data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Greg Brewer' _publ_contact_author_address ; Department of Chemistry Catholic University 620 Michigan Avenue 201 Maloney Hall Washington DC 20064 UNITED STATES OF AMERICA ; _publ_contact_author_email BREWER@CUA.EDU _publ_section_title ; Synthesis and characterization of seven coordinate tripodal imidazole complexes of iron(II) and manganese(II) ; loop_ _publ_author_name 'Greg Brewer' 'Cynthia Brewer' 'R. Butcher' 'Everett E. Carpenter' 'Luciann Cuenca' ; A.M.Schmiedekamp ; 'Carol Viragh' data_llcl2m _database_code_depnum_ccdc_archive 'CCDC 271613' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H36 Cl2 Fe N10 O8' _chemical_formula_weight 719.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5832(14) _cell_length_b 12.1393(15) _cell_length_c 12.3268(15) _cell_angle_alpha 80.843(2) _cell_angle_beta 71.329(2) _cell_angle_gamma 68.328(2) _cell_volume 1524.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 7693 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 28.32 _exptl_crystal_description diamond _exptl_crystal_colour red _exptl_crystal_size_max 0.66 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.567 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 0.735 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7716 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12225 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 28.35 _reflns_number_total 7261 _reflns_number_gt 6048 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0465P)^2^+1.3506P] 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_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7261 _refine_ls_number_parameters 409 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.1052 _refine_ls_wR_factor_gt 0.0985 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 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 Fe Fe 0.66269(2) 0.79380(2) 0.296544(19) 0.01371(5) Uani 1 1 d . . . Cl1 Cl 0.65860(5) 0.45052(4) 0.78691(4) 0.02958(10) Uani 1 1 d . . . Cl2 Cl 0.93138(4) 0.90101(4) -0.18767(3) 0.02250(9) Uani 1 1 d . . . O11 O 0.56096(16) 0.51876(19) 0.73052(17) 0.0610(5) Uani 1 1 d . . . O12 O 0.6270(2) 0.35312(16) 0.85416(16) 0.0591(5) Uani 1 1 d . . . O13 O 0.66585(17) 0.52715(15) 0.85974(16) 0.0486(4) Uani 1 1 d . . . O14 O 0.78304(17) 0.40922(14) 0.70278(14) 0.0439(4) Uani 1 1 d . . . O21 O 0.99085(19) 0.96468(17) -0.28411(14) 0.0545(5) Uani 1 1 d . . . O22 O 1.01134(16) 0.77812(15) -0.19475(17) 0.0472(4) Uani 1 1 d . . . O23 O 0.80449(14) 0.91233(15) -0.18998(13) 0.0402(4) Uani 1 1 d . . . O24 O 0.92407(15) 0.94343(16) -0.08320(12) 0.0432(4) Uani 1 1 d . . . N N 0.77688(13) 0.64244(12) 0.15318(12) 0.0165(3) Uani 1 1 d . . . N1A N 0.84491(13) 0.83657(13) 0.19961(12) 0.0172(3) Uani 1 1 d . . . N2A N 0.60121(13) 0.99198(13) 0.25436(12) 0.0172(3) Uani 1 1 d . . . N3A N 0.65753(14) 1.14231(13) 0.15530(12) 0.0194(3) Uani 1 1 d . . . N1B N 0.70367(13) 0.61774(12) 0.40279(12) 0.0165(3) Uani 1 1 d . . . N2B N 0.73559(13) 0.81578(12) 0.43596(12) 0.0167(3) Uani 1 1 d . . . N3B N 0.82805(13) 0.73456(13) 0.57484(12) 0.0192(3) Uani 1 1 d . . . N1C N 0.51858(13) 0.82336(12) 0.19801(12) 0.0170(3) Uani 1 1 d . . . N2C N 0.47241(13) 0.80909(13) 0.42628(12) 0.0179(3) Uani 1 1 d . . . N3C N 0.27067(13) 0.81445(13) 0.46127(14) 0.0209(3) Uani 1 1 d . . . C1A C 0.91450(16) 0.58090(16) 0.15374(15) 0.0210(4) Uani 1 1 d . . . H1AA H 0.9507 0.5107 0.1064 0.025 Uiso 1 1 calc R . . H1AB H 0.9151 0.5513 0.2333 0.025 Uiso 1 1 calc R . . C2A C 1.00546(16) 0.65259(17) 0.11097(15) 0.0224(4) Uani 1 1 d . . . H2AA H 1.0953 0.5981 0.1037 0.027 Uiso 1 1 calc R . . H2AB H 1.0009 0.6875 0.0335 0.027 Uiso 1 1 calc R . . C3A C 0.97595(16) 0.75188(16) 0.18769(15) 0.0216(4) Uani 1 1 d . . . H3AA H 0.9848 0.7176 0.2643 0.026 Uiso 1 1 calc R . . H3AB H 1.0394 0.7936 0.1545 0.026 Uiso 1 1 calc R . . C4A C 0.83182(16) 0.94484(15) 0.16907(14) 0.0181(3) Uani 1 1 d . . . H4AA H 0.9042 0.9702 0.1336 0.022 Uiso 1 1 calc R . . C5A C 0.69937(16) 1.02714(15) 0.19187(13) 0.0170(3) Uani 1 1 d . . . C6A C 0.7368(2) 1.21116(18) 0.08133(17) 0.0292(4) Uani 1 1 d . . . H6AA H 0.7957 1.2173 0.1204 0.044 Uiso 1 1 calc R . . H6AB H 0.6802 1.2908 0.0650 0.044 Uiso 1 1 calc R . . H6AC H 0.7875 1.1713 0.0093 0.044 Uiso 1 1 calc R . . C7A C 0.52550(17) 1.18210(16) 0.19524(15) 0.0219(4) Uani 1 1 d . . . H7AA H 0.4682 1.2595 0.1832 0.026 Uiso 1 1 calc R . . C8A C 0.49189(16) 1.08847(16) 0.25606(15) 0.0207(4) Uani 1 1 d . . . H8AA H 0.4057 1.0902 0.2937 0.025 Uiso 1 1 calc R . . C1B C 0.71369(17) 0.55061(15) 0.17401(14) 0.0197(3) Uani 1 1 d . . . H1BA H 0.7503 0.5029 0.1052 0.024 Uiso 1 1 calc R . . H1BB H 0.6202 0.5919 0.1820 0.024 Uiso 1 1 calc R . . C2B C 0.72681(17) 0.46593(15) 0.27807(15) 0.0211(4) Uani 1 1 d . . . H2BA H 0.6923 0.4032 0.2758 0.025 Uiso 1 1 calc R . . H2BB H 0.8201 0.4270 0.2724 0.025 Uiso 1 1 calc R . . C3B C 0.65805(17) 0.52316(15) 0.39291(15) 0.0203(3) Uani 1 1 d . . . H3BA H 0.5636 0.5565 0.4023 0.024 Uiso 1 1 calc R . . H3BB H 0.6730 0.4619 0.4552 0.024 Uiso 1 1 calc R . . C4B C 0.74375(16) 0.61411(15) 0.48879(14) 0.0185(3) Uani 1 1 d . . . H4BA H 0.7553 0.5474 0.5414 0.022 Uiso 1 1 calc R . . C5B C 0.77059(15) 0.71857(15) 0.50101(14) 0.0171(3) Uani 1 1 d . . . C6B C 0.8829(2) 0.64750(19) 0.65810(17) 0.0328(4) Uani 1 1 d . . . H6BA H 0.8213 0.6075 0.7016 0.049 Uiso 1 1 calc R . . H6BB H 0.9000 0.6881 0.7108 0.049 Uiso 1 1 calc R . . H6BC H 0.9641 0.5887 0.6175 0.049 Uiso 1 1 calc R . . C7B C 0.82993(16) 0.84838(16) 0.55410(15) 0.0202(4) Uani 1 1 d . . . H7BA H 0.8640 0.8860 0.5921 0.024 Uiso 1 1 calc R . . C8B C 0.77313(16) 0.89711(16) 0.46807(15) 0.0200(4) Uani 1 1 d . . . H8BA H 0.7615 0.9755 0.4355 0.024 Uiso 1 1 calc R . . C1C C 0.77663(16) 0.69755(16) 0.03556(14) 0.0200(4) Uani 1 1 d . . . H1CA H 0.8396 0.6384 -0.0209 0.024 Uiso 1 1 calc R . . H1CB H 0.8083 0.7651 0.0245 0.024 Uiso 1 1 calc R . . C2C C 0.64735(16) 0.74226(16) 0.00799(14) 0.0204(4) Uani 1 1 d . . . H2CA H 0.6628 0.7640 -0.0750 0.024 Uiso 1 1 calc R . . H2CB H 0.6120 0.6766 0.0241 0.024 Uiso 1 1 calc R . . C3C C 0.54615(17) 0.84865(16) 0.07447(14) 0.0211(4) Uani 1 1 d . . . H3CA H 0.5777 0.9168 0.0541 0.025 Uiso 1 1 calc R . . H3CB H 0.4652 0.8711 0.0523 0.025 Uiso 1 1 calc R . . C4C C 0.40218(16) 0.83709(15) 0.25656(15) 0.0191(3) Uani 1 1 d . . . H4CA H 0.3344 0.8568 0.2217 0.023 Uiso 1 1 calc R . . C5C C 0.37912(15) 0.82078(14) 0.37986(15) 0.0177(3) Uani 1 1 d . . . C6C C 0.14782(17) 0.8223(2) 0.4448(2) 0.0333(5) Uani 1 1 d . . . H6CA H 0.1470 0.8508 0.3659 0.050 Uiso 1 1 calc R . . H6CB H 0.0756 0.8777 0.4984 0.050 Uiso 1 1 calc R . . H6CC H 0.1388 0.7437 0.4590 0.050 Uiso 1 1 calc R . . C7C C 0.29695(17) 0.79599(16) 0.56474(16) 0.0229(4) Uani 1 1 d . . . H7CA H 0.2398 0.7873 0.6380 0.027 Uiso 1 1 calc R . . C8C C 0.42165(17) 0.79248(16) 0.54170(15) 0.0214(4) Uani 1 1 d . . . H8CA H 0.4664 0.7803 0.5974 0.026 Uiso 1 1 calc R . . 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 Fe 0.01310(10) 0.01416(10) 0.01456(10) -0.00030(8) -0.00478(8) -0.00484(8) Cl1 0.0373(2) 0.0241(2) 0.0376(2) 0.00834(17) -0.02295(18) -0.01544(18) Cl2 0.02687(19) 0.0247(2) 0.01749(17) -0.00159(15) -0.00608(15) -0.01043(16) O11 0.0424(8) 0.0813(13) 0.0685(11) 0.0336(10) -0.0365(8) -0.0289(9) O12 0.1061(13) 0.0401(9) 0.0538(10) 0.0208(7) -0.0375(9) -0.0471(9) O13 0.0499(9) 0.0397(9) 0.0607(10) -0.0190(8) -0.0098(8) -0.0186(7) O14 0.0524(9) 0.0302(8) 0.0401(8) -0.0031(7) -0.0190(7) 0.0015(7) O21 0.0704(11) 0.0627(11) 0.0252(8) 0.0118(8) 0.0004(8) -0.0342(9) O22 0.0347(8) 0.0325(8) 0.0673(11) -0.0065(8) -0.0166(8) -0.0001(7) O23 0.0261(7) 0.0521(10) 0.0427(8) -0.0087(7) -0.0173(6) -0.0045(7) O24 0.0530(8) 0.0667(10) 0.0234(7) -0.0128(7) -0.0004(6) -0.0403(8) N 0.0167(6) 0.0155(6) 0.0167(6) -0.0011(5) -0.0064(5) -0.0033(5) N1A 0.0140(6) 0.0196(7) 0.0168(6) -0.0021(5) -0.0042(5) -0.0043(5) N2A 0.0170(6) 0.0166(6) 0.0181(6) -0.0010(5) -0.0047(5) -0.0060(5) N3A 0.0253(7) 0.0177(7) 0.0186(6) 0.0021(5) -0.0095(5) -0.0096(6) N1B 0.0171(6) 0.0152(6) 0.0177(6) -0.0012(5) -0.0051(5) -0.0058(5) N2B 0.0161(6) 0.0167(6) 0.0184(6) -0.0016(5) -0.0056(5) -0.0057(5) N3B 0.0170(6) 0.0239(7) 0.0189(6) -0.0016(5) -0.0077(5) -0.0071(5) N1C 0.0189(6) 0.0134(6) 0.0185(6) -0.0011(5) -0.0078(5) -0.0031(5) N2C 0.0166(6) 0.0176(7) 0.0193(6) -0.0014(5) -0.0047(5) -0.0056(5) N3C 0.0133(6) 0.0151(7) 0.0317(8) -0.0047(6) -0.0023(6) -0.0040(5) C1A 0.0164(7) 0.0205(8) 0.0215(8) -0.0039(6) -0.0057(6) 0.0003(6) C2A 0.0143(7) 0.0262(9) 0.0214(8) -0.0037(7) -0.0038(6) -0.0009(7) C3A 0.0129(7) 0.0257(9) 0.0238(8) -0.0026(7) -0.0043(6) -0.0042(6) C4A 0.0183(7) 0.0233(8) 0.0157(7) 0.0001(6) -0.0043(6) -0.0111(6) C5A 0.0213(7) 0.0181(7) 0.0148(7) -0.0005(6) -0.0067(6) -0.0091(6) C6A 0.0389(10) 0.0258(9) 0.0275(9) 0.0082(7) -0.0100(8) -0.0196(8) C7A 0.0242(8) 0.0182(8) 0.0248(8) -0.0028(6) -0.0121(6) -0.0039(7) C8A 0.0165(7) 0.0201(8) 0.0246(8) -0.0033(6) -0.0065(6) -0.0038(6) C1B 0.0242(7) 0.0161(7) 0.0214(7) -0.0028(6) -0.0097(6) -0.0061(6) C2B 0.0262(8) 0.0137(7) 0.0249(8) -0.0015(6) -0.0103(7) -0.0056(6) C3B 0.0260(8) 0.0174(8) 0.0220(7) 0.0018(6) -0.0099(6) -0.0108(6) C4B 0.0188(7) 0.0167(8) 0.0191(7) 0.0012(6) -0.0066(6) -0.0048(6) C5B 0.0145(7) 0.0212(8) 0.0160(7) -0.0020(6) -0.0049(6) -0.0054(6) C6B 0.0419(9) 0.0321(10) 0.0348(9) 0.0075(8) -0.0275(8) -0.0139(8) C7B 0.0157(7) 0.0253(8) 0.0222(8) -0.0057(7) -0.0045(6) -0.0086(6) C8B 0.0195(7) 0.0199(8) 0.0221(8) -0.0024(6) -0.0050(6) -0.0085(6) C1C 0.0202(7) 0.0222(8) 0.0152(7) -0.0017(6) -0.0051(6) -0.0042(7) C2C 0.0235(8) 0.0225(8) 0.0161(7) -0.0010(6) -0.0082(6) -0.0065(7) C3C 0.0226(8) 0.0206(8) 0.0197(7) 0.0021(6) -0.0111(6) -0.0040(7) C4C 0.0171(7) 0.0156(7) 0.0264(8) -0.0040(6) -0.0105(6) -0.0025(6) C5C 0.0145(7) 0.0117(7) 0.0263(8) -0.0036(6) -0.0052(6) -0.0033(6) C6C 0.0142(8) 0.0356(10) 0.0501(12) -0.0119(9) -0.0036(8) -0.0090(8) C7C 0.0224(8) 0.0162(8) 0.0252(8) -0.0009(7) 0.0001(7) -0.0070(7) C8C 0.0200(8) 0.0189(8) 0.0217(8) 0.0000(6) -0.0034(6) -0.0052(7) _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 Fe N2B 2.2313(15) . ? Fe N2C 2.2328(14) . ? Fe N1C 2.2599(15) . ? Fe N2A 2.2669(15) . ? Fe N1A 2.2692(14) . ? Fe N1B 2.2948(14) . ? Fe N 2.4476(14) . ? Cl1 O12 1.4257(18) . ? Cl1 O13 1.4319(18) . ? Cl1 O11 1.4410(17) . ? Cl1 O14 1.4420(17) . ? Cl2 O24 1.4281(15) . ? Cl2 O23 1.4339(16) . ? Cl2 O22 1.4353(17) . ? Cl2 O21 1.4359(17) . ? N C1A 1.492(2) . ? N C1B 1.495(2) . ? N C1C 1.497(2) . ? N1A C4A 1.274(2) . ? N1A C3A 1.461(2) . ? N2A C5A 1.327(2) . ? N2A C8A 1.368(2) . ? N3A C5A 1.353(2) . ? N3A C7A 1.365(2) . ? N3A C6A 1.470(2) . ? N1B C4B 1.275(2) . ? N1B C3B 1.465(2) . ? N2B C5B 1.324(2) . ? N2B C8B 1.368(2) . ? N3B C5B 1.360(2) . ? N3B C7B 1.372(2) . ? N3B C6B 1.466(2) . ? N1C C4C 1.271(2) . ? N1C C3C 1.459(2) . ? N2C C5C 1.331(2) . ? N2C C8C 1.368(2) . ? N3C C5C 1.353(2) . ? N3C C7C 1.370(3) . ? N3C C6C 1.468(2) . ? C1A C2A 1.523(3) . ? C1A H1AA 0.9900 . ? C1A H1AB 0.9900 . ? C2A C3A 1.522(3) . ? C2A H2AA 0.9900 . ? C2A H2AB 0.9900 . ? C3A H3AA 0.9900 . ? C3A H3AB 0.9900 . ? C4A C5A 1.453(2) . ? C4A H4AA 0.9500 . ? C6A H6AA 0.9800 . ? C6A H6AB 0.9800 . ? C6A H6AC 0.9800 . ? C7A C8A 1.369(3) . ? C7A H7AA 0.9500 . ? C8A H8AA 0.9500 . ? C1B C2B 1.522(2) . ? C1B H1BA 0.9900 . ? C1B H1BB 0.9900 . ? C2B C3B 1.518(2) . ? C2B H2BA 0.9900 . ? C2B H2BB 0.9900 . ? C3B H3BA 0.9900 . ? C3B H3BB 0.9900 . ? C4B C5B 1.452(3) . ? C4B H4BA 0.9500 . ? C6B H6BA 0.9800 . ? C6B H6BB 0.9800 . ? C6B H6BC 0.9800 . ? C7B C8B 1.366(2) . ? C7B H7BA 0.9500 . ? C8B H8BA 0.9500 . ? C1C C2C 1.523(2) . ? C1C H1CA 0.9900 . ? C1C H1CB 0.9900 . ? C2C C3C 1.522(2) . ? C2C H2CA 0.9900 . ? C2C H2CB 0.9900 . ? C3C H3CA 0.9900 . ? C3C H3CB 0.9900 . ? C4C C5C 1.451(2) . ? C4C H4CA 0.9500 . ? C6C H6CA 0.9800 . ? C6C H6CB 0.9800 . ? C6C H6CC 0.9800 . ? C7C C8C 1.366(3) . ? C7C H7CA 0.9500 . ? C8C H8CA 0.9500 . ? 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 N2B Fe N2C 88.67(5) . . ? N2B Fe N1C 157.35(5) . . ? N2C Fe N1C 73.25(5) . . ? N2B Fe N2A 90.79(5) . . ? N2C Fe N2A 92.53(5) . . ? N1C Fe N2A 76.84(5) . . ? N2B Fe N1A 76.68(5) . . ? N2C Fe N1A 158.81(5) . . ? N1C Fe N1A 116.36(5) . . ? N2A Fe N1A 72.74(5) . . ? N2B Fe N1B 72.40(5) . . ? N2C Fe N1B 76.02(5) . . ? N1C Fe N1B 114.69(5) . . ? N2A Fe N1B 159.61(5) . . ? N1A Fe N1B 112.94(5) . . ? N2B Fe N 125.62(5) . . ? N2C Fe N 124.46(5) . . ? N1C Fe N 76.71(5) . . ? N2A Fe N 124.30(5) . . ? N1A Fe N 76.74(5) . . ? N1B Fe N 75.79(5) . . ? O12 Cl1 O13 109.40(11) . . ? O12 Cl1 O11 111.07(12) . . ? O13 Cl1 O11 108.06(12) . . ? O12 Cl1 O14 110.59(11) . . ? O13 Cl1 O14 107.93(11) . . ? O11 Cl1 O14 109.71(10) . . ? O24 Cl2 O23 110.13(9) . . ? O24 Cl2 O22 108.93(11) . . ? O23 Cl2 O22 108.99(11) . . ? O24 Cl2 O21 110.17(11) . . ? O23 Cl2 O21 110.86(11) . . ? O22 Cl2 O21 107.70(11) . . ? C1A N C1B 108.00(13) . . ? C1A N C1C 107.90(13) . . ? C1B N C1C 107.46(13) . . ? C1A N Fe 111.39(10) . . ? C1B N Fe 111.48(9) . . ? C1C N Fe 110.46(10) . . ? C4A N1A C3A 118.08(15) . . ? C4A N1A Fe 117.39(11) . . ? C3A N1A Fe 123.68(11) . . ? C5A N2A C8A 105.53(14) . . ? C5A N2A Fe 112.92(11) . . ? C8A N2A Fe 140.50(12) . . ? C5A N3A C7A 106.92(15) . . ? C5A N3A C6A 127.27(15) . . ? C7A N3A C6A 125.73(15) . . ? C4B N1B C3B 118.88(15) . . ? C4B N1B Fe 116.70(12) . . ? C3B N1B Fe 122.81(11) . . ? C5B N2B C8B 105.96(14) . . ? C5B N2B Fe 114.58(12) . . ? C8B N2B Fe 138.72(12) . . ? C5B N3B C7B 106.68(14) . . ? C5B N3B C6B 127.73(16) . . ? C7B N3B C6B 125.55(16) . . ? C4C N1C C3C 118.53(15) . . ? C4C N1C Fe 116.90(12) . . ? C3C N1C Fe 123.58(11) . . ? C5C N2C C8C 105.67(14) . . ? C5C N2C Fe 113.25(11) . . ? C8C N2C Fe 140.11(12) . . ? C5C N3C C7C 107.05(15) . . ? C5C N3C C6C 127.71(17) . . ? C7C N3C C6C 125.22(16) . . ? N C1A C2A 117.36(14) . . ? N C1A H1AA 108.0 . . ? C2A C1A H1AA 108.0 . . ? N C1A H1AB 108.0 . . ? C2A C1A H1AB 108.0 . . ? H1AA C1A H1AB 107.2 . . ? C3A C2A C1A 114.35(14) . . ? C3A C2A H2AA 108.7 . . ? C1A C2A H2AA 108.7 . . ? C3A C2A H2AB 108.7 . . ? C1A C2A H2AB 108.7 . . ? H2AA C2A H2AB 107.6 . . ? N1A C3A C2A 111.05(15) . . ? N1A C3A H3AA 109.4 . . ? C2A C3A H3AA 109.4 . . ? N1A C3A H3AB 109.4 . . ? C2A C3A H3AB 109.4 . . ? H3AA C3A H3AB 108.0 . . ? N1A C4A C5A 115.91(15) . . ? N1A C4A H4AA 122.0 . . ? C5A C4A H4AA 122.0 . . ? N2A C5A N3A 111.46(14) . . ? N2A C5A C4A 120.53(15) . . ? N3A C5A C4A 128.01(15) . . ? N3A C6A H6AA 109.5 . . ? N3A C6A H6AB 109.5 . . ? H6AA C6A H6AB 109.5 . . ? N3A C6A H6AC 109.5 . . ? H6AA C6A H6AC 109.5 . . ? H6AB C6A H6AC 109.5 . . ? N3A C7A C8A 106.42(15) . . ? N3A C7A H7AA 126.8 . . ? C8A C7A H7AA 126.8 . . ? N2A C8A C7A 109.66(15) . . ? N2A C8A H8AA 125.2 . . ? C7A C8A H8AA 125.2 . . ? N C1B C2B 116.69(14) . . ? N C1B H1BA 108.1 . . ? C2B C1B H1BA 108.1 . . ? N C1B H1BB 108.1 . . ? C2B C1B H1BB 108.1 . . ? H1BA C1B H1BB 107.3 . . ? C3B C2B C1B 114.95(14) . . ? C3B C2B H2BA 108.5 . . ? C1B C2B H2BA 108.5 . . ? C3B C2B H2BB 108.5 . . ? C1B C2B H2BB 108.5 . . ? H2BA C2B H2BB 107.5 . . ? N1B C3B C2B 111.85(14) . . ? N1B C3B H3BA 109.2 . . ? C2B C3B H3BA 109.2 . . ? N1B C3B H3BB 109.2 . . ? C2B C3B H3BB 109.2 . . ? H3BA C3B H3BB 107.9 . . ? N1B C4B C5B 115.63(15) . . ? N1B C4B H4BA 122.2 . . ? C5B C4B H4BA 122.2 . . ? N2B C5B N3B 111.25(16) . . ? N2B C5B C4B 120.02(15) . . ? N3B C5B C4B 128.72(15) . . ? N3B C6B H6BA 109.5 . . ? N3B C6B H6BB 109.5 . . ? H6BA C6B H6BB 109.5 . . ? N3B C6B H6BC 109.5 . . ? H6BA C6B H6BC 109.5 . . ? H6BB C6B H6BC 109.5 . . ? C8B C7B N3B 106.50(16) . . ? C8B C7B H7BA 126.7 . . ? N3B C7B H7BA 126.7 . . ? C7B C8B N2B 109.60(16) . . ? C7B C8B H8BA 125.2 . . ? N2B C8B H8BA 125.2 . . ? N C1C C2C 116.67(14) . . ? N C1C H1CA 108.1 . . ? C2C C1C H1CA 108.1 . . ? N C1C H1CB 108.1 . . ? C2C C1C H1CB 108.1 . . ? H1CA C1C H1CB 107.3 . . ? C3C C2C C1C 114.58(15) . . ? C3C C2C H2CA 108.6 . . ? C1C C2C H2CA 108.6 . . ? C3C C2C H2CB 108.6 . . ? C1C C2C H2CB 108.6 . . ? H2CA C2C H2CB 107.6 . . ? N1C C3C C2C 111.78(14) . . ? N1C C3C H3CA 109.3 . . ? C2C C3C H3CA 109.3 . . ? N1C C3C H3CB 109.3 . . ? C2C C3C H3CB 109.3 . . ? H3CA C3C H3CB 107.9 . . ? N1C C4C C5C 115.92(15) . . ? N1C C4C H4CA 122.0 . . ? C5C C4C H4CA 122.0 . . ? N2C C5C N3C 111.15(15) . . ? N2C C5C C4C 120.11(15) . . ? N3C C5C C4C 128.75(16) . . ? N3C C6C H6CA 109.5 . . ? N3C C6C H6CB 109.5 . . ? H6CA C6C H6CB 109.5 . . ? N3C C6C H6CC 109.5 . . ? H6CA C6C H6CC 109.5 . . ? H6CB C6C H6CC 109.5 . . ? C8C C7C N3C 106.34(15) . . ? C8C C7C H7CA 126.8 . . ? N3C C7C H7CA 126.8 . . ? C7C C8C N2C 109.78(16) . . ? C7C C8C H8CA 125.1 . . ? N2C C8C H8CA 125.1 . . ? 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 N2B Fe N C1A -11.99(13) . . . . ? N2C Fe N C1A -129.17(11) . . . . ? N1C Fe N C1A 172.25(12) . . . . ? N2A Fe N C1A 108.63(11) . . . . ? N1A Fe N C1A 50.62(11) . . . . ? N1B Fe N C1A -67.59(11) . . . . ? N2B Fe N C1B 108.72(11) . . . . ? N2C Fe N C1B -8.47(12) . . . . ? N1C Fe N C1B -67.05(10) . . . . ? N2A Fe N C1B -130.67(10) . . . . ? N1A Fe N C1B 171.33(11) . . . . ? N1B Fe N C1B 53.12(10) . . . . ? N2B Fe N C1C -131.89(11) . . . . ? N2C Fe N C1C 110.93(11) . . . . ? N1C Fe N C1C 52.35(11) . . . . ? N2A Fe N C1C -11.27(13) . . . . ? N1A Fe N C1C -69.28(11) . . . . ? N1B Fe N C1C 172.51(12) . . . . ? N2B Fe N1A C4A -94.03(13) . . . . ? N2C Fe N1A C4A -46.6(2) . . . . ? N1C Fe N1A C4A 66.21(14) . . . . ? N2A Fe N1A C4A 1.04(12) . . . . ? N1B Fe N1A C4A -158.08(12) . . . . ? N Fe N1A C4A 133.85(13) . . . . ? N2B Fe N1A C3A 75.18(13) . . . . ? N2C Fe N1A C3A 122.60(16) . . . . ? N1C Fe N1A C3A -124.58(13) . . . . ? N2A Fe N1A C3A 170.25(14) . . . . ? N1B Fe N1A C3A 11.13(14) . . . . ? N Fe N1A C3A -56.93(13) . . . . ? N2B Fe N2A C5A 79.17(12) . . . . ? N2C Fe N2A C5A 167.87(12) . . . . ? N1C Fe N2A C5A -119.99(12) . . . . ? N1A Fe N2A C5A 3.38(11) . . . . ? N1B Fe N2A C5A 112.98(16) . . . . ? N Fe N2A C5A -56.43(13) . . . . ? N2B Fe N2A C8A -114.90(18) . . . . ? N2C Fe N2A C8A -26.20(19) . . . . ? N1C Fe N2A C8A 45.94(18) . . . . ? N1A Fe N2A C8A 169.31(19) . . . . ? N1B Fe N2A C8A -81.1(2) . . . . ? N Fe N2A C8A 109.50(18) . . . . ? N2B Fe N1B C4B 1.52(12) . . . . ? N2C Fe N1B C4B -91.57(12) . . . . ? N1C Fe N1B C4B -155.38(11) . . . . ? N2A Fe N1B C4B -34.2(2) . . . . ? N1A Fe N1B C4B 68.15(13) . . . . ? N Fe N1B C4B 136.79(13) . . . . ? N2B Fe N1B C3B 166.83(13) . . . . ? N2C Fe N1B C3B 73.74(12) . . . . ? N1C Fe N1B C3B 9.93(13) . . . . ? N2A Fe N1B C3B 131.11(15) . . . . ? N1A Fe N1B C3B -126.54(12) . . . . ? N Fe N1B C3B -57.89(12) . . . . ? N2C Fe N2B C5B 79.40(11) . . . . ? N1C Fe N2B C5B 115.84(15) . . . . ? N2A Fe N2B C5B 171.91(11) . . . . ? N1A Fe N2B C5B -116.04(12) . . . . ? N1B Fe N2B C5B 3.64(11) . . . . ? N Fe N2B C5B -53.41(13) . . . . ? N2C Fe N2B C8B -112.26(16) . . . . ? N1C Fe N2B C8B -75.8(2) . . . . ? N2A Fe N2B C8B -19.74(16) . . . . ? N1A Fe N2B C8B 52.30(16) . . . . ? N1B Fe N2B C8B 171.99(17) . . . . ? N Fe N2B C8B 114.94(16) . . . . ? N2B Fe N1C C4C -36.8(2) . . . . ? N2C Fe N1C C4C 1.48(12) . . . . ? N2A Fe N1C C4C -95.28(13) . . . . ? N1A Fe N1C C4C -158.15(12) . . . . ? N1B Fe N1C C4C 66.90(14) . . . . ? N Fe N1C C4C 134.18(13) . . . . ? N2B Fe N1C C3C 131.63(15) . . . . ? N2C Fe N1C C3C 169.96(14) . . . . ? N2A Fe N1C C3C 73.20(13) . . . . ? N1A Fe N1C C3C 10.32(14) . . . . ? N1B Fe N1C C3C -124.62(12) . . . . ? N Fe N1C C3C -57.34(13) . . . . ? N2B Fe N2C C5C 169.42(12) . . . . ? N1C Fe N2C C5C 3.24(11) . . . . ? N2A Fe N2C C5C 78.69(12) . . . . ? N1A Fe N2C C5C 123.64(15) . . . . ? N1B Fe N2C C5C -118.39(12) . . . . ? N Fe N2C C5C -56.91(13) . . . . ? N2B Fe N2C C8C -24.13(19) . . . . ? N1C Fe N2C C8C 169.7(2) . . . . ? N2A Fe N2C C8C -114.87(19) . . . . ? N1A Fe N2C C8C -69.9(2) . . . . ? N1B Fe N2C C8C 48.06(18) . . . . ? N Fe N2C C8C 109.54(19) . . . . ? C1B N C1A C2A 168.14(14) . . . . ? C1C N C1A C2A 52.27(19) . . . . ? Fe N C1A C2A -69.14(16) . . . . ? N C1A C2A C3A 67.8(2) . . . . ? C4A N1A C3A C2A -121.72(17) . . . . ? Fe N1A C3A C2A 69.14(17) . . . . ? C1A C2A C3A N1A -59.5(2) . . . . ? C3A N1A C4A C5A -174.83(14) . . . . ? Fe N1A C4A C5A -5.00(19) . . . . ? C8A N2A C5A N3A 1.02(19) . . . . ? Fe N2A C5A N3A 171.78(11) . . . . ? C8A N2A C5A C4A -178.18(15) . . . . ? Fe N2A C5A C4A -7.4(2) . . . . ? C7A N3A C5A N2A -0.93(19) . . . . ? C6A N3A C5A N2A -177.81(16) . . . . ? C7A N3A C5A C4A 178.20(17) . . . . ? C6A N3A C5A C4A 1.3(3) . . . . ? N1A C4A C5A N2A 8.6(2) . . . . ? N1A C4A C5A N3A -170.45(16) . . . . ? C5A N3A C7A C8A 0.43(19) . . . . ? C6A N3A C7A C8A 177.37(17) . . . . ? C5A N2A C8A C7A -0.7(2) . . . . ? Fe N2A C8A C7A -167.28(13) . . . . ? N3A C7A C8A N2A 0.2(2) . . . . ? C1A N C1B C2B 51.97(18) . . . . ? C1C N C1B C2B 168.13(14) . . . . ? Fe N C1B C2B -70.70(15) . . . . ? N C1B C2B C3B 66.3(2) . . . . ? C4B N1B C3B C2B -126.32(16) . . . . ? Fe N1B C3B C2B 68.67(16) . . . . ? C1B C2B C3B N1B -58.1(2) . . . . ? C3B N1B C4B C5B -171.92(14) . . . . ? Fe N1B C4B C5B -6.01(18) . . . . ? C8B N2B C5B N3B 0.69(18) . . . . ? Fe N2B C5B N3B 172.72(10) . . . . ? C8B N2B C5B C4B 179.65(14) . . . . ? Fe N2B C5B C4B -8.32(18) . . . . ? C7B N3B C5B N2B -0.46(18) . . . . ? C6B N3B C5B N2B -178.22(16) . . . . ? C7B N3B C5B C4B -179.31(16) . . . . ? C6B N3B C5B C4B 2.9(3) . . . . ? N1B C4B C5B N2B 9.8(2) . . . . ? N1B C4B C5B N3B -171.42(16) . . . . ? C5B N3B C7B C8B 0.03(18) . . . . ? C6B N3B C7B C8B 177.86(16) . . . . ? N3B C7B C8B N2B 0.38(18) . . . . ? C5B N2B C8B C7B -0.66(18) . . . . ? Fe N2B C8B C7B -169.64(12) . . . . ? C1A N C1C C2C 167.31(15) . . . . ? C1B N C1C C2C 51.09(19) . . . . ? Fe N C1C C2C -70.71(17) . . . . ? N C1C C2C C3C 67.6(2) . . . . ? C4C N1C C3C C2C -123.64(17) . . . . ? Fe N1C C3C C2C 68.06(18) . . . . ? C1C C2C C3C N1C -58.1(2) . . . . ? C3C N1C C4C C5C -174.72(15) . . . . ? Fe N1C C4C C5C -5.6(2) . . . . ? C8C N2C C5C N3C 1.13(19) . . . . ? Fe N2C C5C N3C 172.14(11) . . . . ? C8C N2C C5C C4C -178.54(15) . . . . ? Fe N2C C5C C4C -7.52(19) . . . . ? C7C N3C C5C N2C -0.93(19) . . . . ? C6C N3C C5C N2C -179.47(17) . . . . ? C7C N3C C5C C4C 178.69(17) . . . . ? C6C N3C C5C C4C 0.2(3) . . . . ? N1C C4C C5C N2C 9.1(2) . . . . ? N1C C4C C5C N3C -170.52(17) . . . . ? C5C N3C C7C C8C 0.34(19) . . . . ? C6C N3C C7C C8C 178.92(17) . . . . ? N3C C7C C8C N2C 0.3(2) . . . . ? C5C N2C C8C C7C -0.9(2) . . . . ? Fe N2C C8C C7C -167.97(14) . . . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 1.104 _refine_diff_density_min -0.819 _refine_diff_density_rms 0.072 #===END data_llc26m _database_code_depnum_ccdc_archive 'CCDC 277350' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H36 Cl2 Mn N10 O8' _chemical_formula_weight 718.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.623(2) _cell_length_b 12.170(3) _cell_length_c 12.343(3) _cell_angle_alpha 81.688(3) _cell_angle_beta 71.360(3) _cell_angle_gamma 67.784(3) _cell_volume 1531.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 6953 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 28.25 _exptl_crystal_description plate _exptl_crystal_colour pale _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 746 _exptl_absorpt_coefficient_mu 0.670 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7199 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11580 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0425 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 28.29 _reflns_number_total 7170 _reflns_number_gt 5882 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0406P)^2^+1.3190P] 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_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7170 _refine_ls_number_parameters 410 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.0972 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.000 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 Mn Mn 0.34022(3) 0.70350(3) 0.19990(2) 0.01143(8) Uani 1 1 d . . . Cl1 Cl -0.07894(5) 0.40052(5) 0.32115(4) 0.01831(11) Uani 1 1 d . . . Cl2 Cl 0.34230(5) 1.05283(5) -0.29081(5) 0.02458(13) Uani 1 1 d . . . O11 O 0.00615(17) 0.27894(16) 0.30851(18) 0.0393(5) Uani 1 1 d . . . O12 O -0.0320(2) 0.4685(2) 0.22332(15) 0.0433(5) Uani 1 1 d . . . O13 O -0.07918(17) 0.44431(17) 0.42334(14) 0.0324(4) Uani 1 1 d . . . O14 O -0.20744(15) 0.40796(16) 0.32845(15) 0.0290(4) Uani 1 1 d . . . O21 O 0.44212(19) 0.9857(2) -0.23688(19) 0.0495(6) Uani 1 1 d . . . O22 O 0.3711(2) 1.15089(18) -0.35666(18) 0.0482(5) Uani 1 1 d . . . O23 O 0.21929(18) 1.09397(16) -0.20399(16) 0.0375(4) Uani 1 1 d . . . O24 O 0.33456(19) 0.97593(17) -0.36360(18) 0.0399(5) Uani 1 1 d . . . N N 0.22506(16) 0.85655(15) 0.34285(14) 0.0138(3) Uani 1 1 d . . . N1A N 0.29861(16) 0.88339(14) 0.08974(14) 0.0143(3) Uani 1 1 d . . . N2A N 0.26670(16) 0.68418(15) 0.05321(14) 0.0146(3) Uani 1 1 d . . . N3A N 0.17504(16) 0.76791(16) -0.08428(15) 0.0167(3) Uani 1 1 d . . . N1B N 0.15409(16) 0.65993(15) 0.29505(14) 0.0148(3) Uani 1 1 d . . . N2B N 0.40024(16) 0.50008(15) 0.24749(14) 0.0148(3) Uani 1 1 d . . . N3B N 0.33761(17) 0.35443(15) 0.34600(15) 0.0161(3) Uani 1 1 d . . . N1C N 0.49131(16) 0.67274(14) 0.29655(14) 0.0147(3) Uani 1 1 d . . . N2C N 0.53814(16) 0.68769(15) 0.06659(15) 0.0151(3) Uani 1 1 d . . . N3C N 0.73814(16) 0.68304(15) 0.03421(15) 0.0173(4) Uani 1 1 d . . . C1A C 0.2861(2) 0.94914(18) 0.32171(17) 0.0166(4) Uani 1 1 d . . . H1AA H 0.3802 0.9081 0.3122 0.020 Uiso 1 1 calc R . . H1AB H 0.2497 0.9970 0.3912 0.020 Uiso 1 1 calc R . . C2A C 0.2706(2) 1.03397(17) 0.21964(18) 0.0177(4) Uani 1 1 d . . . H2AA H 0.3023 1.0977 0.2238 0.021 Uiso 1 1 calc R . . H2AB H 0.1769 1.0717 0.2261 0.021 Uiso 1 1 calc R . . C3A C 0.3408(2) 0.97842(18) 0.10273(17) 0.0170(4) Uani 1 1 d . . . H3AA H 0.3239 1.0404 0.0425 0.020 Uiso 1 1 calc R . . H3AB H 0.4355 0.9460 0.0925 0.020 Uiso 1 1 calc R . . C4A C 0.25942(19) 0.88629(18) 0.00366(17) 0.0157(4) Uani 1 1 d . . . H4AA H 0.2482 0.9524 -0.0484 0.019 Uiso 1 1 calc R . . C5A C 0.23292(18) 0.78208(18) -0.00999(17) 0.0149(4) Uani 1 1 d . . . C6A C 0.22771(19) 0.60506(19) 0.01918(18) 0.0175(4) Uani 1 1 d . . . H6AA H 0.2382 0.5270 0.0503 0.021 Uiso 1 1 calc R . . C7A C 0.17141(19) 0.65548(19) -0.06619(18) 0.0182(4) Uani 1 1 d . . . H7AA H 0.1367 0.6197 -0.1052 0.022 Uiso 1 1 calc R . . C8A C 0.1212(2) 0.8566(2) -0.1661(2) 0.0282(5) Uani 1 1 d . . . H8A1 H 0.0909 0.9363 -0.1364 0.042 Uiso 0.43(4) 1 calc PR A 1 H8A2 H 0.0481 0.8423 -0.1770 0.042 Uiso 0.43(4) 1 calc PR A 1 H8A3 H 0.1884 0.8505 -0.2395 0.042 Uiso 0.43(4) 1 calc PR A 1 H8A4 H 0.1130 0.8165 -0.2251 0.042 Uiso 0.57(4) 1 d PR A 2 H8A5 H 0.1791 0.9012 -0.2019 0.042 Uiso 0.57(4) 1 d PR A 2 H8A6 H 0.0354 0.9113 -0.1259 0.042 Uiso 0.57(4) 1 d PR A 2 C1B C 0.08651(19) 0.91714(18) 0.34457(18) 0.0177(4) Uani 1 1 d . . . H1BA H 0.0845 0.9462 0.2658 0.021 Uiso 1 1 calc R . . H1BB H 0.0495 0.9877 0.3927 0.021 Uiso 1 1 calc R . . C2B C -0.00303(19) 0.84525(18) 0.38756(18) 0.0173(4) Uani 1 1 d . . . H2BA H 0.0050 0.8090 0.4632 0.021 Uiso 1 1 calc R . . H2BB H -0.0938 0.9002 0.3986 0.021 Uiso 1 1 calc R . . C3B C 0.02383(18) 0.74718(19) 0.30870(19) 0.0180(4) Uani 1 1 d . . . H3BA H -0.0407 0.7076 0.3412 0.022 Uiso 1 1 calc R . . H3BB H 0.0149 0.7823 0.2330 0.022 Uiso 1 1 calc R . . C4B C 0.16729(19) 0.55248(18) 0.32564(17) 0.0146(4) Uani 1 1 d . . . H4BA H 0.0945 0.5284 0.3593 0.018 Uiso 1 1 calc R . . C5B C 0.29943(19) 0.46861(17) 0.30649(17) 0.0141(4) Uani 1 1 d . . . C6B C 0.5073(2) 0.40245(18) 0.25113(18) 0.0179(4) Uani 1 1 d . . . H6BA H 0.5945 0.3983 0.2170 0.022 Uiso 1 1 calc R . . C7B C 0.4707(2) 0.31148(19) 0.31102(18) 0.0184(4) Uani 1 1 d . . . H7BA H 0.5263 0.2340 0.3255 0.022 Uiso 1 1 calc R . . C8B C 0.2554(2) 0.2894(2) 0.4181(2) 0.0237(5) Uani 1 1 d . . . H8BA H 0.2003 0.2813 0.3763 0.036 Uiso 1 1 calc R . . H8BB H 0.2006 0.3330 0.4882 0.036 Uiso 1 1 calc R . . H8BC H 0.3104 0.2104 0.4380 0.036 Uiso 1 1 calc R . . C1C C 0.22837(19) 0.80172(18) 0.45867(17) 0.0159(4) Uani 1 1 d . . . H1CA H 0.1995 0.7331 0.4687 0.019 Uiso 1 1 calc R . . H1CB H 0.1639 0.8604 0.5163 0.019 Uiso 1 1 calc R . . C2C C 0.35815(19) 0.75898(18) 0.48546(17) 0.0162(4) Uani 1 1 d . . . H2CA H 0.3917 0.8251 0.4685 0.019 Uiso 1 1 calc R . . H2CB H 0.3427 0.7399 0.5684 0.019 Uiso 1 1 calc R . . C3C C 0.4623(2) 0.65121(18) 0.42067(17) 0.0173(4) Uani 1 1 d . . . H3CA H 0.5424 0.6310 0.4434 0.021 Uiso 1 1 calc R . . H3CB H 0.4327 0.5826 0.4416 0.021 Uiso 1 1 calc R . . C4C C 0.60714(19) 0.65987(17) 0.23763(17) 0.0153(4) Uani 1 1 d . . . H4CA H 0.6750 0.6407 0.2720 0.018 Uiso 1 1 calc R . . C5C C 0.62976(18) 0.67627(17) 0.11452(18) 0.0145(4) Uani 1 1 d . . . C6C C 0.5898(2) 0.70400(18) -0.04825(18) 0.0182(4) Uani 1 1 d . . . H6CA H 0.5462 0.7156 -0.1046 0.022 Uiso 1 1 calc R . . C7C C 0.7136(2) 0.70103(18) -0.06941(18) 0.0191(4) Uani 1 1 d . . . H7CA H 0.7712 0.7097 -0.1418 0.023 Uiso 1 1 calc R . . C8C C 0.8593(2) 0.6767(2) 0.0514(2) 0.0261(5) Uani 1 1 d . . . H8CA H 0.8466 0.6824 0.1331 0.039 Uiso 1 1 calc R . . H8CB H 0.8849 0.7424 0.0090 0.039 Uiso 1 1 calc R . . H8CC H 0.9276 0.6010 0.0237 0.039 Uiso 1 1 calc R . . 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 0.01181(14) 0.01174(14) 0.01135(15) -0.00036(11) -0.00440(11) -0.00393(11) Cl1 0.0210(2) 0.0217(2) 0.0139(2) -0.00180(19) -0.00479(19) -0.0090(2) Cl2 0.0322(3) 0.0198(3) 0.0302(3) 0.0049(2) -0.0185(2) -0.0124(2) O11 0.0314(10) 0.0275(10) 0.0549(13) -0.0131(9) -0.0143(9) -0.0002(8) O12 0.0556(12) 0.0603(14) 0.0211(9) 0.0115(9) -0.0065(9) -0.0366(11) O13 0.0407(10) 0.0479(11) 0.0174(8) -0.0099(8) -0.0030(7) -0.0265(9) O14 0.0216(8) 0.0367(10) 0.0312(9) 0.0008(8) -0.0123(7) -0.0097(7) O21 0.0373(11) 0.0644(14) 0.0567(14) 0.0235(11) -0.0325(10) -0.0223(10) O22 0.0865(16) 0.0350(11) 0.0435(12) 0.0162(9) -0.0305(12) -0.0401(11) O23 0.0436(11) 0.0267(9) 0.0328(10) -0.0027(8) -0.0151(9) 0.0018(8) O24 0.0439(11) 0.0316(10) 0.0493(12) -0.0163(9) -0.0112(9) -0.0152(9) N 0.0138(8) 0.0143(8) 0.0129(8) -0.0011(6) -0.0048(6) -0.0033(6) N1A 0.0156(8) 0.0127(8) 0.0140(8) -0.0013(6) -0.0040(7) -0.0043(6) N2A 0.0155(8) 0.0142(8) 0.0147(8) -0.0017(6) -0.0051(7) -0.0050(6) N3A 0.0163(8) 0.0211(9) 0.0148(8) -0.0008(7) -0.0078(7) -0.0063(7) N1B 0.0145(8) 0.0161(8) 0.0131(8) -0.0019(6) -0.0048(7) -0.0037(7) N2B 0.0156(8) 0.0153(8) 0.0141(8) -0.0009(6) -0.0045(7) -0.0055(7) N3B 0.0211(9) 0.0150(8) 0.0149(8) 0.0003(7) -0.0077(7) -0.0073(7) N1C 0.0166(8) 0.0121(8) 0.0150(8) -0.0016(6) -0.0068(7) -0.0024(6) N2C 0.0151(8) 0.0151(8) 0.0153(8) -0.0007(7) -0.0055(7) -0.0046(7) N3C 0.0139(8) 0.0143(8) 0.0218(9) -0.0019(7) -0.0027(7) -0.0044(7) C1A 0.0229(10) 0.0141(9) 0.0154(10) -0.0024(8) -0.0080(8) -0.0065(8) C2A 0.0237(10) 0.0101(9) 0.0202(10) -0.0013(8) -0.0092(9) -0.0044(8) C3A 0.0229(10) 0.0148(10) 0.0169(10) 0.0022(8) -0.0089(8) -0.0089(8) C4A 0.0182(9) 0.0144(9) 0.0139(9) -0.0002(7) -0.0064(8) -0.0038(8) C5A 0.0136(9) 0.0181(10) 0.0133(9) -0.0016(8) -0.0052(7) -0.0045(8) C6A 0.0180(10) 0.0181(10) 0.0179(10) -0.0022(8) -0.0041(8) -0.0081(8) C7A 0.0157(9) 0.0238(11) 0.0181(10) -0.0055(8) -0.0037(8) -0.0094(8) C8A 0.0385(13) 0.0286(12) 0.0274(12) 0.0066(10) -0.0253(11) -0.0123(10) C1B 0.0148(9) 0.0152(9) 0.0186(10) -0.0027(8) -0.0051(8) 0.0007(8) C2B 0.0122(9) 0.0191(10) 0.0166(10) -0.0042(8) -0.0032(8) -0.0007(8) C3B 0.0112(9) 0.0196(10) 0.0219(11) -0.0018(8) -0.0050(8) -0.0034(8) C4B 0.0155(9) 0.0191(10) 0.0114(9) -0.0010(8) -0.0040(7) -0.0081(8) C5B 0.0182(9) 0.0140(9) 0.0122(9) 0.0001(7) -0.0058(8) -0.0071(8) C6B 0.0148(9) 0.0170(10) 0.0205(10) -0.0043(8) -0.0049(8) -0.0028(8) C7B 0.0215(10) 0.0162(10) 0.0190(10) -0.0011(8) -0.0110(9) -0.0039(8) C8B 0.0308(12) 0.0212(11) 0.0230(11) 0.0053(9) -0.0087(10) -0.0146(10) C1C 0.0169(9) 0.0177(10) 0.0109(9) -0.0009(8) -0.0038(8) -0.0038(8) C2C 0.0197(10) 0.0182(10) 0.0116(9) -0.0009(8) -0.0064(8) -0.0061(8) C3C 0.0195(10) 0.0191(10) 0.0130(10) 0.0019(8) -0.0081(8) -0.0046(8) C4C 0.0157(9) 0.0126(9) 0.0188(10) -0.0026(8) -0.0084(8) -0.0027(7) C5C 0.0127(9) 0.0113(9) 0.0190(10) -0.0034(8) -0.0038(8) -0.0034(7) C6C 0.0201(10) 0.0174(10) 0.0148(10) 0.0008(8) -0.0048(8) -0.0048(8) C7C 0.0224(10) 0.0140(10) 0.0169(10) 0.0004(8) -0.0011(8) -0.0063(8) C8C 0.0142(10) 0.0297(12) 0.0351(13) -0.0064(10) -0.0033(9) -0.0097(9) _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 Mn N2A 2.3080(17) . ? Mn N1C 2.3153(16) . ? Mn N2C 2.3181(17) . ? Mn N1B 2.3247(17) . ? Mn N2B 2.3444(18) . ? Mn N1A 2.3736(17) . ? Mn N 2.4350(17) . ? Cl1 O11 1.4330(18) . ? Cl1 O14 1.4356(16) . ? Cl1 O13 1.4373(16) . ? Cl1 O12 1.4392(18) . ? Cl2 O22 1.4298(19) . ? Cl2 O24 1.4318(18) . ? Cl2 O21 1.4408(18) . ? Cl2 O23 1.441(2) . ? N C1B 1.491(2) . ? N C1C 1.493(2) . ? N C1A 1.498(3) . ? N1A C4A 1.274(3) . ? N1A C3A 1.462(3) . ? N2A C5A 1.325(3) . ? N2A C6A 1.370(3) . ? N3A C5A 1.361(2) . ? N3A C7A 1.369(3) . ? N3A C8A 1.468(3) . ? N1B C4B 1.272(3) . ? N1B C3B 1.456(2) . ? N2B C5B 1.328(3) . ? N2B C6B 1.365(3) . ? N3B C5B 1.357(3) . ? N3B C7B 1.371(3) . ? N3B C8B 1.469(3) . ? N1C C4C 1.270(3) . ? N1C C3C 1.466(3) . ? N2C C5C 1.331(2) . ? N2C C6C 1.369(3) . ? N3C C5C 1.354(3) . ? N3C C7C 1.368(3) . ? N3C C8C 1.462(3) . ? C1A C2A 1.521(3) . ? C1A H1AA 0.9900 . ? C1A H1AB 0.9900 . ? C2A C3A 1.522(3) . ? C2A H2AA 0.9900 . ? C2A H2AB 0.9900 . ? C3A H3AA 0.9900 . ? C3A H3AB 0.9900 . ? C4A C5A 1.457(3) . ? C4A H4AA 0.9500 . ? C6A C7A 1.366(3) . ? C6A H6AA 0.9500 . ? C7A H7AA 0.9500 . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C8A H8A3 0.9800 . ? C8A H8A4 0.9800 . ? C8A H8A5 0.9799 . ? C8A H8A6 0.9800 . ? C1B C2B 1.527(3) . ? C1B H1BA 0.9900 . ? C1B H1BB 0.9900 . ? C2B C3B 1.526(3) . ? C2B H2BA 0.9900 . ? C2B H2BB 0.9900 . ? C3B H3BA 0.9900 . ? C3B H3BB 0.9900 . ? C4B C5B 1.452(3) . ? C4B H4BA 0.9500 . ? C6B C7B 1.368(3) . ? C6B H6BA 0.9500 . ? C7B H7BA 0.9500 . ? C8B H8BA 0.9800 . ? C8B H8BB 0.9800 . ? C8B H8BC 0.9800 . ? C1C C2C 1.527(3) . ? C1C H1CA 0.9900 . ? C1C H1CB 0.9900 . ? C2C C3C 1.519(3) . ? C2C H2CA 0.9900 . ? C2C H2CB 0.9900 . ? C3C H3CA 0.9900 . ? C3C H3CB 0.9900 . ? C4C C5C 1.454(3) . ? C4C H4CA 0.9500 . ? C6C C7C 1.364(3) . ? C6C H6CA 0.9500 . ? C7C H7CA 0.9500 . ? C8C H8CA 0.9800 . ? C8C H8CB 0.9800 . ? C8C H8CC 0.9800 . ? 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 N2A Mn N1C 156.27(6) . . ? N2A Mn N2C 88.49(6) . . ? N1C Mn N2C 71.47(6) . . ? N2A Mn N1B 76.63(6) . . ? N1C Mn N1B 118.48(6) . . ? N2C Mn N1B 158.57(6) . . ? N2A Mn N2B 92.92(6) . . ? N1C Mn N2B 76.72(6) . . ? N2C Mn N2B 94.77(6) . . ? N1B Mn N2B 71.06(6) . . ? N2A Mn N1A 70.60(6) . . ? N1C Mn N1A 114.34(6) . . ? N2C Mn N1A 75.11(6) . . ? N1B Mn N1A 113.17(6) . . ? N2B Mn N1A 160.55(6) . . ? N2A Mn N 125.03(6) . . ? N1C Mn N 77.83(6) . . ? N2C Mn N 123.49(6) . . ? N1B Mn N 77.93(6) . . ? N2B Mn N 122.83(6) . . ? N1A Mn N 76.20(6) . . ? O11 Cl1 O14 109.13(11) . . ? O11 Cl1 O13 108.99(12) . . ? O14 Cl1 O13 110.24(10) . . ? O11 Cl1 O12 108.70(13) . . ? O14 Cl1 O12 110.10(11) . . ? O13 Cl1 O12 109.65(11) . . ? O22 Cl2 O24 109.81(12) . . ? O22 Cl2 O21 110.65(13) . . ? O24 Cl2 O21 108.58(13) . . ? O22 Cl2 O23 110.49(13) . . ? O24 Cl2 O23 108.18(12) . . ? O21 Cl2 O23 109.07(12) . . ? C1B N C1C 108.11(15) . . ? C1B N C1A 108.03(15) . . ? C1C N C1A 107.73(15) . . ? C1B N Mn 111.59(12) . . ? C1C N Mn 109.56(12) . . ? C1A N Mn 111.68(12) . . ? C4A N1A C3A 119.32(17) . . ? C4A N1A Mn 117.09(13) . . ? C3A N1A Mn 122.36(12) . . ? C5A N2A C6A 106.01(16) . . ? C5A N2A Mn 114.59(13) . . ? C6A N2A Mn 138.51(14) . . ? C5A N3A C7A 107.20(17) . . ? C5A N3A C8A 127.29(18) . . ? C7A N3A C8A 125.47(17) . . ? C4B N1B C3B 118.90(17) . . ? C4B N1B Mn 118.02(13) . . ? C3B N1B Mn 122.67(13) . . ? C5B N2B C6B 105.31(17) . . ? C5B N2B Mn 112.74(13) . . ? C6B N2B Mn 140.91(14) . . ? C5B N3B C7B 106.60(17) . . ? C5B N3B C8B 127.82(18) . . ? C7B N3B C8B 125.49(18) . . ? C4C N1C C3C 119.24(17) . . ? C4C N1C Mn 117.95(13) . . ? C3C N1C Mn 122.23(13) . . ? C5C N2C C6C 105.98(17) . . ? C5C N2C Mn 112.82(13) . . ? C6C N2C Mn 140.23(13) . . ? C5C N3C C7C 107.28(17) . . ? C5C N3C C8C 127.93(19) . . ? C7C N3C C8C 124.76(18) . . ? N C1A C2A 117.42(16) . . ? N C1A H1AA 107.9 . . ? C2A C1A H1AA 107.9 . . ? N C1A H1AB 107.9 . . ? C2A C1A H1AB 107.9 . . ? H1AA C1A H1AB 107.2 . . ? C1A C2A C3A 115.57(17) . . ? C1A C2A H2AA 108.4 . . ? C3A C2A H2AA 108.4 . . ? C1A C2A H2AB 108.4 . . ? C3A C2A H2AB 108.4 . . ? H2AA C2A H2AB 107.4 . . ? N1A C3A C2A 111.70(17) . . ? N1A C3A H3AA 109.3 . . ? C2A C3A H3AA 109.3 . . ? N1A C3A H3AB 109.3 . . ? C2A C3A H3AB 109.3 . . ? H3AA C3A H3AB 107.9 . . ? N1A C4A C5A 115.94(18) . . ? N1A C4A H4AA 122.0 . . ? C5A C4A H4AA 122.0 . . ? N2A C5A N3A 110.82(17) . . ? N2A C5A C4A 121.11(17) . . ? N3A C5A C4A 128.07(18) . . ? C7A C6A N2A 109.72(18) . . ? C7A C6A H6AA 125.1 . . ? N2A C6A H6AA 125.1 . . ? C6A C7A N3A 106.24(17) . . ? C6A C7A H7AA 126.9 . . ? N3A C7A H7AA 126.9 . . ? N3A C8A H8A1 109.5 . . ? N3A C8A H8A2 109.5 . . ? N3A C8A H8A3 109.5 . . ? N3A C8A H8A4 109.5 . . ? N3A C8A H8A5 109.5 . . ? H8A4 C8A H8A5 109.5 . . ? N3A C8A H8A6 109.5 . . ? H8A4 C8A H8A6 109.5 . . ? H8A5 C8A H8A6 109.5 . . ? N C1B C2B 117.71(16) . . ? N C1B H1BA 107.9 . . ? C2B C1B H1BA 107.9 . . ? N C1B H1BB 107.9 . . ? C2B C1B H1BB 107.9 . . ? H1BA C1B H1BB 107.2 . . ? C3B C2B C1B 114.80(17) . . ? C3B C2B H2BA 108.6 . . ? C1B C2B H2BA 108.6 . . ? C3B C2B H2BB 108.6 . . ? C1B C2B H2BB 108.6 . . ? H2BA C2B H2BB 107.5 . . ? N1B C3B C2B 110.71(16) . . ? N1B C3B H3BA 109.5 . . ? C2B C3B H3BA 109.5 . . ? N1B C3B H3BB 109.5 . . ? C2B C3B H3BB 109.5 . . ? H3BA C3B H3BB 108.1 . . ? N1B C4B C5B 116.53(18) . . ? N1B C4B H4BA 121.7 . . ? C5B C4B H4BA 121.7 . . ? N2B C5B N3B 111.69(17) . . ? N2B C5B C4B 121.22(18) . . ? N3B C5B C4B 127.06(18) . . ? N2B C6B C7B 110.14(18) . . ? N2B C6B H6BA 124.9 . . ? C7B C6B H6BA 124.9 . . ? C6B C7B N3B 106.24(18) . . ? C6B C7B H7BA 126.9 . . ? N3B C7B H7BA 126.9 . . ? N3B C8B H8BA 109.5 . . ? N3B C8B H8BB 109.5 . . ? H8BA C8B H8BB 109.5 . . ? N3B C8B H8BC 109.5 . . ? H8BA C8B H8BC 109.5 . . ? H8BB C8B H8BC 109.5 . . ? N C1C C2C 117.24(16) . . ? N C1C H1CA 108.0 . . ? C2C C1C H1CA 108.0 . . ? N C1C H1CB 108.0 . . ? C2C C1C H1CB 108.0 . . ? H1CA C1C H1CB 107.2 . . ? C3C C2C C1C 115.47(17) . . ? C3C C2C H2CA 108.4 . . ? C1C C2C H2CA 108.4 . . ? C3C C2C H2CB 108.4 . . ? C1C C2C H2CB 108.4 . . ? H2CA C2C H2CB 107.5 . . ? N1C C3C C2C 111.69(16) . . ? N1C C3C H3CA 109.3 . . ? C2C C3C H3CA 109.3 . . ? N1C C3C H3CB 109.3 . . ? C2C C3C H3CB 109.3 . . ? H3CA C3C H3CB 107.9 . . ? N1C C4C C5C 116.08(17) . . ? N1C C4C H4CA 122.0 . . ? C5C C4C H4CA 122.0 . . ? N2C C5C N3C 110.76(18) . . ? N2C C5C C4C 121.13(18) . . ? N3C C5C C4C 128.12(18) . . ? C7C C6C N2C 109.55(18) . . ? C7C C6C H6CA 125.2 . . ? N2C C6C H6CA 125.2 . . ? C6C C7C N3C 106.42(18) . . ? C6C C7C H7CA 126.8 . . ? N3C C7C H7CA 126.8 . . ? N3C C8C H8CA 109.5 . . ? N3C C8C H8CB 109.5 . . ? H8CA C8C H8CB 109.5 . . ? N3C C8C H8CC 109.5 . . ? H8CA C8C H8CC 109.5 . . ? H8CB C8C H8CC 109.5 . . ? 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 N2A Mn N C1B 15.17(15) . . . . ? N1C Mn N C1B -171.83(14) . . . . ? N2C Mn N C1B 130.34(12) . . . . ? N1B Mn N C1B -48.81(13) . . . . ? N2B Mn N C1B -106.60(13) . . . . ? N1A Mn N C1B 69.02(13) . . . . ? N2A Mn N C1C 134.86(12) . . . . ? N1C Mn N C1C -52.14(12) . . . . ? N2C Mn N C1C -109.97(12) . . . . ? N1B Mn N C1C 70.88(12) . . . . ? N2B Mn N C1C 13.09(14) . . . . ? N1A Mn N C1C -171.29(13) . . . . ? N2A Mn N C1A -105.86(12) . . . . ? N1C Mn N C1A 67.15(12) . . . . ? N2C Mn N C1A 9.32(14) . . . . ? N1B Mn N C1A -169.84(13) . . . . ? N2B Mn N C1A 132.38(12) . . . . ? N1A Mn N C1A -52.01(12) . . . . ? N2A Mn N1A C4A -1.26(14) . . . . ? N1C Mn N1A C4A 153.70(14) . . . . ? N2C Mn N1A C4A 92.46(15) . . . . ? N1B Mn N1A C4A -66.59(16) . . . . ? N2B Mn N1A C4A 32.1(3) . . . . ? N Mn N1A C4A -136.75(16) . . . . ? N2A Mn N1A C3A -168.50(16) . . . . ? N1C Mn N1A C3A -13.54(16) . . . . ? N2C Mn N1A C3A -74.78(15) . . . . ? N1B Mn N1A C3A 126.17(14) . . . . ? N2B Mn N1A C3A -135.12(18) . . . . ? N Mn N1A C3A 56.01(15) . . . . ? N1C Mn N2A C5A -110.38(18) . . . . ? N2C Mn N2A C5A -78.57(14) . . . . ? N1B Mn N2A C5A 116.99(15) . . . . ? N2B Mn N2A C5A -173.26(14) . . . . ? N1A Mn N2A C5A -3.83(13) . . . . ? N Mn N2A C5A 52.40(16) . . . . ? N1C Mn N2A C6A 82.4(3) . . . . ? N2C Mn N2A C6A 114.2(2) . . . . ? N1B Mn N2A C6A -50.2(2) . . . . ? N2B Mn N2A C6A 19.5(2) . . . . ? N1A Mn N2A C6A -171.0(2) . . . . ? N Mn N2A C6A -114.8(2) . . . . ? N2A Mn N1B C4B 96.37(15) . . . . ? N1C Mn N1B C4B -63.95(16) . . . . ? N2C Mn N1B C4B 49.2(2) . . . . ? N2B Mn N1B C4B -1.51(14) . . . . ? N1A Mn N1B C4B 158.13(14) . . . . ? N Mn N1B C4B -132.77(15) . . . . ? N2A Mn N1B C3B -76.19(15) . . . . ? N1C Mn N1B C3B 123.49(14) . . . . ? N2C Mn N1B C3B -123.39(18) . . . . ? N2B Mn N1B C3B -174.06(16) . . . . ? N1A Mn N1B C3B -14.42(16) . . . . ? N Mn N1B C3B 54.67(15) . . . . ? N2A Mn N2B C5B -77.40(13) . . . . ? N1C Mn N2B C5B 124.20(14) . . . . ? N2C Mn N2B C5B -166.13(13) . . . . ? N1B Mn N2B C5B -2.60(12) . . . . ? N1A Mn N2B C5B -108.70(19) . . . . ? N Mn N2B C5B 58.41(14) . . . . ? N2A Mn N2B C6B 116.6(2) . . . . ? N1C Mn N2B C6B -41.8(2) . . . . ? N2C Mn N2B C6B 27.9(2) . . . . ? N1B Mn N2B C6B -168.6(2) . . . . ? N1A Mn N2B C6B 85.3(3) . . . . ? N Mn N2B C6B -107.5(2) . . . . ? N2A Mn N1C C4C 32.7(2) . . . . ? N2C Mn N1C C4C -1.09(14) . . . . ? N1B Mn N1C C4C 158.15(14) . . . . ? N2B Mn N1C C4C 98.65(15) . . . . ? N1A Mn N1C C4C -64.40(16) . . . . ? N Mn N1C C4C -132.97(15) . . . . ? N2A Mn N1C C3C -138.58(16) . . . . ? N2C Mn N1C C3C -172.34(16) . . . . ? N1B Mn N1C C3C -13.10(17) . . . . ? N2B Mn N1C C3C -72.60(15) . . . . ? N1A Mn N1C C3C 124.35(14) . . . . ? N Mn N1C C3C 55.78(14) . . . . ? N2A Mn N2C C5C -170.51(14) . . . . ? N1C Mn N2C C5C -3.44(13) . . . . ? N1B Mn N2C C5C -124.94(17) . . . . ? N2B Mn N2C C5C -77.71(14) . . . . ? N1A Mn N2C C5C 119.17(14) . . . . ? N Mn N2C C5C 57.33(15) . . . . ? N2A Mn N2C C6C 23.0(2) . . . . ? N1C Mn N2C C6C -170.0(2) . . . . ? N1B Mn N2C C6C 68.5(3) . . . . ? N2B Mn N2C C6C 115.8(2) . . . . ? N1A Mn N2C C6C -47.4(2) . . . . ? N Mn N2C C6C -109.2(2) . . . . ? C1B N C1A C2A -51.7(2) . . . . ? C1C N C1A C2A -168.28(17) . . . . ? Mn N C1A C2A 71.36(19) . . . . ? N C1A C2A C3A -67.5(2) . . . . ? C4A N1A C3A C2A 126.86(19) . . . . ? Mn N1A C3A C2A -66.17(19) . . . . ? C1A C2A C3A N1A 58.4(2) . . . . ? C3A N1A C4A C5A 173.38(17) . . . . ? Mn N1A C4A C5A 5.7(2) . . . . ? C6A N2A C5A N3A -0.7(2) . . . . ? Mn N2A C5A N3A -171.96(12) . . . . ? C6A N2A C5A C4A 179.80(18) . . . . ? Mn N2A C5A C4A 8.6(2) . . . . ? C7A N3A C5A N2A 0.5(2) . . . . ? C8A N3A C5A N2A 178.3(2) . . . . ? C7A N3A C5A C4A 179.9(2) . . . . ? C8A N3A C5A C4A -2.3(3) . . . . ? N1A C4A C5A N2A -9.9(3) . . . . ? N1A C4A C5A N3A 170.75(19) . . . . ? C5A N2A C6A C7A 0.7(2) . . . . ? Mn N2A C6A C7A 168.65(15) . . . . ? N2A C6A C7A N3A -0.5(2) . . . . ? C5A N3A C7A C6A 0.0(2) . . . . ? C8A N3A C7A C6A -177.8(2) . . . . ? C1C N C1B C2B -52.0(2) . . . . ? C1A N C1B C2B -168.34(17) . . . . ? Mn N C1B C2B 68.52(19) . . . . ? N C1B C2B C3B -69.6(2) . . . . ? C4B N1B C3B C2B 120.0(2) . . . . ? Mn N1B C3B C2B -67.5(2) . . . . ? C1B C2B C3B N1B 61.7(2) . . . . ? C3B N1B C4B C5B 177.97(17) . . . . ? Mn N1B C4B C5B 5.1(2) . . . . ? C6B N2B C5B N3B -1.0(2) . . . . ? Mn N2B C5B N3B -171.89(12) . . . . ? C6B N2B C5B C4B 177.27(18) . . . . ? Mn N2B C5B C4B 6.4(2) . . . . ? C7B N3B C5B N2B 0.7(2) . . . . ? C8B N3B C5B N2B 177.33(18) . . . . ? C7B N3B C5B C4B -177.43(19) . . . . ? C8B N3B C5B C4B -0.8(3) . . . . ? N1B C4B C5B N2B -8.0(3) . . . . ? N1B C4B C5B N3B 169.98(19) . . . . ? C5B N2B C6B C7B 0.9(2) . . . . ? Mn N2B C6B C7B 167.50(16) . . . . ? N2B C6B C7B N3B -0.5(2) . . . . ? C5B N3B C7B C6B -0.1(2) . . . . ? C8B N3B C7B C6B -176.83(19) . . . . ? C1B N C1C C2C -166.59(17) . . . . ? C1A N C1C C2C -50.1(2) . . . . ? Mn N C1C C2C 71.60(18) . . . . ? N C1C C2C C3C -69.3(2) . . . . ? C4C N1C C3C C2C 123.3(2) . . . . ? Mn N1C C3C C2C -65.6(2) . . . . ? C1C C2C C3C N1C 58.5(2) . . . . ? C3C N1C C4C C5C 176.67(17) . . . . ? Mn N1C C4C C5C 5.2(2) . . . . ? C6C N2C C5C N3C -0.9(2) . . . . ? Mn N2C C5C N3C -171.96(12) . . . . ? C6C N2C C5C C4C 178.73(18) . . . . ? Mn N2C C5C C4C 7.6(2) . . . . ? C7C N3C C5C N2C 0.7(2) . . . . ? C8C N3C C5C N2C 178.92(19) . . . . ? C7C N3C C5C C4C -178.82(19) . . . . ? C8C N3C C5C C4C -0.6(3) . . . . ? N1C C4C C5C N2C -8.9(3) . . . . ? N1C C4C C5C N3C 170.62(19) . . . . ? C5C N2C C6C C7C 0.7(2) . . . . ? Mn N2C C6C C7C 167.77(16) . . . . ? N2C C6C C7C N3C -0.2(2) . . . . ? C5C N3C C7C C6C -0.3(2) . . . . ? C8C N3C C7C C6C -178.55(19) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C4B H4BA O13 0.95 2.46 3.403(3) 171.4 . C4A H4AA O23 0.95 2.41 3.343(3) 169.0 . C8A H8A5 O23 0.98 2.55 3.410(3) 145.7 . C7B H7BA O24 0.95 2.53 3.475(3) 177.0 2_665 _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 0.770 _refine_diff_density_min -0.703 _refine_diff_density_rms 0.069 #===END data_llc22m _database_code_depnum_ccdc_archive 'CCDC 277553' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H30 Cl2 Mn N10 O8' _chemical_formula_weight 676.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.511(13) _cell_length_b 9.737(6) _cell_length_c 17.223(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.83(3) _cell_angle_gamma 90.00 _cell_volume 2768(3) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 5066 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 28.39 _exptl_crystal_description plate _exptl_crystal_colour pale _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.623 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1396 _exptl_absorpt_coefficient_mu 0.736 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5419 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20090 _diffrn_reflns_av_R_equivalents 0.1012 _diffrn_reflns_av_sigmaI/netI 0.0705 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 28.40 _reflns_number_total 6613 _reflns_number_gt 5267 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0612P)^2^+3.7700P] 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_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6613 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0785 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1391 _refine_ls_wR_factor_gt 0.1287 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 Mn Mn 0.24855(2) 0.27078(5) 0.25960(2) 0.01239(12) Uani 1 1 d . . . Cl1 Cl -0.07052(4) 0.22758(7) -0.09928(4) 0.01866(15) Uani 1 1 d . . . Cl2 Cl 0.40347(4) 0.75581(7) -0.09388(4) 0.02000(16) Uani 1 1 d . . . O11 O -0.0443(2) 0.2218(3) -0.17830(15) 0.0528(8) Uani 1 1 d . . . O12 O -0.04926(16) 0.3567(3) -0.06507(16) 0.0378(6) Uani 1 1 d . . . O13 O -0.15626(14) 0.2073(3) -0.09713(18) 0.0415(7) Uani 1 1 d . . . O14 O -0.03138(12) 0.1169(2) -0.05629(13) 0.0241(5) Uani 1 1 d . . . O21 O 0.40240(16) 0.7894(3) -0.17451(14) 0.0396(6) Uani 1 1 d . . . O22 O 0.44335(14) 0.8654(3) -0.05117(14) 0.0334(6) Uani 1 1 d . . . O23 O 0.44678(15) 0.6300(3) -0.07946(16) 0.0397(6) Uani 1 1 d . . . O24 O 0.32105(13) 0.7418(3) -0.06641(15) 0.0311(6) Uani 1 1 d . . . N N 0.24923(13) 0.2791(2) 0.40032(14) 0.0165(5) Uani 1 1 d . . . N1A N 0.15460(13) 0.4453(2) 0.27877(14) 0.0171(5) Uani 1 1 d . . . N2A N 0.13892(13) 0.2301(2) 0.17970(14) 0.0170(5) Uani 1 1 d . . . N3A N 0.04898(14) 0.1909(3) 0.08650(14) 0.0204(5) Uani 1 1 d . . . H3AC H 0.0231 0.1486 0.0484 0.024 Uiso 1 1 calc R . . N1B N 0.38448(13) 0.3237(3) 0.28143(14) 0.0167(5) Uani 1 1 d . . . N2B N 0.28732(13) 0.4398(3) 0.17059(13) 0.0178(5) Uani 1 1 d . . . N3B N 0.31889(14) 0.5653(3) 0.06898(14) 0.0193(5) Uani 1 1 d . . . H3BC H 0.3130 0.6143 0.0264 0.023 Uiso 1 1 calc R . . N1C N 0.21437(13) 0.0452(2) 0.28846(14) 0.0169(5) Uani 1 1 d . . . N2C N 0.32424(13) 0.1170(3) 0.17826(14) 0.0171(5) Uani 1 1 d . . . N3C N 0.39128(15) -0.0155(3) 0.09764(15) 0.0252(6) Uani 1 1 d . . . H3CC H 0.4249 -0.0402 0.0610 0.030 Uiso 1 1 calc R . . C1A C 0.25262(16) 0.4236(3) 0.43002(17) 0.0194(6) Uani 1 1 d . . . H1AA H 0.3004 0.4687 0.4071 0.023 Uiso 1 1 calc R . . H1AB H 0.2621 0.4197 0.4869 0.023 Uiso 1 1 calc R . . C2A C 0.17895(16) 0.5157(3) 0.41464(16) 0.0186(6) Uani 1 1 d . . . H2AA H 0.1296 0.4656 0.4301 0.022 Uiso 1 1 calc R . . H2AB H 0.1837 0.5983 0.4480 0.022 Uiso 1 1 calc R . . C3A C 0.16864(17) 0.5616(3) 0.33078(17) 0.0206(6) Uani 1 1 d . . . H3AA H 0.1223 0.6259 0.3266 0.025 Uiso 1 1 calc R . . H3AB H 0.2179 0.6113 0.3146 0.025 Uiso 1 1 calc R . . C4A C 0.09522(16) 0.4507(3) 0.23067(16) 0.0185(6) Uani 1 1 d . . . H4AA H 0.0587 0.5261 0.2308 0.022 Uiso 1 1 calc R . . C5A C 0.08499(15) 0.3389(3) 0.17577(16) 0.0180(6) Uani 1 1 d . . . C6A C 0.02961(16) 0.3158(3) 0.11676(16) 0.0197(6) Uani 1 1 d . . . H6AA H -0.0133 0.3747 0.1005 0.024 Uiso 1 1 calc R . . C7A C 0.11535(16) 0.1434(3) 0.12548(16) 0.0185(6) Uani 1 1 d . . . H7AA H 0.1413 0.0586 0.1149 0.022 Uiso 1 1 calc R . . C1B C 0.32071(16) 0.2036(3) 0.43407(16) 0.0187(6) Uani 1 1 d . . . H1BA H 0.3197 0.1088 0.4133 0.022 Uiso 1 1 calc R . . H1BB H 0.3134 0.1971 0.4909 0.022 Uiso 1 1 calc R . . C2B C 0.40529(16) 0.2638(3) 0.41961(17) 0.0201(6) Uani 1 1 d . . . H2BA H 0.4044 0.3630 0.4323 0.024 Uiso 1 1 calc R . . H2BB H 0.4446 0.2191 0.4555 0.024 Uiso 1 1 calc R . . C3B C 0.43467(15) 0.2468(3) 0.33731(17) 0.0185(6) Uani 1 1 d . . . H3BA H 0.4914 0.2792 0.3344 0.022 Uiso 1 1 calc R . . H3BB H 0.4338 0.1482 0.3234 0.022 Uiso 1 1 calc R . . C4B C 0.41978(15) 0.3954(3) 0.23015(16) 0.0188(6) Uani 1 1 d . . . H4BA H 0.4769 0.4073 0.2317 0.023 Uiso 1 1 calc R . . C5B C 0.37074(16) 0.4588(3) 0.16912(16) 0.0174(5) Uani 1 1 d . . . C6B C 0.39083(17) 0.5350(3) 0.10556(17) 0.0192(6) Uani 1 1 d . . . H6BA H 0.4436 0.5613 0.0900 0.023 Uiso 1 1 calc R . . C7B C 0.25829(16) 0.5069(3) 0.10971(16) 0.0180(5) Uani 1 1 d . . . H7BA H 0.2024 0.5133 0.0962 0.022 Uiso 1 1 calc R . . C1C C 0.17474(16) 0.2136(3) 0.43291(17) 0.0207(6) Uani 1 1 d . . . H1CA H 0.1270 0.2597 0.4093 0.025 Uiso 1 1 calc R . . H1CB H 0.1741 0.2332 0.4893 0.025 Uiso 1 1 calc R . . C2C C 0.16383(17) 0.0593(3) 0.42220(17) 0.0210(6) Uani 1 1 d . . . H2CA H 0.2135 0.0126 0.4412 0.025 Uiso 1 1 calc R . . H2CB H 0.1186 0.0286 0.4551 0.025 Uiso 1 1 calc R . . C3C C 0.14681(16) 0.0136(3) 0.33957(16) 0.0194(6) Uani 1 1 d . . . H3CA H 0.1367 -0.0866 0.3389 0.023 Uiso 1 1 calc R . . H3CB H 0.0973 0.0601 0.3198 0.023 Uiso 1 1 calc R . . C4C C 0.24262(16) -0.0516(3) 0.24672(16) 0.0199(6) Uani 1 1 d . . . H4CA H 0.2244 -0.1433 0.2532 0.024 Uiso 1 1 calc R . . C5C C 0.30276(16) -0.0192(3) 0.18941(17) 0.0187(6) Uani 1 1 d . . . C6C C 0.34339(18) -0.1011(3) 0.13914(19) 0.0264(7) Uani 1 1 d . . . H6CA H 0.3392 -0.1980 0.1341 0.032 Uiso 1 1 calc R . . C7C C 0.37812(16) 0.1150(3) 0.12263(17) 0.0208(6) Uani 1 1 d . . . H7CA H 0.4043 0.1941 0.1026 0.025 Uiso 1 1 calc R . . 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 0.01355(18) 0.0092(2) 0.0144(2) -0.00023(15) 0.00172(14) -0.00016(13) Cl1 0.0224(3) 0.0147(3) 0.0189(3) 0.0018(3) -0.0011(2) 0.0001(2) Cl2 0.0236(3) 0.0199(4) 0.0166(3) 0.0025(3) 0.0046(2) 0.0029(3) O11 0.090(2) 0.0445(17) 0.0241(13) 0.0078(12) 0.0208(14) 0.0193(16) O12 0.0498(14) 0.0152(12) 0.0480(15) -0.0036(11) -0.0138(12) -0.0010(10) O13 0.0226(11) 0.0357(15) 0.0659(19) 0.0078(14) -0.0083(11) -0.0001(10) O14 0.0295(10) 0.0148(11) 0.0276(11) 0.0007(9) -0.0087(9) 0.0012(8) O21 0.0524(15) 0.0479(17) 0.0184(12) 0.0060(11) 0.0046(10) -0.0033(13) O22 0.0319(11) 0.0359(15) 0.0328(13) -0.0108(11) 0.0059(10) -0.0016(10) O23 0.0392(13) 0.0263(14) 0.0538(17) 0.0070(12) 0.0113(11) 0.0147(11) O24 0.0208(10) 0.0334(14) 0.0393(14) 0.0162(11) 0.0068(9) 0.0049(9) N 0.0160(10) 0.0134(11) 0.0201(12) -0.0004(9) 0.0020(8) -0.0010(8) N1A 0.0186(10) 0.0146(12) 0.0181(11) 0.0006(9) 0.0035(8) -0.0016(9) N2A 0.0174(10) 0.0146(11) 0.0191(11) 0.0007(9) 0.0018(8) 0.0004(9) N3A 0.0200(11) 0.0237(13) 0.0174(12) -0.0023(10) -0.0006(9) -0.0017(10) N1B 0.0169(10) 0.0149(12) 0.0184(11) -0.0018(9) 0.0012(8) 0.0009(9) N2B 0.0191(10) 0.0190(12) 0.0152(11) -0.0016(9) 0.0028(8) 0.0017(9) N3B 0.0272(12) 0.0138(12) 0.0168(11) -0.0014(9) 0.0023(9) -0.0015(10) N1C 0.0188(10) 0.0145(12) 0.0175(11) 0.0007(9) -0.0001(9) -0.0008(9) N2C 0.0185(10) 0.0145(12) 0.0185(11) -0.0003(9) 0.0022(9) 0.0006(9) N3C 0.0254(12) 0.0255(14) 0.0249(13) -0.0035(11) 0.0094(10) 0.0061(11) C1A 0.0197(12) 0.0189(15) 0.0197(14) -0.0044(11) 0.0011(10) -0.0010(11) C2A 0.0200(12) 0.0154(14) 0.0203(14) -0.0077(11) 0.0014(10) 0.0015(10) C3A 0.0233(13) 0.0150(14) 0.0237(15) -0.0043(12) 0.0013(11) 0.0016(11) C4A 0.0190(12) 0.0163(14) 0.0204(14) -0.0005(11) 0.0052(10) 0.0029(10) C5A 0.0174(12) 0.0182(15) 0.0186(13) 0.0019(11) 0.0038(10) 0.0010(10) C6A 0.0170(12) 0.0232(15) 0.0189(13) 0.0014(12) 0.0020(10) 0.0025(11) C7A 0.0184(12) 0.0177(14) 0.0194(14) -0.0003(11) 0.0019(10) -0.0010(10) C1B 0.0216(12) 0.0198(15) 0.0149(13) 0.0012(11) 0.0005(10) 0.0016(11) C2B 0.0184(12) 0.0215(15) 0.0203(14) 0.0008(12) -0.0017(10) 0.0002(11) C3B 0.0168(11) 0.0173(14) 0.0213(14) 0.0012(11) -0.0011(10) 0.0009(10) C4B 0.0157(11) 0.0215(15) 0.0193(13) -0.0010(12) 0.0023(10) -0.0020(10) C5B 0.0185(12) 0.0154(14) 0.0183(13) -0.0015(11) 0.0032(10) -0.0001(10) C6B 0.0212(12) 0.0146(14) 0.0221(14) -0.0018(11) 0.0053(11) -0.0029(11) C7B 0.0192(12) 0.0144(13) 0.0203(14) -0.0023(11) 0.0029(10) -0.0004(10) C1C 0.0198(12) 0.0231(16) 0.0193(14) -0.0018(12) 0.0062(10) -0.0048(11) C2C 0.0220(13) 0.0223(16) 0.0187(14) 0.0014(12) 0.0056(10) -0.0056(11) C3C 0.0209(12) 0.0178(14) 0.0197(14) -0.0007(11) 0.0049(10) -0.0061(11) C4C 0.0225(13) 0.0134(15) 0.0239(15) 0.0002(11) 0.0008(11) 0.0007(10) C5C 0.0178(12) 0.0151(14) 0.0232(14) -0.0005(11) 0.0008(10) 0.0022(10) C6C 0.0283(14) 0.0194(15) 0.0317(17) -0.0047(13) 0.0051(12) 0.0024(12) C7C 0.0212(12) 0.0212(15) 0.0200(14) 0.0005(12) 0.0026(10) 0.0014(11) _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 Mn N2A 2.292(3) . ? Mn N1C 2.324(3) . ? Mn N1A 2.327(3) . ? Mn N1B 2.328(3) . ? Mn N2B 2.344(3) . ? Mn N2C 2.412(3) . ? Mn N 2.425(3) . ? Cl1 O12 1.430(3) . ? Cl1 O13 1.430(3) . ? Cl1 O11 1.435(3) . ? Cl1 O14 1.454(2) . ? Cl2 O21 1.427(3) . ? Cl2 O23 1.438(3) . ? Cl2 O22 1.449(3) . ? Cl2 O24 1.454(2) . ? N C1A 1.497(4) . ? N C1B 1.501(3) . ? N C1C 1.502(4) . ? N1A C4A 1.275(4) . ? N1A C3A 1.461(4) . ? N2A C7A 1.314(4) . ? N2A C5A 1.385(4) . ? N3A C7A 1.358(4) . ? N3A C6A 1.363(4) . ? N3A H3AC 0.8800 . ? N1B C4B 1.274(4) . ? N1B C3B 1.466(3) . ? N2B C7B 1.319(4) . ? N2B C5B 1.390(4) . ? N3B C7B 1.355(4) . ? N3B C6B 1.369(4) . ? N3B H3BC 0.8800 . ? N1C C4C 1.277(4) . ? N1C C3C 1.463(4) . ? N2C C7C 1.317(4) . ? N2C C5C 1.388(4) . ? N3C C6C 1.359(4) . ? N3C C7C 1.361(4) . ? N3C H3CC 0.8800 . ? C1A C2A 1.532(4) . ? C1A H1AA 0.9900 . ? C1A H1AB 0.9900 . ? C2A C3A 1.519(4) . ? C2A H2AA 0.9900 . ? C2A H2AB 0.9900 . ? C3A H3AA 0.9900 . ? C3A H3AB 0.9900 . ? C4A C5A 1.450(4) . ? C4A H4AA 0.9500 . ? C5A C6A 1.376(4) . ? C6A H6AA 0.9500 . ? C7A H7AA 0.9500 . ? C1B C2B 1.538(4) . ? C1B H1BA 0.9900 . ? C1B H1BB 0.9900 . ? C2B C3B 1.514(4) . ? C2B H2BA 0.9900 . ? C2B H2BB 0.9900 . ? C3B H3BA 0.9900 . ? C3B H3BB 0.9900 . ? C4B C5B 1.455(4) . ? C4B H4BA 0.9500 . ? C5B C6B 1.367(4) . ? C6B H6BA 0.9500 . ? C7B H7BA 0.9500 . ? C1C C2C 1.523(4) . ? C1C H1CA 0.9900 . ? C1C H1CB 0.9900 . ? C2C C3C 1.514(4) . ? C2C H2CA 0.9900 . ? C2C H2CB 0.9900 . ? C3C H3CA 0.9900 . ? C3C H3CB 0.9900 . ? C4C C5C 1.445(4) . ? C4C H4CA 0.9500 . ? C5C C6C 1.361(4) . ? C6C H6CA 0.9500 . ? C7C H7CA 0.9500 . ? 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 N2A Mn N1C 76.89(8) . . ? N2A Mn N1A 71.89(9) . . ? N1C Mn N1A 119.70(9) . . ? N2A Mn N1B 152.40(9) . . ? N1C Mn N1B 114.28(8) . . ? N1A Mn N1B 117.29(9) . . ? N2A Mn N2B 87.10(9) . . ? N1C Mn N2B 150.80(9) . . ? N1A Mn N2B 76.65(9) . . ? N1B Mn N2B 71.25(8) . . ? N2A Mn N2C 87.44(9) . . ? N1C Mn N2C 70.54(9) . . ? N1A Mn N2C 152.57(8) . . ? N1B Mn N2C 74.03(9) . . ? N2B Mn N2C 84.68(9) . . ? N2A Mn N 126.73(9) . . ? N1C Mn N 79.37(8) . . ? N1A Mn N 80.05(8) . . ? N1B Mn N 80.83(8) . . ? N2B Mn N 129.25(9) . . ? N2C Mn N 127.33(8) . . ? O12 Cl1 O13 110.35(16) . . ? O12 Cl1 O11 110.46(18) . . ? O13 Cl1 O11 109.4(2) . . ? O12 Cl1 O14 109.73(15) . . ? O13 Cl1 O14 108.49(15) . . ? O11 Cl1 O14 108.39(16) . . ? O21 Cl2 O23 111.26(17) . . ? O21 Cl2 O22 108.93(16) . . ? O23 Cl2 O22 108.56(17) . . ? O21 Cl2 O24 109.87(15) . . ? O23 Cl2 O24 109.23(15) . . ? O22 Cl2 O24 108.95(15) . . ? C1A N C1B 107.6(2) . . ? C1A N C1C 107.4(2) . . ? C1B N C1C 106.9(2) . . ? C1A N Mn 111.87(17) . . ? C1B N Mn 111.28(16) . . ? C1C N Mn 111.55(17) . . ? C4A N1A C3A 118.7(2) . . ? C4A N1A Mn 116.5(2) . . ? C3A N1A Mn 123.57(17) . . ? C7A N2A C5A 105.8(2) . . ? C7A N2A Mn 139.55(19) . . ? C5A N2A Mn 113.51(18) . . ? C7A N3A C6A 107.9(2) . . ? C7A N3A H3AC 126.1 . . ? C6A N3A H3AC 126.1 . . ? C4B N1B C3B 118.4(2) . . ? C4B N1B Mn 117.33(18) . . ? C3B N1B Mn 121.83(17) . . ? C7B N2B C5B 105.6(2) . . ? C7B N2B Mn 140.13(19) . . ? C5B N2B Mn 112.65(18) . . ? C7B N3B C6B 108.3(2) . . ? C7B N3B H3BC 125.9 . . ? C6B N3B H3BC 125.9 . . ? C4C N1C C3C 118.1(3) . . ? C4C N1C Mn 119.0(2) . . ? C3C N1C Mn 121.10(18) . . ? C7C N2C C5C 105.3(2) . . ? C7C N2C Mn 142.5(2) . . ? C5C N2C Mn 112.19(18) . . ? C6C N3C C7C 108.1(2) . . ? C6C N3C H3CC 126.0 . . ? C7C N3C H3CC 126.0 . . ? N C1A C2A 117.7(2) . . ? N C1A H1AA 107.9 . . ? C2A C1A H1AA 107.9 . . ? N C1A H1AB 107.9 . . ? C2A C1A H1AB 107.9 . . ? H1AA C1A H1AB 107.2 . . ? C3A C2A C1A 114.5(2) . . ? C3A C2A H2AA 108.6 . . ? C1A C2A H2AA 108.6 . . ? C3A C2A H2AB 108.6 . . ? C1A C2A H2AB 108.6 . . ? H2AA C2A H2AB 107.6 . . ? N1A C3A C2A 111.7(2) . . ? N1A C3A H3AA 109.3 . . ? C2A C3A H3AA 109.3 . . ? N1A C3A H3AB 109.3 . . ? C2A C3A H3AB 109.3 . . ? H3AA C3A H3AB 107.9 . . ? N1A C4A C5A 118.3(3) . . ? N1A C4A H4AA 120.9 . . ? C5A C4A H4AA 120.9 . . ? C6A C5A N2A 109.3(3) . . ? C6A C5A C4A 132.4(3) . . ? N2A C5A C4A 118.3(2) . . ? N3A C6A C5A 105.7(2) . . ? N3A C6A H6AA 127.1 . . ? C5A C6A H6AA 127.1 . . ? N2A C7A N3A 111.2(3) . . ? N2A C7A H7AA 124.4 . . ? N3A C7A H7AA 124.4 . . ? N C1B C2B 117.5(2) . . ? N C1B H1BA 107.9 . . ? C2B C1B H1BA 107.9 . . ? N C1B H1BB 107.9 . . ? C2B C1B H1BB 107.9 . . ? H1BA C1B H1BB 107.2 . . ? C3B C2B C1B 114.4(2) . . ? C3B C2B H2BA 108.6 . . ? C1B C2B H2BA 108.6 . . ? C3B C2B H2BB 108.6 . . ? C1B C2B H2BB 108.6 . . ? H2BA C2B H2BB 107.6 . . ? N1B C3B C2B 111.9(2) . . ? N1B C3B H3BA 109.2 . . ? C2B C3B H3BA 109.2 . . ? N1B C3B H3BB 109.2 . . ? C2B C3B H3BB 109.2 . . ? H3BA C3B H3BB 107.9 . . ? N1B C4B C5B 118.6(2) . . ? N1B C4B H4BA 120.7 . . ? C5B C4B H4BA 120.7 . . ? C6B C5B N2B 109.8(2) . . ? C6B C5B C4B 132.0(3) . . ? N2B C5B C4B 118.2(2) . . ? C5B C6B N3B 105.5(2) . . ? C5B C6B H6BA 127.3 . . ? N3B C6B H6BA 127.3 . . ? N2B C7B N3B 110.9(2) . . ? N2B C7B H7BA 124.6 . . ? N3B C7B H7BA 124.6 . . ? N C1C C2C 118.0(2) . . ? N C1C H1CA 107.8 . . ? C2C C1C H1CA 107.8 . . ? N C1C H1CB 107.8 . . ? C2C C1C H1CB 107.8 . . ? H1CA C1C H1CB 107.1 . . ? C3C C2C C1C 115.1(3) . . ? C3C C2C H2CA 108.5 . . ? C1C C2C H2CA 108.5 . . ? C3C C2C H2CB 108.5 . . ? C1C C2C H2CB 108.5 . . ? H2CA C2C H2CB 107.5 . . ? N1C C3C C2C 111.8(2) . . ? N1C C3C H3CA 109.3 . . ? C2C C3C H3CA 109.3 . . ? N1C C3C H3CB 109.3 . . ? C2C C3C H3CB 109.3 . . ? H3CA C3C H3CB 107.9 . . ? N1C C4C C5C 119.0(3) . . ? N1C C4C H4CA 120.5 . . ? C5C C4C H4CA 120.5 . . ? C6C C5C N2C 110.1(3) . . ? C6C C5C C4C 131.1(3) . . ? N2C C5C C4C 118.8(3) . . ? N3C C6C C5C 105.7(3) . . ? N3C C6C H6CA 127.1 . . ? C5C C6C H6CA 127.1 . . ? N2C C7C N3C 110.9(3) . . ? N2C C7C H7CA 124.6 . . ? N3C C7C H7CA 124.6 . . ? 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 N2A Mn N C1A -103.20(17) . . . . ? N1C Mn N C1A -167.85(17) . . . . ? N1A Mn N C1A -44.85(17) . . . . ? N1B Mn N C1A 75.14(17) . . . . ? N2B Mn N C1A 18.7(2) . . . . ? N2C Mn N C1A 136.86(16) . . . . ? N2A Mn N C1B 136.37(17) . . . . ? N1C Mn N C1B 71.72(18) . . . . ? N1A Mn N C1B -165.28(18) . . . . ? N1B Mn N C1B -45.29(17) . . . . ? N2B Mn N C1B -101.76(19) . . . . ? N2C Mn N C1B 16.4(2) . . . . ? N2A Mn N C1C 17.1(2) . . . . ? N1C Mn N C1C -47.56(18) . . . . ? N1A Mn N C1C 75.44(19) . . . . ? N1B Mn N C1C -164.57(19) . . . . ? N2B Mn N C1C 138.96(17) . . . . ? N2C Mn N C1C -102.85(19) . . . . ? N2A Mn N1A C4A -10.3(2) . . . . ? N1C Mn N1A C4A -72.8(2) . . . . ? N1B Mn N1A C4A 141.4(2) . . . . ? N2B Mn N1A C4A 81.0(2) . . . . ? N2C Mn N1A C4A 32.6(3) . . . . ? N Mn N1A C4A -144.4(2) . . . . ? N2A Mn N1A C3A -177.2(2) . . . . ? N1C Mn N1A C3A 120.3(2) . . . . ? N1B Mn N1A C3A -25.5(2) . . . . ? N2B Mn N1A C3A -85.9(2) . . . . ? N2C Mn N1A C3A -134.3(2) . . . . ? N Mn N1A C3A 48.7(2) . . . . ? N1C Mn N2A C7A -56.0(3) . . . . ? N1A Mn N2A C7A 176.3(3) . . . . ? N1B Mn N2A C7A 61.7(4) . . . . ? N2B Mn N2A C7A 99.4(3) . . . . ? N2C Mn N2A C7A 14.6(3) . . . . ? N Mn N2A C7A -121.8(3) . . . . ? N1C Mn N2A C5A 138.2(2) . . . . ? N1A Mn N2A C5A 10.55(18) . . . . ? N1B Mn N2A C5A -104.0(2) . . . . ? N2B Mn N2A C5A -66.36(19) . . . . ? N2C Mn N2A C5A -151.15(19) . . . . ? N Mn N2A C5A 72.5(2) . . . . ? N2A Mn N1B C4B 28.0(3) . . . . ? N1C Mn N1B C4B 137.1(2) . . . . ? N1A Mn N1B C4B -75.3(2) . . . . ? N2B Mn N1B C4B -12.1(2) . . . . ? N2C Mn N1B C4B 77.7(2) . . . . ? N Mn N1B C4B -149.1(2) . . . . ? N2A Mn N1B C3B -133.8(2) . . . . ? N1C Mn N1B C3B -24.8(2) . . . . ? N1A Mn N1B C3B 122.8(2) . . . . ? N2B Mn N1B C3B -173.9(2) . . . . ? N2C Mn N1B C3B -84.2(2) . . . . ? N Mn N1B C3B 49.1(2) . . . . ? N2A Mn N2B C7B 11.5(3) . . . . ? N1C Mn N2B C7B 67.7(4) . . . . ? N1A Mn N2B C7B -60.5(3) . . . . ? N1B Mn N2B C7B 174.1(3) . . . . ? N2C Mn N2B C7B 99.2(3) . . . . ? N Mn N2B C7B -125.5(3) . . . . ? N2A Mn N2B C5B -150.91(19) . . . . ? N1C Mn N2B C5B -94.7(2) . . . . ? N1A Mn N2B C5B 137.0(2) . . . . ? N1B Mn N2B C5B 11.70(18) . . . . ? N2C Mn N2B C5B -63.21(19) . . . . ? N Mn N2B C5B 72.1(2) . . . . ? N2A Mn N1C C4C 85.7(2) . . . . ? N1A Mn N1C C4C 145.69(19) . . . . ? N1B Mn N1C C4C -67.6(2) . . . . ? N2B Mn N1C C4C 27.3(3) . . . . ? N2C Mn N1C C4C -6.22(19) . . . . ? N Mn N1C C4C -142.3(2) . . . . ? N2A Mn N1C C3C -78.9(2) . . . . ? N1A Mn N1C C3C -19.0(2) . . . . ? N1B Mn N1C C3C 127.79(19) . . . . ? N2B Mn N1C C3C -137.4(2) . . . . ? N2C Mn N1C C3C -170.9(2) . . . . ? N Mn N1C C3C 53.02(19) . . . . ? N2A Mn N2C C7C 102.5(3) . . . . ? N1C Mn N2C C7C 179.5(3) . . . . ? N1A Mn N2C C7C 62.1(4) . . . . ? N1B Mn N2C C7C -56.8(3) . . . . ? N2B Mn N2C C7C 15.2(3) . . . . ? N Mn N2C C7C -121.5(3) . . . . ? N2A Mn N2C C5C -73.27(19) . . . . ? N1C Mn N2C C5C 3.72(18) . . . . ? N1A Mn N2C C5C -113.7(2) . . . . ? N1B Mn N2C C5C 127.4(2) . . . . ? N2B Mn N2C C5C -160.59(19) . . . . ? N Mn N2C C5C 62.7(2) . . . . ? C1B N C1A C2A -170.3(2) . . . . ? C1C N C1A C2A -55.5(3) . . . . ? Mn N C1A C2A 67.2(3) . . . . ? N C1A C2A C3A -72.3(3) . . . . ? C4A N1A C3A C2A 130.3(3) . . . . ? Mn N1A C3A C2A -63.1(3) . . . . ? C1A C2A C3A N1A 63.1(3) . . . . ? C3A N1A C4A C5A 175.9(2) . . . . ? Mn N1A C4A C5A 8.4(3) . . . . ? C7A N2A C5A C6A -1.1(3) . . . . ? Mn N2A C5A C6A 169.31(18) . . . . ? C7A N2A C5A C4A 178.8(2) . . . . ? Mn N2A C5A C4A -10.8(3) . . . . ? N1A C4A C5A C6A -178.4(3) . . . . ? N1A C4A C5A N2A 1.7(4) . . . . ? C7A N3A C6A C5A -1.5(3) . . . . ? N2A C5A C6A N3A 1.6(3) . . . . ? C4A C5A C6A N3A -178.3(3) . . . . ? C5A N2A C7A N3A 0.2(3) . . . . ? Mn N2A C7A N3A -166.2(2) . . . . ? C6A N3A C7A N2A 0.8(3) . . . . ? C1A N C1B C2B -56.1(3) . . . . ? C1C N C1B C2B -171.1(2) . . . . ? Mn N C1B C2B 66.8(3) . . . . ? N C1B C2B C3B -72.8(3) . . . . ? C4B N1B C3B C2B 134.1(3) . . . . ? Mn N1B C3B C2B -64.3(3) . . . . ? C1B C2B C3B N1B 64.8(3) . . . . ? C3B N1B C4B C5B 172.9(2) . . . . ? Mn N1B C4B C5B 10.4(3) . . . . ? C7B N2B C5B C6B -1.5(3) . . . . ? Mn N2B C5B C6B 166.89(19) . . . . ? C7B N2B C5B C4B -179.9(3) . . . . ? Mn N2B C5B C4B -11.5(3) . . . . ? N1B C4B C5B C6B -176.9(3) . . . . ? N1B C4B C5B N2B 1.1(4) . . . . ? N2B C5B C6B N3B 1.4(3) . . . . ? C4B C5B C6B N3B 179.5(3) . . . . ? C7B N3B C6B C5B -0.7(3) . . . . ? C5B N2B C7B N3B 1.1(3) . . . . ? Mn N2B C7B N3B -162.1(2) . . . . ? C6B N3B C7B N2B -0.3(3) . . . . ? C1A N C1C C2C -170.5(2) . . . . ? C1B N C1C C2C -55.2(3) . . . . ? Mn N C1C C2C 66.6(3) . . . . ? N C1C C2C C3C -69.2(3) . . . . ? C4C N1C C3C C2C 128.2(3) . . . . ? Mn N1C C3C C2C -67.0(3) . . . . ? C1C C2C C3C N1C 63.1(3) . . . . ? C3C N1C C4C C5C 172.9(2) . . . . ? Mn N1C C4C C5C 7.8(3) . . . . ? C7C N2C C5C C6C -1.0(3) . . . . ? Mn N2C C5C C6C 176.37(19) . . . . ? C7C N2C C5C C4C -178.9(2) . . . . ? Mn N2C C5C C4C -1.6(3) . . . . ? N1C C4C C5C C6C 178.6(3) . . . . ? N1C C4C C5C N2C -3.9(4) . . . . ? C7C N3C C6C C5C -0.7(3) . . . . ? N2C C5C C6C N3C 1.1(3) . . . . ? C4C C5C C6C N3C 178.7(3) . . . . ? C5C N2C C7C N3C 0.5(3) . . . . ? Mn N2C C7C N3C -175.5(2) . . . . ? C6C N3C C7C N2C 0.1(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3A H3AC O14 0.88 2.03 2.869(4) 159.8 . N3A H3AC O14 0.88 2.59 3.055(4) 113.8 3 N3B H3BC O24 0.88 2.03 2.897(4) 168.9 . N3C H3CC O22 0.88 2.16 2.952(4) 148.7 1_545 _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 28.40 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 1.494 _refine_diff_density_min -0.652 _refine_diff_density_rms 0.123 #===END