Metallomacrocycle Complexes of Lanthanides with Bridged Amide Ligands: Syntheses and Molecular Structures of [{μ2-p-(Me3SiN)2C6H4}YbCl(THF)2]2and [{μ2-p-(Me3SiN)2C6H4}Nd(μ2-Cl)(THF)]42PhMe
Zhao, Bei; Li, Honghai; Shen, Qi; Zhang, Yong; Yao, Yingming; Lu, Chengrong; Organometallics 25 (2006) 1824–; doi:10.1021/om0509995

data_4074914
_publ_section_title
;
 Metallomacrocycle Complexes of Lanthanides with Bridged Amide
 Ligands:&#x00A0; Syntheses and Molecular Structures of
 [{\m2-p-(Me3SiN)2C6H4}YbCl(THF)2]2and
 [{\m2-p-(Me3SiN)2C6H4}Nd(\m2-Cl)(THF)]42PhMe
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1824
_journal_paper_doi               10.1021/om0509995
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C40 H76 Cl2 N4 O4 Si4 Yb2'
_chemical_formula_sum            'C40 H76 Cl2 N4 O4 Si4 Yb2'
_chemical_formula_weight         1206.39
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 93.481(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.127(3)
_cell_length_b                   12.0839(13)
_cell_length_c                   17.4643(19)
_cell_measurement_reflns_used    9351
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     5292.9(10)
_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      193(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28590
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    3.742
_exptl_absorpt_correction_T_max  0.3998
_exptl_absorpt_correction_T_min  0.2513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.30
_refine_diff_density_max         2.332
_refine_diff_density_min         -2.741
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.232
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         6069
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.247
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0561
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0598P)^2^+26.7858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1299
_refine_ls_wR_factor_ref         0.1350
_reflns_number_gt                5387
_reflns_number_total             6069
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0509995si20051119_092351.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        5293.0(10)
_cod_original_sg_symbol_Hall     '-c 2yc'
_cod_original_sg_symbol_H-M      'c 2/c'
_cod_database_code               4074914