Hydrothermal Syntheses and Crystal Structures of Two Novel, Hybrid Materials Based on Secondary Transition-Metal-Incorporated Polyoxovanadate Cluster Backbones: [Cd(dien)2]2[(dien)CdAs8V13O41(H2O)].4H2O and [Cd(en)2]2[(en)2Cd2As8V12O40]
Shou-Tian Zheng; Jie Zhang; Guo-Yu Yang; Inorganic Chemistry 44 (2005) 2426–2430; doi:10.1021/ic0486015

data_4308991
_publ_contact_author_address
; State Key Laboratory of Structural Chemistry
Fujian Institute of Research on The Structure of Matter
Chinese Academy of Sciences
Fuzhou, Fujian 350002
P. R. China
;
_publ_contact_author_email       ygy@fjirsm.ac.cn
_publ_contact_author_fax         '86 591 83710051'
_publ_contact_author_name        'Professor Guo-Yu Yang'
_publ_contact_author_phone       '86 591 83710051'
_publ_section_title
;
Hydrothermal Syntheses and Crystal Structures of Two Novel, Hybrid
Materials Based on Secondary Transition-Metal-Incorporated Polyoxovanadate
Cluster Backbones: [Cd(dien)2]2[(dien)CdAs8V13O41(H2O)].4H2O and
[Cd(en)2]2[(en)2Cd2As8V12O40]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2426
_journal_page_last               2430
_journal_paper_doi               10.1021/ic0486015
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C12 H48 As8 Cd4 N12 O40 V12'
_chemical_formula_weight         2660.86
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.842(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.3743(7)
_cell_length_b                   19.4268(11)
_cell_length_c                   14.1430(8)
_cell_measurement_reflns_used    209
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.08
_cell_measurement_theta_min      2.69
_cell_volume                     3314.8(3)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       'phi and omega 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  0.0785
_diffrn_reflns_av_sigmaI/netI    0.0932
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10331
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         2.69
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    6.913
_exptl_absorpt_correction_T_max  0.219
_exptl_absorpt_correction_T_min  0.176
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.666
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.409
_refine_diff_density_min         -1.207
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         5628
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_gt           0.0760
_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^)+(0.1045P)^2^+28.6567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_gt          0.1749
_refine_ls_wR_factor_ref         0.2121
_reflns_number_gt                3530
_reflns_number_total             5628
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0486015si20041007_051842.cif
_cod_data_source_block           Cd-en
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_database_code               4308991
_refine_ls_r_factor_ref          0.1304