#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/26/4322626.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4322626
loop_
_publ_author_name
'P. Shiv Halasymani'
'Kevin R. Heier'
'Alexander J. Norquist'
'Charlotte L. Stern'
'Kenneth R. Poeppelmeier'
_publ_contact_author
;
Poeppelmeier, Kenneth R.
Department of Chemistry
Northwestern University
Evanston, Illinois 60208-3113
;
_publ_contact_author_email       krp@nwu.edu
_publ_contact_author_fax         '(847) 491-7713'
_publ_contact_author_phone       '(847) 491-3505'
_publ_section_title
;
 Composition Space of the (CdO, 0.5Nb2O5)/(HF)x.Pyridine/H2O System.
 Structure and Synthesis of CdNb(py)4OF5
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              369
_journal_page_last               371
_journal_paper_doi               10.1021/ic971224u
_journal_volume                  37
_journal_year                    1998
_chemical_formula_moiety         'C20 H20 Cd F5 N4 Nb O '
_chemical_formula_sum            'C20 H20 Cd F5 N4 Nb O'
_chemical_formula_weight         632.71
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_date             'Fri Jul 18 09:48:59 1997'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 97.11(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.993(1)
_cell_length_b                   10.733(1)
_cell_length_c                   16.878(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    153.2
_cell_measurement_theta_max      11.9
_cell_measurement_theta_min      11.0
_cell_volume                     2335.6(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SHELXS86
_diffrn_ambient_temperature      153.2
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       'omega/theta scans'
_diffrn_orient_matrix_UB_11      -0.02130
_diffrn_orient_matrix_UB_12      0.08924
_diffrn_orient_matrix_UB_13      -0.00705
_diffrn_orient_matrix_UB_21      -0.01784
_diffrn_orient_matrix_UB_22      -0.01408
_diffrn_orient_matrix_UB_23      -0.05866
_diffrn_orient_matrix_UB_31      -0.07242
_diffrn_orient_matrix_UB_32      -0.02275
_diffrn_orient_matrix_UB_33      0.00861
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  .0228
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4534
_diffrn_reflns_theta_max         24.97
_diffrn_standards_decay_%        -2.09
_diffrn_standards_interval_count 90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.461
_exptl_absorpt_correction_T_max  0.832
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   Tompa_analytical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.799
_exptl_crystal_density_meas      1.78(2)
_exptl_crystal_density_method    'flotation pycnometry'
_exptl_crystal_description       platey
_exptl_crystal_F_000             1240.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.140
_refine_diff_density_max         1.18
_refine_diff_density_min         -0.63
_refine_ls_extinction_coef       2.19778
_refine_ls_extinction_method     Zachariasen_type_2_Gaussian_isotropic
_refine_ls_goodness_of_fit_obs   2.093
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         3685
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0258
_refine_ls_shift/esd_max         0.0035
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0306
_reflns_number_observed          3685
_reflns_number_total             2163
_reflns_observed_criterion       3.00
_cod_data_source_file            ic971224u.cif
_cod_data_source_block           S72-IC971224U
_cod_original_cell_volume        2335.6(4)
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_original_formula_sum        'C20 H20 Cd F5 N4 Nb O '
_cod_database_code               4322626
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'1/2+x,1/2+y,   +z'
'   -x,   +y,1/2-z'
1/2-x,1/2+y,1/2-z
'   -x,   -y,   -z'
'1/2-x,1/2-y,   -z'
'   +x,   -y,1/2+z'
1/2+x,1/2-y,1/2+z
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
_atom_site_calc_flag
_atom_site_calc_attached_atom
Cd(1) 0.250 0.250 0.500 0.02290(6) Uij ? ?
Nb(1) 0.000 0.000 0.500 0.03077(8) Uij ? ?
F(1) 0.111 0.118 0.498 0.029 Uij ? ?
F(2) -0.0957(1) 0.1209(1) 0.45287(9) 0.0429(4) Uij ? ?
F(3) -0.0223(1) 0.0573(1) 0.60492(8) 0.0388(4) Uij ? ?
O(1) 0.1110(1) 0.1182(1) 0.49781(7) 0.0294(4) Uij ? ?
N(1) 0.2464(1) 0.2222(2) 0.3614(1) 0.0258(5) Uij ? ?
N(2) 0.3593(2) 0.0832(2) 0.5401(1) 0.0324(5) Uij ? ?
C(1) 0.1761(2) 0.1488(2) 0.3194(1) 0.0320(6) Uij ? ?
C(2) 0.1584(2) 0.1499(2) 0.2373(1) 0.0357(7) Uij ? ?
C(3) 0.2163(2) 0.2293(2) 0.1959(1) 0.0399(7) Uij ? ?
C(4) 0.2898(2) 0.3039(2) 0.2383(1) 0.0393(7) Uij ? ?
C(5) 0.3016(2) 0.2990(2) 0.3205(1) 0.0303(6) Uij ? ?
C(6) 0.4470(2) 0.1008(2) 0.5888(2) 0.0431(8) Uij ? ?
C(7) 0.5030(2) 0.0049(3) 0.6256(2) 0.062(1) Uij ? ?
C(8) 0.4690(3) -0.1160(3) 0.6096(2) 0.071(1) Uij ? ?
C(9) 0.3807(3) -0.1355(3) 0.5586(2) 0.065(1) Uij ? ?
C(10) 0.3280(2) -0.0338(2) 0.5255(2) 0.0449(8) Uij ? ?
H(1) 0.137 0.093 0.348 0.038 Uij ? ?
H(2) 0.107 0.097 0.209 0.043 Uij ? ?
H(3) 0.206 0.232 0.139 0.048 Uij ? ?
H(4) 0.332 0.358 0.211 0.047 Uij ? ?
H(5) 0.351 0.352 0.349 0.036 Uij ? ?
H(6) 0.471 0.184 0.598 0.052 Uij ? ?
H(7) 0.564 0.021 0.662 0.075 Uij ? ?
H(8) 0.507 -0.185 0.634 0.085 Uij ? ?
H(9) 0.356 -0.217 0.546 0.079 Uij ? ?
H(10) 0.266 -0.047 0.490 0.053 Uij ? ?
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Nb 0 4 -2.073 0.621 'International Tables'
F 0 20 0.017 0.010 'International Tables'
O 0 4 0.011 0.006 'International Tables'
C 0 80 0.003 0.002 'International Tables'
N 0 16 0.006 0.003 'International Tables'
H 0 80 0.000 0.000 'International Tables'
Cd 0 4 -0.807 1.202 'International Tables'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-4 4 6
4 4 4
3 3 -8
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F(1) Cd(1) F(1) 180.0 ? ? ? yes
F(1) Cd(1) N(1) 89.25(4) ? ? ? yes
F(1) Cd(1) N(1) 90.75(4) ? ? ? yes
F(1) Cd(1) N(2) 88.93(5) ? ? ? yes
F(1) Cd(1) N(2) 91.07(5) ? ? ? yes
F(1) Cd(1) N(1) 90.75(4) ? ? ? yes
F(1) Cd(1) N(1) 89.25(4) ? ? ? yes
F(1) Cd(1) N(2) 91.07(5) ? ? ? yes
F(1) Cd(1) N(2) 88.93(5) ? ? ? yes
N(1) Cd(1) N(1) 180.0 ? ? ? yes
N(1) Cd(1) N(2) 97.33(7) ? ? ? yes
N(1) Cd(1) N(2) 82.67(7) ? ? ? yes
N(1) Cd(1) N(2) 82.67(7) ? ? ? yes
N(1) Cd(1) N(2) 97.33(7) ? ? ? yes
N(2) Cd(1) N(2) 180.0 ? ? ? yes
F(1) Nb(1) F(1) 180.0 ? ? ? yes
F(1) Nb(1) F(2) 89.71(4) ? ? ? yes
F(1) Nb(1) F(2) 90.29(4) ? ? ? yes
F(1) Nb(1) F(3) 90.33(4) ? ? ? yes
F(1) Nb(1) F(3) 89.67(4) ? ? ? yes
F(1) Nb(1) F(2) 90.29(4) ? ? ? yes
F(1) Nb(1) F(2) 89.71(4) ? ? ? yes
F(1) Nb(1) F(3) 89.67(4) ? ? ? yes
F(1) Nb(1) F(3) 90.33(4) ? ? ? yes
F(2) Nb(1) F(2) 180.0 ? ? ? yes
F(2) Nb(1) F(3) 90.08(7) ? ? ? yes
F(2) Nb(1) F(3) 89.92(7) ? ? ? yes
F(2) Nb(1) F(3) 89.92(7) ? ? ? yes
F(2) Nb(1) F(3) 90.08(7) ? ? ? yes
F(3) Nb(1) F(3) 180.0 ? ? ? yes
Cd(1) F(1) Nb(1) 176.3021(1) ? ? ? yes
Cd(1) O(1) Nb(1) 176.30(7) ? ? ? yes
Cd(1) N(1) C(1) 121.9(1) ? ? ? yes
Cd(1) N(1) C(5) 119.2(1) ? ? ? yes
C(1) N(1) C(5) 117.6(2) ? ? ? yes
Cd(1) N(2) C(6) 120.8(2) ? ? ? yes
Cd(1) N(2) C(10) 120.5(2) ? ? ? yes
C(6) N(2) C(10) 117.8(2) ? ? ? yes
N(1) C(1) C(2) 123.0(2) ? ? ? yes
C(1) C(2) C(3) 118.7(2) ? ? ? yes
C(2) C(3) C(4) 118.7(2) ? ? ? yes
C(3) C(4) C(5) 119.1(2) ? ? ? yes
N(1) C(5) C(4) 122.8(2) ? ? ? yes
N(2) C(6) C(7) 122.7(3) ? ? ? yes
C(6) C(7) C(8) 118.6(3) ? ? ? yes
C(7) C(8) C(9) 119.3(3) ? ? ? yes
C(8) C(9) C(10) 118.3(3) ? ? ? yes
N(2) C(10) C(9) 123.3(3) ? ? ? yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd(1) F(1) 2.2909(1) ? ? yes
Cd(1) F(1) 2.2909(1) ? ? yes
Cd(1) N(1) 2.354(2) ? ? yes
Cd(1) N(1) 2.354(2) ? ? yes
Cd(1) N(2) 2.333(2) ? ? yes
Cd(1) N(2) 2.333(2) ? ? yes
Nb(1) F(1) 1.9245(1) ? ? yes
Nb(1) F(1) 1.9245(1) ? ? yes
Nb(1) F(2) 1.902(1) ? ? yes
Nb(1) F(2) 1.902(1) ? ? yes
Nb(1) F(3) 1.930(1) ? ? yes
Nb(1) F(3) 1.930(1) ? ? yes
N(1) C(1) 1.340(3) ? ? yes
N(1) C(5) 1.339(3) ? ? yes
N(2) C(6) 1.333(3) ? ? yes
N(2) C(10) 1.333(3) ? ? yes
C(1) C(2) 1.377(3) ? ? yes
C(2) C(3) 1.382(4) ? ? yes
C(3) C(4) 1.377(4) ? ? yes
C(4) C(5) 1.377(3) ? ? yes
C(6) C(7) 1.365(4) ? ? yes
C(7) C(8) 1.387(5) ? ? yes
C(8) C(9) 1.363(5) ? ? yes
C(9) C(10) 1.370(4) ? ? yes
