Synthesis and reactivity of NHC-coordinated phosphinidene oxide.
Dhara, Debabrata; Pal, Pradeep Kumar; Dolai, Ramapada; Chrysochos, Nicolas; Rawat, Hemant; Elvers, Benedict J.; Krummenacher, Ivo; Braunschweig, Holger; Schulzke, Carola; Chandrasekhar, Vadapalli; Priyakumar, U. Deva; Jana, Anukul; Chemical communications (Cambridge, England) 57 (2021) 9546–9549; doi:10.1039/d1cc04421d

data_7128891
_publ_section_title
;
 Synthesis and reactivity of NHC-coordinated phosphinidene oxide.
;
_journal_issue                   75
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9546
_journal_page_last               9549
_journal_paper_doi               10.1039/d1cc04421d
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C31 H38 N2 P, F6 Sb'
_chemical_formula_sum            'C31 H38 F6 N2 P Sb'
_chemical_formula_weight         705.35
_space_group_crystal_system      orthorhombic
_space_group_IT_number           34
_space_group_name_Hall           'P 2 -2n'
_space_group_name_H-M_alt        'P n n 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmp
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-08-04 deposited with the CCDC.	2021-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   38.1631(19)
_cell_length_b                   9.9045(6)
_cell_length_c                   8.5781(5)
_cell_measurement_reflns_used    7838
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.0490
_cell_measurement_theta_min      2.8430
_cell_volume                     3242.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT-2018 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1157
_diffrn_reflns_av_unetI/netI     0.0863
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            24941
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.833
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.909
_diffrn_reflns_theta_min         2.864
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.957
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92167
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       block
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Flack x determined using 1632 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         7122
_refine_ls_number_restraints     922
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0940
_refine_ls_R_factor_gt           0.0624
_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^)+(0.0923P)^2^+0.1900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1564
_refine_ls_wR_factor_ref         0.1737
_reflns_Friedel_coverage         0.740
_reflns_Friedel_fraction_full    0.959
_reflns_Friedel_fraction_max     0.757
_reflns_number_gt                4681
_reflns_number_total             7122
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04421d2.cif
_cod_data_source_block           AJ1026
_cod_depositor_comments
'Adding full bibliography for 7128887--7128892.cif.'
_cod_database_code               7128891
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.796
_shelx_estimated_absorpt_t_max   0.862
_shelx_res_checksum              29700
_shelx_hkl_checksum              20942