Syntheses and crystal structure of a (2,6-diiso-propyldi-naphtho-[2,1-<i>d</i>:1',2'-<i>f</i>][1,3]dithiepin-4-yl)(phen-yl)methanol atropisomer.
Beare, Neil; Painter, Gavin F.; McAdam, C. John; Acta crystallographica. Section E, Crystallographic communications 79 (2023) 241–245; doi:10.1107/S2056989023001706

data_2312074
_publ_section_title
;
 Syntheses and crystal structure of a
 (2,6-diiso-propyldi-naphtho-[2,1-<i>d</i>:1',2'-<i>f</i>][1,3]dithiepin-4-yl)(phen-yl)methanol
 atropisomer.
;
_journal_coeditor_code           HB8055
_journal_issue                   'Pt 3'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              241
_journal_page_last               245
_journal_paper_doi               10.1107/S2056989023001706
_journal_volume                  79
_journal_year                    2023
_chemical_formula_iupac          'C34 H32 O S2'
_chemical_formula_moiety         'C34 H32 O S2'
_chemical_formula_sum            'C34 H32 O S2'
_chemical_formula_weight         520.71
_chemical_name_systematic
'(2,6-Diisopropyldinaphtho[2,1-<i>d</i>:1',2'-<i>f</i>][1,3]dithiepin-4-yl)(phenyl)methanol atropisomer'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2019/2
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.874(4)
_cell_length_b                   19.579(7)
_cell_length_c                   24.374(9)
_cell_measurement_reflns_used    5483
_cell_measurement_temperature    168(2)
_cell_measurement_theta_max      26.33
_cell_measurement_theta_min      2.17
_cell_volume                     5666(3)
_computing_cell_refinement
;
SAINT (Bruker, 1997)
;
_computing_data_collection
;
SMART (Bruker, 1997)
;
_computing_data_reduction
;
SAINT (Bruker, 1997)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>, 2020)
;
_computing_publication_material
;
PublCIF (Westrip 2010)
;
_computing_structure_refinement
;
<i>SHELXL2019/2</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      168(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1342
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            68261
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.331
_diffrn_reflns_theta_min         2.173
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.213
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.835378
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.276
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         5679
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1169
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0365P)^2^+6.2206P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1270
_reflns_number_gt                3354
_reflns_number_total             5679
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb8055sup1.cif
_cod_data_source_block           I
_cod_database_code               2312074
_shelx_hkl_checksum              85285
_shelx_res_checksum              73143
_cod_database_fobs_code 2312074