#------------------------------------------------------------------------------ #$Date: 2021-10-20 02:23:35 +0300 (Wed, 20 Oct 2021) $ #$Revision: 270043 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/85/7708596.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_7708596 loop_ _publ_author_name 'Newman, Paul David' 'Kariuki, Benson' 'Lowy, Phoebe' 'Jerwood, Kimberley' 'Deeming, Laura' _publ_section_title ; Remote Control: Stereoselective Coordination of Electron-Deficient 2,2’-bipyridine Ligands to Re(I) and Ir(III) Cores ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT02928B _journal_year 2021 _chemical_absolute_configuration ad _chemical_formula_sum 'C23 H28.03 Cl0.89 I1.11 N4 O4.51 Re' _chemical_formula_weight 791.37 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/1 _audit_update_record ; 2021-10-02 deposited with the CCDC. 2021-10-07 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 92.751(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 9.9804(3) _cell_length_b 10.6322(3) _cell_length_c 12.5079(4) _cell_measurement_reflns_used 7589 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 28.6560 _cell_measurement_theta_min 4.1460 _cell_volume 1325.73(7) _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_structure_refinement 'SHELXL-2018/1 (Sheldrick, 2018)' _computing_structure_solution SHELXS _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.870 _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_unetI/netI 0.0454 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.870 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 13244 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.827 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.730 _diffrn_reflns_theta_min 3.192 _exptl_absorpt_coefficient_mu 6.003 _exptl_absorpt_correction_T_max 0.940 _exptl_absorpt_correction_T_min 0.507 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.982 _exptl_crystal_description needle _exptl_crystal_F_000 758 _exptl_crystal_size_max 0.194 _exptl_crystal_size_mid 0.081 _exptl_crystal_size_min 0.061 _refine_diff_density_max 1.009 _refine_diff_density_min -1.157 _refine_diff_density_rms 0.116 _refine_ls_abs_structure_details ; Flack x determined using 2406 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.030(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 343 _refine_ls_number_reflns 6236 _refine_ls_number_restraints 31 _refine_ls_restrained_S_all 1.040 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0290 _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^)+(0.0129P)^2^+1.0671P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.0522 _reflns_Friedel_coverage 0.809 _reflns_Friedel_fraction_full 0.998 _reflns_Friedel_fraction_max 0.779 _reflns_number_gt 5735 _reflns_number_total 6236 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt02928b2.cif _cod_data_source_block pdn1901 _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 7708596 _shelx_shelxl_version_number 2018/1 _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_estimated_absorpt_t_min 0.389 _shelx_estimated_absorpt_t_max 0.711 _shelx_res_file ; TITL pdn1901 in P2(1) shelx.res created by SHELXL-2018/1 at 16:18:11 on 27-Sep-2021 CELL 0.71073 9.9804 10.6322 12.5079 90.000 92.751 90.000 ZERR 2.00 0.0003 0.0003 0.0004 0.000 0.003 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H CL N O I RE UNIT 46 56.06 1.78 8 9.03 2.22 2 MERG 2 isor cl1 i1 simu cl1 i1 isor .01 o4 dfix .95 .01 o4 h41 o4 h42 dfix 1.55 .01 h41 h42 dfix .95 .01 o5 h51 o5 h52 dfix 1.55 .01 h51 h52 FMAP 2 PLAN 10 SIZE 0.061 0.081 0.194 ACTA BOND $H L.S. 4 TEMP 25.00 WGHT 0.012900 1.067100 FVAR 2.89879 0.89099 0.51583 MOLE 1 C1 1 0.345406 0.356259 -0.026197 11.00000 0.03353 0.02674 = 0.02983 0.00355 -0.00060 0.00301 AFIX 43 H1 2 0.333868 0.286602 -0.070660 11.00000 -1.20000 AFIX 0 C2 1 0.452245 0.433415 -0.041307 11.00000 0.02847 0.03508 = 0.04115 0.00700 0.00383 -0.00073 AFIX 43 H2 2 0.511692 0.416680 -0.094539 11.00000 -1.20000 AFIX 0 C3 1 0.469702 0.537223 0.024741 11.00000 0.02963 0.03868 = 0.05491 0.00796 -0.00133 -0.00976 AFIX 43 H3 2 0.542504 0.590658 0.017610 11.00000 -1.20000 AFIX 0 C4 1 0.378551 0.560193 0.100592 11.00000 0.03485 0.03511 = 0.04425 -0.00606 -0.00408 -0.01245 AFIX 43 H4 2 0.388555 0.629872 0.145209 11.00000 -1.20000 AFIX 0 C5 1 0.270345 0.478430 0.110687 11.00000 0.03016 0.02186 = 0.02448 0.00152 -0.00546 -0.00568 C6 1 0.164315 0.500216 0.187368 11.00000 0.03227 0.01928 = 0.02239 -0.00105 -0.00772 -0.00533 C7 1 0.158060 0.612034 0.243889 11.00000 0.04117 0.02182 = 0.03211 -0.00247 -0.00382 -0.01217 AFIX 43 H7 2 0.224647 0.672464 0.237886 11.00000 -1.20000 AFIX 0 C8 1 0.054033 0.633149 0.308285 11.00000 0.05579 0.02241 = 0.03638 -0.00865 0.00073 -0.00604 AFIX 43 H8 2 0.046601 0.709453 0.343866 11.00000 -1.20000 AFIX 0 C9 1 -0.039583 0.540242 0.319885 11.00000 0.04052 0.02480 = 0.03121 -0.00702 -0.00072 0.00250 AFIX 43 H9 2 -0.109632 0.551413 0.365382 11.00000 -1.20000 AFIX 0 C10 1 -0.027971 0.429344 0.262588 11.00000 0.02915 0.01690 = 0.02478 0.00122 -0.00178 0.00036 C11 1 -0.082735 0.224053 0.320958 11.00000 0.02765 0.02391 = 0.02345 0.00076 -0.00353 0.00362 AFIX 43 H11 2 0.008333 0.205413 0.321425 11.00000 -1.20000 AFIX 0 C12 1 -0.270568 0.361807 0.278757 11.00000 0.02928 0.02343 = 0.02427 -0.00104 0.00441 0.00703 AFIX 13 H12 2 -0.288659 0.451482 0.267096 11.00000 -1.20000 AFIX 0 C13 1 -0.343894 0.279792 0.194588 11.00000 0.02673 0.02954 = 0.02887 -0.00413 -0.00030 0.00520 AFIX 23 H13A 2 -0.288342 0.265440 0.134226 11.00000 -1.20000 H13B 2 -0.426929 0.319363 0.168982 11.00000 -1.20000 AFIX 0 C14 1 -0.372555 0.154228 0.252627 11.00000 0.02393 0.02745 = 0.03980 -0.01229 0.00647 -0.00027 AFIX 23 H14A 2 -0.468305 0.138936 0.253582 11.00000 -1.20000 H14B 2 -0.330774 0.084238 0.217272 11.00000 -1.20000 AFIX 0 C15 1 -0.312311 0.170781 0.365783 11.00000 0.03576 0.02035 = 0.03230 0.00612 0.00443 0.00091 C16 1 -0.322999 0.315125 0.385873 11.00000 0.03833 0.02266 = 0.02804 -0.00129 0.00594 0.00450 C17 1 -0.372911 0.088163 0.449032 11.00000 0.06088 0.02570 = 0.04628 -0.00107 0.02174 -0.00568 AFIX 137 H17A 2 -0.467051 0.105792 0.451486 11.00000 -1.50000 H17B 2 -0.329731 0.104786 0.517818 11.00000 -1.50000 H17C 2 -0.360462 0.001407 0.430695 11.00000 -1.50000 AFIX 0 C18 1 -0.469761 0.356471 0.393229 11.00000 0.04815 0.02938 = 0.04713 -0.00360 0.02214 -0.00010 AFIX 137 H18A 2 -0.501669 0.331959 0.461361 11.00000 -1.50000 H18B 2 -0.523619 0.317092 0.337057 11.00000 -1.50000 H18C 2 -0.475706 0.446199 0.385866 11.00000 -1.50000 AFIX 0 C19 1 -0.246711 0.364287 0.486202 11.00000 0.06921 0.02830 = 0.02991 -0.00740 0.01312 -0.00527 AFIX 137 H19A 2 -0.153215 0.344366 0.482627 11.00000 -1.50000 H19B 2 -0.281509 0.325541 0.548405 11.00000 -1.50000 H19C 2 -0.257492 0.453833 0.490590 11.00000 -1.50000 AFIX 0 C20 1 -0.111202 0.016573 0.388347 11.00000 0.04608 0.02431 = 0.05422 0.00788 -0.00583 0.00532 AFIX 137 H20A 2 -0.016879 0.013044 0.376786 11.00000 -1.50000 H20B 2 -0.157353 -0.044918 0.344086 11.00000 -1.50000 H20C 2 -0.125866 -0.000730 0.462202 11.00000 -1.50000 AFIX 0 C21 1 -0.043492 0.130770 0.110017 11.00000 0.02779 0.02415 = 0.03179 -0.01237 0.00442 0.00056 C22 1 -0.022911 0.315841 -0.028720 11.00000 0.04664 0.02084 = 0.02993 -0.00557 -0.01200 0.00085 C23 1 0.148061 0.122781 -0.018683 11.00000 0.02727 0.02138 = 0.02641 -0.00434 0.00208 -0.00799 CL1 3 0.251221 0.166810 0.224667 21.00000 0.03238 0.03061 = 0.03658 0.00185 -0.00663 0.00290 N1 4 0.256330 0.375010 0.048849 11.00000 0.02963 0.01999 = 0.02196 0.00398 -0.00237 -0.00108 N2 4 0.068779 0.408422 0.193255 11.00000 0.02404 0.01786 = 0.02235 0.00086 -0.00655 -0.00216 N3 4 -0.123842 0.332877 0.279524 11.00000 0.02945 0.01835 = 0.02107 -0.00112 -0.00035 -0.00279 N4 4 -0.162381 0.142302 0.360805 11.00000 0.03697 0.01551 = 0.02898 0.00266 -0.00325 0.00114 O1 5 -0.125331 0.056239 0.120138 11.00000 0.03859 0.03386 = 0.05737 -0.02298 0.01660 -0.01634 O2 5 -0.096704 0.351546 -0.094969 11.00000 0.07764 0.03798 = 0.05352 -0.00791 -0.03756 0.01405 O3 5 0.183541 0.046860 -0.076411 11.00000 0.04059 0.03224 = 0.03303 -0.01174 0.00784 -0.00390 I1 6 0.257151 0.130857 0.230066 -21.00000 0.02169 0.04156 = 0.02906 -0.00176 -0.00261 0.00253 I2 6 0.379619 0.229611 0.690028 11.00000 0.09166 0.03214 = 0.03184 0.00276 -0.00012 -0.00118 RE1 7 0.094378 0.247471 0.079745 11.00000 0.02379 0.01651 = 0.02287 -0.00195 -0.00248 -0.00139 MOLE 2 O4 5 0.164753 0.262109 0.463905 11.00000 0.05397 0.12598 = 0.07083 -0.04875 -0.01838 0.02076 H41 2 0.216579 0.199125 0.499834 11.00000 -1.50000 H42 2 0.210898 0.292565 0.404576 11.00000 -1.50000 MOLE 3 O5 5 0.334070 0.864234 0.240181 31.00000 0.04839 0.03725 = 0.08687 -0.00199 -0.00600 -0.00311 H51 2 0.370066 0.939983 0.213128 31.00000 -1.50000 H52 2 0.400770 0.823875 0.284971 31.00000 -1.50000 HKLF 4 REM pdn1901 in P2(1) REM R1 = 0.0290 for 5735 Fo > 4sig(Fo) and 0.0345 for all 6236 data REM 343 parameters refined using 31 restraints END WGHT 0.0129 1.0671 REM Highest difference peak 1.009, deepest hole -1.157, 1-sigma level 0.116 Q1 1 0.2815 0.7448 0.2428 11.00000 0.05 1.01 Q2 1 0.3268 0.2447 0.7242 11.00000 0.05 0.59 Q3 1 0.1714 0.2277 0.0631 11.00000 0.05 0.56 Q4 1 0.1137 0.2625 0.1420 11.00000 0.05 0.54 Q5 1 0.4337 0.2466 0.6952 11.00000 0.05 0.54 Q6 1 0.0050 0.2295 0.1022 11.00000 0.05 0.53 Q7 1 0.0997 0.2400 -0.0083 11.00000 0.05 0.51 Q8 1 0.3026 0.2246 0.1424 11.00000 0.05 0.48 Q9 1 0.1736 0.3005 0.0410 11.00000 0.05 0.47 Q10 1 0.3267 0.2428 0.6370 11.00000 0.05 0.45 ; _shelx_res_checksum 88375 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -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 _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3454(7) 0.3563(7) -0.0262(6) 0.0301(16) Uani 1 1 d . . . . . H1 H 0.333868 0.286602 -0.070660 0.036 Uiso 1 1 calc R U . . . C2 C 0.4522(8) 0.4334(7) -0.0413(7) 0.0348(19) Uani 1 1 d . . . . . H2 H 0.511692 0.416680 -0.094539 0.042 Uiso 1 1 calc R U . . . C3 C 0.4697(8) 0.5372(8) 0.0247(7) 0.041(2) Uani 1 1 d . . . . . H3 H 0.542504 0.590658 0.017610 0.049 Uiso 1 1 calc R U . . . C4 C 0.3786(8) 0.5602(8) 0.1006(7) 0.0383(19) Uani 1 1 d . . . . . H4 H 0.388555 0.629872 0.145209 0.046 Uiso 1 1 calc R U . . . C5 C 0.2703(7) 0.4784(6) 0.1107(5) 0.0257(16) Uani 1 1 d . . . . . C6 C 0.1643(7) 0.5002(6) 0.1874(5) 0.0249(15) Uani 1 1 d . . . . . C7 C 0.1581(8) 0.6120(7) 0.2439(6) 0.0319(17) Uani 1 1 d . . . . . H7 H 0.224647 0.672464 0.237886 0.038 Uiso 1 1 calc R U . . . C8 C 0.0540(9) 0.6331(7) 0.3083(6) 0.0382(19) Uani 1 1 d . . . . . H8 H 0.046601 0.709453 0.343866 0.046 Uiso 1 1 calc R U . . . C9 C -0.0396(8) 0.5402(7) 0.3199(6) 0.0323(17) Uani 1 1 d . . . . . H9 H -0.109632 0.551413 0.365382 0.039 Uiso 1 1 calc R U . . . C10 C -0.0280(7) 0.4293(6) 0.2626(6) 0.0237(15) Uani 1 1 d . . . . . C11 C -0.0827(7) 0.2241(7) 0.3210(5) 0.0252(16) Uani 1 1 d . . . . . H11 H 0.008333 0.205413 0.321425 0.030 Uiso 1 1 calc R U . . . C12 C -0.2706(7) 0.3618(7) 0.2788(5) 0.0256(15) Uani 1 1 d . . . . . H12 H -0.288659 0.451482 0.267096 0.031 Uiso 1 1 calc R U . . . C13 C -0.3439(7) 0.2798(6) 0.1946(6) 0.0284(17) Uani 1 1 d . . . . . H13A H -0.288342 0.265440 0.134226 0.034 Uiso 1 1 calc R U . . . H13B H -0.426929 0.319363 0.168982 0.034 Uiso 1 1 calc R U . . . C14 C -0.3726(7) 0.1542(7) 0.2526(6) 0.0302(17) Uani 1 1 d . . . . . H14A H -0.468305 0.138936 0.253582 0.036 Uiso 1 1 calc R U . . . H14B H -0.330774 0.084238 0.217272 0.036 Uiso 1 1 calc R U . . . C15 C -0.3123(10) 0.1708(8) 0.3658(8) 0.029(2) Uani 1 1 d . . . . . C16 C -0.3230(10) 0.3151(8) 0.3859(8) 0.030(2) Uani 1 1 d . . . . . C17 C -0.3729(9) 0.0882(7) 0.4490(7) 0.044(2) Uani 1 1 d . . . . . H17A H -0.467051 0.105792 0.451486 0.066 Uiso 1 1 calc R U . . . H17B H -0.329731 0.104786 0.517818 0.066 Uiso 1 1 calc R U . . . H17C H -0.360462 0.001407 0.430695 0.066 Uiso 1 1 calc R U . . . C18 C -0.4698(8) 0.3565(7) 0.3932(7) 0.041(2) Uani 1 1 d . . . . . H18A H -0.501669 0.331959 0.461361 0.061 Uiso 1 1 calc R U . . . H18B H -0.523619 0.317092 0.337057 0.061 Uiso 1 1 calc R U . . . H18C H -0.475706 0.446199 0.385866 0.061 Uiso 1 1 calc R U . . . C19 C -0.2467(9) 0.3643(7) 0.4862(6) 0.042(2) Uani 1 1 d . . . . . H19A H -0.153215 0.344366 0.482627 0.063 Uiso 1 1 calc R U . . . H19B H -0.281509 0.325541 0.548405 0.063 Uiso 1 1 calc R U . . . H19C H -0.257492 0.453833 0.490590 0.063 Uiso 1 1 calc R U . . . C20 C -0.1112(8) 0.0166(7) 0.3883(7) 0.042(2) Uani 1 1 d . . . . . H20A H -0.016879 0.013044 0.376786 0.063 Uiso 1 1 calc R U . . . H20B H -0.157353 -0.044918 0.344086 0.063 Uiso 1 1 calc R U . . . H20C H -0.125866 -0.000730 0.462202 0.063 Uiso 1 1 calc R U . . . C21 C -0.0435(7) 0.1308(7) 0.1100(6) 0.0278(16) Uani 1 1 d . . . . . C22 C -0.0229(8) 0.3158(7) -0.0287(6) 0.0329(18) Uani 1 1 d . . . . . C23 C 0.1481(7) 0.1228(6) -0.0187(6) 0.0250(15) Uani 1 1 d . . . . . Cl1 Cl 0.2512(11) 0.1668(6) 0.2247(10) 0.0335(15) Uani 0.891(3) 1 d . U P . . N1 N 0.2563(6) 0.3750(5) 0.0488(4) 0.0240(13) Uani 1 1 d . . . . . N2 N 0.0688(5) 0.4084(5) 0.1933(4) 0.0217(12) Uani 1 1 d . . . . . N3 N -0.1238(6) 0.3329(5) 0.2795(5) 0.0230(12) Uani 1 1 d . . . . . N4 N -0.1624(6) 0.1423(5) 0.3608(5) 0.0273(13) Uani 1 1 d . . . . . O1 O -0.1253(5) 0.0562(5) 0.1201(5) 0.0428(15) Uani 1 1 d . . . . . O2 O -0.0967(7) 0.3515(6) -0.0950(5) 0.0577(19) Uani 1 1 d . . . . . O3 O 0.1835(5) 0.0469(5) -0.0764(4) 0.0351(12) Uani 1 1 d . . . . . I1 I 0.257(2) 0.1309(15) 0.2301(19) 0.031(3) Uani 0.109(3) 1 d . U P . . I2 I 0.37962(7) 0.22961(6) 0.69003(4) 0.05198(17) Uani 1 1 d . . . . . Re1 Re 0.09438(2) 0.24747(3) 0.07975(2) 0.02118(7) Uani 1 1 d . . . . . O4 O 0.1648(6) 0.2621(12) 0.4639(6) 0.084(3) Uani 1 1 d D U . . . H41 H 0.217(10) 0.199(8) 0.500(8) 0.126 Uiso 1 1 d D U . . . H42 H 0.211(10) 0.293(10) 0.405(6) 0.126 Uiso 1 1 d D U . . . O5 O 0.3341(12) 0.8642(11) 0.2402(12) 0.058(5) Uani 0.516(18) 1 d D . P . . H51 H 0.370(15) 0.940(10) 0.213(15) 0.087 Uiso 0.516(18) 1 d D U P . . H52 H 0.401(12) 0.824(14) 0.285(13) 0.087 Uiso 0.516(18) 1 d D U P . . 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 C1 0.034(4) 0.027(4) 0.030(4) 0.004(3) -0.001(3) 0.003(3) C2 0.028(4) 0.035(4) 0.041(5) 0.007(4) 0.004(4) -0.001(3) C3 0.030(5) 0.039(5) 0.055(6) 0.008(4) -0.001(4) -0.010(4) C4 0.035(5) 0.035(4) 0.044(5) -0.006(4) -0.004(4) -0.012(4) C5 0.030(4) 0.022(4) 0.024(4) 0.002(3) -0.005(3) -0.006(3) C6 0.032(4) 0.019(3) 0.022(4) -0.001(3) -0.008(3) -0.005(3) C7 0.041(5) 0.022(4) 0.032(4) -0.002(3) -0.004(3) -0.012(3) C8 0.056(5) 0.022(4) 0.036(5) -0.009(3) 0.001(4) -0.006(4) C9 0.041(4) 0.025(4) 0.031(4) -0.007(3) -0.001(3) 0.003(3) C10 0.029(4) 0.017(3) 0.025(4) 0.001(3) -0.002(3) 0.000(3) C11 0.028(3) 0.024(5) 0.023(3) 0.001(3) -0.004(2) 0.004(3) C12 0.029(4) 0.023(4) 0.024(4) -0.001(3) 0.004(3) 0.007(3) C13 0.027(3) 0.030(5) 0.029(4) -0.004(3) 0.000(3) 0.005(3) C14 0.024(4) 0.027(4) 0.040(5) -0.012(4) 0.006(3) 0.000(3) C15 0.036(5) 0.020(4) 0.032(5) 0.006(4) 0.004(4) 0.001(4) C16 0.038(5) 0.023(4) 0.028(5) -0.001(3) 0.006(4) 0.005(4) C17 0.061(6) 0.026(4) 0.046(5) -0.001(4) 0.022(4) -0.006(4) C18 0.048(5) 0.029(4) 0.047(5) -0.004(4) 0.022(4) 0.000(4) C19 0.069(6) 0.028(4) 0.030(4) -0.007(4) 0.013(4) -0.005(4) C20 0.046(5) 0.024(4) 0.054(6) 0.008(4) -0.006(4) 0.005(4) C21 0.028(4) 0.024(4) 0.032(4) -0.012(3) 0.004(3) 0.001(3) C22 0.047(5) 0.021(4) 0.030(4) -0.006(3) -0.012(3) 0.001(3) C23 0.027(4) 0.021(4) 0.026(4) -0.004(3) 0.002(3) -0.008(3) Cl1 0.032(2) 0.031(3) 0.037(2) 0.002(3) -0.0066(13) 0.003(2) N1 0.030(3) 0.020(3) 0.022(3) 0.004(2) -0.002(2) -0.001(2) N2 0.024(3) 0.018(3) 0.022(3) 0.001(2) -0.007(2) -0.002(2) N3 0.029(3) 0.018(3) 0.021(3) -0.001(2) 0.000(2) -0.003(2) N4 0.037(4) 0.016(3) 0.029(4) 0.003(3) -0.003(3) 0.001(3) O1 0.039(3) 0.034(3) 0.057(4) -0.023(3) 0.017(3) -0.016(3) O2 0.078(5) 0.038(4) 0.054(4) -0.008(3) -0.038(4) 0.014(3) O3 0.041(3) 0.032(3) 0.033(3) -0.012(2) 0.008(2) -0.004(2) I1 0.022(4) 0.042(9) 0.029(4) -0.002(6) -0.003(3) 0.003(6) I2 0.0917(4) 0.0321(4) 0.0318(3) 0.0028(3) -0.0001(2) -0.0012(3) Re1 0.02379(12) 0.01651(11) 0.02287(12) -0.00195(15) -0.00248(8) -0.00139(15) O4 0.054(4) 0.126(7) 0.071(5) -0.049(6) -0.018(3) 0.021(6) O5 0.048(8) 0.037(7) 0.087(11) -0.002(7) -0.006(7) -0.003(6) 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' Cl Cl 0.1484 0.1585 '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' 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 123.8(7) . . ? N1 C1 H1 118.1 . . ? C2 C1 H1 118.1 . . ? C1 C2 C3 118.2(8) . . ? C1 C2 H2 120.9 . . ? C3 C2 H2 120.9 . . ? C4 C3 C2 119.2(8) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 119.6(7) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? N1 C5 C4 121.0(7) . . ? N1 C5 C6 116.2(6) . . ? C4 C5 C6 122.8(6) . . ? N2 C6 C7 122.4(7) . . ? N2 C6 C5 116.4(6) . . ? C7 C6 C5 121.1(6) . . ? C8 C7 C6 119.8(7) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C7 C8 C9 119.1(7) . . ? C7 C8 H8 120.5 . . ? C9 C8 H8 120.5 . . ? C8 C9 C10 118.9(7) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? N2 C10 C9 123.6(6) . . ? N2 C10 N3 118.9(6) . . ? C9 C10 N3 117.5(6) . . ? N4 C11 N3 123.6(6) . . ? N4 C11 H11 118.2 . . ? N3 C11 H11 118.2 . . ? N3 C12 C13 108.9(5) . . ? N3 C12 C16 107.5(6) . . ? C13 C12 C16 104.1(6) . . ? N3 C12 H12 112.0 . . ? C13 C12 H12 112.0 . . ? C16 C12 H12 112.0 . . ? C12 C13 C14 105.2(6) . . ? C12 C13 H13A 110.7 . . ? C14 C13 H13A 110.7 . . ? C12 C13 H13B 110.7 . . ? C14 C13 H13B 110.7 . . ? H13A C13 H13B 108.8 . . ? C15 C14 C13 105.2(6) . . ? C15 C14 H14A 110.7 . . ? C13 C14 H14A 110.7 . . ? C15 C14 H14B 110.7 . . ? C13 C14 H14B 110.7 . . ? H14A C14 H14B 108.8 . . ? C17 C15 C14 114.9(8) . . ? C17 C15 N4 109.7(7) . . ? C14 C15 N4 106.4(7) . . ? C17 C15 C16 115.4(8) . . ? C14 C15 C16 103.7(8) . . ? N4 C15 C16 106.0(8) . . ? C19 C16 C18 107.0(7) . . ? C19 C16 C12 115.2(7) . . ? C18 C16 C12 108.9(7) . . ? C19 C16 C15 115.7(9) . . ? C18 C16 C15 111.3(9) . . ? C12 C16 C15 98.5(7) . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N4 C20 H20A 109.5 . . ? N4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O1 C21 Re1 174.4(6) . . ? O2 C22 Re1 176.7(7) . . ? O3 C23 Re1 178.2(7) . . ? C1 N1 C5 118.0(6) . . ? C1 N1 Re1 124.1(5) . . ? C5 N1 Re1 117.9(5) . . ? C10 N2 C6 116.1(6) . . ? C10 N2 Re1 129.8(4) . . ? C6 N2 Re1 114.1(5) . . ? C11 N3 C10 119.3(6) . . ? C11 N3 C12 117.8(6) . . ? C10 N3 C12 121.0(6) . . ? C11 N4 C20 119.3(6) . . ? C11 N4 C15 120.2(6) . . ? C20 N4 C15 120.1(6) . . ? C22 Re1 C23 89.3(3) . . ? C22 Re1 C21 88.0(3) . . ? C23 Re1 C21 84.5(3) . . ? C22 Re1 N1 94.2(3) . . ? C23 Re1 N1 94.9(2) . . ? C21 Re1 N1 177.7(3) . . ? C22 Re1 N2 94.3(3) . . ? C23 Re1 N2 169.6(2) . . ? C21 Re1 N2 105.4(2) . . ? N1 Re1 N2 75.1(2) . . ? C22 Re1 Cl1 177.6(3) . . ? C23 Re1 Cl1 92.5(3) . . ? C21 Re1 Cl1 93.8(3) . . ? N1 Re1 Cl1 84.1(3) . . ? N2 Re1 Cl1 83.6(3) . . ? C22 Re1 I1 175.5(5) . . ? C23 Re1 I1 87.3(5) . . ? C21 Re1 I1 88.8(5) . . ? N1 Re1 I1 89.0(5) . . ? N2 Re1 I1 89.6(5) . . ? Cl1 Re1 I1 6.9(6) . . ? H41 O4 H42 110(2) . . ? H51 O5 H52 109(2) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.338(9) . ? C1 C2 1.366(10) . ? C1 H1 0.9300 . ? C2 C3 1.385(11) . ? C2 H2 0.9300 . ? C3 C4 1.368(11) . ? C3 H3 0.9300 . ? C4 C5 1.397(10) . ? C4 H4 0.9300 . ? C5 N1 1.348(8) . ? C5 C6 1.480(10) . ? C6 N2 1.369(8) . ? C6 C7 1.386(10) . ? C7 C8 1.363(11) . ? C7 H7 0.9300 . ? C8 C9 1.372(11) . ? C8 H8 0.9300 . ? C9 C10 1.388(10) . ? C9 H9 0.9300 . ? C10 N2 1.347(9) . ? C10 N3 1.425(8) . ? C11 N4 1.294(9) . ? C11 N3 1.325(9) . ? C11 H11 0.9300 . ? C12 N3 1.496(9) . ? C12 C13 1.527(9) . ? C12 C16 1.544(11) . ? C12 H12 0.9800 . ? C13 C14 1.553(10) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.521(12) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C17 1.511(11) . ? C15 N4 1.531(11) . ? C15 C16 1.560(9) . ? C16 C19 1.528(12) . ? C16 C18 1.536(12) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 N4 1.466(9) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 O1 1.149(8) . ? C21 Re1 1.904(7) . ? C22 O2 1.147(9) . ? C22 Re1 1.894(8) . ? C23 O3 1.150(8) . ? C23 Re1 1.904(7) . ? Cl1 Re1 2.490(10) . ? N1 Re1 2.159(6) . ? N2 Re1 2.246(5) . ? I1 Re1 2.72(2) . ? O4 H41 0.946(14) . ? O4 H42 0.949(14) . ? O5 H51 0.951(14) . ? O5 H52 0.951(14) . ?