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_7130824
_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 H47 Cl N3 O2 P'
_chemical_formula_sum            'C33 H47 Cl N3 O2 P'
_chemical_formula_weight         584.15
_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_date             2021-02-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-07-19 deposited with the CCDC.	2022-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.4690(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.5759(5)
_cell_length_b                   11.0110(4)
_cell_length_c                   36.5877(12)
_cell_measurement_reflns_used    55159
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      27.505
_cell_measurement_theta_min      2.183
_cell_volume                     7080.5(4)
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_collection       'Apex2, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector_area_resol_mean 1.75
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '1 deg. \f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0758
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            55159
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.505
_diffrn_reflns_theta_min         2.183
_exptl_absorpt_coefficient_mu    0.183
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_description       plate
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.183
_exptl_crystal_size_min          0.156
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         8144
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+8.9314P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1264
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6217
_reflns_number_total             8144
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04359a2.cif
_cod_data_source_block           rom148
_cod_database_code               7130824
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.952
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C32A) = Uanis(C32B)
Uanis(C33A) = Uanis(C33B) = Uanis(C32A) = Uanis(C32B)
Uanis(Cl1B) = Uanis(Cl1A)
Uanis(C34B) = Uanis(C34A)
Uanis(N3A) = Uanis(N3B)
Uanis(C32B) = Uanis(C32A) = Uanis(C33A) = Uanis(C33B) = Uanis(C34A) =
Uanis(C34B)
Uanis(Cl1A) = Uanis(Cl1B)
3. Others
 Sof(Cl1B)=Sof(C32B)=Sof(H32B)=Sof(C33A)=Sof(H33c)=Sof(H33d)=Sof(C34B)=
 Sof(N3B)=1-FVAR(1)
 Sof(C32A)=Sof(H32A)=Sof(N3A)=Sof(C34A)=Sof(Cl1A)=Sof(C33B)=Sof(H33a)=
 Sof(H33b)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C32A(H32A), C32B(H32B)
4.b Secondary CH2 refined with riding coordinates:
 C17(H17a,H17b), C16(H16a,H16b), C33B(H33a,H33b), C33A(H33c,H33d)
4.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C7(H7), C19(H19), C13(H13)
4.d Idealised Me refined as rotating group:
 C24(H24a,H24b,H24c), C30(H30a,H30b,H30c), C29(H29a,H29b,H29c), C23(H23a,H23b,
 H23c), C5(H5a,H5b,H5c), C28(H28a,H28b,H28c), C11(H11a,H11b,H11c), C4(H4a,H4b,
 H4c), C12(H12a,H12b,H12c), C10(H10a,H10b,H10c), C22(H22a,H22b,H22c), C6(H6a,
 H6b,H6c)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              19197
_shelx_hkl_checksum              95736
_shelx_fab_checksum              72903
_olex2_submission_special_instructions 'No special instructions were received'