# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_asb219 _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H136 Fe2 N10 Na2 O17 S6' _chemical_formula_weight 1932.09 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.5685(19) _cell_length_b 19.6966(16) _cell_length_c 21.9611(18) _cell_angle_alpha 90.00 _cell_angle_beta 109.8619(9) _cell_angle_gamma 90.00 _cell_volume 9588.3(13) _cell_formula_units_Z 4 _cell_measurement_temperature 88(2) _cell_measurement_reflns_used 9947 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.49 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.338 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4112 _exptl_absorpt_coefficient_mu 0.510 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8481 _exptl_absorpt_correction_T_max 0.9183 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 88(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 51099 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 27.49 _reflns_number_total 10993 _reflns_number_gt 9617 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0453P)^2^+10.2754P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'difmap & geom' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10993 _refine_ls_number_parameters 583 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0886 _refine_ls_wR_factor_gt 0.0850 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _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 Fe1 Fe 0.094042(9) 0.699919(10) 0.102350(9) 0.01148(6) Uani 1 1 d . . . S1 S 0.163513(17) 0.847147(18) 0.105959(17) 0.01454(8) Uani 1 1 d . . . S2 S 0.128435(16) 0.553212(18) 0.058049(17) 0.01346(8) Uani 1 1 d . . . S3 S -0.035240(16) 0.620673(18) 0.065137(17) 0.01360(8) Uani 1 1 d . . . Na1 Na -0.01204(3) 0.55561(3) -0.06229(3) 0.01424(12) Uani 1 1 d . . . O1 O 0.13969(5) 0.83684(6) 0.03652(5) 0.0201(2) Uani 1 1 d . . . O2 O 0.22853(5) 0.84915(6) 0.13331(6) 0.0215(2) Uani 1 1 d . . . O3 O 0.08892(5) 0.58018(6) -0.00337(5) 0.0170(2) Uani 1 1 d . . . O4 O 0.10313(5) 0.49610(6) 0.08195(6) 0.0198(2) Uani 1 1 d . . . O5 O -0.04019(5) 0.64042(6) -0.00036(5) 0.0187(2) Uani 1 1 d . . . O6 O -0.02537(5) 0.54851(6) 0.07741(6) 0.0223(2) Uani 1 1 d . . . O7 O -0.04085(6) 0.61545(6) -0.15933(6) 0.0300(3) Uani 1 1 d . B . N1 N 0.12770(5) 0.67929(6) 0.20820(6) 0.0124(2) Uani 1 1 d . . . N2 N 0.13472(6) 0.79301(6) 0.13997(6) 0.0153(3) Uani 1 1 d . . . N3 N 0.14761(6) 0.61358(6) 0.10765(6) 0.0137(2) Uani 1 1 d . . . N4 N 0.01403(5) 0.66638(6) 0.11419(6) 0.0139(2) Uani 1 1 d . . . N5 N 0.06209(6) 0.72432(7) 0.00114(6) 0.0171(3) Uani 1 1 d D . . H5B H 0.0215(7) 0.7285(12) -0.0127(10) 0.037(6) Uiso 1 1 d D . . H5C H 0.0729(10) 0.6886(9) -0.0191(10) 0.032(6) Uiso 1 1 d D . . H5D H 0.0791(9) 0.7639(9) -0.0060(10) 0.028(5) Uiso 1 1 d D . . C1 C 0.13088(7) 0.74518(8) 0.24078(7) 0.0177(3) Uani 1 1 d . . . H1B H 0.1543 0.7402 0.2874 0.021 Uiso 1 1 calc R . . H1C H 0.0897 0.7602 0.2367 0.021 Uiso 1 1 calc R . . C2 C 0.16043(8) 0.79816(8) 0.21142(7) 0.0196(3) Uani 1 1 d . . . H2B H 0.1530 0.8441 0.2255 0.024 Uiso 1 1 calc R . . H2C H 0.2046 0.7905 0.2261 0.024 Uiso 1 1 calc R . . C3 C 0.13623(7) 0.92891(7) 0.11995(7) 0.0148(3) Uani 1 1 d . . . C4 C 0.07400(7) 0.94278(8) 0.08954(8) 0.0176(3) Uani 1 1 d . . . C5 C 0.05251(7) 1.00683(8) 0.09713(8) 0.0214(3) Uani 1 1 d . . . H5A H 0.0107 1.0161 0.0770 0.026 Uiso 1 1 calc R . . C6 C 0.08991(8) 1.05775(8) 0.13305(8) 0.0228(3) Uani 1 1 d . . . C7 C 0.15020(8) 1.04221(8) 0.16412(8) 0.0216(3) Uani 1 1 d . . . H7A H 0.1759 1.0760 0.1902 0.026 Uiso 1 1 calc R . . C8 C 0.17471(7) 0.97871(8) 0.15870(7) 0.0179(3) Uani 1 1 d . . . C9 C 0.02922(7) 0.89175(9) 0.04850(9) 0.0245(4) Uani 1 1 d . . . H9A H -0.0118 0.9091 0.0390 0.037 Uiso 1 1 calc R . . H9B H 0.0336 0.8487 0.0720 0.037 Uiso 1 1 calc R . . H9C H 0.0369 0.8844 0.0079 0.037 Uiso 1 1 calc R . . C10 C 0.06621(9) 1.12818(10) 0.13771(10) 0.0340(4) Uani 1 1 d . . . H10A H 0.0916 1.1498 0.1779 0.051 Uiso 1 1 calc R . . H10B H 0.0247 1.1250 0.1376 0.051 Uiso 1 1 calc R . . H10C H 0.0670 1.1554 0.1006 0.051 Uiso 1 1 calc R . . C11 C 0.24132(8) 0.96929(9) 0.19535(9) 0.0267(4) Uani 1 1 d . . . H11A H 0.2472 0.9298 0.2240 0.040 Uiso 1 1 calc R . . H11B H 0.2573 1.0100 0.2212 0.040 Uiso 1 1 calc R . . H11C H 0.2626 0.9620 0.1646 0.040 Uiso 1 1 calc R . . C12 C 0.18733(7) 0.64788(8) 0.22111(7) 0.0163(3) Uani 1 1 d . . . H12A H 0.2020 0.6296 0.2657 0.020 Uiso 1 1 calc R . . H12B H 0.2163 0.6828 0.2178 0.020 Uiso 1 1 calc R . . C13 C 0.18448(7) 0.59096(8) 0.17351(7) 0.0173(3) Uani 1 1 d . . . H13A H 0.2257 0.5792 0.1747 0.021 Uiso 1 1 calc R . . H13B H 0.1662 0.5500 0.1855 0.021 Uiso 1 1 calc R . . C14 C 0.19562(6) 0.52295(8) 0.04636(7) 0.0137(3) Uani 1 1 d . . . C15 C 0.22286(7) 0.46101(8) 0.07294(7) 0.0159(3) Uani 1 1 d . . . C16 C 0.27733(7) 0.44358(8) 0.06454(8) 0.0179(3) Uani 1 1 d . . . H16A H 0.2964 0.4022 0.0826 0.021 Uiso 1 1 calc R . . C17 C 0.30458(7) 0.48417(8) 0.03096(7) 0.0177(3) Uani 1 1 d . . . C18 C 0.27642(7) 0.54494(8) 0.00498(7) 0.0172(3) Uani 1 1 d . . . H18A H 0.2945 0.5731 -0.0184 0.021 Uiso 1 1 calc R . . C19 C 0.22263(7) 0.56562(8) 0.01214(7) 0.0148(3) Uani 1 1 d . . . C20 C 0.19864(8) 0.41036(8) 0.11015(8) 0.0221(3) Uani 1 1 d . . . H20A H 0.1913 0.4334 0.1463 0.033 Uiso 1 1 calc R . . H20B H 0.2282 0.3740 0.1269 0.033 Uiso 1 1 calc R . . H20C H 0.1608 0.3910 0.0812 0.033 Uiso 1 1 calc R . . C21 C 0.36363(8) 0.46447(9) 0.02307(9) 0.0260(4) Uani 1 1 d . . . H21A H 0.3887 0.5050 0.0269 0.039 Uiso 1 1 calc R . . H21B H 0.3557 0.4438 -0.0196 0.039 Uiso 1 1 calc R . . H21C H 0.3848 0.4318 0.0568 0.039 Uiso 1 1 calc R . . C22 C 0.19731(7) 0.63333(8) -0.01764(8) 0.0181(3) Uani 1 1 d . . . H22A H 0.2272 0.6568 -0.0319 0.027 Uiso 1 1 calc R . . H22B H 0.1878 0.6612 0.0146 0.027 Uiso 1 1 calc R . . H22C H 0.1605 0.6258 -0.0549 0.027 Uiso 1 1 calc R . . C23 C 0.08389(7) 0.63310(8) 0.22112(7) 0.0170(3) Uani 1 1 d . . . H23A H 0.0896 0.6337 0.2679 0.020 Uiso 1 1 calc R . . H23B H 0.0908 0.5862 0.2091 0.020 Uiso 1 1 calc R . . C24 C 0.01979(7) 0.65478(9) 0.18245(7) 0.0179(3) Uani 1 1 d . . . H24A H -0.0089 0.6190 0.1849 0.021 Uiso 1 1 calc R . . H24B H 0.0098 0.6970 0.2011 0.021 Uiso 1 1 calc R . . C25 C -0.10571(6) 0.64069(8) 0.07542(7) 0.0134(3) Uani 1 1 d . . . C26 C -0.12747(7) 0.70772(8) 0.06015(7) 0.0159(3) Uani 1 1 d . . . C27 C -0.18215(7) 0.72538(8) 0.06743(7) 0.0176(3) Uani 1 1 d . . . H27A H -0.1968 0.7704 0.0575 0.021 Uiso 1 1 calc R . . C28 C -0.21584(7) 0.67912(8) 0.08884(7) 0.0175(3) Uani 1 1 d . . . C29 C -0.19357(7) 0.61377(8) 0.10346(7) 0.0167(3) Uani 1 1 d . . . H29A H -0.2167 0.5817 0.1174 0.020 Uiso 1 1 calc R . . C30 C -0.13840(7) 0.59297(8) 0.09851(7) 0.0148(3) Uani 1 1 d . . . C31 C -0.09423(7) 0.76198(8) 0.03716(9) 0.0223(3) Uani 1 1 d . . . H31A H -0.1136 0.8060 0.0371 0.033 Uiso 1 1 calc R . . H31B H -0.0953 0.7512 -0.0068 0.033 Uiso 1 1 calc R . . H31C H -0.0522 0.7639 0.0663 0.033 Uiso 1 1 calc R . . C32 C -0.27395(7) 0.70029(10) 0.09850(8) 0.0246(4) Uani 1 1 d . . . H32A H -0.3033 0.6632 0.0851 0.037 Uiso 1 1 calc R . . H32B H -0.2902 0.7407 0.0724 0.037 Uiso 1 1 calc R . . H32C H -0.2659 0.7106 0.1443 0.037 Uiso 1 1 calc R . . C33 C -0.11832(7) 0.52160(8) 0.12097(8) 0.0191(3) Uani 1 1 d . . . H33A H -0.1483 0.5001 0.1366 0.029 Uiso 1 1 calc R . . H33B H -0.0793 0.5232 0.1561 0.029 Uiso 1 1 calc R . . H33C H -0.1144 0.4952 0.0848 0.029 Uiso 1 1 calc R . . C34 C -0.07575(10) 0.58230(10) -0.21876(9) 0.0325(4) Uani 1 1 d . B . H34A H -0.1071 0.5530 -0.2118 0.039 Uiso 1 1 calc R . . H34B H -0.0494 0.5540 -0.2353 0.039 Uiso 1 1 calc R . . C35 C -0.10440(12) 0.63873(11) -0.26603(10) 0.0487(6) Uani 1 1 d . . . H35A H -0.1415 0.6231 -0.3004 0.058 Uiso 0.50 1 calc PR A 1 H35B H -0.0760 0.6574 -0.2862 0.058 Uiso 0.50 1 calc PR A 1 H35C H -0.1022 0.6287 -0.3093 0.058 Uiso 0.50 1 d PR A 2 H35D H -0.1473 0.6445 -0.2701 0.058 Uiso 0.50 1 d PR A 2 C36 C -0.11852(15) 0.69040(13) -0.22158(13) 0.0457(9) Uani 0.812(6) 1 d P B 1 H36A H -0.1550 0.6777 -0.2115 0.055 Uiso 0.812(6) 1 calc PR B 1 H36B H -0.1237 0.7366 -0.2404 0.055 Uiso 0.812(6) 1 calc PR B 1 C36B C -0.06916(13) 0.70062(10) -0.23827(10) 0.041(4) Uani 0.188(6) 1 d P B 2 H36C H -0.0922 0.7428 -0.2544 0.049 Uiso 0.188(6) 1 calc PR B 2 H36D H -0.0300 0.7022 -0.2457 0.049 Uiso 0.188(6) 1 calc PR B 2 C37 C -0.06100(13) 0.68489(10) -0.16165(10) 0.0522(7) Uani 1 1 d R . . H37A H -0.0296 0.7163 -0.1655 0.063 Uiso 0.50 1 calc PR B 1 H37B H -0.0699 0.6963 -0.1219 0.063 Uiso 0.50 1 calc PR B 1 H37C H -0.0304 0.7146 -0.1314 0.063 Uiso 0.50 1 d PR B 2 H37D H -0.0996 0.6885 -0.1533 0.063 Uiso 0.50 1 d PR B 2 O8 O 0.33005(6) 0.65380(6) 0.20211(6) 0.0254(3) Uani 1 1 d . . . C38 C 0.30216(8) 0.69585(10) 0.14667(9) 0.0280(4) Uani 1 1 d . . . H38A H 0.2925 0.7411 0.1601 0.034 Uiso 1 1 calc R . . H38B H 0.2644 0.6747 0.1179 0.034 Uiso 1 1 calc R . . C39 C 0.34832(10) 0.70198(10) 0.11199(9) 0.0326(4) Uani 1 1 d . . . H39A H 0.3707 0.7453 0.1229 0.039 Uiso 1 1 calc R . . H39B H 0.3285 0.6991 0.0644 0.039 Uiso 1 1 calc R . . C40 C 0.39039(9) 0.64117(11) 0.13772(11) 0.0384(5) Uani 1 1 d . . . H40A H 0.3929 0.6124 0.1018 0.046 Uiso 1 1 calc R . . H40B H 0.4315 0.6564 0.1639 0.046 Uiso 1 1 calc R . . C41 C 0.36073(9) 0.60283(10) 0.17948(10) 0.0324(4) Uani 1 1 d . . . H41A H 0.3320 0.5684 0.1535 0.039 Uiso 1 1 calc R . . H41B H 0.3915 0.5799 0.2161 0.039 Uiso 1 1 calc R . . O9 O 0.0000 0.82749(12) 0.2500 0.0495(6) Uani 1 2 d S . . C42 C -0.0330(2) 0.86917(16) 0.19549(14) 0.0866(12) Uani 1 1 d . . . H42A H -0.0752 0.8534 0.1762 0.104 Uiso 1 1 calc R . . H42B H -0.0138 0.8684 0.1618 0.104 Uiso 1 1 calc R . . C43 C -0.0304(2) 0.93950(19) 0.2238(2) 0.1204(18) Uani 1 1 d . . . H43A H -0.0330 0.9750 0.1910 0.145 Uiso 1 1 calc R . . H43B H -0.0632 0.9465 0.2418 0.145 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 Fe1 0.01361(11) 0.01017(11) 0.01021(10) 0.00017(7) 0.00349(8) -0.00130(7) S1 0.01719(18) 0.01137(17) 0.01624(18) -0.00113(13) 0.00719(14) -0.00252(13) S2 0.01180(17) 0.01318(17) 0.01608(17) -0.00246(13) 0.00562(13) -0.00117(13) S3 0.01223(17) 0.01393(18) 0.01481(17) -0.00318(13) 0.00482(13) -0.00047(13) Na1 0.0146(3) 0.0125(3) 0.0147(3) 0.0005(2) 0.0037(2) -0.0005(2) O1 0.0294(6) 0.0167(6) 0.0173(5) -0.0025(4) 0.0120(5) -0.0068(5) O2 0.0179(6) 0.0172(6) 0.0306(6) -0.0019(5) 0.0099(5) -0.0013(4) O3 0.0141(5) 0.0185(5) 0.0162(5) -0.0044(4) 0.0024(4) 0.0005(4) O4 0.0176(5) 0.0174(6) 0.0276(6) -0.0013(5) 0.0117(5) -0.0031(4) O5 0.0166(5) 0.0256(6) 0.0142(5) -0.0053(4) 0.0054(4) -0.0032(4) O6 0.0190(6) 0.0140(6) 0.0350(7) -0.0037(5) 0.0106(5) 0.0006(4) O7 0.0462(8) 0.0201(6) 0.0177(6) 0.0037(5) 0.0032(5) -0.0016(5) N1 0.0124(6) 0.0121(6) 0.0124(6) -0.0001(5) 0.0040(5) -0.0013(5) N2 0.0208(7) 0.0124(6) 0.0124(6) -0.0004(5) 0.0051(5) -0.0042(5) N3 0.0140(6) 0.0150(6) 0.0115(6) -0.0012(5) 0.0035(5) 0.0002(5) N4 0.0132(6) 0.0171(6) 0.0108(6) -0.0013(5) 0.0033(5) -0.0016(5) N5 0.0218(7) 0.0139(6) 0.0143(6) 0.0001(5) 0.0045(5) -0.0033(5) C1 0.0231(8) 0.0159(7) 0.0134(7) -0.0017(6) 0.0055(6) -0.0005(6) C2 0.0270(8) 0.0162(8) 0.0135(7) -0.0016(6) 0.0040(6) -0.0038(6) C3 0.0179(7) 0.0117(7) 0.0147(7) 0.0008(5) 0.0057(6) -0.0009(5) C4 0.0190(8) 0.0160(7) 0.0181(7) 0.0006(6) 0.0066(6) -0.0023(6) C5 0.0192(8) 0.0202(8) 0.0243(8) 0.0015(6) 0.0068(6) 0.0032(6) C6 0.0301(9) 0.0163(8) 0.0227(8) -0.0007(6) 0.0099(7) 0.0030(6) C7 0.0273(9) 0.0151(8) 0.0204(8) -0.0041(6) 0.0055(6) -0.0033(6) C8 0.0209(8) 0.0155(7) 0.0164(7) 0.0003(6) 0.0050(6) -0.0025(6) C9 0.0186(8) 0.0205(8) 0.0288(9) -0.0006(7) 0.0010(7) -0.0026(6) C10 0.0382(11) 0.0224(9) 0.0374(11) -0.0064(8) 0.0077(9) 0.0071(8) C11 0.0235(9) 0.0174(8) 0.0307(9) -0.0059(7) -0.0017(7) -0.0045(6) C12 0.0151(7) 0.0179(7) 0.0145(7) 0.0005(6) 0.0034(6) 0.0010(6) C13 0.0163(7) 0.0194(8) 0.0149(7) 0.0009(6) 0.0037(6) 0.0035(6) C14 0.0122(7) 0.0155(7) 0.0143(7) -0.0036(5) 0.0057(5) -0.0010(5) C15 0.0175(7) 0.0147(7) 0.0156(7) -0.0017(6) 0.0060(6) -0.0021(6) C16 0.0190(8) 0.0145(7) 0.0206(8) -0.0001(6) 0.0073(6) 0.0027(6) C17 0.0163(7) 0.0184(8) 0.0196(7) -0.0031(6) 0.0076(6) 0.0018(6) C18 0.0184(7) 0.0176(7) 0.0181(7) -0.0005(6) 0.0092(6) -0.0020(6) C19 0.0159(7) 0.0142(7) 0.0138(7) -0.0017(5) 0.0042(6) -0.0007(5) C20 0.0241(8) 0.0172(8) 0.0283(9) 0.0054(6) 0.0133(7) 0.0017(6) C21 0.0227(8) 0.0250(9) 0.0356(10) 0.0028(7) 0.0168(7) 0.0052(7) C22 0.0201(8) 0.0151(7) 0.0207(8) 0.0032(6) 0.0091(6) 0.0011(6) C23 0.0168(7) 0.0187(8) 0.0154(7) 0.0032(6) 0.0054(6) -0.0021(6) C24 0.0157(7) 0.0254(8) 0.0129(7) -0.0003(6) 0.0053(6) -0.0027(6) C25 0.0119(7) 0.0159(7) 0.0120(7) -0.0028(5) 0.0037(5) -0.0003(5) C26 0.0149(7) 0.0164(7) 0.0141(7) -0.0004(6) 0.0021(6) -0.0008(6) C27 0.0172(7) 0.0178(8) 0.0154(7) -0.0003(6) 0.0023(6) 0.0037(6) C28 0.0119(7) 0.0257(8) 0.0126(7) -0.0022(6) 0.0013(5) 0.0014(6) C29 0.0149(7) 0.0219(8) 0.0129(7) -0.0019(6) 0.0041(6) -0.0035(6) C30 0.0158(7) 0.0158(7) 0.0110(7) -0.0024(5) 0.0020(5) -0.0013(6) C31 0.0180(8) 0.0172(8) 0.0304(9) 0.0061(7) 0.0063(7) 0.0013(6) C32 0.0163(8) 0.0351(10) 0.0230(8) 0.0029(7) 0.0077(6) 0.0057(7) C33 0.0225(8) 0.0157(7) 0.0209(8) 0.0005(6) 0.0096(6) -0.0011(6) C34 0.0462(12) 0.0268(10) 0.0219(9) -0.0034(7) 0.0081(8) -0.0038(8) C35 0.0676(16) 0.0359(12) 0.0256(10) 0.0045(9) -0.0062(10) -0.0122(11) C36 0.066(2) 0.0229(13) 0.0305(14) 0.0059(10) -0.0069(13) 0.0025(12) C36B 0.066(9) 0.026(6) 0.019(5) 0.011(4) -0.001(5) 0.004(5) C37 0.0860(19) 0.0216(10) 0.0272(11) 0.0020(8) -0.0090(11) 0.0028(11) O8 0.0294(7) 0.0251(6) 0.0208(6) -0.0013(5) 0.0075(5) 0.0025(5) C38 0.0293(9) 0.0286(9) 0.0226(9) 0.0025(7) 0.0043(7) 0.0000(7) C39 0.0420(11) 0.0317(10) 0.0263(9) -0.0031(8) 0.0144(8) -0.0069(8) C40 0.0310(10) 0.0463(13) 0.0400(11) -0.0113(9) 0.0148(9) -0.0005(9) C41 0.0379(11) 0.0276(10) 0.0313(10) -0.0053(8) 0.0112(8) 0.0053(8) O9 0.0541(14) 0.0454(13) 0.0521(14) 0.000 0.0223(11) 0.000 C42 0.152(4) 0.062(2) 0.0436(16) 0.0117(14) 0.031(2) -0.011(2) C43 0.195(6) 0.069(2) 0.092(3) 0.026(2) 0.042(3) 0.066(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 Fe1 N4 2.0961(12) . ? Fe1 N3 2.0975(13) . ? Fe1 N2 2.1038(12) . ? Fe1 N5 2.1450(13) . ? Fe1 N1 2.2237(12) . ? S1 O2 1.4440(12) . ? S1 O1 1.4492(11) . ? S1 N2 1.5810(13) . ? S1 C3 1.7988(15) . ? S2 O4 1.4523(11) . ? S2 O3 1.4544(11) . ? S2 N3 1.5717(13) . ? S2 C14 1.7901(14) . ? S3 O6 1.4506(12) . ? S3 O5 1.4559(11) . ? S3 N4 1.5714(13) . ? S3 C25 1.7945(15) . ? S3 Na1 3.2881(7) . ? Na1 O4 2.2810(12) 5_565 ? Na1 O6 2.3005(12) 5_565 ? Na1 O7 2.3257(13) . ? Na1 O3 2.3406(12) . ? Na1 O5 2.3861(12) . ? Na1 Na1 3.3985(12) 5_565 ? O4 Na1 2.2810(12) 5_565 ? O6 Na1 2.3004(12) 5_565 ? O7 C34 1.441(2) . ? O7 C37 1.443(2) . ? N1 C1 1.4714(19) . ? N1 C12 1.4723(19) . ? N1 C23 1.4743(18) . ? N2 C2 1.4810(19) . ? N3 C13 1.4804(19) . ? N4 C24 1.4763(18) . ? C1 C2 1.515(2) . ? C3 C8 1.409(2) . ? C3 C4 1.416(2) . ? C4 C5 1.390(2) . ? C4 C9 1.513(2) . ? C5 C6 1.390(2) . ? C6 C7 1.386(2) . ? C6 C10 1.512(2) . ? C7 C8 1.400(2) . ? C8 C11 1.513(2) . ? C12 C13 1.519(2) . ? C14 C15 1.410(2) . ? C14 C19 1.415(2) . ? C15 C16 1.400(2) . ? C15 C20 1.518(2) . ? C16 C17 1.385(2) . ? C17 C18 1.393(2) . ? C17 C21 1.510(2) . ? C18 C19 1.390(2) . ? C19 C22 1.516(2) . ? C23 C24 1.521(2) . ? C25 C30 1.414(2) . ? C25 C26 1.415(2) . ? C26 C27 1.395(2) . ? C26 C31 1.510(2) . ? C27 C28 1.391(2) . ? C28 C29 1.386(2) . ? C28 C32 1.514(2) . ? C29 C30 1.402(2) . ? C30 C33 1.512(2) . ? C34 C35 1.514(3) . ? C35 C36B 1.484(3) . ? C35 C36 1.523(4) . ? C36 C37 1.539(3) . ? C36B C37 1.6567 . ? O8 C41 1.422(2) . ? O8 C38 1.434(2) . ? C38 C39 1.530(3) . ? C39 C40 1.535(3) . ? C40 C41 1.528(3) . ? O9 C42 1.442(3) 2 ? O9 C42 1.442(3) . ? C42 C43 1.511(5) . ? C43 C43 1.504(9) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Fe1 N3 106.71(5) . . ? N4 Fe1 N2 122.35(5) . . ? N3 Fe1 N2 119.96(5) . . ? N4 Fe1 N5 100.67(5) . . ? N3 Fe1 N5 103.41(5) . . ? N2 Fe1 N5 99.46(5) . . ? N4 Fe1 N1 80.17(5) . . ? N3 Fe1 N1 78.44(5) . . ? N2 Fe1 N1 78.20(5) . . ? N5 Fe1 N1 177.58(5) . . ? O2 S1 O1 114.74(7) . . ? O2 S1 N2 112.77(7) . . ? O1 S1 N2 109.12(7) . . ? O2 S1 C3 107.15(7) . . ? O1 S1 C3 105.78(7) . . ? N2 S1 C3 106.70(7) . . ? O4 S2 O3 113.95(7) . . ? O4 S2 N3 113.10(7) . . ? O3 S2 N3 108.01(7) . . ? O4 S2 C14 106.60(7) . . ? O3 S2 C14 107.91(7) . . ? N3 S2 C14 106.93(7) . . ? O6 S3 O5 113.53(7) . . ? O6 S3 N4 113.55(7) . . ? O5 S3 N4 108.46(7) . . ? O6 S3 C25 106.79(7) . . ? O5 S3 C25 107.38(7) . . ? N4 S3 C25 106.73(7) . . ? O6 S3 Na1 73.36(5) . . ? O5 S3 Na1 40.89(5) . . ? N4 S3 Na1 120.59(5) . . ? C25 S3 Na1 128.42(5) . . ? O4 Na1 O6 87.53(4) 5_565 5_565 ? O4 Na1 O7 95.16(5) 5_565 . ? O6 Na1 O7 109.05(5) 5_565 . ? O4 Na1 O3 155.74(5) 5_565 . ? O6 Na1 O3 84.07(4) 5_565 . ? O7 Na1 O3 109.10(5) . . ? O4 Na1 O5 89.68(4) 5_565 . ? O6 Na1 O5 154.26(5) 5_565 . ? O7 Na1 O5 96.68(5) . . ? O3 Na1 O5 88.13(4) . . ? O4 Na1 S3 85.25(3) 5_565 . ? O6 Na1 S3 130.77(4) 5_565 . ? O7 Na1 S3 120.07(4) . . ? O3 Na1 S3 83.15(3) . . ? O5 Na1 S3 23.54(3) . . ? O4 Na1 Na1 75.74(4) 5_565 5_565 ? O6 Na1 Na1 64.80(4) 5_565 5_565 ? O7 Na1 Na1 168.89(5) . 5_565 ? O3 Na1 Na1 80.09(4) . 5_565 ? O5 Na1 Na1 89.72(4) . 5_565 ? S3 Na1 Na1 66.21(2) . 5_565 ? S2 O3 Na1 130.36(7) . . ? S2 O4 Na1 138.86(7) . 5_565 ? S3 O5 Na1 115.57(7) . . ? S3 O6 Na1 153.10(8) . 5_565 ? C34 O7 C37 108.53(14) . . ? C34 O7 Na1 119.95(10) . . ? C37 O7 Na1 120.19(12) . . ? C1 N1 C12 112.92(12) . . ? C1 N1 C23 111.96(12) . . ? C12 N1 C23 112.87(12) . . ? C1 N1 Fe1 106.76(9) . . ? C12 N1 Fe1 104.85(8) . . ? C23 N1 Fe1 106.83(9) . . ? C2 N2 S1 111.57(10) . . ? C2 N2 Fe1 116.33(9) . . ? S1 N2 Fe1 127.86(7) . . ? C13 N3 S2 112.61(10) . . ? C13 N3 Fe1 116.15(9) . . ? S2 N3 Fe1 123.29(7) . . ? C24 N4 S3 113.51(10) . . ? C24 N4 Fe1 113.48(9) . . ? S3 N4 Fe1 125.59(7) . . ? N1 C1 C2 110.82(12) . . ? N2 C2 C1 108.78(12) . . ? C8 C3 C4 120.11(14) . . ? C8 C3 S1 122.17(12) . . ? C4 C3 S1 117.71(11) . . ? C5 C4 C3 118.65(14) . . ? C5 C4 C9 117.73(15) . . ? C3 C4 C9 123.62(14) . . ? C6 C5 C4 122.42(15) . . ? C7 C6 C5 117.80(15) . . ? C7 C6 C10 120.67(16) . . ? C5 C6 C10 121.52(16) . . ? C6 C7 C8 122.64(15) . . ? C7 C8 C3 118.29(14) . . ? C7 C8 C11 116.62(14) . . ? C3 C8 C11 125.09(14) . . ? N1 C12 C13 111.20(12) . . ? N3 C13 C12 108.92(12) . . ? C15 C14 C19 120.69(13) . . ? C15 C14 S2 121.97(11) . . ? C19 C14 S2 117.25(11) . . ? C16 C15 C14 117.81(14) . . ? C16 C15 C20 116.04(14) . . ? C14 C15 C20 126.15(14) . . ? C17 C16 C15 122.72(14) . . ? C16 C17 C18 118.13(14) . . ? C16 C17 C21 121.66(14) . . ? C18 C17 C21 120.20(14) . . ? C19 C18 C17 122.08(14) . . ? C18 C19 C14 118.57(14) . . ? C18 C19 C22 116.70(13) . . ? C14 C19 C22 124.73(13) . . ? N1 C23 C24 110.30(12) . . ? N4 C24 C23 109.98(12) . . ? C30 C25 C26 120.50(13) . . ? C30 C25 S3 122.64(11) . . ? C26 C25 S3 116.85(11) . . ? C27 C26 C25 118.67(14) . . ? C27 C26 C31 117.79(14) . . ? C25 C26 C31 123.53(14) . . ? C28 C27 C26 122.07(14) . . ? C29 C28 C27 118.14(14) . . ? C29 C28 C32 120.86(15) . . ? C27 C28 C32 120.96(15) . . ? C28 C29 C30 122.79(14) . . ? C29 C30 C25 117.78(14) . . ? C29 C30 C33 116.23(13) . . ? C25 C30 C33 125.95(13) . . ? O7 C34 C35 105.82(15) . . ? C36B C35 C34 105.32(17) . . ? C36B C35 C36 53.25(19) . . ? C34 C35 C36 101.22(18) . . ? C35 C36 C37 100.4(2) . . ? C35 C36B C37 96.85(13) . . ? O7 C37 C36 106.30(17) . . ? O7 C37 C36B 97.84(11) . . ? C36 C37 C36B 49.74(17) . . ? C41 O8 C38 104.59(13) . . ? O8 C38 C39 105.66(15) . . ? C38 C39 C40 103.57(15) . . ? C41 C40 C39 103.69(16) . . ? O8 C41 C40 104.55(15) . . ? C42 O9 C42 110.6(3) 2 . ? O9 C42 C43 104.2(3) . . ? C43 C43 C42 102.1(3) 2 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.598 _refine_diff_density_min -0.441 _refine_diff_density_rms 0.057 _database_code_depnum_ccdc_archive 'CCDC 971643' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_asb240 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H48 Fe N5 O6 S3' _chemical_formula_weight 762.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system hexagonal _space_group_IT_number 173 _space_group_name_H-M_alt 'P 63' _space_group_name_Hall 'P 6c' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' _cell_length_a 13.6656(9) _cell_length_b 13.6656(9) _cell_length_c 12.2841(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 1986.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 88(2) _cell_measurement_reflns_used 9990 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 28.23 _exptl_crystal_description hexagon _exptl_crystal_colour red _exptl_crystal_density_meas not_measured _exptl_crystal_density_method not_measured _exptl_crystal_density_diffrn 1.275 _exptl_crystal_F_000 806 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.294 _exptl_crystal_size_mid 0.178 _exptl_crystal_size_min 0.134 _exptl_absorpt_coefficient_mu 0.583 _shelx_estimated_absorpt_T_min 0.847 _shelx_estimated_absorpt_T_max 0.926 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8556 _exptl_absorpt_correction_T_max 0.9721 _exptl_absorpt_process_details 'Bruker SADABS 2008/1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 88(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker SMART APEX II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23645 _diffrn_reflns_av_unetI/netI 0.0195 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.721 _diffrn_reflns_theta_max 28.278 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 3279 _reflns_number_gt 3176 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.900 _reflns_Friedel_fraction_max 0.985 _reflns_Friedel_fraction_full 0.996 _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. ; _computing_data_collection 'Bruker APEX2 2011.4-1, 2011' _computing_cell_refinement 'Bruker SAINT 7.68a, 2009' _computing_data_reduction 'Bruker SAINT 7.68a, 2009' _computing_structure_solution 'Bruker SHELXTL 2008/4' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; There were several high residuals present in the final difference-Fourier map. It was not possible to determine the nature of the residuals although it was probable from the crystallization method that a benzene solvent molecule was present. The SQUEEZE routine in the PLATON program package was used to account for the electrons in the solvent accessible voids. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+0.1507P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ; Flack x determined using 1459 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.025(4) _chemical_absolute_configuration ad _refine_ls_number_reflns 3279 _refine_ls_number_parameters 149 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0233 _refine_ls_R_factor_gt 0.0221 _refine_ls_wR_factor_ref 0.0616 _refine_ls_wR_factor_gt 0.0611 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0.001 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 Fe1 Fe 0.3333 0.6667 0.97482(4) 0.01601(11) Uani 1 3 d S T P . . S1 S 0.48339(4) 0.93012(3) 0.99426(4) 0.01677(11) Uani 1 1 d . . . . . N1 N 0.3333 0.6667 0.7880(3) 0.0213(6) Uani 1 3 d S T P . . N2 N 0.47075(13) 0.81429(13) 0.94821(14) 0.0189(3) Uani 1 1 d . . . . . N3 N 0.3333 0.6667 1.1442(2) 0.0172(6) Uani 1 3 d S T P . . H3A H 0.2615 0.6225 1.1689 0.026 Uiso 0.3333 1 calc R U P . . H3B H 0.3611 0.7385 1.1689 0.026 Uiso 0.3333 1 calc R U P . . H3C H 0.3775 0.6389 1.1689 0.026 Uiso 0.3333 1 calc R U P . . O1 O 0.42291(12) 0.90284(12) 1.09691(12) 0.0201(3) Uani 1 1 d . . . . . O2 O 0.44977(12) 0.98481(12) 0.91376(12) 0.0225(3) Uani 1 1 d . . . . . C1 C 0.42614(19) 0.77962(18) 0.75324(18) 0.0243(4) Uani 1 1 d . . . . . H1A H 0.3975 0.8331 0.7466 0.029 Uiso 1 1 calc R U . . . H1B H 0.4558 0.7738 0.6815 0.029 Uiso 1 1 calc R U . . . C2 C 0.51971(18) 0.82192(17) 0.83851(19) 0.0239(4) Uani 1 1 d . . . . . H2A H 0.5568 0.7756 0.8362 0.029 Uiso 1 1 calc R U . . . H2B H 0.5774 0.9013 0.8228 0.029 Uiso 1 1 calc R U . . . C3 C 0.63011(15) 1.02108(15) 1.02331(16) 0.0169(4) Uani 1 1 d . . . . . C4 C 0.69704(16) 1.12011(16) 0.96167(16) 0.0208(4) Uani 1 1 d . . . . . C5 C 0.81034(16) 1.18862(15) 0.9915(2) 0.0246(4) Uani 1 1 d . . . . . H5A H 0.8563 1.2550 0.9504 0.030 Uiso 1 1 calc R U . . . C6 C 0.85823(19) 1.16321(18) 1.0792(2) 0.0286(5) Uani 1 1 d . . . . . C7 C 0.79075(18) 1.06579(18) 1.13741(19) 0.0264(5) Uani 1 1 d . . . . . H7A H 0.8227 1.0477 1.1974 0.032 Uiso 1 1 calc R U . . . C8 C 0.67759(17) 0.99296(16) 1.11160(17) 0.0204(4) Uani 1 1 d . . . . . C9 C 0.65702(18) 1.15963(18) 0.86514(19) 0.0246(4) Uani 1 1 d . . . . . H9A H 0.7207 1.2283 0.8348 0.037 Uiso 1 1 calc R U . . . H9B H 0.5981 1.1758 0.8887 0.037 Uiso 1 1 calc R U . . . H9C H 0.6264 1.1004 0.8094 0.037 Uiso 1 1 calc R U . . . C10 C 0.9813(2) 1.2395(2) 1.1087(3) 0.0422(7) Uani 1 1 d . . . . . H10A H 1.0113 1.3109 1.0687 0.063 Uiso 1 1 calc R U . . . H10B H 1.0244 1.2023 1.0894 0.063 Uiso 1 1 calc R U . . . H10C H 0.9879 1.2547 1.1871 0.063 Uiso 1 1 calc R U . . . C11 C 0.61310(17) 0.88900(17) 1.18167(18) 0.0215(4) Uani 1 1 d . . . . . H11A H 0.6663 0.8785 1.2268 0.032 Uiso 1 1 calc R U . . . H11B H 0.5708 0.8227 1.1350 0.032 Uiso 1 1 calc R U . . . H11C H 0.5604 0.8984 1.2287 0.032 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01376(14) 0.01376(14) 0.0205(2) 0.000 0.000 0.00688(7) S1 0.01321(19) 0.01326(19) 0.0236(2) 0.00207(17) 0.00275(17) 0.00641(15) N1 0.0203(10) 0.0203(10) 0.0234(15) 0.000 0.000 0.0102(5) N2 0.0159(7) 0.0145(7) 0.0249(9) -0.0007(6) 0.0033(6) 0.0066(6) N3 0.0159(9) 0.0159(9) 0.0200(14) 0.000 0.000 0.0079(4) O1 0.0164(7) 0.0172(7) 0.0272(7) 0.0024(5) 0.0056(5) 0.0087(6) O2 0.0187(7) 0.0199(7) 0.0298(8) 0.0053(6) 0.0013(6) 0.0103(6) C1 0.0257(10) 0.0220(10) 0.0236(10) 0.0044(8) 0.0058(8) 0.0107(8) C2 0.0203(10) 0.0219(10) 0.0278(10) 0.0001(8) 0.0064(8) 0.0093(8) C3 0.0130(8) 0.0137(8) 0.0233(9) 0.0002(7) 0.0031(7) 0.0061(7) C4 0.0203(9) 0.0170(8) 0.0272(11) 0.0021(8) 0.0056(8) 0.0110(7) C5 0.0189(8) 0.0150(8) 0.0365(12) 0.0038(8) 0.0031(10) 0.0058(7) C6 0.0190(10) 0.0170(10) 0.0468(14) -0.0018(9) -0.0040(9) 0.0066(8) C7 0.0210(10) 0.0193(9) 0.0375(12) 0.0007(8) -0.0054(8) 0.0090(8) C8 0.0188(9) 0.0163(9) 0.0274(10) 0.0017(7) 0.0021(8) 0.0096(7) C9 0.0212(10) 0.0193(9) 0.0303(11) 0.0085(8) 0.0062(8) 0.0078(8) C10 0.0224(12) 0.0229(12) 0.070(2) 0.0050(12) -0.0122(12) 0.0028(9) C11 0.0187(9) 0.0191(9) 0.0270(10) 0.0035(8) 0.0013(8) 0.0097(8) _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 Fe1 N2 1.9785(16) 2_665 ? Fe1 N2 1.9786(16) . ? Fe1 N2 1.9786(16) 3_565 ? Fe1 N3 2.080(3) . ? Fe1 N1 2.295(3) . ? S1 O2 1.4460(15) . ? S1 O1 1.4504(15) . ? S1 N2 1.6069(17) . ? S1 C3 1.7890(19) . ? N1 C1 1.488(2) 2_665 ? N1 C1 1.488(2) . ? N1 C1 1.488(2) 3_565 ? N2 C2 1.485(3) . ? C1 C2 1.526(3) . ? C3 C8 1.412(3) . ? C3 C4 1.415(3) . ? C4 C5 1.399(3) . ? C4 C9 1.514(3) . ? C5 C6 1.392(3) . ? C6 C7 1.381(3) . ? C6 C10 1.514(3) . ? C7 C8 1.394(3) . ? C8 C11 1.511(3) . ? 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 N2 Fe1 N2 117.33(3) 2_665 . ? N2 Fe1 N2 117.33(3) 2_665 3_565 ? N2 Fe1 N2 117.33(3) . 3_565 ? N2 Fe1 N3 99.51(5) 2_665 . ? N2 Fe1 N3 99.51(5) . . ? N2 Fe1 N3 99.51(5) 3_565 . ? N2 Fe1 N1 80.49(5) 2_665 . ? N2 Fe1 N1 80.49(5) . . ? N2 Fe1 N1 80.49(5) 3_565 . ? N3 Fe1 N1 180.0 . . ? O2 S1 O1 116.10(9) . . ? O2 S1 N2 111.28(9) . . ? O1 S1 N2 106.62(8) . . ? O2 S1 C3 108.22(9) . . ? O1 S1 C3 107.57(9) . . ? N2 S1 C3 106.60(8) . . ? C1 N1 C1 112.14(13) 2_665 . ? C1 N1 C1 112.14(13) 2_665 3_565 ? C1 N1 C1 112.14(13) . 3_565 ? C1 N1 Fe1 106.65(15) 2_665 . ? C1 N1 Fe1 106.65(15) . . ? C1 N1 Fe1 106.65(15) 3_565 . ? C2 N2 S1 115.31(14) . . ? C2 N2 Fe1 112.72(13) . . ? S1 N2 Fe1 121.73(9) . . ? N1 C1 C2 108.33(19) . . ? N2 C2 C1 109.49(17) . . ? C8 C3 C4 120.39(17) . . ? C8 C3 S1 118.16(14) . . ? C4 C3 S1 121.43(15) . . ? C5 C4 C3 117.99(19) . . ? C5 C4 C9 116.28(18) . . ? C3 C4 C9 125.74(18) . . ? C6 C5 C4 122.47(19) . . ? C7 C6 C5 118.1(2) . . ? C7 C6 C10 121.1(2) . . ? C5 C6 C10 120.8(2) . . ? C6 C7 C8 122.6(2) . . ? C7 C8 C3 118.49(19) . . ? C7 C8 C11 117.31(19) . . ? C3 C8 C11 124.19(17) . . ? _refine_diff_density_max 0.316 _refine_diff_density_min -0.256 _refine_diff_density_rms 0.041 _shelxl_version_number 2013-3 _shelx_res_file ; TITL asb240 in P6(3) CELL 0.71073 13.6656 13.6656 12.2841 90.000 90.000 120.000 ZERR 2.00 0.0009 0.0009 0.0008 0.000 0.000 0.000 LATT -1 SYMM -Y, X-Y, Z SYMM -X+Y, -X, Z SYMM -X, -Y, 0.5+Z SYMM Y, -X+Y, 0.5+Z SYMM X-Y, X, 0.5+Z SFAC C H N O S FE UNIT 66 96 10 12 6 2 TEMP -185.000 SIZE 0.134 0.178 0.294 rem Sonja Peterson 20s ccd1 rem APEX2 2011.4-1, SAINT 7.68a, SADABS 2008/1, SHELXTL 2013/3 rem Squeezed data L.S. 12 0 16 ACTA FMAP 2 PLAN 10 ABIN WGHT 0.039900 0.150700 FVAR 0.15906 FE1 6 0.333333 0.666667 0.974823 10.33333 0.01376 0.01376 = 0.02053 0.00000 0.00000 0.00688 S1 5 0.483387 0.930121 0.994264 11.00000 0.01321 0.01326 = 0.02357 0.00207 0.00275 0.00641 N1 3 0.333333 0.666667 0.787957 10.33333 0.02033 0.02033 = 0.02337 0.00000 0.00000 0.01017 N2 3 0.470754 0.814289 0.948213 11.00000 0.01591 0.01453 = 0.02488 -0.00073 0.00326 0.00660 N3 3 0.333333 0.666667 1.144160 10.33333 0.01587 0.01587 = 0.01996 0.00000 0.00000 0.00794 AFIX 137 H3A 2 0.261457 0.622548 1.168853 10.33333 -1.50000 H3B 2 0.361091 0.738543 1.168854 10.33333 -1.50000 H3C 2 0.377453 0.638909 1.168853 10.33333 -1.50000 AFIX 0 O1 4 0.422911 0.902838 1.096910 11.00000 0.01643 0.01718 = 0.02719 0.00244 0.00556 0.00869 O2 4 0.449769 0.984809 0.913755 11.00000 0.01870 0.01994 = 0.02982 0.00534 0.00133 0.01033 C1 1 0.426144 0.779617 0.753238 11.00000 0.02567 0.02201 = 0.02365 0.00443 0.00580 0.01066 AFIX 23 H1A 2 0.397488 0.833091 0.746627 11.00000 -1.20000 H1B 2 0.455807 0.773781 0.681476 11.00000 -1.20000 AFIX 0 C2 1 0.519715 0.821924 0.838508 11.00000 0.02033 0.02194 = 0.02782 0.00010 0.00638 0.00927 AFIX 23 H2A 2 0.556850 0.775610 0.836178 11.00000 -1.20000 H2B 2 0.577392 0.901287 0.822756 11.00000 -1.20000 AFIX 0 C3 1 0.630114 1.021080 1.023315 11.00000 0.01296 0.01368 = 0.02330 0.00016 0.00311 0.00610 C4 1 0.697043 1.120111 0.961673 11.00000 0.02032 0.01700 = 0.02721 0.00213 0.00563 0.01099 C5 1 0.810336 1.188620 0.991527 11.00000 0.01890 0.01502 = 0.03649 0.00382 0.00314 0.00583 AFIX 43 H5A 2 0.856277 1.254971 0.950382 11.00000 -1.20000 AFIX 0 C6 1 0.858227 1.163210 1.079214 11.00000 0.01895 0.01700 = 0.04682 -0.00178 -0.00400 0.00661 C7 1 0.790751 1.065791 1.137409 11.00000 0.02098 0.01930 = 0.03747 0.00069 -0.00537 0.00898 AFIX 43 H7A 2 0.822683 1.047677 1.197384 11.00000 -1.20000 AFIX 0 C8 1 0.677586 0.992962 1.111597 11.00000 0.01876 0.01631 = 0.02738 0.00172 0.00210 0.00963 C9 1 0.657017 1.159633 0.865138 11.00000 0.02115 0.01925 = 0.03031 0.00847 0.00623 0.00781 AFIX 137 H9A 2 0.720713 1.228276 0.834755 11.00000 -1.50000 H9B 2 0.598074 1.175846 0.888736 11.00000 -1.50000 H9C 2 0.626358 1.100358 0.809442 11.00000 -1.50000 AFIX 0 C10 1 0.981305 1.239516 1.108681 11.00000 0.02242 0.02291 = 0.06986 0.00505 -0.01222 0.00282 AFIX 137 H10A 2 1.011310 1.310857 1.068671 11.00000 -1.50000 H10B 2 1.024384 1.202328 1.089351 11.00000 -1.50000 H10C 2 0.987867 1.254743 1.187090 11.00000 -1.50000 AFIX 0 C11 1 0.613103 0.889000 1.181674 11.00000 0.01871 0.01912 = 0.02703 0.00351 0.00135 0.00967 AFIX 137 H11A 2 0.666288 0.878489 1.226789 11.00000 -1.50000 H11B 2 0.570770 0.822677 1.135010 11.00000 -1.50000 H11C 2 0.560439 0.898421 1.228665 11.00000 -1.50000 AFIX 0 HKLF 4 REM asb240 in P6(3) REM R1 = 0.0221 for 3176 Fo > 4sig(Fo) and 0.0233 for all 3279 data REM 149 parameters refined using 1 restraints END WGHT 0.0399 0.1507 REM Highest difference peak 0.316, deepest hole -0.256, 1-sigma level 0.041 Q1 1 0.3333 0.6667 0.8993 10.33333 0.05 0.32 Q2 1 0.7529 1.1535 0.9777 11.00000 0.05 0.29 Q3 1 0.4680 0.9264 1.0622 11.00000 0.05 0.28 Q4 1 0.3333 0.6667 1.0532 10.33333 0.05 0.26 Q5 1 0.5639 0.9793 1.0033 11.00000 0.05 0.25 Q6 1 0.6599 1.0610 0.9849 11.00000 0.05 0.23 Q7 1 0.4850 0.8683 0.9767 11.00000 0.05 0.20 Q8 1 0.8287 1.1852 1.0469 11.00000 0.05 0.19 Q9 1 1.0277 1.2703 1.0249 11.00000 0.05 0.19 Q10 1 0.4713 0.9294 0.9228 11.00000 0.05 0.19 ; _shelx_res_checksum 14954 _shelx_hkl_file ; 0 1 0 124.76 3.41 -1 0 0 135.17 3.46 1 0 0 136.68 3.51 0 -1 0 115.21 3.42 -1 -1 0 39.23 1.14 1 -2 0 40.02 1.15 2 -1 0 40.85 1.16 1 1 0 39.52 1.11 -1 -1 0 38.89 1.11 -1 2 0 38.84 1.11 1 1 0 38.75 1.13 2 -1 0 41.31 1.11 1 -2 0 38.61 1.11 -2 1 0 40.07 1.14 -1 2 0 39.70 1.13 2 -2 0 121.61 3.29 0 -2 0 122.70 3.35 0 2 0 120.82 3.31 -2 2 0 121.61 3.28 0 2 0 121.29 3.32 -2 2 0 121.81 3.35 0 -2 0 121.03 3.33 2 0 0 124.33 3.32 -2 0 0 125.16 3.34 2 -2 0 127.92 3.40 2 0 0 124.30 3.36 2 -3 0 35.06 1.08 -3 1 0 35.30 1.06 1 2 0 35.61 1.01 -2 3 0 35.92 1.03 1 2 0 34.80 1.06 -1 -2 0 34.61 1.01 3 -1 0 37.03 1.04 2 -3 0 34.17 1.01 -1 -2 0 34.48 1.07 3 -1 0 37.35 1.07 -3 1 0 35.95 1.02 3 -2 0 2.70 0.24 3 -2 0 2.85 0.19 -2 -1 0 2.56 0.23 -3 2 0 3.16 0.22 -2 -1 0 2.44 0.18 -1 3 0 2.29 0.17 2 1 0 2.57 0.17 2 1 0 2.65 0.23 -1 3 0 2.67 0.21 -3 2 0 2.80 0.15 1 -3 0 2.52 0.21 0 -3 0 40.79 1.20 3 0 0 41.64 1.22 3 -3 0 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4.98 0.49 -13 4 0 4.62 0.47 4 9 0 3.66 0.51 -9 13 0 4.16 0.45 -4 -9 0 4.77 0.56 9 -13 0 4.78 0.52 13 -4 0 4.59 0.44 -13 5 0 6.25 0.54 -8 13 0 6.67 0.52 5 8 0 6.01 0.59 8 -13 0 6.58 0.57 13 -5 0 6.16 0.54 13 -5 0 6.58 0.49 -5 -8 0 6.59 0.62 7 -13 0 1.12 0.31 13 -6 0 1.55 0.33 -13 6 0 1.05 0.29 -6 -7 0 1.45 0.37 -7 13 0 1.08 0.26 6 7 0 1.17 0.34 13 -6 0 1.27 0.25 -7 -6 0 5.29 0.54 -6 13 0 5.12 0.44 7 6 0 5.61 0.54 13 -7 0 5.00 0.51 -6 13 0 4.93 0.50 -13 7 0 5.14 0.49 6 -13 0 4.45 0.47 13 -7 0 4.61 0.41 13 -8 0 18.62 0.97 5 -13 0 17.80 0.89 8 5 0 18.24 0.96 -5 13 0 18.81 0.85 -8 -5 0 18.20 0.95 -13 8 0 17.31 0.92 -5 13 0 18.62 0.92 4 -13 0 20.77 1.00 -4 13 0 20.45 0.99 4 -13 0 21.32 0.95 -9 -4 0 20.32 1.00 -13 9 0 19.20 0.99 9 4 0 19.49 1.00 13 -9 0 18.31 1.01 -4 13 0 20.94 0.89 13 -10 0 7.11 0.62 3 -13 0 6.81 0.62 -13 10 0 7.41 0.60 -3 13 0 7.78 0.63 10 3 0 7.31 0.61 -10 -3 0 7.37 0.59 3 -13 0 6.69 0.52 -2 13 0 64.64 2.22 13 -11 0 60.44 2.27 -11 -2 0 63.25 2.16 -13 11 0 59.46 2.21 2 -13 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0.38 -3 15 0 0.19 0.32 -15 12 0 0.66 0.29 13 2 0 3.75 0.53 2 -15 0 3.29 0.55 -13 -2 0 3.43 0.50 15 -13 0 2.72 0.51 -2 15 0 2.42 0.49 -15 13 0 3.19 0.50 15 -14 0 8.48 0.77 -14 -1 0 9.45 0.72 1 -15 0 9.36 0.83 -1 15 0 10.30 0.82 -15 14 0 9.83 0.76 14 1 0 8.62 0.71 -15 15 0 11.89 0.85 15 0 0 11.91 0.83 0 15 0 11.09 0.90 0 -15 0 12.80 0.96 15 -15 0 13.94 0.96 -1 -15 0 0.57 0.43 1 15 0 0.76 0.45 16 -1 0 0.72 0.33 16 -2 0 12.75 0.84 -2 -14 0 13.90 1.02 -14 16 0 13.03 0.90 2 14 0 15.22 1.03 14 -16 0 13.86 0.97 13 -16 0 2.86 0.52 3 13 0 3.22 0.58 -3 -13 0 3.51 0.61 -13 16 0 2.85 0.48 -12 16 0 2.11 0.42 4 12 0 2.17 0.50 12 -16 0 2.42 0.50 -16 4 0 2.17 0.42 -4 -12 0 1.92 0.49 11 -16 0 5.11 0.61 -11 16 0 5.71 0.57 -5 -11 0 5.92 0.68 5 11 0 5.67 0.67 -16 5 0 6.10 0.60 10 -16 0 3.75 0.55 -16 6 0 4.05 0.52 -10 16 0 3.66 0.48 6 10 0 3.69 0.57 -6 -10 0 4.30 0.63 -9 16 0 7.76 0.63 9 -16 0 7.92 0.70 -7 -9 0 6.40 0.69 16 -7 0 8.29 0.69 -16 7 0 7.58 0.66 7 9 0 8.77 0.75 8 8 0 8.39 0.75 16 -8 0 8.73 0.72 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-7 10 13 -0.24 -0.42 -6 10 13 -0.61 -0.57 -5 10 13 -0.69 -0.72 -4 10 13 -0.53 -0.71 -3 10 13 -0.37 -0.46 -2 10 13 -0.20 -0.23 -1 10 13 -0.14 -0.09 -6 11 13 -0.51 -0.26 -5 11 13 -0.47 -0.31 0 0 14 0.99 0.49 0 1 14 1.07 0.43 -1 2 14 1.13 0.32 0 2 14 1.08 0.23 -2 3 14 0.82 -0.02 -1 3 14 0.91 -0.05 0 3 14 0.81 -0.13 -3 4 14 0.38 -0.39 -2 4 14 0.56 -0.40 -1 4 14 0.67 -0.52 0 4 14 0.44 -0.55 -4 5 14 0.16 -0.56 -3 5 14 0.18 -0.68 -2 5 14 0.40 -0.81 -1 5 14 0.44 -0.74 0 5 14 0.09 -0.66 -5 6 14 -0.11 -0.54 -4 6 14 -0.04 -0.70 -3 6 14 0.12 -0.80 -2 6 14 0.11 -0.87 -1 6 14 -0.09 -0.68 0 6 14 -0.26 -0.35 -6 7 14 -0.34 -0.23 -5 7 14 -0.21 -0.47 -4 7 14 -0.25 -0.74 -3 7 14 -0.28 -0.83 -2 7 14 -0.34 -0.62 -1 7 14 -0.50 -0.31 0 7 14 -0.47 0.01 -7 8 14 -0.35 0.15 -6 8 14 -0.37 -0.19 -5 8 14 -0.45 -0.52 -4 8 14 -0.50 -0.65 -3 8 14 -0.58 -0.65 -2 8 14 -0.57 -0.37 -1 8 14 -0.44 0.05 0 8 14 -0.36 0.21 -7 9 14 -0.35 0.05 -6 9 14 -0.36 -0.16 -5 9 14 -0.48 -0.44 -4 9 14 -0.53 -0.53 -2 9 14 -0.33 -0.13 0 1 15 0.00 0.08 -1 2 15 0.05 -0.06 0 2 15 0.12 0.22 -2 3 15 0.03 -0.39 -1 3 15 0.15 0.01 0 3 15 0.15 0.30 -3 4 15 -0.06 -0.49 -2 4 15 0.10 -0.43 -1 4 15 0.18 -0.13 0 4 15 0.08 0.28 -4 5 15 -0.10 -0.57 -3 5 15 0.00 -0.67 -2 5 15 0.04 -0.38 -1 5 15 0.06 -0.04 0 5 15 0.08 0.30 -5 6 15 -0.06 -0.58 -4 6 15 -0.14 -0.65 -3 6 15 -0.02 -0.51 -2 6 15 0.08 -0.20 -1 6 15 0.02 0.18 0 6 15 0.03 0.35 -5 7 15 -0.09 -0.47 -4 7 15 -0.05 -0.49 -3 7 15 0.00 -0.22 -2 7 15 0.10 0.01 0 1 16 -0.21 -0.33 -1 2 16 0.11 -0.45 0 2 16 0.13 -0.50 -2 3 16 0.17 -0.35 -1 3 16 0.18 -0.41 0 3 16 0.27 -0.29 0 0 16 -0.38 -0.12 0 0 0 0.00 0.00 # SQUEEZE RESULTS # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.092 301 83 ' ' 2 0.667 0.333 0.025 8 0 ' ' 3 0.333 0.667 0.525 8 0 ' ' _platon_squeeze_details (replace by semicolon in column 1 when used as .sqf) TITL asb240 in P6(3) CELL 13.6656 13.6656 12.2841 90.00 90.00 120.00 SPGR P63 # Solvent Accessible Volume = 318.2 # Electrons Found in S.A.V. = 82.8 # Note: Atoms in Void as Cxxx and Qxxx all others C101 1.000 1.000 0.969 ! 3.65 eA-3 C102 0.989 0.093 0.391 ! 3.24 eA-3 C103 0.882 0.998 0.373 ! 2.84 eA-3 C104 1.000 0.995 0.282 ! 2.66 eA-3 C105 0.920 0.938 0.293 ! 2.54 eA-3 C106 0.015 0.940 0.361 ! 2.19 eA-3 C107 0.017 0.075 0.914 ! 2.04 eA-3 C108 1.001 0.993 0.046 ! 0.54 eA-3 (replace by semicolon in column 1 when used as .sqf) ; _shelx_fab_checksum 79842 _database_code_depnum_ccdc_archive 'CCDC 971644' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_asb234 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H48 Ga N5 O6 S3' _chemical_formula_weight 776.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system hexagonal _space_group_IT_number 173 _space_group_name_H-M_alt 'P 63' _space_group_name_Hall 'P 6c' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' _cell_length_a 13.6450(9) _cell_length_b 13.6450(9) _cell_length_c 12.2882(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 1981.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 9959 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 28.26 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_density_meas none _exptl_crystal_density_method none _exptl_crystal_density_diffrn 1.302 _exptl_crystal_F_000 816 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.290 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.144 _exptl_absorpt_coefficient_mu 0.898 _shelx_estimated_absorpt_T_min 0.781 _shelx_estimated_absorpt_T_max 0.882 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7934 _exptl_absorpt_correction_T_max 0.8914 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker SMART APEX II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22408 _diffrn_reflns_av_unetI/netI 0.0235 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.723 _diffrn_reflns_theta_max 27.089 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_point_group_measured_fraction_full 0.995 _reflns_number_total 2920 _reflns_number_gt 2869 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.901 _reflns_Friedel_fraction_max 0.992 _reflns_Friedel_fraction_full 0.990 _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. ; _computing_data_collection 'Bruker APEX2 2011.4-1, 2011' _computing_cell_refinement 'Bruker SAINT 7.68a, 2009' _computing_data_reduction 'Bruker SAINT 7.68a, 2009' _computing_structure_solution 'Bruker SHELXTL 2008/4' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; There were several high residuals present in the final difference-Fourier map. It was not possible to determine the nature of the residuals although it was probable that diethylether and/or pentane solvents were present. The SQUEEZE routine in the PLATON program package was used to account for the electrons in the solvent accessible voids. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+0.0212P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ; Flack x determined using 1329 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.017(3) _chemical_absolute_configuration ad _refine_ls_number_reflns 2920 _refine_ls_number_parameters 152 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0190 _refine_ls_R_factor_gt 0.0186 _refine_ls_wR_factor_ref 0.0520 _refine_ls_wR_factor_gt 0.0518 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.015 _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_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 Ga1 Ga 0.3333 0.6667 0.74148(3) 0.01681(10) Uani 1 3 d S T P . . S1 S 0.07317(4) 0.51812(4) 0.76338(4) 0.01860(12) Uani 1 1 d . . . . . O1 O 0.09909(11) 0.57816(12) 0.86582(13) 0.0219(3) Uani 1 1 d . . . . . O2 O 0.01986(13) 0.55248(12) 0.68207(13) 0.0256(3) Uani 1 1 d . . . . . N1 N 0.3333 0.6667 0.5576(3) 0.0237(7) Uani 1 3 d S T P . . N2 N 0.18898(13) 0.52866(12) 0.71989(13) 0.0201(4) Uani 1 1 d . . . . . N3 N 0.3333 0.6667 0.9055(3) 0.0181(7) Uani 1 3 d S T P . . H3 H 0.2663(19) 0.644(2) 0.929(2) 0.025(6) Uiso 1 1 d . . . . . C1 C 0.22162(18) 0.57183(19) 0.52413(18) 0.0269(4) Uani 1 1 d . . . . . H1A H 0.2280 0.5417 0.4528 0.032 Uiso 1 1 calc R U . . . H1B H 0.1665 0.5985 0.5170 0.032 Uiso 1 1 calc R U . . . C2 C 0.18190(18) 0.47982(18) 0.61021(18) 0.0254(4) Uani 1 1 d . . . . . H2A H 0.1028 0.4207 0.5951 0.030 Uiso 1 1 calc R U . . . H2B H 0.2297 0.4441 0.6079 0.030 Uiso 1 1 calc R U . . . C3 C -0.01924(16) 0.37103(16) 0.79169(17) 0.0193(4) Uani 1 1 d . . . . . C4 C 0.00783(17) 0.32277(17) 0.87993(18) 0.0226(4) Uani 1 1 d . . . . . C5 C -0.06588(18) 0.21008(19) 0.90518(19) 0.0281(5) Uani 1 1 d . . . . . H5A H -0.0486 0.1776 0.9653 0.034 Uiso 1 1 calc R U . . . C6 C -0.16361(19) 0.14312(19) 0.8463(2) 0.0305(5) Uani 1 1 d . . . . . C7 C -0.18769(16) 0.19190(16) 0.7593(2) 0.0264(5) Uani 1 1 d . . . . . H7A H -0.2542 0.1466 0.7181 0.032 Uiso 1 1 calc R U . . . C8 C -0.11828(15) 0.30494(16) 0.72966(17) 0.0226(4) Uani 1 1 d . . . . . C9 C 0.11141(18) 0.38596(18) 0.95058(19) 0.0253(4) Uani 1 1 d . . . . . H9A H 0.1209 0.3320 0.9956 0.038 Uiso 1 1 calc R U . . . H9B H 0.1023 0.4388 0.9977 0.038 Uiso 1 1 calc R U . . . H9C H 0.1783 0.4281 0.9044 0.038 Uiso 1 1 calc R U . . . C10 C -0.2409(2) 0.0200(2) 0.8759(2) 0.0442(7) Uani 1 1 d . . . . . H10A H -0.1970 -0.0188 0.8789 0.066 Uiso 1 1 calc R U . . . H10B H -0.3005 -0.0160 0.8209 0.066 Uiso 1 1 calc R U . . . H10C H -0.2753 0.0153 0.9472 0.066 Uiso 1 1 calc R U . . . C11 C -0.15660(19) 0.34607(19) 0.63324(19) 0.0284(5) Uani 1 1 d . . . . . H11A H -0.2241 0.2823 0.6010 0.043 Uiso 1 1 calc R U . . . H11B H -0.0960 0.3787 0.5789 0.043 Uiso 1 1 calc R U . . . H11C H -0.1745 0.4038 0.6573 0.043 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga1 0.01502(12) 0.01502(12) 0.02038(18) 0.000 0.000 0.00751(6) S1 0.0152(2) 0.0155(2) 0.0247(3) -0.00311(17) -0.00187(17) 0.00746(17) O1 0.0182(7) 0.0189(7) 0.0291(8) -0.0054(6) -0.0012(6) 0.0096(6) O2 0.0230(8) 0.0207(7) 0.0338(9) -0.0008(6) -0.0047(6) 0.0114(6) N1 0.0240(11) 0.0240(11) 0.0232(16) 0.000 0.000 0.0120(6) N2 0.0163(7) 0.0170(7) 0.0251(10) -0.0047(6) 0.0005(6) 0.0068(6) N3 0.0165(10) 0.0165(10) 0.0213(16) 0.000 0.000 0.0083(5) C1 0.0254(11) 0.0287(11) 0.0248(10) -0.0066(9) -0.0045(9) 0.0123(9) C2 0.0239(10) 0.0213(10) 0.0283(11) -0.0085(9) -0.0016(8) 0.0093(9) C3 0.0161(9) 0.0157(9) 0.0253(10) -0.0032(7) -0.0005(7) 0.0073(7) C4 0.0193(9) 0.0221(10) 0.0274(10) -0.0026(8) -0.0018(8) 0.0111(8) C5 0.0224(10) 0.0247(11) 0.0354(12) 0.0047(9) -0.0015(9) 0.0105(9) C6 0.0205(11) 0.0226(11) 0.0455(15) 0.0048(10) 0.0030(9) 0.0086(9) C7 0.0167(8) 0.0225(9) 0.0359(12) -0.0052(10) -0.0055(9) 0.0068(7) C8 0.0185(8) 0.0231(9) 0.0277(12) -0.0038(9) -0.0009(8) 0.0116(7) C9 0.0235(10) 0.0227(10) 0.0298(11) -0.0011(9) -0.0048(9) 0.0115(9) C10 0.0261(12) 0.0254(12) 0.068(2) 0.0116(12) -0.0047(13) 0.0034(10) C11 0.0240(11) 0.0249(11) 0.0315(11) -0.0051(9) -0.0100(9) 0.0087(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 N2 1.9460(15) . ? Ga1 N2 1.9461(15) 3_565 ? Ga1 N2 1.9461(15) 2_665 ? Ga1 N3 2.015(3) . ? Ga1 N1 2.259(4) . ? S1 O2 1.4451(15) . ? S1 O1 1.4461(15) . ? S1 N2 1.6050(16) . ? S1 C3 1.791(2) . ? N1 C1 1.482(2) 3_565 ? N1 C1 1.482(2) 2_665 ? N1 C1 1.482(2) . ? N2 C2 1.485(3) . ? C1 C2 1.519(3) . ? C3 C4 1.410(3) . ? C3 C8 1.415(3) . ? C4 C5 1.388(3) . ? C4 C9 1.509(3) . ? C5 C6 1.385(3) . ? C6 C7 1.383(3) . ? C6 C10 1.515(3) . ? C7 C8 1.396(3) . ? C8 C11 1.512(3) . ? 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 N2 Ga1 N2 118.17(2) . 3_565 ? N2 Ga1 N2 118.17(2) . 2_665 ? N2 Ga1 N2 118.17(2) 3_565 2_665 ? N2 Ga1 N3 97.84(5) . . ? N2 Ga1 N3 97.84(5) 3_565 . ? N2 Ga1 N3 97.84(5) 2_665 . ? N2 Ga1 N1 82.16(5) . . ? N2 Ga1 N1 82.16(5) 3_565 . ? N2 Ga1 N1 82.16(5) 2_665 . ? N3 Ga1 N1 180.0 . . ? O2 S1 O1 115.99(9) . . ? O2 S1 N2 111.92(9) . . ? O1 S1 N2 106.75(8) . . ? O2 S1 C3 108.14(9) . . ? O1 S1 C3 107.54(9) . . ? N2 S1 C3 105.97(8) . . ? C1 N1 C1 112.59(14) 3_565 2_665 ? C1 N1 C1 112.59(14) 3_565 . ? C1 N1 C1 112.59(14) 2_665 . ? C1 N1 Ga1 106.13(16) 3_565 . ? C1 N1 Ga1 106.13(16) 2_665 . ? C1 N1 Ga1 106.13(16) . . ? C2 N2 S1 114.95(14) . . ? C2 N2 Ga1 111.42(12) . . ? S1 N2 Ga1 121.08(9) . . ? N1 C1 C2 108.3(2) . . ? N2 C2 C1 110.16(17) . . ? C4 C3 C8 120.42(18) . . ? C4 C3 S1 118.07(15) . . ? C8 C3 S1 121.49(15) . . ? C5 C4 C3 118.38(19) . . ? C5 C4 C9 117.22(19) . . ? C3 C4 C9 124.39(18) . . ? C6 C5 C4 122.7(2) . . ? C7 C6 C5 117.9(2) . . ? C7 C6 C10 121.2(2) . . ? C5 C6 C10 120.9(2) . . ? C6 C7 C8 122.7(2) . . ? C7 C8 C3 117.88(19) . . ? C7 C8 C11 116.46(18) . . ? C3 C8 C11 125.67(18) . . ? _refine_diff_density_max 0.257 _refine_diff_density_min -0.163 _refine_diff_density_rms 0.039 _shelxl_version_number 2013-3 _shelx_res_file ; TITL asb234 in P6(3) CELL 0.71073 13.6450 13.6450 12.2882 90.000 90.000 120.000 ZERR 2.00 0.0009 0.0009 0.0008 0.000 0.000 0.000 LATT -1 SYMM -Y, X-Y, Z SYMM -X+Y, -X, Z SYMM -X, -Y, 0.5+Z SYMM Y, -X+Y, 0.5+Z SYMM X-Y, X, 0.5+Z SFAC C H N O S GA UNIT 66 96 10 12 6 2 TEMP -130.000 SIZE 0.144 0.25 0.29 rem Nathaniel Sickerman 20s ccd2 rem APEX2 2011.4-1, SAINT 7.68a, SADABS 2008/1, SHELXTL 2008/4 & 2013/3 shel 100 0.78 L.S. 12 acta FMAP 2 PLAN 10 ABIN WGHT 0.034400 0.021200 FVAR 0.14706 GA1 6 0.333333 0.666667 0.741481 10.33333 0.01502 0.01502 = 0.02038 0.00000 0.00000 0.00751 S1 5 0.073168 0.518117 0.763380 11.00000 0.01524 0.01554 = 0.02471 -0.00311 -0.00187 0.00746 O1 4 0.099086 0.578158 0.865822 11.00000 0.01823 0.01891 = 0.02911 -0.00536 -0.00117 0.00961 O2 4 0.019865 0.552484 0.682071 11.00000 0.02297 0.02067 = 0.03379 -0.00079 -0.00469 0.01142 N1 3 0.333333 0.666667 0.557633 10.33333 0.02397 0.02397 = 0.02317 0.00000 0.00000 0.01198 N2 3 0.188975 0.528665 0.719885 11.00000 0.01633 0.01699 = 0.02507 -0.00474 0.00047 0.00682 N3 3 0.333333 0.666667 0.905464 10.33333 0.01652 0.01652 = 0.02127 0.00000 0.00000 0.00826 H3 2 0.266342 0.643594 0.929226 11.00000 0.02524 C1 1 0.221623 0.571829 0.524134 11.00000 0.02544 0.02870 = 0.02482 -0.00657 -0.00449 0.01228 AFIX 23 H1A 2 0.228034 0.541735 0.452821 11.00000 -1.20000 H1B 2 0.166481 0.598504 0.517026 11.00000 -1.20000 AFIX 0 C2 1 0.181902 0.479824 0.610212 11.00000 0.02389 0.02125 = 0.02833 -0.00848 -0.00160 0.00931 AFIX 23 H2A 2 0.102780 0.420687 0.595084 11.00000 -1.20000 H2B 2 0.229659 0.444127 0.607891 11.00000 -1.20000 AFIX 0 C3 1 -0.019240 0.371027 0.791693 11.00000 0.01608 0.01567 = 0.02535 -0.00319 -0.00055 0.00734 C4 1 0.007830 0.322775 0.879928 11.00000 0.01931 0.02215 = 0.02737 -0.00260 -0.00183 0.01114 C5 1 -0.065885 0.210081 0.905183 11.00000 0.02240 0.02473 = 0.03536 0.00474 -0.00154 0.01052 AFIX 43 H5A 2 -0.048607 0.177555 0.965278 11.00000 -1.20000 AFIX 0 C6 1 -0.163610 0.143124 0.846321 11.00000 0.02054 0.02264 = 0.04552 0.00479 0.00301 0.00859 C7 1 -0.187687 0.191895 0.759345 11.00000 0.01666 0.02252 = 0.03592 -0.00517 -0.00552 0.00677 AFIX 43 H7A 2 -0.254228 0.146585 0.718071 11.00000 -1.20000 AFIX 0 C8 1 -0.118285 0.304945 0.729663 11.00000 0.01855 0.02313 = 0.02774 -0.00376 -0.00090 0.01160 C9 1 0.111405 0.385957 0.950576 11.00000 0.02345 0.02268 = 0.02979 -0.00115 -0.00481 0.01154 AFIX 137 H9A 2 0.120907 0.331981 0.995569 11.00000 -1.50000 H9B 2 0.102326 0.438850 0.997661 11.00000 -1.50000 H9C 2 0.178267 0.428084 0.904393 11.00000 -1.50000 AFIX 0 C10 1 -0.240941 0.020032 0.875940 11.00000 0.02612 0.02545 = 0.06848 0.01164 -0.00470 0.00340 AFIX 137 H10A 2 -0.196980 -0.018831 0.878876 11.00000 -1.50000 H10B 2 -0.300543 -0.015961 0.820914 11.00000 -1.50000 H10C 2 -0.275327 0.015253 0.947191 11.00000 -1.50000 AFIX 0 C11 1 -0.156596 0.346069 0.633241 11.00000 0.02397 0.02488 = 0.03150 -0.00514 -0.01003 0.00868 AFIX 137 H11A 2 -0.224102 0.282341 0.601021 11.00000 -1.50000 H11B 2 -0.095980 0.378747 0.578877 11.00000 -1.50000 H11C 2 -0.174542 0.403779 0.657319 11.00000 -1.50000 AFIX 0 HKLF 4 REM asb234 in P6(3) REM R1 = 0.0186 for 2869 Fo > 4sig(Fo) and 0.0190 for all 2920 data REM 152 parameters refined using 1 restraints END WGHT 0.0344 0.0212 REM Highest difference peak 0.257, deepest hole -0.163, 1-sigma level 0.039 Q1 1 0.1303 0.5201 0.7421 11.00000 0.05 0.26 Q2 1 0.0245 0.4417 0.7770 11.00000 0.05 0.23 Q3 1 -0.0678 0.3363 0.7546 11.00000 0.05 0.22 Q4 1 -0.1463 0.2471 0.7469 11.00000 0.05 0.22 Q5 1 0.2551 0.5895 0.7422 11.00000 0.05 0.19 Q6 1 -0.3214 0.0141 0.8971 11.00000 0.05 0.19 Q7 1 -0.2260 -0.0015 0.9395 11.00000 0.05 0.18 Q8 1 -0.1904 0.1709 0.8178 11.00000 0.05 0.18 Q9 1 -0.2382 -0.0158 0.8215 11.00000 0.05 0.17 Q10 1 0.0811 0.5578 0.8187 11.00000 0.05 0.17 ; _shelx_res_checksum 42819 _shelx_hkl_file ; 0 1 0 135.95 5.77 1 -1 0 136.49 5.79 1 0 0 131.77 5.78 0 1 0 128.36 6.06 1 0 0 138.93 5.75 -1 1 0 134.21 5.95 0 1 0 136.29 5.92 0 1 0 141.00 5.73 -2 1 0 61.85 2.76 1 1 0 60.00 2.77 1 -2 0 61.03 2.66 1 -2 0 62.24 2.62 2 -1 0 62.49 2.64 1 1 0 61.11 2.67 -1 2 0 61.59 2.80 -1 2 0 62.79 2.72 2 -1 0 62.94 2.67 -1 -1 0 59.09 2.71 2 -2 0 85.82 3.58 -2 0 0 86.42 3.73 0 2 0 86.10 3.72 -2 2 0 86.79 3.81 2 -2 0 86.28 3.65 2 0 0 84.24 3.66 0 2 0 83.43 3.81 2 0 0 84.77 3.63 2 0 0 84.34 3.77 -2 2 0 84.25 3.74 0 2 0 85.10 3.62 0 2 0 81.71 3.64 3 -1 0 3.02 0.21 1 2 0 2.85 0.21 -2 3 0 2.93 0.22 -3 1 0 3.00 0.23 1 2 0 2.96 0.22 1 2 0 3.03 0.21 -2 3 0 2.91 0.22 3 -1 0 3.07 0.17 1 2 0 2.88 0.19 2 -3 0 2.74 0.20 3 -2 0 30.50 1.39 -1 3 0 30.30 1.46 1 -3 0 30.63 1.38 -2 -1 0 31.16 1.41 -1 3 0 31.28 1.41 -3 2 0 31.75 1.43 3 -2 0 31.77 1.35 2 1 0 30.16 1.40 -1 3 0 31.23 1.35 2 1 0 31.47 1.41 -3 2 0 31.29 1.44 -3 3 0 60.51 2.80 0 3 0 60.07 2.67 3 -3 0 61.75 2.68 -3 3 0 61.97 2.75 0 3 0 62.03 2.81 0 3 0 60.78 2.72 -3 0 0 61.90 2.75 -3 3 0 62.11 2.60 3 0 0 61.51 2.68 3 0 0 59.93 2.73 0 3 0 60.05 2.65 3 0 0 60.15 2.69 1 3 0 0.91 0.14 -3 4 0 0.91 0.15 4 -1 0 1.03 0.10 -4 1 0 0.79 0.16 4 -1 0 0.95 0.14 4 -1 0 1.04 0.16 1 3 0 1.10 0.15 -3 4 0 0.98 0.16 1 3 0 1.02 0.15 1 3 0 1.11 0.14 3 -4 0 0.86 0.14 2 2 0 255.67 11.03 -4 2 0 258.14 11.35 2 -4 0 259.23 10.96 4 -2 0 260.36 11.10 2 -4 0 264.50 11.08 2 2 0 262.49 11.55 2 2 0 257.09 11.09 4 -2 0 268.43 11.53 -2 4 0 261.25 11.32 -2 -2 0 252.09 11.30 -2 4 0 257.69 11.60 4 -2 0 260.74 10.99 -4 3 0 7.16 0.45 -3 -1 0 7.47 0.44 4 -3 0 7.67 0.38 1 -4 0 7.54 0.39 1 -4 0 7.40 0.42 -1 4 0 7.53 0.42 3 1 0 7.55 0.45 -1 4 0 7.64 0.46 4 -3 0 7.81 0.45 -4 3 0 7.75 0.43 3 1 0 7.63 0.39 3 1 0 7.78 0.45 4 -4 0 0.85 0.15 -4 4 0 1.00 0.17 0 4 0 1.20 0.16 -4 0 0 1.07 0.18 4 0 0 0.93 0.16 4 0 0 1.28 0.18 0 4 0 0.98 0.16 -4 4 0 1.09 0.09 0 4 0 1.14 0.15 -4 4 0 1.31 0.18 4 0 0 1.25 0.10 0 4 0 1.24 0.15 5 -1 0 21.05 0.98 1 4 0 20.77 1.03 -4 5 0 21.32 1.09 -4 5 0 21.20 1.06 -5 1 0 21.76 1.08 1 4 0 22.18 1.02 1 4 0 21.08 1.07 5 -1 0 21.60 1.03 5 -1 0 20.75 1.05 1 4 0 20.94 1.03 4 -5 0 20.94 1.03 5 -2 0 13.68 0.71 2 3 0 13.00 0.70 2 3 0 12.92 0.70 2 3 0 13.23 0.70 -5 2 0 13.14 0.74 -3 5 0 12.58 0.70 5 -2 0 13.49 0.68 5 -2 0 13.89 0.65 -2 -3 0 13.35 0.68 -3 5 0 13.34 0.74 3 -5 0 13.56 0.69 -2 5 0 188.71 8.32 -5 3 0 193.02 8.48 2 -5 0 193.18 8.03 -2 5 0 190.92 8.55 -3 -2 0 192.12 8.31 5 -3 0 187.97 8.17 -5 3 0 189.50 8.36 2 -5 0 187.73 8.14 5 -3 0 190.13 8.06 3 2 0 188.09 8.16 3 2 0 185.96 8.12 3 2 0 189.12 8.46 5 -4 0 171.84 7.33 1 -5 0 173.97 7.23 1 -5 0 168.58 7.31 -5 4 0 170.76 7.51 -1 5 0 168.25 7.45 -5 4 0 172.89 7.20 -1 5 0 168.88 7.67 -4 -1 0 172.12 7.48 4 1 0 167.52 7.34 -5 4 0 167.76 7.63 4 1 0 169.60 7.56 4 1 0 167.59 7.30 0 5 0 44.92 2.06 0 5 0 45.19 2.17 5 -5 0 45.14 2.07 5 0 0 43.47 2.08 -5 0 0 43.96 2.12 -5 5 0 46.92 1.94 5 0 0 46.18 2.08 0 5 0 44.38 2.07 -5 5 0 45.80 2.13 5 0 0 45.81 2.04 0 -5 0 46.78 2.04 -5 5 0 46.08 2.16 1 5 0 10.56 0.64 1 5 0 10.29 0.62 1 5 0 10.83 0.62 6 -1 0 11.60 0.53 5 -6 0 10.48 0.62 -1 -5 0 10.89 0.62 -6 1 0 11.26 0.66 -5 6 0 11.53 0.66 -5 6 0 10.85 0.65 1 5 0 10.95 0.59 6 -1 0 11.30 0.63 6 -1 0 10.07 0.64 2 4 0 84.39 3.71 -6 2 0 83.42 3.83 2 4 0 83.57 3.72 6 -2 0 84.20 3.69 -4 6 0 84.16 3.80 2 4 0 84.81 3.86 -4 6 0 84.60 3.91 6 -2 0 85.91 3.78 6 -2 0 83.64 3.74 -2 -4 0 82.23 3.75 4 -6 0 85.26 3.72 6 -3 0 121.61 5.42 3 3 0 124.78 5.59 -3 6 0 124.06 5.51 -3 -3 0 126.16 5.49 6 -3 0 125.42 5.57 6 -3 0 126.27 5.34 3 3 0 121.48 5.41 -6 3 0 121.60 5.55 3 -6 0 121.84 5.39 3 3 0 121.66 5.39 3 -6 0 127.57 5.26 -3 6 0 125.96 5.68 -2 6 0 3.79 0.30 4 2 0 3.85 0.34 2 -6 0 4.05 0.31 -6 4 0 3.38 0.32 2 -6 0 4.02 0.25 -2 6 0 3.90 0.34 6 -4 0 3.89 0.33 4 2 0 3.71 0.33 -6 4 0 4.11 0.27 4 2 0 3.70 0.25 -4 -2 0 3.73 0.30 -6 4 0 3.73 0.28 6 -5 0 13.48 0.76 -6 5 0 13.90 0.65 -6 5 0 12.99 0.78 -5 -1 0 13.60 0.76 -1 6 0 13.29 0.80 -6 5 0 13.73 0.76 1 -6 0 13.88 0.74 1 -6 0 14.48 0.70 -1 6 0 14.04 0.73 5 1 0 13.55 0.77 5 1 0 14.15 0.77 5 1 0 14.02 0.67 6 0 0 159.57 6.99 -6 0 0 162.69 7.13 6 -6 0 160.26 6.97 0 6 0 160.37 7.07 0 6 0 159.40 6.96 0 6 0 158.20 7.29 -6 6 0 162.79 7.28 0 -6 0 162.99 6.90 6 0 0 157.60 6.94 -6 6 0 160.48 7.14 1 6 0 11.40 0.69 -6 7 0 10.83 0.68 1 6 0 10.55 0.62 6 -7 0 11.08 0.66 -7 1 0 11.30 0.71 -6 7 0 10.91 0.69 7 -1 0 11.23 0.67 1 6 0 11.37 0.67 7 -1 0 11.50 0.70 -1 -6 0 11.34 0.65 7 -2 0 9.12 0.46 -2 -5 0 9.35 0.53 2 5 0 8.63 0.56 7 -2 0 8.83 0.55 5 -7 0 9.17 0.56 -2 -5 0 9.52 0.58 -7 2 0 8.48 0.59 2 5 0 8.99 0.57 -5 7 0 8.57 0.56 2 5 0 8.37 0.56 -5 7 0 9.45 0.61 3 4 0 4.69 0.35 -3 -4 0 4.56 0.34 3 4 0 4.30 0.37 -4 7 0 4.84 0.37 -7 3 0 4.89 0.42 7 -3 0 5.08 0.30 -7 3 0 4.79 0.36 3 4 0 4.37 0.37 4 -7 0 4.47 0.36 -4 7 0 4.63 0.39 -7 4 0 71.18 3.35 4 3 0 73.70 3.32 -3 7 0 72.72 3.31 3 -7 0 72.99 3.12 -3 7 0 72.53 3.44 4 3 0 71.48 3.26 -4 -3 0 72.05 3.29 4 3 0 71.38 3.27 3 -7 0 73.02 3.24 7 -4 0 74.49 3.33 -7 4 0 72.66 3.18 7 -4 0 72.93 3.28 -5 -2 0 9.83 0.60 7 -5 0 9.53 0.61 -2 7 0 9.29 0.64 -7 5 0 10.24 0.65 5 2 0 8.97 0.61 -2 7 0 9.87 0.58 5 2 0 9.57 0.62 2 -7 0 10.23 0.53 5 2 0 9.52 0.52 -7 5 0 10.16 0.59 -7 5 0 10.15 0.52 2 -7 0 10.23 0.59 -1 7 0 55.68 2.74 6 1 0 56.43 2.62 1 -7 0 56.77 2.60 -7 6 0 57.68 2.70 6 1 0 56.59 2.64 -7 6 0 58.54 2.47 -7 6 0 55.38 2.69 7 -6 0 56.69 2.62 6 1 0 57.58 2.57 -6 -1 0 56.96 2.67 -1 7 0 57.12 2.62 1 -7 0 58.17 2.54 -7 7 0 16.03 0.92 7 0 0 16.12 0.92 0 -7 0 16.39 0.86 -7 0 0 16.01 0.92 7 0 0 16.52 0.92 0 7 0 16.64 0.87 7 -7 0 15.69 0.89 0 7 0 15.74 0.94 0 7 0 16.37 0.89 -7 7 0 16.27 0.93 1 7 0 111.13 5.14 7 -8 0 109.03 4.92 1 7 0 112.14 4.92 -1 -7 0 113.41 4.88 -7 8 0 109.36 5.04 -8 1 0 112.09 4.92 8 -1 0 106.85 4.95 -8 1 0 111.95 5.06 1 7 0 112.26 4.97 -7 8 0 110.55 5.15 -6 8 0 55.40 2.67 -8 2 0 56.98 2.60 -2 -6 0 57.25 2.60 2 6 0 57.84 2.61 2 6 0 56.85 2.71 8 -2 0 55.93 2.64 8 -2 0 56.93 2.55 2 6 0 55.93 2.61 -6 8 0 55.49 2.74 -8 2 0 56.38 2.70 -2 -6 0 56.77 2.60 6 -8 0 55.41 2.60 -8 3 0 14.40 0.79 -5 8 0 13.98 0.87 5 -8 0 13.76 0.80 -8 3 0 14.56 0.86 8 -3 0 14.85 0.85 8 -3 0 14.37 0.72 -5 8 0 13.88 0.82 -3 -5 0 13.94 0.77 3 5 0 14.52 0.81 3 5 0 14.17 0.82 -3 -5 0 14.60 0.83 -8 4 0 11.24 0.74 4 -8 0 11.73 0.69 -4 8 0 11.71 0.70 -4 8 0 11.25 0.75 4 4 0 11.91 0.73 -8 4 0 12.27 0.67 -4 -4 0 12.09 0.73 4 4 0 11.27 0.71 -4 -4 0 11.97 0.68 4 4 0 11.83 0.67 8 -4 0 12.15 0.73 8 -4 0 12.26 0.64 -8 5 0 16.43 0.97 5 3 0 16.04 0.84 -5 -3 0 16.76 0.90 -3 8 0 16.58 0.90 -3 8 0 15.89 0.97 3 -8 0 16.82 0.79 3 -8 0 16.00 0.88 -5 -3 0 16.52 0.94 5 3 0 16.93 0.94 -8 5 0 16.91 0.84 5 3 0 16.61 0.94 8 -5 0 16.72 0.87 -6 -2 0 79.78 3.67 -8 6 0 83.84 3.52 6 2 0 79.24 3.67 -2 8 0 78.95 3.85 -8 6 0 82.97 3.77 -2 8 0 80.40 3.69 2 -8 0 81.77 3.54 2 -8 0 81.31 3.64 6 2 0 82.13 3.67 8 -6 0 79.68 3.67 -6 -2 0 82.47 3.72 -8 6 0 82.75 3.78 6 2 0 79.10 3.68 -7 -1 0 213.74 9.67 1 -8 0 216.70 9.45 1 -8 0 221.60 9.35 7 1 0 214.16 9.50 -1 8 0 227.40 9.63 -8 7 0 219.12 9.87 -1 8 0 220.80 9.93 8 -7 0 212.62 9.47 -8 7 0 218.78 9.72 -7 -1 0 219.27 9.46 -8 8 0 35.21 1.82 -8 0 0 35.64 1.78 8 0 0 34.89 1.79 0 8 0 35.00 1.75 0 -8 0 36.81 1.72 8 -8 0 36.12 1.77 0 8 0 35.81 1.85 -8 0 0 35.14 1.81 0 8 0 36.29 1.74 -8 8 0 36.95 1.84 -8 9 0 12.68 0.83 -9 1 0 12.41 0.80 1 8 0 12.77 0.79 9 -1 0 12.85 0.83 -8 9 0 12.80 0.83 -1 -8 0 12.98 0.78 1 8 0 12.75 0.74 8 -9 0 12.97 0.80 1 8 0 12.38 0.82 -9 1 0 12.50 0.84 2 7 0 3.58 0.38 -9 2 0 3.66 0.43 2 7 0 3.43 0.38 -2 -7 0 3.22 0.36 -7 9 0 3.44 0.39 7 -9 0 3.61 0.38 2 7 0 3.94 0.35 -9 2 0 3.81 0.38 9 -2 0 3.75 0.42 -2 -7 0 3.46 0.33 -7 9 0 3.41 0.39 3 6 0 52.69 2.46 6 -9 0 52.72 2.45 -3 -6 0 51.89 2.43 9 -3 0 50.27 2.48 -9 3 0 52.36 2.43 -6 9 0 51.84 2.51 -9 3 0 51.54 2.55 -3 -6 0 52.41 2.46 -6 9 0 54.06 2.61 3 6 0 52.45 2.52 5 -9 0 18.54 0.99 9 -4 0 18.00 1.03 -5 9 0 17.22 1.06 -4 -5 0 17.34 0.96 -4 -5 0 17.96 1.02 -5 9 0 16.62 0.98 4 5 0 17.76 1.01 -9 4 0 18.66 1.06 9 -4 0 18.51 0.91 -9 4 0 18.90 0.97 4 5 0 17.62 0.97 4 -9 0 5.66 0.45 -9 5 0 5.35 0.49 -4 9 0 6.09 0.46 5 4 0 5.39 0.47 -9 5 0 6.03 0.42 -5 -4 0 5.82 0.49 -5 -4 0 5.29 0.44 9 -5 0 6.15 0.40 9 -5 0 5.54 0.48 -4 9 0 5.73 0.51 5 4 0 6.13 0.41 -3 9 0 34.16 1.68 6 3 0 33.18 1.69 -9 6 0 35.92 1.57 6 3 0 33.89 1.61 -6 -3 0 33.89 1.68 -6 -3 0 32.25 1.69 9 -6 0 33.79 1.67 9 -6 0 33.73 1.70 -3 9 0 31.79 1.77 3 -9 0 34.42 1.66 -9 6 0 34.37 1.76 2 -9 0 3.19 0.34 -7 -2 0 3.58 0.40 -9 7 0 3.59 0.36 -2 9 0 3.06 0.32 -9 7 0 3.03 0.40 9 -7 0 3.56 0.39 -7 -2 0 2.97 0.36 2 -9 0 3.46 0.30 7 2 0 2.98 0.38 -2 9 0 2.85 0.38 -9 8 0 25.80 1.37 -1 9 0 24.64 1.42 9 -8 0 25.44 1.36 -9 8 0 24.40 1.39 -8 -1 0 26.17 1.38 1 -9 0 26.03 1.27 8 1 0 25.41 1.37 -1 9 0 26.31 1.31 1 -9 0 25.53 1.32 -8 -1 0 24.16 1.36 -9 0 0 60.70 2.93 9 0 0 58.63 2.88 9 -9 0 61.09 2.87 -9 9 0 62.48 2.98 0 -9 0 62.14 2.80 0 9 0 60.64 3.00 0 9 0 61.65 2.84 -9 9 0 58.19 2.93 -9 0 0 60.47 2.87 0 9 0 61.87 2.86 1 9 0 19.25 1.10 1 9 0 19.41 1.05 -9 10 0 18.62 1.14 9 -10 0 19.11 1.11 1 9 0 18.50 1.14 -10 1 0 19.20 1.11 -9 10 0 18.94 1.15 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0.08 0 -4 -15 0.10 -0.08 4 -4 -15 -0.09 0.08 4 0 -15 0.09 -0.08 -4 0 -15 -0.09 0.08 0 -4 15 -0.10 -0.08 -4 4 15 -0.09 -0.08 4 0 15 -0.09 -0.08 4 -4 15 0.09 0.08 0 -4 15 -0.10 -0.08 0 4 15 0.10 0.08 1 4 -15 -0.15 0.25 4 -5 -15 -0.14 0.26 -4 5 -15 0.14 -0.26 -1 -4 15 -0.15 -0.25 -4 5 15 -0.14 -0.26 -1 -4 15 -0.15 -0.25 5 -2 -15 0.07 -0.37 -5 2 -15 -0.07 0.37 3 -5 -15 -0.08 0.38 -3 5 -15 0.08 -0.38 -2 -3 15 -0.08 -0.38 3 -5 15 0.08 0.38 -2 -3 15 -0.08 -0.38 -3 5 15 -0.08 -0.38 -5 3 -15 0.00 0.32 -2 5 -15 0.00 -0.34 2 -5 -15 0.00 0.34 5 -3 -15 0.00 -0.32 2 -5 15 0.00 0.34 -2 5 15 0.00 -0.34 -3 -2 15 0.00 -0.33 -5 4 -15 -0.06 0.12 5 -4 -15 0.06 -0.12 1 -5 -15 -0.06 0.13 -1 5 -15 0.06 -0.13 1 -5 15 0.06 0.13 -5 4 15 0.06 0.12 -4 -1 15 -0.06 -0.13 1 -5 15 0.06 0.13 5 -5 -15 -0.06 0.03 0 5 -15 -0.06 0.02 -5 5 -15 0.06 -0.03 0 -5 15 -0.06 -0.02 -5 5 15 -0.06 -0.03 0 -5 15 -0.06 -0.02 -5 6 -15 0.26 -0.06 5 -6 -15 -0.26 0.06 -1 -5 15 -0.26 -0.06 -1 -5 15 -0.26 -0.06 -5 6 15 -0.26 -0.06 4 -6 -15 -0.15 0.24 -4 6 -15 0.15 -0.24 -2 -4 15 -0.15 -0.24 -3 6 -15 0.20 -0.30 -6 3 -15 -0.19 0.29 3 -6 -15 -0.20 0.30 -3 -3 15 -0.20 -0.30 -2 6 -15 0.24 -0.19 -6 4 -15 -0.24 0.17 2 -6 15 0.24 0.19 -4 -2 15 -0.23 -0.18 -6 5 -15 -0.05 0.09 1 -6 15 0.04 0.09 -6 6 -15 0.12 0.11 -6 6 15 -0.12 0.11 -6 0 15 0.13 -0.12 0 -6 15 -0.11 0.11 -7 1 15 0.19 -0.11 -5 7 -15 0.26 -0.07 -4 7 -15 0.21 -0.15 -3 7 -15 0.14 -0.09 -3 7 -15 0.14 -0.09 -2 0 16 0.03 -0.31 -3 1 16 -0.15 -0.28 -2 -1 16 -0.17 -0.27 -3 0 16 -0.25 -0.19 -4 2 16 -0.46 -0.13 -4 2 16 -0.46 -0.13 0 0 0 0.00 0.00 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.075 303 82 ' ' 2 0.333 0.667 0.296 10 0 ' ' 3 0.667 0.333 0.796 10 0 ' ' _platon_squeeze_details TITL asb234 in P6(3) CELL 13.6450 13.6450 12.2882 90.00 90.00 120.00 SPGR P63 # Note: Atoms in Void as Cxxx and Qxxx all others C101 1.000 1.003 0.235 ! 3.62 eA-3 C102 0.908 0.018 0.151 ! 2.72 eA-3 C103 1.000 0.999 0.547 ! 2.51 eA-3 C104 0.920 0.990 0.066 ! 2.49 eA-3 C105 0.999 0.891 0.640 ! 2.25 eA-3 C106 0.014 0.937 0.674 ! 1.85 eA-3 ; _shelx_fab_checksum 61344 _database_code_depnum_ccdc_archive 'CCDC 971645'