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_4308990
_publ_contact_author_address
; Coordination and Hydrothermal Chemistry Group
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            'C20 H75 As8 Cd3 N15 O46 V13'
_chemical_formula_weight         2860.73
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 122.8000(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   33.0247(2)
_cell_length_b                   29.4271(5)
_cell_length_c                   20.5927(3)
_cell_measurement_reflns_used    373
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.83
_cell_volume                     16821.8(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0788
_diffrn_reflns_av_sigmaI/netI    0.0817
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28774
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.83
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    5.325
_exptl_absorpt_correction_T_max  0.727
_exptl_absorpt_correction_T_min  0.413
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.259
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             11000
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.165
_refine_diff_density_min         -1.297
_refine_diff_density_rms         0.224
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.197
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     947
_refine_ls_number_reflns         14091
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.197
_refine_ls_R_factor_gt           0.0918
_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^)+(0.0000P)^2^+1082.0370P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1690
_refine_ls_wR_factor_ref         0.1927
_reflns_number_gt                10260
_reflns_number_total             14091
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0486015si20041007_051748.cif
_cod_data_source_block           Cd-dien
_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               4308990
_refine_ls_r_factor_ref          0.1356