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_7708198
_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            'C34 H27 N O'
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_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
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_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                102.708(11)
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_cell_angle_gamma                98.134(11)
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_cell_length_b                   13.410(3)
_cell_length_c                   17.986(4)
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_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
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_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 0.984
_diffrn_measured_fraction_theta_max 0.985
_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  0.1103
_diffrn_reflns_av_unetI/netI     0.0959
_diffrn_reflns_Laue_measured_fraction_full 0.984
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_diffrn_reflns_limit_h_min       -6
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_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
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_diffrn_reflns_point_group_measured_fraction_full 0.984
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         2.190
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.073
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_exptl_absorpt_correction_T_min  0.5594
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_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_description       block
_exptl_crystal_F_000             492
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_exptl_crystal_size_min          0.113
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_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       0.107(14)
_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   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         4859
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1486
_refine_ls_R_factor_gt           0.1089
_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^)+(0.1426P)^2^+2.8596P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2763
_refine_ls_wR_factor_ref         0.2953
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3271
_reflns_number_total             4859
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02445k2.cif
_cod_data_source_block           jvr190812n2a
_cod_original_cell_volume        1253.6(5)
_cod_database_code               7708198
_exptl_absorpt_special_details
;
The ratio of minimum to maximum
apparent transmission was 0.750
;
_shelxl_version_number           2013-4
_shelx_res_checksum              99655
_shelx_fab_checksum              79783