# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 182 _publ_contact_author_name 'Dr Mohamedally Kurmoo' _publ_contact_author_address ; Tectonique Moleculaire du Solide Universite Louis Pasteur 4 rue Blaise Pascal Strasbourg Alsace 67000 FRANCE ; _publ_contact_author_email KURMOO@CHIMIE.U-STRASBG.FR _publ_requested_journal 'Chemical Communications' _publ_section_title ; Reversible ferromagnetic-antiferromagnetic transformation upon dehydration-hydration of the nanoporous coordination framework, [Co3(OH)2(C4O4)2] 3H2O ; loop_ _publ_author_name _publ_author_address 'Kurmoo, Mohamedally' ; Laboratoire de Chimie de Coordination Organique, UMR7140-CNRS, Universite Louis Pasteur, Institut Le Bel, 4 rue Blaise Pascal, 67000 Strasbourg Cedex, France. ; 'Kumagai, Hitoshi' ; Applied Molecular Science, Institute for Molecular Science (IMS), Nishigounaka 38, Myoudaiji, Okazaki 444-8585, Japan. ; 'Chapman, Karena W.' ; School of Chemistry, F11 University of Sydney NSW 2006 Australia ; 'Kepert, Cameron J.' ; School of Chemistry, F11 University of Sydney NSW 2006 Australia ; _publ_section_abstract ; Reversible crystal-to-crystal transformation accompanied by ferromagnetic to antiferromagnetic ground states at 8 K upon dehydration-rehydration of the nanoporous coordination framework [CoII3(OH)2(C4O4)2]ï3H2O. ; _publ_section_references ; BrukerAXS, SMART, SAINT and XPREP. Area detector control and data integration and reduction software. 1995: Bruker Analytical X-ray Instruments Inc.: Madison, Wisconsin, USA. Sheldrick, G.M., SHELXS97. Program for crystal structure solution. 1997: University of Gottingen, Germany. Sheldrick, G.M., SHELXL97. Program for crystal structure refinement. 1997: University of Gottingen, Germany. Sheldrick, G.M., CIFTAB. Program for generation of crystallographic tables. 1997: University of Gottingen, Germany. Zsolnai, L., Huttner G., XPMA. 1994: University of Heidelberg, Germany. ; data_A.3{H2O},150K _database_code_depnum_ccdc_archive 'CCDC 261656' _audit_creation_method SHELXL-97 _chemical_name_systematic ; cobalt squarate hydroxide hydrate ; _chemical_name_common 'cobalt squarate hydroxide hydrate' _chemical_melting_point ? _chemical_formula_moiety 'C8 H2 Co3 O10, H6 O3' _chemical_formula_sum 'C8 H8 Co3 O13' _chemical_formula_weight 488.94 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m _symmetry_Int_tables_number 12 _symmetry_space_group_name_Hall '-C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 9.2966(10) _cell_length_b 12.8636(13) _cell_length_c 5.4998(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.533(2) _cell_angle_gamma 90.00 _cell_volume 657.68(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 840 _cell_measurement_theta_min 2.7035 _cell_measurement_theta_max 27.75 _exptl_crystal_description parallelepiped _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 482 _exptl_absorpt_coefficient_mu 3.816 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.669 _exptl_absorpt_correction_T_max 0.737 _exptl_absorpt_process_details 'XPREP (BruckerASX)' _exptl_special_details ; 'Secured in a 0.3mm Lindemann glass capillary with thin film of grease' ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Brucker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 38 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 6567 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_sigmaI/netI 0.0193 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 27.95 _reflns_number_total 810 _reflns_number_gt 714 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BrukerAXS)' _computing_cell_refinement 'SMART (BrukerAXS)' _computing_data_reduction 'SAINT+ (BrukerAXS)' _computing_structure_solution 'SHELXS-97 (Sheldrick)' _computing_structure_refinement 'SHELXL-97 (Sheldrick)' _computing_molecular_graphics 'XPMA ' _computing_publication_material 'CIFTAB (Sheldrick)' _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. The structure consists of slightly buckled brucite strips which run parallel to the c-axis, bridged in the ab-plane by the mu4-squarate anion. This defines channels in the structure with contain noncoordinated guest water molecules which have extensive hydrogen bonding interactions with the framework. All non-hydrogen atoms were located from the difference map and modelled with anisotropic atomic displacement parameters. Hydrogen atoms were located in the difference map and refined isotropically, constraining the atomic displacement parameter to be 1.2 or 1.5 times that of the non-hydrogen atom to which they are bonded for framework and guest atoms respectively. ; _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^)+(0.0225P)^2^+4.0019P] where P=(Fo^2^+2Fc^2^)/3' ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 810 _refine_ls_number_parameters 64 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0655 _refine_ls_wR_factor_gt 0.0617 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _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 0.5000 0.5000 0.5000 0.00583(17) Uani 1 4 d S . . Co2 Co 0.5000 0.37986(4) 0.0000 0.00655(15) Uani 1 2 d S . . O1 O 0.3807(2) 0.26264(15) 0.1508(3) 0.0112(4) Uani 1 1 d . . . O11 O 0.3979(3) 0.5000 0.1739(5) 0.0082(5) Uani 1 2 d S . . H11 H 0.318(6) 0.5000 0.156(9) 0.010 Uiso 1 2 d S . . C1 C 0.3098(3) 0.2575(2) 0.3415(4) 0.0093(5) Uani 1 1 d . . . O2 O 0.3688(2) 0.38810(14) 0.6715(3) 0.0091(4) Uani 1 1 d . . . C2 C 0.3039(3) 0.3121(2) 0.5754(4) 0.0080(5) Uani 1 1 d . . . O21 O 0.1083(6) 0.4393(4) 0.0999(10) 0.0365(12) Uiso 0.50 1 d PG . . H21A H 0.0659 0.4386 0.2397 0.044 Uiso 0.50 1 d PG . . H21B H 0.1030 0.3818 0.0185 0.044 Uiso 0.50 1 d PG . . O31 O 0.0739(10) 0.5000 0.5785(17) 0.053(2) Uiso 0.50 2 d SP . . 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 0.0073(3) 0.0055(3) 0.0047(3) 0.000 0.0005(2) 0.000 Co2 0.0092(3) 0.0051(2) 0.0054(2) 0.000 0.00145(17) 0.000 O1 0.0148(10) 0.0104(9) 0.0085(8) -0.0011(7) 0.0044(7) -0.0027(7) O11 0.0051(12) 0.0112(13) 0.0083(12) 0.000 -0.0009(9) 0.000 C1 0.0100(12) 0.0077(12) 0.0103(11) -0.0001(9) -0.0011(9) 0.0001(10) O2 0.0110(9) 0.0080(9) 0.0082(8) -0.0003(7) -0.0001(7) -0.0032(7) C2 0.0086(11) 0.0085(11) 0.0069(11) 0.0009(9) 0.0002(9) -0.0001(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O11 2.021(3) 5_666 ? Co1 O11 2.021(3) . ? Co1 O2 2.1144(18) 2_656 ? Co1 O2 2.1144(18) . ? Co1 O2 2.1144(18) 6_565 ? Co1 O2 2.1144(18) 5_666 ? Co2 O1 2.0514(19) 2_655 ? Co2 O1 2.0514(19) . ? Co2 O11 2.0545(18) . ? Co2 O11 2.0545(18) 5_665 ? Co2 O2 2.1731(18) 1_554 ? Co2 O2 2.1731(18) 2_656 ? O1 C1 1.246(3) . ? O11 Co2 2.0545(18) 5_665 ? O11 H11 0.74(5) . ? C1 C2 1.462(3) 7_556 ? C1 C2 1.467(3) . ? O2 C2 1.262(3) . ? O2 Co2 2.1731(18) 1_556 ? C2 C1 1.462(3) 7_556 ? O21 O21 1.561(11) 6_565 ? O21 H21A 0.8674 . ? O21 H21B 0.8661 . ? O31 O31 1.616(19) 5_566 ? 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 O11 Co1 O11 180.0 5_666 . ? O11 Co1 O2 97.34(8) 5_666 2_656 ? O11 Co1 O2 82.66(8) . 2_656 ? O11 Co1 O2 82.66(8) 5_666 . ? O11 Co1 O2 97.34(8) . . ? O2 Co1 O2 94.19(10) 2_656 . ? O11 Co1 O2 82.66(8) 5_666 6_565 ? O11 Co1 O2 97.34(8) . 6_565 ? O2 Co1 O2 180.0 2_656 6_565 ? O2 Co1 O2 85.81(10) . 6_565 ? O11 Co1 O2 97.34(8) 5_666 5_666 ? O11 Co1 O2 82.66(8) . 5_666 ? O2 Co1 O2 85.81(10) 2_656 5_666 ? O2 Co1 O2 180.00(7) . 5_666 ? O2 Co1 O2 94.19(10) 6_565 5_666 ? O1 Co2 O1 85.38(10) 2_655 . ? O1 Co2 O11 174.23(9) 2_655 . ? O1 Co2 O11 96.37(8) . . ? O1 Co2 O11 96.37(8) 2_655 5_665 ? O1 Co2 O11 174.23(9) . 5_665 ? O11 Co2 O11 82.43(11) . 5_665 ? O1 Co2 O2 90.07(7) 2_655 1_554 ? O1 Co2 O2 94.05(7) . 1_554 ? O11 Co2 O2 95.29(9) . 1_554 ? O11 Co2 O2 80.47(9) 5_665 1_554 ? O1 Co2 O2 94.05(7) 2_655 2_656 ? O1 Co2 O2 90.07(7) . 2_656 ? O11 Co2 O2 80.47(9) . 2_656 ? O11 Co2 O2 95.29(9) 5_665 2_656 ? O2 Co2 O2 174.40(10) 1_554 2_656 ? C1 O1 Co2 132.21(17) . . ? Co1 O11 Co2 101.41(10) . . ? Co1 O11 Co2 101.41(10) . 5_665 ? Co2 O11 Co2 97.57(11) . 5_665 ? Co1 O11 H11 125(4) . . ? Co2 O11 H11 114(2) . . ? Co2 O11 H11 114(2) 5_665 . ? O1 C1 C2 133.3(2) . 7_556 ? O1 C1 C2 137.5(2) . . ? C2 C1 C2 89.2(2) 7_556 . ? C2 O2 Co1 128.01(16) . . ? C2 O2 Co2 124.94(16) . 1_556 ? Co1 O2 Co2 94.73(7) . 1_556 ? O2 C2 C1 133.4(2) . 7_556 ? O2 C2 C1 135.8(2) . . ? C1 C2 C1 90.8(2) 7_556 . ? O21 O21 H21A 90.6 6_565 . ? O21 O21 H21B 148.7 6_565 . ? H21A O21 H21B 115.2 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O11 H11 O21 0.74(5) 2.12(5) 2.829(6) 158.4(6) . O11 H11 O21 0.74(5) 2.12(5) 2.829(6) 158.4(6) 6_565 O21 H21A O31 0.87 1.83 2.581(11) 144.3 5_566 O21 H21A O31 0.87 2.02 2.767(10) 143.0 . O21 H21B O1 0.87 2.08 2.943(6) 171.4 7 _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 27.95 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.781 _refine_diff_density_min -0.623 _refine_diff_density_rms 0.109 #===END data_A,100K _database_code_depnum_ccdc_archive 'CCDC 261657' _publ_section_abstract ; Reversible crystal-to-crystal transformation accompanied by ferromagnetic to antiferromagnetic ground states at 8 K upon dehydration-rehydration of the nanoporous coordination framework [CoII3(OH)2(C4O4)2]ï3H2O. ; _publ_section_references ; BrukerAXS, SMART, SAINT and XPREP. Area detector control and data integration and reduction software. 1995: Bruker Analytical X-ray Instruments Inc.: Madison, Wisconsin, USA. Sheldrick, G.M., SHELXS97. Program for crystal structure solution. 1997: University of Gottingen, Germany. Sheldrick, G.M., SHELXL97. Program for crystal structure refinement. 1997: University of Gottingen, Germany. Sheldrick, G.M., CIFTAB. Program for generation of crystallographic tables. 1997: University of Gottingen, Germany. Zsolnai, L., Huttner G., XPMA. 1994: University of Heidelberg, Germany. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; cobalt squarate hydroxide ; _chemical_name_common 'cobalt squarate hydroxide' _chemical_melting_point ? _chemical_formula_moiety 'C8 H2 Co3 O10' _chemical_formula_sum 'C8 H2 Co3 O10' _chemical_formula_weight 434.89 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m _symmetry_Int_tables_number 12 _symmetry_space_group_name_Hall '-C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 9.4684(11) _cell_length_b 12.7225(15) _cell_length_c 5.4873(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.314(2) _cell_angle_gamma 90.00 _cell_volume 661.00(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 574 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 28.417 _exptl_crystal_description parallelepiped _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.185 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 422 _exptl_absorpt_coefficient_mu 3.766 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.672 _exptl_absorpt_correction_T_max 0.740 _exptl_absorpt_process_details 'XPREP (BruckerASX)' _exptl_special_details ; Secured in a 0.3mm Lindemann glass capillary with thin film of grease ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Brucker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 21 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 2647 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0243 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 27.98 _reflns_number_total 813 _reflns_number_gt 681 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BrukerAXS)' _computing_cell_refinement 'SMART (BrukerAXS)' _computing_data_reduction 'SAINT+ (BrukerAXS)' _computing_structure_solution 'SHELXS-97 (Sheldrick)' _computing_structure_refinement 'SHELXL-97 (Sheldrick)' _computing_molecular_graphics 'XPMA ' _computing_publication_material 'CIFTAB (Sheldrick)' _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. The structure consists of slightly buckled brucite strips which run parallel to the c-axis, bridged in the ab-plane by the mu4-squarate anion. All non-hydrogen atoms were located from the difference map and modelled with anisotropic atomic displacement parameters. Hydrogen atoms were located in the difference map and refined isotropically, constraining the atomic displacement parameter to be 1.2 times that of O11, the non-hydrogen atom to which it is bonded. ; _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^)+(0.0173P)^2^+3.6348P] where P=(Fo^2^+2Fc^2^)/3' ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 813 _refine_ls_number_parameters 54 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0360 _refine_ls_R_factor_gt 0.0249 _refine_ls_wR_factor_ref 0.0598 _refine_ls_wR_factor_gt 0.0538 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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 0.5000 0.5000 0.5000 0.00488(16) Uani 1 4 d S . . Co2 Co 0.5000 0.37601(3) 0.0000 0.00556(14) Uani 1 2 d S . . O1 O 0.37751(17) 0.26220(13) 0.1478(3) 0.0085(3) Uani 1 1 d . . . O11 O 0.3995(3) 0.5000 0.1726(4) 0.0068(5) Uani 1 2 d S . . H11 H 0.329(5) 0.5000 0.158(8) 0.008 Uiso 1 2 d S . . C1 C 0.3081(2) 0.25720(19) 0.3396(4) 0.0072(4) Uani 1 1 d . . . O2 O 0.37308(18) 0.38656(13) 0.6723(3) 0.0075(3) Uani 1 1 d . . . C2 C 0.3054(2) 0.31136(18) 0.5760(4) 0.0067(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 0.0062(3) 0.0052(3) 0.0033(3) 0.000 0.0005(2) 0.000 Co2 0.0065(2) 0.0056(2) 0.0045(2) 0.000 0.00137(16) 0.000 O1 0.0086(9) 0.0095(8) 0.0074(7) 0.0005(6) 0.0039(6) -0.0016(7) O11 0.0043(11) 0.0082(11) 0.0079(11) 0.000 0.0002(9) 0.000 C1 0.0074(11) 0.0074(11) 0.0069(10) 0.0000(9) -0.0008(8) 0.0015(9) O2 0.0091(9) 0.0078(8) 0.0055(7) -0.0006(6) -0.0005(6) -0.0027(6) C2 0.0079(11) 0.0072(11) 0.0049(10) 0.0013(8) 0.0004(8) 0.0030(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O11 2.028(2) . ? Co1 O11 2.028(2) 5_666 ? Co1 O2 2.1055(17) . ? Co1 O2 2.1055(17) 2_656 ? Co1 O2 2.1055(17) 5_666 ? Co1 O2 2.1055(17) 6_565 ? Co2 O1 2.0271(17) . ? Co2 O1 2.0271(17) 2_655 ? Co2 O11 2.0739(17) . ? Co2 O11 2.0739(17) 5_665 ? Co2 O2 2.1617(15) 2_656 ? Co2 O2 2.1617(15) 1_554 ? O1 C1 1.246(3) . ? O11 Co2 2.0739(17) 5_665 ? O11 H11 0.67(4) . ? C1 C2 1.462(3) 7_556 ? C1 C2 1.469(3) . ? O2 C2 1.265(3) . ? O2 Co2 2.1617(15) 1_556 ? C2 C1 1.462(3) 7_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Co1 O11 180.0 . 5_666 ? O11 Co1 O2 97.55(7) . . ? O11 Co1 O2 82.45(7) 5_666 . ? O11 Co1 O2 82.45(7) . 2_656 ? O11 Co1 O2 97.55(7) 5_666 2_656 ? O2 Co1 O2 93.45(9) . 2_656 ? O11 Co1 O2 82.45(7) . 5_666 ? O11 Co1 O2 97.55(7) 5_666 5_666 ? O2 Co1 O2 180.0 . 5_666 ? O2 Co1 O2 86.55(9) 2_656 5_666 ? O11 Co1 O2 97.55(7) . 6_565 ? O11 Co1 O2 82.45(7) 5_666 6_565 ? O2 Co1 O2 86.55(9) . 6_565 ? O2 Co1 O2 180.00(7) 2_656 6_565 ? O2 Co1 O2 93.45(9) 5_666 6_565 ? O1 Co2 O1 88.83(9) . 2_655 ? O1 Co2 O11 95.49(7) . . ? O1 Co2 O11 172.28(8) 2_655 . ? O1 Co2 O11 172.28(8) . 5_665 ? O1 Co2 O11 95.49(7) 2_655 5_665 ? O11 Co2 O11 80.96(11) . 5_665 ? O1 Co2 O2 91.62(6) . 2_656 ? O1 Co2 O2 93.46(6) 2_655 2_656 ? O11 Co2 O2 80.04(8) . 2_656 ? O11 Co2 O2 94.50(8) 5_665 2_656 ? O1 Co2 O2 93.46(6) . 1_554 ? O1 Co2 O2 91.62(6) 2_655 1_554 ? O11 Co2 O2 94.50(8) . 1_554 ? O11 Co2 O2 80.05(8) 5_665 1_554 ? O2 Co2 O2 172.88(9) 2_656 1_554 ? C1 O1 Co2 132.86(16) . . ? Co1 O11 Co2 100.97(9) . 5_665 ? Co1 O11 Co2 100.97(9) . . ? Co2 O11 Co2 99.03(11) 5_665 . ? Co1 O11 H11 125(4) . . ? Co2 O11 H11 114(2) 5_665 . ? Co2 O11 H11 114(2) . . ? O1 C1 C2 133.7(2) . 7_556 ? O1 C1 C2 137.2(2) . . ? C2 C1 C2 89.07(18) 7_556 . ? C2 O2 Co1 128.29(14) . . ? C2 O2 Co2 125.33(14) . 1_556 ? Co1 O2 Co2 95.74(6) . 1_556 ? O2 C2 C1 133.6(2) . 7_556 ? O2 C2 C1 135.4(2) . . ? C1 C2 C1 90.93(18) 7_556 . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 27.98 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.466 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.107