#------------------------------------------------------------------------------ #$Date: 2019-11-07 21:39:51 +0200 (Thu, 07 Nov 2019) $ #$Revision: 223572 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/28/7232869.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7232869 loop_ _publ_author_name 'Zhang, Tao' 'Ling, Bo-Kai' 'Hu, Yue-Qiao' 'Han, Tian' 'Zheng, Yan-Zhen' _publ_section_title ; An anionic manganese(ii) metal--organic framework for uranyl adsorption ; _journal_issue 26 _journal_name_full CrystEngComm _journal_page_first 3901 _journal_paper_doi 10.1039/C9CE00603F _journal_volume 21 _journal_year 2019 _chemical_formula_moiety 'C21 H3 Mn5 N6 O24' _chemical_formula_sum 'C21 H3 Mn5 N6 O24' _chemical_formula_weight 997.99 _space_group_crystal_system tetragonal _space_group_IT_number 120 _space_group_name_Hall 'I -4 -2c' _space_group_name_H-M_alt 'I -4 c 2' _symmetry_space_group_name_Hall 'I -4 -2c' _symmetry_space_group_name_H-M 'I -4 c 2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2018-03-19 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _audit_update_record ; 2019-05-11 deposited with the CCDC. 2019-06-05 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 16 _cell_length_a 26.343(7) _cell_length_b 26.343(7) _cell_length_c 37.301(11) _cell_measurement_reflns_used 9663 _cell_measurement_temperature 150 _cell_measurement_theta_max 24.890 _cell_measurement_theta_min 1.092 _cell_volume 25885(12) _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SIR2004 (Burla et al., 2007)' _diffrn_ambient_temperature 150 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omiga scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1118 _diffrn_reflns_av_unetI/netI 0.0902 _diffrn_reflns_Laue_measured_fraction_full 0.987 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 85188 _diffrn_reflns_point_group_measured_fraction_full 0.987 _diffrn_reflns_point_group_measured_fraction_max 0.987 _diffrn_reflns_theta_full 24.891 _diffrn_reflns_theta_max 24.890 _diffrn_reflns_theta_min 1.092 _exptl_absorpt_coefficient_mu 1.004 _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.024 _exptl_crystal_description cubic _exptl_crystal_F_000 7808 _platon_squeeze_details ; TITL 1 in I-4c2 CELL 26.3430 26.3430 37.3010 90.00 90.00 90.00 SPGR I-4c2 # Solvent Accessible Volume = 15045 # Electrons Found in S.A.V. = 6762 # Note: Atoms in Void as Cxxx and Qxxx all others C101 0.850 0.409 0.350 ! 8.31 eA-3 C102 0.264 0.242 0.189 ! 7.55 eA-3 C103 0.267 0.574 0.485 ! 7.40 eA-3 C104 0.345 0.180 0.385 ! 6.79 eA-3 C105 0.852 0.650 0.342 ! 6.22 eA-3 C106 0.394 0.798 0.365 ! 5.60 eA-3 C107 0.227 0.929 0.062 ! 5.45 eA-3 Q108 0.991 0.364 0.351 ! 5.12 eA-3 C109 0.451 0.197 0.384 ! 4.76 eA-3 C110 0.892 0.250 0.232 ! 4.47 eA-3 Q111 0.153 0.230 0.149 ! 4.47 eA-3 Q112 0.087 0.699 0.290 ! 4.36 eA-3 C113 0.593 0.051 0.390 ! 4.33 eA-3 C114 0.984 0.212 0.484 ! 4.27 eA-3 C115 0.208 0.144 0.182 ! 4.23 eA-3 C116 0.089 0.685 0.312 ! 4.23 eA-3 C117 0.564 0.976 0.352 ! 4.23 eA-3 C118 0.338 0.966 0.353 ! 4.08 eA-3 Q119 0.453 0.528 0.405 ! 3.97 eA-3 C120 0.079 0.042 0.493 ! 3.95 eA-3 C121 0.189 0.312 0.217 ! 3.90 eA-3 C122 0.318 0.468 0.002 ! 3.84 eA-3 C123 0.262 0.772 0.189 ! 3.84 eA-3 C124 0.031 0.787 0.055 ! 3.77 eA-3 C125 0.069 0.932 0.072 ! 3.76 eA-3 C126 0.500 0.498 0.399 ! 3.76 eA-3 C127 0.158 0.862 0.241 ! 3.69 eA-3 C128 0.038 0.713 0.070 ! 3.68 eA-3 Q129 0.345 0.191 0.171 ! 3.67 eA-3 C130 0.951 0.306 0.078 ! 3.67 eA-3 C131 0.295 0.076 0.109 ! 3.63 eA-3 C132 0.189 0.288 0.278 ! 3.58 eA-3 C133 0.189 0.709 0.784 ! 3.54 eA-3 C134 0.500 1.001 0.336 ! 3.54 eA-3 C135 0.430 0.791 0.090 ! 3.53 eA-3 C136 0.268 0.045 0.055 ! 3.48 eA-3 C137 0.282 0.857 0.009 ! 3.47 eA-3 C138 0.547 0.767 0.947 ! 3.47 eA-3 Q139 0.119 0.670 0.162 ! 3.41 eA-3 C140 0.183 0.305 0.250 ! 3.34 eA-3 C141 0.563 0.054 0.365 ! 3.33 eA-3 C142 0.015 0.046 0.027 ! 3.32 eA-3 Q143 0.788 0.103 0.006 ! 3.29 eA-3 C144 0.750 0.614 0.235 ! 3.25 eA-3 Q145 0.563 0.329 0.939 ! 3.20 eA-3 Q146 0.063 0.829 0.439 ! 3.20 eA-3 C147 0.259 0.466 0.429 ! 3.14 eA-3 C148 0.773 0.485 0.010 ! 3.12 eA-3 Q149 0.076 0.271 0.078 ! 3.11 eA-3 C150 0.484 0.856 0.382 ! 3.11 eA-3 C151 0.885 0.323 0.375 ! 3.08 eA-3 C152 0.944 0.068 0.462 ! 3.08 eA-3 C153 0.600 0.563 0.433 ! 3.05 eA-3 C154 0.906 0.341 0.398 ! 3.02 eA-3 C155 0.555 0.928 0.439 ! 3.01 eA-3 C156 0.658 0.882 0.146 ! 3.01 eA-3 Q157 0.834 0.337 0.022 ! 2.99 eA-3 C158 0.935 0.556 0.447 ! 2.98 eA-3 C159 0.532 0.208 0.092 ! 2.97 eA-3 C160 0.038 0.277 0.921 ! 2.94 eA-3 C161 0.538 0.777 0.421 ! 2.94 eA-3 C162 0.295 0.472 0.460 ! 2.94 eA-3 Q163 0.532 0.821 0.354 ! 2.93 eA-3 Q164 0.141 0.328 0.468 ! 2.92 eA-3 C165 0.486 0.145 0.383 ! 2.91 eA-3 C166 0.334 0.090 0.022 ! 2.90 eA-3 C167 0.875 0.313 0.454 ! 2.90 eA-3 C168 0.196 0.827 0.226 ! 2.88 eA-3 C169 0.937 0.464 0.403 ! 2.87 eA-3 C170 0.119 0.648 0.432 ! 2.87 eA-3 C171 0.583 0.785 0.421 ! 2.85 eA-3 C172 0.858 0.511 0.485 ! 2.83 eA-3 Q173 0.304 0.997 0.123 ! 2.80 eA-3 Q174 0.723 0.507 0.431 ! 2.75 eA-3 C175 0.092 0.401 0.014 ! 2.74 eA-3 Q176 0.213 0.702 0.179 ! 2.74 eA-3 Q177 0.339 0.835 0.094 ! 2.73 eA-3 C178 0.968 0.578 0.375 ! 2.73 eA-3 C179 0.169 0.946 0.430 ! 2.71 eA-3 C180 0.189 0.548 0.383 ! 2.70 eA-3 Q181 0.946 0.245 0.226 ! 2.70 eA-3 Q182 0.578 0.183 0.569 ! 2.70 eA-3 Q183 0.078 0.683 0.069 ! 2.70 eA-3 C184 0.390 0.842 0.058 ! 2.70 eA-3 C185 0.765 0.641 0.221 ! 2.70 eA-3 C186 0.337 0.689 0.288 ! 2.69 eA-3 Q187 0.087 0.682 0.181 ! 2.69 eA-3 C188 0.784 0.577 0.009 ! 2.67 eA-3 C189 0.320 0.684 0.344 ! 2.66 eA-3 Q190 0.726 0.213 0.670 ! 2.66 eA-3 Q191 0.501 0.848 0.161 ! 2.65 eA-3 Q192 0.586 0.110 0.155 ! 2.64 eA-3 C193 0.977 0.716 0.016 ! 2.64 eA-3 C194 0.108 0.300 0.065 ! 2.63 eA-3 Q195 0.987 0.052 0.116 ! 2.63 eA-3 C196 0.500 0.999 0.461 ! 2.61 eA-3 C197 0.454 0.863 0.407 ! 2.60 eA-3 C198 0.015 0.551 0.439 ! 2.60 eA-3 C199 0.155 0.157 0.249 ! 2.60 eA-3 ; _refine_diff_density_max 1.000 _refine_diff_density_min -1.183 _refine_diff_density_rms 0.159 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.37(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 506 _refine_ls_number_reflns 11061 _refine_ls_number_restraints 430 _refine_ls_restrained_S_all 1.036 _refine_ls_R_factor_all 0.1094 _refine_ls_R_factor_gt 0.0926 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2405 _refine_ls_wR_factor_ref 0.2546 _reflns_Friedel_coverage 0.901 _reflns_Friedel_fraction_full 0.988 _reflns_Friedel_fraction_max 0.988 _reflns_number_gt 9401 _reflns_number_total 11061 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9ce00603f2.cif _cod_data_source_block 1_sq _cod_depositor_comments 'Adding full bibliography for 7232869.cif.' _cod_original_cell_volume 25885(16) _cod_database_code 7232869 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.63(5) 0.37(5) 2. Fixed Uiso At 1.2 times of: All C(H) groups 3. Restrained distances C20-C19 2.2 with sigma of 0.02 4. Rigid bond restraints C12, C18, C20, C11, C21, C3, C10, C13, C4, C15, C19, C8, C16, C5, C14, C2, C6, C17, C1, C7, C9, N3, N1, N2, N6, N5, N4, O20, O6, O23, O17, O4, O1, O21, O19, O24, O7, O10, O16, O13, O2, O8, O3, O12, O18, O15, O11, O22, O5, O14, O9 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 5. Uiso/Uaniso restraints and constraints C12 \\sim C18 \\sim C20 \\sim C11 \\sim C21 \\sim C3 \\sim C10 \\sim C13 \\sim C4 \\sim C15 \\sim C19 \\sim C8 \\sim C16 \\sim C5 \\sim C14 \\sim C2 \\sim C6 \\sim C17 \\sim C1 \\sim C7 \\sim C9 \\sim N3 \\sim N1 \\sim N2 \\sim N6 \\sim N5 \\sim N4 \\sim O20 \\sim O6 \\sim O23 \\sim O17 \\sim O4 \\sim O1 \\sim O21 \\sim O19 \\sim O24 \\sim O7 \\sim O10 \\sim O16 \\sim O13 \\sim O2 \\sim O8 \\sim O3 \\sim O12 \\sim O18 \\sim O15 \\sim O11 \\sim O22 \\sim O5 \\sim O14 \\sim O9: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.02 Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(O6) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 6.a Aromatic/amide H refined with riding coordinates: C13(H13), C19(H19), C5(H5) ; _shelx_res_file ; 1_sq.res created by SHELXL-2014/7 TITL 1 in I-4c2 CELL 0.71073 26.343 26.343 37.301 90 90 90 ZERR 16 0.007 0.007 0.011 0 0 0 LATT -2 SYMM +Y,-X,-Z SYMM -X,-Y,+Z SYMM -Y,+X,-Z SYMM -X,+Y,0.5+Z SYMM +Y,+X,0.5-Z SYMM +X,-Y,0.5+Z SYMM -Y,-X,0.5-Z SFAC C H Mn N O UNIT 336 48 80 96 384 DFIX 2.2 C20 C19 DELU C12 C18 C20 C11 C21 C3 C10 C13 C4 C15 C19 C8 C16 C5 C14 C2 C6 C17 C1 = C7 C9 N3 N1 N2 N6 N5 N4 O20 O6 O23 O17 O4 O1 O21 O19 O24 O7 O10 O16 O13 O2 = O8 O3 O12 O18 O15 O11 O22 O5 O14 O9 SIMU 0.02 0.02 2 C12 C18 C20 C11 C21 C3 C10 C13 C4 C15 C19 C8 C16 C5 C14 C2 = C6 C17 C1 C7 C9 N3 N1 N2 N6 N5 N4 O20 O6 O23 O17 O4 O1 O21 O19 O24 O7 O10 = O16 O13 O2 O8 O3 O12 O18 O15 O11 O22 O5 O14 O9 ISOR 0.01 0.02 C6 ISOR 0.01 0.02 O6 C11 C3 C7 L.S. 10 0 477 PLAN -5 TEMP -123.15 BOND $H CONF ABIN fmap 2 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 REM REM REM WGHT 0.200000 BASF 0.36778 FVAR 0.08033 MN1 3 0.016950 0.173840 -0.160461 11.00000 0.03695 0.02981 = 0.04368 -0.00396 -0.00640 0.00442 MN3 3 -0.050581 0.357414 -0.244637 11.00000 0.03304 0.03341 = 0.04982 -0.00032 -0.00025 0.00064 MN4 3 -0.017043 0.176553 -0.336523 11.00000 0.03272 0.03906 = 0.03673 -0.00238 -0.00292 -0.00003 MN2 3 -0.137897 0.168414 -0.045105 11.00000 0.04125 0.03554 = 0.02803 0.00145 -0.00014 0.00505 MN5 3 0.221350 0.186276 -0.097440 11.00000 0.03746 0.03326 = 0.02673 0.00010 0.00078 -0.00707 O20 5 -0.063982 0.242690 -0.321268 11.00000 0.02530 0.02191 = 0.02604 0.00741 0.00575 -0.00513 O6 5 -0.164981 0.156567 0.064778 11.00000 0.06766 0.04246 = 0.01763 0.01926 -0.00163 0.01017 O23 5 0.077557 0.440782 -0.216648 11.00000 0.03879 0.03454 = 0.02996 -0.00736 0.00281 -0.00280 O17 5 -0.024617 0.248993 -0.164221 11.00000 0.04628 0.03652 = 0.04088 -0.00678 -0.01225 0.00674 O4 5 -0.183902 0.043883 -0.106002 11.00000 0.05197 0.02988 = 0.03736 0.00108 0.00048 -0.00077 O1 5 -0.002677 0.179303 -0.103365 11.00000 0.04129 0.03720 = 0.04174 -0.00872 0.01361 -0.00829 O21 5 0.024490 0.347709 -0.270080 11.00000 0.03740 0.02896 = 0.04956 -0.01089 0.00896 -0.00888 O19 5 -0.081672 0.301449 -0.277962 11.00000 0.02201 0.03071 = 0.03638 -0.01521 -0.00021 -0.00131 O24 5 0.098889 0.383385 -0.273071 11.00000 0.03010 0.03080 = 0.04833 0.00741 -0.00930 -0.00621 O7 5 -0.149195 0.253230 0.049110 11.00000 0.03965 0.04257 = 0.02953 0.00807 0.00259 0.00294 O10 5 -0.280147 0.235919 -0.068696 11.00000 0.04314 0.05338 = 0.04782 -0.01357 -0.00266 0.02417 O16 5 0.232407 0.042970 -0.145292 11.00000 0.01988 0.04761 = 0.06377 -0.02586 0.00436 0.00738 O13 5 0.087211 0.216672 -0.149552 11.00000 0.05554 0.04471 = 0.05872 -0.00385 0.00094 0.03170 O2 5 -0.063784 0.158083 -0.060616 11.00000 0.04939 0.04686 = 0.02770 -0.00359 0.00677 -0.00568 O8 5 -0.124684 0.233530 -0.008118 11.00000 0.04638 0.06287 = 0.03517 0.00546 0.00417 -0.00062 O3 5 -0.157153 0.093743 -0.065147 11.00000 0.05721 0.02945 = 0.03589 -0.00934 0.00794 0.01485 O12 5 -0.148821 0.219386 -0.089517 11.00000 0.04029 0.06206 = 0.02426 -0.00541 0.00350 0.01854 O18 5 -0.057222 0.305539 -0.200993 11.00000 0.04583 0.03416 = 0.04542 -0.00050 -0.00004 0.01460 O15 5 0.241392 0.122639 -0.132078 11.00000 0.02851 0.04096 = 0.05344 -0.00485 0.00512 -0.00967 O11 5 -0.201591 0.279627 -0.111320 11.00000 0.07689 0.06341 = 0.02516 -0.00889 0.00130 0.03559 O22 5 0.001065 0.407511 -0.212880 11.00000 0.04095 0.03880 = 0.06302 -0.00905 -0.00137 -0.00657 O5 5 -0.147326 0.134248 0.007585 11.00000 0.05692 0.04563 = 0.01243 0.00025 -0.01564 0.00421 O14 5 0.171769 0.209971 -0.137175 11.00000 0.03783 0.04936 = 0.03944 -0.00545 -0.00424 -0.01302 O9 5 -0.223865 0.184741 -0.045142 11.00000 0.05139 0.03559 = 0.03520 0.00942 -0.00278 0.00806 N3 4 0.002768 0.183626 -0.218418 11.00000 0.02569 0.03535 = 0.04106 0.00168 -0.00565 -0.00808 N1 4 -0.116872 0.073572 -0.155970 11.00000 0.02545 0.02741 = 0.03798 0.00287 -0.00379 0.00029 N2 4 -0.051526 0.123528 -0.153539 11.00000 0.03744 0.04139 = 0.02267 -0.00976 0.00574 0.00042 N6 4 0.131807 0.050938 -0.157287 11.00000 0.02706 0.04080 = 0.01980 -0.00288 0.00949 0.00176 N5 4 0.076920 0.117333 -0.159710 11.00000 0.04565 0.03968 = 0.03303 0.00489 0.00083 0.00486 N4 4 -0.012325 0.184792 -0.278533 11.00000 0.04482 0.03720 = 0.04207 -0.00688 0.00258 0.00439 C12 1 -0.029958 0.228868 -0.264321 11.00000 0.03151 0.03768 = 0.02151 -0.00453 -0.00113 0.01830 C18 1 0.125974 0.134218 -0.151208 11.00000 0.02951 0.02805 = 0.01902 -0.00059 -0.00219 0.01036 C20 1 0.156715 0.092832 -0.148581 11.00000 0.03192 0.03222 = 0.02910 -0.00956 0.01736 0.00058 C11 1 -0.022705 0.228489 -0.226634 11.00000 0.00559 0.03593 = 0.02234 0.01626 0.00063 0.00477 C21 1 0.213695 0.087893 -0.140020 11.00000 0.03514 0.02850 = 0.02914 -0.00222 -0.00583 -0.00259 C3 1 -0.115128 0.093205 -0.121345 11.00000 0.01518 0.01644 = 0.03390 -0.00097 0.00628 0.01213 C10 1 -0.033474 0.264241 -0.194286 11.00000 0.01207 0.02847 = 0.03579 -0.00177 -0.01392 0.00306 C13 1 0.008591 0.162212 -0.248605 11.00000 0.03319 0.03821 = 0.05311 0.00028 0.00869 0.01604 AFIX 43 H13 2 0.026955 0.131299 -0.250559 11.00000 -1.20000 AFIX 0 C4 1 -0.154986 0.075509 -0.094587 11.00000 0.02719 0.03061 = 0.02374 -0.00426 -0.00895 0.00662 C15 1 0.053750 0.378873 -0.259795 11.00000 0.04849 0.01686 = 0.04810 -0.00205 -0.01785 -0.00815 C19 1 0.082289 0.067593 -0.162762 11.00000 0.03565 0.05151 = 0.02122 -0.00157 0.00626 -0.00553 AFIX 43 H19 2 0.054945 0.045366 -0.168176 11.00000 -1.20000 AFIX 0 C8 1 -0.236496 0.221460 -0.063460 11.00000 0.04104 0.02640 = 0.04233 0.01421 -0.00384 0.01887 C16 1 0.044964 0.408283 -0.226925 11.00000 0.02850 0.04434 = 0.03135 0.00980 -0.01402 -0.00029 C5 1 -0.082929 0.096761 -0.172760 11.00000 0.05765 0.03810 = 0.02189 0.01003 0.00366 -0.00200 AFIX 43 H5 2 -0.080214 0.094943 -0.198123 11.00000 -1.20000 AFIX 0 C14 1 -0.062750 0.260433 -0.288678 11.00000 0.02676 0.02361 = 0.02007 0.01249 -0.00231 0.00264 C2 1 -0.068749 0.124627 -0.120352 11.00000 0.01802 0.02545 = 0.02392 0.01586 0.00042 0.00375 C6 1 -0.142495 0.222378 0.024393 11.00000 0.01773 0.04086 = 0.00368 0.00242 0.00089 0.01196 C17 1 0.135331 0.190865 -0.146605 11.00000 0.04654 0.03476 = 0.02580 -0.01757 0.01278 -0.00482 C1 1 -0.041265 0.154788 -0.092730 11.00000 0.04639 0.02760 = 0.03190 0.00373 0.01318 -0.00583 C7 1 -0.153560 0.166641 0.032524 11.00000 0.03538 0.03421 = 0.00805 -0.00471 -0.01084 0.01542 C9 1 -0.198752 0.242879 -0.089245 11.00000 0.05204 0.05984 = 0.01653 -0.00505 -0.00237 0.01917 HKLF 4 1 -1 0 0 0 -1 0 0 0 1 REM 1 in I-4c2 REM R1 = 0.0926 for 9401 Fo > 4sig(Fo) and 0.1094 for all 11061 data REM 506 parameters refined using 430 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 1.000, deepest hole -1.183, 1-sigma level 0.159 Q1 1 -0.1158 0.1822 -0.0692 11.00000 0.05 1.00 Q2 1 -0.0585 0.3647 -0.2158 11.00000 0.05 0.89 Q3 1 -0.0218 0.1875 -0.3078 11.00000 0.05 0.85 Q4 1 -0.0449 0.3592 -0.2755 11.00000 0.05 0.82 Q5 1 0.1756 0.1792 -0.0891 11.00000 0.05 0.82 ; _shelx_res_checksum 49490 _shelx_fab_file ; 1 1 0 -1101.34 2.34 2 2 0 84.17 -5.39 3 3 0 6.10 19.44 4 4 0 104.05 -5.78 5 5 0 80.35 2.86 6 6 0 365.06 -0.75 7 7 0 -179.09 -0.21 8 8 0 202.67 -1.13 9 9 0 -101.25 1.79 10 10 0 51.64 -1.32 11 11 0 -87.59 1.13 12 12 0 -42.26 1.33 13 13 0 -10.97 1.11 14 14 0 95.87 4.63 15 15 0 -25.72 -2.33 16 16 0 48.83 -8.09 17 17 0 30.56 18.59 18 18 0 -2.03 -0.65 19 19 0 23.88 -6.39 20 20 0 72.80 -0.16 21 21 0 -71.92 -3.85 22 22 0 10.12 2.01 1 2 1 214.88 14.55 2 3 1 177.09 -28.24 3 4 1 -13.23 -47.63 4 5 1 -71.34 -36.22 5 6 1 -77.59 20.17 6 7 1 -70.33 31.93 7 8 1 9.25 -4.55 8 9 1 157.75 65.15 9 10 1 -19.59 14.74 10 11 1 -38.03 -12.61 11 12 1 -49.77 19.97 12 13 1 37.54 14.00 13 14 1 5.90 10.35 14 15 1 -2.27 -18.58 15 16 1 -1.52 42.67 16 17 1 -19.47 -17.01 17 18 1 -16.50 5.83 18 19 1 7.97 12.03 19 20 1 -6.41 0.72 20 21 1 -4.64 22.26 21 22 1 -6.97 2.42 1 1 2 -163.35 10.79 0 2 2 1140.59 -203.59 1 3 2 207.97 21.00 2 4 2 -9.92 -57.52 3 5 2 -38.90 -9.49 4 6 2 54.80 -53.99 5 7 2 -110.95 -1.47 6 8 2 133.02 65.59 7 9 2 -49.95 -88.88 8 10 2 97.73 1.68 9 11 2 48.63 -1.65 10 12 2 -29.92 31.70 11 13 2 -83.24 -15.21 12 14 2 3.74 -13.55 13 15 2 6.92 20.20 14 16 2 57.25 18.31 15 17 2 -15.25 -8.11 16 18 2 -33.00 -9.90 17 19 2 16.58 36.00 18 20 2 20.65 -23.09 19 21 2 -22.82 19.96 20 22 2 -11.51 15.75 21 23 2 -13.22 27.24 1 2 3 21.28 11.30 1 4 3 92.20 19.12 2 5 3 4.99 12.28 3 6 3 22.87 43.57 4 7 3 61.94 39.32 5 8 3 -16.56 -24.66 6 9 3 8.25 12.91 7 10 3 89.66 -29.28 8 11 3 66.01 -1.85 9 12 3 -70.10 30.49 10 13 3 -68.83 18.98 11 14 3 14.13 -5.76 12 15 3 37.25 25.20 13 16 3 -5.51 38.57 14 17 3 -8.41 3.78 15 18 3 -14.71 -6.53 16 19 3 -29.46 12.77 17 20 3 6.03 33.59 18 21 3 -0.50 13.50 19 22 3 10.26 -2.66 20 23 3 15.37 22.15 2 2 4 -17.29 -8.94 1 3 4 -287.21 -55.48 0 4 4 186.72 -51.01 1 5 4 73.02 -103.90 2 6 4 -94.82 46.86 3 7 4 -176.93 -40.28 4 8 4 -57.26 47.72 5 9 4 -116.88 24.88 6 10 4 68.05 -17.33 7 11 4 76.58 -77.43 8 12 4 -23.61 24.96 9 13 4 -8.08 7.07 10 14 4 -42.31 3.08 11 15 4 -47.45 -34.49 12 16 4 7.77 2.03 13 17 4 -19.20 -29.43 14 18 4 24.07 34.06 15 19 4 20.98 29.23 16 20 4 -7.77 -15.24 17 21 4 -5.84 9.63 18 22 4 -1.14 38.91 19 23 4 18.15 8.23 2 3 5 -69.74 -14.47 1 4 5 134.90 -45.20 1 6 5 50.39 54.91 2 7 5 120.40 -9.08 3 8 5 18.89 -81.93 4 9 5 37.40 -99.40 5 10 5 -14.46 104.40 6 11 5 32.87 -46.10 7 12 5 32.02 -52.02 8 13 5 26.54 27.33 9 14 5 34.64 32.17 10 15 5 -11.16 -4.45 11 16 5 -34.48 11.58 12 17 5 -51.45 -6.02 13 18 5 2.98 39.15 14 19 5 -3.00 8.04 15 20 5 16.57 -3.27 16 21 5 -23.29 2.30 17 22 5 -9.80 1.64 18 23 5 13.47 10.86 19 24 5 1.17 4.62 3 3 6 -198.55 11.84 2 4 6 -209.96 71.33 1 5 6 44.35 -8.84 0 6 6 263.69 161.64 1 7 6 -185.36 -56.42 2 8 6 -122.78 69.40 3 9 6 65.02 -84.87 4 10 6 -134.68 -34.00 5 11 6 13.72 -15.04 6 12 6 -6.33 12.61 7 13 6 -82.70 -17.72 8 14 6 82.05 0.46 9 15 6 -38.37 -14.67 10 16 6 -9.70 -16.29 11 17 6 -21.95 -35.49 12 18 6 -21.82 -28.20 13 19 6 -12.71 7.05 14 20 6 63.57 34.96 15 21 6 9.93 23.58 16 22 6 -3.72 -1.64 17 23 6 -12.81 6.98 18 24 6 7.69 2.33 3 4 7 103.47 -4.49 2 5 7 -51.00 12.30 1 6 7 80.68 34.41 1 8 7 32.93 23.84 2 9 7 34.15 -58.76 3 10 7 -1.20 -17.99 4 11 7 -18.06 -25.87 5 12 7 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13 22 9 -10.20 9.16 14 23 9 -10.66 -17.86 15 24 9 15.31 14.13 16 25 9 4.46 -11.84 5 5 10 136.56 5.62 4 6 10 -89.95 143.61 3 7 10 -18.80 -6.60 2 8 10 -20.67 -1.88 1 9 10 -41.42 50.86 0 10 10 128.08 5.10 1 11 10 -33.98 -44.79 2 12 10 -66.62 -29.63 3 13 10 59.02 32.05 4 14 10 -0.63 -83.44 5 15 10 43.89 2.28 6 16 10 -5.65 11.75 7 17 10 -31.27 -9.19 8 18 10 50.49 -26.48 9 19 10 36.80 23.34 10 20 10 10.80 -13.32 11 21 10 5.20 -10.08 12 22 10 -24.41 23.16 13 23 10 -11.32 -27.85 14 24 10 26.96 59.95 15 25 10 4.93 -29.09 5 6 11 -9.06 1.72 4 7 11 -52.94 -27.14 3 8 11 37.01 8.74 2 9 11 -15.58 27.11 1 10 11 38.65 23.51 1 12 11 36.67 20.19 2 13 11 57.66 -8.97 3 14 11 5.31 -25.75 4 15 11 29.28 34.79 5 16 11 -24.35 1.37 6 17 11 39.86 -13.95 7 18 11 22.95 -14.26 8 19 11 15.50 11.83 9 20 11 7.68 -17.38 10 21 11 -0.96 -8.25 11 22 11 6.88 -10.24 12 23 11 11.48 -14.44 13 24 11 14.67 26.79 14 25 11 8.41 -18.85 6 6 12 69.82 -0.87 5 7 12 100.40 42.10 4 8 12 -9.28 82.14 3 9 12 4.09 -40.69 2 10 12 -37.90 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12.72 23.17 7 21 14 15.69 41.76 8 22 14 33.16 10.71 9 23 14 -37.44 -39.63 10 24 14 2.04 -5.77 11 25 14 13.50 -14.57 12 26 14 -14.60 37.74 7 8 15 -14.78 -92.39 6 9 15 -8.53 58.48 5 10 15 -46.29 4.95 4 11 15 -50.45 -18.03 3 12 15 26.97 9.44 2 13 15 -4.68 -47.71 1 14 15 -0.86 -10.46 1 16 15 25.57 39.92 2 17 15 19.89 -28.36 3 18 15 3.44 -4.58 4 19 15 -28.73 2.22 5 20 15 3.82 -53.45 6 21 15 6.50 -11.20 7 22 15 0.61 4.48 8 23 15 -22.28 -44.95 9 24 15 -3.77 -7.02 10 25 15 -9.84 -20.83 11 26 15 7.96 10.00 8 8 16 -13.20 -2.43 7 9 16 27.15 -1.79 6 10 16 21.29 -13.97 5 11 16 19.04 9.77 4 12 16 64.63 -9.25 3 13 16 -47.33 38.59 2 14 16 49.59 39.74 1 15 16 -39.22 -38.26 0 16 16 31.33 78.55 1 17 16 -45.12 24.01 2 18 16 -8.01 49.02 3 19 16 -6.44 -42.08 4 20 16 -14.32 37.69 5 21 16 -16.42 7.01 6 22 16 2.48 -28.21 7 23 16 -14.84 -5.73 8 24 16 -4.72 1.74 9 25 16 -43.20 3.63 10 26 16 -11.46 -16.17 8 9 17 -0.03 -17.79 7 10 17 28.64 -30.94 6 11 17 -53.42 34.12 5 12 17 44.93 9.45 4 13 17 -27.14 -22.75 3 14 17 -33.03 -1.85 2 15 17 10.30 14.21 1 16 17 -22.30 3.33 1 18 17 15.27 22.95 2 19 17 18.52 -18.85 3 20 17 -14.42 43.82 4 21 17 -27.24 31.64 5 22 17 -14.24 -34.17 6 23 17 -18.45 -16.10 7 24 17 0.48 5.57 8 25 17 13.56 -0.49 9 26 17 -6.81 -8.03 10 27 17 -14.98 11.31 9 9 18 47.87 -2.03 8 10 18 33.07 7.48 7 11 18 32.43 11.34 6 12 18 16.49 32.31 5 13 18 20.55 -26.53 4 14 18 33.10 42.91 3 15 18 20.99 -35.87 2 16 18 -1.09 17.19 1 17 18 -11.42 38.29 0 18 18 -26.25 -40.68 1 19 18 -8.63 -0.46 2 20 18 -7.77 -28.46 3 21 18 -17.86 -17.59 4 22 18 -31.80 -0.93 5 23 18 -17.29 -46.51 6 24 18 -24.74 -4.42 7 25 18 -15.01 -4.59 8 26 18 -6.60 -17.86 9 27 18 -16.81 -7.04 9 10 19 3.77 16.59 8 11 19 -10.35 -1.93 7 12 19 27.08 -30.88 6 13 19 -11.08 40.59 5 14 19 -21.81 8.34 4 15 19 -45.77 12.74 3 16 19 67.71 -5.59 2 17 19 8.21 -9.87 1 18 19 -32.44 -2.56 1 20 19 -4.51 -5.91 2 21 19 -18.13 53.00 3 22 19 1.79 8.41 4 23 19 3.91 -12.85 5 24 19 -35.57 19.72 6 25 19 16.66 -8.71 7 26 19 11.00 -4.53 8 27 19 15.33 12.93 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26 6.03 -22.71 2 24 26 -29.50 30.19 13 14 27 -6.10 11.16 12 15 27 -18.37 40.81 11 16 27 -15.97 15.66 10 17 27 23.58 12.69 9 18 27 -3.62 14.06 8 19 27 12.86 32.50 7 20 27 -10.59 -19.20 6 21 27 -0.95 4.81 5 22 27 18.97 20.60 4 23 27 21.02 -12.73 3 24 27 27.25 -22.30 14 14 28 10.35 2.45 13 15 28 11.36 9.71 12 16 28 38.08 1.56 11 17 28 -0.08 8.74 10 18 28 45.42 -18.13 9 19 28 -2.53 7.01 8 20 28 -0.52 21.71 7 21 28 -8.37 45.06 6 22 28 11.37 -16.66 5 23 28 15.38 7.46 14 15 29 -10.14 -12.10 13 16 29 -21.64 10.70 12 17 29 4.11 2.16 11 18 29 -27.58 -10.60 10 19 29 24.30 -9.15 9 20 29 -22.21 19.45 8 21 29 14.97 -12.67 7 22 29 -12.61 24.13 15 15 30 63.86 -4.60 14 16 30 -7.17 14.20 13 17 30 9.94 -16.64 12 18 30 6.15 40.00 11 19 30 14.70 21.45 10 20 30 12.21 -21.74 15 16 31 -22.40 0.55 22 22 2 -4.80 -1.46 21 23 0 26.17 -0.71 20 22 0 8.75 -1.50 21 21 2 9.66 -1.00 20 20 2 -25.87 3.22 19 21 0 -5.88 1.54 18 20 0 8.01 1.62 19 19 2 10.46 -0.67 18 18 2 32.32 -1.97 17 19 0 21.28 -0.38 16 18 0 24.15 -2.55 17 17 2 8.28 -0.18 15 17 0 -22.19 4.07 16 16 2 -0.15 3.12 14 16 0 -6.64 0.01 15 15 2 -43.48 0.48 13 15 0 -34.51 8.23 14 14 2 -63.79 -6.55 12 14 0 -1.31 -5.69 13 13 2 -31.27 4.03 11 13 0 -2.69 -0.22 12 12 2 20.14 12.48 10 12 0 -98.23 2.07 11 11 2 -18.17 -4.00 9 11 0 26.05 -1.23 10 10 2 -99.13 -2.85 8 10 0 -47.48 -0.53 9 9 2 10.59 -3.98 7 9 0 75.27 -0.32 8 8 2 -100.62 -1.37 6 8 0 -65.28 0.10 6 6 2 -45.31 3.51 5 7 0 114.98 1.77 4 6 0 -189.85 1.23 5 5 2 130.61 -3.88 4 4 2 -4.23 -2.75 3 5 0 -48.14 2.58 2 4 0 275.26 -4.36 3 3 2 -241.89 6.43 1 3 0 677.97 -0.08 2 2 2 -694.61 15.24 0 2 0 180.26 4.40 0 0 2 1143.95 -11.94 21 22 3 27.38 -9.62 20 23 1 10.27 -5.38 19 22 1 13.92 -9.27 20 21 3 -17.15 -1.39 19 20 3 16.00 40.30 18 21 1 -23.34 -8.93 17 20 1 15.40 11.31 18 19 3 20.51 -13.39 16 19 1 -18.54 13.89 17 18 3 -0.75 23.49 16 17 3 3.42 3.53 15 18 1 -16.09 -12.54 14 17 1 7.68 4.35 15 16 3 -8.19 14.28 14 15 3 52.59 -24.75 13 16 1 7.48 22.39 13 14 3 -7.48 -9.31 12 15 1 51.74 -38.37 11 14 1 -39.29 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12 41 0.45 24.97 9 12 41 -10.22 2.34 11 12 41 0.89 -15.07 2 13 41 -13.18 -4.25 4 13 41 6.12 23.21 6 13 41 -17.15 3.09 8 13 41 0.28 -12.61 10 13 41 -20.48 3.20 12 13 41 -1.84 5.17 1 14 41 -13.52 -10.68 3 14 41 -5.64 -20.14 5 14 41 20.64 -0.84 7 14 41 -1.45 0.98 9 14 41 6.64 -5.09 11 14 41 2.44 5.04 2 15 41 27.41 -5.91 4 15 41 -3.61 12.29 6 15 41 6.83 -6.52 8 15 41 -23.31 -13.98 10 15 41 -13.20 11.64 1 16 41 -12.02 -2.49 3 16 41 2.83 1.82 5 16 41 -2.21 -13.87 7 16 41 0.21 5.32 9 16 41 15.06 5.48 2 17 41 -11.59 11.77 4 17 41 1.60 -10.72 6 17 41 4.76 0.57 1 18 41 8.49 -9.78 3 18 41 -0.10 -0.17 7 7 42 -4.80 -1.94 4 8 42 -1.01 -14.33 6 8 42 -19.02 14.98 8 8 42 4.62 0.70 1 9 42 -2.06 4.35 3 9 42 -24.61 19.38 5 9 42 3.06 -0.71 7 9 42 -0.69 2.79 9 9 42 -17.07 -3.19 0 10 42 -9.70 18.62 2 10 42 -7.21 2.31 4 10 42 -4.29 -2.89 6 10 42 -6.71 -16.91 8 10 42 1.26 6.99 10 10 42 1.45 4.70 1 11 42 0.93 -5.68 3 11 42 -5.70 8.10 5 11 42 2.64 0.26 7 11 42 -4.21 -25.22 9 11 42 -3.99 0.95 11 11 42 -9.68 -0.50 0 12 42 0.58 -22.47 2 12 42 -8.34 10.92 4 12 42 -13.21 4.00 6 12 42 -0.91 6.20 8 12 42 -8.95 4.65 10 12 42 -4.71 5.01 12 12 42 26.43 -3.57 1 13 42 0.52 7.45 3 13 42 -10.86 -22.80 5 13 42 2.30 23.32 7 13 42 1.63 -14.86 9 13 42 2.84 -15.59 11 13 42 -3.44 -9.25 0 14 42 -31.56 5.70 2 14 42 -0.21 16.58 4 14 42 -2.99 -6.89 6 14 42 -11.85 -14.82 8 14 42 -2.80 -0.31 10 14 42 -0.69 -7.66 1 15 42 -1.05 6.28 3 15 42 -12.11 23.43 5 15 42 -14.17 -2.90 7 15 42 -14.15 9.63 0 16 42 33.70 -8.79 2 16 42 5.23 -8.99 4 16 42 -4.82 -3.68 6 16 42 -0.76 4.63 1 17 42 -21.09 2.13 3 17 42 20.63 4.86 4 5 43 8.46 0.28 3 6 43 13.95 -8.76 5 6 43 4.17 -10.42 2 7 43 7.82 -0.56 4 7 43 3.40 15.52 6 7 43 17.36 10.94 1 8 43 4.57 7.02 3 8 43 -13.75 -1.79 5 8 43 -48.71 -2.24 7 8 43 2.54 3.66 2 9 43 0.39 6.72 4 9 43 28.61 21.85 6 9 43 28.54 10.23 8 9 43 -13.86 8.85 1 10 43 12.00 -0.38 3 10 43 -3.69 0.13 5 10 43 5.99 16.73 7 10 43 -8.23 1.64 9 10 43 -1.73 2.35 2 11 43 -23.44 -1.52 4 11 43 -24.35 18.65 6 11 43 -13.02 -4.08 8 11 43 20.76 6.15 10 11 43 -6.56 -10.37 1 12 43 5.95 8.09 3 12 43 -1.30 -7.47 5 12 43 27.78 9.00 7 12 43 -14.07 4.58 9 12 43 14.31 6.75 2 13 43 3.57 11.61 4 13 43 -4.26 17.43 6 13 43 -12.05 -2.71 8 13 43 -15.72 -12.04 1 14 43 6.43 -7.34 3 14 43 -4.69 10.40 5 14 43 -21.85 -14.96 7 14 43 14.10 6.49 2 15 43 -1.23 -2.84 4 15 43 12.38 -2.04 6 15 43 -11.13 13.04 1 16 43 -5.88 -0.91 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 21116) # 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 -0.002 -0.030 -0.002 14672 6730 ' ' 2 0.000 0.000 0.250 93 15 ' ' 3 0.000 0.000 0.750 93 15 ' ' 4 0.500 0.500 0.250 93 15 ' ' 5 0.500 0.500 0.750 93 15 ' ' # Missing Reflections Below sin(th)/lambda = 0.25 loop_ _platon_missing_refln_index_h _platon_missing_refln_index_k _platon_missing_refln_index_l _platon_missing_refln_theta 0 10 0 7.753 7 7 2 7.753 _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) TITL 1 in I-4c2 CELL 26.3430 26.3430 37.3010 90.00 90.00 90.00 SPGR I-4c2 # Solvent Accessible Volume = 15045 # Electrons Found in S.A.V. = 6762 # Note: Atoms in Void as Cxxx and Qxxx all others C101 0.850 0.409 0.350 ! 8.31 eA-3 C102 0.264 0.242 0.189 ! 7.55 eA-3 C103 0.267 0.574 0.485 ! 7.40 eA-3 C104 0.345 0.180 0.385 ! 6.79 eA-3 C105 0.852 0.650 0.342 ! 6.22 eA-3 C106 0.394 0.798 0.365 ! 5.60 eA-3 C107 0.227 0.929 0.062 ! 5.45 eA-3 Q108 0.991 0.364 0.351 ! 5.12 eA-3 C109 0.451 0.197 0.384 ! 4.76 eA-3 C110 0.892 0.250 0.232 ! 4.47 eA-3 Q111 0.153 0.230 0.149 ! 4.47 eA-3 Q112 0.087 0.699 0.290 ! 4.36 eA-3 C113 0.593 0.051 0.390 ! 4.33 eA-3 C114 0.984 0.212 0.484 ! 4.27 eA-3 C115 0.208 0.144 0.182 ! 4.23 eA-3 C116 0.089 0.685 0.312 ! 4.23 eA-3 C117 0.564 0.976 0.352 ! 4.23 eA-3 C118 0.338 0.966 0.353 ! 4.08 eA-3 Q119 0.453 0.528 0.405 ! 3.97 eA-3 C120 0.079 0.042 0.493 ! 3.95 eA-3 C121 0.189 0.312 0.217 ! 3.90 eA-3 C122 0.318 0.468 0.002 ! 3.84 eA-3 C123 0.262 0.772 0.189 ! 3.84 eA-3 C124 0.031 0.787 0.055 ! 3.77 eA-3 C125 0.069 0.932 0.072 ! 3.76 eA-3 C126 0.500 0.498 0.399 ! 3.76 eA-3 C127 0.158 0.862 0.241 ! 3.69 eA-3 C128 0.038 0.713 0.070 ! 3.68 eA-3 Q129 0.345 0.191 0.171 ! 3.67 eA-3 C130 0.951 0.306 0.078 ! 3.67 eA-3 C131 0.295 0.076 0.109 ! 3.63 eA-3 C132 0.189 0.288 0.278 ! 3.58 eA-3 C133 0.189 0.709 0.784 ! 3.54 eA-3 C134 0.500 1.001 0.336 ! 3.54 eA-3 C135 0.430 0.791 0.090 ! 3.53 eA-3 C136 0.268 0.045 0.055 ! 3.48 eA-3 C137 0.282 0.857 0.009 ! 3.47 eA-3 C138 0.547 0.767 0.947 ! 3.47 eA-3 Q139 0.119 0.670 0.162 ! 3.41 eA-3 C140 0.183 0.305 0.250 ! 3.34 eA-3 C141 0.563 0.054 0.365 ! 3.33 eA-3 C142 0.015 0.046 0.027 ! 3.32 eA-3 Q143 0.788 0.103 0.006 ! 3.29 eA-3 C144 0.750 0.614 0.235 ! 3.25 eA-3 Q145 0.563 0.329 0.939 ! 3.20 eA-3 Q146 0.063 0.829 0.439 ! 3.20 eA-3 C147 0.259 0.466 0.429 ! 3.14 eA-3 C148 0.773 0.485 0.010 ! 3.12 eA-3 Q149 0.076 0.271 0.078 ! 3.11 eA-3 C150 0.484 0.856 0.382 ! 3.11 eA-3 C151 0.885 0.323 0.375 ! 3.08 eA-3 C152 0.944 0.068 0.462 ! 3.08 eA-3 C153 0.600 0.563 0.433 ! 3.05 eA-3 C154 0.906 0.341 0.398 ! 3.02 eA-3 C155 0.555 0.928 0.439 ! 3.01 eA-3 C156 0.658 0.882 0.146 ! 3.01 eA-3 Q157 0.834 0.337 0.022 ! 2.99 eA-3 C158 0.935 0.556 0.447 ! 2.98 eA-3 C159 0.532 0.208 0.092 ! 2.97 eA-3 C160 0.038 0.277 0.921 ! 2.94 eA-3 C161 0.538 0.777 0.421 ! 2.94 eA-3 C162 0.295 0.472 0.460 ! 2.94 eA-3 Q163 0.532 0.821 0.354 ! 2.93 eA-3 Q164 0.141 0.328 0.468 ! 2.92 eA-3 C165 0.486 0.145 0.383 ! 2.91 eA-3 C166 0.334 0.090 0.022 ! 2.90 eA-3 C167 0.875 0.313 0.454 ! 2.90 eA-3 C168 0.196 0.827 0.226 ! 2.88 eA-3 C169 0.937 0.464 0.403 ! 2.87 eA-3 C170 0.119 0.648 0.432 ! 2.87 eA-3 C171 0.583 0.785 0.421 ! 2.85 eA-3 C172 0.858 0.511 0.485 ! 2.83 eA-3 Q173 0.304 0.997 0.123 ! 2.80 eA-3 Q174 0.723 0.507 0.431 ! 2.75 eA-3 C175 0.092 0.401 0.014 ! 2.74 eA-3 Q176 0.213 0.702 0.179 ! 2.74 eA-3 Q177 0.339 0.835 0.094 ! 2.73 eA-3 C178 0.968 0.578 0.375 ! 2.73 eA-3 C179 0.169 0.946 0.430 ! 2.71 eA-3 C180 0.189 0.548 0.383 ! 2.70 eA-3 Q181 0.946 0.245 0.226 ! 2.70 eA-3 Q182 0.578 0.183 0.569 ! 2.70 eA-3 Q183 0.078 0.683 0.069 ! 2.70 eA-3 C184 0.390 0.842 0.058 ! 2.70 eA-3 C185 0.765 0.641 0.221 ! 2.70 eA-3 C186 0.337 0.689 0.288 ! 2.69 eA-3 Q187 0.087 0.682 0.181 ! 2.69 eA-3 C188 0.784 0.577 0.009 ! 2.67 eA-3 C189 0.320 0.684 0.344 ! 2.66 eA-3 Q190 0.726 0.213 0.670 ! 2.66 eA-3 Q191 0.501 0.848 0.161 ! 2.65 eA-3 Q192 0.586 0.110 0.155 ! 2.64 eA-3 C193 0.977 0.716 0.016 ! 2.64 eA-3 C194 0.108 0.300 0.065 ! 2.63 eA-3 Q195 0.987 0.052 0.116 ! 2.63 eA-3 C196 0.500 0.999 0.461 ! 2.61 eA-3 C197 0.454 0.863 0.407 ! 2.60 eA-3 C198 0.015 0.551 0.439 ! 2.60 eA-3 C199 0.155 0.157 0.249 ! 2.60 eA-3 ) ; _shelx_fab_checksum 14858 _olex2_submission_special_instructions 'No special instructions were received' _platon_squeeze_void_probe_radius 1.20 _platon_1_sq_details ; Disordered volatile and ionic guests per formula unit were removed by SQUEEZE. The values were calculated based on elemental analysis and TGA data. Guest = 5K+,7CH3CN and 8H2O ; loop_ _space_group_symop_operation_xyz 'x, y, z' 'y, -x, -z' '-x, -y, z' '-y, x, -z' '-x, y, z+1/2' 'y, x, -z+1/2' 'x, -y, z+1/2' '-y, -x, -z+1/2' 'x+1/2, y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1/2, y+1/2, z+1' 'y+1/2, x+1/2, -z+1' 'x+1/2, -y+1/2, z+1' '-y+1/2, -x+1/2, -z+1' 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 Mn1 Mn 0.01695(8) 0.17384(8) -0.16046(6) 0.0368(5) Uani 1 1 d . . Mn3 Mn -0.05058(9) 0.35741(9) -0.24464(7) 0.0388(5) Uani 1 1 d . . Mn4 Mn -0.01704(8) 0.17655(9) -0.33652(6) 0.0362(5) Uani 1 1 d . . Mn2 Mn -0.13790(9) 0.16841(8) -0.04510(5) 0.0349(5) Uani 1 1 d . . Mn5 Mn 0.22135(8) 0.18628(8) -0.09744(5) 0.0325(5) Uani 1 1 d . . O20 O -0.0640(3) 0.2427(3) -0.3213(2) 0.0244(17) Uani 1 1 d . U O6 O -0.1650(5) 0.1566(4) 0.0648(2) 0.043(2) Uani 1 1 d . U O23 O 0.0776(4) 0.4408(4) -0.2166(2) 0.034(2) Uani 1 1 d . U O17 O -0.0246(4) 0.2490(4) -0.1642(3) 0.041(2) Uani 1 1 d . U O4 O -0.1839(4) 0.0439(4) -0.1060(3) 0.040(2) Uani 1 1 d . U O1 O -0.0027(4) 0.1793(4) -0.1034(3) 0.040(2) Uani 1 1 d . U O21 O 0.0245(4) 0.3477(4) -0.2701(3) 0.039(2) Uani 1 1 d . U O19 O -0.0817(3) 0.3014(4) -0.2780(2) 0.030(2) Uani 1 1 d . U O24 O 0.0989(3) 0.3834(4) -0.2731(3) 0.036(2) Uani 1 1 d . U O7 O -0.1492(4) 0.2532(4) 0.0491(2) 0.037(2) Uani 1 1 d . U O10 O -0.2801(4) 0.2359(4) -0.0687(3) 0.048(3) Uani 1 1 d . U O16 O 0.2324(4) 0.0430(4) -0.1453(3) 0.044(3) Uani 1 1 d . U O13 O 0.0872(5) 0.2167(4) -0.1496(3) 0.053(3) Uani 1 1 d . U O2 O -0.0638(4) 0.1581(4) -0.0606(3) 0.041(2) Uani 1 1 d . U O8 O -0.1247(4) 0.2335(5) -0.0081(3) 0.048(3) Uani 1 1 d . U O3 O -0.1572(4) 0.0937(4) -0.0651(3) 0.041(2) Uani 1 1 d . U O12 O -0.1488(4) 0.2194(4) -0.0895(2) 0.042(2) Uani 1 1 d . U O18 O -0.0572(4) 0.3055(4) -0.2010(3) 0.042(2) Uani 1 1 d . U O15 O 0.2414(4) 0.1226(4) -0.1321(3) 0.041(2) Uani 1 1 d . U O11 O -0.2016(5) 0.2796(5) -0.1113(3) 0.055(3) Uani 1 1 d . U O22 O 0.0011(4) 0.4075(4) -0.2129(3) 0.048(2) Uani 1 1 d . U O5 O -0.1473(4) 0.1342(4) 0.0076(2) 0.038(2) Uani 1 1 d . U O14 O 0.1718(4) 0.2100(4) -0.1372(3) 0.042(2) Uani 1 1 d . U O9 O -0.2239(4) 0.1847(4) -0.0451(3) 0.041(2) Uani 1 1 d . U N3 N 0.0028(5) 0.1836(4) -0.2184(3) 0.034(2) Uani 1 1 d . U N1 N -0.1169(4) 0.0736(4) -0.1560(3) 0.030(2) Uani 1 1 d . U N2 N -0.0515(5) 0.1235(5) -0.1535(3) 0.034(2) Uani 1 1 d . U N6 N 0.1318(4) 0.0509(4) -0.1573(3) 0.029(2) Uani 1 1 d . U N5 N 0.0769(5) 0.1173(5) -0.1597(3) 0.039(2) Uani 1 1 d . U N4 N -0.0123(5) 0.1848(5) -0.2785(3) 0.041(3) Uani 1 1 d . U C12 C -0.0300(5) 0.2289(5) -0.2643(3) 0.030(3) Uani 1 1 d . U C18 C 0.1260(5) 0.1342(5) -0.1512(3) 0.026(2) Uani 1 1 d . U C20 C 0.1567(5) 0.0928(5) -0.1486(3) 0.031(3) Uani 1 1 d D U C11 C -0.0227(4) 0.2285(5) -0.2266(3) 0.021(2) Uani 1 1 d . U C21 C 0.2137(5) 0.0879(5) -0.1400(3) 0.031(3) Uani 1 1 d . U C3 C -0.1151(4) 0.0932(4) -0.1213(3) 0.022(2) Uani 1 1 d . U C10 C -0.0335(4) 0.2642(5) -0.1943(3) 0.025(2) Uani 1 1 d . U C13 C 0.0086(6) 0.1622(6) -0.2486(4) 0.042(3) Uani 1 1 d . U H13 H 0.0270 0.1313 -0.2506 0.050 Uiso 1 1 calc R . C4 C -0.1550(5) 0.0755(5) -0.0946(3) 0.027(2) Uani 1 1 d . U C15 C 0.0538(6) 0.3789(5) -0.2598(4) 0.038(3) Uani 1 1 d . U C19 C 0.0823(5) 0.0676(6) -0.1628(3) 0.036(3) Uani 1 1 d D U H19 H 0.0549 0.0454 -0.1682 0.043 Uiso 1 1 calc R . C8 C -0.2365(6) 0.2215(5) -0.0635(4) 0.037(3) Uani 1 1 d . U C16 C 0.0450(5) 0.4083(6) -0.2269(4) 0.035(3) Uani 1 1 d . U C5 C -0.0829(6) 0.0968(6) -0.1728(4) 0.039(3) Uani 1 1 d . U H5 H -0.0802 0.0949 -0.1981 0.047 Uiso 1 1 calc R . C14 C -0.0627(5) 0.2604(5) -0.2887(3) 0.023(2) Uani 1 1 d . U C2 C -0.0687(4) 0.1246(5) -0.1204(3) 0.022(2) Uani 1 1 d . U C6 C -0.1425(4) 0.2224(5) 0.0244(3) 0.021(2) Uani 1 1 d . U C17 C 0.1353(6) 0.1909(6) -0.1466(4) 0.036(3) Uani 1 1 d . U C1 C -0.0413(6) 0.1548(5) -0.0927(4) 0.035(3) Uani 1 1 d . U C7 C -0.1536(5) 0.1666(5) 0.0325(3) 0.026(2) Uani 1 1 d . U C9 C -0.1988(6) 0.2429(7) -0.0892(3) 0.043(3) Uani 1 1 d . 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 Mn1 0.0370(13) 0.0298(11) 0.0437(12) -0.0040(10) -0.0064(10) 0.0044(8) Mn3 0.0330(12) 0.0334(12) 0.0498(13) -0.0003(10) -0.0003(10) 0.0006(9) Mn4 0.0327(12) 0.0391(13) 0.0367(11) -0.0024(10) -0.0029(9) 0.0000(9) Mn2 0.0412(13) 0.0355(12) 0.0280(10) 0.0014(9) -0.0001(9) 0.0051(9) Mn5 0.0375(12) 0.0333(11) 0.0267(9) 0.0001(9) 0.0008(9) -0.0071(9) O20 0.025(4) 0.022(4) 0.026(4) 0.007(3) 0.006(3) -0.005(3) O6 0.068(6) 0.042(5) 0.018(4) 0.019(4) -0.002(4) 0.010(5) O23 0.039(5) 0.035(5) 0.030(5) -0.007(4) 0.003(4) -0.003(4) O17 0.046(6) 0.037(5) 0.041(5) -0.007(4) -0.012(5) 0.007(4) O4 0.052(6) 0.030(5) 0.037(5) 0.001(4) 0.000(5) -0.001(4) O1 0.041(5) 0.037(5) 0.042(5) -0.009(4) 0.014(4) -0.008(4) O21 0.037(5) 0.029(5) 0.050(6) -0.011(4) 0.009(4) -0.009(4) O19 0.022(4) 0.031(5) 0.036(5) -0.015(4) 0.000(4) -0.001(4) O24 0.030(5) 0.031(5) 0.048(5) 0.007(4) -0.009(4) -0.006(4) O7 0.040(5) 0.043(5) 0.030(4) 0.008(4) 0.003(4) 0.003(4) O10 0.043(6) 0.053(7) 0.048(6) -0.014(5) -0.003(5) 0.024(5) O16 0.020(5) 0.048(6) 0.064(7) -0.026(5) 0.004(4) 0.007(4) O13 0.056(6) 0.045(6) 0.059(7) -0.004(5) 0.001(6) 0.032(5) O2 0.049(6) 0.047(6) 0.028(4) -0.004(4) 0.007(4) -0.006(5) O8 0.046(6) 0.063(7) 0.035(5) 0.005(5) 0.004(5) -0.001(5) O3 0.057(6) 0.029(5) 0.036(5) -0.009(4) 0.008(5) 0.015(4) O12 0.040(5) 0.062(7) 0.024(5) -0.005(4) 0.003(4) 0.019(5) O18 0.046(6) 0.034(5) 0.045(6) 0.000(4) 0.000(5) 0.015(4) O15 0.029(5) 0.041(5) 0.053(6) -0.005(5) 0.005(5) -0.010(4) O11 0.077(8) 0.063(7) 0.025(5) -0.009(4) 0.001(5) 0.036(6) O22 0.041(6) 0.039(6) 0.063(7) -0.009(5) -0.001(5) -0.007(4) O5 0.057(6) 0.046(5) 0.012(4) 0.000(4) -0.016(4) 0.004(5) O14 0.038(5) 0.049(6) 0.039(5) -0.005(5) -0.004(5) -0.013(4) O9 0.051(6) 0.036(6) 0.035(5) 0.009(4) -0.003(5) 0.008(4) N3 0.026(6) 0.035(6) 0.041(5) 0.002(5) -0.006(5) -0.008(4) N1 0.025(5) 0.027(6) 0.038(5) 0.003(4) -0.004(4) 0.000(4) N2 0.037(6) 0.041(7) 0.023(5) -0.010(5) 0.006(4) 0.000(5) N6 0.027(5) 0.041(6) 0.020(5) -0.003(4) 0.009(4) 0.002(4) N5 0.046(6) 0.040(6) 0.033(6) 0.005(5) 0.001(5) 0.005(5) N4 0.045(7) 0.037(6) 0.042(5) -0.007(5) 0.003(5) 0.004(5) C12 0.032(6) 0.038(6) 0.022(5) -0.005(5) -0.001(5) 0.018(5) C18 0.030(6) 0.028(5) 0.019(5) -0.001(5) -0.002(5) 0.010(4) C20 0.032(5) 0.032(6) 0.029(6) -0.010(5) 0.017(5) 0.001(4) C11 0.006(5) 0.036(5) 0.022(4) 0.016(4) 0.001(4) 0.005(4) C21 0.035(6) 0.028(6) 0.029(6) -0.002(5) -0.006(5) -0.003(5) C3 0.015(5) 0.016(5) 0.034(5) -0.001(4) 0.006(4) 0.012(4) C10 0.012(5) 0.028(6) 0.036(6) -0.002(5) -0.014(5) 0.003(4) C13 0.033(7) 0.038(7) 0.053(7) 0.000(6) 0.009(6) 0.016(6) C4 0.027(6) 0.031(6) 0.024(5) -0.004(5) -0.009(5) 0.007(5) C15 0.048(7) 0.017(6) 0.048(7) -0.002(5) -0.018(6) -0.008(5) C19 0.036(6) 0.052(7) 0.021(6) -0.002(6) 0.006(6) -0.006(5) C8 0.041(6) 0.026(6) 0.042(7) 0.014(5) -0.004(6) 0.019(6) C16 0.029(6) 0.044(7) 0.031(6) 0.010(5) -0.014(5) 0.000(5) C5 0.058(9) 0.038(7) 0.022(5) 0.010(5) 0.004(5) -0.002(6) C14 0.027(6) 0.024(6) 0.020(5) 0.012(4) -0.002(5) 0.003(5) C2 0.018(5) 0.025(6) 0.024(5) 0.016(4) 0.000(4) 0.004(4) C6 0.018(5) 0.041(5) 0.004(4) 0.002(4) 0.001(4) 0.012(4) C17 0.047(7) 0.035(6) 0.026(6) -0.018(5) 0.013(6) -0.005(5) C1 0.046(7) 0.028(7) 0.032(6) 0.004(5) 0.013(5) -0.006(5) C7 0.035(6) 0.034(5) 0.008(4) -0.005(4) -0.011(4) 0.015(5) C9 0.052(7) 0.060(8) 0.017(5) -0.005(5) -0.002(5) 0.019(6) 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' Mn Mn 0.3368 0.7283 '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' 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 O1 Mn1 O17 83.6(4) . . O1 Mn1 O13 89.1(4) . . O1 Mn1 N3 154.4(4) . . O1 Mn1 N2 74.9(4) . . O13 Mn1 O17 88.3(4) . . O13 Mn1 N3 105.2(4) . . O13 Mn1 N2 162.1(4) . . N3 Mn1 O17 75.9(4) . . N3 Mn1 N2 92.6(4) . . N2 Mn1 O17 97.7(4) . . N5 Mn1 O17 162.0(5) . . N5 Mn1 O1 101.8(4) . . N5 Mn1 O13 74.8(4) . . N5 Mn1 N3 102.5(5) . . N5 Mn1 N2 100.2(5) . . O21 Mn3 O23 84.4(4) . 10_454 O21 Mn3 O22 75.6(4) . . O19 Mn3 O23 96.6(4) . 10_454 O19 Mn3 O21 90.8(4) . . O19 Mn3 O24 103.8(3) . 10_454 O19 Mn3 O18 88.3(4) . . O19 Mn3 O22 165.4(4) . . O24 Mn3 O23 73.3(4) 10_454 10_454 O24 Mn3 O21 154.5(4) 10_454 . O24 Mn3 O22 90.8(4) 10_454 . O18 Mn3 O23 165.6(4) . 10_454 O18 Mn3 O21 109.1(4) . . O18 Mn3 O24 92.4(4) . 10_454 O18 Mn3 O22 91.4(4) . . O22 Mn3 O23 87.3(4) . 10_454 O20 Mn4 O4 90.1(4) . 8_554 O20 Mn4 O16 87.5(3) . 6_554 O16 Mn4 O4 83.0(4) 6_554 8_554 N1 Mn4 O20 102.7(4) 8_554 . N1 Mn4 O4 74.2(4) 8_554 8_554 N1 Mn4 O16 154.9(4) 8_554 6_554 N6 Mn4 O20 157.3(4) 6_554 . N6 Mn4 O4 101.8(4) 6_554 8_554 N6 Mn4 O16 75.1(4) 6_554 6_554 N6 Mn4 N1 99.2(4) 6_554 8_554 N6 Mn4 N4 96.5(4) 6_554 . N4 Mn4 O20 72.4(4) . . N4 Mn4 O4 161.7(5) . 8_554 N4 Mn4 O16 101.1(5) . 6_554 N4 Mn4 N1 103.8(5) . 8_554 O2 Mn2 O8 97.3(4) . . O2 Mn2 O3 90.3(4) . . O2 Mn2 O12 89.6(4) . . O2 Mn2 O5 107.9(4) . . O2 Mn2 O9 163.4(4) . . O8 Mn2 O9 90.6(4) . . O3 Mn2 O8 161.8(4) . . O3 Mn2 O5 84.8(4) . . O3 Mn2 O9 86.5(4) . . O12 Mn2 O8 91.0(4) . . O12 Mn2 O3 105.7(4) . . O12 Mn2 O5 159.8(4) . . O12 Mn2 O9 75.6(4) . . O5 Mn2 O8 77.1(4) . . O5 Mn2 O9 88.0(4) . . O6 Mn5 O7 74.2(4) 2 2 O6 Mn5 O10 87.5(4) 2 15_554 O6 Mn5 O15 108.9(4) 2 . O6 Mn5 O11 158.4(4) 2 15_554 O7 Mn5 O10 91.1(4) 2 15_554 O7 Mn5 O11 91.2(4) 2 15_554 O15 Mn5 O7 92.9(4) . 2 O15 Mn5 O10 163.6(4) . 15_554 O15 Mn5 O11 87.3(4) . 15_554 O11 Mn5 O10 76.8(4) 15_554 15_554 O14 Mn5 O6 89.1(4) . 2 O14 Mn5 O7 162.5(4) . 2 O14 Mn5 O10 93.1(4) . 15_554 O14 Mn5 O15 87.7(4) . . O14 Mn5 O11 106.3(4) . 15_554 C14 O20 Mn4 120.6(7) . . C7 O6 Mn5 115.4(8) . 4 C16 O23 Mn3 112.8(9) . 12_554 C10 O17 Mn1 116.0(9) . . C4 O4 Mn4 119.7(9) . 8_554 C1 O1 Mn1 117.3(9) . . C15 O21 Mn3 111.2(10) . . C14 O19 Mn3 129.7(8) . . C15 O24 Mn3 116.2(9) . 12_554 C6 O7 Mn5 114.8(8) . 4 C8 O10 Mn5 109.4(10) . 15_454 C21 O16 Mn4 115.8(8) . 6_554 C17 O13 Mn1 120.7(9) . . C1 O2 Mn2 132.9(10) . . C6 O8 Mn2 109.8(9) . . C4 O3 Mn2 132.0(10) . . C9 O12 Mn2 112.4(8) . . C10 O18 Mn3 130.8(9) . . C21 O15 Mn5 125.6(9) . . C9 O11 Mn5 101.8(10) . 15_454 C16 O22 Mn3 110.2(9) . . C7 O5 Mn2 113.4(8) . . C17 O14 Mn5 128.2(11) . . C8 O9 Mn2 114.4(10) . . C11 N3 Mn1 113.3(9) . . C13 N3 Mn1 142.8(11) . . C13 N3 C11 103.9(12) . . C3 N1 Mn4 113.3(8) . 8_554 C5 N1 Mn4 141.6(10) . 8_554 C5 N1 C3 105.0(11) . . C5 N2 Mn1 139.8(9) . . C5 N2 C2 108.1(12) . . C2 N2 Mn1 111.7(9) . . C20 N6 Mn4 116.6(9) . 6_554 C20 N6 C19 103.8(11) . . C19 N6 Mn4 139.3(10) . 6_554 C18 N5 Mn1 117.1(9) . . C19 N5 Mn1 139.1(11) . . C19 N5 C18 103.6(12) . . C12 N4 Mn4 117.0(10) . . C12 N4 C13 100.9(12) . . C13 N4 Mn4 141.6(10) . . N4 C12 C11 109.6(12) . . N4 C12 C14 115.7(11) . . C11 C12 C14 132.8(11) . . N5 C18 C17 119.0(12) . . C20 C18 N5 108.1(12) . . C20 C18 C17 132.9(13) . . N6 C20 C18 110.8(12) . . N6 C20 C21 117.6(12) . . C18 C20 C21 131.5(12) . . N3 C11 C12 106.8(11) . . N3 C11 C10 115.5(10) . . C12 C11 C10 137.7(11) . . O16 C21 C20 114.6(11) . . O15 C21 O16 119.9(13) . . O15 C21 C20 125.2(13) . . N1 C3 C4 118.2(11) . . N1 C3 C2 105.0(10) . . C2 C3 C4 136.6(11) . . O17 C10 O18 123.8(13) . . O17 C10 C11 118.7(11) . . O18 C10 C11 116.9(11) . . N3 C13 N4 118.6(13) . . N3 C13 H13 120.7 . . N4 C13 H13 120.7 . . O4 C4 C3 114.6(11) . . O3 C4 O4 124.7(14) . . O3 C4 C3 120.7(12) . . O21 C15 O24 122.4(14) . . O21 C15 C16 122.1(15) . . O24 C15 C16 114.6(12) . . N6 C19 H19 123.2 . . N5 C19 N6 113.6(12) . . N5 C19 H19 123.2 . . O10 C8 O9 125.9(15) . . O10 C8 C9 113.8(12) . . O9 C8 C9 118.3(13) . . O23 C16 C15 120.0(13) . . O22 C16 O23 120.1(14) . . O22 C16 C15 118.7(13) . . N1 C5 N2 116.3(12) . . N1 C5 H5 121.9 . . N2 C5 H5 121.9 . . O20 C14 C12 112.3(11) . . O19 C14 O20 126.6(11) . . O19 C14 C12 120.8(11) . . N2 C2 C3 104.4(11) . . N2 C2 C1 119.6(11) . . C3 C2 C1 136.0(11) . . O7 C6 O8 125.5(13) . . O7 C6 C7 117.0(10) . . O8 C6 C7 117.4(11) . . O13 C17 C18 108.1(12) . . O14 C17 O13 123.8(14) . . O14 C17 C18 127.2(15) . . O1 C1 O2 127.0(13) . . O1 C1 C2 116.4(11) . . O2 C1 C2 116.0(12) . . O6 C7 O5 125.7(13) . . O6 C7 C6 115.8(11) . . O5 C7 C6 118.3(10) . . O12 C9 C8 116.5(12) . . O11 C9 O12 111.9(14) . . O11 C9 C8 131.6(14) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Mn1 O17 2.267(10) . Mn1 O1 2.196(10) . Mn1 O13 2.206(14) . Mn1 N3 2.209(12) . Mn1 N2 2.253(12) . Mn1 N5 2.171(13) . Mn3 O23 2.252(10) 10_454 Mn3 O21 2.208(10) . Mn3 O19 2.095(9) . Mn3 O24 2.188(9) 10_454 Mn3 O18 2.133(11) . Mn3 O22 2.235(11) . Mn4 O20 2.211(9) . Mn4 O4 2.266(10) 8_554 Mn4 O16 2.264(10) 6_554 Mn4 N1 2.184(11) 8_554 Mn4 N6 2.156(11) 6_554 Mn4 N4 2.177(13) . Mn2 O2 2.054(11) . Mn2 O8 2.229(12) . Mn2 O3 2.165(10) . Mn2 O12 2.152(11) . Mn2 O5 2.176(9) . Mn2 O9 2.305(11) . Mn5 O6 2.171(11) 2 Mn5 O7 2.216(10) 2 Mn5 O10 2.313(12) 15_554 Mn5 O15 2.181(11) . Mn5 O11 2.279(11) 15_554 Mn5 O14 2.072(11) . O20 C14 1.303(15) . O6 Mn5 2.171(11) 4 O6 C7 1.268(16) . O23 Mn3 2.252(10) 12_554 O23 C16 1.272(17) . O17 C10 1.214(16) . O4 Mn4 2.266(10) 8_554 O4 C4 1.207(17) . O1 C1 1.268(18) . O21 C15 1.190(17) . O19 C14 1.255(16) . O24 Mn3 2.188(9) 12_554 O24 C15 1.294(19) . O7 Mn5 2.216(10) 4 O7 C6 1.242(15) . O10 Mn5 2.314(12) 15_454 O10 C8 1.227(18) . O16 Mn4 2.264(10) 6_554 O16 C21 1.297(17) . O13 C17 1.443(19) . O2 C1 1.340(17) . O8 C6 1.333(15) . O3 C4 1.200(16) . O12 C9 1.454(18) . O18 C10 1.280(16) . O15 C21 1.207(17) . O11 Mn5 2.279(11) 15_454 O11 C9 1.27(2) . O22 C16 1.270(19) . O5 C7 1.273(16) . O14 C17 1.139(18) . O9 C8 1.230(16) . N3 C11 1.393(17) . N3 C13 1.27(2) . N1 Mn4 2.184(11) 8_554 N1 C3 1.392(17) . N1 C5 1.251(19) . N2 C5 1.302(19) . N2 C2 1.319(17) . N6 Mn4 2.156(11) 6_554 N6 C20 1.324(18) . N6 C19 1.391(18) . N5 C18 1.403(19) . N5 C19 1.32(2) . N4 C12 1.358(19) . N4 C13 1.38(2) . C12 C11 1.419(17) . C12 C14 1.504(17) . C18 C20 1.362(19) . C18 C17 1.52(2) . C20 C21 1.54(2) . C11 C10 1.557(18) . C3 C4 1.522(18) . C3 C2 1.476(18) . C13 H13 0.9500 . C15 C16 1.47(2) . C19 H19 0.9500 . C8 C9 1.49(2) . C5 H5 0.9500 . C2 C1 1.49(2) . C6 C7 1.53(2) . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 Mn1 O17 C10 O18 179.0(10) . Mn1 O17 C10 C11 8.3(15) . Mn1 O1 C1 O2 -170.3(12) . Mn1 O1 C1 C2 0.4(16) . Mn1 O13 C17 O14 -171.0(11) . Mn1 O13 C17 C18 -1.5(14) . Mn1 N3 C11 C12 -178.8(9) . Mn1 N3 C11 C10 3.3(13) . Mn1 N3 C13 N4 174.6(11) . Mn1 N2 C5 N1 179.5(11) . Mn1 N2 C2 C3 175.8(7) . Mn1 N2 C2 C1 -3.0(15) . Mn1 N5 C18 C20 173.9(8) . Mn1 N5 C18 C17 -5.8(15) . Mn1 N5 C19 N6 -175.4(10) . Mn3 O23 C16 O22 -163.4(10) 12_554 Mn3 O23 C16 C15 3.7(16) 12_554 Mn3 O21 C15 O24 -174.2(11) . Mn3 O21 C15 C16 17.6(17) . Mn3 O19 C14 O20 -134.8(11) . Mn3 O19 C14 C12 38.0(17) . Mn3 O24 C15 O21 172.1(11) 12_554 Mn3 O24 C15 C16 -18.9(15) 12_554 Mn3 O18 C10 O17 148.8(11) . Mn3 O18 C10 C11 -40.3(16) . Mn3 O22 C16 O23 168.3(10) . Mn3 O22 C16 C15 1.0(15) . Mn4 O20 C14 O19 169.2(10) . Mn4 O20 C14 C12 -4.0(14) . Mn4 O4 C4 O3 176.6(10) 8_554 Mn4 O4 C4 C3 -1.1(15) 8_554 Mn4 O16 C21 O15 -176.2(10) 6_554 Mn4 O16 C21 C20 -2.3(15) 6_554 Mn4 N1 C3 C4 -2.8(13) 8_554 Mn4 N1 C3 C2 172.3(7) 8_554 Mn4 N1 C5 N2 -171.1(11) 8_554 Mn4 N6 C20 C18 170.1(8) 6_554 Mn4 N6 C20 C21 -6.1(14) 6_554 Mn4 N6 C19 N5 -169.4(10) 6_554 Mn4 N4 C12 C11 -178.3(9) . Mn4 N4 C12 C14 15.5(17) . Mn4 N4 C13 N3 176.1(12) . Mn2 O2 C1 O1 129.6(15) . Mn2 O2 C1 C2 -41.2(18) . Mn2 O8 C6 O7 -166.5(10) . Mn2 O8 C6 C7 16.2(13) . Mn2 O3 C4 O4 -147.7(12) . Mn2 O3 C4 C3 29.8(19) . Mn2 O12 C9 O11 167.7(10) . Mn2 O12 C9 C8 -11.0(16) . Mn2 O5 C7 O6 172.4(11) . Mn2 O5 C7 C6 -12.8(14) . Mn2 O9 C8 O10 176.7(13) . Mn2 O9 C8 C9 13.7(18) . Mn5 O6 C7 O5 -169.0(10) 4 Mn5 O6 C7 C6 16.0(15) 4 Mn5 O7 C6 O8 174.4(9) 4 Mn5 O7 C6 C7 -8.3(13) 4 Mn5 O10 C8 O9 170.9(13) 15_454 Mn5 O10 C8 C9 -25.5(16) 15_454 Mn5 O15 C21 O16 -147.2(11) . Mn5 O15 C21 C20 39.5(19) . Mn5 O11 C9 O12 -171.7(9) 15_454 Mn5 O11 C9 C8 7(2) 15_454 Mn5 O14 C17 O13 128.5(13) . Mn5 O14 C17 C18 -39(2) . O21 C15 C16 O23 179.1(14) . O21 C15 C16 O22 -14(2) . O24 C15 C16 O23 10.0(19) . O24 C15 C16 O22 177.4(12) . O7 C6 C7 O6 -5.1(17) . O7 C6 C7 O5 179.5(11) . O10 C8 C9 O12 -167.3(13) . O10 C8 C9 O11 14(3) . O8 C6 C7 O6 172.4(11) . O8 C6 C7 O5 -2.9(17) . O9 C8 C9 O12 -2(2) . O9 C8 C9 O11 179.3(16) . N3 C11 C10 O17 -8.1(16) . N3 C11 C10 O18 -179.4(11) . N1 C3 C4 O4 2.6(16) . N1 C3 C4 O3 -175.1(11) . N1 C3 C2 N2 4.8(13) . N1 C3 C2 C1 -176.7(14) . N2 C2 C1 O1 1.8(19) . N2 C2 C1 O2 173.7(12) . N6 C20 C21 O16 5.6(17) . N6 C20 C21 O15 179.2(13) . N5 C18 C20 N6 4.5(15) . N5 C18 C20 C21 179.9(13) . N5 C18 C17 O13 4.6(16) . N5 C18 C17 O14 173.7(14) . N4 C12 C11 N3 3.3(15) . N4 C12 C11 C10 -179.5(13) . N4 C12 C14 O20 -7.5(17) . N4 C12 C14 O19 178.8(13) . C12 N4 C13 N3 5.6(19) . C12 C11 C10 O17 174.9(14) . C12 C11 C10 O18 4(2) . C18 N5 C19 N6 -0.8(14) . C18 C20 C21 O16 -169.6(14) . C18 C20 C21 O15 4(2) . C20 N6 C19 N5 3.5(14) . C20 C18 C17 O13 -175.0(13) . C20 C18 C17 O14 -6(2) . C11 N3 C13 N4 -3.6(18) . C11 C12 C14 O20 -169.6(14) . C11 C12 C14 O19 17(2) . C3 N1 C5 N2 11.7(17) . C3 C2 C1 O1 -176.5(13) . C3 C2 C1 O2 -5(2) . C13 N3 C11 C12 0.0(15) . C13 N3 C11 C10 -177.8(11) . C13 N4 C12 C11 -4.9(15) . C13 N4 C12 C14 -171.1(13) . C4 C3 C2 N2 178.6(13) . C4 C3 C2 C1 -3(2) . C19 N6 C20 C18 -4.7(14) . C19 N6 C20 C21 179.1(11) . C19 N5 C18 C20 -2.1(14) . C19 N5 C18 C17 178.2(11) . C5 N1 C3 C4 175.3(12) . C5 N1 C3 C2 -9.5(13) . C5 N2 C2 C3 1.5(14) . C5 N2 C2 C1 -177.3(12) . C14 C12 C11 N3 166.2(15) . C14 C12 C11 C10 -17(3) . C2 N2 C5 N1 -8.7(18) . C2 C3 C4 O4 -170.5(13) . C2 C3 C4 O3 12(2) . C17 C18 C20 N6 -175.9(12) . C17 C18 C20 C21 0(2) . 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 -0.002 -0.030 -0.002 14672 6730 ' ' 2 0.000 0.000 0.250 93 15 ' ' 3 0.000 0.000 0.750 93 15 ' ' 4 0.500 0.500 0.250 93 15 ' ' 5 0.500 0.500 0.750 93 15 ' ' loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.63(5) 2 0.37(5)