Energetic Sila-Nitrocarbamates: Silicon Analogues of Neo-Pentane Derivatives.
Axthammer, Quirin J.; Klapötke, Thomas M; Krumm, Burkhard; Reith, Thomas; Inorganic chemistry 55 (2016) 4683–4692; doi:10.1021/acs.inorgchem.6b00602

data_4347786
_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
;
_computing_publication_material
;PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version).
;
_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
;
  1 omega  -47.00   46.10   0.7000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.4519   57.0000  -60.0000 133

  2 omega  -94.00    0.50   0.7000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.4519  -57.0000  150.0000 135

  3 omega  -25.00   20.50   0.7000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.4519  -99.0000   90.0000 65

  4 omega  -14.00   13.30   0.7000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.4519  -99.0000  -60.0000 39

  5 omega -101.00  -73.00   0.7000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.4519 -179.0000  -60.0000 40

  6 omega   18.00   45.30   0.7000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.4519    0.0000  -90.0000 39

  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 \k-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/[\s^2^(Fo^2^)+(0.0506P)^2^+0.2119P] where P=(Fo^2^+2Fc^2^)/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     >2\s(I)
_cod_data_source_file            ic6b00602_si_002.cif
_cod_data_source_block           4b
_cod_database_code               4347786
loop_