Tetraaquatetrakis(4,4'-bipyridine dioxide-κ<i>O</i>)terbium(III) octacyanidotungstate(V)
Shi, Yu-Sheng; Ran, Mao-Qian; Chen, Ying-Ying; Yuan, Ai-Hua; Acta Crystallographica Section E 68 (2012) m288–; doi:10.1107/S1600536812005004

data_2233763
_publ_section_title
;
 Tetraaquatetrakis(4,4'-bipyridine dioxide-\k<i>O</i>)terbium(III)
 octacyanidotungstate(V)
;
_journal_coeditor_code           BX2386
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m288
_journal_paper_doi               10.1107/S1600536812005004
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Tb (C10 H8 N2 O2)4 (H2 O)4] [W (C N)8]'
_chemical_formula_moiety         'C40 H40 N8 O12 Tb 3+, C8 N8 W 3-'
_chemical_formula_sum            'C48 H40 N16 O12 Tb W'
_chemical_formula_weight         1375.73
_chemical_name_systematic
;
Tetraaquatetrakis(4,4'-bipyridine dioxide-\k<i>O</i>)terbium(III)
octacyanidotungstate(V)
;
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :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                   17.9222(7)
_cell_length_b                   17.9222(7)
_cell_length_c                   7.8915(6)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.27
_cell_volume                     2534.8(2)
_computing_cell_refinement       'SMART (Bruker, 2004)'
_computing_data_collection       'SMART (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\f and \w 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  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0168
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            19073
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    3.731
_exptl_absorpt_correction_T_max  0.5224
_exptl_absorpt_correction_T_min  0.4438
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.802
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1350
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.635
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2498
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0158
_refine_ls_R_factor_gt           0.0138
_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^)+(0.0164P)^2^+1.7030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0360
_refine_ls_wR_factor_ref         0.0370
_reflns_number_gt                2299
_reflns_number_total             2498
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bx2386.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               2233763
_cod_database_fobs_code          2233763