A Cyclic Divalent N(I) Species Isoelectronic to Carbodiphosphoranes
Tian, Jiaxin; Cordier, Marie; Bour, Christophe; Auffrant, Audrey; Gandon, Vincent; Chemical Communications  (2022) –; doi:10.1039/D2CC01637K

data_7129984
_publ_section_title
;
 A Cyclic Divalent N(I) Species Isoelectronic to Carbodiphosphoranes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC01637K
_journal_year                    2022
_chemical_formula_moiety         'C34 H26 N P2, F6 P'
_chemical_formula_sum            'C34 H26 F6 N P3'
_chemical_formula_weight         655.47
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-03-03 deposited with the CCDC.	2022-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                101.997(2)
_cell_angle_beta                 91.033(2)
_cell_angle_gamma                111.831(2)
_cell_formula_units_Z            1
_cell_length_a                   8.2282(7)
_cell_length_b                   9.5081(8)
_cell_length_c                   10.7126(8)
_cell_measurement_reflns_used    7940
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      26.7171
_cell_measurement_theta_min      2.3718
_cell_volume                     756.79(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXT(Sheldrick,2014)
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Kappa APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19925
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         26.984
_diffrn_reflns_theta_min         1.954
_exptl_absorpt_coefficient_mu    0.260
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6382
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       block
_exptl_crystal_F_000             336
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.197
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.02(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         6488
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0420P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0774
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                5891
_reflns_number_total             6488
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc01637k2.cif
_cod_data_source_block           tian36_a
_cod_database_code               7129984
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.955
_shelx_estimated_absorpt_t_max   0.974
_shelx_res_checksum              31586
_shelx_hkl_checksum              84343