# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name _publ_author_address 'S.El Ghachtouli' ;Institut de Chimie Mol\'eculaire et des Mat\'eriaux d'Orsay UMR 8182 - B\^at. 420 Universit\'e Paris-Sud 11 15 rue Georges Clemenceau 91405 Orsay Cedex, France ; R.Guillot ;Institut de Chimie Mol\'eculaire et des Mat\'eriaux d'Orsay UMR 8182 - B\^at. 420 Universit\'e Paris-Sud 11 15 rue Georges Clemenceau 91405 Orsay Cedex, France ; P.Dorlet ;Laboratoire du Stress Oxydant et Detoxication CNRS URA 2096 IBITEC-S CEA Saclay B\^at 532 Pce 126A 91191 Gif-sur-Yvette Cedex ; E.Anxolabehere-Mallart ;Laboratoire d'Electrochimie Mol\'eculaire UMR CNRS - P7 7591 Universit\'e Paris Diderot - Paris 7 15 rue Jean-Antoine de Ba\"if 75205 Paris Cedex 13, France ; ; A.Aukauloo ; ;Institut de Chimie Mol\'eculaire et des Mat\'eriaux d'Orsay UMR 8182 - B\^at. 420 Universit\'e Paris-Sud 11 15 rue Georges Clemenceau 91405 Orsay Cedex, France ; _publ_contact_author_name 'Prof. Ally Aukauloo' _publ_contact_author_email ally.aukauloo@u-psud.fr _publ_contact_author_address ;Institut de Chimie Mol\'eculaire et des Mat\'eriaux d'Orsay UMR 8182 - B\^at. 420 Universit\'e Paris-Sud 11 15 rue Georges Clemenceau 91405 Orsay Cedex, France ; _publ_section_title ; Influence of second sphere hydrogen bonding interaction on a manganese(II)-aquo complex ; # Attachment '- 938GuillotICMMOver2.cif' data_938GuillotICMMO _database_code_depnum_ccdc_archive 'CCDC 817802' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety '2(C32 H36 Mn N6 O2), C H4 O, 4(Cl O4)' _chemical_formula_sum 'C65 H76 Cl4 Mn2 N12 O21' _chemical_melting_point ? _exptl_crystal_description column _exptl_crystal_colour yellow-brown _diffrn_ambient_temperature 100(1) _chemical_formula_weight 1613.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0031 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 0.0109 0.0061 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1480 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3370 0.7280 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_int_tables_number 14 _chemical_absolute_configuration . loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.0226(7) _cell_length_b 16.6220(17) _cell_length_c 25.429(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.063(2) _cell_angle_gamma 90.00 _cell_volume 3755.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 5168 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 24.34 _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 0.557 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.8502 _exptl_absorpt_correction_T_max 0.9605 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed X-ray tube' _diffrn_source_type 'kappa X8 APEX II Bruker ICMMO' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52480 _diffrn_reflns_av_R_equivalents 0.0998 _diffrn_reflns_av_sigmaI/netI 0.0819 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 28.22 _reflns_number_total 9098 _reflns_number_gt 5284 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1370P)^2^+12.8026P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 9098 _refine_ls_number_parameters 513 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1387 _refine_ls_R_factor_gt 0.0747 _refine_ls_wR_factor_ref 0.2170 _refine_ls_wR_factor_gt 0.1792 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1068(6) 0.4035(3) 0.7640(2) 0.0300(11) Uani 1 1 d . . . H1 H 0.1299 0.4172 0.8000 0.036 Uiso 1 1 calc R . . C2 C -0.0291(6) 0.4272(3) 0.7354(2) 0.0375(13) Uani 1 1 d . . . H2 H -0.0971 0.4559 0.7517 0.045 Uiso 1 1 calc R . . C3 C -0.0635(7) 0.4078(4) 0.6819(3) 0.0447(15) Uani 1 1 d . . . H3 H -0.1546 0.4233 0.6614 0.054 Uiso 1 1 calc R . . C4 C 0.0404(7) 0.3647(4) 0.6594(3) 0.0455(16) Uani 1 1 d . . . H4 H 0.0199 0.3510 0.6234 0.055 Uiso 1 1 calc R . . C5 C 0.1744(6) 0.3420(4) 0.6904(2) 0.0335(12) Uani 1 1 d . . . C6 C 0.2952(6) 0.2979(4) 0.6670(2) 0.0381(13) Uani 1 1 d . . . H6A H 0.2474 0.2631 0.6384 0.046 Uiso 1 1 calc R . . H6B H 0.3557 0.3369 0.6518 0.046 Uiso 1 1 calc R . . C7 C 0.7617(6) 0.2923(4) 0.8249(3) 0.0386(13) Uani 1 1 d . . . H7 H 0.7437 0.3209 0.8546 0.046 Uiso 1 1 calc R . . C8 C 0.9018(7) 0.2617(5) 0.8252(3) 0.0556(19) Uani 1 1 d . . . H8 H 0.9790 0.2704 0.8541 0.067 Uiso 1 1 calc R . . C9 C 0.9260(7) 0.2176(5) 0.7819(4) 0.063(2) Uani 1 1 d . . . H9 H 1.0201 0.1949 0.7815 0.076 Uiso 1 1 calc R . . C10 C 0.8122(7) 0.2069(4) 0.7393(3) 0.0510(18) Uani 1 1 d . . . H10 H 0.8286 0.1770 0.7099 0.061 Uiso 1 1 calc R . . C11 C 0.6707(6) 0.2413(3) 0.7401(3) 0.0360(13) Uani 1 1 d . . . C12 C 0.5451(6) 0.2375(4) 0.6935(3) 0.0414(14) Uani 1 1 d . . . H12A H 0.5619 0.2781 0.6678 0.050 Uiso 1 1 calc R . . H12B H 0.5476 0.1854 0.6765 0.050 Uiso 1 1 calc R . . C13 C 0.3212(7) 0.1714(4) 0.7152(2) 0.0401(14) Uani 1 1 d . . . H13A H 0.3355 0.1345 0.6870 0.048 Uiso 1 1 calc R . . H13B H 0.2139 0.1795 0.7131 0.048 Uiso 1 1 calc R . . C14 C 0.3858(7) 0.1348(4) 0.7687(3) 0.0398(14) Uani 1 1 d . . . H14A H 0.3336 0.0851 0.7738 0.048 Uiso 1 1 calc R . . H14B H 0.4917 0.1227 0.7702 0.048 Uiso 1 1 calc R . . C15 C 0.3117(5) 0.1674(3) 0.8504(2) 0.0275(11) Uani 1 1 d . . . H15 H 0.2924 0.1126 0.8520 0.033 Uiso 1 1 calc R . . C16 C 0.2760(5) 0.2174(3) 0.8936(2) 0.0255(10) Uani 1 1 d . . . C17 C 0.3093(5) 0.3014(3) 0.89776(19) 0.0235(10) Uani 1 1 d . . . C18 C 0.2565(5) 0.3441(3) 0.93956(19) 0.0232(10) Uani 1 1 d . . . C19 C 0.1806(6) 0.3047(3) 0.9750(2) 0.0273(11) Uani 1 1 d . . . H19 H 0.1476 0.3343 1.0018 0.033 Uiso 1 1 calc R . . C20 C 0.1522(6) 0.2222(3) 0.9719(2) 0.0273(11) Uani 1 1 d . A . C21 C 0.2016(5) 0.1803(3) 0.9305(2) 0.0272(10) Uani 1 1 d . . . H21 H 0.1839 0.1252 0.9276 0.033 Uiso 1 1 calc R . . C22 C 0.2920(5) 0.4286(3) 0.94580(19) 0.0241(10) Uani 1 1 d . . . C23 C 0.3199(6) 0.5533(3) 0.9772(2) 0.0280(11) Uani 1 1 d . . . C24 C 0.3902(6) 0.5481(3) 0.9328(2) 0.0269(11) Uani 1 1 d . . . C25 C 0.4677(6) 0.6126(3) 0.9156(2) 0.0357(12) Uani 1 1 d . . . H25 H 0.5149 0.6088 0.8860 0.043 Uiso 1 1 calc R . . C26 C 0.4707(7) 0.6827(3) 0.9451(2) 0.0384(13) Uani 1 1 d . . . H26 H 0.5215 0.7273 0.9351 0.046 Uiso 1 1 calc R . . C27 C 0.4000(7) 0.6881(3) 0.9891(2) 0.0386(14) Uani 1 1 d . . . H27 H 0.4049 0.7365 1.0077 0.046 Uiso 1 1 calc R . . C28 C 0.3224(6) 0.6245(3) 1.0064(2) 0.0355(12) Uani 1 1 d . . . H28 H 0.2747 0.6289 1.0359 0.043 Uiso 1 1 calc R . . C29 C 0.0734(7) 0.1787(3) 1.0121(2) 0.0362(13) Uani 1 1 d . . . C30A C 0.0492(12) 0.0886(6) 0.9992(4) 0.029(2) Uani 0.50 1 d P A 1 H30A H -0.0070 0.0647 1.0239 0.043 Uiso 0.50 1 calc PR A 1 H30B H 0.1451 0.0623 1.0021 0.043 Uiso 0.50 1 calc PR A 1 H30C H -0.0055 0.0826 0.9635 0.043 Uiso 0.50 1 calc PR A 1 C31A C 0.1876(11) 0.1790(6) 1.0683(4) 0.027(2) Uani 0.50 1 d P A 1 H31A H 0.2828 0.1571 1.0635 0.040 Uiso 0.50 1 calc PR A 1 H31C H 0.1466 0.1470 1.0937 0.040 Uiso 0.50 1 calc PR A 1 H31B H 0.2015 0.2332 1.0812 0.040 Uiso 0.50 1 calc PR A 1 C32A C -0.0675(11) 0.2188(6) 1.0183(5) 0.028(2) Uani 0.50 1 d P A 1 H32A H -0.1084 0.1933 1.0465 0.042 Uiso 0.50 1 calc PR A 1 H32B H -0.1384 0.2149 0.9856 0.042 Uiso 0.50 1 calc PR A 1 H32C H -0.0479 0.2744 1.0270 0.042 Uiso 0.50 1 calc PR A 1 C30B C 0.1537(19) 0.1132(11) 1.0362(6) 0.067(4) Uani 0.50 1 d P A 2 H30E H 0.0884 0.0799 1.0529 0.100 Uiso 0.50 1 calc PR A 2 H30D H 0.2356 0.1320 1.0627 0.100 Uiso 0.50 1 calc PR A 2 H30F H 0.1927 0.0825 1.0097 0.100 Uiso 0.50 1 calc PR A 2 C31B C 0.021(2) 0.2401(10) 1.0523(6) 0.061(4) Uani 0.50 1 d P A 2 H31D H 0.1070 0.2657 1.0730 0.091 Uiso 0.50 1 calc PR A 2 H31F H -0.0341 0.2119 1.0758 0.091 Uiso 0.50 1 calc PR A 2 H31E H -0.0433 0.2801 1.0327 0.091 Uiso 0.50 1 calc PR A 2 C32B C -0.0909(16) 0.1503(9) 0.9766(6) 0.049(3) Uani 0.50 1 d P A 2 H32D H -0.1454 0.1193 0.9988 0.074 Uiso 0.50 1 calc PR A 2 H32E H -0.0737 0.1182 0.9469 0.074 Uiso 0.50 1 calc PR A 2 H32F H -0.1484 0.1971 0.9637 0.074 Uiso 0.50 1 calc PR A 2 C33 C 0.547(3) 0.0969(19) 0.9978(12) 0.0556(19) Uani 0.50 1 d PD . . H33A H 0.5881 0.1500 1.0049 0.067 Uiso 0.50 1 calc PR . . H33B H 0.5868 0.0620 1.0270 0.067 Uiso 0.50 1 calc PR . . H33C H 0.4398 0.0990 0.9939 0.067 Uiso 0.50 1 calc PR . . N1 N 0.3673(5) 0.1927(3) 0.81046(19) 0.0311(10) Uani 1 1 d . . . N2 N 0.3935(5) 0.2497(3) 0.70690(18) 0.0341(11) Uani 1 1 d . . . N3 N 0.6476(5) 0.2831(3) 0.7831(2) 0.0347(11) Uani 1 1 d . . . N4 N 0.2083(5) 0.3614(3) 0.74247(17) 0.0285(9) Uani 1 1 d . . . N5 N 0.3702(5) 0.4703(3) 0.91477(17) 0.0265(9) Uani 1 1 d . . . H5 H 0.4031 0.4511 0.8876 0.032 Uiso 1 1 calc R . . N6 N 0.2601(5) 0.4779(2) 0.98369(17) 0.0259(9) Uani 1 1 d . . . H6 H 0.2102 0.4649 1.0083 0.031 Uiso 1 1 calc R . . O1 O 0.3841(4) 0.3382(2) 0.86584(14) 0.0284(8) Uani 1 1 d . . . O2 O 0.4961(4) 0.4495(2) 0.80401(16) 0.0350(9) Uani 1 1 d D . . H100 H 0.467(6) 0.476(3) 0.7705(14) 0.042 Uiso 1 1 d D . . H101 H 0.594(4) 0.470(3) 0.818(2) 0.042 Uiso 1 1 d D . . O11 O 0.5880(17) 0.0674(12) 0.9507(12) 0.0556(19) Uani 0.50 1 d PD . . H11 H 0.6105 0.1051 0.9329 0.067 Uiso 0.50 1 calc R . . Mn Mn 0.42052(8) 0.31855(5) 0.78931(3) 0.0251(2) Uani 1 1 d . . . O7 O 0.0312(7) 0.5253(5) 0.8675(2) 0.086(2) Uani 1 1 d . . . O8 O -0.1165(19) 0.4412(5) 0.9067(4) 0.206(7) Uani 1 1 d . . . O9 O -0.1070(9) 0.5661(5) 0.9295(3) 0.122(3) Uani 1 1 d . . . O10 O -0.2150(8) 0.5306(9) 0.8439(3) 0.183(6) Uani 1 1 d . . . Cl2 Cl -0.10909(16) 0.51656(8) 0.88639(5) 0.0359(3) Uani 1 1 d . . . O3 O 0.1146(7) 0.9835(3) 0.8759(2) 0.0755(18) Uani 1 1 d . . . O4 O -0.0754(5) 0.9260(3) 0.81179(19) 0.0484(11) Uani 1 1 d . . . O5 O 0.0558(6) 1.0389(3) 0.78935(19) 0.0561(13) Uani 1 1 d . . . O6 O -0.1144(8) 1.0511(4) 0.8484(2) 0.0792(18) Uani 1 1 d . . . Cl1 Cl -0.0061(2) 1.00028(10) 0.83186(7) 0.0506(4) Uani 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 C1 0.029(3) 0.028(3) 0.036(3) -0.002(2) 0.012(2) 0.004(2) C2 0.034(3) 0.033(3) 0.048(4) 0.002(3) 0.016(3) 0.010(2) C3 0.028(3) 0.047(4) 0.054(4) -0.009(3) -0.005(3) 0.007(3) C4 0.039(3) 0.056(4) 0.035(3) -0.016(3) -0.009(3) 0.008(3) C5 0.025(3) 0.041(3) 0.034(3) -0.009(2) 0.006(2) 0.001(2) C6 0.032(3) 0.056(4) 0.026(3) -0.011(3) 0.005(2) 0.005(3) C7 0.025(3) 0.043(3) 0.047(3) 0.010(3) 0.001(2) -0.001(2) C8 0.031(3) 0.063(5) 0.072(5) 0.026(4) 0.005(3) 0.005(3) C9 0.025(3) 0.063(5) 0.102(7) 0.030(5) 0.011(4) 0.013(3) C10 0.040(4) 0.045(4) 0.076(5) 0.013(3) 0.032(4) 0.013(3) C11 0.026(3) 0.033(3) 0.053(3) 0.008(3) 0.018(2) 0.007(2) C12 0.036(3) 0.047(4) 0.047(3) -0.001(3) 0.023(3) 0.010(3) C13 0.036(3) 0.044(3) 0.044(3) -0.021(3) 0.017(3) -0.001(3) C14 0.039(3) 0.033(3) 0.053(4) -0.018(3) 0.024(3) -0.001(2) C15 0.023(2) 0.022(2) 0.037(3) -0.002(2) 0.005(2) 0.0004(19) C16 0.021(2) 0.027(2) 0.028(3) 0.000(2) 0.0028(19) -0.0007(19) C17 0.020(2) 0.027(3) 0.023(2) 0.0037(19) 0.0028(18) -0.0006(18) C18 0.025(2) 0.023(2) 0.020(2) 0.0000(18) -0.0004(18) -0.0011(19) C19 0.023(2) 0.033(3) 0.026(2) -0.003(2) 0.005(2) -0.002(2) C20 0.022(2) 0.034(3) 0.026(2) 0.005(2) 0.0046(19) -0.004(2) C21 0.023(2) 0.023(2) 0.034(3) 0.001(2) 0.001(2) -0.0015(19) C22 0.022(2) 0.024(2) 0.025(2) 0.0012(19) 0.0002(19) -0.0001(18) C23 0.024(2) 0.027(3) 0.030(3) -0.001(2) -0.005(2) 0.001(2) C24 0.025(2) 0.028(3) 0.025(2) 0.004(2) -0.0045(19) 0.001(2) C25 0.034(3) 0.031(3) 0.040(3) 0.007(2) -0.001(2) -0.004(2) C26 0.038(3) 0.026(3) 0.045(3) 0.012(2) -0.009(3) -0.006(2) C27 0.039(3) 0.025(3) 0.045(3) -0.004(2) -0.009(3) 0.000(2) C28 0.035(3) 0.033(3) 0.037(3) -0.003(2) 0.000(2) 0.001(2) C29 0.038(3) 0.036(3) 0.037(3) 0.000(2) 0.013(2) -0.011(2) C30A 0.024(5) 0.026(5) 0.038(6) 0.010(4) 0.007(4) -0.005(4) C31A 0.029(5) 0.032(5) 0.021(5) 0.008(4) 0.009(4) -0.002(4) C32A 0.021(5) 0.025(5) 0.043(6) 0.000(4) 0.016(5) -0.006(4) C30B 0.071(11) 0.079(12) 0.052(9) 0.028(8) 0.016(8) 0.002(9) C31B 0.079(11) 0.067(10) 0.042(8) -0.005(7) 0.026(8) -0.028(9) C32B 0.051(8) 0.051(8) 0.048(8) 0.001(6) 0.016(6) -0.012(6) C33 0.031(3) 0.063(5) 0.072(5) 0.026(4) 0.005(3) 0.005(3) N1 0.028(2) 0.029(2) 0.038(3) -0.0081(19) 0.0100(19) 0.0012(18) N2 0.024(2) 0.046(3) 0.034(2) -0.011(2) 0.0105(19) 0.0056(19) N3 0.023(2) 0.037(3) 0.044(3) 0.009(2) 0.006(2) 0.0032(19) N4 0.027(2) 0.033(2) 0.026(2) -0.0043(18) 0.0069(17) 0.0040(18) N5 0.029(2) 0.027(2) 0.023(2) 0.0004(17) 0.0040(17) -0.0042(17) N6 0.026(2) 0.026(2) 0.026(2) -0.0032(17) 0.0037(17) 0.0005(17) O1 0.0312(19) 0.0285(19) 0.0270(18) -0.0022(14) 0.0092(15) -0.0054(15) O2 0.035(2) 0.035(2) 0.036(2) 0.0002(17) 0.0097(17) -0.0076(17) O11 0.031(3) 0.063(5) 0.072(5) 0.026(4) 0.005(3) 0.005(3) Mn 0.0206(4) 0.0294(4) 0.0264(4) -0.0033(3) 0.0071(3) 0.0012(3) O7 0.061(4) 0.134(6) 0.070(4) 0.009(4) 0.033(3) 0.033(4) O8 0.43(2) 0.064(5) 0.172(9) -0.027(6) 0.188(12) -0.085(8) O9 0.147(7) 0.135(6) 0.114(6) -0.090(5) 0.104(5) -0.091(5) O10 0.055(4) 0.394(18) 0.093(6) 0.083(9) -0.009(4) 0.032(7) Cl2 0.0424(8) 0.0371(7) 0.0293(7) -0.0033(5) 0.0096(6) -0.0040(6) O3 0.109(5) 0.057(3) 0.051(3) -0.002(3) -0.012(3) -0.039(3) O4 0.052(3) 0.044(3) 0.050(3) -0.005(2) 0.013(2) -0.021(2) O5 0.077(3) 0.049(3) 0.046(3) -0.005(2) 0.019(2) -0.026(2) O6 0.125(5) 0.059(3) 0.065(4) -0.007(3) 0.049(4) 0.003(3) Cl1 0.0731(12) 0.0406(8) 0.0406(8) -0.0068(7) 0.0168(8) -0.0209(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C1 N4 1.343(6) . ? C1 C2 1.370(8) . ? C1 H1 0.9300 . ? C2 C3 1.380(9) . ? C2 H2 0.9300 . ? C3 C4 1.380(9) . ? C3 H3 0.9300 . ? C4 C5 1.375(8) . ? C4 H4 0.9300 . ? C5 N4 1.345(7) . ? C5 C6 1.518(7) . ? C6 N2 1.465(8) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N3 1.352(7) . ? C7 C8 1.361(9) . ? C7 H7 0.9300 . ? C8 C9 1.372(12) . ? C8 H8 0.9300 . ? C9 C10 1.368(11) . ? C9 H9 0.9300 . ? C10 C11 1.403(8) . ? C10 H10 0.9300 . ? C11 N3 1.341(8) . ? C11 C12 1.490(9) . ? C12 N2 1.480(7) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N2 1.487(8) . ? C13 C14 1.510(9) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N1 1.465(7) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 N1 1.279(7) . ? C15 C16 1.457(7) . ? C15 H15 0.9300 . ? C16 C21 1.390(7) . ? C16 C17 1.429(7) . ? C17 O1 1.296(6) . ? C17 C18 1.427(7) . ? C18 C19 1.388(7) . ? C18 C22 1.443(7) . ? C19 C20 1.394(7) . ? C19 H19 0.9300 . ? C20 C21 1.399(7) . ? C20 C29 1.526(7) . ? C21 H21 0.9300 . ? C22 N6 1.334(6) . ? C22 N5 1.340(6) . ? C23 N6 1.385(7) . ? C23 C24 1.391(7) . ? C23 C28 1.397(8) . ? C24 N5 1.374(7) . ? C24 C25 1.391(7) . ? C25 C26 1.384(8) . ? C25 H25 0.9300 . ? C26 C27 1.383(9) . ? C26 H26 0.9300 . ? C27 C28 1.382(8) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C30B 1.389(17) . ? C29 C32A 1.469(11) . ? C29 C30A 1.540(12) . ? C29 C31B 1.576(16) . ? C29 C31A 1.608(12) . ? C29 C32B 1.664(15) . ? C30A H30A 0.9600 . ? C30A H30B 0.9600 . ? C30A H30C 0.9600 . ? C31A H31A 0.9600 . ? C31A H31C 0.9600 . ? C31A H31B 0.9600 . ? C32A H32A 0.9600 . ? C32A H32B 0.9600 . ? C32A H32C 0.9600 . ? C30B H30E 0.9600 . ? C30B H30D 0.9600 . ? C30B H30F 0.9600 . ? C31B H31D 0.9600 . ? C31B H31F 0.9600 . ? C31B H31E 0.9600 . ? C32B H32D 0.9600 . ? C32B H32E 0.9600 . ? C32B H32F 0.9600 . ? C33 O11 1.401(2) . ? C33 H33A 0.9613 . ? C33 H33B 0.9613 . ? C33 H33C 0.9612 . ? N1 Mn 2.233(5) . ? N2 Mn 2.363(5) . ? N3 Mn 2.164(4) . ? N4 Mn 2.190(4) . ? N5 H5 0.8600 . ? N6 H6 0.8600 . ? O1 Mn 2.056(4) . ? O2 Mn 2.292(4) . ? O2 H100 0.956(19) . ? O2 H101 0.96(2) . ? O11 H11 0.8201 . ? O7 Cl2 1.437(6) . ? O8 Cl2 1.360(9) . ? O9 Cl2 1.368(6) . ? O10 Cl2 1.332(7) . ? O3 Cl1 1.446(6) . ? O4 Cl1 1.437(4) . ? O5 Cl1 1.450(5) . ? O6 Cl1 1.410(6) . ? 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 N4 C1 C2 123.0(5) . . ? N4 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C1 C2 C3 118.8(5) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C2 C3 C4 118.5(5) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C5 C4 C3 119.9(6) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? N4 C5 C4 121.6(5) . . ? N4 C5 C6 116.5(5) . . ? C4 C5 C6 121.8(5) . . ? N2 C6 C5 112.5(5) . . ? N2 C6 H6A 109.1 . . ? C5 C6 H6A 109.1 . . ? N2 C6 H6B 109.1 . . ? C5 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? N3 C7 C8 122.8(7) . . ? N3 C7 H7 118.6 . . ? C8 C7 H7 118.7 . . ? C7 C8 C9 118.2(7) . . ? C7 C8 H8 120.9 . . ? C9 C8 H8 120.9 . . ? C10 C9 C8 120.2(6) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 119.6(7) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? N3 C11 C10 119.6(6) . . ? N3 C11 C12 117.7(5) . . ? C10 C11 C12 122.6(6) . . ? N2 C12 C11 114.6(5) . . ? N2 C12 H12A 108.6 . . ? C11 C12 H12A 108.6 . . ? N2 C12 H12B 108.6 . . ? C11 C12 H12B 108.6 . . ? H12A C12 H12B 107.6 . . ? N2 C13 C14 111.8(5) . . ? N2 C13 H13A 109.3 . . ? C14 C13 H13A 109.2 . . ? N2 C13 H13B 109.3 . . ? C14 C13 H13B 109.3 . . ? H13A C13 H13B 107.9 . . ? N1 C14 C13 108.2(5) . . ? N1 C14 H14A 110.1 . . ? C13 C14 H14A 110.1 . . ? N1 C14 H14B 110.0 . . ? C13 C14 H14B 110.1 . . ? H14A C14 H14B 108.4 . . ? N1 C15 C16 125.4(5) . . ? N1 C15 H15 117.3 . . ? C16 C15 H15 117.3 . . ? C21 C16 C17 120.2(5) . . ? C21 C16 C15 116.9(5) . . ? C17 C16 C15 122.8(4) . . ? O1 C17 C18 120.6(4) . . ? O1 C17 C16 122.7(4) . . ? C18 C17 C16 116.7(4) . . ? C19 C18 C17 121.0(5) . . ? C19 C18 C22 120.9(5) . . ? C17 C18 C22 118.0(4) . . ? C18 C19 C20 122.3(5) . . ? C18 C19 H19 118.9 . . ? C20 C19 H19 118.9 . . ? C19 C20 C21 116.9(4) . . ? C19 C20 C29 122.1(5) . . ? C21 C20 C29 121.0(5) . . ? C16 C21 C20 122.8(5) . . ? C16 C21 H21 118.6 . . ? C20 C21 H21 118.6 . . ? N6 C22 N5 108.0(4) . . ? N6 C22 C18 127.3(5) . . ? N5 C22 C18 124.6(5) . . ? N6 C23 C24 106.5(4) . . ? N6 C23 C28 132.3(5) . . ? C24 C23 C28 121.1(5) . . ? N5 C24 C25 131.7(5) . . ? N5 C24 C23 106.0(4) . . ? C25 C24 C23 122.2(5) . . ? C26 C25 C24 116.2(6) . . ? C26 C25 H25 121.9 . . ? C24 C25 H25 121.9 . . ? C27 C26 C25 121.7(5) . . ? C27 C26 H26 119.2 . . ? C25 C26 H26 119.2 . . ? C28 C27 C26 122.6(5) . . ? C28 C27 H27 118.7 . . ? C26 C27 H27 118.7 . . ? C27 C28 C23 116.1(5) . . ? C27 C28 H28 121.9 . . ? C23 C28 H28 121.9 . . ? C30B C29 C32A 134.7(9) . . ? C30B C29 C20 113.5(8) . . ? C32A C29 C20 111.7(6) . . ? C30B C29 C30A 51.4(9) . . ? C32A C29 C30A 111.8(7) . . ? C20 C29 C30A 112.6(6) . . ? C30B C29 C31B 114.5(11) . . ? C20 C29 C31B 110.9(7) . . ? C30A C29 C31B 136.1(8) . . ? C30B C29 C31A 53.6(9) . . ? C32A C29 C31A 109.6(7) . . ? C20 C29 C31A 107.0(5) . . ? C30A C29 C31A 103.8(7) . . ? C31B C29 C31A 69.0(8) . . ? C30B C29 C32B 111.4(10) . . ? C32A C29 C32B 58.7(7) . . ? C20 C29 C32B 104.3(6) . . ? C30A C29 C32B 61.9(7) . . ? C31B C29 C32B 101.2(9) . . ? C31A C29 C32B 148.7(7) . . ? C29 C30A H30A 109.4 . . ? C29 C30A H30B 109.5 . . ? C29 C30A H30C 109.5 . . ? C29 C31A H31A 109.5 . . ? C29 C31A H31C 109.5 . . ? C29 C31A H31B 109.5 . . ? C29 C32A H32A 109.4 . . ? C29 C32A H32B 109.5 . . ? C29 C32A H32C 109.5 . . ? C29 C30B H30E 109.5 . . ? C29 C30B H30D 109.4 . . ? H30E C30B H30D 109.5 . . ? C29 C30B H30F 109.5 . . ? H30E C30B H30F 109.5 . . ? H30D C30B H30F 109.5 . . ? C29 C31B H31D 109.4 . . ? C29 C31B H31F 109.5 . . ? H31D C31B H31F 109.5 . . ? C29 C31B H31E 109.5 . . ? H31D C31B H31E 109.5 . . ? H31F C31B H31E 109.5 . . ? C29 C32B H32D 109.4 . . ? C29 C32B H32E 109.4 . . ? H32D C32B H32E 109.5 . . ? C29 C32B H32F 109.6 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? H33A C33 H33B 109.3 . . ? H33A C33 H33C 109.4 . . ? H33B C33 H33C 109.3 . . ? C15 N1 C14 118.0(5) . . ? C15 N1 Mn 129.0(4) . . ? C14 N1 Mn 112.6(4) . . ? C6 N2 C12 112.9(5) . . ? C6 N2 C13 110.5(5) . . ? C12 N2 C13 111.1(5) . . ? C6 N2 Mn 107.7(3) . . ? C12 N2 Mn 108.3(4) . . ? C13 N2 Mn 106.1(3) . . ? C11 N3 C7 119.6(5) . . ? C11 N3 Mn 119.0(4) . . ? C7 N3 Mn 120.8(4) . . ? C1 N4 C5 118.2(5) . . ? C1 N4 Mn 122.8(4) . . ? C5 N4 Mn 119.0(3) . . ? C22 N5 C24 110.1(4) . . ? C22 N5 H5 125.0 . . ? C24 N5 H5 124.9 . . ? C22 N6 C23 109.4(4) . . ? C22 N6 H6 125.3 . . ? C23 N6 H6 125.3 . . ? C17 O1 Mn 134.8(3) . . ? Mn O2 H100 106(3) . . ? Mn O2 H101 129(4) . . ? H100 O2 H101 105(3) . . ? C33 O11 H11 109.0 . . ? O1 Mn N3 114.99(17) . . ? O1 Mn N4 101.19(15) . . ? N3 Mn N4 142.94(17) . . ? O1 Mn N1 81.04(15) . . ? N3 Mn N1 90.49(17) . . ? N4 Mn N1 103.35(17) . . ? O1 Mn O2 77.69(14) . . ? N3 Mn O2 90.69(17) . . ? N4 Mn O2 89.27(16) . . ? N1 Mn O2 157.03(16) . . ? O1 Mn N2 155.22(16) . . ? N3 Mn N2 75.84(17) . . ? N4 Mn N2 74.35(16) . . ? N1 Mn N2 76.50(17) . . ? O2 Mn N2 125.90(16) . . ? O10 Cl2 O8 113.2(9) . . ? O10 Cl2 O9 116.8(7) . . ? O8 Cl2 O9 104.1(6) . . ? O10 Cl2 O7 105.1(5) . . ? O8 Cl2 O7 108.9(7) . . ? O9 Cl2 O7 108.5(4) . . ? O6 Cl1 O4 109.8(4) . . ? O6 Cl1 O3 110.6(4) . . ? O4 Cl1 O3 109.4(3) . . ? O6 Cl1 O5 109.6(3) . . ? O4 Cl1 O5 108.4(3) . . ? O3 Cl1 O5 109.1(4) . . ? 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 N4 C1 C2 C3 -0.6(9) . . . . ? C1 C2 C3 C4 0.4(10) . . . . ? C2 C3 C4 C5 0.2(10) . . . . ? C3 C4 C5 N4 -0.5(10) . . . . ? C3 C4 C5 C6 -177.2(6) . . . . ? N4 C5 C6 N2 28.4(8) . . . . ? C4 C5 C6 N2 -154.8(6) . . . . ? N3 C7 C8 C9 -2.0(10) . . . . ? C7 C8 C9 C10 1.5(11) . . . . ? C8 C9 C10 C11 0.1(11) . . . . ? C9 C10 C11 N3 -1.3(9) . . . . ? C9 C10 C11 C12 175.3(6) . . . . ? N3 C11 C12 N2 -24.4(8) . . . . ? C10 C11 C12 N2 159.0(6) . . . . ? N2 C13 C14 N1 57.1(6) . . . . ? N1 C15 C16 C21 173.4(5) . . . . ? N1 C15 C16 C17 -4.3(8) . . . . ? C21 C16 C17 O1 176.9(5) . . . . ? C15 C16 C17 O1 -5.4(8) . . . . ? C21 C16 C17 C18 -2.8(7) . . . . ? C15 C16 C17 C18 174.8(4) . . . . ? O1 C17 C18 C19 -177.9(5) . . . . ? C16 C17 C18 C19 1.8(7) . . . . ? O1 C17 C18 C22 -1.4(7) . . . . ? C16 C17 C18 C22 178.3(4) . . . . ? C17 C18 C19 C20 0.1(8) . . . . ? C22 C18 C19 C20 -176.3(5) . . . . ? C18 C19 C20 C21 -1.1(7) . . . . ? C18 C19 C20 C29 177.9(5) . . . . ? C17 C16 C21 C20 1.9(8) . . . . ? C15 C16 C21 C20 -175.8(5) . . . . ? C19 C20 C21 C16 0.1(7) . . . . ? C29 C20 C21 C16 -178.9(5) . . . . ? C19 C18 C22 N6 0.2(8) . . . . ? C17 C18 C22 N6 -176.3(5) . . . . ? C19 C18 C22 N5 177.1(5) . . . . ? C17 C18 C22 N5 0.6(7) . . . . ? N6 C23 C24 N5 -0.2(5) . . . . ? C28 C23 C24 N5 178.2(5) . . . . ? N6 C23 C24 C25 -177.6(5) . . . . ? C28 C23 C24 C25 0.8(8) . . . . ? N5 C24 C25 C26 -176.9(5) . . . . ? C23 C24 C25 C26 -0.3(8) . . . . ? C24 C25 C26 C27 -0.2(8) . . . . ? C25 C26 C27 C28 0.1(9) . . . . ? C26 C27 C28 C23 0.5(8) . . . . ? N6 C23 C28 C27 177.1(5) . . . . ? C24 C23 C28 C27 -0.9(8) . . . . ? C19 C20 C29 C30B -126.0(10) . . . . ? C21 C20 C29 C30B 52.9(11) . . . . ? C19 C20 C29 C32A 51.0(8) . . . . ? C21 C20 C29 C32A -130.0(7) . . . . ? C19 C20 C29 C30A 177.8(6) . . . . ? C21 C20 C29 C30A -3.3(8) . . . . ? C19 C20 C29 C31B 4.5(10) . . . . ? C21 C20 C29 C31B -176.5(8) . . . . ? C19 C20 C29 C31A -68.9(7) . . . . ? C21 C20 C29 C31A 110.1(6) . . . . ? C19 C20 C29 C32B 112.6(7) . . . . ? C21 C20 C29 C32B -68.4(8) . . . . ? C16 C15 N1 C14 -175.6(5) . . . . ? C16 C15 N1 Mn -3.0(8) . . . . ? C13 C14 N1 C15 131.6(5) . . . . ? C13 C14 N1 Mn -42.2(5) . . . . ? C5 C6 N2 C12 -153.6(5) . . . . ? C5 C6 N2 C13 81.3(6) . . . . ? C5 C6 N2 Mn -34.2(6) . . . . ? C11 C12 N2 C6 140.8(5) . . . . ? C11 C12 N2 C13 -94.5(6) . . . . ? C11 C12 N2 Mn 21.6(6) . . . . ? C14 C13 N2 C6 -157.9(4) . . . . ? C14 C13 N2 C12 76.1(6) . . . . ? C14 C13 N2 Mn -41.4(5) . . . . ? C10 C11 N3 C7 0.9(8) . . . . ? C12 C11 N3 C7 -175.8(5) . . . . ? C10 C11 N3 Mn -169.9(4) . . . . ? C12 C11 N3 Mn 13.4(7) . . . . ? C8 C7 N3 C11 0.8(9) . . . . ? C8 C7 N3 Mn 171.4(5) . . . . ? C2 C1 N4 C5 0.3(8) . . . . ? C2 C1 N4 Mn -176.9(4) . . . . ? C4 C5 N4 C1 0.3(9) . . . . ? C6 C5 N4 C1 177.1(5) . . . . ? C4 C5 N4 Mn 177.6(5) . . . . ? C6 C5 N4 Mn -5.6(7) . . . . ? N6 C22 N5 C24 0.2(5) . . . . ? C18 C22 N5 C24 -177.2(4) . . . . ? C25 C24 N5 C22 177.1(5) . . . . ? C23 C24 N5 C22 0.0(5) . . . . ? N5 C22 N6 C23 -0.3(5) . . . . ? C18 C22 N6 C23 177.0(5) . . . . ? C24 C23 N6 C22 0.3(5) . . . . ? C28 C23 N6 C22 -177.8(6) . . . . ? C18 C17 O1 Mn -155.2(4) . . . . ? C16 C17 O1 Mn 25.1(7) . . . . ? C17 O1 Mn N3 -110.2(5) . . . . ? C17 O1 Mn N4 78.1(5) . . . . ? C17 O1 Mn N1 -23.9(4) . . . . ? C17 O1 Mn O2 164.8(5) . . . . ? C17 O1 Mn N2 1.2(7) . . . . ? C11 N3 Mn O1 155.7(4) . . . . ? C7 N3 Mn O1 -15.0(5) . . . . ? C11 N3 Mn N4 -37.9(6) . . . . ? C7 N3 Mn N4 151.4(4) . . . . ? C11 N3 Mn N1 75.3(4) . . . . ? C7 N3 Mn N1 -95.3(4) . . . . ? C11 N3 Mn O2 -127.6(4) . . . . ? C7 N3 Mn O2 61.7(4) . . . . ? C11 N3 Mn N2 -0.6(4) . . . . ? C7 N3 Mn N2 -171.3(5) . . . . ? C1 N4 Mn O1 11.9(4) . . . . ? C5 N4 Mn O1 -165.2(4) . . . . ? C1 N4 Mn N3 -155.6(4) . . . . ? C5 N4 Mn N3 27.3(6) . . . . ? C1 N4 Mn N1 95.2(4) . . . . ? C5 N4 Mn N1 -81.9(4) . . . . ? C1 N4 Mn O2 -65.4(4) . . . . ? C5 N4 Mn O2 117.5(4) . . . . ? C1 N4 Mn N2 166.8(5) . . . . ? C5 N4 Mn N2 -10.3(4) . . . . ? C15 N1 Mn O1 12.0(5) . . . . ? C14 N1 Mn O1 -175.0(4) . . . . ? C15 N1 Mn N3 127.3(5) . . . . ? C14 N1 Mn N3 -59.8(4) . . . . ? C15 N1 Mn N4 -87.4(5) . . . . ? C14 N1 Mn N4 85.5(4) . . . . ? C15 N1 Mn O2 34.3(7) . . . . ? C14 N1 Mn O2 -152.7(4) . . . . ? C15 N1 Mn N2 -157.4(5) . . . . ? C14 N1 Mn N2 15.6(4) . . . . ? C6 N2 Mn O1 106.6(5) . . . . ? C12 N2 Mn O1 -131.1(4) . . . . ? C13 N2 Mn O1 -11.8(6) . . . . ? C6 N2 Mn N3 -133.9(4) . . . . ? C12 N2 Mn N3 -11.5(4) . . . . ? C13 N2 Mn N3 107.8(4) . . . . ? C6 N2 Mn N4 23.8(4) . . . . ? C12 N2 Mn N4 146.2(4) . . . . ? C13 N2 Mn N4 -94.5(3) . . . . ? C6 N2 Mn N1 132.1(4) . . . . ? C12 N2 Mn N1 -105.5(4) . . . . ? C13 N2 Mn N1 13.8(3) . . . . ? C6 N2 Mn O2 -53.5(4) . . . . ? C12 N2 Mn O2 68.9(4) . . . . ? C13 N2 Mn O2 -171.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.035 _refine_diff_density_min -0.915 _refine_diff_density_rms 0.139 # Attachment '- 1143GuillotICMMO.cif' data_1143GuillotICMMO _database_code_depnum_ccdc_archive 'CCDC 828978' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C32 H34 Cl Mn N6 O5, C2 H3 N, Cl O4 ' _chemical_formula_sum 'C34 H37 Cl2 Mn N7 O9' _chemical_melting_point ? _exptl_crystal_description plate _exptl_crystal_colour yellow _diffrn_ambient_temperature 100(1) _chemical_formula_weight 813.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0031 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 0.0109 0.0061 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1495 0.1591 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3385 0.7311 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_int_tables_number 14 _chemical_absolute_configuration . loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.4655(5) _cell_length_b 13.8053(7) _cell_length_c 27.3775(15) _cell_angle_alpha 90.00 _cell_angle_beta 94.840(2) _cell_angle_gamma 90.00 _cell_volume 3564.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 9320 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 30.51 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1684 _exptl_absorpt_coefficient_mu 0.586 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.9100 _exptl_absorpt_correction_T_max 0.9842 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'kappa X8 APEX II Bruker ICMMO' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 73536 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 30.68 _reflns_number_total 10833 _reflns_number_gt 8332 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1024P)^2^+13.0776P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 10833 _refine_ls_number_parameters 483 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1017 _refine_ls_R_factor_gt 0.0793 _refine_ls_wR_factor_ref 0.2310 _refine_ls_wR_factor_gt 0.2117 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.002 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6149(4) 0.5059(2) 0.18646(12) 0.0222(6) Uani 1 1 d . . . H1 H 0.6888 0.5180 0.1670 0.027 Uiso 1 1 calc R . . C2 C 0.5578(4) 0.5825(3) 0.21020(14) 0.0280(7) Uani 1 1 d . . . H2 H 0.5926 0.6450 0.2071 0.034 Uiso 1 1 calc R . . C3 C 0.4465(4) 0.5640(3) 0.23892(14) 0.0320(8) Uani 1 1 d . . . H3 H 0.4051 0.6142 0.2553 0.038 Uiso 1 1 calc R . . C4 C 0.3980(4) 0.4701(3) 0.24279(13) 0.0284(7) Uani 1 1 d . . . H4 H 0.3223 0.4566 0.2612 0.034 Uiso 1 1 calc R . . C5 C 0.4637(4) 0.3965(3) 0.21880(13) 0.0246(6) Uani 1 1 d . . . C6 C 0.4190(5) 0.2932(3) 0.22589(18) 0.0415(11) Uani 1 1 d . . . H6A H 0.4417 0.2757 0.2599 0.050 Uiso 1 1 calc R . . H6B H 0.3168 0.2891 0.2193 0.050 Uiso 1 1 calc R . . C7 C 0.8325(5) 0.1211(3) 0.13204(16) 0.0369(9) Uani 1 1 d . . . H7 H 0.8728 0.1602 0.1093 0.044 Uiso 1 1 calc R . . C8 C 0.8756(6) 0.0262(4) 0.13671(19) 0.0470(12) Uani 1 1 d . . . H8 H 0.9449 0.0019 0.1179 0.056 Uiso 1 1 calc R . . C9 C 0.8137(6) -0.0324(3) 0.1700(2) 0.0510(13) Uani 1 1 d . . . H9 H 0.8387 -0.0974 0.1732 0.061 Uiso 1 1 calc R . . C10 C 0.7149(5) 0.0069(3) 0.19820(18) 0.0436(11) Uani 1 1 d . . . H10 H 0.6729 -0.0310 0.2210 0.052 Uiso 1 1 calc R . . C11 C 0.6781(4) 0.1043(3) 0.19230(14) 0.0310(8) Uani 1 1 d . . . C12 C 0.5770(5) 0.1528(3) 0.22351(15) 0.0361(9) Uani 1 1 d . . . H12A H 0.5185 0.1042 0.2376 0.043 Uiso 1 1 calc R . . H12B H 0.6299 0.1866 0.2502 0.043 Uiso 1 1 calc R . . C13 C 0.3783(4) 0.1703(3) 0.16181(16) 0.0305(8) Uani 1 1 d . . . H13A H 0.2972 0.1539 0.1796 0.037 Uiso 1 1 calc R . . H13B H 0.4188 0.1106 0.1506 0.037 Uiso 1 1 calc R . . C14 C 0.3308(4) 0.2325(3) 0.11840(17) 0.0337(8) Uani 1 1 d . . . H14A H 0.2626 0.1977 0.0965 0.040 Uiso 1 1 calc R . . H14B H 0.2861 0.2911 0.1292 0.040 Uiso 1 1 calc R . . C15 C 0.4562(4) 0.2402(3) 0.04722(16) 0.0308(8) Uani 1 1 d . . . H15 H 0.3722 0.2172 0.0313 0.037 Uiso 1 1 calc R . . C16 C 0.5756(4) 0.2535(3) 0.01778(13) 0.0258(7) Uani 1 1 d . . . C17 C 0.7015(4) 0.3021(2) 0.03630(12) 0.0222(6) Uani 1 1 d . . . C18 C 0.8130(3) 0.3069(3) 0.00476(12) 0.0234(6) Uani 1 1 d . . . C19 C 0.8003(4) 0.2631(3) -0.04150(13) 0.0272(7) Uani 1 1 d . . . H19 H 0.8763 0.2661 -0.0609 0.033 Uiso 1 1 calc R . . C20 C 0.6772(4) 0.2152(3) -0.05947(14) 0.0295(8) Uani 1 1 d . . . C21 C 0.5661(4) 0.2133(3) -0.02954(14) 0.0299(7) Uani 1 1 d . . . H21 H 0.4815 0.1840 -0.0413 0.036 Uiso 1 1 calc R . . C22 C 0.9419(4) 0.3563(3) 0.02129(12) 0.0227(6) Uani 1 1 d . . . C23 C 1.1578(4) 0.4207(3) 0.02399(13) 0.0270(7) Uani 1 1 d . . . C24 C 1.1061(4) 0.4346(3) 0.06958(12) 0.0233(6) Uani 1 1 d . . . C25 C 1.1833(4) 0.4817(3) 0.10773(14) 0.0272(7) Uani 1 1 d . . . H25 H 1.1476 0.4919 0.1379 0.033 Uiso 1 1 calc R . . C26 C 1.3172(4) 0.5126(3) 0.09791(16) 0.0320(8) Uani 1 1 d . . . H26 H 1.3743 0.5434 0.1225 0.038 Uiso 1 1 calc R . . C27 C 1.3694(4) 0.4988(3) 0.05206(18) 0.0397(10) Uani 1 1 d . . . H27 H 1.4599 0.5208 0.0471 0.048 Uiso 1 1 calc R . . C28 C 1.2911(4) 0.4538(4) 0.01443(16) 0.0367(9) Uani 1 1 d . . . H28 H 1.3255 0.4458 -0.0161 0.044 Uiso 1 1 calc R . . C29 C 0.6710(5) 0.1677(3) -0.11041(15) 0.0357(9) Uani 1 1 d . . . C30 C 0.5339(5) 0.1096(5) -0.1212(2) 0.0593(16) Uani 1 1 d . . . H30A H 0.5326 0.0814 -0.1533 0.089 Uiso 1 1 calc R . . H30B H 0.4538 0.1518 -0.1198 0.089 Uiso 1 1 calc R . . H30C H 0.5295 0.0591 -0.0972 0.089 Uiso 1 1 calc R . . C31 C 0.7936(5) 0.0969(4) -0.11255(16) 0.0412(10) Uani 1 1 d . . . H31A H 0.7867 0.0651 -0.1438 0.062 Uiso 1 1 calc R . . H31B H 0.7898 0.0496 -0.0870 0.062 Uiso 1 1 calc R . . H31C H 0.8818 0.1315 -0.1081 0.062 Uiso 1 1 calc R . . C32 C 0.6823(9) 0.2441(4) -0.14948(18) 0.070(2) Uani 1 1 d . . . H32A H 0.7755 0.2722 -0.1462 0.104 Uiso 1 1 calc R . . H32B H 0.6129 0.2937 -0.1458 0.104 Uiso 1 1 calc R . . H32C H 0.6658 0.2150 -0.1813 0.104 Uiso 1 1 calc R . . C33 C 0.1401(6) 0.0750(4) 0.0096(2) 0.0506(12) Uani 1 1 d . . . C34 C 0.2391(7) 0.0202(5) -0.0154(2) 0.0612(15) Uani 1 1 d . . . H34A H 0.2594 0.0536 -0.0447 0.092 Uiso 1 1 calc R . . H34B H 0.1995 -0.0422 -0.0237 0.092 Uiso 1 1 calc R . . H34C H 0.3250 0.0122 0.0055 0.092 Uiso 1 1 calc R . . N3 N 0.5684(3) 0.41410(19) 0.19028(11) 0.0210(5) Uani 1 1 d . . . N4 N 0.7345(3) 0.1596(2) 0.15900(12) 0.0274(6) Uani 1 1 d . . . N2 N 0.4852(4) 0.2223(2) 0.19477(13) 0.0301(7) Uani 1 1 d . . . N1 N 0.4565(3) 0.2572(2) 0.09276(13) 0.0276(6) Uani 1 1 d . . . N5 N 0.9719(3) 0.3934(2) 0.06622(10) 0.0230(5) Uani 1 1 d . . . H5 H 0.9162 0.3920 0.0895 0.028 Uiso 1 1 calc R . . N6 N 1.0534(3) 0.3725(3) -0.00462(11) 0.0286(6) Uani 1 1 d . . . H6 H 1.0591 0.3553 -0.0346 0.034 Uiso 1 1 calc R . . N7 N 0.0624(6) 0.1192(4) 0.0310(2) 0.0637(13) Uani 1 1 d . . . O1 O 0.7173(3) 0.34078(19) 0.07938(9) 0.0245(5) Uani 1 1 d . . . O2 O 0.8714(3) 0.37055(19) 0.16642(9) 0.0248(5) Uani 1 1 d . . . O3 O 1.0478(3) 0.4213(2) 0.22593(11) 0.0365(6) Uani 1 1 d . . . O4 O 0.8881(3) 0.29926(19) 0.24436(9) 0.0291(5) Uani 1 1 d . . . O5 O 1.0623(3) 0.2673(2) 0.19002(14) 0.0453(8) Uani 1 1 d . . . O6 O 0.1922(5) 0.2741(3) 0.83661(13) 0.0575(10) Uani 1 1 d . . . O7 O 0.0874(5) 0.3679(3) 0.89480(13) 0.0672(13) Uani 1 1 d . . . O8 O 0.3294(5) 0.3399(4) 0.90107(17) 0.0662(12) Uani 1 1 d . . . O9 O 0.1702(5) 0.2168(3) 0.91664(15) 0.0639(11) Uani 1 1 d . . . Cl1 Cl 0.96889(8) 0.33927(6) 0.20745(3) 0.02141(17) Uani 1 1 d . . . Cl2 Cl 0.19141(14) 0.29743(8) 0.88602(4) 0.0416(3) Uani 1 1 d . . . Mn Mn 0.63936(6) 0.30103(4) 0.143779(19) 0.02189(14) Uani 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 C1 0.0239(15) 0.0172(13) 0.0255(15) -0.0022(11) 0.0015(12) -0.0009(11) C2 0.0343(19) 0.0189(14) 0.0299(17) -0.0044(12) -0.0021(14) 0.0033(13) C3 0.038(2) 0.0299(17) 0.0285(17) -0.0125(14) 0.0037(15) 0.0100(15) C4 0.0234(16) 0.0371(19) 0.0254(16) -0.0102(14) 0.0056(13) 0.0024(14) C5 0.0209(15) 0.0271(16) 0.0265(15) -0.0084(12) 0.0058(12) -0.0025(12) C6 0.048(2) 0.0316(19) 0.051(2) -0.0149(17) 0.037(2) -0.0159(17) C7 0.043(2) 0.0285(18) 0.039(2) -0.0070(15) 0.0050(17) 0.0098(16) C8 0.053(3) 0.037(2) 0.049(3) -0.0131(19) -0.004(2) 0.018(2) C9 0.063(3) 0.0225(18) 0.063(3) -0.0058(19) -0.023(3) 0.0080(19) C10 0.054(3) 0.0251(18) 0.047(2) 0.0103(17) -0.021(2) -0.0139(18) C11 0.038(2) 0.0235(16) 0.0306(18) 0.0020(13) -0.0040(15) -0.0106(14) C12 0.040(2) 0.037(2) 0.0327(19) 0.0015(15) 0.0089(16) -0.0185(17) C13 0.0252(17) 0.0223(15) 0.046(2) -0.0062(14) 0.0149(15) -0.0074(13) C14 0.0187(16) 0.0336(19) 0.050(2) 0.0000(17) 0.0125(15) -0.0004(14) C15 0.0187(16) 0.0275(17) 0.046(2) -0.0058(15) 0.0012(14) -0.0014(13) C16 0.0173(15) 0.0293(16) 0.0305(17) -0.0075(13) 0.0001(12) 0.0007(12) C17 0.0203(15) 0.0242(14) 0.0221(14) -0.0037(11) 0.0024(11) -0.0012(12) C18 0.0181(14) 0.0333(17) 0.0188(14) -0.0023(12) 0.0013(11) -0.0003(12) C19 0.0225(16) 0.0384(19) 0.0205(15) -0.0061(13) 0.0001(12) 0.0073(14) C20 0.0252(17) 0.0353(18) 0.0266(16) -0.0109(14) -0.0064(13) 0.0083(14) C21 0.0217(16) 0.0343(18) 0.0324(18) -0.0107(14) -0.0056(13) 0.0034(13) C22 0.0200(14) 0.0317(16) 0.0168(13) 0.0015(12) 0.0032(11) -0.0015(12) C23 0.0210(16) 0.0374(18) 0.0231(15) 0.0053(13) 0.0038(12) -0.0031(13) C24 0.0199(15) 0.0270(15) 0.0229(14) 0.0063(12) 0.0019(11) -0.0056(12) C25 0.0260(17) 0.0262(16) 0.0289(17) 0.0040(13) -0.0006(13) -0.0067(13) C26 0.0262(18) 0.0275(17) 0.042(2) 0.0047(15) -0.0023(15) -0.0079(14) C27 0.0224(18) 0.046(2) 0.051(2) 0.0097(19) 0.0030(16) -0.0105(16) C28 0.0245(18) 0.054(3) 0.0325(19) 0.0061(17) 0.0076(14) -0.0064(17) C29 0.039(2) 0.039(2) 0.0272(17) -0.0154(15) -0.0094(15) 0.0150(17) C30 0.037(2) 0.076(4) 0.062(3) -0.043(3) -0.014(2) 0.009(2) C31 0.043(2) 0.045(2) 0.035(2) -0.0135(18) -0.0016(17) 0.0181(19) C32 0.133(6) 0.045(3) 0.026(2) -0.0081(19) -0.019(3) 0.020(3) C33 0.052(3) 0.051(3) 0.048(3) 0.012(2) 0.000(2) -0.007(2) C34 0.071(4) 0.055(3) 0.058(3) 0.010(3) 0.011(3) -0.004(3) N3 0.0206(13) 0.0167(11) 0.0266(13) -0.0045(10) 0.0076(10) -0.0027(9) N4 0.0319(16) 0.0190(12) 0.0321(15) -0.0036(11) 0.0067(12) -0.0011(11) N2 0.0335(17) 0.0222(13) 0.0371(16) -0.0093(12) 0.0185(13) -0.0099(12) N1 0.0184(13) 0.0252(14) 0.0403(17) 0.0009(12) 0.0083(12) -0.0002(11) N5 0.0205(13) 0.0308(14) 0.0182(12) 0.0009(10) 0.0036(10) -0.0081(11) N6 0.0206(14) 0.0475(18) 0.0183(12) -0.0007(12) 0.0040(10) -0.0033(13) N7 0.061(3) 0.059(3) 0.072(3) 0.001(3) 0.008(3) 0.005(2) O1 0.0226(11) 0.0302(12) 0.0217(11) -0.0061(9) 0.0071(9) -0.0075(9) O2 0.0234(12) 0.0294(12) 0.0215(11) 0.0046(9) 0.0020(9) -0.0025(9) O3 0.0320(14) 0.0411(16) 0.0353(14) 0.0020(12) -0.0032(11) -0.0141(12) O4 0.0365(14) 0.0280(12) 0.0237(12) 0.0065(10) 0.0083(10) -0.0027(10) O5 0.0367(17) 0.0364(16) 0.066(2) 0.0052(15) 0.0234(15) 0.0173(13) O6 0.100(3) 0.0424(18) 0.0335(16) -0.0031(14) 0.0267(18) 0.0059(19) O7 0.089(3) 0.084(3) 0.0299(16) 0.0024(17) 0.0097(18) 0.056(3) O8 0.058(2) 0.082(3) 0.058(2) 0.008(2) 0.0020(19) -0.013(2) O9 0.092(3) 0.058(2) 0.044(2) 0.0157(17) 0.022(2) -0.017(2) Cl1 0.0202(3) 0.0211(3) 0.0235(3) 0.0031(3) 0.0051(3) 0.0012(3) Cl2 0.0596(7) 0.0341(5) 0.0349(5) 0.0030(4) 0.0262(5) 0.0047(4) Mn 0.0250(3) 0.0160(2) 0.0265(3) -0.00397(17) 0.01310(19) -0.00329(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C1 N3 1.349(4) . ? C1 C2 1.375(5) . ? C2 C3 1.390(6) . ? C3 C4 1.381(6) . ? C4 C5 1.386(5) . ? C5 N3 1.334(4) . ? C5 C6 1.504(5) . ? C6 N2 1.472(5) . ? C7 N4 1.343(5) . ? C7 C8 1.374(6) . ? C8 C9 1.385(8) . ? C9 C10 1.374(8) . ? C10 C11 1.395(6) . ? C11 N4 1.334(5) . ? C11 C12 1.494(6) . ? C12 N2 1.477(6) . ? C13 N2 1.483(5) . ? C13 C14 1.504(6) . ? C14 N1 1.471(5) . ? C15 N1 1.269(5) . ? C15 C16 1.454(5) . ? C16 C21 1.405(5) . ? C16 C17 1.424(5) . ? C17 O1 1.291(4) . ? C17 C18 1.421(5) . ? C18 C19 1.399(5) . ? C18 C22 1.437(5) . ? C19 C20 1.393(5) . ? C20 C21 1.387(6) . ? C20 C29 1.538(5) . ? C22 N6 1.339(4) . ? C22 N5 1.341(4) . ? C23 N6 1.379(5) . ? C23 C28 1.388(5) . ? C23 C24 1.392(5) . ? C24 C25 1.385(5) . ? C24 N5 1.388(4) . ? C25 C26 1.385(5) . ? C26 C27 1.400(7) . ? C27 C28 1.367(6) . ? C29 C32 1.513(8) . ? C29 C31 1.522(6) . ? C29 C30 1.533(7) . ? C33 N7 1.151(8) . ? C33 C34 1.424(9) . ? N3 Mn 2.157(3) . ? N4 Mn 2.176(3) . ? N2 Mn 2.367(3) . ? N1 Mn 2.215(3) . ? O1 Mn 2.043(2) . ? O2 Cl1 1.458(3) . ? O2 Mn 2.429(3) . ? O3 Cl1 1.426(3) . ? O4 Cl1 1.429(3) . ? O5 Cl1 1.438(3) . ? O6 Cl2 1.391(4) . ? O7 Cl2 1.419(4) . ? O8 Cl2 1.459(5) . ? O9 Cl2 1.418(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 C1 C2 122.8(3) . . ? C1 C2 C3 118.2(3) . . ? C4 C3 C2 119.2(3) . . ? C3 C4 C5 119.1(3) . . ? N3 C5 C4 121.9(3) . . ? N3 C5 C6 118.6(3) . . ? C4 C5 C6 119.4(3) . . ? N2 C6 C5 114.6(3) . . ? N4 C7 C8 122.7(5) . . ? C7 C8 C9 118.7(5) . . ? C10 C9 C8 119.0(4) . . ? C9 C10 C11 119.4(4) . . ? N4 C11 C10 121.3(4) . . ? N4 C11 C12 116.6(3) . . ? C10 C11 C12 122.1(4) . . ? N2 C12 C11 111.3(3) . . ? N2 C13 C14 110.3(3) . . ? N1 C14 C13 108.0(3) . . ? N1 C15 C16 125.7(3) . . ? C21 C16 C17 120.1(3) . . ? C21 C16 C15 118.0(3) . . ? C17 C16 C15 121.9(3) . . ? O1 C17 C18 120.1(3) . . ? O1 C17 C16 123.3(3) . . ? C18 C17 C16 116.6(3) . . ? C19 C18 C17 121.2(3) . . ? C19 C18 C22 119.7(3) . . ? C17 C18 C22 119.0(3) . . ? C20 C19 C18 122.0(3) . . ? C21 C20 C19 117.0(3) . . ? C21 C20 C29 123.7(3) . . ? C19 C20 C29 119.3(4) . . ? C20 C21 C16 123.0(3) . . ? N6 C22 N5 107.9(3) . . ? N6 C22 C18 126.7(3) . . ? N5 C22 C18 125.4(3) . . ? N6 C23 C28 132.2(4) . . ? N6 C23 C24 106.7(3) . . ? C28 C23 C24 121.2(4) . . ? C25 C24 N5 131.6(3) . . ? C25 C24 C23 122.6(3) . . ? N5 C24 C23 105.9(3) . . ? C24 C25 C26 115.5(4) . . ? C25 C26 C27 122.0(4) . . ? C28 C27 C26 121.9(4) . . ? C27 C28 C23 116.8(4) . . ? C32 C29 C31 108.7(5) . . ? C32 C29 C30 109.8(5) . . ? C31 C29 C30 107.0(4) . . ? C32 C29 C20 110.1(4) . . ? C31 C29 C20 109.8(3) . . ? C30 C29 C20 111.4(4) . . ? N7 C33 C34 178.2(6) . . ? C5 N3 C1 118.7(3) . . ? C5 N3 Mn 119.8(2) . . ? C1 N3 Mn 120.9(2) . . ? C11 N4 C7 119.0(4) . . ? C11 N4 Mn 117.4(3) . . ? C7 N4 Mn 122.9(3) . . ? C6 N2 C12 112.6(4) . . ? C6 N2 C13 111.8(3) . . ? C12 N2 C13 110.5(3) . . ? C6 N2 Mn 110.5(2) . . ? C12 N2 Mn 104.4(2) . . ? C13 N2 Mn 106.6(2) . . ? C15 N1 C14 119.4(3) . . ? C15 N1 Mn 127.4(3) . . ? C14 N1 Mn 112.5(3) . . ? C22 N5 C24 109.8(3) . . ? C22 N6 C23 109.8(3) . . ? C17 O1 Mn 130.9(2) . . ? Cl1 O2 Mn 125.41(14) . . ? O3 Cl1 O4 110.60(18) . . ? O3 Cl1 O5 110.4(2) . . ? O4 Cl1 O5 110.41(18) . . ? O3 Cl1 O2 108.47(17) . . ? O4 Cl1 O2 108.52(16) . . ? O5 Cl1 O2 108.40(19) . . ? O6 Cl2 O9 113.9(3) . . ? O6 Cl2 O7 112.6(2) . . ? O9 Cl2 O7 107.7(3) . . ? O6 Cl2 O8 106.8(3) . . ? O9 Cl2 O8 108.5(3) . . ? O7 Cl2 O8 107.1(3) . . ? O1 Mn N3 117.91(11) . . ? O1 Mn N4 103.45(12) . . ? N3 Mn N4 132.91(12) . . ? O1 Mn N1 81.32(11) . . ? N3 Mn N1 107.70(11) . . ? N4 Mn N1 99.48(12) . . ? O1 Mn N2 156.61(11) . . ? N3 Mn N2 75.27(10) . . ? N4 Mn N2 74.98(12) . . ? N1 Mn N2 76.04(12) . . ? O1 Mn O2 74.30(9) . . ? N3 Mn O2 83.31(10) . . ? N4 Mn O2 87.42(11) . . ? N1 Mn O2 155.59(10) . . ? N2 Mn O2 128.32(11) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.047 _refine_diff_density_min -0.963 _refine_diff_density_rms 0.132