Carbene insertion into a P-H bond: parent phosphinidene-carbene adducts from PH3 and bis(phosphinidene)mercury complexes.
Bispinghoff, Mark; Tondreau, Aaron M.; Grützmacher, Hansjörg; Faradji, Charly A.; Pringle, Paul G.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 5999–6003; doi:10.1039/c5dt01741f

data_7035589
_publ_section_title
;
 Carbene insertion into a P-H bond: parent phosphinidene-carbene adducts
 from PH3 and bis(phosphinidene)mercury complexes.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5999
_journal_page_last               6003
_journal_paper_doi               10.1039/c5dt01741f
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C54 H76 Hg N4 P2'
_chemical_formula_sum            'C54 H76 Hg N4 P2'
_chemical_formula_weight         1043.71
_chemical_name_systematic
bis((1,3-bis(2,6-diisopropylphenyl)imidazolidin-2-ylidene)phosphanyl)mercury
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-03-24
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-03-25 deposited with the CCDC.
2015-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                103.816(6)
_cell_angle_beta                 110.797(5)
_cell_angle_gamma                96.922(6)
_cell_formula_units_Z            1
_cell_length_a                   10.7696(5)
_cell_length_b                   11.0160(10)
_cell_length_c                   12.2625(6)
_cell_measurement_reflns_used    3543
_cell_measurement_temperature    106.22(15)
_cell_measurement_theta_max      28.7590
_cell_measurement_theta_min      3.0760
_cell_volume                     1286.44(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      106.22(15)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0839
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega    6.00   92.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       27.1678   57.0000   90.0000 86

  2 omega  -11.00   69.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       27.1678  -99.0000 -180.0000 80

  3 omega   19.00   69.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       27.1678  -99.0000  -30.0000 50

  4 omega  -42.00   45.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       27.1678  -57.0000 -150.0000 87

  5 omega   39.00   67.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       27.1678  -99.0000   90.0000 28

  6 omega  -17.00   95.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       27.1678   19.0000   30.0000 112

  7 omega -103.00  -54.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.5428 -179.0000  -60.0000 49
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0257500000
_diffrn_orient_matrix_UB_12      0.0670539000
_diffrn_orient_matrix_UB_13      0.0163706000
_diffrn_orient_matrix_UB_21      0.0608117000
_diffrn_orient_matrix_UB_22      -0.0049282000
_diffrn_orient_matrix_UB_23      0.0450613000
_diffrn_orient_matrix_UB_31      0.0294940000
_diffrn_orient_matrix_UB_32      -0.0106301000
_diffrn_orient_matrix_UB_33      -0.0437969000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_unetI/netI     0.0815
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10844
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.855
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.091
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74571
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pale yellow'
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             538
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         4.591
_refine_diff_density_min         -3.192
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         5259
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0613P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1139
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5170
_reflns_number_total             5259
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01741f2.cif
_cod_data_source_block           Hg(DippNHCstar=P)2
_cod_depositor_comments
'Adding full bibliography for 7035586--7035589.cif.'
_cod_original_cell_volume        1286.44(16)
_cod_database_code               7035589
_chemical_oxdiff_formula         ' C27H38Hg0.5N2P'
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C13(H13), C10(H10), C22(H22), C25(H25)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C7(H7), C18(H18), C19(H19), C20(H20)
2.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C26(H26A,H26B,
 H26C), C23(H23A,H23B,H23C), C11(H11A,H11B,H11C), C27(H27A,H27B,H27C), C12(H12A,
 H12B,H12C)
;
_shelx_res_checksum              38708
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'