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_7706848
_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         'C19 H12 F P'
_chemical_formula_sum            'C19 H12 F P'
_chemical_formula_weight         290.26
_chemical_name_common
(5r,10s)-4-fluoro-10H-5,10-[1,2]benzenoacridophosphine
_chemical_name_systematic
(5r,10s)-4-fluoro-10H-5,10-[1,2]benzenoacridophosphine
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_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                90
_cell_angle_beta                 113.349(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8967(8)
_cell_length_b                   8.1179(3)
_cell_length_c                   13.4003(7)
_cell_measurement_reflns_used    2769
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.0500
_cell_measurement_theta_min      3.8720
_cell_volume                     1387.92(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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 0.970
_diffrn_measured_fraction_theta_max 0.970
_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_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3246
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.246
_diffrn_reflns_theta_max         67.246
_diffrn_reflns_theta_min         6.463
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.756
_exptl_absorpt_correction_T_max  0.613
_exptl_absorpt_correction_T_min  0.495
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_description       block
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.540
_exptl_crystal_size_min          0.410
_refine_diff_density_max         0.173
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.359
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         1216
_refine_ls_number_restraints     209
_refine_ls_restrained_S_all      1.247
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0690
_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^)+4.8682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1533
_refine_ls_wR_factor_ref         0.1536
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1191
_reflns_number_total             1216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00816a2.cif
_cod_data_source_block           nt0805_LHG192_100K
_cod_depositor_comments
'Adding full bibliography for 7706848--7706861.cif.'
_cod_original_cell_volume        1387.93(14)
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               7706848
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.419
_shelx_estimated_absorpt_t_max   0.533
_shelx_res_checksum              87076
_shelx_hkl_checksum              98506