Novel Synthetic Approach to Charge-Compensated Phosphonio-nido-Carboranes. Synthesis and Structural Characterization of Neutral Mono and Bis(Phosphonio) nido-ortho-Carboranes.
Kabytaev, Kuanysh Z.; Safronov, Alexander V.; Sevryugina, Yulia V.; Barnes, Charles L.; Jalisatgi, Satish S.; Hawthorne, M. Frederick; Inorganic chemistry 54 (2015) 4143–4150; doi:10.1021/acs.inorgchem.5b00414

data_4343162
_publ_section_title
;
 Novel Synthetic Approach to Charge-Compensated
 Phosphonio-nido-Carboranes. Synthesis and Structural Characterization of
 Neutral Mono and Bis(Phosphonio) nido-ortho-Carboranes.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4143
_journal_page_last               4150
_journal_paper_doi               10.1021/acs.inorgchem.5b00414
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C20 H25 B9 I P'
_chemical_formula_sum            'C20 H25 B9 I P'
_chemical_formula_weight         520.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 93.3890(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.2403(4)
_cell_length_b                   22.5110(5)
_cell_length_c                   13.1895(3)
_cell_measurement_temperature    100(2)
_cell_volume                     4813.46(19)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_molecular_graphics    'X-SEED, Barbour, 2001'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_laue_measured_fraction_full 0.984
_diffrn_reflns_laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            50559
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.166
_diffrn_reflns_theta_min         2.725
_diffrn_source                   'Incoatec Cu microfocus tube'
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    11.097
_exptl_absorpt_correction_T_max  0.81
_exptl_absorpt_correction_T_min  0.10
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Data were corrected for decay and absorption using the program SADABS 
 (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of
 G\"ottingen, Germany).
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_description       Needle
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.789
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         9134
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+9.5140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.0929
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8858
_reflns_number_total             9134
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00414_si_004.cif
_cod_data_source_block           6-I-9-P
_cod_database_code               4343162
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.072
_shelx_estimated_absorpt_t_max   0.809
_shelx_res_checksum              35433
_shelx_hkl_checksum              85148