Variable-temperature X-ray diffraction study of structural parameters of NH—S hydrogen bonds in triethylammonium and pyridinium silanethiolates
Mielcarek, Agnieszka; Daszkiewicz, Marek; Kazimierczuk, Katarzyna; Ciborska, Anna; Dołega, Anna; Acta Crystallographica Section B 72 (2016) 763–770; doi:10.1107/S2052520616011562

data_2107978
_publ_section_title
;
 Variable-temperature X-ray diffraction study of structural parameters of
 NH---S hydrogen bonds in triethylammonium and pyridinium silanethiolates
;
_journal_coeditor_code           EB5051
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              763
_journal_page_last               770
_journal_paper_doi               10.1107/S2052520616011562
_journal_volume                  72
_journal_year                    2016
_chemical_formula_sum            'C42 H67 N O3 S Si'
_chemical_formula_weight         694.11
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 101.098(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6341(17)
_cell_length_b                   17.8996(16)
_cell_length_c                   20.096(3)
_cell_measurement_reflns_used    1642
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      29.42
_cell_measurement_theta_min      3.44
_cell_volume                     4106.6(9)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  'parabolic x-ray mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0835
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13602
_diffrn_reflns_theta_full        25.998
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         3.074
_exptl_absorpt_coefficient_mu    0.145
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.253
_refine_ls_abs_structure_details
;
 Flack x determined using 1785 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.879
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         7538
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.879
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0501
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0406P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1045
_reflns_number_gt                5341
_reflns_number_total             7538
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            eb5051sup1.cif
_cod_data_source_block           tdst_et3n_90
_cod_original_cell_volume        4106.7(9)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2107978
_cod_database_fobs_code          2107978