The investigation of the steric hindrance of anilines by means of reactions with PCl<sub>3</sub> and BCl<sub>3</sub>.
Němec, Vlastimil; Samsonov, Maksim A.; Růžičková, Zdeňka; Vrána, Jan; Růžička, Aleš; Dalton transactions (Cambridge, England : 2003) 54 (2025) 11845–11856; doi:10.1039/d5dt01182e

data_7719054
_publ_section_title
;
 The investigation of the steric hindrance of anilines by means of
 reactions with PCl<sub>3</sub> and BCl<sub>3</sub>.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11845
_journal_page_last               11856
_journal_paper_doi               10.1039/d5dt01182e
_journal_volume                  54
_journal_year                    2025
_chemical_formula_sum            'C34 H30 Cl2 N P'
_chemical_formula_weight         554.46
_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   mixed
_audit_creation_method           SHELXL-2019/1
_audit_update_record
;
2025-07-01 deposited with the CCDC.	2025-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                85.756(2)
_cell_angle_beta                 81.985(2)
_cell_angle_gamma                79.0550(10)
_cell_formula_units_Z            2
_cell_length_a                   9.4836(4)
_cell_length_b                   11.2516(5)
_cell_length_c                   13.4570(7)
_cell_measurement_reflns_used    39853
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     1394.38(11)
_computing_cell_refinement       'APEX4 v2022.10-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service vV6.2.3'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_molecular_graphics    'Platon (Spek, 2009)'
_computing_publication_material  'Platon (Spek, 2009)'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_solution    'XT, VERSION 2014/5'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            39853
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.566
_diffrn_reflns_theta_min         2.339
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.315
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
Reference: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       block
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.489
_exptl_crystal_size_mid          0.478
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         6415
_refine_ls_number_restraints     302
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0419P)^2^+1.0126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.0992
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5274
_reflns_number_total             6415
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01182e3.cif
_cod_data_source_block           mo_jvr210511P1
_cod_depositor_comments
'Adding full bibliography for 7719051--7719060.cif.'
_cod_database_code               7719054
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_min   0.861
_shelx_estimated_absorpt_t_max   0.934
_exptl_absorpt_special_details
;
The ratio of minimum to maximum
apparent transmission was 0.932
;
_shelx_res_checksum              53892
_shelx_hkl_checksum              87755