# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global #================================================= # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Professor Susumu Kitagawa Department of Synthetic Chemistry and Biological Chemistry Graduate School of Engineering Kyoto University Katsura, Nishikyo-ku, Kyoto 615-8510 Japan ; _publ_contact_author_phone 81-75-383-2736 _publ_contact_author_fax 81-75-383-2732 _publ_contact_author_email kitagawa@sbchem.kyoto-u.ac.jp _publ_requested_journal 'Chem. Commun.' _publ_requested_coeditor_name ? _publ_contact_letter ; Dear Sir or Madam: Please consider this CIF as supplmentary data for a manuscript submitted to Chem. Commun. Susumu Kitagawa ; #================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_coden_Cambridge 182 _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? #======================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Temperature-controlled hydrothermal synthesis of a 2D ferromagnetic coordination bilayered polymer and a novel 3D network with inorganic Co3(OH)2 ferrimagnetic chains ; loop_ _publ_author_name _publ_author_address 'Tong, Ming-Liang' ; School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou 510275 P. R. China ; 'Kitagawa, Susumu' ; Department of Synthetic Chemistry and Biological Chemistry Graduate School of Engineering Kyoto University Kitsura, Nishikyo-ku, Kyoto 615-8510 Japan ; 'Chang, Ho-Chol' ; Department of Synthetic Chemistry and Biological Chemistry Graduate School of Engineering Kyoto University Kitsura, Nishikyo-ku, Kyoto 615-8510 Japan ; 'Ohba, Masaaki' ; Department of Synthetic Chemistry and Biological Chemistry Graduate School of Engineering Kyoto University Kitsura, Nishikyo-ku, Kyoto 615-8510 Japan ; #============================================================ data_complex_1 _database_code_CSD 221040 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H9 Co N O7' _chemical_formula_weight 278.08 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.1114(7) _cell_length_b 7.8730(10) _cell_length_c 9.0284(10) _cell_angle_alpha 76.627(14) _cell_angle_beta 68.437(11) _cell_angle_gamma 76.232(14) _cell_volume 450.77(9) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.049 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 282 _exptl_absorpt_coefficient_mu 1.927 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3086 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 27.63 _reflns_number_total 1844 _reflns_number_gt 1631 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0276P)^2^+0.3729P] 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 1844 _refine_ls_number_parameters 169 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0829 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.082 _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 0.01772(6) 0.24214(5) 0.28290(4) 0.01150(13) Uani 1 1 d . . . O1 O -0.7675(3) 0.3825(2) 0.2637(3) 0.0176(5) Uani 1 1 d . . . O2 O -0.8072(3) 0.6601(3) 0.1236(2) 0.0169(5) Uani 1 1 d . . . O3 O -0.9347(3) 0.8041(2) 0.4508(2) 0.0122(4) Uani 1 1 d . . . O4 O -0.7484(3) 1.0109(2) 0.2794(2) 0.0129(4) Uani 1 1 d . . . O1W O 0.0927(3) 0.2508(3) 0.0371(2) 0.0187(5) Uani 1 1 d D . . H1WA H 0.175(4) 0.161(3) 0.001(4) 0.031(11) Uiso 1 1 d D . . H1WB H 0.020(5) 0.299(4) -0.023(4) 0.054(14) Uiso 1 1 d D . . O2W O -0.1935(3) 0.0668(3) 0.3367(3) 0.0156(4) Uani 1 1 d D . . H2WA H -0.221(5) 0.052(4) 0.257(3) 0.031(11) Uiso 1 1 d D . . H2WB H -0.135(6) -0.031(3) 0.377(4) 0.056(14) Uiso 1 1 d D . . O3W O 0.3318(3) -0.0473(3) -0.0912(3) 0.0181(5) Uani 1 1 d D . . H3WA H 0.306(4) -0.133(3) -0.015(3) 0.026(10) Uiso 1 1 d D . . H3WB H 0.4604(18) -0.054(4) -0.137(4) 0.030(10) Uiso 1 1 d D . . N1 N -0.2269(3) 0.4569(3) 0.2887(3) 0.0103(5) Uani 1 1 d . . . C1 C -0.3794(4) 0.4482(3) 0.2390(3) 0.0120(6) Uani 1 1 d . . . H1A H -0.3648 0.3524 0.1894 0.014 Uiso 1 1 calc R . . C2 C -0.5572(4) 0.5718(3) 0.2562(3) 0.0100(5) Uani 1 1 d . . . C3 C -0.7252(4) 0.5377(4) 0.2088(3) 0.0125(6) Uani 1 1 d . . . C4 C -0.5778(4) 0.7173(3) 0.3262(3) 0.0102(6) Uani 1 1 d . . . C5 C -0.7693(4) 0.8552(4) 0.3544(3) 0.0112(6) Uani 1 1 d . . . C6 C -0.4205(4) 0.7269(3) 0.3796(3) 0.0120(6) Uani 1 1 d . . . H6 H -0.4307 0.8222 0.4284 0.014 Uiso 1 1 calc R . . C7 C -0.2512(4) 0.5967(4) 0.3604(3) 0.0119(6) Uani 1 1 d . . . H7 H -0.1490 0.6049 0.3983 0.014 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 Co1 0.0106(2) 0.0107(2) 0.0155(2) -0.00177(15) -0.00788(16) -0.00046(15) O1 0.0153(11) 0.0122(10) 0.0295(12) -0.0005(9) -0.0130(9) -0.0036(9) O2 0.0181(11) 0.0170(10) 0.0197(10) 0.0023(9) -0.0142(9) -0.0028(9) O3 0.0086(10) 0.0150(10) 0.0139(10) -0.0016(8) -0.0053(8) -0.0016(8) O4 0.0119(10) 0.0102(10) 0.0165(10) -0.0009(8) -0.0069(8) 0.0003(8) O1W 0.0170(12) 0.0238(12) 0.0164(11) -0.0067(9) -0.0102(9) 0.0054(10) O2W 0.0178(11) 0.0129(10) 0.0216(11) -0.0008(9) -0.0142(9) -0.0022(9) O3W 0.0181(12) 0.0169(11) 0.0188(11) 0.0013(9) -0.0080(9) -0.0027(9) N1 0.0086(12) 0.0115(11) 0.0117(11) 0.0005(9) -0.0070(9) 0.0003(9) C1 0.0152(15) 0.0106(13) 0.0132(13) -0.0017(11) -0.0081(11) -0.0024(11) C2 0.0103(14) 0.0099(13) 0.0105(12) 0.0009(10) -0.0059(11) -0.0013(11) C3 0.0111(14) 0.0174(15) 0.0107(13) -0.0054(11) -0.0049(11) -0.0004(12) C4 0.0099(14) 0.0097(13) 0.0105(12) 0.0022(10) -0.0046(11) -0.0024(11) C5 0.0143(15) 0.0131(14) 0.0111(13) -0.0050(11) -0.0105(11) 0.0017(12) C6 0.0138(15) 0.0100(13) 0.0141(13) -0.0004(11) -0.0069(11) -0.0031(11) C7 0.0124(14) 0.0149(14) 0.0118(13) 0.0000(11) -0.0085(11) -0.0032(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.026(2) 1_655 ? Co1 O1W 2.072(2) . ? Co1 N1 2.112(2) . ? Co1 O2W 2.130(2) . ? Co1 O4 2.1514(19) 1_645 ? Co1 O3 2.2171(19) 2_466 ? O1 C3 1.270(3) . ? O1 Co1 2.026(2) 1_455 ? O2 C3 1.257(3) . ? O3 C5 1.270(3) . ? O3 Co1 2.2171(19) 2_466 ? O4 C5 1.269(3) . ? O4 Co1 2.1515(19) 1_465 ? O1W H1WA 0.845(10) . ? O1W H1WB 0.846(10) . ? O2W H2WA 0.847(10) . ? O2W H2WB 0.851(10) . ? O3W H3WA 0.846(10) . ? O3W H3WB 0.848(10) . ? N1 C1 1.337(3) . ? N1 C7 1.348(4) . ? C1 C2 1.381(4) . ? C1 H1A 0.9300 . ? C2 C4 1.386(4) . ? C2 C3 1.505(4) . ? C4 C6 1.394(4) . ? C4 C5 1.506(4) . ? C6 C7 1.368(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O1W 95.60(9) 1_655 . ? O1 Co1 N1 97.45(8) 1_655 . ? O1W Co1 N1 92.35(9) . . ? O1 Co1 O2W 170.20(8) 1_655 . ? O1W Co1 O2W 91.79(9) . . ? N1 Co1 O2W 88.65(8) . . ? O1 Co1 O4 86.70(8) 1_655 1_645 ? O1W Co1 O4 87.44(8) . 1_645 ? N1 Co1 O4 175.84(8) . 1_645 ? O2W Co1 O4 87.20(8) . 1_645 ? O1 Co1 O3 89.91(8) 1_655 2_466 ? O1W Co1 O3 172.49(8) . 2_466 ? N1 Co1 O3 91.99(8) . 2_466 ? O2W Co1 O3 82.19(8) . 2_466 ? O4 Co1 O3 87.79(7) 1_645 2_466 ? C3 O1 Co1 139.1(2) . 1_455 ? C5 O3 Co1 123.81(17) . 2_466 ? C5 O4 Co1 128.01(18) . 1_465 ? Co1 O1W H1WA 114(2) . . ? Co1 O1W H1WB 129(2) . . ? H1WA O1W H1WB 110.4(17) . . ? Co1 O2W H2WA 116(2) . . ? Co1 O2W H2WB 104(3) . . ? H2WA O2W H2WB 109.5(16) . . ? H3WA O3W H3WB 110.0(16) . . ? C1 N1 C7 116.8(2) . . ? C1 N1 Co1 120.41(18) . . ? C7 N1 Co1 122.24(19) . . ? N1 C1 C2 124.5(2) . . ? N1 C1 H1A 117.7 . . ? C2 C1 H1A 117.7 . . ? C1 C2 C4 118.1(3) . . ? C1 C2 C3 119.1(2) . . ? C4 C2 C3 122.7(2) . . ? O2 C3 O1 127.7(3) . . ? O2 C3 C2 118.8(2) . . ? O1 C3 C2 113.5(2) . . ? C2 C4 C6 117.8(3) . . ? C2 C4 C5 121.6(2) . . ? C6 C4 C5 120.5(2) . . ? O4 C5 O3 126.7(3) . . ? O4 C5 C4 116.5(2) . . ? O3 C5 C4 116.8(2) . . ? C7 C6 C4 120.2(3) . . ? C7 C6 H6 119.9 . . ? C4 C6 H6 119.9 . . ? N1 C7 C6 122.5(3) . . ? N1 C7 H7 118.7 . . ? C6 C7 H7 118.7 . . ? 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 O1 Co1 N1 C1 153.9(2) 1_655 . . . ? O1W Co1 N1 C1 57.9(2) . . . . ? O2W Co1 N1 C1 -33.8(2) . . . . ? O4 Co1 N1 C1 -29.1(12) 1_645 . . . ? O3 Co1 N1 C1 -115.9(2) 2_466 . . . ? O1 Co1 N1 C7 -34.9(2) 1_655 . . . ? O1W Co1 N1 C7 -130.8(2) . . . . ? O2W Co1 N1 C7 137.5(2) . . . . ? O4 Co1 N1 C7 142.2(10) 1_645 . . . ? O3 Co1 N1 C7 55.3(2) 2_466 . . . ? C7 N1 C1 C2 0.1(4) . . . . ? Co1 N1 C1 C2 171.8(2) . . . . ? N1 C1 C2 C4 1.6(4) . . . . ? N1 C1 C2 C3 -174.4(2) . . . . ? Co1 O1 C3 O2 -9.3(5) 1_455 . . . ? Co1 O1 C3 C2 170.19(19) 1_455 . . . ? C1 C2 C3 O2 -133.1(3) . . . . ? C4 C2 C3 O2 51.0(4) . . . . ? C1 C2 C3 O1 47.3(3) . . . . ? C4 C2 C3 O1 -128.5(3) . . . . ? C1 C2 C4 C6 -2.0(4) . . . . ? C3 C2 C4 C6 173.9(2) . . . . ? C1 C2 C4 C5 -178.0(2) . . . . ? C3 C2 C4 C5 -2.1(4) . . . . ? Co1 O4 C5 O3 -1.5(4) 1_465 . . . ? Co1 O4 C5 C4 178.67(16) 1_465 . . . ? Co1 O3 C5 O4 -102.1(3) 2_466 . . . ? Co1 O3 C5 C4 77.7(3) 2_466 . . . ? C2 C4 C5 O4 -117.2(3) . . . . ? C6 C4 C5 O4 66.9(3) . . . . ? C2 C4 C5 O3 63.0(3) . . . . ? C6 C4 C5 O3 -112.9(3) . . . . ? C2 C4 C6 C7 0.9(4) . . . . ? C5 C4 C6 C7 176.9(2) . . . . ? C1 N1 C7 C6 -1.4(4) . . . . ? Co1 N1 C7 C6 -172.92(19) . . . . ? C4 C6 C7 N1 0.9(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O3W 0.845(10) 1.928(12) 2.767(3) 172(3) . O1W H1WB O2 0.846(10) 1.970(18) 2.781(3) 160(4) 2_465 O2W H2WA O3W 0.847(10) 1.946(11) 2.782(3) 169(3) 2 O2W H2WB O3 0.851(10) 1.894(17) 2.706(3) 159(4) 1_645 O3W H3WA O2 0.846(10) 1.949(13) 2.766(3) 162(3) 1_645 O3W H3WB O4 0.848(10) 2.040(11) 2.868(3) 165(3) 2_565 _diffrn_measured_fraction_theta_max 0.878 _diffrn_reflns_theta_full 27.63 _diffrn_measured_fraction_theta_full 0.878 _refine_diff_density_max 0.529 _refine_diff_density_min -0.632 _refine_diff_density_rms 0.098 #=================================================END data_complex2 _database_code_CSD 221041 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H12 Co3 N2 O12' _chemical_formula_weight 577.05 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.5875(14) _cell_length_b 6.7860(15) _cell_length_c 9.975(2) _cell_angle_alpha 76.123(15) _cell_angle_beta 71.782(14) _cell_angle_gamma 77.067(16) _cell_volume 405.80(15) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 287 _exptl_absorpt_coefficient_mu 3.112 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.4359 _exptl_absorpt_correction_T_max 0.5749 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1620 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 27.00 _reflns_number_total 1620 _reflns_number_gt 1410 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0871P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1620 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0480 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1160 _refine_ls_wR_factor_gt 0.1123 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.46522(6) 0.47634(6) 0.15804(4) 0.0072(2) Uani 1 d . . . Co2 Co 0.5000 1.0000 0.0000 0.0058(2) Uani 1 d S . . O1 O 0.5863(4) 0.6881(3) -0.0254(2) 0.0073(5) Uani 1 d . . . O2 O 0.1477(4) 0.6580(4) 0.1533(2) 0.0106(5) Uani 1 d . . . O3 O 0.2034(4) 0.9684(4) 0.1620(2) 0.0110(5) Uani 1 d . . . O4 O -0.3246(4) 0.9220(4) 0.1582(2) 0.0101(5) Uani 1 d . . . H1O1 H 0.698(7) 0.676(7) -0.039(5) 0.006(11) Uiso 1 d . . . O5 O -0.4759(4) 0.6444(4) 0.2861(2) 0.0108(5) Uani 1 d . . . O1W O 0.7809(4) 0.2998(4) 0.1382(3) 0.0144(5) Uani 1 d . . . H1WA H 0.757(7) 0.183(9) 0.167(5) 0.022(12) Uiso 1 d . . . H1WB H 0.815(10) 0.316(11) 0.053(8) 0.053(19) Uiso 1 d . . . N1 N -0.3040(4) 0.6938(4) 0.6401(3) 0.0091(6) Uani 1 d . . . C1 C -0.3806(5) 0.7189(5) 0.5260(3) 0.0085(6) Uani 1 d . . . H1 H -0.5232 0.7015 0.5433 0.010 Uiso 1 calc R . . C2 C -0.2615(5) 0.7690(5) 0.3841(3) 0.0073(6) Uani 1 d . . . C3 C -0.3603(5) 0.7793(5) 0.2656(3) 0.0067(6) Uani 1 d . . . C4 C -0.0469(5) 0.7969(5) 0.3583(3) 0.0065(6) Uani 1 d . . . C5 C 0.1121(5) 0.8137(5) 0.2097(3) 0.0078(6) Uani 1 d . . . C6 C 0.0308(5) 0.7778(5) 0.4761(4) 0.0109(7) Uani 1 d . . . H6 H 0.1706 0.8004 0.4625 0.013 Uiso 1 calc R . . C7 C -0.0999(5) 0.7253(5) 0.6135(4) 0.0095(7) Uani 1 d . . . H7 H -0.0441 0.7111 0.6907 0.011 Uiso 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 Co1 0.0087(3) 0.0072(3) 0.0050(3) 0.00146(18) -0.00182(19) -0.00259(18) Co2 0.0062(3) 0.0054(3) 0.0046(3) 0.0024(2) -0.0016(2) -0.0019(2) O1 0.0067(12) 0.0062(11) 0.0078(11) 0.0003(8) -0.0012(9) -0.0015(9) O2 0.0107(11) 0.0104(11) 0.0085(11) -0.0005(9) -0.0008(9) -0.0013(9) O3 0.0091(11) 0.0101(11) 0.0107(12) 0.0017(9) 0.0006(9) -0.0038(9) O4 0.0122(11) 0.0096(11) 0.0083(11) 0.0043(9) -0.0049(9) -0.0047(9) O5 0.0147(12) 0.0102(11) 0.0086(11) 0.0016(9) -0.0039(9) -0.0068(9) O1W 0.0168(13) 0.0103(13) 0.0162(14) -0.0003(11) -0.0082(11) 0.0004(10) N1 0.0110(13) 0.0078(13) 0.0085(13) 0.0016(10) -0.0044(11) -0.0024(10) C1 0.0086(14) 0.0081(15) 0.0073(15) 0.0001(12) -0.0020(12) -0.0004(12) C2 0.0076(14) 0.0052(14) 0.0068(15) 0.0018(11) -0.0007(12) -0.0016(11) C3 0.0062(14) 0.0061(14) 0.0060(14) 0.0010(11) -0.0005(12) -0.0011(11) C4 0.0057(14) 0.0045(14) 0.0080(15) -0.0014(11) 0.0002(12) -0.0007(11) C5 0.0044(14) 0.0105(15) 0.0048(14) 0.0029(12) 0.0003(12) -0.0006(12) C6 0.0106(16) 0.0117(16) 0.0110(16) 0.0015(13) -0.0044(13) -0.0043(12) C7 0.0111(16) 0.0109(16) 0.0073(15) 0.0004(12) -0.0034(13) -0.0046(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.066(2) 2_665 ? Co1 O5 2.071(2) 1_655 ? Co1 O1 2.095(2) . ? Co1 O1W 2.131(3) . ? Co1 N1 2.148(3) 2_566 ? Co1 O2 2.186(2) . ? Co1 Co1 2.9884(10) 2_665 ? Co2 O1 2.120(2) 2_675 ? Co2 O1 2.120(2) . ? Co2 O3 2.126(2) 2_675 ? Co2 O3 2.126(2) . ? Co2 O4 2.138(2) 1_655 ? Co2 O4 2.138(2) 2_575 ? O1 Co1 2.066(2) 2_665 ? O1 H1O1 0.70(4) . ? O2 C5 1.257(4) . ? O3 C5 1.247(4) . ? O4 C3 1.260(4) . ? O4 Co2 2.138(2) 1_455 ? O5 C3 1.258(4) . ? O5 Co1 2.071(2) 1_455 ? O1W H1WA 0.81(6) . ? O1W H1WB 0.80(7) . ? N1 C7 1.342(4) . ? N1 C1 1.344(4) . ? N1 Co1 2.148(3) 2_566 ? C1 C2 1.389(4) . ? C1 H1 0.9300 . ? C2 C4 1.403(4) . ? C2 C3 1.499(5) . ? C4 C6 1.391(5) . ? C4 C5 1.519(4) . ? C6 C7 1.383(5) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O5 178.33(9) 2_665 1_655 ? O1 Co1 O1 88.19(10) 2_665 . ? O5 Co1 O1 90.32(9) 1_655 . ? O1 Co1 O1W 89.24(10) 2_665 . ? O5 Co1 O1W 90.00(10) 1_655 . ? O1 Co1 O1W 90.35(11) . . ? O1 Co1 N1 97.90(10) 2_665 2_566 ? O5 Co1 N1 83.68(10) 1_655 2_566 ? O1 Co1 N1 169.81(10) . 2_566 ? O1W Co1 N1 97.86(11) . 2_566 ? O1 Co1 O2 85.97(10) 2_665 . ? O5 Co1 O2 94.68(9) 1_655 . ? O1 Co1 O2 85.43(9) . . ? O1W Co1 O2 173.72(10) . . ? N1 Co1 O2 86.85(10) 2_566 . ? O1 Co1 Co1 44.48(7) 2_665 2_665 ? O5 Co1 Co1 134.03(7) 1_655 2_665 ? O1 Co1 Co1 43.71(7) . 2_665 ? O1W Co1 Co1 89.73(8) . 2_665 ? N1 Co1 Co1 141.72(8) 2_566 2_665 ? O2 Co1 Co1 84.01(7) . 2_665 ? O1 Co2 O1 180.0 2_675 . ? O1 Co2 O3 96.80(9) 2_675 2_675 ? O1 Co2 O3 83.20(9) . 2_675 ? O1 Co2 O3 83.20(9) 2_675 . ? O1 Co2 O3 96.80(9) . . ? O3 Co2 O3 180.0 2_675 . ? O1 Co2 O4 92.31(9) 2_675 1_655 ? O1 Co2 O4 87.69(9) . 1_655 ? O3 Co2 O4 88.93(9) 2_675 1_655 ? O3 Co2 O4 91.07(9) . 1_655 ? O1 Co2 O4 87.69(9) 2_675 2_575 ? O1 Co2 O4 92.31(9) . 2_575 ? O3 Co2 O4 91.07(9) 2_675 2_575 ? O3 Co2 O4 88.93(9) . 2_575 ? O4 Co2 O4 180.0 1_655 2_575 ? Co1 O1 Co1 91.81(10) 2_665 . ? Co1 O1 Co2 134.21(12) 2_665 . ? Co1 O1 Co2 114.84(11) . . ? Co1 O1 H1O1 106(4) 2_665 . ? Co1 O1 H1O1 109(4) . . ? Co2 O1 H1O1 100(4) . . ? C5 O2 Co1 111.3(2) . . ? C5 O3 Co2 128.0(2) . . ? C3 O4 Co2 123.3(2) . 1_455 ? C3 O5 Co1 135.4(2) . 1_455 ? Co1 O1W H1WA 103(3) . . ? Co1 O1W H1WB 96(5) . . ? H1WA O1W H1WB 106(6) . . ? C7 N1 C1 117.0(3) . . ? C7 N1 Co1 121.3(2) . 2_566 ? C1 N1 Co1 119.1(2) . 2_566 ? N1 C1 C2 124.5(3) . . ? N1 C1 H1 117.7 . . ? C2 C1 H1 117.7 . . ? C1 C2 C4 117.7(3) . . ? C1 C2 C3 119.5(3) . . ? C4 C2 C3 122.7(3) . . ? O5 C3 O4 126.5(3) . . ? O5 C3 C2 115.6(3) . . ? O4 C3 C2 117.9(3) . . ? C6 C4 C2 118.0(3) . . ? C6 C4 C5 118.6(3) . . ? C2 C4 C5 122.7(3) . . ? O3 C5 O2 127.3(3) . . ? O3 C5 C4 118.2(3) . . ? O2 C5 C4 114.3(3) . . ? C7 C6 C4 119.9(3) . . ? C7 C6 H6 120.0 . . ? C4 C6 H6 120.0 . . ? N1 C7 C6 122.8(3) . . ? N1 C7 H7 118.6 . . ? C6 C7 H7 118.6 . . ? 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 O1 Co1 O1 Co1 0.0 2_665 . . 2_665 ? O5 Co1 O1 Co1 179.23(10) 1_655 . . 2_665 ? O1W Co1 O1 Co1 89.23(11) . . . 2_665 ? N1 Co1 O1 Co1 -126.9(5) 2_566 . . 2_665 ? O2 Co1 O1 Co1 -86.10(10) . . . 2_665 ? O1 Co1 O1 Co2 141.57(17) 2_665 . . . ? O5 Co1 O1 Co2 -39.20(13) 1_655 . . . ? O1W Co1 O1 Co2 -129.20(13) . . . . ? N1 Co1 O1 Co2 14.6(6) 2_566 . . . ? O2 Co1 O1 Co2 55.47(13) . . . . ? Co1 Co1 O1 Co2 141.57(17) 2_665 . . . ? O1 Co2 O1 Co1 -43(100) 2_675 . . 2_665 ? O3 Co2 O1 Co1 -88.23(17) 2_675 . . 2_665 ? O3 Co2 O1 Co1 91.77(17) . . . 2_665 ? O4 Co2 O1 Co1 -177.43(17) 1_655 . . 2_665 ? O4 Co2 O1 Co1 2.57(17) 2_575 . . 2_665 ? O1 Co2 O1 Co1 -163(100) 2_675 . . . ? O3 Co2 O1 Co1 151.85(14) 2_675 . . . ? O3 Co2 O1 Co1 -28.15(14) . . . . ? O4 Co2 O1 Co1 62.65(12) 1_655 . . . ? O4 Co2 O1 Co1 -117.35(12) 2_575 . . . ? O1 Co1 O2 C5 -170.4(2) 2_665 . . . ? O5 Co1 O2 C5 8.0(2) 1_655 . . . ? O1 Co1 O2 C5 -81.9(2) . . . . ? O1W Co1 O2 C5 -130.0(9) . . . . ? N1 Co1 O2 C5 91.4(2) 2_566 . . . ? Co1 Co1 O2 C5 -125.8(2) 2_665 . . . ? O1 Co2 O3 C5 174.0(3) 2_675 . . . ? O1 Co2 O3 C5 -6.0(3) . . . . ? O3 Co2 O3 C5 64(100) 2_675 . . . ? O4 Co2 O3 C5 -93.8(3) 1_655 . . . ? O4 Co2 O3 C5 86.2(3) 2_575 . . . ? C7 N1 C1 C2 1.9(5) . . . . ? Co1 N1 C1 C2 -160.0(3) 2_566 . . . ? N1 C1 C2 C4 -0.5(5) . . . . ? N1 C1 C2 C3 176.0(3) . . . . ? Co1 O5 C3 O4 37.5(5) 1_455 . . . ? Co1 O5 C3 C2 -144.1(2) 1_455 . . . ? Co2 O4 C3 O5 11.3(5) 1_455 . . . ? Co2 O4 C3 C2 -167.1(2) 1_455 . . . ? C1 C2 C3 O5 -38.5(4) . . . . ? C4 C2 C3 O5 137.9(3) . . . . ? C1 C2 C3 O4 140.1(3) . . . . ? C4 C2 C3 O4 -43.5(4) . . . . ? C1 C2 C4 C6 -1.6(4) . . . . ? C3 C2 C4 C6 -178.0(3) . . . . ? C1 C2 C4 C5 168.7(3) . . . . ? C3 C2 C4 C5 -7.8(5) . . . . ? Co2 O3 C5 O2 -16.8(5) . . . . ? Co2 O3 C5 C4 157.4(2) . . . . ? Co1 O2 C5 O3 69.2(4) . . . . ? Co1 O2 C5 C4 -105.1(3) . . . . ? C6 C4 C5 O3 -65.2(4) . . . . ? C2 C4 C5 O3 124.6(3) . . . . ? C6 C4 C5 O2 109.8(3) . . . . ? C2 C4 C5 O2 -60.4(4) . . . . ? C2 C4 C6 C7 2.3(5) . . . . ? C5 C4 C6 C7 -168.3(3) . . . . ? C1 N1 C7 C6 -1.1(5) . . . . ? Co1 N1 C7 C6 160.4(3) 2_566 . . . ? C4 C6 C7 N1 -1.0(5) . . . . ? 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 O1W H1WA O4 0.81(6) 1.99(5) 2.750(4) 156(5) 1_645 O1W H1WB O2 0.80(7) 1.96(7) 2.750(4) 171(7) 2_665 _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.915 _refine_diff_density_max 1.043 _refine_diff_density_min -0.919 _refine_diff_density_rms 0.154 #_eof #End of Crystallographic Information File