Triphosphiranes as Phosphinidene-Transfer Agents – Synthesis of Regular and Chelating NHC Phosphinidene Adducts
Siewert, Jan-Erik; Schumann, André; Wellnitz, Tim; Dankert, Fabian; Hering-Junghans, Christian; Dalton Transactions  (2023) –; doi:10.1039/D3DT02690F

data_7714099
_publ_section_title
;
 Triphosphiranes as Phosphinidene-Transfer Agents -- Synthesis of Regular
 and Chelating NHC Phosphinidene Adducts
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02690F
_journal_year                    2023
_chemical_formula_moiety         'C36 H44 N4 P2'
_chemical_formula_sum            'C36 H44 N4 P2'
_chemical_formula_weight         594.69
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2023-09-21 deposited with the CCDC.	2023-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.864(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.3256(7)
_cell_length_b                   27.6449(13)
_cell_length_c                   15.9718(7)
_cell_measurement_reflns_used    9715
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      66.62
_cell_measurement_theta_min      3.20
_cell_volume                     6763.3(5)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEP-3v2020.1 (Farrugia, 2020)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         microfocus
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0734
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            69488
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        66.907
_diffrn_reflns_theta_max         66.907
_diffrn_reflns_theta_min         3.197
_exptl_absorpt_coefficient_mu    1.386
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_correction_T_min  0.819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_description       needle
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     777
_refine_ls_number_reflns         11850
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0645
_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^)+(0.0750P)^2^+9.4561P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1778
_refine_ls_wR_factor_ref         0.1882
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9471
_reflns_number_total             11850
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02690f2.cif
_cod_data_source_block           ax2217_cmpd5a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7714099
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.819
_shelx_estimated_absorpt_t_max   0.934
_shelx_res_checksum              46433