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_7035588
_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 H72 Hg N4 P2'
_chemical_formula_sum            'C54 H68 Hg N4 P2'
_chemical_formula_weight         1035.65
_chemical_name_systematic
bis((1,3-bis(2,6-diisopropylphenyl)-1,3-dihydro-2H-imidazol-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
_audit_creation_date             2015-03-25
_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                103.202(2)
_cell_angle_beta                 112.596(2)
_cell_angle_gamma                95.847(2)
_cell_formula_units_Z            1
_cell_length_a                   10.4911(8)
_cell_length_b                   11.1172(8)
_cell_length_c                   12.5446(9)
_cell_measurement_reflns_used    9672
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.96
_cell_measurement_theta_min      2.84
_cell_volume                     1285.49(17)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.1
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            49394
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.130
_diffrn_reflns_theta_min         2.241
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.093
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       plate
_exptl_crystal_F_000             530
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.287
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         6911
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0215
_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^)+(0.0292P)^2^+0.3845P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0495
_refine_ls_wR_factor_ref         0.0495
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6902
_reflns_number_total             6911
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01741f2.cif
_cod_data_source_block           Hg(DippNHC=P)2
_cod_depositor_comments
'Adding full bibliography for 7035586--7035589.cif.'
_cod_original_cell_volume        1285.49(16)
_cod_database_code               7035588
_shelx_estimated_absorpt_t_max   0.913
_shelx_estimated_absorpt_t_min   0.457
_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:
 C22(H22), C13(H13), C10(H10), C25(H25)
2.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C2(H2), C3(H3), C18(H18), C8(H8), C6(H6), C7(H7), C19(H19)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C23(H23A,H23B,H23C), C12(H12A,H12B,H12C), C24(H24A,H24B,
 H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C11(H11A,H11B,H11C), C15(H15A,
 H15B,H15C)
;
_shelx_res_checksum              25831
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'