#------------------------------------------------------------------------------ #$Date: 2021-10-09 03:25:42 +0300 (Sat, 09 Oct 2021) $ #$Revision: 269871 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/06/10/7061001.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_7061001 loop_ _publ_author_name 'Kumar, Pretam' 'Frontera, Antonio' 'Pandey, Sushil K.' _publ_section_title ; Coordination versus spodium bonds in dinuclear Zn(ii) and Cd(ii) complexes with a dithiophosphate ligand ; _journal_name_full 'New Journal of Chemistry' _journal_paper_doi 10.1039/D1NJ03165A _journal_year 2021 _chemical_formula_moiety 'C40 H52 O4 P2 S4 Zn' _chemical_formula_sum 'C40 H52 O4 P2 S4 Zn' _chemical_formula_weight 852.37 _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 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_date 2021-08-12 _audit_creation_method ; Olex2 1.2-ac21 (compiled 2015.09.16 svn.r134, GUI svn.r4998) ; _audit_update_record ; 2021-08-17 deposited with the CCDC. 2021-09-21 downloaded from the CCDC. ; _cell_angle_alpha 90.00 _cell_angle_beta 91.394(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 21.0546(5) _cell_length_b 13.3289(3) _cell_length_c 30.1770(7) _cell_measurement_reflns_used 4966 _cell_measurement_temperature 150.0(3) _cell_measurement_theta_max 27.9830 _cell_measurement_theta_min 1.9350 _cell_volume 8466.2(3) _computing_cell_refinement 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 150.0(3) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 15.9974 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.982 _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 40.00 110.00 1.00 140.00 -- 26.84 178.00 -60.00 70 2 \w 70.00 116.00 1.00 140.00 -- 26.84 178.00 150.00 46 3 \w -44.00 56.00 1.00 140.00 -- 26.84 -19.00 -30.00 100 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0097401000 _diffrn_orient_matrix_UB_12 0.0472410000 _diffrn_orient_matrix_UB_13 0.0085582000 _diffrn_orient_matrix_UB_21 0.0312505000 _diffrn_orient_matrix_UB_22 -0.0188677000 _diffrn_orient_matrix_UB_23 0.0034725000 _diffrn_orient_matrix_UB_31 0.0080126000 _diffrn_orient_matrix_UB_32 0.0158176000 _diffrn_orient_matrix_UB_33 -0.0215978000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0909 _diffrn_reflns_av_unetI/netI 0.0979 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_number 13538 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 28.39 _diffrn_reflns_theta_min 1.81 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.891 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.525 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'metallic light blue' _exptl_crystal_colour_lustre metallic _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary blue _exptl_crystal_density_diffrn 1.337 _exptl_crystal_density_method 'not measured' _exptl_crystal_description irregular _exptl_crystal_F_000 3584 _exptl_crystal_size_max 0.257 _exptl_crystal_size_mid 0.195 _exptl_crystal_size_min 0.112 _refine_diff_density_max 2.101 _refine_diff_density_min -1.664 _refine_diff_density_rms 0.155 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 472 _refine_ls_number_reflns 9100 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.019 _refine_ls_R_factor_all 0.0977 _refine_ls_R_factor_gt 0.0673 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1201P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1733 _refine_ls_wR_factor_ref 0.2016 _reflns_number_gt 6427 _reflns_number_total 9100 _reflns_threshold_expression >2sigma(I) _iucr_refine_instructions_details ; TITL zn_4t_lt_mo_a.res in C2/c REM Old TITL Zn_4T_LT_Mo in C2/c #15 REM SHELXT solution in C2/c REM R1 0.156, Rweak 0.036, Alpha 0.058, Orientation as input REM Formula found by SHELXT: C18 O1 S6 Zn CELL 0.71073 21.054582 13.328865 30.17704 90 91.3939 90 ZERR 8 0.000472 0.000345 0.000666 0 0.0022 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H O P S Zn UNIT 320 416 32 16 32 8 L.S. 8 PLAN 19 CONN 4 $P BOND $H LIST 6 MORE -1 CONF fmap 2 acta 52 REM REM REM WGHT 0.120100 FVAR 0.80420 ZN1 6 0.580706 0.365348 0.711710 11.00000 0.02711 0.02677 = 0.01777 -0.00291 -0.00216 0.00247 S4 5 0.424281 0.320207 0.713544 11.00000 0.03166 0.02536 = 0.01861 -0.00008 -0.00306 -0.00256 P2 4 0.438491 0.452151 0.684795 11.00000 0.02472 0.02405 = 0.01583 -0.00038 -0.00299 0.00179 S2 5 0.692966 0.367419 0.694549 11.00000 0.02461 0.02595 = 0.02529 -0.00392 -0.00284 -0.00274 S3 5 0.527108 0.505639 0.685384 11.00000 0.02576 0.02655 = 0.02443 0.00351 -0.00336 -0.00140 P1 4 0.666245 0.242452 0.663975 11.00000 0.02386 0.02353 = 0.01701 -0.00115 -0.00412 0.00106 S1 5 0.572480 0.224390 0.664715 11.00000 0.02298 0.03458 = 0.03804 -0.01332 -0.00465 -0.00182 O4 3 0.411388 0.448007 0.634973 11.00000 0.02639 0.03420 = 0.01392 -0.00322 -0.00836 0.00502 O1 3 0.703903 0.151718 0.686008 11.00000 0.03192 0.02254 = 0.02209 0.00144 -0.01106 0.00119 O3 3 0.391147 0.531023 0.705531 11.00000 0.03134 0.02703 = 0.01942 0.00012 0.00099 0.00389 O2 3 0.692582 0.234544 0.614952 11.00000 0.04145 0.02688 = 0.02016 0.00198 0.00064 0.00641 C1 1 0.698288 0.049070 0.675690 11.00000 0.02378 0.02292 = 0.01785 -0.00034 -0.00351 0.00255 C31 1 0.440608 0.389763 0.601968 11.00000 0.02485 0.03428 = 0.01267 0.00128 -0.00543 0.00709 C16 1 0.747025 0.305793 0.555110 11.00000 0.03016 0.02448 = 0.02177 0.00020 -0.00283 0.00559 AFIX 43 H16 2 0.773990 0.250536 0.556153 11.00000 -1.20000 AFIX 0 C11 1 0.697536 0.314047 0.584432 11.00000 0.03319 0.02417 = 0.01555 -0.00169 -0.00612 -0.00054 C34 1 0.495634 0.279304 0.534932 11.00000 0.02451 0.03689 = 0.01880 -0.00258 -0.00721 0.00534 C21 1 0.394061 0.634949 0.695178 11.00000 0.02458 0.02797 = 0.02199 -0.00494 0.00042 0.00558 C35 1 0.506276 0.380680 0.538841 11.00000 0.03183 0.03507 = 0.02410 0.00270 0.00020 0.00051 AFIX 43 H35 2 0.531883 0.412447 0.518446 11.00000 -1.20000 AFIX 0 C4 1 0.695470 -0.158664 0.662807 11.00000 0.02425 0.03182 = 0.01876 0.00507 -0.00134 0.00188 C14 1 0.716013 0.464532 0.521578 11.00000 0.02819 0.02483 = 0.01900 -0.00245 -0.00905 0.00133 C15 1 0.755583 0.381224 0.524272 11.00000 0.02775 0.03393 = 0.02149 0.00026 -0.00413 0.00185 AFIX 43 H15 2 0.788898 0.375949 0.504729 11.00000 -1.20000 AFIX 0 C7 1 0.696273 -0.271569 0.654598 11.00000 0.03586 0.02705 = 0.02717 0.00591 -0.00154 0.00042 C13 1 0.666643 0.469224 0.551571 11.00000 0.02936 0.02848 = 0.02894 0.00060 -0.00573 0.00622 AFIX 43 H13 2 0.639461 0.524225 0.550732 11.00000 -1.20000 AFIX 0 C36 1 0.479760 0.437030 0.572494 11.00000 0.03533 0.02749 = 0.02339 0.00145 -0.00403 0.00082 AFIX 43 H36 2 0.488264 0.505276 0.575077 11.00000 -1.20000 AFIX 0 C32 1 0.427519 0.289104 0.598366 11.00000 0.02991 0.03505 = 0.01913 0.00194 -0.00478 -0.00419 AFIX 43 H32 2 0.400619 0.257920 0.618109 11.00000 -1.20000 AFIX 0 C33 1 0.454987 0.235363 0.564985 11.00000 0.03076 0.02824 = 0.02615 -0.00263 -0.00675 -0.00063 AFIX 43 H33 2 0.446080 0.167243 0.562404 11.00000 -1.20000 AFIX 0 C2 1 0.656992 0.008940 0.644901 11.00000 0.04162 0.02953 = 0.02879 -0.00346 -0.02008 0.01120 AFIX 43 H2 2 0.630105 0.050320 0.628196 11.00000 -1.20000 AFIX 0 C3 1 0.655594 -0.094451 0.638807 11.00000 0.03647 0.03076 = 0.03287 -0.00362 -0.02061 0.00463 AFIX 43 H3 2 0.627091 -0.121485 0.618027 11.00000 -1.20000 AFIX 0 C22 1 0.363607 0.670259 0.657464 11.00000 0.03452 0.03357 = 0.02438 -0.00503 -0.00673 0.00413 AFIX 43 H22 2 0.342374 0.626653 0.638145 11.00000 -1.20000 AFIX 0 C17 1 0.726565 0.544549 0.486572 11.00000 0.03095 0.02650 = 0.02445 0.00191 -0.00661 -0.00072 C12 1 0.656849 0.393749 0.582816 11.00000 0.03101 0.03569 = 0.02216 0.00025 -0.00150 0.00683 AFIX 43 H12 2 0.623220 0.397759 0.602155 11.00000 -1.20000 AFIX 0 C20 1 0.713630 0.498255 0.440236 11.00000 0.05072 0.03580 = 0.02281 0.00281 -0.00353 0.00145 AFIX 137 H20A 2 0.743547 0.445336 0.435241 11.00000 -1.50000 H20B 2 0.718047 0.549063 0.417974 11.00000 -1.50000 H20C 2 0.671267 0.471629 0.438728 11.00000 -1.50000 AFIX 0 C24 1 0.396330 0.839476 0.677315 11.00000 0.02653 0.03161 = 0.03826 -0.00250 -0.00043 0.00352 C6 1 0.738695 -0.012110 0.700246 11.00000 0.03168 0.03107 = 0.03040 0.00079 -0.01672 0.00150 AFIX 43 H6 2 0.766691 0.015260 0.721271 11.00000 -1.20000 AFIX 0 C23 1 0.365324 0.771874 0.648999 11.00000 0.03572 0.04262 = 0.02438 0.00137 -0.00709 0.00304 AFIX 43 H23 2 0.345049 0.796163 0.623462 11.00000 -1.20000 AFIX 0 C25 1 0.424587 0.799258 0.715801 11.00000 0.04526 0.03764 = 0.04174 -0.00727 -0.02469 0.00086 AFIX 43 H25 2 0.444870 0.842024 0.735965 11.00000 -1.20000 AFIX 0 C26 1 0.423113 0.697629 0.724597 11.00000 0.04859 0.03129 = 0.03022 0.00022 -0.01584 0.00351 AFIX 43 H26 2 0.441905 0.672451 0.750495 11.00000 -1.20000 AFIX 0 C5 1 0.737001 -0.114217 0.693197 11.00000 0.04146 0.03240 = 0.03828 0.00561 -0.02183 0.00838 AFIX 43 H5 2 0.764840 -0.154879 0.709486 11.00000 -1.20000 AFIX 0 C37 1 0.525906 0.215349 0.498768 11.00000 0.03478 0.04095 = 0.02573 -0.00981 -0.00259 0.00219 C27 1 0.401155 0.951851 0.667953 11.00000 0.04356 0.02765 = 0.04987 0.00188 0.00100 0.00134 C18 1 0.682925 0.635098 0.491718 11.00000 0.04386 0.03218 = 0.03093 0.00100 -0.00753 0.00742 AFIX 137 H18A 2 0.639444 0.613984 0.488679 11.00000 -1.50000 H18B 2 0.691859 0.683749 0.469255 11.00000 -1.50000 H18C 2 0.690036 0.664485 0.520456 11.00000 -1.50000 AFIX 0 C19 1 0.795634 0.582675 0.489609 11.00000 0.03515 0.03738 = 0.05093 0.00609 -0.00793 -0.00370 AFIX 137 H19A 2 0.803884 0.611018 0.518423 11.00000 -1.50000 H19B 2 0.801850 0.633003 0.467375 11.00000 -1.50000 H19C 2 0.824194 0.527753 0.484922 11.00000 -1.50000 AFIX 0 C10 1 0.711072 -0.329652 0.697656 11.00000 0.12329 0.02972 = 0.04810 0.00674 -0.00250 0.00626 AFIX 137 H10A 2 0.753100 -0.313055 0.708318 11.00000 -1.50000 H10B 2 0.708541 -0.400406 0.691934 11.00000 -1.50000 H10C 2 0.680814 -0.311751 0.719595 11.00000 -1.50000 AFIX 0 C9 1 0.748653 -0.296247 0.622170 11.00000 0.06548 0.03282 = 0.06752 -0.00979 0.02341 0.00471 AFIX 137 H9A 2 0.740294 -0.262221 0.594602 11.00000 -1.50000 H9B 2 0.749678 -0.367336 0.617129 11.00000 -1.50000 H9C 2 0.788897 -0.274688 0.634403 11.00000 -1.50000 AFIX 0 C38 1 0.561325 0.126268 0.520889 11.00000 0.06132 0.04990 = 0.06247 -0.00647 0.01232 0.01873 AFIX 137 H38A 2 0.594049 0.151264 0.540658 11.00000 -1.50000 H38B 2 0.580060 0.085462 0.498482 11.00000 -1.50000 H38C 2 0.531872 0.086729 0.537272 11.00000 -1.50000 AFIX 0 C8 1 0.632749 -0.309452 0.635746 11.00000 0.04505 0.02955 = 0.10020 -0.00365 -0.01374 -0.00780 AFIX 137 H8A 2 0.598960 -0.285217 0.653666 11.00000 -1.50000 H8B 2 0.632595 -0.381476 0.635779 11.00000 -1.50000 H8C 2 0.626745 -0.285487 0.605938 11.00000 -1.50000 AFIX 0 C28 1 0.373392 1.012110 0.705793 11.00000 0.08852 0.03444 = 0.07243 -0.00616 0.00720 0.00583 AFIX 137 H28A 2 0.331850 0.987009 0.712124 11.00000 -1.50000 H28B 2 0.370375 1.081440 0.697384 11.00000 -1.50000 H28C 2 0.400465 1.005834 0.731703 11.00000 -1.50000 AFIX 0 C40 1 0.574706 0.272756 0.472725 11.00000 0.07032 0.05956 = 0.04515 -0.00843 0.02403 0.00723 AFIX 137 H40A 2 0.554105 0.326232 0.456638 11.00000 -1.50000 H40B 2 0.594634 0.228218 0.452283 11.00000 -1.50000 H40C 2 0.606283 0.300173 0.492763 11.00000 -1.50000 AFIX 0 C30 1 0.364555 0.980804 0.625078 11.00000 0.08188 0.03194 = 0.07482 0.01532 -0.01482 -0.00248 AFIX 137 H30A 2 0.378971 0.940257 0.601029 11.00000 -1.50000 H30B 2 0.371919 1.050288 0.618590 11.00000 -1.50000 H30C 2 0.319942 0.969927 0.628868 11.00000 -1.50000 AFIX 0 C39 1 0.473399 0.174316 0.468036 11.00000 0.04839 0.12329 = 0.04773 -0.04754 -0.00677 0.00665 AFIX 137 H39A 2 0.442682 0.139288 0.485225 11.00000 -1.50000 H39B 2 0.491456 0.129023 0.447055 11.00000 -1.50000 H39C 2 0.453046 0.228838 0.452507 11.00000 -1.50000 AFIX 0 C29 1 0.470394 0.979017 0.660877 11.00000 0.04313 0.04794 = 0.13599 0.01279 0.00468 -0.01027 AFIX 137 H29A 2 0.494921 0.964620 0.687350 11.00000 -1.50000 H29B 2 0.473560 1.049182 0.654097 11.00000 -1.50000 H29C 2 0.486368 0.940381 0.636722 11.00000 -1.50000 HKLF 4 REM zn_4t_lt_mo_a.res in C2/c REM R1 = 0.0673 for 6427 Fo > 4sig(Fo) and 0.0977 for all 9100 data REM 472 parameters refined using 0 restraints END WGHT 0.1201 0.0000 REM Highest difference peak 2.101, deepest hole -1.664, 1-sigma level 0.155 Q1 1 0.5803 0.2892 0.7119 11.00000 0.05 2.10 Q2 1 0.5796 0.4377 0.7108 11.00000 0.05 2.05 Q3 1 0.4283 0.3976 0.7137 11.00000 0.05 1.54 Q4 1 0.5604 0.3643 0.7418 11.00000 0.05 1.51 Q5 1 0.5376 0.3609 0.7199 11.00000 0.05 1.16 Q6 1 0.6922 0.2957 0.6972 11.00000 0.05 1.15 Q7 1 0.4230 0.2537 0.7143 11.00000 0.05 1.13 Q8 1 0.4400 0.5187 0.6844 11.00000 0.05 1.11 Q9 1 0.6250 0.3667 0.7037 11.00000 0.05 1.10 Q10 1 0.5998 0.3626 0.6800 11.00000 0.05 1.10 Q11 1 0.5714 0.3018 0.6675 11.00000 0.05 1.07 Q12 1 0.5271 0.4321 0.6869 11.00000 0.05 1.01 Q13 1 0.6700 0.3130 0.6598 11.00000 0.05 0.97 Q14 1 0.6917 0.4401 0.6946 11.00000 0.05 0.93 Q15 1 0.4367 0.3633 0.6791 11.00000 0.05 0.93 Q16 1 0.5712 0.1536 0.6653 11.00000 0.05 0.92 Q17 1 0.5394 0.3641 0.6737 11.00000 0.05 0.92 Q18 1 0.5279 0.5726 0.6823 11.00000 0.05 0.88 Q19 1 0.4032 0.3212 0.7437 11.00000 0.05 0.87 REM The information below was added by Olex2. REM REM R1 = 0.0673 for 6427 Fo > 4sig(Fo) and 0.0977 for all 14004 data REM n/a parameters refined using n/a restraints REM Highest difference peak 2.10, deepest hole -1.66 REM Mean Shift 0, Max Shift 0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0977 REM R1_gt = 0.0673 REM wR_ref = 0.2016 REM GOOF = 1.019 REM Shift_max = 0.001 REM Shift_mean = 0 REM Reflections_all = 14004 REM Reflections_gt = 6427 REM Parameters = n/a REM Hole = -1.66 REM Peak = 2.10 REM Flack = n/a ; _cod_data_source_file d1nj03165a2.cif _cod_data_source_block zn_4t_lt_mo _cod_database_code 7061001 _chemical_oxdiff_formula 'C320 H416 O32 P16 S32 Zn8' _reflns_odcompleteness_completeness 98.01 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C16(H16), C35(H35), C15(H15), C13(H13), C36(H36), C32(H32), C33(H33), C2(H2), C3(H3), C22(H22), C12(H12), C6(H6), C23(H23), C25(H25), C26(H26), C5(H5) 2.b Idealised Me refined as rotating group: C20(H20A,H20B,H20C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C10(H10A,H10B, H10C), C9(H9A,H9B,H9C), C38(H38A,H38B,H38C), C8(H8A,H8B,H8C), C28(H28A,H28B, H28C), C40(H40A,H40B,H40C), C30(H30A,H30B,H30C), C39(H39A,H39B,H39C), C29(H29A, H29B,H29C) ; _olex2_date_sample_data_collection 2021-03-01 _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 11.705 _oxdiff_exptl_absorpt_empirical_full_min 0.441 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y, -z+1/2' 3 'x+1/2, y+1/2, z' 4 '-x+1/2, y+1/2, -z+1/2' 5 '-x, -y, -z' 6 'x, -y, z-1/2' 7 '-x+1/2, -y+1/2, -z' 8 '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_calc_flag _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_refinement_flags_posn Zn1 Zn 0.58071(2) 0.36535(4) 0.711710(14) 0.02392(16) Uani 1 d . . . S4 S 0.42428(5) 0.32021(8) 0.71354(3) 0.0253(2) Uani 1 d . . . P2 P 0.43849(5) 0.45215(8) 0.68479(3) 0.0216(2) Uani 1 d . . . S2 S 0.69297(5) 0.36742(8) 0.69455(3) 0.0253(2) Uani 1 d . . . S3 S 0.52711(5) 0.50564(8) 0.68538(3) 0.0256(2) Uani 1 d . . . P1 P 0.66624(5) 0.24245(8) 0.66397(3) 0.0215(2) Uani 1 d . . . S1 S 0.57248(5) 0.22439(9) 0.66471(4) 0.0320(3) Uani 1 d . . . O4 O 0.41139(13) 0.4480(2) 0.63497(8) 0.0250(6) Uani 1 d . . . O1 O 0.70390(14) 0.1517(2) 0.68601(9) 0.0257(6) Uani 1 d . . . O3 O 0.39115(14) 0.5310(2) 0.70553(9) 0.0259(6) Uani 1 d . . . O2 O 0.69258(15) 0.2345(2) 0.61495(9) 0.0295(7) Uani 1 d . . . C1 C 0.69829(18) 0.0491(3) 0.67569(12) 0.0216(8) Uani 1 d . . . C31 C 0.44061(19) 0.3898(3) 0.60197(12) 0.0240(8) Uani 1 d . . . C16 C 0.7470(2) 0.3058(3) 0.55511(12) 0.0255(9) Uani 1 d . . . H16 H 0.7740 0.2505 0.5562 0.031 Uiso 1 calc . . R C11 C 0.6975(2) 0.3140(3) 0.58443(12) 0.0244(8) Uani 1 d . . . C34 C 0.49563(19) 0.2793(3) 0.53493(12) 0.0269(9) Uani 1 d . . . C21 C 0.39406(19) 0.6349(3) 0.69518(13) 0.0249(9) Uani 1 d . . . C35 C 0.5063(2) 0.3807(3) 0.53884(13) 0.0303(10) Uani 1 d . . . H35 H 0.5319 0.4124 0.5184 0.036 Uiso 1 calc . . R C4 C 0.69547(19) -0.1587(3) 0.66281(13) 0.0250(9) Uani 1 d . . . C14 C 0.71601(19) 0.4645(3) 0.52158(12) 0.0242(8) Uani 1 d . . . C15 C 0.7556(2) 0.3812(3) 0.52427(13) 0.0278(9) Uani 1 d . . . H15 H 0.7889 0.3759 0.5047 0.033 Uiso 1 calc . . R C7 C 0.6963(2) -0.2716(3) 0.65460(14) 0.0301(10) Uani 1 d . . . C13 C 0.6666(2) 0.4692(3) 0.55157(13) 0.0290(9) Uani 1 d . . . H13 H 0.6395 0.5242 0.5507 0.035 Uiso 1 calc . . R C36 C 0.4798(2) 0.4370(3) 0.57249(13) 0.0288(9) Uani 1 d . . . H36 H 0.4883 0.5053 0.5751 0.035 Uiso 1 calc . . R C32 C 0.4275(2) 0.2891(3) 0.59837(13) 0.0281(9) Uani 1 d . . . H32 H 0.4006 0.2579 0.6181 0.034 Uiso 1 calc . . R C33 C 0.4550(2) 0.2354(3) 0.56498(13) 0.0285(9) Uani 1 d . . . H33 H 0.4461 0.1672 0.5624 0.034 Uiso 1 calc . . R C2 C 0.6570(2) 0.0089(3) 0.64490(14) 0.0337(10) Uani 1 d . . . H2 H 0.6301 0.0503 0.6282 0.040 Uiso 1 calc . . R C3 C 0.6556(2) -0.0945(3) 0.63881(14) 0.0337(10) Uani 1 d . . . H3 H 0.6271 -0.1215 0.6180 0.040 Uiso 1 calc . . R C22 C 0.3636(2) 0.6703(3) 0.65746(14) 0.0309(10) Uani 1 d . . . H22 H 0.3424 0.6267 0.6381 0.037 Uiso 1 calc . . R C17 C 0.7266(2) 0.5445(3) 0.48657(13) 0.0274(9) Uani 1 d . . . C12 C 0.6568(2) 0.3937(3) 0.58282(13) 0.0297(9) Uani 1 d . . . H12 H 0.6232 0.3978 0.6022 0.036 Uiso 1 calc . . R C20 C 0.7136(2) 0.4983(3) 0.44024(13) 0.0365(11) Uani 1 d . . . H20A H 0.7435 0.4453 0.4352 0.055 Uiso 1 calc . . GR H20B H 0.7180 0.5491 0.4180 0.055 Uiso 1 calc . . GR H20C H 0.6713 0.4716 0.4387 0.055 Uiso 1 calc . . GR C24 C 0.3963(2) 0.8395(3) 0.67732(15) 0.0322(10) Uani 1 d . . . C6 C 0.7387(2) -0.0121(3) 0.70025(14) 0.0313(10) Uani 1 d . . . H6 H 0.7667 0.0153 0.7213 0.038 Uiso 1 calc . . R C23 C 0.3653(2) 0.7719(4) 0.64900(14) 0.0344(10) Uani 1 d . . . H23 H 0.3450 0.7962 0.6235 0.041 Uiso 1 calc . . R C25 C 0.4246(2) 0.7993(4) 0.71580(16) 0.0420(12) Uani 1 d . . . H25 H 0.4449 0.8420 0.7360 0.050 Uiso 1 calc . . R C26 C 0.4231(2) 0.6976(4) 0.72460(15) 0.0370(11) Uani 1 d . . . H26 H 0.4419 0.6725 0.7505 0.044 Uiso 1 calc . . R C5 C 0.7370(2) -0.1142(4) 0.69320(15) 0.0377(11) Uani 1 d . . . H5 H 0.7648 -0.1549 0.7095 0.045 Uiso 1 calc . . R C37 C 0.5259(2) 0.2153(4) 0.49877(14) 0.0339(10) Uani 1 d . . . C27 C 0.4012(2) 0.9519(4) 0.66795(17) 0.0404(12) Uani 1 d . . . C18 C 0.6829(2) 0.6351(3) 0.49172(15) 0.0358(11) Uani 1 d . . . H18A H 0.6394 0.6140 0.4887 0.054 Uiso 1 calc . . GR H18B H 0.6919 0.6837 0.4693 0.054 Uiso 1 calc . . GR H18C H 0.6900 0.6645 0.5205 0.054 Uiso 1 calc . . GR C19 C 0.7956(2) 0.5827(4) 0.48961(17) 0.0413(11) Uani 1 d . . . H19A H 0.8039 0.6110 0.5184 0.062 Uiso 1 calc . . GR H19B H 0.8018 0.6330 0.4674 0.062 Uiso 1 calc . . GR H19C H 0.8242 0.5278 0.4849 0.062 Uiso 1 calc . . GR C10 C 0.7111(4) -0.3297(4) 0.69766(19) 0.067(2) Uani 1 d . . . H10A H 0.7531 -0.3131 0.7083 0.101 Uiso 1 calc . . GR H10B H 0.7085 -0.4004 0.6919 0.101 Uiso 1 calc . . GR H10C H 0.6808 -0.3118 0.7196 0.101 Uiso 1 calc . . GR C9 C 0.7487(3) -0.2962(4) 0.62217(19) 0.0549(16) Uani 1 d . . . H9A H 0.7403 -0.2622 0.5946 0.082 Uiso 1 calc . . GR H9B H 0.7497 -0.3673 0.6171 0.082 Uiso 1 calc . . GR H9C H 0.7889 -0.2747 0.6344 0.082 Uiso 1 calc . . GR C38 C 0.5613(3) 0.1263(4) 0.5209(2) 0.0577(16) Uani 1 d . . . H38A H 0.5940 0.1513 0.5407 0.087 Uiso 1 calc . . GR H38B H 0.5801 0.0855 0.4985 0.087 Uiso 1 calc . . GR H38C H 0.5319 0.0867 0.5373 0.087 Uiso 1 calc . . GR C8 C 0.6327(3) -0.3095(4) 0.6357(2) 0.0585(16) Uani 1 d . . . H8A H 0.5990 -0.2852 0.6537 0.088 Uiso 1 calc . . GR H8B H 0.6326 -0.3815 0.6358 0.088 Uiso 1 calc . . GR H8C H 0.6267 -0.2855 0.6059 0.088 Uiso 1 calc . . GR C28 C 0.3734(3) 1.0121(4) 0.7058(2) 0.0650(18) Uani 1 d . . . H28A H 0.3318 0.9870 0.7121 0.098 Uiso 1 calc . . GR H28B H 0.3704 1.0814 0.6974 0.098 Uiso 1 calc . . GR H28C H 0.4005 1.0058 0.7317 0.098 Uiso 1 calc . . GR C40 C 0.5747(3) 0.2728(4) 0.47273(18) 0.0580(17) Uani 1 d . . . H40A H 0.5541 0.3262 0.4566 0.087 Uiso 1 calc . . GR H40B H 0.5946 0.2282 0.4523 0.087 Uiso 1 calc . . GR H40C H 0.6063 0.3002 0.4928 0.087 Uiso 1 calc . . GR C30 C 0.3646(3) 0.9808(4) 0.6251(2) 0.0632(17) Uani 1 d . . . H30A H 0.3790 0.9403 0.6010 0.095 Uiso 1 calc . . GR H30B H 0.3719 1.0503 0.6186 0.095 Uiso 1 calc . . GR H30C H 0.3199 0.9699 0.6289 0.095 Uiso 1 calc . . GR C39 C 0.4734(3) 0.1743(6) 0.46804(19) 0.073(2) Uani 1 d . . . H39A H 0.4427 0.1393 0.4852 0.110 Uiso 1 calc . . GR H39B H 0.4915 0.1290 0.4471 0.110 Uiso 1 calc . . GR H39C H 0.4530 0.2288 0.4525 0.110 Uiso 1 calc . . GR C29 C 0.4704(3) 0.9790(5) 0.6609(3) 0.076(2) Uani 1 d . . . H29A H 0.4949 0.9646 0.6873 0.113 Uiso 1 calc . . GR H29B H 0.4736 1.0492 0.6541 0.113 Uiso 1 calc . . GR H29C H 0.4864 0.9404 0.6367 0.113 Uiso 1 calc . . GR 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 0.0271(3) 0.0268(3) 0.0178(3) -0.00291(18) -0.00216(19) 0.00247(18) S4 0.0317(6) 0.0254(5) 0.0186(5) -0.0001(4) -0.0031(4) -0.0026(4) P2 0.0247(5) 0.0240(6) 0.0158(5) -0.0004(4) -0.0030(4) 0.0018(4) S2 0.0246(5) 0.0260(6) 0.0253(5) -0.0039(4) -0.0028(4) -0.0027(4) S3 0.0258(5) 0.0266(6) 0.0244(5) 0.0035(4) -0.0034(4) -0.0014(4) P1 0.0239(5) 0.0235(5) 0.0170(5) -0.0011(4) -0.0041(4) 0.0011(4) S1 0.0230(5) 0.0346(6) 0.0380(6) -0.0133(5) -0.0046(4) -0.0018(4) O4 0.0264(15) 0.0342(17) 0.0139(12) -0.0032(11) -0.0084(11) 0.0050(12) O1 0.0319(16) 0.0225(15) 0.0221(14) 0.0014(11) -0.0111(12) 0.0012(12) O3 0.0313(16) 0.0270(16) 0.0194(13) 0.0001(12) 0.0010(12) 0.0039(12) O2 0.0415(18) 0.0269(16) 0.0202(14) 0.0020(12) 0.0006(13) 0.0064(13) C1 0.024(2) 0.023(2) 0.0178(18) -0.0003(15) -0.0035(15) 0.0025(15) C31 0.025(2) 0.034(2) 0.0127(17) 0.0013(16) -0.0054(15) 0.0071(17) C16 0.030(2) 0.024(2) 0.0218(19) 0.0002(16) -0.0028(17) 0.0056(17) C11 0.033(2) 0.024(2) 0.0155(18) -0.0017(16) -0.0061(16) -0.0005(17) C34 0.025(2) 0.037(2) 0.0188(19) -0.0026(17) -0.0072(16) 0.0053(17) C21 0.025(2) 0.028(2) 0.0220(19) -0.0049(16) 0.0004(16) 0.0056(16) C35 0.032(2) 0.035(3) 0.024(2) 0.0027(18) 0.0002(18) 0.0005(18) C4 0.024(2) 0.032(2) 0.0188(19) 0.0051(16) -0.0013(16) 0.0019(17) C14 0.028(2) 0.025(2) 0.0190(18) -0.0024(16) -0.0090(16) 0.0013(16) C15 0.028(2) 0.034(2) 0.021(2) 0.0003(18) -0.0041(17) 0.0019(18) C7 0.036(2) 0.027(2) 0.027(2) 0.0059(18) -0.0015(18) 0.0004(18) C13 0.029(2) 0.028(2) 0.029(2) 0.0006(18) -0.0057(18) 0.0062(17) C36 0.035(2) 0.027(2) 0.023(2) 0.0014(17) -0.0040(17) 0.0008(18) C32 0.030(2) 0.035(2) 0.0191(19) 0.0019(17) -0.0048(16) -0.0042(18) C33 0.031(2) 0.028(2) 0.026(2) -0.0026(17) -0.0067(17) -0.0006(17) C2 0.042(3) 0.030(2) 0.029(2) -0.0035(19) -0.0201(19) 0.0112(19) C3 0.036(3) 0.031(2) 0.033(2) -0.0036(19) -0.0206(19) 0.0046(19) C22 0.035(2) 0.034(3) 0.024(2) -0.0050(18) -0.0067(18) 0.0041(18) C17 0.031(2) 0.027(2) 0.024(2) 0.0019(17) -0.0066(17) -0.0007(17) C12 0.031(2) 0.036(2) 0.022(2) 0.0003(18) -0.0015(17) 0.0068(18) C20 0.051(3) 0.036(3) 0.023(2) 0.0028(19) -0.004(2) 0.001(2) C24 0.027(2) 0.032(2) 0.038(2) -0.0025(19) -0.0004(19) 0.0035(18) C6 0.032(2) 0.031(2) 0.030(2) 0.0008(19) -0.0167(18) 0.0015(18) C23 0.036(3) 0.043(3) 0.024(2) 0.001(2) -0.0071(18) 0.003(2) C25 0.045(3) 0.038(3) 0.042(3) -0.007(2) -0.025(2) 0.001(2) C26 0.049(3) 0.031(3) 0.030(2) 0.000(2) -0.016(2) 0.004(2) C5 0.041(3) 0.032(3) 0.038(3) 0.006(2) -0.022(2) 0.008(2) C37 0.035(3) 0.041(3) 0.026(2) -0.0098(19) -0.0026(19) 0.002(2) C27 0.044(3) 0.028(3) 0.050(3) 0.002(2) 0.001(2) 0.001(2) C18 0.044(3) 0.032(3) 0.031(2) 0.0010(19) -0.008(2) 0.007(2) C19 0.035(3) 0.037(3) 0.051(3) 0.006(2) -0.008(2) -0.004(2) C10 0.123(6) 0.030(3) 0.048(3) 0.007(3) -0.002(4) 0.006(3) C9 0.065(4) 0.033(3) 0.068(4) -0.010(3) 0.023(3) 0.005(3) C38 0.061(4) 0.050(4) 0.062(4) -0.006(3) 0.012(3) 0.019(3) C8 0.045(3) 0.030(3) 0.100(5) -0.004(3) -0.014(3) -0.008(2) C28 0.089(5) 0.034(3) 0.072(4) -0.006(3) 0.007(4) 0.006(3) C40 0.070(4) 0.060(4) 0.045(3) -0.008(3) 0.024(3) 0.007(3) C30 0.082(5) 0.032(3) 0.075(4) 0.015(3) -0.015(3) -0.002(3) C39 0.048(4) 0.123(6) 0.048(3) -0.048(4) -0.007(3) 0.007(4) C29 0.043(4) 0.048(4) 0.136(7) 0.013(4) 0.005(4) -0.010(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 15 5 -36 0.0966 -15 -5 36 0.0966 27 -4 16 0.1250 -27 4 -16 0.1250 -17 -15 -12 0.0559 17 15 12 0.0559 -23 10 14 0.1172 -5 11 -33 0.1214 20 -14 8 0.1077 -8 9 36 0.0800 0 19 -6 0.0902 9 -3 -41 0.0887 -5 -14 29 0.1145 5 4 41 0.0898 4 3 -42 0.0900 -29 -5 0 0.0793 27 0 -19 0.1167 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 S4 Zn1 S2 105.95(4) 2_656 . ? S4 Zn1 P1 112.53(4) 2_656 . ? S4 Zn1 S1 111.76(4) 2_656 . ? S2 Zn1 P1 43.10(3) . . ? S3 Zn1 S4 120.39(4) . 2_656 ? S3 Zn1 S2 112.70(4) . . ? S3 Zn1 P1 126.83(4) . . ? S3 Zn1 S1 114.16(4) . . ? S1 Zn1 S2 86.48(4) . . ? S1 Zn1 P1 43.64(3) . . ? P2 S4 Zn1 101.78(5) . 2_656 ? S4 P2 S3 117.56(7) . . ? O4 P2 S4 109.06(12) . . ? O4 P2 S3 109.47(11) . . ? O3 P2 S4 108.14(11) . . ? O3 P2 S3 110.82(13) . . ? O3 P2 O4 100.41(15) . . ? P1 S2 Zn1 79.80(5) . . ? P2 S3 Zn1 99.34(5) . . ? S2 P1 S1 111.56(6) . . ? O1 P1 S2 108.26(12) . . ? O1 P1 S1 112.94(12) . . ? O1 P1 O2 99.04(15) . . ? O2 P1 S2 112.74(12) . . ? O2 P1 S1 111.69(13) . . ? P1 S1 Zn1 81.48(5) . . ? C31 O4 P2 122.0(2) . . ? C1 O1 P1 127.7(3) . . ? C21 O3 P2 121.8(2) . . ? C11 O2 P1 126.1(2) . . ? C2 C1 O1 125.4(4) . . ? C2 C1 C6 120.5(4) . . ? C6 C1 O1 114.1(4) . . ? C36 C31 O4 118.7(4) . . ? C32 C31 O4 120.1(3) . . ? C32 C31 C36 121.1(4) . . ? C11 C16 H16 120.6 . . ? C15 C16 H16 120.6 . . ? C15 C16 C11 118.9(4) . . ? C16 C11 O2 115.2(4) . . ? C12 C11 O2 123.5(3) . . ? C12 C11 C16 121.3(4) . . ? C35 C34 C33 117.4(4) . . ? C35 C34 C37 122.5(4) . . ? C33 C34 C37 120.1(4) . . ? C22 C21 O3 119.6(4) . . ? C26 C21 O3 118.6(4) . . ? C26 C21 C22 121.7(4) . . ? C34 C35 H35 119.1 . . ? C34 C35 C36 121.7(4) . . ? C36 C35 H35 119.1 . . ? C3 C4 C7 122.1(4) . . ? C5 C4 C7 121.4(4) . . ? C5 C4 C3 116.4(4) . . ? C15 C14 C13 116.9(4) . . ? C15 C14 C17 120.2(3) . . ? C13 C14 C17 122.8(4) . . ? C16 C15 C14 122.1(4) . . ? C16 C15 H15 118.9 . . ? C14 C15 H15 118.9 . . ? C4 C7 C10 111.2(4) . . ? C4 C7 C9 109.1(4) . . ? C4 C7 C8 112.0(4) . . ? C9 C7 C10 107.3(5) . . ? C8 C7 C10 107.8(5) . . ? C8 C7 C9 109.2(5) . . ? C14 C13 H13 119.0 . . ? C14 C13 C12 122.0(4) . . ? C12 C13 H13 119.0 . . ? C31 C36 C35 118.7(4) . . ? C31 C36 H36 120.6 . . ? C35 C36 H36 120.6 . . ? C31 C32 H32 120.7 . . ? C31 C32 C33 118.7(4) . . ? C33 C32 H32 120.7 . . ? C34 C33 H33 118.8 . . ? C32 C33 C34 122.3(4) . . ? C32 C33 H33 118.8 . . ? C1 C2 H2 120.4 . . ? C1 C2 C3 119.3(4) . . ? C3 C2 H2 120.4 . . ? C4 C3 C2 122.1(4) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? C21 C22 H22 120.8 . . ? C21 C22 C23 118.4(4) . . ? C23 C22 H22 120.8 . . ? C14 C17 C20 108.8(3) . . ? C14 C17 C18 112.6(3) . . ? C14 C17 C19 110.1(4) . . ? C18 C17 C20 108.3(4) . . ? C18 C17 C19 107.6(4) . . ? C19 C17 C20 109.3(4) . . ? C11 C12 C13 118.8(4) . . ? C11 C12 H12 120.6 . . ? C13 C12 H12 120.6 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C23 C24 C25 116.4(4) . . ? C23 C24 C27 123.6(4) . . ? C25 C24 C27 120.0(4) . . ? C1 C6 H6 120.4 . . ? C5 C6 C1 119.2(4) . . ? C5 C6 H6 120.4 . . ? C22 C23 C24 122.4(4) . . ? C22 C23 H23 118.8 . . ? C24 C23 H23 118.8 . . ? C24 C25 H25 119.2 . . ? C26 C25 C24 121.6(4) . . ? C26 C25 H25 119.2 . . ? C21 C26 C25 119.4(4) . . ? C21 C26 H26 120.3 . . ? C25 C26 H26 120.3 . . ? C4 C5 H5 118.7 . . ? C6 C5 C4 122.6(4) . . ? C6 C5 H5 118.7 . . ? C34 C37 C38 108.9(4) . . ? C40 C37 C34 112.7(4) . . ? C40 C37 C38 106.6(4) . . ? C40 C37 C39 110.8(5) . . ? C39 C37 C34 108.9(4) . . ? C39 C37 C38 108.8(5) . . ? C24 C27 C30 111.5(4) . . ? C28 C27 C24 110.5(4) . . ? C28 C27 C30 107.7(5) . . ? C29 C27 C24 109.1(4) . . ? C29 C27 C28 111.5(5) . . ? C29 C27 C30 106.5(5) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38B 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? 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 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40B 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39B 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 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 . . ? 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 S4 2.3394(10) 2_656 ? Zn1 S2 2.4321(11) . ? Zn1 S3 2.3146(11) . ? Zn1 P1 2.8510(10) . ? Zn1 S1 2.3578(12) . ? S4 Zn1 2.3394(10) 2_656 ? S4 P2 1.9869(14) . ? P2 S3 1.9971(15) . ? P2 O4 1.596(3) . ? P2 O3 1.588(3) . ? S2 P1 1.9791(15) . ? P1 S1 1.9895(15) . ? P1 O1 1.584(3) . ? P1 O2 1.596(3) . ? O4 C31 1.415(4) . ? O1 C1 1.407(5) . ? O3 C21 1.422(5) . ? O2 C11 1.410(5) . ? C1 C2 1.366(6) . ? C1 C6 1.381(6) . ? C31 C36 1.380(5) . ? C31 C32 1.373(6) . ? C16 H16 0.9300 . ? C16 C11 1.388(5) . ? C16 C15 1.385(6) . ? C11 C12 1.365(6) . ? C34 C35 1.374(6) . ? C34 C33 1.391(6) . ? C34 C37 1.535(5) . ? C21 C22 1.376(6) . ? C21 C26 1.354(6) . ? C35 H35 0.9300 . ? C35 C36 1.391(6) . ? C4 C7 1.525(6) . ? C4 C3 1.390(6) . ? C4 C5 1.385(6) . ? C14 C15 1.389(6) . ? C14 C13 1.396(5) . ? C14 C17 1.521(6) . ? C15 H15 0.9300 . ? C7 C10 1.538(7) . ? C7 C9 1.528(6) . ? C7 C8 1.527(7) . ? C13 H13 0.9300 . ? C13 C12 1.398(6) . ? C36 H36 0.9300 . ? C32 H32 0.9300 . ? C32 C33 1.375(6) . ? C33 H33 0.9300 . ? C2 H2 0.9300 . ? C2 C3 1.391(6) . ? C3 H3 0.9300 . ? C22 H22 0.9300 . ? C22 C23 1.379(6) . ? C17 C20 1.546(6) . ? C17 C18 1.527(6) . ? C17 C19 1.541(6) . ? C12 H12 0.9300 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C24 C23 1.393(6) . ? C24 C25 1.399(6) . ? C24 C27 1.528(6) . ? C6 H6 0.9300 . ? C6 C5 1.378(6) . ? C23 H23 0.9300 . ? C25 H25 0.9300 . ? C25 C26 1.381(7) . ? C26 H26 0.9300 . ? C5 H5 0.9300 . ? C37 C38 1.545(7) . ? C37 C40 1.516(7) . ? C37 C39 1.527(7) . ? C27 C28 1.524(7) . ? C27 C30 1.539(8) . ? C27 C29 1.522(7) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? 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 Zn1 S4 P2 S3 81.32(7) 2_656 . . . ? Zn1 S4 P2 O4 -153.37(11) 2_656 . . . ? Zn1 S4 P2 O3 -45.05(14) 2_656 . . . ? Zn1 S2 P1 S1 7.01(6) . . . . ? Zn1 S2 P1 O1 -117.85(12) . . . . ? Zn1 S2 P1 O2 133.64(13) . . . . ? S4 Zn1 S2 P1 106.12(5) 2_656 . . . ? S4 Zn1 S3 P2 -74.39(6) 2_656 . . . ? S4 Zn1 S1 P1 -100.32(5) 2_656 . . . ? S4 P2 S3 Zn1 9.55(8) . . . . ? S4 P2 O4 C31 -69.6(3) . . . . ? S4 P2 O3 C21 173.4(3) . . . . ? P2 O4 C31 C36 -100.2(4) . . . . ? P2 O4 C31 C32 82.9(4) . . . . ? P2 O3 C21 C22 84.1(4) . . . . ? P2 O3 C21 C26 -100.6(4) . . . . ? S2 Zn1 S3 P2 159.41(5) . . . . ? S2 Zn1 S1 P1 5.45(5) . . . . ? S2 P1 S1 Zn1 -7.20(6) . . . . ? S2 P1 O1 C1 177.8(3) . . . . ? S2 P1 O2 C11 -38.9(4) . . . . ? S3 Zn1 S2 P1 -120.26(5) . . . . ? S3 Zn1 S1 P1 118.79(5) . . . . ? S3 P2 O4 C31 60.2(3) . . . . ? S3 P2 O3 C21 43.2(3) . . . . ? P1 Zn1 S3 P2 111.91(5) . . . . ? P1 O1 C1 C2 -2.0(6) . . . . ? P1 O1 C1 C6 178.8(3) . . . . ? P1 O2 C11 C16 149.3(3) . . . . ? P1 O2 C11 C12 -31.4(6) . . . . ? S1 Zn1 S2 P1 -5.51(5) . . . . ? S1 Zn1 S3 P2 62.83(6) . . . . ? S1 P1 O1 C1 53.7(3) . . . . ? S1 P1 O2 C11 87.7(3) . . . . ? O4 P2 S3 Zn1 -115.56(12) . . . . ? O4 P2 O3 C21 -72.4(3) . . . . ? O4 C31 C36 C35 -177.2(4) . . . . ? O4 C31 C32 C33 177.8(4) . . . . ? O1 P1 S1 Zn1 115.01(12) . . . . ? O1 P1 O2 C11 -153.1(3) . . . . ? O1 C1 C2 C3 -178.6(4) . . . . ? O1 C1 C6 C5 179.5(4) . . . . ? O3 P2 S3 Zn1 134.59(12) . . . . ? O3 P2 O4 C31 176.9(3) . . . . ? O3 C21 C22 C23 177.8(3) . . . . ? O3 C21 C26 C25 -177.9(4) . . . . ? O2 P1 S1 Zn1 -134.39(12) . . . . ? O2 P1 O1 C1 -64.5(3) . . . . ? O2 C11 C12 C13 179.1(4) . . . . ? C1 C2 C3 C4 -0.7(7) . . . . ? C1 C6 C5 C4 -1.1(7) . . . . ? C31 C32 C33 C34 0.2(7) . . . . ? C16 C11 C12 C13 -1.6(7) . . . . ? C11 C16 C15 C14 -0.4(7) . . . . ? C34 C35 C36 C31 -1.5(7) . . . . ? C21 C22 C23 C24 -0.4(6) . . . . ? C35 C34 C33 C32 -1.9(7) . . . . ? C35 C34 C37 C38 126.0(5) . . . . ? C35 C34 C37 C40 7.9(6) . . . . ? C35 C34 C37 C39 -115.6(5) . . . . ? C14 C13 C12 C11 1.1(7) . . . . ? C15 C16 C11 O2 -179.4(4) . . . . ? C15 C16 C11 C12 1.2(7) . . . . ? C15 C14 C13 C12 -0.4(6) . . . . ? C15 C14 C17 C20 65.7(5) . . . . ? C15 C14 C17 C18 -174.2(4) . . . . ? C15 C14 C17 C19 -54.0(5) . . . . ? C7 C4 C3 C2 -177.0(4) . . . . ? C7 C4 C5 C6 177.9(4) . . . . ? C13 C14 C15 C16 0.0(6) . . . . ? C13 C14 C17 C20 -113.1(4) . . . . ? C13 C14 C17 C18 7.1(6) . . . . ? C13 C14 C17 C19 127.2(4) . . . . ? C36 C31 C32 C33 0.9(6) . . . . ? C32 C31 C36 C35 -0.3(6) . . . . ? C33 C34 C35 C36 2.6(6) . . . . ? C33 C34 C37 C38 -55.0(6) . . . . ? C33 C34 C37 C40 -173.1(5) . . . . ? C33 C34 C37 C39 63.5(6) . . . . ? C2 C1 C6 C5 0.2(6) . . . . ? C3 C4 C7 C10 -147.4(5) . . . . ? C3 C4 C7 C9 94.4(5) . . . . ? C3 C4 C7 C8 -26.7(6) . . . . ? C3 C4 C5 C6 1.0(7) . . . . ? C22 C21 C26 C25 -2.7(7) . . . . ? C17 C14 C15 C16 -178.9(4) . . . . ? C17 C14 C13 C12 178.5(4) . . . . ? C24 C25 C26 C21 0.5(7) . . . . ? C6 C1 C2 C3 0.6(6) . . . . ? C23 C24 C25 C26 1.6(7) . . . . ? C23 C24 C27 C28 122.9(5) . . . . ? C23 C24 C27 C30 3.2(6) . . . . ? C23 C24 C27 C29 -114.2(5) . . . . ? C25 C24 C23 C22 -1.6(7) . . . . ? C25 C24 C27 C28 -57.8(6) . . . . ? C25 C24 C27 C30 -177.6(5) . . . . ? C25 C24 C27 C29 65.0(6) . . . . ? C26 C21 C22 C23 2.6(6) . . . . ? C5 C4 C7 C10 35.9(6) . . . . ? C5 C4 C7 C9 -82.3(5) . . . . ? C5 C4 C7 C8 156.7(5) . . . . ? C5 C4 C3 C2 -0.1(6) . . . . ? C37 C34 C35 C36 -178.3(4) . . . . ? C37 C34 C33 C32 179.0(4) . . . . ? C27 C24 C23 C22 177.6(4) . . . . ? C27 C24 C25 C26 -177.7(4) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 14.9631 4.9399 -35.9853 0.0711 0.2494 0.9752 -14.9631 -4.9399 35.9853 -0.0711 -0.2494 -0.9752 26.9936 -3.9426 16.0001 0.2136 0.9735 -0.1916 -26.9936 3.9426 -16.0001 -0.2136 -0.9735 0.1916 -16.9296 -14.9851 -11.9484 -0.9751 -0.2878 -0.1146 16.9296 14.9851 11.9484 0.9751 0.2878 0.1146 -23.0160 9.9737 13.9593 0.3665 -0.8590 -0.3281 -5.0418 10.9111 -33.0057 0.1839 -0.4780 0.8450 20.0367 -13.9294 8.0347 -0.3941 0.9169 -0.2333 -8.0225 9.0221 35.9455 0.6557 -0.2961 -0.6979 -0.0731 18.9321 -6.0497 0.8419 -0.3805 0.4295 8.9981 -3.0476 -40.9587 -0.4069 0.1965 0.9085 -4.9386 -13.9156 29.0170 -0.4572 0.2090 -0.8864 4.9858 4.0550 40.9565 0.5906 0.2215 -0.7805 3.9796 2.9286 -41.9753 -0.1821 -0.0767 0.9848 -28.9555 -5.0063 0.0130 -0.5184 -0.8104 -0.3115 26.9738 -0.0093 -18.9838 0.0998 0.7772 0.6260