Degradation and Modification of Metallaboranes: Reactions of the Hexaborane(10) Analogue nido-(PPh3)2(CO)OsB5H9 with Phosphines and the Crystal and Molecular Structure of [2,2,2-(PPh3)2(CO)-nido-2-OsB4H7-3-BH2.PPh2Me]
Paul McQuade; Kevin Hupp; Jonathan Bould; Hong Fang; Nigam P. Rath; Rhodri Ll. Thomas; Lawrence Barton; Inorganic Chemistry 38 (1999) 5415–5424; doi:10.1021/ic990688k

data_4322407
_publ_section_title
;
 Degradation and Modification of Metallaboranes: Reactions of the
 Hexaborane(10) Analogue nido-(PPh3)2(CO)OsB5H9 with Phosphines and the
 Crystal and Molecular Structure of
 [2,2,2-(PPh3)2(CO)-nido-2-OsB4H7-3-BH2.PPh2Me]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5415
_journal_page_last               5424
_journal_paper_doi               10.1021/ic990688k
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C51 H53 B5 Cl3 O Os P3'
_chemical_formula_weight         1125.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.259(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.7986(2)
_cell_length_b                   12.0402(3)
_cell_length_c                   19.9108(5)
_cell_measurement_reflns_used    7528
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      2.0
_cell_volume                     2561.90(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXTL (Sheldrick, 1999)'
_computing_structure_solution    'SHELXTL (Sheldrick, 1999)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.071
_diffrn_reflns_av_sigmaI/netI    0.1269
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23503
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    2.775
_exptl_absorpt_correction_T_max  0.8737
_exptl_absorpt_correction_T_min  0.7688
_exptl_absorpt_correction_type   'empirical, sadabs'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.343
_refine_diff_density_min         -1.816
_refine_diff_density_rms         0.141
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.065(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         9305
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_gt           0.0741
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1676
_refine_ls_wR_factor_ref         0.1855
_reflns_number_gt                6473
_reflns_number_total             9305
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990688k.cif
_cod_data_source_block           b9895
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'no' 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        2561.9(1)
_cod_database_code               4322407