#------------------------------------------------------------------------------
#$Date: 2019-11-23 08:01:50 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232500 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/77/4347787.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_4347787
loop_
_publ_author_name
'Axthammer, Quirin J.'
'Klapötke, Thomas M'
'Krumm, Burkhard'
'Reith, Thomas'
_publ_section_title
;
 Energetic Sila-Nitrocarbamates: Silicon Analogues of Neo-Pentane
 Derivatives.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4683
_journal_page_last               4692
_journal_paper_doi               10.1021/acs.inorgchem.6b00602
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C8 H18 N4 O9 Si2'
_chemical_formula_weight         370.421
_chemical_name_common
'(1,1,3,3-tetramethyldisiloxane-1,3-diyl)bis(methylene) bis(nitrocarbamate)'
_chemical_name_systematic
'(1,1,3,3-tetramethyldisiloxane-1,3-diyl)bis(methylene) bis(nitrocarbamate)'
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date
;
'Sat Feb 07 10:22:08 2015'
;
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.0
_cell_angle_beta                 91.258(5)
_cell_angle_gamma                90.0
_cell_formula_units_Z            6
_cell_length_a                   25.7845(17)
_cell_length_b                   11.6651(9)
_cell_length_c                   8.7953(4)
_cell_measurement_reflns_used    2433
_cell_measurement_temperature    172.9(8)
_cell_measurement_theta_max      30.5060
_cell_measurement_theta_min      4.3090
_cell_volume                     2644.8(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics
;
'ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid
# Plot Program for Crystal Structure Illustrations, Oak Ridge National
# Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ.
# Glasgow) used --- SCHAKAL (E. Keller, University of  Freiburg (Breisgau),
# Germany, 1995)'
;
_computing_publication_material
;PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version).
# --- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses).
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      172.9(8)
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.9963
_diffrn_measured_fraction_theta_max 0.9061
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   58.00  100.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   57.0000  -60.0000 42

#__ type_ start__ end____ width___ exp.time_
  2 omega   37.00  109.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  179.0000  -60.0000 72

#__ type_ start__ end____ width___ exp.time_
  3 omega  -11.00   74.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000    0.0000 85

#__ type_ start__ end____ width___ exp.time_
  4 omega  -98.00  -29.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -38.0000    0.0000 69

;
_diffrn_measurement_device       'CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       omega-scan
_diffrn_orient_matrix_UB_11      0.0157883000
_diffrn_orient_matrix_UB_12      0.0442852000
_diffrn_orient_matrix_UB_13      0.0310769000
_diffrn_orient_matrix_UB_21      0.0172875000
_diffrn_orient_matrix_UB_22      -0.0416043000
_diffrn_orient_matrix_UB_23      0.0310219000
_diffrn_orient_matrix_UB_31      0.0144807000
_diffrn_orient_matrix_UB_32      0.0012721000
_diffrn_orient_matrix_UB_33      -0.0676638000
_diffrn_radiation_collimation    0.5
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_sigmaI/netI    0.0724
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16460
_diffrn_reflns_theta_full        30.4405
_diffrn_reflns_theta_max         32.3341
_diffrn_reflns_theta_min         4.2230
_diffrn_source_current           40
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.248
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         5376
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0383P)²+0.7909P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0916
_refine_ls_wR_factor_ref         0.1014
_reflns_number_gt                4021
_reflns_number_total             5376
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic6b00602_si_002.cif
_cod_data_source_block           5
_cod_database_code               4347787
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
C5 C 0.37415(9) 0.0578(2) 0.2704(3) 0.0346(5) Uani 1 1 d .
H5A H 0.38080(14) -0.0207(14) 0.2655(3) 0.042 Uiso 1 1 calc R
H5B H 0.36668(15) 0.0842(5) 0.1721(17) 0.042 Uiso 1 1 calc R
C6 C 0.44686(8) 0.18224(18) 0.2416(2) 0.0249(5) Uani 1 1 d .
C9 C 0.29878(9) -0.06582(19) 0.8360(2) 0.0311(5) Uani 1 1 d .
H9B H 0.3122(2) -0.1006(6) 0.9270(15) 0.037 Uiso 1 1 calc R
H9A H 0.2863(2) 0.0089(12) 0.8602(5) 0.037 Uiso 1 1 calc R
C10 C 0.22536(8) -0.18588(18) 0.8658(2) 0.0255(5) Uani 1 1 d .
C1 C 1.03639(9) 0.0691(2) 0.2870(3) 0.0345(5) Uani 1 1 d .
H1A H 1.0254(2) 0.1036(6) 0.3817(16) 0.041 Uiso 1 1 calc R
H1B H 1.04719(19) -0.0094(13) 0.3077(5) 0.041 Uiso 1 1 calc R
C2 C 1.11113(8) 0.18603(19) 0.3218(2) 0.0281(5) Uani 1 1 d .
C8 C 0.31153(11) 0.2425(2) 0.4161(3) 0.0517(7) Uani 1 1 d .
H8C H 0.2825 0.2602 0.4823 0.077 Uiso 1 1 calc R
H8B H 0.3051 0.2766 0.3157 0.077 Uiso 1 1 calc R
H8A H 0.3437 0.2739 0.4608 0.077 Uiso 1 1 calc R
C7 C 0.25942(11) 0.0187(3) 0.3111(3) 0.0574(8) Uani 1 1 d .
H7C H 0.2662 -0.0628 0.2929 0.086 Uiso 1 1 calc R
H7A H 0.2507 0.0566 0.2144 0.086 Uiso 1 1 calc R
H7B H 0.2304 0.0266 0.3804 0.086 Uiso 1 1 calc R
C11 C 0.36065(11) -0.1984(2) 0.6093(4) 0.0626(9) Uani 1 1 d .
H11A H 0.3283 -0.2246 0.5601 0.094 Uiso 1 1 calc R
H11C H 0.3708 -0.2521 0.6904 0.094 Uiso 1 1 calc R
H11B H 0.3880 -0.1951 0.5339 0.094 Uiso 1 1 calc R
C12 C 0.41118(10) -0.0003(3) 0.7799(3) 0.0528(7) Uani 1 1 d .
H12B H 0.4374 0.0103 0.7021 0.079 Uiso 1 1 calc R
H12C H 0.4240 -0.0551 0.8563 0.079 Uiso 1 1 calc R
H12A H 0.4041 0.0733 0.8288 0.079 Uiso 1 1 calc R
C4 C 0.97034(14) 0.2201(4) 0.0892(5) 0.1077(16) Uani 1 1 d .
H4B H 1.0028 0.2547 0.0563 0.162 Uiso 1 1 calc R
H4C H 0.9573 0.2626 0.1766 0.162 Uiso 1 1 calc R
H4A H 0.9446 0.2230 0.0056 0.162 Uiso 1 1 calc R
C3 C 0.92453(11) 0.0050(3) 0.2274(4) 0.0665(9) Uani 1 1 d .
H3B H 0.8962 0.0022 0.1512 0.100 Uiso 1 1 calc R
H3A H 0.9137 0.0506 0.3148 0.100 Uiso 1 1 calc R
H3C H 0.9330 -0.0730 0.2611 0.100 Uiso 1 1 calc R
N5 N 0.18855(7) -0.24450(19) 0.7789(2) 0.0352(5) Uani 1 1 d .
N6 N 0.15556(7) -0.3259(2) 0.8350(2) 0.0430(5) Uani 1 1 d .
N3 N 0.48502(7) 0.23545(17) 0.3310(2) 0.0299(4) Uani 1 1 d .
N4 N 0.51676(7) 0.32076(18) 0.2770(2) 0.0336(5) Uani 1 1 d .
N1 N 1.14911(7) 0.23944(19) 0.2377(2) 0.0354(5) Uani 1 1 d .
N2 N 1.18275(7) 0.32155(19) 0.2940(2) 0.0392(5) Uani 1 1 d .
O6A O 0.3319(4) 0.0430(16) 0.5683(9) 0.034(2) Uani 0.74(7) 1 d P
O11 O 0.25693(6) -0.13553(14) 0.77021(15) 0.0337(4) Uani 1 1 d .
O12 O 0.22833(6) -0.18168(15) 1.00097(16) 0.0429(4) Uani 1 1 d .
O13 O 0.13205(8) -0.3803(2) 0.7380(2) 0.0736(7) Uani 1 1 d .
O14 O 0.15193(7) -0.33705(17) 0.97123(19) 0.0550(5) Uani 1 1 d .
O7 O 0.41955(6) 0.11833(14) 0.33449(15) 0.0340(4) Uani 1 1 d .
O8 O 0.44018(6) 0.19320(14) 0.10774(15) 0.0347(4) Uani 1 1 d .
O9 O 0.52572(7) 0.32380(17) 0.14212(17) 0.0508(5) Uani 1 1 d .
O10 O 0.53471(7) 0.38515(17) 0.37350(19) 0.0494(5) Uani 1 1 d .
O1 O 1.00022(19) -0.0352(3) 0.0245(5) 0.0488(12) Uani 0.50 1 d P
O2 O 1.07943(6) 0.13457(14) 0.22405(16) 0.0357(4) Uani 1 1 d .
O3 O 1.10796(6) 0.18607(16) 0.45657(17) 0.0444(5) Uani 1 1 d .
O5 O 1.18561(7) 0.33748(17) 0.43051(18) 0.0488(5) Uani 1 1 d .
O4 O 1.20789(7) 0.37031(19) 0.1986(2) 0.0631(6) Uani 1 1 d .
O6B O 0.3273(6) -0.003(7) 0.539(5) 0.050(9) Uani 0.26(7) 1 d P
Si3 Si 0.35104(2) -0.05581(5) 0.69039(7) 0.02914(16) Uani 1 1 d .
Si2 Si 0.31777(2) 0.08591(5) 0.39677(7) 0.02886(16) Uani 1 1 d .
Si1 Si 0.98194(3) 0.07093(7) 0.14358(7) 0.0408(2) Uani 1 1 d .
H2 H 0.4814(9) 0.244(2) 0.426(3) 0.038(7) Uiso 1 1 d .
H1 H 1.1452(9) 0.243(2) 0.147(3) 0.032(7) Uiso 1 1 d .
H3 H 0.1928(9) -0.250(2) 0.690(3) 0.042(8) Uiso 1 1 d .
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
H H 0.0000 0.0000 '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
O7 C5 Si2 108.04(14) . .
O7 C5 H5A 110.1 . .
Si2 C5 H5A 110.1 . .
O7 C5 H5B 110.1 . .
Si2 C5 H5B 110.1 . .
H5A C5 H5B 108.4 . .
O8 C6 O7 127.1(2) . .
O8 C6 N3 126.50(19) . .
O7 C6 N3 106.36(17) . .
O11 C9 Si3 107.39(13) . .
O11 C9 H9B 110.2 . .
Si3 C9 H9B 110.2 . .
O11 C9 H9A 110.2 . .
Si3 C9 H9A 110.2 . .
H9B C9 H9A 108.5 . .
O12 C10 O11 126.2(2) . .
O12 C10 N5 126.8(2) . .
O11 C10 N5 107.01(17) . .
O2 C1 Si1 107.65(14) . .
O2 C1 H1A 110.2 . .
Si1 C1 H1A 110.2 . .
O2 C1 H1B 110.2 . .
Si1 C1 H1B 110.2 . .
H1A C1 H1B 108.5 . .
O3 C2 O2 126.5(2) . .
O3 C2 N1 126.5(2) . .
O2 C2 N1 106.96(17) . .
Si2 C8 H8C 109.5 . .
Si2 C8 H8B 109.5 . .
H8C C8 H8B 109.5 . .
Si2 C8 H8A 109.5 . .
H8C C8 H8A 109.5 . .
H8B C8 H8A 109.5 . .
Si2 C7 H7C 109.5 . .
Si2 C7 H7A 109.5 . .
H7C C7 H7A 109.5 . .
Si2 C7 H7B 109.5 . .
H7C C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
Si3 C11 H11A 109.5 . .
Si3 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
Si3 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
H11C C11 H11B 109.5 . .
Si3 C12 H12B 109.5 . .
Si3 C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
Si3 C12 H12A 109.5 . .
H12B C12 H12A 109.5 . .
H12C C12 H12A 109.5 . .
Si1 C4 H4B 109.5 . .
Si1 C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
Si1 C4 H4A 109.5 . .
H4B C4 H4A 109.5 . .
H4C C4 H4A 109.5 . .
Si1 C3 H3B 109.5 . .
Si1 C3 H3A 109.5 . .
H3B C3 H3A 109.5 . .
Si1 C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
N6 N5 C10 124.41(19) . .
N6 N5 H3 113.5(19) . .
C10 N5 H3 118.4(18) . .
O14 N6 O13 126.2(2) . .
O14 N6 N5 119.4(2) . .
O13 N6 N5 114.4(2) . .
N4 N3 C6 122.96(17) . .
N4 N3 H2 109.7(17) . .
C6 N3 H2 121.0(16) . .
O9 N4 O10 125.9(2) . .
O9 N4 N3 119.01(19) . .
O10 N4 N3 115.10(17) . .
N2 N1 C2 124.55(19) . .
N2 N1 H1 113.0(17) . .
C2 N1 H1 118.3(17) . .
O4 N2 O5 126.1(2) . .
O4 N2 N1 114.83(19) . .
O5 N2 N1 119.0(2) . .
O6B O6A Si2 80.9(19) . .
O6B O6A Si3 73(2) . .
Si2 O6A Si3 151.8(12) . .
C10 O11 C9 117.12(16) . .
C6 O7 C5 117.69(16) . .
O1 O1 Si1 78.6(5) 3_755 3_755
O1 O1 Si1 69.0(5) 3_755 .
Si1 O1 Si1 147.6(2) 3_755 .
C2 O2 C1 117.05(16) . .
O6A O6B Si3 85(4) . .
O6A O6B Si2 78(3) . .
Si3 O6B Si2 160(5) . .
O6B Si3 O6A 22(3) . .
O6B Si3 C11 94(3) . .
O6A Si3 C11 115.1(6) . .
O6B Si3 C12 122(2) . .
O6A Si3 C12 105.7(7) . .
C11 Si3 C12 111.49(14) . .
O6B Si3 C9 109.1(10) . .
O6A Si3 C9 106.19(19) . .
C11 Si3 C9 108.30(12) . .
C12 Si3 C9 109.86(11) . .
O6A Si2 O6B 22(2) . .
O6A Si2 C8 103.8(7) . .
O6B Si2 C8 125(3) . .
O6A Si2 C7 114.4(7) . .
O6B Si2 C7 99(2) . .
C8 Si2 C7 112.80(13) . .
O6A Si2 C5 109.58(19) . .
O6B Si2 C5 103.6(16) . .
C8 Si2 C5 107.34(12) . .
C7 Si2 C5 108.62(12) . .
O1 Si1 O1 32.4(2) 3_755 .
O1 Si1 C4 93.16(19) 3_755 .
O1 Si1 C4 125.45(19) . .
O1 Si1 C3 120.55(19) 3_755 .
O1 Si1 C3 100.36(19) . .
C4 Si1 C3 112.01(16) . .
O1 Si1 C1 113.02(19) 3_755 .
O1 Si1 C1 101.18(18) . .
C4 Si1 C1 107.70(15) . .
C3 Si1 C1 108.94(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C5 O7 1.469(3) .
C5 Si2 1.878(2) .
C5 H5A 0.9333 .
C5 H5B 0.9333 .
C6 O8 1.193(2) .
C6 O7 1.321(2) .
C6 N3 1.393(3) .
C9 O11 1.460(3) .
C9 Si3 1.883(2) .
C9 H9B 0.9551 .
C9 H9A 0.9551 .
C10 O12 1.190(2) .
C10 O11 1.321(2) .
C10 N5 1.386(3) .
C1 O2 1.466(3) .
C1 Si1 1.867(2) .
C1 H1A 0.9729 .
C1 H1B 0.9729 .
C2 O3 1.190(2) .
C2 O2 1.318(2) .
C2 N1 1.388(3) .
C8 Si2 1.841(3) .
C8 H8C 0.9800 .
C8 H8B 0.9800 .
C8 H8A 0.9800 .
C7 Si2 1.843(3) .
C7 H7C 0.9800 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C11 Si3 1.829(3) .
C11 H11A 0.9800 .
C11 H11C 0.9800 .
C11 H11B 0.9800 .
C12 Si3 1.841(3) .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C12 H12A 0.9800 .
C4 Si1 1.827(4) .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C4 H4A 0.9800 .
C3 Si1 1.837(3) .
C3 H3B 0.9800 .
C3 H3A 0.9800 .
C3 H3C 0.9800 .
N5 N6 1.374(3) .
N5 H3 0.80(2) .
N6 O14 1.211(2) .
N6 O13 1.214(2) .
N3 N4 1.379(3) .
N3 H2 0.85(2) .
N4 O9 1.214(2) .
N4 O10 1.217(2) .
N1 N2 1.377(3) .
N1 H1 0.81(2) .
N2 O4 1.213(2) .
N2 O5 1.216(2) .
O6A O6B 0.61(7) .
O6A Si2 1.624(6) .
O6A Si3 1.643(8) .
O1 O1 0.927(7) 3_755
O1 Si1 1.613(4) 3_755
O1 Si1 1.694(4) .
O6B Si3 1.577(18) .
O6B Si2 1.64(2) .
Si1 O1 1.613(4) 3_755
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_4
O12 C10 N5 N6 -13.6(4) . .
O11 C10 N5 N6 166.1(2) . .
C10 N5 N6 O14 11.7(4) . .
C10 N5 N6 O13 -168.8(2) . .
O8 C6 N3 N4 8.4(3) . .
O7 C6 N3 N4 -171.12(19) . .
C6 N3 N4 O9 -26.7(3) . .
C6 N3 N4 O10 155.5(2) . .
O3 C2 N1 N2 -14.9(4) . .
O2 C2 N1 N2 165.5(2) . .
C2 N1 N2 O4 -169.5(2) . .
C2 N1 N2 O5 11.8(3) . .
O12 C10 O11 C9 -1.5(3) . .
N5 C10 O11 C9 178.73(18) . .
Si3 C9 O11 C10 157.47(15) . .
O8 C6 O7 C5 -3.4(3) . .
N3 C6 O7 C5 176.14(17) . .
Si2 C5 O7 C6 -131.14(16) . .
O3 C2 O2 C1 -1.1(3) . .
N1 C2 O2 C1 178.46(18) . .
Si1 C1 O2 C2 151.27(16) . .
Si2 O6A O6B Si3 169.1(8) . .
Si3 O6A O6B Si2 -169.1(8) . .
Si2 O6B Si3 O6A 32(10) . .
O6A O6B Si3 C11 -163(3) . .
Si2 O6B Si3 C11 -131(12) . .
O6A O6B Si3 C12 -44(4) . .
Si2 O6B Si3 C12 -12(14) . .
O6A O6B Si3 C9 86(2) . .
Si2 O6B Si3 C9 118(11) . .
Si2 O6A Si3 O6B -23.2(14) . .
O6B O6A Si3 C11 19(3) . .
Si2 O6A Si3 C11 -5(2) . .
O6B O6A Si3 C12 142(3) . .
Si2 O6A Si3 C12 119.0(19) . .
O6B O6A Si3 C9 -101(3) . .
Si2 O6A Si3 C9 -124.3(17) . .
O11 C9 Si3 O6B 57(3) . .
O11 C9 Si3 O6A 79.9(8) . .
O11 C9 Si3 C11 -44.22(19) . .
O11 C9 Si3 C12 -166.20(15) . .
Si3 O6A Si2 O6B 22.4(13) . .
O6B O6A Si2 C8 168(3) . .
Si3 O6A Si2 C8 -169.3(18) . .
O6B O6A Si2 C7 45(3) . .
Si3 O6A Si2 C7 67.4(17) . .
O6B O6A Si2 C5 -77(3) . .
Si3 O6A Si2 C5 -55(2) . .
Si3 O6B Si2 O6A -33(10) . .
O6A O6B Si2 C8 -14(3) . .
Si3 O6B Si2 C8 -47(12) . .
O6A O6B Si2 C7 -139(2) . .
Si3 O6B Si2 C7 -172(12) . .
O6A O6B Si2 C5 109(3) . .
Si3 O6B Si2 C5 76(13) . .
O7 C5 Si2 O6A -58.1(8) . .
O7 C5 Si2 O6B -80(3) . .
O7 C5 Si2 C8 53.97(18) . .
O7 C5 Si2 C7 176.22(16) . .
Si1 O1 Si1 O1 0.0 3_755 3_755
O1 O1 Si1 C4 5.8(7) 3_755 .
Si1 O1 Si1 C4 5.8(7) 3_755 .
O1 O1 Si1 C3 132.5(6) 3_755 .
Si1 O1 Si1 C3 132.5(6) 3_755 .
O1 O1 Si1 C1 -115.6(6) 3_755 .
Si1 O1 Si1 C1 -115.6(6) 3_755 .
O2 C1 Si1 O1 50.0(2) . 3_755
O2 C1 Si1 O1 81.7(2) . .
O2 C1 Si1 C4 -51.4(2) . .
O2 C1 Si1 C3 -173.12(17) . .
loop_
_iucr_refine_instructions_details
;
TITL tri in P-1                       New: P21/c
CELL  0.71073  25.7850  11.6650   8.7950   90.000   91.258   90.000
ZERR     6.00   0.0000   0.0000   0.0000    0.000    0.000    0.000
LATT   1
SYMM  - X, 1/2 + Y, 1/2 - Z
SFAC  C    N    O    SI   H
UNIT  48   24   54   12   108
MERG   2
OMIT     0   0   2
OMIT    -4   2   4
OMIT    -6   1   2
SHEL 0.8 1000
FMAP   2
PLAN   20
ACTA    50.00
BOND   $H
CONF
L.S.  10
TEMP  -100.00
WGHT    0.038300    0.790900
FVAR       0.21319   0.73808
C5    1    0.374152    0.057824    0.270375    11.00000    0.03811    0.03521 =
         0.03083   -0.00280    0.00586   -0.01013
AFIX  24
H5A   5    0.380801   -0.020721    0.265539    11.00000   -1.20000
H5B   5    0.366677    0.084215    0.172144    11.00000   -1.20000
AFIX   0
C6    1    0.446856    0.182240    0.241563    11.00000    0.02234    0.03016 =
         0.02243   -0.00127    0.00604    0.00498
C9    1    0.298784   -0.065820    0.835973    11.00000    0.04181    0.02627 =
         0.02537    0.00314    0.00198   -0.00840
AFIX  24
H9B   5    0.312157   -0.100557    0.927018    11.00000   -1.20000
H9A   5    0.286259    0.008882    0.860225    11.00000   -1.20000
AFIX   0
C10   1    0.225356   -0.185882    0.865819    11.00000    0.02626    0.02775 =
         0.02267    0.00297    0.00552    0.00445
C1    1    1.036394    0.069100    0.287001    11.00000    0.03643    0.03363 =
         0.03361   -0.00006    0.00271   -0.00723
AFIX  24
H1A   5    1.025405    0.103609    0.381716    11.00000   -1.20000
H1B   5    1.047194   -0.009387    0.307670    11.00000   -1.20000
AFIX   0
C2    1    1.111128    0.186031    0.321797    11.00000    0.02454    0.03544 =
         0.02409    0.00003   -0.00497    0.00545
C8    1    0.311534    0.242456    0.416148    11.00000    0.05064    0.04565 =
         0.05848   -0.01113   -0.00354    0.01109
AFIX 137
H8C   5    0.282505    0.260164    0.482283    11.00000   -1.50000
H8B   5    0.305120    0.276630    0.315695    11.00000   -1.50000
H8A   5    0.343660    0.273888    0.460777    11.00000   -1.50000
AFIX   0
C7    1    0.259418    0.018704    0.311064    11.00000    0.04379    0.06104 =
         0.06755   -0.01240    0.00497   -0.01354
AFIX 137
H7C   5    0.266155   -0.062775    0.292851    11.00000   -1.50000
H7A   5    0.250680    0.056555    0.214378    11.00000   -1.50000
H7B   5    0.230392    0.026597    0.380387    11.00000   -1.50000
AFIX   0
C11   1    0.360651   -0.198447    0.609290    11.00000    0.04818    0.05623 =
         0.08409   -0.02925    0.01804   -0.00241
AFIX 137
H11A  5    0.328281   -0.224561    0.560147    11.00000   -1.50000
H11C  5    0.370785   -0.252099    0.690378    11.00000   -1.50000
H11B  5    0.388036   -0.195093    0.533894    11.00000   -1.50000
AFIX   0
C12   1    0.411180   -0.000340    0.779880    11.00000    0.04344    0.05933 =
         0.05580   -0.00681    0.00445   -0.01148
AFIX 137
H12B  5    0.437391    0.010279    0.702097    11.00000   -1.50000
H12C  5    0.424037   -0.055099    0.856345    11.00000   -1.50000
H12A  5    0.404126    0.073331    0.828833    11.00000   -1.50000
AFIX   0
C4    1    0.970335    0.220106    0.089242    11.00000    0.05813    0.12380 =
         0.14018    0.09300   -0.01868   -0.00349
AFIX 137
H4B   5    1.002850    0.254727    0.056338    11.00000   -1.50000
H4C   5    0.957312    0.262584    0.176636    11.00000   -1.50000
H4A   5    0.944618    0.223003    0.005616    11.00000   -1.50000
AFIX   0
C3    1    0.924526    0.005001    0.227448    11.00000    0.04621    0.07587 =
         0.07747    0.00131   -0.00016   -0.01711
AFIX 137
H3B   5    0.896249    0.002209    0.151245    11.00000   -1.50000
H3A   5    0.913693    0.050626    0.314761    11.00000   -1.50000
H3C   5    0.933010   -0.073002    0.261076    11.00000   -1.50000
AFIX   0
N5    2    0.188551   -0.244500    0.778930    11.00000    0.03439    0.05181 =
         0.01966   -0.00327    0.00753   -0.00998
N6    2    0.155563   -0.325900    0.835000    11.00000    0.02744    0.06171 =
         0.04015   -0.00723    0.00737   -0.01303
N3    2    0.485023    0.235455    0.331041    11.00000    0.02893    0.04566 =
         0.01539   -0.00057    0.00412   -0.00540
N4    2    0.516762    0.320755    0.276990    11.00000    0.02356    0.04948 =
         0.02797   -0.00216    0.00182   -0.00417
N1    2    1.149114    0.239439    0.237697    11.00000    0.03034    0.05635 =
         0.01915    0.00109   -0.00434   -0.00639
N2    2    1.182755    0.321554    0.293950    11.00000    0.02686    0.05635 =
         0.03407    0.00437   -0.00504   -0.00433
O6A   3    0.331920    0.042973    0.568334    21.00000    0.04122    0.03218 =
         0.02824    0.00996    0.00784    0.00009
O11   3    0.256931   -0.135526    0.770205    11.00000    0.03919    0.04141 =
         0.02077    0.00320    0.00577   -0.01185
O12   3    0.228332   -0.181678    1.000969    11.00000    0.04378    0.06518 =
         0.01999    0.00380    0.00413   -0.01972
O13   3    0.132045   -0.380263    0.738039    11.00000    0.05827    0.10994 =
         0.05292   -0.02353    0.00593   -0.04749
O14   3    0.151926   -0.337053    0.971227    11.00000    0.04864    0.08160 =
         0.03519    0.00710    0.00867   -0.02745
O7    3    0.419551    0.118328    0.334495    11.00000    0.03387    0.04590 =
         0.02261    0.00239    0.00704   -0.01036
O8    3    0.440179    0.193204    0.107744    11.00000    0.03629    0.05019 =
         0.01770    0.00327    0.00016   -0.01101
O9    3    0.525722    0.323801    0.142120    11.00000    0.04612    0.08243 =
         0.02432   -0.00139    0.01072   -0.02661
O10   3    0.534714    0.385151    0.373502    11.00000    0.04366    0.06641 =
         0.03800   -0.01222   -0.00076   -0.01968
O1    3    1.000217   -0.035151    0.024540    10.50000    0.05425    0.06117 =
         0.03090   -0.02258   -0.00273   -0.00453
O2    3    1.079428    0.134571    0.224051    11.00000    0.03427    0.05025 =
         0.02250   -0.00216   -0.00418   -0.00906
O3    3    1.107960    0.186073    0.456572    11.00000    0.04461    0.06726 =
         0.02137   -0.00256   -0.00159   -0.01763
O5    3    1.185613    0.337478    0.430512    11.00000    0.04062    0.07206 =
         0.03333   -0.00788   -0.00555   -0.01549
O4    3    1.207889    0.370313    0.198620    11.00000    0.05141    0.09129 =
         0.04670    0.01495    0.00134   -0.03139
O6B   3    0.327268   -0.003379    0.539012   -21.00000    0.05255    0.05534 =
         0.04107    0.02598    0.00465   -0.01250
SI3   4    0.351039   -0.055814    0.690393    11.00000    0.02932    0.03157 =
         0.02666    0.00549    0.00353   -0.00022
SI2   4    0.317770    0.085907    0.396774    11.00000    0.02823    0.03280 =
         0.02570    0.00545    0.00397    0.00060
SI1   4    0.981944    0.070934    0.143576    11.00000    0.02905    0.06370 =
         0.02952   -0.01394    0.00099   -0.00351
H2    5    0.481397    0.243596    0.426318    11.00000    0.03826
H1    5    1.145157    0.242536    0.146558    11.00000    0.03238
H3    5    0.192755   -0.249812    0.689624    11.00000    0.04218
HKLF    4  1.0  0.00  0.00  1.00  0.00 -1.00  0.00  1.00  0.00  0.00
 
REM  tri in P-1                       New: P21/c
REM R1 =  0.0448 for   4021 Fo > 4sig(Fo)  and  0.0690 for all   5376 data
REM    347 parameters refined using      0 restraints
 
END
 
WGHT      0.0383      0.7909
REM Highest difference peak  0.355,  deepest hole -0.291,  1-sigma level  0.049
Q1    1   0.9775  0.1996  0.0102  11.00000  0.05    0.35
Q2    1   0.9821  0.2521  0.1295  11.00000  0.05    0.35
Q3    1   0.3543 -0.1423  0.6820  11.00000  0.05    0.34
Q4    1   0.3190 -0.0657  0.7475  11.00000  0.05    0.33
Q5    1   1.0098  0.0814  0.2127  11.00000  0.05    0.31
Q6    1   0.3166  0.1790  0.4742  11.00000  0.05    0.29
Q7    1   0.3843 -0.0437  0.7608  11.00000  0.05    0.25
Q8    1   0.9539  0.0359  0.1926  11.00000  0.05    0.24
Q9    1   0.1126 -0.3158  0.7450  11.00000  0.05    0.24
Q10   1   0.1406 -0.4007  0.7710  11.00000  0.05    0.23
Q11   1   0.3487  0.0969  0.3432  11.00000  0.05    0.22
Q12   1   0.3600 -0.2746  0.6446  11.00000  0.05    0.21
Q13   1   0.2964  0.0251  0.3392  11.00000  0.05    0.21
Q14   1   0.3881  0.0162  0.7085  11.00000  0.05    0.21
Q15   1   0.1252 -0.4115  0.7358  11.00000  0.05    0.20
Q16   1   0.3290 -0.2525  0.6630  11.00000  0.05    0.19
Q17   1   0.3211  0.2320  0.5248  11.00000  0.05    0.18
Q18   1   0.2309 -0.1336  0.8042  11.00000  0.05    0.18
Q19   1   0.3188 -0.0474  0.5039  11.00000  0.05    0.17
Q20   1   0.4205  0.1438  0.4311  11.00000  0.05    0.16
;
