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_4309362
_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         '[Sm(HDFPSCPTSC)2]Cl*H2O'
_chemical_formula_sum            'C42 H36 N15 O6 S2 Sm'
_chemical_formula_weight         1061.33
_chemical_name_common            '[Sm(HDFPSCPTSC)2]Cl*H2O'
_chemical_name_systematic
;
Bis(2,6-diformylpyridine-4-phenylsemicarbazone-4-phenylthiosemicarbazonato)-
samarium(III) nitrate water solvate
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            18
_cell_length_a                   49.76(5)
_cell_length_b                   49.76(5)
_cell_length_c                   13.85(3)
_cell_measurement_reflns_used    916
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      41.588
_cell_measurement_theta_min      2.250
_cell_volume                     29699(8)
_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    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0943
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -58
_diffrn_reflns_limit_k_max       58
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11364
_diffrn_reflns_theta_full        24.87
_diffrn_reflns_theta_max         24.87
_diffrn_reflns_theta_min         1.42
_diffrn_standards_interval_time  '20sec / frame'
_exptl_absorpt_coefficient_mu    0.997
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.068
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             9630
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.285
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         11364
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.1261
_refine_ls_R_factor_gt           0.0669
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1069P)^2^+49.3899P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1558
_refine_ls_wR_factor_ref         0.1894
_reflns_number_gt                6888
_reflns_number_total             11364
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050556tsi20050411_050949_3.cif
_cod_data_source_block           ajl21z
_cod_original_cell_volume        29706(80)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4309362