Synthesis of β-diketiminate-ligated bimetallic and monometallic lanthanide amide complexes and their reactivity with isoprene and AlMe3.
Sun, Song; Ouyang, Hao; Luo, Yunjie; Zhang, Yong; Shen, Qi; Yao, Yingming; Dalton transactions (Cambridge, England : 2003) 42 (2013) 16355–16364; doi:10.1039/c3dt52014e

data_7023945
_publ_section_title
;
 Synthesis of \b-diketiminate-ligated bimetallic and monometallic
 lanthanide amide complexes and their reactivity with isoprene and AlMe3.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16355
_journal_page_last               16364
_journal_paper_doi               10.1039/c3dt52014e
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C35 H65 N4 O Si4 Y'
_chemical_formula_weight         759.18
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.189(2)
_cell_length_b                   14.5123(12)
_cell_length_c                   16.414(5)
_cell_measurement_reflns_used    5763
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.8750
_cell_measurement_theta_min      3.8890
_cell_volume                     4332.7(14)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w 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  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0587
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24412
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    1.486
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.52291
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.7500
_exptl_crystal_size_mid          0.6000
_exptl_crystal_size_min          0.2000
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.023(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         8388
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0587P)^2^+1.3792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1142
_reflns_number_gt                6598
_reflns_number_total             8388
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52014e.txt
_cod_data_source_block           complex7
_cod_original_cell_volume        4332.8(15)
_cod_database_code               7023945