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_7130827
_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_sum            'C30 H45 N2 O2 P'
_chemical_formula_weight         496.65
_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-2016/6
_audit_update_record
;
2021-07-19 deposited with the CCDC.	2022-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                86.840(3)
_cell_angle_beta                 84.371(3)
_cell_angle_gamma                88.463(3)
_cell_formula_units_Z            4
_cell_length_a                   13.9369(7)
_cell_length_b                   14.1054(8)
_cell_length_c                   14.7011(8)
_cell_measurement_reflns_used    34792
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      25.242
_cell_measurement_theta_min      1.924
_cell_volume                     2871.0(3)
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_collection       'Apex2, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 1.75
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '0.5 deg. \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0927
_diffrn_reflns_av_unetI/netI     0.1663
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34792
_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         26.724
_diffrn_reflns_theta_min         1.924
_diffrn_source                   'ImuS micro focus'
_exptl_absorpt_coefficient_mu    0.124
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.032
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.0042(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         12121
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.1692
_refine_ls_R_factor_gt           0.0680
_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^)+(0.0686P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1375
_refine_ls_wR_factor_ref         0.1754
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5818
_reflns_number_total             12121
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04359a2.cif
_cod_data_source_block           rom30
_cod_database_code               7130827
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.983
_shelx_estimated_absorpt_t_max   0.996
_shelx_res_checksum              6664
_shelx_hkl_checksum              30662