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_7058485
_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_formula_moiety         'C40 H53 Au N4 O Se, C2 H6 O'
_chemical_formula_sum            'C42 H59 Au N4 O2 Se'
_chemical_formula_weight         927.85
_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_date             2019-03-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 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                 101.693(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1899(3)
_cell_length_b                   16.2803(4)
_cell_length_c                   18.4131(5)
_cell_measurement_reflns_used    8112
_cell_measurement_temperature    157(11)
_cell_measurement_theta_max      29.0540
_cell_measurement_theta_min      2.8860
_cell_volume                     4165.44(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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      157(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2705
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.851
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -4.00  37.00   1.00   90.00    --   15.59 -99.00  90.00   41
  2  \w    -38.00  28.00   1.00   90.00    --   15.59 -57.00 -60.00   66
  3  \w      7.00  52.00   1.00   90.00    --   15.59 -99.00  60.00   45
  4  \w      9.00  82.00   1.00   90.00    --   15.59  57.00 150.00   73
  5  \w    -27.00  44.00   1.00   90.00    --   15.59   0.00 120.00   71
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0007896000
_diffrn_orient_matrix_UB_12      -0.0366388000
_diffrn_orient_matrix_UB_13      0.0209565000
_diffrn_orient_matrix_UB_21      0.0332638000
_diffrn_orient_matrix_UB_22      -0.0175931000
_diffrn_orient_matrix_UB_23      -0.0195634000
_diffrn_orient_matrix_UB_31      0.0386958000
_diffrn_orient_matrix_UB_32      0.0157609000
_diffrn_orient_matrix_UB_33      0.0269211000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.851
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25188
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.851
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.572
_diffrn_reflns_theta_min         2.379
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.444
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       plate
_exptl_crystal_F_000             1872
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Ethanol, hexanes'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.068
_refine_diff_density_min         -1.384
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         9924
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+7.6414P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0870
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7802
_reflns_number_total             9924
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj02229e1.cif
_cod_data_source_block           jk14_se_lt
_cod_depositor_comments
'Adding full bibliography for 7058484--7058486.cif.'
_cod_original_cell_volume        4165.47(18)
_cod_database_code               7058485
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C39H49N4O1Se1Au1
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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, All O(H) groups
2. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim N1 \\sim N2: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
3.a Ternary CH refined with riding coordinates:
 C18(H18), C25(H25), C6(H6), C13(H13)
3.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C31(H31A,H31B), C41(H41A,H41B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2), C23(H23), C21(H21), C35(H35), C22(H22), C40(H40), C36(H36),
 C11(H11), C9(H9), C10(H10), C39(H39)
3.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C32(H32A,H32B,H32C), C7(H7A,H7B,
 H7C), C8(H8A,H8B,H8C), C27(H27A,H27B,H27C), C30(H30A,H30B,H30C), C26(H26A,H26B,
 H26C), C15(H15A,H15B,H15C), C42(H42A,H42B,H42C), C14(H14A,H14B,H14C), C38(H38A,
 H38B,H38C)
3.e Idealised tetrahedral OH refined as rotating group:
 O2(H2A)
;
_shelx_res_checksum              33107
_olex2_date_sample_data_collection 2018-05-09
_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 1.644
_oxdiff_exptl_absorpt_empirical_full_min 0.708