Tris[2,2,6,6-tetramethyl-8-(trimethylsilyl)benzo[1,2-<i>d</i>;4,5-<i>d</i>']bis(1,3-dithiol)-4-yl]methanol diethyl ether monosolvate
Fleck, Nico; Schnakenburg, Gregor; Filippou, Alexander C.; Schiemann, Olav; Acta Crystallographica Section E 74 (2018) 539–542; doi:10.1107/S2056989018004516

data_2242430
_publ_section_title
;
 Tris[2,2,6,6-tetramethyl-8-(trimethylsilyl)benzo[1,2-<i>d</i>;4,5-<i>d</i>']bis(1,3-dithiol)-4-yl]methanol
 diethyl ether monosolvate
;
_journal_coeditor_code           NK2246
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              539
_journal_page_last               542
_journal_paper_doi               10.1107/S2056989018004516
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C46 H64 O S12 Si3'
_chemical_formula_moiety         'C46 H64 O S12 Si3'
_chemical_formula_sum            'C46 H64 O S12 Si3'
_chemical_formula_weight         1101.96
_chemical_name_systematic
'Tris[2,2,6,6-tetramethyl-8-(trimethylsilyl)benzo[1,2-<i>d</i>;4,5-<i>d</i>']bis(1,3-dithiol)-4-yl]methanol diethyl ether monosolvate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.03.09 svn.r3491 for OlexSys, GUI svn.r5479)
;
_cell_angle_alpha                91.6815(13)
_cell_angle_beta                 117.6083(11)
_cell_angle_gamma                99.1383(12)
_cell_formula_units_Z            2
_cell_length_a                   14.9964(4)
_cell_length_b                   15.1070(4)
_cell_length_c                   16.0026(4)
_cell_measurement_reflns_used    9511
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.28
_cell_measurement_theta_min      2.98
_cell_volume                     3149.79(15)
_computing_cell_refinement
;
SAINT (Bruker, 2015)
;
_computing_data_collection
;
SMART (Bruker, 2015)
;
_computing_data_reduction
;
SAINT (Bruker, 2015)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
<i>SHELXL2014/7</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8-Venture'
_diffrn_measurement_method       'fine slicing \w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0912
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            74526
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.744
_diffrn_reflns_theta_min         2.983
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.637
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.2521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2015)
;
_exptl_crystal_colour            'clear yellowish blue'
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_description       plate
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.891
_refine_diff_density_min         -1.338
_refine_ls_extinction_coef       0.0018(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
<i>SHELXL2014/7</i> (Sheldrick 2015)
;
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         11369
_refine_ls_number_restraints     214
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0641
_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^)+(0.1335P)^2^+2.6751P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1726
_refine_ls_wR_factor_ref         0.1833
_reflns_number_gt                9723
_reflns_number_total             11369
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nk2246sup1.cif
_cod_data_source_block           I
_cod_database_code               2242430
_cod_database_fobs_code          2242430
_shelx_estimated_absorpt_t_min   0.302
_shelx_estimated_absorpt_t_max   0.836
_shelx_hkl_checksum              25368
_shelx_res_checksum              89109
_shelx_fab_checksum              45041