data_ST-4_sq _audit_creation_date 2017-07-14 _audit_creation_method ; Olex2 1.2-alpha (compiled 2017.07.12 svn.r3442 for OlexSys, GUI svn.r5363) ; _shelx_SHELXL_version_number '2014/7' _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_id_orcid ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety '0.06(C3648 H2208 N576 O1040 Zn320)' _chemical_formula_sum 'C228 H138 N36 O65 Zn20' _chemical_formula_weight 5729.14 _chemical_absolute_configuration syn _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0050 0.0020 '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' 0.0090 0.0050 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0160 0.0090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.1740 1.9090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'cubic' _space_group_IT_number 209 _space_group_name_H-M_alt 'F 4 3 2' _space_group_name_Hall 'F 4 2 3' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, -z' '-y, -x, -z' 'y, -x, z' '-y, x, z' 'x, z, -y' '-x, z, y' '-x, -z, -y' 'x, -z, y' 'z, y, -x' 'z, -y, x' '-z, y, x' '-z, -y, -x' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x+1/2, y+1/2' 'z, -x+1/2, -y+1/2' '-z, -x+1/2, y+1/2' '-z, x+1/2, -y+1/2' 'y, z+1/2, x+1/2' '-y, z+1/2, -x+1/2' 'y, -z+1/2, -x+1/2' '-y, -z+1/2, x+1/2' 'y, x+1/2, -z+1/2' '-y, -x+1/2, -z+1/2' 'y, -x+1/2, z+1/2' '-y, x+1/2, z+1/2' 'x, z+1/2, -y+1/2' '-x, z+1/2, y+1/2' '-x, -z+1/2, -y+1/2' 'x, -z+1/2, y+1/2' 'z, y+1/2, -x+1/2' 'z, -y+1/2, x+1/2' '-z, y+1/2, x+1/2' '-z, -y+1/2, -x+1/2' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+1/2, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'z+1/2, x, y+1/2' 'z+1/2, -x, -y+1/2' '-z+1/2, -x, y+1/2' '-z+1/2, x, -y+1/2' 'y+1/2, z, x+1/2' '-y+1/2, z, -x+1/2' 'y+1/2, -z, -x+1/2' '-y+1/2, -z, x+1/2' 'y+1/2, x, -z+1/2' '-y+1/2, -x, -z+1/2' 'y+1/2, -x, z+1/2' '-y+1/2, x, z+1/2' 'x+1/2, z, -y+1/2' '-x+1/2, z, y+1/2' '-x+1/2, -z, -y+1/2' 'x+1/2, -z, y+1/2' 'z+1/2, y, -x+1/2' 'z+1/2, -y, x+1/2' '-z+1/2, y, x+1/2' '-z+1/2, -y, -x+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'z+1/2, x+1/2, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x+1/2, y' '-z+1/2, x+1/2, -y' 'y+1/2, z+1/2, x' '-y+1/2, z+1/2, -x' 'y+1/2, -z+1/2, -x' '-y+1/2, -z+1/2, x' 'y+1/2, x+1/2, -z' '-y+1/2, -x+1/2, -z' 'y+1/2, -x+1/2, z' '-y+1/2, x+1/2, z' 'x+1/2, z+1/2, -y' '-x+1/2, z+1/2, y' '-x+1/2, -z+1/2, -y' 'x+1/2, -z+1/2, y' 'z+1/2, y+1/2, -x' 'z+1/2, -y+1/2, x' '-z+1/2, y+1/2, x' '-z+1/2, -y+1/2, -x' _cell_length_a 77.569(9) _cell_length_b 77.569(9) _cell_length_c 77.569(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 466729(162) _cell_formula_units_Z 16 _cell_measurement_reflns_used 15653 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 26.077 _cell_measurement_theta_min 1.331 _shelx_estimated_absorpt_T_max 0.928 _shelx_estimated_absorpt_T_min 0.928 _exptl_absorpt_coefficient_mu 0.632 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_correction_T_min 0.928 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 0.326 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description cube _exptl_crystal_F_000 46048 _exptl_crystal_preparation ? _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_unetI/netI 0.0370 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 82 _diffrn_reflns_limit_h_min 3 _diffrn_reflns_limit_k_max 58 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 57 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 25164 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 26.077 _diffrn_reflns_theta_max 26.077 _diffrn_reflns_theta_min 1.331 _diffrn_ambient_temperature 298(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type SSRF _diffrn_measurement_method '\w scans' _diffrn_radiation_type ? _diffrn_radiation_wavelength 0.8265 _diffrn_source ? _reflns_Friedel_coverage 0.814 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 1.000 _reflns_number_gt 15653 _reflns_number_total 24546 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XT (Sheldrick, 2015)' _refine_diff_density_max 0.053 _refine_diff_density_min -0.063 _refine_diff_density_rms 0.008 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.494(5) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 524 _refine_ls_number_reflns 24546 _refine_ls_number_restraints 348 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_gt 0.0345 _refine_ls_restrained_S_all 0.962 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+42.5788P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0817 _refine_ls_wR_factor_ref 0.0901 _refine_special_details ; Refined as a 2-component inversion twin. ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.506(5) 0.494(5) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H) groups 3. Restrained distances O12_$1-C37 \\sim O12-C37 \\sim O13-C46 \\sim O13_$1-C46 with sigma of 0.02 O12-C38 \\sim C38-O12_$1 \\sim C45-O13 \\sim C45-O13_$1 with sigma of 0.02 O13_$1-C45 \\sim O13-C45 \\sim C39-C39_$1 \\sim C39_$1-C41 \\sim C41-C39 \\sim C38-C40_$1 ~ C40_$1-C40 \\sim C40-C38 \\sim C42-C44 \\sim C42-C44_$1 \\sim C44_$1-C44 \\sim C43-C43_$1 \\sim C43_$1- C45 \\sim C45-C43 with sigma of 0.02 C39_$1-C38 \\sim C39-C38 \\sim C39-C40 \\sim C40-C41 \\sim C40_$1-C41 \\sim C39_$1-C40_$1 ~ C43_$1-C42 \\sim C43-C42 \\sim C43-C44 \\sim C44-C45 \\sim C44_$1-C45 \\sim C43_$1-C44_$1 with sigma of 0.02 C41-C42 \\sim C37-C38 \\sim C45-C46 with sigma of 0.02 4. Restrained planarity O12_$1, C40_$1, C39_$1, C38, C37, C41, C40, C39, O12 with sigma of 0.1 C44_$1, C43_$1, O13_$1, C45, C42, C44, C43, C46, O13 with sigma of 0.1 C45, C42, C44_$1, C44, C43_$1, C43, C46, O13_$1, O13 with sigma of 0.1 5. Uiso/Uaniso restraints and constraints Uanis(O12) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O12) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 6. Rigid body (RIGU) restrains O12, O12, C38, C37, C41, C40, C40, C39, C39, C45, C42, C44, C44, C43, C43, C46, O13, O13 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 7. Others Fixed Sof: O12(0.5) C38(0.25) C37(0.25) C41(0.25) C40(0.5) H40(0.5) C39(0.5) H39(0.5) C45(0.25) C42(0.25) C44(0.5) H44(0.5) C43(0.5) H43(0.5) C46(0.25) O13(0.5) 8.a Riding coordinates: N4(H4A), N5(H5), N6(H6A) 8.b Aromatic/amide H refined with riding coordinates: C7(H7), C6(H6), C4(H4), C3(H3), C34(H34), C11(H11), C10(H10), C14(H14), C13(H13), C27(H27), C35(H35), C28(H28), C18(H18), C17(H17), C21(H21), C20(H20), C31(H31), C30(H30), C40(H40), C39(H39), C44(H44), C43(H43) 8.c Fitted hexagon refined as free rotating group: C2(C7,C6,C5,C4,C3), C12(C11,C10,C9,C14,C13), C19(C18,C17,C16,C21,C20), C22(N1, C24,N3,C23,N2) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary ? _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.62162(2) 0.59636(2) 0.87235(2) 0.12537(16) Uani 1 1 d . . . . . Zn2 Zn 0.59576(2) 0.59576(2) 0.90424(2) 0.1384(3) Uani 1 3 d S T P . . Zn3 Zn 0.66808(2) 0.49529(2) 0.69586(2) 0.14092(18) Uani 1 1 d . . . . . Zn4 Zn 0.66507(2) 0.48019(2) 0.65800(2) 0.1523(2) Uani 1 1 d . . . . . O1 O 0.61051(3) 0.61051(3) 0.88949(3) 0.1103(11) Uani 1 3 d S T P . . O2 O 0.67180(3) 0.5000 0.67180(3) 0.1273(10) Uani 1 2 d S T P . . O11 O 0.68995(4) 0.49359(5) 0.70828(4) 0.1750(12) Uani 1 1 d . . . . . O3 O 0.61423(4) 0.60257(5) 0.84961(3) 0.1681(11) Uani 1 1 d . . . . . O5 O 0.52671(5) 0.65718(5) 0.69955(5) 0.1872(14) Uani 1 1 d . . . . . O9 O 0.61634(6) 0.57197(5) 0.87563(6) 0.1912(15) Uani 1 1 d . . . . . O7 O 0.65055(5) 0.53106(5) 0.68584(5) 0.2032(14) Uani 1 1 d . . . . . O4 O 0.59800(4) 0.62610(4) 0.85350(4) 0.1745(12) Uani 1 1 d . . . . . O10 O 0.60044(5) 0.57222(5) 0.89897(5) 0.1970(15) Uani 1 1 d . . . . . O8 O 0.65670(5) 0.51424(6) 0.70778(5) 0.2044(15) Uani 1 1 d . . . . . O6 O 0.53615(5) 0.65306(5) 0.67306(5) 0.2045(15) Uani 1 1 d . . . . . C32 C 0.70400(7) 0.5000 0.70400(7) 0.153(2) Uani 1 2 d S T P . . C15 C 0.65134(7) 0.52817(10) 0.70203(8) 0.185(2) Uani 1 1 d . . . . . C8 C 0.53712(9) 0.65138(7) 0.68873(8) 0.182(2) Uani 1 1 d . . . . . C33 C 0.71773(8) 0.5000 0.71773(8) 0.188(3) Uani 1 2 d S T P . . C1 C 0.60520(7) 0.61527(8) 0.84448(6) 0.1676(18) Uani 1 1 d . . . . . O12 O 0.64975(7) 0.48539(10) 0.63949(7) 0.173(2) Uani 0.5 1 d D U . . . C26 C 0.60902(8) 0.54625(8) 0.88734(10) 0.188(2) Uani 1 1 d . . . . . C2 C 0.60187(6) 0.61623(6) 0.82519(4) 0.192(2) Uani 1 1 d . . . . . C7 C 0.60967(5) 0.60431(5) 0.81432(6) 0.238(3) Uani 1 1 d G . . . . H7 H 0.6168 0.5958 0.8189 0.286 Uiso 1 1 calc R . . . . C6 C 0.60683(6) 0.60511(6) 0.79664(5) 0.267(4) Uani 1 1 d G . . . . H6 H 0.6120 0.5971 0.7894 0.320 Uiso 1 1 calc R . . . . C5 C 0.59618(7) 0.61782(7) 0.78985(4) 0.256(4) Uani 1 1 d G . . . . C4 C 0.58838(6) 0.62973(6) 0.80072(6) 0.266(4) Uani 1 1 d G . . . . H4 H 0.5812 0.6382 0.7962 0.319 Uiso 1 1 calc R . . . . C3 C 0.59122(6) 0.62894(5) 0.81840(5) 0.241(3) Uani 1 1 d G . . . . H3 H 0.5860 0.6369 0.8257 0.289 Uiso 1 1 calc R . . . . C34 C 0.71425(7) 0.49482(9) 0.73388(8) 0.225(3) Uani 1 1 d . . . . . H34 H 0.7034 0.4905 0.7365 0.270 Uiso 1 1 calc R . . . . C36 C 0.74316(6) 0.5000 0.74316(6) 0.183(3) Uani 1 2 d S T P . . N4 N 0.59112(9) 0.61885(9) 0.77349(6) 0.335(5) Uani 1 1 d . . . . . H4A H 0.5830 0.6261 0.7715 0.402 Uiso 1 1 d R . . . . C12 C 0.57846(7) 0.62156(8) 0.70885(6) 0.313(5) Uani 1 1 d . . . . . C11 C 0.57618(7) 0.62268(7) 0.69111(5) 0.353(6) Uani 1 1 d G . . . . H11 H 0.5837 0.6170 0.6837 0.424 Uiso 1 1 calc R . . . . C10 C 0.56258(7) 0.63223(7) 0.68441(4) 0.279(4) Uani 1 1 d G . . . . H10 H 0.5611 0.6330 0.6725 0.335 Uiso 1 1 calc R . . . . C9 C 0.55126(6) 0.64067(6) 0.69545(6) 0.217(3) Uani 1 1 d G . . . . C14 C 0.55354(6) 0.63955(6) 0.71319(6) 0.235(3) Uani 1 1 d G . . . . H14 H 0.5460 0.6452 0.7206 0.282 Uiso 1 1 calc R . . . . C13 C 0.56714(8) 0.63000(8) 0.71989(4) 0.355(6) Uani 1 1 d G . . . . H13 H 0.5687 0.6292 0.7318 0.426 Uiso 1 1 calc R . . . . N5 N 0.59047(9) 0.60996(9) 0.71446(5) 0.340(5) Uani 1 1 d . . . . . H5 H 0.5956 0.6045 0.7063 0.408 Uiso 1 1 d R . . . . N6 N 0.62493(11) 0.57594(10) 0.74902(7) 0.406(6) Uani 1 1 d . . . . . H6A H 0.6295 0.5751 0.7591 1.2(3) Uiso 1 1 d R . . . . C27 C 0.61724(10) 0.53672(8) 0.87519(10) 0.243(3) Uani 1 1 d . . . . . H27 H 0.6224 0.5427 0.8662 0.291 Uiso 1 1 calc R . . . . C35 C 0.72695(7) 0.49592(11) 0.74696(8) 0.247(3) Uani 1 1 d . . . . . H35 H 0.7239 0.4938 0.7584 0.297 Uiso 1 1 calc R . . . . C28 C 0.61861(10) 0.51861(8) 0.87498(10) 0.253(3) Uani 1 1 d . . . . . H28 H 0.6244 0.5128 0.8662 0.303 Uiso 1 1 calc R . . . . C19 C 0.63024(7) 0.56373(7) 0.73662(6) 0.268(4) Uani 1 1 d . . . . . C18 C 0.63876(7) 0.54926(8) 0.74289(4) 0.339(6) Uani 1 1 d G . . . . H18 H 0.6398 0.5476 0.7547 0.407 Uiso 1 1 calc R . . . . C17 C 0.64572(7) 0.53733(6) 0.73149(7) 0.291(4) Uani 1 1 d G . . . . H17 H 0.6514 0.5276 0.7357 0.350 Uiso 1 1 calc R . . . . C16 C 0.64417(6) 0.53985(6) 0.71381(6) 0.213(3) Uani 1 1 d G . . . . C21 C 0.63565(7) 0.55432(7) 0.70755(4) 0.275(4) Uani 1 1 d G . . . . H21 H 0.6346 0.5560 0.6957 0.330 Uiso 1 1 calc R . . . . C20 C 0.62869(7) 0.56626(6) 0.71895(7) 0.324(5) Uani 1 1 d G . . . . H20 H 0.6230 0.5759 0.7148 0.388 Uiso 1 1 calc R . . . . C31 C 0.60107(12) 0.53671(10) 0.89941(11) 0.279(4) Uani 1 1 d . . . . . H31 H 0.5950 0.5426 0.9079 0.334 Uiso 1 1 calc R . . . . C22 C 0.59657(7) 0.61010(6) 0.76006(4) 0.295(4) Uani 1 1 d . . . . . N1 N 0.60849(7) 0.59679(6) 0.76144(4) 0.306(4) Uani 1 1 d G . . . . C24 C 0.61398(7) 0.58813(7) 0.74675(6) 0.372(7) Uani 1 1 d G . . . . N3 N 0.60756(8) 0.59278(7) 0.73067(4) 0.359(5) Uani 1 1 d G . . . . C23 C 0.59564(7) 0.60609(7) 0.72930(4) 0.305(5) Uani 1 1 d G . . . . N2 N 0.59015(6) 0.61475(6) 0.74399(5) 0.310(4) Uani 1 1 d G . . . . C30 C 0.60109(12) 0.51926(10) 0.90023(11) 0.305(5) Uani 1 1 d . . . . . H30 H 0.5945 0.5138 0.9086 0.366 Uiso 1 1 calc R . . . . C25 C 0.60897(8) 0.56434(8) 0.88772(11) 0.177(2) Uani 1 1 d . . . . . C29 C 0.61061(9) 0.50958(7) 0.88892(11) 0.206(2) Uani 1 1 d . . . . . C38 C 0.62610(9) 0.5000 0.62610(9) 0.265(9) Uani 0.5 2 d DS TU P . . C37 C 0.64022(13) 0.5000 0.64022(13) 0.204(7) Uani 0.5 2 d DS TU P . . C41 C 0.60097(12) 0.5000 0.60097(12) 0.274(10) Uani 0.5 2 d DS TU P . . C40 C 0.61332(18) 0.48737(17) 0.60097(18) 0.376(13) Uani 0.5 1 d D U . . . H40 H 0.6135 0.4791 0.5923 0.451 Uiso 0.5 1 calc R . . . . C39 C 0.62561(14) 0.48692(12) 0.61406(14) 0.296(8) Uani 0.5 1 d D U . . . H39 H 0.6334 0.4779 0.6147 0.355 Uiso 0.5 1 calc R . . A . C45 C 0.56200(13) 0.5000 0.56200(13) 0.400(19) Uani 0.5 2 d DS TU P A 2 C42 C 0.58694(14) 0.5000 0.58694(14) 0.338(14) Uani 0.5 2 d DS TU P A 2 C44 C 0.57535(17) 0.48831(16) 0.56097(17) 0.406(14) Uani 0.5 1 d D U . A 2 H44 H 0.5759 0.4806 0.5518 0.487 Uiso 0.5 1 calc R . . A 2 C43 C 0.58786(19) 0.48814(17) 0.57367(18) 0.380(13) Uani 0.5 1 d D U . A 2 H43 H 0.5968 0.4802 0.5733 0.456 Uiso 0.5 1 calc R . . A 2 C46 C 0.5479(2) 0.5000 0.5479(2) 0.47(3) Uani 0.5 2 d DS TU P A 2 O13 O 0.5512(2) 0.4881(2) 0.5358(2) 0.60(2) Uani 0.5 1 d D U . A 2 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 0.1286(3) 0.1181(3) 0.1294(3) -0.0114(2) -0.0123(3) 0.0150(3) Zn2 0.1384(3) 0.1384(3) 0.1384(3) -0.0013(3) -0.0013(3) 0.0013(3) Zn3 0.1367(4) 0.1674(4) 0.1186(3) -0.0023(3) 0.0007(3) 0.0056(3) Zn4 0.1354(4) 0.1941(5) 0.1273(4) -0.0114(3) 0.0158(3) -0.0227(3) O1 0.1103(11) 0.1103(11) 0.1103(11) -0.0064(12) -0.0064(12) 0.0064(12) O2 0.1013(13) 0.179(3) 0.1013(13) 0.0076(13) 0.0090(17) -0.0076(13) O11 0.151(3) 0.220(3) 0.154(3) 0.005(2) -0.019(2) -0.013(2) O3 0.192(3) 0.189(3) 0.123(2) -0.0055(19) -0.0244(19) 0.056(2) O5 0.233(4) 0.194(3) 0.134(3) -0.018(2) -0.039(2) 0.070(3) O9 0.246(4) 0.115(3) 0.213(4) -0.017(2) -0.003(3) -0.008(2) O7 0.218(3) 0.231(4) 0.160(3) 0.001(3) 0.035(3) 0.076(3) O4 0.220(3) 0.188(3) 0.116(2) -0.030(2) -0.020(2) 0.054(2) O10 0.231(4) 0.139(3) 0.221(4) -0.012(2) 0.021(3) 0.017(2) O8 0.220(4) 0.245(4) 0.149(3) -0.021(3) 0.018(2) 0.071(3) O6 0.265(4) 0.203(3) 0.146(3) -0.008(2) -0.031(3) 0.080(3) C32 0.135(3) 0.191(7) 0.135(3) -0.010(4) -0.017(6) 0.010(4) C15 0.169(4) 0.253(7) 0.134(5) 0.027(5) 0.010(4) 0.089(4) C8 0.251(7) 0.184(5) 0.111(4) -0.018(4) -0.041(4) 0.046(4) C33 0.137(3) 0.289(10) 0.137(3) -0.003(4) -0.009(6) 0.003(4) C1 0.199(5) 0.189(5) 0.115(4) -0.015(4) -0.020(3) 0.046(4) O12 0.142(5) 0.268(8) 0.110(4) 0.019(4) -0.028(3) -0.008(4) C26 0.221(6) 0.109(5) 0.233(7) 0.006(5) 0.049(4) 0.009(4) C2 0.212(5) 0.252(6) 0.112(4) -0.006(4) -0.021(3) 0.094(4) C7 0.320(8) 0.269(6) 0.126(4) -0.052(4) -0.043(4) 0.168(6) C6 0.320(8) 0.350(9) 0.131(5) -0.028(5) -0.035(4) 0.205(7) C5 0.339(8) 0.324(8) 0.105(4) -0.030(5) -0.033(4) 0.201(7) C4 0.369(9) 0.290(7) 0.140(5) -0.037(5) -0.032(5) 0.207(7) C3 0.332(8) 0.259(6) 0.131(4) -0.021(4) -0.023(4) 0.169(6) C34 0.159(5) 0.361(9) 0.154(5) 0.042(5) -0.027(4) -0.018(5) C36 0.139(3) 0.271(9) 0.139(3) 0.021(4) -0.022(5) -0.021(4) N4 0.463(9) 0.428(9) 0.115(3) -0.079(4) -0.040(4) 0.316(8) C12 0.368(9) 0.446(12) 0.126(5) -0.025(6) -0.044(5) 0.279(9) C11 0.492(13) 0.446(11) 0.122(5) -0.033(5) -0.046(6) 0.349(11) C10 0.339(9) 0.346(9) 0.153(5) -0.036(5) -0.021(5) 0.199(8) C9 0.283(7) 0.214(5) 0.153(5) -0.031(4) -0.036(5) 0.116(5) C14 0.285(7) 0.309(7) 0.112(4) -0.038(4) -0.038(4) 0.173(6) C13 0.526(14) 0.425(11) 0.113(4) -0.032(5) -0.015(6) 0.326(11) N5 0.467(9) 0.447(9) 0.105(3) -0.042(4) -0.074(4) 0.322(8) N6 0.578(12) 0.484(10) 0.155(4) -0.038(5) -0.033(5) 0.446(10) C27 0.340(9) 0.102(4) 0.286(8) 0.003(4) 0.061(7) -0.004(5) C35 0.171(5) 0.417(10) 0.154(5) 0.006(5) -0.032(5) -0.015(6) C28 0.364(10) 0.121(5) 0.273(8) -0.011(5) 0.045(7) 0.001(5) C19 0.316(8) 0.340(9) 0.148(5) -0.028(6) 0.008(5) 0.173(7) C18 0.446(12) 0.397(10) 0.173(5) -0.048(6) -0.057(6) 0.328(10) C17 0.344(9) 0.369(10) 0.160(6) -0.024(6) -0.026(5) 0.233(8) C16 0.245(6) 0.262(7) 0.132(5) -0.027(4) -0.003(4) 0.128(5) C21 0.342(9) 0.332(9) 0.152(5) -0.018(5) -0.018(5) 0.200(7) C20 0.456(12) 0.384(10) 0.131(5) -0.009(5) 0.028(6) 0.300(9) C31 0.390(11) 0.128(5) 0.319(10) -0.012(6) 0.105(8) 0.040(6) C22 0.370(10) 0.358(10) 0.158(6) 0.008(6) -0.045(6) 0.222(8) N1 0.440(9) 0.350(7) 0.129(3) -0.033(4) -0.047(4) 0.269(7) C24 0.446(12) 0.544(16) 0.126(5) -0.042(7) -0.028(6) 0.342(12) N3 0.494(10) 0.475(10) 0.109(3) -0.055(4) -0.050(4) 0.352(9) C23 0.393(10) 0.369(10) 0.154(6) -0.058(6) -0.029(6) 0.259(9) N2 0.420(8) 0.376(7) 0.134(3) -0.047(4) -0.056(4) 0.287(7) C30 0.448(12) 0.128(5) 0.340(10) -0.024(6) 0.194(9) -0.018(6) C25 0.182(6) 0.104(5) 0.244(8) -0.004(4) -0.003(5) 0.007(4) C29 0.244(6) 0.118(4) 0.258(7) -0.011(5) 0.029(5) -0.009(4) C38 0.250(13) 0.294(19) 0.250(13) -0.019(12) -0.143(14) 0.019(12) C37 0.179(9) 0.254(15) 0.179(9) -0.003(8) -0.073(11) 0.003(8) C41 0.282(14) 0.258(19) 0.282(14) 0.018(12) -0.116(16) -0.018(12) C40 0.40(2) 0.40(2) 0.324(18) -0.119(17) -0.233(17) 0.131(17) C39 0.323(16) 0.310(16) 0.254(14) -0.047(11) -0.155(13) 0.042(12) C45 0.42(2) 0.37(3) 0.42(2) -0.07(2) -0.20(2) 0.07(2) C42 0.345(19) 0.32(3) 0.345(19) -0.008(17) -0.17(2) 0.008(17) C44 0.42(3) 0.41(3) 0.40(2) -0.087(19) -0.21(2) 0.090(19) C43 0.40(2) 0.38(2) 0.36(2) -0.046(17) -0.192(18) 0.064(18) C46 0.48(3) 0.45(4) 0.48(3) -0.17(3) -0.25(3) 0.17(3) O13 0.62(3) 0.64(3) 0.55(3) -0.30(3) -0.34(2) 0.33(3) _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 Zn1 Zn1 3.1538(8) 35_566 ? Zn1 Zn1 3.1540(8) 56_656 ? Zn1 O1 1.9271(13) . ? Zn1 O3 1.917(3) . ? Zn1 O9 1.952(4) . ? Zn1 O4 1.938(3) 56_656 ? Zn2 O1 1.982(4) . ? Zn2 O10 1.906(4) . ? Zn2 O10 1.906(4) 35_566 ? Zn2 O10 1.906(4) 56_656 ? Zn3 Zn3 3.1328(10) 22_565 ? Zn3 Zn4 3.1518(8) 22_565 ? Zn3 O2 1.9234(18) . ? Zn3 O11 1.955(4) . ? Zn3 O5 1.926(4) 15_565 ? Zn3 O8 1.948(4) . ? Zn4 Zn3 3.1516(8) 22_565 ? Zn4 O2 1.9440(19) . ? Zn4 O7 1.922(4) 22_565 ? Zn4 O6 1.959(4) 15_565 ? Zn4 O12 1.907(5) . ? O1 Zn1 1.9270(13) 35_566 ? O1 Zn1 1.9270(13) 56_656 ? O2 Zn3 1.9234(18) 22_565 ? O2 Zn4 1.9444(19) 22_565 ? O11 C32 1.243(4) . ? O3 C1 1.272(5) . ? O5 Zn3 1.927(4) 16_655 ? O5 C8 1.249(6) . ? O9 C25 1.248(6) . ? O7 Zn4 1.922(4) 22_565 ? O7 C15 1.277(5) . ? O4 Zn1 1.938(3) 35_566 ? O4 C1 1.228(5) . ? O10 C25 1.254(6) . ? O8 C15 1.241(6) . ? O6 Zn4 1.959(4) 16_655 ? O6 C8 1.225(5) . ? C32 O11 1.243(4) 22_565 ? C32 C33 1.507(10) . ? C15 C16 1.402(7) . ? C8 C9 1.471(6) . ? C33 C34 1.343(6) 22_565 ? C33 C34 1.343(6) . ? C1 C2 1.520(5) . ? O12 C37 1.354(7) . ? C26 C27 1.357(7) . ? C26 C31 1.343(8) . ? C26 C25 1.404(7) . ? C2 C7 1.3900 . ? C2 C3 1.3900 . ? C7 H7 0.9300 . ? C7 C6 1.3900 . ? C6 H6 0.9300 . ? C6 C5 1.3900 . ? C5 C4 1.3900 . ? C5 N4 1.331(5) . ? C4 H4 0.9300 . ? C4 C3 1.3900 . ? C3 H3 0.9300 . ? C34 H34 0.9300 . ? C34 C35 1.417(7) . ? C36 C36 1.500(14) 51_656 ? C36 C35 1.330(6) 22_565 ? C36 C35 1.329(6) . ? N4 H4A 0.8590 . ? N4 C22 1.313(4) . ? C12 C11 1.3900 . ? C12 C13 1.3900 . ? C12 N5 1.367(5) . ? C11 H11 0.9300 . ? C11 C10 1.3900 . ? C10 H10 0.9300 . ? C10 C9 1.3900 . ? C9 C14 1.3900 . ? C14 H14 0.9300 . ? C14 C13 1.3900 . ? C13 H13 0.9300 . ? N5 H5 0.8591 . ? N5 C23 1.255(4) . ? N6 H6A 0.8602 . ? N6 C19 1.411(6) . ? N6 C24 1.283(5) . ? C27 H27 0.9300 . ? C27 C28 1.409(7) . ? C35 H35 0.9300 . ? C28 H28 0.9300 . ? C28 C29 1.430(7) . ? C19 C18 1.3900 . ? C19 C20 1.3900 . ? C18 H18 0.9300 . ? C18 C17 1.3900 . ? C17 H17 0.9300 . ? C17 C16 1.3900 . ? C16 C21 1.3900 . ? C21 H21 0.9300 . ? C21 C20 1.3900 . ? C20 H20 0.9300 . ? C31 H31 0.9300 . ? C31 C30 1.355(8) . ? C22 N1 1.3900 . ? C22 N2 1.3900 . ? N1 C24 1.3900 . ? C24 N3 1.3900 . ? N3 C23 1.3900 . ? C23 N2 1.3900 . ? C30 H30 0.9300 . ? C30 C29 1.371(7) . ? C29 C29 1.487(10) 72_666 ? C38 C37 1.549(16) . ? C38 C39 1.379(8) . ? C38 C39 1.379(8) 22_565 ? C37 O12 1.354(7) 22_565 ? C41 C40 1.370(8) 22_565 ? C41 C40 1.370(8) . ? C41 C42 1.540(17) . ? C40 H40 0.9300 . ? C40 C39 1.394(10) . ? C39 H39 0.9300 . ? C45 C44 1.379(9) 22_565 ? C45 C44 1.379(9) . ? C45 C46 1.54(2) . ? C42 C43 1.382(9) 22_565 ? C42 C43 1.382(9) . ? C44 H44 0.9300 . ? C44 C43 1.383(11) . ? C43 H43 0.9300 . ? C46 O13 1.342(12) 22_565 ? C46 O13 1.342(12) . ? 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 Zn1 Zn1 Zn1 59.999(2) 35_566 56_656 ? O1 Zn1 Zn1 35.08(5) . 35_566 ? O1 Zn1 Zn1 35.08(5) . 56_656 ? O1 Zn1 O9 111.64(17) . . ? O1 Zn1 O4 111.41(11) . 56_656 ? O3 Zn1 Zn1 75.95(10) . 35_566 ? O3 Zn1 Zn1 126.62(10) . 56_656 ? O3 Zn1 O1 110.98(11) . . ? O3 Zn1 O9 107.52(16) . . ? O3 Zn1 O4 109.76(14) . 56_656 ? O9 Zn1 Zn1 122.20(12) . 56_656 ? O9 Zn1 Zn1 126.60(13) . 35_566 ? O4 Zn1 Zn1 123.99(10) 56_656 35_566 ? O4 Zn1 Zn1 76.35(10) 56_656 56_656 ? O4 Zn1 O9 105.32(16) 56_656 . ? O10 Zn2 O1 108.62(13) 35_566 . ? O10 Zn2 O1 108.62(13) . . ? O10 Zn2 O1 108.62(13) 56_656 . ? O10 Zn2 O10 110.31(12) 35_566 . ? O10 Zn2 O10 110.32(12) 56_656 . ? O10 Zn2 O10 110.31(12) 56_656 35_566 ? Zn3 Zn3 Zn4 60.600(15) 22_565 22_565 ? O2 Zn3 Zn3 35.47(7) . 22_565 ? O2 Zn3 Zn4 35.64(4) . 22_565 ? O2 Zn3 O11 111.17(12) . . ? O2 Zn3 O5 112.23(12) . 15_565 ? O2 Zn3 O8 112.66(13) . . ? O11 Zn3 Zn3 75.99(10) . 22_565 ? O11 Zn3 Zn4 129.02(10) . 22_565 ? O5 Zn3 Zn3 127.65(13) 15_565 22_565 ? O5 Zn3 Zn4 122.57(11) 15_565 22_565 ? O5 Zn3 O11 104.35(15) 15_565 . ? O5 Zn3 O8 113.49(18) 15_565 . ? O8 Zn3 Zn3 117.54(13) . 22_565 ? O8 Zn3 Zn4 77.99(13) . 22_565 ? O8 Zn3 O11 102.14(17) . . ? O2 Zn4 Zn3 35.21(4) . 22_565 ? O2 Zn4 O6 108.10(12) . 15_565 ? O7 Zn4 Zn3 73.34(12) 22_565 22_565 ? O7 Zn4 O2 107.43(13) 22_565 . ? O7 Zn4 O6 106.51(18) 22_565 15_565 ? O6 Zn4 Zn3 127.05(11) 15_565 22_565 ? O12 Zn4 Zn3 122.1(2) . 22_565 ? O12 Zn4 O2 114.5(2) . . ? O12 Zn4 O7 113.1(2) . 22_565 ? O12 Zn4 O6 106.8(2) . 15_565 ? Zn1 O1 Zn1 109.84(10) 56_656 35_566 ? Zn1 O1 Zn1 109.84(10) 56_656 . ? Zn1 O1 Zn1 109.83(10) 35_566 . ? Zn1 O1 Zn2 109.10(10) 56_656 . ? Zn1 O1 Zn2 109.11(10) . . ? Zn1 O1 Zn2 109.10(10) 35_566 . ? Zn3 O2 Zn3 109.05(15) . 22_565 ? Zn3 O2 Zn4 109.15(2) . 22_565 ? Zn3 O2 Zn4 110.13(2) 22_565 22_565 ? Zn3 O2 Zn4 109.16(2) 22_565 . ? Zn3 O2 Zn4 110.12(2) . . ? Zn4 O2 Zn4 109.22(15) . 22_565 ? C32 O11 Zn3 127.0(4) . . ? C1 O3 Zn1 130.3(3) . . ? C8 O5 Zn3 129.1(4) . 16_655 ? C25 O9 Zn1 130.8(4) . . ? C15 O7 Zn4 136.9(4) . 22_565 ? C1 O4 Zn1 129.7(3) . 35_566 ? C25 O10 Zn2 135.8(4) . . ? C15 O8 Zn3 129.7(4) . . ? C8 O6 Zn4 133.0(4) . 16_655 ? O11 C32 O11 128.9(7) . 22_565 ? O11 C32 C33 115.5(4) . . ? O11 C32 C33 115.5(4) 22_565 . ? O7 C15 C16 120.6(6) . . ? O8 C15 O7 121.5(6) . . ? O8 C15 C16 117.5(6) . . ? O5 C8 C9 116.6(5) . . ? O6 C8 O5 126.1(6) . . ? O6 C8 C9 117.2(6) . . ? C34 C33 C32 121.2(4) . . ? C34 C33 C32 121.2(4) 22_565 . ? C34 C33 C34 117.7(8) 22_565 . ? O3 C1 C2 116.0(5) . . ? O4 C1 O3 127.0(5) . . ? O4 C1 C2 116.7(5) . . ? C37 O12 Zn4 119.0(8) . . ? C27 C26 C25 124.1(7) . . ? C31 C26 C27 113.6(6) . . ? C31 C26 C25 122.3(7) . . ? C7 C2 C1 119.4(4) . . ? C7 C2 C3 120.0 . . ? C3 C2 C1 120.6(4) . . ? C2 C7 H7 120.0 . . ? C2 C7 C6 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C6 H6 120.0 . . ? C5 C6 C7 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C5 C4 120.0 . . ? N4 C5 C6 125.4(4) . . ? N4 C5 C4 114.2(4) . . ? C5 C4 H4 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 H4 120.0 . . ? C2 C3 H3 120.0 . . ? C4 C3 C2 120.0 . . ? C4 C3 H3 120.0 . . ? C33 C34 H34 119.7 . . ? C33 C34 C35 120.7(7) . . ? C35 C34 H34 119.7 . . ? C35 C36 C36 120.8(4) 22_565 51_656 ? C35 C36 C36 120.8(4) . 51_656 ? C35 C36 C35 118.4(8) . 22_565 ? C5 N4 H4A 115.5 . . ? C22 N4 C5 129.1(4) . . ? C22 N4 H4A 115.4 . . ? C11 C12 C13 120.0 . . ? N5 C12 C11 116.3(4) . . ? N5 C12 C13 123.0(4) . . ? C12 C11 H11 120.0 . . ? C10 C11 C12 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C10 H10 120.0 . . ? C11 C10 C9 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C9 C8 121.2(4) . . ? C10 C9 C14 120.0 . . ? C14 C9 C8 118.7(4) . . ? C9 C14 H14 120.0 . . ? C13 C14 C9 120.0 . . ? C13 C14 H14 120.0 . . ? C12 C13 H13 120.0 . . ? C14 C13 C12 120.0 . . ? C14 C13 H13 120.0 . . ? C12 N5 H5 114.0 . . ? C23 N5 C12 131.9(4) . . ? C23 N5 H5 114.1 . . ? C19 N6 H6A 116.7 . . ? C24 N6 H6A 116.8 . . ? C24 N6 C19 126.4(5) . . ? C26 C27 H27 117.0 . . ? C26 C27 C28 125.9(7) . . ? C28 C27 H27 117.0 . . ? C34 C35 H35 119.6 . . ? C36 C35 C34 120.9(7) . . ? C36 C35 H35 119.6 . . ? C27 C28 H28 121.7 . . ? C27 C28 C29 116.5(6) . . ? C29 C28 H28 121.7 . . ? C18 C19 N6 116.3(4) . . ? C18 C19 C20 120.0 . . ? C20 C19 N6 123.5(4) . . ? C19 C18 H18 120.0 . . ? C17 C18 C19 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C17 H17 120.0 . . ? C18 C17 C16 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C16 C15 121.2(5) . . ? C21 C16 C15 118.8(5) . . ? C21 C16 C17 120.0 . . ? C16 C21 H21 120.0 . . ? C16 C21 C20 120.0 . . ? C20 C21 H21 120.0 . . ? C19 C20 H20 120.0 . . ? C21 C20 C19 120.0 . . ? C21 C20 H20 120.0 . . ? C26 C31 H31 117.2 . . ? C26 C31 C30 125.6(7) . . ? C30 C31 H31 117.2 . . ? N4 C22 N1 122.5(3) . . ? N4 C22 N2 117.5(3) . . ? N2 C22 N1 120.0 . . ? C24 N1 C22 120.0 . . ? N6 C24 N1 116.5(4) . . ? N6 C24 N3 123.5(4) . . ? N1 C24 N3 120.0 . . ? C23 N3 C24 120.0 . . ? N5 C23 N3 117.4(4) . . ? N5 C23 N2 122.5(4) . . ? N2 C23 N3 120.0 . . ? C23 N2 C22 120.0 . . ? C31 C30 H30 119.4 . . ? C31 C30 C29 121.2(7) . . ? C29 C30 H30 119.4 . . ? O9 C25 O10 122.3(6) . . ? O9 C25 C26 117.2(7) . . ? O10 C25 C26 120.2(7) . . ? C28 C29 C29 119.8(4) . 72_666 ? C30 C29 C28 116.7(6) . . ? C30 C29 C29 123.0(5) . 72_666 ? C39 C38 C37 119.9(5) 22_565 . ? C39 C38 C37 119.9(5) . . ? C39 C38 C39 120.2(10) . 22_565 ? O12 C37 O12 138.3(14) 22_565 . ? O12 C37 C38 110.9(7) . . ? O12 C37 C38 110.9(7) 22_565 . ? C40 C41 C40 120.8(12) 22_565 . ? C40 C41 C42 119.6(6) 22_565 . ? C40 C41 C42 119.6(6) . . ? C41 C40 H40 120.1 . . ? C41 C40 C39 119.7(8) . . ? C39 C40 H40 120.1 . . ? C38 C39 C40 119.6(7) . . ? C38 C39 H39 120.2 . . ? C40 C39 H39 120.2 . . ? C44 C45 C44 121.3(12) 22_565 . ? C44 C45 C46 119.4(6) 22_565 . ? C44 C45 C46 119.4(6) . . ? C43 C42 C41 119.3(6) 22_565 . ? C43 C42 C41 119.3(6) . . ? C43 C42 C43 121.3(12) . 22_565 ? C45 C44 H44 120.3 . . ? C45 C44 C43 119.5(8) . . ? C43 C44 H44 120.3 . . ? C42 C43 C44 119.2(8) . . ? C42 C43 H43 120.4 . . ? C44 C43 H43 120.4 . . ? O13 C46 C45 111.2(13) . . ? O13 C46 C45 111.2(13) 22_565 . ? O13 C46 O13 138(3) . 22_565 ? _smtbx_masks_special_details ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.989 -0.909 -0.244 398145.2 16377.8 ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma _refln_scale_group_code 3 3 1 39843 79 1 4 4 4 303641 1624 1 5 3 3 114634 1567 1 5 5 1 157646 840 1 5 5 3 67652 79 1 6 0 2 58897 68 1 6 2 0 63378 57 1 6 6 2 19299 295 1 6 6 4 10351 409 1 7 1 3 71215 999 1 7 3 1 74933 806 1 7 3 3 105386 1976 1 7 3 5 271860 8903 1 7 5 3 246057 5474 1 7 5 5 290360 3816 1 7 7 1 65913 261 1 7 7 3 216061 1488 1 7 7 5 57217 341 1 8 0 2 89558 1136 1 8 2 0 88424 1226 1 8 2 4 93345 3327 1 8 2 6 143560 2828 1 8 4 2 71966 2771 1 8 4 6 135378 1147 1 8 6 2 150478 2680 1 8 6 4 137492 1045 1 8 6 6 2416 79 1 8 8 0 22677 295 1 8 8 4 2927 159 1 8 8 6 129601 2862 1 9 1 5 59821 1817 1 9 1 7 281153 2862 1 9 3 5 503790 9108 1 9 3 7 114520 988 1 9 5 1 50744 1737 1 9 5 3 496321 5837 1 9 5 7 229562 1749 1 9 7 1 290467 2544 1 9 7 3 133900 840 1 9 7 5 207272 1692 1 9 7 7 85356 284 1 9 9 1 238313 4406 1 9 9 5 5039 102 1 9 9 7 6966 295 1 9 9 9 628967 20021 1 10 0 2 37782 647 1 10 0 6 488257 8687 1 10 0 8 417085 4985 1 10 2 0 33159 874 1 10 2 2 444712 8585 1 10 2 4 25596 397 1 10 2 6 21350 318 1 10 2 8 49535 852 1 10 4 2 18558 273 1 10 4 4 57830 1261 1 10 4 6 67204 522 1 10 4 8 34343 659 1 10 6 2 15812 318 1 10 6 4 63580 477 1 10 6 6 440961 3271 1 10 6 8 80331 1840 1 10 8 0 398444 4622 1 10 8 2 69403 806 1 10 8 4 33650 715 1 10 8 6 77113 1942 1 10 8 8 63113 863 1 10 10 2 177201 920 1 10 10 4 162012 1567 1 10 10 6 5045 136 1 10 10 8 144817 2669 1 10 10 10 173803 3452 1 11 1 1 81553 795 1 11 1 3 26981 375 1 11 1 5 115414 3055 1 11 1 7 134725 965 1 11 1 9 303934 4168 1 11 3 1 21426 375 1 11 3 3 33207 307 1 11 3 5 273952 2862 1 11 3 7 27220 159 1 11 3 9 482029 6007 1 11 5 1 112937 2601 1 11 5 3 252874 2612 1 11 5 5 229276 1726 1 11 5 7 61687 613 1 11 5 9 6226 454 1 11 7 1 137902 727 1 11 7 3 26391 125 1 11 7 5 52489 568 1 11 7 7 6098 114 1 11 7 9 151679 2646 1 11 9 1 341791 3577 1 11 9 3 475709 5894 1 11 9 5 11785 534 1 11 9 7 151093 2805 1 11 9 9 59100 965 1 11 11 1 150225 2975 1 11 11 3 182549 1908 1 11 11 5 948811 28572 1 11 11 7 145365 1772 1 11 11 9 9241 227 1 11 11 11 111969 3305 1 12 0 2 140258 2146 1 12 0 4 340547 5826 1 12 0 8 15003 284 1 12 0 10 26366 170 1 12 2 0 146108 3123 1 12 2 2 10371 114 1 12 2 4 62564 488 1 12 2 6 165925 1840 1 12 2 8 614380 11799 1 12 2 10 119027 4554 1 12 4 0 344901 7188 1 12 4 2 48167 466 1 12 4 4 3538 125 1 12 4 6 16141 284 1 12 4 8 43890 545 1 12 4 10 239858 4531 1 12 6 0 602739 18965 1 12 6 2 138418 1624 1 12 6 4 16923 284 1 12 6 6 656282 24018 1 12 6 8 153205 2771 1 12 6 10 95488 2260 1 12 8 0 23439 216 1 12 8 2 436272 12424 1 12 8 4 50586 443 1 12 8 6 171086 2771 1 12 8 8 200529 1783 1 12 8 10 88873 1908 1 12 10 0 36274 182 1 12 10 2 123421 3157 1 12 10 4 259268 4452 1 12 10 6 95497 2373 1 12 10 8 104349 1896 1 12 10 10 490773 8029 1 12 12 0 58217 2941 1 12 12 2 698188 13741 1 12 12 4 25750 386 1 12 12 6 309612 5474 1 12 12 8 242980 5076 1 12 12 10 145041 1465 1 12 12 12 107315 2680 1 13 1 3 374165 4440 1 13 1 5 141842 2101 1 13 1 7 70383 840 1 13 1 9 423939 10754 1 13 1 11 12570 568 1 13 3 1 406113 5303 1 13 3 3 33115 182 1 13 3 5 19872 227 1 13 3 7 6794 102 1 13 3 9 73702 1613 1 13 3 11 110103 1749 1 13 5 1 140507 1942 1 13 5 3 20049 159 1 13 5 5 387337 4293 1 13 5 7 199346 3168 1 13 5 9 64569 1056 1 13 5 11 8178 125 1 13 7 1 70871 659 1 13 7 3 3593 91 1 13 7 5 198151 3691 1 13 7 7 49363 886 1 13 7 9 130513 2805 1 13 7 11 79571 1124 1 13 9 1 399711 9925 1 13 9 3 73272 1567 1 13 9 5 68519 1147 1 13 9 7 112753 2566 1 13 9 9 7303 318 1 13 9 11 39374 1454 1 13 11 1 22019 545 1 13 11 3 95018 1544 1 13 11 5 8644 125 1 13 11 7 77035 1238 1 13 11 9 35195 1431 1 13 11 11 117559 3361 1 13 13 1 404109 13775 1 13 13 3 184157 3850 1 13 13 5 208690 2884 1 13 13 7 103612 2169 1 13 13 9 280687 4542 1 13 13 11 97465 1783 1 13 13 13 15774 749 1 14 0 2 181184 6314 1 14 0 6 145864 3747 1 14 0 12 165924 3906 1 14 2 0 214259 7302 1 14 2 2 12273 1226 1 14 2 4 159157 3327 1 14 2 6 20413 670 1 14 2 8 11754 386 1 14 2 10 47232 988 1 14 2 12 134983 2044 1 14 4 2 166484 3759 1 14 4 4 63895 1567 1 14 4 6 126560 2862 1 14 4 8 138 148 1 14 4 10 398685 7790 1 14 4 12 17742 397 1 14 6 0 142338 3475 1 14 6 2 24649 488 1 14 6 4 127895 2328 1 14 6 6 13532 284 1 14 6 8 59553 1976 1 14 6 10 14196 216 1 14 6 12 122545 2362 1 14 8 2 14384 341 1 14 8 4 664 91 1 14 8 6 69620 1828 1 14 8 8 277610 3713 1 14 8 10 60072 1090 1 14 8 12 59098 1261 1 14 10 2 44286 954 1 14 10 4 433497 8585 1 14 10 6 11411 250 1 14 10 8 66974 965 1 14 10 10 102 159 1 14 10 12 55801 1613 1 14 12 0 191100 3952 1 14 12 2 139731 1953 1 14 12 4 14659 397 1 14 12 6 125806 2737 1 14 12 8 60302 1238 1 14 12 10 56662 1499 1 14 12 12 5817 159 1 14 14 2 143987 2317 1 14 14 4 8412 148 1 14 14 6 3292 79 1 14 14 8 4889 182 1 14 14 10 173094 3202 1 14 14 12 106754 2033 1 14 14 14 219339 7211 1 15 1 1 323350 11947 1 15 1 3 150663 1999 1 15 1 5 144647 3134 1 15 1 7 76211 1999 1 15 1 9 159758 2669 1 15 1 11 1474 125 1 15 1 13 64158 1226 1 15 3 1 137008 2703 1 15 3 3 505732 15705 1 15 3 5 62722 1192 1 15 3 7 22028 670 1 15 3 9 47480 1124 1 15 3 11 264816 5156 1 15 3 13 279790 5303 1 15 5 1 146248 2737 1 15 5 3 69832 1079 1 15 5 5 132100 2464 1 15 5 7 30867 1204 1 15 5 9 43246 1919 1 15 5 11 73581 1385 1 15 5 13 150476 2317 1 15 7 1 76411 1908 1 15 7 3 23117 466 1 15 7 5 39050 1317 1 15 7 9 45852 681 1 15 7 11 210600 3816 1 15 7 13 44856 727 1 15 9 1 143886 2305 1 15 9 3 41203 1090 1 15 9 5 44403 1544 1 15 9 7 47147 556 1 15 9 9 420987 7393 1 15 9 11 94558 1794 1 15 9 13 70980 1102 1 15 11 1 251 125 1 15 11 3 261871 4224 1 15 11 5 73930 1204 1 15 11 7 207257 3747 1 15 11 9 92941 1635 1 15 11 11 1058355 19249 1 15 11 13 45532 1215 1 15 13 1 76597 1226 1 15 13 3 279455 4236 1 15 13 5 139425 2226 1 15 13 7 40868 761 1 15 13 9 78988 1022 1 15 13 11 51615 1147 1 15 13 13 65377 840 1 15 15 1 57 79 1 15 15 3 515138 7597 1 15 15 5 1542 125 1 15 15 7 391434 6053 1 15 15 9 72160 1976 1 15 15 11 423799 5905 1 15 15 13 30822 818 1 15 15 15 36867 1669 1 16 0 0 192353 6916 1 16 0 2 36968 1578 1 16 0 4 5088 931 1 16 0 6 545259 20963 1 16 0 8 87979 2930 1 16 0 10 16985 727 1 16 0 12 11528 545 1 16 0 14 151329 3509 1 16 2 0 33460 1953 1 16 2 2 290551 6359 1 16 2 4 144783 3895 1 16 2 6 146173 3918 1 16 2 8 659007 17250 1 16 2 10 112029 2237 1 16 2 12 315340 4224 1 16 2 14 164750 1760 1 16 4 0 2728 1295 1 16 4 2 144536 4781 1 16 4 4 31161 704 1 16 4 6 23421 852 1 16 4 8 73713 1601 1 16 4 10 315928 8642 1 16 4 12 44131 420 1 16 4 14 26211 647 1 16 6 2 163100 3645 1 16 6 4 21415 829 1 16 6 6 468927 7211 1 16 6 8 52256 1442 1 16 6 10 328810 5576 1 16 6 12 186472 2555 1 16 6 14 39771 715 1 16 8 0 99446 2078 1 16 8 2 621623 22496 1 16 8 4 75546 1431 1 16 8 6 53608 1329 1 16 8 8 16194 943 1 16 8 10 22045 545 1 16 8 12 189174 2896 1 16 8 14 25276 500 1 16 10 0 20159 522 1 16 10 2 120471 2101 1 16 10 4 294682 7268 1 16 10 6 345550 5190 1 16 10 8 26352 522 1 16 10 10 20028 341 1 16 10 12 96974 1919 1 16 10 14 64925 1124 1 16 12 0 11283 534 1 16 12 2 351621 4202 1 16 12 4 42789 352 1 16 12 6 187693 2521 1 16 12 8 204976 3089 1 16 12 10 92981 1794 1 16 12 12 382593 5076 1 16 12 14 34980 602 1 16 14 0 147529 3271 1 16 14 2 177670 1806 1 16 14 4 23928 488 1 16 14 6 43126 704 1 16 14 8 25483 534 1 16 14 10 73161 1170 1 16 14 12 40276 647 1 16 14 14 46361 1238 1 16 16 0 198022 3441 1 16 16 2 48471 784 1 16 16 4 51359 1862 1 16 16 6 45274 579 1 16 16 8 552211 8301 1 16 16 10 330689 5031 1 16 16 12 941256 11560 1 16 16 14 215213 3259 1 16 16 16 1001282 39530 1 17 1 1 315590 9653 1 17 1 3 46849 1363 1 17 1 5 21007 772 1 17 1 7 250264 5803 1 17 1 9 46632 1181 1 17 1 11 13087 522 1 17 1 13 15876 307 1 17 1 15 46607 761 1 17 3 1 49521 1295 1 17 3 5 49777 931 1 17 3 7 14220 432 1 17 3 9 68985 1908 1 17 3 11 86875 1578 1 17 3 13 77453 1420 1 17 3 15 297353 4747 1 17 5 1 26813 1158 1 17 5 3 46745 818 1 17 5 5 171821 5769 1 17 5 7 35340 1102 1 17 5 9 75015 1726 1 17 5 11 28447 704 1 17 5 13 21383 341 1 17 5 15 227409 4134 1 17 7 1 261771 6007 1 17 7 3 15456 397 1 17 7 5 36147 1113 1 17 7 7 40125 1067 1 17 7 9 35235 602 1 17 7 11 497268 9482 1 17 7 13 342469 6802 1 17 7 15 211968 3645 1 17 9 1 45542 999 1 17 9 3 62083 1510 1 17 9 5 72426 1601 1 17 9 7 32651 659 1 17 9 9 196033 3475 1 17 9 11 33022 1079 1 17 9 13 5510 204 1 17 9 15 79791 2124 1 17 11 1 16782 454 1 17 11 3 91832 1522 1 17 11 5 22605 500 1 17 11 7 473565 8392 1 17 11 9 30476 1045 1 17 11 11 674285 7983 1 17 11 13 53654 1510 1 17 11 15 166258 2362 1 17 13 1 20070 295 1 17 13 3 73349 1192 1 17 13 5 24415 273 1 17 13 7 348331 6416 1 17 13 9 6734 273 1 17 13 11 57993 1317 1 17 13 13 52139 1033 1 17 13 15 40444 988 1 17 15 1 51470 818 1 17 15 3 279540 4224 1 17 15 5 232731 3679 1 17 15 7 192400 3498 1 17 15 9 76867 2112 1 17 15 11 167999 2373 1 17 15 13 35917 977 1 17 15 15 159705 2487 1 17 17 1 19614 273 1 17 17 3 79186 670 1 17 17 5 70818 1272 1 17 17 7 14360 284 1 17 17 9 2290 114 1 17 17 11 99318 1828 1 17 17 13 126919 1726 1 17 17 15 176624 2601 1 17 17 17 158176 5485 1 18 0 2 872 375 1 18 0 4 4280 238 1 18 0 6 3298 647 1 18 0 8 55061 3180 1 18 0 10 465316 14240 1 18 0 12 4894 636 1 18 0 14 77001 2214 1 18 0 16 18617 1033 1 18 2 0 362 227 1 18 2 2 17578 1965 1 18 2 4 128861 2919 1 18 2 6 92902 3305 1 18 2 8 29111 1442 1 18 2 10 124644 3214 1 18 2 12 40410 897 1 18 2 14 12279 250 1 18 2 16 32128 806 1 18 4 0 3503 397 1 18 4 2 109688 2510 1 18 4 4 65899 3305 1 18 4 6 51561 1692 1 18 4 8 31899 1056 1 18 4 10 201276 5417 1 18 4 12 47799 1204 1 18 4 14 8850 307 1 18 4 16 80973 1340 1 18 6 0 19549 636 1 18 6 2 88981 2487 1 18 6 4 51773 1374 1 18 6 6 4696 852 1 18 6 8 22402 704 1 18 6 10 371011 6371 1 18 6 12 217872 3963 1 18 6 14 70625 1226 1 18 6 16 43174 908 1 18 8 0 54281 3248 1 18 8 2 27677 1102 1 18 8 4 33987 1136 1 18 8 6 14622 795 1 18 8 8 34818 1102 1 18 8 10 62412 1476 1 18 8 12 1151 148 1 18 8 14 81855 1590 1 18 8 16 76116 1056 1 18 10 0 442936 12140 1 18 10 2 131454 2748 1 18 10 4 191451 4202 1 18 10 6 366861 6893 1 18 10 8 69651 1465 1 18 10 10 16069 352 1 18 10 12 24196 466 1 18 10 14 27759 625 1 18 10 16 99171 1726 1 18 12 0 2961 318 1 18 12 2 41314 738 1 18 12 4 49645 943 1 18 12 6 199072 3486 1 18 12 8 682 102 1 18 12 10 25218 420 1 18 12 12 186412 2953 1 18 12 14 42204 1090 1 18 12 16 45170 772 1 18 14 0 82115 1885 1 18 14 2 12326 204 1 18 14 4 6062 238 1 18 14 6 70635 1090 1 18 14 8 85752 1658 1 18 14 10 26397 591 1 18 14 12 41380 1102 1 18 14 14 2470 148 1 18 14 16 10410 386 1 18 16 0 16478 1090 1 18 16 2 26947 943 1 18 16 4 75114 1136 1 18 16 6 39198 863 1 18 16 8 81914 1079 1 18 16 10 101270 1817 1 18 16 12 46387 863 1 18 16 14 12577 420 1 18 16 16 17585 386 1 18 18 0 14465 193 1 18 18 2 7329 466 1 18 18 4 4180 261 1 18 18 6 89835 1136 1 18 18 8 10443 136 1 18 18 10 51943 908 1 18 18 12 337657 5303 1 18 18 14 84964 1420 1 18 18 16 27980 568 1 18 18 18 193981 5326 1 19 1 1 657 284 1 19 1 3 126132 4065 1 19 1 5 257812 6780 1 19 1 7 22611 715 1 19 1 9 117865 2975 1 19 1 11 105906 1578 1 19 1 13 4237 159 1 19 1 15 49491 1090 1 19 1 17 198332 3236 1 19 3 1 126963 3418 1 19 3 5 34453 931 1 19 3 7 42420 1249 1 19 3 9 495056 9585 1 19 3 11 50254 931 1 19 3 13 81768 1170 1 19 3 15 14354 454 1 19 3 17 167101 3202 1 19 5 1 282979 9971 1 19 5 3 27536 784 1 19 5 7 39166 1113 1 19 5 9 63942 1306 1 19 5 11 77488 1681 1 19 5 13 1623 148 1 19 5 15 85240 1272 1 19 5 17 34772 749 1 19 7 1 22552 613 1 19 7 3 44690 1011 1 19 7 5 30047 1033 1 19 7 7 98406 2896 1 19 7 9 971 148 1 19 7 11 140161 2158 1 19 7 13 4876 114 1 19 7 15 165205 2612 1 19 7 17 121822 1749 1 19 9 1 121453 2589 1 19 9 3 506910 8812 1 19 9 5 70682 1340 1 19 9 7 445 159 1 19 9 9 14938 273 1 19 9 11 5783 375 1 19 9 13 24894 397 1 19 9 15 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1048 250 1 76 24 8 94 284 1 76 24 10 1 238 1 76 24 12 301 295 1 76 24 14 13 216 1 76 24 16 4 238 1 76 24 18 260 273 1 76 24 20 6 227 1 76 26 0 650 409 1 76 26 2 468 261 1 76 26 4 813 261 1 76 26 6 321 238 1 76 26 8 7 250 1 76 26 10 0 261 1 76 26 12 22 227 1 76 26 14 160 273 1 76 26 16 32 261 1 76 26 18 12 204 1 76 28 0 137 375 1 76 28 2 230 273 1 76 28 4 2 227 1 76 28 6 45 227 1 76 28 8 155 238 1 76 28 10 486 227 1 76 28 12 9 284 1 76 28 14 576 261 1 76 30 0 283 420 1 76 30 2 312 284 1 76 30 4 27 261 1 76 30 6 99 250 1 76 30 8 124 295 1 76 30 10 409 261 1 76 32 0 18 420 1 76 32 2 588 250 1 77 1 1 1748 204 1 77 1 3 573 193 1 77 1 5 1296 182 1 77 1 7 44 159 1 77 1 9 660 170 1 77 1 11 866 227 1 77 1 13 731 261 1 77 1 15 195 227 1 77 1 17 712 204 1 77 1 19 119 273 1 77 1 21 58 250 1 77 1 23 863 216 1 77 1 25 298 204 1 77 1 27 18 204 1 77 1 29 249 182 1 77 3 1 755 273 1 77 3 3 704 204 1 77 3 5 1120 193 1 77 3 7 811 204 1 77 3 9 2392 273 1 77 3 11 8 182 1 77 3 13 770 125 1 77 3 15 465 284 1 77 3 17 481 238 1 77 3 19 658 193 1 77 3 21 56 227 1 77 3 23 966 216 1 77 3 25 7 216 1 77 3 27 569 216 1 77 3 29 32 204 1 77 5 1 796 238 1 77 5 3 237 182 1 77 5 5 5871 329 1 77 5 7 154 307 1 77 5 9 206 250 1 77 5 11 907 216 1 77 5 13 1368 204 1 77 5 15 745 159 1 77 5 17 19 250 1 77 5 19 50 227 1 77 5 21 203 204 1 77 5 23 201 227 1 77 5 25 293 250 1 77 5 27 18 193 1 77 5 29 298 182 1 77 7 1 231 193 1 77 7 3 452 250 1 77 7 5 22 204 1 77 7 7 15 250 1 77 7 9 484 295 1 77 7 11 1648 318 1 77 7 13 140 216 1 77 7 15 8 193 1 77 7 17 903 227 1 77 7 19 701 193 1 77 7 21 175 250 1 77 7 23 224 227 1 77 7 25 242 193 1 77 7 27 254 204 1 77 9 1 286 159 1 77 9 3 2831 273 1 77 9 5 932 238 1 77 9 7 616 261 1 77 9 9 73 250 1 77 9 11 590 295 1 77 9 13 1270 227 1 77 9 15 781 204 1 77 9 17 165 204 1 77 9 19 310 216 1 77 9 21 52 227 1 77 9 23 0 204 1 77 9 25 528 227 1 77 9 27 128 182 1 77 11 1 15 182 1 77 11 3 34 261 1 77 11 5 459 193 1 77 11 7 713 238 1 77 11 9 729 238 1 77 11 11 566 250 1 77 11 13 696 273 1 77 11 15 33 250 1 77 11 17 25 216 1 77 11 19 1062 193 1 77 11 21 423 250 1 77 11 23 218 227 1 77 11 25 85 170 1 77 11 27 4 216 1 77 13 1 864 227 1 77 13 3 24 204 1 77 13 5 1138 273 1 77 13 7 56 273 1 77 13 9 2 250 1 77 13 11 40 227 1 77 13 13 23 238 1 77 13 15 414 216 1 77 13 17 291 250 1 77 13 19 29 216 1 77 13 21 52 227 1 77 13 23 343 227 1 77 13 25 189 273 1 77 15 1 453 295 1 77 15 3 1050 307 1 77 15 5 358 204 1 77 15 7 276 216 1 77 15 9 20 284 1 77 15 11 349 238 1 77 15 13 171 273 1 77 15 15 580 250 1 77 15 17 418 273 1 77 15 19 5 204 1 77 15 21 122 238 1 77 15 23 52 238 1 77 15 25 777 250 1 77 17 1 508 170 1 77 17 3 235 329 1 77 17 5 272 261 1 77 17 7 1224 227 1 77 17 9 250 227 1 77 17 11 141 238 1 77 17 13 93 250 1 77 17 15 383 238 1 77 17 17 353 204 1 77 17 19 110 227 1 77 17 21 100 227 1 77 17 23 158 227 1 77 19 1 26 250 1 77 19 3 225 250 1 77 19 5 465 284 1 77 19 7 402 284 1 77 19 9 146 216 1 77 19 11 512 216 1 77 19 13 4 227 1 77 19 15 7 216 1 77 19 17 3 227 1 77 19 19 6 227 1 77 19 21 411 227 1 77 21 1 406 318 1 77 21 3 59 216 1 77 21 5 25 216 1 77 21 7 458 307 1 77 21 9 31 318 1 77 21 11 369 227 1 77 21 13 24 216 1 77 21 15 51 227 1 77 21 17 426 273 1 77 21 19 183 216 1 77 23 1 426 238 1 77 23 3 36 295 1 77 23 5 6 273 1 77 23 7 76 261 1 77 23 9 1056 250 1 77 23 11 464 227 1 77 23 13 78 261 1 77 23 15 4 227 1 77 23 17 130 204 1 77 25 1 518 227 1 77 25 3 540 273 1 77 25 5 66 261 1 77 25 7 206 238 1 77 25 9 4 216 1 77 25 11 8 204 1 77 25 13 1 238 1 77 25 15 822 273 1 77 27 1 265 238 1 77 27 3 49 238 1 77 27 5 37 238 1 77 27 7 21 227 1 77 27 9 212 284 1 77 27 11 411 261 1 77 29 1 46 250 1 77 29 3 32 284 1 77 29 5 169 261 1 78 0 0 1662 363 1 78 0 2 47 250 1 78 0 4 2143 341 1 78 0 6 292 250 1 78 0 8 169 170 1 78 0 10 9 318 1 78 0 12 812 329 1 78 0 14 213 250 1 78 0 16 5 307 1 78 0 18 3 284 1 78 0 20 3 284 1 78 0 22 113 341 1 78 0 24 2 261 1 78 0 26 567 307 1 78 2 0 169 273 1 78 2 2 129 170 1 78 2 4 30 182 1 78 2 6 40 170 1 78 2 8 560 204 1 78 2 10 527 148 1 78 2 12 21 250 1 78 2 14 12 227 1 78 2 16 103 204 1 78 2 18 478 216 1 78 2 20 236 238 1 78 2 22 10 193 1 78 2 24 227 250 1 78 2 26 174 216 1 78 4 0 1283 341 1 78 4 2 314 227 1 78 4 4 117 182 1 78 4 6 8 250 1 78 4 8 769 193 1 78 4 10 4 182 1 78 4 12 254 170 1 78 4 14 783 114 1 78 4 16 19 238 1 78 4 18 41 261 1 78 4 20 314 227 1 78 4 22 6 204 1 78 4 24 16 227 1 78 4 26 43 204 1 78 6 0 237 318 1 78 6 2 15 193 1 78 6 4 429 204 1 78 6 6 169 238 1 78 6 8 127 284 1 78 6 10 93 295 1 78 6 12 83 216 1 78 6 14 22 216 1 78 6 16 41 148 1 78 6 18 14 227 1 78 6 20 667 307 1 78 6 22 28 261 1 78 6 24 4 204 1 78 6 26 16 216 1 78 8 0 594 273 1 78 8 2 142 261 1 78 8 4 1610 250 1 78 8 6 1 193 1 78 8 8 265 284 1 78 8 10 384 261 1 78 8 12 275 273 1 78 8 14 60 216 1 78 8 16 1077 216 1 78 8 18 1 227 1 78 8 20 121 295 1 78 8 22 12 227 1 78 8 24 391 193 1 78 10 0 45 363 1 78 10 2 450 250 1 78 10 4 1076 238 1 78 10 6 74 227 1 78 10 8 1101 273 1 78 10 10 21 273 1 78 10 12 287 261 1 78 10 14 780 250 1 78 10 16 116 204 1 78 10 18 322 227 1 78 10 20 452 227 1 78 10 22 25 227 1 78 10 24 98 193 1 78 12 0 249 420 1 78 12 2 8 182 1 78 12 4 455 238 1 78 12 6 32 238 1 78 12 8 311 238 1 78 12 10 174 216 1 78 12 12 476 227 1 78 12 14 108 204 1 78 12 16 310 204 1 78 12 18 112 193 1 78 12 20 712 227 1 78 12 22 30 193 1 78 12 24 27 193 1 78 14 0 43 454 1 78 14 2 3 216 1 78 14 4 858 216 1 78 14 6 35 216 1 78 14 8 49 227 1 78 14 10 789 261 1 78 14 12 239 250 1 78 14 14 31 250 1 78 14 16 509 227 1 78 14 18 272 204 1 78 14 20 23 227 1 78 14 22 834 250 1 78 16 0 297 409 1 78 16 2 18 227 1 78 16 4 993 307 1 78 16 6 37 193 1 78 16 8 488 227 1 78 16 10 161 238 1 78 16 12 251 261 1 78 16 14 5 227 1 78 16 16 31 204 1 78 16 18 111 227 1 78 16 20 901 238 1 78 18 0 11 363 1 78 18 2 3 284 1 78 18 4 108 238 1 78 18 6 320 250 1 78 18 8 5 227 1 78 18 10 40 216 1 78 18 12 192 204 1 78 18 14 1 193 1 78 18 16 62 216 1 78 18 18 4 182 1 78 18 20 181 227 1 78 20 0 772 386 1 78 20 2 218 250 1 78 20 4 140 273 1 78 20 6 763 273 1 78 20 8 192 261 1 78 20 10 537 238 1 78 20 12 217 227 1 78 20 14 1 238 1 78 20 16 1089 193 1 78 20 18 34 204 1 78 22 0 320 477 1 78 22 2 2 227 1 78 22 4 7 261 1 78 22 6 38 227 1 78 22 8 268 261 1 78 22 10 268 284 1 78 22 12 560 170 1 78 22 14 6 204 1 78 24 0 451 363 1 78 24 2 75 261 1 78 24 4 19 216 1 78 24 6 511 250 1 78 24 8 176 250 1 78 24 10 7 193 1 78 24 12 228 193 1 78 26 0 549 397 1 78 26 2 21 295 1 78 26 4 56 250 1 78 26 6 296 273 1 79 1 1 773 193 1 79 1 3 307 182 1 79 1 5 822 182 1 79 1 7 60 148 1 79 1 9 112 136 1 79 1 11 17 250 1 79 1 13 337 238 1 79 1 15 8 193 1 79 1 17 12 204 1 79 1 19 586 227 1 79 1 21 443 204 1 79 1 23 93 204 1 79 3 1 262 182 1 79 3 3 279 182 1 79 3 5 279 136 1 79 3 7 55 204 1 79 3 9 36 159 1 79 3 11 31 148 1 79 3 13 493 204 1 79 3 15 48 238 1 79 3 17 211 170 1 79 3 19 458 193 1 79 3 21 368 204 1 79 3 23 374 273 1 79 5 1 446 216 1 79 5 3 78 170 1 79 5 5 56 227 1 79 5 7 235 318 1 79 5 9 186 238 1 79 5 11 279 170 1 79 5 13 25 182 1 79 5 15 34 227 1 79 5 17 65 193 1 79 5 19 7 250 1 79 5 21 242 227 1 79 5 23 123 193 1 79 7 1 115 193 1 79 7 3 102 250 1 79 7 5 529 261 1 79 7 7 169 329 1 79 7 9 454 238 1 79 7 11 449 273 1 79 7 13 142 227 1 79 7 15 144 204 1 79 7 17 401 216 1 79 7 19 161 227 1 79 7 21 16 204 1 79 9 1 129 216 1 79 9 3 49 227 1 79 9 5 90 227 1 79 9 7 332 204 1 79 9 9 1009 273 1 79 9 11 77 273 1 79 9 13 2 238 1 79 9 15 879 204 1 79 9 17 26 227 1 79 9 19 47 216 1 79 9 21 28 250 1 79 11 1 428 284 1 79 11 3 106 204 1 79 11 5 320 261 1 79 11 7 541 227 1 79 11 9 7 227 1 79 11 11 10 238 1 79 11 13 24 238 1 79 11 15 236 238 1 79 11 17 130 238 1 79 11 19 60 216 1 79 11 21 22 227 1 79 13 1 18 284 1 79 13 3 237 250 1 79 13 5 19 216 1 79 13 7 221 193 1 79 13 9 51 238 1 79 13 11 255 250 1 79 13 13 12 250 1 79 13 15 73 261 1 79 13 17 233 227 1 79 13 19 68 238 1 79 15 1 116 307 1 79 15 3 725 238 1 79 15 5 152 273 1 79 15 7 500 216 1 79 15 9 40 216 1 79 15 11 438 216 1 79 15 13 15 227 1 79 15 15 470 227 1 79 15 17 205 227 1 79 17 1 456 250 1 79 17 3 436 250 1 79 17 5 72 238 1 79 17 7 124 250 1 79 17 9 114 216 1 79 17 11 271 193 1 79 17 13 310 204 1 79 17 15 287 238 1 79 19 1 183 284 1 79 19 3 283 273 1 79 19 5 44 216 1 79 19 7 192 261 1 79 19 9 141 261 1 79 19 11 252 238 1 79 19 13 5 193 1 79 21 1 8 227 1 79 21 3 891 318 1 79 21 5 20 238 1 79 21 7 122 250 1 79 21 9 24 250 1 79 21 11 45 250 1 79 23 1 25 238 1 79 23 3 137 273 1 79 23 5 860 295 1 80 0 0 717 477 1 80 0 2 56 284 1 80 0 4 108 261 1 80 0 6 52 250 1 80 0 8 177 352 1 80 0 10 786 341 1 80 0 12 545 295 1 80 0 14 76 318 1 80 0 16 36 318 1 80 0 18 9 386 1 80 0 20 134 284 1 80 2 0 429 295 1 80 2 2 329 193 1 80 2 4 8 193 1 80 2 6 70 182 1 80 2 8 396 216 1 80 2 10 614 227 1 80 2 12 149 227 1 80 2 14 290 216 1 80 2 16 233 238 1 80 2 18 379 204 1 80 2 20 681 227 1 80 4 0 80 273 1 80 4 2 26 182 1 80 4 4 22 250 1 80 4 6 58 227 1 80 4 8 315 204 1 80 4 10 9 204 1 80 4 12 26 148 1 80 4 14 429 261 1 80 4 16 46 170 1 80 4 18 37 216 1 80 6 0 896 261 1 80 6 2 55 125 1 80 6 4 826 261 1 80 6 6 551 238 1 80 6 8 563 261 1 80 6 10 13 284 1 80 6 12 343 182 1 80 6 14 266 170 1 80 6 16 12 250 1 80 6 18 978 227 1 80 8 0 109 238 1 80 8 2 21 238 1 80 8 4 2 284 1 80 8 6 125 250 1 80 8 8 54 261 1 80 8 10 279 250 1 80 8 12 100 238 1 80 8 14 103 238 1 80 8 16 101 227 1 80 8 18 47 238 1 80 10 0 19 386 1 80 10 2 1323 227 1 80 10 4 65 227 1 80 10 6 187 238 1 80 10 8 23 204 1 80 10 10 151 227 1 80 10 12 63 261 1 80 10 14 140 238 1 80 10 16 120 238 1 80 12 0 964 397 1 80 12 2 261 227 1 80 12 4 219 216 1 80 12 6 553 227 1 80 12 8 661 182 1 80 12 10 545 261 1 80 12 12 34 261 1 80 12 14 453 318 1 80 12 16 192 238 1 80 14 0 405 397 1 80 14 2 684 295 1 80 14 4 511 250 1 80 14 6 90 250 1 80 14 8 213 193 1 80 14 10 427 227 1 80 14 12 562 250 1 80 14 14 111 238 1 80 16 0 88 352 1 80 16 2 367 261 1 80 16 4 268 261 1 80 16 6 1036 227 1 80 16 8 616 204 1 80 16 10 59 238 1 80 16 12 4 204 1 80 18 0 5 534 1 80 18 2 895 238 1 80 18 4 17 216 1 80 18 6 28 261 1 80 18 8 72 261 1 80 20 0 57 511 1 80 20 2 56 284 1 81 1 1 6672 182 1 81 1 3 765 182 1 81 1 5 3 204 1 81 1 7 63 182 1 81 1 9 141 227 1 81 1 11 69 238 1 81 1 13 1125 238 1 81 1 15 127 250 1 81 3 1 1094 204 1 81 3 3 38 170 1 81 3 5 226 193 1 81 3 7 9 204 1 81 3 9 62 170 1 81 3 11 28 250 1 81 3 13 5 204 1 81 3 15 2 216 1 81 5 1 231 193 1 81 5 3 244 261 1 81 5 5 58 182 1 81 5 7 81 250 1 81 5 9 55 238 1 81 5 11 9 170 1 81 5 13 306 227 1 81 7 1 18 216 1 81 7 3 47 216 1 81 7 5 48 261 1 81 7 7 39 250 1 81 7 9 246 250 1 81 7 11 62 216 1 81 7 13 161 261 1 81 9 1 142 170 1 81 9 3 59 238 1 81 9 5 37 261 1 81 9 7 10 227 1 81 9 9 196 261 1 81 9 11 2 250 1 81 11 1 52 295 1 81 11 3 8 193 1 81 11 5 90 204 1 81 11 7 968 261 1 81 11 9 45 238 1 81 11 11 198 261 1 81 13 1 53 273 1 81 13 3 420 261 1 81 13 5 235 318 1 81 13 7 106 227 1 81 15 1 515 273 1 81 15 3 70 273 1 82 0 0 478 409 1 82 0 2 488 273 1 82 0 4 33 397 1 82 0 6 214 273 1 82 0 8 236 341 1 82 2 0 359 261 1 82 2 2 91 204 1 82 2 4 81 238 1 82 2 6 78 273 1 82 2 8 172 250 1 82 4 0 438 363 1 82 4 2 312 204 1 82 4 4 327 216 1 82 4 6 7 182 1 82 4 8 349 193 1 82 6 0 10 556 1 82 6 2 88 318 1 82 6 4 255 227 1 82 6 6 520 216 1 82 8 0 471 363 1 82 8 2 702 295 1 82 8 4 32 295 1 _iucr_refine_instructions_details ; ST-4_sq.res created by SHELXL-2014/7 TITL ST-4_sq.res in F432 CELL 0.8265 77.569 77.569 77.569 90 90 90 ZERR 16 0.009 0.009 0.009 0 0 0 LATT -4 SYMM -X,-Y,+Z SYMM -X,+Y,-Z SYMM +X,-Y,-Z SYMM +Z,+X,+Y SYMM +Z,-X,-Y SYMM -Z,-X,+Y SYMM -Z,+X,-Y SYMM +Y,+Z,+X SYMM -Y,+Z,-X SYMM +Y,-Z,-X SYMM -Y,-Z,+X SYMM +Y,+X,-Z SYMM -Y,-X,-Z SYMM +Y,-X,+Z SYMM -Y,+X,+Z SYMM +X,+Z,-Y SYMM -X,+Z,+Y SYMM -X,-Z,-Y SYMM +X,-Z,+Y SYMM +Z,+Y,-X SYMM +Z,-Y,+X SYMM -Z,+Y,+X SYMM -Z,-Y,-X SFAC C H N O Zn DISP C 0.005 0.002 16.098 DISP H -0 0 0.63 DISP N 0.009 0.005 28.748 DISP O 0.016 0.009 48.778 DISP Zn 0.174 1.909 8814.402 UNIT 3648 2208 576 1040 320 EQIV $1 +Z,1-Y,+X SADI O12_$1 C37 O12 C37 O13 C46 O13_$1 C46 SADI O12 C38 C38 O12_$1 C45 O13 C45 O13_$1 SADI O13_$1 C45 O13 C45 C39 C39_$1 C39_$1 C41 C41 C39 C38 C40_$1 C40_$1 C40 = C40 C38 C42 C44 C42 C44_$1 C44_$1 C44 C43 C43_$1 C43_$1 C45 C45 C43 SADI C39_$1 C38 C39 C38 C39 C40 C40 C41 C40_$1 C41 C39_$1 C40_$1 C43_$1 C42 = C43 C42 C43 C44 C44 C45 C44_$1 C45 C43_$1 C44_$1 SADI C41 C42 C37 C38 C45 C46 FLAT O12_$1 C40_$1 C39_$1 C38 C37 C41 C40 C39 O12 FLAT C44_$1 C43_$1 O13_$1 C45 C42 C44 C43 C46 O13 FLAT C45 C42 C44_$1 C44 C43_$1 C43 C46 O13_$1 O13 RIGU O12 O12 C38 C37 C41 C40 C40 C39 C39 C45 C42 C44 C44 C43 C43 C46 O13 O13 ISOR O12 C38 C37 C41 C40 C40 C39 C39 C45 C42 C44 C44 C43 C43 C46 O13 O13 O12 L.S. 100 PLAN 20 SIZE 0.12 0.12 0.12 TEMP 25 BOND $H list 4 ABIN fmap 2 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 REM REM REM WGHT 0.040600 42.578800 BASF 0.49409 FVAR 0.39455 ZN1 5 0.621616 0.596359 0.872352 11.00000 0.12857 0.11814 = 0.12940 -0.01136 -0.01228 0.01496 ZN2 5 0.595760 0.595760 0.904240 10.33333 0.13839 0.13839 = 0.13839 -0.00129 -0.00129 0.00129 ZN3 5 0.668083 0.495293 0.695856 11.00000 0.13673 0.16743 = 0.11860 -0.00229 0.00065 0.00561 ZN4 5 0.665067 0.480190 0.657998 11.00000 0.13537 0.19411 = 0.12731 -0.01138 0.01583 -0.02275 O1 4 0.610513 0.610513 0.889487 10.33333 0.11025 0.11025 = 0.11025 -0.00640 -0.00640 0.00640 O2 4 0.671796 0.500000 0.671796 10.50000 0.10133 0.17912 = 0.10133 0.00764 0.00903 -0.00764 O11 4 0.689951 0.493589 0.708277 11.00000 0.15092 0.21970 = 0.15440 0.00524 -0.01924 -0.01315 O3 4 0.614230 0.602575 0.849606 11.00000 0.19215 0.18907 = 0.12303 -0.00552 -0.02443 0.05561 O5 4 0.526708 0.657176 0.699554 11.00000 0.23290 0.19419 = 0.13445 -0.01799 -0.03870 0.06951 O9 4 0.616344 0.571970 0.875628 11.00000 0.24560 0.11487 = 0.21323 -0.01725 -0.00253 -0.00792 O7 4 0.650547 0.531063 0.685844 11.00000 0.21816 0.23112 = 0.16045 0.00114 0.03546 0.07645 O4 4 0.598001 0.626104 0.853497 11.00000 0.22015 0.18762 = 0.11564 -0.03002 -0.01980 0.05447 O10 4 0.600441 0.572223 0.898968 11.00000 0.23108 0.13911 = 0.22084 -0.01188 0.02067 0.01744 O8 4 0.656696 0.514242 0.707780 11.00000 0.21953 0.24500 = 0.14855 -0.02087 0.01773 0.07128 O6 4 0.536150 0.653059 0.673062 11.00000 0.26534 0.20254 = 0.14564 -0.00790 -0.03101 0.08003 C32 1 0.703998 0.500000 0.703998 10.50000 0.13463 0.19083 = 0.13463 -0.01047 -0.01713 0.01047 C15 1 0.651341 0.528172 0.702029 11.00000 0.16864 0.25318 = 0.13416 0.02666 0.00966 0.08937 C8 1 0.537122 0.651378 0.688733 11.00000 0.25128 0.18436 = 0.11078 -0.01821 -0.04103 0.04649 C33 1 0.717732 0.500000 0.717732 10.50000 0.13733 0.28922 = 0.13733 -0.00336 -0.00897 0.00336 C1 1 0.605196 0.615268 0.844484 11.00000 0.19935 0.18878 = 0.11479 -0.01450 -0.02043 0.04631 O12 4 0.649752 0.485386 0.639488 10.50000 0.14156 0.26821 = 0.10964 0.01913 -0.02808 -0.00816 C26 1 0.609022 0.546248 0.887342 11.00000 0.22064 0.10932 = 0.23296 0.00557 0.04946 0.00931 AFIX 66 C2 1 0.601874 0.616229 0.825194 11.00000 0.21204 0.25216 = 0.11167 -0.00575 -0.02146 0.09378 C7 1 0.609675 0.604315 0.814317 11.00000 0.32026 0.26941 = 0.12557 -0.05155 -0.04256 0.16810 AFIX 43 H7 2 0.616800 0.595812 0.818865 11.00000 -1.20000 AFIX 65 C6 1 0.606826 0.605108 0.796643 11.00000 0.31979 0.34953 = 0.13127 -0.02763 -0.03528 0.20529 AFIX 43 H6 2 0.612045 0.597136 0.789366 11.00000 -1.20000 AFIX 65 C5 1 0.596176 0.617816 0.789846 11.00000 0.33929 0.32365 = 0.10469 -0.02977 -0.03289 0.20109 C4 1 0.588375 0.629730 0.800722 11.00000 0.36896 0.28950 = 0.14015 -0.03705 -0.03196 0.20697 AFIX 43 H4 2 0.581250 0.638233 0.796175 11.00000 -1.20000 AFIX 65 C3 1 0.591224 0.628937 0.818396 11.00000 0.33228 0.25888 = 0.13050 -0.02117 -0.02280 0.16920 AFIX 43 H3 2 0.586005 0.636909 0.825673 11.00000 -1.20000 AFIX 0 C34 1 0.714254 0.494815 0.733885 11.00000 0.15929 0.36097 = 0.15405 0.04218 -0.02688 -0.01768 AFIX 43 H34 2 0.703398 0.490455 0.736510 11.00000 -1.20000 AFIX 0 C36 1 0.743161 0.500000 0.743161 10.50000 0.13881 0.27080 = 0.13881 0.02092 -0.02186 -0.02092 N4 3 0.591118 0.618846 0.773486 11.00000 0.46280 0.42786 = 0.11454 -0.07867 -0.04032 0.31610 AFIX 3 H4A 2 0.582988 0.626086 0.771456 11.00000 -1.20000 AFIX 66 C12 1 0.578455 0.621559 0.708852 11.00000 0.36805 0.44617 = 0.12584 -0.02549 -0.04390 0.27942 C11 1 0.576176 0.622677 0.691113 11.00000 0.49188 0.44605 = 0.12207 -0.03306 -0.04553 0.34851 AFIX 43 H11 2 0.583749 0.617033 0.683728 11.00000 -1.20000 AFIX 65 C10 1 0.562579 0.632233 0.684411 11.00000 0.33930 0.34608 = 0.15277 -0.03620 -0.02075 0.19932 AFIX 43 H10 2 0.561055 0.632982 0.672543 11.00000 -1.20000 AFIX 65 C9 1 0.551261 0.640670 0.695448 11.00000 0.28339 0.21436 = 0.15339 -0.03111 -0.03604 0.11612 C14 1 0.553540 0.639552 0.713187 11.00000 0.28513 0.30882 = 0.11214 -0.03786 -0.03835 0.17318 AFIX 43 H14 2 0.545967 0.645197 0.720572 11.00000 -1.20000 AFIX 65 C13 1 0.567137 0.629996 0.719889 11.00000 0.52612 0.42510 = 0.11294 -0.03198 -0.01546 0.32647 AFIX 43 H13 2 0.568661 0.629248 0.731757 11.00000 -1.20000 AFIX 0 N5 3 0.590470 0.609956 0.714463 11.00000 0.46735 0.44740 = 0.10534 -0.04243 -0.07358 0.32161 AFIX 3 H5 2 0.595610 0.604496 0.706313 11.00000 -1.20000 AFIX 0 N6 3 0.624929 0.575944 0.749021 11.00000 0.57825 0.48391 = 0.15456 -0.03850 -0.03274 0.44595 AFIX 3 H6A 2 0.629479 0.575124 0.759101 11.00000 1.22116 AFIX 0 C27 1 0.617243 0.536723 0.875193 11.00000 0.33957 0.10196 = 0.28608 0.00324 0.06120 -0.00365 AFIX 43 H27 2 0.622450 0.542689 0.866190 11.00000 -1.20000 AFIX 0 C35 1 0.726955 0.495921 0.746960 11.00000 0.17052 0.41691 = 0.15444 0.00560 -0.03210 -0.01475 AFIX 43 H35 2 0.723914 0.493765 0.758355 11.00000 -1.20000 AFIX 0 C28 1 0.618607 0.518608 0.874980 11.00000 0.36360 0.12146 = 0.27304 -0.01063 0.04521 0.00079 AFIX 43 H28 2 0.624412 0.512824 0.866227 11.00000 -1.20000 AFIX 66 C19 1 0.630240 0.563732 0.736624 11.00000 0.31593 0.33970 = 0.14751 -0.02779 0.00783 0.17296 C18 1 0.638755 0.549264 0.742891 11.00000 0.44640 0.39703 = 0.17293 -0.04816 -0.05658 0.32780 AFIX 43 H18 2 0.639794 0.547573 0.754715 11.00000 -1.20000 AFIX 65 C17 1 0.645718 0.537325 0.731486 11.00000 0.34417 0.36935 = 0.16028 -0.02380 -0.02552 0.23254 AFIX 43 H17 2 0.651416 0.527645 0.735680 11.00000 -1.20000 AFIX 65 C16 1 0.644166 0.539853 0.713814 11.00000 0.24515 0.26232 = 0.13242 -0.02674 -0.00279 0.12770 C21 1 0.635651 0.554321 0.707547 11.00000 0.34159 0.33204 = 0.15177 -0.01810 -0.01799 0.19981 AFIX 43 H21 2 0.634612 0.556013 0.695723 11.00000 -1.20000 AFIX 65 C20 1 0.628687 0.566261 0.718952 11.00000 0.45601 0.38400 = 0.13120 -0.00861 0.02845 0.30030 AFIX 43 H20 2 0.622990 0.575940 0.714758 11.00000 -1.20000 AFIX 0 C31 1 0.601073 0.536710 0.899412 11.00000 0.38954 0.12793 = 0.31877 -0.01176 0.10453 0.04046 AFIX 43 H31 2 0.595041 0.542588 0.907945 11.00000 -1.20000 AFIX 66 C22 1 0.596572 0.610104 0.760059 11.00000 0.37033 0.35764 = 0.15799 0.00844 -0.04515 0.22180 N1 3 0.608489 0.596792 0.761437 11.00000 0.43973 0.34956 = 0.12901 -0.03325 -0.04680 0.26895 C24 1 0.613983 0.588128 0.746745 11.00000 0.44595 0.54361 = 0.12594 -0.04159 -0.02839 0.34168 N3 3 0.607561 0.592776 0.730675 11.00000 0.49350 0.47465 = 0.10878 -0.05469 -0.05049 0.35221 C23 1 0.595645 0.606088 0.729296 11.00000 0.39347 0.36893 = 0.15366 -0.05800 -0.02884 0.25921 N2 3 0.590150 0.614752 0.743988 11.00000 0.41957 0.37615 = 0.13428 -0.04662 -0.05645 0.28664 AFIX 0 C30 1 0.601088 0.519262 0.900226 11.00000 0.44793 0.12830 = 0.33960 -0.02413 0.19374 -0.01819 AFIX 43 H30 2 0.594521 0.513754 0.908610 11.00000 -1.20000 AFIX 0 C25 1 0.608966 0.564343 0.887716 11.00000 0.18193 0.10447 = 0.24398 -0.00434 -0.00290 0.00734 C29 1 0.610605 0.509581 0.888916 11.00000 0.24398 0.11754 = 0.25775 -0.01105 0.02892 -0.00909 C38 1 0.626101 0.500000 0.626101 10.25000 0.24997 0.29422 = 0.24997 -0.01949 -0.14320 0.01949 C37 1 0.640224 0.500000 0.640224 10.25000 0.17866 0.25368 = 0.17866 -0.00286 -0.07349 0.00286 C41 1 0.600972 0.500000 0.600972 10.25000 0.28171 0.25794 = 0.28171 0.01837 -0.11637 -0.01837 C40 1 0.613315 0.487374 0.600968 10.50000 0.40389 0.39993 = 0.32354 -0.11933 -0.23266 0.13103 AFIX 43 H40 2 0.613493 0.479134 0.592261 10.50000 -1.20000 AFIX 0 C39 1 0.625610 0.486922 0.614065 10.50000 0.32319 0.30955 = 0.25380 -0.04658 -0.15535 0.04220 AFIX 43 H39 2 0.633434 0.477859 0.614683 10.50000 -1.20000 AFIX 0 PART 2 C45 1 0.561997 0.500000 0.561997 10.25000 0.41541 0.37026 = 0.41541 -0.07302 -0.19909 0.07302 C42 1 0.586938 0.500000 0.586938 10.25000 0.34486 0.32471 = 0.34486 -0.00806 -0.17075 0.00806 C44 1 0.575351 0.488315 0.560970 10.50000 0.41689 0.40592 = 0.39507 -0.08735 -0.21297 0.08965 AFIX 43 H44 2 0.575941 0.480606 0.551806 10.50000 -1.20000 AFIX 0 C43 1 0.587861 0.488145 0.573670 10.50000 0.40070 0.37926 = 0.35896 -0.04631 -0.19164 0.06370 AFIX 43 H43 2 0.596787 0.480150 0.573287 10.50000 -1.20000 AFIX 0 C46 1 0.547925 0.500000 0.547925 10.25000 0.47951 0.45284 = 0.47951 -0.16694 -0.25229 0.16694 O13 4 0.551242 0.488138 0.535778 10.50000 0.62198 0.63546 = 0.54568 -0.30434 -0.33963 0.32961 HKLF 4 REM 1_a.res in F432 REM R1 = 0.0345 for 15653 Fo > 4sig(Fo) and 0.0572 for all 24546 data REM 524 parameters refined using 348 restraints END WGHT 0.0406 42.5694 REM Highest difference peak 0.053, deepest hole -0.063, 1-sigma level 0.008 Q1 1 0.5000 0.5000 1.0000 10.04167 0.05 0.05 Q2 1 0.6797 0.4894 0.6778 11.00000 0.05 0.05 Q3 1 0.6424 0.5103 0.6895 11.00000 0.05 0.05 Q4 1 0.5399 0.6363 0.6701 11.00000 0.05 0.05 Q5 1 0.6032 0.6395 0.8468 11.00000 0.05 0.05 Q6 1 0.6000 0.6059 0.8658 11.00000 0.05 0.04 Q7 1 0.5192 0.6608 0.6765 11.00000 0.05 0.04 Q8 1 0.6385 0.5109 0.7191 11.00000 0.05 0.04 Q9 1 0.6303 0.5807 0.8947 11.00000 0.05 0.04 Q10 1 0.6927 0.4810 0.6900 11.00000 0.05 0.04 Q11 1 0.6304 0.6160 0.8403 11.00000 0.05 0.04 Q12 1 0.5203 0.6578 0.6793 11.00000 0.05 0.04 Q13 1 0.5349 0.6392 0.6694 11.00000 0.05 0.04 Q14 1 0.5124 0.6610 0.7229 11.00000 0.05 0.04 Q15 1 0.6275 0.5765 0.8611 11.00000 0.05 0.04 Q16 1 0.6394 0.6394 0.8606 10.33333 0.05 0.04 Q17 1 0.6096 0.5822 0.8850 11.00000 0.05 0.04 Q18 1 0.6021 0.6284 0.9007 11.00000 0.05 0.04 Q19 1 0.6258 0.5973 0.8946 11.00000 0.05 0.04 Q20 1 0.6199 0.6199 0.8801 10.33333 0.05 0.04 REM The information below was added by Olex2. REM REM R1 = 0.0345 for 15653 Fo > 4sig(Fo) and 0.0572 for all 25164 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.05, deepest hole -0.06 REM Mean Shift 0, Max Shift -0.004. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0572 REM R1_gt = 0.0345 REM wR_ref = 0.0901 REM GOOF = 0.966 REM Shift_max = -0.004 REM Shift_mean = 0 REM Reflections_all = 25164 REM Reflections_gt = 15653 REM Parameters = n/a REM Hole = -0.06 REM Peak = 0.05 REM Flack = n/a ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.506(5) 2 0.494(5) _shelx_fab_file ; -45 -49 -47 -14.4132 -18.8881 -44 -52 -46 11.4147 -32.6835 -44 -50 -48 0.5582 3.1297 -44 -50 -46 -21.4107 15.6311 -44 -48 -46 32.4420 -4.6167 -43 -53 -45 24.6748 -14.2952 -43 -51 -47 -27.4296 -53.8346 -43 -51 -45 -4.6996 -8.5499 -43 -49 -47 12.4786 -58.0314 -43 -49 -45 -9.9641 -9.3097 -43 -47 -45 -56.5285 35.7413 -42 -54 -46 2.9548 -32.4708 -42 -54 -44 1.4737 17.7152 -42 -52 -48 0.9947 -34.1308 -42 -52 -46 -10.3470 -8.0405 -42 -52 -44 34.2251 4.0338 -42 -50 -48 -15.6587 14.2200 -42 -50 -46 -3.6579 -8.0049 -42 -50 -44 -4.2649 3.1145 -42 -48 -46 -16.9750 -2.6217 -42 -48 -44 -11.5094 8.6904 -42 -46 -44 36.5337 7.9009 -41 -57 -43 47.7032 -16.3172 -41 -55 -45 -29.1889 -27.0058 -41 -55 -43 -25.6326 -43.1771 -41 -53 -47 -14.1302 -4.2518 -41 -53 -45 26.3339 -23.9918 -41 -53 -43 18.4742 11.9635 -41 -51 -49 16.2753 4.0361 -41 -51 -47 -17.6929 -5.3253 -41 -51 -45 1.7865 1.2540 -41 -51 -43 -47.6613 39.5263 -41 -49 -47 -5.2805 -36.1851 -41 -49 -45 -7.5296 15.9304 -41 -49 -43 -9.3043 -12.5668 -41 -47 -45 16.7458 41.5153 -41 -47 -43 13.8898 2.7687 -41 -45 -43 -47.8492 20.3211 -40 -58 -42 19.8828 -11.4452 -40 -56 -44 -18.6590 1.1564 -40 -56 -42 29.5681 3.8927 -40 -54 -46 -8.7853 -11.1045 -40 -54 -44 56.6213 -7.2167 -40 -54 -42 -2.6455 -10.3449 -40 -52 -50 -3.3637 30.8030 -40 -52 -48 25.3020 11.5800 -40 -52 -46 16.1513 -20.6525 -40 -52 -44 14.5919 -11.0967 -40 -52 -42 36.0745 1.8700 -40 -50 -48 30.5975 10.1727 -40 -50 -46 -24.4430 6.2848 -40 -50 -44 -16.5999 16.5837 -40 -50 -42 41.1535 -8.0250 -40 -48 -46 -2.8704 16.7557 -40 -48 -44 18.2605 -13.4582 -40 -48 -42 -4.6224 -18.2489 -40 -46 -44 20.9144 -16.4405 -40 -46 -42 -20.8179 -40.1882 -40 -44 -42 -32.3735 3.2591 -39 -59 -41 -0.3137 -10.4377 -39 -57 -45 16.1238 1.8650 -39 -57 -43 18.4770 -1.4881 -39 -57 -41 -14.9607 8.1720 -39 -55 -47 -35.4508 24.8712 -39 -55 -45 -10.0263 -9.3436 -39 -55 -43 -5.7939 -19.6584 -39 -55 -41 5.0133 17.4020 -39 -53 -49 39.1036 -0.7519 -39 -53 -47 -3.8877 1.7020 -39 -53 -45 -6.2820 16.9898 -39 -53 -43 -21.4114 10.2054 -39 -53 -41 16.3339 -5.2469 -39 -51 -49 1.1608 17.1898 -39 -51 -47 12.1759 -7.2285 -39 -51 -45 -57.8478 13.1413 -39 -51 -43 1.8814 -15.0368 -39 -51 -41 -10.9855 13.9248 -39 -49 -47 -18.6201 4.8102 -39 -49 -45 -9.2437 -21.5765 -39 -49 -43 6.7599 -13.0163 -39 -49 -41 28.6342 -10.1812 -39 -47 -45 -17.2985 -4.5011 -39 -47 -43 11.5331 13.0312 -39 -47 -41 8.7310 20.4187 -39 -45 -43 33.5709 6.8314 -39 -45 -41 31.9651 41.3653 -39 -43 -41 14.0327 -10.2584 -38 -60 -42 -0.8043 -2.0329 -38 -60 -40 -16.2102 -23.1236 -38 -58 -44 -10.5434 10.5555 -38 -58 -42 -13.5610 -7.1091 -38 -58 -40 -14.7690 -8.0096 -38 -56 -46 2.4042 -1.7668 -38 -56 -44 44.1532 14.7248 -38 -56 -42 -35.8526 -4.8030 -38 -56 -40 18.2556 17.9621 -38 -54 -48 10.3907 -2.9387 -38 -54 -46 -10.5594 36.8455 -38 -54 -44 1.3427 -27.9856 -38 -54 -42 18.5112 -31.9738 -38 -54 -40 32.2673 -0.6816 -38 -52 -50 23.1646 12.9554 -38 -52 -48 -13.0464 16.7162 -38 -52 -46 3.9940 -1.1192 -38 -52 -44 26.5953 2.2600 -38 -52 -42 -14.3783 -11.9015 -38 -52 -40 -10.9713 -30.9115 -38 -50 -48 27.9504 -0.0237 -38 -50 -46 -3.2183 3.1365 -38 -50 -44 33.2795 -7.4756 -38 -50 -42 14.8204 -4.7235 -38 -50 -40 31.4207 -8.5778 -38 -48 -46 4.5667 -1.1368 -38 -48 -44 9.6047 13.9489 -38 -48 -42 20.1157 19.1221 -38 -48 -40 16.1217 -1.0035 -38 -46 -44 5.6290 20.9634 -38 -46 -42 -18.1453 -11.4509 -38 -46 -40 70.1355 -27.7167 -38 -44 -42 -6.2485 -17.4598 -38 -44 -40 -16.9917 -10.6956 -38 -42 -40 -11.2005 -4.9332 -37 -61 -41 1.8158 -19.7840 -37 -61 -39 -17.0164 5.5017 -37 -59 -43 -24.6137 3.1184 -37 -59 -41 1.2207 32.5859 -37 -59 -39 -37.1132 45.1274 -37 -57 -45 -3.1187 -10.8721 -37 -57 -43 11.7946 -20.8103 -37 -57 -41 -5.7983 -21.5226 -37 -57 -39 25.8266 13.4791 -37 -55 -49 12.3062 7.5809 -37 -55 -47 -1.0708 19.1689 -37 -55 -45 14.1978 -19.4712 -37 -55 -43 -10.2441 11.7186 -37 -55 -41 5.4805 2.4389 -37 -55 -39 -14.7384 22.7426 -37 -53 -51 15.0006 7.9013 -37 -53 -49 -1.4226 -9.8626 -37 -53 -47 -23.2658 -14.5353 -37 -53 -45 -30.9412 -22.5028 -37 -53 -43 -13.1066 14.5912 -37 -53 -41 9.4782 -14.4267 -37 -53 -39 -34.2172 -4.1037 -37 -51 -49 3.8640 -14.8273 -37 -51 -47 2.2070 -13.3168 -37 -51 -45 3.7175 4.3115 -37 -51 -43 -7.3581 8.2214 -37 -51 -41 -16.0129 -24.5258 -37 -51 -39 -7.4048 45.8645 -37 -49 -47 -12.8790 41.7983 -37 -49 -45 -17.6002 9.8740 -37 -49 -43 27.5075 -18.4542 -37 -49 -41 -56.9937 6.4931 -37 -49 -39 21.6618 39.2266 -37 -47 -45 24.8171 -13.2592 -37 -47 -43 -19.4293 -6.8573 -37 -47 -41 18.6020 -18.0260 -37 -47 -39 -1.9856 -10.8889 -37 -45 -43 53.9204 66.0004 -37 -45 -41 37.5557 -54.2928 -37 -45 -39 22.3438 -17.3103 -37 -43 -41 -19.8978 -3.9151 -37 -43 -39 14.9374 -21.3170 -37 -41 -39 19.0262 -24.7845 -36 -62 -40 -5.1197 -37.0342 -36 -62 -38 7.3824 -12.5984 -36 -60 -42 3.6015 -9.8581 -36 -60 -40 19.4086 -19.1393 -36 -60 -38 -20.3026 -6.6306 -36 -58 -46 21.9688 -42.8909 -36 -58 -44 28.6668 18.0607 -36 -58 -42 -1.2757 -9.8001 -36 -58 -40 8.1762 2.9338 -36 -58 -38 -13.1033 -17.5848 -36 -56 -48 -15.6050 23.1874 -36 -56 -46 -9.3268 -8.0339 -36 -56 -44 0.4669 -3.5704 -36 -56 -42 26.8806 -29.7314 -36 -56 -40 20.4479 4.6561 -36 -56 -38 13.5305 28.3252 -36 -54 -50 17.9482 -11.0011 -36 -54 -48 38.5651 -6.1118 -36 -54 -46 7.6680 21.1227 -36 -54 -44 -11.7534 15.6118 -36 -54 -42 -7.7993 -32.3557 -36 -54 -40 -16.7377 18.4725 -36 -54 -38 15.3866 -6.9047 -36 -52 -50 3.7292 39.6058 -36 -52 -48 24.5820 -11.2133 -36 -52 -46 14.9914 -16.7355 -36 -52 -44 1.1429 -6.1403 -36 -52 -42 22.7323 7.0894 -36 -52 -40 -7.7764 3.0549 -36 -52 -38 11.2596 -7.6953 -36 -50 -48 26.9046 -14.6896 -36 -50 -46 1.2993 -20.6060 -36 -50 -44 -17.9434 -14.1253 -36 -50 -42 28.7531 -35.7637 -36 -50 -40 33.7445 6.4738 -36 -50 -38 -24.3843 0.4073 -36 -48 -46 -20.2401 11.3927 -36 -48 -44 19.5897 -6.4163 -36 -48 -42 32.2661 43.2150 -36 -48 -40 -12.8313 5.5127 -36 -48 -38 25.5187 -13.3094 -36 -46 -44 7.0047 10.6149 -36 -46 -42 -1.4051 -7.5880 -36 -46 -40 6.9222 18.3319 -36 -46 -38 -109.2852 -54.4806 -36 -44 -42 -9.9828 13.6799 -36 -44 -40 -8.8414 -13.0550 -36 -44 -38 21.4584 -28.6442 -36 -42 -40 2.9226 15.2852 -36 -42 -38 -0.1482 -4.3171 -36 -40 -38 1.8010 12.0205 -35 -63 -39 1.1791 20.2177 -35 -63 -37 13.6547 -0.9033 -35 -61 -43 -10.7738 9.9274 -35 -61 -41 -5.5917 -33.0818 -35 -61 -39 -13.8549 11.9463 -35 -61 -37 3.4783 -21.5854 -35 -59 -45 14.2527 -14.9274 -35 -59 -43 -1.3017 4.7135 -35 -59 -41 2.5791 28.3936 -35 -59 -39 -8.7216 -6.0154 -35 -59 -37 -6.6750 13.0622 -35 -57 -47 -0.3071 -39.2874 -35 -57 -45 -14.8988 -14.5405 -35 -57 -43 3.9581 15.6312 -35 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_shelx_fab_checksum 71879 # start Validation Reply Form _vrf_THETM01_ST-4_sq ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: Due to the highly porous nature of the crystal, diffractions at higher 2-Theta angles were too weak to be incorporated for structure determination. A resolution cut-off was applied at 1.19 angstrom. ; _vrf_PLAT241_ST-4_sq ; PROBLEM: High 'MainMol' Ueq as Compared to Neighbors of N4 Check RESPONSE: This is a consequence of the relatively low resolution obtained for this structure, resulting from weak diffraction. The weak diffraction is due to intrinsic disorder in the crystal. ; _vrf_PLAT242_ST-4_sq ; PROBLEM: Low 'MainMol' Ueq as Compared to Neighbors of C14 Check RESPONSE: This is a consequence of the relatively low resolution obtained for this structure, resulting from weak diffraction. The weak diffraction is due to intrinsic disorder in the crystal. ; # end Validation Reply Form