Hydrido-sulfido-bridged triangular Os~3~ cluster compounds with different phosphine ligand substitution patterns
Flörke, Ulrich; Egold, Hans; Schraa, Markus; Acta Crystallographica Section C 56 (2000) 760–762; doi:10.1107/S0108270100004571

data_2011128
_publ_section_title
;
 Hydrido-sulfido-bridged triangular Os~3~ cluster compounds with
 different phosphine ligand substitution patterns
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              760
_journal_page_last               762
_journal_paper_doi               10.1107/S0108270100004571
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac          '[Os3 (C O)9 H (C10 H7 S) (C12 H23 P)]'
_chemical_formula_moiety         'C31 H31 O9 Os3 P S'
_chemical_formula_sum            'C31 H31 O9 Os3 P S'
_chemical_formula_weight         1181.19
_chemical_name_systematic
;
nonacarbonyl-1\k^3^C,2\k^2^C,3\k^4^C-dicyclohexylphosphine-2\kP-\m-hydrido-
1:2\k^2^H-\m-(2-naphthylthio)-1:2\k^2^S-triangulo-triosmium
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                69.160(10)
_cell_angle_beta                 80.580(10)
_cell_angle_gamma                76.620(10)
_cell_formula_units_Z            2
_cell_length_a                   10.214(2)
_cell_length_b                   12.997(2)
_cell_length_c                   14.4090(10)
_cell_measurement_reflns_used    29
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      34.89
_cell_measurement_theta_min      14.60
_cell_volume                     1732.2(5)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1994)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    SHELXTL/NT
_computing_publication_material  SHELXTL/NT
_computing_structure_refinement  SHELXTL/NT
_computing_structure_solution    'SHELXTL/NT (Siemens, 1995)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full .980
_diffrn_measured_fraction_theta_max .980
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .019
_diffrn_reflns_av_sigmaI/netI    .045
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9107
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.95
_diffrn_standards_decay_%        4
_diffrn_standards_interval_count 397
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    11.132
_exptl_absorpt_correction_T_max  .235
_exptl_absorpt_correction_T_min  .126
_exptl_absorpt_correction_type   \y-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.265
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          .50
_exptl_crystal_size_mid          .15
_exptl_crystal_size_min          .13
_refine_diff_density_max         .990
_refine_diff_density_min         -.908
_refine_ls_extinction_coef       .00020(14)
_refine_ls_extinction_method     'SHELXTL/NT (Siemens, 1995)'
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         7794
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          .057
_refine_ls_R_factor_gt           .040
_refine_ls_shift/su_max          .003
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0618P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .104
_reflns_number_gt                6138
_reflns_number_total             7794
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gs1077.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1732.2(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2011128
_cod_database_fobs_code          2011128