Redox interactions of Au(iii) with carboxylated dithiafulvenes and tetrathiafulvalene analogues in polar organic media.
Adows, Hadeel; Zhao, Yuming; Chemical communications (Cambridge, England) 52 (2016) 13101–13104; doi:10.1039/c6cc07769b

data_7125238
_publ_section_title
;
 Redox interactions of Au(iii) with carboxylated dithiafulvenes and
 tetrathiafulvalene analogues in polar organic media.
;
_journal_issue                   89
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              13101
_journal_page_last               13104
_journal_paper_doi               10.1039/c6cc07769b
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C32 H30 O8 S8'
_chemical_formula_sum            'C32 H30 O8 S8'
_chemical_formula_weight         799.04
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-20
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-09-11 deposited with the CCDC.
2016-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.315(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3602(9)
_cell_length_b                   9.8696(5)
_cell_length_c                   20.8727(10)
_cell_measurement_reflns_used    6160
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.3830
_cell_measurement_theta_min      2.3640
_cell_volume                     3554.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41o (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41o (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41o (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_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -70.00 110.00   0.50   15.00    --   20.00  54.00   0.00  360
  2  \w    -70.00 110.00   0.50   15.00    --   20.00  54.00  90.00  360
  3  \w    -70.00 110.00   0.50   15.00    --   20.00  54.00 180.00  360
  4  \w    -70.00 110.00   0.50   15.00    --   20.00  54.00 270.00  360
;
_diffrn_measurement_device       'Rigaku Saturn 70'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0018740000
_diffrn_orient_matrix_UB_12      0.0701346000
_diffrn_orient_matrix_UB_13      0.0070307000
_diffrn_orient_matrix_UB_21      -0.0376085000
_diffrn_orient_matrix_UB_22      -0.0090462000
_diffrn_orient_matrix_UB_23      0.0095981000
_diffrn_orient_matrix_UB_31      0.0165022000
_diffrn_orient_matrix_UB_32      -0.0127383000
_diffrn_orient_matrix_UB_33      0.0320554000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22845
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         2.361
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.552
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94431
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41o (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_F_000             1656
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3365
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0565
_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^)+(0.0749P)^2^+5.8465P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1364
_refine_ls_wR_factor_ref         0.1501
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2541
_reflns_number_total             3365
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc07769b2.cif
_cod_data_source_block           mun1039
_cod_database_code               7125238
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C32 H30 S8 O8'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C10(H10)
2.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12C,H12A,H12B), C14(H14B,H14C,H14A), C16(H16C,H16A,
 H16B)
;
_shelx_res_checksum              51262
_shelx_hkl_checksum              83995
_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
- Detector area scaling
;