Syntheses, Characterizations, and Coordination Chemistry of the 10-Vertex Phosphadicarbaboranes 6-R-arachno-6,8,9-PC2B7H11 and 6-R-arachno-6,5,7-PC2B7H11
Daewon Hong; Scott E. Rathmill; Patrick J. Carroll; Larry G. Sneddon; Journal of the American Chemical Society 125 (2003) 16058–16073; doi:10.1021/ja037799+

data_4114524
_publ_section_title
;
 Syntheses, Characterizations, and Coordination Chemistry of the 10-Vertex
 Phosphadicarbaboranes 6-R-arachno-6,8,9-PC2B7H11 and
 6-R-arachno-6,5,7-PC2B7H11
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16058
_journal_page_last               16073
_journal_paper_doi               10.1021/ja037799+
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C53 H53 B7 P3 Pt'
_chemical_formula_weight         1053.62
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                92.702(2)
_cell_angle_beta                 114.316(1)
_cell_angle_gamma                81.214(2)
_cell_formula_units_Z            2
_cell_length_a                   12.9520(3)
_cell_length_b                   18.3819(4)
_cell_length_c                   11.2556(3)
_cell_measurement_temperature    200(2)
_cell_volume                     2413.01(10)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Altomare, 1993)'
_diffrn_ambient_temperature      200(2)
_diffrn_measurement_device       'image plate area detector'
_diffrn_measurement_device_type  'Rigaku R-AXIS IIc'
_diffrn_measurement_method       'phi oscillations'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            25744
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    3.043
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_F_000             1058
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.956
_refine_diff_density_min         -2.061
_refine_diff_density_rms         0.154
_refine_ls_extinction_coef       0.0290(12)
_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_all   1.113
_refine_ls_goodness_of_fit_obs   1.103
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         10157
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_restrained_S_obs      1.103
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_obs          0.0499
_refine_ls_shift/esd_max         0.245
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0927P)^2^+3.8400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1425
_refine_ls_wR_factor_obs         0.1372
_reflns_number_observed          9610
_reflns_number_total             10157
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja0377992Bsi20030808_011327.cif
_cod_data_source_block           Cmpd_9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0927P)^2^+3.8400P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0927P)^2^+3.8400P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4114524