Selective Si−C(sp3) Bond Cleavage of Silyl−Bridged Amido Alkyl Ligand in an Yttrium Complex
Cai, Jiamin; Zhang, Jie; Zhou, Xigeng; Dalton Transactions  (2023) –; doi:10.1039/D3DT00149K

data_7712336
_publ_section_title
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 Selective Si&#x2212;C(sp3) Bond Cleavage of Silyl&#x2212;Bridged Amido
 Alkyl Ligand in an Yttrium Complex
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00149K
_journal_year                    2023
_chemical_formula_moiety         'C38 H58 B N8 O Si3 Y, [+ solvents]'
_chemical_formula_sum            'C38 H58 B N8 O Si3 Y'
_chemical_formula_weight         826.91
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-09-26 deposited with the CCDC.	2023-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                87.551(2)
_cell_angle_beta                 82.318(2)
_cell_angle_gamma                84.784(2)
_cell_formula_units_Z            2
_cell_length_a                   9.7167(6)
_cell_length_b                   10.5316(7)
_cell_length_c                   22.2080(13)
_cell_measurement_reflns_used    9637
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      53
_cell_measurement_theta_min      3
_cell_volume                     2241.8(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            67949
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        52.995
_diffrn_reflns_theta_max         52.995
_diffrn_reflns_theta_min         3.496
_diffrn_source_current           2.86
_diffrn_source_power             0.1999426
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           69.91
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.917
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.6035
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1375 before and 0.0694 after correction.
The Ratio of minimum to maximum transmission is 0.8030.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.763
_refine_diff_density_rms         0.202
_refine_ls_extinction_coef       0.0113(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.229
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         7944
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.229
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0701P)^2^+1.7792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1118
_refine_ls_wR_factor_ref         0.1253
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7706
_reflns_number_total             7944
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00149k2.cif
_cod_data_source_block           ga_210123a_a
_cod_database_code               7712336
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.910
_shelx_estimated_absorpt_t_min   0.606
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups,
  All Si(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H16C)=Sof(H16D)=Sof(C17B)=Sof(H17C)=Sof(H17D)=1-FVAR(1)
 Sof(H16A)=Sof(H16B)=Sof(C17A)=Sof(H17A)=Sof(H17B)=FVAR(1)
 Sof(C18B)=Sof(H18C)=Sof(H18D)=Sof(H19C)=Sof(H19D)=1-FVAR(2)
 Sof(C18A)=Sof(H18A)=Sof(H18B)=Sof(H19A)=Sof(H19B)=FVAR(2)
3.a Ternary CH refined with riding coordinates:
 C25(H25), B1(H1)
3.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C16(H16C,H16D), C17A(H17A,H17B), C17B(H17C,H17D), C18A(H18A,
 H18B), C18B(H18C,H18D), C19(H19A,H19B), C19(H19C,H19D)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C13(H13), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
 C34(H34), C35(H35), C36(H36), C37(H37), C38(H38)
3.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'