Isolable cyclic (alkyl)(amino)carbene-phosphonyl radical adducts.
Livshits-Kritsman, Yulia; Tumanskii, Boris; Ménard, Gabriel; Dobrovetsky, Roman; Chemical communications (Cambridge, England) 56 (2020) 1341–1344; doi:10.1039/c9cc09244g

data_7125674
_publ_section_title
;
 Isolable cyclic (alkyl)(amino)carbene-phosphonyl radical adducts.
;
_journal_issue                   9
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1341
_journal_page_last               1344
_journal_paper_doi               10.1039/c9cc09244g
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C24 B F20, C32 H41 N O P '
_chemical_formula_sum            'C56 H41 B F20 N O P'
_chemical_formula_weight         1165.68
_space_group_crystal_system      orthorhombic
_space_group_IT_number           32
_space_group_name_Hall           'P 2 -2ab'
_space_group_name_H-M_alt        'P b a 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2019-11-21 deposited with the CCDC.	2019-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.439(4)
_cell_length_b                   35.468(4)
_cell_length_c                   7.9392(8)
_cell_measurement_reflns_used    43433
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      25.213
_cell_measurement_theta_min      1.816
_cell_volume                     9979.2(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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0775
_diffrn_reflns_av_unetI/netI     0.0736
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            43433
_diffrn_reflns_point_group_measured_fraction_full 0.706
_diffrn_reflns_point_group_measured_fraction_max 0.706
_diffrn_reflns_theta_full        25.213
_diffrn_reflns_theta_max         25.213
_diffrn_reflns_theta_min         1.816
_diffrn_source                   'ImuS micro-focus'
_exptl_absorpt_coefficient_mu    0.174
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       prism
_exptl_crystal_F_000             4736
_exptl_crystal_size_max          0.437
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.134
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 2149 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1458
_refine_ls_number_reflns         12732
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0387P)^2^+0.2452P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.0982
_reflns_Friedel_coverage         0.328
_reflns_Friedel_fraction_full    0.379
_reflns_Friedel_fraction_max     0.379
_reflns_number_gt                10231
_reflns_number_total             12732
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09244g2.cif
_cod_data_source_block           rom49
_cod_depositor_comments
'Adding full bibliography for 7125674--7125677.cif.'
_cod_database_code               7125674
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.928
_shelx_estimated_absorpt_t_max   0.977
_shelx_res_checksum              56035