Sol–gel analogous aminolysis–ammonolysis of chlorosilanes to chlorine-free Si/(C)/N–materials
Wiltzsch, Conny; Wagler, Jörg; Roewer, Gerhard; Kroke, Edwin; Dalton Transactions  (2009) 5474–5477; doi:10.1039/b823030g

data_7001666
_publ_section_title
;
 Sol--gel analogous aminolysis--ammonolysis of chlorosilanes to
 chlorine-free Si/(C)/N--materials
;
_journal_issue                   28
_journal_name_full               'Dalton Transactions'
_journal_page_first              5474
_journal_page_last               5477
_journal_paper_doi               10.1039/b823030g
_journal_year                    2009
_chemical_formula_moiety         'C9 H39 N13 Si9'
_chemical_formula_sum            'C9 H39 N13 Si9'
_chemical_formula_weight         582.34
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   12.5915(7)
_cell_length_b                   12.5915(7)
_cell_length_c                   30.8770(14)
_cell_measurement_reflns_used    7399
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      29.15
_cell_measurement_theta_min      3.23
_cell_volume                     4239.6(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP32 (Farugia)'
_computing_publication_material  'Ciftab (Sheldrick)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0149
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            20394
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    0.449
_exptl_absorpt_correction_T_max  0.9156
_exptl_absorpt_correction_T_min  0.8255
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1860
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.218
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         2172
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.218
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0275P)^2^+28.6407P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1140
_reflns_number_gt                2020
_reflns_number_total             2172
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b823030g.txt
_cod_data_source_block           cw01_r-3
_cod_original_sg_symbol_Hall     -R3
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7001666