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_7712339
_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         'C40 H62 B N8 O2 Si3 Y'
_chemical_formula_sum            'C40 H62 B N8 O2 Si3 Y'
_chemical_formula_weight         870.96
_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             2022-09-24
_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                98.8250(10)
_cell_angle_beta                 92.4230(10)
_cell_angle_gamma                96.4810(10)
_cell_formula_units_Z            2
_cell_length_a                   9.7543(3)
_cell_length_b                   10.6068(3)
_cell_length_c                   22.0190(7)
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      51.286
_cell_measurement_theta_min      3.836
_cell_volume                     2232.65(12)
_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      173.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0692
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_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       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27407
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        51.374
_diffrn_reflns_theta_max         51.374
_diffrn_reflns_theta_min         3.836
_diffrn_source                   'microfocus sealed X-ray tube'
_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    1.953
_exptl_absorpt_correction_T_max  0.7501
_exptl_absorpt_correction_T_min  0.2934
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.288
_refine_diff_density_min         -0.875
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         7355
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0842P)^2^+0.6425P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1362
_refine_ls_wR_factor_ref         0.1429
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6303
_reflns_number_total             7355
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00149k2.cif
_cod_data_source_block           ga_220227a
_cod_database_code               7712339
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.875
_shelx_estimated_absorpt_t_min   0.673
_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:
 C26(H26), B1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C33(H33a,H33b), C19(H19a,H19b), C17(H17a,H17b), C16(H16a,H16b), C18(H18a,H18b)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C13(H13), C39(H39), C28(H28), C32(H32), C35(H35), C38(H38),
 C29(H29), C36(H36), C31(H31), C30(H30)
2.d Idealised Me refined as rotating group:
 C5(H5a,H5b,H5c), C21(H21a,H21b,H21c), C23(H23a,H23b,H23c), C10(H10a,H10b,
 H10c), C1(H1c,H1d,H1e), C6(H6a,H6b,H6c), C15(H15a,H15b,H15c), C24(H24a,H24b,
 H24c), C11(H11a,H11b,H11c), C22(H22a,H22b,H22c), C20(H20a,H20b,H20c), C40(H40a,
 H40b,H40c)
;
_shelx_res_checksum              13089
_olex2_submission_special_instructions 'No special instructions were received'