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_7125237
_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         'C16 H16 O4 S4'
_chemical_formula_sum            'C16 H16 O4 S4'
_chemical_formula_weight         400.53
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-15
_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                106.268(5)
_cell_angle_beta                 100.626(6)
_cell_angle_gamma                91.743(5)
_cell_formula_units_Z            2
_cell_length_a                   7.6541(6)
_cell_length_b                   9.3183(4)
_cell_length_c                   12.9177(9)
_cell_measurement_reflns_used    2883
_cell_measurement_temperature    172.9(2)
_cell_measurement_theta_max      61.4210
_cell_measurement_theta_min      3.6340
_cell_volume                     865.98(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      172.9(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6144
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.822
_diffrn_measured_fraction_theta_max 0.958
_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    -23.00  42.00   1.00    1.00    --    0.00  38.00 -30.00   65
  2  \w     46.00  73.00   1.00    1.00    --    0.00  38.00 -30.00   27
  3  \w     87.00 155.00   1.00    1.00    --   82.59  61.00 120.00   68
  4  \w     32.00 160.00   1.00    1.00    --   82.59  15.00  90.00  128
  5  \w     23.00 117.00   1.00    1.00    --   82.59-125.00-120.00   94
  6  \w     14.00 108.00   1.00    1.00    --   82.59 -61.00  60.00   94
  7  \w     13.00 114.00   1.00    1.00    --   82.59 -77.00 -60.00  101
  8  \w     11.00  87.00   1.00    1.00    --   82.59 -61.00-150.00   76
  9  \w    -89.00 -39.00   1.00    1.00    --    0.00-178.00  30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1571137000
_diffrn_orient_matrix_UB_12      -0.0145802000
_diffrn_orient_matrix_UB_13      0.0567623000
_diffrn_orient_matrix_UB_21      -0.1197396000
_diffrn_orient_matrix_UB_22      0.0684031000
_diffrn_orient_matrix_UB_23      -0.0801435000
_diffrn_orient_matrix_UB_31      -0.0568694000
_diffrn_orient_matrix_UB_32      -0.1580985000
_diffrn_orient_matrix_UB_33      -0.0802459000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 0.822
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3842
_diffrn_reflns_point_group_measured_fraction_full 0.822
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         61.536
_diffrn_reflns_theta_min         3.639
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.207
_exptl_absorpt_correction_T_max  0.647
_exptl_absorpt_correction_T_min  0.458
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_description       block
_exptl_crystal_F_000             416
_exptl_crystal_recrystallization_method 'crystalliozed from hexane/DCM/ether'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         2578
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0717P)^2^+0.0258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1042
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2333
_reflns_number_total             2578
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc07769b2.cif
_cod_data_source_block           16tyk-rt01
_cod_database_code               7125237
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C16 H16 O4 S4'
_reflns_odcompleteness_completeness 94.02
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     62.05
_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:
 C1(H1), C22(H22), C24(H24), C26(H26)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C)
;
_olex2_date_sample_data_collection 2016-04-11
_olex2_date_sample_submission    2016-04-06
_olex2_exptl_crystal_mounting_method 'mounted on a loop'
_olex2_submission_original_sample_id 9H
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.333
_oxdiff_exptl_absorpt_empirical_full_min 0.776