First hexadecavanadate compound: hydrothermal synthesis and characterization of a three-dimensional framework [{Cu(1,2-pn)2}7{V16O38(H2O)}2]??4H2O
Lin, Bi-Zhou; Liu, Shi-Xiong; Chemical Communications  (2002) 2126–; doi:10.1039/b206880j

data_7114029
_publ_section_title
;
 First hexadecavanadate compound: hydrothermal synthesis and
 characterization of a three-dimensional framework
 [{Cu(1,2-pn)2}7{V16O38(H2O)}2]??4H2O
;
_journal_issue                   18
_journal_name_full               'Chemical Communications'
_journal_page_first              2126
_journal_paper_doi               10.1039/b206880j
_journal_year                    2002
_chemical_formula_moiety         'Cu7 C42 N28 H152 V32 O82'
_chemical_formula_sum            'C42 H152 Cu7 N28 O82 V32'
_chemical_formula_weight         4436.78
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.170(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   21.510(2)
_cell_length_b                   25.580(3)
_cell_length_c                   12.6320(10)
_cell_measurement_reflns_used    350
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      10
_cell_volume                     6949.0(12)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection
;
Rigaku R-AXIS RAPID diffractometer Control Software (RAPID AUTO)
;
_computing_data_reduction
;
TEXRAY (Molecuar Structure Corporation, 1987)
;
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_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 0.952
_diffrn_measured_fraction_theta_max 0.823
_diffrn_measurement_device_type  'Rigaku R-AXIS-Parid IP'
_diffrn_measurement_method       'Oscillation scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0731
_diffrn_reflns_av_sigmaI/netI    0.1912
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25395
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.59
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.179
_exptl_absorpt_correction_T_max  0.7851
_exptl_absorpt_correction_T_min  0.4294
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1995). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.120
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhomb
_exptl_crystal_F_000             4390
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.945
_refine_diff_density_rms         0.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.869
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     847
_refine_ls_number_reflns         15162
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.869
_refine_ls_R_factor_all          0.1543
_refine_ls_R_factor_gt           0.0655
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0871P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1611
_refine_ls_wR_factor_ref         0.1813
_reflns_number_gt                5546
_reflns_number_total             15162
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b206880j.txt
_cod_data_source_block           Cu7V16
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7114029