A Mixed-Valence Polyoxovanadate(III,IV) Cluster with a Calixarene Cap Exhibiting Ferromagnetic V(III)-V(IV) Interactions
Christophe Aronica; Guillaume Chastanet; Ekaterina Zueva; Serguei A. Borshch; Juan M. Clemente-Juan; Dominique Luneau; Journal of the American Chemical Society 130 (2008) 2365–2371; doi:10.1021/ja078030q

data_4107438
_publ_section_title
;
 A Mixed-Valence Polyoxovanadate(III,IV) Cluster with a Calixarene Cap
 Exhibiting Ferromagnetic V(III)-V(IV) Interactions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2365
_journal_page_last               2371
_journal_paper_doi               10.1021/ja078030q
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C58 H86 N1 O19 V6'
_chemical_formula_sum            'C58 H86 N O19 V6'
_chemical_formula_weight         1406.95
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             05-07-12
_audit_creation_method           CRYSTALS_ver_12.50
_cell_angle_alpha                90
_cell_angle_beta                 104.676(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.798(5)
_cell_length_b                   15.555(5)
_cell_length_c                   28.662(5)
_cell_measurement_reflns_used    10918
_cell_measurement_temperature    293
_cell_measurement_theta_max      26
_cell_measurement_theta_min      0
_cell_volume                     6814(3)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius BV, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            22198
_diffrn_reflns_theta_full        25.188
_diffrn_reflns_theta_max         25.702
_diffrn_reflns_theta_min         1.868
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.855
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_description       plate
_exptl_crystal_F_000             2916
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.15
_refine_diff_density_min         -0.35
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.1430
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         4938
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1596
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.000768
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 1.81 1.56 1.34 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1208
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0664
_reflns_limit_h_max              18
_reflns_limit_h_min              -19
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              34
_reflns_limit_l_min              0
_reflns_number_gt                4938
_reflns_number_total             12563
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            ja078030q-file001.cif
_cod_data_source_block           CRYSTALS_cif
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C58 H86 N1 O19 V6'
_cod_database_code               4107438