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_7058486
_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 Se'
_chemical_formula_sum            'C39 H50 Au N5 O3 Se'
_chemical_formula_weight         912.76
_chemical_properties_physical    'see paper'
_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     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                JK534
_audit_creation_date             2018-07-03
_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                 91.39(2)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   19.003(7)
_cell_length_b                   21.806(3)
_cell_length_c                   37.911(6)
_cell_measurement_reflns_used    440599
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.0999
_cell_measurement_theta_min      2.6042
_cell_volume                     15705(7)
_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 0.998
_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  0.0908
_diffrn_reflns_av_unetI/netI     0.0736
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            405585
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.974
_diffrn_reflns_theta_min         2.599
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.716
_exptl_absorpt_correction_T_max  0.82692
_exptl_absorpt_correction_T_min  0.53237
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2012)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_description       plate
_exptl_crystal_F_000             7296
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent:  see paper'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         6.693
_refine_diff_density_min         -3.646
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1805
_refine_ls_number_reflns         58942
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1142
_refine_ls_R_factor_gt           0.0614
_refine_ls_shift/su_max          0.003
_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^+103.2848P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1157
_refine_ls_wR_factor_ref         0.1355
_reflns_Friedel_coverage         0.000
_reflns_number_gt                38355
_reflns_number_total             58942
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj02229e1.cif
_cod_data_source_block           11671sadabs
_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      P21/c
_cod_database_code               7058486
_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
 Sof(O6B)=1-FVAR(1)
 Sof(O6A)=FVAR(1)
 Fixed Sof: H25A(0.5) H25(0.5) C26B(0.5) H26A(0.5) H26B(0.5) H26C(0.5)
 C27B(0.5) H27A(0.5) H27B(0.5) H27C(0.5) C26A(0.5) H26D(0.5) H26E(0.5)
 H26F(0.5) C27A(0.5) H27D(0.5) H27E(0.5) H27F(0.5)
3.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25A), C25(H25), C90(H90), C93(H93),
 C102(H102), C105(H105), C50(H50), C53(H53), C62(H62), C65(H65), C130(H130),
 C133(H133), C142(H142), C145(H145)
3.b Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C38(H38A,H38B), C116(H11D,H11E), C118(H11I,H11J), C76(H76A,
 H76B), C78(H78A,H78B), C158(H15D,H15E), C156(H15I,H15J)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20),
 C31(H31), C32(H32), C34(H34), C35(H35), C82(H82), C83(H83), C86(H86), C87(H87),
  C88(H88), C98(H98), C99(H99), C100(H100), C111(H111), C112(H112), C114(H114),
 C115(H115), C42(H42), C43(H43), C46(H46), C47(H47), C48(H48), C58(H58),
 C59(H59), C60(H60), C71(H71), C72(H72), C74(H74), C75(H75), C122(H122),
 C123(H123), C126(H126), C127(H127), C128(H128), C138(H138), C139(H139),
 C140(H140), C151(H151), C152(H152), C154(H154), C155(H155)
3.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26B(H26A,H26B,H26C),
 C27B(H27A,H27B,H27C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C91(H91A,H91B,
 H91C), C92(H92A,H92B,H92C), C95(H95A,H95B,H95C), C94(H94A,H94B,H94C),
 C103(H10A,H10B,H10C), C104(H10D,H10E,H10F), C106(H10G,H10H,H10I), C107(H10J,
 H10K,H10L), C117(H11F,H11G,H11H), C119(H11K,H11L,H11M), C51(H51A,H51B,H51C),
 C52(H52A,H52B,H52C), C55(H55A,H55B,H55C), C54(H54A,H54B,H54C), C63(H63A,H63B,
 H63C), C64(H64A,H64B,H64C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C77(H77A,
 H77B,H77C), C79(H79A,H79B,H79C), C132(H13A,H13B,H13C), C131(H13D,H13E,H13F),
 C135(H13G,H13H,H13I), C134(H13J,H13K,H13L), C143(H14D,H14E,H14F), C144(H14G,
 H14H,H14I), C146(H14J,H14K,H14L), C147(H14M,H14N,H14O), C159(H15F,H15G,H15H),
 C157(H15K,H15L,H15M), C26A(H26D,H26E,H26F), C27A(H27D,H27E,H27F)
;
_shelx_res_checksum              94230
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_shelxl_version_number     2016/6