Acylseleno- and acylthioureato complexes of gold(i) N-heterocyclic carbenes
Kuchar, Julia; Rust, Jörg; Lehmann, Christian W.; Mohr, Fabian; New Journal of Chemistry 43 (2019) 10750–; doi:10.1039/C9NJ02229E

data_7058484
_publ_section_title
;
 Acylseleno- and acylthioureato complexes of gold(i) N-heterocyclic
 carbenes
;
_journal_issue                   27
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10750
_journal_paper_doi               10.1039/C9NJ02229E
_journal_volume                  43
_journal_year                    2019
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C39 H50 Au N5 O3 S'
_chemical_formula_sum            'C39 H50 Au N5 O3 S'
_chemical_formula_weight         865.86
_chemical_properties_physical    none
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                JK533
_audit_creation_date             2018-06-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-03 deposited with the CCDC.    2019-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.145(18)
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   33.860(7)
_cell_length_b                   36.211(7)
_cell_length_c                   19.899(3)
_cell_measurement_reflns_used    182951
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.4998
_cell_measurement_theta_min      2.6485
_cell_volume                     23314(8)
_computing_cell_refinement       'REVALCCD V. 1.6, 2008'
_computing_data_collection       'DATCOL (Bruker AXS, 2006)'
_computing_data_reduction        'REVALCCD V. 1.6, 2008'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 1997-2013)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 18.02
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker AXS Enraf-Nonius KappaCCD'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  'Incoatec Helios focusing multilayer optics'
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1649
_diffrn_reflns_av_unetI/netI     0.1352
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            133811
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.300
_diffrn_reflns_theta_min         2.646
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.882
_exptl_absorpt_correction_T_max  0.91446
_exptl_absorpt_correction_T_min  0.77544
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2012)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       plate
_exptl_crystal_F_000             10512
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent:  see paper'
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.398
_refine_diff_density_min         -2.025
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1350
_refine_ls_number_reflns         28915
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1559
_refine_ls_R_factor_gt           0.0659
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0381P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1048
_refine_ls_wR_factor_ref         0.1315
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14755
_reflns_number_total             28915
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj02229e1.cif
_cod_data_source_block           11636sadabs
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'MONOCLINIC' changed to 'monoclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7058484--7058486.cif.
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7058484
_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. Others
 Fixed Sof: O5B(0.5) O6B(0.5) O8B(0.5) O9B(0.5) O6A(0.5) O5A(0.5) O9A(0.5)
 O8A(0.5)
3.a Ternary CH refined with riding coordinates:
 C10A(H10A), C13A(H13A), C22A(H22A), C25A(H25A), C10B(H10B), C13B(H13B),
 C22B(H22B), C25B(H25B), C10C(H10C), C13C(H13C), C22C(H22C), C25C(H25C)
3.b Secondary CH2 refined with riding coordinates:
 C29A(H29E,H29F), C31A(H31E,H31F), C29B(H29A,H29B), C31B(H31A,H31B), C29C(H29C,
 H29D), C31C(H31C,H31D)
3.c Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C3A(H3A), C6A(H6A), C7A(H7A), C8A(H8A), C18A(H18A), C19A(H19A),
 C20A(H20A), C35A(H35A), C36A(H36A), C38A(H38A), C39A(H39A), C2B(H2B), C3B(H3B),
  C6B(H6B), C7B(H7B), C8B(H8B), C18B(H18B), C19B(H19B), C20B(H20B), C35B(H35B),
 C36B(H36B), C38B(H38B), C39B(H39B), C2C(H2C), C3C(H3C), C6C(H6C), C7C(H7C),
 C8C(H8C), C18C(H18C), C19C(H19C), C20C(H20C), C35C(H35C), C36C(H36C),
 C38C(H38C), C39C(H39C)
3.d Idealised Me refined as rotating group:
 C11A(H11G,H11H,H11I), C12A(H12G,H12H,H12I), C14A(H14G,H14H,H14I), C15A(H15G,
 H15H,H15I), C23A(H23G,H23H,H23I), C24A(H24G,H24H,H24I), C26A(H26G,H26H,H26I),
 C27A(H27G,H27H,H27I), C30A(H30G,H30H,H30I), C32A(H32G,H32H,H32I), C11B(H11A,
 H11B,H11C), C12B(H12A,H12B,H12C), C14B(H14A,H14B,H14C), C15B(H15A,H15B,H15C),
 C23B(H23A,H23B,H23C), C24B(H24A,H24B,H24C), C26B(H26A,H26B,H26C), C27B(H27A,
 H27B,H27C), C30B(H30A,H30B,H30C), C32B(H32A,H32B,H32C), C11C(H11D,H11E,H11F),
 C12C(H12D,H12E,H12F), C14C(H14D,H14E,H14F), C15C(H15D,H15E,H15F), C23C(H23D,
 H23E,H23F), C24C(H24D,H24E,H24F), C26C(H26D,H26E,H26F), C27C(H27D,H27E,H27F),
 C30C(H30D,H30E,H30F), C32C(H32D,H32E,H32F)
;
_shelx_res_checksum              60202
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_shelxl_version_number     2016/6