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_7042356
_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 Se'
_chemical_formula_sum            'C6 H25 B20 P Se'
_chemical_formula_weight         423.39
_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
_audit_creation_date             2016-05-09
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-01-12 deposited with the CCDC.
2017-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                111.478(9)
_cell_angle_beta                 92.125(9)
_cell_angle_gamma                104.679(6)
_cell_formula_units_Z            2
_cell_length_a                   7.1663(7)
_cell_length_b                   11.0308(15)
_cell_length_c                   14.573(2)
_cell_measurement_reflns_used    6562
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.98
_cell_measurement_theta_min      2.94
_cell_volume                     1026.2(2)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5691
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.136
_diffrn_reflns_theta_min         2.936
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.898
_exptl_absorpt_correction_T_max  0.745975
_exptl_absorpt_correction_T_min  0.504496
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2008/4 (Bruker,2010) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0914 before and 0.0514 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1235 before and 0.0695 after correction.
 The Ratio of minimum to maximum transmission is 0.66.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 40190 reflections, Rint = 0.0763
 (18654 with I > 3sig(I), Rint = 0.0572)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         5691
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0420P)^2^+0.2446P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0939
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4426
_reflns_number_total             5691
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00485k2.cif
_cod_data_source_block           5450
_cod_depositor_comments
'Adding full bibliography for 7042355--7042360.cif.'
_cod_database_code               7042356
_shelx_estimated_absorpt_t_max   0.726
_shelx_estimated_absorpt_t_min   0.450
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.688(2) 0.312(2)
2. 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
3.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B)
3.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C)
;
_shelx_res_checksum              42017
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'