Lanthanide Complexes of Macrocyclic Polyoxovanadates by VO4 Units: Synthesis, Characterization, and Structure Elucidation by X-ray Crystallography and EXAFS Spectroscopy
Masaki Nishio; Shinnosuke Inami; Misaki Katayama; Kazuhiko Ozutsumi; Yoshihito Hayashi; Inorganic Chemistry 51 (2012) 784–793; doi:10.1021/ic200638f

data_4327938
_publ_contact_author_address
;   Department of Chemistry 
    Graduate School of Natural Science
    Kanazawa University
    Kakuma
    Kanazawa 920-1192
    Japan
;
_publ_contact_author_email       hayashi@se.kanazawa-u.ac.jp
_publ_contact_author_fax         '+81 762 2645742'
_publ_contact_author_name
;   
Dr. Yoshihito HAYASHI
;
_publ_contact_author_phone       '+81 762 2645695'
_publ_section_title
;
 Lanthanide Complexes of Macrocyclic Polyoxovanadates by VO4 Units:
 Synthesis, Characterization, and Structure Elucidation by X-ray
 Crystallography and EXAFS Spectroscopy
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              784
_journal_page_last               793
_journal_paper_doi               10.1021/ic200638f
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C168 Dy3 N30 O81.25 V27'
_chemical_formula_weight         5600.86
_chemical_name_systematic
; 
 ? 
;
_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   notdet
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.365(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.693(2)
_cell_length_b                   44.032(4)
_cell_length_c                   25.265(3)
_cell_measurement_reflns_used    6484
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.1021
_cell_measurement_theta_min      3.1680
_cell_volume                     26242(5)
_computing_cell_refinement       'CrystalClear v1.3.7(Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear v1.3.7(Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear v1.3.7(Rigaku Corp., 2000)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 14.4613
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Mercury CCD (2x2 bin mode)'
_diffrn_measurement_method       dtintegrate.ref
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.1373
_diffrn_reflns_av_sigmaI/netI    0.1561
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            133300
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.17
_exptl_absorpt_coefficient_mu    1.825
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4355
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_description       Block
_exptl_crystal_F_000             10746
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.2000
_refine_diff_density_max         5.887
_refine_diff_density_min         -2.507
_refine_diff_density_rms         0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2788
_refine_ls_number_reflns         42864
_refine_ls_number_restraints     2196
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1532
_refine_ls_R_factor_gt           0.1256
_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^)+(0.1142P)^2^+487.9859P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2935
_refine_ls_wR_factor_ref         0.3091
_reflns_number_gt                31535
_reflns_number_total             42864
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200638f_si_002_4.cif
_cod_data_source_block           Dy
_cod_original_cell_volume        26243(4)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4327938