Tetraaquatetrakis(4,4'-bipyridine dioxide-κ<i>O</i>)terbium(III) octacyanidomolybdate(V)
Qian, Su-Yan; Yuan, Ai-Hua; Acta Crystallographica Section E 67 (2011) m845–; doi:10.1107/S1600536811020022

data_2230578
_publ_section_title
;
 Tetraaquatetrakis(4,4'-bipyridine dioxide-\k<i>O</i>)terbium(III)
 octacyanidomolybdate(V)
;
_journal_coeditor_code           BT5505
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m845
_journal_paper_doi               10.1107/S1600536811020022
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Tb (C10 H8 N2 O2)4 (H2 O)4] [Mo (C N)8]'
_chemical_formula_moiety         'C40 H40 N8 O12 Tb 3+, C8 Mo N8 3-'
_chemical_formula_sum            'C48 H40 Mo N16 O12 Tb'
_chemical_formula_weight         1287.72
_chemical_name_systematic
;
Tetraaquatetrakis(4,4'-bipyridine dioxide-\k<i>O</i>)terbium(III)
octacyanidomolybdate(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                   17.9226(7)
_cell_length_b                   17.9226(7)
_cell_length_c                   7.8877(6)
_cell_measurement_reflns_used    9881
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.27
_cell_volume                     2533.7(2)
_computing_cell_refinement       'SAINT (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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0143
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            21243
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    1.711
_exptl_absorpt_correction_T_max  0.843
_exptl_absorpt_correction_T_min  0.693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1286
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.287
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2921
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0176
_refine_ls_R_factor_gt           0.0158
_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^)+(0.0183P)^2^+1.8165P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0416
_refine_ls_wR_factor_ref         0.0429
_reflns_number_gt                2730
_reflns_number_total             2921
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt5505.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               2230578
_cod_database_fobs_code          2230578