Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'A. M. Funston' 'W. D. Mc Fadyen' 'P. A. Tregloan' _publ_contact_author_name 'Dr Peter A Tregloan' _publ_contact_author_address ; Dr Peter A Tregloan School of Chemistry University of Melbourne Victoria 3010 AUSTRALIA ; _publ_contact_author_email 'PATREG@UNIMELB.EDU.AU' _publ_section_title ; A Pulse Radiolysis Study of the Rate of Ligand Dissociation from Mixed Ligand Cobalt(II) Complexes ; data_af8 _database_code_CSD 169187 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'bis-(ammonia)bis-(2,2'-bipyridine)cobalt(III) perchlorate' ; _chemical_name_common '[Co(bipy)2(NH3)2](ClO4)3' _chemical_melting_point ? _chemical_formula_moiety C20H22N6O12Cl3Co _chemical_formula_sum 'C20 H22 Cl3 Co N6 O12' _chemical_formula_weight 703.72 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21 /c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.793(3) _cell_length_b 13.978(3) _cell_length_c 17.462(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.69(2) _cell_angle_gamma 90.00 _cell_volume 2726.7(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(1) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8.37 _cell_measurement_theta_max 18.72 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.14 _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 1432 _exptl_absorpt_coefficient_mu 0.997 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_process_details 'Sheldrick, 1976' _exptl_absorpt_correction_T_min 0.7517 _exptl_absorpt_correction_T_max 0.8272 _exptl_special_details ; 'bis-(ammonia)bis-(2,2'-bipyridine)cobalt(III) perchlorate' ; _diffrn_ambient_temperature 293(1) _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 'Enraf-Nonius CAD4-MachS Diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% none _diffrn_reflns_number 7049 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 26.97 _reflns_number_total 5930 _reflns_number_gt 4083 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD-4 Software' _computing_data_reduction 'PROCESS_DATA (Gable et al., 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for WINDOWS (Farrugia, 1997)' _computing_publication_material SHELXL _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^)+(0.1146P)^2^+1.7970P] 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 5930 _refine_ls_number_parameters 472 _refine_ls_number_restraints 144 _refine_ls_R_factor_all 0.0960 _refine_ls_R_factor_gt 0.0650 _refine_ls_wR_factor_ref 0.1928 _refine_ls_wR_factor_gt 0.1755 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.076 _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 Co Co 0.20910(5) 0.08687(4) 0.20080(4) 0.03073(19) Uani 1 1 d . . . N1 N 0.2458(4) -0.0490(3) 0.2085(2) 0.0370(8) Uani 1 1 d . . . C2 C 0.3245(4) -0.0759(3) 0.1713(3) 0.0378(10) Uani 1 1 d . . . C3 C 0.3512(5) -0.1711(4) 0.1644(4) 0.0547(14) Uani 1 1 d . . . H3 H 0.4045 -0.1884 0.1375 0.07(2) Uiso 1 1 calc R . . C4 C 0.2986(6) -0.2398(4) 0.1976(4) 0.0644(17) Uani 1 1 d . . . H4 H 0.3144 -0.3042 0.1925 0.059(17) Uiso 1 1 calc R . . C5 C 0.2229(6) -0.2124(4) 0.2382(4) 0.0656(17) Uani 1 1 d . . . H5 H 0.1887 -0.2578 0.2630 0.066(18) Uiso 1 1 calc R . . C6 C 0.1974(5) -0.1163(4) 0.2423(4) 0.0534(14) Uani 1 1 d . . . H6 H 0.1447 -0.0980 0.2695 0.043(14) Uiso 1 1 calc R . . N1' N 0.3364(3) 0.0907(3) 0.1517(2) 0.0343(8) Uani 1 1 d . . . C2' C 0.3798(4) 0.0044(3) 0.1418(3) 0.0380(10) Uani 1 1 d . . . C3' C 0.4745(5) -0.0055(4) 0.1110(3) 0.0474(12) Uani 1 1 d . . . H3' H 0.5032 -0.0658 0.1042 0.047(15) Uiso 1 1 calc R . . C4' C 0.5249(5) 0.0754(4) 0.0907(3) 0.0525(13) Uani 1 1 d . . . H4' H 0.5881 0.0705 0.0699 0.062(17) Uiso 1 1 calc R . . C5' C 0.4812(5) 0.1628(4) 0.1015(4) 0.0556(14) Uani 1 1 d . . . H5' H 0.5154 0.2182 0.0891 0.12(3) Uiso 1 1 calc R . . C6' C 0.3867(5) 0.1687(4) 0.1307(3) 0.0473(12) Uani 1 1 d . . . H6' H 0.3561 0.2287 0.1361 0.048(15) Uiso 1 1 calc R . . N1* N 0.0926(3) 0.0742(2) 0.2573(3) 0.0366(8) Uani 1 1 d . . . C2* C 0.1399(4) 0.0790(3) 0.3387(3) 0.0396(10) Uani 1 1 d . . . C3* C 0.0692(5) 0.0697(4) 0.3875(4) 0.0582(15) Uani 1 1 d . . . H3* H 0.1030 0.0740 0.4434 0.051(16) Uiso 1 1 calc R . . C4* C -0.0516(6) 0.0540(5) 0.3532(5) 0.0649(17) Uani 1 1 d . . . H4* H -0.1005 0.0483 0.3855 0.08(2) Uiso 1 1 calc R . . C5* C -0.0990(5) 0.0470(4) 0.2710(4) 0.0594(15) Uani 1 1 d . . . H5* H -0.1800 0.0342 0.2469 0.048(15) Uiso 1 1 calc R . . C6* C -0.0260(4) 0.0590(4) 0.2242(4) 0.0471(12) Uani 1 1 d . . . H6* H -0.0593 0.0565 0.1682 0.037(13) Uiso 1 1 calc R . . N1'* N 0.3190(3) 0.1067(2) 0.3094(2) 0.0309(8) Uani 1 1 d . . . C2'* C 0.2695(4) 0.0947(3) 0.3688(3) 0.0361(10) Uani 1 1 d . . . C3'* C 0.3362(5) 0.0988(4) 0.4488(3) 0.0493(12) Uani 1 1 d . . . H3'* H 0.3004 0.0906 0.4886 0.054(16) Uiso 1 1 calc R . . C4'* C 0.4585(5) 0.1154(4) 0.4696(3) 0.0475(12) Uani 1 1 d . . . H4'* H 0.5063 0.1169 0.5235 0.040(13) Uiso 1 1 calc R . . C5'* C 0.5080(4) 0.1299(4) 0.4086(3) 0.0425(11) Uani 1 1 d . . . H5'* H 0.5893 0.1428 0.4210 0.07(2) Uiso 1 1 calc R . . C6'* C 0.4355(4) 0.1247(3) 0.3297(3) 0.0374(10) Uani 1 1 d . . . H6'* H 0.4691 0.1343 0.2889 0.033(12) Uiso 1 1 calc R . . N3 N 0.1705(4) 0.2229(3) 0.1886(3) 0.0496(11) Uani 1 1 d . . . H3A H 0.2106 0.2536 0.2338 0.055 Uiso 1 1 calc R . . H3B H 0.0922 0.2308 0.1789 0.055 Uiso 1 1 calc R . . H3C H 0.1909 0.2464 0.1475 0.055 Uiso 1 1 calc R . . N4 N 0.0948(4) 0.0625(4) 0.0934(3) 0.0540(11) Uani 1 1 d . . . H4A H 0.0743 0.0010 0.0891 0.059 Uiso 1 1 calc R . . H4B H 0.1283 0.0772 0.0559 0.059 Uiso 1 1 calc R . . H4C H 0.0298 0.0983 0.0863 0.059 Uiso 1 1 calc R . . Cl1 Cl -0.36160(11) -0.07434(8) 0.32044(8) 0.0416(3) Uani 1 1 d D . . O11A O -0.456(3) -0.081(3) 0.355(3) 0.042(7) Uani 0.32(12) 1 d PDU A 1 O12A O -0.250(2) -0.098(3) 0.381(2) 0.043(7) Uani 0.32(12) 1 d PDU A 1 O13A O -0.355(4) 0.0209(17) 0.292(3) 0.054(12) Uani 0.32(12) 1 d PDU A 1 O14A O -0.383(4) -0.140(3) 0.254(2) 0.047(8) Uani 0.32(12) 1 d PDU A 1 O11B O -0.2612(19) -0.0997(16) 0.3891(13) 0.059(4) Uani 0.68(12) 1 d PD A 2 O12B O -0.3537(18) 0.0237(7) 0.2993(14) 0.062(6) Uani 0.68(12) 1 d PD A 2 O13B O -0.4705(19) -0.0900(13) 0.338(2) 0.055(4) Uani 0.68(12) 1 d PD A 2 O14B O -0.361(3) -0.1338(15) 0.2530(9) 0.056(4) Uani 0.68(12) 1 d PD A 2 Cl2A Cl 0.8246(10) 0.2906(7) 0.0596(6) 0.090(3) Uani 0.375(9) 1 d PDU B 1 O21A O 0.8325(17) 0.3087(12) -0.0167(9) 0.109(4) Uiso 0.375(9) 1 d PD B 1 O22A O 0.7459(16) 0.2027(10) 0.0450(11) 0.109(4) Uiso 0.375(9) 1 d PD B 1 O23A O 0.9203(14) 0.2953(12) 0.1279(9) 0.109(4) Uiso 0.375(9) 1 d PD B 1 O24A O 0.7413(13) 0.3595(11) 0.0778(10) 0.109(4) Uiso 0.375(9) 1 d PD B 1 Cl2B Cl 0.8327(4) 0.2556(5) 0.0471(4) 0.0822(17) Uani 0.625(9) 1 d PDU B 2 O21B O 0.8238(12) 0.3408(8) 0.0020(8) 0.131(3) Uiso 0.625(9) 1 d PD B 2 O22B O 0.8735(10) 0.1752(8) 0.0144(7) 0.131(3) Uiso 0.625(9) 1 d PD B 2 O23B O 0.9107(11) 0.2613(9) 0.1276(7) 0.131(3) Uiso 0.625(9) 1 d PD B 2 O24B O 0.7160(10) 0.2398(9) 0.0535(8) 0.131(3) Uiso 0.625(9) 1 d PD B 2 Cl3 Cl 0.8255(2) 0.84895(12) 0.08615(10) 0.0779(5) Uani 1 1 d D . . O31A O 0.8315(12) 0.7807(9) 0.0244(7) 0.080(4) Uani 0.697(13) 1 d PDU C 1 O32A O 0.8282(11) 0.9407(5) 0.0596(5) 0.104(4) Uani 0.697(13) 1 d PDU C 1 O33A O 0.8988(10) 0.8231(8) 0.1603(5) 0.114(4) Uani 0.697(13) 1 d PDU C 1 O34A O 0.7057(9) 0.8348(8) 0.0931(6) 0.129(4) Uani 0.697(13) 1 d PDU C 1 O31B O 0.9484(14) 0.8907(15) 0.0977(12) 0.110(8) Uani 0.303(13) 1 d PDU C 2 O32B O 0.752(2) 0.9315(14) 0.0733(14) 0.119(9) Uani 0.303(13) 1 d PDU C 2 O33B O 0.800(2) 0.7919(19) 0.0182(13) 0.068(7) Uani 0.303(13) 1 d PDU C 2 O34B O 0.833(2) 0.8077(16) 0.1566(11) 0.106(8) Uani 0.303(13) 1 d PDU C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.0289(3) 0.0298(3) 0.0343(3) 0.0019(2) 0.0112(2) -0.0015(2) N1 0.047(2) 0.0290(17) 0.039(2) -0.0041(16) 0.0188(18) -0.0045(16) C2 0.043(3) 0.033(2) 0.038(2) -0.0018(19) 0.014(2) 0.0019(19) C3 0.063(4) 0.035(3) 0.073(4) -0.010(3) 0.032(3) 0.003(2) C4 0.080(4) 0.031(3) 0.091(5) -0.009(3) 0.039(4) 0.000(3) C5 0.090(5) 0.032(3) 0.089(5) -0.001(3) 0.048(4) -0.008(3) C6 0.073(4) 0.034(2) 0.068(4) -0.005(2) 0.043(3) -0.006(2) N1' 0.039(2) 0.0356(19) 0.0310(19) 0.0039(16) 0.0145(16) -0.0011(16) C2' 0.042(2) 0.044(3) 0.029(2) -0.0007(19) 0.0132(19) 0.000(2) C3' 0.049(3) 0.054(3) 0.043(3) 0.000(2) 0.021(2) 0.008(2) C4' 0.051(3) 0.072(4) 0.043(3) 0.007(3) 0.026(2) 0.004(3) C5' 0.062(4) 0.059(3) 0.057(3) 0.011(3) 0.034(3) -0.010(3) C6' 0.055(3) 0.042(3) 0.052(3) 0.007(2) 0.026(3) -0.006(2) N1* 0.0316(19) 0.0302(18) 0.051(2) -0.0010(17) 0.0177(17) -0.0023(15) C2* 0.039(2) 0.037(2) 0.049(3) -0.003(2) 0.023(2) -0.0043(19) C3* 0.054(3) 0.068(4) 0.063(4) -0.004(3) 0.034(3) -0.008(3) C4* 0.058(4) 0.067(4) 0.087(5) -0.007(3) 0.048(4) -0.009(3) C5* 0.036(3) 0.059(3) 0.089(5) -0.007(3) 0.029(3) -0.007(2) C6* 0.034(2) 0.049(3) 0.059(3) -0.001(2) 0.015(2) -0.006(2) N1'* 0.0294(18) 0.0292(17) 0.036(2) -0.0016(14) 0.0132(16) 0.0010(13) C2'* 0.037(2) 0.038(2) 0.037(2) -0.0008(19) 0.0170(19) -0.0001(19) C3'* 0.052(3) 0.059(3) 0.041(3) -0.004(2) 0.020(2) -0.005(2) C4'* 0.054(3) 0.046(3) 0.037(3) -0.004(2) 0.007(2) -0.002(2) C5'* 0.034(2) 0.045(3) 0.045(3) -0.003(2) 0.009(2) 0.000(2) C6'* 0.032(2) 0.040(2) 0.041(3) -0.002(2) 0.014(2) -0.0019(19) N3 0.032(2) 0.039(2) 0.080(3) 0.011(2) 0.020(2) 0.0056(17) N4 0.048(3) 0.069(3) 0.044(3) 0.006(2) 0.012(2) -0.010(2) Cl1 0.0466(6) 0.0365(6) 0.0484(7) 0.0043(5) 0.0248(5) 0.0034(5) O11A 0.047(9) 0.051(11) 0.037(10) 0.007(8) 0.025(7) -0.010(6) O12A 0.040(10) 0.046(11) 0.045(10) -0.004(7) 0.018(7) 0.005(7) O13A 0.054(15) 0.054(15) 0.058(13) 0.010(8) 0.022(9) -0.005(9) O14A 0.045(11) 0.043(10) 0.053(10) -0.006(7) 0.018(7) 0.008(7) O11B 0.065(7) 0.068(7) 0.048(6) 0.004(5) 0.025(5) 0.007(5) O12B 0.065(9) 0.031(7) 0.109(15) 0.013(5) 0.055(9) 0.005(5) O13B 0.053(5) 0.057(5) 0.065(9) -0.014(6) 0.033(6) -0.015(4) O14B 0.061(9) 0.066(7) 0.044(5) -0.005(4) 0.020(5) 0.015(5) Cl2A 0.126(6) 0.080(5) 0.044(3) -0.002(3) 0.000(3) 0.009(4) Cl2B 0.0523(18) 0.120(4) 0.074(3) 0.037(3) 0.0192(18) 0.020(2) Cl3 0.1153(16) 0.0607(10) 0.0524(9) 0.0030(7) 0.0193(10) -0.0110(9) O31A 0.089(7) 0.071(5) 0.074(6) -0.011(4) 0.018(5) -0.006(5) O32A 0.172(9) 0.067(5) 0.076(5) -0.003(4) 0.045(5) -0.019(5) O33A 0.116(7) 0.128(7) 0.080(6) 0.009(5) 0.006(5) -0.013(6) O34A 0.147(8) 0.139(8) 0.110(7) -0.024(5) 0.054(6) 0.004(6) O31B 0.102(10) 0.112(11) 0.121(11) -0.033(8) 0.043(8) -0.060(8) O32B 0.112(12) 0.099(11) 0.130(12) -0.004(9) 0.013(9) 0.033(9) O33B 0.068(10) 0.075(11) 0.053(10) -0.016(7) 0.009(7) -0.006(8) O34B 0.127(12) 0.111(11) 0.094(11) 0.008(8) 0.053(9) -0.023(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 Co N1* 1.939(4) . Y Co N1 1.943(4) . Y Co N1'* 1.944(4) . Y Co N3 1.951(4) . Y Co N1' 1.953(4) . Y Co N4 1.957(4) . Y N1 C6 1.331(6) . ? N1 C2 1.345(6) . ? C2 C3 1.382(6) . ? C2 C2' 1.472(6) . ? C3 C4 1.368(8) . ? C3 H3 0.9300 . ? C4 C5 1.360(8) . ? C4 H4 0.9300 . ? C5 C6 1.384(7) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? N1' C2' 1.344(6) . ? N1' C6' 1.347(6) . ? C2' C3' 1.394(7) . ? C3' C4' 1.375(8) . ? C3' H3' 0.9300 . ? C4' C5' 1.363(8) . ? C4' H4' 0.9300 . ? C5' C6' 1.368(7) . ? C5' H5' 0.9300 . ? C6' H6' 0.9300 . ? N1* C6* 1.349(6) . ? N1* C2* 1.352(6) . ? C2* C3* 1.376(7) . ? C2* C2'* 1.465(6) . ? C3* C4* 1.375(9) . ? C3* H3* 0.9300 . ? C4* C5* 1.368(9) . ? C4* H4* 0.9300 . ? C5* C6* 1.373(8) . ? C5* H5* 0.9300 . ? C6* H6* 0.9300 . ? N1'* C6'* 1.329(6) . ? N1'* C2'* 1.353(5) . ? C2'* C3'* 1.367(7) . ? C3'* C4'* 1.390(8) . ? C3'* H3'* 0.9300 . ? C4'* C5'* 1.382(7) . ? C4'* H4'* 0.9300 . ? C5'* C6'* 1.372(7) . ? C5'* H5'* 0.9300 . ? C6'* H6'* 0.9300 . ? N3 H3A 0.8900 . ? N3 H3B 0.8900 . ? N3 H3C 0.8900 . ? N4 H4A 0.8900 . ? N4 H4B 0.8900 . ? N4 H4C 0.8900 . ? Cl1 O13B 1.427(9) . ? Cl1 O11A 1.429(16) . ? Cl1 O12B 1.430(8) . ? Cl1 O13A 1.433(16) . ? Cl1 O11B 1.433(10) . ? Cl1 O14A 1.438(16) . ? Cl1 O12A 1.439(15) . ? Cl1 O14B 1.445(9) . ? Cl2A O23A 1.356(14) . ? Cl2A O21A 1.389(14) . ? Cl2A O24A 1.480(14) . ? Cl2A O22A 1.511(14) . ? Cl2B O21B 1.412(11) . ? Cl2B O22B 1.412(11) . ? Cl2B O23B 1.414(11) . ? Cl2B O24B 1.434(11) . ? Cl3 O34B 1.336(14) . ? Cl3 O33A 1.355(8) . ? Cl3 O32A 1.368(7) . ? Cl3 O33B 1.381(14) . ? Cl3 O32B 1.414(14) . ? Cl3 O31A 1.459(9) . ? Cl3 O34A 1.469(9) . ? Cl3 O31B 1.516(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1* Co N1 93.10(15) . . Y N1* Co N1'* 82.86(16) . . Y N1 Co N1'* 90.42(16) . . Y N1* Co N3 88.04(17) . . Y N1 Co N3 177.82(19) . . Y N1'* Co N3 91.57(18) . . Y N1* Co N1' 174.31(16) . . Y N1 Co N1' 82.65(15) . . Y N1'* Co N1' 93.34(15) . . Y N3 Co N1' 96.33(17) . . Y N1* Co N4 95.12(18) . . Y N1 Co N4 88.08(19) . . Y N1'* Co N4 177.42(17) . . Y N3 Co N4 90.0(2) . . Y N1' Co N4 88.54(18) . . Y C6 N1 C2 118.5(4) . . ? C6 N1 Co 127.1(4) . . ? C2 N1 Co 114.3(3) . . ? N1 C2 C3 121.5(5) . . ? N1 C2 C2' 114.1(4) . . ? C3 C2 C2' 124.3(5) . . ? C4 C3 C2 119.4(5) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C5 C4 C3 119.1(5) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C4 C5 C6 119.3(5) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? N1 C6 C5 122.1(5) . . ? N1 C6 H6 119.0 . . ? C5 C6 H6 119.0 . . ? C2' N1' C6' 118.2(4) . . ? C2' N1' Co 114.2(3) . . ? C6' N1' Co 127.6(3) . . ? N1' C2' C3' 121.6(4) . . ? N1' C2' C2 114.2(4) . . ? C3' C2' C2 124.1(4) . . ? C4' C3' C2' 118.9(5) . . ? C4' C3' H3' 120.5 . . ? C2' C3' H3' 120.5 . . ? C5' C4' C3' 119.2(5) . . ? C5' C4' H4' 120.4 . . ? C3' C4' H4' 120.4 . . ? C4' C5' C6' 119.7(5) . . ? C4' C5' H5' 120.2 . . ? C6' C5' H5' 120.2 . . ? N1' C6' C5' 122.3(5) . . ? N1' C6' H6' 118.8 . . ? C5' C6' H6' 118.8 . . ? C6* N1* C2* 118.7(4) . . ? C6* N1* Co 127.1(4) . . ? C2* N1* Co 114.2(3) . . ? N1* C2* C3* 121.2(5) . . ? N1* C2* C2'* 114.5(4) . . ? C3* C2* C2'* 124.2(5) . . ? C4* C3* C2* 119.7(6) . . ? C4* C3* H3* 120.2 . . ? C2* C3* H3* 120.2 . . ? C5* C4* C3* 119.1(6) . . ? C5* C4* H4* 120.5 . . ? C3* C4* H4* 120.5 . . ? C4* C5* C6* 119.5(5) . . ? C4* C5* H5* 120.2 . . ? C6* C5* H5* 120.2 . . ? N1* C6* C5* 121.7(5) . . ? N1* C6* H6* 119.1 . . ? C5* C6* H6* 119.1 . . ? C6'* N1'* C2'* 118.8(4) . . ? C6'* N1'* Co 126.6(3) . . ? C2'* N1'* Co 114.5(3) . . ? N1'* C2'* C3'* 122.0(4) . . ? N1'* C2'* C2* 113.6(4) . . ? C3'* C2'* C2* 124.4(4) . . ? C2'* C3'* C4'* 118.9(5) . . ? C2'* C3'* H3'* 120.6 . . ? C4'* C3'* H3'* 120.6 . . ? C5'* C4'* C3'* 118.9(5) . . ? C5'* C4'* H4'* 120.6 . . ? C3'* C4'* H4'* 120.6 . . ? C6'* C5'* C4'* 119.0(5) . . ? C6'* C5'* H5'* 120.5 . . ? C4'* C5'* H5'* 120.5 . . ? N1'* C6'* C5'* 122.4(4) . . ? N1'* C6'* H6'* 118.8 . . ? C5'* C6'* H6'* 118.8 . . ? Co N3 H3A 109.5 . . ? Co N3 H3B 109.5 . . ? H3A N3 H3B 109.5 . . ? Co N3 H3C 109.5 . . ? H3A N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? Co N4 H4A 109.5 . . ? Co N4 H4B 109.5 . . ? H4A N4 H4B 109.5 . . ? Co N4 H4C 109.5 . . ? H4A N4 H4C 109.5 . . ? H4B N4 H4C 109.5 . . ? O13B Cl1 O11A 12.8(19) . . ? O13B Cl1 O12B 109.8(7) . . ? O11A Cl1 O12B 107(2) . . ? O13B Cl1 O13A 111(2) . . ? O11A Cl1 O13A 110.0(14) . . ? O12B Cl1 O13A 5(3) . . ? O13B Cl1 O11B 110.1(8) . . ? O11A Cl1 O11B 100.3(18) . . ? O12B Cl1 O11B 110.4(8) . . ? O13A Cl1 O11B 114(2) . . ? O13B Cl1 O14A 98(2) . . ? O11A Cl1 O14A 109.6(14) . . ? O12B Cl1 O14A 115(2) . . ? O13A Cl1 O14A 109.3(15) . . ? O11B Cl1 O14A 114(2) . . ? O13B Cl1 O12A 119(2) . . ? O11A Cl1 O12A 109.6(14) . . ? O12B Cl1 O12A 107(2) . . ? O13A Cl1 O12A 109.6(14) . . ? O11B Cl1 O12A 9(2) . . ? O14A Cl1 O12A 108.8(14) . . ? O13B Cl1 O14B 109.1(8) . . ? O11A Cl1 O14B 121.1(19) . . ? O12B Cl1 O14B 108.8(8) . . ? O13A Cl1 O14B 104(2) . . ? O11B Cl1 O14B 108.6(8) . . ? O14A Cl1 O14B 11(2) . . ? O12A Cl1 O14B 102(2) . . ? O23A Cl2A O21A 122.8(13) . . ? O23A Cl2A O24A 101.6(10) . . ? O21A Cl2A O24A 109.9(11) . . ? O23A Cl2A O22A 118.8(11) . . ? O21A Cl2A O22A 102.3(10) . . ? O24A Cl2A O22A 98.7(10) . . ? O21B Cl2B O22B 114.8(8) . . ? O21B Cl2B O23B 114.5(8) . . ? O22B Cl2B O23B 104.4(7) . . ? O21B Cl2B O24B 105.8(8) . . ? O22B Cl2B O24B 111.7(9) . . ? O23B Cl2B O24B 105.4(8) . . ? O34B Cl3 O33A 34.2(9) . . ? O34B Cl3 O32A 135.7(11) . . ? O33A Cl3 O32A 119.8(6) . . ? O34B Cl3 O33B 118.4(13) . . ? O33A Cl3 O33B 124.2(14) . . ? O32A Cl3 O33B 105.8(14) . . ? O34B Cl3 O32B 110.7(12) . . ? O33A Cl3 O32B 122.6(11) . . ? O32A Cl3 O32B 42.3(10) . . ? O33B Cl3 O32B 112.5(12) . . ? O34B Cl3 O31A 113.2(13) . . ? O33A Cl3 O31A 111.4(7) . . ? O32A Cl3 O31A 110.5(6) . . ? O33B Cl3 O31A 15.1(14) . . ? O32B Cl3 O31A 126.0(12) . . ? O34B Cl3 O34A 69.2(10) . . ? O33A Cl3 O34A 102.8(6) . . ? O32A Cl3 O34A 106.4(7) . . ? O33B Cl3 O34A 92.7(12) . . ? O32B Cl3 O34A 64.5(11) . . ? O31A Cl3 O34A 104.4(6) . . ? O34B Cl3 O31B 105.5(11) . . ? O33A Cl3 O31B 71.6(9) . . ? O32A Cl3 O31B 63.8(9) . . ? O33B Cl3 O31B 105.5(12) . . ? O32B Cl3 O31B 102.4(11) . . ? O31A Cl3 O31B 94.5(10) . . ? O34A Cl3 O31B 160.9(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 N1* Co N1 C6 0.7(5) . . . . ? N1'* Co N1 C6 83.6(5) . . . . ? N3 Co N1 C6 -121(4) . . . . ? N1' Co N1 C6 176.9(5) . . . . ? N4 Co N1 C6 -94.3(5) . . . . ? N1* Co N1 C2 177.0(3) . . . . ? N1'* Co N1 C2 -100.2(3) . . . . ? N3 Co N1 C2 55(4) . . . . ? N1' Co N1 C2 -6.8(3) . . . . ? N4 Co N1 C2 81.9(4) . . . . ? C6 N1 C2 C3 3.0(7) . . . . ? Co N1 C2 C3 -173.6(4) . . . . ? C6 N1 C2 C2' -175.4(5) . . . . ? Co N1 C2 C2' 8.0(5) . . . . ? N1 C2 C3 C4 -1.4(9) . . . . ? C2' C2 C3 C4 176.8(5) . . . . ? C2 C3 C4 C5 -1.4(10) . . . . ? C3 C4 C5 C6 2.5(11) . . . . ? C2 N1 C6 C5 -1.9(9) . . . . ? Co N1 C6 C5 174.3(5) . . . . ? C4 C5 C6 N1 -0.9(10) . . . . ? N1* Co N1' C2' 46.2(17) . . . . ? N1 Co N1' C2' 4.3(3) . . . . ? N1'* Co N1' C2' 94.3(3) . . . . ? N3 Co N1' C2' -173.8(3) . . . . ? N4 Co N1' C2' -84.0(4) . . . . ? N1* Co N1' C6' -130.9(15) . . . . ? N1 Co N1' C6' -172.9(4) . . . . ? N1'* Co N1' C6' -82.9(4) . . . . ? N3 Co N1' C6' 9.1(4) . . . . ? N4 Co N1' C6' 98.9(4) . . . . ? C6' N1' C2' C3' 0.3(7) . . . . ? Co N1' C2' C3' -177.1(4) . . . . ? C6' N1' C2' C2 176.2(4) . . . . ? Co N1' C2' C2 -1.2(5) . . . . ? N1 C2 C2' N1' -4.5(6) . . . . ? C3 C2 C2' N1' 177.2(5) . . . . ? N1 C2 C2' C3' 171.4(4) . . . . ? C3 C2 C2' C3' -7.0(8) . . . . ? N1' C2' C3' C4' 0.3(8) . . . . ? C2 C2' C3' C4' -175.2(5) . . . . ? C2' C3' C4' C5' 0.2(8) . . . . ? C3' C4' C5' C6' -1.3(9) . . . . ? C2' N1' C6' C5' -1.5(8) . . . . ? Co N1' C6' C5' 175.6(4) . . . . ? C4' C5' C6' N1' 2.0(9) . . . . ? N1 Co N1* C6* -91.4(4) . . . . ? N1'* Co N1* C6* 178.5(4) . . . . ? N3 Co N1* C6* 86.7(4) . . . . ? N1' Co N1* C6* -133.0(15) . . . . ? N4 Co N1* C6* -3.1(4) . . . . ? N1 Co N1* C2* 86.6(3) . . . . ? N1'* Co N1* C2* -3.5(3) . . . . ? N3 Co N1* C2* -95.3(3) . . . . ? N1' Co N1* C2* 45.0(17) . . . . ? N4 Co N1* C2* 174.9(3) . . . . ? C6* N1* C2* C3* -0.8(7) . . . . ? Co N1* C2* C3* -178.9(4) . . . . ? C6* N1* C2* C2'* 179.3(4) . . . . ? Co N1* C2* C2'* 1.2(5) . . . . ? N1* C2* C3* C4* 0.8(8) . . . . ? C2'* C2* C3* C4* -179.3(5) . . . . ? C2* C3* C4* C5* 0.7(9) . . . . ? C3* C4* C5* C6* -2.2(10) . . . . ? C2* N1* C6* C5* -0.9(7) . . . . ? Co N1* C6* C5* 177.0(4) . . . . ? C4* C5* C6* N1* 2.4(9) . . . . ? N1* Co N1'* C6'* -178.7(4) . . . . ? N1 Co N1'* C6'* 88.2(4) . . . . ? N3 Co N1'* C6'* -90.9(4) . . . . ? N1' Co N1'* C6'* 5.5(4) . . . . ? N4 Co N1'* C6'* 143(4) . . . . ? N1* Co N1'* C2'* 5.3(3) . . . . ? N1 Co N1'* C2'* -87.8(3) . . . . ? N3 Co N1'* C2'* 93.1(3) . . . . ? N1' Co N1'* C2'* -170.4(3) . . . . ? N4 Co N1'* C2'* -33(4) . . . . ? C6'* N1'* C2'* C3'* -1.3(7) . . . . ? Co N1'* C2'* C3'* 174.9(4) . . . . ? C6'* N1'* C2'* C2* 177.7(4) . . . . ? Co N1'* C2'* C2* -6.0(5) . . . . ? N1* C2* C2'* N1'* 3.2(6) . . . . ? C3* C2* C2'* N1'* -176.7(5) . . . . ? N1* C2* C2'* C3'* -177.8(5) . . . . ? C3* C2* C2'* C3'* 2.3(8) . . . . ? N1'* C2'* C3'* C4'* -0.2(8) . . . . ? C2* C2'* C3'* C4'* -179.1(5) . . . . ? C2'* C3'* C4'* C5'* 1.7(8) . . . . ? C3'* C4'* C5'* C6'* -1.7(7) . . . . ? C2'* N1'* C6'* C5'* 1.3(7) . . . . ? Co N1'* C6'* C5'* -174.5(3) . . . . ? C4'* C5'* C6'* N1'* 0.2(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3A O34B 0.89 2.26 2.963(15) 135.3 2_645 N3 H3A O14B 0.89 2.32 2.94(3) 125.9 2 N3 H3A O14A 0.89 2.47 3.06(4) 123.7 2 N3 H3A O33A 0.89 2.75 3.313(12) 122.4 2_645 N3 H3A O34A 0.89 3.08 3.942(12) 163.8 2_645 N3 H3A Cl3 0.89 3.56 4.297(5) 141.5 2_645 N3 H3B O23B 0.89 2.08 2.952(13) 165.3 1_455 N3 H3B O23A 0.89 2.14 2.974(16) 156.9 1_455 N3 H3B Cl2B 0.89 3.21 3.984(6) 147.5 1_455 N3 H3B O22B 0.89 3.28 3.890(13) 127.8 1_455 N3 H3B Cl2A 0.89 3.28 4.089(11) 151.6 1_455 N3 H3C O12A 0.89 2.38 3.05(4) 132.4 2 N3 H3C O11B 0.89 2.46 3.17(3) 137.0 2 N3 H3C O31A 0.89 2.95 3.711(12) 144.5 3_665 N3 H3C O33B 0.89 2.97 3.74(2) 145.1 3_665 N3 H3C Cl1 0.89 3.15 3.656(4) 118.2 2 N4 H4A O31B 0.89 2.18 2.973(15) 148.3 1_445 N4 H4A O32A 0.89 2.91 3.456(12) 121.6 1_445 N4 H4A O22B 0.89 3.23 3.896(11) 133.5 3_655 N4 H4A N4 0.89 3.29 3.744(9) 113.9 3 N4 H4B O32A 0.89 2.25 3.085(10) 156.4 3_665 N4 H4B O33B 0.89 2.53 3.32(3) 147.1 3_665 N4 H4B O31A 0.89 2.56 3.306(15) 141.7 3_665 N4 H4B O31B 0.89 2.58 3.28(2) 135.6 3_665 N4 H4B Cl3 0.89 2.90 3.759(5) 164.2 3_665 N4 H4B O32B 0.89 3.02 3.88(3) 164.4 3_665 N4 H4C O22B 0.89 2.16 2.981(12) 154.0 1_455 N4 H4C O23B 0.89 2.89 3.690(14) 151.1 1_455 N4 H4C Cl2B 0.89 3.11 3.986(8) 167.7 1_455 N4 H4C O23A 0.89 3.22 3.998(19) 147.0 1_455 N4 H4C O22A 0.89 3.51 4.39(2) 169.9 1_455 N4 H4C Cl2A 0.89 3.55 4.411(12) 164.9 1_455 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.228 _refine_diff_density_min -0.733 _refine_diff_density_rms 0.104 #===END data_af9 _database_code_CSD 169188 _audit_creation_method shelxl-97 _chemical_name_systematic ; tetra(ammino)(2,2'-bipyridine)cobalt(III) perchlorate hydrate ; _chemical_name_common '[Co(bipy)(NH3)4](ClO4)2.5(Cl)0.5.1.5H2O' _chemical_melting_point ? _chemical_formula_moiety C10H23N6Cl3O11.5Co _chemical_formula_sum 'c10 h20 cl3 co n6 o11.50' _chemical_formula_weight 573.60 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' 'cl' 'cl' 0.1484 0.1585 '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' 'n' 'n' 0.0061 0.0033 'international tables vol c tables 4.2.6.8 and 6.1.1.4' 'o' 'o' 0.0106 0.0060 'international tables vol c tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ORTHORHOMBIC _symmetry_space_group_name_h-m Pcca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' 'x+1/2, -y, -z+1/2' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' '-x-1/2, y, z-1/2' 'x, -y, z-1/2' _cell_length_a 18.499(3) _cell_length_b 32.113(5) _cell_length_c 14.620(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8685(3) _cell_formula_units_z 16 _cell_measurement_temperature 293(1) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 4.36 _cell_measurement_theta_max 11.90 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.755 _exptl_crystal_density_method 'not measured' _exptl_crystal_f_000 4672 _exptl_absorpt_coefficient_mu 1.227 _exptl_absorpt_correction_type Empirical _exptl_absorpt_process_details 'Walker, N. & Stuart, D (1983) Acta' _exptl_absorpt_correction_t_min 0.3502 _exptl_absorpt_correction_t_max 0.7275 _exptl_absorpt_process_details ? _exptl_special_details ; tetra(ammino)(2,2'-bipyridine)cobalt(III) perchlorate hydrate ; _diffrn_ambient_temperature 293(1) _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 'Enraf Nonius CAD4-MachS Diffractometer' _diffrn_measurement_method w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 160 _diffrn_standards_decay_% 35 _diffrn_reflns_number 7680 _diffrn_reflns_av_r_equivalents 0.0000 _diffrn_reflns_av_sigmai/neti 0.0918 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 25.05 _reflns_number_total 7680 _reflns_number_gt 4202 _reflns_threshold_expression >2sigma(i) _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD-4 Software' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'shelxl-97 (sheldrick, 1997)' _computing_molecular_graphics 'ORTEPIII For WINDOWS (L. J. Farrugia, J. Appl' _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^)+(0.1768p)^2^+60.0270p] 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 7680 _refine_ls_number_parameters 619 _refine_ls_number_restraints 102 _refine_ls_r_factor_all 0.1637 _refine_ls_r_factor_gt 0.0990 _refine_ls_wr_factor_ref 0.3455 _refine_ls_wr_factor_gt 0.3061 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_s_all 1.090 _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 0.10140(8) 0.15308(5) 0.98174(10) 0.0324(4) uani 1 1 d . . . n1 n 0.1960(5) 0.1563(3) 0.9253(6) 0.035(2) uani 1 1 d . . . c2 c 0.2183(6) 0.1209(4) 0.8827(8) 0.038(3) uani 1 1 d . . . c3 c 0.2831(7) 0.1185(5) 0.8370(9) 0.051(3) uani 1 1 d . . . h3 h 0.2958 0.0943 0.8059 0.056 uiso 1 1 calc r . . c4 c 0.3277(7) 0.1514(6) 0.8378(9) 0.061(4) uani 1 1 d . . . h4 h 0.3734 0.1494 0.8115 0.067 uiso 1 1 calc r . . c5 c 0.3053(7) 0.1889(5) 0.8787(10) 0.059(4) uani 1 1 d . . . h5 h 0.3345 0.2124 0.8758 0.065 uiso 1 1 calc r . . c6 c 0.2405(7) 0.1905(4) 0.9225(9) 0.049(3) uani 1 1 d . . . h6 h 0.2262 0.2151 0.9509 0.054 uiso 1 1 calc r . . n1' n 0.1091(5) 0.0950(3) 0.9472(6) 0.037(2) uani 1 1 d . . . c2' c 0.1691(7) 0.0871(5) 0.8945(9) 0.049(3) uani 1 1 d . . . c3' c 0.1798(8) 0.0470(5) 0.8565(11) 0.060(4) uani 1 1 d . . . h3' h 0.2206 0.0412 0.8217 0.066 uiso 1 1 calc r . . c4' c 0.1295(9) 0.0174(5) 0.8718(12) 0.072(5) uani 1 1 d . . . h4' h 0.1361 -0.0089 0.8465 0.079 uiso 1 1 calc r . . c5' c 0.0701(9) 0.0247(5) 0.9226(11) 0.067(4) uani 1 1 d . . . h5' h 0.0352 0.0042 0.9317 0.074 uiso 1 1 calc r . . c6' c 0.0630(8) 0.0643(4) 0.9611(10) 0.057(4) uani 1 1 d . . . h6' h 0.0234 0.0693 0.9988 0.062 uiso 1 1 calc r . . n2 n 0.0049(6) 0.1462(3) 1.0373(7) 0.046(3) uani 1 1 d . . . h2a h -0.0106 0.1203 1.0281 0.051 uiso 1 1 calc r . . h2b h -0.0259 0.1641 1.0117 0.051 uiso 1 1 calc r . . h2c h 0.0075 0.1512 1.0971 0.051 uiso 1 1 calc r . . n3 n 0.0980(5) 0.2120(3) 1.0116(7) 0.040(2) uani 1 1 d . . . h3a h 0.0580 0.2173 1.0435 0.045 uiso 1 1 calc r . . h3b h 0.0978 0.2268 0.9603 0.045 uiso 1 1 calc r . . h3c h 0.1366 0.2187 1.0448 0.045 uiso 1 1 calc r . . n4 n 0.1482(6) 0.1394(3) 1.0996(7) 0.047(3) uani 1 1 d . . . h4a h 0.1215 0.1207 1.1294 0.052 uiso 1 1 calc r . . h4b h 0.1522 0.1623 1.1332 0.052 uiso 1 1 calc r . . h4c h 0.1919 0.1288 1.0891 0.052 uiso 1 1 calc r . . n5 n 0.0557(6) 0.1655(3) 0.8647(6) 0.043(3) uani 1 1 d . . . h5a h 0.0768 0.1506 0.8209 0.048 uiso 1 1 calc r . . h5b h 0.0606 0.1925 0.8524 0.048 uiso 1 1 calc r . . h5c h 0.0090 0.1590 0.8675 0.048 uiso 1 1 calc r . . co2 co 0.11315(7) 0.35414(5) 0.50049(10) 0.0295(4) uani 1 1 d . . . n1" n 0.0436(5) 0.3972(3) 0.4692(6) 0.035(2) uani 1 1 d . . . c2" c 0.0686(7) 0.4257(4) 0.4088(8) 0.042(3) uani 1 1 d . . . c3" c 0.0273(9) 0.4593(4) 0.3796(11) 0.063(4) uani 1 1 d . . . h3" h 0.0468 0.4794 0.3410 0.069 uiso 1 1 calc r . . c4" c -0.0424(8) 0.4620(4) 0.4091(13) 0.070(5) uani 1 1 d . . . h4" h -0.0723 0.4833 0.3885 0.077 uiso 1 1 calc r . . c5" c -0.0690(8) 0.4313(6) 0.4728(13) 0.074(5) uani 1 1 d . . . h5" h -0.1163 0.4323 0.4943 0.082 uiso 1 1 calc r . . c6" c -0.0235(7) 0.4015(5) 0.5001(11) 0.059(4) uani 1 1 d . . . h6" h -0.0399 0.3825 0.5435 0.065 uiso 1 1 calc r . . n1"' n 0.1753(5) 0.3858(3) 0.4177(6) 0.037(2) uani 1 1 d . . . c2"' c 0.1433(6) 0.4185(4) 0.3785(8) 0.037(3) uani 1 1 d . . . c3"' c 0.1794(8) 0.4438(5) 0.3174(10) 0.060(4) uani 1 1 d . . . h3'" h 0.1557 0.4661 0.2900 0.066 uiso 1 1 calc r . . c4"' c 0.2504(9) 0.4357(5) 0.2975(9) 0.059(4) uani 1 1 d . . . h4"' h 0.2750 0.4515 0.2542 0.065 uiso 1 1 calc r . . c5"' c 0.2827(8) 0.4055(5) 0.3407(10) 0.061(4) uani 1 1 d . . . h5"' h 0.3317 0.4010 0.3309 0.068 uiso 1 1 calc r . . c6"' c 0.2452(7) 0.3795(4) 0.4018(8) 0.043(3) uani 1 1 d . . . h6"' h 0.2693 0.3579 0.4312 0.047 uiso 1 1 calc r . . n2" n 0.1841(5) 0.3101(3) 0.5236(7) 0.036(2) uani 1 1 d . . . h2a" h 0.2185 0.3198 0.5605 0.040 uiso 1 1 calc r . . h2b" h 0.2037 0.3021 0.4709 0.040 uiso 1 1 calc r . . h2c" h 0.1623 0.2885 0.5499 0.040 uiso 1 1 calc r . . n3" n 0.0455(5) 0.3255(3) 0.5847(7) 0.044(3) uani 1 1 d . . . h3a" h 0.0210 0.3443 0.6167 0.048 uiso 1 1 calc r . . h3b" h 0.0704 0.3093 0.6227 0.048 uiso 1 1 calc r . . h3c" h 0.0149 0.3100 0.5525 0.048 uiso 1 1 calc r . . n4" n 0.0758(5) 0.3199(3) 0.3993(7) 0.043(2) uani 1 1 d . . . h4a" h 0.1113 0.3043 0.3767 0.047 uiso 1 1 calc r . . h4b" h 0.0586 0.3365 0.3555 0.047 uiso 1 1 calc r . . h4c" h 0.0406 0.3035 0.4198 0.047 uiso 1 1 calc r . . n5" n 0.1519(5) 0.3867(3) 0.6033(6) 0.039(2) uani 1 1 d . . . h5a" h 0.1213 0.4072 0.6170 0.042 uiso 1 1 calc r . . h5b" h 0.1945 0.3975 0.5878 0.042 uiso 1 1 calc r . . h5c" h 0.1574 0.3703 0.6518 0.042 uiso 1 1 calc r . . cl1 cl 0.0000 0.06811(17) 0.2500 0.0666(15) uani 1 2 d s . . o11 o 0.0000 0.0268(10) 0.2500 0.152(6) uiso 1 2 d s . . o12 o 0.049(2) 0.0779(13) 0.331(3) 0.152(6) uiso 0.50 1 d p . . o13 o -0.075(2) 0.0835(13) 0.281(3) 0.152(6) uiso 0.50 1 d p . . o14 o 0.006(3) 0.0817(14) 0.167(3) 0.152(6) uiso 0.50 1 d p . . cl2 cl 0.0000 0.43291(14) 0.7500 0.0439(10) uani 1 2 d s . . o21 o 0.0000 0.3871(7) 0.7500 0.119(7) uani 1 2 d su . . o22 o 0.0136(17) 0.4439(9) 0.655(2) 0.102(9) uani 0.50 1 d pu . . o23 o 0.0635(16) 0.4510(10) 0.795(2) 0.103(9) uani 0.50 1 d pu . . o24 o -0.0600(13) 0.4507(8) 0.781(2) 0.079(7) uani 0.50 1 d pu . . cl3 cl 0.0000 0.22087(16) 0.2500 0.0457(11) uani 1 2 d s . . o31 o 0.0329(13) 0.2293(8) 0.3407(16) 0.070(6) uani 0.50 1 d pu . . o32 o 0.0670(16) 0.2100(9) 0.210(2) 0.090(8) uani 0.50 1 d pu . . o33 o -0.025(2) 0.2517(13) 0.207(3) 0.143(13) uani 0.50 1 d pu . . o34 o -0.0337(17) 0.1881(11) 0.293(2) 0.104(9) uani 0.50 1 d pu . . cl4 cl 0.35735(19) 0.29143(11) 0.3178(2) 0.0522(8) uani 1 1 d . . . o41a o 0.3864(14) 0.3220(8) 0.3768(17) 0.065(7) uani 0.50 1 d pu a 1 o42a o 0.3919(19) 0.2515(11) 0.321(3) 0.088(11) uani 0.50 1 d pu a 1 o43a o 0.281(2) 0.2825(14) 0.355(3) 0.078(12) uani 0.50 1 d pu a 1 o44a o 0.3445(12) 0.3074(7) 0.2277(15) 0.049(5) uani 0.50 1 d pu a 1 o41b o 0.3925(15) 0.3304(8) 0.335(2) 0.073(8) uani 0.50 1 d pu a 2 o42b o 0.4135(14) 0.2614(8) 0.335(2) 0.059(7) uani 0.50 1 d pu a 2 o43b o 0.2986(18) 0.2852(12) 0.373(2) 0.061(9) uani 0.50 1 d pu a 2 o44b o 0.3356(15) 0.2878(8) 0.2206(18) 0.069(7) uani 0.50 1 d pu a 2 cl5 cl 0.13264(18) 0.33405(13) 0.1512(2) 0.0584(10) uani 1 1 d . b 2 o51 o 0.0800(6) 0.3596(4) 0.1956(8) 0.082(4) uani 1 1 d . b 2 o52 o 0.0959(8) 0.3106(4) 0.0838(9) 0.100(4) uani 1 1 d . b 2 o53 o 0.1626(7) 0.3070(4) 0.2198(8) 0.087(4) uani 1 1 d . b 2 o54 o 0.1879(6) 0.3587(4) 0.1088(10) 0.096(4) uani 1 1 d . b 2 cl6 cl 0.07435(19) 0.22967(11) 0.5456(3) 0.0574(9) uani 1 1 d . c 2 cl7 cl 0.7500 0.5000 0.4436(4) 0.0566(13) uani 1 2 d s . 2 o71 o 0.8058(16) 0.4966(10) 0.367(2) 0.105(4) uiso 0.50 1 d p . 2 o72 o 0.7385(16) 0.5461(9) 0.455(2) 0.105(4) uiso 0.50 1 d p . 2 o73 o 0.7967(16) 0.4867(9) 0.516(2) 0.105(4) uiso 0.50 1 d p . 2 o74 o 0.6871(17) 0.4764(10) 0.415(2) 0.105(4) uiso 0.50 1 d p . 2 cl8 cl 0.3467(3) 0.07678(18) 0.0806(3) 0.0837(14) uani 1 1 d . d 2 o81 o 0.3792(11) 0.0498(6) 0.1391(14) 0.145(6) uani 1 1 d u d 2 o82a o 0.375(2) 0.1132(14) 0.047(3) 0.145(8) uiso 0.50 1 d p e 1 o83a o 0.303(2) 0.1142(13) 0.077(3) 0.145(8) uiso 0.50 1 d p e 1 o84a o 0.295(2) 0.0467(13) 0.032(3) 0.145(8) uiso 0.50 1 d p f 1 o82b o 0.400(2) 0.1070(13) 0.113(3) 0.141(8) uiso 0.50 1 d p d 2 o83b o 0.294(2) 0.0953(13) 0.131(3) 0.141(8) uiso 0.50 1 d p d 2 o84b o 0.383(2) 0.0760(13) -0.002(3) 0.141(8) uiso 0.50 1 d p d 2 o1 o 0.2176(6) 0.2258(4) 0.1446(8) 0.085(4) uani 1 1 d . g 2 o2 o 0.0000 0.0944(5) 0.7500 0.080(5) uani 1 2 d s h 2 o3 o 0.1530(7) 0.1828(4) 0.7046(8) 0.088(4) uani 1 1 d . i 2 o4 o 0.1761(16) 0.0429(9) 0.169(2) 0.106(9) uiso 0.50 1 d p j 2 loop_ _atom_site_aniso_label _atom_site_aniso_u_11 _atom_site_aniso_u_22 _atom_site_aniso_u_33 _atom_site_aniso_u_23 _atom_site_aniso_u_13 _atom_site_aniso_u_12 co1 0.0322(8) 0.0407(8) 0.0244(7) 0.0009(6) 0.0031(6) 0.0023(7) n1 0.038(5) 0.038(5) 0.029(5) -0.002(4) -0.001(4) 0.003(4) c2 0.037(6) 0.041(6) 0.036(6) -0.006(5) 0.004(5) 0.004(5) c3 0.034(7) 0.071(9) 0.046(8) -0.007(7) 0.003(6) 0.004(7) c4 0.030(7) 0.114(13) 0.039(7) -0.003(8) 0.007(6) -0.009(8) c5 0.043(8) 0.084(11) 0.050(8) -0.015(8) 0.004(7) -0.022(8) c6 0.052(8) 0.046(7) 0.048(8) -0.005(6) -0.003(7) -0.018(6) n1' 0.040(5) 0.040(5) 0.030(5) 0.004(4) 0.005(4) 0.005(5) c2' 0.038(7) 0.062(8) 0.046(7) -0.006(7) 0.006(6) 0.011(6) c3' 0.055(9) 0.053(8) 0.072(10) -0.010(8) 0.017(8) 0.008(7) c4' 0.079(11) 0.044(8) 0.094(13) -0.026(8) 0.011(10) -0.006(8) c5' 0.079(11) 0.044(8) 0.079(11) 0.004(8) 0.032(9) -0.014(8) c6' 0.073(10) 0.044(7) 0.053(8) 0.001(6) 0.034(8) -0.004(7) n2 0.045(6) 0.044(6) 0.049(6) 0.005(5) 0.009(5) 0.002(5) n3 0.041(5) 0.050(6) 0.031(5) 0.002(5) 0.002(5) -0.003(5) n4 0.055(7) 0.053(6) 0.033(5) 0.008(5) 0.006(5) 0.011(5) n5 0.043(6) 0.063(7) 0.023(5) 0.000(5) 0.002(4) 0.001(5) co2 0.0235(7) 0.0402(8) 0.0247(7) 0.0002(6) 0.0015(6) 0.0007(6) n1" 0.033(5) 0.041(5) 0.032(5) -0.001(4) -0.001(4) 0.004(4) c2" 0.052(7) 0.039(7) 0.036(7) 0.003(5) -0.008(6) 0.004(6) c3" 0.067(10) 0.043(8) 0.078(11) 0.024(7) 0.005(9) 0.013(7) c4" 0.055(9) 0.044(8) 0.111(14) 0.015(9) -0.018(10) 0.019(7) c5" 0.038(8) 0.093(13) 0.092(13) 0.002(11) 0.008(8) 0.017(8) c6" 0.029(6) 0.087(10) 0.061(9) -0.001(8) 0.002(7) 0.021(7) n1"' 0.034(5) 0.052(6) 0.026(5) 0.000(4) 0.010(4) -0.005(5) c2"' 0.040(7) 0.042(6) 0.030(6) 0.012(5) 0.000(5) -0.001(6) c3"' 0.062(9) 0.060(9) 0.058(9) 0.017(7) -0.003(8) -0.009(8) c4"' 0.061(9) 0.077(10) 0.040(7) 0.017(7) 0.005(7) -0.008(8) c5"' 0.054(8) 0.082(11) 0.049(8) -0.010(8) 0.007(7) -0.031(8) c6"' 0.032(6) 0.060(8) 0.036(6) 0.004(6) 0.015(6) 0.003(6) n2" 0.032(5) 0.027(5) 0.049(6) 0.007(4) 0.012(5) 0.003(4) n3" 0.031(5) 0.056(6) 0.044(6) 0.002(5) 0.009(5) -0.003(5) n4" 0.036(5) 0.057(6) 0.036(6) -0.005(5) -0.005(5) -0.006(5) n5" 0.037(5) 0.053(6) 0.025(5) -0.008(4) -0.001(4) -0.006(5) cl1 0.095(4) 0.056(3) 0.048(3) 0.000 -0.012(3) 0.000 cl2 0.051(3) 0.046(2) 0.034(2) 0.000 0.004(2) 0.000 o21 0.129(11) 0.106(10) 0.122(10) 0.000 0.004(9) 0.000 o22 0.117(12) 0.104(11) 0.085(11) 0.009(9) 0.012(9) -0.001(9) o23 0.096(12) 0.102(12) 0.110(12) -0.003(9) -0.016(9) -0.008(9) o24 0.071(10) 0.074(10) 0.092(10) -0.011(8) 0.012(9) 0.003(8) cl3 0.040(2) 0.063(3) 0.035(2) 0.000 -0.0037(19) 0.000 o31 0.079(10) 0.076(9) 0.056(9) -0.013(8) -0.014(8) 0.008(8) o32 0.093(11) 0.080(11) 0.098(11) 0.004(9) 0.013(9) 0.015(9) o33 0.156(16) 0.132(15) 0.139(16) 0.018(10) -0.005(10) 0.010(10) o34 0.103(12) 0.109(12) 0.101(12) 0.025(9) -0.002(9) -0.009(9) cl4 0.057(2) 0.060(2) 0.0398(17) 0.0083(15) -0.0052(16) 0.0042(17) o41a 0.064(10) 0.072(10) 0.059(10) -0.011(8) -0.012(8) -0.002(8) o42a 0.090(14) 0.080(14) 0.093(14) -0.001(9) -0.001(9) 0.009(9) o43a 0.075(15) 0.082(14) 0.076(15) -0.001(9) 0.005(9) 0.001(9) o44a 0.058(9) 0.052(9) 0.038(8) 0.005(7) -0.007(7) -0.004(8) o41b 0.070(10) 0.069(10) 0.079(11) 0.007(9) 0.000(9) -0.013(8) o42b 0.053(10) 0.056(10) 0.069(10) 0.005(8) -0.015(8) 0.003(8) o43b 0.057(12) 0.071(12) 0.054(11) -0.001(8) 0.011(9) -0.011(9) o44b 0.075(11) 0.069(10) 0.062(10) 0.005(9) -0.003(8) 0.011(9) cl5 0.0398(17) 0.084(3) 0.0511(19) 0.0002(19) 0.0044(16) 0.0034(18) o51 0.068(7) 0.093(8) 0.084(8) 0.005(7) 0.032(7) 0.018(6) o52 0.120(11) 0.096(9) 0.083(9) -0.014(8) -0.020(8) -0.009(9) o53 0.088(8) 0.099(9) 0.076(8) -0.001(7) -0.011(7) 0.022(7) o54 0.070(7) 0.087(9) 0.130(11) -0.011(8) 0.048(8) -0.029(7) cl6 0.0506(19) 0.054(2) 0.068(2) -0.0060(17) 0.0002(18) -0.0103(16) cl7 0.052(3) 0.066(3) 0.052(3) 0.000 0.000 0.020(3) cl8 0.070(3) 0.104(4) 0.077(3) 0.019(3) 0.004(2) 0.012(3) o81 0.150(10) 0.141(10) 0.144(10) 0.033(8) -0.012(8) 0.007(8) o1 0.078(8) 0.101(9) 0.074(8) -0.031(7) -0.030(7) 0.012(7) o2 0.090(12) 0.080(11) 0.069(10) 0.000 -0.032(9) 0.000 o3 0.096(9) 0.105(9) 0.062(7) 0.003(7) -0.004(7) -0.011(8) _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 n1 1.938(10) . Y co1 n1' 1.938(10) . Y co1 n3 1.942(10) . Y co1 n5 1.949(9) . Y co1 n2 1.974(10) . Y co1 n4 1.977(10) . Y n1 c2 1.361(14) . ? n1 c6 1.374(15) . ? c2 c3 1.373(17) . ? c2 c2' 1.426(18) . ? c3 c4 1.34(2) . ? c4 c5 1.41(2) . ? c5 c6 1.359(19) . ? n1' c6' 1.319(16) . ? n1' c2' 1.375(15) . ? c2' c3' 1.418(19) . ? c3' c4' 1.35(2) . ? c4' c5' 1.35(2) . ? c5' c6' 1.40(2) . ? co2 n1" 1.943(9) . Y co2 n1"' 1.953(9) . Y co2 n2" 1.957(9) . Y co2 n5" 1.967(9) . Y co2 n4" 1.968(10) . Y co2 n3" 1.982(10) . Y n1" c6" 1.328(16) . ? n1" c2" 1.353(15) . ? c2" c3" 1.390(18) . ? c2" c2"' 1.470(17) . ? c3" c4" 1.36(2) . ? c4" c5" 1.44(2) . ? c5" c6" 1.34(2) . ? n1"' c6"' 1.330(15) . ? n1"' c2"' 1.336(15) . ? c2"' c3"' 1.378(18) . ? c3"' c4"' 1.37(2) . ? c4"' c5"' 1.30(2) . ? c5"' c6"' 1.406(18) . ? cl1 o14 1.29(4) 4 ? cl1 o14 1.29(4) . ? cl1 o11 1.33(3) . ? cl1 o12 1.52(4) 4 ? cl1 o12 1.52(4) . ? cl1 o13 1.54(4) 4 ? cl1 o13 1.54(4) . ? o12 o14 1.04(5) 4 ? o12 o13 1.70(6) 4 ? o13 o14 1.48(5) 4 ? o13 o12 1.70(6) 4 ? o14 o12 1.04(5) 4 ? o14 o13 1.48(5) 4 ? cl2 o24 1.33(2) 4_556 ? cl2 o24 1.33(2) . ? cl2 o22 1.46(3) . ? cl2 o22 1.46(3) 4_556 ? cl2 o23 1.47(3) . ? cl2 o23 1.47(3) 4_556 ? cl2 o21 1.47(2) . ? o22 o24 1.29(4) 4_556 ? o22 o23 1.62(4) 4_556 ? o23 o24 1.12(3) 4_556 ? o23 o22 1.62(4) 4_556 ? o24 o23 1.12(3) 4_556 ? o24 o22 1.29(4) 4_556 ? cl3 o33 1.26(4) 4 ? cl3 o33 1.26(4) . ? cl3 o34 1.37(3) . ? cl3 o34 1.37(3) 4 ? cl3 o32 1.41(3) . ? cl3 o32 1.41(3) 4 ? cl3 o31 1.48(2) 4 ? cl3 o31 1.48(2) . ? o31 o33 1.01(4) 4 ? o32 o34 0.94(3) 4 ? o33 o31 1.01(4) 4 ? o33 o33 1.55(8) 4 ? o34 o32 0.94(3) 4 ? o34 o34 1.77(6) 4 ? cl4 o43b 1.37(3) . ? cl4 o41a 1.41(2) . ? cl4 o41b 1.43(3) . ? cl4 o44a 1.43(2) . ? cl4 o42a 1.43(3) . ? cl4 o42b 1.44(3) . ? cl4 o44b 1.48(3) . ? cl4 o43a 1.53(4) . ? cl5 o52 1.413(13) . ? cl5 o51 1.429(11) . ? cl5 o54 1.434(11) . ? cl5 o53 1.438(12) . ? cl7 o73 1.43(3) . ? cl7 o73 1.43(3) 2_665 ? cl7 o74 1.45(3) 2_665 ? cl7 o74 1.45(3) . ? cl7 o72 1.51(3) . ? cl7 o72 1.51(3) 2_665 ? cl7 o71 1.53(3) . ? cl7 o71 1.53(3) 2_665 ? o71 o74 1.12(4) 2_665 ? o72 o73 1.52(4) 2_665 ? o72 o74 1.66(4) 2_665 ? o73 o72 1.52(4) 2_665 ? o74 o71 1.12(4) 2_665 ? o74 o72 1.66(4) 2_665 ? cl8 o83b 1.35(4) . ? cl8 o81 1.358(18) . ? cl8 o84b 1.39(4) . ? cl8 o82b 1.46(4) . ? o82a o83a 1.41(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag n1 co1 n1' 82.8(4) . . Y n1 co1 n3 94.2(4) . . Y n1' co1 n3 176.8(4) . . Y n1 co1 n5 90.4(4) . . Y n1' co1 n5 90.0(4) . . Y n3 co1 n5 89.1(4) . . Y n1 co1 n2 176.5(4) . . Y n1' co1 n2 93.8(4) . . Y n3 co1 n2 89.2(4) . . Y n5 co1 n2 89.5(5) . . Y n1 co1 n4 89.3(4) . . Y n1' co1 n4 88.9(4) . . Y n3 co1 n4 92.0(4) . . Y n5 co1 n4 178.9(5) . . Y n2 co1 n4 90.7(4) . . Y c2 n1 c6 118.3(10) . . ? c2 n1 co1 115.1(8) . . ? c6 n1 co1 126.6(8) . . ? n1 c2 c3 122.2(12) . . ? n1 c2 c2' 112.7(10) . . ? c3 c2 c2' 125.0(12) . . ? c4 c3 c2 119.3(14) . . ? c3 c4 c5 119.7(13) . . ? c6 c5 c4 119.6(14) . . ? c5 c6 n1 120.7(13) . . ? c6' n1' c2' 118.2(11) . . ? c6' n1' co1 129.2(9) . . ? c2' n1' co1 112.4(9) . . ? n1' c2' c3' 119.9(13) . . ? n1' c2' c2 116.4(11) . . ? c3' c2' c2 123.7(12) . . ? c4' c3' c2' 118.7(14) . . ? c3' c4' c5' 122.1(14) . . ? c4' c5' c6' 117.3(14) . . ? n1' c6' c5' 123.8(13) . . ? n1" co2 n1"' 82.7(4) . . Y n1" co2 n2" 176.3(4) . . Y n1"' co2 n2" 95.1(4) . . Y n1" co2 n5" 92.4(4) . . Y n1"' co2 n5" 89.0(4) . . Y n2" co2 n5" 90.5(4) . . Y n1" co2 n4" 89.3(4) . . Y n1"' co2 n4" 91.8(4) . . Y n2" co2 n4" 87.8(4) . . Y n5" co2 n4" 178.2(5) . . Y n1" co2 n3" 93.4(4) . . Y n1"' co2 n3" 176.0(4) . . Y n2" co2 n3" 88.9(4) . . Y n5" co2 n3" 90.1(4) . . Y n4" co2 n3" 89.2(4) . . Y c6" n1" c2" 118.1(12) . . ? c6" n1" co2 127.8(10) . . ? c2" n1" co2 114.1(8) . . ? n1" c2" c3" 122.6(13) . . ? n1" c2" c2"' 114.4(10) . . ? c3" c2" c2"' 123.0(12) . . ? c4" c3" c2" 118.2(14) . . ? c3" c4" c5" 118.9(13) . . ? c6" c5" c4" 117.9(14) . . ? n1" c6" c5" 124.2(16) . . ? c6"' n1"' c2"' 118.3(10) . . ? c6"' n1"' co2 127.0(9) . . ? c2"' n1"' co2 114.5(8) . . ? n1"' c2"' c3"' 121.8(12) . . ? n1"' c2"' c2" 114.2(10) . . ? c3"' c2"' c2" 124.0(12) . . ? c4"' c3"' c2"' 119.4(14) . . ? c5"' c4"' c3"' 118.4(14) . . ? c4"' c5"' c6"' 121.7(15) . . ? n1"' c6"' c5"' 120.1(13) . . ? o14 cl1 o14 141(4) 4 . ? o14 cl1 o11 110(2) 4 . ? o14 cl1 o11 110(2) . . ? o14 cl1 o12 127(2) 4 4 ? o14 cl1 o12 42(2) . 4 ? o11 cl1 o12 101.9(16) . 4 ? o14 cl1 o12 42(2) 4 . ? o14 cl1 o12 127(2) . . ? o11 cl1 o12 101.9(16) . . ? o12 cl1 o12 156(3) 4 . ? o14 cl1 o13 104(2) 4 4 ? o14 cl1 o13 62(2) . 4 ? o11 cl1 o13 108.8(16) . 4 ? o12 cl1 o13 104(2) 4 4 ? o12 cl1 o13 68(2) . 4 ? o14 cl1 o13 62(2) 4 . ? o14 cl1 o13 104(2) . . ? o11 cl1 o13 108.8(16) . . ? o12 cl1 o13 68(2) 4 . ? o12 cl1 o13 104(2) . . ? o13 cl1 o13 142(3) 4 . ? o14 o12 cl1 57(4) 4 . ? o14 o12 o13 107(5) 4 4 ? cl1 o12 o13 57(2) . 4 ? o14 o13 cl1 51(2) 4 . ? o14 o13 o12 104(3) 4 4 ? cl1 o13 o12 56(2) . 4 ? o12 o14 cl1 81(4) 4 . ? o12 o14 o13 147(6) 4 4 ? cl1 o14 o13 67(3) . 4 ? o24 cl2 o24 129(2) 4_556 . ? o24 cl2 o22 54.8(15) 4_556 . ? o24 cl2 o22 111.7(16) . . ? o24 cl2 o22 111.7(16) 4_556 4_556 ? o24 cl2 o22 54.8(15) . 4_556 ? o22 cl2 o22 152(2) . 4_556 ? o24 cl2 o23 46.8(14) 4_556 . ? o24 cl2 o23 110.2(14) . . ? o22 cl2 o23 101.3(17) . . ? o22 cl2 o23 67.3(17) 4_556 . ? o24 cl2 o23 110.2(14) 4_556 4_556 ? o24 cl2 o23 46.8(14) . 4_556 ? o22 cl2 o23 67.3(16) . 4_556 ? o22 cl2 o23 101.3(17) 4_556 4_556 ? o23 cl2 o23 133(2) . 4_556 ? o24 cl2 o21 115.4(11) 4_556 . ? o24 cl2 o21 115.4(11) . . ? o22 cl2 o21 104.0(12) . . ? o22 cl2 o21 104.0(12) 4_556 . ? o23 cl2 o21 113.3(12) . . ? o23 cl2 o21 113.3(12) 4_556 . ? o24 o22 cl2 57.4(16) 4_556 . ? o24 o22 o23 103(2) 4_556 4_556 ? cl2 o22 o23 56.6(15) . 4_556 ? o24 o23 cl2 60(2) 4_556 . ? o24 o23 o22 114(3) 4_556 4_556 ? cl2 o23 o22 56.1(15) . 4_556 ? o23 o24 o22 140(3) 4_556 4_556 ? o23 o24 cl2 73(2) 4_556 . ? o22 o24 cl2 67.8(18) 4_556 . ? o33 cl3 o33 76(4) 4 . ? o33 cl3 o34 123(2) 4 . ? o33 cl3 o34 132(2) . . ? o33 cl3 o34 132(2) 4 4 ? o33 cl3 o34 123(2) . 4 ? o34 cl3 o34 80(3) . 4 ? o33 cl3 o32 95(2) 4 . ? o33 cl3 o32 108(2) . . ? o34 cl3 o32 113(2) . . ? o34 cl3 o32 39.3(14) 4 . ? o33 cl3 o32 108(2) 4 4 ? o33 cl3 o32 95(2) . 4 ? o34 cl3 o32 39.3(14) . 4 ? o34 cl3 o32 113(2) 4 4 ? o32 cl3 o32 151(2) . 4 ? o33 cl3 o31 117(2) 4 4 ? o33 cl3 o31 42.4(18) . 4 ? o34 cl3 o31 111.1(16) . 4 ? o34 cl3 o31 85.3(17) 4 4 ? o32 cl3 o31 92.1(15) . 4 ? o32 cl3 o31 93.0(16) 4 4 ? o33 cl3 o31 42.4(18) 4 . ? o33 cl3 o31 117(2) . . ? o34 cl3 o31 85.3(17) . . ? o34 cl3 o31 111.1(16) 4 . ? o32 cl3 o31 93.0(16) . . ? o32 cl3 o31 92.1(15) 4 . ? o31 cl3 o31 159(2) 4 . ? o33 o31 cl3 57(2) 4 . ? o34 o32 cl3 68(3) 4 . ? o31 o33 cl3 81(3) 4 . ? o31 o33 o33 130(3) 4 4 ? cl3 o33 o33 51.8(19) . 4 ? o32 o34 cl3 73(3) 4 . ? o32 o34 o34 115(3) 4 4 ? cl3 o34 o34 50.0(15) . 4 ? o43b cl4 o41a 92.5(19) . . ? o43b cl4 o41b 113(2) . . ? o41a cl4 o41b 27.6(12) . . ? o43b cl4 o44a 117.7(18) . . ? o41a cl4 o44a 112.0(15) . . ? o41b cl4 o44a 85.6(15) . . ? o43b cl4 o42a 102(2) . . ? o41a cl4 o42a 115.6(18) . . ? o41b cl4 o42a 125.0(18) . . ? o44a cl4 o42a 115.2(18) . . ? o43b cl4 o42b 112(2) . . ? o41a cl4 o42b 95.1(16) . . ? o41b cl4 o42b 103.3(16) . . ? o44a cl4 o42b 121.1(15) . . ? o42a cl4 o42b 21.9(17) . . ? o43b cl4 o44b 109.9(19) . . ? o41a cl4 o44b 138.0(16) . . ? o41b cl4 o44b 111.1(16) . . ? o44a cl4 o44b 26.1(11) . . ? o42a cl4 o44b 94.8(18) . . ? o42b cl4 o44b 107.8(16) . . ? o43b cl4 o43a 15(2) . . ? o41a cl4 o43a 105.2(19) . . ? o41b cl4 o43a 121(2) . . ? o44a cl4 o43a 103.9(18) . . ? o42a cl4 o43a 103(2) . . ? o42b cl4 o43a 118(2) . . ? o44b cl4 o43a 94.4(19) . . ? o52 cl5 o51 107.1(8) . . ? o52 cl5 o54 109.5(9) . . ? o51 cl5 o54 111.4(8) . . ? o52 cl5 o53 110.5(8) . . ? o51 cl5 o53 107.1(8) . . ? o54 cl5 o53 111.1(9) . . ? o73 cl7 o73 85(2) . 2_665 ? o73 cl7 o74 83.3(17) . 2_665 ? o73 cl7 o74 122.9(17) 2_665 2_665 ? o73 cl7 o74 122.9(17) . . ? o73 cl7 o74 83.3(17) 2_665 . ? o74 cl7 o74 146(3) 2_665 . ? o73 cl7 o72 107.1(17) . . ? o73 cl7 o72 62.4(15) 2_665 . ? o74 cl7 o72 68.4(17) 2_665 . ? o74 cl7 o72 115.7(17) . . ? o73 cl7 o72 62.4(15) . 2_665 ? o73 cl7 o72 107.1(17) 2_665 2_665 ? o74 cl7 o72 115.7(17) 2_665 2_665 ? o74 cl7 o72 68.4(17) . 2_665 ? o72 cl7 o72 167(2) . 2_665 ? o73 cl7 o71 96.4(16) . . ? o73 cl7 o71 166.4(18) 2_665 . ? o74 cl7 o71 44.2(14) 2_665 . ? o74 cl7 o71 107.0(18) . . ? o72 cl7 o71 104.4(17) . . ? o72 cl7 o71 85.3(17) 2_665 . ? o73 cl7 o71 166.4(17) . 2_665 ? o73 cl7 o71 96.4(16) 2_665 2_665 ? o74 cl7 o71 107.0(18) 2_665 2_665 ? o74 cl7 o71 44.2(14) . 2_665 ? o72 cl7 o71 85.3(17) . 2_665 ? o72 cl7 o71 104.4(17) 2_665 2_665 ? o71 cl7 o71 86(2) . 2_665 ? o74 o71 cl7 64(2) 2_665 . ? cl7 o72 o73 56.2(15) . 2_665 ? cl7 o72 o74 54.2(15) . 2_665 ? o73 o72 o74 105(2) 2_665 2_665 ? cl7 o73 o72 61.3(16) . 2_665 ? o71 o74 cl7 72(2) 2_665 . ? o71 o74 o72 117(3) 2_665 2_665 ? cl7 o74 o72 57.4(15) . 2_665 ? o83b cl8 o81 105(2) . . ? o83b cl8 o84b 146(3) . . ? o81 cl8 o84b 108.8(19) . . ? o83b cl8 o82b 91(2) . . ? o81 cl8 o82b 85.3(18) . . ? o84b cl8 o82b 88(2) . . ? 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 h2a o82a 0.89 2.39 2.90(5) 116.2 6_556 n2 h2a o84b 0.89 2.45 3.23(4) 145.4 6_556 n2 h2a o12 0.89 2.58 3.09(5) 117.5 4_556 n2 h2a o82b 0.89 2.68 3.19(4) 117.6 6_556 n2 h2a cl8 0.89 3.38 4.062(12) 135.0 6_556 n2 h2b cl6 0.89 2.44 3.286(11) 159.4 4_556 n2 h2c o34 0.89 2.06 2.87(3) 152.3 4_556 n2 h2c o32 0.89 2.74 3.45(3) 137.6 1_556 n2 h2c o31 0.89 2.77 3.28(3) 118.0 4_556 n2 h2c o13 0.89 3.08 3.58(4) 117.8 4_556 n2 h2c cl3 0.89 3.17 3.928(11) 144.9 1_556 n2 h2c o34 0.89 3.19 4.03(4) 159.1 1_556 n2 h2c cl1 0.89 3.48 3.996(11) 119.4 1_556 n3 h3a o31 0.89 2.42 3.29(3) 167.1 4_556 n3 h3a o32 0.89 2.46 2.96(3) 116.4 1_556 n3 h3a o34 0.89 2.61 3.19(3) 123.6 4_556 n3 h3a cl6 0.89 2.80 3.345(11) 120.7 4_556 n3 h3a o33 0.89 3.05 3.87(4) 153.9 1_556 n3 h3a cl3 0.89 3.21 3.939(10) 141.0 1_556 n3 h3b o42b 0.89 2.16 3.04(3) 174.5 7_656 n3 h3b o42a 0.89 2.19 3.07(4) 167.6 7_656 n3 h3b o43b 0.89 2.97 3.64(4) 134.3 7_656 n3 h3b cl4 0.89 3.05 3.902(10) 159.8 7_656 n3 h3b o43a 0.89 3.25 3.92(4) 133.8 7_656 n3 h3b o41a 0.89 3.30 4.06(3) 143.9 7_656 n3 h3c o1 0.89 2.10 2.979(15) 167.4 1_556 n4 h4a o13 0.89 1.97 2.85(4) 167.2 4_556 n4 h4a o14 0.89 2.53 3.36(5) 155.0 1_556 n4 h4a o4 0.89 2.76 3.30(3) 120.5 1_556 n4 h4a cl1 0.89 3.32 4.194(11) 168.1 1_556 n4 h4a o12 0.89 3.50 4.28(5) 148.0 4_556 n4 h4a o12 0.89 3.51 4.32(5) 152.2 1_556 n4 h4b o1 0.89 2.38 3.129(17) 142.5 1_556 n4 h4b o32 0.89 2.47 3.16(3) 135.4 1_556 n4 h4b o34 0.89 2.58 3.07(3) 115.2 4_556 n4 h4c o83a 0.89 2.11 2.99(5) 169.0 1_556 n4 h4c o83b 0.89 2.26 3.09(4) 153.6 1_556 n4 h4c cl8 0.89 3.32 4.196(11) 169.2 1_556 n4 h4c o84a 0.89 3.35 4.14(4) 148.8 1_556 n4 h4c o82a 0.89 3.48 4.35(4) 165.9 1_556 n5 h5a o3 0.89 2.44 3.005(16) 121.9 . n5 h5a o2 0.89 2.52 3.016(17) 115.7 . n5 h5a o82b 0.89 3.37 4.21(4) 158.2 7_656 n5 h5b o42a 0.89 2.14 3.00(4) 161.4 7_656 n5 h5b o42b 0.89 2.28 3.16(3) 171.9 7_656 n5 h5b cl4 0.89 3.56 4.406(12) 160.3 7_656 n5 h5c o82b 0.89 2.63 3.45(4) 153.7 6_556 n5 h5c o82a 0.89 3.14 3.95(5) 153.3 6_556 n5 h5c o3 0.89 3.27 4.032(16) 145.3 4_556 n2" h2a" o54 0.89 2.25 3.097(16) 159.1 7_656 n2" h2a" cl5 0.89 3.09 3.946(11) 161.7 7_656 n2" h2a" o53 0.89 3.23 4.036(17) 151.7 7_656 n2" h2a" o52 0.89 3.46 4.164(18) 137.7 7_656 n2" h2b" o43a 0.89 2.31 3.18(4) 165.5 . n2" h2b" o43b 0.89 2.33 3.16(3) 155.1 . n2" h2c" cl6 0.89 2.49 3.301(10) 151.1 . n2" h2c" o44b 0.89 2.50 2.99(3) 115.6 7_656 n2" h2c" o1 0.89 3.30 3.711(16) 110.6 7_656 n3" h3a" o21 0.89 2.42 3.235(17) 153.3 . n3" h3a" o41b 0.89 2.52 3.07(3) 120.6 6_556 n3" h3a" o22 0.89 3.25 3.98(3) 141.3 . n3" h3a" cl2 0.89 3.47 4.296(11) 155.5 . n3" h3b" o44a 0.89 2.20 2.97(3) 145.3 7_656 n3" h3b" o44b 0.89 2.35 3.20(3) 158.9 7_656 n3" h3b" cl4 0.89 3.20 4.004(11) 151.3 7_656 n3" h3b" o41b 0.89 3.25 3.84(3) 125.7 7_656 n3" h3b" o42b 0.89 3.47 4.26(3) 149.4 7_656 n3" h3b" o42a 0.89 3.51 4.35(4) 158.0 7_656 n3" h3c" o52 0.89 2.86 3.626(17) 145.3 4 n3" h3c" o42b 0.89 2.95 3.41(3) 113.9 6_556 n3" h3c" o42a 0.89 3.48 3.95(4) 115.9 6_556 n4" h4a" o53 0.89 2.48 3.104(17) 127.2 . n4" h4a" o43a 0.89 3.24 4.04(4) 151.1 . n4" h4a" o43b 0.89 3.52 4.29(4) 146.2 . n4" h4b" o51 0.89 2.49 3.240(16) 142.9 . n4" h4b" o51 0.89 2.77 3.443(17) 133.2 4 n4" h4b" cl5 0.89 3.29 3.802(11) 119.4 . n4" h4c" cl5 0.89 3.51 3.952(11) 113.8 4 n4" h4c" o52 0.89 2.54 3.201(18) 132.0 4 n4" h4c" o31 0.89 2.65 3.14(3) 115.1 . n4" h4c" cl6 0.89 3.07 3.602(12) 120.7 . n4" h4c" cl5 0.89 3.51 3.952(11) 113.8 4 n5" h5a" o22 0.89 2.38 3.24(3) 161.8 . n5" h5a" o21 0.89 3.04 3.534(10) 117.1 . n5" h5a" cl2 0.89 3.08 3.833(10) 143.3 . n5" h5a" o23 0.89 3.15 3.84(3) 137.0 . n5" h5a" o71 0.89 3.38 3.85(3) 116.0 5_666 n5" h5b" o72 0.89 2.28 3.08(3) 149.2 5_666 n5" h5b" o54 0.89 2.53 3.099(15) 122.7 7_656 n5" h5b" o74 0.89 2.54 2.96(3) 110.1 6_556 n5" h5b" cl7 0.89 3.48 4.123(10) 131.5 5_666 n5" h5c" o44a 0.89 2.30 3.13(2) 154.5 7_656 n5" h5c" o44b 0.89 2.84 3.62(3) 147.4 7_656 n5" h5c" o41b 0.89 3.11 3.93(3) 153.7 7_656 n5" h5c" cl4 0.89 3.52 4.385(11) 165.5 7_656 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.018 _refine_diff_density_min -0.932 _refine_diff_density_rms 0.174 #===END data_af6 _database_code_CSD 169189 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'bis-(ammonia)bis-(1,10-phenanthroline)cobalt(III) perchlorate monohydrate' ; _chemical_name_common '[Co(phen)2(NH3)2](ClO4)3.H2O' _chemical_melting_point ? _chemical_formula_moiety C24H24N6O13Cl3Co _chemical_formula_sum 'C24 H24 Cl3 Co N6 O13' _chemical_formula_weight 769.77 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21 /c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.199(5) _cell_length_b 14.569(2) _cell_length_c 14.467(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.477(19) _cell_angle_gamma 90.00 _cell_volume 2991.7(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(1) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8.63 _cell_measurement_theta_max 17.29 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.709 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 0.919 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_process_details 'Sheldrick, 1976' _exptl_absorpt_correction_T_min 0.7767 _exptl_absorpt_correction_T_max 0.8740 _exptl_special_details ; 'bis-(ammonia)bis-(1,10-phenanthroline)cobalt(III) perchlorate monohydrate' ; _diffrn_ambient_temperature 293(1) _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 'Enraf Nonius CAD4-MachS Diffractometer' _diffrn_measurement_method \w:2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% none _diffrn_reflns_number 8299 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.1069 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 27.59 _reflns_number_total 6883 _reflns_number_gt 3471 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD-4 Software' _computing_data_reduction 'PROCESS_DATA (Gable et al., 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material SHELXL _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^)+(0.0672P)^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 6883 _refine_ls_number_parameters 537 _refine_ls_number_restraints 180 _refine_ls_R_factor_all 0.1449 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.1521 _refine_ls_wR_factor_gt 0.1275 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.994 _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 Co Co 0.19168(5) 0.03140(4) 0.18231(4) 0.03233(18) Uani 1 1 d . . . N1 N 0.2676(3) 0.0860(3) 0.0866(2) 0.0350(9) Uani 1 1 d . . . C2 C 0.2783(4) 0.1727(4) 0.0626(4) 0.0479(14) Uani 1 1 d . . . H2 H 0.2482 0.2180 0.0961 0.063(18) Uiso 1 1 calc R . . C3 C 0.3329(4) 0.1982(4) -0.0111(4) 0.0595(17) Uani 1 1 d . . . H3 H 0.3398 0.2600 -0.0254 0.08(2) Uiso 1 1 calc R . . C4 C 0.3765(4) 0.1339(4) -0.0625(4) 0.0571(16) Uani 1 1 d . . . H4 H 0.4113 0.1514 -0.1132 0.074(19) Uiso 1 1 calc R . . C4A C 0.3687(4) 0.0413(4) -0.0389(3) 0.0419(12) Uani 1 1 d . . . C4B C 0.3128(3) 0.0210(3) 0.0368(3) 0.0321(11) Uani 1 1 d . . . C5 C 0.4105(4) -0.0326(4) -0.0869(4) 0.0531(14) Uani 1 1 d . . . H5 H 0.4454 -0.0204 -0.1390 0.053(16) Uiso 1 1 calc R . . C6 C 0.4006(4) -0.1205(4) -0.0585(4) 0.0532(15) Uani 1 1 d . . . H6 H 0.4291 -0.1675 -0.0910 0.054(16) Uiso 1 1 calc R . . C6A C 0.3468(4) -0.1418(3) 0.0211(3) 0.0408(12) Uani 1 1 d . . . C6B C 0.3034(3) -0.0710(3) 0.0679(3) 0.0328(11) Uani 1 1 d . . . C7 C 0.3341(4) -0.2304(4) 0.0568(4) 0.0532(15) Uani 1 1 d . . . H7 H 0.3604 -0.2808 0.0276 0.070(19) Uiso 1 1 calc R . . C8 C 0.2830(4) -0.2423(4) 0.1343(4) 0.0522(15) Uani 1 1 d . . . H8 H 0.2761 -0.3008 0.1590 0.08(2) Uiso 1 1 calc R . . C9 C 0.2411(4) -0.1675(3) 0.1768(3) 0.0429(13) Uani 1 1 d . . . H9 H 0.2058 -0.1771 0.2292 0.040(14) Uiso 1 1 calc R . . N10 N 0.2503(3) -0.0828(3) 0.1443(2) 0.0342(9) Uani 1 1 d . . . N1' N 0.1227(3) -0.0261(3) 0.2816(3) 0.0401(10) Uani 1 1 d . . . C2' C 0.0370(4) -0.0643(4) 0.2806(4) 0.0537(15) Uani 1 1 d . . . H2' H 0.0029 -0.0681 0.2250 0.08(2) Uiso 1 1 calc R . . C3' C -0.0022(5) -0.0983(4) 0.3608(5) 0.0684(19) Uani 1 1 d . . . H3' H -0.0616 -0.1253 0.3583 0.063(18) Uiso 1 1 calc R . . C4' C 0.0460(5) -0.0920(4) 0.4422(5) 0.070(2) Uani 1 1 d . . . H4' H 0.0189 -0.1137 0.4958 0.08(2) Uiso 1 1 calc R . . C4A' C 0.1357(5) -0.0534(4) 0.4467(4) 0.0538(16) Uani 1 1 d . . . C4B' C 0.1716(4) -0.0215(3) 0.3642(3) 0.0420(13) Uani 1 1 d . . . C5' C 0.1927(6) -0.0438(4) 0.5290(4) 0.0677(19) Uani 1 1 d . . . H5' H 0.1702 -0.0648 0.5850 0.062(17) Uiso 1 1 calc R . . C6' C 0.2778(6) -0.0049(4) 0.5267(4) 0.069(2) Uani 1 1 d . . . H6' H 0.3131 0.0009 0.5814 0.066(19) Uiso 1 1 calc R . . C6A' C 0.3160(5) 0.0280(4) 0.4429(4) 0.0502(14) Uani 1 1 d . . . C6B' C 0.2605(4) 0.0204(3) 0.3620(3) 0.0381(12) Uani 1 1 d . . . C7' C 0.4036(5) 0.0687(4) 0.4339(4) 0.0644(19) Uani 1 1 d . . . H7' H 0.4435 0.0752 0.4855 0.047(15) Uiso 1 1 calc R . . C8' C 0.4314(4) 0.0992(4) 0.3504(4) 0.0545(15) Uani 1 1 d . . . H8' H 0.4903 0.1262 0.3447 0.049(16) Uiso 1 1 calc R . . C9' C 0.3715(4) 0.0900(4) 0.2729(4) 0.0470(13) Uani 1 1 d . . . H9' H 0.3912 0.1118 0.2161 0.033(13) Uiso 1 1 calc R . . N10' N 0.2882(3) 0.0516(3) 0.2779(3) 0.0364(10) Uani 1 1 d . . . N2 N 0.0919(3) 0.0080(3) 0.0897(3) 0.0424(11) Uani 1 1 d . . . H2A H 0.0848 -0.0523 0.0822 0.047 Uiso 1 1 calc R . . H2B H 0.1073 0.0334 0.0362 0.047 Uiso 1 1 calc R . . H2C H 0.0381 0.0322 0.1085 0.047 Uiso 1 1 calc R . . N3 N 0.1334(3) 0.1479(3) 0.2133(3) 0.0434(11) Uani 1 1 d . . . H3A H 0.0798 0.1544 0.1806 0.048 Uiso 1 1 calc R . . H3B H 0.1723 0.1937 0.2001 0.048 Uiso 1 1 calc R . . H3C H 0.1213 0.1489 0.2733 0.048 Uiso 1 1 calc R . . Cl1 Cl 0.50052(10) 0.34892(10) 0.19111(9) 0.0478(4) Uani 1 1 d D . . O11A O 0.5513(6) 0.3534(5) 0.1092(5) 0.085(2) Uani 0.857(10) 1 d PDU A 1 O12A O 0.5465(4) 0.3961(4) 0.2645(4) 0.086(2) Uani 0.857(10) 1 d PDU A 1 O13A O 0.4140(4) 0.3957(6) 0.1759(5) 0.108(3) Uani 0.857(10) 1 d PDU A 1 O14A O 0.4850(5) 0.2584(4) 0.2191(5) 0.095(3) Uani 0.857(10) 1 d PDU A 1 O11B O 0.5800(18) 0.362(3) 0.136(2) 0.068(15) Uani 0.143(10) 1 d PDU A 2 O12B O 0.438(2) 0.284(2) 0.151(2) 0.097(14) Uani 0.143(10) 1 d PDU A 2 O13B O 0.451(2) 0.4303(15) 0.204(2) 0.071(12) Uani 0.143(10) 1 d PDU A 2 O14B O 0.533(2) 0.314(3) 0.2770(15) 0.096(15) Uani 0.143(10) 1 d PDU A 2 Cl2 Cl -0.06130(12) -0.28433(10) 0.56737(10) 0.0576(4) Uani 1 1 d D . . O21A O -0.0768(18) -0.2856(15) 0.4701(9) 0.072(5) Uani 0.48(4) 1 d PDU B 1 O22A O -0.1120(14) -0.3551(13) 0.6122(19) 0.088(7) Uani 0.48(4) 1 d PDU B 1 O23A O -0.0850(19) -0.1966(9) 0.6008(10) 0.065(5) Uani 0.48(4) 1 d PDU B 1 O24A O 0.0396(8) -0.2976(13) 0.5897(15) 0.074(5) Uani 0.48(4) 1 d PDU B 1 O21B O -0.1232(17) -0.2081(10) 0.5820(15) 0.076(5) Uani 0.52(4) 1 d PDU B 2 O22B O -0.1103(13) -0.3682(10) 0.5896(12) 0.071(5) Uani 0.52(4) 1 d PDU B 2 O23B O 0.0237(15) -0.2749(17) 0.6167(15) 0.104(6) Uani 0.52(4) 1 d PDU B 2 O24B O -0.0439(17) -0.2902(13) 0.4693(8) 0.068(5) Uani 0.52(4) 1 d PDU B 2 Cl3 Cl 0.14971(11) -0.39070(12) 0.32247(10) 0.0624(4) Uani 1 1 d D . . O31A O 0.2179(6) -0.4344(8) 0.2703(6) 0.101(3) Uani 0.71(2) 1 d PDU C 1 O32A O 0.1765(8) -0.2974(6) 0.3392(6) 0.100(3) Uani 0.71(2) 1 d PDU C 1 O33A O 0.1449(9) -0.4325(5) 0.4115(5) 0.090(3) Uani 0.71(2) 1 d PDU C 1 O34A O 0.0608(6) -0.3961(9) 0.2798(9) 0.127(4) Uani 0.71(2) 1 d PDU C 1 O31B O 0.0796(12) -0.3637(13) 0.2498(11) 0.073(5) Uiso 0.29(2) 1 d PD C 2 O32B O 0.1001(15) -0.4245(13) 0.3963(11) 0.073(5) Uiso 0.29(2) 1 d PD C 2 O33B O 0.2135(13) -0.3212(13) 0.3326(13) 0.073(5) Uiso 0.29(2) 1 d PD C 2 O34B O 0.1980(14) -0.4712(12) 0.2786(13) 0.073(5) Uiso 0.29(2) 1 d PD C 2 O4 O 0.2332(4) 0.1751(5) 0.7353(6) 0.100(2) Uani 1 1 d . . . H4A H 0.269(7) 0.147(6) 0.734(7) 0.110 Uiso 1 1 d . . . H4B H 0.266(7) 0.211(6) 0.756(7) 0.110 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.0389(4) 0.0327(3) 0.0255(3) -0.0018(3) 0.0039(3) -0.0026(3) N1 0.041(2) 0.033(2) 0.031(2) 0.0015(17) 0.0026(18) -0.0028(19) C2 0.054(4) 0.039(3) 0.051(3) 0.006(3) 0.006(3) 0.003(3) C3 0.073(5) 0.046(4) 0.060(4) 0.016(3) 0.019(3) -0.008(3) C4 0.063(4) 0.066(4) 0.043(3) 0.017(3) 0.019(3) -0.011(3) C4A 0.045(3) 0.054(3) 0.027(2) 0.004(2) 0.003(2) -0.004(3) C4B 0.033(3) 0.035(3) 0.028(2) -0.002(2) 0.001(2) -0.001(2) C5 0.054(4) 0.068(4) 0.038(3) -0.005(3) 0.015(3) -0.003(3) C6 0.047(3) 0.066(4) 0.047(3) -0.017(3) 0.013(3) 0.001(3) C6A 0.044(3) 0.037(3) 0.042(3) -0.003(2) 0.002(2) 0.000(2) C6B 0.033(3) 0.038(3) 0.027(2) -0.006(2) 0.000(2) -0.004(2) C7 0.059(4) 0.046(3) 0.055(4) -0.013(3) 0.002(3) 0.006(3) C8 0.066(4) 0.030(3) 0.061(4) -0.003(3) 0.003(3) -0.001(3) C9 0.050(3) 0.039(3) 0.041(3) 0.003(2) 0.008(3) -0.005(3) N10 0.043(2) 0.031(2) 0.029(2) -0.0005(17) 0.0037(18) -0.0019(19) N1' 0.048(3) 0.040(2) 0.033(2) 0.002(2) 0.0057(19) -0.001(2) C2' 0.053(4) 0.055(4) 0.054(4) -0.004(3) 0.016(3) -0.013(3) C3' 0.074(5) 0.061(4) 0.071(4) -0.006(3) 0.036(4) -0.024(4) C4' 0.103(6) 0.056(4) 0.051(4) 0.003(3) 0.031(4) -0.009(4) C4A' 0.086(5) 0.041(3) 0.035(3) 0.001(2) 0.015(3) 0.007(3) C4B' 0.061(4) 0.033(3) 0.033(3) -0.003(2) 0.004(2) 0.004(3) C5' 0.106(6) 0.061(4) 0.036(3) 0.014(3) 0.004(4) 0.009(4) C6' 0.120(7) 0.054(4) 0.032(3) 0.002(3) -0.017(4) 0.023(4) C6A' 0.074(4) 0.034(3) 0.042(3) 0.000(3) -0.011(3) 0.010(3) C6B' 0.061(4) 0.028(3) 0.025(2) -0.002(2) -0.002(2) 0.010(3) C7' 0.096(6) 0.041(3) 0.055(4) -0.017(3) -0.033(4) 0.023(4) C8' 0.045(4) 0.042(3) 0.075(4) -0.008(3) -0.022(3) 0.003(3) C9' 0.049(4) 0.041(3) 0.051(3) -0.003(3) -0.001(3) -0.004(3) N10' 0.045(3) 0.033(2) 0.031(2) -0.0036(17) -0.0018(19) -0.001(2) N2 0.044(3) 0.045(2) 0.038(2) -0.0045(19) 0.006(2) -0.002(2) N3 0.049(3) 0.042(2) 0.040(2) -0.004(2) 0.008(2) -0.001(2) Cl1 0.0522(9) 0.0483(8) 0.0433(7) 0.0003(6) 0.0077(6) -0.0033(7) O11A 0.116(5) 0.076(4) 0.066(4) 0.000(3) 0.047(4) 0.006(4) O12A 0.098(4) 0.084(4) 0.075(4) -0.014(3) -0.023(3) -0.019(3) O13A 0.059(4) 0.150(6) 0.114(5) 0.036(5) 0.000(4) 0.023(4) O14A 0.135(5) 0.054(3) 0.097(5) 0.012(3) 0.031(4) -0.023(3) O11B 0.067(17) 0.070(17) 0.069(17) -0.005(10) 0.022(10) -0.008(10) O12B 0.090(16) 0.097(17) 0.103(17) -0.009(10) -0.005(10) -0.014(10) O13B 0.074(15) 0.057(14) 0.081(15) -0.012(9) 0.007(10) 0.010(9) O14B 0.097(17) 0.101(17) 0.089(16) 0.013(10) -0.009(10) 0.009(10) Cl2 0.0791(12) 0.0473(8) 0.0463(8) 0.0008(7) 0.0009(8) -0.0062(8) O21A 0.073(9) 0.094(8) 0.051(6) -0.021(6) 0.003(5) -0.018(7) O22A 0.097(9) 0.066(8) 0.101(10) 0.037(7) 0.017(7) -0.008(7) O23A 0.086(10) 0.061(6) 0.048(6) -0.014(5) 0.007(6) 0.007(6) O24A 0.061(7) 0.084(8) 0.077(8) -0.010(6) -0.018(5) 0.005(5) O21B 0.089(9) 0.059(6) 0.081(8) -0.011(5) 0.002(7) 0.002(6) O22B 0.095(8) 0.057(7) 0.061(7) -0.006(5) 0.003(6) -0.009(6) O23B 0.118(9) 0.112(10) 0.081(8) -0.006(7) -0.031(7) -0.024(7) O24B 0.073(9) 0.081(7) 0.052(6) -0.020(5) 0.011(5) -0.017(6) Cl3 0.0500(9) 0.0836(12) 0.0536(9) 0.0206(8) 0.0010(7) -0.0080(9) O31A 0.091(5) 0.116(5) 0.098(4) 0.001(4) 0.032(4) 0.004(4) O32A 0.108(5) 0.083(4) 0.109(5) 0.015(4) 0.019(4) -0.016(4) O33A 0.110(5) 0.092(4) 0.067(4) 0.033(3) 0.017(3) 0.001(4) O34A 0.092(5) 0.145(6) 0.141(6) 0.020(4) -0.025(4) -0.008(4) O4 0.087(5) 0.093(5) 0.118(5) 0.026(4) -0.006(4) 0.027(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 Co N10' 1.944(4) . Y Co N3 1.946(4) . Y Co N1 1.946(4) . Y Co N10 1.946(4) . Y Co N1' 1.948(4) . Y Co N2 1.955(4) . Y N1 C2 1.320(6) . ? N1 C4B 1.360(6) . ? C2 C3 1.385(7) . ? C2 H2 0.9300 . ? C3 C4 1.355(8) . ? C3 H3 0.9300 . ? C4 C4A 1.398(7) . ? C4 H4 0.9300 . ? C4A C4B 1.401(6) . ? C4A C5 1.419(7) . ? C4B C6B 1.421(6) . ? C5 C6 1.352(8) . ? C5 H5 0.9300 . ? C6 C6A 1.432(7) . ? C6 H6 0.9300 . ? C6A C6B 1.387(6) . ? C6A C7 1.404(7) . ? C6B N10 1.365(5) . ? C7 C8 1.362(8) . ? C7 H7 0.9300 . ? C8 C9 1.392(7) . ? C8 H8 0.9300 . ? C9 N10 1.328(6) . ? C9 H9 0.9300 . ? N1' C2' 1.338(7) . ? N1' C4B' 1.368(6) . ? C2' C3' 1.392(8) . ? C2' H2' 0.9300 . ? C3' C4' 1.350(9) . ? C3' H3' 0.9300 . ? C4' C4A' 1.392(9) . ? C4' H4' 0.9300 . ? C4A' C4B' 1.391(7) . ? C4A' C5' 1.430(9) . ? C4B' C6B' 1.403(7) . ? C5' C6' 1.336(9) . ? C5' H5' 0.9300 . ? C6' C6A' 1.424(8) . ? C6' H6' 0.9300 . ? C6A' C7' 1.387(9) . ? C6A' C6B' 1.398(7) . ? C6B' N10' 1.366(6) . ? C7' C8' 1.355(8) . ? C7' H7' 0.9300 . ? C8' C9' 1.397(7) . ? C8' H8' 0.9300 . ? C9' N10' 1.312(6) . ? C9' H9' 0.9300 . ? N2 H2A 0.8900 . ? N2 H2B 0.8900 . ? N2 H2C 0.8900 . ? N3 H3A 0.8900 . ? N3 H3B 0.8900 . ? N3 H3C 0.8900 . ? Cl1 O13B 1.396(16) . ? Cl1 O14A 1.399(5) . ? Cl1 O11A 1.404(5) . ? Cl1 O11B 1.407(16) . ? Cl1 O12A 1.410(5) . ? Cl1 O14B 1.411(16) . ? Cl1 O12B 1.414(16) . ? Cl1 O13A 1.417(6) . ? Cl2 O23B 1.392(12) . ? Cl2 O23A 1.411(10) . ? Cl2 O21A 1.419(11) . ? Cl2 O22A 1.423(11) . ? Cl2 O21B 1.435(11) . ? Cl2 O22B 1.446(11) . ? Cl2 O24B 1.449(10) . ? Cl2 O24A 1.474(10) . ? Cl3 O33B 1.363(12) . ? Cl3 O32B 1.384(12) . ? Cl3 O34A 1.394(7) . ? Cl3 O31A 1.396(7) . ? Cl3 O33A 1.428(6) . ? Cl3 O32A 1.430(7) . ? Cl3 O31B 1.482(12) . ? Cl3 O34B 1.507(12) . ? O4 H4A 0.65(8) . ? O4 H4B 0.75(8) . ? 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 N10' Co N3 90.03(17) . . Y N10' Co N1 92.92(17) . . Y N3 Co N1 93.11(16) . . Y N10' Co N10 91.81(16) . . Y N3 Co N10 176.84(16) . . Y N1 Co N10 84.23(16) . . Y N10' Co N1' 84.22(17) . . Y N3 Co N1' 88.90(17) . . Y N1 Co N1' 176.51(18) . . Y N10 Co N1' 93.84(16) . . Y N10' Co N2 177.68(17) . . Y N3 Co N2 90.28(17) . . Y N1 Co N2 89.35(17) . . Y N10 Co N2 87.99(17) . . Y N1' Co N2 93.50(17) . . Y C2 N1 C4B 117.9(4) . . ? C2 N1 Co 130.4(4) . . ? C4B N1 Co 111.7(3) . . ? N1 C2 C3 122.0(5) . . ? N1 C2 H2 119.0 . . ? C3 C2 H2 119.0 . . ? C4 C3 C2 120.6(5) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C4A 119.6(5) . . ? C3 C4 H4 120.2 . . ? C4A C4 H4 120.2 . . ? C4 C4A C4B 116.4(5) . . ? C4 C4A C5 125.2(5) . . ? C4B C4A C5 118.4(5) . . ? N1 C4B C4A 123.5(4) . . ? N1 C4B C6B 116.1(4) . . ? C4A C4B C6B 120.4(4) . . ? C6 C5 C4A 121.4(5) . . ? C6 C5 H5 119.3 . . ? C4A C5 H5 119.3 . . ? C5 C6 C6A 120.8(5) . . ? C5 C6 H6 119.6 . . ? C6A C6 H6 119.6 . . ? C6B C6A C7 116.2(5) . . ? C6B C6A C6 118.9(5) . . ? C7 C6A C6 124.9(5) . . ? N10 C6B C6A 124.3(4) . . ? N10 C6B C4B 115.7(4) . . ? C6A C6B C4B 120.0(4) . . ? C8 C7 C6A 119.7(5) . . ? C8 C7 H7 120.1 . . ? C6A C7 H7 120.1 . . ? C7 C8 C9 120.4(5) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? N10 C9 C8 121.6(5) . . ? N10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? C9 N10 C6B 117.7(4) . . ? C9 N10 Co 130.4(3) . . ? C6B N10 Co 111.7(3) . . ? C2' N1' C4B' 118.1(5) . . ? C2' N1' Co 130.2(4) . . ? C4B' N1' Co 111.7(3) . . ? N1' C2' C3' 121.5(6) . . ? N1' C2' H2' 119.2 . . ? C3' C2' H2' 119.2 . . ? C4' C3' C2' 119.9(6) . . ? C4' C3' H3' 120.1 . . ? C2' C3' H3' 120.1 . . ? C3' C4' C4A' 120.7(6) . . ? C3' C4' H4' 119.6 . . ? C4A' C4' H4' 119.6 . . ? C4B' C4A' C4' 116.8(6) . . ? C4B' C4A' C5' 118.0(6) . . ? C4' C4A' C5' 125.2(6) . . ? N1' C4B' C4A' 123.0(5) . . ? N1' C4B' C6B' 116.0(4) . . ? C4A' C4B' C6B' 121.0(5) . . ? C6' C5' C4A' 120.9(6) . . ? C6' C5' H5' 119.5 . . ? C4A' C5' H5' 119.5 . . ? C5' C6' C6A' 121.9(6) . . ? C5' C6' H6' 119.0 . . ? C6A' C6' H6' 119.0 . . ? C7' C6A' C6B' 116.3(5) . . ? C7' C6A' C6' 125.9(6) . . ? C6B' C6A' C6' 117.8(6) . . ? N10' C6B' C6A' 123.4(5) . . ? N10' C6B' C4B' 116.4(4) . . ? C6A' C6B' C4B' 120.2(5) . . ? C8' C7' C6A' 120.4(6) . . ? C8' C7' H7' 119.8 . . ? C6A' C7' H7' 119.8 . . ? C7' C8' C9' 120.0(6) . . ? C7' C8' H8' 120.0 . . ? C9' C8' H8' 120.0 . . ? N10' C9' C8' 121.8(5) . . ? N10' C9' H9' 119.1 . . ? C8' C9' H9' 119.1 . . ? C9' N10' C6B' 118.1(5) . . ? C9' N10' Co 130.2(4) . . ? C6B' N10' Co 111.7(3) . . ? Co N2 H2A 109.5 . . ? Co N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? Co N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? Co N3 H3A 109.5 . . ? Co N3 H3B 109.5 . . ? H3A N3 H3B 109.5 . . ? Co N3 H3C 109.5 . . ? H3A N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? O14A Cl1 O11A 112.0(4) . . ? O13B Cl1 O11B 112.4(15) . . ? O14A Cl1 O12A 108.4(4) . . ? O11A Cl1 O12A 112.0(5) . . ? O13B Cl1 O14B 109.9(14) . . ? O11B Cl1 O14B 106.9(14) . . ? O13B Cl1 O12B 108.4(14) . . ? O11A Cl1 O12B 90.9(14) . . ? O11B Cl1 O12B 111.2(14) . . ? O14B Cl1 O12B 108.0(14) . . ? O14A Cl1 O13A 110.9(4) . . ? O11A Cl1 O13A 108.0(4) . . ? O12A Cl1 O13A 105.4(4) . . ? O12B Cl1 O13A 74.3(13) . . ? O23A Cl2 O21A 108.6(9) . . ? O23A Cl2 O22A 111.9(9) . . ? O21A Cl2 O22A 112.0(11) . . ? O23B Cl2 O21B 112.0(8) . . ? O23B Cl2 O22B 112.6(9) . . ? O21B Cl2 O22B 108.7(9) . . ? O23B Cl2 O24B 109.9(8) . . ? O21B Cl2 O24B 108.1(8) . . ? O22B Cl2 O24B 105.3(8) . . ? O23A Cl2 O24A 106.5(8) . . ? O21A Cl2 O24A 110.0(8) . . ? O22A Cl2 O24A 107.8(9) . . ? O22B Cl2 O24A 108.1(12) . . ? O33B Cl3 O32B 122.0(11) . . ? O34A Cl3 O31A 111.6(6) . . ? O34A Cl3 O33A 108.2(5) . . ? O31A Cl3 O33A 110.0(5) . . ? O34A Cl3 O32A 111.3(5) . . ? O31A Cl3 O32A 109.8(5) . . ? O33A Cl3 O32A 105.8(5) . . ? O33B Cl3 O31B 108.1(9) . . ? O32B Cl3 O31B 107.2(9) . . ? O33B Cl3 O34B 108.4(9) . . ? O32B Cl3 O34B 107.1(9) . . ? O31B Cl3 O34B 102.2(9) . . ? H4A O4 H4B 88(10) . . ? 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 N10' Co N1 C2 -84.4(5) . . . . ? N3 Co N1 C2 5.8(5) . . . . ? N10 Co N1 C2 -175.9(5) . . . . ? N1' Co N1 C2 -119(3) . . . . ? N2 Co N1 C2 96.0(5) . . . . ? N10' Co N1 C4B 98.0(3) . . . . ? N3 Co N1 C4B -171.8(3) . . . . ? N10 Co N1 C4B 6.5(3) . . . . ? N1' Co N1 C4B 63(3) . . . . ? N2 Co N1 C4B -81.5(3) . . . . ? C4B N1 C2 C3 0.4(8) . . . . ? Co N1 C2 C3 -177.0(4) . . . . ? N1 C2 C3 C4 1.1(9) . . . . ? C2 C3 C4 C4A -2.2(9) . . . . ? C3 C4 C4A C4B 1.7(8) . . . . ? C3 C4 C4A C5 179.9(6) . . . . ? C2 N1 C4B C4A -0.8(7) . . . . ? Co N1 C4B C4A 177.1(4) . . . . ? C2 N1 C4B C6B 176.9(5) . . . . ? Co N1 C4B C6B -5.3(5) . . . . ? C4 C4A C4B N1 -0.2(8) . . . . ? C5 C4A C4B N1 -178.5(5) . . . . ? C4 C4A C4B C6B -177.8(5) . . . . ? C5 C4A C4B C6B 3.9(7) . . . . ? C4 C4A C5 C6 179.0(6) . . . . ? C4B C4A C5 C6 -2.9(8) . . . . ? C4A C5 C6 C6A 0.4(9) . . . . ? C5 C6 C6A C6B 1.1(8) . . . . ? C5 C6 C6A C7 -178.7(6) . . . . ? C7 C6A C6B N10 -0.3(8) . . . . ? C6 C6A C6B N10 179.9(5) . . . . ? C7 C6A C6B C4B 179.8(5) . . . . ? C6 C6A C6B C4B -0.1(7) . . . . ? N1 C4B C6B N10 -0.2(6) . . . . ? C4A C4B C6B N10 177.5(4) . . . . ? N1 C4B C6B C6A 179.8(4) . . . . ? C4A C4B C6B C6A -2.5(7) . . . . ? C6B C6A C7 C8 -1.3(8) . . . . ? C6 C6A C7 C8 178.6(5) . . . . ? C6A C7 C8 C9 1.8(9) . . . . ? C7 C8 C9 N10 -0.8(9) . . . . ? C8 C9 N10 C6B -0.7(8) . . . . ? C8 C9 N10 Co 174.0(4) . . . . ? C6A C6B N10 C9 1.2(7) . . . . ? C4B C6B N10 C9 -178.8(4) . . . . ? C6A C6B N10 Co -174.4(4) . . . . ? C4B C6B N10 Co 5.6(5) . . . . ? N10' Co N10 C9 85.7(5) . . . . ? N3 Co N10 C9 -149(3) . . . . ? N1 Co N10 C9 178.4(5) . . . . ? N1' Co N10 C9 1.3(5) . . . . ? N2 Co N10 C9 -92.0(5) . . . . ? N10' Co N10 C6B -99.4(3) . . . . ? N3 Co N10 C6B 26(3) . . . . ? N1 Co N10 C6B -6.6(3) . . . . ? N1' Co N10 C6B 176.3(3) . . . . ? N2 Co N10 C6B 82.9(3) . . . . ? N10' Co N1' C2' 179.0(5) . . . . ? N3 Co N1' C2' 88.9(5) . . . . ? N1 Co N1' C2' -146(3) . . . . ? N10 Co N1' C2' -89.6(5) . . . . ? N2 Co N1' C2' -1.4(5) . . . . ? N10' Co N1' C4B' 1.9(3) . . . . ? N3 Co N1' C4B' -88.3(3) . . . . ? N1 Co N1' C4B' 37(3) . . . . ? N10 Co N1' C4B' 93.3(3) . . . . ? N2 Co N1' C4B' -178.5(3) . . . . ? C4B' N1' C2' C3' 0.2(8) . . . . ? Co N1' C2' C3' -176.8(4) . . . . ? N1' C2' C3' C4' 0.9(9) . . . . ? C2' C3' C4' C4A' -1.3(10) . . . . ? C3' C4' C4A' C4B' 0.6(9) . . . . ? C3' C4' C4A' C5' -179.8(6) . . . . ? C2' N1' C4B' C4A' -0.9(7) . . . . ? Co N1' C4B' C4A' 176.7(4) . . . . ? C2' N1' C4B' C6B' -179.0(5) . . . . ? Co N1' C4B' C6B' -1.5(5) . . . . ? C4' C4A' C4B' N1' 0.5(8) . . . . ? C5' C4A' C4B' N1' -179.1(5) . . . . ? C4' C4A' C4B' C6B' 178.5(5) . . . . ? C5' C4A' C4B' C6B' -1.1(8) . . . . ? C4B' C4A' C5' C6' 0.2(9) . . . . ? C4' C4A' C5' C6' -179.3(6) . . . . ? C4A' C5' C6' C6A' -0.5(10) . . . . ? C5' C6' C6A' C7' -179.7(6) . . . . ? C5' C6' C6A' C6B' 1.5(9) . . . . ? C7' C6A' C6B' N10' -0.8(7) . . . . ? C6' C6A' C6B' N10' 178.1(5) . . . . ? C7' C6A' C6B' C4B' 178.8(5) . . . . ? C6' C6A' C6B' C4B' -2.3(7) . . . . ? N1' C4B' C6B' N10' -0.1(6) . . . . ? C4A' C4B' C6B' N10' -178.3(4) . . . . ? N1' C4B' C6B' C6A' -179.7(4) . . . . ? C4A' C4B' C6B' C6A' 2.2(7) . . . . ? C6B' C6A' C7' C8' 0.4(8) . . . . ? C6' C6A' C7' C8' -178.4(5) . . . . ? C6A' C7' C8' C9' 0.3(8) . . . . ? C7' C8' C9' N10' -0.6(8) . . . . ? C8' C9' N10' C6B' 0.2(7) . . . . ? C8' C9' N10' Co 179.4(4) . . . . ? C6A' C6B' N10' C9' 0.5(7) . . . . ? C4B' C6B' N10' C9' -179.1(4) . . . . ? C6A' C6B' N10' Co -178.8(4) . . . . ? C4B' C6B' N10' Co 1.6(5) . . . . ? N3 Co N10' C9' -92.2(4) . . . . ? N1 Co N10' C9' 0.9(4) . . . . ? N10 Co N10' C9' 85.2(4) . . . . ? N1' Co N10' C9' 178.9(4) . . . . ? N2 Co N10' C9' 170(4) . . . . ? N3 Co N10' C6B' 87.0(3) . . . . ? N1 Co N10' C6B' -179.9(3) . . . . ? N10 Co N10' C6B' -95.6(3) . . . . ? N1' Co N10' C6B' -1.9(3) . . . . ? N2 Co N10' C6B' -11(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 H2A O24A 0.89 2.28 3.153(19) 166.0 4 N2 H2A O23B 0.89 2.71 3.56(3) 158.2 4 N2 H2A O22B 0.89 3.01 3.52(2) 118.5 4 N2 H2B O33A 0.89 2.40 2.919(7) 117.7 4 N2 H2B O32B 0.89 2.57 3.056(16) 115.0 4 N2 H2A O22A 0.89 3.14 3.67(2) 120.3 4 N2 H2A Cl2 0.89 3.16 3.926(4) 145.4 4 N2 H2A O24B 0.89 3.33 4.08(2) 142.9 4 N2 H2B O22B 0.89 2.32 3.176(19) 161.7 2 N2 H2B O33A 0.89 2.40 2.919(7) 117.7 4 N2 H2B O32B 0.89 2.57 3.056(16) 115.0 4 N2 H2B O21A 0.89 2.67 3.13(2) 113.3 2 N2 H2B O22A 0.89 2.69 3.55(3) 162.7 2 N2 H2B Cl2 0.89 3.11 3.802(4) 136.1 2 N2 H2B O24B 0.89 2.72 3.132(19) 109.2 2 N2 H2C O32B 0.89 2.06 2.911(19) 159.2 2 N2 H2C O34A 0.89 2.41 3.229(15) 153.8 2 N2 H2C O33A 0.89 2.66 3.472(13) 152.5 2 N2 H2C O31B 0.89 3.08 3.89(2) 152.1 2 N2 H2C Cl3 0.89 3.08 3.973(4) 177.8 2 N2 H2B O24B 0.89 2.72 3.132(19) 109.2 2 N2 H2B O21A 0.89 2.67 3.13(2) 113.3 2 N3 H3A O34A 0.89 2.22 2.835(10) 126.1 2 N3 H3A O21A 0.89 2.35 2.918(13) 121.9 2 N3 H3A O24B 0.89 2.36 3.039(17) 133.4 2 N3 H3A O31B 0.89 2.52 3.089(19) 122.8 2 N3 H3A O32B 0.89 2.99 3.79(2) 150.1 2 N3 H3A Cl3 0.89 3.32 4.079(5) 144.1 2 N3 H3B O4 0.89 2.15 2.956(7) 149.5 4_565 N3 H3C O23A 0.89 2.03 2.882(13) 160.4 3_556 N3 H3C O21B 0.89 2.26 3.10(2) 155.6 3_556 N3 H3C Cl2 0.89 3.17 3.903(4) 141.5 3_556 N3 H3C O23B 0.89 3.21 3.84(3) 129.5 3_556 N3 H3C O22A 0.89 3.43 3.95(3) 119.7 3_556 N3 H3A O31B 0.89 2.52 3.089(19) 122.8 2 O4 H4A O13A 0.65(8) 2.33(9) 2.916(10) 151(11) 4_566 O4 H4A O13B 0.65(8) 2.86(9) 3.49(4) 163(11) 4_566 O4 H4A O12B 0.65(8) 2.90(10) 3.24(3) 117(10) 4_566 O4 H4A O31A 0.65(8) 3.23(10) 3.551(14) 115(10) 4_556 O4 H4A Cl1 0.65(8) 3.36(9) 3.881(7) 140(10) 4_566 O4 H4B O14A 0.75(8) 3.20(10) 3.717(10) 128(9) 4_566 O4 H4A O34B 0.65(8) 2.83(10) 3.079(17) 106(10) 4_556 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.524 _refine_diff_density_min -0.415 _refine_diff_density_rms 0.084 #===END data_af7 _database_code_CSD 169190 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'tetra-(ammonia)(1,10-phenanthroline)cobalt(III) perchlorate' ; _chemical_name_common '[Co(phen)(NH3)4](ClO4)3' _chemical_melting_point ? _chemical_formula_moiety C12H20N6O12Cl3Co _chemical_formula_sum 'C12 H20 Cl3 Co N6 O12' _chemical_formula_weight 605.62 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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21 /c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.551(4) _cell_length_b 28.226(4) _cell_length_c 15.1401(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.838(17) _cell_angle_gamma 90.00 _cell_volume 4508.4(19) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.88 _cell_measurement_theta_max 15.31 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.784 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2464 _exptl_absorpt_coefficient_mu 1.189 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.6370 _exptl_absorpt_correction_T_max 0.7792 _exptl_absorpt_process_details 'Sheldrick, 1976' _exptl_special_details ; 'tetra-(ammonia)(1,10-phenanthroline)cobalt(III) perchlorate' ; _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 \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% none _diffrn_reflns_number 8367 _diffrn_reflns_av_R_equivalents 0.0136 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7912 _reflns_number_gt 5929 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD-4 Software' _computing_data_reduction 'PROCESS_DATA (Gable et al., 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL _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^)+(0.0797P)^2^+7.4637P] 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 7912 _refine_ls_number_parameters 761 _refine_ls_number_restraints 272 _refine_ls_R_factor_all 0.0755 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1507 _refine_ls_wR_factor_gt 0.1398 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.110 _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 Co Co 0.19190(6) 0.23892(2) 0.12029(4) 0.02784(18) Uani 1 1 d . . . N1 N 0.0062(4) 0.23856(16) 0.1248(3) 0.0395(10) Uani 1 1 d . . . C2 C -0.0795(6) 0.2612(3) 0.0755(4) 0.0590(17) Uani 1 1 d . . . H2 H -0.0525 0.2811 0.0306 0.065 Uiso 1 1 calc R . . C3 C -0.2100(7) 0.2557(3) 0.0894(6) 0.085(3) Uani 1 1 d . . . H3 H -0.2687 0.2715 0.0536 0.094 Uiso 1 1 calc R . . C4 C -0.2495(7) 0.2272(4) 0.1556(7) 0.093(3) Uani 1 1 d . . . H4 H -0.3358 0.2238 0.1654 0.102 Uiso 1 1 calc R . . C4A C -0.1642(6) 0.2034(3) 0.2083(5) 0.0669(19) Uani 1 1 d . . . C4B C -0.0356(5) 0.2104(2) 0.1912(4) 0.0450(13) Uani 1 1 d . . . C5 C -0.1959(8) 0.1722(3) 0.2793(7) 0.096(3) Uani 1 1 d . . . H5 H -0.2807 0.1669 0.2918 0.106 Uiso 1 1 calc R . . C6 C -0.1074(10) 0.1506(3) 0.3278(6) 0.092(3) Uani 1 1 d . . . H6 H -0.1320 0.1309 0.3738 0.101 Uiso 1 1 calc R . . C6A C 0.0245(7) 0.1567(2) 0.3115(4) 0.0596(18) Uani 1 1 d . . . C6B C 0.0572(5) 0.18788(18) 0.2428(3) 0.0405(12) Uani 1 1 d . . . C7 C 0.1244(9) 0.1350(2) 0.3586(4) 0.072(2) Uani 1 1 d . . . H7 H 0.1074 0.1145 0.4049 0.079 Uiso 1 1 calc R . . C8 C 0.2440(8) 0.1442(2) 0.3366(4) 0.0629(19) Uani 1 1 d . . . H8 H 0.3101 0.1295 0.3672 0.069 Uiso 1 1 calc R . . C9 C 0.2707(6) 0.17545(18) 0.2684(3) 0.0449(13) Uani 1 1 d . . . H9 H 0.3548 0.1816 0.2548 0.049 Uiso 1 1 calc R . . N10 N 0.1790(4) 0.19680(13) 0.2220(2) 0.0323(9) Uani 1 1 d . . . N2 N 0.3780(4) 0.23750(15) 0.1225(3) 0.0393(10) Uani 1 1 d . . . H2A H 0.4075 0.2613 0.0902 0.043 Uiso 1 1 calc R . . H2B H 0.4047 0.2101 0.1003 0.043 Uiso 1 1 calc R . . H2C H 0.4061 0.2404 0.1779 0.043 Uiso 1 1 calc R . . N3 N 0.1960(4) 0.29507(14) 0.1967(3) 0.0382(10) Uani 1 1 d . . . H3A H 0.2518 0.3158 0.1761 0.042 Uiso 1 1 calc R . . H3B H 0.2185 0.2866 0.2513 0.042 Uiso 1 1 calc R . . H3C H 0.1194 0.3083 0.1973 0.042 Uiso 1 1 calc R . . N4 N 0.1887(4) 0.18241(14) 0.0446(3) 0.0356(9) Uani 1 1 d . . . H4A H 0.2316 0.1882 -0.0044 0.039 Uiso 1 1 calc R . . H4B H 0.1088 0.1752 0.0305 0.039 Uiso 1 1 calc R . . H4C H 0.2242 0.1582 0.0734 0.039 Uiso 1 1 calc R . . N5 N 0.1945(4) 0.27964(15) 0.0162(3) 0.0409(10) Uani 1 1 d . . . H5A H 0.2743 0.2844 0.0002 0.045 Uiso 1 1 calc R . . H5B H 0.1585 0.3073 0.0287 0.045 Uiso 1 1 calc R . . H5C H 0.1519 0.2658 -0.0279 0.045 Uiso 1 1 calc R . . Co' Co 0.30397(6) 0.56521(2) 0.66016(4) 0.02661(17) Uani 1 1 d . . . N1' N 0.3101(4) 0.52253(13) 0.7626(3) 0.0333(9) Uani 1 1 d . . . C2' C 0.2161(6) 0.50701(18) 0.8129(4) 0.0443(13) Uani 1 1 d . . . H2' H 0.1328 0.5137 0.7962 0.049 Uiso 1 1 calc R . . C3' C 0.2393(7) 0.4811(2) 0.8897(4) 0.0579(17) Uani 1 1 d . . . H3' H 0.1718 0.4718 0.9245 0.064 Uiso 1 1 calc R . . C4' C 0.3586(8) 0.4692(2) 0.9142(4) 0.0629(19) Uani 1 1 d . . . H4' H 0.3735 0.4515 0.9651 0.069 Uiso 1 1 calc R . . C4A' C 0.4595(7) 0.48391(19) 0.8619(4) 0.0535(16) Uani 1 1 d . . . C4B' C 0.4298(5) 0.51152(17) 0.7872(3) 0.0376(12) Uani 1 1 d . . . C5' C 0.5908(8) 0.4736(2) 0.8796(5) 0.074(2) Uani 1 1 d . . . H5' H 0.6127 0.4549 0.9279 0.081 Uiso 1 1 calc R . . C6' C 0.6815(8) 0.4903(3) 0.8282(6) 0.077(2) Uani 1 1 d . . . H6' H 0.7655 0.4828 0.8415 0.085 Uiso 1 1 calc R . . C6A' C 0.6539(6) 0.5194(2) 0.7533(4) 0.0550(16) Uani 1 1 d . . . C6B' C 0.5277(5) 0.53015(18) 0.7340(3) 0.0380(12) Uani 1 1 d . . . C7' C 0.7432(6) 0.5392(3) 0.6966(6) 0.073(2) Uani 1 1 d . . . H7' H 0.8290 0.5332 0.7060 0.080 Uiso 1 1 calc R . . C8' C 0.7058(6) 0.5670(3) 0.6280(5) 0.069(2) Uani 1 1 d . . . H8' H 0.7654 0.5794 0.5897 0.076 Uiso 1 1 calc R . . C9' C 0.5770(5) 0.5769(2) 0.6153(4) 0.0489(14) Uani 1 1 d . . . H9' H 0.5526 0.5970 0.5695 0.054 Uiso 1 1 calc R . . N10' N 0.4885(4) 0.55868(15) 0.6664(3) 0.0365(9) Uani 1 1 d . . . N2' N 0.2965(4) 0.51140(14) 0.5782(3) 0.0385(10) Uani 1 1 d . . . H2A' H 0.2460 0.5186 0.5325 0.042 Uiso 1 1 calc R . . H2B' H 0.2660 0.4861 0.6060 0.042 Uiso 1 1 calc R . . H2C' H 0.3740 0.5051 0.5590 0.042 Uiso 1 1 calc R . . N3' N 0.3113(4) 0.61898(14) 0.7414(3) 0.0341(9) Uani 1 1 d . . . H3A' H 0.2511 0.6397 0.7268 0.038 Uiso 1 1 calc R . . H3B' H 0.3869 0.6328 0.7381 0.038 Uiso 1 1 calc R . . H3C' H 0.2994 0.6088 0.7963 0.038 Uiso 1 1 calc R . . N4' N 0.3068(4) 0.60908(15) 0.5591(3) 0.0368(9) Uani 1 1 d . . . H4A' H 0.3330 0.5937 0.5114 0.040 Uiso 1 1 calc R . . H4B' H 0.3594 0.6329 0.5712 0.040 Uiso 1 1 calc R . . H4C' H 0.2291 0.6204 0.5492 0.040 Uiso 1 1 calc R . . N5' N 0.1184(4) 0.56757(15) 0.6583(3) 0.0352(9) Uani 1 1 d . . . H5A' H 0.0876 0.5382 0.6557 0.039 Uiso 1 1 calc R . . H5B' H 0.0918 0.5839 0.6113 0.039 Uiso 1 1 calc R . . H6C' H 0.0916 0.5817 0.7072 0.039 Uiso 1 1 calc R . . Cl1 Cl 0.47337(13) 0.40169(4) 0.63461(8) 0.0422(3) Uani 1 1 d D . . O11 O 0.5323(4) 0.44025(13) 0.5891(3) 0.0578(11) Uani 1 1 d D A . O12A O 0.510(2) 0.3988(7) 0.7232(8) 0.077(6) Uani 0.48(5) 1 d PDU A 1 O13A O 0.507(2) 0.3585(5) 0.5921(15) 0.071(5) Uani 0.48(5) 1 d PDU A 1 O14A O 0.3396(10) 0.4065(7) 0.6271(17) 0.066(5) Uani 0.48(5) 1 d PDU A 1 O12B O 0.544(3) 0.3871(10) 0.7090(16) 0.128(9) Uani 0.52(5) 1 d PD A 2 O13B O 0.456(3) 0.3638(6) 0.5749(10) 0.072(6) Uani 0.52(5) 1 d PD A 2 O14B O 0.354(2) 0.4180(7) 0.666(2) 0.091(7) Uani 0.52(5) 1 d PD A 2 Cl2 Cl 0.01114(12) 0.56399(4) 0.40842(8) 0.0379(3) Uani 1 1 d D . . O21 O -0.0036(6) 0.61015(15) 0.3792(4) 0.0902(17) Uani 1 1 d D . . O22 O -0.0249(5) 0.53150(17) 0.3426(3) 0.0826(15) Uani 1 1 d D . . O23 O 0.1369(5) 0.5555(2) 0.4354(4) 0.0950(18) Uani 1 1 d D . . O24 O -0.0678(6) 0.5574(2) 0.4845(4) 0.107(2) Uani 1 1 d D . . Cl3 Cl 0.46834(13) 0.27667(5) 0.37302(8) 0.0431(3) Uani 1 1 d D . . O31A O 0.3350(6) 0.2738(4) 0.3807(6) 0.076(3) Uani 0.750(14) 1 d PDU B 1 O32A O 0.5055(8) 0.2457(4) 0.3047(6) 0.085(3) Uani 0.750(14) 1 d PDU B 1 O33A O 0.5100(10) 0.3223(3) 0.3568(8) 0.122(4) Uani 0.750(14) 1 d PDU B 1 O34A O 0.5204(9) 0.2607(4) 0.4544(5) 0.115(4) Uani 0.750(14) 1 d PDU B 1 O31B O 0.5417(17) 0.3044(8) 0.4262(15) 0.078(8) Uani 0.250(14) 1 d PDU B 2 O32B O 0.461(3) 0.2323(7) 0.4169(19) 0.128(12) Uani 0.250(14) 1 d PDU B 2 O33B O 0.504(2) 0.2706(10) 0.2881(10) 0.077(8) Uani 0.250(14) 1 d PDU B 2 O34B O 0.3409(15) 0.2966(9) 0.3721(16) 0.070(8) Uani 0.250(14) 1 d PDU B 2 Cl4 Cl -0.00833(16) 0.40489(5) 0.09294(10) 0.0571(4) Uani 1 1 d D . . O41A O 0.0047(8) 0.4374(2) 0.0262(5) 0.107(3) Uani 0.859(12) 1 d PDU C 1 O42A O 0.0473(9) 0.3608(3) 0.0709(5) 0.095(3) Uani 0.859(12) 1 d PDU C 1 O43A O -0.1404(6) 0.3953(3) 0.1038(6) 0.109(3) Uani 0.859(12) 1 d PDU C 1 O44A O 0.0347(7) 0.4213(3) 0.1761(5) 0.112(3) Uani 0.859(12) 1 d PDU C 1 O41B O -0.086(3) 0.4149(14) 0.0189(19) 0.105(17) Uani 0.141(12) 1 d PDU C 2 O42B O 0.092(3) 0.3752(11) 0.072(3) 0.065(13) Uani 0.141(12) 1 d PDU C 2 O43B O 0.053(3) 0.4511(8) 0.112(3) 0.094(15) Uani 0.141(12) 1 d PDU C 2 O44B O -0.074(4) 0.3933(13) 0.166(2) 0.103(16) Uani 0.141(12) 1 d PDU C 2 Cl5 Cl 0.05709(15) 0.69581(5) 0.63304(9) 0.0529(4) Uani 1 1 d D . . O51A O -0.0426(7) 0.7294(2) 0.6250(4) 0.0533(18) Uani 0.847(10) 1 d PDU D 1 O52A O 0.0597(6) 0.6767(2) 0.7190(3) 0.073(2) Uani 0.847(10) 1 d PDU D 1 O53A O 0.0485(7) 0.6623(2) 0.5656(4) 0.073(2) Uani 0.847(10) 1 d PDU D 1 O54A O 0.1800(6) 0.7187(3) 0.6233(5) 0.115(3) Uani 0.847(10) 1 d PDU D 1 O51B O 0.133(3) 0.6942(13) 0.7071(18) 0.114(18) Uani 0.153(10) 1 d PDU D 2 O52B O 0.114(3) 0.6798(12) 0.5561(16) 0.086(14) Uani 0.153(10) 1 d PDU D 2 O53B O -0.047(3) 0.6610(10) 0.647(3) 0.119(17) Uani 0.153(10) 1 d PDU D 2 O54B O -0.004(3) 0.7397(8) 0.620(3) 0.056(14) Uani 0.153(10) 1 d PDU D 2 O61 O 0.5338(5) 0.40510(16) 0.0837(4) 0.0868(17) Uani 1 1 d D . . Cl6A Cl 0.4950(11) 0.3623(3) 0.0563(7) 0.062(2) Uani 0.370(11) 1 d PD E 1 O62A O 0.526(2) 0.3275(6) 0.1213(11) 0.127(5) Uiso 0.370(11) 1 d PD E 1 O63A O 0.3848(15) 0.3514(7) 0.0191(12) 0.127(5) Uiso 0.370(11) 1 d PD E 1 O64A O 0.5615(16) 0.3563(6) -0.0251(10) 0.127(5) Uiso 0.370(11) 1 d PD E 1 Cl6B Cl 0.4580(6) 0.36568(19) 0.0868(4) 0.0554(12) Uani 0.630(11) 1 d PD E 2 O62B O 0.4218(11) 0.3585(4) 0.1768(7) 0.140(3) Uiso 0.630(11) 1 d PD E 2 O63B O 0.5388(12) 0.3244(4) 0.0817(9) 0.140(3) Uiso 0.630(11) 1 d PD E 2 O64B O 0.3466(11) 0.3698(5) 0.0465(8) 0.140(3) Uiso 0.630(11) 1 d PD E 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.0302(3) 0.0276(3) 0.0258(3) -0.0014(2) 0.0028(2) -0.0001(3) N1 0.032(2) 0.049(3) 0.038(2) -0.012(2) 0.0019(19) 0.0015(19) C2 0.046(3) 0.083(5) 0.047(4) -0.014(3) -0.005(3) 0.017(3) C3 0.043(4) 0.127(7) 0.085(6) -0.034(5) -0.014(4) 0.026(4) C4 0.037(4) 0.129(8) 0.112(7) -0.040(6) 0.019(4) -0.020(5) C4A 0.036(3) 0.086(5) 0.080(5) -0.022(4) 0.015(3) -0.014(3) C4B 0.041(3) 0.046(3) 0.049(3) -0.016(3) 0.015(3) -0.010(2) C5 0.068(5) 0.102(7) 0.119(8) -0.023(6) 0.056(5) -0.042(5) C6 0.107(7) 0.078(6) 0.092(6) -0.002(5) 0.060(6) -0.025(5) C6A 0.086(5) 0.039(3) 0.055(4) -0.009(3) 0.031(4) -0.021(3) C6B 0.051(3) 0.035(3) 0.035(3) -0.011(2) 0.010(2) -0.009(2) C7 0.142(8) 0.039(3) 0.036(3) 0.004(3) 0.023(4) 0.006(4) C8 0.113(6) 0.039(3) 0.037(3) 0.008(3) -0.006(4) 0.007(4) C9 0.061(4) 0.038(3) 0.035(3) -0.001(2) -0.008(3) 0.000(3) N10 0.045(2) 0.025(2) 0.028(2) -0.0034(16) 0.0017(18) -0.0027(17) N2 0.034(2) 0.037(2) 0.047(3) 0.0006(19) 0.0067(19) 0.0000(18) N3 0.045(2) 0.034(2) 0.036(2) -0.0025(18) 0.0074(19) 0.0012(19) N4 0.042(2) 0.034(2) 0.031(2) -0.0022(17) 0.0009(18) 0.0003(18) N5 0.054(3) 0.037(2) 0.032(2) 0.0019(18) 0.006(2) 0.006(2) Co' 0.0251(3) 0.0289(3) 0.0258(3) -0.0015(2) 0.0021(2) 0.0006(2) N1' 0.040(2) 0.028(2) 0.032(2) -0.0025(17) 0.0012(18) 0.0011(17) C2' 0.054(3) 0.036(3) 0.043(3) 0.001(2) 0.014(3) -0.002(2) C3' 0.089(5) 0.042(3) 0.043(3) 0.005(3) 0.019(3) -0.006(3) C4' 0.112(6) 0.037(3) 0.040(3) 0.009(3) -0.009(4) -0.003(4) C4A' 0.080(4) 0.034(3) 0.046(3) -0.001(3) -0.017(3) 0.010(3) C4B' 0.049(3) 0.029(3) 0.035(3) -0.005(2) -0.010(2) 0.005(2) C5' 0.093(6) 0.049(4) 0.077(5) 0.001(4) -0.040(5) 0.016(4) C6' 0.066(5) 0.069(5) 0.096(6) -0.015(4) -0.041(4) 0.031(4) C6A' 0.040(3) 0.056(4) 0.068(4) -0.017(3) -0.016(3) 0.014(3) C6B' 0.034(3) 0.039(3) 0.041(3) -0.014(2) -0.007(2) 0.010(2) C7' 0.033(3) 0.089(5) 0.097(6) -0.024(5) -0.013(4) 0.013(3) C8' 0.034(3) 0.107(6) 0.067(4) -0.017(4) 0.013(3) -0.002(3) C9' 0.031(3) 0.069(4) 0.047(3) -0.004(3) 0.008(2) -0.001(3) N10' 0.032(2) 0.042(2) 0.035(2) -0.0091(19) -0.0012(18) 0.0044(18) N2' 0.042(2) 0.036(2) 0.037(2) -0.0040(18) -0.0008(19) 0.0060(19) N3' 0.035(2) 0.036(2) 0.031(2) -0.0025(17) -0.0017(17) -0.0010(18) N4' 0.036(2) 0.040(2) 0.034(2) 0.0027(18) 0.0049(18) 0.0001(19) N5' 0.028(2) 0.040(2) 0.037(2) -0.0016(18) 0.0034(17) 0.0014(17) Cl1 0.0492(8) 0.0384(7) 0.0392(7) -0.0016(5) 0.0047(6) 0.0007(6) O11 0.065(3) 0.040(2) 0.069(3) -0.005(2) 0.018(2) -0.0153(19) O12A 0.087(9) 0.092(9) 0.049(7) -0.009(6) -0.005(6) -0.011(7) O13A 0.085(9) 0.046(6) 0.083(9) -0.006(6) 0.022(7) 0.003(6) O14A 0.038(6) 0.069(8) 0.092(9) 0.019(7) 0.001(6) -0.002(5) O12B 0.119(14) 0.159(18) 0.103(13) 0.037(12) -0.044(11) 0.032(13) O13B 0.117(15) 0.046(7) 0.053(7) -0.009(5) 0.010(8) -0.032(7) O14B 0.097(10) 0.072(9) 0.107(15) 0.030(9) 0.069(9) 0.029(7) Cl2 0.0418(7) 0.0319(6) 0.0399(7) 0.0012(5) -0.0064(5) -0.0018(5) O21 0.148(5) 0.039(2) 0.084(4) 0.012(2) 0.005(3) 0.014(3) O22 0.101(4) 0.066(3) 0.080(3) -0.028(3) -0.021(3) -0.016(3) O23 0.060(3) 0.107(4) 0.116(5) 0.002(4) -0.038(3) 0.007(3) O24 0.109(5) 0.134(5) 0.078(4) 0.010(4) 0.043(3) -0.024(4) Cl3 0.0438(7) 0.0523(8) 0.0334(7) -0.0030(6) 0.0042(5) -0.0130(6) O31A 0.051(4) 0.095(6) 0.084(5) -0.007(5) 0.025(3) -0.018(4) O32A 0.090(5) 0.091(6) 0.074(5) -0.043(4) 0.020(4) -0.010(5) O33A 0.152(7) 0.063(5) 0.152(8) 0.007(5) 0.050(6) -0.037(5) O34A 0.123(7) 0.162(8) 0.060(4) 0.013(5) -0.009(4) 0.034(6) O31B 0.078(10) 0.072(11) 0.084(11) -0.031(8) -0.015(8) -0.021(8) O32B 0.134(15) 0.116(14) 0.134(15) 0.030(10) 0.002(10) -0.017(10) O33B 0.082(11) 0.102(12) 0.048(9) -0.001(8) 0.011(8) -0.015(9) O34B 0.064(10) 0.080(12) 0.065(10) 0.003(9) -0.009(8) 0.006(8) Cl4 0.0758(11) 0.0476(8) 0.0487(8) -0.0026(6) 0.0249(8) 0.0118(7) O41A 0.149(6) 0.072(4) 0.103(5) 0.036(4) 0.061(5) 0.011(4) O42A 0.122(6) 0.070(4) 0.093(5) -0.016(4) 0.018(4) 0.039(5) O43A 0.078(4) 0.119(5) 0.130(6) -0.002(5) 0.033(4) -0.010(4) O44A 0.115(6) 0.144(6) 0.076(5) -0.049(4) 0.003(4) -0.001(5) O41B 0.103(19) 0.111(19) 0.100(19) -0.005(10) -0.004(10) 0.008(10) O42B 0.062(15) 0.069(16) 0.063(15) -0.007(10) 0.008(10) 0.016(10) O43B 0.093(17) 0.085(17) 0.103(18) -0.007(10) 0.000(10) -0.006(10) O44B 0.107(19) 0.107(18) 0.096(18) 0.001(10) 0.017(10) 0.000(10) Cl5 0.0581(9) 0.0615(9) 0.0390(7) -0.0053(6) -0.0024(6) 0.0239(7) O51A 0.057(4) 0.053(3) 0.050(3) -0.004(3) -0.002(3) 0.031(3) O52A 0.087(4) 0.087(4) 0.046(3) 0.016(3) 0.001(3) 0.043(4) O53A 0.089(5) 0.066(4) 0.064(4) -0.026(3) -0.024(3) 0.035(3) O54A 0.067(4) 0.155(6) 0.122(6) -0.012(5) 0.014(4) -0.033(4) O51B 0.12(2) 0.11(2) 0.11(2) -0.003(10) -0.007(11) 0.004(10) O52B 0.085(16) 0.083(16) 0.090(16) -0.004(10) 0.012(10) 0.015(10) O53B 0.113(19) 0.115(19) 0.13(2) 0.005(10) 0.006(10) 0.001(10) O54B 0.059(17) 0.053(16) 0.055(15) 0.001(9) -0.006(10) -0.001(9) O61 0.116(4) 0.050(3) 0.093(4) 0.007(3) -0.036(3) -0.032(3) Cl6A 0.083(6) 0.043(3) 0.058(5) 0.013(3) -0.026(4) -0.001(3) Cl6B 0.076(3) 0.0401(17) 0.050(3) 0.0078(17) -0.0221(19) -0.0189(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co N5 1.952(4) . Y Co N10 1.952(4) . Y Co N1 1.962(4) . Y Co N3 1.962(4) . Y Co N2 1.964(4) . Y Co N4 1.964(4) . Y N1 C2 1.327(7) . ? N1 C4B 1.360(7) . ? C2 C3 1.404(10) . ? C2 H2 0.9300 . ? C3 C4 1.356(12) . ? C3 H3 0.9300 . ? C4 C4A 1.370(12) . ? C4 H4 0.9300 . ? C4A C4B 1.400(8) . ? C4A C5 1.434(12) . ? C4B C6B 1.397(8) . ? C5 C6 1.327(13) . ? C5 H5 0.9300 . ? C6 C6A 1.427(11) . ? C6 H6 0.9300 . ? C6A C7 1.404(10) . ? C6A C6B 1.410(8) . ? C6B N10 1.351(7) . ? C7 C8 1.335(11) . ? C7 H7 0.9300 . ? C8 C9 1.391(8) . ? C8 H8 0.9300 . ? C9 N10 1.331(7) . ? C9 H9 0.9300 . ? N2 H2A 0.8900 . ? N2 H2B 0.8900 . ? N2 H2C 0.8900 . ? N3 H3A 0.8900 . ? N3 H3B 0.8900 . ? N3 H3C 0.8900 . ? N4 H4A 0.8900 . ? N4 H4B 0.8900 . ? N4 H4C 0.8900 . ? N5 H5A 0.8900 . ? N5 H5B 0.8900 . ? N5 H5C 0.8900 . ? Co' N3' 1.955(4) . Y Co' N10' 1.957(4) . Y Co' N5' 1.958(4) . Y Co' N2' 1.962(4) . Y Co' N1' 1.964(4) . Y Co' N4' 1.969(4) . Y N1' C2' 1.333(6) . ? N1' C4B' 1.348(6) . ? C2' C3' 1.393(8) . ? C2' H2' 0.9300 . ? C3' C4' 1.349(10) . ? C3' H3' 0.9300 . ? C4' C4A' 1.399(9) . ? C4' H4' 0.9300 . ? C4A' C4B' 1.405(7) . ? C4A' C5' 1.437(10) . ? C4B' C6B' 1.420(8) . ? C5' C6' 1.328(11) . ? C5' H5' 0.9300 . ? C6' C6A' 1.426(10) . ? C6' H6' 0.9300 . ? C6A' C6B' 1.393(7) . ? C6A' C7' 1.401(10) . ? C6B' N10' 1.361(7) . ? C7' C8' 1.355(10) . ? C7' H7' 0.9300 . ? C8' C9' 1.398(8) . ? C8' H8' 0.9300 . ? C9' N10' 1.326(7) . ? C9' H9' 0.9300 . ? N2' H2A' 0.8900 . ? N2' H2B' 0.8900 . ? N2' H2C' 0.8900 . ? N3' H3A' 0.8900 . ? N3' H3B' 0.8900 . ? N3' H3C' 0.8900 . ? N4' H4A' 0.8900 . ? N4' H4B' 0.8900 . ? N4' H4C' 0.8900 . ? N5' H5A' 0.8900 . ? N5' H5B' 0.8900 . ? N5' H6C' 0.8900 . ? Cl1 O12A 1.392(11) . ? Cl1 O12B 1.404(11) . ? Cl1 O13B 1.412(10) . ? Cl1 O14A 1.421(11) . ? Cl1 O13A 1.425(11) . ? Cl1 O14B 1.433(10) . ? Cl1 O11 1.435(4) . ? Cl2 O21 1.384(4) . ? Cl2 O22 1.402(4) . ? Cl2 O23 1.403(5) . ? Cl2 O24 1.443(5) . ? Cl3 O33B 1.354(14) . ? Cl3 O31B 1.357(12) . ? Cl3 O33A 1.383(7) . ? Cl3 O32A 1.414(6) . ? Cl3 O34A 1.415(7) . ? Cl3 O31A 1.416(6) . ? Cl3 O32B 1.420(15) . ? Cl3 O34B 1.458(14) . ? Cl4 O44B 1.355(17) . ? Cl4 O41A 1.373(6) . ? Cl4 O42B 1.392(17) . ? Cl4 O41B 1.407(18) . ? Cl4 O44A 1.410(6) . ? Cl4 O42A 1.418(6) . ? Cl4 O43A 1.432(6) . ? Cl4 O43B 1.482(17) . ? Cl5 O51B 1.372(17) . ? Cl5 O52B 1.393(17) . ? Cl5 O53A 1.394(5) . ? Cl5 O54B 1.408(17) . ? Cl5 O52A 1.410(5) . ? Cl5 O51A 1.420(5) . ? Cl5 O54A 1.458(6) . ? Cl5 O53B 1.495(18) . ? O61 Cl6A 1.341(10) . ? O61 Cl6B 1.372(7) . ? Cl6A O63A 1.320(14) . ? Cl6A O62A 1.426(14) . ? Cl6A O64A 1.437(15) . ? Cl6B O64B 1.322(11) . ? Cl6B O62B 1.434(11) . ? Cl6B O63B 1.446(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 N5 Co N10 176.46(18) . . Y N5 Co N1 93.25(19) . . Y N10 Co N1 83.60(18) . . Y N5 Co N3 90.01(18) . . Y N10 Co N3 91.60(16) . . Y N1 Co N3 89.83(17) . . Y N5 Co N2 89.98(19) . . Y N10 Co N2 93.18(18) . . Y N1 Co N2 176.72(19) . . Y N3 Co N2 89.62(18) . . Y N5 Co N4 90.41(17) . . Y N10 Co N4 87.99(16) . . Y N1 Co N4 90.41(17) . . Y N3 Co N4 179.51(18) . . Y N2 Co N4 90.12(18) . . Y C2 N1 C4B 118.1(5) . . ? C2 N1 Co 130.6(4) . . ? C4B N1 Co 111.3(4) . . ? N1 C2 C3 121.6(7) . . ? N1 C2 H2 119.2 . . ? C3 C2 H2 119.2 . . ? C4 C3 C2 119.3(8) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C4A 121.0(7) . . ? C3 C4 H4 119.5 . . ? C4A C4 H4 119.5 . . ? C4 C4A C4B 117.0(7) . . ? C4 C4A C5 125.5(7) . . ? C4B C4A C5 117.6(7) . . ? N1 C4B C6B 116.6(5) . . ? N1 C4B C4A 123.0(6) . . ? C6B C4B C4A 120.4(6) . . ? C6 C5 C4A 121.9(7) . . ? C6 C5 H5 119.1 . . ? C4A C5 H5 119.1 . . ? C5 C6 C6A 121.9(8) . . ? C5 C6 H6 119.0 . . ? C6A C6 H6 119.0 . . ? C7 C6A C6B 117.1(6) . . ? C7 C6A C6 125.9(7) . . ? C6B C6A C6 116.9(7) . . ? N10 C6B C4B 116.5(5) . . ? N10 C6B C6A 122.2(6) . . ? C4B C6B C6A 121.3(6) . . ? C8 C7 C6A 119.6(6) . . ? C8 C7 H7 120.2 . . ? C6A C7 H7 120.2 . . ? C7 C8 C9 120.7(7) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? N10 C9 C8 121.7(6) . . ? N10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? C9 N10 C6B 118.6(5) . . ? C9 N10 Co 129.3(4) . . ? C6B N10 Co 112.0(3) . . ? Co N2 H2A 109.5 . . ? Co N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? Co N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? Co N3 H3A 109.5 . . ? Co N3 H3B 109.5 . . ? H3A N3 H3B 109.5 . . ? Co N3 H3C 109.5 . . ? H3A N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? Co N4 H4A 109.5 . . ? Co N4 H4B 109.5 . . ? H4A N4 H4B 109.5 . . ? Co N4 H4C 109.5 . . ? H4A N4 H4C 109.5 . . ? H4B N4 H4C 109.5 . . ? Co N5 H5A 109.5 . . ? Co N5 H5B 109.5 . . ? H5A N5 H5B 109.5 . . ? Co N5 H5C 109.5 . . ? H5A N5 H5C 109.5 . . ? H5B N5 H5C 109.5 . . ? N3' Co' N10' 90.69(17) . . Y N3' Co' N5' 90.75(17) . . Y N10' Co' N5' 176.02(18) . . Y N3' Co' N2' 179.79(18) . . Y N10' Co' N2' 89.36(17) . . Y N5' Co' N2' 89.21(17) . . Y N3' Co' N1' 88.77(16) . . Y N10' Co' N1' 83.27(17) . . Y N5' Co' N1' 93.06(17) . . Y N2' Co' N1' 91.44(17) . . Y N3' Co' N4' 89.98(17) . . Y N10' Co' N4' 94.06(18) . . Y N5' Co' N4' 89.65(17) . . Y N2' Co' N4' 89.81(18) . . Y N1' Co' N4' 177.03(18) . . Y C2' N1' C4B' 117.9(5) . . ? C2' N1' Co' 129.5(4) . . ? C4B' N1' Co' 112.3(3) . . ? N1' C2' C3' 121.8(6) . . ? N1' C2' H2' 119.1 . . ? C3' C2' H2' 119.1 . . ? C4' C3' C2' 120.8(6) . . ? C4' C3' H3' 119.6 . . ? C2' C3' H3' 119.6 . . ? C3' C4' C4A' 119.0(6) . . ? C3' C4' H4' 120.5 . . ? C4A' C4' H4' 120.5 . . ? C4' C4A' C4B' 117.2(6) . . ? C4' C4A' C5' 125.0(6) . . ? C4B' C4A' C5' 117.7(6) . . ? N1' C4B' C4A' 123.2(5) . . ? N1' C4B' C6B' 116.4(4) . . ? C4A' C4B' C6B' 120.4(5) . . ? C6' C5' C4A' 121.3(7) . . ? C6' C5' H5' 119.3 . . ? C4A' C5' H5' 119.3 . . ? C5' C6' C6A' 122.0(6) . . ? C5' C6' H6' 119.0 . . ? C6A' C6' H6' 119.0 . . ? C6B' C6A' C7' 115.7(6) . . ? C6B' C6A' C6' 118.4(6) . . ? C7' C6A' C6' 125.9(6) . . ? N10' C6B' C6A' 124.4(5) . . ? N10' C6B' C4B' 115.4(4) . . ? C6A' C6B' C4B' 120.1(5) . . ? C8' C7' C6A' 120.7(6) . . ? C8' C7' H7' 119.7 . . ? C6A' C7' H7' 119.7 . . ? C7' C8' C9' 119.6(6) . . ? C7' C8' H8' 120.2 . . ? C9' C8' H8' 120.2 . . ? N10' C9' C8' 122.2(6) . . ? N10' C9' H9' 118.9 . . ? C8' C9' H9' 118.9 . . ? C9' N10' C6B' 117.4(5) . . ? C9' N10' Co' 130.1(4) . . ? C6B' N10' Co' 112.5(3) . . ? Co' N2' H2A' 109.5 . . ? Co' N2' H2B' 109.5 . . ? H2A' N2' H2B' 109.5 . . ? Co' N2' H2C' 109.5 . . ? H2A' N2' H2C' 109.5 . . ? H2B' N2' H2C' 109.5 . . ? Co' N3' H3A' 109.5 . . ? Co' N3' H3B' 109.5 . . ? H3A' N3' H3B' 109.5 . . ? Co' N3' H3C' 109.5 . . ? H3A' N3' H3C' 109.5 . . ? H3B' N3' H3C' 109.5 . . ? Co' N4' H4A' 109.5 . . ? Co' N4' H4B' 109.5 . . ? H4A' N4' H4B' 109.5 . . ? Co' N4' H4C' 109.5 . . ? H4A' N4' H4C' 109.5 . . ? H4B' N4' H4C' 109.5 . . ? Co' N5' H5A' 109.5 . . ? Co' N5' H5B' 109.5 . . ? H5A' N5' H5B' 109.5 . . ? Co' N5' H6C' 109.5 . . ? H5A' N5' H6C' 109.5 . . ? H5B' N5' H6C' 109.5 . . ? O12B Cl1 O13B 110.7(9) . . ? O12A Cl1 O14A 110.0(9) . . ? O12A Cl1 O13A 108.6(9) . . ? O12B Cl1 O14B 106.9(9) . . ? O13B Cl1 O14B 110.4(9) . . ? O12A Cl1 O11 113.0(7) . . ? O12B Cl1 O11 112.2(9) . . ? O13B Cl1 O11 108.7(6) . . ? O14A Cl1 O11 109.1(7) . . ? O13A Cl1 O11 108.7(8) . . ? O14B Cl1 O11 107.8(6) . . ? O21 Cl2 O22 111.2(3) . . ? O21 Cl2 O23 110.8(4) . . ? O22 Cl2 O23 109.9(3) . . ? O21 Cl2 O24 108.3(4) . . ? O22 Cl2 O24 109.2(3) . . ? O23 Cl2 O24 107.4(4) . . ? O33B Cl3 O31B 118.3(12) . . ? O33A Cl3 O32A 110.7(5) . . ? O33A Cl3 O34A 109.3(6) . . ? O32A Cl3 O34A 109.4(6) . . ? O33A Cl3 O31A 112.8(6) . . ? O32A Cl3 O31A 108.1(5) . . ? O34A Cl3 O31A 106.5(5) . . ? O33B Cl3 O32B 110.5(13) . . ? O31B Cl3 O32B 105.3(12) . . ? O33B Cl3 O34B 107.8(12) . . ? O31B Cl3 O34B 107.5(11) . . ? O32B Cl3 O34B 106.8(12) . . ? O44B Cl4 O42B 116.1(16) . . ? O44B Cl4 O41B 113.5(16) . . ? O42B Cl4 O41B 112.3(16) . . ? O41A Cl4 O44A 113.8(5) . . ? O41A Cl4 O42A 111.5(4) . . ? O44A Cl4 O42A 111.7(5) . . ? O41A Cl4 O43A 108.6(5) . . ? O44A Cl4 O43A 105.1(5) . . ? O42A Cl4 O43A 105.5(5) . . ? O44B Cl4 O43B 106.6(15) . . ? O42B Cl4 O43B 104.0(14) . . ? O41B Cl4 O43B 102.8(14) . . ? O51B Cl5 O52B 114.7(16) . . ? O51B Cl5 O54B 113.9(16) . . ? O52B Cl5 O54B 111.5(15) . . ? O53A Cl5 O52A 114.6(4) . . ? O53A Cl5 O51A 110.5(4) . . ? O52A Cl5 O51A 109.9(4) . . ? O53A Cl5 O54A 105.9(4) . . ? O52A Cl5 O54A 104.9(4) . . ? O51A Cl5 O54A 110.8(5) . . ? O51B Cl5 O53B 106.8(15) . . ? O52B Cl5 O53B 103.5(14) . . ? O54B Cl5 O53B 105.3(14) . . ? O63A Cl6A O61 127.2(11) . . ? O63A Cl6A O62A 109.2(12) . . ? O61 Cl6A O62A 109.9(10) . . ? O63A Cl6A O64A 92.6(10) . . ? O61 Cl6A O64A 102.7(10) . . ? O62A Cl6A O64A 113.6(12) . . ? O64B Cl6B O61 115.3(7) . . ? O64B Cl6B O62B 101.7(8) . . ? O61 Cl6B O62B 108.1(6) . . ? O64B Cl6B O63B 124.6(8) . . ? O61 Cl6B O63B 107.8(7) . . ? O62B Cl6B O63B 95.9(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 N5 Co N1 C2 -3.5(5) . . . . ? N10 Co N1 C2 178.2(5) . . . . ? N3 Co N1 C2 86.5(5) . . . . ? N2 Co N1 C2 167(3) . . . . ? N4 Co N1 C2 -93.9(5) . . . . ? N5 Co N1 C4B 177.4(3) . . . . ? N10 Co N1 C4B -0.9(3) . . . . ? N3 Co N1 C4B -92.6(4) . . . . ? N2 Co N1 C4B -12(3) . . . . ? N4 Co N1 C4B 87.0(3) . . . . ? C4B N1 C2 C3 -1.4(9) . . . . ? Co N1 C2 C3 179.6(5) . . . . ? N1 C2 C3 C4 1.0(11) . . . . ? C2 C3 C4 C4A -0.6(13) . . . . ? C3 C4 C4A C4B 0.8(12) . . . . ? C3 C4 C4A C5 -179.4(8) . . . . ? C2 N1 C4B C6B -178.8(5) . . . . ? Co N1 C4B C6B 0.4(6) . . . . ? C2 N1 C4B C4A 1.6(8) . . . . ? Co N1 C4B C4A -179.2(5) . . . . ? C4 C4A C4B N1 -1.3(9) . . . . ? C5 C4A C4B N1 178.9(6) . . . . ? C4 C4A C4B C6B 179.2(6) . . . . ? C5 C4A C4B C6B -0.7(9) . . . . ? C4 C4A C5 C6 -179.6(9) . . . . ? C4B C4A C5 C6 0.3(12) . . . . ? C4A C5 C6 C6A -0.9(14) . . . . ? C5 C6 C6A C7 -179.4(8) . . . . ? C5 C6 C6A C6B 1.8(12) . . . . ? N1 C4B C6B N10 0.7(7) . . . . ? C4A C4B C6B N10 -179.7(5) . . . . ? N1 C4B C6B C6A -177.8(5) . . . . ? C4A C4B C6B C6A 1.8(8) . . . . ? C7 C6A C6B N10 0.4(8) . . . . ? C6 C6A C6B N10 179.3(5) . . . . ? C7 C6A C6B C4B 178.8(5) . . . . ? C6 C6A C6B C4B -2.3(8) . . . . ? C6B C6A C7 C8 -0.7(9) . . . . ? C6 C6A C7 C8 -179.5(7) . . . . ? C6A C7 C8 C9 1.0(9) . . . . ? C7 C8 C9 N10 -0.9(9) . . . . ? C8 C9 N10 C6B 0.5(7) . . . . ? C8 C9 N10 Co -176.3(4) . . . . ? C4B C6B N10 C9 -178.8(4) . . . . ? C6A C6B N10 C9 -0.3(7) . . . . ? C4B C6B N10 Co -1.4(5) . . . . ? C6A C6B N10 Co 177.1(4) . . . . ? N5 Co N10 C9 151(3) . . . . ? N1 Co N10 C9 178.3(4) . . . . ? N3 Co N10 C9 -92.0(4) . . . . ? N2 Co N10 C9 -2.3(4) . . . . ? N4 Co N10 C9 87.7(4) . . . . ? N5 Co N10 C6B -26(3) . . . . ? N1 Co N10 C6B 1.3(3) . . . . ? N3 Co N10 C6B 90.9(3) . . . . ? N2 Co N10 C6B -179.4(3) . . . . ? N4 Co N10 C6B -89.3(3) . . . . ? N3' Co' N1' C2' 85.0(4) . . . . ? N10' Co' N1' C2' 175.8(4) . . . . ? N5' Co' N1' C2' -5.7(4) . . . . ? N2' Co' N1' C2' -95.0(4) . . . . ? N4' Co' N1' C2' 150(3) . . . . ? N3' Co' N1' C4B' -89.1(3) . . . . ? N10' Co' N1' C4B' 1.8(3) . . . . ? N5' Co' N1' C4B' -179.8(3) . . . . ? N2' Co' N1' C4B' 91.0(3) . . . . ? N4' Co' N1' C4B' -24(3) . . . . ? C4B' N1' C2' C3' 1.4(7) . . . . ? Co' N1' C2' C3' -172.4(4) . . . . ? N1' C2' C3' C4' -2.5(9) . . . . ? C2' C3' C4' C4A' 0.9(9) . . . . ? C3' C4' C4A' C4B' 1.5(8) . . . . ? C3' C4' C4A' C5' -179.6(6) . . . . ? C2' N1' C4B' C4A' 1.2(7) . . . . ? Co' N1' C4B' C4A' 176.0(4) . . . . ? C2' N1' C4B' C6B' -177.7(4) . . . . ? Co' N1' C4B' C6B' -2.9(5) . . . . ? C4' C4A' C4B' N1' -2.7(8) . . . . ? C5' C4A' C4B' N1' 178.3(5) . . . . ? C4' C4A' C4B' C6B' 176.2(5) . . . . ? C5' C4A' C4B' C6B' -2.8(8) . . . . ? C4' C4A' C5' C6' -177.6(7) . . . . ? C4B' C4A' C5' C6' 1.3(10) . . . . ? C4A' C5' C6' C6A' 0.2(11) . . . . ? C5' C6' C6A' C6B' -0.3(10) . . . . ? C5' C6' C6A' C7' 178.9(7) . . . . ? C7' C6A' C6B' N10' -1.4(8) . . . . ? C6' C6A' C6B' N10' 177.8(5) . . . . ? C7' C6A' C6B' C4B' 179.5(5) . . . . ? C6' C6A' C6B' C4B' -1.3(8) . . . . ? N1' C4B' C6B' N10' 2.7(6) . . . . ? C4A' C4B' C6B' N10' -176.3(4) . . . . ? N1' C4B' C6B' C6A' -178.2(5) . . . . ? C4A' C4B' C6B' C6A' 2.9(7) . . . . ? C6B' C6A' C7' C8' 0.2(10) . . . . ? C6' C6A' C7' C8' -178.9(7) . . . . ? C6A' C7' C8' C9' 1.6(11) . . . . ? C7' C8' C9' N10' -2.5(10) . . . . ? C8' C9' N10' C6B' 1.3(8) . . . . ? C8' C9' N10' Co' -177.7(5) . . . . ? C6A' C6B' N10' C9' 0.7(7) . . . . ? C4B' C6B' N10' C9' 179.8(5) . . . . ? C6A' C6B' N10' Co' 179.9(4) . . . . ? C4B' C6B' N10' Co' -1.1(5) . . . . ? N3' Co' N10' C9' -92.7(5) . . . . ? N5' Co' N10' C9' 156(2) . . . . ? N2' Co' N10' C9' 87.1(5) . . . . ? N1' Co' N10' C9' 178.6(5) . . . . ? N4' Co' N10' C9' -2.7(5) . . . . ? N3' Co' N10' C6B' 88.3(3) . . . . ? N5' Co' N10' C6B' -23(3) . . . . ? N2' Co' N10' C6B' -91.9(3) . . . . ? N1' Co' N10' C6B' -0.4(3) . . . . ? N4' Co' N10' C6B' 178.3(3) . . . . ? Cl6B O61 Cl6A O63A 66.3(17) . . . . ? Cl6B O61 Cl6A O62A -69.2(16) . . . . ? Cl6B O61 Cl6A O64A 169.6(18) . . . . ? Cl6A O61 Cl6B O64B -97.8(15) . . . . ? Cl6A O61 Cl6B O62B 149.2(17) . . . . ? Cl6A O61 Cl6B O63B 46.5(14) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.363 _refine_diff_density_min -0.902 _refine_diff_density_rms 0.104