Controlled Ligand Deprotonation in Lanthanide Chelates with Asymmetric Semicarbazone/Benzoylhydrazone or Semicarbazone/Thiosemicarbazone Coordination Spheres
Alexander Jagst; Agustin Sánchez; Ezequiel M. Vázquez-López; Ulrich Abram; Inorganic Chemistry 44 (2005) 5738–5744; doi:10.1021/ic050556t

data_4309361
_publ_contact_author
;
      Ulrich Abram
      Free University of Berlin     
      Institute of Chemistry             
      Fabeckstrasse 34-36                     
      D-14195 Berlin         
      Germany                          
;
_publ_contact_author_email       abram@chemie.fu-berlin.de
_publ_contact_author_fax         '0049 (0)30 838 52676'
_publ_contact_author_phone       '0049 (0)30 838 54002'
_publ_section_title
;
Controlled Ligand Deprotonation in Lanthanide Chelates with Asymmetric
Semicarbazone/Benzoylhydrazone or Semicarbazone/Thiosemicarbazone
Coordination Spheres
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5738
_journal_page_last               5744
_journal_paper_doi               10.1021/ic050556t
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         '[Ce(HDAPBHPSC)2]2SO4*7EtOH'
_chemical_formula_sum            'C110 H138 Ce2 N24 O21 S'
_chemical_formula_weight         2444.74
_chemical_name_common            '[Ce(HDAPBHPSC)2]2SO4*7EtOH'
_chemical_name_systematic
;
Bis(2,6-diacetylpyridin-benzoylhydrazonato-4-phenylsemicarbazone)-
cerium(III)-sulfate ethanol solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 93.067(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   23.169(5)
_cell_length_b                   20.064(5)
_cell_length_c                   25.288(5)
_cell_measurement_reflns_used    1011
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.188
_cell_measurement_theta_min      2.531
_cell_volume                     11739(5)
_computing_cell_refinement       'Bruker Smart'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        'Bruker Smart'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'ccd area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            94435
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.16
_diffrn_standards_interval_time  '20sec / frame'
_exptl_absorpt_coefficient_mu    0.860
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.846705
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5064
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1475
_refine_ls_number_reflns         20010
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.129
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0807
_reflns_number_gt                14854
_reflns_number_total             20010
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050556tsi20050411_050949_2.cif
_cod_data_source_block           ce4(l8)2
_cod_database_code               4309361