#------------------------------------------------------------------------------ #$Date: 2020-09-01 04:41:55 +0300 (Tue, 01 Sep 2020) $ #$Revision: 255771 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/53/7705327.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_7705327 loop_ _publ_author_name 'Lippi, Martina' 'Caputo, Josefina' 'Meneghetti, Fiorella' 'Castellano, Carlo' 'Marti-Rujas, Javier' 'Cametti, Massimo' _publ_section_title ; Tuneable Solvent Adsorption and Exchange by 1D Bispidine-Based Mn(II) Coordination Polymers via Ligand Design ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT02734K _journal_year 2020 _chemical_formula_sum 'C52 H62 Cl8 Mn N8 O10' _chemical_formula_weight 1297.63 _space_group_crystal_system triclinic _space_group_IT_number 1 _space_group_name_Hall 'P 1' _space_group_name_H-M_alt 'P 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2017/1 _audit_update_record ; 2020-07-12 deposited with the CCDC. 2020-08-31 downloaded from the CCDC. ; _cell_angle_alpha 77.600(5) _cell_angle_beta 85.900(5) _cell_angle_gamma 69.600(5) _cell_formula_units_Z 1 _cell_length_a 9.715(5) _cell_length_b 12.840(5) _cell_length_c 13.069(5) _cell_measurement_reflns_used 7868 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 31.172 _cell_measurement_theta_min 2.177 _cell_volume 1492.3(11) _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _diffrn_ambient_temperature 120(2) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.887 _diffrn_measurement_device_type 'Bruker APEX II CCD diffractometer' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0 _diffrn_reflns_av_unetI/netI 0.0184 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.887 _diffrn_reflns_number 15671 _diffrn_reflns_point_group_measured_fraction_full 0.950 _diffrn_reflns_point_group_measured_fraction_max 0.782 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.596 _diffrn_reflns_theta_min 1.595 _exptl_absorpt_coefficient_mu 0.641 _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.444 _exptl_crystal_description prism _exptl_crystal_F_000 671 _exptl_crystal_size_max 0.070 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.030 _refine_diff_density_max 1.205 _refine_diff_density_min -0.982 _refine_diff_density_rms 0.090 _refine_ls_abs_structure_details ; Flack x determined using 5965 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.517(8) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 712 _refine_ls_number_reflns 15671 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.045 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0507 _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^)+(0.0498P)^2^+3.0297P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1206 _refine_ls_wR_factor_ref 0.1278 _reflns_Friedel_coverage 0.764 _reflns_Friedel_fraction_full 0.905 _reflns_Friedel_fraction_max 0.677 _reflns_number_gt 14637 _reflns_number_total 15671 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02734k2.cif _cod_data_source_block shelx _cod_database_code 7705327 _shelx_shelxl_version_number 2017/1 _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. ; _shelx_estimated_absorpt_t_min 0.957 _shelx_estimated_absorpt_t_max 0.981 _shelx_res_file ; TITL TCMny_120_p1 in P1 shelx.res created by SHELXL-2017/1 at 11:37:57 on 08-Jul-2020 CELL 0.71073 9.7150 12.8400 13.0690 77.600 85.900 69.600 ZERR 1.00 0.0050 0.0050 0.0050 0.005 0.005 0.005 LATT -1 SFAC C N O CL MN H UNIT 52 8 10 8 1 62 MERG 2 FMAP 2 PLAN 20 SIZE 0.030 0.050 0.070 ACTA L.S. 8 TEMP -153.00 WGHT 0.049800 3.029700 FVAR 0.32722 MN 5 0.977175 0.614727 0.254418 11.00000 0.01660 0.00740 = 0.01171 -0.00292 0.00021 -0.00449 CL1 4 0.721915 0.712503 0.190999 11.00000 0.01747 0.01397 = 0.01908 -0.00501 -0.00163 -0.00253 CL2 4 1.233878 0.515294 0.318214 11.00000 0.01719 0.01493 = 0.02087 -0.00515 -0.00202 -0.00341 CL3 4 1.292598 1.539435 -0.036554 11.00000 0.05269 0.08032 = 0.04591 -0.01304 0.01286 -0.02312 CL4 4 1.443444 1.626829 0.410785 11.00000 0.05051 0.06467 = 0.07410 -0.03143 0.01749 -0.03382 CL5 4 1.650670 1.642524 0.550002 11.00000 0.05139 0.12462 = 0.05276 -0.04221 -0.01028 0.01260 CL6 4 1.529390 1.380691 0.090414 11.00000 0.07467 0.05244 = 0.07363 -0.00314 0.00272 0.00278 CL7 4 1.483403 1.619898 0.061125 11.00000 0.08215 0.09676 = 0.15922 -0.08263 0.06246 -0.06835 CL8 4 1.433193 1.843935 0.444424 11.00000 0.09177 0.04542 = 0.05414 -0.00695 0.01206 -0.02075 N1 2 0.947334 0.738439 -0.633215 11.00000 0.01810 0.01085 = 0.01521 -0.00445 0.00001 -0.00276 N2 2 0.901535 1.485179 -0.626235 11.00000 0.02163 0.01444 = 0.01337 -0.00028 -0.00147 -0.00765 N3 2 1.051561 0.746206 0.134469 11.00000 0.02108 0.01143 = 0.01541 -0.00203 -0.00066 -0.00678 N4 2 1.050975 1.145163 0.004375 11.00000 0.02072 0.00904 = 0.01290 -0.00540 0.00432 -0.00551 N5 2 1.358309 1.097289 -0.000417 11.00000 0.02019 0.01385 = 0.01213 -0.00247 -0.00388 -0.00647 N6 2 1.010685 1.490803 0.141805 11.00000 0.01994 0.01081 = 0.01429 -0.00491 -0.00047 -0.00576 N7 2 0.593503 1.169021 -0.501505 11.00000 0.01680 0.01886 = 0.01418 -0.00386 -0.00333 -0.00621 N8 2 0.908807 1.086964 -0.497300 11.00000 0.01845 0.00862 = 0.01450 -0.00409 0.00384 -0.00804 O6 3 1.133753 0.964332 -0.245251 11.00000 0.03116 0.02249 = 0.02128 -0.01130 -0.00412 -0.00864 O8 3 1.043963 1.420118 -0.240971 11.00000 0.02691 0.01807 = 0.02287 0.00426 -0.00340 -0.00703 O1 3 0.720602 1.057500 -0.209793 11.00000 0.04221 0.01874 = 0.00932 -0.00281 0.00284 -0.01230 C47 1 1.162552 1.356752 -0.210932 11.00000 0.02270 0.01157 = 0.01524 -0.00323 0.00131 -0.00908 O3 3 0.626458 1.355106 -0.291098 11.00000 0.02836 0.03314 = 0.04832 -0.03066 -0.00848 0.00471 O9 3 1.287816 1.372647 -0.246472 11.00000 0.02103 0.01802 = 0.02440 0.00797 -0.00252 -0.00907 O7 3 1.217445 1.168585 -0.288085 11.00000 0.03330 0.01757 = 0.01275 -0.00209 0.00273 -0.00913 C3 1 0.823910 1.428545 -0.656620 11.00000 0.02401 0.01520 = 0.01237 -0.00022 -0.00121 -0.01060 AFIX 43 H3 6 0.773261 1.459189 -0.721748 11.00000 -1.20000 AFIX 0 C1 1 1.400280 1.519375 0.073441 11.00000 0.04148 0.04085 = 0.04059 -0.01598 0.01451 -0.01901 AFIX 13 H1 6 1.335138 1.524578 0.136320 11.00000 -1.20000 AFIX 0 C21 1 0.837456 0.927569 -0.600522 11.00000 0.02040 0.01033 = 0.01413 -0.00485 -0.00264 0.00018 AFIX 43 H21 6 0.773112 1.003239 -0.623339 11.00000 -1.20000 AFIX 0 C14 1 0.896707 0.979699 -0.435901 11.00000 0.02019 0.00887 = 0.01130 -0.00317 -0.00183 -0.00499 AFIX 13 H14 6 0.977745 0.945850 -0.382821 11.00000 -1.20000 AFIX 0 C31 1 1.224974 1.039611 -0.121425 11.00000 0.01621 0.00916 = 0.00957 -0.00338 0.00042 -0.00415 O4 3 0.870124 0.825817 -0.258742 11.00000 0.04439 0.01576 = 0.01920 0.00256 -0.00375 -0.01340 O5 3 1.358026 0.866878 -0.176870 11.00000 0.02627 0.01788 = 0.03535 -0.01711 0.00364 -0.00428 C35 1 1.053857 1.254451 -0.059176 11.00000 0.01882 0.00983 = 0.01393 -0.00269 -0.00019 -0.00721 AFIX 13 H35 6 0.965304 1.286955 -0.105734 11.00000 -1.20000 AFIX 0 C4 1 0.813674 1.327524 -0.597930 11.00000 0.02260 0.01758 = 0.01200 -0.00049 -0.00390 -0.00988 AFIX 43 H4 6 0.760345 1.288839 -0.623519 11.00000 -1.20000 AFIX 0 C32 1 1.366210 1.007693 -0.055706 11.00000 0.01585 0.01264 = 0.01360 -0.00131 -0.00046 -0.00472 AFIX 23 H32A 6 1.378898 0.936088 -0.004246 11.00000 -1.20000 H32B 6 1.452637 0.995112 -0.102537 11.00000 -1.20000 AFIX 0 O10 3 0.642394 0.852268 -0.310973 11.00000 0.04487 0.03032 = 0.04025 0.00423 -0.00477 -0.02667 C36 1 1.076721 1.057965 -0.058676 11.00000 0.01667 0.00836 = 0.01171 -0.00307 -0.00089 -0.00355 AFIX 13 H36 6 0.994747 1.084973 -0.110678 11.00000 -1.20000 AFIX 0 C53 1 0.746401 1.264965 -0.290171 11.00000 0.02333 0.01149 = 0.01478 -0.00497 0.00324 -0.00671 C27 1 1.074464 0.946512 0.009670 11.00000 0.01683 0.01092 = 0.01329 -0.00425 0.00160 -0.00558 C34 1 1.192215 1.244294 -0.131396 11.00000 0.01837 0.00977 = 0.01118 -0.00307 -0.00111 -0.00545 C15 1 0.738967 1.077913 -0.304021 11.00000 0.01686 0.01157 = 0.01320 -0.00191 -0.00013 -0.00597 C26 1 0.994205 0.888836 -0.024497 11.00000 0.02113 0.01075 = 0.01429 -0.00020 -0.00248 -0.00857 AFIX 43 H26 6 0.946484 0.916219 -0.090807 11.00000 -1.20000 AFIX 0 C8 1 0.883141 1.172686 -0.432162 11.00000 0.01731 0.00927 = 0.01268 -0.00308 0.00069 -0.00559 AFIX 13 H8 6 0.967154 1.145320 -0.381823 11.00000 -1.20000 AFIX 0 C45 1 1.108469 1.384752 0.163812 11.00000 0.02049 0.01344 = 0.01505 -0.00492 -0.00247 -0.00268 AFIX 43 H45 6 1.169958 1.363612 0.223541 11.00000 -1.20000 AFIX 0 C38 1 1.209212 1.152994 -0.194155 11.00000 0.01579 0.01159 = 0.01183 -0.00403 0.00062 -0.00446 C25 1 0.985863 0.790753 0.040623 11.00000 0.02661 0.01479 = 0.01708 -0.00224 -0.00163 -0.01241 AFIX 43 H25 6 0.929934 0.752588 0.017236 11.00000 -1.20000 AFIX 0 C5 1 0.884083 1.283999 -0.499863 11.00000 0.01696 0.00744 = 0.01214 -0.00151 -0.00100 -0.00475 C20 1 0.915578 0.897045 -0.507094 11.00000 0.01976 0.00966 = 0.01398 -0.00321 -0.00064 -0.00454 C24 1 1.013021 0.785847 -0.480129 11.00000 0.02287 0.01236 = 0.01263 -0.00386 -0.00427 -0.00165 AFIX 43 H24 6 1.069347 0.761839 -0.417499 11.00000 -1.20000 AFIX 0 O2 3 0.850916 1.242434 -0.235275 11.00000 0.02940 0.02087 = 0.02309 -0.01105 -0.00752 -0.00490 C7 1 0.963630 1.444400 -0.531075 11.00000 0.02738 0.01453 = 0.01839 -0.00158 -0.00300 -0.01355 AFIX 43 H7 6 1.015478 1.485156 -0.507100 11.00000 -1.20000 AFIX 0 C6 1 0.956482 1.345957 -0.465534 11.00000 0.02307 0.01501 = 0.01402 -0.00176 -0.00458 -0.00764 AFIX 43 H6 6 1.000654 1.321376 -0.398016 11.00000 -1.20000 AFIX 0 C13 1 0.746609 0.998901 -0.376328 11.00000 0.02384 0.00939 = 0.01441 -0.00131 -0.00019 -0.00830 C23 1 1.027080 0.710545 -0.545464 11.00000 0.01924 0.00870 = 0.01766 -0.00300 -0.00323 -0.00368 AFIX 43 H23 6 1.096268 0.635924 -0.527219 11.00000 -1.20000 AFIX 0 C33 1 1.340391 1.203852 -0.073346 11.00000 0.01880 0.01364 = 0.01747 -0.00384 -0.00314 -0.00545 AFIX 23 H33A 6 1.421836 1.193397 -0.124514 11.00000 -1.20000 H33B 6 1.342921 1.261687 -0.034851 11.00000 -1.20000 AFIX 0 C37 1 0.902420 1.165361 0.051502 11.00000 0.02248 0.01559 = 0.02596 -0.00802 0.00928 -0.00924 AFIX 133 H37A 6 0.828557 1.192408 -0.004339 11.00000 -1.20000 H37B 6 0.883010 1.222598 0.094681 11.00000 -1.20000 H37C 6 0.897762 1.094392 0.095229 11.00000 -1.20000 AFIX 0 C9 1 0.739311 1.192340 -0.366587 11.00000 0.01866 0.00943 = 0.01204 -0.00155 -0.00135 -0.00535 C12 1 0.603409 1.055935 -0.442788 11.00000 0.01627 0.02103 = 0.01590 -0.00704 -0.00075 -0.00758 AFIX 23 H12A 6 0.601396 1.007934 -0.492283 11.00000 -1.20000 H12B 6 0.517385 1.062081 -0.396009 11.00000 -1.20000 AFIX 0 C44 1 0.926698 1.519275 0.056333 11.00000 0.02341 0.01098 = 0.01469 -0.00400 -0.00082 -0.00398 AFIX 43 H44 6 0.855009 1.593132 0.040943 11.00000 -1.20000 AFIX 0 C17 1 0.469086 1.224032 -0.576672 11.00000 0.01912 0.02246 = 0.01878 -0.00373 -0.00465 -0.00273 AFIX 13 H17 6 0.462649 1.304960 -0.600844 11.00000 -1.20000 AFIX 0 C28 1 1.144957 0.900573 0.105624 11.00000 0.02321 0.01631 = 0.01665 -0.00326 0.00051 -0.01332 AFIX 43 H28 6 1.201196 0.937338 0.130855 11.00000 -1.20000 AFIX 0 C22 1 0.854525 0.846241 -0.660089 11.00000 0.02424 0.01354 = 0.01377 -0.00415 -0.00403 -0.00525 AFIX 43 H22 6 0.798286 0.867581 -0.722512 11.00000 -1.20000 AFIX 0 C19 1 1.057582 1.062926 -0.540415 11.00000 0.02348 0.01767 = 0.02678 -0.01069 0.00908 -0.00798 AFIX 133 H19A 6 1.065354 1.131867 -0.586240 11.00000 -1.20000 H19B 6 1.078034 1.003143 -0.580826 11.00000 -1.20000 H19C 6 1.128814 1.037698 -0.483003 11.00000 -1.20000 AFIX 0 C42 1 1.040209 1.336536 0.012154 11.00000 0.01663 0.01016 = 0.01308 -0.00423 0.00060 -0.00665 C46 1 1.123814 1.304733 0.103412 11.00000 0.02045 0.01087 = 0.01618 -0.00337 -0.00347 -0.00320 AFIX 43 H46 6 1.190279 1.229390 0.123897 11.00000 -1.20000 AFIX 0 C43 1 0.939344 1.445931 -0.011023 11.00000 0.01858 0.01247 = 0.01799 -0.00397 -0.00365 -0.00685 AFIX 43 H43 6 0.879698 1.470445 -0.072071 11.00000 -1.20000 AFIX 0 C39 1 1.473619 1.067379 0.078578 11.00000 0.01780 0.01756 = 0.01684 -0.00129 -0.00465 -0.00498 AFIX 13 H39 6 1.465738 1.139049 0.100838 11.00000 -1.20000 AFIX 0 C10 1 0.595091 1.241489 -0.431272 11.00000 0.01630 0.01412 = 0.01489 -0.00312 -0.00035 -0.00414 AFIX 23 H10A 6 0.510242 1.248902 -0.383206 11.00000 -1.20000 H10B 6 0.585586 1.318060 -0.472308 11.00000 -1.20000 AFIX 0 C16 1 0.320824 1.225410 -0.529245 11.00000 0.02066 0.04046 = 0.02500 -0.00018 -0.00180 -0.01038 AFIX 133 H16A 6 0.326470 1.147881 -0.496334 11.00000 -1.20000 H16B 6 0.245803 1.256389 -0.584485 11.00000 -1.20000 H16C 6 0.294775 1.272847 -0.476391 11.00000 -1.20000 AFIX 0 C29 1 1.133094 0.800079 0.165133 11.00000 0.01990 0.01699 = 0.01537 0.00017 -0.00442 -0.00685 AFIX 43 H29 6 1.184567 0.768348 0.229881 11.00000 -1.20000 AFIX 0 C48 1 1.269763 1.471204 -0.329755 11.00000 0.03002 0.02080 = 0.03124 0.01101 -0.00170 -0.01050 AFIX 133 H48A 6 1.218207 1.465313 -0.388874 11.00000 -1.20000 H48B 6 1.366451 1.475039 -0.352718 11.00000 -1.20000 H48C 6 1.212417 1.539945 -0.304023 11.00000 -1.20000 AFIX 0 C40 1 1.630286 1.018290 0.039712 11.00000 0.01506 0.03439 = 0.02614 -0.00288 -0.00148 -0.00880 AFIX 133 H40A 6 1.643159 0.946786 0.018444 11.00000 -1.20000 H40B 6 1.699783 1.004255 0.096085 11.00000 -1.20000 H40C 6 1.648498 1.072313 -0.020346 11.00000 -1.20000 AFIX 0 C49 1 1.232130 0.953848 -0.189324 11.00000 0.02353 0.01383 = 0.01567 -0.00646 0.00493 -0.00983 C54 1 0.634184 1.425738 -0.218451 11.00000 0.04625 0.05216 = 0.07581 -0.05566 -0.01885 0.01488 AFIX 133 H54A 6 0.635589 1.383802 -0.146185 11.00000 -1.20000 H54B 6 0.548283 1.495522 -0.228828 11.00000 -1.20000 H54C 6 0.723833 1.445018 -0.231864 11.00000 -1.20000 AFIX 0 C50 1 1.371958 0.783683 -0.239646 11.00000 0.03599 0.02472 = 0.05167 -0.02827 0.00997 -0.01094 AFIX 133 H50A 6 1.297957 0.747508 -0.217861 11.00000 -1.20000 H50B 6 1.470238 0.725985 -0.229925 11.00000 -1.20000 H50C 6 1.357121 0.821188 -0.313685 11.00000 -1.20000 AFIX 0 C18 1 0.499763 1.170981 -0.672985 11.00000 0.03398 0.04035 = 0.02475 -0.01286 -0.01071 0.00103 AFIX 133 H18A 6 0.595197 1.171665 -0.702362 11.00000 -1.20000 H18B 6 0.422669 1.214539 -0.725438 11.00000 -1.20000 H18C 6 0.501201 1.092535 -0.653255 11.00000 -1.20000 AFIX 0 C41 1 1.444558 0.987519 0.175366 11.00000 0.01995 0.02215 = 0.01681 -0.00115 -0.00266 -0.00468 AFIX 133 H41A 6 1.347905 1.024165 0.203991 11.00000 -1.20000 H41B 6 1.520381 0.969743 0.228259 11.00000 -1.20000 H41C 6 1.446709 0.917319 0.156055 11.00000 -1.20000 AFIX 0 C51 1 0.874347 0.716183 -0.198890 11.00000 0.06655 0.01743 = 0.02702 0.00686 -0.00890 -0.01442 AFIX 133 H51A 6 0.794286 0.726151 -0.147788 11.00000 -1.20000 H51B 6 0.968669 0.678043 -0.162040 11.00000 -1.20000 H51C 6 0.862952 0.669975 -0.246236 11.00000 -1.20000 AFIX 0 C52 1 0.743798 0.885237 -0.312464 11.00000 0.03748 0.01397 = 0.01581 -0.00362 0.00069 -0.01133 C2 1 1.545900 1.705947 0.433587 11.00000 0.03572 0.05088 = 0.03291 -0.01707 0.00937 -0.01425 AFIX 13 H2 6 1.614444 1.711399 0.373452 11.00000 -1.20000 AFIX 0 HKLF 4 REM TCMny_120_p1 in P1 REM R1 = 0.0507 for 14637 Fo > 4sig(Fo) and 0.0567 for all 15671 data REM 712 parameters refined using 3 restraints END WGHT 0.0494 3.0376 REM Highest difference peak 1.205, deepest hole -0.982, 1-sigma level 0.090 Q1 1 1.4973 1.5769 0.4679 11.00000 0.05 1.20 Q2 1 1.3657 1.8110 0.4054 11.00000 0.05 1.20 Q3 1 1.5836 1.4239 0.1007 11.00000 0.05 1.15 Q4 1 1.6136 1.7352 0.5109 11.00000 0.05 1.14 Q5 1 1.3077 1.6027 -0.0440 11.00000 0.05 1.08 Q6 1 1.5151 1.6019 0.1047 11.00000 0.05 0.78 Q7 1 0.9054 0.6607 0.2568 11.00000 0.05 0.72 Q8 1 1.0390 0.5723 0.2472 11.00000 0.05 0.66 Q9 1 1.3406 1.4913 0.0073 11.00000 0.05 0.64 Q10 1 0.9409 1.3968 -0.5004 11.00000 0.05 0.56 Q11 1 0.9592 0.5605 0.2699 11.00000 0.05 0.54 Q12 1 1.4505 1.6597 0.0398 11.00000 0.05 0.51 Q13 1 0.7385 1.1414 -0.3391 11.00000 0.05 0.50 Q14 1 1.0627 0.6268 0.1878 11.00000 0.05 0.49 Q15 1 0.7657 0.9471 -0.3413 11.00000 0.05 0.49 Q16 1 0.9087 1.3243 -0.4749 11.00000 0.05 0.48 Q17 1 1.0052 0.6609 0.2413 11.00000 0.05 0.48 Q18 1 1.2250 1.0947 -0.1557 11.00000 0.05 0.47 Q19 1 0.8989 0.5978 0.3263 11.00000 0.05 0.47 Q20 1 1.0417 0.9204 -0.0211 11.00000 0.05 0.47 ; _shelx_res_checksum 18949 loop_ _space_group_symop_operation_xyz 'x, y, z' 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 Mn Mn 0.97718(8) 0.61473(6) 0.25442(6) 0.01165(10) Uani 1 1 d . . . . . Cl1 Cl 0.72191(10) 0.71250(8) 0.19100(8) 0.0173(2) Uani 1 1 d . . . . . Cl2 Cl 1.23388(11) 0.51529(8) 0.31821(8) 0.0179(2) Uani 1 1 d . . . . . Cl3 Cl 1.2926(2) 1.5394(2) -0.03655(16) 0.0602(5) Uani 1 1 d . . . . . Cl4 Cl 1.4434(2) 1.62683(19) 0.41078(18) 0.0574(5) Uani 1 1 d . . . . . Cl5 Cl 1.6507(3) 1.6425(3) 0.55000(18) 0.0834(9) Uani 1 1 d . . . . . Cl6 Cl 1.5294(3) 1.3807(2) 0.0904(2) 0.0752(7) Uani 1 1 d . . . . . Cl7 Cl 1.4834(3) 1.6199(3) 0.0611(3) 0.0967(11) Uani 1 1 d . . . . . Cl8 Cl 1.4332(3) 1.84394(18) 0.44442(17) 0.0656(6) Uani 1 1 d . . . . . N1 N 0.9473(4) 0.7384(3) -0.6332(3) 0.0150(7) Uani 1 1 d . . . . . N2 N 0.9015(5) 1.4852(3) -0.6262(3) 0.0164(7) Uani 1 1 d . . . . . N3 N 1.0516(4) 0.7462(3) 0.1345(3) 0.0157(7) Uani 1 1 d . . . . . N4 N 1.0510(4) 1.1452(3) 0.0044(3) 0.0138(7) Uani 1 1 d . . . . . N5 N 1.3583(4) 1.0973(3) -0.0004(3) 0.0150(7) Uani 1 1 d . . . . . N6 N 1.0107(4) 1.4908(3) 0.1418(3) 0.0145(7) Uani 1 1 d . . . . . N7 N 0.5935(4) 1.1690(3) -0.5015(3) 0.0163(7) Uani 1 1 d . . . . . N8 N 0.9088(4) 1.0870(3) -0.4973(3) 0.0129(7) Uani 1 1 d . . . . . O6 O 1.1338(4) 0.9643(3) -0.2453(3) 0.0238(7) Uani 1 1 d . . . . . O8 O 1.0440(4) 1.4201(3) -0.2410(3) 0.0240(7) Uani 1 1 d . . . . . O1 O 0.7206(5) 1.0575(3) -0.2098(3) 0.0231(7) Uani 1 1 d . . . . . C47 C 1.1626(5) 1.3568(3) -0.2109(3) 0.0156(7) Uani 1 1 d . . . . . O3 O 0.6265(4) 1.3551(4) -0.2911(4) 0.0367(10) Uani 1 1 d . . . . . O9 O 1.2878(3) 1.3726(3) -0.2465(3) 0.0223(6) Uani 1 1 d . . . . . O7 O 1.2174(4) 1.1686(3) -0.2881(3) 0.0214(7) Uani 1 1 d . . . . . C3 C 0.8239(5) 1.4285(4) -0.6566(3) 0.0165(8) Uani 1 1 d . . . . . H3 H 0.773261 1.459189 -0.721748 0.020 Uiso 1 1 calc R U . . . C1 C 1.4003(8) 1.5194(6) 0.0734(5) 0.0392(14) Uani 1 1 d . . . . . H1 H 1.335138 1.524578 0.136320 0.047 Uiso 1 1 calc R U . . . C21 C 0.8375(5) 0.9276(4) -0.6005(3) 0.0159(8) Uani 1 1 d . . . . . H21 H 0.773112 1.003239 -0.623339 0.019 Uiso 1 1 calc R U . . . C14 C 0.8967(5) 0.9797(4) -0.4359(3) 0.0132(8) Uani 1 1 d . . . . . H14 H 0.977745 0.945850 -0.382821 0.016 Uiso 1 1 calc R U . . . C31 C 1.2250(5) 1.0396(3) -0.1214(3) 0.0115(7) Uani 1 1 d . . . . . O4 O 0.8701(5) 0.8258(3) -0.2587(3) 0.0264(8) Uani 1 1 d . . . . . O5 O 1.3580(4) 0.8669(3) -0.1769(3) 0.0257(7) Uani 1 1 d . . . . . C35 C 1.0539(5) 1.2545(4) -0.0592(3) 0.0135(8) Uani 1 1 d . . . . . H35 H 0.965304 1.286955 -0.105734 0.016 Uiso 1 1 calc R U . . . C4 C 0.8137(5) 1.3275(4) -0.5979(3) 0.0168(9) Uani 1 1 d . . . . . H4 H 0.760345 1.288839 -0.623519 0.020 Uiso 1 1 calc R U . . . C32 C 1.3662(5) 1.0077(4) -0.0557(3) 0.0143(8) Uani 1 1 d . . . . . H32A H 1.378898 0.936088 -0.004246 0.017 Uiso 1 1 calc R U . . . H32B H 1.452637 0.995112 -0.102537 0.017 Uiso 1 1 calc R U . . . O10 O 0.6424(5) 0.8523(3) -0.3110(3) 0.0363(9) Uani 1 1 d . . . . . C36 C 1.0767(5) 1.0580(3) -0.0587(3) 0.0122(7) Uani 1 1 d . . . . . H36 H 0.994747 1.084973 -0.110678 0.015 Uiso 1 1 calc R U . . . C53 C 0.7464(5) 1.2650(4) -0.2902(3) 0.0161(8) Uani 1 1 d . . . . . C27 C 1.0745(5) 0.9465(4) 0.0097(3) 0.0132(8) Uani 1 1 d . . . . . C34 C 1.1922(5) 1.2443(3) -0.1314(3) 0.0127(7) Uani 1 1 d . . . . . C15 C 0.7390(5) 1.0779(4) -0.3040(3) 0.0137(8) Uani 1 1 d . . . . . C26 C 0.9942(5) 0.8888(4) -0.0245(3) 0.0148(8) Uani 1 1 d . . . . . H26 H 0.946484 0.916219 -0.090807 0.018 Uiso 1 1 calc R U . . . C8 C 0.8831(5) 1.1727(3) -0.4322(3) 0.0127(7) Uani 1 1 d . . . . . H8 H 0.967154 1.145320 -0.381823 0.015 Uiso 1 1 calc R U . . . C45 C 1.1085(5) 1.3848(4) 0.1638(4) 0.0167(8) Uani 1 1 d . . . . . H45 H 1.169958 1.363612 0.223541 0.020 Uiso 1 1 calc R U . . . C38 C 1.2092(5) 1.1530(4) -0.1942(3) 0.0129(7) Uani 1 1 d . . . . . C25 C 0.9859(6) 0.7908(4) 0.0406(4) 0.0181(9) Uani 1 1 d . . . . . H25 H 0.929934 0.752588 0.017236 0.022 Uiso 1 1 calc R U . . . C5 C 0.8841(5) 1.2840(3) -0.4999(3) 0.0120(7) Uani 1 1 d . . . . . C20 C 0.9156(5) 0.8970(4) -0.5071(3) 0.0144(8) Uani 1 1 d . . . . . C24 C 1.0130(5) 0.7858(4) -0.4801(4) 0.0167(8) Uani 1 1 d . . . . . H24 H 1.069347 0.761839 -0.417499 0.020 Uiso 1 1 calc R U . . . O2 O 0.8509(4) 1.2424(3) -0.2353(3) 0.0240(7) Uani 1 1 d . . . . . C7 C 0.9636(6) 1.4444(4) -0.5311(4) 0.0185(9) Uani 1 1 d . . . . . H7 H 1.015478 1.485156 -0.507100 0.022 Uiso 1 1 calc R U . . . C6 C 0.9565(5) 1.3460(4) -0.4655(3) 0.0170(8) Uani 1 1 d . . . . . H6 H 1.000654 1.321376 -0.398016 0.020 Uiso 1 1 calc R U . . . C13 C 0.7466(5) 0.9989(4) -0.3763(3) 0.0153(8) Uani 1 1 d . . . . . C23 C 1.0271(5) 0.7105(4) -0.5455(3) 0.0153(8) Uani 1 1 d . . . . . H23 H 1.096268 0.635924 -0.527219 0.018 Uiso 1 1 calc R U . . . C33 C 1.3404(5) 1.2039(4) -0.0733(3) 0.0164(8) Uani 1 1 d . . . . . H33A H 1.421836 1.193397 -0.124514 0.020 Uiso 1 1 calc R U . . . H33B H 1.342921 1.261687 -0.034851 0.020 Uiso 1 1 calc R U . . . C37 C 0.9024(5) 1.1654(4) 0.0515(4) 0.0205(9) Uani 1 1 d . . . . . H37A H 0.828557 1.192408 -0.004339 0.025 Uiso 1 1 calc R U . . . H37B H 0.883010 1.222598 0.094681 0.025 Uiso 1 1 calc R U . . . H37C H 0.897762 1.094392 0.095229 0.025 Uiso 1 1 calc R U . . . C9 C 0.7393(5) 1.1923(4) -0.3666(3) 0.0133(8) Uani 1 1 d . . . . . C12 C 0.6034(5) 1.0559(4) -0.4428(3) 0.0168(8) Uani 1 1 d . . . . . H12A H 0.601396 1.007934 -0.492283 0.020 Uiso 1 1 calc R U . . . H12B H 0.517385 1.062081 -0.396009 0.020 Uiso 1 1 calc R U . . . C44 C 0.9267(5) 1.5193(4) 0.0563(3) 0.0166(8) Uani 1 1 d . . . . . H44 H 0.855009 1.593132 0.040943 0.020 Uiso 1 1 calc R U . . . C17 C 0.4691(5) 1.2240(4) -0.5767(3) 0.0211(8) Uani 1 1 d . . . . . H17 H 0.462649 1.304960 -0.600844 0.025 Uiso 1 1 calc R U . . . C28 C 1.1450(5) 0.9006(4) 0.1056(4) 0.0170(8) Uani 1 1 d . . . . . H28 H 1.201196 0.937338 0.130855 0.020 Uiso 1 1 calc R U . . . C22 C 0.8545(5) 0.8462(4) -0.6601(3) 0.0171(8) Uani 1 1 d . . . . . H22 H 0.798286 0.867581 -0.722512 0.020 Uiso 1 1 calc R U . . . C19 C 1.0576(6) 1.0629(4) -0.5404(4) 0.0219(9) Uani 1 1 d . . . . . H19A H 1.065354 1.131867 -0.586240 0.026 Uiso 1 1 calc R U . . . H19B H 1.078034 1.003143 -0.580826 0.026 Uiso 1 1 calc R U . . . H19C H 1.128814 1.037698 -0.483003 0.026 Uiso 1 1 calc R U . . . C42 C 1.0402(5) 1.3365(3) 0.0122(3) 0.0125(7) Uani 1 1 d . . . . . C46 C 1.1238(5) 1.3047(4) 0.1034(4) 0.0161(8) Uani 1 1 d . . . . . H46 H 1.190279 1.229390 0.123897 0.019 Uiso 1 1 calc R U . . . C43 C 0.9393(5) 1.4459(4) -0.0110(4) 0.0156(8) Uani 1 1 d . . . . . H43 H 0.879698 1.470445 -0.072071 0.019 Uiso 1 1 calc R U . . . C39 C 1.4736(4) 1.0674(4) 0.0786(3) 0.0178(7) Uani 1 1 d . . . . . H39 H 1.465738 1.139049 0.100838 0.021 Uiso 1 1 calc R U . . . C10 C 0.5951(5) 1.2415(4) -0.4313(3) 0.0153(8) Uani 1 1 d . . . . . H10A H 0.510242 1.248902 -0.383206 0.018 Uiso 1 1 calc R U . . . H10B H 0.585586 1.318060 -0.472308 0.018 Uiso 1 1 calc R U . . . C16 C 0.3208(6) 1.2254(5) -0.5292(5) 0.0297(11) Uani 1 1 d . . . . . H16A H 0.326470 1.147881 -0.496334 0.036 Uiso 1 1 calc R U . . . H16B H 0.245803 1.256389 -0.584485 0.036 Uiso 1 1 calc R U . . . H16C H 0.294775 1.272847 -0.476391 0.036 Uiso 1 1 calc R U . . . C29 C 1.1331(5) 0.8001(4) 0.1651(4) 0.0176(8) Uani 1 1 d . . . . . H29 H 1.184567 0.768348 0.229881 0.021 Uiso 1 1 calc R U . . . C48 C 1.2698(6) 1.4712(4) -0.3298(4) 0.0294(10) Uani 1 1 d . . . . . H48A H 1.218207 1.465313 -0.388874 0.035 Uiso 1 1 calc R U . . . H48B H 1.366451 1.475039 -0.352718 0.035 Uiso 1 1 calc R U . . . H48C H 1.212417 1.539945 -0.304023 0.035 Uiso 1 1 calc R U . . . C40 C 1.6303(5) 1.0183(5) 0.0397(4) 0.0255(10) Uani 1 1 d . . . . . H40A H 1.643159 0.946786 0.018444 0.031 Uiso 1 1 calc R U . . . H40B H 1.699783 1.004255 0.096085 0.031 Uiso 1 1 calc R U . . . H40C H 1.648498 1.072313 -0.020346 0.031 Uiso 1 1 calc R U . . . C49 C 1.2321(5) 0.9538(4) -0.1893(3) 0.0164(8) Uani 1 1 d . . . . . C54 C 0.6342(8) 1.4257(6) -0.2185(7) 0.059(2) Uani 1 1 d . . . . . H54A H 0.635589 1.383802 -0.146185 0.071 Uiso 1 1 calc R U . . . H54B H 0.548283 1.495522 -0.228828 0.071 Uiso 1 1 calc R U . . . H54C H 0.723833 1.445018 -0.231864 0.071 Uiso 1 1 calc R U . . . C50 C 1.3720(6) 0.7837(4) -0.2396(5) 0.0345(12) Uani 1 1 d . . . . . H50A H 1.297957 0.747508 -0.217861 0.041 Uiso 1 1 calc R U . . . H50B H 1.470238 0.725985 -0.229925 0.041 Uiso 1 1 calc R U . . . H50C H 1.357121 0.821188 -0.313685 0.041 Uiso 1 1 calc R U . . . C18 C 0.4998(6) 1.1710(5) -0.6730(4) 0.0352(12) Uani 1 1 d . . . . . H18A H 0.595197 1.171665 -0.702362 0.042 Uiso 1 1 calc R U . . . H18B H 0.422669 1.214539 -0.725438 0.042 Uiso 1 1 calc R U . . . H18C H 0.501201 1.092535 -0.653255 0.042 Uiso 1 1 calc R U . . . C41 C 1.4446(5) 0.9875(4) 0.1754(3) 0.0206(8) Uani 1 1 d . . . . . H41A H 1.347905 1.024165 0.203991 0.025 Uiso 1 1 calc R U . . . H41B H 1.520381 0.969743 0.228259 0.025 Uiso 1 1 calc R U . . . H41C H 1.446709 0.917319 0.156055 0.025 Uiso 1 1 calc R U . . . C51 C 0.8743(8) 0.7162(4) -0.1989(4) 0.0383(13) Uani 1 1 d . . . . . H51A H 0.794286 0.726151 -0.147788 0.046 Uiso 1 1 calc R U . . . H51B H 0.968669 0.678043 -0.162040 0.046 Uiso 1 1 calc R U . . . H51C H 0.862952 0.669975 -0.246236 0.046 Uiso 1 1 calc R U . . . C52 C 0.7438(6) 0.8852(4) -0.3125(3) 0.0217(9) Uani 1 1 d . . . . . C2 C 1.5459(7) 1.7059(6) 0.4336(5) 0.0391(14) Uani 1 1 d . . . . . H2 H 1.614444 1.711399 0.373452 0.047 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 Mn 0.0166(2) 0.00740(19) 0.0117(2) -0.00292(15) 0.00021(16) -0.00449(16) Cl1 0.0175(5) 0.0140(5) 0.0191(5) -0.0050(4) -0.0016(4) -0.0025(4) Cl2 0.0172(5) 0.0149(5) 0.0209(5) -0.0051(4) -0.0020(4) -0.0034(4) Cl3 0.0527(10) 0.0803(14) 0.0459(9) -0.0130(9) 0.0129(8) -0.0231(9) Cl4 0.0505(10) 0.0647(11) 0.0741(12) -0.0314(10) 0.0175(9) -0.0338(9) Cl5 0.0514(11) 0.125(2) 0.0528(11) -0.0422(13) -0.0103(9) 0.0126(12) Cl6 0.0747(15) 0.0524(12) 0.0736(15) -0.0031(10) 0.0027(12) 0.0028(10) Cl7 0.0821(17) 0.0968(19) 0.159(3) -0.083(2) 0.0625(18) -0.0683(16) Cl8 0.0918(16) 0.0454(10) 0.0541(11) -0.0070(8) 0.0121(10) -0.0207(10) N1 0.0181(18) 0.0108(17) 0.0152(17) -0.0044(13) 0.0000(14) -0.0028(14) N2 0.0216(19) 0.0144(17) 0.0134(17) -0.0003(13) -0.0015(14) -0.0077(15) N3 0.0211(19) 0.0114(16) 0.0154(17) -0.0020(13) -0.0007(14) -0.0068(14) N4 0.0207(18) 0.0090(15) 0.0129(16) -0.0054(12) 0.0043(14) -0.0055(13) N5 0.0202(16) 0.0139(16) 0.0121(15) -0.0025(12) -0.0039(12) -0.0065(13) N6 0.0199(18) 0.0108(16) 0.0143(17) -0.0049(13) -0.0005(14) -0.0058(14) N7 0.0168(16) 0.0189(17) 0.0142(15) -0.0039(13) -0.0033(12) -0.0062(13) N8 0.0185(18) 0.0086(15) 0.0145(16) -0.0041(12) 0.0038(13) -0.0080(13) O6 0.0312(18) 0.0225(16) 0.0213(16) -0.0113(12) -0.0041(13) -0.0086(14) O8 0.0269(17) 0.0181(15) 0.0229(16) 0.0043(12) -0.0034(13) -0.0070(13) O1 0.042(2) 0.0187(15) 0.0093(14) -0.0028(11) 0.0028(13) -0.0123(14) C47 0.023(2) 0.0116(16) 0.0152(18) -0.0032(13) 0.0013(15) -0.0091(15) O3 0.0284(19) 0.033(2) 0.048(2) -0.0307(19) -0.0085(17) 0.0047(15) O9 0.0210(15) 0.0180(14) 0.0244(15) 0.0080(11) -0.0025(12) -0.0091(11) O7 0.0333(18) 0.0176(15) 0.0128(14) -0.0021(11) 0.0027(13) -0.0091(13) C3 0.024(2) 0.015(2) 0.0124(19) -0.0002(15) -0.0012(16) -0.0106(17) C1 0.041(4) 0.041(3) 0.041(3) -0.016(3) 0.015(3) -0.019(3) C21 0.020(2) 0.0103(18) 0.0141(19) -0.0048(14) -0.0026(15) 0.0002(15) C14 0.020(2) 0.0089(17) 0.0113(18) -0.0032(13) -0.0018(15) -0.0050(15) C31 0.0162(19) 0.0092(17) 0.0096(16) -0.0034(13) 0.0004(14) -0.0041(14) O4 0.044(2) 0.0158(15) 0.0192(16) 0.0026(12) -0.0037(15) -0.0134(15) O5 0.0263(17) 0.0179(15) 0.0354(19) -0.0171(14) 0.0036(14) -0.0043(13) C35 0.019(2) 0.0098(18) 0.0139(19) -0.0027(14) -0.0002(15) -0.0072(15) C4 0.023(2) 0.018(2) 0.0120(19) -0.0005(15) -0.0039(17) -0.0099(18) C32 0.0159(18) 0.0126(17) 0.0136(17) -0.0013(13) -0.0005(14) -0.0047(14) O10 0.045(2) 0.0303(19) 0.040(2) 0.0042(15) -0.0048(17) -0.0267(17) C36 0.0167(19) 0.0084(17) 0.0117(18) -0.0031(14) -0.0009(15) -0.0036(14) C53 0.023(2) 0.0115(17) 0.0148(18) -0.0050(14) 0.0032(15) -0.0067(15) C27 0.017(2) 0.0109(18) 0.0133(19) -0.0043(14) 0.0016(15) -0.0056(15) C34 0.0184(19) 0.0098(17) 0.0112(17) -0.0031(13) -0.0011(14) -0.0055(14) C15 0.0169(19) 0.0116(18) 0.0132(18) -0.0019(14) -0.0001(15) -0.0060(15) C26 0.021(2) 0.0108(18) 0.0143(19) -0.0002(14) -0.0025(16) -0.0086(15) C8 0.0173(19) 0.0093(18) 0.0127(18) -0.0031(14) 0.0007(15) -0.0056(15) C45 0.020(2) 0.0134(19) 0.0151(19) -0.0049(15) -0.0025(16) -0.0027(16) C38 0.0158(19) 0.0116(18) 0.0118(18) -0.0040(13) 0.0006(15) -0.0045(15) C25 0.027(2) 0.015(2) 0.017(2) -0.0022(15) -0.0016(18) -0.0124(18) C5 0.0170(19) 0.0074(17) 0.0121(18) -0.0015(13) -0.0010(15) -0.0048(14) C20 0.020(2) 0.0097(18) 0.0140(19) -0.0032(14) -0.0006(16) -0.0045(15) C24 0.023(2) 0.0124(19) 0.0126(19) -0.0039(15) -0.0043(16) -0.0016(16) O2 0.0294(18) 0.0209(16) 0.0231(16) -0.0110(13) -0.0075(13) -0.0049(13) C7 0.027(2) 0.015(2) 0.018(2) -0.0016(16) -0.0030(18) -0.0135(18) C6 0.023(2) 0.015(2) 0.0140(19) -0.0018(15) -0.0046(17) -0.0076(17) C13 0.024(2) 0.0094(17) 0.0144(18) -0.0013(13) -0.0002(15) -0.0083(15) C23 0.019(2) 0.0087(18) 0.018(2) -0.0030(15) -0.0032(16) -0.0037(15) C33 0.0188(19) 0.0136(18) 0.0175(19) -0.0038(14) -0.0031(15) -0.0055(15) C37 0.022(2) 0.016(2) 0.026(2) -0.0080(17) 0.0093(19) -0.0092(18) C9 0.019(2) 0.0094(17) 0.0120(17) -0.0016(13) -0.0013(15) -0.0053(15) C12 0.0163(18) 0.021(2) 0.0159(19) -0.0070(15) -0.0008(14) -0.0076(15) C44 0.023(2) 0.0110(19) 0.015(2) -0.0040(15) -0.0008(17) -0.0040(16) C17 0.0191(19) 0.022(2) 0.0188(19) -0.0037(15) -0.0047(15) -0.0027(16) C28 0.023(2) 0.016(2) 0.017(2) -0.0033(16) 0.0005(17) -0.0133(17) C22 0.024(2) 0.014(2) 0.0138(19) -0.0041(15) -0.0040(16) -0.0052(16) C19 0.023(2) 0.018(2) 0.027(2) -0.0107(18) 0.0091(19) -0.0080(18) C42 0.0166(19) 0.0102(18) 0.0131(18) -0.0042(14) 0.0006(15) -0.0067(15) C46 0.020(2) 0.0109(18) 0.016(2) -0.0034(15) -0.0035(16) -0.0032(15) C43 0.019(2) 0.0125(19) 0.018(2) -0.0040(15) -0.0037(16) -0.0068(16) C39 0.0178(18) 0.0176(18) 0.0168(18) -0.0013(14) -0.0046(14) -0.0050(15) C10 0.0163(18) 0.0141(18) 0.0149(18) -0.0031(14) -0.0003(14) -0.0041(14) C16 0.021(2) 0.040(3) 0.025(2) 0.000(2) -0.0018(19) -0.010(2) C29 0.020(2) 0.017(2) 0.015(2) 0.0002(15) -0.0044(17) -0.0068(17) C48 0.030(2) 0.021(2) 0.031(2) 0.0110(17) -0.0017(19) -0.0105(18) C40 0.015(2) 0.034(3) 0.026(2) -0.0029(19) -0.0015(18) -0.0088(19) C49 0.024(2) 0.0138(18) 0.0157(18) -0.0065(14) 0.0049(15) -0.0098(16) C54 0.046(4) 0.052(4) 0.076(5) -0.056(4) -0.019(3) 0.015(3) C50 0.036(3) 0.025(2) 0.052(3) -0.028(2) 0.010(2) -0.011(2) C18 0.034(3) 0.040(3) 0.025(2) -0.013(2) -0.011(2) 0.001(2) C41 0.0199(19) 0.022(2) 0.0168(18) -0.0011(15) -0.0027(15) -0.0047(15) C51 0.067(4) 0.017(2) 0.027(2) 0.0069(18) -0.009(2) -0.014(2) C52 0.037(3) 0.0140(18) 0.0158(19) -0.0036(14) 0.0007(17) -0.0113(17) C2 0.036(3) 0.051(4) 0.033(3) -0.017(3) 0.009(3) -0.014(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 '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' H H 0.0000 0.0000 '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 _geom_angle_publ_flag N2 Mn N6 85.31(14) 1_546 1_545 ? N2 Mn N3 179.55(19) 1_546 . ? N6 Mn N3 94.94(14) 1_545 . ? N2 Mn N1 95.14(14) 1_546 1_556 ? N6 Mn N1 179.14(17) 1_545 1_556 ? N3 Mn N1 84.61(14) . 1_556 ? N2 Mn Cl1 89.59(11) 1_546 . ? N6 Mn Cl1 89.39(10) 1_545 . ? N3 Mn Cl1 90.04(11) . . ? N1 Mn Cl1 91.34(10) 1_556 . ? N2 Mn Cl2 90.18(11) 1_546 . ? N6 Mn Cl2 90.36(10) 1_545 . ? N3 Mn Cl2 90.19(11) . . ? N1 Mn Cl2 88.91(10) 1_556 . ? Cl1 Mn Cl2 179.68(5) . . ? C23 N1 C22 117.5(4) . . ? C23 N1 Mn 122.9(3) . 1_554 ? C22 N1 Mn 119.4(3) . 1_554 ? C7 N2 C3 117.0(4) . . ? C7 N2 Mn 119.8(3) . 1_564 ? C3 N2 Mn 121.2(3) . 1_564 ? C25 N3 C29 117.0(4) . . ? C25 N3 Mn 120.3(3) . . ? C29 N3 Mn 120.7(3) . . ? C36 N4 C35 112.5(3) . . ? C36 N4 C37 107.9(3) . . ? C35 N4 C37 107.6(4) . . ? C33 N5 C32 111.1(3) . . ? C33 N5 C39 113.6(3) . . ? C32 N5 C39 115.5(3) . . ? C44 N6 C45 117.4(4) . . ? C44 N6 Mn 121.4(3) . 1_565 ? C45 N6 Mn 121.1(3) . 1_565 ? C10 N7 C12 110.7(3) . . ? C10 N7 C17 111.6(3) . . ? C12 N7 C17 114.8(3) . . ? C19 N8 C8 108.6(3) . . ? C19 N8 C14 108.2(4) . . ? C8 N8 C14 111.9(3) . . ? O8 C47 O9 123.7(4) . . ? O8 C47 C34 124.8(4) . . ? O9 C47 C34 111.4(4) . . ? C53 O3 C54 113.2(4) . . ? C47 O9 C48 114.8(3) . . ? N2 C3 C4 123.6(4) . . ? Cl7 C1 Cl3 112.5(4) . . ? Cl7 C1 Cl6 112.0(4) . . ? Cl3 C1 Cl6 107.1(4) . . ? C22 C21 C20 119.4(4) . . ? N8 C14 C20 109.9(3) . . ? N8 C14 C13 112.0(3) . . ? C20 C14 C13 110.1(3) . . ? C38 C31 C49 108.0(3) . . ? C38 C31 C32 106.1(3) . . ? C49 C31 C32 113.7(4) . . ? C38 C31 C36 106.0(3) . . ? C49 C31 C36 106.1(3) . . ? C32 C31 C36 116.4(3) . . ? C52 O4 C51 113.9(4) . . ? C49 O5 C50 114.8(4) . . ? N4 C35 C42 109.5(3) . . ? N4 C35 C34 114.2(4) . . ? C42 C35 C34 110.6(3) . . ? C3 C4 C5 118.4(4) . . ? N5 C32 C31 111.1(3) . . ? N4 C36 C27 110.9(3) . . ? N4 C36 C31 111.7(3) . . ? C27 C36 C31 110.6(3) . . ? O2 C53 O3 123.7(4) . . ? O2 C53 C9 123.0(4) . . ? O3 C53 C9 113.3(4) . . ? C28 C27 C26 118.0(4) . . ? C28 C27 C36 123.3(4) . . ? C26 C27 C36 118.6(4) . . ? C38 C34 C47 106.7(3) . . ? C38 C34 C33 104.0(3) . . ? C47 C34 C33 113.6(3) . . ? C38 C34 C35 108.6(3) . . ? C47 C34 C35 108.2(3) . . ? C33 C34 C35 115.4(3) . . ? O1 C15 C13 124.9(4) . . ? O1 C15 C9 124.2(4) . . ? C13 C15 C9 110.5(3) . . ? C25 C26 C27 118.4(4) . . ? N8 C8 C5 110.0(3) . . ? N8 C8 C9 114.3(3) . . ? C5 C8 C9 109.9(4) . . ? N6 C45 C46 123.1(4) . . ? O7 C38 C31 125.4(4) . . ? O7 C38 C34 123.7(4) . . ? C31 C38 C34 110.8(3) . . ? N3 C25 C26 124.2(4) . . ? C6 C5 C4 118.1(4) . . ? C6 C5 C8 119.8(4) . . ? C4 C5 C8 122.1(4) . . ? C21 C20 C24 117.5(4) . . ? C21 C20 C14 122.1(4) . . ? C24 C20 C14 120.3(4) . . ? C23 C24 C20 119.6(4) . . ? N2 C7 C6 123.7(4) . . ? C5 C6 C7 119.1(4) . . ? C15 C13 C52 109.9(4) . . ? C15 C13 C12 105.2(4) . . ? C52 C13 C12 108.0(4) . . ? C15 C13 C14 106.9(3) . . ? C52 C13 C14 109.0(4) . . ? C12 C13 C14 117.6(3) . . ? N1 C23 C24 123.0(4) . . ? N5 C33 C34 109.4(3) . . ? C15 C9 C53 108.5(4) . . ? C15 C9 C10 104.8(4) . . ? C53 C9 C10 113.2(4) . . ? C15 C9 C8 108.2(4) . . ? C53 C9 C8 106.6(4) . . ? C10 C9 C8 115.3(4) . . ? N7 C12 C13 111.3(3) . . ? N6 C44 C43 123.2(4) . . ? N7 C17 C18 110.7(4) . . ? N7 C17 C16 114.0(4) . . ? C18 C17 C16 111.0(4) . . ? C27 C28 C29 119.7(4) . . ? N1 C22 C21 122.9(4) . . ? C43 C42 C46 118.0(4) . . ? C43 C42 C35 120.0(4) . . ? C46 C42 C35 122.0(4) . . ? C45 C46 C42 119.0(4) . . ? C42 C43 C44 119.1(4) . . ? N5 C39 C41 110.1(3) . . ? N5 C39 C40 114.9(4) . . ? C41 C39 C40 110.6(4) . . ? N7 C10 C9 110.9(4) . . ? N3 C29 C28 122.6(4) . . ? O6 C49 O5 124.6(4) . . ? O6 C49 C31 123.2(4) . . ? O5 C49 C31 112.2(4) . . ? O10 C52 O4 124.1(4) . . ? O10 C52 C13 124.1(5) . . ? O4 C52 C13 111.8(4) . . ? Cl4 C2 Cl8 111.4(4) . . ? Cl4 C2 Cl5 111.6(4) . . ? Cl8 C2 Cl5 107.9(4) . . ? 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 Mn N2 2.305(4) 1_546 ? Mn N6 2.319(4) 1_545 ? Mn N3 2.320(4) . ? Mn N1 2.320(4) 1_556 ? Mn Cl1 2.4677(16) . ? Mn Cl2 2.4829(17) . ? Cl3 C1 1.759(8) . ? Cl4 C2 1.729(7) . ? Cl5 C2 1.768(7) . ? Cl6 C1 1.763(7) . ? Cl7 C1 1.721(7) . ? Cl8 C2 1.758(7) . ? N1 C23 1.342(6) . ? N1 C22 1.349(6) . ? N2 C7 1.339(6) . ? N2 C3 1.343(6) . ? N3 C25 1.340(6) . ? N3 C29 1.346(6) . ? N4 C36 1.472(5) . ? N4 C35 1.478(6) . ? N4 C37 1.487(6) . ? N5 C33 1.452(5) . ? N5 C32 1.463(5) . ? N5 C39 1.471(5) . ? N6 C44 1.339(6) . ? N6 C45 1.345(6) . ? N7 C10 1.445(5) . ? N7 C12 1.463(6) . ? N7 C17 1.484(5) . ? N8 C19 1.466(6) . ? N8 C8 1.476(5) . ? N8 C14 1.476(5) . ? O6 C49 1.197(6) . ? O8 C47 1.191(6) . ? O1 C15 1.216(5) . ? C47 O9 1.338(5) . ? C47 C34 1.535(6) . ? O3 C53 1.324(6) . ? O3 C54 1.469(6) . ? O9 C48 1.448(5) . ? O7 C38 1.202(5) . ? C3 C4 1.390(6) . ? C21 C22 1.391(6) . ? C21 C20 1.393(6) . ? C14 C20 1.513(6) . ? C14 C13 1.569(6) . ? C31 C38 1.522(6) . ? C31 C49 1.537(6) . ? C31 C32 1.554(6) . ? C31 C36 1.575(6) . ? O4 C52 1.350(6) . ? O4 C51 1.444(6) . ? O5 C49 1.330(6) . ? O5 C50 1.446(6) . ? C35 C42 1.518(6) . ? C35 C34 1.570(6) . ? C4 C5 1.405(6) . ? O10 C52 1.198(6) . ? C36 C27 1.522(6) . ? C53 O2 1.200(6) . ? C53 C9 1.525(6) . ? C27 C28 1.383(6) . ? C27 C26 1.396(6) . ? C34 C38 1.527(6) . ? C34 C33 1.544(6) . ? C15 C13 1.509(6) . ? C15 C9 1.521(6) . ? C26 C25 1.385(6) . ? C8 C5 1.513(6) . ? C8 C9 1.558(6) . ? C45 C46 1.388(6) . ? C5 C6 1.385(6) . ? C20 C24 1.396(6) . ? C24 C23 1.389(6) . ? C7 C6 1.387(6) . ? C13 C52 1.526(6) . ? C13 C12 1.554(6) . ? C9 C10 1.549(6) . ? C44 C43 1.392(6) . ? C17 C18 1.520(6) . ? C17 C16 1.523(7) . ? C28 C29 1.394(6) . ? C42 C43 1.387(6) . ? C42 C46 1.395(6) . ? C39 C41 1.525(6) . ? C39 C40 1.526(7) . ?