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_7712341
_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         'C39 H60 B N8 O Si3 Y'
_chemical_formula_sum            'C39 H60 B N8 O Si3 Y'
_chemical_formula_weight         840.94
_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                100.208(2)
_cell_angle_beta                 90.122(2)
_cell_angle_gamma                95.118(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8288(6)
_cell_length_b                   10.6314(6)
_cell_length_c                   21.1115(12)
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    172.99
_cell_volume                     2162.1(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      172.99
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f 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  0.0593
_diffrn_reflns_av_unetI/netI     0.0540
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30186
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         56.367
_diffrn_reflns_theta_min         3.691
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           2.86
_diffrn_source_power             0.199914
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           69.9
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.993
_exptl_absorpt_correction_T_max  0.7510
_exptl_absorpt_correction_T_min  0.4838
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_description       rod
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.320
_refine_diff_density_min         -1.383
_refine_diff_density_rms         0.205
_refine_ls_extinction_coef       0.0048(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   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         8489
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0570
_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^)+(0.1221P)^2^+2.3351P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1785
_refine_ls_wR_factor_ref         0.1852
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7562
_reflns_number_total             8489
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00149k2.cif
_cod_data_source_block           ga_210430c
_cod_database_code               7712341
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.715
_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 Si(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C21(H21), B1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C00Y(H00A,H00B), C014(H01A,H01B), C018(H01C,H01D), C01H(H01E,
 H01F)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C13(H13), C8(H8), C26(H26), C27(H27), C25(H25), C29(H29), C31(H31),
 C28(H28), C35(H35), C33(H33), C34(H34), C32(H32)
2.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C1(H1A,H1B,H1C), C6(H6A,H6B,H6C), C11(H11A,H11B,H11C),
 C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C10(H10A,H10B,H10C), C5(H5A,H5B,H5C),
  C18(H18A,H18B,H18C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C)
;
_olex2_submission_special_instructions 'No special instructions were received'