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_7125677
_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         '2(C23 H38 N O3 P), C6 H6'
_chemical_formula_sum            'C52 H82 N2 O6 P2'
_chemical_formula_weight         893.13
_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
;
2019-11-21 deposited with the CCDC.	2019-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.0850(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   15.6255(3)
_cell_length_c                   17.7751(5)
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_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.326
_cell_measurement_theta_min      1.714
_cell_volume                     5079.0(2)
_computing_cell_refinement       'Saint, Bruker-AXS'
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_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 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '0.5 deg. \f and \w scans'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0566
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
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_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            46348
_diffrn_reflns_point_group_measured_fraction_full 0.999
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.326
_diffrn_reflns_theta_min         1.714
_diffrn_source                   'ImuS micro-focus'
_exptl_absorpt_coefficient_mu    0.134
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_description       needle
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.292
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         12634
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0464P)^2^+1.6797P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1133
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8894
_reflns_number_total             12634
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09244g2.cif
_cod_data_source_block           rom62a
_cod_depositor_comments
'Adding full bibliography for 7125674--7125677.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7125677
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.962
_shelx_estimated_absorpt_t_max   0.995
_shelx_res_checksum              46665