Crystal structure of 1,3,5-tris((trimethylsilyl)methyl)-1,3,5-triazinane-2,4,6-trione, C15H33N3O3Si3
Tong, Ya-Yan; Xu, Bo; Yin, Guang-Da; Song, Rong-Fei; Guo, Li-Bing; Zhao, Pei-Zheng; Zeitschrift für Kristallographie - New Crystal Structures 233 (2018) 147–148; doi:10.1515/ncrs-2017-0236

data_8106079
_publ_section_title
;
 Crystal structure of
 1,3,5-tris((trimethylsilyl)methyl)-1,3,5-triazinane-2,4,6-trione,
 C15H33N3O3Si3
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              147
_journal_page_last               148
_journal_paper_doi               10.1515/ncrs-2017-0236
_journal_volume                  233
_journal_year                    2018
_chemical_formula_moiety         'C5 H11 N O Si'
_chemical_formula_sum            'C5 H11 N O Si'
_chemical_formula_weight         129.23
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_Int_Tables_number      148
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   17.8622(4)
_cell_length_b                   17.8622(4)
_cell_length_c                   12.5153(3)
_cell_measurement_reflns_used    2802
_cell_measurement_temperature    293
_cell_measurement_theta_max      72.2400
_cell_measurement_theta_min      6.7080
_cell_volume                     3458.13(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0528
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.9797
_diffrn_measured_fraction_theta_max 0.9797
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     24.00  81.00   1.00    2.03    --   36.07  38.00  30.00   57
  2  \w     42.00  96.00   1.00    2.03    --   36.07  57.00  90.00   54
  3  \w    135.00 174.00   1.00    8.11    --  109.31  77.00  30.00   39
  4  \w     92.00 118.00   1.00    8.11    --  109.31  77.00  30.00   26
  5  \w     71.00 178.00   1.00    8.11    --  109.31  15.00  30.00  107
  6  \w     84.00 127.00   1.00    8.11    --  109.31 -61.00 -90.00   43
  7  \w    103.00 131.00   1.00    8.11    --  109.31 -30.00-180.00   28
  8  \w     63.00  93.00   1.00    8.11    --  109.31 -30.00-180.00   30
  9  \w     55.00 109.00   1.00    8.11    --  109.31 -95.00 -90.00   54
 10  \w     45.00 101.00   1.00    8.11    --  109.31 -45.00-120.00   56
 11  \w     48.00  88.00   1.00    2.03    --   36.07-125.00-120.00   40
 12  \w     26.00  58.00   1.00    2.03    --   36.07-125.00  90.00   32
 13  \w     61.00  86.00   1.00    2.03    --   36.07-125.00  90.00   25
 14  \w     34.00  75.00   1.00    2.03    --   36.07 -99.00 150.00   41
 15  \w    -30.00  -1.00   1.00    2.03    --   36.07 -57.00 -90.00   29
 16  \w    -30.00  47.00   1.00    2.03    --   36.07 -38.00-180.00   77
 17  \w     67.00 150.00   1.00    8.11    --  109.31 178.00 150.00   83
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0244179333
_diffrn_orient_matrix_UB_12      0.0927936667
_diffrn_orient_matrix_UB_13      -0.0316596333
_diffrn_orient_matrix_UB_21      0.0828388667
_diffrn_orient_matrix_UB_22      0.0120919333
_diffrn_orient_matrix_UB_23      -0.0541656667
_diffrn_orient_matrix_UB_31      -0.0495718000
_diffrn_orient_matrix_UB_32      -0.0338949000
_diffrn_orient_matrix_UB_33      -0.1059375000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4196
_diffrn_reflns_theta_full        72.3880
_diffrn_reflns_theta_max         72.39
_diffrn_reflns_theta_min         4.54
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.032
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25033
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.1169
_exptl_crystal_description       prism
_exptl_crystal_F_000             1267.6452
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.2840
_refine_diff_density_min         -0.6377
_refine_diff_density_rms         0.1324
_refine_ls_d_res_high            0.8088
_refine_ls_d_res_low             9.7297
_refine_ls_goodness_of_fit_ref   1.0308
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    15
_refine_ls_number_parameters     76
_refine_ls_number_reflns         1493
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0308
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0689
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1307P)^2^+2.4991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1808
_refine_ls_wR_factor_ref         0.1876
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              18
_reflns_limit_h_min              0
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              -15
_reflns_number_gt                1340
_reflns_number_total             1493
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            suppl_ncrs-2017-0236_suppl.cif
_cod_data_source_block           xxxxSi
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               8106079
_chemical_oxdiff_formula         'C1 O1 H1 N1 Si1'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H3a,H3b)
2.b Idealised Me refined as rotating group:
 C7(H7a,H7b,H7c), C5(H5a,H5b,H5c), C6(H6a,H6b,H6c)
;
_olex2_date_sample_data_collection 2017-08-02
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.792
_oxdiff_exptl_absorpt_empirical_full_min 0.471