#------------------------------------------------------------------------------ #$Date: 2024-01-06 09:55:54 +0200 (Sat, 06 Jan 2024) $ #$Revision: 288781 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/76/7247639.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7247639 loop_ _publ_author_name 'Rizzuto, Felix J.' 'Pal, Shyam C.' 'Kearns, Eleanor R.' 'Hua, Carol' 'Solomon, Marcello B.' 'Doheny, Patrick W.' 'Faust, Thomas B.' 'Kepert, Cameron J.' 'Das, Madhab C.' 'D'Alessandro, Deanna M.' _publ_section_title ; The physical and electronic properties of Metal--Organic Frameworks containing dipyridylthiazolo[5,4-d]thiazole ; _journal_issue 46 _journal_name_full CrystEngComm _journal_page_first 6434 _journal_page_last 6440 _journal_paper_doi 10.1039/D3CE00541K _journal_volume 25 _journal_year 2023 _chemical_formula_sum 'C28 H16 N4 O5 S2 Zn' _chemical_formula_weight 617.96 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2023-05-03 deposited with the CCDC. 2023-10-27 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 96.56(2) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 32.53(2) _cell_length_b 8.664(3) _cell_length_c 22.10(2) _cell_measurement_reflns_used 9934 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 26.03 _cell_measurement_theta_min 2.34 _cell_volume 6188(7) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_unetI/netI 0.0432 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 34533 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 24.802 _diffrn_reflns_theta_max 24.802 _diffrn_reflns_theta_min 1.855 _exptl_absorpt_coefficient_mu 0.969 _exptl_absorpt_correction_type none _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.327 _exptl_crystal_description block _exptl_crystal_F_000 2512 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _refine_diff_density_max 0.291 _refine_diff_density_min -0.198 _refine_diff_density_rms 0.049 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 361 _refine_ls_number_reflns 5310 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.058 _refine_ls_R_factor_all 0.0367 _refine_ls_R_factor_gt 0.0316 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+2.0705P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0838 _refine_ls_wR_factor_ref 0.0859 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4599 _reflns_number_total 5310 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ce00541k2.cif _cod_data_source_block 2-Zn _cod_depositor_comments 'Adding full bibliography for 7247635--7247639.cif.' _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 7247639 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.5484 _shelx_estimated_absorpt_t_max 0.7461 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL mcd_sp_PY2N2_0m_a.res in C2/c CELL 0.71073 32.5306 8.6642 22.1020 90.000 96.558 90.000 ZERR 8.00 0.0545 0.0142 0.0457 0.000 0.059 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N O S ZN UNIT 224 128 32 40 16 8 MERG 2 FMAP 2 PLAN 20 ACTA BOND $H LIST 6 L.S. 10 TEMP 23.00 WGHT 0.041000 2.070500 FVAR 1.11600 ZN1 6 0.533298 0.888672 0.511080 11.00000 0.03076 0.03107 = 0.03353 0.00120 0.00150 0.01177 S1 5 0.653115 0.185468 0.521873 11.00000 0.03325 0.03699 = 0.10078 -0.00440 -0.00231 0.00977 S2 5 0.772932 0.203540 0.596991 11.00000 0.03898 0.03761 = 0.08636 -0.00193 -0.00774 0.01374 O2 4 0.499275 0.802325 0.573703 11.00000 0.04629 0.06404 = 0.05022 0.01469 0.01573 0.01299 O1 4 0.448950 0.971095 0.553464 11.00000 0.06130 0.04819 = 0.05230 0.01709 0.01583 0.01310 O3 4 0.491362 0.212770 0.948490 11.00000 0.04078 0.05610 = 0.05454 0.01653 -0.00938 -0.00866 N1 3 0.578806 0.729153 0.513528 11.00000 0.03225 0.03489 = 0.04478 -0.00019 0.00198 0.01232 O4 4 0.441403 0.042233 0.926852 11.00000 0.05404 0.04666 = 0.05341 0.01571 -0.00909 -0.00953 O5 4 0.376832 0.593165 0.757231 11.00000 0.04083 0.09903 = 0.08495 0.05734 0.01726 0.01765 N2 3 0.704765 0.396660 0.563604 11.00000 0.03794 0.03457 = 0.07487 -0.00315 -0.00470 0.01312 N3 3 0.720757 -0.006884 0.555835 11.00000 0.04038 0.03359 = 0.09189 0.00079 0.00397 0.01244 C6 1 0.667101 0.374186 0.538848 11.00000 0.03483 0.03503 = 0.05904 -0.00184 0.00715 0.01082 C3 1 0.637041 0.497852 0.528017 11.00000 0.03252 0.03737 = 0.05171 -0.00001 0.00546 0.01061 C15 1 0.464895 0.858110 0.581252 11.00000 0.04640 0.04089 = 0.03506 0.00276 0.00155 0.00164 C5 1 0.571762 0.592623 0.487929 11.00000 0.04217 0.04778 = 0.05637 -0.01126 -0.00980 0.01636 AFIX 43 H5 2 0.546502 0.575836 0.464631 11.00000 -1.20000 AFIX 0 C25 1 0.435166 0.283816 0.879470 11.00000 0.03951 0.04623 = 0.03977 0.00988 0.00382 -0.00419 C26 1 0.448363 0.434279 0.879370 11.00000 0.04405 0.05236 = 0.04856 0.01365 0.00535 -0.00520 AFIX 43 H26 2 0.470821 0.465245 0.906487 11.00000 -1.20000 AFIX 0 C16 1 0.441523 0.785012 0.626592 11.00000 0.04118 0.03962 = 0.03727 0.00418 0.00524 0.00619 C4 1 0.599628 0.475735 0.494011 11.00000 0.04604 0.04163 = 0.06673 -0.01654 -0.00748 0.01670 AFIX 43 H4 2 0.593375 0.381233 0.475224 11.00000 -1.20000 AFIX 0 C21 1 0.456205 0.653559 0.657213 11.00000 0.04430 0.04195 = 0.04601 0.00814 0.00928 0.01517 AFIX 43 H21 2 0.480739 0.609156 0.647901 11.00000 -1.20000 AFIX 0 C24 1 0.401917 0.240272 0.839955 11.00000 0.05181 0.05636 = 0.05898 0.01847 -0.00849 -0.01240 AFIX 43 H24 2 0.392148 0.139494 0.840708 11.00000 -1.20000 AFIX 0 C28 1 0.457582 0.171219 0.921811 11.00000 0.03821 0.04579 = 0.03744 0.00607 0.00443 -0.00260 C22 1 0.396557 0.491675 0.798966 11.00000 0.04302 0.07022 = 0.05610 0.03175 0.01403 0.00776 C8 1 0.702034 0.131582 0.550069 11.00000 0.03287 0.03519 = 0.07253 0.00114 0.00314 0.01011 C23 1 0.382608 0.344762 0.798768 11.00000 0.04227 0.08161 = 0.05860 0.02347 -0.00822 -0.00519 AFIX 43 H23 2 0.360298 0.314297 0.771274 11.00000 -1.20000 AFIX 0 C27 1 0.428731 0.539233 0.839658 11.00000 0.05407 0.05121 = 0.06559 0.02013 0.01279 -0.00254 AFIX 43 H27 2 0.437253 0.641744 0.840448 11.00000 -1.20000 AFIX 0 C18 1 0.383634 0.781094 0.683675 11.00000 0.04180 0.06826 = 0.05791 0.02225 0.01451 0.01967 AFIX 43 H18 2 0.358705 0.823365 0.692414 11.00000 -1.20000 AFIX 0 C9 1 0.758606 0.014764 0.580219 11.00000 0.03846 0.03570 = 0.06443 0.00296 0.00663 0.01099 C7 1 0.724119 0.258013 0.569160 11.00000 0.03541 0.03864 = 0.06440 -0.00069 0.00133 0.01252 C17 1 0.404705 0.846077 0.640029 11.00000 0.05125 0.04605 = 0.04989 0.01784 0.00527 0.01826 AFIX 43 H17 2 0.393939 0.932908 0.619138 11.00000 -1.20000 AFIX 0 C19 1 0.399500 0.653387 0.714408 11.00000 0.04031 0.05846 = 0.05313 0.02236 0.00904 0.00902 C1 1 0.615354 0.751401 0.545104 11.00000 0.03779 0.03205 = 0.07808 -0.00546 -0.00291 0.00742 AFIX 43 H1 2 0.621070 0.847619 0.562738 11.00000 -1.20000 AFIX 0 C20 1 0.435511 0.587843 0.700668 11.00000 0.05148 0.04376 = 0.05588 0.02015 0.00862 0.01224 AFIX 43 H20 2 0.445743 0.499240 0.720835 11.00000 -1.20000 AFIX 0 C2 1 0.644917 0.640408 0.552985 11.00000 0.03075 0.04108 = 0.08006 -0.00397 -0.00487 0.01035 AFIX 43 H2 2 0.670332 0.661295 0.575214 11.00000 -1.20000 AFIX 0 C10 1 0.787975 -0.110153 0.593204 11.00000 0.04424 0.04024 = 0.06838 0.00664 0.00848 0.01836 C13 1 0.828472 -0.084995 0.616269 11.00000 0.05281 0.05304 = 0.08607 0.00258 -0.00012 0.02069 AFIX 43 H13 2 0.838211 0.014644 0.624396 11.00000 -1.20000 AFIX 0 N4 3 0.843251 -0.351392 0.616006 11.00000 0.08233 0.06076 = 0.13941 0.00968 -0.00199 0.04075 C11 1 0.776191 -0.259230 0.580611 11.00000 0.06152 0.03776 = 0.14409 0.00434 -0.00449 0.01308 AFIX 43 H11 2 0.749317 -0.282445 0.564110 11.00000 -1.20000 AFIX 0 C14 1 0.854060 -0.208832 0.626991 11.00000 0.05665 0.07033 = 0.10806 0.00798 -0.00793 0.03009 AFIX 43 H14 2 0.881218 -0.190011 0.643350 11.00000 -1.20000 AFIX 0 C12 1 0.804900 -0.373003 0.592892 11.00000 0.08579 0.04168 = 0.18634 -0.00023 -0.00059 0.02448 AFIX 43 H12 2 0.796516 -0.473953 0.584121 11.00000 -1.20000 AFIX 0 HKLF 4 REM mcd_sp_PY2N2_0m_a.res in C2/c REM R1 = 0.0316 for 4599 Fo > 4sig(Fo) and 0.0367 for all 5310 data REM 361 parameters refined using 0 restraints END WGHT 0.0408 2.1110 REM Highest difference peak 0.291, deepest hole -0.198, 1-sigma level 0.049 Q1 1 0.5542 0.7949 0.5228 11.00000 0.05 0.29 Q2 1 0.4534 0.0052 0.9664 11.00000 0.05 0.28 Q3 1 0.7680 0.0981 0.5898 11.00000 0.05 0.26 Q4 1 0.5083 0.8867 0.4763 11.00000 0.05 0.25 Q5 1 0.6813 0.1356 0.5425 11.00000 0.05 0.25 Q6 1 0.4435 0.7140 0.6336 11.00000 0.05 0.22 Q7 1 0.4825 0.7929 0.5554 11.00000 0.05 0.22 Q8 1 0.7474 0.2463 0.5813 11.00000 0.05 0.22 Q9 1 0.4446 0.2606 0.9025 11.00000 0.05 0.22 Q10 1 0.6367 0.1543 0.5100 11.00000 0.05 0.22 Q11 1 0.7177 0.3183 0.5643 11.00000 0.05 0.22 Q12 1 0.4182 0.4991 0.8074 11.00000 0.05 0.21 Q13 1 0.4430 0.3466 0.8748 11.00000 0.05 0.21 Q14 1 0.4480 0.7976 0.5982 11.00000 0.05 0.21 Q15 1 0.3828 0.5015 0.7322 11.00000 0.05 0.21 Q16 1 0.6602 0.2936 0.5119 11.00000 0.05 0.20 Q17 1 0.5769 0.6914 0.4966 11.00000 0.05 0.20 Q18 1 0.4495 0.0693 0.9139 11.00000 0.05 0.20 Q19 1 0.3864 0.6997 0.6867 11.00000 0.05 0.20 Q20 1 0.3856 0.3137 0.8296 11.00000 0.05 0.20 ; _shelx_res_checksum 63407 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.53330(2) 0.88867(2) 0.51108(2) 0.03195(9) Uani 1 1 d . . . . . S1 S 0.65312(2) 0.18547(7) 0.52187(4) 0.05777(19) Uani 1 1 d . . . . . S2 S 0.77293(2) 0.20354(7) 0.59699(3) 0.05546(18) Uani 1 1 d . . . . . O2 O 0.49927(5) 0.8023(2) 0.57370(7) 0.0527(4) Uani 1 1 d . . . . . O1 O 0.44895(5) 0.97110(18) 0.55346(7) 0.0532(4) Uani 1 1 d . . . . . O3 O 0.49136(5) 0.21277(19) 0.94849(7) 0.0516(4) Uani 1 1 d . . . . . N1 N 0.57881(5) 0.7292(2) 0.51353(8) 0.0375(4) Uani 1 1 d . . . . . O4 O 0.44140(5) 0.04223(18) 0.92685(7) 0.0525(4) Uani 1 1 d . . . . . O5 O 0.37683(5) 0.5932(2) 0.75723(9) 0.0742(6) Uani 1 1 d . . . . . N2 N 0.70476(6) 0.3967(2) 0.56360(10) 0.0500(5) Uani 1 1 d . . . . . N3 N 0.72076(6) -0.0069(2) 0.55583(10) 0.0556(5) Uani 1 1 d . . . . . C6 C 0.66710(7) 0.3742(2) 0.53885(11) 0.0428(5) Uani 1 1 d . . . . . C3 C 0.63704(7) 0.4979(2) 0.52802(10) 0.0405(5) Uani 1 1 d . . . . . C15 C 0.46489(7) 0.8581(3) 0.58125(9) 0.0410(5) Uani 1 1 d . . . . . C5 C 0.57176(8) 0.5926(3) 0.48793(11) 0.0500(6) Uani 1 1 d . . . . . H5 H 0.5465 0.5758 0.4646 0.060 Uiso 1 1 calc R U . . . C25 C 0.43517(7) 0.2838(3) 0.87947(9) 0.0419(5) Uani 1 1 d . . . . . C26 C 0.44836(7) 0.4343(3) 0.87937(10) 0.0483(6) Uani 1 1 d . . . . . H26 H 0.4708 0.4652 0.9065 0.058 Uiso 1 1 calc R U . . . C16 C 0.44152(7) 0.7850(2) 0.62659(9) 0.0393(5) Uani 1 1 d . . . . . C4 C 0.59963(7) 0.4757(3) 0.49401(11) 0.0525(6) Uani 1 1 d . . . . . H4 H 0.5934 0.3812 0.4752 0.063 Uiso 1 1 calc R U . . . C21 C 0.45620(7) 0.6536(3) 0.65721(10) 0.0438(5) Uani 1 1 d . . . . . H21 H 0.4807 0.6092 0.6479 0.053 Uiso 1 1 calc R U . . . C24 C 0.40192(8) 0.2403(3) 0.83995(11) 0.0569(7) Uani 1 1 d . . . . . H24 H 0.3921 0.1395 0.8407 0.068 Uiso 1 1 calc R U . . . C28 C 0.45758(7) 0.1712(3) 0.92181(9) 0.0405(5) Uani 1 1 d . . . . . C22 C 0.39656(8) 0.4917(3) 0.79897(11) 0.0558(7) Uani 1 1 d . . . . . C8 C 0.70203(7) 0.1316(2) 0.55007(12) 0.0471(6) Uani 1 1 d . . . . . C23 C 0.38261(8) 0.3448(3) 0.79877(12) 0.0619(7) Uani 1 1 d . . . . . H23 H 0.3603 0.3143 0.7713 0.074 Uiso 1 1 calc R U . . . C27 C 0.42873(8) 0.5392(3) 0.83966(11) 0.0565(6) Uani 1 1 d . . . . . H27 H 0.4373 0.6417 0.8404 0.068 Uiso 1 1 calc R U . . . C18 C 0.38363(8) 0.7811(3) 0.68367(11) 0.0553(6) Uani 1 1 d . . . . . H18 H 0.3587 0.8234 0.6924 0.066 Uiso 1 1 calc R U . . . C9 C 0.75861(7) 0.0148(3) 0.58022(11) 0.0461(6) Uani 1 1 d . . . . . C7 C 0.72412(7) 0.2580(3) 0.56916(11) 0.0465(6) Uani 1 1 d . . . . . C17 C 0.40470(8) 0.8461(3) 0.64003(10) 0.0491(6) Uani 1 1 d . . . . . H17 H 0.3939 0.9329 0.6191 0.059 Uiso 1 1 calc R U . . . C19 C 0.39950(7) 0.6534(3) 0.71441(11) 0.0503(6) Uani 1 1 d . . . . . C1 C 0.61535(7) 0.7514(3) 0.54510(12) 0.0500(6) Uani 1 1 d . . . . . H1 H 0.6211 0.8476 0.5627 0.060 Uiso 1 1 calc R U . . . C20 C 0.43551(8) 0.5878(3) 0.70067(11) 0.0502(6) Uani 1 1 d . . . . . H20 H 0.4457 0.4992 0.7208 0.060 Uiso 1 1 calc R U . . . C2 C 0.64492(7) 0.6404(3) 0.55299(12) 0.0515(6) Uani 1 1 d . . . . . H2 H 0.6703 0.6613 0.5752 0.062 Uiso 1 1 calc R U . . . C10 C 0.78798(8) -0.1102(3) 0.59320(12) 0.0508(6) Uani 1 1 d . . . . . C13 C 0.82847(9) -0.0850(3) 0.61627(13) 0.0646(7) Uani 1 1 d . . . . . H13 H 0.8382 0.0146 0.6244 0.078 Uiso 1 1 calc R U . . . N4 N 0.84325(10) -0.3514(3) 0.61601(15) 0.0953(10) Uani 1 1 d . . . . . C11 C 0.77619(10) -0.2592(3) 0.58061(17) 0.0824(10) Uani 1 1 d . . . . . H11 H 0.7493 -0.2824 0.5641 0.099 Uiso 1 1 calc R U . . . C14 C 0.85406(10) -0.2088(4) 0.62699(15) 0.0797(9) Uani 1 1 d . . . . . H14 H 0.8812 -0.1900 0.6433 0.096 Uiso 1 1 calc R U . . . C12 C 0.80490(13) -0.3730(4) 0.5929(2) 0.1058(14) Uani 1 1 d . . . . . H12 H 0.7965 -0.4740 0.5841 0.127 Uiso 1 1 calc R U . . . 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 Zn1 0.03076(15) 0.03107(15) 0.03353(14) 0.00120(9) 0.00150(10) 0.01177(9) S1 0.0332(3) 0.0370(3) 0.1008(5) -0.0044(3) -0.0023(3) 0.0098(3) S2 0.0390(3) 0.0376(3) 0.0864(5) -0.0019(3) -0.0077(3) 0.0137(3) O2 0.0463(10) 0.0640(11) 0.0502(9) 0.0147(8) 0.0157(8) 0.0130(8) O1 0.0613(11) 0.0482(10) 0.0523(9) 0.0171(8) 0.0158(8) 0.0131(8) O3 0.0408(9) 0.0561(10) 0.0545(9) 0.0165(8) -0.0094(8) -0.0087(8) N1 0.0322(10) 0.0349(10) 0.0448(9) -0.0002(8) 0.0020(8) 0.0123(8) O4 0.0540(10) 0.0467(10) 0.0534(9) 0.0157(8) -0.0091(8) -0.0095(8) O5 0.0408(10) 0.0990(15) 0.0850(13) 0.0573(12) 0.0173(9) 0.0176(10) N2 0.0379(11) 0.0346(11) 0.0749(14) -0.0031(9) -0.0047(10) 0.0131(8) N3 0.0404(12) 0.0336(10) 0.0919(15) 0.0008(10) 0.0040(11) 0.0124(9) C6 0.0348(13) 0.0350(12) 0.0590(14) -0.0018(10) 0.0072(10) 0.0108(9) C3 0.0325(12) 0.0374(12) 0.0517(12) 0.0000(9) 0.0055(10) 0.0106(9) C15 0.0464(14) 0.0409(12) 0.0351(11) 0.0028(9) 0.0016(10) 0.0016(10) C5 0.0422(13) 0.0478(14) 0.0564(14) -0.0113(11) -0.0098(11) 0.0164(11) C25 0.0395(12) 0.0462(13) 0.0398(11) 0.0099(9) 0.0038(10) -0.0042(10) C26 0.0440(13) 0.0524(14) 0.0486(13) 0.0136(11) 0.0053(10) -0.0052(11) C16 0.0412(13) 0.0396(12) 0.0373(11) 0.0042(9) 0.0052(9) 0.0062(10) C4 0.0460(14) 0.0416(13) 0.0667(15) -0.0165(11) -0.0075(12) 0.0167(11) C21 0.0443(13) 0.0420(12) 0.0460(12) 0.0081(10) 0.0093(10) 0.0152(10) C24 0.0518(15) 0.0564(15) 0.0590(14) 0.0185(12) -0.0085(12) -0.0124(12) C28 0.0382(13) 0.0458(13) 0.0374(11) 0.0061(9) 0.0044(10) -0.0026(10) C22 0.0430(14) 0.0702(17) 0.0561(14) 0.0318(13) 0.0140(12) 0.0078(13) C8 0.0329(12) 0.0352(12) 0.0725(16) 0.0011(10) 0.0031(11) 0.0101(10) C23 0.0423(14) 0.0816(19) 0.0586(15) 0.0235(14) -0.0082(12) -0.0052(14) C27 0.0541(16) 0.0512(15) 0.0656(16) 0.0201(12) 0.0128(13) -0.0025(12) C18 0.0418(14) 0.0683(17) 0.0579(14) 0.0222(12) 0.0145(11) 0.0197(12) C9 0.0385(13) 0.0357(12) 0.0644(14) 0.0030(10) 0.0066(11) 0.0110(10) C7 0.0354(12) 0.0386(12) 0.0644(14) -0.0007(11) 0.0013(11) 0.0125(10) C17 0.0513(15) 0.0461(13) 0.0499(13) 0.0178(11) 0.0053(11) 0.0183(11) C19 0.0403(13) 0.0585(14) 0.0531(13) 0.0224(11) 0.0090(11) 0.0090(11) C1 0.0378(13) 0.0321(11) 0.0781(16) -0.0055(11) -0.0029(12) 0.0074(10) C20 0.0515(15) 0.0438(13) 0.0559(14) 0.0201(11) 0.0086(12) 0.0122(11) C2 0.0307(12) 0.0411(13) 0.0801(17) -0.0040(12) -0.0049(12) 0.0103(10) C10 0.0442(14) 0.0402(13) 0.0684(16) 0.0066(11) 0.0085(12) 0.0184(10) C13 0.0528(17) 0.0530(15) 0.0861(19) 0.0026(14) -0.0001(14) 0.0207(13) N4 0.082(2) 0.0608(17) 0.139(3) 0.0097(16) -0.0020(19) 0.0407(16) C11 0.0615(19) 0.0378(15) 0.144(3) 0.0043(17) -0.0045(19) 0.0131(13) C14 0.0566(18) 0.070(2) 0.108(2) 0.0080(18) -0.0079(17) 0.0301(16) C12 0.086(3) 0.0417(17) 0.186(4) 0.000(2) -0.001(3) 0.0245(17) 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' S S 0.1246 0.1234 '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' 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 O1 Zn1 O2 159.85(7) 5_676 . ? O1 Zn1 O4 87.48(16) 5_676 2_666 ? O2 Zn1 O4 89.49(15) . 2_666 ? O1 Zn1 N1 99.41(12) 5_676 . ? O2 Zn1 N1 100.72(12) . . ? O4 Zn1 N1 101.07(12) 2_666 . ? O1 Zn1 O3 90.19(15) 5_676 6_565 ? O2 Zn1 O3 85.88(16) . 6_565 ? O4 Zn1 O3 159.97(7) 2_666 6_565 ? N1 Zn1 O3 98.94(12) . 6_565 ? O1 Zn1 Zn1 75.38(10) 5_676 5_676 ? O2 Zn1 Zn1 84.52(11) . 5_676 ? O4 Zn1 Zn1 85.12(11) 2_666 5_676 ? N1 Zn1 Zn1 171.84(5) . 5_676 ? O3 Zn1 Zn1 75.04(11) 6_565 5_676 ? C8 S1 C6 88.17(13) . . ? C7 S2 C9 88.13(13) . . ? C15 O2 Zn1 121.33(16) . . ? C15 O1 Zn1 133.85(17) . 5_676 ? C28 O3 Zn1 133.55(17) . 6_566 ? C5 N1 C1 117.29(18) . . ? C5 N1 Zn1 120.70(17) . . ? C1 N1 Zn1 121.74(17) . . ? C28 O4 Zn1 120.57(16) . 2_646 ? C19 O5 C22 117.4(2) . . ? C6 N2 C7 108.2(2) . . ? C9 N3 C8 107.9(2) . . ? N2 C6 C3 123.0(2) . . ? N2 C6 S1 116.50(16) . . ? C3 C6 S1 120.5(2) . . ? C2 C3 C4 117.6(2) . . ? C2 C3 C6 120.6(2) . . ? C4 C3 C6 121.8(2) . . ? O1 C15 O2 124.9(2) . . ? O1 C15 C16 117.3(2) . . ? O2 C15 C16 117.8(2) . . ? N1 C5 C4 123.1(2) . . ? N1 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? C24 C25 C26 119.2(2) . . ? C24 C25 C28 121.2(2) . . ? C26 C25 C28 119.6(2) . . ? C27 C26 C25 120.6(2) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C17 C16 C21 118.2(2) . . ? C17 C16 C15 120.9(2) . . ? C21 C16 C15 120.8(2) . . ? C5 C4 C3 119.5(2) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C20 C21 C16 121.3(2) . . ? C20 C21 H21 119.3 . . ? C16 C21 H21 119.3 . . ? C25 C24 C23 120.5(3) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? O3 C28 O4 125.4(2) . . ? O3 C28 C25 117.0(2) . . ? O4 C28 C25 117.6(2) . . ? C23 C22 C27 121.3(2) . . ? C23 C22 O5 117.9(3) . . ? C27 C22 O5 120.8(3) . . ? N3 C8 C7 118.3(2) . . ? N3 C8 S1 132.22(19) . . ? C7 C8 S1 109.43(19) . . ? C22 C23 C24 119.2(3) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? C22 C27 C26 119.2(3) . . ? C22 C27 H27 120.4 . . ? C26 C27 H27 120.4 . . ? C17 C18 C19 119.5(2) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? N3 C9 C10 123.1(2) . . ? N3 C9 S2 116.40(17) . . ? C10 C9 S2 120.5(2) . . ? C8 C7 N2 117.7(2) . . ? C8 C7 S2 109.20(19) . . ? N2 C7 S2 133.06(19) . . ? C18 C17 C16 120.9(2) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C20 C19 O5 122.6(2) . . ? C20 C19 C18 120.7(2) . . ? O5 C19 C18 116.7(2) . . ? N1 C1 C2 123.1(2) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C21 C20 C19 119.3(2) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? C1 C2 C3 119.5(2) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C11 C10 C13 117.4(2) . . ? C11 C10 C9 120.1(3) . . ? C13 C10 C9 122.5(2) . . ? C14 C13 C10 118.7(3) . . ? C14 C13 H13 120.6 . . ? C10 C13 H13 120.6 . . ? C14 N4 C12 115.8(3) . . ? C12 C11 C10 118.2(3) . . ? C12 C11 H11 120.9 . . ? C10 C11 H11 120.9 . . ? N4 C14 C13 124.7(3) . . ? N4 C14 H14 117.6 . . ? C13 C14 H14 117.6 . . ? N4 C12 C11 125.2(3) . . ? N4 C12 H12 117.4 . . ? C11 C12 H12 117.4 . . ? 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 Zn1 O1 2.008(3) 5_676 ? Zn1 O2 2.013(3) . ? Zn1 O4 2.018(3) 2_666 ? Zn1 N1 2.021(3) . ? Zn1 O3 2.029(3) 6_565 ? Zn1 Zn1 2.900(3) 5_676 ? S1 C8 1.707(3) . ? S1 C6 1.727(3) . ? S2 C7 1.703(3) . ? S2 C9 1.729(3) . ? O2 C15 1.247(3) . ? O1 C15 1.238(3) . ? O1 Zn1 2.008(3) 5_676 ? O3 C28 1.240(3) . ? O3 Zn1 2.029(3) 6_566 ? N1 C5 1.320(3) . ? N1 C1 1.322(3) . ? O4 C28 1.246(3) . ? O4 Zn1 2.018(3) 2_646 ? O5 C19 1.368(3) . ? O5 C22 1.379(3) . ? N2 C6 1.298(3) . ? N2 C7 1.355(3) . ? N3 C9 1.300(4) . ? N3 C8 1.345(3) . ? C6 C3 1.452(3) . ? C3 C2 1.365(4) . ? C3 C4 1.369(4) . ? C15 C16 1.469(4) . ? C5 C4 1.356(3) . ? C5 H5 0.9300 . ? C25 C24 1.364(4) . ? C25 C26 1.373(4) . ? C25 C28 1.484(3) . ? C26 C27 1.370(4) . ? C26 H26 0.9300 . ? C16 C17 1.373(4) . ? C16 C21 1.382(3) . ? C4 H4 0.9300 . ? C21 C20 1.359(4) . ? C21 H21 0.9300 . ? C24 C23 1.383(4) . ? C24 H24 0.9300 . ? C22 C23 1.351(4) . ? C22 C27 1.363(4) . ? C8 C7 1.351(4) . ? C23 H23 0.9300 . ? C27 H27 0.9300 . ? C18 C17 1.367(4) . ? C18 C19 1.368(4) . ? C18 H18 0.9300 . ? C9 C10 1.450(3) . ? C17 H17 0.9300 . ? C19 C20 1.367(4) . ? C1 C2 1.357(3) . ? C1 H1 0.9300 . ? C20 H20 0.9300 . ? C2 H2 0.9300 . ? C10 C11 1.367(4) . ? C10 C13 1.375(4) . ? C13 C14 1.362(4) . ? C13 H13 0.9300 . ? N4 C14 1.300(4) . ? N4 C12 1.306(5) . ? C11 C12 1.364(4) . ? C11 H11 0.9300 . ? C14 H14 0.9300 . ? C12 H12 0.9300 . ?