Grid-Type Two-Dimensional Magnetic Multinuclear Metal Complex: Strands of {[CuII(μ-4,4'-bpy)]2+}n Cross-Linked by Octacyanotungstate(V) Ions
Tomasz Korzeniak; Katarzyna Stadnicka; Michał Rams; Barbara Sieklucka; Inorganic Chemistry 43 (2004) 4811–4813; doi:10.1021/ic049402o

data_4311402
_publ_section_title
;
 Grid-Type Two-Dimensional Magnetic Multinuclear Metal Complex: Strands of
 {[CuII(\m-4,4'-bpy)]2+}n Cross-Linked by Octacyanotungstate(V) Ions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4811
_journal_page_last               4813
_journal_paper_doi               10.1021/ic049402o
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         3[Cu(4,4'-bpy)2],2[W(CN)8],6(DMF),2(H2O)
_chemical_formula_sum            'C64 H70 Cu3 N28 O8 W2'
_chemical_formula_weight         1917.80
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.6167(1)
_cell_length_b                   19.0794(3)
_cell_length_c                   11.1204(4)
_cell_measurement_reflns_used    3613
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.753
_cell_volume                     3737.75(15)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL DENZO and Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1999)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al, 1994)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\f and \w scans to fill Ewald sphere'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.046
_diffrn_reflns_av_sigmaI/netI    0.032
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    3.977
_exptl_absorpt_correction_T_max  0.7682
_exptl_absorpt_correction_T_min  0.2677
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1898
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.726
_refine_diff_density_min         -1.619
_refine_diff_density_rms         0.250
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.283
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         6555
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.283
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0273
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0516P)^2^+0.2858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0865
_reflns_number_gt                6386
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049402osi20040507_055914.cif
_cod_data_source_block           1
_cod_database_code               4311402
_diffrn_reflns_number_total      22809
_reflns_number_unique            6555