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_7039678
_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         'C48 H59 Cl2 N2 P Rh, C F3 O3 S, C4 H10 O'
_chemical_formula_sum            'C53 H69 Cl2 F3 N2 O4 P Rh S'
_chemical_formula_weight         1091.94
_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_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                71.9557(17)
_cell_angle_beta                 88.5118(16)
_cell_angle_gamma                78.384(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8203(3)
_cell_length_b                   14.3026(4)
_cell_length_c                   18.3756(2)
_cell_measurement_reflns_used    14661
_cell_measurement_temperature    100.1(2)
_cell_measurement_theta_max      76.3330
_cell_measurement_theta_min      3.3170
_cell_volume                     2646.51(11)
_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      100.1(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5700
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  1  \w    -57.00  17.00   0.50    2.00    --  -38.50  38.00 -90.00  148
  2  \w     85.00 112.00   0.50    2.00    --   42.75  57.00   0.00   54
  3  \w    104.00 147.00   0.50    6.00    --  111.00  30.00  30.00   86
  4  \w    120.00 169.00   0.50    6.00    --  111.00  15.00 -60.00   98
  5  \w    105.00 171.00   0.50    6.00    --  111.00  45.00-150.00  132
  6  \w    103.00 178.00   0.50    6.00    --  111.00  77.00 -60.00  150
  7  \w     95.00 126.00   0.50    6.00    --  111.00 125.00-120.00   62
  8  \w     88.00 123.00   0.50    6.00    --  111.00  45.00   0.00   70
  9  \w     86.00 178.00   0.50    6.00    --  111.00  77.00  60.00  184
 10  \w    113.00 178.00   0.50    6.00    --  111.00  77.00 150.00  130
 11  \w    105.00 134.00   0.50    6.00    --  111.00 -61.00 -30.00   58
 12  \w     87.00 121.00   0.50    6.00    --  111.00-125.00-120.00   68
 13  \w     88.00 115.00   0.50    6.00    --  111.00 -77.00-180.00   54
 14  \w     71.00 118.00   0.50    6.00    --  111.00-125.00-150.00   94
 15  \w     77.00 121.00   0.50    6.00    --  111.00-125.00 -90.00   88
 16  \w     67.00 121.00   0.50    6.00    --  111.00-125.00 -30.00  108
 17  \w     62.00 120.00   0.50    6.00    --  111.00-125.00  60.00  116
 18  \w     75.00 134.00   0.50    6.00    --  111.00 -45.00  30.00  118
 19  \w     70.00 116.00   0.50    6.00    --  111.00  15.00 -60.00   92
 20  \w     52.00  79.00   0.50    6.00    --  111.00 -77.00-180.00   54
 21  \w     40.00  66.00   0.50    6.00    --  111.00-125.00-120.00   52
 22  \w     32.00 103.00   0.50    6.00    --  111.00 -95.00 -30.00  142
 23  \w     54.00  81.00   0.50    6.00    --  111.00 -95.00   0.00   54
 24  \w     36.00  96.00   0.50    6.00    --  111.00 -95.00  60.00  120
 25  \w     42.00 121.00   0.50    6.00    --  111.00-125.00 150.00  158
 26  \w     41.00 130.00   0.50    6.00    --  111.00 -45.00 150.00  178
 27  \w     34.00  73.00   0.50    2.00    --   42.75 -99.00 150.00   78
 28  \w     31.00  81.00   0.50    6.00    --  111.00 -95.00 150.00  100
 29  \w    -62.00  32.00   0.50    2.00    --  -38.50  57.00 120.00  188
 30  \w    -85.00  -3.00   0.50    2.00    --  -38.50 125.00-120.00  164
 31  \w   -108.00 -13.00   0.50    2.00    --  -38.50 -57.00 -30.00  190
;
_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      -0.0717266000
_diffrn_orient_matrix_UB_12      -0.0869513000
_diffrn_orient_matrix_UB_13      0.0217958000
_diffrn_orient_matrix_UB_21      -0.0802047000
_diffrn_orient_matrix_UB_22      0.0480567000
_diffrn_orient_matrix_UB_23      0.0545848000
_diffrn_orient_matrix_UB_31      -0.0978903000
_diffrn_orient_matrix_UB_32      0.0593023000
_diffrn_orient_matrix_UB_33      -0.0658176000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26966
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.617
_diffrn_reflns_theta_min         2.531
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.647
_exptl_absorpt_correction_T_max  0.854
_exptl_absorpt_correction_T_min  0.660
_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    1.370
_exptl_crystal_description       block
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.144
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.038
_refine_diff_density_max         1.827
_refine_diff_density_min         -1.013
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         10839
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0687P)^2^+1.0759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1086
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9934
_reflns_number_total             10839
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01871h2.cif
_cod_data_source_block           23OTf
_cod_depositor_comments
'Adding full bibliography for 7039669--7039682.cif.'
_cod_original_cell_volume        2646.53(10)
_cod_database_code               7039678
_chemical_oxdiff_formula         'C104 H142 Cl4 F6 N8 O6 P2 Rh2 S2 '
_reflns_odcompleteness_completeness 98.99
_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:
 C41(H41), C10(H10), C25(H25), C42(H42), C22(H22), C13(H13), C45(H45), C46(H46)
2.b Secondary CH2 refined with riding coordinates:
 C48(H48A,H48B), C47(H47A,H47B), C43(H43A,H43B), C44(H44A,H44B), C50(H50A,
 H50B), C52(H52A,H52B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C33(H33), C29(H29), C20(H20), C39(H39), C38(H38), C30(H30), C35(H35),
 C31(H31), C19(H19), C8(H8), C7(H7), C18(H18), C32(H32), C37(H37), C36(H36)
2.d Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C27(H27A,H27B,H27C), C23(H23A,H23B,H23C), C12(H12A,H12B,
 H12C), C24(H24A,H24B,H24C), C15(H15A,H15B,H15C), C11(H11A,H11B,H11C), C14(H14A,
 H14B,H14C), C26(H26A,H26B,H26C), C53(H53A,H53B,H53C), C51(H51A,H51B,H51C)
;
_shelx_res_checksum              51698
_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 1.508
_oxdiff_exptl_absorpt_empirical_full_min 0.744