#------------------------------------------------------------------------------
#$Date: 2019-11-23 08:01:50 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232500 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/77/4347786.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_4347786
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_moiety         'C8 H12 N8 O16 Si'
_chemical_formula_sum            'C8 H12 N8 O16 Si'
_chemical_formula_weight         504.311
_chemical_name_common            sila-PETNC
_chemical_name_systematic        Tetrakis(nitrocarbamoylmethyl)silane
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      114
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date
;
'Wed Nov 04 03:50:47 2015'
;
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.0675(4)
_cell_length_b                   10.0675(4)
_cell_length_c                   9.7196(7)
_cell_measurement_reflns_used    1538
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.5120
_cell_measurement_theta_min      4.5190
_cell_volume                     985.13(9)
_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      173(2)
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -47.00   46.10   0.7000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.4519   57.0000  -60.0000 133

#__ type_ start__ end____ width___ exp.time_
  2 omega  -94.00    0.50   0.7000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.4519  -57.0000  150.0000 135

#__ type_ start__ end____ width___ exp.time_
  3 omega  -25.00   20.50   0.7000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.4519  -99.0000   90.0000 65

#__ type_ start__ end____ width___ exp.time_
  4 omega  -14.00   13.30   0.7000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.4519  -99.0000  -60.0000 39

#__ type_ start__ end____ width___ exp.time_
  5 omega -101.00  -73.00   0.7000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.4519 -179.0000  -60.0000 40

#__ type_ start__ end____ width___ exp.time_
  6 omega   18.00   45.30   0.7000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.4519    0.0000  -90.0000 39

#__ type_ start__ end____ width___ exp.time_
  7 omega  -30.00   98.10   0.7000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       24.5457   19.0000  120.0000 183

;
_diffrn_measurement_device       'CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       omega-scan
_diffrn_orient_matrix_UB_11      0.0535020000
_diffrn_orient_matrix_UB_12      0.0347177000
_diffrn_orient_matrix_UB_13      0.0309097000
_diffrn_orient_matrix_UB_21      0.0377174000
_diffrn_orient_matrix_UB_22      -0.0595246000
_diffrn_orient_matrix_UB_23      0.0016532000
_diffrn_orient_matrix_UB_31      0.0260275000
_diffrn_orient_matrix_UB_32      0.0147889000
_diffrn_orient_matrix_UB_33      -0.0660692000
_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  0.0487
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7794
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         4.19
_diffrn_source_current           40
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.221
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84532
_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    1.7002
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.180
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         1119
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0409
_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)+(0.0506P)²+0.2119P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0938
_refine_ls_wR_factor_ref         0.0997
_reflns_number_gt                957
_reflns_number_total             1119
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic6b00602_si_002.cif
_cod_data_source_block           4b
_cod_database_code               4347786
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'-y, x, -z'
'y, -x, -z'
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
Si1 Si 0.0000 1.0000 0.0000 0.0254(3) Uani 1 4 d S
O1 O -0.07175(17) 0.74496(16) -0.02627(18) 0.0330(4) Uani 1 1 d .
O2 O -0.1290(2) 0.62097(19) -0.21127(18) 0.0386(5) Uani 1 1 d .
O4 O -0.2211(3) 0.38607(19) -0.1244(2) 0.0557(6) Uani 1 1 d .
N2 N -0.2214(2) 0.4337(2) -0.0114(3) 0.0449(6) Uani 1 1 d .
N1 N -0.1537(2) 0.5491(2) 0.0130(3) 0.0336(5) Uani 1 1 d .
C1 C -0.0360(3) 0.8562(2) -0.1156(3) 0.0316(6) Uani 1 1 d .
O3 O -0.2725(4) 0.3850(3) 0.0886(3) 0.0997(13) Uani 1 1 d .
C2 C -0.1197(2) 0.6377(2) -0.0904(2) 0.0292(5) Uani 1 1 d .
H1A H 0.034(3) 0.830(3) -0.170(4) 0.042(8) Uiso 1 1 d .
H1B H -0.108(3) 0.866(3) -0.183(3) 0.031(7) Uiso 1 1 d .
H1 H -0.157(3) 0.578(3) 0.094(3) 0.033(7) 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'
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'
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'
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
C1 Si1 C1 111.20(8) 7_665 .
C1 Si1 C1 106.06(16) 7_665 8_465
C1 Si1 C1 111.20(8) . 8_465
C1 Si1 C1 111.20(8) 7_665 2_575
C1 Si1 C1 106.06(16) . 2_575
C1 Si1 C1 111.20(8) 8_465 2_575
C2 O1 C1 115.50(19) . .
O4 N2 O3 125.3(2) . .
O4 N2 N1 119.8(2) . .
O3 N2 N1 114.8(2) . .
N2 N1 C2 123.0(2) . .
N2 N1 H1 116(2) . .
C2 N1 H1 118(2) . .
O1 C1 Si1 106.51(17) . .
O1 C1 H1A 108(2) . .
Si1 C1 H1A 115(2) . .
O1 C1 H1B 107.0(16) . .
Si1 C1 H1B 117.6(17) . .
H1A C1 H1B 102(2) . .
O2 C2 O1 127.1(2) . .
O2 C2 N1 127.2(2) . .
O1 C2 N1 105.70(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 C1 1.868(3) 7_665
Si1 C1 1.868(3) .
Si1 C1 1.868(3) 8_465
Si1 C1 1.868(3) 2_575
O1 C2 1.337(3) .
O1 C1 1.462(3) .
O2 C2 1.190(3) .
O4 N2 1.199(3) .
N2 O3 1.203(3) .
N2 N1 1.367(3) .
N1 C2 1.387(3) .
N1 H1 0.84(3) .
C1 H1A 0.92(3) .
C1 H1B 0.98(3) .
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
O4 N2 N1 C2 21.4(4) .
O3 N2 N1 C2 -162.0(3) .
C2 O1 C1 Si1 170.72(16) .
C1 Si1 C1 O1 62.2(2) 7_665
C1 Si1 C1 O1 -55.8(2) 8_465
C1 Si1 C1 O1 -176.8(2) 2_575
C1 O1 C2 O2 4.5(4) .
C1 O1 C2 N1 -176.65(19) .
N2 N1 C2 O2 -9.4(4) .
N2 N1 C2 O1 171.7(2) .
loop_
_iucr_refine_instructions_details
;
TITL kx414_P42(1)c in P-42(1)c
CELL  0.71073  10.0675  10.0675   9.7196   90.000   90.000   90.000
ZERR     2.00   0.0004   0.0004   0.0007    0.000    0.000    0.000
LATT  -1
SYMM  - X, - Y,   Z
SYMM  1/2 + X, 1/2 - Y, 1/2 - Z
SYMM  1/2 - X, 1/2 + Y, 1/2 - Z
SYMM  1/2 + Y, 1/2 + X, 1/2 + Z
SYMM  1/2 - Y, 1/2 - X, 1/2 + Z
SYMM  - Y,   X, - Z
SYMM    Y, - X, - Z
SFAC  C    H    N    O    SI
UNIT  16   24   16   32   2
MERG   2
OMIT     0   2   2
OMIT     0   2   1
OMIT     0   1   3
OMIT     0   3   0
OMIT     0   3   1
OMIT     1   2   3
OMIT     0   1   7
OMIT    -1   2   3
OMIT     0   1   5
OMIT    -1   1  10
OMIT     0   4   3
SHEL 0.77 1000
FMAP   2
PLAN   25
ACTA
HTAB
BOND   $H
CONF
L.S.  10
TEMP  -100.00
WGHT    0.050600    0.211900
FVAR       0.32402
Si1  5    0.000000    1.000000    0.000000    10.25000    0.02411    0.02411 =
         0.02794    0.00000    0.00000    0.00000
O1    4   -0.071752    0.744959   -0.026266    11.00000    0.04396    0.02702 =
         0.02787   -0.00033   -0.00016   -0.00941
O2    4   -0.129013    0.620966   -0.211275    11.00000    0.04868    0.03902 =
         0.02822   -0.00257    0.00266   -0.00822
O4    4   -0.221052    0.386071   -0.124381    11.00000    0.08725    0.04030 =
         0.03958   -0.01258    0.00318   -0.01589
N2    3   -0.221423    0.433730   -0.011358    11.00000    0.06277    0.03381 =
         0.03816   -0.00498    0.00191   -0.01548
N1    3   -0.153691    0.549085    0.012990    11.00000    0.04383    0.02892 =
         0.02797   -0.00398   -0.00268   -0.00646
C1    1   -0.035953    0.856151   -0.115595    11.00000    0.03709    0.02797 =
         0.02967    0.00094    0.00174   -0.00501
O3    4   -0.272488    0.385023    0.088560    11.00000    0.18367    0.07001 =
         0.04550   -0.01400    0.03449   -0.07796
C2    1   -0.119684    0.637681   -0.090420    11.00000    0.02732    0.03066 =
         0.02958   -0.00144   -0.00236   -0.00102
H1A    2    0.034036    0.829520   -0.170445    11.00000    0.04239
H1B    2   -0.107855    0.866237   -0.182531    11.00000    0.03131
H1    2   -0.157065    0.577697    0.093562    11.00000    0.03268
HKLF    4
 
REM  kx414_P42(1)c in P-42(1)c
REM R1 =  0.0409 for    957 Fo > 4sig(Fo)  and  0.0514 for all   1119 data
REM     87 parameters refined using      0 restraints
 
END
 
WGHT      0.0508      0.2076
REM Highest difference peak  0.317,  deepest hole -0.180,  1-sigma level  0.049
Q1    1  -0.4484  0.4895  0.0111  11.00000  0.05    0.32
Q2    1  -0.1923  0.3767  0.0668  11.00000  0.05    0.20
Q3    1  -0.1903  0.4784 -0.1381  11.00000  0.05    0.19
Q4    1  -0.3189  0.4409  0.0438  11.00000  0.05    0.18
Q5    1  -0.1629  0.6935 -0.0039  11.00000  0.05    0.16
Q6    1  -0.2934  0.4409 -0.1158  11.00000  0.05    0.16
Q7    1  -0.1741  0.4572 -0.0071  11.00000  0.05    0.15
Q8    1  -0.0311  0.7007 -0.1059  11.00000  0.05    0.15
Q9    1  -0.2441  0.3746  0.1221  11.00000  0.05    0.15
Q10   1  -0.1163  0.7206 -0.0630  11.00000  0.05    0.14
Q11   1  -0.0858  0.6060 -0.1557  11.00000  0.05    0.14
Q12   1  -0.2684  0.2664 -0.0002  11.00000  0.05    0.14
Q13   1  -0.0581  1.0353  0.0304  11.00000  0.05    0.14
Q14   1  -0.0675  0.7074 -0.0198  11.00000  0.05    0.13
Q15   1   0.0062  0.6911  0.0417  11.00000  0.05    0.13
Q16   1   0.0177  0.9356 -0.0835  11.00000  0.05    0.12
Q17   1   0.0037  0.9077 -0.0467  11.00000  0.05    0.12
Q18   1  -0.0491  0.8071 -0.0858  11.00000  0.05    0.12
Q19   1   0.0093  0.6867 -0.0404  11.00000  0.05    0.12
Q20   1  -0.0743  1.0031 -0.2746  11.00000  0.05    0.12
Q21   1  -0.1889  0.3747 -0.0626  11.00000  0.05    0.12
Q22   1  -0.0671  0.8184 -0.2058  11.00000  0.05    0.12
Q23   1   0.0755  0.7445  0.0159  11.00000  0.05    0.11
Q24   1  -0.0628  0.5108  0.0034  11.00000  0.05    0.11
Q25   1  -0.0551  0.6521 -0.2530  11.00000  0.05    0.11
;
