#------------------------------------------------------------------------------ #$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/03/2010368.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2010368 loop_ _publ_author_name 'Knoeppel, D.W.' 'Chung, J.-H.' 'Shore, S.G.' _publ_section_title ; (\m-H)(\m-OH)Os~3~(CO)~10~ ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 42 _journal_page_last 45 _journal_volume 51 _journal_year 1995 _chemical_formula_moiety '[Os3 H (OH) (CO)10 ]' _chemical_formula_sum 'C10 H2 O11 Os3' _chemical_formula_weight 868.7 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_type_scat_source ' IntTabIV for non-H atoms' _cell_angle_alpha 90. _cell_angle_beta 107.140(10) _cell_angle_gamma 90. _cell_formula_units_Z 4 _cell_length_a 7.3470(10) _cell_length_b 24.849(6) _cell_length_c 9.0010(10) _cell_measurement_reflns_used 25 _cell_measurement_temperature 213 _cell_measurement_theta_max 15 _cell_measurement_theta_min 12 _cell_volume 1570.3(5) _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w-2\q _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.034 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 5606 _diffrn_reflns_theta_max 25 _diffrn_standards_decay_% -2.2 _diffrn_standards_interval_time 180 _diffrn_standards_number 4 _exptl_absorpt_coefficient_mu 24.3 _exptl_absorpt_correction_T_max 0.998 _exptl_absorpt_correction_T_min 0.633 _exptl_absorpt_correction_type \y-scans _exptl_crystal_colour orange _exptl_crystal_density_diffrn 3.674 _exptl_crystal_description cube _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _refine_diff_density_max 1.726 _refine_diff_density_min -2.461 _refine_ls_goodness_of_fit_obs 0.947 _refine_ls_hydrogen_treatment 'H atoms not located' _refine_ls_number_parameters 218 _refine_ls_number_reflns 2165 _refine_ls_R_factor_obs 0.026 _refine_ls_shift/esd_max 0.02 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme '[\s(I)^2^+0.03(I)^2^]^-1/2^' _refine_ls_wR_factor_obs 0.031 _reflns_number_observed 2165 _reflns_number_total 2714 _reflns_observed_criterion I>=3\s(I) _[local]_cod_data_source_file gr1012.cif _[local]_cod_data_source_block gr1012_structure_1_of_1 _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_original_cell_volume 1570.5 _cod_database_code 2010368 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Os1 .18135(4) .345160(10) .10752(4) Os2 .37618(4) .38640(2) -.09610(4) Os3 .50486(4) .411060(10) .22203(4) O .3730(8) .4605(3) .0257(7) O11 -.0526(9) .4481(3) .0240(10) O12 .1220(10) .3314(4) .4289(8) O13 -.1600(10) .2798(4) -.0820(10) O14 .4700(10) .2517(3) .1446(9) O21 .0001(9) .4024(3) -.3472(8) O22 .4040(10) .2747(3) -.2219(9) O23 .6320(10) .4283(9) -.2823(9) O31 .3090(10) .4620(3) .4417(8) O32 .6690(10) .3259(3) .4611(9) O33 .8719(9) .4773(3) .3306(9) C11 .0360(10) .4110(4) .0600(10) C12 .1380(10) .3362(4) .3070(10) C13 -.0320(10) .3024(4) -.0160(10) C14 .3650(10) .2868(4) .1320(10) C21 .1410(10) .3955(4) -.2560(10) C22 .3930(10) .3165(4) -.1740(10) C23 .5360(10) .4153(4) -.2110(10) C31 .3860(10) .4423(4) .3600(10) C32 .6110(10) .3570(5) .3700(10) C33 .7360(10) .4542(4) .2820(10) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Os1 Os2 2.8295(5) yes Os1 Os3 2.8196(5) yes Os2 Os3 2.8061(5) yes Os2 O 2.146(7) yes Os3 O 2.136(7) yes Os1 C11 1.930(10) yes Os1 C12 1.920(10) yes Os1 C13 1.949(9) yes Os1 C14 1.950(10) yes Os2 C21 1.906(9) yes Os2 C22 1.890(10) yes Os2 C23 1.920(10) yes Os3 C31 1.880(10) yes Os3 C32 1.890(10) yes Os3 C33 1.950(10) yes C11 O11 1.120(10) yes C12 O12 1.150(10) yes C13 O13 1.100(10) yes C14 O14 1.150(10) yes C21 O21 1.130(10) yes C22 O22 1.130(10) yes C23 O23 1.130(10) yes C31 O31 1.160(10) yes C32 O32 1.120(10) yes C33 O33 1.120(10) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag Os2 Os1 Os3 59.570(10) yes Os1 Os2 Os3 60.040(10) yes Os1 Os3 Os2 60.390(10) yes Os1 Os2 O 84.0(2) yes Os1 Os3 O 84.5(2) yes Os3 Os2 O 48.9(2) yes Os2 Os3 O 49.2(2) yes Os2 O Os3 81.9(2) yes O Os2 C21 98.0(4) yes O Os2 C22 171.6(3) yes O Os2 C23 93.2(4) yes O Os3 C31 97.1(4) yes O Os3 C32 169.7(4) yes O Os3 C33 93.3(4) yes Os1 C11 O11 176.0(10) yes Os1 C12 O12 176.0(10) yes Os1 C13 O13 175.0(10) yes Os1 C14 O14 178.8(9) yes Os2 C21 O21 177.0(10) yes Os2 C22 O22 179.0(10) yes Os2 C23 O23 175.0(10) yes Os3 C31 O31 178.2(8) yes Os3 C32 O32 177.0(10) yes Os3 C33 O33 173.1(9) yes Os2 Os1 C11 84.3(3) yes Os2 Os1 C12 154.2(3) yes Os2 Os1 C13 107.5(3) yes Os2 Os1 C14 82.9(3) yes Os3 Os1 C11 86.6(3) yes Os3 Os1 C12 94.6(3) yes Os3 Os1 C13 167.1(3) yes Os3 Os1 C14 84.9(3) yes Os1 Os2 C21 90.7(3) yes Os1 Os2 C22 90.5(3) yes Os1 Os2 C23 172.7(3) yes Os3 Os2 C21 134.5(3) yes Os3 Os2 C22 122.7(3) yes Os3 Os2 C23 113.1(3) yes Os1 Os3 C31 88.6(3) yes Os1 Os3 C32 88.4(3) yes Os1 Os3 C33 173.8(3) yes Os2 Os3 C31 132.9(3) yes Os2 Os3 C32 120.6(3) yes Os2 Os3 C33 113.9(3) yes _journal_paper_doi 10.1107/S0108270194006128