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_7039677
_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         'C39 H44 Au Cl2 F N2 P, C F3 O3 S, C H2 Cl2'
_chemical_formula_sum            'C41 H46 Au Cl4 F4 N2 O3 P S'
_chemical_formula_weight         1092.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                 92.001(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8603(6)
_cell_length_b                   28.3452(14)
_cell_length_c                   13.1731(6)
_cell_measurement_reflns_used    9905
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.212
_cell_measurement_theta_min      2.352
_cell_volume                     4425.9(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            70316
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.665
_diffrn_reflns_theta_min         2.111
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.705
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0579 before and 0.0469 after correction.
The Ratio of minimum to maximum transmission is 0.8479.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_description       block
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.055
_refine_diff_density_max         1.525
_refine_diff_density_min         -1.763
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         14924
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+4.3286P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0697
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11901
_reflns_number_total             14924
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01871h2.cif
_cod_data_source_block           21OTf
_cod_depositor_comments
'Adding full bibliography for 7039669--7039682.cif.'
_cod_database_code               7039677
_shelx_estimated_absorpt_t_max   0.822
_shelx_estimated_absorpt_t_min   0.563
_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. Restrained distances
 Cl3-C41 = Cl4-C41 = Cl8-C43 = Cl7-C43 = Cl5-C42 = Cl6-C42
 1.77 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl3 \\sim Cl4 \\sim Cl5 \\sim Cl6 \\sim Cl7 \\sim Cl8 \\sim C41 \\sim C43 \\sim
C42: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Others
 1*[Sof(Cl3)+Sof(Cl4)+Sof(C41)+Sof(H41A)+Sof(H41B)]+1*[Sof(Cl5)+Sof(Cl6)+
 Sof(C42)+Sof(H42A)+Sof(H42B)]+1*[Sof(Cl7)+Sof(Cl8)+Sof(C43)+Sof(H43A)+
 Sof(H43B)]=1 with esd of 0.0001
 Sof(Cl3)=Sof(Cl4)=Sof(C41)=Sof(H41A)=Sof(H41B)=FVAR(1)
 Sof(Cl5)=Sof(Cl6)=Sof(C42)=Sof(H42A)=Sof(H42B)=FVAR(2)
 Sof(Cl7)=Sof(Cl8)=Sof(C43)=Sof(H43A)=Sof(H43B)=FVAR(3)
5.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25)
5.b Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C43(H43A,H43B), C42(H42A,H42B)
5.c Aromatic/amide H refined with riding coordinates:
 C36(H36), C7(H7), C39(H39), C6(H6), C33(H33), C29(H29), C8(H8), C35(H35),
 C32(H32), C18(H18), C38(H38), C19(H19), C30(H30), C20(H20), C31(H31), C37(H37)
5.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C)
;
_shelx_res_checksum              12411
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id jjw0319
_olex2_submission_special_instructions 'No special instructions were received'