#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/16/7001666.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7001666
loop_
_publ_author_name
'Wiltzsch, Conny'
'Wagler, Jörg'
'Roewer, Gerhard'
'Kroke, Edwin'
_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
_chemical_name_systematic
;
?
;
_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/[σ²(Fo²)+(0.0275P)²+28.6407P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.55926(8) 0.38937(7) 0.21295(2) 0.0242(2) Uani 1 1 d . . .
Si2 Si 0.50510(7) 0.45868(7) 0.12034(3) 0.01980(19) Uani 1 1 d . . .
Si3 Si 0.73254(7) 0.49159(7) 0.07324(2) 0.02006(19) Uani 1 1 d . . .
N1 N 0.5228(3) 0.2390(2) 0.20793(9) 0.0326(6) Uani 1 1 d . . .
H1 H 0.4453 0.1881 0.2017 0.039 Uiso 1 1 calc R . .
N2 N 0.4846(2) 0.4283(2) 0.17449(8) 0.0274(5) Uani 1 1 d . . .
H2 H 0.4227 0.4336 0.1852 0.033 Uiso 1 1 calc R . .
N3 N 0.4470(2) 0.3326(2) 0.08612(9) 0.0297(6) Uani 1 1 d . . .
H3 H 0.3767 0.3126 0.0736 0.036 Uiso 1 1 calc R . .
N4 N 0.6606(2) 0.5350(2) 0.11104(7) 0.0198(5) Uani 1 1 d . . .
H4 H 0.7067 0.6007 0.1267 0.024 Uiso 1 1 calc R . .
N5 N 0.6667 0.3333 0.07392(13) 0.0221(8) Uani 1 3 d S . .
C1 C 0.5117(4) 0.4176(3) 0.26655(11) 0.0476(10) Uani 1 1 d . . .
H1A H 0.4221 0.3701 0.2689 0.071 Uiso 1 1 calc R . .
H1B H 0.5394 0.5051 0.2696 0.071 Uiso 1 1 calc R . .
H1C H 0.5483 0.3924 0.2895 0.071 Uiso 1 1 calc R . .
C2 C 0.4244(3) 0.5443(3) 0.10646(13) 0.0378(8) Uani 1 1 d . . .
H2A H 0.3359 0.4905 0.1102 0.057 Uiso 1 1 calc R . .
H2B H 0.4420 0.5721 0.0763 0.057 Uiso 1 1 calc R . .
H2C H 0.4530 0.6155 0.1256 0.057 Uiso 1 1 calc R . .
C3 C 0.7196(4) 0.5454(4) 0.01854(10) 0.0415(9) Uani 1 1 d . . .
H3A H 0.7700 0.6350 0.0172 0.062 Uiso 1 1 calc R . .
H3B H 0.6338 0.5208 0.0128 0.062 Uiso 1 1 calc R . .
H3C H 0.7482 0.5088 -0.0033 0.062 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Si1 N1 106.76(18) . 3_665 ?
N1 Si1 N2 111.50(13) . . ?
N1 Si1 N2 111.56(12) 3_665 . ?
N1 Si1 C1 110.98(16) . . ?
N1 Si1 C1 109.53(16) 3_665 . ?
N2 Si1 C1 106.55(18) . . ?
N2 Si2 N4 106.92(12) . . ?
N2 Si2 N3 116.39(14) . . ?
N4 Si2 N3 104.51(12) . . ?
N2 Si2 C2 106.86(16) . . ?
N4 Si2 C2 115.85(14) . . ?
N3 Si2 C2 106.70(14) . . ?
N4 Si3 N3 110.35(13) . 3_665 ?
N4 Si3 N5 109.30(13) . . ?
N3 Si3 N5 107.29(10) 3_665 . ?
N4 Si3 C3 110.12(14) . . ?
N3 Si3 C3 109.16(17) 3_665 . ?
N5 Si3 C3 110.57(18) . . ?
Si1 N1 Si1 131.56(17) . 2_655 ?
Si1 N1 H1 114.2 . . ?
Si1 N1 H1 114.2 2_655 . ?
Si2 N2 Si1 133.91(14) . . ?
Si2 N2 H2 113.0 . . ?
Si1 N2 H2 113.0 . . ?
Si3 N3 Si2 128.86(14) 2_655 . ?
Si3 N3 H3 115.6 2_655 . ?
Si2 N3 H3 115.6 . . ?
Si2 N4 Si3 124.58(13) . . ?
Si2 N4 H4 117.7 . . ?
Si3 N4 H4 117.7 . . ?
Si3 N5 Si3 119.987(7) 3_665 . ?
Si3 N5 Si3 119.985(7) 3_665 2_655 ?
Si3 N5 Si3 119.985(7) . 2_655 ?
Si1 C1 H1A 109.5 . . ?
Si1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Si1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si2 C2 H2A 109.5 . . ?
Si2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Si2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si3 C3 H3A 109.5 . . ?
Si3 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Si3 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 N1 1.718(3) . ?
Si1 N1 1.723(3) 3_665 ?
Si1 N2 1.731(3) . ?
Si1 C1 1.854(3) . ?
Si2 N2 1.706(3) . ?
Si2 N4 1.720(2) . ?
Si2 N3 1.735(3) . ?
Si2 C2 1.864(3) . ?
Si3 N4 1.725(2) . ?
Si3 N3 1.726(3) 3_665 ?
Si3 N5 1.7339(8) . ?
Si3 C3 1.857(3) . ?
N1 H1 0.8800 . ?
N2 H2 0.8800 . ?
N3 H3 0.8800 . ?
N4 H4 0.8800 . ?
N5 Si3 1.7339(8) 3_665 ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Si1 N1 Si1 18.6(3) 3_665 . . 2_655 ?
N2 Si1 N1 Si1 140.7(2) . . . 2_655 ?
C1 Si1 N1 Si1 -100.7(3) . . . 2_655 ?
N4 Si2 N2 Si1 -36.1(3) . . . . ?
N3 Si2 N2 Si1 80.2(2) . . . . ?
C2 Si2 N2 Si1 -160.7(2) . . . . ?
N1 Si1 N2 Si2 -75.4(2) . . . . ?
N1 Si1 N2 Si2 43.8(3) 3_665 . . . ?
C1 Si1 N2 Si2 163.3(2) . . . . ?
N2 Si2 N3 Si3 -78.9(2) . . . 2_655 ?
N4 Si2 N3 Si3 38.8(2) . . . 2_655 ?
C2 Si2 N3 Si3 162.0(2) . . . 2_655 ?
N2 Si2 N4 Si3 126.77(16) . . . . ?
N3 Si2 N4 Si3 2.8(2) . . . . ?
C2 Si2 N4 Si3 -114.27(19) . . . . ?
N3 Si3 N4 Si2 -158.55(15) 3_665 . . . ?
N5 Si3 N4 Si2 -40.8(2) . . . . ?
C3 Si3 N4 Si2 80.9(2) . . . . ?
N4 Si3 N5 Si3 -135.0(2) . . . 3_665 ?
N3 Si3 N5 Si3 -15.4(3) 3_665 . . 3_665 ?
C3 Si3 N5 Si3 103.6(3) . . . 3_665 ?
N4 Si3 N5 Si3 47.3(3) . . . 2_655 ?
N3 Si3 N5 Si3 167.0(2) 3_665 . . 2_655 ?
C3 Si3 N5 Si3 -74.1(3) . . . 2_655 ?
