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_7128888
_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 H37 N2 O P'
_chemical_formula_sum            'C31 H37 N2 O P'
_chemical_formula_weight         484.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-24 deposited with the CCDC.	2021-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.457(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.0570(6)
_cell_length_b                   14.0475(13)
_cell_length_c                   12.2644(9)
_cell_measurement_reflns_used    5593
_cell_measurement_temperature    298.16(10)
_cell_measurement_theta_max      27.1700
_cell_measurement_theta_min      2.8910
_cell_volume                     1381.80(19)
_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  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298.16(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -43.00 -18.00   0.50   17.00    --    7.20 -43.00  24.00   50
  2  \w    -28.00  -1.00   0.50   17.00    --    7.20  43.00 176.00   54
  3  \w     -6.00  19.00   0.50   17.00    --   -7.60  43.00 176.00   50
  4  \w    -82.00 -11.00   0.50   17.00    --    7.20 -57.00 150.00  142
  5  \w     50.00  92.00   0.50   17.00    --    7.20  77.00   0.00   84
  6  \w     11.00  37.00   0.50   17.00    --    7.20 -57.00 150.00   52
  7  \w    -74.00  32.00   0.50   17.00    --   -7.60 -77.00-180.00  212
  8  \w    -30.00  33.00   0.50   17.00    --   -7.60 -82.00   0.00  126
  9  \w    -63.00 -38.00   0.50   17.00    --   -7.60 -82.00   0.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0184985000
_diffrn_orient_matrix_UB_12      0.0049700000
_diffrn_orient_matrix_UB_13      -0.0574421000
_diffrn_orient_matrix_UB_21      -0.0739723000
_diffrn_orient_matrix_UB_22      -0.0269395000
_diffrn_orient_matrix_UB_23      0.0027114000
_diffrn_orient_matrix_UB_31      -0.0447578000
_diffrn_orient_matrix_UB_32      0.0424017000
_diffrn_orient_matrix_UB_33      0.0084236000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1035
_diffrn_reflns_av_unetI/netI     0.0980
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.882
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15907
_diffrn_reflns_point_group_measured_fraction_full 0.907
_diffrn_reflns_point_group_measured_fraction_max 0.759
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.958
_diffrn_reflns_theta_min         2.900
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.125
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39367
_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            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_description       plate
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.201
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 1371 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5547
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0681
_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^)+(0.1084P)^2^+0.0463P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1850
_refine_ls_wR_factor_ref         0.1970
_reflns_Friedel_coverage         0.656
_reflns_Friedel_fraction_full    0.807
_reflns_Friedel_fraction_max     0.626
_reflns_number_gt                4143
_reflns_number_total             5547
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04421d2.cif
_cod_data_source_block           aj1010
_cod_depositor_comments
'Adding full bibliography for 7128887--7128892.cif.'
_cod_database_code               7128888
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H N O '
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.959
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C10(H10), C16(H16), C25(H25), C11(H11), C27(H27), C18(H18)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C20(H20A,H20B,H20C), C4(H4A,H4B,H4C), C22(H22A,H22B,H22C),
 C7(H7A,H7B,H7C), C29(H29A,H29B,H29C), C6(H6A,H6B,H6C), C30(H30A,H30B,H30C),
 C31(H31A,H31B,H31C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              21546
_shelx_hkl_checksum              57793
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.118
_oxdiff_exptl_absorpt_empirical_full_min 0.305