#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/54/2005463.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_2005463
loop_
_publ_author_name
'Halasyamani, P.'
'Willis, M. J.'
'Heier, K. R.'
'Stern, C. L.'
'Poeppelmeier, K. R.'
_publ_contact_author
;
    Poeppelmeier, Kenneth
    Department of Chemistry
    Northwestern University
    Evanston, Illinois 60208-3113
    USA
;
_publ_section_title
;
 [pyH⁺]₂[CdNb₂(py)₄O₂F₁₀]^2{-^}
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2491
_journal_page_last               2493
_journal_paper_doi               10.1107/S0108270196007573
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          '(C5 H6 N)2 [Cd Nb2 F10 O2(C5 H5 N)4]'
_chemical_formula_moiety         'C30 H32 Cd F10 N6 Nb2 O2'
_chemical_formula_sum            'C30 H32 Cd F10 N6 Nb2 O2'
_chemical_formula_weight         996.83
_space_group_IT_number           98
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4bw 2bw'
_symmetry_space_group_name_H-M   'I 41 2 2'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.490(2)
_cell_length_b                   11.490(2)
_cell_length_c                   30.906(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    153.2
_cell_measurement_theta_max      12.08
_cell_measurement_theta_min      10.01
_cell_volume                     4080.2(11)
_computing_cell_refinement       'DIRDIF (Beurskens et al., 1992)'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1992)'
_computing_publication_material  TEXSAN
_computing_structure_refinement  TEXSAN
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      153.2
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       'ω/θ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            2043
_diffrn_reflns_theta_max         24.97
_diffrn_standards_decay_%        1.15
_diffrn_standards_interval_count 90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.148
_exptl_absorpt_correction_T_max  0.836
_exptl_absorpt_correction_T_min  0.632
_exptl_absorpt_correction_type   'analytical (de Meulenaer & Tompa, 1965)'
_exptl_absorpt_process_details   Tompa_analytical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.62
_exptl_crystal_density_meas      1.61(1)
_exptl_crystal_density_method    'flotation pycnometry'
_exptl_crystal_description       faceted
_exptl_crystal_F_000             1960.00
_exptl_crystal_size_max          0.386
_exptl_crystal_size_mid          0.258
_exptl_crystal_size_min          0.172
_refine_diff_density_max         0.60
_refine_diff_density_min         -0.57
_refine_ls_extinction_coef       0.85668
_refine_ls_extinction_method     Zachariasen_(1968)_type_2_Gaussian_isotropic
_refine_ls_goodness_of_fit_obs   2.350
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         982
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0245
_refine_ls_shift/esd_max         0.2180
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0289
_reflns_number_observed          982
_reflns_number_total             1098
_reflns_observed_criterion       >3\s(I)
_cod_data_source_file            bk1219.cif
_cod_data_source_block           BK1219
_cod_depositor_comments
;

  Replacing the provided, obviously errorneous symmetry operator list
  (e.g. it contains duplicate symmetry operators like '-y,-x,-z') with
  the symmetry operators for the declared spacegroup 'I 41 2 2'. This
  yields consistent composition computed in different ways from the
  coordinates, but the computed composition is different from the
  provided in the _chemical_formula_sum data item (heavy atom count
  differs).

  Saulius Gra\<zulis
  2014-06-18

;
_cod_original_cell_volume        4080.2(9)
_cod_original_sg_symbol_H-M      'I 41 2 2   '
_cod_original_formula_sum        'C30 H32 Cd F10 N6 Nb2 O2 '
_cod_database_code               2005463
loop_
_symmetry_equiv_pos_as_xyz
X,Y,Z
1/2-X,1/2-Y,1/2+Z
-Y,1/2+X,1/4+Z
1/2+Y,-X,3/4+Z
1/2-X,Y,3/4-Z
X,1/2-Y,1/4-Z
1/2+Y,1/2+X,1/2-Z
-Y,-X,-Z
1/2+X,1/2+Y,1/2+Z
-X,-Y,Z
1/2-Y,X,3/4+Z
Y,1/2-X,1/4+Z
-X,1/2+Y,1/4-Z
1/2+X,-Y,3/4-Z
Y,X,-Z
1/2-Y,1/2-X,1/2-Z
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Cd 0.0116(2) 0.0116 0.0161(3) -0.0016(3) 0.0000 0.0000
Nb 0.0116(2) 0.0116 0.0200(3) -0.0020(3) -0.0001 0.0001(2)
F(1) 0.015(2) 0.022(2) 0.036(2) 0.0020(10) 0.000(2) -0.001(2)
F(2) 0.029(2) 0.029(2) 0.0250(10) 0.002(2) -0.0110(10) -0.0080(10)
F(3) 0.021(2) 0.0209 0.131(5) -0.009(2) -0.0038 0.004(4)
O(1) 0.010(2) 0.0103 0.022(3) 0.003(2) -0.0013 0.001(3)
N(1) 0.024(4) 0.027(4) 0.017(2) -0.005(4) 0.0000 0.0000
N(2) 0.014(2) 0.0144 0.029(4) -0.005(3) -0.0035 -0.004(5)
C(1) 0.054(6) 0.058(6) 0.024(3) -0.044(3) 0.010(5) -0.002(5)
C(2) 0.072(7) 0.064(7) 0.022(3) -0.045(4) -0.004(7) -0.008(6)
C(3) 0.050(10) 0.050(10) 0.016(3) -0.028(6) 0.0000 0.0000
C(4) 0.024(3) 0.018(3) 0.085(6) 0.002(3) -0.001(5) -0.015(4)
C(5) 0.014(3) 0.031(4) 0.107(7) 0.004(3) -0.012(5) 0.000(5)
C(6) 0.024(3) 0.0245 0.054(5) 0.007(4) -0.0057 -0.006(5)
C(7) 0.055(5) 0.057(5) 0.027(3) -0.034(3) -0.001(7) 0.002(7)
C(8) 0.080(10) 0.090(10) 0.020(3) -0.052(4) -0.008(5) 0.001(5)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
Cd 0.5000 0.5000 0.5000 0.01311(9) Uani
Nb 0.75125(4) 0.7513 0.5000 0.01439(8) Uani
F(1) 0.8800(3) 0.6446(3) 0.4933(1) 0.0245(9) Uani
F(2) 0.7785(3) 0.7516(3) 0.56182(9) 0.0279(9) Uani
F(3) 0.8802(3) 0.8802 0.5000 0.058(1) Uani
O(1) 0.6436(4) 0.6436 0.5000 0.0142(8) Uani
N(1) 0.5000 0.5000 0.5755(1) 0.022(2) Uani
N(2) 0.3548(5) 0.6452 0.5000 0.019(1) Uani
N(3) 0.9593(7) 0.9576(8) 0.4160(2) 0.034(1) iso
C(1) 0.5700(8) 0.5685(8) 0.5978(2) 0.045(2) Uani
C(2) 0.573(1) 0.571(1) 0.6425(2) 0.052(3) Uani
C(3) 0.5000 0.5000 0.6652(2) 0.037(4) Uani
C(4) 0.2428(5) 0.6198(5) 0.4941(4) 0.042(2) Uani
C(5) 0.1552(5) 0.7016(6) 0.4951(4) 0.051(2) Uani
C(6) 0.1839(5) 0.8161 0.5000 0.034(1) Uani
C(7) 0.9201(9) 0.9135(9) 0.3785(2) 0.046(2) Uani
C(8) 0.959(1) 0.957(1) 0.3399(2) 0.062(5) Uani
C(9) 0.9593 0.9576 0.4160 0.0339 iso
H(1) 0.6216 0.6186 0.5820 0.0507 equiv
H(2) 0.6245 0.6233 0.6576 0.0507 equiv
H(3) 0.5000 0.5000 0.6962 0.0507 equiv
H(4) 0.2224 0.5409 0.4874 0.0507 equiv
H(5) 0.0748 0.6787 0.4953 0.0507 equiv
H(6) 0.1246 0.8754 0.5000 0.0507 equiv
H(7) 0.8637 0.8508 0.3783 0.0507 equiv
H(8) 0.9290 0.9272 0.3130 0.0507 equiv
H(9) 0.9310 0.9271 0.4430 0.0507 equiv
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cd -0.807 1.202 'International Tables'
Nb -2.073 0.621 'International Tables'
F 0.017 0.010 'International Tables'
N 0.006 0.003 'International Tables'
C 0.003 0.002 'International Tables'
H 0.000 0.000 'International Tables'
O 0.011 0.006 'International Tables'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
5 1 12
-2 3 15
-4 -4 4
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O(1) Cd O(1) 11_666 180.0 no
O(1) Cd O(1) 3_665 180.0 no
O(1) Cd N(1) ? 90.0 yes
O(1) Cd N(2) ? 90.000(10) yes
O(1) Cd N(1) ? 90.0 no
O(1) Cd N(2) ? 90.000(10) no
N(1) Cd N(1) 11_666 180.0 no
N(1) Cd N(1) 9_556 180.0 no
N(1) Cd N(2) ? 90.0 yes
N(2) Cd N(2) 3_665 180.0 no
N(2) Cd N(2) 9_556 180.0 no
F(1) Nb F(1) 9_556 169.3(2) yes
F(1) Nb F(2) ? 89.00(10) yes
F(1) Nb F(2) 9_556 89.80(10) yes
F(1) Nb F(3) ? 84.70(10) yes
F(1) Nb O(1) ? 95.30(10) yes
F(2) Nb F(2) 9_556 166.7(2) yes
F(2) Nb F(3) ? 83.30(10) yes
F(2) Nb O(1) ? 96.60(10) yes
F(3) Nb O(1) ? 180.0 yes
Cd O(1) Nb ? 180.0 yes
Cd N(1) C(1) ? 121.4(3) no
C(1) N(1) C(1) 3_665 117.2(5) no
Cd N(2) C(4) ? 121.9(4) no
C(4) N(2) C(4) 11_666 116.2(7) no
N(3) N(3) C(7) ? 120.3(3) no
N(1) C(1) C(2) ? 123.2(5) no
C(1) C(2) C(3) ? 119.2(5) no
C(2) C(3) C(2) ? 118.2(6) no
N(2) C(4) C(5) ? 123.6(6) no
C(4) C(5) C(6) ? 118.9(6) no
C(5) C(6) C(5) ? 118.5(8) no
N(3) C(7) C(8) ? 120.2(5) no
C(7) C(8) C(8) ? 119.5(3) no
N(3) C(9) C(7) ? 120.3(3) no
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
Cd O(1) ? 2.333(6) yes
Cd N(1) ? 2.335(4) yes
Cd N(2) ? 2.359(8) yes
Nb F(1) ? 1.932(3) yes
Nb F(2) ? 1.936(3) yes
Nb F(3) ? 2.095(4) yes
Nb O(1) ? 1.750(6) yes
N(1) C(1) ? 1.318(6) no
N(2) C(4) ? 1.332(7) no
N(3) N(3) 4_775 1.351(9) no
N(3) C(7) ? 1.344(7) no
C(1) C(2) ? 1.384(8) no
C(2) C(3) ? 1.361(7) no
C(4) C(5) ? 1.378(9) no
C(5) C(6) ? 1.365(8) no
C(7) C(8) ? 1.368(8) no
C(8) C(8) 4_775 1.360(10) no
