Stable exo-nido-Metallacarboranes (M = OsIV) that Incorporatemeta-Carborane-Based Dicarbollide Ligands
Elena V. Balagurova; Dmitri N. Cheredilin; Galina D. Kolomnikova; Oleg L. Tok; Fedor M. Dolgushin; Alexander I. Yanovsky; Igor T. Chizhevsky; Journal of the American Chemical Society 129 (2007) 3745–3753; doi:10.1021/ja067838s

data_4109213
_publ_section_title
;
 Stable exo-nido-Metallacarboranes (M = OsIV) that
 Incorporatemeta-Carborane-Based Dicarbollide Ligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3745
_journal_page_last               3753
_journal_paper_doi               10.1021/ja067838s
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C38 H42 B9 Cl Os P2'
_chemical_formula_sum            'C38 H42 B9 Cl Os P2'
_chemical_formula_weight         883.60
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.62(3)
_cell_angle_beta                 106.15(3)
_cell_angle_gamma                91.10(3)
_cell_formula_units_Z            2
_cell_length_a                   11.216(4)
_cell_length_b                   12.711(6)
_cell_length_c                   14.318(5)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      24
_cell_measurement_theta_min      12
_cell_volume                     1949.0(14)
_computing_cell_refinement       'Siemens P3/PC'
_computing_data_collection       'Siemens P3/PC'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Syntex P2(1)'
_diffrn_measurement_method       '\q/2\q scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0581
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6780
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        3
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.450
_exptl_absorpt_correction_T_max  1.303
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
'DIFABS, N.Walker and D.Stuart, Acta Cryst. (1983), A39, 158-166'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_description       prism
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.010
_refine_diff_density_min         -1.313
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         6780
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+2.6297P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0908
_reflns_number_gt                5526
_reflns_number_total             6780
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja067838ssi20061101_072848.cif
_cod_data_source_block           osmcb
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geom and difmap' was changed
to 'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        1948.8(13)
_cod_database_code               4109213