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_4343164
_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         'C38 H38 B9 I P2'
_chemical_formula_sum            'C38 H38 B9 I P2'
_chemical_formula_weight         780.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 95.005(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7556(4)
_cell_length_b                   25.5594(9)
_cell_length_c                   15.4202(6)
_cell_measurement_reflns_used    9848
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.2
_cell_measurement_theta_min      3.4
_cell_volume                     3830.3(3)
_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 0.900
_diffrn_measured_fraction_theta_max 0.954
_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  0.0575
_diffrn_reflns_av_unetI/netI     0.2290
_diffrn_reflns_Laue_measured_fraction_full 0.900
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_number            34627
_diffrn_reflns_point_group_measured_fraction_full 0.900
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.079
_diffrn_reflns_theta_min         3.357
_diffrn_source                   'Incoatec microfocus Cu tube'
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    7.548
_exptl_absorpt_correction_T_max  0.70
_exptl_absorpt_correction_T_min  0.41
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Data were corrected for decay and absorption using the program TWINABS 
 (Sheldrick, G. M. (2003). TWINABS. University of G\"ottingen, Germany).
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.556
_refine_diff_density_min         -1.256
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         6240
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0727
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1467
_refine_ls_wR_factor_ref         0.1496
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4503
_reflns_number_total             6240
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00414_si_006.cif
_cod_data_source_block           Diphos-071813
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4343164
_shelx_estimated_absorpt_t_min   0.178
_shelx_estimated_absorpt_t_max   0.704
_shelxl_version_number           2013-4
_shelx_res_checksum              58468
_shelx_hkl_checksum              4206