# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email pjs80@cam.ac.uk _publ_contact_author_name 'Paul Saines' loop_ _publ_author_name 'Paul Saines' 'Phillip Barton' 'Prashant Jain' 'Tony Cheetham' data_1 _database_code_depnum_ccdc_archive 'CCDC 836980' #TrackingRef '- Merged_deposit.cif' _audit_creation_date 2011-03-21T17:18:50-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C10 H20 Mn2 O12, 2(H2 0)' _chemical_formula_sum 'C10 H24 Mn2 O14' _chemical_formula_weight 478.17 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.6205(5) _cell_length_b 7.9261(5) _cell_length_c 8.0664(7) _cell_angle_alpha 85.402(7) _cell_angle_beta 81.432(6) _cell_angle_gamma 70.018(6) _cell_volume 452.55(6) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2536 _cell_measurement_theta_min 3.5788 _cell_measurement_theta_max 29.1337 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description 'irregular block' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.449 _exptl_crystal_size_mid 0.361 _exptl_crystal_size_min 0.184 _exptl_crystal_density_diffrn 1.755 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 246 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.464 _exptl_absorpt_correction_T_min 0.646 _exptl_absorpt_correction_T_max 0.806 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a __diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 16.1183 _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_unetI/netI 0.0384 _diffrn_reflns_number 3166 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 29.2 _diffrn_measured_fraction_theta_max 0.842 _diffrn_reflns_theta_full 26.32 _diffrn_measured_fraction_theta_full 0.997 _reflns_number_total 2055 _reflns_number_gt 1938 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlisPro, Oxford Diffraction, 2010' _computing_cell_refinement 'CrysAlisPro, Oxford Diffraction, 2010' _computing_data_reduction 'CrysAlisPro, Oxford Diffraction, 2010' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond (Brandenburg 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+0.1911P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 2055 _refine_ls_number_parameters 136 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0279 _refine_ls_R_factor_gt 0.0265 _refine_ls_wR_factor_ref 0.0687 _refine_ls_wR_factor_gt 0.0672 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.385 _refine_diff_density_min -0.431 _refine_diff_density_rms 0.070 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.71703(3) 0.65589(3) 0.61833(3) 0.01108(9) Uani 1 1 d . . . O11 O 0.44604(16) 0.71015(15) 0.79939(15) 0.0164(3) Uani 1 1 d . . . O2 O 0.93555(15) 0.71824(15) 0.46128(15) 0.0150(2) Uani 1 1 d . . . O1 O 0.75083(15) 0.37970(15) 0.58107(15) 0.0147(2) Uani 1 1 d . . . O1W O 0.86418(17) 0.61659(18) 0.82918(16) 0.0199(3) Uani 1 1 d D . . H1WA H 0.815(3) 0.595(3) 0.927(2) 0.030 Uiso 1 1 d D . . H1WB H 0.983(2) 0.570(3) 0.824(3) 0.030 Uiso 1 1 d D . . O3W O 0.76318(16) 0.50886(17) 0.14382(15) 0.0170(3) Uani 1 1 d D . . H3WA H 0.710(3) 0.431(2) 0.149(3) 0.026 Uiso 1 1 d D . . H3WB H 0.702(3) 0.585(2) 0.223(2) 0.026 Uiso 1 1 d D . . O2W O 0.55555(16) 0.72226(15) 0.40359(15) 0.0134(2) Uani 1 1 d D . . H2WA H 0.462(2) 0.688(2) 0.412(3) 0.020 Uiso 1 1 d D . . H2WB H 0.525(3) 0.831(2) 0.367(3) 0.020 Uiso 1 1 d D . . O12 O 0.53701(15) 0.93918(15) 0.71091(15) 0.0153(2) Uani 1 1 d . . . C13 C 0.0891(2) 0.9282(2) 0.9598(2) 0.0150(3) Uani 1 1 d . . . H13A H 0.1348 0.8307 1.0438 0.018 Uiso 1 1 calc R . . H13B H 0.0575 0.8757 0.8657 0.018 Uiso 1 1 calc R . . C1 C 0.9097(2) 0.2564(2) 0.54940(19) 0.0120(3) Uani 1 1 d . . . C11 C 0.4179(2) 0.8773(2) 0.7973(2) 0.0131(3) Uani 1 1 d . . . C2 C 0.9050(2) 0.0687(2) 0.5288(2) 0.0137(3) Uani 1 1 d . . . H2A H 0.8531 0.0261 0.6375 0.016 Uiso 1 1 calc R . . H2B H 0.8181 0.0760 0.4466 0.016 Uiso 1 1 calc R . . C12 C 0.2452(2) 1.0053(2) 0.8946(2) 0.0161(3) Uani 1 1 d . . . H12A H 0.1932 1.1120 0.8215 0.019 Uiso 1 1 calc R . . H12B H 0.2843 1.0465 0.9913 0.019 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.00918(14) 0.01019(14) 0.01322(15) -0.00174(9) -0.00031(10) -0.00258(10) O11 0.0134(5) 0.0127(6) 0.0215(6) -0.0024(5) 0.0028(5) -0.0037(5) O2 0.0114(5) 0.0147(5) 0.0192(6) -0.0009(5) 0.0002(4) -0.0056(5) O1 0.0104(5) 0.0109(5) 0.0214(6) -0.0023(4) -0.0010(4) -0.0020(5) O1W 0.0138(6) 0.0305(7) 0.0141(6) 0.0010(5) -0.0027(5) -0.0057(6) O3W 0.0157(6) 0.0179(6) 0.0180(6) -0.0045(5) 0.0022(5) -0.0072(5) O2W 0.0116(5) 0.0114(5) 0.0179(6) 0.0007(4) -0.0030(4) -0.0044(5) O12 0.0124(5) 0.0134(5) 0.0184(6) -0.0010(4) 0.0017(4) -0.0037(5) C13 0.0112(7) 0.0135(8) 0.0176(8) -0.0032(6) 0.0032(6) -0.0020(7) C1 0.0136(7) 0.0120(7) 0.0097(7) 0.0004(6) -0.0019(6) -0.0033(6) C11 0.0112(7) 0.0137(7) 0.0139(8) -0.0010(6) -0.0028(6) -0.0029(6) C2 0.0109(7) 0.0114(7) 0.0180(8) -0.0025(6) -0.0004(6) -0.0030(7) C12 0.0137(8) 0.0148(8) 0.0176(8) -0.0047(6) 0.0026(6) -0.0029(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O2 2.1108(11) . ? Mn1 O1W 2.1194(12) . ? Mn1 O1 2.1554(11) . ? Mn1 O2W 2.1995(12) . ? Mn1 O11 2.2755(12) . ? Mn1 O12 2.3108(11) . ? O11 C11 1.267(2) . ? O2 C1 1.2522(18) 2_766 ? O1 C1 1.2745(19) . ? O12 C11 1.269(2) . ? C13 C12 1.525(2) . ? C13 C13 1.536(3) 2_577 ? C1 O2 1.2522(18) 2_766 ? C1 C2 1.523(2) . ? C11 C12 1.512(2) . ? C2 C2 1.517(3) 2_756 ? 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 Mn1 O1W 91.53(5) . . ? O2 Mn1 O1 107.75(4) . . ? O1W Mn1 O1 98.59(5) . . ? O2 Mn1 O2W 87.81(4) . . ? O1W Mn1 O2W 174.93(5) . . ? O1 Mn1 O2W 86.39(4) . . ? O2 Mn1 O11 156.79(4) . . ? O1W Mn1 O11 88.08(5) . . ? O1 Mn1 O11 95.24(4) . . ? O2W Mn1 O11 90.54(4) . . ? O2 Mn1 O12 99.79(4) . . ? O1W Mn1 O12 88.79(5) . . ? O1 Mn1 O12 151.19(4) . . ? O2W Mn1 O12 86.37(4) . . ? O11 Mn1 O12 57.00(4) . . ? C11 O11 Mn1 92.66(10) . . ? C1 O2 Mn1 147.06(11) 2_766 . ? C1 O1 Mn1 124.10(10) . . ? C11 O12 Mn1 90.97(9) . . ? C12 C13 C13 111.99(16) . 2_577 ? O2 C1 O1 123.69(14) 2_766 . ? O2 C1 C2 119.85(14) 2_766 . ? O1 C1 C2 116.44(13) . . ? O11 C11 O12 119.35(15) . . ? O11 C11 C12 121.57(14) . . ? O12 C11 C12 119.08(14) . . ? C2 C2 C1 114.55(16) 2_756 . ? C11 C12 C13 115.25(13) . . ? #==END #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_2 _database_code_depnum_ccdc_archive 'CCDC 836981' #TrackingRef '- Merged_deposit.cif' _audit_creation_date 2011-03-21T19:37:40-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C22 H34 Co6 O26, 5(H2 O)' _chemical_formula_sum 'C22 H44 Co6 O31' _chemical_formula_weight 1158.15 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0862(5) _cell_length_b 10.7299(5) _cell_length_c 19.5496(7) _cell_angle_alpha 89.452(3) _cell_angle_beta 87.337(4) _cell_angle_gamma 80.347(4) _cell_volume 1876.95(15) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4138 _cell_measurement_theta_min 2.8729 _cell_measurement_theta_max 29.1208 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description rod _exptl_crystal_colour 'light pink' _exptl_crystal_size_max 0.147 _exptl_crystal_size_mid 0.049 _exptl_crystal_size_min 0.045 _exptl_crystal_density_diffrn 2.049 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1172 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.698 _exptl_absorpt_correction_T_min 0.721 _exptl_absorpt_correction_T_max 0.892 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_detector_area_resol_mean 16.1183 _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.1052 _diffrn_reflns_number 14344 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 29.19 _diffrn_reflns_theta_full 26.32 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.833 _reflns_number_total 8479 _reflns_number_gt 5540 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlisPro, Oxford Diffraction, 2010' _computing_cell_refinement 'CrysAlisPro, Oxford Diffraction, 2010' _computing_data_reduction 'CrysAlisPro, Oxford Diffraction, 2010' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond (Brandenburg 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0222P)^2^+2.4525P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 8479 _refine_ls_number_parameters 597 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.073 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.0865 _refine_ls_wR_factor_gt 0.0699 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.825 _refine_diff_density_min -0.48 _refine_diff_density_rms 0.112 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co2 Co 1.17207(6) 0.25159(5) 0.22156(2) 0.00918(12) Uani 1 1 d . . . Co1 Co 0.84697(6) 0.23484(5) 0.27697(2) 0.00892(12) Uani 1 1 d . . . Co4 Co 1.06547(6) 0.24082(5) 0.41060(2) 0.00782(11) Uani 1 1 d . . . Co3 Co 0.94238(6) 0.25597(5) 0.08892(2) 0.00784(11) Uani 1 1 d . . . Co6 Co 1 0.5 0.5 0.00855(16) Uani 1 2 d S . . Co5 Co 1 0 0 0.00794(16) Uani 1 2 d S . . Co8 Co 1 0.5 0 0.00796(15) Uani 1 2 d S . . Co7 Co 1 0 0.5 0.00824(16) Uani 1 2 d S . . O2H O 1.0624(3) 0.1920(2) 0.31075(13) 0.0085(6) Uani 1 1 d . . . H2H H 1.078(5) 0.117(4) 0.310(2) 0.013 Uiso 1 1 d . . . O1 O 0.6595(3) 0.5006(3) 0.14559(13) 0.0201(7) Uani 1 1 d . . . O1H O 0.9565(3) 0.2973(2) 0.18812(13) 0.0084(6) Uani 1 1 d . . . H1H H 0.937(5) 0.370(4) 0.193(2) 0.013 Uiso 1 1 d . . . O31 O 1.3775(3) 0.0355(3) 0.37358(13) 0.0191(6) Uani 1 1 d . . . O8W O 1.1627(3) 0.4377(3) 0.26390(14) 0.0154(6) Uani 1 1 d D . . H8WA H 1.085(3) 0.489(3) 0.2538(18) 0.023 Uiso 1 1 d D . . H8WB H 1.160(4) 0.418(4) 0.3060(8) 0.023 Uiso 1 1 d D . . O14 O 1.2088(3) 0.0707(2) 0.18326(13) 0.0120(6) Uani 1 1 d . . . O23 O 0.9640(3) -0.1287(2) 0.42588(12) 0.0127(6) Uani 1 1 d . A . O6W O 0.6448(3) 0.2850(3) 0.22330(13) 0.0119(6) Uani 1 1 d D . . H6WA H 0.662(5) 0.239(3) 0.1875(12) 0.018 Uiso 1 1 d D . . H6WB H 0.634(5) 0.3624(12) 0.2117(17) 0.018 Uiso 1 1 d D . . O7W O 0.8528(3) 0.0478(3) 0.23786(14) 0.0154(6) Uani 1 1 d D . . H7WA H 0.932(2) 0.006(3) 0.2541(19) 0.023 Uiso 1 1 d D . . H7WB H 0.778(3) 0.015(3) 0.2514(19) 0.023 Uiso 1 1 d D . . O52 O 1.2509(3) 0.3319(2) 0.39461(13) 0.0129(6) Uani 1 1 d . . . O22 O 0.8050(3) 0.4223(2) 0.31191(13) 0.0118(6) Uani 1 1 d . . . O41 O 0.7448(3) 0.1793(2) 0.10059(12) 0.0119(6) Uani 1 1 d . . . O4 O 1.1201(3) 0.3556(2) 0.05686(12) 0.0088(5) Uani 1 1 d . . . O33 O 0.7211(3) 0.1845(2) 0.36016(13) 0.0119(6) Uani 1 1 d . . . O11 O 1.0215(3) 0.6283(2) 0.07558(13) 0.0129(6) Uani 1 1 d . . . O42 O 0.8037(3) -0.0106(2) 0.04933(12) 0.0115(6) Uani 1 1 d . . . O3 O 1.2879(3) 0.3161(3) 0.13794(13) 0.0127(6) Uani 1 1 d . . . O13 O 1.0731(3) 0.0737(2) 0.09014(12) 0.0105(6) Uani 1 1 d . . . O3W O 0.6329(4) 0.4139(3) 0.80732(18) 0.0314(8) Uani 1 1 d D . . H3WA H 0.5399(17) 0.441(4) 0.816(2) 0.047 Uiso 1 1 d D . . H3WB H 0.671(4) 0.472(3) 0.786(2) 0.047 Uiso 1 1 d D . . O24 O 1.0704(3) 0.3004(2) 0.51403(12) 0.0111(6) Uani 1 1 d . . . O21 O 0.9317(3) 0.4250(2) 0.40708(12) 0.0107(6) Uani 1 1 d . . . O32 O 1.1725(3) 0.0595(2) 0.44203(12) 0.0106(6) Uani 1 1 d . . . O2 O 0.8253(3) 0.4393(2) 0.05966(12) 0.0104(6) Uani 1 1 d . . . O34 O 0.8844(3) 0.1478(2) 0.44311(12) 0.0098(5) Uani 1 1 d . . . C12 C 1.0880(5) 0.8026(4) 0.13465(19) 0.0142(9) Uani 1 1 d . . . H12A H 1.1136 0.7378 0.1705 0.017 Uiso 1 1 calc R . . H12B H 0.9971 0.8606 0.1512 0.017 Uiso 1 1 calc R . . O51 O 1.1956(3) 0.5158(2) 0.45204(13) 0.0123(6) Uani 1 1 d . . . C1 C 0.7108(4) 0.5125(3) 0.08589(19) 0.0102(8) Uani 1 1 d . . . C11 C 1.0541(4) 0.7385(3) 0.07043(18) 0.0093(8) Uani 1 1 d . . . O12 O 0.9406(3) 0.2018(2) -0.01410(12) 0.0105(6) Uani 1 1 d . . . C51 C 1.2850(4) 0.4320(3) 0.41869(18) 0.0101(8) Uani 1 1 d . . . C33 C 1.3667(4) -0.1086(4) 0.53446(18) 0.0128(8) Uani 1 1 d . . . H33A H 1.4645 -0.1558 0.5477 0.015 Uiso 1 1 calc R . . H33B H 1.367 -0.0179 0.5433 0.015 Uiso 1 1 calc R . . C31 C 1.3000(4) -0.0032(4) 0.4202(2) 0.0134(8) Uani 1 1 d . . . C24 C 0.9317(4) -0.2380(4) 0.43066(19) 0.0115(8) Uani 1 1 d . . . C3 C 0.6331(4) 0.5961(4) -0.03352(18) 0.0118(8) Uani 1 1 d . . . H3A H 0.6443 0.5035 -0.0398 0.014 Uiso 1 1 calc R . . H3B H 0.5328 0.6339 -0.0485 0.014 Uiso 1 1 calc R . . C14 C 1.1644(4) 0.0177(3) 0.13338(18) 0.0088(8) Uani 1 1 d . . . C21 C 0.8397(4) 0.4774(3) 0.36324(19) 0.0100(8) Uani 1 1 d . . . C41 C 0.7135(4) 0.0747(4) 0.08094(18) 0.0099(8) Uani 1 1 d . . . C32 C 1.3532(4) -0.1260(4) 0.45649(18) 0.0137(9) Uani 1 1 d . . . H32A H 1.4519 -0.1646 0.4361 0.016 Uiso 1 1 calc R . . H32B H 1.2825 -0.185 0.4493 0.016 Uiso 1 1 calc R . . C43 C 0.4776(4) 0.0586(3) 0.02264(19) 0.0124(8) Uani 1 1 d . . . H43A H 0.3681 0.0718 0.032 0.015 Uiso 1 1 calc R . . H43B H 0.5013 0.1332 -0.0031 0.015 Uiso 1 1 calc R . . C2 C 0.6407(4) 0.6233(4) 0.04337(18) 0.0135(8) Uani 1 1 d . . . H2A H 0.6982 0.6931 0.0483 0.016 Uiso 1 1 calc R . . H2B H 0.538 0.6531 0.0622 0.016 Uiso 1 1 calc R . . C53 C 1.5228(4) 0.4422(4) 0.47667(18) 0.0133(9) Uani 1 1 d . . . H53A H 1.4992 0.3664 0.5012 0.016 Uiso 1 1 calc R . . H53B H 1.6322 0.4296 0.4672 0.016 Uiso 1 1 calc R . . O1W O 0.9085(3) 0.0769(3) 0.69910(14) 0.0199(7) Uani 1 1 d D . . H1WA H 0.8183(19) 0.113(4) 0.7038(19) 0.03 Uiso 1 1 d D . . H1WB H 0.948(4) 0.094(4) 0.6605(12) 0.03 Uiso 1 1 d D . . O4W O 0.4210(4) 0.0501(3) 0.73170(17) 0.0300(8) Uani 1 1 d D . . H4WA H 0.426(5) 0.043(5) 0.6881(6) 0.045 Uiso 1 1 d D . . H4WB H 0.486(4) -0.001(4) 0.7524(19) 0.045 Uiso 1 1 d D . . O2W O 0.6336(4) 0.2324(3) 0.70835(17) 0.0360(8) Uani 1 1 d D . . H2WA H 0.565(4) 0.189(4) 0.720(2) 0.054 Uiso 1 1 d D . . H2WB H 0.623(6) 0.299(3) 0.733(2) 0.054 Uiso 1 1 d D . . O5W O 0.0744(4) 0.4210(3) 0.79237(14) 0.0229(7) Uani 1 1 d D . . H5WA H 0.041(4) 0.409(4) 0.8328(10) 0.034 Uiso 1 1 d D . . H5WB H 0.1656(19) 0.431(5) 0.7919(19) 0.034 Uiso 1 1 d D . . C4 C 1.2501(4) 0.3545(3) 0.07984(19) 0.0110(8) Uani 1 1 d . . . C42 C 0.5550(4) 0.0517(4) 0.09166(19) 0.0122(8) Uani 1 1 d . . . H42A H 0.4991 0.116 0.1234 0.015 Uiso 1 1 calc R . . H42B H 0.5549 -0.0326 0.1126 0.015 Uiso 1 1 calc R . . C13 C 1.2178(4) -0.1217(3) 0.12422(19) 0.0124(8) Uani 1 1 d . . . H13A H 1.295 -0.151 0.1576 0.015 Uiso 1 1 calc R . . H13B H 1.2641 -0.1376 0.0776 0.015 Uiso 1 1 calc R . . C34 C 0.7543(4) 0.1509(3) 0.41964(18) 0.0097(8) Uani 1 1 d . . . C52 C 1.4444(4) 0.4539(4) 0.40799(19) 0.0129(8) Uani 1 1 d . . . H52A H 1.4453 0.5392 0.3884 0.015 Uiso 1 1 calc R . . H52B H 1.499 0.391 0.3752 0.015 Uiso 1 1 calc R . . C22 C 0.7743(4) 0.6152(3) 0.3741(2) 0.0135(8) Uani 1 1 d . . . H22A H 0.6928 0.6371 0.342 0.016 Uiso 0.39(5) 1 calc PR A 7 H22B H 0.7277 0.6236 0.421 0.016 Uiso 0.39(5) 1 calc PR A 7 H22C H 0.7263 0.6278 0.4206 0.016 Uiso 0.61(5) 1 calc PR A 8 H22D H 0.6976 0.6429 0.3403 0.016 Uiso 0.61(5) 1 calc PR A 8 C23A C 0.871(3) -0.2897(16) 0.3662(6) 0.0065(12) Uiso 0.39(5) 1 d P . 7 H23A H 0.8153 -0.2168 0.3416 0.008 Uiso 0.39(5) 1 calc PR A 7 H23B H 0.9578 -0.3256 0.336 0.008 Uiso 0.39(5) 1 calc PR A 7 C23 C 0.908(2) -0.3034(10) 0.3650(4) 0.0065(12) Uiso 0.61(5) 1 d P . 8 H23C H 1.0012 -0.3601 0.3504 0.008 Uiso 0.61(5) 1 calc PR A 8 H23D H 0.8839 -0.2393 0.3286 0.008 Uiso 0.61(5) 1 calc PR A 8 O9W O 1.3805(3) 0.2021(3) 0.26570(13) 0.0155(6) Uani 1 1 d D . . H9WA H 1.373(4) 0.177(4) 0.3066(9) 0.023 Uiso 1 1 d D . . H9WB H 1.453(3) 0.242(4) 0.2575(17) 0.023 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co2 0.0101(3) 0.0107(3) 0.0074(3) 0.0002(2) -0.0006(2) -0.0037(2) Co1 0.0097(3) 0.0103(3) 0.0073(3) 0.0001(2) -0.0001(2) -0.0032(2) Co4 0.0090(3) 0.0078(2) 0.0070(3) 0.0000(2) -0.0003(2) -0.0025(2) Co3 0.0092(3) 0.0074(2) 0.0070(3) -0.0002(2) -0.0002(2) -0.0019(2) Co6 0.0094(4) 0.0079(3) 0.0085(4) -0.0009(3) -0.0011(3) -0.0016(3) Co5 0.0084(4) 0.0080(3) 0.0074(4) -0.0009(3) 0.0002(3) -0.0015(3) Co8 0.0091(4) 0.0073(3) 0.0076(4) 0.0000(3) -0.0002(3) -0.0017(3) Co7 0.0101(4) 0.0073(3) 0.0078(4) -0.0001(3) -0.0003(3) -0.0028(3) O2H 0.0106(13) 0.0074(12) 0.0080(13) 0.0000(11) -0.0006(10) -0.0025(11) O1 0.0213(16) 0.0221(16) 0.0132(14) 0.0033(12) 0.0065(12) 0.0050(13) O1H 0.0109(13) 0.0046(12) 0.0107(14) -0.0004(11) -0.0003(10) -0.0046(11) O31 0.0194(16) 0.0179(15) 0.0182(15) 0.0072(12) 0.0063(12) 0.0001(13) O8W 0.0210(16) 0.0143(14) 0.0118(14) 0.0011(12) -0.0022(12) -0.0056(13) O14 0.0128(14) 0.0119(14) 0.0110(14) -0.0011(11) -0.0021(11) -0.0009(12) O23 0.0192(15) 0.0118(13) 0.0084(14) -0.0013(11) -0.0010(11) -0.0062(12) O6W 0.0112(14) 0.0099(13) 0.0143(14) -0.0009(11) -0.0012(11) -0.0004(12) O7W 0.0167(15) 0.0104(14) 0.0204(16) 0.0000(12) -0.0010(13) -0.0064(12) O52 0.0111(14) 0.0159(14) 0.0119(14) -0.0046(11) 0.0023(11) -0.0031(12) O22 0.0146(14) 0.0080(13) 0.0132(14) -0.0019(11) -0.0039(11) -0.0021(11) O41 0.0117(14) 0.0142(14) 0.0106(14) -0.0027(11) 0.0006(11) -0.0051(12) O4 0.0079(13) 0.0078(12) 0.0116(14) 0.0009(10) -0.0013(10) -0.0039(11) O33 0.0128(14) 0.0148(14) 0.0095(14) 0.0047(11) -0.0026(11) -0.0063(12) O11 0.0195(15) 0.0088(13) 0.0115(14) 0.0000(11) 0.0010(11) -0.0056(12) O42 0.0106(14) 0.0118(13) 0.0122(14) -0.0034(11) 0.0011(11) -0.0028(11) O3 0.0106(14) 0.0172(14) 0.0109(14) 0.0052(11) -0.0011(11) -0.0040(12) O13 0.0133(14) 0.0087(13) 0.0095(14) -0.0014(11) -0.0025(11) -0.0012(11) O3W 0.0229(18) 0.0222(17) 0.049(2) -0.0030(16) 0.0105(16) -0.0061(15) O24 0.0155(14) 0.0077(12) 0.0096(14) 0.0008(11) -0.0001(11) -0.0007(11) O21 0.0125(14) 0.0093(13) 0.0105(14) -0.0005(11) -0.0024(11) -0.0015(11) O32 0.0105(13) 0.0081(13) 0.0132(14) 0.0005(11) 0.0010(11) -0.0023(11) O2 0.0107(13) 0.0097(13) 0.0096(14) 0.0004(11) 0.0006(10) 0.0017(11) O34 0.0112(13) 0.0085(13) 0.0098(13) 0.0034(10) -0.0010(11) -0.0025(11) C12 0.021(2) 0.0082(18) 0.015(2) -0.0005(15) 0.0000(16) -0.0081(17) O51 0.0105(14) 0.0122(13) 0.0152(14) -0.0027(11) 0.0009(11) -0.0051(12) C1 0.0108(19) 0.0095(18) 0.011(2) 0.0010(15) -0.0004(15) -0.0037(16) C11 0.0094(18) 0.0068(17) 0.0113(19) 0.0011(15) 0.0007(15) -0.0006(15) O12 0.0145(14) 0.0064(12) 0.0108(14) -0.0003(11) 0.0005(11) -0.0027(11) C51 0.0120(19) 0.0099(18) 0.010(2) 0.0014(15) -0.0008(15) -0.0059(16) C33 0.0105(19) 0.015(2) 0.012(2) 0.0016(16) -0.0020(15) -0.0020(16) C31 0.014(2) 0.0124(19) 0.015(2) -0.0013(16) 0.0001(16) -0.0045(16) C24 0.0102(19) 0.0098(18) 0.015(2) 0.0013(16) 0.0026(15) -0.0039(16) C3 0.0102(19) 0.0122(19) 0.014(2) 0.0027(16) -0.0008(15) -0.0066(16) C14 0.0116(19) 0.0098(18) 0.0062(19) 0.0014(15) 0.0008(15) -0.0054(16) C21 0.0116(19) 0.0095(18) 0.009(2) -0.0002(15) 0.0027(15) -0.0033(16) C41 0.013(2) 0.0129(19) 0.0042(18) 0.0030(15) -0.0042(15) -0.0039(16) C32 0.013(2) 0.015(2) 0.012(2) -0.0004(16) 0.0040(16) 0.0016(17) C43 0.0076(19) 0.013(2) 0.018(2) -0.0033(17) -0.0023(16) -0.0033(16) C2 0.012(2) 0.015(2) 0.012(2) 0.0024(16) 0.0035(15) 0.0019(17) C53 0.011(2) 0.014(2) 0.014(2) -0.0007(16) -0.0020(16) -0.0001(17) O1W 0.0224(17) 0.0201(16) 0.0156(15) 0.0038(12) 0.0035(12) -0.0005(14) O4W 0.0283(19) 0.0287(19) 0.0326(19) -0.0058(15) 0.0055(15) -0.0050(15) O2W 0.038(2) 0.031(2) 0.036(2) -0.0049(16) 0.0005(16) -0.0013(17) O5W 0.0273(18) 0.0254(17) 0.0191(16) 0.0049(14) 0.0002(13) -0.0139(15) C4 0.013(2) 0.0092(18) 0.010(2) -0.0019(15) -0.0009(15) -0.0007(16) C42 0.013(2) 0.0132(19) 0.011(2) -0.0044(16) -0.0001(16) -0.0055(17) C13 0.0119(19) 0.0112(19) 0.014(2) -0.0008(16) -0.0047(15) 0.0007(16) C34 0.0102(19) 0.0100(18) 0.0075(19) -0.0017(15) 0.0003(15) 0.0022(16) C52 0.0086(19) 0.015(2) 0.015(2) -0.0012(17) 0.0017(16) -0.0047(16) C22 0.017(2) 0.0085(18) 0.016(2) -0.0010(16) -0.0023(16) -0.0044(17) O9W 0.0127(15) 0.0202(16) 0.0146(15) 0.0060(12) -0.0032(12) -0.0052(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co2 O14 2.055(3) . ? Co2 O1H 2.072(3) . ? Co2 O3 2.079(3) . ? Co2 O9W 2.102(3) . ? Co2 O2H 2.115(3) . ? Co2 O8W 2.156(3) . ? Co1 O33 2.064(3) . ? Co1 O2H 2.071(3) . ? Co1 O22 2.098(2) . ? Co1 O1H 2.121(3) . ? Co1 O6W 2.145(3) . ? Co1 O7W 2.146(3) . ? Co4 O2H 2.029(2) . ? Co4 O52 2.095(3) . ? Co4 O32 2.123(3) . ? Co4 O24 2.131(2) . ? Co4 O34 2.132(3) . ? Co4 O21 2.141(3) . ? Co3 O1H 2.008(3) . ? Co3 O41 2.098(3) . ? Co3 O12 2.103(2) . ? Co3 O13 2.112(2) . ? Co3 O4 2.148(3) . ? Co3 O2 2.159(3) . ? Co6 O51 2.003(3) . ? Co6 O51 2.003(2) 2_766 ? Co6 O24 2.149(2) . ? Co6 O24 2.149(2) 2_766 ? Co6 O21 2.152(2) 2_766 ? Co6 O21 2.152(2) . ? Co5 O42 2.008(2) 2_755 ? Co5 O42 2.008(2) . ? Co5 O13 2.118(2) 2_755 ? Co5 O13 2.118(2) . ? Co5 O12 2.160(2) 2_755 ? Co5 O12 2.160(2) . ? Co8 O11 2.067(2) . ? Co8 O11 2.067(2) 2_765 ? Co8 O4 2.083(3) 2_765 ? Co8 O4 2.083(3) . ? Co8 O2 2.113(3) 2_765 ? Co8 O2 2.113(3) . ? Co7 O32 2.075(2) 2_756 ? Co7 O32 2.075(3) . ? Co7 O23 2.085(2) 2_756 ? Co7 O23 2.085(2) . ? Co7 O34 2.091(3) 2_756 ? Co7 O34 2.091(3) . ? O1 C1 1.250(4) . ? O31 C31 1.237(4) . ? O14 C14 1.250(4) . ? O23 C24 1.257(4) . ? O52 C51 1.267(4) . ? O22 C21 1.249(4) . ? O41 C41 1.270(4) . ? O4 C4 1.281(4) . ? O33 C34 1.249(4) . ? O11 C11 1.269(4) . ? O42 C41 1.266(4) . ? O3 C4 1.248(4) . ? O13 C14 1.285(4) . ? O24 C24 1.268(4) 2_756 ? O21 C21 1.285(4) . ? O32 C31 1.294(4) . ? O2 C1 1.283(4) . ? O34 C34 1.283(4) . ? C12 C11 1.505(5) . ? C12 C13 1.546(5) 1_565 ? O51 C51 1.269(4) . ? C1 C2 1.512(5) . ? C11 O12 1.272(4) 2_765 ? O12 C11 1.272(4) 2_765 ? C51 C52 1.510(5) . ? C33 C34 1.513(5) 2_756 ? C33 C32 1.551(5) . ? C31 C32 1.508(5) . ? C24 O24 1.267(4) 2_756 ? C24 C23 1.511(8) . ? C24 C23A 1.544(13) . ? C3 C4 1.523(5) 2_765 ? C3 C2 1.541(5) . ? C14 C13 1.502(5) . ? C21 C22 1.511(5) . ? C41 C42 1.507(5) . ? C43 C43 1.532(7) 2_655 ? C43 C42 1.546(5) . ? C53 C53 1.535(7) 2_866 ? C53 C52 1.543(5) . ? C4 C3 1.522(5) 2_765 ? C13 C12 1.546(5) 1_545 ? C34 C33 1.513(5) 2_756 ? C22 C23A 1.456(15) 1_565 ? C22 C23 1.611(12) 1_565 ? C23A C22 1.456(15) 1_545 ? C23 C22 1.611(12) 1_545 ? 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 O14 Co2 O1H 95.18(10) . . ? O14 Co2 O3 91.46(10) . . ? O1H Co2 O3 99.21(10) . . ? O14 Co2 O9W 85.95(11) . . ? O1H Co2 O9W 173.97(10) . . ? O3 Co2 O9W 86.67(11) . . ? O14 Co2 O2H 90.98(10) . . ? O1H Co2 O2H 83.31(10) . . ? O3 Co2 O2H 176.32(10) . . ? O9W Co2 O2H 90.75(11) . . ? O14 Co2 O8W 172.90(11) . . ? O1H Co2 O8W 91.79(11) . . ? O3 Co2 O8W 86.11(10) . . ? O9W Co2 O8W 87.25(11) . . ? O2H Co2 O8W 91.15(10) . . ? O33 Co1 O2H 102.17(10) . . ? O33 Co1 O22 89.05(10) . . ? O2H Co1 O22 96.22(10) . . ? O33 Co1 O1H 174.35(10) . . ? O2H Co1 O1H 83.20(10) . . ? O22 Co1 O1H 88.60(10) . . ? O33 Co1 O6W 88.74(10) . . ? O2H Co1 O6W 168.96(10) . . ? O22 Co1 O6W 85.47(10) . . ? O1H Co1 O6W 85.94(10) . . ? O33 Co1 O7W 87.70(10) . . ? O2H Co1 O7W 92.81(11) . . ? O22 Co1 O7W 170.87(11) . . ? O1H Co1 O7W 93.85(10) . . ? O6W Co1 O7W 85.93(11) . . ? O2H Co4 O52 93.66(10) . . ? O2H Co4 O32 94.51(10) . . ? O52 Co4 O32 100.36(10) . . ? O2H Co4 O24 177.42(10) . . ? O52 Co4 O24 84.46(10) . . ? O32 Co4 O24 87.57(10) . . ? O2H Co4 O34 94.75(10) . . ? O52 Co4 O34 171.18(10) . . ? O32 Co4 O34 76.33(10) . . ? O24 Co4 O34 87.22(10) . . ? O2H Co4 O21 99.22(10) . . ? O52 Co4 O21 86.55(10) . . ? O32 Co4 O21 164.21(9) . . ? O24 Co4 O21 78.92(10) . . ? O34 Co4 O21 94.72(10) . . ? O1H Co3 O41 96.53(10) . . ? O1H Co3 O12 175.82(11) . . ? O41 Co3 O12 84.71(10) . . ? O1H Co3 O13 97.47(10) . . ? O41 Co3 O13 91.13(10) . . ? O12 Co3 O13 78.49(10) . . ? O1H Co3 O4 93.08(10) . . ? O41 Co3 O4 166.76(10) . . ? O12 Co3 O4 86.35(10) . . ? O13 Co3 O4 96.63(10) . . ? O1H Co3 O2 96.30(10) . . ? O41 Co3 O2 93.02(10) . . ? O12 Co3 O2 87.61(9) . . ? O13 Co3 O2 165.07(9) . . ? O4 Co3 O2 76.85(10) . . ? O51 Co6 O51 179.9990(10) . 2_766 ? O51 Co6 O24 91.18(10) . . ? O51 Co6 O24 88.82(10) 2_766 . ? O51 Co6 O24 88.82(10) . 2_766 ? O51 Co6 O24 91.18(10) 2_766 2_766 ? O24 Co6 O24 179.9990(10) . 2_766 ? O51 Co6 O21 91.16(10) . 2_766 ? O51 Co6 O21 88.84(10) 2_766 2_766 ? O24 Co6 O21 101.71(10) . 2_766 ? O24 Co6 O21 78.29(10) 2_766 2_766 ? O51 Co6 O21 88.84(10) . . ? O51 Co6 O21 91.17(10) 2_766 . ? O24 Co6 O21 78.29(10) . . ? O24 Co6 O21 101.71(10) 2_766 . ? O21 Co6 O21 180 2_766 . ? O42 Co5 O42 180 2_755 . ? O42 Co5 O13 89.13(10) 2_755 2_755 ? O42 Co5 O13 90.87(10) . 2_755 ? O42 Co5 O13 90.87(10) 2_755 . ? O42 Co5 O13 89.13(10) . . ? O13 Co5 O13 180.00(7) 2_755 . ? O42 Co5 O12 92.22(10) 2_755 2_755 ? O42 Co5 O12 87.78(10) . 2_755 ? O13 Co5 O12 77.13(10) 2_755 2_755 ? O13 Co5 O12 102.87(10) . 2_755 ? O42 Co5 O12 87.78(10) 2_755 . ? O42 Co5 O12 92.22(10) . . ? O13 Co5 O12 102.87(10) 2_755 . ? O13 Co5 O12 77.13(10) . . ? O12 Co5 O12 180 2_755 . ? O11 Co8 O11 180 . 2_765 ? O11 Co8 O4 90.02(10) . 2_765 ? O11 Co8 O4 89.98(10) 2_765 2_765 ? O11 Co8 O4 89.98(10) . . ? O11 Co8 O4 90.02(10) 2_765 . ? O4 Co8 O4 180 2_765 . ? O11 Co8 O2 90.47(10) . 2_765 ? O11 Co8 O2 89.53(10) 2_765 2_765 ? O4 Co8 O2 79.27(9) 2_765 2_765 ? O4 Co8 O2 100.73(10) . 2_765 ? O11 Co8 O2 89.53(10) . . ? O11 Co8 O2 90.47(10) 2_765 . ? O4 Co8 O2 100.73(10) 2_765 . ? O4 Co8 O2 79.27(9) . . ? O2 Co8 O2 180 2_765 . ? O32 Co7 O32 179.9980(10) 2_756 . ? O32 Co7 O23 93.09(10) 2_756 2_756 ? O32 Co7 O23 86.92(10) . 2_756 ? O32 Co7 O23 86.92(10) 2_756 . ? O32 Co7 O23 93.08(10) . . ? O23 Co7 O23 180 2_756 . ? O32 Co7 O34 78.27(10) 2_756 2_756 ? O32 Co7 O34 101.73(10) . 2_756 ? O23 Co7 O34 89.98(10) 2_756 2_756 ? O23 Co7 O34 90.02(10) . 2_756 ? O32 Co7 O34 101.73(10) 2_756 . ? O32 Co7 O34 78.27(10) . . ? O23 Co7 O34 90.02(10) 2_756 . ? O23 Co7 O34 89.98(10) . . ? O34 Co7 O34 180 2_756 . ? Co4 O2H Co1 110.13(12) . . ? Co4 O2H Co2 131.76(13) . . ? Co1 O2H Co2 96.84(11) . . ? Co3 O1H Co2 112.77(12) . . ? Co3 O1H Co1 130.58(13) . . ? Co2 O1H Co1 96.64(11) . . ? C14 O14 Co2 135.1(2) . . ? C24 O23 Co7 131.7(2) . . ? C51 O52 Co4 133.1(2) . . ? C21 O22 Co1 134.6(2) . . ? C41 O41 Co3 131.1(2) . . ? C4 O4 Co8 126.2(2) . . ? C4 O4 Co3 131.5(2) . . ? Co8 O4 Co3 99.54(10) . . ? C34 O33 Co1 132.2(2) . . ? C11 O11 Co8 129.8(2) . . ? C41 O42 Co5 129.4(2) . . ? C4 O3 Co2 133.0(2) . . ? C14 O13 Co3 132.1(2) . . ? C14 O13 Co5 128.6(2) . . ? Co3 O13 Co5 99.13(11) . . ? C24 O24 Co4 130.2(2) 2_756 . ? C24 O24 Co6 127.6(2) 2_756 . ? Co4 O24 Co6 98.94(10) . . ? C21 O21 Co4 131.7(2) . . ? C21 O21 Co6 129.8(2) . . ? Co4 O21 Co6 98.52(10) . . ? C31 O32 Co7 130.1(3) . . ? C31 O32 Co4 128.3(2) . . ? Co7 O32 Co4 100.51(10) . . ? C1 O2 Co8 125.0(2) . . ? C1 O2 Co3 132.8(2) . . ? Co8 O2 Co3 98.29(10) . . ? C34 O34 Co7 125.6(2) . . ? C34 O34 Co4 131.5(2) . . ? Co7 O34 Co4 99.68(11) . . ? C11 C12 C13 113.2(3) . 1_565 ? C51 O51 Co6 128.3(2) . . ? O1 C1 O2 123.5(4) . . ? O1 C1 C2 118.6(3) . . ? O2 C1 C2 117.8(3) . . ? O11 C11 O12 123.7(3) . 2_765 ? O11 C11 C12 118.2(3) . . ? O12 C11 C12 118.1(3) 2_765 . ? C11 O12 Co3 133.1(2) 2_765 . ? C11 O12 Co5 126.3(2) 2_765 . ? Co3 O12 Co5 98.07(10) . . ? O52 C51 O51 125.0(3) . . ? O52 C51 C52 118.2(3) . . ? O51 C51 C52 116.8(3) . . ? C34 C33 C32 115.9(3) 2_756 . ? O31 C31 O32 122.8(4) . . ? O31 C31 C32 120.9(3) . . ? O32 C31 C32 116.2(3) . . ? O23 C24 O24 124.4(4) . 2_756 ? O23 C24 C23 117.4(4) . . ? O24 C24 C23 117.9(4) 2_756 . ? O23 C24 C23A 116.3(6) . . ? O24 C24 C23A 118.8(5) 2_756 . ? C23 C24 C23A 12.8(6) . . ? C4 C3 C2 115.2(3) 2_765 . ? O14 C14 O13 124.4(3) . . ? O14 C14 C13 118.0(3) . . ? O13 C14 C13 117.6(3) . . ? O22 C21 O21 123.9(3) . . ? O22 C21 C22 118.9(3) . . ? O21 C21 C22 117.2(3) . . ? O42 C41 O41 125.1(3) . . ? O42 C41 C42 116.4(3) . . ? O41 C41 C42 118.4(3) . . ? C31 C32 C33 112.7(3) . . ? C43 C43 C42 114.6(4) 2_655 . ? C1 C2 C3 115.3(3) . . ? C53 C53 C52 113.7(4) 2_866 . ? O3 C4 O4 124.6(3) . . ? O3 C4 C3 117.4(3) . 2_765 ? O4 C4 C3 118.1(3) . 2_765 ? C41 C42 C43 110.3(3) . . ? C14 C13 C12 111.4(3) . 1_545 ? O33 C34 O34 124.0(3) . . ? O33 C34 C33 117.2(3) . 2_756 ? O34 C34 C33 118.8(3) . 2_756 ? C51 C52 C53 110.2(3) . . ? C23A C22 C21 119.5(11) 1_565 . ? C23A C22 C23 11.4(7) 1_565 1_565 ? C21 C22 C23 108.2(6) . 1_565 ? C22 C23A C24 119.0(8) 1_545 . ? C24 C23 C22 111.8(7) . 1_545 ? #==END #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_2a _database_code_depnum_ccdc_archive 'CCDC 836982' #TrackingRef '- Merged_deposit.cif' #0101022cosuccadirt _audit_creation_date 2011-03-22T09:48:02-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C6 H8 Co1 O4' _chemical_formula_sum 'C6 H8 Co O4' _chemical_formula_weight 203.05 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 2/c 1' _symmetry_space_group_name_Hall '-P 2yc' _symmetry_Int_Tables_number 13 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 16.1859(7) _cell_length_b 4.8014(2) _cell_length_c 9.2596(4) _cell_angle_alpha 90 _cell_angle_beta 90.191(4) _cell_angle_gamma 90 _cell_volume 719.60(6) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 1758 _cell_measurement_theta_min 3.331 _cell_measurement_theta_max 29.0062 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description sheet _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.1641 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.0323 _exptl_crystal_density_diffrn 1.874 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 412 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.341 _exptl_absorpt_correction_T_min 0.738 _exptl_absorpt_correction_T_max 0.929 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.41a (release 15-10-2010 CrysAlis171 .NET) (compiled Oct 15 2010,13:39:29) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_detector_area_resol_mean 16.1183 _diffrn_radiation_probe x-ray _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_unetI/netI 0.0642 _diffrn_reflns_number 3312 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -3 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.78 _diffrn_reflns_theta_max 29.07 _diffrn_reflns_theta_full 26.34 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.854 _reflns_number_total 1660 _reflns_number_gt 1419 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlisPro, Oxford Diffraction, 2010' _computing_cell_refinement 'CrysAlisPro, Oxford Diffraction, 2010' _computing_data_reduction 'CrysAlisPro, Oxford Diffraction, 2010' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond (Brandenburg 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0928P)^2^+6.8749P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 1660 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0939 _refine_ls_R_factor_gt 0.083 _refine_ls_wR_factor_ref 0.2361 _refine_ls_wR_factor_gt 0.2275 _refine_ls_goodness_of_fit_ref 1.185 _refine_ls_restrained_S_all 1.185 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.467 _refine_diff_density_min -0.788 _refine_diff_density_rms 0.19 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.24878(6) 0.0359(2) 0.77864(11) 0.0237(4) Uani 1 1 d . . . O3 O 0.2191(4) 0.4293(13) 0.7620(8) 0.0407(15) Uani 1 1 d . . . O1 O 0.2773(5) 0.0111(14) 0.9851(7) 0.0419(15) Uani 1 1 d . . . C6 C 0.1584(5) 0.5581(17) 0.7054(10) 0.0335(18) Uani 1 1 d . . . C4 C 0.0317(5) 0.5827(16) 0.5426(9) 0.0287(16) Uani 1 1 d . . . H4A H 0.0597 0.7095 0.4776 0.034 Uiso 1 1 calc R . . H4B H 0.0032 0.6939 0.6144 0.034 Uiso 1 1 calc R . . C3 C 0.4690(5) 0.4250(18) 1.0469(8) 0.0307(17) Uani 1 1 d . . . H3A H 0.4974 0.2818 1.1018 0.037 Uiso 1 1 calc R . . H3B H 0.4457 0.5565 1.1151 0.037 Uiso 1 1 calc R . . C1 C 0.3403(5) 0.1237(19) 1.0470(9) 0.0327(17) Uani 1 1 d . . . C2 C 0.3996(6) 0.292(2) 0.9618(9) 0.038(2) Uani 1 1 d . . . H2A H 0.3692 0.4384 0.9127 0.045 Uiso 1 1 calc R . . H2B H 0.4236 0.1737 0.8883 0.045 Uiso 1 1 calc R . . C5 C 0.0952(6) 0.4045(18) 0.6174(10) 0.038(2) Uani 1 1 d . . . H5A H 0.0666 0.275 0.6803 0.046 Uiso 1 1 calc R . . H5B H 0.1238 0.2956 0.5449 0.046 Uiso 1 1 calc R . . O2 O 0.3477(4) 0.1100(15) 1.1840(6) 0.0378(14) Uani 1 1 d . . . O4 O 0.1503(4) 0.8192(13) 0.7215(7) 0.0373(14) 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 0.0222(5) 0.0227(6) 0.0263(6) -0.0032(4) -0.0052(4) 0.0015(4) O3 0.033(3) 0.030(3) 0.059(4) -0.006(3) -0.022(3) 0.007(3) O1 0.048(4) 0.045(4) 0.033(3) 0.001(3) -0.009(3) -0.008(3) C6 0.032(4) 0.029(4) 0.040(4) 0.000(3) -0.013(3) -0.001(3) C4 0.027(4) 0.023(4) 0.035(4) -0.002(3) -0.015(3) -0.002(3) C3 0.036(4) 0.034(4) 0.022(3) 0.000(3) 0.001(3) -0.006(4) C1 0.036(4) 0.032(4) 0.030(4) -0.002(3) -0.008(3) -0.002(4) C2 0.040(5) 0.044(5) 0.028(4) 0.001(4) -0.006(3) -0.010(4) C5 0.037(5) 0.026(4) 0.051(5) -0.008(4) -0.019(4) 0.008(4) O2 0.030(3) 0.049(4) 0.034(3) 0.015(3) -0.005(2) -0.007(3) O4 0.026(3) 0.029(3) 0.057(4) -0.014(3) -0.015(3) 0.002(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O3 1.955(6) . ? Co1 O2 1.958(6) 4 ? Co1 O1 1.969(6) . ? Co1 O4 1.974(6) 1_545 ? O3 C6 1.272(10) . ? O1 C1 1.287(11) . ? C6 O4 1.269(10) . ? C6 C5 1.499(11) . ? C4 C5 1.504(11) . ? C4 C4 1.516(14) 3_566 ? C3 C2 1.511(11) . ? C3 C3 1.512(15) 3_667 ? C1 O2 1.275(10) . ? C1 C2 1.484(12) . ? O2 Co1 1.958(6) 4_556 ? O4 Co1 1.974(6) 1_565 ? 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 O2 120.8(3) . 4 ? O3 Co1 O1 101.0(3) . . ? O2 Co1 O1 102.9(3) 4 . ? O3 Co1 O4 106.9(3) . 1_545 ? O2 Co1 O4 110.6(3) 4 1_545 ? O1 Co1 O4 114.5(3) . 1_545 ? C6 O3 Co1 133.7(6) . . ? C1 O1 Co1 126.1(6) . . ? O4 C6 O3 120.8(8) . . ? O4 C6 C5 118.6(7) . . ? O3 C6 C5 120.6(7) . . ? C5 C4 C4 113.7(8) . 3_566 ? C2 C3 C3 113.3(8) . 3_667 ? O2 C1 O1 119.5(8) . . ? O2 C1 C2 119.8(7) . . ? O1 C1 C2 120.4(7) . . ? C1 C2 C3 115.7(7) . . ? C6 C5 C4 115.7(7) . . ? C1 O2 Co1 112.9(5) . 4_556 ? C6 O4 Co1 118.0(6) . 1_565 ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF