Chalcogen controlled redox behaviour in peri-substituted S, Se and Te naphthalene derivatives
Roemmele, Tracey L.; Knight, Fergus R.; Crawford, Ellis; Robertson, Stuart D.; Bode, Bela E.; Bühl, Michael; Slawin, Alexandra M. Z.; Woollins, J. Derek; Boeré, René T.; New Journal of Chemistry 46 (2022) 22363–22383; doi:10.1039/D2NJ04737C

data_7062029
_publ_section_title
;
 Chalcogen controlled redox behaviour in peri-substituted S, Se and Te
 naphthalene derivatives
;
_journal_issue                   46
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              22363
_journal_page_last               22383
_journal_paper_doi               10.1039/D2NJ04737C
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C25 H21 O S Te, B F4, H2 O'
_chemical_formula_sum            'C25 H23 B F4 O2 S Te'
_chemical_formula_weight         601.90
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2022-10-20
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-10-28 deposited with the CCDC.	2022-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                83.26(3)
_cell_angle_beta                 71.08(2)
_cell_angle_gamma                68.25(2)
_cell_formula_units_Z            4
_cell_length_a                   11.7625(19)
_cell_length_b                   14.972(4)
_cell_length_c                   15.390(3)
_cell_measurement_reflns_used    9268
_cell_measurement_temperature    125
_cell_measurement_theta_max      29.13
_cell_measurement_theta_min      1.40
_cell_volume                     2381.3(10)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r6'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r6 (Rigaku, 2010)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r6'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-1997  (Sheldrick, 2008)'
_diffrn_ambient_temperature      125.15
_diffrn_detector_area_resol_mean 28.626
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0839
_diffrn_reflns_av_unetI/netI     0.1415
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18166
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         1.399
_exptl_absorpt_coefficient_mu    1.389
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.827
_refine_diff_density_min         -1.215
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         8545
_refine_ls_number_restraints     506
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1284
_refine_ls_R_factor_gt           0.0758
_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^)+(0.0413P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1447
_refine_ls_wR_factor_ref         0.1740
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5239
_reflns_number_total             8545
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj04737c2.cif
_cod_data_source_block           A19
_cod_depositor_comments
'Adding full bibliography for 7062029--7062033.cif.'
_cod_original_cell_volume        2381.4(10)
_cod_database_code               7062029
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.819
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Free rotating group:
 O3(H3A,H3B), O4(H4A,H4B)
4.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C41(H41A,H41B), C42(H42A,H42B)
4.c Me refined with riding coordinates:
 C19(H19A,H19B,H19C), C49(H49A,H49B,H49C)
4.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C8(H8), C14(H14), C15(H15), C16(H16), C17(H17),
 C18(H18), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C32(H32), C33(H33),
  C37(H37), C38(H38), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48),
 C51(H51), C52(H52), C53(H53), C54(H54), C55(H55)
;
_shelx_res_checksum              51172
_olex2_submission_special_instructions 'No special instructions were received'