) -0.0002(14) 0.0133(14) 0.0047(14) C20 0.0264(15) 0.0235(17) 0.0399(19) 0.0020(15) 0.0124(14) 0.0009(14) C21 0.0324(17) 0.050(2) 0.0333(18) -0.0100(17) 0.0049(15) -0.0052(17) C22 0.059(3) 0.156(6) 0.047(3) -0.045(3) 0.027(2) -0.022(3) C23 0.156(6) 0.060(4) 0.056(3) -0.023(3) 0.023(3) -0.035(4) C24 0.093(4) 0.126(6) 0.035(2) 0.000(3) 0.010(2) 0.037(4) C25 0.0329(17) 0.0270(19) 0.0377(18) -0.0042(15) 0.0078(15) -0.0070(15) C26 0.047(2) 0.028(2) 0.055(2) -0.0084(18) 0.0123(18) -0.0093(17) C27 0.049(2) 0.040(2) 0.048(2) -0.020(2) 0.0140(19) -0.009(2) C28 0.0335(17) 0.044(2) 0.0368(19) -0.0121(17) 0.0119(15) -0.0015(17) C29 0.044(2) 0.067(3) 0.0334(19) -0.016(2) 0.0141(17) -0.005(2) C30 0.0452(18) 0.072(3) 0.0277(16) -0.004(2) 0.0146(14) -0.001(3) C31 0.0275(15) 0.046(2) 0.0282(17) 0.0073(15) 0.0083(13) 0.0013(16) C32 0.050(2) 0.052(3) 0.048(2) 0.017(2) 0.0228(19) -0.001(2) C33 0.050(2) 0.031(2) 0.058(2) 0.0149(19) 0.022(2) -0.0025(19) C34 0.0384(18) 0.0263(19) 0.0400(19) -0.0018(16) 0.0095(16) -0.0038(16) C35 0.0241(13) 0.030(2) 0.0263(15) 0.0018(13) 0.0066(12) 0.0027(13) C36 0.0255(15) 0.0273(18) 0.0302(17) -0.0014(14) 0.0101(13) 0.0018(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 O4 1.923(2) 2 ? Cu1 O1 1.958(2) . ? Cu1 N2 2.019(3) . ? Cu1 N1 2.053(3) . ? Cu1 O5 2.312(2) . ? Cu1 O8 2.434(2) 1_455 ? O1 C7 1.275(4) . ? O2 C7 1.251(4) . ? O3 C8 1.253(4) . ? O4 C8 1.263(4) . ? O4 Cu1 1.923(2) 2_545 ? O5 C19 1.219(4) . ? O6 C19 1.314(4) . ? O6 H6B 0.8400 . ? O7 C20 1.318(4) . ? O7 H7A 0.8400 . ? O8 C20 1.216(4) . ? O8 Cu1 2.434(2) 1_655 ? N1 C25 1.322(4) . ? N1 C36 1.362(4) . ? N2 C34 1.319(4) . ? N2 C35 1.356(4) . ? C1 C2 1.378(4) . ? C1 C6 1.402(4) . ? C1 C7 1.507(4) . ? C2 C3 1.392(4) . ? C2 H2A 0.9500 . ? C3 C4 1.378(4) . ? C3 C8 1.497(4) . ? C4 C5 1.407(4) . ? C4 H4A 0.9500 . ? C5 C6 1.405(4) . ? C5 C9 1.528(4) . ? C6 H6A 0.9500 . ? C9 C10 1.531(5) . ? C9 C11 1.547(6) . ? C9 C12 1.552(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.391(4) . ? C13 C18 1.396(4) . ? C13 C19 1.470(4) . ? C14 C15 1.377(4) . ? C14 H14A 0.9500 . ? C15 C16 1.395(4) . ? C15 C20 1.495(4) . ? C16 C17 1.386(5) . ? C16 H16A 0.9500 . ? C17 C18 1.405(4) . ? C17 C21 1.539(5) . ? C18 H18A 0.9500 . ? C21 C24 1.505(6) . ? C21 C22 1.511(5) . ? C21 C23 1.515(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.395(5) . ? C25 H25A 0.9500 . ? C26 C27 1.374(6) . ? C26 H26A 0.9500 . ? C27 C28 1.407(6) . ? C27 H27A 0.9500 . ? C28 C36 1.399(5) . ? C28 C29 1.433(6) . ? C29 C30 1.354(7) . ? C29 H29A 0.9500 . ? C30 C31 1.439(5) . ? C30 H30A 0.9500 . ? C31 C35 1.406(4) . ? C31 C32 1.410(6) . ? C32 C33 1.361(6) . ? C32 H32A 0.9500 . ? C33 C34 1.394(5) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? C35 C36 1.432(5) . ? 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 O4 Cu1 O1 98.54(9) 2 . ? O4 Cu1 N2 168.67(10) 2 . ? O1 Cu1 N2 92.76(10) . . ? O4 Cu1 N1 87.44(10) 2 . ? O1 Cu1 N1 167.93(9) . . ? N2 Cu1 N1 81.30(11) . . ? O4 Cu1 O5 89.97(9) 2 . ? O1 Cu1 O5 101.11(9) . . ? N2 Cu1 O5 88.68(10) . . ? N1 Cu1 O5 89.31(9) . . ? O4 Cu1 O8 96.92(9) 2 1_455 ? O1 Cu1 O8 91.17(8) . 1_455 ? N2 Cu1 O8 81.92(10) . 1_455 ? N1 Cu1 O8 77.65(9) . 1_455 ? O5 Cu1 O8 164.90(8) . 1_455 ? C7 O1 Cu1 124.69(19) . . ? C8 O4 Cu1 127.8(2) . 2_545 ? C19 O5 Cu1 121.7(2) . . ? C19 O6 H6B 109.5 . . ? C20 O7 H7A 109.5 . . ? C20 O8 Cu1 123.3(2) . 1_655 ? C25 N1 C36 118.1(3) . . ? C25 N1 Cu1 129.2(2) . . ? C36 N1 Cu1 111.8(2) . . ? C34 N2 C35 117.9(3) . . ? C34 N2 Cu1 129.5(2) . . ? C35 N2 Cu1 112.5(2) . . ? C2 C1 C6 119.8(3) . . ? C2 C1 C7 116.6(3) . . ? C6 C1 C7 123.6(3) . . ? C1 C2 C3 120.9(3) . . ? C1 C2 H2A 119.5 . . ? C3 C2 H2A 119.5 . . ? C4 C3 C2 119.0(3) . . ? C4 C3 C8 122.8(3) . . ? C2 C3 C8 118.2(3) . . ? C3 C4 C5 122.2(3) . . ? C3 C4 H4A 118.9 . . ? C5 C4 H4A 118.9 . . ? C6 C5 C4 117.4(3) . . ? C6 C5 C9 123.4(3) . . ? C4 C5 C9 119.2(3) . . ? C1 C6 C5 120.7(3) . . ? C1 C6 H6A 119.7 . . ? C5 C6 H6A 119.7 . . ? O2 C7 O1 126.2(3) . . ? O2 C7 C1 115.4(3) . . ? O1 C7 C1 118.3(3) . . ? O3 C8 O4 126.2(3) . . ? O3 C8 C3 118.0(3) . . ? O4 C8 C3 115.8(3) . . ? C5 C9 C10 112.8(3) . . ? C5 C9 C11 109.3(3) . . ? C10 C9 C11 108.2(3) . . ? C5 C9 C12 110.3(3) . . ? C10 C9 C12 108.1(3) . . ? C11 C9 C12 108.0(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 119.6(3) . . ? C14 C13 C19 122.4(3) . . ? C18 C13 C19 118.0(3) . . ? C15 C14 C13 119.4(3) . . ? C15 C14 H14A 120.3 . . ? C13 C14 H14A 120.3 . . ? C14 C15 C16 120.4(3) . . ? C14 C15 C20 122.8(3) . . ? C16 C15 C20 116.8(3) . . ? C17 C16 C15 122.0(3) . . ? C17 C16 H16A 119.0 . . ? C15 C16 H16A 119.0 . . ? C16 C17 C18 116.5(3) . . ? C16 C17 C21 120.3(3) . . ? C18 C17 C21 123.1(3) . . ? C13 C18 C17 122.0(3) . . ? C13 C18 H18A 119.0 . . ? C17 C18 H18A 119.0 . . ? O5 C19 O6 123.8(3) . . ? O5 C19 C13 122.0(3) . . ? O6 C19 C13 114.2(3) . . ? O8 C20 O7 124.0(3) . . ? O8 C20 C15 121.5(3) . . ? O7 C20 C15 114.5(3) . . ? C24 C21 C22 108.9(4) . . ? C24 C21 C23 110.9(4) . . ? C22 C21 C23 107.4(4) . . ? C24 C21 C17 108.8(3) . . ? C22 C21 C17 111.8(3) . . ? C23 C21 C17 109.1(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N1 C25 C26 123.0(4) . . ? N1 C25 H25A 118.5 . . ? C26 C25 H25A 118.5 . . ? C27 C26 C25 118.8(4) . . ? C27 C26 H26A 120.6 . . ? C25 C26 H26A 120.6 . . ? C26 C27 C28 120.1(4) . . ? C26 C27 H27A 120.0 . . ? C28 C27 H27A 120.0 . . ? C36 C28 C27 116.7(3) . . ? C36 C28 C29 118.7(4) . . ? C27 C28 C29 124.6(4) . . ? C30 C29 C28 121.1(4) . . ? C30 C29 H29A 119.4 . . ? C28 C29 H29A 119.4 . . ? C29 C30 C31 120.7(3) . . ? C29 C30 H30A 119.6 . . ? C31 C30 H30A 119.6 . . ? C35 C31 C32 116.2(3) . . ? C35 C31 C30 119.5(4) . . ? C32 C31 C30 124.3(4) . . ? C33 C32 C31 119.7(4) . . ? C33 C32 H32A 120.1 . . ? C31 C32 H32A 120.1 . . ? C32 C33 C34 119.8(4) . . ? C32 C33 H33A 120.1 . . ? C34 C33 H33A 120.1 . . ? N2 C34 C33 122.7(4) . . ? N2 C34 H34A 118.7 . . ? C33 C34 H34A 118.7 . . ? N2 C35 C31 123.7(3) . . ? N2 C35 C36 117.5(3) . . ? C31 C35 C36 118.8(3) . . ? N1 C36 C28 123.2(3) . . ? N1 C36 C35 115.8(3) . . ? C28 C36 C35 120.9(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Cu1 O1 C7 38.9(3) 2 . . . ? N2 Cu1 O1 C7 -141.9(2) . . . . ? N1 Cu1 O1 C7 158.0(4) . . . . ? O5 Cu1 O1 C7 -52.7(3) . . . . ? O8 Cu1 O1 C7 136.1(2) 1_455 . . . ? O4 Cu1 O5 C19 -5.9(3) 2 . . . ? O1 Cu1 O5 C19 92.8(3) . . . . ? N2 Cu1 O5 C19 -174.7(3) . . . . ? N1 Cu1 O5 C19 -93.3(3) . . . . ? O8 Cu1 O5 C19 -123.3(3) 1_455 . . . ? O4 Cu1 N1 C25 2.7(3) 2 . . . ? O1 Cu1 N1 C25 -117.4(5) . . . . ? N2 Cu1 N1 C25 -178.5(3) . . . . ? O5 Cu1 N1 C25 92.7(3) . . . . ? O8 Cu1 N1 C25 -94.9(3) 1_455 . . . ? O4 Cu1 N1 C36 171.5(2) 2 . . . ? O1 Cu1 N1 C36 51.4(6) . . . . ? N2 Cu1 N1 C36 -9.8(2) . . . . ? O5 Cu1 N1 C36 -98.5(2) . . . . ? O8 Cu1 N1 C36 73.8(2) 1_455 . . . ? O4 Cu1 N2 C34 -170.5(4) 2 . . . ? O1 Cu1 N2 C34 13.8(3) . . . . ? N1 Cu1 N2 C34 -176.8(3) . . . . ? O5 Cu1 N2 C34 -87.3(3) . . . . ? O8 Cu1 N2 C34 104.6(3) 1_455 . . . ? O4 Cu1 N2 C35 14.2(6) 2 . . . ? O1 Cu1 N2 C35 -161.5(2) . . . . ? N1 Cu1 N2 C35 7.9(2) . . . . ? O5 Cu1 N2 C35 97.4(2) . . . . ? O8 Cu1 N2 C35 -70.7(2) 1_455 . . . ? C6 C1 C2 C3 -0.2(5) . . . . ? C7 C1 C2 C3 -179.0(3) . . . . ? C1 C2 C3 C4 1.7(5) . . . . ? C1 C2 C3 C8 -179.9(3) . . . . ? C2 C3 C4 C5 -1.3(5) . . . . ? C8 C3 C4 C5 -179.6(3) . . . . ? C3 C4 C5 C6 -0.5(5) . . . . ? C3 C4 C5 C9 -179.5(3) . . . . ? C2 C1 C6 C5 -1.7(5) . . . . ? C7 C1 C6 C5 177.0(3) . . . . ? C4 C5 C6 C1 2.0(5) . . . . ? C9 C5 C6 C1 -179.1(3) . . . . ? Cu1 O1 C7 O2 8.9(5) . . . . ? Cu1 O1 C7 C1 -173.7(2) . . . . ? C2 C1 C7 O2 35.7(4) . . . . ? C6 C1 C7 O2 -143.0(3) . . . . ? C2 C1 C7 O1 -141.9(3) . . . . ? C6 C1 C7 O1 39.4(5) . . . . ? Cu1 O4 C8 O3 -6.5(5) 2_545 . . . ? Cu1 O4 C8 C3 173.1(2) 2_545 . . . ? C4 C3 C8 O3 -171.0(3) . . . . ? C2 C3 C8 O3 10.7(5) . . . . ? C4 C3 C8 O4 9.4(5) . . . . ? C2 C3 C8 O4 -168.9(3) . . . . ? C6 C5 C9 C10 4.5(5) . . . . ? C4 C5 C9 C10 -176.6(3) . . . . ? C6 C5 C9 C11 -115.9(4) . . . . ? C4 C5 C9 C11 63.0(4) . . . . ? C6 C5 C9 C12 125.5(4) . . . . ? C4 C5 C9 C12 -55.6(5) . . . . ? C18 C13 C14 C15 1.9(6) . . . . ? C19 C13 C14 C15 179.9(3) . . . . ? C13 C14 C15 C16 -0.9(6) . . . . ? C13 C14 C15 C20 178.3(4) . . . . ? C14 C15 C16 C17 -1.5(5) . . . . ? C20 C15 C16 C17 179.3(3) . . . . ? C15 C16 C17 C18 2.7(5) . . . . ? C15 C16 C17 C21 -176.1(3) . . . . ? C14 C13 C18 C17 -0.5(6) . . . . ? C19 C13 C18 C17 -178.7(3) . . . . ? C16 C17 C18 C13 -1.7(5) . . . . ? C21 C17 C18 C13 177.1(3) . . . . ? Cu1 O5 C19 O6 -58.8(4) . . . . ? Cu1 O5 C19 C13 120.3(3) . . . . ? C14 C13 C19 O5 169.3(4) . . . . ? C18 C13 C19 O5 -12.6(5) . . . . ? C14 C13 C19 O6 -11.5(5) . . . . ? C18 C13 C19 O6 166.6(3) . . . . ? Cu1 O8 C20 O7 -49.7(4) 1_655 . . . ? Cu1 O8 C20 C15 132.0(3) 1_655 . . . ? C14 C15 C20 O8 -169.3(3) . . . . ? C16 C15 C20 O8 9.9(5) . . . . ? C14 C15 C20 O7 12.2(5) . . . . ? C16 C15 C20 O7 -168.6(3) . . . . ? C16 C17 C21 C24 -68.3(5) . . . . ? C18 C17 C21 C24 112.9(4) . . . . ? C16 C17 C21 C22 171.4(4) . . . . ? C18 C17 C21 C22 -7.4(6) . . . . ? C16 C17 C21 C23 52.8(5) . . . . ? C18 C17 C21 C23 -126.0(4) . . . . ? C36 N1 C25 C26 -1.5(5) . . . . ? Cu1 N1 C25 C26 166.6(3) . . . . ? N1 C25 C26 C27 0.4(6) . . . . ? C25 C26 C27 C28 1.6(6) . . . . ? C26 C27 C28 C36 -2.4(5) . . . . ? C26 C27 C28 C29 177.6(3) . . . . ? C36 C28 C29 C30 1.0(5) . . . . ? C27 C28 C29 C30 -179.0(4) . . . . ? C28 C29 C30 C31 -2.0(6) . . . . ? C29 C30 C31 C35 0.2(5) . . . . ? C29 C30 C31 C32 -178.1(4) . . . . ? C35 C31 C32 C33 0.0(5) . . . . ? C30 C31 C32 C33 178.3(4) . . . . ? C31 C32 C33 C34 -1.6(6) . . . . ? C35 N2 C34 C33 -0.3(5) . . . . ? Cu1 N2 C34 C33 -175.3(3) . . . . ? C32 C33 C34 N2 1.7(6) . . . . ? C34 N2 C35 C31 -1.4(4) . . . . ? Cu1 N2 C35 C31 174.5(2) . . . . ? C34 N2 C35 C36 179.1(3) . . . . ? Cu1 N2 C35 C36 -5.0(3) . . . . ? C32 C31 C35 N2 1.5(5) . . . . ? C30 C31 C35 N2 -176.9(3) . . . . ? C32 C31 C35 C36 -179.0(3) . . . . ? C30 C31 C35 C36 2.6(4) . . . . ? C25 N1 C36 C28 0.7(4) . . . . ? Cu1 N1 C36 C28 -169.5(2) . . . . ? C25 N1 C36 C35 -179.9(3) . . . . ? Cu1 N1 C36 C35 10.0(3) . . . . ? C27 C28 C36 N1 1.2(5) . . . . ? C29 C28 C36 N1 -178.7(3) . . . . ? C27 C28 C36 C35 -178.1(3) . . . . ? C29 C28 C36 C35 1.9(5) . . . . ? N2 C35 C36 N1 -3.5(4) . . . . ? C31 C35 C36 N1 177.0(3) . . . . ? N2 C35 C36 C28 175.9(3) . . . . ? C31 C35 C36 C28 -3.6(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6 H6B O2 0.84 1.69 2.526(3) 172.7 . O7 H7A O3 0.84 1.73 2.565(3) 179.1 2_655 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.427 _refine_diff_density_min -0.705 _refine_diff_density_rms 0.068 #============================================================================== data_ZnBpy-[Zn(bpy)(tbip)(H2O)]4 _database_code_depnum_ccdc_archive 'CCDC 835419' #TrackingRef '- revised cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C88 H88 N8 O20 Zn4' _chemical_formula_sum 'C88 H88 N8 O20 Zn4' _chemical_formula_weight 1839.14 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 triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3469(5) _cell_length_b 13.1507(7) _cell_length_c 18.4605(9) _cell_angle_alpha 98.535(1) _cell_angle_beta 97.856(1) _cell_angle_gamma 107.013(1) _cell_volume 2106.52(19) _cell_formula_units_Z 1 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 4636 _cell_measurement_theta_min 2.1838 _cell_measurement_theta_max 27.7526 _exptl_crystal_description grain _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 1.202 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7265 _exptl_absorpt_correction_T_max 0.7654 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18693 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0769 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 28.65 _reflns_number_total 9719 _reflns_number_gt 7246 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. EADP and ISOR 0.01 are applied to the six carbon atoms of the ter-butyl. ; _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^)+(0.0748P)^2^+1.2795P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9719 _refine_ls_number_parameters 572 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0876 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1693 _refine_ls_wR_factor_gt 0.1518 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.004 _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 Zn1 Zn 0.02630(5) 0.23748(4) 0.53892(2) 0.03021(13) Uani 1 1 d . . . Zn2 Zn 0.32248(5) 0.45580(4) 0.12294(3) 0.03584(14) Uani 1 1 d . . . O1W O -0.1299(3) 0.0800(2) 0.49669(17) 0.0385(7) Uani 1 1 d D . . H1WA H -0.117(6) 0.051(4) 0.4551(14) 0.058 Uiso 1 1 d D . . H1WB H -0.099(5) 0.050(4) 0.531(2) 0.058 Uiso 1 1 d D . . O1 O 0.1994(3) 0.2013(3) 0.49318(16) 0.0434(7) Uani 1 1 d . . . O2W O 0.4777(4) 0.3965(3) 0.0727(2) 0.0559(9) Uani 1 1 d D . . H2WA H 0.496(7) 0.399(5) 0.0292(14) 0.084 Uiso 1 1 d D . . H2WB H 0.461(7) 0.338(3) 0.089(3) 0.084 Uiso 1 1 d D . . O2 O 0.0537(3) 0.2578(2) 0.41607(18) 0.0460(8) Uani 1 1 d . . . O3 O 0.3047(3) 0.3565(2) 0.19444(17) 0.0425(7) Uani 1 1 d . . . O4 O 0.3979(5) 0.2361(3) 0.1386(2) 0.0784(13) Uani 1 1 d . . . O5 O 0.4823(4) 0.5931(3) 0.17601(18) 0.0528(9) Uani 1 1 d . . . O6 O 0.4525(3) 0.6347(3) 0.06509(17) 0.0493(8) Uani 1 1 d . . . O7 O 0.9439(3) 0.7962(2) 0.35844(15) 0.0394(7) Uani 1 1 d . . . O8 O 0.9798(3) 0.9736(2) 0.38338(16) 0.0411(7) Uani 1 1 d . . . N1 N 0.1552(3) 0.4015(3) 0.59142(18) 0.0318(7) Uani 1 1 d . . . N2 N -0.1404(3) 0.3164(3) 0.53975(18) 0.0311(7) Uani 1 1 d . . . N3 N 0.1436(4) 0.5131(3) 0.1570(2) 0.0412(8) Uani 1 1 d . . . N4 N 0.1340(4) 0.3763(3) 0.03587(19) 0.0366(8) Uani 1 1 d . . . C1 C 0.2405(4) 0.1910(3) 0.3687(2) 0.0322(8) Uani 1 1 d . . . C2 C 0.2472(4) 0.2416(3) 0.3088(2) 0.0331(8) Uani 1 1 d . . . H2A H 0.2016 0.2953 0.3056 0.040 Uiso 1 1 calc R . . C3 C 0.3218(4) 0.2128(3) 0.2531(2) 0.0324(8) Uani 1 1 d . . . C4 C 0.3807(4) 0.1286(3) 0.2569(2) 0.0350(9) Uani 1 1 d . . . H4A H 0.4259 0.1067 0.2182 0.042 Uiso 1 1 calc R . . C5 C 0.3746(4) 0.0754(3) 0.3168(2) 0.0342(9) Uani 1 1 d . . . C6 C 0.3062(4) 0.1102(3) 0.3728(2) 0.0346(9) Uani 1 1 d . . . H6A H 0.3043 0.0784 0.4146 0.041 Uiso 1 1 calc R . . C7 C 0.1595(5) 0.2188(3) 0.4294(3) 0.0375(9) Uani 1 1 d . . . C8 C 0.3422(5) 0.2719(4) 0.1899(2) 0.0399(10) Uani 1 1 d . . . C9 C 0.4421(6) -0.0171(4) 0.3178(3) 0.0493(12) Uani 1 1 d . . . C10 C 0.3823(9) -0.0981(5) 0.2459(4) 0.094(2) Uani 1 1 d . . . H10A H 0.2732 -0.1266 0.2386 0.141 Uiso 1 1 calc R . . H10B H 0.4246 -0.1562 0.2475 0.141 Uiso 1 1 calc R . . H10C H 0.4106 -0.0634 0.2054 0.141 Uiso 1 1 calc R . . C11 C 0.4165(11) -0.0692(6) 0.3842(4) 0.120(3) Uani 1 1 d . . . H11A H 0.3093 -0.1039 0.3807 0.180 Uiso 1 1 calc R . . H11B H 0.4553 -0.0147 0.4291 0.180 Uiso 1 1 calc R . . H11C H 0.4685 -0.1222 0.3853 0.180 Uiso 1 1 calc R . . C12 C 0.6165(7) 0.0317(6) 0.3242(4) 0.093(2) Uani 1 1 d . . . H12A H 0.6621 -0.0248 0.3249 0.139 Uiso 1 1 calc R . . H12B H 0.6583 0.0852 0.3695 0.139 Uiso 1 1 calc R . . H12C H 0.6372 0.0651 0.2823 0.139 Uiso 1 1 calc R . . C13 C 0.8429(4) 0.8709(3) 0.2642(2) 0.0307(8) Uani 1 1 d . . . C14 C 0.7300(4) 0.7742(3) 0.2327(2) 0.0303(8) Uani 1 1 d . . . H14A H 0.7132 0.7172 0.2582 0.036 Uiso 1 1 calc R . . C15 C 0.6417(4) 0.7613(3) 0.1637(2) 0.0312(8) Uani 1 1 d . . . C16 C 0.6711(4) 0.8461(3) 0.1255(2) 0.0353(9) Uani 1 1 d . . . H16A H 0.6136 0.8368 0.0783 0.042 Uiso 1 1 calc R . . C17 C 0.7841(5) 0.9443(4) 0.1560(2) 0.0406(10) Uani 1 1 d . A . C18 C 0.8699(5) 0.9555(3) 0.2261(2) 0.0365(9) Uani 1 1 d . . . H18A H 0.9464 1.0206 0.2476 0.044 Uiso 1 1 calc R . . C19 C 0.9300(4) 0.8833(3) 0.3415(2) 0.0313(8) Uani 1 1 d . . . C20 C 0.5165(4) 0.6565(4) 0.1316(2) 0.0373(9) Uani 1 1 d . . . C21 C 0.8159(6) 1.0376(4) 0.1130(3) 0.0577(13) Uani 1 1 d . . . C22 C 0.9830(10) 1.0624(8) 0.0996(5) 0.086(3) Uani 0.761(7) 1 d P A 1 H22A H 1.0515 1.0784 0.1466 0.130 Uiso 0.761(7) 1 calc PR A 1 H22B H 1.0080 1.1238 0.0758 0.130 Uiso 0.761(7) 1 calc PR A 1 H22C H 0.9921 1.0004 0.0682 0.130 Uiso 0.761(7) 1 calc PR A 1 C22' C 0.944(3) 1.124(3) 0.1403(18) 0.086(3) Uani 0.239(7) 1 d P A 2 H22D H 0.9546 1.1449 0.1933 0.130 Uiso 0.239(7) 1 calc PR A 2 H22E H 0.9368 1.1842 0.1175 0.130 Uiso 0.239(7) 1 calc PR A 2 H22F H 1.0315 1.1054 0.1292 0.130 Uiso 0.239(7) 1 calc PR A 2 C23 C 0.8145(16) 1.1412(7) 0.1639(6) 0.123(5) Uani 0.761(7) 1 d P A 1 H23A H 0.8724 1.1487 0.2126 0.184 Uiso 0.761(7) 1 calc PR A 1 H23B H 0.7113 1.1363 0.1676 0.184 Uiso 0.761(7) 1 calc PR A 1 H23C H 0.8589 1.2032 0.1431 0.184 Uiso 0.761(7) 1 calc PR A 1 C23' C 0.813(6) 0.983(3) 0.024(2) 0.123(5) Uani 0.239(7) 1 d P A 2 H23D H 0.7166 0.9742 -0.0063 0.184 Uiso 0.239(7) 1 calc PR A 2 H23E H 0.8284 0.9136 0.0218 0.184 Uiso 0.239(7) 1 calc PR A 2 H23F H 0.8932 1.0303 0.0054 0.184 Uiso 0.239(7) 1 calc PR A 2 C24 C 0.7189(12) 1.0114(9) 0.0378(6) 0.097(3) Uani 0.761(7) 1 d PU A 1 H24A H 0.6207 1.0180 0.0423 0.145 Uiso 0.761(7) 1 calc PR A 1 H24B H 0.7069 0.9385 0.0142 0.145 Uiso 0.761(7) 1 calc PR A 1 H24C H 0.7662 1.0609 0.0081 0.145 Uiso 0.761(7) 1 calc PR A 1 C24' C 0.662(3) 1.069(3) 0.0968(19) 0.097(3) Uani 0.239(7) 1 d PU A 2 H24D H 0.6409 1.0997 0.1431 0.145 Uiso 0.239(7) 1 calc PR A 2 H24E H 0.5790 1.0052 0.0728 0.145 Uiso 0.239(7) 1 calc PR A 2 H24F H 0.6753 1.1212 0.0650 0.145 Uiso 0.239(7) 1 calc PR A 2 C25 C 0.3025(5) 0.4348(4) 0.6212(3) 0.0443(11) Uani 1 1 d . . . H25A H 0.3559 0.3853 0.6168 0.053 Uiso 1 1 calc R . . C26 C 0.3794(5) 0.5393(4) 0.6585(3) 0.0578(14) Uani 1 1 d . . . H26A H 0.4822 0.5602 0.6800 0.069 Uiso 1 1 calc R . . C27 C 0.2987(6) 0.6128(4) 0.6629(3) 0.0637(15) Uani 1 1 d . . . H27A H 0.3477 0.6846 0.6869 0.076 Uiso 1 1 calc R . . C28 C 0.1462(5) 0.5791(4) 0.6317(3) 0.0507(12) Uani 1 1 d . . . H28A H 0.0910 0.6276 0.6335 0.061 Uiso 1 1 calc R . . C29 C 0.0768(4) 0.4707(3) 0.5973(2) 0.0326(8) Uani 1 1 d . . . C30 C -0.0893(4) 0.4234(3) 0.5680(2) 0.0318(8) Uani 1 1 d . . . C31 C -0.1890(5) 0.4830(4) 0.5706(3) 0.0462(11) Uani 1 1 d . . . H31A H -0.1523 0.5574 0.5894 0.055 Uiso 1 1 calc R . . C32 C -0.3417(5) 0.4321(4) 0.5452(3) 0.0582(14) Uani 1 1 d . . . H32A H -0.4095 0.4715 0.5466 0.070 Uiso 1 1 calc R . . C33 C -0.3941(5) 0.3226(4) 0.5178(3) 0.0551(13) Uani 1 1 d . . . H33A H -0.4976 0.2860 0.5012 0.066 Uiso 1 1 calc R . . C34 C -0.2890(5) 0.2681(4) 0.5155(2) 0.0405(10) Uani 1 1 d . . . H34A H -0.3237 0.1940 0.4959 0.049 Uiso 1 1 calc R . . C35 C 0.1580(7) 0.5850(4) 0.2195(3) 0.0602(14) Uani 1 1 d . . . H35A H 0.2540 0.6194 0.2493 0.072 Uiso 1 1 calc R . . C36 C 0.0332(9) 0.6089(5) 0.2407(4) 0.0751(19) Uani 1 1 d . . . H36A H 0.0458 0.6600 0.2836 0.090 Uiso 1 1 calc R . . C37 C -0.1080(9) 0.5572(6) 0.1983(4) 0.087(2) Uani 1 1 d . . . H37A H -0.1930 0.5720 0.2121 0.104 Uiso 1 1 calc R . . C38 C -0.1225(6) 0.4838(5) 0.1357(4) 0.0640(15) Uani 1 1 d . . . H38A H -0.2183 0.4469 0.1065 0.077 Uiso 1 1 calc R . . C39 C 0.0055(5) 0.4639(4) 0.1152(3) 0.0407(10) Uani 1 1 d . . . C40 C 0.0006(4) 0.3887(3) 0.0461(2) 0.0382(9) Uani 1 1 d . . . C41 C -0.1314(5) 0.3338(4) -0.0053(3) 0.0572(14) Uani 1 1 d . . . H41A H -0.2235 0.3429 0.0024 0.069 Uiso 1 1 calc R . . C42 C -0.1256(7) 0.2653(5) -0.0684(3) 0.0677(16) Uani 1 1 d . . . H42A H -0.2134 0.2283 -0.1038 0.081 Uiso 1 1 calc R . . C43 C 0.0090(7) 0.2527(5) -0.0778(3) 0.0636(15) Uani 1 1 d . . . H43A H 0.0152 0.2063 -0.1197 0.076 Uiso 1 1 calc R . . C44 C 0.1370(6) 0.3092(4) -0.0248(3) 0.0545(12) Uani 1 1 d . . . H44A H 0.2296 0.3002 -0.0317 0.065 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0335(2) 0.0298(2) 0.0282(2) 0.00227(18) 0.00667(18) 0.01267(18) Zn2 0.0335(2) 0.0375(3) 0.0322(3) 0.0086(2) 0.00245(19) 0.00570(19) O1W 0.0449(16) 0.0316(16) 0.0371(17) 0.0013(13) 0.0047(14) 0.0137(13) O1 0.0506(17) 0.0502(19) 0.0357(17) 0.0054(14) 0.0182(14) 0.0228(15) O2W 0.0528(19) 0.074(3) 0.056(2) 0.028(2) 0.0273(17) 0.0287(19) O2 0.0480(17) 0.0406(17) 0.061(2) 0.0110(15) 0.0229(15) 0.0252(14) O3 0.0530(17) 0.0392(17) 0.0433(18) 0.0194(14) 0.0163(14) 0.0182(14) O4 0.138(4) 0.076(3) 0.059(2) 0.035(2) 0.059(3) 0.062(3) O5 0.0519(18) 0.0451(19) 0.0436(19) 0.0105(15) 0.0011(15) -0.0084(15) O6 0.0434(16) 0.059(2) 0.0359(17) 0.0010(15) -0.0014(13) 0.0106(15) O7 0.0614(18) 0.0324(16) 0.0279(15) 0.0044(12) 0.0052(13) 0.0222(14) O8 0.0527(17) 0.0281(15) 0.0367(16) -0.0014(13) 0.0035(13) 0.0101(13) N1 0.0328(16) 0.0266(17) 0.0339(18) 0.0053(14) 0.0051(13) 0.0072(13) N2 0.0317(15) 0.0316(17) 0.0294(17) 0.0037(14) 0.0045(13) 0.0110(13) N3 0.049(2) 0.042(2) 0.040(2) 0.0116(17) 0.0148(17) 0.0196(17) N4 0.0358(17) 0.0369(19) 0.0307(18) 0.0003(15) -0.0017(14) 0.0086(14) C1 0.0294(18) 0.028(2) 0.037(2) -0.0002(17) 0.0099(16) 0.0072(15) C2 0.0339(19) 0.027(2) 0.038(2) 0.0019(17) 0.0058(16) 0.0122(15) C3 0.0338(19) 0.030(2) 0.031(2) 0.0060(16) 0.0067(16) 0.0061(15) C4 0.040(2) 0.033(2) 0.034(2) 0.0020(17) 0.0109(17) 0.0149(17) C5 0.037(2) 0.036(2) 0.032(2) 0.0052(17) 0.0093(16) 0.0149(17) C6 0.043(2) 0.030(2) 0.033(2) 0.0065(17) 0.0131(17) 0.0111(17) C7 0.040(2) 0.026(2) 0.047(3) 0.0037(18) 0.0187(19) 0.0072(16) C8 0.045(2) 0.038(2) 0.036(2) 0.0106(19) 0.0097(18) 0.0086(19) C9 0.072(3) 0.054(3) 0.044(3) 0.018(2) 0.024(2) 0.042(3) C10 0.148(7) 0.057(4) 0.081(5) -0.012(3) 0.003(4) 0.060(4) C11 0.232(10) 0.123(6) 0.104(6) 0.079(5) 0.108(6) 0.143(7) C12 0.084(4) 0.129(6) 0.097(5) 0.023(5) 0.026(4) 0.077(5) C13 0.0335(18) 0.032(2) 0.029(2) 0.0050(16) 0.0111(15) 0.0118(16) C14 0.0351(19) 0.0277(19) 0.0298(19) 0.0084(16) 0.0079(15) 0.0106(15) C15 0.0292(17) 0.036(2) 0.0279(19) 0.0056(16) 0.0095(15) 0.0091(16) C16 0.0340(19) 0.044(2) 0.029(2) 0.0111(18) 0.0048(16) 0.0131(17) C17 0.039(2) 0.045(3) 0.041(2) 0.021(2) 0.0142(18) 0.0095(18) C18 0.038(2) 0.032(2) 0.036(2) 0.0077(18) 0.0085(17) 0.0059(16) C19 0.0335(18) 0.029(2) 0.031(2) 0.0032(16) 0.0088(16) 0.0083(15) C20 0.0315(19) 0.043(2) 0.035(2) 0.0061(19) 0.0085(17) 0.0092(17) C21 0.063(3) 0.054(3) 0.053(3) 0.029(3) 0.011(2) 0.007(2) C22 0.090(6) 0.087(7) 0.076(7) 0.046(5) 0.031(5) -0.001(5) C22' 0.090(6) 0.087(7) 0.076(7) 0.046(5) 0.031(5) -0.001(5) C23 0.237(14) 0.076(7) 0.120(9) 0.078(7) 0.099(10) 0.089(8) C23' 0.237(14) 0.076(7) 0.120(9) 0.078(7) 0.099(10) 0.089(8) C24 0.104(5) 0.093(5) 0.086(5) 0.062(5) -0.013(4) 0.013(4) C24' 0.104(5) 0.093(5) 0.086(5) 0.062(5) -0.013(4) 0.013(4) C25 0.035(2) 0.045(3) 0.052(3) 0.009(2) 0.0083(19) 0.0118(19) C26 0.038(2) 0.051(3) 0.065(3) 0.000(3) -0.005(2) -0.001(2) C27 0.060(3) 0.034(3) 0.077(4) -0.003(3) -0.004(3) -0.001(2) C28 0.053(3) 0.035(2) 0.061(3) 0.003(2) 0.008(2) 0.013(2) C29 0.040(2) 0.028(2) 0.030(2) 0.0069(16) 0.0088(16) 0.0097(16) C30 0.039(2) 0.031(2) 0.030(2) 0.0098(16) 0.0103(16) 0.0139(16) C31 0.049(2) 0.036(2) 0.058(3) 0.008(2) 0.010(2) 0.021(2) C32 0.046(3) 0.064(3) 0.077(4) 0.020(3) 0.013(3) 0.033(3) C33 0.031(2) 0.058(3) 0.073(4) 0.013(3) -0.004(2) 0.014(2) C34 0.038(2) 0.036(2) 0.041(2) 0.0040(19) 0.0010(18) 0.0084(18) C35 0.092(4) 0.048(3) 0.043(3) 0.003(2) 0.017(3) 0.026(3) C36 0.133(6) 0.057(4) 0.065(4) 0.019(3) 0.057(4) 0.055(4) C37 0.108(5) 0.088(5) 0.112(6) 0.044(5) 0.072(5) 0.067(5) C38 0.056(3) 0.059(3) 0.091(4) 0.022(3) 0.030(3) 0.029(3) C39 0.046(2) 0.038(2) 0.049(3) 0.020(2) 0.020(2) 0.0206(19) C40 0.035(2) 0.036(2) 0.044(2) 0.0158(19) 0.0040(18) 0.0100(17) C41 0.038(2) 0.058(3) 0.069(4) 0.020(3) -0.006(2) 0.008(2) C42 0.067(4) 0.056(3) 0.056(3) 0.008(3) -0.021(3) 0.000(3) C43 0.078(4) 0.056(3) 0.044(3) 0.000(3) 0.002(3) 0.010(3) C44 0.059(3) 0.058(3) 0.041(3) 0.000(2) 0.007(2) 0.017(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O7 2.010(3) 2_666 ? Zn1 O1 2.064(3) . ? Zn1 N2 2.111(3) . ? Zn1 O1W 2.114(3) . ? Zn1 N1 2.141(3) . ? Zn1 O2 2.362(3) . ? Zn1 C7 2.534(4) . ? Zn2 O3 1.979(3) . ? Zn2 O5 1.987(3) . ? Zn2 O2W 2.095(3) . ? Zn2 N4 2.105(3) . ? Zn2 N3 2.155(4) . ? O1W H1WA 0.85(4) . ? O1W H1WB 0.86(4) . ? O1 C7 1.261(5) . ? O2W H2WA 0.85(4) . ? O2W H2WB 0.85(4) . ? O2 C7 1.252(5) . ? O3 C8 1.255(5) . ? O4 C8 1.239(5) . ? O5 C20 1.260(5) . ? O6 C20 1.242(5) . ? O7 C19 1.268(5) . ? O7 Zn1 2.010(3) 2_666 ? O8 C19 1.236(4) . ? N1 C25 1.326(5) . ? N1 C29 1.327(5) . ? N2 C34 1.327(5) . ? N2 C30 1.342(5) . ? N3 C39 1.330(6) . ? N3 C35 1.342(6) . ? N4 C44 1.328(6) . ? N4 C40 1.338(5) . ? C1 C2 1.372(5) . ? C1 C6 1.381(5) . ? C1 C7 1.495(5) . ? C2 C3 1.387(5) . ? C2 H2A 0.9300 . ? C3 C4 1.379(5) . ? C3 C8 1.499(5) . ? C4 C5 1.393(5) . ? C4 H4A 0.9300 . ? C5 C6 1.378(5) . ? C5 C9 1.526(6) . ? C6 H6A 0.9300 . ? C9 C10 1.496(7) . ? C9 C11 1.505(7) . ? C9 C12 1.548(8) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.377(5) . ? C13 C18 1.384(5) . ? C13 C19 1.504(5) . ? C14 C15 1.379(5) . ? C14 H14A 0.9300 . ? C15 C16 1.386(5) . ? C15 C20 1.498(5) . ? C16 C17 1.388(6) . ? C16 H16A 0.9300 . ? C17 C18 1.390(6) . ? C17 C21 1.537(6) . ? C18 H18A 0.9300 . ? C21 C22' 1.36(3) . ? C21 C24 1.484(10) . ? C21 C23 1.540(10) . ? C21 C22 1.562(10) . ? C21 C24' 1.61(3) . ? C21 C23' 1.69(3) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C22' H22D 0.9600 . ? C22' H22E 0.9600 . ? C22' H22F 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C23' H23D 0.9600 . ? C23' H23E 0.9600 . ? C23' H23F 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C24' H24D 0.9600 . ? C24' H24E 0.9600 . ? C24' H24F 0.9600 . ? C25 C26 1.372(6) . ? C25 H25A 0.9300 . ? C26 C27 1.389(7) . ? C26 H26A 0.9300 . ? C27 C28 1.375(7) . ? C27 H27A 0.9300 . ? C28 C29 1.390(6) . ? C28 H28A 0.9300 . ? C29 C30 1.481(5) . ? C30 C31 1.384(5) . ? C31 C32 1.368(6) . ? C31 H31A 0.9300 . ? C32 C33 1.369(7) . ? C32 H32A 0.9300 . ? C33 C34 1.376(6) . ? C33 H33A 0.9300 . ? C34 H34A 0.9300 . ? C35 C36 1.383(8) . ? C35 H35A 0.9300 . ? C36 C37 1.360(9) . ? C36 H36A 0.9300 . ? C37 C38 1.354(9) . ? C37 H37A 0.9300 . ? C38 C39 1.387(6) . ? C38 H38A 0.9300 . ? C39 C40 1.480(6) . ? C40 C41 1.378(6) . ? C41 C42 1.380(8) . ? C41 H41A 0.9300 . ? C42 C43 1.347(8) . ? C42 H42A 0.9300 . ? C43 C44 1.373(7) . ? C43 H43A 0.9300 . ? C44 H44A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Zn1 O1 103.91(12) 2_666 . ? O7 Zn1 N2 104.19(12) 2_666 . ? O1 Zn1 N2 150.40(13) . . ? O7 Zn1 O1W 90.65(12) 2_666 . ? O1 Zn1 O1W 93.31(12) . . ? N2 Zn1 O1W 95.49(12) . . ? O7 Zn1 N1 85.93(12) 2_666 . ? O1 Zn1 N1 96.30(12) . . ? N2 Zn1 N1 76.65(12) . . ? O1W Zn1 N1 170.33(12) . . ? O7 Zn1 O2 162.83(11) 2_666 . ? O1 Zn1 O2 58.93(11) . . ? N2 Zn1 O2 92.84(11) . . ? O1W Zn1 O2 89.79(11) . . ? N1 Zn1 O2 96.14(12) . . ? O7 Zn1 C7 133.47(13) 2_666 . ? O1 Zn1 C7 29.66(12) . . ? N2 Zn1 C7 122.03(14) . . ? O1W Zn1 C7 90.04(12) . . ? N1 Zn1 C7 98.88(13) . . ? O2 Zn1 C7 29.37(12) . . ? O3 Zn2 O5 105.73(13) . . ? O3 Zn2 O2W 93.33(13) . . ? O5 Zn2 O2W 93.03(16) . . ? O3 Zn2 N4 104.06(13) . . ? O5 Zn2 N4 148.33(14) . . ? O2W Zn2 N4 95.76(15) . . ? O3 Zn2 N3 92.53(13) . . ? O5 Zn2 N3 91.98(15) . . ? O2W Zn2 N3 170.98(14) . . ? N4 Zn2 N3 76.15(14) . . ? Zn1 O1W H1WA 113(4) . . ? Zn1 O1W H1WB 97(3) . . ? H1WA O1W H1WB 109(5) . . ? C7 O1 Zn1 96.3(2) . . ? Zn2 O2W H2WA 128(4) . . ? Zn2 O2W H2WB 97(4) . . ? H2WA O2W H2WB 121(6) . . ? C7 O2 Zn1 82.9(3) . . ? C8 O3 Zn2 127.1(3) . . ? C20 O5 Zn2 110.3(3) . . ? C19 O7 Zn1 127.2(3) . 2_666 ? C25 N1 C29 119.6(4) . . ? C25 N1 Zn1 124.4(3) . . ? C29 N1 Zn1 115.9(3) . . ? C34 N2 C30 118.8(3) . . ? C34 N2 Zn1 125.0(3) . . ? C30 N2 Zn1 116.1(2) . . ? C39 N3 C35 118.7(4) . . ? C39 N3 Zn2 115.5(3) . . ? C35 N3 Zn2 125.5(4) . . ? C44 N4 C40 118.7(4) . . ? C44 N4 Zn2 124.4(3) . . ? C40 N4 Zn2 116.7(3) . . ? C2 C1 C6 119.9(4) . . ? C2 C1 C7 121.6(4) . . ? C6 C1 C7 118.5(4) . . ? C1 C2 C3 120.1(4) . . ? C1 C2 H2A 120.0 . . ? C3 C2 H2A 120.0 . . ? C4 C3 C2 118.9(4) . . ? C4 C3 C8 119.5(4) . . ? C2 C3 C8 121.7(4) . . ? C3 C4 C5 122.2(4) . . ? C3 C4 H4A 118.9 . . ? C5 C4 H4A 118.9 . . ? C6 C5 C4 117.0(4) . . ? C6 C5 C9 123.4(4) . . ? C4 C5 C9 119.6(4) . . ? C5 C6 C1 121.8(4) . . ? C5 C6 H6A 119.1 . . ? C1 C6 H6A 119.1 . . ? O2 C7 O1 121.5(4) . . ? O2 C7 C1 120.0(4) . . ? O1 C7 C1 118.5(4) . . ? O2 C7 Zn1 67.7(2) . . ? O1 C7 Zn1 54.1(2) . . ? C1 C7 Zn1 170.4(3) . . ? O4 C8 O3 125.1(4) . . ? O4 C8 C3 118.3(4) . . ? O3 C8 C3 116.6(4) . . ? C10 C9 C11 112.0(6) . . ? C10 C9 C5 110.4(4) . . ? C11 C9 C5 112.0(4) . . ? C10 C9 C12 107.4(5) . . ? C11 C9 C12 107.1(5) . . ? C5 C9 C12 107.6(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 120.0(4) . . ? C14 C13 C19 118.5(3) . . ? C18 C13 C19 121.4(4) . . ? C13 C14 C15 120.5(4) . . ? C13 C14 H14A 119.7 . . ? C15 C14 H14A 119.7 . . ? C14 C15 C16 119.0(4) . . ? C14 C15 C20 119.5(4) . . ? C16 C15 C20 121.5(4) . . ? C15 C16 C17 121.6(4) . . ? C15 C16 H16A 119.2 . . ? C17 C16 H16A 119.2 . . ? C16 C17 C18 118.1(4) . . ? C16 C17 C21 121.2(4) . . ? C18 C17 C21 120.7(4) . . ? C13 C18 C17 120.7(4) . . ? C13 C18 H18A 119.6 . . ? C17 C18 H18A 119.6 . . ? O8 C19 O7 125.3(4) . . ? O8 C19 C13 119.7(4) . . ? O7 C19 C13 115.0(3) . . ? O6 C20 O5 123.1(4) . . ? O6 C20 C15 121.1(4) . . ? O5 C20 C15 115.8(4) . . ? C22' C21 C24 126.6(13) . . ? C22' C21 C17 117.9(13) . . ? C24 C21 C17 114.2(5) . . ? C22' C21 C23 57.6(15) . . ? C24 C21 C23 114.8(7) . . ? C17 C21 C23 108.7(5) . . ? C22' C21 C22 47.6(15) . . ? C24 C21 C22 105.5(7) . . ? C17 C21 C22 107.8(5) . . ? C23 C21 C22 105.1(7) . . ? C22' C21 C24' 114(2) . . ? C24 C21 C24' 57.0(12) . . ? C17 C21 C24' 107.8(10) . . ? C23 C21 C24' 64.6(13) . . ? C22 C21 C24' 144.3(11) . . ? C22' C21 C23' 111(2) . . ? C17 C21 C23' 107.2(10) . . ? C23 C21 C23' 143.2(10) . . ? C22 C21 C23' 70.8(17) . . ? C24' C21 C23' 96.8(19) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? C21 C22' H22D 109.5 . . ? C21 C22' H22E 109.5 . . ? H22D C22' H22E 109.5 . . ? C21 C22' H22F 109.5 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? C21 C23' H23D 109.5 . . ? C21 C23' H23E 109.5 . . ? H23D C23' H23E 109.5 . . ? C21 C23' H23F 109.5 . . ? H23D C23' H23F 109.5 . . ? H23E C23' H23F 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? C21 C24' H24D 109.5 . . ? C21 C24' H24E 109.5 . . ? H24D C24' H24E 109.5 . . ? C21 C24' H24F 109.5 . . ? H24D C24' H24F 109.5 . . ? H24E C24' H24F 109.5 . . ? N1 C25 C26 122.7(4) . . ? N1 C25 H25A 118.6 . . ? C26 C25 H25A 118.6 . . ? C25 C26 C27 117.8(4) . . ? C25 C26 H26A 121.1 . . ? C27 C26 H26A 121.1 . . ? C28 C27 C26 119.8(5) . . ? C28 C27 H27A 120.1 . . ? C26 C27 H27A 120.1 . . ? C27 C28 C29 118.3(4) . . ? C27 C28 H28A 120.9 . . ? C29 C28 H28A 120.9 . . ? N1 C29 C28 121.6(4) . . ? N1 C29 C30 115.4(3) . . ? C28 C29 C30 122.9(4) . . ? N2 C30 C31 120.8(4) . . ? N2 C30 C29 115.9(3) . . ? C31 C30 C29 123.4(4) . . ? C32 C31 C30 119.7(4) . . ? C32 C31 H31A 120.2 . . ? C30 C31 H31A 120.2 . . ? C31 C32 C33 119.5(4) . . ? C31 C32 H32A 120.2 . . ? C33 C32 H32A 120.2 . . ? C32 C33 C34 118.1(4) . . ? C32 C33 H33A 121.0 . . ? C34 C33 H33A 121.0 . . ? N2 C34 C33 123.1(4) . . ? N2 C34 H34A 118.4 . . ? C33 C34 H34A 118.4 . . ? N3 C35 C36 121.4(6) . . ? N3 C35 H35A 119.3 . . ? C36 C35 H35A 119.3 . . ? C37 C36 C35 119.7(6) . . ? C37 C36 H36A 120.2 . . ? C35 C36 H36A 120.2 . . ? C38 C37 C36 118.8(6) . . ? C38 C37 H37A 120.6 . . ? C36 C37 H37A 120.6 . . ? C37 C38 C39 120.0(6) . . ? C37 C38 H38A 120.0 . . ? C39 C38 H38A 120.0 . . ? N3 C39 C38 121.4(5) . . ? N3 C39 C40 115.1(4) . . ? C38 C39 C40 123.5(5) . . ? N4 C40 C41 121.0(4) . . ? N4 C40 C39 115.8(4) . . ? C41 C40 C39 123.2(4) . . ? C40 C41 C42 119.4(5) . . ? C40 C41 H41A 120.3 . . ? C42 C41 H41A 120.3 . . ? C43 C42 C41 119.1(5) . . ? C43 C42 H42A 120.4 . . ? C41 C42 H42A 120.4 . . ? C42 C43 C44 119.0(5) . . ? C42 C43 H43A 120.5 . . ? C44 C43 H43A 120.5 . . ? N4 C44 C43 122.7(5) . . ? N4 C44 H44A 118.6 . . ? C43 C44 H44A 118.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O7 Zn1 O1 C7 175.8(2) 2_666 . . . ? N2 Zn1 O1 C7 -22.9(4) . . . . ? O1W Zn1 O1 C7 84.3(3) . . . . ? N1 Zn1 O1 C7 -96.9(3) . . . . ? O2 Zn1 O1 C7 -3.5(2) . . . . ? O7 Zn1 O2 C7 1.1(5) 2_666 . . . ? O1 Zn1 O2 C7 3.5(2) . . . . ? N2 Zn1 O2 C7 174.1(2) . . . . ? O1W Zn1 O2 C7 -90.5(2) . . . . ? N1 Zn1 O2 C7 97.2(2) . . . . ? O5 Zn2 O3 C8 -111.6(4) . . . . ? O2W Zn2 O3 C8 -17.5(4) . . . . ? N4 Zn2 O3 C8 79.3(4) . . . . ? N3 Zn2 O3 C8 155.6(4) . . . . ? O3 Zn2 O5 C20 171.1(3) . . . . ? O2W Zn2 O5 C20 76.8(3) . . . . ? N4 Zn2 O5 C20 -29.3(5) . . . . ? N3 Zn2 O5 C20 -95.7(3) . . . . ? O7 Zn1 N1 C25 68.5(3) 2_666 . . . ? O1 Zn1 N1 C25 -35.1(4) . . . . ? N2 Zn1 N1 C25 174.1(4) . . . . ? O2 Zn1 N1 C25 -94.4(3) . . . . ? C7 Zn1 N1 C25 -64.9(4) . . . . ? O7 Zn1 N1 C29 -107.4(3) 2_666 . . . ? O1 Zn1 N1 C29 149.0(3) . . . . ? N2 Zn1 N1 C29 -1.8(3) . . . . ? O2 Zn1 N1 C29 89.7(3) . . . . ? C7 Zn1 N1 C29 119.2(3) . . . . ? O7 Zn1 N2 C34 -95.0(3) 2_666 . . . ? O1 Zn1 N2 C34 103.8(4) . . . . ? O1W Zn1 N2 C34 -2.9(3) . . . . ? N1 Zn1 N2 C34 -177.2(4) . . . . ? O2 Zn1 N2 C34 87.2(3) . . . . ? C7 Zn1 N2 C34 90.6(3) . . . . ? O7 Zn1 N2 C30 84.3(3) 2_666 . . . ? O1 Zn1 N2 C30 -77.0(4) . . . . ? O1W Zn1 N2 C30 176.4(3) . . . . ? N1 Zn1 N2 C30 2.1(3) . . . . ? O2 Zn1 N2 C30 -93.5(3) . . . . ? C7 Zn1 N2 C30 -90.1(3) . . . . ? O3 Zn2 N3 C39 -95.8(3) . . . . ? O5 Zn2 N3 C39 158.4(3) . . . . ? N4 Zn2 N3 C39 8.1(3) . . . . ? O3 Zn2 N3 C35 77.3(4) . . . . ? O5 Zn2 N3 C35 -28.5(4) . . . . ? N4 Zn2 N3 C35 -178.8(4) . . . . ? O3 Zn2 N4 C44 -92.1(4) . . . . ? O5 Zn2 N4 C44 108.1(4) . . . . ? O2W Zn2 N4 C44 2.8(4) . . . . ? N3 Zn2 N4 C44 178.7(4) . . . . ? O3 Zn2 N4 C40 82.6(3) . . . . ? O5 Zn2 N4 C40 -77.2(4) . . . . ? O2W Zn2 N4 C40 177.5(3) . . . . ? N3 Zn2 N4 C40 -6.6(3) . . . . ? C6 C1 C2 C3 -1.0(6) . . . . ? C7 C1 C2 C3 -179.2(4) . . . . ? C1 C2 C3 C4 3.8(6) . . . . ? C1 C2 C3 C8 -175.2(4) . . . . ? C2 C3 C4 C5 -3.4(6) . . . . ? C8 C3 C4 C5 175.6(4) . . . . ? C3 C4 C5 C6 0.2(6) . . . . ? C3 C4 C5 C9 -179.9(4) . . . . ? C4 C5 C6 C1 2.7(6) . . . . ? C9 C5 C6 C1 -177.2(4) . . . . ? C2 C1 C6 C5 -2.4(6) . . . . ? C7 C1 C6 C5 175.9(4) . . . . ? Zn1 O2 C7 O1 -5.8(4) . . . . ? Zn1 O2 C7 C1 173.6(3) . . . . ? Zn1 O1 C7 O2 6.6(4) . . . . ? Zn1 O1 C7 C1 -172.8(3) . . . . ? C2 C1 C7 O2 25.3(6) . . . . ? C6 C1 C7 O2 -152.9(4) . . . . ? C2 C1 C7 O1 -155.2(4) . . . . ? C6 C1 C7 O1 26.5(5) . . . . ? O7 Zn1 C7 O2 -179.6(2) 2_666 . . . ? O1 Zn1 C7 O2 -173.9(4) . . . . ? N2 Zn1 C7 O2 -7.0(3) . . . . ? O1W Zn1 C7 O2 89.5(2) . . . . ? N1 Zn1 C7 O2 -86.7(2) . . . . ? O7 Zn1 C7 O1 -5.7(3) 2_666 . . . ? N2 Zn1 C7 O1 166.9(2) . . . . ? O1W Zn1 C7 O1 -96.6(3) . . . . ? N1 Zn1 C7 O1 87.1(3) . . . . ? O2 Zn1 C7 O1 173.9(4) . . . . ? Zn2 O3 C8 O4 0.1(7) . . . . ? Zn2 O3 C8 C3 178.0(3) . . . . ? C4 C3 C8 O4 7.3(6) . . . . ? C2 C3 C8 O4 -173.7(4) . . . . ? C4 C3 C8 O3 -170.8(4) . . . . ? C2 C3 C8 O3 8.2(6) . . . . ? C6 C5 C9 C10 129.0(5) . . . . ? C4 C5 C9 C10 -50.9(6) . . . . ? C6 C5 C9 C11 3.4(7) . . . . ? C4 C5 C9 C11 -176.5(5) . . . . ? C6 C5 C9 C12 -114.1(5) . . . . ? C4 C5 C9 C12 66.0(6) . . . . ? C18 C13 C14 C15 -0.9(6) . . . . ? C19 C13 C14 C15 176.5(3) . . . . ? C13 C14 C15 C16 1.8(6) . . . . ? C13 C14 C15 C20 -178.2(3) . . . . ? C14 C15 C16 C17 -1.8(6) . . . . ? C20 C15 C16 C17 178.1(4) . . . . ? C15 C16 C17 C18 0.9(6) . . . . ? C15 C16 C17 C21 179.8(4) . . . . ? C14 C13 C18 C17 0.0(6) . . . . ? C19 C13 C18 C17 -177.3(4) . . . . ? C16 C17 C18 C13 -0.1(6) . . . . ? C21 C17 C18 C13 -178.9(4) . . . . ? Zn1 O7 C19 O8 24.9(6) 2_666 . . . ? Zn1 O7 C19 C13 -154.0(3) 2_666 . . . ? C14 C13 C19 O8 -148.7(4) . . . . ? C18 C13 C19 O8 28.6(6) . . . . ? C14 C13 C19 O7 30.3(5) . . . . ? C18 C13 C19 O7 -152.4(4) . . . . ? Zn2 O5 C20 O6 2.5(5) . . . . ? Zn2 O5 C20 C15 -177.1(3) . . . . ? C14 C15 C20 O6 -167.4(4) . . . . ? C16 C15 C20 O6 12.7(6) . . . . ? C14 C15 C20 O5 12.2(6) . . . . ? C16 C15 C20 O5 -167.7(4) . . . . ? C16 C17 C21 C22' -169.0(19) . . . . ? C18 C17 C21 C22' 10(2) . . . . ? C16 C17 C21 C24 -1.3(9) . . . . ? C18 C17 C21 C24 177.6(7) . . . . ? C16 C17 C21 C23 128.4(7) . . . . ? C18 C17 C21 C23 -52.8(8) . . . . ? C16 C17 C21 C22 -118.2(6) . . . . ? C18 C17 C21 C22 60.7(7) . . . . ? C16 C17 C21 C24' 59.9(16) . . . . ? C18 C17 C21 C24' -121.3(15) . . . . ? C16 C17 C21 C23' -43.4(19) . . . . ? C18 C17 C21 C23' 135.4(18) . . . . ? C29 N1 C25 C26 -0.1(7) . . . . ? Zn1 N1 C25 C26 -175.9(4) . . . . ? N1 C25 C26 C27 -1.7(8) . . . . ? C25 C26 C27 C28 1.2(9) . . . . ? C26 C27 C28 C29 1.0(8) . . . . ? C25 N1 C29 C28 2.5(6) . . . . ? Zn1 N1 C29 C28 178.6(3) . . . . ? C25 N1 C29 C30 -174.9(4) . . . . ? Zn1 N1 C29 C30 1.2(4) . . . . ? C27 C28 C29 N1 -2.9(7) . . . . ? C27 C28 C29 C30 174.3(4) . . . . ? C34 N2 C30 C31 -1.2(6) . . . . ? Zn1 N2 C30 C31 179.5(3) . . . . ? C34 N2 C30 C29 177.2(4) . . . . ? Zn1 N2 C30 C29 -2.2(4) . . . . ? N1 C29 C30 N2 0.6(5) . . . . ? C28 C29 C30 N2 -176.7(4) . . . . ? N1 C29 C30 C31 178.9(4) . . . . ? C28 C29 C30 C31 1.6(6) . . . . ? N2 C30 C31 C32 1.1(7) . . . . ? C29 C30 C31 C32 -177.1(4) . . . . ? C30 C31 C32 C33 0.2(8) . . . . ? C31 C32 C33 C34 -1.3(8) . . . . ? C30 N2 C34 C33 0.0(7) . . . . ? Zn1 N2 C34 C33 179.2(4) . . . . ? C32 C33 C34 N2 1.3(8) . . . . ? C39 N3 C35 C36 -0.4(7) . . . . ? Zn2 N3 C35 C36 -173.4(4) . . . . ? N3 C35 C36 C37 1.4(9) . . . . ? C35 C36 C37 C38 -0.6(9) . . . . ? C36 C37 C38 C39 -1.0(9) . . . . ? C35 N3 C39 C38 -1.2(7) . . . . ? Zn2 N3 C39 C38 172.4(3) . . . . ? C35 N3 C39 C40 178.1(4) . . . . ? Zn2 N3 C39 C40 -8.3(5) . . . . ? C37 C38 C39 N3 2.0(8) . . . . ? C37 C38 C39 C40 -177.3(5) . . . . ? C44 N4 C40 C41 -0.4(6) . . . . ? Zn2 N4 C40 C41 -175.4(3) . . . . ? C44 N4 C40 C39 179.4(4) . . . . ? Zn2 N4 C40 C39 4.4(5) . . . . ? N3 C39 C40 N4 2.7(5) . . . . ? C38 C39 C40 N4 -178.0(4) . . . . ? N3 C39 C40 C41 -177.5(4) . . . . ? C38 C39 C40 C41 1.8(7) . . . . ? N4 C40 C41 C42 -0.2(7) . . . . ? C39 C40 C41 C42 180.0(4) . . . . ? C40 C41 C42 C43 0.7(8) . . . . ? C41 C42 C43 C44 -0.6(9) . . . . ? C40 N4 C44 C43 0.5(7) . . . . ? Zn2 N4 C44 C43 175.1(4) . . . . ? C42 C43 C44 N4 0.0(9) . . . . ? 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 O2W H2WB O4 0.86(4) 1.73(2) 2.564(5) 164(6) . O1W H1WA O8 0.85(4) 2.02(5) 2.818(4) 158(5) 1_445 O1W H1WB O8 0.85(4) 1.93(2) 2.749(4) 162(5) 2_666 O2W H2WA O6 0.85(4) 1.89(2) 2.714(5) 163(6) 2_665 _diffrn_measured_fraction_theta_max 0.895 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.514 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.081 #============================================================================== data_ZnPhen1a-{[Zn(phen)(tbip)(H2O)].H2O}n _database_code_depnum_ccdc_archive 'CCDC 835420' #TrackingRef '- revised cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H22 N2 O5 Zn, H2 O' _chemical_formula_sum 'C24 H24 N2 O6 Zn' _chemical_formula_weight 501.82 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 triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0401(4) _cell_length_b 10.1153(5) _cell_length_c 13.3557(5) _cell_angle_alpha 105.9573(15) _cell_angle_beta 93.6439(10) _cell_angle_gamma 95.9421(15) _cell_volume 1162.49(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8739 _cell_measurement_theta_min 6.25 _cell_measurement_theta_max 54.98 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 1.099 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8102 _exptl_absorpt_correction_T_max 0.8981 _exptl_absorpt_process_details 'Tompa_analytical (Rigaku Corporation, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Rigaku R-AXIS RAPID imaging plate' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11538 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0582 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5279 _reflns_number_gt 3754 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'PROCESS-AUTO (Rigaku Corporation,1998)' _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan (Molecular Structure Corporation & Rigaku Corporation, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. DFIX 0.85 0.01 is applied to the lattice water molecule O2w. ; _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^)+(0.0769P)^2^+0.9980P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5279 _refine_ls_number_parameters 307 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.1432 _refine_ls_wR_factor_gt 0.1016 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 Zn1 Zn 0.55196(4) 0.73961(4) 0.68288(3) 0.02230(14) Uani 1 1 d . . . O1W O 0.6079(3) 0.7058(3) 0.52839(18) 0.0326(6) Uani 1 1 d . . . H1A H 0.5505 0.6385 0.4889 0.049 Uiso 1 1 calc R . . H1B H 0.6126 0.7807 0.5124 0.049 Uiso 1 1 d R . . O1 O 0.7177(3) 0.6389(2) 0.7362(2) 0.0296(5) Uani 1 1 d . . . O2W O 0.6996(5) 0.9348(4) 0.4661(2) 0.0600(9) Uani 1 1 d D . . H2A H 0.639(5) 0.952(6) 0.421(4) 0.090 Uiso 1 1 d D . . H2B H 0.751(6) 1.005(4) 0.508(4) 0.090 Uiso 1 1 d D . . O2 O 0.5257(3) 0.4946(2) 0.64671(18) 0.0272(5) Uani 1 1 d . . . O3 O 0.4771(3) 0.0137(3) 0.6886(2) 0.0440(7) Uani 1 1 d . . . O4 O 0.6840(3) -0.0757(2) 0.71820(18) 0.0283(5) Uani 1 1 d . . . N1 N 0.3181(3) 0.7304(3) 0.6476(2) 0.0234(6) Uani 1 1 d . . . N2 N 0.4681(3) 0.7787(3) 0.8366(2) 0.0283(6) Uani 1 1 d . . . C1 C 0.7230(4) 0.3998(3) 0.7200(2) 0.0225(7) Uani 1 1 d . . . C2 C 0.6395(3) 0.2712(3) 0.7052(2) 0.0222(6) Uani 1 1 d . . . H2 H 0.5352 0.2593 0.6849 0.027 Uiso 1 1 calc R . . C3 C 0.7076(4) 0.1604(3) 0.7199(2) 0.0213(6) Uani 1 1 d . . . C4 C 0.8622(4) 0.1793(3) 0.7498(3) 0.0260(7) Uani 1 1 d . . . H4 H 0.9094 0.1029 0.7583 0.031 Uiso 1 1 calc R . . C5 C 0.9476(4) 0.3078(3) 0.7672(3) 0.0239(7) Uani 1 1 d . . . C6 C 0.8747(4) 0.4177(3) 0.7535(2) 0.0233(7) Uani 1 1 d . . . H6 H 0.9301 0.5070 0.7673 0.028 Uiso 1 1 calc R . . C7 C 0.6510(4) 0.5179(3) 0.6999(2) 0.0241(7) Uani 1 1 d . . . C8 C 0.6152(4) 0.0227(3) 0.7067(2) 0.0254(7) Uani 1 1 d . . . C9 C 1.1166(4) 0.3311(4) 0.8001(3) 0.0345(8) Uani 1 1 d . . . C10 C 1.1990(5) 0.3892(5) 0.7210(4) 0.0587(14) Uani 1 1 d . . . H10A H 1.3059 0.4106 0.7445 0.088 Uiso 1 1 calc R . . H10B H 1.1591 0.4739 0.7158 0.088 Uiso 1 1 calc R . . H10C H 1.1843 0.3202 0.6523 0.088 Uiso 1 1 calc R . . C11 C 1.1777(5) 0.1961(5) 0.8008(5) 0.0602(14) Uani 1 1 d . . . H11A H 1.1286 0.1565 0.8512 0.090 Uiso 1 1 calc R . . H11B H 1.2857 0.2149 0.8208 0.090 Uiso 1 1 calc R . . H11C H 1.1581 0.1303 0.7308 0.090 Uiso 1 1 calc R . . C12 C 1.1482(6) 0.4340(7) 0.9078(4) 0.0774(18) Uani 1 1 d . . . H12A H 1.1109 0.3909 0.9602 0.116 Uiso 1 1 calc R . . H12B H 1.0979 0.5158 0.9095 0.116 Uiso 1 1 calc R . . H12C H 1.2561 0.4620 0.9235 0.116 Uiso 1 1 calc R . . C13 C 0.2441(4) 0.7011(4) 0.5539(3) 0.0369(9) Uani 1 1 d . . . H13A H 0.2964 0.6716 0.4938 0.044 Uiso 1 1 calc R . . C14 C 0.0919(5) 0.7120(6) 0.5401(3) 0.0523(12) Uani 1 1 d . . . H14A H 0.0423 0.6877 0.4715 0.063 Uiso 1 1 calc R . . C15 C 0.0140(4) 0.7572(5) 0.6245(3) 0.0436(10) Uani 1 1 d . . . H15A H -0.0888 0.7674 0.6151 0.052 Uiso 1 1 calc R . . C16 C 0.0880(4) 0.7885(4) 0.7253(3) 0.0280(7) Uani 1 1 d . . . C17 C 0.0159(4) 0.8325(4) 0.8190(3) 0.0335(8) Uani 1 1 d . . . H17A H -0.0866 0.8457 0.8142 0.040 Uiso 1 1 calc R . . C18 C 0.0910(4) 0.8556(4) 0.9140(3) 0.0355(8) Uani 1 1 d . . . H18A H 0.0403 0.8837 0.9750 0.043 Uiso 1 1 calc R . . C19 C 0.2469(4) 0.8382(4) 0.9243(3) 0.0330(8) Uani 1 1 d . . . C20 C 0.3297(5) 0.8580(5) 1.0211(3) 0.0496(11) Uani 1 1 d . . . H20A H 0.2842 0.8863 1.0845 0.059 Uiso 1 1 calc R . . C21 C 0.4747(6) 0.8363(6) 1.0231(3) 0.0585(13) Uani 1 1 d . . . H21A H 0.5310 0.8473 1.0880 0.070 Uiso 1 1 calc R . . C22 C 0.5427(4) 0.7976(5) 0.9292(3) 0.0423(10) Uani 1 1 d . . . H22A H 0.6453 0.7846 0.9323 0.051 Uiso 1 1 calc R . . C23 C 0.3214(4) 0.7989(3) 0.8343(2) 0.0240(7) Uani 1 1 d . . . C24 C 0.2410(3) 0.7729(3) 0.7329(2) 0.0219(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0194(2) 0.0198(2) 0.0294(2) 0.00942(15) 0.00179(15) 0.00366(14) O1W 0.0362(14) 0.0306(14) 0.0312(12) 0.0108(11) 0.0068(11) -0.0027(11) O1 0.0271(12) 0.0164(12) 0.0445(14) 0.0088(10) -0.0008(11) 0.0016(10) O2W 0.083(3) 0.050(2) 0.0439(18) 0.0209(16) -0.0112(17) -0.0164(18) O2 0.0251(12) 0.0240(13) 0.0357(13) 0.0128(10) 0.0004(10) 0.0064(10) O3 0.0273(14) 0.0307(15) 0.077(2) 0.0244(14) -0.0031(14) -0.0013(11) O4 0.0315(13) 0.0153(12) 0.0388(13) 0.0102(10) -0.0011(11) 0.0023(9) N1 0.0214(13) 0.0226(15) 0.0250(13) 0.0057(11) -0.0005(11) 0.0019(11) N2 0.0231(14) 0.0375(18) 0.0273(14) 0.0127(13) 0.0020(12) 0.0086(12) C1 0.0237(16) 0.0203(16) 0.0268(15) 0.0107(13) 0.0062(13) 0.0043(13) C2 0.0177(15) 0.0253(17) 0.0244(15) 0.0086(13) 0.0009(13) 0.0028(12) C3 0.0261(16) 0.0169(16) 0.0215(14) 0.0058(12) 0.0056(13) 0.0022(12) C4 0.0266(17) 0.0229(17) 0.0332(17) 0.0125(14) 0.0059(14) 0.0098(13) C5 0.0219(16) 0.0231(17) 0.0288(16) 0.0098(14) 0.0055(13) 0.0033(13) C6 0.0220(16) 0.0193(16) 0.0288(16) 0.0070(13) 0.0047(13) 0.0015(12) C7 0.0239(16) 0.0249(18) 0.0272(16) 0.0110(14) 0.0092(14) 0.0063(13) C8 0.0302(18) 0.0212(17) 0.0252(16) 0.0072(13) 0.0019(14) 0.0033(13) C9 0.0215(17) 0.034(2) 0.051(2) 0.0164(18) 0.0030(16) 0.0057(15) C10 0.027(2) 0.062(3) 0.104(4) 0.051(3) 0.014(2) 0.005(2) C11 0.028(2) 0.057(3) 0.110(4) 0.044(3) -0.001(2) 0.013(2) C12 0.043(3) 0.101(5) 0.070(3) -0.002(3) -0.016(3) 0.014(3) C13 0.0284(19) 0.048(2) 0.0289(18) 0.0037(17) -0.0003(15) 0.0030(17) C14 0.029(2) 0.089(4) 0.034(2) 0.012(2) -0.0070(17) 0.006(2) C15 0.0222(18) 0.065(3) 0.044(2) 0.018(2) -0.0027(17) 0.0038(18) C16 0.0223(16) 0.0270(19) 0.0337(18) 0.0087(15) 0.0028(14) -0.0005(13) C17 0.0241(17) 0.030(2) 0.044(2) 0.0058(16) 0.0066(16) 0.0010(15) C18 0.0309(19) 0.038(2) 0.0356(19) 0.0054(17) 0.0125(16) 0.0050(16) C19 0.037(2) 0.035(2) 0.0276(17) 0.0088(15) 0.0061(15) 0.0066(16) C20 0.050(3) 0.069(3) 0.0271(19) 0.009(2) 0.0047(18) 0.012(2) C21 0.059(3) 0.092(4) 0.0253(19) 0.015(2) -0.0032(19) 0.021(3) C22 0.032(2) 0.062(3) 0.0320(19) 0.0119(19) -0.0062(16) 0.0117(19) C23 0.0248(16) 0.0214(17) 0.0247(15) 0.0054(13) 0.0019(13) 0.0022(13) C24 0.0200(15) 0.0189(16) 0.0259(15) 0.0058(13) 0.0021(13) 0.0000(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 O4 2.029(2) 1_565 ? Zn1 O1 2.091(2) . ? Zn1 O1W 2.100(2) . ? Zn1 N1 2.123(3) . ? Zn1 N2 2.182(3) . ? Zn1 O2 2.374(2) . ? Zn1 C7 2.560(3) . ? O1W H1A 0.8400 . ? O1W H1B 0.8400 . ? O1 C7 1.257(4) . ? O2W H2A 0.85(5) . ? O2W H2B 0.85(5) . ? O2 C7 1.263(4) . ? O3 C8 1.245(4) . ? O4 C8 1.266(4) . ? O4 Zn1 2.029(2) 1_545 ? N1 C13 1.323(4) . ? N1 C24 1.365(4) . ? N2 C22 1.326(4) . ? N2 C23 1.362(4) . ? C1 C6 1.392(4) . ? C1 C2 1.393(4) . ? C1 C7 1.496(4) . ? C2 C3 1.386(4) . ? C2 H2 0.9500 . ? C3 C4 1.408(5) . ? C3 C8 1.508(5) . ? C4 C5 1.394(5) . ? C4 H4 0.9500 . ? C5 C6 1.397(4) . ? C5 C9 1.538(5) . ? C6 H6 0.9500 . ? C9 C12 1.516(7) . ? C9 C11 1.527(5) . ? C9 C10 1.538(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.396(5) . ? C13 H13A 0.9500 . ? C14 C15 1.364(6) . ? C14 H14A 0.9500 . ? C15 C16 1.403(5) . ? C15 H15A 0.9500 . ? C16 C24 1.409(4) . ? C16 C17 1.430(5) . ? C17 C18 1.350(5) . ? C17 H17A 0.9500 . ? C18 C19 1.441(5) . ? C18 H18A 0.9500 . ? C19 C23 1.397(5) . ? C19 C20 1.405(5) . ? C20 C21 1.352(6) . ? C20 H20A 0.9500 . ? C21 C22 1.407(6) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C24 1.440(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 O4 Zn1 O1 93.70(9) 1_565 . ? O4 Zn1 O1W 87.56(10) 1_565 . ? O1 Zn1 O1W 97.79(10) . . ? O4 Zn1 N1 119.87(10) 1_565 . ? O1 Zn1 N1 144.00(10) . . ? O1W Zn1 N1 96.34(10) . . ? O4 Zn1 N2 94.39(11) 1_565 . ? O1 Zn1 N2 88.49(10) . . ? O1W Zn1 N2 173.30(10) . . ? N1 Zn1 N2 77.12(10) . . ? O4 Zn1 O2 150.04(9) 1_565 . ? O1 Zn1 O2 58.53(9) . . ? O1W Zn1 O2 85.64(9) . . ? N1 Zn1 O2 89.89(9) . . ? N2 Zn1 O2 95.74(10) . . ? O4 Zn1 C7 122.32(10) 1_565 . ? O1 Zn1 C7 29.20(10) . . ? O1W Zn1 C7 92.58(10) . . ? N1 Zn1 C7 117.40(11) . . ? N2 Zn1 C7 91.80(10) . . ? O2 Zn1 C7 29.34(9) . . ? Zn1 O1W H1A 109.5 . . ? Zn1 O1W H1B 109.5 . . ? H1A O1W H1B 116.8 . . ? C7 O1 Zn1 96.6(2) . . ? H2A O2W H2B 115(6) . . ? C7 O2 Zn1 83.52(19) . . ? C8 O4 Zn1 113.4(2) . 1_545 ? C13 N1 C24 117.9(3) . . ? C13 N1 Zn1 127.3(2) . . ? C24 N1 Zn1 114.5(2) . . ? C22 N2 C23 117.8(3) . . ? C22 N2 Zn1 129.0(2) . . ? C23 N2 Zn1 112.8(2) . . ? C6 C1 C2 119.4(3) . . ? C6 C1 C7 120.1(3) . . ? C2 C1 C7 120.5(3) . . ? C3 C2 C1 120.4(3) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C2 C3 C4 119.3(3) . . ? C2 C3 C8 119.9(3) . . ? C4 C3 C8 120.8(3) . . ? C5 C4 C3 121.3(3) . . ? C5 C4 H4 119.3 . . ? C3 C4 H4 119.3 . . ? C4 C5 C6 117.8(3) . . ? C4 C5 C9 122.3(3) . . ? C6 C5 C9 119.9(3) . . ? C1 C6 C5 121.7(3) . . ? C1 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? O1 C7 O2 121.3(3) . . ? O1 C7 C1 118.9(3) . . ? O2 C7 C1 119.8(3) . . ? O1 C7 Zn1 54.23(16) . . ? O2 C7 Zn1 67.14(17) . . ? C1 C7 Zn1 172.9(2) . . ? O3 C8 O4 124.2(3) . . ? O3 C8 C3 118.6(3) . . ? O4 C8 C3 117.1(3) . . ? C12 C9 C11 109.8(4) . . ? C12 C9 C10 109.4(4) . . ? C11 C9 C10 107.1(3) . . ? C12 C9 C5 109.4(3) . . ? C11 C9 C5 111.9(3) . . ? C10 C9 C5 109.2(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C14 122.4(3) . . ? N1 C13 H13A 118.8 . . ? C14 C13 H13A 118.8 . . ? C15 C14 C13 120.4(4) . . ? C15 C14 H14A 119.8 . . ? C13 C14 H14A 119.8 . . ? C14 C15 C16 119.0(4) . . ? C14 C15 H15A 120.5 . . ? C16 C15 H15A 120.5 . . ? C15 C16 C24 117.2(3) . . ? C15 C16 C17 123.6(3) . . ? C24 C16 C17 119.2(3) . . ? C18 C17 C16 121.1(3) . . ? C18 C17 H17A 119.5 . . ? C16 C17 H17A 119.5 . . ? C17 C18 C19 121.0(3) . . ? C17 C18 H18A 119.5 . . ? C19 C18 H18A 119.5 . . ? C23 C19 C20 117.4(3) . . ? C23 C19 C18 119.2(3) . . ? C20 C19 C18 123.4(3) . . ? C21 C20 C19 119.2(4) . . ? C21 C20 H20A 120.4 . . ? C19 C20 H20A 120.4 . . ? C20 C21 C22 120.2(4) . . ? C20 C21 H21A 119.9 . . ? C22 C21 H21A 119.9 . . ? N2 C22 C21 122.1(4) . . ? N2 C22 H22A 119.0 . . ? C21 C22 H22A 119.0 . . ? N2 C23 C19 123.2(3) . . ? N2 C23 C24 117.0(3) . . ? C19 C23 C24 119.8(3) . . ? N1 C24 C16 123.0(3) . . ? N1 C24 C23 117.3(3) . . ? C16 C24 C23 119.6(3) . . ? 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 O1W H1B O2W 0.84 1.94 2.737(4) 158.0 . O1W H1A O2 0.84 1.97 2.751(3) 154.4 2_666 O2W H2A O3 0.85(5) 1.88(5) 2.727(4) 173(6) 2_666 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.214 _refine_diff_density_min -0.956 _refine_diff_density_rms 0.112 #============================================================================== data_ZnPhen1b-[Zn(tbip)(H2tbip)(phen)]n _database_code_depnum_ccdc_archive 'CCDC 835421' #TrackingRef '- revised cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H34 N2 O8 Zn' _chemical_formula_sum 'C36 H34 N2 O8 Zn' _chemical_formula_weight 688.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.991(2) _cell_length_b 14.254(3) _cell_length_c 11.361(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.93(3) _cell_angle_gamma 90.00 _cell_volume 1683.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 13639 _cell_measurement_theta_min 6.27 _cell_measurement_theta_max 55.02 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716 _exptl_absorpt_coefficient_mu 0.783 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6955 _exptl_absorpt_correction_T_max 0.7990 _exptl_absorpt_process_details 'Tompa_analytical (Rigaku Corporation, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Rigaku R-AXIS RAPID imaging plate' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16450 _diffrn_reflns_av_R_equivalents 0.0642 _diffrn_reflns_av_sigmaI/netI 0.0948 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 27.47 _reflns_number_total 7607 _reflns_number_gt 6225 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'PROCESS-AUTO (Rigaku Corporation,1998)' _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan (Molecular Structure Corporation & Rigaku Corporation, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.025(10) _refine_ls_number_reflns 7607 _refine_ls_number_parameters 430 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0632 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1225 _refine_ls_wR_factor_gt 0.1043 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.11873(3) 0.71206(3) 0.36521(3) 0.02572(11) Uani 1 1 d . . . O1 O 0.00690(19) 0.62507(18) 0.2443(2) 0.0267(5) Uani 1 1 d . . . O2 O 0.1195(2) 0.61836(19) 0.1099(2) 0.0312(6) Uani 1 1 d . . . O3 O 0.0493(2) 0.3242(2) -0.1202(2) 0.0358(6) Uani 1 1 d . . . O4 O -0.1513(2) 0.29996(18) -0.2504(2) 0.0277(5) Uani 1 1 d . . . O5 O 0.31836(19) 0.64488(18) 0.3967(2) 0.0299(6) Uani 1 1 d . . . O6 O 0.3520(2) 0.6633(2) 0.2146(2) 0.0388(7) Uani 1 1 d . . . H6B H 0.2741 0.6481 0.1858 0.058 Uiso 1 1 calc R . . O7 O 0.7798(2) 0.7628(2) 0.2080(2) 0.0332(6) Uani 1 1 d . . . H7A H 0.8357 0.7828 0.1783 0.050 Uiso 1 1 calc R . . O8 O 0.9331(2) 0.79195(19) 0.3893(2) 0.0314(6) Uani 1 1 d . . . N1 N 0.2025(2) 0.8071(2) 0.5041(3) 0.0260(6) Uani 1 1 d . . . N2 N 0.1052(2) 0.6379(2) 0.5120(3) 0.0249(6) Uani 1 1 d . . . C1 C -0.0775(3) 0.5406(2) 0.0528(3) 0.0243(7) Uani 1 1 d . . . C2 C -0.0357(3) 0.4716(3) -0.0088(3) 0.0253(7) Uani 1 1 d . . . H2A H 0.0540 0.4630 0.0079 0.030 Uiso 1 1 calc R . . C3 C -0.1216(3) 0.4139(3) -0.0950(3) 0.0243(7) Uani 1 1 d . . . C4 C -0.2521(3) 0.4281(3) -0.1200(3) 0.0247(7) Uani 1 1 d . . . H4A H -0.3111 0.3896 -0.1803 0.030 Uiso 1 1 calc R . . C5 C -0.3007(3) 0.4979(3) -0.0588(3) 0.0261(7) Uani 1 1 d . . . C6 C -0.2108(3) 0.5532(2) 0.0299(3) 0.0244(7) Uani 1 1 d . . . H6A H -0.2397 0.5995 0.0749 0.029 Uiso 1 1 calc R . . C7 C 0.0247(3) 0.6003(2) 0.1423(3) 0.0225(7) Uani 1 1 d . . . C8 C -0.0697(3) 0.3401(3) -0.1592(3) 0.0265(8) Uani 1 1 d . . . C9 C -0.4455(3) 0.5090(3) -0.0919(4) 0.0361(9) Uani 1 1 d . . . C10 C -0.4828(4) 0.5915(3) -0.0231(4) 0.0493(12) Uani 1 1 d . . . H10A H -0.4513 0.5795 0.0667 0.074 Uiso 1 1 calc R . . H10B H -0.5767 0.5980 -0.0511 0.074 Uiso 1 1 calc R . . H10C H -0.4443 0.6495 -0.0411 0.074 Uiso 1 1 calc R . . C11 C -0.5022(4) 0.4182(4) -0.0541(5) 0.0524(12) Uani 1 1 d . . . H11A H -0.4704 0.4114 0.0366 0.079 Uiso 1 1 calc R . . H11B H -0.4756 0.3637 -0.0924 0.079 Uiso 1 1 calc R . . H11C H -0.5963 0.4222 -0.0828 0.079 Uiso 1 1 calc R . . C12 C -0.5101(4) 0.5241(4) -0.2320(4) 0.0541(13) Uani 1 1 d . . . H12A H -0.4721 0.5790 -0.2588 0.081 Uiso 1 1 calc R . . H12B H -0.6025 0.5346 -0.2496 0.081 Uiso 1 1 calc R . . H12C H -0.4972 0.4685 -0.2772 0.081 Uiso 1 1 calc R . . C13 C 0.5165(3) 0.7075(3) 0.3959(3) 0.0273(6) Uani 1 1 d . . . C14 C 0.6023(3) 0.7206(3) 0.3306(3) 0.0271(7) Uani 1 1 d . . . H14A H 0.5787 0.7043 0.2450 0.033 Uiso 1 1 calc R . . C15 C 0.7232(3) 0.7580(3) 0.3921(3) 0.0292(8) Uani 1 1 d . . . C16 C 0.7562(3) 0.7836(3) 0.5185(3) 0.0309(8) Uani 1 1 d . . . H16A H 0.8397 0.8076 0.5602 0.037 Uiso 1 1 calc R . . C17 C 0.6703(3) 0.7747(3) 0.5831(3) 0.0318(8) Uani 1 1 d . . . C18 C 0.5504(3) 0.7350(3) 0.5211(3) 0.0308(9) Uani 1 1 d . . . H18A H 0.4906 0.7265 0.5646 0.037 Uiso 1 1 calc R . . C19 C 0.3862(3) 0.6689(3) 0.3360(3) 0.0289(7) Uani 1 1 d . . . C20 C 0.8224(3) 0.7720(3) 0.3306(3) 0.0284(7) Uani 1 1 d . . . C21 C 0.7087(3) 0.8096(3) 0.7194(3) 0.0366(9) Uani 1 1 d . . . C22 C 0.5952(4) 0.8067(5) 0.7682(5) 0.083(2) Uani 1 1 d . . . H22A H 0.6233 0.8271 0.8553 0.124 Uiso 1 1 calc R . . H22B H 0.5620 0.7425 0.7625 0.124 Uiso 1 1 calc R . . H22C H 0.5273 0.8486 0.7184 0.124 Uiso 1 1 calc R . . C23 C 0.7529(7) 0.9111(4) 0.7242(5) 0.089(2) Uani 1 1 d . . . H23A H 0.8432 0.9128 0.7281 0.133 Uiso 1 1 calc R . . H23B H 0.7437 0.9417 0.7981 0.133 Uiso 1 1 calc R . . H23C H 0.7001 0.9441 0.6493 0.133 Uiso 1 1 calc R . . C24 C 0.8128(5) 0.7473(5) 0.7998(4) 0.078(2) Uani 1 1 d . . . H24A H 0.8850 0.7458 0.7671 0.117 Uiso 1 1 calc R . . H24B H 0.7790 0.6837 0.7998 0.117 Uiso 1 1 calc R . . H24C H 0.8423 0.7718 0.8850 0.117 Uiso 1 1 calc R . . C25 C 0.2475(3) 0.8916(3) 0.4950(3) 0.0327(8) Uani 1 1 d . . . H25A H 0.2597 0.9091 0.4189 0.039 Uiso 1 1 calc R . . C26 C 0.2781(4) 0.9566(3) 0.5924(4) 0.0430(10) Uani 1 1 d . . . H26A H 0.3098 1.0171 0.5825 0.052 Uiso 1 1 calc R . . C27 C 0.2612(4) 0.9310(3) 0.7034(4) 0.0441(10) Uani 1 1 d . . . H27A H 0.2791 0.9746 0.7701 0.053 Uiso 1 1 calc R . . C28 C 0.2178(3) 0.8408(3) 0.7175(4) 0.0373(9) Uani 1 1 d . . . C29 C 0.2022(4) 0.8063(4) 0.8299(4) 0.0464(11) Uani 1 1 d . . . H29A H 0.2216 0.8461 0.9007 0.056 Uiso 1 1 calc R . . C30 C 0.1599(3) 0.7172(4) 0.8373(3) 0.0466(10) Uani 1 1 d . . . H30A H 0.1523 0.6951 0.9135 0.056 Uiso 1 1 calc R . . C31 C 0.1267(3) 0.6564(3) 0.7304(3) 0.0341(9) Uani 1 1 d . . . C32 C 0.0798(4) 0.5641(3) 0.7307(4) 0.0471(11) Uani 1 1 d . . . H32A H 0.0691 0.5383 0.8038 0.057 Uiso 1 1 calc R . . C33 C 0.0498(4) 0.5122(3) 0.6225(4) 0.0439(10) Uani 1 1 d . . . H33A H 0.0222 0.4489 0.6216 0.053 Uiso 1 1 calc R . . C34 C 0.0600(4) 0.5520(3) 0.5161(4) 0.0355(9) Uani 1 1 d . . . H34A H 0.0332 0.5163 0.4414 0.043 Uiso 1 1 calc R . . C35 C 0.1395(3) 0.6887(2) 0.6186(3) 0.0267(8) Uani 1 1 d . . . C36 C 0.1877(3) 0.7812(3) 0.6134(3) 0.0248(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02594(18) 0.0245(2) 0.02588(18) -0.00066(18) 0.00718(14) -0.00365(17) O1 0.0253(11) 0.0269(13) 0.0289(12) -0.0025(11) 0.0103(9) -0.0027(10) O2 0.0264(11) 0.0380(16) 0.0287(12) -0.0098(11) 0.0082(10) -0.0088(11) O3 0.0231(12) 0.0459(18) 0.0380(14) -0.0125(13) 0.0094(11) 0.0011(12) O4 0.0270(11) 0.0269(13) 0.0259(12) -0.0056(10) 0.0039(9) 0.0017(10) O5 0.0206(10) 0.0328(15) 0.0382(14) -0.0001(11) 0.0120(10) -0.0027(10) O6 0.0253(11) 0.0569(19) 0.0348(13) -0.0116(13) 0.0108(10) -0.0127(12) O7 0.0217(10) 0.0440(16) 0.0352(14) -0.0004(12) 0.0111(10) -0.0051(11) O8 0.0187(11) 0.0350(15) 0.0405(14) -0.0016(12) 0.0094(10) -0.0043(10) N1 0.0201(13) 0.0234(15) 0.0294(14) -0.0015(12) 0.0008(11) -0.0017(12) N2 0.0253(13) 0.0212(15) 0.0277(14) 0.0019(12) 0.0078(11) -0.0008(12) C1 0.0252(15) 0.0270(19) 0.0222(15) -0.0018(14) 0.0100(13) -0.0043(14) C2 0.0241(16) 0.0264(19) 0.0242(16) -0.0036(14) 0.0063(14) -0.0043(15) C3 0.0253(16) 0.0267(19) 0.0227(16) 0.0012(14) 0.0102(13) -0.0033(14) C4 0.0238(15) 0.0242(18) 0.0240(16) -0.0035(14) 0.0047(13) -0.0025(14) C5 0.0251(16) 0.0274(19) 0.0245(16) 0.0010(14) 0.0061(13) -0.0005(14) C6 0.0266(15) 0.0206(17) 0.0268(16) -0.0004(13) 0.0098(13) 0.0012(14) C7 0.0256(16) 0.0210(18) 0.0231(16) -0.0014(14) 0.0110(13) -0.0025(14) C8 0.0287(17) 0.0239(19) 0.0259(17) -0.0018(15) 0.0075(14) 0.0001(15) C9 0.0235(17) 0.042(2) 0.040(2) -0.0121(18) 0.0070(15) 0.0021(17) C10 0.0311(19) 0.057(3) 0.057(3) -0.018(2) 0.0106(18) 0.014(2) C11 0.0277(18) 0.059(3) 0.072(3) -0.008(3) 0.018(2) -0.011(2) C12 0.036(2) 0.076(4) 0.040(2) -0.008(2) -0.0027(19) 0.014(2) C13 0.0224(13) 0.0243(17) 0.0330(15) 0.0007(19) 0.0059(12) 0.0017(18) C14 0.0175(12) 0.032(2) 0.0305(15) -0.0003(19) 0.0065(11) -0.0008(16) C15 0.0229(15) 0.0277(19) 0.0359(19) -0.0022(16) 0.0080(14) -0.0004(15) C16 0.0230(15) 0.030(2) 0.0380(19) -0.0023(16) 0.0073(14) -0.0056(15) C17 0.0290(16) 0.030(2) 0.0340(18) -0.0069(16) 0.0067(15) -0.0017(15) C18 0.0233(15) 0.036(2) 0.0358(18) -0.0005(15) 0.0130(14) -0.0018(14) C19 0.0276(16) 0.0270(18) 0.0331(18) 0.0003(15) 0.0114(15) 0.0031(15) C20 0.0228(15) 0.0218(18) 0.0399(19) 0.0019(15) 0.0092(14) 0.0000(14) C21 0.0318(18) 0.046(2) 0.0322(19) -0.0104(18) 0.0105(15) -0.0057(18) C22 0.052(3) 0.160(7) 0.042(3) -0.041(4) 0.024(2) -0.022(4) C23 0.148(6) 0.058(4) 0.054(3) -0.025(3) 0.022(4) -0.028(4) C24 0.079(3) 0.122(6) 0.032(2) 0.001(3) 0.015(2) 0.032(4) C25 0.0304(17) 0.026(2) 0.0367(19) -0.0026(16) 0.0044(15) -0.0070(16) C26 0.048(2) 0.028(2) 0.053(2) -0.0100(18) 0.018(2) -0.0102(18) C27 0.045(2) 0.039(2) 0.045(2) -0.019(2) 0.0107(19) -0.011(2) C28 0.0304(17) 0.045(2) 0.035(2) -0.0133(18) 0.0080(16) -0.0014(18) C29 0.044(2) 0.067(3) 0.032(2) -0.016(2) 0.0181(18) -0.005(2) C30 0.0415(19) 0.073(3) 0.0257(16) -0.003(2) 0.0115(15) 0.001(3) C31 0.0297(17) 0.043(2) 0.0284(18) 0.0076(16) 0.0083(14) 0.0020(17) C32 0.044(2) 0.053(3) 0.048(2) 0.018(2) 0.0208(19) 0.000(2) C33 0.044(2) 0.029(2) 0.056(3) 0.016(2) 0.013(2) -0.004(2) C34 0.041(2) 0.024(2) 0.040(2) -0.0036(16) 0.0120(17) -0.0032(17) C35 0.0241(14) 0.030(2) 0.0252(15) 0.0000(14) 0.0069(13) 0.0020(14) C36 0.0219(15) 0.0275(19) 0.0252(17) -0.0007(14) 0.0077(13) 0.0022(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 Zn1 O4 1.925(2) 2 ? Zn1 O1 1.959(2) . ? Zn1 N2 2.021(3) . ? Zn1 N1 2.057(3) . ? Zn1 O5 2.313(2) . ? Zn1 O8 2.428(2) 1_455 ? O1 C7 1.286(4) . ? O2 C7 1.240(4) . ? O3 C8 1.258(4) . ? O4 C8 1.266(4) . ? O4 Zn1 1.925(2) 2_545 ? O5 C19 1.217(4) . ? O6 C19 1.309(4) . ? O6 H6B 0.8400 . ? O7 C20 1.325(4) . ? O7 H7A 0.8400 . ? O8 C20 1.216(4) . ? O8 Zn1 2.428(2) 1_655 ? N1 C25 1.318(5) . ? N1 C36 1.355(4) . ? N2 C34 1.327(5) . ? N2 C35 1.355(4) . ? C1 C2 1.369(5) . ? C1 C6 1.414(4) . ? C1 C7 1.510(4) . ? C2 C3 1.389(5) . ? C2 H2A 0.9500 . ? C3 C4 1.384(4) . ? C3 C8 1.494(5) . ? C4 C5 1.414(5) . ? C4 H4A 0.9500 . ? C5 C6 1.403(5) . ? C5 C9 1.520(5) . ? C6 H6A 0.9500 . ? C9 C12 1.533(5) . ? C9 C10 1.539(5) . ? C9 C11 1.557(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.389(4) . ? C13 C18 1.404(4) . ? C13 C19 1.479(4) . ? C14 C15 1.391(4) . ? C14 H14A 0.9500 . ? C15 C16 1.411(5) . ? C15 C20 1.487(5) . ? C16 C17 1.376(5) . ? C16 H16A 0.9500 . ? C17 C18 1.396(5) . ? C17 C21 1.549(5) . ? C18 H18A 0.9500 . ? C21 C24 1.501(6) . ? C21 C23 1.521(7) . ? C21 C22 1.521(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.398(5) . ? C25 H25A 0.9500 . ? C26 C27 1.382(6) . ? C26 H26A 0.9500 . ? C27 C28 1.398(6) . ? C27 H27A 0.9500 . ? C28 C36 1.407(5) . ? C28 C29 1.430(6) . ? C29 C30 1.364(7) . ? C29 H29A 0.9500 . ? C30 C31 1.439(6) . ? C30 H30A 0.9500 . ? C31 C35 1.399(5) . ? C31 C32 1.415(6) . ? C32 C33 1.380(6) . ? C32 H32A 0.9500 . ? C33 C34 1.373(6) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? C35 C36 1.429(5) . ? 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 O4 Zn1 O1 98.58(10) 2 . ? O4 Zn1 N2 168.52(11) 2 . ? O1 Zn1 N2 92.88(10) . . ? O4 Zn1 N1 87.46(11) 2 . ? O1 Zn1 N1 167.82(10) . . ? N2 Zn1 N1 81.14(12) . . ? O4 Zn1 O5 89.91(9) 2 . ? O1 Zn1 O5 101.20(9) . . ? N2 Zn1 O5 88.62(10) . . ? N1 Zn1 O5 89.31(10) . . ? O4 Zn1 O8 96.84(10) 2 1_455 ? O1 Zn1 O8 90.96(9) . 1_455 ? N2 Zn1 O8 82.12(10) . 1_455 ? N1 Zn1 O8 77.76(10) . 1_455 ? O5 Zn1 O8 165.09(8) . 1_455 ? C7 O1 Zn1 124.1(2) . . ? C8 O4 Zn1 127.6(2) . 2_545 ? C19 O5 Zn1 121.3(2) . . ? C19 O6 H6B 109.5 . . ? C20 O7 H7A 109.5 . . ? C20 O8 Zn1 123.8(2) . 1_655 ? C25 N1 C36 118.8(3) . . ? C25 N1 Zn1 128.8(3) . . ? C36 N1 Zn1 111.4(2) . . ? C34 N2 C35 117.4(3) . . ? C34 N2 Zn1 129.8(3) . . ? C35 N2 Zn1 112.6(2) . . ? C2 C1 C6 119.8(3) . . ? C2 C1 C7 116.7(3) . . ? C6 C1 C7 123.5(3) . . ? C1 C2 C3 121.4(3) . . ? C1 C2 H2A 119.3 . . ? C3 C2 H2A 119.3 . . ? C4 C3 C2 118.7(3) . . ? C4 C3 C8 122.5(3) . . ? C2 C3 C8 118.8(3) . . ? C3 C4 C5 122.3(3) . . ? C3 C4 H4A 118.9 . . ? C5 C4 H4A 118.9 . . ? C6 C5 C4 117.3(3) . . ? C6 C5 C9 123.8(3) . . ? C4 C5 C9 119.0(3) . . ? C5 C6 C1 120.5(3) . . ? C5 C6 H6A 119.8 . . ? C1 C6 H6A 119.8 . . ? O2 C7 O1 126.8(3) . . ? O2 C7 C1 115.5(3) . . ? O1 C7 C1 117.7(3) . . ? O3 C8 O4 125.9(3) . . ? O3 C8 C3 118.2(3) . . ? O4 C8 C3 115.9(3) . . ? C5 C9 C12 111.5(3) . . ? C5 C9 C10 112.6(3) . . ? C12 C9 C10 108.1(4) . . ? C5 C9 C11 109.0(3) . . ? C12 C9 C11 108.1(4) . . ? C10 C9 C11 107.4(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 120.1(3) . . ? C14 C13 C19 121.9(3) . . ? C18 C13 C19 118.0(3) . . ? C13 C14 C15 119.1(3) . . ? C13 C14 H14A 120.5 . . ? C15 C14 H14A 120.5 . . ? C14 C15 C16 119.9(3) . . ? C14 C15 C20 122.8(3) . . ? C16 C15 C20 117.3(3) . . ? C17 C16 C15 121.7(3) . . ? C17 C16 H16A 119.2 . . ? C15 C16 H16A 119.2 . . ? C16 C17 C18 117.8(3) . . ? C16 C17 C21 119.5(3) . . ? C18 C17 C21 122.7(3) . . ? C17 C18 C13 121.4(3) . . ? C17 C18 H18A 119.3 . . ? C13 C18 H18A 119.3 . . ? O5 C19 O6 124.1(3) . . ? O5 C19 C13 121.6(3) . . ? O6 C19 C13 114.3(3) . . ? O8 C20 O7 123.3(3) . . ? O8 C20 C15 122.0(3) . . ? O7 C20 C15 114.7(3) . . ? C24 C21 C23 111.7(4) . . ? C24 C21 C22 108.4(4) . . ? C23 C21 C22 107.6(5) . . ? C24 C21 C17 108.9(4) . . ? C23 C21 C17 108.7(4) . . ? C22 C21 C17 111.5(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N1 C25 C26 122.9(4) . . ? N1 C25 H25A 118.6 . . ? C26 C25 H25A 118.6 . . ? C27 C26 C25 118.6(4) . . ? C27 C26 H26A 120.7 . . ? C25 C26 H26A 120.7 . . ? C26 C27 C28 119.9(4) . . ? C26 C27 H27A 120.0 . . ? C28 C27 H27A 120.0 . . ? C27 C28 C36 117.1(4) . . ? C27 C28 C29 124.3(4) . . ? C36 C28 C29 118.6(4) . . ? C30 C29 C28 121.1(4) . . ? C30 C29 H29A 119.4 . . ? C28 C29 H29A 119.4 . . ? C29 C30 C31 120.4(4) . . ? C29 C30 H30A 119.8 . . ? C31 C30 H30A 119.8 . . ? C35 C31 C32 116.9(4) . . ? C35 C31 C30 119.7(4) . . ? C32 C31 C30 123.4(4) . . ? C33 C32 C31 118.6(4) . . ? C33 C32 H32A 120.7 . . ? C31 C32 H32A 120.7 . . ? C34 C33 C32 119.9(4) . . ? C34 C33 H33A 120.0 . . ? C32 C33 H33A 120.0 . . ? N2 C34 C33 123.4(4) . . ? N2 C34 H34A 118.3 . . ? C33 C34 H34A 118.3 . . ? N2 C35 C31 123.7(3) . . ? N2 C35 C36 117.1(3) . . ? C31 C35 C36 119.3(3) . . ? N1 C36 C28 122.7(3) . . ? N1 C36 C35 116.6(3) . . ? C28 C36 C35 120.8(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Zn1 O1 C7 39.4(3) 2 . . . ? N2 Zn1 O1 C7 -141.3(3) . . . . ? N1 Zn1 O1 C7 158.5(5) . . . . ? O5 Zn1 O1 C7 -52.2(3) . . . . ? O8 Zn1 O1 C7 136.5(3) 1_455 . . . ? O4 Zn1 O5 C19 -6.0(3) 2 . . . ? O1 Zn1 O5 C19 92.7(3) . . . . ? N2 Zn1 O5 C19 -174.6(3) . . . . ? N1 Zn1 O5 C19 -93.5(3) . . . . ? O8 Zn1 O5 C19 -123.2(4) 1_455 . . . ? O4 Zn1 N1 C25 2.8(3) 2 . . . ? O1 Zn1 N1 C25 -117.4(5) . . . . ? N2 Zn1 N1 C25 -178.6(3) . . . . ? O5 Zn1 N1 C25 92.7(3) . . . . ? O8 Zn1 N1 C25 -94.8(3) 1_455 . . . ? O4 Zn1 N1 C36 171.4(2) 2 . . . ? O1 Zn1 N1 C36 51.3(6) . . . . ? N2 Zn1 N1 C36 -9.9(2) . . . . ? O5 Zn1 N1 C36 -98.6(2) . . . . ? O8 Zn1 N1 C36 73.9(2) 1_455 . . . ? O4 Zn1 N2 C34 -170.9(5) 2 . . . ? O1 Zn1 N2 C34 13.0(3) . . . . ? N1 Zn1 N2 C34 -177.7(3) . . . . ? O5 Zn1 N2 C34 -88.2(3) . . . . ? O8 Zn1 N2 C34 103.5(3) 1_455 . . . ? O4 Zn1 N2 C35 14.6(7) 2 . . . ? O1 Zn1 N2 C35 -161.5(2) . . . . ? N1 Zn1 N2 C35 7.8(2) . . . . ? O5 Zn1 N2 C35 97.3(2) . . . . ? O8 Zn1 N2 C35 -71.0(2) 1_455 . . . ? C6 C1 C2 C3 0.8(5) . . . . ? C7 C1 C2 C3 -178.7(3) . . . . ? C1 C2 C3 C4 1.0(5) . . . . ? C1 C2 C3 C8 179.9(3) . . . . ? C2 C3 C4 C5 -1.4(5) . . . . ? C8 C3 C4 C5 179.9(3) . . . . ? C3 C4 C5 C6 -0.1(5) . . . . ? C3 C4 C5 C9 179.9(3) . . . . ? C4 C5 C6 C1 2.0(5) . . . . ? C9 C5 C6 C1 -178.0(3) . . . . ? C2 C1 C6 C5 -2.4(5) . . . . ? C7 C1 C6 C5 177.1(3) . . . . ? Zn1 O1 C7 O2 8.0(5) . . . . ? Zn1 O1 C7 C1 -173.8(2) . . . . ? C2 C1 C7 O2 36.4(5) . . . . ? C6 C1 C7 O2 -143.1(3) . . . . ? C2 C1 C7 O1 -142.0(3) . . . . ? C6 C1 C7 O1 38.6(5) . . . . ? Zn1 O4 C8 O3 -6.0(6) 2_545 . . . ? Zn1 O4 C8 C3 172.9(2) 2_545 . . . ? C4 C3 C8 O3 -171.3(3) . . . . ? C2 C3 C8 O3 9.9(5) . . . . ? C4 C3 C8 O4 9.7(5) . . . . ? C2 C3 C8 O4 -169.1(3) . . . . ? C6 C5 C9 C12 125.1(4) . . . . ? C4 C5 C9 C12 -54.9(5) . . . . ? C6 C5 C9 C10 3.4(5) . . . . ? C4 C5 C9 C10 -176.6(3) . . . . ? C6 C5 C9 C11 -115.7(4) . . . . ? C4 C5 C9 C11 64.3(4) . . . . ? C18 C13 C14 C15 2.3(6) . . . . ? C19 C13 C14 C15 179.5(4) . . . . ? C13 C14 C15 C16 -1.2(6) . . . . ? C13 C14 C15 C20 178.2(4) . . . . ? C14 C15 C16 C17 -1.5(6) . . . . ? C20 C15 C16 C17 179.0(4) . . . . ? C15 C16 C17 C18 3.0(6) . . . . ? C15 C16 C17 C21 -176.2(4) . . . . ? C16 C17 C18 C13 -1.8(6) . . . . ? C21 C17 C18 C13 177.4(4) . . . . ? C14 C13 C18 C17 -0.8(6) . . . . ? C19 C13 C18 C17 -178.1(4) . . . . ? Zn1 O5 C19 O6 -59.1(5) . . . . ? Zn1 O5 C19 C13 120.9(3) . . . . ? C14 C13 C19 O5 169.2(4) . . . . ? C18 C13 C19 O5 -13.6(6) . . . . ? C14 C13 C19 O6 -10.8(6) . . . . ? C18 C13 C19 O6 166.4(3) . . . . ? Zn1 O8 C20 O7 -50.0(5) 1_655 . . . ? Zn1 O8 C20 C15 131.4(3) 1_655 . . . ? C14 C15 C20 O8 -169.4(4) . . . . ? C16 C15 C20 O8 10.1(5) . . . . ? C14 C15 C20 O7 12.0(5) . . . . ? C16 C15 C20 O7 -168.5(3) . . . . ? C16 C17 C21 C24 -68.7(5) . . . . ? C18 C17 C21 C24 112.2(5) . . . . ? C16 C17 C21 C23 53.3(5) . . . . ? C18 C17 C21 C23 -125.9(5) . . . . ? C16 C17 C21 C22 171.8(5) . . . . ? C18 C17 C21 C22 -7.4(6) . . . . ? C36 N1 C25 C26 -1.4(5) . . . . ? Zn1 N1 C25 C26 166.5(3) . . . . ? N1 C25 C26 C27 0.4(6) . . . . ? C25 C26 C27 C28 1.7(6) . . . . ? C26 C27 C28 C36 -2.8(6) . . . . ? C26 C27 C28 C29 177.4(4) . . . . ? C27 C28 C29 C30 -179.7(4) . . . . ? C36 C28 C29 C30 0.5(6) . . . . ? C28 C29 C30 C31 -1.6(6) . . . . ? C29 C30 C31 C35 0.8(5) . . . . ? C29 C30 C31 C32 -178.7(4) . . . . ? C35 C31 C32 C33 -0.1(5) . . . . ? C30 C31 C32 C33 179.4(4) . . . . ? C31 C32 C33 C34 -3.1(6) . . . . ? C35 N2 C34 C33 -1.8(5) . . . . ? Zn1 N2 C34 C33 -176.1(3) . . . . ? C32 C33 C34 N2 4.2(6) . . . . ? C34 N2 C35 C31 -1.7(5) . . . . ? Zn1 N2 C35 C31 173.6(3) . . . . ? C34 N2 C35 C36 -179.8(3) . . . . ? Zn1 N2 C35 C36 -4.5(3) . . . . ? C32 C31 C35 N2 2.6(5) . . . . ? C30 C31 C35 N2 -177.0(3) . . . . ? C32 C31 C35 C36 -179.4(3) . . . . ? C30 C31 C35 C36 1.1(5) . . . . ? C25 N1 C36 C28 0.3(5) . . . . ? Zn1 N1 C36 C28 -169.7(3) . . . . ? C25 N1 C36 C35 -179.5(3) . . . . ? Zn1 N1 C36 C35 10.5(3) . . . . ? C27 C28 C36 N1 1.8(5) . . . . ? C29 C28 C36 N1 -178.4(3) . . . . ? C27 C28 C36 C35 -178.4(3) . . . . ? C29 C28 C36 C35 1.5(5) . . . . ? N2 C35 C36 N1 -4.2(4) . . . . ? C31 C35 C36 N1 177.6(3) . . . . ? N2 C35 C36 C28 175.9(3) . . . . ? C31 C35 C36 C28 -2.2(5) . . . . ? 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 O6 H6B O2 0.84 1.69 2.526(3) 172.7 . O7 H7A O3 0.84 1.71 2.551(3) 179.1 2_655 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.554 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.068 #============================================================================== data_ZnPhen-{[Zn(phen)(tbip)(H2O)].0.5H2O}n _database_code_depnum_ccdc_archive 'CCDC 835422' #TrackingRef '- revised cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C24 H22 N2 O5 Zn), H2 O' _chemical_formula_sum 'C48 H46 N4 O11 Zn2' _chemical_formula_weight 985.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.638(5) _cell_length_b 9.995(2) _cell_length_c 19.913(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.34(3) _cell_angle_gamma 90.00 _cell_volume 4478.2(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 19003 _cell_measurement_theta_min 6.18 _cell_measurement_theta_max 54.99 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2040 _exptl_absorpt_coefficient_mu 1.138 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7641 _exptl_absorpt_correction_T_max 0.8756 _exptl_absorpt_process_details 'Tompa_analytical (Rigaku Corporation, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Rigaku R-AXIS RAPID imaging plate' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32712 _diffrn_reflns_av_R_equivalents 0.1278 _diffrn_reflns_av_sigmaI/netI 0.0826 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5116 _reflns_number_gt 3161 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'PROCESS-AUTO (Rigaku Corporation,1998)' _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan (Molecular Structure Corporation & Rigaku Corporation, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. DFIX 0.90 0.01 is applied to the lattice water molecule O2w. ; _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^)+(0.1033P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0036(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5116 _refine_ls_number_parameters 301 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1138 _refine_ls_R_factor_gt 0.0719 _refine_ls_wR_factor_ref 0.2172 _refine_ls_wR_factor_gt 0.1746 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_restrained_S_all 1.150 _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 Zn1 Zn 0.40182(2) 0.64085(5) 0.55479(2) 0.0373(2) Uani 1 1 d . . . O1 O 0.34381(14) 0.5307(3) 0.48837(15) 0.0443(8) Uani 1 1 d . . . O1W O 0.46154(14) 0.4843(3) 0.57880(16) 0.0443(8) Uani 1 1 d . . . H1WA H 0.4716 0.4834 0.6207 0.053 Uiso 1 1 calc R . . H1WB H 0.4921 0.4923 0.5578 0.053 Uiso 1 1 d R . . O2 O 0.42472(14) 0.5883(4) 0.44195(15) 0.0426(8) Uani 1 1 d . . . O2W O 0.5000 0.7215(7) 0.2500 0.097(2) Uani 1 2 d SD . . H2WA H 0.521(3) 0.647(4) 0.263(4) 0.117 Uiso 1 1 d D . . O3 O 0.43553(15) 0.4826(4) 0.20074(17) 0.0594(11) Uani 1 1 d . . . O4 O 0.36055(14) 0.3764(3) 0.13902(15) 0.0419(8) Uani 1 1 d . . . N1 N 0.46430(17) 0.7920(4) 0.59249(19) 0.0406(9) Uani 1 1 d . . . N2 N 0.36241(18) 0.8247(4) 0.50969(18) 0.0406(10) Uani 1 1 d . . . C1 C 0.3458(2) 0.4761(5) 0.3723(2) 0.0380(11) Uani 1 1 d . . . C2 C 0.37760(19) 0.4732(4) 0.3162(2) 0.0356(10) Uani 1 1 d . . . H2A H 0.4173 0.5055 0.3198 0.043 Uiso 1 1 calc R . . C3 C 0.3514(2) 0.4235(5) 0.2551(2) 0.0382(11) Uani 1 1 d . . . C4 C 0.2924(2) 0.3799(5) 0.2496(2) 0.0401(11) Uani 1 1 d . . . H4A H 0.2747 0.3461 0.2075 0.048 Uiso 1 1 calc R . . C5 C 0.2588(2) 0.3846(5) 0.3044(2) 0.0375(11) Uani 1 1 d . . . C6 C 0.2873(2) 0.4322(5) 0.3656(2) 0.0390(11) Uani 1 1 d . . . H6A H 0.2658 0.4347 0.4039 0.047 Uiso 1 1 calc R . . C7 C 0.3739(2) 0.5346(5) 0.4381(2) 0.0372(11) Uani 1 1 d . . . C8 C 0.3854(2) 0.4279(5) 0.1935(2) 0.0399(11) Uani 1 1 d . . . C9 C 0.1937(2) 0.3451(5) 0.2988(2) 0.0445(12) Uani 1 1 d . . . C10 C 0.1698(2) 0.2954(6) 0.2274(2) 0.0529(14) Uani 1 1 d . . . H10A H 0.1938 0.2197 0.2148 0.079 Uiso 1 1 calc R . . H10B H 0.1720 0.3681 0.1947 0.079 Uiso 1 1 calc R . . H10C H 0.1283 0.2669 0.2273 0.079 Uiso 1 1 calc R . . C11 C 0.1568(2) 0.4705(6) 0.3132(3) 0.0577(15) Uani 1 1 d . . . H11A H 0.1615 0.5390 0.2790 0.087 Uiso 1 1 calc R . . H11B H 0.1707 0.5057 0.3580 0.087 Uiso 1 1 calc R . . H11C H 0.1147 0.4459 0.3115 0.087 Uiso 1 1 calc R . . C12 C 0.1843(2) 0.2348(6) 0.3499(3) 0.0556(14) Uani 1 1 d . . . H12A H 0.2048 0.1533 0.3381 0.083 Uiso 1 1 calc R . . H12B H 0.1417 0.2165 0.3492 0.083 Uiso 1 1 calc R . . H12C H 0.2003 0.2641 0.3953 0.083 Uiso 1 1 calc R . . C13 C 0.5125(2) 0.7756(6) 0.6364(3) 0.0535(14) Uani 1 1 d . . . H13A H 0.5217 0.6880 0.6529 0.064 Uiso 1 1 calc R . . C14 C 0.5501(3) 0.8797(6) 0.6594(3) 0.0668(18) Uani 1 1 d . . . H14A H 0.5842 0.8631 0.6905 0.080 Uiso 1 1 calc R . . C15 C 0.5371(2) 1.0066(6) 0.6364(3) 0.0671(17) Uani 1 1 d . . . H15A H 0.5624 1.0790 0.6515 0.080 Uiso 1 1 calc R . . C16 C 0.4862(2) 1.0296(5) 0.5903(3) 0.0490(13) Uani 1 1 d . . . C17 C 0.4686(3) 1.1588(5) 0.5645(3) 0.0604(16) Uani 1 1 d . . . H17A H 0.4929 1.2343 0.5769 0.072 Uiso 1 1 calc R . . C18 C 0.4178(3) 1.1750(6) 0.5226(3) 0.0616(16) Uani 1 1 d . . . H18A H 0.4072 1.2616 0.5057 0.074 Uiso 1 1 calc R . . C19 C 0.3800(2) 1.0650(5) 0.5035(3) 0.0502(13) Uani 1 1 d . . . C20 C 0.3245(3) 1.0761(7) 0.4617(3) 0.0630(16) Uani 1 1 d . . . H20A H 0.3112 1.1612 0.4451 0.076 Uiso 1 1 calc R . . C21 C 0.2904(3) 0.9645(6) 0.4455(3) 0.0570(15) Uani 1 1 d . . . H21A H 0.2535 0.9716 0.4179 0.068 Uiso 1 1 calc R . . C22 C 0.3113(2) 0.8398(5) 0.4705(2) 0.0478(13) Uani 1 1 d . . . H22A H 0.2878 0.7627 0.4589 0.057 Uiso 1 1 calc R . . C23 C 0.3963(2) 0.9354(5) 0.5259(2) 0.0415(11) Uani 1 1 d . . . C24 C 0.4510(2) 0.9170(5) 0.5706(2) 0.0415(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0479(4) 0.0330(4) 0.0307(4) -0.0008(2) 0.0025(2) -0.0033(2) O1 0.059(2) 0.045(2) 0.0289(17) -0.0076(14) 0.0074(15) -0.0056(16) O1W 0.054(2) 0.040(2) 0.0399(19) -0.0005(15) 0.0080(15) -0.0014(16) O2 0.045(2) 0.044(2) 0.0376(18) -0.0057(15) 0.0022(14) -0.0071(16) O2W 0.122(6) 0.051(5) 0.112(6) 0.000 -0.020(5) 0.000 O3 0.045(2) 0.094(3) 0.041(2) -0.0176(19) 0.0074(16) -0.019(2) O4 0.049(2) 0.046(2) 0.0304(17) -0.0034(14) -0.0003(14) -0.0024(15) N1 0.045(2) 0.033(2) 0.042(2) -0.0019(17) 0.0003(17) 0.0023(18) N2 0.050(2) 0.042(2) 0.030(2) -0.0004(17) 0.0045(17) -0.0024(19) C1 0.050(3) 0.032(3) 0.031(2) 0.0003(19) 0.003(2) 0.002(2) C2 0.037(2) 0.035(3) 0.034(2) 0.0009(19) 0.0019(18) 0.0017(19) C3 0.046(3) 0.038(3) 0.031(2) -0.003(2) 0.0051(19) 0.001(2) C4 0.050(3) 0.040(3) 0.030(2) -0.0026(19) 0.000(2) -0.001(2) C5 0.042(3) 0.035(3) 0.035(2) 0.0005(19) 0.002(2) -0.002(2) C6 0.046(3) 0.041(3) 0.031(2) -0.002(2) 0.0073(19) -0.007(2) C7 0.046(3) 0.033(3) 0.032(2) 0.0006(19) 0.003(2) 0.005(2) C8 0.043(3) 0.044(3) 0.033(2) -0.001(2) 0.003(2) 0.007(2) C9 0.045(3) 0.050(3) 0.039(3) 0.000(2) 0.004(2) -0.004(2) C10 0.050(3) 0.063(4) 0.044(3) -0.006(3) -0.002(2) -0.003(3) C11 0.050(3) 0.067(4) 0.057(3) -0.003(3) 0.006(3) 0.007(3) C12 0.057(3) 0.057(4) 0.052(3) 0.003(3) 0.003(3) -0.015(3) C13 0.053(3) 0.043(3) 0.061(3) 0.000(3) -0.011(3) -0.001(2) C14 0.061(4) 0.055(4) 0.079(4) -0.011(3) -0.019(3) -0.007(3) C15 0.058(4) 0.048(4) 0.093(5) -0.019(3) -0.002(3) -0.016(3) C16 0.050(3) 0.033(3) 0.065(4) -0.009(2) 0.009(3) -0.001(2) C17 0.066(4) 0.034(3) 0.083(4) -0.001(3) 0.018(3) -0.001(3) C18 0.075(4) 0.035(3) 0.078(4) 0.006(3) 0.023(3) 0.006(3) C19 0.060(3) 0.040(3) 0.053(3) 0.008(2) 0.016(3) 0.009(3) C20 0.077(4) 0.055(4) 0.058(4) 0.016(3) 0.011(3) 0.022(3) C21 0.058(4) 0.067(4) 0.045(3) 0.008(3) 0.002(2) 0.014(3) C22 0.049(3) 0.053(4) 0.040(3) 0.002(2) 0.001(2) 0.002(2) C23 0.050(3) 0.039(3) 0.037(3) 0.003(2) 0.011(2) 0.004(2) C24 0.047(3) 0.035(3) 0.043(3) -0.005(2) 0.008(2) -0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O4 2.015(3) 6_566 ? Zn1 O1 2.074(3) . ? Zn1 O1W 2.088(3) . ? Zn1 N1 2.148(4) . ? Zn1 N2 2.191(4) . ? Zn1 O2 2.419(3) . ? Zn1 C7 2.569(5) . ? O1 C7 1.271(5) . ? O1W H1WA 0.8400 . ? O1W H1WB 0.8499 . ? O2 C7 1.264(5) . ? O2W H2WA 0.91(5) . ? O3 C8 1.253(5) . ? O4 C8 1.275(5) . ? O4 Zn1 2.015(3) 6_565 ? N1 C13 1.332(6) . ? N1 C24 1.346(6) . ? N2 C22 1.332(6) . ? N2 C23 1.365(6) . ? C1 C6 1.388(6) . ? C1 C2 1.395(6) . ? C1 C7 1.510(6) . ? C2 C3 1.384(6) . ? C2 H2A 0.9500 . ? C3 C4 1.398(6) . ? C3 C8 1.520(6) . ? C4 C5 1.397(6) . ? C4 H4A 0.9500 . ? C5 C6 1.398(6) . ? C5 C9 1.517(7) . ? C6 H6A 0.9500 . ? C9 C12 1.532(7) . ? C9 C10 1.547(6) . ? C9 C11 1.551(7) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.389(7) . ? C13 H13A 0.9500 . ? C14 C15 1.369(8) . ? C14 H14A 0.9500 . ? C15 C16 1.411(8) . ? C15 H15A 0.9500 . ? C16 C24 1.410(7) . ? C16 C17 1.430(7) . ? C17 C18 1.356(8) . ? C17 H17A 0.9500 . ? C18 C19 1.419(8) . ? C18 H18A 0.9500 . ? C19 C23 1.406(7) . ? C19 C20 1.431(7) . ? C20 C21 1.375(8) . ? C20 H20A 0.9500 . ? C21 C22 1.405(7) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C24 1.455(7) . ? 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 O4 Zn1 O1 99.58(13) 6_566 . ? O4 Zn1 O1W 95.36(13) 6_566 . ? O1 Zn1 O1W 95.55(13) . . ? O4 Zn1 N1 96.72(14) 6_566 . ? O1 Zn1 N1 160.46(14) . . ? O1W Zn1 N1 93.57(14) . . ? O4 Zn1 N2 101.98(14) 6_566 . ? O1 Zn1 N2 89.04(14) . . ? O1W Zn1 N2 161.07(14) . . ? N1 Zn1 N2 77.05(15) . . ? O4 Zn1 O2 157.10(13) 6_566 . ? O1 Zn1 O2 58.53(12) . . ? O1W Zn1 O2 81.38(12) . . ? N1 Zn1 O2 106.08(13) . . ? N2 Zn1 O2 85.45(13) . . ? O4 Zn1 C7 128.82(15) 6_566 . ? O1 Zn1 C7 29.39(13) . . ? O1W Zn1 C7 89.18(14) . . ? N1 Zn1 C7 133.92(15) . . ? N2 Zn1 C7 85.86(14) . . ? O2 Zn1 C7 29.17(12) . . ? C7 O1 Zn1 97.4(3) . . ? Zn1 O1W H1WA 109.5 . . ? Zn1 O1W H1WB 111.0 . . ? H1WA O1W H1WB 110.1 . . ? C7 O2 Zn1 82.0(3) . . ? C8 O4 Zn1 122.8(3) . 6_565 ? C13 N1 C24 117.7(4) . . ? C13 N1 Zn1 127.1(4) . . ? C24 N1 Zn1 115.1(3) . . ? C22 N2 C23 118.4(4) . . ? C22 N2 Zn1 128.6(4) . . ? C23 N2 Zn1 113.0(3) . . ? C6 C1 C2 119.2(4) . . ? C6 C1 C7 120.8(4) . . ? C2 C1 C7 119.9(4) . . ? C3 C2 C1 120.1(4) . . ? C3 C2 H2A 119.9 . . ? C1 C2 H2A 119.9 . . ? C2 C3 C4 119.6(4) . . ? C2 C3 C8 119.4(4) . . ? C4 C3 C8 120.7(4) . . ? C5 C4 C3 121.7(4) . . ? C5 C4 H4A 119.2 . . ? C3 C4 H4A 119.2 . . ? C4 C5 C6 117.0(4) . . ? C4 C5 C9 122.8(4) . . ? C6 C5 C9 120.2(4) . . ? C1 C6 C5 122.4(4) . . ? C1 C6 H6A 118.8 . . ? C5 C6 H6A 118.8 . . ? O2 C7 O1 121.9(4) . . ? O2 C7 C1 120.6(4) . . ? O1 C7 C1 117.4(4) . . ? O2 C7 Zn1 68.8(2) . . ? O1 C7 Zn1 53.2(2) . . ? C1 C7 Zn1 169.4(3) . . ? O3 C8 O4 125.7(4) . . ? O3 C8 C3 117.0(4) . . ? O4 C8 C3 117.4(4) . . ? C5 C9 C12 110.1(4) . . ? C5 C9 C10 113.0(4) . . ? C12 C9 C10 108.6(4) . . ? C5 C9 C11 108.4(4) . . ? C12 C9 C11 109.9(5) . . ? C10 C9 C11 106.7(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C14 123.5(5) . . ? N1 C13 H13A 118.3 . . ? C14 C13 H13A 118.3 . . ? C15 C14 C13 118.9(5) . . ? C15 C14 H14A 120.6 . . ? C13 C14 H14A 120.6 . . ? C14 C15 C16 119.9(5) . . ? C14 C15 H15A 120.1 . . ? C16 C15 H15A 120.1 . . ? C24 C16 C15 116.5(5) . . ? C24 C16 C17 119.6(5) . . ? C15 C16 C17 123.8(5) . . ? C18 C17 C16 120.8(5) . . ? C18 C17 H17A 119.6 . . ? C16 C17 H17A 119.6 . . ? C17 C18 C19 121.3(5) . . ? C17 C18 H18A 119.4 . . ? C19 C18 H18A 119.4 . . ? C23 C19 C18 119.9(5) . . ? C23 C19 C20 116.0(5) . . ? C18 C19 C20 124.1(5) . . ? C21 C20 C19 120.5(5) . . ? C21 C20 H20A 119.7 . . ? C19 C20 H20A 119.7 . . ? C20 C21 C22 118.5(5) . . ? C20 C21 H21A 120.7 . . ? C22 C21 H21A 120.7 . . ? N2 C22 C21 123.1(5) . . ? N2 C22 H22A 118.5 . . ? C21 C22 H22A 118.5 . . ? N2 C23 C19 123.4(5) . . ? N2 C23 C24 117.4(4) . . ? C19 C23 C24 119.2(5) . . ? N1 C24 C16 123.5(5) . . ? N1 C24 C23 117.4(4) . . ? C16 C24 C23 119.1(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Zn1 O1 C7 -174.8(3) 6_566 . . . ? O1W Zn1 O1 C7 -78.4(3) . . . . ? N1 Zn1 O1 C7 39.1(5) . . . . ? N2 Zn1 O1 C7 83.2(3) . . . . ? O2 Zn1 O1 C7 -2.0(3) . . . . ? O4 Zn1 O2 C7 20.6(5) 6_566 . . . ? O1 Zn1 O2 C7 2.0(3) . . . . ? O1W Zn1 O2 C7 104.0(3) . . . . ? N1 Zn1 O2 C7 -164.8(3) . . . . ? N2 Zn1 O2 C7 -89.7(3) . . . . ? O4 Zn1 N1 C13 74.9(4) 6_566 . . . ? O1 Zn1 N1 C13 -138.6(5) . . . . ? O1W Zn1 N1 C13 -20.9(4) . . . . ? N2 Zn1 N1 C13 175.7(5) . . . . ? O2 Zn1 N1 C13 -103.0(4) . . . . ? C7 Zn1 N1 C13 -113.2(4) . . . . ? O4 Zn1 N1 C24 -102.3(3) 6_566 . . . ? O1 Zn1 N1 C24 44.1(6) . . . . ? O1W Zn1 N1 C24 161.9(3) . . . . ? N2 Zn1 N1 C24 -1.5(3) . . . . ? O2 Zn1 N1 C24 79.8(3) . . . . ? C7 Zn1 N1 C24 69.6(4) . . . . ? O4 Zn1 N2 C22 -83.6(4) 6_566 . . . ? O1 Zn1 N2 C22 15.9(4) . . . . ? O1W Zn1 N2 C22 120.4(5) . . . . ? N1 Zn1 N2 C22 -177.9(4) . . . . ? O2 Zn1 N2 C22 74.4(4) . . . . ? C7 Zn1 N2 C22 45.2(4) . . . . ? O4 Zn1 N2 C23 95.8(3) 6_566 . . . ? O1 Zn1 N2 C23 -164.6(3) . . . . ? O1W Zn1 N2 C23 -60.2(6) . . . . ? N1 Zn1 N2 C23 1.5(3) . . . . ? O2 Zn1 N2 C23 -106.1(3) . . . . ? C7 Zn1 N2 C23 -135.4(3) . . . . ? C6 C1 C2 C3 -1.9(7) . . . . ? C7 C1 C2 C3 -178.0(4) . . . . ? C1 C2 C3 C4 1.8(7) . . . . ? C1 C2 C3 C8 176.8(4) . . . . ? C2 C3 C4 C5 -0.2(7) . . . . ? C8 C3 C4 C5 -175.0(4) . . . . ? C3 C4 C5 C6 -1.4(7) . . . . ? C3 C4 C5 C9 176.5(5) . . . . ? C2 C1 C6 C5 0.2(7) . . . . ? C7 C1 C6 C5 176.3(4) . . . . ? C4 C5 C6 C1 1.4(7) . . . . ? C9 C5 C6 C1 -176.6(4) . . . . ? Zn1 O2 C7 O1 -3.3(4) . . . . ? Zn1 O2 C7 C1 174.7(4) . . . . ? Zn1 O1 C7 O2 3.8(5) . . . . ? Zn1 O1 C7 C1 -174.2(3) . . . . ? C6 C1 C7 O2 -171.9(4) . . . . ? C2 C1 C7 O2 4.2(7) . . . . ? C6 C1 C7 O1 6.2(7) . . . . ? C2 C1 C7 O1 -177.7(4) . . . . ? C6 C1 C7 Zn1 -20(2) . . . . ? C2 C1 C7 Zn1 156.3(16) . . . . ? O4 Zn1 C7 O2 -169.9(2) 6_566 . . . ? O1 Zn1 C7 O2 -176.5(4) . . . . ? O1W Zn1 C7 O2 -73.6(3) . . . . ? N1 Zn1 C7 O2 20.5(3) . . . . ? N2 Zn1 C7 O2 88.1(3) . . . . ? O4 Zn1 C7 O1 6.6(3) 6_566 . . . ? O1W Zn1 C7 O1 102.9(3) . . . . ? N1 Zn1 C7 O1 -163.0(3) . . . . ? N2 Zn1 C7 O1 -95.4(3) . . . . ? O2 Zn1 C7 O1 176.5(4) . . . . ? O4 Zn1 C7 C1 35.7(19) 6_566 . . . ? O1 Zn1 C7 C1 29.1(17) . . . . ? O1W Zn1 C7 C1 131.9(18) . . . . ? N1 Zn1 C7 C1 -133.9(18) . . . . ? N2 Zn1 C7 C1 -66.3(18) . . . . ? O2 Zn1 C7 C1 -154(2) . . . . ? Zn1 O4 C8 O3 5.7(7) 6_565 . . . ? Zn1 O4 C8 C3 -174.7(3) 6_565 . . . ? C2 C3 C8 O3 -3.0(7) . . . . ? C4 C3 C8 O3 171.9(5) . . . . ? C2 C3 C8 O4 177.3(4) . . . . ? C4 C3 C8 O4 -7.8(7) . . . . ? C4 C5 C9 C12 123.5(5) . . . . ? C6 C5 C9 C12 -58.6(6) . . . . ? C4 C5 C9 C10 1.9(7) . . . . ? C6 C5 C9 C10 179.8(4) . . . . ? C4 C5 C9 C11 -116.2(5) . . . . ? C6 C5 C9 C11 61.7(6) . . . . ? C24 N1 C13 C14 -1.4(8) . . . . ? Zn1 N1 C13 C14 -178.6(4) . . . . ? N1 C13 C14 C15 0.5(10) . . . . ? C13 C14 C15 C16 0.1(10) . . . . ? C14 C15 C16 C24 0.2(9) . . . . ? C14 C15 C16 C17 178.9(6) . . . . ? C24 C16 C17 C18 1.6(9) . . . . ? C15 C16 C17 C18 -177.0(6) . . . . ? C16 C17 C18 C19 0.7(9) . . . . ? C17 C18 C19 C23 -2.6(9) . . . . ? C17 C18 C19 C20 177.3(6) . . . . ? C23 C19 C20 C21 -0.1(8) . . . . ? C18 C19 C20 C21 -179.9(5) . . . . ? C19 C20 C21 C22 -0.3(8) . . . . ? C23 N2 C22 C21 -0.5(7) . . . . ? Zn1 N2 C22 C21 178.9(4) . . . . ? C20 C21 C22 N2 0.6(8) . . . . ? C22 N2 C23 C19 0.0(7) . . . . ? Zn1 N2 C23 C19 -179.4(4) . . . . ? C22 N2 C23 C24 178.1(4) . . . . ? Zn1 N2 C23 C24 -1.4(5) . . . . ? C18 C19 C23 N2 -179.9(5) . . . . ? C20 C19 C23 N2 0.2(8) . . . . ? C18 C19 C23 C24 2.1(7) . . . . ? C20 C19 C23 C24 -177.8(4) . . . . ? C13 N1 C24 C16 1.8(7) . . . . ? Zn1 N1 C24 C16 179.3(4) . . . . ? C13 N1 C24 C23 -176.2(4) . . . . ? Zn1 N1 C24 C23 1.3(5) . . . . ? C15 C16 C24 N1 -1.2(8) . . . . ? C17 C16 C24 N1 -179.9(5) . . . . ? C15 C16 C24 C23 176.8(5) . . . . ? C17 C16 C24 C23 -2.0(7) . . . . ? N2 C23 C24 N1 0.1(6) . . . . ? C19 C23 C24 N1 178.2(4) . . . . ? N2 C23 C24 C16 -178.0(4) . . . . ? C19 C23 C24 C16 0.1(7) . . . . ? 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 O1W H1WA O3 0.84 1.90 2.582(5) 137.5 6_566 O1W H1WB O2 0.85 2.05 2.750(5) 139.5 5_666 O2W H2WA O3 0.91(5) 2.01(5) 2.912(7) 175(9) 2_655 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.964 _refine_diff_density_min -1.488 _refine_diff_density_rms 0.138 #==============================================================================