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_7712337
_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         'C48 H60 B N10 Si3 Y'
_chemical_formula_sum            'C48 H60 B N10 Si3 Y'
_chemical_formula_weight         961.05
_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             2022-09-20
_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                91.3010(10)
_cell_angle_beta                 97.5760(10)
_cell_angle_gamma                95.7210(10)
_cell_formula_units_Z            2
_cell_length_a                   10.2029(4)
_cell_length_b                   10.7900(4)
_cell_length_c                   23.0484(7)
_cell_measurement_reflns_used    4741
_cell_measurement_temperature    172.99
_cell_measurement_theta_max      44.64
_cell_measurement_theta_min      3.58
_cell_volume                     2501.05(16)
_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      172.99
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0702
_diffrn_reflns_av_unetI/netI     0.0691
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20829
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        44.941
_diffrn_reflns_theta_max         44.941
_diffrn_reflns_theta_min         3.584
_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    1.766
_exptl_absorpt_correction_T_max  0.7489
_exptl_absorpt_correction_T_min  0.6332
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0925 before and 0.0620 after correction.
The Ratio of minimum to maximum transmission is 0.8455.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_description       Block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.00110(12)
_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   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         6118
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0266P)^2^+2.1266P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0911
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4778
_reflns_number_total             6118
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00149k2.cif
_cod_data_source_block           ga_210702i
_cod_database_code               7712337
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.933
_shelx_estimated_absorpt_t_min   0.872
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All Si(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 B1(H1c)
2.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C6(H6), C7(H7), C29(H29), C34(H34), C1(H1), C20(H20), C9(H9),
 C15(H15), C8(H8), C39(H39), C4(H4), C17(H17), C11(H11), C19(H19), C14(H14),
 C44(H44), C18(H18), C12(H12), C13(H13), C48(H48), C46(H46), C45(H45), C47(H47)
2.c Idealised Me refined as rotating group:
 C31(H31a,H31b,H31c), C27(H27a,H27b,H27c), C36(H36a,H36b,H36c), C41(H41a,H41b,
 H41c), C32(H32a,H32b,H32c), C23(H23a,H23b,H23c), C22(H22a,H22b,H22c), C37(H37a,
 H37b,H37c), C26(H26a,H26b,H26c), C25(H25a,H25b,H25c), C24(H24a,H24b,H24c)
;
_shelx_res_checksum              5283
_olex2_submission_special_instructions 'No special instructions were received'