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_4089215
_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 H56 Lu N3 O Si3'
_chemical_formula_sum            'C22 H56 Lu N3 O Si3'
_chemical_formula_weight         637.93
_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     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 104.645(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9537(17)
_cell_length_b                   16.540(2)
_cell_length_c                   16.687(2)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    173.(2)
_cell_measurement_theta_max      28.7460
_cell_measurement_theta_min      2.2551
_cell_volume                     3192.1(7)
_computing_cell_refinement       'SAINT V7.66A (Bruker AXS, 2013)'
_computing_data_collection       'APEX2 Suite (Bruker AXS, 2013)'
_computing_data_reduction        'SAINT V7.66A (Bruker AXS, 2013)'
_computing_molecular_graphics    'XSHELL (Bruker AXS, 2007)'
_computing_publication_material  'APEX2 Suite (Bruker AXS, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       ' full spere \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33770
_diffrn_reflns_theta_full        28.76
_diffrn_reflns_theta_max         28.76
_diffrn_reflns_theta_min         1.76
_diffrn_source                   'X-ray tuve'
_diffrn_source_type              'Sealed tube'
_exptl_absorpt_coefficient_mu    3.222
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_correction_T_min  0.48
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2013)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.559
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         8241
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0204
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0192P)^2^+1.6472P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0462
_refine_ls_wR_factor_ref         0.0541
_reflns_number_gt                7184
_reflns_number_total             8241
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00956_si_002.cif
_cod_data_source_block           3THF_LuNSiHTHF
_cod_original_cell_volume        3192.1(8)
_cod_database_code               4089215
_shelx_res_checksum              53889
_shelx_hkl_checksum              62568