#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/05/2230578.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2230578
loop_
_publ_author_name
'Qian, Su-Yan'
'Yuan, Ai-Hua'
_publ_section_title
;
 Tetraaquatetrakis(4,4'-bipyridine dioxide-κO)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-κO)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       'φ and ω'
_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/[σ²(Fo²)+(0.0183P)²+1.8165P] where P=(Fo²+2Fc²)/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>2σ(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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+1/2, x, z'
'-x+1/2, -y+1/2, z'
'y, -x+1/2, z'
'-x, -y, -z'
'y-1/2, -x, -z'
'x-1/2, y-1/2, -z'
'-y, x-1/2, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb Tb1 0.7500 0.2500 0.0000 0.01136(5) Uani d S 1 4 . .
Mo Mo1 0.7500 0.7500 -0.24987(4) 0.02019(7) Uani d S 1 4 . .
O O1 0.64962(6) 0.17736(7) 0.10113(14) 0.0251(3) Uani d . 1 1 . .
O O2 0.27973(7) -0.11246(7) -0.50459(14) 0.0223(2) Uani d . 1 1 . .
O O3 0.70614(6) 0.31664(6) 0.24591(13) 0.0183(2) Uani d . 1 1 . .
N N1 0.60473(10) 0.81932(10) -0.4592(3) 0.0422(4) Uani d . 1 1 . .
N N2 0.59644(10) 0.70470(10) -0.0373(3) 0.0393(4) Uani d . 1 1 . .
N N3 0.60104(8) 0.13848(8) 0.00837(16) 0.0201(3) Uani d . 1 1 . .
N N4 0.33441(7) -0.07064(7) -0.44088(17) 0.0176(2) Uani d . 1 1 . .
C C1 0.65693(10) 0.79577(9) -0.3922(3) 0.0300(4) Uani d . 1 1 . .
C C2 0.65123(10) 0.71973(9) -0.1057(3) 0.0293(4) Uani d . 1 1 . .
C C3 0.62224(9) 0.07458(9) -0.0674(2) 0.0234(3) Uani d . 1 1 . .
H H3 0.6709 0.0575 -0.0537 0.028 Uiso calc R 1 1 . .
C C4 0.57297(9) 0.03404(9) -0.1648(2) 0.0215(3) Uani d . 1 1 . .
H H4 0.5888 -0.0098 -0.2166 0.026 Uiso calc R 1 1 . .
C C5 0.49930(8) 0.05822(8) -0.1867(2) 0.0175(3) Uani d . 1 1 . .
C C6 0.47918(9) 0.12409(9) -0.1031(2) 0.0248(3) Uani d . 1 1 . .
H H6 0.4306 0.1419 -0.1129 0.030 Uiso calc R 1 1 . .
C C7 0.53013(10) 0.16301(10) -0.0063(2) 0.0257(4) Uani d . 1 1 . .
H H7 0.5155 0.2064 0.0491 0.031 Uiso calc R 1 1 . .
C C8 0.44383(8) 0.01450(8) -0.28394(19) 0.0168(3) Uani d . 1 1 . .
C C9 0.45913(8) -0.05724(8) -0.3460(2) 0.0182(3) Uani d . 1 1 . .
H H9 0.5070 -0.0768 -0.3356 0.022 Uiso calc R 1 1 . .
C C10 0.40389(8) -0.09908(8) -0.4224(2) 0.0189(3) Uani d . 1 1 . .
H H10 0.4144 -0.1469 -0.4613 0.023 Uiso calc R 1 1 . .
C C12 0.37208(9) 0.04249(8) -0.3126(2) 0.0209(3) Uani d . 1 1 . .
H H12 0.3604 0.0907 -0.2780 0.025 Uiso calc R 1 1 . .
C C13 0.31847(9) -0.00028(9) -0.3913(2) 0.0217(3) Uani d . 1 1 . .
H H13 0.2712 0.0193 -0.4103 0.026 Uiso calc R 1 1 . .
H H3WA 0.6727 0.3040 0.3134 0.033 Uiso d R 1 1 . .
H H3WB 0.7363 0.3368 0.3136 0.033 Uiso d R 1 1 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Tb1 O1 8_655 3_655 96.562(17) ?
O1 Tb1 O1 8_655 . 96.562(17) ?
O1 Tb1 O1 3_655 . 140.48(5) ?
O1 Tb1 O1 8_655 6_665 140.48(5) ?
O1 Tb1 O1 3_655 6_665 96.562(17) ?
O1 Tb1 O1 . 6_665 96.562(17) ?
O1 Tb1 O3 8_655 8_655 75.68(4) ?
O1 Tb1 O3 3_655 8_655 146.10(4) ?
O1 Tb1 O3 . 8_655 73.39(4) ?
O1 Tb1 O3 6_665 8_655 72.73(4) ?
O1 Tb1 O3 8_655 3_655 73.39(4) ?
O1 Tb1 O3 3_655 3_655 75.68(4) ?
O1 Tb1 O3 . 3_655 72.73(4) ?
O1 Tb1 O3 6_665 3_655 146.10(4) ?
O3 Tb1 O3 8_655 3_655 130.38(3) ?
O1 Tb1 O3 8_655 . 146.10(4) ?
O1 Tb1 O3 3_655 . 72.73(4) ?
O1 Tb1 O3 . . 75.68(4) ?
O1 Tb1 O3 6_665 . 73.39(4) ?
O3 Tb1 O3 8_655 . 130.38(3) ?
O3 Tb1 O3 3_655 . 72.79(5) ?
O1 Tb1 O3 8_655 6_665 72.73(4) ?
O1 Tb1 O3 3_655 6_665 73.39(4) ?
O1 Tb1 O3 . 6_665 146.10(4) ?
O1 Tb1 O3 6_665 6_665 75.68(4) ?
O3 Tb1 O3 8_655 6_665 72.79(5) ?
O3 Tb1 O3 3_655 6_665 130.38(3) ?
O3 Tb1 O3 . 6_665 130.38(3) ?
C1 Mo1 C1 2_655 . 74.50(5) ?
C1 Mo1 C1 2_655 4_565 117.74(11) ?
C1 Mo1 C1 . 4_565 74.50(5) ?
C1 Mo1 C1 2_655 3_665 74.50(5) ?
C1 Mo1 C1 . 3_665 117.74(11) ?
C1 Mo1 C1 4_565 3_665 74.50(5) ?
C1 Mo1 C2 2_655 2_655 74.88(7) ?
C1 Mo1 C2 . 2_655 140.36(6) ?
C1 Mo1 C2 4_565 2_655 143.33(6) ?
C1 Mo1 C2 3_665 2_655 76.77(7) ?
C1 Mo1 C2 2_655 . 76.77(7) ?
C1 Mo1 C2 . . 74.88(7) ?
C1 Mo1 C2 4_565 . 140.36(6) ?
C1 Mo1 C2 3_665 . 143.33(6) ?
C2 Mo1 C2 2_655 . 74.10(5) ?
C1 Mo1 C2 2_655 3_665 140.36(6) ?
C1 Mo1 C2 . 3_665 143.33(6) ?
C1 Mo1 C2 4_565 3_665 76.77(7) ?
C1 Mo1 C2 3_665 3_665 74.88(7) ?
C2 Mo1 C2 2_655 3_665 74.10(5) ?
C2 Mo1 C2 . 3_665 116.87(11) ?
C1 Mo1 C2 2_655 4_565 143.33(6) ?
C1 Mo1 C2 . 4_565 76.77(7) ?
C1 Mo1 C2 4_565 4_565 74.88(7) ?
C1 Mo1 C2 3_665 4_565 140.36(6) ?
C2 Mo1 C2 2_655 4_565 116.87(11) ?
C2 Mo1 C2 . 4_565 74.10(5) ?
C2 Mo1 C2 3_665 4_565 74.10(5) ?
N3 O1 Tb1 . . 126.90(9) ?
Tb1 O3 H3WA . . 128.0 ?
Tb1 O3 H3WB . . 120.9 ?
H3WA O3 H3WB . . 100.0 ?
O1 N3 C3 . . 120.24(14) ?
O1 N3 C7 . . 119.45(14) ?
C3 N3 C7 . . 120.30(14) ?
O2 N4 C13 . . 118.60(13) ?
O2 N4 C10 . . 120.38(13) ?
C13 N4 C10 . . 121.00(13) ?
N1 C1 Mo1 . . 175.79(19) ?
N2 C2 Mo1 . . 176.07(18) ?
N3 C3 C4 . . 121.02(15) ?
N3 C3 H3 . . 119.5 ?
C4 C3 H3 . . 119.5 ?
C3 C4 C5 . . 120.65(15) ?
C3 C4 H4 . . 119.7 ?
C5 C4 H4 . . 119.7 ?
C6 C5 C4 . . 116.49(14) ?
C6 C5 C8 . . 121.17(14) ?
C4 C5 C8 . . 122.23(14) ?
C7 C6 C5 . . 121.10(15) ?
C7 C6 H6 . . 119.4 ?
C5 C6 H6 . . 119.4 ?
N3 C7 C6 . . 120.42(16) ?
N3 C7 H7 . . 119.8 ?
C6 C7 H7 . . 119.8 ?
C12 C8 C9 . . 116.87(14) ?
C12 C8 C5 . . 120.77(13) ?
C9 C8 C5 . . 122.32(13) ?
C10 C9 C8 . . 120.66(14) ?
C10 C9 H9 . . 119.7 ?
C8 C9 H9 . . 119.7 ?
N4 C10 C9 . . 120.16(14) ?
N4 C10 H10 . . 119.9 ?
C9 C10 H10 . . 119.9 ?
C13 C12 C8 . . 120.98(14) ?
C13 C12 H12 . . 119.5 ?
C8 C12 H12 . . 119.5 ?
N4 C13 C12 . . 120.17(14) ?
N4 C13 H13 . . 119.9 ?
C12 C13 H13 . . 119.9 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Tb1 O1 8_655 2.3596(11) ?
Tb1 O1 3_655 2.3596(11) ?
Tb1 O1 . 2.3596(11) ?
Tb1 O1 6_665 2.3596(11) ?
Tb1 O3 8_655 2.4097(10) ?
Tb1 O3 3_655 2.4097(10) ?
Tb1 O3 . 2.4097(10) ?
Tb1 O3 6_665 2.4097(10) ?
Mo1 C1 2_655 2.1715(18) ?
Mo1 C1 . 2.1715(18) ?
Mo1 C1 4_565 2.1715(18) ?
Mo1 C1 3_665 2.1715(18) ?
Mo1 C2 2_655 2.1731(18) ?
Mo1 C2 . 2.1731(18) ?
Mo1 C2 3_665 2.1731(18) ?
Mo1 C2 4_565 2.1731(18) ?
O1 N3 . 1.3338(17) ?
O2 N4 . 1.3323(16) ?
O3 H3WA . 0.8326 ?
O3 H3WB . 0.8422 ?
N1 C1 . 1.155(2) ?
N2 C2 . 1.152(2) ?
N3 C3 . 1.346(2) ?
N3 C7 . 1.350(2) ?
N4 C13 . 1.351(2) ?
N4 C10 . 1.3533(19) ?
C3 C4 . 1.378(2) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.400(2) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.400(2) ?
C5 C8 . 1.480(2) ?
C6 C7 . 1.379(2) ?
C6 H6 . 0.9300 ?
C7 H7 . 0.9300 ?
C8 C12 . 1.399(2) ?
C8 C9 . 1.403(2) ?
C9 C10 . 1.380(2) ?
C9 H9 . 0.9300 ?
C10 H10 . 0.9300 ?
C12 C13 . 1.377(2) ?
C12 H12 . 0.9300 ?
C13 H13 . 0.9300 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O3 H3WA O2 2_556 0.83 1.85 2.6702(15) 169
O3 H3WB O2 7_665 0.84 1.92 2.7417(16) 164
O3 H3WB N4 7_665 0.84 2.62 3.4251(16) 161
