#------------------------------------------------------------------------------ #$Date: 2020-09-01 04:41:55 +0300 (Tue, 01 Sep 2020) $ #$Revision: 255771 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/53/7705323.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_7705323 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 'C32 H34 Cl7 Mn0.5 N4 O6' _chemical_formula_weight 846.25 _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 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 103.95(3) _cell_angle_beta 112.74(3) _cell_angle_gamma 100.61(3) _cell_formula_units_Z 2 _cell_length_a 12.498(3) _cell_length_b 13.003(3) _cell_length_c 14.074(3) _cell_measurement_reflns_used 4848 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 23.475 _cell_measurement_theta_min 2.528 _cell_volume 1946.5(11) _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _diffrn_ambient_temperature 120(2) _diffrn_measured_fraction_theta_full 0.960 _diffrn_measured_fraction_theta_max 0.960 _diffrn_measurement_device_type 'Bruker APEX II CCD diffractometer' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0641 _diffrn_reflns_av_unetI/netI 0.0832 _diffrn_reflns_Laue_measured_fraction_full 0.960 _diffrn_reflns_Laue_measured_fraction_max 0.960 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 10407 _diffrn_reflns_point_group_measured_fraction_full 0.960 _diffrn_reflns_point_group_measured_fraction_max 0.960 _diffrn_reflns_theta_full 23.623 _diffrn_reflns_theta_max 23.623 _diffrn_reflns_theta_min 1.671 _exptl_absorpt_coefficient_mu 0.711 _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.444 _exptl_crystal_description prism _exptl_crystal_F_000 867 _exptl_crystal_size_max 0.060 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.030 _refine_diff_density_max 1.835 _refine_diff_density_min -0.696 _refine_diff_density_rms 0.098 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 448 _refine_ls_number_reflns 5616 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.097 _refine_ls_R_factor_all 0.0995 _refine_ls_R_factor_gt 0.0636 _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^)+(0.0852P)^2^+3.6749P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1652 _refine_ls_wR_factor_ref 0.1810 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3896 _reflns_number_total 5616 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02734k2.cif _cod_data_source_block L5TCM _cod_original_cell_volume 1946.4(8) _cod_original_formula_sum 'C32 H34 Cl7 Mn0.50 N4 O6' _cod_database_code 7705323 _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 0.959 _shelx_estimated_absorpt_t_max 0.979 _shelx_res_file ; TITL TCMnw in P-1 shelx.res created by SHELXL-2017/1 at 10:58:40 on 08-Jul-2020 CELL 0.71073 12.4980 13.0030 14.0740 103.952 112.736 100.615 ZERR 2.00 0.0025 0.0026 0.0028 0.030 0.030 0.030 LATT 1 SFAC C H N O MN CL UNIT 64 68 8 12 1 14 MERG 2 FMAP 2 PLAN 10 SIZE 0.06 0.05 0.03 ACTA L.S. 8 TEMP -153.00 WGHT 0.085200 3.674900 FVAR 0.17671 MN 5 1.000000 0.000000 0.500000 10.50000 0.01233 0.00817 = 0.01044 0.00459 0.00741 0.00405 CL3 6 0.632172 -0.393355 0.189219 11.00000 0.07604 0.03894 = 0.04533 0.01329 0.03996 0.00509 CL7 6 1.127865 -0.155025 0.205526 11.00000 0.07511 0.06093 = 0.05410 0.03934 0.04259 0.04522 CL4 6 0.725149 -0.434137 0.025558 11.00000 0.07673 0.04635 = 0.05903 0.02444 0.04734 0.03403 CL2 6 0.556143 -0.307005 0.008939 11.00000 0.05451 0.04759 = 0.04752 0.01240 0.01245 0.02178 CL6 6 1.107630 0.055233 0.183052 11.00000 0.06990 0.02799 = 0.06686 0.02026 0.04867 0.01540 N1 3 1.221844 0.524727 0.433304 11.00000 0.01411 0.00617 = 0.01072 0.00237 0.00786 0.00333 CL5 6 0.897729 -0.139409 0.057016 11.00000 0.04745 0.05264 = 0.03297 -0.00173 0.01701 0.00649 N3 3 1.099600 0.873439 0.458165 11.00000 0.01242 0.01579 = 0.01334 0.00472 0.00579 0.00527 O1 4 1.449940 0.524338 0.294235 11.00000 0.01645 0.01784 = 0.02656 0.00865 0.01389 0.00567 O2 4 1.445595 0.329908 0.379003 11.00000 0.01828 0.02836 = 0.02721 0.01044 0.01029 0.01381 N2 3 1.086410 0.441731 0.194707 11.00000 0.00987 0.00927 = 0.01003 0.00388 0.00271 0.00197 N4 3 1.095215 0.138952 0.453229 11.00000 0.01615 0.01566 = 0.00878 0.00411 0.00612 0.00742 O3 4 1.313388 0.246476 0.198234 11.00000 0.02157 0.02093 = 0.02624 -0.00305 0.01087 0.01354 O4 4 1.452699 0.769909 0.382006 11.00000 0.02051 0.01653 = 0.02508 0.00837 0.00893 -0.00166 C6 1 1.280777 0.403892 0.300980 11.00000 0.00904 0.00772 = 0.01169 0.00225 0.00613 0.00184 C5 1 1.278406 0.435406 0.417000 11.00000 0.01096 0.00692 = 0.01071 0.00414 0.00272 0.00111 AFIX 13 H5 2 1.364644 0.463147 0.475800 11.00000 -1.20000 AFIX 0 O5 4 1.328537 0.705297 0.198460 11.00000 0.01916 0.02813 = 0.02252 0.01709 0.00686 -0.00466 C22 1 1.211435 0.332464 0.429481 11.00000 0.01164 0.00733 = 0.00792 0.00125 0.00654 0.00329 C4 1 1.280817 0.624495 0.416878 11.00000 0.01040 0.01167 = 0.00561 0.00376 0.00207 0.00286 AFIX 13 H4 2 1.366763 0.657193 0.476312 11.00000 -1.20000 AFIX 0 C20 1 1.282969 0.821503 0.495977 11.00000 0.00813 0.01510 = 0.01639 0.00294 0.00319 0.00093 AFIX 43 H20 2 1.369590 0.843685 0.532119 11.00000 -1.20000 AFIX 0 C29 1 1.364493 0.700840 0.300381 11.00000 0.01343 0.01450 = 0.02471 0.00990 0.01261 0.00936 C23 1 1.083262 0.288329 0.379191 11.00000 0.01672 0.01257 = 0.01309 0.00816 0.00913 0.00721 AFIX 43 H23 2 1.033942 0.324014 0.337051 11.00000 -1.20000 AFIX 0 C2 1 1.159346 0.545365 0.195661 11.00000 0.01571 0.01155 = 0.01211 0.00462 0.00957 0.00400 AFIX 23 H2A 2 1.113692 0.600129 0.193072 11.00000 -1.20000 H2B 2 1.173357 0.529381 0.129760 11.00000 -1.20000 AFIX 0 C21 1 1.221377 0.898191 0.508493 11.00000 0.02430 0.00979 = 0.01996 0.00315 0.01254 0.00308 AFIX 43 H21 2 1.268227 0.972736 0.555531 11.00000 -1.20000 AFIX 0 C27 1 1.355401 0.323150 0.299194 11.00000 0.01287 0.01456 = 0.02073 0.00906 0.01261 0.00391 C7 1 1.153536 0.359590 0.197496 11.00000 0.01749 0.00908 = 0.00962 0.00273 0.00894 0.00705 AFIX 23 H7A 2 1.165448 0.340811 0.130561 11.00000 -1.20000 H7B 2 1.104255 0.290485 0.197278 11.00000 -1.20000 AFIX 0 C8 1 0.966674 0.394832 0.094327 11.00000 0.01082 0.01663 = 0.01197 0.00307 0.00266 0.00345 AFIX 23 H8A 2 0.978187 0.355307 0.031198 11.00000 -1.20000 H8B 2 0.935578 0.456510 0.078214 11.00000 -1.20000 AFIX 0 C24 1 1.029568 0.192354 0.391652 11.00000 0.00873 0.01779 = 0.01367 0.00475 0.00682 0.00232 AFIX 43 H24 2 0.943104 0.162532 0.355606 11.00000 -1.20000 AFIX 0 C19 1 1.215222 0.710968 0.429196 11.00000 0.01874 0.01143 = 0.01153 0.00760 0.00996 0.00482 C17 1 1.034088 0.766419 0.393710 11.00000 0.01417 0.01375 = 0.01403 0.00421 0.00794 0.00285 AFIX 43 H17 2 0.947664 0.747247 0.357594 11.00000 -1.20000 AFIX 0 O6 4 0.615065 0.109292 0.159282 11.00000 0.02296 0.03604 = 0.03723 0.02059 0.01732 0.00231 C3 1 1.285138 0.596211 0.301277 11.00000 0.00924 0.00929 = 0.01835 0.00555 0.00560 0.00281 C1 1 1.353142 0.510139 0.298371 11.00000 0.01293 0.01190 = 0.00650 0.00344 0.00397 0.00318 C25 1 1.218582 0.184364 0.502272 11.00000 0.01529 0.01736 = 0.02177 0.01374 0.00848 0.00985 AFIX 43 H25 2 1.266308 0.149135 0.546374 11.00000 -1.20000 AFIX 0 C18 1 1.087604 0.683011 0.377875 11.00000 0.01624 0.00692 = 0.01187 0.00278 0.00724 0.00157 AFIX 43 H18 2 1.038470 0.608387 0.333040 11.00000 -1.20000 AFIX 0 C26 1 1.279500 0.278589 0.492313 11.00000 0.00673 0.01703 = 0.01975 0.00634 0.00521 0.00467 AFIX 43 H26 2 1.366126 0.305834 0.527756 11.00000 -1.20000 AFIX 0 C14 1 0.854655 0.201045 0.074883 11.00000 0.00755 0.02173 = 0.02019 0.00051 0.00537 0.00240 AFIX 43 H14 2 0.899531 0.171039 0.040373 11.00000 -1.20000 AFIX 0 C9 1 0.873737 0.315009 0.107875 11.00000 0.00720 0.01948 = 0.00884 0.00303 -0.00188 0.00007 C33 1 1.237124 0.558882 0.549283 11.00000 0.02542 0.01439 = 0.01077 0.00587 0.01006 0.00592 AFIX 133 H33A 2 1.193135 0.495540 0.559989 11.00000 -1.20000 H33B 2 1.204187 0.620797 0.562291 11.00000 -1.20000 H33C 2 1.323976 0.582495 0.600901 11.00000 -1.20000 AFIX 0 C13 1 0.770465 0.129082 0.091383 11.00000 0.01257 0.01209 = 0.02575 0.00317 0.00426 0.00176 AFIX 43 H13 2 0.759606 0.051341 0.068749 11.00000 -1.20000 AFIX 0 C10 1 0.804712 0.355951 0.158888 11.00000 0.01697 0.01496 = 0.01841 0.00226 0.00515 0.00195 AFIX 43 H10 2 0.816841 0.433871 0.182938 11.00000 -1.20000 AFIX 0 C12 1 0.702364 0.171217 0.141025 11.00000 0.01100 0.02850 = 0.02075 0.01290 0.00632 0.00444 C11 1 0.720239 0.286359 0.174891 11.00000 0.01604 0.03025 = 0.01797 0.00239 0.01149 0.00865 AFIX 43 H11 2 0.674656 0.316320 0.208572 11.00000 -1.20000 AFIX 0 C32 1 1.034499 -0.070696 0.187085 11.00000 0.03456 0.02674 = 0.02999 0.00590 0.02359 0.00890 AFIX 13 H32 2 1.011233 -0.055410 0.248351 11.00000 -1.20000 AFIX 0 C28 1 1.387289 0.173102 0.190853 11.00000 0.03226 0.03294 = 0.04509 -0.00308 0.01376 0.02200 AFIX 133 H28A 2 1.473283 0.217785 0.224668 11.00000 -1.20000 H28B 2 1.360789 0.130942 0.113570 11.00000 -1.20000 H28C 2 1.377475 0.121253 0.229360 11.00000 -1.20000 AFIX 0 C31 1 0.676517 -0.338537 0.101557 11.00000 0.03869 0.02513 = 0.03297 0.00531 0.01764 0.00397 AFIX 13 H31 2 0.746291 -0.268254 0.147766 11.00000 -1.20000 AFIX 0 CL1 6 0.835361 -0.083809 0.306672 11.00000 0.01546 0.01621 = 0.01163 0.00358 0.00466 0.00468 C30 1 1.405376 0.797654 0.188569 11.00000 0.02927 0.03147 = 0.04564 0.02583 0.01822 -0.00148 AFIX 133 H30A 2 1.419126 0.867699 0.243757 11.00000 -1.20000 H30B 2 1.364573 0.801683 0.115098 11.00000 -1.20000 H30C 2 1.483871 0.785409 0.200231 11.00000 -1.20000 AFIX 0 C34 1 0.595143 -0.008253 0.127560 11.00000 0.02521 0.03634 = 0.06008 0.03707 0.01498 0.00659 AFIX 133 H34A 2 0.597237 -0.035079 0.057176 11.00000 -1.20000 H34B 2 0.515340 -0.045915 0.120142 11.00000 -1.20000 H34C 2 0.659190 -0.024374 0.183608 11.00000 -1.20000 AFIX 0 HKLF 4 REM TCMnw in P-1 REM R1 = 0.0636 for 3896 Fo > 4sig(Fo) and 0.0995 for all 5616 data REM 448 parameters refined using 0 restraints END WGHT 0.0853 3.6700 REM Highest difference peak 1.835, deepest hole -0.696, 1-sigma level 0.098 Q1 1 1.2069 -0.0767 0.2687 11.00000 0.05 1.84 Q2 1 0.9623 -0.1985 0.1142 11.00000 0.05 1.73 Q3 1 1.0183 -0.0018 0.1221 11.00000 0.05 0.98 Q4 1 0.8114 -0.3789 0.0972 11.00000 0.05 0.55 Q5 1 0.9983 0.0730 0.4850 11.00000 0.05 0.36 Q6 1 0.9437 -0.0216 0.4479 11.00000 0.05 0.35 Q7 1 1.1529 0.2985 0.3908 11.00000 0.05 0.34 Q8 1 1.4757 0.8249 0.2401 11.00000 0.05 0.33 Q9 1 0.6426 -0.3959 0.0033 11.00000 0.05 0.32 Q10 1 0.7640 0.1557 0.1459 11.00000 0.05 0.32 ; _shelx_res_checksum 1271 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 Mn Mn 1.000000 0.000000 0.500000 0.0091(3) Uani 1 2 d S . P . . Cl3 Cl 0.6322(2) -0.39336(16) 0.18922(17) 0.0514(6) Uani 1 1 d . . . . . Cl7 Cl 1.1279(2) -0.15502(18) 0.20553(17) 0.0512(6) Uani 1 1 d . . . . . Cl4 Cl 0.7251(2) -0.43414(17) 0.02556(18) 0.0515(6) Uani 1 1 d . . . . . Cl2 Cl 0.5561(2) -0.30701(17) 0.00894(17) 0.0534(6) Uani 1 1 d . . . . . Cl6 Cl 1.1076(2) 0.05523(15) 0.18305(18) 0.0481(6) Uani 1 1 d . . . . . N1 N 1.2218(4) 0.5247(4) 0.4333(4) 0.0096(10) Uani 1 1 d . . . . . Cl5 Cl 0.89773(18) -0.13941(17) 0.05702(16) 0.0494(5) Uani 1 1 d . . . . . N3 N 1.0996(4) 0.8734(4) 0.4582(4) 0.0138(11) Uani 1 1 d . . . . . O1 O 1.4499(4) 0.5243(3) 0.2942(3) 0.0186(9) Uani 1 1 d . . . . . O2 O 1.4456(4) 0.3299(3) 0.3790(3) 0.0234(10) Uani 1 1 d . . . . . N2 N 1.0864(4) 0.4417(4) 0.1947(4) 0.0104(10) Uani 1 1 d . . . . . N4 N 1.0952(4) 0.1390(4) 0.4532(4) 0.0130(11) Uani 1 1 d . . . . . O3 O 1.3134(4) 0.2465(3) 0.1982(3) 0.0241(10) Uani 1 1 d . . . . . O4 O 1.4527(4) 0.7699(3) 0.3820(3) 0.0221(10) Uani 1 1 d . . . . . C6 C 1.2808(5) 0.4039(4) 0.3010(4) 0.0093(12) Uani 1 1 d . . . . . C5 C 1.2784(5) 0.4354(4) 0.4170(4) 0.0103(12) Uani 1 1 d . . . . . H5 H 1.364644 0.463147 0.475800 0.012 Uiso 1 1 calc R U . . . O5 O 1.3285(4) 0.7053(3) 0.1985(3) 0.0243(10) Uani 1 1 d . . . . . C22 C 1.2114(5) 0.3325(4) 0.4295(4) 0.0085(12) Uani 1 1 d . . . . . C4 C 1.2808(5) 0.6245(4) 0.4169(4) 0.0097(12) Uani 1 1 d . . . . . H4 H 1.366763 0.657193 0.476312 0.012 Uiso 1 1 calc R U . . . C20 C 1.2830(5) 0.8215(5) 0.4960(5) 0.0149(13) Uani 1 1 d . . . . . H20 H 1.369590 0.843685 0.532119 0.018 Uiso 1 1 calc R U . . . C29 C 1.3645(5) 0.7008(5) 0.3004(5) 0.0148(13) Uani 1 1 d . . . . . C23 C 1.0833(5) 0.2883(4) 0.3792(4) 0.0122(13) Uani 1 1 d . . . . . H23 H 1.033942 0.324014 0.337051 0.015 Uiso 1 1 calc R U . . . C2 C 1.1593(5) 0.5454(4) 0.1957(5) 0.0119(12) Uani 1 1 d . . . . . H2A H 1.113692 0.600129 0.193072 0.014 Uiso 1 1 calc R U . . . H2B H 1.173357 0.529381 0.129760 0.014 Uiso 1 1 calc R U . . . C21 C 1.2214(5) 0.8982(5) 0.5085(5) 0.0179(14) Uani 1 1 d . . . . . H21 H 1.268227 0.972736 0.555531 0.021 Uiso 1 1 calc R U . . . C27 C 1.3554(5) 0.3231(5) 0.2992(5) 0.0138(13) Uani 1 1 d . . . . . C7 C 1.1535(5) 0.3596(4) 0.1975(4) 0.0108(12) Uani 1 1 d . . . . . H7A H 1.165448 0.340811 0.130561 0.013 Uiso 1 1 calc R U . . . H7B H 1.104255 0.290485 0.197278 0.013 Uiso 1 1 calc R U . . . C8 C 0.9667(5) 0.3948(5) 0.0943(5) 0.0145(13) Uani 1 1 d . . . . . H8A H 0.978187 0.355307 0.031198 0.017 Uiso 1 1 calc R U . . . H8B H 0.935578 0.456510 0.078214 0.017 Uiso 1 1 calc R U . . . C24 C 1.0296(5) 0.1924(5) 0.3917(5) 0.0132(13) Uani 1 1 d . . . . . H24 H 0.943104 0.162532 0.355606 0.016 Uiso 1 1 calc R U . . . C19 C 1.2152(5) 0.7110(4) 0.4292(4) 0.0121(13) Uani 1 1 d . . . . . C17 C 1.0341(5) 0.7664(5) 0.3937(5) 0.0138(13) Uani 1 1 d . . . . . H17 H 0.947664 0.747247 0.357594 0.017 Uiso 1 1 calc R U . . . O6 O 0.6151(4) 0.1093(4) 0.1593(4) 0.0302(11) Uani 1 1 d . . . . . C3 C 1.2851(5) 0.5962(4) 0.3013(5) 0.0124(13) Uani 1 1 d . . . . . C1 C 1.3531(5) 0.5101(4) 0.2984(4) 0.0106(12) Uani 1 1 d . . . . . C25 C 1.2186(5) 0.1844(5) 0.5023(5) 0.0160(14) Uani 1 1 d . . . . . H25 H 1.266308 0.149135 0.546374 0.019 Uiso 1 1 calc R U . . . C18 C 1.0876(5) 0.6830(4) 0.3779(4) 0.0118(13) Uani 1 1 d . . . . . H18 H 1.038470 0.608387 0.333040 0.014 Uiso 1 1 calc R U . . . C26 C 1.2795(5) 0.2786(5) 0.4923(5) 0.0146(13) Uani 1 1 d . . . . . H26 H 1.366126 0.305834 0.527756 0.018 Uiso 1 1 calc R U . . . C14 C 0.8547(5) 0.2010(5) 0.0749(5) 0.0185(14) Uani 1 1 d . . . . . H14 H 0.899531 0.171039 0.040373 0.022 Uiso 1 1 calc R U . . . C9 C 0.8737(5) 0.3150(5) 0.1079(4) 0.0147(13) Uani 1 1 d . . . . . C33 C 1.2371(6) 0.5589(5) 0.5493(4) 0.0159(13) Uani 1 1 d . . . . . H33A H 1.193135 0.495540 0.559989 0.019 Uiso 1 1 calc R U . . . H33B H 1.204187 0.620797 0.562291 0.019 Uiso 1 1 calc R U . . . H33C H 1.323976 0.582495 0.600901 0.019 Uiso 1 1 calc R U . . . C13 C 0.7705(5) 0.1291(5) 0.0914(5) 0.0193(14) Uani 1 1 d . . . . . H13 H 0.759606 0.051341 0.068749 0.023 Uiso 1 1 calc R U . . . C10 C 0.8047(5) 0.3560(5) 0.1589(5) 0.0189(14) Uani 1 1 d . . . . . H10 H 0.816841 0.433871 0.182938 0.023 Uiso 1 1 calc R U . . . C12 C 0.7024(5) 0.1712(5) 0.1410(5) 0.0197(14) Uani 1 1 d . . . . . C11 C 0.7202(5) 0.2864(5) 0.1749(5) 0.0211(14) Uani 1 1 d . . . . . H11 H 0.674656 0.316320 0.208572 0.025 Uiso 1 1 calc R U . . . C32 C 1.0345(6) -0.0707(5) 0.1871(6) 0.0282(16) Uani 1 1 d . . . . . H32 H 1.011233 -0.055410 0.248351 0.034 Uiso 1 1 calc R U . . . C28 C 1.3873(7) 0.1731(6) 0.1909(6) 0.0395(19) Uani 1 1 d . . . . . H28A H 1.473283 0.217785 0.224668 0.047 Uiso 1 1 calc R U . . . H28B H 1.360789 0.130942 0.113570 0.047 Uiso 1 1 calc R U . . . H28C H 1.377475 0.121253 0.229360 0.047 Uiso 1 1 calc R U . . . C31 C 0.6765(7) -0.3385(6) 0.1016(6) 0.0336(17) Uani 1 1 d . . . . . H31 H 0.746291 -0.268254 0.147766 0.040 Uiso 1 1 calc R U . . . Cl1 Cl 0.83536(12) -0.08381(11) 0.30667(11) 0.0152(4) Uani 1 1 d . . . . . C30 C 1.4054(6) 0.7977(6) 0.1886(6) 0.0341(18) Uani 1 1 d . . . . . H30A H 1.419126 0.867699 0.243757 0.041 Uiso 1 1 calc R U . . . H30B H 1.364573 0.801683 0.115098 0.041 Uiso 1 1 calc R U . . . H30C H 1.483871 0.785409 0.200231 0.041 Uiso 1 1 calc R U . . . C34 C 0.5951(6) -0.0083(6) 0.1276(6) 0.0383(19) Uani 1 1 d . . . . . H34A H 0.597237 -0.035079 0.057176 0.046 Uiso 1 1 calc R U . . . H34B H 0.515340 -0.045915 0.120142 0.046 Uiso 1 1 calc R U . . . H34C H 0.659190 -0.024374 0.183608 0.046 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 0.0123(7) 0.0082(6) 0.0104(7) 0.0046(5) 0.0074(5) 0.0040(5) Cl3 0.0760(15) 0.0389(12) 0.0453(12) 0.0133(9) 0.0400(11) 0.0051(10) Cl7 0.0751(15) 0.0609(14) 0.0541(13) 0.0393(11) 0.0426(12) 0.0452(12) Cl4 0.0767(15) 0.0464(12) 0.0590(14) 0.0244(10) 0.0473(12) 0.0340(11) Cl2 0.0545(13) 0.0476(12) 0.0475(13) 0.0124(10) 0.0125(10) 0.0218(10) Cl6 0.0699(15) 0.0280(11) 0.0669(14) 0.0203(10) 0.0487(12) 0.0154(10) N1 0.014(3) 0.006(2) 0.011(3) 0.002(2) 0.008(2) 0.003(2) Cl5 0.0474(13) 0.0526(13) 0.0330(11) -0.0017(9) 0.0170(10) 0.0065(10) N3 0.012(3) 0.016(3) 0.013(3) 0.005(2) 0.006(2) 0.005(2) O1 0.016(2) 0.018(2) 0.027(2) 0.0086(19) 0.014(2) 0.0057(18) O2 0.018(3) 0.028(3) 0.027(3) 0.010(2) 0.010(2) 0.014(2) N2 0.010(3) 0.009(2) 0.010(2) 0.004(2) 0.003(2) 0.002(2) N4 0.016(3) 0.016(3) 0.009(3) 0.004(2) 0.006(2) 0.007(2) O3 0.022(2) 0.021(2) 0.026(3) -0.003(2) 0.011(2) 0.014(2) O4 0.021(3) 0.017(2) 0.025(3) 0.008(2) 0.009(2) -0.002(2) C6 0.009(3) 0.008(3) 0.012(3) 0.002(2) 0.006(2) 0.002(2) C5 0.011(3) 0.007(3) 0.011(3) 0.004(2) 0.003(3) 0.001(2) O5 0.019(2) 0.028(3) 0.023(2) 0.017(2) 0.007(2) -0.0047(19) C22 0.012(3) 0.007(3) 0.008(3) 0.001(2) 0.007(2) 0.003(2) C4 0.010(3) 0.012(3) 0.006(3) 0.004(2) 0.002(2) 0.003(2) C20 0.008(3) 0.015(3) 0.016(3) 0.003(3) 0.003(3) 0.001(3) C29 0.013(3) 0.015(3) 0.025(4) 0.010(3) 0.013(3) 0.009(3) C23 0.017(3) 0.013(3) 0.013(3) 0.008(3) 0.009(3) 0.007(3) C2 0.016(3) 0.012(3) 0.012(3) 0.005(2) 0.010(3) 0.004(3) C21 0.024(4) 0.010(3) 0.020(3) 0.003(3) 0.013(3) 0.003(3) C27 0.013(3) 0.015(3) 0.021(4) 0.009(3) 0.013(3) 0.004(3) C7 0.017(3) 0.009(3) 0.010(3) 0.003(2) 0.009(3) 0.007(2) C8 0.011(3) 0.017(3) 0.012(3) 0.003(3) 0.003(3) 0.003(3) C24 0.009(3) 0.018(3) 0.014(3) 0.005(3) 0.007(3) 0.002(3) C19 0.019(4) 0.011(3) 0.012(3) 0.008(3) 0.010(3) 0.005(3) C17 0.014(3) 0.014(3) 0.014(3) 0.004(3) 0.008(3) 0.003(3) O6 0.023(3) 0.036(3) 0.037(3) 0.021(2) 0.017(2) 0.002(2) C3 0.009(3) 0.009(3) 0.018(3) 0.006(3) 0.006(3) 0.003(2) C1 0.013(3) 0.012(3) 0.006(3) 0.003(2) 0.004(3) 0.003(2) C25 0.015(4) 0.017(3) 0.022(3) 0.014(3) 0.008(3) 0.010(3) C18 0.016(3) 0.007(3) 0.012(3) 0.003(2) 0.007(3) 0.002(2) C26 0.007(3) 0.017(3) 0.020(3) 0.006(3) 0.005(3) 0.005(3) C14 0.008(3) 0.022(4) 0.020(3) 0.001(3) 0.005(3) 0.002(3) C9 0.007(3) 0.019(3) 0.009(3) 0.003(3) -0.002(2) 0.000(3) C33 0.025(4) 0.014(3) 0.011(3) 0.006(3) 0.010(3) 0.006(3) C13 0.013(3) 0.012(3) 0.026(4) 0.003(3) 0.004(3) 0.002(3) C10 0.017(3) 0.015(3) 0.018(3) 0.002(3) 0.005(3) 0.002(3) C12 0.011(3) 0.028(4) 0.021(4) 0.013(3) 0.006(3) 0.004(3) C11 0.016(4) 0.030(4) 0.018(3) 0.002(3) 0.011(3) 0.009(3) C32 0.035(4) 0.027(4) 0.030(4) 0.006(3) 0.024(3) 0.009(3) C28 0.032(4) 0.033(4) 0.045(5) -0.003(4) 0.014(4) 0.022(4) C31 0.039(5) 0.025(4) 0.033(4) 0.005(3) 0.018(4) 0.004(3) Cl1 0.0155(8) 0.0162(8) 0.0116(8) 0.0036(6) 0.0047(6) 0.0047(6) C30 0.029(4) 0.031(4) 0.046(5) 0.026(4) 0.018(4) -0.001(3) C34 0.025(4) 0.036(4) 0.060(5) 0.037(4) 0.015(4) 0.007(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' Mn Mn 0.3368 0.7283 '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' 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 Mn N3 180.0(2) 2_766 1_545 ? N3 Mn N4 96.03(16) 2_766 2_756 ? N3 Mn N4 83.97(16) 1_545 2_756 ? N3 Mn N4 83.97(16) 2_766 . ? N3 Mn N4 96.03(16) 1_545 . ? N4 Mn N4 180.0 2_756 . ? N3 Mn Cl1 90.65(12) 2_766 . ? N3 Mn Cl1 89.35(12) 1_545 . ? N4 Mn Cl1 90.37(12) 2_756 . ? N4 Mn Cl1 89.63(12) . . ? N3 Mn Cl1 89.35(12) 2_766 2_756 ? N3 Mn Cl1 90.65(12) 1_545 2_756 ? N4 Mn Cl1 89.63(12) 2_756 2_756 ? N4 Mn Cl1 90.37(12) . 2_756 ? Cl1 Mn Cl1 180.00(7) . 2_756 ? C5 N1 C4 111.5(4) . . ? C5 N1 C33 108.8(4) . . ? C4 N1 C33 108.2(4) . . ? C21 N3 C17 117.3(5) . . ? C21 N3 Mn 122.2(4) . 1_565 ? C17 N3 Mn 119.8(4) . 1_565 ? C7 N2 C2 109.6(4) . . ? C7 N2 C8 109.6(4) . . ? C2 N2 C8 110.3(4) . . ? C25 N4 C24 116.2(5) . . ? C25 N4 Mn 121.6(3) . . ? C24 N4 Mn 121.0(4) . . ? C27 O3 C28 114.7(5) . . ? C1 C6 C27 106.1(4) . . ? C1 C6 C7 107.4(4) . . ? C27 C6 C7 112.4(4) . . ? C1 C6 C5 106.5(4) . . ? C27 C6 C5 107.8(4) . . ? C7 C6 C5 115.9(4) . . ? N1 C5 C22 109.9(4) . . ? N1 C5 C6 112.3(4) . . ? C22 C5 C6 110.6(4) . . ? C29 O5 C30 115.6(5) . . ? C26 C22 C23 118.0(5) . . ? C26 C22 C5 118.9(5) . . ? C23 C22 C5 123.1(4) . . ? N1 C4 C19 109.2(4) . . ? N1 C4 C3 113.1(4) . . ? C19 C4 C3 110.8(4) . . ? C21 C20 C19 118.7(5) . . ? O4 C29 O5 124.0(5) . . ? O4 C29 C3 124.0(5) . . ? O5 C29 C3 111.9(5) . . ? C24 C23 C22 119.5(5) . . ? N2 C2 C3 110.9(4) . . ? N3 C21 C20 123.9(5) . . ? O2 C27 O3 123.7(5) . . ? O2 C27 C6 123.5(5) . . ? O3 C27 C6 112.8(5) . . ? N2 C7 C6 112.2(4) . . ? N2 C8 C9 111.8(4) . . ? N4 C24 C23 123.0(5) . . ? C20 C19 C18 118.2(5) . . ? C20 C19 C4 119.6(5) . . ? C18 C19 C4 122.2(5) . . ? N3 C17 C18 122.9(5) . . ? C12 O6 C34 116.8(5) . . ? C1 C3 C29 106.3(4) . . ? C1 C3 C2 107.0(4) . . ? C29 C3 C2 111.4(4) . . ? C1 C3 C4 106.3(4) . . ? C29 C3 C4 108.6(4) . . ? C2 C3 C4 116.7(4) . . ? O1 C1 C6 125.4(5) . . ? O1 C1 C3 125.1(5) . . ? C6 C1 C3 109.5(5) . . ? N4 C25 C26 124.5(5) . . ? C17 C18 C19 118.9(5) . . ? C25 C26 C22 118.8(5) . . ? C9 C14 C13 121.4(5) . . ? C14 C9 C10 117.3(5) . . ? C14 C9 C8 122.5(5) . . ? C10 C9 C8 120.2(5) . . ? C12 C13 C14 120.3(5) . . ? C11 C10 C9 122.3(5) . . ? O6 C12 C13 125.9(5) . . ? O6 C12 C11 114.9(5) . . ? C13 C12 C11 119.1(5) . . ? C10 C11 C12 119.5(5) . . ? Cl7 C32 Cl6 111.2(4) . . ? Cl7 C32 Cl5 109.9(4) . . ? Cl6 C32 Cl5 107.1(4) . . ? Cl2 C31 Cl3 111.2(4) . . ? Cl2 C31 Cl4 108.9(4) . . ? Cl3 C31 Cl4 111.3(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 N3 2.336(4) 2_766 ? Mn N3 2.336(4) 1_545 ? Mn N4 2.345(5) 2_756 ? Mn N4 2.345(5) . ? Mn Cl1 2.4983(19) . ? Mn Cl1 2.4983(19) 2_756 ? Cl3 C31 1.773(7) . ? Cl7 C32 1.734(7) . ? Cl4 C31 1.788(7) . ? Cl2 C31 1.761(7) . ? Cl6 C32 1.747(7) . ? N1 C5 1.483(7) . ? N1 C4 1.484(7) . ? N1 C33 1.509(7) . ? Cl5 C32 1.817(7) . ? N3 C21 1.341(7) . ? N3 C17 1.352(7) . ? O1 C1 1.216(6) . ? O2 C27 1.215(7) . ? N2 C7 1.473(6) . ? N2 C2 1.475(7) . ? N2 C8 1.490(7) . ? N4 C25 1.359(7) . ? N4 C24 1.363(7) . ? O3 C27 1.355(7) . ? O3 C28 1.458(7) . ? O4 C29 1.225(7) . ? C6 C1 1.522(8) . ? C6 C27 1.529(8) . ? C6 C7 1.565(8) . ? C6 C5 1.598(8) . ? C5 C22 1.529(7) . ? O5 C29 1.347(7) . ? O5 C30 1.464(7) . ? C22 C26 1.390(7) . ? C22 C23 1.409(8) . ? C4 C19 1.524(7) . ? C4 C3 1.604(8) . ? C20 C21 1.386(8) . ? C20 C19 1.397(8) . ? C29 C3 1.535(8) . ? C23 C24 1.388(8) . ? C2 C3 1.567(8) . ? C8 C9 1.512(8) . ? C19 C18 1.403(8) . ? C17 C18 1.393(8) . ? O6 C12 1.378(7) . ? O6 C34 1.429(8) . ? C3 C1 1.527(8) . ? C25 C26 1.386(8) . ? C14 C9 1.386(8) . ? C14 C13 1.403(8) . ? C9 C10 1.417(8) . ? C13 C12 1.400(8) . ? C10 C11 1.384(8) . ? C12 C11 1.403(9) . ?