Base-stabilized silaimine and its donor-free dimer derived from the reaction of NHC-supported silylene with SiCl4.
Cui, Haiyan; Cui, Chunming; Dalton transactions (Cambridge, England : 2003) 44 (2015) 20326–20329; doi:10.1039/c5dt03917g

data_7037057
_publ_section_title
;
 Base-stabilized silaimine and its donor-free dimer derived from the
 reaction of NHC-supported silylene with SiCl4.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              20326
_journal_page_last               20329
_journal_paper_doi               10.1039/c5dt03917g
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C23 H37 Cl2 N3 Si, C7 H8'
_chemical_formula_sum            'C30 H45 Cl2 N3 Si'
_chemical_formula_weight         546.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-10-25
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-10-26 deposited with the CCDC.
2015-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.321(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.490(4)
_cell_length_b                   14.842(6)
_cell_length_c                   21.882(9)
_cell_measurement_reflns_used    9391
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      1.7
_cell_volume                     3081(2)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      113
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
scan:
    Number of images: 180
               Slice: -110.0000 - 70.0000
         Image width: 1.0000
            Exp time: 20.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 44.9835
              2theta: -19.9948
scan:
    Number of images: 140
               Slice: -110.0000 - 30.0000
         Image width: 1.0000
            Exp time: 20.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 44.9835
              2theta: -19.9948
scan:
    Number of images: 75
               Slice: -110.0000 - -35.0000
         Image width: 1.0000
            Exp time: 20.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 44.9835
              2theta: -19.9948
;
_diffrn_measurement_device
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.029407
_diffrn_orient_matrix_UB_12      0.066919
_diffrn_orient_matrix_UB_13      -0.075942
_diffrn_orient_matrix_UB_21      -0.061404
_diffrn_orient_matrix_UB_22      -0.027730
_diffrn_orient_matrix_UB_23      -0.000658
_diffrn_orient_matrix_UB_31      -0.014128
_diffrn_orient_matrix_UB_32      0.030551
_diffrn_orient_matrix_UB_33      0.030929
_diffrn_radiation_monochromator  Multilayer
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0749
_diffrn_reflns_av_unetI/netI     0.0659
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            23056
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.007
_diffrn_reflns_theta_max         25.007
_diffrn_reflns_theta_min         1.658
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.272
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.741
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5427
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0656
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0980P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1669
_refine_ls_wR_factor_ref         0.1781
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4578
_reflns_number_total             5427
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03917g2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7037056--7037057.cif.
;
_cod_database_code               7037057
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: C24(0.5) C25(0.5) H25(0.5) C26(0.5) H26(0.5) C27(0.5) H27(0.5)
 C28(0.5) H28(0.5) C29(0.5) H29(0.5) C30(0.5) H30A(0.5) H30B(0.5) H30C(0.5)
 C32(0.5) H32(0.5) C31(0.5) C36(0.5) H36(0.5) C35(0.5) H35(0.5) C34(0.5)
 H34(0.5) C33(0.5) H33(0.5) C37(0.5) H37A(0.5) H37B(0.5) H37C(0.5)
4.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C16(H16), C21(H21)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29),
 C32(H32), C36(H36), C35(H35), C34(H34), C33(H33)
4.c Fitted hexagon refined as free rotating group:
 C32(C31,C36,C35,C34,C33)
4.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C30(H30A,H30B,H30C), C37(H37A,
 H37B,H37C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'