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_4112151
_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 H49 Ag B11 P'
_chemical_formula_weight         667.44
_chemical_name_common            'compound 2'
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                111.6370(10)
_cell_angle_beta                 95.0050(10)
_cell_angle_gamma                100.3360(10)
_cell_formula_units_Z            2
_cell_length_a                   9.18400(10)
_cell_length_b                   13.6170(2)
_cell_length_c                   15.1520(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     1708.23(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      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            38763
_diffrn_reflns_theta_full        30.06
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         3.57
_exptl_absorpt_coefficient_mu    0.658
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description       Plate
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.126
_refine_ls_extinction_coef       0.0074(11)
_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   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         9965
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.061
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc
 [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/
   [\s^2^(Fo^2^)+0.0000+0.4216*P+(0.0516P)^2^+0.0000sin\q/\l]
 where P = 0.00000Fo^2^ + 1.00000Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1043
_reflns_number_gt                7255
_reflns_number_total             9965
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja038173msi20030828_055709.cif
_cod_data_source_block           c:\backup\helix\h02asw2\h02asw2
_cod_database_code               4112151