3D Supramolecular Array Assembled by Cross-like Arrangement of 1D Sandwich Mixed Molybdenum−Vanadium Polyoxometalate Bridged Coordination Polymer Chains: Hydrothermal Synthesis and Crystal Structure of {[MoVI5MoV3VIV8O40(PO4)][Ni(en)2]}[Ni(en)2]2·4H2O
Liu, Cai-Ming; Zhang, De-Qing; Zhu, Dao-Ben; Crystal Growth & Design 5 (2005) 1639–; doi:10.1021/cg049556e

data_4504858
_publ_section_title
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 3D Supramolecular Array Assembled by Cross-like Arrangement of 1D
 Sandwich Mixed Molybdenum&#x2212;Vanadium Polyoxometalate Bridged
 Coordination Polymer Chains:&#x2009; Hydrothermal Synthesis and Crystal
 Structure of {[MoVI5MoV3VIV8O40(PO4)][Ni(en)2]}[Ni(en)2]2&#x00B7;4H2O
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_journal_issue                   4
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1639
_journal_paper_doi               10.1021/cg049556e
_journal_volume                  5
_journal_year                    2005
_chemical_formula_sum            'C12 H48 Mo8 N12 Ni3 O48 P V8'
_chemical_formula_weight         2510.76
_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                 106.60(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.186(5)
_cell_length_b                   13.520(3)
_cell_length_c                   19.559(4)
_cell_measurement_temperature    293(2)
_cell_volume                     6636(3)
_computing_cell_refinement       'RAPID AUTO (Rigaku, 2001)'
_computing_data_collection       'RAPID AUTO (Rigaku, 2001)'
_computing_data_reduction        'RAPID AUTO (Rigaku, 2001)'
_computing_molecular_graphics    'SHELXTL-97 (Siemens, 1994)'
_computing_publication_material  'SHELXTL-97 (Siemens, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_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  0.0250
_diffrn_reflns_av_sigmaI/netI    0.0535
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14112
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    3.477
_exptl_absorpt_correction_T_max  1.1252
_exptl_absorpt_correction_T_min  0.7211
_exptl_absorpt_correction_type   'PSI scans'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    2.513
_exptl_crystal_density_meas      Empirical
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             4828
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.886
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.136
_refine_ls_extinction_coef       0.00008(2)
_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   0.932
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         7550
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0562P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.0987
_reflns_number_gt                5115
_reflns_number_total             7550
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg049556esi20041231_021539.cif
_cod_data_source_block           1
_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_values 1715 2011-07-08 13:25:40Z adriana 
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_cod_original_cell_volume        6636(2)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4504858