An Entry to Stable Mixed Phosphine-Osmium-NHC Polyhydrides.
Buil, María L; Cardo, Juan J. F.; Esteruelas, Miguel A.; Fernández, Israel; Oñate, Enrique; Inorganic chemistry 55 (2016) 5062–5070; doi:10.1021/acs.inorgchem.6b00658

data_4347822
_publ_section_title
;
 An Entry to Stable Mixed Phosphine-Osmium-NHC Polyhydrides.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5062
_journal_page_last               5070
_journal_paper_doi               10.1021/acs.inorgchem.6b00658
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C45 H58 B N2 Os P'
_chemical_formula_weight         858.91
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 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                 100.2510(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.4514(17)
_cell_length_b                   10.3031(8)
_cell_length_c                   38.022(3)
_cell_measurement_reflns_used    8884
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24
_cell_measurement_theta_min      2
_cell_volume                     8269.3(11)
_computing_cell_refinement       'SAINT+ v. 7.56a (Bruker AXS, 2008)'
_computing_data_collection       'apex2 v. 7.0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+ v. 7.56a (Bruker AXS, 2008)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.14 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.14 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'Bruker APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0610
_diffrn_reflns_av_sigmaI/netI    0.0517
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            48295
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.49
_diffrn_reflns_theta_min         1.09
_exptl_absorpt_coefficient_mu    3.155
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Absorption correction performed with SADABS program. This is based on the
method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33.

SADABS: Area-Detector Absorption Correction. Bruker-AXS 
within SAINT+ package, v. 7.56a (2008).
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             3504
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.421
_refine_diff_density_min         -1.178
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         9839
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0324P)^2^+34.4873P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0878
_reflns_number_gt                7899
_reflns_number_total             9839
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00658_si_002.cif
_cod_data_source_block           enrique113
_cod_original_cell_volume        8269.4(11)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4347822