Synthesis, X-ray Structure, and Solution NMR Studies of Ln(III) Complexes with a Macrocyclic Asymmetric Compartmental Schiff Base. Preference of the Ln(III) Ions for a Crown-Like Coordination Site
Umberto Casellato; Sergio Tamburini; Patrizia Tomasin; Pietro A. Vigato; Silvio Aime; Mauro Botta; Inorganic Chemistry 38 (1999) 2906–2916; doi:10.1021/ic980715r

data_4322061
_publ_contact_author
;
      Umberto Casellato
      ICTIMA - C.N.R.
      Corso Stati Uniti 4
      35127 Padova
      Italy
;
_publ_contact_author_email       berto@ictr.pd.cnr.it
_publ_contact_author_fax         '0039 49 8702911'
_publ_contact_author_phone       '0039 49 8295959'
_publ_section_title
;
 Synthesis, X-ray Structure, and Solution NMR Studies of Ln(III) Complexes
 with a Macrocyclic Asymmetric Compartmental Schiff Base. Preference of
 the Ln(III) Ions for a Crown-Like Coordination Site
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2906
_journal_page_last               2916
_journal_paper_doi               10.1021/ic980715r
_journal_volume                  38
_journal_year                    1999
_chemical_compound_source        synthesis
_chemical_formula_moiety
;
[Ce(C~23~H~31~N~3~O~5~)(H~2~O)~4~]^.^Cl~3~^.^H~2~O 
;
_chemical_formula_sum            'C23 H39 Ce Cl3 N3 O10'
_chemical_formula_weight         764.05
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 98.03(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.983(5)
_cell_length_b                   16.960(6)
_cell_length_c                   9.058(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      6
_cell_volume                     1670.7(12)
_computing_cell_refinement       'Philips PW1100 Febo-system'
_computing_data_collection       'Philips PW1100 Febo-system'
_computing_data_reduction        'Digital DEC 3000'
_computing_molecular_graphics    'ORTEP II'
_computing_publication_material  'Parst-94 (Nardelli 1995)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Philips PW1100 (FEBO system) diffractometer'
_diffrn_measurement_method       \q/2\q
_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  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3500
_diffrn_reflns_theta_max         30.99
_diffrn_reflns_theta_min         3.05
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    15.4
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   \y-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.49
_exptl_crystal_description       prism
_exptl_crystal_F_000             774
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.392
_refine_ls_goodness_of_fit_obs   2.392
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         3039
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.600
_refine_ls_restrained_S_obs      2.390
_refine_ls_R_factor_all          0.0922
_refine_ls_R_factor_obs          0.0813
_refine_ls_shift/esd_max         -0.778
_refine_ls_shift/esd_mean        0.044
_refine_ls_structure_factor_coef Fsqd
_refine_ls_wR_factor_all         0.2379
_refine_ls_wR_factor_obs         0.2084
_reflns_number_observed          3050
_reflns_number_total             3268
_reflns_observed_criterion       >3\s(I)
_cod_data_source_file            ic980715r_1.cif
_cod_data_source_block           ceri03
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'heavy-atom' was changed to
'heavy'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        1670(1)
_cod_original_sg_symbol_H-M      'P 21 '
_cod_database_code               4322061