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_7130825
_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         'C31 H45 N2 O3 P, 0.5(C6 H14)'
_chemical_formula_sum            'C34 H52 N2 O3 P'
_chemical_formula_weight         567.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2021-07-19 deposited with the CCDC.	2022-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.6310(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2720(6)
_cell_length_b                   16.6838(5)
_cell_length_c                   10.9853(4)
_cell_measurement_reflns_used    27461
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.330
_cell_measurement_theta_min      1.661
_cell_volume                     3310.90(19)
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_collection       'Apex2, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0308
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            27461
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.330
_diffrn_reflns_theta_min         1.661
_diffrn_source                   'ImuS micro focus'
_exptl_absorpt_coefficient_mu    0.117
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.983
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_description       rhomb
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.257
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.108
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         8249
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+1.5608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1066
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6654
_reflns_number_total             8249
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04359a2.cif
_cod_data_source_block           rom27
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7130825
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.971
_shelx_estimated_absorpt_t_max   0.987
_shelx_res_checksum              69387
_shelx_hkl_checksum              90536