Cationic 5-phosphonio-substituted N-heterocyclic carbenes.
Schwedtmann, Kai; Schoemaker, Robin; Hennersdorf, Felix; Bauzá, Antonio; Frontera, Antonio; Weiss, Robert; Weigand, Jan J.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 11384–11396; doi:10.1039/c6dt01871h

data_7039680
_publ_section_title
;
 Cationic 5-phosphonio-substituted N-heterocyclic carbenes.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11384
_journal_page_last               11396
_journal_paper_doi               10.1039/c6dt01871h
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C41 H49 Au Cl2 N2 P, C F3 O3 S, C2 H3 N'
_chemical_formula_sum            'C44 H52 Au Cl2 F3 N3 O3 P S'
_chemical_formula_weight         1058.78
_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_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-06-02 deposited with the CCDC.
2016-06-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.332(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7069(2)
_cell_length_b                   21.3249(4)
_cell_length_c                   19.5715(5)
_cell_measurement_reflns_used    11197
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.7480
_cell_measurement_theta_min      3.0950
_cell_volume                     4365.53(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5700
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  1  \w    -72.00 -28.00   0.50    0.50    --  -38.50 125.00-180.00   88
  2  \w   -101.00 -12.00   0.50    0.50    --  -38.50 -57.00  30.00  178
  3  \w   -108.00 -25.00   0.50    0.50    --  -38.50 -38.00 120.00  166
  4  \w     27.00  54.00   0.50    0.50    --   42.75-125.00-180.00   54
  5  \w     32.00 105.00   0.50    1.00    --  111.00 -95.00-120.00  146
  6  \w     85.00 110.00   0.50    1.00    --  111.00-125.00-120.00   50
  7  \w     67.00  94.00   0.50    1.00    --  111.00 -95.00   0.00   54
  8  \w     51.00 133.00   0.50    1.00    --  111.00 -61.00 -90.00  164
  9  \w     87.00 162.00   0.50    1.00    --  111.00  30.00  60.00  150
 10  \w    131.00 156.00   0.50    1.00    --  111.00 -15.00 120.00   50
 11  \w    108.00 177.00   0.50    1.00    --  111.00  30.00 150.00  138
 12  \w     97.00 147.00   0.50    1.00    --  111.00 125.00  30.00  100
 13  \w     37.00 117.00   0.50    1.00    --  111.00 -30.00  60.00  160
 14  \w     45.00  74.00   0.50    1.00    --  111.00 -95.00  60.00   58
 15  \w     38.00 108.00   0.50    1.00    --  111.00 -95.00 -60.00  140
 16  \w     30.00  79.00   0.50    1.00    --  111.00 -95.00 -90.00   98
 17  \w     37.00  73.00   0.50    1.00    --  111.00 -15.00 120.00   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1339498000
_diffrn_orient_matrix_UB_12      -0.0127388000
_diffrn_orient_matrix_UB_13      -0.0452788000
_diffrn_orient_matrix_UB_21      -0.0507261000
_diffrn_orient_matrix_UB_22      -0.0133406000
_diffrn_orient_matrix_UB_23      0.0664918000
_diffrn_orient_matrix_UB_31      -0.0340613000
_diffrn_orient_matrix_UB_32      0.0698895000
_diffrn_orient_matrix_UB_33      0.0044778000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25208
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.762
_diffrn_reflns_theta_min         3.104
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.718
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.968
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_description       block
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.234
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.121
_refine_diff_density_max         2.016
_refine_diff_density_min         -1.303
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         9104
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+7.6561P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0775
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8508
_reflns_number_total             9104
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01871h2.cif
_cod_data_source_block           36OTf
_cod_depositor_comments
'Adding full bibliography for 7039669--7039682.cif.'
_cod_original_cell_volume        4365.52(16)
_cod_database_code               7039680
_chemical_oxdiff_formula         'C172 H208 Au4 Cl8 F12 N16 O12 P4 S4 '
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C11(H11), C14(H14), C26(H26), C23(H23)
2.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B)
2.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C37(H37), C31(H31), C35(H35), C7(H7), C34(H34), C41(H41), C9(H9),
 C21(H21), C33(H33), C19(H19), C39(H39), C40(H40), C20(H20), C38(H38), C32(H32)
2.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C12(H12A,H12B,H12C), C16(H16A,H16B,H16C), C15(H15A,H15B,
 H15C), C28(H28A,H28B,H28C), C24(H24A,H24B,H24C), C13(H13A,H13B,H13C), C27(H27A,
 H27B,H27C), C44(H44A,H44B,H44C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              5654
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.325
_oxdiff_exptl_absorpt_empirical_full_min 0.772