N-Heterocyclic carbene phosphaketene adducts as precursors to carbene-phosphinidene adducts and a rearranged π-system.
Li, Zhongshu; Chen, Xiaodan; Li, Yaqi; Su, Cheng-Yong; Grützmacher, Hansjörg; Chemical communications (Cambridge, England) 52 (2016) 11343–11346; doi:10.1039/c6cc05916c

data_7124963
_publ_section_title
;
 N-Heterocyclic carbene phosphaketene adducts as precursors to
 carbene-phosphinidene adducts and a rearranged \p-system.
;
_journal_issue                   76
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11343
_journal_page_last               11346
_journal_paper_doi               10.1039/c6cc05916c
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C46 H51 N2 O P Si'
_chemical_formula_sum            'C46 H51 N2 O P Si'
_chemical_formula_weight         706.95
_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     direct
_audit_creation_date             2015-02-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-09-18 deposited with the CCDC.
2016-08-09 downloaded from the CCDC.
;
_cell_angle_alpha                85.360(4)
_cell_angle_beta                 78.369(3)
_cell_angle_gamma                76.089(3)
_cell_formula_units_Z            2
_cell_length_a                   9.4352(3)
_cell_length_b                   12.6209(7)
_cell_length_c                   17.8147(8)
_cell_measurement_reflns_used    7024
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      65.3490
_cell_measurement_theta_min      4.3470
_cell_volume                     2015.71(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector_area_resol_mean 10.6525
_diffrn_measured_fraction_theta_full 0.9855
_diffrn_measured_fraction_theta_max 0.9855
_diffrn_measurement_details
;
  1 omega -110.00  -16.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2474  -57.0000   30.0000 94

  2 omega  -66.00   29.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2474   57.0000 -180.0000 95

  3 omega   29.00  103.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932  -95.0000   90.0000 74

  4 omega   72.00  160.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932   45.0000   60.0000 88

  5 omega   23.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932  -95.0000 -180.0000 86

  6 omega    8.00  108.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932  -95.0000  -30.0000 100

  7 omega   65.00  155.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932   30.0000  150.0000 90

  8 omega  109.00  160.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932  125.0000   30.0000 51

  9 omega   21.00   75.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932  -30.0000  -60.0000 54

 10 omega   14.00   82.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932  -30.0000  150.0000 68
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0066548000
_diffrn_orient_matrix_UB_12      -0.0735902000
_diffrn_orient_matrix_UB_13      0.0733661000
_diffrn_orient_matrix_UB_21      -0.0362958000
_diffrn_orient_matrix_UB_22      -0.0880489000
_diffrn_orient_matrix_UB_23      -0.0432381000
_diffrn_orient_matrix_UB_31      0.1672524000
_diffrn_orient_matrix_UB_32      -0.0516152000
_diffrn_orient_matrix_UB_33      -0.0234968000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.902
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10387
_diffrn_reflns_point_group_measured_fraction_full 0.902
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         65.371
_diffrn_reflns_theta_min         3.610
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.158
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         6580
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0510
_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^)+(0.0950P)^2^+0.6200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1406
_refine_ls_wR_factor_ref         0.1445
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6096
_reflns_number_total             6580
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc05916c2.cif
_cod_data_source_block           test1
_cod_database_code               7124963
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C H N P O Si'
_reflns_odcompleteness_completeness 98.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_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 Ternary CH refined with riding coordinates:
 C15(H15), C24(H24), C27(H27), C12(H12)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C7(H7), C9(H9), C20(H20), C8(H8), C41(H41), C19(H19),
 C29(H29), C18(H18), C45(H45), C43(H43), C39(H39), C35(H35), C44(H44), C33(H33),
  C37(H37), C42(H42), C31(H31), C30(H30), C36(H36), C32(H32), C38(H38)
2.c Idealised Me refined as rotating group:
 C25(H25a,H25b,H25c), C14(H14a,H14b,H14c), C16(H16a,H16b,H16c), C11(H11a,H11b,
 H11c), C23(H23a,H23b,H23c), C28(H28a,H28b,H28c), C26(H26a,H26b,H26c), C13(H13a,
 H13b,H13c)
;
_shelx_res_checksum              91468
_olex2_submission_special_instructions 'No special instructions were received'