Discrete spherical hexadecavanadates incorporating a bromide with oxidative bromination activity.
Kato, Naohiro; Hayashi, Yoshihito; Dalton transactions (Cambridge, England : 2003) 42 (2013) 11804–11811; doi:10.1039/c3dt50521a

data_7021609
_publ_section_title
;
 Discrete spherical hexadecavanadates incorporating a bromide with
 oxidative bromination activity.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11804
_journal_page_last               11811
_journal_paper_doi               10.1039/c3dt50521a
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'O38 V16, 4(C16 H36 N), Br'
_chemical_formula_sum            'C64 H144 Br N4 O38 V16'
_chemical_formula_weight         2472.77
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      18
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.996(2)
_cell_length_b                   16.885(2)
_cell_length_c                   18.218(3)
_cell_measurement_reflns_used    21098
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.5171
_cell_measurement_theta_min      3.0318
_cell_volume                     4920.5(12)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0542
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            54121
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    1.924
_exptl_absorpt_correction_T_max  0.9378
_exptl_absorpt_correction_T_min  0.5872
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            'Deep Green'
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             2526
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.2000
_refine_diff_density_max         3.177
_refine_diff_density_min         -1.155
_refine_diff_density_rms         0.143
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.035(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         11222
_refine_ls_number_restraints     278
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0699
_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^)+(0.1246P)^2^+4.5163P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1917
_refine_ls_wR_factor_ref         0.2063
_reflns_number_gt                9600
_reflns_number_total             11222
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt50521a.txt
_cod_data_source_block           V16Br
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Numerical'
changed to 'numerical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
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_cod_database_code               7021609