The first polyoxoalkoxovanadium germanate anion with a novel cage-like structure: solvothermal synthesis and characterization
Chen, Yan-Min; Wang, En-Bo; Lin, Bi-Zhou; Wang, Shu-Tao; Dalton Transactions  (2003) 519–; doi:10.1039/b208489a

data_7012200
_publ_section_title
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 The first polyoxoalkoxovanadium germanate anion with a novel cage-like
 structure: solvothermal synthesis and characterization
;
_journal_issue                   4
_journal_name_full               'Dalton Transactions'
_journal_page_first              519
_journal_paper_doi               10.1039/b208489a
_journal_year                    2003
_chemical_formula_sum            'C12 H33 Ge6 N O39 V9'
_chemical_formula_weight         1709.39
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           58
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2 2n'
_symmetry_space_group_name_H-M   'P n n m'
_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            4
_cell_length_a                   18.5773(6)
_cell_length_b                   22.7989(9)
_cell_length_c                   14.5097(4)
_cell_measurement_reflns_used    63155
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.98
_cell_measurement_theta_min      1.67
_cell_volume                     6145.5(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       'Oscillation scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         '18 kW rotate anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0870
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12985
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    4.265
_exptl_absorpt_correction_T_max  0.263
_exptl_absorpt_correction_T_min  0.158
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1995). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.848
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3292
_exptl_crystal_size_max          0.412
_exptl_crystal_size_mid          0.367
_exptl_crystal_size_min          0.313
_refine_diff_density_max         0.995
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.196
_refine_ls_extinction_coef       0.00130(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         7129
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0574
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1588
_refine_ls_wR_factor_ref         0.1665
_reflns_number_gt                3883
_reflns_number_total             7129
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b208489a.txt
_cod_data_source_block           m054
_cod_depositor_comments
;
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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      Pnnm
_cod_database_code               7012200