Synthesis, characterization and theoretical calculations of model compounds of silanols catalyzed by TEMPO to elucidate the presence of Si-O-Si and Si-O-N bonds.
Percino, M. Judith; Pacheco, José Alberto; Soriano, Guillermo; Ceron, Margarita; Castro, María Eugenia; Chapela, Víctor M.; bonilla-cruz, jose; Lara, Tania; Flores, Mildred; Saldivar, Enrique; RSC Adv.  (2015) –; doi:10.1039/C5RA10056A

data_7222038
_publ_section_title
;
 Synthesis, characterization and theoretical calculations of model
 compounds of silanols catalyzed by TEMPO to elucidate the presence of
 Si-O-Si and Si-O-N bonds.
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA10056A
_journal_year                    2015
_chemical_formula_moiety         'C36 H30 O Si2'
_chemical_formula_sum            'C36 H30 O Si2'
_chemical_formula_weight         534.78
_chemical_melting_point          498
_chemical_name_common            'hexaphenyldisiloxane '
_chemical_name_systematic        di(triphenylsilane)ether
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-05-09 deposited with the CCDC.
2015-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                95.951(4)
_cell_angle_beta                 111.779(4)
_cell_angle_gamma                113.352(4)
_cell_formula_units_Z            1
_cell_length_a                   8.5829(4)
_cell_length_b                   9.4856(4)
_cell_length_c                   10.9694(5)
_cell_measurement_reflns_used    7041
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      71.95
_cell_measurement_theta_min      4.51
_cell_volume                     727.71(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9218
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.896
_diffrn_reflns_theta_min         4.541
_exptl_absorpt_coefficient_mu    1.305
_exptl_absorpt_correction_T_max  0.837
_exptl_absorpt_correction_T_min  0.772
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_description       block
_exptl_crystal_F_000             282
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2833
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0360P)^2^+0.3704P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0828
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2707
_reflns_number_total             2833
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra10056a1.cif
_cod_data_source_block           '[di(triphenylsilane)ether]'
_cod_original_cell_volume        727.71(6)
_cod_database_code               7222038
_shelxl_version_number           2013-2
_shelx_res_checksum              71667
_shelx_hkl_checksum              95211