Novel Tungstovanadate Wells−Dawson Organic‒Inorganic Heteropolyoxometalate Compound: Synthesis and Crystal Structure of [Cu2(2,2′-bipy)2(Inic)2(H2O)2][Y(Inic)2(H2O)5]H3[V2W18O62]·5.5H2O (Where 2,2′-bipy = 2,2′-Bipyridine, Inic = γ-Picolinic Acid)
Wang, Jingping; Li, Suzhi; Shen, Yue; Niu, Jingyang; Crystal Growth & Design 8 (2008) 372–; doi:10.1021/cg070234v

data_4503076
_publ_section_title
;
 Novel Tungstovanadate Wells&#x2212;Dawson Organic--Inorganic
 Heteropolyoxometalate Compound: Synthesis and Crystal Structure of
 [Cu2(2,2&#x2032;-bipy)2(Inic)2(H2O)2][Y(Inic)2(H2O)5]H3[V2W18O62]&#x00B7;5.5H2O
 (Where 2,2&#x2032;-bipy = 2,2&#x2032;-Bipyridine, Inic = \g-Picolinic
 Acid)
;
_journal_issue                   2
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              372
_journal_paper_doi               10.1021/cg070234v
_journal_volume                  8
_journal_year                    2008
_chemical_formula_sum            'C44 H60 Cu2 N8 O82.5 V2 W18 Y'
_chemical_formula_weight         5647.95
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 106.909(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.061(4)
_cell_length_b                   19.050(5)
_cell_length_c                   18.765(5)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.5
_cell_volume                     5151(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  R-axis-IV
_diffrn_measurement_method       \w
_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  0.0637
_diffrn_reflns_av_sigmaI/netI    0.0847
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25342
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    21.247
_exptl_absorpt_correction_T_max  0.2034
_exptl_absorpt_correction_T_min  0.1428
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.642
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             5030
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.483
_refine_diff_density_min         -3.166
_refine_diff_density_rms         0.356
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         9318
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0612P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1254
_reflns_number_gt                6631
_reflns_number_total             9318
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg070234v-file001.cif
_cod_data_source_block           njy1
_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.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' 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 
;
_cod_original_sg_symbol_H-M      P2(1)/m
_cod_original_formula_sum        'C44 H60 Cu2 N8 O82.50 V2 W18 Y'
_cod_database_code               4503076