Dinuclear Lanthanide(III) Complexes by Metal-Ion-Assisted Hydration of Di-2-pyridyl Ketone Azine
Nikolaos C. Anastasiadis; Carlos M. Granadeiro; Nikolaos Klouras; Luís Cunha-Silva; Catherine P. Raptopoulou; Vassilis Psycharis; Vlasoula Bekiari; Salete S. Balula; Albert Escuer; Spyros P. Perlepes; Inorganic Chemistry 52 (2013) 4145–4147; doi:10.1021/ic400185e

data_4334511
_publ_section_title
;
 Dinuclear Lanthanide(III) Complexes by Metal-Ion-Assisted Hydration of
 Di-2-pyridyl Ketone Azine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4145
_journal_page_last               4147
_journal_paper_doi               10.1021/ic400185e
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C47 H38.9 N17.5 Nd2 O14.2'
_chemical_formula_weight         1364.54
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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                 103.9560(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   45.7579(8)
_cell_length_b                   14.8658(3)
_cell_length_c                   17.4000(3)
_cell_measurement_reflns_used    40287
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      72.05
_cell_measurement_theta_min      6.50
_cell_volume                     11486.6(4)
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       '\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_sigmaI/netI    0.0550
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            42422
_diffrn_reflns_theta_full        65.00
_diffrn_reflns_theta_max         65.00
_diffrn_reflns_theta_min         6.51
_exptl_absorpt_coefficient_mu    14.291
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.309
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             5416
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.341
_refine_diff_density_min         -2.041
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     756
_refine_ls_number_reflns         9725
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0544
_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^)+(0.0851P)^2^+68.1654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1438
_refine_ls_wR_factor_ref         0.1472
_reflns_number_gt                8956
_reflns_number_total             9725
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400185e_si_002_1.cif
_cod_data_source_block           compound2
_cod_original_formula_sum        'C47 H38.90 N17.50 Nd2 O14.20'
_cod_database_code               4334511