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_4327939
_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            'C48 Ho N9 O25 V8'
_chemical_formula_weight         1675.02
_chemical_name_systematic
; 
 ? 
;
_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   notdet
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.743(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.080(8)
_cell_length_b                   21.551(8)
_cell_length_c                   19.928(8)
_cell_measurement_reflns_used    7352
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.1021
_cell_measurement_theta_min      3.8227
_cell_volume                     7557(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 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Mercury CCD (2x2 bin mode)'
_diffrn_measurement_method       dtintegrate.ref
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_sigmaI/netI    0.0783
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            53311
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         3.82
_exptl_absorpt_coefficient_mu    2.045
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6558
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_description       Block
_exptl_crystal_F_000             3207
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.2000
_refine_diff_density_max         2.506
_refine_diff_density_min         -2.772
_refine_diff_density_rms         0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     922
_refine_ls_number_reflns         14341
_refine_ls_number_restraints     444
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0985
_refine_ls_R_factor_gt           0.0788
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1136P)^2^+77.3276P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2084
_refine_ls_wR_factor_ref         0.2320
_reflns_number_gt                10881
_reflns_number_total             14341
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200638f_si_002_5.cif
_cod_data_source_block           Ho
_cod_database_code               4327939