Nitrile formation via dichlorocarbene insertion into the Si-N bond of Ln(III) bis(trimethylsilyl)amide complexes
Li, Yangjuan; Gong, Yu; Chemical Communications  (2022) –; doi:10.1039/D2CC04538A

data_7130878
_publ_section_title
;
 Nitrile formation via dichlorocarbene insertion into the Si-N bond of
 Ln(III) bis(trimethylsilyl)amide complexes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04538A
_journal_year                    2022
_chemical_formula_moiety         'C26 H72 N5 Si8 Yb'
_chemical_formula_sum            'C26 H72 N5 Si8 Yb'
_chemical_formula_weight         852.64
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      tetragonal
_space_group_IT_number           110
_space_group_name_Hall           'I 4bw -2c'
_space_group_name_H-M_alt        'I 41 c d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-17
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-01-27 deposited with the CCDC.	2022-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.0586(3)
_cell_length_b                   20.0586(3)
_cell_length_c                   23.4376(5)
_cell_measurement_reflns_used    8829
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      30.9040
_cell_measurement_theta_min      2.2490
_cell_volume                     9430.1(3)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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    -36.00  34.00   0.50    1.00    --    4.55 -92.00  44.00  140
  2  \w    -18.00  27.00   0.50    1.00    --   -6.43 -99.00-120.00   90
  3  \w    -82.00 -30.00   0.50    1.00    --   -6.43 -19.00 -60.00  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0160714000
_diffrn_orient_matrix_UB_12      -0.0060313000
_diffrn_orient_matrix_UB_13      0.0264742000
_diffrn_orient_matrix_UB_21      -0.0098294000
_diffrn_orient_matrix_UB_22      0.0319823000
_diffrn_orient_matrix_UB_23      0.0097249000
_diffrn_orient_matrix_UB_31      -0.0299368000
_diffrn_orient_matrix_UB_32      -0.0137696000
_diffrn_orient_matrix_UB_33      0.0110021000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            24214
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         2.031
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.208
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_description       block
_exptl_crystal_F_000             3560
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 1507 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.020(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         4540
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0225
_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^)+(0.0249P)^2^+11.8588P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0556
_refine_ls_wR_factor_ref         0.0611
_reflns_Friedel_coverage         0.837
_reflns_Friedel_fraction_full    0.909
_reflns_Friedel_fraction_max     0.883
_reflns_number_gt                3736
_reflns_number_total             4540
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04538a2.cif
_cod_data_source_block           yj-575-3_auto
_cod_database_code               7130878
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Yb1Li1C1Si1N1Cl1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H11A,H11B,H11C} of C11, {H9A,H9B,H9C} of C9
 At 1.5 times of:
  {H10A,H10B,H10C} of C10, {H8A,H8B,H8C} of C8, {H6A,H6B,H6C} of C6, {H5A,H5B,
  H5C} of C5, {H2A,H2B,H2C} of C2, {H4A,H4B,H4C} of C4, {H13A,H13B,H13C} of C13,
   {H3A,H3B,H3C} of C3, {H12A,H12B,H12C} of C12, {H7A,H7B,H7C} of C7
2.a Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C4(H4A,H4B,H4C), C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C12(H12A,
 H12B,H12C), C7(H7A,H7B,H7C), C13(H13A,H13B,H13C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              76021
_shelx_hkl_checksum              84773
_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 1.494
_oxdiff_exptl_absorpt_empirical_full_min 0.721