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_7002136
_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            'C54 H56 Br4 F9 La N10 O17 S3'
_chemical_formula_weight         1842.82
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   'at O301 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                 103.985(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.6299(4)
_cell_length_b                   16.7038(4)
_cell_length_c                   21.2816(6)
_cell_measurement_reflns_used    12242
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      0.41
_cell_volume                     7116.2(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.098
_diffrn_reflns_av_sigmaI/netI    0.0908
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            45951
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    3.028
_exptl_absorpt_correction_T_max  0.8634
_exptl_absorpt_correction_T_min  0.4636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.720
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3648
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.164
_refine_diff_density_min         -0.904
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     889
_refine_ls_number_reflns         12499
_refine_ls_number_restraints     252
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1425
_refine_ls_R_factor_gt           0.0806
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0740P)^2^+50.1277P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1741
_refine_ls_wR_factor_ref         0.2025
_reflns_number_gt                7607
_reflns_number_total             12499
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b905049c.txt
_cod_data_source_block           fro4513
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7002136