# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1676 data_global # SUBMISSION DETAILS _publ_contact_author_name 'Dr Elisabeth Bouwman' _publ_contact_author_address ; Leiden Institute of Chemistry Gorlaeus Laboratories Leiden University PO Box 9502 2300 RA Leiden The Netherlands ; _publ_contact_author_email bouwman@chem.leidenuniv.nl _publ_contact_author_fax '(071) 527 4451' _publ_contact_author_phone '(071) 527 4459' _publ_contact_letter ; The following structures related to the manuscript submitted to Chem. Commun.: Novel Tetrahedral and Octahedral Cobalt(III) centres: Crystal Structures of [Co~4~(\m-Cl)~6~Cl~2~(thf)~4~(MeOH)~2~]~n~ and [{Co~4~(\m-Cl)~6~Cl~2~(thf)~4~(H~2~O)~2~}.2THF]~n~. Manuscript number: The crystallisation solvents used were methanol and dichloromethane. The hydrogen atoms involved in inter and intra molecular hydrogen bonding, were located in the difference Fourier and their thermal parameters allowed to refined freely. All other hydrogen atoms were constrained to have U~iso~ = 1.2Ueq of parent atom. ; _publ_requested_journal 'Chemical Communication' _publ_requested_category ? _publ_requested_coeditor_name ? # TITLE AND AUTHOR LIST _publ_section_title ; Unique Chains of alternating octahedral and tetrahedral cobalt(II) sites: crustal structures of the novel chloro-bridged complexes [Co~4~(\m-Cl)~6~Cl~2~(thf)~4~(MeOH)~2~]~n~ and [Co~4~(\m-Cl)~6~Cl~2~(thf)~4~(H~2~O)~2~.2THF]~n~ ; _publ_section_title_footnote ; ? ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Hierso, Jean-Cyrille' ;? ; ; Leiden Institute of Chemistry Gorlaeus Laboratories Leiden University PO Box 9502 2300 RA Leiden The Netherlands ; 'Ellis, Dianne D' ;For correspondence concerning the crystallographic studies ; ; Bijvoet Center for Biomolecular Research Department of Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; 'Spek, Anthony L' ;? ; ; Bijvoet Center for Biomolecular Research Department of Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; 'Bouwman, Elisabeth' ;? ; ; Leiden Institute of Chemistry Gorlaeus Laboratories Leiden University PO Box 9502 2300 RA Leiden The Netherlands ; 'Reedijk, Jan' ;? ; ; Leiden Institute of Chemistry Gorlaeus Laboratories Leiden University PO Box 9502 2300 RA Leiden The Netherlands ; #======================================================================= # TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_acknowledgements ; ? ; _publ_section_references ; Nonius B.V. (1998). Collect. Data Collection Software. Sheldrick, G.M. (1997a). SHELXL97. Program for Crystal Structure Refinement. University of G\"ottingen, Germany. Sheldrick, G.M. (1997b). SHELXS97. Program for Crystal Structure Solution. University of G\"ottingen, Germany. Spek, A.L. (2000). PLATON. A Multipurpose Crystallographic Tool. Utrecht University, The Netherlands. ; _publ_section_figure_captions ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; Diffracted intensities were collected on an Nonius Kappa CCD with rotating anode using graphite-monochromated Mo-Ka X-radiation. The final unit cell dimensions were determined from all reflections. The data were corrected for Lorentz, polarization and absorption effects. Hydrogen atoms, except those on oxygen were constrained to idealized geometries and assigned isotropic displacement paramaters 1.2 times U~iso~ value of their attached carbon atoms. The hydrogen atoms involved in hydrogen bonding were located in the Fourier map and their coordinates and thermal parameters freely refined. ; #======================================================================= data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H20 Cl4 Co2 O3' _chemical_formula_sum 'C9 H20 Cl4 Co2 O3' _chemical_formula_weight 435.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.9390(3) _cell_length_b 12.1510(4) _cell_length_c 12.6313(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.068(2) _cell_angle_gamma 90.00 _cell_volume 1635.47(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plates _exptl_crystal_colour blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.770 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 2.677 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5956 _exptl_absorpt_correction_T_max 0.6461 _exptl_absorpt_process_details 'MULscanABS in PLATON (Spek, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '\p scans with \k at 0\% and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% negligible _diffrn_reflns_number 15654 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_sigmaI/netI 0.0450 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3728 _reflns_number_gt 2975 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT ' _computing_cell_refinement 'DENZO 1.11.0' _computing_data_reduction 'DENZO 1.11.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997b)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)' _computing_molecular_graphics 'PLATON (Spek, 2000)' _computing_publication_material 'PLATON (Spek, 2000)' _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^)+(0.0231P)^2^+1.7350P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 3728 _refine_ls_number_parameters 171 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0488 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0736 _refine_ls_wR_factor_gt 0.0682 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.5000 0.5000 0.0000 0.01628(12) Uani 1 2 d S . . Co2 Co 0.71063(3) 0.47359(3) 0.22579(3) 0.01948(10) Uani 1 1 d . . . Co3 Co 1.0000 0.5000 0.5000 0.01722(12) Uani 1 2 d S . . Cl1 Cl 0.49854(6) 0.50308(6) 0.19444(5) 0.02185(15) Uani 1 1 d . . . Cl2 Cl 0.73657(6) 0.52806(6) 0.05902(5) 0.02383(16) Uani 1 1 d . . . Cl3 Cl 0.77143(7) 0.29723(6) 0.25794(5) 0.02548(16) Uani 1 1 d . . . Cl4 Cl 0.80623(6) 0.57385(6) 0.37511(5) 0.02349(16) Uani 1 1 d . . . O1 O 1.07727(19) 0.65599(16) 0.51336(17) 0.0226(4) Uani 1 1 d . . . H1 H 1.120(3) 0.664(3) 0.565(3) 0.040(12) Uiso 1 1 d . . . C2 C 1.0313(3) 0.7619(2) 0.4705(2) 0.0271(7) Uani 1 1 d . . . H2A H 0.9983 0.7561 0.3918 0.041 Uiso 1 1 calc R . . H2B H 1.1001 0.8154 0.4854 0.041 Uiso 1 1 calc R . . H2C H 0.9644 0.7862 0.5052 0.041 Uiso 1 1 calc R . . O10 O 0.52518(18) 0.33389(15) 0.01191(15) 0.0230(4) Uani 1 1 d . . . C11 C 0.6092(4) 0.2726(3) -0.0405(3) 0.0430(9) Uani 1 1 d . . . H11A H 0.5934 0.2921 -0.1185 0.052 Uiso 1 1 calc R . . H11B H 0.6976 0.2904 -0.0062 0.052 Uiso 1 1 calc R . . C12 C 0.5859(4) 0.1581(3) -0.0282(4) 0.0610(12) Uani 1 1 d . . . H12A H 0.6656 0.1199 0.0037 0.073 Uiso 1 1 calc R . . H12B H 0.5501 0.1250 -0.1002 0.073 Uiso 1 1 calc R . . C13 C 0.4982(4) 0.1445(3) 0.0426(3) 0.0414(9) Uani 1 1 d . . . H13A H 0.5403 0.1085 0.1115 0.050 Uiso 1 1 calc R . . H13B H 0.4260 0.0985 0.0066 0.050 Uiso 1 1 calc R . . C14 C 0.4549(3) 0.2564(2) 0.0643(3) 0.0286(7) Uani 1 1 d . . . H14A H 0.3636 0.2640 0.0337 0.034 Uiso 1 1 calc R . . H14B H 0.4718 0.2704 0.1435 0.034 Uiso 1 1 calc R . . O20 O 1.07433(19) 0.46593(15) 0.36677(15) 0.0242(4) Uani 1 1 d . . . C21 C 1.1290(3) 0.3618(2) 0.3435(2) 0.0276(7) Uani 1 1 d . . . H21A H 1.0627 0.3089 0.3099 0.033 Uiso 1 1 calc R . . H21B H 1.1802 0.3289 0.4108 0.033 Uiso 1 1 calc R . . C22 C 1.2100(3) 0.3916(3) 0.2652(3) 0.0380(8) Uani 1 1 d . . . H22A H 1.2953 0.4135 0.3046 0.046 Uiso 1 1 calc R . . H22B H 1.2165 0.3293 0.2163 0.046 Uiso 1 1 calc R . . C23 C 1.1406(3) 0.4873(3) 0.2028(3) 0.0385(8) Uani 1 1 d . . . H23A H 1.1980 0.5342 0.1720 0.046 Uiso 1 1 calc R . . H23B H 1.0716 0.4614 0.1431 0.046 Uiso 1 1 calc R . . C24 C 1.0904(3) 0.5486(3) 0.2870(3) 0.0365(8) Uani 1 1 d . . . H24A H 1.1502 0.6062 0.3216 0.044 Uiso 1 1 calc R . . H24B H 1.0092 0.5839 0.2538 0.044 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 0.0161(3) 0.0181(3) 0.0145(3) -0.0001(2) 0.0030(2) 0.0007(2) Co2 0.0190(2) 0.0221(2) 0.01588(19) -0.00019(15) 0.00091(15) 0.00085(15) Co3 0.0182(3) 0.0184(3) 0.0147(3) 0.0004(2) 0.0031(2) -0.0011(2) Cl1 0.0190(3) 0.0302(4) 0.0164(3) -0.0009(3) 0.0040(3) 0.0008(3) Cl2 0.0203(3) 0.0311(4) 0.0203(3) 0.0030(3) 0.0051(3) -0.0003(3) Cl3 0.0301(4) 0.0221(4) 0.0211(3) -0.0021(3) -0.0008(3) 0.0033(3) Cl4 0.0218(3) 0.0233(3) 0.0217(3) -0.0030(3) -0.0026(3) 0.0010(3) O1 0.0235(11) 0.0205(10) 0.0201(11) 0.0017(9) -0.0027(9) -0.0038(8) C2 0.0329(17) 0.0193(14) 0.0259(16) 0.0063(12) 0.0003(13) -0.0027(12) O10 0.0270(11) 0.0174(10) 0.0283(11) 0.0010(8) 0.0142(9) 0.0016(8) C11 0.056(2) 0.0298(18) 0.057(2) 0.0008(16) 0.0416(19) 0.0105(16) C12 0.075(3) 0.0221(18) 0.108(3) -0.011(2) 0.067(3) -0.0063(18) C13 0.058(2) 0.0215(16) 0.054(2) 0.0050(15) 0.0317(18) 0.0029(16) C14 0.0280(16) 0.0240(16) 0.0377(18) 0.0007(13) 0.0155(14) -0.0043(12) O20 0.0333(12) 0.0210(10) 0.0216(10) 0.0017(8) 0.0129(9) 0.0005(9) C21 0.0285(16) 0.0274(16) 0.0282(16) -0.0029(13) 0.0091(13) 0.0036(13) C22 0.0342(19) 0.044(2) 0.0405(19) -0.0038(16) 0.0183(16) 0.0002(15) C23 0.048(2) 0.040(2) 0.0323(18) -0.0007(15) 0.0197(16) -0.0018(16) C24 0.052(2) 0.0324(18) 0.0311(17) 0.0088(14) 0.0220(16) -0.0007(15) _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 O10 2.0381(18) . y Co1 O10 2.0381(18) 3_665 y Co1 Cl1 2.4599(6) . y Co1 Cl1 2.4599(6) 3_665 y Co1 Cl2 2.5488(7) 3_665 y Co1 Cl2 2.5488(7) . y Co2 Cl3 2.2533(8) . y Co2 Cl2 2.2862(7) . y Co2 Cl4 2.2898(7) . y Co2 Cl1 2.2918(7) . y Co3 O1 2.067(2) . y Co3 O1 2.067(2) 3_766 y Co3 O20 2.0695(18) 3_766 y Co3 O20 2.0696(18) . y Co3 Cl4 2.5049(7) 3_766 y Co3 Cl4 2.5049(7) . y O1 C2 1.442(3) . y O1 H1 0.72(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? O10 C11 1.453(3) . ? O10 C14 1.465(3) . ? C11 C12 1.430(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.462(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.485(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? O20 C21 1.457(3) . ? O20 C24 1.462(3) . ? C21 C22 1.513(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.510(5) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.500(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? 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 O10 Co1 O10 180.0 . 3_665 y O10 Co1 Cl1 88.43(5) . . y O10 Co1 Cl1 91.57(5) 3_665 . y O10 Co1 Cl1 91.57(5) . 3_665 y O10 Co1 Cl1 88.43(5) 3_665 3_665 ? Cl1 Co1 Cl1 179.999(1) . 3_665 y O10 Co1 Cl2 90.02(6) . 3_665 y O10 Co1 Cl2 89.97(6) 3_665 3_665 ? Cl1 Co1 Cl2 93.36(2) . 3_665 y Cl1 Co1 Cl2 86.64(2) 3_665 3_665 ? O10 Co1 Cl2 89.98(6) . . y O10 Co1 Cl2 90.03(6) 3_665 . y Cl1 Co1 Cl2 86.64(2) . . y Cl1 Co1 Cl2 93.36(2) 3_665 . ? Cl2 Co1 Cl2 180.0 3_665 . y Cl3 Co2 Cl2 110.38(3) . . y Cl3 Co2 Cl4 107.24(3) . . y Cl2 Co2 Cl4 118.44(3) . . y Cl3 Co2 Cl1 115.21(3) . . y Cl2 Co2 Cl1 97.31(3) . . y Cl4 Co2 Cl1 108.37(3) . . y O1 Co3 O1 180.0 . 3_766 y O1 Co3 O20 88.78(8) . 3_766 y O1 Co3 O20 91.21(8) 3_766 3_766 ? O1 Co3 O20 91.22(8) . . y O1 Co3 O20 88.79(8) 3_766 . ? O20 Co3 O20 180.00(15) 3_766 . y O1 Co3 Cl4 90.28(6) . 3_766 y O1 Co3 Cl4 89.72(6) 3_766 3_766 ? O20 Co3 Cl4 89.52(6) 3_766 3_766 ? O20 Co3 Cl4 90.48(6) . 3_766 y O1 Co3 Cl4 89.72(6) . . y O1 Co3 Cl4 90.28(6) 3_766 . ? O20 Co3 Cl4 90.48(6) 3_766 . ? O20 Co3 Cl4 89.52(6) . . y Cl4 Co3 Cl4 180.00(3) 3_766 . y Co2 Cl1 Co1 86.29(2) . . y Co2 Cl2 Co1 84.34(2) . . y Co2 Cl4 Co3 119.47(3) . . y C2 O1 Co3 133.36(17) . . y C2 O1 H1 109(3) . . ? Co3 O1 H1 112(3) . . ? O1 C2 H2A 109.5 . . ? O1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? O1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C11 O10 C14 109.1(2) . . ? C11 O10 Co1 124.22(17) . . ? C14 O10 Co1 126.44(16) . . ? C12 C11 O10 107.6(3) . . ? C12 C11 H11A 110.2 . . ? O10 C11 H11A 110.2 . . ? C12 C11 H11B 110.2 . . ? O10 C11 H11B 110.2 . . ? H11A C11 H11B 108.5 . . ? C11 C12 C13 109.5(3) . . ? C11 C12 H12A 109.8 . . ? C13 C12 H12A 109.8 . . ? C11 C12 H12B 109.8 . . ? C13 C12 H12B 109.8 . . ? H12A C12 H12B 108.2 . . ? C12 C13 C14 106.9(3) . . ? C12 C13 H13A 110.3 . . ? C14 C13 H13A 110.3 . . ? C12 C13 H13B 110.3 . . ? C14 C13 H13B 110.3 . . ? H13A C13 H13B 108.6 . . ? O10 C14 C13 106.5(2) . . ? O10 C14 H14A 110.4 . . ? C13 C14 H14A 110.4 . . ? O10 C14 H14B 110.4 . . ? C13 C14 H14B 110.4 . . ? H14A C14 H14B 108.6 . . ? C21 O20 C24 109.8(2) . . ? C21 O20 Co3 126.30(16) . . ? C24 O20 Co3 123.63(17) . . ? O20 C21 C22 104.6(2) . . ? O20 C21 H21A 110.8 . . ? C22 C21 H21A 110.8 . . ? O20 C21 H21B 110.8 . . ? C22 C21 H21B 110.8 . . ? H21A C21 H21B 108.9 . . ? C23 C22 C21 103.1(3) . . ? C23 C22 H22A 111.2 . . ? C21 C22 H22A 111.2 . . ? C23 C22 H22B 111.2 . . ? C21 C22 H22B 111.2 . . ? H22A C22 H22B 109.1 . . ? C24 C23 C22 103.5(3) . . ? C24 C23 H23A 111.1 . . ? C22 C23 H23A 111.1 . . ? C24 C23 H23B 111.1 . . ? C22 C23 H23B 111.1 . . ? H23A C23 H23B 109.0 . . ? O20 C24 C23 105.5(2) . . ? O20 C24 H24A 110.6 . . ? C23 C24 H24A 110.6 . . ? O20 C24 H24B 110.6 . . ? C23 C24 H24B 110.6 . . ? H24A C24 H24B 108.8 . . ? 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 Cl3 Co2 Cl1 Co1 -97.94(3) . . . . ? Cl2 Co2 Cl1 Co1 18.71(3) . . . . ? Cl4 Co2 Cl1 Co1 141.97(3) . . . . ? O10 Co1 Cl1 Co2 73.46(6) . . . . ? O10 Co1 Cl1 Co2 -106.54(6) 3_665 . . . ? Cl1 Co1 Cl1 Co2 38(24) 3_665 . . . ? Cl2 Co1 Cl1 Co2 163.39(2) 3_665 . . . ? Cl2 Co1 Cl1 Co2 -16.61(2) . . . . ? Cl3 Co2 Cl2 Co1 102.29(3) . . . . ? Cl4 Co2 Cl2 Co1 -133.60(3) . . . . ? Cl1 Co2 Cl2 Co1 -18.08(3) . . . . ? O10 Co1 Cl2 Co2 -71.73(5) . . . . ? O10 Co1 Cl2 Co2 108.27(5) 3_665 . . . ? Cl1 Co1 Cl2 Co2 16.70(2) . . . . ? Cl1 Co1 Cl2 Co2 -163.30(2) 3_665 . . . ? Cl2 Co1 Cl2 Co2 23(12) 3_665 . . . ? Cl3 Co2 Cl4 Co3 21.58(4) . . . . ? Cl2 Co2 Cl4 Co3 -104.07(4) . . . . ? Cl1 Co2 Cl4 Co3 146.53(3) . . . . ? O1 Co3 Cl4 Co2 139.28(6) . . . . ? O1 Co3 Cl4 Co2 -40.72(6) 3_766 . . . ? O20 Co3 Cl4 Co2 -131.94(6) 3_766 . . . ? O20 Co3 Cl4 Co2 48.06(6) . . . . ? Cl4 Co3 Cl4 Co2 -33(41) 3_766 . . . ? O1 Co3 O1 C2 -86(32) 3_766 . . . ? O20 Co3 O1 C2 -87.9(2) 3_766 . . . ? O20 Co3 O1 C2 92.1(2) . . . . ? Cl4 Co3 O1 C2 -177.4(2) 3_766 . . . ? Cl4 Co3 O1 C2 2.6(2) . . . . ? O10 Co1 O10 C11 126(3) 3_665 . . . ? Cl1 Co1 O10 C11 -139.2(2) . . . . ? Cl1 Co1 O10 C11 40.8(2) 3_665 . . . ? Cl2 Co1 O10 C11 127.5(2) 3_665 . . . ? Cl2 Co1 O10 C11 -52.5(2) . . . . ? O10 Co1 O10 C14 -48(3) 3_665 . . . ? Cl1 Co1 O10 C14 47.1(2) . . . . ? Cl1 Co1 O10 C14 -132.9(2) 3_665 . . . ? Cl2 Co1 O10 C14 -46.3(2) 3_665 . . . ? Cl2 Co1 O10 C14 133.7(2) . . . . ? C14 O10 C11 C12 4.1(4) . . . . ? Co1 O10 C11 C12 -170.6(3) . . . . ? O10 C11 C12 C13 -6.6(5) . . . . ? C11 C12 C13 C14 6.6(5) . . . . ? C11 O10 C14 C13 0.0(3) . . . . ? Co1 O10 C14 C13 174.5(2) . . . . ? C12 C13 C14 O10 -3.9(4) . . . . ? O1 Co3 O20 C21 140.5(2) . . . . ? O1 Co3 O20 C21 -39.5(2) 3_766 . . . ? O20 Co3 O20 C21 -66(13) 3_766 . . . ? Cl4 Co3 O20 C21 50.2(2) 3_766 . . . ? Cl4 Co3 O20 C21 -129.8(2) . . . . ? O1 Co3 O20 C24 -33.2(2) . . . . ? O1 Co3 O20 C24 146.8(2) 3_766 . . . ? O20 Co3 O20 C24 121(13) 3_766 . . . ? Cl4 Co3 O20 C24 -123.5(2) 3_766 . . . ? Cl4 Co3 O20 C24 56.5(2) . . . . ? C24 O20 C21 C22 14.9(3) . . . . ? Co3 O20 C21 C22 -159.43(19) . . . . ? O20 C21 C22 C23 -31.8(3) . . . . ? C21 C22 C23 C24 36.7(3) . . . . ? C21 O20 C24 C23 8.2(3) . . . . ? Co3 O20 C24 C23 -177.3(2) . . . . ? C22 C23 C24 O20 -28.0(3) . . . . ? 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 _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # O1 H1 Cl3 0.72(4) 2.33(4) 3.041(2) 170(4) 3_766 yes _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.687 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.092 #===end #======================================================================= data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H18 Cl4 Co2 O3, C4 H8 O' _chemical_formula_sum 'C12 H26 Cl4 Co2 O4' _chemical_formula_weight 493.99 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6714(3) _cell_length_b 10.8418(3) _cell_length_c 11.8514(5) _cell_angle_alpha 76.563(2) _cell_angle_beta 77.804(2) _cell_angle_gamma 68.245(2) _cell_volume 996.81(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needles _exptl_crystal_colour blue _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.646 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 504 _exptl_absorpt_coefficient_mu 2.210 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.71659 _exptl_absorpt_correction_T_max 0.77039 _exptl_absorpt_process_details 'MULscanABS in PLATON (Spek, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '\f scans with \k at 0\% and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10959 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4520 _reflns_number_gt 3674 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'DENZO 1.11.0' _computing_data_reduction 'DENZO 1.11.0' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997b)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997a)' _computing_molecular_graphics 'PLATON (Spek, 1999)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997b)' _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^)+(0.0181P)^2^+0.3456P] 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 4520 _refine_ls_number_parameters 210 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0699 _refine_ls_wR_factor_gt 0.0651 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 0.0000 0.0000 1.0000 0.01776(10) Uani 1 2 d S . . Co2 Co -0.09792(4) 0.22120(3) 0.76607(3) 0.02132(9) Uani 1 1 d . . . Co3 Co 0.0000 0.5000 0.5000 0.01940(11) Uani 1 2 d S . . Cl1 Cl 0.04700(7) 0.21313(5) 0.91070(5) 0.02503(14) Uani 1 1 d . . . Cl2 Cl -0.08369(7) -0.00083(5) 0.81272(5) 0.02445(13) Uani 1 1 d . . . Cl3 Cl -0.36211(7) 0.36674(6) 0.77951(6) 0.03533(16) Uani 1 1 d . . . Cl4 Cl 0.04571(7) 0.25833(5) 0.58491(5) 0.02309(13) Uani 1 1 d . . . O1 O 0.2463(2) 0.44397(19) 0.43518(16) 0.0300(4) Uani 1 1 d . . . H1A H 0.319(3) 0.377(3) 0.464(2) 0.043(9) Uiso 1 1 d . . . H1B H 0.284(3) 0.491(3) 0.388(3) 0.044(9) Uiso 1 1 d . . . O10 O 0.24701(18) -0.10804(15) 0.94454(14) 0.0260(4) Uani 1 1 d . . . C11 C 0.3921(3) -0.0729(3) 0.9494(2) 0.0372(6) Uani 1 1 d . . . H11A H 0.3927 -0.0614 1.0297 0.045 Uiso 1 1 calc R . . H11B H 0.3902 0.0121 0.8952 0.045 Uiso 1 1 calc R . . C12 C 0.5423(3) -0.1869(3) 0.9135(3) 0.0460(7) Uani 1 1 d . . . H12A H 0.5832 -0.2538 0.9827 0.055 Uiso 1 1 calc R . . H12B H 0.6341 -0.1542 0.8693 0.055 Uiso 1 1 calc R . . C13 C 0.4810(4) -0.2469(3) 0.8374(3) 0.0553(9) Uani 1 1 d . . . H13A H 0.5479 -0.3435 0.8384 0.066 Uiso 1 1 calc R . . H13B H 0.4863 -0.1987 0.7555 0.066 Uiso 1 1 calc R . . C14 C 0.3025(3) -0.2288(2) 0.8919(2) 0.0307(6) Uani 1 1 d . . . H14A H 0.2322 -0.2171 0.8318 0.037 Uiso 1 1 calc R . . H14B H 0.2964 -0.3078 0.9522 0.037 Uiso 1 1 calc R . . O20 O -0.0519(2) 0.46862(15) 0.34626(14) 0.0286(4) Uani 1 1 d . . . C21 C -0.2032(3) 0.5445(2) 0.29269(19) 0.0227(5) Uani 1 1 d . . . H21A H -0.2215 0.6422 0.2784 0.027 Uiso 1 1 calc R . . H21B H -0.3020 0.5281 0.3443 0.027 Uiso 1 1 calc R . . C22 C -0.1762(3) 0.4950(2) 0.1774(2) 0.0300(6) Uani 1 1 d . . . H22A H -0.2500 0.4426 0.1810 0.036 Uiso 1 1 calc R . . H22B H -0.1992 0.5716 0.1116 0.036 Uiso 1 1 calc R . . C23 C 0.0068(3) 0.4065(3) 0.1631(2) 0.0384(6) Uani 1 1 d . . . H23A H 0.0243 0.3319 0.1217 0.046 Uiso 1 1 calc R . . H23B H 0.0790 0.4595 0.1194 0.046 Uiso 1 1 calc R . . C24 C 0.0420(3) 0.3545(2) 0.2864(2) 0.0361(6) Uani 1 1 d . . . H24A H 0.0029 0.2771 0.3210 0.043 Uiso 1 1 calc R . . H24B H 0.1634 0.3261 0.2905 0.043 Uiso 1 1 calc R . . O50 O 0.4950(2) 0.23637(18) 0.51517(17) 0.0506(6) Uani 1 1 d . . . C51 C 0.5132(3) 0.1317(2) 0.6159(2) 0.0390(6) Uani 1 1 d . . . H51A H 0.4146 0.1016 0.6364 0.047 Uiso 1 1 calc R . . H51B H 0.5263 0.1632 0.6841 0.047 Uiso 1 1 calc R . . C52 C 0.6690(3) 0.0194(2) 0.5800(2) 0.0391(7) Uani 1 1 d . . . H52A H 0.6407 -0.0464 0.5500 0.047 Uiso 1 1 calc R . . H52B H 0.7327 -0.0282 0.6467 0.047 Uiso 1 1 calc R . . C53 C 0.7677(4) 0.0904(3) 0.4846(3) 0.0682(11) Uani 1 1 d . . . H53A H 0.8742 0.0810 0.5094 0.082 Uiso 1 1 calc R . . H53B H 0.7939 0.0519 0.4121 0.082 Uiso 1 1 calc R . . C54 C 0.6593(3) 0.2354(3) 0.4644(3) 0.0407(7) Uani 1 1 d . . . H54A H 0.6961 0.2897 0.5027 0.049 Uiso 1 1 calc R . . H54B H 0.6631 0.2722 0.3796 0.049 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 0.0211(2) 0.0178(2) 0.0163(2) -0.00071(17) -0.00369(17) -0.00941(18) Co2 0.02314(18) 0.02125(16) 0.01801(17) 0.00083(12) -0.00355(13) -0.00785(13) Co3 0.0182(2) 0.0202(2) 0.0151(2) -0.00110(17) -0.00098(17) -0.00301(17) Cl1 0.0357(3) 0.0231(3) 0.0216(3) 0.0014(2) -0.0076(2) -0.0171(3) Cl2 0.0339(3) 0.0236(3) 0.0200(3) -0.0012(2) -0.0075(2) -0.0138(2) Cl3 0.0253(3) 0.0335(3) 0.0332(4) 0.0057(3) 0.0016(3) -0.0039(3) Cl4 0.0256(3) 0.0201(3) 0.0192(3) -0.0006(2) 0.0000(2) -0.0062(2) O1 0.0198(9) 0.0275(9) 0.0278(10) 0.0090(8) 0.0008(8) -0.0014(8) O10 0.0200(8) 0.0261(8) 0.0359(10) -0.0146(7) -0.0008(7) -0.0087(7) C11 0.0239(14) 0.0484(16) 0.0494(18) -0.0204(14) 0.0004(12) -0.0195(13) C12 0.0254(15) 0.0510(17) 0.063(2) -0.0189(15) -0.0021(14) -0.0106(13) C13 0.0384(18) 0.0575(19) 0.075(2) -0.0380(17) 0.0118(16) -0.0162(15) C14 0.0302(14) 0.0288(13) 0.0367(15) -0.0166(11) -0.0003(11) -0.0096(11) O20 0.0289(9) 0.0268(8) 0.0236(9) -0.0101(7) -0.0106(7) 0.0052(7) C21 0.0204(12) 0.0232(11) 0.0233(13) -0.0018(10) -0.0047(10) -0.0064(9) C22 0.0356(15) 0.0295(13) 0.0285(14) -0.0054(11) -0.0108(11) -0.0114(11) C23 0.0379(16) 0.0464(16) 0.0316(15) -0.0159(13) -0.0053(12) -0.0091(13) C24 0.0381(16) 0.0316(13) 0.0296(15) -0.0133(11) -0.0040(12) 0.0028(12) O50 0.0264(10) 0.0441(11) 0.0514(13) 0.0195(9) -0.0010(9) 0.0033(8) C51 0.0410(16) 0.0341(14) 0.0340(16) 0.0015(12) -0.0060(13) -0.0078(12) C52 0.0416(16) 0.0300(13) 0.0445(17) -0.0078(12) -0.0213(13) -0.0017(12) C53 0.0373(19) 0.0429(17) 0.107(3) -0.0182(18) 0.0143(19) -0.0035(15) C54 0.0279(15) 0.0425(15) 0.0454(18) -0.0045(13) -0.0019(13) -0.0081(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 O10 2.0724(15) . y Co1 O10 2.0725(15) 2_557 y Co1 Cl1 2.4505(5) . y Co1 Cl1 2.4505(5) 2_557 y Co1 Cl2 2.4794(5) . y Co1 Cl2 2.4795(5) 2_557 y Co2 Cl3 2.2464(7) . y Co2 Cl4 2.2723(6) . y Co2 Cl1 2.2986(6) . y Co2 Cl2 2.3034(6) . y Co3 O1 2.0203(17) . y Co3 O1 2.0203(17) 2_566 y Co3 O20 2.0944(16) . y Co3 O20 2.0944(16) 2_566 y Co3 Cl4 2.4916(5) 2_566 y Co3 Cl4 2.4916(5) . y O1 H1A 0.82(3) . y O1 H1B 0.77(3) . y O10 C14 1.456(3) . ? O10 C11 1.458(3) . ? C11 C12 1.491(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.501(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.504(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? O20 C21 1.452(2) . ? O20 C24 1.454(3) . ? C21 C22 1.523(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.517(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.491(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? O50 C54 1.421(3) . ? O50 C51 1.434(3) . ? C51 C52 1.505(4) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.510(4) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.496(4) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? 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 O10 Co1 O10 180.0 . 2_557 y O10 Co1 Cl1 90.91(4) . . y O10 Co1 Cl1 89.09(4) 2_557 . y O10 Co1 Cl1 89.09(4) . 2_557 ? O10 Co1 Cl1 90.91(4) 2_557 2_557 ? Cl1 Co1 Cl1 180.0 . 2_557 y O10 Co1 Cl2 90.84(5) . . y O10 Co1 Cl2 89.16(5) 2_557 . y Cl1 Co1 Cl2 88.197(17) . . y Cl1 Co1 Cl2 91.804(17) 2_557 . y O10 Co1 Cl2 89.16(5) . 2_557 ? O10 Co1 Cl2 90.84(5) 2_557 2_557 ? Cl1 Co1 Cl2 91.805(17) . 2_557 ? Cl1 Co1 Cl2 88.194(17) 2_557 2_557 ? Cl2 Co1 Cl2 180.0 . 2_557 y Cl3 Co2 Cl4 111.43(2) . . y Cl3 Co2 Cl1 113.96(3) . . y Cl4 Co2 Cl1 111.55(2) . . y Cl3 Co2 Cl2 113.06(2) . . y Cl4 Co2 Cl2 109.57(2) . . y Cl1 Co2 Cl2 96.40(2) . . y O1 Co3 O1 179.999(2) . 2_566 y O1 Co3 O20 89.38(7) . . y O1 Co3 O20 90.63(7) 2_566 . y O1 Co3 O20 90.62(7) . 2_566 ? O1 Co3 O20 89.37(7) 2_566 2_566 ? O20 Co3 O20 180.0 . 2_566 y O1 Co3 Cl4 92.47(5) . 2_566 y O1 Co3 Cl4 87.53(5) 2_566 2_566 ? O20 Co3 Cl4 90.53(4) . 2_566 ? O20 Co3 Cl4 89.47(4) 2_566 2_566 ? O1 Co3 Cl4 87.53(5) . . y O1 Co3 Cl4 92.47(5) 2_566 . ? O20 Co3 Cl4 89.47(4) . . y O20 Co3 Cl4 90.53(4) 2_566 . y Cl4 Co3 Cl4 180.0 2_566 . y Co2 Cl1 Co1 86.261(18) . . y Co2 Cl2 Co1 85.482(19) . . y Co2 Cl4 Co3 114.92(2) . . y Co3 O1 H1A 124.6(19) . . ? Co3 O1 H1B 122(2) . . ? H1A O1 H1B 112(3) . . ? C14 O10 C11 109.37(17) . . ? C14 O10 Co1 125.37(13) . . ? C11 O10 Co1 125.24(14) . . ? O10 C11 C12 106.0(2) . . ? O10 C11 H11A 110.5 . . ? C12 C11 H11A 110.5 . . ? O10 C11 H11B 110.5 . . ? C12 C11 H11B 110.5 . . ? H11A C11 H11B 108.7 . . ? C11 C12 C13 104.1(2) . . ? C11 C12 H12A 110.9 . . ? C13 C12 H12A 110.9 . . ? C11 C12 H12B 110.9 . . ? C13 C12 H12B 110.9 . . ? H12A C12 H12B 108.9 . . ? C12 C13 C14 103.6(2) . . ? C12 C13 H13A 111.0 . . ? C14 C13 H13A 111.0 . . ? C12 C13 H13B 111.0 . . ? C14 C13 H13B 111.0 . . ? H13A C13 H13B 109.0 . . ? O10 C14 C13 105.21(18) . . ? O10 C14 H14A 110.7 . . ? C13 C14 H14A 110.7 . . ? O10 C14 H14B 110.7 . . ? C13 C14 H14B 110.7 . . ? H14A C14 H14B 108.8 . . ? C21 O20 C24 107.95(17) . . ? C21 O20 Co3 125.42(13) . . ? C24 O20 Co3 125.89(14) . . ? O20 C21 C22 106.18(18) . . ? O20 C21 H21A 110.5 . . ? C22 C21 H21A 110.5 . . ? O20 C21 H21B 110.5 . . ? C22 C21 H21B 110.5 . . ? H21A C21 H21B 108.7 . . ? C23 C22 C21 104.50(19) . . ? C23 C22 H22A 110.9 . . ? C21 C22 H22A 110.9 . . ? C23 C22 H22B 110.9 . . ? C21 C22 H22B 110.9 . . ? H22A C22 H22B 108.9 . . ? C24 C23 C22 103.1(2) . . ? C24 C23 H23A 111.1 . . ? C22 C23 H23A 111.1 . . ? C24 C23 H23B 111.1 . . ? C22 C23 H23B 111.1 . . ? H23A C23 H23B 109.1 . . ? O20 C24 C23 103.93(19) . . ? O20 C24 H24A 111.0 . . ? C23 C24 H24A 111.0 . . ? O20 C24 H24B 111.0 . . ? C23 C24 H24B 111.0 . . ? H24A C24 H24B 109.0 . . ? C54 O50 C51 106.72(19) . . ? O50 C51 C52 104.7(2) . . ? O50 C51 H51A 110.8 . . ? C52 C51 H51A 110.8 . . ? O50 C51 H51B 110.8 . . ? C52 C51 H51B 110.8 . . ? H51A C51 H51B 108.9 . . ? C51 C52 C53 103.8(2) . . ? C51 C52 H52A 111.0 . . ? C53 C52 H52A 111.0 . . ? C51 C52 H52B 111.0 . . ? C53 C52 H52B 111.0 . . ? H52A C52 H52B 109.0 . . ? C54 C53 C52 106.2(2) . . ? C54 C53 H53A 110.5 . . ? C52 C53 H53A 110.5 . . ? C54 C53 H53B 110.5 . . ? C52 C53 H53B 110.5 . . ? H53A C53 H53B 108.7 . . ? O50 C54 C53 105.0(2) . . ? O50 C54 H54A 110.7 . . ? C53 C54 H54A 110.7 . . ? O50 C54 H54B 110.7 . . ? C53 C54 H54B 110.7 . . ? H54A C54 H54B 108.8 . . ? 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 Cl3 Co2 Cl1 Co1 103.71(2) . . . . ? Cl4 Co2 Cl1 Co1 -129.05(2) . . . . ? Cl2 Co2 Cl1 Co1 -15.05(2) . . . . ? O10 Co1 Cl1 Co2 104.69(5) . . . . ? O10 Co1 Cl1 Co2 -75.31(5) 2_557 . . . ? Cl1 Co1 Cl1 Co2 -143(20) 2_557 . . . ? Cl2 Co1 Cl1 Co2 13.88(2) . . . . ? Cl2 Co1 Cl1 Co2 -166.12(2) 2_557 . . . ? Cl3 Co2 Cl2 Co1 -104.57(3) . . . . ? Cl4 Co2 Cl2 Co1 130.49(2) . . . . ? Cl1 Co2 Cl2 Co1 14.89(2) . . . . ? O10 Co1 Cl2 Co2 -104.75(4) . . . . ? O10 Co1 Cl2 Co2 75.25(4) 2_557 . . . ? Cl1 Co1 Cl2 Co2 -13.87(2) . . . . ? Cl1 Co1 Cl2 Co2 166.13(2) 2_557 . . . ? Cl2 Co1 Cl2 Co2 150.9(15) 2_557 . . . ? Cl3 Co2 Cl4 Co3 42.41(3) . . . . ? Cl1 Co2 Cl4 Co3 -86.19(3) . . . . ? Cl2 Co2 Cl4 Co3 168.29(2) . . . . ? O1 Co3 Cl4 Co2 141.31(6) . . . . ? O1 Co3 Cl4 Co2 -38.69(6) 2_566 . . . ? O20 Co3 Cl4 Co2 -129.29(5) . . . . ? O20 Co3 Cl4 Co2 50.71(5) 2_566 . . . ? Cl4 Co3 Cl4 Co2 1(9) 2_566 . . . ? O10 Co1 O10 C14 114(4) 2_557 . . . ? Cl1 Co1 O10 C14 -136.10(17) . . . . ? Cl1 Co1 O10 C14 43.90(17) 2_557 . . . ? Cl2 Co1 O10 C14 -47.89(17) . . . . ? Cl2 Co1 O10 C14 132.11(17) 2_557 . . . ? O10 Co1 O10 C11 -68(4) 2_557 . . . ? Cl1 Co1 O10 C11 42.22(18) . . . . ? Cl1 Co1 O10 C11 -137.78(18) 2_557 . . . ? Cl2 Co1 O10 C11 130.42(17) . . . . ? Cl2 Co1 O10 C11 -49.58(17) 2_557 . . . ? C14 O10 C11 C12 -7.8(3) . . . . ? Co1 O10 C11 C12 173.61(16) . . . . ? O10 C11 C12 C13 26.3(3) . . . . ? C11 C12 C13 C14 -34.3(3) . . . . ? C11 O10 C14 C13 -13.7(3) . . . . ? Co1 O10 C14 C13 164.79(18) . . . . ? C12 C13 C14 O10 29.6(3) . . . . ? O1 Co3 O20 C21 -147.47(16) . . . . ? O1 Co3 O20 C21 32.53(16) 2_566 . . . ? O20 Co3 O20 C21 109(10) 2_566 . . . ? Cl4 Co3 O20 C21 -55.00(15) 2_566 . . . ? Cl4 Co3 O20 C21 125.00(15) . . . . ? O1 Co3 O20 C24 43.62(18) . . . . ? O1 Co3 O20 C24 -136.38(18) 2_566 . . . ? O20 Co3 O20 C24 -60(10) 2_566 . . . ? Cl4 Co3 O20 C24 136.09(18) 2_566 . . . ? Cl4 Co3 O20 C24 -43.91(18) . . . . ? C24 O20 C21 C22 -14.9(2) . . . . ? Co3 O20 C21 C22 174.52(13) . . . . ? O20 C21 C22 C23 -9.1(2) . . . . ? C21 C22 C23 C24 28.7(2) . . . . ? C21 O20 C24 C23 33.5(2) . . . . ? Co3 O20 C24 C23 -156.03(15) . . . . ? C22 C23 C24 O20 -38.0(2) . . . . ? C54 O50 C51 C52 -37.5(3) . . . . ? O50 C51 C52 C53 24.8(3) . . . . ? C51 C52 C53 C54 -4.4(3) . . . . ? C51 O50 C54 C53 34.4(3) . . . . ? C52 C53 C54 O50 -17.7(3) . . . . ? 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 _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # O1 H1A O50 0.82(3) 1.81(3) 2.625(3) 174(3) . yes O1 H1B Cl3 0.77(3) 2.36(3) 3.117(2) 168(3) 2_566 yes _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.562 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.079