Synthesis, Characterization, and Reactivity of Lanthanide Amides Incorporating Neutral Pyrrole Ligand. Isolation and Characterization of Active Catalyst for Cyanosilylation of Ketones
Wang, Fenhua; Wei, Yun; Wang, Shaowu; Zhu, Xiancui; Zhou, Shuangliu; Yang, Gaosheng; Gu, Xiaoxia; Zhang, Guangchao; Mu, Xiaolong; Organometallics 34 (2015) 86–; doi:10.1021/om500924q

data_4085168
_publ_section_title
;
 Synthesis, Characterization, and Reactivity of Lanthanide Amides
 Incorporating Neutral Pyrrole Ligand. Isolation and Characterization of
 Active Catalyst for Cyanosilylation of Ketones
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              86
_journal_paper_doi               10.1021/om500924q
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C41 H96 La2 N8 Si8'
_chemical_formula_weight         1203.80
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.8260(10)
_cell_angle_beta                 88.2900(10)
_cell_angle_gamma                72.5680(10)
_cell_formula_units_Z            2
_cell_length_a                   11.2896(9)
_cell_length_b                   16.1701(12)
_cell_length_c                   18.0350(14)
_cell_measurement_temperature    293(2)
_cell_volume                     3139.7(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            27522
_diffrn_reflns_theta_full        27.77
_diffrn_reflns_theta_max         27.77
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    1.527
_exptl_absorpt_correction_T_max  0.8380
_exptl_absorpt_correction_T_min  0.7922
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.026
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         14334
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+1.3692P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0923
_reflns_number_gt                11233
_reflns_number_total             14334
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500924q_si_002.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2935 2014-11-11 08:27:57Z andrius 

 Adding full bibliography for 4085164--4085170.cif.
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4085168