Intramolecular C−N Bond Activation by Geometrically Constrained PIII-Centre
Bawari, Deependra; Volodarsky , Solomon; Ginzburg, Yael; Jaiswal, Kuldeep; Joshi, Pooja; Dobrovetsky, Roman; Chemical Communications  (2022) –; doi:10.1039/D2CC04359A

data_7130826
_publ_section_title
;
 Intramolecular C&#x2212;N Bond Activation by Geometrically Constrained
 PIII-Centre
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04359A
_journal_year                    2022
_chemical_formula_moiety         'C33 H46 N3 O2 P'
_chemical_formula_sum            'C33 H46 N3 O2 P'
_chemical_formula_weight         547.70
_chemical_name_common            RomanTA41b
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-07-19 deposited with the CCDC.	2022-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.186(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   36.162(5)
_cell_length_b                   5.9937(8)
_cell_length_c                   29.921(4)
_cell_measurement_reflns_used    5182
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.491
_cell_measurement_theta_min      1.632
_cell_volume                     6383.0(15)
_computing_cell_refinement       'APEX2 v2010.7-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v2010.7.0.0'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 95
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'APEX2 (Bruker AXS)'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0857
_diffrn_reflns_av_unetI/netI     0.1051
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            17211
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        24.491
_diffrn_reflns_theta_max         24.491
_diffrn_reflns_theta_min         1.632
_exptl_absorpt_coefficient_mu    0.118
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_description       needle
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.699
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         5182
_refine_ls_number_restraints     362
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.1482
_refine_ls_R_factor_gt           0.0661
_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^)+(0.1065P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1625
_refine_ls_wR_factor_ref         0.2046
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2722
_reflns_number_total             5182
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04359a2.cif
_cod_data_source_block           RomanTA41b
_cod_original_cell_volume        6383.0(14)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7130826
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.962
_shelx_estimated_absorpt_t_max   0.993
_shelx_res_checksum              38457
_shelx_hkl_checksum              23564