# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1585 data_complex1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety [CoL1]1/2Br1/2NO3.5H2O _chemical_formula_sum 'C18 H31 Br0.50 Co N4.50 O8' _chemical_formula_weight 537.36 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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinc _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.635(11) _cell_length_b 12.653(14) _cell_length_c 18.08(2) _cell_angle_alpha 90.31 _cell_angle_beta 93.818(10) _cell_angle_gamma 90.00 _cell_volume 2199(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.623 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1116 _exptl_absorpt_coefficient_mu 1.743 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7044 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7044 _reflns_number_gt 5118 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1288P)^2^+5.2432P] 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 7044 _refine_ls_number_parameters 614 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1060 _refine_ls_R_factor_gt 0.0737 _refine_ls_wR_factor_ref 0.2226 _refine_ls_wR_factor_gt 0.1997 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.098 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group CoA Co 0.14952(8) 0.37418(6) 0.24889(4) 0.0283(2) Uani 1 d . A 1 N1A N 0.0336(5) 0.3564(4) 0.1508(3) 0.0385(12) Uani 1 d . A 1 C2A C 0.1139(8) 0.3867(6) 0.0870(4) 0.0543(18) Uani 1 d . A 1 H2A1 H 0.1383 0.4609 0.0919 0.065 Uiso 1 calc R A 1 H2A2 H 0.0542 0.3787 0.0419 0.065 Uiso 1 calc R A 1 C3A C 0.2472(8) 0.3231(6) 0.0784(4) 0.0528(18) Uani 1 d . A 1 H3A1 H 0.2267 0.2484 0.0822 0.063 Uiso 1 calc R A 1 H3A2 H 0.2795 0.3355 0.0295 0.063 Uiso 1 calc R A 1 C4A C 0.3616(7) 0.3523(6) 0.1362(3) 0.0452(16) Uani 1 d . A 1 H4A1 H 0.4467 0.3173 0.1240 0.054 Uiso 1 calc R A 1 H4A2 H 0.3775 0.4279 0.1342 0.054 Uiso 1 calc R A 1 N5A N 0.3314(5) 0.3234(4) 0.2145(3) 0.0327(11) Uani 1 d . A 1 C6A C 0.4418(6) 0.3731(5) 0.2659(3) 0.0357(13) Uani 1 d . A 1 H6A1 H 0.5254 0.3303 0.2671 0.043 Uiso 1 calc R A 1 H6A2 H 0.4642 0.4427 0.2480 0.043 Uiso 1 calc R A 1 C7A C 0.3927(6) 0.3821(5) 0.3414(3) 0.0346(13) Uani 1 d . A 1 N8A N 0.2536(5) 0.3892(4) 0.3402(3) 0.0321(11) Uani 1 d . A 1 C9A C 0.1842(7) 0.3984(5) 0.4027(3) 0.0370(14) Uani 1 d . A 1 C10A C 0.0301(7) 0.3960(5) 0.3853(3) 0.0407(15) Uani 1 d . A 1 H10A H -0.0047 0.3250 0.3920 0.049 Uiso 1 calc R A 1 H10B H -0.0151 0.4429 0.4188 0.049 Uiso 1 calc R A 1 N11A N -0.0028(5) 0.4301(4) 0.3070(3) 0.0325(11) Uani 1 d . A 1 C12A C -0.1429(6) 0.3854(5) 0.2824(4) 0.0413(15) Uani 1 d . A 1 H12A H -0.1384 0.3090 0.2857 0.050 Uiso 1 calc R A 1 H12B H -0.2101 0.4097 0.3164 0.050 Uiso 1 calc R A 1 C13A C -0.1941(7) 0.4146(7) 0.2051(4) 0.0565(19) Uani 1 d . A 1 H13A H -0.2512 0.4775 0.2083 0.068 Uiso 1 calc R A 1 H13B H -0.2545 0.3582 0.1857 0.068 Uiso 1 calc R A 1 C14A C -0.0869(7) 0.4358(6) 0.1485(4) 0.0488(17) Uani 1 d . A 1 H14A H -0.0491 0.5062 0.1570 0.059 Uiso 1 calc R A 1 H14B H -0.1335 0.4344 0.0993 0.059 Uiso 1 calc R A 1 C21A C 0.4690(7) 0.3845(5) 0.4095(4) 0.0456(16) Uani 1 d . A 1 H21A H 0.5655 0.3790 0.4116 0.055 Uiso 1 calc R A 1 C22A C 0.4008(8) 0.3951(5) 0.4739(4) 0.0481(17) Uani 1 d . A 1 H22A H 0.4514 0.3976 0.5195 0.058 Uiso 1 calc R A 1 C23A C 0.2568(8) 0.4021(5) 0.4706(3) 0.0453(16) Uani 1 d . A 1 H23A H 0.2102 0.4091 0.5138 0.054 Uiso 1 calc R A 1 C41A C -0.0260(8) 0.2485(5) 0.1377(4) 0.0536(18) Uani 1 d . A 1 H41A H -0.0826 0.2477 0.0920 0.064 Uiso 1 calc R A 1 H41B H -0.0819 0.2303 0.1778 0.064 Uiso 1 calc R A 1 H41C H 0.0481 0.1983 0.1350 0.064 Uiso 1 calc R A 1 C51A C 0.3322(6) 0.2062(4) 0.2248(3) 0.0343(13) Uani 1 d . A 1 H51A H 0.4204 0.1855 0.2494 0.041 Uiso 1 calc R A 1 H51B H 0.3248 0.1722 0.1765 0.041 Uiso 1 calc R A 1 C52A C 0.2151(6) 0.1670(5) 0.2697(3) 0.0323(13) Uani 1 d . A 1 O53A O 0.2151(5) 0.0782(3) 0.2936(2) 0.0391(10) Uani 1 d . A 1 O54A O 0.1128(4) 0.2337(3) 0.2773(2) 0.0340(9) Uani 1 d . A 1 C61A C 0.0023(7) 0.5473(5) 0.3015(4) 0.0389(14) Uani 1 d . A 1 H61A H 0.0228 0.5769 0.3506 0.047 Uiso 1 calc R A 1 H61B H -0.0887 0.5728 0.2834 0.047 Uiso 1 calc R A 1 C62A C 0.1100(6) 0.5867(5) 0.2505(3) 0.0376(14) Uani 1 d . A 1 O63A O 0.1150(5) 0.6789(3) 0.2343(3) 0.0512(12) Uani 1 d . A 1 O64A O 0.1912(4) 0.5151(3) 0.2241(2) 0.0353(9) Uani 1 d . A 1 CoB Co 1.33623(8) 1.12556(6) 0.69448(4) 0.0275(2) Uani 1 d . B 2 N1B N 1.2959(6) 1.1325(4) 0.8038(3) 0.0372(12) Uani 1 d . B 2 C2B C 1.4218(9) 1.1058(7) 0.8536(4) 0.067(2) Uani 1 d . B 2 H2B1 H 1.4484 1.0332 0.8444 0.081 Uiso 1 calc R B 2 H2B2 H 1.3979 1.1110 0.9048 0.081 Uiso 1 calc R B 2 C3B C 1.5491(7) 1.1799(6) 0.8422(4) 0.0507(17) Uani 1 d . B 2 H3B1 H 1.5180 1.2528 0.8399 0.061 Uiso 1 calc R B 2 H3B2 H 1.6167 1.1733 0.8841 0.061 Uiso 1 calc R B 2 C4B C 1.6166(6) 1.1519(5) 0.7720(3) 0.0394(14) Uani 1 d . B 2 H4B1 H 1.6331 1.0763 0.7710 0.047 Uiso 1 calc R B 2 H4B2 H 1.7062 1.1870 0.7723 0.047 Uiso 1 calc R B 2 N5B N 1.5309(5) 1.1824(4) 0.7027(3) 0.0309(10) Uani 1 d . B 2 C6B C 1.6014(6) 1.1358(5) 0.6381(3) 0.0352(13) Uani 1 d . B 2 H6B1 H 1.6346 1.0652 0.6501 0.042 Uiso 1 calc R B 2 H6B2 H 1.6805 1.1790 0.6271 0.042 Uiso 1 calc R B 2 C7B C 1.4978(6) 1.1317(5) 0.5717(3) 0.0358(13) Uani 1 d . B 2 N8B N 1.3686(5) 1.1198(4) 0.5937(2) 0.0297(10) Uani 1 d . B 2 C9B C 1.2584(6) 1.1107(4) 0.5437(3) 0.0332(13) Uani 1 d . B 2 C10B C 1.1238(6) 1.1076(5) 0.5812(3) 0.0401(14) Uani 1 d . B 2 H10C H 1.0841 1.1780 0.5828 0.048 Uiso 1 calc R B 2 H10D H 1.0578 1.0619 0.5536 0.048 Uiso 1 calc R B 2 N11B N 1.1516(5) 1.0666(4) 0.6582(3) 0.0307(10) Uani 1 d . B 2 C12B C 1.0326(6) 1.1021(5) 0.7030(4) 0.0414(15) Uani 1 d . B 2 H12C H 1.0276 1.1787 0.7017 0.050 Uiso 1 calc R B 2 H12D H 0.9464 1.0749 0.6795 0.050 Uiso 1 calc R B 2 C13B C 1.0440(7) 1.0674(6) 0.7827(4) 0.0497(17) Uani 1 d . B 2 H13C H 0.9923 1.0019 0.7856 0.060 Uiso 1 calc R B 2 H13D H 0.9970 1.1198 0.8113 0.060 Uiso 1 calc R B 2 C14B C 1.1900(9) 1.0494(7) 0.8214(4) 0.061(2) Uani 1 d . B 2 H14C H 1.1820 1.0483 0.8746 0.073 Uiso 1 calc R B 2 H14D H 1.2238 0.9807 0.8068 0.073 Uiso 1 calc R B 2 C21B C 1.5234(7) 1.1358(5) 0.4980(3) 0.0367(13) Uani 1 d . B 2 H21B H 1.6129 1.1460 0.4831 0.044 Uiso 1 calc R B 2 C22B C 1.4107(7) 1.1242(5) 0.4463(3) 0.0409(15) Uani 1 d . B 2 H22B H 1.4249 1.1263 0.3960 0.049 Uiso 1 calc R B 2 C23B C 1.2794(8) 1.1098(5) 0.4687(3) 0.0446(16) Uani 1 d . B 2 H23B H 1.2050 1.0994 0.4339 0.054 Uiso 1 calc R B 2 C41B C 1.2376(9) 1.2360(7) 0.8306(5) 0.067(2) Uani 1 d . B 2 H41D H 1.1551 1.2537 0.8006 0.081 Uiso 1 calc R B 2 H41E H 1.3056 1.2909 0.8271 0.081 Uiso 1 calc R B 2 H41F H 1.2152 1.2289 0.8813 0.081 Uiso 1 calc R B 2 C51B C 1.5206(6) 1.2994(4) 0.6950(4) 0.0357(13) Uani 1 d . B 2 H51C H 1.5776 1.3219 0.6558 0.043 Uiso 1 calc R B 2 H51D H 1.5570 1.3325 0.7408 0.043 Uiso 1 calc R B 2 C52B C 1.3711(6) 1.3367(5) 0.6774(3) 0.0342(13) Uani 1 d . B 2 O53B O 1.3498(5) 1.4286(3) 0.6647(3) 0.0518(12) Uani 1 d . B 2 O54B O 1.2746(4) 1.2656(3) 0.6794(2) 0.0330(9) Uani 1 d . B 2 C61B C 1.1662(6) 0.9493(4) 0.6576(3) 0.0358(13) Uani 1 d . B 2 H61C H 1.1476 0.9235 0.6073 0.043 Uiso 1 calc R B 2 H61D H 1.0970 0.9188 0.6878 0.043 Uiso 1 calc R B 2 C62B C 1.3093(7) 0.9122(5) 0.6864(3) 0.0375(14) Uani 1 d . B 2 O63B O 1.3355(5) 0.8185(3) 0.6897(3) 0.0606(14) Uani 1 d . B 2 O64B O 1.3996(4) 0.9854(3) 0.7055(2) 0.0351(9) Uani 1 d . B 2 BrA Br 0.7534(3) 0.9769(3) 0.94708(19) 0.0840(6) Uiso 0.40 d P C 1 BrB Br 0.807(3) 1.0721(19) 0.9857(13) 0.170(5) Uiso 0.10 d P . 2 BrC Br 0.7138(3) 0.9565(3) 0.95337(19) 0.0840(6) Uiso 0.40 d P D 3 BrD Br 0.829(2) 0.9857(18) 0.8931(13) 0.170(5) Uiso 0.10 d P E 4 N100 N 0.8511(6) 1.2918(5) 0.5278(3) 0.0443(13) Uani 1 d . . . O101 O 0.8496(7) 1.2042(6) 0.4969(4) 0.098(2) Uani 1 d . . . O102 O 0.9661(6) 1.3332(5) 0.5414(3) 0.0687(16) Uani 1 d . . . O103 O 0.7483(7) 1.3338(6) 0.5468(5) 0.097(2) Uani 1 d . . . O200 O 0.6373(7) 0.3595(5) 1.0038(3) 0.0696(15) Uani 1 d D . . H201 H 0.609(8) 0.302(3) 1.022(5) 0.084 Uiso 1 d D . . H202 H 0.707(6) 0.347(6) 0.979(4) 0.084 Uiso 1 d D . . O300 O 0.8672(9) 0.3174(7) 0.9231(4) 0.101(2) Uani 1 d D . . H301 H 0.866(13) 0.314(8) 0.8761(8) 0.121 Uiso 1 d D . . H302 H 0.881(14) 0.256(4) 0.941(5) 0.121 Uiso 1 d D . . O400 O 0.4108(8) 0.4458(5) 0.9125(4) 0.085(2) Uani 1 d D . . H401 H 0.380(10) 0.498(5) 0.936(4) 0.102 Uiso 1 d D . . H402 H 0.472(8) 0.413(6) 0.940(4) 0.102 Uiso 1 d D . . O500 O 0.5762(11) 0.1590(6) 1.0562(5) 0.114(3) Uani 1 d D . . H501 H 0.633(8) 0.114(7) 1.040(7) 0.136 Uiso 1 d D . . H502 H 0.495(4) 0.133(8) 1.053(8) 0.136 Uiso 1 d D . . O600 O 0.9842(16) 0.1415(10) 0.9657(7) 0.164(4) Uani 1 d D . . H601 H 1.035(15) 0.123(13) 1.004(6) 0.197 Uiso 1 d D . . H602 H 0.923(16) 0.094(11) 0.956(10) 0.197 Uiso 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 CoA 0.0283(4) 0.0287(4) 0.0285(4) 0.0016(3) 0.0054(3) 0.0026(3) N1A 0.035(3) 0.043(3) 0.037(3) 0.001(2) 0.002(2) 0.000(2) C2A 0.072(5) 0.056(4) 0.034(4) 0.008(3) 0.001(3) 0.000(4) C3A 0.063(5) 0.067(5) 0.029(3) 0.002(3) 0.010(3) -0.002(4) C4A 0.046(4) 0.052(4) 0.040(4) 0.007(3) 0.022(3) 0.000(3) N5A 0.030(3) 0.036(3) 0.033(3) 0.004(2) 0.0085(19) -0.001(2) C6A 0.030(3) 0.032(3) 0.046(4) 0.001(2) 0.007(2) -0.002(3) C7A 0.033(3) 0.027(3) 0.044(3) 0.004(2) 0.005(2) -0.003(3) N8A 0.037(3) 0.032(3) 0.027(2) 0.0002(19) 0.0054(19) 0.004(2) C9A 0.049(4) 0.027(3) 0.036(3) 0.003(2) 0.008(3) -0.001(3) C10A 0.045(4) 0.041(4) 0.038(3) 0.004(3) 0.016(3) 0.003(3) N11A 0.026(2) 0.035(3) 0.038(3) 0.001(2) 0.0114(19) 0.000(2) C12A 0.028(3) 0.038(4) 0.059(4) 0.002(3) 0.013(3) 0.004(3) C13A 0.036(4) 0.073(5) 0.060(5) -0.003(4) 0.003(3) 0.005(4) C14A 0.043(4) 0.055(4) 0.047(4) 0.005(3) -0.007(3) 0.012(3) C21A 0.038(4) 0.040(4) 0.057(4) 0.005(3) -0.007(3) -0.005(3) C22A 0.066(5) 0.041(4) 0.035(4) 0.003(3) -0.013(3) 0.000(3) C23A 0.067(5) 0.043(4) 0.026(3) -0.001(2) 0.000(3) 0.001(3) C41A 0.060(5) 0.041(4) 0.058(5) -0.005(3) -0.008(3) -0.009(4) C51A 0.039(3) 0.029(3) 0.035(3) -0.004(2) 0.006(2) 0.005(3) C52A 0.036(3) 0.032(3) 0.028(3) -0.004(2) -0.002(2) 0.000(3) O53A 0.047(3) 0.030(2) 0.041(2) 0.0050(17) 0.0045(18) 0.001(2) O54A 0.033(2) 0.032(2) 0.038(2) 0.0036(16) 0.0079(16) 0.0021(19) C61A 0.041(3) 0.030(3) 0.046(4) 0.000(2) 0.012(3) 0.008(3) C62A 0.039(3) 0.027(3) 0.046(4) 0.000(2) 0.002(3) -0.002(3) O63A 0.059(3) 0.028(2) 0.069(3) 0.007(2) 0.018(2) 0.000(2) O64A 0.035(2) 0.029(2) 0.043(2) 0.0008(16) 0.0097(17) 0.0009(18) CoB 0.0291(4) 0.0245(4) 0.0283(4) -0.0023(3) -0.0016(3) 0.0003(3) N1B 0.048(3) 0.032(3) 0.031(3) -0.002(2) -0.003(2) -0.003(2) C2B 0.083(6) 0.082(6) 0.035(4) 0.009(4) -0.006(4) 0.012(5) C3B 0.047(4) 0.065(5) 0.037(4) -0.008(3) -0.014(3) 0.001(4) C4B 0.037(3) 0.035(3) 0.045(4) 0.002(3) -0.010(3) -0.005(3) N5B 0.031(2) 0.025(2) 0.036(3) -0.0041(18) -0.0044(19) -0.001(2) C6B 0.034(3) 0.034(3) 0.038(3) -0.001(2) 0.005(2) 0.002(3) C7B 0.038(3) 0.030(3) 0.039(3) -0.001(2) 0.002(2) 0.005(3) N8B 0.031(3) 0.026(2) 0.031(2) -0.0036(18) -0.0030(19) 0.003(2) C9B 0.039(3) 0.025(3) 0.035(3) -0.001(2) -0.005(2) -0.001(3) C10B 0.032(3) 0.047(4) 0.040(3) 0.001(3) -0.011(3) -0.003(3) N11B 0.026(2) 0.028(2) 0.039(3) -0.0056(19) 0.0009(19) 0.000(2) C12B 0.029(3) 0.040(4) 0.055(4) -0.005(3) 0.004(3) 0.001(3) C13B 0.039(4) 0.060(5) 0.051(4) -0.011(3) 0.009(3) -0.006(3) C14B 0.068(5) 0.067(5) 0.049(4) 0.000(4) 0.012(4) -0.013(4) C21B 0.040(3) 0.031(3) 0.040(3) 0.003(2) 0.013(3) 0.005(3) C22B 0.058(4) 0.039(3) 0.026(3) 0.000(2) 0.008(3) 0.000(3) C23B 0.061(4) 0.039(4) 0.031(3) -0.002(3) -0.015(3) -0.002(3) C41B 0.078(6) 0.059(5) 0.066(5) -0.013(4) 0.017(4) 0.016(5) C51B 0.036(3) 0.024(3) 0.047(4) -0.003(2) -0.002(3) -0.003(3) C52B 0.039(3) 0.029(3) 0.036(3) -0.007(2) 0.004(2) 0.004(3) O53B 0.050(3) 0.029(2) 0.078(4) 0.006(2) 0.011(2) 0.005(2) O54B 0.031(2) 0.029(2) 0.038(2) -0.0033(16) 0.0009(16) 0.0049(18) C61B 0.035(3) 0.027(3) 0.045(4) -0.009(2) 0.002(3) -0.006(3) C62B 0.040(3) 0.026(3) 0.046(4) 0.000(2) 0.000(3) -0.003(3) O63B 0.051(3) 0.024(2) 0.104(4) -0.004(2) -0.014(3) 0.002(2) O64B 0.033(2) 0.025(2) 0.046(2) -0.0015(16) -0.0029(17) 0.0028(18) N100 0.040(3) 0.053(4) 0.040(3) 0.006(2) 0.007(2) -0.005(3) O101 0.066(4) 0.099(5) 0.125(6) -0.058(5) -0.022(4) 0.012(4) O102 0.058(3) 0.092(4) 0.056(3) 0.000(3) 0.000(3) -0.018(3) O103 0.066(4) 0.073(5) 0.155(7) -0.007(4) 0.028(4) -0.002(4) O200 0.075(4) 0.067(4) 0.067(4) -0.010(3) 0.005(3) 0.013(3) O300 0.113(6) 0.131(7) 0.059(4) -0.002(4) 0.012(4) -0.010(6) O400 0.106(5) 0.062(4) 0.082(4) -0.011(3) -0.026(4) -0.002(4) O500 0.153(8) 0.082(5) 0.111(6) 0.003(4) 0.050(6) 0.021(6) O600 0.192(13) 0.170(11) 0.128(9) -0.005(8) -0.014(8) 0.047(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag CoA N8A 1.882(5) . ? CoA O64A 1.891(4) . ? CoA O54A 1.892(4) . ? CoA N11A 1.989(5) . ? CoA N5A 2.002(5) . ? CoA N1A 2.043(5) . ? N1A C2A 1.484(9) . ? N1A C41A 1.493(8) . ? N1A C14A 1.533(8) . ? C2A C3A 1.532(10) . ? C2A H2A1 0.9700 . ? C2A H2A2 0.9700 . ? C3A C4A 1.513(10) . ? C3A H3A1 0.9700 . ? C3A H3A2 0.9700 . ? C4A N5A 1.511(8) . ? C4A H4A1 0.9700 . ? C4A H4A2 0.9700 . ? N5A C51A 1.496(7) . ? N5A C6A 1.500(8) . ? C6A C7A 1.477(9) . ? C6A H6A1 0.9700 . ? C6A H6A2 0.9700 . ? C7A N8A 1.342(8) . ? C7A C21A 1.392(9) . ? N8A C9A 1.356(8) . ? C9A C23A 1.372(9) . ? C9A C10A 1.498(9) . ? C10A N11A 1.495(8) . ? C10A H10A 0.9700 . ? C10A H10B 0.9700 . ? N11A C61A 1.488(8) . ? N11A C12A 1.503(8) . ? C12A C13A 1.499(10) . ? C12A H12A 0.9700 . ? C12A H12B 0.9700 . ? C13A C14A 1.527(10) . ? C13A H13A 0.9700 . ? C13A H13B 0.9700 . ? C14A H14A 0.9700 . ? C14A H14B 0.9700 . ? C21A C22A 1.381(10) . ? C21A H21A 0.9300 . ? C22A C23A 1.387(10) . ? C22A H22A 0.9300 . ? C23A H23A 0.9300 . ? C41A H41A 0.9600 . ? C41A H41B 0.9600 . ? C41A H41C 0.9600 . ? C51A C52A 1.518(8) . ? C51A H51A 0.9700 . ? C51A H51B 0.9700 . ? C52A O53A 1.206(7) . ? C52A O54A 1.312(7) . ? C61A C62A 1.519(9) . ? C61A H61A 0.9700 . ? C61A H61B 0.9700 . ? C62A O63A 1.206(7) . ? C62A O64A 1.306(7) . ? CoB N8B 1.870(5) . ? CoB O64B 1.883(4) . ? CoB O54B 1.884(4) . ? CoB N11B 1.997(5) . ? CoB N5B 2.005(5) . ? CoB N1B 2.041(5) . ? N1B C2B 1.501(9) . ? N1B C14B 1.515(9) . ? N1B C41B 1.515(9) . ? C2B C3B 1.570(12) . ? C2B H2B1 0.9700 . ? C2B H2B2 0.9700 . ? C3B C4B 1.505(10) . ? C3B H3B1 0.9700 . ? C3B H3B2 0.9700 . ? C4B N5B 1.506(7) . ? C4B H4B1 0.9700 . ? C4B H4B2 0.9700 . ? N5B C51B 1.490(7) . ? N5B C6B 1.507(7) . ? C6B C7B 1.509(8) . ? C6B H6B1 0.9700 . ? C6B H6B2 0.9700 . ? C7B N8B 1.340(8) . ? C7B C21B 1.373(9) . ? N8B C9B 1.353(7) . ? C9B C23B 1.385(9) . ? C9B C10B 1.503(9) . ? C10B N11B 1.497(8) . ? C10B H10C 0.9700 . ? C10B H10D 0.9700 . ? N11B C61B 1.492(7) . ? N11B C12B 1.513(8) . ? C12B C13B 1.505(10) . ? C12B H12C 0.9700 . ? C12B H12D 0.9700 . ? C13B C14B 1.547(11) . ? C13B H13C 0.9700 . ? C13B H13D 0.9700 . ? C14B H14C 0.9700 . ? C14B H14D 0.9700 . ? C21B C22B 1.392(9) . ? C21B H21B 0.9300 . ? C22B C23B 1.366(10) . ? C22B H22B 0.9300 . ? C23B H23B 0.9300 . ? C41B H41D 0.9600 . ? C41B H41E 0.9600 . ? C41B H41F 0.9600 . ? C51B C52B 1.529(8) . ? C51B H51C 0.9700 . ? C51B H51D 0.9700 . ? C52B O53B 1.202(7) . ? C52B O54B 1.297(7) . ? C61B C62B 1.516(9) . ? C61B H61C 0.9700 . ? C61B H61D 0.9700 . ? C62B O63B 1.213(7) . ? C62B O64B 1.300(7) . ? BrB O600 1.98(3) 1_565 ? N100 O103 1.194(8) . ? N100 O102 1.235(8) . ? N100 O101 1.239(8) . ? O200 H201 0.848(10) . ? O200 H202 0.849(10) . ? O300 H301 0.851(10) . ? O300 H302 0.851(10) . ? O400 H401 0.848(10) . ? O400 H402 0.851(10) . ? O500 H501 0.850(10) . ? O500 H502 0.852(11) . ? O600 BrB 1.98(3) 1_545 ? O600 H601 0.853(10) . ? O600 H602 0.855(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N8A CoA O64A 90.5(2) . . ? N8A CoA O54A 87.2(2) . . ? O64A CoA O54A 177.62(18) . . ? N8A CoA N11A 82.6(2) . . ? O64A CoA N11A 88.14(19) . . ? O54A CoA N11A 91.76(19) . . ? N8A CoA N5A 82.9(2) . . ? O64A CoA N5A 91.38(19) . . ? O54A CoA N5A 88.12(18) . . ? N11A CoA N5A 165.5(2) . . ? N8A CoA N1A 178.9(2) . . ? O64A CoA N1A 90.3(2) . . ? O54A CoA N1A 92.0(2) . . ? N11A CoA N1A 96.6(2) . . ? N5A CoA N1A 97.8(2) . . ? C2A N1A C41A 109.3(6) . . ? C2A N1A C14A 103.9(5) . . ? C41A N1A C14A 108.1(5) . . ? C2A N1A CoA 111.4(4) . . ? C41A N1A CoA 114.6(4) . . ? C14A N1A CoA 108.9(4) . . ? N1A C2A C3A 115.2(6) . . ? N1A C2A H2A1 108.5 . . ? C3A C2A H2A1 108.5 . . ? N1A C2A H2A2 108.5 . . ? C3A C2A H2A2 108.5 . . ? H2A1 C2A H2A2 107.5 . . ? C4A C3A C2A 112.4(6) . . ? C4A C3A H3A1 109.1 . . ? C2A C3A H3A1 109.1 . . ? C4A C3A H3A2 109.1 . . ? C2A C3A H3A2 109.1 . . ? H3A1 C3A H3A2 107.9 . . ? N5A C4A C3A 114.3(5) . . ? N5A C4A H4A1 108.7 . . ? C3A C4A H4A1 108.7 . . ? N5A C4A H4A2 108.7 . . ? C3A C4A H4A2 108.7 . . ? H4A1 C4A H4A2 107.6 . . ? C51A N5A C6A 109.8(4) . . ? C51A N5A C4A 111.2(5) . . ? C6A N5A C4A 107.7(5) . . ? C51A N5A CoA 106.0(3) . . ? C6A N5A CoA 105.9(3) . . ? C4A N5A CoA 116.0(4) . . ? C7A C6A N5A 110.1(5) . . ? C7A C6A H6A1 109.6 . . ? N5A C6A H6A1 109.6 . . ? C7A C6A H6A2 109.6 . . ? N5A C6A H6A2 109.6 . . ? H6A1 C6A H6A2 108.1 . . ? N8A C7A C21A 118.8(6) . . ? N8A C7A C6A 111.7(5) . . ? C21A C7A C6A 129.5(6) . . ? C7A N8A C9A 122.6(5) . . ? C7A N8A CoA 118.8(4) . . ? C9A N8A CoA 118.4(4) . . ? N8A C9A C23A 119.9(6) . . ? N8A C9A C10A 111.0(5) . . ? C23A C9A C10A 128.9(6) . . ? N11A C10A C9A 109.8(5) . . ? N11A C10A H10A 109.7 . . ? C9A C10A H10A 109.7 . . ? N11A C10A H10B 109.7 . . ? C9A C10A H10B 109.7 . . ? H10A C10A H10B 108.2 . . ? C61A N11A C10A 110.5(5) . . ? C61A N11A C12A 112.7(5) . . ? C10A N11A C12A 107.4(4) . . ? C61A N11A CoA 106.7(3) . . ? C10A N11A CoA 106.2(4) . . ? C12A N11A CoA 113.0(4) . . ? C13A C12A N11A 114.5(5) . . ? C13A C12A H12A 108.6 . . ? N11A C12A H12A 108.6 . . ? C13A C12A H12B 108.6 . . ? N11A C12A H12B 108.6 . . ? H12A C12A H12B 107.6 . . ? C12A C13A C14A 118.3(6) . . ? C12A C13A H13A 107.7 . . ? C14A C13A H13A 107.7 . . ? C12A C13A H13B 107.7 . . ? C14A C13A H13B 107.7 . . ? H13A C13A H13B 107.1 . . ? C13A C14A N1A 114.2(6) . . ? C13A C14A H14A 108.7 . . ? N1A C14A H14A 108.7 . . ? C13A C14A H14B 108.7 . . ? N1A C14A H14B 108.7 . . ? H14A C14A H14B 107.6 . . ? C22A C21A C7A 119.6(6) . . ? C22A C21A H21A 120.2 . . ? C7A C21A H21A 120.2 . . ? C21A C22A C23A 120.0(6) . . ? C21A C22A H22A 120.0 . . ? C23A C22A H22A 120.0 . . ? C9A C23A C22A 119.0(6) . . ? C9A C23A H23A 120.5 . . ? C22A C23A H23A 120.5 . . ? N5A C51A C52A 113.3(4) . . ? N5A C51A H51A 108.9 . . ? C52A C51A H51A 108.9 . . ? N5A C51A H51B 108.9 . . ? C52A C51A H51B 108.9 . . ? H51A C51A H51B 107.7 . . ? O53A C52A O54A 123.0(6) . . ? O53A C52A C51A 121.1(5) . . ? O54A C52A C51A 115.8(5) . . ? C52A O54A CoA 114.9(4) . . ? N11A C61A C62A 113.4(5) . . ? N11A C61A H61A 108.9 . . ? C62A C61A H61A 108.9 . . ? N11A C61A H61B 108.9 . . ? C62A C61A H61B 108.9 . . ? H61A C61A H61B 107.7 . . ? O63A C62A O64A 123.1(6) . . ? O63A C62A C61A 120.6(6) . . ? O64A C62A C61A 116.3(5) . . ? C62A O64A CoA 115.1(4) . . ? N8B CoB O64B 89.83(19) . . ? N8B CoB O54B 87.85(18) . . ? O64B CoB O54B 177.67(17) . . ? N8B CoB N11B 82.6(2) . . ? O64B CoB N11B 87.69(19) . . ? O54B CoB N11B 92.12(19) . . ? N8B CoB N5B 82.4(2) . . ? O64B CoB N5B 91.99(19) . . ? O54B CoB N5B 87.59(19) . . ? N11B CoB N5B 165.0(2) . . ? N8B CoB N1B 178.6(2) . . ? O64B CoB N1B 90.84(19) . . ? O54B CoB N1B 91.49(19) . . ? N11B CoB N1B 96.3(2) . . ? N5B CoB N1B 98.7(2) . . ? C2B N1B C14B 104.1(6) . . ? C2B N1B C41B 107.8(6) . . ? C14B N1B C41B 105.2(6) . . ? C2B N1B CoB 112.0(4) . . ? C14B N1B CoB 110.6(4) . . ? C41B N1B CoB 116.2(4) . . ? N1B C2B C3B 113.0(6) . . ? N1B C2B H2B1 109.0 . . ? C3B C2B H2B1 109.0 . . ? N1B C2B H2B2 109.0 . . ? C3B C2B H2B2 109.0 . . ? H2B1 C2B H2B2 107.8 . . ? C4B C3B C2B 111.0(6) . . ? C4B C3B H3B1 109.4 . . ? C2B C3B H3B1 109.4 . . ? C4B C3B H3B2 109.4 . . ? C2B C3B H3B2 109.4 . . ? H3B1 C3B H3B2 108.0 . . ? C3B C4B N5B 113.4(5) . . ? C3B C4B H4B1 108.9 . . ? N5B C4B H4B1 108.9 . . ? C3B C4B H4B2 108.9 . . ? N5B C4B H4B2 108.9 . . ? H4B1 C4B H4B2 107.7 . . ? C51B N5B C4B 111.5(5) . . ? C51B N5B C6B 110.0(5) . . ? C4B N5B C6B 107.1(5) . . ? C51B N5B CoB 107.0(3) . . ? C4B N5B CoB 115.3(4) . . ? C6B N5B CoB 105.8(3) . . ? N5B C6B C7B 108.6(5) . . ? N5B C6B H6B1 110.0 . . ? C7B C6B H6B1 110.0 . . ? N5B C6B H6B2 110.0 . . ? C7B C6B H6B2 110.0 . . ? H6B1 C6B H6B2 108.3 . . ? N8B C7B C21B 121.5(6) . . ? N8B C7B C6B 110.3(5) . . ? C21B C7B C6B 128.2(6) . . ? C7B N8B C9B 121.0(5) . . ? C7B N8B CoB 120.2(4) . . ? C9B N8B CoB 118.6(4) . . ? N8B C9B C23B 119.7(6) . . ? N8B C9B C10B 111.4(5) . . ? C23B C9B C10B 128.9(5) . . ? N11B C10B C9B 108.8(5) . . ? N11B C10B H10C 109.9 . . ? C9B C10B H10C 109.9 . . ? N11B C10B H10D 109.9 . . ? C9B C10B H10D 109.9 . . ? H10C C10B H10D 108.3 . . ? C61B N11B C10B 110.7(5) . . ? C61B N11B C12B 111.8(5) . . ? C10B N11B C12B 107.4(5) . . ? C61B N11B CoB 106.9(3) . . ? C10B N11B CoB 106.0(3) . . ? C12B N11B CoB 113.9(4) . . ? C13B C12B N11B 114.5(5) . . ? C13B C12B H12C 108.6 . . ? N11B C12B H12C 108.6 . . ? C13B C12B H12D 108.6 . . ? N11B C12B H12D 108.6 . . ? H12C C12B H12D 107.6 . . ? C12B C13B C14B 118.9(6) . . ? C12B C13B H13C 107.6 . . ? C14B C13B H13C 107.6 . . ? C12B C13B H13D 107.6 . . ? C14B C13B H13D 107.6 . . ? H13C C13B H13D 107.0 . . ? N1B C14B C13B 114.0(6) . . ? N1B C14B H14C 108.8 . . ? C13B C14B H14C 108.8 . . ? N1B C14B H14D 108.8 . . ? C13B C14B H14D 108.8 . . ? H14C C14B H14D 107.7 . . ? C7B C21B C22B 117.7(6) . . ? C7B C21B H21B 121.1 . . ? C22B C21B H21B 121.1 . . ? C23B C22B C21B 120.8(6) . . ? C23B C22B H22B 119.6 . . ? C21B C22B H22B 119.6 . . ? C22B C23B C9B 119.2(6) . . ? C22B C23B H23B 120.4 . . ? C9B C23B H23B 120.4 . . ? N1B C41B H41D 109.5 . . ? N1B C41B H41E 109.5 . . ? H41D C41B H41E 109.5 . . ? N1B C41B H41F 109.5 . . ? H41D C41B H41F 109.5 . . ? H41E C41B H41F 109.5 . . ? N5B C51B C52B 112.5(5) . . ? N5B C51B H51C 109.1 . . ? C52B C51B H51C 109.1 . . ? N5B C51B H51D 109.1 . . ? C52B C51B H51D 109.1 . . ? H51C C51B H51D 107.8 . . ? O53B C52B O54B 124.3(6) . . ? O53B C52B C51B 119.1(5) . . ? O54B C52B C51B 116.5(5) . . ? C52B O54B CoB 115.9(3) . . ? N11B C61B C62B 113.0(5) . . ? N11B C61B H61C 109.0 . . ? C62B C61B H61C 109.0 . . ? N11B C61B H61D 109.0 . . ? C62B C61B H61D 109.0 . . ? H61C C61B H61D 107.8 . . ? O63B C62B O64B 123.2(6) . . ? O63B C62B C61B 120.2(5) . . ? O64B C62B C61B 116.5(5) . . ? C62B O64B CoB 115.8(4) . . ? O103 N100 O102 120.4(7) . . ? O103 N100 O101 122.7(7) . . ? O102 N100 O101 116.8(6) . . ? H201 O200 H202 109.7(18) . . ? H301 O300 H302 109.1(18) . . ? H401 O400 H402 109.8(19) . . ? H501 O500 H502 109.1(19) . . ? BrB O600 H601 101(10) 1_545 . ? BrB O600 H602 30(10) 1_545 . ? H601 O600 H602 108.7(18) . . ? 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 C9A N8A C7A C6A -179.8(5) . . . . ? N8A C7A C6A N5A -27.2(7) . . . . ? C7A C6A N5A C4A 159.2(5) . . . . ? C6A N5A C4A C3A -170.7(5) . . . . ? N5A C4A C3A C2A 66.4(8) . . . . ? C4A C3A C2A N1A -73.0(8) . . . . ? C3A C2A N1A C14A 176.8(6) . . . . ? C2A N1A C14A C13A 174.5(6) . . . . ? N1A C14A C13A C12A 43.0(10) . . . . ? C14A C13A C12A N11A 29.0(10) . . . . ? C13A C12A N11A C10A 178.4(6) . . . . ? C12A N11A C10A C9A 157.1(5) . . . . ? N11A C10A C9A N8A -24.0(7) . . . . ? C10A C9A N8A C7A -175.5(5) . . . . ? C9A N8A C7A C6A -179.8(5) . . . . ? C9B N8B C7B C6B -177.9(5) . . . . ? N8B C7B C6B N5B -29.8(7) . . . . ? C7B C6B N5B C4B 161.0(5) . . . . ? C6B N5B C4B C3B -172.1(5) . . . . ? N5B C4B C3B C2B 71.8(7) . . . . ? C4B C3B C2B N1B -75.4(8) . . . . ? C3B C2B N1B C14B 177.5(6) . . . . ? C2B N1B C14B C13B 173.7(6) . . . . ? N1B C14B C13B C12B 41.7(9) . . . . ? C14B C13B C12B N11B 28.3(9) . . . . ? C13B C12B N11B C10B 180.0(5) . . . . ? C12B N11B C10B C9B 158.9(5) . . . . ? N11B C10B C9B N8B -25.6(7) . . . . ? C10B C9B N8B C7B -175.1(5) . . . . ? C9B N8B C7B C6B -177.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.815 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.815 _refine_diff_density_max 1.072 _refine_diff_density_min -1.649 _refine_diff_density_rms 0.115 #=== END data_complex2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety [Ni(HL1)Br.4H2O _chemical_formula_sum 'C18 H34 Br N4 Ni O8' _chemical_formula_weight 573.11 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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n 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 11.966(12) _cell_length_b 14.529(17) _cell_length_c 14.196(16) _cell_angle_alpha 90.00 _cell_angle_beta 93.009(10) _cell_angle_gamma 90.00 _cell_volume 2465(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.545 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1188 _exptl_absorpt_coefficient_mu 2.457 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7441 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.0645 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 26.12 _reflns_number_total 4300 _reflns_number_gt 2953 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1843P)^2^+2.5480P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0009(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4300 _refine_ls_number_parameters 319 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1350 _refine_ls_R_factor_gt 0.0965 _refine_ls_wR_factor_ref 0.2946 _refine_ls_wR_factor_gt 0.2628 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.339 _refine_ls_shift/su_mean 0.017 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.84650(7) 0.21858(6) 0.36992(6) 0.0461(4) Uani 1 d . . . N8 N 0.8618(5) 0.3532(4) 0.3828(4) 0.0526(14) Uani 1 d . . . C9 C 0.8014(7) 0.3967(6) 0.4453(5) 0.062(2) Uani 1 d . . . C10 C 0.7249(8) 0.3338(7) 0.4961(6) 0.074(3) Uani 1 d . . . H10A H 0.7605 0.3161 0.5563 0.089 Uiso 1 calc R . . H10B H 0.6562 0.3660 0.5081 0.089 Uiso 1 calc R . . N11 N 0.6981(6) 0.2489(6) 0.4386(5) 0.0656(18) Uani 1 d . . . C12 C 0.6686(9) 0.1722(10) 0.5034(7) 0.103(4) Uani 1 d . . . H12A H 0.5996 0.1874 0.5329 0.123 Uiso 1 calc R A 1 H12B H 0.7271 0.1659 0.5529 0.123 Uiso 1 calc R A 1 N1 N 0.8282(8) 0.0768(5) 0.3582(6) 0.086(3) Uani 0.558(17) d P B 1 C2 C 0.8666(16) 0.0504(13) 0.2652(13) 0.079(5) Uiso 0.558(17) d P B 1 H2A H 0.8252 0.0851 0.2165 0.095 Uiso 0.558(17) calc PR B 1 H2B H 0.8516 -0.0145 0.2544 0.095 Uiso 0.558(17) calc PR B 1 C3 C 0.9968(13) 0.0693(10) 0.2583(13) 0.137(6) Uani 0.558(17) d P B 1 H3A H 1.0355 0.0599 0.3194 0.165 Uiso 0.558(17) calc PR B 1 H3B H 1.0280 0.0274 0.2135 0.165 Uiso 0.558(17) calc PR B 1 C13 C 0.6536(13) 0.0777(10) 0.4492(13) 0.142(7) Uani 0.558(17) d P B 1 H13A H 0.6810 0.0306 0.4930 0.170 Uiso 0.558(17) calc PR B 1 H13B H 0.5735 0.0681 0.4403 0.170 Uiso 0.558(17) calc PR B 1 C14 C 0.7005(16) 0.0552(13) 0.3584(13) 0.080(5) Uiso 0.558(17) d P B 1 H14A H 0.6613 0.0902 0.3087 0.096 Uiso 0.558(17) calc PR B 1 H14B H 0.6886 -0.0097 0.3451 0.096 Uiso 0.558(17) calc PR B 1 C41 C 0.8787(17) 0.0206(14) 0.4368(13) 0.086(6) Uiso 0.558(17) d P B 1 H41A H 0.8563 -0.0425 0.4285 0.103 Uiso 0.558(17) calc PR B 1 H41B H 0.8537 0.0431 0.4957 0.103 Uiso 0.558(17) calc PR B 1 H41C H 0.9588 0.0248 0.4369 0.103 Uiso 0.558(17) calc PR B 1 N1B N 0.8282(8) 0.0768(5) 0.3582(6) 0.086(3) Uani 0.442(17) d P B 2 C2B C 0.946(2) 0.039(2) 0.3595(19) 0.097(8) Uiso 0.442(17) d P B 2 H2E H 0.9452 -0.0270 0.3659 0.116 Uiso 0.442(17) calc PR B 2 H2F H 0.9907 0.0653 0.4118 0.116 Uiso 0.442(17) calc PR B 2 C3B C 0.9968(13) 0.0693(10) 0.2583(13) 0.137(6) Uani 0.442(17) d P B 2 H3G H 1.0701 0.0409 0.2571 0.165 Uiso 0.442(17) calc PR B 2 H3H H 0.9502 0.0394 0.2094 0.165 Uiso 0.442(17) calc PR B 2 C13B C 0.6536(13) 0.0777(10) 0.4492(13) 0.142(7) Uani 0.442(17) d P B 2 H13I H 0.6228 0.0871 0.3853 0.170 Uiso 0.442(17) calc PR B 2 H13J H 0.6053 0.0363 0.4819 0.170 Uiso 0.442(17) calc PR B 2 C14B C 0.780(3) 0.038(2) 0.449(2) 0.108(10) Uiso 0.442(17) d P B 2 H14L H 0.8236 0.0594 0.5047 0.130 Uiso 0.442(17) calc PR B 2 H14M H 0.7800 -0.0284 0.4488 0.130 Uiso 0.442(17) calc PR B 2 C41B C 0.770(3) 0.044(2) 0.273(2) 0.108(9) Uiso 0.442(17) d P B 2 H41K H 0.7812 -0.0214 0.2671 0.130 Uiso 0.442(17) calc PR B 2 H41L H 0.7983 0.0744 0.2192 0.130 Uiso 0.442(17) calc PR B 2 H41M H 0.6912 0.0562 0.2755 0.130 Uiso 0.442(17) calc PR B 2 C4 C 1.0107(10) 0.1640(11) 0.2277(7) 0.108(5) Uani 1 d . . . H4A H 0.9554 0.1765 0.1770 0.129 Uiso 1 calc R C 1 H4B H 1.0840 0.1699 0.2021 0.129 Uiso 1 calc R C 1 N5 N 0.9997(5) 0.2382(5) 0.3050(4) 0.0560(15) Uani 1 d . . . C6 C 0.9920(7) 0.3326(6) 0.2661(5) 0.065(2) Uani 1 d . . . H6A H 0.9471 0.3320 0.2072 0.078 Uiso 1 calc R . . H6B H 1.0662 0.3544 0.2530 0.078 Uiso 1 calc R . . C7 C 0.9409(7) 0.3961(6) 0.3337(5) 0.060(2) Uani 1 d . . . C21 C 0.9617(10) 0.4890(7) 0.3487(8) 0.090(4) Uani 1 d . . . H21 H 1.0165 0.5193 0.3166 0.108 Uiso 1 calc R . . C22 C 0.9021(12) 0.5332(8) 0.4095(9) 0.093(3) Uani 1 d . . . H22 H 0.9156 0.5957 0.4186 0.112 Uiso 1 calc R . . C23 C 0.8209(10) 0.4923(7) 0.4604(7) 0.088(3) Uani 1 d . . . H23 H 0.7805 0.5257 0.5029 0.106 Uiso 1 calc R . . C51 C 1.0921(7) 0.2324(6) 0.3779(6) 0.0600(19) Uani 1 d . . . H51A H 1.1370 0.2878 0.3752 0.072 Uiso 1 calc R . . H51B H 1.1395 0.1807 0.3634 0.072 Uiso 1 calc R . . C52 C 1.0542(6) 0.2212(5) 0.4763(5) 0.0483(16) Uani 1 d . . . O53 O 1.1304(4) 0.2256(4) 0.5423(4) 0.0577(13) Uani 1 d . . . O54 O 0.9524(4) 0.2076(3) 0.4917(3) 0.0540(13) Uani 1 d . . . C61 C 0.6060(7) 0.2690(7) 0.3678(6) 0.070(2) Uani 1 d . . . H61A H 0.5764 0.3299 0.3793 0.084 Uiso 1 calc R . . H61B H 0.5461 0.2249 0.3743 0.084 Uiso 1 calc R . . C62 C 0.6463(6) 0.2645(5) 0.2675(5) 0.0528(17) Uani 1 d . . . O63 O 0.5716(5) 0.2883(4) 0.2034(4) 0.0642(15) Uani 1 d . . . O64 O 0.7441(4) 0.2413(4) 0.2483(3) 0.0554(13) Uani 1 d . . . Br Br 1.16391(11) 0.57654(8) 0.17377(9) 0.0991(5) Uani 1 d . . . O100 O 1.467(3) 0.443(2) 0.4801(18) 0.136(7) Uiso 0.50 d PD D 1 H101 H 1.524(14) 0.46(3) 0.448(17) 0.164 Uiso 0.50 d PD E 1 H102 H 1.42(2) 0.41(3) 0.44(3) 0.164 Uiso 0.50 d PD F 1 O100 O 1.423(2) 0.3935(19) 0.4859(15) 0.120(7) Uiso 0.50 d PD G 2 H101 H 1.42(2) 0.335(2) 0.488(18) 0.144 Uiso 0.50 d PD H 2 H102 H 1.48(3) 0.408(17) 0.45(2) 0.144 Uiso 0.50 d PD I 2 O200 O 1.3311(7) 0.2739(7) 0.2145(6) 0.102(2) Uani 1 d D . . H201 H 1.318(11) 0.223(4) 0.242(7) 0.122 Uiso 1 d D . . H202 H 1.365(11) 0.310(6) 0.253(6) 0.122 Uiso 1 d D . . O300 O 1.2809(9) 0.4233(8) 0.3310(7) 0.118(3) Uani 1 d D . . H301 H 1.263(10) 0.463(8) 0.289(8) 0.142 Uiso 1 d D . . H302 H 1.346(6) 0.403(10) 0.321(9) 0.142 Uiso 1 d D . . O400 O 1.3687(8) 0.2019(10) 0.5284(8) 0.143(4) Uani 1 d D . . H401 H 1.368(11) 0.184(13) 0.471(4) 0.171 Uiso 1 d D . . H402 H 1.436(4) 0.202(11) 0.552(9) 0.171 Uiso 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.0475(7) 0.0499(6) 0.0406(6) 0.0003(3) 0.0003(4) 0.0022(3) N8 0.054(4) 0.060(4) 0.044(3) 0.004(2) 0.003(3) 0.010(3) C9 0.059(5) 0.076(5) 0.050(4) -0.020(3) 0.000(3) 0.024(4) C10 0.063(5) 0.115(8) 0.045(4) -0.014(4) 0.004(4) 0.021(5) N11 0.053(4) 0.095(5) 0.049(4) 0.015(3) 0.001(3) 0.000(3) C12 0.065(6) 0.169(11) 0.073(6) 0.067(7) -0.009(5) -0.036(7) N1 0.107(6) 0.047(4) 0.099(6) -0.002(3) -0.049(5) 0.000(3) C3 0.141(12) 0.104(11) 0.168(14) -0.081(10) 0.012(10) 0.047(9) C13 0.117(11) 0.129(12) 0.175(15) 0.081(11) -0.021(10) -0.057(9) N1B 0.107(6) 0.047(4) 0.099(6) -0.002(3) -0.049(5) 0.000(3) C3B 0.141(12) 0.104(11) 0.168(14) -0.081(10) 0.012(10) 0.047(9) C13B 0.117(11) 0.129(12) 0.175(15) 0.081(11) -0.021(10) -0.057(9) C4 0.081(7) 0.178(13) 0.062(6) -0.052(7) -0.019(5) 0.041(8) N5 0.052(4) 0.073(4) 0.043(3) -0.015(3) 0.005(3) 0.013(3) C6 0.060(5) 0.091(6) 0.045(4) 0.010(4) 0.011(3) -0.002(4) C7 0.053(5) 0.069(5) 0.056(4) 0.015(3) -0.005(3) -0.010(3) C21 0.098(8) 0.065(6) 0.104(8) 0.021(5) -0.034(6) -0.018(5) C22 0.110(9) 0.068(7) 0.101(8) -0.007(6) -0.013(7) 0.006(6) C23 0.099(8) 0.088(7) 0.075(6) -0.033(5) -0.012(6) 0.042(6) C51 0.045(4) 0.081(5) 0.054(4) -0.006(4) 0.004(3) 0.012(4) C52 0.046(5) 0.050(4) 0.049(4) -0.006(3) 0.003(3) 0.005(3) O53 0.046(3) 0.077(3) 0.048(3) -0.009(2) -0.006(2) 0.002(2) O54 0.056(4) 0.064(3) 0.042(3) 0.003(2) 0.000(2) -0.002(2) C61 0.053(5) 0.113(7) 0.046(4) 0.013(4) 0.002(3) 0.005(4) C62 0.045(5) 0.059(4) 0.055(4) 0.005(3) 0.000(3) -0.003(3) O63 0.053(3) 0.086(4) 0.053(3) 0.009(2) -0.007(2) 0.010(3) O64 0.053(3) 0.070(3) 0.043(3) 0.007(2) 0.000(2) 0.008(2) Br 0.1015(10) 0.0944(9) 0.1025(9) 0.0080(6) 0.0154(6) -0.0212(6) O200 0.076(5) 0.130(7) 0.100(6) 0.024(5) 0.003(4) 0.001(4) O300 0.112(7) 0.136(8) 0.107(7) 0.025(5) 0.019(5) -0.005(6) O400 0.087(6) 0.211(12) 0.129(8) -0.054(8) -0.002(5) 0.010(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 Ni N8 1.972(7) . ? Ni N1B 2.077(7) . ? Ni N1 2.077(7) . ? Ni O64 2.090(5) . ? Ni O54 2.095(5) . ? Ni N5 2.114(7) . ? Ni N11 2.116(8) . ? N8 C9 1.333(10) . ? N8 C7 1.357(10) . ? C9 C23 1.422(14) . ? C9 C10 1.504(14) . ? C10 N11 1.504(12) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? N11 C61 1.482(10) . ? N11 C12 1.499(12) . ? C12 C13B 1.58(2) . ? C12 C13 1.58(2) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? N1 C2 1.47(2) . ? N1 C41 1.49(2) . ? N1 C14 1.56(2) . ? C2 C3 1.59(2) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.45(2) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C13 C14 1.47(3) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? N1B C41B 1.45(3) . ? N1B C2B 1.51(3) . ? N1B C14B 1.55(3) . ? C2B C3B 1.65(3) . ? C2B H2E 0.9700 . ? C2B H2F 0.9700 . ? C3B C4 1.45(2) . ? C3B H3G 0.9700 . ? C3B H3H 0.9700 . ? C13B C14B 1.62(4) . ? C13B H13I 0.9700 . ? C13B H13J 0.9700 . ? C14B H14L 0.9700 . ? C14B H14M 0.9700 . ? C41B H41K 0.9600 . ? C41B H41L 0.9600 . ? C41B H41M 0.9600 . ? C4 N5 1.549(12) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? N5 C51 1.475(9) . ? N5 C6 1.480(12) . ? C6 C7 1.485(13) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C21 1.387(13) . ? C21 C22 1.316(17) . ? C21 H21 0.9300 . ? C22 C23 1.376(17) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C51 C52 1.501(11) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 O54 1.264(9) . ? C52 O53 1.274(8) . ? C61 C62 1.529(12) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 O64 1.261(10) . ? C62 O63 1.288(9) . ? O100 H101 0.86(5) . ? O100 H102 0.87(11) . ? O100 H102 0.7(3) . ? O100 H102 0.7(5) . ? O100 H101 0.851(18) . ? O100 H102 0.87(9) . ? O200 H201 0.850(10) . ? O200 H202 0.851(10) . ? O300 H301 0.851(10) . ? O300 H302 0.852(10) . ? O400 H401 0.851(10) . ? O400 H402 0.851(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N8 Ni N1B 178.9(4) . . ? N8 Ni N1 178.9(4) . . ? N1B Ni N1 0.0(5) . . ? N8 Ni O64 88.2(2) . . ? N1B Ni O64 92.0(2) . . ? N1 Ni O64 92.0(2) . . ? N8 Ni O54 87.1(2) . . ? N1B Ni O54 92.7(2) . . ? N1 Ni O54 92.7(2) . . ? O64 Ni O54 175.2(2) . . ? N8 Ni N5 80.1(3) . . ? N1B Ni N5 100.9(4) . . ? N1 Ni N5 100.9(4) . . ? O64 Ni N5 95.9(2) . . ? O54 Ni N5 82.5(2) . . ? N8 Ni N11 80.0(3) . . ? N1B Ni N11 98.9(4) . . ? N1 Ni N11 98.9(4) . . ? O64 Ni N11 83.0(2) . . ? O54 Ni N11 97.0(2) . . ? N5 Ni N11 160.1(3) . . ? C9 N8 C7 122.8(8) . . ? C9 N8 Ni 118.8(6) . . ? C7 N8 Ni 118.2(5) . . ? N8 C9 C23 118.2(9) . . ? N8 C9 C10 113.2(7) . . ? C23 C9 C10 128.4(8) . . ? N11 C10 C9 110.9(7) . . ? N11 C10 H10A 109.5 . . ? C9 C10 H10A 109.5 . . ? N11 C10 H10B 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 108.0 . . ? C61 N11 C12 111.8(7) . . ? C61 N11 C10 109.6(7) . . ? C12 N11 C10 109.0(8) . . ? C61 N11 Ni 110.0(5) . . ? C12 N11 Ni 111.0(7) . . ? C10 N11 Ni 105.1(5) . . ? N11 C12 C13B 111.8(10) . . ? N11 C12 C13 111.8(10) . . ? C13B C12 C13 0.0(16) . . ? N11 C12 H12A 109.3 . . ? C13B C12 H12A 109.3 . . ? C13 C12 H12A 109.3 . . ? N11 C12 H12B 109.3 . . ? C13B C12 H12B 109.3 . . ? C13 C12 H12B 109.3 . . ? H12A C12 H12B 107.9 . . ? C2 N1 C41 113.3(13) . . ? C2 N1 C14 107.5(11) . . ? C41 N1 C14 104.3(13) . . ? C2 N1 Ni 107.1(9) . . ? C41 N1 Ni 116.6(9) . . ? C14 N1 Ni 107.4(8) . . ? N1 C2 C3 111.3(13) . . ? N1 C2 H2A 109.4 . . ? C3 C2 H2A 109.4 . . ? N1 C2 H2B 109.4 . . ? C3 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C4 C3 C2 108.0(12) . . ? C4 C3 H3A 110.1 . . ? C2 C3 H3A 110.1 . . ? C4 C3 H3B 110.1 . . ? C2 C3 H3B 110.1 . . ? H3A C3 H3B 108.4 . . ? C14 C13 C12 125.6(11) . . ? C14 C13 H13A 105.9 . . ? C12 C13 H13A 105.9 . . ? C14 C13 H13B 105.9 . . ? C12 C13 H13B 105.9 . . ? H13A C13 H13B 106.2 . . ? C13 C14 N1 112.1(13) . . ? C13 C14 H14A 109.2 . . ? N1 C14 H14A 109.2 . . ? C13 C14 H14B 109.2 . . ? N1 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C41B N1B C2B 107.4(18) . . ? C41B N1B C14B 113.3(19) . . ? C2B N1B C14B 104.4(16) . . ? C41B N1B Ni 116.1(13) . . ? C2B N1B Ni 105.2(12) . . ? C14B N1B Ni 109.5(13) . . ? N1B C2B C3B 106.5(17) . . ? N1B C2B H2E 110.4 . . ? C3B C2B H2E 110.4 . . ? N1B C2B H2F 110.4 . . ? C3B C2B H2F 110.5 . . ? H2E C2B H2F 108.6 . . ? C4 C3B C2B 124.3(13) . . ? C4 C3B H3G 106.3 . . ? C2B C3B H3G 106.2 . . ? C4 C3B H3H 106.3 . . ? C2B C3B H3H 106.3 . . ? H3G C3B H3H 106.4 . . ? C12 C13B C14B 103.0(14) . . ? C12 C13B H13I 111.2 . . ? C14B C13B H13I 111.2 . . ? C12 C13B H13J 111.2 . . ? C14B C13B H13J 111.2 . . ? H13I C13B H13J 109.1 . . ? N1B C14B C13B 105.1(18) . . ? N1B C14B H14L 110.7 . . ? C13B C14B H14L 110.7 . . ? N1B C14B H14M 110.7 . . ? C13B C14B H14M 110.7 . . ? H14L C14B H14M 108.8 . . ? N1B C41B H41K 109.5 . . ? N1B C41B H41L 109.5 . . ? H41K C41B H41L 109.5 . . ? N1B C41B H41M 109.5 . . ? H41K C41B H41M 109.5 . . ? H41L C41B H41M 109.5 . . ? C3B C4 C3 0.0(18) . . ? C3B C4 N5 115.6(10) . . ? C3 C4 N5 115.6(10) . . ? C3B C4 H4A 108.4 . . ? C3 C4 H4A 108.4 . . ? N5 C4 H4A 108.4 . . ? C3B C4 H4B 108.4 . . ? C3 C4 H4B 108.4 . . ? N5 C4 H4B 108.4 . . ? H4A C4 H4B 107.5 . . ? C51 N5 C6 110.1(6) . . ? C51 N5 C4 111.6(6) . . ? C6 N5 C4 112.8(8) . . ? C51 N5 Ni 108.8(5) . . ? C6 N5 Ni 104.4(5) . . ? C4 N5 Ni 108.8(6) . . ? N5 C6 C7 110.7(6) . . ? N5 C6 H6A 109.5 . . ? C7 C6 H6A 109.5 . . ? N5 C6 H6B 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? N8 C7 C21 119.5(9) . . ? N8 C7 C6 111.6(7) . . ? C21 C7 C6 128.8(9) . . ? C22 C21 C7 118.6(11) . . ? C22 C21 H21 120.7 . . ? C7 C21 H21 120.7 . . ? C21 C22 C23 123.7(11) . . ? C21 C22 H22 118.2 . . ? C23 C22 H22 118.2 . . ? C22 C23 C9 117.3(9) . . ? C22 C23 H23 121.3 . . ? C9 C23 H23 121.4 . . ? N5 C51 C52 114.0(7) . . ? N5 C51 H51A 108.8 . . ? C52 C51 H51A 108.8 . . ? N5 C51 H51B 108.7 . . ? C52 C51 H51B 108.7 . . ? H51A C51 H51B 107.6 . . ? O54 C52 O53 122.7(7) . . ? O54 C52 C51 121.2(6) . . ? O53 C52 C51 116.1(7) . . ? C52 O54 Ni 113.1(4) . . ? N11 C61 C62 111.3(7) . . ? N11 C61 H61A 109.4 . . ? C62 C61 H61A 109.4 . . ? N11 C61 H61B 109.4 . . ? C62 C61 H61B 109.4 . . ? H61A C61 H61B 108.0 . . ? O64 C62 O63 122.5(7) . . ? O64 C62 C61 123.7(6) . . ? O63 C62 C61 113.9(7) . . ? C62 O64 Ni 112.0(5) . . ? H101 O100 H102 108(8) . . ? H101 O100 H102 70(10) . . ? H102 O100 H102 50(10) . . ? H102 O100 H101 116(10) . . ? H102 O100 H102 51(10) . . ? H101 O100 H102 109(4) . . ? H201 O200 H202 109.4(18) . . ? H301 O300 H302 109.0(18) . . ? H401 O400 H402 109.2(18) . . ? 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 C9 N8 C7 C6 -177.6(6) . . . . ? N8 C7 C6 N5 -34.4(9) . . . . ? C7 C6 N5 C4 159.1(7) . . . . ? C6 N5 C4 C3 -168.5(10) . . . . ? N5 C4 C3 C2 78.1(13) . . . . ? C4 C3 C2 N1 -87.1(15) . . . . ? C3 C2 N1 C14 -179.6(13) . . . . ? C2 N1 C14 C13 179.1(13) . . . . ? N1 C14 C13 C12 50(2) . . . . ? C14 C13 C12 N11 21.5(19) . . . . ? C13 C12 N11 C10 -173.1(9) . . . . ? C12 N11 C10 C9 154.8(7) . . . . ? N11 C10 C9 N8 -24.1(9) . . . . ? C10 C9 N8 C7 -175.8(6) . . . . ? C9 N8 C7 C6 -177.6(6) . . . . ? C6 N5 C4 C3B -168.5(10) . . . . ? N5 C4 C3B C2B 13(2) . . . . ? C4 C3B C2B N1B 61(2) . . . . ? C3B C2B N1B C14B 174.2(17) . . . . ? C2B N1B C14B C13B -179.9(18) . . . . ? N1B C14B C13B C12 -89.8(18) . . . . ? C14B C13B C12 N11 85.5(15) . . . . ? C13B C12 N11 C10 -173.1(9) . . . . ? _diffrn_measured_fraction_theta_max 0.841 _diffrn_reflns_theta_full 26.12 _diffrn_measured_fraction_theta_full 0.841 _refine_diff_density_max 1.120 _refine_diff_density_min -1.800 _refine_diff_density_rms 0.138 #===END data_complex3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety Ca[CuL3]NO3.CH3CN.2H2O _chemical_formula_sum 'C21 H32 Ca Cu N6 O11' _chemical_formula_weight 648.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ca' 'Ca' 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n 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 8.643(11) _cell_length_b 18.98(2) _cell_length_c 17.09(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.490(10) _cell_angle_gamma 90.00 _cell_volume 2727(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.579 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1348 _exptl_absorpt_coefficient_mu 1.057 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9363 _diffrn_reflns_av_R_equivalents 0.1020 _diffrn_reflns_av_sigmaI/netI 0.1406 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 25.99 _reflns_number_total 5019 _reflns_number_gt 3126 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0622P)^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 5019 _refine_ls_number_parameters 374 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1644 _refine_ls_R_factor_gt 0.0910 _refine_ls_wR_factor_ref 0.1701 _refine_ls_wR_factor_gt 0.1455 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.070 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.09787(9) 0.17111(4) 0.79672(5) 0.0286(2) Uani 1 d . . . N1 N 0.1950(6) 0.2200(3) 0.9040(3) 0.0342(14) Uani 1 d . . . C2 C 0.0658(8) 0.2485(4) 0.9395(5) 0.0395(18) Uani 1 d . . . H2A H 0.0097 0.2846 0.9037 0.047 Uiso 1 calc R . . H2B H 0.1146 0.2711 0.9901 0.047 Uiso 1 calc R . . C3 C -0.0545(8) 0.1960(4) 0.9547(5) 0.0421(19) Uani 1 d . . . H3A H -0.1131 0.2173 0.9905 0.051 Uiso 1 calc R . . H3B H 0.0022 0.1557 0.9824 0.051 Uiso 1 calc R . . C4 C -0.1729(8) 0.1699(4) 0.8803(4) 0.0374(17) Uani 1 d . . . H4A H -0.2564 0.1442 0.8972 0.045 Uiso 1 calc R . . H4B H -0.2217 0.2104 0.8496 0.045 Uiso 1 calc R . . N5 N -0.1058(6) 0.1241(3) 0.8268(3) 0.0261(13) Uani 1 d . . . C6 C -0.2224(8) 0.1134(4) 0.7475(4) 0.0385(19) Uani 1 d . . . H6A H -0.2902 0.0735 0.7516 0.046 Uiso 1 calc R . . H6B H -0.2895 0.1548 0.7350 0.046 Uiso 1 calc R . . C7 C -0.1416(9) 0.1007(4) 0.6815(5) 0.0405(19) Uani 1 d . . . N8 N 0.0103(7) 0.1229(3) 0.6954(3) 0.0342(14) Uani 1 d . . . C9 C 0.0946(9) 0.1226(4) 0.6398(5) 0.047(2) Uani 1 d . . . C10 C 0.2537(9) 0.1510(4) 0.6691(5) 0.050(2) Uani 1 d . . . H10A H 0.2920 0.1688 0.6238 0.060 Uiso 1 calc R . . H10B H 0.3245 0.1135 0.6938 0.060 Uiso 1 calc R . . N11 N 0.2592(6) 0.2086(3) 0.7286(4) 0.0385(15) Uani 1 d . . . C12 C 0.4223(9) 0.2175(5) 0.7801(6) 0.061(3) Uani 1 d . . . H12A H 0.4916 0.2344 0.7469 0.074 Uiso 1 calc R . . H12B H 0.4617 0.1718 0.8011 0.074 Uiso 1 calc R . . C13 C 0.4327(8) 0.2679(5) 0.8502(6) 0.063(3) Uani 1 d . . . H13A H 0.4680 0.3130 0.8340 0.076 Uiso 1 calc R . . H13B H 0.5164 0.2508 0.8942 0.076 Uiso 1 calc R . . C14 C 0.2861(9) 0.2820(4) 0.8841(5) 0.047(2) Uani 1 d . . . H14A H 0.3203 0.3098 0.9327 0.056 Uiso 1 calc R . . H14B H 0.2131 0.3109 0.8456 0.056 Uiso 1 calc R . . C21 C -0.2178(12) 0.0754(5) 0.6061(6) 0.068(3) Uani 1 d . . . H21 H -0.3237 0.0612 0.5957 0.082 Uiso 1 calc R . . C22 C -0.1320(14) 0.0715(6) 0.5459(6) 0.081(3) Uani 1 d . . . H22 H -0.1781 0.0525 0.4957 0.097 Uiso 1 calc R . . C23 C 0.0237(13) 0.0968(5) 0.5628(6) 0.073(3) Uani 1 d . . . H23 H 0.0808 0.0966 0.5229 0.088 Uiso 1 calc R . . C41 C 0.3028(8) 0.1724(4) 0.9631(4) 0.0431(19) Uani 1 d . . . H41A H 0.3982 0.1986 0.9875 0.052 Uiso 1 calc R . . H41B H 0.2496 0.1609 1.0055 0.052 Uiso 1 calc R . . C42 C 0.3518(7) 0.1055(3) 0.9306(4) 0.0255(15) Uani 1 d . . . O43 O 0.4468(5) 0.0676(2) 0.9792(3) 0.0316(11) Uani 1 d . . . O44 O 0.2975(5) 0.0896(2) 0.8574(3) 0.0271(10) Uani 1 d . . . C51 C -0.0475(7) 0.0552(3) 0.8630(4) 0.0293(16) Uani 1 d . . . H51A H 0.0343 0.0649 0.9112 0.035 Uiso 1 calc R . . H51B H 0.0044 0.0317 0.8256 0.035 Uiso 1 calc R . . C52 C -0.1656(8) 0.0009(4) 0.8865(4) 0.0322(16) Uani 1 d . . . O53 O -0.1018(5) -0.0568(3) 0.9104(3) 0.0425(13) Uani 1 d . . . O54 O -0.3066(5) 0.0195(3) 0.8820(3) 0.0403(13) Uani 1 d . . . C61 C 0.1995(8) 0.2757(4) 0.6857(5) 0.045(2) Uani 1 d . . . H61A H 0.1969 0.2697 0.6291 0.054 Uiso 1 calc R . . H61B H 0.2758 0.3127 0.7061 0.054 Uiso 1 calc R . . C62 C 0.0363(8) 0.3005(4) 0.6931(4) 0.0338(17) Uani 1 d . . . O63 O -0.0123(5) 0.3551(3) 0.6537(3) 0.0398(12) Uani 1 d . . . O64 O -0.0356(5) 0.2683(2) 0.7382(3) 0.0377(12) Uani 1 d . . . Ca Ca 0.44316(13) -0.03283(7) 0.88158(8) 0.0207(3) Uani 1 d . . . N200 N -0.167(2) 0.3860(9) 0.9646(8) 0.198(8) Uani 1 d . . . C201 C -0.2074(16) 0.3940(7) 0.8963(9) 0.094(4) Uani 1 d . . . C202 C -0.2437(16) 0.4081(6) 0.8114(8) 0.113(4) Uani 1 d . . . H20A H -0.1648 0.4392 0.7993 0.136 Uiso 1 calc R . . H20B H -0.3466 0.4298 0.7956 0.136 Uiso 1 calc R . . H20C H -0.2438 0.3647 0.7825 0.136 Uiso 1 calc R . . O300 O 0.2708(5) 0.4290(3) 0.5592(3) 0.0423(13) Uani 1 d D . . H301 H 0.355(5) 0.405(3) 0.577(3) 0.051 Uiso 1 d D . . H302 H 0.274(7) 0.446(4) 0.513(2) 0.051 Uiso 1 d D . . O400 O -0.3655(8) 0.2945(4) 0.6525(5) 0.088(2) Uani 1 d D . . H401 H -0.268(4) 0.284(4) 0.669(6) 0.106 Uiso 1 d D . . H402 H -0.381(10) 0.336(3) 0.669(7) 0.106 Uiso 1 d D . . N100 N 0.2296(16) 0.4609(4) 0.7879(5) 0.080(3) Uani 1 d . . . O101 O 0.0923(11) 0.4877(4) 0.7680(5) 0.085(2) Uani 1 d . . . O102 O 0.2970(8) 0.4427(4) 0.7341(5) 0.084(2) Uani 1 d . . . O103 O 0.2994(16) 0.4547(5) 0.8586(5) 0.178(6) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0303(4) 0.0239(5) 0.0323(5) 0.0050(4) 0.0083(3) 0.0017(4) N1 0.038(3) 0.021(3) 0.041(4) 0.004(3) 0.002(3) 0.010(3) C2 0.048(4) 0.031(4) 0.041(5) -0.002(4) 0.012(4) 0.009(3) C3 0.046(4) 0.034(5) 0.051(5) 0.012(4) 0.022(4) 0.008(3) C4 0.038(4) 0.034(4) 0.044(5) 0.003(4) 0.015(3) 0.000(3) N5 0.026(3) 0.020(3) 0.031(3) 0.006(3) 0.005(2) -0.001(2) C6 0.027(4) 0.037(5) 0.048(5) 0.006(4) 0.001(3) -0.004(3) C7 0.051(5) 0.026(4) 0.040(5) 0.005(4) 0.001(4) -0.007(3) N8 0.045(4) 0.023(3) 0.035(4) 0.008(3) 0.011(3) 0.006(3) C9 0.058(5) 0.046(5) 0.036(5) 0.008(4) 0.007(4) 0.012(4) C10 0.066(5) 0.043(5) 0.055(6) 0.017(4) 0.043(5) 0.028(4) N11 0.034(3) 0.032(4) 0.055(4) 0.015(3) 0.021(3) 0.005(3) C12 0.040(5) 0.049(6) 0.101(8) 0.018(6) 0.026(5) -0.001(4) C13 0.027(4) 0.066(7) 0.095(8) -0.008(6) 0.010(4) -0.009(4) C14 0.049(5) 0.029(5) 0.057(6) -0.012(4) 0.000(4) -0.006(4) C21 0.085(7) 0.060(7) 0.052(6) -0.001(5) 0.001(5) -0.002(5) C22 0.111(9) 0.067(8) 0.054(7) -0.001(6) -0.002(6) 0.011(7) C23 0.107(8) 0.065(7) 0.054(7) 0.010(5) 0.033(6) 0.021(6) C41 0.050(4) 0.030(4) 0.043(5) -0.005(4) -0.002(3) 0.005(4) C42 0.021(3) 0.027(4) 0.031(4) -0.001(3) 0.011(3) 0.000(3) O43 0.033(2) 0.027(3) 0.032(3) 0.000(2) 0.000(2) 0.006(2) O44 0.029(2) 0.023(3) 0.030(3) 0.004(2) 0.007(2) 0.0040(19) C51 0.037(4) 0.026(4) 0.027(4) -0.002(3) 0.011(3) -0.005(3) C52 0.038(4) 0.029(4) 0.033(4) -0.006(3) 0.016(3) -0.009(3) O53 0.035(3) 0.032(3) 0.060(4) 0.008(3) 0.011(2) -0.010(2) O54 0.032(3) 0.036(3) 0.057(4) 0.003(3) 0.018(2) 0.000(2) C61 0.046(4) 0.036(5) 0.060(6) 0.022(4) 0.029(4) 0.015(4) C62 0.035(4) 0.022(4) 0.038(4) -0.002(4) -0.003(3) 0.004(3) O63 0.040(3) 0.027(3) 0.052(3) 0.010(3) 0.009(2) 0.004(2) O64 0.041(3) 0.030(3) 0.047(3) 0.014(2) 0.020(2) 0.004(2) Ca 0.0233(6) 0.0163(7) 0.0226(7) -0.0008(6) 0.0058(5) -0.0014(5) N200 0.257(17) 0.25(2) 0.095(10) 0.022(12) 0.059(11) 0.152(15) C201 0.118(10) 0.074(9) 0.095(10) 0.003(8) 0.037(9) 0.033(7) C202 0.162(12) 0.083(10) 0.104(11) -0.006(8) 0.052(10) -0.002(9) O300 0.035(3) 0.049(4) 0.046(3) 0.003(3) 0.015(2) 0.015(2) O400 0.069(4) 0.089(6) 0.108(6) 0.009(5) 0.025(4) 0.003(4) N100 0.165(10) 0.033(5) 0.026(5) 0.006(4) -0.010(6) -0.019(6) O101 0.152(7) 0.062(5) 0.057(5) -0.020(4) 0.054(5) -0.027(5) O102 0.087(5) 0.072(5) 0.070(6) 0.013(4) -0.028(4) -0.008(4) O103 0.343(16) 0.103(8) 0.047(6) 0.014(5) -0.040(8) -0.030(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu N8 1.949(6) . ? Cu N1 2.051(6) . ? Cu N11 2.137(6) . ? Cu N5 2.140(5) . ? Cu O64 2.279(5) . ? Cu O44 2.369(4) . ? N1 C2 1.491(8) . ? N1 C14 1.498(9) . ? N1 C41 1.505(8) . ? C2 C3 1.506(10) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.518(10) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N5 1.475(8) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? N5 C51 1.484(8) . ? N5 C6 1.502(8) . ? C6 C7 1.478(10) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N8 1.346(9) . ? C7 C21 1.389(11) . ? N8 C9 1.326(9) . ? C9 C23 1.403(12) . ? C9 C10 1.454(11) . ? C10 N11 1.487(10) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? N11 C12 1.487(10) . ? N11 C61 1.499(8) . ? C12 C13 1.520(12) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.536(10) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C21 C22 1.403(14) . ? C21 H21 0.9300 . ? C22 C23 1.394(14) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C41 C42 1.487(9) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 O43 1.250(7) . ? C42 O44 1.266(7) . ? C42 Ca 2.920(7) . ? O43 Ca 2.438(5) 3_657 ? O43 Ca 2.529(5) . ? O44 Ca 2.630(5) . ? C51 C52 1.568(9) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 O53 1.251(8) . ? C52 O54 1.254(8) . ? O54 Ca 2.379(5) 1_455 ? C61 C62 1.520(9) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 O63 1.254(8) . ? C62 O64 1.256(8) . ? O63 Ca 2.328(5) 2_556 ? Ca O63 2.328(5) 2_546 ? Ca O54 2.379(5) 1_655 ? Ca O300 2.417(5) 2_546 ? Ca O43 2.438(5) 3_657 ? Ca O101 2.534(8) 2_546 ? Ca O102 2.553(7) 2_546 ? Ca N100 2.936(9) 2_546 ? Ca Ca 4.129(5) 3_657 ? N200 C201 1.147(15) . ? C201 C202 1.437(16) . ? C202 H20A 0.9600 . ? C202 H20B 0.9600 . ? C202 H20C 0.9600 . ? O300 Ca 2.417(5) 2_556 ? O300 H301 0.853(10) . ? O300 H302 0.853(10) . ? O400 H401 0.851(10) . ? O400 H402 0.853(10) . ? N100 O103 1.223(11) . ? N100 O102 1.248(12) . ? N100 O101 1.262(11) . ? N100 Ca 2.936(9) 2_556 ? O101 Ca 2.534(8) 2_556 ? O102 Ca 2.553(7) 2_556 ? 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 N8 Cu N1 178.5(2) . . ? N8 Cu N11 80.8(3) . . ? N1 Cu N11 98.8(2) . . ? N8 Cu N5 81.2(2) . . ? N1 Cu N5 99.4(2) . . ? N11 Cu N5 161.4(2) . . ? N8 Cu O64 86.5(2) . . ? N1 Cu O64 94.9(2) . . ? N11 Cu O64 79.6(2) . . ? N5 Cu O64 94.72(19) . . ? N8 Cu O44 100.0(2) . . ? N1 Cu O44 78.47(19) . . ? N11 Cu O44 87.4(2) . . ? N5 Cu O44 100.29(19) . . ? O64 Cu O44 164.36(16) . . ? C2 N1 C14 106.9(5) . . ? C2 N1 C41 110.4(6) . . ? C14 N1 C41 110.3(6) . . ? C2 N1 Cu 109.8(4) . . ? C14 N1 Cu 106.3(4) . . ? C41 N1 Cu 112.8(4) . . ? N1 C2 C3 116.3(6) . . ? N1 C2 H2A 108.2 . . ? C3 C2 H2A 108.2 . . ? N1 C2 H2B 108.2 . . ? C3 C2 H2B 108.2 . . ? H2A C2 H2B 107.4 . . ? C2 C3 C4 115.4(6) . . ? C2 C3 H3A 108.4 . . ? C4 C3 H3A 108.4 . . ? C2 C3 H3B 108.4 . . ? C4 C3 H3B 108.4 . . ? H3A C3 H3B 107.5 . . ? N5 C4 C3 115.2(6) . . ? N5 C4 H4A 108.5 . . ? C3 C4 H4A 108.5 . . ? N5 C4 H4B 108.5 . . ? C3 C4 H4B 108.5 . . ? H4A C4 H4B 107.5 . . ? C4 N5 C51 113.9(5) . . ? C4 N5 C6 111.1(5) . . ? C51 N5 C6 110.4(5) . . ? C4 N5 Cu 111.6(4) . . ? C51 N5 Cu 104.4(4) . . ? C6 N5 Cu 104.9(4) . . ? C7 C6 N5 111.9(6) . . ? C7 C6 H6A 109.2 . . ? N5 C6 H6A 109.2 . . ? C7 C6 H6B 109.2 . . ? N5 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? N8 C7 C21 120.3(8) . . ? N8 C7 C6 115.4(7) . . ? C21 C7 C6 123.9(8) . . ? C9 N8 C7 123.3(7) . . ? C9 N8 Cu 118.3(5) . . ? C7 N8 Cu 117.7(5) . . ? N8 C9 C23 118.7(8) . . ? N8 C9 C10 112.7(7) . . ? C23 C9 C10 128.6(8) . . ? C9 C10 N11 112.7(6) . . ? C9 C10 H10A 109.1 . . ? N11 C10 H10A 109.1 . . ? C9 C10 H10B 109.1 . . ? N11 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? C10 N11 C12 111.2(6) . . ? C10 N11 C61 109.8(6) . . ? C12 N11 C61 111.3(6) . . ? C10 N11 Cu 101.9(4) . . ? C12 N11 Cu 111.4(5) . . ? C61 N11 Cu 110.8(4) . . ? N11 C12 C13 114.3(6) . . ? N11 C12 H12A 108.7 . . ? C13 C12 H12A 108.7 . . ? N11 C12 H12B 108.7 . . ? C13 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? C12 C13 C14 120.4(6) . . ? C12 C13 H13A 107.2 . . ? C14 C13 H13A 107.2 . . ? C12 C13 H13B 107.2 . . ? C14 C13 H13B 107.2 . . ? H13A C13 H13B 106.9 . . ? N1 C14 C13 118.2(6) . . ? N1 C14 H14A 107.8 . . ? C13 C14 H14A 107.8 . . ? N1 C14 H14B 107.8 . . ? C13 C14 H14B 107.8 . . ? H14A C14 H14B 107.1 . . ? C7 C21 C22 118.7(10) . . ? C7 C21 H21 120.6 . . ? C22 C21 H21 120.6 . . ? C23 C22 C21 118.7(10) . . ? C23 C22 H22 120.7 . . ? C21 C22 H22 120.7 . . ? C22 C23 C9 120.3(9) . . ? C22 C23 H23 119.9 . . ? C9 C23 H23 119.9 . . ? C42 C41 N1 116.6(6) . . ? C42 C41 H41A 108.1 . . ? N1 C41 H41A 108.1 . . ? C42 C41 H41B 108.1 . . ? N1 C41 H41B 108.1 . . ? H41A C41 H41B 107.3 . . ? O43 C42 O44 123.7(6) . . ? O43 C42 C41 116.3(6) . . ? O44 C42 C41 120.0(6) . . ? O43 C42 Ca 59.6(3) . . ? O44 C42 Ca 64.2(3) . . ? C41 C42 Ca 174.2(5) . . ? C42 O43 Ca 148.3(4) . 3_657 ? C42 O43 Ca 95.1(4) . . ? Ca O43 Ca 112.43(19) 3_657 . ? C42 O44 Cu 110.0(4) . . ? C42 O44 Ca 90.1(4) . . ? Cu O44 Ca 156.8(2) . . ? N5 C51 C52 120.6(5) . . ? N5 C51 H51A 107.2 . . ? C52 C51 H51A 107.2 . . ? N5 C51 H51B 107.2 . . ? C52 C51 H51B 107.2 . . ? H51A C51 H51B 106.8 . . ? O53 C52 O54 127.9(6) . . ? O53 C52 C51 113.3(6) . . ? O54 C52 C51 118.8(6) . . ? C52 O54 Ca 138.9(5) . 1_455 ? N11 C61 C62 116.2(6) . . ? N11 C61 H61A 108.2 . . ? C62 C61 H61A 108.2 . . ? N11 C61 H61B 108.2 . . ? C62 C61 H61B 108.2 . . ? H61A C61 H61B 107.4 . . ? O63 C62 O64 125.4(6) . . ? O63 C62 C61 114.4(6) . . ? O64 C62 C61 120.2(6) . . ? C62 O63 Ca 145.2(4) . 2_556 ? C62 O64 Cu 113.0(4) . . ? O63 Ca O54 95.39(18) 2_546 1_655 ? O63 Ca O300 95.89(19) 2_546 2_546 ? O54 Ca O300 155.22(19) 1_655 2_546 ? O63 Ca O43 86.56(18) 2_546 3_657 ? O54 Ca O43 87.86(17) 1_655 3_657 ? O300 Ca O43 70.89(18) 2_546 3_657 ? O63 Ca O43 153.62(17) 2_546 . ? O54 Ca O43 79.17(16) 1_655 . ? O300 Ca O43 80.93(18) 2_546 . ? O43 Ca O43 67.57(19) 3_657 . ? O63 Ca O101 81.8(2) 2_546 2_546 ? O54 Ca O101 80.5(3) 1_655 2_546 ? O300 Ca O101 123.0(3) 2_546 2_546 ? O43 Ca O101 162.6(2) 3_657 2_546 ? O43 Ca O101 122.0(2) . 2_546 ? O63 Ca O102 81.1(2) 2_546 2_546 ? O54 Ca O102 130.8(3) 1_655 2_546 ? O300 Ca O102 72.9(3) 2_546 2_546 ? O43 Ca O102 140.2(2) 3_657 2_546 ? O43 Ca O102 122.0(2) . 2_546 ? O101 Ca O102 50.3(3) 2_546 2_546 ? O63 Ca O44 155.46(17) 2_546 . ? O54 Ca O44 91.89(17) 1_655 . ? O300 Ca O44 86.89(18) 2_546 . ? O43 Ca O44 117.16(15) 3_657 . ? O43 Ca O44 50.89(15) . . ? O101 Ca O44 76.38(19) 2_546 . ? O102 Ca O44 76.5(2) 2_546 . ? O63 Ca C42 177.89(18) 2_546 . ? O54 Ca C42 86.02(18) 1_655 . ? O300 Ca C42 82.21(19) 2_546 . ? O43 Ca C42 91.93(19) 3_657 . ? O43 Ca C42 25.24(15) . . ? O101 Ca C42 100.0(2) 2_546 . ? O102 Ca C42 99.2(2) 2_546 . ? O44 Ca C42 25.70(15) . . ? O63 Ca N100 79.0(2) 2_546 2_546 ? O54 Ca N100 105.8(3) 1_655 2_546 ? O300 Ca N100 98.0(3) 2_546 2_546 ? O43 Ca N100 160.9(2) 3_657 2_546 ? O43 Ca N100 127.4(2) . 2_546 ? O101 Ca N100 25.3(2) 2_546 2_546 ? O102 Ca N100 25.1(3) 2_546 2_546 ? O44 Ca N100 76.46(19) . 2_546 ? C42 Ca N100 102.1(2) . 2_546 ? O63 Ca Ca 120.89(14) 2_546 3_657 ? O54 Ca Ca 82.12(13) 1_655 3_657 ? O300 Ca Ca 73.15(14) 2_546 3_657 ? O43 Ca Ca 34.49(12) 3_657 3_657 ? O43 Ca Ca 33.08(10) . 3_657 ? O101 Ca Ca 152.6(2) 2_546 3_657 ? O102 Ca Ca 141.1(2) 2_546 3_657 ? O44 Ca Ca 83.29(11) . 3_657 ? C42 Ca Ca 57.71(14) . 3_657 ? N100 Ca Ca 158.4(2) 2_546 3_657 ? N200 C201 C202 174.1(19) . . ? C201 C202 H20A 109.5 . . ? C201 C202 H20B 109.5 . . ? H20A C202 H20B 109.5 . . ? C201 C202 H20C 109.5 . . ? H20A C202 H20C 109.5 . . ? H20B C202 H20C 109.5 . . ? Ca O300 H301 133(4) 2_556 . ? Ca O300 H302 118(4) 2_556 . ? H301 O300 H302 108.6(18) . . ? H401 O400 H402 109.2(18) . . ? O103 N100 O102 119.6(13) . . ? O103 N100 O101 121.4(13) . . ? O102 N100 O101 119.0(8) . . ? O103 N100 Ca 176.7(7) . 2_556 ? O102 N100 Ca 60.0(5) . 2_556 ? O101 N100 Ca 59.2(5) . 2_556 ? N100 O101 Ca 95.4(6) . 2_556 ? N100 O102 Ca 94.9(6) . 2_556 ? 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 C9 N8 C7 C6 -172.5(7) . . . . ? N8 C7 C6 N5 -20.8(9) . . . . ? C7 C6 N5 C4 151.3(6) . . . . ? C6 N5 C4 C3 -168.2(6) . . . . ? N5 C4 C3 C2 69.4(8) . . . . ? C4 C3 C2 N1 -73.7(8) . . . . ? C3 C2 N1 C14 172.6(6) . . . . ? C2 N1 C14 C13 177.1(7) . . . . ? N1 C14 C13 C12 49.6(12) . . . . ? C14 C13 C12 N11 24.4(12) . . . . ? C13 C12 N11 C10 -171.5(7) . . . . ? C12 N11 C10 C9 157.8(7) . . . . ? N11 C10 C9 N8 -33.8(9) . . . . ? C10 C9 N8 C7 178.3(6) . . . . ? C9 N8 C7 C6 -172.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.907 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.907 _refine_diff_density_max 0.431 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.087 #===END data_complex4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety [CoL3]2H2O _chemical_formula_sum 'C19 H29 Co N4 O8' _chemical_formula_weight 500.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n 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 9.889(12) _cell_length_b 17.52(2) _cell_length_c 12.398(15) _cell_angle_alpha 90.00 _cell_angle_beta 97.300(10) _cell_angle_gamma 90.00 _cell_volume 2131(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.560 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 0.861 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5912 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 25.92 _reflns_number_total 3244 _reflns_number_gt 2690 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+2.0883P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0046(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3244 _refine_ls_number_parameters 302 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.1029 _refine_ls_wR_factor_gt 0.0963 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.040 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.22498(4) 0.227569(18) 0.07686(3) 0.02322(15) Uani 1 d . . . N1 N 0.0829(3) 0.30796(14) 0.04069(19) 0.0324(6) Uani 1 d . . . C2 C -0.0446(4) 0.2769(2) -0.0238(3) 0.0436(8) Uani 1 d . . . H2A H -0.0233 0.2628 -0.0953 0.052 Uiso 1 calc R . . H2B H -0.1116 0.3176 -0.0335 0.052 Uiso 1 calc R . . C3 C -0.1087(4) 0.2090(2) 0.0246(3) 0.0499(9) Uani 1 d . . . H3A H -0.1998 0.2017 -0.0133 0.060 Uiso 1 calc R . . H3B H -0.1172 0.2198 0.1002 0.060 Uiso 1 calc R . . C4 C -0.0285(4) 0.1358(2) 0.0184(3) 0.0440(8) Uani 1 d . . . H4A H -0.0849 0.0931 0.0348 0.053 Uiso 1 calc R . . H4B H -0.0074 0.1293 -0.0553 0.053 Uiso 1 calc R . . N5 N 0.1012(3) 0.13426(13) 0.0947(2) 0.0319(6) Uani 1 d . . . C6 C 0.1853(4) 0.06682(16) 0.0660(3) 0.0390(8) Uani 1 d . . . H6A H 0.1534 0.0207 0.0978 0.047 Uiso 1 calc R . . H6B H 0.1754 0.0603 -0.0123 0.047 Uiso 1 calc R . . C7 C 0.3308(3) 0.08010(15) 0.1079(2) 0.0340(7) Uani 1 d . . . N8 N 0.3633(3) 0.15479(12) 0.11391(19) 0.0276(5) Uani 1 d . . . C9 C 0.4921(3) 0.17926(16) 0.1405(2) 0.0309(6) Uani 1 d . . . C10 C 0.5014(3) 0.26478(15) 0.1397(3) 0.0321(7) Uani 1 d . . . H10A H 0.5878 0.2805 0.1175 0.039 Uiso 1 calc R . . H10B H 0.4957 0.2848 0.2119 0.039 Uiso 1 calc R . . N11 N 0.3854(3) 0.29473(12) 0.06095(19) 0.0284(5) Uani 1 d . . . C12 C 0.3686(4) 0.37695(15) 0.0891(3) 0.0389(8) Uani 1 d . . . H12A H 0.4530 0.4036 0.0823 0.047 Uiso 1 calc R . . H12B H 0.3523 0.3804 0.1644 0.047 Uiso 1 calc R . . C13 C 0.2525(4) 0.41716(17) 0.0183(3) 0.0535(10) Uani 1 d . . . H13A H 0.2188 0.4575 0.0614 0.064 Uiso 1 calc R . . H13B H 0.2905 0.4414 -0.0414 0.064 Uiso 1 calc R . . C14 C 0.1314(4) 0.36976(18) -0.0295(3) 0.0455(9) Uani 1 d . . . H14A H 0.0557 0.4042 -0.0502 0.055 Uiso 1 calc R . . H14B H 0.1542 0.3462 -0.0957 0.055 Uiso 1 calc R . . C21 C 0.4312(4) 0.02618(17) 0.1345(3) 0.0508(9) Uani 1 d . . . H21 H 0.4100 -0.0255 0.1326 0.061 Uiso 1 calc R . . C22 C 0.5646(4) 0.0503(2) 0.1640(3) 0.0569(10) Uani 1 d . . . H22 H 0.6330 0.0145 0.1827 0.068 Uiso 1 calc R . . C23 C 0.5964(4) 0.12772(19) 0.1657(3) 0.0461(8) Uani 1 d . . . H23 H 0.6859 0.1442 0.1833 0.055 Uiso 1 calc R . . C41 C 0.0506(4) 0.34051(18) 0.1460(2) 0.0391(8) Uani 1 d . . . H41A H -0.0411 0.3255 0.1570 0.047 Uiso 1 calc R . . H41B H 0.0529 0.3958 0.1420 0.047 Uiso 1 calc R . . C42 C 0.1491(3) 0.31431(15) 0.2422(2) 0.0326(7) Uani 1 d . . . O43 O 0.1455(3) 0.34289(14) 0.33160(18) 0.0544(7) Uani 1 d . . . O44 O 0.2315(2) 0.25988(10) 0.22265(15) 0.0274(4) Uani 1 d . . . C51 C 0.0747(3) 0.12577(15) 0.2103(2) 0.0333(7) Uani 1 d . . . H51A H 0.0226 0.1699 0.2280 0.040 Uiso 1 calc R . . H51B H 0.1620 0.1283 0.2557 0.040 Uiso 1 calc R . . C52 C -0.0006(4) 0.05375(16) 0.2447(3) 0.0405(8) Uani 1 d . . . O53 O -0.0075(3) 0.05096(13) 0.34382(19) 0.0565(7) Uani 1 d . . . O54 O -0.0479(4) 0.00503(16) 0.1769(2) 0.0751(10) Uani 1 d . . . C61 C 0.4162(3) 0.28393(15) -0.0533(2) 0.0324(7) Uani 1 d . . . H61A H 0.5045 0.2595 -0.0516 0.039 Uiso 1 calc R . . H61B H 0.4217 0.3335 -0.0872 0.039 Uiso 1 calc R . . C62 C 0.3109(3) 0.23650(15) -0.1213(2) 0.0317(7) Uani 1 d . . . O63 O 0.3142(3) 0.23097(12) -0.22065(17) 0.0416(6) Uani 1 d . . . O64 O 0.2206(2) 0.20226(11) -0.07218(16) 0.0316(5) Uani 1 d . . . O100 O 0.2275(3) 0.07892(14) -0.2889(3) 0.0606(7) Uani 1 d D . . H101 H 0.164(3) 0.0586(19) -0.259(3) 0.073 Uiso 1 d D . . H102 H 0.244(4) 0.1231(12) -0.263(3) 0.073 Uiso 1 d D . . O200 O 0.2041(4) 0.11163(18) 0.4899(3) 0.0755(9) Uani 1 d D . . H201 H 0.145(4) 0.088(2) 0.448(3) 0.091 Uiso 1 d D . . H202 H 0.217(5) 0.091(2) 0.5518(17) 0.091 Uiso 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.0261(2) 0.0230(2) 0.0213(2) -0.00155(12) 0.00604(18) -0.00240(14) N1 0.0337(14) 0.0416(13) 0.0221(12) 0.0019(10) 0.0048(12) 0.0072(11) C2 0.0303(19) 0.073(2) 0.0267(17) -0.0017(14) -0.0012(16) 0.0097(15) C3 0.0258(18) 0.088(3) 0.0351(19) -0.0119(17) 0.0011(16) -0.0089(17) C4 0.0353(19) 0.065(2) 0.0308(17) -0.0146(14) 0.0015(16) -0.0226(16) N5 0.0373(15) 0.0340(12) 0.0268(13) -0.0088(9) 0.0131(12) -0.0118(10) C6 0.055(2) 0.0293(14) 0.0367(17) -0.0124(11) 0.0204(17) -0.0160(13) C7 0.0506(19) 0.0231(13) 0.0310(15) -0.0027(10) 0.0153(16) -0.0031(12) N8 0.0344(14) 0.0215(11) 0.0276(12) -0.0007(8) 0.0069(12) -0.0003(9) C9 0.0320(17) 0.0337(14) 0.0273(15) -0.0005(11) 0.0048(14) -0.0006(12) C10 0.0265(16) 0.0312(15) 0.0373(17) 0.0004(11) -0.0011(14) -0.0071(11) N11 0.0332(14) 0.0230(11) 0.0297(13) 0.0011(9) 0.0071(12) -0.0043(9) C12 0.050(2) 0.0215(13) 0.0480(18) -0.0028(12) 0.0189(17) -0.0067(12) C13 0.072(3) 0.0266(15) 0.067(2) 0.0117(14) 0.029(2) 0.0086(15) C14 0.056(2) 0.0460(17) 0.0384(18) 0.0174(14) 0.0208(18) 0.0210(16) C21 0.075(3) 0.0238(14) 0.056(2) 0.0052(13) 0.021(2) 0.0093(15) C22 0.063(3) 0.0465(19) 0.062(2) 0.0100(17) 0.012(2) 0.0223(18) C23 0.0383(19) 0.0499(19) 0.050(2) 0.0059(15) 0.0057(18) 0.0124(15) C41 0.0416(19) 0.0460(17) 0.0310(16) -0.0026(12) 0.0094(16) 0.0134(14) C42 0.0411(18) 0.0268(13) 0.0302(15) -0.0021(11) 0.0052(14) 0.0005(12) O43 0.0782(19) 0.0530(14) 0.0307(12) -0.0155(10) 0.0024(13) 0.0215(13) O44 0.0346(12) 0.0230(9) 0.0251(10) -0.0005(7) 0.0053(10) -0.0007(7) C51 0.0434(18) 0.0328(14) 0.0273(15) -0.0076(11) 0.0190(15) -0.0124(12) C52 0.049(2) 0.0333(15) 0.0435(18) -0.0086(13) 0.0221(17) -0.0136(13) O53 0.092(2) 0.0410(12) 0.0428(13) -0.0044(10) 0.0316(15) -0.0211(13) O54 0.113(3) 0.0687(17) 0.0510(15) -0.0247(13) 0.0374(18) -0.0624(17) C61 0.0344(18) 0.0307(14) 0.0341(16) 0.0047(11) 0.0121(15) -0.0006(11) C62 0.0332(18) 0.0344(15) 0.0287(16) 0.0027(11) 0.0090(15) 0.0045(12) O63 0.0461(15) 0.0549(14) 0.0254(11) -0.0019(9) 0.0100(12) -0.0038(10) O64 0.0324(12) 0.0378(10) 0.0262(10) -0.0052(8) 0.0096(10) -0.0053(8) O100 0.0567(17) 0.0417(14) 0.084(2) 0.0085(13) 0.0110(16) -0.0119(12) O200 0.081(2) 0.0660(19) 0.080(2) 0.0100(16) 0.013(2) -0.0243(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co N8 1.884(3) . ? Co O44 1.887(3) . ? Co O64 1.895(3) . ? Co N1 2.000(3) . ? Co N11 2.005(3) . ? Co N5 2.071(3) . ? N1 C41 1.496(4) . ? N1 C14 1.505(4) . ? N1 C2 1.506(5) . ? C2 C3 1.508(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.516(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N5 1.494(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? N5 C51 1.497(4) . ? N5 C6 1.513(4) . ? C6 C7 1.485(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N8 1.348(4) . ? C7 C21 1.380(5) . ? N8 C9 1.345(4) . ? C9 C23 1.377(5) . ? C9 C10 1.502(4) . ? C10 N11 1.503(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? N11 C12 1.497(4) . ? N11 C61 1.498(4) . ? C12 C13 1.526(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.515(6) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C21 C22 1.389(6) . ? C21 H21 0.9300 . ? C22 C23 1.392(5) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C41 C42 1.512(5) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 O43 1.221(4) . ? C42 O44 1.297(4) . ? C51 C52 1.552(4) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 O53 1.240(4) . ? C52 O54 1.247(4) . ? C61 C62 1.504(5) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 O63 1.241(4) . ? C62 O64 1.290(4) . ? O100 H101 0.852(10) . ? O100 H102 0.846(10) . ? O200 H201 0.843(10) . ? O200 H202 0.846(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N8 Co O44 91.95(10) . . ? N8 Co O64 90.30(10) . . ? O44 Co O64 176.01(8) . . ? N8 Co N1 177.72(10) . . ? O44 Co N1 86.62(10) . . ? O64 Co N1 91.03(10) . . ? N8 Co N11 82.08(13) . . ? O44 Co N11 89.25(9) . . ? O64 Co N11 87.80(9) . . ? N1 Co N11 96.12(14) . . ? N8 Co N5 81.96(14) . . ? O44 Co N5 94.79(9) . . ? O64 Co N5 88.78(9) . . ? N1 Co N5 99.92(14) . . ? N11 Co N5 163.66(10) . . ? C41 N1 C14 110.4(3) . . ? C41 N1 C2 110.1(3) . . ? C14 N1 C2 105.1(2) . . ? C41 N1 Co 107.14(18) . . ? C14 N1 Co 111.7(2) . . ? C2 N1 Co 112.4(2) . . ? N1 C2 C3 116.1(3) . . ? N1 C2 H2A 108.3 . . ? C3 C2 H2A 108.3 . . ? N1 C2 H2B 108.3 . . ? C3 C2 H2B 108.3 . . ? H2A C2 H2B 107.4 . . ? C2 C3 C4 113.5(3) . . ? C2 C3 H3A 108.9 . . ? C4 C3 H3A 108.9 . . ? C2 C3 H3B 108.9 . . ? C4 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? N5 C4 C3 113.3(3) . . ? N5 C4 H4A 108.9 . . ? C3 C4 H4A 108.9 . . ? N5 C4 H4B 108.9 . . ? C3 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? C4 N5 C51 111.5(2) . . ? C4 N5 C6 108.6(2) . . ? C51 N5 C6 108.4(2) . . ? C4 N5 Co 112.9(2) . . ? C51 N5 Co 111.00(16) . . ? C6 N5 Co 103.98(19) . . ? C7 C6 N5 109.4(2) . . ? C7 C6 H6A 109.8 . . ? N5 C6 H6A 109.8 . . ? C7 C6 H6B 109.8 . . ? N5 C6 H6B 109.8 . . ? H6A C6 H6B 108.2 . . ? N8 C7 C21 119.5(3) . . ? N8 C7 C6 112.7(3) . . ? C21 C7 C6 127.8(3) . . ? C9 N8 C7 122.4(3) . . ? C9 N8 Co 118.66(19) . . ? C7 N8 Co 118.9(2) . . ? N8 C9 C23 120.4(3) . . ? N8 C9 C10 112.0(2) . . ? C23 C9 C10 127.7(3) . . ? C9 C10 N11 108.1(2) . . ? C9 C10 H10A 110.1 . . ? N11 C10 H10A 110.1 . . ? C9 C10 H10B 110.1 . . ? N11 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? C12 N11 C61 112.6(2) . . ? C12 N11 C10 106.5(2) . . ? C61 N11 C10 109.9(2) . . ? C12 N11 Co 115.4(2) . . ? C61 N11 Co 106.09(17) . . ? C10 N11 Co 106.23(17) . . ? N11 C12 C13 114.1(3) . . ? N11 C12 H12A 108.7 . . ? C13 C12 H12A 108.7 . . ? N11 C12 H12B 108.7 . . ? C13 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? C14 C13 C12 118.1(3) . . ? C14 C13 H13A 107.8 . . ? C12 C13 H13A 107.8 . . ? C14 C13 H13B 107.8 . . ? C12 C13 H13B 107.8 . . ? H13A C13 H13B 107.1 . . ? N1 C14 C13 117.5(3) . . ? N1 C14 H14A 107.9 . . ? C13 C14 H14A 107.9 . . ? N1 C14 H14B 107.9 . . ? C13 C14 H14B 107.9 . . ? H14A C14 H14B 107.2 . . ? C7 C21 C22 119.0(3) . . ? C7 C21 H21 120.5 . . ? C22 C21 H21 120.5 . . ? C21 C22 C23 120.4(3) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C9 C23 C22 118.3(4) . . ? C9 C23 H23 120.8 . . ? C22 C23 H23 120.8 . . ? N1 C41 C42 112.6(2) . . ? N1 C41 H41A 109.1 . . ? C42 C41 H41A 109.1 . . ? N1 C41 H41B 109.1 . . ? C42 C41 H41B 109.1 . . ? H41A C41 H41B 107.8 . . ? O43 C42 O44 124.2(3) . . ? O43 C42 C41 120.1(3) . . ? O44 C42 C41 115.7(3) . . ? C42 O44 Co 116.97(18) . . ? N5 C51 C52 119.5(2) . . ? N5 C51 H51A 107.4 . . ? C52 C51 H51A 107.4 . . ? N5 C51 H51B 107.4 . . ? C52 C51 H51B 107.4 . . ? H51A C51 H51B 107.0 . . ? O53 C52 O54 125.3(3) . . ? O53 C52 C51 113.1(3) . . ? O54 C52 C51 121.6(3) . . ? N11 C61 C62 112.9(2) . . ? N11 C61 H61A 109.0 . . ? C62 C61 H61A 109.0 . . ? N11 C61 H61B 109.0 . . ? C62 C61 H61B 109.0 . . ? H61A C61 H61B 107.8 . . ? O63 C62 O64 122.7(3) . . ? O63 C62 C61 119.7(3) . . ? O64 C62 C61 117.7(3) . . ? C62 O64 Co 114.81(19) . . ? H101 O100 H102 109.6(17) . . ? H201 O200 H202 110.8(18) . . ? 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 C9 N8 C7 C6 -174.0(3) . . . . ? N8 C7 C6 N5 -28.5(3) . . . . ? C7 C6 N5 C4 158.0(2) . . . . ? C6 N5 C4 C3 -168.8(3) . . . . ? N5 C4 C3 C2 71.8(4) . . . . ? C4 C3 C2 N1 -72.3(4) . . . . ? C3 C2 N1 C14 175.2(3) . . . . ? C2 N1 C14 C13 174.5(3) . . . . ? N1 C14 C13 C12 38.7(4) . . . . ? C14 C13 C12 N11 28.8(4) . . . . ? C13 C12 N11 C10 -179.0(3) . . . . ? C12 N11 C10 C9 161.1(2) . . . . ? N11 C10 C9 N8 -27.1(3) . . . . ? C10 C9 N8 C7 179.0(2) . . . . ? C9 N8 C7 C6 -174.0(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _diffrn_measured_fraction_theta_max 0.777 _diffrn_reflns_theta_full 25.92 _diffrn_measured_fraction_theta_full 0.777 _refine_diff_density_max 0.387 _refine_diff_density_min -0.664 _refine_diff_density_rms 0.057