On the edge of the steric repulsion and reactivity of bulky anilines; a case study of chloro(imino)phosphine synthesis
Vrána, Jan; Němec, Vlastimil; Samsonov, Maksim Andreevich; Růžička, Aleš; Dalton Transactions  (2021) –; doi:10.1039/D1DT02445K

data_7708196
_publ_section_title
;
 On the edge of the steric repulsion and reactivity of bulky anilines; a
 case study of chloro(imino)phosphine synthesis
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02445K
_journal_year                    2021
_chemical_formula_sum            'C39 H45 N Si2'
_chemical_formula_weight         583.94
_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
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2021-06-02 deposited with the CCDC.	2021-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                78.955(2)
_cell_angle_beta                 84.572(2)
_cell_angle_gamma                69.270(2)
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_cell_length_a                   9.3294(5)
_cell_length_b                   10.4494(6)
_cell_length_c                   18.6129(10)
_cell_measurement_reflns_used    18789
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     1664.89(16)
_computing_cell_refinement       'APEX3 v2016.9-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service vV6.2.3'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'XT, VERSION 2014/5'
_diffrn_ambient_temperature      150(2)
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_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0871
_diffrn_reflns_av_unetI/netI     0.0870
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18789
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.492
_diffrn_reflns_theta_min         2.420
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.159
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.3518
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_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
;
_exptl_crystal_colour            colourless
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_exptl_crystal_description       needle
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_exptl_crystal_size_max          0.563
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.102
_refine_diff_density_max         1.013
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       0.0105(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         6207
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.1455
_refine_ls_R_factor_gt           0.1341
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0437P)^2^+28.5468P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3657
_refine_ls_wR_factor_ref         0.3715
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5223
_reflns_number_total             6207
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02445k2.cif
_cod_data_source_block           jvr170926Si1a
_cod_database_code               7708196
_exptl_absorpt_special_details
;
The ratio of minimum to maximum
apparent transmission was 0.896
;
_shelxl_version_number           2013-4
_shelx_res_checksum              30559