# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email jazubiet@syr.edu _publ_contact_author_name 'Jon Zubieta' loop_ _publ_author_name W.Ouellette K.Darling A.V.Prosvirin K.Whitenack K.Dunbar J.Zubieta ##### data_pm-3m #(Me2NH2)3[Cd12Cl3(btt)8(DMF)12]\/Y12DMF\/Y5MeOH (6\/Y12DMF\/Y5MeOH). _database_code_depnum_ccdc_archive 'CCDC 826916' #TrackingRef '- AllCIFsDT-ART-05-2011-010984.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C1.5 H0.50 N2 Cd0.25 Cl0.0625 O0.25, C1.73 H4.42 N0.563 O0.354 ; _chemical_formula_sum ; C3.23 H4.92 Cd0.25 Cl0.0625 N2.56 O0.60 ; _chemical_formula_weight 119.62 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'P m -3 m' _symmetry_space_group_name_Hall '-P 4 2 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, -z' '-y, -x, -z' 'y, -x, z' '-y, x, z' 'x, z, -y' '-x, z, y' '-x, -z, -y' 'x, -z, y' 'z, y, -x' 'z, -y, x' '-z, y, x' '-z, -y, -x' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-z, -x, -y' '-z, x, y' 'z, x, -y' 'z, -x, y' '-y, -z, -x' 'y, -z, x' '-y, z, x' 'y, z, -x' '-y, -x, z' 'y, x, z' '-y, x, -z' 'y, -x, -z' '-x, -z, y' 'x, -z, -y' 'x, z, y' '-x, z, -y' '-z, -y, x' '-z, y, -x' 'z, -y, -x' 'z, y, x' _cell_length_a 19.3273(3) _cell_length_b 19.3273(3) _cell_length_c 19.3273(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7219.61(19) _cell_formula_units_Z 48 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 346 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 28.27 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 1.29(2) _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_method flotation _exptl_crystal_F_000 2886 _exptl_absorpt_coefficient_mu 0.962 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8756 _exptl_absorpt_correction_T_max 0.9143 _exptl_absorpt_process_details 'SADABS (Bruker, 1998)' _exptl_special_details ; In this X-ray diffraction analysis, there were several residual peaks within the void from Fourier difference map. However, the highly disordered solvents within the void could not be crystallographically defined. ; _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_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_reflns_number 69660 _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.0142 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 28.05 _reflns_number_total 1789 _reflns_number_gt 1745 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'CrystalMaker (Palmer, 2006)' _computing_publication_material 'Bruker SHELXTL (Sheldrick, 2008)' _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^)+(0.0495P)^2^+11.2700P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1789 _refine_ls_number_parameters 47 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0969 _refine_ls_wR_factor_gt 0.0954 _refine_ls_goodness_of_fit_ref 1.173 _refine_ls_restrained_S_all 1.173 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 # SQUEEZE RESULTS _platon_squeeze_details ; Although there were several peaks within the void from Fourier difference map, the highly disordered solvents within the void were not crystallographically well defined. The SQUEEZE routine of the program PLATON was used in order to eliminate the contribution of disordered solvents molecules, thereby a final model based only on the ordered part of the crystal structure was obtained. The SQUEEZE routine suggested that a total potential solvent area volume of 4807 Ang^3^[66.6% of cell volume], and a void electron population of 866 per cell. Refinement after the SQUEEZE routine gave significantly improved R values. [R values before SQUEEZE] R1 = 0.173 for >2sigma(I) data R1 = 0.198 , wR2 = 0.277, GooF = S = 1.83 for all data ( 1789 data and 0 restraint / 47 parameters) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.024 -0.014 0.215 4807 866 ' ' _platon_squeeze_details ? ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.855032(17) 1.0000 0.5000 0.01451(13) Uani 1 4 d S . . Cl1 Cl 1.0000 1.0000 0.5000 0.0169(4) Uani 1 16 d S . . O1 O 0.7369(3) 1.0000 0.5000 0.093(3) Uani 1 4 d S . . N1 N 0.86563(11) 0.91338(11) 0.58204(11) 0.0244(5) Uani 1 1 d . . . N2 N 0.82272(12) 0.90386(12) 0.63497(12) 0.0316(5) Uani 1 1 d . . . C1 C 0.84729(16) 0.84729(16) 0.6659(2) 0.0315(9) Uani 1 2 d S . . C2 C 0.81647(18) 0.81647(18) 0.7280(2) 0.0386(11) Uani 1 2 d S . . C3 C 0.75743(18) 0.8455(2) 0.75743(18) 0.0382(11) Uani 1 2 d S . . H3 H 0.7375 0.8846 0.7375 0.046 Uiso 1 2 calc SR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.01957(18) 0.01207(17) 0.01188(17) 0.000 0.000 0.000 Cl1 0.0141(6) 0.0141(6) 0.0223(10) 0.000 0.000 0.000 O1 0.033(3) 0.053(3) 0.191(9) 0.000 0.000 0.000 N1 0.0284(11) 0.0232(10) 0.0216(10) 0.0067(9) 0.0088(8) 0.0034(8) N2 0.0352(12) 0.0309(12) 0.0287(12) 0.0139(9) 0.0145(10) 0.0098(10) C1 0.0316(12) 0.0316(12) 0.0313(19) 0.0147(12) 0.0147(12) 0.0114(16) C2 0.0400(15) 0.0400(15) 0.036(2) 0.0215(14) 0.0215(14) 0.0191(19) C3 0.0379(14) 0.039(2) 0.0379(14) 0.0217(14) 0.0209(18) 0.0217(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1 2.284(6) . ? Cd1 N1 2.315(2) 27_575 ? Cd1 N1 2.315(2) 26_556 ? Cd1 N1 2.315(2) 4_576 ? Cd1 N1 2.315(2) . ? Cd1 Cl1 2.8018(3) . ? N1 N1 1.305(4) 38 ? N1 N2 1.330(3) . ? N2 C1 1.334(3) . ? C1 N2 1.334(3) 38 ? C1 C2 1.466(5) . ? C2 C3 1.393(3) . ? C2 C3 1.393(3) 9 ? C3 C2 1.393(3) 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 O1 Cd1 N1 95.07(5) . 27_575 ? O1 Cd1 N1 95.07(5) . 26_556 ? N1 Cd1 N1 169.85(11) 27_575 26_556 ? O1 Cd1 N1 95.07(5) . 4_576 ? N1 Cd1 N1 86.46(11) 27_575 4_576 ? N1 Cd1 N1 92.64(11) 26_556 4_576 ? O1 Cd1 N1 95.07(5) . . ? N1 Cd1 N1 92.64(11) 27_575 . ? N1 Cd1 N1 86.46(11) 26_556 . ? N1 Cd1 N1 169.85(11) 4_576 . ? O1 Cd1 Cl1 180.0 . . ? N1 Cd1 Cl1 84.93(5) 27_575 . ? N1 Cd1 Cl1 84.93(5) 26_556 . ? N1 Cd1 Cl1 84.93(5) 4_576 . ? N1 Cd1 Cl1 84.93(5) . . ? Cd1 Cl1 Cd1 90.0 25_776 37_775 ? Cd1 Cl1 Cd1 90.0 25_776 13_556 ? Cd1 Cl1 Cd1 180.0 37_775 13_556 ? Cd1 Cl1 Cd1 180.0 25_776 . ? Cd1 Cl1 Cd1 90.0 37_775 . ? Cd1 Cl1 Cd1 90.0 13_556 . ? N1 N1 N2 110.07(13) 38 . ? N1 N1 Cd1 125.02(5) 38 . ? N2 N1 Cd1 124.88(16) . . ? N1 N2 C1 103.7(2) . . ? N2 C1 N2 112.5(3) . 38 ? N2 C1 C2 123.75(17) . . ? N2 C1 C2 123.76(17) 38 . ? C3 C2 C3 119.6(4) . 9 ? C3 C2 C1 120.18(19) . . ? C3 C2 C1 120.18(19) 9 . ? C2 C3 C2 120.4(4) . 5 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.05 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.036 _refine_diff_density_min -0.526 _refine_diff_density_rms 0.100 ##### data_c2c #[Co4(OH)2(SO4)(bdt)2(H2O)4] (2). _database_code_depnum_ccdc_archive 'CCDC 826917' #TrackingRef '- AllCIFsDT-ART-05-2011-010984.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H18 Co4 N16 O10 S' _chemical_formula_weight 862.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.828(2) _cell_length_b 6.4136(5) _cell_length_c 13.9560(11) _cell_angle_alpha 90.00 _cell_angle_beta 91.547(2) _cell_angle_gamma 90.00 _cell_volume 2579.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 98(2) _cell_measurement_reflns_used 2345 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 28.27 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 2.23(2) _exptl_crystal_density_diffrn 2.220 _exptl_crystal_density_method flotation _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 2.699 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3455 _exptl_absorpt_correction_T_max 0.8997 _exptl_absorpt_process_details 'SADABS (Bruker, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 98(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 512 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 13043 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 28.28 _reflns_number_total 3211 _reflns_number_gt 2845 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'CrystalMaker (Palmer, 2006)' _computing_publication_material 'Bruker SHELXTL (Sheldrick, 2008)' _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^)+(0.0307P)^2^+5.7856P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3211 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0332 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0662 _refine_ls_wR_factor_gt 0.0637 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.090315(10) 0.04645(4) 0.40355(2) 0.00705(8) Uani 1 1 d . . . Co2 Co -0.008329(10) 0.20276(4) 0.44638(2) 0.00629(8) Uani 1 1 d . . . S1 S 0.0000 -0.09872(11) 0.2500 0.00739(14) Uani 1 2 d S . . O1 O 0.02218(5) 0.0423(2) 0.32482(11) 0.0089(3) Uani 1 1 d . . . O2 O -0.03617(5) -0.2255(2) 0.29278(11) 0.0113(3) Uani 1 1 d . . . O3 O 0.04597(5) 0.0543(2) 0.51819(11) 0.0075(3) Uani 1 1 d . . . H3A H 0.0554 0.1264 0.5664 0.026(8) Uiso 1 1 d . . . O90 O 0.15031(5) 0.0956(3) 0.48686(12) 0.0145(3) Uani 1 1 d . . . H90A H 0.1724 0.0811 0.4479 0.039(10) Uiso 1 1 d . . . H90B H 0.1592 0.0342 0.5386 0.026(9) Uiso 1 1 d . . . O91 O -0.05558(6) 0.3620(3) 0.35911(12) 0.0135(3) Uani 1 1 d . . . H91A H -0.0755 0.2909 0.3265 0.024(8) Uiso 1 1 d . . . H91B H -0.0471 0.4668 0.3261 0.026(9) Uiso 1 1 d . . . N1 N 0.13808(6) 0.0600(3) 0.29327(14) 0.0106(4) Uani 1 1 d . . . N2 N 0.12735(7) 0.0902(3) 0.20241(14) 0.0131(4) Uani 1 1 d . . . N3 N 0.18451(6) 0.0511(3) 0.30763(14) 0.0107(4) Uani 1 1 d . . . N4 N 0.16701(6) 0.0993(3) 0.15424(14) 0.0128(4) Uani 1 1 d . . . N5 N 0.08179(6) 0.3798(3) 0.38917(13) 0.0085(3) Uani 1 1 d . . . N6 N 0.04127(6) 0.4430(3) 0.42437(13) 0.0075(3) Uani 1 1 d . . . N7 N 0.04257(6) 0.6438(3) 0.43960(13) 0.0072(3) Uani 1 1 d . . . N8 N 0.08410(6) 0.7178(3) 0.41246(13) 0.0078(3) Uani 1 1 d . . . C1 C 0.20111(8) 0.0744(3) 0.22001(16) 0.0096(4) Uani 1 1 d . . . C2 C 0.25060(7) 0.0716(3) 0.19649(16) 0.0097(4) Uani 1 1 d . . . C3 C 0.26268(8) 0.0726(4) 0.10022(16) 0.0126(4) Uani 1 1 d . . . H3 H 0.2391 0.0774 0.0513 0.015 Uiso 1 1 calc R . . C4 C 0.28532(8) 0.0681(3) 0.26734(16) 0.0108(4) Uani 1 1 d . . . H4 H 0.2773 0.0694 0.3329 0.013 Uiso 1 1 calc R . . C5 C 0.30912(8) 0.0666(4) 0.07598(16) 0.0122(4) Uani 1 1 d . . . H5 H 0.3173 0.0672 0.0105 0.015 Uiso 1 1 calc R . . C6 C 0.33184(8) 0.0625(3) 0.24322(16) 0.0110(4) Uani 1 1 d . . . H6 H 0.3554 0.0605 0.2921 0.013 Uiso 1 1 calc R . . C7 C 0.34355(7) 0.0598(3) 0.14742(16) 0.0090(4) Uani 1 1 d . . . C8 C 0.10752(7) 0.5524(3) 0.38264(15) 0.0080(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.00667(14) 0.00613(14) 0.00849(14) 0.00020(10) 0.00284(10) 0.00010(10) Co2 0.00583(14) 0.00594(14) 0.00717(14) 0.00030(10) 0.00142(10) -0.00006(10) S1 0.0088(3) 0.0065(3) 0.0069(3) 0.000 0.0000(3) 0.000 O1 0.0104(7) 0.0087(7) 0.0075(7) -0.0017(6) 0.0004(6) -0.0003(6) O2 0.0118(7) 0.0110(7) 0.0109(7) 0.0008(6) 0.0004(6) -0.0024(6) O3 0.0070(7) 0.0070(7) 0.0087(7) -0.0010(6) 0.0016(5) -0.0014(5) O90 0.0097(8) 0.0215(9) 0.0121(8) 0.0031(7) 0.0008(6) -0.0012(7) O91 0.0129(8) 0.0110(8) 0.0162(8) 0.0032(6) -0.0047(6) -0.0013(6) N1 0.0089(9) 0.0093(9) 0.0138(9) -0.0002(7) 0.0010(7) -0.0001(7) N2 0.0106(9) 0.0174(10) 0.0114(9) -0.0022(8) 0.0028(7) 0.0002(8) N3 0.0088(9) 0.0089(9) 0.0147(9) -0.0002(7) 0.0037(7) 0.0003(7) N4 0.0084(9) 0.0170(10) 0.0131(9) -0.0021(8) 0.0038(7) -0.0008(7) N5 0.0046(8) 0.0103(9) 0.0108(9) 0.0001(7) 0.0014(7) 0.0004(7) N6 0.0068(8) 0.0073(8) 0.0084(8) -0.0005(7) 0.0018(6) 0.0002(7) N7 0.0067(8) 0.0067(8) 0.0084(8) 0.0006(7) 0.0010(6) -0.0006(7) N8 0.0061(8) 0.0089(8) 0.0086(8) 0.0005(7) 0.0025(6) -0.0006(7) C1 0.0107(10) 0.0063(9) 0.0119(10) -0.0007(8) 0.0039(8) 0.0005(8) C2 0.0097(10) 0.0071(9) 0.0124(10) 0.0007(8) 0.0037(8) -0.0005(8) C3 0.0106(10) 0.0170(11) 0.0101(10) 0.0010(9) -0.0009(8) 0.0001(8) C4 0.0131(10) 0.0100(10) 0.0097(10) 0.0002(8) 0.0048(8) 0.0011(8) C5 0.0109(10) 0.0145(11) 0.0115(10) 0.0003(8) 0.0034(8) -0.0003(8) C6 0.0105(10) 0.0104(10) 0.0121(10) 0.0007(8) 0.0004(8) 0.0001(8) C7 0.0073(10) 0.0051(9) 0.0149(10) 0.0011(8) 0.0033(8) 0.0004(7) C8 0.0081(10) 0.0072(10) 0.0086(9) 0.0004(8) 0.0008(7) 0.0002(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O3 2.0754(15) . ? Co1 O90 2.0817(16) . ? Co1 N1 2.0944(17) . ? Co1 N8 2.1190(18) 1_545 ? Co1 N5 2.1610(19) . ? Co1 O1 2.2246(15) . ? Co2 O3 2.0419(15) 5_556 ? Co2 O3 2.0679(15) . ? Co2 O91 2.0717(16) . ? Co2 N6 2.1297(18) . ? Co2 N7 2.1354(18) 5_566 ? Co2 O1 2.1889(15) . ? S1 O2 1.4622(16) 2 ? S1 O2 1.4622(16) . ? S1 O1 1.5104(15) 2 ? S1 O1 1.5104(15) . ? N1 N2 1.311(3) . ? N1 N3 1.349(3) . ? N2 N4 1.343(3) . ? N3 C1 1.334(3) . ? N4 C1 1.336(3) . ? N5 C8 1.337(3) . ? N5 N6 1.342(2) . ? N6 N7 1.306(2) . ? N7 N8 1.351(2) . ? N8 C8 1.331(3) . ? C1 C2 1.472(3) . ? C2 C4 1.388(3) . ? C2 C3 1.397(3) . ? C3 C5 1.390(3) . ? C3 H3 0.9500 . ? C4 C6 1.392(3) . ? C4 H4 0.9500 . ? C5 C7 1.388(3) . ? C5 H5 0.9500 . ? C6 C7 1.388(3) . ? C6 H6 0.9500 . ? C7 C8 1.483(3) 4_545 ? C8 C7 1.483(3) 4 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Co1 O90 94.90(6) . . ? O3 Co1 N1 175.11(7) . . ? O90 Co1 N1 81.45(7) . . ? O3 Co1 N8 85.65(6) . 1_545 ? O90 Co1 N8 100.84(7) . 1_545 ? N1 Co1 N8 98.21(7) . 1_545 ? O3 Co1 N5 88.66(6) . . ? O90 Co1 N5 89.58(7) . . ? N1 Co1 N5 88.06(7) . . ? N8 Co1 N5 168.50(7) 1_545 . ? O3 Co1 O1 80.04(6) . . ? O90 Co1 O1 170.66(6) . . ? N1 Co1 O1 103.10(7) . . ? N8 Co1 O1 86.69(6) 1_545 . ? N5 Co1 O1 82.49(6) . . ? O3 Co2 O3 84.90(6) 5_556 . ? O3 Co2 O91 101.25(6) 5_556 . ? O3 Co2 O91 171.47(6) . . ? O3 Co2 N6 169.18(7) 5_556 . ? O3 Co2 N6 84.30(6) . . ? O91 Co2 N6 89.54(7) . . ? O3 Co2 N7 86.12(6) 5_556 5_566 ? O3 Co2 N7 102.13(6) . 5_566 ? O91 Co2 N7 84.32(7) . 5_566 ? N6 Co2 N7 95.73(7) . 5_566 ? O3 Co2 O1 92.02(6) 5_556 . ? O3 Co2 O1 81.05(6) . . ? O91 Co2 O1 92.73(6) . . ? N6 Co2 O1 86.73(6) . . ? N7 Co2 O1 176.14(6) 5_566 . ? O2 S1 O2 112.45(13) 2 . ? O2 S1 O1 110.12(8) 2 2 ? O2 S1 O1 108.77(8) . 2 ? O2 S1 O1 108.78(8) 2 . ? O2 S1 O1 110.12(8) . . ? O1 S1 O1 106.42(12) 2 . ? S1 O1 Co2 130.23(9) . . ? S1 O1 Co1 134.45(9) . . ? Co2 O1 Co1 88.82(5) . . ? Co2 O3 Co2 95.10(6) 5_556 . ? Co2 O3 Co1 120.63(7) 5_556 . ? N2 N1 N3 110.91(18) . . ? N2 N1 Co1 125.04(15) . . ? N3 N1 Co1 123.94(15) . . ? N1 N2 N4 107.98(18) . . ? C1 N3 N1 103.78(18) . . ? C1 N4 N2 105.75(18) . . ? C8 N5 N6 105.39(17) . . ? C8 N5 Co1 139.77(15) . . ? N6 N5 Co1 111.25(13) . . ? N7 N6 N5 109.61(17) . . ? N7 N6 Co2 134.95(14) . . ? N5 N6 Co2 115.40(13) . . ? N6 N7 N8 108.83(17) . . ? N6 N7 Co2 124.33(14) . 5_566 ? N8 N7 Co2 118.54(13) . 5_566 ? C8 N8 N7 105.55(17) . . ? C8 N8 Co1 136.93(15) . 1_565 ? N7 N8 Co1 116.28(13) . 1_565 ? N3 C1 N4 111.57(19) . . ? N3 C1 C2 125.2(2) . . ? N4 C1 C2 123.19(19) . . ? C4 C2 C3 119.4(2) . . ? C4 C2 C1 121.7(2) . . ? C3 C2 C1 118.9(2) . . ? C5 C3 C2 120.0(2) . . ? C5 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C2 C4 C6 120.6(2) . . ? C2 C4 H4 119.7 . . ? C6 C4 H4 119.7 . . ? C7 C5 C3 120.0(2) . . ? C7 C5 H5 120.0 . . ? C3 C5 H5 120.0 . . ? C7 C6 C4 119.6(2) . . ? C7 C6 H6 120.2 . . ? C4 C6 H6 120.2 . . ? C5 C7 C6 120.2(2) . . ? C5 C7 C8 117.69(19) . 4_545 ? C6 C7 C8 122.1(2) . 4_545 ? N8 C8 N5 110.60(18) . . ? N8 C8 C7 123.85(19) . 4 ? N5 C8 C7 125.44(19) . 4 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 S1 O1 Co2 -159.22(11) 2 . . . ? O2 S1 O1 Co2 -35.57(14) . . . . ? O1 S1 O1 Co2 82.16(11) 2 . . . ? O2 S1 O1 Co1 -16.83(15) 2 . . . ? O2 S1 O1 Co1 106.82(13) . . . . ? O1 S1 O1 Co1 -135.45(14) 2 . . . ? O3 Co2 O1 S1 43.13(12) 5_556 . . . ? O3 Co2 O1 S1 127.64(12) . . . . ? O91 Co2 O1 S1 -58.24(12) . . . . ? N6 Co2 O1 S1 -147.62(12) . . . . ? O3 Co2 O1 Co1 -111.03(6) 5_556 . . . ? O3 Co2 O1 Co1 -26.52(5) . . . . ? O91 Co2 O1 Co1 147.60(6) . . . . ? N6 Co2 O1 Co1 58.21(6) . . . . ? O3 Co1 O1 S1 -125.72(13) . . . . ? N1 Co1 O1 S1 58.10(14) . . . . ? N8 Co1 O1 S1 -39.56(13) 1_545 . . . ? N5 Co1 O1 S1 144.33(13) . . . . ? O3 Co1 O1 Co2 26.50(5) . . . . ? N1 Co1 O1 Co2 -149.68(6) . . . . ? N8 Co1 O1 Co2 112.66(6) 1_545 . . . ? N5 Co1 O1 Co2 -63.45(6) . . . . ? O3 Co2 O3 Co2 0.0 5_556 . . 5_556 ? N6 Co2 O3 Co2 179.56(7) . . . 5_556 ? N7 Co2 O3 Co2 84.91(7) 5_566 . . 5_556 ? O1 Co2 O3 Co2 -92.86(6) . . . 5_556 ? O3 Co2 O3 Co1 121.65(8) 5_556 . . . ? N6 Co2 O3 Co1 -58.79(6) . . . . ? N7 Co2 O3 Co1 -153.44(6) 5_566 . . . ? O1 Co2 O3 Co1 28.79(6) . . . . ? O90 Co1 O3 Co2 -116.49(9) . . . 5_556 ? N8 Co1 O3 Co2 -15.95(9) 1_545 . . 5_556 ? N5 Co1 O3 Co2 154.05(9) . . . 5_556 ? O1 Co1 O3 Co2 71.44(8) . . . 5_556 ? O90 Co1 O3 Co2 143.70(6) . . . . ? N8 Co1 O3 Co2 -115.77(7) 1_545 . . . ? N5 Co1 O3 Co2 54.23(7) . . . . ? O1 Co1 O3 Co2 -28.37(6) . . . . ? O90 Co1 N1 N2 -162.84(19) . . . . ? N8 Co1 N1 N2 97.34(18) 1_545 . . . ? N5 Co1 N1 N2 -72.97(18) . . . . ? O1 Co1 N1 N2 8.85(19) . . . . ? O90 Co1 N1 N3 13.00(16) . . . . ? N8 Co1 N1 N3 -86.82(17) 1_545 . . . ? N5 Co1 N1 N3 102.87(17) . . . . ? O1 Co1 N1 N3 -175.31(16) . . . . ? N3 N1 N2 N4 0.8(2) . . . . ? Co1 N1 N2 N4 177.07(14) . . . . ? N2 N1 N3 C1 -0.9(2) . . . . ? Co1 N1 N3 C1 -177.27(14) . . . . ? N1 N2 N4 C1 -0.3(2) . . . . ? O3 Co1 N5 C8 128.8(2) . . . . ? O90 Co1 N5 C8 33.9(2) . . . . ? N1 Co1 N5 C8 -47.6(2) . . . . ? N8 Co1 N5 C8 -170.9(3) 1_545 . . . ? O1 Co1 N5 C8 -151.0(2) . . . . ? O3 Co1 N5 N6 -25.42(14) . . . . ? O90 Co1 N5 N6 -120.34(14) . . . . ? N1 Co1 N5 N6 158.20(14) . . . . ? N8 Co1 N5 N6 34.9(4) 1_545 . . . ? O1 Co1 N5 N6 54.71(13) . . . . ? C8 N5 N6 N7 -0.8(2) . . . . ? Co1 N5 N6 N7 162.32(13) . . . . ? C8 N5 N6 Co2 -179.02(13) . . . . ? Co1 N5 N6 Co2 -15.94(17) . . . . ? O3 Co2 N6 N7 -125.0(3) 5_556 . . . ? O3 Co2 N6 N7 -127.4(2) . . . . ? O91 Co2 N6 N7 58.6(2) . . . . ? N7 Co2 N6 N7 -25.7(2) 5_566 . . . ? O1 Co2 N6 N7 151.3(2) . . . . ? O3 Co2 N6 N5 52.6(4) 5_556 . . . ? O3 Co2 N6 N5 50.33(14) . . . . ? O91 Co2 N6 N5 -123.76(14) . . . . ? N7 Co2 N6 N5 152.00(14) 5_566 . . . ? O1 Co2 N6 N5 -30.99(14) . . . . ? N5 N6 N7 N8 1.3(2) . . . . ? Co2 N6 N7 N8 179.09(15) . . . . ? N5 N6 N7 Co2 -146.29(14) . . . 5_566 ? Co2 N6 N7 Co2 31.5(3) . . . 5_566 ? N6 N7 N8 C8 -1.3(2) . . . . ? Co2 N7 N8 C8 148.44(14) 5_566 . . . ? N6 N7 N8 Co1 168.18(13) . . . 1_565 ? Co2 N7 N8 Co1 -42.08(18) 5_566 . . 1_565 ? N1 N3 C1 N4 0.7(2) . . . . ? N1 N3 C1 C2 -178.7(2) . . . . ? N2 N4 C1 N3 -0.3(2) . . . . ? N2 N4 C1 C2 179.1(2) . . . . ? N3 C1 C2 C4 -7.7(3) . . . . ? N4 C1 C2 C4 172.9(2) . . . . ? N3 C1 C2 C3 172.3(2) . . . . ? N4 C1 C2 C3 -7.1(3) . . . . ? C4 C2 C3 C5 1.0(3) . . . . ? C1 C2 C3 C5 -179.0(2) . . . . ? C3 C2 C4 C6 -0.9(3) . . . . ? C1 C2 C4 C6 179.1(2) . . . . ? C2 C3 C5 C7 0.0(4) . . . . ? C2 C4 C6 C7 -0.2(3) . . . . ? C3 C5 C7 C6 -1.1(3) . . . . ? C3 C5 C7 C8 179.6(2) . . . 4_545 ? C4 C6 C7 C5 1.2(3) . . . . ? C4 C6 C7 C8 -179.5(2) . . . 4_545 ? N7 N8 C8 N5 0.8(2) . . . . ? Co1 N8 C8 N5 -165.29(16) 1_565 . . . ? N7 N8 C8 C7 -175.52(19) . . . 4 ? Co1 N8 C8 C7 18.3(3) 1_565 . . 4 ? N6 N5 C8 N8 -0.1(2) . . . . ? Co1 N5 C8 N8 -155.25(17) . . . . ? N6 N5 C8 C7 176.2(2) . . . 4 ? Co1 N5 C8 C7 21.0(4) . . . 4 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.531 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.096 ##### data_pnma #[Co3(OH)(SO4)(btt)(H2O)4]\/Y3H2O (3\/Y3H2O). _database_code_depnum_ccdc_archive 'CCDC 826918' #TrackingRef '- AllCIFsDT-ART-05-2011-010984.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H12 Co3 N12 O9 S H2 O 2(H2 O)' _chemical_formula_sum 'C9 H18 Co3 N12 O12 S' _chemical_formula_weight 695.20 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P nma' _symmetry_space_group_name_Hall "-P 2ac 2n'" loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 7.3246(4) _cell_length_b 13.2240(7) _cell_length_c 22.7669(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2205.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 98(2) _cell_measurement_reflns_used 1232 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 28.27 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 2.07(2) _exptl_crystal_density_diffrn 2.094 _exptl_crystal_density_method flotation _exptl_crystal_F_000 1396 _exptl_absorpt_coefficient_mu 2.413 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6988 _exptl_absorpt_correction_T_max 0.7288 _exptl_absorpt_process_details 'SADABS (Bruker, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 98(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 512 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 21880 _diffrn_reflns_av_R_equivalents 0.0548 _diffrn_reflns_av_sigmaI/netI 0.0294 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 28.08 _reflns_number_total 2793 _reflns_number_gt 2336 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'CrystalMaker (Palmer, 2006)' _computing_publication_material 'Bruker SHELXTL (Sheldrick, 2008)' _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^)+(0.0472P)^2^+4.1794P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2793 _refine_ls_number_parameters 196 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.0979 _refine_ls_wR_factor_gt 0.0924 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 0.34357(8) 0.2500 0.25854(2) 0.01322(14) Uani 1 2 d S . . Co2 Co -0.17312(6) 0.11722(3) 0.110612(17) 0.01559(12) Uani 1 1 d . . . S1 S 0.17587(14) 0.2500 0.14792(4) 0.0138(2) Uani 1 2 d S . . O1 O 0.2561(4) 0.2500 0.34536(13) 0.0136(6) Uani 1 2 d S . . H1A H 0.1397 0.2500 0.3495 0.019(13) Uiso 1 2 d S . . O2 O 0.1050(4) 0.2500 0.21016(12) 0.0140(6) Uani 1 2 d S . . O3 O 0.3736(4) 0.2500 0.15561(14) 0.0222(7) Uani 1 2 d S . . O4 O 0.1107(3) 0.15912(16) 0.11747(9) 0.0173(4) Uani 1 1 d . . . O90 O -0.0878(4) -0.01725(19) 0.07101(13) 0.0352(7) Uani 1 1 d . . . H90A H -0.1482 -0.0323 0.0393 0.064(17) Uiso 1 1 d . . . H90B H 0.0254 -0.0118 0.0621 0.064(15) Uiso 1 1 d . . . O91 O -0.4392(4) 0.0634(2) 0.10260(10) 0.0281(6) Uani 1 1 d . . . H91A H -0.5053 0.0601 0.1336 0.040(13) Uiso 1 1 d . . . H91B H -0.5014 0.0711 0.0710 0.063(17) Uiso 1 1 d . . . O92 O 0.2519(8) 0.7500 0.3938(2) 0.118(4) Uani 1 2 d S . . H92A H 0.1533 0.7500 0.3727 0.166 Uiso 1 2 d S . . H92B H 0.2612 0.8132 0.3992 0.166 Uiso 0.50 1 d P . . O93A O 0.2796(5) 0.0447(3) 0.02721(17) 0.0181(12) Uani 0.540(7) 1 d P A 1 O93B O 0.2980(8) 0.1314(5) 0.0069(2) 0.0294(16) Uani 0.460(7) 1 d P A 2 N1 N 0.3593(4) 0.0934(2) 0.25756(11) 0.0167(5) Uani 1 1 d . . . N2 N 0.3448(4) 0.0446(2) 0.30816(11) 0.0192(6) Uani 1 1 d . . . N3 N 0.3659(3) 0.0273(2) 0.21343(11) 0.0153(5) Uani 1 1 d . . . N4 N 0.3406(4) -0.0550(2) 0.29829(12) 0.0190(6) Uani 1 1 d . . . N5 N 0.2231(4) -0.16638(19) 0.02271(11) 0.0192(6) Uani 1 1 d . . . N6 N 0.1943(3) -0.20000(19) -0.03168(11) 0.0152(5) Uani 1 1 d . . . C1 C 0.3526(4) -0.0627(2) 0.23987(13) 0.0152(6) Uani 1 1 d . . . C2 C 0.3415(4) -0.1592(2) 0.20813(13) 0.0153(6) Uani 1 1 d . . . C3 C 0.3641(6) -0.2500 0.23785(18) 0.0162(8) Uani 1 2 d S . . H3 H 0.3950 -0.2500 0.2784 0.019 Uiso 1 2 calc SR . . C4 C 0.2994(4) -0.1591(2) 0.14831(13) 0.0157(6) Uani 1 1 d . . . H4 H 0.2834 -0.0969 0.1281 0.019 Uiso 1 1 calc R . . C5 C 0.2808(6) -0.2500 0.11837(18) 0.0151(8) Uani 1 2 d S . . C6 C 0.2409(6) -0.2500 0.05478(18) 0.0138(8) Uani 1 2 d S . . 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 0.0126(3) 0.0184(3) 0.0087(3) 0.000 -0.0005(2) 0.000 Co2 0.0238(2) 0.0140(2) 0.00895(19) 0.00114(15) -0.00323(16) -0.00490(16) S1 0.0101(5) 0.0217(5) 0.0097(4) 0.000 -0.0002(4) 0.000 O1 0.0098(14) 0.0206(15) 0.0103(13) 0.000 0.0018(11) 0.000 O2 0.0112(13) 0.0225(15) 0.0083(13) 0.000 0.0009(11) 0.000 O3 0.0105(15) 0.042(2) 0.0139(15) 0.000 0.0006(12) 0.000 O4 0.0184(11) 0.0201(11) 0.0133(10) -0.0029(8) -0.0007(8) 0.0039(9) O90 0.0359(15) 0.0207(12) 0.0491(17) -0.0159(12) -0.0238(13) 0.0119(11) O91 0.0310(13) 0.0387(15) 0.0146(11) -0.0029(10) 0.0021(10) -0.0190(11) O92 0.043(3) 0.276(12) 0.034(3) 0.000 -0.006(3) 0.000 O93A 0.020(2) 0.020(2) 0.014(2) -0.0042(16) -0.0007(16) -0.0037(16) O93B 0.029(3) 0.040(4) 0.020(3) -0.005(2) 0.001(2) 0.002(2) N1 0.0199(13) 0.0197(12) 0.0104(12) 0.0000(10) 0.0007(10) -0.0041(10) N2 0.0272(15) 0.0181(13) 0.0123(12) -0.0017(10) 0.0008(10) -0.0051(11) N3 0.0180(12) 0.0180(12) 0.0099(11) -0.0032(10) -0.0006(9) -0.0019(10) N4 0.0248(14) 0.0182(13) 0.0141(12) -0.0031(10) 0.0000(10) -0.0030(11) N5 0.0323(15) 0.0164(13) 0.0091(11) -0.0003(10) -0.0038(11) -0.0028(11) N6 0.0187(12) 0.0156(12) 0.0113(11) -0.0007(9) -0.0018(10) -0.0013(10) C1 0.0148(14) 0.0184(14) 0.0125(14) -0.0024(11) -0.0006(10) -0.0006(11) C2 0.0168(14) 0.0182(14) 0.0108(13) -0.0029(11) 0.0011(11) -0.0011(11) C3 0.020(2) 0.021(2) 0.0076(18) 0.000 -0.0001(15) 0.000 C4 0.0178(15) 0.0162(14) 0.0131(14) 0.0007(11) 0.0004(11) 0.0005(11) C5 0.016(2) 0.019(2) 0.0100(19) 0.000 -0.0013(15) 0.000 C6 0.017(2) 0.0128(19) 0.0119(19) 0.000 0.0010(15) 0.000 _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 O2 2.043(3) 6_656 ? Co1 O2 2.066(3) . ? Co1 N1 2.074(3) 7_565 ? Co1 N1 2.074(3) . ? Co1 O1 2.078(3) . ? Co1 O3 2.354(3) . ? Co2 O91 2.083(2) . ? Co2 O1 2.0873(16) 6_556 ? Co2 N2 2.088(3) 6_556 ? Co2 O90 2.089(2) . ? Co2 N6 2.110(2) 5 ? Co2 O4 2.157(2) . ? S1 O3 1.459(3) . ? S1 O4 1.467(2) . ? S1 O4 1.467(2) 7_565 ? S1 O2 1.509(3) . ? O1 Co2 2.0873(16) 4 ? O1 Co2 2.0873(16) 6_656 ? O2 Co1 2.043(3) 6_556 ? N1 N2 1.325(4) . ? N1 N3 1.332(3) . ? N2 N4 1.335(4) . ? N2 Co2 2.088(3) 6_656 ? N3 C1 1.337(4) . ? N4 C1 1.337(4) . ? N5 C6 1.331(3) . ? N5 N6 1.333(3) . ? N6 N6 1.322(5) 7 ? N6 Co2 2.110(2) 5 ? C1 C2 1.469(4) . ? C2 C3 1.389(4) . ? C2 C4 1.396(4) . ? C3 C2 1.389(4) 7 ? C3 H3 0.9500 . ? C4 C5 1.389(4) . ? C4 H4 0.9500 . ? C5 C4 1.389(4) 7 ? C5 C6 1.477(6) . ? C6 N5 1.331(3) 7 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Co1 O2 168.19(8) 6_656 . ? O2 Co1 N1 87.22(7) 6_656 7_565 ? O2 Co1 N1 92.37(7) . 7_565 ? O2 Co1 N1 87.22(7) 6_656 . ? O2 Co1 N1 92.37(7) . . ? N1 Co1 N1 173.49(15) 7_565 . ? O2 Co1 O1 87.55(11) 6_656 . ? O2 Co1 O1 104.27(11) . . ? N1 Co1 O1 91.57(7) 7_565 . ? N1 Co1 O1 91.57(7) . . ? O2 Co1 O3 105.05(11) 6_656 . ? O2 Co1 O3 63.14(11) . . ? N1 Co1 O3 89.09(7) 7_565 . ? N1 Co1 O3 89.09(7) . . ? O1 Co1 O3 167.40(11) . . ? O91 Co2 O1 95.57(11) . 6_556 ? O91 Co2 N2 88.81(10) . 6_556 ? O1 Co2 N2 88.71(10) 6_556 6_556 ? O91 Co2 O90 87.21(11) . . ? O1 Co2 O90 175.93(10) 6_556 . ? N2 Co2 O90 88.38(11) 6_556 . ? O91 Co2 N6 91.95(10) . 5 ? O1 Co2 N6 87.38(10) 6_556 5 ? N2 Co2 N6 176.07(10) 6_556 5 ? O90 Co2 N6 95.51(11) . 5 ? O91 Co2 O4 174.81(10) . . ? O1 Co2 O4 89.34(9) 6_556 . ? N2 Co2 O4 89.63(9) 6_556 . ? O90 Co2 O4 87.80(10) . . ? N6 Co2 O4 89.95(9) 5 . ? O3 S1 O4 112.33(11) . . ? O3 S1 O4 112.32(11) . 7_565 ? O4 S1 O4 109.98(18) . 7_565 ? O3 S1 O2 103.23(18) . . ? O4 S1 O2 109.37(11) . . ? O4 S1 O2 109.37(11) 7_565 . ? Co1 O1 Co2 112.35(8) . 4 ? Co1 O1 Co2 112.35(8) . 6_656 ? Co2 O1 Co2 114.54(13) 4 6_656 ? S1 O2 Co1 130.54(18) . 6_556 ? S1 O2 Co1 102.10(15) . . ? Co1 O2 Co1 127.36(14) 6_556 . ? S1 O3 Co1 91.54(15) . . ? S1 O4 Co2 123.94(13) . . ? N2 N1 N3 109.8(2) . . ? N2 N1 Co1 118.2(2) . . ? N3 N1 Co1 131.7(2) . . ? N1 N2 N4 109.7(2) . . ? N1 N2 Co2 123.4(2) . 6_656 ? N4 N2 Co2 126.9(2) . 6_656 ? N1 N3 C1 104.0(2) . . ? N2 N4 C1 103.9(3) . . ? C6 N5 N6 104.4(3) . . ? N6 N6 N5 109.49(16) 7 . ? N6 N6 Co2 121.26(7) 7 5 ? N5 N6 Co2 129.05(19) . 5 ? N4 C1 N3 112.6(3) . . ? N4 C1 C2 123.5(3) . . ? N3 C1 C2 123.8(3) . . ? C3 C2 C4 120.1(3) . . ? C3 C2 C1 120.4(3) . . ? C4 C2 C1 119.4(3) . . ? C2 C3 C2 119.8(4) 7 . ? C2 C3 H3 120.1 7 . ? C2 C3 H3 120.1 . . ? C5 C4 C2 120.0(3) . . ? C5 C4 H4 120.0 . . ? C2 C4 H4 120.0 . . ? C4 C5 C4 119.9(4) 7 . ? C4 C5 C6 120.04(19) 7 . ? C4 C5 C6 120.04(19) . . ? N5 C6 N5 112.3(4) . 7 ? N5 C6 C5 123.84(18) . . ? N5 C6 C5 123.84(18) 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 O2 Co1 O1 Co2 65.44(11) 6_656 . . 4 ? O2 Co1 O1 Co2 -114.56(11) . . . 4 ? N1 Co1 O1 Co2 -21.71(13) 7_565 . . 4 ? N1 Co1 O1 Co2 152.59(13) . . . 4 ? O3 Co1 O1 Co2 -114.56(11) . . . 4 ? O2 Co1 O1 Co2 -65.44(11) 6_656 . . 6_656 ? O2 Co1 O1 Co2 114.56(11) . . . 6_656 ? N1 Co1 O1 Co2 -152.59(13) 7_565 . . 6_656 ? N1 Co1 O1 Co2 21.71(13) . . . 6_656 ? O3 Co1 O1 Co2 114.56(11) . . . 6_656 ? O3 S1 O2 Co1 180.0 . . . 6_556 ? O4 S1 O2 Co1 -60.25(11) . . . 6_556 ? O4 S1 O2 Co1 60.25(11) 7_565 . . 6_556 ? O3 S1 O2 Co1 0.0 . . . . ? O4 S1 O2 Co1 119.75(11) . . . . ? O4 S1 O2 Co1 -119.75(11) 7_565 . . . ? O2 Co1 O2 S1 0.000(1) 6_656 . . . ? N1 Co1 O2 S1 87.77(7) 7_565 . . . ? N1 Co1 O2 S1 -87.77(7) . . . . ? O1 Co1 O2 S1 180.0 . . . . ? O3 Co1 O2 S1 0.0 . . . . ? O2 Co1 O2 Co1 180.0 6_656 . . 6_556 ? N1 Co1 O2 Co1 -92.23(7) 7_565 . . 6_556 ? N1 Co1 O2 Co1 92.23(7) . . . 6_556 ? O1 Co1 O2 Co1 0.0 . . . 6_556 ? O3 Co1 O2 Co1 180.0 . . . 6_556 ? O4 S1 O3 Co1 -117.70(11) . . . . ? O4 S1 O3 Co1 117.69(11) 7_565 . . . ? O2 S1 O3 Co1 0.0 . . . . ? O2 Co1 O3 S1 180.0 6_656 . . . ? O2 Co1 O3 S1 0.0 . . . . ? N1 Co1 O3 S1 -93.12(7) 7_565 . . . ? N1 Co1 O3 S1 93.12(7) . . . . ? O1 Co1 O3 S1 0.0 . . . . ? O3 S1 O4 Co2 169.00(15) . . . . ? O4 S1 O4 Co2 -65.1(2) 7_565 . . . ? O2 S1 O4 Co2 55.02(19) . . . . ? O1 Co2 O4 S1 2.74(16) 6_556 . . . ? N2 Co2 O4 S1 -85.97(16) 6_556 . . . ? O90 Co2 O4 S1 -174.36(17) . . . . ? N6 Co2 O4 S1 90.13(16) 5 . . . ? O2 Co1 N1 N2 76.5(2) 6_656 . . . ? O2 Co1 N1 N2 -115.3(2) . . . . ? O1 Co1 N1 N2 -10.9(2) . . . . ? O3 Co1 N1 N2 -178.4(2) . . . . ? O2 Co1 N1 N3 -110.5(3) 6_656 . . . ? O2 Co1 N1 N3 57.7(3) . . . . ? O1 Co1 N1 N3 162.0(3) . . . . ? O3 Co1 N1 N3 -5.4(3) . . . . ? N3 N1 N2 N4 -0.3(4) . . . . ? Co1 N1 N2 N4 174.1(2) . . . . ? N3 N1 N2 Co2 -179.27(19) . . . 6_656 ? Co1 N1 N2 Co2 -4.8(3) . . . 6_656 ? N2 N1 N3 C1 0.7(3) . . . . ? Co1 N1 N3 C1 -172.7(2) . . . . ? N1 N2 N4 C1 -0.2(3) . . . . ? Co2 N2 N4 C1 178.7(2) 6_656 . . . ? C6 N5 N6 N6 0.2(3) . . . 7 ? C6 N5 N6 Co2 -174.5(2) . . . 5 ? N2 N4 C1 N3 0.7(4) . . . . ? N2 N4 C1 C2 -176.0(3) . . . . ? N1 N3 C1 N4 -0.8(3) . . . . ? N1 N3 C1 C2 175.8(3) . . . . ? N4 C1 C2 C3 -16.5(5) . . . . ? N3 C1 C2 C3 167.2(3) . . . . ? N4 C1 C2 C4 160.5(3) . . . . ? N3 C1 C2 C4 -15.8(5) . . . . ? C4 C2 C3 C2 -1.1(6) . . . 7 ? C1 C2 C3 C2 175.8(2) . . . 7 ? C3 C2 C4 C5 -0.3(5) . . . . ? C1 C2 C4 C5 -177.3(3) . . . . ? C2 C4 C5 C4 1.7(6) . . . 7 ? C2 C4 C5 C6 -178.5(3) . . . . ? N6 N5 C6 N5 -0.4(5) . . . 7 ? N6 N5 C6 C5 178.0(4) . . . . ? C4 C5 C6 N5 -179.2(4) 7 . . . ? C4 C5 C6 N5 1.0(6) . . . . ? C4 C5 C6 N5 -1.0(6) 7 . . 7 ? C4 C5 C6 N5 179.2(4) . . . 7 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.08 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.724 _refine_diff_density_min -0.761 _refine_diff_density_rms 0.111 data_p21c #[Co5F2(dbdt)4(H2O)6]\/Y2H2O (1\/Y2H2O). _database_code_depnum_ccdc_archive 'CCDC 826919' #TrackingRef '- AllCIFsDT-ART-05-2011-010984.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H44 Co5 F2 N32 O6, 2(H2 O)' _chemical_formula_sum 'C56 H48 Co5 F2 N32 O8' _chemical_formula_weight 1629.91 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.0142(6) _cell_length_b 25.4144(11) _cell_length_c 8.7031(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.2400(10) _cell_angle_gamma 90.00 _cell_volume 3050.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 98(2) _cell_measurement_reflns_used 987 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 28.27 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 1.79(2) _exptl_crystal_density_diffrn 1.775 _exptl_crystal_density_method flotation _exptl_crystal_F_000 1650 _exptl_absorpt_coefficient_mu 1.424 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6747 _exptl_absorpt_correction_T_max 0.8707 _exptl_absorpt_process_details 'SADABS (Bruker, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 98(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 512 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_reflns_number 31767 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 28.08 _reflns_number_total 7420 _reflns_number_gt 6163 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'CrystalMaker (Palmer, 2006)' _computing_publication_material 'Bruker SHELXTL (Sheldrick, 2008)' _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^)+(0.0577P)^2^+3.5532P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7420 _refine_ls_number_parameters 472 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1135 _refine_ls_wR_factor_gt 0.1065 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.5000 0.5000 1.0000 0.01323(11) Uani 1 2 d S . . Co2 Co 0.42511(2) 0.543871(14) 0.64119(4) 0.01421(10) Uani 1 1 d . . . Co3 Co 0.53917(3) 0.633276(15) 0.95310(4) 0.01723(10) Uani 1 1 d . . . F1 F 0.45507(12) 0.56762(7) 0.87679(19) 0.0213(3) Uani 1 1 d . . . O90 O 0.30719(14) 0.59438(8) 0.6001(2) 0.0215(4) Uani 1 1 d . . . H90A H 0.2940 0.6005 0.5026 0.032(10) Uiso 1 1 d . . . H90B H 0.3182 0.6249 0.6397 0.036(14) Uiso 1 1 d . . . O91 O 0.46463(15) 0.63882(8) 1.1459(2) 0.0224(4) Uani 1 1 d . . . H91A H 0.4333 0.6666 1.1587 0.032(10) Uiso 1 1 d . . . H91B H 0.4911 0.6300 1.2376 0.035(14) Uiso 1 1 d . . . O92 O 0.63109(17) 0.69451(10) 1.0272(3) 0.0328(5) Uani 1 1 d . . . H92A H 0.6368 0.7038 1.1218 0.037(11) Uiso 1 1 d . . . H92B H 0.5935 0.7148 0.9662 0.045(12) Uiso 1 1 d . . . O93 O 0.6532(2) 0.72414(13) 0.3174(4) 0.0586(8) Uani 1 1 d . . . H93A H 0.5949 0.7359 0.3111 0.087 Uiso 1 1 d . . . H93B H 0.6540 0.6960 0.3723 0.087 Uiso 1 1 d . . . N1 N 0.39465(16) 0.46062(9) 0.8486(3) 0.0177(5) Uani 1 1 d . . . N2 N 0.36091(17) 0.41529(10) 0.8870(3) 0.0185(5) Uani 1 1 d . . . N3 N 0.28048(17) 0.40309(10) 0.7845(3) 0.0198(5) Uani 1 1 d . . . N4 N 0.33853(16) 0.47946(9) 0.7177(3) 0.0166(5) Uani 1 1 d . . . N5 N -0.40414(16) 0.48991(9) -0.1624(3) 0.0167(5) Uani 1 1 d . . . N6 N -0.45069(16) 0.49284(9) -0.3111(3) 0.0165(5) Uani 1 1 d . . . N7 N -0.39641(16) 0.47121(9) -0.4014(3) 0.0170(5) Uani 1 1 d . . . N8 N -0.31376(17) 0.45343(10) -0.3142(3) 0.0219(5) Uani 1 1 d . . . N9 N 0.52722(17) 0.60472(10) 0.6146(3) 0.0186(5) Uani 1 1 d . . . N10 N 0.55353(17) 0.61846(10) 0.4832(3) 0.0210(5) Uani 1 1 d . . . N11 N 0.63822(18) 0.64449(11) 0.5156(3) 0.0248(5) Uani 1 1 d . . . N12 N 0.59408(17) 0.62165(9) 0.7369(3) 0.0190(5) Uani 1 1 d . . . N13 N 1.34531(17) 0.81495(10) 1.2622(3) 0.0219(5) Uani 1 1 d . . . N14 N 1.43866(18) 0.81025(10) 1.3286(3) 0.0236(5) Uani 1 1 d . . . N15 N 1.4664(2) 0.76129(11) 1.3170(4) 0.0355(7) Uani 1 1 d . . . N16 N 1.3912(2) 0.73241(11) 1.2458(4) 0.0348(7) Uani 1 1 d . . . C1 C 0.26794(19) 0.44308(11) 0.6836(3) 0.0171(5) Uani 1 1 d . . . C2 C 0.18419(19) 0.44622(11) 0.5551(3) 0.0185(5) Uani 1 1 d . . . C3 C 0.1531(2) 0.49411(12) 0.4867(3) 0.0225(6) Uani 1 1 d . . . H3 H 0.1883 0.5253 0.5197 0.027 Uiso 1 1 calc R . . C4 C 0.0716(2) 0.49686(12) 0.3709(4) 0.0242(6) Uani 1 1 d . . . H4 H 0.0519 0.5299 0.3252 0.029 Uiso 1 1 calc R . . C5 C 0.1310(2) 0.40101(12) 0.5055(3) 0.0228(6) Uani 1 1 d . . . H5 H 0.1505 0.3680 0.5518 0.027 Uiso 1 1 calc R . . C6 C 0.0495(2) 0.40406(12) 0.3886(4) 0.0243(6) Uani 1 1 d . . . H6 H 0.0148 0.3728 0.3548 0.029 Uiso 1 1 calc R . . C7 C 0.0175(2) 0.45177(12) 0.3199(3) 0.0204(6) Uani 1 1 d . . . C8 C -0.0716(2) 0.45525(12) 0.1980(3) 0.0207(6) Uani 1 1 d . . . C9 C -0.0883(3) 0.49863(13) 0.0991(4) 0.0354(8) Uani 1 1 d . . . H9 H -0.0431 0.5269 0.1117 0.042 Uiso 1 1 calc R . . C10 C -0.1698(3) 0.50131(13) -0.0174(4) 0.0341(8) Uani 1 1 d . . . H10 H -0.1788 0.5309 -0.0853 0.041 Uiso 1 1 calc R . . C11 C -0.1415(2) 0.41640(14) 0.1791(4) 0.0318(7) Uani 1 1 d . . . H11 H -0.1329 0.3867 0.2466 0.038 Uiso 1 1 calc R . . C12 C -0.2244(2) 0.41939(14) 0.0637(4) 0.0324(8) Uani 1 1 d . . . H12 H -0.2716 0.3922 0.0542 0.039 Uiso 1 1 calc R . . C13 C -0.23775(19) 0.46152(12) -0.0357(3) 0.0189(6) Uani 1 1 d . . . C14 C -0.32022(19) 0.46658(11) -0.1682(3) 0.0173(5) Uani 1 1 d . . . C15 C 0.6621(2) 0.64540(12) 0.6714(3) 0.0212(6) Uani 1 1 d . . . C16 C 0.7548(2) 0.66626(12) 0.7557(3) 0.0221(6) Uani 1 1 d . . . C17 C 0.8036(2) 0.70622(12) 0.6909(4) 0.0244(6) Uani 1 1 d . . . H17 H 0.7755 0.7213 0.5934 0.029 Uiso 1 1 calc R . . C18 C 0.8929(2) 0.72398(12) 0.7686(4) 0.0245(6) Uani 1 1 d . . . H18 H 0.9250 0.7516 0.7247 0.029 Uiso 1 1 calc R . . C19 C 0.7967(2) 0.64481(12) 0.8982(4) 0.0246(6) Uani 1 1 d . . . H19 H 0.7636 0.6179 0.9436 0.030 Uiso 1 1 calc R . . C20 C 0.8864(2) 0.66210(13) 0.9751(4) 0.0249(6) Uani 1 1 d . . . H20 H 0.9142 0.6469 1.0725 0.030 Uiso 1 1 calc R . . C21 C 0.9361(2) 0.70168(12) 0.9109(4) 0.0224(6) Uani 1 1 d . . . C22 C 1.0338(2) 0.71920(12) 0.9897(4) 0.0236(6) Uani 1 1 d . . . C23 C 1.0990(2) 0.68321(13) 1.0711(4) 0.0318(7) Uani 1 1 d . . . H23 H 1.0802 0.6475 1.0773 0.038 Uiso 1 1 calc R . . C24 C 1.1910(2) 0.69879(14) 1.1432(4) 0.0343(8) Uani 1 1 d . . . H24 H 1.2345 0.6736 1.1972 0.041 Uiso 1 1 calc R . . C25 C 1.0635(2) 0.77136(13) 0.9842(4) 0.0266(6) Uani 1 1 d . . . H25 H 1.0204 0.7965 0.9289 0.032 Uiso 1 1 calc R . . C26 C 1.1549(2) 0.78712(12) 1.0579(4) 0.0283(7) Uani 1 1 d . . . H26 H 1.1731 0.8230 1.0541 0.034 Uiso 1 1 calc R . . C27 C 1.2201(2) 0.75098(12) 1.1372(4) 0.0244(6) Uani 1 1 d . . . C28 C 1.3181(2) 0.76657(12) 1.2140(4) 0.0246(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0108(2) 0.0191(3) 0.0086(2) -0.00155(18) -0.00150(17) 0.00192(18) Co2 0.01213(17) 0.01830(19) 0.01101(17) -0.00072(13) -0.00121(13) 0.00145(13) Co3 0.01701(19) 0.01741(19) 0.01599(19) -0.00015(14) -0.00053(14) 0.00025(14) F1 0.0228(8) 0.0225(8) 0.0175(8) -0.0015(6) 0.0006(7) 0.0011(7) O90 0.0206(10) 0.0238(11) 0.0183(10) -0.0017(8) -0.0014(8) 0.0048(8) O91 0.0233(11) 0.0219(11) 0.0213(11) -0.0036(8) 0.0024(8) 0.0048(8) O92 0.0302(13) 0.0330(13) 0.0325(13) -0.0034(10) -0.0021(10) -0.0064(10) O93 0.065(2) 0.0554(19) 0.0546(19) 0.0037(15) 0.0095(16) -0.0069(16) N1 0.0154(11) 0.0223(12) 0.0141(11) -0.0004(9) -0.0005(9) 0.0024(9) N2 0.0177(11) 0.0220(12) 0.0155(11) 0.0004(9) 0.0017(9) 0.0030(9) N3 0.0170(11) 0.0253(12) 0.0156(11) -0.0016(9) -0.0015(9) -0.0012(9) N4 0.0123(10) 0.0222(12) 0.0143(11) -0.0012(9) -0.0008(8) 0.0028(9) N5 0.0159(11) 0.0215(12) 0.0117(10) -0.0022(8) -0.0002(9) 0.0023(9) N6 0.0150(11) 0.0204(11) 0.0133(10) -0.0016(9) 0.0001(8) 0.0020(9) N7 0.0128(10) 0.0243(12) 0.0133(11) -0.0013(9) 0.0000(8) 0.0006(9) N8 0.0136(11) 0.0359(14) 0.0144(11) -0.0022(10) -0.0021(9) 0.0069(10) N9 0.0151(11) 0.0237(12) 0.0164(11) 0.0000(9) 0.0010(9) -0.0001(9) N10 0.0184(12) 0.0271(13) 0.0170(11) 0.0001(10) 0.0022(9) -0.0030(10) N11 0.0221(13) 0.0317(14) 0.0208(12) -0.0029(10) 0.0045(10) -0.0054(11) N12 0.0164(11) 0.0214(12) 0.0181(11) -0.0008(9) -0.0002(9) -0.0023(9) N13 0.0172(12) 0.0217(12) 0.0246(13) -0.0015(10) -0.0021(10) -0.0022(9) N14 0.0198(12) 0.0224(12) 0.0269(13) -0.0020(10) -0.0004(10) 0.0002(10) N15 0.0236(14) 0.0259(14) 0.0538(19) -0.0113(13) -0.0022(13) 0.0013(11) N16 0.0213(13) 0.0244(14) 0.0548(19) -0.0121(13) -0.0035(13) -0.0010(11) C1 0.0133(12) 0.0232(14) 0.0144(12) -0.0039(10) 0.0009(10) 0.0016(10) C2 0.0135(12) 0.0267(15) 0.0139(12) -0.0030(10) -0.0010(10) 0.0010(10) C3 0.0191(14) 0.0247(15) 0.0211(14) -0.0029(11) -0.0034(11) -0.0020(11) C4 0.0194(14) 0.0253(15) 0.0241(15) 0.0024(12) -0.0067(12) 0.0000(11) C5 0.0199(14) 0.0230(14) 0.0222(14) -0.0018(11) -0.0052(11) 0.0021(11) C6 0.0191(14) 0.0246(15) 0.0255(15) -0.0044(12) -0.0061(12) -0.0002(11) C7 0.0138(12) 0.0264(15) 0.0188(13) -0.0015(11) -0.0033(10) 0.0014(11) C8 0.0163(13) 0.0270(15) 0.0160(13) -0.0048(11) -0.0042(10) 0.0044(11) C9 0.0322(18) 0.0250(16) 0.0396(19) 0.0023(14) -0.0189(15) -0.0045(13) C10 0.0301(17) 0.0262(16) 0.0377(19) 0.0054(14) -0.0170(14) 0.0013(13) C11 0.0255(16) 0.0403(19) 0.0252(16) 0.0135(14) -0.0073(13) -0.0041(14) C12 0.0211(15) 0.0429(19) 0.0283(17) 0.0113(14) -0.0085(13) -0.0106(14) C13 0.0131(12) 0.0288(15) 0.0139(12) -0.0044(11) -0.0002(10) 0.0042(11) C14 0.0132(12) 0.0232(14) 0.0147(13) -0.0015(10) 0.0003(10) -0.0012(10) C15 0.0171(13) 0.0251(15) 0.0212(14) -0.0007(11) 0.0025(11) -0.0011(11) C16 0.0170(13) 0.0265(15) 0.0228(14) -0.0034(11) 0.0034(11) -0.0021(11) C17 0.0204(14) 0.0285(16) 0.0232(15) 0.0021(12) 0.0013(12) -0.0007(12) C18 0.0218(14) 0.0269(15) 0.0254(15) -0.0021(12) 0.0061(12) -0.0049(12) C19 0.0198(14) 0.0277(16) 0.0265(15) 0.0015(12) 0.0043(12) -0.0036(12) C20 0.0206(14) 0.0308(16) 0.0225(15) -0.0004(12) 0.0015(12) -0.0013(12) C21 0.0177(13) 0.0250(15) 0.0240(15) -0.0063(12) 0.0022(11) -0.0029(11) C22 0.0170(13) 0.0278(15) 0.0259(15) -0.0043(12) 0.0035(11) -0.0027(11) C23 0.0238(16) 0.0224(16) 0.046(2) -0.0003(14) -0.0028(14) -0.0065(12) C24 0.0229(16) 0.0296(17) 0.046(2) 0.0010(15) -0.0052(14) -0.0002(13) C25 0.0195(14) 0.0274(16) 0.0314(17) -0.0015(13) 0.0001(12) 0.0018(12) C26 0.0223(15) 0.0216(15) 0.0400(19) -0.0039(13) 0.0029(13) -0.0034(12) C27 0.0168(14) 0.0253(15) 0.0299(16) -0.0052(12) 0.0004(12) -0.0037(11) C28 0.0198(14) 0.0222(15) 0.0304(16) -0.0030(12) 0.0010(12) -0.0004(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 2.056(2) 3_667 ? Co1 N1 2.056(2) . ? Co1 F1 2.064(2) 3_667 ? Co1 F1 2.064(2) . ? Co1 N5 2.132(2) 3_566 ? Co1 N5 2.132(2) 1_656 ? Co2 O90 2.073(2) . ? Co2 N7 2.090(2) 3_565 ? Co2 F1 2.107(2) . ? Co2 N9 2.147(2) . ? Co2 N6 2.151(2) 1_656 ? Co2 N4 2.210(2) . ? Co3 O92 2.050(2) . ? Co3 F1 2.082(2) . ? Co3 O91 2.133(2) . ? Co3 N14 2.162(3) 4_475 ? Co3 N2 2.174(2) 3_667 ? Co3 N12 2.176(2) . ? N1 N2 1.311(3) . ? N1 N4 1.351(3) . ? N2 N3 1.343(3) . ? N2 Co3 2.174(2) 3_667 ? N3 C1 1.334(4) . ? N4 C1 1.348(4) . ? N5 C14 1.326(3) . ? N5 N6 1.343(3) . ? N5 Co1 2.132(2) 1_454 ? N6 N7 1.308(3) . ? N6 Co2 2.151(2) 1_454 ? N7 N8 1.345(3) . ? N7 Co2 2.090(2) 3_565 ? N8 C14 1.332(4) . ? N9 N10 1.310(3) . ? N9 N12 1.357(3) . ? N10 N11 1.344(3) . ? N11 C15 1.337(4) . ? N12 C15 1.339(4) . ? N13 C28 1.333(4) . ? N13 N14 1.338(3) . ? N14 N15 1.313(4) . ? N14 Co3 2.162(3) 4_676 ? N15 N16 1.342(4) . ? N16 C28 1.334(4) . ? C1 C2 1.473(4) . ? C2 C3 1.390(4) . ? C2 C5 1.396(4) . ? C3 C4 1.384(4) . ? C3 H3 0.9500 . ? C4 C7 1.402(4) . ? C4 H4 0.9500 . ? C5 C6 1.390(4) . ? C5 H5 0.9500 . ? C6 C7 1.391(4) . ? C6 H6 0.9500 . ? C7 C8 1.490(4) . ? C8 C11 1.380(4) . ? C8 C9 1.392(4) . ? C9 C10 1.388(4) . ? C9 H9 0.9500 . ? C10 C13 1.379(4) . ? C10 H10 0.9500 . ? C11 C12 1.397(4) . ? C11 H11 0.9500 . ? C12 C13 1.368(4) . ? C12 H12 0.9500 . ? C13 C14 1.486(4) . ? C15 C16 1.472(4) . ? C16 C19 1.386(4) . ? C16 C17 1.398(4) . ? C17 C18 1.388(4) . ? C17 H17 0.9500 . ? C18 C21 1.398(4) . ? C18 H18 0.9500 . ? C19 C20 1.386(4) . ? C19 H19 0.9500 . ? C20 C21 1.396(4) . ? C20 H20 0.9500 . ? C21 C22 1.486(4) . ? C22 C25 1.393(4) . ? C22 C23 1.395(5) . ? C23 C24 1.387(4) . ? C23 H23 0.9500 . ? C24 C27 1.391(4) . ? C24 H24 0.9500 . ? C25 C26 1.386(4) . ? C25 H25 0.9500 . ? C26 C27 1.390(4) . ? C26 H26 0.9500 . ? C27 C28 1.470(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N1 180.00(11) 3_667 . ? N1 Co1 F1 87.38(8) 3_667 3_667 ? N1 Co1 F1 92.62(8) . 3_667 ? N1 Co1 F1 92.62(8) 3_667 . ? N1 Co1 F1 87.38(8) . . ? F1 Co1 F1 180.00(9) 3_667 . ? N1 Co1 N5 88.96(9) 3_667 3_566 ? N1 Co1 N5 91.04(9) . 3_566 ? F1 Co1 N5 85.73(8) 3_667 3_566 ? F1 Co1 N5 94.27(8) . 3_566 ? N1 Co1 N5 91.04(9) 3_667 1_656 ? N1 Co1 N5 88.96(9) . 1_656 ? F1 Co1 N5 94.27(8) 3_667 1_656 ? F1 Co1 N5 85.73(8) . 1_656 ? N5 Co1 N5 180.0 3_566 1_656 ? O90 Co2 N7 86.28(8) . 3_565 ? O90 Co2 F1 90.31(7) . . ? N7 Co2 F1 173.88(8) 3_565 . ? O90 Co2 N9 93.53(9) . . ? N7 Co2 N9 92.18(9) 3_565 . ? F1 Co2 N9 82.95(8) . . ? O90 Co2 N6 178.44(9) . 1_656 ? N7 Co2 N6 95.04(9) 3_565 1_656 ? F1 Co2 N6 88.30(8) . 1_656 ? N9 Co2 N6 85.59(9) . 1_656 ? O90 Co2 N4 92.70(8) . . ? N7 Co2 N4 98.44(9) 3_565 . ? F1 Co2 N4 86.79(7) . . ? N9 Co2 N4 168.01(9) . . ? N6 Co2 N4 87.93(9) 1_656 . ? O92 Co3 F1 175.65(9) . . ? O92 Co3 O91 94.04(9) . . ? F1 Co3 O91 88.58(7) . . ? O92 Co3 N14 88.32(10) . 4_475 ? F1 Co3 N14 95.21(8) . 4_475 ? O91 Co3 N14 89.07(9) . 4_475 ? O92 Co3 N2 86.12(10) . 3_667 ? F1 Co3 N2 90.74(8) . 3_667 ? O91 Co3 N2 83.32(8) . 3_667 ? N14 Co3 N2 170.23(9) 4_475 3_667 ? O92 Co3 N12 94.37(9) . . ? F1 Co3 N12 83.25(8) . . ? O91 Co3 N12 170.81(9) . . ? N14 Co3 N12 87.48(9) 4_475 . ? N2 Co3 N12 100.95(9) 3_667 . ? Co1 F1 Co3 113.48(8) . . ? Co1 F1 Co2 104.87(7) . . ? Co3 F1 Co2 122.93(8) . . ? N2 N1 N4 110.1(2) . . ? N2 N1 Co1 120.99(17) . . ? N4 N1 Co1 127.71(18) . . ? N1 N2 N3 109.4(2) . . ? N1 N2 Co3 116.20(17) . 3_667 ? N3 N2 Co3 131.51(19) . 3_667 ? C1 N3 N2 105.0(2) . . ? C1 N4 N1 103.7(2) . . ? C1 N4 Co2 149.60(19) . . ? N1 N4 Co2 104.36(16) . . ? C14 N5 N6 105.7(2) . . ? C14 N5 Co1 138.32(19) . 1_454 ? N6 N5 Co1 112.12(16) . 1_454 ? N7 N6 N5 108.7(2) . . ? N7 N6 Co2 132.41(18) . 1_454 ? N5 N6 Co2 117.21(17) . 1_454 ? N6 N7 N8 109.7(2) . . ? N6 N7 Co2 130.38(18) . 3_565 ? N8 N7 Co2 119.69(17) . 3_565 ? C14 N8 N7 104.8(2) . . ? N10 N9 N12 109.8(2) . . ? N10 N9 Co2 125.62(18) . . ? N12 N9 Co2 121.62(17) . . ? N9 N10 N11 108.8(2) . . ? C15 N11 N10 105.9(2) . . ? C15 N12 N9 104.7(2) . . ? C15 N12 Co3 134.1(2) . . ? N9 N12 Co3 114.86(17) . . ? C28 N13 N14 104.9(2) . . ? N15 N14 N13 109.4(2) . . ? N15 N14 Co3 119.5(2) . 4_676 ? N13 N14 Co3 131.06(19) . 4_676 ? N14 N15 N16 109.6(3) . . ? C28 N16 N15 104.5(3) . . ? N3 C1 N4 111.8(2) . . ? N3 C1 C2 122.4(3) . . ? N4 C1 C2 125.8(3) . . ? C3 C2 C5 118.6(3) . . ? C3 C2 C1 121.3(3) . . ? C5 C2 C1 120.0(3) . . ? C4 C3 C2 120.7(3) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C7 121.3(3) . . ? C3 C4 H4 119.3 . . ? C7 C4 H4 119.3 . . ? C6 C5 C2 120.3(3) . . ? C6 C5 H5 119.8 . . ? C2 C5 H5 119.8 . . ? C5 C6 C7 121.6(3) . . ? C5 C6 H6 119.2 . . ? C7 C6 H6 119.2 . . ? C6 C7 C4 117.5(3) . . ? C6 C7 C8 121.5(3) . . ? C4 C7 C8 121.0(3) . . ? C11 C8 C9 117.1(3) . . ? C11 C8 C7 122.0(3) . . ? C9 C8 C7 120.9(3) . . ? C10 C9 C8 121.1(3) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C13 C10 C9 120.7(3) . . ? C13 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C8 C11 C12 121.9(3) . . ? C8 C11 H11 119.0 . . ? C12 C11 H11 119.0 . . ? C13 C12 C11 120.0(3) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C10 119.1(3) . . ? C12 C13 C14 123.9(3) . . ? C10 C13 C14 116.9(3) . . ? N5 C14 N8 111.1(2) . . ? N5 C14 C13 125.6(2) . . ? N8 C14 C13 122.9(2) . . ? N11 C15 N12 110.8(3) . . ? N11 C15 C16 123.5(3) . . ? N12 C15 C16 125.6(3) . . ? C19 C16 C17 119.1(3) . . ? C19 C16 C15 120.0(3) . . ? C17 C16 C15 120.8(3) . . ? C18 C17 C16 120.2(3) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C21 120.7(3) . . ? C17 C18 H18 119.6 . . ? C21 C18 H18 119.6 . . ? C16 C19 C20 120.7(3) . . ? C16 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C19 C20 C21 120.6(3) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C20 C21 C18 118.6(3) . . ? C20 C21 C22 121.0(3) . . ? C18 C21 C22 120.4(3) . . ? C25 C22 C23 117.9(3) . . ? C25 C22 C21 121.7(3) . . ? C23 C22 C21 120.3(3) . . ? C24 C23 C22 121.0(3) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C23 C24 C27 120.7(3) . . ? C23 C24 H24 119.6 . . ? C27 C24 H24 119.6 . . ? C26 C25 C22 121.1(3) . . ? C26 C25 H25 119.4 . . ? C22 C25 H25 119.4 . . ? C25 C26 C27 120.7(3) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C26 C27 C24 118.5(3) . . ? C26 C27 C28 121.8(3) . . ? C24 C27 C28 119.8(3) . . ? N13 C28 N16 111.6(3) . . ? N13 C28 C27 125.7(3) . . ? N16 C28 C27 122.7(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Co1 F1 Co3 4.00(10) 3_667 . . . ? N1 Co1 F1 Co3 -176.00(10) . . . . ? N5 Co1 F1 Co3 93.15(9) 3_566 . . . ? N1 Co1 F1 Co2 140.76(9) 3_667 . . . ? N1 Co1 F1 Co2 -39.24(9) . . . . ? N5 Co1 F1 Co2 -130.09(8) 3_566 . . . ? N5 Co1 F1 Co2 49.91(8) 1_656 . . . ? O91 Co3 F1 Co1 -77.59(9) . . . . ? N14 Co3 F1 Co1 -166.53(10) 4_475 . . . ? N2 Co3 F1 Co1 5.71(9) 3_667 . . . ? N12 Co3 F1 Co1 106.64(9) . . . . ? O91 Co3 F1 Co2 154.48(10) . . . . ? N14 Co3 F1 Co2 65.54(11) 4_475 . . . ? N2 Co3 F1 Co2 -122.22(10) 3_667 . . . ? N12 Co3 F1 Co2 -21.29(10) . . . . ? O90 Co2 F1 Co1 142.25(8) . . . . ? N9 Co2 F1 Co1 -124.23(9) . . . . ? N6 Co2 F1 Co1 -38.46(9) 1_656 . . . ? N4 Co2 F1 Co1 49.56(8) . . . . ? O90 Co2 F1 Co3 -86.22(10) . . . . ? N9 Co2 F1 Co3 7.30(10) . . . . ? N6 Co2 F1 Co3 93.07(11) 1_656 . . . ? N4 Co2 F1 Co3 -178.90(10) . . . . ? F1 Co1 N1 N2 21.4(2) 3_667 . . . ? F1 Co1 N1 N2 -158.6(2) . . . . ? N5 Co1 N1 N2 -64.3(2) 3_566 . . . ? N5 Co1 N1 N2 115.7(2) 1_656 . . . ? F1 Co1 N1 N4 -172.2(2) 3_667 . . . ? F1 Co1 N1 N4 7.8(2) . . . . ? N5 Co1 N1 N4 102.0(2) 3_566 . . . ? N5 Co1 N1 N4 -78.0(2) 1_656 . . . ? N4 N1 N2 N3 -1.1(3) . . . . ? Co1 N1 N2 N3 167.44(17) . . . . ? N4 N1 N2 Co3 161.88(16) . . . 3_667 ? Co1 N1 N2 Co3 -29.6(2) . . . 3_667 ? N1 N2 N3 C1 0.0(3) . . . . ? Co3 N2 N3 C1 -159.39(19) 3_667 . . . ? N2 N1 N4 C1 1.6(3) . . . . ? Co1 N1 N4 C1 -165.92(18) . . . . ? N2 N1 N4 Co2 -166.57(17) . . . . ? Co1 N1 N4 Co2 25.9(2) . . . . ? O90 Co2 N4 C1 68.5(4) . . . . ? N7 Co2 N4 C1 -18.1(4) 3_565 . . . ? F1 Co2 N4 C1 158.7(4) . . . . ? N9 Co2 N4 C1 -170.2(4) . . . . ? N6 Co2 N4 C1 -112.9(4) 1_656 . . . ? O90 Co2 N4 N1 -134.64(16) . . . . ? N7 Co2 N4 N1 138.72(16) 3_565 . . . ? F1 Co2 N4 N1 -44.48(16) . . . . ? N9 Co2 N4 N1 -13.4(5) . . . . ? N6 Co2 N4 N1 43.93(16) 1_656 . . . ? C14 N5 N6 N7 0.9(3) . . . . ? Co1 N5 N6 N7 -161.18(17) 1_454 . . . ? C14 N5 N6 Co2 -166.15(18) . . . 1_454 ? Co1 N5 N6 Co2 31.8(2) 1_454 . . 1_454 ? N5 N6 N7 N8 0.4(3) . . . . ? Co2 N6 N7 N8 164.7(2) 1_454 . . . ? N5 N6 N7 Co2 174.62(18) . . . 3_565 ? Co2 N6 N7 Co2 -21.1(4) 1_454 . . 3_565 ? N6 N7 N8 C14 -1.4(3) . . . . ? Co2 N7 N8 C14 -176.40(18) 3_565 . . . ? O90 Co2 N9 N10 -89.1(2) . . . . ? N7 Co2 N9 N10 -2.7(2) 3_565 . . . ? F1 Co2 N9 N10 -179.0(2) . . . . ? N6 Co2 N9 N10 92.2(2) 1_656 . . . ? N4 Co2 N9 N10 149.7(4) . . . . ? O90 Co2 N9 N12 112.5(2) . . . . ? N7 Co2 N9 N12 -161.1(2) 3_565 . . . ? F1 Co2 N9 N12 22.6(2) . . . . ? N6 Co2 N9 N12 -66.2(2) 1_656 . . . ? N4 Co2 N9 N12 -8.7(5) . . . . ? N12 N9 N10 N11 0.2(3) . . . . ? Co2 N9 N10 N11 -160.30(19) . . . . ? N9 N10 N11 C15 0.6(3) . . . . ? N10 N9 N12 C15 -0.9(3) . . . . ? Co2 N9 N12 C15 160.51(19) . . . . ? N10 N9 N12 Co3 155.07(18) . . . . ? Co2 N9 N12 Co3 -43.5(2) . . . . ? O92 Co3 N12 C15 -0.7(3) . . . . ? F1 Co3 N12 C15 -177.0(3) . . . . ? N14 Co3 N12 C15 87.4(3) 4_475 . . . ? N2 Co3 N12 C15 -87.6(3) 3_667 . . . ? O92 Co3 N12 N9 -147.52(19) . . . . ? F1 Co3 N12 N9 36.15(18) . . . . ? N14 Co3 N12 N9 -59.40(19) 4_475 . . . ? N2 Co3 N12 N9 125.60(19) 3_667 . . . ? C28 N13 N14 N15 1.4(3) . . . . ? C28 N13 N14 Co3 -175.0(2) . . . 4_676 ? N13 N14 N15 N16 -1.4(4) . . . . ? Co3 N14 N15 N16 175.5(2) 4_676 . . . ? N14 N15 N16 C28 0.8(4) . . . . ? N2 N3 C1 N4 1.0(3) . . . . ? N2 N3 C1 C2 -177.2(2) . . . . ? N1 N4 C1 N3 -1.6(3) . . . . ? Co2 N4 C1 N3 155.3(3) . . . . ? N1 N4 C1 C2 176.5(2) . . . . ? Co2 N4 C1 C2 -26.6(5) . . . . ? N3 C1 C2 C3 157.2(3) . . . . ? N4 C1 C2 C3 -20.8(4) . . . . ? N3 C1 C2 C5 -19.2(4) . . . . ? N4 C1 C2 C5 162.8(3) . . . . ? C5 C2 C3 C4 -0.5(4) . . . . ? C1 C2 C3 C4 -176.9(3) . . . . ? C2 C3 C4 C7 0.4(5) . . . . ? C3 C2 C5 C6 0.9(4) . . . . ? C1 C2 C5 C6 177.4(3) . . . . ? C2 C5 C6 C7 -1.2(5) . . . . ? C5 C6 C7 C4 1.1(5) . . . . ? C5 C6 C7 C8 -178.1(3) . . . . ? C3 C4 C7 C6 -0.7(5) . . . . ? C3 C4 C7 C8 178.5(3) . . . . ? C6 C7 C8 C11 19.4(5) . . . . ? C4 C7 C8 C11 -159.8(3) . . . . ? C6 C7 C8 C9 -161.5(3) . . . . ? C4 C7 C8 C9 19.4(5) . . . . ? C11 C8 C9 C10 -2.7(5) . . . . ? C7 C8 C9 C10 178.1(3) . . . . ? C8 C9 C10 C13 1.7(6) . . . . ? C9 C8 C11 C12 1.6(5) . . . . ? C7 C8 C11 C12 -179.2(3) . . . . ? C8 C11 C12 C13 0.6(6) . . . . ? C11 C12 C13 C10 -1.7(5) . . . . ? C11 C12 C13 C14 176.0(3) . . . . ? C9 C10 C13 C12 0.6(5) . . . . ? C9 C10 C13 C14 -177.2(3) . . . . ? N6 N5 C14 N8 -1.8(3) . . . . ? Co1 N5 C14 N8 152.8(2) 1_454 . . . ? N6 N5 C14 C13 170.5(3) . . . . ? Co1 N5 C14 C13 -34.9(5) 1_454 . . . ? N7 N8 C14 N5 2.0(3) . . . . ? N7 N8 C14 C13 -170.6(3) . . . . ? C12 C13 C14 N5 92.0(4) . . . . ? C10 C13 C14 N5 -90.3(4) . . . . ? C12 C13 C14 N8 -96.5(4) . . . . ? C10 C13 C14 N8 81.2(4) . . . . ? N10 N11 C15 N12 -1.2(3) . . . . ? N10 N11 C15 C16 174.4(3) . . . . ? N9 N12 C15 N11 1.3(3) . . . . ? Co3 N12 C15 N11 -147.8(2) . . . . ? N9 N12 C15 C16 -174.2(3) . . . . ? Co3 N12 C15 C16 36.7(5) . . . . ? N11 C15 C16 C19 -148.2(3) . . . . ? N12 C15 C16 C19 26.7(5) . . . . ? N11 C15 C16 C17 29.1(5) . . . . ? N12 C15 C16 C17 -156.0(3) . . . . ? C19 C16 C17 C18 0.1(5) . . . . ? C15 C16 C17 C18 -177.2(3) . . . . ? C16 C17 C18 C21 1.2(5) . . . . ? C17 C16 C19 C20 -0.8(5) . . . . ? C15 C16 C19 C20 176.6(3) . . . . ? C16 C19 C20 C21 0.3(5) . . . . ? C19 C20 C21 C18 0.9(5) . . . . ? C19 C20 C21 C22 -177.9(3) . . . . ? C17 C18 C21 C20 -1.6(5) . . . . ? C17 C18 C21 C22 177.2(3) . . . . ? C20 C21 C22 C25 -145.7(3) . . . . ? C18 C21 C22 C25 35.5(4) . . . . ? C20 C21 C22 C23 34.8(4) . . . . ? C18 C21 C22 C23 -144.0(3) . . . . ? C25 C22 C23 C24 -0.5(5) . . . . ? C21 C22 C23 C24 179.0(3) . . . . ? C22 C23 C24 C27 0.6(6) . . . . ? C23 C22 C25 C26 -0.3(5) . . . . ? C21 C22 C25 C26 -179.8(3) . . . . ? C22 C25 C26 C27 1.2(5) . . . . ? C25 C26 C27 C24 -1.1(5) . . . . ? C25 C26 C27 C28 178.9(3) . . . . ? C23 C24 C27 C26 0.2(5) . . . . ? C23 C24 C27 C28 -179.8(3) . . . . ? N14 N13 C28 N16 -0.9(4) . . . . ? N14 N13 C28 C27 178.1(3) . . . . ? N15 N16 C28 N13 0.1(4) . . . . ? N15 N16 C28 C27 -178.9(3) . . . . ? C26 C27 C28 N13 23.4(5) . . . . ? C24 C27 C28 N13 -156.7(3) . . . . ? C26 C27 C28 N16 -157.7(3) . . . . ? C24 C27 C28 N16 22.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.08 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.812 _refine_diff_density_min -1.049 _refine_diff_density_rms 0.104 #### data_cmmm #[Ni2(H0.67bdt)3]\/Y10.5H2O (4\/Y10.5H2O). _database_code_depnum_ccdc_archive 'CCDC 826920' #TrackingRef '- AllCIFsDT-ART-05-2011-010984.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C3 H1.75 N3 Ni0.25, 1.31(H2 O)' _chemical_formula_sum 'C3 H4.38 N3 Ni0.25 O1.31' _chemical_formula_weight 118.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C m m m' _symmetry_space_group_name_Hall '-C 2 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' _cell_length_a 7.5423(9) _cell_length_b 26.318(3) _cell_length_c 12.5387(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2488.9(5) _cell_formula_units_Z 16 _cell_measurement_temperature 98(2) _cell_measurement_reflns_used 1324 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 28.27 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 1.23(2) _exptl_crystal_density_diffrn 1.261 _exptl_crystal_density_method flotation _exptl_crystal_F_000 974 _exptl_absorpt_coefficient_mu 0.824 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8526 _exptl_absorpt_correction_T_max 0.9222 _exptl_absorpt_process_details 'SADABS (Bruker, 1998)' _exptl_special_details ; In this X-ray diffraction analysis, there were several residual peaks within the void from Fourier difference map. However, the highly disordered solvents within the void could not be crystallographically defined. ; _diffrn_ambient_temperature 98(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_reflns_number 12789 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 27.97 _reflns_number_total 1699 _reflns_number_gt 1455 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'CrystalMaker (Palmer, 2006)' _computing_publication_material 'Bruker SHELXTL (Sheldrick, 2008)' _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^)+(0.0667P)^2^+8.0323P] 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 1699 _refine_ls_number_parameters 77 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0690 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.1374 _refine_ls_wR_factor_gt 0.1319 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 # SQUEEZE RESULTS _platon_squeeze_details ; Although there were several peaks within the void from Fourier difference map, the highly disordered solvents within the void were not crystallographically well defined. The SQUEEZE routine of the program PLATON was used in order to eliminate the contribution of disordered solvents molecules, thereby a final model based only on the ordered part of the crystal structure was obtained. The SQUEEZE routine suggested that a total potential solvent area volume of 625.1 Ang^3^[25.1% of cell volume], and a void electron population of 106 per cell. Refinement after the SQUEEZE routine gave significantly improved R values. [R values before SQUEEZE] R1 = 0.131 for >2sigma(I) data R1 = 0.148 , wR2 = 0.270, GooF = S = 1.83 for all data ( 1699 data and 0 restraint / 77 parameters) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.071 0.000 -0.003 625.1 105.5 2 -0.055 0.500 0.043 625.1 105.5 _platon_squeeze_details ? ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.2500 0.2500 0.5000 0.0066(2) Uani 1 4 d S . . N1 N 0.0882(4) 0.31474(11) 0.5000 0.0063(6) Uani 1 2 d S . . N2 N 0.1473(4) 0.36254(11) 0.5000 0.0102(6) Uani 1 2 d S . . N3 N 0.0879(3) 0.21602(8) 0.38054(16) 0.0065(4) Uani 1 1 d . . . N4 N 0.1469(3) 0.20064(8) 0.28547(16) 0.0076(4) Uani 1 1 d . . . H4 H 0.2604 0.1967 0.2650 0.009 Uiso 0.25 1 d PR . . C1 C 0.0000 0.39128(19) 0.5000 0.0100(10) Uani 1 4 d S . . C2 C 0.0000 0.4473(2) 0.5000 0.0151(11) Uani 1 4 d S . . C3 C 0.1414(9) 0.4732(2) 0.4588(6) 0.0342(19) Uani 0.50 1 d P . . H3 H 0.2359 0.4544 0.4193 0.041 Uiso 0.50 1 calc PR . . C4 C 0.0000 0.19229(13) 0.2267(3) 0.0076(6) Uani 1 2 d S . . C5 C 0.0000 0.18296(14) 0.1121(3) 0.0094(7) Uani 1 2 d S . . C6 C 0.1586(4) 0.18127(17) 0.0549(2) 0.0299(9) Uani 1 1 d . . . H6 H 0.249(7) 0.181(2) 0.088(4) 0.056(15) 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 Ni1 0.0016(3) 0.0098(3) 0.0082(3) 0.000 0.000 0.0002(2) N1 0.0020(14) 0.0085(14) 0.0085(13) 0.000 0.000 0.0002(11) N2 0.0039(14) 0.0080(14) 0.0187(16) 0.000 0.000 0.0009(11) N3 0.0007(10) 0.0117(9) 0.0070(9) -0.0004(8) 0.0005(7) -0.0005(8) N4 0.0034(10) 0.0071(10) 0.0063(9) -0.0027(8) 0.0000(8) -0.0016(7) C1 0.003(2) 0.009(2) 0.018(3) 0.000 0.000 0.000 C2 0.004(2) 0.008(2) 0.034(3) 0.000 0.000 0.000 C3 0.015(3) 0.012(3) 0.076(6) 0.000(3) 0.020(3) 0.002(2) C4 0.0042(15) 0.0129(16) 0.0057(15) 0.0011(12) 0.000 0.000 C5 0.0062(16) 0.0154(17) 0.0065(16) -0.0024(13) 0.000 0.000 C6 0.0022(14) 0.058(3) 0.0092(14) 0.0005(15) -0.0027(10) 0.0085(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.096(3) . ? Ni1 N1 2.096(3) 13_556 ? Ni1 N3 2.130(2) . ? Ni1 N3 2.130(2) 13_556 ? Ni1 N3 2.130(2) 10_556 ? Ni1 N3 2.130(2) 6 ? N1 N1 1.330(6) 3_556 ? N1 N2 1.335(4) . ? N2 C1 1.344(4) . ? N3 N3 1.326(4) 12 ? N3 N4 1.335(3) . ? N4 C4 1.348(3) . ? C1 N2 1.344(4) 3_556 ? C1 C2 1.476(7) . ? C2 C3 1.367(7) 10_556 ? C2 C3 1.367(7) 3_556 ? C3 C3 1.409(12) 11_565 ? C4 N4 1.348(3) 12 ? C4 C5 1.459(5) . ? C5 C6 1.395(3) 12 ? C5 C6 1.395(3) . ? C6 C6 1.377(6) 10 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N1 180.00(15) . 13_556 ? N1 Ni1 N3 90.41(8) . . ? N1 Ni1 N3 89.59(8) 13_556 . ? N1 Ni1 N3 89.59(8) . 13_556 ? N1 Ni1 N3 90.41(8) 13_556 13_556 ? N3 Ni1 N3 180.0 . 13_556 ? N1 Ni1 N3 90.41(8) . 10_556 ? N1 Ni1 N3 89.59(8) 13_556 10_556 ? N3 Ni1 N3 89.36(11) . 10_556 ? N3 Ni1 N3 90.64(11) 13_556 10_556 ? N1 Ni1 N3 89.59(8) . 6 ? N1 Ni1 N3 90.41(8) 13_556 6 ? N3 Ni1 N3 90.64(11) . 6 ? N3 Ni1 N3 89.36(11) 13_556 6 ? N3 Ni1 N3 180.00(10) 10_556 6 ? N1 N1 N2 109.52(18) 3_556 . ? N1 N1 Ni1 125.61(8) 3_556 . ? N2 N1 Ni1 124.9(2) . . ? N1 N2 C1 104.7(3) . . ? N3 N3 N4 109.46(12) 12 . ? N3 N3 Ni1 125.03(5) 12 . ? N4 N3 Ni1 124.32(15) . . ? N3 N4 C4 105.3(2) . . ? N2 C1 N2 111.5(5) . 3_556 ? N2 C1 C2 124.2(2) . . ? C3 C2 C3 120.2(7) 3_556 . ? C3 C2 C1 119.9(3) 10_556 . ? C2 C3 C3 119.9(3) . 11_565 ? N4 C4 C5 124.46(15) . . ? C6 C5 C6 118.0(3) 12 . ? C6 C5 C4 120.78(18) 12 . ? C6 C5 C4 120.78(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Ni1 N1 N1 44.68(5) . . . 3_556 ? N3 Ni1 N1 N1 -135.32(5) 13_556 . . 3_556 ? N3 Ni1 N1 N1 -44.68(5) 10_556 . . 3_556 ? N3 Ni1 N1 N1 135.32(5) 6 . . 3_556 ? N3 Ni1 N1 N2 -135.32(5) . . . . ? N3 Ni1 N1 N2 44.68(5) 13_556 . . . ? N3 Ni1 N1 N2 135.32(5) 10_556 . . . ? N3 Ni1 N1 N2 -44.68(5) 6 . . . ? N1 N1 N2 C1 0.0 3_556 . . . ? Ni1 N1 N2 C1 180.0 . . . . ? N1 Ni1 N3 N3 -44.28(7) . . . 12 ? N1 Ni1 N3 N3 135.72(7) 13_556 . . 12 ? N3 Ni1 N3 N3 46.13(9) 10_556 . . 12 ? N3 Ni1 N3 N3 -133.87(9) 6 . . 12 ? N1 Ni1 N3 N4 121.91(19) . . . . ? N1 Ni1 N3 N4 -58.10(19) 13_556 . . . ? N3 Ni1 N3 N4 -147.69(15) 10_556 . . . ? N3 Ni1 N3 N4 32.31(15) 6 . . . ? N3 N3 N4 C4 1.3(2) 12 . . . ? Ni1 N3 N4 C4 -166.8(2) . . . . ? N1 N2 C1 N2 0.0 . . . 3_556 ? N1 N2 C1 C2 180.0 . . . . ? N2 C1 C2 C3 -25.8(4) . . . 10_556 ? N2 C1 C2 C3 154.2(4) 3_556 . . 10_556 ? N2 C1 C2 C3 154.2(4) . . . 12 ? N2 C1 C2 C3 -25.8(4) 3_556 . . 12 ? N2 C1 C2 C3 -154.2(4) . . . 3_556 ? N2 C1 C2 C3 25.8(4) 3_556 . . 3_556 ? N2 C1 C2 C3 25.8(4) . . . . ? N2 C1 C2 C3 -154.2(4) 3_556 . . . ? C3 C2 C3 C3 120.6(5) 12 . . 10_556 ? C3 C2 C3 C3 76.4(3) 3_556 . . 10_556 ? C1 C2 C3 C3 -103.6(3) . . . 10_556 ? C3 C2 C3 C3 -76.4(3) 10_556 . . 11_565 ? C3 C2 C3 C3 44.1(6) 12 . . 11_565 ? C3 C2 C3 C3 0.000(1) 3_556 . . 11_565 ? C1 C2 C3 C3 180.000(1) . . . 11_565 ? C3 C2 C3 C3 -43.7(5) 10_556 . . 4_566 ? C3 C2 C3 C3 76.9(7) 12 . . 4_566 ? C3 C2 C3 C3 32.7(3) 3_556 . . 4_566 ? C1 C2 C3 C3 -147.3(3) . . . 4_566 ? N3 N4 C4 N4 -2.1(4) . . . 12 ? N3 N4 C4 C5 169.5(3) . . . . ? N4 C4 C5 C6 -1.1(6) 12 . . 12 ? N4 C4 C5 C6 -171.5(4) . . . 12 ? N4 C4 C5 C6 171.5(4) 12 . . . ? N4 C4 C5 C6 1.1(6) . . . . ? C6 C5 C6 C6 4.1(5) 12 . . 10 ? C4 C5 C6 C6 -168.7(2) . . . 10 ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.97 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.977 _refine_diff_density_min -0.686 _refine_diff_density_rms 0.104 ##### data_p212121 #[Zn(bdt)] (5). _database_code_depnum_ccdc_archive 'CCDC 826921' #TrackingRef '- AllCIFsDT-ART-05-2011-010984.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H4 N8 Zn' _chemical_formula_weight 277.56 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.0626(5) _cell_length_b 8.7291(6) _cell_length_c 12.9913(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 914.32(11) _cell_formula_units_Z 4 _cell_measurement_temperature 98(2) _cell_measurement_reflns_used 987 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 28.27 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 2.02(2) _exptl_crystal_density_diffrn 2.016 _exptl_crystal_density_method flotation _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 2.674 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6743 _exptl_absorpt_correction_T_max 0.8146 _exptl_absorpt_process_details 'SADABS (Bruker, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 98(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 512 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 9704 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 28.30 _reflns_number_total 1311 _reflns_number_gt 1307 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'CrystalMaker (Palmer, 2006)' _computing_publication_material 'Bruker SHELXTL (Sheldrick, 2008)' _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^)+(0.0403P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.031(15) _refine_ls_number_reflns 2281 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0307 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0699 _refine_ls_wR_factor_gt 0.0694 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 1.02208(4) 0.09000(3) 1.38149(2) 0.00874(9) Uani 1 1 d . . . N1 N 0.9204(3) 0.1851(3) 1.25458(18) 0.0100(5) Uani 1 1 d . . . N2 N 0.9425(3) 0.3333(3) 1.24790(17) 0.0117(5) Uani 1 1 d . . . N3 N 0.8857(3) 0.1215(3) 1.16190(18) 0.0118(5) Uani 1 1 d . . . N4 N 0.9230(3) 0.3721(3) 1.14887(17) 0.0099(5) Uani 1 1 d . . . N5 N 0.8935(3) 0.1502(3) 0.50596(18) 0.0112(5) Uani 1 1 d . . . N6 N 0.9361(3) 0.1173(3) 0.60406(17) 0.0118(5) Uani 1 1 d . . . N7 N 0.7737(3) 0.2504(3) 0.5010(2) 0.0119(5) Uani 1 1 d . . . N8 N 0.7332(3) 0.2870(3) 0.59832(17) 0.0104(5) Uani 1 1 d . . . C1 C 0.8878(3) 0.2406(3) 1.0980(2) 0.0095(5) Uani 1 1 d . . . C2 C 0.8645(4) 0.2286(3) 0.9864(2) 0.0096(5) Uani 1 1 d . . . C3 C 0.9074(3) 0.0928(4) 0.9348(2) 0.0120(5) Uani 1 1 d . . . H3 H 0.9455 0.0068 0.9729 0.014 Uiso 1 1 calc R . . C4 C 0.8074(4) 0.3536(3) 0.9297(2) 0.0106(6) Uani 1 1 d . . . H4 H 0.7764 0.4453 0.9641 0.013 Uiso 1 1 calc R . . C5 C 0.8945(3) 0.0839(4) 0.8288(2) 0.0126(5) Uani 1 1 d . . . H5 H 0.9228 -0.0085 0.7943 0.015 Uiso 1 1 calc R . . C6 C 0.7958(4) 0.3448(3) 0.8236(2) 0.0100(5) Uani 1 1 d . . . H6 H 0.7577 0.4308 0.7855 0.012 Uiso 1 1 calc R . . C7 C 0.8396(4) 0.2108(3) 0.7723(2) 0.0104(5) Uani 1 1 d . . . C8 C 0.8348(3) 0.2035(3) 0.6592(2) 0.0099(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01382(15) 0.00896(14) 0.00342(13) -0.00037(11) 0.00002(11) -0.00002(11) N1 0.0132(12) 0.0099(11) 0.0069(11) 0.0003(9) -0.0008(9) 0.0004(9) N2 0.0172(12) 0.0115(12) 0.0066(11) 0.0017(9) -0.0007(9) -0.0010(9) N3 0.0164(12) 0.0127(12) 0.0064(10) -0.0018(9) -0.0002(9) -0.0004(9) N4 0.0140(11) 0.0104(11) 0.0051(10) 0.0001(8) -0.0001(8) 0.0008(8) N5 0.0141(12) 0.0136(11) 0.0058(11) 0.0009(9) 0.0000(9) -0.0002(10) N6 0.0138(11) 0.0148(12) 0.0068(11) 0.0004(9) 0.0002(8) 0.0008(8) N7 0.0168(12) 0.0121(10) 0.0068(10) -0.0008(8) 0.0020(9) 0.0007(9) N8 0.0152(11) 0.0129(11) 0.0060(11) -0.0013(9) 0.0013(8) 0.0007(9) C1 0.0097(12) 0.0130(13) 0.0057(13) 0.0001(10) -0.0009(9) 0.0003(10) C2 0.0108(13) 0.0134(14) 0.0047(12) 0.0006(11) -0.0013(10) -0.0001(11) C3 0.0145(13) 0.0122(13) 0.0092(12) 0.0018(12) -0.0027(10) 0.0011(13) C4 0.0131(13) 0.0090(13) 0.0096(13) 0.0000(10) -0.0019(10) 0.0003(11) C5 0.0178(14) 0.0112(13) 0.0088(12) -0.0034(12) -0.0030(10) 0.0028(13) C6 0.0127(13) 0.0110(13) 0.0063(12) 0.0031(11) -0.0020(10) -0.0010(11) C7 0.0115(13) 0.0136(14) 0.0059(12) 0.0011(11) -0.0008(10) -0.0022(11) C8 0.0130(13) 0.0104(13) 0.0064(12) 0.0009(10) 0.0006(10) -0.0018(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N5 1.991(2) 1_556 ? Zn1 N4 1.993(2) 3_747 ? Zn1 N1 2.020(2) . ? Zn1 N8 2.030(2) 4_557 ? N1 N2 1.308(3) . ? N1 N3 1.355(3) . ? N2 N4 1.340(3) . ? N3 C1 1.330(4) . ? N4 C1 1.355(3) . ? N5 N7 1.305(4) . ? N5 N6 1.351(3) . ? N6 C8 1.321(4) . ? N7 N8 1.344(3) . ? N8 C8 1.352(4) . ? C2 C4 1.395(4) . ? C2 C3 1.405(4) . ? C3 C5 1.383(3) . ? C3 H3 0.9500 . ? C4 C6 1.384(4) . ? C4 H4 0.9500 . ? C5 C7 1.401(4) . ? C5 H5 0.9500 . ? C6 C7 1.392(4) . ? C6 H6 0.9500 . ? C7 C8 1.471(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Zn1 N4 121.88(10) 1_556 3_747 ? N5 Zn1 N1 110.07(9) 1_556 . ? N4 Zn1 N1 108.72(10) 3_747 . ? N5 Zn1 N8 101.08(10) 1_556 4_557 ? N4 Zn1 N8 110.15(10) 3_747 4_557 ? N1 Zn1 N8 103.21(10) . 4_557 ? N2 N1 N3 112.0(2) . . ? N2 N1 Zn1 113.90(18) . . ? N3 N1 Zn1 129.84(19) . . ? N1 N2 N4 107.3(2) . . ? C1 N3 N1 103.4(2) . . ? N2 N4 C1 106.2(2) . . ? N2 N4 Zn1 113.92(17) . 3_757 ? C1 N4 Zn1 139.37(19) . 3_757 ? N7 N5 N6 112.1(2) . . ? N7 N5 Zn1 121.49(19) . 1_554 ? N6 N5 Zn1 125.32(19) . 1_554 ? C8 N6 N5 103.5(2) . . ? N5 N7 N8 107.1(2) . . ? N7 N8 C8 105.9(2) . . ? N7 N8 Zn1 116.82(18) . 4_457 ? C8 N8 Zn1 135.88(19) . 4_457 ? N3 C1 N4 111.1(2) . . ? N3 C1 C2 124.0(3) . . ? N4 C1 C2 124.7(3) . . ? C4 C2 C3 119.3(3) . . ? C4 C2 C1 120.6(3) . . ? C3 C2 C1 120.0(3) . . ? C5 C3 C2 120.2(3) . . ? C5 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C6 C4 C2 120.3(3) . . ? C6 C4 H4 119.9 . . ? C2 C4 H4 119.9 . . ? C3 C5 C7 120.1(3) . . ? C3 C5 H5 120.0 . . ? C7 C5 H5 120.0 . . ? C4 C6 C7 120.5(3) . . ? C4 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C6 C7 C5 119.6(3) . . ? C6 C7 C8 120.5(3) . . ? C5 C7 C8 119.9(3) . . ? N6 C8 N8 111.4(2) . . ? N6 C8 C7 123.4(3) . . ? N8 C8 C7 125.2(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Zn1 N1 N2 71.3(2) 1_556 . . . ? N4 Zn1 N1 N2 -152.8(2) 3_747 . . . ? N8 Zn1 N1 N2 -35.9(2) 4_557 . . . ? N5 Zn1 N1 N3 -134.1(2) 1_556 . . . ? N4 Zn1 N1 N3 1.7(3) 3_747 . . . ? N8 Zn1 N1 N3 118.7(2) 4_557 . . . ? N3 N1 N2 N4 -0.2(3) . . . . ? Zn1 N1 N2 N4 158.98(17) . . . . ? N2 N1 N3 C1 0.0(3) . . . . ? Zn1 N1 N3 C1 -155.0(2) . . . . ? N1 N2 N4 C1 0.3(3) . . . . ? N1 N2 N4 Zn1 -173.12(17) . . . 3_757 ? N7 N5 N6 C8 0.1(3) . . . . ? Zn1 N5 N6 C8 168.33(19) 1_554 . . . ? N6 N5 N7 N8 0.0(3) . . . . ? Zn1 N5 N7 N8 -168.81(18) 1_554 . . . ? N5 N7 N8 C8 0.0(3) . . . . ? N5 N7 N8 Zn1 -168.80(18) . . . 4_457 ? N1 N3 C1 N4 0.2(3) . . . . ? N1 N3 C1 C2 177.0(3) . . . . ? N2 N4 C1 N3 -0.3(3) . . . . ? Zn1 N4 C1 N3 170.4(2) 3_757 . . . ? N2 N4 C1 C2 -177.1(3) . . . . ? Zn1 N4 C1 C2 -6.3(5) 3_757 . . . ? N3 C1 C2 C4 156.0(3) . . . . ? N4 C1 C2 C4 -27.7(4) . . . . ? N3 C1 C2 C3 -27.2(4) . . . . ? N4 C1 C2 C3 149.2(3) . . . . ? C4 C2 C3 C5 0.5(5) . . . . ? C1 C2 C3 C5 -176.4(3) . . . . ? C3 C2 C4 C6 -1.1(5) . . . . ? C1 C2 C4 C6 175.8(3) . . . . ? C2 C3 C5 C7 0.5(5) . . . . ? C2 C4 C6 C7 0.5(5) . . . . ? C4 C6 C7 C5 0.5(5) . . . . ? C4 C6 C7 C8 -177.1(3) . . . . ? C3 C5 C7 C6 -1.0(4) . . . . ? C3 C5 C7 C8 176.6(3) . . . . ? N5 N6 C8 N8 -0.1(3) . . . . ? N5 N6 C8 C7 -177.5(3) . . . . ? N7 N8 C8 N6 0.1(3) . . . . ? Zn1 N8 C8 N6 165.6(2) 4_457 . . . ? N7 N8 C8 C7 177.5(3) . . . . ? Zn1 N8 C8 C7 -17.0(5) 4_457 . . . ? C6 C7 C8 N6 148.8(3) . . . . ? C5 C7 C8 N6 -28.8(4) . . . . ? C6 C7 C8 N8 -28.3(4) . . . . ? C5 C7 C8 N8 154.1(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.088 _refine_diff_density_min -0.681 _refine_diff_density_rms 0.100