NHC-stabilized 1-hydrosilaimine: synthesis, structure and reactivity
Dhara, Debabrata; Vijayakanth, Thangavel; Barman, Milan Kr.; Naik, Khevath Praveen Kumar; Chrysochos, Nicolas; Yildiz, Cem B.; Boomishankar, Ramamoorthy; Schulzke, Carola; Chandrasekhar, Vadapalli; Jana, Anukul; Chem. Commun.  (2017) –; doi:10.1039/C7CC03912C

data_7120477
_publ_section_title
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 NHC-stabilized 1-hydrosilaimine: synthesis, structure and reactivity
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC03912C
_journal_year                    2017
_chemical_formula_moiety         'C48 H68 N O Si, C7 H13 N2'
_chemical_formula_sum            'C55 H81 N3 O Si'
_chemical_formula_weight         828.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-02-23
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-04-05 deposited with the CCDC.
2017-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.470(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.730(6)
_cell_length_b                   17.458(8)
_cell_length_c                   24.128(10)
_cell_measurement_reflns_used    7237
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.62
_cell_measurement_theta_min      2.33
_cell_volume                     6203(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1534
_diffrn_reflns_av_unetI/netI     0.1416
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            108845
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.584
_diffrn_reflns_theta_min         1.383
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.887
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       0.0039(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         15682
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1841
_refine_ls_R_factor_gt           0.0731
_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^)+(0.1135P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1926
_refine_ls_wR_factor_ref         0.2444
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6732
_reflns_number_total             15682
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc03912c2.cif
_cod_data_source_block           platon_sq
_cod_original_cell_volume        6202(5)
_cod_database_code               7120477
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All Si(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C36I) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
3.a Ternary CH refined with riding coordinates:
 Si1(H1), C22I(H22I), C11I(H11I), C28I(H28I), C31I(H31I), C37I(H37I),
 C14I(H14I), C25I(H25I), C34I(H34I)
3.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C1(H1A), C24(H24), C25(H25), C14(H14), C15(H15), C13(H13),
 C26P(H26P), C24P(H24P), C32P(H32P), C30P(H30P)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C12I(H12A,H12B,H12C), C4(H4A,H4B,H4C), C30I(H30A,H30B,H30C),
 C29I(H29A,H29B,H29C), C6(H6A,H6B,H6C), C5(H5A,H5B,H5C), C39I(H39A,H39B,H39C),
 C24I(H24A,H24B,H24C), C23I(H23A,H23B,H23C), C35I(H35A,H35B,H35C), C33I(H33A,
 H33B,H33C), C32I(H32A,H32B,H32C), C15I(H15A,H15B,H15C), C38I(H38A,H38B,H38C),
 C27I(H27A,H27B,H27C), C16I(H16A,H16B,H16C), C36I(H36A,H36B,H36C), C26I(H26A,
 H26B,H26C), C13I(H13A,H13B,H13C)
;
_shelx_res_checksum              53400
_shelx_hkl_checksum              34970
_shelx_fab_checksum              14341
_olex2_submission_special_instructions 'No special instructions were received'