[4]Helicene based anions in electrocrystallization with tetrachalcogenafulvalene donors
zigon, nicolas; Avarvari, Narcis; CrystEngComm  (2022) –; doi:10.1039/D2CE00091A

data_7244376
_publ_section_title
;
 [4]Helicene based anions in electrocrystallization with
 tetrachalcogenafulvalene donors
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00091A
_journal_year                    2022
_chemical_formula_moiety         'C48 H34 O4 S4'
_chemical_formula_sum            'C48 H34 O4 S4'
_chemical_formula_weight         802.99
_chemical_name_systematic        TMTTF-([4]heliceneCOO)2
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-07-29
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2022-01-17 deposited with the CCDC.	2022-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   14.0945(2)
_cell_length_b                   12.8981(2)
_cell_length_c                   20.6753(3)
_cell_measurement_reflns_used    12098
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      75.2940
_cell_measurement_theta_min      4.2430
_cell_volume                     3758.61(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_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   -116.00   8.00   1.00    5.00    --  -41.11   0.00-120.00  124
  2  \w    -25.00  43.00   1.00    5.00    --   41.11 -38.00   0.00   68
  3  \w     -2.00  24.00   1.00    5.00    --   41.11 -19.00-180.00   26
  4  \w    107.00 158.00   1.00   12.00    --  112.00  61.00 -30.00   51
  5  \w    118.00 147.00   1.00   12.00    --  112.00  77.00 150.00   29
  6  \w     40.00  69.00   1.00   12.00    --  112.00 -61.00-150.00   29
  7  \w    125.00 153.00   1.00   12.00    --  112.00  77.00   0.00   28
  8  \w    127.00 157.00   1.00   12.00    --  112.00 111.00   0.00   30
  9  \w     40.00  65.00   1.00   12.00    --  112.00 -61.00 -90.00   25
 10  \w     85.00 112.00   1.00   12.00    --  112.00  61.00 -60.00   27
 11  \w    129.00 154.00   1.00   12.00    --  112.00  61.00 -60.00   25
 12  \w     38.00 107.00   1.00   12.00    --  112.00-111.00  60.00   69
 13  \w     30.00  66.00   1.00   12.00    --  112.00 -94.00-150.00   36
 14  \w     88.00 119.00   1.00   12.00    --  112.00  45.00  90.00   31
 15  \w     40.00  77.00   1.00   12.00    --  112.00-111.00-150.00   37
 16  \w    117.00 158.00   1.00   12.00    --  112.00  30.00  30.00   41
 17  \w     41.00 106.00   1.00   12.00    --  112.00-111.00 120.00   65
 18  \w    107.00 158.00   1.00   12.00    --  112.00  30.00 150.00   51
 19  \w     44.00  69.00   1.00   12.00    --  112.00 -61.00-120.00   25
 20  \w     44.00  71.00   1.00   12.00    --  112.00 -61.00  30.00   27
 21  \w     85.00 121.00   1.00   12.00    --  112.00  61.00  90.00   36
 22  \w     87.00 127.00   1.00   12.00    --  112.00 111.00-180.00   40
 23  \w     37.00  65.00   1.00   12.00    --  112.00 -94.00  30.00   28
 24  \w     76.00 101.00   1.00   12.00    --  112.00 -94.00  30.00   25
 25  \w    113.00 140.00   1.00   12.00    --  112.00  45.00  60.00   27
 26  \w     37.00  73.00   1.00   12.00    --  112.00-111.00-180.00   36
 27  \w     88.00 122.00   1.00   12.00    --  112.00  61.00   0.00   34
 28  \w     60.00 120.00   1.00   12.00    --  112.00 178.00-150.00   60
 29  \w     86.00 111.00   1.00   12.00    --  112.00 111.00   0.00   25
 30  \w    129.00 154.00   1.00   12.00    --  112.00  45.00  90.00   25
 31  \w     85.00 110.00   1.00   12.00    --  112.00  77.00   0.00   25
 32  \w     42.00  69.00   1.00   12.00    --  112.00 -85.00   0.00   27
 33  \w     42.00 109.00   1.00   12.00    --  112.00-111.00-120.00   67
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova (Cu) X-ray Source'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0610460000
_diffrn_orient_matrix_UB_12      -0.0533644000
_diffrn_orient_matrix_UB_13      0.0520819000
_diffrn_orient_matrix_UB_21      0.0177610000
_diffrn_orient_matrix_UB_22      -0.0916992000
_diffrn_orient_matrix_UB_23      -0.0462679000
_diffrn_orient_matrix_UB_31      0.0888102000
_diffrn_orient_matrix_UB_32      0.0549646000
_diffrn_orient_matrix_UB_33      -0.0265094000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            26709
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.101
_diffrn_reflns_theta_min         4.277
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.707
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_exptl_crystal_preparation       electrocrystallization
_exptl_crystal_recrystallization_method electrocrystallization
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         3923
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0792P)^2^+1.0747P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1217
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3607
_reflns_number_total             3923
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00091a2.cif
_cod_data_source_block           exp_1286_a
_cod_original_cell_volume        3758.61(11)
_cod_database_code               7244376
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C19H23O2S8
_chemical_oxdiff_usercomment     'purple block'
_cell_oxdiff_angle_alpha         90.044(2)
_cell_oxdiff_angle_beta          90.026(2)
_cell_oxdiff_angle_gamma         89.977(2)
_cell_oxdiff_length_a            14.1050(4)
_cell_oxdiff_length_b            12.8930(3)
_cell_oxdiff_length_c            20.6680(5)
_cell_oxdiff_measurement_reflns_used 12098
_cell_oxdiff_volume              3758.61(16)
_shelx_estimated_absorpt_t_max   0.007
_shelx_estimated_absorpt_t_min   0.007
_diffrn_oxdiff_digest_frames
;
01b06ecbd72c9ed28696e41d7bbdaaa73e00027aa22
;
_diffrn_oxdiff_digest_hkl
;
010ceb0f389822129ee4e83a32104d125178e8
;
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C006(H006), C00E(H00E), C00F(H00F), C00G(H00G), C00K(H00K), C00M(H00M),
 C00N(H00N), C00O(H00O), C00Q(H00Q), C00R(H00R), C00S(H00S)
2.b Idealised Me refined as rotating group:
 C00I(H00A,H00B,H00C), C00P(H00D,H00H,H00I)
;
_olex2_exptl_crystal_mounting_method 'paraffin oil'
_olex2_submission_original_sample_id exp_1286
_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 1.328
_oxdiff_exptl_absorpt_empirical_full_min 0.750