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#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/86/2018695.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_2018695
loop_
_publ_author_name
'Feldmann, Claus'
'Freudenmann, Dominic'
_publ_section_title
;
 [Te₈][NbOCl₄]₂ containing an infinite chain-like
 {[Te--Te--Te--(Te₅)]²⁺}ₙ polycation
;
_journal_coeditor_code           YP3015
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              i68
_journal_page_last               i70
_journal_paper_doi               10.1107/S0108270112038176
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Te8] [Nb O Cl4]2'
_chemical_formula_moiety         'Te8 2+, 2(Cl4 Nb O -)'
_chemical_formula_sum            'Cl8 Nb2 O2 Te8'
_chemical_formula_weight         1522.22
_chemical_name_systematic        ?
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                80.85(3)
_cell_angle_beta                 82.17(3)
_cell_angle_gamma                78.84(3)
_cell_formula_units_Z            2
_cell_length_a                   7.8670(16)
_cell_length_b                   12.049(2)
_cell_length_c                   12.481(3)
_cell_measurement_reflns_used    1058
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      60.0
_cell_measurement_theta_min      3.0
_cell_volume                     1139.1(4)
_computing_cell_refinement       'CELL and SELECT (Stoe & Cie, 2001)'
_computing_data_collection       'EXPOSE (Stoe & Cie, 2001)'
_computing_data_reduction        'INTEGRATE (Stoe & Cie, 2001)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2012)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       'image-plate diffraction system'
_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  0.0699
_diffrn_reflns_av_sigmaI/netI    0.1201
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8557
_diffrn_reflns_theta_full        15
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    11.979
_exptl_absorpt_correction_T_max  0.54
_exptl_absorpt_correction_T_min  0.39
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE; Stoe & Cie, 2001)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.866
_refine_diff_density_min         -1.527
_refine_ls_extinction_coef       0.00159(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   0.908
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         4371
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.908
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0414P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1149
_reflns_number_gt                2699
_reflns_number_total             4371
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            yp3015.cif
_cod_data_source_block           I
_cod_database_code               2018695
_cod_database_fobs_code          2018695
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_occupancy
_atom_site_symmetry_multiplicity
Te Te3 0.43168(16) 0.42340(10) 0.28111(10) 0.0290(3) Uani d 1 1
Te Te7 0.24771(17) 0.12246(10) 0.24102(11) 0.0327(3) Uani d 1 1
Te Te4 0.75713(17) 0.34177(11) 0.35879(11) 0.0356(3) Uani d 1 1
Te Te6 0.21770(16) 0.26864(11) 0.38746(10) 0.0313(3) Uani d 1 1
Te Te1 0.76503(17) 0.15379(10) 0.12227(10) 0.0326(3) Uani d 1 1
Te Te2 0.51624(17) 0.35157(11) 0.08236(10) 0.0341(3) Uani d 1 1
Te Te5 0.72432(18) 0.12996(10) 0.34614(11) 0.0353(3) Uani d 1 1
Te Te8 0.07161(18) 0.24869(11) 0.08088(10) 0.0344(3) Uani d 1 1
Nb Nb1 0.4428(2) 0.24104(13) 0.73156(13) 0.0230(4) Uani d 1 1
Nb Nb2 0.9443(2) 0.24170(13) 0.72627(12) 0.0218(4) Uani d 1 1
Cl Cl1 0.8496(6) 0.3614(4) 0.8686(4) 0.0317(10) Uani d 1 1
Cl Cl2 0.4310(6) 0.0993(4) 0.8827(4) 0.0382(12) Uani d 1 1
Cl Cl3 0.9092(6) 0.4073(3) 0.5978(4) 0.0289(10) Uani d 1 1
Cl Cl4 0.4908(6) 0.1030(4) 0.6088(4) 0.0332(10) Uani d 1 1
Cl Cl5 0.3830(6) 0.3893(4) 0.5838(4) 0.0318(10) Uani d 1 1
Cl Cl6 0.9606(6) 0.1270(4) 0.5871(3) 0.0300(10) Uani d 1 1
Cl Cl7 0.3216(6) 0.3822(4) 0.8482(4) 0.0313(10) Uani d 1 1
Cl Cl8 0.9176(6) 0.0814(4) 0.8615(4) 0.0311(10) Uani d 1 1
O O1 1.1645(16) 0.2310(9) 0.7293(9) 0.027(3) Uani d 1 1
O O2 0.6563(15) 0.2508(10) 0.7300(9) 0.028(3) Uani d 1 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.5308 1.6751 '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
Te2 Te3 Te4 . . 97.02(6)
Te2 Te3 Te6 . . 101.47(6)
Te4 Te3 Te6 . . 105.06(6)
Te8 Te7 Te6 . . 102.70(6)
Te5 Te4 Te3 . . 90.18(6)
Te7 Te6 Te3 . . 102.08(6)
Te5 Te1 Te2 . . 98.46(6)
Te5 Te1 Te8 . 1_655 99.51(6)
Te2 Te1 Te8 . 1_655 100.02(6)
Te3 Te2 Te1 . . 103.32(6)
Te4 Te5 Te1 . . 95.31(6)
Te7 Te8 Te1 . 1_455 99.24(6)
O2 Nb1 O1 . 1_455 178.5(5)
O2 Nb1 Cl2 . . 96.9(4)
O1 Nb1 Cl2 1_455 . 84.6(3)
O2 Nb1 Cl4 . . 96.2(4)
O1 Nb1 Cl4 1_455 . 83.4(3)
Cl2 Nb1 Cl4 . . 91.51(18)
O2 Nb1 Cl5 . . 96.2(4)
O1 Nb1 Cl5 1_455 . 82.4(3)
Cl2 Nb1 Cl5 . . 166.65(18)
Cl4 Nb1 Cl5 . . 89.86(16)
O2 Nb1 Cl7 . . 97.6(4)
O1 Nb1 Cl7 1_455 . 82.7(3)
Cl2 Nb1 Cl7 . . 89.31(18)
Cl4 Nb1 Cl7 . . 165.90(16)
Cl5 Nb1 Cl7 . . 86.18(16)
O1 Nb2 O2 . . 177.3(5)
O1 Nb2 Cl3 . . 96.5(4)
O2 Nb2 Cl3 . . 86.0(3)
O1 Nb2 Cl6 . . 97.3(4)
O2 Nb2 Cl6 . . 83.7(3)
Cl3 Nb2 Cl6 . . 90.48(16)
O1 Nb2 Cl8 . . 94.8(4)
O2 Nb2 Cl8 . . 82.7(3)
Cl3 Nb2 Cl8 . . 168.48(17)
Cl6 Nb2 Cl8 . . 90.41(16)
O1 Nb2 Cl1 . . 97.2(4)
O2 Nb2 Cl1 . . 81.8(3)
Cl3 Nb2 Cl1 . . 88.36(16)
Cl6 Nb2 Cl1 . . 165.53(17)
Cl8 Nb2 Cl1 . . 87.91(16)
Nb2 O1 Nb1 . 1_655 172.7(6)
Nb1 O2 Nb2 . . 173.2(7)
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
Te3 Te2 . 2.7121(19) y
Te3 Te4 . 2.8037(18) y
Te3 Te6 . 2.809(2) y
Te7 Te8 . 2.6832(19) y
Te7 Te6 . 2.6915(19) y
Te4 Te5 . 2.6455(18) y
Te1 Te5 . 2.7439(19) y
Te1 Te2 . 2.800(2) y
Te1 Te8 1_655 2.8164(19) y
Te8 Te1 1_455 2.8164(19) ?
Nb1 O2 . 1.704(11) ?
Nb1 O1 1_455 2.221(11) ?
Nb1 Cl2 . 2.339(5) ?
Nb1 Cl4 . 2.381(5) ?
Nb1 Cl5 . 2.382(4) ?
Nb1 Cl7 . 2.388(5) ?
Nb2 O1 . 1.718(12) ?
Nb2 O2 . 2.241(11) ?
Nb2 Cl3 . 2.349(4) ?
Nb2 Cl6 . 2.361(4) ?
Nb2 Cl8 . 2.376(4) ?
Nb2 Cl1 . 2.415(5) ?
O1 Nb1 1_655 2.221(11) ?
