## Identification No.: IC048986R ## This CIF file contains four structures: ## 1 at 87 K and 180 K, 2 at 105 K and 180 K ## Crystallographic data for 1, [Co3(HCOO)6](CH3OH)(H2O), at 87K data_1-at-87K _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H12 Co3 O14' _chemical_formula_weight 496.96 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 'P 2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.247(2) _cell_length_b 9.8119(15) _cell_length_c 18.103(3) _cell_angle_alpha 90.00 _cell_angle_beta 127.245(3) _cell_angle_gamma 90.00 _cell_volume 1590.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 87(2) _cell_measurement_reflns_used 9763 _cell_measurement_theta_min 3.0817 _cell_measurement_theta_max 27.4835 _exptl_crystal_description 'thin plate' _exptl_crystal_colour 'violet red' _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.076 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 988 _exptl_absorpt_coefficient_mu 3.162 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.8815 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private Communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 87(2) _diffrn_source_power '5.4 kW' _diffrn_source_voltage 50.0000 _diffrn_source_current 100.0000 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_detector 'CCD' _diffrn_measurement_method 'CCD' _diffrn_measurement_device_type 'Rigaku Mercury CCD (AFC7)' _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 26374 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.0416 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3620 _reflns_number_gt 2869 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _publ_section_references ; data collect, cell refinement and data reduction: "CrystalClear" software, Rigaku Corp., Japan, 2000. absorption correction: Jacobson, R. (1998). Private Communication. Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen, Germany. ; _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^)+(0.0436P)^2^+0.2084P] 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 SHELXL _refine_ls_extinction_coef 0.0022(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3620 _refine_ls_number_parameters 246 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0538 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0848 _refine_ls_wR_factor_gt 0.0809 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.116 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.37793(4) 0.07973(4) 0.13304(3) 0.00973(13) Uani 1 1 d . . . Co2 Co 0.57092(4) -0.10962(4) 0.31114(3) 0.01008(13) Uani 1 1 d . . . Co3 Co 0.5000 0.0000 0.0000 0.01125(15) Uani 1 2 d S . . Co4 Co 0.0000 0.0000 0.0000 0.01130(15) Uani 1 2 d S . . O1 O 0.4357(2) 0.20098(19) 0.24499(14) 0.0115(4) Uani 1 1 d . . . O2 O 0.5512(2) 0.0607(2) 0.36810(15) 0.0148(5) Uani 1 1 d . . . O3 O 0.5912(2) -0.00394(19) 0.21981(15) 0.0115(5) Uani 1 1 d . . . O4 O 0.6838(3) 0.0053(2) 0.14060(16) 0.0182(5) Uani 1 1 d . . . O5 O 0.4555(2) 0.2578(2) 0.10840(14) 0.0120(5) Uani 1 1 d . . . O6 O 0.4792(3) 0.2093(2) -0.00291(15) 0.0160(5) Uani 1 1 d . . . O7 O 0.3452(2) -0.0837(2) 0.19531(15) 0.0127(5) Uani 1 1 d . . . O8 O 0.1002(2) -0.1042(2) 0.12417(16) 0.0173(5) Uani 1 1 d . . . O9 O 0.3390(2) -0.0277(2) 0.02344(15) 0.0120(5) Uani 1 1 d . . . O10 O 0.1153(2) -0.1164(2) -0.03330(16) 0.0158(5) Uani 1 1 d . . . O11 O 0.1628(2) 0.1550(2) 0.05988(15) 0.0119(5) Uani 1 1 d . . . O12 O 0.2032(2) 0.3791(2) 0.08991(16) 0.0146(5) Uani 1 1 d . . . C1 C 0.4985(4) 0.1731(3) 0.3301(2) 0.0142(7) Uani 1 1 d . . . C2 C 0.6962(4) -0.0121(3) 0.2124(2) 0.0146(7) Uani 1 1 d . . . C3 C 0.4704(4) 0.2893(3) 0.0465(2) 0.0146(7) Uani 1 1 d . . . C4 C 0.2326(3) -0.1289(3) 0.1877(2) 0.0151(7) Uani 1 1 d . . . C5 C 0.2269(4) -0.1079(3) -0.0301(2) 0.0147(7) Uani 1 1 d . . . C6 C 0.1211(4) 0.2788(3) 0.0489(2) 0.0132(7) Uani 1 1 d . . . H1 H 0.503(4) 0.244(4) 0.368(2) 0.021(9) Uiso 1 1 d . . . H2 H 0.789(4) -0.035(4) 0.266(3) 0.024(10) Uiso 1 1 d . . . H3 H 0.483(4) 0.383(4) 0.038(3) 0.023(10) Uiso 1 1 d . . . H4 H 0.018(4) 0.295(3) 0.007(2) 0.008(8) Uiso 1 1 d . . . H5 H 0.234(4) -0.161(3) -0.071(2) 0.012(8) Uiso 1 1 d . . . H6 H 0.250(4) -0.193(4) 0.238(3) 0.023(10) Uiso 1 1 d . . . O13 O -0.150(5) -0.352(4) 0.245(3) 0.395(18) Uiso 0.50 1 d PD . . C13 C -0.028(11) -0.316(12) 0.244(10) 0.65(8) Uiso 0.50 1 d PD . . O14 O -0.211(5) -0.568(5) 0.150(3) 0.44(3) Uiso 0.50 1 d PD . . C14 C -0.061(5) -0.627(5) 0.221(3) 0.30(2) Uiso 0.50 1 d PD . . O15 O -0.116(4) -0.207(4) 0.147(3) 0.177(13) Uiso 0.25 1 d P . . O16 O -0.164(3) -0.529(3) 0.095(2) 0.270(12) Uiso 0.50 1 d P . . O17 O -0.089(6) -0.358(6) 0.160(4) 0.27(2) Uiso 0.25 1 d P . . 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 0.0099(2) 0.0098(2) 0.0099(2) -0.00037(16) 0.00611(18) -0.00018(16) Co2 0.0107(2) 0.0086(2) 0.0106(2) 0.00073(16) 0.00630(18) 0.00060(16) Co3 0.0119(3) 0.0124(3) 0.0123(3) -0.0015(2) 0.0088(3) -0.0011(2) Co4 0.0090(3) 0.0120(3) 0.0119(3) -0.0013(2) 0.0058(3) -0.0021(2) O1 0.0155(11) 0.0087(10) 0.0107(11) 0.0006(8) 0.0081(10) 0.0008(9) O2 0.0189(11) 0.0109(11) 0.0136(11) 0.0014(9) 0.0093(10) 0.0028(9) O3 0.0110(11) 0.0126(11) 0.0133(11) -0.0001(8) 0.0087(10) -0.0006(8) O4 0.0137(12) 0.0263(13) 0.0155(12) 0.0007(10) 0.0093(11) 0.0000(9) O5 0.0148(11) 0.0114(10) 0.0123(11) -0.0007(9) 0.0095(10) -0.0002(9) O6 0.0242(12) 0.0130(11) 0.0164(12) 0.0002(9) 0.0153(11) 0.0023(9) O7 0.0115(11) 0.0122(10) 0.0132(11) 0.0008(9) 0.0069(10) -0.0010(9) O8 0.0119(11) 0.0227(12) 0.0159(12) 0.0021(9) 0.0076(10) -0.0032(9) O9 0.0117(11) 0.0131(10) 0.0135(11) -0.0043(9) 0.0088(10) -0.0029(9) O10 0.0127(11) 0.0178(11) 0.0176(12) -0.0037(9) 0.0096(10) -0.0030(9) O11 0.0094(10) 0.0123(10) 0.0133(11) -0.0022(9) 0.0066(9) -0.0015(9) O12 0.0120(11) 0.0119(11) 0.0163(11) -0.0021(9) 0.0068(10) -0.0019(9) C1 0.0170(16) 0.0135(16) 0.0128(16) -0.0004(13) 0.0094(14) -0.0004(13) C2 0.0112(15) 0.0179(16) 0.0111(16) -0.0036(13) 0.0049(14) -0.0030(13) C3 0.0177(16) 0.0105(15) 0.0208(17) 0.0016(13) 0.0143(15) -0.0009(13) C4 0.0133(16) 0.0165(16) 0.0143(17) 0.0020(13) 0.0078(14) -0.0016(13) C5 0.0151(16) 0.0164(16) 0.0145(16) -0.0011(13) 0.0100(14) 0.0010(13) C6 0.0111(16) 0.0158(16) 0.0129(16) 0.0025(13) 0.0073(14) 0.0035(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 O9 2.047(2) . ? Co1 O11 2.068(2) . ? Co1 O3 2.082(2) . ? Co1 O1 2.086(2) . ? Co1 O7 2.117(2) . ? Co1 O5 2.117(2) . ? Co2 O12 2.041(2) 2_645 ? Co2 O2 2.045(2) . ? Co2 O3 2.078(2) . ? Co2 O1 2.098(2) 2_645 ? Co2 O5 2.104(2) 2_645 ? Co2 O7 2.112(2) . ? Co3 O6 2.064(2) 3_655 ? Co3 O6 2.064(2) . ? Co3 O4 2.094(2) . ? Co3 O4 2.094(2) 3_655 ? Co3 O9 2.112(2) . ? Co3 O9 2.112(2) 3_655 ? Co4 O10 2.073(2) 3 ? Co4 O10 2.073(2) . ? Co4 O8 2.074(2) . ? Co4 O8 2.074(2) 3 ? Co4 O11 2.107(2) 3 ? Co4 O11 2.107(2) . ? O1 C1 1.277(4) . ? O1 Co2 2.098(2) 2_655 ? O2 C1 1.244(4) . ? O3 C2 1.268(4) . ? O4 C2 1.234(4) . ? O5 C3 1.268(4) . ? O5 Co2 2.104(2) 2_655 ? O6 C3 1.237(4) . ? O7 C4 1.268(4) . ? O8 C4 1.235(4) . ? O9 C5 1.292(4) . ? O10 C5 1.223(4) . ? O11 C6 1.273(4) . ? O12 C6 1.242(4) . ? O12 Co2 2.041(2) 2_655 ? C1 H1 0.95(4) . ? C2 H2 0.93(4) . ? C3 H3 0.95(4) . ? C4 H6 1.02(4) . ? C5 H5 0.95(4) . ? C6 H4 0.94(3) . ? O13 C13 1.43(2) . ? C13 O17 1.30(14) . ? C13 O15 1.76(12) . ? C13 C14 2.02(10) 2 ? O14 O16 1.42(5) . ? O14 C14 1.484(19) . ? C14 C13 2.02(10) 2_545 ? O15 O17 1.51(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Co1 O11 94.73(8) . . ? O9 Co1 O3 90.05(8) . . ? O11 Co1 O3 172.49(9) . . ? O9 Co1 O1 173.63(9) . . ? O11 Co1 O1 88.52(8) . . ? O3 Co1 O1 87.29(8) . . ? O9 Co1 O7 97.00(8) . . ? O11 Co1 O7 95.67(8) . . ? O3 Co1 O7 77.97(8) . . ? O1 Co1 O7 88.11(8) . . ? O9 Co1 O5 95.42(8) . . ? O11 Co1 O5 92.39(8) . . ? O3 Co1 O5 92.92(8) . . ? O1 Co1 O5 78.95(8) . . ? O7 Co1 O5 164.57(8) . . ? O12 Co2 O2 93.38(9) 2_645 . ? O12 Co2 O3 92.74(9) 2_645 . ? O2 Co2 O3 95.22(8) . . ? O12 Co2 O1 92.14(8) 2_645 2_645 ? O2 Co2 O1 170.19(9) . 2_645 ? O3 Co2 O1 92.60(8) . 2_645 ? O12 Co2 O5 88.90(9) 2_645 2_645 ? O2 Co2 O5 93.02(9) . 2_645 ? O3 Co2 O5 171.49(8) . 2_645 ? O1 Co2 O5 78.99(8) 2_645 2_645 ? O12 Co2 O7 170.87(9) 2_645 . ? O2 Co2 O7 88.31(8) . . ? O3 Co2 O7 78.16(8) . . ? O1 Co2 O7 87.52(8) 2_645 . ? O5 Co2 O7 99.98(8) 2_645 . ? O6 Co3 O6 180.00(14) 3_655 . ? O6 Co3 O4 88.87(9) 3_655 . ? O6 Co3 O4 91.13(9) . . ? O6 Co3 O4 91.13(9) 3_655 3_655 ? O6 Co3 O4 88.87(9) . 3_655 ? O4 Co3 O4 180.00(12) . 3_655 ? O6 Co3 O9 87.97(8) 3_655 . ? O6 Co3 O9 92.03(8) . . ? O4 Co3 O9 95.44(9) . . ? O4 Co3 O9 84.56(9) 3_655 . ? O6 Co3 O9 92.03(8) 3_655 3_655 ? O6 Co3 O9 87.97(8) . 3_655 ? O4 Co3 O9 84.56(9) . 3_655 ? O4 Co3 O9 95.44(9) 3_655 3_655 ? O9 Co3 O9 180.00(15) . 3_655 ? O10 Co4 O10 180.00(10) 3 . ? O10 Co4 O8 88.95(9) 3 . ? O10 Co4 O8 91.05(9) . . ? O10 Co4 O8 91.05(9) 3 3 ? O10 Co4 O8 88.95(9) . 3 ? O8 Co4 O8 180.00(16) . 3 ? O10 Co4 O11 92.60(8) 3 3 ? O10 Co4 O11 87.40(8) . 3 ? O8 Co4 O11 86.26(8) . 3 ? O8 Co4 O11 93.74(8) 3 3 ? O10 Co4 O11 87.40(8) 3 . ? O10 Co4 O11 92.60(8) . . ? O8 Co4 O11 93.74(8) . . ? O8 Co4 O11 86.26(8) 3 . ? O11 Co4 O11 180.00(8) 3 . ? C1 O1 Co1 132.04(19) . . ? C1 O1 Co2 127.29(19) . 2_655 ? Co1 O1 Co2 97.80(9) . 2_655 ? C1 O2 Co2 127.3(2) . . ? C2 O3 Co2 127.5(2) . . ? C2 O3 Co1 131.8(2) . . ? Co2 O3 Co1 99.55(9) . . ? C2 O4 Co3 132.5(2) . . ? C3 O5 Co2 127.65(19) . 2_655 ? C3 O5 Co1 132.8(2) . . ? Co2 O5 Co1 96.65(9) 2_655 . ? C3 O6 Co3 132.0(2) . . ? C4 O7 Co2 126.0(2) . . ? C4 O7 Co1 133.7(2) . . ? Co2 O7 Co1 97.35(8) . . ? C4 O8 Co4 131.6(2) . . ? C5 O9 Co1 125.4(2) . . ? C5 O9 Co3 119.6(2) . . ? Co1 O9 Co3 114.97(9) . . ? C5 O10 Co4 138.9(2) . . ? C6 O11 Co1 128.20(19) . . ? C6 O11 Co4 119.01(19) . . ? Co1 O11 Co4 112.78(9) . . ? C6 O12 Co2 130.4(2) . 2_655 ? O2 C1 O1 126.0(3) . . ? O2 C1 H1 117(2) . . ? O1 C1 H1 117(2) . . ? O4 C2 O3 125.8(3) . . ? O4 C2 H2 118(2) . . ? O3 C2 H2 116(2) . . ? O6 C3 O5 126.5(3) . . ? O6 C3 H3 114(2) . . ? O5 C3 H3 119(2) . . ? O8 C4 O7 126.5(3) . . ? O8 C4 H6 115(2) . . ? O7 C4 H6 119(2) . . ? O10 C5 O9 125.8(3) . . ? O10 C5 H5 120(2) . . ? O9 C5 H5 114(2) . . ? O12 C6 O11 126.3(3) . . ? O12 C6 H4 117(2) . . ? O11 C6 H4 117(2) . . ? O17 C13 O13 96(8) . . ? O17 C13 O15 57(6) . . ? O13 C13 O15 102(7) . . ? O17 C13 C14 118(8) . 2 ? O13 C13 C14 122(8) . 2 ? O15 C13 C14 68(4) . 2 ? O16 O14 C14 90(4) . . ? O14 C14 C13 136(5) . 2_545 ? O17 O15 C13 46(5) . . ? C13 O17 O15 77(7) . . ? 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 C1 H1 O3 0.95(4) 2.78(4) 3.282(4) 114(3) 2_655 C1 H1 O6 0.95(4) 2.56(4) 3.364(4) 143(3) 4_566 C1 H1 O9 0.95(4) 2.80(4) 3.622(4) 146(3) 2_655 C2 H2 O12 0.93(4) 2.70(4) 3.212(4) 116(3) 2_645 C3 H3 O2 0.95(4) 2.62(4) 3.162(4) 117(3) 2_655 C4 H6 O5 1.02(4) 2.79(4) 3.391(4) 118(3) 2_645 C5 H5 O4 0.95(4) 2.48(3) 2.908(4) 107(2) 3_655 C5 H5 O6 0.95(4) 2.68(3) 3.144(4) 110(2) 3_655 C6 H4 O8 0.94(3) 2.66(3) 3.083(4) 108(2) 3 C6 H4 O10 0.94(3) 2.54(3) 2.964(4) 108(2) 3 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.676 _refine_diff_density_min -0.523 _refine_diff_density_rms 0.113 ## End of data_1-at-87K ## Crystallographic data for 1, [Co3(HCOO)6](CH3OH)(H2O), at 180K data_1-at-180K _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H12 Co3 O14' _chemical_formula_weight 496.96 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 'P 2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.2539(16) _cell_length_b 9.8321(10) _cell_length_c 18.108(3) _cell_angle_alpha 90.00 _cell_angle_beta 127.222(2) _cell_angle_gamma 90.00 _cell_volume 1595.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 180(1) _cell_measurement_reflns_used 10196 _cell_measurement_theta_min 3.08 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'thin plate' _exptl_crystal_colour 'violet red' _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.069 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 988 _exptl_absorpt_coefficient_mu 3.152 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.8785 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private Communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(1) _diffrn_source_power '5.4 kW' _diffrn_source_voltage 50.0000 _diffrn_source_current 100.0000 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_detector 'CCD' _diffrn_measurement_method 'CCD' _diffrn_measurement_device_type 'Rigaku Mercury CCD (AFC7)' _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 27214 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3621 _reflns_number_gt 2915 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _publ_section_references ; data collect, cell refinement and data reduction: "CrystalClear" software, Rigaku Corp., Japan, 2000. absorption correction: Jacobson, R. (1998). Private Communication Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen, Germany. ; _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^)+(0.0427P)^2^+0.2840P] 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 SHELXL _refine_ls_extinction_coef 0.0024(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3621 _refine_ls_number_parameters 246 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0799 _refine_ls_wR_factor_gt 0.0763 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.37793(4) 0.07944(4) 0.13307(3) 0.01336(12) Uani 1 1 d . . . Co2 Co 0.57069(4) -0.11028(4) 0.31090(3) 0.01402(12) Uani 1 1 d . . . Co3 Co 0.5000 0.0000 0.0000 0.01585(14) Uani 1 2 d S . . Co4 Co 0.0000 0.0000 0.0000 0.01599(15) Uani 1 2 d S . . O1 O 0.4368(2) 0.19983(18) 0.24547(13) 0.0165(4) Uani 1 1 d . . . O2 O 0.5521(2) 0.0603(2) 0.36827(14) 0.0217(5) Uani 1 1 d . . . O3 O 0.5908(2) -0.00485(18) 0.21954(14) 0.0159(4) Uani 1 1 d . . . O4 O 0.6835(2) 0.0044(2) 0.14047(15) 0.0268(5) Uani 1 1 d . . . O5 O 0.4555(2) 0.25713(18) 0.10850(13) 0.0162(4) Uani 1 1 d . . . O6 O 0.4799(2) 0.2089(2) -0.00228(15) 0.0234(5) Uani 1 1 d . . . O7 O 0.3449(2) -0.08356(19) 0.19522(14) 0.0176(4) Uani 1 1 d . . . O8 O 0.1005(2) -0.1043(2) 0.12383(15) 0.0255(5) Uani 1 1 d . . . O9 O 0.3389(2) -0.0274(2) 0.02343(14) 0.0170(4) Uani 1 1 d . . . O10 O 0.1155(2) -0.1153(2) -0.03335(16) 0.0232(5) Uani 1 1 d . . . O11 O 0.1628(2) 0.15480(19) 0.06006(14) 0.0165(4) Uani 1 1 d . . . O12 O 0.2037(2) 0.37792(19) 0.09039(15) 0.0219(5) Uani 1 1 d . . . C1 C 0.4993(3) 0.1716(3) 0.3301(2) 0.0191(6) Uani 1 1 d . . . C2 C 0.6950(4) -0.0135(3) 0.2120(2) 0.0209(7) Uani 1 1 d . . . C3 C 0.4714(4) 0.2881(3) 0.0472(2) 0.0221(7) Uani 1 1 d . . . C4 C 0.2322(3) -0.1286(3) 0.1874(2) 0.0226(7) Uani 1 1 d . . . C5 C 0.2264(3) -0.1069(3) -0.0301(2) 0.0202(6) Uani 1 1 d . . . C6 C 0.1215(3) 0.2788(3) 0.0495(2) 0.0202(6) Uani 1 1 d . . . H1 H 0.508(3) 0.242(3) 0.369(2) 0.014(7) Uiso 1 1 d . . . H2 H 0.786(5) -0.038(4) 0.261(3) 0.042(11) Uiso 1 1 d . . . H3 H 0.481(4) 0.379(4) 0.036(2) 0.032(10) Uiso 1 1 d . . . H4 H 0.018(3) 0.288(3) 0.009(2) 0.008(7) Uiso 1 1 d . . . H5 H 0.228(3) -0.158(3) -0.071(2) 0.015(8) Uiso 1 1 d . . . H6 H 0.249(3) -0.198(3) 0.233(2) 0.020(8) Uiso 1 1 d . . . O13 O -0.183(7) -0.359(5) 0.231(4) 0.57(3) Uiso 0.50 1 d PDU . . C13 C -0.062(7) -0.324(7) 0.231(5) 0.41(3) Uiso 0.50 1 d PDU . . O14 O -0.195(7) -0.596(8) 0.170(5) 0.72(5) Uiso 0.50 1 d PDU . . C14 C -0.042(7) -0.645(6) 0.229(4) 0.38(3) Uiso 0.50 1 d PDU . . O15 O -0.115(4) -0.210(4) 0.144(3) 0.203(14) Uiso 0.25 1 d PU . . O16 O -0.190(3) -0.533(3) 0.099(2) 0.302(13) Uiso 0.50 1 d PU . . O17 O -0.087(6) -0.377(6) 0.152(4) 0.30(2) Uiso 0.25 1 d PU . . 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 0.0135(2) 0.0134(2) 0.0131(2) -0.00064(14) 0.00800(17) -0.00035(15) Co2 0.0150(2) 0.0122(2) 0.0145(2) 0.00112(15) 0.00869(17) 0.00087(15) Co3 0.0166(3) 0.0181(3) 0.0170(3) -0.0024(2) 0.0123(2) -0.0020(2) Co4 0.0119(3) 0.0174(3) 0.0170(3) -0.0023(2) 0.0078(2) -0.0031(2) O1 0.0228(11) 0.0125(9) 0.0142(10) -0.0010(8) 0.0112(9) 0.0004(8) O2 0.0307(12) 0.0164(10) 0.0169(11) 0.0030(9) 0.0137(10) 0.0053(9) O3 0.0168(10) 0.0156(10) 0.0189(11) 0.0005(8) 0.0128(9) 0.0010(8) O4 0.0196(11) 0.0440(14) 0.0196(12) 0.0019(10) 0.0132(10) -0.0006(10) O5 0.0216(10) 0.0142(9) 0.0169(10) -0.0009(8) 0.0137(9) -0.0021(8) O6 0.0351(13) 0.0208(11) 0.0254(12) -0.0019(9) 0.0242(11) 0.0003(9) O7 0.0156(10) 0.0168(10) 0.0196(11) 0.0016(8) 0.0103(9) -0.0010(8) O8 0.0143(10) 0.0366(13) 0.0217(11) 0.0060(9) 0.0089(9) -0.0033(9) O9 0.0167(10) 0.0203(10) 0.0175(10) -0.0053(8) 0.0121(9) -0.0038(8) O10 0.0153(10) 0.0280(11) 0.0276(12) -0.0071(9) 0.0136(10) -0.0047(9) O11 0.0128(9) 0.0150(9) 0.0190(11) -0.0034(8) 0.0083(9) -0.0028(8) O12 0.0171(10) 0.0169(10) 0.0241(11) -0.0039(9) 0.0084(9) -0.0025(9) C1 0.0247(16) 0.0149(14) 0.0181(15) -0.0029(12) 0.0132(14) -0.0002(12) C2 0.0159(15) 0.0262(16) 0.0161(16) -0.0022(13) 0.0073(13) -0.0009(12) C3 0.0299(17) 0.0154(15) 0.0292(17) 0.0025(13) 0.0222(15) 0.0001(13) C4 0.0187(15) 0.0230(16) 0.0216(16) 0.0035(13) 0.0098(14) -0.0040(13) C5 0.0211(15) 0.0237(16) 0.0192(15) -0.0068(13) 0.0139(14) -0.0040(12) C6 0.0133(15) 0.0227(16) 0.0205(15) 0.0028(13) 0.0081(13) 0.0040(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 O9 2.045(2) . ? Co1 O11 2.0704(19) . ? Co1 O3 2.0835(19) . ? Co1 O1 2.0859(19) . ? Co1 O7 2.1163(19) . ? Co1 O5 2.1173(19) . ? Co2 O12 2.040(2) 2_645 ? Co2 O2 2.049(2) . ? Co2 O3 2.078(2) . ? Co2 O1 2.1049(19) 2_645 ? Co2 O5 2.106(2) 2_645 ? Co2 O7 2.115(2) . ? Co3 O6 2.064(2) 3_655 ? Co3 O6 2.064(2) . ? Co3 O4 2.093(2) . ? Co3 O4 2.093(2) 3_655 ? Co3 O9 2.1148(19) . ? Co3 O9 2.1148(19) 3_655 ? Co4 O10 2.071(2) 3 ? Co4 O10 2.071(2) . ? Co4 O8 2.072(2) . ? Co4 O8 2.072(2) 3 ? Co4 O11 2.1084(18) . ? Co4 O11 2.1084(18) 3 ? O1 C1 1.271(4) . ? O1 Co2 2.1049(19) 2_655 ? O2 C1 1.238(4) . ? O3 C2 1.262(4) . ? O4 C2 1.234(4) . ? O5 C3 1.264(4) . ? O5 Co2 2.1065(19) 2_655 ? O6 C3 1.233(4) . ? O7 C4 1.268(4) . ? O8 C4 1.231(4) . ? O9 C5 1.291(4) . ? O10 C5 1.216(4) . ? O11 C6 1.277(3) . ? O12 C6 1.235(4) . ? O12 Co2 2.040(2) 2_655 ? C1 H1 0.95(3) . ? C2 H2 0.89(4) . ? C3 H3 0.93(4) . ? C4 H6 0.99(3) . ? C5 H5 0.91(3) . ? C6 H4 0.94(3) . ? O13 C13 1.41(2) . ? C13 O17 1.38(8) . ? C13 O15 1.71(7) . ? C13 C14 1.98(6) 2 ? O14 O16 1.46(8) . ? O14 C14 1.46(2) . ? C14 C13 1.98(6) 2_545 ? O15 O17 1.66(6) . ? O16 O17 1.80(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Co1 O11 94.72(8) . . ? O9 Co1 O3 89.96(8) . . ? O11 Co1 O3 172.44(8) . . ? O9 Co1 O1 173.51(8) . . ? O11 Co1 O1 88.77(8) . . ? O3 Co1 O1 87.15(8) . . ? O9 Co1 O7 97.08(8) . . ? O11 Co1 O7 95.57(8) . . ? O3 Co1 O7 77.94(7) . . ? O1 Co1 O7 88.01(8) . . ? O9 Co1 O5 95.39(8) . . ? O11 Co1 O5 92.41(8) . . ? O3 Co1 O5 93.05(7) . . ? O1 Co1 O5 78.97(8) . . ? O7 Co1 O5 164.58(7) . . ? O12 Co2 O2 93.26(9) 2_645 . ? O12 Co2 O3 92.79(8) 2_645 . ? O2 Co2 O3 95.11(8) . . ? O12 Co2 O1 92.18(8) 2_645 2_645 ? O2 Co2 O1 170.20(8) . 2_645 ? O3 Co2 O1 92.76(7) . 2_645 ? O12 Co2 O5 88.81(8) 2_645 2_645 ? O2 Co2 O5 93.17(8) . 2_645 ? O3 Co2 O5 171.46(8) . 2_645 ? O1 Co2 O5 78.79(7) 2_645 2_645 ? O12 Co2 O7 170.86(8) 2_645 . ? O2 Co2 O7 88.32(8) . . ? O3 Co2 O7 78.10(8) . . ? O1 Co2 O7 87.60(8) 2_645 . ? O5 Co2 O7 100.10(8) 2_645 . ? O6 Co3 O6 180.00(13) 3_655 . ? O6 Co3 O4 88.90(8) 3_655 . ? O6 Co3 O4 91.10(8) . . ? O6 Co3 O4 91.10(8) 3_655 3_655 ? O6 Co3 O4 88.90(8) . 3_655 ? O4 Co3 O4 180.00(12) . 3_655 ? O6 Co3 O9 88.05(8) 3_655 . ? O6 Co3 O9 91.95(8) . . ? O4 Co3 O9 95.39(8) . . ? O4 Co3 O9 84.61(8) 3_655 . ? O6 Co3 O9 91.95(8) 3_655 3_655 ? O6 Co3 O9 88.05(8) . 3_655 ? O4 Co3 O9 84.61(8) . 3_655 ? O4 Co3 O9 95.39(8) 3_655 3_655 ? O9 Co3 O9 180.00(14) . 3_655 ? O10 Co4 O10 180.00(9) 3 . ? O10 Co4 O8 89.05(9) 3 . ? O10 Co4 O8 90.95(9) . . ? O10 Co4 O8 90.95(9) 3 3 ? O10 Co4 O8 89.05(9) . 3 ? O8 Co4 O8 180.00(15) . 3 ? O10 Co4 O11 87.56(8) 3 . ? O10 Co4 O11 92.44(8) . . ? O8 Co4 O11 93.67(8) . . ? O8 Co4 O11 86.33(8) 3 . ? O10 Co4 O11 92.44(8) 3 3 ? O10 Co4 O11 87.56(8) . 3 ? O8 Co4 O11 86.33(8) . 3 ? O8 Co4 O11 93.67(8) 3 3 ? O11 Co4 O11 180.00(12) . 3 ? C1 O1 Co1 132.06(18) . . ? C1 O1 Co2 127.50(18) . 2_655 ? Co1 O1 Co2 97.72(8) . 2_655 ? C1 O2 Co2 127.03(19) . . ? C2 O3 Co2 127.47(19) . . ? C2 O3 Co1 131.8(2) . . ? Co2 O3 Co1 99.61(8) . . ? C2 O4 Co3 132.3(2) . . ? C3 O5 Co2 127.82(18) . 2_655 ? C3 O5 Co1 132.75(19) . . ? Co2 O5 Co1 96.70(8) 2_655 . ? C3 O6 Co3 132.0(2) . . ? C4 O7 Co2 126.07(19) . . ? C4 O7 Co1 133.65(19) . . ? Co2 O7 Co1 97.39(8) . . ? C4 O8 Co4 131.9(2) . . ? C5 O9 Co1 125.27(19) . . ? C5 O9 Co3 119.76(19) . . ? Co1 O9 Co3 114.98(9) . . ? C5 O10 Co4 139.1(2) . . ? C6 O11 Co1 128.03(18) . . ? C6 O11 Co4 119.22(18) . . ? Co1 O11 Co4 112.74(9) . . ? C6 O12 Co2 130.83(19) . 2_655 ? O2 C1 O1 126.5(3) . . ? O2 C1 H1 115.9(18) . . ? O1 C1 H1 117.6(18) . . ? O4 C2 O3 126.1(3) . . ? O4 C2 H2 114(3) . . ? O3 C2 H2 120(3) . . ? O6 C3 O5 126.9(3) . . ? O6 C3 H3 112(2) . . ? O5 C3 H3 121(2) . . ? O8 C4 O7 126.5(3) . . ? O8 C4 H6 115.4(19) . . ? O7 C4 H6 117.8(19) . . ? O10 C5 O9 126.0(3) . . ? O10 C5 H5 117(2) . . ? O9 C5 H5 117(2) . . ? O12 C6 O11 126.2(3) . . ? O12 C6 H4 121.3(18) . . ? O11 C6 H4 112.3(18) . . ? O17 C13 O13 108(7) . . ? O17 C13 O15 64(4) . . ? O13 C13 O15 111(5) . . ? O17 C13 C14 115(6) . 2 ? O13 C13 C14 125(6) . 2 ? O15 C13 C14 64(3) . 2 ? O16 O14 C14 97(6) . . ? O14 C14 C13 137(6) . 2_545 ? O17 O15 C13 48(3) . . ? O14 O16 O17 105(4) . . ? C13 O17 O15 68(4) . . ? C13 O17 O16 123(5) . . ? O15 O17 O16 140(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 C1 H1 O3 0.95(3) 2.80(3) 3.294(3) 114(2) 2_655 C1 H1 O6 0.95(3) 2.59(3) 3.383(4) 142(2) 4_566 C1 H1 O9 0.95(3) 2.80(3) 3.642(4) 149(2) 2_655 C2 H2 O12 0.89(4) 2.76(4) 3.211(4) 113(3) 2_645 C3 H3 O2 0.93(4) 2.67(4) 3.173(4) 115(3) 2_655 C4 H6 O5 0.99(3) 2.82(3) 3.400(4) 118(2) 2_645 C5 H5 O4 0.91(3) 2.52(3) 2.914(4) 107(2) 3_655 C5 H5 O6 0.91(3) 2.74(3) 3.151(4) 108(2) 3_655 C6 H4 O8 0.94(3) 2.64(3) 3.090(4) 110(2) 3 C6 H4 O10 0.94(3) 2.47(3) 2.974(4) 114(2) 3 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.469 _refine_diff_density_min -0.523 _refine_diff_density_rms 0.100 ## End of data_1-at-180K ## Crystallographic data for 2, [Co3(HCOO)6], at 105K data_2-105K _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H6 Co3 O12' _chemical_formula_weight 446.90 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 'P 2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.2783(4) _cell_length_b 9.8567(4) _cell_length_c 18.1630(6) _cell_angle_alpha 90.00 _cell_angle_beta 127.204(2) _cell_angle_gamma 90.00 _cell_volume 1608.21(10) _cell_formula_units_Z 4 _cell_measurement_temperature 105.0(1) _cell_measurement_reflns_used 28713 _cell_measurement_theta_min 3.39 _cell_measurement_theta_max 27.47 _exptl_crystal_description 'thin plate' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.846 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 876 _exptl_absorpt_coefficient_mu 3.107 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.672 _exptl_absorpt_correction_T_max 0.860 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995, 1997) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 105.0(1) _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 'NONIUS KappaCCD' _diffrn_measurement_method 'CCD' _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 28713 _diffrn_reflns_av_R_equivalents 0.1230 _diffrn_reflns_av_sigmaI/netI 0.0766 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3671 _reflns_number_gt 2619 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _publ_section_references ; collect: "Collect" data collection software, Nonius B.V., Delft, The Netherlands, 1998. HKL Scalepack & HKL Denzo: Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R.M. Sweet, Eds., Academic Press. absorption correction: R.H. Blessing (1995) Acta Cryst. A51, 33-37. R.H. Blessing (1997) J.Appl. Cryst. 30, 421-426. maXus: S.Mackay, C.J.Gilmore, C.Edwards, M. Tremayne, N. Stuart, K.Shankland "maXus: a computer program for the solution and refinement of crystal structures from diffraction data", University of Glasgow, Scotland, UK, Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama, Japan (1998). Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen, Germany. ; _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^)+(0.0376P)^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 SHELXL _refine_ls_extinction_coef 0.0030(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3671 _refine_ls_number_parameters 213 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.0862 _refine_ls_wR_factor_gt 0.0800 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.37787(5) 0.07823(4) 0.13313(3) 0.01511(14) Uani 1 1 d . . . Co2 Co 0.57001(5) -0.11166(4) 0.31050(3) 0.01589(14) Uani 1 1 d . . . Co3 Co 0.5000 0.0000 0.0000 0.01674(17) Uani 1 2 d S . . Co4 Co 0.0000 0.0000 0.0000 0.01687(17) Uani 1 2 d S . . O1 O 0.4367(3) 0.1989(2) 0.24506(14) 0.0176(5) Uani 1 1 d . . . O2 O 0.5510(3) 0.0584(2) 0.36783(15) 0.0203(5) Uani 1 1 d . . . O3 O 0.5894(3) -0.0062(2) 0.21875(15) 0.0178(5) Uani 1 1 d . . . O4 O 0.6817(3) 0.0061(2) 0.13968(16) 0.0230(6) Uani 1 1 d . . . O5 O 0.4555(3) 0.2554(2) 0.10876(14) 0.0180(5) Uani 1 1 d . . . O6 O 0.4793(3) 0.2089(2) -0.00256(15) 0.0213(6) Uani 1 1 d . . . O7 O 0.3454(3) -0.0846(2) 0.19520(15) 0.0187(5) Uani 1 1 d . . . O8 O 0.0999(3) -0.1053(2) 0.12315(16) 0.0224(6) Uani 1 1 d . . . O9 O 0.3392(3) -0.0279(2) 0.02358(15) 0.0176(5) Uani 1 1 d . . . O10 O 0.1152(3) -0.1155(2) -0.03300(16) 0.0209(5) Uani 1 1 d . . . O11 O 0.1639(3) 0.1534(2) 0.06035(14) 0.0168(5) Uani 1 1 d . . . O12 O 0.2045(3) 0.3771(2) 0.09124(15) 0.0195(5) Uani 1 1 d . . . C1 C 0.4991(4) 0.1712(3) 0.3303(2) 0.0218(8) Uani 1 1 d . . . C2 C 0.6939(5) -0.0133(3) 0.2116(3) 0.0210(8) Uani 1 1 d . . . C3 C 0.4689(4) 0.2881(3) 0.0464(2) 0.0211(8) Uani 1 1 d . . . C4 C 0.2309(4) -0.1304(3) 0.1862(2) 0.0208(8) Uani 1 1 d . . . C5 C 0.2265(4) -0.1071(3) -0.0295(2) 0.0195(8) Uani 1 1 d . . . C6 C 0.1219(5) 0.2778(3) 0.0501(2) 0.0209(8) Uani 1 1 d . . . H1 H 0.508(4) 0.255(3) 0.370(2) 0.018(4) Uiso 1 1 d . . . H2 H 0.781(5) -0.029(3) 0.262(2) 0.018(4) Uiso 1 1 d . . . H3 H 0.482(4) 0.391(3) 0.040(2) 0.018(4) Uiso 1 1 d . . . H4 H 0.250(4) -0.201(3) 0.233(2) 0.018(4) Uiso 1 1 d . . . H5 H 0.238(4) -0.157(3) -0.069(2) 0.018(4) Uiso 1 1 d . . . H6 H 0.012(4) 0.295(3) 0.006(2) 0.018(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0190(3) 0.0120(2) 0.0159(2) -0.00038(17) 0.0114(2) -0.00022(19) Co2 0.0204(3) 0.0117(2) 0.0168(2) 0.00058(17) 0.0119(2) 0.00051(19) Co3 0.0208(4) 0.0150(3) 0.0185(3) -0.0012(2) 0.0140(3) -0.0012(3) Co4 0.0183(4) 0.0143(3) 0.0184(3) -0.0013(2) 0.0113(3) -0.0020(3) O1 0.0230(15) 0.0131(11) 0.0161(11) -0.0002(9) 0.0115(11) 0.0005(10) O2 0.0285(16) 0.0143(12) 0.0192(12) 0.0024(9) 0.0150(12) 0.0027(11) O3 0.0217(15) 0.0144(12) 0.0196(12) -0.0004(9) 0.0137(12) -0.0002(10) O4 0.0256(16) 0.0273(13) 0.0222(13) 0.0006(10) 0.0176(13) -0.0004(11) O5 0.0251(15) 0.0145(11) 0.0193(12) -0.0011(9) 0.0158(12) -0.0028(11) O6 0.0336(17) 0.0172(12) 0.0233(12) -0.0007(10) 0.0226(13) 0.0006(11) O7 0.0225(15) 0.0151(12) 0.0188(12) -0.0005(9) 0.0127(12) -0.0007(10) O8 0.0230(16) 0.0224(13) 0.0214(12) 0.0008(10) 0.0132(12) -0.0031(11) O9 0.0198(15) 0.0155(12) 0.0202(12) -0.0030(9) 0.0135(11) -0.0026(11) O10 0.0211(15) 0.0189(12) 0.0257(13) -0.0045(10) 0.0158(12) -0.0042(11) O11 0.0193(14) 0.0123(12) 0.0185(12) -0.0012(9) 0.0113(11) -0.0008(10) O12 0.0207(14) 0.0142(12) 0.0211(12) -0.0033(9) 0.0112(11) -0.0027(11) C1 0.028(2) 0.0155(18) 0.0245(19) 0.0010(14) 0.0176(18) -0.0004(16) C2 0.018(2) 0.0184(18) 0.0237(19) -0.0013(14) 0.0107(17) -0.0006(16) C3 0.026(2) 0.0146(17) 0.0276(18) 0.0002(14) 0.0191(18) -0.0001(15) C4 0.023(2) 0.0181(18) 0.0221(19) -0.0012(14) 0.0144(18) -0.0016(16) C5 0.026(2) 0.0166(18) 0.0202(18) -0.0009(14) 0.0162(18) 0.0011(16) C6 0.024(2) 0.023(2) 0.0199(18) 0.0015(15) 0.0150(18) -0.0014(17) _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 O9 2.048(2) . ? Co1 O11 2.065(2) . ? Co1 O3 2.077(2) . ? Co1 O1 2.088(2) . ? Co1 O5 2.116(2) . ? Co1 O7 2.117(2) . ? Co2 O12 2.043(3) 2_645 ? Co2 O2 2.052(2) . ? Co2 O3 2.085(2) . ? Co2 O1 2.102(2) 2_645 ? Co2 O5 2.112(2) 2_645 ? Co2 O7 2.112(2) . ? Co3 O6 2.069(2) 3_655 ? Co3 O6 2.069(2) . ? Co3 O4 2.086(2) . ? Co3 O4 2.086(2) 3_655 ? Co3 O9 2.119(2) 3_655 ? Co3 O9 2.119(2) . ? Co4 O10 2.070(2) 3 ? Co4 O10 2.070(2) . ? Co4 O8 2.074(2) . ? Co4 O8 2.074(2) 3 ? Co4 O11 2.110(2) 3 ? Co4 O11 2.110(2) . ? O1 C1 1.284(4) . ? O1 Co2 2.102(2) 2_655 ? O2 C1 1.249(4) . ? O3 C2 1.263(4) . ? O4 C2 1.243(4) . ? O5 C3 1.271(4) . ? O5 Co2 2.112(2) 2_655 ? O6 C3 1.242(4) . ? O7 C4 1.281(4) . ? O8 C4 1.229(4) . ? O9 C5 1.293(4) . ? O10 C5 1.221(4) . ? O11 C6 1.287(4) . ? O12 C6 1.242(4) . ? O12 Co2 2.043(2) 2_655 ? C1 H1 1.06(3) . ? C2 H2 0.86(4) . ? C3 H3 1.05(3) . ? C4 H4 1.02(3) . ? C5 H5 0.94(3) . ? C6 H6 1.00(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Co1 O11 94.66(9) . . ? O9 Co1 O3 89.80(9) . . ? O11 Co1 O3 172.61(8) . . ? O9 Co1 O1 173.18(10) . . ? O11 Co1 O1 88.80(9) . . ? O3 Co1 O1 87.39(9) . . ? O9 Co1 O5 95.19(8) . . ? O11 Co1 O5 92.35(9) . . ? O3 Co1 O5 93.11(9) . . ? O1 Co1 O5 78.78(8) . . ? O9 Co1 O7 97.27(8) . . ? O11 Co1 O7 95.81(9) . . ? O3 Co1 O7 77.76(9) . . ? O1 Co1 O7 88.20(8) . . ? O5 Co1 O7 164.49(9) . . ? O12 Co2 O2 93.32(9) 2_645 . ? O12 Co2 O3 92.80(9) 2_645 . ? O2 Co2 O3 95.28(8) . . ? O12 Co2 O1 92.03(9) 2_645 2_645 ? O2 Co2 O1 170.03(9) . 2_645 ? O3 Co2 O1 92.85(8) . 2_645 ? O12 Co2 O5 88.83(9) 2_645 2_645 ? O2 Co2 O5 93.14(8) . 2_645 ? O3 Co2 O5 171.32(8) . 2_645 ? O1 Co2 O5 78.56(8) 2_645 2_645 ? O12 Co2 O7 170.49(9) 2_645 . ? O2 Co2 O7 88.23(9) . . ? O3 Co2 O7 77.71(9) . . ? O1 Co2 O7 87.88(9) 2_645 . ? O5 Co2 O7 100.47(9) 2_645 . ? O6 Co3 O6 180.00(14) 3_655 . ? O6 Co3 O4 89.25(9) 3_655 . ? O6 Co3 O4 90.75(9) . . ? O6 Co3 O4 90.75(9) 3_655 3_655 ? O6 Co3 O4 89.25(9) . 3_655 ? O4 Co3 O4 180.00(12) . 3_655 ? O6 Co3 O9 92.00(9) 3_655 3_655 ? O6 Co3 O9 88.00(9) . 3_655 ? O4 Co3 O9 84.87(9) . 3_655 ? O4 Co3 O9 95.13(9) 3_655 3_655 ? O6 Co3 O9 88.00(9) 3_655 . ? O6 Co3 O9 92.00(9) . . ? O4 Co3 O9 95.13(9) . . ? O4 Co3 O9 84.87(9) 3_655 . ? O9 Co3 O9 180.00(15) 3_655 . ? O10 Co4 O10 180.00(10) 3 . ? O10 Co4 O8 89.39(9) 3 . ? O10 Co4 O8 90.61(9) . . ? O10 Co4 O8 90.61(9) 3 3 ? O10 Co4 O8 89.39(9) . 3 ? O8 Co4 O8 180.00(17) . 3 ? O10 Co4 O11 92.20(9) 3 3 ? O10 Co4 O11 87.80(9) . 3 ? O8 Co4 O11 86.31(9) . 3 ? O8 Co4 O11 93.69(9) 3 3 ? O10 Co4 O11 87.80(9) 3 . ? O10 Co4 O11 92.20(9) . . ? O8 Co4 O11 93.69(9) . . ? O8 Co4 O11 86.31(9) 3 . ? O11 Co4 O11 180.00(15) 3 . ? C1 O1 Co1 132.3(2) . . ? C1 O1 Co2 127.0(2) . 2_655 ? Co1 O1 Co2 98.08(8) . 2_655 ? C1 O2 Co2 127.5(2) . . ? C2 O3 Co1 131.7(2) . . ? C2 O3 Co2 127.6(2) . . ? Co1 O3 Co2 99.80(10) . . ? C2 O4 Co3 132.6(3) . . ? C3 O5 Co2 126.9(2) . 2_655 ? C3 O5 Co1 133.0(2) . . ? Co2 O5 Co1 96.88(9) 2_655 . ? C3 O6 Co3 131.9(2) . . ? C4 O7 Co2 126.5(2) . . ? C4 O7 Co1 133.2(2) . . ? Co2 O7 Co1 97.68(10) . . ? C4 O8 Co4 131.9(2) . . ? C5 O9 Co1 124.7(2) . . ? C5 O9 Co3 120.2(2) . . ? Co1 O9 Co3 115.13(11) . . ? C5 O10 Co4 138.9(2) . . ? C6 O11 Co1 128.3(2) . . ? C6 O11 Co4 118.5(2) . . ? Co1 O11 Co4 113.15(9) . . ? C6 O12 Co2 130.8(2) . 2_655 ? O2 C1 O1 125.6(3) . . ? O2 C1 H1 120.3(17) . . ? O1 C1 H1 114.1(17) . . ? O4 C2 O3 125.6(4) . . ? O4 C2 H2 119(2) . . ? O3 C2 H2 116(2) . . ? O6 C3 O5 126.4(3) . . ? O6 C3 H3 116.8(17) . . ? O5 C3 H3 116.7(17) . . ? O8 C4 O7 126.8(3) . . ? O8 C4 H4 117(2) . . ? O7 C4 H4 116(2) . . ? O10 C5 O9 126.5(3) . . ? O10 C5 H5 122(2) . . ? O9 C5 H5 111(2) . . ? O12 C6 O11 126.0(4) . . ? O12 C6 H6 117.7(19) . . ? O11 C6 H6 116.3(19) . . ? 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 C1 H1 O3 1.06(3) 2.68(3) 3.291(4) 116(2) 2_655 C1 H1 O6 1.06(3) 2.55(3) 3.388(4) 136(2) 4_566 C1 H1 O9 1.06(3) 2.70(3) 3.649(4) 150(3) 2_655 C2 H2 O12 0.86(4) 2.73(3) 3.216(4) 117(3) 2_645 C3 H3 O2 1.05(3) 2.53(3) 3.162(4) 118(2) 2_655 C4 H4 O5 1.02(3) 2.81(4) 3.424(4) 119(2) 2_645 C5 H5 O4 0.94(3) 2.47(3) 2.927(4) 110(2) 3_655 C5 H5 O6 0.94(3) 2.67(4) 3.165(5) 114(3) 3_655 C6 H6 O8 1.00(4) 2.65(3) 3.087(4) 107(2) 3 C6 H6 O10 1.00(4) 2.50(3) 2.967(5) 108(2) 3 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.610 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.122 ## End of data_2-at-105K ## Crystallographic data for 2, [Co3(HCOO)6], at 180K data_2-at-180K _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H6 Co3 O12' _chemical_formula_weight 446.90 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 'P 2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.2858(4) _cell_length_b 9.8690(4) _cell_length_c 18.1797(6) _cell_angle_alpha 90.00 _cell_angle_beta 127.193(2) _cell_angle_gamma 90.00 _cell_volume 1613.00(10) _cell_formula_units_Z 4 _cell_measurement_temperature 180.0(1) _cell_measurement_reflns_used 28990 _cell_measurement_theta_min 3.49 _cell_measurement_theta_max 27.47 _exptl_crystal_description 'thin plate' _exptl_crystal_colour 'violet red' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.840 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 876 _exptl_absorpt_coefficient_mu 3.098 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.704 _exptl_absorpt_correction_T_max 0.860 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995, 1997) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180.0(1) _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 'NONIUS KappaCCD' _diffrn_measurement_method 'CCD' _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 28990 _diffrn_reflns_av_R_equivalents 0.1137 _diffrn_reflns_av_sigmaI/netI 0.0718 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3688 _reflns_number_gt 2583 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _publ_section_references ; collect: "Collect" data collection software, Nonius B.V., Delft, The Netherlands, 1998. HKL Scalepack & HKL Denzo: Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R.M. Sweet, Eds., Academic Press. absorption correction: R.H. Blessing (1995) Acta Cryst. A51, 33-37. R.H. Blessing (1997) J.Appl. Cryst. 30, 421-426. maXus: S.Mackay, C.J.Gilmore, C.Edwards, M. Tremayne, N. Stuart, K.Shankland "maXus: a computer program for the solution and refinement of crystal structures from diffraction data", University of Glasgow, Scotland, UK, Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama, Japan (1998). Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen, Germany. ; _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^)+(0.0362P)^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 SHELXL _refine_ls_extinction_coef 0.0030(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3688 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0807 _refine_ls_wR_factor_gt 0.0750 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.981 _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 0.37780(5) 0.07788(4) 0.13315(3) 0.01832(13) Uani 1 1 d . . . Co2 Co 0.56982(5) -0.11228(4) 0.31021(3) 0.01953(14) Uani 1 1 d . . . Co3 Co 0.5000 0.0000 0.0000 0.02065(17) Uani 1 2 d S . . Co4 Co 0.0000 0.0000 0.0000 0.02096(17) Uani 1 2 d S . . O1 O 0.4371(2) 0.19830(19) 0.24532(13) 0.0209(5) Uani 1 1 d . . . O2 O 0.5507(3) 0.0577(2) 0.36741(14) 0.0271(5) Uani 1 1 d . . . O3 O 0.5892(3) -0.0068(2) 0.21842(14) 0.0210(5) Uani 1 1 d . . . O4 O 0.6813(3) 0.0047(2) 0.13954(15) 0.0295(6) Uani 1 1 d . . . O5 O 0.4551(3) 0.25505(19) 0.10878(14) 0.0222(5) Uani 1 1 d . . . O6 O 0.4794(3) 0.2082(2) -0.00224(15) 0.0279(6) Uani 1 1 d . . . O7 O 0.3451(3) -0.0845(2) 0.19484(14) 0.0223(5) Uani 1 1 d . . . O8 O 0.1007(3) -0.1057(2) 0.12313(16) 0.0299(6) Uani 1 1 d . . . O9 O 0.3390(3) -0.0275(2) 0.02360(14) 0.0221(5) Uani 1 1 d . . . O10 O 0.1152(3) -0.1147(2) -0.03321(15) 0.0265(5) Uani 1 1 d . . . O11 O 0.1642(2) 0.1533(2) 0.06063(13) 0.0215(5) Uani 1 1 d . . . O12 O 0.2052(3) 0.3761(2) 0.09180(15) 0.0253(5) Uani 1 1 d . . . C1 C 0.4993(4) 0.1707(3) 0.3299(2) 0.0266(8) Uani 1 1 d . . . C2 C 0.6931(4) -0.0145(3) 0.2111(2) 0.0266(8) Uani 1 1 d . . . C3 C 0.4693(4) 0.2873(3) 0.0471(2) 0.0279(8) Uani 1 1 d . . . C4 C 0.2310(4) -0.1303(3) 0.1858(2) 0.0264(8) Uani 1 1 d . . . C5 C 0.2254(4) -0.1061(3) -0.0298(2) 0.0253(8) Uani 1 1 d . . . C6 C 0.1218(4) 0.2775(3) 0.0504(2) 0.0245(8) Uani 1 1 d . . . H1 H 0.511(3) 0.255(3) 0.3701(17) 0.009(7) Uiso 1 1 d . . . H2 H 0.784(4) -0.038(3) 0.264(2) 0.032(10) Uiso 1 1 d . . . H3 H 0.475(4) 0.386(3) 0.038(2) 0.024(9) Uiso 1 1 d . . . H4 H 0.256(4) -0.200(3) 0.235(2) 0.034(9) Uiso 1 1 d . . . H5 H 0.234(4) -0.156(3) -0.068(2) 0.028(9) Uiso 1 1 d . . . H6 H 0.013(4) 0.299(3) 0.005(2) 0.020(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0218(3) 0.0154(2) 0.0191(2) -0.00062(16) 0.0130(2) -0.00029(18) Co2 0.0240(3) 0.0151(2) 0.0205(2) 0.00152(16) 0.0139(2) 0.00124(18) Co3 0.0246(4) 0.0201(3) 0.0225(3) -0.0020(2) 0.0170(3) -0.0014(3) Co4 0.0202(4) 0.0195(3) 0.0227(3) -0.0019(2) 0.0128(3) -0.0026(3) O1 0.0284(14) 0.0153(11) 0.0178(11) -0.0014(8) 0.0134(10) -0.0021(10) O2 0.0390(16) 0.0192(12) 0.0239(12) 0.0044(9) 0.0195(12) 0.0058(11) O3 0.0217(13) 0.0208(12) 0.0234(11) 0.0018(9) 0.0152(11) 0.0022(9) O4 0.0285(15) 0.0403(14) 0.0255(13) 0.0010(10) 0.0195(12) -0.0008(11) O5 0.0317(15) 0.0173(11) 0.0241(11) -0.0007(9) 0.0203(11) -0.0019(10) O6 0.0416(16) 0.0230(12) 0.0318(13) -0.0020(10) 0.0288(13) -0.0007(11) O7 0.0247(14) 0.0190(11) 0.0239(11) 0.0002(9) 0.0150(11) -0.0008(10) O8 0.0224(14) 0.0361(14) 0.0281(12) 0.0033(10) 0.0136(12) -0.0045(11) O9 0.0239(14) 0.0208(12) 0.0236(11) -0.0053(9) 0.0154(11) -0.0035(10) O10 0.0228(14) 0.0284(13) 0.0335(13) -0.0066(10) 0.0198(12) -0.0048(10) O11 0.0236(13) 0.0166(11) 0.0254(11) -0.0023(9) 0.0153(11) -0.0018(10) O12 0.0246(14) 0.0188(11) 0.0260(12) -0.0047(9) 0.0117(11) -0.0025(10) C1 0.033(2) 0.0182(17) 0.0297(19) -0.0002(14) 0.0193(17) 0.0008(15) C2 0.022(2) 0.0253(19) 0.0277(19) 0.0008(14) 0.0129(17) 0.0001(15) C3 0.039(2) 0.0166(17) 0.0341(18) 0.0014(14) 0.0252(18) 0.0005(15) C4 0.029(2) 0.0263(19) 0.0244(18) 0.0008(14) 0.0163(17) -0.0023(16) C5 0.034(2) 0.0202(18) 0.0261(18) -0.0036(14) 0.0200(17) -0.0006(16) C6 0.023(2) 0.0244(19) 0.0242(17) 0.0004(14) 0.0133(17) 0.0009(16) _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 O9 2.046(2) . ? Co1 O11 2.064(2) . ? Co1 O3 2.078(2) . ? Co1 O1 2.0899(19) . ? Co1 O7 2.112(2) . ? Co1 O5 2.117(2) . ? Co2 O12 2.041(2) 2_645 ? Co2 O2 2.053(2) . ? Co2 O3 2.087(2) . ? Co2 O1 2.1033(19) 2_645 ? Co2 O5 2.113(2) 2_645 ? Co2 O7 2.115(2) . ? Co3 O6 2.065(2) 3_655 ? Co3 O6 2.065(2) . ? Co3 O4 2.085(2) . ? Co3 O4 2.085(2) 3_655 ? Co3 O9 2.122(2) . ? Co3 O9 2.122(2) 3_655 ? Co4 O10 2.070(2) 3 ? Co4 O10 2.070(2) . ? Co4 O8 2.077(2) . ? Co4 O8 2.077(2) 3 ? Co4 O11 2.114(2) 3 ? Co4 O11 2.114(2) . ? O1 C1 1.276(4) . ? O1 Co2 2.1033(19) 2_655 ? O2 C1 1.251(4) . ? O3 C2 1.260(4) . ? O4 C2 1.240(4) . ? O5 C3 1.265(4) . ? O5 Co2 2.113(2) 2_655 ? O6 C3 1.246(4) . ? O7 C4 1.278(4) . ? O8 C4 1.222(4) . ? O9 C5 1.297(4) . ? O10 C5 1.211(4) . ? O11 C6 1.288(4) . ? O12 C6 1.241(4) . ? O12 Co2 2.041(2) 2_655 ? C1 H1 1.06(3) . ? C2 H2 0.91(4) . ? C3 H3 0.99(3) . ? C4 H4 1.02(3) . ? C5 H5 0.91(3) . ? C6 H6 1.01(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Co1 O11 94.67(8) . . ? O9 Co1 O3 89.75(8) . . ? O11 Co1 O3 172.71(8) . . ? O9 Co1 O1 173.05(9) . . ? O11 Co1 O1 88.84(8) . . ? O3 Co1 O1 87.39(8) . . ? O9 Co1 O7 97.35(8) . . ? O11 Co1 O7 95.83(8) . . ? O3 Co1 O7 77.83(8) . . ? O1 Co1 O7 88.24(8) . . ? O9 Co1 O5 95.10(8) . . ? O11 Co1 O5 92.19(8) . . ? O3 Co1 O5 93.19(8) . . ? O1 Co1 O5 78.75(8) . . ? O7 Co1 O5 164.58(8) . . ? O12 Co2 O2 93.43(9) 2_645 . ? O12 Co2 O3 92.86(9) 2_645 . ? O2 Co2 O3 95.21(8) . . ? O12 Co2 O1 91.99(9) 2_645 2_645 ? O2 Co2 O1 169.97(9) . 2_645 ? O3 Co2 O1 92.94(8) . 2_645 ? O12 Co2 O5 88.63(9) 2_645 2_645 ? O2 Co2 O5 93.13(8) . 2_645 ? O3 Co2 O5 171.42(8) . 2_645 ? O1 Co2 O5 78.56(8) 2_645 2_645 ? O12 Co2 O7 170.41(8) 2_645 . ? O2 Co2 O7 88.07(8) . . ? O3 Co2 O7 77.57(8) . . ? O1 Co2 O7 87.98(8) 2_645 . ? O5 Co2 O7 100.75(9) 2_645 . ? O6 Co3 O6 180.0 3_655 . ? O6 Co3 O4 88.99(9) 3_655 . ? O6 Co3 O4 91.01(9) . . ? O6 Co3 O4 91.01(9) 3_655 3_655 ? O6 Co3 O4 88.99(9) . 3_655 ? O4 Co3 O4 180.00(12) . 3_655 ? O6 Co3 O9 88.21(8) 3_655 . ? O6 Co3 O9 91.79(8) . . ? O4 Co3 O9 95.01(8) . . ? O4 Co3 O9 84.99(8) 3_655 . ? O6 Co3 O9 91.79(8) 3_655 3_655 ? O6 Co3 O9 88.21(8) . 3_655 ? O4 Co3 O9 84.99(8) . 3_655 ? O4 Co3 O9 95.01(8) 3_655 3_655 ? O9 Co3 O9 180.00(9) . 3_655 ? O10 Co4 O10 180.00(9) 3 . ? O10 Co4 O8 89.50(9) 3 . ? O10 Co4 O8 90.50(9) . . ? O10 Co4 O8 90.50(9) 3 3 ? O10 Co4 O8 89.50(9) . 3 ? O8 Co4 O8 180.00(17) . 3 ? O10 Co4 O11 92.07(8) 3 3 ? O10 Co4 O11 87.93(8) . 3 ? O8 Co4 O11 86.48(8) . 3 ? O8 Co4 O11 93.52(8) 3 3 ? O10 Co4 O11 87.93(8) 3 . ? O10 Co4 O11 92.07(8) . . ? O8 Co4 O11 93.52(8) . . ? O8 Co4 O11 86.48(8) 3 . ? O11 Co4 O11 180.0 3 . ? C1 O1 Co1 132.31(19) . . ? C1 O1 Co2 127.04(19) . 2_655 ? Co1 O1 Co2 98.06(8) . 2_655 ? C1 O2 Co2 127.5(2) . . ? C2 O3 Co1 131.9(2) . . ? C2 O3 Co2 127.4(2) . . ? Co1 O3 Co2 99.75(9) . . ? C2 O4 Co3 132.6(2) . . ? C3 O5 Co2 127.12(19) . 2_655 ? C3 O5 Co1 133.0(2) . . ? Co2 O5 Co1 96.92(8) 2_655 . ? C3 O6 Co3 131.9(2) . . ? C4 O7 Co1 133.3(2) . . ? C4 O7 Co2 126.3(2) . . ? Co1 O7 Co2 97.78(9) . . ? C4 O8 Co4 132.1(2) . . ? C5 O9 Co1 124.5(2) . . ? C5 O9 Co3 120.3(2) . . ? Co1 O9 Co3 115.23(10) . . ? C5 O10 Co4 139.0(2) . . ? C6 O11 Co1 128.6(2) . . ? C6 O11 Co4 118.3(2) . . ? Co1 O11 Co4 113.07(9) . . ? C6 O12 Co2 131.3(2) . 2_655 ? O2 C1 O1 125.7(3) . . ? O2 C1 H1 120.0(14) . . ? O1 C1 H1 114.3(14) . . ? O4 C2 O3 125.8(4) . . ? O4 C2 H2 118(2) . . ? O3 C2 H2 116(2) . . ? O6 C3 O5 126.6(3) . . ? O6 C3 H3 117.3(18) . . ? O5 C3 H3 116.1(18) . . ? O8 C4 O7 126.9(3) . . ? O8 C4 H4 119(2) . . ? O7 C4 H4 113(2) . . ? O10 C5 O9 126.8(3) . . ? O10 C5 H5 121(2) . . ? O9 C5 H5 113(2) . . ? O12 C6 O11 125.4(3) . . ? O12 C6 H6 115.9(17) . . ? O11 C6 H6 118.8(17) . . ? 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 C1 H1 O3 1.06(3) 2.68(3) 3.293(4) 116.3(17) 2_655 C1 H1 O6 1.06(3) 2.58(3) 3.409(4) 134.5(19) 4_566 C1 H1 O9 1.06(3) 2.69(3) 3.663(4) 152(2) 2_655 C2 H2 O12 0.91(4) 2.70(3) 3.217(4) 117(3) 2_645 C3 H3 O2 0.99(3) 2.55(3) 3.165(4) 120(2) 2_655 C4 H4 O5 1.02(3) 2.77(4) 3.432(4) 123(2) 2_645 C5 H5 O4 0.91(3) 2.51(3) 2.937(4) 109(2) 3_655 C5 H5 O6 0.91(3) 2.71(3) 3.178(4) 113(3) 3_655 C6 H6 O8 1.01(3) 2.66(3) 3.092(4) 106(2) 3 C6 H6 O10 1.01(3) 2.56(3) 2.971(4) 104(2) 3 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.455 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.110 ## End of data_2-at-180K