Sterically Hindered and Robust Pnictogen Ligands Derived from Carboranes: Synthesis and X-ray Structure Determination of Tris(1'-methyl(1,2-dicarba-closo-dodecaboran-1-yl))phosphine, Tris(1'-methyl(1,2-dicarba-closo-dodecaboran-1-yl))arsine and Chloro(Tris(1'-methyl(1,2-dicarba-closo-dodecaboran-1-yl))phosphine)gold(I)
Arienne S. King; George Ferguson; James F. Britten; John F. Valliant; Inorganic Chemistry 43 (2004) 3507–3513; doi:10.1021/ic049947i

data_4311087
_publ_section_title
;
 Sterically Hindered and Robust Pnictogen Ligands Derived from Carboranes:
 Synthesis and X-ray Structure Determination of
 Tris(1'-methyl(1,2-dicarba-closo-dodecaboran-1-yl))phosphine,
 Tris(1'-methyl(1,2-dicarba-closo-dodecaboran-1-yl))arsine and
 Chloro(Tris(1'-methyl(1,2-dicarba-closo-dodecaboran-1-yl))phosphine)gold(I)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3507
_journal_page_last               3513
_journal_paper_doi               10.1021/ic049947i
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C9 H39 As B30'
_chemical_formula_weight         546.62
_chemical_name_systematic
; 
 tris(1'-methyl(1,2-dicarba-closo-
dodecaboran-1-yl))arsine 
;
_space_group_IT_number           173
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_space_group_name_H-M   'P 63'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   12.330(3)
_cell_length_b                   12.330(3)
_cell_length_c                   11.474(4)
_cell_measurement_reflns_used    9246
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      27.399
_cell_measurement_theta_min      2.605
_cell_volume                     1510.7(7)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      190(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13340
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    1.131
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.749348
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.036
_refine_diff_density_min         -1.062
_refine_diff_density_rms         0.153
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.73(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         2303
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0930
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1187P)^2^+8.8780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2450
_refine_ls_wR_factor_ref         0.2481
_reflns_number_gt                2140
_reflns_number_total             2303
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049947isi20040112_044000_2.cif
_cod_data_source_block           askas
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
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 
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_cod_database_code               4311087