All-carbon phosphoranes <i>via</i> difluorocarbene trapping.
Smirnov, Vladimir O.; Volodin, Alexander D.; Korlyukov, Alexander A.; Dilman, Alexander D.; Chemical communications (Cambridge, England) 57 (2021) 4823–4826; doi:10.1039/d1cc01075a

data_7128145
_publ_section_title
;
 All-carbon phosphoranes <i>via</i> difluorocarbene trapping.
;
_journal_issue                   39
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4823
_journal_page_last               4826
_journal_paper_doi               10.1039/d1cc01075a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C20 H15 F2 O2 P'
_chemical_formula_sum            'C20 H15 F2 O2 P'
_chemical_formula_weight         356.29
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-05
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-02-08 deposited with the CCDC.	2021-04-07 downloaded from the CCDC.
;
_cell_angle_alpha                89.257(2)
_cell_angle_beta                 74.417(2)
_cell_angle_gamma                75.991(2)
_cell_formula_units_Z            4
_cell_length_a                   10.1354(6)
_cell_length_b                   12.5827(8)
_cell_length_c                   14.7085(9)
_cell_measurement_reflns_used    9629
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      30.514
_cell_measurement_theta_min      3.025
_cell_volume                     1750.37(19)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_unetI/netI     0.0625
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28652
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.607
_diffrn_reflns_theta_min         2.144
_diffrn_source                   'sealed tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.187
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6357
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1376 before and 0.0475 after correction.
The Ratio of minimum to maximum transmission is 0.8520.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.643
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         10683
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0800P)^2^+0.1970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1483
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7989
_reflns_number_total             10683
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01075a2.cif
_cod_data_source_block           sv1033
_cod_depositor_comments
'Adding full bibliography for 7128144--7128146.cif.'
_cod_database_code               7128145
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.919
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C1A(H1A), C1(H1)
2.b Aromatic/amide H refined with riding coordinates:
 C10A(H10A), C10(H10), C4(H4), C16A(H16A), C7A(H7A), C17A(H17A), C7(H7),
 C16(H16), C6A(H6A), C20A(H20A), C4A(H4A), C12A(H12A), C14A(H14A), C20(H20),
 C13A(H13A), C11A(H11A), C6(H6), C12(H12), C5(H5), C17(H17), C11(H11), C14(H14),
  C13(H13), C5A(H5A), C18A(H18A), C19A(H19A), C18(H18), C19(H19)
;
_shelx_res_checksum              25780
_olex2_submission_special_instructions 'No special instructions were received'