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_7021392
_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            'C56 H74 N4'
_chemical_formula_weight         803.19
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                84.17(3)
_cell_angle_beta                 75.17(2)
_cell_angle_gamma                77.17(3)
_cell_formula_units_Z            3
_cell_length_a                   15.22(3)
_cell_length_b                   15.72(3)
_cell_length_c                   18.26(3)
_cell_measurement_reflns_used    3577
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.75
_cell_measurement_theta_min      2.31
_cell_volume                     4113(13)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.973
_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  0.0264
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_Laue_measured_fraction_full 0.952
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17247
_diffrn_reflns_point_group_measured_fraction_full 0.952
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_min         1.155
_exptl_absorpt_coefficient_mu    0.056
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.973
_exptl_crystal_description       block
_exptl_crystal_F_000             1314
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_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
793.7 Ang^3^, and a void electron population of 102 per cell.
Because the solvent involved in the recrystallization is toluene,
the amount of the disordered solvent was 2 per cell suggested by electron count.
The overall formula should be (C56H74N4).0.667(C7H8), considering the
contribution of solvent.
;
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     844
_refine_ls_number_reflns         14163
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1306
_refine_ls_R_factor_gt           0.0753
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+4.8500P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1700
_refine_ls_wR_factor_ref         0.1825
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7022
_reflns_number_total             14163
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt33040k.txt
_cod_data_source_block           a00122d
_cod_original_cell_volume        4112(13)
_cod_database_code               7021392
_shelx_estimated_absorpt_t_min   0.978
_shelx_estimated_absorpt_t_max   0.994
_shelxl_version_number           2013-2