Sterically hindered ortho-substituted phosphatriptycenes as configurationally stable P-chirogenic triarylphosphines.
Hu, Lei; Mahaut, Damien; Tumanov, Nikolay; Wouters, Johan; Collard, Laurent; Robiette, Raphaël; Berionni, Guillaume; Dalton transactions (Cambridge, England : 2003) 50 (2021) 4772–4777; doi:10.1039/d1dt00816a

data_7706851
_publ_section_title
;
 Sterically hindered ortho-substituted phosphatriptycenes as
 configurationally stable P-chirogenic triarylphosphines.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4772
_journal_page_last               4777
_journal_paper_doi               10.1039/d1dt00816a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C18 H9 Br6 P'
_chemical_formula_sum            'C18 H9 Br6 P'
_chemical_formula_weight         735.68
_chemical_name_common
(2,3-dibromophenyl)bis(2,6-dibromophenyl)phosphane
_chemical_name_systematic
(2,3-dibromophenyl)bis(2,6-dibromophenyl)phosphane
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   dual
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-02-08 deposited with the CCDC.	2021-03-15 downloaded from the CCDC.
;
_cell_angle_alpha                78.126(13)
_cell_angle_beta                 82.433(12)
_cell_angle_gamma                81.201(11)
_cell_formula_units_Z            2
_cell_length_a                   7.4004(9)
_cell_length_b                   8.9219(12)
_cell_length_c                   15.889(3)
_cell_measurement_reflns_used    1068
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      40.7270
_cell_measurement_theta_min      5.3480
_cell_volume                     1009.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.1856
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur, Ruby, Gemini ultra
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2316
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        40.794
_diffrn_reflns_theta_max         40.794
_diffrn_reflns_theta_min         2.857
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    15.123
_exptl_absorpt_correction_T_max  0.736
_exptl_absorpt_correction_T_min  0.153
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.421
_exptl_crystal_description       plate
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.021
_refine_diff_density_max         1.023
_refine_diff_density_min         -1.221
_refine_diff_density_rms         0.229
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         2316
_refine_ls_number_restraints     171
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0735
_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^)+(0.1624P)^2^+3.0830P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2115
_refine_ls_wR_factor_ref         0.2272
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1816
_reflns_number_total             2316
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00816a2.cif
_cod_data_source_block           test23_Lie91_lowres
_cod_depositor_comments
'Adding full bibliography for 7706848--7706861.cif.'
_cod_database_code               7706851
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.059
_shelx_estimated_absorpt_t_max   0.742
_shelx_res_checksum              61962
_shelx_hkl_checksum              68620