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_4347787
_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
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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      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
;
  1 omega   58.00  100.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   57.0000  -60.0000 42

  2 omega   37.00  109.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  179.0000  -60.0000 72

  3 omega  -11.00   74.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000    0.0000 85

  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 \k-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/[\s^2^(Fo^2^)+(0.0383P)^2^+0.7909P] where P=(Fo^2^+2Fc^2^)/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     >2\s(I)
_cod_data_source_file            ic6b00602_si_002.cif
_cod_data_source_block           5
_cod_database_code               4347787
loop_