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_2012330
_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          '[(B9 H13 Os) (C18 H15 P)2 (C O)]'
_chemical_formula_moiety         'C37 H43 B9 O Os P2'
_chemical_formula_sum            'C37 H43 B9 O Os P2'
_chemical_formula_weight         853.14
_chemical_name_systematic
;
[6-carbonyl-6,6-bis(triphenylphosphine)-nido-6-osmadecaborane(13)]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELXL97
_cell_angle_alpha                90
_cell_angle_beta                 91.080(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.46170(10)
_cell_length_b                   15.68210(10)
_cell_length_c                   22.6315(3)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     3712.30(7)
_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      223(2)
_diffrn_measured_fraction_theta_full .991
_diffrn_measured_fraction_theta_max .991
_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  .01
_diffrn_reflns_av_sigmaI/netI    .051
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            74813
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        <2
_diffrn_standards_interval_count 0
_diffrn_standards_number         'area detector data, no'
_exptl_absorpt_coefficient_mu    3.552
_exptl_absorpt_correction_T_max  .871
_exptl_absorpt_correction_T_min  .436
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Blessing, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          .28
_exptl_crystal_size_mid          .20
_exptl_crystal_size_min          .04
_refine_diff_density_max         1.26
_refine_diff_density_min         -1.16
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         6483
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          .084
_refine_ls_R_factor_gt           .057
_refine_ls_shift/su_max          .002
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0197P)^2^+26.7668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .116
_reflns_number_gt                5001
_reflns_number_total             6483
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            iz1015.cif
_cod_data_source_block           IV
_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        3712.29(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2012330
_cod_database_fobs_code          2012330