#------------------------------------------------------------------------------ #$Date: 2019-11-07 22:54:29 +0200 (Thu, 07 Nov 2019) $ #$Revision: 223889 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/05/7700514.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_7700514 loop_ _publ_author_name 'Wolf, Silke' 'Feldmann, Claus' _publ_section_title ; Ionic-liquid-based synthesis of tellurium-rhenium carbonyls with specific reaction control. ; _journal_issue 41 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 15521 _journal_page_last 15528 _journal_paper_doi 10.1039/c9dt01897b _journal_volume 48 _journal_year 2019 _chemical_formula_sum 'C3 I7 O3 Re Te3' _chemical_formula_weight 1541.33 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _audit_creation_method SHELXL-2013 _audit_update_record ; 2019-06-28 deposited with the CCDC. 2019-07-10 downloaded from the CCDC. ; _cell_angle_alpha 84.28(3) _cell_angle_beta 72.82(3) _cell_angle_gamma 85.97(3) _cell_formula_units_Z 2 _cell_length_a 8.5380(17) _cell_length_b 9.961(2) _cell_length_c 13.229(3) _cell_measurement_reflns_used 10458 _cell_measurement_temperature 200(2) _cell_measurement_theta_max 58.6 _cell_measurement_theta_min 4.1 _cell_volume 1068.5(4) _computing_cell_refinement ; X-Area Recipe 1.33.0.0 (STOE, 2015) PLATON (A.L.Spek, 2009) ; _computing_data_collection 'X-Area 1.31.127.0 (STOE, 2016)' _computing_data_reduction ; X-Area Integrate 1.71.0.0 (STOE, 2016) X-Area LANA 1.70.0.0 (STOE, 2017) PLATON (A.L.Spek, 2009) ; _computing_molecular_graphics 'Diamond 4' _computing_publication_material ; STOE & Cie GmbH, X-Area, software package for collecting single-crystal or multi-domain crystal data on STOE area-detector diffractometers, for image processing, for the correction and scaling of reflection intensities and for outlier rejection, version 1.77, Darmstadt 2016 MS Word (Microsoft) Diamond 4 ; _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution 'SHELXS-2013 (Sheldrick, 2013)' _diffrn_ambient_temperature 200(2) _diffrn_detector_area_resol_mean 'image plate' _diffrn_measured_fraction_theta_full 0.942 _diffrn_measured_fraction_theta_max 0.913 _diffrn_measurement_device_type graphite _diffrn_measurement_method 'STOE IPDS II' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0583 _diffrn_reflns_av_unetI/netI 0.1287 _diffrn_reflns_Laue_measured_fraction_full 0.942 _diffrn_reflns_Laue_measured_fraction_max 0.913 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 10377 _diffrn_reflns_point_group_measured_fraction_full 0.942 _diffrn_reflns_point_group_measured_fraction_max 0.913 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 29.234 _diffrn_reflns_theta_min 1.617 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 19.807 _exptl_absorpt_correction_T_max 0.9093 _exptl_absorpt_correction_T_min 0.8017 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details '(X-RED, Data Reduction Program, Version 1.14, Stoe & Cie GmbH, Darmstadt 1999.; X-SHAPE, Crystal Optimisation for Numerical Absorption Correction, Version 1.06, Stoe & Cie GmbH, Darmstadt 1999.)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 4.790 _exptl_crystal_description prism _exptl_crystal_F_000 1288 _exptl_crystal_size_max 0.510 _exptl_crystal_size_mid 0.490 _exptl_crystal_size_min 0.420 _refine_diff_density_max 1.911 _refine_diff_density_min -1.871 _refine_diff_density_rms 0.278 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.705 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 154 _refine_ls_number_reflns 5317 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.705 _refine_ls_R_factor_all 0.0915 _refine_ls_R_factor_gt 0.0332 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0096P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.0548 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2691 _reflns_number_total 5317 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9dt01897b2.cif _cod_data_source_block Re(CO)3Te3I7 _cod_depositor_comments 'Adding full bibliography for 7700512--7700515.cif.' _cod_original_cell_volume 1068.6(4) _cod_database_code 7700514 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelxl_version_number 2013-2 _shelx_res_file ; TITL p-1 in P-1 CELL 0.71073 8.5380 9.9610 13.2290 84.280 72.820 85.974 ZERR 2.00 0.0017 0.0020 0.0026 0.030 0.030 0.030 LATT 1 SFAC C O TE I RE UNIT 6 6 6 14 2 L.S. 10 BOND ACTA 50 FMAP 2 PLAN 20 WGHT 0.009600 FVAR 0.05707 MOLE 1 RE1 5 0.156270 0.189440 0.305880 11.00000 0.02412 0.02417 = 0.02241 -0.00212 -0.00597 -0.00132 C1 1 0.060987 0.293325 0.428306 11.00000 0.04273 0.04036 = 0.02894 -0.00422 0.00116 -0.01316 O1 2 0.000531 0.343842 0.502215 11.00000 0.05253 0.04755 = 0.03013 -0.00595 -0.00931 -0.00190 C2 1 0.179171 0.031529 0.397431 11.00000 0.02098 0.05276 = 0.02253 -0.02018 0.00286 0.00013 O2 2 0.188704 -0.063652 0.452982 11.00000 0.04810 0.03547 = 0.03333 0.00897 -0.00777 0.00369 C3 1 -0.057013 0.137176 0.307286 11.00000 0.02417 0.02633 = 0.03171 0.00034 -0.00721 -0.00247 O3 2 -0.186488 0.109223 0.311513 11.00000 0.03615 0.03820 = 0.05138 -0.01059 -0.01307 0.00344 TE1 3 0.301053 0.044871 0.135853 11.00000 0.03544 0.02950 = 0.02406 -0.00521 -0.00734 -0.00013 TE2 3 0.133062 0.406682 0.165970 11.00000 0.03304 0.02679 = 0.03147 -0.00031 -0.01137 -0.00085 TE3 3 0.455657 0.274991 0.298321 11.00000 0.02736 0.03167 = 0.03485 -0.00543 -0.01108 0.00038 I1 4 0.511457 0.303800 0.038744 11.00000 0.03819 0.03324 = 0.03325 -0.00009 0.00029 -0.00529 I2 4 0.562805 -0.074119 0.198566 11.00000 0.03752 0.04109 = 0.03972 -0.00536 -0.01340 0.00552 I3 4 0.018395 0.278138 0.029244 11.00000 0.06161 0.04543 = 0.04331 -0.00510 -0.03001 -0.00324 I4 4 0.373937 0.546618 0.297807 11.00000 0.04139 0.03025 = 0.06224 -0.01020 -0.01812 -0.00063 I5 4 0.093584 -0.174780 0.201451 11.00000 0.04425 0.03032 = 0.04621 -0.00881 -0.00947 -0.00759 I6 4 -0.166467 0.516332 0.279669 11.00000 0.03119 0.03608 = 0.06537 -0.00249 -0.00507 0.00322 I7 4 0.439066 0.231101 0.510637 11.00000 0.05224 0.07268 = 0.03783 -0.01257 -0.02266 0.01130 MOLE 2 HKLF 4 REM p-1 in P-1 REM R1 = 0.0332 for 2691 Fo > 4sig(Fo) and 0.0915 for all 5317 data REM 154 parameters refined using 0 restraints END WGHT 0.0096 0.0000 REM Highest difference peak 1.911, deepest hole -1.871, 1-sigma level 0.278 Q1 1 0.1126 0.2029 0.3341 11.00000 0.05 1.91 Q2 1 0.1864 0.1990 0.2675 11.00000 0.05 1.63 Q3 1 0.2258 0.2077 0.3145 11.00000 0.05 1.38 Q4 1 0.0803 0.2200 0.4073 11.00000 0.05 1.33 Q5 1 -0.0229 0.1652 0.0331 11.00000 0.05 1.24 Q6 1 0.3110 0.1756 0.3130 11.00000 0.05 1.15 Q7 1 0.1930 0.0454 0.1254 11.00000 0.05 1.15 Q8 1 0.3323 0.0536 0.1105 11.00000 0.05 1.09 Q9 1 0.0720 0.1268 0.2380 11.00000 0.05 1.09 Q10 1 0.5108 0.2038 0.2317 11.00000 0.05 1.08 Q11 1 0.2571 0.0984 0.2354 11.00000 0.05 1.07 Q12 1 0.0920 0.3955 0.2015 11.00000 0.05 1.06 Q13 1 0.5268 -0.0823 0.2375 11.00000 0.05 1.05 Q14 1 0.1684 0.3926 0.1296 11.00000 0.05 1.05 Q15 1 0.3670 0.2444 0.1812 11.00000 0.05 1.04 Q16 1 -0.0024 0.1840 0.3097 11.00000 0.05 1.03 Q17 1 0.4873 0.5172 0.3475 11.00000 0.05 1.03 Q18 1 0.1840 0.1416 0.2077 11.00000 0.05 1.02 Q19 1 0.1394 0.1213 0.4025 11.00000 0.05 1.01 Q20 1 0.3731 0.3216 0.4664 11.00000 0.05 1.01 ; _shelx_res_checksum 15981 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag Re1 Re 0.15627(5) 0.18944(5) 0.30588(3) 0.02371(11) Uani 1 1 d C1 C 0.0610(15) 0.2933(13) 0.4283(10) 0.039(3) Uani 1 1 d O1 O 0.0005(11) 0.3438(9) 0.5022(7) 0.044(2) Uani 1 1 d C2 C 0.1792(13) 0.0315(13) 0.3974(9) 0.033(3) Uani 1 1 d O2 O 0.1887(10) -0.0637(8) 0.4530(6) 0.041(2) Uani 1 1 d C3 C -0.0570(14) 0.1372(11) 0.3073(9) 0.028(3) Uani 1 1 d O3 O -0.1865(10) 0.1092(8) 0.3115(7) 0.042(2) Uani 1 1 d Te1 Te 0.30105(9) 0.04487(8) 0.13585(6) 0.02980(19) Uani 1 1 d Te2 Te 0.13306(9) 0.40668(8) 0.16597(6) 0.03017(19) Uani 1 1 d Te3 Te 0.45566(9) 0.27499(8) 0.29832(6) 0.03075(19) Uani 1 1 d I1 I 0.51146(10) 0.30380(8) 0.03874(6) 0.0372(2) Uani 1 1 d I2 I 0.56280(10) -0.07412(8) 0.19857(6) 0.0392(2) Uani 1 1 d I3 I 0.01840(12) 0.27814(9) 0.02924(7) 0.0468(2) Uani 1 1 d I4 I 0.37394(10) 0.54662(8) 0.29781(7) 0.0436(2) Uani 1 1 d I5 I 0.09358(10) -0.17478(8) 0.20145(7) 0.0404(2) Uani 1 1 d I6 I -0.16647(10) 0.51633(8) 0.27967(8) 0.0465(2) Uani 1 1 d I7 I 0.43907(11) 0.23110(10) 0.51064(7) 0.0523(3) Uani 1 1 d loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.0241(2) 0.0242(2) 0.0224(2) -0.00212(19) -0.0060(2) -0.00132(19) C1 0.043(8) 0.040(7) 0.029(7) -0.004(6) 0.001(6) -0.013(6) O1 0.053(6) 0.048(6) 0.030(5) -0.006(4) -0.009(4) -0.002(5) C2 0.021(6) 0.053(8) 0.023(6) -0.020(6) 0.003(5) 0.000(6) O2 0.048(5) 0.035(5) 0.033(5) 0.009(4) -0.008(4) 0.004(4) C3 0.024(6) 0.026(6) 0.032(6) 0.000(5) -0.007(5) -0.002(5) O3 0.036(5) 0.038(5) 0.051(6) -0.011(4) -0.013(5) 0.003(4) Te1 0.0354(4) 0.0295(4) 0.0241(4) -0.0052(3) -0.0073(3) -0.0001(3) Te2 0.0330(4) 0.0268(4) 0.0315(4) -0.0003(3) -0.0114(4) -0.0008(3) Te3 0.0274(4) 0.0317(4) 0.0349(4) -0.0054(4) -0.0111(3) 0.0004(3) I1 0.0382(5) 0.0332(4) 0.0332(4) -0.0001(4) 0.0003(4) -0.0053(3) I2 0.0375(5) 0.0411(5) 0.0397(4) -0.0054(4) -0.0134(4) 0.0055(4) I3 0.0616(6) 0.0454(5) 0.0433(5) -0.0051(4) -0.0300(4) -0.0032(4) I4 0.0414(5) 0.0303(4) 0.0622(6) -0.0102(4) -0.0181(4) -0.0006(4) I5 0.0443(5) 0.0303(4) 0.0462(5) -0.0088(4) -0.0095(4) -0.0076(4) I6 0.0312(4) 0.0361(5) 0.0654(6) -0.0025(4) -0.0051(4) 0.0032(4) I7 0.0522(6) 0.0727(7) 0.0378(5) -0.0126(5) -0.0227(4) 0.0113(5) 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' O O 0.0106 0.0060 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 '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 C2 Re1 C3 90.6(5) C2 Re1 C1 90.7(5) C3 Re1 C1 91.3(5) C2 Re1 Te3 92.2(4) C3 Re1 Te3 177.2(3) C1 Re1 Te3 88.4(4) C2 Re1 Te1 88.7(3) C3 Re1 Te1 90.8(3) C1 Re1 Te1 177.8(4) Te3 Re1 Te1 89.52(4) C2 Re1 Te2 176.8(3) C3 Re1 Te2 89.7(3) C1 Re1 Te2 92.4(3) Te3 Re1 Te2 87.47(4) Te1 Re1 Te2 88.11(3) O1 C1 Re1 174.5(11) O2 C2 Re1 178.3(10) O3 C3 Re1 177.2(11) Re1 Te1 I2 99.49(4) Re1 Te1 I5 96.42(4) I2 Te1 I5 97.29(4) Re1 Te1 I1 85.92(4) I2 Te1 I1 89.32(4) I5 Te1 I1 172.51(4) Re1 Te2 I3 98.61(4) Re1 Te2 I6 98.46(4) I3 Te2 I6 96.93(5) Re1 Te3 I4 97.34(4) Re1 Te3 I7 99.69(4) I4 Te3 I7 97.04(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Re1 C2 1.923(12) Re1 C3 1.923(12) Re1 C1 1.948(13) Re1 Te3 2.7218(12) Re1 Te1 2.7229(13) Re1 Te2 2.7397(12) C1 O1 1.113(13) C2 O2 1.154(12) C3 O3 1.143(13) Te1 I2 2.7595(13) Te1 I5 2.8170(15) Te1 I1 3.1869(15) Te2 I3 2.7483(15) Te2 I6 2.7674(15) Te3 I4 2.7462(13) Te3 I7 2.7621(13)