Pentasulfurated benzene-cored asterisks: relationship between crystal structure and luminescence properties
Villa, Marco; D’Agostino, Simone; Sabatino, Piera; Noel, Raymond; Busto, José; Roy, Myriam; Gingras, Marc; Ceroni, Paola; New Journal of Chemistry 44 (2020) 3249–3254; doi:10.1039/C9NJ05905A

data_7059238
_publ_section_title
;
 Pentasulfurated benzene-cored asterisks: relationship between crystal
 structure and luminescence properties
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3249
_journal_page_last               3254
_journal_paper_doi               10.1039/C9NJ05905A
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C43 H38 S5'
_chemical_formula_sum            'C43 H38 S5'
_chemical_formula_weight         715.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-16 deposited with the CCDC.	2020-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.45(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.507(3)
_cell_length_b                   5.9240(10)
_cell_length_c                   23.648(5)
_cell_measurement_reflns_used    614
_cell_measurement_temperature    300
_cell_measurement_theta_max      18.3180
_cell_measurement_theta_min      3.6590
_cell_volume                     1886.5(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53a (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_temperature      300
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1340
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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     -9.00  39.00   1.00  275.00    --   18.00  77.00 150.00   48
  2  \w     -8.00  17.00   1.00  475.00    --   18.00  77.00   0.00   25
  3  \w     40.00  68.00   1.00  475.00    --   18.00 178.00-150.00   28
  4  \w    -54.00  55.00   1.00  475.00    --   18.00 -19.00 -30.00  109
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0462188000
_diffrn_orient_matrix_UB_12      -0.0475868000
_diffrn_orient_matrix_UB_13      0.0100891000
_diffrn_orient_matrix_UB_21      -0.0106063000
_diffrn_orient_matrix_UB_22      0.0246387000
_diffrn_orient_matrix_UB_23      0.0282443000
_diffrn_orient_matrix_UB_31      -0.0230051000
_diffrn_orient_matrix_UB_32      -0.1071002000
_diffrn_orient_matrix_UB_33      0.0019699000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0888
_diffrn_reflns_av_unetI/netI     0.3236
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            6942
_diffrn_reflns_point_group_measured_fraction_full 0.797
_diffrn_reflns_point_group_measured_fraction_max 0.797
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.366
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.337
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.06933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53a (Rigaku Oxford Diffraction, 2019)
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    1.259
_exptl_crystal_description       needle
_exptl_crystal_F_000             752
_exptl_crystal_recrystallization_method 'slow evaporation'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.201
_refine_diff_density_min         -0.189
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.861
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         5287
_refine_ls_number_restraints     384
_refine_ls_restrained_S_all      0.839
_refine_ls_R_factor_all          0.2822
_refine_ls_R_factor_gt           0.0721
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1612
_reflns_Friedel_coverage         0.451
_reflns_Friedel_fraction_full    0.555
_reflns_Friedel_fraction_max     0.555
_reflns_number_gt                1478
_reflns_number_total             5287
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj05905a2.cif
_cod_data_source_block           a5-dl_r2
_cod_depositor_comments
;Adding full bibliography for 7059238--7059241.cif.

 Adding full bibliography for 7059238--7059241.cif.
;
_cod_database_code               7059238
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C50 H40 S5'
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.974
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C42-C43
 1.32 with sigma of 0.02
 C43-C6
 2.45 with sigma of 0.04
3. Rigid body (RIGU) restrains
 C43, C42, C6, C1, C2, C3, C4, C5, S2, S3, S4, S5, S1, C7, C8, C9, C10, C11,
 C12, C13, C35, C36, C37, C38, C39, C40, C41, C34, C31, C32, C33, C28, C29, C30,
  C21, C22, C23, C26, C25, C24, C27, C19, C14, C15, C18, C17, C16, C20
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C11(H11), C12(H12), C15(H15), C16(H16), C18(H18), C19(H19),
 C22(H22), C23(H23), C25(H25), C26(H26), C29(H29), C30(H30), C32(H32), C33(H33),
  C36(H36), C37(H37), C39(H39), C40(H40), C42(H42)
4.b X=CH2 refined with riding coordinates:
 C43(H43A,H43B)
4.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C20(H20A,H20B,H20C), C27(H27A,H27B,H27C), C34(H34A,H34B,
 H34C), C41(H41A,H41B,H41C)
;
_shelx_res_checksum              85047
_olex2_exptl_crystal_mounting_method 'fomblin oil'
_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 5.475
_oxdiff_exptl_absorpt_empirical_full_min 0.390