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_4327962
_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_compound_source        'synthesis as described'
_chemical_formula_moiety         'C36 H51 O3 S Si, C36 H44 Na O10, 2(C7 H8)'
_chemical_formula_sum            'C86 H111 Na O13 S Si'
_chemical_formula_weight         1435.89
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_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             2010-12-02T20:27:18-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                82.752(4)
_cell_angle_beta                 87.179(4)
_cell_angle_gamma                68.636(4)
_cell_formula_units_Z            2
_cell_length_a                   15.0557(6)
_cell_length_b                   16.9264(8)
_cell_length_c                   16.9715(7)
_cell_measurement_reflns_used    11788
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.7122
_cell_measurement_theta_min      2.4146
_cell_measurement_wavelength     0.71073
_cell_volume                     3995.6(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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0484027
_diffrn_orient_matrix_UB_12      0.0276786
_diffrn_orient_matrix_UB_13      0.0011581
_diffrn_orient_matrix_UB_21      -0.0068542
_diffrn_orient_matrix_UB_22      -0.0239803
_diffrn_orient_matrix_UB_23      0.0356087
_diffrn_orient_matrix_UB_31      0.013013
_diffrn_orient_matrix_UB_32      0.026671
_diffrn_orient_matrix_UB_33      0.0224868
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0658
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25869
_diffrn_reflns_theta_full        25.5
_diffrn_reflns_theta_max         25.5
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    0.122
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_description       prism
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.143
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.08
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     933
_refine_ls_number_reflns         14837
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.08
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0686
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0991P)^2^+4.4683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1977
_refine_ls_wR_factor_ref         0.2063
_reflns_number_gt                9767
_reflns_number_total             14837
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic2013073_si_001_4.cif
_cod_data_source_block           ania80_5
_cod_database_code               4327962