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_4343163
_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 H26 B9 P'
_chemical_formula_sum            'C20 H26 B9 P'
_chemical_formula_weight         394.67
_chemical_melting_point          ?
_chemical_name_systematic
;
 5-Triphenylphosphonio-7,8-dicarba-nido-undecaborane
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                71.2550(10)
_cell_angle_beta                 87.3180(10)
_cell_angle_gamma                74.6270(10)
_cell_formula_units_Z            2
_cell_length_a                   9.7892(3)
_cell_length_b                   9.9725(2)
_cell_length_c                   12.1570(3)
_cell_measurement_reflns_used    9873
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.16
_cell_measurement_theta_min      3.84
_cell_volume                     1082.68(5)
_computing_cell_refinement       'Bruker SAINT 7.68A'
_computing_data_collection       'Bruker APEX 2010.9.1'
_computing_data_reduction        'Bruker SADABS 2008/1'
_computing_molecular_graphics    'Bruker XP 5.1'
_computing_publication_material  'SHELXCIF-2014/1 (Sheldrick, 2014)'
_computing_structure_refinement  'Bruker SHELXTL 2008/4'
_computing_structure_solution    'Bruker SHELXTL 2008/4'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.5 deg wide \w exposures'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_source         'ImuS micro-focus source with Quazar optics'
_diffrn_radiation_type           Cu-K\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0167
_diffrn_reflns_av_unetI/netI     0.0136
_diffrn_reflns_laue_measured_fraction_full 0.947
_diffrn_reflns_laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14889
_diffrn_reflns_point_group_measured_fraction_full 0.947
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.463
_diffrn_reflns_theta_min         3.843
_exptl_absorpt_coefficient_mu    1.121
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Bruker SADABS 2008/1
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             412
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         3703
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0545P)^2^+0.5028P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.0964
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3634
_reflns_number_total             3703
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00414_si_002.cif
_cod_data_source_block           '[C2B9H11]PPh3_mfh245'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 
;
_cod_database_code               4343163
_shelx_estimated_absorpt_t_min   0.824
_shelx_estimated_absorpt_t_max   0.926
_shelxl_version_number           2014-3
_shelx_res_checksum              75568
_shelx_hkl_checksum              62986