#------------------------------------------------------------------------------ #$Date: 2020-09-01 04:41:55 +0300 (Tue, 01 Sep 2020) $ #$Revision: 255771 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/53/7705324.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_7705324 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 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2017/1 _audit_update_record ; 2020-07-15 deposited with the CCDC. 2020-08-31 downloaded from the CCDC. ; _cell_angle_alpha 77.75(3) _cell_angle_beta 85.95(3) _cell_angle_gamma 69.83(3) _cell_formula_units_Z 1 _cell_length_a 9.967(2) _cell_length_b 12.819(3) _cell_length_c 13.148(3) _cell_measurement_reflns_used 7868 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 31.172 _cell_measurement_theta_min 2.177 _cell_volume 1541.0(7) _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.895 _diffrn_measurement_device_type 'Bruker APEX II CCD diffractometer' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0200 _diffrn_reflns_av_unetI/netI 0.0287 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.895 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 16242 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.895 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.550 _diffrn_reflns_theta_min 1.585 _exptl_absorpt_coefficient_mu 0.621 _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.398 _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 0.949 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.068 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 471 _refine_ls_number_reflns 9229 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.072 _refine_ls_R_factor_all 0.0809 _refine_ls_R_factor_gt 0.0591 _refine_ls_shift/su_max 0.045 _refine_ls_shift/su_mean 0.006 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0888P)^2^+0.7369P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1608 _refine_ls_wR_factor_ref 0.1765 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6804 _reflns_number_total 9229 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02734k2.cif _cod_data_source_block 2TCM_RT _cod_original_cell_volume 1540.9(6) _cod_database_code 7705324 _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 0.958 _shelx_estimated_absorpt_t_max 0.982 _shelx_res_file ; TITL tcmny in P -1 shelx.res created by SHELXL-2017/1 at 16:38:39 on 08-Jul-2020 CELL 0.71073 9.9668 12.8189 13.1477 77.751 85.952 69.835 ZERR 1.00 0.0020 0.0026 0.0026 0.030 0.030 0.030 LATT 1 SFAC C H N O CL MN UNIT 52 62 8 10 8 1 MERG 2 FMAP 2 PLAN 20 ACTA L.S. 4 SIZE 0.07 0.05 0.03 TEMP 25.00 WGHT 0.088800 0.736900 FVAR 0.42078 MN1 6 0.000000 0.000000 0.000000 10.50000 0.04028 0.01958 = 0.02885 -0.00567 0.00098 -0.01287 O5 4 -0.080715 0.199406 0.490903 11.00000 0.13257 0.05171 = 0.06836 0.00555 0.00949 -0.04492 N2 3 -0.070446 0.470273 0.250562 11.00000 0.04569 0.02450 = 0.03221 -0.01015 0.00918 -0.01837 N3 3 -0.068531 -0.134301 0.119553 11.00000 0.05406 0.02852 = 0.03320 -0.00052 -0.00115 -0.02154 C2 1 -0.237725 0.575657 0.377620 11.00000 0.04435 0.02660 = 0.02570 -0.00516 0.00105 -0.01476 N4 3 -0.031785 0.124277 0.112833 11.00000 0.04836 0.02507 = 0.03207 -0.00945 -0.00048 -0.01294 O1 4 -0.239216 0.443842 0.538377 11.00000 0.11559 0.04322 = 0.02784 -0.00635 0.01539 -0.03124 C24 1 -0.062315 0.279540 0.241279 11.00000 0.04809 0.02411 = 0.03038 -0.00802 0.00164 -0.01666 N1 3 -0.374675 0.531988 0.251932 11.00000 0.04642 0.09527 = 0.03607 -0.02350 0.00307 -0.03457 O3 4 -0.359543 0.738758 0.447725 11.00000 0.07204 0.07446 = 0.11990 -0.06922 -0.00334 0.00456 O2 4 -0.138526 0.642014 0.501791 11.00000 0.08248 0.05941 = 0.05697 -0.03188 -0.01328 -0.01905 C6 1 -0.078115 0.361997 0.312187 11.00000 0.05045 0.02397 = 0.02916 -0.00784 0.00145 -0.01788 C19 1 -0.092630 -0.332483 0.245940 11.00000 0.04122 0.02304 = 0.02840 -0.00443 0.00241 -0.01501 C20 1 -0.161306 -0.287257 0.150208 11.00000 0.05263 0.03983 = 0.03223 -0.00223 -0.00278 -0.02927 C26 1 0.046832 0.096118 0.198987 11.00000 0.05600 0.02214 = 0.03730 -0.00660 -0.00585 -0.01076 C28 1 -0.139125 0.310785 0.149432 11.00000 0.04949 0.02467 = 0.03771 -0.00958 -0.00343 -0.00550 C7 1 -0.095786 0.557067 0.314178 11.00000 0.04313 0.02253 = 0.02776 -0.00491 0.00129 -0.01590 C5 1 -0.217152 0.375869 0.378738 11.00000 0.06763 0.03704 = 0.03951 -0.01567 0.01696 -0.03443 C9 1 -0.238187 0.654745 0.450155 11.00000 0.05949 0.03090 = 0.03302 -0.01084 0.00760 -0.01731 C3 1 -0.376529 0.614259 0.313326 11.00000 0.04250 0.05189 = 0.03488 -0.00279 0.00133 -0.01822 C23 1 -0.015023 -0.273786 0.277655 11.00000 0.06206 0.03500 = 0.03235 0.00169 -0.01060 -0.02893 C25 1 0.033064 0.169598 0.265748 11.00000 0.05709 0.02582 = 0.03510 -0.00595 -0.01013 -0.01260 C18 1 0.073546 0.448666 0.205803 11.00000 0.05367 0.03794 = 0.06351 -0.01931 0.02253 -0.02235 C8 1 -0.195006 0.259784 0.455105 11.00000 0.15491 0.04733 = 0.08599 -0.03477 0.07314 -0.06538 C22 1 -0.005072 -0.177238 0.212031 11.00000 0.07293 0.03779 = 0.03952 -0.00073 -0.00954 -0.03664 C27 1 -0.123166 0.230902 0.089078 11.00000 0.05057 0.02980 = 0.03340 -0.01110 -0.00729 -0.00806 C21 1 -0.148834 -0.187932 0.090937 11.00000 0.05131 0.04062 = 0.03183 0.00265 -0.00508 -0.02541 C1 1 -0.228952 0.461860 0.445152 11.00000 0.05625 0.03227 = 0.02825 -0.00728 0.00708 -0.02133 C4 1 -0.358613 0.422680 0.317768 11.00000 0.05982 0.08143 = 0.06426 -0.04316 0.02363 -0.04850 C11 1 -0.364888 0.813806 0.518626 11.00000 0.13843 0.12763 = 0.21767 -0.14579 0.00243 -0.00122 AFIX 33 H11A 2 -0.456312 0.873105 0.512822 11.00000 -1.50000 H11B 2 -0.350959 0.771090 0.588798 11.00000 -1.50000 H11C 2 -0.290904 0.846524 0.500837 11.00000 -1.50000 AFIX 0 O4 4 -0.312463 0.239677 0.476445 11.00000 0.11444 0.06641 = 0.26441 0.03275 0.06505 -0.04899 C29 1 -0.493939 0.569532 0.177526 11.00000 0.05881 0.24021 = 0.04385 -0.01899 -0.00415 -0.07580 AFIX 13 H29 2 -0.495808 0.647990 0.155309 11.00000 -1.20000 AFIX 0 C30 1 -0.640033 0.596937 0.221663 11.00000 0.05005 0.12707 = 0.07117 -0.00441 -0.00187 -0.03673 AFIX 33 H30A 2 -0.638941 0.612807 0.289692 11.00000 -1.50000 H30B 2 -0.703574 0.662198 0.177246 11.00000 -1.50000 H30C 2 -0.672250 0.533565 0.226653 11.00000 -1.50000 AFIX 0 C100 1 0.435543 0.909718 0.824381 11.00000 0.10315 0.11976 = 0.09292 -0.04272 0.03863 -0.05082 AFIX 13 H100 2 0.377623 0.905121 0.887497 11.00000 -1.20000 AFIX 0 PART 1 C10A 1 -0.105668 0.103159 0.548697 10.30000 0.13673 0.02893 = 0.04721 0.01798 -0.01780 -0.03347 AFIX 33 H10A 2 -0.017952 0.049983 0.580270 10.30000 -1.50000 H10B 2 -0.174690 0.124475 0.601944 10.30000 -1.50000 H10C 2 -0.141524 0.068827 0.503622 10.30000 -1.50000 AFIX 0 PART 2 C10 1 -0.283840 0.140715 0.578741 10.70000 0.11568 0.09504 = 0.14118 0.06236 -0.00911 -0.06054 AFIX 33 H10D 2 -0.369697 0.123211 0.597244 10.70000 -1.50000 H10F 2 -0.209188 0.074228 0.565022 10.70000 -1.50000 H10E 2 -0.255530 0.165562 0.635092 10.70000 -1.50000 AFIX 0 PART 0 CL1 5 -0.250337 0.095751 -0.060427 11.00000 0.04155 0.03869 = 0.05045 -0.01098 -0.00497 -0.00923 PART 1 CL2 5 0.529149 0.990898 0.839215 10.70000 0.14123 0.18386 = 0.19821 -0.08692 0.05049 -0.10991 CL3 5 0.329860 0.915992 0.725792 10.70000 0.17999 0.29073 = 0.16199 -0.11112 0.07443 -0.15244 CL4 5 0.538408 0.770974 0.819781 10.70000 0.19796 0.11329 = 0.15548 -0.03011 0.02685 -0.04371 PART 2 CL4A 5 0.612845 0.809026 0.853874 10.30000 0.13331 0.16587 = 0.20839 -0.03056 -0.00285 0.02766 CL3A 5 0.337368 0.986331 0.709025 10.30000 0.09202 0.18854 = 0.09718 -0.03976 -0.01501 -0.01003 CL2A 5 0.475164 1.035360 0.772454 10.30000 0.20086 0.14235 = 0.13869 -0.01309 -0.00077 -0.10957 PART 1 C31 1 -0.481738 0.545350 0.080737 10.30000 0.05412 0.06164 = 0.05513 -0.02990 -0.01673 -0.01743 AFIX 33 H31A 2 -0.573152 0.578595 0.046640 10.30000 -1.50000 H31B 2 -0.414332 0.575780 0.040952 10.30000 -1.50000 H31C 2 -0.449118 0.464606 0.086301 10.30000 -1.50000 AFIX 0 PART 2 C31A 1 -0.462809 0.622141 0.082390 10.70000 0.06079 0.12605 = 0.04590 0.01596 -0.01264 -0.01247 AFIX 33 H31D 2 -0.543475 0.644910 0.036882 10.70000 -1.50000 H31E 2 -0.441304 0.687814 0.089176 10.70000 -1.50000 H31F 2 -0.381659 0.570859 0.053914 10.70000 -1.50000 AFIX 0 PART 0 H25 2 0.090455 0.142676 0.327824 11.00000 0.03968 H27 2 -0.173809 0.250649 0.028764 11.00000 0.03818 H26 2 0.121228 0.017442 0.212489 11.00000 0.03964 H28 2 -0.206581 0.386664 0.130252 11.00000 0.04737 H6 2 0.000390 0.327246 0.363896 11.00000 0.02574 H23 2 0.035044 -0.300241 0.339882 11.00000 0.04884 H21 2 -0.202145 -0.152506 0.023206 11.00000 0.04733 H22 2 0.054753 -0.135934 0.230937 11.00000 0.05429 H20 2 -0.220724 -0.321333 0.124850 11.00000 0.05461 H31 2 -0.385349 0.688327 0.267827 11.00000 0.04310 H30 2 -0.456549 0.623730 0.364612 11.00000 0.04836 H182 2 0.082861 0.512501 0.164674 11.00000 0.05120 H41 2 -0.361750 0.368608 0.275813 11.00000 0.08431 H183 2 0.094693 0.394344 0.167258 11.00000 0.06096 H42 2 -0.427079 0.422368 0.372649 11.00000 0.06297 H181 2 0.146198 0.418767 0.258185 11.00000 0.06451 H71 2 -0.019886 0.532444 0.367936 11.00000 0.02907 HKLF 4 REM tcmny in P -1 REM R1 = 0.0591 for 6804 Fo > 4sig(Fo) and 0.0809 for all 9229 data REM 471 parameters refined using 0 restraints END WGHT 0.0885 0.7890 REM Highest difference peak 0.949, deepest hole -0.673, 1-sigma level 0.068 Q1 1 -0.2990 0.2476 0.5031 11.00000 0.05 0.95 Q2 1 -0.2713 0.2837 0.4335 11.00000 0.05 0.66 Q3 1 -0.3611 0.2555 0.4267 11.00000 0.05 0.63 Q4 1 -0.1776 0.2500 0.4795 11.00000 0.05 0.60 Q5 1 -0.5062 0.6188 0.1659 11.00000 0.05 0.56 Q6 1 0.1018 -0.0270 0.0024 11.00000 0.05 0.53 Q7 1 0.4210 0.8205 0.7667 11.00000 0.05 0.52 Q8 1 -0.4731 0.5386 0.1827 11.00000 0.05 0.48 Q9 1 0.2874 0.9187 0.7002 11.00000 0.05 0.44 Q10 1 -0.3586 0.6874 0.4900 11.00000 0.05 0.44 Q11 1 -0.4788 0.4693 0.1531 11.00000 0.05 0.42 Q12 1 -0.3364 0.5054 0.2421 11.00000 0.05 0.39 Q13 1 -0.0221 0.0465 0.0253 11.00000 0.05 0.38 Q14 1 -0.3787 0.5774 0.2571 11.00000 0.05 0.37 Q15 1 -0.3018 0.5904 0.3504 11.00000 0.05 0.36 Q16 1 -0.1686 0.6896 0.4590 11.00000 0.05 0.36 Q17 1 -0.1247 0.2682 0.1216 11.00000 0.05 0.35 Q18 1 -0.0225 0.0883 0.0704 11.00000 0.05 0.34 Q19 1 0.4010 1.0525 0.7293 11.00000 0.05 0.34 Q20 1 -0.2131 0.4144 0.4079 11.00000 0.05 0.33 ; _shelx_res_checksum 45208 loop_ _space_group_symop_operation_xyz 'x, y, z' '-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 Mn1 Mn 0.000000 0.000000 0.000000 0.02876(12) Uani 1 2 d S . P . . O5 O -0.0807(4) 0.1994(2) 0.4909(2) 0.0838(8) Uani 1 1 d . . . . . N2 N -0.07045(19) 0.47027(13) 0.25056(13) 0.0322(3) Uani 1 1 d . . . . . N3 N -0.0685(2) -0.13430(14) 0.11955(14) 0.0374(4) Uani 1 1 d . . . . . C2 C -0.2377(2) 0.57566(16) 0.37762(14) 0.0315(4) Uani 1 1 d . . . . . N4 N -0.0318(2) 0.12428(14) 0.11283(13) 0.0344(4) Uani 1 1 d . . . . . O1 O -0.2392(3) 0.44384(15) 0.53838(13) 0.0620(6) Uani 1 1 d . . . . . C24 C -0.0623(2) 0.27954(16) 0.24128(15) 0.0327(4) Uani 1 1 d . . . . . N1 N -0.3747(2) 0.5320(2) 0.25193(16) 0.0550(6) Uani 1 1 d . . . . . O3 O -0.3595(3) 0.7388(2) 0.4477(2) 0.0886(8) Uani 1 1 d . . . . . O2 O -0.1385(3) 0.64201(18) 0.50179(16) 0.0637(5) Uani 1 1 d . . . . . C6 C -0.0781(2) 0.36200(16) 0.31219(15) 0.0328(4) Uani 1 1 d . . . . . C19 C -0.0926(2) -0.33248(15) 0.24594(14) 0.0300(4) Uani 1 1 d . . . . . C20 C -0.1613(3) -0.28726(19) 0.15021(16) 0.0386(5) Uani 1 1 d . . . . . C26 C 0.0468(3) 0.09612(17) 0.19899(17) 0.0387(5) Uani 1 1 d . . . . . C28 C -0.1391(3) 0.31078(17) 0.14943(17) 0.0385(5) Uani 1 1 d . . . . . C7 C -0.0958(2) 0.55707(15) 0.31418(15) 0.0299(4) Uani 1 1 d . . . . . C5 C -0.2172(3) 0.37587(19) 0.37874(18) 0.0432(5) Uani 1 1 d . . . . . C9 C -0.2382(3) 0.65475(18) 0.45016(17) 0.0403(5) Uani 1 1 d . . . . . C3 C -0.3765(3) 0.6143(2) 0.31333(18) 0.0435(5) Uani 1 1 d . . . . . C23 C -0.0150(3) -0.27379(18) 0.27765(17) 0.0406(5) Uani 1 1 d . . . . . C25 C 0.0331(3) 0.16960(17) 0.26575(17) 0.0392(5) Uani 1 1 d . . . . . C18 C 0.0735(3) 0.4487(2) 0.2058(2) 0.0496(6) Uani 1 1 d . . . . . C8 C -0.1950(6) 0.2598(3) 0.4551(3) 0.0881(15) Uani 1 1 d . . . . . C22 C -0.0051(3) -0.17724(19) 0.21203(18) 0.0459(6) Uani 1 1 d . . . . . C27 C -0.1232(3) 0.23090(17) 0.08908(17) 0.0383(5) Uani 1 1 d . . . . . C21 C -0.1488(3) -0.18793(19) 0.09094(17) 0.0399(5) Uani 1 1 d . . . . . C1 C -0.2290(3) 0.46186(18) 0.44515(16) 0.0374(4) Uani 1 1 d . . . . . C4 C -0.3586(3) 0.4227(3) 0.3178(2) 0.0587(8) Uani 1 1 d . . . . . C11 C -0.3649(7) 0.8138(5) 0.5186(6) 0.156(3) Uani 1 1 d . . . . . H11A H -0.456312 0.873105 0.512822 0.233 Uiso 1 1 calc R U . . . H11B H -0.350959 0.771090 0.588798 0.233 Uiso 1 1 calc R U . . . H11C H -0.290904 0.846524 0.500837 0.233 Uiso 1 1 calc R U . . . O4 O -0.3125(4) 0.2397(3) 0.4764(4) 0.157(2) Uani 1 1 d . . . . . C29 C -0.4939(4) 0.5695(6) 0.1775(3) 0.1088(19) Uani 1 1 d . . . . . H29 H -0.495808 0.647990 0.155309 0.131 Uiso 1 1 calc R U . A 1 C30 C -0.6400(4) 0.5969(4) 0.2217(3) 0.0833(11) Uani 1 1 d . . . . . H30A H -0.638941 0.612807 0.289692 0.125 Uiso 1 1 calc R U . . . H30B H -0.703574 0.662198 0.177246 0.125 Uiso 1 1 calc R U . . . H30C H -0.672250 0.533565 0.226653 0.125 Uiso 1 1 calc R U . . . C100 C 0.4355(5) 0.9097(4) 0.8244(4) 0.1004(14) Uani 1 1 d . . . . . H100 H 0.377623 0.905121 0.887497 0.120 Uiso 1 1 calc R U . B 1 C10A C -0.1057(15) 0.1032(7) 0.5487(8) 0.073(3) Uani 0.3 1 d . . P C 1 H10A H -0.017952 0.049983 0.580270 0.109 Uiso 0.3 1 calc R U P C 1 H10B H -0.174690 0.124475 0.601944 0.109 Uiso 0.3 1 calc R U P C 1 H10C H -0.141524 0.068827 0.503622 0.109 Uiso 0.3 1 calc R U P C 1 C10 C -0.2838(8) 0.1407(6) 0.5787(6) 0.124(3) Uani 0.7 1 d . . P D 2 H10D H -0.369697 0.123211 0.597244 0.186 Uiso 0.7 1 calc R U P D 2 H10F H -0.209188 0.074228 0.565022 0.186 Uiso 0.7 1 calc R U P D 2 H10E H -0.255530 0.165562 0.635092 0.186 Uiso 0.7 1 calc R U P D 2 Cl1 Cl -0.25034(6) 0.09575(5) -0.06043(5) 0.04414(15) Uani 1 1 d . . . . . Cl2 Cl 0.5291(3) 0.9909(3) 0.8392(3) 0.1547(12) Uani 0.7 1 d . . P E 1 Cl3 Cl 0.3299(5) 0.9160(4) 0.7258(3) 0.185(2) Uani 0.7 1 d . . P E 1 Cl4 Cl 0.5384(4) 0.7710(3) 0.8198(3) 0.1588(12) Uani 0.7 1 d . . P E 1 Cl4A Cl 0.6128(9) 0.8090(8) 0.8539(8) 0.191(4) Uani 0.3 1 d . . P E 2 Cl3A Cl 0.3374(7) 0.9863(7) 0.7090(5) 0.133(2) Uani 0.3 1 d . . P E 2 Cl2A Cl 0.4752(10) 1.0354(7) 0.7725(6) 0.149(3) Uani 0.3 1 d . . P E 2 C31 C -0.4817(10) 0.5453(9) 0.0807(8) 0.054(2) Uani 0.3 1 d . . P F 1 H31A H -0.573152 0.578595 0.046640 0.081 Uiso 0.3 1 calc R U P F 1 H31B H -0.414332 0.575780 0.040952 0.081 Uiso 0.3 1 calc R U P F 1 H31C H -0.449118 0.464606 0.086301 0.081 Uiso 0.3 1 calc R U P F 1 C31A C -0.4628(5) 0.6221(6) 0.0824(4) 0.0872(19) Uani 0.7 1 d . . P F 2 H31D H -0.543475 0.644910 0.036882 0.131 Uiso 0.7 1 calc R U P F 2 H31E H -0.441304 0.687814 0.089176 0.131 Uiso 0.7 1 calc R U P F 2 H31F H -0.381659 0.570859 0.053914 0.131 Uiso 0.7 1 calc R U P F 2 H25 H 0.090(3) 0.143(2) 0.328(2) 0.040(6) Uiso 1 1 d . . . . . H27 H -0.174(3) 0.251(2) 0.029(2) 0.038(6) Uiso 1 1 d . . . . . H26 H 0.121(3) 0.017(2) 0.212(2) 0.040(6) Uiso 1 1 d . . . . . H28 H -0.207(3) 0.387(2) 0.130(2) 0.047(7) Uiso 1 1 d . . . . . H6 H 0.000(2) 0.3272(19) 0.3639(18) 0.026(5) Uiso 1 1 d . . . . . H23 H 0.035(3) -0.300(2) 0.340(2) 0.049(7) Uiso 1 1 d . . . . . H21 H -0.202(3) -0.153(2) 0.023(2) 0.047(7) Uiso 1 1 d . . . . . H22 H 0.055(3) -0.136(3) 0.231(2) 0.054(8) Uiso 1 1 d . . . . . H20 H -0.221(3) -0.321(3) 0.125(2) 0.055(8) Uiso 1 1 d . . . . . H31 H -0.385(3) 0.688(2) 0.268(2) 0.043(7) Uiso 1 1 d . . . . . H30 H -0.457(3) 0.624(2) 0.365(2) 0.048(7) Uiso 1 1 d . . . . . H182 H 0.083(3) 0.513(3) 0.165(2) 0.051(8) Uiso 1 1 d . . . . . H41 H -0.362(4) 0.369(3) 0.276(3) 0.084(11) Uiso 1 1 d . . . . . H183 H 0.095(3) 0.394(3) 0.167(3) 0.061(9) Uiso 1 1 d . . . . . H42 H -0.427(4) 0.422(3) 0.373(3) 0.063(9) Uiso 1 1 d . . . . . H181 H 0.146(4) 0.419(3) 0.258(3) 0.065(10) Uiso 1 1 d . . . . . H71 H -0.020(2) 0.5324(19) 0.3679(18) 0.029(5) Uiso 1 1 d . . . . . 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 0.0403(2) 0.01958(18) 0.0289(2) -0.00567(14) 0.00098(15) -0.01287(15) O5 0.133(2) 0.0517(13) 0.0684(15) 0.0055(11) 0.0095(15) -0.0449(15) N2 0.0457(9) 0.0245(7) 0.0322(8) -0.0101(6) 0.0092(7) -0.0184(7) N3 0.0541(11) 0.0285(8) 0.0332(8) -0.0005(6) -0.0012(7) -0.0215(7) C2 0.0444(11) 0.0266(8) 0.0257(8) -0.0052(7) 0.0011(7) -0.0148(8) N4 0.0484(10) 0.0251(7) 0.0321(8) -0.0094(6) -0.0005(7) -0.0129(7) O1 0.1156(17) 0.0432(9) 0.0278(8) -0.0064(7) 0.0154(9) -0.0312(10) C24 0.0481(11) 0.0241(8) 0.0304(9) -0.0080(7) 0.0016(8) -0.0167(8) N1 0.0464(11) 0.0953(18) 0.0361(10) -0.0235(11) 0.0031(8) -0.0346(12) O3 0.0720(15) 0.0745(15) 0.120(2) -0.0692(16) -0.0033(14) 0.0046(12) O2 0.0825(14) 0.0594(12) 0.0570(11) -0.0319(9) -0.0133(10) -0.0190(10) C6 0.0505(12) 0.0240(8) 0.0292(9) -0.0078(7) 0.0015(8) -0.0179(8) C19 0.0412(10) 0.0230(8) 0.0284(9) -0.0044(6) 0.0024(7) -0.0150(7) C20 0.0526(13) 0.0398(11) 0.0322(10) -0.0022(8) -0.0028(9) -0.0293(10) C26 0.0560(13) 0.0221(8) 0.0373(10) -0.0066(7) -0.0058(9) -0.0108(8) C28 0.0495(12) 0.0247(9) 0.0377(10) -0.0096(8) -0.0034(9) -0.0055(8) C7 0.0431(10) 0.0225(8) 0.0278(8) -0.0049(6) 0.0013(7) -0.0159(7) C5 0.0676(15) 0.0370(11) 0.0395(11) -0.0157(9) 0.0170(10) -0.0344(11) C9 0.0595(14) 0.0309(10) 0.0330(10) -0.0108(8) 0.0076(9) -0.0173(9) C3 0.0425(12) 0.0519(13) 0.0349(11) -0.0028(9) 0.0013(9) -0.0182(10) C23 0.0621(14) 0.0350(10) 0.0323(10) 0.0017(8) -0.0106(9) -0.0289(10) C25 0.0571(13) 0.0258(9) 0.0351(10) -0.0059(7) -0.0101(9) -0.0126(9) C18 0.0537(15) 0.0379(12) 0.0635(16) -0.0193(12) 0.0225(13) -0.0224(11) C8 0.155(4) 0.0473(17) 0.086(2) -0.0348(17) 0.073(3) -0.065(2) C22 0.0729(16) 0.0378(11) 0.0395(11) -0.0007(9) -0.0095(11) -0.0366(11) C27 0.0506(12) 0.0298(9) 0.0334(10) -0.0111(8) -0.0073(9) -0.0081(9) C21 0.0513(12) 0.0406(11) 0.0318(10) 0.0027(8) -0.0051(9) -0.0254(10) C1 0.0562(13) 0.0323(9) 0.0282(9) -0.0073(7) 0.0071(8) -0.0213(9) C4 0.0598(16) 0.081(2) 0.0643(17) -0.0432(15) 0.0236(13) -0.0485(15) C11 0.138(5) 0.128(4) 0.218(7) -0.146(5) 0.002(4) -0.001(4) O4 0.114(2) 0.0664(17) 0.264(5) 0.033(2) 0.065(3) -0.0490(17) C29 0.0588(19) 0.240(6) 0.0439(16) -0.019(2) -0.0042(14) -0.076(3) C30 0.0500(17) 0.127(3) 0.071(2) -0.004(2) -0.0019(15) -0.0367(19) C100 0.103(3) 0.120(4) 0.093(3) -0.043(3) 0.039(2) -0.051(3) C10A 0.137(10) 0.029(4) 0.047(5) 0.018(3) -0.018(6) -0.033(5) C10 0.116(5) 0.095(4) 0.141(6) 0.062(4) -0.009(4) -0.061(4) Cl1 0.0415(3) 0.0387(3) 0.0505(3) -0.0110(2) -0.0050(2) -0.0092(2) Cl2 0.141(2) 0.184(3) 0.198(3) -0.087(3) 0.050(2) -0.110(2) Cl3 0.180(3) 0.291(5) 0.162(3) -0.111(3) 0.074(2) -0.152(4) Cl4 0.198(3) 0.1133(18) 0.155(3) -0.0301(16) 0.027(2) -0.044(2) Cl4A 0.133(6) 0.166(7) 0.208(8) -0.031(6) -0.003(5) 0.028(5) Cl3A 0.092(3) 0.189(7) 0.097(3) -0.040(4) -0.015(3) -0.010(4) Cl2A 0.201(7) 0.142(5) 0.139(5) -0.013(4) -0.001(5) -0.110(5) C31 0.054(5) 0.062(5) 0.055(5) -0.030(4) -0.017(4) -0.017(4) C31A 0.061(3) 0.126(5) 0.046(2) 0.016(3) -0.013(2) -0.012(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' 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' 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' 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 N3 Mn1 N3 180.0 2 . ? N3 Mn1 N4 95.28(6) 2 2 ? N3 Mn1 N4 84.72(6) . 2 ? N3 Mn1 N4 84.72(6) 2 . ? N3 Mn1 N4 95.28(6) . . ? N4 Mn1 N4 180.0 2 . ? N3 Mn1 Cl1 90.05(6) 2 2 ? N3 Mn1 Cl1 89.95(6) . 2 ? N4 Mn1 Cl1 90.62(5) 2 2 ? N4 Mn1 Cl1 89.38(5) . 2 ? N3 Mn1 Cl1 89.95(6) 2 . ? N3 Mn1 Cl1 90.05(6) . . ? N4 Mn1 Cl1 89.38(5) 2 . ? N4 Mn1 Cl1 90.62(5) . . ? Cl1 Mn1 Cl1 180.0 2 . ? C8 O5 C10A 104.4(6) . . ? C18 N2 C7 108.33(17) . . ? C18 N2 C6 108.02(18) . . ? C7 N2 C6 112.43(15) . . ? C22 N3 C21 116.85(17) . . ? C22 N3 Mn1 120.41(14) . . ? C21 N3 Mn1 121.25(14) . . ? C1 C2 C9 107.51(16) . . ? C1 C2 C3 105.34(18) . . ? C9 C2 C3 113.85(19) . . ? C1 C2 C7 106.97(16) . . ? C9 C2 C7 106.55(17) . . ? C3 C2 C7 116.12(17) . . ? C26 N4 C27 117.12(17) . . ? C26 N4 Mn1 122.08(14) . . ? C27 N4 Mn1 120.60(14) . . ? C28 C24 C25 117.54(18) . . ? C28 C24 C6 121.98(18) . . ? C25 C24 C6 120.47(18) . . ? C4 N1 C3 111.0(2) . . ? C4 N1 C29 112.5(3) . . ? C3 N1 C29 114.8(3) . . ? C9 O3 C11 113.9(3) . . ? N2 C6 C24 109.86(16) . . ? N2 C6 C5 113.39(17) . . ? C24 C6 C5 110.73(17) . . ? C23 C19 C20 117.22(17) . . ? C23 C19 C7 119.54(17) . 1_545 ? C20 C19 C7 123.22(17) . 1_545 ? C21 C20 C19 119.58(19) . . ? N4 C26 C25 123.24(19) . . ? C24 C28 C27 119.43(19) . . ? N2 C7 C19 109.97(15) . 1_565 ? N2 C7 C2 112.95(15) . . ? C19 C7 C2 110.95(16) 1_565 . ? C1 C5 C4 104.7(2) . . ? C1 C5 C8 106.7(2) . . ? C4 C5 C8 113.9(3) . . ? C1 C5 C6 108.06(17) . . ? C4 C5 C6 116.1(2) . . ? C8 C5 C6 106.9(2) . . ? O2 C9 O3 123.8(2) . . ? O2 C9 C2 123.5(2) . . ? O3 C9 C2 112.6(2) . . ? N1 C3 C2 111.5(2) . . ? C22 C23 C19 119.2(2) . . ? C26 C25 C24 119.39(19) . . ? O5 C8 O4 124.9(3) . . ? O5 C8 C5 122.6(3) . . ? O4 C8 C5 112.4(4) . . ? N3 C22 C23 124.0(2) . . ? N4 C27 C28 123.1(2) . . ? N3 C21 C20 123.1(2) . . ? O1 C1 C5 124.27(19) . . ? O1 C1 C2 124.78(19) . . ? C5 C1 C2 110.79(17) . . ? N1 C4 C5 110.9(2) . . ? C8 O4 C10 107.0(5) . . ? C31 C29 N1 124.4(5) . . ? C31A C29 N1 112.6(3) . . ? C31 C29 C30 115.0(5) . . ? C31A C29 C30 123.5(4) . . ? N1 C29 C30 116.8(3) . . ? Cl2 C100 Cl3 131.8(4) . . ? Cl2 C100 Cl4 114.3(3) . . ? Cl3 C100 Cl4 91.4(3) . . ? Cl3A C100 Cl2A 68.2(4) . . ? Cl3A C100 Cl4A 135.3(5) . . ? Cl2A C100 Cl4A 100.7(6) . . ? C100 Cl3 Cl4 44.8(2) . . ? C100 Cl4 Cl3 43.8(2) . . ? C100 Cl3A Cl2A 56.0(3) . . ? C100 Cl2A Cl3A 55.8(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 Mn1 N3 2.3263(18) 2 ? Mn1 N3 2.3264(18) . ? Mn1 N4 2.3297(17) 2 ? Mn1 N4 2.3297(17) . ? Mn1 Cl1 2.4734(10) 2 ? Mn1 Cl1 2.4734(10) . ? O5 C8 1.196(6) . ? O5 C10A 1.396(8) . ? N2 C18 1.469(3) . ? N2 C7 1.474(2) . ? N2 C6 1.475(2) . ? N3 C22 1.329(3) . ? N3 C21 1.337(3) . ? C2 C1 1.516(3) . ? C2 C9 1.531(3) . ? C2 C3 1.546(3) . ? C2 C7 1.562(3) . ? N4 C26 1.336(3) . ? N4 C27 1.340(3) . ? O1 C1 1.202(3) . ? C24 C28 1.385(3) . ? C24 C25 1.386(3) . ? C24 C6 1.515(3) . ? N1 C4 1.445(4) . ? N1 C3 1.453(3) . ? N1 C29 1.474(4) . ? O3 C9 1.310(3) . ? O3 C11 1.461(4) . ? O2 C9 1.188(3) . ? C6 C5 1.563(3) . ? C19 C23 1.385(3) . ? C19 C20 1.388(3) . ? C19 C7 1.516(2) 1_545 ? C20 C21 1.385(3) . ? C26 C25 1.386(3) . ? C28 C27 1.385(3) . ? C5 C1 1.515(3) . ? C5 C4 1.537(4) . ? C5 C8 1.563(4) . ? C23 C22 1.380(3) . ? C8 O4 1.283(5) . ? O4 C10 1.606(6) . ? C29 C31 1.360(9) . ? C29 C31A 1.359(6) . ? C29 C30 1.482(5) . ? C100 Cl2 1.665(5) . ? C100 Cl3 1.699(7) . ? C100 Cl4 1.731(6) . ? C100 Cl3A 1.771(8) . ? C100 Cl2A 1.775(8) . ? C100 Cl4A 1.803(9) . ? Cl3 Cl4 2.455(7) . ? Cl3A Cl2A 1.989(11) . ?