1 : 1 vs. 2 : 1 coordination of pentadentate hydrazone-type ligands to lanthanide(iii) ions. Formation of cationic as well as dicationic complexes
Albrecht, Markus; Yulia, Yeni; Exarchos, Anna; Nachev, Philipp; Fröhlich, Roland; Dalton Transactions  (2009) 7421–7427; doi:10.1039/b905049c

data_7002137
_publ_section_title
;
 1 : 1 vs. 2 : 1 coordination of pentadentate hydrazone-type ligands to
 lanthanide(iii) ions. Formation of cationic as well as dicationic
 complexes
;
_journal_issue                   36
_journal_name_full               'Dalton Transactions'
_journal_page_first              7421
_journal_page_last               7427
_journal_paper_doi               10.1039/b905049c
_journal_year                    2009
_chemical_formula_sum            'C17 H27 N10 Nd O13'
_chemical_formula_weight         723.73
_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   'at N3 from difmap. others geom'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.920(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.8305(2)
_cell_length_b                   13.0671(2)
_cell_length_c                   11.9848(1)
_cell_measurement_reflns_used    2984
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      0.41
_cell_volume                     2860.40(6)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SCHAKAL (Keller, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode Nonius FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9102
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    1.892
_exptl_absorpt_correction_T_max  0.6491
_exptl_absorpt_correction_T_min  0.4831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995 & 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1452
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.0041(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         3368
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0195
_refine_ls_R_factor_gt           0.0183
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0190P)^2^+1.8282P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0458
_refine_ls_wR_factor_ref         0.0463
_reflns_number_gt                3232
_reflns_number_total             3368
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b905049c.txt
_cod_data_source_block           fro4515
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7002137