Bridging the gap between solution and solid state studies in polyoxometalate chemistry: Discovery of a family of [V1M17]-based cages encapsulating two {VVO4} moieties
Miras, Haralampos N.; Long, De-Liang; Kögerler, Paul; Cronin, Leroy; Dalton Transactions  (2008) 214–221; doi:10.1039/b714285d

data_7003208
_publ_section_title
;
 Bridging the gap between solution and solid state studies in
 polyoxometalate chemistry: Discovery of a family of [V1M17]-based
 cages encapsulating two {VVO4} moieties
;
_journal_issue                   2
_journal_name_full               'Dalton Transactions'
_journal_page_first              214
_journal_page_last               221
_journal_paper_doi               10.1039/b714285d
_journal_year                    2008
_chemical_formula_sum            'H34 N2 Na4 O74 V3 W17'
_chemical_formula_weight         4616.52
_chemical_name_systematic
;
?
;
_space_group_IT_number           166
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_atom_sites_solution_hydrogens   none
_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            9
_cell_length_a                   37.655(3)
_cell_length_b                   37.655(3)
_cell_length_c                   13.0008(13)
_cell_measurement_reflns_used    3121
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      44.03
_cell_measurement_theta_min      4.33
_cell_volume                     15964(2)
_computing_cell_refinement       'Bruker ApexII'
_computing_data_collection       'Bruker ApexII'
_computing_data_reduction        'Bruker ApexII'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker ApexII CCD'
_diffrn_measurement_method       '\w & \p 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  0.0839
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            21914
_diffrn_reflns_theta_full        20.82
_diffrn_reflns_theta_max         20.82
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    27.947
_exptl_absorpt_correction_T_max  0.1665
_exptl_absorpt_correction_T_min  0.0815
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    4.322
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             18099
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.48
_refine_diff_density_min         -1.72
_refine_diff_density_rms         0.30
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         1970
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0410P)^2^+2660.1404P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1163
_reflns_number_gt                1582
_reflns_number_total             1970
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b714285d.txt
_cod_data_source_block           hm335a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Empirical' changed to 'empirical'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        15965(2)
_cod_original_sg_symbol_H-M      R-3m
_cod_database_code               7003208