Intramolecular Interactions in Crystals of Tris(2,6-diisopropylphenoxy)silanethiol and Its Sodium Salts
Anna Dołęga; Wojciech Marynowski; Katarzyna Baranowska; Maciej Śmiechowski; Janusz Stangret; Inorganic Chemistry 51 (2012) 836–843; doi:10.1021/ic2013073

data_4327959
_publ_contact_author_address
;
Department of Chemistry
Gda\'nsk University of Technology
Narutowicza 11/12,
PL-80233 Gda\'nsk, Poland
;
_publ_contact_author_email       anna.dolega@pg.gda.pl
_publ_contact_author_fax         '048 58 3472694'
_publ_contact_author_name        'Dolega, Anna'
_publ_contact_author_phone       '048 58 3472351'
_publ_section_title
;
 Intramolecular Interactions in Crystals of
 Tris(2,6-diisopropylphenoxy)silanethiol and Its Sodium Salts
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              836
_journal_page_last               843
_journal_paper_doi               10.1021/ic2013073
_journal_volume                  51
_journal_year                    2012
_chemical_absolute_configuration unk
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C36 H52 O3 S1 Si1'
_chemical_formula_sum            'C36 H52 O3 S Si'
_chemical_formula_weight         592.93
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2011-03-21T11:23:16-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 122.677(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4061(8)
_cell_length_b                   35.0837(9)
_cell_length_c                   10.2841(4)
_cell_measurement_reflns_used    14402
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.8389
_cell_measurement_theta_min      2.3191
_cell_measurement_wavelength     0.71073
_cell_volume                     3464.0(3)
_computing_cell_refinement
;
        CrysAlis RED (Oxford Diffraction, 2006)

;
_computing_data_collection
;
        CrysAlis CCD (Oxford Diffraction, 2006)

;
_computing_data_reduction
;
        CrysAlis RED (Oxford Diffraction, 2006)

;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.1883
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0506948329
_diffrn_orient_matrix_UB_12      0.0104612437
_diffrn_orient_matrix_UB_13      -0.0047682039
_diffrn_orient_matrix_UB_21      -0.053284721
_diffrn_orient_matrix_UB_22      0.0114989664
_diffrn_orient_matrix_UB_23      -0.0591500539
_diffrn_orient_matrix_UB_31      0.0063138666
_diffrn_orient_matrix_UB_32      0.012916694
_diffrn_orient_matrix_UB_33      0.0564959809
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0151
_diffrn_reflns_av_unetI/netI     0.0139
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10968
_diffrn_reflns_theta_full        25.5
_diffrn_reflns_theta_max         25.5
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    0.16
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.943
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_description       prism
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.6562
_exptl_crystal_size_mid          0.3494
_exptl_crystal_size_min          0.1981
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.214
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.87(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         5572
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+1.3698P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0783
_reflns_number_gt                5446
_reflns_number_total             5572
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic2013073_si_001_1.cif
_cod_data_source_block           ania75_1
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4327959