Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'P. Bernhardt' 'Nathan Kilah' 'Andrew P. Meacham' 'Paul Meredith' 'Robert Vogel' _publ_contact_author_name 'Dr P Bernhardt' _publ_contact_author_address ; Department of Chemistry University of Queensland Brisbane 4072 AUSTRALIA ; _publ_contact_author_email P.BERNHARDT@UQ.EDU.AU _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Immobilisation of Electroactive Macrocyclic Complexes within Titania Films ; _publ_requested_category FM # CIF produced by WinGX routine CIF_UPDATE # Created on 2005-04-06 at 11:03:45 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.1 # Request file : c:\wingx\files\archive.dat # CIF files read : 1975nk2 dreduc struct # compound [Co(HL10)(CN)](ClO4)2.H2O data_1975nk2 _database_code_depnum_ccdc_archive 'CCDC 270349' _audit_creation_date 2005-04-06T11:03:45-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C21 H36 Co1 N7 O2, 2(Cl O4), H2 O' _chemical_formula_sum 'C21 H38 Cl2 Co N7 O11' _chemical_formula_weight 694.41 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.366(1) _cell_length_b 13.012(2) _cell_length_c 13.069(1) _cell_angle_alpha 106.045(9) _cell_angle_beta 105.90(1) _cell_angle_gamma 93.07(1) _cell_volume 1457.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.626 _cell_measurement_theta_max 14.618 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.841 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_ub_11 -0.19516E-1 _diffrn_orient_matrix_ub_12 -0.76359E-1 _diffrn_orient_matrix_ub_13 -0.133E-3 _diffrn_orient_matrix_ub_21 0.07991 _diffrn_orient_matrix_ub_22 -0.19569E-1 _diffrn_orient_matrix_ub_23 -0.36416E-1 _diffrn_orient_matrix_ub_31 0.76193E-1 _diffrn_orient_matrix_ub_32 0.17578E-1 _diffrn_orient_matrix_ub_33 0.75126E-1 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius TurboCAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 17 _diffrn_standards_decay_corr_max 1.356 _diffrn_standards_decay_corr_min 0.894 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 -8 2 5 0 -5 2 2 6 _diffrn_reflns_number 5460 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_unetI/netI 0.0315 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 5119 _reflns_number_gt 3890 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0784P)^2^+0.9285P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5119 _refine_ls_number_parameters 393 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.1258 _refine_ls_wR_factor_gt 0.1134 _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_restrained_S_all 1.02 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.426 _refine_diff_density_min -1.007 _refine_diff_density_rms 0.075 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.21084(4) 0.22482(3) 0.15234(3) 0.02520(14) Uani 1 1 d . . . C1 C 0.2114(4) 0.2547(3) -0.0535(3) 0.0382(8) Uani 1 1 d . . . H1B H 0.1301 0.2418 -0.1221 0.046 Uiso 1 1 calc R . . H1C H 0.3054 0.2582 -0.0711 0.046 Uiso 1 1 calc R . . C2 C 0.2049(4) 0.3608(3) 0.0291(3) 0.0329(7) Uani 1 1 d . . . C3 C 0.0532(4) 0.3675(3) 0.0519(3) 0.0353(7) Uani 1 1 d . . . H3B H 0.0527 0.4389 0.1002 0.042 Uiso 1 1 calc R . . H3C H -0.026 0.3552 -0.0178 0.042 Uiso 1 1 calc R . . C4 C -0.0267(4) 0.3248(3) 0.2058(3) 0.0409(8) Uani 1 1 d . . . H4B H -0.0821 0.2659 0.2171 0.049 Uiso 1 1 calc R . . H4C H -0.0924 0.3786 0.1951 0.049 Uiso 1 1 calc R . . C5 C 0.1094(4) 0.3741(3) 0.3059(3) 0.0358(8) Uani 1 1 d . . . H5C H 0.1558 0.44 0.3003 0.043 Uiso 1 1 calc R . . H5D H 0.0808 0.3914 0.374 0.043 Uiso 1 1 calc R . . C6 C 0.3639(3) 0.3417(2) 0.3909(3) 0.0306(7) Uani 1 1 d . . . H6B H 0.3495 0.3684 0.4639 0.037 Uiso 1 1 calc R . . H6C H 0.4025 0.4031 0.3731 0.037 Uiso 1 1 calc R . . C7 C 0.4807(3) 0.2641(2) 0.3969(3) 0.0304(7) Uani 1 1 d . . . C8 C 0.5231(3) 0.2305(3) 0.2895(3) 0.0328(7) Uani 1 1 d . . . H8A H 0.5585 0.2949 0.2751 0.039 Uiso 1 1 calc R . . H8B H 0.6057 0.1887 0.3001 0.039 Uiso 1 1 calc R . . C9 C 0.4512(4) 0.1385(3) 0.0889(3) 0.0368(8) Uani 1 1 d . . . H9A H 0.5216 0.0868 0.0937 0.044 Uiso 1 1 calc R . . H9B H 0.5007 0.2029 0.0827 0.044 Uiso 1 1 calc R . . C10 C 0.3146(4) 0.0907(3) -0.0116(3) 0.0406(8) Uani 1 1 d . . . H10A H 0.3412 0.0832 -0.0797 0.049 Uiso 1 1 calc R . . H10B H 0.276 0.0198 -0.0122 0.049 Uiso 1 1 calc R . . C11 C 0.2530(5) 0.4568(3) -0.0036(3) 0.0475(9) Uani 1 1 d . . . H11A H 0.2472 0.5223 0.0505 0.071 Uiso 1 1 calc R . . H11B H 0.188 0.4537 -0.0757 0.071 Uiso 1 1 calc R . . H11C H 0.3543 0.4555 -0.0063 0.071 Uiso 1 1 calc R . . C12 C 0.6234(4) 0.3264(3) 0.4910(3) 0.0432(9) Uani 1 1 d . . . H12A H 0.6997 0.2801 0.4973 0.065 Uiso 1 1 calc R . . H12B H 0.6005 0.3496 0.5604 0.065 Uiso 1 1 calc R . . H12C H 0.6588 0.3884 0.4738 0.065 Uiso 1 1 calc R . . C13 C 0.1002(4) 0.0974(3) 0.1494(3) 0.0320(7) Uani 1 1 d . . . C14 C 0.3915(4) 0.1737(3) 0.5189(3) 0.0428(8) Uani 1 1 d . . . H14A H 0.3391 0.2352 0.538 0.051 Uiso 1 1 calc R . . H14B H 0.4865 0.186 0.5769 0.051 Uiso 1 1 calc R . . C15 C 0.2995(4) 0.0730(3) 0.5138(3) 0.0354(7) Uani 1 1 d . . . C16 C 0.2707(4) 0.0634(3) 0.6098(3) 0.0434(9) Uani 1 1 d . . . H16 H 0.3122 0.1181 0.6769 0.052 Uiso 1 1 calc R . . C17 C 0.1819(4) -0.0255(3) 0.6077(3) 0.0429(8) Uani 1 1 d . . . H17 H 0.1619 -0.0296 0.6724 0.051 Uiso 1 1 calc R . . C18 C 0.2381(5) -0.0096(3) 0.4154(3) 0.0460(9) Uani 1 1 d . . . H18 H 0.2556 -0.0047 0.3502 0.055 Uiso 1 1 calc R . . C19 C 0.1506(4) -0.0995(3) 0.4133(3) 0.0472(9) Uani 1 1 d . . . H19 H 0.11 -0.1547 0.3464 0.057 Uiso 1 1 calc R . . C20 C 0.1226(4) -0.1086(3) 0.5089(3) 0.0372(8) Uani 1 1 d . . . C21 C 0.0268(4) -0.2041(3) 0.5062(4) 0.0457(9) Uani 1 1 d . . . O1 O -0.0143(4) -0.2143(2) 0.5828(3) 0.0671(9) Uani 1 1 d . . . O2 O -0.0092(4) -0.2812(3) 0.4090(3) 0.0686(9) Uani 1 1 d . . . H21 H -0.0698 -0.3293 0.4088 0.103 Uiso 1 1 calc R . . N1 N 0.1988(3) 0.1638(2) -0.0050(2) 0.0335(6) Uani 1 1 d . . . H1A H 0.1071 0.1237 -0.0416 0.04 Uiso 1 1 calc R . . N2 N 0.0259(3) 0.2843(2) 0.1063(2) 0.0329(6) Uani 1 1 d . . . H2A H -0.0443 0.23 0.055 0.04 Uiso 1 1 calc R . . N3 N 0.2164(3) 0.2928(2) 0.3073(2) 0.0270(5) Uani 1 1 d . . . H3A H 0.1782 0.2407 0.3305 0.032 Uiso 1 1 calc R . . N4 N 0.3996(3) 0.1658(2) 0.1900(2) 0.0289(6) Uani 1 1 d . . . H4A H 0.377 0.1023 0.2023 0.035 Uiso 1 1 calc R . . N5 N 0.3074(3) 0.3571(2) 0.1382(2) 0.0291(6) Uani 1 1 d . . . H5A H 0.3086 0.4158 0.1946 0.035 Uiso 1 1 calc R . . H5B H 0.4015 0.3509 0.1351 0.035 Uiso 1 1 calc R . . N6 N 0.4192(3) 0.1651(2) 0.4122(2) 0.0355(6) Uani 1 1 d . . . H6A H 0.477 0.1156 0.4014 0.043 Uiso 1 1 d R . . N7 N 0.0304(4) 0.0211(3) 0.1452(3) 0.0502(8) Uani 1 1 d . . . O3 O 0.1446(5) 0.6137(3) 0.2338(3) 0.0939(13) Uani 1 1 d . . . H3D H 0.221 0.6319 0.228 0.141 Uiso 1 1 d R . . H3E H 0.1228 0.6425 0.3038 0.141 Uiso 1 1 d R . . Cl1 Cl 0.66285(10) 0.53364(7) 0.27811(7) 0.0441(2) Uani 1 1 d . . . O1A O 0.5350(4) 0.5346(3) 0.3177(3) 0.0827(12) Uani 1 1 d . . . O1B O 0.6409(3) 0.4375(2) 0.1867(2) 0.0548(7) Uani 1 1 d . . . O1C O 0.7928(4) 0.5346(3) 0.3676(3) 0.0885(12) Uani 1 1 d . . . O1D O 0.6834(4) 0.6264(2) 0.2452(3) 0.0696(9) Uani 1 1 d . . . Cl2 Cl 0.65834(10) 0.16847(7) -0.12556(8) 0.0462(2) Uani 1 1 d . . . O2A O 0.5830(4) 0.0637(2) -0.1901(3) 0.0712(9) Uani 1 1 d . A . O2B O 0.7676(7) 0.2028(4) -0.1658(4) 0.096(2) Uani 0.864(7) 1 d P A 1 O2C O 0.7271(4) 0.1630(4) -0.0140(3) 0.0733(14) Uani 0.864(7) 1 d P A 1 O2D O 0.5491(5) 0.2396(3) -0.1178(5) 0.0962(19) Uani 0.864(7) 1 d P A 1 O2E O 0.819(3) 0.158(2) -0.125(2) 0.064(7) Uiso 0.136(7) 1 d P A 2 O2F O 0.671(4) 0.240(3) -0.020(3) 0.086(10) Uiso 0.136(7) 1 d P A 2 O2G O 0.620(3) 0.2323(17) -0.2066(18) 0.057(7) Uiso 0.136(7) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0187(2) 0.0265(2) 0.0275(2) 0.00708(16) 0.00421(16) -0.00073(15) C1 0.0412(19) 0.0442(19) 0.0294(17) 0.0152(15) 0.0075(15) 0.0024(15) C2 0.0303(17) 0.0381(18) 0.0304(17) 0.0135(14) 0.0066(14) 0.0032(14) C3 0.0273(17) 0.0413(18) 0.0360(18) 0.0172(15) 0.0018(14) 0.0061(14) C4 0.0240(17) 0.056(2) 0.047(2) 0.0198(17) 0.0116(15) 0.0119(15) C5 0.0310(18) 0.0426(19) 0.0367(18) 0.0124(15) 0.0127(15) 0.0149(15) C6 0.0271(16) 0.0269(15) 0.0302(17) 0.0042(13) 0.0017(13) 0.0001(12) C7 0.0243(16) 0.0307(16) 0.0319(17) 0.0099(13) 0.0016(13) 0.0010(13) C8 0.0226(16) 0.0387(18) 0.0364(18) 0.0134(14) 0.0058(13) 0.0035(13) C9 0.0386(19) 0.0381(18) 0.0385(19) 0.0086(15) 0.0206(16) 0.0130(15) C10 0.050(2) 0.0321(18) 0.0374(19) 0.0031(15) 0.0175(17) 0.0059(16) C11 0.052(2) 0.051(2) 0.047(2) 0.0250(18) 0.0167(19) 0.0075(18) C12 0.0284(18) 0.048(2) 0.042(2) 0.0113(17) -0.0036(15) -0.0030(15) C13 0.0255(16) 0.0347(18) 0.0278(16) 0.0052(13) 0.0013(13) -0.0034(14) C14 0.049(2) 0.043(2) 0.0321(18) 0.0109(15) 0.0074(16) -0.0049(16) C15 0.0328(18) 0.0367(18) 0.0351(18) 0.0144(15) 0.0044(14) 0.0027(14) C16 0.043(2) 0.049(2) 0.0338(19) 0.0139(16) 0.0040(16) -0.0003(17) C17 0.044(2) 0.053(2) 0.0351(19) 0.0210(17) 0.0110(16) 0.0025(17) C18 0.060(2) 0.043(2) 0.0360(19) 0.0131(16) 0.0167(18) -0.0050(18) C19 0.050(2) 0.045(2) 0.040(2) 0.0089(17) 0.0098(17) -0.0062(17) C20 0.0292(17) 0.0434(19) 0.044(2) 0.0206(16) 0.0123(15) 0.0063(14) C21 0.0283(18) 0.049(2) 0.063(3) 0.023(2) 0.0127(18) 0.0048(16) O1 0.075(2) 0.0645(19) 0.077(2) 0.0311(17) 0.0391(18) -0.0030(16) O2 0.057(2) 0.064(2) 0.070(2) 0.0076(16) 0.0160(16) -0.0317(15) N1 0.0310(14) 0.0322(14) 0.0303(14) 0.0036(11) 0.0055(12) -0.0031(11) N2 0.0209(13) 0.0418(15) 0.0322(15) 0.0113(12) 0.0026(11) -0.0013(11) N3 0.0217(13) 0.0311(14) 0.0284(13) 0.0105(11) 0.0066(11) 0.0019(10) N4 0.0261(13) 0.0285(13) 0.0311(14) 0.0084(11) 0.0077(11) 0.0027(10) N5 0.0212(13) 0.0337(14) 0.0297(14) 0.0092(11) 0.0045(11) 0.0004(11) N6 0.0374(16) 0.0338(15) 0.0373(16) 0.0142(12) 0.0108(13) 0.0054(12) N7 0.050(2) 0.0456(18) 0.0458(19) 0.0155(15) 0.0033(15) -0.0166(15) O3 0.151(4) 0.060(2) 0.055(2) 0.0066(16) 0.025(2) -0.019(2) Cl1 0.0373(5) 0.0466(5) 0.0421(5) 0.0079(4) 0.0108(4) -0.0113(4) O1A 0.065(2) 0.087(2) 0.076(2) -0.0205(18) 0.0425(19) -0.0289(18) O1B 0.0468(16) 0.0479(15) 0.0635(18) 0.0027(13) 0.0231(14) -0.0045(12) O1C 0.067(2) 0.091(3) 0.082(2) 0.042(2) -0.0251(18) -0.0279(19) O1D 0.088(2) 0.0502(17) 0.071(2) 0.0238(15) 0.0207(18) 0.0013(16) Cl2 0.0429(5) 0.0418(5) 0.0476(5) 0.0133(4) 0.0045(4) 0.0024(4) O2A 0.064(2) 0.0450(17) 0.084(2) 0.0179(16) -0.0069(17) -0.0073(14) O2B 0.121(5) 0.080(3) 0.100(4) 0.021(3) 0.065(3) -0.023(3) O2C 0.058(2) 0.099(3) 0.051(2) 0.028(2) -0.0023(17) -0.015(2) O2D 0.081(3) 0.064(3) 0.142(5) 0.028(3) 0.029(3) 0.035(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C13 1.893(3) . ? Co1 N2 1.947(3) . ? Co1 N1 1.957(3) . ? Co1 N4 1.958(3) . ? Co1 N3 1.958(2) . ? Co1 N5 1.979(3) . ? C1 N1 1.502(4) . ? C1 C2 1.515(5) . ? C2 N5 1.500(4) . ? C2 C11 1.512(5) . ? C2 C3 1.531(5) . ? C3 N2 1.497(4) . ? C4 N2 1.487(4) . ? C4 C5 1.511(5) . ? C5 N3 1.496(4) . ? C6 N3 1.484(4) . ? C6 C7 1.529(4) . ? C7 N6 1.470(4) . ? C7 C8 1.517(5) . ? C7 C12 1.546(4) . ? C8 N4 1.485(4) . ? C9 N4 1.488(4) . ? C9 C10 1.514(5) . ? C10 N1 1.485(4) . ? C13 N7 1.139(4) . ? C14 N6 1.463(4) . ? C14 C15 1.505(5) . ? C15 C18 1.380(5) . ? C15 C16 1.390(5) . ? C16 C17 1.377(5) . ? C17 C20 1.384(5) . ? C18 C19 1.381(5) . ? C19 C20 1.379(5) . ? C20 C21 1.479(5) . ? C21 O1 1.203(5) . ? C21 O2 1.327(5) . ? Cl1 O1D 1.410(3) . ? Cl1 O1A 1.427(3) . ? Cl1 O1B 1.430(3) . ? Cl1 O1C 1.435(3) . ? Cl2 O2B 1.378(4) . ? Cl2 O2F 1.41(3) . ? Cl2 O2A 1.416(3) . ? Cl2 O2D 1.421(4) . ? Cl2 O2C 1.447(4) . ? Cl2 O2G 1.50(2) . ? Cl2 O2E 1.52(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 Co1 N2 90.51(13) . . ? C13 Co1 N1 91.19(13) . . ? N2 Co1 N1 89.04(11) . . ? C13 Co1 N4 91.35(12) . . ? N2 Co1 N4 176.34(11) . . ? N1 Co1 N4 87.76(11) . . ? C13 Co1 N3 90.52(12) . . ? N2 Co1 N3 87.90(11) . . ? N1 Co1 N3 176.51(11) . . ? N4 Co1 N3 95.24(10) . . ? C13 Co1 N5 172.94(12) . . ? N2 Co1 N5 84.23(11) . . ? N1 Co1 N5 84.03(11) . . ? N4 Co1 N5 93.65(11) . . ? N3 Co1 N5 93.99(11) . . ? N1 C1 C2 110.0(3) . . ? N5 C2 C11 112.3(3) . . ? N5 C2 C1 104.1(3) . . ? C11 C2 C1 112.0(3) . . ? N5 C2 C3 102.7(2) . . ? C11 C2 C3 111.8(3) . . ? C1 C2 C3 113.3(3) . . ? N2 C3 C2 109.6(3) . . ? N2 C4 C5 108.0(3) . . ? N3 C5 C4 107.3(3) . . ? N3 C6 C7 114.1(2) . . ? N6 C7 C8 106.9(3) . . ? N6 C7 C6 110.0(3) . . ? C8 C7 C6 111.4(3) . . ? N6 C7 C12 114.4(3) . . ? C8 C7 C12 107.2(3) . . ? C6 C7 C12 107.1(3) . . ? N4 C8 C7 114.6(3) . . ? N4 C9 C10 107.7(3) . . ? N1 C10 C9 108.5(3) . . ? N7 C13 Co1 178.1(3) . . ? N6 C14 C15 111.4(3) . . ? C18 C15 C16 118.4(3) . . ? C18 C15 C14 122.0(3) . . ? C16 C15 C14 119.6(3) . . ? C17 C16 C15 121.4(3) . . ? C16 C17 C20 119.8(3) . . ? C15 C18 C19 120.4(3) . . ? C20 C19 C18 120.9(3) . . ? C19 C20 C17 119.2(3) . . ? C19 C20 C21 120.9(3) . . ? C17 C20 C21 120.0(3) . . ? O1 C21 O2 121.8(4) . . ? O1 C21 C20 125.3(4) . . ? O2 C21 C20 112.9(3) . . ? C10 N1 C1 115.3(3) . . ? C10 N1 Co1 108.0(2) . . ? C1 N1 Co1 108.75(19) . . ? C4 N2 C3 114.7(3) . . ? C4 N2 Co1 108.0(2) . . ? C3 N2 Co1 109.02(19) . . ? C6 N3 C5 110.7(2) . . ? C6 N3 Co1 118.25(19) . . ? C5 N3 Co1 107.09(19) . . ? C8 N4 C9 110.6(2) . . ? C8 N4 Co1 118.44(19) . . ? C9 N4 Co1 107.4(2) . . ? C2 N5 Co1 100.68(18) . . ? C14 N6 C7 117.5(3) . . ? O1D Cl1 O1A 110.4(2) . . ? O1D Cl1 O1B 110.99(19) . . ? O1A Cl1 O1B 108.46(17) . . ? O1D Cl1 O1C 108.4(2) . . ? O1A Cl1 O1C 108.4(2) . . ? O1B Cl1 O1C 110.2(2) . . ? O2B Cl2 O2A 112.8(3) . . ? O2F Cl2 O2A 136.4(12) . . ? O2B Cl2 O2D 113.0(3) . . ? O2A Cl2 O2D 108.2(2) . . ? O2B Cl2 O2C 109.2(3) . . ? O2A Cl2 O2C 106.4(2) . . ? O2D Cl2 O2C 106.7(3) . . ? O2F Cl2 O2G 106.4(16) . . ? O2A Cl2 O2G 102.9(8) . . ? O2F Cl2 O2E 104.6(16) . . ? O2A Cl2 O2E 102.3(10) . . ? O2G Cl2 O2E 98.2(14) . . ? #===END # compound [CoL10(OH)](ClO4).5H2O # CIF produced by WinGX routine CIF_UPDATE # Created on 2005-04-06 at 11:59:53 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.1 # Request file : c:\wingx\files\archive.dat # CIF files read : 2000nk6 dreduc struct data_2000nk6 _database_code_depnum_ccdc_archive 'CCDC 270350' _audit_creation_date 2005-04-06T11:59:53-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C20 H36 Co N6 O3, Cl O4, 5(H2 O)' _chemical_formula_sum 'C20 H46 Cl Co N6 O12' _chemical_formula_weight 657.01 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.235(3) _cell_length_b 24.023(3) _cell_length_c 13.845(2) _cell_angle_alpha 90 _cell_angle_beta 109.01(2) _cell_angle_gamma 90 _cell_volume 2904.0(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.306 _cell_measurement_theta_max 12.768 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.751 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_ub_11 -0.29807E-1 _diffrn_orient_matrix_ub_12 -0.38147E-1 _diffrn_orient_matrix_ub_13 -0.28326E-1 _diffrn_orient_matrix_ub_21 0.99978E-1 _diffrn_orient_matrix_ub_22 -0.14878E-1 _diffrn_orient_matrix_ub_23 0.45648E-1 _diffrn_orient_matrix_ub_31 -0.47159E-1 _diffrn_orient_matrix_ub_32 -0.00742 _diffrn_orient_matrix_ub_33 0.54326E-1 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius TurboCAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 19 _diffrn_standards_decay_corr_max 1.727 _diffrn_standards_decay_corr_min 0.969 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 -13 -2 4 -5 3 -3 -3 8 _diffrn_reflns_number 5441 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_unetI/netI 0.0407 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.7 _diffrn_reflns_theta_max 24.98 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 5105 _reflns_number_gt 3606 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.1708P)^2^+2.5288P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5105 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1032 _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.2381 _refine_ls_wR_factor_gt 0.2061 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.502 _refine_diff_density_min -1.875 _refine_diff_density_rms 0.134 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 0.08045(7) 0.08907(3) 1.08476(5) 0.0203(3) Uani 1 1 d . . . C1 C 0.1672(7) 0.1109(2) 0.9106(4) 0.0323(12) Uani 1 1 d . . . H1B H 0.1267 0.0964 0.8416 0.039 Uiso 1 1 calc R . . H1C H 0.268 0.1263 0.92 0.039 Uiso 1 1 calc R . . C2 C 0.0618(6) 0.1559(2) 0.9270(4) 0.0275(12) Uani 1 1 d . . . C3 C -0.1037(6) 0.1370(2) 0.8998(4) 0.0300(12) Uani 1 1 d . . . H3B H -0.1681 0.1682 0.9039 0.036 Uiso 1 1 calc R . . H3C H -0.1394 0.1227 0.8305 0.036 Uiso 1 1 calc R . . C4 C -0.2379(6) 0.1029(2) 1.0178(4) 0.0311(12) Uani 1 1 d . . . H4B H -0.2706 0.0679 1.0388 0.037 Uiso 1 1 calc R . . H4C H -0.3254 0.1201 0.9675 0.037 Uiso 1 1 calc R . . C5 C -0.1758(6) 0.1410(2) 1.1092(4) 0.0306(12) Uani 1 1 d . . . H5C H -0.1563 0.1779 1.0877 0.037 Uiso 1 1 calc R . . H5D H -0.2479 0.1441 1.1465 0.037 Uiso 1 1 calc R . . C6 C 0.0537(6) 0.1483(2) 1.2649(4) 0.0288(12) Uani 1 1 d . . . H6B H -0.0133 0.1564 1.3044 0.035 Uiso 1 1 calc R . . H6C H 0.0849 0.1833 1.243 0.035 Uiso 1 1 calc R . . C7 C 0.1949(6) 0.1170(2) 1.3316(4) 0.0275(12) Uani 1 1 d . . . C8 C 0.3211(6) 0.1169(2) 1.2812(4) 0.0289(12) Uani 1 1 d . . . H8A H 0.3375 0.1547 1.2624 0.035 Uiso 1 1 calc R . . H8B H 0.416 0.1038 1.3302 0.035 Uiso 1 1 calc R . . C9 C 0.3998(6) 0.0824(2) 1.1363(4) 0.0314(12) Uani 1 1 d . . . H9A H 0.4962 0.0675 1.1805 0.038 Uiso 1 1 calc R . . H9B H 0.4167 0.1202 1.1178 0.038 Uiso 1 1 calc R . . C10 C 0.3372(6) 0.0468(2) 1.0416(4) 0.0304(12) Uani 1 1 d . . . H10A H 0.4001 0.051 0.998 0.036 Uiso 1 1 calc R . . H10B H 0.338 0.0079 1.0606 0.036 Uiso 1 1 calc R . . C11 C 0.0712(8) 0.2087(2) 0.8685(5) 0.0396(14) Uani 1 1 d . . . H11A H 0.1762 0.2203 0.886 0.059 Uiso 1 1 calc R . . H11B H 0.0126 0.2377 0.8861 0.059 Uiso 1 1 calc R . . H11C H 0.0308 0.2016 0.7964 0.059 Uiso 1 1 calc R . . C12 C 0.2574(7) 0.1489(2) 1.4335(4) 0.0345(13) Uani 1 1 d . . . H12A H 0.1809 0.1499 1.4666 0.052 Uiso 1 1 calc R . . H12B H 0.283 0.1863 1.4203 0.052 Uiso 1 1 calc R . . H12C H 0.3474 0.1305 1.4769 0.052 Uiso 1 1 calc R . . C13 C 0.2536(7) 0.0242(2) 1.4155(5) 0.0399(15) Uani 1 1 d . . . H13A H 0.2735 0.0399 1.4832 0.048 Uiso 1 1 calc R . . H13B H 0.3493 0.0245 1.4007 0.048 Uiso 1 1 calc R . . C14 C 0.2013(7) -0.0357(2) 1.4165(4) 0.0384(14) Uani 1 1 d . . . C15 C 0.3114(7) -0.0754(2) 1.4522(5) 0.0444(16) Uani 1 1 d . . . H15A H 0.4141 -0.0652 1.4713 0.053 Uiso 1 1 calc R . . C16 C 0.0480(8) -0.0524(3) 1.3858(5) 0.0480(17) Uani 1 1 d . . . H16A H -0.0291 -0.0261 1.3611 0.058 Uiso 1 1 calc R . . C17 C 0.2737(8) -0.1304(3) 1.4608(5) 0.0465(16) Uani 1 1 d . . . H17A H 0.351 -0.1566 1.4858 0.056 Uiso 1 1 calc R . . C18 C 0.0098(7) -0.1077(2) 1.3920(5) 0.0412(15) Uani 1 1 d . . . H18A H -0.0925 -0.1185 1.3685 0.049 Uiso 1 1 calc R . . C19 C 0.1219(6) -0.1470(2) 1.4325(4) 0.0306(12) Uani 1 1 d . . . C20 C 0.0853(7) -0.2070(2) 1.4451(5) 0.0367(14) Uani 1 1 d . . . N1 N 0.1782(5) 0.06503(17) 0.9865(3) 0.0244(9) Uani 1 1 d . . . H1A H 0.1255 0.0352 0.952 0.029 Uiso 1 1 calc R . . N2 N -0.1130(5) 0.09283(17) 0.9726(3) 0.0286(10) Uani 1 1 d . . . H2A H -0.1299 0.0595 0.9394 0.034 Uiso 1 1 calc R . . N3 N -0.0305(5) 0.11462(17) 1.1739(3) 0.0246(9) Uani 1 1 d . . . H3A H -0.0596 0.0831 1.1992 0.03 Uiso 1 1 calc R . . N4 N 0.2813(5) 0.08125(17) 1.1892(3) 0.0299(11) Uani 1 1 d . . . H4A H 0.2834 0.0458 1.213 0.036 Uiso 1 1 calc R . . N5 N 0.1147(5) 0.16427(16) 1.0403(3) 0.0251(10) Uani 1 1 d . . . H5A H 0.0579 0.1899 1.0589 0.03 Uiso 1 1 calc R . . H5B H 0.2141 0.174 1.0645 0.03 Uiso 1 1 calc R . . N6 N 0.1448(5) 0.05943(17) 1.3421(3) 0.0306(10) Uani 1 1 d . . . H6A H 0.059 0.0612 1.3594 0.037 Uiso 1 1 d R . . O1 O 0.0399(4) 0.01366(13) 1.1115(3) 0.0249(8) Uani 1 1 d . . . H1 H 0.0527 0.0079 1.1755 0.03 Uiso 1 1 d R . . O2 O 0.1839(5) -0.23546(16) 1.5118(4) 0.0473(12) Uani 1 1 d . . . O3 O -0.0413(5) -0.22671(17) 1.3912(3) 0.0453(11) Uani 1 1 d . . . Cl1 Cl 0.5295(2) -0.05492(7) 1.26390(12) 0.0528(5) Uani 1 1 d . . . O1A O 0.3667(6) -0.0495(3) 1.2188(5) 0.0802(19) Uani 1 1 d . . . O1B O 0.5662(12) -0.1036(3) 1.3218(6) 0.129(3) Uani 1 1 d . . . O1C O 0.5737(8) -0.0090(3) 1.3332(5) 0.091(2) Uani 1 1 d . . . O1D O 0.5993(9) -0.0501(4) 1.1886(6) 0.116(3) Uani 1 1 d . . . O4 O 0.6641(6) -0.2067(2) 1.2708(4) 0.0639(14) Uani 1 1 d . . . H4G H 0.6386 -0.1739 1.2685 0.096 Uiso 1 1 d R . . H4H H 0.7438 -0.2092 1.2571 0.096 Uiso 1 1 d R . . O5 O 0.5564(6) -0.2830(2) 1.3797(4) 0.0631(14) Uani 1 1 d . . . H5G H 0.5756 -0.2526 1.3597 0.095 Uiso 1 1 d R . . H5H H 0.5506 -0.2793 1.4372 0.095 Uiso 1 1 d R . . O6 O 0.3134(7) -0.3228(2) 1.1959(4) 0.0789(18) Uani 1 1 d . . . H6G H 0.2914 -0.3055 1.1418 0.118 Uiso 1 1 d R . . H6H H 0.3755 -0.3044 1.2408 0.118 Uiso 1 1 d R . . O7 O 0.4829(7) -0.2744(3) 1.5553(5) 0.0778(17) Uani 1 1 d . . . H7G H 0.4057 -0.2553 1.5455 0.117 Uiso 1 1 d R . . H7H H 0.5342 -0.2723 1.616 0.117 Uiso 1 1 d R . . O8 O 0.2019(6) -0.4302(2) 1.1937(5) 0.0708(16) Uani 1 1 d . . . H8G H 0.2458 -0.4029 1.1808 0.106 Uiso 1 1 d R . . H8H H 0.2365 -0.4586 1.1764 0.106 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0204(4) 0.0150(4) 0.0218(4) 0.0000(2) 0.0016(3) 0.0008(2) C1 0.036(3) 0.030(3) 0.030(3) 0.000(2) 0.009(2) -0.002(2) C2 0.034(3) 0.020(2) 0.026(3) 0.004(2) 0.006(2) -0.001(2) C3 0.025(3) 0.030(3) 0.029(3) 0.003(2) 0.000(2) 0.005(2) C4 0.023(3) 0.029(3) 0.034(3) -0.002(2) 0.000(2) 0.003(2) C5 0.027(3) 0.029(3) 0.033(3) 0.000(2) 0.007(2) 0.009(2) C6 0.035(3) 0.018(2) 0.030(3) -0.003(2) 0.006(2) -0.004(2) C7 0.033(3) 0.017(2) 0.026(3) -0.002(2) 0.001(2) -0.003(2) C8 0.031(3) 0.022(3) 0.027(3) -0.004(2) 0.001(2) -0.004(2) C9 0.018(3) 0.029(3) 0.042(3) -0.003(2) 0.002(2) 0.007(2) C10 0.025(3) 0.032(3) 0.034(3) -0.003(2) 0.010(2) 0.008(2) C11 0.050(4) 0.028(3) 0.040(3) 0.010(2) 0.014(3) 0.002(3) C12 0.048(4) 0.027(3) 0.024(3) -0.004(2) 0.004(2) -0.004(2) C13 0.040(3) 0.025(3) 0.042(3) 0.006(2) -0.005(3) -0.006(2) C14 0.041(3) 0.030(3) 0.036(3) 0.002(2) 0.001(3) -0.009(3) C15 0.035(3) 0.031(3) 0.060(4) 0.010(3) 0.005(3) -0.003(3) C16 0.043(4) 0.033(3) 0.057(4) 0.013(3) 0.002(3) 0.006(3) C17 0.040(4) 0.032(3) 0.062(4) 0.011(3) 0.010(3) -0.003(3) C18 0.034(3) 0.030(3) 0.051(4) 0.002(3) 0.001(3) -0.005(2) C19 0.034(3) 0.022(3) 0.033(3) 0.000(2) 0.008(2) -0.004(2) C20 0.037(3) 0.026(3) 0.044(3) 0.003(2) 0.009(3) -0.002(2) N1 0.022(2) 0.021(2) 0.027(2) -0.0025(17) 0.0036(18) 0.0001(17) N2 0.033(3) 0.020(2) 0.026(2) 0.0012(17) -0.0007(19) -0.0018(18) N3 0.022(2) 0.021(2) 0.026(2) -0.0006(17) 0.0011(18) 0.0004(17) N4 0.026(2) 0.019(2) 0.034(2) 0.0001(18) -0.0061(19) 0.0012(17) N5 0.025(2) 0.0161(19) 0.031(2) 0.0005(17) 0.0040(18) 0.0007(17) N6 0.033(2) 0.024(2) 0.029(2) 0.0016(18) 0.0019(19) -0.0054(19) O1 0.032(2) 0.0166(16) 0.0228(17) -0.0003(13) 0.0036(15) -0.0021(14) O2 0.049(3) 0.026(2) 0.057(3) 0.0090(19) 0.003(2) -0.0009(19) O3 0.043(3) 0.029(2) 0.056(3) 0.0061(19) 0.005(2) -0.0103(19) Cl1 0.0544(10) 0.0524(10) 0.0413(9) 0.0043(7) 0.0015(8) 0.0148(8) O1A 0.054(3) 0.094(5) 0.073(4) 0.015(3) -0.008(3) -0.004(3) O1B 0.203(9) 0.080(5) 0.103(6) 0.041(4) 0.047(6) 0.079(6) O1C 0.103(5) 0.099(5) 0.064(4) -0.025(3) 0.018(3) -0.039(4) O1D 0.122(6) 0.163(8) 0.087(5) 0.020(5) 0.068(5) 0.061(6) O4 0.055(3) 0.058(3) 0.075(4) 0.002(3) 0.017(3) 0.004(3) O5 0.077(4) 0.038(3) 0.075(3) -0.002(2) 0.027(3) -0.002(2) O6 0.089(4) 0.079(4) 0.057(3) 0.008(3) 0.008(3) -0.027(3) O7 0.057(3) 0.104(5) 0.070(4) 0.004(3) 0.018(3) 0.015(3) O8 0.048(3) 0.060(3) 0.107(5) -0.022(3) 0.029(3) -0.002(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 1.910(3) . ? Co1 N3 1.943(4) . ? Co1 N1 1.949(4) . ? Co1 N2 1.950(4) . ? Co1 N4 1.954(4) . ? Co1 N5 1.967(4) . ? C1 N1 1.503(7) . ? C1 C2 1.521(8) . ? C2 N5 1.496(6) . ? C2 C3 1.520(7) . ? C2 C11 1.523(7) . ? C3 N2 1.485(7) . ? C4 N2 1.500(7) . ? C4 C5 1.516(7) . ? C5 N3 1.490(6) . ? C6 N3 1.486(6) . ? C6 C7 1.528(7) . ? C7 N6 1.480(7) . ? C7 C8 1.541(8) . ? C7 C12 1.544(7) . ? C8 N4 1.478(7) . ? C9 N4 1.503(8) . ? C9 C10 1.513(7) . ? C10 N1 1.483(6) . ? C13 N6 1.446(7) . ? C13 C14 1.519(7) . ? C14 C15 1.364(9) . ? C14 C16 1.398(9) . ? C15 C17 1.382(8) . ? C16 C18 1.386(9) . ? C17 C19 1.385(8) . ? C18 C19 1.378(8) . ? C19 C20 1.503(7) . ? C20 O3 1.257(7) . ? C20 O2 1.265(7) . ? Cl1 O1B 1.396(7) . ? Cl1 O1D 1.397(7) . ? Cl1 O1C 1.433(6) . ? Cl1 O1A 1.434(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 N3 89.95(17) . . ? O1 Co1 N1 91.09(17) . . ? N3 Co1 N1 175.63(16) . . ? O1 Co1 N2 90.69(16) . . ? N3 Co1 N2 87.45(19) . . ? N1 Co1 N2 88.29(19) . . ? O1 Co1 N4 87.94(16) . . ? N3 Co1 N4 97.48(19) . . ? N1 Co1 N4 86.80(19) . . ? N2 Co1 N4 174.9(2) . . ? O1 Co1 N5 173.31(16) . . ? N3 Co1 N5 94.63(18) . . ? N1 Co1 N5 83.99(18) . . ? N2 Co1 N5 84.66(17) . . ? N4 Co1 N5 96.28(18) . . ? N1 C1 C2 108.5(4) . . ? N5 C2 C3 105.0(4) . . ? N5 C2 C1 104.2(4) . . ? C3 C2 C1 113.1(4) . . ? N5 C2 C11 112.9(4) . . ? C3 C2 C11 110.1(4) . . ? C1 C2 C11 111.3(5) . . ? N2 C3 C2 108.7(4) . . ? N2 C4 C5 108.2(4) . . ? N3 C5 C4 105.5(4) . . ? N3 C6 C7 110.7(4) . . ? N6 C7 C6 106.7(4) . . ? N6 C7 C8 110.6(4) . . ? C6 C7 C8 110.4(4) . . ? N6 C7 C12 114.2(4) . . ? C6 C7 C12 107.4(4) . . ? C8 C7 C12 107.5(4) . . ? N4 C8 C7 112.2(4) . . ? N4 C9 C10 106.1(4) . . ? N1 C10 C9 108.3(4) . . ? N6 C13 C14 114.2(5) . . ? C15 C14 C16 118.1(5) . . ? C15 C14 C13 117.7(5) . . ? C16 C14 C13 124.2(5) . . ? C14 C15 C17 121.4(6) . . ? C18 C16 C14 120.7(6) . . ? C15 C17 C19 120.8(6) . . ? C19 C18 C16 120.6(6) . . ? C18 C19 C17 118.3(5) . . ? C18 C19 C20 122.4(5) . . ? C17 C19 C20 119.3(5) . . ? O3 C20 O2 122.6(5) . . ? O3 C20 C19 119.6(5) . . ? O2 C20 C19 117.8(5) . . ? C10 N1 C1 114.0(4) . . ? C10 N1 Co1 109.5(3) . . ? C1 N1 Co1 109.3(3) . . ? C3 N2 C4 112.9(4) . . ? C3 N2 Co1 109.5(3) . . ? C4 N2 Co1 107.7(3) . . ? C6 N3 C5 113.5(4) . . ? C6 N3 Co1 118.2(3) . . ? C5 N3 Co1 108.1(3) . . ? C8 N4 C9 113.2(4) . . ? C8 N4 Co1 119.4(3) . . ? C9 N4 Co1 107.7(3) . . ? C2 N5 Co1 100.0(3) . . ? C13 N6 C7 116.6(4) . . ? O1B Cl1 O1D 114.4(5) . . ? O1B Cl1 O1C 107.4(5) . . ? O1D Cl1 O1C 109.6(5) . . ? O1B Cl1 O1A 110.5(5) . . ? O1D Cl1 O1A 109.9(4) . . ? O1C Cl1 O1A 104.5(4) . . ? #===END