The <i>nido</i>‒osmaboranes [2,2,2-(CO)(PPh~3~)~2~-<i>nido</i>-2-OsB~5~H~9~] and [6,6,6-(CO)(PPh~3~)~2~-<i>nido</i>-6-OsB~9~H~13~]
Bould, Jonathan; Kennedy, John D.; Thomas, Rhodri Ll.; Rath, Nigam P.; Barton, Lawrence; Acta Crystallographica Section C 57 (2001) 1245–1247; doi:10.1107/S0108270101012689

data_2012329
_publ_section_title
;
 The <i>nido</i>--osmaboranes
 [2,2,2-(CO)(PPh~3~)~2~-<i>nido</i>-2-OsB~5~H~9~] and
 [6,6,6-(CO)(PPh~3~)~2~-<i>nido</i>-6-OsB~9~H~13~]
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1245
_journal_page_last               1247
_journal_paper_doi               10.1107/S0108270101012689
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          '[(B5 H9 Os) (C18 H15 P)2 (C O)]'
_chemical_formula_moiety         'C37 H39 B5 O Os P2'
_chemical_formula_sum            'C37 H39 B5 O Os P2'
_chemical_formula_weight         805.87
_chemical_name_systematic
;
[2-carbonyl-2,2-bis(triphenylphosphine)-nido-2-osmahexaborane(9)]
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90
_cell_angle_beta                 105.290(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.00540(10)
_cell_length_b                   13.02000(10)
_cell_length_c                   17.24450(10)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      33
_cell_measurement_theta_min      2
_cell_volume                     3466.39(17)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1999)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full .999
_diffrn_measured_fraction_theta_max .999
_diffrn_measurement_device_type  'Bruker SMART Query CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .041
_diffrn_reflns_av_sigmaI/netI    .050
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31883
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        <2
_diffrn_standards_interval_count 0
_diffrn_standards_number         'area detector data, no'
_exptl_absorpt_coefficient_mu    3.801
_exptl_absorpt_correction_T_max  .751
_exptl_absorpt_correction_T_min  .450
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          .25
_exptl_crystal_size_mid          .20
_exptl_crystal_size_min          .08
_refine_diff_density_max         2.20
_refine_diff_density_min         -1.78
_refine_ls_abs_structure_details 'Flack, 1983'
_refine_ls_abs_structure_Flack   .002(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         9961
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          .028
_refine_ls_R_factor_gt           .026
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0182P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .059
_reflns_number_gt                9460
_reflns_number_total             9961
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            iz1015.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

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        3466.39(4)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2012329
_cod_database_fobs_code          2012329