# Electronic Supplementary Material (ESI) for Dalton Transactions. # This journal is © The Royal Society of Chemistry 2023 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_db39b_reprocess_twin1_hklf4 _database_code_depnum_ccdc_archive 'CCDC 2285019' loop_ _audit_author_name _audit_author_address 'Marina Uzelac' ;University of Edinburgh United Kingdom ; _audit_update_record ; 2023-07-27 deposited with the CCDC. 2023-11-13 downloaded from the CCDC. ; _audit_creation_date 2022-06-17 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C35 H47 N3 O Zn' _chemical_formula_sum 'C35 H47 N3 O Zn' _chemical_formula_weight 591.12 _chemical_melting_point ? _chemical_oxdiff_formula 'Zn1 N3 O1 C35 H47' _chemical_oxdiff_usercomment '120 K' 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' 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3962(3) _cell_length_b 16.5432(4) _cell_length_c 17.1649(4) _cell_angle_alpha 78.352(2) _cell_angle_beta 83.508(2) _cell_angle_gamma 70.096(2) _cell_volume 3237.86(14) _cell_formula_units_Z 4 _cell_measurement_reflns_used 16680 _cell_measurement_temperature 120.0(5) _cell_measurement_theta_max 25.2800 _cell_measurement_theta_min 3.9140 _shelx_estimated_absorpt_T_max 0.945 _shelx_estimated_absorpt_T_min 0.730 _exptl_absorpt_coefficient_mu 0.789 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.79920 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.213 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 1264 _exptl_crystal_recrystallization_method 'Crystallised from hexanes by cooling to -27 C.' _exptl_crystal_size_max 0.425 _exptl_crystal_size_mid 0.216 _exptl_crystal_size_min 0.073 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_av_unetI/netI 0.1119 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 19098 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.375 _diffrn_reflns_theta_min 3.272 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 120.0(5) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.0521 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -70.00 -2.00 1.00 20.00 -- -15.82 126.00 2.00 68 2 \w -81.00 -14.00 1.00 20.00 -- -15.82 145.00 170.00 67 3 \w 14.00 83.00 1.00 20.00 -- 17.54-145.00 117.00 69 4 \w 2.00 72.00 1.00 20.00 -- 17.54-126.00 -74.00 70 5 \w 39.00 90.00 1.00 20.00 -- 17.54 178.00 60.00 51 6 \w -9.00 39.00 1.00 20.00 -- 17.54 77.00 150.00 48 7 \w -12.00 89.00 1.00 20.00 -- 17.54 19.00 -60.00 101 8 \w -9.00 39.00 1.00 20.00 -- 17.54 77.00 0.00 48 9 \w -12.00 89.00 1.00 20.00 -- 17.54 19.00-150.00 101 10 \w 1.00 85.00 1.00 20.00 -- 17.54 57.00 90.00 84 11 \w -39.00 11.00 1.00 20.00 -- -15.82 -77.00 -30.00 50 12 \w -1.00 87.00 1.00 20.00 -- 17.54 38.00 -30.00 88 13 \w 1.00 85.00 1.00 20.00 -- 17.54 57.00 30.00 84 14 \w -9.00 39.00 1.00 20.00 -- 17.54 77.00-120.00 48 15 \w -20.00 56.00 1.00 20.00 -- 17.54 -99.00 0.00 76 16 \w -50.00 34.00 1.00 20.00 -- 17.54 -57.00-120.00 84 17 \w -20.00 56.00 1.00 20.00 -- 17.54 -99.00-150.00 76 18 \w -50.00 34.00 1.00 20.00 -- 17.54 -57.00 150.00 84 19 \w -20.00 22.00 1.00 20.00 -- 17.54 -99.00 30.00 42 20 \w -20.00 56.00 1.00 20.00 -- 17.54 -99.00 150.00 76 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0335975000 _diffrn_orient_matrix_UB_12 -0.0147033000 _diffrn_orient_matrix_UB_13 0.0340613000 _diffrn_orient_matrix_UB_21 0.0506952000 _diffrn_orient_matrix_UB_22 -0.0114476000 _diffrn_orient_matrix_UB_23 -0.0248064000 _diffrn_orient_matrix_UB_31 0.0036173000 _diffrn_orient_matrix_UB_32 0.0423994000 _diffrn_orient_matrix_UB_33 -0.0029560000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 11599 _reflns_number_total 19098 _reflns_special_details ; _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. Completness statistics refer to single and composite reflections containing twin component 1 only. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _refine_diff_density_max 0.626 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.081 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.915 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 744 _refine_ls_number_reflns 19098 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0960 _refine_ls_R_factor_gt 0.0503 _refine_ls_restrained_S_all 0.915 _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^)+(0.0459P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0934 _refine_ls_wR_factor_ref 0.1010 _refine_special_details ; Atoms C28 and C29 are suggested to be disordered over two positions. All attempts of modelling this disorder resulted in NPD atoms. Minor non-merohedral twinning was handled with CrysAlisPro and refined twin scale factor 0.1264(4). ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.8736 0.1264 2. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 3. Rigid bond restraints C27, C28, C29 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 C12, C13, C14 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 4. Uiso/Uaniso restraints and constraints C27 \\sim C28 \\sim C29: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A C12 \\sim C13 \\sim C14: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A 5.a Ternary CH refined with riding coordinates: C12(H12), C15(H15), C24(H24), C27(H27), C47(H47), C50(H50), C59(H59), C62(H62) 5.b Aromatic/amide H refined with riding coordinates: C2(H2), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C31(H31), C32(H32), C33(H33), C37(H37), C43(H43), C44(H44), C45(H45), C55(H55), C56(H56), C57(H57), C67(H67), C68(H68), C69(H69) 5.c Idealised Me refined as rotating group: C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B, H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C35(H35A,H35B,H35C), C39(H39A, H39B,H39C), C40(H40A,H40B,H40C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C60(H60A,H60B,H60C), C61(H61A,H61B, H61C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C70(H70A,H70B,H70C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 0.0574(3) 0.9702(2) 0.8104(2) 0.0190(8) Uani 1 1 d . . . . . C2 C 0.1159(3) 0.9315(2) 0.8809(2) 0.0238(9) Uani 1 1 d . . . . . H2 H 0.083557 0.958149 0.924698 0.029 Uiso 1 1 calc R U . . . C3 C 0.2149(4) 0.8593(2) 0.8956(2) 0.0236(9) Uani 1 1 d . . . . . C4 C -0.0594(3) 1.0390(2) 0.8170(2) 0.0265(9) Uani 1 1 d . . . . . H4A H -0.057477 1.093798 0.786087 0.040 Uiso 1 1 calc R U . . . H4B H -0.078438 1.045155 0.871801 0.040 Uiso 1 1 calc R U . . . H4C H -0.116205 1.021660 0.797465 0.040 Uiso 1 1 calc R U . . . C5 C 0.2426(4) 0.8241(3) 0.9823(2) 0.0404(12) Uani 1 1 d . . . . . H5A H 0.212082 0.777312 1.001984 0.061 Uiso 1 1 calc R U . . . H5B H 0.208861 0.869933 1.012932 0.061 Uiso 1 1 calc R U . . . H5C H 0.324384 0.802822 0.986815 0.061 Uiso 1 1 calc R U . . . C6 C 0.0222(3) 0.9865(2) 0.6739(2) 0.0211(9) Uani 1 1 d . . . . . C7 C -0.0446(3) 0.9391(2) 0.6567(2) 0.0238(9) Uani 1 1 d . . . . . C8 C -0.1181(3) 0.9778(3) 0.5946(2) 0.0295(10) Uani 1 1 d . . . . . H8 H -0.164989 0.948789 0.582921 0.035 Uiso 1 1 calc R U . . . C9 C -0.1235(3) 1.0580(3) 0.5496(2) 0.0316(10) Uani 1 1 d . . . . . H9 H -0.174229 1.082875 0.508721 0.038 Uiso 1 1 calc R U . . . C10 C -0.0531(3) 1.1010(2) 0.5658(2) 0.0279(10) Uani 1 1 d . . . . . H10 H -0.055282 1.154296 0.534285 0.034 Uiso 1 1 calc R U . . . C11 C 0.0206(3) 1.0668(2) 0.6279(2) 0.0224(9) Uani 1 1 d . . . . . C12 C -0.0350(3) 0.8483(2) 0.7029(2) 0.0303(10) Uani 1 1 d . U . . . H12 H 0.045611 0.819919 0.716175 0.036 Uiso 1 1 calc R U . . . C13 C -0.1051(5) 0.8490(3) 0.7812(3) 0.0677(16) Uani 1 1 d . U . . . H13A H -0.184421 0.880766 0.771425 0.101 Uiso 1 1 calc R U . . . H13B H -0.077863 0.876442 0.815353 0.101 Uiso 1 1 calc R U . . . H13C H -0.097343 0.790038 0.806377 0.101 Uiso 1 1 calc R U . . . C14 C -0.0634(5) 0.7904(3) 0.6563(3) 0.0647(16) Uani 1 1 d . U . . . H14A H -0.050905 0.733512 0.688194 0.097 Uiso 1 1 calc R U . . . H14B H -0.014901 0.785617 0.608593 0.097 Uiso 1 1 calc R U . . . H14C H -0.142344 0.815367 0.642644 0.097 Uiso 1 1 calc R U . . . C15 C 0.0992(3) 1.1147(2) 0.6435(2) 0.0292(10) Uani 1 1 d . . . . . H15 H 0.133861 1.085840 0.694676 0.035 Uiso 1 1 calc R U . . . C16 C 0.1964(3) 1.1078(2) 0.5791(2) 0.0386(11) Uani 1 1 d . . . . . H16A H 0.164910 1.138387 0.528679 0.058 Uiso 1 1 calc R U . . . H16B H 0.235675 1.047471 0.575843 0.058 Uiso 1 1 calc R U . . . H16C H 0.249443 1.133197 0.592299 0.058 Uiso 1 1 calc R U . . . C17 C 0.0373(4) 1.2112(2) 0.6482(2) 0.0374(11) Uani 1 1 d . . . . . H17A H 0.088509 1.234613 0.667043 0.056 Uiso 1 1 calc R U . . . H17B H -0.028865 1.216511 0.684201 0.056 Uiso 1 1 calc R U . . . H17C H 0.013643 1.242893 0.596256 0.056 Uiso 1 1 calc R U . . . C18 C 0.3675(3) 0.7359(2) 0.86282(19) 0.0205(9) Uani 1 1 d . . . . . C19 C 0.3356(3) 0.6598(2) 0.8842(2) 0.0204(9) Uani 1 1 d . . . . . C20 C 0.4205(3) 0.5809(2) 0.9060(2) 0.0253(9) Uani 1 1 d . . . . . H20 H 0.400658 0.530234 0.919503 0.030 Uiso 1 1 calc R U . . . C21 C 0.5331(3) 0.5751(2) 0.9081(2) 0.0270(9) Uani 1 1 d . . . . . H21 H 0.588092 0.521448 0.924968 0.032 Uiso 1 1 calc R U . . . C22 C 0.5644(3) 0.6490(2) 0.8852(2) 0.0270(9) Uani 1 1 d . . . . . H22 H 0.641185 0.644728 0.885404 0.032 Uiso 1 1 calc R U . . . C23 C 0.4825(3) 0.7302(2) 0.8619(2) 0.0253(9) Uani 1 1 d . . . . . C24 C 0.2131(3) 0.6626(2) 0.8788(2) 0.0243(9) Uani 1 1 d . . . . . H24 H 0.163968 0.723931 0.872199 0.029 Uiso 1 1 calc R U . . . C25 C 0.1692(4) 0.6131(3) 0.9548(2) 0.0388(11) Uani 1 1 d . . . . . H25A H 0.089504 0.621181 0.950696 0.058 Uiso 1 1 calc R U . . . H25B H 0.178271 0.635311 1.000295 0.058 Uiso 1 1 calc R U . . . H25C H 0.212610 0.552041 0.960590 0.058 Uiso 1 1 calc R U . . . C26 C 0.2013(3) 0.6262(2) 0.8064(2) 0.0319(10) Uani 1 1 d . . . . . H26A H 0.245425 0.565289 0.812787 0.048 Uiso 1 1 calc R U . . . H26B H 0.229011 0.657010 0.759235 0.048 Uiso 1 1 calc R U . . . H26C H 0.121952 0.633575 0.801539 0.048 Uiso 1 1 calc R U . . . C27 C 0.5212(4) 0.8099(3) 0.8363(3) 0.0536(14) Uani 1 1 d . U . . . H27 H 0.460158 0.854959 0.805169 0.064 Uiso 1 1 calc R U . . . C28 C 0.5353(6) 0.8473(3) 0.9074(4) 0.105(2) Uani 1 1 d . U . . . H28A H 0.464055 0.861907 0.938387 0.157 Uiso 1 1 calc R U . . . H28B H 0.556558 0.898770 0.888775 0.157 Uiso 1 1 calc R U . . . H28C H 0.594119 0.804608 0.939786 0.157 Uiso 1 1 calc R U . . . C29 C 0.6294(4) 0.7915(4) 0.7821(4) 0.109(2) Uani 1 1 d . U . . . H29A H 0.692849 0.750903 0.811817 0.163 Uiso 1 1 calc R U . . . H29B H 0.645379 0.844967 0.761732 0.163 Uiso 1 1 calc R U . . . H29C H 0.618439 0.767081 0.738656 0.163 Uiso 1 1 calc R U . . . C30 C 0.3468(3) 0.8094(2) 0.6068(2) 0.0239(9) Uani 1 1 d . . . . . C31 C 0.4073(4) 0.7831(2) 0.5364(2) 0.0313(10) Uani 1 1 d . . . . . H31 H 0.390150 0.743382 0.512669 0.038 Uiso 1 1 calc R U . . . C32 C 0.4911(4) 0.8171(3) 0.5042(2) 0.0373(11) Uani 1 1 d . . . . . H32 H 0.532025 0.800388 0.457957 0.045 Uiso 1 1 calc R U . . . C33 C 0.5164(4) 0.8766(3) 0.5397(2) 0.0358(11) Uani 1 1 d . . . . . H33 H 0.574779 0.898800 0.517812 0.043 Uiso 1 1 calc R U . . . C34 C 0.4552(3) 0.9022(2) 0.6067(2) 0.0270(9) Uani 1 1 d . . . . . C35 C 0.4752(4) 0.9682(3) 0.6469(2) 0.0391(11) Uani 1 1 d . . . . . H35A H 0.417641 1.023913 0.632267 0.059 Uiso 1 1 calc R U . . . H35B H 0.549836 0.972737 0.630454 0.059 Uiso 1 1 calc R U . . . H35C H 0.470862 0.950010 0.703584 0.059 Uiso 1 1 calc R U . . . N1 N 0.0962(2) 0.94852(17) 0.74008(16) 0.0190(7) Uani 1 1 d . . . . . N2 N 0.2809(3) 0.81847(18) 0.83902(16) 0.0191(7) Uani 1 1 d . . . . . N3 N 0.3719(3) 0.86898(18) 0.63970(16) 0.0212(7) Uani 1 1 d . . . . . O1 O 0.2664(2) 0.78216(15) 0.64598(14) 0.0253(6) Uani 1 1 d . . . . . Zn1 Zn 0.24605(4) 0.86083(3) 0.72752(2) 0.02033(12) Uani 1 1 d . . . . . C36 C 0.2515(3) 0.3519(2) 0.9023(2) 0.0174(8) Uani 1 1 d . . . . . C37 C 0.3558(3) 0.3653(2) 0.9051(2) 0.0175(8) Uani 1 1 d . . . . . H37 H 0.368171 0.378733 0.952681 0.021 Uiso 1 1 calc R U . . . C38 C 0.4454(3) 0.3615(2) 0.8462(2) 0.0167(8) Uani 1 1 d . . . . . C39 C 0.1827(3) 0.3449(2) 0.9807(2) 0.0249(9) Uani 1 1 d . . . . . H39A H 0.102598 0.374387 0.971869 0.037 Uiso 1 1 calc R U . . . H39B H 0.207192 0.371431 1.017172 0.037 Uiso 1 1 calc R U . . . H39C H 0.194819 0.284521 1.002584 0.037 Uiso 1 1 calc R U . . . C40 C 0.5565(3) 0.3658(2) 0.8713(2) 0.0223(9) Uani 1 1 d . . . . . H40A H 0.618884 0.315304 0.860466 0.033 Uiso 1 1 calc R U . . . H40B H 0.550480 0.367398 0.927256 0.033 Uiso 1 1 calc R U . . . H40C H 0.570420 0.417561 0.842028 0.033 Uiso 1 1 calc R U . . . C41 C 0.1134(3) 0.3122(2) 0.84480(19) 0.0192(8) Uani 1 1 d . . . . . C42 C 0.0063(3) 0.3711(2) 0.8230(2) 0.0194(8) Uani 1 1 d . . . . . C43 C -0.0852(3) 0.3394(3) 0.8270(2) 0.0260(9) Uani 1 1 d . . . . . H43 H -0.157055 0.377901 0.812040 0.031 Uiso 1 1 calc R U . . . C44 C -0.0713(3) 0.2523(3) 0.8526(2) 0.0306(10) Uani 1 1 d . . . . . H44 H -0.133299 0.232092 0.855271 0.037 Uiso 1 1 calc R U . . . C45 C 0.0350(4) 0.1953(3) 0.8742(2) 0.0313(10) Uani 1 1 d . . . . . H45 H 0.043562 0.136621 0.891783 0.038 Uiso 1 1 calc R U . . . C46 C 0.1299(3) 0.2221(2) 0.8709(2) 0.0257(9) Uani 1 1 d . . . . . C47 C -0.0135(3) 0.4678(2) 0.7958(2) 0.0253(9) Uani 1 1 d . . . . . H47 H 0.062008 0.475352 0.783219 0.030 Uiso 1 1 calc R U . . . C48 C -0.0724(4) 0.5198(3) 0.8612(2) 0.0485(13) Uani 1 1 d . . . . . H48A H -0.082243 0.580489 0.842300 0.073 Uiso 1 1 calc R U . . . H48B H -0.026069 0.499154 0.906852 0.073 Uiso 1 1 calc R U . . . H48C H -0.146135 0.512654 0.875648 0.073 Uiso 1 1 calc R U . . . C49 C -0.0815(4) 0.5053(3) 0.7211(3) 0.0483(13) Uani 1 1 d . . . . . H49A H -0.157668 0.501973 0.732387 0.072 Uiso 1 1 calc R U . . . H49B H -0.044101 0.472538 0.679784 0.072 Uiso 1 1 calc R U . . . H49C H -0.085839 0.565249 0.703838 0.072 Uiso 1 1 calc R U . . . C50 C 0.2470(3) 0.1555(2) 0.8906(2) 0.0300(10) Uani 1 1 d . . . . . H50 H 0.299162 0.187517 0.894266 0.036 Uiso 1 1 calc R U . . . C51 C 0.2953(4) 0.1019(2) 0.8242(2) 0.0384(11) Uani 1 1 d . . . . . H51A H 0.371989 0.063917 0.835659 0.058 Uiso 1 1 calc R U . . . H51B H 0.296686 0.140441 0.774460 0.058 Uiso 1 1 calc R U . . . H51C H 0.247752 0.067577 0.820940 0.058 Uiso 1 1 calc R U . . . C52 C 0.2447(4) 0.0949(3) 0.9705(2) 0.0448(12) Uani 1 1 d . . . . . H52A H 0.202017 0.057272 0.966460 0.067 Uiso 1 1 calc R U . . . H52B H 0.208701 0.129222 1.011015 0.067 Uiso 1 1 calc R U . . . H52C H 0.321812 0.060232 0.984168 0.067 Uiso 1 1 calc R U . . . C53 C 0.5392(3) 0.3395(2) 0.7198(2) 0.0198(9) Uani 1 1 d . . . . . C54 C 0.5693(3) 0.4105(2) 0.6750(2) 0.0261(9) Uani 1 1 d . . . . . C55 C 0.6643(3) 0.3940(3) 0.6231(2) 0.0355(11) Uani 1 1 d . . . . . H55 H 0.684725 0.440441 0.592858 0.043 Uiso 1 1 calc R U . . . C56 C 0.7298(3) 0.3095(3) 0.6155(2) 0.0395(11) Uani 1 1 d . . . . . H56 H 0.794544 0.299397 0.580885 0.047 Uiso 1 1 calc R U . . . C57 C 0.6995(4) 0.2405(3) 0.6588(2) 0.0359(11) Uani 1 1 d . . . . . H57 H 0.744355 0.183946 0.653025 0.043 Uiso 1 1 calc R U . . . C58 C 0.6037(3) 0.2529(2) 0.7109(2) 0.0237(9) Uani 1 1 d . . . . . C59 C 0.4963(4) 0.5049(3) 0.6786(2) 0.0359(11) Uani 1 1 d . . . . . H59 H 0.437480 0.504462 0.721735 0.043 Uiso 1 1 calc R U . . . C60 C 0.5665(4) 0.5593(3) 0.6959(2) 0.0466(12) Uani 1 1 d . . . . . H60A H 0.611632 0.528700 0.741253 0.070 Uiso 1 1 calc R U . . . H60B H 0.515422 0.614595 0.706795 0.070 Uiso 1 1 calc R U . . . H60C H 0.616433 0.568536 0.650460 0.070 Uiso 1 1 calc R U . . . C61 C 0.4359(4) 0.5477(3) 0.6015(3) 0.0510(13) Uani 1 1 d . . . . . H61A H 0.491377 0.555488 0.559407 0.076 Uiso 1 1 calc R U . . . H61B H 0.380958 0.603432 0.607635 0.076 Uiso 1 1 calc R U . . . H61C H 0.397105 0.511138 0.588553 0.076 Uiso 1 1 calc R U . . . C62 C 0.5687(3) 0.1764(2) 0.7564(2) 0.0264(9) Uani 1 1 d . . . . . H62 H 0.484542 0.195253 0.758430 0.032 Uiso 1 1 calc R U . . . C63 C 0.6119(4) 0.0962(2) 0.7161(2) 0.0428(12) Uani 1 1 d . . . . . H63A H 0.694028 0.072478 0.717491 0.064 Uiso 1 1 calc R U . . . H63B H 0.590021 0.112629 0.661766 0.064 Uiso 1 1 calc R U . . . H63C H 0.578715 0.053060 0.743677 0.064 Uiso 1 1 calc R U . . . C64 C 0.6054(4) 0.1487(2) 0.8424(2) 0.0377(11) Uani 1 1 d . . . . . H64A H 0.584345 0.098351 0.866995 0.057 Uiso 1 1 calc R U . . . H64B H 0.567753 0.195669 0.871203 0.057 Uiso 1 1 calc R U . . . H64C H 0.687076 0.134760 0.843010 0.057 Uiso 1 1 calc R U . . . C65 C 0.2556(3) 0.3390(2) 0.6031(2) 0.0226(9) Uani 1 1 d . . . . . C66 C 0.1711(3) 0.4924(2) 0.5799(2) 0.0250(9) Uani 1 1 d . . . . . C67 C 0.1456(3) 0.4912(3) 0.5046(2) 0.0333(10) Uani 1 1 d . . . . . H67 H 0.108375 0.542996 0.471369 0.040 Uiso 1 1 calc R U . . . C68 C 0.1760(3) 0.4116(3) 0.4785(2) 0.0340(11) Uani 1 1 d . . . . . H68 H 0.158483 0.410503 0.427547 0.041 Uiso 1 1 calc R U . . . C69 C 0.2309(3) 0.3353(3) 0.5264(2) 0.0278(9) Uani 1 1 d . . . . . H69 H 0.251409 0.282290 0.508693 0.033 Uiso 1 1 calc R U . . . C70 C 0.1404(4) 0.5753(2) 0.6123(2) 0.0389(11) Uani 1 1 d . . . . . H70A H 0.147012 0.561854 0.668974 0.058 Uiso 1 1 calc R U . . . H70B H 0.062906 0.610503 0.600048 0.058 Uiso 1 1 calc R U . . . H70C H 0.191670 0.606804 0.588563 0.058 Uiso 1 1 calc R U . . . N4 N 0.2116(2) 0.34145(17) 0.83728(16) 0.0169(7) Uani 1 1 d . . . . . N5 N 0.4384(2) 0.35372(17) 0.77220(16) 0.0163(7) Uani 1 1 d . . . . . N6 N 0.2258(2) 0.41686(19) 0.62812(16) 0.0194(7) Uani 1 1 d . . . . . O2 O 0.3075(2) 0.27217(15) 0.65556(13) 0.0226(6) Uani 1 1 d . . . . . Zn2 Zn 0.29733(4) 0.35034(3) 0.73582(2) 0.01946(12) 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 C1 0.019(2) 0.019(2) 0.022(2) -0.0053(17) 0.0029(17) -0.0116(17) C2 0.038(3) 0.018(2) 0.019(2) -0.0082(17) 0.0008(18) -0.012(2) C3 0.040(3) 0.021(2) 0.018(2) -0.0036(17) -0.0017(19) -0.020(2) C4 0.027(2) 0.027(2) 0.025(2) -0.0104(18) 0.0033(18) -0.0062(19) C5 0.065(3) 0.033(3) 0.017(2) -0.0067(19) -0.010(2) -0.006(2) C6 0.015(2) 0.031(2) 0.014(2) -0.0099(17) 0.0014(16) -0.0007(18) C7 0.020(2) 0.031(2) 0.021(2) -0.0128(18) 0.0009(17) -0.0047(19) C8 0.021(2) 0.036(3) 0.034(3) -0.021(2) -0.0022(19) -0.0039(19) C9 0.025(3) 0.037(3) 0.026(2) -0.017(2) -0.0070(19) 0.006(2) C10 0.028(2) 0.027(2) 0.021(2) -0.0081(18) -0.0012(18) 0.0033(19) C11 0.020(2) 0.023(2) 0.019(2) -0.0079(17) -0.0012(17) 0.0020(17) C12 0.021(2) 0.036(2) 0.038(3) -0.008(2) -0.0042(19) -0.0124(19) C13 0.091(5) 0.056(3) 0.071(4) -0.022(3) 0.028(3) -0.048(3) C14 0.106(5) 0.035(3) 0.058(3) -0.018(2) -0.009(3) -0.022(3) C15 0.038(3) 0.028(2) 0.021(2) 0.0017(18) -0.0087(19) -0.011(2) C16 0.031(3) 0.029(2) 0.056(3) -0.013(2) -0.001(2) -0.006(2) C17 0.043(3) 0.034(3) 0.037(3) -0.013(2) 0.004(2) -0.012(2) C18 0.028(2) 0.024(2) 0.009(2) -0.0011(16) -0.0064(16) -0.0078(19) C19 0.026(2) 0.022(2) 0.015(2) -0.0050(16) -0.0011(17) -0.0094(18) C20 0.035(3) 0.020(2) 0.024(2) -0.0062(17) 0.0000(18) -0.012(2) C21 0.034(3) 0.023(2) 0.022(2) -0.0068(17) -0.0090(18) -0.0021(19) C22 0.023(2) 0.041(3) 0.017(2) -0.0027(18) -0.0070(17) -0.010(2) C23 0.029(3) 0.028(2) 0.019(2) 0.0055(17) -0.0129(18) -0.011(2) C24 0.023(2) 0.020(2) 0.028(2) -0.0031(18) 0.0008(18) -0.0072(18) C25 0.042(3) 0.043(3) 0.037(3) -0.011(2) 0.010(2) -0.022(2) C26 0.031(3) 0.037(3) 0.033(3) -0.005(2) -0.0016(19) -0.019(2) C27 0.034(3) 0.038(3) 0.084(4) 0.032(3) -0.033(3) -0.021(2) C28 0.155(6) 0.050(4) 0.141(5) 0.027(3) -0.098(5) -0.070(4) C29 0.032(3) 0.089(5) 0.173(6) 0.068(4) -0.011(4) -0.029(3) C30 0.021(2) 0.019(2) 0.024(2) -0.0022(18) -0.0086(18) 0.0031(18) C31 0.039(3) 0.025(2) 0.023(2) -0.0061(18) -0.005(2) 0.000(2) C32 0.038(3) 0.039(3) 0.018(2) -0.001(2) 0.005(2) 0.005(2) C33 0.034(3) 0.042(3) 0.025(2) 0.004(2) 0.004(2) -0.012(2) C34 0.028(3) 0.027(2) 0.021(2) 0.0037(18) -0.0046(19) -0.006(2) C35 0.045(3) 0.042(3) 0.034(3) 0.006(2) -0.007(2) -0.025(2) N1 0.0172(18) 0.0208(17) 0.0178(18) -0.0035(14) -0.0023(14) -0.0039(14) N2 0.0205(19) 0.0223(17) 0.0169(17) -0.0030(14) -0.0058(14) -0.0089(15) N3 0.0220(19) 0.0247(18) 0.0132(17) 0.0019(14) -0.0037(14) -0.0051(15) O1 0.0312(17) 0.0265(15) 0.0210(15) -0.0060(12) -0.0004(12) -0.0123(13) Zn1 0.0198(3) 0.0229(3) 0.0156(3) -0.0011(2) -0.0016(2) -0.0045(2) C36 0.018(2) 0.016(2) 0.015(2) -0.0036(16) 0.0022(17) -0.0019(17) C37 0.020(2) 0.017(2) 0.015(2) -0.0049(15) -0.0035(16) -0.0036(17) C38 0.016(2) 0.0085(18) 0.021(2) -0.0030(15) -0.0056(16) 0.0028(16) C39 0.024(2) 0.032(2) 0.021(2) -0.0081(18) -0.0016(18) -0.0098(19) C40 0.023(2) 0.024(2) 0.022(2) -0.0061(17) -0.0008(17) -0.0079(18) C41 0.021(2) 0.029(2) 0.010(2) -0.0093(16) 0.0004(16) -0.0083(18) C42 0.018(2) 0.029(2) 0.014(2) -0.0095(16) 0.0035(16) -0.0097(18) C43 0.020(2) 0.038(3) 0.021(2) -0.0144(19) 0.0015(17) -0.007(2) C44 0.024(3) 0.040(3) 0.034(3) -0.014(2) 0.0022(19) -0.016(2) C45 0.042(3) 0.029(2) 0.032(2) -0.0096(19) 0.000(2) -0.021(2) C46 0.032(3) 0.027(2) 0.020(2) -0.0084(18) 0.0005(18) -0.010(2) C47 0.016(2) 0.033(2) 0.025(2) -0.0006(18) -0.0052(17) -0.0063(18) C48 0.071(4) 0.030(3) 0.036(3) -0.005(2) 0.006(2) -0.009(2) C49 0.047(3) 0.048(3) 0.046(3) 0.008(2) -0.019(2) -0.015(2) C50 0.030(3) 0.020(2) 0.044(3) -0.005(2) -0.010(2) -0.012(2) C51 0.034(3) 0.028(2) 0.051(3) -0.005(2) -0.008(2) -0.006(2) C52 0.059(3) 0.030(3) 0.044(3) 0.001(2) -0.020(2) -0.012(2) C53 0.015(2) 0.030(2) 0.016(2) -0.0079(17) -0.0030(16) -0.0079(18) C54 0.022(2) 0.034(2) 0.022(2) -0.0060(18) 0.0041(18) -0.0101(19) C55 0.032(3) 0.040(3) 0.035(3) -0.005(2) 0.007(2) -0.015(2) C56 0.022(3) 0.061(3) 0.034(3) -0.016(2) 0.0120(19) -0.011(2) C57 0.032(3) 0.038(3) 0.035(3) -0.019(2) -0.001(2) -0.001(2) C58 0.021(2) 0.029(2) 0.020(2) -0.0093(18) -0.0054(17) -0.0022(18) C59 0.036(3) 0.031(2) 0.038(3) -0.002(2) 0.013(2) -0.013(2) C60 0.061(3) 0.044(3) 0.038(3) -0.011(2) 0.006(2) -0.022(3) C61 0.040(3) 0.034(3) 0.077(4) 0.002(3) -0.013(3) -0.014(2) C62 0.020(2) 0.024(2) 0.031(2) -0.0129(18) -0.0032(18) 0.0033(18) C63 0.060(3) 0.032(3) 0.036(3) -0.014(2) -0.009(2) -0.009(2) C64 0.044(3) 0.029(2) 0.036(3) -0.011(2) -0.002(2) -0.004(2) C65 0.018(2) 0.029(2) 0.023(2) 0.0007(18) 0.0009(17) -0.0136(19) C66 0.019(2) 0.029(2) 0.025(2) 0.0016(18) 0.0017(18) -0.0089(19) C67 0.032(3) 0.040(3) 0.024(2) 0.011(2) -0.0076(19) -0.014(2) C68 0.032(3) 0.053(3) 0.018(2) -0.004(2) -0.0075(19) -0.015(2) C69 0.035(3) 0.035(2) 0.017(2) -0.0037(18) -0.0052(18) -0.015(2) C70 0.041(3) 0.027(2) 0.043(3) 0.000(2) 0.001(2) -0.007(2) N4 0.0147(18) 0.0187(17) 0.0161(17) -0.0011(13) -0.0037(13) -0.0042(14) N5 0.0155(18) 0.0153(16) 0.0173(17) -0.0041(13) -0.0007(13) -0.0031(13) N6 0.0179(19) 0.0264(18) 0.0150(17) -0.0021(14) -0.0043(14) -0.0085(15) O2 0.0285(16) 0.0212(14) 0.0176(14) -0.0039(11) -0.0053(12) -0.0057(12) Zn2 0.0201(3) 0.0238(3) 0.0141(2) -0.00383(19) -0.0028(2) -0.0056(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C2 1.404(5) . ? C1 C4 1.516(5) . ? C1 N1 1.320(4) . ? C2 H2 0.9300 . ? C2 C3 1.396(5) . ? C3 C5 1.516(5) . ? C3 N2 1.333(4) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.407(5) . ? C6 C11 1.396(5) . ? C6 N1 1.442(4) . ? C7 C8 1.386(5) . ? C7 C12 1.523(5) . ? C8 H8 0.9300 . ? C8 C9 1.376(5) . ? C9 H9 0.9300 . ? C9 C10 1.380(5) . ? C10 H10 0.9300 . ? C10 C11 1.385(5) . ? C11 C15 1.523(5) . ? C12 H12 0.9800 . ? C12 C13 1.515(6) . ? C12 C14 1.510(5) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15 0.9800 . ? C15 C16 1.531(5) . ? C15 C17 1.532(5) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.412(5) . ? C18 C23 1.395(5) . ? C18 N2 1.436(4) . ? C19 C20 1.382(5) . ? C19 C24 1.516(5) . ? C20 H20 0.9300 . ? C20 C21 1.370(5) . ? C21 H21 0.9300 . ? C21 C22 1.377(5) . ? C22 H22 0.9300 . ? C22 C23 1.394(5) . ? C23 C27 1.521(5) . ? C24 H24 0.9800 . ? C24 C25 1.542(5) . ? C24 C26 1.528(5) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27 0.9800 . ? C27 C28 1.526(7) . ? C27 C29 1.520(7) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 C31 1.413(5) . ? C30 N3 1.365(4) . ? C30 O1 1.296(4) . ? C31 H31 0.9300 . ? C31 C32 1.358(5) . ? C32 H32 0.9300 . ? C32 C33 1.391(5) . ? C33 H33 0.9300 . ? C33 C34 1.363(5) . ? C34 C35 1.501(5) . ? C34 N3 1.348(4) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? N1 Zn1 1.950(3) . ? N2 Zn1 1.944(3) . ? N3 Zn1 2.062(3) . ? O1 Zn1 2.037(2) . ? C36 C37 1.392(5) . ? C36 C39 1.515(5) . ? C36 N4 1.335(4) . ? C37 H37 0.9300 . ? C37 C38 1.408(5) . ? C38 C40 1.517(4) . ? C38 N5 1.317(4) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C42 1.392(5) . ? C41 C46 1.416(5) . ? C41 N4 1.439(4) . ? C42 C43 1.391(5) . ? C42 C47 1.516(5) . ? C43 H43 0.9300 . ? C43 C44 1.376(5) . ? C44 H44 0.9300 . ? C44 C45 1.373(5) . ? C45 H45 0.9300 . ? C45 C46 1.383(5) . ? C46 C50 1.518(5) . ? C47 H47 0.9800 . ? C47 C48 1.520(5) . ? C47 C49 1.519(5) . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 H50 0.9800 . ? C50 C51 1.527(5) . ? C50 C52 1.530(5) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 C54 1.408(5) . ? C53 C58 1.413(5) . ? C53 N5 1.434(4) . ? C54 C55 1.377(5) . ? C54 C59 1.524(5) . ? C55 H55 0.9300 . ? C55 C56 1.381(5) . ? C56 H56 0.9300 . ? C56 C57 1.373(5) . ? C57 H57 0.9300 . ? C57 C58 1.385(5) . ? C58 C62 1.517(5) . ? C59 H59 0.9800 . ? C59 C60 1.534(5) . ? C59 C61 1.516(5) . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 H62 0.9800 . ? C62 C63 1.526(5) . ? C62 C64 1.527(5) . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 C69 1.404(5) . ? C65 N6 1.357(4) . ? C65 O2 1.301(4) . ? C66 C67 1.369(5) . ? C66 C70 1.497(5) . ? C66 N6 1.356(4) . ? C67 H67 0.9300 . ? C67 C68 1.393(5) . ? C68 H68 0.9300 . ? C68 C69 1.361(5) . ? C69 H69 0.9300 . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? N4 Zn2 1.942(3) . ? N5 Zn2 1.943(3) . ? N6 Zn2 2.074(3) . ? O2 Zn2 2.038(2) . ? 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 C2 C1 C4 117.1(3) . . ? N1 C1 C2 124.2(3) . . ? N1 C1 C4 118.7(3) . . ? C1 C2 H2 115.0 . . ? C3 C2 C1 130.1(3) . . ? C3 C2 H2 115.0 . . ? C2 C3 C5 116.3(4) . . ? N2 C3 C2 123.9(3) . . ? N2 C3 C5 119.7(4) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 N1 117.9(3) . . ? C11 C6 C7 122.0(3) . . ? C11 C6 N1 120.1(3) . . ? C6 C7 C12 121.6(3) . . ? C8 C7 C6 117.2(3) . . ? C8 C7 C12 121.2(3) . . ? C7 C8 H8 119.0 . . ? C9 C8 C7 121.9(4) . . ? C9 C8 H8 119.0 . . ? C8 C9 H9 120.3 . . ? C8 C9 C10 119.4(4) . . ? C10 C9 H9 120.3 . . ? C9 C10 H10 119.2 . . ? C9 C10 C11 121.5(4) . . ? C11 C10 H10 119.2 . . ? C6 C11 C15 121.6(3) . . ? C10 C11 C6 117.8(3) . . ? C10 C11 C15 120.5(3) . . ? C7 C12 H12 106.5 . . ? C13 C12 C7 113.7(3) . . ? C13 C12 H12 106.5 . . ? C14 C12 C7 114.4(3) . . ? C14 C12 H12 106.5 . . ? C14 C12 C13 108.7(4) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 H15 107.8 . . ? C11 C15 C16 110.2(3) . . ? C11 C15 C17 114.0(3) . . ? C16 C15 H15 107.8 . . ? C16 C15 C17 109.0(3) . . ? C17 C15 H15 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 N2 119.2(3) . . ? C23 C18 C19 120.3(3) . . ? C23 C18 N2 120.5(3) . . ? C18 C19 C24 121.6(3) . . ? C20 C19 C18 118.3(3) . . ? C20 C19 C24 120.0(3) . . ? C19 C20 H20 119.1 . . ? C21 C20 C19 121.8(3) . . ? C21 C20 H20 119.1 . . ? C20 C21 H21 120.1 . . ? C20 C21 C22 119.7(4) . . ? C22 C21 H21 120.1 . . ? C21 C22 H22 119.6 . . ? C21 C22 C23 120.8(4) . . ? C23 C22 H22 119.6 . . ? C18 C23 C27 122.0(3) . . ? C22 C23 C18 119.0(3) . . ? C22 C23 C27 119.0(4) . . ? C19 C24 H24 107.8 . . ? C19 C24 C25 112.4(3) . . ? C19 C24 C26 111.1(3) . . ? C25 C24 H24 107.8 . . ? C26 C24 H24 107.8 . . ? C26 C24 C25 109.7(3) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 H27 107.0 . . ? C23 C27 C28 112.0(4) . . ? C28 C27 H27 107.0 . . ? C29 C27 C23 112.0(4) . . ? C29 C27 H27 107.0 . . ? C29 C27 C28 111.5(4) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N3 C30 C31 119.7(4) . . ? O1 C30 C31 126.5(3) . . ? O1 C30 N3 113.8(3) . . ? C30 C31 H31 120.7 . . ? C32 C31 C30 118.5(4) . . ? C32 C31 H31 120.7 . . ? C31 C32 H32 119.7 . . ? C31 C32 C33 120.6(4) . . ? C33 C32 H32 119.7 . . ? C32 C33 H33 120.1 . . ? C34 C33 C32 119.8(4) . . ? C34 C33 H33 120.1 . . ? C33 C34 C35 122.8(4) . . ? N3 C34 C33 120.5(4) . . ? N3 C34 C35 116.8(3) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35B 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C1 N1 C6 118.7(3) . . ? C1 N1 Zn1 120.7(2) . . ? C6 N1 Zn1 120.5(2) . . ? C3 N2 C18 118.3(3) . . ? C3 N2 Zn1 120.7(3) . . ? C18 N2 Zn1 120.4(2) . . ? C30 N3 Zn1 88.6(2) . . ? C34 N3 C30 120.9(3) . . ? C34 N3 Zn1 150.5(3) . . ? C30 O1 Zn1 91.7(2) . . ? N1 Zn1 N3 127.05(11) . . ? N1 Zn1 O1 118.19(11) . . ? N2 Zn1 N1 99.27(12) . . ? N2 Zn1 N3 122.08(12) . . ? N2 Zn1 O1 124.24(11) . . ? O1 Zn1 N3 65.89(11) . . ? C37 C36 C39 116.1(3) . . ? N4 C36 C37 124.9(3) . . ? N4 C36 C39 118.9(3) . . ? C36 C37 H37 115.4 . . ? C36 C37 C38 129.3(3) . . ? C38 C37 H37 115.4 . . ? C37 C38 C40 116.8(3) . . ? N5 C38 C37 124.2(3) . . ? N5 C38 C40 119.0(3) . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39B 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40B 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C46 121.3(3) . . ? C42 C41 N4 120.2(3) . . ? C46 C41 N4 118.5(3) . . ? C41 C42 C47 122.1(3) . . ? C43 C42 C41 118.4(3) . . ? C43 C42 C47 119.5(3) . . ? C42 C43 H43 119.4 . . ? C44 C43 C42 121.3(4) . . ? C44 C43 H43 119.4 . . ? C43 C44 H44 120.3 . . ? C45 C44 C43 119.3(4) . . ? C45 C44 H44 120.3 . . ? C44 C45 H45 118.8 . . ? C44 C45 C46 122.4(4) . . ? C46 C45 H45 118.8 . . ? C41 C46 C50 122.6(3) . . ? C45 C46 C41 117.2(4) . . ? C45 C46 C50 120.1(3) . . ? C42 C47 H47 107.5 . . ? C42 C47 C48 111.7(3) . . ? C42 C47 C49 112.9(3) . . ? C48 C47 H47 107.5 . . ? C49 C47 H47 107.5 . . ? C49 C47 C48 109.6(3) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48B 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49B 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C46 C50 H50 107.6 . . ? C46 C50 C51 111.0(3) . . ? C46 C50 C52 112.6(3) . . ? C51 C50 H50 107.6 . . ? C51 C50 C52 110.2(3) . . ? C52 C50 H50 107.6 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51B 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52B 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 C53 C58 120.8(3) . . ? C54 C53 N5 120.6(3) . . ? C58 C53 N5 118.5(3) . . ? C53 C54 C59 122.1(3) . . ? C55 C54 C53 118.7(4) . . ? C55 C54 C59 119.1(3) . . ? C54 C55 H55 119.5 . . ? C54 C55 C56 121.0(4) . . ? C56 C55 H55 119.5 . . ? C55 C56 H56 120.0 . . ? C57 C56 C55 120.1(4) . . ? C57 C56 H56 120.0 . . ? C56 C57 H57 119.2 . . ? C56 C57 C58 121.7(4) . . ? C58 C57 H57 119.2 . . ? C53 C58 C62 121.0(3) . . ? C57 C58 C53 117.7(3) . . ? C57 C58 C62 121.3(3) . . ? C54 C59 H59 108.0 . . ? C54 C59 C60 112.7(3) . . ? C60 C59 H59 108.0 . . ? C61 C59 C54 110.4(3) . . ? C61 C59 H59 108.0 . . ? C61 C59 C60 109.6(3) . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60B 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C59 C61 H61A 109.5 . . ? C59 C61 H61B 109.5 . . ? C59 C61 H61C 109.5 . . ? H61A C61 H61B 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C58 C62 H62 107.0 . . ? C58 C62 C63 113.4(3) . . ? C58 C62 C64 113.5(3) . . ? C63 C62 H62 107.0 . . ? C63 C62 C64 108.4(3) . . ? C64 C62 H62 107.0 . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63B 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C62 C64 H64A 109.5 . . ? C62 C64 H64B 109.5 . . ? C62 C64 H64C 109.5 . . ? H64A C64 H64B 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? N6 C65 C69 120.4(3) . . ? O2 C65 C69 125.4(3) . . ? O2 C65 N6 114.2(3) . . ? C67 C66 C70 122.2(4) . . ? N6 C66 C67 120.3(3) . . ? N6 C66 C70 117.5(3) . . ? C66 C67 H67 120.4 . . ? C66 C67 C68 119.2(4) . . ? C68 C67 H67 120.4 . . ? C67 C68 H68 119.4 . . ? C69 C68 C67 121.1(4) . . ? C69 C68 H68 119.4 . . ? C65 C69 H69 120.9 . . ? C68 C69 C65 118.1(4) . . ? C68 C69 H69 120.9 . . ? C66 C70 H70A 109.5 . . ? C66 C70 H70B 109.5 . . ? C66 C70 H70C 109.5 . . ? H70A C70 H70B 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C36 N4 C41 119.5(3) . . ? C36 N4 Zn2 120.0(2) . . ? C41 N4 Zn2 120.0(2) . . ? C38 N5 C53 119.4(3) . . ? C38 N5 Zn2 121.0(2) . . ? C53 N5 Zn2 119.3(2) . . ? C65 N6 Zn2 88.5(2) . . ? C66 N6 C65 120.9(3) . . ? C66 N6 Zn2 150.6(3) . . ? C65 O2 Zn2 91.6(2) . . ? N4 Zn2 N5 99.41(12) . . ? N4 Zn2 N6 124.89(11) . . ? N4 Zn2 O2 122.14(11) . . ? N5 Zn2 N6 125.07(11) . . ? N5 Zn2 O2 119.01(11) . . ? O2 Zn2 N6 65.73(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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C2 C3 C5 -168.7(3) . . . . ? C1 C2 C3 N2 7.9(6) . . . . ? C2 C1 N1 C6 173.3(3) . . . . ? C2 C1 N1 Zn1 -2.5(5) . . . . ? C2 C3 N2 C18 -168.6(3) . . . . ? C2 C3 N2 Zn1 2.5(5) . . . . ? C4 C1 C2 C3 169.9(4) . . . . ? C4 C1 N1 C6 -4.5(5) . . . . ? C4 C1 N1 Zn1 179.7(2) . . . . ? C5 C3 N2 C18 7.9(5) . . . . ? C5 C3 N2 Zn1 179.0(3) . . . . ? C6 C7 C8 C9 1.9(5) . . . . ? C6 C7 C12 C13 82.6(5) . . . . ? C6 C7 C12 C14 -151.7(4) . . . . ? C6 C11 C15 C16 106.0(4) . . . . ? C6 C11 C15 C17 -131.1(4) . . . . ? C7 C6 C11 C10 2.6(5) . . . . ? C7 C6 C11 C15 -175.8(3) . . . . ? C7 C6 N1 C1 -94.2(4) . . . . ? C7 C6 N1 Zn1 81.6(4) . . . . ? C7 C8 C9 C10 0.8(6) . . . . ? C8 C7 C12 C13 -98.9(4) . . . . ? C8 C7 C12 C14 26.8(5) . . . . ? C8 C9 C10 C11 -2.0(6) . . . . ? C9 C10 C11 C6 0.3(5) . . . . ? C9 C10 C11 C15 178.7(3) . . . . ? C10 C11 C15 C16 -72.3(4) . . . . ? C10 C11 C15 C17 50.5(5) . . . . ? C11 C6 C7 C8 -3.7(5) . . . . ? C11 C6 C7 C12 174.9(3) . . . . ? C11 C6 N1 C1 87.3(4) . . . . ? C11 C6 N1 Zn1 -96.9(3) . . . . ? C12 C7 C8 C9 -176.7(3) . . . . ? C18 C19 C20 C21 0.8(5) . . . . ? C18 C19 C24 C25 -132.6(3) . . . . ? C18 C19 C24 C26 104.1(4) . . . . ? C18 C23 C27 C28 97.3(5) . . . . ? C18 C23 C27 C29 -136.6(4) . . . . ? C19 C18 C23 C22 -2.4(5) . . . . ? C19 C18 C23 C27 177.7(4) . . . . ? C19 C18 N2 C3 80.0(4) . . . . ? C19 C18 N2 Zn1 -91.1(3) . . . . ? C19 C20 C21 C22 -2.5(5) . . . . ? C20 C19 C24 C25 51.3(4) . . . . ? C20 C19 C24 C26 -72.0(4) . . . . ? C20 C21 C22 C23 1.7(5) . . . . ? C21 C22 C23 C18 0.7(5) . . . . ? C21 C22 C23 C27 -179.4(4) . . . . ? C22 C23 C27 C28 -82.5(5) . . . . ? C22 C23 C27 C29 43.6(5) . . . . ? C23 C18 C19 C20 1.7(5) . . . . ? C23 C18 C19 C24 -174.5(3) . . . . ? C23 C18 N2 C3 -102.5(4) . . . . ? C23 C18 N2 Zn1 86.4(4) . . . . ? C24 C19 C20 C21 177.1(3) . . . . ? C30 C31 C32 C33 -0.2(6) . . . . ? C31 C30 N3 C34 -1.1(5) . . . . ? C31 C30 N3 Zn1 179.3(3) . . . . ? C31 C30 O1 Zn1 -179.3(3) . . . . ? C31 C32 C33 C34 -1.1(6) . . . . ? C32 C33 C34 C35 -178.1(4) . . . . ? C32 C33 C34 N3 1.3(6) . . . . ? C33 C34 N3 C30 -0.2(5) . . . . ? C33 C34 N3 Zn1 179.0(3) . . . . ? C35 C34 N3 C30 179.2(3) . . . . ? C35 C34 N3 Zn1 -1.6(7) . . . . ? N1 C1 C2 C3 -7.9(6) . . . . ? N1 C6 C7 C8 177.9(3) . . . . ? N1 C6 C7 C12 -3.5(5) . . . . ? N1 C6 C11 C10 -179.0(3) . . . . ? N1 C6 C11 C15 2.6(5) . . . . ? N2 C18 C19 C20 179.2(3) . . . . ? N2 C18 C19 C24 3.0(5) . . . . ? N2 C18 C23 C22 -179.9(3) . . . . ? N2 C18 C23 C27 0.2(5) . . . . ? N3 C30 C31 C32 1.3(5) . . . . ? N3 C30 O1 Zn1 0.9(3) . . . . ? O1 C30 C31 C32 -178.5(3) . . . . ? O1 C30 N3 C34 178.7(3) . . . . ? O1 C30 N3 Zn1 -0.9(3) . . . . ? C36 C37 C38 C40 -171.0(3) . . . . ? C36 C37 C38 N5 8.3(6) . . . . ? C37 C36 N4 C41 168.6(3) . . . . ? C37 C36 N4 Zn2 -3.2(5) . . . . ? C37 C38 N5 C53 -172.2(3) . . . . ? C37 C38 N5 Zn2 2.0(4) . . . . ? C39 C36 C37 C38 169.5(3) . . . . ? C39 C36 N4 C41 -8.4(5) . . . . ? C39 C36 N4 Zn2 179.8(2) . . . . ? C40 C38 N5 C53 7.1(4) . . . . ? C40 C38 N5 Zn2 -178.7(2) . . . . ? C41 C42 C43 C44 0.7(5) . . . . ? C41 C42 C47 C48 -102.5(4) . . . . ? C41 C42 C47 C49 133.5(4) . . . . ? C41 C46 C50 C51 -104.2(4) . . . . ? C41 C46 C50 C52 131.8(4) . . . . ? C42 C41 C46 C45 -0.3(5) . . . . ? C42 C41 C46 C50 176.4(3) . . . . ? C42 C41 N4 C36 104.2(4) . . . . ? C42 C41 N4 Zn2 -84.1(3) . . . . ? C42 C43 C44 C45 -0.4(5) . . . . ? C43 C42 C47 C48 77.2(4) . . . . ? C43 C42 C47 C49 -46.8(5) . . . . ? C43 C44 C45 C46 -0.4(6) . . . . ? C44 C45 C46 C41 0.7(5) . . . . ? C44 C45 C46 C50 -176.1(3) . . . . ? C45 C46 C50 C51 72.5(4) . . . . ? C45 C46 C50 C52 -51.5(5) . . . . ? C46 C41 C42 C43 -0.3(5) . . . . ? C46 C41 C42 C47 179.3(3) . . . . ? C46 C41 N4 C36 -78.9(4) . . . . ? C46 C41 N4 Zn2 92.9(3) . . . . ? C47 C42 C43 C44 -179.0(3) . . . . ? C53 C54 C55 C56 -0.6(6) . . . . ? C53 C54 C59 C60 128.1(4) . . . . ? C53 C54 C59 C61 -108.9(4) . . . . ? C53 C58 C62 C63 155.3(3) . . . . ? C53 C58 C62 C64 -80.3(4) . . . . ? C54 C53 C58 C57 2.2(5) . . . . ? C54 C53 C58 C62 -177.4(3) . . . . ? C54 C53 N5 C38 -87.9(4) . . . . ? C54 C53 N5 Zn2 97.7(3) . . . . ? C54 C55 C56 C57 1.2(6) . . . . ? C55 C54 C59 C60 -55.5(5) . . . . ? C55 C54 C59 C61 67.5(5) . . . . ? C55 C56 C57 C58 0.0(6) . . . . ? C56 C57 C58 C53 -1.7(6) . . . . ? C56 C57 C58 C62 177.9(3) . . . . ? C57 C58 C62 C63 -24.3(5) . . . . ? C57 C58 C62 C64 100.1(4) . . . . ? C58 C53 C54 C55 -1.2(5) . . . . ? C58 C53 C54 C59 175.3(3) . . . . ? C58 C53 N5 C38 95.6(4) . . . . ? C58 C53 N5 Zn2 -78.7(3) . . . . ? C59 C54 C55 C56 -177.1(4) . . . . ? C66 C67 C68 C69 -0.3(6) . . . . ? C67 C66 N6 C65 -0.3(5) . . . . ? C67 C66 N6 Zn2 179.5(4) . . . . ? C67 C68 C69 C65 0.3(6) . . . . ? C69 C65 N6 C66 0.3(5) . . . . ? C69 C65 N6 Zn2 -179.6(3) . . . . ? C69 C65 O2 Zn2 179.6(3) . . . . ? C70 C66 C67 C68 -179.6(4) . . . . ? C70 C66 N6 C65 179.6(3) . . . . ? C70 C66 N6 Zn2 -0.6(7) . . . . ? N4 C36 C37 C38 -7.6(6) . . . . ? N4 C41 C42 C43 176.5(3) . . . . ? N4 C41 C42 C47 -3.8(5) . . . . ? N4 C41 C46 C45 -177.2(3) . . . . ? N4 C41 C46 C50 -0.5(5) . . . . ? N5 C53 C54 C55 -177.5(3) . . . . ? N5 C53 C54 C59 -1.1(5) . . . . ? N5 C53 C58 C57 178.7(3) . . . . ? N5 C53 C58 C62 -0.9(5) . . . . ? N6 C65 C69 C68 -0.3(5) . . . . ? N6 C65 O2 Zn2 -0.1(3) . . . . ? N6 C66 C67 C68 0.3(6) . . . . ? O2 C65 C69 C68 -179.9(3) . . . . ? O2 C65 N6 C66 180.0(3) . . . . ? O2 C65 N6 Zn2 0.1(3) . . . . ? _shelx_res_file ; TITL db39b_reprocess_twin1_hklf4_a.res in P-1 db39b_reprocess_twin1_hklf4.res created by SHELXL-2018/3 at 11:39:20 on 17-Jun-2022 REM Old TITL DB39b_reprocess_twin1_hklf4 in P-1 REM SHELXT solution in P-1: R1 0.153, Rweak 0.022, Alpha 0.071 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C69 N4 O5 Zn2 CELL 0.71073 12.3962 16.5432 17.1649 78.352 83.508 70.096 ZERR 4 0.0003 0.0004 0.0004 0.002 0.002 0.002 LATT 1 SFAC C H N O Zn UNIT 140 188 12 4 4 DELU C27 C29 C28 SIMU 0.04 0.08 1.7 C27 C29 C28 SIMU 0.04 0.08 1.7 C12 C13 C14 DELU C14 C12 C13 L.S. 20 0 0 PLAN 10 SIZE 0.073 0.216 0.425 CONF FREE Zn1 C30 FREE C65 Zn2 BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.045900 BASF 0.12640 FVAR 2.62138 C1 1 0.057425 0.970199 0.810369 11.00000 0.01950 0.01904 = 0.02241 -0.00527 0.00293 -0.01158 C2 1 0.115876 0.931498 0.880924 11.00000 0.03788 0.01828 = 0.01946 -0.00822 0.00084 -0.01246 AFIX 43 H2 2 0.083557 0.958149 0.924698 11.00000 -1.20000 AFIX 0 C3 1 0.214903 0.859281 0.895628 11.00000 0.03972 0.02126 = 0.01801 -0.00358 -0.00167 -0.02008 C4 1 -0.059385 1.039013 0.817042 11.00000 0.02687 0.02743 = 0.02464 -0.01040 0.00330 -0.00621 AFIX 137 H4A 2 -0.057477 1.093798 0.786087 11.00000 -1.50000 H4B 2 -0.078438 1.045155 0.871801 11.00000 -1.50000 H4C 2 -0.116205 1.021660 0.797465 11.00000 -1.50000 AFIX 0 C5 1 0.242598 0.824111 0.982288 11.00000 0.06548 0.03344 = 0.01739 -0.00672 -0.01020 -0.00585 AFIX 137 H5A 2 0.212082 0.777312 1.001984 11.00000 -1.50000 H5B 2 0.208861 0.869933 1.012932 11.00000 -1.50000 H5C 2 0.324384 0.802822 0.986815 11.00000 -1.50000 AFIX 0 C6 1 0.022249 0.986501 0.673881 11.00000 0.01508 0.03087 = 0.01404 -0.00988 0.00143 -0.00067 C7 1 -0.044650 0.939136 0.656694 11.00000 0.01961 0.03112 = 0.02091 -0.01276 0.00089 -0.00467 C8 1 -0.118052 0.977832 0.594578 11.00000 0.02093 0.03615 = 0.03397 -0.02094 -0.00218 -0.00389 AFIX 43 H8 2 -0.164989 0.948789 0.582921 11.00000 -1.20000 AFIX 0 C9 1 -0.123522 1.057968 0.549643 11.00000 0.02480 0.03750 = 0.02600 -0.01690 -0.00698 0.00623 AFIX 43 H9 2 -0.174229 1.082875 0.508721 11.00000 -1.20000 AFIX 0 C10 1 -0.053133 1.101032 0.565827 11.00000 0.02793 0.02689 = 0.02113 -0.00805 -0.00117 0.00331 AFIX 43 H10 2 -0.055282 1.154296 0.534285 11.00000 -1.20000 AFIX 0 C11 1 0.020621 1.066794 0.627932 11.00000 0.01985 0.02332 = 0.01877 -0.00794 -0.00119 0.00201 C12 1 -0.035028 0.848327 0.702903 11.00000 0.02097 0.03556 = 0.03821 -0.00812 -0.00421 -0.01240 AFIX 13 H12 2 0.045611 0.819919 0.716175 11.00000 -1.20000 AFIX 0 C13 1 -0.105079 0.848950 0.781184 11.00000 0.09111 0.05584 = 0.07147 -0.02197 0.02789 -0.04753 AFIX 137 H13A 2 -0.184421 0.880766 0.771425 11.00000 -1.50000 H13B 2 -0.077863 0.876442 0.815353 11.00000 -1.50000 H13C 2 -0.097343 0.790038 0.806377 11.00000 -1.50000 AFIX 0 C14 1 -0.063377 0.790431 0.656342 11.00000 0.10615 0.03512 = 0.05771 -0.01835 -0.00912 -0.02191 AFIX 137 H14A 2 -0.050905 0.733512 0.688194 11.00000 -1.50000 H14B 2 -0.014901 0.785617 0.608593 11.00000 -1.50000 H14C 2 -0.142344 0.815367 0.642644 11.00000 -1.50000 AFIX 0 C15 1 0.099194 1.114704 0.643507 11.00000 0.03817 0.02766 = 0.02116 0.00170 -0.00870 -0.01120 AFIX 13 H15 2 0.133861 1.085840 0.694676 11.00000 -1.20000 AFIX 0 C16 1 0.196363 1.107796 0.579076 11.00000 0.03119 0.02891 = 0.05555 -0.01332 -0.00117 -0.00639 AFIX 137 H16A 2 0.164910 1.138387 0.528679 11.00000 -1.50000 H16B 2 0.235675 1.047471 0.575843 11.00000 -1.50000 H16C 2 0.249443 1.133197 0.592299 11.00000 -1.50000 AFIX 0 C17 1 0.037349 1.211184 0.648189 11.00000 0.04294 0.03355 = 0.03680 -0.01304 0.00359 -0.01177 AFIX 137 H17A 2 0.088509 1.234613 0.667043 11.00000 -1.50000 H17B 2 -0.028865 1.216511 0.684201 11.00000 -1.50000 H17C 2 0.013643 1.242893 0.596256 11.00000 -1.50000 AFIX 0 C18 1 0.367543 0.735857 0.862824 11.00000 0.02839 0.02449 = 0.00869 -0.00113 -0.00639 -0.00783 C19 1 0.335595 0.659837 0.884215 11.00000 0.02576 0.02208 = 0.01529 -0.00498 -0.00106 -0.00943 C20 1 0.420487 0.580873 0.905958 11.00000 0.03532 0.01993 = 0.02393 -0.00616 -0.00005 -0.01219 AFIX 43 H20 2 0.400658 0.530234 0.919503 11.00000 -1.20000 AFIX 0 C21 1 0.533081 0.575082 0.908124 11.00000 0.03398 0.02310 = 0.02152 -0.00676 -0.00898 -0.00215 AFIX 43 H21 2 0.588092 0.521448 0.924968 11.00000 -1.20000 AFIX 0 C22 1 0.564425 0.649028 0.885249 11.00000 0.02261 0.04143 = 0.01690 -0.00270 -0.00701 -0.00967 AFIX 43 H22 2 0.641185 0.644728 0.885404 11.00000 -1.20000 AFIX 0 C23 1 0.482506 0.730213 0.861872 11.00000 0.02889 0.02805 = 0.01895 0.00548 -0.01287 -0.01101 C24 1 0.213108 0.662649 0.878831 11.00000 0.02335 0.02047 = 0.02816 -0.00307 0.00080 -0.00721 AFIX 13 H24 2 0.163968 0.723931 0.872199 11.00000 -1.20000 AFIX 0 C25 1 0.169233 0.613122 0.954769 11.00000 0.04154 0.04326 = 0.03734 -0.01147 0.00962 -0.02235 AFIX 137 H25A 2 0.089504 0.621181 0.950696 11.00000 -1.50000 H25B 2 0.178271 0.635311 1.000295 11.00000 -1.50000 H25C 2 0.212610 0.552041 0.960590 11.00000 -1.50000 AFIX 0 C26 1 0.201274 0.626247 0.806362 11.00000 0.03138 0.03700 = 0.03324 -0.00534 -0.00161 -0.01908 AFIX 137 H26A 2 0.245425 0.565289 0.812787 11.00000 -1.50000 H26B 2 0.229011 0.657010 0.759235 11.00000 -1.50000 H26C 2 0.121952 0.633575 0.801539 11.00000 -1.50000 AFIX 0 C27 1 0.521236 0.809928 0.836297 11.00000 0.03394 0.03818 = 0.08403 0.03193 -0.03314 -0.02071 AFIX 13 H27 2 0.460158 0.854959 0.805169 11.00000 -1.20000 AFIX 0 C28 1 0.535295 0.847263 0.907401 11.00000 0.15527 0.04981 = 0.14053 0.02712 -0.09815 -0.06979 AFIX 137 H28A 2 0.464055 0.861907 0.938387 11.00000 -1.50000 H28B 2 0.556558 0.898770 0.888775 11.00000 -1.50000 H28C 2 0.594119 0.804608 0.939786 11.00000 -1.50000 AFIX 0 C29 1 0.629442 0.791525 0.782137 11.00000 0.03159 0.08913 = 0.17276 0.06834 -0.01080 -0.02889 AFIX 137 H29A 2 0.692849 0.750903 0.811817 11.00000 -1.50000 H29B 2 0.645379 0.844967 0.761732 11.00000 -1.50000 H29C 2 0.618439 0.767081 0.738656 11.00000 -1.50000 AFIX 0 C30 1 0.346760 0.809350 0.606781 11.00000 0.02129 0.01947 = 0.02438 -0.00223 -0.00859 0.00311 C31 1 0.407319 0.783068 0.536396 11.00000 0.03920 0.02528 = 0.02306 -0.00613 -0.00518 -0.00034 AFIX 43 H31 2 0.390150 0.743382 0.512669 11.00000 -1.20000 AFIX 0 C32 1 0.491130 0.817053 0.504187 11.00000 0.03775 0.03915 = 0.01789 -0.00053 0.00528 0.00453 AFIX 43 H32 2 0.532025 0.800388 0.457957 11.00000 -1.20000 AFIX 0 C33 1 0.516370 0.876558 0.539707 11.00000 0.03413 0.04206 = 0.02526 0.00421 0.00423 -0.01249 AFIX 43 H33 2 0.574779 0.898800 0.517812 11.00000 -1.20000 AFIX 0 C34 1 0.455215 0.902189 0.606733 11.00000 0.02761 0.02727 = 0.02115 0.00372 -0.00460 -0.00612 C35 1 0.475188 0.968157 0.646877 11.00000 0.04455 0.04233 = 0.03414 0.00639 -0.00745 -0.02454 AFIX 137 H35A 2 0.417641 1.023913 0.632267 11.00000 -1.50000 H35B 2 0.549836 0.972737 0.630454 11.00000 -1.50000 H35C 2 0.470862 0.950010 0.703584 11.00000 -1.50000 AFIX 0 N1 3 0.096153 0.948521 0.740080 11.00000 0.01720 0.02076 = 0.01777 -0.00353 -0.00226 -0.00392 N2 3 0.280861 0.818469 0.839015 11.00000 0.02050 0.02227 = 0.01690 -0.00295 -0.00580 -0.00891 N3 3 0.371895 0.868982 0.639702 11.00000 0.02204 0.02470 = 0.01317 0.00188 -0.00371 -0.00507 O1 4 0.266368 0.782163 0.645979 11.00000 0.03123 0.02651 = 0.02101 -0.00597 -0.00042 -0.01226 ZN1 5 0.246051 0.860828 0.727520 11.00000 0.01975 0.02286 = 0.01562 -0.00115 -0.00158 -0.00449 C36 1 0.251532 0.351924 0.902271 11.00000 0.01787 0.01611 = 0.01506 -0.00357 0.00224 -0.00187 C37 1 0.355845 0.365328 0.905070 11.00000 0.02046 0.01691 = 0.01464 -0.00494 -0.00349 -0.00359 AFIX 43 H37 2 0.368171 0.378733 0.952681 11.00000 -1.20000 AFIX 0 C38 1 0.445374 0.361508 0.846185 11.00000 0.01648 0.00850 = 0.02119 -0.00299 -0.00564 0.00278 C39 1 0.182733 0.344925 0.980654 11.00000 0.02392 0.03181 = 0.02119 -0.00807 -0.00162 -0.00982 AFIX 137 H39A 2 0.102598 0.374387 0.971869 11.00000 -1.50000 H39B 2 0.207192 0.371431 1.017172 11.00000 -1.50000 H39C 2 0.194819 0.284521 1.002584 11.00000 -1.50000 AFIX 0 C40 1 0.556493 0.365841 0.871289 11.00000 0.02258 0.02377 = 0.02155 -0.00614 -0.00080 -0.00785 AFIX 137 H40A 2 0.618884 0.315304 0.860466 11.00000 -1.50000 H40B 2 0.550480 0.367398 0.927256 11.00000 -1.50000 H40C 2 0.570420 0.417561 0.842028 11.00000 -1.50000 AFIX 0 C41 1 0.113399 0.312204 0.844800 11.00000 0.02051 0.02900 = 0.01048 -0.00928 0.00037 -0.00831 C42 1 0.006252 0.371061 0.823019 11.00000 0.01846 0.02929 = 0.01353 -0.00948 0.00352 -0.00970 C43 1 -0.085160 0.339416 0.826992 11.00000 0.01994 0.03849 = 0.02126 -0.01443 0.00154 -0.00717 AFIX 43 H43 2 -0.157055 0.377901 0.812040 11.00000 -1.20000 AFIX 0 C44 1 -0.071281 0.252253 0.852623 11.00000 0.02383 0.04037 = 0.03403 -0.01416 0.00220 -0.01551 AFIX 43 H44 2 -0.133299 0.232092 0.855271 11.00000 -1.20000 AFIX 0 C45 1 0.035046 0.195348 0.874248 11.00000 0.04175 0.02868 = 0.03189 -0.00956 0.00005 -0.02056 AFIX 43 H45 2 0.043562 0.136621 0.891783 11.00000 -1.20000 AFIX 0 C46 1 0.129948 0.222146 0.870915 11.00000 0.03234 0.02704 = 0.01966 -0.00844 0.00046 -0.01017 C47 1 -0.013460 0.467799 0.795787 11.00000 0.01593 0.03284 = 0.02474 -0.00056 -0.00522 -0.00625 AFIX 13 H47 2 0.062008 0.475352 0.783219 11.00000 -1.20000 AFIX 0 C48 1 -0.072406 0.519815 0.861168 11.00000 0.07118 0.03001 = 0.03627 -0.00539 0.00642 -0.00918 AFIX 137 H48A 2 -0.082243 0.580489 0.842300 11.00000 -1.50000 H48B 2 -0.026069 0.499154 0.906852 11.00000 -1.50000 H48C 2 -0.146135 0.512654 0.875648 11.00000 -1.50000 AFIX 0 C49 1 -0.081533 0.505346 0.721071 11.00000 0.04709 0.04785 = 0.04617 0.00813 -0.01871 -0.01480 AFIX 137 H49A 2 -0.157668 0.501973 0.732387 11.00000 -1.50000 H49B 2 -0.044101 0.472538 0.679784 11.00000 -1.50000 H49C 2 -0.085839 0.565249 0.703838 11.00000 -1.50000 AFIX 0 C50 1 0.246966 0.155460 0.890574 11.00000 0.02974 0.02031 = 0.04401 -0.00463 -0.00964 -0.01152 AFIX 13 H50 2 0.299162 0.187517 0.894266 11.00000 -1.20000 AFIX 0 C51 1 0.295340 0.101873 0.824249 11.00000 0.03422 0.02758 = 0.05123 -0.00500 -0.00801 -0.00636 AFIX 137 H51A 2 0.371989 0.063917 0.835659 11.00000 -1.50000 H51B 2 0.296686 0.140441 0.774460 11.00000 -1.50000 H51C 2 0.247752 0.067577 0.820940 11.00000 -1.50000 AFIX 0 C52 1 0.244659 0.094904 0.970503 11.00000 0.05912 0.03024 = 0.04388 0.00085 -0.01992 -0.01184 AFIX 137 H52A 2 0.202017 0.057272 0.966460 11.00000 -1.50000 H52B 2 0.208701 0.129222 1.011015 11.00000 -1.50000 H52C 2 0.321812 0.060232 0.984168 11.00000 -1.50000 AFIX 0 C53 1 0.539154 0.339507 0.719837 11.00000 0.01531 0.03041 = 0.01642 -0.00793 -0.00303 -0.00793 C54 1 0.569298 0.410542 0.675004 11.00000 0.02247 0.03358 = 0.02218 -0.00600 0.00414 -0.01012 C55 1 0.664342 0.394025 0.623142 11.00000 0.03187 0.04006 = 0.03460 -0.00523 0.00699 -0.01536 AFIX 43 H55 2 0.684725 0.440441 0.592858 11.00000 -1.20000 AFIX 0 C56 1 0.729818 0.309539 0.615455 11.00000 0.02208 0.06077 = 0.03392 -0.01638 0.01203 -0.01107 AFIX 43 H56 2 0.794544 0.299397 0.580885 11.00000 -1.20000 AFIX 0 C57 1 0.699471 0.240488 0.658792 11.00000 0.03190 0.03839 = 0.03467 -0.01934 -0.00098 -0.00099 AFIX 43 H57 2 0.744355 0.183946 0.653025 11.00000 -1.20000 AFIX 0 C58 1 0.603734 0.252912 0.710864 11.00000 0.02069 0.02904 = 0.01990 -0.00926 -0.00539 -0.00218 C59 1 0.496337 0.504897 0.678576 11.00000 0.03558 0.03056 = 0.03775 -0.00230 0.01271 -0.01275 AFIX 13 H59 2 0.437480 0.504462 0.721735 11.00000 -1.20000 AFIX 0 C60 1 0.566523 0.559269 0.695891 11.00000 0.06112 0.04363 = 0.03828 -0.01053 0.00587 -0.02208 AFIX 137 H60A 2 0.611632 0.528700 0.741253 11.00000 -1.50000 H60B 2 0.515422 0.614595 0.706795 11.00000 -1.50000 H60C 2 0.616433 0.568536 0.650460 11.00000 -1.50000 AFIX 0 C61 1 0.435902 0.547660 0.601472 11.00000 0.04003 0.03411 = 0.07718 0.00198 -0.01284 -0.01365 AFIX 137 H61A 2 0.491377 0.555488 0.559407 11.00000 -1.50000 H61B 2 0.380958 0.603432 0.607635 11.00000 -1.50000 H61C 2 0.397105 0.511138 0.588553 11.00000 -1.50000 AFIX 0 C62 1 0.568654 0.176391 0.756418 11.00000 0.01954 0.02417 = 0.03136 -0.01291 -0.00322 0.00334 AFIX 13 H62 2 0.484542 0.195253 0.758430 11.00000 -1.20000 AFIX 0 C63 1 0.611861 0.096204 0.716100 11.00000 0.05985 0.03248 = 0.03644 -0.01352 -0.00937 -0.00907 AFIX 137 H63A 2 0.694028 0.072478 0.717491 11.00000 -1.50000 H63B 2 0.590021 0.112629 0.661766 11.00000 -1.50000 H63C 2 0.578715 0.053060 0.743677 11.00000 -1.50000 AFIX 0 C64 1 0.605365 0.148725 0.842386 11.00000 0.04410 0.02910 = 0.03605 -0.01050 -0.00175 -0.00440 AFIX 137 H64A 2 0.584345 0.098351 0.866995 11.00000 -1.50000 H64B 2 0.567753 0.195669 0.871203 11.00000 -1.50000 H64C 2 0.687076 0.134760 0.843010 11.00000 -1.50000 AFIX 0 C65 1 0.255650 0.339036 0.603112 11.00000 0.01772 0.02878 = 0.02322 0.00069 0.00090 -0.01359 C66 1 0.171125 0.492363 0.579881 11.00000 0.01896 0.02854 = 0.02483 0.00159 0.00166 -0.00886 C67 1 0.145567 0.491242 0.504628 11.00000 0.03161 0.04039 = 0.02422 0.01069 -0.00762 -0.01438 AFIX 43 H67 2 0.108375 0.542996 0.471369 11.00000 -1.20000 AFIX 0 C68 1 0.175989 0.411584 0.478522 11.00000 0.03207 0.05303 = 0.01804 -0.00392 -0.00755 -0.01483 AFIX 43 H68 2 0.158483 0.410503 0.427547 11.00000 -1.20000 AFIX 0 C69 1 0.230882 0.335343 0.526355 11.00000 0.03488 0.03505 = 0.01736 -0.00369 -0.00517 -0.01547 AFIX 43 H69 2 0.251409 0.282290 0.508693 11.00000 -1.20000 AFIX 0 C70 1 0.140424 0.575325 0.612273 11.00000 0.04068 0.02676 = 0.04286 -0.00027 0.00069 -0.00715 AFIX 137 H70A 2 0.147012 0.561854 0.668974 11.00000 -1.50000 H70B 2 0.062906 0.610503 0.600048 11.00000 -1.50000 H70C 2 0.191670 0.606804 0.588563 11.00000 -1.50000 AFIX 0 N4 3 0.211563 0.341446 0.837285 11.00000 0.01474 0.01868 = 0.01608 -0.00113 -0.00370 -0.00420 N5 3 0.438351 0.353720 0.772204 11.00000 0.01548 0.01526 = 0.01728 -0.00405 -0.00065 -0.00309 N6 3 0.225787 0.416863 0.628121 11.00000 0.01787 0.02643 = 0.01499 -0.00215 -0.00433 -0.00849 O2 4 0.307532 0.272168 0.655564 11.00000 0.02851 0.02119 = 0.01759 -0.00395 -0.00529 -0.00567 ZN2 5 0.297330 0.350338 0.735822 11.00000 0.02008 0.02376 = 0.01409 -0.00383 -0.00278 -0.00564 HKLF 5 REM db39b_reprocess_twin1_hklf4_a.res in P-1 REM wR2 = 0.1010, GooF = S = 0.915, Restrained GooF = 0.915 for all data REM R1 = 0.0503 for 11599 Fo > 4sig(Fo) and 0.0960 for all 19098 data REM 744 parameters refined using 30 restraints END WGHT 0.0457 0.0000 REM Highest difference peak 0.626, deepest hole -0.506, 1-sigma level 0.081 Q1 1 0.2052 0.3734 0.7340 11.00000 0.05 0.63 Q2 1 0.3766 0.3378 0.7571 11.00000 0.05 0.61 Q3 1 0.2987 0.8442 0.6783 11.00000 0.05 0.58 Q4 1 0.1623 0.8993 0.7229 11.00000 0.05 0.57 Q5 1 0.2477 0.3738 0.7859 11.00000 0.05 0.56 Q6 1 0.3372 0.8367 0.7354 11.00000 0.05 0.55 Q7 1 0.2699 0.3291 0.7979 11.00000 0.05 0.53 Q8 1 0.2564 0.3999 0.6793 11.00000 0.05 0.52 Q9 1 0.2896 0.8270 0.7873 11.00000 0.05 0.44 Q10 1 -0.1649 0.8532 0.7329 11.00000 0.05 0.42 ; _shelx_res_checksum 37540 _olex2_exptl_crystal_mounting_method 'The crystal was mounted on MITEGEN holder in oil' _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.260 _oxdiff_exptl_absorpt_empirical_full_min 0.795 _oxdiff_twin_integration_method simultaneous _oxdiff_twin_items 2 loop_ _twin_individual_id _twin_individual_mass_fraction_refined _oxdiff_twin_reflns_isolated _oxdiff_twin_reflns_overlapped _twin_individual_twin_lattice_type _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 1 0.8736 19416 64841 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 2 0.1264 19319 64841 nmt 1.0008 -0.4949 -0.0722 0.0035 -1.0005 -0.0008 -0.0100 0.0040 -0.9992 _twin_special_details ; Component 2 rotated by 179.9192\% around [1.00 0.00 -0.00] (reciprocal) or [0.97 -0.24 -0.03] (direct) ; ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_db8-8_reprocessed _database_code_depnum_ccdc_archive 'CCDC 2285020' loop_ _audit_author_name _audit_author_address 'Marina Uzelac' ;University of Edinburgh United Kingdom ; _audit_update_record ; 2023-07-27 deposited with the CCDC. 2023-11-13 downloaded from the CCDC. ; _audit_creation_date 2021-12-08 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C34 H45 N3 O Zn, 0.5(C H2 Cl2)' _chemical_formula_sum 'C34.50 H46 Cl N3 O Zn' _chemical_formula_weight 619.56 _chemical_melting_point ? _chemical_oxdiff_formula 'Zn1 N3 O1 C34 H46' _chemical_oxdiff_usercomment '@ 120 K ' 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' 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' _cell_length_a 13.2654(6) _cell_length_b 16.8069(3) _cell_length_c 21.0819(11) _cell_angle_alpha 90 _cell_angle_beta 135.126(9) _cell_angle_gamma 90 _cell_volume 3316.2(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 23702 _cell_measurement_temperature 120.01(11) _cell_measurement_theta_max 28.9070 _cell_measurement_theta_min 3.4570 _shelx_estimated_absorpt_T_max 0.927 _shelx_estimated_absorpt_T_min 0.706 _exptl_absorpt_coefficient_mu 0.851 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.82761 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.241 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 1316 _exptl_crystal_size_max 0.439 _exptl_crystal_size_mid 0.158 _exptl_crystal_size_min 0.09 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_unetI/netI 0.0300 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.904 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 72427 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.904 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.535 _diffrn_reflns_theta_min 3.320 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 120.01(11) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.0521 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.904 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -69.00 0.00 1.00 25.00 -- -15.82 124.00 168.00 69 2 \w -83.00 -14.00 1.00 25.00 -- -15.82 148.00 -26.00 69 3 \w 14.00 85.00 1.00 25.00 -- 17.54-148.00 -74.00 71 4 \w 0.00 70.00 1.00 25.00 -- 17.54-124.00 89.00 70 5 \w -88.00 -39.00 1.00 25.00 -- -15.82-178.00-150.00 49 6 \w -85.00 3.00 1.00 25.00 -- -15.82 -38.00 150.00 88 7 \w -35.00 53.00 1.00 25.00 -- -15.82 38.00 -30.00 88 8 \w -33.00 51.00 1.00 25.00 -- -15.82 57.00 -90.00 84 9 \w -9.00 39.00 1.00 25.00 -- 17.54 77.00-180.00 48 10 \w -9.00 39.00 1.00 25.00 -- 17.54 77.00 -30.00 48 11 \w -9.00 39.00 1.00 25.00 -- 17.54 77.00 150.00 48 12 \w -33.00 51.00 1.00 25.00 -- -15.82 57.00 120.00 84 13 \w -39.00 11.00 1.00 25.00 -- -15.82 -77.00-150.00 50 14 \w -9.00 20.00 1.00 25.00 -- 17.54 77.00 120.00 29 15 \w 1.00 85.00 1.00 25.00 -- 17.54 57.00 30.00 84 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0445632000 _diffrn_orient_matrix_UB_12 -0.0265418000 _diffrn_orient_matrix_UB_13 0.0370152000 _diffrn_orient_matrix_UB_21 0.0301785000 _diffrn_orient_matrix_UB_22 0.0326000000 _diffrn_orient_matrix_UB_23 0.0300909000 _diffrn_orient_matrix_UB_31 -0.0533769000 _diffrn_orient_matrix_UB_32 -0.0037062000 _diffrn_orient_matrix_UB_33 -0.0001161000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 6909 _reflns_number_total 8388 _reflns_odcompleteness_completeness 99.70 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _refine_diff_density_max 0.594 _refine_diff_density_min -0.483 _refine_diff_density_rms 0.056 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 411 _refine_ls_number_reflns 8388 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0326 _refine_ls_restrained_S_all 1.031 _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^)+(0.0339P)^2^+1.8135P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0735 _refine_ls_wR_factor_ref 0.0795 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances Zn1-O1 \\sim Zn1-O1A with sigma of 0.02 N3-C31 \\sim N3A-C31A with sigma of 0.02 N3-C30 \\sim N3A-C30A with sigma of 0.02 C31-C32 \\sim C31A-C32A with sigma of 0.02 C33-C34 \\sim C33A-C34A with sigma of 0.02 C33-C32 \\sim C33A-C32A with sigma of 0.02 C30-C34 \\sim C30A-C34A with sigma of 0.02 C30-O1 \\sim C30A-O1A with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(O1A) = Uanis(O1) Uanis(N3A) = Uanis(N3) Uanis(C34) = Uanis(C34A) Uanis(C33) = Uanis(C33A) Uanis(C32) = Uanis(C32A) Uanis(C31) = Uanis(C31A) Uanis(C30) = Uanis(C30A) 4. Others Sof(C30A)=Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33A)= Sof(C34A)=Sof(H34A)=Sof(N3A)=Sof(O1A)=1-FVAR(1) Sof(C30)=Sof(C31)=Sof(H31)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=Sof(C34)= Sof(H34)=Sof(N3)=Sof(O1)=FVAR(1) Fixed Sof: C35(0.5) H35A(0.5) H35B(0.5) Cl1(0.5) Cl1A(0.5) 5.a Ternary CH refined with riding coordinates: C10(H10), C13(H13), C22(H22), C25(H25) 5.b Secondary CH2 refined with riding coordinates: C35(H35A,H35B) 5.c Aromatic/amide H refined with riding coordinates: C2(H2), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20), C31(H31), C31A(H31A), C32(H32), C32A(H32A), C33(H33), C33A(H33A), C34(H34), C34A(H34A) 5.d Idealised Me refined as rotating group: C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B, H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A, H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 0.75254(16) 0.28024(9) 0.70529(10) 0.0169(3) Uani 1 1 d . . . . . C2 C 0.66086(16) 0.26827(9) 0.71660(10) 0.0184(3) Uani 1 1 d . . . . . H2 H 0.660412 0.216912 0.732808 0.022 Uiso 1 1 calc R U . . . C3 C 0.56982(16) 0.32251(9) 0.70700(10) 0.0168(3) Uani 1 1 d . . . . . C4 C 0.86530(16) 0.36002(9) 0.67596(11) 0.0182(3) Uani 1 1 d . . . . . C5 C 0.98144(17) 0.40703(10) 0.74789(11) 0.0224(3) Uani 1 1 d . . . . . C6 C 1.08998(18) 0.42275(11) 0.75246(13) 0.0304(4) Uani 1 1 d . . . . . H6 H 1.167829 0.453487 0.799474 0.036 Uiso 1 1 calc R U . . . C7 C 1.08395(19) 0.39362(12) 0.68869(14) 0.0348(5) Uani 1 1 d . . . . . H7 H 1.158398 0.403603 0.693778 0.042 Uiso 1 1 calc R U . . . C8 C 0.96787(19) 0.34981(11) 0.61762(13) 0.0307(4) Uani 1 1 d . . . . . H8 H 0.963953 0.331322 0.574329 0.037 Uiso 1 1 calc R U . . . C9 C 0.85572(18) 0.33247(10) 0.60898(11) 0.0230(3) Uani 1 1 d . . . . . C10 C 0.98762(18) 0.44032(11) 0.81744(12) 0.0263(4) Uani 1 1 d . . . . . H10 H 0.889431 0.453008 0.786251 0.032 Uiso 1 1 calc R U . . . C11 C 1.0454(2) 0.37999(13) 0.89119(13) 0.0381(5) Uani 1 1 d . . . . . H11A H 1.139848 0.363946 0.921072 0.057 Uiso 1 1 calc R U . . . H11B H 0.983890 0.334278 0.864802 0.057 Uiso 1 1 calc R U . . . H11C H 1.048525 0.403912 0.933928 0.057 Uiso 1 1 calc R U . . . C12 C 1.0742(2) 0.51699(12) 0.86096(15) 0.0417(5) Uani 1 1 d . . . . . H12A H 1.173957 0.505081 0.900664 0.063 Uiso 1 1 calc R U . . . H12B H 1.058194 0.541061 0.894492 0.063 Uiso 1 1 calc R U . . . H12C H 1.044991 0.553076 0.815096 0.063 Uiso 1 1 calc R U . . . C13 C 0.72572(19) 0.28842(10) 0.52686(12) 0.0254(4) Uani 1 1 d . . . . . H13 H 0.666644 0.274493 0.537255 0.031 Uiso 1 1 calc R U . . . C14 C 0.6371(2) 0.34315(12) 0.44436(12) 0.0315(4) Uani 1 1 d . . . . . H14A H 0.616045 0.391678 0.457114 0.047 Uiso 1 1 calc R U . . . H14B H 0.549435 0.317019 0.394058 0.047 Uiso 1 1 calc R U . . . H14C H 0.690270 0.354979 0.430314 0.047 Uiso 1 1 calc R U . . . C15 C 0.7629(3) 0.21113(13) 0.50862(16) 0.0456(5) Uani 1 1 d . . . . . H15A H 0.816725 0.223324 0.495062 0.068 Uiso 1 1 calc R U . . . H15B H 0.676556 0.183982 0.458510 0.068 Uiso 1 1 calc R U . . . H15C H 0.818876 0.177664 0.560857 0.068 Uiso 1 1 calc R U . . . C16 C 0.45269(16) 0.44648(9) 0.67240(10) 0.0162(3) Uani 1 1 d . . . . . C17 C 0.30274(17) 0.44054(9) 0.60641(11) 0.0182(3) Uani 1 1 d . . . . . C18 C 0.22679(18) 0.49112(10) 0.61298(12) 0.0238(3) Uani 1 1 d . . . . . H18 H 0.127610 0.488043 0.569893 0.029 Uiso 1 1 calc R U . . . C19 C 0.29584(19) 0.54548(10) 0.68198(12) 0.0267(4) Uani 1 1 d . . . . . H19 H 0.243602 0.577161 0.686447 0.032 Uiso 1 1 calc R U . . . C20 C 0.44306(19) 0.55284(10) 0.74463(12) 0.0247(3) Uani 1 1 d . . . . . H20 H 0.488804 0.590504 0.790169 0.030 Uiso 1 1 calc R U . . . C21 C 0.52363(17) 0.50461(9) 0.74041(11) 0.0188(3) Uani 1 1 d . . . . . C22 C 0.22148(16) 0.38396(10) 0.52725(11) 0.0204(3) Uani 1 1 d . . . . . H22 H 0.291091 0.348833 0.537766 0.025 Uiso 1 1 calc R U . . . C23 C 0.11437(19) 0.33166(11) 0.51549(13) 0.0294(4) Uani 1 1 d . . . . . H23A H 0.039561 0.364386 0.499156 0.044 Uiso 1 1 calc R U . . . H23B H 0.162472 0.304699 0.570928 0.044 Uiso 1 1 calc R U . . . H23C H 0.074062 0.293178 0.469018 0.044 Uiso 1 1 calc R U . . . C24 C 0.14403(18) 0.43061(11) 0.44076(12) 0.0268(4) Uani 1 1 d . . . . . H24A H 0.068259 0.461275 0.425541 0.040 Uiso 1 1 calc R U . . . H24B H 0.104903 0.394201 0.392834 0.040 Uiso 1 1 calc R U . . . H24C H 0.210311 0.465641 0.449636 0.040 Uiso 1 1 calc R U . . . C25 C 0.68557(18) 0.51409(10) 0.80896(11) 0.0242(3) Uani 1 1 d . . . . . H25 H 0.714591 0.499903 0.778692 0.029 Uiso 1 1 calc R U . . . C26 C 0.7355(2) 0.59954(11) 0.84317(13) 0.0309(4) Uani 1 1 d . . . . . H26A H 0.682093 0.635318 0.792939 0.046 Uiso 1 1 calc R U . . . H26B H 0.835305 0.603920 0.877885 0.046 Uiso 1 1 calc R U . . . H26C H 0.720229 0.612953 0.880123 0.046 Uiso 1 1 calc R U . . . C27 C 0.7624(2) 0.45731(12) 0.88838(13) 0.0372(4) Uani 1 1 d . . . . . H27A H 0.742632 0.403360 0.867443 0.056 Uiso 1 1 calc R U . . . H27B H 0.729347 0.466179 0.916170 0.056 Uiso 1 1 calc R U . . . H27C H 0.863464 0.466699 0.931430 0.056 Uiso 1 1 calc R U . . . C28 C 0.85573(18) 0.21369(10) 0.73606(12) 0.0248(4) Uani 1 1 d . . . . . H28A H 0.828627 0.189077 0.684677 0.037 Uiso 1 1 calc R U . . . H28B H 0.853483 0.174833 0.768417 0.037 Uiso 1 1 calc R U . . . H28C H 0.950587 0.234906 0.774601 0.037 Uiso 1 1 calc R U . . . C29 C 0.50811(19) 0.29413(10) 0.74199(12) 0.0238(3) Uani 1 1 d . . . . . H29A H 0.517225 0.335461 0.777218 0.036 Uiso 1 1 calc R U . . . H29B H 0.559029 0.247747 0.778674 0.036 Uiso 1 1 calc R U . . . H29C H 0.408990 0.281190 0.692230 0.036 Uiso 1 1 calc R U . . . C30 C 0.6560(7) 0.5915(2) 0.5998(4) 0.0171(8) Uani 0.878(17) 1 d D . P A 1 C30A C 0.653(6) 0.5984(14) 0.608(3) 0.0171(8) Uani 0.122(17) 1 d D . P A 2 C31 C 0.5973(6) 0.7134(3) 0.5268(4) 0.0199(7) Uani 0.878(17) 1 d D . P A 1 H31 H 0.543731 0.741497 0.473257 0.024 Uiso 0.878(17) 1 calc R U P A 1 C31A C 0.587(5) 0.717(3) 0.534(3) 0.0199(7) Uani 0.122(17) 1 d D . P A 2 H31A H 0.524430 0.744927 0.479493 0.024 Uiso 0.122(17) 1 calc R U P A 2 C32 C 0.6944(5) 0.7541(3) 0.6060(3) 0.0292(9) Uani 0.878(17) 1 d D . P A 1 H32 H 0.705696 0.808732 0.606111 0.035 Uiso 0.878(17) 1 calc R U P A 1 C32A C 0.679(4) 0.761(2) 0.609(2) 0.0292(9) Uani 0.122(17) 1 d D . P A 2 H32A H 0.693115 0.815534 0.612020 0.035 Uiso 0.122(17) 1 calc R U P A 2 C33 C 0.7767(5) 0.7124(3) 0.6870(3) 0.0289(7) Uani 0.878(17) 1 d D . P A 1 H33 H 0.844974 0.738161 0.742067 0.035 Uiso 0.878(17) 1 calc R U P A 1 C33A C 0.748(4) 0.711(2) 0.683(3) 0.0289(7) Uani 0.122(17) 1 d D . P A 2 H33A H 0.787700 0.737651 0.735677 0.035 Uiso 0.122(17) 1 calc R U P A 2 C34 C 0.7535(9) 0.6325(3) 0.6826(4) 0.0252(7) Uani 0.878(17) 1 d D . P A 1 H34 H 0.803203 0.604323 0.735683 0.030 Uiso 0.878(17) 1 calc R U P A 1 C34A C 0.768(7) 0.631(2) 0.693(3) 0.0252(7) Uani 0.122(17) 1 d D . P A 2 H34A H 0.843057 0.603315 0.745455 0.030 Uiso 0.122(17) 1 calc R U P A 2 N1 N 0.75138(13) 0.34552(7) 0.66959(8) 0.0148(2) Uani 1 1 d . . . . . N2 N 0.53593(13) 0.39424(7) 0.67003(8) 0.0146(2) Uani 1 1 d . . . . . N3 N 0.5753(17) 0.6340(4) 0.5225(5) 0.0152(8) Uani 0.878(17) 1 d D . P A 1 N3A N 0.578(13) 0.636(3) 0.528(4) 0.0152(8) Uani 0.122(17) 1 d D . P A 2 O1 O 0.6451(4) 0.51560(15) 0.59468(17) 0.0284(7) Uani 0.878(17) 1 d D . P A 1 O1A O 0.620(2) 0.5249(9) 0.6022(14) 0.0284(7) Uani 0.122(17) 1 d D . P A 2 Zn1 Zn 0.58121(2) 0.41714(2) 0.59970(2) 0.01280(5) Uani 1 1 d D . . . . C35 C 0.5007(5) -0.0286(4) 0.5541(4) 0.077(2) Uani 0.5 1 d . . P B -1 H35A H 0.419579 -0.038796 0.545428 0.093 Uiso 0.5 1 calc R U P B -1 H35B H 0.583065 -0.055538 0.608685 0.093 Uiso 0.5 1 calc R U P B -1 Cl1 Cl 0.5312(6) 0.0659(3) 0.5654(3) 0.0973(11) Uani 0.5 1 d . . P B -1 Cl1A Cl 0.4635(4) -0.0691(2) 0.4579(3) 0.1028(12) Uani 0.5 1 d . . P B -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0169(7) 0.0152(7) 0.0140(7) 0.0033(5) 0.0094(6) 0.0024(5) C2 0.0213(8) 0.0132(7) 0.0207(8) 0.0052(6) 0.0149(7) 0.0020(6) C3 0.0176(7) 0.0178(7) 0.0141(7) 0.0007(6) 0.0109(7) -0.0026(6) C4 0.0164(7) 0.0179(7) 0.0211(8) 0.0079(6) 0.0135(7) 0.0055(6) C5 0.0163(7) 0.0218(8) 0.0229(8) 0.0095(6) 0.0116(7) 0.0049(6) C6 0.0167(8) 0.0313(10) 0.0339(10) 0.0139(8) 0.0147(8) 0.0041(7) C7 0.0246(9) 0.0428(11) 0.0461(12) 0.0241(9) 0.0282(10) 0.0129(8) C8 0.0315(10) 0.0387(10) 0.0359(10) 0.0184(8) 0.0288(9) 0.0161(8) C9 0.0247(8) 0.0232(8) 0.0253(9) 0.0119(7) 0.0192(8) 0.0109(6) C10 0.0162(8) 0.0280(9) 0.0226(9) -0.0015(7) 0.0094(7) -0.0016(6) C11 0.0402(11) 0.0425(12) 0.0261(10) 0.0021(8) 0.0216(10) 0.0011(9) C12 0.0277(10) 0.0380(11) 0.0365(12) -0.0089(9) 0.0147(10) -0.0084(8) C13 0.0335(9) 0.0252(9) 0.0256(9) 0.0039(7) 0.0238(8) 0.0070(7) C14 0.0323(10) 0.0392(11) 0.0254(9) 0.0067(8) 0.0213(9) 0.0059(8) C15 0.0631(15) 0.0353(11) 0.0473(13) -0.0001(9) 0.0423(13) 0.0133(10) C16 0.0202(7) 0.0158(7) 0.0174(8) 0.0027(6) 0.0150(7) 0.0010(6) C17 0.0208(8) 0.0174(7) 0.0205(8) -0.0003(6) 0.0161(7) -0.0010(6) C18 0.0225(8) 0.0244(8) 0.0309(9) -0.0001(7) 0.0211(8) 0.0016(6) C19 0.0316(9) 0.0244(9) 0.0366(10) -0.0030(7) 0.0285(9) 0.0023(7) C20 0.0317(9) 0.0221(8) 0.0259(9) -0.0056(7) 0.0224(8) -0.0022(7) C21 0.0217(8) 0.0188(8) 0.0184(8) 0.0006(6) 0.0150(7) -0.0003(6) C22 0.0172(7) 0.0228(8) 0.0225(8) -0.0032(6) 0.0145(7) -0.0015(6) C23 0.0290(9) 0.0298(9) 0.0354(10) -0.0072(8) 0.0249(9) -0.0077(7) C24 0.0219(8) 0.0337(10) 0.0223(9) -0.0020(7) 0.0148(8) -0.0019(7) C25 0.0232(8) 0.0261(9) 0.0216(9) -0.0052(7) 0.0153(8) -0.0031(7) C26 0.0295(9) 0.0313(10) 0.0283(10) -0.0102(7) 0.0192(9) -0.0085(7) C27 0.0292(10) 0.0375(11) 0.0241(10) 0.0015(8) 0.0116(9) -0.0001(8) C28 0.0260(9) 0.0196(8) 0.0305(9) 0.0106(7) 0.0206(8) 0.0089(6) C29 0.0301(9) 0.0217(8) 0.0283(9) 0.0072(7) 0.0238(8) 0.0028(7) C30 0.0175(8) 0.0171(10) 0.0190(15) 0.0013(8) 0.0137(9) -0.0004(9) C30A 0.0175(8) 0.0171(10) 0.0190(15) 0.0013(8) 0.0137(9) -0.0004(9) C31 0.0225(12) 0.0168(10) 0.0204(13) 0.0023(8) 0.0152(8) 0.0003(8) C31A 0.0225(12) 0.0168(10) 0.0204(13) 0.0023(8) 0.0152(8) 0.0003(8) C32 0.0306(16) 0.0145(13) 0.0320(11) -0.0056(9) 0.0185(10) -0.0047(10) C32A 0.0306(16) 0.0145(13) 0.0320(11) -0.0056(9) 0.0185(10) -0.0047(10) C33 0.0212(18) 0.0320(10) 0.0201(10) -0.0108(8) 0.0100(14) -0.0062(13) C33A 0.0212(18) 0.0320(10) 0.0201(10) -0.0108(8) 0.0100(14) -0.0062(13) C34 0.021(2) 0.0329(10) 0.013(2) 0.0042(10) 0.0088(17) 0.0019(10) C34A 0.021(2) 0.0329(10) 0.013(2) 0.0042(10) 0.0088(17) 0.0019(10) N1 0.0139(6) 0.0159(6) 0.0142(6) 0.0021(5) 0.0098(5) 0.0018(5) N2 0.0154(6) 0.0147(6) 0.0145(6) 0.0011(5) 0.0108(6) 0.0015(5) N3 0.0152(8) 0.0149(8) 0.0138(13) -0.0009(8) 0.0097(15) -0.0019(8) N3A 0.0152(8) 0.0149(8) 0.0138(13) -0.0009(8) 0.0097(15) -0.0019(8) O1 0.0296(10) 0.0153(7) 0.0430(9) 0.0060(6) 0.0267(8) -0.0006(7) O1A 0.0296(10) 0.0153(7) 0.0430(9) 0.0060(6) 0.0267(8) -0.0006(7) Zn1 0.01366(9) 0.01165(9) 0.01251(9) 0.00190(6) 0.00907(8) 0.00088(6) C35 0.020(2) 0.090(4) 0.082(4) 0.033(4) 0.022(3) 0.010(2) Cl1 0.123(2) 0.101(2) 0.0915(16) 0.0147(12) 0.0845(17) 0.0115(15) Cl1A 0.0642(13) 0.0558(13) 0.136(3) 0.0032(16) 0.052(2) 0.0144(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C2 1.410(2) . ? C1 C28 1.512(2) . ? C1 N1 1.3243(19) . ? C2 H2 0.9300 . ? C2 C3 1.409(2) . ? C3 C29 1.516(2) . ? C3 N2 1.3289(19) . ? C4 C5 1.409(2) . ? C4 C9 1.404(2) . ? C4 N1 1.4400(18) . ? C5 C6 1.399(2) . ? C5 C10 1.516(2) . ? C6 H6 0.9300 . ? C6 C7 1.379(3) . ? C7 H7 0.9300 . ? C7 C8 1.374(3) . ? C8 H8 0.9300 . ? C8 C9 1.396(2) . ? C9 C13 1.513(3) . ? C10 H10 0.9800 . ? C10 C11 1.531(3) . ? C10 C12 1.526(3) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13 0.9800 . ? C13 C14 1.535(2) . ? C13 C15 1.532(2) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.407(2) . ? C16 C21 1.408(2) . ? C16 N2 1.4392(19) . ? C17 C18 1.398(2) . ? C17 C22 1.517(2) . ? C18 H18 0.9300 . ? C18 C19 1.379(2) . ? C19 H19 0.9300 . ? C19 C20 1.385(2) . ? C20 H20 0.9300 . ? C20 C21 1.394(2) . ? C21 C25 1.526(2) . ? C22 H22 0.9800 . ? C22 C23 1.534(2) . ? C22 C24 1.530(2) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25 0.9800 . ? C25 C26 1.531(2) . ? C25 C27 1.528(3) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 C34 1.413(4) . ? C30 N3 1.356(3) . ? C30 O1 1.280(3) . ? C30A C34A 1.401(19) . ? C30A N3A 1.358(18) . ? C30A O1A 1.288(18) . ? C31 H31 0.9300 . ? C31 C32 1.367(3) . ? C31 N3 1.355(4) . ? C31A H31A 0.9300 . ? C31A C32A 1.351(18) . ? C31A N3A 1.359(18) . ? C32 H32 0.9300 . ? C32 C33 1.399(3) . ? C32A H32A 0.9300 . ? C32A C33A 1.394(18) . ? C33 H33 0.9300 . ? C33 C34 1.365(5) . ? C33A H33A 0.9300 . ? C33A C34A 1.364(19) . ? C34 H34 0.9300 . ? C34A H34A 0.9300 . ? N1 Zn1 2.0005(12) . ? N2 Zn1 1.9923(12) . ? N3 Zn1 2.026(9) 3_666 ? N3A Zn1 2.12(6) 3_666 ? O1 Zn1 1.8963(18) . ? O1A Zn1 1.874(12) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C35 Cl1 1.615(8) . ? C35 Cl1A 1.845(8) . ? 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 C2 C1 C28 116.69(13) . . ? N1 C1 C2 123.39(13) . . ? N1 C1 C28 119.92(14) . . ? C1 C2 H2 115.2 . . ? C3 C2 C1 129.64(14) . . ? C3 C2 H2 115.2 . . ? C2 C3 C29 115.47(13) . . ? N2 C3 C2 124.79(13) . . ? N2 C3 C29 119.74(13) . . ? C5 C4 N1 118.04(14) . . ? C9 C4 C5 121.20(14) . . ? C9 C4 N1 120.63(14) . . ? C4 C5 C10 121.07(14) . . ? C6 C5 C4 117.85(16) . . ? C6 C5 C10 121.08(16) . . ? C5 C6 H6 119.3 . . ? C7 C6 C5 121.35(18) . . ? C7 C6 H6 119.3 . . ? C6 C7 H7 120.0 . . ? C8 C7 C6 119.96(16) . . ? C8 C7 H7 120.0 . . ? C7 C8 H8 119.3 . . ? C7 C8 C9 121.43(17) . . ? C9 C8 H8 119.3 . . ? C4 C9 C13 122.00(14) . . ? C8 C9 C4 118.15(17) . . ? C8 C9 C13 119.79(16) . . ? C5 C10 H10 107.2 . . ? C5 C10 C11 112.51(15) . . ? C5 C10 C12 113.25(16) . . ? C11 C10 H10 107.2 . . ? C12 C10 H10 107.2 . . ? C12 C10 C11 109.09(16) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 H13 107.7 . . ? C9 C13 C14 109.90(15) . . ? C9 C13 C15 113.16(16) . . ? C14 C13 H13 107.7 . . ? C15 C13 H13 107.7 . . ? C15 C13 C14 110.37(15) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 120.82(14) . . ? C17 C16 N2 120.28(13) . . ? C21 C16 N2 118.88(13) . . ? C16 C17 C22 122.46(13) . . ? C18 C17 C16 118.16(15) . . ? C18 C17 C22 119.33(14) . . ? C17 C18 H18 119.3 . . ? C19 C18 C17 121.39(16) . . ? C19 C18 H18 119.3 . . ? C18 C19 H19 120.0 . . ? C18 C19 C20 119.92(15) . . ? C20 C19 H19 120.0 . . ? C19 C20 H20 119.5 . . ? C19 C20 C21 120.94(15) . . ? C21 C20 H20 119.5 . . ? C16 C21 C25 120.88(14) . . ? C20 C21 C16 118.62(15) . . ? C20 C21 C25 120.49(14) . . ? C17 C22 H22 107.9 . . ? C17 C22 C23 113.06(13) . . ? C17 C22 C24 110.09(14) . . ? C23 C22 H22 107.9 . . ? C24 C22 H22 107.9 . . ? C24 C22 C23 109.77(14) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 H25 107.3 . . ? C21 C25 C26 113.11(14) . . ? C21 C25 C27 111.75(14) . . ? C26 C25 H25 107.3 . . ? C27 C25 H25 107.3 . . ? C27 C25 C26 109.86(15) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C1 C28 H28A 109.5 . . ? C1 C28 H28B 109.5 . . ? C1 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C3 C29 H29A 109.5 . . ? C3 C29 H29B 109.5 . . ? C3 C29 H29C 109.5 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N3 C30 C34 118.7(5) . . ? O1 C30 C34 122.7(5) . . ? O1 C30 N3 118.5(4) . . ? N3A C30A C34A 125(4) . . ? O1A C30A C34A 119(4) . . ? O1A C30A N3A 115(4) . . ? C32 C31 H31 118.4 . . ? N3 C31 H31 118.4 . . ? N3 C31 C32 123.1(6) . . ? C32A C31A H31A 116.8 . . ? C32A C31A N3A 126(5) . . ? N3A C31A H31A 116.8 . . ? C31 C32 H32 120.5 . . ? C31 C32 C33 119.0(5) . . ? C33 C32 H32 120.5 . . ? C31A C32A H32A 125.5 . . ? C31A C32A C33A 109(4) . . ? C33A C32A H32A 125.5 . . ? C32 C33 H33 121.1 . . ? C34 C33 C32 117.8(5) . . ? C34 C33 H33 121.1 . . ? C32A C33A H33A 114.1 . . ? C34A C33A C32A 132(4) . . ? C34A C33A H33A 114.1 . . ? C30 C34 H34 119.1 . . ? C33 C34 C30 121.9(6) . . ? C33 C34 H34 119.1 . . ? C30A C34A H34A 127.1 . . ? C33A C34A C30A 106(4) . . ? C33A C34A H34A 127.0 . . ? C1 N1 C4 119.90(12) . . ? C1 N1 Zn1 118.01(10) . . ? C4 N1 Zn1 121.92(9) . . ? C3 N2 C16 118.82(12) . . ? C3 N2 Zn1 117.17(10) . . ? C16 N2 Zn1 123.46(9) . . ? C30 N3 Zn1 122.0(5) . 3_666 ? C31 N3 C30 119.3(7) . . ? C31 N3 Zn1 118.7(5) . 3_666 ? C30A N3A C31A 115(5) . . ? C30A N3A Zn1 125(4) . 3_666 ? C31A N3A Zn1 119(4) . 3_666 ? C30 O1 Zn1 153.3(4) . . ? C30A O1A Zn1 177(3) . . ? N1 Zn1 N3 106.6(4) . 3_666 ? N1 Zn1 N3A 105(3) . 3_666 ? N2 Zn1 N1 96.52(5) . . ? N2 Zn1 N3 106.7(5) . 3_666 ? N2 Zn1 N3A 108(4) . 3_666 ? N3 Zn1 N3A 2(5) 3_666 3_666 ? O1 Zn1 N1 104.50(14) . . ? O1 Zn1 N2 126.35(17) . . ? O1 Zn1 N3 113.3(3) . 3_666 ? O1 Zn1 N3A 112(2) . 3_666 ? O1A Zn1 N1 114.6(7) . . ? O1A Zn1 N2 112.9(9) . . ? H35A C35 H35B 108.0 . . ? Cl1 C35 H35A 109.3 . . ? Cl1 C35 H35B 109.3 . . ? Cl1 C35 Cl1A 111.6(4) . . ? Cl1A C35 H35A 109.3 . . ? Cl1A C35 H35B 109.3 . . ? 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 C1 C2 C3 C29 -168.37(16) . . . . ? C1 C2 C3 N2 11.9(3) . . . . ? C2 C1 N1 C4 168.07(15) . . . . ? C2 C1 N1 Zn1 -16.6(2) . . . . ? C2 C3 N2 C16 -174.07(14) . . . . ? C2 C3 N2 Zn1 14.1(2) . . . . ? C4 C5 C6 C7 0.2(2) . . . . ? C4 C5 C10 C11 82.92(19) . . . . ? C4 C5 C10 C12 -152.79(16) . . . . ? C4 C9 C13 C14 105.44(17) . . . . ? C4 C9 C13 C15 -130.67(17) . . . . ? C5 C4 C9 C8 2.9(2) . . . . ? C5 C4 C9 C13 -174.28(14) . . . . ? C5 C4 N1 C1 -94.13(17) . . . . ? C5 C4 N1 Zn1 90.70(15) . . . . ? C5 C6 C7 C8 1.6(3) . . . . ? C6 C5 C10 C11 -97.83(19) . . . . ? C6 C5 C10 C12 26.5(2) . . . . ? C6 C7 C8 C9 -1.3(3) . . . . ? C7 C8 C9 C4 -1.0(2) . . . . ? C7 C8 C9 C13 176.26(16) . . . . ? C8 C9 C13 C14 -71.68(19) . . . . ? C8 C9 C13 C15 52.2(2) . . . . ? C9 C4 C5 C6 -2.5(2) . . . . ? C9 C4 C5 C10 176.75(14) . . . . ? C9 C4 N1 C1 90.06(18) . . . . ? C9 C4 N1 Zn1 -85.11(16) . . . . ? C10 C5 C6 C7 -179.04(16) . . . . ? C16 C17 C18 C19 -0.1(2) . . . . ? C16 C17 C22 C23 129.01(16) . . . . ? C16 C17 C22 C24 -107.83(17) . . . . ? C16 C21 C25 C26 149.87(15) . . . . ? C16 C21 C25 C27 -85.52(19) . . . . ? C17 C16 C21 C20 4.2(2) . . . . ? C17 C16 C21 C25 -176.63(14) . . . . ? C17 C16 N2 C3 -84.39(18) . . . . ? C17 C16 N2 Zn1 86.84(16) . . . . ? C17 C18 C19 C20 2.5(3) . . . . ? C18 C17 C22 C23 -53.5(2) . . . . ? C18 C17 C22 C24 69.68(18) . . . . ? C18 C19 C20 C21 -1.6(3) . . . . ? C19 C20 C21 C16 -1.7(2) . . . . ? C19 C20 C21 C25 179.07(16) . . . . ? C20 C21 C25 C26 -30.9(2) . . . . ? C20 C21 C25 C27 93.68(19) . . . . ? C21 C16 C17 C18 -3.3(2) . . . . ? C21 C16 C17 C22 174.26(14) . . . . ? C21 C16 N2 C3 97.13(17) . . . . ? C21 C16 N2 Zn1 -91.64(15) . . . . ? C22 C17 C18 C19 -177.69(16) . . . . ? C28 C1 C2 C3 169.75(16) . . . . ? C28 C1 N1 C4 -12.1(2) . . . . ? C28 C1 N1 Zn1 163.23(12) . . . . ? C29 C3 N2 C16 6.2(2) . . . . ? C29 C3 N2 Zn1 -165.54(11) . . . . ? C30 O1 Zn1 N1 -136.0(7) . . . . ? C30 O1 Zn1 N2 -26.4(8) . . . . ? C30 O1 Zn1 N3 108.4(9) . . . 3_666 ? C31 C32 C33 C34 -1.2(8) . . . . ? C31A C32A C33A C34A 20(8) . . . . ? C32 C31 N3 C30 -2(2) . . . . ? C32 C31 N3 Zn1 176.1(6) . . . 3_666 ? C32 C33 C34 C30 3.6(13) . . . . ? C32A C31A N3A C30A 10(16) . . . . ? C32A C31A N3A Zn1 178(5) . . . 3_666 ? C32A C33A C34A C30A -28(10) . . . . ? C34 C30 N3 C31 5(2) . . . . ? C34 C30 N3 Zn1 -173.9(10) . . . 3_666 ? C34 C30 O1 Zn1 79.0(11) . . . . ? C34A C30A N3A C31A -20(16) . . . . ? C34A C30A N3A Zn1 173(7) . . . 3_666 ? N1 C1 C2 C3 -10.4(3) . . . . ? N1 C4 C5 C6 -178.31(13) . . . . ? N1 C4 C5 C10 1.0(2) . . . . ? N1 C4 C9 C8 178.57(14) . . . . ? N1 C4 C9 C13 1.4(2) . . . . ? N2 C16 C17 C18 178.28(14) . . . . ? N2 C16 C17 C22 -4.2(2) . . . . ? N2 C16 C21 C20 -177.37(14) . . . . ? N2 C16 C21 C25 1.8(2) . . . . ? N3 C30 C34 C33 -5.4(17) . . . . ? N3 C30 O1 Zn1 -104.1(11) . . . . ? N3 C31 C32 C33 0.6(11) . . . . ? N3A C30A C34A C33A 26(12) . . . . ? N3A C31A C32A C33A -9(10) . . . . ? O1 C30 C34 C33 171.5(8) . . . . ? O1 C30 N3 C31 -172.4(11) . . . . ? O1 C30 N3 Zn1 9.1(17) . . . 3_666 ? O1A C30A C34A C33A -159(5) . . . . ? O1A C30A N3A C31A 165(8) . . . . ? O1A C30A N3A Zn1 -2(13) . . . 3_666 ? _shelx_res_file ; TITL db8.8_reprocessed_a.res in P2(1)/c db8.8_reprocessed.res created by SHELXL-2018/3 at 12:59:46 on 08-Dec-2021 REM Old TITL db8.8_reprocessed_a.res in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.113, Rweak 0.005, Alpha 0.035 REM 0.524 for 246 systematic absences, Orientation as input REM Formula found by SHELXT: C31 O5 Zn CELL 0.71073 13.2654 16.8069 21.0819 90 135.126 90 ZERR 4 0.0006 0.0003 0.0011 0 0.009 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl N O Zn UNIT 138 184 4 12 4 4 SADI Zn1 O1 Zn1 O1A SADI N3 C31 N3A C31A SADI N3 C30 N3A C30A SADI C31 C32 C31A C32A SADI C33 C34 C33A C34A SADI C33 C32 C33A C32A SADI C30 C34 C30A C34A SADI C30 O1 C30A O1A EADP O1A O1 EADP N3A N3 EADP C34 C34A EADP C33 C33A EADP C32 C32A EADP C31 C31A EADP C30 C30A L.S. 20 0 0 PLAN 4 SIZE 0.09 0.158 0.439 CONF list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.033900 1.813500 FVAR 0.35065 0.87752 C1 1 0.752539 0.280241 0.705292 11.00000 0.01695 0.01521 = 0.01405 0.00332 0.00935 0.00238 C2 1 0.660855 0.268275 0.716596 11.00000 0.02129 0.01323 = 0.02074 0.00517 0.01492 0.00197 AFIX 43 H2 2 0.660412 0.216912 0.732808 11.00000 -1.20000 AFIX 0 C3 1 0.569815 0.322514 0.706996 11.00000 0.01761 0.01777 = 0.01406 0.00066 0.01093 -0.00259 C4 1 0.865302 0.360019 0.675965 11.00000 0.01636 0.01787 = 0.02110 0.00793 0.01354 0.00546 C5 1 0.981436 0.407033 0.747892 11.00000 0.01629 0.02175 = 0.02287 0.00947 0.01163 0.00493 C6 1 1.089984 0.422753 0.752462 11.00000 0.01672 0.03125 = 0.03392 0.01392 0.01468 0.00406 AFIX 43 H6 2 1.167829 0.453487 0.799474 11.00000 -1.20000 AFIX 0 C7 1 1.083950 0.393615 0.688691 11.00000 0.02464 0.04281 = 0.04605 0.02410 0.02825 0.01287 AFIX 43 H7 2 1.158398 0.403603 0.693778 11.00000 -1.20000 AFIX 0 C8 1 0.967867 0.349811 0.617617 11.00000 0.03152 0.03872 = 0.03594 0.01842 0.02885 0.01605 AFIX 43 H8 2 0.963953 0.331322 0.574329 11.00000 -1.20000 AFIX 0 C9 1 0.855722 0.332466 0.608983 11.00000 0.02474 0.02318 = 0.02528 0.01193 0.01921 0.01087 C10 1 0.987616 0.440321 0.817442 11.00000 0.01623 0.02796 = 0.02258 -0.00147 0.00945 -0.00161 AFIX 13 H10 2 0.889431 0.453008 0.786251 11.00000 -1.20000 AFIX 0 C11 1 1.045354 0.379988 0.891188 11.00000 0.04022 0.04249 = 0.02613 0.00205 0.02164 0.00112 AFIX 137 H11A 2 1.139848 0.363946 0.921072 11.00000 -1.50000 H11B 2 0.983890 0.334278 0.864802 11.00000 -1.50000 H11C 2 1.048525 0.403912 0.933928 11.00000 -1.50000 AFIX 0 C12 1 1.074218 0.516993 0.860958 11.00000 0.02766 0.03803 = 0.03650 -0.00888 0.01468 -0.00840 AFIX 137 H12A 2 1.173957 0.505081 0.900664 11.00000 -1.50000 H12B 2 1.058194 0.541061 0.894492 11.00000 -1.50000 H12C 2 1.044991 0.553076 0.815096 11.00000 -1.50000 AFIX 0 C13 1 0.725717 0.288420 0.526856 11.00000 0.03352 0.02518 = 0.02563 0.00392 0.02377 0.00699 AFIX 13 H13 2 0.666644 0.274493 0.537255 11.00000 -1.20000 AFIX 0 C14 1 0.637070 0.343146 0.444365 11.00000 0.03232 0.03922 = 0.02544 0.00673 0.02135 0.00592 AFIX 137 H14A 2 0.616045 0.391678 0.457114 11.00000 -1.50000 H14B 2 0.549435 0.317019 0.394058 11.00000 -1.50000 H14C 2 0.690270 0.354979 0.430314 11.00000 -1.50000 AFIX 0 C15 1 0.762945 0.211130 0.508618 11.00000 0.06312 0.03526 = 0.04727 -0.00009 0.04228 0.01333 AFIX 137 H15A 2 0.816725 0.223324 0.495062 11.00000 -1.50000 H15B 2 0.676556 0.183982 0.458510 11.00000 -1.50000 H15C 2 0.818876 0.177664 0.560857 11.00000 -1.50000 AFIX 0 C16 1 0.452685 0.446478 0.672405 11.00000 0.02016 0.01578 = 0.01741 0.00266 0.01499 0.00102 C17 1 0.302742 0.440538 0.606415 11.00000 0.02076 0.01739 = 0.02053 -0.00027 0.01608 -0.00102 C18 1 0.226789 0.491121 0.612976 11.00000 0.02250 0.02436 = 0.03087 -0.00013 0.02113 0.00158 AFIX 43 H18 2 0.127610 0.488043 0.569893 11.00000 -1.20000 AFIX 0 C19 1 0.295836 0.545480 0.681983 11.00000 0.03157 0.02441 = 0.03656 -0.00295 0.02854 0.00228 AFIX 43 H19 2 0.243602 0.577161 0.686447 11.00000 -1.20000 AFIX 0 C20 1 0.443056 0.552839 0.744633 11.00000 0.03171 0.02213 = 0.02594 -0.00559 0.02243 -0.00223 AFIX 43 H20 2 0.488804 0.590504 0.790169 11.00000 -1.20000 AFIX 0 C21 1 0.523634 0.504606 0.740414 11.00000 0.02166 0.01878 = 0.01842 0.00059 0.01505 -0.00033 C22 1 0.221476 0.383962 0.527251 11.00000 0.01724 0.02278 = 0.02248 -0.00319 0.01449 -0.00154 AFIX 13 H22 2 0.291091 0.348833 0.537766 11.00000 -1.20000 AFIX 0 C23 1 0.114373 0.331664 0.515488 11.00000 0.02902 0.02978 = 0.03541 -0.00716 0.02493 -0.00768 AFIX 137 H23A 2 0.039561 0.364386 0.499156 11.00000 -1.50000 H23B 2 0.162472 0.304699 0.570928 11.00000 -1.50000 H23C 2 0.074062 0.293178 0.469018 11.00000 -1.50000 AFIX 0 C24 1 0.144027 0.430613 0.440764 11.00000 0.02188 0.03370 = 0.02234 -0.00205 0.01475 -0.00194 AFIX 137 H24A 2 0.068259 0.461275 0.425541 11.00000 -1.50000 H24B 2 0.104903 0.394201 0.392834 11.00000 -1.50000 H24C 2 0.210311 0.465641 0.449636 11.00000 -1.50000 AFIX 0 C25 1 0.685573 0.514091 0.808961 11.00000 0.02319 0.02611 = 0.02160 -0.00524 0.01526 -0.00310 AFIX 13 H25 2 0.714591 0.499903 0.778692 11.00000 -1.20000 AFIX 0 C26 1 0.735451 0.599537 0.843166 11.00000 0.02948 0.03126 = 0.02832 -0.01022 0.01918 -0.00853 AFIX 137 H26A 2 0.682093 0.635318 0.792939 11.00000 -1.50000 H26B 2 0.835305 0.603920 0.877885 11.00000 -1.50000 H26C 2 0.720229 0.612953 0.880123 11.00000 -1.50000 AFIX 0 C27 1 0.762392 0.457306 0.888381 11.00000 0.02924 0.03753 = 0.02407 0.00151 0.01162 -0.00010 AFIX 137 H27A 2 0.742632 0.403360 0.867443 11.00000 -1.50000 H27B 2 0.729347 0.466179 0.916170 11.00000 -1.50000 H27C 2 0.863464 0.466699 0.931430 11.00000 -1.50000 AFIX 0 C28 1 0.855732 0.213687 0.736056 11.00000 0.02599 0.01964 = 0.03053 0.01057 0.02064 0.00887 AFIX 137 H28A 2 0.828627 0.189077 0.684677 11.00000 -1.50000 H28B 2 0.853483 0.174833 0.768417 11.00000 -1.50000 H28C 2 0.950587 0.234906 0.774601 11.00000 -1.50000 AFIX 0 C29 1 0.508108 0.294126 0.741987 11.00000 0.03007 0.02174 = 0.02829 0.00721 0.02377 0.00278 AFIX 137 H29A 2 0.517225 0.335461 0.777218 11.00000 -1.50000 H29B 2 0.559029 0.247747 0.778674 11.00000 -1.50000 H29C 2 0.408990 0.281190 0.692230 11.00000 -1.50000 AFIX 0 PART 1 C30 1 0.656043 0.591509 0.599805 21.00000 0.01752 0.01711 = 0.01902 0.00132 0.01375 -0.00041 PART 2 C30A 1 0.653278 0.598416 0.608074 -21.00000 0.01752 0.01711 = 0.01902 0.00132 0.01375 -0.00041 PART 1 C31 1 0.597268 0.713377 0.526770 21.00000 0.02247 0.01679 = 0.02039 0.00231 0.01516 0.00032 AFIX 43 H31 2 0.543731 0.741497 0.473257 21.00000 -1.20000 AFIX 0 PART 2 C31A 1 0.587084 0.717185 0.533568 -21.00000 0.02247 0.01679 = 0.02039 0.00231 0.01516 0.00032 AFIX 43 H31A 2 0.524430 0.744927 0.479493 -21.00000 -1.20000 AFIX 0 PART 1 C32 1 0.694445 0.754104 0.606036 21.00000 0.03060 0.01453 = 0.03203 -0.00565 0.01849 -0.00467 AFIX 43 H32 2 0.705696 0.808732 0.606111 21.00000 -1.20000 AFIX 0 PART 2 C32A 1 0.678665 0.761008 0.609489 -21.00000 0.03060 0.01453 = 0.03203 -0.00565 0.01849 -0.00467 AFIX 43 H32A 2 0.693115 0.815534 0.612020 -21.00000 -1.20000 AFIX 0 PART 1 C33 1 0.776712 0.712362 0.687039 21.00000 0.02119 0.03201 = 0.02013 -0.01076 0.00998 -0.00623 AFIX 43 H33 2 0.844974 0.738161 0.742067 21.00000 -1.20000 AFIX 0 PART 2 C33A 1 0.748026 0.711248 0.683450 -21.00000 0.02119 0.03201 = 0.02013 -0.01076 0.00998 -0.00623 AFIX 43 H33A 2 0.787700 0.737651 0.735677 -21.00000 -1.20000 AFIX 0 PART 1 C34 1 0.753473 0.632525 0.682636 21.00000 0.02095 0.03294 = 0.01270 0.00424 0.00880 0.00190 AFIX 43 H34 2 0.803203 0.604323 0.735683 21.00000 -1.20000 AFIX 0 PART 2 C34A 1 0.768268 0.630897 0.693130 -21.00000 0.02095 0.03294 = 0.01270 0.00424 0.00880 0.00190 AFIX 43 H34A 2 0.843057 0.603315 0.745455 -21.00000 -1.20000 AFIX 0 PART 0 N1 4 0.751381 0.345516 0.669594 11.00000 0.01391 0.01590 = 0.01421 0.00207 0.00978 0.00176 N2 4 0.535934 0.394237 0.670035 11.00000 0.01537 0.01466 = 0.01448 0.00107 0.01085 0.00148 PART 1 N3 4 0.575267 0.633993 0.522485 21.00000 0.01522 0.01491 = 0.01377 -0.00094 0.00970 -0.00189 PART 2 N3A 4 0.577555 0.636477 0.528487 -21.00000 0.01522 0.01491 = 0.01377 -0.00094 0.00970 -0.00189 PART 1 O1 5 0.645138 0.515599 0.594683 21.00000 0.02964 0.01531 = 0.04303 0.00595 0.02668 -0.00060 PART 2 O1A 5 0.620234 0.524864 0.602182 -21.00000 0.02964 0.01531 = 0.04303 0.00595 0.02668 -0.00060 PART 0 ZN1 6 0.581206 0.417140 0.599704 11.00000 0.01366 0.01165 = 0.01251 0.00190 0.00907 0.00088 PART -1 C35 1 0.500677 -0.028597 0.554119 10.50000 0.01966 0.08965 = 0.08221 0.03323 0.02190 0.01003 AFIX 23 H35A 2 0.419579 -0.038796 0.545428 10.50000 -1.20000 H35B 2 0.583065 -0.055538 0.608685 10.50000 -1.20000 AFIX 0 CL1 3 0.531200 0.065940 0.565403 10.50000 0.12299 0.10144 = 0.09153 0.01470 0.08449 0.01145 CL1A 3 0.463455 -0.069128 0.457862 10.50000 0.06420 0.05578 = 0.13562 0.00323 0.05229 0.01437 HKLF 4 REM db8.8_reprocessed_a.res in P2(1)/c REM wR2 = 0.0795, GooF = S = 1.032, Restrained GooF = 1.031 for all data REM R1 = 0.0326 for 6909 Fo > 4sig(Fo) and 0.0469 for all 8388 data REM 411 parameters refined using 8 restraints END WGHT 0.0342 1.7918 REM Highest difference peak 0.594, deepest hole -0.483, 1-sigma level 0.056 Q1 1 0.5237 0.0200 0.5760 11.00000 0.05 0.59 Q2 1 0.5177 -0.0603 0.6021 11.00000 0.05 0.39 Q3 1 0.6861 0.3807 0.6558 11.00000 0.05 0.34 Q4 1 0.8196 0.3458 0.6787 11.00000 0.05 0.34 ; _shelx_res_checksum 1946 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.272 _oxdiff_exptl_absorpt_empirical_full_min 0.832