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_4309360
_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]Cl'
_chemical_formula_sum            'C46 H42 Ce Cl N12 O4'
_chemical_formula_weight         1002.49
_chemical_name_common            '[Ce(HDAPBHPSC)2]Cl'
_chemical_name_systematic
;
Bis(2,6-diacetylpyridine-benzoylhydrazonato-4-phenylsemicarbazone)cerium(III)
chlorid
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.891(1)
_cell_length_b                   21.859(2)
_cell_length_c                   35.026(4)
_cell_measurement_temperature    293(2)
_cell_volume                     9869.8(16)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        SHELXTL
_computing_molecular_graphics    SCHAKAL
_computing_publication_material  WINGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1305
_diffrn_reflns_av_sigmaI/netI    0.3150
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            46252
_diffrn_reflns_theta_full        28.09
_diffrn_reflns_theta_max         28.09
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '20 sec / frame'
_exptl_absorpt_coefficient_mu    1.029
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.834
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4072
_exptl_crystal_size_max          .2
_exptl_crystal_size_mid          .07
_exptl_crystal_size_min          .06
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.865
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         11563
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.865
_refine_ls_R_factor_all          0.3008
_refine_ls_R_factor_gt           0.0653
_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^)+(0.0510P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1693
_reflns_number_gt                3486
_reflns_number_total             11563
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050556tsi20050411_050949_1.cif
_cod_data_source_block           cecl
_cod_original_cell_volume        9870(2)
_cod_database_code               4309360