Encapsulation of paramagnetic 3d1-vanadium(IV) in an antiferromagnetically coupled dodecanuclear copper(II) cage
Mukherjee, Arindam; Nethaji, Munirathinam; Chakravarty, Akhil R.; Chemical Communications (Cambridge, United Kingdom)  (2003) 2978–2979; doi:10.1039/b310521k

data_7113607
_publ_section_title
;
 Encapsulation of paramagnetic 3d1-vanadium(IV) in an
 antiferromagnetically coupled dodecanuclear copper(II) cage
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   24
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              2978
_journal_page_last               2979
_journal_paper_doi               10.1039/b310521k
_journal_year                    2003
_chemical_formula_moiety         'C104 H102 Cl6 Cu12 N12 O28 V1'
_chemical_formula_sum            'C104 H102 Cl6 Cu12 N12 O28 V'
_chemical_formula_weight         2994.10
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :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            6
_cell_length_a                   16.001(3)
_cell_length_b                   16.001(3)
_cell_length_c                   79.15(4)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      1.54
_cell_volume                     17550(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      273(2)
_diffrn_detector_area_resol_mean 0.03
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_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  0.0447
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       101
_diffrn_reflns_limit_l_min       -100
_diffrn_reflns_number            43444
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    2.421
_exptl_absorpt_correction_T_max  0.94907
_exptl_absorpt_correction_T_min  0.69426
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             9042
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_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.577
_refine_diff_density_min         -1.098
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     239
_refine_ls_number_reflns         4318
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0729
_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^)+(0.1561P)^2^+49.2700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2191
_refine_ls_wR_factor_ref         0.2494
_reflns_number_gt                3121
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_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7103913
_cod_data_source_file            b310521k.txt
_cod_data_source_block           '[Cu12VO5L6].2CHCl3.5H2O'
_cod_original_cell_volume        17552(9)
_cod_original_sg_symbol_H-M      R-3c
_cod_database_code               7113607