Synthesis, structure and reactivity of dinuclear rare earth metal bis(o-aminobenzyl) complexes bearing a 1,4-phenylenediamidinate co-ligand.
Li, Meng; Hong, Jianquan; Chen, Zhenxia; Zhou, Xigeng; Zhang, Lixin; Dalton transactions (Cambridge, England : 2003) 42 (2013) 8288–8297; doi:10.1039/c3dt33040k

data_7021394
_publ_section_title
;
 Synthesis, structure and reactivity of dinuclear rare earth metal
 bis(o-aminobenzyl) complexes bearing a 1,4-phenylenediamidinate
 co-ligand.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8288
_journal_page_last               8297
_journal_paper_doi               10.1039/c3dt33040k
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C120 H140 N12 S4 Y2'
_chemical_formula_weight         2056.49
_chemical_name_systematic
;
?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d'
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.625(3)
_cell_length_b                   36.414(10)
_cell_length_c                   63.656(18)
_cell_measurement_reflns_used    5579
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.18
_cell_measurement_theta_min      2.45
_cell_volume                     26946(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0614
_diffrn_reflns_av_unetI/netI     0.0689
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -75
_diffrn_reflns_number            27109
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.280
_exptl_absorpt_coefficient_mu    0.963
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.014
_exptl_crystal_description       block
_exptl_crystal_F_000             8688
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_platon_squeeze_details
;
The disordered solvents within the void were not crystallographically
well defined.
The SQUEEZE routine of the program PLATON was used
in order to eliminate the contribution of disordered solvents molecules,
thereby a final model based only on the ordered part of the crystal
structure was obtained.
The SQUEEZE routine suggested that
a total potential solvent area volume of 6580.0 Ang^3^,
and a void electron population of 1619 per cell.
Because the solvent we used in the recrystalization of this complex is
toluene, the amount of the disordered solvent was 32 per cell suggested
by electron count. The overall formula should be (C120H140N12S4Y2).4(C7H8),
considering the contribution of solvent.
;
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         5944
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+48.0000P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1342
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3383
_reflns_number_total             5944
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt33040k.txt
_cod_data_source_block           a10122a
_cod_original_cell_volume        26947(13)
_cod_database_code               7021394
_shelx_estimated_absorpt_t_min   0.831
_shelx_estimated_absorpt_t_max   0.927
_shelxl_version_number           2013-2