Extending N-heterocyclic carbene ligands into the third dimension: a new type of hybrid phosphazane/NHC system
Roth, Torsten; Vasilenko, Vladislav; Benson, Callum G. M.; Wadepohl, Hubert; Wright, Dominic S.; Gade, Lutz H.; Chem. Sci. 6 (2015) 2506–; doi:10.1039/C4SC03966A

data_1518731
_publ_section_title
;
 Extending N-heterocyclic carbene ligands into the third dimension: a new
 type of hybrid phosphazane/NHC system
;
_journal_issue                   4
_journal_name_full               'Chem. Sci.'
_journal_page_first              2506
_journal_paper_doi               10.1039/C4SC03966A
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C53 H56 Au2 Cl3 Ir N4 P2'
_chemical_formula_sum            'C55.5 H62 Au2 Cl3 Ir N4 P2'
_chemical_formula_weight         1539.51
_chemical_properties_physical    air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_tro117
_audit_creation_date
;
'Mon Dec 01 10:42:56 2014'
;
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3107 for OlexSys, GUI svn.r4957)
;
_audit_update_record
;
2014-12-19 deposited with the CCDC.
2015-02-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.5872(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.88426(10)
_cell_length_b                   13.46559(9)
_cell_length_c                   30.9781(2)
_cell_measurement_reflns_used    113200
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      32.0200
_cell_measurement_theta_min      3.5740
_cell_volume                     5299.46(7)
_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
'encif (Wadepohl, 2009-14); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_ambient_temperature      120(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
  1 omega  -36.00   68.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316  -80.0000  -65.2109 208

  2 omega   -6.00   19.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316   79.0000  -68.2498 50

  3 omega   -6.00   19.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316   79.0000  -22.6609 50

  4 omega  -43.00   66.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316  -80.0000 -135.7914 218

  5 omega  -41.00   -1.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316  -57.0000   60.0000 80

  6 omega  -43.00    1.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316  -77.0000    0.0000 88

  7 omega   31.00  103.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316   57.0000   60.0000 144

  8 omega    5.00  105.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316   77.0000 -180.0000 200

  9 omega  -27.00   61.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316  -77.0000  120.0000 176

 10 omega    4.00  103.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316   57.0000  -90.0000 198

 11 omega   -6.00   20.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316   79.0000   -0.4661 52

 12 omega    7.00   76.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316   38.0000   30.0000 138

 13 omega  -15.00   66.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316  -77.0000   30.0000 162

 14 omega   -3.00   23.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316   77.0000  120.0000 52

 15 omega    5.00   31.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316   77.0000  150.0000 52

 16 omega  -39.00    9.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316  -80.0000  175.2414 96

 17 omega   36.00   62.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316  -80.0000  175.2414 52

 18 omega   -3.00   71.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316   38.0000 -180.0000 148

 19 omega   -7.00   23.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316   80.0000   50.8130 60

 20 omega   -6.00  107.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316   38.0000  -60.0000 226

 21 omega    4.00  103.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316   57.0000  150.0000 198

 22 omega  -43.00   66.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316  -77.0000   30.0000 218

 23 omega  -42.00   58.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316  -57.0000 -180.0000 200

 24 omega    4.00  103.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316   57.0000   30.0000 198

 25 omega  -43.00   66.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316  -77.0000  150.0000 218

 26 omega    4.00  103.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316   57.0000 -120.0000 198

 27 omega    4.00  103.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316   57.0000   90.0000 198

 28 omega   -6.00   25.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316   79.0000  -22.6609 62

 29 omega  -45.00   67.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316  -38.0000 -120.0000 224

 30 omega  -42.00   58.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316  -57.0000   60.0000 200

 31 omega   -5.00  105.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316   77.0000 -180.0000 220

 32 omega  -44.00   68.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316  -80.0000  175.2414 224

 33 omega  -43.00   66.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316  -77.0000   60.0000 218

 34 omega   -7.00   24.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316   80.0000   50.8130 62

 35 omega  -44.00   41.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7316  -80.0000 -135.7914 170

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_UB_11      -0.0069781000
_diffrn_orient_matrix_UB_12      -0.0016027000
_diffrn_orient_matrix_UB_13      -0.0231897000
_diffrn_orient_matrix_UB_21      -0.0460989000
_diffrn_orient_matrix_UB_22      0.0293294000
_diffrn_orient_matrix_UB_23      -0.0011887000
_diffrn_orient_matrix_UB_31      0.0306943000
_diffrn_orient_matrix_UB_32      0.0437331000
_diffrn_orient_matrix_UB_33      -0.0000510000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            315804
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.168
_diffrn_reflns_theta_min         3.207
_diffrn_source                   'microfocus X-Ray tube'
_exptl_absorpt_coefficient_mu    8.281
_exptl_absorpt_correction_T_max  0.780
_exptl_absorpt_correction_T_min  0.268
_exptl_absorpt_correction_type   gaussian
_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)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.930
_exptl_crystal_description       plate
_exptl_crystal_F_000             2956
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.031
_refine_diff_density_max         2.636
_refine_diff_density_min         -1.643
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.333
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         18285
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.333
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0220P)^2^+25.0536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0843
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16689
_reflns_number_total             18285
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4sc03966a2.cif
_cod_data_source_block           ga_tro117_sq
_cod_depositor_comments
'Adding full bibliography for 1518727--1518731.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C55.50 H62 Au2 Cl3 Ir N4 P2'
_cod_database_code               1518731
_audit_block_refno               2282
_audit_block_usercomment         'tr1506 orange plate'
_chemical_oxdiff_formula         'C55 H56 Au2 Cl3 Ir1 P2 N4'
_chemical_oxdiff_usercomment     'tr1506 orange plate'
_shelx_estimated_absorpt_t_max   0.491
_shelx_estimated_absorpt_t_min   0.491
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_shelxl_version_number           2014/6
_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. Rigid body (RIGU) restrains
 C40, C41, C42, C43, C44, C45
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3.a Ternary CH refined with riding coordinates:
 C20(H20), C33(H33), C46(H46), C47(H47), C50(H50), C51(H51)
3.b Secondary CH2 refined with riding coordinates:
 C48(H48A,H48B), C49(H49A,H49B), C52(H52A,H52B), C53(H53A,H53B)
3.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C13(H13), C15(H15), C22(H22), C23(H23), C24(H24), C25(H25),
 C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36),
  C37(H37), C38(H38), C39(H39), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C17(H17A,H17B,H17C),
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              81126
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            12.88538(9)
_cell_oxdiff_length_b            13.46387(9)
_cell_oxdiff_length_c            30.9760(2)
_cell_oxdiff_angle_alpha         89.9987(6)
_cell_oxdiff_angle_beta          99.5503(6)
_cell_oxdiff_angle_gamma         90.0287(5)
_cell_oxdiff_volume              5299.46(6)
_cell_oxdiff_measurement_reflns_used 113200
_platon_squeeze_void_probe_radius 1.20