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

data_7244375
_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         'C18 H11 O3 S, C10 H12 S4'
_chemical_formula_sum            'C28 H23 O3 S5'
_chemical_formula_weight         567.76
_chemical_name_systematic        ([4]heliceneSO3)2(TMTTF)2
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-13
_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
_cell_angle_beta                 102.089(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.5199(9)
_cell_length_b                   21.0758(15)
_cell_length_c                   19.3165(10)
_cell_measurement_reflns_used    2545
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      71.6810
_cell_measurement_theta_min      3.8460
_cell_volume                     4984.0(6)
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.953
_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    -38.00   4.00   1.00   16.50    --   41.11 -19.00-180.00   42
  2  \w     38.00  79.00   1.00   16.50    --   41.11-125.00  30.00   41
  3  \w    -30.00  26.00   1.00   16.50    --   41.11 -19.00 -60.00   56
  4  \w    -27.00  64.00   1.00   16.50    --   41.11 -57.00  60.00   91
  5  \w     22.00 106.00   1.00   66.00    --  103.45 -94.00 -60.00   84
  6  \w     38.00  67.00   1.00   66.00    --  103.45 -61.00 -30.00   29
  7  \w     52.00 158.00   1.00   66.00    --  103.45  15.00 -90.00  106
  8  \w     78.00 152.00   1.00   66.00    --  103.45  45.00 150.00   74
  9  \w     35.00  71.00   1.00   66.00    --  103.45 -61.00-150.00   36
 10  \w     27.00 105.00   1.00   66.00    --  103.45 -77.00 120.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1014154000
_diffrn_orient_matrix_UB_12      -0.0092726000
_diffrn_orient_matrix_UB_13      -0.0323833000
_diffrn_orient_matrix_UB_21      0.0743003000
_diffrn_orient_matrix_UB_22      0.0182806000
_diffrn_orient_matrix_UB_23      0.0713094000
_diffrn_orient_matrix_UB_31      0.0059428000
_diffrn_orient_matrix_UB_32      -0.0701352000
_diffrn_orient_matrix_UB_33      0.0228307000
_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  0.0630
_diffrn_reflns_av_unetI/netI     0.0924
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18501
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.108
_diffrn_reflns_theta_min         2.339
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.542
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.755
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
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    1.513
_exptl_crystal_description       block
_exptl_crystal_F_000             2360
_exptl_crystal_preparation       electrocrystallization
_exptl_crystal_recrystallization_method electrocrystallization
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.057
_refine_diff_density_max         1.217
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         9372
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1446
_refine_ls_R_factor_gt           0.0952
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1130P)^2^+34.8087P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2419
_refine_ls_wR_factor_ref         0.2851
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6052
_reflns_number_total             9372
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00091a2.cif
_cod_data_source_block           exp_1570
_cod_depositor_comments
;

2024-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C56 H46 O6 S10'
_cod_original_formula_weight         1135.53
_cod_original_formula_moiety         '2(C18 H11 O3 S), 2(C10 H12 S4)'
_cod_original_formula_units_Z            4
_cod_database_code               7244375
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C46 H32 O6 S6'
_chemical_oxdiff_usercomment     'purple platelets'
_diffrn_oxdiff_digest_frames
;
0187f8fa3ad90dc5f3ae776562d3b379bb006658a05
;
_diffrn_oxdiff_digest_hkl
;
01f2c9a12142968b6e73b80de6e1caa6fa00ce
;
_reflns_odcompleteness_completeness 98.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9251(15)
 0.0749(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C6) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(C14) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(C22) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
4. Rigid body (RIGU) restrains
 C6, C5, C4, C3, C2, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C14, C13, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C16(H16), C11(H11), C3(H3), C4(H4), C7(H7), C8(H8), C18(H18),
 C17(H17), C2(H2), C1(H1), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25),
 C26(H26), C29(H29), C30(H30), C34(H34), C35(H35), C36(H36)
5.b Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C40(H40A,H40B,H40C), C45(H45A,H45B,H45C), C46(H46A,H46B,
 H46C), C47(H47A,H47B,H47C), C50(H50A,H50B,H50C), C55(H55A,H55B,H55C), C56(H56A,
 H56B,H56C)
;
_ins_header
;
TITL exp_1570 in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184  12.519922  21.075814  19.316516  90.0000 102.0890  90.0000
ZERR    5.00   0.000946   0.001454   0.001037   0.0000   0.0062   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H O S
UNIT 230.00 160.00 30.00 30.00
TREF
HKLF 4
END
;
_olex2_date_sample_data_collection 2020-09-23
_olex2_exptl_crystal_mounting_method 'paraffin oil'
_olex2_submission_original_sample_id exp_1570
_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 1.155
_oxdiff_exptl_absorpt_empirical_full_min 0.874