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_7124966
_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         'C45 H51 Ge N2 P'
_chemical_formula_sum            'C45 H51 Ge N2 P'
_chemical_formula_weight         723.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 94.7933(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.06280(20)
_cell_length_b                   12.81520(9)
_cell_length_c                   25.4632(2)
_cell_measurement_reflns_used    22361
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      65.3780
_cell_measurement_theta_min      3.8520
_cell_volume                     7824.62(11)
_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 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
  1 omega  -50.00   31.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2474   38.0000  -90.0000 81

  2 omega  -48.00   30.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2474   38.0000   30.0000 78

  3 omega  -50.00   30.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2474   38.0000  150.0000 80

  4 omega    8.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932  -95.0000  -30.0000 101

  5 omega   19.00   63.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932  -61.0000  -30.0000 44

  6 omega   75.00  116.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932  -61.0000  -30.0000 41

  7 omega   60.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932  -95.0000 -150.0000 49

  8 omega   19.00   47.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932  -95.0000 -150.0000 28

  9 omega   43.00  167.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932   15.0000 -180.0000 124

 10 omega   14.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932  -30.0000 -180.0000 77

 11 omega   69.00  142.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932   45.0000   60.0000 73

 12 omega   22.00   96.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932  -77.0000  120.0000 74
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0316032000
_diffrn_orient_matrix_UB_12      -0.1042334000
_diffrn_orient_matrix_UB_13      -0.0070364000
_diffrn_orient_matrix_UB_21      0.0554438000
_diffrn_orient_matrix_UB_22      -0.0597503000
_diffrn_orient_matrix_UB_23      0.0099265000
_diffrn_orient_matrix_UB_31      -0.0075041000
_diffrn_orient_matrix_UB_32      -0.0023832000
_diffrn_orient_matrix_UB_33      0.0594956000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 0.928
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            42736
_diffrn_reflns_point_group_measured_fraction_full 0.928
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         65.405
_diffrn_reflns_theta_min         3.687
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.686
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.228
_exptl_crystal_description       block
_exptl_crystal_F_000             3056
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     899
_refine_ls_number_reflns         13144
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+3.2880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0770
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11618
_reflns_number_total             13144
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc05916c2.cif
_cod_data_source_block           exp_2172
_cod_original_cell_volume        7824.60(11)
_cod_database_code               7124966
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C H N O P Ge'
_reflns_odcompleteness_completeness 99.68
_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:
 C71(H71), C23(H23), C68(H68), C59(H59), C11(H11), C26(H26), C14(H14), C56(H56)
2.b Aromatic/amide H refined with riding coordinates:
 C48(H48), C3(H3), C47(H47), C45(H45), C18(H18), C2(H2), C51(H51), C84(H84),
 C29(H29), C35(H35), C52(H52), C20(H20), C34(H34), C33(H33), C41(H41), C36(H36),
  C8(H8), C63(H63), C53(H53), C65(H65), C37(H37), C78(H78), C42(H42), C64(H64),
 C19(H19), C80(H80), C6(H6), C38(H38), C30(H30), C7(H7), C31(H31), C90(H90),
 C32(H32), C77(H77), C44(H44), C82(H82), C89(H89), C88(H88), C86(H86), C83(H83),
  C81(H81), C75(H75), C74(H74), C43(H43), C87(H87), C76(H76)
2.c Idealised Me refined as rotating group:
 C22(H22a,H22b,H22c), C10(H10a,H10b,H10c), C12(H12a,H12b,H12c), C24(H24a,H24b,
 H24c), C27(H27a,H27b,H27c), C72(H72a,H72b,H72c), C58(H58a,H58b,H58c), C13(H13a,
 H13b,H13c), C25(H25a,H25b,H25c), C70(H70a,H70b,H70c), C60(H60a,H60b,H60c),
 C55(H55a,H55b,H55c), C15(H15a,H15b,H15c), C67(H67a,H67b,H67c), C57(H57a,H57b,
 H57c), C69(H69a,H69b,H69c)
;
_olex2_date_sample_data_collection 2015-08-08
_olex2_submission_special_instructions 'No special instructions were received'