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_4074913
_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         'C64 H120 Cl4 N8 Nd4 O4 Si8, 2(C7 H8)'
_chemical_formula_sum            'C78 H136 Cl4 N8 Nd4 O4 Si8'
_chemical_formula_weight         2193.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                61.759(5)
_cell_angle_beta                 85.629(9)
_cell_angle_gamma                86.579(9)
_cell_formula_units_Z            1
_cell_length_a                   13.8273(15)
_cell_length_b                   14.2373(11)
_cell_length_c                   14.7960(10)
_cell_measurement_reflns_used    9064
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      3.0
_cell_volume                     2557.7(4)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0485
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25563
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    2.239
_exptl_absorpt_correction_T_max  0.6630
_exptl_absorpt_correction_T_min  0.5629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.687
_refine_diff_density_min         -0.693
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         9305
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0315P)^2^+8.8331P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1079
_reflns_number_gt                7674
_reflns_number_total             9305
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0509995si20051119_092238.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_Hall     '-p 1'
_cod_original_sg_symbol_H-M      'p -1'
_cod_database_code               4074913