Silver-Phosphine Complexes of the Highly Methylated Carborane Monoanion [closo-1-H-CB11Me11]-
Adam J. Clarke; Michael J. Ingleson; Gabriele Kociok-Köhn; Mary F. Mahon; Nathan J. Patmore; Jonathan P. Rourke; Giuseppe D. Ruggiero; Andrew S. Weller; Journal of the American Chemical Society 126 (2004) 1503–1517; doi:10.1021/ja038173m

data_4112154
_publ_section_title
;
 Silver-Phosphine Complexes of the Highly Methylated Carborane Monoanion
 [closo-1-H-CB11Me11]-
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1503
_journal_page_last               1517
_journal_paper_doi               10.1021/ja038173m
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C38 H69 Ag B11 O2 P'
_chemical_formula_weight         815.68
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 102.378(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.0080(5)
_cell_length_b                   12.2830(4)
_cell_length_c                   37.4810(11)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     8997.1(5)
_computing_data_reduction
'Denzo and Scalepack (otwinowski & Minor, 1997'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.691
_diffrn_measured_fraction_theta_max 0.691
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       KappaCCD
_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  0.1117
_diffrn_reflns_av_sigmaI/netI    0.1596
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            24296
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         3.51
_exptl_absorpt_coefficient_mu    0.515
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_description       Needle
_exptl_crystal_F_000             3440
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.140
_refine_ls_extinction_coef       0.00107(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     986
_refine_ls_number_reflns         9740
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1718
_refine_ls_R_factor_gt           0.0754
_refine_ls_shift/su_max          0.090
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0837P)^2^+4.5843P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1464
_refine_ls_wR_factor_ref         0.1927
_reflns_number_gt                5116
_reflns_number_total             9740
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja038173msi20031125_071226.cif
_cod_data_source_block           c:\backup\kappa\k03asw22\k03asw22
_cod_database_code               4112154