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_7712340
_publ_section_title
;
 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         'C24 H45 B N7 O S Si2 Y'
_chemical_formula_sum            'C24 H45 B N7 O S Si2 Y'
_chemical_formula_weight         635.63
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2022-09-26 deposited with the CCDC.	2023-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.192(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0031(3)
_cell_length_b                   22.2150(8)
_cell_length_c                   14.0346(7)
_cell_measurement_reflns_used    1996
_cell_measurement_temperature    173.01
_cell_volume                     3259.1(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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.01
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.5056
_diffrn_reflns_av_unetI/netI     0.1461
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            60567
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         68.734
_diffrn_reflns_theta_min         3.363
_diffrn_source_current           2.86
_diffrn_source_power             0.1999426
_diffrn_source_voltage           69.91
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.690
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5996
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.734
_refine_diff_density_min         -2.711
_refine_diff_density_rms         0.267
_refine_ls_extinction_coef       0.0296(13)
_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   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         9130
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0854
_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^)+(0.1319P)^2^+1.3605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1976
_refine_ls_wR_factor_ref         0.2134
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8042
_reflns_number_total             9130
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00149k2.cif
_cod_data_source_block           ga_210727c
_cod_database_code               7712340
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.877
_shelx_estimated_absorpt_t_min   0.721
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 B1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C17(H17a,H17b), C18(H18a,H18b), C16(H16a,H16b), C19(H19a,H19b)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C8(H8), C3(H3)
2.d Idealised Me refined as rotating group:
 C6(H6a,H6b,H6c), C10(H10a,H10b,H10c), C11(H11a,H11b,H11c), C22(H22a,H22b,
 H22c), C15(H15a,H15b,H15c), C1(H1a,H1b,H1c), C23(H23a,H23b,H23c), C5(H5a,H5b,
 H5c), C21(H21a,H21b,H21c), C20(H20a,H20b,H20c), C24(H24a,H24b,H24c)
;
_shelx_res_checksum              90045
_olex2_submission_special_instructions 'No special instructions were received'