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_4347782
_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         'C7 H15 N3 O6 Si, C4 H8 O2'
_chemical_formula_sum            'C11 H23 N3 O8 Si'
_chemical_formula_weight         353.41
_chemical_name_common
'(methylsilanetriyl)tris(methylene) tricarbamate'
_chemical_name_systematic
'(methylsilanetriyl)tris(methylene) tricarbamate'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date
;
'Thu Apr 02 16:59:49 2015'
;
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.236(5)
_cell_angle_beta                 109.668(6)
_cell_angle_gamma                119.019(7)
_cell_formula_units_Z            2
_cell_length_a                   9.8851(6)
_cell_length_b                   9.8992(7)
_cell_length_c                   11.3628(7)
_cell_measurement_reflns_used    1853
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.7900
_cell_measurement_theta_min      4.5700
_cell_volume                     870.75(14)
_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
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
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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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega  -43.00   40.20   0.8000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       25.3533  -57.0000   30.0000 104

  2 omega  -12.00   19.20   0.8000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.2596  -99.0000  150.0000 39

  3 omega  -23.00   56.20   0.8000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       25.3533  -99.0000  -90.0000 99

  4 omega  -47.00   49.00   0.8000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       25.3533  -77.0000  120.0000 120

  5 omega  -88.00    3.20   0.8000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.2596  -77.0000  -30.0000 114

  6 omega   49.00   94.60   0.8000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       25.3533   57.0000 -180.0000 57

;
_diffrn_measurement_device       'CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       omega-scan
_diffrn_orient_matrix_UB_11      0.0755739000
_diffrn_orient_matrix_UB_12      0.0365768000
_diffrn_orient_matrix_UB_13      0.0599357000
_diffrn_orient_matrix_UB_21      0.0494678000
_diffrn_orient_matrix_UB_22      0.0113813000
_diffrn_orient_matrix_UB_23      -0.0355729000
_diffrn_orient_matrix_UB_31      0.0129203000
_diffrn_orient_matrix_UB_32      0.0771743000
_diffrn_orient_matrix_UB_33      0.0008938000
_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  0.0243
_diffrn_reflns_av_sigmaI/netI    0.0569
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6440
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         4.34
_diffrn_source_current           40
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.177
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98591
_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    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         3550
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0308P)^2^+0.0266P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0999
_reflns_number_gt                2771
_reflns_number_total             3550
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic6b00602_si_002.cif
_cod_data_source_block           3a
_cod_original_cell_volume        870.75(13)
_cod_database_code               4347782
loop_