β-SiH-Containing Tris(silazido) Rare-Earth Complexes as Homogeneous and Grafted Single-Site Catalyst Precursors for Hydroamination
Eedugurala, Naresh; Wang, Zhuoran; Yan, KaKing; Boteju, Kasuni C.; Chaudhary, Umesh; Kobayashi, Takeshi; Ellern, Arkady; Slowing, Igor I.; Pruski, Marek; Sadow, Aaron D.; Organometallics 36 (2017) 1142–; doi:10.1021/acs.organomet.6b00956

data_4089212
_publ_section_title
;
 \b-SiH-Containing Tris(silazido) Rare-Earth Complexes as Homogeneous and
 Grafted Single-Site Catalyst Precursors for Hydroamination
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1142
_journal_paper_doi               10.1021/acs.organomet.6b00956
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C22 H58 N3 O Si3 Y'
_chemical_formula_sum            'C22 H58 N3 O Si3 Y'
_chemical_formula_weight         553.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 114.423(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.229(2)
_cell_length_b                   10.9623(12)
_cell_length_c                   16.9486(18)
_cell_measurement_reflns_used    7926
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.19
_cell_volume                     3253.0(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.998
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30184
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.520
_diffrn_reflns_theta_min         1.163
_exptl_absorpt_coefficient_mu    1.920
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker, SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.320
_refine_diff_density_max         1.643
_refine_diff_density_min         -1.038
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.197
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         7450
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.197
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0090P)^2^+12.5770P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1214
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6212
_reflns_number_total             7450
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00956_si_002.cif
_cod_data_source_block           2Et2O_YNSiHtBuEt2O
_cod_original_cell_volume        3252.9(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4089212
_shelxl_version_number           2014/7
_shelx_estimated_absorpt_t_min   0.486
_shelx_estimated_absorpt_t_max   0.579
_shelx_res_checksum              1924
_shelx_hkl_checksum              47935