Large, weakly basic bis(carboranyl)phosphines: an experimental and computational study.
Riley, Laura E.; Krämer, Tobias; McMullin, Claire L.; Ellis, David; Rosair, Georgina M.; Sivaev, Igor B.; Welch, Alan J.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 5218–5228; doi:10.1039/c7dt00485k

data_7042360
_publ_section_title
;
 Large, weakly basic bis(carboranyl)phosphines: an experimental and
 computational study.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5218
_journal_page_last               5228
_journal_paper_doi               10.1039/c7dt00485k
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C6 H25 B20 P'
_chemical_formula_sum            'C6 H25 B20 P'
_chemical_formula_weight         344.43
_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_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-01-09
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2017-01-12 deposited with the CCDC.
2017-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.290(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.441(2)
_cell_length_b                   7.2690(6)
_cell_length_c                   24.083(2)
_cell_measurement_reflns_used    1924
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.023
_cell_measurement_theta_min      2.607
_cell_volume                     3896.3(6)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1415
_diffrn_reflns_av_unetI/netI     0.1046
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            44057
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        23.771
_diffrn_reflns_theta_max         23.771
_diffrn_reflns_theta_min         1.058
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.6011
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0989 before and 0.0760 after correction.
The Ratio of minimum to maximum transmission is 0.8068.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_description       needle
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.071
_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     609
_refine_ls_number_reflns         5928
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1435
_refine_ls_R_factor_gt           0.0795
_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^)+(0.0821P)^2^+9.4025P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1841
_refine_ls_wR_factor_ref         0.2133
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3517
_reflns_number_total             5928
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00485k2.cif
_cod_data_source_block           5428
_cod_depositor_comments
'Adding full bibliography for 7042355--7042360.cif.'
_cod_original_cell_volume        3896.2(6)
_cod_database_code               7042360
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.948
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C11C(H11X,H11Y), C11A(H11P,H11Q)
2.b Idealised Me refined as rotating group:
 C12C(H12X,H12Y,H12Z), C12A(H12P,H12Q,H12R)
;
_shelx_res_checksum              51575
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'