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_4112152
_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            'C30 H67 Ag B11 P'
_chemical_formula_weight         685.59
_chemical_name_common            'Compound 3'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 113.0110(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1270(2)
_cell_length_b                   15.5380(3)
_cell_length_c                   17.9050(2)
_cell_measurement_temperature    150(2)
_cell_volume                     3873.58(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0472
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            42682
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.581
_exptl_absorpt_correction_T_max  0.9442
_exptl_absorpt_correction_T_min  0.8008
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.607
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         11139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0391P)^2^+2.0128P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0966
_reflns_number_gt                8769
_reflns_number_total             11139
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja038173msi20030828_055726.cif
_cod_data_source_block           k03asw11
_cod_database_code               4112152