#------------------------------------------------------------------------------ #$Date: 2020-09-01 04:41:55 +0300 (Tue, 01 Sep 2020) $ #$Revision: 255771 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/53/7705326.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_7705326 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 'C72 H74 Cl2 Mn N10 O14' _chemical_formula_weight 1429.25 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2017/1 _audit_update_record ; 2020-08-02 deposited with the CCDC. 2020-08-31 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 106.49(14) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 12.34(3) _cell_length_b 22.76(7) _cell_length_c 11.13(2) _cell_measurement_reflns_used 79 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 61.60 _cell_measurement_theta_min 34.02 _cell_volume 2997(13) _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.940 _diffrn_measured_fraction_theta_max 0.940 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_unetI/netI 0.0306 _diffrn_reflns_Laue_measured_fraction_full 0.940 _diffrn_reflns_Laue_measured_fraction_max 0.940 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 14249 _diffrn_reflns_point_group_measured_fraction_full 0.940 _diffrn_reflns_point_group_measured_fraction_max 0.940 _diffrn_reflns_theta_full 66.723 _diffrn_reflns_theta_max 66.722 _diffrn_reflns_theta_min 3.734 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 3.308 _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.583 _exptl_crystal_description block _exptl_crystal_F_000 1494 _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.070 _refine_diff_density_max 0.791 _refine_diff_density_min -0.704 _refine_diff_density_rms 0.086 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 421 _refine_ls_number_reflns 4997 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.058 _refine_ls_R_factor_all 0.0931 _refine_ls_R_factor_gt 0.0778 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1566P)^2^+3.9966P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2327 _refine_ls_wR_factor_ref 0.2482 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3914 _reflns_number_total 4997 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02734k2.cif _cod_data_source_block 1_o_NO2Toluene _cod_original_cell_volume 2998(12) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7705326 _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 0.733 _shelx_estimated_absorpt_t_max 0.801 _shelx_res_file ; TITL test_2 in P2(1)/c shelx.res created by SHELXL-2017/1 at 17:59:31 on 24-Jun-2019 CELL 1.54178 12.3437 22.7592 11.1301 90.000 106.491 90.000 ZERR 2.00 0.0258 0.0679 0.0198 0.000 0.143 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C N O CL MN H UNIT 144 20 28 4 2 148 MERG 2 DFIX 1.360 0.010 C27A C22A DFIX 1.350 0.005 C2S C3S DFIX 1.370 0.003 C2S C7S DFIX 1.460 0.010 C15A N2 DFIX 1.440 0.010 C12A N4 DFIX 1.430 0.010 C12A C13A FMAP 2 PLAN 6 SIZE 0.070 0.100 0.100 ACTA BOND $H CONF L.S. 5 TEMP 23.00 WGHT 0.156600 3.996600 FVAR 0.14410 N2 2 0.580948 0.961977 0.251834 11.00000 0.03169 0.04380 = 0.04634 0.00509 0.01496 0.00329 MN1 5 1.000000 1.000000 0.000000 10.50000 0.03179 0.04579 = 0.04800 -0.00123 0.01491 0.00042 CL2 4 0.976087 0.903054 -0.083408 11.00000 0.05178 0.05026 = 0.06577 -0.00762 0.02157 -0.00075 C32A 1 0.236269 0.944151 0.077081 11.00000 0.04511 0.04945 = 0.04826 -0.00397 0.01591 0.00169 AFIX 43 H32A 6 0.205313 0.925309 0.000899 11.00000 -1.20000 AFIX 0 C12A 1 0.509015 0.840085 0.296360 11.00000 0.04545 0.04784 = 0.05446 -0.00010 0.01512 -0.00569 AFIX 23 H12A 6 0.520078 0.804360 0.345890 11.00000 -1.20000 H12B 6 0.432820 0.839641 0.240293 11.00000 -1.20000 AFIX 0 O2 3 0.862493 0.939645 0.542144 11.00000 0.05662 0.07051 = 0.05637 -0.00412 -0.00114 -0.00429 O3 3 0.666154 0.878510 0.565042 11.00000 0.06029 0.08636 = 0.04396 0.00955 0.01666 0.00271 O4 3 0.448338 0.924808 0.524767 11.00000 0.08281 0.07647 = 0.07810 -0.00983 0.05389 -0.01372 N1 2 0.912589 0.974685 0.132251 11.00000 0.03831 0.05214 = 0.04875 -0.00379 0.01904 -0.00322 N3 2 0.174003 0.976310 0.119934 11.00000 0.03891 0.05440 = 0.05317 -0.00412 0.01689 0.00371 N4 2 0.585045 0.842030 0.227941 11.00000 0.04349 0.04297 = 0.04674 -0.00145 0.01223 -0.00115 C14A 1 0.714945 0.896529 0.392146 11.00000 0.03775 0.04871 = 0.04299 0.00360 0.01137 0.00319 C3S 1 0.146667 0.731881 0.305127 11.00000 0.05685 0.06365 = 0.06675 -0.00293 0.01415 -0.00365 C2S 1 0.153616 0.775894 0.228162 11.00000 0.08141 0.09104 = 0.06401 -0.00157 0.01415 -0.03709 C3A 1 0.767501 0.962953 0.257514 11.00000 0.03582 0.04150 = 0.04709 -0.00087 0.01352 0.00251 C4A 1 0.861563 0.994213 0.301974 11.00000 0.04230 0.05816 = 0.04792 -0.00996 0.01292 -0.00965 AFIX 43 H4 6 0.876465 1.012168 0.380033 11.00000 -1.20000 AFIX 0 C5A 1 0.930067 0.999339 0.238005 11.00000 0.03685 0.06523 = 0.05408 -0.00565 0.01655 -0.01180 AFIX 43 H3 6 0.995041 1.021732 0.268997 11.00000 -1.20000 AFIX 0 C1A 1 0.821874 0.943933 0.089519 11.00000 0.04659 0.04717 = 0.04992 -0.00430 0.01940 -0.00943 AFIX 43 H1 6 0.810662 0.925076 0.012826 11.00000 -1.20000 AFIX 0 C2A 1 0.748337 0.938276 0.146282 11.00000 0.03799 0.04594 = 0.04738 -0.00240 0.01363 -0.00471 AFIX 43 H2 6 0.682242 0.917324 0.111117 11.00000 -1.20000 AFIX 0 C4S 1 0.068967 0.730502 0.355935 11.00000 0.07789 0.08405 = 0.09008 0.00526 0.03417 -0.00706 AFIX 43 H4S 6 0.064125 0.699918 0.409585 11.00000 -1.20000 AFIX 0 C30A 1 0.391136 0.960474 0.246278 11.00000 0.03728 0.05075 = 0.04363 -0.00190 0.01757 -0.00059 C29A 1 0.326750 0.994179 0.288666 11.00000 0.04496 0.06322 = 0.05099 -0.00940 0.01298 0.00358 AFIX 43 H29A 6 0.355714 1.013647 0.364482 11.00000 -1.20000 AFIX 0 C28A 1 0.220555 1.001162 0.225394 11.00000 0.04284 0.06851 = 0.05445 -0.01103 0.01815 0.00844 AFIX 43 H28A 6 0.176227 1.025619 0.258965 11.00000 -1.20000 AFIX 0 C31A 1 0.344102 0.935864 0.135556 11.00000 0.04241 0.05108 = 0.04668 0.00030 0.01702 0.00628 AFIX 43 H31A 6 0.387727 0.912505 0.098811 11.00000 -1.20000 AFIX 0 C13A 1 0.523395 0.891234 0.379309 11.00000 0.04364 0.04974 = 0.04616 0.00047 0.01843 -0.00240 C21A 1 0.566001 0.793577 0.147741 11.00000 0.06290 0.04933 = 0.05329 -0.00655 0.01570 -0.00690 AFIX 23 H21A 6 0.598254 0.758719 0.194480 11.00000 -1.20000 H21B 6 0.485352 0.787354 0.113521 11.00000 -1.20000 AFIX 66 C22A 1 0.611482 0.801879 0.056089 11.00000 0.05954 0.04561 = 0.05778 -0.01430 0.01079 -0.00219 C23A 1 0.555575 0.835274 -0.047527 11.00000 0.07578 0.06335 = 0.06027 -0.01202 0.01450 -0.00188 AFIX 43 H13A 6 0.482687 0.848725 -0.055723 11.00000 -1.20000 AFIX 65 C24A 1 0.608607 0.848567 -0.138893 11.00000 0.11428 0.06614 = 0.05876 -0.01309 0.02785 -0.00952 AFIX 43 H24A 6 0.571202 0.870911 -0.208219 11.00000 -1.20000 AFIX 65 C25A 1 0.717546 0.828463 -0.126644 11.00000 0.10020 0.07189 = 0.08860 -0.02924 0.03238 -0.01650 AFIX 43 H25A 6 0.753027 0.837357 -0.187775 11.00000 -1.20000 AFIX 65 C26A 1 0.773454 0.795068 -0.023029 11.00000 0.08063 0.08628 = 0.09557 -0.04191 0.03993 -0.01047 AFIX 43 H26A 6 0.846341 0.781618 -0.014834 11.00000 -1.20000 AFIX 65 C27A 1 0.720423 0.781775 0.068338 11.00000 0.06742 0.06428 = 0.07450 -0.01876 0.02329 0.00738 AFIX 43 H27A 6 0.757829 0.759431 0.137664 11.00000 -1.20000 AFIX 0 C11A 1 0.695097 0.844133 0.308013 11.00000 0.04205 0.04389 = 0.04886 0.00257 0.01341 0.00396 AFIX 23 H11B 6 0.748064 0.844901 0.258202 11.00000 -1.20000 H11A 6 0.709475 0.808785 0.358767 11.00000 -1.20000 AFIX 0 C8A 1 0.827494 0.898954 0.483436 11.00000 0.04191 0.06127 = 0.04740 0.00277 0.00892 0.00453 C18A 1 0.638628 0.888805 0.460386 11.00000 0.04764 0.04472 = 0.04558 0.00008 0.01475 0.00105 C19A 1 0.451286 0.888730 0.455183 11.00000 0.05321 0.06207 = 0.05164 0.00475 0.02027 -0.00914 O5 3 0.395236 0.841787 0.439567 11.00000 0.11501 0.11234 = 0.09334 -0.03802 0.07348 -0.06656 C17A 1 0.563924 1.020488 0.204931 11.00000 0.04833 0.04918 = 0.06617 0.01481 0.02301 0.00644 AFIX 33 H17A 6 0.614953 1.028499 0.155983 11.00000 -1.50000 H17C 6 0.487492 1.024847 0.153416 11.00000 -1.50000 H17B 6 0.577852 1.047564 0.273773 11.00000 -1.50000 AFIX 0 C20A 1 0.326815 0.837584 0.513268 11.00000 0.18060 0.19819 = 0.14432 -0.07382 0.12922 -0.12561 AFIX 33 H2A 6 0.286424 0.801040 0.497270 11.00000 -1.50000 H20C 6 0.370879 0.839087 0.599489 11.00000 -1.50000 H20B 6 0.274028 0.869607 0.495948 11.00000 -1.50000 AFIX 0 O1 3 0.878846 0.850633 0.492264 11.00000 0.05694 0.07889 = 0.07534 -0.01145 -0.01099 0.02632 C9A 1 0.982242 0.848929 0.586958 11.00000 0.07874 0.12484 = 0.11348 -0.01862 -0.04146 0.03843 AFIX 33 H9A 6 1.016174 0.810915 0.587894 11.00000 -1.50000 H9B 6 1.031923 0.878464 0.570961 11.00000 -1.50000 H9C 6 0.969213 0.856247 0.666664 11.00000 -1.50000 AFIX 0 C16A 1 0.692882 0.955213 0.327601 11.00000 0.03524 0.04271 = 0.04130 -0.00259 0.01162 0.00068 AFIX 13 H16A 6 0.707726 0.985791 0.392224 11.00000 -1.20000 AFIX 0 C15A 1 0.507173 0.951702 0.321249 11.00000 0.03557 0.04885 = 0.04277 -0.00087 0.01485 0.00126 AFIX 13 H15A 6 0.523221 0.980447 0.389599 11.00000 -1.20000 AFIX 0 C7S 1 0.073419 0.818906 0.211001 11.00000 0.10954 0.07832 = 0.08976 0.02077 0.00691 -0.01116 AFIX 43 H7S 6 0.075658 0.850689 0.159244 11.00000 -1.20000 AFIX 0 C5S 1 -0.006088 0.773016 0.332434 11.00000 0.08171 0.12157 = 0.12093 -0.00669 0.04523 0.00771 AFIX 43 H5S 6 -0.065229 0.771167 0.368698 11.00000 -1.20000 AFIX 0 C6S 1 -0.001763 0.815916 0.263508 11.00000 0.09473 0.09246 = 0.12638 0.01139 0.03009 0.01175 AFIX 43 H6S 6 -0.055511 0.845607 0.251949 11.00000 -1.20000 AFIX 0 C1S 1 0.238207 0.776341 0.172277 11.00000 0.12238 0.18474 = 0.11517 -0.03504 0.06231 -0.07683 AFIX 33 H2X 6 0.231318 0.810613 0.120364 11.00000 -1.50000 H3X 6 0.309812 0.776984 0.235311 11.00000 -1.50000 H1X 6 0.233260 0.741740 0.121668 11.00000 -1.50000 AFIX 0 O2S 3 0.272701 0.672361 0.429571 11.00000 0.13027 N1S 2 0.222800 0.685105 0.328952 11.00000 0.09447 O1S 3 0.238156 0.662610 0.244025 11.00000 0.15330 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 REM test_2 in P2(1)/c REM R1 = 0.0778 for 3914 Fo > 4sig(Fo) and 0.0931 for all 4997 data REM 421 parameters refined using 6 restraints END WGHT 0.1517 3.8102 REM Highest difference peak 0.791, deepest hole -0.704, 1-sigma level 0.086 Q1 1 0.7408 0.7974 -0.0208 11.00000 0.05 0.79 Q2 1 0.6998 0.8263 -0.1023 11.00000 0.05 0.78 Q3 1 0.5850 0.8329 -0.0623 11.00000 0.05 0.75 Q4 1 0.6351 0.8021 0.0452 11.00000 0.05 0.74 Q5 1 0.2026 0.6361 0.2982 11.00000 0.05 0.72 Q6 1 0.6853 0.7852 0.0385 11.00000 0.05 0.62 ; _shelx_res_checksum 90955 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 N2 N 0.5809(3) 0.96198(16) 0.2518(3) 0.0398(8) Uani 1 1 d D . . . . Mn1 Mn 1.000000 1.000000 0.000000 0.0411(3) Uani 1 2 d S . P . . Cl2 Cl 0.97609(10) 0.90305(5) -0.08341(12) 0.0549(4) Uani 1 1 d . . . . . C32A C 0.2363(4) 0.9442(2) 0.0771(4) 0.0471(11) Uani 1 1 d . . . . . H32A H 0.205313 0.925309 0.000899 0.056 Uiso 1 1 calc R U . . . C12A C 0.5090(4) 0.8401(2) 0.2964(4) 0.0491(11) Uani 1 1 d D . . . . H12A H 0.520078 0.804360 0.345890 0.059 Uiso 1 1 calc R U . . . H12B H 0.432820 0.839641 0.240293 0.059 Uiso 1 1 calc R U . . . O2 O 0.8625(3) 0.93965(18) 0.5421(3) 0.0647(10) Uani 1 1 d . . . . . O3 O 0.6662(3) 0.87851(19) 0.5650(3) 0.0632(10) Uani 1 1 d . . . . . O4 O 0.4483(4) 0.92481(19) 0.5248(4) 0.0727(12) Uani 1 1 d . . . . . N1 N 0.9126(3) 0.97468(18) 0.1323(4) 0.0450(9) Uani 1 1 d . . . . . N3 N 0.1740(3) 0.97631(18) 0.1199(4) 0.0480(9) Uani 1 1 d . . . . . N4 N 0.5850(3) 0.84203(16) 0.2279(3) 0.0445(9) Uani 1 1 d D . . . . C14A C 0.7149(4) 0.8965(2) 0.3921(4) 0.0432(10) Uani 1 1 d . . . . . C3S C 0.1467(5) 0.7319(2) 0.3051(5) 0.0631(14) Uani 1 1 d D . . . . C2S C 0.1536(6) 0.7759(3) 0.2282(6) 0.0802(19) Uani 1 1 d D . . . . C3A C 0.7675(4) 0.96295(19) 0.2575(4) 0.0411(10) Uani 1 1 d . . . . . C4A C 0.8616(4) 0.9942(2) 0.3020(5) 0.0494(11) Uani 1 1 d . . . . . H4 H 0.876465 1.012168 0.380033 0.059 Uiso 1 1 calc R U . . . C5A C 0.9301(4) 0.9993(2) 0.2380(5) 0.0513(12) Uani 1 1 d . . . . . H3 H 0.995041 1.021732 0.268997 0.062 Uiso 1 1 calc R U . . . C1A C 0.8219(4) 0.9439(2) 0.0895(5) 0.0467(11) Uani 1 1 d . . . . . H1 H 0.810662 0.925076 0.012826 0.056 Uiso 1 1 calc R U . . . C2A C 0.7483(4) 0.9383(2) 0.1463(4) 0.0435(10) Uani 1 1 d . . . . . H2 H 0.682242 0.917324 0.111117 0.052 Uiso 1 1 calc R U . . . C4S C 0.0690(6) 0.7305(3) 0.3559(7) 0.0819(18) Uani 1 1 d . . . . . H4S H 0.064125 0.699918 0.409585 0.098 Uiso 1 1 calc R U . . . C30A C 0.3911(4) 0.9605(2) 0.2463(4) 0.0426(10) Uani 1 1 d . . . . . C29A C 0.3268(4) 0.9942(2) 0.2887(5) 0.0532(12) Uani 1 1 d . . . . . H29A H 0.355714 1.013647 0.364482 0.064 Uiso 1 1 calc R U . . . C28A C 0.2206(4) 1.0012(2) 0.2254(5) 0.0544(13) Uani 1 1 d . . . . . H28A H 0.176227 1.025619 0.258965 0.065 Uiso 1 1 calc R U . . . C31A C 0.3441(4) 0.9359(2) 0.1356(4) 0.0458(10) Uani 1 1 d . . . . . H31A H 0.387727 0.912505 0.098811 0.055 Uiso 1 1 calc R U . . . C13A C 0.5234(4) 0.8912(2) 0.3793(4) 0.0453(10) Uani 1 1 d D . . . . C21A C 0.5660(5) 0.7936(2) 0.1477(5) 0.0553(12) Uani 1 1 d . . . . . H21A H 0.598254 0.758719 0.194480 0.066 Uiso 1 1 calc R U . . . H21B H 0.485352 0.787354 0.113521 0.066 Uiso 1 1 calc R U . . . C22A C 0.6115(3) 0.80188(16) 0.0561(3) 0.0555(12) Uani 1 1 d DG . . . . C23A C 0.5556(3) 0.83527(17) -0.0475(3) 0.0675(15) Uani 1 1 d G . . . . H13A H 0.482687 0.848725 -0.055723 0.081 Uiso 1 1 calc R U . . . C24A C 0.6086(4) 0.84857(17) -0.1389(3) 0.0790(19) Uani 1 1 d G . . . . H24A H 0.571202 0.870911 -0.208219 0.095 Uiso 1 1 calc R U . . . C25A C 0.7175(4) 0.8285(2) -0.1266(4) 0.086(2) Uani 1 1 d G . . . . H25A H 0.753027 0.837357 -0.187775 0.103 Uiso 1 1 calc R U . . . C26A C 0.7735(3) 0.7951(2) -0.0230(4) 0.084(2) Uani 1 1 d G . . . . H26A H 0.846341 0.781618 -0.014834 0.101 Uiso 1 1 calc R U . . . C27A C 0.7204(3) 0.78178(16) 0.0683(3) 0.0681(15) Uani 1 1 d DG . . . . H27A H 0.757829 0.759431 0.137664 0.082 Uiso 1 1 calc R U . . . C11A C 0.6951(4) 0.8441(2) 0.3080(4) 0.0448(10) Uani 1 1 d . . . . . H11B H 0.748064 0.844901 0.258202 0.054 Uiso 1 1 calc R U . . . H11A H 0.709475 0.808785 0.358767 0.054 Uiso 1 1 calc R U . . . C8A C 0.8275(4) 0.8990(2) 0.4834(5) 0.0510(12) Uani 1 1 d . . . . . C18A C 0.6386(4) 0.8888(2) 0.4604(4) 0.0457(10) Uani 1 1 d . . . . . C19A C 0.4513(5) 0.8887(2) 0.4552(5) 0.0545(12) Uani 1 1 d . . . . . O5 O 0.3952(4) 0.8418(2) 0.4396(4) 0.0979(18) Uani 1 1 d . . . . . C17A C 0.5639(4) 1.0205(2) 0.2049(5) 0.0532(12) Uani 1 1 d . . . . . H17A H 0.614953 1.028499 0.155983 0.080 Uiso 1 1 calc R U . . . H17C H 0.487492 1.024847 0.153416 0.080 Uiso 1 1 calc R U . . . H17B H 0.577852 1.047564 0.273773 0.080 Uiso 1 1 calc R U . . . C20A C 0.3268(10) 0.8376(5) 0.5133(10) 0.157(5) Uani 1 1 d . . . . . H2A H 0.286424 0.801040 0.497270 0.236 Uiso 1 1 calc R U . . . H20C H 0.370879 0.839087 0.599489 0.236 Uiso 1 1 calc R U . . . H20B H 0.274028 0.869607 0.495948 0.236 Uiso 1 1 calc R U . . . O1 O 0.8788(3) 0.85063(19) 0.4923(4) 0.0765(12) Uani 1 1 d . . . . . C9A C 0.9822(7) 0.8489(4) 0.5870(8) 0.120(3) Uani 1 1 d . . . . . H9A H 1.016174 0.810915 0.587894 0.180 Uiso 1 1 calc R U . . . H9B H 1.031923 0.878464 0.570961 0.180 Uiso 1 1 calc R U . . . H9C H 0.969213 0.856247 0.666664 0.180 Uiso 1 1 calc R U . . . C16A C 0.6929(3) 0.95521(19) 0.3276(4) 0.0396(9) Uani 1 1 d . . . . . H16A H 0.707726 0.985791 0.392224 0.048 Uiso 1 1 calc R U . . . C15A C 0.5072(3) 0.9517(2) 0.3212(4) 0.0416(10) Uani 1 1 d D . . . . H15A H 0.523221 0.980447 0.389599 0.050 Uiso 1 1 calc R U . . . C7S C 0.0734(7) 0.8189(3) 0.2110(8) 0.097(2) Uani 1 1 d D . . . . H7S H 0.075658 0.850689 0.159244 0.116 Uiso 1 1 calc R U . . . C5S C -0.0061(7) 0.7730(5) 0.3324(9) 0.105(3) Uani 1 1 d . . . . . H5S H -0.065229 0.771167 0.368698 0.126 Uiso 1 1 calc R U . . . C6S C -0.0018(8) 0.8159(4) 0.2635(9) 0.105(3) Uani 1 1 d . . . . . H6S H -0.055511 0.845607 0.251949 0.126 Uiso 1 1 calc R U . . . C1S C 0.2382(8) 0.7763(5) 0.1723(9) 0.135(4) Uani 1 1 d . . . . . H2X H 0.231318 0.810613 0.120364 0.202 Uiso 1 1 calc R U . . . H3X H 0.309812 0.776984 0.235311 0.202 Uiso 1 1 calc R U . . . H1X H 0.233260 0.741740 0.121668 0.202 Uiso 1 1 calc R U . . . O2S O 0.2727(6) 0.6724(3) 0.4296(7) 0.130(2) Uiso 1 1 d . . . . . N1S N 0.2228(6) 0.6851(3) 0.3290(7) 0.0945(18) Uiso 1 1 d . . . . . O1S O 0.2382(7) 0.6626(4) 0.2440(8) 0.153(3) 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 N2 0.0317(17) 0.0438(19) 0.046(2) 0.0051(16) 0.0150(15) 0.0033(15) Mn1 0.0318(5) 0.0458(6) 0.0480(6) -0.0012(4) 0.0149(4) 0.0004(4) Cl2 0.0518(7) 0.0503(7) 0.0658(8) -0.0076(5) 0.0216(6) -0.0007(5) C32A 0.045(2) 0.049(2) 0.048(3) -0.004(2) 0.016(2) 0.002(2) C12A 0.045(3) 0.048(3) 0.054(3) 0.000(2) 0.015(2) -0.006(2) O2 0.057(2) 0.071(2) 0.056(2) -0.0041(19) -0.0011(17) -0.0043(19) O3 0.060(2) 0.086(3) 0.044(2) 0.0096(18) 0.0167(16) 0.003(2) O4 0.083(3) 0.076(3) 0.078(3) -0.010(2) 0.054(2) -0.014(2) N1 0.038(2) 0.052(2) 0.049(2) -0.0038(18) 0.0190(17) -0.0032(18) N3 0.039(2) 0.054(2) 0.053(2) -0.0041(19) 0.0169(17) 0.0037(18) N4 0.043(2) 0.0430(19) 0.047(2) -0.0014(16) 0.0122(17) -0.0011(16) C14A 0.038(2) 0.049(2) 0.043(2) 0.0036(19) 0.0114(19) 0.0032(19) C3S 0.057(3) 0.064(3) 0.067(3) -0.003(3) 0.014(3) -0.004(3) C2S 0.081(4) 0.091(5) 0.064(4) -0.002(3) 0.014(3) -0.037(4) C3A 0.036(2) 0.041(2) 0.047(2) -0.0009(19) 0.0135(18) 0.0025(18) C4A 0.042(3) 0.058(3) 0.048(3) -0.010(2) 0.013(2) -0.010(2) C5A 0.037(2) 0.065(3) 0.054(3) -0.006(2) 0.017(2) -0.012(2) C1A 0.047(3) 0.047(2) 0.050(3) -0.004(2) 0.019(2) -0.009(2) C2A 0.038(2) 0.046(2) 0.047(3) -0.0024(19) 0.0136(19) -0.0047(19) C4S 0.078(4) 0.084(5) 0.090(5) 0.005(4) 0.034(4) -0.007(4) C30A 0.037(2) 0.051(2) 0.044(2) -0.0019(19) 0.0176(19) -0.001(2) C29A 0.045(3) 0.063(3) 0.051(3) -0.009(2) 0.013(2) 0.004(2) C28A 0.043(3) 0.069(3) 0.054(3) -0.011(2) 0.018(2) 0.008(2) C31A 0.042(2) 0.051(3) 0.047(3) 0.000(2) 0.017(2) 0.006(2) C13A 0.044(2) 0.050(2) 0.046(2) 0.000(2) 0.018(2) -0.002(2) C21A 0.063(3) 0.049(3) 0.053(3) -0.007(2) 0.016(2) -0.007(2) C22A 0.060(3) 0.046(3) 0.058(3) -0.014(2) 0.011(2) -0.002(2) C23A 0.076(4) 0.063(3) 0.060(3) -0.012(3) 0.014(3) -0.002(3) C24A 0.114(6) 0.066(4) 0.059(3) -0.013(3) 0.028(4) -0.010(4) C25A 0.100(5) 0.072(4) 0.089(5) -0.029(4) 0.032(4) -0.016(4) C26A 0.081(4) 0.086(5) 0.096(5) -0.042(4) 0.040(4) -0.010(4) C27A 0.067(4) 0.064(3) 0.074(4) -0.019(3) 0.023(3) 0.007(3) C11A 0.042(2) 0.044(2) 0.049(3) 0.0026(19) 0.0134(19) 0.0040(19) C8A 0.042(2) 0.061(3) 0.047(3) 0.003(2) 0.009(2) 0.005(2) C18A 0.048(3) 0.045(2) 0.046(3) 0.0001(19) 0.015(2) 0.001(2) C19A 0.053(3) 0.062(3) 0.052(3) 0.005(2) 0.020(2) -0.009(3) O5 0.115(4) 0.112(4) 0.093(3) -0.038(3) 0.073(3) -0.067(3) C17A 0.048(3) 0.049(3) 0.066(3) 0.015(2) 0.023(2) 0.006(2) C20A 0.181(10) 0.198(11) 0.144(8) -0.074(8) 0.129(8) -0.126(9) O1 0.057(2) 0.079(3) 0.075(3) -0.011(2) -0.0110(19) 0.026(2) C9A 0.079(5) 0.125(7) 0.113(6) -0.019(5) -0.041(5) 0.038(5) C16A 0.035(2) 0.043(2) 0.041(2) -0.0026(18) 0.0116(17) 0.0007(18) C15A 0.036(2) 0.049(2) 0.043(2) -0.0009(19) 0.0149(18) 0.0013(19) C7S 0.110(6) 0.078(5) 0.090(5) 0.021(4) 0.007(5) -0.011(5) C5S 0.082(5) 0.122(7) 0.121(7) -0.007(6) 0.045(5) 0.008(5) C6S 0.095(6) 0.092(6) 0.126(7) 0.011(5) 0.030(5) 0.012(5) C1S 0.122(7) 0.185(11) 0.115(7) -0.035(7) 0.062(6) -0.077(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn -0.5299 2.8052 '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 C15A N2 C16A 109.9(4) . . ? C15A N2 C17A 108.3(4) . . ? C16A N2 C17A 109.8(4) . . ? N1 Mn1 N1 180.00(14) . 3_775 ? N1 Mn1 N3 83.7(2) . 3_675 ? N1 Mn1 N3 96.3(2) 3_775 3_675 ? N1 Mn1 N3 96.3(2) . 1_655 ? N1 Mn1 N3 83.7(2) 3_775 1_655 ? N3 Mn1 N3 180.0 3_675 1_655 ? N1 Mn1 Cl2 89.30(15) . . ? N1 Mn1 Cl2 90.70(15) 3_775 . ? N3 Mn1 Cl2 89.94(15) 3_675 . ? N3 Mn1 Cl2 90.06(15) 1_655 . ? N1 Mn1 Cl2 90.70(15) . 3_775 ? N1 Mn1 Cl2 89.30(15) 3_775 3_775 ? N3 Mn1 Cl2 90.06(15) 3_675 3_775 ? N3 Mn1 Cl2 89.94(15) 1_655 3_775 ? Cl2 Mn1 Cl2 180.0 . 3_775 ? N3 C32A C31A 122.6(5) . . ? N3 C32A H32A 118.7 . . ? C31A C32A H32A 118.7 . . ? N4 C12A C13A 110.2(4) . . ? N4 C12A H12A 109.6 . . ? C13A C12A H12A 109.6 . . ? N4 C12A H12B 109.6 . . ? C13A C12A H12B 109.6 . . ? H12A C12A H12B 108.1 . . ? C5A N1 C1A 118.9(4) . . ? C5A N1 Mn1 122.3(4) . . ? C1A N1 Mn1 116.6(3) . . ? C32A N3 C28A 116.3(5) . . ? C32A N3 Mn1 120.1(4) . 1_455 ? C28A N3 Mn1 122.8(4) . 1_455 ? C12A N4 C21A 108.2(4) . . ? C12A N4 C11A 110.0(4) . . ? C21A N4 C11A 113.0(4) . . ? C18A C14A C8A 106.5(4) . . ? C18A C14A C11A 103.2(4) . . ? C8A C14A C11A 114.7(4) . . ? C18A C14A C16A 108.5(4) . . ? C8A C14A C16A 107.7(4) . . ? C11A C14A C16A 115.7(4) . . ? C4S C3S C2S 120.5(7) . . ? C4S C3S N1S 117.3(6) . . ? C2S C3S N1S 122.1(6) . . ? C3S C2S C1S 119.8(8) . . ? C3S C2S C7S 116.8(6) . . ? C1S C2S C7S 123.4(8) . . ? C2A C3A C4A 118.8(5) . . ? C2A C3A C16A 120.5(4) . . ? C4A C3A C16A 120.7(4) . . ? C5A C4A C3A 119.7(5) . . ? C5A C4A H4 120.2 . . ? C3A C4A H4 120.2 . . ? C4A C5A N1 121.4(5) . . ? C4A C5A H3 119.3 . . ? N1 C5A H3 119.3 . . ? C2A C1A N1 123.2(5) . . ? C2A C1A H1 118.4 . . ? N1 C1A H1 118.4 . . ? C1A C2A C3A 117.9(5) . . ? C1A C2A H2 121.1 . . ? C3A C2A H2 121.1 . . ? C3S C4S C5S 118.8(8) . . ? C3S C4S H4S 120.6 . . ? C5S C4S H4S 120.6 . . ? C29A C30A C31A 116.0(5) . . ? C29A C30A C15A 118.8(4) . . ? C31A C30A C15A 125.1(4) . . ? C30A C29A C28A 120.2(5) . . ? C30A C29A H29A 119.9 . . ? C28A C29A H29A 119.9 . . ? N3 C28A C29A 124.0(5) . . ? N3 C28A H28A 118.0 . . ? C29A C28A H28A 118.0 . . ? C32A C31A C30A 120.8(5) . . ? C32A C31A H31A 119.6 . . ? C30A C31A H31A 119.6 . . ? C19A C13A C18A 107.7(4) . . ? C19A C13A C12A 111.5(4) . . ? C18A C13A C12A 106.5(4) . . ? C19A C13A C15A 105.5(4) . . ? C18A C13A C15A 106.7(4) . . ? C12A C13A C15A 118.5(4) . . ? C22A C21A N4 110.6(4) . . ? C22A C21A H21A 109.5 . . ? N4 C21A H21A 109.5 . . ? C22A C21A H21B 109.5 . . ? N4 C21A H21B 109.5 . . ? H21A C21A H21B 108.1 . . ? C21A C22A C23A 120.2(4) . . ? C21A C22A C27A 119.5(4) . . ? C23A C22A C27A 120.0 . . ? C24A C23A C22A 120.0 . . ? C24A C23A H13A 120.0 . . ? C22A C23A H13A 120.0 . . ? C23A C24A C25A 120.0 . . ? C23A C24A H24A 120.0 . . ? C25A C24A H24A 120.0 . . ? C26A C25A C24A 120.0 . . ? C26A C25A H25A 120.0 . . ? C24A C25A H25A 120.0 . . ? C27A C26A C25A 120.0 . . ? C27A C26A H26A 120.0 . . ? C25A C26A H26A 120.0 . . ? C26A C27A C22A 120.0 . . ? C26A C27A H27A 120.0 . . ? C22A C27A H27A 120.0 . . ? N4 C11A C14A 112.6(4) . . ? N4 C11A H11B 109.1 . . ? C14A C11A H11B 109.1 . . ? N4 C11A H11A 109.1 . . ? C14A C11A H11A 109.1 . . ? H11B C11A H11A 107.8 . . ? O2 C8A O1 124.2(5) . . ? O2 C8A C14A 123.6(5) . . ? O1 C8A C14A 112.1(5) . . ? O3 C18A C14A 122.4(5) . . ? O3 C18A C13A 126.7(5) . . ? C14A C18A C13A 110.8(4) . . ? O4 C19A O5 125.8(5) . . ? O4 C19A C13A 122.3(5) . . ? O5 C19A C13A 111.9(5) . . ? C19A O5 C20A 113.2(6) . . ? N2 C17A H17A 109.5 . . ? N2 C17A H17C 109.5 . . ? H17A C17A H17C 109.5 . . ? N2 C17A H17B 109.5 . . ? H17A C17A H17B 109.5 . . ? H17C C17A H17B 109.5 . . ? O5 C20A H2A 109.5 . . ? O5 C20A H20C 109.5 . . ? H2A C20A H20C 109.5 . . ? O5 C20A H20B 109.5 . . ? H2A C20A H20B 109.5 . . ? H20C C20A H20B 109.5 . . ? C8A O1 C9A 114.3(5) . . ? O1 C9A H9A 109.5 . . ? O1 C9A H9B 109.5 . . ? H9A C9A H9B 109.5 . . ? O1 C9A H9C 109.5 . . ? H9A C9A H9C 109.5 . . ? H9B C9A H9C 109.5 . . ? C3A C16A N2 110.3(4) . . ? C3A C16A C14A 108.9(4) . . ? N2 C16A C14A 113.4(4) . . ? C3A C16A H16A 108.0 . . ? N2 C16A H16A 108.0 . . ? C14A C16A H16A 108.0 . . ? N2 C15A C30A 110.9(4) . . ? N2 C15A C13A 111.6(4) . . ? C30A C15A C13A 111.1(4) . . ? N2 C15A H15A 107.7 . . ? C30A C15A H15A 107.7 . . ? C13A C15A H15A 107.7 . . ? C6S C7S C2S 120.5(8) . . ? C6S C7S H7S 119.7 . . ? C2S C7S H7S 119.7 . . ? C6S C5S C4S 123.1(9) . . ? C6S C5S H5S 118.5 . . ? C4S C5S H5S 118.5 . . ? C7S C6S C5S 120.2(9) . . ? C7S C6S H6S 119.9 . . ? C5S C6S H6S 119.9 . . ? C2S C1S H2X 109.5 . . ? C2S C1S H3X 109.5 . . ? H2X C1S H3X 109.5 . . ? C2S C1S H1X 109.5 . . ? H2X C1S H1X 109.5 . . ? H3X C1S H1X 109.5 . . ? O1S N1S O2S 121.7(9) . . ? O1S N1S C3S 116.6(8) . . ? O2S N1S C3S 121.5(8) . . ? 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 N2 C15A 1.371(5) . ? N2 C16A 1.408(6) . ? N2 C17A 1.424(7) . ? Mn1 N1 2.136(5) . ? Mn1 N1 2.136(5) 3_775 ? Mn1 N3 2.249(6) 3_675 ? Mn1 N3 2.249(6) 1_655 ? Mn1 Cl2 2.379(6) . ? Mn1 Cl2 2.379(6) 3_775 ? C32A N3 1.250(6) . ? C32A C31A 1.319(7) . ? C32A H32A 0.9300 . ? C12A N4 1.367(6) . ? C12A C13A 1.465(6) . ? C12A H12A 0.9700 . ? C12A H12B 0.9700 . ? O2 C8A 1.145(7) . ? O3 C18A 1.141(6) . ? O4 C19A 1.136(7) . ? N1 C5A 1.266(7) . ? N1 C1A 1.291(6) . ? N3 C28A 1.283(7) . ? N4 C21A 1.396(7) . ? N4 C11A 1.398(6) . ? C14A C18A 1.379(7) . ? C14A C8A 1.471(7) . ? C14A C11A 1.493(7) . ? C14A C16A 1.504(7) . ? C3S C4S 1.244(9) . ? C3S C2S 1.337(5) . ? C3S N1S 1.395(9) . ? C2S C1S 1.359(10) . ? C2S C7S 1.367(4) . ? C3A C2A 1.318(7) . ? C3A C4A 1.332(7) . ? C3A C16A 1.377(6) . ? C4A C5A 1.256(8) . ? C4A H4 0.9300 . ? C5A H3 0.9300 . ? C1A C2A 1.251(7) . ? C1A H1 0.9300 . ? C2A H2 0.9300 . ? C4S C5S 1.314(12) . ? C4S H4S 0.9300 . ? C30A C29A 1.287(7) . ? C30A C31A 1.328(7) . ? C30A C15A 1.452(7) . ? C29A C28A 1.310(8) . ? C29A H29A 0.9300 . ? C28A H28A 0.9300 . ? C31A H31A 0.9300 . ? C13A C19A 1.391(7) . ? C13A C18A 1.453(7) . ? C13A C15A 1.509(7) . ? C21A C22A 1.310(6) . ? C21A H21A 0.9700 . ? C21A H21B 0.9700 . ? C22A C23A 1.3900 . ? C22A C27A 1.3900 . ? C23A C24A 1.3900 . ? C23A H13A 0.9300 . ? C24A C25A 1.3900 . ? C24A H24A 0.9300 . ? C25A C26A 1.3900 . ? C25A H25A 0.9300 . ? C26A C27A 1.3900 . ? C26A H26A 0.9300 . ? C27A H27A 0.9300 . ? C11A H11B 0.9700 . ? C11A H11A 0.9700 . ? C8A O1 1.259(7) . ? C19A O5 1.258(7) . ? O5 C20A 1.337(8) . ? C17A H17A 0.9600 . ? C17A H17C 0.9600 . ? C17A H17B 0.9600 . ? C20A H2A 0.9600 . ? C20A H20C 0.9600 . ? C20A H20B 0.9600 . ? O1 C9A 1.406(8) . ? C9A H9A 0.9600 . ? C9A H9B 0.9600 . ? C9A H9C 0.9600 . ? C16A H16A 0.9800 . ? C15A H15A 0.9800 . ? C7S C6S 1.231(11) . ? C7S H7S 0.9300 . ? C5S C6S 1.252(12) . ? C5S H5S 0.9300 . ? C6S H6S 0.9300 . ? C1S H2X 0.9600 . ? C1S H3X 0.9600 . ? C1S H1X 0.9600 . ? O2S N1S 1.152(8) . ? N1S O1S 1.137(9) . ? 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 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C31A C32A N3 C28A -0.2(8) . . . . ? C31A C32A N3 Mn1 169.7(4) . . . 1_455 ? C13A C12A N4 C21A -178.2(4) . . . . ? C13A C12A N4 C11A 57.8(5) . . . . ? C4S C3S C2S C1S -179.2(7) . . . . ? N1S C3S C2S C1S -1.2(10) . . . . ? C4S C3S C2S C7S 1.2(10) . . . . ? N1S C3S C2S C7S 179.2(6) . . . . ? C2A C3A C4A C5A -0.4(8) . . . . ? C16A C3A C4A C5A 178.0(5) . . . . ? C3A C4A C5A N1 -1.0(9) . . . . ? C1A N1 C5A C4A 0.4(8) . . . . ? Mn1 N1 C5A C4A 163.1(4) . . . . ? C5A N1 C1A C2A 1.7(8) . . . . ? Mn1 N1 C1A C2A -161.9(4) . . . . ? N1 C1A C2A C3A -3.0(8) . . . . ? C4A C3A C2A C1A 2.3(7) . . . . ? C16A C3A C2A C1A -176.0(4) . . . . ? C2S C3S C4S C5S 0.1(11) . . . . ? N1S C3S C4S C5S -178.0(7) . . . . ? C31A C30A C29A C28A 2.1(8) . . . . ? C15A C30A C29A C28A -177.4(5) . . . . ? C32A N3 C28A C29A -0.6(8) . . . . ? Mn1 N3 C28A C29A -170.2(4) 1_455 . . . ? C30A C29A C28A N3 -0.4(9) . . . . ? N3 C32A C31A C30A 2.0(8) . . . . ? C29A C30A C31A C32A -2.9(7) . . . . ? C15A C30A C31A C32A 176.6(5) . . . . ? N4 C12A C13A C19A -176.7(4) . . . . ? N4 C12A C13A C18A -59.5(5) . . . . ? N4 C12A C13A C15A 60.6(6) . . . . ? C12A N4 C21A C22A 161.3(4) . . . . ? C11A N4 C21A C22A -76.6(5) . . . . ? N4 C21A C22A C23A -81.1(5) . . . . ? N4 C21A C22A C27A 92.9(5) . . . . ? C21A C22A C23A C24A 174.0(4) . . . . ? C27A C22A C23A C24A 0.0 . . . . ? C22A C23A C24A C25A 0.0 . . . . ? C23A C24A C25A C26A 0.0 . . . . ? C24A C25A C26A C27A 0.0 . . . . ? C25A C26A C27A C22A 0.0 . . . . ? C21A C22A C27A C26A -174.0(4) . . . . ? C23A C22A C27A C26A 0.0 . . . . ? C12A N4 C11A C14A -59.6(5) . . . . ? C21A N4 C11A C14A 179.2(4) . . . . ? C18A C14A C11A N4 61.2(5) . . . . ? C8A C14A C11A N4 176.5(4) . . . . ? C16A C14A C11A N4 -57.1(5) . . . . ? C18A C14A C8A O2 -78.3(6) . . . . ? C11A C14A C8A O2 168.3(5) . . . . ? C16A C14A C8A O2 37.9(7) . . . . ? C18A C14A C8A O1 99.5(5) . . . . ? C11A C14A C8A O1 -13.9(6) . . . . ? C16A C14A C8A O1 -144.3(5) . . . . ? C8A C14A C18A O3 -9.5(7) . . . . ? C11A C14A C18A O3 111.6(5) . . . . ? C16A C14A C18A O3 -125.1(5) . . . . ? C8A C14A C18A C13A 174.8(4) . . . . ? C11A C14A C18A C13A -64.1(5) . . . . ? C16A C14A C18A C13A 59.1(5) . . . . ? C19A C13A C18A O3 10.0(7) . . . . ? C12A C13A C18A O3 -109.6(6) . . . . ? C15A C13A C18A O3 122.9(5) . . . . ? C19A C13A C18A C14A -174.5(4) . . . . ? C12A C13A C18A C14A 65.9(5) . . . . ? C15A C13A C18A C14A -61.6(5) . . . . ? C18A C13A C19A O4 64.8(7) . . . . ? C12A C13A C19A O4 -178.8(5) . . . . ? C15A C13A C19A O4 -48.9(7) . . . . ? C18A C13A C19A O5 -112.9(6) . . . . ? C12A C13A C19A O5 3.6(7) . . . . ? C15A C13A C19A O5 133.4(5) . . . . ? O4 C19A O5 C20A 1.1(12) . . . . ? C13A C19A O5 C20A 178.7(8) . . . . ? O2 C8A O1 C9A 3.6(10) . . . . ? C14A C8A O1 C9A -174.1(6) . . . . ? C2A C3A C16A N2 -44.6(6) . . . . ? C4A C3A C16A N2 137.1(5) . . . . ? C2A C3A C16A C14A 80.5(6) . . . . ? C4A C3A C16A C14A -97.8(5) . . . . ? C15A N2 C16A C3A 177.4(4) . . . . ? C17A N2 C16A C3A -63.6(5) . . . . ? C15A N2 C16A C14A 54.9(5) . . . . ? C17A N2 C16A C14A 173.9(4) . . . . ? C18A C14A C16A C3A -179.0(4) . . . . ? C8A C14A C16A C3A 66.1(5) . . . . ? C11A C14A C16A C3A -63.7(5) . . . . ? C18A C14A C16A N2 -55.8(5) . . . . ? C8A C14A C16A N2 -170.6(4) . . . . ? C11A C14A C16A N2 59.5(5) . . . . ? C16A N2 C15A C30A 177.9(4) . . . . ? C17A N2 C15A C30A 58.0(5) . . . . ? C16A N2 C15A C13A -57.5(5) . . . . ? C17A N2 C15A C13A -177.5(4) . . . . ? C29A C30A C15A N2 -128.6(5) . . . . ? C31A C30A C15A N2 51.9(6) . . . . ? C29A C30A C15A C13A 106.6(5) . . . . ? C31A C30A C15A C13A -72.9(6) . . . . ? C19A C13A C15A N2 174.8(4) . . . . ? C18A C13A C15A N2 60.4(5) . . . . ? C12A C13A C15A N2 -59.5(5) . . . . ? C19A C13A C15A C30A -60.8(5) . . . . ? C18A C13A C15A C30A -175.2(4) . . . . ? C12A C13A C15A C30A 64.9(5) . . . . ? C3S C2S C7S C6S -1.0(12) . . . . ? C1S C2S C7S C6S 179.5(9) . . . . ? C3S C4S C5S C6S -1.9(15) . . . . ? C2S C7S C6S C5S -0.7(15) . . . . ? C4S C5S C6S C7S 2.2(16) . . . . ? C4S C3S N1S O1S 128.3(9) . . . . ? C2S C3S N1S O1S -49.7(11) . . . . ? C4S C3S N1S O2S -56.4(10) . . . . ? C2S C3S N1S O2S 125.6(8) . . . . ?