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_7035587
_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         'C27 H41 N2 P'
_chemical_formula_sum            'C27 H41 N2 P'
_chemical_formula_weight         424.59
_chemical_name_systematic
1,3-bis(2,6-diisopropylphenyl)-2-phosphanylimidazolidine
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Heat-sensitive, Oxygen-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_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                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.1771(3)
_cell_length_b                   16.0504(3)
_cell_length_c                   26.4131(5)
_cell_measurement_reflns_used    13677
_cell_measurement_temperature    105.7(3)
_cell_measurement_theta_max      31.5100
_cell_measurement_theta_min      2.9680
_cell_volume                     5162.37(19)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      105.7(3)
_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  -97.00  -48.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3865  -77.0000   30.0000 49

  2 omega   53.00   96.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8553  179.0000 -180.0000 43

  3 omega   36.00  103.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8553  179.0000   60.0000 67

  4 omega  -36.00   10.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3865  -90.0000   57.0000 46

  5 omega  -95.00   -5.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3865  -57.0000 -120.0000 90

  6 omega  -95.00  -26.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3865  -57.0000  150.0000 69

  7 omega   34.00  103.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8553  179.0000  -60.0000 69
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0537990000
_diffrn_orient_matrix_UB_12      -0.0015834000
_diffrn_orient_matrix_UB_13      -0.0102996000
_diffrn_orient_matrix_UB_21      -0.0208417000
_diffrn_orient_matrix_UB_22      0.0196946000
_diffrn_orient_matrix_UB_23      0.0220481000
_diffrn_orient_matrix_UB_31      0.0082180000
_diffrn_orient_matrix_UB_32      0.0394941000
_diffrn_orient_matrix_UB_33      -0.0113696000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            38487
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.97
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.122
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91700
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1856
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-hexane'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         5270
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0545
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0545P)^2^+3.1252P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1323
_reflns_number_gt                4669
_reflns_number_total             5270
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt01741f2.cif
_cod_data_source_block           DippNHCstarH-PH2
_cod_depositor_comments
'Adding full bibliography for 7035586--7035589.cif.'
_cod_original_cell_volume        5162.35(19)
_cod_database_code               7035587
_chemical_oxdiff_formula         C27H41N2P
_reflns_odcompleteness_completeness 99.74
_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:
 C22(H22), C1(H1), C10(H10), C25(H25), C13(H13)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C20(H20), C8(H8), C18(H18), C19(H19)
2.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C23(H23A,H23B,H23C), C27(H27A,H27B,H27C), C24(H24A,H24B,
 H24C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C)
;
_olex2_submission_special_instructions 'No special instructions were received'