#------------------------------------------------------------------------------ #$Date: 2019-07-12 04:00:12 +0300 (Fri, 12 Jul 2019) $ #$Revision: 216969 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/05/7700512.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_7700512 loop_ _publ_author_name 'Wolf, Silke' 'Feldmann, Claus' _publ_section_title ; Ionic-Liquid-Based Synthesis of Tellurium-Rhenium Carbonyls with Specific Reaction Control ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/C9DT01897B _journal_year 2019 _chemical_formula_moiety 'C8 H13 N2, C4 I6 O4 Re Te2' _chemical_formula_sum 'C12 H15 I6 N2 O4 Re Te2' _chemical_formula_weight 1454.06 _chemical_properties_physical Air-sensitive,Moisture-sensitive _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _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 90 _cell_angle_beta 108.62(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.7094(19) _cell_length_b 13.539(3) _cell_length_c 22.976(6) _cell_measurement_reflns_used 25280 _cell_measurement_temperature 200(2) _cell_measurement_theta_max 3.0 _cell_measurement_theta_min 58.5 _cell_volume 2862.2(12) _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_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 0.998 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measurement_device_type 'STOE IPDS II' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0720 _diffrn_reflns_av_unetI/netI 0.0186 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 7707 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.232 _diffrn_reflns_theta_min 1.771 _exptl_absorpt_coefficient_mu 12.734 _exptl_absorpt_correction_T_max 0.1645 _exptl_absorpt_correction_T_min 0.0757 _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 3.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 2520 _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.45 _refine_diff_density_max 1.670 _refine_diff_density_min -1.736 _refine_diff_density_rms 0.167 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 264 _refine_ls_number_reflns 7707 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.956 _refine_ls_R_factor_all 0.0411 _refine_ls_R_factor_gt 0.0324 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0650P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0930 _refine_ls_wR_factor_ref 0.0960 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5754 _reflns_number_total 7707 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9dt01897b2.cif _cod_data_source_block '[BMIm][Re(CO)4Te2I6]' _cod_database_code 7700512 _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. ; _shelx_res_file ; TITL P21n in P2(1)/n New: P21/c p21n.res created by SHELXL-2018/3 at 16:53:44 on 25-Jun-2019 CELL 0.71073 9.7094 13.539 22.976 90 108.62 90 ZERR 4 0.0019 0.003 0.006 0 0.03 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H I N O Re Te UNIT 48 60 24 8 16 4 8 L.S. 10 PLAN -20 BOND $H CONF fmap 2 acta REM REM REM WGHT 0.065000 FVAR 0.04159 N1 4 -0.260599 -0.279307 -0.168403 11.00000 0.07214 0.07503 = 0.06501 -0.01061 0.01886 -0.01547 N2 4 -0.181660 -0.224824 -0.239490 11.00000 0.06550 0.07255 = 0.06545 -0.00439 0.01904 -0.00546 C5 1 -0.336948 -0.284257 -0.122563 11.00000 0.10542 0.09869 = 0.08363 -0.01293 0.04021 -0.02742 AFIX 137 H5A 2 -0.271369 -0.266306 -0.082986 11.00000 -1.50000 H5B 2 -0.371565 -0.350286 -0.120929 11.00000 -1.50000 H5C 2 -0.417759 -0.239411 -0.133843 11.00000 -1.50000 AFIX 0 C6 1 -0.136067 -0.320256 -0.228088 11.00000 0.07832 0.06846 = 0.09006 -0.00694 0.02897 0.00432 AFIX 43 H6 2 -0.080706 -0.355334 -0.247443 11.00000 -1.20000 AFIX 0 C7 1 -0.185740 -0.353846 -0.183987 11.00000 0.07992 0.06820 = 0.09034 0.00087 0.02462 -0.00797 AFIX 43 H7 2 -0.171645 -0.416869 -0.167008 11.00000 -1.20000 AFIX 0 C8 1 -0.257609 -0.201620 -0.202817 11.00000 0.06768 0.07163 = 0.06892 -0.00134 0.01742 0.00018 AFIX 43 H8 2 -0.301449 -0.140966 -0.201472 11.00000 -1.20000 AFIX 0 C9 1 -0.151277 -0.158466 -0.284846 11.00000 0.07530 0.08435 = 0.06854 0.00958 0.02216 -0.00166 PART 1 C10A 1 0.007750 -0.146182 -0.267868 10.35000 0.08999 0.07005 = 0.07618 -0.00413 0.06073 0.00108 AFIX 23 H10A 2 0.033298 -0.197126 -0.292287 10.35000 -1.20000 H10B 2 0.015623 -0.084804 -0.288353 10.35000 -1.20000 AFIX 0 PART 0 PART 2 C10B 1 -0.019465 -0.089128 -0.255494 10.65000 0.07780 0.06543 = 0.06375 0.00804 0.02902 0.01055 AFIX 23 H10C 2 0.029767 -0.085369 -0.286117 10.65000 -1.20000 H10D 2 -0.062993 -0.024631 -0.255531 10.65000 -1.20000 AFIX 0 PART 0 PART 1 C11A 1 0.118874 -0.143207 -0.221393 10.65000 0.07059 0.06643 = 0.07391 -0.00321 0.01072 0.00597 AFIX 23 H11A 2 0.163872 -0.206967 -0.222101 10.65000 -1.20000 H11B 2 0.079386 -0.147028 -0.187641 10.65000 -1.20000 AFIX 0 PART 0 PART 2 C11B 1 0.073489 -0.092001 -0.209463 10.35000 0.09507 0.07331 = 0.07607 -0.00743 0.03419 -0.02996 AFIX 23 H11C 2 0.065172 -0.156196 -0.192139 10.35000 -1.20000 H11D 2 0.047679 -0.043978 -0.183370 10.35000 -1.20000 AFIX 0 PART 0 C12 1 0.244690 -0.076487 -0.197524 11.00000 0.07933 0.08726 = 0.09704 0.00465 0.03173 -0.00296 PART 1 AFIX 137 H12A 2 0.244997 -0.028897 -0.228455 10.65000 -1.50000 H12B 2 0.332897 -0.114298 -0.186866 10.65000 -1.50000 H12C 2 0.237956 -0.042898 -0.161734 10.65000 -1.50000 AFIX 137 PART 0 PART 2 H12D 2 0.297290 -0.132068 -0.175281 10.35000 -1.50000 H12E 2 0.276448 -0.017358 -0.174002 10.35000 -1.50000 H12F 2 0.262430 -0.070784 -0.236167 10.35000 -1.50000 AFIX 0 PART 0 RE1 6 0.303467 -0.336124 -0.455857 11.00000 0.04516 0.04695 = 0.05858 0.00082 0.01854 0.00079 I1 3 0.630767 -0.140028 -0.467076 11.00000 0.05030 0.06300 = 0.06895 0.00342 0.02208 -0.00390 I2 3 0.255591 -0.143077 -0.606887 11.00000 0.08122 0.07049 = 0.05909 0.00351 0.01367 -0.00063 I3 3 0.006241 -0.114555 -0.457658 11.00000 0.05332 0.06175 = 0.09532 0.01918 0.02879 0.01004 I4 3 0.416862 -0.104014 -0.333582 11.00000 0.06518 0.06298 = 0.06658 -0.01015 0.01866 -0.00249 I5 3 -0.069741 -0.394990 -0.404406 11.00000 0.06123 0.06931 = 0.09831 0.00421 0.03774 -0.00707 I6 3 0.337514 -0.398375 -0.270067 11.00000 0.08490 0.06733 = 0.06309 0.01150 0.02033 0.00382 TE1 7 0.176978 -0.269565 -0.370896 11.00000 0.05515 0.05281 = 0.06434 0.00276 0.02624 0.00267 TE2 7 0.339012 -0.138751 -0.478759 11.00000 0.04933 0.04901 = 0.06069 0.00304 0.01847 -0.00074 O1 5 0.607584 -0.341081 -0.354319 11.00000 0.05562 0.07352 = 0.08076 0.00633 0.01709 0.00668 O2 5 0.260588 -0.550660 -0.420851 11.00000 0.07703 0.05130 = 0.09763 0.00615 0.03099 0.00047 O3 5 0.005701 -0.331873 -0.562658 11.00000 0.06208 0.07450 = 0.08338 0.00037 0.01233 -0.00738 O4 5 0.457167 -0.403629 -0.546798 11.00000 0.08344 0.09124 = 0.07941 0.00141 0.03929 0.01844 C1 1 0.499314 -0.336903 -0.390283 11.00000 0.04977 0.05482 = 0.06053 0.00317 0.01191 0.00251 C2 1 0.273256 -0.472643 -0.434357 11.00000 0.05537 0.04904 = 0.06708 -0.00228 0.02190 -0.00060 C3 1 0.110010 -0.332680 -0.523193 11.00000 0.05097 0.05807 = 0.06557 -0.00168 0.00552 -0.00439 C4 1 0.399743 -0.377618 -0.513943 11.00000 0.05266 0.06015 = 0.06869 0.00345 0.02193 0.00811 HKLF 4 1 1 0 0 0 -1 0 -1 0 -1 REM P21n in P2(1)/n New: P21/c REM wR2 = 0.0960, GooF = S = 0.956, Restrained GooF = 0.956 for all data REM R1 = 0.0324 for 5754 Fo > 4sig(Fo) and 0.0411 for all 7707 data REM 264 parameters refined using 0 restraints END WGHT 0.0650 0.0000 REM Highest difference peak 1.670, deepest hole -1.736, 1-sigma level 0.167 Q1 1 0.2029 -0.3375 -0.4528 11.00000 0.05 1.67 Q2 1 0.4050 -0.3401 -0.4597 11.00000 0.05 1.64 Q3 1 0.3170 -0.3778 -0.4252 11.00000 0.05 1.40 Q4 1 0.4362 -0.1375 -0.4826 11.00000 0.05 1.19 Q5 1 0.2784 -0.2975 -0.4881 11.00000 0.05 1.15 Q6 1 0.2782 -0.3774 -0.4867 11.00000 0.05 1.14 Q7 1 0.3179 -0.2981 -0.4244 11.00000 0.05 1.14 Q8 1 0.1807 -0.1402 -0.6008 11.00000 0.05 1.05 Q9 1 0.2391 -0.2650 -0.4573 11.00000 0.05 1.05 Q10 1 0.0826 -0.2693 -0.3661 11.00000 0.05 1.00 Q11 1 0.2654 -0.2689 -0.3762 11.00000 0.05 0.98 Q12 1 0.5249 -0.1387 -0.4641 11.00000 0.05 0.94 Q13 1 0.2497 -0.3971 -0.2683 11.00000 0.05 0.92 Q14 1 0.3163 -0.1036 -0.5092 11.00000 0.05 0.92 Q15 1 0.4374 -0.1445 -0.3022 11.00000 0.05 0.89 Q16 1 0.3521 -0.1003 -0.4511 11.00000 0.05 0.88 Q17 1 0.6051 -0.1785 -0.5002 11.00000 0.05 0.88 Q18 1 -0.0272 -0.1444 -0.4902 11.00000 0.05 0.88 Q19 1 0.6400 -0.0991 -0.4389 11.00000 0.05 0.87 Q20 1 0.3634 -0.4246 -0.2379 11.00000 0.05 0.86 ; _shelx_res_checksum 62133 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 _atom_site_refinement_flags_posn _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group N1 N -0.2606(8) -0.2793(6) -0.1684(3) 0.0714(17) Uani 1 1 d . . . . N2 N -0.1817(8) -0.2248(5) -0.2395(3) 0.0683(16) Uani 1 1 d . . . . C5 C -0.3369(14) -0.2843(9) -0.1226(5) 0.094(3) Uani 1 1 d . . . . H5A H -0.271369 -0.266306 -0.082986 0.140 Uiso 1 1 calc GR . . . H5B H -0.371565 -0.350286 -0.120929 0.140 Uiso 1 1 calc GR . . . H5C H -0.417759 -0.239411 -0.133843 0.140 Uiso 1 1 calc GR . . . C6 C -0.1361(11) -0.3203(7) -0.2281(5) 0.078(2) Uani 1 1 d . . . . H6 H -0.080706 -0.355334 -0.247443 0.094 Uiso 1 1 calc R . . . C7 C -0.1857(11) -0.3538(7) -0.1840(5) 0.080(2) Uani 1 1 d . . . . H7 H -0.171645 -0.416869 -0.167008 0.096 Uiso 1 1 calc R . . . C8 C -0.2576(10) -0.2016(7) -0.2028(4) 0.0705(19) Uani 1 1 d . . . . H8 H -0.301449 -0.140966 -0.201472 0.085 Uiso 1 1 calc R . . . C9 C -0.1513(11) -0.1585(7) -0.2848(4) 0.076(2) Uani 1 1 d . . . . C10A C 0.008(3) -0.146(2) -0.2679(12) 0.071(6) Uani 0.35 1 d . P A 1 H10A H 0.033298 -0.197126 -0.292287 0.085 Uiso 0.35 1 calc R P A 1 H10B H 0.015623 -0.084804 -0.288353 0.085 Uiso 0.35 1 calc R P A 1 C10B C -0.0195(15) -0.0891(10) -0.2555(7) 0.067(3) Uani 0.65 1 d . P A 2 H10C H 0.029767 -0.085369 -0.286117 0.081 Uiso 0.65 1 calc R P A 2 H10D H -0.062993 -0.024631 -0.255531 0.081 Uiso 0.65 1 calc R P A 2 C11A C 0.1189(16) -0.1432(11) -0.2214(8) 0.073(3) Uani 0.65 1 d . P A 1 H11A H 0.163872 -0.206967 -0.222101 0.088 Uiso 0.65 1 calc R P A 1 H11B H 0.079386 -0.147028 -0.187641 0.088 Uiso 0.65 1 calc R P A 1 C11B C 0.073(4) -0.092(2) -0.2095(14) 0.080(7) Uani 0.35 1 d . P A 2 H11C H 0.065172 -0.156196 -0.192139 0.096 Uiso 0.35 1 calc R P A 2 H11D H 0.047679 -0.043978 -0.183370 0.096 Uiso 0.35 1 calc R P A 2 C12 C 0.2447(12) -0.0765(9) -0.1975(6) 0.087(3) Uani 1 1 d . . . . H12A H 0.244997 -0.028897 -0.228455 0.131 Uiso 0.65 1 calc GR P A 1 H12B H 0.332897 -0.114298 -0.186866 0.131 Uiso 0.65 1 calc GR P A 1 H12C H 0.237956 -0.042898 -0.161734 0.131 Uiso 0.65 1 calc GR P A 1 H12D H 0.297290 -0.132068 -0.175281 0.131 Uiso 0.35 1 calc GR P A 2 H12E H 0.276448 -0.017358 -0.174002 0.131 Uiso 0.35 1 calc GR P A 2 H12F H 0.262430 -0.070784 -0.236167 0.131 Uiso 0.35 1 calc GR P A 2 Re1 Re 0.30347(3) -0.33612(2) -0.45586(2) 0.04976(7) Uani 1 1 d . . . . I1 I 0.63077(5) -0.14003(4) -0.46708(2) 0.06003(11) Uani 1 1 d . . . . I2 I 0.25559(7) -0.14308(4) -0.60689(3) 0.07234(14) Uani 1 1 d . . . . I3 I 0.00624(5) -0.11456(4) -0.45766(3) 0.06893(14) Uani 1 1 d . . . . I4 I 0.41686(6) -0.10401(4) -0.33358(3) 0.06548(12) Uani 1 1 d . . . . I5 I -0.06974(6) -0.39499(4) -0.40441(3) 0.07337(15) Uani 1 1 d . . . . I6 I 0.33751(7) -0.39838(4) -0.27007(3) 0.07255(14) Uani 1 1 d . . . . Te1 Te 0.17698(5) -0.26956(3) -0.37090(2) 0.05574(11) Uani 1 1 d . . . . Te2 Te 0.33901(5) -0.13875(3) -0.47876(2) 0.05280(10) Uani 1 1 d . . . . O1 O 0.6076(6) -0.3411(4) -0.3543(3) 0.0711(14) Uani 1 1 d . . . . O2 O 0.2606(7) -0.5507(4) -0.4209(3) 0.0746(15) Uani 1 1 d . . . . O3 O 0.0057(7) -0.3319(5) -0.5627(3) 0.0759(15) Uani 1 1 d . . . . O4 O 0.4572(8) -0.4036(5) -0.5468(3) 0.0815(17) Uani 1 1 d . . . . C1 C 0.4993(8) -0.3369(5) -0.3903(4) 0.0564(14) Uani 1 1 d . . . . C2 C 0.2733(8) -0.4726(5) -0.4344(4) 0.0566(15) Uani 1 1 d . . . . C3 C 0.1100(8) -0.3327(6) -0.5232(4) 0.0613(16) Uani 1 1 d . . . . C4 C 0.3997(8) -0.3776(6) -0.5139(4) 0.0599(16) 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 N1 0.072(4) 0.075(4) 0.065(4) -0.011(3) 0.019(3) -0.015(3) N2 0.066(4) 0.073(4) 0.065(4) -0.004(3) 0.019(3) -0.005(3) C5 0.105(8) 0.099(7) 0.084(6) -0.013(5) 0.040(6) -0.027(6) C6 0.078(5) 0.068(5) 0.090(6) -0.007(4) 0.029(5) 0.004(4) C7 0.080(6) 0.068(5) 0.090(7) 0.001(4) 0.025(5) -0.008(4) C8 0.068(4) 0.072(5) 0.069(5) -0.001(4) 0.017(4) 0.000(4) C9 0.075(5) 0.084(6) 0.069(5) 0.010(4) 0.022(4) -0.002(4) C10A 0.090(17) 0.070(14) 0.076(15) -0.004(11) 0.061(15) 0.001(12) C10B 0.078(8) 0.065(7) 0.064(7) 0.008(6) 0.029(7) 0.011(6) C11A 0.071(8) 0.066(7) 0.074(8) -0.003(6) 0.011(7) 0.006(6) C11B 0.10(2) 0.073(17) 0.076(18) -0.007(13) 0.034(16) -0.030(15) C12 0.079(6) 0.087(6) 0.097(7) 0.005(5) 0.032(5) -0.003(5) Re1 0.04516(12) 0.04695(12) 0.05858(14) 0.00082(10) 0.01854(10) 0.00079(9) I1 0.0503(2) 0.0630(2) 0.0690(3) 0.0034(2) 0.02208(19) -0.00390(18) I2 0.0812(3) 0.0705(3) 0.0591(3) 0.0035(2) 0.0137(2) -0.0006(2) I3 0.0533(2) 0.0617(3) 0.0953(4) 0.0192(2) 0.0288(2) 0.01004(19) I4 0.0652(3) 0.0630(3) 0.0666(3) -0.0102(2) 0.0187(2) -0.0025(2) I5 0.0612(3) 0.0693(3) 0.0983(4) 0.0042(3) 0.0377(3) -0.0071(2) I6 0.0849(4) 0.0673(3) 0.0631(3) 0.0115(2) 0.0203(2) 0.0038(2) Te1 0.0551(2) 0.0528(2) 0.0643(3) 0.00276(18) 0.02624(19) 0.00267(17) Te2 0.0493(2) 0.0490(2) 0.0607(2) 0.00304(17) 0.01847(17) -0.00074(15) O1 0.056(3) 0.074(3) 0.081(4) 0.006(3) 0.017(3) 0.007(2) O2 0.077(4) 0.051(3) 0.098(4) 0.006(3) 0.031(3) 0.000(2) O3 0.062(3) 0.074(4) 0.083(4) 0.000(3) 0.012(3) -0.007(3) O4 0.083(4) 0.091(4) 0.079(4) 0.001(3) 0.039(3) 0.018(3) C1 0.050(3) 0.055(3) 0.061(4) 0.003(3) 0.012(3) 0.003(3) C2 0.055(3) 0.049(3) 0.067(4) -0.002(3) 0.022(3) -0.001(3) C3 0.051(3) 0.058(4) 0.066(4) -0.002(3) 0.006(3) -0.004(3) C4 0.053(3) 0.060(4) 0.069(4) 0.003(3) 0.022(3) 0.008(3) 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' H H 0.0000 0.0000 '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' N N 0.0061 0.0033 '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' Re Re -1.0185 7.2310 '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 C7 N1 C5 126.2(9) C8 N1 C5 125.3(9) C8 N1 C7 108.5(8) C6 N2 C9 125.9(8) C8 N2 C6 108.4(8) C8 N2 C9 125.7(8) N1 C5 H5A 109.5 N1 C5 H5B 109.5 N1 C5 H5C 109.5 H5A C5 H5B 109.5 H5A C5 H5C 109.5 H5B C5 H5C 109.5 N2 C6 H6 126.4 C7 C6 N2 107.2(9) C7 C6 H6 126.4 N1 C7 H7 126.2 C6 C7 N1 107.5(9) C6 C7 H7 126.2 N1 C8 N2 108.4(8) N1 C8 H8 125.8 N2 C8 H8 125.8 N2 C9 C10A 108.1(12) N2 C9 C10B 112.5(8) C9 C10A H10A 101.9 C9 C10A H10B 101.9 H10A C10A H10B 104.7 C11A C10A C9 140.5(19) C11A C10A H10A 101.9 C11A C10A H10B 101.9 C9 C10B H10C 104.2 C9 C10B H10D 104.2 H10C C10B H10D 105.5 C11B C10B C9 132.3(17) C11B C10B H10C 104.2 C11B C10B H10D 104.2 C10A C11A H11A 103.1 C10A C11A H11B 103.1 C10A C11A C12 136.1(18) H11A C11A H11B 105.1 C12 C11A H11A 103.1 C12 C11A H11B 103.1 C10B C11B H11C 105.3 C10B C11B H11D 105.3 C10B C11B C12 128(2) H11C C11B H11D 106.0 C12 C11B H11C 105.3 C12 C11B H11D 105.3 C11A C12 H12A 109.5 C11A C12 H12B 109.5 C11A C12 H12C 109.5 C11B C12 H12D 109.5 C11B C12 H12E 109.5 C11B C12 H12F 109.5 H12A C12 H12B 109.5 H12A C12 H12C 109.5 H12B C12 H12C 109.5 H12D C12 H12E 109.5 H12D C12 H12F 109.5 H12E C12 H12F 109.5 Te2 Re1 Te1 85.989(19) C1 Re1 Te1 90.0(2) C1 Re1 Te2 90.1(2) C1 Re1 C3 178.2(3) C2 Re1 Te1 89.6(2) C2 Re1 Te2 175.6(2) C2 Re1 C1 89.3(3) C2 Re1 C3 92.1(3) C3 Re1 Te1 91.1(2) C3 Re1 Te2 88.5(2) C4 Re1 Te1 177.1(2) C4 Re1 Te2 91.8(2) C4 Re1 C1 88.0(3) C4 Re1 C2 92.5(3) C4 Re1 C3 90.8(3) Re1 Te1 I3 91.98(2) Re1 Te1 I4 88.14(2) Re1 Te1 I5 98.06(3) Re1 Te1 I6 96.91(3) I3 Te1 I4 83.50(3) I5 Te1 I3 89.93(3) I5 Te1 I4 171.14(2) I5 Te1 I6 92.78(3) I6 Te1 I3 170.24(2) I6 Te1 I4 92.75(3) Re1 Te2 I2 99.69(2) I1 Te2 Re1 99.324(19) I1 Te2 I2 92.61(4) O1 C1 Re1 177.4(7) O2 C2 Re1 177.7(7) O3 C3 Re1 176.6(8) O4 C4 Re1 178.3(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance N1 C5 1.470(13) N1 C7 1.357(13) N1 C8 1.322(12) N2 C6 1.364(12) N2 C8 1.323(11) N2 C9 1.475(12) C5 H5A 0.9600 C5 H5B 0.9600 C5 H5C 0.9600 C6 H6 0.9300 C6 C7 1.333(15) C7 H7 0.9300 C8 H8 0.9300 C9 C10A 1.48(3) C9 C10B 1.557(18) C10A H10A 0.9700 C10A H10B 0.9700 C10A C11A 1.25(3) C10B H10C 0.9700 C10B H10D 0.9700 C10B C11B 1.15(3) C11A H11A 0.9700 C11A H11B 0.9700 C11A C12 1.477(18) C11B H11C 0.9700 C11B H11D 0.9700 C11B C12 1.61(3) C12 H12A 0.9600 C12 H12B 0.9600 C12 H12C 0.9600 C12 H12D 0.9600 C12 H12E 0.9600 C12 H12F 0.9600 Re1 Te1 2.7680(8) Re1 Te2 2.7664(8) Re1 C1 2.014(7) Re1 C2 1.959(7) Re1 C3 2.017(7) Re1 C4 1.941(8) I1 Te2 2.7589(9) I2 Te2 2.7934(11) I3 Te1 3.0027(10) I4 Te1 3.1478(9) I5 Te1 2.8350(9) I6 Te1 2.9210(10) O1 C1 1.112(9) O2 C2 1.119(9) O3 C3 1.123(9) O4 C4 1.128(10) loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion N2 C6 C7 N1 -0.3(11) N2 C9 C10A C11A -32(4) N2 C9 C10B C11B 17(3) C5 N1 C7 C6 178.5(9) C5 N1 C8 N2 -178.6(8) C6 N2 C8 N1 0.4(10) C6 N2 C9 C10A -60.9(15) C6 N2 C9 C10B -97.0(12) C7 N1 C8 N2 -0.5(10) C8 N1 C7 C6 0.5(11) C8 N2 C6 C7 -0.1(11) C8 N2 C9 C10A 118.9(14) C8 N2 C9 C10B 82.8(12) C9 N2 C6 C7 179.8(9) C9 N2 C8 N1 -179.5(8) C9 C10A C11A C12 -130(3) C9 C10B C11B C12 133(2)