#------------------------------------------------------------------------------ #$Date: 2013-08-29 18:37:19 +0300 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: file:///home/coder/svn-repositories/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 ; [Te~8~][NbOCl~4~]~2~ containing an infinite chain-like {[Te--Te--Te--(Te~5~)]^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_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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.0414P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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>2\s(I) _iucr_refine_instructions_details ; TITL I in P-1 CELL 0.71073 7.8670 12.0490 12.4810 80.850 82.170 78.840 ZERR 2.00 0.0016 0.0024 0.0025 0.030 0.030 0.030 LATT 1 SFAC O CL NB TE UNIT 4 16 4 16 L.S. 14 BOND FMAP 2 PLAN 20 ACTA WGHT 0.041400 EXTI 0.001594 FVAR 0.06330 MOLE 1 TE3 4 0.431685 0.423401 0.281111 11.00000 0.02764 0.02744 = 0.03151 -0.00565 -0.00243 -0.00310 TE7 4 0.247713 0.122455 0.241022 11.00000 0.03334 0.03147 = 0.03533 -0.00523 -0.00912 -0.00655 TE4 4 0.757133 0.341769 0.358792 11.00000 0.03488 0.04055 = 0.03408 -0.01386 -0.01152 -0.00047 TE6 4 0.217705 0.268642 0.387460 11.00000 0.02935 0.04055 = 0.02616 -0.00676 -0.00303 -0.00945 TE1 4 0.765028 0.153793 0.122269 11.00000 0.03319 0.03696 = 0.02930 -0.01206 -0.00353 -0.00411 TE2 4 0.516237 0.351567 0.082355 11.00000 0.03670 0.04100 = 0.02325 -0.00007 -0.00483 -0.00590 TE5 4 0.724319 0.129964 0.346144 11.00000 0.03826 0.03193 = 0.03170 0.00055 -0.00365 -0.00030 TE8 4 0.071612 0.248694 0.080878 11.00000 0.03490 0.04142 = 0.02635 -0.00199 -0.00219 -0.00871 NB1 3 0.442842 0.241040 0.731558 11.00000 0.01850 0.02791 = 0.02325 -0.00295 -0.00259 -0.00590 NB2 3 0.944251 0.241705 0.726266 11.00000 0.01801 0.02701 = 0.02083 -0.00317 -0.00241 -0.00479 CL1 2 0.849591 0.361433 0.868595 11.00000 0.03355 0.03629 = 0.02608 -0.01016 -0.00369 -0.00311 CL2 2 0.431039 0.099340 0.882710 11.00000 0.03407 0.04426 = 0.03324 0.00424 -0.00445 -0.00678 CL3 2 0.909159 0.407319 0.597775 11.00000 0.03314 0.02564 = 0.02610 0.00001 -0.00214 -0.00404 CL4 2 0.490787 0.102958 0.608805 11.00000 0.03180 0.03614 = 0.03263 -0.00933 -0.00415 -0.00386 CL5 2 0.382971 0.389280 0.583812 11.00000 0.03609 0.03441 = 0.02526 -0.00156 -0.00304 -0.00935 CL6 2 0.960567 0.126978 0.587138 11.00000 0.03169 0.03496 = 0.02448 -0.00930 -0.00329 -0.00418 CL7 2 0.321590 0.382206 0.848205 11.00000 0.03063 0.03995 = 0.02603 -0.00989 -0.00139 -0.00978 CL8 2 0.917612 0.081427 0.861545 11.00000 0.03563 0.03210 = 0.02635 -0.00081 -0.00704 -0.00765 O2 1 0.656328 0.250844 0.729991 11.00000 0.01961 0.04311 = 0.02052 -0.00451 -0.00212 -0.00304 O1 1 0.164517 0.230960 0.729281 11.00000 0.03913 0.02323 = 0.02723 0.00247 -0.01508 -0.02195 MOLE 2 HKLF 4 REM P-1 in P-1 REM R1 = 0.0472 for 2699 Fo > 4sig(Fo) and 0.0854 for all 4371 data REM 182 parameters refined using 0 restraints END WGHT 0.0414 0.0000 REM Highest difference peak 1.866, deepest hole -1.527, 1-sigma level 0.322 Q1 1 -0.0146 0.4124 0.1372 11.00000 0.05 1.87 Q2 1 0.6564 0.2556 0.0795 11.00000 0.05 1.31 Q3 1 0.3815 0.0597 0.1816 11.00000 0.05 1.27 Q4 1 0.2589 0.2159 0.4189 11.00000 0.05 1.24 Q5 1 0.2854 0.1950 0.4305 11.00000 0.05 1.23 Q6 1 0.7391 0.2168 0.0160 11.00000 0.05 1.18 Q7 1 0.3752 0.1622 0.6858 11.00000 0.05 1.15 Q8 1 0.2092 0.1645 0.0343 11.00000 0.05 1.15 Q9 1 0.8133 0.4606 0.6310 11.00000 0.05 1.14 Q10 1 0.1031 0.3030 0.4628 11.00000 0.05 1.13 Q11 1 0.3639 0.0806 0.1969 11.00000 0.05 1.13 Q12 1 1.0311 0.3601 0.5363 11.00000 0.05 1.09 Q13 1 0.7386 0.2130 0.2368 11.00000 0.05 1.08 Q14 1 0.3644 0.2129 0.3165 11.00000 0.05 1.08 Q15 1 0.0750 0.1735 0.1129 11.00000 0.05 1.08 Q16 1 0.1182 0.2151 0.1835 11.00000 0.05 1.08 Q17 1 0.6116 0.2002 0.1991 11.00000 0.05 1.07 Q18 1 0.6117 0.1866 0.4125 11.00000 0.05 1.06 Q19 1 0.9913 0.3001 0.8002 11.00000 0.05 1.05 Q20 1 0.0544 0.2208 0.3512 11.00000 0.05 1.05 ; _[local]_cod_data_source_file yp3015.cif _[local]_cod_data_source_block I _cod_database_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_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 Te3 0.0276(7) 0.0274(6) 0.0315(7) -0.0031(5) -0.0024(6) -0.0056(5) Te7 0.0333(7) 0.0315(6) 0.0353(7) -0.0066(5) -0.0091(6) -0.0052(5) Te4 0.0349(8) 0.0406(7) 0.0341(7) -0.0005(6) -0.0115(6) -0.0139(6) Te6 0.0294(7) 0.0405(7) 0.0262(6) -0.0094(6) -0.0030(6) -0.0068(5) Te1 0.0332(7) 0.0370(7) 0.0293(7) -0.0041(6) -0.0035(6) -0.0121(5) Te2 0.0367(8) 0.0410(7) 0.0232(6) -0.0059(6) -0.0048(6) -0.0001(5) Te5 0.0383(8) 0.0319(7) 0.0317(7) -0.0003(6) -0.0036(6) 0.0005(5) Te8 0.0349(7) 0.0414(7) 0.0263(6) -0.0087(6) -0.0022(6) -0.0020(5) Nb1 0.0185(8) 0.0279(8) 0.0232(8) -0.0059(6) -0.0026(7) -0.0029(6) Nb2 0.0180(8) 0.0270(8) 0.0208(8) -0.0048(6) -0.0024(7) -0.0032(6) Cl1 0.034(3) 0.036(2) 0.026(2) -0.003(2) -0.004(2) -0.0102(18) Cl2 0.034(3) 0.044(3) 0.033(3) -0.007(2) -0.004(2) 0.004(2) Cl3 0.033(3) 0.026(2) 0.026(2) -0.0040(18) -0.002(2) 0.0000(17) Cl4 0.032(3) 0.036(2) 0.033(2) -0.004(2) -0.004(2) -0.0093(19) Cl5 0.036(3) 0.034(2) 0.025(2) -0.009(2) -0.003(2) -0.0016(18) Cl6 0.032(3) 0.035(2) 0.024(2) -0.0042(19) -0.003(2) -0.0093(18) Cl7 0.031(2) 0.040(2) 0.026(2) -0.010(2) -0.001(2) -0.0099(19) Cl8 0.036(3) 0.032(2) 0.026(2) -0.008(2) -0.007(2) -0.0008(18) O1 0.039(7) 0.023(6) 0.027(6) -0.022(5) -0.015(6) 0.002(5) O2 0.020(7) 0.043(7) 0.021(6) -0.003(6) -0.002(6) -0.005(5) 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) ? _cod_database_fobs_code 2018695