# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 # Attachment '- CCDC_deposided_merged_cifs_notepad.cif' data_complete #TrackingRef '- CCDC_deposided_merged_cifs_notepad.cif' _audit_creation_date 08-07-29 _audit_creation_method CRYSTALS_ver_12.80 _publ_contact_author_name 'Sofia I. Pascu' _publ_contact_author_address ; Department of Chemistry University of Bath Claverton Downs Bath BA2 7AY UK ; _publ_contact_author_email s.pascu@bath.ac.uk _publ_contact_author_fax '(01225) 386627' _publ_contact_author_phone '(01225) 386231' _publ_author_name S.I.Pascu #=============================================================================== data_san0006 _database_code_depnum_ccdc_archive 'CCDC 715661' #TrackingRef '- CCDC_deposided_merged_cifs_notepad.cif' _audit_creation_date 05-12-19 _audit_creation_method CRYSTALS_ver_12.82 _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 13.629(2) _cell_length_b 16.504(3) _cell_length_c 16.554(3) _cell_angle_alpha 112.529(2) _cell_angle_beta 96.328(2) _cell_angle_gamma 104.184(2) _cell_volume 3246.8(10) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Zn 0.2839 1.4301 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097 1.3041 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 1 _chemical_formula_sum 'C147 H184 Cl2 N10 O4 Zn2' _chemical_formula_moiety '2(C60 H76 N4 Zn), C26 H30 N2 O4, C H2 Cl2' _chemical_compound_source ? _chemical_formula_weight 2356.72 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6484 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 28.47 _exptl_crystal_description lath _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'Bruker SADABS' # absolute Tmin and Tmax unknown, but SADABS gives ratio as 0.708 _exptl_special_details ; Crystal was extremly small and weakly diffracting. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.6709 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART APEX2 CCD diffractometer' _diffrn_measurement_method 'fine-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5 _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _exptl_crystal_density_diffrn 1.205 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1262 _exptl_absorpt_coefficient_mu 0.468 _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_reflns_number 24110 _reflns_number_total 11363 _diffrn_reflns_av_R_equivalents 0.033 # Number of reflections with Friedels Law is 11363 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 11470 _diffrn_reflns_theta_min 2.236 _diffrn_reflns_theta_max 23.536 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 21.653 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _reflns_limit_h_min -16 _reflns_limit_h_max 16 _reflns_limit_k_min -19 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.80 _refine_diff_density_max 1.13 _refine_ls_number_reflns 6579 _refine_ls_number_restraints 5 _refine_ls_number_parameters 742 #_refine_ls_R_factor_ref 0.0615 _refine_ls_wR_factor_ref 0.0621 _refine_ls_goodness_of_fit_ref 1.1489 #_reflns_number_all 11322 _refine_ls_R_factor_all 0.1045 _refine_ls_wR_factor_all 0.0774 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 6579 _refine_ls_R_factor_gt 0.0615 _refine_ls_wR_factor_gt 0.0621 _refine_ls_shift/su_max 0.042750 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.975 1.00 0.674 ; _publ_section_references ; Data collection: APEX2, Bruker AXS Inc., Madison, USA, 2004 Data reduction (frames integration): SAINT, Bruker AXS Inc., Madison, USA, 2004 Cell refinement: SAINT, Bruker AXS Inc., Madison, USA, 2004 Absorption correction: SADABS, Bruker AXS Inc., Madison, USA, 2004 Station 9.8: R. J. Cernik, W. Clegg, C. R. A. Catlow, G. Bushnell-Wye, J. V. Flaherty,G. N. Greaves, M. Hamichi, I. Burrows, D. J. Taylor and S. J. Teat, J. Synchotron Radiation 1997, 4, 279-286; 7, 40. Synchrotron chemical crystallography: W. Clegg, J. Chem. Soc., Dalton Trans. 2000, 3223-3232. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of G\"ottingen, Federal Republic of Germany. Watkin D.J. (1994). Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Zn1 Zn 0.17236(4) 0.00633(3) 0.04648(4) 0.0311 1.0000 Uani . . . . . . N1 N 0.1054(2) 0.0814(2) -0.0015(2) 0.0336 1.0000 Uani . . . . . . N2 N 0.1903(2) -0.0610(2) -0.0811(2) 0.0331 1.0000 Uani . . . . . . N3 N 0.2515(2) -0.0619(2) 0.0957(2) 0.0324 1.0000 Uani . . . . . . N4 N 0.1693(2) 0.0833(2) 0.1759(2) 0.0329 1.0000 Uani . . . . . . N5 N 0.3903(2) 0.1763(2) 0.0969(3) 0.0430 1.0000 Uani . . . . . . C1 C 0.0933(3) 0.0820(3) -0.0846(3) 0.0335 1.0000 Uani . . . . . . C2 C 0.0430(3) 0.1502(3) -0.0851(3) 0.0379 1.0000 Uani . . . . . . C3 C 0.0250(3) 0.1894(3) -0.0025(3) 0.0342 1.0000 Uani . . . . . . C4 C 0.0649(3) 0.1472(3) 0.0502(3) 0.0324 1.0000 Uani . . . . . . C5 C 0.0713(3) 0.1770(3) 0.1416(3) 0.0362 1.0000 Uani . . . . . . C6 C 0.1223(3) 0.1505(2) 0.2001(3) 0.0346 1.0000 Uani . . . . . . C7 C 0.1396(3) 0.1965(3) 0.2960(3) 0.0380 1.0000 Uani . . . . . . C8 C 0.1980(3) 0.1569(3) 0.3314(3) 0.0380 1.0000 Uani . . . . . . C9 C 0.2143(3) 0.0832(3) 0.2538(3) 0.0360 1.0000 Uani . . . . . . C10 C 0.2662(3) 0.0199(3) 0.2582(3) 0.0355 1.0000 Uani . . . . . . C11 C 0.2824(3) -0.0490(3) 0.1833(3) 0.0333 1.0000 Uani . . . . . . C12 C 0.3349(3) -0.1171(3) 0.1839(3) 0.0353 1.0000 Uani . . . . . . C13 C 0.3313(3) -0.1696(3) 0.0966(3) 0.0350 1.0000 Uani . . . . . . C14 C 0.2810(3) -0.1343(2) 0.0421(3) 0.0344 1.0000 Uani . . . . . . C15 C 0.2701(3) -0.1660(2) -0.0493(3) 0.0327 1.0000 Uani . . . . . . C16 C 0.2294(3) -0.1338(2) -0.1070(3) 0.0318 1.0000 Uani . . . . . . C17 C 0.2279(3) -0.1684(3) -0.2008(3) 0.0363 1.0000 Uani . . . . . . C18 C 0.1892(3) -0.1150(3) -0.2332(3) 0.0415 1.0000 Uani . . . . . . C19 C 0.1659(3) -0.0468(3) -0.1563(3) 0.0348 1.0000 Uani . . . . . . C20 C 0.1256(3) 0.0248(3) -0.1565(3) 0.0377 1.0000 Uani . . . . . . C21 C 0.1238(3) 0.0445(3) -0.2374(3) 0.0375 1.0000 Uani . . . . . . C22 C 0.2103(3) 0.1069(3) -0.2401(3) 0.0437 1.0000 Uani . . . . . . C23 C 0.2120(4) 0.1300(3) -0.3129(3) 0.0518 1.0000 Uani . . . . . . C24 C 0.1257(4) 0.0908(3) -0.3820(3) 0.0551 1.0000 Uani . . . . . . C25 C 0.0388(4) 0.0289(3) -0.3804(3) 0.0531 1.0000 Uani . . . . . . C26 C 0.0369(3) 0.0055(3) -0.3085(3) 0.0480 1.0000 Uani . . . . . . C27 C 0.3071(3) 0.0273(3) 0.3486(3) 0.0368 1.0000 Uani . . . . . . C28 C 0.4074(3) 0.0832(3) 0.3977(3) 0.0480 1.0000 Uani . . . . . . C29 C 0.4431(4) 0.0892(4) 0.4811(4) 0.0624 1.0000 Uani . . . . . . C30 C 0.3802(4) 0.0410(4) 0.5187(3) 0.0630 1.0000 Uani . . . . . . C31 C 0.2809(4) -0.0153(3) 0.4712(3) 0.0555 1.0000 Uani . . . . . . C32 C 0.2441(3) -0.0220(3) 0.3859(3) 0.0419 1.0000 Uani . . . . . . C33 C 0.2335(4) 0.1864(3) 0.4291(3) 0.0544 1.0000 Uani . . . . . . C34 C 0.3883(4) -0.1269(3) 0.2615(3) 0.0486 1.0000 Uani . . . . . . C35 C 0.1732(4) -0.1290(3) -0.3292(3) 0.0541 1.0000 Uani . . . . . . C36 C 0.0134(4) 0.1786(4) -0.1584(3) 0.0576 1.0000 Uani . . . . . . C37 C -0.0186(3) 0.2680(3) 0.0343(3) 0.0360 1.0000 Uani . . . . . . C38 C 0.0655(3) 0.3614(3) 0.0779(3) 0.0390 1.0000 Uani . . . . . . C39 C 0.0229(3) 0.4421(3) 0.1100(3) 0.0426 1.0000 Uani . . . . . . C40 C 0.1050(3) 0.5353(3) 0.1618(3) 0.0453 1.0000 Uani . . . . . . C41 C 0.0636(4) 0.6168(3) 0.1895(4) 0.0555 1.0000 Uani . . . . . . C42 C 0.1454(4) 0.7087(3) 0.2453(4) 0.0599 1.0000 Uani . . . . . . C43 C 0.1036(3) 0.2780(3) 0.3448(3) 0.0414 1.0000 Uani . . . . . . C44 C 0.1820(3) 0.3695(3) 0.3597(3) 0.0435 1.0000 Uani . . . . . . C45 C 0.1452(4) 0.4534(3) 0.3987(3) 0.0467 1.0000 Uani . . . . . . C46 C 0.2282(4) 0.5420(3) 0.4187(3) 0.0522 1.0000 Uani . . . . . . C47 C 0.1939(4) 0.6289(3) 0.4538(4) 0.0602 1.0000 Uani . . . . . . C48 C 0.2818(5) 0.7164(4) 0.4748(4) 0.0726 1.0000 Uani . . . . . . C49 C 0.2613(3) -0.2509(3) -0.2516(3) 0.0422 1.0000 Uani . . . . . . C50 C 0.1771(3) -0.3426(3) -0.2767(3) 0.0427 1.0000 Uani . . . . . . C51 C 0.2164(4) -0.4254(3) -0.3130(3) 0.0473 1.0000 Uani . . . . . . C52 C 0.1319(5) -0.5164(3) -0.3399(4) 0.0615 1.0000 Uani . . . . . . C53 C 0.1686(6) -0.6007(4) -0.3724(4) 0.0742 1.0000 Uani . . . . . . C54 C 0.0815(7) -0.6902(4) -0.3989(5) 0.1097 1.0000 Uani . . . . . . C55 C 0.3729(3) -0.2503(3) 0.0587(3) 0.0384 1.0000 Uani . . . . . . C56 C 0.2869(3) -0.3437(3) 0.0160(3) 0.0430 1.0000 Uani . . . . . . C57 C 0.3270(3) -0.4245(3) -0.0266(3) 0.0451 1.0000 Uani . . . . . . C58 C 0.2394(4) -0.5163(3) -0.0763(4) 0.0587 1.0000 Uani . . . . . . C59 C 0.2747(4) -0.6008(3) -0.1233(4) 0.0598 1.0000 Uani . . . . . . C60 C 0.3377(6) -0.6234(4) -0.0606(5) 0.0867 1.0000 Uani . . . . . . C61 C 0.3880(3) 0.1459(3) 0.0056(3) 0.0400 1.0000 Uani . . . . . . C62 C 0.4322(3) 0.0702(3) -0.0355(3) 0.0364 1.0000 Uani . . . . . . C63 C 0.4780(3) 0.0360(3) 0.0200(3) 0.0319 1.0000 Uani . . . . . . C64 C 0.4835(3) 0.0710(3) 0.1119(3) 0.0374 1.0000 Uani . . . . . . C65 C 0.4404(3) 0.1481(3) 0.1550(3) 0.0410 1.0000 Uani . . . . . . C66 C 0.4285(3) 0.0343(3) -0.1253(3) 0.0399 1.0000 Uani . . . . . . C67 C 0.5302(3) 0.0376(3) 0.1669(3) 0.0405 1.0000 Uani . . . . . . C68 C 0.3498(3) 0.2543(3) 0.1376(3) 0.0474 1.0000 Uani . . . . . . C69 C 0.4328(3) 0.3462(3) 0.1613(4) 0.0529 1.0000 Uani . . . . . . C70 C 0.3925(3) 0.4282(3) 0.2020(4) 0.0573 1.0000 Uani . . . . . . C71 C 0.4731(4) 0.5189(3) 0.2215(4) 0.0547 1.0000 Uani . . . . . . C72 C 0.4388(4) 0.6037(3) 0.2649(4) 0.0636 1.0000 Uani . . . . . . C73 C 0.5239(4) 0.6934(3) 0.2889(4) 0.0647 1.0000 Uani . . . . . . O1 O 0.4484(2) 0.1848(2) 0.2355(2) 0.0527 1.0000 Uani . . . . . . O2 O 0.3530(2) 0.1821(2) -0.0372(2) 0.0491 1.0000 Uani . . . . . . C74 C 0.4726(16) 0.3526(7) 0.4193(8) 0.166(2) 0.5000 Uiso D U . . . . Cl1 Cl 0.4611(5) 0.3778(5) 0.5188(5) 0.1659(19) 0.5000 Uiso D U . . . . Cl2 Cl 0.5427(5) 0.4234(5) 0.3925(5) 0.173(2) 0.5000 Uiso D U . . . . H51 H 0.0348 0.2231 0.1688 0.0441 1.0000 Uiso . . . . . . H151 H 0.2950 -0.2201 -0.0783 0.0372 1.0000 Uiso . . . . . . H221 H 0.2728 0.1361 -0.1890 0.0517 1.0000 Uiso . . . . . . H231 H 0.2756 0.1746 -0.3146 0.0625 1.0000 Uiso . . . . . . H241 H 0.1260 0.1075 -0.4340 0.0687 1.0000 Uiso . . . . . . H251 H -0.0236 0.0004 -0.4315 0.0613 1.0000 Uiso . . . . . . H261 H -0.0269 -0.0395 -0.3076 0.0544 1.0000 Uiso . . . . . . H281 H 0.4537 0.1190 0.3719 0.0534 1.0000 Uiso . . . . . . H291 H 0.5154 0.1290 0.5153 0.0709 1.0000 Uiso . . . . . . H301 H 0.4068 0.0470 0.5801 0.0758 1.0000 Uiso . . . . . . H311 H 0.2355 -0.0511 0.4977 0.0702 1.0000 Uiso . . . . . . H321 H 0.1721 -0.0626 0.3513 0.0519 1.0000 Uiso . . . . . . H331 H 0.2751 0.1475 0.4391 0.0725 1.0000 Uiso . . . . . . H332 H 0.2776 0.2527 0.4579 0.0725 1.0000 Uiso . . . . . . H333 H 0.1718 0.1790 0.4563 0.0725 1.0000 Uiso . . . . . . H341 H 0.4158 -0.1804 0.2390 0.0586 1.0000 Uiso . . . . . . H342 H 0.4471 -0.0692 0.2992 0.0586 1.0000 Uiso . . . . . . H343 H 0.3378 -0.1378 0.2986 0.0586 1.0000 Uiso . . . . . . H351 H 0.1442 -0.0812 -0.3359 0.0669 1.0000 Uiso . . . . . . H352 H 0.2412 -0.1231 -0.3475 0.0669 1.0000 Uiso . . . . . . H353 H 0.1235 -0.1919 -0.3684 0.0669 1.0000 Uiso . . . . . . H361 H -0.0202 0.2280 -0.1354 0.0725 1.0000 Uiso . . . . . . H362 H 0.0771 0.2028 -0.1774 0.0725 1.0000 Uiso . . . . . . H363 H -0.0364 0.1240 -0.2110 0.0725 1.0000 Uiso . . . . . . H371 H -0.0679 0.2667 -0.0160 0.0441 1.0000 Uiso . . . . . . H372 H -0.0569 0.2599 0.0803 0.0441 1.0000 Uiso . . . . . . H381 H 0.1068 0.3674 0.0330 0.0489 1.0000 Uiso . . . . . . H382 H 0.1118 0.3640 0.1307 0.0489 1.0000 Uiso . . . . . . H391 H -0.0175 0.4429 0.0562 0.0518 1.0000 Uiso . . . . . . H392 H -0.0244 0.4324 0.1497 0.0518 1.0000 Uiso . . . . . . H401 H 0.1548 0.5433 0.1232 0.0549 1.0000 Uiso . . . . . . H402 H 0.1426 0.5356 0.2173 0.0549 1.0000 Uiso . . . . . . H411 H 0.0296 0.6188 0.1339 0.0643 1.0000 Uiso . . . . . . H412 H 0.0109 0.6072 0.2252 0.0643 1.0000 Uiso . . . . . . H421 H 0.1122 0.7588 0.2609 0.0689 1.0000 Uiso . . . . . . H422 H 0.1985 0.7199 0.2104 0.0689 1.0000 Uiso . . . . . . H423 H 0.1798 0.7083 0.3017 0.0689 1.0000 Uiso . . . . . . H431 H 0.0945 0.2797 0.4045 0.0550 1.0000 Uiso . . . . . . H432 H 0.0356 0.2704 0.3085 0.0550 1.0000 Uiso . . . . . . H441 H 0.2470 0.3799 0.4019 0.0538 1.0000 Uiso . . . . . . H442 H 0.1975 0.3640 0.3005 0.0538 1.0000 Uiso . . . . . . H451 H 0.1244 0.4568 0.4557 0.0580 1.0000 Uiso . . . . . . H452 H 0.0838 0.4462 0.3545 0.0580 1.0000 Uiso . . . . . . H461 H 0.2879 0.5501 0.4650 0.0613 1.0000 Uiso . . . . . . H462 H 0.2514 0.5365 0.3621 0.0613 1.0000 Uiso . . . . . . H471 H 0.1693 0.6344 0.5099 0.0755 1.0000 Uiso . . . . . . H472 H 0.1355 0.6224 0.4071 0.0755 1.0000 Uiso . . . . . . H481 H 0.2560 0.7710 0.4974 0.0867 1.0000 Uiso . . . . . . H482 H 0.3404 0.7239 0.5218 0.0867 1.0000 Uiso . . . . . . H483 H 0.3066 0.7118 0.4191 0.0867 1.0000 Uiso . . . . . . H491 H 0.2778 -0.2478 -0.3080 0.0481 1.0000 Uiso . . . . . . H492 H 0.3249 -0.2485 -0.2133 0.0481 1.0000 Uiso . . . . . . H501 H 0.1185 -0.3500 -0.3237 0.0494 1.0000 Uiso . . . . . . H502 H 0.1514 -0.3408 -0.2219 0.0494 1.0000 Uiso . . . . . . H511 H 0.2436 -0.4263 -0.3669 0.0590 1.0000 Uiso . . . . . . H512 H 0.2738 -0.4188 -0.2654 0.0590 1.0000 Uiso . . . . . . H521 H 0.0762 -0.5238 -0.3892 0.0776 1.0000 Uiso . . . . . . H522 H 0.1025 -0.5137 -0.2865 0.0776 1.0000 Uiso . . . . . . H531 H 0.1980 -0.6039 -0.4259 0.0948 1.0000 Uiso . . . . . . H532 H 0.2239 -0.5940 -0.3232 0.0948 1.0000 Uiso . . . . . . H541 H 0.1097 -0.7434 -0.4198 0.1415 1.0000 Uiso . . . . . . H542 H 0.0258 -0.6980 -0.4485 0.1415 1.0000 Uiso . . . . . . H543 H 0.0517 -0.6881 -0.3459 0.1415 1.0000 Uiso . . . . . . H551 H 0.4227 -0.2494 0.1084 0.0466 1.0000 Uiso . . . . . . H552 H 0.4102 -0.2432 0.0119 0.0466 1.0000 Uiso . . . . . . H561 H 0.2522 -0.3522 0.0637 0.0507 1.0000 Uiso . . . . . . H562 H 0.2351 -0.3432 -0.0314 0.0507 1.0000 Uiso . . . . . . H571 H 0.3736 -0.4288 0.0217 0.0556 1.0000 Uiso . . . . . . H572 H 0.3674 -0.4133 -0.0702 0.0556 1.0000 Uiso . . . . . . H581 H 0.2005 -0.5275 -0.0318 0.0669 1.0000 Uiso . . . . . . H582 H 0.1919 -0.5105 -0.1229 0.0669 1.0000 Uiso . . . . . . H591 H 0.2115 -0.6554 -0.1585 0.0702 1.0000 Uiso . . . . . . H592 H 0.3173 -0.5884 -0.1652 0.0702 1.0000 Uiso . . . . . . H601 H 0.3579 -0.6788 -0.0957 0.1123 1.0000 Uiso . . . . . . H602 H 0.2959 -0.6368 -0.0186 0.1123 1.0000 Uiso . . . . . . H603 H 0.4018 -0.5698 -0.0254 0.1123 1.0000 Uiso . . . . . . H661 H 0.3955 0.0599 -0.1629 0.0511 1.0000 Uiso . . . . . . H671 H 0.5342 0.0639 0.2330 0.0447 1.0000 Uiso . . . . . . H681 H 0.3286 0.2540 0.1934 0.0567 1.0000 Uiso . . . . . . H682 H 0.2880 0.2474 0.0939 0.0567 1.0000 Uiso . . . . . . H691 H 0.4940 0.3533 0.2056 0.0650 1.0000 Uiso . . . . . . H692 H 0.4547 0.3457 0.1055 0.0650 1.0000 Uiso . . . . . . H701 H 0.3737 0.4304 0.2594 0.0686 1.0000 Uiso . . . . . . H702 H 0.3293 0.4196 0.1588 0.0686 1.0000 Uiso . . . . . . H711 H 0.5370 0.5256 0.2627 0.0638 1.0000 Uiso . . . . . . H712 H 0.4899 0.5166 0.1635 0.0638 1.0000 Uiso . . . . . . H721 H 0.4176 0.6042 0.3210 0.0733 1.0000 Uiso . . . . . . H722 H 0.3780 0.5995 0.2221 0.0733 1.0000 Uiso . . . . . . H731 H 0.4972 0.7466 0.3171 0.0762 1.0000 Uiso . . . . . . H732 H 0.5850 0.6987 0.3322 0.0762 1.0000 Uiso . . . . . . H733 H 0.5453 0.6940 0.2333 0.0762 1.0000 Uiso . . . . . . H741 H 0.4992 0.2982 0.4015 0.1996 0.5000 Uiso . . . . . . H742 H 0.4008 0.3334 0.3820 0.1996 0.5000 Uiso . . . . . . 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 0.0269(2) 0.0280(2) 0.0401(3) 0.01374(19) 0.01221(19) 0.01066(17) N1 0.0298(16) 0.0301(16) 0.041(2) 0.0140(15) 0.0110(15) 0.0099(14) N2 0.0262(15) 0.0290(16) 0.041(2) 0.0117(15) 0.0106(15) 0.0078(13) N3 0.0272(15) 0.0295(17) 0.041(2) 0.0131(15) 0.0132(15) 0.0102(14) N4 0.0354(17) 0.0269(16) 0.042(2) 0.0169(15) 0.0162(15) 0.0120(14) N5 0.0293(17) 0.0319(17) 0.070(3) 0.0221(18) 0.0163(17) 0.0116(15) C1 0.0259(18) 0.034(2) 0.039(2) 0.0154(18) 0.0063(17) 0.0079(16) C2 0.028(2) 0.037(2) 0.046(3) 0.0156(19) 0.0027(18) 0.0123(17) C3 0.0233(18) 0.0306(19) 0.047(3) 0.0152(18) 0.0052(17) 0.0082(16) C4 0.0228(18) 0.0282(19) 0.044(3) 0.0127(18) 0.0141(17) 0.0067(16) C5 0.030(2) 0.0283(19) 0.052(3) 0.0154(19) 0.0148(19) 0.0122(17) C6 0.034(2) 0.0245(18) 0.050(3) 0.0167(18) 0.0208(19) 0.0107(17) C7 0.039(2) 0.0297(19) 0.055(3) 0.0211(19) 0.024(2) 0.0157(17) C8 0.045(2) 0.033(2) 0.041(2) 0.0164(18) 0.0189(19) 0.0146(18) C9 0.035(2) 0.032(2) 0.046(3) 0.0183(18) 0.0180(19) 0.0118(17) C10 0.0305(19) 0.033(2) 0.045(3) 0.0176(18) 0.0137(18) 0.0105(16) C11 0.0277(18) 0.0283(19) 0.042(2) 0.0117(17) 0.0110(17) 0.0084(16) C12 0.0239(18) 0.033(2) 0.049(3) 0.0175(19) 0.0088(17) 0.0088(16) C13 0.0272(18) 0.0265(19) 0.050(3) 0.0146(18) 0.0116(18) 0.0083(16) C14 0.030(2) 0.0247(19) 0.046(3) 0.0128(18) 0.0104(18) 0.0072(17) C15 0.0260(18) 0.0251(18) 0.042(2) 0.0085(18) 0.0130(17) 0.0065(16) C16 0.0257(18) 0.0255(18) 0.042(2) 0.0109(17) 0.0121(17) 0.0074(16) C17 0.0264(19) 0.031(2) 0.045(2) 0.0109(18) 0.0105(17) 0.0049(16) C18 0.037(2) 0.035(2) 0.046(3) 0.0128(19) 0.0145(19) 0.0048(18) C19 0.0280(19) 0.039(2) 0.038(2) 0.0187(19) 0.0093(17) 0.0084(17) C20 0.0283(19) 0.035(2) 0.045(3) 0.0161(19) 0.0056(18) 0.0036(17) C21 0.036(2) 0.036(2) 0.042(2) 0.0160(18) 0.0090(18) 0.0143(18) C22 0.038(2) 0.039(2) 0.052(3) 0.023(2) 0.002(2) 0.0069(18) C23 0.050(3) 0.043(2) 0.063(3) 0.030(2) 0.011(2) 0.005(2) C24 0.063(3) 0.057(3) 0.052(3) 0.029(2) 0.014(2) 0.019(2) C25 0.054(3) 0.060(3) 0.039(3) 0.018(2) 0.008(2) 0.014(2) C26 0.042(2) 0.050(3) 0.043(3) 0.016(2) 0.010(2) 0.008(2) C27 0.038(2) 0.036(2) 0.039(2) 0.0145(18) 0.0110(18) 0.0169(18) C28 0.044(2) 0.039(2) 0.050(3) 0.008(2) 0.009(2) 0.014(2) C29 0.048(3) 0.068(3) 0.061(3) 0.013(3) 0.008(2) 0.027(3) C30 0.078(4) 0.068(3) 0.043(3) 0.015(2) 0.000(3) 0.045(3) C31 0.068(3) 0.056(3) 0.052(3) 0.026(2) 0.017(3) 0.028(3) C32 0.046(2) 0.042(2) 0.042(3) 0.0194(19) 0.009(2) 0.0183(19) C33 0.081(3) 0.053(3) 0.048(3) 0.023(2) 0.029(2) 0.042(3) C34 0.050(2) 0.039(2) 0.057(3) 0.016(2) 0.009(2) 0.024(2) C35 0.080(3) 0.044(2) 0.043(3) 0.017(2) 0.024(2) 0.026(2) C36 0.065(3) 0.064(3) 0.051(3) 0.022(2) 0.011(2) 0.040(3) C37 0.0259(19) 0.037(2) 0.048(3) 0.0186(19) 0.0077(17) 0.0129(17) C38 0.0287(19) 0.037(2) 0.057(3) 0.022(2) 0.0137(19) 0.0133(17) C39 0.037(2) 0.038(2) 0.054(3) 0.020(2) 0.014(2) 0.0130(19) C40 0.042(2) 0.036(2) 0.059(3) 0.020(2) 0.016(2) 0.0134(19) C41 0.061(3) 0.039(2) 0.062(3) 0.015(2) 0.012(2) 0.017(2) C42 0.074(3) 0.041(2) 0.057(3) 0.019(2) 0.007(3) 0.012(2) C43 0.051(2) 0.039(2) 0.047(3) 0.021(2) 0.026(2) 0.025(2) C44 0.048(2) 0.037(2) 0.049(3) 0.0164(19) 0.019(2) 0.0195(19) C45 0.058(3) 0.036(2) 0.051(3) 0.018(2) 0.018(2) 0.021(2) C46 0.060(3) 0.041(2) 0.052(3) 0.014(2) 0.016(2) 0.019(2) C47 0.081(3) 0.038(2) 0.069(3) 0.024(2) 0.033(3) 0.024(2) C48 0.103(4) 0.044(3) 0.069(4) 0.019(3) 0.033(3) 0.024(3) C49 0.040(2) 0.035(2) 0.045(3) 0.0081(19) 0.0177(19) 0.0121(18) C50 0.044(2) 0.034(2) 0.046(2) 0.0104(18) 0.0128(19) 0.0141(19) C51 0.059(3) 0.041(2) 0.047(3) 0.017(2) 0.017(2) 0.025(2) C52 0.092(4) 0.036(2) 0.065(3) 0.020(2) 0.046(3) 0.026(3) C53 0.122(5) 0.048(3) 0.067(4) 0.024(3) 0.041(4) 0.044(3) C54 0.182(8) 0.042(3) 0.130(6) 0.035(3) 0.111(6) 0.047(4) C55 0.034(2) 0.032(2) 0.051(3) 0.0163(19) 0.0111(18) 0.0142(17) C56 0.038(2) 0.031(2) 0.058(3) 0.015(2) 0.016(2) 0.0102(18) C57 0.042(2) 0.034(2) 0.063(3) 0.019(2) 0.019(2) 0.0175(19) C58 0.050(3) 0.032(2) 0.085(4) 0.015(2) 0.024(3) 0.010(2) C59 0.055(3) 0.035(2) 0.086(4) 0.017(2) 0.028(3) 0.017(2) C60 0.126(5) 0.057(3) 0.097(5) 0.035(3) 0.038(4) 0.055(4) C61 0.0237(19) 0.036(2) 0.059(3) 0.020(2) 0.0101(19) 0.0064(17) C62 0.0238(18) 0.0285(19) 0.057(3) 0.019(2) 0.0104(18) 0.0051(16) C63 0.0221(17) 0.0297(18) 0.044(2) 0.0163(17) 0.0055(16) 0.0072(15) C64 0.0247(18) 0.034(2) 0.054(3) 0.021(2) 0.0129(18) 0.0061(17) C65 0.0265(19) 0.030(2) 0.062(3) 0.016(2) 0.015(2) 0.0068(17) C66 0.0247(19) 0.044(2) 0.059(3) 0.029(2) 0.0119(19) 0.0116(18) C67 0.032(2) 0.038(2) 0.042(3) 0.012(2) 0.0061(18) 0.0035(18) C68 0.036(2) 0.032(2) 0.074(3) 0.017(2) 0.022(2) 0.0151(18) C69 0.040(2) 0.037(2) 0.085(4) 0.022(2) 0.031(2) 0.017(2) C70 0.040(2) 0.040(2) 0.091(4) 0.022(2) 0.028(2) 0.015(2) C71 0.047(2) 0.035(2) 0.078(3) 0.017(2) 0.025(2) 0.011(2) C72 0.055(3) 0.042(3) 0.086(4) 0.016(3) 0.026(3) 0.017(2) C73 0.070(3) 0.037(2) 0.083(4) 0.020(2) 0.021(3) 0.018(2) O1 0.0490(17) 0.0441(17) 0.061(2) 0.0153(16) 0.0270(16) 0.0138(15) O2 0.0356(15) 0.0412(16) 0.073(2) 0.0257(16) 0.0069(15) 0.0157(14) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.1476(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zn1 . N1 . 2.037(3) yes Zn1 . N2 . 2.050(3) yes Zn1 . N3 . 2.050(3) yes Zn1 . N4 . 2.041(3) yes N1 . C1 . 1.370(5) yes N1 . C4 . 1.380(5) yes N2 . C16 . 1.371(5) yes N2 . C19 . 1.374(5) yes N3 . C11 . 1.381(5) yes N3 . C14 . 1.370(5) yes N4 . C6 . 1.365(5) yes N4 . C9 . 1.367(5) yes N5 . C61 . 1.392(6) yes N5 . C65 . 1.401(6) yes N5 . C68 . 1.478(5) yes C1 . C2 . 1.456(5) yes C1 . C20 . 1.401(6) yes C2 . C3 . 1.350(6) yes C2 . C36 . 1.510(7) yes C3 . C4 . 1.445(6) yes C3 . C37 . 1.504(5) yes C4 . C5 . 1.384(6) yes C5 . C6 . 1.393(6) yes C5 . H51 . 1.000 no C6 . C7 . 1.434(6) yes C7 . C8 . 1.360(6) yes C7 . C43 . 1.511(5) yes C8 . C9 . 1.476(5) yes C8 . C33 . 1.482(7) yes C9 . C10 . 1.416(5) yes C10 . C11 . 1.409(6) yes C10 . C27 . 1.485(6) yes C11 . C12 . 1.474(5) yes C12 . C13 . 1.358(6) yes C12 . C34 . 1.491(6) yes C13 . C14 . 1.445(6) yes C13 . C55 . 1.516(5) yes C14 . C15 . 1.376(6) yes C15 . C16 . 1.384(6) yes C15 . H151 . 1.000 no C16 . C17 . 1.430(6) yes C17 . C18 . 1.367(6) yes C17 . C49 . 1.510(6) yes C18 . C19 . 1.469(6) yes C18 . C35 . 1.498(7) yes C19 . C20 . 1.419(6) yes C20 . C21 . 1.492(6) yes C21 . C22 . 1.380(6) yes C21 . C26 . 1.393(6) yes C22 . C23 . 1.399(6) yes C22 . H221 . 1.000 no C23 . C24 . 1.368(7) yes C23 . H231 . 1.000 no C24 . C25 . 1.372(7) yes C24 . H241 . 1.000 no C25 . C26 . 1.387(7) yes C25 . H251 . 1.000 no C26 . H261 . 1.000 no C27 . C28 . 1.395(6) yes C27 . C32 . 1.392(6) yes C28 . C29 . 1.368(7) yes C28 . H281 . 1.000 no C29 . C30 . 1.385(8) yes C29 . H291 . 1.000 no C30 . C31 . 1.379(7) yes C30 . H301 . 1.000 no C31 . C32 . 1.399(7) yes C31 . H311 . 1.000 no C32 . H321 . 1.000 no C33 . H331 . 1.000 no C33 . H332 . 1.000 no C33 . H333 . 1.000 no C34 . H341 . 1.000 no C34 . H342 . 1.000 no C34 . H343 . 1.000 no C35 . H351 . 1.000 no C35 . H352 . 1.000 no C35 . H353 . 1.000 no C36 . H361 . 1.000 no C36 . H362 . 1.000 no C36 . H363 . 1.000 no C37 . C38 . 1.520(6) yes C37 . H371 . 1.000 no C37 . H372 . 1.000 no C38 . C39 . 1.516(6) yes C38 . H381 . 1.000 no C38 . H382 . 1.000 no C39 . C40 . 1.512(6) yes C39 . H391 . 1.000 no C39 . H392 . 1.000 no C40 . C41 . 1.514(6) yes C40 . H401 . 1.000 no C40 . H402 . 1.000 no C41 . C42 . 1.505(7) yes C41 . H411 . 1.000 no C41 . H412 . 1.000 no C42 . H421 . 1.000 no C42 . H422 . 1.000 no C42 . H423 . 1.000 no C43 . C44 . 1.533(6) yes C43 . H431 . 1.000 no C43 . H432 . 1.000 no C44 . C45 . 1.521(6) yes C44 . H441 . 1.000 no C44 . H442 . 1.000 no C45 . C46 . 1.504(6) yes C45 . H451 . 1.000 no C45 . H452 . 1.000 no C46 . C47 . 1.537(6) yes C46 . H461 . 1.000 no C46 . H462 . 1.000 no C47 . C48 . 1.522(8) yes C47 . H471 . 1.000 no C47 . H472 . 1.000 no C48 . H481 . 1.000 no C48 . H482 . 1.000 no C48 . H483 . 1.000 no C49 . C50 . 1.530(6) yes C49 . H491 . 1.000 no C49 . H492 . 1.000 no C50 . C51 . 1.523(6) yes C50 . H501 . 1.000 no C50 . H502 . 1.000 no C51 . C52 . 1.519(7) yes C51 . H511 . 1.000 no C51 . H512 . 1.000 no C52 . C53 . 1.516(7) yes C52 . H521 . 1.000 no C52 . H522 . 1.000 no C53 . C54 . 1.521(9) yes C53 . H531 . 1.000 no C53 . H532 . 1.000 no C54 . H541 . 1.000 no C54 . H542 . 1.000 no C54 . H543 . 1.000 no C55 . C56 . 1.531(6) yes C55 . H551 . 1.000 no C55 . H552 . 1.000 no C56 . C57 . 1.515(6) yes C56 . H561 . 1.000 no C56 . H562 . 1.000 no C57 . C58 . 1.529(6) yes C57 . H571 . 1.000 no C57 . H572 . 1.000 no C58 . C59 . 1.537(6) yes C58 . H581 . 1.000 no C58 . H582 . 1.000 no C59 . C60 . 1.487(9) yes C59 . H591 . 1.000 no C59 . H592 . 1.000 no C60 . H601 . 1.000 no C60 . H602 . 1.000 no C60 . H603 . 1.000 no C61 . C62 . 1.482(6) yes C61 . O2 . 1.215(5) yes C62 . C63 . 1.413(6) yes C62 . C66 . 1.362(6) yes C63 . C63 2_655 1.430(8) yes C63 . C64 . 1.392(6) yes C64 . C65 . 1.495(6) yes C64 . C67 . 1.401(6) yes C65 . O1 . 1.212(6) yes C66 . C67 2_655 1.410(6) yes C66 . H661 . 1.000 no C67 . H671 . 1.000 no C68 . C69 . 1.529(6) yes C68 . H681 . 1.000 no C68 . H682 . 1.000 no C69 . C70 . 1.528(6) yes C69 . H691 . 1.000 no C69 . H692 . 1.000 no C70 . C71 . 1.516(6) yes C70 . H701 . 1.000 no C70 . H702 . 1.000 no C71 . C72 . 1.522(7) yes C71 . H711 . 1.000 no C71 . H712 . 1.000 no C72 . C73 . 1.517(7) yes C72 . H721 . 1.000 no C72 . H722 . 1.000 no C73 . H731 . 1.000 no C73 . H732 . 1.000 no C73 . H733 . 1.000 no C74 . Cl1 . 1.573(13) yes C74 . Cl2 . 1.554(13) yes C74 . H741 . 1.002 no C74 . H742 . 1.002 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Zn1 . N2 . 86.89(13) yes N1 . Zn1 . N3 . 175.25(13) yes N2 . Zn1 . N3 . 92.42(13) yes N1 . Zn1 . N4 . 92.94(13) yes N2 . Zn1 . N4 . 173.96(13) yes N3 . Zn1 . N4 . 87.25(13) yes Zn1 . N1 . C1 . 130.4(3) yes Zn1 . N1 . C4 . 123.2(3) yes C1 . N1 . C4 . 106.3(3) yes Zn1 . N2 . C16 . 124.0(3) yes Zn1 . N2 . C19 . 129.6(3) yes C16 . N2 . C19 . 106.4(3) yes Zn1 . N3 . C11 . 129.6(2) yes Zn1 . N3 . C14 . 123.3(3) yes C11 . N3 . C14 . 107.1(3) yes Zn1 . N4 . C6 . 123.8(3) yes Zn1 . N4 . C9 . 129.6(2) yes C6 . N4 . C9 . 106.5(3) yes C61 . N5 . C65 . 125.4(4) yes C61 . N5 . C68 . 116.5(4) yes C65 . N5 . C68 . 117.5(4) yes N1 . C1 . C2 . 109.7(3) yes N1 . C1 . C20 . 123.8(4) yes C2 . C1 . C20 . 126.5(4) yes C1 . C2 . C3 . 107.1(4) yes C1 . C2 . C36 . 130.9(4) yes C3 . C2 . C36 . 122.0(4) yes C2 . C3 . C4 . 107.0(3) yes C2 . C3 . C37 . 128.6(4) yes C4 . C3 . C37 . 124.2(4) yes C3 . C4 . N1 . 109.9(4) yes C3 . C4 . C5 . 123.8(4) yes N1 . C4 . C5 . 125.9(4) yes C4 . C5 . C6 . 127.8(4) yes C4 . C5 . H51 . 116.1 no C6 . C5 . H51 . 116.1 no C5 . C6 . N4 . 125.7(4) yes C5 . C6 . C7 . 123.5(3) yes N4 . C6 . C7 . 110.7(4) yes C6 . C7 . C8 . 107.4(3) yes C6 . C7 . C43 . 124.1(4) yes C8 . C7 . C43 . 128.3(4) yes C7 . C8 . C9 . 105.7(4) yes C7 . C8 . C33 . 123.8(4) yes C9 . C8 . C33 . 130.6(4) yes C8 . C9 . N4 . 109.6(3) yes C8 . C9 . C10 . 125.8(4) yes N4 . C9 . C10 . 124.6(4) yes C9 . C10 . C11 . 124.7(4) yes C9 . C10 . C27 . 117.5(3) yes C11 . C10 . C27 . 117.8(3) yes C10 . C11 . N3 . 124.0(3) yes C10 . C11 . C12 . 127.0(4) yes N3 . C11 . C12 . 109.0(3) yes C11 . C12 . C13 . 106.2(4) yes C11 . C12 . C34 . 129.5(4) yes C13 . C12 . C34 . 124.2(4) yes C12 . C13 . C14 . 107.9(3) yes C12 . C13 . C55 . 128.5(4) yes C14 . C13 . C55 . 123.6(4) yes C13 . C14 . N3 . 109.8(4) yes C13 . C14 . C15 . 124.5(4) yes N3 . C14 . C15 . 125.6(4) yes C14 . C15 . C16 . 129.3(4) yes C14 . C15 . H151 . 115.4 no C16 . C15 . H151 . 115.4 no C15 . C16 . N2 . 124.6(4) yes C15 . C16 . C17 . 124.7(3) yes N2 . C16 . C17 . 110.6(4) yes C16 . C17 . C18 . 107.5(3) yes C16 . C17 . C49 . 124.2(4) yes C18 . C17 . C49 . 128.3(4) yes C17 . C18 . C19 . 105.8(4) yes C17 . C18 . C35 . 124.8(4) yes C19 . C18 . C35 . 129.5(4) yes C18 . C19 . N2 . 109.7(3) yes C18 . C19 . C20 . 126.6(4) yes N2 . C19 . C20 . 123.7(4) yes C19 . C20 . C1 . 125.0(4) yes C19 . C20 . C21 . 117.5(3) yes C1 . C20 . C21 . 117.3(3) yes C20 . C21 . C22 . 118.6(4) yes C20 . C21 . C26 . 122.8(4) yes C22 . C21 . C26 . 118.6(4) yes C21 . C22 . C23 . 121.2(4) yes C21 . C22 . H221 . 119.4 no C23 . C22 . H221 . 119.4 no C22 . C23 . C24 . 119.1(4) yes C22 . C23 . H231 . 120.4 no C24 . C23 . H231 . 120.4 no C23 . C24 . C25 . 120.6(4) yes C23 . C24 . H241 . 119.7 no C25 . C24 . H241 . 119.7 no C24 . C25 . C26 . 120.4(4) yes C24 . C25 . H251 . 119.8 no C26 . C25 . H251 . 119.8 no C21 . C26 . C25 . 120.0(4) yes C21 . C26 . H261 . 120.0 no C25 . C26 . H261 . 120.0 no C10 . C27 . C28 . 121.5(4) yes C10 . C27 . C32 . 119.7(4) yes C28 . C27 . C32 . 118.8(4) yes C27 . C28 . C29 . 120.4(4) yes C27 . C28 . H281 . 119.8 no C29 . C28 . H281 . 119.8 no C28 . C29 . C30 . 120.9(5) yes C28 . C29 . H291 . 119.6 no C30 . C29 . H291 . 119.6 no C29 . C30 . C31 . 119.9(5) yes C29 . C30 . H301 . 120.0 no C31 . C30 . H301 . 120.0 no C30 . C31 . C32 . 119.5(5) yes C30 . C31 . H311 . 120.3 no C32 . C31 . H311 . 120.3 no C31 . C32 . C27 . 120.5(4) yes C31 . C32 . H321 . 119.7 no C27 . C32 . H321 . 119.7 no C8 . C33 . H331 . 109.5 no C8 . C33 . H332 . 109.5 no H331 . C33 . H332 . 109.5 no C8 . C33 . H333 . 109.5 no H331 . C33 . H333 . 109.5 no H332 . C33 . H333 . 109.5 no C12 . C34 . H341 . 109.5 no C12 . C34 . H342 . 109.5 no H341 . C34 . H342 . 109.5 no C12 . C34 . H343 . 109.5 no H341 . C34 . H343 . 109.5 no H342 . C34 . H343 . 109.5 no C18 . C35 . H351 . 109.5 no C18 . C35 . H352 . 109.5 no H351 . C35 . H352 . 109.5 no C18 . C35 . H353 . 109.5 no H351 . C35 . H353 . 109.5 no H352 . C35 . H353 . 109.5 no C2 . C36 . H361 . 109.5 no C2 . C36 . H362 . 109.5 no H361 . C36 . H362 . 109.5 no C2 . C36 . H363 . 109.5 no H361 . C36 . H363 . 109.5 no H362 . C36 . H363 . 109.5 no C3 . C37 . C38 . 112.4(3) yes C3 . C37 . H371 . 108.7 no C38 . C37 . H371 . 108.7 no C3 . C37 . H372 . 108.7 no C38 . C37 . H372 . 108.7 no H371 . C37 . H372 . 109.5 no C37 . C38 . C39 . 113.4(3) yes C37 . C38 . H381 . 108.5 no C39 . C38 . H381 . 108.5 no C37 . C38 . H382 . 108.5 no C39 . C38 . H382 . 108.5 no H381 . C38 . H382 . 109.5 no C38 . C39 . C40 . 114.4(3) yes C38 . C39 . H391 . 108.2 no C40 . C39 . H391 . 108.2 no C38 . C39 . H392 . 108.2 no C40 . C39 . H392 . 108.2 no H391 . C39 . H392 . 109.5 no C39 . C40 . C41 . 114.8(4) yes C39 . C40 . H401 . 108.1 no C41 . C40 . H401 . 108.1 no C39 . C40 . H402 . 108.1 no C41 . C40 . H402 . 108.1 no H401 . C40 . H402 . 109.5 no C40 . C41 . C42 . 114.2(4) yes C40 . C41 . H411 . 108.3 no C42 . C41 . H411 . 108.3 no C40 . C41 . H412 . 108.3 no C42 . C41 . H412 . 108.3 no H411 . C41 . H412 . 109.5 no C41 . C42 . H421 . 109.5 no C41 . C42 . H422 . 109.5 no H421 . C42 . H422 . 109.5 no C41 . C42 . H423 . 109.5 no H421 . C42 . H423 . 109.5 no H422 . C42 . H423 . 109.5 no C7 . C43 . C44 . 111.8(3) yes C7 . C43 . H431 . 108.9 no C44 . C43 . H431 . 108.9 no C7 . C43 . H432 . 108.9 no C44 . C43 . H432 . 108.9 no H431 . C43 . H432 . 109.5 no C43 . C44 . C45 . 114.7(3) yes C43 . C44 . H441 . 108.2 no C45 . C44 . H441 . 108.2 no C43 . C44 . H442 . 108.2 no C45 . C44 . H442 . 108.2 no H441 . C44 . H442 . 109.5 no C44 . C45 . C46 . 112.3(4) yes C44 . C45 . H451 . 108.8 no C46 . C45 . H451 . 108.8 no C44 . C45 . H452 . 108.8 no C46 . C45 . H452 . 108.8 no H451 . C45 . H452 . 109.5 no C45 . C46 . C47 . 114.7(4) yes C45 . C46 . H461 . 108.1 no C47 . C46 . H461 . 108.1 no C45 . C46 . H462 . 108.1 no C47 . C46 . H462 . 108.1 no H461 . C46 . H462 . 109.5 no C46 . C47 . C48 . 112.2(4) yes C46 . C47 . H471 . 108.8 no C48 . C47 . H471 . 108.8 no C46 . C47 . H472 . 108.8 no C48 . C47 . H472 . 108.8 no H471 . C47 . H472 . 109.5 no C47 . C48 . H481 . 109.5 no C47 . C48 . H482 . 109.5 no H481 . C48 . H482 . 109.5 no C47 . C48 . H483 . 109.5 no H481 . C48 . H483 . 109.5 no H482 . C48 . H483 . 109.5 no C17 . C49 . C50 . 112.5(3) yes C17 . C49 . H491 . 108.7 no C50 . C49 . H491 . 108.7 no C17 . C49 . H492 . 108.7 no C50 . C49 . H492 . 108.7 no H491 . C49 . H492 . 109.5 no C49 . C50 . C51 . 112.8(3) yes C49 . C50 . H501 . 108.6 no C51 . C50 . H501 . 108.6 no C49 . C50 . H502 . 108.6 no C51 . C50 . H502 . 108.6 no H501 . C50 . H502 . 109.5 no C50 . C51 . C52 . 112.6(4) yes C50 . C51 . H511 . 108.7 no C52 . C51 . H511 . 108.7 no C50 . C51 . H512 . 108.7 no C52 . C51 . H512 . 108.7 no H511 . C51 . H512 . 109.5 no C51 . C52 . C53 . 114.5(5) yes C51 . C52 . H521 . 108.2 no C53 . C52 . H521 . 108.2 no C51 . C52 . H522 . 108.2 no C53 . C52 . H522 . 108.2 no H521 . C52 . H522 . 109.5 no C52 . C53 . C54 . 112.7(5) yes C52 . C53 . H531 . 108.7 no C54 . C53 . H531 . 108.7 no C52 . C53 . H532 . 108.7 no C54 . C53 . H532 . 108.7 no H531 . C53 . H532 . 109.5 no C53 . C54 . H541 . 109.5 no C53 . C54 . H542 . 109.5 no H541 . C54 . H542 . 109.5 no C53 . C54 . H543 . 109.5 no H541 . C54 . H543 . 109.5 no H542 . C54 . H543 . 109.5 no C13 . C55 . C56 . 112.7(3) yes C13 . C55 . H551 . 108.7 no C56 . C55 . H551 . 108.7 no C13 . C55 . H552 . 108.7 no C56 . C55 . H552 . 108.7 no H551 . C55 . H552 . 109.5 no C55 . C56 . C57 . 113.1(3) yes C55 . C56 . H561 . 108.6 no C57 . C56 . H561 . 108.6 no C55 . C56 . H562 . 108.6 no C57 . C56 . H562 . 108.6 no H561 . C56 . H562 . 109.5 no C56 . C57 . C58 . 112.6(3) yes C56 . C57 . H571 . 108.7 no C58 . C57 . H571 . 108.7 no C56 . C57 . H572 . 108.7 no C58 . C57 . H572 . 108.7 no H571 . C57 . H572 . 109.5 no C57 . C58 . C59 . 115.2(4) yes C57 . C58 . H581 . 108.0 no C59 . C58 . H581 . 108.0 no C57 . C58 . H582 . 108.0 no C59 . C58 . H582 . 108.0 no H581 . C58 . H582 . 109.5 no C58 . C59 . C60 . 113.9(5) yes C58 . C59 . H591 . 108.4 no C60 . C59 . H591 . 108.4 no C58 . C59 . H592 . 108.4 no C60 . C59 . H592 . 108.4 no H591 . C59 . H592 . 109.5 no C59 . C60 . H601 . 109.5 no C59 . C60 . H602 . 109.5 no H601 . C60 . H602 . 109.5 no C59 . C60 . H603 . 109.5 no H601 . C60 . H603 . 109.5 no H602 . C60 . H603 . 109.5 no N5 . C61 . C62 . 117.3(4) yes N5 . C61 . O2 . 120.6(4) yes C62 . C61 . O2 . 122.1(4) yes C61 . C62 . C63 . 118.8(4) yes C61 . C62 . C66 . 120.4(4) yes C63 . C62 . C66 . 120.8(4) yes C63 2_655 C63 . C62 . 118.4(5) yes C63 2_655 C63 . C64 . 119.1(5) yes C62 . C63 . C64 . 122.5(4) yes C63 . C64 . C65 . 119.6(4) yes C63 . C64 . C67 . 122.2(4) yes C65 . C64 . C67 . 118.1(4) yes C64 . C65 . N5 . 116.1(4) yes C64 . C65 . O1 . 122.4(4) yes N5 . C65 . O1 . 121.5(4) yes C67 2_655 C66 . C62 . 122.1(4) yes C67 2_655 C66 . H661 . 119.0 no C62 . C66 . H661 . 119.0 no C66 2_655 C67 . C64 . 117.4(4) yes C66 2_655 C67 . H671 . 121.3 no C64 . C67 . H671 . 121.3 no N5 . C68 . C69 . 110.6(3) yes N5 . C68 . H681 . 109.2 no C69 . C68 . H681 . 109.2 no N5 . C68 . H682 . 109.2 no C69 . C68 . H682 . 109.2 no H681 . C68 . H682 . 109.5 no C68 . C69 . C70 . 111.8(3) yes C68 . C69 . H691 . 108.9 no C70 . C69 . H691 . 108.9 no C68 . C69 . H692 . 108.9 no C70 . C69 . H692 . 108.9 no H691 . C69 . H692 . 109.5 no C69 . C70 . C71 . 111.8(3) yes C69 . C70 . H701 . 108.9 no C71 . C70 . H701 . 108.9 no C69 . C70 . H702 . 108.9 no C71 . C70 . H702 . 108.9 no H701 . C70 . H702 . 109.5 no C70 . C71 . C72 . 114.4(4) yes C70 . C71 . H711 . 108.2 no C72 . C71 . H711 . 108.2 no C70 . C71 . H712 . 108.2 no C72 . C71 . H712 . 108.2 no H711 . C71 . H712 . 109.5 no C71 . C72 . C73 . 112.8(4) yes C71 . C72 . H721 . 108.6 no C73 . C72 . H721 . 108.6 no C71 . C72 . H722 . 108.6 no C73 . C72 . H722 . 108.6 no H721 . C72 . H722 . 109.5 no C72 . C73 . H731 . 109.5 no C72 . C73 . H732 . 109.5 no H731 . C73 . H732 . 109.5 no C72 . C73 . H733 . 109.5 no H731 . C73 . H733 . 109.5 no H732 . C73 . H733 . 109.5 no Cl1 . C74 . Cl2 . 122.0(2) yes Cl1 . C74 . H741 . 106.3 no Cl2 . C74 . H741 . 106.3 no Cl1 . C74 . H742 . 106.3 no Cl2 . C74 . H742 . 106.3 no H741 . C74 . H742 . 109.2 no #===END data_san0007 _database_code_depnum_ccdc_archive 'CCDC 715662' #TrackingRef '- CCDC_deposided_merged_cifs_notepad.cif' _audit_creation_date 05-12-19 _audit_creation_method CRYSTALS_ver_12.82 _oxford_structure_analysis_title 'san0007 in P-1' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 13.465(2) _cell_length_b 16.552(3) _cell_length_c 16.697(3) _cell_angle_alpha 112.645(2) _cell_angle_beta 95.228(2) _cell_angle_gamma 103.286(2) _cell_volume 3275.0(10) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 1 _chemical_formula_sum 'C147 H187 Cl3 N10 O4' _chemical_formula_moiety 'C121 H157 Cl3 N8, C26 H30 N2 O4' _chemical_compound_source ? _chemical_formula_weight 2264.42 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4844 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 26.98 _exptl_crystal_description lath _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'Bruker SADABS' # absolute Tmin and Tmax unknown, but SADABS gives ratio as 0.643 _exptl_special_details ; Crystals were extremly small and weakly diffracting, which accounts for severe shortage of data ; _exptl_crystal_density_diffrn 1.148 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1222 _exptl_absorpt_coefficient_mu 0.127 _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.6709 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART APEX2 CCD diffractometer' _diffrn_measurement_method 'fine-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5 _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_reflns_number 24342 _reflns_number_total 11417 _diffrn_reflns_av_R_equivalents 0.028 # Number of reflections with Friedels Law is 11417 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 11559 _diffrn_reflns_theta_min 2.257 _diffrn_reflns_theta_max 23.536 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 21.654 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _reflns_limit_h_min -16 _reflns_limit_h_max 15 _reflns_limit_k_min -19 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.32 _refine_diff_density_max 1.46 _refine_ls_number_reflns 5490 _refine_ls_number_restraints 36 _refine_ls_number_parameters 758 #_refine_ls_R_factor_ref 0.1088 _refine_ls_wR_factor_ref 0.1160 _refine_ls_goodness_of_fit_ref 1.1925 #_reflns_number_all 11386 _refine_ls_R_factor_all 0.1697 _refine_ls_wR_factor_all 0.1448 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 5490 _refine_ls_R_factor_gt 0.1088 _refine_ls_wR_factor_gt 0.1160 _refine_ls_shift/su_max 0.041645 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.34 1.35 0.834 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Data collection: APEX2, Bruker AXS Inc., Madison, USA, 2004 Data reduction (frames integration): SAINT, Bruker AXS Inc., Madison, USA, 2004 Cell refinement: SAINT, Bruker AXS Inc., Madison, USA, 2004 Absorption correction: SADABS, Bruker AXS Inc., Madison, USA, 2004 Station 9.8: R. J. Cernik, W. Clegg, C. R. A. Catlow, G. Bushnell-Wye, J. V. Flaherty, G. N. Greaves, M. Hamichi, I. Burrows, D. J. Taylor, S. J. Teat, J. Synchotron Radiation 1997, 4, 279-286; 7, 40. Synchrotron chemical crystallography: W. Clegg, J. Chem. Soc., Dalton Trans. 2000, 3223-3232. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of G\"ottingen, Federal Republic of Germany. Watkin D.J. (1994). Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens N1 N 0.1048(4) 0.0811(3) -0.0062(3) 0.0351 1.0000 Uani . . . . . . N2 N 0.1897(4) -0.0569(3) -0.0814(3) 0.0354 1.0000 Uani . . . . . . N3 N 0.2514(4) -0.0636(3) 0.1020(3) 0.0360 1.0000 Uani . . . . . . N4 N 0.1721(4) 0.0778(3) 0.1773(3) 0.0356 1.0000 Uani . . . . . . N5 N 0.3875(4) 0.1782(3) 0.0949(4) 0.0443 1.0000 Uani . . . . . . O1 O 0.3487(3) 0.1810(3) -0.0383(3) 0.0502 1.0000 Uani . . . . . . O2 O 0.4402(4) 0.1847(3) 0.2316(3) 0.0519 1.0000 Uani . . . . . . C1 C 0.0666(4) 0.1455(4) 0.0505(4) 0.0349 1.0000 Uani . . . . . . C2 C 0.0270(5) 0.1908(4) 0.0024(4) 0.0383 1.0000 Uani . . . . . . C3 C 0.0436(5) 0.1544(4) -0.0811(4) 0.0405 1.0000 Uani . . . . . . C4 C 0.0937(4) 0.0827(4) -0.0876(4) 0.0339 1.0000 Uani . . . . . . C5 C 0.1272(4) 0.0250(4) -0.1594(4) 0.0362 1.0000 Uani . . . . . . C6 C 0.1681(4) -0.0441(4) -0.1573(4) 0.0348 1.0000 Uani . . . . . . C7 C 0.1955(5) -0.1138(4) -0.2321(4) 0.0421 1.0000 Uani . . . . . . C8 C 0.2323(4) -0.1662(4) -0.1982(4) 0.0380 1.0000 Uani . . . . . . C9 C 0.2294(4) -0.1294(3) -0.1044(4) 0.0351 1.0000 Uani . . . . . . C10 C 0.2689(4) -0.1625(4) -0.0477(4) 0.0365 1.0000 Uani . . . . . . C11 C 0.2798(4) -0.1351(4) 0.0423(4) 0.0343 1.0000 Uani . . . . . . C12 C 0.3318(4) -0.1708(4) 0.0927(4) 0.0362 1.0000 Uani . . . . . . C13 C 0.3364(5) -0.1205(4) 0.1818(4) 0.0393 1.0000 Uani . . . . . . C14 C 0.2842(4) -0.0521(4) 0.1870(4) 0.0344 1.0000 Uani . . . . . . C15 C 0.2673(4) 0.0173(4) 0.2619(4) 0.0382 1.0000 Uani . . . . . . C16 C 0.2153(5) 0.0805(4) 0.2558(4) 0.0398 1.0000 Uani . . . . . . C17 C 0.1950(5) 0.1542(4) 0.3301(4) 0.0401 1.0000 Uani . . . . . . C18 C 0.1371(4) 0.1924(4) 0.2948(4) 0.0386 1.0000 Uani . . . . . . C19 C 0.1240(4) 0.1453(4) 0.1986(4) 0.0349 1.0000 Uani . . . . . . C20 C 0.0732(4) 0.1720(4) 0.1414(4) 0.0361 1.0000 Uani . . . . . . C21 C 0.3082(5) 0.0243(4) 0.3510(4) 0.0445 1.0000 Uani . . . . . . C22 C 0.4064(6) 0.0799(5) 0.3973(5) 0.0553 1.0000 Uani . . . . . . C23 C 0.4423(6) 0.0868(6) 0.4816(5) 0.0692 1.0000 Uani . . . . . . C24 C 0.3798(7) 0.0382(6) 0.5185(5) 0.0715 1.0000 Uani . . . . . . C25 C 0.2819(7) -0.0198(5) 0.4711(5) 0.0639 1.0000 Uani . . . . . . C26 C 0.2456(5) -0.0269(4) 0.3871(4) 0.0496 1.0000 Uani . . . . . . C27 C 0.1256(5) 0.0455(4) -0.2396(4) 0.0383 1.0000 Uani . . . . . . C28 C 0.2116(5) 0.1077(4) -0.2432(4) 0.0437 1.0000 Uani . . . . . . C29 C 0.2115(6) 0.1305(4) -0.3153(4) 0.0527 1.0000 Uani . . . . . . C30 C 0.1257(6) 0.0913(4) -0.3834(5) 0.0539 1.0000 Uani . . . . . . C31 C 0.0388(6) 0.0304(5) -0.3796(4) 0.0527 1.0000 Uani . . . . . . C32 C 0.0387(5) 0.0074(4) -0.3077(4) 0.0485 1.0000 Uani . . . . . . C33 C 0.1854(6) -0.1276(5) -0.3270(4) 0.0580 1.0000 Uani . . . . . . C34 C 0.3916(5) -0.1334(4) 0.2558(4) 0.0496 1.0000 Uani . . . . . . C35 C 0.2288(7) 0.1851(5) 0.4294(4) 0.0616 1.0000 Uani . . . . . . C36 C 0.0110(5) 0.1823(4) -0.1526(4) 0.0518 1.0000 Uani . . . . . . C37 C 0.2696(5) -0.2481(4) -0.2454(4) 0.0452 1.0000 Uani . . . . . . C38 C 0.1865(5) -0.3391(4) -0.2696(4) 0.0490 1.0000 Uani . . . . . . C39 C 0.2281(6) -0.4212(4) -0.3067(4) 0.0520 1.0000 Uani . . . . . . C40 C 0.1479(6) -0.5100(4) -0.3290(5) 0.0686 1.0000 Uani D . . . . . C41 C 0.1889(6) -0.5944(5) -0.3649(6) 0.0966 1.0000 Uani D U . . . . C420 C 0.0995(13) -0.6843(9) -0.3978(13) 0.0976 0.5000 Uani D U . 2 1 . C421 C 0.1104(14) -0.6804(9) -0.3699(14) 0.0971 0.5000 Uani D U . 2 2 . C43 C 0.3732(5) -0.2526(4) 0.0513(4) 0.0410 1.0000 Uani . . . . . . C44 C 0.2882(5) -0.3437(4) 0.0137(4) 0.0476 1.0000 Uani . . . . . . C45 C 0.3281(5) -0.4258(4) -0.0303(4) 0.0477 1.0000 Uani . . . . . . C46 C 0.2420(6) -0.5148(4) -0.0732(5) 0.0612 1.0000 Uani . . . . . . C47 C 0.2769(6) -0.6005(4) -0.1216(5) 0.0619 1.0000 Uani . . . . . . C48 C 0.3420(9) -0.6222(6) -0.0607(6) 0.0899 1.0000 Uani . . . . . . C49 C 0.0974(5) 0.2736(4) 0.3411(4) 0.0425 1.0000 Uani . . . . . . C50 C 0.1733(6) 0.3643(4) 0.3543(5) 0.0536 1.0000 Uani . . . . . . C51 C 0.1344(6) 0.4473(5) 0.3977(5) 0.0609 1.0000 Uani . . . . . . C52 C 0.2169(8) 0.5356(5) 0.4121(5) 0.0763 1.0000 Uani . . . . . . C53 C 0.1796(9) 0.6202(6) 0.4486(6) 0.0926 1.0000 Uani . . . . . . C54 C 0.2676(13) 0.7088(7) 0.4680(7) 0.1319 1.0000 Uani . . . . . . C55 C -0.0163(4) 0.2701(4) 0.0416(4) 0.0376 1.0000 Uani . . . . . . C56 C 0.0676(5) 0.3617(4) 0.0814(4) 0.0434 1.0000 Uani . . . . . . C57 C 0.0239(5) 0.4427(4) 0.1138(4) 0.0453 1.0000 Uani . . . . . . C58 C 0.1064(5) 0.5345(4) 0.1601(5) 0.0501 1.0000 Uani . . . . . . C59 C 0.0640(6) 0.6155(4) 0.1900(5) 0.0584 1.0000 Uani . . . . . . C60 C 0.1450(6) 0.7053(5) 0.2408(5) 0.0621 1.0000 Uani . . . . . . C61 C 0.4345(5) 0.1479(4) 0.1516(4) 0.0429 1.0000 Uani . . . . . . C62 C 0.4794(4) 0.0716(4) 0.1106(4) 0.0394 1.0000 Uani . . . . . . C63 C 0.5259(5) 0.0375(4) 0.1623(4) 0.0449 1.0000 Uani . . . . . . C64 C 0.4777(4) 0.0356(4) 0.0186(4) 0.0390 1.0000 Uani . . . . . . C65 C 0.4297(4) 0.0697(4) -0.0359(4) 0.0380 1.0000 Uani . . . . . . C66 C 0.4298(5) 0.0333(4) -0.1256(4) 0.0407 1.0000 Uani . . . . . . C67 C 0.3848(4) 0.1452(4) 0.0044(4) 0.0427 1.0000 Uani . . . . . . C68 C 0.3465(5) 0.2564(4) 0.1359(5) 0.0487 1.0000 Uani . . . . . . C69 C 0.4281(5) 0.3460(4) 0.1578(5) 0.0481 1.0000 Uani . . . . . . C70 C 0.3893(5) 0.4293(4) 0.2016(5) 0.0513 1.0000 Uani . . . . . . C71 C 0.4713(5) 0.5183(4) 0.2236(5) 0.0547 1.0000 Uani . . . . . . C72 C 0.4378(6) 0.6034(5) 0.2698(6) 0.0702 1.0000 Uani . . . . . . C73 C 0.5226(7) 0.6907(5) 0.2935(6) 0.0741 1.0000 Uani . . . . . . C74 C 0.4606(7) 0.3403(5) 0.4161(5) 0.149(2) 0.5000 Uiso D U . . . . Cl1 Cl 0.5046(11) 0.4154(9) 0.3757(9) 0.141(3) 0.2500 Uiso D U . 1 2 . Cl2 Cl 0.4164(11) 0.3971(10) 0.5170(9) 0.143(3) 0.2500 Uiso D U . 1 2 . Cl3 Cl 0.5720(10) 0.2961(9) 0.4440(8) 0.129(3) 0.2500 Uiso D U . 1 2 . Cl4 Cl 0.5567(11) 0.4053(10) 0.4092(9) 0.163(3) 0.2500 Uiso D U . 1 1 . Cl5 Cl 0.4510(11) 0.3735(11) 0.5263(9) 0.155(3) 0.2500 Uiso D U . 1 1 . Cl6 Cl 0.3473(12) 0.3468(12) 0.3564(10) 0.172(3) 0.2500 Uiso D U . 1 1 . H1 H 0.1393 0.0348 0.0043 0.0500 1.0000 Uiso . . . . . . H2 H 0.2195 -0.0204 0.0913 0.0500 1.0000 Uiso . . . . . . H741 H 0.3975 0.2884 0.3756 0.1955 0.2500 Uiso . . . 1 2 . H742 H 0.4451 0.2727 0.3834 0.1955 0.2500 Uiso . . . 1 1 . H101 H 0.2942 -0.2166 -0.0780 0.0450 1.0000 Uiso . . . . . . H201 H 0.0351 0.2175 0.1697 0.0489 1.0000 Uiso . . . . . . H221 H 0.4519 0.1152 0.3706 0.0665 1.0000 Uiso . . . . . . H231 H 0.5136 0.1270 0.5153 0.0817 1.0000 Uiso . . . . . . H241 H 0.4049 0.0448 0.5796 0.0932 1.0000 Uiso . . . . . . H251 H 0.2375 -0.0564 0.4972 0.0888 1.0000 Uiso . . . . . . H261 H 0.1751 -0.0686 0.3528 0.0662 1.0000 Uiso . . . . . . H281 H 0.2740 0.1364 -0.1938 0.0516 1.0000 Uiso . . . . . . H291 H 0.2739 0.1754 -0.3176 0.0649 1.0000 Uiso . . . . . . H301 H 0.1263 0.1070 -0.4355 0.0672 1.0000 Uiso . . . . . . H311 H -0.0239 0.0028 -0.4285 0.0648 1.0000 Uiso . . . . . . H321 H -0.0243 -0.0367 -0.3051 0.0582 1.0000 Uiso . . . . . . H331 H 0.2108 -0.1807 -0.3610 0.0725 1.0000 Uiso . . . . . . H332 H 0.2280 -0.0713 -0.3303 0.0725 1.0000 Uiso . . . . . . H333 H 0.1107 -0.1401 -0.3531 0.0725 1.0000 Uiso . . . . . . H341 H 0.3834 -0.0888 0.3137 0.0670 1.0000 Uiso . . . . . . H342 H 0.4673 -0.1229 0.2536 0.0670 1.0000 Uiso . . . . . . H343 H 0.3611 -0.1971 0.2496 0.0670 1.0000 Uiso . . . . . . H351 H 0.2018 0.2375 0.4621 0.0805 1.0000 Uiso . . . . . . H352 H 0.3066 0.2048 0.4457 0.0805 1.0000 Uiso . . . . . . H353 H 0.2003 0.1333 0.4455 0.0805 1.0000 Uiso . . . . . . H361 H 0.0318 0.1459 -0.2083 0.0686 1.0000 Uiso . . . . . . H362 H 0.0458 0.2488 -0.1336 0.0686 1.0000 Uiso . . . . . . H363 H -0.0663 0.1708 -0.1634 0.0686 1.0000 Uiso . . . . . . H371 H 0.2891 -0.2460 -0.3011 0.0563 1.0000 Uiso . . . . . . H372 H 0.3322 -0.2451 -0.2061 0.0563 1.0000 Uiso . . . . . . H381 H 0.1277 -0.3457 -0.3149 0.0590 1.0000 Uiso . . . . . . H382 H 0.1604 -0.3379 -0.2151 0.0590 1.0000 Uiso . . . . . . H391 H 0.2531 -0.4229 -0.3618 0.0661 1.0000 Uiso . . . . . . H392 H 0.2877 -0.4139 -0.2617 0.0661 1.0000 Uiso . . . . . . H401 H 0.0891 -0.5176 -0.3749 0.0858 1.0000 Uiso . . . . . . H402 H 0.1217 -0.5074 -0.2741 0.0858 1.0000 Uiso . . . . . . H411 H 0.2021 -0.6049 -0.4256 0.1276 1.0000 Uiso . . . . . . H412 H 0.2555 -0.5826 -0.3248 0.1276 1.0000 Uiso . . . . . . H4201 H 0.1283 -0.7376 -0.4206 0.1281 0.5000 Uiso . . . 2 1 . H4202 H 0.0473 -0.6875 -0.4464 0.1281 0.5000 Uiso . . . 2 1 . H4203 H 0.0650 -0.6858 -0.3476 0.1281 0.5000 Uiso . . . 2 1 . H4211 H 0.1392 -0.7336 -0.3934 0.1279 0.5000 Uiso . . . 2 2 . H4212 H 0.0436 -0.6929 -0.4103 0.1279 0.5000 Uiso . . . 2 2 . H4213 H 0.0970 -0.6706 -0.3094 0.1279 0.5000 Uiso . . . 2 2 . H431 H 0.4259 -0.2523 0.0977 0.0531 1.0000 Uiso . . . . . . H432 H 0.4072 -0.2465 0.0023 0.0531 1.0000 Uiso . . . . . . H441 H 0.2557 -0.3504 0.0631 0.0604 1.0000 Uiso . . . . . . H442 H 0.2344 -0.3430 -0.0313 0.0604 1.0000 Uiso . . . . . . H451 H 0.3778 -0.4295 0.0157 0.0622 1.0000 Uiso . . . . . . H452 H 0.3654 -0.4170 -0.0768 0.0622 1.0000 Uiso . . . . . . H461 H 0.2065 -0.5237 -0.0259 0.0735 1.0000 Uiso . . . . . . H462 H 0.1914 -0.5094 -0.1172 0.0735 1.0000 Uiso . . . . . . H471 H 0.2135 -0.6537 -0.1535 0.0731 1.0000 Uiso . . . . . . H472 H 0.3180 -0.5899 -0.1654 0.0731 1.0000 Uiso . . . . . . H481 H 0.3623 -0.6781 -0.0955 0.1195 1.0000 Uiso . . . . . . H482 H 0.3015 -0.6335 -0.0168 0.1195 1.0000 Uiso . . . . . . H483 H 0.4061 -0.5697 -0.0287 0.1195 1.0000 Uiso . . . . . . H491 H 0.0865 0.2762 0.4004 0.0564 1.0000 Uiso . . . . . . H492 H 0.0295 0.2651 0.3046 0.0564 1.0000 Uiso . . . . . . H501 H 0.2401 0.3733 0.3926 0.0700 1.0000 Uiso . . . . . . H502 H 0.1862 0.3602 0.2951 0.0700 1.0000 Uiso . . . . . . H511 H 0.1188 0.4510 0.4562 0.0775 1.0000 Uiso . . . . . . H512 H 0.0694 0.4407 0.3586 0.0775 1.0000 Uiso . . . . . . H521 H 0.2796 0.5440 0.4548 0.0978 1.0000 Uiso . . . . . . H522 H 0.2364 0.5291 0.3540 0.0978 1.0000 Uiso . . . . . . H531 H 0.1559 0.6250 0.5049 0.1134 1.0000 Uiso . . . . . . H532 H 0.1200 0.6142 0.4043 0.1134 1.0000 Uiso . . . . . . H541 H 0.2404 0.7629 0.4919 0.1594 1.0000 Uiso . . . . . . H542 H 0.3274 0.7155 0.5125 0.1594 1.0000 Uiso . . . . . . H543 H 0.2916 0.7047 0.4120 0.1594 1.0000 Uiso . . . . . . H551 H -0.0675 0.2697 -0.0060 0.0478 1.0000 Uiso . . . . . . H552 H -0.0526 0.2630 0.0892 0.0478 1.0000 Uiso . . . . . . H561 H 0.1081 0.3662 0.0352 0.0571 1.0000 Uiso . . . . . . H562 H 0.1151 0.3643 0.1326 0.0571 1.0000 Uiso . . . . . . H571 H -0.0192 0.4426 0.0617 0.0567 1.0000 Uiso . . . . . . H572 H -0.0213 0.4353 0.1564 0.0567 1.0000 Uiso . . . . . . H581 H 0.1529 0.5408 0.1181 0.0629 1.0000 Uiso . . . . . . H582 H 0.1479 0.5352 0.2133 0.0629 1.0000 Uiso . . . . . . H591 H 0.0267 0.6174 0.1364 0.0688 1.0000 Uiso . . . . . . H592 H 0.0136 0.6071 0.2286 0.0688 1.0000 Uiso . . . . . . H601 H 0.1108 0.7555 0.2583 0.0737 1.0000 Uiso . . . . . . H602 H 0.1957 0.7153 0.2030 0.0737 1.0000 Uiso . . . . . . H603 H 0.1825 0.7051 0.2952 0.0737 1.0000 Uiso . . . . . . H631 H 0.5279 0.0641 0.2275 0.0534 1.0000 Uiso . . . . . . H661 H 0.3981 0.0580 -0.1644 0.0492 1.0000 Uiso . . . . . . H681 H 0.3250 0.2562 0.1916 0.0584 1.0000 Uiso . . . . . . H682 H 0.2846 0.2505 0.0938 0.0584 1.0000 Uiso . . . . . . H691 H 0.4902 0.3509 0.1991 0.0573 1.0000 Uiso . . . . . . H692 H 0.4489 0.3458 0.1018 0.0573 1.0000 Uiso . . . . . . H701 H 0.3682 0.4294 0.2575 0.0617 1.0000 Uiso . . . . . . H702 H 0.3275 0.4246 0.1602 0.0617 1.0000 Uiso . . . . . . H711 H 0.5338 0.5213 0.2632 0.0666 1.0000 Uiso . . . . . . H712 H 0.4905 0.5183 0.1671 0.0666 1.0000 Uiso . . . . . . H721 H 0.4163 0.6028 0.3254 0.0840 1.0000 Uiso . . . . . . H722 H 0.3771 0.6021 0.2295 0.0840 1.0000 Uiso . . . . . . H731 H 0.4960 0.7442 0.3236 0.0879 1.0000 Uiso . . . . . . H732 H 0.5837 0.6933 0.3343 0.0879 1.0000 Uiso . . . . . . H733 H 0.5445 0.6925 0.2384 0.0879 1.0000 Uiso . . . . . . 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 N1 0.040(3) 0.033(2) 0.040(3) 0.019(2) 0.018(2) 0.015(2) N2 0.038(3) 0.030(2) 0.041(3) 0.016(2) 0.013(2) 0.009(2) N3 0.039(3) 0.030(2) 0.049(3) 0.021(2) 0.017(2) 0.018(2) N4 0.040(3) 0.035(2) 0.044(3) 0.023(2) 0.021(2) 0.017(2) N5 0.039(3) 0.041(3) 0.061(4) 0.026(3) 0.018(3) 0.014(2) O1 0.044(2) 0.040(2) 0.073(3) 0.027(2) 0.009(2) 0.016(2) O2 0.061(3) 0.041(2) 0.053(3) 0.015(2) 0.026(2) 0.015(2) C1 0.034(3) 0.031(3) 0.048(4) 0.021(3) 0.015(3) 0.013(2) C2 0.042(3) 0.035(3) 0.044(4) 0.020(3) 0.015(3) 0.014(3) C3 0.039(3) 0.034(3) 0.049(4) 0.020(3) 0.006(3) 0.008(3) C4 0.033(3) 0.028(3) 0.040(3) 0.013(2) 0.011(3) 0.010(2) C5 0.036(3) 0.033(3) 0.040(3) 0.018(3) 0.009(3) 0.007(3) C6 0.040(3) 0.033(3) 0.036(3) 0.015(2) 0.016(3) 0.011(3) C7 0.055(4) 0.035(3) 0.044(4) 0.019(3) 0.024(3) 0.018(3) C8 0.042(3) 0.030(3) 0.041(3) 0.011(3) 0.017(3) 0.011(3) C9 0.034(3) 0.025(3) 0.050(4) 0.017(3) 0.018(3) 0.007(2) C10 0.034(3) 0.028(3) 0.050(4) 0.014(3) 0.022(3) 0.013(2) C11 0.030(3) 0.027(3) 0.049(4) 0.015(3) 0.020(3) 0.010(2) C12 0.031(3) 0.032(3) 0.054(4) 0.021(3) 0.019(3) 0.015(3) C13 0.040(3) 0.034(3) 0.052(4) 0.021(3) 0.016(3) 0.016(3) C14 0.036(3) 0.033(3) 0.044(4) 0.021(3) 0.017(3) 0.018(3) C15 0.040(3) 0.037(3) 0.046(4) 0.022(3) 0.015(3) 0.015(3) C16 0.046(4) 0.040(3) 0.045(4) 0.023(3) 0.024(3) 0.022(3) C17 0.049(4) 0.037(3) 0.045(4) 0.021(3) 0.025(3) 0.019(3) C18 0.043(3) 0.031(3) 0.054(4) 0.023(3) 0.027(3) 0.017(3) C19 0.033(3) 0.032(3) 0.047(4) 0.020(3) 0.019(3) 0.013(3) C20 0.036(3) 0.038(3) 0.049(4) 0.024(3) 0.026(3) 0.019(3) C21 0.054(4) 0.043(3) 0.047(4) 0.018(3) 0.018(3) 0.031(3) C22 0.056(4) 0.054(4) 0.056(4) 0.017(3) 0.016(3) 0.024(4) C23 0.070(5) 0.085(5) 0.049(5) 0.013(4) 0.009(4) 0.043(5) C24 0.089(6) 0.097(6) 0.047(5) 0.032(5) 0.013(4) 0.058(6) C25 0.097(6) 0.068(5) 0.057(5) 0.038(4) 0.029(5) 0.053(5) C26 0.067(4) 0.052(4) 0.046(4) 0.026(3) 0.024(3) 0.033(3) C27 0.047(4) 0.032(3) 0.040(3) 0.016(3) 0.018(3) 0.015(3) C28 0.046(4) 0.036(3) 0.047(4) 0.018(3) 0.008(3) 0.007(3) C29 0.063(5) 0.049(4) 0.050(4) 0.026(3) 0.016(4) 0.012(3) C30 0.074(5) 0.045(4) 0.049(4) 0.024(3) 0.018(4) 0.019(4) C31 0.060(4) 0.060(4) 0.042(4) 0.025(3) 0.012(3) 0.017(3) C32 0.051(4) 0.047(4) 0.047(4) 0.020(3) 0.018(3) 0.011(3) C33 0.091(5) 0.048(4) 0.042(4) 0.018(3) 0.025(4) 0.030(4) C34 0.062(4) 0.051(4) 0.055(4) 0.029(3) 0.019(3) 0.036(3) C35 0.097(6) 0.062(4) 0.043(4) 0.020(3) 0.026(4) 0.052(4) C36 0.067(4) 0.051(4) 0.054(4) 0.028(3) 0.017(3) 0.035(4) C37 0.056(4) 0.037(3) 0.047(4) 0.016(3) 0.028(3) 0.019(3) C38 0.054(4) 0.035(3) 0.058(4) 0.015(3) 0.019(3) 0.018(3) C39 0.075(5) 0.042(3) 0.049(4) 0.017(3) 0.030(3) 0.030(3) C40 0.099(6) 0.039(4) 0.076(5) 0.020(4) 0.048(5) 0.031(4) C41 0.185(8) 0.044(3) 0.090(6) 0.032(4) 0.091(6) 0.055(4) C420 0.186(8) 0.044(3) 0.090(6) 0.031(4) 0.092(6) 0.054(4) C421 0.186(8) 0.044(3) 0.090(6) 0.032(4) 0.091(6) 0.054(4) C43 0.041(3) 0.037(3) 0.055(4) 0.021(3) 0.016(3) 0.022(3) C44 0.049(4) 0.035(3) 0.067(4) 0.024(3) 0.025(3) 0.017(3) C45 0.052(4) 0.038(3) 0.066(4) 0.026(3) 0.025(3) 0.024(3) C46 0.056(4) 0.034(3) 0.094(5) 0.021(3) 0.032(4) 0.016(3) C47 0.061(4) 0.038(4) 0.084(5) 0.019(4) 0.019(4) 0.019(3) C48 0.137(9) 0.067(5) 0.094(7) 0.044(5) 0.034(6) 0.060(6) C49 0.057(4) 0.041(3) 0.043(4) 0.021(3) 0.024(3) 0.027(3) C50 0.074(5) 0.042(3) 0.059(4) 0.025(3) 0.035(4) 0.027(3) C51 0.082(5) 0.048(4) 0.063(5) 0.024(3) 0.021(4) 0.036(4) C52 0.135(8) 0.049(4) 0.060(5) 0.024(4) 0.043(5) 0.043(5) C53 0.156(9) 0.052(5) 0.076(6) 0.024(4) 0.014(6) 0.049(6) C54 0.253(16) 0.058(6) 0.088(7) 0.026(5) 0.065(9) 0.045(8) C55 0.038(3) 0.033(3) 0.049(4) 0.021(3) 0.012(3) 0.014(3) C56 0.041(3) 0.037(3) 0.064(4) 0.026(3) 0.027(3) 0.020(3) C57 0.050(4) 0.039(3) 0.053(4) 0.021(3) 0.017(3) 0.018(3) C58 0.048(4) 0.041(3) 0.068(4) 0.025(3) 0.024(3) 0.018(3) C59 0.058(4) 0.037(3) 0.077(5) 0.017(3) 0.016(4) 0.019(3) C60 0.071(5) 0.044(4) 0.070(5) 0.024(4) 0.008(4) 0.015(4) C61 0.035(3) 0.033(3) 0.056(4) 0.016(3) 0.018(3) 0.003(3) C62 0.033(3) 0.035(3) 0.051(4) 0.018(3) 0.016(3) 0.011(3) C63 0.041(4) 0.044(4) 0.049(4) 0.021(3) 0.015(3) 0.005(3) C64 0.033(3) 0.029(3) 0.056(4) 0.020(3) 0.013(3) 0.004(2) C65 0.033(3) 0.036(3) 0.051(4) 0.023(3) 0.014(3) 0.009(3) C66 0.044(3) 0.032(3) 0.048(4) 0.020(3) 0.006(3) 0.008(3) C67 0.031(3) 0.034(3) 0.061(4) 0.020(3) 0.012(3) 0.005(3) C68 0.041(4) 0.035(3) 0.069(4) 0.018(3) 0.022(3) 0.014(3) C69 0.040(3) 0.033(3) 0.070(4) 0.016(3) 0.021(3) 0.015(3) C70 0.050(4) 0.035(3) 0.069(4) 0.016(3) 0.027(3) 0.018(3) C71 0.056(4) 0.039(3) 0.072(5) 0.020(3) 0.027(4) 0.019(3) C72 0.076(5) 0.042(4) 0.091(6) 0.020(4) 0.029(4) 0.025(4) C73 0.089(6) 0.039(4) 0.092(6) 0.022(4) 0.021(5) 0.022(4) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2169(10) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag N1 . C1 . 1.363(7) yes N1 . C4 . 1.365(7) yes N1 . H1 . 1.042 no N2 . C6 . 1.380(7) yes N2 . C9 . 1.359(7) yes N3 . C11 . 1.381(7) yes N3 . C14 . 1.373(7) yes N3 . H2 . 0.977 no N4 . C16 . 1.364(8) yes N4 . C19 . 1.366(7) yes N5 . C61 . 1.396(8) yes N5 . C67 . 1.389(8) yes N5 . C68 . 1.471(8) yes O1 . C67 . 1.221(7) yes O2 . C61 . 1.223(7) yes C1 . C2 . 1.436(8) yes C1 . C20 . 1.396(8) yes C2 . C3 . 1.353(8) yes C2 . C55 . 1.501(8) yes C3 . C4 . 1.469(8) yes C3 . C36 . 1.500(9) yes C4 . C5 . 1.402(8) yes C5 . C6 . 1.389(8) yes C5 . C27 . 1.503(8) yes C6 . C7 . 1.482(8) yes C7 . C8 . 1.358(8) yes C7 . C33 . 1.501(9) yes C8 . C9 . 1.453(8) yes C8 . C37 . 1.508(8) yes C9 . C10 . 1.386(8) yes C10 . C11 . 1.374(8) yes C10 . H101 . 1.000 no C11 . C12 . 1.419(8) yes C12 . C13 . 1.385(8) yes C12 . C43 . 1.522(7) yes C13 . C14 . 1.445(8) yes C13 . C34 . 1.493(9) yes C14 . C15 . 1.414(8) yes C15 . C16 . 1.415(8) yes C15 . C21 . 1.489(9) yes C16 . C17 . 1.466(8) yes C17 . C18 . 1.336(8) yes C17 . C35 . 1.523(9) yes C18 . C19 . 1.463(8) yes C18 . C49 . 1.515(8) yes C19 . C20 . 1.387(8) yes C20 . H201 . 1.000 no C21 . C22 . 1.379(9) yes C21 . C26 . 1.396(9) yes C22 . C23 . 1.400(10) yes C22 . H221 . 1.000 no C23 . C24 . 1.378(12) yes C23 . H231 . 1.000 no C24 . C25 . 1.388(12) yes C24 . H241 . 1.000 no C25 . C26 . 1.393(10) yes C25 . H251 . 1.000 no C26 . H261 . 1.000 no C27 . C28 . 1.383(8) yes C27 . C32 . 1.388(9) yes C28 . C29 . 1.394(9) yes C28 . H281 . 1.000 no C29 . C30 . 1.376(10) yes C29 . H291 . 1.000 no C30 . C31 . 1.383(10) yes C30 . H301 . 1.000 no C31 . C32 . 1.391(9) yes C31 . H311 . 1.000 no C32 . H321 . 1.000 no C33 . H331 . 1.000 no C33 . H332 . 1.000 no C33 . H333 . 1.000 no C34 . H341 . 1.000 no C34 . H342 . 1.000 no C34 . H343 . 1.000 no C35 . H351 . 1.000 no C35 . H352 . 1.000 no C35 . H353 . 1.000 no C36 . H361 . 1.000 no C36 . H362 . 1.000 no C36 . H363 . 1.000 no C37 . C38 . 1.536(8) yes C37 . H371 . 1.000 no C37 . H372 . 1.000 no C38 . C39 . 1.519(8) yes C38 . H381 . 1.000 no C38 . H382 . 1.000 no C39 . C40 . 1.499(9) yes C39 . H391 . 1.000 no C39 . H392 . 1.000 no C40 . C41 . 1.545(9) yes C40 . H401 . 1.000 no C40 . H402 . 1.000 no C41 . C420 . 1.545(16) yes C41 . H411 . 1.000 no C41 . H412 . 1.000 no C41 . C421 . 1.533(15) yes C41 . H411 . 1.000 no C41 . H412 . 1.000 no C420 . H4201 . 1.000 no C420 . H4202 . 1.000 no C420 . H4203 . 1.000 no C421 . H4211 . 1.000 no C421 . H4212 . 1.000 no C421 . H4213 . 1.000 no C43 . C44 . 1.525(8) yes C43 . H431 . 1.000 no C43 . H432 . 1.000 no C44 . C45 . 1.522(8) yes C44 . H441 . 1.000 no C44 . H442 . 1.000 no C45 . C46 . 1.509(9) yes C45 . H451 . 1.000 no C45 . H452 . 1.000 no C46 . C47 . 1.542(9) yes C46 . H461 . 1.000 no C46 . H462 . 1.000 no C47 . C48 . 1.482(12) yes C47 . H471 . 1.000 no C47 . H472 . 1.000 no C48 . H481 . 1.000 no C48 . H482 . 1.000 no C48 . H483 . 1.000 no C49 . C50 . 1.532(9) yes C49 . H491 . 1.000 no C49 . H492 . 1.000 no C50 . C51 . 1.523(9) yes C50 . H501 . 1.000 no C50 . H502 . 1.000 no C51 . C52 . 1.537(11) yes C51 . H511 . 1.000 no C51 . H512 . 1.000 no C52 . C53 . 1.519(10) yes C52 . H521 . 1.000 no C52 . H522 . 1.000 no C53 . C54 . 1.556(16) yes C53 . H531 . 1.000 no C53 . H532 . 1.000 no C54 . H541 . 1.000 no C54 . H542 . 1.000 no C54 . H543 . 1.000 no C55 . C56 . 1.522(8) yes C55 . H551 . 1.000 no C55 . H552 . 1.000 no C56 . C57 . 1.516(8) yes C56 . H561 . 1.000 no C56 . H562 . 1.000 no C57 . C58 . 1.517(9) yes C57 . H571 . 1.000 no C57 . H572 . 1.000 no C58 . C59 . 1.504(9) yes C58 . H581 . 1.000 no C58 . H582 . 1.000 no C59 . C60 . 1.494(10) yes C59 . H591 . 1.000 no C59 . H592 . 1.000 no C60 . H601 . 1.000 no C60 . H602 . 1.000 no C60 . H603 . 1.000 no C61 . C62 . 1.480(8) yes C62 . C63 . 1.376(9) yes C62 . C64 . 1.414(8) yes C63 . C66 2_655 1.393(8) yes C63 . H631 . 1.000 no C64 . C64 2_655 1.402(11) yes C64 . C65 . 1.421(8) yes C65 . C66 . 1.384(8) yes C65 . C67 . 1.466(8) yes C66 . H661 . 1.000 no C68 . C69 . 1.517(8) yes C68 . H681 . 1.000 no C68 . H682 . 1.000 no C69 . C70 . 1.528(8) yes C69 . H691 . 1.000 no C69 . H692 . 1.000 no C70 . C71 . 1.513(9) yes C70 . H701 . 1.000 no C70 . H702 . 1.000 no C71 . C72 . 1.517(9) yes C71 . H711 . 1.000 no C71 . H712 . 1.000 no C72 . C73 . 1.505(11) yes C72 . H721 . 1.000 no C72 . H722 . 1.000 no C73 . H731 . 1.000 no C73 . H732 . 1.000 no C73 . H733 . 1.000 no C74 . Cl1 . 1.652(14) yes C74 . Cl2 . 1.817(14) yes C74 . Cl3 . 1.908(13) yes C74 . H741 . 1.014 no C74 . Cl4 . 1.526(15) yes C74 . Cl5 . 1.734(15) yes C74 . Cl6 . 1.793(15) yes C74 . H742 . 0.997 no Cl3 . H542 2_666 1.564 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 . N1 . C4 . 110.3(4) yes C1 . N1 . H1 . 130.3 no C4 . N1 . H1 . 119.4 no C6 . N2 . C9 . 106.5(4) yes C11 . N3 . C14 . 110.3(4) yes C11 . N3 . H2 . 129.1 no C14 . N3 . H2 . 120.3 no C16 . N4 . C19 . 106.0(4) yes C61 . N5 . C67 . 124.8(5) yes C61 . N5 . C68 . 117.0(5) yes C67 . N5 . C68 . 117.9(5) yes N1 . C1 . C2 . 107.8(5) yes N1 . C1 . C20 . 127.9(5) yes C2 . C1 . C20 . 123.9(5) yes C1 . C2 . C3 . 108.0(5) yes C1 . C2 . C55 . 125.1(5) yes C3 . C2 . C55 . 126.7(5) yes C2 . C3 . C4 . 107.5(5) yes C2 . C3 . C36 . 124.2(5) yes C4 . C3 . C36 . 128.2(5) yes C3 . C4 . N1 . 106.4(5) yes C3 . C4 . C5 . 130.1(5) yes N1 . C4 . C5 . 123.5(5) yes C4 . C5 . C6 . 123.7(5) yes C4 . C5 . C27 . 116.8(5) yes C6 . C5 . C27 . 119.4(5) yes C5 . C6 . N2 . 123.2(5) yes C5 . C6 . C7 . 127.3(5) yes N2 . C6 . C7 . 109.5(4) yes C6 . C7 . C8 . 106.0(5) yes C6 . C7 . C33 . 129.0(5) yes C8 . C7 . C33 . 125.0(5) yes C7 . C8 . C9 . 107.2(5) yes C7 . C8 . C37 . 128.5(5) yes C9 . C8 . C37 . 124.4(5) yes C8 . C9 . N2 . 110.9(5) yes C8 . C9 . C10 . 122.6(5) yes N2 . C9 . C10 . 126.5(5) yes C9 . C10 . C11 . 132.3(5) yes C9 . C10 . H101 . 113.8 no C11 . C10 . H101 . 113.8 no N3 . C11 . C10 . 127.6(5) yes N3 . C11 . C12 . 106.6(5) yes C10 . C11 . C12 . 125.6(5) yes C11 . C12 . C13 . 109.3(5) yes C11 . C12 . C43 . 123.3(5) yes C13 . C12 . C43 . 127.4(5) yes C12 . C13 . C14 . 106.4(5) yes C12 . C13 . C34 . 125.0(5) yes C14 . C13 . C34 . 128.5(5) yes C13 . C14 . N3 . 107.4(5) yes C13 . C14 . C15 . 130.0(5) yes N3 . C14 . C15 . 122.6(5) yes C14 . C15 . C16 . 123.1(5) yes C14 . C15 . C21 . 117.8(5) yes C16 . C15 . C21 . 119.1(5) yes C15 . C16 . N4 . 123.4(5) yes C15 . C16 . C17 . 126.3(5) yes N4 . C16 . C17 . 110.3(5) yes C16 . C17 . C18 . 106.6(5) yes C16 . C17 . C35 . 129.7(5) yes C18 . C17 . C35 . 123.7(5) yes C17 . C18 . C19 . 106.9(5) yes C17 . C18 . C49 . 129.0(6) yes C19 . C18 . C49 . 124.0(5) yes C18 . C19 . N4 . 110.2(5) yes C18 . C19 . C20 . 122.1(5) yes N4 . C19 . C20 . 127.6(5) yes C1 . C20 . C19 . 130.3(5) yes C1 . C20 . H201 . 114.9 no C19 . C20 . H201 . 114.9 no C15 . C21 . C22 . 120.9(6) yes C15 . C21 . C26 . 119.0(6) yes C22 . C21 . C26 . 120.2(6) yes C21 . C22 . C23 . 119.8(7) yes C21 . C22 . H221 . 120.1 no C23 . C22 . H221 . 120.1 no C22 . C23 . C24 . 120.2(7) yes C22 . C23 . H231 . 119.9 no C24 . C23 . H231 . 119.9 no C23 . C24 . C25 . 120.1(7) yes C23 . C24 . H241 . 120.0 no C25 . C24 . H241 . 120.0 no C24 . C25 . C26 . 120.0(7) yes C24 . C25 . H251 . 120.0 no C26 . C25 . H251 . 120.0 no C21 . C26 . C25 . 119.7(7) yes C21 . C26 . H261 . 120.2 no C25 . C26 . H261 . 120.2 no C5 . C27 . C28 . 118.7(5) yes C5 . C27 . C32 . 121.8(5) yes C28 . C27 . C32 . 119.4(5) yes C27 . C28 . C29 . 120.2(6) yes C27 . C28 . H281 . 119.9 no C29 . C28 . H281 . 119.9 no C28 . C29 . C30 . 120.1(6) yes C28 . C29 . H291 . 119.9 no C30 . C29 . H291 . 119.9 no C29 . C30 . C31 . 120.0(6) yes C29 . C30 . H301 . 120.0 no C31 . C30 . H301 . 120.0 no C30 . C31 . C32 . 120.0(7) yes C30 . C31 . H311 . 120.0 no C32 . C31 . H311 . 120.0 no C31 . C32 . C27 . 120.2(6) yes C31 . C32 . H321 . 119.9 no C27 . C32 . H321 . 119.9 no C7 . C33 . H331 . 109.5 no C7 . C33 . H332 . 109.5 no H331 . C33 . H332 . 109.5 no C7 . C33 . H333 . 109.5 no H331 . C33 . H333 . 109.5 no H332 . C33 . H333 . 109.5 no C13 . C34 . H341 . 109.5 no C13 . C34 . H342 . 109.5 no H341 . C34 . H342 . 109.5 no C13 . C34 . H343 . 109.5 no H341 . C34 . H343 . 109.5 no H342 . C34 . H343 . 109.5 no C17 . C35 . H351 . 109.5 no C17 . C35 . H352 . 109.5 no H351 . C35 . H352 . 109.5 no C17 . C35 . H353 . 109.5 no H351 . C35 . H353 . 109.5 no H352 . C35 . H353 . 109.5 no C3 . C36 . H361 . 109.5 no C3 . C36 . H362 . 109.5 no H361 . C36 . H362 . 109.5 no C3 . C36 . H363 . 109.5 no H361 . C36 . H363 . 109.5 no H362 . C36 . H363 . 109.5 no C8 . C37 . C38 . 112.7(5) yes C8 . C37 . H371 . 108.7 no C38 . C37 . H371 . 108.7 no C8 . C37 . H372 . 108.7 no C38 . C37 . H372 . 108.7 no H371 . C37 . H372 . 109.5 no C37 . C38 . C39 . 112.7(5) yes C37 . C38 . H381 . 108.7 no C39 . C38 . H381 . 108.7 no C37 . C38 . H382 . 108.7 no C39 . C38 . H382 . 108.7 no H381 . C38 . H382 . 109.5 no C38 . C39 . C40 . 112.9(6) yes C38 . C39 . H391 . 108.6 no C40 . C39 . H391 . 108.6 no C38 . C39 . H392 . 108.6 no C40 . C39 . H392 . 108.6 no H391 . C39 . H392 . 109.5 no C39 . C40 . C41 . 114.0(5) yes C39 . C40 . H401 . 108.3 no C41 . C40 . H401 . 108.3 no C39 . C40 . H402 . 108.3 no C41 . C40 . H402 . 108.3 no H401 . C40 . H402 . 109.5 no C40 . C41 . C420 . 111.3(2) yes C40 . C41 . H411 . 109.0 no C420 . C41 . H411 . 94.0 no C40 . C41 . H412 . 109.0 no C420 . C41 . H412 . 122.7 no H411 . C41 . H412 . 109.4 no C40 . C41 . C421 . 111.5(2) yes C40 . C41 . H411 . 109.0 no C421 . C41 . H411 . 109.0 no C40 . C41 . H412 . 109.0 no C421 . C41 . H412 . 109.0 no H411 . C41 . H412 . 109.4 no C41 . C420 . H4201 . 109.5 no C41 . C420 . H4202 . 109.5 no H4201 . C420 . H4202 . 109.5 no C41 . C420 . H4203 . 109.5 no H4201 . C420 . H4203 . 109.5 no H4202 . C420 . H4203 . 109.5 no C41 . C421 . H4211 . 109.5 no C41 . C421 . H4212 . 109.4 no H4211 . C421 . H4212 . 109.5 no C41 . C421 . H4213 . 109.5 no H4211 . C421 . H4213 . 109.5 no H4212 . C421 . H4213 . 109.5 no C12 . C43 . C44 . 113.0(5) yes C12 . C43 . H431 . 108.6 no C44 . C43 . H431 . 108.6 no C12 . C43 . H432 . 108.6 no C44 . C43 . H432 . 108.6 no H431 . C43 . H432 . 109.5 no C43 . C44 . C45 . 113.5(5) yes C43 . C44 . H441 . 108.5 no C45 . C44 . H441 . 108.5 no C43 . C44 . H442 . 108.5 no C45 . C44 . H442 . 108.5 no H441 . C44 . H442 . 109.5 no C44 . C45 . C46 . 112.8(5) yes C44 . C45 . H451 . 108.6 no C46 . C45 . H451 . 108.6 no C44 . C45 . H452 . 108.6 no C46 . C45 . H452 . 108.6 no H451 . C45 . H452 . 109.5 no C45 . C46 . C47 . 115.4(6) yes C45 . C46 . H461 . 108.0 no C47 . C46 . H461 . 108.0 no C45 . C46 . H462 . 108.0 no C47 . C46 . H462 . 108.0 no H461 . C46 . H462 . 109.5 no C46 . C47 . C48 . 112.9(7) yes C46 . C47 . H471 . 108.6 no C48 . C47 . H471 . 108.6 no C46 . C47 . H472 . 108.6 no C48 . C47 . H472 . 108.6 no H471 . C47 . H472 . 109.5 no C47 . C48 . H481 . 109.5 no C47 . C48 . H482 . 109.5 no H481 . C48 . H482 . 109.5 no C47 . C48 . H483 . 109.5 no H481 . C48 . H483 . 109.5 no H482 . C48 . H483 . 109.5 no C18 . C49 . C50 . 112.5(5) yes C18 . C49 . H491 . 108.7 no C50 . C49 . H491 . 108.7 no C18 . C49 . H492 . 108.7 no C50 . C49 . H492 . 108.7 no H491 . C49 . H492 . 109.5 no C49 . C50 . C51 . 114.1(6) yes C49 . C50 . H501 . 108.3 no C51 . C50 . H501 . 108.3 no C49 . C50 . H502 . 108.3 no C51 . C50 . H502 . 108.3 no H501 . C50 . H502 . 109.5 no C50 . C51 . C52 . 110.7(6) yes C50 . C51 . H511 . 109.2 no C52 . C51 . H511 . 109.2 no C50 . C51 . H512 . 109.2 no C52 . C51 . H512 . 109.2 no H511 . C51 . H512 . 109.5 no C51 . C52 . C53 . 113.3(8) yes C51 . C52 . H521 . 108.5 no C53 . C52 . H521 . 108.5 no C51 . C52 . H522 . 108.5 no C53 . C52 . H522 . 108.5 no H521 . C52 . H522 . 109.5 no C52 . C53 . C54 . 111.7(9) yes C52 . C53 . H531 . 108.9 no C54 . C53 . H531 . 108.9 no C52 . C53 . H532 . 108.9 no C54 . C53 . H532 . 108.9 no H531 . C53 . H532 . 109.5 no C53 . C54 . H541 . 109.5 no C53 . C54 . H542 . 109.5 no H541 . C54 . H542 . 109.5 no C53 . C54 . H543 . 109.5 no H541 . C54 . H543 . 109.5 no H542 . C54 . H543 . 109.5 no C2 . C55 . C56 . 112.6(5) yes C2 . C55 . H551 . 108.7 no C56 . C55 . H551 . 108.7 no C2 . C55 . H552 . 108.7 no C56 . C55 . H552 . 108.7 no H551 . C55 . H552 . 109.5 no C55 . C56 . C57 . 113.0(5) yes C55 . C56 . H561 . 108.6 no C57 . C56 . H561 . 108.6 no C55 . C56 . H562 . 108.6 no C57 . C56 . H562 . 108.6 no H561 . C56 . H562 . 109.5 no C56 . C57 . C58 . 114.0(5) yes C56 . C57 . H571 . 108.3 no C58 . C57 . H571 . 108.3 no C56 . C57 . H572 . 108.3 no C58 . C57 . H572 . 108.3 no H571 . C57 . H572 . 109.5 no C57 . C58 . C59 . 114.5(5) yes C57 . C58 . H581 . 108.2 no C59 . C58 . H581 . 108.2 no C57 . C58 . H582 . 108.2 no C59 . C58 . H582 . 108.2 no H581 . C58 . H582 . 109.5 no C58 . C59 . C60 . 114.3(6) yes C58 . C59 . H591 . 108.3 no C60 . C59 . H591 . 108.3 no C58 . C59 . H592 . 108.3 no C60 . C59 . H592 . 108.3 no H591 . C59 . H592 . 109.5 no C59 . C60 . H601 . 109.5 no C59 . C60 . H602 . 109.5 no H601 . C60 . H602 . 109.5 no C59 . C60 . H603 . 109.5 no H601 . C60 . H603 . 109.5 no H602 . C60 . H603 . 109.5 no N5 . C61 . O2 . 121.1(5) yes N5 . C61 . C62 . 117.0(5) yes O2 . C61 . C62 . 121.9(6) yes C61 . C62 . C63 . 120.2(6) yes C61 . C62 . C64 . 120.0(5) yes C63 . C62 . C64 . 119.8(5) yes C66 2_655 C63 . C62 . 121.4(6) yes C66 2_655 C63 . H631 . 119.3 no C62 . C63 . H631 . 119.3 no C62 . C64 . C64 2_655 119.0(7) yes C62 . C64 . C65 . 120.6(5) yes C64 2_655 C64 . C65 . 120.4(7) yes C64 . C65 . C66 . 119.2(5) yes C64 . C65 . C67 . 119.6(5) yes C66 . C65 . C67 . 121.2(5) yes C63 2_655 C66 . C65 . 120.2(5) yes C63 2_655 C66 . H661 . 119.9 no C65 . C66 . H661 . 119.9 no C65 . C67 . N5 . 118.0(5) yes C65 . C67 . O1 . 122.3(6) yes N5 . C67 . O1 . 119.7(5) yes N5 . C68 . C69 . 111.0(5) yes N5 . C68 . H681 . 109.1 no C69 . C68 . H681 . 109.1 no N5 . C68 . H682 . 109.1 no C69 . C68 . H682 . 109.1 no H681 . C68 . H682 . 109.5 no C68 . C69 . C70 . 112.8(5) yes C68 . C69 . H691 . 108.6 no C70 . C69 . H691 . 108.6 no C68 . C69 . H692 . 108.6 no C70 . C69 . H692 . 108.6 no H691 . C69 . H692 . 109.5 no C69 . C70 . C71 . 112.5(5) yes C69 . C70 . H701 . 108.7 no C71 . C70 . H701 . 108.7 no C69 . C70 . H702 . 108.7 no C71 . C70 . H702 . 108.7 no H701 . C70 . H702 . 109.5 no C70 . C71 . C72 . 114.6(6) yes C70 . C71 . H711 . 108.2 no C72 . C71 . H711 . 108.2 no C70 . C71 . H712 . 108.2 no C72 . C71 . H712 . 108.2 no H711 . C71 . H712 . 109.5 no C71 . C72 . C73 . 113.1(6) yes C71 . C72 . H721 . 108.6 no C73 . C72 . H721 . 108.6 no C71 . C72 . H722 . 108.6 no C73 . C72 . H722 . 108.6 no H721 . C72 . H722 . 109.5 no C72 . C73 . H731 . 109.5 no C72 . C73 . H732 . 109.5 no H731 . C73 . H732 . 109.5 no C72 . C73 . H733 . 109.5 no H731 . C73 . H733 . 109.5 no H732 . C73 . H733 . 109.5 no Cl1 . C74 . Cl2 . 108.8(2) yes Cl1 . C74 . Cl3 . 108.7(2) yes Cl2 . C74 . Cl3 . 108.8(2) yes Cl1 . C74 . H741 . 113.6 no Cl2 . C74 . H741 . 105.0 no Cl3 . C74 . H741 . 111.8 no Cl4 . C74 . Cl5 . 109.3(2) yes Cl4 . C74 . Cl6 . 108.7(2) yes Cl5 . C74 . Cl6 . 108.8(2) yes Cl4 . C74 . H742 . 121.2 no Cl5 . C74 . H742 . 112.5 no Cl6 . C74 . H742 . 94.8 no C74 . Cl3 . H542 2_666 165.3 no C54 . H542 . Cl3 2_666 162.2 no #===END data_js0509 _database_code_depnum_ccdc_archive 'CCDC 715663' #TrackingRef '- CCDC_deposided_merged_cifs_notepad.cif' _audit_creation_date 05-05-25 _audit_creation_method CRYSTALS_ver_12.20 #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment mixed #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2003) ; _computing_publication_material ; CRYSTALS (Watkin et al 2003) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 5.7210(3) _cell_angle_alpha 96.580(2) _cell_length_b 14.9720(7) _cell_angle_beta 100.950(3) _cell_length_c 15.1570(14) _cell_angle_gamma 96.3100(16) _cell_volume 1254.64(15) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'Zn ' 0.2839 1.4301 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097 1.3041 International_Tables_Vol_IV_Table_2.2B 'F ' 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 1 _chemical_formula_sum ' C60 H72 F4 N4 Zn1 ' _chemical_formula_moiety ' C60 H72 F4 N4 Zn1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 990.63 _cell_measurement_reflns_used 107257 _cell_measurement_theta_min 1 _cell_measurement_theta_max 25 _cell_measurement_temperature 150 _exptl_crystal_description ' block ' _exptl_crystal_colour ' red ' _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.311 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 526 _exptl_absorpt_coefficient_mu 0.548 _diffrn_measurement_device_type ; Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.837 _exptl_absorpt_correction_T_max 0.973 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 4103 _reflns_number_total 4103 _diffrn_reflns_av_R_equivalents 0.05 # Number of reflections with Friedels Law is 4103 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 4423 _diffrn_reflns_theta_min 1.382 _diffrn_reflns_theta_max 25.007 _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 18.755 _diffrn_measured_fraction_theta_full 0.953 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _reflns_limit_h_min -6 _reflns_limit_h_max 6 _reflns_limit_k_min -17 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 17 _refine_diff_density_min -0.43 _refine_diff_density_max 0.66 _refine_ls_number_reflns 2404 _refine_ls_number_restraints 0 _refine_ls_number_parameters 314 #_refine_ls_R_factor_ref 0.0696 _refine_ls_wR_factor_ref 0.0736 _refine_ls_goodness_of_fit_ref 1.0782 #_reflns_number_all 4087 _refine_ls_R_factor_all 0.1156 _refine_ls_wR_factor_all 0.0952 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 2404 _refine_ls_R_factor_gt 0.0696 _refine_ls_wR_factor_gt 0.0736 _refine_ls_shift/su_max 0.026626 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.66 0.852 1.28 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius BV, COLLECT Software, 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens F1 F 0.7311(9) 0.4229(3) 0.7745(3) 0.0584 1.0000 Uani . . . . . . F2 F 0.1845(7) 0.4280(3) 0.9685(3) 0.0517 1.0000 Uani . . . . . . N1 N 0.6885(9) 0.0225(3) 0.9181(3) 0.0271 1.0000 Uani . . . . . . N2 N 1.0407(9) 0.1338(4) 1.0557(3) 0.0247 1.0000 Uani . . . . . . C1 C 0.5924(11) 0.1031(5) 0.9128(4) 0.0302 1.0000 Uani . . . . . . C2 C 0.6944(11) 0.1867(4) 0.9631(4) 0.0283 1.0000 Uani . . . . . . C3 C 0.8962(11) 0.2002(4) 1.0370(4) 0.0288 1.0000 Uani . . . . . . C4 C 0.9849(12) 0.2816(4) 1.1017(4) 0.0318 1.0000 Uani . . . . . . C5 C 1.1856(11) 0.2635(4) 1.1576(4) 0.0274 1.0000 Uani . . . . . . C6 C 1.2239(11) 0.1724(4) 1.1266(4) 0.0268 1.0000 Uani . . . . . . C7 C 1.4225(11) 0.1326(4) 1.1636(4) 0.0256 1.0000 Uani . . . . . . C8 C 1.4638(11) 0.0435(4) 1.1420(4) 0.0252 1.0000 Uani . . . . . . C9 C 1.6701(11) 0.0071(4) 1.1862(4) 0.0291 1.0000 Uani . . . . . . C10 C 1.6384(11) -0.0839(4) 1.1544(4) 0.0293 1.0000 Uani . . . . . . C11 C 1.8152(12) -0.1465(5) 1.1831(5) 0.0400 1.0000 Uani . . . . . . C12 C 1.8835(11) 0.0587(5) 1.2526(5) 0.0331 1.0000 Uani . . . . . . C13 C 1.8844(12) 0.0543(5) 1.3536(5) 0.0404 1.0000 Uani . . . . . . C14 C 1.7021(13) 0.1051(5) 1.3917(5) 0.0402 1.0000 Uani . . . . . . C15 C 1.7320(13) 0.1102(5) 1.4941(5) 0.0461 1.0000 Uani . . . . . . C16 C 1.5618(15) 0.1661(6) 1.5338(5) 0.0550 1.0000 Uani . . . . . . C17 C 1.5983(18) 0.1735(8) 1.6360(6) 0.0731 1.0000 Uani . . . . . . C18 C 1.3349(14) 0.3237(5) 1.2416(5) 0.0401 1.0000 Uani . . . . . . C19 C 1.215(3) 0.3120(6) 1.3263(6) 0.1046 1.0000 Uani . . . . . . C20 C 1.297(2) 0.3735(7) 1.4068(8) 0.0879 1.0000 Uani . . . . . . C21 C 1.140(3) 0.3575(10) 1.4770(9) 0.1057 1.0000 Uani . . . . . . C22 C 1.237(2) 0.4208(11) 1.5609(12) 0.1189 1.0000 Uani . . . . . . C23 C 1.105(3) 0.4059(12) 1.6338(9) 0.1230 1.0000 Uani . . . . . . C24 C 0.8783(14) 0.3680(5) 1.1120(5) 0.0410 1.0000 Uani . . . . . . C25 C 0.6005(11) 0.2695(4) 0.9326(4) 0.0304 1.0000 Uani . . . . . . C26 C 0.4239(11) 0.3109(5) 0.9672(4) 0.0323 1.0000 Uani . . . . . . C27 C 0.3544(11) 0.3887(4) 0.9329(5) 0.0359 1.0000 Uani . . . . . . C28 C 0.4539(14) 0.4282(5) 0.8701(5) 0.0434 1.0000 Uani . . . . . . C29 C 0.6305(12) 0.3863(5) 0.8385(5) 0.0391 1.0000 Uani . . . . . . C30 C 0.7064(12) 0.3085(5) 0.8671(4) 0.0352 1.0000 Uani . . . . . . Zn1 Zn 1.0000 0.0000 1.0000 0.0243 1.0000 Uani S . . . . . H71 H 1.5534 0.1740 1.2110 0.0351 1.0000 Uiso . . . . . . H111 H 1.9559 -0.1150 1.2288 0.0541 1.0000 Uiso . . . . . . H112 H 1.7368 -0.1991 1.2073 0.0541 1.0000 Uiso . . . . . . H113 H 1.8776 -0.1734 1.1275 0.0541 1.0000 Uiso . . . . . . H121 H 2.0344 0.0399 1.2381 0.0379 1.0000 Uiso . . . . . . H122 H 1.8860 0.1267 1.2451 0.0379 1.0000 Uiso . . . . . . H131 H 2.0500 0.0776 1.3910 0.0500 1.0000 Uiso . . . . . . H132 H 1.8499 -0.0126 1.3606 0.0500 1.0000 Uiso . . . . . . H141 H 1.7193 0.1686 1.3753 0.0510 1.0000 Uiso . . . . . . H142 H 1.5353 0.0743 1.3615 0.0510 1.0000 Uiso . . . . . . H151 H 1.9044 0.1358 1.5222 0.0582 1.0000 Uiso . . . . . . H152 H 1.7060 0.0455 1.5084 0.0582 1.0000 Uiso . . . . . . H161 H 1.5847 0.2292 1.5163 0.0678 1.0000 Uiso . . . . . . H162 H 1.3913 0.1382 1.5069 0.0678 1.0000 Uiso . . . . . . H171 H 1.4854 0.2120 1.6608 0.0979 1.0000 Uiso . . . . . . H172 H 1.7695 0.2033 1.6657 0.0979 1.0000 Uiso . . . . . . H173 H 1.5762 0.1122 1.6563 0.0979 1.0000 Uiso . . . . . . H181 H 1.5019 0.3027 1.2558 0.0463 1.0000 Uiso . . . . . . H182 H 1.3574 0.3878 1.2312 0.0463 1.0000 Uiso . . . . . . H191 H 1.2091 0.2481 1.3400 0.1128 1.0000 Uiso . . . . . . H192 H 1.0312 0.3204 1.3045 0.1128 1.0000 Uiso . . . . . . H201 H 1.4699 0.3628 1.4335 0.1185 1.0000 Uiso . . . . . . H202 H 1.3072 0.4383 1.3945 0.1185 1.0000 Uiso . . . . . . H211 H 1.1267 0.2913 1.4891 0.1463 1.0000 Uiso . . . . . . H212 H 0.9643 0.3669 1.4502 0.1463 1.0000 Uiso . . . . . . H221 H 1.4191 0.4155 1.5830 0.1407 1.0000 Uiso . . . . . . H222 H 1.2388 0.4875 1.5487 0.1407 1.0000 Uiso . . . . . . H231 H 1.1785 0.4488 1.6919 0.1439 1.0000 Uiso . . . . . . H232 H 1.1163 0.3419 1.6484 0.1439 1.0000 Uiso . . . . . . H233 H 0.9359 0.4139 1.6141 0.1439 1.0000 Uiso . . . . . . H241 H 0.9802 0.4117 1.1642 0.0484 1.0000 Uiso . . . . . . H242 H 0.7120 0.3550 1.1274 0.0484 1.0000 Uiso . . . . . . H243 H 0.8610 0.3960 1.0559 0.0484 1.0000 Uiso . . . . . . H261 H 0.3515 0.2847 1.0171 0.0404 1.0000 Uiso . . . . . . H281 H 0.4014 0.4860 0.8479 0.0464 1.0000 Uiso . . . . . . H301 H 0.8371 0.2794 0.8413 0.0405 1.0000 Uiso . . . . . . 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 F1 0.073(3) 0.056(3) 0.058(3) 0.030(2) 0.025(2) 0.016(2) F2 0.041(2) 0.039(2) 0.078(3) 0.005(2) 0.017(2) 0.0163(19) N1 0.020(3) 0.027(3) 0.034(3) 0.006(2) 0.002(2) 0.008(2) N2 0.025(3) 0.025(3) 0.022(3) -0.002(2) 0.001(2) 0.007(2) C1 0.030(4) 0.038(4) 0.025(4) 0.008(3) 0.007(3) 0.009(3) C2 0.032(3) 0.030(4) 0.025(3) 0.009(3) 0.008(3) 0.006(3) C3 0.027(3) 0.028(4) 0.031(4) 0.000(3) 0.003(3) 0.008(3) C4 0.039(4) 0.031(3) 0.028(4) -0.001(3) 0.015(3) 0.005(3) C5 0.028(3) 0.025(3) 0.026(3) 0.002(3) 0.003(3) -0.002(3) C6 0.038(4) 0.022(3) 0.022(3) 0.001(3) 0.008(3) 0.004(3) C7 0.029(3) 0.029(3) 0.021(3) 0.006(3) 0.005(3) 0.007(3) C8 0.028(3) 0.022(3) 0.025(3) -0.003(3) 0.008(3) 0.003(3) C9 0.024(3) 0.032(4) 0.031(4) 0.003(3) 0.005(3) 0.004(3) C10 0.029(3) 0.030(4) 0.032(4) 0.009(3) 0.008(3) 0.011(3) C11 0.036(4) 0.039(4) 0.040(4) -0.001(3) 0.000(3) 0.007(3) C12 0.023(3) 0.041(4) 0.033(4) 0.005(3) 0.001(3) 0.002(3) C13 0.038(4) 0.037(4) 0.042(4) 0.001(3) 0.001(3) 0.004(3) C14 0.043(4) 0.041(4) 0.033(4) 0.003(3) -0.001(3) 0.008(3) C15 0.044(4) 0.049(5) 0.043(5) 0.006(3) 0.005(3) 0.003(4) C16 0.055(5) 0.071(6) 0.040(4) 0.002(4) 0.010(4) 0.019(4) C17 0.067(6) 0.108(8) 0.040(5) -0.002(5) 0.014(4) 0.001(6) C18 0.053(4) 0.028(4) 0.035(4) 0.005(3) -0.004(3) 0.009(3) C19 0.212(15) 0.044(5) 0.036(5) 0.010(4) -0.007(7) -0.026(7) C20 0.097(8) 0.074(7) 0.082(8) -0.003(6) -0.001(6) 0.014(6) C21 0.150(11) 0.129(10) 0.099(9) 0.075(8) 0.097(9) 0.099(9) C22 0.078(8) 0.132(12) 0.154(14) 0.007(11) 0.031(10) 0.043(8) C23 0.102(10) 0.189(16) 0.069(8) 0.003(9) -0.004(7) 0.033(10) C24 0.052(4) 0.030(4) 0.039(4) 0.000(3) 0.002(3) 0.008(3) C25 0.029(4) 0.032(4) 0.029(3) 0.008(3) 0.000(3) 0.004(3) C26 0.027(3) 0.037(4) 0.039(4) 0.020(3) 0.007(3) 0.016(3) C27 0.024(3) 0.028(4) 0.053(5) -0.004(3) 0.006(3) 0.006(3) C28 0.055(5) 0.027(4) 0.048(5) 0.012(3) -0.001(4) 0.018(3) C29 0.041(4) 0.039(4) 0.039(4) 0.019(3) 0.002(3) 0.008(3) C30 0.033(4) 0.041(4) 0.033(4) 0.003(3) 0.006(3) 0.012(3) Zn1 0.0254(7) 0.0208(7) 0.0267(7) 0.0064(6) 0.0010(6) 0.0081(5) _refine_ls_extinction_method None loop_ _oxford_twin_element_scale_factors 0.631(3) 0.369(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag F1 . C29 . 1.355(8) yes F2 . C27 . 1.354(8) yes N1 . C8 2_757 1.366(8) yes N1 . C1 . 1.386(8) yes N1 . Zn1 . 2.054(5) yes N2 . C3 . 1.381(8) yes N2 . C6 . 1.373(8) yes N2 . Zn1 . 2.053(5) yes C1 . C10 2_757 1.484(9) yes C1 . C2 . 1.393(9) yes C2 . C3 . 1.426(9) yes C2 . C25 . 1.490(9) yes C3 . C4 . 1.452(9) yes C4 . C5 . 1.364(9) yes C4 . C24 . 1.494(10) yes C5 . C6 . 1.445(9) yes C5 . C18 . 1.522(9) yes C6 . C7 . 1.394(9) yes C7 . C8 . 1.394(8) yes C7 . H71 . 1.026 no C8 . C9 . 1.436(8) yes C9 . C10 . 1.373(9) yes C9 . C12 . 1.500(9) yes C10 . C11 . 1.491(9) yes C11 . H111 . 0.990 no C11 . H112 . 1.004 no C11 . H113 . 1.033 no C12 . C13 . 1.539(10) yes C12 . H121 . 0.992 no C12 . H122 . 1.037 no C13 . C14 . 1.517(10) yes C13 . H131 . 1.009 no C13 . H132 . 1.021 no C14 . C15 . 1.522(10) yes C14 . H141 . 1.008 no C14 . H142 . 1.011 no C15 . C16 . 1.515(11) yes C15 . H151 . 1.011 no C15 . H152 . 1.017 no C16 . C17 . 1.512(11) yes C16 . H161 . 1.012 no C16 . H162 . 1.006 no C17 . H171 . 1.008 no C17 . H172 . 1.026 no C17 . H173 . 1.003 no C18 . C19 . 1.583(14) yes C18 . H181 . 1.030 no C18 . H182 . 0.988 no C19 . C20 . 1.410(14) yes C19 . H191 . 1.000 no C19 . H192 . 1.069 no C20 . C21 . 1.540(15) yes C20 . H201 . 1.030 no C20 . H202 . 1.005 no C21 . C22 . 1.47(2) yes C21 . H211 . 1.026 no C21 . H212 . 1.044 no C22 . C23 . 1.48(2) yes C22 . H221 . 1.047 no C22 . H222 . 1.035 no C23 . H231 . 1.018 no C23 . H232 . 1.014 no C23 . H233 . 0.981 no C24 . H241 . 1.008 no C24 . H242 . 1.026 no C24 . H243 . 0.984 no C25 . C26 . 1.394(9) yes C25 . C30 . 1.407(10) yes C26 . C27 . 1.395(9) yes C26 . H261 . 1.024 no C27 . C28 . 1.358(10) yes C28 . C29 . 1.379(11) yes C28 . H281 . 1.018 no C29 . C30 . 1.374(9) yes C30 . H301 . 1.022 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C8 2_757 N1 . C1 . 107.7(5) yes C8 2_757 N1 . Zn1 . 124.1(4) yes C1 . N1 . Zn1 . 128.2(4) yes C3 . N2 . C6 . 106.5(5) yes C3 . N2 . Zn1 . 130.2(4) yes C6 . N2 . Zn1 . 123.2(4) yes C10 2_757 C1 . N1 . 107.9(5) yes C10 2_757 C1 . C2 . 126.6(6) yes N1 . C1 . C2 . 125.5(6) yes C1 . C2 . C3 . 125.0(6) yes C1 . C2 . C25 . 117.7(6) yes C3 . C2 . C25 . 117.1(6) yes C2 . C3 . N2 . 122.6(6) yes C2 . C3 . C4 . 127.5(6) yes N2 . C3 . C4 . 109.8(5) yes C3 . C4 . C5 . 106.4(6) yes C3 . C4 . C24 . 128.9(6) yes C5 . C4 . C24 . 124.6(6) yes C4 . C5 . C6 . 107.3(5) yes C4 . C5 . C18 . 127.4(6) yes C6 . C5 . C18 . 125.1(6) yes C5 . C6 . N2 . 109.8(5) yes C5 . C6 . C7 . 123.6(6) yes N2 . C6 . C7 . 126.6(6) yes C6 . C7 . C8 . 127.0(6) yes C6 . C7 . H71 . 116.204 no C8 . C7 . H71 . 116.753 no C7 . C8 . N1 2_757 126.0(6) yes C7 . C8 . C9 . 123.3(5) yes N1 2_757 C8 . C9 . 110.6(5) yes C8 . C9 . C10 . 107.0(5) yes C8 . C9 . C12 . 126.8(6) yes C10 . C9 . C12 . 126.1(6) yes C1 2_757 C10 . C9 . 106.7(5) yes C1 2_757 C10 . C11 . 129.4(6) yes C9 . C10 . C11 . 123.9(6) yes C10 . C11 . H111 . 112.148 no C10 . C11 . H112 . 110.749 no H111 . C11 . H112 . 109.984 no C10 . C11 . H113 . 109.550 no H111 . C11 . H113 . 107.629 no H112 . C11 . H113 . 106.576 no C9 . C12 . C13 . 116.3(5) yes C9 . C12 . H121 . 110.348 no C13 . C12 . H121 . 109.577 no C9 . C12 . H122 . 107.490 no C13 . C12 . H122 . 105.493 no H121 . C12 . H122 . 107.124 no C12 . C13 . C14 . 115.1(6) yes C12 . C13 . H131 . 109.663 no C14 . C13 . H131 . 109.022 no C12 . C13 . H132 . 106.961 no C14 . C13 . H132 . 108.644 no H131 . C13 . H132 . 107.097 no C13 . C14 . C15 . 113.4(6) yes C13 . C14 . H141 . 108.191 no C15 . C14 . H141 . 109.122 no C13 . C14 . H142 . 108.664 no C15 . C14 . H142 . 109.324 no H141 . C14 . H142 . 108.009 no C14 . C15 . C16 . 114.0(6) yes C14 . C15 . H151 . 107.673 no C16 . C15 . H151 . 110.414 no C14 . C15 . H152 . 107.458 no C16 . C15 . H152 . 109.802 no H151 . C15 . H152 . 107.269 no C15 . C16 . C17 . 113.7(7) yes C15 . C16 . H161 . 108.640 no C17 . C16 . H161 . 108.823 no C15 . C16 . H162 . 109.286 no C17 . C16 . H162 . 108.287 no H161 . C16 . H162 . 107.990 no C16 . C17 . H171 . 112.172 no C16 . C17 . H172 . 110.332 no H171 . C17 . H172 . 106.845 no C16 . C17 . H173 . 111.473 no H171 . C17 . H173 . 108.580 no H172 . C17 . H173 . 107.208 no C5 . C18 . C19 . 110.0(6) yes C5 . C18 . H181 . 108.582 no C19 . C18 . H181 . 107.111 no C5 . C18 . H182 . 111.198 no C19 . C18 . H182 . 111.763 no H181 . C18 . H182 . 108.004 no C18 . C19 . C20 . 119.4(10) yes C18 . C19 . H191 . 111.018 no C20 . C19 . H191 . 110.320 no C18 . C19 . H192 . 105.499 no C20 . C19 . H192 . 105.018 no H191 . C19 . H192 . 104.225 no C19 . C20 . C21 . 111.4(11) yes C19 . C20 . H201 . 107.356 no C21 . C20 . H201 . 108.606 no C19 . C20 . H202 . 111.694 no C21 . C20 . H202 . 110.827 no H201 . C20 . H202 . 106.726 no C20 . C21 . C22 . 109.7(13) yes C20 . C21 . H211 . 111.429 no C22 . C21 . H211 . 111.680 no C20 . C21 . H212 . 109.374 no C22 . C21 . H212 . 110.358 no H211 . C21 . H212 . 104.202 no C21 . C22 . C23 . 113.0(13) yes C21 . C22 . H221 . 109.384 no C23 . C22 . H221 . 110.167 no C21 . C22 . H222 . 111.039 no C23 . C22 . H222 . 109.534 no H221 . C22 . H222 . 103.313 no C22 . C23 . H231 . 111.682 no C22 . C23 . H232 . 108.564 no H231 . C23 . H232 . 106.958 no C22 . C23 . H233 . 110.127 no H231 . C23 . H233 . 109.567 no H232 . C23 . H233 . 109.878 no C4 . C24 . H241 . 110.205 no C4 . C24 . H242 . 109.478 no H241 . C24 . H242 . 106.795 no C4 . C24 . H243 . 111.397 no H241 . C24 . H243 . 110.132 no H242 . C24 . H243 . 108.710 no C2 . C25 . C26 . 124.2(6) yes C2 . C25 . C30 . 116.4(6) yes C26 . C25 . C30 . 119.4(6) yes C25 . C26 . C27 . 118.1(6) yes C25 . C26 . H261 . 119.905 no C27 . C26 . H261 . 122.001 no C26 . C27 . F2 . 116.7(6) yes C26 . C27 . C28 . 123.9(6) yes F2 . C27 . C28 . 119.3(6) yes C27 . C28 . C29 . 116.4(6) yes C27 . C28 . H281 . 121.666 no C29 . C28 . H281 . 121.939 no F1 . C29 . C28 . 118.1(6) yes F1 . C29 . C30 . 118.4(6) yes C28 . C29 . C30 . 123.5(6) yes C25 . C30 . C29 . 118.7(6) yes C25 . C30 . H301 . 120.542 no C29 . C30 . H301 . 120.756 no N1 . Zn1 . N1 2_757 179.994 yes N1 . Zn1 . N2 . 87.45(19) yes N1 2_757 Zn1 . N2 . 92.55(19) yes N1 . Zn1 . N2 2_757 92.55(19) yes N1 2_757 Zn1 . N2 2_757 87.45(19) yes N2 . Zn1 . N2 2_757 179.994 yes #===END data_js0413 _database_code_depnum_ccdc_archive 'CCDC 715664' #TrackingRef '- CCDC_deposided_merged_cifs_notepad.cif' _audit_creation_date 04-10-14 _audit_creation_method CRYSTALS_ver_12.20 #**************************************************************************** #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment mixed #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2003) ; _computing_publication_material ; CRYSTALS (Watkin et al 2003) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 8.1034(2) _cell_angle_alpha 106.0538(10) _cell_length_b 13.3167(3) _cell_angle_beta 95.4992(10) _cell_length_c 13.5586(4) _cell_angle_gamma 105.8473(15) _cell_volume 1329.18(6) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'F ' 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'Zn ' 0.2839 1.4301 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097 1.3041 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 1 _chemical_formula_sum ' C60 H66 F10 N4 Zn1 ' _chemical_formula_moiety ' C60 H66 F10 N4 Zn1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 1098.57 _cell_measurement_reflns_used 8366 _cell_measurement_theta_min 5 _cell_measurement_theta_max 25 _cell_measurement_temperature 180 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' red ' _exptl_crystal_size_min 0.07 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_max 0.27 _exptl_crystal_density_diffrn 1.372 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 574 _exptl_absorpt_coefficient_mu 0.541 _diffrn_measurement_device_type ; Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR97 (Altomare et al, 1999) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.96 # Sheldrick geometric definitions 0.88 0.96 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 180 _diffrn_reflns_number 10193 _reflns_number_total 4812 _diffrn_reflns_av_R_equivalents 0.04 # Number of reflections with Friedels Law is 4812 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 4872 _diffrn_reflns_theta_min 4.638 _diffrn_reflns_theta_max 25.363 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_full 0.989 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _reflns_limit_h_min -9 _reflns_limit_h_max 9 _reflns_limit_k_min -16 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _refine_diff_density_min -0.61 _refine_diff_density_max 0.56 _refine_ls_number_reflns 3977 _refine_ls_number_restraints 0 _refine_ls_number_parameters 340 #_refine_ls_R_factor_ref 0.0445 _refine_ls_wR_factor_ref 0.0544 _refine_ls_goodness_of_fit_ref 1.2213 #_reflns_number_all 4812 _refine_ls_R_factor_all 0.0563 _refine_ls_wR_factor_all 0.0596 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 3977 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_gt 0.0544 _refine_ls_shift/su_max 0.014812 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.37 0.707 0.981 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. and Spagna, R. (1999) SIR97: a new tool for crystal structure determination and refinement.J. App. Cryst. 32, 115-119 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius BV, COLLECT Software, 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Zn1 Zn 0.0000 0.5000 0.5000 0.0218 1.0000 Uani S . . . . . N1 N -0.1749(3) 0.49011(16) 0.37565(15) 0.0231 1.0000 Uani . . . . . . N2 N -0.1055(3) 0.59409(16) 0.60606(15) 0.0231 1.0000 Uani . . . . . . F1 F 0.0844(2) 0.45844(12) 0.07706(12) 0.0348 1.0000 Uani . . . . . . F2 F 0.0098(2) 0.34682(14) -0.12862(12) 0.0415 1.0000 Uani . . . . . . F3 F -0.2328(2) 0.14464(15) -0.20248(12) 0.0473 1.0000 Uani . . . . . . F4 F -0.4048(2) 0.05556(14) -0.06980(14) 0.0485 1.0000 Uani . . . . . . F5 F -0.3399(2) 0.16972(13) 0.13544(13) 0.0398 1.0000 Uani . . . . . . C1 C 0.2870(3) 0.3063(2) 0.33019(19) 0.0263 1.0000 Uani . . . . . . C2 C 0.1707(3) 0.29649(19) 0.24631(19) 0.0247 1.0000 Uani . . . . . . C3 C 0.0551(3) 0.36068(19) 0.28687(18) 0.0223 1.0000 Uani . . . . . . C4 C -0.0835(3) 0.37677(19) 0.22921(19) 0.0237 1.0000 Uani . . . . . . C5 C -0.1904(3) 0.43897(19) 0.26998(18) 0.0230 1.0000 Uani . . . . . . C6 C -0.3342(3) 0.4588(2) 0.21196(19) 0.0257 1.0000 Uani . . . . . . C7 C -0.4043(3) 0.51946(19) 0.28442(19) 0.0253 1.0000 Uani . . . . . . C8 C -0.3047(3) 0.53879(19) 0.38538(18) 0.0240 1.0000 Uani . . . . . . C9 C -0.3369(3) 0.5988(2) 0.47836(19) 0.0265 1.0000 Uani . . . . . . C10 C -0.2454(3) 0.62624(19) 0.57882(19) 0.0246 1.0000 Uani . . . . . . C11 C 0.1754(4) 0.2359(2) 0.1361(2) 0.0338 1.0000 Uani . . . . . . C12 C -0.3963(3) 0.4249(2) 0.0963(2) 0.0326 1.0000 Uani . . . . . . C13 C -0.1250(3) 0.3185(2) 0.11369(19) 0.0249 1.0000 Uani . . . . . . C14 C -0.0411(3) 0.3602(2) 0.04300(19) 0.0259 1.0000 Uani . . . . . . C15 C -0.0766(3) 0.3042(2) -0.0630(2) 0.0304 1.0000 Uani . . . . . . C16 C -0.1997(4) 0.2015(2) -0.1004(2) 0.0330 1.0000 Uani . . . . . . C17 C -0.2861(3) 0.1564(2) -0.0328(2) 0.0327 1.0000 Uani . . . . . . C18 C -0.2503(3) 0.2148(2) 0.0721(2) 0.0293 1.0000 Uani . . . . . . C19 C -0.5539(3) 0.5640(2) 0.2690(2) 0.0297 1.0000 Uani . . . . . . C20 C -0.4962(4) 0.6872(2) 0.2817(2) 0.0360 1.0000 Uani . . . . . . C21 C -0.3983(4) 0.7150(3) 0.1986(2) 0.0434 1.0000 Uani . . . . . . C22 C -0.3186(4) 0.8371(2) 0.2156(2) 0.0407 1.0000 Uani . . . . . . C23 C -0.2309(6) 0.8602(3) 0.1277(3) 0.0604 1.0000 Uani . . . . . . C24 C -0.1299(6) 0.9777(3) 0.1463(4) 0.0692 1.0000 Uani . . . . . . C25 C 0.4336(3) 0.2575(2) 0.3332(2) 0.0308 1.0000 Uani . . . . . . C26 C 0.3847(4) 0.1505(2) 0.3613(2) 0.0401 1.0000 Uani . . . . . . C27 C 0.5356(5) 0.1035(3) 0.3694(3) 0.0500 1.0000 Uani . . . . . . C28 C 0.6798(5) 0.1708(4) 0.4612(3) 0.0618 1.0000 Uani . . . . . . C29 C 0.8279(8) 0.1238(6) 0.4712(4) 0.0992 1.0000 Uani . . . . . . C30 C 0.9608(7) 0.1831(7) 0.5672(5) 0.1091 1.0000 Uani . . . . . . H91 H -0.4393 0.6263 0.4723 0.0329 1.0000 Uiso . . . . . . H111 H 0.0775 0.2392 0.0877 0.0417 1.0000 Uiso . . . . . . H112 H 0.2892 0.2701 0.1178 0.0417 1.0000 Uiso . . . . . . H113 H 0.1621 0.1571 0.1294 0.0417 1.0000 Uiso . . . . . . H121 H -0.3251 0.3812 0.0591 0.0394 1.0000 Uiso . . . . . . H122 H -0.3827 0.4921 0.0741 0.0394 1.0000 Uiso . . . . . . H123 H -0.5218 0.3792 0.0782 0.0394 1.0000 Uiso . . . . . . H191 H -0.6292 0.5511 0.3215 0.0363 1.0000 Uiso . . . . . . H192 H -0.6236 0.5228 0.1970 0.0363 1.0000 Uiso . . . . . . H201 H -0.6021 0.7117 0.2785 0.0460 1.0000 Uiso . . . . . . H202 H -0.4183 0.7279 0.3514 0.0460 1.0000 Uiso . . . . . . H211 H -0.4816 0.6819 0.1302 0.0530 1.0000 Uiso . . . . . . H212 H -0.3021 0.6812 0.1956 0.0530 1.0000 Uiso . . . . . . H221 H -0.4134 0.8721 0.2219 0.0509 1.0000 Uiso . . . . . . H222 H -0.2302 0.8700 0.2818 0.0509 1.0000 Uiso . . . . . . H231 H -0.3228 0.8354 0.0638 0.0771 1.0000 Uiso . . . . . . H232 H -0.1480 0.8162 0.1154 0.0771 1.0000 Uiso . . . . . . H241 H -0.0771 0.9847 0.0836 0.0871 1.0000 Uiso . . . . . . H242 H -0.2109 1.0233 0.1573 0.0871 1.0000 Uiso . . . . . . H243 H -0.0361 1.0042 0.2089 0.0871 1.0000 Uiso . . . . . . H251 H 0.5353 0.3122 0.3864 0.0390 1.0000 Uiso . . . . . . H252 H 0.4674 0.2416 0.2628 0.0390 1.0000 Uiso . . . . . . H261 H 0.3451 0.1654 0.4299 0.0485 1.0000 Uiso . . . . . . H262 H 0.2869 0.0944 0.3059 0.0485 1.0000 Uiso . . . . . . H271 H 0.4888 0.0282 0.3755 0.0644 1.0000 Uiso . . . . . . H272 H 0.5858 0.0985 0.3043 0.0644 1.0000 Uiso . . . . . . H281 H 0.6293 0.1779 0.5263 0.0775 1.0000 Uiso . . . . . . H282 H 0.7290 0.2458 0.4543 0.0775 1.0000 Uiso . . . . . . H291 H 0.7759 0.0458 0.4702 0.1286 1.0000 Uiso . . . . . . H292 H 0.8858 0.1244 0.4098 0.1286 1.0000 Uiso . . . . . . H301 H 1.0528 0.1459 0.5674 0.1322 1.0000 Uiso . . . . . . H302 H 0.9048 0.1820 0.6297 0.1322 1.0000 Uiso . . . . . . H303 H 1.0147 0.2606 0.5692 0.1322 1.0000 Uiso . . . . . . 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 0.0216(2) 0.0246(2) 0.0198(2) 0.00540(15) 0.00207(14) 0.01062(15) N1 0.0244(10) 0.0250(10) 0.0199(9) 0.0055(8) 0.0012(8) 0.0103(8) N2 0.0248(10) 0.0249(10) 0.0219(10) 0.0076(8) 0.0047(8) 0.0112(8) F1 0.0347(8) 0.0317(8) 0.0319(8) 0.0102(6) 0.0029(6) 0.0018(6) F2 0.0508(10) 0.0487(10) 0.0300(8) 0.0169(7) 0.0166(7) 0.0161(8) F3 0.0556(11) 0.0515(10) 0.0220(8) -0.0045(7) 0.0012(7) 0.0147(8) F4 0.0484(10) 0.0332(9) 0.0420(9) -0.0039(7) 0.0027(8) -0.0036(7) F5 0.0418(9) 0.0344(8) 0.0367(9) 0.0094(7) 0.0140(7) 0.0014(7) C1 0.0268(12) 0.0267(12) 0.0278(12) 0.0089(10) 0.0077(10) 0.0112(10) C2 0.0280(12) 0.0238(11) 0.0245(12) 0.0080(9) 0.0086(9) 0.0099(10) C3 0.0231(11) 0.0229(11) 0.0207(11) 0.0064(9) 0.0042(9) 0.0073(9) C4 0.0258(11) 0.0205(11) 0.0229(11) 0.0059(9) 0.0043(9) 0.0051(9) C5 0.0217(11) 0.0223(11) 0.0228(11) 0.0067(9) 0.0015(9) 0.0048(9) C6 0.0248(12) 0.0249(12) 0.0250(12) 0.0083(9) -0.0009(9) 0.0054(9) C7 0.0246(12) 0.0244(11) 0.0250(12) 0.0071(9) 0.0009(9) 0.0069(9) C8 0.0221(11) 0.0259(11) 0.0245(12) 0.0073(9) 0.0013(9) 0.0100(9) C9 0.0238(11) 0.0298(12) 0.0289(13) 0.0088(10) 0.0023(10) 0.0143(10) C10 0.0243(11) 0.0247(11) 0.0261(12) 0.0076(10) 0.0051(9) 0.0102(9) C11 0.0379(14) 0.0411(15) 0.0268(13) 0.0063(11) 0.0082(11) 0.0229(12) C12 0.0333(13) 0.0404(14) 0.0234(12) 0.0073(11) -0.0029(10) 0.0162(11) C13 0.0246(11) 0.0270(12) 0.0231(11) 0.0060(10) 0.0011(9) 0.0112(10) C14 0.0246(11) 0.0238(11) 0.0270(12) 0.0057(10) 0.0021(9) 0.0070(9) C15 0.0332(13) 0.0374(14) 0.0236(12) 0.0100(11) 0.0073(10) 0.0150(11) C16 0.0347(14) 0.0359(14) 0.0220(12) -0.0006(10) -0.0009(10) 0.0130(11) C17 0.0296(13) 0.0267(13) 0.0327(13) 0.0000(11) -0.0001(11) 0.0058(10) C18 0.0291(12) 0.0289(13) 0.0292(13) 0.0083(11) 0.0070(10) 0.0085(10) C19 0.0266(12) 0.0355(14) 0.0287(12) 0.0097(11) 0.0003(10) 0.0146(11) C20 0.0379(14) 0.0413(15) 0.0360(14) 0.0135(12) 0.0070(12) 0.0225(12) C21 0.0553(18) 0.0402(16) 0.0372(15) 0.0107(13) 0.0130(14) 0.0189(14) C22 0.0449(16) 0.0381(15) 0.0446(16) 0.0166(13) 0.0080(13) 0.0183(13) C23 0.073(2) 0.0471(19) 0.072(2) 0.0230(18) 0.035(2) 0.0249(18) C24 0.073(3) 0.055(2) 0.089(3) 0.033(2) 0.036(2) 0.017(2) C25 0.0323(13) 0.0376(14) 0.0280(12) 0.0083(11) 0.0079(10) 0.0209(11) C26 0.0396(15) 0.0341(14) 0.0479(16) 0.0099(12) 0.0036(13) 0.0180(12) C27 0.062(2) 0.0458(17) 0.0523(19) 0.0137(15) 0.0060(16) 0.0367(16) C28 0.057(2) 0.074(2) 0.061(2) 0.0190(19) 0.0044(17) 0.0371(19) C29 0.090(3) 0.149(5) 0.083(3) 0.037(3) 0.000(3) 0.081(4) C30 0.070(3) 0.160(6) 0.108(4) 0.073(4) -0.008(3) 0.030(3) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zn1 . N2 2_566 2.0479(19) yes Zn1 . N1 2_566 2.0461(19) yes Zn1 . N1 . 2.0461(19) yes Zn1 . N2 . 2.0479(19) yes N1 . C5 . 1.383(3) yes N1 . C8 . 1.377(3) yes N2 . C3 2_566 1.380(3) yes N2 . C10 . 1.370(3) yes F1 . C14 . 1.344(3) yes F2 . C15 . 1.336(3) yes F3 . C16 . 1.341(3) yes F4 . C17 . 1.345(3) yes F5 . C18 . 1.338(3) yes C1 . C10 2_566 1.440(3) yes C1 . C2 . 1.358(4) yes C1 . C25 . 1.504(3) yes C2 . C3 . 1.479(3) yes C2 . C11 . 1.499(3) yes C3 . C4 . 1.405(3) yes C4 . C5 . 1.405(3) yes C4 . C13 . 1.501(3) yes C5 . C6 . 1.468(3) yes C6 . C7 . 1.363(3) yes C6 . C12 . 1.500(3) yes C7 . C8 . 1.439(3) yes C7 . C19 . 1.509(3) yes C8 . C9 . 1.384(3) yes C9 . C10 . 1.386(3) yes C9 . H91 . 0.999 no C11 . H111 . 0.999 no C11 . H112 . 0.998 no C11 . H113 . 1.003 no C12 . H121 . 1.001 no C12 . H122 . 1.001 no C12 . H123 . 0.999 no C13 . C14 . 1.380(4) yes C13 . C18 . 1.396(4) yes C14 . C15 . 1.384(4) yes C15 . C16 . 1.378(4) yes C16 . C17 . 1.375(4) yes C17 . C18 . 1.377(4) yes C19 . C20 . 1.534(4) yes C19 . H191 . 1.002 no C19 . H192 . 1.001 no C20 . C21 . 1.509(4) yes C20 . H201 . 0.999 no C20 . H202 . 1.000 no C21 . C22 . 1.517(4) yes C21 . H211 . 1.001 no C21 . H212 . 1.000 no C22 . C23 . 1.505(5) yes C22 . H221 . 1.000 no C22 . H222 . 0.999 no C23 . C24 . 1.492(5) yes C23 . H231 . 0.999 no C23 . H232 . 1.002 no C24 . H241 . 1.003 no C24 . H242 . 1.005 no C24 . H243 . 0.994 no C25 . C26 . 1.533(4) yes C25 . H251 . 1.000 no C25 . H252 . 1.000 no C26 . C27 . 1.526(4) yes C26 . H261 . 0.999 no C26 . H262 . 1.001 no C27 . C28 . 1.500(5) yes C27 . H271 . 1.000 no C27 . H272 . 1.000 no C28 . C29 . 1.510(5) yes C28 . H281 . 1.000 no C28 . H282 . 1.003 no C29 . C30 . 1.475(8) yes C29 . H291 . 1.005 no C29 . H292 . 0.994 no C30 . H301 . 1.002 no C30 . H302 . 1.001 no C30 . H303 . 0.996 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N2 2_566 Zn1 . N1 2_566 93.13(8) yes N2 2_566 Zn1 . N1 . 86.87(8) yes N1 2_566 Zn1 . N1 . 179.994 yes N2 2_566 Zn1 . N2 . 179.994 yes N1 2_566 Zn1 . N2 . 86.87(8) yes N1 . Zn1 . N2 . 93.13(8) yes Zn1 . N1 . C5 . 130.32(15) yes Zn1 . N1 . C8 . 123.42(15) yes C5 . N1 . C8 . 106.26(19) yes C3 2_566 N2 . Zn1 . 129.90(15) yes C3 2_566 N2 . C10 . 106.63(19) yes Zn1 . N2 . C10 . 123.44(15) yes C10 2_566 C1 . C2 . 107.3(2) yes C10 2_566 C1 . C25 . 124.1(2) yes C2 . C1 . C25 . 128.6(2) yes C1 . C2 . C3 . 106.4(2) yes C1 . C2 . C11 . 123.5(2) yes C3 . C2 . C11 . 129.9(2) yes C2 . C3 . N2 2_566 108.9(2) yes C2 . C3 . C4 . 127.4(2) yes N2 2_566 C3 . C4 . 123.6(2) yes C3 . C4 . C5 . 126.1(2) yes C3 . C4 . C13 . 116.8(2) yes C5 . C4 . C13 . 117.1(2) yes C4 . C5 . N1 . 123.1(2) yes C4 . C5 . C6 . 127.5(2) yes N1 . C5 . C6 . 109.4(2) yes C5 . C6 . C7 . 106.6(2) yes C5 . C6 . C12 . 129.4(2) yes C7 . C6 . C12 . 124.0(2) yes C6 . C7 . C8 . 107.2(2) yes C6 . C7 . C19 . 129.5(2) yes C8 . C7 . C19 . 123.3(2) yes C7 . C8 . N1 . 110.6(2) yes C7 . C8 . C9 . 123.8(2) yes N1 . C8 . C9 . 125.6(2) yes C8 . C9 . C10 . 128.6(2) yes C8 . C9 . H91 . 115.760 no C10 . C9 . H91 . 115.666 no C1 2_566 C10 . C9 . 123.6(2) yes C1 2_566 C10 . N2 . 110.7(2) yes C9 . C10 . N2 . 125.8(2) yes C2 . C11 . H111 . 109.512 no C2 . C11 . H112 . 109.595 no H111 . C11 . H112 . 109.695 no C2 . C11 . H113 . 109.278 no H111 . C11 . H113 . 109.306 no H112 . C11 . H113 . 109.441 no C6 . C12 . H121 . 109.462 no C6 . C12 . H122 . 109.460 no H121 . C12 . H122 . 109.290 no C6 . C12 . H123 . 109.620 no H121 . C12 . H123 . 109.507 no H122 . C12 . H123 . 109.487 no C4 . C13 . C14 . 123.5(2) yes C4 . C13 . C18 . 120.6(2) yes C14 . C13 . C18 . 116.0(2) yes F1 . C14 . C13 . 119.7(2) yes F1 . C14 . C15 . 117.3(2) yes C13 . C14 . C15 . 123.0(2) yes C14 . C15 . F2 . 121.1(2) yes C14 . C15 . C16 . 119.1(2) yes F2 . C15 . C16 . 119.8(2) yes F3 . C16 . C15 . 120.0(3) yes F3 . C16 . C17 . 120.0(2) yes C15 . C16 . C17 . 120.0(2) yes F4 . C17 . C16 . 119.6(2) yes F4 . C17 . C18 . 120.7(3) yes C16 . C17 . C18 . 119.7(2) yes C13 . C18 . F5 . 119.5(2) yes C13 . C18 . C17 . 122.3(2) yes F5 . C18 . C17 . 118.2(2) yes C7 . C19 . C20 . 113.8(2) yes C7 . C19 . H191 . 108.309 no C20 . C19 . H191 . 108.423 no C7 . C19 . H192 . 108.438 no C20 . C19 . H192 . 108.496 no H191 . C19 . H192 . 109.264 no C19 . C20 . C21 . 113.2(2) yes C19 . C20 . H201 . 108.650 no C21 . C20 . H201 . 108.533 no C19 . C20 . H202 . 108.493 no C21 . C20 . H202 . 108.378 no H201 . C20 . H202 . 109.547 no C20 . C21 . C22 . 115.1(3) yes C20 . C21 . H211 . 107.935 no C22 . C21 . H211 . 108.086 no C20 . C21 . H212 . 108.080 no C22 . C21 . H212 . 108.139 no H211 . C21 . H212 . 109.375 no C21 . C22 . C23 . 112.9(3) yes C21 . C22 . H221 . 108.590 no C23 . C22 . H221 . 108.527 no C21 . C22 . H222 . 108.580 no C23 . C22 . H222 . 108.688 no H221 . C22 . H222 . 109.492 no C22 . C23 . C24 . 115.3(3) yes C22 . C23 . H231 . 108.055 no C24 . C23 . H231 . 108.338 no C22 . C23 . H232 . 107.853 no C24 . C23 . H232 . 107.725 no H231 . C23 . H232 . 109.431 no C23 . C24 . H241 . 109.394 no C23 . C24 . H242 . 109.226 no H241 . C24 . H242 . 108.857 no C23 . C24 . H243 . 110.011 no H241 . C24 . H243 . 109.732 no H242 . C24 . H243 . 109.600 no C1 . C25 . C26 . 113.1(2) yes C1 . C25 . H251 . 108.647 no C26 . C25 . H251 . 108.458 no C1 . C25 . H252 . 108.585 no C26 . C25 . H252 . 108.525 no H251 . C25 . H252 . 109.466 no C25 . C26 . C27 . 113.3(3) yes C25 . C26 . H261 . 108.600 no C27 . C26 . H261 . 108.568 no C25 . C26 . H262 . 108.487 no C27 . C26 . H262 . 108.357 no H261 . C26 . H262 . 109.478 no C26 . C27 . C28 . 114.1(3) yes C26 . C27 . H271 . 108.407 no C28 . C27 . H271 . 108.092 no C26 . C27 . H272 . 108.425 no C28 . C27 . H272 . 108.231 no H271 . C27 . H272 . 109.526 no C27 . C28 . C29 . 114.5(4) yes C27 . C28 . H281 . 108.424 no C29 . C28 . H281 . 108.501 no C27 . C28 . H282 . 108.229 no C29 . C28 . H282 . 107.909 no H281 . C28 . H282 . 109.216 no C28 . C29 . C30 . 114.7(5) yes C28 . C29 . H291 . 107.441 no C30 . C29 . H291 . 108.224 no C28 . C29 . H292 . 108.195 no C30 . C29 . H292 . 108.674 no H291 . C29 . H292 . 109.541 no C29 . C30 . H301 . 109.122 no C29 . C30 . H302 . 109.577 no H301 . C30 . H302 . 109.312 no C29 . C30 . H303 . 109.412 no H301 . C30 . H303 . 109.660 no H302 . C30 . H303 . 109.742 no #===END data_js0510c _database_code_depnum_ccdc_archive 'CCDC 715665' #TrackingRef '- CCDC_deposided_merged_cifs_notepad.cif' _audit_creation_date 05-05-16 _audit_creation_method CRYSTALS_ver_12.80 _oxford_structure_analysis_title '5161911 Compound X' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 8.2430(2) _cell_length_b 13.0858(3) _cell_length_c 13.5204(4) _cell_angle_alpha 76.6654(11) _cell_angle_beta 85.1757(11) _cell_angle_gamma 79.9850(16) _cell_volume 1395.98(6) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Zn 0.2839 1.4301 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097 1.3041 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 1 # Given Formula = C64 H84 N4 O4 Zn1 # Dc = 1.24 Fooo = 558.00 Mu = 4.91 M = 519.39 # Found Formula = C64 H84 N4 O4 Zn1 # Dc = 1.24 FOOO = 558.00 Mu = 4.91 M = 519.39 _chemical_formula_sum 'C64 H84 N4 O4 Zn1' _chemical_formula_moiety 'C64 H84 N4 O4 Zn1' _chemical_compound_source ? _chemical_formula_weight 1038.78 _cell_measurement_reflns_used 10184 _cell_measurement_theta_min 3 _cell_measurement_theta_max 25 _cell_measurement_temperature 180 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.236 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 558 _exptl_absorpt_coefficient_mu 0.491 # Sheldrick geometric approximatio 0.95 0.95 # No experimental values of Tmin/max available _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.95 _exptl_absorpt_correction_T_max 0.95 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'Nonius (1997-2001). COLLECT.' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 180 _diffrn_reflns_number 12448 _reflns_number_total 5049 _diffrn_reflns_av_R_equivalents 0.049 # Number of reflections with Friedels Law is 5049 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 5092 _diffrn_reflns_theta_min 2.929 _diffrn_reflns_theta_max 25.312 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _reflns_limit_h_min -9 _reflns_limit_h_max 9 _reflns_limit_k_min -15 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.49 _refine_diff_density_max 1.04 _refine_ls_number_reflns 4025 _refine_ls_number_restraints 0 _refine_ls_number_parameters 331 #_refine_ls_R_factor_ref 0.0439 _refine_ls_wR_factor_ref 0.0522 _refine_ls_goodness_of_fit_ref 1.0937 #_reflns_number_all 5033 _refine_ls_R_factor_all 0.0574 _refine_ls_wR_factor_all 0.0573 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 4025 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_gt 0.0522 _refine_ls_shift/su_max 0.000278 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.82 0.683 1.47 ; # Check this file using the IUCr facility at: # http://checkcif.iucr.org/ # The content below is held in the file 'script/refcif.dat'. This is a text # file which you may edit to reflect local conditions. # Items which need looking at are represented by a '?'. # Items for which there are choices are prefixed with 'choose from'. # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens O1 O 0.4814(2) -0.13589(14) 0.44429(14) 0.0434 1.0000 Uani . . . . . . O2 O 0.8050(2) -0.43190(14) 0.65059(15) 0.0452 1.0000 Uani . . . . . . N1 N 0.3251(2) 0.00897(14) 1.11600(14) 0.0259 1.0000 Uani . . . . . . N2 N 0.3770(2) -0.08952(14) 0.93652(14) 0.0265 1.0000 Uani . . . . . . C1 C 0.1873(3) -0.03976(17) 1.12847(17) 0.0274 1.0000 Uani . . . . . . C2 C 0.1428(3) -0.09559(17) 1.06227(17) 0.0288 1.0000 Uani . . . . . . C3 C 0.2283(3) -0.11952(17) 0.97578(17) 0.0278 1.0000 Uani . . . . . . C4 C 0.1745(3) -0.18395(18) 0.91565(18) 0.0300 1.0000 Uani . . . . . . C5 C 0.2933(3) -0.19621(18) 0.84121(19) 0.0325 1.0000 Uani . . . . . . C6 C 0.4204(3) -0.13413(17) 0.85332(17) 0.0280 1.0000 Uani . . . . . . C7 C 0.5636(3) -0.11952(17) 0.79004(17) 0.0281 1.0000 Uani . . . . . . C8 C 0.6812(3) -0.05804(17) 0.80308(17) 0.0267 1.0000 Uani . . . . . . C9 C 0.8277(3) -0.03660(18) 0.73651(18) 0.0304 1.0000 Uani . . . . . . C10 C 0.9077(3) 0.02363(17) 0.78029(17) 0.0291 1.0000 Uani . . . . . . C11 C 0.5930(3) -0.17599(17) 0.70453(17) 0.0290 1.0000 Uani . . . . . . C12 C 0.6899(3) -0.27825(18) 0.72120(18) 0.0328 1.0000 Uani . . . . . . C13 C 0.7150(3) -0.33188(18) 0.64311(19) 0.0325 1.0000 Uani . . . . . . C14 C 0.6489(3) -0.28720(19) 0.54860(18) 0.0333 1.0000 Uani . . . . . . C15 C 0.5550(3) -0.18669(19) 0.53319(18) 0.0321 1.0000 Uani . . . . . . C16 C 0.5276(3) -0.13118(18) 0.61133(18) 0.0324 1.0000 Uani . . . . . . C17 C 0.5018(3) -0.1899(2) 0.3626(2) 0.0447 1.0000 Uani . . . . . . C18 C 0.8754(4) -0.4815(2) 0.7454(2) 0.0523 1.0000 Uani . . . . . . C19 C 0.8842(3) -0.0681(2) 0.6378(2) 0.0403 1.0000 Uani . . . . . . C20 C 0.2832(4) -0.2617(3) 0.7652(2) 0.0536 1.0000 Uani . . . . . . C21 C 0.0169(3) -0.22964(19) 0.93715(18) 0.0327 1.0000 Uani . . . . . . C22 C 0.0293(3) -0.3325(2) 1.0180(2) 0.0434 1.0000 Uani . . . . . . C23 C -0.1303(4) -0.3808(2) 1.0359(2) 0.0495 1.0000 Uani . . . . . . C24 C -0.2698(4) -0.3181(3) 1.0850(3) 0.0631 1.0000 Uani . . . . . . C25 C -0.4282(5) -0.3671(3) 1.1019(3) 0.0685 1.0000 Uani . . . . . . C26 C -0.5483(7) -0.3242(5) 1.1718(5) 0.1036 1.0000 Uani . . . . . . C27 C 1.0589(3) 0.0743(2) 0.74294(19) 0.0350 1.0000 Uani . . . . . . C28 C 1.0131(3) 0.1946(2) 0.6950(2) 0.0376 1.0000 Uani . . . . . . C29 C 0.9458(3) 0.2168(2) 0.59035(19) 0.0381 1.0000 Uani . . . . . . C30 C 0.8803(3) 0.3341(2) 0.5484(2) 0.0413 1.0000 Uani . . . . . . C31 C 0.8110(4) 0.3544(2) 0.4446(2) 0.0473 1.0000 Uani . . . . . . C32 C 0.7337(5) 0.4699(3) 0.4048(3) 0.0639 1.0000 Uani . . . . . . Zn1 Zn 0.5000 0.0000 1.0000 0.0245 1.0000 Uani S . . . . . H21 H 0.0388 -0.1219 1.0789 0.0420 1.0000 Uiso . . . . . . H121 H 0.7372 -0.3101 0.7869 0.0500 1.0000 Uiso . . . . . . H141 H 0.6696 -0.3266 0.4956 0.0510 1.0000 Uiso . . . . . . H161 H 0.4625 -0.0612 0.5996 0.0500 1.0000 Uiso . . . . . . H171 H 0.4426 -0.1452 0.3033 0.0835 1.0000 Uiso . . . . . . H172 H 0.6190 -0.2054 0.3418 0.0839 1.0000 Uiso . . . . . . H173 H 0.4594 -0.2584 0.3821 0.0838 1.0000 Uiso . . . . . . H181 H 0.9323 -0.5522 0.7409 0.0908 1.0000 Uiso . . . . . . H182 H 0.9534 -0.4396 0.7610 0.0907 1.0000 Uiso . . . . . . H183 H 0.7888 -0.4889 0.7988 0.0904 1.0000 Uiso . . . . . . H191 H 0.9894 -0.0437 0.6121 0.0798 1.0000 Uiso . . . . . . H192 H 0.9001 -0.1445 0.6430 0.0797 1.0000 Uiso . . . . . . H193 H 0.8036 -0.0357 0.5853 0.0800 1.0000 Uiso . . . . . . H201 H 0.3830 -0.3122 0.7594 0.1127 1.0000 Uiso . . . . . . H202 H 0.1898 -0.2993 0.7815 0.1125 1.0000 Uiso . . . . . . H203 H 0.2682 -0.2165 0.6975 0.1128 1.0000 Uiso . . . . . . H211 H -0.0719 -0.1756 0.9582 0.0509 1.0000 Uiso . . . . . . H212 H -0.0157 -0.2432 0.8715 0.0509 1.0000 Uiso . . . . . . H221 H 0.0594 -0.3179 1.0830 0.0649 1.0000 Uiso . . . . . . H222 H 0.1223 -0.3851 0.9958 0.0651 1.0000 Uiso . . . . . . H231 H -0.1086 -0.4531 1.0816 0.0715 1.0000 Uiso . . . . . . H232 H -0.1651 -0.3888 0.9690 0.0713 1.0000 Uiso . . . . . . H241 H -0.2397 -0.3106 1.1513 0.1014 1.0000 Uiso . . . . . . H242 H -0.2972 -0.2441 1.0424 0.1013 1.0000 Uiso . . . . . . H251 H -0.3930 -0.4426 1.1343 0.1046 1.0000 Uiso . . . . . . H252 H -0.4794 -0.3811 1.0357 0.1020 1.0000 Uiso . . . . . . H261 H -0.6574 -0.3511 1.1759 0.2065 1.0000 Uiso . . . . . . H262 H -0.5002 -0.3442 1.2396 0.2064 1.0000 Uiso . . . . . . H263 H -0.5653 -0.2439 1.1492 0.2067 1.0000 Uiso . . . . . . H271 H 1.1299 0.0641 0.8027 0.0525 1.0000 Uiso . . . . . . H272 H 1.1236 0.0385 0.6910 0.0529 1.0000 Uiso . . . . . . H281 H 1.1115 0.2301 0.6886 0.0584 1.0000 Uiso . . . . . . H282 H 0.9267 0.2287 0.7411 0.0576 1.0000 Uiso . . . . . . H291 H 1.0360 0.1911 0.5429 0.0591 1.0000 Uiso . . . . . . H292 H 0.8558 0.1750 0.5928 0.0588 1.0000 Uiso . . . . . . H301 H 0.9714 0.3766 0.5432 0.0632 1.0000 Uiso . . . . . . H302 H 0.7921 0.3601 0.5967 0.0631 1.0000 Uiso . . . . . . H311 H 0.9025 0.3342 0.3951 0.0710 1.0000 Uiso . . . . . . H312 H 0.7269 0.3070 0.4482 0.0709 1.0000 Uiso . . . . . . H321 H 0.6920 0.4786 0.3363 0.1149 1.0000 Uiso . . . . . . H322 H 0.8156 0.5173 0.3999 0.1150 1.0000 Uiso . . . . . . H323 H 0.6405 0.4911 0.4501 0.1151 1.0000 Uiso . . . . . . 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 O1 0.0588(11) 0.0390(10) 0.0316(9) -0.0105(7) -0.0127(8) 0.0033(8) O2 0.0585(12) 0.0304(9) 0.0447(11) -0.0135(8) -0.0111(9) 0.0093(8) N1 0.0258(9) 0.0245(9) 0.0286(9) -0.0072(7) 0.0000(7) -0.0054(7) N2 0.0295(9) 0.0262(9) 0.0257(9) -0.0079(7) -0.0010(7) -0.0068(7) C1 0.0256(11) 0.0267(10) 0.0295(11) -0.0069(9) -0.0017(8) -0.0023(8) C2 0.0269(11) 0.0276(11) 0.0324(12) -0.0056(9) -0.0015(9) -0.0067(9) C3 0.0288(11) 0.0247(10) 0.0306(11) -0.0058(9) -0.0045(9) -0.0054(8) C4 0.0327(12) 0.0269(11) 0.0319(11) -0.0054(9) -0.0076(9) -0.0073(9) C5 0.0367(12) 0.0306(11) 0.0341(12) -0.0111(10) -0.0030(9) -0.0099(9) C6 0.0298(11) 0.0264(11) 0.0298(11) -0.0090(9) -0.0022(9) -0.0058(9) C7 0.0315(11) 0.0252(10) 0.0284(11) -0.0077(9) -0.0033(9) -0.0031(9) C8 0.0287(11) 0.0239(10) 0.0281(11) -0.0071(9) -0.0031(9) -0.0033(8) C9 0.0304(11) 0.0285(11) 0.0323(12) -0.0086(9) 0.0020(9) -0.0038(9) C10 0.0287(11) 0.0261(11) 0.0316(12) -0.0062(9) 0.0014(9) -0.0037(8) C11 0.0330(11) 0.0278(11) 0.0291(11) -0.0098(9) 0.0007(9) -0.0090(9) C12 0.0364(12) 0.0314(12) 0.0307(12) -0.0059(9) -0.0055(9) -0.0050(9) C13 0.0356(12) 0.0265(11) 0.0363(12) -0.0108(9) -0.0002(10) -0.0029(9) C14 0.0379(12) 0.0341(12) 0.0313(12) -0.0135(10) 0.0007(9) -0.0076(10) C15 0.0361(12) 0.0330(12) 0.0277(11) -0.0071(9) -0.0022(9) -0.0055(9) C16 0.0375(12) 0.0268(11) 0.0330(12) -0.0090(9) -0.0026(10) -0.0014(9) C17 0.0471(15) 0.0574(17) 0.0309(13) -0.0160(12) -0.0059(11) -0.0011(12) C18 0.0683(19) 0.0371(14) 0.0446(16) -0.0074(12) -0.0078(13) 0.0101(13) C19 0.0425(14) 0.0445(14) 0.0384(14) -0.0187(11) 0.0086(11) -0.0111(11) C20 0.0511(16) 0.0692(19) 0.0592(18) -0.0391(16) 0.0124(13) -0.0336(15) C21 0.0334(12) 0.0329(12) 0.0350(12) -0.0078(10) -0.0065(9) -0.0111(9) C22 0.0405(14) 0.0349(13) 0.0534(16) 0.0006(11) -0.0119(12) -0.0118(11) C23 0.0475(16) 0.0437(15) 0.0567(17) 0.0019(13) -0.0095(13) -0.0193(12) C24 0.0554(19) 0.078(2) 0.064(2) -0.0248(18) 0.0090(16) -0.0273(17) C25 0.057(2) 0.081(2) 0.068(2) -0.0097(19) 0.0065(16) -0.0260(18) C26 0.085(3) 0.116(4) 0.110(4) -0.022(3) -0.008(3) -0.017(3) C27 0.0293(11) 0.0399(13) 0.0372(13) -0.0122(10) 0.0053(9) -0.0080(10) C28 0.0374(13) 0.0391(13) 0.0402(13) -0.0118(11) 0.0042(10) -0.0151(10) C29 0.0415(13) 0.0398(13) 0.0365(13) -0.0124(11) 0.0043(10) -0.0131(11) C30 0.0512(15) 0.0375(13) 0.0400(14) -0.0134(11) 0.0010(11) -0.0147(11) C31 0.0599(17) 0.0425(15) 0.0427(15) -0.0103(12) -0.0059(13) -0.0139(12) C32 0.079(2) 0.0531(18) 0.057(2) -0.0082(15) -0.0161(17) -0.0025(16) Zn1 0.0251(2) 0.0237(2) 0.0265(2) -0.00798(14) -0.00159(13) -0.00528(13) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.7051(16) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 . C15 . 1.367(3) yes O1 . C17 . 1.427(3) yes O2 . C13 . 1.374(3) yes O2 . C18 . 1.419(4) yes N1 . C8 2_657 1.384(3) yes N1 . C1 . 1.377(3) yes N1 . Zn1 . 2.0487(18) yes N2 . C3 . 1.379(3) yes N2 . C6 . 1.377(3) yes N2 . Zn1 . 2.0396(18) yes C1 . C10 2_657 1.442(3) yes C1 . C2 . 1.386(3) yes C2 . C3 . 1.384(3) yes C2 . H21 . 0.969 no C3 . C4 . 1.440(3) yes C4 . C5 . 1.361(3) yes C4 . C21 . 1.502(3) yes C5 . C6 . 1.473(3) yes C5 . C20 . 1.498(3) yes C6 . C7 . 1.412(3) yes C7 . C8 . 1.409(3) yes C7 . C11 . 1.492(3) yes C8 . C9 . 1.472(3) yes C9 . C10 . 1.367(3) yes C9 . C19 . 1.500(3) yes C10 . C27 . 1.509(3) yes C11 . C12 . 1.414(3) yes C11 . C16 . 1.373(3) yes C12 . C13 . 1.380(3) yes C12 . H121 . 0.972 no C13 . C14 . 1.390(4) yes C14 . C15 . 1.385(3) yes C14 . H141 . 0.963 no C15 . C16 . 1.397(3) yes C16 . H161 . 0.964 no C17 . H171 . 0.986 no C17 . H172 . 0.983 no C17 . H173 . 0.990 no C18 . H181 . 0.975 no C18 . H182 . 0.978 no C18 . H183 . 0.972 no C19 . H191 . 0.985 no C19 . H192 . 0.973 no C19 . H193 . 0.983 no C20 . H201 . 0.972 no C20 . H202 . 0.968 no C20 . H203 . 0.972 no C21 . C22 . 1.520(3) yes C21 . H211 . 0.997 no C21 . H212 . 1.011 no C22 . C23 . 1.534(4) yes C22 . H221 . 1.001 no C22 . H222 . 1.012 no C23 . C24 . 1.494(5) yes C23 . H231 . 0.999 no C23 . H232 . 1.005 no C24 . C25 . 1.530(5) yes C24 . H241 . 0.981 no C24 . H242 . 1.004 no C25 . C26 . 1.443(7) yes C25 . H251 . 0.987 no C25 . H252 . 1.085 no C26 . H261 . 1.015 no C26 . H262 . 0.991 no C26 . H263 . 1.013 no C27 . C28 . 1.551(4) yes C27 . H271 . 1.007 no C27 . H272 . 0.999 no C28 . C29 . 1.510(4) yes C28 . H281 . 0.991 no C28 . H282 . 1.019 no C29 . C30 . 1.526(4) yes C29 . H291 . 1.005 no C29 . H292 . 0.990 no C30 . C31 . 1.510(4) yes C30 . H301 . 0.998 no C30 . H302 . 1.003 no C31 . C32 . 1.525(4) yes C31 . H311 . 1.007 no C31 . H312 . 0.999 no C32 . H321 . 0.990 no C32 . H322 . 0.982 no C32 . H323 . 0.984 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C15 . O1 . C17 . 118.01(19) yes C13 . O2 . C18 . 116.7(2) yes C8 2_657 N1 . C1 . 106.08(17) yes C8 2_657 N1 . Zn1 . 130.14(14) yes C1 . N1 . Zn1 . 123.75(15) yes C3 . N2 . C6 . 106.65(18) yes C3 . N2 . Zn1 . 123.30(15) yes C6 . N2 . Zn1 . 130.02(15) yes C10 2_657 C1 . N1 . 110.83(19) yes C10 2_657 C1 . C2 . 123.9(2) yes N1 . C1 . C2 . 125.2(2) yes C1 . C2 . C3 . 128.4(2) yes C1 . C2 . H21 . 115.9 no C3 . C2 . H21 . 115.6 no C2 . C3 . N2 . 126.1(2) yes C2 . C3 . C4 . 123.7(2) yes N2 . C3 . C4 . 110.2(2) yes C3 . C4 . C5 . 107.4(2) yes C3 . C4 . C21 . 124.1(2) yes C5 . C4 . C21 . 128.5(2) yes C4 . C5 . C6 . 106.5(2) yes C4 . C5 . C20 . 122.9(2) yes C6 . C5 . C20 . 130.6(2) yes C5 . C6 . N2 . 109.18(19) yes C5 . C6 . C7 . 126.6(2) yes N2 . C6 . C7 . 124.2(2) yes C6 . C7 . C8 . 125.0(2) yes C6 . C7 . C11 . 116.89(19) yes C8 . C7 . C11 . 118.1(2) yes C7 . C8 . N1 2_657 123.5(2) yes C7 . C8 . C9 . 126.9(2) yes N1 2_657 C8 . C9 . 109.60(18) yes C8 . C9 . C10 . 106.4(2) yes C8 . C9 . C19 . 129.8(2) yes C10 . C9 . C19 . 123.8(2) yes C1 2_657 C10 . C9 . 107.1(2) yes C1 2_657 C10 . C27 . 122.8(2) yes C9 . C10 . C27 . 130.0(2) yes C7 . C11 . C12 . 118.6(2) yes C7 . C11 . C16 . 121.5(2) yes C12 . C11 . C16 . 119.9(2) yes C11 . C12 . C13 . 118.9(2) yes C11 . C12 . H121 . 120.2 no C13 . C12 . H121 . 120.8 no C12 . C13 . O2 . 124.2(2) yes C12 . C13 . C14 . 121.6(2) yes O2 . C13 . C14 . 114.2(2) yes C13 . C14 . C15 . 118.9(2) yes C13 . C14 . H141 . 119.4 no C15 . C14 . H141 . 121.7 no C14 . C15 . O1 . 124.0(2) yes C14 . C15 . C16 . 120.5(2) yes O1 . C15 . C16 . 115.5(2) yes C15 . C16 . C11 . 120.3(2) yes C15 . C16 . H161 . 119.7 no C11 . C16 . H161 . 120.1 no O1 . C17 . H171 . 110.1 no O1 . C17 . H172 . 110.7 no H171 . C17 . H172 . 108.2 no O1 . C17 . H173 . 111.7 no H171 . C17 . H173 . 108.5 no H172 . C17 . H173 . 107.5 no O2 . C18 . H181 . 108.1 no O2 . C18 . H182 . 110.3 no H181 . C18 . H182 . 109.9 no O2 . C18 . H183 . 109.8 no H181 . C18 . H183 . 108.6 no H182 . C18 . H183 . 110.1 no C9 . C19 . H191 . 110.8 no C9 . C19 . H192 . 113.3 no H191 . C19 . H192 . 107.4 no C9 . C19 . H193 . 111.0 no H191 . C19 . H193 . 107.2 no H192 . C19 . H193 . 106.8 no C5 . C20 . H201 . 113.0 no C5 . C20 . H202 . 110.9 no H201 . C20 . H202 . 109.4 no C5 . C20 . H203 . 110.5 no H201 . C20 . H203 . 105.7 no H202 . C20 . H203 . 107.0 no C4 . C21 . C22 . 113.93(19) yes C4 . C21 . H211 . 109.0 no C22 . C21 . H211 . 109.5 no C4 . C21 . H212 . 107.9 no C22 . C21 . H212 . 109.0 no H211 . C21 . H212 . 107.3 no C21 . C22 . C23 . 113.4(2) yes C21 . C22 . H221 . 108.3 no C23 . C22 . H221 . 109.6 no C21 . C22 . H222 . 107.9 no C23 . C22 . H222 . 109.6 no H221 . C22 . H222 . 107.9 no C22 . C23 . C24 . 114.4(3) yes C22 . C23 . H231 . 109.1 no C24 . C23 . H231 . 106.9 no C22 . C23 . H232 . 109.0 no C24 . C23 . H232 . 109.1 no H231 . C23 . H232 . 108.1 no C23 . C24 . C25 . 113.7(3) yes C23 . C24 . H241 . 110.7 no C25 . C24 . H241 . 107.6 no C23 . C24 . H242 . 110.6 no C25 . C24 . H242 . 107.3 no H241 . C24 . H242 . 106.6 no C24 . C25 . C26 . 114.0(4) yes C24 . C25 . H251 . 104.9 no C26 . C25 . H251 . 106.4 no C24 . C25 . H252 . 117.4 no C26 . C25 . H252 . 114.7 no H251 . C25 . H252 . 96.6 no C25 . C26 . H261 . 113.0 no C25 . C26 . H262 . 107.4 no H261 . C26 . H262 . 109.9 no C25 . C26 . H263 . 107.9 no H261 . C26 . H263 . 110.2 no H262 . C26 . H263 . 108.2 no C10 . C27 . C28 . 111.67(19) yes C10 . C27 . H271 . 108.0 no C28 . C27 . H271 . 109.8 no C10 . C27 . H272 . 110.2 no C28 . C27 . H272 . 108.8 no H271 . C27 . H272 . 108.3 no C27 . C28 . C29 . 113.4(2) yes C27 . C28 . H281 . 110.2 no C29 . C28 . H281 . 107.4 no C27 . C28 . H282 . 109.3 no C29 . C28 . H282 . 108.4 no H281 . C28 . H282 . 108.1 no C28 . C29 . C30 . 113.6(2) yes C28 . C29 . H291 . 108.3 no C30 . C29 . H291 . 109.6 no C28 . C29 . H292 . 109.1 no C30 . C29 . H292 . 108.8 no H291 . C29 . H292 . 107.3 no C29 . C30 . C31 . 112.9(2) yes C29 . C30 . H301 . 109.4 no C31 . C30 . H301 . 108.2 no C29 . C30 . H302 . 109.5 no C31 . C30 . H302 . 109.0 no H301 . C30 . H302 . 107.7 no C30 . C31 . C32 . 113.6(2) yes C30 . C31 . H311 . 108.7 no C32 . C31 . H311 . 108.7 no C30 . C31 . H312 . 108.3 no C32 . C31 . H312 . 109.7 no H311 . C31 . H312 . 107.7 no C31 . C32 . H321 . 109.9 no C31 . C32 . H322 . 110.5 no H321 . C32 . H322 . 108.6 no C31 . C32 . H323 . 110.5 no H321 . C32 . H323 . 108.3 no H322 . C32 . H323 . 109.0 no N1 . Zn1 . N1 2_657 179.994 yes N1 . Zn1 . N2 . 93.10(7) yes N1 2_657 Zn1 . N2 . 86.90(7) yes N1 . Zn1 . N2 2_657 86.90(7) yes N1 2_657 Zn1 . N2 2_657 93.10(7) yes N2 . Zn1 . N2 2_657 179.994 yes #===END data_js0522 _database_code_depnum_ccdc_archive 'CCDC 715666' #TrackingRef '- CCDC_deposided_merged_cifs_notepad.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H38 N2 O4' _chemical_formula_sum 'C38 H38 N2 O4' _chemical_formula_weight 586.70 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 16.017(1) _cell_length_b 8.561(1) _cell_length_c 22.982(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3151.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 13675 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.237 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.906 _exptl_absorpt_correction_T_max 0.992 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; Molecule is almost centrosymmetric but all attempts to solve/refine in a higher group have failed. Refinement was performed by Dr John Davies, Cambridge Chemistry. 2658 Friedel pairs were averaged for the refinement. ; _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.383 _refine_diff_density_min -0.219 _refine_diff_density_rms 0.062 _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 16259 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0305 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3661 _reflns_number_gt 3299 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0704P)^2^+0.6961P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.7(15) _refine_ls_number_reflns 3661 _refine_ls_number_parameters 405 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1251 _refine_ls_wR_factor_gt 0.1196 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.15259(13) 0.5169(3) 0.33876(10) 0.0381(5) Uani 1 1 d . . . O2 O 0.36108(13) 0.4803(2) 0.47228(9) 0.0321(5) Uani 1 1 d . . . O3 O 0.59023(13) 0.0033(3) 0.27983(11) 0.0406(5) Uani 1 1 d . . . O4 O 0.38119(12) 0.0366(2) 0.14701(8) 0.0305(4) Uani 1 1 d . . . N1 N 0.25789(13) 0.5016(2) 0.40500(10) 0.0219(4) Uani 1 1 d . . . N2 N 0.48645(13) 0.0246(2) 0.21304(10) 0.0227(5) Uani 1 1 d . . . C1 C 0.33628(15) 0.4485(3) 0.42404(11) 0.0231(5) Uani 1 1 d . . . C2 C 0.38510(15) 0.3539(3) 0.38196(11) 0.0208(5) Uani 1 1 d . . . C3 C 0.46455(16) 0.3066(3) 0.39622(11) 0.0257(5) Uani 1 1 d . . . H3 H 0.4884 0.3375 0.4323 0.031 Uiso 1 1 calc R . . C4 C 0.51053(16) 0.2126(3) 0.35752(12) 0.0270(5) Uani 1 1 d . . . H4 H 0.5657 0.1818 0.3673 0.032 Uiso 1 1 calc R . . C5 C 0.47609(15) 0.1655(3) 0.30590(11) 0.0220(5) Uani 1 1 d . . . C6 C 0.52359(15) 0.0588(3) 0.26696(11) 0.0249(5) Uani 1 1 d . . . C7 C 0.40757(15) 0.0730(3) 0.19452(11) 0.0230(5) Uani 1 1 d . . . C8 C 0.35860(15) 0.1697(3) 0.23632(11) 0.0223(5) Uani 1 1 d . . . C9 C 0.27887(15) 0.2151(3) 0.22252(11) 0.0261(5) Uani 1 1 d . . . H9 H 0.2545 0.1817 0.1869 0.031 Uiso 1 1 calc R . . C10 C 0.23303(16) 0.3101(3) 0.26050(12) 0.0274(5) Uani 1 1 d . . . H10 H 0.1780 0.3413 0.2505 0.033 Uiso 1 1 calc R . . C11 C 0.26765(15) 0.3586(3) 0.31244(11) 0.0224(5) Uani 1 1 d . . . C12 C 0.21987(15) 0.4639(3) 0.35160(12) 0.0254(5) Uani 1 1 d . . . C13 C 0.34924(15) 0.3102(3) 0.32839(11) 0.0201(5) Uani 1 1 d . . . C14 C 0.39516(15) 0.2145(3) 0.28969(11) 0.0200(4) Uani 1 1 d . . . C15 C 0.21105(15) 0.6025(3) 0.44426(11) 0.0237(5) Uani 1 1 d . . . C16 C 0.15237(16) 0.5338(3) 0.48102(12) 0.0262(6) Uani 1 1 d . . . C17 C 0.13738(18) 0.3588(3) 0.48286(14) 0.0339(6) Uani 1 1 d . . . H17 H 0.1848 0.3075 0.4619 0.041 Uiso 1 1 calc R . . C18 C 0.0572(2) 0.3132(4) 0.45147(18) 0.0506(9) Uani 1 1 d . . . H18A H 0.0589 0.3524 0.4114 0.076 Uiso 1 1 calc R . . H18B H 0.0092 0.3587 0.4718 0.076 Uiso 1 1 calc R . . H18C H 0.0519 0.1991 0.4510 0.076 Uiso 1 1 calc R . . C19 C 0.1372(2) 0.2968(4) 0.54519(17) 0.0479(8) Uani 1 1 d . . . H19A H 0.1885 0.3297 0.5649 0.072 Uiso 1 1 calc R . . H19B H 0.1343 0.1825 0.5446 0.072 Uiso 1 1 calc R . . H19C H 0.0887 0.3385 0.5660 0.072 Uiso 1 1 calc R . . C20 C 0.10692(17) 0.6343(3) 0.51720(13) 0.0323(6) Uani 1 1 d . . . H20 H 0.0660 0.5923 0.5427 0.039 Uiso 1 1 calc R . . C21 C 0.12071(19) 0.7939(3) 0.51647(13) 0.0350(6) Uani 1 1 d . . . H21 H 0.0890 0.8603 0.5411 0.042 Uiso 1 1 calc R . . C22 C 0.18036(19) 0.8568(3) 0.48002(14) 0.0353(6) Uani 1 1 d . . . H22 H 0.1892 0.9665 0.4800 0.042 Uiso 1 1 calc R . . C23 C 0.22792(16) 0.7624(3) 0.44321(12) 0.0282(5) Uani 1 1 d . . . C24 C 0.2952(2) 0.8301(3) 0.40340(15) 0.0378(7) Uani 1 1 d . . . H24 H 0.3368 0.7448 0.3967 0.045 Uiso 1 1 calc R . . C25 C 0.3428(3) 0.9660(5) 0.4306(2) 0.0656(12) Uani 1 1 d . . . H25A H 0.3903 0.9936 0.4057 0.098 Uiso 1 1 calc R . . H25B H 0.3632 0.9354 0.4691 0.098 Uiso 1 1 calc R . . H25C H 0.3056 1.0563 0.4344 0.098 Uiso 1 1 calc R . . C26 C 0.2617(3) 0.8743(6) 0.3451(2) 0.0768(14) Uani 1 1 d . . . H26A H 0.3082 0.8985 0.3189 0.115 Uiso 1 1 calc R . . H26B H 0.2257 0.9662 0.3489 0.115 Uiso 1 1 calc R . . H26C H 0.2293 0.7871 0.3291 0.115 Uiso 1 1 calc R . . C27 C 0.53369(15) -0.0749(3) 0.17358(11) 0.0237(5) Uani 1 1 d . . . C28 C 0.59430(17) -0.0063(3) 0.13798(13) 0.0267(6) Uani 1 1 d . . . C29 C 0.61419(18) 0.1668(3) 0.14013(14) 0.0359(7) Uani 1 1 d . . . H29 H 0.5682 0.2196 0.1620 0.043 Uiso 1 1 calc R . . C30 C 0.6959(3) 0.1975(4) 0.1731(2) 0.0648(11) Uani 1 1 d . . . H30A H 0.6926 0.1505 0.2119 0.097 Uiso 1 1 calc R . . H30B H 0.7046 0.3104 0.1768 0.097 Uiso 1 1 calc R . . H30C H 0.7426 0.1512 0.1516 0.097 Uiso 1 1 calc R . . C31 C 0.6180(3) 0.2393(4) 0.07983(18) 0.0540(9) Uani 1 1 d . . . H31A H 0.5677 0.2109 0.0580 0.081 Uiso 1 1 calc R . . H31B H 0.6674 0.2005 0.0593 0.081 Uiso 1 1 calc R . . H31C H 0.6213 0.3532 0.0833 0.081 Uiso 1 1 calc R . . C32 C 0.63783(17) -0.1058(3) 0.10070(13) 0.0316(6) Uani 1 1 d . . . H32 H 0.6800 -0.0640 0.0761 0.038 Uiso 1 1 calc R . . C33 C 0.62089(18) -0.2642(3) 0.09877(13) 0.0341(6) Uani 1 1 d . . . H33 H 0.6508 -0.3294 0.0726 0.041 Uiso 1 1 calc R . . C34 C 0.56054(18) -0.3282(3) 0.13481(14) 0.0326(6) Uani 1 1 d . . . H34 H 0.5499 -0.4373 0.1333 0.039 Uiso 1 1 calc R . . C35 C 0.51501(16) -0.2348(3) 0.17333(12) 0.0268(5) Uani 1 1 d . . . C36 C 0.44888(18) -0.3045(3) 0.21306(14) 0.0310(6) Uani 1 1 d . . . H36 H 0.4094 -0.2184 0.2235 0.037 Uiso 1 1 calc R . . C37 C 0.3976(2) -0.4323(4) 0.18392(17) 0.0481(8) Uani 1 1 d . . . H37A H 0.3716 -0.3908 0.1486 0.072 Uiso 1 1 calc R . . H37B H 0.3542 -0.4685 0.2107 0.072 Uiso 1 1 calc R . . H37C H 0.4342 -0.5199 0.1737 0.072 Uiso 1 1 calc R . . C38 C 0.4874(2) -0.3637(5) 0.26985(18) 0.0603(11) Uani 1 1 d . . . H38A H 0.5196 -0.2795 0.2880 0.090 Uiso 1 1 calc R . . H38B H 0.5244 -0.4522 0.2615 0.090 Uiso 1 1 calc R . . H38C H 0.4429 -0.3972 0.2963 0.090 Uiso 1 1 calc R . . 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 O1 0.0287(10) 0.0507(12) 0.0351(13) -0.0130(10) -0.0066(9) 0.0151(9) O2 0.0375(11) 0.0382(11) 0.0207(10) -0.0063(8) -0.0047(9) 0.0076(8) O3 0.0313(11) 0.0539(12) 0.0366(13) -0.0148(10) -0.0068(10) 0.0166(9) O4 0.0352(10) 0.0345(10) 0.0219(10) -0.0052(8) -0.0026(8) 0.0076(8) N1 0.0211(10) 0.0247(9) 0.0200(11) -0.0031(8) 0.0008(9) 0.0026(8) N2 0.0244(10) 0.0228(10) 0.0210(12) -0.0026(8) 0.0038(9) 0.0021(8) C1 0.0251(11) 0.0220(11) 0.0223(12) 0.0007(9) 0.0002(10) -0.0006(9) C2 0.0228(11) 0.0194(11) 0.0202(12) -0.0002(9) 0.0011(9) -0.0015(8) C3 0.0252(12) 0.0296(13) 0.0223(12) -0.0052(10) -0.0049(9) 0.0005(9) C4 0.0218(12) 0.0298(13) 0.0292(14) -0.0041(10) -0.0053(10) 0.0027(9) C5 0.0211(11) 0.0234(11) 0.0214(12) -0.0015(9) 0.0010(9) -0.0012(9) C6 0.0230(11) 0.0276(12) 0.0242(13) -0.0037(10) -0.0017(10) 0.0013(9) C7 0.0259(12) 0.0220(11) 0.0210(12) -0.0012(9) 0.0007(10) -0.0002(9) C8 0.0242(12) 0.0225(11) 0.0204(12) -0.0002(9) 0.0007(9) -0.0005(9) C9 0.0264(12) 0.0288(12) 0.0232(13) -0.0048(10) -0.0043(10) 0.0016(9) C10 0.0213(12) 0.0347(13) 0.0262(13) -0.0030(10) -0.0028(10) 0.0058(10) C11 0.0217(11) 0.0239(12) 0.0215(12) -0.0031(9) 0.0002(9) 0.0016(9) C12 0.0240(12) 0.0281(12) 0.0241(13) -0.0024(10) 0.0002(10) 0.0026(9) C13 0.0222(11) 0.0185(11) 0.0195(12) 0.0006(8) 0.0008(9) -0.0023(8) C14 0.0202(10) 0.0191(10) 0.0207(11) 0.0000(9) -0.0004(8) -0.0021(8) C15 0.0252(11) 0.0238(12) 0.0220(12) -0.0017(9) 0.0006(10) 0.0051(9) C16 0.0265(13) 0.0290(13) 0.0231(14) 0.0025(10) 0.0023(11) 0.0040(10) C17 0.0370(15) 0.0278(13) 0.0367(16) 0.0029(12) 0.0141(12) 0.0032(11) C18 0.063(2) 0.0374(17) 0.051(2) 0.0017(15) -0.0014(17) -0.0135(15) C19 0.053(2) 0.0412(18) 0.049(2) 0.0153(15) 0.0024(16) -0.0006(14) C20 0.0335(14) 0.0380(15) 0.0254(13) -0.0004(11) 0.0063(11) 0.0073(11) C21 0.0392(15) 0.0349(15) 0.0307(15) -0.0102(12) 0.0030(12) 0.0122(12) C22 0.0457(16) 0.0240(13) 0.0361(16) -0.0061(11) -0.0030(13) 0.0045(11) C23 0.0308(13) 0.0262(12) 0.0275(13) 0.0004(10) -0.0003(11) 0.0016(10) C24 0.0453(17) 0.0299(14) 0.0381(16) 0.0013(12) 0.0059(13) -0.0040(12) C25 0.081(3) 0.061(2) 0.054(2) -0.0030(19) 0.004(2) -0.037(2) C26 0.069(3) 0.112(3) 0.050(2) 0.035(2) -0.011(2) -0.037(3) C27 0.0255(12) 0.0251(12) 0.0207(11) -0.0034(9) -0.0004(9) 0.0052(9) C28 0.0262(12) 0.0292(13) 0.0247(15) 0.0012(10) 0.0007(11) 0.0050(10) C29 0.0367(14) 0.0281(14) 0.0429(18) 0.0029(11) 0.0146(13) 0.0019(11) C30 0.069(3) 0.045(2) 0.081(3) -0.0022(19) -0.010(2) -0.0192(17) C31 0.068(2) 0.0418(18) 0.052(2) 0.0161(16) 0.0152(19) 0.0072(16) C32 0.0308(13) 0.0387(15) 0.0254(13) 0.0004(11) 0.0058(11) 0.0058(11) C33 0.0345(14) 0.0382(15) 0.0297(15) -0.0076(12) 0.0017(12) 0.0106(12) C34 0.0338(14) 0.0267(13) 0.0372(15) -0.0076(11) -0.0024(12) 0.0037(11) C35 0.0268(12) 0.0270(12) 0.0266(13) -0.0032(10) -0.0026(10) 0.0018(9) C36 0.0330(13) 0.0244(12) 0.0356(15) 0.0010(11) 0.0044(12) -0.0014(10) C37 0.0441(18) 0.0438(17) 0.056(2) -0.0023(16) 0.0030(16) -0.0142(14) C38 0.055(2) 0.080(3) 0.046(2) 0.0265(19) -0.0093(17) -0.0247(19) _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 O1 C12 1.206(3) . ? O2 C1 1.209(3) . ? O3 C6 1.205(3) . ? O4 C7 1.212(3) . ? N1 C1 1.405(3) . ? N1 C12 1.407(3) . ? N1 C15 1.457(3) . ? N2 C7 1.396(3) . ? N2 C6 1.405(3) . ? N2 C27 1.456(3) . ? C1 C2 1.484(3) . ? C2 C3 1.375(3) . ? C2 C13 1.409(3) . ? C3 C4 1.407(4) . ? C3 H3 0.9500 . ? C4 C5 1.369(4) . ? C4 H4 0.9500 . ? C5 C14 1.412(3) . ? C5 C6 1.488(3) . ? C7 C8 1.491(3) . ? C8 C9 1.372(3) . ? C8 C14 1.412(3) . ? C9 C10 1.401(4) . ? C9 H9 0.9500 . ? C10 C11 1.380(4) . ? C10 H10 0.9500 . ? C11 C13 1.419(3) . ? C11 C12 1.486(3) . ? C13 C14 1.415(3) . ? C15 C16 1.394(4) . ? C15 C23 1.396(4) . ? C16 C20 1.401(4) . ? C16 C17 1.518(4) . ? C17 C18 1.524(5) . ? C17 C19 1.528(5) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.384(4) . ? C20 H20 0.9500 . ? C21 C22 1.380(4) . ? C21 H21 0.9500 . ? C22 C23 1.396(4) . ? C22 H22 0.9500 . ? C23 C24 1.527(4) . ? C24 C26 1.492(5) . ? C24 C25 1.526(5) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.399(4) . ? C27 C35 1.401(3) . ? C28 C32 1.395(4) . ? C28 C29 1.517(4) . ? C29 C31 1.520(5) . ? C29 C30 1.534(5) . ? C29 H29 1.0000 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.383(4) . ? C32 H32 0.9500 . ? C33 C34 1.386(4) . ? C33 H33 0.9500 . ? C34 C35 1.398(4) . ? C34 H34 0.9500 . ? C35 C36 1.521(4) . ? C36 C37 1.523(4) . ? C36 C38 1.530(5) . ? C36 H36 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? 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 C1 N1 C12 125.7(2) . . ? C1 N1 C15 117.3(2) . . ? C12 N1 C15 116.9(2) . . ? C7 N2 C6 126.2(2) . . ? C7 N2 C27 117.0(2) . . ? C6 N2 C27 116.8(2) . . ? O2 C1 N1 120.4(2) . . ? O2 C1 C2 123.2(2) . . ? N1 C1 C2 116.4(2) . . ? C3 C2 C13 120.5(2) . . ? C3 C2 C1 119.5(2) . . ? C13 C2 C1 120.0(2) . . ? C2 C3 C4 120.1(2) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 120.3(2) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C14 120.7(2) . . ? C4 C5 C6 119.7(2) . . ? C14 C5 C6 119.5(2) . . ? O3 C6 N2 120.6(2) . . ? O3 C6 C5 123.2(2) . . ? N2 C6 C5 116.2(2) . . ? O4 C7 N2 120.9(2) . . ? O4 C7 C8 122.7(2) . . ? N2 C7 C8 116.4(2) . . ? C9 C8 C14 120.7(2) . . ? C9 C8 C7 119.9(2) . . ? C14 C8 C7 119.5(2) . . ? C8 C9 C10 120.5(2) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C11 C10 C9 120.2(2) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C13 120.4(2) . . ? C10 C11 C12 120.0(2) . . ? C13 C11 C12 119.7(2) . . ? O1 C12 N1 120.9(2) . . ? O1 C12 C11 122.7(2) . . ? N1 C12 C11 116.4(2) . . ? C2 C13 C14 119.4(2) . . ? C2 C13 C11 121.6(2) . . ? C14 C13 C11 119.0(2) . . ? C8 C14 C5 121.9(2) . . ? C8 C14 C13 119.2(2) . . ? C5 C14 C13 118.9(2) . . ? C16 C15 C23 123.7(2) . . ? C16 C15 N1 118.2(2) . . ? C23 C15 N1 118.1(2) . . ? C15 C16 C20 116.8(2) . . ? C15 C16 C17 122.7(2) . . ? C20 C16 C17 120.5(2) . . ? C16 C17 C18 111.9(3) . . ? C16 C17 C19 111.7(3) . . ? C18 C17 C19 110.7(3) . . ? C16 C17 H17 107.4 . . ? C18 C17 H17 107.4 . . ? C19 C17 H17 107.4 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C16 121.1(3) . . ? C21 C20 H20 119.5 . . ? C16 C20 H20 119.5 . . ? C22 C21 C20 120.2(2) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 121.3(2) . . ? C21 C22 H22 119.3 . . ? C23 C22 H22 119.3 . . ? C22 C23 C15 116.8(2) . . ? C22 C23 C24 121.9(2) . . ? C15 C23 C24 121.2(2) . . ? C26 C24 C25 110.7(3) . . ? C26 C24 C23 112.4(3) . . ? C25 C24 C23 113.4(3) . . ? C26 C24 H24 106.6 . . ? C25 C24 H24 106.6 . . ? C23 C24 H24 106.6 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C35 123.8(2) . . ? C28 C27 N2 118.6(2) . . ? C35 C27 N2 117.6(2) . . ? C32 C28 C27 116.8(2) . . ? C32 C28 C29 120.8(3) . . ? C27 C28 C29 122.5(2) . . ? C28 C29 C31 112.2(3) . . ? C28 C29 C30 111.3(3) . . ? C31 C29 C30 110.2(3) . . ? C28 C29 H29 107.7 . . ? C31 C29 H29 107.7 . . ? C30 C29 H29 107.7 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C28 121.3(3) . . ? C33 C32 H32 119.3 . . ? C28 C32 H32 119.3 . . ? C32 C33 C34 120.3(2) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? C33 C34 C35 121.1(2) . . ? C33 C34 H34 119.5 . . ? C35 C34 H34 119.5 . . ? C34 C35 C27 116.7(2) . . ? C34 C35 C36 121.2(2) . . ? C27 C35 C36 122.0(2) . . ? C35 C36 C37 113.2(3) . . ? C35 C36 C38 111.2(2) . . ? C37 C36 C38 110.8(3) . . ? C35 C36 H36 107.1 . . ? C37 C36 H36 107.1 . . ? C38 C36 H36 107.1 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? 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 C12 N1 C1 O2 -175.5(2) . . . . ? C15 N1 C1 O2 3.4(3) . . . . ? C12 N1 C1 C2 4.7(3) . . . . ? C15 N1 C1 C2 -176.4(2) . . . . ? O2 C1 C2 C3 -4.0(4) . . . . ? N1 C1 C2 C3 175.8(2) . . . . ? O2 C1 C2 C13 174.5(2) . . . . ? N1 C1 C2 C13 -5.7(3) . . . . ? C13 C2 C3 C4 -0.6(4) . . . . ? C1 C2 C3 C4 177.9(2) . . . . ? C2 C3 C4 C5 -1.1(4) . . . . ? C3 C4 C5 C14 2.2(4) . . . . ? C3 C4 C5 C6 -176.5(2) . . . . ? C7 N2 C6 O3 175.6(3) . . . . ? C27 N2 C6 O3 -2.2(4) . . . . ? C7 N2 C6 C5 -4.4(4) . . . . ? C27 N2 C6 C5 177.7(2) . . . . ? C4 C5 C6 O3 4.2(4) . . . . ? C14 C5 C6 O3 -174.5(3) . . . . ? C4 C5 C6 N2 -175.7(2) . . . . ? C14 C5 C6 N2 5.6(3) . . . . ? C6 N2 C7 O4 -179.8(2) . . . . ? C27 N2 C7 O4 -1.9(3) . . . . ? C6 N2 C7 C8 -0.1(3) . . . . ? C27 N2 C7 C8 177.7(2) . . . . ? O4 C7 C8 C9 2.9(4) . . . . ? N2 C7 C8 C9 -176.7(2) . . . . ? O4 C7 C8 C14 -176.7(2) . . . . ? N2 C7 C8 C14 3.7(3) . . . . ? C14 C8 C9 C10 1.7(4) . . . . ? C7 C8 C9 C10 -177.9(2) . . . . ? C8 C9 C10 C11 -0.3(4) . . . . ? C9 C10 C11 C13 -1.3(4) . . . . ? C9 C10 C11 C12 177.9(2) . . . . ? C1 N1 C12 O1 -179.1(3) . . . . ? C15 N1 C12 O1 2.0(4) . . . . ? C1 N1 C12 C11 0.0(4) . . . . ? C15 N1 C12 C11 -178.9(2) . . . . ? C10 C11 C12 O1 -4.0(4) . . . . ? C13 C11 C12 O1 175.2(3) . . . . ? C10 C11 C12 N1 176.9(2) . . . . ? C13 C11 C12 N1 -3.9(3) . . . . ? C3 C2 C13 C14 1.2(3) . . . . ? C1 C2 C13 C14 -177.4(2) . . . . ? C3 C2 C13 C11 -179.4(2) . . . . ? C1 C2 C13 C11 2.0(3) . . . . ? C10 C11 C13 C2 -178.0(2) . . . . ? C12 C11 C13 C2 2.9(3) . . . . ? C10 C11 C13 C14 1.4(3) . . . . ? C12 C11 C13 C14 -177.7(2) . . . . ? C9 C8 C14 C5 178.0(2) . . . . ? C7 C8 C14 C5 -2.4(3) . . . . ? C9 C8 C14 C13 -1.5(3) . . . . ? C7 C8 C14 C13 178.1(2) . . . . ? C4 C5 C14 C8 179.0(2) . . . . ? C6 C5 C14 C8 -2.3(3) . . . . ? C4 C5 C14 C13 -1.6(3) . . . . ? C6 C5 C14 C13 177.1(2) . . . . ? C2 C13 C14 C8 179.3(2) . . . . ? C11 C13 C14 C8 -0.1(3) . . . . ? C2 C13 C14 C5 -0.1(3) . . . . ? C11 C13 C14 C5 -179.5(2) . . . . ? C1 N1 C15 C16 -94.4(3) . . . . ? C12 N1 C15 C16 84.6(3) . . . . ? C1 N1 C15 C23 85.2(3) . . . . ? C12 N1 C15 C23 -95.8(3) . . . . ? C23 C15 C16 C20 2.0(4) . . . . ? N1 C15 C16 C20 -178.5(2) . . . . ? C23 C15 C16 C17 -177.8(3) . . . . ? N1 C15 C16 C17 1.8(4) . . . . ? C15 C16 C17 C18 -103.9(3) . . . . ? C20 C16 C17 C18 76.3(4) . . . . ? C15 C16 C17 C19 131.3(3) . . . . ? C20 C16 C17 C19 -48.4(4) . . . . ? C15 C16 C20 C21 -0.6(4) . . . . ? C17 C16 C20 C21 179.2(3) . . . . ? C16 C20 C21 C22 -0.4(4) . . . . ? C20 C21 C22 C23 0.1(5) . . . . ? C21 C22 C23 C15 1.2(4) . . . . ? C21 C22 C23 C24 -178.9(3) . . . . ? C16 C15 C23 C22 -2.3(4) . . . . ? N1 C15 C23 C22 178.1(2) . . . . ? C16 C15 C23 C24 177.8(3) . . . . ? N1 C15 C23 C24 -1.7(4) . . . . ? C22 C23 C24 C26 -90.0(4) . . . . ? C15 C23 C24 C26 89.8(4) . . . . ? C22 C23 C24 C25 36.5(4) . . . . ? C15 C23 C24 C25 -143.6(3) . . . . ? C7 N2 C27 C28 97.9(3) . . . . ? C6 N2 C27 C28 -84.0(3) . . . . ? C7 N2 C27 C35 -81.6(3) . . . . ? C6 N2 C27 C35 96.4(3) . . . . ? C35 C27 C28 C32 -0.2(4) . . . . ? N2 C27 C28 C32 -179.8(2) . . . . ? C35 C27 C28 C29 -178.8(3) . . . . ? N2 C27 C28 C29 1.7(4) . . . . ? C32 C28 C29 C31 48.8(4) . . . . ? C27 C28 C29 C31 -132.7(3) . . . . ? C32 C28 C29 C30 -75.2(4) . . . . ? C27 C28 C29 C30 103.3(4) . . . . ? C27 C28 C32 C33 0.7(4) . . . . ? C29 C28 C32 C33 179.3(3) . . . . ? C28 C32 C33 C34 -0.9(4) . . . . ? C32 C33 C34 C35 0.6(4) . . . . ? C33 C34 C35 C27 -0.1(4) . . . . ? C33 C34 C35 C36 -179.8(3) . . . . ? C28 C27 C35 C34 0.0(4) . . . . ? N2 C27 C35 C34 179.5(2) . . . . ? C28 C27 C35 C36 179.7(3) . . . . ? N2 C27 C35 C36 -0.8(4) . . . . ? C34 C35 C36 C37 -38.8(4) . . . . ? C27 C35 C36 C37 141.5(3) . . . . ? C34 C35 C36 C38 86.6(3) . . . . ? C27 C35 C36 C38 -93.1(3) . . . . ? #===END #===END data_cam184 _database_code_depnum_ccdc_archive 'CCDC 766219' #TrackingRef '- CCDC_deposided_merged_cifs_notepad.cif' _audit_creation_date 04-07-12 _audit_creation_method CRYSTALS_ver_12.20 _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 9.207(1) _cell_angle_alpha 88.83(2) _cell_length_b 12.543(1) _cell_angle_beta 86.38(3) _cell_length_c 17.287(1) _cell_angle_gamma 87.52(3) _cell_volume 1990.2(3) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'Zn ' 0.2839 1.4301 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097 1.3041 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 1 _chemical_formula_sum ' C92 H114 N6 O6 Zn ' _chemical_formula_moiety ' C66 H84 N4 O2 Zn, C26 H30 N2 O4 ' _chemical_compound_source ; ? ; _chemical_formula_weight 1465.28 _cell_measurement_reflns_used 11416 _cell_measurement_theta_min 0 _cell_measurement_theta_max 21 _cell_measurement_temperature 150 _exptl_crystal_description ' needle ' _exptl_crystal_colour ' red ' _exptl_crystal_size_min 0.01 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_max 0.03 _exptl_crystal_density_diffrn 1.223 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 786 _exptl_absorpt_coefficient_mu 0.367 _exptl_absorpt_process_details ; Correction applied by SADABS - note that the transmission factors are not real since they include corrections for beam decay and possibly crystal decay (the two cannot be distinguished). The numbers listed in the CIF are those calculated by CRYSTALS. ; _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 1.00 _exptl_absorpt_correction_T_max 1.00 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART APEX2 CCD' _diffrn_measurement_method 'fine-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5 _diffrn_radiation_wavelength 0.67750 _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution Sir2000 _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_ambient_temperature 150 _diffrn_reflns_number 11416 _reflns_number_total 4720 _diffrn_reflns_av_R_equivalents 0.07 # Number of reflections with Friedels Law is 4720 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 4843 _diffrn_reflns_theta_min 1.125 _diffrn_reflns_theta_max 20.863 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 20.863 _diffrn_measured_fraction_theta_full 0.977 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -9 _reflns_limit_h_max 9 _reflns_limit_k_min -13 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 18 _refine_diff_density_min -0.42 _refine_diff_density_max 0.46 _refine_ls_number_reflns 3440 _refine_ls_number_restraints 0 _refine_ls_number_parameters 475 #_refine_ls_R_factor_ref 0.0348 _refine_ls_wR_factor_ref 0.0396 _refine_ls_goodness_of_fit_ref 1.1401 #_reflns_number_all 4704 _refine_ls_R_factor_all 0.0479 _refine_ls_wR_factor_all 0.0429 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 3440 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_gt 0.0396 _diffrn_special_details ; The small crystal size, large unit cell and high degree of disorder within the crystal gave rise to very weak scattering despite the use of a synchrotron radiation source. As high-angle data had negligable intensity, they were not measured. ; _refine_special_details ; All hexyl chains were disordered on more than two sites and refined with restrains Phenyl rings in molecule were also severely disordered: refinement was carried out with similarity restrains ; _refine_ls_shift/su_max 0.000144 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.66 -0.874 1.18 ; ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Data collection: APEX2, Bruker AXS Inc., Madison, USA, 2004 Data reduction (frames integration): SAINT, Bruker AXS Inc., Madison, USA, 2004 Cell refinement: SAINT, Bruker AXS Inc., Madison, USA, 2004 Absorption correction: SADABS, Bruker AXS Inc., Madison, USA, 2004 Station 9.8: R. J. Cernik, W. Clegg, C. R. A. Catlow, G. Bushnell-Wye, J. V. Flaherty, G. N. Greaves, M. Hamichi, I. Burrows, D. J. Taylor and S. J. Teat, J. Synchotron Radiation 1997, 4, 279-286; 7, 40. Synchrotron chemical crystallography: W. Clegg, J. Chem. Soc., Dalton Trans. 2000, 3223-3232. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Siemens Industrial Automation, Inc (1996). Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of G\"ottingen, Germany. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Zn1 Zn 0.5000 0.5000 0.0000 0.0283 1.0000 Uani S . . . . . O1 O 0.1451(2) -0.00114(15) 0.26418(11) 0.0453 1.0000 Uani . . . . . . O2 O 0.2872(2) 0.70387(18) 0.09535(11) 0.0531 1.0000 Uani . . . . . . O3 O 0.1467(2) 0.39500(16) 0.21512(11) 0.0512 1.0000 Uani . . . . . . N1 N 0.5447(2) 0.41907(16) 0.10138(11) 0.0280 1.0000 Uani . . . . . . N2 N 0.3714(2) 0.37682(16) -0.02264(11) 0.0278 1.0000 Uani . . . . . . N3 N 0.2215(2) 0.54737(18) 0.15345(12) 0.0372 1.0000 Uani . . . . . . C1 C 0.6356(3) 0.4555(2) 0.15381(14) 0.0289 1.0000 Uani . . . . . . C2 C 0.6485(3) 0.3806(2) 0.21786(14) 0.0314 1.0000 Uani . . . . . . C3 C 0.5629(3) 0.2974(2) 0.20443(14) 0.0312 1.0000 Uani . . . . . . C4 C 0.4998(3) 0.3215(2) 0.12943(14) 0.0288 1.0000 Uani . . . . . . C5 C 0.4084(3) 0.2567(2) 0.08983(14) 0.0289 1.0000 Uani . . . . . . C6 C 0.3464(3) 0.2839(2) 0.01912(14) 0.0292 1.0000 Uani . . . . . . C7 C 0.2479(3) 0.2192(2) -0.02291(14) 0.0316 1.0000 Uani . . . . . . C8 C 0.2193(3) 0.27496(19) -0.08914(14) 0.0292 1.0000 Uani . . . . . . C9 C 0.2965(3) 0.3727(2) -0.08861(14) 0.0288 1.0000 Uani . . . . . . C10 C 0.2932(3) 0.4495(2) -0.14717(14) 0.0295 1.0000 Uani . . . . . . C11 C 0.3835(3) 0.1468(2) 0.12271(15) 0.0323 1.0000 Uani . . . . . . C12 C 0.4752(3) 0.0617(2) 0.09645(15) 0.0380 1.0000 Uani . . . . . . C13 C 0.4515(3) -0.0412(2) 0.12455(17) 0.0448 1.0000 Uani . . . . . . C14 C 0.3401(3) -0.0597(2) 0.17997(17) 0.0441 1.0000 Uani . . . . . . C15 C 0.2506(3) 0.0257(2) 0.20767(15) 0.0358 1.0000 Uani . . . . . . C16 C 0.2706(3) 0.12820(19) 0.17843(14) 0.0304 1.0000 Uani . . . . . . C17 C 0.0492(3) 0.0821(2) 0.29483(17) 0.0478 1.0000 Uani . . . . . . C18 C -0.0710(3) 0.1128(2) 0.24429(19) 0.0479 1.0000 Uani . . . . . . C19 C -0.0981(3) 0.0681(2) 0.17946(19) 0.0518 1.0000 Uani . . . . . . C20 C 0.5393(3) 0.2050(2) 0.25997(15) 0.0399 1.0000 Uani . . . . . . C21 C 0.1804(3) 0.1150(2) -0.00009(15) 0.0383 1.0000 Uani . . . . . . C22 C 0.7408(3) 0.3975(2) 0.28530(15) 0.0334 1.0000 Uani . . . . . . C23 C 0.6732(3) 0.4758(2) 0.34606(15) 0.0350 1.0000 Uani . . . . . . C24 C 0.7802(3) 0.5005(2) 0.40667(15) 0.0353 1.0000 Uani . . . . . . C25 C 0.7144(3) 0.5670(2) 0.47364(15) 0.0371 1.0000 Uani . . . . . . C26 C 0.8214(3) 0.5859(2) 0.53494(16) 0.0416 1.0000 Uani . . . . . . C27 C 0.7573(4) 0.6502(2) 0.60306(17) 0.0509 1.0000 Uani . . . . . . C28 C 0.1356(3) 0.2439(2) -0.15657(15) 0.0319 1.0000 Uani . . . . . . C29 C 0.2363(3) 0.1973(2) -0.22287(15) 0.0347 1.0000 Uani . . . . . . C30 C 0.1650(3) 0.1845(2) -0.29850(15) 0.0352 1.0000 Uani . . . . . . C31 C 0.2679(3) 0.1345(2) -0.36181(15) 0.0384 1.0000 Uani . . . . . . C32 C 0.2021(3) 0.1234(2) -0.43938(15) 0.0387 1.0000 Uani . . . . . . C33 C 0.3113(3) 0.0800(2) -0.50223(17) 0.0477 1.0000 Uani . . . . . . C34 C -0.0298(3) 0.3448(2) 0.09408(15) 0.0375 1.0000 Uani . . . . . . C35 C 0.0508(3) 0.4349(2) 0.09299(14) 0.0325 1.0000 Uani . . . . . . C36 C 0.0449(3) 0.5091(2) 0.03070(14) 0.0295 1.0000 Uani . . . . . . C37 C 0.1261(3) 0.6026(2) 0.02839(15) 0.0328 1.0000 Uani . . . . . . C38 C 0.2182(3) 0.6231(2) 0.09331(16) 0.0378 1.0000 Uani . . . . . . C39 C 0.1417(3) 0.4546(2) 0.15873(16) 0.0384 1.0000 Uani . . . . . . C40 C 0.1190(3) 0.6737(2) -0.03328(16) 0.0382 1.0000 Uani . . . . . . C41 C 0.3080(3) 0.5711(2) 0.22004(16) 0.0422 1.0000 Uani . . . . . . C42 C 0.2155(3) 0.6361(2) 0.28038(15) 0.0377 1.0000 Uani . . . . . . C43 C 0.3032(3) 0.6703(2) 0.34681(15) 0.0378 1.0000 Uani . . . . . . C44 C 0.2084(3) 0.7321(2) 0.40756(15) 0.0368 1.0000 Uani . . . . . . C45 C 0.2879(3) 0.7662(2) 0.47646(16) 0.0415 1.0000 Uani . . . . . . C46 C 0.1856(3) 0.8185(2) 0.53874(16) 0.0456 1.0000 Uani . . . . . . H101 H 0.2309 0.4343 -0.1906 0.0356 1.0000 Uiso . . . . . . H121 H 0.5577 0.0748 0.0575 0.0456 1.0000 Uiso . . . . . . H131 H 0.5155 -0.1023 0.1045 0.0539 1.0000 Uiso . . . . . . H141 H 0.3237 -0.1338 0.2001 0.0533 1.0000 Uiso . . . . . . H161 H 0.2042 0.1887 0.1973 0.0367 1.0000 Uiso . . . . . . H171 H 0.0056 0.0576 0.3462 0.0572 1.0000 Uiso . . . . . . H172 H 0.1072 0.1464 0.3019 0.0572 1.0000 Uiso . . . . . . H181 H -0.1379 0.1737 0.2617 0.0568 1.0000 Uiso . . . . . . H191 H -0.1823 0.0952 0.1499 0.0625 1.0000 Uiso . . . . . . H192 H -0.0345 0.0068 0.1594 0.0625 1.0000 Uiso . . . . . . H201 H 0.4729 0.1543 0.2377 0.0484 1.0000 Uiso . . . . . . H202 H 0.6350 0.1673 0.2687 0.0484 1.0000 Uiso . . . . . . H203 H 0.4944 0.2320 0.3104 0.0484 1.0000 Uiso . . . . . . H211 H 0.1188 0.0928 -0.0421 0.0467 1.0000 Uiso . . . . . . H212 H 0.2591 0.0590 0.0078 0.0467 1.0000 Uiso . . . . . . H213 H 0.1185 0.1240 0.0492 0.0467 1.0000 Uiso . . . . . . H221 H 0.8357 0.4255 0.2644 0.0403 1.0000 Uiso . . . . . . H222 H 0.7585 0.3269 0.3117 0.0403 1.0000 Uiso . . . . . . H231 H 0.6432 0.5439 0.3192 0.0424 1.0000 Uiso . . . . . . H232 H 0.5856 0.4437 0.3728 0.0424 1.0000 Uiso . . . . . . H241 H 0.8618 0.5402 0.3804 0.0428 1.0000 Uiso . . . . . . H242 H 0.8194 0.4313 0.4283 0.0428 1.0000 Uiso . . . . . . H251 H 0.6796 0.6377 0.4526 0.0450 1.0000 Uiso . . . . . . H252 H 0.6298 0.5290 0.4987 0.0450 1.0000 Uiso . . . . . . H261 H 0.9048 0.6250 0.5099 0.0506 1.0000 Uiso . . . . . . H262 H 0.8577 0.5150 0.5550 0.0506 1.0000 Uiso . . . . . . H271 H 0.8339 0.6592 0.6407 0.0617 1.0000 Uiso . . . . . . H272 H 0.7215 0.7219 0.5842 0.0617 1.0000 Uiso . . . . . . H273 H 0.6743 0.6118 0.6293 0.0617 1.0000 Uiso . . . . . . H281 H 0.0815 0.3086 -0.1764 0.0387 1.0000 Uiso . . . . . . H282 H 0.0647 0.1892 -0.1384 0.0387 1.0000 Uiso . . . . . . H291 H 0.3192 0.2457 -0.2328 0.0422 1.0000 Uiso . . . . . . H292 H 0.2744 0.1254 -0.2057 0.0422 1.0000 Uiso . . . . . . H301 H 0.1300 0.2565 -0.3172 0.0425 1.0000 Uiso . . . . . . H302 H 0.0801 0.1378 -0.2888 0.0425 1.0000 Uiso . . . . . . H311 H 0.3543 0.1801 -0.3699 0.0461 1.0000 Uiso . . . . . . H312 H 0.3003 0.0617 -0.3434 0.0461 1.0000 Uiso . . . . . . H321 H 0.1637 0.1952 -0.4566 0.0466 1.0000 Uiso . . . . . . H322 H 0.1201 0.0736 -0.4325 0.0466 1.0000 Uiso . . . . . . H331 H 0.2620 0.0744 -0.5518 0.0573 1.0000 Uiso . . . . . . H332 H 0.3936 0.1294 -0.5101 0.0573 1.0000 Uiso . . . . . . H333 H 0.3500 0.0078 -0.4860 0.0573 1.0000 Uiso . . . . . . H341 H -0.0247 0.2925 0.1383 0.0445 1.0000 Uiso . . . . . . H401 H 0.1778 0.7389 -0.0347 0.0455 1.0000 Uiso . . . . . . H411 H 0.3937 0.6128 0.2011 0.0510 1.0000 Uiso . . . . . . H412 H 0.3427 0.5025 0.2445 0.0510 1.0000 Uiso . . . . . . H421 H 0.1738 0.7014 0.2544 0.0453 1.0000 Uiso . . . . . . H422 H 0.1345 0.5916 0.3021 0.0453 1.0000 Uiso . . . . . . H431 H 0.3823 0.7167 0.3255 0.0455 1.0000 Uiso . . . . . . H432 H 0.3473 0.6052 0.3720 0.0455 1.0000 Uiso . . . . . . H441 H 0.1664 0.7977 0.3820 0.0442 1.0000 Uiso . . . . . . H442 H 0.1278 0.6859 0.4271 0.0442 1.0000 Uiso . . . . . . H451 H 0.3622 0.8184 0.4581 0.0501 1.0000 Uiso . . . . . . H452 H 0.3377 0.7019 0.4996 0.0501 1.0000 Uiso . . . . . . H461 H 0.2428 0.8395 0.5828 0.0549 1.0000 Uiso . . . . . . H462 H 0.1356 0.8833 0.5164 0.0549 1.0000 Uiso . . . . . . H463 H 0.1111 0.7668 0.5579 0.0549 1.0000 Uiso . . . . . . 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 0.0226(2) 0.0379(3) 0.0249(3) -0.00824(18) -0.00320(18) -0.00206(18) O1 0.0484(12) 0.0404(11) 0.0467(12) 0.0031(9) 0.0022(10) -0.0056(9) O2 0.0469(12) 0.0669(15) 0.0471(12) -0.0112(11) -0.0041(10) -0.0136(11) O3 0.0679(14) 0.0533(13) 0.0330(11) -0.0041(10) -0.0159(10) 0.0098(10) N1 0.0200(11) 0.0361(13) 0.0280(11) -0.0097(9) -0.0007(9) -0.0007(9) N2 0.0237(11) 0.0345(13) 0.0256(11) -0.0067(10) -0.0027(9) -0.0003(9) N3 0.0363(13) 0.0470(14) 0.0282(12) -0.0124(11) -0.0071(10) 0.0116(11) C1 0.0237(13) 0.0371(15) 0.0264(13) -0.0105(12) -0.0043(11) 0.0033(11) C2 0.0298(14) 0.0389(15) 0.0260(14) -0.0096(12) -0.0045(11) 0.0034(12) C3 0.0257(13) 0.0391(15) 0.0287(14) -0.0098(12) -0.0004(11) 0.0018(12) C4 0.0233(13) 0.0373(16) 0.0255(13) -0.0083(11) 0.0014(11) 0.0020(11) C5 0.0244(13) 0.0353(15) 0.0266(14) -0.0095(12) 0.0036(11) 0.0019(11) C6 0.0219(13) 0.0376(16) 0.0278(14) -0.0102(12) 0.0016(11) 0.0019(11) C7 0.0252(14) 0.0376(15) 0.0318(15) -0.0113(12) 0.0005(11) -0.0001(11) C8 0.0238(13) 0.0353(15) 0.0287(14) -0.0113(12) -0.0015(11) 0.0011(11) C9 0.0195(12) 0.0394(15) 0.0278(14) -0.0133(12) -0.0033(11) 0.0029(11) C10 0.0228(13) 0.0403(16) 0.0259(14) -0.0099(12) -0.0049(11) 0.0028(11) C11 0.0309(14) 0.0363(16) 0.0306(14) -0.0086(12) -0.0084(12) 0.0011(12) C12 0.0329(15) 0.0470(18) 0.0340(15) -0.0086(13) -0.0045(12) 0.0049(13) C13 0.0490(18) 0.0432(18) 0.0426(17) -0.0105(14) -0.0119(15) 0.0113(14) C14 0.0526(18) 0.0356(16) 0.0449(17) -0.0034(13) -0.0118(15) 0.0006(14) C15 0.0362(15) 0.0391(17) 0.0327(15) -0.0035(12) -0.0033(13) -0.0046(13) C16 0.0296(14) 0.0314(15) 0.0308(14) -0.0069(11) -0.0035(12) -0.0009(11) C17 0.0558(19) 0.0470(18) 0.0402(17) -0.0077(14) 0.0119(15) -0.0148(15) C18 0.0429(18) 0.0382(17) 0.061(2) -0.0054(15) 0.0127(16) -0.0027(14) C19 0.0476(18) 0.0468(18) 0.062(2) 0.0025(16) -0.0040(16) -0.0116(14) C20 0.0417(16) 0.0478(17) 0.0315(15) -0.0017(13) -0.0095(12) -0.0053(13) C21 0.0366(15) 0.0419(16) 0.0381(15) -0.0072(12) -0.0087(13) -0.0084(13) C22 0.0333(14) 0.0371(15) 0.0303(14) -0.0057(12) -0.0065(12) 0.0020(12) C23 0.0350(15) 0.0417(16) 0.0294(14) -0.0078(12) -0.0070(12) -0.0024(12) C24 0.0372(15) 0.0380(16) 0.0317(15) -0.0070(12) -0.0066(12) -0.0023(12) C25 0.0408(16) 0.0399(16) 0.0318(15) -0.0068(12) -0.0066(12) -0.0041(12) C26 0.0541(18) 0.0380(16) 0.0345(15) -0.0034(12) -0.0097(13) -0.0102(13) C27 0.074(2) 0.0464(18) 0.0337(16) -0.0074(13) -0.0064(15) -0.0101(16) C28 0.0289(14) 0.0354(15) 0.0324(14) -0.0077(12) -0.0056(11) -0.0046(11) C29 0.0335(14) 0.0356(15) 0.0364(15) -0.0091(12) -0.0082(12) -0.0032(12) C30 0.0357(15) 0.0350(15) 0.0356(15) -0.0039(12) -0.0067(12) -0.0029(12) C31 0.0405(16) 0.0377(16) 0.0371(16) -0.0089(12) -0.0021(13) 0.0006(12) C32 0.0444(16) 0.0358(16) 0.0363(15) -0.0074(12) -0.0038(13) -0.0030(12) C33 0.0533(18) 0.0501(18) 0.0398(16) -0.0108(14) -0.0011(14) -0.0024(14) C34 0.0420(16) 0.0400(17) 0.0293(15) -0.0046(12) 0.0023(13) 0.0091(13) C35 0.0324(14) 0.0367(16) 0.0276(15) -0.0114(12) 0.0002(12) 0.0121(12) C36 0.0261(13) 0.0349(15) 0.0263(13) -0.0114(12) 0.0028(10) 0.0115(11) C37 0.0299(14) 0.0384(16) 0.0293(15) -0.0116(12) 0.0036(12) 0.0066(12) C38 0.0300(15) 0.0498(18) 0.0332(16) -0.0152(14) 0.0017(12) 0.0034(14) C39 0.0417(16) 0.0417(17) 0.0309(16) -0.0101(14) -0.0047(12) 0.0151(14) C40 0.0428(16) 0.0354(16) 0.0354(16) -0.0096(13) 0.0039(13) 0.0026(13) C41 0.0384(16) 0.0541(18) 0.0349(16) -0.0166(13) -0.0099(13) 0.0093(13) C42 0.0336(15) 0.0461(17) 0.0334(15) -0.0123(12) -0.0027(12) 0.0042(12) C43 0.0390(16) 0.0419(16) 0.0329(15) -0.0100(12) -0.0043(12) 0.0005(12) C44 0.0370(15) 0.0394(16) 0.0340(15) -0.0078(12) -0.0017(12) -0.0001(12) C45 0.0470(17) 0.0419(17) 0.0364(16) -0.0104(13) -0.0056(13) -0.0025(13) C46 0.0602(19) 0.0430(17) 0.0339(16) -0.0110(13) -0.0031(14) -0.0021(14) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zn1 . N1 2_665 2.062(2) yes Zn1 . N2 2_665 2.046(2) yes Zn1 . N1 . 2.062(2) yes Zn1 . N2 . 2.046(2) yes O1 . C15 . 1.381(3) yes O1 . C17 . 1.426(4) yes O2 . C38 . 1.221(3) yes O3 . C39 . 1.218(3) yes N1 . C1 . 1.369(3) yes N1 . C4 . 1.378(3) yes N2 . C6 . 1.379(3) yes N2 . C9 . 1.372(3) yes N3 . C38 . 1.395(4) yes N3 . C39 . 1.401(4) yes N3 . C41 . 1.482(3) yes C1 . C10 2_665 1.385(4) yes C1 . C2 . 1.444(4) yes C2 . C3 . 1.367(4) yes C2 . C22 . 1.509(3) yes C3 . C4 . 1.474(4) yes C3 . C20 . 1.504(4) yes C4 . C5 . 1.412(3) yes C5 . C6 . 1.411(4) yes C5 . C11 . 1.502(4) yes C6 . C7 . 1.475(3) yes C7 . C8 . 1.363(4) yes C7 . C21 . 1.507(4) yes C8 . C9 . 1.445(4) yes C8 . C28 . 1.504(3) yes C9 . C10 . 1.384(4) yes C10 . H101 . 1.000 no C11 . C12 . 1.396(4) yes C11 . C16 . 1.395(4) yes C12 . C13 . 1.391(4) yes C12 . H121 . 1.000 no C13 . C14 . 1.382(4) yes C13 . H131 . 1.000 no C14 . C15 . 1.396(4) yes C14 . H141 . 1.000 no C15 . C16 . 1.387(4) yes C16 . H161 . 1.000 no C17 . C18 . 1.486(5) yes C17 . H171 . 1.000 no C17 . H172 . 1.000 no C18 . C19 . 1.306(4) yes C18 . H181 . 1.000 no C19 . H191 . 1.000 no C19 . H192 . 1.000 no C20 . H201 . 1.000 no C20 . H202 . 1.000 no C20 . H203 . 1.000 no C21 . H211 . 1.000 no C21 . H212 . 1.000 no C21 . H213 . 1.000 no C22 . C23 . 1.537(4) yes C22 . H221 . 1.000 no C22 . H222 . 1.000 no C23 . C24 . 1.528(4) yes C23 . H231 . 1.000 no C23 . H232 . 1.000 no C24 . C25 . 1.520(4) yes C24 . H241 . 1.000 no C24 . H242 . 1.000 no C25 . C26 . 1.521(4) yes C25 . H251 . 1.000 no C25 . H252 . 1.000 no C26 . C27 . 1.515(4) yes C26 . H261 . 1.000 no C26 . H262 . 1.000 no C27 . H271 . 1.000 no C27 . H272 . 1.000 no C27 . H273 . 1.000 no C28 . C29 . 1.536(4) yes C28 . H281 . 1.000 no C28 . H282 . 1.000 no C29 . C30 . 1.514(4) yes C29 . H291 . 1.000 no C29 . H292 . 1.000 no C30 . C31 . 1.528(4) yes C30 . H301 . 1.000 no C30 . H302 . 1.000 no C31 . C32 . 1.518(4) yes C31 . H311 . 1.000 no C31 . H312 . 1.000 no C32 . C33 . 1.526(4) yes C32 . H321 . 1.000 no C32 . H322 . 1.000 no C33 . H331 . 1.000 no C33 . H332 . 1.000 no C33 . H333 . 1.000 no C34 . C40 2_565 1.403(4) yes C34 . C35 . 1.377(4) yes C34 . H341 . 1.000 no C35 . C36 . 1.411(4) yes C35 . C39 . 1.484(4) yes C36 . C36 2_565 1.414(5) yes C36 . C37 . 1.416(4) yes C37 . C38 . 1.482(4) yes C37 . C40 . 1.379(4) yes C40 . H401 . 1.000 no C41 . C42 . 1.530(4) yes C41 . H411 . 1.000 no C41 . H412 . 1.000 no C42 . C43 . 1.524(4) yes C42 . H421 . 1.000 no C42 . H422 . 1.000 no C43 . C44 . 1.524(4) yes C43 . H431 . 1.000 no C43 . H432 . 1.000 no C44 . C45 . 1.515(4) yes C44 . H441 . 1.000 no C44 . H442 . 1.000 no C45 . C46 . 1.524(4) yes C45 . H451 . 1.000 no C45 . H452 . 1.000 no C46 . H461 . 1.000 no C46 . H462 . 1.000 no C46 . H463 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 2_665 Zn1 . N2 2_665 86.86(8) yes N1 2_665 Zn1 . N1 . 179.994 yes N2 2_665 Zn1 . N1 . 93.14(8) yes N1 2_665 Zn1 . N2 . 93.14(8) yes N2 2_665 Zn1 . N2 . 179.994 yes N1 . Zn1 . N2 . 86.86(8) yes C15 . O1 . C17 . 117.9(2) yes Zn1 . N1 . C1 . 123.40(17) yes Zn1 . N1 . C4 . 130.13(15) yes C1 . N1 . C4 . 106.4(2) yes Zn1 . N2 . C6 . 129.78(15) yes Zn1 . N2 . C9 . 123.00(17) yes C6 . N2 . C9 . 107.2(2) yes C38 . N3 . C39 . 125.4(2) yes C38 . N3 . C41 . 117.2(2) yes C39 . N3 . C41 . 117.3(2) yes C10 2_665 C1 . N1 . 125.3(2) yes C10 2_665 C1 . C2 . 123.9(2) yes N1 . C1 . C2 . 110.8(2) yes C1 . C2 . C3 . 107.1(2) yes C1 . C2 . C22 . 123.7(2) yes C3 . C2 . C22 . 129.2(2) yes C2 . C3 . C4 . 106.1(2) yes C2 . C3 . C20 . 123.9(2) yes C4 . C3 . C20 . 129.9(2) yes C3 . C4 . N1 . 109.6(2) yes C3 . C4 . C5 . 127.0(2) yes N1 . C4 . C5 . 123.4(2) yes C4 . C5 . C6 . 125.4(2) yes C4 . C5 . C11 . 117.3(2) yes C6 . C5 . C11 . 117.2(2) yes C5 . C6 . N2 . 124.3(2) yes C5 . C6 . C7 . 126.8(2) yes N2 . C6 . C7 . 108.9(2) yes C6 . C7 . C8 . 106.5(2) yes C6 . C7 . C21 . 130.0(2) yes C8 . C7 . C21 . 123.4(2) yes C7 . C8 . C9 . 107.3(2) yes C7 . C8 . C28 . 129.9(2) yes C9 . C8 . C28 . 122.6(2) yes C8 . C9 . N2 . 110.1(2) yes C8 . C9 . C10 . 123.6(2) yes N2 . C9 . C10 . 126.3(2) yes C1 2_665 C10 . C9 . 128.8(2) yes C1 2_665 C10 . H101 . 115.580 no C9 . C10 . H101 . 115.581 no C5 . C11 . C12 . 119.0(2) yes C5 . C11 . C16 . 121.3(2) yes C12 . C11 . C16 . 119.7(3) yes C11 . C12 . C13 . 119.9(3) yes C11 . C12 . H121 . 120.041 no C13 . C12 . H121 . 120.044 no C12 . C13 . C14 . 120.5(3) yes C12 . C13 . H131 . 119.764 no C14 . C13 . H131 . 119.764 no C13 . C14 . C15 . 119.6(3) yes C13 . C14 . H141 . 120.182 no C15 . C14 . H141 . 120.181 no C14 . C15 . O1 . 114.9(2) yes C14 . C15 . C16 . 120.4(2) yes O1 . C15 . C16 . 124.7(2) yes C11 . C16 . C15 . 119.9(2) yes C11 . C16 . H161 . 120.048 no C15 . C16 . H161 . 120.046 no O1 . C17 . C18 . 113.6(2) yes O1 . C17 . H171 . 108.433 no C18 . C17 . H171 . 108.431 no O1 . C17 . H172 . 108.431 no C18 . C17 . H172 . 108.430 no H171 . C17 . H172 . 109.469 no C17 . C18 . C19 . 126.6(3) yes C17 . C18 . H181 . 116.713 no C19 . C18 . H181 . 116.711 no C18 . C19 . H191 . 120.000 no C18 . C19 . H192 . 120.001 no H191 . C19 . H192 . 120.000 no C3 . C20 . H201 . 109.464 no C3 . C20 . H202 . 109.464 no H201 . C20 . H202 . 109.474 no C3 . C20 . H203 . 109.468 no H201 . C20 . H203 . 109.477 no H202 . C20 . H203 . 109.479 no C7 . C21 . H211 . 109.467 no C7 . C21 . H212 . 109.467 no H211 . C21 . H212 . 109.475 no C7 . C21 . H213 . 109.467 no H211 . C21 . H213 . 109.476 no H212 . C21 . H213 . 109.475 no C2 . C22 . C23 . 114.8(2) yes C2 . C22 . H221 . 108.123 no C23 . C22 . H221 . 108.123 no C2 . C22 . H222 . 108.121 no C23 . C22 . H222 . 108.123 no H221 . C22 . H222 . 109.468 no C22 . C23 . C24 . 111.9(2) yes C22 . C23 . H231 . 108.856 no C24 . C23 . H231 . 108.856 no C22 . C23 . H232 . 108.855 no C24 . C23 . H232 . 108.854 no H231 . C23 . H232 . 109.464 no C23 . C24 . C25 . 114.4(2) yes C23 . C24 . H241 . 108.235 no C25 . C24 . H241 . 108.237 no C23 . C24 . H242 . 108.237 no C25 . C24 . H242 . 108.238 no H241 . C24 . H242 . 109.467 no C24 . C25 . C26 . 113.2(2) yes C24 . C25 . H251 . 108.527 no C26 . C25 . H251 . 108.525 no C24 . C25 . H252 . 108.526 no C26 . C25 . H252 . 108.525 no H251 . C25 . H252 . 109.466 no C25 . C26 . C27 . 114.2(3) yes C25 . C26 . H261 . 108.284 no C27 . C26 . H261 . 108.285 no C25 . C26 . H262 . 108.283 no C27 . C26 . H262 . 108.285 no H261 . C26 . H262 . 109.464 no C26 . C27 . H271 . 109.468 no C26 . C27 . H272 . 109.468 no H271 . C27 . H272 . 109.477 no C26 . C27 . H273 . 109.466 no H271 . C27 . H273 . 109.473 no H272 . C27 . H273 . 109.475 no C8 . C28 . C29 . 112.0(2) yes C8 . C28 . H281 . 108.842 no C29 . C28 . H281 . 108.840 no C8 . C28 . H282 . 108.840 no C29 . C28 . H282 . 108.842 no H281 . C28 . H282 . 109.466 no C28 . C29 . C30 . 115.1(2) yes C28 . C29 . H291 . 108.054 no C30 . C29 . H291 . 108.053 no C28 . C29 . H292 . 108.051 no C30 . C29 . H292 . 108.050 no H291 . C29 . H292 . 109.467 no C29 . C30 . C31 . 113.2(2) yes C29 . C30 . H301 . 108.542 no C31 . C30 . H301 . 108.545 no C29 . C30 . H302 . 108.544 no C31 . C30 . H302 . 108.546 no H301 . C30 . H302 . 109.466 no C30 . C31 . C32 . 114.8(2) yes C30 . C31 . H311 . 108.121 no C32 . C31 . H311 . 108.119 no C30 . C31 . H312 . 108.120 no C32 . C31 . H312 . 108.118 no H311 . C31 . H312 . 109.467 no C31 . C32 . C33 . 113.0(2) yes C31 . C32 . H321 . 108.577 no C33 . C32 . H321 . 108.580 no C31 . C32 . H322 . 108.577 no C33 . C32 . H322 . 108.579 no H321 . C32 . H322 . 109.467 no C32 . C33 . H331 . 109.469 no C32 . C33 . H332 . 109.468 no H331 . C33 . H332 . 109.475 no C32 . C33 . H333 . 109.468 no H331 . C33 . H333 . 109.474 no H332 . C33 . H333 . 109.473 no C40 2_565 C34 . C35 . 120.2(2) yes C40 2_565 C34 . H341 . 119.903 no C35 . C34 . H341 . 119.903 no C34 . C35 . C36 . 120.4(2) yes C34 . C35 . C39 . 119.5(2) yes C36 . C35 . C39 . 120.1(3) yes C36 2_565 C36 . C35 . 119.7(3) yes C36 2_565 C36 . C37 . 118.8(3) yes C35 . C36 . C37 . 121.5(2) yes C36 . C37 . C38 . 119.1(3) yes C36 . C37 . C40 . 120.4(2) yes C38 . C37 . C40 . 120.5(3) yes C37 . C38 . N3 . 117.5(3) yes C37 . C38 . O2 . 121.8(3) yes N3 . C38 . O2 . 120.7(3) yes C35 . C39 . N3 . 116.4(3) yes C35 . C39 . O3 . 122.7(3) yes N3 . C39 . O3 . 120.9(3) yes C34 2_565 C40 . C37 . 120.5(3) yes C34 2_565 C40 . H401 . 119.759 no C37 . C40 . H401 . 119.756 no N3 . C41 . C42 . 110.6(2) yes N3 . C41 . H411 . 109.180 no C42 . C41 . H411 . 109.181 no N3 . C41 . H412 . 109.177 no C42 . C41 . H412 . 109.178 no H411 . C41 . H412 . 109.467 no C41 . C42 . C43 . 112.5(2) yes C41 . C42 . H421 . 108.704 no C43 . C42 . H421 . 108.705 no C41 . C42 . H422 . 108.706 no C43 . C42 . H422 . 108.703 no H421 . C42 . H422 . 109.466 no C42 . C43 . C44 . 111.8(2) yes C42 . C43 . H431 . 108.886 no C44 . C43 . H431 . 108.886 no C42 . C43 . H432 . 108.889 no C44 . C43 . H432 . 108.888 no H431 . C43 . H432 . 109.466 no C43 . C44 . C45 . 114.7(2) yes C43 . C44 . H441 . 108.160 no C45 . C44 . H441 . 108.161 no C43 . C44 . H442 . 108.160 no C45 . C44 . H442 . 108.160 no H441 . C44 . H442 . 109.466 no C44 . C45 . C46 . 112.4(2) yes C44 . C45 . H451 . 108.726 no C46 . C45 . H451 . 108.728 no C44 . C45 . H452 . 108.729 no C46 . C45 . H452 . 108.729 no H451 . C45 . H452 . 109.466 no C45 . C46 . H461 . 109.468 no C45 . C46 . H462 . 109.467 no H461 . C46 . H462 . 109.472 no C45 . C46 . H463 . 109.468 no H461 . C46 . H463 . 109.478 no H462 . C46 . H463 . 109.475 no #===END data_cam213 _database_code_depnum_ccdc_archive 'CCDC 766220' #TrackingRef '- CCDC_deposided_merged_cifs_notepad.cif' _audit_creation_date 10-01-07 _audit_creation_method CRYSTALS_ver_12.80 _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 15.952(6) _cell_length_b 9.578(4) _cell_length_c 27.437(10) _cell_angle_alpha 90 _cell_angle_beta 93.065(6) _cell_angle_gamma 90 _cell_volume 4186(3) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y+1/2,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Zn 0.2839 1.4301 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097 1.3041 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 _chemical_formula_sum 'C87 H106 Cl2 N8 O9 Zn' _chemical_formula_moiety 'C86 H104 N8 O8 Zn, C H2 Cl2, 1(O)' _chemical_compound_source ? _chemical_formula_weight 1544.73 _cell_measurement_reflns_used 13163 _cell_measurement_theta_min 1 _cell_measurement_theta_max 25 _cell_measurement_temperature 150(2) _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_min 0.01 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_max 0.03 _exptl_crystal_density_diffrn 1.225 _exptl_crystal_density_meas ? _exptl_crystal_F_000 1640 _exptl_absorpt_coefficient_mu 0.352 _exptl_absorpt_process_details ; Correction applied by SADABS - note that the transmission factors are not real since they include corrections for beam decay and possibly crystal decay (the two cannot be distinguished). The numbers listed in the CIF are those calculated by CRYSTALS. ; _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 1.00 _exptl_absorpt_correction_T_max 1.00 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART APEX2 CCD' _diffrn_measurement_method 'fine-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5 _diffrn_radiation_wavelength 0.67750 _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution Sir2000 _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_ambient_temperature 150 _diffrn_reflns_number 13163 _reflns_number_total 4843 _diffrn_reflns_av_R_equivalents 0.044 _diffrn_reflns_theta_min 0.713 _diffrn_reflns_theta_max 19.968 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 19.968 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _reflns_limit_h_min -15 _reflns_limit_h_max 15 _reflns_limit_k_min -9 _reflns_limit_k_max 9 _reflns_limit_l_min 0 _reflns_limit_l_max 27 _diffrn_special_details ; The small crystal size, large unit cell and high degree of disorder within the crystal gave rise to very weak scattering despite the use of a synchrotron radiation source. As high-angle data had negligable intensity, they were not measured. ; _refine_special_details ; Crystal was extremly weakly diffracting: Due to the low number of observed data, anisotropic atomic displacement parameters could not be included in the model and an attempt do refine the Flack parameter led to a meaningless value There is more than one disordered water molecule in the asymmetric unit. The partial occupancies of these solvent-occupied sites located in a Fourier map and tentativelly assigned to H2O were refined. Hydrogen atoms attached to the corresponding oxygen atoms could not be identified by examination of a difference Fourier map. Hydrogen atoms on carbon atoms were placed geometrically after each cycle. All hexyl chains were disordered and refined with restrains Phenyl rings in molecule are severely disordered: refinement was carried out with similarity restrains ; _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.84 _refine_diff_density_max 1.92 _refine_ls_number_reflns 3771 _refine_ls_number_restraints 125 _refine_ls_number_parameters 452 #_refine_ls_R_factor_ref 0.1264 _refine_ls_wR_factor_ref 0.1390 _refine_ls_goodness_of_fit_ref 1.1586 #_reflns_number_all 8142 _refine_ls_R_factor_all 0.2164 _refine_ls_wR_factor_all 0.2266 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 3771 _refine_ls_R_factor_gt 0.1264 _refine_ls_wR_factor_gt 0.1390 _refine_ls_shift/su_max 0.012790 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration unk _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 5.66 -1.63 3.87 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Data collection: APEX2, Bruker AXS Inc., Madison, USA, 2004 Data reduction (frames integration): SAINT, Bruker AXS Inc., Madison, USA, 2004 Cell refinement: SAINT, Bruker AXS Inc., Madison, USA, 2004 Absorption correction: SADABS, Bruker AXS Inc., Madison, USA, 2004 Station 9.8: R. J. Cernik, W. Clegg, C. R. A. Catlow, G. Bushnell-Wye, J. V. Flaherty, G. N. Greaves, M. Hamichi, I. Burrows, D. J. Taylor and S. J. Teat, J. Synchotron Radiation 1997, 4, 279-286; 7, 40. Synchrotron chemical crystallography: W. Clegg, J. Chem. Soc., Dalton Trans. 2000, 3223-3232. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Siemens Industrial Automation, Inc (1996). Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of G\"ottingen, Germany. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Zn1 Zn 0.6884(3) 0.3308(6) 0.74543(16) 0.0031(11) 0.5000 Uiso D U . 1 1 . Zn2 Zn 0.7159(3) 0.3039(6) 0.73399(17) 0.0037(11) 0.5000 Uiso D U . 1 2 . N1 N 0.7166(10) 0.3810(17) 0.6692(5) 0.0061(16) 1.0000 Uiso D U . . . . N2 N 0.8051(10) 0.4384(16) 0.7653(6) 0.0053(15) 1.0000 Uiso D U . . . . N3 N 0.6966(10) 0.2327(17) 0.8095(5) 0.0058(16) 1.0000 Uiso D U . . . . N4 N 0.6144(9) 0.1732(17) 0.7142(6) 0.0049(16) 1.0000 Uiso D U . . . . N5 N 0.6212(18) 0.570(3) 0.8339(11) 0.086(5) 1.0000 Uiso D U . . . . N6 N 0.8547(14) 1.096(2) 0.7118(9) 0.050(4) 1.0000 Uiso D U . . . . N7 N 1.0598(15) 0.361(2) 1.0244(8) 0.049(7) 1.0000 Uiso . . . . . . N8 N 0.4808(14) 0.143(2) 0.4221(8) 0.044(6) 1.0000 Uiso . . . . . . O1 O 0.5791(11) 0.4854(18) 0.7575(7) 0.044(5) 1.0000 Uiso . . . . . . O2 O 0.7842(10) 1.0316(18) 0.6405(6) 0.042(5) 1.0000 Uiso . . . . . . O3 O 0.9339(10) 1.1370(18) 0.7830(6) 0.038(5) 1.0000 Uiso . . . . . . O4 O 0.6873(11) 0.6370(19) 0.9075(7) 0.052(5) 1.0000 Uiso . . . . . . O5 O 1.0355(12) 0.439(2) 1.0576(7) 0.062(6) 1.0000 Uiso . . . . . . O6 O 1.1197(13) 0.291(2) 1.0170(6) 0.058(6) 1.0000 Uiso . . . . . . O7 O 0.4133(12) 0.2186(19) 0.4132(6) 0.049(5) 1.0000 Uiso . . . . . . O8 O 0.5247(12) 0.081(2) 0.3979(7) 0.049(5) 1.0000 Uiso . . . . . . C1 C 0.7597(17) 0.480(3) 0.6579(10) 0.037(2) 1.0000 Uiso . U . . . . C2 C 0.7593(17) 0.531(3) 0.6041(10) 0.040(2) 1.0000 Uiso . U . . . . C3 C 0.6962(16) 0.433(3) 0.5847(9) 0.038(2) 1.0000 Uiso . U . . . . C4 C 0.6701(16) 0.344(3) 0.6253(9) 0.038(2) 1.0000 Uiso . U . . . . C5 C 0.6078(17) 0.237(3) 0.6257(10) 0.039(3) 1.0000 Uiso . U . . . . C6 C 0.5834(17) 0.159(3) 0.6639(9) 0.041(3) 1.0000 Uiso . U . . . . C7 C 0.5192(17) 0.049(3) 0.6639(10) 0.043(2) 1.0000 Uiso . U . . . . C8 C 0.5069(17) 0.004(3) 0.7087(11) 0.045(2) 1.0000 Uiso . U . . . . C9 C 0.5681(18) 0.085(3) 0.7399(10) 0.044(2) 1.0000 Uiso . U . . . . C10 C 0.5777(17) 0.074(3) 0.7905(10) 0.043(2) 1.0000 Uiso . U . . . . C11 C 0.6486(18) 0.128(3) 0.8227(10) 0.044(2) 1.0000 Uiso . U . . . . C12 C 0.6542(17) 0.098(3) 0.8749(10) 0.044(2) 1.0000 Uiso . U . . . . C13 C 0.7253(17) 0.179(3) 0.8923(10) 0.041(2) 1.0000 Uiso . U . . . . C14 C 0.7519(17) 0.263(3) 0.8529(10) 0.039(2) 1.0000 Uiso . U . . . . C15 C 0.8209(16) 0.356(3) 0.8515(9) 0.037(3) 1.0000 Uiso . U . . . . C16 C 0.8433(16) 0.443(3) 0.8144(9) 0.037(2) 1.0000 Uiso . U . . . . C17 C 0.9108(16) 0.553(3) 0.8135(10) 0.036(2) 1.0000 Uiso . U . . . . C18 C 0.9113(16) 0.602(3) 0.7683(10) 0.036(2) 1.0000 Uiso . U . . . . C19 C 0.8410(16) 0.535(3) 0.7388(10) 0.035(2) 1.0000 Uiso . U . . . . C20 C 0.8262(16) 0.568(3) 0.6861(10) 0.036(2) 1.0000 Uiso . U . . . . C21 C 0.6203(16) 0.585(3) 0.7808(9) 0.029(3) 1.0000 Uiso . U . . . . C22 C 0.6608(15) 0.692(3) 0.7583(9) 0.029(2) 1.0000 Uiso . U . . . . C23 C 0.7181(15) 0.779(2) 0.7847(9) 0.027(2) 1.0000 Uiso . U . . . . C24 C 0.7348(15) 0.755(2) 0.8373(8) 0.026(2) 1.0000 Uiso . U . . . . C25 C 0.6888(15) 0.651(3) 0.8604(9) 0.026(3) 1.0000 Uiso . U . . . . C26 C 0.7997(13) 0.838(3) 0.8619(8) 0.026(2) 1.0000 Uiso . U . . . . C27 C 0.8438(15) 0.937(2) 0.8392(8) 0.025(2) 1.0000 Uiso . U . . . . C28 C 0.8291(15) 0.966(2) 0.7880(8) 0.024(2) 1.0000 Uiso . U . . . . C29 C 0.7595(15) 0.878(3) 0.7610(9) 0.024(2) 1.0000 Uiso . U . . . . C30 C 0.7489(15) 0.910(3) 0.7092(8) 0.026(2) 1.0000 Uiso . U . . . . C31 C 0.6813(14) 0.828(3) 0.6864(8) 0.027(2) 1.0000 Uiso . U . . . . C32 C 0.6414(15) 0.725(3) 0.7090(9) 0.028(2) 1.0000 Uiso . U . . . . C33 C 0.8775(15) 1.061(3) 0.7638(9) 0.023(3) 1.0000 Uiso . U . . . . C34 C 0.7880(16) 1.009(3) 0.6898(9) 0.026(3) 1.0000 Uiso . U . . . . C35 C 0.4665(16) -0.020(3) 0.6205(10) 0.043(3) 1.0000 Uiso . U . . . . C36 C 0.6737(16) 0.435(3) 0.5315(9) 0.038(3) 1.0000 Uiso . U . . . . C37 C 0.9753(16) 0.604(3) 0.8544(9) 0.037(3) 1.0000 Uiso . U . . . . C38 C 0.7586(17) 0.161(3) 0.9453(9) 0.041(3) 1.0000 Uiso . U . . . . C39 C 0.8808(15) 0.358(2) 0.8975(8) 0.027(7) 1.0000 Uiso . . . . . . C40 C 0.8598(15) 0.449(3) 0.9373(9) 0.033(7) 1.0000 Uiso . . . . . . C41 C 0.922(2) 0.442(4) 0.9784(12) 0.068(10) 1.0000 Uiso . . . . . . C42 C 0.9921(14) 0.364(2) 0.9747(8) 0.023(6) 1.0000 Uiso . . . . . . C43 C 1.0112(14) 0.277(2) 0.9395(8) 0.025(7) 1.0000 Uiso . . . . . . C44 C 0.9507(15) 0.275(2) 0.8972(8) 0.029(7) 1.0000 Uiso . . . . . . C45 C 0.5711(14) 0.197(2) 0.5753(8) 0.021(6) 1.0000 Uiso . . . . . . C46 C 0.4918(16) 0.262(3) 0.5568(9) 0.041(8) 1.0000 Uiso . . . . . . C47 C 0.4685(15) 0.233(3) 0.5071(9) 0.024(6) 1.0000 Uiso . . . . . . C48 C 0.5117(15) 0.161(3) 0.4791(9) 0.030(7) 1.0000 Uiso . . . . . . C49 C 0.5890(15) 0.089(2) 0.4935(9) 0.026(6) 1.0000 Uiso . . . . . . C50 C 0.6175(16) 0.123(3) 0.5451(9) 0.035(7) 1.0000 Uiso . . . . . . C51 C 0.9651(16) 0.704(3) 0.7485(9) 0.038(2) 1.0000 Uiso D U . . . . C52 C 1.0395(15) 0.650(3) 0.7198(9) 0.040(3) 1.0000 Uiso D U . . . . C53 C 1.0936(16) 0.752(3) 0.6914(9) 0.042(3) 1.0000 Uiso D U . . . . C54 C 1.1593(16) 0.683(3) 0.6622(9) 0.044(3) 1.0000 Uiso D U . . . . C55 C 1.2069(15) 0.787(3) 0.6321(9) 0.045(3) 1.0000 Uiso D U . . . . C56 C 1.2711(16) 0.726(3) 0.6008(9) 0.046(4) 1.0000 Uiso D U . . . . C57 C 0.8053(17) 0.630(3) 0.5818(10) 0.044(3) 1.0000 Uiso D U . . . . C58 C 0.8900(16) 0.589(3) 0.5648(10) 0.049(3) 1.0000 Uiso D U . . . . C59 C 0.9483(17) 0.702(3) 0.5476(10) 0.053(3) 1.0000 Uiso D U . . . . C60 C 1.0224(18) 0.635(3) 0.5231(10) 0.057(3) 1.0000 Uiso D U . . . . C61 C 1.0724(18) 0.727(3) 0.4950(11) 0.060(4) 1.0000 Uiso D U . . . . C62 C 1.1406(19) 0.650(3) 0.4707(11) 0.061(4) 1.0000 Uiso D U . . . . C63 C 0.4417(17) -0.086(3) 0.7312(10) 0.050(3) 1.0000 Uiso D U . . . . C64 C 0.3651(17) -0.009(3) 0.7515(10) 0.054(3) 1.0000 Uiso D U . . . . C65 C 0.3122(17) -0.108(3) 0.7791(10) 0.058(3) 1.0000 Uiso D U . . . . C66 C 0.2352(18) -0.037(3) 0.7974(11) 0.060(3) 1.0000 Uiso D U . . . . C67 C 0.1783(18) -0.120(3) 0.8295(10) 0.061(4) 1.0000 Uiso D U . . . . C68 C 0.1077(19) -0.045(3) 0.8509(11) 0.062(4) 1.0000 Uiso D U . . . . C69 C 0.6067(17) -0.003(3) 0.9023(10) 0.048(3) 1.0000 Uiso D U . . . . C70 C 0.5340(17) 0.059(3) 0.9290(10) 0.053(3) 1.0000 Uiso D U . . . . C71 C 0.4861(18) -0.053(3) 0.9540(11) 0.057(3) 1.0000 Uiso D U . . . . C72 C 0.4117(18) -0.003(3) 0.9812(10) 0.060(3) 1.0000 Uiso D U . . . . C73 C 0.3471(18) 0.067(3) 0.9383(11) 0.063(4) 1.0000 Uiso D U . . . . C74 C 0.2661(19) 0.091(3) 0.9588(11) 0.064(4) 1.0000 Uiso D U . . . . C75 C 0.567(2) 0.481(4) 0.8594(13) 0.087(5) 1.0000 Uiso D U . . . . C76 C 0.488(2) 0.559(4) 0.8749(13) 0.089(5) 1.0000 Uiso D U . . . . C77 C 0.424(2) 0.473(4) 0.8966(13) 0.091(5) 1.0000 Uiso D U . . . . C78 C 0.337(2) 0.551(4) 0.9000(14) 0.093(5) 1.0000 Uiso D U . . . . C79 C 0.268(2) 0.482(4) 0.9213(14) 0.094(5) 1.0000 Uiso D U . . . . C80 C 0.194(2) 0.571(4) 0.9270(14) 0.093(5) 1.0000 Uiso D U . . . . C81 C 0.9016(17) 1.190(3) 0.6874(10) 0.051(4) 1.0000 Uiso D U . . . . C82 C 0.9819(17) 1.138(3) 0.6681(10) 0.052(4) 1.0000 Uiso D U . . . . C83 C 1.0325(17) 1.243(3) 0.6428(10) 0.053(3) 1.0000 Uiso D U . . . . C84 C 1.1083(17) 1.187(3) 0.6192(10) 0.054(4) 1.0000 Uiso D U . . . . C85 C 1.1613(16) 1.285(3) 0.5904(9) 0.054(4) 1.0000 Uiso D U . . . . C86 C 1.2328(17) 1.215(3) 0.5632(10) 0.055(4) 1.0000 Uiso D U . . . . C87 C 0.4182(18) 0.388(3) 0.7115(11) 0.056(9) 1.0000 Uiso . . . . . . Cl1 Cl 0.3583(10) 0.3470(18) 0.6585(6) 0.046(5) 0.5000 Uiso . . . 1 1 . Cl3 Cl 0.3360(11) 0.303(2) 0.6720(6) 0.057(6) 0.5000 Uiso . . . 1 2 . Cl4 Cl 0.3820(12) 0.531(2) 0.7417(7) 0.074(6) 0.5000 Uiso . . . 1 1 . Cl2 Cl 0.3593(15) 0.469(3) 0.7601(9) 0.108(8) 0.5000 Uiso . . . 1 2 . O9 O 0.816(2) 0.798(5) 0.2595(15) 0.078(19) 0.50(6) Uiso . U P 1 1 2 O10 O 0.845(5) 0.836(10) 0.157(3) 0.078(19) 0.27(4) Uiso . U P 1 2 2 O100 O 0.891(5) 0.772(8) 0.226(3) 0.078(19) 0.27(5) Uiso . U P 1 3 2 H101 H 0.5352 0.0201 0.8070 0.0680 1.0000 Uiso . . . . . . H261 H 0.8105 0.8117 0.8956 0.0380 1.0000 Uiso . . . . . . H271 H 0.8825 0.9868 0.8576 0.0361 1.0000 Uiso . . . . . . H311 H 0.6644 0.8488 0.6531 0.0382 1.0000 Uiso . . . . . . H321 H 0.6029 0.6662 0.6920 0.0391 1.0000 Uiso . . . . . . H351 H 0.4284 -0.0900 0.6349 0.0840 1.0000 Uiso . . . . . . H352 H 0.4999 -0.0684 0.5983 0.0840 1.0000 Uiso . . . . . . H353 H 0.4309 0.0469 0.6034 0.0840 1.0000 Uiso . . . . . . H361 H 0.6158 0.4031 0.5260 0.0740 1.0000 Uiso . . . . . . H362 H 0.7090 0.3655 0.5154 0.0739 1.0000 Uiso . . . . . . H363 H 0.6808 0.5224 0.5170 0.0740 1.0000 Uiso . . . . . . H371 H 0.9998 0.6909 0.8482 0.0680 1.0000 Uiso . . . . . . H372 H 0.9453 0.6086 0.8847 0.0680 1.0000 Uiso . . . . . . H373 H 1.0194 0.5330 0.8599 0.0680 1.0000 Uiso . . . . . . H381 H 0.8203 0.1670 0.9464 0.0780 1.0000 Uiso . . . . . . H382 H 0.7389 0.2334 0.9664 0.0780 1.0000 Uiso . . . . . . H383 H 0.7442 0.0713 0.9584 0.0779 1.0000 Uiso . . . . . . H411 H 0.9227 0.5049 1.0052 0.0841 1.0000 Uiso . . . . . . H431 H 1.0610 0.2234 0.9418 0.0501 1.0000 Uiso . . . . . . H441 H 0.9599 0.2138 0.8699 0.0441 1.0000 Uiso . . . . . . H471 H 0.4168 0.2667 0.4930 0.0321 1.0000 Uiso . . . . . . H501 H 0.6672 0.0827 0.5575 0.0491 1.0000 Uiso . . . . . . H511 H 0.9914 0.7646 0.7744 0.0590 1.0000 Uiso . . . . . . H512 H 0.9343 0.7693 0.7255 0.0590 1.0000 Uiso . . . . . . H521 H 1.0772 0.6019 0.7430 0.0621 1.0000 Uiso . . . . . . H522 H 1.0164 0.5840 0.6960 0.0620 1.0000 Uiso . . . . . . H531 H 1.1214 0.8158 0.7155 0.0651 1.0000 Uiso . . . . . . H532 H 1.0564 0.8071 0.6699 0.0650 1.0000 Uiso . . . . . . H541 H 1.1995 0.6336 0.6848 0.0671 1.0000 Uiso . . . . . . H542 H 1.1322 0.6132 0.6407 0.0670 1.0000 Uiso . . . . . . H551 H 1.2323 0.8562 0.6551 0.0691 1.0000 Uiso . . . . . . H552 H 1.1648 0.8363 0.6115 0.0690 1.0000 Uiso . . . . . . H561 H 1.2971 0.7962 0.5834 0.0869 1.0000 Uiso . . . . . . H562 H 1.3148 0.6804 0.6229 0.0870 1.0000 Uiso . . . . . . H563 H 1.2467 0.6556 0.5806 0.0870 1.0000 Uiso . . . . . . H571 H 0.8165 0.7123 0.6023 0.0690 1.0000 Uiso . . . . . . H572 H 0.7738 0.6666 0.5514 0.0690 1.0000 Uiso . . . . . . H581 H 0.9184 0.5314 0.5906 0.0750 1.0000 Uiso . . . . . . H582 H 0.8801 0.5193 0.5363 0.0751 1.0000 Uiso . . . . . . H591 H 0.9728 0.7470 0.5758 0.0800 1.0000 Uiso . . . . . . H592 H 0.9216 0.7584 0.5249 0.0801 1.0000 Uiso . . . . . . H601 H 1.0612 0.5846 0.5473 0.0851 1.0000 Uiso . . . . . . H602 H 1.0024 0.5584 0.4998 0.0850 1.0000 Uiso . . . . . . H611 H 1.1041 0.7983 0.5166 0.0881 1.0000 Uiso . . . . . . H612 H 1.0410 0.7818 0.4702 0.0881 1.0000 Uiso . . . . . . H621 H 1.1926 0.6993 0.4672 0.1120 1.0000 Uiso . . . . . . H622 H 1.1538 0.5611 0.4883 0.1120 1.0000 Uiso . . . . . . H623 H 1.1204 0.6190 0.4369 0.1121 1.0000 Uiso . . . . . . H631 H 0.4688 -0.1429 0.7561 0.0761 1.0000 Uiso . . . . . . H632 H 0.4178 -0.1498 0.7052 0.0760 1.0000 Uiso . . . . . . H641 H 0.3878 0.0556 0.7752 0.0810 1.0000 Uiso . . . . . . H642 H 0.3324 0.0283 0.7267 0.0810 1.0000 Uiso . . . . . . H651 H 0.3407 -0.1517 0.8091 0.0860 1.0000 Uiso . . . . . . H652 H 0.2888 -0.1883 0.7598 0.0860 1.0000 Uiso . . . . . . H661 H 0.2582 0.0558 0.8164 0.0890 1.0000 Uiso . . . . . . H662 H 0.2047 0.0126 0.7684 0.0890 1.0000 Uiso . . . . . . H671 H 0.2192 -0.1604 0.8530 0.0910 1.0000 Uiso . . . . . . H672 H 0.1619 -0.1934 0.8053 0.0911 1.0000 Uiso . . . . . . H681 H 0.0788 -0.1070 0.8667 0.1150 1.0000 Uiso . . . . . . H682 H 0.1319 0.0310 0.8690 0.1150 1.0000 Uiso . . . . . . H683 H 0.0755 -0.0039 0.8221 0.1150 1.0000 Uiso . . . . . . H691 H 0.6419 -0.0505 0.9267 0.0730 1.0000 Uiso . . . . . . H692 H 0.5818 -0.0756 0.8798 0.0730 1.0000 Uiso . . . . . . H701 H 0.5529 0.1279 0.9519 0.0780 1.0000 Uiso . . . . . . H702 H 0.4933 0.1040 0.9048 0.0781 1.0000 Uiso . . . . . . H711 H 0.5248 -0.0986 0.9792 0.0820 1.0000 Uiso . . . . . . H712 H 0.4679 -0.1276 0.9311 0.0820 1.0000 Uiso . . . . . . H721 H 0.4285 0.0747 1.0021 0.0860 1.0000 Uiso . . . . . . H722 H 0.3827 -0.0715 0.9961 0.0860 1.0000 Uiso . . . . . . H731 H 0.3728 0.1512 0.9287 0.0900 1.0000 Uiso . . . . . . H732 H 0.3442 -0.0014 0.9129 0.0900 1.0000 Uiso . . . . . . H741 H 0.2219 0.0916 0.9292 0.1151 1.0000 Uiso . . . . . . H742 H 0.2605 0.1833 0.9722 0.1150 1.0000 Uiso . . . . . . H743 H 0.2471 0.0224 0.9798 0.1150 1.0000 Uiso . . . . . . H751 H 0.5967 0.4435 0.8878 0.1340 1.0000 Uiso . . . . . . H752 H 0.5490 0.4027 0.8378 0.1339 1.0000 Uiso . . . . . . H761 H 0.5069 0.6265 0.8980 0.1350 1.0000 Uiso . . . . . . H762 H 0.4627 0.5994 0.8458 0.1350 1.0000 Uiso . . . . . . H771 H 0.4366 0.4483 0.9312 0.1370 1.0000 Uiso . . . . . . H772 H 0.4070 0.3885 0.8794 0.1370 1.0000 Uiso . . . . . . H781 H 0.3514 0.6481 0.9168 0.1381 1.0000 Uiso . . . . . . H782 H 0.3227 0.5898 0.8645 0.1380 1.0000 Uiso . . . . . . H791 H 0.2937 0.4436 0.9520 0.1381 1.0000 Uiso . . . . . . H792 H 0.2578 0.3996 0.8993 0.1380 1.0000 Uiso . . . . . . H801 H 0.1565 0.5160 0.9477 0.1730 1.0000 Uiso . . . . . . H802 H 0.2094 0.6529 0.9423 0.1730 1.0000 Uiso . . . . . . H803 H 0.1658 0.5829 0.8961 0.1731 1.0000 Uiso . . . . . . H821 H 1.0162 1.0975 0.6958 0.0890 1.0000 Uiso . . . . . . H822 H 0.9674 1.0567 0.6460 0.0890 1.0000 Uiso . . . . . . H831 H 1.0493 1.3138 0.6648 0.0900 1.0000 Uiso . . . . . . H832 H 0.9956 1.2820 0.6160 0.0900 1.0000 Uiso . . . . . . H841 H 1.1468 1.1479 0.6449 0.0900 1.0000 Uiso . . . . . . H842 H 1.0916 1.1083 0.5973 0.0900 1.0000 Uiso . . . . . . H851 H 1.1851 1.3548 0.6110 0.0900 1.0000 Uiso . . . . . . H852 H 1.1241 1.3273 0.5645 0.0901 1.0000 Uiso . . . . . . H861 H 1.2641 1.2867 0.5463 0.1130 1.0000 Uiso . . . . . . H862 H 1.2708 1.1703 0.5866 0.1130 1.0000 Uiso . . . . . . H863 H 1.2114 1.1487 0.5399 0.1130 1.0000 Uiso . . . . . . H871 H 0.4429 0.3138 0.7340 0.0619 0.5000 Uiso . . . 1 1 . H872 H 0.4670 0.4202 0.6904 0.0619 0.5000 Uiso . . . 1 1 . H873 H 0.4494 0.3024 0.7247 0.0619 0.5000 Uiso . . . 1 2 . H874 H 0.4642 0.4582 0.7026 0.0619 0.5000 Uiso . . . 1 2 . H811 H 0.9160 1.2703 0.7102 0.0735 1.0000 Uiso . . . . . . H812 H 0.8653 1.2270 0.6591 0.0735 1.0000 Uiso . . . . . . H201 H 0.8659 0.6375 0.6688 0.0474 1.0000 Uiso . . . . . . H491 H 0.6190 0.0210 0.4722 0.0325 1.0000 Uiso . . . . . . H461 H 0.4508 0.3197 0.5815 0.0651 1.0000 Uiso . . . . . . H401 H 0.8055 0.4982 0.9391 0.0357 1.0000 Uiso . . . . . . _refine_ls_extinction_method None _oxford_refine_ls_scale 0.393(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zn1 . N1 . 2.215(15) yes Zn1 . N2 . 2.171(15) yes Zn1 . N3 . 1.993(15) yes Zn1 . N4 . 2.073(15) yes Zn1 . O1 . 2.326(18) yes Zn2 . N1 . 1.925(15) yes Zn2 . N2 . 2.071(15) yes Zn2 . N3 . 2.220(16) yes Zn2 . N4 . 2.095(15) yes N1 . C1 . 1.22(3) yes N1 . C4 . 1.43(3) yes N2 . C16 . 1.45(3) yes N2 . C19 . 1.32(3) yes N3 . C11 . 1.32(3) yes N3 . C14 . 1.47(3) yes N4 . C6 . 1.45(3) yes N4 . C9 . 1.35(3) yes N5 . C21 . 1.46(4) yes N5 . C25 . 1.49(4) yes N5 . C75 . 1.42(3) yes N6 . C33 . 1.49(3) yes N6 . C34 . 1.45(3) yes N6 . C81 . 1.37(3) yes N7 . O5 . 1.26(3) yes N7 . O6 . 1.19(2) yes N7 . C42 . 1.69(3) yes N8 . O7 . 1.31(3) yes N8 . O8 . 1.16(2) yes N8 . C48 . 1.62(3) yes O1 . C21 . 1.30(3) yes O2 . C34 . 1.37(3) yes O3 . C33 . 1.25(3) yes O4 . C25 . 1.30(3) yes C1 . C2 . 1.55(4) yes C1 . C20 . 1.54(4) yes C2 . C3 . 1.45(4) yes C2 . C57 . 1.36(4) yes C3 . C4 . 1.48(4) yes C3 . C36 . 1.48(3) yes C4 . C5 . 1.43(3) yes C5 . C6 . 1.36(3) yes C5 . C45 . 1.52(3) yes C6 . C7 . 1.47(4) yes C7 . C8 . 1.33(4) yes C7 . C35 . 1.56(4) yes C8 . C9 . 1.48(4) yes C8 . C63 . 1.51(4) yes C9 . C10 . 1.39(4) yes C10 . C11 . 1.49(4) yes C10 . H101 . 0.983 no C11 . C12 . 1.46(4) yes C12 . C13 . 1.43(4) yes C12 . C69 . 1.46(4) yes C13 . C14 . 1.43(4) yes C13 . C38 . 1.53(3) yes C14 . C15 . 1.42(3) yes C15 . C16 . 1.38(3) yes C15 . C39 . 1.54(3) yes C16 . C17 . 1.51(4) yes C17 . C18 . 1.32(3) yes C17 . C37 . 1.56(3) yes C18 . C19 . 1.49(3) yes C18 . C51 . 1.43(3) yes C19 . C20 . 1.49(4) yes C20 . H201 . 1.050 no C21 . C22 . 1.38(3) yes C22 . C23 . 1.41(3) yes C22 . C32 . 1.41(3) yes C23 . C24 . 1.47(3) yes C23 . C29 . 1.34(3) yes C24 . C25 . 1.41(3) yes C24 . C26 . 1.44(3) yes C26 . C27 . 1.35(3) yes C26 . H261 . 0.966 no C27 . C28 . 1.44(3) yes C27 . H271 . 0.911 no C28 . C29 . 1.55(3) yes C28 . C33 . 1.38(3) yes C29 . C30 . 1.45(3) yes C30 . C31 . 1.45(3) yes C30 . C34 . 1.27(3) yes C31 . C32 . 1.34(3) yes C31 . H311 . 0.959 no C32 . H321 . 0.939 no C35 . H351 . 1.003 no C35 . H352 . 0.953 no C35 . H353 . 0.960 no C36 . H361 . 0.975 no C36 . H362 . 0.988 no C36 . H363 . 0.941 no C37 . H371 . 0.937 no C37 . H372 . 0.981 no C37 . H373 . 0.985 no C38 . H381 . 0.986 no C38 . H382 . 0.968 no C38 . H383 . 0.962 no C39 . C40 . 1.45(3) yes C39 . C44 . 1.37(3) yes C40 . C41 . 1.46(4) yes C40 . H401 . 0.991 no C41 . C42 . 1.36(4) yes C41 . H411 . 0.949 no C42 . C43 . 1.32(3) yes C43 . C44 . 1.47(3) yes C43 . H431 . 0.945 no C44 . H441 . 0.967 no C45 . C46 . 1.47(3) yes C45 . C50 . 1.34(3) yes C46 . C47 . 1.42(3) yes C46 . H461 . 1.115 no C47 . C48 . 1.26(3) yes C47 . H471 . 0.950 no C48 . C49 . 1.45(3) yes C49 . C50 . 1.50(3) yes C49 . H491 . 1.010 no C50 . H501 . 0.931 no C51 . C52 . 1.55(3) yes C51 . H511 . 0.990 no C51 . H512 . 0.997 no C52 . C53 . 1.54(3) yes C52 . H521 . 0.968 no C52 . H522 . 0.966 no C53 . C54 . 1.51(3) yes C53 . H531 . 0.986 no C53 . H532 . 0.969 no C54 . C55 . 1.52(3) yes C54 . H541 . 0.991 no C54 . H542 . 0.979 no C55 . C56 . 1.49(3) yes C55 . H551 . 0.986 no C55 . H552 . 0.977 no C56 . H561 . 0.935 no C56 . H562 . 0.999 no C56 . H563 . 0.942 no C57 . C58 . 1.51(3) yes C57 . H571 . 0.981 no C57 . H572 . 1.012 no C58 . C59 . 1.52(3) yes C58 . H581 . 0.987 no C58 . H582 . 1.032 no C59 . C60 . 1.53(3) yes C59 . H591 . 0.952 no C59 . H592 . 0.913 no C60 . C61 . 1.44(3) yes C60 . H601 . 1.005 no C60 . H602 . 1.013 no C61 . C62 . 1.50(3) yes C61 . H611 . 1.020 no C61 . H612 . 0.976 no C62 . H621 . 0.961 no C62 . H622 . 1.000 no C62 . H623 . 1.010 no C63 . C64 . 1.56(3) yes C63 . H631 . 0.960 no C63 . H632 . 1.000 no C64 . C65 . 1.50(3) yes C64 . H641 . 0.955 no C64 . H642 . 0.907 no C65 . C66 . 1.52(3) yes C65 . H651 . 1.008 no C65 . H652 . 0.994 no C66 . C67 . 1.52(3) yes C66 . H661 . 1.080 no C66 . H662 . 1.024 no C67 . C68 . 1.48(3) yes C67 . H671 . 0.974 no C67 . H672 . 0.994 no C68 . H681 . 0.878 no C68 . H682 . 0.954 no C68 . H683 . 1.001 no C69 . C70 . 1.53(3) yes C69 . H691 . 0.964 no C69 . H692 . 0.997 no C70 . C71 . 1.50(3) yes C70 . H701 . 0.947 no C70 . H702 . 1.001 no C71 . C72 . 1.51(3) yes C71 . H711 . 1.002 no C71 . H712 . 0.989 no C72 . C73 . 1.66(3) yes C72 . H721 . 0.969 no C72 . H722 . 0.912 no C73 . C74 . 1.45(3) yes C73 . H731 . 0.950 no C73 . H732 . 0.954 no C74 . H741 . 1.046 no C74 . H742 . 0.967 no C74 . H743 . 0.934 no C75 . C76 . 1.54(3) yes C75 . H751 . 0.959 no C75 . H752 . 0.993 no C76 . C77 . 1.47(3) yes C76 . H761 . 0.944 no C76 . H762 . 0.959 no C77 . C78 . 1.59(3) yes C77 . H771 . 0.988 no C77 . H772 . 0.966 no C78 . C79 . 1.43(3) yes C78 . H781 . 1.062 no C78 . H782 . 1.057 no C79 . C80 . 1.47(3) yes C79 . H791 . 0.989 no C79 . H792 . 0.999 no C80 . H801 . 0.995 no C80 . H802 . 0.918 no C80 . H803 . 0.946 no C81 . C82 . 1.50(3) yes C81 . H811 . 1.005 no C81 . H812 . 1.007 no C82 . C83 . 1.48(3) yes C82 . H821 . 0.992 no C82 . H822 . 1.008 no C83 . C84 . 1.50(3) yes C83 . H831 . 0.938 no C83 . H832 . 0.992 no C84 . C85 . 1.51(3) yes C84 . H841 . 0.987 no C84 . H842 . 0.993 no C85 . C86 . 1.55(3) yes C85 . H851 . 0.940 no C85 . H852 . 0.988 no C86 . H861 . 0.977 no C86 . H862 . 0.961 no C86 . H863 . 0.952 no C87 . Cl1 . 1.74(3) yes C87 . Cl3 . 1.85(3) yes C87 . Cl4 . 1.71(4) yes C87 . Cl2 . 1.84(4) yes C87 . H871 . 1.007 no C87 . H872 . 1.042 no C87 . H873 . 1.016 no C87 . H874 . 1.034 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Zn1 . N2 . 85.4(6) yes N1 . Zn1 . N3 . 158.2(7) yes N2 . Zn1 . N3 . 89.3(6) yes N1 . Zn1 . N4 . 84.7(6) yes N2 . Zn1 . N4 . 155.6(7) yes N3 . Zn1 . N4 . 91.7(7) yes N1 . Zn1 . O1 . 100.9(6) yes N2 . Zn1 . O1 . 107.6(7) yes N3 . Zn1 . O1 . 100.9(7) yes N4 . Zn1 . O1 . 96.2(6) yes N1 . Zn2 . N2 . 96.1(7) yes N1 . Zn2 . N3 . 171.2(7) yes N2 . Zn2 . N3 . 86.0(6) yes N1 . Zn2 . N4 . 91.9(7) yes N2 . Zn2 . N4 . 169.5(8) yes N3 . Zn2 . N4 . 85.1(6) yes Zn1 . N1 . C1 . 123.7(16) yes Zn2 . N1 . C1 . 124.4(16) yes Zn1 . N1 . C4 . 128.4(15) yes Zn2 . N1 . C4 . 131.0(15) yes C1 . N1 . C4 . 104.6(19) yes Zn1 . N2 . C16 . 124.1(15) yes Zn2 . N2 . C16 . 130.6(15) yes Zn1 . N2 . C19 . 125.7(14) yes Zn2 . N2 . C19 . 120.9(15) yes C16 . N2 . C19 . 108.4(19) yes Zn2 . N3 . C11 . 126.7(15) yes Zn1 . N3 . C11 . 125.9(15) yes Zn2 . N3 . C14 . 126.0(14) yes Zn1 . N3 . C14 . 129.0(15) yes C11 . N3 . C14 . 105.1(18) yes Zn2 . N4 . C6 . 121.5(15) yes Zn1 . N4 . C6 . 128.3(16) yes Zn2 . N4 . C9 . 132.7(15) yes Zn1 . N4 . C9 . 124.0(15) yes C6 . N4 . C9 . 105.7(19) yes C21 . N5 . C25 . 114(2) yes C21 . N5 . C75 . 125(3) yes C25 . N5 . C75 . 121(3) yes C33 . N6 . C34 . 114(2) yes C33 . N6 . C81 . 120(2) yes C34 . N6 . C81 . 126(2) yes O5 . N7 . O6 . 138(2) yes O5 . N7 . C42 . 111(2) yes O6 . N7 . C42 . 111(2) yes O7 . N8 . O8 . 134(2) yes O7 . N8 . C48 . 109(2) yes O8 . N8 . C48 . 117(2) yes Zn1 . O1 . C21 . 99.9(14) yes N1 . C1 . C2 . 121(2) yes N1 . C1 . C20 . 133(2) yes C2 . C1 . C20 . 106(2) yes C1 . C2 . C3 . 97(2) yes C1 . C2 . C57 . 132(2) yes C3 . C2 . C57 . 131(3) yes C2 . C3 . C4 . 108(2) yes C2 . C3 . C36 . 119(2) yes C4 . C3 . C36 . 133(2) yes C3 . C4 . N1 . 110(2) yes C3 . C4 . C5 . 130(2) yes N1 . C4 . C5 . 120(2) yes C4 . C5 . C6 . 129(2) yes C4 . C5 . C45 . 114(2) yes C6 . C5 . C45 . 117(2) yes N4 . C6 . C5 . 126(2) yes N4 . C6 . C7 . 106(2) yes C5 . C6 . C7 . 128(2) yes C6 . C7 . C8 . 112(2) yes C6 . C7 . C35 . 130(2) yes C8 . C7 . C35 . 118(3) yes C7 . C8 . C9 . 104(3) yes C7 . C8 . C63 . 135(3) yes C9 . C8 . C63 . 121(3) yes C8 . C9 . N4 . 113(2) yes C8 . C9 . C10 . 125(3) yes N4 . C9 . C10 . 122(2) yes C9 . C10 . C11 . 127(3) yes C9 . C10 . H101 . 117.1 no C11 . C10 . H101 . 115.4 no C10 . C11 . N3 . 122(2) yes C10 . C11 . C12 . 121(3) yes N3 . C11 . C12 . 114(2) yes C11 . C12 . C13 . 103(3) yes C11 . C12 . C69 . 129(2) yes C13 . C12 . C69 . 128(3) yes C12 . C13 . C14 . 108(2) yes C12 . C13 . C38 . 119(3) yes C14 . C13 . C38 . 133(2) yes N3 . C14 . C13 . 108(2) yes N3 . C14 . C15 . 122(2) yes C13 . C14 . C15 . 129(2) yes C14 . C15 . C16 . 129(2) yes C14 . C15 . C39 . 116(2) yes C16 . C15 . C39 . 115(2) yes N2 . C16 . C15 . 124(2) yes N2 . C16 . C17 . 106(2) yes C15 . C16 . C17 . 131(2) yes C16 . C17 . C18 . 107(2) yes C16 . C17 . C37 . 131(2) yes C18 . C17 . C37 . 122(2) yes C17 . C18 . C19 . 108(2) yes C17 . C18 . C51 . 129(2) yes C19 . C18 . C51 . 122(2) yes C18 . C19 . N2 . 110(2) yes C18 . C19 . C20 . 121(2) yes N2 . C19 . C20 . 129(2) yes C1 . C20 . C19 . 116(2) yes C1 . C20 . H201 . 122.5 no C19 . C20 . H201 . 120.6 no N5 . C21 . O1 . 113(2) yes N5 . C21 . C22 . 123(2) yes O1 . C21 . C22 . 124(2) yes C21 . C22 . C23 . 121(2) yes C21 . C22 . C32 . 121(2) yes C23 . C22 . C32 . 118(2) yes C22 . C23 . C24 . 120(2) yes C22 . C23 . C29 . 119(2) yes C24 . C23 . C29 . 121(2) yes C23 . C24 . C25 . 119(2) yes C23 . C24 . C26 . 118(2) yes C25 . C24 . C26 . 124(2) yes N5 . C25 . C24 . 122(2) yes N5 . C25 . O4 . 112(2) yes C24 . C25 . O4 . 124(2) yes C24 . C26 . C27 . 123(2) yes C24 . C26 . H261 . 113.2 no C27 . C26 . H261 . 123.5 no C26 . C27 . C28 . 122(2) yes C26 . C27 . H271 . 117.9 no C28 . C27 . H271 . 120.5 no C27 . C28 . C29 . 116(2) yes C27 . C28 . C33 . 122(2) yes C29 . C28 . C33 . 122(2) yes C28 . C29 . C23 . 121(2) yes C28 . C29 . C30 . 113(2) yes C23 . C29 . C30 . 126(2) yes C29 . C30 . C31 . 111(2) yes C29 . C30 . C34 . 122(2) yes C31 . C30 . C34 . 127(2) yes C30 . C31 . C32 . 124(2) yes C30 . C31 . H311 . 117.6 no C32 . C31 . H311 . 118.4 no C22 . C32 . C31 . 122(2) yes C22 . C32 . H321 . 116.6 no C31 . C32 . H321 . 121.6 no N6 . C33 . C28 . 120(2) yes N6 . C33 . O3 . 114(2) yes C28 . C33 . O3 . 126(2) yes N6 . C34 . O2 . 108(2) yes N6 . C34 . C30 . 128(2) yes O2 . C34 . C30 . 122(2) yes C7 . C35 . H351 . 107.3 no C7 . C35 . H352 . 113.4 no H351 . C35 . H352 . 107.0 no C7 . C35 . H353 . 112.1 no H351 . C35 . H353 . 106.4 no H352 . C35 . H353 . 110.3 no C3 . C36 . H361 . 109.2 no C3 . C36 . H362 . 108.6 no H361 . C36 . H362 . 106.4 no C3 . C36 . H363 . 113.2 no H361 . C36 . H363 . 110.2 no H362 . C36 . H363 . 109.0 no C17 . C37 . H371 . 114.4 no C17 . C37 . H372 . 106.9 no H371 . C37 . H372 . 110.0 no C17 . C37 . H373 . 109.3 no H371 . C37 . H373 . 109.7 no H372 . C37 . H373 . 106.2 no C13 . C38 . H381 . 108.6 no C13 . C38 . H382 . 112.4 no H381 . C38 . H382 . 107.0 no C13 . C38 . H383 . 112.2 no H381 . C38 . H383 . 107.5 no H382 . C38 . H383 . 109.0 no C15 . C39 . C40 . 118(2) yes C15 . C39 . C44 . 117(2) yes C40 . C39 . C44 . 125(2) yes C39 . C40 . C41 . 112(2) yes C39 . C40 . H401 . 124.2 no C41 . C40 . H401 . 122.7 no C40 . C41 . C42 . 120(3) yes C40 . C41 . H411 . 123.5 no C42 . C41 . H411 . 115.4 no N7 . C42 . C41 . 116(2) yes N7 . C42 . C43 . 114.6(20) yes C41 . C42 . C43 . 129(2) yes C42 . C43 . C44 . 115(2) yes C42 . C43 . H431 . 121.2 no C44 . C43 . H431 . 124.1 no C43 . C44 . C39 . 119(2) yes C43 . C44 . H441 . 119.8 no C39 . C44 . H441 . 120.9 no C5 . C45 . C46 . 119(2) yes C5 . C45 . C50 . 120(2) yes C46 . C45 . C50 . 120(2) yes C45 . C46 . C47 . 115(2) yes C45 . C46 . H461 . 121.5 no C47 . C46 . H461 . 123.1 no C46 . C47 . C48 . 124(2) yes C46 . C47 . H471 . 120.1 no C48 . C47 . H471 . 115.4 no N8 . C48 . C47 . 120(2) yes N8 . C48 . C49 . 115(2) yes C47 . C48 . C49 . 125(2) yes C48 . C49 . C50 . 111(2) yes C48 . C49 . H491 . 124.9 no C50 . C49 . H491 . 123.9 no C49 . C50 . C45 . 123(2) yes C49 . C50 . H501 . 117.6 no C45 . C50 . H501 . 118.7 no C18 . C51 . C52 . 117(2) yes C18 . C51 . H511 . 111.6 no C52 . C51 . H511 . 104.7 no C18 . C51 . H512 . 112.6 no C52 . C51 . H512 . 104.7 no H511 . C51 . H512 . 105.3 no C51 . C52 . C53 . 120(2) yes C51 . C52 . H521 . 106.9 no C53 . C52 . H521 . 106.8 no C51 . C52 . H522 . 106.7 no C53 . C52 . H522 . 106.1 no H521 . C52 . H522 . 109.6 no C52 . C53 . C54 . 114(2) yes C52 . C53 . H531 . 107.4 no C54 . C53 . H531 . 109.0 no C52 . C53 . H532 . 108.2 no C54 . C53 . H532 . 109.5 no H531 . C53 . H532 . 108.2 no C53 . C54 . C55 . 113(2) yes C53 . C54 . H541 . 108.8 no C55 . C54 . H541 . 109.2 no C53 . C54 . H542 . 108.9 no C55 . C54 . H542 . 109.8 no H541 . C54 . H542 . 107.3 no C54 . C55 . C56 . 116(2) yes C54 . C55 . H551 . 107.0 no C56 . C55 . H551 . 111.2 no C54 . C55 . H552 . 106.4 no C56 . C55 . H552 . 109.1 no H551 . C55 . H552 . 107.1 no C55 . C56 . H561 . 110.3 no C55 . C56 . H562 . 107.3 no H561 . C56 . H562 . 108.1 no C55 . C56 . H563 . 110.1 no H561 . C56 . H563 . 113.3 no H562 . C56 . H563 . 107.5 no C2 . C57 . C58 . 118(2) yes C2 . C57 . H571 . 112.9 no C58 . C57 . H571 . 104.4 no C2 . C57 . H572 . 110.9 no C58 . C57 . H572 . 104.4 no H571 . C57 . H572 . 105.0 no C57 . C58 . C59 . 119(2) yes C57 . C58 . H581 . 107.8 no C59 . C58 . H581 . 110.8 no C57 . C58 . H582 . 107.4 no C59 . C58 . H582 . 107.3 no H581 . C58 . H582 . 103.4 no C58 . C59 . C60 . 110(2) yes C58 . C59 . H591 . 107.7 no C60 . C59 . H591 . 104.7 no C58 . C59 . H592 . 111.3 no C60 . C59 . H592 . 107.0 no H591 . C59 . H592 . 116.3 no C59 . C60 . C61 . 116(3) yes C59 . C60 . H601 . 111.9 no C61 . C60 . H601 . 107.9 no C59 . C60 . H602 . 110.9 no C61 . C60 . H602 . 105.6 no H601 . C60 . H602 . 103.6 no C60 . C61 . C62 . 112(3) yes C60 . C61 . H611 . 111.8 no C62 . C61 . H611 . 103.8 no C60 . C61 . H612 . 115.1 no C62 . C61 . H612 . 108.1 no H611 . C61 . H612 . 105.5 no C61 . C62 . H621 . 117.2 no C61 . C62 . H622 . 110.0 no H621 . C62 . H622 . 107.7 no C61 . C62 . H623 . 110.6 no H621 . C62 . H623 . 106.8 no H622 . C62 . H623 . 103.7 no C8 . C63 . C64 . 117(2) yes C8 . C63 . H631 . 108.7 no C64 . C63 . H631 . 110.3 no C8 . C63 . H632 . 107.6 no C64 . C63 . H632 . 105.6 no H631 . C63 . H632 . 107.4 no C63 . C64 . C65 . 111(2) yes C63 . C64 . H641 . 105.9 no C65 . C64 . H641 . 105.6 no C63 . C64 . H642 . 110.3 no C65 . C64 . H642 . 108.2 no H641 . C64 . H642 . 116.0 no C64 . C65 . C66 . 112(2) yes C64 . C65 . H651 . 115.6 no C66 . C65 . H651 . 104.7 no C64 . C65 . H652 . 115.3 no C66 . C65 . H652 . 103.7 no H651 . C65 . H652 . 104.8 no C65 . C66 . C67 . 118(2) yes C65 . C66 . H661 . 105.7 no C67 . C66 . H661 . 110.3 no C65 . C66 . H662 . 108.1 no C67 . C66 . H662 . 114.6 no H661 . C66 . H662 . 97.7 no C66 . C67 . C68 . 118(3) yes C66 . C67 . H671 . 101.2 no C68 . C67 . H671 . 115.3 no C66 . C67 . H672 . 97.5 no C68 . C67 . H672 . 115.3 no H671 . C67 . H672 . 107.5 no C67 . C68 . H681 . 107.6 no C67 . C68 . H682 . 106.3 no H681 . C68 . H682 . 117.8 no C67 . C68 . H683 . 104.3 no H681 . C68 . H683 . 113.2 no H682 . C68 . H683 . 106.6 no C12 . C69 . C70 . 115(2) yes C12 . C69 . H691 . 111.7 no C70 . C69 . H691 . 106.2 no C12 . C69 . H692 . 110.0 no C70 . C69 . H692 . 106.3 no H691 . C69 . H692 . 107.6 no C69 . C70 . C71 . 111(2) yes C69 . C70 . H701 . 111.6 no C71 . C70 . H701 . 110.0 no C69 . C70 . H702 . 109.4 no C71 . C70 . H702 . 106.3 no H701 . C70 . H702 . 108.4 no C70 . C71 . C72 . 116(2) yes C70 . C71 . H711 . 108.6 no C72 . C71 . H711 . 105.7 no C70 . C71 . H712 . 111.4 no C72 . C71 . H712 . 109.3 no H711 . C71 . H712 . 105.4 no C71 . C72 . C73 . 105(2) yes C71 . C72 . H721 . 109.5 no C73 . C72 . H721 . 104.7 no C71 . C72 . H722 . 115.2 no C73 . C72 . H722 . 107.3 no H721 . C72 . H722 . 114.6 no C72 . C73 . C74 . 109(2) yes C72 . C73 . H731 . 106.2 no C74 . C73 . H731 . 112.2 no C72 . C73 . H732 . 104.2 no C74 . C73 . H732 . 112.3 no H731 . C73 . H732 . 112.6 no C73 . C74 . H741 . 106.1 no C73 . C74 . H742 . 113.2 no H741 . C74 . H742 . 102.5 no C73 . C74 . H743 . 116.9 no H741 . C74 . H743 . 105.0 no H742 . C74 . H743 . 111.5 no N5 . C75 . C76 . 112(3) yes N5 . C75 . H751 . 110.1 no C76 . C75 . H751 . 109.2 no N5 . C75 . H752 . 108.9 no C76 . C75 . H752 . 108.1 no H751 . C75 . H752 . 108.3 no C75 . C76 . C77 . 116(3) yes C75 . C76 . H761 . 106.3 no C77 . C76 . H761 . 108.5 no C75 . C76 . H762 . 106.3 no C77 . C76 . H762 . 106.9 no H761 . C76 . H762 . 112.5 no C76 . C77 . C78 . 113(3) yes C76 . C77 . H771 . 114.2 no C78 . C77 . H771 . 101.1 no C76 . C77 . H772 . 116.9 no C78 . C77 . H772 . 101.6 no H771 . C77 . H772 . 107.9 no C77 . C78 . C79 . 120(3) yes C77 . C78 . H781 . 105.2 no C79 . C78 . H781 . 112.8 no C77 . C78 . H782 . 104.7 no C79 . C78 . H782 . 114.4 no H781 . C78 . H782 . 96.8 no C78 . C79 . C80 . 114(3) yes C78 . C79 . H791 . 102.9 no C80 . C79 . H791 . 115.0 no C78 . C79 . H792 . 102.6 no C80 . C79 . H792 . 114.8 no H791 . C79 . H792 . 105.8 no C79 . C80 . H801 . 105.2 no C79 . C80 . H802 . 110.4 no H801 . C80 . H802 . 110.3 no C79 . C80 . H803 . 108.5 no H801 . C80 . H803 . 107.8 no H802 . C80 . H803 . 114.2 no N6 . C81 . C82 . 117(2) yes N6 . C81 . H811 . 108.2 no C82 . C81 . H811 . 107.6 no N6 . C81 . H812 . 107.4 no C82 . C81 . H812 . 108.1 no H811 . C81 . H812 . 108.5 no C81 . C82 . C83 . 116(2) yes C81 . C82 . H821 . 107.9 no C83 . C82 . H821 . 109.5 no C81 . C82 . H822 . 107.3 no C83 . C82 . H822 . 110.8 no H821 . C82 . H822 . 104.9 no C82 . C83 . C84 . 116(2) yes C82 . C83 . H831 . 109.5 no C84 . C83 . H831 . 109.0 no C82 . C83 . H832 . 106.7 no C84 . C83 . H832 . 105.8 no H831 . C83 . H832 . 110.0 no C83 . C84 . C85 . 119(2) yes C83 . C84 . H841 . 108.1 no C85 . C84 . H841 . 105.5 no C83 . C84 . H842 . 109.7 no C85 . C84 . H842 . 107.2 no H841 . C84 . H842 . 106.1 no C84 . C85 . C86 . 116(2) yes C84 . C85 . H851 . 110.3 no C86 . C85 . H851 . 108.2 no C84 . C85 . H852 . 107.3 no C86 . C85 . H852 . 105.0 no H851 . C85 . H852 . 110.4 no C85 . C86 . H861 . 109.5 no C85 . C86 . H862 . 108.9 no H861 . C86 . H862 . 108.1 no C85 . C86 . H863 . 111.5 no H861 . C86 . H863 . 109.0 no H862 . C86 . H863 . 109.8 no Cl1 . C87 . Cl4 . 113.5(17) yes Cl3 . C87 . Cl4 . 112.8(17) yes Cl1 . C87 . Cl2 . 114.9(17) yes Cl3 . C87 . Cl2 . 103.7(17) yes Cl1 . C87 . H871 . 122.0 no Cl3 . C87 . H871 . 106.9 no Cl4 . C87 . H871 . 113.5 no Cl3 . C87 . H872 . 109.3 no Cl4 . C87 . H872 . 108.4 no Cl2 . C87 . H872 . 134.7 no H871 . C87 . H872 . 105.6 no Cl1 . C87 . H873 . 110.6 no Cl3 . C87 . H873 . 100.0 no Cl4 . C87 . H873 . 130.0 no Cl2 . C87 . H873 . 110.0 no Cl1 . C87 . H874 . 108.2 no Cl3 . C87 . H874 . 129.5 no Cl2 . C87 . H874 . 107.1 no H871 . C87 . H874 . 110.2 no H873 . C87 . H874 . 105.6 no #===END data_cam221 _database_code_depnum_ccdc_archive 'CCDC 767031' #TrackingRef '- CCDC_deposided_merged_cifs_notepad.cif' _audit_creation_date 10-02-19 _audit_creation_method CRYSTALS_ver_12.82 _oxford_structure_analysis_title 'cam221 in P -1' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 13.9065(11) _cell_length_b 16.3006(13) _cell_length_c 17.908(2) _cell_angle_alpha 105.980(2) _cell_angle_beta 94.520(2) _cell_angle_gamma 115.1360(10) _cell_volume 3442.5(5) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Zn 0.2839 1.4301 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097 1.3041 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 _chemical_formula_sum 'C76 H108 N4 Zn1' _chemical_formula_moiety 'C76 H108 N4 Zn1' _chemical_compound_source ? _chemical_formula_weight 1143.10 _cell_measurement_reflns_used 30113 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27 _cell_measurement_temperature 200 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.103 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1244 _exptl_absorpt_coefficient_mu 0.400 _exptl_absorpt_process_details ; Correction applied by SADABS - note that the transmission factors are not real since they include corrections for beam decay and possibly crystal decay (the two cannot be distinguished). The numbers listed in the CIF are those calculated by CRYSTALS. ; _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 1.00 _exptl_absorpt_correction_T_max 1.00 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART APEX2 CCD' _diffrn_measurement_method 'fine-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5 _diffrn_radiation_wavelength 0.71069 _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution Sir2000 _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_ambient_temperature 200 _diffrn_reflns_number 30113 _reflns_number_total 13920 _diffrn_reflns_av_R_equivalents 0.022 # Number of reflections with Friedels Law is 13920 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 14089 _diffrn_reflns_theta_min 1.468 _diffrn_reflns_theta_max 26.376 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.057 _diffrn_measured_fraction_theta_full 0.988 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min -17 _reflns_limit_h_max 17 _reflns_limit_k_min -20 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.06 _refine_diff_density_max 1.12 _refine_ls_number_reflns 8468 _refine_ls_number_restraints 242 _refine_ls_number_parameters 760 #_refine_ls_R_factor_ref 0.1012 _refine_ls_wR_factor_ref 0.1117 _refine_ls_goodness_of_fit_ref 1.1307 #_reflns_number_all 13881 _refine_ls_R_factor_all 0.1351 _refine_ls_wR_factor_all 0.1310 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 8468 _refine_ls_R_factor_gt 0.1012 _refine_ls_wR_factor_gt 0.1117 _refine_ls_shift/su_max 0.046459 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_special_details ; The crystal was extremly weakly diffracting Severe disorder on more than 2 sites was observed for some of the tert-butyl groups: these were idealised and refined with restrains. Low bond precision due to shortage of data and severe disorder in the peripheral sites (tBu groups) of the molecule accounts for remaining errors in the cif but disorder did not affect the overall geometry of the molecule and the core of the porphyrin Hydrogen atoms were placed at the corresponding carbon atoms geometrically after each cycle ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.43 1.22 0.925 ; # Check this file using the IUCr facility at: # http://checkcif.iucr.org/ # Insert your own references if required - in alphabetical order _publ_section_references ; Data collection: APEX2, Bruker AXS Inc., Madison, USA, 2004 Data reduction (frames integration): SAINT, Bruker AXS Inc., Madison, USA, 2004 Cell refinement: SAINT, Bruker AXS Inc., Madison, USA, 2004 Absorption correction: SADABS, Bruker AXS Inc., Madison, USA, 2004 Station 9.8: R. J. Cernik, W. Clegg, C. R. A. Catlow, G. Bushnell-Wye, J. V. Flaherty, G. N. Greaves, M. Hamichi, I. Burrows, D. J. Taylor and S. J. Teat, J. Synchotron Radiation 1997, 4, 279-286; 7, 40. Synchrotron chemical crystallography: W. Clegg, J. Chem. Soc., Dalton Trans. 2000, 3223-3232. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Siemens Industrial Automation, Inc (1996). Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of G\"ottingen, Germany. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Zn1 Zn 0.0000 1.0000 0.0000 0.0298 1.0000 Uani S . . . . . Zn2 Zn -0.5000 0.5000 0.0000 0.0369 1.0000 Uani S . . . . . N1 N -0.0298(3) 1.0951(3) -0.0399(2) 0.0405 1.0000 Uani . . . . . . N2 N -0.0928(3) 0.8961(3) -0.1083(2) 0.0387 1.0000 Uani . . . . . . N3 N -0.3644(3) 0.6010(3) 0.0859(2) 0.0451 1.0000 Uani . . . . . . N4 N -0.5134(3) 0.4057(3) 0.0595(2) 0.0466 1.0000 Uani . . . . . . C1 C -0.0756(4) 0.7638(4) -0.0810(3) 0.0455 1.0000 Uani . . . . . . C2 C -0.1146(4) 0.8018(4) -0.1279(3) 0.0416 1.0000 Uani . . . . . . C3 C -0.1904(4) 0.7450(4) -0.2040(3) 0.0445 1.0000 Uani D . . . . . C4 C -0.2155(4) 0.8064(4) -0.2299(3) 0.0454 1.0000 Uani . . . . . . C5 C -0.1510(4) 0.9037(4) -0.1693(3) 0.0387 1.0000 Uani . . . . . . C6 C -0.1481(4) 0.9891(4) -0.1724(3) 0.0369 1.0000 Uani . . . . . . C7 C -0.0884(4) 1.0802(4) -0.1126(3) 0.0404 1.0000 Uani . . . . . . C8 C -0.0792(4) 1.1729(4) -0.1140(3) 0.0462 1.0000 Uani . . . . . . C9 C -0.0191(4) 1.2396(4) -0.0418(3) 0.0452 1.0000 Uani . . . . . . C10 C 0.0105(4) 1.1896(4) 0.0033(3) 0.0424 1.0000 Uani . . . . . . C11 C -0.1201(6) 1.1963(4) -0.1810(4) 0.0644 1.0000 Uani . . . . . . C12 C -0.3011(5) 0.7724(5) -0.3046(3) 0.0592 1.0000 Uani . . . . . . C13 C -0.2165(4) 0.9838(4) -0.2446(3) 0.0394 1.0000 Uani . . . . . . C14 C -0.1790(4) 0.9840(4) -0.3141(3) 0.0481 1.0000 Uani . . . . . . C15 C -0.2428(5) 0.9797(6) -0.3815(3) 0.0711 1.0000 Uani D U . . . . C16 C -0.3424(5) 0.9757(4) -0.3755(3) 0.0510 1.0000 Uani . . . . . . C17 C -0.3819(5) 0.9767(6) -0.3061(4) 0.0678 1.0000 Uani D U . . . . C18 C -0.3180(4) 0.9801(4) -0.2412(3) 0.0429 1.0000 Uani . . . . . . C19 C -0.1994(4) 0.9797(5) -0.4568(3) 0.0840 1.0000 Uani D U . . . . C20 C -0.1891(7) 0.8870(5) -0.4913(4) 0.0910 1.0000 Uani D U . . . . C21 C -0.2768(6) 0.9805(7) -0.5227(4) 0.0899 1.0000 Uani D U . . . . C22 C -0.0874(5) 1.0682(6) -0.4387(4) 0.0928 1.0000 Uani D U . . . . C23 C -0.4922(4) 0.9741(5) -0.3037(3) 0.0786 1.0000 Uani D U . . . . C24 C -0.4885(7) 1.0616(6) -0.3232(5) 0.0856 1.0000 Uani D U . . . . C25 C -0.5145(7) 0.9876(7) -0.2194(4) 0.0834 1.0000 Uani D U . . . . C26 C -0.5811(6) 0.8809(6) -0.3674(5) 0.0918 1.0000 Uani D U . . . . C27 C 0.0154(5) 1.3454(4) -0.0125(3) 0.0524 1.0000 Uani . . . . . . C28 C 0.1323(5) 1.4076(4) -0.0135(4) 0.0566 1.0000 Uani . . . . . . C29 C 0.1729(6) 1.5150(5) 0.0357(5) 0.0764 1.0000 Uani . . . . . . C30 C 0.2918(7) 1.5771(5) 0.0479(5) 0.0743 1.0000 Uani . . . . . . C31 C 0.3305(8) 1.6774(5) 0.1076(5) 0.0806 1.0000 Uani . . . . . . C32 C 0.4532(9) 1.7379(7) 0.1170(8) 0.1234 1.0000 Uani . . . . . . C33 C -0.2357(4) 0.6360(3) -0.2424(3) 0.0648 1.0000 Uani D U . . . . C34 C -0.3398(4) 0.5811(3) -0.2157(4) 0.0748 1.0000 Uani D U . . . . C35 C -0.3685(6) 0.4742(3) -0.2352(3) 0.0888 1.0000 Uani D U . . . . C36 C -0.4001(9) 0.4208(3) -0.3257(3) 0.1039 1.0000 Uani D U . . . . C37 C -0.4422(9) 0.3116(3) -0.3453(4) 0.1131 1.0000 Uani D U . . . . C38 C -0.4360(10) 0.2635(5) -0.4304(5) 0.1187 1.0000 Uani D U . . . . C101 C -0.3220(4) 0.7327(4) 0.0326(3) 0.0508 1.0000 Uani . . . . . . C102 C -0.3049(4) 0.6944(4) 0.0888(3) 0.0494 1.0000 Uani . . . . . . C103 C -0.2225(4) 0.7513(4) 0.1629(3) 0.0543 1.0000 Uani D . . . . . C104 C -0.2315(5) 0.6897(5) 0.2037(3) 0.0576 1.0000 Uani . . . . . . C105 C -0.3194(4) 0.5947(4) 0.1546(3) 0.0464 1.0000 Uani . . . . . . C106 C -0.3514(4) 0.5073(4) 0.1693(3) 0.0477 1.0000 Uani . . . . . . C107 C -0.4415(4) 0.4174(4) 0.1238(3) 0.0482 1.0000 Uani . . . . . . C108 C -0.4756(5) 0.3260(5) 0.1370(3) 0.0551 1.0000 Uani . . . . . . C109 C -0.5703(5) 0.2611(4) 0.0825(3) 0.0533 1.0000 Uani . . . . . . C110 C -0.5924(4) 0.3111(4) 0.0341(3) 0.0481 1.0000 Uani . . . . . . C111 C -0.4198(7) 0.2975(5) 0.1942(4) 0.0734 1.0000 Uani . . . . . . C112 C -0.1670(6) 0.7237(5) 0.2884(4) 0.0753 1.0000 Uani . . . . . . C113 C -0.2822(4) 0.5113(4) 0.2405(3) 0.0513 1.0000 Uani . . . . . . C114 C -0.1824(4) 0.5140(4) 0.2341(3) 0.0451 1.0000 Uani . . . . . . C115 C -0.1136(4) 0.5199(5) 0.2996(3) 0.0556 1.0000 Uani D U . . . . C116 C -0.1507(5) 0.5194(5) 0.3696(3) 0.0564 1.0000 Uani . . . . . . C117 C -0.2542(7) 0.5144(8) 0.3759(3) 0.0961 1.0000 Uani D U . . . . C118 C -0.3169(5) 0.5105(6) 0.3108(3) 0.0657 1.0000 Uani . . . . . . C119 C -0.2940(5) 0.5148(6) 0.4526(3) 0.1056 1.0000 Uani D U . . . . C120 C -0.3042(8) 0.6078(6) 0.4856(5) 0.1118 1.0000 Uani D U . . . . C121 C -0.2189(7) 0.5057(8) 0.5142(4) 0.1094 1.0000 Uani D U . . . . C122 C -0.4082(6) 0.4284(7) 0.4334(4) 0.1104 1.0000 Uani D U . . . . C123 C -0.0013(4) 0.5280(4) 0.2954(3) 0.0624 1.0000 Uani D U . . . . C124 C 0.0189(10) 0.5131(10) 0.2105(4) 0.0594 0.5000 Uani D U . . . . C125 C 0.0852(8) 0.6251(6) 0.3563(6) 0.0670 0.5000 Uani D U . . . . C126 C -0.0047(10) 0.4411(7) 0.3158(7) 0.0623 0.5000 Uani D U . . . . C127 C -0.6399(5) 0.1572(5) 0.0701(4) 0.0614 1.0000 Uani . . . . . . C128 C -0.6206(4) 0.0895(4) 0.0037(4) 0.0516 1.0000 Uani . . . . . . C129 C -0.6972(5) -0.0184(5) -0.0108(4) 0.0638 1.0000 Uani . . . . . . C130 C -0.6874(6) -0.0858(6) -0.0846(5) 0.0736 1.0000 Uani . . . . . . C131 C -0.7698(7) -0.1945(6) -0.1035(6) 0.0868 1.0000 Uani . . . . . . C132 C -0.7446(7) -0.2354(7) -0.0462(6) 0.0936 1.0000 Uani . . . . . . C133 C -0.1430(4) 0.8579(3) 0.1840(4) 0.0768 1.0000 Uani D U . . . . C134 C -0.1902(4) 0.9224(3) 0.2278(5) 0.0806 1.0000 Uani D U . . . . C135 C -0.1110(5) 1.0299(3) 0.2470(5) 0.0907 1.0000 Uani D U . . . . C136 C -0.1488(5) 1.0947(3) 0.3030(6) 0.0976 1.0000 Uani D U . . . . C137 C -0.0602(6) 1.2007(3) 0.3348(6) 0.1114 1.0000 Uani D U . . . . C138 C -0.0958(7) 1.2643(4) 0.3945(7) 0.1173 1.0000 Uani D U . . . . C224 C 0.0633(10) 0.6165(7) 0.2714(8) 0.0681 0.5000 Uani D U . . . . C225 C -0.0015(11) 0.4475(8) 0.2257(6) 0.0679 0.5000 Uani D U . . . . C226 C 0.0749(10) 0.5473(11) 0.3724(5) 0.0683 0.5000 Uani D U . . . . H11 H -0.0960 0.6975 -0.1046 0.0563 1.0000 Uiso . . . . . . H121 H -0.3501 0.8010 -0.2943 0.0853 1.0000 Uiso . . . . . . H122 H -0.3441 0.7036 -0.3233 0.0854 1.0000 Uiso . . . . . . H123 H -0.2665 0.7921 -0.3458 0.0855 1.0000 Uiso . . . . . . H141 H -0.1103 0.9872 -0.3159 0.0581 1.0000 Uiso . . . . . . H161 H -0.3857 0.9720 -0.4202 0.0630 1.0000 Uiso . . . . . . H181 H -0.3440 0.9800 -0.1945 0.0584 1.0000 Uiso . . . . . . H201 H -0.1772 0.8821 -0.5438 0.1310 1.0000 Uiso . . . . . . H202 H -0.2561 0.8329 -0.4919 0.1311 1.0000 Uiso . . . . . . H203 H -0.1269 0.8941 -0.4564 0.1311 1.0000 Uiso . . . . . . H211 H -0.2457 0.9839 -0.5682 0.1309 1.0000 Uiso . . . . . . H212 H -0.2941 1.0311 -0.5043 0.1310 1.0000 Uiso . . . . . . H213 H -0.3448 0.9182 -0.5401 0.1311 1.0000 Uiso . . . . . . H221 H -0.0557 1.0648 -0.4855 0.1310 1.0000 Uiso . . . . . . H222 H -0.0965 1.1262 -0.4239 0.1310 1.0000 Uiso . . . . . . H223 H -0.0396 1.0709 -0.3948 0.1311 1.0000 Uiso . . . . . . H241 H -0.5628 1.0559 -0.3246 0.1470 1.0000 Uiso . . . . . . H242 H -0.4726 1.0572 -0.3758 0.1472 1.0000 Uiso . . . . . . H243 H -0.4366 1.1202 -0.2829 0.1472 1.0000 Uiso . . . . . . H251 H -0.5344 1.0378 -0.2039 0.1442 1.0000 Uiso . . . . . . H252 H -0.4492 1.0014 -0.1825 0.1444 1.0000 Uiso . . . . . . H253 H -0.5750 0.9242 -0.2213 0.1443 1.0000 Uiso . . . . . . H261 H -0.6518 0.8771 -0.3623 0.1492 1.0000 Uiso . . . . . . H262 H -0.5697 0.8868 -0.4205 0.1491 1.0000 Uiso . . . . . . H263 H -0.5766 0.8278 -0.3617 0.1490 1.0000 Uiso . . . . . . H271 H -0.0315 1.3594 -0.0444 0.0673 1.0000 Uiso . . . . . . H272 H 0.0098 1.3646 0.0429 0.0671 1.0000 Uiso . . . . . . H281 H 0.1370 1.4022 -0.0683 0.0712 1.0000 Uiso . . . . . . H282 H 0.1789 1.3838 0.0075 0.0712 1.0000 Uiso . . . . . . H291 H 0.1345 1.5394 0.0086 0.0993 1.0000 Uiso . . . . . . H292 H 0.1560 1.5201 0.0897 0.0995 1.0000 Uiso . . . . . . H301 H 0.3082 1.5800 -0.0038 0.0994 1.0000 Uiso . . . . . . H302 H 0.3328 1.5480 0.0693 0.0993 1.0000 Uiso . . . . . . H311 H 0.2915 1.7078 0.0862 0.0990 1.0000 Uiso . . . . . . H312 H 0.3108 1.6734 0.1576 0.0993 1.0000 Uiso . . . . . . H321 H 0.4834 1.7946 0.1642 0.1850 1.0000 Uiso . . . . . . H322 H 0.4692 1.7565 0.0718 0.1852 1.0000 Uiso . . . . . . H323 H 0.4885 1.6984 0.1231 0.1851 1.0000 Uiso . . . . . . H331 H -0.2519 0.6166 -0.3018 0.0885 1.0000 Uiso . . . . . . H332 H -0.1803 0.6147 -0.2274 0.0881 1.0000 Uiso . . . . . . H341 H -0.4008 0.5865 -0.2459 0.0952 1.0000 Uiso . . . . . . H342 H -0.3317 0.6111 -0.1607 0.0952 1.0000 Uiso . . . . . . H351 H -0.4266 0.4418 -0.2118 0.1040 1.0000 Uiso . . . . . . H352 H -0.3023 0.4691 -0.2144 0.1046 1.0000 Uiso . . . . . . H361 H -0.4596 0.4327 -0.3476 0.1135 1.0000 Uiso . . . . . . H362 H -0.3379 0.4481 -0.3500 0.1133 1.0000 Uiso . . . . . . H371 H -0.5171 0.2856 -0.3371 0.1199 1.0000 Uiso . . . . . . H372 H -0.3973 0.3033 -0.3050 0.1204 1.0000 Uiso . . . . . . H381 H -0.4573 0.1980 -0.4389 0.1553 1.0000 Uiso . . . . . . H382 H -0.4851 0.2728 -0.4661 0.1553 1.0000 Uiso . . . . . . H383 H -0.3609 0.2989 -0.4352 0.1550 1.0000 Uiso . . . . . . H1011 H -0.2689 0.7979 0.0415 0.0616 1.0000 Uiso . . . . . . H1111 H -0.4370 0.2293 0.1710 0.1030 1.0000 Uiso . . . . . . H1112 H -0.4469 0.3056 0.2425 0.1030 1.0000 Uiso . . . . . . H1113 H -0.3433 0.3364 0.2068 0.1029 1.0000 Uiso . . . . . . H1121 H -0.1910 0.6687 0.3071 0.1024 1.0000 Uiso . . . . . . H1122 H -0.1815 0.7725 0.3226 0.1022 1.0000 Uiso . . . . . . H1123 H -0.0921 0.7481 0.2892 0.1025 1.0000 Uiso . . . . . . H1141 H -0.1608 0.5121 0.1855 0.0541 1.0000 Uiso . . . . . . H1161 H -0.1072 0.5210 0.4129 0.0614 1.0000 Uiso . . . . . . H1181 H -0.3843 0.5078 0.3139 0.0667 1.0000 Uiso . . . . . . H1201 H -0.3370 0.6099 0.5316 0.1562 1.0000 Uiso . . . . . . H1202 H -0.3540 0.6099 0.4444 0.1560 1.0000 Uiso . . . . . . H1203 H -0.2354 0.6649 0.4990 0.1559 1.0000 Uiso . . . . . . H1211 H -0.2487 0.5029 0.5613 0.1541 1.0000 Uiso . . . . . . H1212 H -0.1492 0.5633 0.5294 0.1542 1.0000 Uiso . . . . . . H1213 H -0.2109 0.4493 0.4911 0.1539 1.0000 Uiso . . . . . . H1221 H -0.4324 0.4282 0.4821 0.1540 1.0000 Uiso . . . . . . H1222 H -0.4589 0.4353 0.3982 0.1539 1.0000 Uiso . . . . . . H1223 H -0.4038 0.3712 0.4088 0.1540 1.0000 Uiso . . . . . . H1271 H -0.7165 0.1445 0.0549 0.0713 1.0000 Uiso . . . . . . H1272 H -0.6293 0.1459 0.1190 0.0713 1.0000 Uiso . . . . . . H1281 H -0.6342 0.1010 -0.0452 0.0634 1.0000 Uiso . . . . . . H1282 H -0.5447 0.1033 0.0160 0.0633 1.0000 Uiso . . . . . . H1291 H -0.7738 -0.0292 -0.0193 0.0773 1.0000 Uiso . . . . . . H1292 H -0.6792 -0.0328 0.0360 0.0774 1.0000 Uiso . . . . . . H1301 H -0.6980 -0.0659 -0.1307 0.0915 1.0000 Uiso . . . . . . H1302 H -0.6129 -0.0768 -0.0734 0.0913 1.0000 Uiso . . . . . . H1311 H -0.8421 -0.2002 -0.1047 0.1040 1.0000 Uiso . . . . . . H1312 H -0.7670 -0.2304 -0.1560 0.1042 1.0000 Uiso . . . . . . H1331 H -0.1307 0.8735 0.1324 0.0943 1.0000 Uiso . . . . . . H1332 H -0.0710 0.8772 0.2160 0.0947 1.0000 Uiso . . . . . . H1341 H -0.2576 0.9086 0.1934 0.0985 1.0000 Uiso . . . . . . H1342 H -0.2101 0.9071 0.2757 0.0979 1.0000 Uiso . . . . . . H1351 H -0.1073 1.0463 0.1993 0.1052 1.0000 Uiso . . . . . . H1352 H -0.0362 1.0455 0.2735 0.1059 1.0000 Uiso . . . . . . H1361 H -0.2166 1.0875 0.2736 0.1105 1.0000 Uiso . . . . . . H1362 H -0.1673 1.0689 0.3480 0.1103 1.0000 Uiso . . . . . . H1371 H -0.0514 1.2175 0.2890 0.1192 1.0000 Uiso . . . . . . H1372 H 0.0098 1.2065 0.3596 0.1187 1.0000 Uiso . . . . . . H1381 H -0.0575 1.3283 0.3979 0.1543 1.0000 Uiso . . . . . . H1382 H -0.1760 1.2391 0.3713 0.1542 1.0000 Uiso . . . . . . H1383 H -0.0890 1.2537 0.4439 0.1540 1.0000 Uiso . . . . . . H1321 H -0.7987 -0.3047 -0.0603 0.1197 1.0000 Uiso . . . . . . H1322 H -0.7451 -0.1988 0.0093 0.1197 1.0000 Uiso . . . . . . H1323 H -0.6693 -0.2304 -0.0449 0.1197 1.0000 Uiso . . . . . . H111 H -0.0998 1.2658 -0.1636 0.0799 1.0000 Uiso . . . . . . H112 H -0.2003 1.1561 -0.1998 0.0799 1.0000 Uiso . . . . . . H113 H -0.0846 1.1811 -0.2270 0.0799 1.0000 Uiso . . . . . . H1251 H 0.0824 0.6793 0.3396 0.0878 0.5000 Uiso . . . . . . H1252 H 0.0669 0.6323 0.4102 0.0878 0.5000 Uiso . . . . . . H1253 H 0.1586 0.6308 0.3589 0.0878 0.5000 Uiso . . . . . . H1241 H -0.0413 0.4471 0.1740 0.0844 0.5000 Uiso . . . . . . H1242 H 0.0121 0.5630 0.1913 0.0844 0.5000 Uiso . . . . . . H1243 H 0.0898 0.5153 0.2088 0.0844 0.5000 Uiso . . . . . . H1261 H -0.0158 0.4473 0.3712 0.0858 0.5000 Uiso . . . . . . H1262 H 0.0653 0.4383 0.3118 0.0858 0.5000 Uiso . . . . . . H1263 H -0.0666 0.3802 0.2773 0.0858 0.5000 Uiso . . . . . . H2241 H 0.0185 0.6072 0.2183 0.0892 0.5000 Uiso . . . . . . H2242 H 0.0747 0.6757 0.3114 0.0892 0.5000 Uiso . . . . . . H2243 H 0.1338 0.6185 0.2609 0.0892 0.5000 Uiso . . . . . . H2261 H 0.0724 0.6011 0.4175 0.0888 0.5000 Uiso . . . . . . H2262 H 0.1505 0.5687 0.3666 0.0888 0.5000 Uiso . . . . . . H2263 H 0.0482 0.4886 0.3881 0.0888 0.5000 Uiso . . . . . . H2251 H -0.0417 0.3843 0.2329 0.0888 0.5000 Uiso . . . . . . H2252 H -0.0414 0.4455 0.1744 0.0888 0.5000 Uiso . . . . . . H2253 H 0.0737 0.4610 0.2217 0.0888 0.5000 Uiso . . . . . . 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 0.0266(4) 0.0389(4) 0.0245(3) 0.0112(3) 0.0064(3) 0.0154(3) Zn2 0.0272(4) 0.0441(5) 0.0299(4) -0.0004(3) 0.0040(3) 0.0167(3) N1 0.038(2) 0.050(2) 0.0325(19) 0.0150(17) 0.0028(16) 0.0198(18) N2 0.0354(19) 0.051(2) 0.0314(18) 0.0154(17) 0.0066(15) 0.0213(18) N3 0.0337(19) 0.049(2) 0.041(2) 0.0007(18) 0.0022(17) 0.0191(18) N4 0.036(2) 0.057(3) 0.037(2) 0.0020(18) 0.0050(17) 0.0226(19) C1 0.045(3) 0.050(3) 0.042(2) 0.009(2) 0.008(2) 0.027(2) C2 0.038(2) 0.050(3) 0.033(2) 0.008(2) 0.0061(19) 0.021(2) C3 0.041(2) 0.054(3) 0.033(2) 0.007(2) 0.0066(19) 0.023(2) C4 0.041(2) 0.056(3) 0.036(2) 0.011(2) 0.008(2) 0.022(2) C5 0.033(2) 0.054(3) 0.027(2) 0.0106(19) 0.0062(18) 0.021(2) C6 0.030(2) 0.054(3) 0.026(2) 0.015(2) 0.0046(18) 0.017(2) C7 0.040(2) 0.052(3) 0.036(2) 0.022(2) 0.008(2) 0.023(2) C8 0.047(3) 0.055(3) 0.041(2) 0.020(2) 0.008(2) 0.025(2) C9 0.043(2) 0.054(3) 0.049(3) 0.022(2) 0.013(2) 0.028(2) C10 0.040(2) 0.051(3) 0.041(2) 0.014(2) 0.012(2) 0.026(2) C11 0.083(4) 0.053(3) 0.052(3) 0.025(3) -0.008(3) 0.027(3) C12 0.057(3) 0.060(3) 0.043(3) 0.005(2) -0.011(3) 0.023(3) C13 0.038(2) 0.055(3) 0.029(2) 0.019(2) 0.0065(19) 0.023(2) C14 0.036(2) 0.072(4) 0.035(2) 0.023(2) 0.013(2) 0.020(2) C15 0.057(2) 0.117(3) 0.0364(19) 0.040(2) 0.0105(18) 0.030(2) C16 0.052(3) 0.067(4) 0.036(3) 0.026(3) 0.003(2) 0.026(3) C17 0.071(2) 0.114(3) 0.060(2) 0.047(2) 0.020(2) 0.069(2) C18 0.043(3) 0.061(3) 0.037(2) 0.026(2) 0.016(2) 0.028(2) C19 0.066(2) 0.127(3) 0.0415(17) 0.0346(19) 0.0151(16) 0.025(2) C20 0.071(2) 0.130(3) 0.048(2) 0.027(2) 0.017(2) 0.027(2) C21 0.071(2) 0.132(4) 0.045(2) 0.035(2) 0.011(2) 0.025(3) C22 0.072(2) 0.131(4) 0.046(2) 0.033(2) 0.016(2) 0.019(2) C23 0.074(2) 0.124(3) 0.070(2) 0.040(2) 0.0174(18) 0.070(2) C24 0.083(3) 0.124(3) 0.075(3) 0.041(2) 0.014(2) 0.068(3) C25 0.075(3) 0.129(4) 0.072(2) 0.038(3) 0.020(2) 0.068(3) C26 0.078(3) 0.132(4) 0.079(3) 0.033(3) 0.017(2) 0.063(3) C27 0.052(3) 0.060(3) 0.055(3) 0.018(3) 0.011(2) 0.037(3) C28 0.055(3) 0.047(3) 0.074(4) 0.019(3) 0.017(3) 0.031(3) C29 0.076(4) 0.054(4) 0.114(6) 0.030(4) 0.027(4) 0.041(4) C30 0.089(5) 0.061(4) 0.095(5) 0.037(4) 0.057(4) 0.043(4) C31 0.108(6) 0.057(4) 0.083(5) 0.021(4) 0.045(5) 0.042(4) C32 0.116(8) 0.078(5) 0.169(10) 0.029(6) 0.098(8) 0.035(5) C33 0.077(3) 0.064(2) 0.064(2) 0.016(2) 0.019(2) 0.044(2) C34 0.083(3) 0.067(2) 0.071(2) 0.0164(19) 0.020(2) 0.036(2) C35 0.096(3) 0.069(2) 0.084(2) 0.016(2) 0.020(2) 0.029(2) C36 0.107(3) 0.077(2) 0.090(3) 0.013(2) 0.019(2) 0.020(2) C37 0.115(3) 0.080(3) 0.099(3) 0.012(2) 0.016(3) 0.017(3) C38 0.119(4) 0.083(3) 0.101(3) 0.010(3) 0.017(3) 0.014(3) C101 0.038(2) 0.054(3) 0.055(3) 0.008(2) 0.011(2) 0.023(2) C102 0.034(2) 0.050(3) 0.056(3) 0.001(2) 0.008(2) 0.023(2) C103 0.038(3) 0.058(3) 0.059(3) 0.001(3) -0.001(2) 0.028(2) C104 0.044(3) 0.061(3) 0.050(3) -0.007(3) -0.009(2) 0.028(3) C105 0.036(2) 0.055(3) 0.037(2) -0.002(2) -0.002(2) 0.024(2) C106 0.041(3) 0.065(4) 0.029(2) 0.004(2) 0.005(2) 0.024(3) C107 0.038(2) 0.059(3) 0.036(2) 0.006(2) 0.004(2) 0.019(2) C108 0.048(3) 0.068(4) 0.037(3) 0.010(2) 0.012(2) 0.020(3) C109 0.046(3) 0.066(3) 0.043(3) 0.014(2) 0.018(2) 0.023(3) C110 0.037(2) 0.058(3) 0.043(3) 0.006(2) 0.013(2) 0.023(2) C111 0.085(5) 0.068(4) 0.046(3) 0.020(3) 0.003(3) 0.019(4) C112 0.077(4) 0.060(4) 0.061(4) -0.011(3) -0.028(3) 0.034(3) C113 0.042(3) 0.066(4) 0.031(2) 0.006(2) 0.002(2) 0.019(3) C114 0.051(3) 0.055(3) 0.034(2) 0.013(2) 0.010(2) 0.029(3) C115 0.062(2) 0.077(3) 0.047(2) 0.0263(19) 0.0145(18) 0.046(2) C116 0.053(3) 0.072(4) 0.030(2) 0.008(2) 0.001(2) 0.024(3) C117 0.073(3) 0.155(5) 0.040(2) 0.017(3) 0.019(2) 0.045(3) C118 0.046(3) 0.101(5) 0.026(2) 0.000(3) 0.003(2) 0.027(3) C119 0.081(2) 0.161(4) 0.0426(19) 0.017(2) 0.0201(19) 0.039(3) C120 0.086(3) 0.163(5) 0.050(2) 0.011(3) 0.019(2) 0.039(3) C121 0.085(3) 0.164(5) 0.045(2) 0.019(3) 0.018(2) 0.037(3) C122 0.085(3) 0.163(5) 0.046(2) 0.019(3) 0.019(2) 0.035(3) C123 0.063(2) 0.085(3) 0.0540(19) 0.0235(18) 0.0121(16) 0.048(2) C124 0.061(3) 0.084(3) 0.053(2) 0.026(2) 0.012(2) 0.050(3) C125 0.063(3) 0.088(3) 0.057(3) 0.020(2) 0.013(2) 0.045(3) C126 0.064(3) 0.085(3) 0.053(3) 0.024(2) 0.013(2) 0.048(3) C127 0.051(3) 0.076(4) 0.052(3) 0.027(3) 0.020(3) 0.021(3) C128 0.046(3) 0.058(3) 0.056(3) 0.032(3) 0.014(2) 0.022(3) C129 0.059(3) 0.058(4) 0.076(4) 0.032(3) 0.020(3) 0.022(3) C130 0.068(4) 0.082(5) 0.087(5) 0.035(4) 0.028(4) 0.043(4) C131 0.075(5) 0.066(4) 0.109(6) 0.013(4) 0.019(4) 0.035(4) C132 0.078(5) 0.082(5) 0.121(7) 0.037(5) 0.036(5) 0.034(4) C133 0.064(3) 0.064(3) 0.097(3) 0.010(2) -0.001(2) 0.038(2) C134 0.069(2) 0.064(2) 0.101(3) 0.010(2) 0.004(2) 0.0382(19) C135 0.076(2) 0.068(2) 0.109(3) 0.008(2) 0.010(2) 0.033(2) C136 0.083(3) 0.070(2) 0.117(3) 0.006(2) 0.015(2) 0.032(2) C137 0.093(3) 0.076(3) 0.126(3) 0.004(3) 0.017(3) 0.025(2) C138 0.097(3) 0.079(3) 0.130(4) 0.001(3) 0.019(3) 0.023(3) C224 0.066(3) 0.087(3) 0.058(3) 0.024(2) 0.011(2) 0.043(3) C225 0.066(3) 0.088(3) 0.057(3) 0.020(2) 0.013(2) 0.046(3) C226 0.066(3) 0.089(3) 0.057(3) 0.024(2) 0.009(2) 0.044(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3009(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zn1 . N2 2_575 2.058(4) yes Zn1 . N1 2_575 2.048(4) yes Zn1 . N1 . 2.048(4) yes Zn1 . N2 . 2.058(4) yes Zn2 . N4 2_465 2.055(5) yes Zn2 . N3 2_465 2.035(4) yes Zn2 . N3 . 2.035(4) yes Zn2 . N4 . 2.055(5) yes N1 . C7 . 1.381(6) yes N1 . C10 . 1.353(6) yes N2 . C2 . 1.367(7) yes N2 . C5 . 1.372(6) yes N3 . C102 . 1.373(7) yes N3 . C105 . 1.386(7) yes N4 . C107 . 1.378(7) yes N4 . C110 . 1.373(7) yes C1 . C10 2_575 1.402(7) yes C1 . C2 . 1.374(7) yes C1 . H11 . 0.945 no C2 . C3 . 1.440(7) yes C3 . C4 . 1.365(8) yes C3 . C33 . 1.528(7) yes C4 . C5 . 1.479(7) yes C4 . C12 . 1.515(7) yes C5 . C6 . 1.392(7) yes C6 . C7 . 1.406(7) yes C6 . C13 . 1.503(6) yes C7 . C8 . 1.468(7) yes C8 . C9 . 1.355(7) yes C8 . C11 . 1.496(7) yes C9 . C10 . 1.443(7) yes C9 . C27 . 1.496(8) yes C11 . H111 . 0.991 no C11 . H112 . 0.992 no C11 . H113 . 1.019 no C12 . H121 . 0.979 no C12 . H122 . 0.959 no C12 . H123 . 0.967 no C13 . C14 . 1.387(6) yes C13 . C18 . 1.394(7) yes C14 . C15 . 1.406(8) yes C14 . H141 . 0.939 no C15 . C16 . 1.373(8) yes C15 . C19 . 1.520(2) yes C16 . C17 . 1.397(8) yes C16 . H161 . 0.935 no C17 . C18 . 1.380(7) yes C17 . C23 . 1.521(2) yes C18 . H181 . 0.936 no C19 . C20 . 1.540(2) yes C19 . C21 . 1.540(2) yes C19 . C22 . 1.539(2) yes C20 . H201 . 0.955 no C20 . H202 . 0.970 no C20 . H203 . 0.970 no C21 . H211 . 0.956 no C21 . H212 . 0.938 no C21 . H213 . 0.993 no C22 . H221 . 0.976 no C22 . H222 . 0.974 no C22 . H223 . 0.967 no C23 . C24 . 1.540(2) yes C23 . C25 . 1.539(2) yes C23 . C26 . 1.538(2) yes C24 . H241 . 0.995 no C24 . H242 . 0.975 no C24 . H243 . 0.952 no C25 . H251 . 0.950 no C25 . H252 . 0.981 no C25 . H253 . 1.007 no C26 . H261 . 0.972 no C26 . H262 . 1.000 no C26 . H263 . 0.926 no C27 . C28 . 1.512(8) yes C27 . H271 . 0.972 no C27 . H272 . 0.975 no C28 . C29 . 1.546(9) yes C28 . H281 . 0.971 no C28 . H282 . 0.982 no C29 . C30 . 1.485(11) yes C29 . H291 . 0.963 no C29 . H292 . 1.001 no C30 . C31 . 1.519(10) yes C30 . H301 . 0.979 no C30 . H302 . 0.998 no C31 . C32 . 1.532(13) yes C31 . H311 . 0.993 no C31 . H312 . 0.967 no C32 . H321 . 0.965 no C32 . H322 . 0.949 no C32 . H323 . 0.983 no C33 . C34 . 1.539(2) yes C33 . H331 . 0.999 no C33 . H332 . 1.017 no C34 . C35 . 1.539(2) yes C34 . H341 . 1.018 no C34 . H342 . 0.945 no C35 . C36 . 1.538(2) yes C35 . H351 . 0.959 no C35 . H352 . 1.010 no C36 . C37 . 1.540(2) yes C36 . H361 . 1.002 no C36 . H362 . 0.986 no C37 . C38 . 1.538(2) yes C37 . H371 . 0.985 no C37 . H372 . 0.992 no C38 . H381 . 0.940 no C38 . H382 . 0.986 no C38 . H383 . 0.980 no C101 . C110 2_465 1.392(7) yes C101 . C102 . 1.377(8) yes C101 . H1011 . 0.960 no C102 . C103 . 1.453(7) yes C103 . C104 . 1.368(9) yes C103 . C133 . 1.525(8) yes C104 . C105 . 1.462(8) yes C104 . C112 . 1.521(8) yes C105 . C106 . 1.409(8) yes C106 . C107 . 1.415(7) yes C106 . C113 . 1.504(7) yes C107 . C108 . 1.452(9) yes C108 . C109 . 1.361(8) yes C108 . C111 . 1.521(10) yes C109 . C110 . 1.438(8) yes C109 . C127 . 1.490(9) yes C111 . H1111 . 0.985 no C111 . H1112 . 0.969 no C111 . H1113 . 0.946 no C112 . H1121 . 0.979 no C112 . H1122 . 0.967 no C112 . H1123 . 0.941 no C113 . C114 . 1.384(8) yes C113 . C118 . 1.385(8) yes C114 . C115 . 1.408(7) yes C114 . H1141 . 0.940 no C115 . C116 . 1.394(8) yes C115 . C123 . 1.521(2) yes C116 . C117 . 1.422(10) yes C116 . H1161 . 0.932 no C117 . C118 . 1.369(10) yes C117 . C119 . 1.521(2) yes C118 . H1181 . 0.926 no C119 . C120 . 1.540(2) yes C119 . C121 . 1.540(2) yes C119 . C122 . 1.540(2) yes C120 . H1201 . 0.971 no C120 . H1202 . 0.989 no C120 . H1203 . 0.961 no C121 . H1211 . 0.972 no C121 . H1212 . 0.970 no C121 . H1213 . 0.955 no C122 . H1221 . 0.959 no C122 . H1222 . 0.970 no C122 . H1223 . 0.945 no C123 . C124 . 1.539(2) yes C123 . C125 . 1.539(2) yes C123 . C126 . 1.541(2) yes C123 . C224 . 1.541(2) yes C123 . C225 . 1.540(2) yes C123 . C226 . 1.540(2) yes C124 . C224 . 1.553(18) yes C124 . C225 . 1.101(18) yes C124 . H1241 . 1.023 no C124 . H1242 . 1.001 no C124 . H1243 . 0.975 no C124 . H2252 . 1.035 no C125 . C224 . 1.482(17) yes C125 . C226 . 1.329(19) yes C125 . H1251 . 1.021 no C125 . H1252 . 1.005 no C125 . H1253 . 0.981 no C125 . H2261 . 1.262 no C126 . C225 . 1.647(17) yes C126 . C226 . 1.575(18) yes C126 . H1261 . 1.001 no C126 . H1262 . 1.000 no C126 . H1263 . 1.003 no C126 . H2263 . 1.278 no C127 . C128 . 1.511(9) yes C127 . H1271 . 0.994 no C127 . H1272 . 0.956 no C128 . C129 . 1.553(8) yes C128 . H1281 . 0.965 no C128 . H1282 . 0.974 no C129 . C130 . 1.525(11) yes C129 . H1291 . 0.995 no C129 . H1292 . 0.972 no C130 . C131 . 1.566(11) yes C130 . H1301 . 0.988 no C130 . H1302 . 0.979 no C131 . C132 . 1.462(14) yes C131 . H1311 . 0.967 no C131 . H1312 . 0.975 no C132 . H1321 . 0.998 no C132 . H1322 . 1.012 no C132 . H1323 . 1.013 no C133 . C134 . 1.538(2) yes C133 . H1331 . 1.032 no C133 . H1332 . 0.986 no C134 . C135 . 1.540(2) yes C134 . H1341 . 0.980 no C134 . H1342 . 0.985 no C135 . C136 . 1.538(2) yes C135 . H1351 . 0.963 no C135 . H1352 . 1.002 no C136 . C137 . 1.539(2) yes C136 . H1361 . 0.987 no C136 . H1362 . 1.010 no C137 . C138 . 1.540(2) yes C137 . H1371 . 0.935 no C137 . H1372 . 0.991 no C138 . H1381 . 0.929 no C138 . H1382 . 1.015 no C138 . H1383 . 0.952 no C224 . H2241 . 1.031 no C224 . H2242 . 0.970 no C224 . H2243 . 1.002 no C225 . H1241 . 1.037 no C225 . H2251 . 0.993 no C225 . H2252 . 1.020 no C225 . H2253 . 0.987 no C226 . H2261 . 1.030 no C226 . H2262 . 0.982 no C226 . H2263 . 0.998 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N2 2_575 Zn1 . N1 2_575 87.17(16) yes N2 2_575 Zn1 . N1 . 92.83(16) yes N1 2_575 Zn1 . N1 . 179.994 yes N2 2_575 Zn1 . N2 . 179.994 yes N1 2_575 Zn1 . N2 . 92.83(16) yes N1 . Zn1 . N2 . 87.17(16) yes N4 2_465 Zn2 . N3 2_465 87.96(18) yes N4 2_465 Zn2 . N3 . 92.04(18) yes N3 2_465 Zn2 . N3 . 179.994 yes N4 2_465 Zn2 . N4 . 179.994 yes N3 2_465 Zn2 . N4 . 92.04(18) yes N3 . Zn2 . N4 . 87.96(18) yes Zn1 . N1 . C7 . 129.7(3) yes Zn1 . N1 . C10 . 123.7(3) yes C7 . N1 . C10 . 106.6(4) yes Zn1 . N2 . C2 . 123.3(3) yes Zn1 . N2 . C5 . 128.6(3) yes C2 . N2 . C5 . 107.8(4) yes Zn2 . N3 . C102 . 124.3(4) yes Zn2 . N3 . C105 . 129.0(4) yes C102 . N3 . C105 . 106.4(4) yes Zn2 . N4 . C107 . 129.0(4) yes Zn2 . N4 . C110 . 124.4(4) yes C107 . N4 . C110 . 106.1(5) yes C10 2_575 C1 . C2 . 128.3(5) yes C10 2_575 C1 . H11 . 116.7 no C2 . C1 . H11 . 115.0 no C1 . C2 . N2 . 125.9(4) yes C1 . C2 . C3 . 123.6(5) yes N2 . C2 . C3 . 110.4(4) yes C2 . C3 . C4 . 106.7(5) yes C2 . C3 . C33 . 124.2(5) yes C4 . C3 . C33 . 129.0(5) yes C3 . C4 . C5 . 107.1(4) yes C3 . C4 . C12 . 122.9(5) yes C5 . C4 . C12 . 129.9(5) yes C4 . C5 . N2 . 108.0(4) yes C4 . C5 . C6 . 127.0(4) yes N2 . C5 . C6 . 125.0(4) yes C5 . C6 . C7 . 125.6(4) yes C5 . C6 . C13 . 117.6(4) yes C7 . C6 . C13 . 116.8(4) yes C6 . C7 . N1 . 123.5(4) yes C6 . C7 . C8 . 127.8(4) yes N1 . C7 . C8 . 108.7(4) yes C7 . C8 . C9 . 106.9(4) yes C7 . C8 . C11 . 129.3(5) yes C9 . C8 . C11 . 123.7(5) yes C8 . C9 . C10 . 106.5(5) yes C8 . C9 . C27 . 128.7(5) yes C10 . C9 . C27 . 124.8(5) yes C9 . C10 . C1 2_575 122.9(5) yes C9 . C10 . N1 . 111.2(4) yes C1 2_575 C10 . N1 . 125.9(5) yes C8 . C11 . H111 . 110.0 no C8 . C11 . H112 . 110.1 no H111 . C11 . H112 . 110.9 no C8 . C11 . H113 . 108.5 no H111 . C11 . H113 . 108.7 no H112 . C11 . H113 . 108.6 no C4 . C12 . H121 . 110.8 no C4 . C12 . H122 . 110.8 no H121 . C12 . H122 . 108.1 no C4 . C12 . H123 . 110.0 no H121 . C12 . H123 . 107.6 no H122 . C12 . H123 . 109.5 no C6 . C13 . C14 . 120.8(4) yes C6 . C13 . C18 . 119.5(4) yes C14 . C13 . C18 . 119.7(4) yes C13 . C14 . C15 . 120.7(5) yes C13 . C14 . H141 . 119.3 no C15 . C14 . H141 . 120.0 no C14 . C15 . C16 . 117.6(4) yes C14 . C15 . C19 . 119.3(5) yes C16 . C15 . C19 . 123.1(5) yes C15 . C16 . C17 . 123.2(5) yes C15 . C16 . H161 . 118.1 no C17 . C16 . H161 . 118.7 no C16 . C17 . C18 . 118.0(4) yes C16 . C17 . C23 . 120.0(5) yes C18 . C17 . C23 . 122.1(5) yes C13 . C18 . C17 . 120.9(4) yes C13 . C18 . H181 . 120.4 no C17 . C18 . H181 . 118.7 no C15 . C19 . C20 . 109.8(5) yes C15 . C19 . C21 . 112.2(5) yes C20 . C19 . C21 . 106.2(6) yes C15 . C19 . C22 . 110.5(5) yes C20 . C19 . C22 . 109.5(6) yes C21 . C19 . C22 . 108.4(6) yes C19 . C20 . H201 . 107.9 no C19 . C20 . H202 . 108.0 no H201 . C20 . H202 . 111.6 no C19 . C20 . H203 . 106.5 no H201 . C20 . H203 . 111.1 no H202 . C20 . H203 . 111.6 no C19 . C21 . H211 . 110.4 no C19 . C21 . H212 . 111.7 no H211 . C21 . H212 . 110.8 no C19 . C21 . H213 . 107.9 no H211 . C21 . H213 . 106.9 no H212 . C21 . H213 . 109.0 no C19 . C22 . H221 . 110.7 no C19 . C22 . H222 . 108.9 no H221 . C22 . H222 . 108.7 no C19 . C22 . H223 . 109.1 no H221 . C22 . H223 . 110.1 no H222 . C22 . H223 . 109.3 no C17 . C23 . C24 . 107.7(5) yes C17 . C23 . C25 . 111.7(5) yes C24 . C23 . C25 . 105.5(6) yes C17 . C23 . C26 . 109.3(5) yes C24 . C23 . C26 . 109.1(6) yes C25 . C23 . C26 . 113.4(6) yes C23 . C24 . H241 . 106.0 no C23 . C24 . H242 . 108.7 no H241 . C24 . H242 . 109.3 no C23 . C24 . H243 . 110.6 no H241 . C24 . H243 . 109.7 no H242 . C24 . H243 . 112.4 no C23 . C25 . H251 . 110.1 no C23 . C25 . H252 . 108.8 no H251 . C25 . H252 . 111.6 no C23 . C25 . H253 . 107.1 no H251 . C25 . H253 . 111.2 no H252 . C25 . H253 . 107.9 no C23 . C26 . H261 . 108.6 no C23 . C26 . H262 . 107.1 no H261 . C26 . H262 . 107.9 no C23 . C26 . H263 . 110.2 no H261 . C26 . H263 . 111.3 no H262 . C26 . H263 . 111.6 no C9 . C27 . C28 . 114.0(4) yes C9 . C27 . H271 . 110.1 no C28 . C27 . H271 . 108.4 no C9 . C27 . H272 . 108.7 no C28 . C27 . H272 . 106.2 no H271 . C27 . H272 . 109.4 no C27 . C28 . C29 . 112.1(5) yes C27 . C28 . H281 . 108.5 no C29 . C28 . H281 . 108.5 no C27 . C28 . H282 . 109.2 no C29 . C28 . H282 . 110.0 no H281 . C28 . H282 . 108.5 no C28 . C29 . C30 . 114.5(6) yes C28 . C29 . H291 . 108.2 no C30 . C29 . H291 . 108.4 no C28 . C29 . H292 . 109.1 no C30 . C29 . H292 . 107.5 no H291 . C29 . H292 . 109.1 no C29 . C30 . C31 . 112.2(6) yes C29 . C30 . H301 . 108.6 no C31 . C30 . H301 . 111.2 no C29 . C30 . H302 . 109.5 no C31 . C30 . H302 . 107.0 no H301 . C30 . H302 . 108.2 no C30 . C31 . C32 . 109.7(6) yes C30 . C31 . H311 . 107.8 no C32 . C31 . H311 . 108.9 no C30 . C31 . H312 . 110.3 no C32 . C31 . H312 . 112.9 no H311 . C31 . H312 . 107.2 no C31 . C32 . H321 . 111.1 no C31 . C32 . H322 . 111.9 no H321 . C32 . H322 . 109.5 no C31 . C32 . H323 . 107.8 no H321 . C32 . H323 . 107.7 no H322 . C32 . H323 . 108.7 no C3 . C33 . C34 . 111.27(10) yes C3 . C33 . H331 . 110.6 no C34 . C33 . H331 . 109.5 no C3 . C33 . H332 . 111.0 no C34 . C33 . H332 . 108.0 no H331 . C33 . H332 . 106.3 no C33 . C34 . C35 . 111.43(11) yes C33 . C34 . H341 . 106.6 no C35 . C34 . H341 . 109.8 no C33 . C34 . H342 . 110.1 no C35 . C34 . H342 . 111.0 no H341 . C34 . H342 . 107.8 no C34 . C35 . C36 . 111.33(10) yes C34 . C35 . H351 . 111.9 no C36 . C35 . H351 . 109.3 no C34 . C35 . H352 . 109.7 no C36 . C35 . H352 . 105.9 no H351 . C35 . H352 . 108.5 no C35 . C36 . C37 . 111.29(11) yes C35 . C36 . H361 . 106.3 no C37 . C36 . H361 . 109.5 no C35 . C36 . H362 . 110.4 no C37 . C36 . H362 . 111.2 no H361 . C36 . H362 . 107.9 no C36 . C37 . C38 . 111.27(10) yes C36 . C37 . H371 . 106.5 no C38 . C37 . H371 . 112.6 no C36 . C37 . H372 . 107.3 no C38 . C37 . H372 . 111.4 no H371 . C37 . H372 . 107.5 no C37 . C38 . H381 . 108.9 no C37 . C38 . H382 . 105.7 no H381 . C38 . H382 . 112.7 no C37 . C38 . H383 . 107.2 no H381 . C38 . H383 . 112.8 no H382 . C38 . H383 . 109.1 no C110 2_465 C101 . C102 . 127.8(5) yes C110 2_465 C101 . H1011 . 116.8 no C102 . C101 . H1011 . 115.4 no C101 . C102 . N3 . 126.1(5) yes C101 . C102 . C103 . 123.2(5) yes N3 . C102 . C103 . 110.6(5) yes C102 . C103 . C104 . 106.4(5) yes C102 . C103 . C133 . 123.3(6) yes C104 . C103 . C133 . 130.3(5) yes C103 . C104 . C105 . 107.2(5) yes C103 . C104 . C112 . 122.7(6) yes C105 . C104 . C112 . 129.8(6) yes C104 . C105 . N3 . 109.3(5) yes C104 . C105 . C106 . 127.3(5) yes N3 . C105 . C106 . 123.3(4) yes C105 . C106 . C107 . 126.3(5) yes C105 . C106 . C113 . 116.0(5) yes C107 . C106 . C113 . 117.7(5) yes C106 . C107 . N4 . 123.0(5) yes C106 . C107 . C108 . 127.5(5) yes N4 . C107 . C108 . 109.5(5) yes C107 . C108 . C109 . 107.1(5) yes C107 . C108 . C111 . 130.6(5) yes C109 . C108 . C111 . 122.1(6) yes C108 . C109 . C110 . 106.6(5) yes C108 . C109 . C127 . 129.2(6) yes C110 . C109 . C127 . 124.2(5) yes C109 . C110 . C101 2_465 124.2(5) yes C109 . C110 . N4 . 110.7(5) yes C101 2_465 C110 . N4 . 125.0(5) yes C108 . C111 . H1111 . 110.8 no C108 . C111 . H1112 . 108.4 no H1111 . C111 . H1112 . 108.1 no C108 . C111 . H1113 . 110.8 no H1111 . C111 . H1113 . 109.2 no H1112 . C111 . H1113 . 109.5 no C104 . C112 . H1121 . 108.5 no C104 . C112 . H1122 . 109.5 no H1121 . C112 . H1122 . 108.8 no C104 . C112 . H1123 . 109.9 no H1121 . C112 . H1123 . 109.4 no H1122 . C112 . H1123 . 110.8 no C106 . C113 . C114 . 118.4(5) yes C106 . C113 . C118 . 121.7(5) yes C114 . C113 . C118 . 119.9(5) yes C113 . C114 . C115 . 120.6(4) yes C113 . C114 . H1141 . 119.3 no C115 . C114 . H1141 . 120.1 no C114 . C115 . C116 . 118.1(4) yes C114 . C115 . C123 . 121.6(5) yes C116 . C115 . C123 . 120.3(5) yes C115 . C116 . C117 . 121.5(5) yes C115 . C116 . H1161 . 119.2 no C117 . C116 . H1161 . 119.3 no C116 . C117 . C118 . 117.9(5) yes C116 . C117 . C119 . 121.4(7) yes C118 . C117 . C119 . 120.6(7) yes C113 . C118 . C117 . 122.0(6) yes C113 . C118 . H1181 . 118.7 no C117 . C118 . H1181 . 119.3 no C117 . C119 . C120 . 108.0(6) yes C117 . C119 . C121 . 112.2(6) yes C120 . C119 . C121 . 111.7(7) yes C117 . C119 . C122 . 109.0(6) yes C120 . C119 . C122 . 108.0(7) yes C121 . C119 . C122 . 107.8(7) yes C119 . C120 . H1201 . 112.8 no C119 . C120 . H1202 . 108.6 no H1201 . C120 . H1202 . 105.6 no C119 . C120 . H1203 . 112.4 no H1201 . C120 . H1203 . 109.2 no H1202 . C120 . H1203 . 107.9 no C119 . C121 . H1211 . 110.0 no C119 . C121 . H1212 . 107.0 no H1211 . C121 . H1212 . 108.5 no C119 . C121 . H1213 . 109.8 no H1211 . C121 . H1213 . 110.6 no H1212 . C121 . H1213 . 110.8 no C119 . C122 . H1221 . 108.6 no C119 . C122 . H1222 . 109.5 no H1221 . C122 . H1222 . 108.4 no C119 . C122 . H1223 . 108.5 no H1221 . C122 . H1223 . 111.2 no H1222 . C122 . H1223 . 110.5 no C115 . C123 . C124 . 112.8(6) yes C115 . C123 . C125 . 108.8(6) yes C124 . C123 . C125 . 112.8(8) yes C115 . C123 . C126 . 103.9(6) yes C124 . C123 . C126 . 105.7(7) yes C125 . C123 . C126 . 112.6(8) yes C115 . C123 . C224 . 108.0(6) yes C126 . C123 . C224 . 148.1(7) yes C115 . C123 . C225 . 114.1(6) yes C125 . C123 . C225 . 136.4(8) yes C224 . C123 . C225 . 100.5(8) yes C115 . C123 . C226 . 118.5(6) yes C124 . C123 . C226 . 128.8(7) yes C224 . C123 . C226 . 102.8(8) yes C225 . C123 . C226 . 110.6(8) yes C224 . C124 . C225 . 125.4(6) yes C123 . C124 . H1241 . 107.8 no C224 . C124 . H1241 . 154.3 no C123 . C124 . H1242 . 109.1 no C225 . C124 . H1242 . 162.1 no H1241 . C124 . H1242 . 107.6 no C123 . C124 . H1243 . 111.2 no C224 . C124 . H1243 . 96.0 no H1241 . C124 . H1243 . 109.6 no H1242 . C124 . H1243 . 111.4 no C123 . C124 . H2252 . 107.1 no C224 . C124 . H2252 . 154.9 no H1242 . C124 . H2252 . 109.0 no H1243 . C124 . H2252 . 108.9 no C224 . C125 . C226 . 117.8(7) yes C123 . C125 . H1251 . 108.4 no C226 . C125 . H1251 . 172.2 no C123 . C125 . H1252 . 109.6 no C224 . C125 . H1252 . 153.0 no C226 . C125 . H1252 . 73.5 no H1251 . C125 . H1252 . 107.4 no C123 . C125 . H1253 . 111.4 no C224 . C125 . H1253 . 96.2 no C226 . C125 . H1253 . 77.1 no H1251 . C125 . H1253 . 109.3 no H1252 . C125 . H1253 . 110.6 no C123 . C125 . H2261 . 96.9 no C224 . C125 . H2261 . 158.0 no H1251 . C125 . H2261 . 134.7 no C225 . C126 . C226 . 103.6(7) yes C123 . C126 . H1261 . 109.7 no C225 . C126 . H1261 . 165.8 no C123 . C126 . H1262 . 110.0 no C225 . C126 . H1262 . 82.5 no C226 . C126 . H1262 . 82.5 no H1261 . C126 . H1262 . 109.4 no C123 . C126 . H1263 . 109.3 no C226 . C126 . H1263 . 166.6 no H1261 . C126 . H1263 . 109.2 no H1262 . C126 . H1263 . 109.2 no C123 . C126 . H2263 . 96.1 no C225 . C126 . H2263 . 140.7 no H1262 . C126 . H2263 . 80.1 no H1263 . C126 . H2263 . 146.9 no C109 . C127 . C128 . 113.7(4) yes C109 . C127 . H1271 . 106.1 no C128 . C127 . H1271 . 107.5 no C109 . C127 . H1272 . 109.4 no C128 . C127 . H1272 . 110.6 no H1271 . C127 . H1272 . 109.3 no C127 . C128 . C129 . 113.0(5) yes C127 . C128 . H1281 . 108.8 no C129 . C128 . H1281 . 107.4 no C127 . C128 . H1282 . 108.9 no C129 . C128 . H1282 . 110.2 no H1281 . C128 . H1282 . 108.5 no C128 . C129 . C130 . 112.5(5) yes C128 . C129 . H1291 . 108.3 no C130 . C129 . H1291 . 107.5 no C128 . C129 . H1292 . 108.3 no C130 . C129 . H1292 . 109.8 no H1291 . C129 . H1292 . 110.4 no C129 . C130 . C131 . 113.2(6) yes C129 . C130 . H1301 . 109.0 no C131 . C130 . H1301 . 110.0 no C129 . C130 . H1302 . 106.0 no C131 . C130 . H1302 . 109.3 no H1301 . C130 . H1302 . 109.2 no C130 . C131 . C132 . 113.5(7) yes C130 . C131 . H1311 . 108.2 no C132 . C131 . H1311 . 109.8 no C130 . C131 . H1312 . 107.5 no C132 . C131 . H1312 . 108.2 no H1311 . C131 . H1312 . 109.5 no C131 . C132 . H1321 . 111.1 no C131 . C132 . H1322 . 110.4 no H1321 . C132 . H1322 . 108.7 no C131 . C132 . H1323 . 110.5 no H1321 . C132 . H1323 . 108.6 no H1322 . C132 . H1323 . 107.5 no C103 . C133 . C134 . 111.40(10) yes C103 . C133 . H1331 . 109.6 no C134 . C133 . H1331 . 105.4 no C103 . C133 . H1332 . 113.4 no C134 . C133 . H1332 . 109.3 no H1331 . C133 . H1332 . 107.3 no C133 . C134 . C135 . 111.25(10) yes C133 . C134 . H1341 . 109.5 no C135 . C134 . H1341 . 106.9 no C133 . C134 . H1342 . 109.9 no C135 . C134 . H1342 . 112.5 no H1341 . C134 . H1342 . 106.7 no C134 . C135 . C136 . 111.21(10) yes C134 . C135 . H1351 . 110.9 no C136 . C135 . H1351 . 106.9 no C134 . C135 . H1352 . 110.4 no C136 . C135 . H1352 . 108.3 no H1351 . C135 . H1352 . 109.1 no C135 . C136 . C137 . 111.40(10) yes C135 . C136 . H1361 . 108.4 no C137 . C136 . H1361 . 111.2 no C135 . C136 . H1362 . 107.1 no C137 . C136 . H1362 . 111.1 no H1361 . C136 . H1362 . 107.5 no C136 . C137 . C138 . 111.23(10) yes C136 . C137 . H1371 . 103.9 no C138 . C137 . H1371 . 111.9 no C136 . C137 . H1372 . 110.7 no C138 . C137 . H1372 . 110.5 no H1371 . C137 . H1372 . 108.3 no C137 . C138 . H1381 . 110.6 no C137 . C138 . H1382 . 105.0 no H1381 . C138 . H1382 . 109.2 no C137 . C138 . H1383 . 108.6 no H1381 . C138 . H1383 . 114.5 no H1382 . C138 . H1383 . 108.5 no C124 . C224 . C125 . 115.2(6) yes C123 . C224 . H1251 . 95.7 no C124 . C224 . H1251 . 155.4 no C123 . C224 . H2241 . 107.4 no C125 . C224 . H2241 . 156.6 no H1251 . C224 . H2241 . 127.1 no C123 . C224 . H2242 . 111.4 no C124 . C224 . H2242 . 167.2 no H2241 . C224 . H2242 . 109.4 no C123 . C224 . H2243 . 109.7 no H1251 . C224 . H2243 . 108.8 no H2241 . C224 . H2243 . 106.9 no H2242 . C224 . H2243 . 111.9 no C126 . C225 . C124 . 125.4(5) yes C123 . C225 . H1241 . 107.0 no C126 . C225 . H1241 . 148.0 no C123 . C225 . H2251 . 109.8 no C124 . C225 . H2251 . 163.3 no H1241 . C225 . H2251 . 109.5 no C123 . C225 . H2252 . 107.9 no C126 . C225 . H2252 . 147.9 no H2251 . C225 . H2252 . 108.4 no C123 . C225 . H2253 . 110.6 no C126 . C225 . H2253 . 103.1 no H1241 . C225 . H2253 . 108.8 no H2251 . C225 . H2253 . 111.1 no H2252 . C225 . H2253 . 108.9 no C126 . C226 . C125 . 123.6(4) yes C123 . C226 . H2261 . 108.2 no C126 . C226 . H2261 . 138.4 no C123 . C226 . H2262 . 111.5 no C126 . C226 . H2262 . 113.0 no C125 . C226 . H2262 . 84.5 no H2261 . C226 . H2262 . 108.5 no C123 . C226 . H2263 . 110.2 no C125 . C226 . H2263 . 164.1 no H2261 . C226 . H2263 . 107.2 no H2262 . C226 . H2263 . 111.1 no #===END data_js0513 _database_code_depnum_ccdc_archive 'CCDC 767032' #TrackingRef '- CCDC_deposided_merged_cifs_notepad.cif' _audit_creation_date 10-02-16 _audit_creation_method CRYSTALS_ver_12.82 _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 8.2012(2) _cell_length_b 12.8303(4) _cell_length_c 13.6161(4) _cell_angle_alpha 73.4069(16) _cell_angle_beta 84.6669(16) _cell_angle_gamma 89.6182(12) _cell_volume 1366.83(7) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Zn 0.2839 1.4301 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097 1.3041 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 1 _chemical_formula_sum 'C62 H74 F8 N4 O2 Zn1' _chemical_formula_moiety 'C62 H74 F8 N4 O2 Zn1' _chemical_compound_source ? _chemical_formula_weight 1124.64 # Structure does not match formula _cell_measurement_reflns_used 8990 _cell_measurement_theta_min 3 _cell_measurement_theta_max 25 _cell_measurement_temperature 180 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_max 0.50 _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 0.520 # Sheldrick geometric approximatio 0.89 0.96 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SORTAV (Blessing)' _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 0.96 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q _computing_data_collection 'COLLECT. Nonius (1997-2001).' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 180 _diffrn_reflns_number 11767 _reflns_number_total 4987 _diffrn_reflns_av_R_equivalents 0.108 # Number of reflections with Friedels Law is 4987 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 5006 _diffrn_reflns_theta_min 2.587 _diffrn_reflns_theta_max 25.366 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _reflns_limit_h_min -9 _reflns_limit_h_max 9 _reflns_limit_k_min -14 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.10 _refine_diff_density_max 0.45 _refine_ls_number_reflns 3681 _refine_ls_number_restraints 0 _refine_ls_number_parameters 335 #_refine_ls_R_factor_ref 0.0580 _refine_ls_wR_factor_ref 0.0676 _refine_ls_goodness_of_fit_ref 0.9926 #_reflns_number_all 4968 _refine_ls_R_factor_all 0.0750 _refine_ls_wR_factor_all 0.0781 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 3681 _refine_ls_R_factor_gt 0.0580 _refine_ls_wR_factor_gt 0.0676 _refine_ls_shift/su_max 0.001012 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.82 1.45 1.29 ; # Check this file using the IUCr facility at: # http://checkcif.iucr.org/ _refine_special_details ; A hexyl chain disordered over two position was refined with restrains The molecule contains one MeOH group, also disordered over two positions, bound to Zn centre. The corresponding H could not be located with precision in the Fourier map ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Zn1 Zn 1.0000 0.0000 1.0000 0.0353 1.0000 Uani S . . . . . N1 N 0.8284(3) 0.11306(18) 1.01778(18) 0.0277 1.0000 Uani . . . . . . N2 N 1.1328(3) 0.05100(18) 1.09859(18) 0.0289 1.0000 Uani . . . . . . F1 F 1.1126(3) 0.40133(16) 1.04187(18) 0.0520 1.0000 Uani . . . . . . F2 F 1.1033(3) 0.56349(18) 1.1280(2) 0.0751 1.0000 Uani . . . . . . F3 F 0.7780(4) 0.3439(2) 1.4159(2) 0.0794 1.0000 Uani . . . . . . F4 F 0.7909(3) 0.18019(19) 1.32981(17) 0.0586 1.0000 Uani . . . . . . C1 C 0.6881(3) 0.1305(2) 0.9685(2) 0.0289 1.0000 Uani . . . . . . C2 C 0.6398(3) 0.0738(2) 0.9028(2) 0.0295 1.0000 Uani . . . . . . C3 C 1.2791(3) 0.0086(2) 1.1288(2) 0.0294 1.0000 Uani . . . . . . C4 C 1.3415(4) 0.0607(2) 1.1988(2) 0.0340 1.0000 Uani . . . . . . C5 C 1.2301(4) 0.1360(3) 1.2118(3) 0.0373 1.0000 Uani . . . . . . C6 C 1.0990(4) 0.1306(2) 1.1471(2) 0.0306 1.0000 Uani . . . . . . C7 C 0.9591(4) 0.1957(2) 1.1332(2) 0.0321 1.0000 Uani . . . . . . C8 C 0.8311(3) 0.1880(2) 1.0723(2) 0.0300 1.0000 Uani . . . . . . C9 C 0.6851(4) 0.2547(2) 1.0573(2) 0.0328 1.0000 Uani . . . . . . C10 C 0.5979(3) 0.2186(2) 0.9931(2) 0.0307 1.0000 Uani . . . . . . C11 C 0.4379(4) 0.2621(3) 0.9525(3) 0.0365 1.0000 Uani . . . . . . C12 C 0.4574(4) 0.3708(3) 0.8683(3) 0.0415 1.0000 Uani . . . . . . C13 C 0.5555(4) 0.3655(3) 0.7702(3) 0.0442 1.0000 Uani . . . . . . C14 C 0.5874(5) 0.4772(3) 0.6910(3) 0.0521 1.0000 Uani . . . . . . C15 C 0.6891(7) 0.4751(4) 0.5957(4) 0.0701 1.0000 Uani . . . . . . C16 C 0.7279(9) 0.5877(5) 0.5211(4) 0.0983 1.0000 Uani . . . . . . C17 C 1.4983(4) 0.0318(3) 1.2497(3) 0.0405 1.0000 Uani . . . . . . C18 C 1.4764(5) -0.0607(3) 1.3489(3) 0.0531 1.0000 Uani . . . . . . C23 C 0.9495(3) 0.2861(2) 1.1825(2) 0.0348 1.0000 Uani . . . . . . C24 C 1.0278(4) 0.3859(3) 1.1340(3) 0.0420 1.0000 Uani . . . . . . C25 C 1.0227(5) 0.4693(3) 1.1789(3) 0.0526 1.0000 Uani . . . . . . C26 C 0.9395(5) 0.4581(3) 1.2735(4) 0.0587 1.0000 Uani . . . . . . C27 C 0.8616(5) 0.3599(4) 1.3226(3) 0.0565 1.0000 Uani . . . . . . C28 C 0.8685(4) 0.2753(3) 1.2777(3) 0.0412 1.0000 Uani . . . . . . C29 C 1.2477(5) 0.2055(3) 1.2824(4) 0.0607 1.0000 Uani . . . . . . C31 C 0.6292(4) 0.3457(3) 1.1020(3) 0.0442 1.0000 Uani . . . . . . C19 C 1.6577(11) -0.0842(6) 1.3896(7) 0.0484(18) 0.5000 Uiso . . . 1 1 . C20 C 1.7813(10) -0.1313(7) 1.3255(7) 0.0565(18) 0.5000 Uiso . . . 1 1 . C21 C 1.9403(12) -0.1537(8) 1.3709(7) 0.067(2) 0.5000 Uiso . . . 1 1 . C22 C 2.0562(15) -0.2171(10) 1.3158(9) 0.085(3) 0.5000 Uiso . . . 1 1 . C190 C 1.6020(11) -0.0764(7) 1.4235(7) 0.0527(19) 0.5000 Uiso . . . 1 2 . C200 C 1.7663(10) -0.1019(6) 1.3713(6) 0.0473(16) 0.5000 Uiso . . . 1 2 . C210 C 1.9037(12) -0.1180(8) 1.4411(7) 0.067(2) 0.5000 Uiso . . . 1 2 . C220 C 2.0610(16) -0.1460(10) 1.3920(10) 0.088(3) 0.5000 Uiso . . . 1 2 . O1 O 1.1309(6) 0.1340(4) 0.8560(4) 0.1074(13) 1.0000 Uiso . . . 1 1 1 C30 C 1.0744(10) 0.2425(6) 0.8316(6) 0.113(2) 1.0000 Uiso . . . . . . H21 H 0.5320 0.0943 0.8753 0.0336 1.0000 Uiso . . . . . . H111 H 0.3616 0.2721 1.0109 0.0422 1.0000 Uiso . . . . . . H112 H 0.3878 0.2073 0.9235 0.0422 1.0000 Uiso . . . . . . H121 H 0.5138 0.4235 0.8958 0.0487 1.0000 Uiso . . . . . . H122 H 0.3458 0.3976 0.8508 0.0487 1.0000 Uiso . . . . . . H131 H 0.6633 0.3322 0.7873 0.0513 1.0000 Uiso . . . . . . H132 H 0.4937 0.3187 0.7377 0.0513 1.0000 Uiso . . . . . . H141 H 0.6443 0.5243 0.7246 0.0580 1.0000 Uiso . . . . . . H142 H 0.4784 0.5087 0.6722 0.0580 1.0000 Uiso . . . . . . H151 H 0.7939 0.4388 0.6139 0.0829 1.0000 Uiso . . . . . . H152 H 0.6275 0.4319 0.5586 0.0829 1.0000 Uiso . . . . . . H161 H 0.7955 0.5806 0.4579 0.1084 1.0000 Uiso . . . . . . H162 H 0.7897 0.6317 0.5550 0.1084 1.0000 Uiso . . . . . . H163 H 0.6233 0.6248 0.4998 0.1084 1.0000 Uiso . . . . . . H171 H 1.5400 0.0977 1.2655 0.0503 1.0000 Uiso . . . . . . H172 H 1.5799 0.0099 1.2006 0.0503 1.0000 Uiso . . . . . . H181 H 1.3973 -0.0396 1.4015 0.0626 1.0000 Uiso . . . . . . H182 H 1.4298 -0.1276 1.3361 0.0626 1.0000 Uiso . . . . . . H191 H 1.6402 -0.1386 1.4619 0.0535 0.5000 Uiso . . . 1 1 . H192 H 1.7007 -0.0151 1.3972 0.0535 0.5000 Uiso . . . 1 1 . H201 H 1.7363 -0.2014 1.3169 0.0720 0.5000 Uiso . . . 1 1 . H202 H 1.7994 -0.0779 1.2537 0.0720 0.5000 Uiso . . . 1 1 . H211 H 1.9259 -0.1965 1.4424 0.0856 0.5000 Uiso . . . 1 1 . H212 H 2.0009 -0.0829 1.3625 0.0856 0.5000 Uiso . . . 1 1 . H1901 H 1.6114 -0.0093 1.4470 0.0622 0.5000 Uiso . . . 1 2 . H1902 H 1.5659 -0.1392 1.4873 0.0622 0.5000 Uiso . . . 1 2 . H2001 H 1.7949 -0.0391 1.3087 0.0558 0.5000 Uiso . . . 1 2 . H2002 H 1.7498 -0.1690 1.3495 0.0558 0.5000 Uiso . . . 1 2 . H2101 H 1.9223 -0.0510 1.4617 0.0772 0.5000 Uiso . . . 1 2 . H2102 H 1.8743 -0.1805 1.5046 0.0772 0.5000 Uiso . . . 1 2 . H261 H 0.9343 0.5184 1.3070 0.0766 1.0000 Uiso . . . . . . H291 H 1.3521 0.1889 1.3160 0.0801 1.0000 Uiso . . . . . . H292 H 1.1531 0.1901 1.3379 0.0801 1.0000 Uiso . . . . . . H293 H 1.2478 0.2842 1.2429 0.0801 1.0000 Uiso . . . . . . H311 H 0.5221 0.3729 1.0753 0.0554 1.0000 Uiso . . . . . . H312 H 0.6128 0.3168 1.1789 0.0554 1.0000 Uiso . . . . . . H313 H 0.7124 0.4053 1.0815 0.0554 1.0000 Uiso . . . . . . H301 H 1.1398 0.2923 0.7672 0.1996 1.0000 Uiso . . . . . . H302 H 1.0838 0.2760 0.8889 0.1996 1.0000 Uiso . . . . . . H303 H 0.9555 0.2467 0.8154 0.1996 1.0000 Uiso . . . . . . H2201 H 2.1490 -0.1567 1.4395 0.1074 0.5000 Uiso . . . 1 2 . H2202 H 2.0960 -0.0869 1.3272 0.1074 0.5000 Uiso . . . 1 22 . H2203 H 2.0461 -0.2159 1.3725 0.1074 0.5000 Uiso . . . 1 2 . H221 H 2.1603 -0.2301 1.3499 0.1025 0.5000 Uiso . . . 1 1 . H222 H 2.0031 -0.2889 1.3208 0.1025 0.5000 Uiso . . . 1 1 . H223 H 2.0794 -0.1749 1.2424 0.1025 0.5000 Uiso . . . 1 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 Zn1 0.0263(3) 0.0411(3) 0.0479(3) -0.0263(2) -0.0095(2) 0.0109(2) N1 0.0258(11) 0.0254(12) 0.0339(13) -0.0116(10) -0.0035(9) 0.0045(9) N2 0.0297(12) 0.0249(12) 0.0345(13) -0.0115(10) -0.0052(10) 0.0046(9) F1 0.0492(11) 0.0389(10) 0.0663(14) -0.0161(10) 0.0065(10) -0.0032(9) F2 0.0782(16) 0.0378(12) 0.117(2) -0.0319(13) -0.0194(15) -0.0075(11) F3 0.0953(19) 0.099(2) 0.0592(15) -0.0491(14) -0.0012(13) 0.0241(16) F4 0.0652(14) 0.0625(14) 0.0491(12) -0.0218(11) 0.0078(10) -0.0053(11) C1 0.0271(13) 0.0267(14) 0.0319(14) -0.0079(12) 0.0002(11) 0.0020(11) C2 0.0254(13) 0.0260(13) 0.0360(15) -0.0064(12) -0.0049(11) 0.0028(10) C3 0.0278(14) 0.0263(13) 0.0341(15) -0.0078(12) -0.0056(12) 0.0010(11) C4 0.0338(15) 0.0291(14) 0.0398(16) -0.0088(13) -0.0099(12) 0.0024(12) C5 0.0400(16) 0.0314(15) 0.0452(18) -0.0164(14) -0.0101(14) 0.0030(12) C6 0.0335(14) 0.0250(13) 0.0354(16) -0.0113(12) -0.0058(12) 0.0017(11) C7 0.0316(14) 0.0269(14) 0.0389(16) -0.0120(12) -0.0018(12) 0.0020(11) C8 0.0270(13) 0.0275(14) 0.0365(15) -0.0121(12) 0.0012(11) 0.0023(11) C9 0.0326(15) 0.0268(14) 0.0396(16) -0.0118(13) 0.0011(12) 0.0040(12) C10 0.0266(13) 0.0283(14) 0.0359(15) -0.0084(12) 0.0009(11) 0.0023(11) C11 0.0294(14) 0.0380(16) 0.0442(17) -0.0158(14) -0.0019(13) 0.0102(12) C12 0.0369(16) 0.0358(16) 0.054(2) -0.0156(15) -0.0093(14) 0.0141(13) C13 0.0478(18) 0.0380(17) 0.0478(19) -0.0127(15) -0.0096(15) 0.0086(14) C14 0.059(2) 0.0413(19) 0.052(2) -0.0059(16) -0.0106(17) 0.0070(16) C15 0.089(3) 0.065(3) 0.053(2) -0.015(2) 0.000(2) -0.010(2) C16 0.125(5) 0.094(4) 0.062(3) -0.001(3) 0.000(3) -0.028(4) C17 0.0396(16) 0.0385(17) 0.0509(19) -0.0206(15) -0.0174(14) 0.0055(13) C18 0.064(2) 0.048(2) 0.050(2) -0.0135(17) -0.0206(18) 0.0114(17) C23 0.0292(14) 0.0361(16) 0.0450(18) -0.0198(14) -0.0084(13) 0.0079(12) C24 0.0370(16) 0.0323(16) 0.062(2) -0.0207(15) -0.0103(15) 0.0062(13) C25 0.052(2) 0.0367(18) 0.080(3) -0.0288(18) -0.0211(19) 0.0072(15) C26 0.063(2) 0.049(2) 0.082(3) -0.043(2) -0.024(2) 0.0134(18) C27 0.053(2) 0.075(3) 0.057(2) -0.041(2) -0.0129(17) 0.022(2) C28 0.0401(16) 0.0395(18) 0.0484(19) -0.0190(15) -0.0061(14) 0.0032(14) C29 0.060(2) 0.063(2) 0.084(3) -0.052(2) -0.035(2) 0.0218(19) C31 0.0360(16) 0.0467(19) 0.061(2) -0.0314(17) -0.0110(15) 0.0148(14) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.5474(16) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zn1 . O1 2_757 2.379(5) yes Zn1 . N1 2_757 2.062(2) yes Zn1 . N2 2_757 2.049(2) yes Zn1 . N1 . 2.062(2) yes Zn1 . N2 . 2.049(2) yes Zn1 . O1 . 2.379(5) yes N1 . C1 . 1.370(4) yes N1 . C8 . 1.374(4) yes N2 . C3 . 1.364(4) yes N2 . C6 . 1.380(4) yes F1 . C24 . 1.340(4) yes F2 . C25 . 1.350(5) yes F3 . C27 . 1.349(5) yes F4 . C28 . 1.353(4) yes C1 . C2 . 1.390(4) yes C1 . C10 . 1.447(4) yes C2 . C3 2_757 1.393(4) yes C2 . H21 . 0.996 no C3 . C4 . 1.441(4) yes C4 . C5 . 1.362(4) yes C4 . C17 . 1.511(4) yes C5 . C6 . 1.466(4) yes C5 . C29 . 1.502(5) yes C6 . C7 . 1.410(4) yes C7 . C8 . 1.417(4) yes C7 . C23 . 1.496(4) yes C8 . C9 . 1.463(4) yes C9 . C10 . 1.357(4) yes C9 . C31 . 1.513(4) yes C10 . C11 . 1.512(4) yes C11 . C12 . 1.529(5) yes C11 . H111 . 1.002 no C11 . H112 . 1.006 no C12 . C13 . 1.512(5) yes C12 . H121 . 0.997 no C12 . H122 . 1.001 no C13 . C14 . 1.535(5) yes C13 . H131 . 0.998 no C13 . H132 . 1.006 no C14 . C15 . 1.483(6) yes C14 . H141 . 0.996 no C14 . H142 . 1.003 no C15 . C16 . 1.526(7) yes C15 . H151 . 0.993 no C15 . H152 . 1.014 no C16 . H161 . 1.006 no C16 . H162 . 0.993 no C16 . H163 . 1.004 no C17 . C18 . 1.519(5) yes C17 . H171 . 1.000 no C17 . H172 . 0.998 no C18 . C19 . 1.631(9) yes C18 . C190 . 1.485(9) yes C18 . H181 . 1.014 no C18 . H182 . 1.008 no C23 . C24 . 1.391(5) yes C23 . C28 . 1.371(5) yes C24 . C25 . 1.375(5) yes C25 . C26 . 1.371(6) yes C26 . C27 . 1.375(6) yes C26 . H261 . 1.003 no C27 . C28 . 1.387(5) yes C29 . H291 . 1.001 no C29 . H292 . 1.010 no C29 . H293 . 1.000 no C31 . H311 . 1.004 no C31 . H312 . 1.001 no C31 . H313 . 0.989 no C19 . C20 . 1.511(13) yes C19 . H191 . 1.029 no C19 . H192 . 0.992 no C20 . C21 . 1.487(13) yes C20 . H202 . 1.020 no C20 . H2001 . 1.144 no C20 . H2002 . 0.551 no C21 . C22 . 1.528(15) yes C21 . H211 . 0.968 no C21 . H212 . 1.010 no C21 . H2203 . 1.172 no C22 . H2203 . 0.774 no C22 . H221 . 1.000 no C22 . H222 . 1.004 no C22 . H223 . 0.992 no C190 . C200 . 1.541(12) yes C190 . H1901 . 1.007 no C190 . H1902 . 1.023 no C200 . C210 . 1.517(12) yes C200 . H2001 . 1.003 no C200 . H2002 . 1.001 no C210 . C220 . 1.487(16) yes C210 . H2101 . 0.993 no C210 . H2102 . 1.008 no C220 . H2201 . 0.996 no C220 . H2202 . 1.005 no C220 . H2203 . 1.016 no O1 . C30 . 1.421(9) yes C30 . H301 . 1.030 no C30 . H302 . 1.002 no C30 . H303 . 1.018 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 2_757 Zn1 . N1 2_757 88.95(14) yes O1 2_757 Zn1 . N2 2_757 91.11(14) yes N1 2_757 Zn1 . N2 2_757 87.33(9) yes O1 2_757 Zn1 . N1 . 91.05(14) yes N1 2_757 Zn1 . N1 . 179.994 yes N2 2_757 Zn1 . N1 . 92.67(9) yes O1 2_757 Zn1 . N2 . 88.89(14) yes N1 2_757 Zn1 . N2 . 92.67(9) yes N2 2_757 Zn1 . N2 . 179.994 yes N1 . Zn1 . N2 . 87.33(9) yes O1 2_757 Zn1 . O1 . 179.995 yes N1 2_757 Zn1 . O1 . 91.05(14) yes N2 2_757 Zn1 . O1 . 88.89(14) yes N1 . Zn1 . O1 . 88.95(14) yes N2 . Zn1 . O1 . 91.11(14) yes Zn1 . N1 . C1 . 123.71(18) yes Zn1 . N1 . C8 . 129.77(18) yes C1 . N1 . C8 . 106.4(2) yes Zn1 . N2 . C3 . 124.03(19) yes Zn1 . N2 . C6 . 129.74(19) yes C3 . N2 . C6 . 106.2(2) yes N1 . C1 . C2 . 125.3(3) yes N1 . C1 . C10 . 110.2(2) yes C2 . C1 . C10 . 124.4(3) yes C3 2_757 C2 . C1 . 128.7(3) yes C3 2_757 C2 . H21 . 115.9 no C1 . C2 . H21 . 115.4 no C2 2_757 C3 . N2 . 125.6(3) yes C2 2_757 C3 . C4 . 123.5(3) yes N2 . C3 . C4 . 110.9(2) yes C3 . C4 . C5 . 106.9(3) yes C3 . C4 . C17 . 125.1(3) yes C5 . C4 . C17 . 127.9(3) yes C4 . C5 . C6 . 106.4(3) yes C4 . C5 . C29 . 123.4(3) yes C6 . C5 . C29 . 130.2(3) yes C5 . C6 . N2 . 109.5(2) yes C5 . C6 . C7 . 127.0(3) yes N2 . C6 . C7 . 123.5(3) yes C6 . C7 . C8 . 126.5(3) yes C6 . C7 . C23 . 116.7(3) yes C8 . C7 . C23 . 116.6(2) yes C7 . C8 . N1 . 123.1(2) yes C7 . C8 . C9 . 127.1(3) yes N1 . C8 . C9 . 109.8(2) yes C8 . C9 . C10 . 106.5(2) yes C8 . C9 . C31 . 130.3(3) yes C10 . C9 . C31 . 123.2(3) yes C1 . C10 . C9 . 107.1(3) yes C1 . C10 . C11 . 125.7(3) yes C9 . C10 . C11 . 127.2(3) yes C10 . C11 . C12 . 113.4(3) yes C10 . C11 . H111 . 108.9 no C12 . C11 . H111 . 108.4 no C10 . C11 . H112 . 108.7 no C12 . C11 . H112 . 108.5 no H111 . C11 . H112 . 108.8 no C11 . C12 . C13 . 114.5(3) yes C11 . C12 . H121 . 108.2 no C13 . C12 . H121 . 108.0 no C11 . C12 . H122 . 108.5 no C13 . C12 . H122 . 108.1 no H121 . C12 . H122 . 109.6 no C12 . C13 . C14 . 113.4(3) yes C12 . C13 . H131 . 109.1 no C14 . C13 . H131 . 108.3 no C12 . C13 . H132 . 108.7 no C14 . C13 . H132 . 108.1 no H131 . C13 . H132 . 109.2 no C13 . C14 . C15 . 114.6(3) yes C13 . C14 . H141 . 107.7 no C15 . C14 . H141 . 108.4 no C13 . C14 . H142 . 107.7 no C15 . C14 . H142 . 108.8 no H141 . C14 . H142 . 109.5 no C14 . C15 . C16 . 113.7(5) yes C14 . C15 . H151 . 109.5 no C16 . C15 . H151 . 108.5 no C14 . C15 . H152 . 108.5 no C16 . C15 . H152 . 107.7 no H151 . C15 . H152 . 108.9 no C15 . C16 . H161 . 109.7 no C15 . C16 . H162 . 109.5 no H161 . C16 . H162 . 109.6 no C15 . C16 . H163 . 109.7 no H161 . C16 . H163 . 108.7 no H162 . C16 . H163 . 109.7 no C4 . C17 . C18 . 113.3(3) yes C4 . C17 . H171 . 108.3 no C18 . C17 . H171 . 108.6 no C4 . C17 . H172 . 108.4 no C18 . C17 . H172 . 108.5 no H171 . C17 . H172 . 109.6 no C17 . C18 . C19 . 106.5(4) yes C17 . C18 . C190 . 119.5(5) yes C17 . C18 . H181 . 110.3 no C19 . C18 . H181 . 111.2 no C190 . C18 . H181 . 88.0 no C17 . C18 . H182 . 110.6 no C19 . C18 . H182 . 110.6 no C190 . C18 . H182 . 117.6 no H181 . C18 . H182 . 107.7 no C7 . C23 . C24 . 120.8(3) yes C7 . C23 . C28 . 122.7(3) yes C24 . C23 . C28 . 116.4(3) yes C23 . C24 . F1 . 119.7(3) yes C23 . C24 . C25 . 121.7(4) yes F1 . C24 . C25 . 118.6(3) yes F2 . C25 . C24 . 118.5(4) yes F2 . C25 . C26 . 120.1(3) yes C24 . C25 . C26 . 121.4(4) yes C25 . C26 . C27 . 117.7(3) yes C25 . C26 . H261 . 122.2 no C27 . C26 . H261 . 120.1 no F3 . C27 . C26 . 120.4(4) yes F3 . C27 . C28 . 118.8(4) yes C26 . C27 . C28 . 120.9(4) yes F4 . C28 . C27 . 118.4(3) yes F4 . C28 . C23 . 119.6(3) yes C27 . C28 . C23 . 122.0(3) yes C5 . C29 . H291 . 110.2 no C5 . C29 . H292 . 109.8 no H291 . C29 . H292 . 108.5 no C5 . C29 . H293 . 110.2 no H291 . C29 . H293 . 109.4 no H292 . C29 . H293 . 108.7 no C9 . C31 . H311 . 108.7 no C9 . C31 . H312 . 109.2 no H311 . C31 . H312 . 109.0 no C9 . C31 . H313 . 109.7 no H311 . C31 . H313 . 110.0 no H312 . C31 . H313 . 110.3 no C18 . C19 . C20 . 116.7(6) yes C18 . C19 . H191 . 106.2 no C20 . C19 . H191 . 107.9 no C18 . C19 . H192 . 107.5 no C20 . C19 . H192 . 110.4 no H191 . C19 . H192 . 107.7 no C19 . C20 . C21 . 112.6(8) yes C19 . C20 . H202 . 108.5 no C21 . C20 . H202 . 109.7 no C21 . C20 . H2001 . 94.0 no C21 . C20 . H2002 . 96.1 no H202 . C20 . H2002 . 145.7 no H2001 . C20 . H2002 . 146.9 no C20 . C21 . C22 . 112.8(9) yes C20 . C21 . H211 . 111.9 no C22 . C21 . H211 . 106.3 no C20 . C21 . H212 . 109.7 no C22 . C21 . H212 . 104.6 no H211 . C21 . H212 . 111.2 no C20 . C21 . H2203 . 137.1 no H212 . C21 . H2203 . 103.2 no C21 . C22 . H221 . 109.2 no H2203 . C22 . H221 . 66.5 no C21 . C22 . H222 . 109.0 no H2203 . C22 . H222 . 101.9 no H221 . C22 . H222 . 109.2 no C21 . C22 . H223 . 109.6 no H221 . C22 . H223 . 110.1 no H222 . C22 . H223 . 109.8 no C18 . C190 . C200 . 108.7(7) yes C18 . C190 . H1901 . 109.8 no C200 . C190 . H1901 . 111.4 no C18 . C190 . H1902 . 109.5 no C200 . C190 . H1902 . 110.4 no H1901 . C190 . H1902 . 107.1 no C190 . C200 . C210 . 112.7(7) yes C190 . C200 . H2001 . 107.3 no C210 . C200 . H2001 . 109.5 no C190 . C200 . H2002 . 108.0 no C210 . C200 . H2002 . 110.2 no H2001 . C200 . H2002 . 109.1 no C200 . C210 . C220 . 112.8(9) yes C200 . C210 . H2101 . 110.5 no C220 . C210 . H2101 . 108.2 no C200 . C210 . H2102 . 109.5 no C220 . C210 . H2102 . 106.4 no H2101 . C210 . H2102 . 109.3 no C210 . C220 . H2201 . 111.3 no H211 . C220 . H2201 . 109.4 no C210 . C220 . H2202 . 110.2 no H211 . C220 . H2202 . 139.2 no H2201 . C220 . H2202 . 109.3 no C210 . C220 . H2203 . 109.7 no H2201 . C220 . H2203 . 108.5 no H2202 . C220 . H2203 . 107.8 no Zn1 . O1 . C30 . 119.4(4) yes O1 . C30 . H301 . 111.9 no O1 . C30 . H302 . 112.2 no H301 . C30 . H302 . 106.9 no O1 . C30 . H303 . 111.8 no H301 . C30 . H303 . 105.7 no H302 . C30 . H303 . 107.9 no #===END data_js0512 _database_code_depnum_ccdc_archive 'CCDC 767033' #TrackingRef '- CCDC_deposided_merged_cifs_notepad.cif' _audit_creation_date 10-02-19 _audit_creation_method CRYSTALS_ver_12.82 _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 5.71690(10) _cell_length_b 14.8893(3) _cell_length_c 15.0975(4) _cell_angle_alpha 95.7726(10) _cell_angle_beta 100.8123(11) _cell_angle_gamma 96.9559(12) _cell_volume 1242.94(5) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Zn 0.2839 1.4301 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097 1.3041 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 1 _chemical_formula_sum 'C60 H71 F2 N4 Zn1' _chemical_formula_moiety 'C60 H71 F2 N4 Zn1' _chemical_compound_source ? _chemical_formula_weight 951.63 _cell_measurement_reflns_used 10573 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27 _cell_measurement_temperature 180 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_min 0.07 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_max 0.46 _exptl_crystal_density_diffrn 1.271 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 507 _exptl_absorpt_coefficient_mu 0.545 # Sheldrick geometric approximatio 0.88 0.96 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.96 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q _computing_data_collection 'COLLECT. Nonius (1997-2001).' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 180 _diffrn_reflns_number 13167 _reflns_number_total 5607 _diffrn_reflns_av_R_equivalents 0.103 # Number of reflections with Friedels Law is 5607 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 5656 _diffrn_reflns_theta_min 2.937 _diffrn_reflns_theta_max 27.410 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _reflns_limit_h_min -7 _reflns_limit_h_max 7 _reflns_limit_k_min -19 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.17 _refine_diff_density_max 2.22 _refine_ls_number_reflns 4463 _refine_ls_number_restraints 106 _refine_ls_number_parameters 349 #_refine_ls_R_factor_ref 0.0920 _refine_ls_wR_factor_ref 0.1026 _refine_ls_goodness_of_fit_ref 1.0860 #_reflns_number_all 5598 _refine_ls_R_factor_all 0.1091 _refine_ls_wR_factor_all 0.1160 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 4463 _refine_ls_R_factor_gt 0.0920 _refine_ls_wR_factor_gt 0.1026 _refine_ls_shift/su_max 0.014524 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 2.85 1.42 1.97 ; _refine_special_details ; Severe disorder on more than 2 sites in hexyl chains were observed: disordered chains were idealised and refined with restrains. The entire molecule is disordered over two sites: fluorine atoms were refined with partial occupancies Hydrogen atoms were placed geometrically after each cycle, the preferred orientations of those groups whose conformations could not be assigned unambiguously having been previously identified by examination of a difference Fourier map. ; # Check this file using the IUCr facility at: # http://checkcif.iucr.org/ # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin D.J. (1994). Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Zn1 Zn 1.0000 0.0000 1.0000 0.0222 1.0000 Uani S . . . . . N1 N 0.6940(6) 0.0229(2) 0.9172(2) 0.0236 1.0000 Uani . . . . . . N2 N 0.9532(6) -0.1345(2) 0.9455(2) 0.0222 1.0000 Uani . . . . . . F1 F 0.7268(8) 0.4288(2) 0.7703(2) 0.0447 0.7500 Uani D U . 1 1 . F2 F 0.1950(15) 0.4320(7) 0.9642(8) 0.0395 0.2500 Uani D U . 1 2 . C1 C 0.9017(7) 0.2004(2) 1.0331(3) 0.0239 1.0000 Uani . . . . . . C2 C 0.7017(7) 0.1875(2) 0.9608(3) 0.0244 1.0000 Uani . . . . . . C3 C 0.5961(7) 0.1032(2) 0.9102(2) 0.0230 1.0000 Uani . . . . . . C4 C 0.3688(7) 0.0855(3) 0.8432(3) 0.0260 1.0000 Uani . . . . . . C5 C 0.3321(6) -0.0059(3) 0.8117(3) 0.0242 1.0000 Uani . . . . . . C6 C 0.5381(7) -0.0431(2) 0.8566(2) 0.0236 1.0000 Uani . . . . . . C7 C 0.5773(7) -0.1323(2) 0.8370(2) 0.0235 1.0000 Uani . . . . . . C8 C 0.7731(7) -0.1734(2) 0.8743(3) 0.0235 1.0000 Uani . . . . . . C9 C 0.8060(7) -0.2657(3) 0.8456(3) 0.0275 1.0000 Uani D . . . . . C10 C 1.0056(7) -0.2835(2) 0.9025(3) 0.0250 1.0000 Uani . . . . . . C11 C 1.1064(9) -0.3724(3) 0.8942(3) 0.0372 1.0000 Uani . . . . . . C12 C 0.6704(8) -0.3246(3) 0.7595(3) 0.0533 1.0000 Uani D U . . . . C13 C 0.8250(11) -0.3185(7) 0.6863(3) 0.0581 0.5000 Uani D U . . . . C14 C 0.6818(14) -0.3662(8) 0.5934(4) 0.0636 0.5000 Uani D U . . . . C15 C 0.8306(19) -0.3489(7) 0.5200(4) 0.0685 0.5000 Uani D U . . . . C16 C 0.7273(17) -0.4164(8) 0.4335(5) 0.0742 0.5000 Uani D U . . . . C17 C 0.8971(14) -0.4078(5) 0.3658(3) 0.0777 1.0000 Uani D U . . . . C18 C 0.1167(7) -0.0587(3) 0.7468(3) 0.0291 1.0000 Uani . . . . . . C19 C 0.1161(8) -0.0537(3) 0.6457(3) 0.0334 1.0000 Uani . . . . . . C20 C 0.2996(8) -0.1048(3) 0.6085(3) 0.0366 1.0000 Uani . . . . . . C21 C 0.2689(9) -0.1106(3) 0.5051(3) 0.0388 1.0000 Uani . . . . . . C22 C 0.4398(10) -0.1667(4) 0.4674(3) 0.0487 1.0000 Uani . . . . . . C23 C 0.4008(13) -0.1767(5) 0.3641(4) 0.0610 1.0000 Uani . . . . . . C24 C 0.1887(7) 0.1479(3) 0.8148(3) 0.0314 1.0000 Uani . . . . . . C25 C 0.6091(7) 0.2716(2) 0.9290(3) 0.0245 1.0000 Uani . . . . . . C26 C 0.4282(8) 0.3106(3) 0.9628(3) 0.0313 1.0000 Uani . . . . . . C27 C 0.3547(8) 0.3891(3) 0.9309(3) 0.0380 1.0000 Uani D U . . . . C28 C 0.4561(9) 0.4305(3) 0.8673(3) 0.0377 1.0000 Uani . . . . . . C29 C 0.6339(9) 0.3905(3) 0.8336(3) 0.0403 1.0000 Uani D U . . . . C30 C 0.7125(7) 0.3123(3) 0.8638(3) 0.0284 1.0000 Uani . . . . . . C130 C 0.7816(17) -0.2999(4) 0.6782(3) 0.0565 0.5000 Uani D U . . . . C140 C 0.7154(19) -0.3799(5) 0.6007(5) 0.0614 0.5000 Uani D U . . . . C150 C 0.8680(17) -0.3633(7) 0.5284(4) 0.0664 0.5000 Uani D U . . . . C160 C 0.771(2) -0.4333(6) 0.4433(5) 0.0733 0.5000 Uani D U . . . . H71 H 0.4529 -0.1702 0.7953 0.0289 1.0000 Uiso . . . . . . H111 H 1.0143 -0.4145 0.8444 0.0570 1.0000 Uiso . . . . . . H112 H 1.1112 -0.3999 0.9488 0.0570 1.0000 Uiso . . . . . . H113 H 1.2728 -0.3614 0.8841 0.0569 1.0000 Uiso . . . . . . H181 H 0.1061 -0.1231 0.7565 0.0349 1.0000 Uiso . . . . . . H182 H -0.0297 -0.0351 0.7603 0.0349 1.0000 Uiso . . . . . . H191 H 0.1451 0.0112 0.6358 0.0409 1.0000 Uiso . . . . . . H192 H -0.0475 -0.0782 0.6101 0.0410 1.0000 Uiso . . . . . . H201 H 0.2815 -0.1667 0.6260 0.0439 1.0000 Uiso . . . . . . H202 H 0.4629 -0.0746 0.6382 0.0439 1.0000 Uiso . . . . . . H211 H 0.0987 -0.1363 0.4769 0.0469 1.0000 Uiso . . . . . . H212 H 0.2906 -0.0476 0.4893 0.0469 1.0000 Uiso . . . . . . H221 H 0.4216 -0.2287 0.4866 0.0610 1.0000 Uiso . . . . . . H222 H 0.6072 -0.1390 0.4931 0.0611 1.0000 Uiso . . . . . . H231 H 0.5073 -0.2154 0.3431 0.0970 1.0000 Uiso . . . . . . H232 H 0.2341 -0.2022 0.3373 0.0970 1.0000 Uiso . . . . . . H233 H 0.4330 -0.1166 0.3446 0.0970 1.0000 Uiso . . . . . . H241 H 0.0469 0.1144 0.7727 0.0501 1.0000 Uiso . . . . . . H242 H 0.1319 0.1739 0.8672 0.0500 1.0000 Uiso . . . . . . H243 H 0.2545 0.1973 0.7868 0.0500 1.0000 Uiso . . . . . . H261 H 0.3589 0.2827 1.0061 0.0402 1.0000 Uiso . . . . . . H281 H 0.4003 0.4827 0.8441 0.0462 1.0000 Uiso . . . . . . H301 H 0.8353 0.2864 0.8396 0.0339 1.0000 Uiso . . . . . . H121 H 0.6418 -0.3891 0.7653 0.0999 1.0000 Uiso . . . . . . H122 H 0.5044 -0.3098 0.7409 0.1000 1.0000 Uiso . . . . . . H1301 H 0.9563 -0.2858 0.6974 0.0814 0.5000 Uiso . . . . . . H1302 H 0.7137 -0.2450 0.6538 0.0814 0.5000 Uiso . . . . . . H131 H 0.9622 -0.3549 0.7028 0.0826 0.5000 Uiso . . . . . . H132 H 0.8831 -0.2562 0.6816 0.0826 0.5000 Uiso . . . . . . H141 H 0.6347 -0.4330 0.5923 0.0855 0.5000 Uiso . . . . . . H142 H 0.5199 -0.3389 0.5785 0.0855 0.5000 Uiso . . . . . . H1401 H 0.7482 -0.4383 0.6264 0.0838 0.5000 Uiso . . . . . . H1402 H 0.5390 -0.3872 0.5718 0.0838 0.5000 Uiso . . . . . . H151 H 0.9941 -0.3545 0.5428 0.0880 0.5000 Uiso . . . . . . H152 H 0.8166 -0.2827 0.5050 0.0880 0.5000 Uiso . . . . . . H1501 H 1.0385 -0.3697 0.5540 0.0863 0.5000 Uiso . . . . . . H1502 H 0.8597 -0.2997 0.5128 0.0863 0.5000 Uiso . . . . . . H161 H 0.6995 -0.4779 0.4495 0.0903 0.5000 Uiso . . . . . . H162 H 0.5570 -0.3997 0.4041 0.0903 0.5000 Uiso . . . . . . H1601 H 0.7992 -0.4951 0.4579 0.0894 0.5000 Uiso . . . . . . H1602 H 0.5892 -0.4332 0.4254 0.0894 0.5000 Uiso . . . . . . H171 H 0.8264 -0.4489 0.3106 0.0916 0.5000 Uiso . . . . . . H172 H 1.0524 -0.4198 0.3967 0.0916 0.5000 Uiso . . . . . . H173 H 0.9099 -0.3416 0.3513 0.0916 0.5000 Uiso . . . . . . H291 H 0.7093 0.4191 0.7862 0.0505 0.2500 Uiso . . . . . . H271 H 0.2247 0.4164 0.9554 0.0442 0.7500 Uiso . . . . . . 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 0.0226(3) 0.0211(3) 0.0215(3) 0.0011(2) 0.0006(2) 0.0052(2) N1 0.0244(15) 0.0225(14) 0.0236(15) 0.0021(11) 0.0029(12) 0.0054(11) N2 0.0229(14) 0.0198(13) 0.0233(14) 0.0005(11) 0.0040(12) 0.0036(11) F1 0.064(2) 0.0368(15) 0.0388(16) 0.0167(13) 0.0168(15) 0.0074(14) F2 0.034(2) 0.034(2) 0.050(3) -0.003(2) 0.006(2) 0.013(2) C1 0.0259(17) 0.0227(16) 0.0252(17) 0.0053(13) 0.0076(14) 0.0060(13) C2 0.0254(17) 0.0213(16) 0.0285(18) 0.0046(13) 0.0074(14) 0.0071(13) C3 0.0226(16) 0.0229(16) 0.0239(17) 0.0039(13) 0.0035(13) 0.0057(13) C4 0.0217(17) 0.0297(18) 0.0270(18) 0.0073(14) 0.0020(14) 0.0068(14) C5 0.0214(16) 0.0275(17) 0.0240(17) 0.0041(14) 0.0032(13) 0.0063(13) C6 0.0233(17) 0.0264(17) 0.0214(17) 0.0055(13) 0.0023(13) 0.0059(13) C7 0.0237(17) 0.0233(16) 0.0222(16) 0.0032(13) 0.0019(13) 0.0016(13) C8 0.0237(17) 0.0209(16) 0.0250(17) 0.0045(13) 0.0023(14) 0.0026(13) C9 0.0321(19) 0.0235(17) 0.0282(18) 0.0047(14) 0.0084(15) 0.0042(14) C10 0.0302(18) 0.0212(16) 0.0255(18) 0.0024(13) 0.0086(14) 0.0072(14) C11 0.044(2) 0.0245(18) 0.041(2) -0.0046(16) 0.0017(19) 0.0121(17) C12 0.072(2) 0.0377(19) 0.050(2) 0.0094(16) 0.0021(18) 0.0208(18) C13 0.074(3) 0.045(2) 0.055(2) 0.012(2) 0.004(2) 0.019(2) C14 0.077(3) 0.054(3) 0.059(2) 0.012(2) 0.001(2) 0.019(2) C15 0.080(3) 0.062(3) 0.062(3) 0.014(2) 0.003(2) 0.020(3) C16 0.084(3) 0.069(3) 0.067(3) 0.011(2) 0.001(2) 0.020(2) C17 0.086(3) 0.074(3) 0.069(2) 0.010(2) 0.002(2) 0.020(2) C18 0.0226(17) 0.0331(19) 0.0299(19) 0.0046(15) 0.0017(14) 0.0018(14) C19 0.0284(19) 0.040(2) 0.030(2) 0.0041(16) -0.0014(15) 0.0060(16) C20 0.036(2) 0.046(2) 0.027(2) 0.0021(17) 0.0007(16) 0.0118(18) C21 0.041(2) 0.046(2) 0.026(2) 0.0024(17) -0.0011(17) 0.0064(19) C22 0.049(3) 0.066(3) 0.029(2) 0.000(2) 0.004(2) 0.013(2) C23 0.064(4) 0.082(4) 0.036(3) 0.002(3) 0.011(3) 0.010(3) C24 0.0248(18) 0.0297(19) 0.038(2) 0.0041(16) 0.0007(16) 0.0080(15) C25 0.0250(17) 0.0227(16) 0.0264(17) 0.0039(13) 0.0036(14) 0.0073(13) C26 0.0287(19) 0.0290(19) 0.039(2) 0.0034(16) 0.0105(16) 0.0082(15) C27 0.033(2) 0.0322(19) 0.048(2) -0.0027(17) 0.0047(17) 0.0130(15) C28 0.045(2) 0.0265(19) 0.041(2) 0.0073(16) -0.0001(19) 0.0130(17) C29 0.058(2) 0.0312(16) 0.0358(17) 0.0146(14) 0.0142(16) 0.0088(15) C30 0.0292(18) 0.0263(18) 0.0294(19) 0.0020(14) 0.0058(15) 0.0045(14) C130 0.075(3) 0.043(2) 0.053(2) 0.0125(19) 0.005(2) 0.025(2) C140 0.077(3) 0.051(3) 0.058(2) 0.010(2) 0.005(2) 0.026(2) C150 0.079(3) 0.060(3) 0.062(3) 0.014(2) 0.007(2) 0.027(2) C160 0.083(3) 0.068(3) 0.068(2) 0.011(2) 0.002(2) 0.025(2) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.872(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zn1 . N2 2_757 2.053(3) yes Zn1 . N1 2_757 2.037(3) yes Zn1 . N1 . 2.037(3) yes Zn1 . N2 . 2.053(3) yes N1 . C3 . 1.386(5) yes N1 . C6 . 1.378(5) yes N2 . C1 2_757 1.384(5) yes N2 . C8 . 1.366(5) yes F1 . C29 . 1.3229(19) yes F2 . C27 . 1.320(2) yes C1 . C10 2_757 1.470(5) yes C1 . C2 . 1.404(5) yes C2 . C3 . 1.404(5) yes C2 . C25 . 1.506(5) yes C3 . C4 . 1.467(5) yes C4 . C5 . 1.374(5) yes C4 . C24 . 1.501(5) yes C5 . C6 . 1.445(5) yes C5 . C18 . 1.501(5) yes C6 . C7 . 1.386(5) yes C7 . C8 . 1.393(5) yes C7 . H71 . 0.940 no C8 . C9 . 1.444(5) yes C9 . C10 . 1.364(6) yes C9 . C12 . 1.513(6) yes C10 . C11 . 1.509(5) yes C11 . H111 . 0.955 no C11 . H112 . 0.954 no C11 . H113 . 0.988 no C12 . C13 . 1.542(2) yes C12 . C130 . 1.541(2) yes C12 . H121 . 0.969 no C12 . H122 . 0.996 no C13 . C14 . 1.540(2) yes C13 . C140 . 1.489(7) yes C13 . H1301 . 0.823 no C13 . H131 . 1.014 no C13 . H132 . 0.960 no C14 . C15 . 1.541(2) yes C14 . C130 . 1.508(7) yes C14 . C150 . 1.576(7) yes C14 . H141 . 0.996 no C14 . H142 . 1.051 no C14 . H1401 . 1.297 no C14 . H1402 . 0.829 no C15 . C16 . 1.539(2) yes C15 . C140 . 1.572(6) yes C15 . C160 . 1.579(8) yes C15 . H151 . 0.950 no C15 . H152 . 1.043 no C15 . H1501 . 1.289 no C15 . H1502 . 0.755 no C16 . C17 . 1.539(2) yes C16 . C150 . 1.585(8) yes C16 . H161 . 0.972 no C16 . H162 . 1.060 no C16 . H1602 . 0.782 no C17 . C160 . 1.540(2) yes C17 . H171 . 0.971 no C17 . H172 . 0.967 no C17 . H173 . 1.029 no C18 . C19 . 1.535(6) yes C18 . H181 . 0.981 no C18 . H182 . 0.993 no C19 . C20 . 1.524(6) yes C19 . H191 . 0.991 no C19 . H192 . 0.992 no C20 . C21 . 1.530(6) yes C20 . H201 . 0.984 no C20 . H202 . 0.988 no C21 . C22 . 1.512(7) yes C21 . H211 . 0.998 no C21 . H212 . 0.991 no C22 . C23 . 1.523(7) yes C22 . H221 . 0.995 no C22 . H222 . 0.985 no C23 . H231 . 0.962 no C23 . H232 . 0.976 no C23 . H233 . 0.977 no C24 . H241 . 0.977 no C24 . H242 . 0.973 no C24 . H243 . 0.957 no C25 . C26 . 1.396(5) yes C25 . C30 . 1.392(6) yes C26 . C27 . 1.390(6) yes C26 . H261 . 0.932 no C27 . C28 . 1.371(7) yes C27 . H271 . 1.000 no C28 . C29 . 1.388(7) yes C28 . H281 . 0.950 no C29 . C30 . 1.385(6) yes C29 . H291 . 1.006 no C30 . H301 . 0.953 no C130 . C140 . 1.540(2) yes C130 . H1301 . 0.977 no C130 . H1302 . 1.018 no C130 . H132 . 0.808 no C140 . C150 . 1.540(2) yes C140 . H141 . 0.851 no C140 . H1401 . 1.012 no C140 . H1402 . 1.009 no C150 . C160 . 1.540(2) yes C150 . H1501 . 0.998 no C150 . H1502 . 1.002 no C160 . H1601 . 0.992 no C160 . H1602 . 1.023 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N2 2_757 Zn1 . N1 2_757 92.12(12) yes N2 2_757 Zn1 . N1 . 87.88(12) yes N1 2_757 Zn1 . N1 . 179.994 yes N2 2_757 Zn1 . N2 . 179.994 yes N1 2_757 Zn1 . N2 . 87.88(12) yes N1 . Zn1 . N2 . 92.12(12) yes Zn1 . N1 . C3 . 129.2(3) yes Zn1 . N1 . C6 . 124.6(2) yes C3 . N1 . C6 . 106.2(3) yes C1 2_757 N2 . Zn1 . 128.6(3) yes C1 2_757 N2 . C8 . 107.1(3) yes Zn1 . N2 . C8 . 124.1(2) yes C10 2_757 C1 . N2 2_757 108.6(3) yes C10 2_757 C1 . C2 . 127.3(3) yes N2 2_757 C1 . C2 . 124.2(3) yes C1 . C2 . C3 . 125.2(3) yes C1 . C2 . C25 . 117.2(3) yes C3 . C2 . C25 . 117.3(3) yes C2 . C3 . N1 . 124.2(3) yes C2 . C3 . C4 . 126.4(3) yes N1 . C3 . C4 . 109.4(3) yes C3 . C4 . C5 . 106.9(3) yes C3 . C4 . C24 . 130.3(3) yes C5 . C4 . C24 . 122.7(3) yes C4 . C5 . C6 . 106.5(3) yes C4 . C5 . C18 . 127.4(3) yes C6 . C5 . C18 . 126.1(3) yes C5 . C6 . N1 . 111.0(3) yes C5 . C6 . C7 . 123.8(3) yes N1 . C6 . C7 . 125.1(3) yes C6 . C7 . C8 . 128.0(3) yes C6 . C7 . H71 . 115.6 no C8 . C7 . H71 . 116.4 no C7 . C8 . N2 . 125.4(3) yes C7 . C8 . C9 . 124.1(3) yes N2 . C8 . C9 . 110.4(3) yes C8 . C9 . C10 . 106.9(3) yes C8 . C9 . C12 . 125.8(4) yes C10 . C9 . C12 . 126.5(4) yes C1 2_757 C10 . C9 . 106.9(3) yes C1 2_757 C10 . C11 . 129.2(4) yes C9 . C10 . C11 . 123.8(4) yes C10 . C11 . H111 . 112.1 no C10 . C11 . H112 . 110.5 no H111 . C11 . H112 . 108.9 no C10 . C11 . H113 . 110.1 no H111 . C11 . H113 . 107.5 no H112 . C11 . H113 . 107.6 no C9 . C12 . C13 . 108.60(18) yes C9 . C12 . C130 . 110.06(18) yes C9 . C12 . H121 . 114.3 no C13 . C12 . H121 . 104.7 no C130 . C12 . H121 . 115.9 no C9 . C12 . H122 . 111.8 no C13 . C12 . H122 . 114.8 no C130 . C12 . H122 . 101.2 no H121 . C12 . H122 . 102.5 no C12 . C13 . C14 . 110.82(18) yes C12 . C13 . C140 . 112.8(4) yes C12 . C13 . H1301 . 120.5 no C14 . C13 . H1301 . 127.9 no C140 . C13 . H1301 . 126.7 no C12 . C13 . H131 . 107.7 no C14 . C13 . H131 . 105.1 no C140 . C13 . H131 . 93.8 no C12 . C13 . H132 . 111.2 no C14 . C13 . H132 . 110.2 no C140 . C13 . H132 . 118.0 no H131 . C13 . H132 . 111.6 no C13 . C14 . C15 . 109.26(19) yes C15 . C14 . C130 . 110.3(3) yes C13 . C14 . C150 . 105.1(4) yes C130 . C14 . C150 . 109.5(5) yes C13 . C14 . H141 . 113.6 no C15 . C14 . H141 . 109.8 no C130 . C14 . H141 . 124.9 no C150 . C14 . H141 . 102.1 no C13 . C14 . H142 . 108.3 no C15 . C14 . H142 . 110.0 no C130 . C14 . H142 . 94.2 no C150 . C14 . H142 . 122.1 no H141 . C14 . H142 . 105.8 no C13 . C14 . H1401 . 82.5 no C15 . C14 . H1401 . 105.7 no C130 . C14 . H1401 . 96.8 no C150 . C14 . H1401 . 93.8 no C13 . C14 . H1402 . 135.7 no C15 . C14 . H1402 . 113.1 no C130 . C14 . H1402 . 127.9 no C150 . C14 . H1402 . 118.9 no H142 . C14 . H1401 . 136.1 no H1401 . C14 . H1402 . 97.9 no C14 . C15 . C16 . 110.11(19) yes C16 . C15 . C140 . 109.7(4) yes C14 . C15 . C160 . 109.5(3) yes C140 . C15 . C160 . 106.2(5) yes C14 . C15 . H151 . 109.7 no C16 . C15 . H151 . 110.8 no C140 . C15 . H151 . 100.0 no C160 . C15 . H151 . 98.3 no C14 . C15 . H152 . 107.1 no C16 . C15 . H152 . 109.1 no C140 . C15 . H152 . 117.0 no C160 . C15 . H152 . 121.7 no H151 . C15 . H152 . 109.9 no C14 . C15 . H1501 . 103.9 no C16 . C15 . H1501 . 107.0 no C140 . C15 . H1501 . 93.4 no C160 . C15 . H1501 . 93.5 no C14 . C15 . H1502 . 115.9 no C16 . C15 . H1502 . 115.7 no C140 . C15 . H1502 . 123.7 no C160 . C15 . H1502 . 125.6 no H152 . C15 . H1501 . 119.5 no H1501 . C15 . H1502 . 102.9 no C15 . C16 . C17 . 109.71(19) yes C17 . C16 . C150 . 107.5(4) yes C15 . C16 . H161 . 109.7 no C17 . C16 . H161 . 112.7 no C150 . C16 . H161 . 100.5 no C15 . C16 . H162 . 108.0 no C17 . C16 . H162 . 109.7 no C150 . C16 . H162 . 119.4 no H161 . C16 . H162 . 106.8 no C15 . C16 . H1602 . 115.1 no C17 . C16 . H1602 . 130.8 no C150 . C16 . H1602 . 120.6 no C16 . C17 . H171 . 108.8 no C160 . C17 . H171 . 109.8 no C16 . C17 . H172 . 106.9 no C160 . C17 . H172 . 93.7 no H171 . C17 . H172 . 114.8 no C16 . C17 . H173 . 106.9 no C160 . C17 . H173 . 118.8 no H171 . C17 . H173 . 109.4 no H172 . C17 . H173 . 109.8 no C5 . C18 . C19 . 115.3(3) yes C5 . C18 . H181 . 108.9 no C19 . C18 . H181 . 107.8 no C5 . C18 . H182 . 108.5 no C19 . C18 . H182 . 107.6 no H181 . C18 . H182 . 108.6 no C18 . C19 . C20 . 114.6(3) yes C18 . C19 . H191 . 108.9 no C20 . C19 . H191 . 109.1 no C18 . C19 . H192 . 108.5 no C20 . C19 . H192 . 109.2 no H191 . C19 . H192 . 106.1 no C19 . C20 . C21 . 113.2(4) yes C19 . C20 . H201 . 107.8 no C21 . C20 . H201 . 109.3 no C19 . C20 . H202 . 108.8 no C21 . C20 . H202 . 110.1 no H201 . C20 . H202 . 107.4 no C20 . C21 . C22 . 113.3(4) yes C20 . C21 . H211 . 108.7 no C22 . C21 . H211 . 110.3 no C20 . C21 . H212 . 107.8 no C22 . C21 . H212 . 110.9 no H211 . C21 . H212 . 105.5 no C21 . C22 . C23 . 113.3(5) yes C21 . C22 . H221 . 109.9 no C23 . C22 . H221 . 108.4 no C21 . C22 . H222 . 109.8 no C23 . C22 . H222 . 108.8 no H221 . C22 . H222 . 106.4 no C22 . C23 . H231 . 110.4 no C22 . C23 . H232 . 110.1 no H231 . C23 . H232 . 109.8 no C22 . C23 . H233 . 109.2 no H231 . C23 . H233 . 109.1 no H232 . C23 . H233 . 108.2 no C4 . C24 . H241 . 110.8 no C4 . C24 . H242 . 110.3 no H241 . C24 . H242 . 106.4 no C4 . C24 . H243 . 112.3 no H241 . C24 . H243 . 108.9 no H242 . C24 . H243 . 107.9 no C2 . C25 . C26 . 123.0(3) yes C2 . C25 . C30 . 117.8(3) yes C26 . C25 . C30 . 119.2(3) yes C25 . C26 . C27 . 119.6(4) yes C25 . C26 . H261 . 118.7 no C27 . C26 . H261 . 121.6 no C26 . C27 . F2 . 122.3(6) yes C26 . C27 . C28 . 121.9(4) yes F2 . C27 . C28 . 115.7(6) yes C26 . C27 . H271 . 119.0 no C28 . C27 . H271 . 119.1 no C27 . C28 . C29 . 117.8(4) yes C27 . C28 . H281 . 121.3 no C29 . C28 . H281 . 120.7 no C28 . C29 . F1 . 117.9(4) yes C28 . C29 . C30 . 122.0(3) yes F1 . C29 . C30 . 120.2(4) yes C28 . C29 . H291 . 119.3 no C30 . C29 . H291 . 118.8 no C25 . C30 . C29 . 119.5(4) yes C25 . C30 . H301 . 120.4 no C29 . C30 . H301 . 120.1 no C12 . C130 . C14 . 112.6(4) yes C12 . C130 . C140 . 110.08(18) yes C12 . C130 . H1301 . 109.7 no C14 . C130 . H1301 . 117.8 no C140 . C130 . H1301 . 110.0 no C12 . C130 . H1302 . 109.7 no C14 . C130 . H1302 . 96.3 no C140 . C130 . H1302 . 107.6 no H1301 . C130 . H1302 . 109.8 no C12 . C130 . H132 . 122.7 no C14 . C130 . H132 . 124.6 no C140 . C130 . H132 . 125.8 no C130 . C140 . C15 . 107.0(4) yes C15 . C140 . C13 . 110.3(5) yes C130 . C140 . C150 . 109.73(19) yes C13 . C140 . C150 . 109.6(3) yes C130 . C140 . H141 . 136.1 no C15 . C140 . H141 . 116.9 no C13 . C140 . H141 . 130.6 no C150 . C140 . H141 . 113.3 no C130 . C140 . H1401 . 109.1 no C15 . C140 . H1401 . 121.1 no C13 . C140 . H1401 . 95.5 no C150 . C140 . H1401 . 109.5 no C130 . C140 . H1402 . 110.9 no C15 . C140 . H1402 . 100.4 no C13 . C140 . H1402 . 123.4 no C150 . C140 . H1402 . 109.7 no H1401 . C140 . H1402 . 107.8 no C140 . C150 . C16 . 109.0(3) yes C14 . C150 . C16 . 106.0(5) yes C140 . C150 . C160 . 109.78(19) yes C14 . C150 . C160 . 109.7(4) yes C140 . C150 . H151 . 118.0 no C14 . C150 . H151 . 125.2 no C16 . C150 . H151 . 125.6 no C160 . C150 . H151 . 116.3 no C140 . C150 . H1501 . 109.1 no C14 . C150 . H1501 . 118.6 no C16 . C150 . H1501 . 122.0 no C160 . C150 . H1501 . 109.6 no C140 . C150 . H1502 . 108.5 no C14 . C150 . H1502 . 98.5 no C16 . C150 . H1502 . 97.8 no C160 . C150 . H1502 . 110.4 no H1501 . C150 . H1502 . 109.4 no C150 . C160 . C17 . 109.81(19) yes C17 . C160 . C15 . 107.7(4) yes C150 . C160 . H161 . 117.3 no C17 . C160 . H161 . 130.7 no C15 . C160 . H161 . 121.5 no C150 . C160 . H1601 . 109.5 no C17 . C160 . H1601 . 110.2 no C15 . C160 . H1601 . 120.7 no C150 . C160 . H1602 . 107.9 no C17 . C160 . H1602 . 111.1 no H1601 . C160 . H1602 . 108.2 no