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_7003206
_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            'C102 H227 Mo17 N9 O62 V3'
_chemical_formula_weight         4355.73
_chemical_name_systematic
;
?
;
_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   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.542(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   31.2232(11)
_cell_length_b                   15.8592(5)
_cell_length_c                   33.5475(14)
_cell_measurement_reflns_used    9623
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5214
_cell_measurement_theta_min      3.1031
_cell_volume                     16215.5(11)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 15.9832
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Oxford Gemini Kappa 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  0.1339
_diffrn_reflns_av_sigmaI/netI    0.1682
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            70889
_diffrn_reflns_theta_full        23.00
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         3.11
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.507
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8724
_exptl_crystal_size_max          0.1833
_exptl_crystal_size_mid          0.1009
_exptl_crystal_size_min          0.0571
_refine_diff_density_max         1.35
_refine_diff_density_min         -0.83
_refine_diff_density_rms         0.19
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1168
_refine_ls_number_reflns         22223
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.2136
_refine_ls_R_factor_gt           0.1112
_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^)+(0.1023P)^2^+303.8330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2382
_refine_ls_wR_factor_ref         0.2913
_reflns_number_gt                10929
_reflns_number_total             22223
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b714285d.txt
_cod_data_source_block           hm380tba
_cod_depositor_comments
;
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        16215.5(10)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7003206