Supplementary data (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ;Synthesis and structure of two tetranuclear osmium carbonyl isotopomers: A crystallographic isotope effect ; _publ_contact_author_name 'John Canal' _publ_contact_author_email JCANAL@SFU.CA loop_ _publ_author_name 'John Canal' 'Michael C. Jennings' 'R. Pomeroy' 'Glenn P. A. Yap' #END # Attachment '2.cif' data_03110 _database_code_depnum_ccdc_archive 'CCDC 657923' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H2 O14 Os4' _chemical_formula_sum 'C13 H2 O14 Os4' _chemical_formula_weight 1142.95 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' Os Os -1.2165 7.6030 '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/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.2448(2) _cell_length_b 14.2439(3) _cell_length_c 15.2035(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.040(10) _cell_angle_gamma 90.00 _cell_volume 1986.93(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5872 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 30.03 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.821 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1984 _exptl_absorpt_coefficient_mu 25.568 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0538 _exptl_absorpt_correction_T_max 0.1423 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24430 _diffrn_reflns_av_R_equivalents 0.121 _diffrn_reflns_av_sigmaI/netI 0.0696 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3494 _reflns_number_gt 2791 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Nonius, 1997-2001)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 2001)' _computing_publication_material SHELXTL/PC _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^)+(0.0602P)^2^] 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 0.00119(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3494 _refine_ls_number_parameters 152 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.1067 _refine_ls_wR_factor_gt 0.1008 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 Os1 Os 0.75374(5) 0.80293(4) -0.09968(4) 0.00743(18) Uani 1 1 d D . . Os2 Os 0.74010(6) 0.84450(4) 0.08910(4) 0.00846(18) Uani 1 1 d D . . H H 0.693(14) 0.900(9) -0.026(2) 0.013 Uiso 1 1 d D . . Os3 Os 0.77562(6) 0.65932(4) 0.02998(4) 0.00786(18) Uani 1 1 d . . . Os4 Os 0.49120(6) 0.73324(4) 0.02781(4) 0.00909(18) Uani 1 1 d . . . O1 O 0.6948(11) 0.9607(8) -0.2357(7) 0.024(3) Uiso 1 1 d . . . C1 C 0.7155(14) 0.9050(10) -0.1836(9) 0.011(3) Uiso 1 1 d . . . O2 O 1.0778(11) 0.8362(8) -0.0798(7) 0.024(3) Uiso 1 1 d . . . C2 C 0.9565(16) 0.8224(10) -0.0888(10) 0.015(3) Uiso 1 1 d . . . O3 O 0.7790(12) 0.6617(8) -0.2453(8) 0.031(3) Uiso 1 1 d . . . C3 C 0.7673(16) 0.7141(11) -0.1898(10) 0.017(3) Uiso 1 1 d . . . O4 O 0.5779(11) 1.0253(7) 0.1179(7) 0.021(3) Uiso 1 1 d . . . C4 C 0.6375(17) 0.9575(12) 0.1060(10) 0.021(4) Uiso 1 1 d . . . O5 O 1.0238(12) 0.9505(8) 0.1272(8) 0.031(3) Uiso 1 1 d . . . C5 C 0.9206(15) 0.9105(11) 0.1141(10) 0.015(3) Uiso 1 1 d . . . O6 O 0.7390(12) 0.7742(8) 0.2769(7) 0.030(3) Uiso 1 1 d . . . C6 C 0.7410(15) 0.8007(10) 0.2078(9) 0.010(3) Uiso 1 1 d . . . O7 O 1.0750(12) 0.7267(8) 0.1131(7) 0.027(3) Uiso 1 1 d . . . C7 C 0.9575(15) 0.7130(10) 0.0845(9) 0.013(3) Uiso 1 1 d . . . O8 O 0.7729(12) 0.5279(9) 0.1903(8) 0.032(3) Uiso 1 1 d . . . C8 C 0.7704(14) 0.5783(10) 0.1321(9) 0.012(3) Uiso 1 1 d . . . O9 O 0.9296(10) 0.5300(7) -0.0892(7) 0.019(2) Uiso 1 1 d . . . C9 C 0.8773(16) 0.5784(11) -0.0420(10) 0.019(4) Uiso 1 1 d . . . O10 O 0.4706(12) 0.6502(8) 0.2091(7) 0.025(3) Uiso 1 1 d . . . C10 C 0.4791(14) 0.6829(10) 0.1396(9) 0.007(3) Uiso 1 1 d . . . O11 O 0.2170(11) 0.6225(8) -0.0421(7) 0.021(3) Uiso 1 1 d . . . C11 C 0.3225(15) 0.6643(10) -0.0188(10) 0.012(3) Uiso 1 1 d . . . O12 O 0.3166(11) 0.9068(8) 0.0656(7) 0.025(3) Uiso 1 1 d . . . C12 C 0.3868(16) 0.8421(11) 0.0522(10) 0.018(4) Uiso 1 1 d . . . O13 O 0.5366(11) 0.5474(8) -0.0853(7) 0.024(3) Uiso 1 1 d . . . C13 C 0.5975(13) 0.6013(10) -0.0350(8) 0.005(3) Uiso 1 1 d . . . O14 O 0.5277(10) 0.7762(7) -0.1006(6) 0.014(2) Uiso 1 1 d D . . H14 H 0.512(11) 0.835(2) -0.101(9) 0.021 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os1 0.0059(3) 0.0057(3) 0.0118(3) 0.0004(2) 0.0055(2) 0.0008(2) Os2 0.0065(3) 0.0067(3) 0.0130(3) -0.0022(2) 0.0043(2) 0.0003(2) Os3 0.0060(3) 0.0051(3) 0.0133(3) 0.0007(2) 0.0046(2) 0.0018(2) Os4 0.0035(3) 0.0101(4) 0.0148(3) 0.0008(2) 0.0055(2) -0.0001(2) _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 Os1 C3 1.880(15) . ? Os1 C2 1.882(14) . ? Os1 C1 1.939(14) . ? Os1 O14 2.123(9) . ? Os1 Os3 2.8308(8) . ? Os1 Os2 2.9484(8) . ? Os1 H 1.91(9) . ? Os2 C4 1.902(16) . ? Os2 C6 1.908(14) . ? Os2 C5 1.912(15) . ? Os2 Os3 2.8187(8) . ? Os2 Os4 2.8546(8) . ? Os2 H 1.91(9) . ? Os3 C9 1.913(15) . ? Os3 C7 1.938(15) . ? Os3 C8 1.939(14) . ? Os3 C13 1.993(13) . ? Os3 Os4 2.8287(7) . ? Os4 C10 1.861(13) . ? Os4 C12 1.887(15) . ? Os4 C11 1.905(14) . ? Os4 O14 2.111(10) . ? Os4 C13 2.375(13) . ? O1 C1 1.120(16) . ? O2 C2 1.130(17) . ? O3 C3 1.143(18) . ? O4 C4 1.137(17) . ? O5 C5 1.109(17) . ? O6 C6 1.119(16) . ? O7 C7 1.137(17) . ? O8 C8 1.138(17) . ? O9 C9 1.144(17) . ? O10 C10 1.166(17) . ? O11 C11 1.160(17) . ? O12 C12 1.159(17) . ? O13 C13 1.176(16) . ? O14 H14 0.856(18) . ? 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 C3 Os1 C2 90.5(6) . . ? C3 Os1 C1 92.8(6) . . ? C2 Os1 C1 92.7(6) . . ? C3 Os1 O14 91.6(5) . . ? C2 Os1 O14 175.0(5) . . ? C1 Os1 O14 91.8(5) . . ? C3 Os1 Os3 90.9(5) . . ? C2 Os1 Os3 93.4(5) . . ? C1 Os1 Os3 172.9(4) . . ? O14 Os1 Os3 82.0(3) . . ? C3 Os1 Os2 149.2(5) . . ? C2 Os1 Os2 92.6(4) . . ? C1 Os1 Os2 117.7(4) . . ? O14 Os1 Os2 83.3(3) . . ? Os3 Os1 Os2 58.341(19) . . ? C3 Os1 H 165(3) . . ? C2 Os1 H 102(4) . . ? C1 Os1 H 79(3) . . ? O14 Os1 H 77(4) . . ? Os3 Os1 H 96(3) . . ? Os2 Os1 H 40(3) . . ? C4 Os2 C6 95.4(6) . . ? C4 Os2 C5 89.7(6) . . ? C6 Os2 C5 94.0(6) . . ? C4 Os2 Os3 156.1(5) . . ? C6 Os2 Os3 90.5(4) . . ? C5 Os2 Os3 113.0(4) . . ? C4 Os2 Os4 96.8(5) . . ? C6 Os2 Os4 92.1(4) . . ? C5 Os2 Os4 170.6(4) . . ? Os3 Os2 Os4 59.81(2) . . ? C4 Os2 Os1 112.5(5) . . ? C6 Os2 Os1 149.2(4) . . ? C5 Os2 Os1 98.7(4) . . ? Os3 Os2 Os1 58.743(19) . . ? Os4 Os2 Os1 72.52(2) . . ? C4 Os2 H 73(3) . . ? C6 Os2 H 166(3) . . ? C5 Os2 H 94(4) . . ? Os3 Os2 H 97(3) . . ? Os4 Os2 H 81(4) . . ? Os1 Os2 H 40(3) . . ? C9 Os3 C7 91.2(6) . . ? C9 Os3 C8 99.3(6) . . ? C7 Os3 C8 89.9(6) . . ? C9 Os3 C13 84.3(6) . . ? C7 Os3 C13 175.1(5) . . ? C8 Os3 C13 92.9(6) . . ? C9 Os3 Os2 146.1(5) . . ? C7 Os3 Os2 67.9(4) . . ? C8 Os3 Os2 106.6(4) . . ? C13 Os3 Os2 115.1(4) . . ? C9 Os3 Os4 137.6(5) . . ? C7 Os3 Os4 127.9(4) . . ? C8 Os3 Os4 96.7(4) . . ? C13 Os3 Os4 55.8(4) . . ? Os2 Os3 Os4 60.725(19) . . ? C9 Os3 Os1 92.0(5) . . ? C7 Os3 Os1 89.8(4) . . ? C8 Os3 Os1 168.7(4) . . ? C13 Os3 Os1 88.3(4) . . ? Os2 Os3 Os1 62.92(2) . . ? Os4 Os3 Os1 74.69(2) . . ? C10 Os4 C12 92.7(6) . . ? C10 Os4 C11 90.2(6) . . ? C12 Os4 C11 94.7(6) . . ? C10 Os4 O14 172.0(5) . . ? C12 Os4 O14 95.0(5) . . ? C11 Os4 O14 91.2(5) . . ? C10 Os4 C13 97.8(5) . . ? C12 Os4 C13 167.5(6) . . ? C11 Os4 C13 78.6(5) . . ? O14 Os4 C13 74.7(4) . . ? C10 Os4 Os3 90.3(4) . . ? C12 Os4 Os3 143.2(5) . . ? C11 Os4 Os3 122.0(4) . . ? O14 Os4 Os3 82.2(3) . . ? C13 Os4 Os3 44.0(3) . . ? C10 Os4 Os2 93.0(4) . . ? C12 Os4 Os2 83.7(5) . . ? C11 Os4 Os2 176.5(4) . . ? O14 Os4 Os2 85.8(3) . . ? C13 Os4 Os2 102.4(3) . . ? Os3 Os4 Os2 59.464(19) . . ? O1 C1 Os1 176.2(13) . . ? O2 C2 Os1 177.6(14) . . ? O3 C3 Os1 177.9(14) . . ? O4 C4 Os2 178.4(14) . . ? O5 C5 Os2 178.2(15) . . ? O6 C6 Os2 178.6(14) . . ? O7 C7 Os3 165.9(13) . . ? O8 C8 Os3 176.3(13) . . ? O9 C9 Os3 175.3(13) . . ? O10 C10 Os4 179.1(13) . . ? O11 C11 Os4 175.8(12) . . ? O12 C12 Os4 176.8(14) . . ? O13 C13 Os3 153.3(11) . . ? O13 C13 Os4 126.1(10) . . ? Os3 C13 Os4 80.2(5) . . ? Os4 O14 Os1 108.4(4) . . ? Os4 O14 H14 104(10) . . ? Os1 O14 H14 89(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 Os1 Os2 C4 -152.1(10) . . . . ? C2 Os1 Os2 C4 112.6(7) . . . . ? C1 Os1 Os2 C4 18.2(7) . . . . ? O14 Os1 Os2 C4 -70.3(6) . . . . ? Os3 Os1 Os2 C4 -155.0(5) . . . . ? C3 Os1 Os2 C6 1.2(12) . . . . ? C2 Os1 Os2 C6 -94.1(9) . . . . ? C1 Os1 Os2 C6 171.5(9) . . . . ? O14 Os1 Os2 C6 83.0(8) . . . . ? Os3 Os1 Os2 C6 -1.7(8) . . . . ? C3 Os1 Os2 C5 114.6(10) . . . . ? C2 Os1 Os2 C5 19.2(6) . . . . ? C1 Os1 Os2 C5 -75.2(6) . . . . ? O14 Os1 Os2 C5 -163.6(5) . . . . ? Os3 Os1 Os2 C5 111.6(5) . . . . ? C3 Os1 Os2 Os3 3.0(9) . . . . ? C2 Os1 Os2 Os3 -92.4(5) . . . . ? C1 Os1 Os2 Os3 173.2(4) . . . . ? O14 Os1 Os2 Os3 84.7(3) . . . . ? C3 Os1 Os2 Os4 -61.8(9) . . . . ? C2 Os1 Os2 Os4 -157.2(5) . . . . ? C1 Os1 Os2 Os4 108.4(4) . . . . ? O14 Os1 Os2 Os4 19.9(3) . . . . ? Os3 Os1 Os2 Os4 -64.81(2) . . . . ? C4 Os2 Os3 C9 120.8(14) . . . . ? C6 Os2 Os3 C9 -134.7(9) . . . . ? C5 Os2 Os3 C9 -40.0(10) . . . . ? Os4 Os2 Os3 C9 133.2(8) . . . . ? Os1 Os2 Os3 C9 46.2(8) . . . . ? C4 Os2 Os3 C7 176.4(12) . . . . ? C6 Os2 Os3 C7 -79.1(6) . . . . ? C5 Os2 Os3 C7 15.5(6) . . . . ? Os4 Os2 Os3 C7 -171.3(4) . . . . ? Os1 Os2 Os3 C7 101.8(4) . . . . ? C4 Os2 Os3 C8 -100.7(12) . . . . ? C6 Os2 Os3 C8 3.8(6) . . . . ? C5 Os2 Os3 C8 98.4(6) . . . . ? Os4 Os2 Os3 C8 -88.4(4) . . . . ? Os1 Os2 Os3 C8 -175.3(4) . . . . ? C4 Os2 Os3 C13 0.7(12) . . . . ? C6 Os2 Os3 C13 105.2(6) . . . . ? C5 Os2 Os3 C13 -160.2(6) . . . . ? Os4 Os2 Os3 C13 13.0(4) . . . . ? Os1 Os2 Os3 C13 -73.9(4) . . . . ? C4 Os2 Os3 Os4 -12.3(12) . . . . ? C6 Os2 Os3 Os4 92.2(4) . . . . ? C5 Os2 Os3 Os4 -173.2(5) . . . . ? Os1 Os2 Os3 Os4 -86.94(2) . . . . ? C4 Os2 Os3 Os1 74.6(12) . . . . ? C6 Os2 Os3 Os1 179.1(4) . . . . ? C5 Os2 Os3 Os1 -86.3(5) . . . . ? Os4 Os2 Os3 Os1 86.94(2) . . . . ? C3 Os1 Os3 C9 25.3(6) . . . . ? C2 Os1 Os3 C9 -65.3(6) . . . . ? C1 Os1 Os3 C9 146(3) . . . . ? O14 Os1 Os3 C9 116.8(5) . . . . ? Os2 Os1 Os3 C9 -156.3(5) . . . . ? C3 Os1 Os3 C7 116.5(6) . . . . ? C2 Os1 Os3 C7 25.9(6) . . . . ? C1 Os1 Os3 C7 -123(3) . . . . ? O14 Os1 Os3 C7 -152.1(5) . . . . ? Os2 Os1 Os3 C7 -65.1(4) . . . . ? C3 Os1 Os3 C8 -155(2) . . . . ? C2 Os1 Os3 C8 114(2) . . . . ? C1 Os1 Os3 C8 -34(4) . . . . ? O14 Os1 Os3 C8 -64(2) . . . . ? Os2 Os1 Os3 C8 23(2) . . . . ? C3 Os1 Os3 C13 -59.0(6) . . . . ? C2 Os1 Os3 C13 -149.5(6) . . . . ? C1 Os1 Os3 C13 62(3) . . . . ? O14 Os1 Os3 C13 32.5(4) . . . . ? Os2 Os1 Os3 C13 119.5(4) . . . . ? C3 Os1 Os3 Os2 -178.5(4) . . . . ? C2 Os1 Os3 Os2 91.0(4) . . . . ? C1 Os1 Os3 Os2 -58(3) . . . . ? O14 Os1 Os3 Os2 -87.0(3) . . . . ? C3 Os1 Os3 Os4 -113.9(4) . . . . ? C2 Os1 Os3 Os4 155.5(4) . . . . ? C1 Os1 Os3 Os4 7(3) . . . . ? O14 Os1 Os3 Os4 -22.4(3) . . . . ? Os2 Os1 Os3 Os4 64.57(2) . . . . ? C9 Os3 Os4 C10 123.8(8) . . . . ? C7 Os3 Os4 C10 -83.0(7) . . . . ? C8 Os3 Os4 C10 12.1(6) . . . . ? C13 Os3 Os4 C10 101.0(6) . . . . ? Os2 Os3 Os4 C10 -93.3(4) . . . . ? Os1 Os3 Os4 C10 -160.5(4) . . . . ? C9 Os3 Os4 C12 -141.2(10) . . . . ? C7 Os3 Os4 C12 12.0(10) . . . . ? C8 Os3 Os4 C12 107.0(9) . . . . ? C13 Os3 Os4 C12 -164.0(9) . . . . ? Os2 Os3 Os4 C12 1.7(8) . . . . ? Os1 Os3 Os4 C12 -65.5(8) . . . . ? C9 Os3 Os4 C11 33.4(8) . . . . ? C7 Os3 Os4 C11 -173.4(7) . . . . ? C8 Os3 Os4 C11 -78.4(7) . . . . ? C13 Os3 Os4 C11 10.6(7) . . . . ? Os2 Os3 Os4 C11 176.3(5) . . . . ? Os1 Os3 Os4 C11 109.1(5) . . . . ? C9 Os3 Os4 O14 -53.2(7) . . . . ? C7 Os3 Os4 O14 100.0(6) . . . . ? C8 Os3 Os4 O14 -164.9(5) . . . . ? C13 Os3 Os4 O14 -76.0(5) . . . . ? Os2 Os3 Os4 O14 89.7(3) . . . . ? Os1 Os3 Os4 O14 22.5(3) . . . . ? C9 Os3 Os4 C13 22.8(8) . . . . ? C7 Os3 Os4 C13 176.0(7) . . . . ? C8 Os3 Os4 C13 -88.9(6) . . . . ? Os2 Os3 Os4 C13 165.7(4) . . . . ? Os1 Os3 Os4 C13 98.6(4) . . . . ? C9 Os3 Os4 Os2 -142.9(7) . . . . ? C7 Os3 Os4 Os2 10.3(5) . . . . ? C8 Os3 Os4 Os2 105.3(4) . . . . ? C13 Os3 Os4 Os2 -165.7(4) . . . . ? Os1 Os3 Os4 Os2 -67.19(2) . . . . ? C4 Os2 Os4 C10 -96.4(6) . . . . ? C6 Os2 Os4 C10 -0.7(6) . . . . ? C5 Os2 Os4 C10 130(3) . . . . ? Os3 Os2 Os4 C10 88.6(4) . . . . ? Os1 Os2 Os4 C10 152.1(4) . . . . ? C4 Os2 Os4 C12 -4.0(7) . . . . ? C6 Os2 Os4 C12 91.7(6) . . . . ? C5 Os2 Os4 C12 -137(3) . . . . ? Os3 Os2 Os4 C12 -179.0(5) . . . . ? Os1 Os2 Os4 C12 -115.5(5) . . . . ? C4 Os2 Os4 C11 59(7) . . . . ? C6 Os2 Os4 C11 155(7) . . . . ? C5 Os2 Os4 C11 -74(8) . . . . ? Os3 Os2 Os4 C11 -116(7) . . . . ? Os1 Os2 Os4 C11 -52(7) . . . . ? C4 Os2 Os4 O14 91.6(5) . . . . ? C6 Os2 Os4 O14 -172.8(5) . . . . ? C5 Os2 Os4 O14 -42(3) . . . . ? Os3 Os2 Os4 O14 -83.4(3) . . . . ? Os1 Os2 Os4 O14 -19.9(3) . . . . ? C4 Os2 Os4 C13 164.9(6) . . . . ? C6 Os2 Os4 C13 -99.4(5) . . . . ? C5 Os2 Os4 C13 31(3) . . . . ? Os3 Os2 Os4 C13 -10.1(3) . . . . ? Os1 Os2 Os4 C13 53.4(3) . . . . ? C4 Os2 Os4 Os3 175.0(5) . . . . ? C6 Os2 Os4 Os3 -89.3(4) . . . . ? C5 Os2 Os4 Os3 42(3) . . . . ? Os1 Os2 Os4 Os3 63.50(2) . . . . ? C3 Os1 C1 O1 -6(19) . . . . ? C2 Os1 C1 O1 85(19) . . . . ? O14 Os1 C1 O1 -98(19) . . . . ? Os3 Os1 C1 O1 -127(17) . . . . ? Os2 Os1 C1 O1 179(100) . . . . ? C3 Os1 C2 O2 -177(100) . . . . ? C1 Os1 C2 O2 91(35) . . . . ? O14 Os1 C2 O2 -62(38) . . . . ? Os3 Os1 C2 O2 -86(35) . . . . ? Os2 Os1 C2 O2 -27(35) . . . . ? C2 Os1 C3 O3 -32(42) . . . . ? C1 Os1 C3 O3 61(42) . . . . ? O14 Os1 C3 O3 152(42) . . . . ? Os3 Os1 C3 O3 -126(42) . . . . ? Os2 Os1 C3 O3 -128(42) . . . . ? C6 Os2 C4 O4 40(53) . . . . ? C5 Os2 C4 O4 -54(53) . . . . ? Os3 Os2 C4 O4 143(52) . . . . ? Os4 Os2 C4 O4 133(53) . . . . ? Os1 Os2 C4 O4 -153(53) . . . . ? C4 Os2 C5 O5 -43(47) . . . . ? C6 Os2 C5 O5 -139(47) . . . . ? Os3 Os2 C5 O5 129(46) . . . . ? Os4 Os2 C5 O5 91(47) . . . . ? Os1 Os2 C5 O5 69(47) . . . . ? C4 Os2 C6 O6 92(61) . . . . ? C5 Os2 C6 O6 -178(100) . . . . ? Os3 Os2 C6 O6 -65(61) . . . . ? Os4 Os2 C6 O6 -5(61) . . . . ? Os1 Os2 C6 O6 -64(61) . . . . ? C9 Os3 C7 O7 -30(5) . . . . ? C8 Os3 C7 O7 70(5) . . . . ? C13 Os3 C7 O7 -54(10) . . . . ? Os2 Os3 C7 O7 178(5) . . . . ? Os4 Os3 C7 O7 168(5) . . . . ? Os1 Os3 C7 O7 -122(5) . . . . ? C9 Os3 C8 O8 15(22) . . . . ? C7 Os3 C8 O8 -76(21) . . . . ? C13 Os3 C8 O8 100(21) . . . . ? Os2 Os3 C8 O8 -143(21) . . . . ? Os4 Os3 C8 O8 156(21) . . . . ? Os1 Os3 C8 O8 -165(20) . . . . ? C7 Os3 C9 O9 -154(17) . . . . ? C8 Os3 C9 O9 116(17) . . . . ? C13 Os3 C9 O9 24(17) . . . . ? Os2 Os3 C9 O9 -104(17) . . . . ? Os4 Os3 C9 O9 5(17) . . . . ? Os1 Os3 C9 O9 -64(17) . . . . ? C12 Os4 C10 O10 126(83) . . . . ? C11 Os4 C10 O10 31(83) . . . . ? O14 Os4 C10 O10 -69(84) . . . . ? C13 Os4 C10 O10 -48(83) . . . . ? Os3 Os4 C10 O10 -91(83) . . . . ? Os2 Os4 C10 O10 -151(83) . . . . ? C10 Os4 C11 O11 28(18) . . . . ? C12 Os4 C11 O11 -65(18) . . . . ? O14 Os4 C11 O11 -160(18) . . . . ? C13 Os4 C11 O11 126(18) . . . . ? Os3 Os4 C11 O11 118(18) . . . . ? Os2 Os4 C11 O11 -128(15) . . . . ? C10 Os4 C12 O12 -91(24) . . . . ? C11 Os4 C12 O12 -1(24) . . . . ? O14 Os4 C12 O12 91(24) . . . . ? C13 Os4 C12 O12 56(25) . . . . ? Os3 Os4 C12 O12 175(24) . . . . ? Os2 Os4 C12 O12 176(100) . . . . ? C9 Os3 C13 O13 5(3) . . . . ? C7 Os3 C13 O13 29(8) . . . . ? C8 Os3 C13 O13 -94(3) . . . . ? Os2 Os3 C13 O13 156(2) . . . . ? Os4 Os3 C13 O13 170(3) . . . . ? Os1 Os3 C13 O13 97(3) . . . . ? C9 Os3 C13 Os4 -164.8(5) . . . . ? C7 Os3 C13 Os4 -141(7) . . . . ? C8 Os3 C13 Os4 96.1(5) . . . . ? Os2 Os3 C13 Os4 -13.7(4) . . . . ? Os1 Os3 C13 Os4 -72.6(2) . . . . ? C10 Os4 C13 O13 103.3(13) . . . . ? C12 Os4 C13 O13 -44(3) . . . . ? C11 Os4 C13 O13 14.7(13) . . . . ? O14 Os4 C13 O13 -79.7(13) . . . . ? Os3 Os4 C13 O13 -174.4(15) . . . . ? Os2 Os4 C13 O13 -161.9(12) . . . . ? C10 Os4 C13 Os3 -82.3(5) . . . . ? C12 Os4 C13 Os3 131(2) . . . . ? C11 Os4 C13 Os3 -170.9(6) . . . . ? O14 Os4 C13 Os3 94.7(4) . . . . ? Os2 Os4 C13 Os3 12.5(4) . . . . ? C10 Os4 O14 Os1 -53(4) . . . . ? C12 Os4 O14 Os1 111.8(6) . . . . ? C11 Os4 O14 Os1 -153.4(6) . . . . ? C13 Os4 O14 Os1 -75.6(5) . . . . ? Os3 Os4 O14 Os1 -31.3(3) . . . . ? Os2 Os4 O14 Os1 28.4(3) . . . . ? C3 Os1 O14 Os4 122.0(6) . . . . ? C2 Os1 O14 Os4 7(6) . . . . ? C1 Os1 O14 Os4 -145.2(6) . . . . ? Os3 Os1 O14 Os4 31.3(3) . . . . ? Os2 Os1 O14 Os4 -27.6(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 O14 H14 O4 0.856(18) 2.156(18) 2.993(14) 166(9) 3_675 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.098 _refine_diff_density_min -2.947 _refine_diff_density_rms 0.466 # Attachment '1.H20.cif' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # If this CIF has been generated directly or indirectly from an entry in the # Cambridge Structural Database, then it will include bibliographic, chemical, # crystal, experimental, refinement or atomic coordinate data resulting from # the CCDC's data processing and validation procedures. Files generated from # CSD entries are Copyright 2005 Cambridge Crystallographic Data Centre. They # may be used in bona fide research applications only, and may not be copied or # further disseminated in any form, whether machine-readable or not, except for # the purposes of generating routine backup copies on your local computer # system. # # Files arising from any other source may also contain material that is the # copyright of third parties, including the originator, and you should check # with the originator concerning the permitted uses of the information # contained in this CIF. # # For further information on the CCDC and the free tools enCIFer and Mercury # for validating and visualising CIF files, please visit www.ccdc.cam.ac.uk # ####################################################################### data_CRYSTALS_cif _database_code_depnum_ccdc_archive 'CCDC 667076' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z 3 1/2+x,1/2+y,z 4 1/2-x,1/2-y,-z 5 -x,y,1/2-z 6 x,-y,1/2+z 7 1/2-x,1/2+y,1/2-z 8 1/2+x,1/2-y,1/2+z _cell_length_a 29.882(2) _cell_length_b 9.4147(7) _cell_length_c 15.2741(12) _cell_angle_alpha 90 _cell_angle_beta 105.2270(10) _cell_angle_gamma 90 _cell_volume 4146.21 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Os1 Os 0.0687 -0.3140 1.0475 Os2 Os 0.1668 -0.2516 1.0527 Os3 Os 0.1387 -0.2923 1.2131 Os4 Os 0.1322 -0.0168 1.1324 C1 C 0.0264 -0.3103 0.9259 O1 O 0.0025 -0.3184 0.8557 C2 C 0.0754 -0.5101 1.0401 O2 O 0.0792 -0.6316 1.0342 C3 C 0.0234 -0.3358 1.1143 O3 O -0.0037 -0.3506 1.1532 C4 C 0.1696 -0.1404 0.9514 O4 O 0.1727 -0.0749 0.8902 C5 C 0.1834 -0.4243 1.0015 O5 O 0.1940 -0.5265 0.9720 C6 C 0.2291 -0.2069 1.1154 O6 O 0.2665 -0.1782 1.1500 C7 C 0.1660 -0.4609 1.1723 O7 O 0.1775 -0.5761 1.1635 C8 C 0.1937 -0.2487 1.3088 O8 O 0.2261 -0.2255 1.3663 C9 C 0.1107 -0.4139 1.2833 O9 O 0.0935 -0.4856 1.3248 C10 C 0.1924 0.0302 1.2018 O10 O 0.2285 0.0582 1.2442 C11 C 0.1067 0.1360 1.1896 O11 O 0.0956 0.2261 1.2277 C12 C 0.1400 0.0987 1.0358 O12 O 0.1445 0.1755 0.9802 C13 C 0.1004 -0.1418 1.2451 O13 O 0.0739(2) -0.0917(7) 1.2788(4) O14 O 0.0651(2) -0.0900(6) 1.0602(3) H1 H 0.1101 -0.2870 0.9860 O15 O 0.0164(2) 0.0146(7) 0.9013(4) O24 O -0.0651(2) 0.0900(6) 0.9398(3) O25 O -0.0164(2) -0.0146(7) 1.0987(4) O23 O 0.0739(2) 0.0917(7) 0.7788(4) O45 O 0.0164(2) -0.0146(7) 1.4013(4)