#------------------------------------------------------------------------------ #$Date: 2026-06-30 01:17:23 +0100 (Tue, 30 Jun 2026) $ #$Revision: 306684 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/11/7721184.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_7721184 loop_ _publ_author_name 'Jacobs, Frederick J. F.' 'Fourie, Eleanor' 'Brink, Alice' _publ_section_title ; Engineering the rhenium metalation of phenanthroline imino complexes for variable structure activity relationships. ; _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_paper_doi 10.1039/d6dt00636a _journal_year 2026 _chemical_formula_sum 'C32 H24 Cl N3 O4 Re' _chemical_formula_weight 736.19 _chemical_name_common fac-[Re(CO)3(Phen5MeSalH)(Cl)] _chemical_name_systematic fac-Tricarbonyl-{2-([1,10-phenanthrolin-5-ylimino]methyl)phenol-N,N'}-(chlorido)-rhenium(I) _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2026-06-02 deposited with the CCDC. 2026-06-15 downloaded from the CCDC. ; _cell_angle_alpha 110.547(5) _cell_angle_beta 91.907(5) _cell_angle_gamma 116.622(4) _cell_formula_units_Z 2 _cell_length_a 10.9122(15) _cell_length_b 10.9820(13) _cell_length_c 14.3688(19) _cell_measurement_reflns_used 9422 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 2.453 _cell_measurement_theta_min 28.322 _cell_volume 1403.6(3) _computing_data_collection 'APEX5 (Bruker, 2016)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.963 _diffrn_measured_fraction_theta_max 0.932 _diffrn_measurement_device_type 'Bruker D8 Quest Eco Chi Photon II CPAD diffractometer' _diffrn_measurement_method 'phi and omega scan methods were used' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_unetI/netI 0.0523 _diffrn_reflns_Laue_measured_fraction_full 0.963 _diffrn_reflns_Laue_measured_fraction_max 0.932 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 26522 _diffrn_reflns_point_group_measured_fraction_full 0.963 _diffrn_reflns_point_group_measured_fraction_max 0.932 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.349 _diffrn_reflns_theta_min 2.921 _exptl_absorpt_coefficient_mu 4.467 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.5515 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1199 before and 0.0656 after correction. The Ratio of minimum to maximum transmission is 0.7396. The \l/2 correction factor is Not present. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.742 _exptl_crystal_description needle _exptl_crystal_F_000 722 _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.038 _exptl_crystal_size_min 0.032 _refine_diff_density_max 1.391 _refine_diff_density_min -2.227 _refine_diff_density_rms 0.215 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.184 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 370 _refine_ls_number_reflns 6553 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.184 _refine_ls_R_factor_all 0.0549 _refine_ls_R_factor_gt 0.0397 _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^)+6.5887P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0750 _refine_ls_wR_factor_ref 0.0817 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5564 _reflns_number_total 6553 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00636a2.cif _cod_data_source_block q1_22ffj1_0m _cod_database_code 7721184 _shelx_shelxl_version_number 2018/3 _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 0.348 _shelx_estimated_absorpt_t_max 0.870 _shelx_res_file ; TITL q1_22ffj1_0m_a.res in P-1 q1_22ffj1_0m.res created by SHELXL-2018/3 at 20:15:10 on 31-May-2026 REM Old TITL Q1_22Ffj1_0m in P-1 #2 REM SHELXT solution in P-1: R1 0.078, Rweak 0.018, Alpha 0.033 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C32 Cl N2 O5 Re CELL 0.71073 10.9122 10.982 14.3688 110.547 91.907 116.622 ZERR 2 0.0015 0.0013 0.0019 0.005 0.005 0.004 LATT 1 SFAC C H Cl N O Re UNIT 64 48 2 6 8 2 EADP C27A C28B EADP C26A C25B EADP C25A C24B EADP C24A C29B EADP C29A C27B EADP C28A C26B L.S. 12 PLAN 5 SIZE 0.032 0.038 0.3 TEMP -173.15 CONF HTAB O4 N3 BOND list 4 MORE -1 BOND $H fmap 2 53 acta OMIT -4 -7 17 OMIT -2 -9 17 OMIT -2 0 3 OMIT 2 -13 12 OMIT 4 -14 10 OMIT 4 -14 11 OMIT 4 -13 10 OMIT 4 -13 13 OMIT 4 -12 12 OMIT 5 -13 13 OMIT 5 -12 12 REM REM REM WGHT 0.000000 6.588700 FVAR 0.30673 0.66861 RE01 6 0.948587 0.736680 0.759849 11.00000 0.01706 0.02383 = 0.01711 0.00471 0.00265 0.01136 CL02 3 0.950321 0.813232 0.616895 11.00000 0.02406 0.03737 = 0.02508 0.01497 0.00797 0.01872 O2 5 1.087301 1.058412 0.923851 11.00000 0.03744 0.02192 = 0.03672 0.00002 0.00995 0.00937 N2 4 0.730670 0.690553 0.743453 11.00000 0.01694 0.02175 = 0.01734 0.00543 0.00441 0.00906 O3 5 1.233958 0.752238 0.744287 11.00000 0.02431 0.04495 = 0.02865 0.00475 0.00424 0.02242 O1 5 0.932657 0.633292 0.933110 11.00000 0.04448 0.04389 = 0.02893 0.01796 0.00562 0.02046 N1 4 0.829601 0.513312 0.636706 11.00000 0.01925 0.02030 = 0.01859 0.00060 0.00191 0.01083 C1 1 1.036764 0.939848 0.862035 11.00000 0.02311 0.03262 = 0.03132 0.01672 0.01212 0.01525 O4 5 0.287147 -0.061297 0.232896 11.00000 0.02940 0.03361 = 0.02755 0.00219 0.01030 0.00388 C11 1 0.689429 0.463450 0.607853 11.00000 0.01718 0.02176 = 0.01511 0.00653 0.00309 0.01055 N3 4 0.364497 0.136815 0.424156 11.00000 0.01905 0.02692 = 0.01920 0.00504 -0.00014 0.01070 C9 1 0.637624 0.558517 0.664849 11.00000 0.01729 0.01870 = 0.01475 0.00380 0.00333 0.00915 C2 1 0.937513 0.669792 0.867480 11.00000 0.02064 0.02466 = 0.03119 0.00571 0.00110 0.01033 C12 1 0.600017 0.327268 0.527191 11.00000 0.02103 0.02789 = 0.01958 0.00878 0.00411 0.01360 C3 1 1.129460 0.751016 0.754265 11.00000 0.03444 0.02915 = 0.01316 -0.00045 -0.00042 0.01936 C6 1 0.447313 0.609689 0.697006 11.00000 0.01681 0.02884 = 0.02593 0.01151 0.00776 0.01345 AFIX 43 H6 2 0.351668 0.585001 0.680954 11.00000 -1.20000 AFIX 0 C10 1 0.451676 0.279249 0.504623 11.00000 0.01879 0.02286 = 0.01769 0.00546 0.00113 0.00722 C7 1 0.493269 0.511567 0.639068 11.00000 0.01723 0.01887 = 0.01896 0.00548 0.00462 0.00745 C15 1 0.882695 0.430167 0.584412 11.00000 0.02065 0.03192 = 0.02767 0.00488 0.00245 0.01618 AFIX 43 H15 2 0.980284 0.464571 0.604498 11.00000 -1.20000 AFIX 0 C8 1 0.402480 0.370067 0.557808 11.00000 0.01533 0.02711 = 0.02115 0.01165 0.00484 0.01152 AFIX 43 H8 2 0.305146 0.338570 0.540459 11.00000 -1.20000 AFIX 0 C4 1 0.681870 0.777385 0.796883 11.00000 0.02109 0.02735 = 0.02412 0.00813 0.00374 0.01298 AFIX 43 H4A 2 0.746059 0.869244 0.851831 11.00000 -1.20000 AFIX 0 C14 1 0.801155 0.294868 0.501494 11.00000 0.02847 0.03432 = 0.02811 0.00441 0.00704 0.02086 AFIX 43 H14 2 0.843055 0.238889 0.465112 11.00000 -1.20000 AFIX 0 C17 1 0.143129 -0.089484 0.355145 11.00000 0.02580 0.02267 = 0.02252 0.01105 0.00320 0.01367 C22 1 0.167287 -0.141984 0.257101 11.00000 0.02609 0.02763 = 0.02400 0.01215 0.00542 0.01257 C13 1 0.660003 0.242342 0.472308 11.00000 0.02449 0.03238 = 0.02562 0.00608 0.00500 0.01467 AFIX 43 H13 2 0.603075 0.149649 0.415673 11.00000 -1.20000 AFIX 0 C5 1 0.541576 0.741056 0.776717 11.00000 0.02142 0.02566 = 0.02484 0.00535 0.00816 0.01416 AFIX 43 H5 2 0.511180 0.806483 0.817687 11.00000 -1.20000 AFIX 0 C19 1 -0.083673 -0.312093 0.298653 11.00000 0.02569 0.02385 = 0.03815 0.01043 0.01008 0.00511 AFIX 43 H19 2 -0.169811 -0.369782 0.313319 11.00000 -1.20000 AFIX 0 C32 1 0.642639 0.065440 0.003315 11.00000 0.02725 0.03428 = 0.02789 0.00530 0.00316 0.00709 AFIX 43 H32 2 0.740722 0.110609 0.005717 11.00000 -1.20000 AFIX 0 C21 1 0.066053 -0.278706 0.181697 11.00000 0.03090 0.02588 = 0.01935 0.00354 0.00272 0.01076 AFIX 43 H21 2 0.084180 -0.313250 0.115999 11.00000 -1.20000 AFIX 0 C18 1 0.015022 -0.179535 0.372877 11.00000 0.03110 0.02988 = 0.02897 0.01417 0.00956 0.01125 AFIX 43 H18 2 -0.003437 -0.147031 0.438693 11.00000 -1.20000 AFIX 0 C16 1 0.243535 0.051770 0.435169 11.00000 0.02764 0.02066 = 0.02081 0.00771 0.00513 0.01468 AFIX 43 H16 2 0.219417 0.083541 0.498851 11.00000 -1.20000 AFIX 0 C20 1 -0.060314 -0.365012 0.200766 11.00000 0.02950 0.02076 = 0.03546 0.00868 -0.00173 0.01026 C30 1 0.439868 -0.106217 0.039431 11.00000 0.04860 0.02495 = 0.02254 0.01059 0.00612 0.01266 AFIX 43 H30 2 0.398419 -0.178998 0.066594 11.00000 -1.20000 AFIX 0 C31 1 0.582814 -0.041433 0.042856 11.00000 0.04679 0.03100 = 0.02161 0.00178 -0.00172 0.02037 AFIX 43 H31 2 0.639542 -0.069791 0.071991 11.00000 -1.20000 AFIX 0 C23 1 -0.170298 -0.510531 0.117489 11.00000 0.03492 0.03140 = 0.03690 0.00469 -0.00324 0.01292 AFIX 137 H23A 2 -0.131393 -0.577979 0.093377 11.00000 -1.50000 H23B 2 -0.198528 -0.491888 0.060673 11.00000 -1.50000 H23C 2 -0.252525 -0.556394 0.144243 11.00000 -1.50000 AFIX 66 PART 1 C24A 1 0.319614 0.202117 0.776960 21.00000 0.04335 0.04106 = 0.06396 0.03479 0.01456 0.02358 AFIX 43 H24A 2 0.222363 0.162168 0.777161 21.00000 -1.20000 AFIX 65 C29A 1 0.417029 0.341911 0.850837 21.00000 0.07059 0.06665 = 0.05981 0.04021 0.02597 0.04243 AFIX 43 H29A 2 0.386358 0.397504 0.901528 21.00000 -1.20000 AFIX 65 C28A 1 0.559321 0.400363 0.850543 21.00000 0.05210 0.05839 = 0.04485 0.02894 0.00671 0.02570 AFIX 43 H28A 2 0.625900 0.495905 0.901035 21.00000 -1.20000 AFIX 65 C27A 1 0.604199 0.319022 0.776373 21.00000 0.04645 0.04667 = 0.05351 0.03605 0.01132 0.01812 AFIX 43 H27A 2 0.701449 0.358972 0.776173 21.00000 -1.20000 AFIX 65 C26A 1 0.506785 0.179228 0.702497 21.00000 0.05117 0.04149 = 0.04349 0.03098 0.01588 0.01686 AFIX 43 H26A 2 0.537457 0.123636 0.651805 21.00000 -1.20000 AFIX 65 C25A 1 0.364492 0.120775 0.702789 21.00000 0.04952 0.02967 = 0.04565 0.02022 0.00348 0.01824 AFIX 43 H25A 2 0.297914 0.025232 0.652297 21.00000 -1.20000 AFIX 66 PART -1 C28B 1 0.597225 0.317326 0.789121 -21.00000 0.04645 0.04667 = 0.05351 0.03605 0.01132 0.01812 AFIX 43 H28B 2 0.689446 0.335238 0.782512 -21.00000 -1.20000 AFIX 65 C25B 1 0.480990 0.181830 0.725808 -21.00000 0.05117 0.04149 = 0.04349 0.03098 0.01588 0.01686 AFIX 43 H25B 2 0.493770 0.107137 0.675927 -21.00000 -1.20000 AFIX 65 C24B 1 0.346055 0.155621 0.735479 -21.00000 0.04952 0.02967 = 0.04565 0.02022 0.00348 0.01824 AFIX 43 H24B 2 0.266615 0.063015 0.692207 -21.00000 -1.20000 AFIX 65 C29B 1 0.327355 0.264907 0.808463 -21.00000 0.04335 0.04106 = 0.06396 0.03479 0.01456 0.02358 AFIX 43 H29B 2 0.235132 0.246994 0.815072 -21.00000 -1.20000 AFIX 65 C27B 1 0.443588 0.400404 0.871776 -21.00000 0.07059 0.06665 = 0.05981 0.04021 0.02597 0.04243 AFIX 43 H27B 2 0.430806 0.475096 0.921658 -21.00000 -1.20000 AFIX 65 C26B 1 0.578523 0.426615 0.862107 -21.00000 0.05210 0.05839 = 0.04485 0.02894 0.00671 0.02570 AFIX 43 H26B 2 0.657964 0.519221 0.905379 -21.00000 -1.20000 AFIX 0 PART 0 H4 2 0.338599 0.016891 0.288745 11.00000 0.06894 HKLF 4 REM q1_22ffj1_0m_a.res in P-1 REM wR2 = 0.0817, GooF = S = 1.184, Restrained GooF = 1.184 for all data REM R1 = 0.0397 for 5564 Fo > 4sig(Fo) and 0.0549 for all 6553 data REM 370 parameters refined using 0 restraints END WGHT 0.0000 6.5889 REM Highest difference peak 1.391, deepest hole -2.227, 1-sigma level 0.215 Q1 1 0.9795 0.7435 0.8395 11.00000 0.05 1.39 Q2 1 1.1596 0.7958 0.7215 11.00000 0.05 1.31 Q3 1 0.8882 0.6783 0.7256 11.00000 0.05 1.27 Q4 1 0.9061 0.7252 0.6750 11.00000 0.05 1.22 Q5 1 0.8890 0.6202 0.6540 11.00000 0.05 1.22 ; _shelx_res_checksum 24886 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 _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Re01 Re 0.94859(2) 0.73668(3) 0.75985(2) 0.01997(7) Uani 1 1 d . . . . . Cl02 Cl 0.95032(13) 0.81323(16) 0.61690(10) 0.0266(3) Uani 1 1 d . . . . . O2 O 1.0873(4) 1.0584(5) 0.9239(3) 0.0380(10) Uani 1 1 d . . . . . N2 N 0.7307(4) 0.6906(5) 0.7435(3) 0.0197(9) Uani 1 1 d . . . . . O3 O 1.2340(4) 0.7522(5) 0.7443(3) 0.0337(10) Uani 1 1 d . . . . . O1 O 0.9327(5) 0.6333(5) 0.9331(3) 0.0387(10) Uani 1 1 d . . . . . N1 N 0.8296(4) 0.5133(5) 0.6367(3) 0.0213(9) Uani 1 1 d . . . . . C1 C 1.0368(6) 0.9398(7) 0.8620(4) 0.0270(12) Uani 1 1 d . . . . . O4 O 0.2871(4) -0.0613(5) 0.2329(3) 0.0382(11) Uani 1 1 d . . . . . C11 C 0.6894(5) 0.4635(6) 0.6079(4) 0.0179(10) Uani 1 1 d . . . . . N3 N 0.3645(4) 0.1368(5) 0.4242(3) 0.0235(10) Uani 1 1 d . . . . . C9 C 0.6376(5) 0.5585(6) 0.6648(4) 0.0178(10) Uani 1 1 d . . . . . C2 C 0.9375(6) 0.6698(7) 0.8675(4) 0.0278(12) Uani 1 1 d . . . . . C12 C 0.6000(5) 0.3273(6) 0.5272(4) 0.0225(11) Uani 1 1 d . . . . . C3 C 1.1295(6) 0.7510(7) 0.7543(4) 0.0270(12) Uani 1 1 d . . . . . C6 C 0.4473(5) 0.6097(6) 0.6970(4) 0.0227(11) Uani 1 1 d . . . . . H6 H 0.351668 0.585001 0.680954 0.027 Uiso 1 1 calc R U . . . C10 C 0.4517(5) 0.2792(6) 0.5046(4) 0.0220(11) Uani 1 1 d . . . . . C7 C 0.4933(5) 0.5116(6) 0.6391(4) 0.0197(10) Uani 1 1 d . . . . . C15 C 0.8827(6) 0.4302(7) 0.5844(4) 0.0278(12) Uani 1 1 d . . . . . H15 H 0.980284 0.464571 0.604498 0.033 Uiso 1 1 calc R U . . . C8 C 0.4025(5) 0.3701(6) 0.5578(4) 0.0202(11) Uani 1 1 d . . . . . H8 H 0.305146 0.338570 0.540459 0.024 Uiso 1 1 calc R U . . . C4 C 0.6819(5) 0.7774(6) 0.7969(4) 0.0245(12) Uani 1 1 d . . . . . H4A H 0.746059 0.869244 0.851831 0.029 Uiso 1 1 calc R U . . . C14 C 0.8012(6) 0.2949(7) 0.5015(4) 0.0306(13) Uani 1 1 d . . . . . H14 H 0.843055 0.238889 0.465112 0.037 Uiso 1 1 calc R U . . . C17 C 0.1431(5) -0.0895(6) 0.3551(4) 0.0224(11) Uani 1 1 d . . . . . C22 C 0.1673(6) -0.1420(7) 0.2571(4) 0.0257(12) Uani 1 1 d . . . . . C13 C 0.6600(6) 0.2423(7) 0.4723(4) 0.0290(13) Uani 1 1 d . . . . . H13 H 0.603075 0.149649 0.415673 0.035 Uiso 1 1 calc R U . . . C5 C 0.5416(5) 0.7411(6) 0.7767(4) 0.0244(12) Uani 1 1 d . . . . . H5 H 0.511180 0.806483 0.817687 0.029 Uiso 1 1 calc R U . . . C19 C -0.0837(6) -0.3121(7) 0.2987(5) 0.0328(14) Uani 1 1 d . . . . . H19 H -0.169811 -0.369782 0.313319 0.039 Uiso 1 1 calc R U . . . C32 C 0.6426(6) 0.0654(7) 0.0033(4) 0.0356(14) Uani 1 1 d . . . . . H32 H 0.740722 0.110609 0.005717 0.043 Uiso 1 1 calc R U . . . C21 C 0.0661(6) -0.2787(6) 0.1817(4) 0.0286(12) Uani 1 1 d . . . . . H21 H 0.084180 -0.313250 0.115999 0.034 Uiso 1 1 calc R U . . . C18 C 0.0150(6) -0.1795(7) 0.3729(4) 0.0308(13) Uani 1 1 d . . . . . H18 H -0.003437 -0.147031 0.438693 0.037 Uiso 1 1 calc R U . . . C16 C 0.2435(5) 0.0518(6) 0.4352(4) 0.0221(11) Uani 1 1 d . . . . . H16 H 0.219417 0.083541 0.498851 0.027 Uiso 1 1 calc R U . . . C20 C -0.0603(6) -0.3650(7) 0.2008(5) 0.0306(13) Uani 1 1 d . . . . . C30 C 0.4399(7) -0.1062(7) 0.0394(4) 0.0341(14) Uani 1 1 d . . . . . H30 H 0.398419 -0.178998 0.066594 0.041 Uiso 1 1 calc R U . . . C31 C 0.5828(7) -0.0414(7) 0.0429(4) 0.0357(14) Uani 1 1 d . . . . . H31 H 0.639542 -0.069791 0.071991 0.043 Uiso 1 1 calc R U . . . C23 C -0.1703(6) -0.5105(7) 0.1175(5) 0.0391(15) Uani 1 1 d . . . . . H23A H -0.131393 -0.577979 0.093377 0.059 Uiso 1 1 calc R U . . . H23B H -0.198528 -0.491888 0.060673 0.059 Uiso 1 1 calc R U . . . H23C H -0.252525 -0.556394 0.144243 0.059 Uiso 1 1 calc R U . . . C24A C 0.3196(10) 0.2021(19) 0.7770(12) 0.044(4) Uani 0.67(3) 1 d G . P A 1 H24A H 0.222363 0.162168 0.777161 0.053 Uiso 0.67(3) 1 calc R U P A 1 C29A C 0.4170(17) 0.3419(19) 0.8508(13) 0.057(4) Uani 0.67(3) 1 d G . P A 1 H29A H 0.386358 0.397504 0.901528 0.069 Uiso 0.67(3) 1 calc R U P A 1 C28A C 0.5593(15) 0.4004(18) 0.8505(17) 0.050(2) Uani 0.67(3) 1 d G . P A 1 H28A H 0.625900 0.495905 0.901035 0.060 Uiso 0.67(3) 1 calc R U P A 1 C27A C 0.6042(10) 0.319(2) 0.7764(17) 0.046(3) Uani 0.67(3) 1 d G . P A 1 H27A H 0.701449 0.358972 0.776173 0.055 Uiso 0.67(3) 1 calc R U P A 1 C26A C 0.5068(14) 0.1792(17) 0.7025(12) 0.043(3) Uani 0.67(3) 1 d G . P A 1 H26A H 0.537457 0.123636 0.651805 0.052 Uiso 0.67(3) 1 calc R U P A 1 C25A C 0.3645(12) 0.1208(13) 0.7028(11) 0.041(3) Uani 0.67(3) 1 d G . P A 1 H25A H 0.297914 0.025232 0.652297 0.049 Uiso 0.67(3) 1 calc R U P A 1 C28B C 0.597(2) 0.317(5) 0.789(4) 0.046(3) Uani 0.33(3) 1 d G . P A -1 H28B H 0.689446 0.335238 0.782512 0.055 Uiso 0.33(3) 1 calc R U P A -1 C25B C 0.481(3) 0.182(4) 0.726(3) 0.043(3) Uani 0.33(3) 1 d G . P A -1 H25B H 0.493770 0.107137 0.675927 0.052 Uiso 0.33(3) 1 calc R U P A -1 C24B C 0.346(2) 0.156(3) 0.735(2) 0.041(3) Uani 0.33(3) 1 d G . P A -1 H24B H 0.266615 0.063015 0.692207 0.049 Uiso 0.33(3) 1 calc R U P A -1 C29B C 0.327(3) 0.265(3) 0.808(2) 0.044(4) Uani 0.33(3) 1 d G . P A -1 H29B H 0.235132 0.246994 0.815072 0.053 Uiso 0.33(3) 1 calc R U P A -1 C27B C 0.444(4) 0.400(3) 0.872(3) 0.057(4) Uani 0.33(3) 1 d G . P A -1 H27B H 0.430806 0.475096 0.921658 0.069 Uiso 0.33(3) 1 calc R U P A -1 C26B C 0.579(3) 0.427(4) 0.862(4) 0.050(2) Uani 0.33(3) 1 d G . P A -1 H26B H 0.657964 0.519221 0.905379 0.060 Uiso 0.33(3) 1 calc R U P A -1 H4 H 0.339(9) 0.017(10) 0.289(6) 0.07(3) Uiso 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 Re01 0.01706(10) 0.02383(12) 0.01711(10) 0.00471(8) 0.00265(7) 0.01136(8) Cl02 0.0241(6) 0.0374(8) 0.0251(6) 0.0150(6) 0.0080(5) 0.0187(6) O2 0.037(2) 0.022(2) 0.037(2) 0.000(2) 0.0099(19) 0.0094(19) N2 0.017(2) 0.022(2) 0.017(2) 0.0054(18) 0.0044(16) 0.0091(18) O3 0.024(2) 0.045(3) 0.029(2) 0.0048(19) 0.0042(17) 0.022(2) O1 0.044(3) 0.044(3) 0.029(2) 0.018(2) 0.0056(19) 0.020(2) N1 0.019(2) 0.020(2) 0.019(2) 0.0006(18) 0.0019(17) 0.0108(18) C1 0.023(3) 0.033(3) 0.031(3) 0.017(3) 0.012(2) 0.015(3) O4 0.029(2) 0.034(3) 0.028(2) 0.002(2) 0.0103(18) 0.0039(19) C11 0.017(2) 0.022(3) 0.015(2) 0.007(2) 0.0031(18) 0.011(2) N3 0.019(2) 0.027(3) 0.019(2) 0.0050(19) -0.0001(17) 0.0107(19) C9 0.017(2) 0.019(3) 0.015(2) 0.004(2) 0.0033(18) 0.009(2) C2 0.021(3) 0.025(3) 0.031(3) 0.006(3) 0.001(2) 0.010(2) C12 0.021(2) 0.028(3) 0.020(3) 0.009(2) 0.004(2) 0.014(2) C3 0.034(3) 0.029(3) 0.013(2) 0.000(2) 0.000(2) 0.019(3) C6 0.017(2) 0.029(3) 0.026(3) 0.012(2) 0.008(2) 0.013(2) C10 0.019(2) 0.023(3) 0.018(2) 0.005(2) 0.0011(19) 0.007(2) C7 0.017(2) 0.019(3) 0.019(2) 0.005(2) 0.0046(19) 0.007(2) C15 0.021(3) 0.032(3) 0.028(3) 0.005(2) 0.002(2) 0.016(2) C8 0.015(2) 0.027(3) 0.021(3) 0.012(2) 0.0048(19) 0.012(2) C4 0.021(3) 0.027(3) 0.024(3) 0.008(2) 0.004(2) 0.013(2) C14 0.028(3) 0.034(3) 0.028(3) 0.004(3) 0.007(2) 0.021(3) C17 0.026(3) 0.023(3) 0.023(3) 0.011(2) 0.003(2) 0.014(2) C22 0.026(3) 0.028(3) 0.024(3) 0.012(2) 0.005(2) 0.013(2) C13 0.024(3) 0.032(3) 0.026(3) 0.006(2) 0.005(2) 0.015(2) C5 0.021(3) 0.026(3) 0.025(3) 0.005(2) 0.008(2) 0.014(2) C19 0.026(3) 0.024(3) 0.038(3) 0.010(3) 0.010(3) 0.005(2) C32 0.027(3) 0.034(4) 0.028(3) 0.005(3) 0.003(2) 0.007(3) C21 0.031(3) 0.026(3) 0.019(3) 0.004(2) 0.003(2) 0.011(2) C18 0.031(3) 0.030(3) 0.029(3) 0.014(3) 0.010(2) 0.011(3) C16 0.028(3) 0.021(3) 0.021(3) 0.008(2) 0.005(2) 0.015(2) C20 0.030(3) 0.021(3) 0.035(3) 0.009(3) -0.002(2) 0.010(2) C30 0.049(4) 0.025(3) 0.023(3) 0.011(2) 0.006(3) 0.013(3) C31 0.047(4) 0.031(4) 0.022(3) 0.002(3) -0.002(3) 0.020(3) C23 0.035(3) 0.031(4) 0.037(3) 0.005(3) -0.003(3) 0.013(3) C24A 0.043(5) 0.041(10) 0.064(10) 0.035(9) 0.015(6) 0.024(7) C29A 0.071(10) 0.067(13) 0.060(9) 0.040(10) 0.026(9) 0.042(11) C28A 0.052(6) 0.058(8) 0.045(6) 0.029(6) 0.007(5) 0.026(5) C27A 0.046(4) 0.047(5) 0.054(7) 0.036(5) 0.011(4) 0.018(4) C26A 0.051(7) 0.041(5) 0.043(8) 0.031(5) 0.016(5) 0.017(5) C25A 0.050(6) 0.030(7) 0.046(9) 0.020(6) 0.003(5) 0.018(5) C28B 0.046(4) 0.047(5) 0.054(7) 0.036(5) 0.011(4) 0.018(4) C25B 0.051(7) 0.041(5) 0.043(8) 0.031(5) 0.016(5) 0.017(5) C24B 0.050(6) 0.030(7) 0.046(9) 0.020(6) 0.003(5) 0.018(5) C29B 0.043(5) 0.041(10) 0.064(10) 0.035(9) 0.015(6) 0.024(7) C27B 0.071(10) 0.067(13) 0.060(9) 0.040(10) 0.026(9) 0.042(11) C26B 0.052(6) 0.058(8) 0.045(6) 0.029(6) 0.007(5) 0.026(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' 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' 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 C3 Re01 C2 90.4(2) . . ? C3 Re01 C1 90.3(2) . . ? C2 Re01 C1 88.8(2) . . ? C3 Re01 N2 171.09(19) . . ? C2 Re01 N2 92.46(19) . . ? C1 Re01 N2 98.15(19) . . ? C3 Re01 N1 95.54(19) . . ? C2 Re01 N1 95.5(2) . . ? C1 Re01 N1 172.7(2) . . ? N2 Re01 N1 75.80(15) . . ? C3 Re01 Cl02 91.67(17) . . ? C2 Re01 Cl02 177.11(16) . . ? C1 Re01 Cl02 93.15(17) . . ? N2 Re01 Cl02 85.17(12) . . ? N1 Re01 Cl02 82.32(12) . . ? C4 N2 C9 118.0(4) . . ? C4 N2 Re01 127.8(4) . . ? C9 N2 Re01 114.2(3) . . ? C15 N1 C11 118.6(4) . . ? C15 N1 Re01 126.2(4) . . ? C11 N1 Re01 115.0(3) . . ? O2 C1 Re01 178.4(5) . . ? C22 O4 H4 106(5) . . ? N1 C11 C12 122.4(4) . . ? N1 C11 C9 116.7(4) . . ? C12 C11 C9 121.0(4) . . ? C16 N3 C10 118.6(4) . . ? N2 C9 C7 122.8(4) . . ? N2 C9 C11 118.2(4) . . ? C7 C9 C11 119.0(4) . . ? O1 C2 Re01 178.4(6) . . ? C11 C12 C13 117.6(5) . . ? C11 C12 C10 118.9(5) . . ? C13 C12 C10 123.5(5) . . ? O3 C3 Re01 175.4(5) . . ? C5 C6 C7 119.6(5) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C8 C10 N3 123.3(5) . . ? C8 C10 C12 120.1(5) . . ? N3 C10 C12 116.6(4) . . ? C9 C7 C6 116.9(5) . . ? C9 C7 C8 119.3(4) . . ? C6 C7 C8 123.8(5) . . ? N1 C15 C14 122.4(5) . . ? N1 C15 H15 118.8 . . ? C14 C15 H15 118.8 . . ? C10 C8 C7 121.6(5) . . ? C10 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? N2 C4 C5 123.3(5) . . ? N2 C4 H4A 118.3 . . ? C5 C4 H4A 118.3 . . ? C13 C14 C15 119.7(5) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C18 C17 C22 117.4(5) . . ? C18 C17 C16 120.1(5) . . ? C22 C17 C16 122.4(5) . . ? O4 C22 C21 118.3(5) . . ? O4 C22 C17 121.4(5) . . ? C21 C22 C17 120.3(5) . . ? C14 C13 C12 119.3(5) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C6 C5 C4 119.3(5) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? C18 C19 C20 121.0(5) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C30 C32 C31 120.3(6) 2_655 . ? C30 C32 H32 119.9 2_655 . ? C31 C32 H32 119.9 . . ? C20 C21 C22 121.2(5) . . ? C20 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? C19 C18 C17 121.9(5) . . ? C19 C18 H18 119.1 . . ? C17 C18 H18 119.1 . . ? N3 C16 C17 122.8(5) . . ? N3 C16 H16 118.6 . . ? C17 C16 H16 118.6 . . ? C21 C20 C19 118.2(5) . . ? C21 C20 C23 120.5(5) . . ? C19 C20 C23 121.3(5) . . ? C32 C30 C31 120.2(6) 2_655 . ? C32 C30 H30 119.9 2_655 . ? C31 C30 H30 119.9 . . ? C30 C31 C32 119.5(6) . . ? C30 C31 H31 120.3 . . ? C32 C31 H31 120.3 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C29B C24A C24B 151(5) . . ? C29B C24A C29A 36(3) . . ? C24B C24A C29A 119(2) . . ? C29B C24A C25A 151(3) . . ? C24B C24A C25A 1(2) . . ? C29A C24A C25A 120.0 . . ? C29B C24A C27B 32.0(18) . . ? C24B C24A C27B 122(3) . . ? C29A C24A C27B 6(2) . . ? C25A C24A C27B 122.2(15) . . ? C29B C24A C25B 122(3) . . ? C24B C24A C25B 31.5(14) . . ? C29A C24A C25B 88.2(13) . . ? C25A C24A C25B 32.1(13) . . ? C27B C24A C25B 91.0(12) . . ? C29B C24A H24A 86.4 . . ? C24B C24A H24A 120.5 . . ? C29A C24A H24A 120.0 . . ? C25A C24A H24A 120.0 . . ? C27B C24A H24A 117.5 . . ? C25B C24A H24A 151.5 . . ? C27B C29A C29B 139(9) . . ? C27B C29A C28A 70(6) . . ? C29B C29A C28A 140.8(16) . . ? C27B C29A C24A 159(8) . . ? C29B C29A C24A 23.5(13) . . ? C28A C29A C24A 120.0 . . ? C27B C29A C26B 63(4) . . ? C29B C29A C26B 148(3) . . ? C28A C29A C26B 8(2) . . ? C24A C29A C26B 127.6(19) . . ? C27B C29A C24B 158(7) . . ? C29B C29A C24B 43.8(10) . . ? C28A C29A C24B 98.8(9) . . ? C24A C29A C24B 21.2(9) . . ? C26B C29A C24B 106.5(18) . . ? C27B C29A H29A 53.4 . . ? C29B C29A H29A 98.1 . . ? C28A C29A H29A 120.0 . . ? C24A C29A H29A 120.0 . . ? C26B C29A H29A 112.3 . . ? C24B C29A H29A 141.2 . . ? C28B C28A C27B 140(2) . . ? C28B C28A C27A 7(4) . . ? C27B C28A C27A 140.5(13) . . ? C28B C28A C29A 118.0(15) . . ? C27B C28A C29A 22.3(11) . . ? C27A C28A C29A 120.0 . . ? C28B C28A H28A 121.6 . . ? C27B C28A H28A 98.9 . . ? C27A C28A H28A 120.0 . . ? C29A C28A H28A 120.0 . . ? C28A C27A C26A 120.0 . . ? C28A C27A C25B 102.7(10) . . ? C26A C27A C25B 18.4(12) . . ? C28A C27A C26B 8.8(12) . . ? C26A C27A C26B 128.7(13) . . ? C25B C27A C26B 111(2) . . ? C28A C27A H27A 120.0 . . ? C26A C27A H27A 120.0 . . ? C25B C27A H27A 136.8 . . ? C26B C27A H27A 111.3 . . ? C25A C26A C27A 120.0 . . ? C25A C26A C28B 114.2(14) . . ? C27A C26A C28B 8(3) . . ? C25A C26A C24B 17.2(7) . . ? C27A C26A C24B 102.8(7) . . ? C28B C26A C24B 97.0(17) . . ? C25A C26A H26A 120.0 . . ? C27A C26A H26A 120.0 . . ? C28B C26A H26A 125.5 . . ? C24B C26A H26A 137.2 . . ? C24B C25A C25B 105(4) . . ? C24B C25A C26A 119(3) . . ? C25B C25A C26A 16.0(19) . . ? C24B C25A C24A 1(3) . . ? C25B C25A C24A 106.1(18) . . ? C26A C25A C24A 120.0 . . ? C24B C25A C29B 9(3) . . ? C25B C25A C29B 98.7(16) . . ? C26A C25A C29B 111.9(10) . . ? C24A C25A C29B 9.2(10) . . ? C24B C25A H25A 120.6 . . ? C25B C25A H25A 133.2 . . ? C26A C25A H25A 120.0 . . ? C24A C25A H25A 120.0 . . ? C29B C25A H25A 127.9 . . ? C28A C28B C25B 110.6(13) . . ? C28A C28B C26B 9.4(12) . . ? C25B C28B C26B 120.0 . . ? C28A C28B C26A 126(3) . . ? C25B C28B C26A 18.0(11) . . ? C26B C28B C26A 135.3(13) . . ? C28A C28B H28B 129.3 . . ? C25B C28B H28B 120.0 . . ? C26B C28B H28B 120.0 . . ? C26A C28B H28B 103.9 . . ? C25A C25B C24B 24.5(10) . . ? C25A C25B C28B 143.8(11) . . ? C24B C25B C28B 120.0 . . ? C25A C25B C27A 147(3) . . ? C24B C25B C27A 125(2) . . ? C28B C25B C27A 8(3) . . ? C25A C25B C24A 41.8(9) . . ? C24B C25B C24A 17.3(7) . . ? C28B C25B C24A 102.8(7) . . ? C27A C25B C24A 108(2) . . ? C25A C25B H25B 95.9 . . ? C24B C25B H25B 120.0 . . ? C28B C25B H25B 120.0 . . ? C27A C25B H25B 114.6 . . ? C24A C25B H25B 137.1 . . ? C25A C24B C24A 177(6) . . ? C25A C24B C25B 50(4) . . ? C24A C24B C25B 131(2) . . ? C25A C24B C29B 167(4) . . ? C24A C24B C29B 13(2) . . ? C25B C24B C29B 120.0 . . ? C25A C24B C26A 43(2) . . ? C24A C24B C26A 138(3) . . ? C25B C24B C26A 9.1(18) . . ? C29B C24B C26A 125.6(17) . . ? C25A C24B C29A 142(4) . . ? C24A C24B C29A 39.3(14) . . ? C25B C24B C29A 92.1(13) . . ? C29B C24B C29A 28.2(14) . . ? C26A C24B C29A 98.4(13) . . ? C25A C24B H24B 70.5 . . ? C24A C24B H24B 108.4 . . ? C25B C24B H24B 120.0 . . ? C29B C24B H24B 120.0 . . ? C26A C24B H24B 114.0 . . ? C29A C24B H24B 147.7 . . ? C24A C29B C29A 120(4) . . ? C24A C29B C27B 134(2) . . ? C29A C29B C27B 15(3) . . ? C24A C29B C24B 16(3) . . ? C29A C29B C24B 108(2) . . ? C27B C29B C24B 120.0 . . ? C24A C29B C25A 20(2) . . ? C29A C29B C25A 105(2) . . ? C27B C29B C25A 116.9(11) . . ? C24B C29B C25A 4.0(12) . . ? C24A C29B H29B 105.6 . . ? C29A C29B H29B 131.3 . . ? C27B C29B H29B 120.0 . . ? C24B C29B H29B 120.0 . . ? C25A C29B H29B 123.0 . . ? C29A C27B C28A 87(6) . . ? C29A C27B C29B 27(6) . . ? C28A C27B C29B 109.8(15) . . ? C29A C27B C26B 98(5) . . ? C28A C27B C26B 10.2(15) . . ? C29B C27B C26B 120.0 . . ? C29A C27B C24A 15(6) . . ? C28A C27B C24A 95.8(16) . . ? C29B C27B C24A 14.2(7) . . ? C26B C27B C24A 106.0(7) . . ? C29A C27B H27B 139.6 . . ? C28A C27B H27B 130.2 . . ? C29B C27B H27B 120.0 . . ? C26B C27B H27B 120.0 . . ? C24A C27B H27B 133.9 . . ? C27B C26B C28B 120.00(6) . . ? C27B C26B C27A 122.0(14) . . ? C28B C26B C27A 6(3) . . ? C27B C26B C29A 19.7(11) . . ? C28B C26B C29A 100.9(9) . . ? C27A C26B C29A 103.6(18) . . ? C27B C26B H26B 120.0 . . ? C28B C26B H26B 120.0 . . ? C27A C26B H26B 117.6 . . ? C29A C26B H26B 138.8 . . ? 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 Re01 C3 1.915(6) . ? Re01 C2 1.917(6) . ? Re01 C1 1.934(6) . ? Re01 N2 2.183(4) . ? Re01 N1 2.186(4) . ? Re01 Cl02 2.4752(14) . ? O2 C1 1.140(7) . ? N2 C4 1.323(7) . ? N2 C9 1.365(6) . ? O3 C3 1.149(6) . ? O1 C2 1.141(7) . ? N1 C15 1.325(7) . ? N1 C11 1.364(6) . ? O4 C22 1.351(7) . ? O4 H4 0.87(9) . ? C11 C12 1.390(7) . ? C11 C9 1.428(7) . ? N3 C16 1.285(7) . ? N3 C10 1.419(7) . ? C9 C7 1.408(7) . ? C12 C13 1.409(7) . ? C12 C10 1.443(7) . ? C6 C5 1.372(7) . ? C6 C7 1.410(7) . ? C6 H6 0.9500 . ? C10 C8 1.356(7) . ? C7 C8 1.425(7) . ? C15 C14 1.386(8) . ? C15 H15 0.9500 . ? C8 H8 0.9500 . ? C4 C5 1.389(7) . ? C4 H4A 0.9500 . ? C14 C13 1.368(7) . ? C14 H14 0.9500 . ? C17 C18 1.400(8) . ? C17 C22 1.406(7) . ? C17 C16 1.439(7) . ? C22 C21 1.393(8) . ? C13 H13 0.9500 . ? C5 H5 0.9500 . ? C19 C18 1.358(8) . ? C19 C20 1.401(8) . ? C19 H19 0.9500 . ? C32 C30 1.381(9) 2_655 ? C32 C31 1.390(9) . ? C32 H32 0.9500 . ? C21 C20 1.382(8) . ? C21 H21 0.9500 . ? C18 H18 0.9500 . ? C16 H16 0.9500 . ? C20 C23 1.506(8) . ? C30 C31 1.385(9) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24A C29B 0.643(19) . ? C24A C24B 0.79(2) . ? C24A C29A 1.3900 . ? C24A C25A 1.3900 . ? C24A C27B 1.89(2) . ? C24A C25B 2.00(2) . ? C24A H24A 0.9500 . ? C29A C27B 0.53(2) . ? C29A C29B 0.95(4) . ? C29A C28A 1.3900 . ? C29A C26B 1.55(4) . ? C29A C24B 1.91(2) . ? C29A H29A 0.9500 . ? C28A C28B 1.26(6) . ? C28A C27B 1.31(5) . ? C28A C27A 1.3900 . ? C28A H28A 0.9500 . ? C27A C26A 1.3900 . ? C27A C25B 1.40(4) . ? C27A C26B 1.51(6) . ? C27A H27A 0.9500 . ? C26A C25A 1.3900 . ? C26A C28B 1.44(5) . ? C26A C24B 1.76(3) . ? C26A H26A 0.9500 . ? C25A C24B 0.60(2) . ? C25A C25B 1.11(4) . ? C25A C29B 1.98(2) . ? C25A H25A 0.9500 . ? C28B C25B 1.3900 . ? C28B C26B 1.3900 . ? C28B H28B 0.9500 . ? C25B C24B 1.3900 . ? C25B H25B 0.9500 . ? C24B C29B 1.3900 . ? C24B H24B 0.9500 . ? C29B C27B 1.3900 . ? C29B H29B 0.9500 . ? C27B C26B 1.3900 . ? C27B H27B 0.9500 . ? C26B H26B 0.9500 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O4 H4 N3 0.87(9) 1.85(8) 2.646(6) 151(8) . yes 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 N1 C11 C12 1.5(8) . . . . ? Re01 N1 C11 C12 176.5(4) . . . . ? C15 N1 C11 C9 -178.5(5) . . . . ? Re01 N1 C11 C9 -3.4(6) . . . . ? C4 N2 C9 C7 -0.3(8) . . . . ? Re01 N2 C9 C7 -177.3(4) . . . . ? C4 N2 C9 C11 -179.1(5) . . . . ? Re01 N2 C9 C11 3.8(6) . . . . ? N1 C11 C9 N2 -0.3(7) . . . . ? C12 C11 C9 N2 179.7(5) . . . . ? N1 C11 C9 C7 -179.2(5) . . . . ? C12 C11 C9 C7 0.8(8) . . . . ? N1 C11 C12 C13 -2.3(8) . . . . ? C9 C11 C12 C13 177.7(5) . . . . ? N1 C11 C12 C10 177.0(5) . . . . ? C9 C11 C12 C10 -3.0(8) . . . . ? C16 N3 C10 C8 -41.9(8) . . . . ? C16 N3 C10 C12 139.5(5) . . . . ? C11 C12 C10 C8 3.8(8) . . . . ? C13 C12 C10 C8 -177.0(5) . . . . ? C11 C12 C10 N3 -177.6(5) . . . . ? C13 C12 C10 N3 1.7(8) . . . . ? N2 C9 C7 C6 1.6(8) . . . . ? C11 C9 C7 C6 -179.5(5) . . . . ? N2 C9 C7 C8 -178.1(5) . . . . ? C11 C9 C7 C8 0.7(7) . . . . ? C5 C6 C7 C9 -2.5(8) . . . . ? C5 C6 C7 C8 177.3(5) . . . . ? C11 N1 C15 C14 0.2(9) . . . . ? Re01 N1 C15 C14 -174.3(4) . . . . ? N3 C10 C8 C7 179.1(5) . . . . ? C12 C10 C8 C7 -2.3(8) . . . . ? C9 C7 C8 C10 0.1(8) . . . . ? C6 C7 C8 C10 -179.7(5) . . . . ? C9 N2 C4 C5 -0.2(8) . . . . ? Re01 N2 C4 C5 176.3(4) . . . . ? N1 C15 C14 C13 -1.0(10) . . . . ? C18 C17 C22 O4 179.0(5) . . . . ? C16 C17 C22 O4 -0.2(8) . . . . ? C18 C17 C22 C21 0.0(8) . . . . ? C16 C17 C22 C21 -179.2(5) . . . . ? C15 C14 C13 C12 0.1(9) . . . . ? C11 C12 C13 C14 1.4(8) . . . . ? C10 C12 C13 C14 -177.8(5) . . . . ? C7 C6 C5 C4 2.1(8) . . . . ? N2 C4 C5 C6 -0.7(9) . . . . ? O4 C22 C21 C20 -178.4(5) . . . . ? C17 C22 C21 C20 0.6(9) . . . . ? C20 C19 C18 C17 0.6(10) . . . . ? C22 C17 C18 C19 -0.6(9) . . . . ? C16 C17 C18 C19 178.6(6) . . . . ? C10 N3 C16 C17 175.0(5) . . . . ? C18 C17 C16 N3 177.8(5) . . . . ? C22 C17 C16 N3 -3.0(8) . . . . ? C22 C21 C20 C19 -0.7(9) . . . . ? C22 C21 C20 C23 178.3(6) . . . . ? C18 C19 C20 C21 0.1(9) . . . . ? C18 C19 C20 C23 -178.9(6) . . . . ? C32 C30 C31 C32 0.3(10) 2_655 . . . ? C30 C32 C31 C30 -0.3(10) 2_655 . . . ? C29B C24A C29A C27B -42(14) . . . . ? C24B C24A C29A C27B 116(15) . . . . ? C25A C24A C29A C27B 115(15) . . . . ? C25B C24A C29A C27B 119(15) . . . . ? C24B C24A C29A C29B 158(7) . . . . ? C25A C24A C29A C29B 156(6) . . . . ? C27B C24A C29A C29B 42(14) . . . . ? C25B C24A C29A C29B 161(6) . . . . ? C29B C24A C29A C28A -156(6) . . . . ? C24B C24A C29A C28A 1(3) . . . . ? C25A C24A C29A C28A 0.0 . . . . ? C27B C24A C29A C28A -115(15) . . . . ? C25B C24A C29A C28A 4.6(14) . . . . ? C29B C24A C29A C26B -155(8) . . . . ? C24B C24A C29A C26B 2(6) . . . . ? C25A C24A C29A C26B 1(5) . . . . ? C27B C24A C29A C26B -114(18) . . . . ? C25B C24A C29A C26B 6(4) . . . . ? C29B C24A C29A C24B -158(7) . . . . ? C25A C24A C29A C24B -1(3) . . . . ? C27B C24A C29A C24B -116(15) . . . . ? C25B C24A C29A C24B 3(3) . . . . ? C27B C29A C28A C28B -167(12) . . . . ? C29B C29A C28A C28B -22(6) . . . . ? C24A C29A C28A C28B -7(5) . . . . ? C26B C29A C28A C28B 179(100) . . . . ? C24B C29A C28A C28B -7(5) . . . . ? C29B C29A C28A C27B 145(11) . . . . ? C24A C29A C28A C27B 160(8) . . . . ? C26B C29A C28A C27B -13(21) . . . . ? C24B C29A C28A C27B 160(8) . . . . ? C27B C29A C28A C27A -160(8) . . . . ? C29B C29A C28A C27A -15(3) . . . . ? C24A C29A C28A C27A 0.0 . . . . ? C26B C29A C28A C27A -173(29) . . . . ? C24B C29A C28A C27A 0.4(10) . . . . ? C28B C28A C27A C26A 74(16) . . . . ? C27B C28A C27A C26A -12(5) . . . . ? C29A C28A C27A C26A 0.0 . . . . ? C28B C28A C27A C25B 67(15) . . . . ? C27B C28A C27A C25B -19(5) . . . . ? C29A C28A C27A C25B -7(2) . . . . ? C28B C28A C27A C26B -112(37) . . . . ? C27B C28A C27A C26B 162(30) . . . . ? C29A C28A C27A C26B 174(26) . . . . ? C28A C27A C26A C25A 0.0 . . . . ? C25B C27A C26A C25A 21(6) . . . . ? C26B C27A C26A C25A -1(5) . . . . ? C28A C27A C26A C28B -45(21) . . . . ? C25B C27A C26A C28B -23(17) . . . . ? C26B C27A C26A C28B -46(17) . . . . ? C28A C27A C26A C24B -0.5(11) . . . . ? C25B C27A C26A C24B 21(6) . . . . ? C26B C27A C26A C24B -2(5) . . . . ? C27A C26A C25A C24B -2(4) . . . . ? C28B C26A C25A C24B 5(6) . . . . ? C27A C26A C25A C25B -32(9) . . . . ? C28B C26A C25A C25B -25(7) . . . . ? C24B C26A C25A C25B -30(9) . . . . ? C27A C26A C25A C24A 0.0 . . . . ? C28B C26A C25A C24A 6(4) . . . . ? C24B C26A C25A C24A 2(4) . . . . ? C27A C26A C25A C29B 4.7(12) . . . . ? C28B C26A C25A C29B 11(4) . . . . ? C24B C26A C25A C29B 6(3) . . . . ? C29B C24A C25A C24B 92(100) . . . . ? C29A C24A C25A C24B 64(100) . . . . ? C27B C24A C25A C24B 70(100) . . . . ? C25B C24A C25A C24B 55(100) . . . . ? C29B C24A C25A C25B 37(8) . . . . ? C24B C24A C25A C25B -55(100) . . . . ? C29A C24A C25A C25B 9(3) . . . . ? C27B C24A C25A C25B 15(3) . . . . ? C29B C24A C25A C26A 29(7) . . . . ? C24B C24A C25A C26A -64(100) . . . . ? C29A C24A C25A C26A 0.0 . . . . ? C27B C24A C25A C26A 6(3) . . . . ? C25B C24A C25A C26A -9(3) . . . . ? C24B C24A C25A C29B -92(100) . . . . ? C29A C24A C25A C29B -29(7) . . . . ? C27B C24A C25A C29B -23(6) . . . . ? C25B C24A C25A C29B -37(8) . . . . ? C27B C28A C28B C25B -2(13) . . . . ? C27A C28A C28B C25B -104(19) . . . . ? C29A C28A C28B C25B 5(6) . . . . ? C27B C28A C28B C26B 173(37) . . . . ? C27A C28A C28B C26B 71(40) . . . . ? C29A C28A C28B C26B -179(100) . . . . ? C27B C28A C28B C26A 8(16) . . . . ? C27A C28A C28B C26A -94(21) . . . . ? C29A C28A C28B C26A 15(9) . . . . ? C25A C26A C28B C28A -15(9) . . . . ? C27A C26A C28B C28A 123(28) . . . . ? C24B C26A C28B C28A -13(8) . . . . ? C25A C26A C28B C25B 18(5) . . . . ? C27A C26A C28B C25B 156(17) . . . . ? C24B C26A C28B C25B 19(5) . . . . ? C25A C26A C28B C26B -18(5) . . . . ? C27A C26A C28B C26B 120(24) . . . . ? C24B C26A C28B C26B -17(5) . . . . ? C26A C25A C25B C24B 153(8) . . . . ? C24A C25A C25B C24B 1(3) . . . . ? C29B C25A C25B C24B 7(3) . . . . ? C24B C25A C25B C28B -17(8) . . . . ? C26A C25A C25B C28B 136(11) . . . . ? C24A C25A C25B C28B -15(5) . . . . ? C29B C25A C25B C28B -10(5) . . . . ? C24B C25A C25B C27A -30(10) . . . . ? C26A C25A C25B C27A 123(15) . . . . ? C24A C25A C25B C27A -29(8) . . . . ? C29B C25A C25B C27A -23(7) . . . . ? C24B C25A C25B C24A -1(3) . . . . ? C26A C25A C25B C24A 152(8) . . . . ? C29B C25A C25B C24A 5.6(12) . . . . ? C28A C28B C25B C25A 9(7) . . . . ? C26B C28B C25B C25A 8(4) . . . . ? C26A C28B C25B C25A -144(10) . . . . ? C28A C28B C25B C24B 1(4) . . . . ? C26B C28B C25B C24B 0.0 . . . . ? C26A C28B C25B C24B -152(8) . . . . ? C28A C28B C25B C27A 130(26) . . . . ? C26B C28B C25B C27A 129(22) . . . . ? C26A C28B C25B C27A -23(17) . . . . ? C28A C28B C25B C24A -2(5) . . . . ? C26B C28B C25B C24A -2.6(10) . . . . ? C26A C28B C25B C24A -154(8) . . . . ? C28A C27A C25B C25A 28(8) . . . . ? C26A C27A C25B C25A -133(13) . . . . ? C26B C27A C25B C25A 28(11) . . . . ? C28A C27A C25B C24B 14(4) . . . . ? C26A C27A C25B C24B -148(9) . . . . ? C26B C27A C25B C24B 14(8) . . . . ? C28A C27A C25B C28B -42(21) . . . . ? C26A C27A C25B C28B 157(17) . . . . ? C26B C27A C25B C28B -42(17) . . . . ? C28A C27A C25B C24A 9(3) . . . . ? C26A C27A C25B C24A -153(8) . . . . ? C26B C27A C25B C24A 9(6) . . . . ? C26A C25A C24B C25B -8(2) . . . . ? C24A C25A C24B C25B -125(100) . . . . ? C29B C25A C24B C25B -47(19) . . . . ? C25B C25A C24B C29B 47(19) . . . . ? C26A C25A C24B C29B 38(19) . . . . ? C24A C25A C24B C29B -79(100) . . . . ? C25B C25A C24B C26A 8(2) . . . . ? C24A C25A C24B C26A -117(100) . . . . ? C29B C25A C24B C26A -38(19) . . . . ? C25B C25A C24B C29A 11(8) . . . . ? C26A C25A C24B C29A 3(7) . . . . ? C24A C25A C24B C29A -114(100) . . . . ? C29B C25A C24B C29A -35(13) . . . . ? C29B C24A C24B C25B 34(12) . . . . ? C29A C24A C24B C25B 7(5) . . . . ? C25A C24A C24B C25B 124(100) . . . . ? C27B C24A C24B C25B 13(5) . . . . ? C29A C24A C24B C29B -27(9) . . . . ? C25A C24A C24B C29B 90(100) . . . . ? C27B C24A C24B C29B -21(8) . . . . ? C25B C24A C24B C29B -34(12) . . . . ? C29B C24A C24B C26A 25(13) . . . . ? C29A C24A C24B C26A -2(6) . . . . ? C25A C24A C24B C26A 115(100) . . . . ? C27B C24A C24B C26A 4(6) . . . . ? C25B C24A C24B C26A -9(3) . . . . ? C29B C24A C24B C29A 27(9) . . . . ? C25A C24A C24B C29A 117(100) . . . . ? C27B C24A C24B C29A 6(3) . . . . ? C25B C24A C24B C29A -7(5) . . . . ? C28B C25B C24B C25A 169(5) . . . . ? C27A C25B C24B C25A 161(7) . . . . ? C24A C25B C24B C25A 177(7) . . . . ? C25A C25B C24B C24A -177(7) . . . . ? C28B C25B C24B C24A -8(3) . . . . ? C27A C25B C24B C24A -16(6) . . . . ? C25A C25B C24B C29B -169(5) . . . . ? C28B C25B C24B C29B 0.0 . . . . ? C27A C25B C24B C29B -8(4) . . . . ? C24A C25B C24B C29B 8(3) . . . . ? C25A C25B C24B C26A -39(10) . . . . ? C28B C25B C24B C26A 130(11) . . . . ? C27A C25B C24B C26A 122(14) . . . . ? C24A C25B C24B C26A 138(12) . . . . ? C25A C25B C24B C29A -173(5) . . . . ? C28B C25B C24B C29A -4.2(17) . . . . ? C27A C25B C24B C29A -12(4) . . . . ? C24A C25B C24B C29A 4(3) . . . . ? C27A C26A C24B C25A 179(3) . . . . ? C28B C26A C24B C25A -176(5) . . . . ? C25A C26A C24B C24A -177(8) . . . . ? C27A C26A C24B C24A 2(5) . . . . ? C28B C26A C24B C24A 8(6) . . . . ? C25A C26A C24B C25B 136(12) . . . . ? C27A C26A C24B C25B -46(12) . . . . ? C28B C26A C24B C25B -40(9) . . . . ? C25A C26A C24B C29B -170(6) . . . . ? C27A C26A C24B C29B 9(3) . . . . ? C28B C26A C24B C29B 14(4) . . . . ? C25A C26A C24B C29A -178(5) . . . . ? C27A C26A C24B C29A 0.6(14) . . . . ? C28B C26A C24B C29A 6(4) . . . . ? C24B C24A C29B C29A -43(13) . . . . ? C25A C24A C29B C29A -45(11) . . . . ? C27B C24A C29B C29A -7(3) . . . . ? C25B C24A C29B C29A -23(7) . . . . ? C24B C24A C29B C27B -36(13) . . . . ? C29A C24A C29B C27B 7(3) . . . . ? C25A C24A C29B C27B -38(10) . . . . ? C25B C24A C29B C27B -15(6) . . . . ? C29A C24A C29B C24B 43(13) . . . . ? C25A C24A C29B C24B -2(5) . . . . ? C27B C24A C29B C24B 36(13) . . . . ? C25B C24A C29B C24B 20(7) . . . . ? C24B C24A C29B C25A 2(5) . . . . ? C29A C24A C29B C25A 45(11) . . . . ? C27B C24A C29B C25A 38(10) . . . . ? C25B C24A C29B C25A 22(5) . . . . ? C27B C29A C29B C24A 159(8) . . . . ? C28A C29A C29B C24A 33(8) . . . . ? C26B C29A C29B C24A 39(12) . . . . ? C24B C29A C29B C24A 12(4) . . . . ? C28A C29A C29B C27B -126(13) . . . . ? C24A C29A C29B C27B -159(8) . . . . ? C26B C29A C29B C27B -120(18) . . . . ? C24B C29A C29B C27B -147(10) . . . . ? C27B C29A C29B C24B 147(10) . . . . ? C28A C29A C29B C24B 22(5) . . . . ? C24A C29A C29B C24B -12(4) . . . . ? C26B C29A C29B C24B 27(10) . . . . ? C27B C29A C29B C25A 144(10) . . . . ? C28A C29A C29B C25A 19(4) . . . . ? C24A C29A C29B C25A -15(4) . . . . ? C26B C29A C29B C25A 24(10) . . . . ? C24B C29A C29B C25A -3.1(13) . . . . ? C25A C24B C29B C24A 169(23) . . . . ? C25B C24B C29B C24A -151(11) . . . . ? C26A C24B C29B C24A -160(11) . . . . ? C29A C24B C29B C24A -142(12) . . . . ? C25A C24B C29B C29A -49(18) . . . . ? C24A C24B C29B C29A 142(12) . . . . ? C25B C24B C29B C29A -9(3) . . . . ? C26A C24B C29B C29A -17(4) . . . . ? C25A C24B C29B C27B -40(17) . . . . ? C24A C24B C29B C27B 151(11) . . . . ? C25B C24B C29B C27B 0.0 . . . . ? C26A C24B C29B C27B -9(2) . . . . ? C29A C24B C29B C27B 9(3) . . . . ? C24A C24B C29B C25A -169(23) . . . . ? C25B C24B C29B C25A 40(17) . . . . ? C26A C24B C29B C25A 32(16) . . . . ? C29A C24B C29B C25A 49(18) . . . . ? C29B C29A C27B C28A -147(7) . . . . ? C24A C29A C27B C28A -123(13) . . . . ? C26B C29A C27B C28A 2(3) . . . . ? C24B C29A C27B C28A -63(20) . . . . ? C28A C29A C27B C29B 147(7) . . . . ? C24A C29A C27B C29B 24(8) . . . . ? C26B C29A C27B C29B 149(9) . . . . ? C24B C29A C27B C29B 84(23) . . . . ? C29B C29A C27B C26B -149(9) . . . . ? C28A C29A C27B C26B -2(3) . . . . ? C24A C29A C27B C26B -125(14) . . . . ? C24B C29A C27B C26B -65(19) . . . . ? C29B C29A C27B C24A -24(8) . . . . ? C28A C29A C27B C24A 123(13) . . . . ? C26B C29A C27B C24A 125(14) . . . . ? C24B C29A C27B C24A 60(21) . . . . ? C28B C28A C27B C29A 18(16) . . . . ? C27A C28A C27B C29A 28(12) . . . . ? C28B C28A C27B C29B 2(13) . . . . ? C27A C28A C27B C29B 13(7) . . . . ? C29A C28A C27B C29B -15(5) . . . . ? C28B C28A C27B C26B -174(33) . . . . ? C27A C28A C27B C26B -163(28) . . . . ? C29A C28A C27B C26B 169(18) . . . . ? C28B C28A C27B C24A 5(11) . . . . ? C27A C28A C27B C24A 15(6) . . . . ? C29A C28A C27B C24A -13(5) . . . . ? C24A C29B C27B C29A -25(10) . . . . ? C24B C29B C27B C29A -36(11) . . . . ? C25A C29B C27B C29A -39(11) . . . . ? C24A C29B C27B C28A 10(6) . . . . ? C29A C29B C27B C28A 35(8) . . . . ? C24B C29B C27B C28A -1(4) . . . . ? C25A C29B C27B C28A -4(5) . . . . ? C24A C29B C27B C26B 11(4) . . . . ? C29A C29B C27B C26B 36(11) . . . . ? C24B C29B C27B C26B 0.0 . . . . ? C25A C29B C27B C26B -2.9(14) . . . . ? C29A C29B C27B C24A 25(10) . . . . ? C24B C29B C27B C24A -11(4) . . . . ? C25A C29B C27B C24A -14(4) . . . . ? C29B C24A C27B C29A 132(16) . . . . ? C24B C24A C27B C29A -67(16) . . . . ? C25A C24A C27B C29A -68(16) . . . . ? C25B C24A C27B C29A -61(15) . . . . ? C29B C24A C27B C28A -171(6) . . . . ? C24B C24A C27B C28A -10(5) . . . . ? C29A C24A C27B C28A 57(14) . . . . ? C25A C24A C27B C28A -11(5) . . . . ? C25B C24A C27B C28A -4(4) . . . . ? C24B C24A C27B C29B 160(7) . . . . ? C29A C24A C27B C29B -132(16) . . . . ? C25A C24A C27B C29B 159(6) . . . . ? C25B C24A C27B C29B 167(5) . . . . ? C29B C24A C27B C26B -170(4) . . . . ? C24B C24A C27B C26B -10(4) . . . . ? C29A C24A C27B C26B 57(15) . . . . ? C25A C24A C27B C26B -11(2) . . . . ? C25B C24A C27B C26B -3.3(13) . . . . ? C29A C27B C26B C28B 16(6) . . . . ? C28A C27B C26B C28B 4(23) . . . . ? C29B C27B C26B C28B 0.0 . . . . ? C24A C27B C26B C28B 2.7(11) . . . . ? C29A C27B C26B C27A 23(5) . . . . ? C28A C27B C26B C27A 11(19) . . . . ? C29B C27B C26B C27A 7(4) . . . . ? C24A C27B C26B C27A 10(4) . . . . ? C28A C27B C26B C29A -11(18) . . . . ? C29B C27B C26B C29A -16(6) . . . . ? C24A C27B C26B C29A -13(6) . . . . ? C28A C28B C26B C27B -5(26) . . . . ? C25B C28B C26B C27B 0.0 . . . . ? C26A C28B C26B C27B 12(3) . . . . ? C28A C28B C26B C27A -115(41) . . . . ? C25B C28B C26B C27A -110(17) . . . . ? C26A C28B C26B C27A -98(19) . . . . ? C28A C28B C26B C29A 0(24) . . . . ? C25B C28B C26B C29A 5(2) . . . . ? C26A C28B C26B C29A 17(4) . . . . ? C28A C27A C26B C27B -13(21) . . . . ? C26A C27A C26B C27B -6(7) . . . . ? C25B C27A C26B C27B -13(8) . . . . ? C28A C27A C26B C28B 61(38) . . . . ? C26A C27A C26B C28B 68(14) . . . . ? C25B C27A C26B C28B 60(13) . . . . ? C28A C27A C26B C29A -5(21) . . . . ? C26A C27A C26B C29A 2(8) . . . . ? C25B C27A C26B C29A -6(8) . . . . ? C29B C29A C26B C27B 140(15) . . . . ? C28A C29A C26B C27B 166(23) . . . . ? C24A C29A C26B C27B 158(10) . . . . ? C24B C29A C26B C27B 159(8) . . . . ? C27B C29A C26B C28B -166(5) . . . . ? C29B C29A C26B C28B -26(10) . . . . ? C28A C29A C26B C28B -1(27) . . . . ? C24A C29A C26B C28B -8(5) . . . . ? C24B C29A C26B C28B -7(3) . . . . ? C27B C29A C26B C27A -160(4) . . . . ? C29B C29A C26B C27A -20(12) . . . . ? C28A C29A C26B C27A 5(23) . . . . ? C24A C29A C26B C27A -2(8) . . . . ? C24B C29A C26B C27A -1(6) . . . . ?