# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global #TrackingRef '- cif.cif' _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Shan Gao' _publ_contact_author_address ; Key Laboratory of Functional Inorganic Material Chemistry, Ministry of Education, Heilongjiang University, Harbin 150080 CHINA ; _publ_contact_author_email shangao67@yahoo.com _publ_section_title ; Syntheses, crystal structures and properties of transition metal coordination polymers based on isophthalic acid and flexible bis(pyridyl) ligand with unsymmetrical spacer: influence of metal cations, ligand conformations and coordination modes ; loop_ _publ_author_name 'Zhao-Peng Deng' 'Zhu-Yan Zhang' 'Li-Hua Huo' 'Hui Zhao' 'Shan Gao' data_complex1 #TrackingRef '- cif.cif' _database_code_depnum_ccdc_archive 'CCDC 870296' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H36 Mn2 N6 O11, H2 O' _chemical_formula_sum 'C38 H38 Mn2 N6 O12' _chemical_formula_weight 880.62 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 '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.182(2) _cell_length_b 10.773(2) _cell_length_c 20.706(4) _cell_angle_alpha 89.93(3) _cell_angle_beta 77.78(3) _cell_angle_gamma 62.19(3) _cell_volume 1950.9(9) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 5021 _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 908 _exptl_absorpt_coefficient_mu 0.718 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8816 _exptl_absorpt_correction_T_max 0.9251 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 15257 _diffrn_reflns_av_R_equivalents 0.0666 _diffrn_reflns_av_sigmaI/netI 0.0787 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6755 _reflns_number_gt 4051 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0003P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6755 _refine_ls_number_parameters 529 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0703 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.1250 _refine_ls_wR_factor_gt 0.0880 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.68568(14) 0.10459(13) 0.30198(6) 0.0501(4) Uani 1 1 d . . . Mn2 Mn 0.46764(13) 0.37328(13) 0.78120(6) 0.0417(4) Uani 1 1 d . . . O1W O 0.6682(6) 0.2286(5) 0.2170(2) 0.0621(17) Uani 1 1 d . . . H1W1 H 0.7238 0.2649 0.2150 0.093 Uiso 1 1 d R . . H1W2 H 0.5831 0.2910 0.2153 0.093 Uiso 1 1 d R . . O1 O 0.4465(6) 0.2168(6) 0.3451(3) 0.0571(17) Uani 1 1 d . . . O2W O 0.7770(5) -0.0853(5) 0.2347(2) 0.0591(16) Uani 1 1 d . . . H2W1 H 0.7664 -0.1561 0.2380 0.089 Uiso 1 1 d R . . H2W2 H 0.7945 -0.0747 0.1952 0.089 Uiso 1 1 d R . . O2 O 0.4316(7) 0.0346(7) 0.3074(3) 0.079(2) Uani 1 1 d . . . O3 O -0.2896(6) 0.2707(5) 0.3626(2) 0.0544(17) Uani 1 1 d . . . O3W O 0.5732(5) 0.1505(5) 0.7813(2) 0.0582(16) Uani 1 1 d . . . H3W1 H 0.5732 0.0942 0.7547 0.087 Uiso 1 1 d R . . H3W2 H 0.6579 0.1162 0.7894 0.087 Uiso 1 1 d R . . O4 O -0.0907(6) 0.1116(6) 0.2871(3) 0.0527(17) Uani 1 1 d . . . O4W O 0.8471(5) 0.0458(5) 0.8107(2) 0.0679(17) Uani 1 1 d . . . H4W1 H 0.9222 -0.0045 0.7809 0.102 Uiso 1 1 d R . . H4W2 H 0.8242 0.1285 0.8061 0.102 Uiso 1 1 d R . . O5 O 0.5631(6) 0.5082(5) 0.7905(2) 0.0490(16) Uani 1 1 d . . . O6 O 0.7774(7) 0.3170(6) 0.7929(3) 0.082(2) Uani 1 1 d . . . O7 O 1.2541(6) 0.3524(6) 0.7736(2) 0.0505(16) Uani 1 1 d . . . O8 O 1.2370(5) 0.5612(5) 0.7912(2) 0.0503(16) Uani 1 1 d . . . N1 N 0.7645(8) -0.0272(7) 0.3855(3) 0.0442(19) Uani 1 1 d . . . N2 N 0.5615(9) 0.1210(8) 0.4664(3) 0.054(2) Uani 1 1 d D . . H2N H 0.523(8) 0.153(8) 0.433(2) 0.064 Uiso 1 1 d D . . N3 N 0.5258(7) 0.3691(7) 0.6722(3) 0.0460(19) Uani 1 1 d . . . N4 N 0.3915(7) 0.3973(7) 0.8937(3) 0.049(2) Uani 1 1 d . . . N5 N 0.0890(10) 0.7661(8) 1.0753(3) 0.057(2) Uani 1 1 d D . . H5N H 0.083(9) 0.775(8) 1.1174(9) 0.069 Uiso 1 1 d D . . N6 N -0.1676(11) 0.9176(8) 1.0990(4) 0.062(2) Uani 1 1 d . . . C1 C 0.3707(10) 0.1568(10) 0.3315(4) 0.052(3) Uani 1 1 d . . . C2 C 0.1998(9) 0.2407(9) 0.3507(4) 0.044(2) Uani 1 1 d . . . C3 C 0.1102(9) 0.1856(8) 0.3342(3) 0.043(2) Uani 1 1 d . . . H3 H 0.1549 0.0961 0.3111 0.052 Uiso 1 1 calc R . . C4 C -0.0501(9) 0.2693(9) 0.3534(4) 0.040(2) Uani 1 1 d . . . C5 C -0.1167(9) 0.4035(9) 0.3869(4) 0.055(3) Uani 1 1 d . . . H5 H -0.2226 0.4579 0.3984 0.066 Uiso 1 1 calc R . . C6 C -0.0276(10) 0.4569(10) 0.4033(4) 0.074(3) Uani 1 1 d . . . H6 H -0.0715 0.5468 0.4260 0.089 Uiso 1 1 calc R . . C7 C 0.1304(10) 0.3725(10) 0.3852(4) 0.062(3) Uani 1 1 d . . . H7 H 0.1915 0.4070 0.3969 0.075 Uiso 1 1 calc R . . C8 C -0.1522(10) 0.2151(10) 0.3332(5) 0.053(3) Uani 1 1 d . . . C9 C 0.7065(11) 0.0150(10) 0.4510(5) 0.048(2) Uani 1 1 d . . . C10 C 0.7847(12) -0.0466(11) 0.4978(5) 0.069(3) Uani 1 1 d . . . H10 H 0.7390 -0.0167 0.5428 0.083 Uiso 1 1 calc R . . C11 C 0.9307(14) -0.1524(13) 0.4777(6) 0.093(4) Uani 1 1 d . . . H11 H 0.9875 -0.1929 0.5089 0.112 Uiso 1 1 calc R . . C12 C 0.9963(12) -0.2010(11) 0.4099(6) 0.089(3) Uani 1 1 d . . . H12 H 1.0953 -0.2751 0.3954 0.106 Uiso 1 1 calc R . . C13 C 0.9090(12) -0.1353(11) 0.3657(4) 0.066(3) Uani 1 1 d . . . H13 H 0.9505 -0.1661 0.3205 0.080 Uiso 1 1 calc R . . C14 C 0.4743(9) 0.1810(9) 0.5345(4) 0.062(3) Uani 1 1 d . . . H14A H 0.4822 0.1049 0.5612 0.074 Uiso 1 1 calc R . . H14B H 0.3674 0.2391 0.5345 0.074 Uiso 1 1 calc R . . C15 C 0.4968(8) 0.2873(8) 0.6354(4) 0.050(2) Uani 1 1 d . . . H15 H 0.4510 0.2376 0.6581 0.060 Uiso 1 1 calc R . . C16 C 0.5288(8) 0.2695(8) 0.5659(4) 0.045(2) Uani 1 1 d . . . C17 C 0.5949(9) 0.3442(9) 0.5322(4) 0.052(2) Uani 1 1 d . . . H17 H 0.6200 0.3357 0.4860 0.062 Uiso 1 1 calc R . . C18 C 0.6224(9) 0.4305(9) 0.5683(4) 0.060(3) Uani 1 1 d . . . H18 H 0.6667 0.4820 0.5463 0.072 Uiso 1 1 calc R . . C19 C 0.5864(8) 0.4436(8) 0.6365(4) 0.049(2) Uani 1 1 d . . . H19 H 0.6043 0.5063 0.6593 0.059 Uiso 1 1 calc R . . C20 C 0.6985(11) 0.4485(11) 0.7944(4) 0.046(3) Uani 1 1 d . . . C21 C 0.7759(9) 0.5362(8) 0.8020(3) 0.035(2) Uani 1 1 d . . . C22 C 0.9340(9) 0.4743(8) 0.7898(3) 0.043(2) Uani 1 1 d . . . H22 H 0.9938 0.3784 0.7752 0.052 Uiso 1 1 calc R . . C23 C 1.0034(9) 0.5564(9) 0.7995(4) 0.041(2) Uani 1 1 d . . . C24 C 0.9173(9) 0.6976(9) 0.8191(4) 0.048(2) Uani 1 1 d . . . H24 H 0.9640 0.7523 0.8238 0.058 Uiso 1 1 calc R . . C25 C 0.7617(9) 0.7581(8) 0.8317(4) 0.054(3) Uani 1 1 d . . . H25 H 0.7029 0.8536 0.8472 0.065 Uiso 1 1 calc R . . C26 C 0.6904(9) 0.6815(8) 0.8222(4) 0.047(2) Uani 1 1 d . . . H26 H 0.5845 0.7261 0.8291 0.057 Uiso 1 1 calc R . . C27 C 1.1750(10) 0.4845(10) 0.7862(4) 0.046(2) Uani 1 1 d . . . C28 C 0.3569(9) 0.5132(9) 0.9306(4) 0.054(2) Uani 1 1 d . . . H28 H 0.3934 0.5724 0.9110 0.064 Uiso 1 1 calc R . . C29 C 0.2713(9) 0.5547(9) 0.9956(4) 0.048(2) Uani 1 1 d . . . C30 C 0.2183(10) 0.4655(10) 1.0222(4) 0.074(3) Uani 1 1 d . . . H30 H 0.1590 0.4876 1.0656 0.089 Uiso 1 1 calc R . . C31 C 0.2511(11) 0.3449(11) 0.9860(4) 0.083(4) Uani 1 1 d . . . H31 H 0.2154 0.2843 1.0044 0.099 Uiso 1 1 calc R . . C32 C 0.3385(10) 0.3140(9) 0.9214(4) 0.065(3) Uani 1 1 d . . . H32 H 0.3607 0.2318 0.8966 0.078 Uiso 1 1 calc R . . C33 C 0.2435(9) 0.6849(8) 1.0334(4) 0.059(3) Uani 1 1 d . . . H33A H 0.3159 0.6592 1.0612 0.071 Uiso 1 1 calc R . . H33B H 0.2632 0.7449 1.0021 0.071 Uiso 1 1 calc R . . C34 C -0.0371(13) 0.8491(10) 1.0535(5) 0.055(3) Uani 1 1 d . . . C35 C -0.0339(11) 0.8628(9) 0.9858(5) 0.056(3) Uani 1 1 d . . . H35 H 0.0564 0.8141 0.9532 0.067 Uiso 1 1 calc R . . C36 C -0.1645(15) 0.9479(12) 0.9702(5) 0.075(3) Uani 1 1 d . . . H36 H -0.1632 0.9612 0.9257 0.090 Uiso 1 1 calc R . . C37 C -0.3020(14) 1.0175(12) 1.0164(7) 0.096(4) Uani 1 1 d . . . H37 H -0.3936 1.0739 1.0047 0.115 Uiso 1 1 calc R . . C38 C -0.2932(13) 0.9974(11) 1.0807(6) 0.074(3) Uani 1 1 d . . . H38 H -0.3831 1.0437 1.1138 0.089 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 0.0412(9) 0.0538(10) 0.0536(9) 0.0004(8) -0.0115(7) -0.0212(8) Mn2 0.0352(8) 0.0418(9) 0.0458(8) -0.0032(7) -0.0076(6) -0.0174(8) O1W 0.061(4) 0.055(4) 0.069(4) 0.011(3) -0.020(3) -0.025(4) O1 0.044(4) 0.076(5) 0.070(4) 0.004(3) -0.023(3) -0.040(4) O2W 0.066(4) 0.055(4) 0.054(4) -0.007(3) -0.007(3) -0.029(4) O2 0.042(4) 0.064(5) 0.116(6) -0.026(4) -0.019(4) -0.013(4) O3 0.035(4) 0.059(4) 0.069(4) -0.004(3) -0.006(3) -0.024(4) O3W 0.052(4) 0.044(4) 0.076(4) -0.005(3) -0.023(3) -0.018(3) O4 0.030(4) 0.061(5) 0.063(4) 0.002(3) -0.006(3) -0.021(3) O4W 0.059(4) 0.044(4) 0.075(4) -0.001(3) -0.013(3) -0.005(3) O5 0.032(4) 0.054(4) 0.066(4) 0.007(3) -0.017(3) -0.024(4) O6 0.058(5) 0.054(5) 0.130(6) -0.016(4) -0.013(4) -0.028(4) O7 0.039(4) 0.052(4) 0.055(4) -0.002(3) -0.004(3) -0.020(4) O8 0.037(4) 0.056(4) 0.068(4) 0.002(3) -0.013(3) -0.031(4) N1 0.039(5) 0.038(5) 0.049(5) -0.005(4) -0.009(4) -0.013(4) N2 0.059(6) 0.052(6) 0.047(5) -0.006(4) -0.012(4) -0.025(5) N3 0.047(5) 0.050(5) 0.047(5) -0.007(4) -0.008(4) -0.028(4) N4 0.048(5) 0.043(5) 0.059(5) -0.007(4) -0.005(4) -0.025(4) N5 0.062(6) 0.055(6) 0.039(5) -0.004(5) -0.002(5) -0.020(5) N6 0.053(6) 0.039(6) 0.072(6) -0.022(5) 0.008(5) -0.013(5) C1 0.048(7) 0.059(8) 0.042(6) 0.010(5) -0.021(5) -0.017(6) C2 0.024(5) 0.039(6) 0.064(6) 0.009(5) -0.020(5) -0.007(5) C3 0.036(6) 0.048(6) 0.044(5) -0.006(4) -0.011(4) -0.019(5) C4 0.038(6) 0.045(6) 0.034(5) 0.002(4) -0.010(4) -0.015(5) C5 0.046(6) 0.045(7) 0.063(6) -0.008(5) -0.001(5) -0.017(6) C6 0.061(7) 0.057(7) 0.114(9) -0.015(6) -0.019(6) -0.036(7) C7 0.044(7) 0.063(8) 0.081(7) 0.006(6) -0.010(5) -0.030(6) C8 0.039(6) 0.054(7) 0.066(7) 0.019(5) -0.024(5) -0.018(6) C9 0.056(7) 0.044(7) 0.049(6) -0.002(6) -0.015(6) -0.026(6) C10 0.067(8) 0.078(9) 0.062(7) 0.004(7) -0.033(7) -0.027(7) C11 0.100(11) 0.094(11) 0.113(10) 0.056(9) -0.077(9) -0.048(10) C12 0.076(9) 0.073(9) 0.102(10) 0.000(8) -0.040(8) -0.016(7) C13 0.075(8) 0.075(9) 0.045(7) 0.008(6) -0.014(6) -0.032(7) C14 0.078(7) 0.081(8) 0.039(6) -0.019(5) -0.002(5) -0.052(7) C15 0.049(6) 0.053(7) 0.045(6) -0.006(5) -0.007(5) -0.024(5) C16 0.034(5) 0.038(6) 0.053(6) -0.015(5) -0.015(4) -0.006(5) C17 0.051(6) 0.066(7) 0.048(6) 0.009(5) -0.010(5) -0.036(6) C18 0.073(7) 0.076(8) 0.044(6) -0.001(5) -0.010(5) -0.048(6) C19 0.054(6) 0.054(6) 0.051(6) 0.007(5) -0.024(5) -0.030(6) C20 0.054(7) 0.060(7) 0.035(5) -0.015(5) -0.001(5) -0.040(7) C21 0.043(6) 0.034(6) 0.029(5) -0.001(4) -0.015(4) -0.016(5) C22 0.033(5) 0.045(6) 0.056(6) 0.003(5) -0.017(4) -0.020(5) C23 0.038(6) 0.045(6) 0.041(5) 0.003(5) -0.011(4) -0.020(5) C24 0.040(6) 0.046(6) 0.069(6) 0.007(5) -0.014(5) -0.028(6) C25 0.042(6) 0.036(6) 0.100(7) -0.007(5) -0.027(5) -0.027(5) C26 0.032(5) 0.049(6) 0.071(6) 0.002(5) -0.010(5) -0.027(5) C27 0.054(7) 0.051(7) 0.031(5) 0.011(5) -0.017(5) -0.021(6) C28 0.065(7) 0.051(7) 0.057(6) 0.012(5) -0.023(5) -0.034(6) C29 0.053(6) 0.052(7) 0.043(6) -0.001(5) -0.006(5) -0.030(6) C30 0.087(8) 0.071(8) 0.060(7) -0.002(6) 0.004(6) -0.043(7) C31 0.135(10) 0.097(9) 0.047(7) -0.008(6) 0.010(6) -0.094(9) C32 0.086(8) 0.047(7) 0.060(7) -0.010(6) -0.016(6) -0.031(6) C33 0.056(7) 0.054(7) 0.062(6) -0.018(5) -0.013(5) -0.022(6) C34 0.070(8) 0.044(7) 0.073(8) 0.025(6) -0.031(7) -0.040(7) C35 0.070(8) 0.047(7) 0.055(7) 0.008(5) -0.019(6) -0.030(7) C36 0.108(10) 0.069(9) 0.084(9) 0.036(7) -0.067(8) -0.055(9) C37 0.101(11) 0.077(10) 0.142(13) 0.016(10) -0.062(10) -0.055(10) C38 0.057(8) 0.045(8) 0.109(10) -0.012(7) -0.011(8) -0.018(7) _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 2.127(5) . ? Mn1 O2W 2.162(5) . ? Mn1 O1W 2.196(4) . ? Mn1 O4 2.269(5) 1_655 ? Mn1 N1 2.273(7) . ? Mn1 O3 2.324(5) 1_655 ? Mn1 C8 2.616(9) 1_655 ? Mn2 O5 2.119(5) . ? Mn2 O3W 2.123(5) . ? Mn2 N3 2.204(6) . ? Mn2 O8 2.240(5) 1_455 ? Mn2 N4 2.269(6) . ? Mn2 O7 2.325(5) 1_455 ? Mn2 C27 2.620(9) 1_455 ? O1W H1W1 0.8200 . ? O1W H1W2 0.8200 . ? O1 C1 1.285(8) . ? O2W H2W1 0.8199 . ? O2W H2W2 0.8201 . ? O2 C1 1.215(9) . ? O3 C8 1.244(8) . ? O3 Mn1 2.324(5) 1_455 ? O3W H3W1 0.8199 . ? O3W H3W2 0.8201 . ? O4 C8 1.282(9) . ? O4 Mn1 2.269(5) 1_455 ? O4W H4W1 0.8199 . ? O4W H4W2 0.8200 . ? O5 C20 1.241(9) . ? O6 C20 1.258(9) . ? O7 C27 1.259(8) . ? O7 Mn2 2.325(5) 1_655 ? O8 C27 1.267(8) . ? O8 Mn2 2.240(5) 1_655 ? N1 C9 1.343(9) . ? N1 C13 1.355(10) . ? N2 C9 1.347(10) . ? N2 C14 1.460(9) . ? N2 H2N 0.86(9) . ? N3 C15 1.336(8) . ? N3 C19 1.356(7) . ? N4 C28 1.321(8) . ? N4 C32 1.321(7) . ? N5 C34 1.351(10) . ? N5 C33 1.461(9) . ? N5 H5N 0.86(9) . ? N6 C38 1.303(11) . ? N6 C34 1.325(10) . ? C1 C2 1.498(10) . ? C2 C7 1.370(10) . ? C2 C3 1.392(9) . ? C3 C4 1.410(9) . ? C3 H3 0.9300 . ? C4 C5 1.386(9) . ? C4 C8 1.532(10) . ? C5 C6 1.375(9) . ? C5 H5 0.9300 . ? C6 C7 1.391(10) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 Mn1 2.616(9) 1_455 ? C9 C10 1.359(11) . ? C10 C11 1.357(12) . ? C10 H10 0.9300 . ? C11 C12 1.404(12) . ? C11 H11 0.9300 . ? C12 C13 1.372(11) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C16 1.512(9) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.399(9) . ? C15 H15 0.9300 . ? C16 C17 1.376(8) . ? C17 C18 1.354(9) . ? C17 H17 0.9300 . ? C18 C19 1.372(9) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.512(9) . ? C21 C22 1.387(9) . ? C21 C26 1.400(9) . ? C22 C23 1.403(9) . ? C22 H22 0.9300 . ? C23 C24 1.361(9) . ? C23 C27 1.504(10) . ? C24 C25 1.366(9) . ? C24 H24 0.9300 . ? C25 C26 1.367(8) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 Mn2 2.620(9) 1_655 ? C28 C29 1.384(9) . ? C28 H28 0.9300 . ? C29 C30 1.370(9) . ? C29 C33 1.483(9) . ? C30 C31 1.361(9) . ? C30 H30 0.9300 . ? C31 C32 1.383(9) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.403(10) . ? C35 C36 1.326(11) . ? C35 H35 0.9300 . ? C36 C37 1.376(13) . ? C36 H36 0.9300 . ? C37 C38 1.364(12) . ? C37 H37 0.9300 . ? C38 H38 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 O1 Mn1 O2W 119.20(19) . . ? O1 Mn1 O1W 93.3(2) . . ? O2W Mn1 O1W 89.87(18) . . ? O1 Mn1 O4 144.8(2) . 1_655 ? O2W Mn1 O4 95.60(19) . 1_655 ? O1W Mn1 O4 80.62(19) . 1_655 ? O1 Mn1 N1 99.5(2) . . ? O2W Mn1 N1 90.4(2) . . ? O1W Mn1 N1 165.1(2) . . ? O4 Mn1 N1 84.6(2) 1_655 . ? O1 Mn1 O3 87.9(2) . 1_655 ? O2W Mn1 O3 152.90(18) . 1_655 ? O1W Mn1 O3 89.98(18) . 1_655 ? O4 Mn1 O3 57.69(18) 1_655 1_655 ? N1 Mn1 O3 83.0(2) . 1_655 ? O1 Mn1 C8 116.1(3) . 1_655 ? O2W Mn1 C8 124.7(3) . 1_655 ? O1W Mn1 C8 85.5(2) . 1_655 ? O4 Mn1 C8 29.3(2) 1_655 1_655 ? N1 Mn1 C8 82.1(2) . 1_655 ? O3 Mn1 C8 28.4(2) 1_655 1_655 ? O5 Mn2 O3W 127.8(2) . . ? O5 Mn2 N3 89.9(2) . . ? O3W Mn2 N3 95.5(2) . . ? O5 Mn2 O8 90.3(2) . 1_455 ? O3W Mn2 O8 140.95(17) . 1_455 ? N3 Mn2 O8 92.3(2) . 1_455 ? O5 Mn2 N4 88.6(2) . . ? O3W Mn2 N4 89.2(2) . . ? N3 Mn2 N4 175.0(2) . . ? O8 Mn2 N4 82.9(2) 1_455 . ? O5 Mn2 O7 147.8(2) . 1_455 ? O3W Mn2 O7 84.34(19) . 1_455 ? N3 Mn2 O7 89.1(2) . 1_455 ? O8 Mn2 O7 57.55(17) 1_455 1_455 ? N4 Mn2 O7 89.7(2) . 1_455 ? O5 Mn2 C27 119.2(3) . 1_455 ? O3W Mn2 C27 112.4(2) . 1_455 ? N3 Mn2 C27 92.2(2) . 1_455 ? O8 Mn2 C27 28.91(19) 1_455 1_455 ? N4 Mn2 C27 84.4(2) . 1_455 ? O7 Mn2 C27 28.71(18) 1_455 1_455 ? Mn1 O1W H1W1 109.6 . . ? Mn1 O1W H1W2 117.8 . . ? H1W1 O1W H1W2 107.6 . . ? C1 O1 Mn1 114.8(5) . . ? Mn1 O2W H2W1 131.9 . . ? Mn1 O2W H2W2 114.7 . . ? H2W1 O2W H2W2 108.1 . . ? C8 O3 Mn1 89.0(5) . 1_455 ? Mn2 O3W H3W1 126.2 . . ? Mn2 O3W H3W2 113.8 . . ? H3W1 O3W H3W2 108.5 . . ? C8 O4 Mn1 90.5(5) . 1_455 ? H4W1 O4W H4W2 108.4 . . ? C20 O5 Mn2 115.6(6) . . ? C27 O7 Mn2 88.8(5) . 1_655 ? C27 O8 Mn2 92.4(5) . 1_655 ? C9 N1 C13 117.8(8) . . ? C9 N1 Mn1 126.1(6) . . ? C13 N1 Mn1 112.5(6) . . ? C9 N2 C14 123.4(8) . . ? C9 N2 H2N 115(6) . . ? C14 N2 H2N 121(6) . . ? C15 N3 C19 114.2(6) . . ? C15 N3 Mn2 118.3(5) . . ? C19 N3 Mn2 127.4(5) . . ? C28 N4 C32 116.9(7) . . ? C28 N4 Mn2 121.9(6) . . ? C32 N4 Mn2 118.3(5) . . ? C34 N5 C33 125.4(8) . . ? C34 N5 H5N 118(6) . . ? C33 N5 H5N 115(6) . . ? C38 N6 C34 119.7(9) . . ? O2 C1 O1 122.8(9) . . ? O2 C1 C2 119.7(9) . . ? O1 C1 C2 117.4(8) . . ? C7 C2 C3 119.5(8) . . ? C7 C2 C1 119.9(8) . . ? C3 C2 C1 120.6(8) . . ? C2 C3 C4 118.2(8) . . ? C2 C3 H3 120.9 . . ? C4 C3 H3 120.9 . . ? C5 C4 C3 120.9(8) . . ? C5 C4 C8 119.3(8) . . ? C3 C4 C8 119.6(7) . . ? C6 C5 C4 120.6(8) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C7 118.0(9) . . ? C5 C6 H6 121.0 . . ? C7 C6 H6 121.0 . . ? C2 C7 C6 122.8(9) . . ? C2 C7 H7 118.6 . . ? C6 C7 H7 118.6 . . ? O3 C8 O4 122.7(8) . . ? O3 C8 C4 119.2(8) . . ? O4 C8 C4 118.1(8) . . ? O3 C8 Mn1 62.6(5) . 1_455 ? O4 C8 Mn1 60.1(4) . 1_455 ? C4 C8 Mn1 175.7(6) . 1_455 ? N1 C9 N2 113.9(9) . . ? N1 C9 C10 123.2(10) . . ? N2 C9 C10 122.8(9) . . ? C11 C10 C9 118.8(10) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? C10 C11 C12 120.2(11) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C13 C12 C11 117.6(11) . . ? C13 C12 H12 121.2 . . ? C11 C12 H12 121.2 . . ? N1 C13 C12 122.3(9) . . ? N1 C13 H13 118.8 . . ? C12 C13 H13 118.8 . . ? N2 C14 C16 112.9(6) . . ? N2 C14 H14A 109.0 . . ? C16 C14 H14A 109.0 . . ? N2 C14 H14B 109.0 . . ? C16 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? N3 C15 C16 126.1(7) . . ? N3 C15 H15 116.9 . . ? C16 C15 H15 116.9 . . ? C17 C16 C15 117.0(7) . . ? C17 C16 C14 125.4(8) . . ? C15 C16 C14 117.3(8) . . ? C18 C17 C16 118.1(8) . . ? C18 C17 H17 120.9 . . ? C16 C17 H17 120.9 . . ? C17 C18 C19 121.5(8) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? N3 C19 C18 122.9(7) . . ? N3 C19 H19 118.6 . . ? C18 C19 H19 118.6 . . ? O5 C20 O6 123.7(8) . . ? O5 C20 C21 119.5(9) . . ? O6 C20 C21 116.8(8) . . ? C22 C21 C26 118.2(7) . . ? C22 C21 C20 120.8(8) . . ? C26 C21 C20 121.0(8) . . ? C21 C22 C23 119.9(8) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 120.6(8) . . ? C24 C23 C27 121.3(7) . . ? C22 C23 C27 118.1(8) . . ? C23 C24 C25 119.4(7) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? C24 C25 C26 121.5(8) . . ? C24 C25 H25 119.2 . . ? C26 C25 H25 119.2 . . ? C25 C26 C21 120.3(8) . . ? C25 C26 H26 119.9 . . ? C21 C26 H26 119.9 . . ? O7 C27 O8 121.0(8) . . ? O7 C27 C23 121.4(8) . . ? O8 C27 C23 117.5(8) . . ? O7 C27 Mn2 62.5(5) . 1_655 ? O8 C27 Mn2 58.7(4) . 1_655 ? C23 C27 Mn2 171.6(6) . 1_655 ? N4 C28 C29 125.9(7) . . ? N4 C28 H28 117.0 . . ? C29 C28 H28 117.0 . . ? C30 C29 C28 115.1(8) . . ? C30 C29 C33 123.3(8) . . ? C28 C29 C33 121.6(7) . . ? C31 C30 C29 120.9(8) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C30 C31 C32 118.8(8) . . ? C30 C31 H31 120.6 . . ? C32 C31 H31 120.6 . . ? N4 C32 C31 122.3(8) . . ? N4 C32 H32 118.9 . . ? C31 C32 H32 118.9 . . ? N5 C33 C29 114.4(7) . . ? N5 C33 H33A 108.7 . . ? C29 C33 H33A 108.7 . . ? N5 C33 H33B 108.7 . . ? C29 C33 H33B 108.7 . . ? H33A C33 H33B 107.6 . . ? N6 C34 N5 117.1(10) . . ? N6 C34 C35 120.2(10) . . ? N5 C34 C35 122.7(10) . . ? C36 C35 C34 117.5(10) . . ? C36 C35 H35 121.2 . . ? C34 C35 H35 121.2 . . ? C35 C36 C37 123.3(11) . . ? C35 C36 H36 118.4 . . ? C37 C36 H36 118.4 . . ? C38 C37 C36 114.7(12) . . ? C38 C37 H37 122.6 . . ? C36 C37 H37 122.6 . . ? N6 C38 C37 124.5(11) . . ? N6 C38 H38 117.7 . . ? C37 C38 H38 117.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2W Mn1 O1 C1 4.9(6) . . . . ? O1W Mn1 O1 C1 96.6(6) . . . . ? O4 Mn1 O1 C1 174.9(5) 1_655 . . . ? N1 Mn1 O1 C1 -91.0(6) . . . . ? O3 Mn1 O1 C1 -173.6(6) 1_655 . . . ? C8 Mn1 O1 C1 -176.8(5) 1_655 . . . ? O3W Mn2 O5 C20 2.4(6) . . . . ? N3 Mn2 O5 C20 -94.5(6) . . . . ? O8 Mn2 O5 C20 173.2(6) 1_455 . . . ? N4 Mn2 O5 C20 90.3(6) . . . . ? O7 Mn2 O5 C20 177.4(5) 1_455 . . . ? C27 Mn2 O5 C20 173.0(5) 1_455 . . . ? O1 Mn1 N1 C9 -37.0(6) . . . . ? O2W Mn1 N1 C9 -156.7(6) . . . . ? O1W Mn1 N1 C9 112.1(10) . . . . ? O4 Mn1 N1 C9 107.7(6) 1_655 . . . ? O3 Mn1 N1 C9 49.6(6) 1_655 . . . ? C8 Mn1 N1 C9 78.2(6) 1_655 . . . ? O1 Mn1 N1 C13 164.8(6) . . . . ? O2W Mn1 N1 C13 45.1(6) . . . . ? O1W Mn1 N1 C13 -46.0(12) . . . . ? O4 Mn1 N1 C13 -50.5(6) 1_655 . . . ? O3 Mn1 N1 C13 -108.5(6) 1_655 . . . ? C8 Mn1 N1 C13 -79.9(6) 1_655 . . . ? O5 Mn2 N3 C15 176.6(6) . . . . ? O3W Mn2 N3 C15 48.6(6) . . . . ? O8 Mn2 N3 C15 -93.1(6) 1_455 . . . ? O7 Mn2 N3 C15 -35.6(6) 1_455 . . . ? C27 Mn2 N3 C15 -64.1(6) 1_455 . . . ? O5 Mn2 N3 C19 -4.9(6) . . . . ? O3W Mn2 N3 C19 -132.9(6) . . . . ? O8 Mn2 N3 C19 85.4(6) 1_455 . . . ? O7 Mn2 N3 C19 142.9(6) 1_455 . . . ? C27 Mn2 N3 C19 114.3(6) 1_455 . . . ? O5 Mn2 N4 C28 30.0(7) . . . . ? O3W Mn2 N4 C28 157.9(6) . . . . ? O8 Mn2 N4 C28 -60.5(6) 1_455 . . . ? O7 Mn2 N4 C28 -117.8(7) 1_455 . . . ? C27 Mn2 N4 C28 -89.5(7) 1_455 . . . ? O5 Mn2 N4 C32 -169.8(6) . . . . ? O3W Mn2 N4 C32 -41.9(6) . . . . ? O8 Mn2 N4 C32 99.7(6) 1_455 . . . ? O7 Mn2 N4 C32 42.4(6) 1_455 . . . ? C27 Mn2 N4 C32 70.7(6) 1_455 . . . ? Mn1 O1 C1 O2 13.7(11) . . . . ? Mn1 O1 C1 C2 -170.1(5) . . . . ? O2 C1 C2 C7 172.1(8) . . . . ? O1 C1 C2 C7 -4.1(12) . . . . ? O2 C1 C2 C3 -7.5(13) . . . . ? O1 C1 C2 C3 176.3(7) . . . . ? C7 C2 C3 C4 0.4(12) . . . . ? C1 C2 C3 C4 -179.9(7) . . . . ? C2 C3 C4 C5 1.0(12) . . . . ? C2 C3 C4 C8 177.1(7) . . . . ? C3 C4 C5 C6 -1.3(13) . . . . ? C8 C4 C5 C6 -177.4(7) . . . . ? C4 C5 C6 C7 0.2(13) . . . . ? C3 C2 C7 C6 -1.6(14) . . . . ? C1 C2 C7 C6 178.7(8) . . . . ? C5 C6 C7 C2 1.3(14) . . . . ? Mn1 O3 C8 O4 3.0(9) 1_455 . . . ? Mn1 O3 C8 C4 -175.5(7) 1_455 . . . ? Mn1 O4 C8 O3 -3.1(9) 1_455 . . . ? Mn1 O4 C8 C4 175.5(6) 1_455 . . . ? C5 C4 C8 O3 -20.9(12) . . . . ? C3 C4 C8 O3 162.9(7) . . . . ? C5 C4 C8 O4 160.5(8) . . . . ? C3 C4 C8 O4 -15.7(12) . . . . ? C13 N1 C9 N2 -178.8(7) . . . . ? Mn1 N1 C9 N2 24.0(10) . . . . ? C13 N1 C9 C10 -0.9(12) . . . . ? Mn1 N1 C9 C10 -158.0(7) . . . . ? C14 N2 C9 N1 178.3(6) . . . . ? C14 N2 C9 C10 0.4(13) . . . . ? N1 C9 C10 C11 2.5(14) . . . . ? N2 C9 C10 C11 -179.7(9) . . . . ? C9 C10 C11 C12 -2.8(16) . . . . ? C10 C11 C12 C13 1.6(16) . . . . ? C9 N1 C13 C12 -0.4(13) . . . . ? Mn1 N1 C13 C12 159.7(7) . . . . ? C11 C12 C13 N1 0.0(15) . . . . ? C9 N2 C14 C16 72.0(10) . . . . ? C19 N3 C15 C16 2.7(12) . . . . ? Mn2 N3 C15 C16 -178.6(6) . . . . ? N3 C15 C16 C17 -0.7(13) . . . . ? N3 C15 C16 C14 -175.1(8) . . . . ? N2 C14 C16 C17 29.7(12) . . . . ? N2 C14 C16 C15 -156.6(7) . . . . ? C15 C16 C17 C18 -0.8(12) . . . . ? C14 C16 C17 C18 173.0(8) . . . . ? C16 C17 C18 C19 0.2(13) . . . . ? C15 N3 C19 C18 -3.3(11) . . . . ? Mn2 N3 C19 C18 178.2(6) . . . . ? C17 C18 C19 N3 2.0(13) . . . . ? Mn2 O5 C20 O6 0.3(11) . . . . ? Mn2 O5 C20 C21 -179.3(5) . . . . ? O5 C20 C21 C22 -163.5(7) . . . . ? O6 C20 C21 C22 16.9(11) . . . . ? O5 C20 C21 C26 17.1(11) . . . . ? O6 C20 C21 C26 -162.5(7) . . . . ? C26 C21 C22 C23 1.7(11) . . . . ? C20 C21 C22 C23 -177.6(7) . . . . ? C21 C22 C23 C24 -1.8(12) . . . . ? C21 C22 C23 C27 179.4(7) . . . . ? C22 C23 C24 C25 2.5(12) . . . . ? C27 C23 C24 C25 -178.8(7) . . . . ? C23 C24 C25 C26 -3.1(13) . . . . ? C24 C25 C26 C21 3.1(13) . . . . ? C22 C21 C26 C25 -2.4(12) . . . . ? C20 C21 C26 C25 177.0(7) . . . . ? Mn2 O7 C27 O8 5.3(7) 1_655 . . . ? Mn2 O7 C27 C23 -171.4(7) 1_655 . . . ? Mn2 O8 C27 O7 -5.5(8) 1_655 . . . ? Mn2 O8 C27 C23 171.3(6) 1_655 . . . ? C24 C23 C27 O7 173.9(7) . . . . ? C22 C23 C27 O7 -7.4(11) . . . . ? C24 C23 C27 O8 -2.9(11) . . . . ? C22 C23 C27 O8 175.8(7) . . . . ? C32 N4 C28 C29 0.6(13) . . . . ? Mn2 N4 C28 C29 161.0(6) . . . . ? N4 C28 C29 C30 -0.8(13) . . . . ? N4 C28 C29 C33 177.9(8) . . . . ? C28 C29 C30 C31 0.7(14) . . . . ? C33 C29 C30 C31 -177.9(9) . . . . ? C29 C30 C31 C32 -0.5(16) . . . . ? C28 N4 C32 C31 -0.2(13) . . . . ? Mn2 N4 C32 C31 -161.4(7) . . . . ? C30 C31 C32 N4 0.2(15) . . . . ? C34 N5 C33 C29 -76.0(11) . . . . ? C30 C29 C33 N5 -41.3(12) . . . . ? C28 C29 C33 N5 140.2(8) . . . . ? C38 N6 C34 N5 -178.9(8) . . . . ? C38 N6 C34 C35 0.3(13) . . . . ? C33 N5 C34 N6 -178.5(7) . . . . ? C33 N5 C34 C35 2.4(13) . . . . ? N6 C34 C35 C36 1.2(13) . . . . ? N5 C34 C35 C36 -179.7(8) . . . . ? C34 C35 C36 C37 -2.8(15) . . . . ? C35 C36 C37 C38 2.7(16) . . . . ? C34 N6 C38 C37 -0.3(15) . . . . ? C36 C37 C38 N6 -1.1(16) . . . . ? 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 H1W1 O8 0.82 2.09 2.838(6) 152.1 2_766 O1W H1W2 O5 0.82 2.00 2.744(7) 151.5 2_666 O2W H2W1 O7 0.82 2.24 3.047(6) 169.4 2_756 O2W H2W2 N6 0.82 1.94 2.750(8) 168.9 1_644 O3W H3W1 O2 0.82 1.92 2.736(7) 178.7 2_656 O3W H3W2 O4W 0.82 1.86 2.684(7) 177.3 . O4W H4W1 O4 0.82 1.84 2.661(7) 177.9 2_656 O4W H4W2 O6 0.82 1.89 2.711(8) 177.9 . N2 H2N O1 0.86(9) 2.12(9) 2.976(9) 175(8) . N5 H5N O6 0.86(9) 2.50(5) 3.245(10) 145(7) 2_667 _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.453 _refine_diff_density_min -0.578 _refine_diff_density_rms 0.085 # start Validation Reply Form _vrf_PLAT417_complex1 ; PROBLEM: Short Inter D-H..H-D H3W2 .. H4W2 .. 1.86 Ang. RESPONSE: This short distance may cause by the strong hydrogen bonds between O3w and O4w and the packing effect of crystal. If replace this hydrogen bond with another one, short Mn-H distance will be detected. It should be noted that O4w does not affect the formation of the final network. ; # end Validation Reply Form #===END data_complex2 #TrackingRef '- cif.cif' _database_code_depnum_ccdc_archive 'CCDC 870297' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H17 Co N3 O5' _chemical_formula_sum 'C19 H17 Co N3 O5' _chemical_formula_weight 426.29 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 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.6544(19) _cell_length_b 20.825(4) _cell_length_c 10.138(2) _cell_angle_alpha 90.00 _cell_angle_beta 117.47(3) _cell_angle_gamma 90.00 _cell_volume 1808.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 7139 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 876 _exptl_absorpt_coefficient_mu 0.987 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8581 _exptl_absorpt_correction_T_max 0.8908 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 14082 _diffrn_reflns_av_R_equivalents 0.0766 _diffrn_reflns_av_sigmaI/netI 0.0894 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6273 _reflns_number_gt 4005 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0380P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.37(3) _refine_ls_number_reflns 6273 _refine_ls_number_parameters 512 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1267 _refine_ls_R_factor_gt 0.0715 _refine_ls_wR_factor_ref 0.1519 _refine_ls_wR_factor_gt 0.1320 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.012 _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 0.51518(13) 0.60397(6) 0.63070(11) 0.0448(3) Uani 1 1 d . . . Co2 Co 1.05372(13) 0.39604(6) 0.38591(11) 0.0468(4) Uani 1 1 d . . . O1 O 0.6269(7) 0.6841(3) 0.7699(6) 0.0526(17) Uani 1 1 d . . . O1W O 0.4487(6) 0.5113(3) 0.5465(6) 0.0585(18) Uani 1 1 d . . . H1W1 H 0.3873 0.5287 0.4687 0.088 Uiso 1 1 d R . . H1W2 H 0.4022 0.4827 0.5653 0.088 Uiso 1 1 d R . . O2 O 0.7289(7) 0.5882(3) 0.8340(7) 0.0508(18) Uani 1 1 d . . . O2W O 1.0019(7) 0.4883(4) 0.2975(6) 0.0622(18) Uani 1 1 d D . . H2W1 H 0.941(7) 0.477(5) 0.208(4) 0.093 Uiso 1 1 d D . . H2W2 H 0.949(8) 0.503(5) 0.338(8) 0.093 Uiso 1 1 d D . . O3 O 1.3335(7) 0.6461(3) 1.4442(6) 0.0504(17) Uani 1 1 d . . . O4 O 1.2341(7) 0.5617(3) 1.2931(7) 0.0568(18) Uani 1 1 d . . . O5 O 1.2703(7) 0.4151(3) 0.5925(7) 0.0519(19) Uani 1 1 d . . . O6 O 1.1610(7) 0.3194(3) 0.5346(7) 0.0546(18) Uani 1 1 d . . . O7 O 1.7704(8) 0.4402(4) 1.0570(8) 0.076(2) Uani 1 1 d . . . O8 O 1.8739(7) 0.3544(3) 1.2058(6) 0.0534(17) Uani 1 1 d . . . N1 N 0.3818(8) 0.5930(4) 0.7607(8) 0.050(2) Uani 1 1 d . . . N2 N 0.1902(8) 0.6644(4) 0.6373(9) 0.050(2) Uani 1 1 d . . . H2N H 0.2388 0.6726 0.5864 0.060 Uiso 1 1 calc R . . N3 N -0.3383(9) 0.6142(4) 0.5197(8) 0.049(2) Uani 1 1 d . . . N4 N 0.9206(8) 0.4152(3) 0.5086(8) 0.047(2) Uani 1 1 d . . . N5 N 0.7342(9) 0.3360(4) 0.3993(9) 0.059(2) Uani 1 1 d . . . H5N H 0.7840 0.3256 0.3507 0.070 Uiso 1 1 calc R . . N6 N 0.2039(9) 0.3814(4) 0.2785(8) 0.053(2) Uani 1 1 d . . . C1 C 0.7337(10) 0.6470(5) 0.8600(10) 0.044(2) Uani 1 1 d . . . C2 C 0.8642(11) 0.6752(5) 0.9941(10) 0.049(3) Uani 1 1 d . . . C3 C 0.9822(10) 0.6373(5) 1.0860(10) 0.042(2) Uani 1 1 d . . . H3 H 0.9799 0.5938 1.0645 0.051 Uiso 1 1 calc R . . C4 C 1.1107(10) 0.6623(5) 1.2156(9) 0.049(3) Uani 1 1 d . . . C5 C 1.1149(12) 0.7281(6) 1.2398(11) 0.084(4) Uani 1 1 d . . . H5 H 1.1993 0.7464 1.3208 0.101 Uiso 1 1 calc R . . C6 C 0.9916(15) 0.7670(7) 1.1420(13) 0.109(5) Uani 1 1 d . . . H6 H 0.9930 0.8109 1.1593 0.130 Uiso 1 1 calc R . . C7 C 0.8699(13) 0.7404(6) 1.0220(12) 0.083(4) Uani 1 1 d . . . H7 H 0.7889 0.7666 0.9573 0.100 Uiso 1 1 calc R . . C8 C 1.2377(10) 0.6203(5) 1.3270(10) 0.041(2) Uani 1 1 d . . . C9 C 0.2551(11) 0.6225(5) 0.7474(9) 0.047(3) Uani 1 1 d . . . C10 C 0.1991(11) 0.6133(5) 0.8500(10) 0.051(3) Uani 1 1 d . . . H10 H 0.1124 0.6360 0.8415 0.062 Uiso 1 1 calc R . . C11 C 0.2719(12) 0.5710(5) 0.9625(11) 0.061(3) Uani 1 1 d . . . H11 H 0.2332 0.5637 1.0299 0.073 Uiso 1 1 calc R . . C12 C 0.4050(12) 0.5381(5) 0.9782(10) 0.059(3) Uani 1 1 d . . . H12 H 0.4571 0.5091 1.0553 0.071 Uiso 1 1 calc R . . C13 C 0.4557(12) 0.5509(5) 0.8727(10) 0.053(3) Uani 1 1 d . . . H13 H 0.5436 0.5297 0.8797 0.064 Uiso 1 1 calc R . . C14 C 0.0385(10) 0.6986(5) 0.5943(10) 0.052(3) Uani 1 1 d . . . H14A H 0.0272 0.7325 0.5245 0.063 Uiso 1 1 calc R . . H14B H 0.0413 0.7184 0.6821 0.063 Uiso 1 1 calc R . . C15 C -0.2118(10) 0.6509(5) 0.5732(10) 0.045(2) Uani 1 1 d . . . H15 H -0.1964 0.6770 0.6532 0.054 Uiso 1 1 calc R . . C16 C -0.1014(11) 0.6549(5) 0.5249(10) 0.047(3) Uani 1 1 d . . . C17 C -0.1305(12) 0.6147(6) 0.4054(11) 0.060(3) Uani 1 1 d . . . H17 H -0.0597 0.6137 0.3669 0.073 Uiso 1 1 calc R . . C18 C -0.2586(13) 0.5770(5) 0.3435(11) 0.066(3) Uani 1 1 d . . . H18 H -0.2761 0.5504 0.2635 0.079 Uiso 1 1 calc R . . C19 C -0.3626(11) 0.5785(5) 0.4011(11) 0.060(3) Uani 1 1 d . . . H19 H -0.4530 0.5540 0.3559 0.072 Uiso 1 1 calc R . . C20 C 1.2685(12) 0.3571(6) 0.6218(10) 0.046(3) Uani 1 1 d . . . C21 C 1.4042(12) 0.3272(5) 0.7557(11) 0.052(3) Uani 1 1 d . . . C22 C 1.5263(11) 0.3645(5) 0.8566(9) 0.046(2) Uani 1 1 d . . . H22 H 1.5250 0.4086 0.8416 0.056 Uiso 1 1 calc R . . C23 C 1.6481(11) 0.3379(5) 0.9773(11) 0.053(3) Uani 1 1 d . . . C24 C 1.6479(12) 0.2739(6) 1.0016(11) 0.060(3) Uani 1 1 d . . . H24 H 1.7307 0.2557 1.0841 0.092 Uiso 1 1 calc R . . C25 C 1.5271(15) 0.2353(7) 0.9061(14) 0.073(3) Uani 1 1 d . . . H25 H 1.5279 0.1915 0.9238 0.140 Uiso 1 1 calc R . . C26 C 1.4049(14) 0.2628(6) 0.7838(11) 0.062(3) Uani 1 1 d . . . H26 H 1.3220 0.2372 0.7197 0.105 Uiso 1 1 calc R . . C27 C 1.7715(10) 0.3838(6) 1.0858(10) 0.053(3) Uani 1 1 d . . . C28 C 0.7951(10) 0.3831(5) 0.5030(10) 0.052(3) Uani 1 1 d . . . C29 C 0.7320(11) 0.3979(6) 0.6018(10) 0.057(3) Uani 1 1 d . . . H29 H 0.6461 0.3754 0.5957 0.069 Uiso 1 1 calc R . . C30 C 0.7964(12) 0.4442(5) 0.7028(11) 0.063(3) Uani 1 1 d . . . H30 H 0.7573 0.4531 0.7692 0.076 Uiso 1 1 calc R . . C31 C 0.9240(12) 0.4796(5) 0.7094(11) 0.068(3) Uani 1 1 d . . . H31 H 0.9709 0.5126 0.7774 0.081 Uiso 1 1 calc R . . C32 C 0.9736(12) 0.4617(5) 0.6078(10) 0.058(3) Uani 1 1 d . . . H32 H 1.0556 0.4856 0.6092 0.070 Uiso 1 1 calc R . . C33 C 0.5894(11) 0.3020(5) 0.3649(10) 0.056(3) Uani 1 1 d . . . H33A H 0.5943 0.2861 0.4569 0.067 Uiso 1 1 calc R . . H33B H 0.5816 0.2651 0.3034 0.067 Uiso 1 1 calc R . . C34 C 0.3408(10) 0.3459(5) 0.3440(11) 0.050(3) Uani 1 1 d . . . H34 H 0.3638 0.3236 0.4312 0.060 Uiso 1 1 calc R . . C35 C 0.4439(12) 0.3421(5) 0.2860(11) 0.055(3) Uani 1 1 d . . . C36 C 0.4035(12) 0.3726(5) 0.1522(11) 0.061(3) Uani 1 1 d . . . H36 H 0.4711 0.3711 0.1102 0.074 Uiso 1 1 calc R . . C37 C 0.2635(11) 0.4054(5) 0.0799(10) 0.054(3) Uani 1 1 d . . . H37 H 0.2365 0.4260 -0.0100 0.064 Uiso 1 1 calc R . . C38 C 0.1643(11) 0.4068(5) 0.1446(11) 0.060(3) Uani 1 1 d . . . H38 H 0.0669 0.4261 0.0931 0.071 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0217(6) 0.0629(8) 0.0356(6) -0.0012(6) 0.0011(5) -0.0005(6) Co2 0.0221(7) 0.0651(9) 0.0366(6) 0.0014(6) -0.0007(5) -0.0016(6) O1 0.025(4) 0.076(5) 0.037(3) 0.006(3) -0.004(3) 0.004(4) O1W 0.023(4) 0.074(5) 0.054(4) -0.007(4) -0.003(3) -0.005(3) O2 0.025(4) 0.060(5) 0.049(4) -0.001(3) 0.001(3) 0.006(3) O2W 0.038(4) 0.088(5) 0.049(4) -0.002(4) 0.011(3) -0.003(4) O3 0.028(4) 0.075(5) 0.039(3) 0.004(3) 0.007(3) 0.000(3) O4 0.027(4) 0.076(5) 0.043(4) -0.007(4) -0.005(3) -0.002(3) O5 0.027(4) 0.066(5) 0.045(4) 0.016(3) 0.002(3) -0.004(3) O6 0.027(4) 0.066(4) 0.045(4) -0.001(3) -0.006(3) -0.003(3) O7 0.039(5) 0.062(5) 0.082(5) 0.009(4) -0.012(4) -0.007(4) O8 0.025(4) 0.077(5) 0.041(3) 0.004(3) 0.000(3) 0.002(4) N1 0.028(4) 0.065(6) 0.047(4) 0.001(4) 0.009(4) -0.003(4) N2 0.021(4) 0.061(6) 0.062(5) -0.001(4) 0.014(4) -0.001(4) N3 0.029(4) 0.060(6) 0.041(4) -0.001(4) 0.001(4) -0.004(4) N4 0.021(4) 0.049(5) 0.045(4) -0.003(4) -0.009(3) -0.008(4) N5 0.035(5) 0.076(6) 0.061(6) -0.016(5) 0.018(5) -0.002(5) N6 0.031(5) 0.073(6) 0.043(4) 0.003(4) 0.008(4) -0.003(4) C1 0.023(6) 0.067(8) 0.041(5) -0.007(6) 0.014(5) -0.001(5) C2 0.028(6) 0.059(7) 0.038(5) -0.005(5) -0.004(4) 0.006(5) C3 0.030(5) 0.048(6) 0.046(5) -0.017(5) 0.014(5) -0.003(5) C4 0.029(6) 0.061(7) 0.037(5) 0.000(5) -0.001(5) -0.005(5) C5 0.048(8) 0.070(9) 0.063(7) -0.011(6) -0.035(6) 0.000(6) C6 0.077(10) 0.061(9) 0.099(9) 0.001(7) -0.036(8) -0.001(7) C7 0.055(8) 0.057(8) 0.075(7) 0.003(6) -0.024(6) 0.006(6) C8 0.024(5) 0.053(7) 0.035(5) -0.010(5) 0.006(4) -0.007(4) C9 0.036(6) 0.061(7) 0.028(5) -0.001(4) 0.000(5) -0.011(5) C10 0.047(6) 0.051(6) 0.059(6) 0.010(5) 0.027(5) -0.001(5) C11 0.050(7) 0.082(8) 0.047(6) -0.001(6) 0.020(5) 0.003(6) C12 0.052(7) 0.065(7) 0.041(5) 0.018(5) 0.004(5) -0.008(6) C13 0.045(7) 0.055(6) 0.056(6) 0.017(5) 0.020(5) 0.005(5) C14 0.021(5) 0.066(7) 0.060(6) 0.006(5) 0.011(5) 0.008(5) C15 0.029(5) 0.061(6) 0.039(5) -0.010(5) 0.011(5) 0.001(5) C16 0.021(5) 0.070(7) 0.036(5) -0.002(5) 0.002(4) 0.003(5) C17 0.042(7) 0.083(8) 0.055(6) -0.008(6) 0.021(5) 0.000(6) C18 0.058(8) 0.086(9) 0.055(6) -0.033(6) 0.028(6) -0.017(6) C19 0.034(6) 0.086(8) 0.053(6) -0.016(6) 0.014(5) -0.005(5) C20 0.028(6) 0.071(8) 0.027(5) -0.009(6) 0.003(5) -0.005(6) C21 0.031(6) 0.063(8) 0.048(6) -0.001(5) 0.007(5) -0.008(5) C22 0.037(6) 0.052(6) 0.043(5) -0.007(5) 0.013(5) -0.001(5) C23 0.020(6) 0.067(8) 0.055(6) 0.002(6) 0.002(5) 0.005(5) C24 0.038(6) 0.069(8) 0.054(6) -0.001(5) 0.013(5) -0.002(5) C25 0.063(7) 0.080(8) 0.062(6) 0.005(6) 0.025(6) -0.007(6) C26 0.031(6) 0.075(8) 0.062(5) 0.008(6) 0.011(5) 0.015(6) C27 0.018(5) 0.091(9) 0.040(5) -0.001(6) 0.005(4) 0.005(6) C28 0.025(5) 0.064(7) 0.050(6) -0.005(5) 0.002(5) 0.011(5) C29 0.031(5) 0.082(8) 0.055(6) -0.008(7) 0.016(5) 0.013(7) C30 0.047(7) 0.082(8) 0.056(6) -0.011(6) 0.020(6) 0.016(6) C31 0.059(7) 0.076(8) 0.059(6) -0.001(6) 0.019(6) -0.015(6) C32 0.052(7) 0.073(7) 0.043(5) 0.009(6) 0.016(5) -0.010(6) C33 0.032(6) 0.057(7) 0.054(6) 0.006(5) -0.001(5) 0.004(5) C34 0.019(5) 0.076(7) 0.050(6) -0.004(5) 0.012(5) 0.000(5) C35 0.033(6) 0.062(7) 0.060(6) 0.002(6) 0.011(5) 0.007(5) C36 0.050(7) 0.077(8) 0.053(6) -0.001(6) 0.021(5) 0.007(6) C37 0.048(6) 0.064(7) 0.043(5) 0.002(5) 0.016(5) 0.012(6) C38 0.034(6) 0.069(8) 0.056(6) 0.010(6) 0.004(5) 0.007(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1W 2.087(6) . ? Co1 O3 2.089(6) 1_454 ? Co1 O1 2.130(6) . ? Co1 O2 2.166(6) . ? Co1 N3 2.186(8) 1_655 ? Co1 N1 2.240(7) . ? Co1 C1 2.476(9) . ? Co2 O8 2.044(6) 1_454 ? Co2 O2W 2.081(8) . ? Co2 O6 2.111(6) . ? Co2 N4 2.199(8) . ? Co2 N6 2.200(7) 1_655 ? Co2 O5 2.208(6) . ? Co2 C20 2.470(10) . ? O1 C1 1.275(11) . ? O1W H1W1 0.8200 . ? O1W H1W2 0.8200 . ? O2 C1 1.251(11) . ? O2W H2W1 0.85(5) . ? O2W H2W2 0.85(5) . ? O3 C8 1.241(10) . ? O3 Co1 2.089(6) 1_656 ? O4 C8 1.265(11) . ? O5 C20 1.247(11) . ? O6 C20 1.276(11) . ? O7 C27 1.208(13) . ? O8 C27 1.313(11) . ? O8 Co2 2.044(6) 1_656 ? N1 C9 1.318(11) . ? N1 C13 1.349(11) . ? N2 C9 1.324(11) . ? N2 C14 1.501(11) . ? N2 H2N 0.8600 . ? N3 C15 1.327(11) . ? N3 C19 1.338(11) . ? N3 Co1 2.186(8) 1_455 ? N4 C32 1.317(11) . ? N4 C28 1.363(11) . ? N5 C28 1.358(11) . ? N5 C33 1.459(12) . ? N5 H5N 0.8600 . ? N6 C38 1.338(11) . ? N6 C34 1.387(11) . ? N6 Co2 2.200(7) 1_455 ? C1 C2 1.484(12) . ? C2 C3 1.345(12) . ? C2 C7 1.383(15) . ? C3 C4 1.425(12) . ? C3 H3 0.9300 . ? C4 C5 1.390(14) . ? C4 C8 1.505(12) . ? C5 C6 1.402(14) . ? C5 H5 0.9300 . ? C6 C7 1.359(14) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C9 C10 1.390(12) . ? C10 C11 1.354(13) . ? C10 H10 0.9300 . ? C11 C12 1.399(13) . ? C11 H11 0.9300 . ? C12 C13 1.391(12) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C16 1.507(12) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.366(12) . ? C15 H15 0.9300 . ? C16 C17 1.391(13) . ? C17 C18 1.350(13) . ? C17 H17 0.9300 . ? C18 C19 1.375(13) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.518(14) . ? C21 C26 1.371(15) . ? C21 C22 1.388(13) . ? C22 C23 1.364(12) . ? C22 H22 0.9300 . ? C23 C24 1.355(14) . ? C23 C27 1.528(14) . ? C24 C25 1.379(15) . ? C24 H24 0.9300 . ? C25 C26 1.381(14) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C28 C29 1.425(12) . ? C29 C30 1.332(15) . ? C29 H29 0.9300 . ? C30 C31 1.411(14) . ? C30 H30 0.9300 . ? C31 C32 1.372(12) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C35 1.508(13) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.372(13) . ? C34 H34 0.9300 . ? C35 C36 1.381(13) . ? C36 C37 1.384(12) . ? C36 H36 0.9300 . ? C37 C38 1.389(13) . ? C37 H37 0.9300 . ? C38 H38 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 O1W Co1 O3 92.7(2) . 1_454 ? O1W Co1 O1 164.0(2) . . ? O3 Co1 O1 103.1(2) 1_454 . ? O1W Co1 O2 103.1(2) . . ? O3 Co1 O2 163.5(3) 1_454 . ? O1 Co1 O2 61.3(2) . . ? O1W Co1 N3 91.7(3) . 1_655 ? O3 Co1 N3 88.0(3) 1_454 1_655 ? O1 Co1 N3 90.9(3) . 1_655 ? O2 Co1 N3 86.9(3) . 1_655 ? O1W Co1 N1 89.7(3) . . ? O3 Co1 N1 96.0(3) 1_454 . ? O1 Co1 N1 86.7(3) . . ? O2 Co1 N1 88.7(3) . . ? N3 Co1 N1 175.7(3) 1_655 . ? O1W Co1 C1 133.4(3) . . ? O3 Co1 C1 133.9(3) 1_454 . ? O1 Co1 C1 31.0(3) . . ? O2 Co1 C1 30.3(3) . . ? N3 Co1 C1 88.6(3) 1_655 . ? N1 Co1 C1 87.5(3) . . ? O8 Co2 O2W 94.1(3) 1_454 . ? O8 Co2 O6 104.6(3) 1_454 . ? O2W Co2 O6 161.3(2) . . ? O8 Co2 N4 96.1(3) 1_454 . ? O2W Co2 N4 89.4(2) . . ? O6 Co2 N4 87.5(3) . . ? O8 Co2 N6 88.9(3) 1_454 1_655 ? O2W Co2 N6 89.9(3) . 1_655 ? O6 Co2 N6 91.7(3) . 1_655 ? N4 Co2 N6 175.0(3) . 1_655 ? O8 Co2 O5 165.1(3) 1_454 . ? O2W Co2 O5 100.2(3) . . ? O6 Co2 O5 61.4(2) . . ? N4 Co2 O5 88.6(2) . . ? N6 Co2 O5 86.7(3) 1_655 . ? O8 Co2 C20 135.5(3) 1_454 . ? O2W Co2 C20 130.4(3) . . ? O6 Co2 C20 31.1(3) . . ? N4 Co2 C20 87.8(3) . . ? N6 Co2 C20 89.0(3) 1_655 . ? O5 Co2 C20 30.3(3) . . ? C1 O1 Co1 89.7(6) . . ? Co1 O1W H1W1 86.3 . . ? Co1 O1W H1W2 132.5 . . ? H1W1 O1W H1W2 108.2 . . ? C1 O2 Co1 88.7(6) . . ? Co2 O2W H2W1 97(8) . . ? Co2 O2W H2W2 102(7) . . ? H2W1 O2W H2W2 110(7) . . ? C8 O3 Co1 128.9(6) . 1_656 ? C20 O5 Co2 86.6(6) . . ? C20 O6 Co2 90.2(6) . . ? C27 O8 Co2 126.5(7) . 1_656 ? C9 N1 C13 119.7(8) . . ? C9 N1 Co1 130.5(7) . . ? C13 N1 Co1 109.7(6) . . ? C9 N2 C14 125.2(8) . . ? C9 N2 H2N 117.4 . . ? C14 N2 H2N 117.4 . . ? C15 N3 C19 115.7(8) . . ? C15 N3 Co1 122.5(6) . 1_455 ? C19 N3 Co1 121.5(7) . 1_455 ? C32 N4 C28 114.6(8) . . ? C32 N4 Co2 116.3(6) . . ? C28 N4 Co2 128.9(6) . . ? C28 N5 C33 124.1(8) . . ? C28 N5 H5N 118.0 . . ? C33 N5 H5N 118.0 . . ? C38 N6 C34 117.4(8) . . ? C38 N6 Co2 120.1(7) . 1_455 ? C34 N6 Co2 122.5(6) . 1_455 ? O2 C1 O1 120.3(9) . . ? O2 C1 C2 121.0(10) . . ? O1 C1 C2 118.7(9) . . ? O2 C1 Co1 61.0(5) . . ? O1 C1 Co1 59.3(5) . . ? C2 C1 Co1 177.7(8) . . ? C3 C2 C7 119.6(9) . . ? C3 C2 C1 119.5(9) . . ? C7 C2 C1 120.8(9) . . ? C2 C3 C4 121.5(9) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? C5 C4 C3 117.7(9) . . ? C5 C4 C8 119.5(8) . . ? C3 C4 C8 122.7(9) . . ? C4 C5 C6 119.9(10) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C7 C6 C5 120.0(12) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C2 121.2(11) . . ? C6 C7 H7 119.4 . . ? C2 C7 H7 119.4 . . ? O3 C8 O4 126.3(9) . . ? O3 C8 C4 117.1(9) . . ? O4 C8 C4 116.5(8) . . ? N1 C9 N2 116.7(8) . . ? N1 C9 C10 121.4(9) . . ? N2 C9 C10 121.7(10) . . ? C11 C10 C9 119.4(10) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 120.5(9) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C13 C12 C11 116.7(9) . . ? C13 C12 H12 121.7 . . ? C11 C12 H12 121.7 . . ? N1 C13 C12 122.3(9) . . ? N1 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? N2 C14 C16 113.1(8) . . ? N2 C14 H14A 109.0 . . ? C16 C14 H14A 109.0 . . ? N2 C14 H14B 109.0 . . ? C16 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? N3 C15 C16 127.8(9) . . ? N3 C15 H15 116.1 . . ? C16 C15 H15 116.1 . . ? C15 C16 C17 113.5(9) . . ? C15 C16 C14 123.3(9) . . ? C17 C16 C14 123.2(9) . . ? C18 C17 C16 121.9(9) . . ? C18 C17 H17 119.0 . . ? C16 C17 H17 119.0 . . ? C17 C18 C19 118.7(9) . . ? C17 C18 H18 120.6 . . ? C19 C18 H18 120.6 . . ? N3 C19 C18 122.4(9) . . ? N3 C19 H19 118.8 . . ? C18 C19 H19 118.8 . . ? O5 C20 O6 121.8(9) . . ? O5 C20 C21 120.6(10) . . ? O6 C20 C21 117.3(10) . . ? O5 C20 Co2 63.1(5) . . ? O6 C20 Co2 58.7(5) . . ? C21 C20 Co2 173.2(7) . . ? C26 C21 C22 118.3(10) . . ? C26 C21 C20 120.4(9) . . ? C22 C21 C20 121.2(10) . . ? C23 C22 C21 121.4(10) . . ? C23 C22 H22 119.3 . . ? C21 C22 H22 119.3 . . ? C24 C23 C22 119.4(10) . . ? C24 C23 C27 123.4(9) . . ? C22 C23 C27 117.0(10) . . ? C23 C24 C25 121.1(10) . . ? C23 C24 H24 119.4 . . ? C25 C24 H24 119.4 . . ? C24 C25 C26 119.0(12) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? C21 C26 C25 120.8(11) . . ? C21 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? O7 C27 O8 126.6(10) . . ? O7 C27 C23 121.1(9) . . ? O8 C27 C23 112.2(10) . . ? N5 C28 N4 116.5(8) . . ? N5 C28 C29 121.9(10) . . ? N4 C28 C29 121.6(10) . . ? C30 C29 C28 119.9(11) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? C29 C30 C31 120.1(10) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C32 C31 C30 114.9(10) . . ? C32 C31 H31 122.5 . . ? C30 C31 H31 122.5 . . ? N4 C32 C31 128.7(10) . . ? N4 C32 H32 115.6 . . ? C31 C32 H32 115.6 . . ? N5 C33 C35 114.4(9) . . ? N5 C33 H33A 108.7 . . ? C35 C33 H33A 108.7 . . ? N5 C33 H33B 108.7 . . ? C35 C33 H33B 108.7 . . ? H33A C33 H33B 107.6 . . ? C35 C34 N6 123.0(9) . . ? C35 C34 H34 118.5 . . ? N6 C34 H34 118.5 . . ? C34 C35 C36 117.5(10) . . ? C34 C35 C33 119.1(9) . . ? C36 C35 C33 123.2(9) . . ? C35 C36 C37 120.8(9) . . ? C35 C36 H36 119.6 . . ? C37 C36 H36 119.6 . . ? C36 C37 C38 118.6(9) . . ? C36 C37 H37 120.7 . . ? C38 C37 H37 120.7 . . ? N6 C38 C37 122.3(9) . . ? N6 C38 H38 118.9 . . ? C37 C38 H38 118.9 . . ? 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 O1W Co1 O1 C1 13.3(11) . . . . ? O3 Co1 O1 C1 -174.0(5) 1_454 . . . ? O2 Co1 O1 C1 0.3(5) . . . . ? N3 Co1 O1 C1 -85.8(5) 1_655 . . . ? N1 Co1 O1 C1 90.6(5) . . . . ? O1W Co1 O2 C1 -176.6(5) . . . . ? O3 Co1 O2 C1 20.0(12) 1_454 . . . ? O1 Co1 O2 C1 -0.3(5) . . . . ? N3 Co1 O2 C1 92.4(6) 1_655 . . . ? N1 Co1 O2 C1 -87.2(6) . . . . ? O8 Co2 O5 C20 -20.6(13) 1_454 . . . ? O2W Co2 O5 C20 177.0(6) . . . . ? O6 Co2 O5 C20 0.1(6) . . . . ? N4 Co2 O5 C20 88.0(6) . . . . ? N6 Co2 O5 C20 -93.7(6) 1_655 . . . ? O8 Co2 O6 C20 174.5(5) 1_454 . . . ? O2W Co2 O6 C20 -9.5(11) . . . . ? N4 Co2 O6 C20 -89.9(6) . . . . ? N6 Co2 O6 C20 85.2(6) 1_655 . . . ? O5 Co2 O6 C20 -0.1(5) . . . . ? O1W Co1 N1 C9 -113.0(8) . . . . ? O3 Co1 N1 C9 -20.3(9) 1_454 . . . ? O1 Co1 N1 C9 82.6(8) . . . . ? O2 Co1 N1 C9 143.9(8) . . . . ? C1 Co1 N1 C9 113.6(9) . . . . ? O1W Co1 N1 C13 70.7(6) . . . . ? O3 Co1 N1 C13 163.3(6) 1_454 . . . ? O1 Co1 N1 C13 -93.8(6) . . . . ? O2 Co1 N1 C13 -32.4(6) . . . . ? C1 Co1 N1 C13 -62.8(7) . . . . ? O8 Co2 N4 C32 -156.6(6) 1_454 . . . ? O2W Co2 N4 C32 -62.5(6) . . . . ? O6 Co2 N4 C32 99.0(6) . . . . ? O5 Co2 N4 C32 37.7(6) . . . . ? C20 Co2 N4 C32 67.9(7) . . . . ? O8 Co2 N4 C28 27.8(7) 1_454 . . . ? O2W Co2 N4 C28 121.8(7) . . . . ? O6 Co2 N4 C28 -76.6(7) . . . . ? O5 Co2 N4 C28 -138.0(7) . . . . ? C20 Co2 N4 C28 -107.8(7) . . . . ? Co1 O2 C1 O1 0.5(9) . . . . ? Co1 O2 C1 C2 -178.6(8) . . . . ? Co1 O1 C1 O2 -0.5(9) . . . . ? Co1 O1 C1 C2 178.6(7) . . . . ? O1W Co1 C1 O2 4.5(7) . . . . ? O3 Co1 C1 O2 -172.3(5) 1_454 . . . ? O1 Co1 C1 O2 179.5(9) . . . . ? N3 Co1 C1 O2 -86.4(6) 1_655 . . . ? N1 Co1 C1 O2 91.8(6) . . . . ? O1W Co1 C1 O1 -175.0(4) . . . . ? O3 Co1 C1 O1 8.2(6) 1_454 . . . ? O2 Co1 C1 O1 -179.5(9) . . . . ? N3 Co1 C1 O1 94.1(5) 1_655 . . . ? N1 Co1 C1 O1 -87.8(5) . . . . ? O2 C1 C2 C3 2.7(15) . . . . ? O1 C1 C2 C3 -176.4(9) . . . . ? O2 C1 C2 C7 179.5(10) . . . . ? O1 C1 C2 C7 0.4(15) . . . . ? C7 C2 C3 C4 2.6(16) . . . . ? C1 C2 C3 C4 179.5(8) . . . . ? C2 C3 C4 C5 -3.6(15) . . . . ? C2 C3 C4 C8 174.9(9) . . . . ? C3 C4 C5 C6 2.9(17) . . . . ? C8 C4 C5 C6 -175.6(11) . . . . ? C4 C5 C6 C7 -1(2) . . . . ? C5 C6 C7 C2 0(2) . . . . ? C3 C2 C7 C6 -1.0(19) . . . . ? C1 C2 C7 C6 -177.8(11) . . . . ? Co1 O3 C8 O4 -2.9(14) 1_656 . . . ? Co1 O3 C8 C4 175.3(5) 1_656 . . . ? C5 C4 C8 O3 6.9(14) . . . . ? C3 C4 C8 O3 -171.5(8) . . . . ? C5 C4 C8 O4 -174.7(10) . . . . ? C3 C4 C8 O4 6.9(13) . . . . ? C13 N1 C9 N2 178.4(8) . . . . ? Co1 N1 C9 N2 2.4(13) . . . . ? C13 N1 C9 C10 2.8(14) . . . . ? Co1 N1 C9 C10 -173.3(7) . . . . ? C14 N2 C9 N1 174.3(8) . . . . ? C14 N2 C9 C10 -10.1(14) . . . . ? N1 C9 C10 C11 -3.0(15) . . . . ? N2 C9 C10 C11 -178.5(9) . . . . ? C9 C10 C11 C12 1.9(15) . . . . ? C10 C11 C12 C13 -0.6(15) . . . . ? C9 N1 C13 C12 -1.4(14) . . . . ? Co1 N1 C13 C12 175.4(8) . . . . ? C11 C12 C13 N1 0.3(14) . . . . ? C9 N2 C14 C16 -70.0(11) . . . . ? C19 N3 C15 C16 -2.4(15) . . . . ? Co1 N3 C15 C16 171.2(8) 1_455 . . . ? N3 C15 C16 C17 -0.1(15) . . . . ? N3 C15 C16 C14 179.9(9) . . . . ? N2 C14 C16 C15 127.6(10) . . . . ? N2 C14 C16 C17 -52.3(13) . . . . ? C15 C16 C17 C18 1.4(15) . . . . ? C14 C16 C17 C18 -178.6(10) . . . . ? C16 C17 C18 C19 -0.1(17) . . . . ? C15 N3 C19 C18 3.8(15) . . . . ? Co1 N3 C19 C18 -169.9(8) 1_455 . . . ? C17 C18 C19 N3 -2.7(17) . . . . ? Co2 O5 C20 O6 -0.1(10) . . . . ? Co2 O5 C20 C21 173.5(8) . . . . ? Co2 O6 C20 O5 0.2(10) . . . . ? Co2 O6 C20 C21 -173.7(7) . . . . ? O8 Co2 C20 O5 172.6(5) 1_454 . . . ? O2W Co2 C20 O5 -3.8(7) . . . . ? O6 Co2 C20 O5 -179.9(9) . . . . ? N4 Co2 C20 O5 -91.1(6) . . . . ? N6 Co2 C20 O5 85.1(6) 1_655 . . . ? O8 Co2 C20 O6 -7.6(7) 1_454 . . . ? O2W Co2 C20 O6 176.0(5) . . . . ? N4 Co2 C20 O6 88.8(5) . . . . ? N6 Co2 C20 O6 -95.0(6) 1_655 . . . ? O5 Co2 C20 O6 179.9(9) . . . . ? O5 C20 C21 C26 -177.1(10) . . . . ? O6 C20 C21 C26 -3.2(15) . . . . ? O5 C20 C21 C22 6.2(15) . . . . ? O6 C20 C21 C22 -179.9(9) . . . . ? C26 C21 C22 C23 3.0(16) . . . . ? C20 C21 C22 C23 179.8(9) . . . . ? C21 C22 C23 C24 -1.9(16) . . . . ? C21 C22 C23 C27 -176.6(8) . . . . ? C22 C23 C24 C25 0.3(18) . . . . ? C27 C23 C24 C25 174.7(12) . . . . ? C23 C24 C25 C26 0(2) . . . . ? C22 C21 C26 C25 -2.6(18) . . . . ? C20 C21 C26 C25 -179.4(12) . . . . ? C24 C25 C26 C21 1(2) . . . . ? Co2 O8 C27 O7 4.5(14) 1_656 . . . ? Co2 O8 C27 C23 -176.9(5) 1_656 . . . ? C24 C23 C27 O7 177.1(11) . . . . ? C22 C23 C27 O7 -8.3(14) . . . . ? C24 C23 C27 O8 -1.5(14) . . . . ? C22 C23 C27 O8 173.0(8) . . . . ? C33 N5 C28 N4 -172.3(9) . . . . ? C33 N5 C28 C29 8.2(14) . . . . ? C32 N4 C28 N5 178.2(8) . . . . ? Co2 N4 C28 N5 -6.1(12) . . . . ? C32 N4 C28 C29 -2.3(13) . . . . ? Co2 N4 C28 C29 173.4(7) . . . . ? N5 C28 C29 C30 179.4(9) . . . . ? N4 C28 C29 C30 -0.1(16) . . . . ? C28 C29 C30 C31 1.8(16) . . . . ? C29 C30 C31 C32 -1.0(15) . . . . ? C28 N4 C32 C31 3.4(14) . . . . ? Co2 N4 C32 C31 -172.9(9) . . . . ? C30 C31 C32 N4 -1.8(16) . . . . ? C28 N5 C33 C35 70.2(12) . . . . ? C38 N6 C34 C35 7.6(14) . . . . ? Co2 N6 C34 C35 -172.8(7) 1_455 . . . ? N6 C34 C35 C36 -3.4(15) . . . . ? N6 C34 C35 C33 -179.7(9) . . . . ? N5 C33 C35 C34 -126.5(10) . . . . ? N5 C33 C35 C36 57.4(13) . . . . ? C34 C35 C36 C37 -0.3(16) . . . . ? C33 C35 C36 C37 175.8(9) . . . . ? C35 C36 C37 C38 -0.2(15) . . . . ? C34 N6 C38 C37 -8.1(15) . . . . ? Co2 N6 C38 C37 172.3(8) 1_455 . . . ? C36 C37 C38 N6 4.6(15) . . . . ? 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 H1W1 O4 0.82 1.84 2.661(8) 174.1 1_454 O1W H1W1 O3 0.82 2.49 3.022(9) 123.6 1_454 O1W H1W2 O5 0.82 2.00 2.818(9) 174.4 1_455 O2W H2W1 O7 0.85(5) 1.82(4) 2.629(9) 157(9) 1_454 O2W H2W2 N4 0.85(5) 2.61(10) 3.010(10) 110(8) . N2 H2N O3 0.86 2.11 2.897(10) 152.6 1_454 N5 H5N O8 0.86 2.11 2.873(10) 147.8 1_454 _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.791 _refine_diff_density_min -0.480 _refine_diff_density_rms 0.097 #===END data_complex3 #TrackingRef '- cif.cif' _database_code_depnum_ccdc_archive 'CCDC 870298' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H15 N3 O4 Zn' _chemical_formula_sum 'C19 H15 N3 O4 Zn' _chemical_formula_weight 414.71 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 9.1940(18) _cell_length_b 10.167(2) _cell_length_c 10.905(2) _cell_angle_alpha 114.80(3) _cell_angle_beta 97.60(3) _cell_angle_gamma 102.10(3) _cell_volume 876.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 7228 _cell_measurement_theta_min 3.17 _cell_measurement_theta_max 27.47 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.571 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 424 _exptl_absorpt_coefficient_mu 1.432 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7826 _exptl_absorpt_correction_T_max 0.8469 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8660 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0606 _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 -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3964 _reflns_number_gt 3364 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0477P)^2^+0.6746P] 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 3964 _refine_ls_number_parameters 247 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.1090 _refine_ls_wR_factor_gt 0.0905 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _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 0.39546(3) 0.84008(3) 0.76077(3) 0.02655(12) Uani 1 1 d . . . O1 O 0.3139(2) 0.7161(2) 0.8509(2) 0.0329(4) Uani 1 1 d . . . O2 O 0.3843(2) 0.5416(2) 0.6854(2) 0.0374(5) Uani 1 1 d . . . O3 O 0.3429(2) 0.0271(2) 0.8728(2) 0.0337(4) Uani 1 1 d . . . O4 O 0.4606(2) 0.1007(2) 0.7380(2) 0.0413(5) Uani 1 1 d . . . N1 N 0.2577(2) 0.7661(2) 0.5663(2) 0.0274(5) Uani 1 1 d . . . N2 N 0.0479(2) 0.6786(3) 0.6335(2) 0.0296(5) Uani 1 1 d D . . H2N H 0.113(3) 0.685(4) 0.701(2) 0.036 Uiso 1 1 d D . . N3 N -0.3794(2) 0.8690(2) 0.7710(2) 0.0259(4) Uani 1 1 d . . . C1 C 0.3407(3) 0.5867(3) 0.7940(3) 0.0271(5) Uani 1 1 d . . . C2 C 0.3133(3) 0.4887(3) 0.8654(3) 0.0260(5) Uani 1 1 d . . . C3 C 0.3576(3) 0.3573(3) 0.8182(3) 0.0263(5) Uani 1 1 d . . . H3A H 0.4042 0.3323 0.7441 0.032 Uiso 1 1 calc R . . C4 C 0.3335(3) 0.2630(3) 0.8801(3) 0.0259(5) Uani 1 1 d . . . C5 C 0.2640(3) 0.3000(3) 0.9901(3) 0.0327(6) Uani 1 1 d . . . H5A H 0.2463 0.2366 1.0314 0.039 Uiso 1 1 calc R . . C6 C 0.2205(4) 0.4323(3) 1.0386(3) 0.0405(7) Uani 1 1 d . . . H6A H 0.1746 0.4576 1.1131 0.049 Uiso 1 1 calc R . . C7 C 0.2450(3) 0.5262(3) 0.9770(3) 0.0352(6) Uani 1 1 d . . . H7A H 0.2159 0.6146 1.0101 0.042 Uiso 1 1 calc R . . C8 C 0.3847(3) 0.1218(3) 0.8254(3) 0.0290(6) Uani 1 1 d . . . C9 C 0.1039(3) 0.7217(3) 0.5433(3) 0.0263(5) Uani 1 1 d . . . C10 C 0.0100(3) 0.7195(4) 0.4301(3) 0.0406(7) Uani 1 1 d . . . H10A H -0.0961 0.6941 0.4172 0.049 Uiso 1 1 calc R . . C11 C 0.0762(4) 0.7553(5) 0.3386(4) 0.0542(9) Uani 1 1 d . . . H11A H 0.0147 0.7538 0.2629 0.065 Uiso 1 1 calc R . . C12 C 0.2334(4) 0.7934(4) 0.3579(4) 0.0517(9) Uani 1 1 d . . . H12A H 0.2794 0.8137 0.2942 0.062 Uiso 1 1 calc R . . C13 C 0.3190(3) 0.8005(4) 0.4739(3) 0.0378(7) Uani 1 1 d . . . H13A H 0.4254 0.8306 0.4900 0.045 Uiso 1 1 calc R . . C14 C -0.1129(3) 0.6409(3) 0.6327(3) 0.0291(6) Uani 1 1 d . . . H14A H -0.1320 0.5735 0.6745 0.035 Uiso 1 1 calc R . . H14B H -0.1734 0.5864 0.5368 0.035 Uiso 1 1 calc R . . C15 C -0.3220(3) 0.7579(3) 0.6971(3) 0.0271(5) Uani 1 1 d . . . H15A H -0.3901 0.6635 0.6344 0.032 Uiso 1 1 calc R . . C16 C -0.1663(3) 0.7775(3) 0.7101(3) 0.0244(5) Uani 1 1 d . . . C17 C -0.0669(3) 0.9214(3) 0.8018(3) 0.0321(6) Uani 1 1 d . . . H17A H 0.0386 0.9401 0.8120 0.039 Uiso 1 1 calc R . . C18 C -0.1261(3) 1.0358(3) 0.8772(3) 0.0351(6) Uani 1 1 d . . . H18A H -0.0607 1.1322 0.9383 0.042 Uiso 1 1 calc R . . C19 C -0.2819(3) 1.0065(3) 0.8617(3) 0.0291(5) Uani 1 1 d . . . H19A H -0.3210 1.0831 0.9149 0.035 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 0.02318(17) 0.02649(17) 0.0393(2) 0.02026(14) 0.01147(13) 0.01227(12) O1 0.0412(10) 0.0236(9) 0.0437(11) 0.0222(8) 0.0127(9) 0.0128(8) O2 0.0466(12) 0.0322(10) 0.0444(12) 0.0252(9) 0.0173(10) 0.0133(9) O3 0.0404(11) 0.0242(9) 0.0465(11) 0.0222(9) 0.0137(9) 0.0145(8) O4 0.0437(11) 0.0341(10) 0.0636(14) 0.0292(10) 0.0289(11) 0.0217(9) N1 0.0245(10) 0.0291(11) 0.0329(11) 0.0158(10) 0.0114(9) 0.0103(9) N2 0.0212(10) 0.0384(12) 0.0371(12) 0.0218(11) 0.0103(9) 0.0129(10) N3 0.0249(10) 0.0266(10) 0.0309(11) 0.0151(9) 0.0097(9) 0.0113(9) C1 0.0245(12) 0.0236(12) 0.0374(14) 0.0190(11) 0.0049(11) 0.0065(10) C2 0.0268(12) 0.0207(11) 0.0327(13) 0.0154(10) 0.0040(11) 0.0068(10) C3 0.0256(12) 0.0246(12) 0.0340(13) 0.0171(11) 0.0085(11) 0.0093(10) C4 0.0241(12) 0.0221(11) 0.0356(13) 0.0164(11) 0.0053(11) 0.0093(10) C5 0.0411(15) 0.0276(13) 0.0399(15) 0.0237(12) 0.0116(13) 0.0124(12) C6 0.0559(18) 0.0389(15) 0.0415(16) 0.0238(14) 0.0266(15) 0.0228(14) C7 0.0461(16) 0.0258(13) 0.0429(16) 0.0187(12) 0.0169(13) 0.0186(12) C8 0.0267(12) 0.0238(12) 0.0411(15) 0.0194(11) 0.0051(12) 0.0094(10) C9 0.0250(12) 0.0232(11) 0.0329(13) 0.0133(10) 0.0091(11) 0.0094(10) C10 0.0291(14) 0.0517(18) 0.0432(17) 0.0282(15) 0.0025(13) 0.0068(13) C11 0.0493(19) 0.073(2) 0.0468(19) 0.0410(19) 0.0027(16) 0.0086(18) C12 0.0515(19) 0.067(2) 0.0456(18) 0.0367(18) 0.0180(16) 0.0072(17) C13 0.0330(14) 0.0450(16) 0.0403(16) 0.0233(14) 0.0157(13) 0.0092(13) C14 0.0237(12) 0.0275(12) 0.0377(14) 0.0149(11) 0.0124(11) 0.0077(10) C15 0.0227(12) 0.0268(12) 0.0331(13) 0.0149(11) 0.0074(10) 0.0075(10) C16 0.0217(12) 0.0271(12) 0.0286(12) 0.0152(10) 0.0087(10) 0.0087(10) C17 0.0220(12) 0.0308(13) 0.0407(15) 0.0150(12) 0.0061(11) 0.0062(11) C18 0.0298(14) 0.0268(13) 0.0414(15) 0.0127(12) 0.0022(12) 0.0046(11) C19 0.0330(13) 0.0256(12) 0.0317(13) 0.0134(11) 0.0094(11) 0.0133(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O3 1.983(2) 1_565 ? Zn1 O1 1.9882(19) . ? Zn1 N3 2.010(2) 1_655 ? Zn1 N1 2.054(2) . ? O1 C1 1.292(3) . ? O2 C1 1.233(3) . ? O3 C8 1.288(3) . ? O3 Zn1 1.983(2) 1_545 ? O4 C8 1.228(3) . ? N1 C9 1.345(3) . ? N1 C13 1.349(3) . ? N2 C9 1.352(3) . ? N2 C14 1.445(3) . ? N2 H2N 0.854(10) . ? N3 C15 1.342(3) . ? N3 C19 1.348(3) . ? N3 Zn1 2.010(2) 1_455 ? C1 C2 1.503(3) . ? C2 C3 1.387(3) . ? C2 C7 1.391(4) . ? C3 C4 1.385(3) . ? C3 H3A 0.9300 . ? C4 C5 1.384(4) . ? C4 C8 1.509(3) . ? C5 C6 1.390(4) . ? C5 H5A 0.9300 . ? C6 C7 1.379(4) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C9 C10 1.399(4) . ? C10 C11 1.367(5) . ? C10 H10A 0.9300 . ? C11 C12 1.378(5) . ? C11 H11A 0.9300 . ? C12 C13 1.364(5) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C16 1.515(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.383(3) . ? C15 H15A 0.9300 . ? C16 C17 1.395(4) . ? C17 C18 1.381(4) . ? C17 H17A 0.9300 . ? C18 C19 1.373(4) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zn1 O1 98.98(8) 1_565 . ? O3 Zn1 N3 114.72(9) 1_565 1_655 ? O1 Zn1 N3 112.68(9) . 1_655 ? O3 Zn1 N1 101.81(9) 1_565 . ? O1 Zn1 N1 111.49(9) . . ? N3 Zn1 N1 115.51(9) 1_655 . ? C1 O1 Zn1 109.17(17) . . ? C8 O3 Zn1 107.81(17) . 1_545 ? C9 N1 C13 118.6(2) . . ? C9 N1 Zn1 120.46(18) . . ? C13 N1 Zn1 118.55(18) . . ? C9 N2 C14 124.0(2) . . ? C9 N2 H2N 117(2) . . ? C14 N2 H2N 118(2) . . ? C15 N3 C19 119.0(2) . . ? C15 N3 Zn1 123.58(17) . 1_455 ? C19 N3 Zn1 117.32(18) . 1_455 ? O2 C1 O1 123.1(2) . . ? O2 C1 C2 120.2(2) . . ? O1 C1 C2 116.7(2) . . ? C3 C2 C7 119.3(2) . . ? C3 C2 C1 118.8(2) . . ? C7 C2 C1 121.9(2) . . ? C4 C3 C2 120.8(2) . . ? C4 C3 H3A 119.6 . . ? C2 C3 H3A 119.6 . . ? C5 C4 C3 119.6(2) . . ? C5 C4 C8 121.7(2) . . ? C3 C4 C8 118.7(2) . . ? C4 C5 C6 119.9(2) . . ? C4 C5 H5A 120.1 . . ? C6 C5 H5A 120.1 . . ? C7 C6 C5 120.4(3) . . ? C7 C6 H6A 119.8 . . ? C5 C6 H6A 119.8 . . ? C6 C7 C2 120.1(3) . . ? C6 C7 H7A 120.0 . . ? C2 C7 H7A 120.0 . . ? O4 C8 O3 123.2(2) . . ? O4 C8 C4 119.9(2) . . ? O3 C8 C4 116.9(2) . . ? N1 C9 N2 116.4(2) . . ? N1 C9 C10 120.6(2) . . ? N2 C9 C10 123.1(2) . . ? C11 C10 C9 119.1(3) . . ? C11 C10 H10A 120.5 . . ? C9 C10 H10A 120.5 . . ? C10 C11 C12 120.5(3) . . ? C10 C11 H11A 119.8 . . ? C12 C11 H11A 119.8 . . ? C13 C12 C11 117.6(3) . . ? C13 C12 H12A 121.2 . . ? C11 C12 H12A 121.2 . . ? N1 C13 C12 123.5(3) . . ? N1 C13 H13A 118.2 . . ? C12 C13 H13A 118.2 . . ? N2 C14 C16 113.8(2) . . ? N2 C14 H14A 108.8 . . ? C16 C14 H14A 108.8 . . ? N2 C14 H14B 108.8 . . ? C16 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? N3 C15 C16 123.0(2) . . ? N3 C15 H15A 118.5 . . ? C16 C15 H15A 118.5 . . ? C15 C16 C17 117.4(2) . . ? C15 C16 C14 118.8(2) . . ? C17 C16 C14 123.7(2) . . ? C18 C17 C16 119.6(2) . . ? C18 C17 H17A 120.2 . . ? C16 C17 H17A 120.2 . . ? C19 C18 C17 119.7(2) . . ? C19 C18 H18A 120.2 . . ? C17 C18 H18A 120.2 . . ? N3 C19 C18 121.3(2) . . ? N3 C19 H19A 119.3 . . ? C18 C19 H19A 119.3 . . ? 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 Zn1 O1 C1 -178.36(17) 1_565 . . . ? N3 Zn1 O1 C1 -56.70(19) 1_655 . . . ? N1 Zn1 O1 C1 75.08(19) . . . . ? O3 Zn1 N1 C9 -64.8(2) 1_565 . . . ? O1 Zn1 N1 C9 39.9(2) . . . . ? N3 Zn1 N1 C9 170.18(18) 1_655 . . . ? O3 Zn1 N1 C13 97.5(2) 1_565 . . . ? O1 Zn1 N1 C13 -157.8(2) . . . . ? N3 Zn1 N1 C13 -27.5(2) 1_655 . . . ? Zn1 O1 C1 O2 -11.9(3) . . . . ? Zn1 O1 C1 C2 169.22(17) . . . . ? O2 C1 C2 C3 8.7(4) . . . . ? O1 C1 C2 C3 -172.4(2) . . . . ? O2 C1 C2 C7 -171.3(3) . . . . ? O1 C1 C2 C7 7.6(4) . . . . ? C7 C2 C3 C4 0.6(4) . . . . ? C1 C2 C3 C4 -179.5(2) . . . . ? C2 C3 C4 C5 0.2(4) . . . . ? C2 C3 C4 C8 -179.7(2) . . . . ? C3 C4 C5 C6 -0.7(4) . . . . ? C8 C4 C5 C6 179.1(3) . . . . ? C4 C5 C6 C7 0.6(5) . . . . ? C5 C6 C7 C2 0.1(5) . . . . ? C3 C2 C7 C6 -0.7(4) . . . . ? C1 C2 C7 C6 179.3(3) . . . . ? Zn1 O3 C8 O4 -8.2(3) 1_545 . . . ? Zn1 O3 C8 C4 170.64(18) 1_545 . . . ? C5 C4 C8 O4 -172.2(3) . . . . ? C3 C4 C8 O4 7.6(4) . . . . ? C5 C4 C8 O3 8.9(4) . . . . ? C3 C4 C8 O3 -171.2(2) . . . . ? C13 N1 C9 N2 175.6(2) . . . . ? Zn1 N1 C9 N2 -22.1(3) . . . . ? C13 N1 C9 C10 -3.6(4) . . . . ? Zn1 N1 C9 C10 158.7(2) . . . . ? C14 N2 C9 N1 174.1(2) . . . . ? C14 N2 C9 C10 -6.8(4) . . . . ? N1 C9 C10 C11 3.5(5) . . . . ? N2 C9 C10 C11 -175.6(3) . . . . ? C9 C10 C11 C12 -0.2(6) . . . . ? C10 C11 C12 C13 -2.8(6) . . . . ? C9 N1 C13 C12 0.4(5) . . . . ? Zn1 N1 C13 C12 -162.3(3) . . . . ? C11 C12 C13 N1 2.8(5) . . . . ? C9 N2 C14 C16 -83.3(3) . . . . ? C19 N3 C15 C16 0.3(4) . . . . ? Zn1 N3 C15 C16 -176.80(19) 1_455 . . . ? N3 C15 C16 C17 -1.9(4) . . . . ? N3 C15 C16 C14 174.0(2) . . . . ? N2 C14 C16 C15 169.5(2) . . . . ? N2 C14 C16 C17 -14.9(4) . . . . ? C15 C16 C17 C18 1.5(4) . . . . ? C14 C16 C17 C18 -174.1(3) . . . . ? C16 C17 C18 C19 0.3(4) . . . . ? C15 N3 C19 C18 1.7(4) . . . . ? Zn1 N3 C19 C18 179.0(2) 1_455 . . . ? C17 C18 C19 N3 -2.0(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 N2 H2N O1 0.854(10) 2.170(12) 3.011(3) 168(3) . _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.878 _refine_diff_density_min -0.543 _refine_diff_density_rms 0.097 #===END data_complex4 #TrackingRef '- cif.cif' _database_code_depnum_ccdc_archive 'CCDC 870299' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H19 Cd2 N3 O8' _chemical_formula_sum 'C27 H19 Cd2 N3 O8' _chemical_formula_weight 738.25 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_space_group_name_Hall '-P 2yn ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.055(2) _cell_length_b 13.112(3) _cell_length_c 16.940(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.21(3) _cell_angle_gamma 90.00 _cell_volume 2557.7(9) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 17109 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 27.46 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.917 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 1.720 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7139 _exptl_absorpt_correction_T_max 0.7947 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 24200 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5830 _reflns_number_gt 5063 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0801P)^2^+3.4956P] 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 5830 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1349 _refine_ls_wR_factor_gt 0.1302 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _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 Cd1 Cd 0.64387(2) 0.146382(19) 0.776846(18) 0.01929(12) Uani 1 1 d . . . Cd2 Cd 0.83303(2) 0.356175(19) 0.703733(18) 0.01922(12) Uani 1 1 d . . . O1 O 0.5267(2) 0.2432(2) 0.67785(18) 0.0265(6) Uani 1 1 d . . . O2 O 0.6637(3) 0.3523(2) 0.74175(18) 0.0252(6) Uani 1 1 d . . . O3 O 0.2814(3) 0.3436(2) 0.39966(19) 0.0269(7) Uani 1 1 d . . . O4 O 0.2168(3) 0.4998(2) 0.37724(19) 0.0320(8) Uani 1 1 d . . . O5 O 0.7751(3) 0.1453(2) 0.70080(18) 0.0245(6) Uani 1 1 d . . . O6 O 0.7436(3) 0.2558(2) 0.59740(17) 0.0274(6) Uani 1 1 d . . . O7 O 0.4563(3) -0.0020(2) 0.28881(19) 0.0316(7) Uani 1 1 d . . . O8 O 0.4519(3) 0.1548(2) 0.3341(2) 0.0289(7) Uani 1 1 d . . . N1 N 0.5047(3) 0.1880(3) 0.8484(2) 0.0349(9) Uani 1 1 d . . . N2 N 0.3465(4) 0.1165(3) 0.7542(3) 0.0451(10) Uani 1 1 d . . . H2N H 0.3945 0.0834 0.7349 0.054 Uiso 1 1 calc R . . N3 N 0.0029(3) 0.3213(3) 0.6663(2) 0.0318(8) Uani 1 1 d . . . C1 C 0.5697(3) 0.3327(3) 0.6888(3) 0.0205(8) Uani 1 1 d . . . C2 C 0.5018(3) 0.4139(3) 0.6331(2) 0.0177(7) Uani 1 1 d . . . C3 C 0.4252(3) 0.3886(3) 0.5577(2) 0.0186(7) Uani 1 1 d . . . H3 H 0.4169 0.3207 0.5410 0.022 Uiso 1 1 calc R . . C4 C 0.3597(3) 0.4637(3) 0.5060(2) 0.0181(7) Uani 1 1 d . . . C5 C 0.3713(3) 0.5642(3) 0.5322(2) 0.0231(8) Uani 1 1 d . . . H5 H 0.3263 0.6145 0.4991 0.028 Uiso 1 1 calc R . . C6 C 0.4502(4) 0.5905(3) 0.6079(3) 0.0251(8) Uani 1 1 d . . . H6 H 0.4589 0.6585 0.6243 0.030 Uiso 1 1 calc R . . C7 C 0.5156(3) 0.5159(3) 0.6587(2) 0.0209(8) Uani 1 1 d . . . H7 H 0.5681 0.5333 0.7092 0.025 Uiso 1 1 calc R . . C8 C 0.2817(3) 0.4344(3) 0.4228(2) 0.0197(7) Uani 1 1 d . . . C9 C 0.7395(3) 0.1668(3) 0.6246(2) 0.0205(8) Uani 1 1 d . . . C10 C 0.6930(3) 0.0857(3) 0.5623(2) 0.0196(7) Uani 1 1 d . . . C11 C 0.6192(3) 0.1111(3) 0.4849(2) 0.0198(7) Uani 1 1 d . . . H11 H 0.5994 0.1791 0.4726 0.024 Uiso 1 1 calc R . . C12 C 0.5747(3) 0.0368(3) 0.4261(2) 0.0202(7) Uani 1 1 d . . . C13 C 0.6048(4) -0.0646(3) 0.4447(3) 0.0256(8) Uani 1 1 d . . . H13 H 0.5759 -0.1150 0.4054 0.031 Uiso 1 1 calc R . . C14 C 0.6780(4) -0.0909(3) 0.5221(3) 0.0291(9) Uani 1 1 d . . . H14 H 0.6975 -0.1589 0.5344 0.035 Uiso 1 1 calc R . . C15 C 0.7220(4) -0.0164(3) 0.5810(3) 0.0244(8) Uani 1 1 d . . . H15 H 0.7708 -0.0343 0.6328 0.029 Uiso 1 1 calc R . . C16 C 0.4888(3) 0.0647(3) 0.3451(2) 0.0208(8) Uani 1 1 d . . . C17 C 0.3901(4) 0.1738(4) 0.8232(3) 0.0380(11) Uani 1 1 d . . . C18 C 0.3190(5) 0.2157(6) 0.8666(4) 0.0633(18) Uani 1 1 d . . . H18 H 0.2393 0.2043 0.8487 0.076 Uiso 1 1 calc R . . C19 C 0.3660(6) 0.2730(8) 0.9348(4) 0.089(3) Uani 1 1 d . . . H19 H 0.3195 0.2999 0.9647 0.107 Uiso 1 1 calc R . . C20 C 0.4836(6) 0.2908(7) 0.9590(4) 0.079(2) Uani 1 1 d . . . H20 H 0.5177 0.3322 1.0042 0.095 Uiso 1 1 calc R . . C21 C 0.5490(5) 0.2463(5) 0.9154(3) 0.0564(16) Uani 1 1 d . . . H21 H 0.6288 0.2569 0.9331 0.068 Uiso 1 1 calc R . . C22 C 0.2236(4) 0.1081(4) 0.7113(4) 0.0474(13) Uani 1 1 d . . . H22A H 0.1851 0.0764 0.7478 0.057 Uiso 1 1 calc R . . H22B H 0.2132 0.0639 0.6637 0.057 Uiso 1 1 calc R . . C23 C 0.0574(4) 0.2322(4) 0.6896(3) 0.0333(9) Uani 1 1 d . . . H23 H 0.0201 0.1826 0.7118 0.040 Uiso 1 1 calc R . . C24 C 0.1661(4) 0.2102(4) 0.6824(3) 0.0367(10) Uani 1 1 d . . . C25 C 0.2211(5) 0.2857(5) 0.6504(4) 0.0488(13) Uani 1 1 d . . . H25 H 0.2950 0.2747 0.6453 0.059 Uiso 1 1 calc R . . C26 C 0.1658(5) 0.3761(4) 0.6264(4) 0.0539(15) Uani 1 1 d . . . H26 H 0.2018 0.4267 0.6044 0.065 Uiso 1 1 calc R . . C27 C 0.0565(5) 0.3932(4) 0.6346(3) 0.0429(12) Uani 1 1 d . . . H27 H 0.0197 0.4553 0.6179 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 Cd1 0.02034(18) 0.01990(18) 0.01450(17) 0.00224(10) 0.00031(12) 0.00167(9) Cd2 0.01906(18) 0.01938(18) 0.01583(18) -0.00188(10) -0.00004(12) -0.00077(9) O1 0.0286(15) 0.0166(13) 0.0281(15) 0.0034(12) -0.0013(12) -0.0013(11) O2 0.0366(18) 0.0271(15) 0.0107(13) -0.0040(10) 0.0050(12) -0.0007(11) O3 0.0296(17) 0.0253(14) 0.0190(15) -0.0041(11) -0.0033(12) -0.0016(11) O4 0.0312(17) 0.0288(17) 0.0253(15) 0.0088(12) -0.0082(13) -0.0030(11) O5 0.0238(16) 0.0310(16) 0.0151(14) -0.0018(11) 0.0000(11) 0.0039(10) O6 0.0391(17) 0.0177(13) 0.0211(13) -0.0017(12) 0.0024(12) -0.0047(12) O7 0.0405(19) 0.0281(17) 0.0178(14) -0.0037(12) -0.0041(12) -0.0104(12) O8 0.0331(18) 0.0258(15) 0.0195(15) 0.0000(11) -0.0048(12) 0.0051(12) N1 0.028(2) 0.051(3) 0.0243(18) 0.0004(18) 0.0065(15) 0.0057(17) N2 0.024(2) 0.050(2) 0.060(3) -0.007(2) 0.0103(19) 0.0051(18) N3 0.0271(19) 0.038(2) 0.0301(19) -0.0024(17) 0.0077(15) -0.0010(16) C1 0.0207(19) 0.0216(18) 0.0198(19) 0.0083(16) 0.0071(15) 0.0038(15) C2 0.0206(18) 0.0157(17) 0.0156(17) 0.0006(14) 0.0034(14) -0.0003(13) C3 0.0185(18) 0.0195(17) 0.0147(16) -0.0016(15) -0.0001(13) -0.0016(14) C4 0.0164(17) 0.0182(17) 0.0177(17) 0.0021(15) 0.0019(13) -0.0002(13) C5 0.0227(19) 0.0246(19) 0.0182(18) 0.0039(16) 0.0001(15) 0.0033(15) C6 0.031(2) 0.0190(18) 0.0228(19) -0.0063(16) 0.0038(16) -0.0039(15) C7 0.0236(19) 0.0224(18) 0.0137(16) -0.0030(15) 0.0012(14) -0.0011(15) C8 0.0174(18) 0.0247(18) 0.0150(17) 0.0026(15) 0.0019(14) -0.0021(14) C9 0.0180(18) 0.0256(18) 0.0169(18) -0.0014(16) 0.0037(14) -0.0011(15) C10 0.0202(18) 0.0217(18) 0.0148(17) -0.0019(15) 0.0017(14) -0.0018(14) C11 0.0236(19) 0.0160(17) 0.0178(17) 0.0014(15) 0.0030(14) -0.0004(14) C12 0.0181(18) 0.0250(19) 0.0151(17) 0.0005(15) 0.0013(14) -0.0010(14) C13 0.029(2) 0.0222(19) 0.0215(19) -0.0060(17) 0.0006(16) -0.0030(16) C14 0.033(2) 0.0212(19) 0.028(2) 0.0023(17) 0.0004(17) 0.0040(16) C15 0.023(2) 0.0245(19) 0.0209(18) 0.0040(16) -0.0010(15) 0.0019(15) C16 0.0180(18) 0.0266(19) 0.0149(17) -0.0004(16) 0.0005(14) -0.0045(15) C17 0.033(3) 0.048(3) 0.036(3) 0.004(2) 0.015(2) 0.009(2) C18 0.037(3) 0.114(6) 0.043(3) -0.004(4) 0.018(2) 0.009(3) C19 0.056(4) 0.174(9) 0.041(3) -0.025(4) 0.023(3) 0.029(5) C20 0.061(4) 0.133(7) 0.040(3) -0.035(4) 0.012(3) 0.020(4) C21 0.037(3) 0.087(4) 0.045(3) -0.027(3) 0.010(2) 0.004(3) C22 0.026(3) 0.044(3) 0.070(4) -0.006(3) 0.010(2) -0.001(2) C23 0.027(2) 0.038(2) 0.035(2) 0.000(2) 0.0089(18) -0.0023(18) C24 0.026(2) 0.042(2) 0.042(3) -0.007(2) 0.0086(19) -0.0016(19) C25 0.031(3) 0.056(3) 0.067(4) 0.001(3) 0.028(3) 0.000(2) C26 0.048(3) 0.051(3) 0.074(4) 0.010(3) 0.035(3) -0.003(3) C27 0.045(3) 0.039(3) 0.048(3) 0.012(2) 0.020(2) 0.008(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 Cd1 O1 2.240(3) . ? Cd1 O3 2.248(3) 4_666 ? Cd1 O5 2.317(3) . ? Cd1 O7 2.342(3) 3_656 ? Cd1 N1 2.405(4) . ? Cd1 O4 2.540(3) 4_666 ? Cd1 C8 2.751(4) 4_666 ? Cd2 O6 2.234(3) . ? Cd2 O8 2.254(3) 4_666 ? Cd2 O4 2.307(3) 3_666 ? Cd2 O2 2.316(3) . ? Cd2 N3 2.360(4) 1_655 ? Cd2 O7 2.583(3) 4_666 ? O1 C1 1.275(5) . ? O2 C1 1.246(5) . ? O3 C8 1.254(5) . ? O3 Cd1 2.248(3) 4_565 ? O4 C8 1.259(5) . ? O4 Cd2 2.307(3) 3_666 ? O4 Cd1 2.540(3) 4_565 ? O5 C9 1.266(5) . ? O6 C9 1.261(5) . ? O7 C16 1.267(5) . ? O7 Cd1 2.342(3) 3_656 ? O7 Cd2 2.583(3) 4_565 ? O8 C16 1.256(5) . ? O8 Cd2 2.254(3) 4_565 ? N1 C17 1.333(6) . ? N1 C21 1.341(7) . ? N2 C17 1.359(7) . ? N2 C22 1.449(6) . ? N2 H2N 0.8600 . ? N3 C23 1.342(6) . ? N3 C27 1.342(6) . ? N3 Cd2 2.360(4) 1_455 ? C1 C2 1.495(5) . ? C2 C3 1.378(5) . ? C2 C7 1.400(5) . ? C3 C4 1.397(5) . ? C3 H3 0.9300 . ? C4 C5 1.384(5) . ? C4 C8 1.494(5) . ? C5 C6 1.395(6) . ? C5 H5 0.9300 . ? C6 C7 1.385(6) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 Cd1 2.751(4) 4_565 ? C9 C10 1.486(5) . ? C10 C11 1.389(5) . ? C10 C15 1.396(5) . ? C11 C12 1.385(5) . ? C11 H11 0.9300 . ? C12 C13 1.389(6) . ? C12 C16 1.499(5) . ? C13 C14 1.389(6) . ? C13 H13 0.9300 . ? C14 C15 1.385(6) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C17 C18 1.396(7) . ? C18 C19 1.353(10) . ? C18 H18 0.9300 . ? C19 C20 1.374(10) . ? C19 H19 0.9300 . ? C20 C21 1.360(7) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C24 1.521(7) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.383(6) . ? C23 H23 0.9300 . ? C24 C25 1.388(7) . ? C25 C26 1.362(8) . ? C25 H25 0.9300 . ? C26 C27 1.383(7) . ? C26 H26 0.9300 . ? C27 H27 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 O1 Cd1 O3 142.08(10) . 4_666 ? O1 Cd1 O5 88.29(11) . . ? O3 Cd1 O5 94.42(11) 4_666 . ? O1 Cd1 O7 88.86(10) . 3_656 ? O3 Cd1 O7 128.48(10) 4_666 3_656 ? O5 Cd1 O7 94.13(12) . 3_656 ? O1 Cd1 N1 82.50(12) . . ? O3 Cd1 N1 87.33(12) 4_666 . ? O5 Cd1 N1 166.99(12) . . ? O7 Cd1 N1 94.85(14) 3_656 . ? O1 Cd1 O4 160.97(10) . 4_666 ? O3 Cd1 O4 53.86(10) 4_666 4_666 ? O5 Cd1 O4 102.12(11) . 4_666 ? O7 Cd1 O4 74.68(10) 3_656 4_666 ? N1 Cd1 O4 89.33(13) . 4_666 ? O1 Cd1 C8 166.10(11) . 4_666 ? O3 Cd1 C8 26.71(11) 4_666 4_666 ? O5 Cd1 C8 99.64(11) . 4_666 ? O7 Cd1 C8 101.82(11) 3_656 4_666 ? N1 Cd1 C8 87.70(12) . 4_666 ? O4 Cd1 C8 27.15(10) 4_666 4_666 ? O6 Cd2 O8 140.19(10) . 4_666 ? O6 Cd2 O4 91.39(10) . 3_666 ? O8 Cd2 O4 127.80(10) 4_666 3_666 ? O6 Cd2 O2 87.50(11) . . ? O8 Cd2 O2 94.77(12) 4_666 . ? O4 Cd2 O2 95.04(12) 3_666 . ? O6 Cd2 N3 85.39(12) . 1_655 ? O8 Cd2 N3 84.28(13) 4_666 1_655 ? O4 Cd2 N3 95.32(14) 3_666 1_655 ? O2 Cd2 N3 167.57(12) . 1_655 ? O6 Cd2 O7 161.20(11) . 4_666 ? O8 Cd2 O7 53.58(10) 4_666 4_666 ? O4 Cd2 O7 74.41(10) 3_666 4_666 ? O2 Cd2 O7 105.67(11) . 4_666 ? N3 Cd2 O7 83.77(13) 1_655 4_666 ? C1 O1 Cd1 105.9(2) . . ? C1 O2 Cd2 119.5(3) . . ? C8 O3 Cd1 99.6(2) . 4_565 ? C8 O4 Cd2 158.0(3) . 3_666 ? C8 O4 Cd1 85.8(2) . 4_565 ? Cd2 O4 Cd1 104.00(11) 3_666 4_565 ? C9 O5 Cd1 119.0(3) . . ? C9 O6 Cd2 108.2(2) . . ? C16 O7 Cd1 156.4(3) . 3_656 ? C16 O7 Cd2 84.7(2) . 4_565 ? Cd1 O7 Cd2 101.69(11) 3_656 4_565 ? C16 O8 Cd2 100.3(2) . 4_565 ? C17 N1 C21 117.7(4) . . ? C17 N1 Cd1 128.2(3) . . ? C21 N1 Cd1 113.2(3) . . ? C17 N2 C22 123.5(4) . . ? C17 N2 H2N 118.3 . . ? C22 N2 H2N 118.3 . . ? C23 N3 C27 118.5(4) . . ? C23 N3 Cd2 118.6(3) . 1_455 ? C27 N3 Cd2 122.1(3) . 1_455 ? O2 C1 O1 122.6(4) . . ? O2 C1 C2 121.2(4) . . ? O1 C1 C2 116.2(4) . . ? C3 C2 C7 120.1(3) . . ? C3 C2 C1 120.3(3) . . ? C7 C2 C1 119.5(3) . . ? C2 C3 C4 120.7(4) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 119.0(3) . . ? C5 C4 C8 121.5(3) . . ? C3 C4 C8 119.4(3) . . ? C4 C5 C6 120.5(4) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C7 C6 C5 120.3(4) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C2 119.3(4) . . ? C6 C7 H7 120.4 . . ? C2 C7 H7 120.4 . . ? O3 C8 O4 120.7(4) . . ? O3 C8 C4 118.8(3) . . ? O4 C8 C4 120.5(3) . . ? O3 C8 Cd1 53.7(2) . 4_565 ? O4 C8 Cd1 67.1(2) . 4_565 ? C4 C8 Cd1 172.2(3) . 4_565 ? O6 C9 O5 122.6(4) . . ? O6 C9 C10 116.8(3) . . ? O5 C9 C10 120.5(3) . . ? C11 C10 C15 119.5(3) . . ? C11 C10 C9 120.0(3) . . ? C15 C10 C9 120.5(3) . . ? C12 C11 C10 120.9(4) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C11 C12 C13 119.3(3) . . ? C11 C12 C16 120.2(4) . . ? C13 C12 C16 120.3(3) . . ? C12 C13 C14 120.1(4) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C15 C14 C13 120.4(4) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C10 119.7(4) . . ? C14 C15 H15 120.1 . . ? C10 C15 H15 120.1 . . ? O8 C16 O7 121.4(4) . . ? O8 C16 C12 118.9(3) . . ? O7 C16 C12 119.7(3) . . ? N1 C17 N2 116.9(4) . . ? N1 C17 C18 121.1(5) . . ? N2 C17 C18 122.0(5) . . ? C19 C18 C17 120.0(6) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C20 118.9(5) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C21 C20 C19 118.5(6) . . ? C21 C20 H20 120.7 . . ? C19 C20 H20 120.7 . . ? N1 C21 C20 123.7(6) . . ? N1 C21 H21 118.2 . . ? C20 C21 H21 118.2 . . ? N2 C22 C24 113.3(4) . . ? N2 C22 H22A 108.9 . . ? C24 C22 H22A 108.9 . . ? N2 C22 H22B 108.9 . . ? C24 C22 H22B 108.9 . . ? H22A C22 H22B 107.7 . . ? N3 C23 C24 123.3(4) . . ? N3 C23 H23 118.3 . . ? C24 C23 H23 118.3 . . ? C23 C24 C25 117.5(5) . . ? C23 C24 C22 120.5(4) . . ? C25 C24 C22 121.9(4) . . ? C26 C25 C24 119.2(5) . . ? C26 C25 H25 120.4 . . ? C24 C25 H25 120.4 . . ? C25 C26 C27 120.6(5) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? N3 C27 C26 120.8(5) . . ? N3 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? 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 O3 Cd1 O1 C1 18.3(3) 4_666 . . . ? O5 Cd1 O1 C1 -76.7(3) . . . . ? O7 Cd1 O1 C1 -170.9(3) 3_656 . . . ? N1 Cd1 O1 C1 94.0(3) . . . . ? O4 Cd1 O1 C1 159.4(3) 4_666 . . . ? C8 Cd1 O1 C1 48.5(6) 4_666 . . . ? O6 Cd2 O2 C1 -23.1(3) . . . . ? O8 Cd2 O2 C1 -163.3(3) 4_666 . . . ? O4 Cd2 O2 C1 68.1(3) 3_666 . . . ? N3 Cd2 O2 C1 -78.2(6) 1_655 . . . ? O7 Cd2 O2 C1 143.3(3) 4_666 . . . ? O1 Cd1 O5 C9 -19.6(3) . . . . ? O3 Cd1 O5 C9 -161.8(3) 4_666 . . . ? O7 Cd1 O5 C9 69.1(3) 3_656 . . . ? N1 Cd1 O5 C9 -64.5(6) . . . . ? O4 Cd1 O5 C9 144.3(3) 4_666 . . . ? C8 Cd1 O5 C9 171.8(3) 4_666 . . . ? O8 Cd2 O6 C9 19.1(4) 4_666 . . . ? O4 Cd2 O6 C9 -170.3(3) 3_666 . . . ? O2 Cd2 O6 C9 -75.3(3) . . . . ? N3 Cd2 O6 C9 94.5(3) 1_655 . . . ? O7 Cd2 O6 C9 149.4(3) 4_666 . . . ? O1 Cd1 N1 C17 55.2(4) . . . . ? O3 Cd1 N1 C17 -161.4(4) 4_666 . . . ? O5 Cd1 N1 C17 100.6(7) . . . . ? O7 Cd1 N1 C17 -33.0(4) 3_656 . . . ? O4 Cd1 N1 C17 -107.5(4) 4_666 . . . ? C8 Cd1 N1 C17 -134.6(4) 4_666 . . . ? O1 Cd1 N1 C21 -113.8(4) . . . . ? O3 Cd1 N1 C21 29.6(4) 4_666 . . . ? O5 Cd1 N1 C21 -68.4(7) . . . . ? O7 Cd1 N1 C21 158.0(4) 3_656 . . . ? O4 Cd1 N1 C21 83.5(4) 4_666 . . . ? C8 Cd1 N1 C21 56.4(4) 4_666 . . . ? Cd2 O2 C1 O1 95.3(4) . . . . ? Cd2 O2 C1 C2 -83.5(4) . . . . ? Cd1 O1 C1 O2 5.0(5) . . . . ? Cd1 O1 C1 C2 -176.1(3) . . . . ? O2 C1 C2 C3 155.7(4) . . . . ? O1 C1 C2 C3 -23.2(5) . . . . ? O2 C1 C2 C7 -25.1(6) . . . . ? O1 C1 C2 C7 156.0(4) . . . . ? C7 C2 C3 C4 -0.5(6) . . . . ? C1 C2 C3 C4 178.7(3) . . . . ? C2 C3 C4 C5 -1.1(6) . . . . ? C2 C3 C4 C8 177.0(3) . . . . ? C3 C4 C5 C6 2.1(6) . . . . ? C8 C4 C5 C6 -175.9(4) . . . . ? C4 C5 C6 C7 -1.7(6) . . . . ? C5 C6 C7 C2 0.1(6) . . . . ? C3 C2 C7 C6 0.9(6) . . . . ? C1 C2 C7 C6 -178.3(4) . . . . ? Cd1 O3 C8 O4 -1.8(4) 4_565 . . . ? Cd1 O3 C8 C4 177.6(3) 4_565 . . . ? Cd2 O4 C8 O3 -116.1(7) 3_666 . . . ? Cd1 O4 C8 O3 1.5(4) 4_565 . . . ? Cd2 O4 C8 C4 64.5(9) 3_666 . . . ? Cd1 O4 C8 C4 -177.9(3) 4_565 . . . ? Cd2 O4 C8 Cd1 -117.7(8) 3_666 . . 4_565 ? C5 C4 C8 O3 174.4(4) . . . . ? C3 C4 C8 O3 -3.7(5) . . . . ? C5 C4 C8 O4 -6.2(6) . . . . ? C3 C4 C8 O4 175.7(4) . . . . ? Cd2 O6 C9 O5 4.2(5) . . . . ? Cd2 O6 C9 C10 -174.4(3) . . . . ? Cd1 O5 C9 O6 93.3(4) . . . . ? Cd1 O5 C9 C10 -88.2(4) . . . . ? O6 C9 C10 C11 -23.6(5) . . . . ? O5 C9 C10 C11 157.7(4) . . . . ? O6 C9 C10 C15 156.9(4) . . . . ? O5 C9 C10 C15 -21.7(6) . . . . ? C15 C10 C11 C12 -0.4(6) . . . . ? C9 C10 C11 C12 -179.9(3) . . . . ? C10 C11 C12 C13 -0.2(6) . . . . ? C10 C11 C12 C16 175.8(4) . . . . ? C11 C12 C13 C14 0.6(6) . . . . ? C16 C12 C13 C14 -175.4(4) . . . . ? C12 C13 C14 C15 -0.4(7) . . . . ? C13 C14 C15 C10 -0.2(7) . . . . ? C11 C10 C15 C14 0.6(6) . . . . ? C9 C10 C15 C14 -179.9(4) . . . . ? Cd2 O8 C16 O7 0.3(4) 4_565 . . . ? Cd2 O8 C16 C12 179.1(3) 4_565 . . . ? Cd1 O7 C16 O8 -107.5(7) 3_656 . . . ? Cd2 O7 C16 O8 -0.3(4) 4_565 . . . ? Cd1 O7 C16 C12 73.7(8) 3_656 . . . ? Cd2 O7 C16 C12 -179.1(3) 4_565 . . . ? C11 C12 C16 O8 -5.1(6) . . . . ? C13 C12 C16 O8 170.9(4) . . . . ? C11 C12 C16 O7 173.8(4) . . . . ? C13 C12 C16 O7 -10.3(6) . . . . ? C21 N1 C17 N2 178.5(5) . . . . ? Cd1 N1 C17 N2 10.0(7) . . . . ? C21 N1 C17 C18 -1.9(8) . . . . ? Cd1 N1 C17 C18 -170.4(5) . . . . ? C22 N2 C17 N1 -169.3(5) . . . . ? C22 N2 C17 C18 11.1(9) . . . . ? N1 C17 C18 C19 0.9(10) . . . . ? N2 C17 C18 C19 -179.5(7) . . . . ? C17 C18 C19 C20 1.4(13) . . . . ? C18 C19 C20 C21 -2.7(14) . . . . ? C17 N1 C21 C20 0.5(10) . . . . ? Cd1 N1 C21 C20 170.7(6) . . . . ? C19 C20 C21 N1 1.9(13) . . . . ? C17 N2 C22 C24 58.1(7) . . . . ? C27 N3 C23 C24 -0.2(7) . . . . ? Cd2 N3 C23 C24 -169.7(4) 1_455 . . . ? N3 C23 C24 C25 1.0(7) . . . . ? N3 C23 C24 C22 179.1(5) . . . . ? N2 C22 C24 C23 -138.7(5) . . . . ? N2 C22 C24 C25 39.3(7) . . . . ? C23 C24 C25 C26 -1.2(8) . . . . ? C22 C24 C25 C26 -179.3(6) . . . . ? C24 C25 C26 C27 0.7(10) . . . . ? C23 N3 C27 C26 -0.3(8) . . . . ? Cd2 N3 C27 C26 168.8(5) 1_455 . . . ? C25 C26 C27 N3 0.1(10) . . . . ? 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 N2 H2N O7 0.86 2.23 3.075(6) 168.2 3_656 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.317 _refine_diff_density_min -0.855 _refine_diff_density_rms 0.183 #===END data_complex5 #TrackingRef '- cif.cif' _database_code_depnum_ccdc_archive 'CCDC 870300' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H17 Mn N3 O5, C H4 O' _chemical_formula_sum 'C20 H21 Mn N3 O6' _chemical_formula_weight 454.34 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 '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0247(18) _cell_length_b 10.475(2) _cell_length_c 12.242(2) _cell_angle_alpha 99.96(3) _cell_angle_beta 110.61(3) _cell_angle_gamma 106.37(3) _cell_volume 990.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 5951 _cell_measurement_theta_min 3.24 _cell_measurement_theta_max 27.46 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 470 _exptl_absorpt_coefficient_mu 0.710 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8828 _exptl_absorpt_correction_T_max 0.9071 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9771 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0582 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 27.47 _reflns_number_total 4473 _reflns_number_gt 3255 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0567P)^2^+0.7730P] 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 4473 _refine_ls_number_parameters 284 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0703 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1408 _refine_ls_wR_factor_gt 0.1034 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _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 0.55704(6) 0.21343(4) 0.16593(4) 0.02864(15) Uani 1 1 d . . . O1 O 0.4981(3) 0.40768(19) 0.2065(2) 0.0353(5) Uani 1 1 d . . . O1W O 0.6883(3) 0.2565(2) 0.3665(2) 0.0402(5) Uani 1 1 d D . . H1W1 H 0.687(4) 0.337(2) 0.392(3) 0.060 Uiso 1 1 d D . . H1W2 H 0.787(2) 0.257(3) 0.407(3) 0.060 Uiso 1 1 d D . . O2 O 0.6644(4) 0.5002(3) 0.4075(2) 0.0646(8) Uani 1 1 d . . . O3 O 0.6206(3) 1.03089(19) 0.1439(2) 0.0373(5) Uani 1 1 d . . . O4 O 0.5641(3) 0.81990(19) 0.02604(19) 0.0343(5) Uani 1 1 d . . . O5 O 0.0171(4) 0.2590(3) 0.4806(3) 0.0690(8) Uani 1 1 d D . . H5O H 0.108(4) 0.332(4) 0.515(5) 0.103 Uiso 1 1 d D . . N1 N 0.3093(3) 0.0953(2) 0.1685(2) 0.0332(6) Uani 1 1 d . . . N2 N -0.1541(4) -0.3587(3) 0.0179(3) 0.0454(7) Uani 1 1 d D . . H2N H -0.256(2) -0.390(4) -0.040(3) 0.054 Uiso 1 1 d D . . N3 N -0.2063(3) -0.6286(3) 0.1709(3) 0.0362(6) Uani 1 1 d . . . C1 C 0.5725(4) 0.5050(3) 0.3050(3) 0.0347(7) Uani 1 1 d . . . C2 C 0.5539(4) 0.6442(3) 0.3051(3) 0.0290(6) Uani 1 1 d . . . C3 C 0.5638(4) 0.7026(3) 0.2133(3) 0.0282(6) Uani 1 1 d . . . H3 H 0.5702 0.6515 0.1461 0.034 Uiso 1 1 calc R . . C4 C 0.5643(4) 0.8376(3) 0.2206(3) 0.0304(6) Uani 1 1 d . . . C5 C 0.5490(5) 0.9103(3) 0.3191(3) 0.0410(8) Uani 1 1 d . . . H5 H 0.5499 1.0003 0.3252 0.049 Uiso 1 1 calc R . . C6 C 0.5325(5) 0.8504(3) 0.4089(3) 0.0465(9) Uani 1 1 d . . . H6 H 0.5171 0.8984 0.4728 0.056 Uiso 1 1 calc R . . C7 C 0.5390(4) 0.7187(3) 0.4030(3) 0.0371(7) Uani 1 1 d . . . H7 H 0.5332 0.6804 0.4651 0.044 Uiso 1 1 calc R . . C8 C 0.5835(4) 0.9012(3) 0.1222(3) 0.0292(6) Uani 1 1 d . . . C9 C 0.2139(4) -0.0324(3) 0.0895(3) 0.0320(6) Uani 1 1 d . . . H9 H 0.2482 -0.0648 0.0304 0.038 Uiso 1 1 calc R . . C10 C 0.0667(4) -0.1199(3) 0.0901(3) 0.0335(7) Uani 1 1 d . . . C11 C 0.0158(5) -0.0701(3) 0.1766(3) 0.0446(8) Uani 1 1 d . . . H11 H -0.0821 -0.1254 0.1802 0.054 Uiso 1 1 calc R . . C12 C 0.1107(5) 0.0625(4) 0.2583(4) 0.0495(9) Uani 1 1 d . . . H12 H 0.0765 0.0982 0.3163 0.059 Uiso 1 1 calc R . . C13 C 0.2573(4) 0.1414(3) 0.2524(3) 0.0415(8) Uani 1 1 d . . . H13 H 0.3225 0.2298 0.3086 0.050 Uiso 1 1 calc R . . C14 C -0.0268(4) -0.2593(3) -0.0022(3) 0.0371(7) Uani 1 1 d . . . H14A H -0.0819 -0.2468 -0.0812 0.044 Uiso 1 1 calc R . . H14B H 0.0559 -0.2996 -0.0073 0.044 Uiso 1 1 calc R . . C15 C -0.2343(4) -0.5479(3) 0.0984(3) 0.0324(6) Uani 1 1 d . . . H15 H -0.3463 -0.5680 0.0443 0.039 Uiso 1 1 calc R . . C16 C -0.1065(4) -0.4353(3) 0.0984(3) 0.0340(7) Uani 1 1 d . . . C17 C 0.0599(4) -0.4069(3) 0.1792(3) 0.0429(8) Uani 1 1 d . . . H17 H 0.1499 -0.3338 0.1822 0.051 Uiso 1 1 calc R . . C18 C 0.0898(4) -0.4892(4) 0.2553(4) 0.0491(9) Uani 1 1 d . . . H18 H 0.2004 -0.4707 0.3111 0.059 Uiso 1 1 calc R . . C19 C -0.0447(4) -0.5989(4) 0.2482(3) 0.0442(8) Uani 1 1 d . . . H19 H -0.0222 -0.6542 0.2990 0.053 Uiso 1 1 calc R . . C20 C 0.0046(7) 0.1864(6) 0.5647(5) 0.0880(16) Uani 1 1 d . . . H20A H 0.0758 0.1325 0.5718 0.132 Uiso 1 1 calc R . . H20B H -0.1116 0.1252 0.5370 0.132 Uiso 1 1 calc R . . H20C H 0.0410 0.2517 0.6432 0.132 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 0.0351(3) 0.0196(2) 0.0312(3) 0.00874(17) 0.0155(2) 0.00775(17) O1 0.0440(13) 0.0213(9) 0.0388(12) 0.0074(9) 0.0171(10) 0.0113(8) O1W 0.0511(15) 0.0275(10) 0.0383(13) 0.0092(9) 0.0132(11) 0.0170(10) O2 0.111(2) 0.0410(14) 0.0390(15) 0.0132(11) 0.0155(15) 0.0447(15) O3 0.0491(13) 0.0218(10) 0.0446(13) 0.0126(9) 0.0212(11) 0.0149(9) O4 0.0478(13) 0.0269(10) 0.0300(12) 0.0089(8) 0.0180(10) 0.0140(9) O5 0.062(2) 0.080(2) 0.0553(19) 0.0267(16) 0.0131(16) 0.0245(15) N1 0.0343(14) 0.0286(12) 0.0381(15) 0.0119(11) 0.0196(12) 0.0074(10) N2 0.0333(15) 0.0364(14) 0.057(2) 0.0213(13) 0.0132(14) 0.0022(11) N3 0.0355(15) 0.0329(13) 0.0424(16) 0.0152(11) 0.0196(12) 0.0096(11) C1 0.0456(18) 0.0262(14) 0.0362(18) 0.0106(12) 0.0204(15) 0.0143(12) C2 0.0330(15) 0.0207(12) 0.0319(16) 0.0079(11) 0.0119(12) 0.0102(11) C3 0.0353(16) 0.0210(12) 0.0269(15) 0.0041(11) 0.0132(12) 0.0104(11) C4 0.0353(16) 0.0246(13) 0.0285(15) 0.0055(11) 0.0121(13) 0.0106(11) C5 0.065(2) 0.0276(15) 0.0398(19) 0.0122(13) 0.0256(17) 0.0251(15) C6 0.085(3) 0.0364(17) 0.0354(18) 0.0118(14) 0.0345(19) 0.0342(17) C7 0.054(2) 0.0313(15) 0.0309(17) 0.0133(12) 0.0209(15) 0.0176(14) C8 0.0284(15) 0.0249(13) 0.0343(16) 0.0122(12) 0.0114(12) 0.0105(11) C9 0.0376(17) 0.0264(13) 0.0360(17) 0.0114(12) 0.0211(14) 0.0094(12) C10 0.0375(17) 0.0274(14) 0.0391(18) 0.0160(13) 0.0176(14) 0.0115(12) C11 0.045(2) 0.0428(18) 0.055(2) 0.0182(16) 0.0324(18) 0.0118(15) C12 0.062(2) 0.0448(19) 0.055(2) 0.0139(17) 0.040(2) 0.0193(17) C13 0.047(2) 0.0359(16) 0.0409(19) 0.0103(14) 0.0229(16) 0.0098(14) C14 0.0398(18) 0.0300(15) 0.0414(19) 0.0166(13) 0.0189(15) 0.0074(12) C15 0.0252(15) 0.0305(14) 0.0390(18) 0.0126(12) 0.0136(13) 0.0055(11) C16 0.0352(17) 0.0270(14) 0.0382(18) 0.0101(12) 0.0177(14) 0.0062(12) C17 0.0368(18) 0.0350(16) 0.050(2) 0.0144(15) 0.0161(16) 0.0060(13) C18 0.0313(18) 0.050(2) 0.055(2) 0.0202(17) 0.0095(16) 0.0091(14) C19 0.0415(19) 0.0489(19) 0.049(2) 0.0264(16) 0.0202(16) 0.0189(15) C20 0.072(3) 0.106(4) 0.085(4) 0.053(3) 0.023(3) 0.029(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O4 2.129(2) 2_665 ? Mn1 O3 2.146(2) 1_545 ? Mn1 O1W 2.214(2) . ? Mn1 N1 2.244(3) . ? Mn1 O1 2.262(2) . ? Mn1 N3 2.277(3) 1_665 ? O1 C1 1.250(4) . ? O1W H1W1 0.85(3) . ? O1W H1W2 0.86(4) . ? O2 C1 1.256(4) . ? O3 C8 1.259(3) . ? O3 Mn1 2.146(2) 1_565 ? O4 C8 1.252(4) . ? O4 Mn1 2.129(2) 2_665 ? O5 C20 1.399(5) . ? O5 H5O 0.86(5) . ? N1 C9 1.336(4) . ? N1 C13 1.343(4) . ? N2 C16 1.403(4) . ? N2 C14 1.442(4) . ? N2 H2N 0.86(4) . ? N3 C15 1.338(4) . ? N3 C19 1.338(4) . ? N3 Mn1 2.277(3) 1_445 ? C1 C2 1.515(4) . ? C2 C7 1.383(4) . ? C2 C3 1.386(4) . ? C3 C4 1.400(4) . ? C3 H3 0.9300 . ? C4 C5 1.383(4) . ? C4 C8 1.511(4) . ? C5 C6 1.388(5) . ? C5 H5 0.9300 . ? C6 C7 1.387(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C9 C10 1.389(4) . ? C9 H9 0.9300 . ? C10 C11 1.375(5) . ? C10 C14 1.478(4) . ? C11 C12 1.382(5) . ? C11 H11 0.9300 . ? C12 C13 1.383(5) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.398(4) . ? C15 H15 0.9300 . ? C16 C17 1.387(5) . ? C17 C18 1.384(5) . ? C17 H17 0.9300 . ? C18 C19 1.381(5) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 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 O4 Mn1 O3 93.54(9) 2_665 1_545 ? O4 Mn1 O1W 177.82(8) 2_665 . ? O3 Mn1 O1W 87.96(9) 1_545 . ? O4 Mn1 N1 91.64(10) 2_665 . ? O3 Mn1 N1 92.31(9) 1_545 . ? O1W Mn1 N1 89.88(10) . . ? O4 Mn1 O1 91.34(8) 2_665 . ? O3 Mn1 O1 175.08(8) 1_545 . ? O1W Mn1 O1 87.18(9) . . ? N1 Mn1 O1 86.90(9) . . ? O4 Mn1 N3 88.45(10) 2_665 1_665 ? O3 Mn1 N3 99.24(9) 1_545 1_665 ? O1W Mn1 N3 89.74(10) . 1_665 ? N1 Mn1 N3 168.42(9) . 1_665 ? O1 Mn1 N3 81.52(9) . 1_665 ? C1 O1 Mn1 126.4(2) . . ? Mn1 O1W H1W1 101(3) . . ? Mn1 O1W H1W2 127(3) . . ? H1W1 O1W H1W2 108.9(16) . . ? C8 O3 Mn1 152.1(2) . 1_565 ? C8 O4 Mn1 137.38(19) . 2_665 ? C20 O5 H5O 110(4) . . ? C9 N1 C13 117.4(3) . . ? C9 N1 Mn1 119.1(2) . . ? C13 N1 Mn1 123.3(2) . . ? C16 N2 C14 120.4(3) . . ? C16 N2 H2N 120(3) . . ? C14 N2 H2N 115(3) . . ? C15 N3 C19 117.4(3) . . ? C15 N3 Mn1 115.9(2) . 1_445 ? C19 N3 Mn1 126.3(2) . 1_445 ? O1 C1 O2 126.4(3) . . ? O1 C1 C2 118.9(3) . . ? O2 C1 C2 114.8(3) . . ? C7 C2 C3 119.5(2) . . ? C7 C2 C1 119.2(3) . . ? C3 C2 C1 121.1(3) . . ? C2 C3 C4 120.8(3) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 118.8(3) . . ? C5 C4 C8 121.5(2) . . ? C3 C4 C8 119.7(3) . . ? C4 C5 C6 120.6(3) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C7 C6 C5 119.8(3) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C2 C7 C6 120.3(3) . . ? C2 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? O4 C8 O3 125.3(3) . . ? O4 C8 C4 116.7(2) . . ? O3 C8 C4 118.0(3) . . ? N1 C9 C10 124.0(3) . . ? N1 C9 H9 118.0 . . ? C10 C9 H9 118.0 . . ? C11 C10 C9 117.5(3) . . ? C11 C10 C14 124.0(3) . . ? C9 C10 C14 118.5(3) . . ? C10 C11 C12 119.7(3) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C11 C12 C13 118.8(3) . . ? C11 C12 H12 120.6 . . ? C13 C12 H12 120.6 . . ? N1 C13 C12 122.5(3) . . ? N1 C13 H13 118.7 . . ? C12 C13 H13 118.7 . . ? N2 C14 C10 116.9(3) . . ? N2 C14 H14A 108.1 . . ? C10 C14 H14A 108.1 . . ? N2 C14 H14B 108.1 . . ? C10 C14 H14B 108.1 . . ? H14A C14 H14B 107.3 . . ? N3 C15 C16 124.4(3) . . ? N3 C15 H15 117.8 . . ? C16 C15 H15 117.8 . . ? C17 C16 C15 117.1(3) . . ? C17 C16 N2 124.5(3) . . ? C15 C16 N2 118.4(3) . . ? C18 C17 C16 118.8(3) . . ? C18 C17 H17 120.6 . . ? C16 C17 H17 120.6 . . ? C19 C18 C17 119.9(3) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? N3 C19 C18 122.4(3) . . ? N3 C19 H19 118.8 . . ? C18 C19 H19 118.8 . . ? O5 C20 H20A 109.5 . . ? O5 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O5 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 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 O4 Mn1 O1 C1 -159.1(3) 2_665 . . . ? O1W Mn1 O1 C1 19.3(3) . . . . ? N1 Mn1 O1 C1 109.3(3) . . . . ? N3 Mn1 O1 C1 -70.9(3) 1_665 . . . ? O4 Mn1 N1 C9 51.8(2) 2_665 . . . ? O3 Mn1 N1 C9 -41.9(2) 1_545 . . . ? O1W Mn1 N1 C9 -129.8(2) . . . . ? O1 Mn1 N1 C9 143.0(2) . . . . ? N3 Mn1 N1 C9 142.1(4) 1_665 . . . ? O4 Mn1 N1 C13 -133.9(3) 2_665 . . . ? O3 Mn1 N1 C13 132.5(3) 1_545 . . . ? O1W Mn1 N1 C13 44.6(3) . . . . ? O1 Mn1 N1 C13 -42.6(3) . . . . ? N3 Mn1 N1 C13 -43.6(6) 1_665 . . . ? Mn1 O1 C1 O2 -18.0(5) . . . . ? Mn1 O1 C1 C2 162.0(2) . . . . ? O1 C1 C2 C7 141.4(3) . . . . ? O2 C1 C2 C7 -38.6(4) . . . . ? O1 C1 C2 C3 -43.3(4) . . . . ? O2 C1 C2 C3 136.7(3) . . . . ? C7 C2 C3 C4 2.0(4) . . . . ? C1 C2 C3 C4 -173.3(3) . . . . ? C2 C3 C4 C5 -2.1(4) . . . . ? C2 C3 C4 C8 177.2(3) . . . . ? C3 C4 C5 C6 -0.4(5) . . . . ? C8 C4 C5 C6 -179.6(3) . . . . ? C4 C5 C6 C7 2.9(6) . . . . ? C3 C2 C7 C6 0.6(5) . . . . ? C1 C2 C7 C6 175.9(3) . . . . ? C5 C6 C7 C2 -3.0(6) . . . . ? Mn1 O4 C8 O3 -43.5(5) 2_665 . . . ? Mn1 O4 C8 C4 137.9(2) 2_665 . . . ? Mn1 O3 C8 O4 107.5(5) 1_565 . . . ? Mn1 O3 C8 C4 -73.9(5) 1_565 . . . ? C5 C4 C8 O4 -166.9(3) . . . . ? C3 C4 C8 O4 13.8(4) . . . . ? C5 C4 C8 O3 14.4(4) . . . . ? C3 C4 C8 O3 -164.8(3) . . . . ? C13 N1 C9 C10 -0.8(5) . . . . ? Mn1 N1 C9 C10 173.9(2) . . . . ? N1 C9 C10 C11 1.0(5) . . . . ? N1 C9 C10 C14 -179.7(3) . . . . ? C9 C10 C11 C12 0.0(5) . . . . ? C14 C10 C11 C12 -179.2(3) . . . . ? C10 C11 C12 C13 -1.2(6) . . . . ? C9 N1 C13 C12 -0.5(5) . . . . ? Mn1 N1 C13 C12 -174.9(3) . . . . ? C11 C12 C13 N1 1.5(6) . . . . ? C16 N2 C14 C10 -81.4(4) . . . . ? C11 C10 C14 N2 -14.8(5) . . . . ? C9 C10 C14 N2 166.0(3) . . . . ? C19 N3 C15 C16 -0.1(5) . . . . ? Mn1 N3 C15 C16 172.8(2) 1_445 . . . ? N3 C15 C16 C17 0.2(5) . . . . ? N3 C15 C16 N2 -179.6(3) . . . . ? C14 N2 C16 C17 11.9(5) . . . . ? C14 N2 C16 C15 -168.4(3) . . . . ? C15 C16 C17 C18 -0.7(5) . . . . ? N2 C16 C17 C18 179.0(3) . . . . ? C16 C17 C18 C19 1.2(6) . . . . ? C15 N3 C19 C18 0.5(5) . . . . ? Mn1 N3 C19 C18 -171.5(3) 1_445 . . . ? C17 C18 C19 N3 -1.1(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 N2 H2N O1 0.86(4) 2.340(16) 3.172(4) 162(3) 2 O1W H1W1 O2 0.85(3) 1.766(13) 2.599(3) 166(4) . O1W H1W2 O5 0.86(4) 1.941(12) 2.790(4) 173(4) 1_655 O5 H5O O2 0.86(5) 2.052(12) 2.906(5) 176(6) 2_666 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.711 _refine_diff_density_min -0.575 _refine_diff_density_rms 0.091 #===END data_complex6 #TrackingRef '- cif.cif' _database_code_depnum_ccdc_archive 'CCDC 870301' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H17 Co N3 O5, H2 O' _chemical_formula_sum 'C19 H19 Co N3 O6' _chemical_formula_weight 444.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 orthorhombic _symmetry_space_group_name_H-M 'P nc2 ' _symmetry_space_group_name_Hall 'P 2 -2bc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y+1/2, z+1/2' '-x, y+1/2, z+1/2' _cell_length_a 9.5360(12) _cell_length_b 17.804(2) _cell_length_c 11.4530(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1944.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 13279 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 27.45 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.518 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 916 _exptl_absorpt_coefficient_mu 0.924 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8155 _exptl_absorpt_correction_T_max 0.8815 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 18023 _diffrn_reflns_av_R_equivalents 0.0481 _diffrn_reflns_av_sigmaI/netI 0.0482 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4451 _reflns_number_gt 3819 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0884P)^2^+0.5178P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.48(3) _refine_ls_number_reflns 4451 _refine_ls_number_parameters 271 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1455 _refine_ls_wR_factor_gt 0.1404 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.062 _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 0.25691(4) 0.77883(2) 0.49994(9) 0.03610(15) Uani 1 1 d . . . O1 O 0.3129(3) 0.82524(14) 0.3280(2) 0.0515(6) Uani 1 1 d . . . O2 O 0.3539(3) 0.88785(12) 0.4870(2) 0.0488(6) Uani 1 1 d . . . O3 O 0.1739(3) 0.67609(13) 0.4924(4) 0.0657(7) Uani 1 1 d . . . O4 O 0.1396(5) 0.6190(2) 0.3221(3) 0.1009(16) Uani 1 1 d . . . O1W O 0.2530(3) 0.78217(15) 0.6767(3) 0.0544(9) Uani 1 1 d D . . H1W1 H 0.202(5) 0.807(2) 0.723(4) 0.082 Uiso 1 1 d D . . H1W2 H 0.237(5) 0.7356(8) 0.688(6) 0.082 Uiso 1 1 d D . . O2W O 0.3574(9) 0.9799(4) 0.7058(8) 0.196(3) Uani 1 1 d U . . H2W1 H 0.2974 0.9561 0.7464 0.294 Uiso 1 1 d R . . H2W2 H 0.3648 0.9579 0.6402 0.294 Uiso 1 1 d R . . N1 N 0.4618(3) 0.72622(15) 0.5010(3) 0.0486(6) Uani 1 1 d . . . N2 N 0.7522(5) 0.6740(5) 0.7838(6) 0.0869(14) Uani 1 1 d . . . H2N H 0.6703 0.6539 0.7830 0.145 Uiso 1 1 calc R . . N3 N 1.0545(3) 0.67153(16) 0.9808(3) 0.0500(8) Uani 1 1 d . . . C1 C 0.3618(4) 0.88253(18) 0.3784(3) 0.0409(7) Uani 1 1 d . . . C2 C 0.5000 1.0000 0.3693(4) 0.0358(9) Uani 1 2 d S . . H2A H 0.5000 1.0000 0.4505 0.043 Uiso 1 2 calc SR . . C3 C 0.4327(4) 0.94269(18) 0.3097(3) 0.0396(7) Uani 1 1 d . . . C4 C 0.4327(4) 0.9432(2) 0.1882(3) 0.0451(8) Uani 1 1 d . . . H4 H 0.3872 0.9053 0.1472 0.054 Uiso 1 1 calc R . . C5 C 0.5000 1.0000 0.1286(5) 0.0556(14) Uani 1 2 d S . . H5 H 0.5000 1.0000 0.0474 0.067 Uiso 1 2 calc SR . . C6 C 0.1303(4) 0.6226(2) 0.4281(4) 0.0573(12) Uani 1 1 d . . . C7 C 0.0000 0.5000 0.4330(5) 0.0453(11) Uani 1 2 d S . . H7 H 0.0000 0.5000 0.3518 0.054 Uiso 1 2 calc SR . . C8 C 0.0636(3) 0.55864(15) 0.4946(4) 0.0411(7) Uani 1 1 d . . . C9 C 0.0643(4) 0.5580(2) 0.6154(4) 0.0505(9) Uani 1 1 d . . . H9 H 0.1081 0.5966 0.6562 0.061 Uiso 1 1 calc R . . C10 C 0.0000 0.5000 0.6757(5) 0.0591(15) Uani 1 2 d S . . H10 H 0.0000 0.5000 0.7569 0.071 Uiso 1 2 calc SR . . C11 C 0.5602(4) 0.7390(3) 0.5842(4) 0.0624(11) Uani 1 1 d . . . H11A H 0.5395 0.7737 0.6424 0.075 Uiso 1 1 calc R . . C12 C 0.6882(5) 0.7042(4) 0.5877(5) 0.0769(14) Uani 1 1 d . . . C13 C 0.7161(5) 0.6519(4) 0.5026(9) 0.096(2) Uani 1 1 d . . . H13 H 0.8002 0.6255 0.5036 0.116 Uiso 1 1 calc R . . C14 C 0.6189(6) 0.6386(3) 0.4155(6) 0.0864(16) Uani 1 1 d . . . H14 H 0.6384 0.6046 0.3560 0.104 Uiso 1 1 calc R . . C15 C 0.4940(5) 0.6759(3) 0.4178(4) 0.0601(10) Uani 1 1 d . . . H15 H 0.4286 0.6661 0.3595 0.072 Uiso 1 1 calc R . . C16 C 0.7882(7) 0.7178(5) 0.6907(8) 0.0869(12) Uani 1 1 d . . . H16A H 0.8835 0.7064 0.6670 0.149 Uiso 1 1 calc R . . H16B H 0.7845 0.7703 0.7132 0.149 Uiso 1 1 calc R . . C17 C 0.9704(4) 0.6919(3) 0.8930(4) 0.0601(10) Uani 1 1 d . . . H17 H 1.0008 0.7281 0.8403 0.072 Uiso 1 1 calc R . . C18 C 0.8359(5) 0.6595(4) 0.8784(5) 0.0819(16) Uani 1 1 d . . . C19 C 0.7938(7) 0.6082(5) 0.9601(6) 0.103(2) Uani 1 1 d . . . H19 H 0.7044 0.5876 0.9553 0.124 Uiso 1 1 calc R . . C20 C 0.8797(6) 0.5871(4) 1.0472(7) 0.102(2) Uani 1 1 d . . . H20 H 0.8520 0.5512 1.1015 0.123 Uiso 1 1 calc R . . C21 C 1.0089(6) 0.6201(3) 1.0537(5) 0.0754(13) Uani 1 1 d . . . H21A H 1.0684 0.6052 1.1136 0.091 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 0.0417(2) 0.0360(2) 0.0306(2) 0.0017(2) -0.0056(2) -0.00461(15) O1 0.0707(18) 0.0439(12) 0.0400(14) -0.0026(11) -0.0046(12) -0.0200(14) O2 0.0650(14) 0.0457(11) 0.0357(14) -0.0020(11) -0.0010(13) -0.0167(11) O3 0.0742(17) 0.0420(12) 0.081(2) -0.0044(16) -0.002(2) -0.0169(13) O4 0.171(4) 0.082(2) 0.050(2) 0.0143(18) -0.003(2) -0.075(3) O1W 0.084(3) 0.0502(19) 0.0288(15) 0.0029(11) -0.0038(12) 0.0130(15) O2W 0.228(6) 0.187(6) 0.173(6) -0.007(5) 0.012(6) -0.045(6) N1 0.0472(13) 0.0556(15) 0.0430(16) 0.0061(16) -0.0037(18) 0.0025(12) N2 0.064(3) 0.135(5) 0.068(3) -0.005(3) -0.008(2) -0.001(3) N3 0.0472(14) 0.0514(15) 0.051(2) -0.0038(14) -0.0085(15) -0.0010(13) C1 0.0443(17) 0.0362(16) 0.0421(19) 0.0033(13) -0.0062(14) -0.0094(14) C2 0.041(2) 0.036(2) 0.030(2) 0.000 0.000 0.0005(19) C3 0.0413(16) 0.0377(16) 0.0396(19) 0.0011(13) 0.0024(13) -0.0021(14) C4 0.059(2) 0.0431(18) 0.0338(19) -0.0064(14) -0.0073(15) -0.0063(17) C5 0.081(4) 0.057(3) 0.028(2) 0.000 0.000 -0.016(3) C6 0.080(3) 0.058(2) 0.028(3) 0.000 0.000 -0.014(2) C7 0.053(3) 0.045(3) 0.038(3) 0.000 0.000 -0.010(2) C8 0.0425(14) 0.0350(14) 0.0458(18) -0.0001(18) -0.0045(18) -0.0055(12) C9 0.061(2) 0.0477(19) 0.043(2) -0.0058(16) -0.0017(16) -0.0080(18) C10 0.084(4) 0.062(3) 0.032(3) 0.000 0.000 -0.009(3) C11 0.052(2) 0.090(3) 0.045(2) 0.007(2) -0.0073(18) 0.005(2) C12 0.049(2) 0.116(4) 0.065(3) 0.024(3) -0.008(2) 0.008(3) C13 0.062(2) 0.132(5) 0.095(4) 0.030(5) 0.007(4) 0.041(3) C14 0.090(4) 0.089(3) 0.080(4) -0.001(3) 0.016(3) 0.034(3) C15 0.065(2) 0.068(3) 0.047(2) 0.0039(19) -0.004(2) 0.018(2) C16 0.064(2) 0.134(5) 0.068(4) -0.008(3) -0.011(2) -0.002(3) C17 0.053(2) 0.075(3) 0.052(2) -0.003(2) -0.0133(18) -0.002(2) C18 0.058(3) 0.126(5) 0.061(3) -0.012(3) -0.016(2) -0.009(3) C19 0.077(3) 0.140(6) 0.093(5) 0.014(4) -0.019(3) -0.056(4) C20 0.092(4) 0.109(5) 0.105(5) 0.020(4) -0.013(4) -0.047(4) C21 0.074(3) 0.074(3) 0.078(3) 0.008(3) -0.015(3) -0.025(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O3 1.995(2) . ? Co1 O1W 2.026(3) . ? Co1 N3 2.134(3) 3_464 ? Co1 O2 2.155(2) . ? Co1 N1 2.167(3) . ? Co1 O1 2.201(3) . ? O1 C1 1.261(4) . ? O2 C1 1.250(5) . ? O3 C6 1.273(5) . ? O4 C6 1.219(6) . ? O1W H1W1 0.85(4) . ? O1W H1W2 0.85(4) . ? O2W H2W1 0.8500 . ? O2W H2W2 0.8500 . ? N1 C15 1.343(6) . ? N1 C11 1.356(5) . ? N2 C16 1.365(10) . ? N2 C18 1.370(8) . ? N2 H2N 0.8600 . ? N3 C21 1.312(6) . ? N3 C17 1.337(5) . ? N3 Co1 2.134(3) 3_665 ? C1 C3 1.491(5) . ? C2 C3 1.385(4) . ? C2 C3 1.385(4) 2_675 ? C2 H2A 0.9300 . ? C3 C4 1.391(5) . ? C4 C5 1.379(5) . ? C4 H4 0.9300 . ? C5 C4 1.379(5) 2_675 ? C5 H5 0.9300 . ? C6 C8 1.511(5) . ? C7 C8 1.398(4) . ? C7 C8 1.398(4) 2_565 ? C7 H7 0.9300 . ? C8 C9 1.383(6) . ? C9 C10 1.386(5) . ? C9 H9 0.9300 . ? C10 C9 1.386(5) 2_565 ? C10 H10 0.9300 . ? C11 C12 1.370(7) . ? C11 H11A 0.9300 . ? C12 C13 1.374(11) . ? C12 C16 1.536(10) . ? C13 C14 1.382(11) . ? C13 H13 0.9300 . ? C14 C15 1.364(7) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.416(6) . ? C17 H17 0.9300 . ? C18 C19 1.367(8) . ? C19 C20 1.345(9) . ? C19 H19 0.9300 . ? C20 C21 1.367(7) . ? C20 H20 0.9300 . ? C21 H21A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Co1 O1W 93.60(15) . . ? O3 Co1 N3 90.94(12) . 3_464 ? O1W Co1 N3 94.24(13) . 3_464 ? O3 Co1 O2 173.26(16) . . ? O1W Co1 O2 92.86(12) . . ? N3 Co1 O2 90.47(11) 3_464 . ? O3 Co1 N1 87.81(12) . . ? O1W Co1 N1 91.34(14) . . ? N3 Co1 N1 174.35(17) 3_464 . ? O2 Co1 N1 90.16(10) . . ? O3 Co1 O1 113.69(15) . . ? O1W Co1 O1 152.55(11) . . ? N3 Co1 O1 88.40(13) 3_464 . ? O2 Co1 O1 59.77(9) . . ? N1 Co1 O1 87.06(13) . . ? C1 O1 Co1 89.1(2) . . ? C1 O2 Co1 91.49(19) . . ? C6 O3 Co1 147.1(4) . . ? Co1 O1W H1W1 131(4) . . ? Co1 O1W H1W2 97(4) . . ? H1W1 O1W H1W2 108(5) . . ? H2W1 O2W H2W2 108.1 . . ? C15 N1 C11 116.9(4) . . ? C15 N1 Co1 119.3(3) . . ? C11 N1 Co1 123.7(3) . . ? C16 N2 C18 125.4(5) . . ? C16 N2 H2N 117.3 . . ? C18 N2 H2N 117.3 . . ? C21 N3 C17 117.9(4) . . ? C21 N3 Co1 121.5(3) . 3_665 ? C17 N3 Co1 120.5(3) . 3_665 ? O2 C1 O1 119.6(3) . . ? O2 C1 C3 119.9(3) . . ? O1 C1 C3 120.5(3) . . ? C3 C2 C3 120.9(4) . 2_675 ? C3 C2 H2A 119.5 . . ? C3 C2 H2A 119.5 2_675 . ? C2 C3 C4 119.2(3) . . ? C2 C3 C1 118.6(3) . . ? C4 C3 C1 122.2(3) . . ? C5 C4 C3 120.1(3) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C4 120.6(5) 2_675 . ? C4 C5 H5 119.7 2_675 . ? C4 C5 H5 119.7 . . ? O4 C6 O3 126.3(4) . . ? O4 C6 C8 119.5(3) . . ? O3 C6 C8 114.2(4) . . ? C8 C7 C8 119.4(5) . 2_565 ? C8 C7 H7 120.3 . . ? C8 C7 H7 120.3 2_565 . ? C9 C8 C7 120.0(4) . . ? C9 C8 C6 120.6(3) . . ? C7 C8 C6 119.4(4) . . ? C8 C9 C10 120.2(4) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C9 C10 C9 120.2(5) 2_565 . ? C9 C10 H10 119.9 2_565 . ? C9 C10 H10 119.9 . . ? N1 C11 C12 124.1(5) . . ? N1 C11 H11A 117.9 . . ? C12 C11 H11A 117.9 . . ? C11 C12 C13 117.3(5) . . ? C11 C12 C16 120.3(7) . . ? C13 C12 C16 122.1(6) . . ? C12 C13 C14 119.9(5) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C15 C14 C13 119.2(6) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? N1 C15 C14 122.5(5) . . ? N1 C15 H15 118.7 . . ? C14 C15 H15 118.7 . . ? N2 C16 C12 110.7(6) . . ? N2 C16 H16A 109.5 . . ? C12 C16 H16A 109.5 . . ? N2 C16 H16B 109.5 . . ? C12 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? N3 C17 C18 121.5(5) . . ? N3 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C19 C18 N2 119.7(5) . . ? C19 C18 C17 117.2(5) . . ? N2 C18 C17 123.0(6) . . ? C20 C19 C18 121.1(5) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C19 C20 C21 117.9(6) . . ? C19 C20 H20 121.0 . . ? C21 C20 H20 121.0 . . ? N3 C21 C20 124.4(5) . . ? N3 C21 H21A 117.8 . . ? C20 C21 H21A 117.8 . . ? 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 O3 Co1 O1 C1 -177.0(2) . . . . ? O1W Co1 O1 C1 -3.4(4) . . . . ? N3 Co1 O1 C1 92.7(2) 3_464 . . . ? O2 Co1 O1 C1 1.2(2) . . . . ? N1 Co1 O1 C1 -90.7(2) . . . . ? O1W Co1 O2 C1 176.7(2) . . . . ? N3 Co1 O2 C1 -89.1(2) 3_464 . . . ? N1 Co1 O2 C1 85.3(2) . . . . ? O1 Co1 O2 C1 -1.2(2) . . . . ? O1W Co1 O3 C6 178.1(5) . . . . ? N3 Co1 O3 C6 83.8(5) 3_464 . . . ? N1 Co1 O3 C6 -90.7(5) . . . . ? O1 Co1 O3 C6 -4.9(6) . . . . ? O3 Co1 N1 C15 52.3(3) . . . . ? O1W Co1 N1 C15 145.9(3) . . . . ? O2 Co1 N1 C15 -121.3(3) . . . . ? O1 Co1 N1 C15 -61.6(3) . . . . ? O3 Co1 N1 C11 -125.3(3) . . . . ? O1W Co1 N1 C11 -31.7(3) . . . . ? O2 Co1 N1 C11 61.1(3) . . . . ? O1 Co1 N1 C11 120.8(3) . . . . ? Co1 O2 C1 O1 2.1(4) . . . . ? Co1 O2 C1 C3 -176.1(3) . . . . ? Co1 O1 C1 O2 -2.0(3) . . . . ? Co1 O1 C1 C3 176.1(3) . . . . ? C3 C2 C3 C4 -0.3(2) 2_675 . . . ? C3 C2 C3 C1 -179.9(3) 2_675 . . . ? O2 C1 C3 C2 6.0(5) . . . . ? O1 C1 C3 C2 -172.2(3) . . . . ? O2 C1 C3 C4 -173.7(3) . . . . ? O1 C1 C3 C4 8.2(5) . . . . ? C2 C3 C4 C5 0.5(5) . . . . ? C1 C3 C4 C5 -179.8(3) . . . . ? C3 C4 C5 C4 -0.3(2) . . . 2_675 ? Co1 O3 C6 O4 6.7(9) . . . . ? Co1 O3 C6 C8 -174.4(3) . . . . ? C8 C7 C8 C9 0.6(3) 2_565 . . . ? C8 C7 C8 C6 -179.0(3) 2_565 . . . ? O4 C6 C8 C9 173.5(5) . . . . ? O3 C6 C8 C9 -5.5(5) . . . . ? O4 C6 C8 C7 -6.9(6) . . . . ? O3 C6 C8 C7 174.0(3) . . . . ? C7 C8 C9 C10 -1.1(5) . . . . ? C6 C8 C9 C10 178.5(3) . . . . ? C8 C9 C10 C9 0.6(3) . . . 2_565 ? C15 N1 C11 C12 0.1(7) . . . . ? Co1 N1 C11 C12 177.7(4) . . . . ? N1 C11 C12 C13 -1.4(8) . . . . ? N1 C11 C12 C16 -175.2(5) . . . . ? C11 C12 C13 C14 2.5(10) . . . . ? C16 C12 C13 C14 176.2(6) . . . . ? C12 C13 C14 C15 -2.3(10) . . . . ? C11 N1 C15 C14 0.2(7) . . . . ? Co1 N1 C15 C14 -177.6(4) . . . . ? C13 C14 C15 N1 0.9(9) . . . . ? C18 N2 C16 C12 164.3(8) . . . . ? C11 C12 C16 N2 81.5(9) . . . . ? C13 C12 C16 N2 -92.0(10) . . . . ? C21 N3 C17 C18 0.1(7) . . . . ? Co1 N3 C17 C18 179.7(4) 3_665 . . . ? C16 N2 C18 C19 -173.0(9) . . . . ? C16 N2 C18 C17 3.0(14) . . . . ? N3 C17 C18 C19 2.1(9) . . . . ? N3 C17 C18 N2 -174.0(6) . . . . ? N2 C18 C19 C20 173.1(8) . . . . ? C17 C18 C19 C20 -3.1(11) . . . . ? C18 C19 C20 C21 1.9(12) . . . . ? C17 N3 C21 C20 -1.5(9) . . . . ? Co1 N3 C21 C20 178.9(5) 3_665 . . . ? C19 C20 C21 N3 0.5(11) . . . . ? 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 H1W2 O1 0.85(4) 2.07(6) 2.643(4) 124(5) 3_565 O1W H1W1 O4 0.85(4) 1.83(4) 2.653(4) 162(5) 3_565 O2W H2W2 O2 0.85 2.16 2.994(9) 169.1 . O2W H2W1 O4 0.85 2.19 3.031(9) 169.1 3_565 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.086 _refine_diff_density_min -0.760 _refine_diff_density_rms 0.085 #===END data_complex7 #TrackingRef '- cif.cif' _database_code_depnum_ccdc_archive 'CCDC 870302' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H17 N3 Ni O5, H2 O' _chemical_formula_sum 'C19 H19 N3 Ni O6' _chemical_formula_weight 444.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P nc2 ' _symmetry_space_group_name_Hall 'P 2 -2bc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y+1/2, z+1/2' '-x, y+1/2, z+1/2' _cell_length_a 9.4225(18) _cell_length_b 17.784(4) _cell_length_c 11.416(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1912.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 8319 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 27.64 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 1.057 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8086 _exptl_absorpt_correction_T_max 0.8661 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 18025 _diffrn_reflns_av_R_equivalents 0.0481 _diffrn_reflns_av_sigmaI/netI 0.0482 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.77 _reflns_number_total 4452 _reflns_number_gt 3820 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0988P)^2^+0.5161P] 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 0.48(3) _refine_ls_number_reflns 4452 _refine_ls_number_parameters 265 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0633 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1589 _refine_ls_wR_factor_gt 0.1535 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.084 _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 0.25684(4) 0.77883(2) 0.49995(10) 0.03664(16) Uani 1 1 d . . . O1 O 0.3126(3) 0.82534(15) 0.3279(3) 0.0487(7) Uani 1 1 d . . . O2 O 0.3539(3) 0.88785(13) 0.4871(2) 0.0455(6) Uani 1 1 d . . . O3 O 0.1736(3) 0.67625(14) 0.4929(4) 0.0624(8) Uani 1 1 d . . . O4 O 0.1397(6) 0.6190(2) 0.3223(3) 0.0966(17) Uani 1 1 d . . . O1W O 0.2521(3) 0.78220(16) 0.6767(3) 0.0522(10) Uani 1 1 d . . . H1W1 H 0.2738 0.7455 0.7209 0.078 Uiso 1 1 d R . . H1W2 H 0.2148 0.8163 0.7188 0.078 Uiso 1 1 d R . . O2W O 0.3565(10) 0.9796(4) 0.7052(8) 0.180(3) Uani 1 1 d U . . H2W1 H 0.3640 0.9575 0.6394 0.271 Uiso 1 1 d R . . H2W2 H 0.2963 0.9556 0.7462 0.271 Uiso 1 1 d R . . N1 N 0.4617(3) 0.72622(16) 0.5012(4) 0.0453(7) Uani 1 1 d . . . N2 N 0.7525(5) 0.6726(6) 0.7836(7) 0.0913(16) Uani 1 1 d . . . H2N H 0.6709 0.6510 0.7817 0.139 Uiso 1 1 calc R . . N3 N 1.0546(3) 0.67149(17) 0.9809(3) 0.0469(8) Uani 1 1 d . . . C1 C 0.3618(4) 0.88264(19) 0.3785(3) 0.0388(8) Uani 1 1 d . . . C2 C 0.5000 1.0000 0.3694(4) 0.0337(10) Uani 1 2 d S . . H2 H 0.5000 1.0000 0.4509 0.040 Uiso 1 2 calc SR . . C3 C 0.4327(4) 0.94274(19) 0.3098(3) 0.0371(7) Uani 1 1 d . . . C4 C 0.4323(4) 0.9433(2) 0.1882(3) 0.0429(8) Uani 1 1 d . . . H4 H 0.3862 0.9052 0.1472 0.052 Uiso 1 1 calc R . . C5 C 0.5000 1.0000 0.1285(5) 0.0531(15) Uani 1 2 d S . . H5 H 0.5000 1.0000 0.0470 0.064 Uiso 1 2 calc SR . . C6 C 0.1299(5) 0.6227(2) 0.4279(4) 0.0523(15) Uani 1 1 d . . . C7 C 0.0000 0.5000 0.4330(5) 0.0427(11) Uani 1 2 d S . . H7 H 0.0000 0.5000 0.3515 0.051 Uiso 1 2 calc SR . . C8 C 0.0636(3) 0.55866(16) 0.4947(4) 0.0389(7) Uani 1 1 d . . . C9 C 0.0645(5) 0.5581(2) 0.6151(4) 0.0479(9) Uani 1 1 d . . . H9 H 0.1085 0.5968 0.6560 0.057 Uiso 1 1 calc R . . C10 C 0.0000 0.5000 0.6759(6) 0.0568(15) Uani 1 2 d S . . H10 H 0.0000 0.5000 0.7573 0.068 Uiso 1 2 calc SR . . C11 C 0.5604(5) 0.7392(3) 0.5840(5) 0.0597(11) Uani 1 1 d . . . H11 H 0.5402 0.7743 0.6421 0.072 Uiso 1 1 calc R . . C12 C 0.6882(5) 0.7037(4) 0.5873(5) 0.0733(15) Uani 1 1 d . . . C13 C 0.7158(6) 0.6515(4) 0.5027(9) 0.092(2) Uani 1 1 d . . . H13 H 0.8003 0.6246 0.5043 0.111 Uiso 1 1 calc R . . C14 C 0.6185(7) 0.6388(4) 0.4153(6) 0.0823(17) Uani 1 1 d . . . H14 H 0.6384 0.6050 0.3552 0.099 Uiso 1 1 calc R . . C15 C 0.4942(5) 0.6758(3) 0.4178(4) 0.0576(11) Uani 1 1 d . . . H15 H 0.4279 0.6661 0.3593 0.069 Uiso 1 1 calc R . . C16 C 0.7876(8) 0.7173(6) 0.6906(8) 0.0853(16) Uani 1 1 d . . . H16A H 0.8845 0.7068 0.6670 0.148 Uiso 1 1 calc R . . H16B H 0.7823 0.7696 0.7139 0.148 Uiso 1 1 calc R . . C17 C 0.9703(5) 0.6917(3) 0.8933(4) 0.0577(11) Uani 1 1 d . . . H17 H 1.0013 0.7280 0.8405 0.069 Uiso 1 1 calc R . . C18 C 0.8353(6) 0.6596(4) 0.8785(5) 0.0789(17) Uani 1 1 d . . . C19 C 0.7934(8) 0.6087(5) 0.9599(6) 0.099(2) Uani 1 1 d . . . H19 H 0.7025 0.5885 0.9552 0.118 Uiso 1 1 calc R . . C20 C 0.8801(7) 0.5867(4) 1.0476(7) 0.097(2) Uani 1 1 d . . . H20 H 0.8526 0.5502 1.1014 0.116 Uiso 1 1 calc R . . C21 C 1.0087(6) 0.6201(3) 1.0534(5) 0.0720(14) Uani 1 1 d . . . H21 H 1.0692 0.6053 1.1135 0.086 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 0.0414(2) 0.0371(2) 0.0314(2) 0.0017(2) -0.0056(2) -0.00440(16) O1 0.0663(19) 0.0418(13) 0.0380(14) -0.0030(12) -0.0042(13) -0.0195(14) O2 0.0599(14) 0.0434(12) 0.0331(14) -0.0020(11) -0.0001(13) -0.0160(11) O3 0.0695(18) 0.0400(12) 0.078(2) -0.0046(17) 0.001(2) -0.0169(13) O4 0.161(5) 0.080(2) 0.049(2) 0.0146(19) -0.003(2) -0.075(3) O1W 0.081(3) 0.050(2) 0.0258(16) 0.0038(11) -0.0040(12) 0.0167(14) O2W 0.208(6) 0.179(6) 0.154(6) -0.010(5) 0.011(6) -0.033(6) N1 0.0426(14) 0.0529(16) 0.0403(16) 0.0059(17) -0.0041(18) 0.0027(12) N2 0.069(2) 0.138(5) 0.069(3) -0.001(3) -0.002(2) 0.000(3) N3 0.0438(14) 0.0488(16) 0.048(2) -0.0042(15) -0.0084(15) -0.0007(13) C1 0.0412(18) 0.0339(16) 0.041(2) 0.0033(14) -0.0063(15) -0.0099(15) C2 0.038(2) 0.035(2) 0.028(2) 0.000 0.000 0.000(2) C3 0.0389(17) 0.0357(16) 0.0367(19) 0.0012(13) 0.0025(14) -0.0019(14) C4 0.056(2) 0.0415(19) 0.0310(19) -0.0054(15) -0.0078(16) -0.0057(17) C5 0.078(4) 0.056(3) 0.026(2) 0.000 0.000 -0.018(3) C6 0.074(4) 0.052(4) 0.028(2) 0.000 0.000 -0.013(3) C7 0.050(3) 0.043(3) 0.035(3) 0.000 0.000 -0.010(2) C8 0.0398(15) 0.0329(15) 0.0441(19) -0.0005(18) -0.0039(19) -0.0060(13) C9 0.057(2) 0.047(2) 0.040(2) -0.0050(16) -0.0018(17) -0.0083(19) C10 0.079(4) 0.060(4) 0.032(3) 0.000 0.000 -0.010(3) C11 0.048(2) 0.087(3) 0.044(2) 0.006(2) -0.0078(19) 0.004(2) C12 0.045(2) 0.113(4) 0.063(3) 0.022(3) -0.008(2) 0.006(3) C13 0.057(2) 0.126(5) 0.093(4) 0.030(5) 0.008(5) 0.039(3) C14 0.084(4) 0.087(4) 0.076(4) -0.003(3) 0.015(3) 0.034(4) C15 0.061(2) 0.067(3) 0.045(2) 0.003(2) -0.004(2) 0.017(2) C16 0.062(2) 0.133(5) 0.064(3) -0.008(3) -0.007(2) -0.001(3) C17 0.050(2) 0.072(3) 0.051(3) -0.002(2) -0.0127(19) -0.003(2) C18 0.054(3) 0.126(5) 0.057(3) -0.013(3) -0.015(2) -0.007(3) C19 0.072(3) 0.136(6) 0.088(5) 0.012(4) -0.018(3) -0.054(4) C20 0.088(4) 0.104(5) 0.098(5) 0.020(4) -0.012(4) -0.045(4) C21 0.068(3) 0.072(3) 0.075(3) 0.007(3) -0.015(3) -0.022(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O3 1.987(3) . ? Ni1 O1W 2.019(4) . ? Ni1 N3 2.112(3) 3_464 ? Ni1 N1 2.145(3) . ? Ni1 O2 2.149(2) . ? Ni1 O1 2.195(3) . ? O1 C1 1.259(4) . ? O2 C1 1.246(5) . ? O3 C6 1.276(5) . ? O4 C6 1.210(6) . ? O1W H1W1 0.8499 . ? O1W H1W2 0.8501 . ? O2W H2W1 0.8501 . ? O2W H2W2 0.8499 . ? N1 C15 1.343(6) . ? N1 C11 1.346(6) . ? N2 C18 1.355(8) . ? N2 C16 1.366(11) . ? N2 H2N 0.8600 . ? N3 C21 1.307(6) . ? N3 C17 1.326(6) . ? N3 Ni1 2.112(3) 3_665 ? C1 C3 1.484(5) . ? C2 C3 1.379(4) . ? C2 C3 1.379(4) 2_675 ? C2 H2 0.9300 . ? C3 C4 1.388(5) . ? C4 C5 1.375(5) . ? C4 H4 0.9300 . ? C5 C4 1.375(5) 2_675 ? C5 H5 0.9300 . ? C6 C8 1.506(5) . ? C7 C8 1.394(5) . ? C7 C8 1.394(5) 2_565 ? C7 H7 0.9300 . ? C8 C9 1.375(6) . ? C9 C10 1.384(5) . ? C9 H9 0.9300 . ? C10 C9 1.384(5) 2_565 ? C10 H10 0.9300 . ? C11 C12 1.360(7) . ? C11 H11 0.9300 . ? C12 C13 1.364(11) . ? C12 C16 1.525(10) . ? C13 C14 1.374(11) . ? C13 H13 0.9300 . ? C14 C15 1.345(7) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.405(7) . ? C17 H17 0.9300 . ? C18 C19 1.355(9) . ? C19 C20 1.351(10) . ? C19 H19 0.9300 . ? C20 C21 1.351(8) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Ni1 O1W 93.38(16) . . ? O3 Ni1 N3 91.36(13) . 3_464 ? O1W Ni1 N3 94.04(14) . 3_464 ? O3 Ni1 N1 87.42(12) . . ? O1W Ni1 N1 91.52(14) . . ? N3 Ni1 N1 174.37(18) 3_464 . ? O3 Ni1 O2 173.44(17) . . ? O1W Ni1 O2 92.93(12) . . ? N3 Ni1 O2 89.98(11) 3_464 . ? N1 Ni1 O2 90.63(11) . . ? O3 Ni1 O1 113.83(16) . . ? O1W Ni1 O1 152.67(12) . . ? N3 Ni1 O1 88.07(14) 3_464 . ? N1 Ni1 O1 87.41(14) . . ? O2 Ni1 O1 59.79(10) . . ? C1 O1 Ni1 89.0(2) . . ? C1 O2 Ni1 91.5(2) . . ? C6 O3 Ni1 146.8(4) . . ? Ni1 O1W H1W1 124.4 . . ? Ni1 O1W H1W2 126.5 . . ? H1W1 O1W H1W2 108.2 . . ? H2W1 O2W H2W2 108.1 . . ? C15 N1 C11 117.1(4) . . ? C15 N1 Ni1 119.4(3) . . ? C11 N1 Ni1 123.5(3) . . ? C18 N2 C16 125.6(6) . . ? C18 N2 H2N 117.2 . . ? C16 N2 H2N 117.2 . . ? C21 N3 C17 117.9(4) . . ? C21 N3 Ni1 121.7(3) . 3_665 ? C17 N3 Ni1 120.3(3) . 3_665 ? O2 C1 O1 119.6(3) . . ? O2 C1 C3 119.9(3) . . ? O1 C1 C3 120.4(3) . . ? C3 C2 C3 120.9(5) . 2_675 ? C3 C2 H2 119.6 . . ? C3 C2 H2 119.6 2_675 . ? C2 C3 C4 119.3(3) . . ? C2 C3 C1 118.6(3) . . ? C4 C3 C1 122.1(3) . . ? C5 C4 C3 120.0(4) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C4 120.5(5) 2_675 . ? C4 C5 H5 119.7 2_675 . ? C4 C5 H5 119.7 . . ? O4 C6 O3 126.5(4) . . ? O4 C6 C8 119.7(4) . . ? O3 C6 C8 113.8(4) . . ? C8 C7 C8 119.3(6) . 2_565 ? C8 C7 H7 120.3 . . ? C8 C7 H7 120.3 2_565 . ? C9 C8 C7 120.1(4) . . ? C9 C8 C6 120.6(3) . . ? C7 C8 C6 119.2(4) . . ? C8 C9 C10 120.3(4) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C9 C10 C9 119.9(6) 2_565 . ? C9 C10 H10 120.1 2_565 . ? C9 C10 H10 120.1 . . ? N1 C11 C12 123.5(5) . . ? N1 C11 H11 118.3 . . ? C12 C11 H11 118.3 . . ? C11 C12 C13 117.7(5) . . ? C11 C12 C16 119.4(7) . . ? C13 C12 C16 122.5(7) . . ? C12 C13 C14 120.0(5) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 119.0(6) . . ? C15 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? N1 C15 C14 122.7(5) . . ? N1 C15 H15 118.6 . . ? C14 C15 H15 118.6 . . ? N2 C16 C12 111.1(7) . . ? N2 C16 H16A 109.4 . . ? C12 C16 H16A 109.4 . . ? N2 C16 H16B 109.4 . . ? C12 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? N3 C17 C18 121.5(5) . . ? N3 C17 H17 119.2 . . ? C18 C17 H17 119.2 . . ? N2 C18 C19 119.7(6) . . ? N2 C18 C17 123.2(6) . . ? C19 C18 C17 116.9(5) . . ? C20 C19 C18 121.7(5) . . ? C20 C19 H19 119.1 . . ? C18 C19 H19 119.1 . . ? C21 C20 C19 116.8(6) . . ? C21 C20 H20 121.6 . . ? C19 C20 H20 121.6 . . ? N3 C21 C20 125.0(6) . . ? N3 C21 H21 117.5 . . ? C20 C21 H21 117.5 . . ? 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 O3 Ni1 O1 C1 -177.1(2) . . . . ? O1W Ni1 O1 C1 -2.8(4) . . . . ? N3 Ni1 O1 C1 92.3(2) 3_464 . . . ? N1 Ni1 O1 C1 -91.0(2) . . . . ? O2 Ni1 O1 C1 1.2(2) . . . . ? O1W Ni1 O2 C1 177.0(2) . . . . ? N3 Ni1 O2 C1 -89.0(2) 3_464 . . . ? N1 Ni1 O2 C1 85.4(2) . . . . ? O1 Ni1 O2 C1 -1.2(2) . . . . ? O1W Ni1 O3 C6 178.0(5) . . . . ? N3 Ni1 O3 C6 83.8(5) 3_464 . . . ? N1 Ni1 O3 C6 -90.7(5) . . . . ? O1 Ni1 O3 C6 -4.7(6) . . . . ? O3 Ni1 N1 C15 52.5(4) . . . . ? O1W Ni1 N1 C15 145.8(3) . . . . ? O2 Ni1 N1 C15 -121.2(3) . . . . ? O1 Ni1 N1 C15 -61.5(3) . . . . ? O3 Ni1 N1 C11 -125.5(4) . . . . ? O1W Ni1 N1 C11 -32.1(4) . . . . ? O2 Ni1 N1 C11 60.8(4) . . . . ? O1 Ni1 N1 C11 120.5(4) . . . . ? Ni1 O2 C1 O1 2.1(4) . . . . ? Ni1 O2 C1 C3 -176.1(3) . . . . ? Ni1 O1 C1 O2 -2.0(4) . . . . ? Ni1 O1 C1 C3 176.1(3) . . . . ? C3 C2 C3 C4 -0.4(3) 2_675 . . . ? C3 C2 C3 C1 -179.9(4) 2_675 . . . ? O2 C1 C3 C2 5.9(5) . . . . ? O1 C1 C3 C2 -172.3(3) . . . . ? O2 C1 C3 C4 -173.7(4) . . . . ? O1 C1 C3 C4 8.2(6) . . . . ? C2 C3 C4 C5 0.7(5) . . . . ? C1 C3 C4 C5 -179.7(3) . . . . ? C3 C4 C5 C4 -0.4(3) . . . 2_675 ? Ni1 O3 C6 O4 6.8(9) . . . . ? Ni1 O3 C6 C8 -174.7(3) . . . . ? C8 C7 C8 C9 0.6(3) 2_565 . . . ? C8 C7 C8 C6 -178.9(3) 2_565 . . . ? O4 C6 C8 C9 173.3(5) . . . . ? O3 C6 C8 C9 -5.3(5) . . . . ? O4 C6 C8 C7 -7.3(6) . . . . ? O3 C6 C8 C7 174.1(3) . . . . ? C7 C8 C9 C10 -1.2(5) . . . . ? C6 C8 C9 C10 178.3(3) . . . . ? C8 C9 C10 C9 0.6(3) . . . 2_565 ? C15 N1 C11 C12 -0.6(7) . . . . ? Ni1 N1 C11 C12 177.4(4) . . . . ? N1 C11 C12 C13 -1.0(9) . . . . ? N1 C11 C12 C16 -174.7(5) . . . . ? C11 C12 C13 C14 2.8(10) . . . . ? C16 C12 C13 C14 176.3(7) . . . . ? C12 C13 C14 C15 -3.1(11) . . . . ? C11 N1 C15 C14 0.4(7) . . . . ? Ni1 N1 C15 C14 -177.7(5) . . . . ? C13 C14 C15 N1 1.4(10) . . . . ? C18 N2 C16 C12 165.6(8) . . . . ? C11 C12 C16 N2 82.9(10) . . . . ? C13 C12 C16 N2 -90.5(10) . . . . ? C21 N3 C17 C18 0.4(7) . . . . ? Ni1 N3 C17 C18 180.0(4) 3_665 . . . ? C16 N2 C18 C19 -174.1(10) . . . . ? C16 N2 C18 C17 0.5(15) . . . . ? N3 C17 C18 N2 -172.7(7) . . . . ? N3 C17 C18 C19 2.0(9) . . . . ? N2 C18 C19 C20 171.3(8) . . . . ? C17 C18 C19 C20 -3.6(12) . . . . ? C18 C19 C20 C21 2.7(13) . . . . ? C17 N3 C21 C20 -1.4(9) . . . . ? Ni1 N3 C21 C20 179.0(6) 3_665 . . . ? C19 C20 C21 N3 -0.1(12) . . . . ? 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 H1W1 O1 0.85 1.79 2.639(4) 173.4 3_565 O1W H1W2 O4 0.85 1.79 2.640(5) 173.1 3_565 O2W H2W1 O2 0.85 2.14 2.977(9) 169.2 . O2W H2W2 O4 0.85 2.17 3.006(10) 169.3 3_565 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.77 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.187 _refine_diff_density_min -0.796 _refine_diff_density_rms 0.100 #===END data_complex8 #TrackingRef '- cif.cif' _database_code_depnum_ccdc_archive 'CCDC 870303' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H32 N6 O10 Zn3' _chemical_formula_sum 'C38 H32 N6 O10 Zn3' _chemical_formula_weight 928.81 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 orthorhombic _symmetry_space_group_name_H-M 'P nn2 ' _symmetry_space_group_name_Hall 'P 2 -2n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' _cell_length_a 18.662(4) _cell_length_b 20.461(4) _cell_length_c 9.4272(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3599.7(13) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 20371 _cell_measurement_theta_min 3.17 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.714 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 2.053 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7088 _exptl_absorpt_correction_T_max 0.7907 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 34240 _diffrn_reflns_av_R_equivalents 0.0861 _diffrn_reflns_av_sigmaI/netI 0.0745 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8211 _reflns_number_gt 5924 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0554P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.406(14) _refine_ls_number_reflns 8211 _refine_ls_number_parameters 523 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0781 _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.1173 _refine_ls_wR_factor_gt 0.1009 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.045 _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 0.63447(3) 0.66738(3) 0.25348(7) 0.03298(15) Uani 1 1 d . . . Zn2 Zn 0.72762(3) 0.61648(4) 0.55135(8) 0.04456(18) Uani 1 1 d . . . Zn3 Zn 0.82264(3) 0.57596(3) 0.85601(6) 0.03260(15) Uani 1 1 d . . . O1 O 0.5700(2) 0.6960(2) 0.4107(4) 0.0455(10) Uani 1 1 d . . . O2 O 0.6302(2) 0.6652(2) 0.6022(5) 0.0509(12) Uani 1 1 d . . . O3 O 0.3881(2) 0.8606(2) 0.4413(5) 0.0528(11) Uani 1 1 d . . . O4 O 0.3211(2) 0.8706(2) 0.6321(5) 0.0578(12) Uani 1 1 d . . . O5 O 0.5668(2) 0.6055(2) 0.1667(4) 0.0457(10) Uani 1 1 d . . . O6 O 0.6395(2) 0.6190(2) -0.0160(5) 0.0528(11) Uani 1 1 d . . . O7 O 0.8275(2) 0.5738(2) 0.4981(4) 0.0494(12) Uani 1 1 d . . . O8 O 0.8862(2) 0.5499(2) 0.6974(4) 0.0540(12) Uani 1 1 d . . . O9 O 0.71606(18) 0.6363(2) 0.3475(4) 0.0416(9) Uani 1 1 d D . . H9O H 0.7575(16) 0.637(4) 0.310(7) 0.062 Uiso 1 1 d D . . O10 O 0.7404(2) 0.6029(2) 0.7585(4) 0.0402(9) Uani 1 1 d D . . H10O H 0.714(3) 0.621(3) 0.820(5) 0.060 Uiso 1 1 d D . . N1 N 0.6400(2) 0.7550(2) 0.1458(5) 0.0400(11) Uani 1 1 d . . . N2 N 0.7375(3) 0.9003(3) -0.2205(7) 0.0628(18) Uani 1 1 d D . . H2A H 0.7674 0.9287 -0.1885 0.087 Uiso 1 1 calc R . . N3 N 0.6660(2) 0.9910(2) -0.5245(5) 0.0400(11) Uani 1 1 d . . . N4 N 0.6714(3) 0.5161(2) 0.5266(5) 0.0442(12) Uani 1 1 d . . . N5 N 0.6613(5) 0.3619(3) 0.7243(7) 0.090(3) Uani 1 1 d . . . H5A H 0.6493 0.3221 0.7072 0.113 Uiso 1 1 calc R . . N6 N 0.7043(3) 0.2224(3) 1.0677(6) 0.0547(14) Uani 1 1 d . . . C1 C 0.5804(3) 0.6946(2) 0.5426(6) 0.0316(11) Uani 1 1 d . . . C2 C 0.5274(2) 0.7313(3) 0.6316(6) 0.0301(11) Uani 1 1 d . . . C3 C 0.4751(3) 0.7687(2) 0.5685(6) 0.0324(11) Uani 1 1 d . . . H3 H 0.4723 0.7695 0.4700 0.039 Uiso 1 1 calc R . . C4 C 0.4264(2) 0.8052(2) 0.6469(6) 0.0312(11) Uani 1 1 d . . . C5 C 0.4304(3) 0.8038(3) 0.7925(6) 0.0379(13) Uani 1 1 d . . . H5 H 0.3980 0.8275 0.8469 0.045 Uiso 1 1 calc R . . C6 C 0.4832(3) 0.7667(3) 0.8574(7) 0.0463(14) Uani 1 1 d . . . H6 H 0.4859 0.7659 0.9559 0.056 Uiso 1 1 calc R . . C7 C 0.5317(3) 0.7311(3) 0.7796(6) 0.0363(12) Uani 1 1 d . . . H7 H 0.5671 0.7070 0.8251 0.044 Uiso 1 1 calc R . . C8 C 0.3733(3) 0.8483(3) 0.5717(6) 0.0336(12) Uani 1 1 d . . . C9 C 0.5870(3) 0.5934(3) 0.0394(6) 0.0374(13) Uani 1 1 d . . . C10 C 0.5000 0.5000 0.0346(9) 0.0368(18) Uani 1 2 d S . . H10 H 0.5000 0.5000 0.1333 0.044 Uiso 1 2 calc SR . . C11 C 0.5428(3) 0.5446(3) -0.0403(6) 0.0339(12) Uani 1 1 d . . . C12 C 0.5429(3) 0.5444(3) -0.1883(6) 0.0421(14) Uani 1 1 d . . . H12 H 0.5714 0.5736 -0.2385 0.050 Uiso 1 1 calc R . . C13 C 0.5000 0.5000 -0.2591(9) 0.044(2) Uani 1 2 d S . . H13 H 0.5000 0.5000 -0.3577 0.053 Uiso 1 2 calc SR . . C14 C 0.8795(3) 0.5527(2) 0.5642(6) 0.0333(12) Uani 1 1 d . . . C15 C 1.0000 0.5000 0.5522(8) 0.0302(15) Uani 1 2 d S . . H15 H 1.0000 0.5000 0.6508 0.036 Uiso 1 2 calc SR . . C16 C 0.9421(3) 0.5265(2) 0.4794(5) 0.0269(11) Uani 1 1 d . . . C17 C 0.9421(3) 0.5264(3) 0.3328(6) 0.0374(13) Uani 1 1 d . . . H17 H 0.9035 0.5439 0.2835 0.045 Uiso 1 1 calc R . . C18 C 1.0000 0.5000 0.2587(9) 0.0394(18) Uani 1 2 d S . . H18 H 1.0000 0.5000 0.1601 0.047 Uiso 1 2 calc SR . . C19 C 0.6830(3) 0.7666(3) 0.0356(7) 0.0425(14) Uani 1 1 d . . . H19 H 0.7138 0.7337 0.0050 0.051 Uiso 1 1 calc R . . C20 C 0.6832(3) 0.8261(3) -0.0348(6) 0.0478(16) Uani 1 1 d D . . C21 C 0.6360(4) 0.8721(3) 0.0073(7) 0.068(2) Uani 1 1 d . . . H21 H 0.6342 0.9120 -0.0402 0.082 Uiso 1 1 calc R . . C22 C 0.5909(5) 0.8610(3) 0.1184(9) 0.073(2) Uani 1 1 d . . . H22 H 0.5584 0.8928 0.1470 0.101 Uiso 1 1 calc R . . C23 C 0.5943(4) 0.8016(4) 0.1879(7) 0.065(2) Uani 1 1 d . . . H23 H 0.5644 0.7939 0.2651 0.078 Uiso 1 1 calc R . . C24 C 0.7332(4) 0.8360(3) -0.1552(8) 0.0588(18) Uani 1 1 d D . . H24A H 0.7809 0.8245 -0.1227 0.071 Uiso 1 1 calc R . . H24B H 0.7204 0.8050 -0.2288 0.071 Uiso 1 1 calc R . . C25 C 0.7053(3) 0.9732(3) -0.4127(6) 0.0415(14) Uani 1 1 d . . . H25 H 0.7428 1.0004 -0.3852 0.050 Uiso 1 1 calc R . . C26 C 0.6935(3) 0.9161(3) -0.3346(7) 0.0448(15) Uani 1 1 d D . . C27 C 0.6356(4) 0.8792(4) -0.3762(8) 0.0627(19) Uani 1 1 d . . . H27 H 0.6246 0.8411 -0.3271 0.075 Uiso 1 1 calc R . . C28 C 0.5942(4) 0.8974(4) -0.4874(8) 0.071(2) Uani 1 1 d . . . H28 H 0.5551 0.8721 -0.5143 0.085 Uiso 1 1 calc R . . C29 C 0.6107(4) 0.9539(3) -0.5603(8) 0.0586(18) Uani 1 1 d . . . H29 H 0.5823 0.9663 -0.6367 0.070 Uiso 1 1 calc R . . C30 C 0.6845(3) 0.4693(3) 0.6223(7) 0.0479(15) Uani 1 1 d . . . H30 H 0.7181 0.4774 0.6929 0.058 Uiso 1 1 calc R . . C31 C 0.6494(4) 0.4082(3) 0.6204(8) 0.0560(17) Uani 1 1 d . . . C32 C 0.6026(4) 0.3973(3) 0.5101(7) 0.0595(19) Uani 1 1 d . . . H32 H 0.5803 0.3568 0.5007 0.071 Uiso 1 1 calc R . . C33 C 0.5888(4) 0.4456(3) 0.4149(8) 0.0573(17) Uani 1 1 d . . . H33 H 0.5554 0.4393 0.3430 0.069 Uiso 1 1 calc R . . C34 C 0.6249(3) 0.5038(3) 0.4265(8) 0.0539(17) Uani 1 1 d . . . H34 H 0.6158 0.5361 0.3595 0.065 Uiso 1 1 calc R . . C35 C 0.6914(6) 0.3763(4) 0.8540(9) 0.070(2) Uani 1 1 d . . . H35A H 0.6737 0.4184 0.8857 0.113 Uiso 1 1 calc R . . H35B H 0.7430 0.3800 0.8428 0.113 Uiso 1 1 calc R . . C36 C 0.7151(4) 0.2687(3) 0.9718(7) 0.0559(18) Uani 1 1 d . . . H36 H 0.7511 0.2624 0.9049 0.067 Uiso 1 1 calc R . . C37 C 0.6756(5) 0.3260(3) 0.9661(8) 0.065(2) Uani 1 1 d . . . C38 C 0.6210(4) 0.3343(3) 1.0647(9) 0.067(2) Uani 1 1 d . . . H38 H 0.5933 0.3721 1.0642 0.081 Uiso 1 1 calc R . . C39 C 0.6085(4) 0.2863(4) 1.1624(9) 0.069(2) Uani 1 1 d . . . H39 H 0.5715 0.2903 1.2278 0.083 Uiso 1 1 calc R . . C40 C 0.6520(4) 0.2320(4) 1.1616(8) 0.0632(19) Uani 1 1 d . . . H40 H 0.6444 0.2002 1.2305 0.076 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 0.0377(3) 0.0308(3) 0.0305(3) 0.0015(3) -0.0004(3) 0.0038(3) Zn2 0.0416(3) 0.0599(4) 0.0322(3) 0.0098(3) 0.0030(3) 0.0217(3) Zn3 0.0334(3) 0.0343(3) 0.0301(3) 0.0006(3) -0.0026(3) 0.0012(3) O1 0.051(2) 0.056(3) 0.029(2) -0.0016(19) -0.0021(17) 0.021(2) O2 0.048(2) 0.068(3) 0.037(2) 0.010(2) 0.0059(17) 0.027(2) O3 0.063(3) 0.057(3) 0.038(3) 0.000(2) 0.002(2) 0.023(2) O4 0.046(2) 0.071(3) 0.056(3) 0.008(2) 0.015(2) 0.024(2) O5 0.052(2) 0.053(3) 0.032(2) -0.0048(19) 0.0040(19) -0.012(2) O6 0.046(2) 0.058(3) 0.054(3) -0.011(2) 0.008(2) -0.013(2) O7 0.040(2) 0.075(3) 0.034(2) 0.009(2) -0.0014(16) 0.027(2) O8 0.048(2) 0.083(3) 0.030(2) 0.001(2) 0.0027(17) 0.024(2) O9 0.0358(19) 0.050(2) 0.039(2) 0.018(2) 0.0069(18) 0.0099(19) O10 0.0351(19) 0.052(2) 0.033(2) 0.006(2) 0.0031(17) 0.0092(18) N1 0.051(3) 0.027(2) 0.042(3) -0.001(2) -0.001(2) 0.001(2) N2 0.083(5) 0.043(4) 0.068(4) 0.028(3) 0.011(4) 0.010(2) N3 0.046(3) 0.038(3) 0.036(3) 0.001(2) 0.005(2) -0.011(2) N4 0.052(3) 0.038(3) 0.043(3) 0.009(2) -0.002(2) 0.003(2) N5 0.172(9) 0.045(4) 0.049(5) 0.012(4) -0.048(6) -0.008(5) N6 0.073(3) 0.045(3) 0.046(3) 0.013(3) -0.006(3) -0.006(3) C1 0.031(3) 0.031(3) 0.033(3) 0.007(2) 0.004(2) 0.006(2) C2 0.029(3) 0.030(3) 0.031(3) 0.003(2) 0.001(2) -0.001(2) C3 0.043(3) 0.030(3) 0.025(3) -0.001(2) 0.004(2) -0.004(2) C4 0.026(2) 0.026(3) 0.041(3) 0.001(2) 0.002(2) -0.002(2) C5 0.048(3) 0.036(3) 0.030(3) 0.000(2) 0.007(2) 0.008(3) C6 0.054(3) 0.058(4) 0.027(3) -0.001(3) 0.003(3) -0.003(3) C7 0.041(3) 0.035(3) 0.033(3) 0.007(2) -0.004(2) 0.004(3) C8 0.033(3) 0.029(3) 0.038(4) -0.001(2) 0.004(2) 0.000(2) C9 0.035(3) 0.037(3) 0.040(3) 0.007(3) 0.005(2) -0.001(2) C10 0.034(4) 0.043(5) 0.033(4) 0.000 0.000 -0.001(3) C11 0.034(3) 0.037(3) 0.031(3) 0.002(2) 0.000(2) 0.009(2) C12 0.046(3) 0.045(3) 0.036(3) 0.005(3) 0.007(2) 0.003(3) C13 0.061(5) 0.047(5) 0.024(4) 0.000 0.000 -0.006(4) C14 0.034(3) 0.027(3) 0.039(3) 0.004(2) 0.003(2) 0.007(2) C15 0.033(3) 0.030(4) 0.028(4) 0.000 0.000 -0.004(3) C16 0.030(3) 0.026(3) 0.024(3) -0.001(2) 0.0035(19) -0.004(2) C17 0.030(3) 0.047(3) 0.035(3) 0.004(3) -0.003(2) 0.000(2) C18 0.037(4) 0.059(5) 0.022(4) 0.000 0.000 0.003(4) C19 0.052(3) 0.026(3) 0.050(4) 0.001(3) 0.000(3) 0.009(3) C20 0.078(5) 0.026(3) 0.039(4) 0.006(3) -0.003(3) 0.003(3) C21 0.119(6) 0.044(4) 0.042(4) 0.014(3) 0.005(4) 0.025(4) C22 0.125(6) 0.049(4) 0.047(3) 0.018(4) 0.010(4) 0.030(3) C23 0.087(5) 0.059(5) 0.049(4) 0.014(3) 0.017(4) 0.041(4) C24 0.079(5) 0.037(4) 0.060(4) 0.020(3) 0.005(4) 0.003(3) C25 0.047(3) 0.033(3) 0.044(4) 0.007(2) 0.001(3) -0.007(3) C26 0.056(4) 0.040(3) 0.039(4) 0.005(3) 0.005(3) -0.001(3) C27 0.085(5) 0.051(4) 0.053(4) 0.008(3) 0.002(4) -0.027(4) C28 0.094(6) 0.066(5) 0.053(5) 0.010(4) -0.010(4) -0.042(5) C29 0.068(4) 0.060(4) 0.048(4) 0.007(3) -0.008(3) -0.026(4) C30 0.061(4) 0.038(3) 0.044(4) 0.008(3) -0.006(3) 0.000(3) C31 0.081(5) 0.037(3) 0.050(4) 0.012(3) 0.002(4) 0.005(3) C32 0.088(5) 0.042(4) 0.049(4) -0.001(3) 0.003(4) -0.017(4) C33 0.072(4) 0.050(4) 0.049(4) 0.012(3) -0.007(3) -0.009(4) C34 0.063(4) 0.043(4) 0.056(4) 0.018(3) -0.009(3) 0.003(3) C35 0.113(5) 0.045(3) 0.051(4) 0.015(3) -0.012(4) -0.006(4) C36 0.085(5) 0.034(3) 0.048(4) 0.009(3) 0.002(3) -0.012(4) C37 0.108(6) 0.041(4) 0.046(4) 0.011(3) -0.019(4) -0.012(4) C38 0.086(5) 0.042(4) 0.074(6) 0.003(4) -0.023(4) 0.010(4) C39 0.076(5) 0.069(5) 0.062(5) -0.006(4) 0.003(4) -0.002(4) C40 0.080(5) 0.056(5) 0.053(5) 0.017(4) -0.005(4) -0.006(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 Zn1 O9 1.873(4) . ? Zn1 O5 1.966(4) . ? Zn1 O1 1.996(4) . ? Zn1 N1 2.062(5) . ? Zn1 O6 2.728(5) . ? Zn2 O9 1.976(4) . ? Zn2 O10 1.987(4) . ? Zn2 O7 2.119(4) . ? Zn2 O2 2.128(4) . ? Zn2 N4 2.318(5) . ? Zn2 N6 2.517(6) 4_654 ? Zn3 O10 1.873(4) . ? Zn3 O3 1.956(4) 3_565 ? Zn3 O8 1.981(4) . ? Zn3 N3 2.082(5) 4_646 ? O1 C1 1.259(7) . ? O2 C1 1.242(6) . ? O3 C8 1.284(7) . ? O3 Zn3 1.956(4) 3_464 ? O4 C8 1.217(6) . ? O5 C9 1.282(7) . ? O6 C9 1.228(6) . ? O7 C14 1.231(6) . ? O8 C14 1.263(6) . ? O9 H9O 0.85(4) . ? O10 H10O 0.85(4) . ? N1 C19 1.334(7) . ? N1 C23 1.340(8) . ? N2 C26 1.392(7) . ? N2 C24 1.454(8) . ? N2 H2A 0.8600 . ? N3 C29 1.324(7) . ? N3 C25 1.334(7) . ? N3 Zn3 2.082(5) 4_653 ? N4 C34 1.307(8) . ? N4 C30 1.337(7) . ? N5 C35 1.378(10) . ? N5 C31 1.380(9) . ? N5 H5A 0.8600 . ? N6 C36 1.325(8) . ? N6 C40 1.332(9) . ? N6 Zn2 2.517(6) 4_645 ? C1 C2 1.498(7) . ? C2 C3 1.374(7) . ? C2 C7 1.398(8) . ? C3 C4 1.391(7) . ? C3 H3 0.9300 . ? C4 C5 1.374(8) . ? C4 C8 1.504(7) . ? C5 C6 1.387(8) . ? C5 H5 0.9300 . ? C6 C7 1.373(8) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C9 C11 1.497(8) . ? C10 C11 1.404(7) 2_665 ? C10 C11 1.404(7) . ? C10 H10 0.9300 . ? C11 C12 1.395(8) . ? C12 C13 1.382(7) . ? C12 H12 0.9300 . ? C13 C12 1.382(7) 2_665 ? C13 H13 0.9300 . ? C14 C16 1.513(7) . ? C15 C16 1.390(6) . ? C15 C16 1.390(6) 2_765 ? C15 H15 0.9300 . ? C16 C17 1.382(7) . ? C17 C18 1.395(7) . ? C17 H17 0.9300 . ? C18 C17 1.395(7) 2_765 ? C18 H18 0.9300 . ? C19 C20 1.386(8) . ? C19 H19 0.9300 . ? C20 C21 1.350(9) . ? C20 C24 1.483(7) . ? C21 C22 1.363(10) . ? C21 H21 0.9300 . ? C22 C23 1.382(9) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.399(8) . ? C25 H25 0.9300 . ? C26 C27 1.374(9) . ? C27 C28 1.354(10) . ? C27 H27 0.9300 . ? C28 C29 1.380(9) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.412(9) . ? C30 H30 0.9300 . ? C31 C32 1.377(10) . ? C32 C33 1.360(9) . ? C32 H32 0.9300 . ? C33 C34 1.372(9) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C37 1.504(10) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.387(10) . ? C36 H36 0.9300 . ? C37 C38 1.390(11) . ? C38 C39 1.366(11) . ? C38 H38 0.9300 . ? C39 C40 1.376(10) . ? C39 H39 0.9300 . ? C40 H40 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 O9 Zn1 O5 120.04(18) . . ? O9 Zn1 O1 103.79(17) . . ? O5 Zn1 O1 96.37(17) . . ? O9 Zn1 N1 119.14(18) . . ? O5 Zn1 N1 112.77(18) . . ? O1 Zn1 N1 98.06(18) . . ? O9 Zn2 O10 176.12(19) . . ? O9 Zn2 O7 87.16(15) . . ? O10 Zn2 O7 94.02(16) . . ? O9 Zn2 O2 91.70(16) . . ? O10 Zn2 O2 86.91(16) . . ? O7 Zn2 O2 176.40(19) . . ? O9 Zn2 N4 91.99(17) . . ? O10 Zn2 N4 91.69(18) . . ? O7 Zn2 N4 90.57(18) . . ? O2 Zn2 N4 92.88(18) . . ? O9 Zn2 N6 86.43(18) . 4_654 ? O10 Zn2 N6 89.96(18) . 4_654 ? O7 Zn2 N6 85.68(18) . 4_654 ? O2 Zn2 N6 90.84(18) . 4_654 ? N4 Zn2 N6 176.00(18) . 4_654 ? O10 Zn3 O3 121.21(19) . 3_565 ? O10 Zn3 O8 101.53(17) . . ? O3 Zn3 O8 96.59(19) 3_565 . ? O10 Zn3 N3 126.51(19) . 4_646 ? O3 Zn3 N3 105.55(19) 3_565 4_646 ? O8 Zn3 N3 97.06(19) . 4_646 ? C1 O1 Zn1 129.4(3) . . ? C1 O2 Zn2 139.9(4) . . ? C8 O3 Zn3 112.9(3) . 3_464 ? C9 O5 Zn1 109.0(3) . . ? C14 O7 Zn2 135.9(4) . . ? C14 O8 Zn3 132.8(3) . . ? Zn1 O9 Zn2 128.21(19) . . ? Zn1 O9 H9O 122(5) . . ? Zn2 O9 H9O 108(5) . . ? Zn3 O10 Zn2 128.4(2) . . ? Zn3 O10 H10O 106(5) . . ? Zn2 O10 H10O 122(5) . . ? C19 N1 C23 119.1(5) . . ? C19 N1 Zn1 124.6(4) . . ? C23 N1 Zn1 116.2(4) . . ? C26 N2 C24 120.3(6) . . ? C26 N2 H2A 119.9 . . ? C24 N2 H2A 119.9 . . ? C29 N3 C25 118.2(5) . . ? C29 N3 Zn3 114.8(4) . 4_653 ? C25 N3 Zn3 126.8(4) . 4_653 ? C34 N4 C30 118.1(6) . . ? C34 N4 Zn2 123.0(4) . . ? C30 N4 Zn2 118.9(4) . . ? C35 N5 C31 123.2(6) . . ? C35 N5 H5A 118.4 . . ? C31 N5 H5A 118.4 . . ? C36 N6 C40 117.4(6) . . ? C36 N6 Zn2 119.8(5) . 4_645 ? C40 N6 Zn2 122.5(4) . 4_645 ? O2 C1 O1 124.9(5) . . ? O2 C1 C2 118.9(5) . . ? O1 C1 C2 116.1(4) . . ? C3 C2 C7 118.3(5) . . ? C3 C2 C1 120.3(5) . . ? C7 C2 C1 121.3(5) . . ? C2 C3 C4 122.2(5) . . ? C2 C3 H3 118.9 . . ? C4 C3 H3 118.9 . . ? C5 C4 C3 118.9(5) . . ? C5 C4 C8 121.3(5) . . ? C3 C4 C8 119.7(5) . . ? C4 C5 C6 119.4(5) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C7 C6 C5 121.5(6) . . ? C7 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C6 C7 C2 119.6(5) . . ? C6 C7 H7 120.2 . . ? C2 C7 H7 120.2 . . ? O4 C8 O3 123.1(5) . . ? O4 C8 C4 121.8(5) . . ? O3 C8 C4 115.1(4) . . ? O6 C9 O5 123.4(5) . . ? O6 C9 C11 120.7(5) . . ? O5 C9 C11 115.9(5) . . ? C11 C10 C11 119.5(7) 2_665 . ? C11 C10 H10 120.2 2_665 . ? C11 C10 H10 120.2 . . ? C12 C11 C10 120.1(6) . . ? C12 C11 C9 120.2(5) . . ? C10 C11 C9 119.6(5) . . ? C13 C12 C11 119.0(6) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C12 C13 C12 122.3(8) . 2_665 ? C12 C13 H13 118.9 . . ? C12 C13 H13 118.9 2_665 . ? O7 C14 O8 126.6(5) . . ? O7 C14 C16 117.7(5) . . ? O8 C14 C16 115.7(4) . . ? C16 C15 C16 120.8(7) . 2_765 ? C16 C15 H15 119.6 . . ? C16 C15 H15 119.6 2_765 . ? C17 C16 C15 119.5(5) . . ? C17 C16 C14 121.9(5) . . ? C15 C16 C14 118.5(5) . . ? C16 C17 C18 120.1(5) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C17 119.9(8) . 2_765 ? C17 C18 H18 120.0 . . ? C17 C18 H18 120.0 2_765 . ? N1 C19 C20 122.0(5) . . ? N1 C19 H19 119.0 . . ? C20 C19 H19 119.0 . . ? C21 C20 C19 118.1(6) . . ? C21 C20 C24 122.6(6) . . ? C19 C20 C24 119.3(5) . . ? C20 C21 C22 120.8(6) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C21 C22 C23 118.9(7) . . ? C21 C22 H22 120.5 . . ? C23 C22 H22 120.5 . . ? N1 C23 C22 121.0(6) . . ? N1 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? N2 C24 C20 118.9(6) . . ? N2 C24 H24A 107.6 . . ? C20 C24 H24A 107.6 . . ? N2 C24 H24B 107.6 . . ? C20 C24 H24B 107.6 . . ? H24A C24 H24B 107.0 . . ? N3 C25 C26 123.8(5) . . ? N3 C25 H25 118.1 . . ? C26 C25 H25 118.1 . . ? C27 C26 N2 123.9(6) . . ? C27 C26 C25 115.6(6) . . ? N2 C26 C25 120.5(5) . . ? C28 C27 C26 121.3(6) . . ? C28 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? C27 C28 C29 119.2(7) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? N3 C29 C28 121.8(6) . . ? N3 C29 H29 119.1 . . ? C28 C29 H29 119.1 . . ? N4 C30 C31 122.7(6) . . ? N4 C30 H30 118.6 . . ? C31 C30 H30 118.6 . . ? C32 C31 N5 121.7(7) . . ? C32 C31 C30 116.6(6) . . ? N5 C31 C30 121.7(7) . . ? C33 C32 C31 120.0(7) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C34 119.1(7) . . ? C32 C33 H33 120.5 . . ? C34 C33 H33 120.5 . . ? N4 C34 C33 123.4(6) . . ? N4 C34 H34 118.3 . . ? C33 C34 H34 118.3 . . ? N5 C35 C37 113.4(7) . . ? N5 C35 H35A 108.9 . . ? C37 C35 H35A 108.9 . . ? N5 C35 H35B 108.9 . . ? C37 C35 H35B 108.9 . . ? H35A C35 H35B 107.7 . . ? N6 C36 C37 123.4(7) . . ? N6 C36 H36 118.3 . . ? C37 C36 H36 118.3 . . ? C36 C37 C38 117.8(6) . . ? C36 C37 C35 120.1(8) . . ? C38 C37 C35 122.0(8) . . ? C39 C38 C37 119.2(7) . . ? C39 C38 H38 120.4 . . ? C37 C38 H38 120.4 . . ? C38 C39 C40 118.5(8) . . ? C38 C39 H39 120.8 . . ? C40 C39 H39 120.8 . . ? N6 C40 C39 123.7(7) . . ? N6 C40 H40 118.2 . . ? C39 C40 H40 118.2 . . ? 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 O9 Zn1 O1 C1 0.5(5) . . . . ? O5 Zn1 O1 C1 123.6(5) . . . . ? N1 Zn1 O1 C1 -122.3(5) . . . . ? O9 Zn2 O2 C1 1.4(6) . . . . ? O10 Zn2 O2 C1 177.8(6) . . . . ? N4 Zn2 O2 C1 -90.7(6) . . . . ? N6 Zn2 O2 C1 87.9(6) 4_654 . . . ? O9 Zn1 O5 C9 -88.2(4) . . . . ? O1 Zn1 O5 C9 161.8(4) . . . . ? N1 Zn1 O5 C9 60.3(4) . . . . ? O9 Zn2 O7 C14 170.6(6) . . . . ? O10 Zn2 O7 C14 -5.7(6) . . . . ? N4 Zn2 O7 C14 -97.4(6) . . . . ? N6 Zn2 O7 C14 84.0(6) 4_654 . . . ? O10 Zn3 O8 C14 4.0(6) . . . . ? O3 Zn3 O8 C14 -119.8(6) 3_565 . . . ? N3 Zn3 O8 C14 133.6(6) 4_646 . . . ? O5 Zn1 O9 Zn2 -92.8(3) . . . . ? O1 Zn1 O9 Zn2 13.1(3) . . . . ? N1 Zn1 O9 Zn2 120.7(3) . . . . ? O7 Zn2 O9 Zn1 170.4(3) . . . . ? O2 Zn2 O9 Zn1 -13.0(3) . . . . ? N4 Zn2 O9 Zn1 80.0(3) . . . . ? N6 Zn2 O9 Zn1 -103.7(3) 4_654 . . . ? O3 Zn3 O10 Zn2 95.5(3) 3_565 . . . ? O8 Zn3 O10 Zn2 -9.6(3) . . . . ? N3 Zn3 O10 Zn2 -117.5(3) 4_646 . . . ? O7 Zn2 O10 Zn3 9.7(3) . . . . ? O2 Zn2 O10 Zn3 -166.8(3) . . . . ? N4 Zn2 O10 Zn3 100.4(3) . . . . ? N6 Zn2 O10 Zn3 -76.0(3) 4_654 . . . ? O9 Zn1 N1 C19 62.1(5) . . . . ? O5 Zn1 N1 C19 -86.7(5) . . . . ? O1 Zn1 N1 C19 172.8(5) . . . . ? O9 Zn1 N1 C23 -121.0(5) . . . . ? O5 Zn1 N1 C23 90.2(5) . . . . ? O1 Zn1 N1 C23 -10.3(5) . . . . ? O9 Zn2 N4 C34 -25.9(5) . . . . ? O10 Zn2 N4 C34 152.9(5) . . . . ? O7 Zn2 N4 C34 -113.0(5) . . . . ? O2 Zn2 N4 C34 65.9(5) . . . . ? O9 Zn2 N4 C30 157.1(4) . . . . ? O10 Zn2 N4 C30 -24.1(5) . . . . ? O7 Zn2 N4 C30 69.9(5) . . . . ? O2 Zn2 N4 C30 -111.1(5) . . . . ? Zn2 O2 C1 O1 11.0(10) . . . . ? Zn2 O2 C1 C2 -169.5(4) . . . . ? Zn1 O1 C1 O2 -11.8(9) . . . . ? Zn1 O1 C1 C2 168.7(3) . . . . ? O2 C1 C2 C3 174.8(5) . . . . ? O1 C1 C2 C3 -5.7(7) . . . . ? O2 C1 C2 C7 -2.2(8) . . . . ? O1 C1 C2 C7 177.3(5) . . . . ? C7 C2 C3 C4 -0.7(7) . . . . ? C1 C2 C3 C4 -177.8(5) . . . . ? C2 C3 C4 C5 -0.3(8) . . . . ? C2 C3 C4 C8 176.3(5) . . . . ? C3 C4 C5 C6 0.7(8) . . . . ? C8 C4 C5 C6 -175.7(5) . . . . ? C4 C5 C6 C7 -0.2(9) . . . . ? C5 C6 C7 C2 -0.8(8) . . . . ? C3 C2 C7 C6 1.2(8) . . . . ? C1 C2 C7 C6 178.3(5) . . . . ? Zn3 O3 C8 O4 4.6(7) 3_464 . . . ? Zn3 O3 C8 C4 -173.9(3) 3_464 . . . ? C5 C4 C8 O4 -18.6(8) . . . . ? C3 C4 C8 O4 165.0(5) . . . . ? C5 C4 C8 O3 160.0(5) . . . . ? C3 C4 C8 O3 -16.4(7) . . . . ? Zn1 O5 C9 O6 -1.9(7) . . . . ? Zn1 O5 C9 C11 177.5(4) . . . . ? C11 C10 C11 C12 -0.2(4) 2_665 . . . ? C11 C10 C11 C9 178.3(5) 2_665 . . . ? O6 C9 C11 C12 -23.3(8) . . . . ? O5 C9 C11 C12 157.3(5) . . . . ? O6 C9 C11 C10 158.2(5) . . . . ? O5 C9 C11 C10 -21.2(7) . . . . ? C10 C11 C12 C13 0.3(7) . . . . ? C9 C11 C12 C13 -178.1(4) . . . . ? C11 C12 C13 C12 -0.2(4) . . . 2_665 ? Zn2 O7 C14 O8 1.6(10) . . . . ? Zn2 O7 C14 C16 -179.2(4) . . . . ? Zn3 O8 C14 O7 -0.3(10) . . . . ? Zn3 O8 C14 C16 -179.5(4) . . . . ? C16 C15 C16 C17 0.1(4) 2_765 . . . ? C16 C15 C16 C14 178.2(5) 2_765 . . . ? O7 C14 C16 C17 0.6(8) . . . . ? O8 C14 C16 C17 179.9(5) . . . . ? O7 C14 C16 C15 -177.4(4) . . . . ? O8 C14 C16 C15 1.9(7) . . . . ? C15 C16 C17 C18 -0.2(7) . . . . ? C14 C16 C17 C18 -178.2(4) . . . . ? C16 C17 C18 C17 0.1(4) . . . 2_765 ? C23 N1 C19 C20 1.6(9) . . . . ? Zn1 N1 C19 C20 178.5(5) . . . . ? N1 C19 C20 C21 -2.8(10) . . . . ? N1 C19 C20 C24 179.0(6) . . . . ? C19 C20 C21 C22 1.8(11) . . . . ? C24 C20 C21 C22 180.0(8) . . . . ? C20 C21 C22 C23 0.1(13) . . . . ? C19 N1 C23 C22 0.4(11) . . . . ? Zn1 N1 C23 C22 -176.7(7) . . . . ? C21 C22 C23 N1 -1.3(14) . . . . ? C26 N2 C24 C20 -90.6(8) . . . . ? C21 C20 C24 N2 7.2(10) . . . . ? C19 C20 C24 N2 -174.7(6) . . . . ? C29 N3 C25 C26 2.9(9) . . . . ? Zn3 N3 C25 C26 178.2(4) 4_653 . . . ? C24 N2 C26 C27 12.5(11) . . . . ? C24 N2 C26 C25 -169.4(6) . . . . ? N3 C25 C26 C27 -2.7(9) . . . . ? N3 C25 C26 N2 179.0(6) . . . . ? N2 C26 C27 C28 179.3(7) . . . . ? C25 C26 C27 C28 1.1(11) . . . . ? C26 C27 C28 C29 0.2(12) . . . . ? C25 N3 C29 C28 -1.4(10) . . . . ? Zn3 N3 C29 C28 -177.2(6) 4_653 . . . ? C27 C28 C29 N3 -0.1(12) . . . . ? C34 N4 C30 C31 -1.1(10) . . . . ? Zn2 N4 C30 C31 176.1(5) . . . . ? C35 N5 C31 C32 -161.8(9) . . . . ? C35 N5 C31 C30 17.8(14) . . . . ? N4 C30 C31 C32 2.9(10) . . . . ? N4 C30 C31 N5 -176.8(7) . . . . ? N5 C31 C32 C33 175.8(7) . . . . ? C30 C31 C32 C33 -4.0(11) . . . . ? C31 C32 C33 C34 3.3(11) . . . . ? C30 N4 C34 C33 0.3(10) . . . . ? Zn2 N4 C34 C33 -176.8(5) . . . . ? C32 C33 C34 N4 -1.4(11) . . . . ? C31 N5 C35 C37 159.5(8) . . . . ? C40 N6 C36 C37 0.7(10) . . . . ? Zn2 N6 C36 C37 174.3(5) 4_645 . . . ? N6 C36 C37 C38 -1.3(11) . . . . ? N6 C36 C37 C35 179.8(7) . . . . ? N5 C35 C37 C36 80.7(10) . . . . ? N5 C35 C37 C38 -98.1(10) . . . . ? C36 C37 C38 C39 0.0(11) . . . . ? C35 C37 C38 C39 178.9(7) . . . . ? C37 C38 C39 C40 1.7(11) . . . . ? C36 N6 C40 C39 1.1(11) . . . . ? Zn2 N6 C40 C39 -172.3(6) 4_645 . . . ? C38 C39 C40 N6 -2.3(12) . . . . ? 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 O9 H9O O4 0.85(4) 2.06(4) 2.826(6) 150(6) 3_564 O10 H10O O6 0.85(4) 2.08(3) 2.858(6) 152(6) 1_556 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.107 _refine_diff_density_min -0.667 _refine_diff_density_rms 0.099