Organometallic chemistry in aqua regia: metal and ligand based oxidations of (NHC)AuCl complexes.
Levchenko, Volodymyr; Glessi, Cristiano; Øien-Ødegaard, Sigurd; Tilset, Mats; Dalton transactions (Cambridge, England : 2003) 49 (2020) 3473–3479; doi:10.1039/c9dt04472h

data_7703543
_publ_section_title
;
 Organometallic chemistry in aqua regia: metal and ligand based oxidations
 of (NHC)AuCl complexes.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3473
_journal_page_last               3479
_journal_paper_doi               10.1039/c9dt04472h
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C25 H21 Au Cl3 N3 O4, C H2 Cl2'
_chemical_formula_sum            'C26 H23 Au Cl5 N3 O4'
_chemical_formula_weight         815.69
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-04-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-23 deposited with the CCDC.	2020-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.209(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.4915(14)
_cell_length_b                   15.0501(11)
_cell_length_c                   21.4077(16)
_cell_measurement_reflns_used    9947
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.495
_cell_measurement_theta_min      2.646
_cell_volume                     5771.7(7)
_computing_cell_refinement       'APEX3 (Bruker, 2018)'
_computing_data_collection       'APEX3 (Bruker, 2018)'
_computing_data_reduction        'APEX3 (Bruker, 2018)'
_computing_molecular_graphics    'Diamond v4 (Brandenburg, 2014)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker Photon100 area detector'
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            84147
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.545
_diffrn_reflns_theta_min         2.263
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.599
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.5383
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.0857 before and 0.0449 after correction. 
The Ratio of minimum to maximum transmission is 0.7214. 
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.877
_exptl_crystal_description       block
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          0.268
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.082
_refine_diff_density_max         3.180
_refine_diff_density_min         -2.370
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         19243
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0368P)^2^+10.3859P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0825
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14959
_reflns_number_total             19243
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04472h2.cif
_cod_data_source_block           lv67-064-ar-reintegrated_pl
_cod_depositor_comments
'Adding full bibliography for 7703541--7703546.cif.'
_cod_database_code               7703543
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.657
_shelx_estimated_absorpt_t_min   0.315
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: Cl8(0.627) Cl9(0.373) H51A(0.627) H51B(0.627) H7(0.373) H51(0.373)
3.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C3(H3A,H3B), C51(H51A,H51B), C52(H52A,H52B)
3.b Aromatic/amide H refined with riding coordinates:
 C30(H30), C46(H46), C27(H27), C38(H38), C47(H47), C34(H34), C35(H35),
 C44(H44), C39(H39), C48(H48), C50(H50), C49(H49), C43(H43), C5(H5), C2(H2),
 C10(H10), C22(H22), C21(H21), C9(H9), C13(H13), C19(H19), C14(H14), C23(H23),
 C25(H25), C18(H18), C24(H24)
3.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C33(H33A,H33B,H33C), C17(H17A,H17B,H17C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              63726
_olex2_submission_special_instructions 'No special instructions were received'