Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2006 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 ; Syntesis and characterization of manganese(II) and iron(III) d5 tripodal imidazole complexes. Effect of oxidation state, protonation state and ligand conformation on coordination number and spin state ; _publ_section_references ; Bruker (1999). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Flack, H.D. (1983), Acta Cryst. A39, 876-881. Spek, A. L. (1990). Acta Cryst., A46, C-34. Sheldrick, G. M. (1990). Acta Cryst. A46, 467-473. Sheldrick, G. M. (1997). SHELXL-97. University of Gottingen, Germany. ; loop_ _publ_author_name 'Greg Brewer' 'Cynthia Brewer' 'R. Butcher' 'Everett E. Carpenter' 'Luciann Cuenca' 'Bruce C. Noll' ; W.Scheidt ; 'Carol Viragh' 'Peter Y. Zavalij' 'Daniel Zielaski' # Attachment 'daltond5rev.cif' data_1139ff _database_code_depnum_ccdc_archive 'CCDC 267248' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety (C21H30MnN10)(ClO4)2 _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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 11.3654(3) _cell_length_b 20.6178(6) _cell_length_c 12.9278(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.901(1) _cell_angle_gamma 90.00 _cell_volume 2952.90(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8951 _cell_measurement_theta_min 2.375 _cell_measurement_theta_max 27.465 _exptl_crystal_description Hexagon _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1396 _exptl_absorpt_coefficient_mu 0.690 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7304 _exptl_absorpt_correction_T_max 0.9261 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _diffrn_ambient_temperature 173(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_% 0 _diffrn_reflns_number 47247 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0155 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6775 _reflns_number_gt 5599 _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^)+(0.0200P)^2^+2.9610P] 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_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6775 _refine_ls_number_parameters 412 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0457 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0785 _refine_ls_wR_factor_gt 0.0742 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.001 _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 Mn1 Mn 0.29745(2) 0.109732(13) 0.84070(2) 0.02926(7) Uani 1 1 d . . . C1 C 0.28061(18) 0.24165(10) 1.02481(15) 0.0380(4) Uani 1 1 d . . . H1A H 0.2764 0.2804 0.9789 0.039(6) Uiso 1 1 calc R . . H1B H 0.2884 0.2566 1.0988 0.042(6) Uiso 1 1 calc R . . N1 N 0.38617(14) 0.20301(7) 1.01766(11) 0.0316(3) Uani 1 1 d . . . C2 C 0.16520(17) 0.20224(10) 0.99053(15) 0.0380(4) Uani 1 1 d . . . H2A H 0.1653 0.1659 1.0406 0.041(6) Uiso 1 1 calc R . . H2B H 0.0943 0.2300 0.9913 0.034(5) Uiso 1 1 calc R . . N2 N 0.15759(13) 0.17688(7) 0.88333(11) 0.0321(3) Uani 1 1 d . . . C3 C 0.07292(16) 0.19599(9) 0.80740(14) 0.0338(4) Uani 1 1 d . . . H3 H 0.0138 0.2259 0.8196 0.041(6) Uiso 1 1 calc R . . N3 N 0.16043(14) 0.12944(8) 0.68890(11) 0.0325(3) Uani 1 1 d . . . C4 C 0.06920(16) 0.17100(9) 0.70216(14) 0.0322(4) Uani 1 1 d . . . N4 N 0.03167(15) 0.14267(8) 0.53637(12) 0.0381(4) Uani 1 1 d . . . H4 H -0.0020 0.1384 0.4685 0.060(7) Uiso 1 1 calc R . . C5 C -0.01150(17) 0.17997(9) 0.60724(15) 0.0352(4) Uani 1 1 d . . . C6 C 0.13491(18) 0.11336(9) 0.58818(14) 0.0361(4) Uani 1 1 d . . . H6 H 0.1822 0.0851 0.5560 0.038(5) Uiso 1 1 calc R . . C7 C -0.12135(19) 0.22099(12) 0.57687(18) 0.0506(5) Uani 1 1 d . . . H7A H -0.1063 0.2563 0.5308 0.099(11) Uiso 1 1 calc R . . H7B H -0.1413 0.2392 0.6409 0.099(11) Uiso 1 1 calc R . . H7C H -0.1889 0.1945 0.5389 0.092(10) Uiso 1 1 calc R . . C11 C 0.43090(17) 0.16157(9) 1.10987(14) 0.0352(4) Uani 1 1 d . . . H11A H 0.3649 0.1528 1.1466 0.036(5) Uiso 1 1 calc R . . H11B H 0.4965 0.1842 1.1602 0.032(5) Uiso 1 1 calc R . . C12 C 0.47805(17) 0.09779(9) 1.07595(14) 0.0351(4) Uani 1 1 d . . . H12A H 0.5472 0.1060 1.0428 0.035(5) Uiso 1 1 calc R . . H12B H 0.5059 0.0695 1.1385 0.042(6) Uiso 1 1 calc R . . N12 N 0.38040(13) 0.06609(7) 0.99995(11) 0.0309(3) Uani 1 1 d . . . C13 C 0.32736(17) 0.01769(9) 1.02989(14) 0.0325(4) Uani 1 1 d . . . H13 H 0.3555 -0.0004 1.0985 0.041(6) Uiso 1 1 calc R . . N13 N 0.18887(14) 0.01806(8) 0.85719(12) 0.0353(3) Uani 1 1 d . . . C14 C 0.22348(17) -0.00919(9) 0.95747(14) 0.0339(4) Uani 1 1 d . . . N14 N 0.06395(18) -0.05993(10) 0.87470(16) 0.0554(5) Uani 1 1 d . . . H14 H 0.0024 -0.0868 0.8584 0.079(9) Uiso 1 1 calc R . . C15 C 0.1458(2) -0.05745(11) 0.96966(17) 0.0477(5) Uani 1 1 d . . . C16 C 0.0933(2) -0.01432(11) 0.80998(17) 0.0467(5) Uani 1 1 d . . . H16 H 0.0500 -0.0068 0.7392 0.049(6) Uiso 1 1 calc R . . C17 C 0.1401(3) -0.10035(15) 1.0614(2) 0.0801(10) Uani 1 1 d . . . H17A H 0.1660 -0.1442 1.0474 0.115(13) Uiso 1 1 calc R . . H17B H 0.0571 -0.1017 1.0712 0.128(15) Uiso 1 1 calc R . . H17C H 0.1936 -0.0833 1.1258 0.093(10) Uiso 1 1 calc R . . C21 C 0.48091(18) 0.24033(9) 0.98497(15) 0.0363(4) Uani 1 1 d . . . H21A H 0.5596 0.2184 1.0103 0.034(5) Uiso 1 1 calc R . . H21B H 0.4862 0.2840 1.0177 0.039(5) Uiso 1 1 calc R . . C22 C 0.45510(19) 0.24705(9) 0.86492(15) 0.0364(4) Uani 1 1 d . . . H22A H 0.3807 0.2728 0.8398 0.031(5) Uiso 1 1 calc R . . H22B H 0.5228 0.2698 0.8438 0.032(5) Uiso 1 1 calc R . . N22 N 0.44004(14) 0.18214(7) 0.81701(11) 0.0310(3) Uani 1 1 d . . . C23 C 0.51380(17) 0.16350(9) 0.76173(14) 0.0337(4) Uani 1 1 d . . . H23 H 0.5756 0.1916 0.7497 0.026(5) Uiso 1 1 calc R . . N23 N 0.40965(13) 0.05901(7) 0.73726(11) 0.0310(3) Uani 1 1 d . . . C24 C 0.50116(17) 0.09870(9) 0.71787(14) 0.0327(4) Uani 1 1 d . . . N24 N 0.51413(16) 0.00650(8) 0.64000(13) 0.0409(4) Uani 1 1 d . . . H24 H 0.5369 -0.0251 0.6031 0.067(8) Uiso 1 1 calc R . . C25 C 0.56733(19) 0.06622(10) 0.65761(16) 0.0404(4) Uani 1 1 d . . . C26 C 0.42058(17) 0.00425(9) 0.68893(14) 0.0346(4) Uani 1 1 d . . . H26 H 0.3695 -0.0323 0.6883 0.036(5) Uiso 1 1 calc R . . C27 C 0.6740(2) 0.08623(13) 0.6155(2) 0.0622(7) Uani 1 1 d . . . H27A H 0.7065 0.1270 0.6490 0.083(10) Uiso 1 1 calc R . . H27B H 0.6493 0.0923 0.5385 0.096(11) Uiso 1 1 calc R . . H27C H 0.7362 0.0525 0.6314 0.103(11) Uiso 1 1 calc R . . Cl31 Cl 0.21744(4) 0.09364(3) 0.31294(4) 0.04294(12) Uani 1 1 d . . . O31 O 0.33095(14) 0.10211(8) 0.38749(14) 0.0554(4) Uani 1 1 d . . . O32 O 0.13329(15) 0.06286(9) 0.36426(12) 0.0585(4) Uani 1 1 d . . . O33 O 0.17197(19) 0.15491(11) 0.2724(2) 0.0968(8) Uani 1 1 d . . . O34 O 0.23500(18) 0.05370(12) 0.22763(14) 0.0785(6) Uani 1 1 d . . . Cl41 Cl 0.77454(4) 0.32753(2) 0.78751(4) 0.03817(11) Uani 1 1 d . . . O41 O 0.75672(16) 0.25931(8) 0.79898(15) 0.0612(4) Uani 1 1 d . . . O42 O 0.73220(15) 0.34620(10) 0.67939(13) 0.0657(5) Uani 1 1 d . . . O43 O 0.90175(13) 0.33973(9) 0.81828(12) 0.0522(4) Uani 1 1 d . . . O44 O 0.71147(18) 0.36161(9) 0.85419(16) 0.0705(5) 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 Mn1 0.02882(14) 0.03358(15) 0.02538(13) 0.00184(10) 0.00604(10) 0.00104(11) C1 0.0439(11) 0.0382(10) 0.0324(9) -0.0088(8) 0.0092(8) 0.0028(8) N1 0.0343(8) 0.0326(8) 0.0284(7) -0.0021(6) 0.0078(6) -0.0022(6) C2 0.0372(10) 0.0476(11) 0.0311(9) -0.0068(8) 0.0113(8) 0.0045(8) N2 0.0320(8) 0.0363(8) 0.0283(7) -0.0037(6) 0.0070(6) 0.0000(6) C3 0.0317(9) 0.0353(10) 0.0356(9) 0.0001(7) 0.0099(7) 0.0027(7) N3 0.0343(8) 0.0360(8) 0.0261(7) 0.0002(6) 0.0047(6) 0.0037(6) C4 0.0305(9) 0.0341(9) 0.0315(9) 0.0024(7) 0.0060(7) 0.0006(7) N4 0.0400(9) 0.0432(9) 0.0275(8) 0.0019(7) -0.0002(7) -0.0027(7) C5 0.0326(9) 0.0393(10) 0.0326(9) 0.0061(8) 0.0046(7) -0.0026(8) C6 0.0419(10) 0.0372(10) 0.0275(9) -0.0007(7) 0.0038(7) 0.0032(8) C7 0.0370(11) 0.0659(15) 0.0464(12) 0.0115(11) 0.0040(9) 0.0098(10) C11 0.0380(10) 0.0409(10) 0.0253(8) -0.0030(7) 0.0037(7) -0.0060(8) C12 0.0346(9) 0.0365(10) 0.0298(9) 0.0016(7) -0.0024(7) -0.0045(8) N12 0.0334(8) 0.0307(8) 0.0270(7) -0.0012(6) 0.0031(6) -0.0025(6) C13 0.0401(10) 0.0305(9) 0.0270(8) 0.0000(7) 0.0078(7) -0.0001(7) N13 0.0352(8) 0.0379(9) 0.0315(8) -0.0019(6) 0.0048(6) -0.0052(7) C14 0.0395(10) 0.0324(9) 0.0310(9) -0.0025(7) 0.0106(7) -0.0044(8) N14 0.0522(11) 0.0565(12) 0.0546(11) -0.0046(9) 0.0057(9) -0.0277(10) C15 0.0560(13) 0.0435(12) 0.0438(11) -0.0029(9) 0.0119(10) -0.0170(10) C16 0.0442(12) 0.0515(13) 0.0413(11) -0.0047(9) 0.0029(9) -0.0116(10) C17 0.107(3) 0.070(2) 0.0617(17) 0.0106(14) 0.0158(17) -0.0470(18) C21 0.0403(10) 0.0339(10) 0.0346(10) -0.0050(8) 0.0083(8) -0.0078(8) C22 0.0455(11) 0.0296(9) 0.0365(10) -0.0012(7) 0.0146(8) -0.0031(8) N22 0.0369(8) 0.0295(7) 0.0270(7) 0.0002(6) 0.0079(6) -0.0013(6) C23 0.0370(10) 0.0332(9) 0.0330(9) 0.0035(7) 0.0118(8) -0.0016(8) N23 0.0324(8) 0.0319(8) 0.0285(7) 0.0017(6) 0.0064(6) 0.0010(6) C24 0.0357(9) 0.0338(9) 0.0302(9) 0.0031(7) 0.0109(7) 0.0014(7) N24 0.0503(10) 0.0371(9) 0.0381(9) -0.0047(7) 0.0160(8) 0.0048(8) C25 0.0467(11) 0.0392(10) 0.0397(10) 0.0012(8) 0.0192(9) 0.0026(9) C26 0.0376(10) 0.0329(9) 0.0320(9) 0.0005(7) 0.0048(7) 0.0013(8) C27 0.0686(16) 0.0555(15) 0.0779(18) -0.0017(13) 0.0493(15) -0.0019(13) Cl31 0.0360(2) 0.0526(3) 0.0415(3) -0.0041(2) 0.0113(2) -0.0021(2) O31 0.0397(8) 0.0489(9) 0.0720(11) -0.0211(8) 0.0008(7) -0.0003(7) O32 0.0538(9) 0.0811(12) 0.0448(9) -0.0121(8) 0.0204(7) -0.0213(9) O33 0.0680(13) 0.0811(15) 0.141(2) 0.0441(15) 0.0222(13) 0.0224(11) O34 0.0733(12) 0.1210(18) 0.0476(10) -0.0332(11) 0.0272(9) -0.0135(12) Cl41 0.0294(2) 0.0447(3) 0.0384(2) 0.00268(19) 0.00331(18) 0.00193(18) O41 0.0682(11) 0.0455(9) 0.0732(11) -0.0035(8) 0.0226(9) -0.0107(8) O42 0.0457(9) 0.0975(14) 0.0458(9) 0.0210(9) -0.0069(7) 0.0038(9) O43 0.0344(7) 0.0756(11) 0.0412(8) 0.0056(7) -0.0028(6) -0.0113(7) O44 0.0794(13) 0.0642(11) 0.0775(13) 0.0023(9) 0.0382(10) 0.0273(10) _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 Mn1 N12 2.2517(15) . ? Mn1 N3 2.2532(15) . ? Mn1 N2 2.2668(15) . ? Mn1 N22 2.2739(15) . ? Mn1 N13 2.2931(16) . ? Mn1 N23 2.2955(15) . ? C1 N1 1.460(2) . ? C1 C2 1.522(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? N1 C21 1.460(2) . ? N1 C11 1.463(2) . ? C2 N2 1.465(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N2 C3 1.274(2) . ? C3 C4 1.447(3) . ? C3 H3 0.9500 . ? N3 C6 1.312(2) . ? N3 C4 1.385(2) . ? C4 C5 1.371(2) . ? N4 C6 1.356(2) . ? N4 C5 1.368(3) . ? N4 H4 0.8800 . ? C5 C7 1.486(3) . ? C6 H6 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C11 C12 1.521(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N12 1.462(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? N12 C13 1.270(2) . ? C13 C14 1.444(3) . ? C13 H13 0.9500 . ? N13 C16 1.305(2) . ? N13 C14 1.387(2) . ? C14 C15 1.363(3) . ? N14 C16 1.349(3) . ? N14 C15 1.365(3) . ? N14 H14 0.8800 . ? C15 C17 1.492(3) . ? C16 H16 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C21 C22 1.520(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 N22 1.469(2) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? N22 C23 1.276(2) . ? C23 C24 1.446(3) . ? C23 H23 0.9500 . ? N23 C26 1.310(2) . ? N23 C24 1.389(2) . ? C24 C25 1.372(3) . ? N24 C26 1.354(3) . ? N24 C25 1.368(3) . ? N24 H24 0.8800 . ? C25 C27 1.494(3) . ? C26 H26 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? Cl31 O33 1.420(2) . ? Cl31 O34 1.4256(17) . ? Cl31 O32 1.4285(16) . ? Cl31 O31 1.4383(16) . ? Cl41 O44 1.4236(17) . ? Cl41 O42 1.4259(16) . ? Cl41 O43 1.4335(15) . ? Cl41 O41 1.4335(17) . ? 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 N12 Mn1 N3 159.27(6) . . ? N12 Mn1 N2 101.24(5) . . ? N3 Mn1 N2 73.49(5) . . ? N12 Mn1 N22 102.71(5) . . ? N3 Mn1 N22 98.00(6) . . ? N2 Mn1 N22 101.03(6) . . ? N12 Mn1 N13 73.13(5) . . ? N3 Mn1 N13 87.02(6) . . ? N2 Mn1 N13 93.42(6) . . ? N22 Mn1 N13 165.51(6) . . ? N12 Mn1 N23 100.19(5) . . ? N3 Mn1 N23 86.59(5) . . ? N2 Mn1 N23 158.56(5) . . ? N22 Mn1 N23 73.46(5) . . ? N13 Mn1 N23 93.39(6) . . ? N1 C1 C2 110.92(15) . . ? N1 C1 H1A 109.5 . . ? C2 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 108.0 . . ? C1 N1 C21 113.59(15) . . ? C1 N1 C11 114.08(15) . . ? C21 N1 C11 113.52(15) . . ? N2 C2 C1 109.31(15) . . ? N2 C2 H2A 109.8 . . ? C1 C2 H2A 109.8 . . ? N2 C2 H2B 109.8 . . ? C1 C2 H2B 109.8 . . ? H2A C2 H2B 108.3 . . ? C3 N2 C2 119.55(16) . . ? C3 N2 Mn1 116.84(12) . . ? C2 N2 Mn1 123.46(12) . . ? N2 C3 C4 118.23(17) . . ? N2 C3 H3 120.9 . . ? C4 C3 H3 120.9 . . ? C6 N3 C4 105.87(15) . . ? C6 N3 Mn1 140.86(13) . . ? C4 N3 Mn1 113.25(11) . . ? C5 C4 N3 110.03(16) . . ? C5 C4 C3 131.85(17) . . ? N3 C4 C3 118.12(16) . . ? C6 N4 C5 108.65(15) . . ? C6 N4 H4 125.7 . . ? C5 N4 H4 125.7 . . ? N4 C5 C4 104.79(16) . . ? N4 C5 C7 123.27(17) . . ? C4 C5 C7 131.92(19) . . ? N3 C6 N4 110.66(17) . . ? N3 C6 H6 124.7 . . ? N4 C6 H6 124.7 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C11 C12 110.53(14) . . ? N1 C11 H11A 109.5 . . ? C12 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? N12 C12 C11 108.47(15) . . ? N12 C12 H12A 110.0 . . ? C11 C12 H12A 110.0 . . ? N12 C12 H12B 110.0 . . ? C11 C12 H12B 110.0 . . ? H12A C12 H12B 108.4 . . ? C13 N12 C12 119.15(15) . . ? C13 N12 Mn1 117.54(12) . . ? C12 N12 Mn1 122.40(11) . . ? N12 C13 C14 118.62(16) . . ? N12 C13 H13 120.7 . . ? C14 C13 H13 120.7 . . ? C16 N13 C14 105.23(17) . . ? C16 N13 Mn1 141.95(15) . . ? C14 N13 Mn1 112.00(11) . . ? C15 C14 N13 110.36(17) . . ? C15 C14 C13 131.50(18) . . ? N13 C14 C13 118.10(16) . . ? C16 N14 C15 108.58(18) . . ? C16 N14 H14 125.7 . . ? C15 N14 H14 125.7 . . ? C14 C15 N14 104.61(18) . . ? C14 C15 C17 132.0(2) . . ? N14 C15 C17 123.4(2) . . ? N13 C16 N14 111.21(19) . . ? N13 C16 H16 124.4 . . ? N14 C16 H16 124.4 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N1 C21 C22 110.90(15) . . ? N1 C21 H21A 109.5 . . ? C22 C21 H21A 109.5 . . ? N1 C21 H21B 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 108.0 . . ? N22 C22 C21 108.98(15) . . ? N22 C22 H22A 109.9 . . ? C21 C22 H22A 109.9 . . ? N22 C22 H22B 109.9 . . ? C21 C22 H22B 109.9 . . ? H22A C22 H22B 108.3 . . ? C23 N22 C22 118.77(16) . . ? C23 N22 Mn1 117.05(12) . . ? C22 N22 Mn1 124.13(11) . . ? N22 C23 C24 118.53(17) . . ? N22 C23 H23 120.7 . . ? C24 C23 H23 120.7 . . ? C26 N23 C24 105.49(15) . . ? C26 N23 Mn1 142.65(13) . . ? C24 N23 Mn1 111.86(11) . . ? C25 C24 N23 110.01(17) . . ? C25 C24 C23 130.89(18) . . ? N23 C24 C23 119.10(16) . . ? C26 N24 C25 108.48(16) . . ? C26 N24 H24 125.8 . . ? C25 N24 H24 125.8 . . ? N24 C25 C24 104.83(17) . . ? N24 C25 C27 123.53(19) . . ? C24 C25 C27 131.6(2) . . ? N23 C26 N24 111.19(17) . . ? N23 C26 H26 124.4 . . ? N24 C26 H26 124.4 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O33 Cl31 O34 109.28(15) . . ? O33 Cl31 O32 109.91(13) . . ? O34 Cl31 O32 109.07(11) . . ? O33 Cl31 O31 109.72(13) . . ? O34 Cl31 O31 109.21(11) . . ? O32 Cl31 O31 109.64(11) . . ? O44 Cl41 O42 110.79(12) . . ? O44 Cl41 O43 111.00(12) . . ? O42 Cl41 O43 108.87(10) . . ? O44 Cl41 O41 108.65(11) . . ? O42 Cl41 O41 109.99(12) . . ? O43 Cl41 O41 107.49(11) . . ? 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 N24 H24 O31 0.88 2.17 2.919(2) 142.6 3_656 N14 H14 Cl31 0.88 2.95 3.6236(19) 134.8 3_556 N4 H4 O43 0.88 2.05 2.899(2) 160.3 4_465 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.430 _refine_diff_density_min -0.360 _refine_diff_density_rms 0.052 _exptl_crystal_id 'Brewer 1139' _diffrn_measurement_total_frames-CCD 1868 _diffrn_measurement_frame_width-CCD 0.30 _diffrn_detector_distance-CCD 4.99 _diffrn_source_voltage 50 _diffrn_source_current 40 _diffrn_measurement_frame_time-CCD 15 _diffrn_measurement_total_time-CCD 12 _diffrn_measurement_frame_size-CCD 512 _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker Smart1000' #===END data_1140ff _database_code_depnum_ccdc_archive 'CCDC 267249' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C21 H30 Mn N10, 2(Cl O4), C2 H6 O, H2 O' _chemical_formula_sum 'C23 H38 Cl2 Mn N10 O10' _chemical_formula_weight 740.47 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 Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 16.6695(4) _cell_length_b 15.4756(4) _cell_length_c 12.9951(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.119(1) _cell_angle_gamma 90.00 _cell_volume 3251.08(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8072 _cell_measurement_theta_min 2.222 _cell_measurement_theta_max 27.500 _exptl_crystal_description Hexagon _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1540 _exptl_absorpt_coefficient_mu 0.638 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7750 _exptl_absorpt_correction_T_max 0.8090 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _diffrn_ambient_temperature 173(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_% 0 _diffrn_reflns_number 61025 _diffrn_reflns_av_R_equivalents 0.0194 _diffrn_reflns_av_sigmaI/netI 0.0097 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7462 _reflns_number_gt 6586 _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^)+(0.0150P)^2^+3.7150P] 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 7462 _refine_ls_number_parameters 496 _refine_ls_number_restraints 99 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0786 _refine_ls_wR_factor_gt 0.0761 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.000 _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 Mn1 Mn 0.265696(18) 0.460766(18) 0.44953(2) 0.03012(8) Uani 1 1 d . . . C1 C 0.21240(13) 0.37315(13) 0.19073(14) 0.0357(4) Uani 1 1 d . . . H1A H 0.1805 0.3312 0.1392 0.048(7) Uiso 1 1 calc R . . H1B H 0.2585 0.3951 0.1622 0.030(5) Uiso 1 1 calc R . . N1 N 0.24609(10) 0.32965(10) 0.29248(12) 0.0325(3) Uani 1 1 d . . . C2 C 0.15642(13) 0.44812(12) 0.20395(15) 0.0350(4) Uani 1 1 d . . . H2A H 0.1375 0.4794 0.1359 0.044(6) Uiso 1 1 calc R . . H2B H 0.1072 0.4260 0.2254 0.040(6) Uiso 1 1 calc R . . N2 N 0.20310(10) 0.50656(10) 0.28526(12) 0.0308(3) Uani 1 1 d . . . C3 C 0.20866(12) 0.58668(12) 0.26492(15) 0.0318(4) Uani 1 1 d . . . H3 H 0.1810 0.6095 0.1978 0.040(6) Uiso 1 1 calc R . . N3 N 0.29945(10) 0.60613(10) 0.44159(12) 0.0325(3) Uani 1 1 d . . . C4 C 0.25764(11) 0.64196(12) 0.34549(15) 0.0308(4) Uani 1 1 d . . . N4 N 0.32425(10) 0.74592(11) 0.44229(14) 0.0371(4) Uani 1 1 d . . . H4 H 0.3445 0.7968 0.4652 0.054(7) Uiso 1 1 calc R . . C5 C 0.27303(12) 0.72895(13) 0.34509(16) 0.0355(4) Uani 1 1 d . . . C6 C 0.33837(12) 0.67109(13) 0.49713(16) 0.0358(4) Uani 1 1 d . . . H6 H 0.3722 0.6661 0.5672 0.045(6) Uiso 1 1 calc R . . C7 C 0.24568(18) 0.79648(15) 0.2631(2) 0.0559(7) Uani 1 1 d . . . H7A H 0.2141 0.7696 0.1973 0.080(10) Uiso 1 1 calc R . . H7B H 0.2942 0.8259 0.2497 0.087(11) Uiso 1 1 calc R . . H7C H 0.2107 0.8385 0.2880 0.083(10) Uiso 1 1 calc R . . C11 C 0.32856(13) 0.29314(14) 0.30062(15) 0.0385(4) Uani 1 1 d . . . H11A H 0.3313 0.2683 0.2313 0.046(6) Uiso 1 1 calc R . . H11B H 0.3389 0.2460 0.3538 0.037(6) Uiso 1 1 calc R . . C12 C 0.39477(13) 0.36239(15) 0.33309(15) 0.0408(5) Uani 1 1 d . . . H12A H 0.4504 0.3363 0.3438 0.043(6) Uiso 1 1 calc R . . H12B H 0.3883 0.4068 0.2769 0.044(6) Uiso 1 1 calc R . . N12 N 0.38532(10) 0.40173(11) 0.43205(12) 0.0351(4) Uani 1 1 d . . . C13 C 0.44163(13) 0.39008(14) 0.51675(15) 0.0368(4) Uani 1 1 d . . . H13 H 0.4918 0.3620 0.5145 0.039(6) Uiso 1 1 calc R . . N13 N 0.35290(10) 0.45821(11) 0.61699(12) 0.0349(4) Uani 1 1 d . . . C14 C 0.42809(12) 0.42019(13) 0.61631(15) 0.0340(4) Uani 1 1 d . . . N14 N 0.43056(11) 0.44967(12) 0.77976(13) 0.0435(4) Uani 1 1 d . . . H14 H 0.4459 0.4549 0.8492 0.068(9) Uiso 1 1 calc R . . C15 C 0.47681(13) 0.41432(14) 0.71724(16) 0.0386(4) Uani 1 1 d . . . C16 C 0.35735(14) 0.47538(14) 0.71723(16) 0.0413(5) Uani 1 1 d . . . H16 H 0.3146 0.5024 0.7425 0.045(6) Uiso 1 1 calc R . . C17 C 0.56103(15) 0.3778(2) 0.7597(2) 0.0572(7) Uani 1 1 d . . . H17A H 0.5784 0.3465 0.7032 0.095(11) Uiso 1 1 calc R . . H17B H 0.5601 0.3381 0.8181 0.117(14) Uiso 1 1 calc R . . H17C H 0.6001 0.4248 0.7858 0.139(16) Uiso 1 1 calc R . . C21 C 0.18820(14) 0.26697(12) 0.31835(15) 0.0363(4) Uani 1 1 d . . . H21A H 0.1979 0.2096 0.2898 0.039(6) Uiso 1 1 calc R . . H21B H 0.1308 0.2847 0.2841 0.038(6) Uiso 1 1 calc R . . C22 C 0.19834(14) 0.26012(12) 0.43817(15) 0.0358(4) Uani 1 1 d . . . H22A H 0.1557 0.2211 0.4536 0.036(6) Uiso 1 1 calc R . . H22B H 0.2535 0.2362 0.4723 0.040(6) Uiso 1 1 calc R . . N22 N 0.18961(10) 0.34651(10) 0.47976(12) 0.0313(3) Uani 1 1 d . . . C23 C 0.13624(12) 0.35981(12) 0.53381(14) 0.0316(4) Uani 1 1 d . . . H23 H 0.1055 0.3134 0.5530 0.037(6) Uiso 1 1 calc R . . N23 N 0.16513(10) 0.51289(10) 0.52492(12) 0.0326(3) Uani 1 1 d . . . C24 C 0.12403(12) 0.44767(12) 0.56492(14) 0.0310(4) Uani 1 1 d . . . N24 N 0.08495(11) 0.57028(11) 0.61828(14) 0.0391(4) Uani 1 1 d . . . H24 H 0.0606 0.6100 0.6484 0.059(8) Uiso 1 1 calc R . . C25 C 0.07429(12) 0.48270(13) 0.62409(15) 0.0354(4) Uani 1 1 d . . . C26 C 0.13923(13) 0.58508(13) 0.55835(16) 0.0370(4) Uani 1 1 d . . . H26 H 0.1565 0.6410 0.5424 0.044(6) Uiso 1 1 calc R . . C27 C 0.01890(14) 0.44313(16) 0.68542(19) 0.0481(5) Uani 1 1 d . . . H27A H 0.0382 0.4590 0.7604 0.068(8) Uiso 1 1 calc R . . H27B H 0.0198 0.3801 0.6784 0.076(9) Uiso 1 1 calc R . . H27C H -0.0377 0.4643 0.6578 0.079(10) Uiso 1 1 calc R . . O51 O 0.33799(10) 0.57210(11) 0.96290(15) 0.0511(4) Uani 1 1 d D . . H51 H 0.3754(15) 0.5370(17) 0.985(2) 0.084(11) Uiso 1 1 d D . . C51 C 0.26899(17) 0.53897(19) 0.9921(2) 0.0603(7) Uani 1 1 d . . . H51A H 0.2295 0.5866 0.9929 0.153(18) Uiso 1 1 calc R . . H51B H 0.2866 0.5156 1.0650 0.116(14) Uiso 1 1 calc R . . C52 C 0.2256(2) 0.46917(19) 0.9195(3) 0.0665(7) Uani 1 1 d . . . H52A H 0.2122 0.4902 0.8462 0.143(17) Uiso 1 1 calc R . . H52B H 0.1746 0.4531 0.9395 0.045(6) Uiso 1 1 calc R . . H52C H 0.2618 0.4185 0.9256 0.16(2) Uiso 1 1 calc R . . O61 O 0.01887(15) 0.71666(14) 0.68724(17) 0.0671(5) Uani 1 1 d D . . H61 H 0.027(2) 0.728(2) 0.7507(10) 0.083(11) Uiso 1 1 d D . . H62 H 0.023(2) 0.7596(15) 0.651(3) 0.096(13) Uiso 1 1 d D . . Cl3 Cl 0.53334(3) 0.85416(3) 0.43155(4) 0.04311(12) Uani 0.50 1 d PDU A 1 O31 O 0.47081(11) 0.84049(13) 0.33713(13) 0.0639(5) Uani 0.50 1 d PDU A 1 O32 O 0.5083(3) 0.8057(2) 0.5158(3) 0.0457(11) Uani 0.50 1 d PDU A 1 O33 O 0.6150(2) 0.8359(3) 0.4331(4) 0.0640(13) Uani 0.50 1 d PDU A 1 O34 O 0.52880(19) 0.94591(16) 0.4686(2) 0.0418(7) Uani 0.50 1 d PDU A 1 Cl3A Cl 0.53334(3) 0.85416(3) 0.43155(4) 0.04311(12) Uani 0.50 1 d PDU B 2 O31A O 0.47081(11) 0.84049(13) 0.33713(13) 0.0639(5) Uani 0.50 1 d PDU B 2 O32A O 0.5664(3) 0.9374(2) 0.4142(3) 0.0696(11) Uani 0.50 1 d PDU B 2 O33A O 0.5088(4) 0.8416(3) 0.5240(3) 0.0648(15) Uani 0.50 1 d PDU B 2 O34A O 0.5981(3) 0.7920(3) 0.4225(5) 0.0784(17) Uani 0.50 1 d PDU B 2 Cl4 Cl 0.94771(4) 0.16511(4) 0.53344(5) 0.05627(16) Uani 1 1 d DU . . O41 O 0.93796(13) 0.09298(14) 0.59746(19) 0.0877(7) Uani 1 1 d DU . . O42 O 0.99098(16) 0.23214(15) 0.59907(15) 0.0936(8) Uani 1 1 d DU . . O43 O 0.99379(18) 0.14177(16) 0.4577(2) 0.1041(9) Uani 1 1 d DU . . O44 O 0.86922(13) 0.19625(14) 0.47678(18) 0.0818(7) Uani 1 1 d DU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.03658(16) 0.02871(14) 0.02522(14) 0.00317(11) 0.00786(11) 0.00220(11) C1 0.0491(11) 0.0342(10) 0.0234(8) -0.0009(7) 0.0082(8) -0.0005(8) N1 0.0439(9) 0.0306(8) 0.0245(7) 0.0015(6) 0.0110(7) 0.0026(7) C2 0.0427(11) 0.0319(10) 0.0270(9) -0.0004(7) 0.0017(8) -0.0021(8) N2 0.0367(8) 0.0288(8) 0.0260(7) 0.0003(6) 0.0060(6) -0.0003(6) C3 0.0349(9) 0.0302(9) 0.0295(9) 0.0037(7) 0.0062(7) 0.0021(7) N3 0.0355(8) 0.0310(8) 0.0300(8) 0.0028(6) 0.0061(6) -0.0012(6) C4 0.0323(9) 0.0283(9) 0.0313(9) 0.0035(7) 0.0070(7) 0.0011(7) N4 0.0381(9) 0.0296(8) 0.0413(9) -0.0011(7) 0.0053(7) -0.0047(7) C5 0.0371(10) 0.0299(9) 0.0379(10) 0.0023(8) 0.0062(8) -0.0017(8) C6 0.0339(10) 0.0371(10) 0.0344(10) 0.0013(8) 0.0045(8) -0.0018(8) C7 0.0733(17) 0.0308(11) 0.0524(14) 0.0096(10) -0.0061(12) -0.0053(11) C11 0.0505(12) 0.0390(11) 0.0282(9) -0.0023(8) 0.0138(8) 0.0089(9) C12 0.0439(11) 0.0533(13) 0.0284(9) -0.0013(9) 0.0148(8) 0.0060(10) N12 0.0399(9) 0.0398(9) 0.0270(8) -0.0008(7) 0.0110(7) 0.0025(7) C13 0.0355(10) 0.0423(11) 0.0336(10) -0.0021(8) 0.0102(8) 0.0026(8) N13 0.0406(9) 0.0359(9) 0.0275(8) 0.0004(6) 0.0068(7) 0.0075(7) C14 0.0358(10) 0.0346(10) 0.0308(9) -0.0012(8) 0.0067(8) 0.0022(8) N14 0.0480(10) 0.0534(11) 0.0256(8) -0.0085(8) 0.0022(7) 0.0049(9) C15 0.0383(10) 0.0423(11) 0.0326(10) -0.0050(8) 0.0037(8) 0.0001(9) C16 0.0471(12) 0.0439(11) 0.0320(10) -0.0054(9) 0.0081(9) 0.0093(9) C17 0.0403(12) 0.0832(19) 0.0416(13) -0.0078(13) -0.0027(10) 0.0107(13) C21 0.0527(12) 0.0271(9) 0.0312(9) -0.0031(7) 0.0142(9) -0.0014(8) C22 0.0531(12) 0.0254(9) 0.0328(9) 0.0008(7) 0.0182(9) 0.0031(8) N22 0.0431(9) 0.0262(7) 0.0260(7) 0.0007(6) 0.0112(6) 0.0023(6) C23 0.0393(10) 0.0290(9) 0.0272(9) 0.0011(7) 0.0095(7) -0.0003(8) N23 0.0383(9) 0.0289(8) 0.0302(8) -0.0018(6) 0.0076(7) 0.0010(7) C24 0.0344(9) 0.0320(9) 0.0260(8) -0.0024(7) 0.0062(7) 0.0011(7) N24 0.0377(9) 0.0373(9) 0.0412(9) -0.0133(7) 0.0074(7) 0.0046(7) C25 0.0321(9) 0.0410(11) 0.0319(9) -0.0081(8) 0.0057(8) 0.0015(8) C26 0.0412(11) 0.0314(10) 0.0358(10) -0.0053(8) 0.0044(8) 0.0021(8) C27 0.0446(12) 0.0575(14) 0.0477(13) -0.0132(11) 0.0215(10) -0.0035(11) O51 0.0437(9) 0.0400(9) 0.0678(11) 0.0110(8) 0.0101(8) 0.0045(7) C51 0.0578(15) 0.0577(16) 0.0687(18) 0.0000(13) 0.0219(13) -0.0048(13) C52 0.0709(19) 0.0534(16) 0.075(2) -0.0023(14) 0.0166(15) -0.0103(14) O61 0.0952(15) 0.0596(12) 0.0542(12) -0.0030(10) 0.0334(11) 0.0250(11) Cl3 0.0380(3) 0.0391(3) 0.0495(3) 0.0033(2) 0.0055(2) -0.0012(2) O31 0.0630(11) 0.0819(13) 0.0427(9) -0.0092(9) 0.0050(8) -0.0153(10) O32 0.053(2) 0.044(2) 0.042(2) -0.0046(17) 0.0148(17) 0.001(2) O33 0.0379(18) 0.088(3) 0.070(3) 0.010(3) 0.0207(17) 0.005(2) O34 0.0446(17) 0.0349(15) 0.0420(16) 0.0028(13) 0.0027(13) -0.0059(13) Cl3A 0.0380(3) 0.0391(3) 0.0495(3) 0.0033(2) 0.0055(2) -0.0012(2) O31A 0.0630(11) 0.0819(13) 0.0427(9) -0.0092(9) 0.0050(8) -0.0153(10) O32A 0.076(3) 0.046(2) 0.078(3) -0.0019(19) 0.002(2) -0.0204(19) O33A 0.067(3) 0.092(4) 0.040(2) -0.027(3) 0.0240(18) 0.007(3) O34A 0.086(3) 0.076(3) 0.091(4) 0.035(3) 0.056(3) 0.039(3) Cl4 0.0655(4) 0.0437(3) 0.0499(3) 0.0075(2) -0.0045(3) -0.0078(3) O41 0.0754(14) 0.0655(13) 0.1103(18) 0.0430(13) 0.0001(13) -0.0131(11) O42 0.128(2) 0.1001(17) 0.0481(11) -0.0062(11) 0.0135(12) -0.0736(16) O43 0.144(2) 0.0768(16) 0.1030(19) 0.0045(14) 0.0527(18) 0.0284(16) O44 0.0808(14) 0.0668(13) 0.0803(14) 0.0129(11) -0.0140(11) 0.0043(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 Mn1 N2 2.2498(15) . ? Mn1 N12 2.2547(17) . ? Mn1 N22 2.2655(16) . ? Mn1 N23 2.2851(16) . ? Mn1 N13 2.3037(16) . ? Mn1 N3 2.3272(16) . ? C1 N1 1.468(2) . ? C1 C2 1.525(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? N1 C21 1.464(2) . ? N1 C11 1.466(3) . ? C2 N2 1.462(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N2 C3 1.276(2) . ? C3 C4 1.441(3) . ? C3 H3 0.9500 . ? N3 C6 1.313(2) . ? N3 C4 1.389(2) . ? C4 C5 1.371(3) . ? N4 C6 1.350(3) . ? N4 C5 1.366(3) . ? N4 H4 0.8800 . ? C5 C7 1.483(3) . ? C6 H6 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C11 C12 1.522(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N12 1.466(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? N12 C13 1.273(3) . ? C13 C14 1.444(3) . ? C13 H13 0.9500 . ? N13 C16 1.314(2) . ? N13 C14 1.387(2) . ? C14 C15 1.367(3) . ? N14 C16 1.351(3) . ? N14 C15 1.363(3) . ? N14 H14 0.8800 . ? C15 C17 1.489(3) . ? C16 H16 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C21 C22 1.528(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 N22 1.463(2) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? N22 C23 1.277(2) . ? C23 C24 1.447(3) . ? C23 H23 0.9500 . ? N23 C26 1.310(2) . ? N23 C24 1.390(2) . ? C24 C25 1.372(3) . ? N24 C26 1.350(3) . ? N24 C25 1.371(3) . ? N24 H24 0.8800 . ? C25 C27 1.491(3) . ? C26 H26 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? O51 C51 1.394(3) . ? O51 H51 0.825(11) . ? C51 C52 1.498(4) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? O61 H61 0.821(11) . ? O61 H62 0.824(11) . ? Cl3 O33 1.385(3) . ? Cl3 O31 1.4187(16) . ? Cl3 O32 1.469(3) . ? Cl3 O34 1.507(3) . ? Cl4 O44 1.4200(19) . ? Cl4 O42 1.4225(19) . ? Cl4 O41 1.4250(18) . ? Cl4 O43 1.434(2) . ? 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 N2 Mn1 N12 104.41(6) . . ? N2 Mn1 N22 105.11(6) . . ? N12 Mn1 N22 104.33(6) . . ? N2 Mn1 N23 94.40(6) . . ? N12 Mn1 N23 161.01(6) . . ? N22 Mn1 N23 72.59(6) . . ? N2 Mn1 N13 160.30(6) . . ? N12 Mn1 N13 73.65(6) . . ? N22 Mn1 N13 94.23(6) . . ? N23 Mn1 N13 87.76(6) . . ? N2 Mn1 N3 73.42(6) . . ? N12 Mn1 N3 99.09(6) . . ? N22 Mn1 N3 156.03(6) . . ? N23 Mn1 N3 83.59(6) . . ? N13 Mn1 N3 87.41(6) . . ? N1 C1 C2 110.96(15) . . ? N1 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? C21 N1 C11 112.78(16) . . ? C21 N1 C1 112.46(16) . . ? C11 N1 C1 112.80(15) . . ? N2 C2 C1 108.64(16) . . ? N2 C2 H2A 110.0 . . ? C1 C2 H2A 110.0 . . ? N2 C2 H2B 110.0 . . ? C1 C2 H2B 110.0 . . ? H2A C2 H2B 108.3 . . ? C3 N2 C2 120.27(16) . . ? C3 N2 Mn1 117.54(13) . . ? C2 N2 Mn1 122.18(12) . . ? N2 C3 C4 118.89(17) . . ? N2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C6 N3 C4 105.12(16) . . ? C6 N3 Mn1 143.91(13) . . ? C4 N3 Mn1 110.62(12) . . ? C5 C4 N3 110.02(17) . . ? C5 C4 C3 130.80(18) . . ? N3 C4 C3 119.17(16) . . ? C6 N4 C5 108.20(16) . . ? C6 N4 H4 125.9 . . ? C5 N4 H4 125.9 . . ? N4 C5 C4 105.10(17) . . ? N4 C5 C7 122.84(18) . . ? C4 C5 C7 132.06(19) . . ? N3 C6 N4 111.56(17) . . ? N3 C6 H6 124.2 . . ? N4 C6 H6 124.2 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C11 C12 110.63(17) . . ? N1 C11 H11A 109.5 . . ? C12 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? N12 C12 C11 108.05(16) . . ? N12 C12 H12A 110.1 . . ? C11 C12 H12A 110.1 . . ? N12 C12 H12B 110.1 . . ? C11 C12 H12B 110.1 . . ? H12A C12 H12B 108.4 . . ? C13 N12 C12 119.04(17) . . ? C13 N12 Mn1 116.99(13) . . ? C12 N12 Mn1 122.94(13) . . ? N12 C13 C14 119.05(18) . . ? N12 C13 H13 120.5 . . ? C14 C13 H13 120.5 . . ? C16 N13 C14 105.05(17) . . ? C16 N13 Mn1 143.44(15) . . ? C14 N13 Mn1 111.36(12) . . ? C15 C14 N13 110.39(17) . . ? C15 C14 C13 130.72(19) . . ? N13 C14 C13 118.80(17) . . ? C16 N14 C15 108.60(17) . . ? C16 N14 H14 125.7 . . ? C15 N14 H14 125.7 . . ? N14 C15 C14 104.78(18) . . ? N14 C15 C17 123.40(19) . . ? C14 C15 C17 131.8(2) . . ? N13 C16 N14 111.17(19) . . ? N13 C16 H16 124.4 . . ? N14 C16 H16 124.4 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N1 C21 C22 111.38(16) . . ? N1 C21 H21A 109.4 . . ? C22 C21 H21A 109.4 . . ? N1 C21 H21B 109.4 . . ? C22 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? N22 C22 C21 108.47(15) . . ? N22 C22 H22A 110.0 . . ? C21 C22 H22A 110.0 . . ? N22 C22 H22B 110.0 . . ? C21 C22 H22B 110.0 . . ? H22A C22 H22B 108.4 . . ? C23 N22 C22 119.72(16) . . ? C23 N22 Mn1 117.65(13) . . ? C22 N22 Mn1 122.62(12) . . ? N22 C23 C24 117.99(17) . . ? N22 C23 H23 121.0 . . ? C24 C23 H23 121.0 . . ? C26 N23 C24 105.24(16) . . ? C26 N23 Mn1 141.18(14) . . ? C24 N23 Mn1 112.59(12) . . ? C25 C24 N23 110.06(17) . . ? C25 C24 C23 132.31(18) . . ? N23 C24 C23 117.52(16) . . ? C26 N24 C25 108.28(16) . . ? C26 N24 H24 125.9 . . ? C25 N24 H24 125.9 . . ? N24 C25 C24 104.80(18) . . ? N24 C25 C27 122.75(18) . . ? C24 C25 C27 132.4(2) . . ? N23 C26 N24 111.61(18) . . ? N23 C26 H26 124.2 . . ? N24 C26 H26 124.2 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C51 O51 H51 105(2) . . ? O51 C51 C52 113.4(2) . . ? O51 C51 H51A 108.9 . . ? C52 C51 H51A 108.9 . . ? O51 C51 H51B 108.9 . . ? C52 C51 H51B 108.9 . . ? H51A C51 H51B 107.7 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? H61 O61 H62 113(3) . . ? O33 Cl3 O31 119.6(2) . . ? O33 Cl3 O32 110.0(3) . . ? O31 Cl3 O32 106.6(2) . . ? O33 Cl3 O34 108.3(2) . . ? O31 Cl3 O34 109.46(14) . . ? O32 Cl3 O34 101.39(19) . . ? O44 Cl4 O42 109.37(15) . . ? O44 Cl4 O41 110.28(14) . . ? O42 Cl4 O41 109.55(13) . . ? O44 Cl4 O43 108.04(16) . . ? O42 Cl4 O43 108.48(16) . . ? O41 Cl4 O43 111.07(15) . . ? 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 N4 H4 O51 0.88 2.03 2.833(2) 151.0 4_575 N14 H14 O34 0.88 2.31 3.174(3) 169.4 2_646 N14 H14 O34 0.88 2.37 3.058(3) 135.0 4_576 N14 H14 O33A 0.88 2.40 3.010(5) 127.0 2_646 N14 H14 O32A 0.88 2.59 3.050(4) 113.6 4_576 N24 H24 O61 0.88 1.91 2.762(3) 163.9 . O51 H51 O34 0.825(11) 2.105(11) 2.928(3) 176(3) 2_646 O51 H51 O32A 0.825(11) 2.101(18) 2.863(4) 154(3) 2_646 O61 H61 O42 0.821(11) 2.045(16) 2.832(3) 160(3) 2_656 O61 H61 Cl4 0.821(11) 2.90(2) 3.624(2) 149(3) 2_656 O61 H62 O43 0.824(11) 2.055(14) 2.864(3) 167(4) 3_666 O61 H62 Cl4 0.824(11) 2.82(2) 3.558(2) 151(3) 3_666 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.629 _refine_diff_density_min -0.652 _refine_diff_density_rms 0.052 _exptl_crystal_id 'Brewer 1140' _diffrn_measurement_total_frames-CCD 1868 _diffrn_measurement_frame_width-CCD 0.30 _diffrn_detector_distance-CCD 4.99 _diffrn_source_voltage 50 _diffrn_source_current 40 _diffrn_measurement_frame_time-CCD 15 _diffrn_measurement_total_time-CCD 12 _diffrn_measurement_frame_size-CCD 512 _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker Smart1000' #===END data_wrs1302m _database_code_depnum_ccdc_archive 'CCDC 267250' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C21 H30 Fe N6), 6(Cl O4), 3(C2 H6 O)' _chemical_formula_sum 'C48 H78 Cl6 Fe2 N20 O27' _chemical_formula_weight 1691.70 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 hexagonal _symmetry_space_group_name_H-M 'R 3' _symmetry_space_group_name_Hall 'R 3' _symmetry_int_tables_number 146 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' _cell_length_a 16.5805(8) _cell_length_b 16.5805(8) _cell_length_c 22.0774(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5256.2(5) _cell_formula_units_Z 3 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8957 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 28.29 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2628 _exptl_absorpt_coefficient_mu 0.737 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7094 _exptl_absorpt_correction_T_max 0.7569 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Siemens KFFMO2K-90' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18624 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 28.29 _reflns_number_total 5525 _reflns_number_gt 5521 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2002; Sheldrick, 1998)' _computing_structure_solution 'XS (Sheldrick, 2001)' _computing_structure_refinement 'XL (Sheldrick, 2001)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'enCIFer (CCDC, 2004)' _refine_special_details ; The asymmetric unit is comprised of two 1/3-cations, two perchlorate anions, and one molecule of ethanol. All non-hydrogen atoms were refined with parameters for anisotropic thermal motion. Hydrogens were placed at calculated geometries and allowed to ride on the position of the parent atom. Hydrogen thermal parameters were set to 1.2x the equivalent isotropic U of the parent, 1.5x for methyl and hydroxy hydrogens. The assignment of the oxygen in the ethanol was made based on hydrogen bonding, rather than a strict analysis of the size of the thermal parameter. The crystal is twinned by merohedry, twin law 0 1 0 1 0 0 0 0 -1. The twin ratio is 0.3848(12). Hydrogen bonding is summarized below in the data tables below. 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^)+(0.0716P)^2^+4.2046P] 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_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.025(19) _refine_ls_number_reflns 5525 _refine_ls_number_parameters 313 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0367 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0962 _refine_ls_wR_factor_gt 0.0962 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.001 _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 Fe1 Fe 1.0000 1.0000 0.70163(3) 0.01614(14) Uani 1 3 d S . . N1 N 1.0000 1.0000 0.8189(2) 0.0211(9) Uani 1 3 d S . . N2 N 0.97609(18) 0.8705(2) 0.73420(13) 0.0193(5) Uani 1 1 d . . . N3 N 0.9024(2) 0.9003(2) 0.63753(13) 0.0190(5) Uani 1 1 d . . . N4 N 0.8208(2) 0.8091(2) 0.56278(12) 0.0199(5) Uani 1 1 d . . . H4A H 0.7885 0.7911 0.5289 0.024 Uiso 1 1 calc R . . C1 C 0.9767(2) 0.9058(3) 0.83884(15) 0.0236(6) Uani 1 1 d . . . H1A H 0.9083 0.8661 0.8428 0.028 Uiso 1 1 calc R . . H1B H 1.0050 0.9094 0.8789 0.028 Uiso 1 1 calc R . . C2 C 1.0126(3) 0.8636(2) 0.79352(15) 0.0238(6) Uani 1 1 d . . . H2A H 1.0815 0.8979 0.7932 0.029 Uiso 1 1 calc R . . H2B H 0.9905 0.7976 0.8037 0.029 Uiso 1 1 calc R . . C3 C 0.9264(2) 0.7979(2) 0.70217(15) 0.0217(6) Uani 1 1 d . . . H3A H 0.9153 0.7381 0.7140 0.026 Uiso 1 1 calc R . . C4 C 0.8883(2) 0.8118(2) 0.64736(15) 0.0199(6) Uani 1 1 d . . . C5 C 0.8372(2) 0.7534(2) 0.60005(14) 0.0200(6) Uani 1 1 d . . . C6 C 0.8618(2) 0.8961(2) 0.58568(14) 0.0208(6) Uani 1 1 d . . . H6A H 0.8614 0.9474 0.5668 0.025 Uiso 1 1 calc R . . C7 C 0.8073(3) 0.6546(2) 0.58765(18) 0.0291(7) Uani 1 1 d . . . H7A H 0.7711 0.6350 0.5500 0.035 Uiso 1 1 calc R . . H7B H 0.7688 0.6158 0.6212 0.035 Uiso 1 1 calc R . . H7C H 0.8623 0.6475 0.5835 0.035 Uiso 1 1 calc R . . Fe2 Fe 0.6667 0.3333 0.56102(3) 0.01694(14) Uani 1 3 d S . . N21 N 0.6667 0.3333 0.4381(2) 0.0187(8) Uani 1 3 d S . . N22 N 0.7886(2) 0.44683(19) 0.52499(13) 0.0201(5) Uani 1 1 d . . . N23 N 0.8748(3) 0.3638(3) 0.69139(16) 0.0348(8) Uani 1 1 d . . . H23A H 0.8973 0.3519 0.7242 0.042 Uiso 1 1 calc R . . N24 N 0.7740(2) 0.3522(2) 0.62307(14) 0.0237(5) Uani 1 1 d . . . C21 C 0.7564(2) 0.4135(2) 0.41931(16) 0.0216(6) Uani 1 1 d . . . H21A H 0.7493 0.4373 0.3798 0.026 Uiso 1 1 calc R . . H21B H 0.8036 0.3940 0.4149 0.026 Uiso 1 1 calc R . . C22 C 0.7876(2) 0.4893(2) 0.46709(16) 0.0229(6) Uani 1 1 d . . . H22A H 0.8505 0.5415 0.4574 0.028 Uiso 1 1 calc R . . H22B H 0.7439 0.5136 0.4689 0.028 Uiso 1 1 calc R . . C23 C 0.8665(2) 0.4734(2) 0.55330(16) 0.0243(6) Uani 1 1 d . . . H23B H 0.9237 0.5233 0.5389 0.029 Uiso 1 1 calc R . . C24 C 0.8616(2) 0.4241(3) 0.60686(15) 0.0256(6) Uani 1 1 d . . . C25 C 0.9252(3) 0.4303(3) 0.65005(18) 0.0333(9) Uani 1 1 d . . . C26 C 0.7848(3) 0.3185(3) 0.67452(17) 0.0294(7) Uani 1 1 d . . . H26A H 0.7358 0.2691 0.6966 0.035 Uiso 1 1 calc R . . C27 C 1.0276(3) 0.4915(4) 0.6562(2) 0.0452(12) Uani 1 1 d . . . H27A H 1.0487 0.4759 0.6935 0.054 Uiso 1 1 calc R . . H27B H 1.0430 0.5568 0.6577 0.054 Uiso 1 1 calc R . . H27C H 1.0588 0.4823 0.6214 0.054 Uiso 1 1 calc R . . Cl1 Cl 0.03333(5) 0.32449(6) 0.79659(4) 0.02211(14) Uani 1 1 d . . . O1 O 0.13009(19) 0.3941(2) 0.79131(16) 0.0360(7) Uani 1 1 d . . . O2 O 0.0172(3) 0.2754(3) 0.85268(16) 0.0464(8) Uani 1 1 d . . . O3 O 0.0060(2) 0.2603(2) 0.74672(16) 0.0418(7) Uani 1 1 d . . . O4 O -0.02195(18) 0.3709(2) 0.79573(12) 0.0264(5) Uani 1 1 d . . . Cl2 Cl 0.68706(5) 0.12177(6) 0.78767(4) 0.02554(16) Uani 1 1 d . . . O21 O 0.6314(3) 0.1607(4) 0.8036(2) 0.0635(13) Uani 1 1 d . . . O22 O 0.6599(4) 0.0359(3) 0.8202(3) 0.0848(17) Uani 1 1 d . . . O23 O 0.7821(2) 0.1865(3) 0.80095(19) 0.0501(9) Uani 1 1 d . . . O24 O 0.6809(3) 0.1042(3) 0.72440(18) 0.0543(10) Uani 1 1 d . . . C1S C 0.3215(6) 0.2423(7) 0.9726(5) 0.099(4) Uani 1 1 d . . . H1SB H 0.3900 0.2752 0.9677 0.119 Uiso 1 1 calc R . . H1SC H 0.3060 0.2572 1.0129 0.119 Uiso 1 1 calc R . . C2S C 0.2804(5) 0.1410(6) 0.9645(3) 0.0606(14) Uani 1 1 d . . . H2S1 H 0.2123 0.1111 0.9657 0.091 Uiso 1 1 calc R . . H2S2 H 0.3017 0.1160 0.9970 0.091 Uiso 1 1 calc R . . H2S3 H 0.2997 0.1286 0.9253 0.091 Uiso 1 1 calc R . . O1S O 0.2747(5) 0.2677(5) 0.9212(3) 0.0853(16) Uani 1 1 d . . . H1S H 0.3054 0.2773 0.8891 0.128 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 Fe1 0.0138(2) 0.0138(2) 0.0209(3) 0.000 0.000 0.00689(10) N1 0.0256(14) 0.0256(14) 0.0122(18) 0.000 0.000 0.0128(7) N2 0.0142(12) 0.0166(12) 0.0261(13) 0.0051(10) 0.0015(10) 0.0070(10) N3 0.0152(12) 0.0168(12) 0.0250(13) 0.0009(10) -0.0001(9) 0.0079(10) N4 0.0191(12) 0.0189(12) 0.0188(11) -0.0004(9) -0.0001(9) 0.0075(11) C1 0.0261(16) 0.0280(16) 0.0167(13) 0.0048(11) 0.0017(11) 0.0136(13) C2 0.0274(16) 0.0251(16) 0.0244(15) 0.0015(12) -0.0048(12) 0.0172(14) C3 0.0214(14) 0.0180(14) 0.0268(16) 0.0018(11) 0.0025(11) 0.0107(12) C4 0.0153(13) 0.0146(13) 0.0264(14) 0.0007(10) 0.0024(10) 0.0049(10) C5 0.0177(14) 0.0154(14) 0.0237(14) -0.0012(11) 0.0026(11) 0.0057(12) C6 0.0213(14) 0.0200(14) 0.0212(14) -0.0017(11) 0.0005(11) 0.0105(12) C7 0.0319(19) 0.0137(14) 0.0342(16) -0.0027(12) -0.0018(13) 0.0059(13) Fe2 0.0140(2) 0.0140(2) 0.0229(3) 0.000 0.000 0.00699(10) N21 0.0142(12) 0.0142(12) 0.028(2) 0.000 0.000 0.0071(6) N22 0.0185(12) 0.0171(12) 0.0243(13) -0.0036(9) 0.0003(9) 0.0085(9) N23 0.0349(18) 0.053(2) 0.0280(15) -0.0109(14) -0.0080(13) 0.0308(18) N24 0.0210(14) 0.0273(14) 0.0253(13) -0.0041(11) -0.0025(11) 0.0139(12) C21 0.0191(14) 0.0202(14) 0.0242(14) 0.0026(11) 0.0044(11) 0.0088(12) C22 0.0157(14) 0.0157(13) 0.0309(15) 0.0028(12) 0.0039(11) 0.0029(11) C23 0.0193(15) 0.0219(15) 0.0291(16) -0.0068(12) -0.0021(12) 0.0083(13) C24 0.0134(13) 0.0306(18) 0.0325(15) -0.0096(14) -0.0070(11) 0.0109(14) C25 0.0253(18) 0.051(2) 0.0313(18) -0.0201(17) -0.0112(14) 0.0250(18) C26 0.0294(18) 0.035(2) 0.0312(17) -0.0020(14) -0.0041(14) 0.0219(16) C27 0.024(2) 0.062(3) 0.044(2) -0.018(2) -0.0154(17) 0.018(2) Cl1 0.0172(3) 0.0175(3) 0.0297(3) -0.0025(3) -0.0013(3) 0.0072(3) O1 0.0149(12) 0.0274(14) 0.0587(19) -0.0030(13) -0.0022(11) 0.0051(10) O2 0.050(2) 0.0438(19) 0.0513(19) 0.0164(15) 0.0064(15) 0.0274(17) O3 0.0336(15) 0.0317(15) 0.0574(19) -0.0217(13) -0.0091(14) 0.0143(13) O4 0.0222(12) 0.0304(13) 0.0308(12) -0.0025(10) -0.0015(9) 0.0164(11) Cl2 0.0166(3) 0.0246(4) 0.0315(4) -0.0039(3) 0.0003(3) 0.0073(3) O21 0.0405(18) 0.084(3) 0.084(3) -0.040(2) -0.0075(19) 0.045(2) O22 0.066(3) 0.038(2) 0.123(5) 0.034(3) 0.021(3) 0.005(2) O23 0.0196(14) 0.049(2) 0.073(2) -0.0278(17) -0.0088(14) 0.0112(14) O24 0.049(2) 0.072(3) 0.060(2) -0.0157(19) -0.0101(16) 0.043(2) C1S 0.065(5) 0.078(5) 0.125(8) -0.042(5) 0.034(5) 0.014(4) C2S 0.064(3) 0.061(4) 0.050(3) -0.006(3) 0.005(2) 0.026(3) O1S 0.092(4) 0.091(4) 0.093(4) 0.025(3) 0.023(3) 0.061(4) _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 Fe1 N2 2.106(3) 3_675 ? Fe1 N2 2.106(3) 2_765 ? Fe1 N2 2.106(3) . ? Fe1 N3 2.163(3) 3_675 ? Fe1 N3 2.163(3) . ? Fe1 N3 2.163(3) 2_765 ? N1 C1 1.476(4) 3_675 ? N1 C1 1.476(4) 2_765 ? N1 C1 1.476(4) . ? N2 C3 1.278(5) . ? N2 C2 1.471(4) . ? N3 C6 1.311(4) . ? N3 C4 1.383(4) . ? N4 C6 1.348(4) . ? N4 C5 1.361(4) . ? N4 H4A 0.8800 . ? C1 C2 1.504(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.436(5) . ? C3 H3A 0.9500 . ? C4 C5 1.388(4) . ? C5 C7 1.481(4) . ? C6 H6A 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? Fe2 N22 2.111(3) 2_655 ? Fe2 N22 2.111(3) 3_665 ? Fe2 N22 2.111(3) . ? Fe2 N24 2.141(3) 3_665 ? Fe2 N24 2.141(3) 2_655 ? Fe2 N24 2.141(3) . ? N21 C21 1.474(4) 3_665 ? N21 C21 1.474(4) . ? N21 C21 1.474(4) 2_655 ? N22 C23 1.297(4) . ? N22 C22 1.464(4) . ? N23 C26 1.345(5) . ? N23 C25 1.352(6) . ? N23 H23A 0.8800 . ? N24 C26 1.317(5) . ? N24 C24 1.389(5) . ? C21 C22 1.520(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.416(5) . ? C23 H23B 0.9500 . ? C24 C25 1.386(5) . ? C25 C27 1.487(6) . ? C26 H26A 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? Cl1 O2 1.432(3) . ? Cl1 O1 1.438(3) . ? Cl1 O3 1.439(3) . ? Cl1 O4 1.462(3) . ? Cl2 O21 1.410(3) . ? Cl2 O24 1.420(4) . ? Cl2 O23 1.424(3) . ? Cl2 O22 1.450(5) . ? C1S C2S 1.474(12) . ? C1S O1S 1.548(15) . ? C1S H1SB 0.9900 . ? C1S H1SC 0.9900 . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? O1S H1S 0.8400 . ? 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 N2 Fe1 N2 108.98(9) 3_675 2_765 ? N2 Fe1 N2 108.98(9) 3_675 . ? N2 Fe1 N2 108.98(9) 2_765 . ? N2 Fe1 N3 75.92(11) 3_675 3_675 ? N2 Fe1 N3 89.55(10) 2_765 3_675 ? N2 Fe1 N3 157.09(12) . 3_675 ? N2 Fe1 N3 89.55(10) 3_675 . ? N2 Fe1 N3 157.09(12) 2_765 . ? N2 Fe1 N3 75.93(11) . . ? N3 Fe1 N3 81.83(12) 3_675 . ? N2 Fe1 N3 157.09(11) 3_675 2_765 ? N2 Fe1 N3 75.92(11) 2_765 2_765 ? N2 Fe1 N3 89.55(10) . 2_765 ? N3 Fe1 N3 81.83(12) 3_675 2_765 ? N3 Fe1 N3 81.83(12) . 2_765 ? C1 N1 C1 111.53(19) 3_675 2_765 ? C1 N1 C1 111.53(19) 3_675 . ? C1 N1 C1 111.53(19) 2_765 . ? C3 N2 C2 121.1(3) . . ? C3 N2 Fe1 118.3(2) . . ? C2 N2 Fe1 120.5(2) . . ? C6 N3 C4 105.7(3) . . ? C6 N3 Fe1 141.2(2) . . ? C4 N3 Fe1 111.9(2) . . ? C6 N4 C5 109.5(3) . . ? C6 N4 H4A 125.2 . . ? C5 N4 H4A 125.2 . . ? N1 C1 C2 109.8(3) . . ? N1 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? N1 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? N2 C2 C1 106.4(3) . . ? N2 C2 H2A 110.4 . . ? C1 C2 H2A 110.4 . . ? N2 C2 H2B 110.4 . . ? C1 C2 H2B 110.4 . . ? H2A C2 H2B 108.6 . . ? N2 C3 C4 116.3(3) . . ? N2 C3 H3A 121.8 . . ? C4 C3 H3A 121.8 . . ? N3 C4 C5 110.0(3) . . ? N3 C4 C3 116.6(3) . . ? C5 C4 C3 133.3(3) . . ? N4 C5 C4 103.9(3) . . ? N4 C5 C7 124.7(3) . . ? C4 C5 C7 131.4(3) . . ? N3 C6 N4 110.8(3) . . ? N3 C6 H6A 124.6 . . ? N4 C6 H6A 124.6 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N22 Fe2 N22 106.68(9) 2_655 3_665 ? N22 Fe2 N22 106.68(9) 2_655 . ? N22 Fe2 N22 106.68(9) 3_665 . ? N22 Fe2 N24 91.90(11) 2_655 3_665 ? N22 Fe2 N24 75.83(12) 3_665 3_665 ? N22 Fe2 N24 159.18(12) . 3_665 ? N22 Fe2 N24 75.82(12) 2_655 2_655 ? N22 Fe2 N24 159.18(12) 3_665 2_655 ? N22 Fe2 N24 91.90(11) . 2_655 ? N24 Fe2 N24 83.47(12) 3_665 2_655 ? N22 Fe2 N24 159.17(12) 2_655 . ? N22 Fe2 N24 91.91(11) 3_665 . ? N22 Fe2 N24 75.83(12) . . ? N24 Fe2 N24 83.47(12) 3_665 . ? N24 Fe2 N24 83.47(12) 2_655 . ? C21 N21 C21 112.4(2) 3_665 . ? C21 N21 C21 112.4(2) 3_665 2_655 ? C21 N21 C21 112.4(2) . 2_655 ? C23 N22 C22 120.4(3) . . ? C23 N22 Fe2 117.9(2) . . ? C22 N22 Fe2 121.4(2) . . ? C26 N23 C25 109.2(3) . . ? C26 N23 H23A 125.4 . . ? C25 N23 H23A 125.4 . . ? C26 N24 C24 106.3(3) . . ? C26 N24 Fe2 140.2(3) . . ? C24 N24 Fe2 113.4(2) . . ? N21 C21 C22 108.9(3) . . ? N21 C21 H21A 109.9 . . ? C22 C21 H21A 109.9 . . ? N21 C21 H21B 109.9 . . ? C22 C21 H21B 109.9 . . ? H21A C21 H21B 108.3 . . ? N22 C22 C21 106.8(3) . . ? N22 C22 H22A 110.4 . . ? C21 C22 H22A 110.4 . . ? N22 C22 H22B 110.4 . . ? C21 C22 H22B 110.4 . . ? H22A C22 H22B 108.6 . . ? N22 C23 C24 116.5(3) . . ? N22 C23 H23B 121.7 . . ? C24 C23 H23B 121.7 . . ? C25 C24 N24 108.4(4) . . ? C25 C24 C23 135.2(4) . . ? N24 C24 C23 116.3(3) . . ? N23 C25 C24 105.5(4) . . ? N23 C25 C27 121.6(4) . . ? C24 C25 C27 132.9(5) . . ? N24 C26 N23 110.5(4) . . ? N24 C26 H26A 124.8 . . ? N23 C26 H26A 124.8 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O2 Cl1 O1 110.1(2) . . ? O2 Cl1 O3 109.9(2) . . ? O1 Cl1 O3 110.1(2) . . ? O2 Cl1 O4 108.8(2) . . ? O1 Cl1 O4 108.51(17) . . ? O3 Cl1 O4 109.36(18) . . ? O21 Cl2 O24 110.0(3) . . ? O21 Cl2 O23 109.6(2) . . ? O24 Cl2 O23 107.2(2) . . ? O21 Cl2 O22 111.9(3) . . ? O24 Cl2 O22 109.3(3) . . ? O23 Cl2 O22 108.7(3) . . ? C2S C1S O1S 102.2(7) . . ? C2S C1S H1SB 111.3 . . ? O1S C1S H1SB 111.3 . . ? C2S C1S H1SC 111.3 . . ? O1S C1S H1SC 111.3 . . ? H1SB C1S H1SC 109.2 . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? C1S O1S H1S 109.5 . . ? 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 _geom_hbond_publ_flag N4 H4A O4 0.880 2.087 2.869 147.49 9_554 ? N4 H4A O23 0.880 2.500 3.099 125.88 9_664 ? N23 H23A O4 0.880 1.992 2.837 160.65 1_655 ? N23 H23A CL1 0.880 2.980 3.800 155.93 1_655 ? O1S H1S O22 0.840 1.884 2.687 159.50 3_665 ? O1S H1S CL2 0.840 2.948 3.781 171.70 3_665 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.342 _refine_diff_density_min -0.380 _refine_diff_density_rms 0.091 _chemical_compound_source synthesized #===END data_1215 _database_code_depnum_ccdc_archive 'CCDC 270795' _audit_creation_method 'SHELXL-97 & ZCIF' _chemical_name_systematic ; Fe(3+) . NL3(3-)H(1+) . I3(1-)1-x . I(1-)x . nH2O x=0.475, n=2.625 ; _chemical_name_common ;Fe(3+) . NL3(3-)H(1+) . I3(1-)1-x . I(1-)x . nH2O x=0.475, n=2.625 ; _chemical_melting_point ? _chemical_formula_moiety '(C21 H28 N10 Fe), 0.525(I3), 0.475(I), 2.625(H2 O)' _chemical_formula_sum 'C21 H33.25 Fe I2.05 N10 O2.625' _chemical_formula_weight 783.82 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'F -4 3 c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+1/2, -y+1/2' 'z+1/2, y+1/2, x+1/2' 'z+1/2, -y+1/2, -x+1/2' '-z+1/2, y+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x+1/2, y+1/2' 'z, -x+1/2, -y+1/2' '-z, -x+1/2, y+1/2' '-z, x+1/2, -y+1/2' 'y, z+1/2, x+1/2' '-y, z+1/2, -x+1/2' 'y, -z+1/2, -x+1/2' '-y, -z+1/2, x+1/2' 'y+1/2, x+1, z+1' '-y+1/2, -x+1, z+1' 'y+1/2, -x+1, -z+1' '-y+1/2, x+1, -z+1' 'x+1/2, z+1, y+1' '-x+1/2, z+1, -y+1' '-x+1/2, -z+1, y+1' 'x+1/2, -z+1, -y+1' 'z+1/2, y+1, x+1' 'z+1/2, -y+1, -x+1' '-z+1/2, y+1, -x+1' '-z+1/2, -y+1, x+1' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+1/2, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'z+1/2, x, y+1/2' 'z+1/2, -x, -y+1/2' '-z+1/2, -x, y+1/2' '-z+1/2, x, -y+1/2' 'y+1/2, z, x+1/2' '-y+1/2, z, -x+1/2' 'y+1/2, -z, -x+1/2' '-y+1/2, -z, x+1/2' 'y+1, x+1/2, z+1' '-y+1, -x+1/2, z+1' 'y+1, -x+1/2, -z+1' '-y+1, x+1/2, -z+1' 'x+1, z+1/2, y+1' '-x+1, z+1/2, -y+1' '-x+1, -z+1/2, y+1' 'x+1, -z+1/2, -y+1' 'z+1, y+1/2, x+1' 'z+1, -y+1/2, -x+1' '-z+1, y+1/2, -x+1' '-z+1, -y+1/2, x+1' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'z+1/2, x+1/2, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x+1/2, y' '-z+1/2, x+1/2, -y' 'y+1/2, z+1/2, x' '-y+1/2, z+1/2, -x' 'y+1/2, -z+1/2, -x' '-y+1/2, -z+1/2, x' 'y+1, x+1, z+1/2' '-y+1, -x+1, z+1/2' 'y+1, -x+1, -z+1/2' '-y+1, x+1, -z+1/2' 'x+1, z+1, y+1/2' '-x+1, z+1, -y+1/2' '-x+1, -z+1, y+1/2' 'x+1, -z+1, -y+1/2' 'z+1, y+1, x+1/2' 'z+1, -y+1, -x+1/2' '-z+1, y+1, -x+1/2' '-z+1, -y+1, x+1/2' _cell_length_a 29.6863(3) _cell_length_b 29.6863(3) _cell_length_c 29.6863(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 26161.8(5) _cell_formula_units_Z 32 _cell_measurement_temperature 233(2) _cell_measurement_reflns_used 9240 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 28.3 _exptl_crystal_description pyramid _exptl_crystal_colour black _exptl_crystal_size_max 0.370 _exptl_crystal_size_mid 0.290 _exptl_crystal_size_min 0.260 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 12317 _exptl_absorpt_coefficient_mu 2.432 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.352 _exptl_absorpt_correction_T_max 0.531 _exptl_absorpt_process_details 'XPREP (Sheldrick, 1997)' _diffrn_ambient_temperature 233(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 'three-circle diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_decay_% 0.16 _diffrn_reflns_number 54720 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0113 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2516 _reflns_number_gt 1927 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Platon (Spek, 1990)' _computing_publication_material SHELXL-97 _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 'w=1/[\s^2^(Fo^2^)+(0.067P)^2^+243.5P], P=(max(Fo^2^,0)+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_extinction_method none _refine_ls_abs_structure_details '(Flack, 1983)' _refine_ls_abs_structure_Flack -0.01(5) _refine_ls_number_reflns 2516 # 1337 w/o Fiedel pairs _refine_ls_number_parameters 132 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0678 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1512 _refine_ls_wR_factor_gt 0.1283 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.000 _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 I1 I 0.0000 0.2500 0.5000 0.0600(4) Uani 0.633(2) 4 d SP . . I2 I 0.20550(3) 0.20550(3) 0.29450(3) 0.0829(5) Uani 0.5251(18) 3 d SP . . I3 I 0.15087(3) 0.15087(3) 0.34913(3) 0.0741(4) Uani 0.5251(18) 3 d SP . . I4 I 0.0875(3) 0.1001(2) 0.4086(3) 0.106(2) Uani 0.1750(6) 1 d PU . . Fe1 Fe 0.37297(2) 0.12703(2) 0.37297(2) 0.0412(3) Uani 1 3 d S . . N1 N 0.43393(16) 0.06607(16) 0.43393(16) 0.070(2) Uani 1 3 d S . . C2 C 0.3998(3) 0.0500(3) 0.4644(2) 0.0786(19) Uani 1 1 d . . . H21A H 0.4124 0.0476 0.4948 0.094 Uiso 1 1 calc R . . H22B H 0.3899 0.0199 0.4551 0.094 Uiso 1 1 calc R . . C3 C 0.3593(2) 0.0820(2) 0.46494(19) 0.0632(15) Uani 1 1 d . . . H31A H 0.3351 0.0694 0.4835 0.076 Uiso 1 1 calc R . . H32B H 0.3681 0.1112 0.4777 0.076 Uiso 1 1 calc R . . N4 N 0.34363(15) 0.08789(16) 0.41820(15) 0.0502(10) Uani 1 1 d . . . C5 C 0.3080(2) 0.06802(19) 0.40484(19) 0.0559(13) Uani 1 1 d . . . H51 H 0.2909 0.0497 0.4242 0.067 Uiso 1 1 calc R . . C6 C 0.29527(19) 0.07504(19) 0.35914(18) 0.0545(12) Uani 1 1 d . . . N7 N 0.32404(15) 0.10363(15) 0.33667(14) 0.0495(10) Uani 1 1 d . . . C8 C 0.3086(2) 0.1053(2) 0.29509(18) 0.0553(13) Uani 1 1 d . . . H81 H 0.3220 0.1224 0.2720 0.066 Uiso 1 1 calc R . . N9 N 0.27207(18) 0.07993(18) 0.28948(17) 0.0631(12) Uani 1 1 d . . . H91 H 0.2569 0.0766 0.2647 0.076 Uiso 0.33 1 calc PR . . C10 C 0.2628(2) 0.0599(2) 0.3303(2) 0.0610(14) Uani 1 1 d . . . C11 C 0.2240(3) 0.0287(3) 0.3377(3) 0.088(2) Uani 1 1 d . . . H111 H 0.1960 0.0455 0.3360 0.132 Uiso 1 1 calc R . . H112 H 0.2265 0.0149 0.3672 0.132 Uiso 1 1 calc R . . H113 H 0.2241 0.0054 0.3148 0.132 Uiso 1 1 calc R . . O1W O 0.05683(19) 0.18869(19) 0.4081(2) 0.086(2) Uani 0.875(15) 1 d PD . . H1W H 0.0466(19) 0.1633(11) 0.417(3) 0.103 Uiso 0.875(15) 1 d PD . . H2W H 0.0339(12) 0.2052(17) 0.404(3) 0.103 Uiso 0.875(15) 1 d PD . . 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 I1 0.0613(5) 0.0575(7) 0.0613(5) 0.000 0.000 0.000 I2 0.0829(5) 0.0829(5) 0.0829(5) 0.0038(5) 0.0038(5) -0.0038(5) I3 0.0741(4) 0.0741(4) 0.0741(4) -0.0028(4) -0.0028(4) 0.0028(4) I4 0.112(5) 0.133(5) 0.074(3) -0.002(3) -0.004(3) -0.038(4) Fe1 0.0412(3) 0.0412(3) 0.0412(3) 0.0053(2) -0.0053(2) 0.0053(2) N1 0.070(2) 0.070(2) 0.070(2) 0.018(2) -0.018(2) 0.018(2) C2 0.096(5) 0.078(4) 0.061(3) 0.026(3) -0.020(3) 0.014(4) C3 0.065(3) 0.082(4) 0.042(3) 0.011(3) -0.005(2) 0.001(3) N4 0.050(2) 0.058(3) 0.044(2) 0.0092(18) -0.0015(18) -0.0027(19) C5 0.059(3) 0.056(3) 0.053(3) 0.003(2) 0.003(3) -0.006(3) C6 0.052(3) 0.060(3) 0.051(3) 0.003(2) -0.006(2) -0.004(2) N7 0.048(2) 0.051(2) 0.049(2) 0.0064(18) -0.0096(18) 0.0019(18) C8 0.064(3) 0.055(3) 0.046(3) 0.001(2) -0.012(2) 0.003(2) N9 0.066(3) 0.064(3) 0.060(3) -0.003(2) -0.018(2) 0.000(2) C10 0.055(3) 0.064(3) 0.064(3) -0.008(3) -0.012(3) 0.001(3) C11 0.075(4) 0.089(5) 0.099(6) -0.012(4) -0.006(4) -0.025(4) O1W 0.069(3) 0.071(4) 0.117(6) 0.003(3) -0.037(3) 0.004(3) _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 I2 I3 2.809(2) . ? I3 I4 2.986(3) . ? Fe1 N7 1.937(4) 84 ? Fe1 N7 1.937(4) 30 ? Fe1 N7 1.937(4) . ? Fe1 N4 1.978(4) 84 ? Fe1 N4 1.978(4) . ? Fe1 N4 1.978(4) 30 ? N1 C2 1.441(8) 84 ? N1 C2 1.441(8) . ? N1 C2 1.441(8) 30 ? C2 C3 1.532(9) . ? C2 H21A 0.9800 . ? C2 H22B 0.9800 . ? C3 N4 1.474(7) . ? C3 H31A 0.9800 . ? C3 H32B 0.9800 . ? N4 C5 1.276(7) . ? C5 C6 1.423(8) . ? C5 H51 0.9400 . ? C6 C10 1.365(8) . ? C6 N7 1.376(7) . ? N7 C8 1.317(7) . ? C8 N9 1.331(8) . ? C8 H81 0.9400 . ? N9 C10 1.377(8) . ? N9 H91 0.8700 . ? C10 C11 1.495(9) . ? C11 H111 0.9700 . ? C11 H112 0.9700 . ? C11 H113 0.9700 . ? O1W H1W 0.851(10) . ? O1W H2W 0.849(10) . ? 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 I2 I3 I4 174.79(16) . . ? N7 Fe1 N7 92.94(18) 84 30 ? N7 Fe1 N7 92.94(18) 84 . ? N7 Fe1 N7 92.94(18) 30 . ? N7 Fe1 N4 80.61(18) 84 84 ? N7 Fe1 N4 173.5(2) 30 84 ? N7 Fe1 N4 87.25(19) . 84 ? N7 Fe1 N4 173.54(19) 84 . ? N7 Fe1 N4 87.25(19) 30 . ? N7 Fe1 N4 80.61(18) . . ? N4 Fe1 N4 99.14(16) 84 . ? N7 Fe1 N4 87.25(19) 84 30 ? N7 Fe1 N4 80.61(18) 30 30 ? N7 Fe1 N4 173.54(19) . 30 ? N4 Fe1 N4 99.14(16) 84 30 ? N4 Fe1 N4 99.14(16) . 30 ? C2 N1 C2 117.9(2) 84 . ? C2 N1 C2 117.9(2) 84 30 ? C2 N1 C2 117.9(2) . 30 ? N1 C2 C3 110.7(6) . . ? N1 C2 H21A 109.5 . . ? C3 C2 H21A 109.5 . . ? N1 C2 H22B 109.5 . . ? C3 C2 H22B 109.5 . . ? H21A C2 H22B 108.1 . . ? N4 C3 C2 108.2(5) . . ? N4 C3 H31A 110.1 . . ? C2 C3 H31A 110.1 . . ? N4 C3 H32B 110.1 . . ? C2 C3 H32B 110.1 . . ? H31A C3 H32B 108.4 . . ? C5 N4 C3 120.0(5) . . ? C5 N4 Fe1 115.2(4) . . ? C3 N4 Fe1 124.7(4) . . ? N4 C5 C6 116.6(5) . . ? N4 C5 H51 121.7 . . ? C6 C5 H51 121.7 . . ? C10 C6 N7 109.7(5) . . ? C10 C6 C5 137.4(5) . . ? N7 C6 C5 112.8(5) . . ? C8 N7 C6 105.2(5) . . ? C8 N7 Fe1 140.2(4) . . ? C6 N7 Fe1 114.6(3) . . ? N7 C8 N9 112.3(5) . . ? N7 C8 H81 123.9 . . ? N9 C8 H81 123.9 . . ? C8 N9 C10 107.3(5) . . ? C8 N9 H91 126.4 . . ? C10 N9 H91 126.4 . . ? C6 C10 N9 105.6(5) . . ? C6 C10 C11 131.0(6) . . ? N9 C10 C11 123.4(6) . . ? C10 C11 H111 109.5 . . ? C10 C11 H112 109.5 . . ? H111 C11 H112 109.5 . . ? C10 C11 H113 109.5 . . ? H111 C11 H113 109.5 . . ? H112 C11 H113 109.5 . . ? H1W O1W H2W 106(2) . . ? 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 C2 N1 C2 C3 -126.5(8) 84 . . . ? C2 N1 C2 C3 82.2(9) 30 . . . ? N1 C2 C3 N4 54.3(7) . . . . ? C2 C3 N4 C5 104.5(7) . . . . ? C2 C3 N4 Fe1 -77.8(6) . . . . ? N7 Fe1 N4 C5 -1(2) 84 . . . ? N7 Fe1 N4 C5 91.1(4) 30 . . . ? N7 Fe1 N4 C5 -2.4(4) . . . . ? N4 Fe1 N4 C5 -88.0(5) 84 . . . ? N4 Fe1 N4 C5 171.1(4) 30 . . . ? N7 Fe1 N4 C3 -179(100) 84 . . . ? N7 Fe1 N4 C3 -86.8(5) 30 . . . ? N7 Fe1 N4 C3 179.8(5) . . . . ? N4 Fe1 N4 C3 94.1(4) 84 . . . ? N4 Fe1 N4 C3 -6.8(5) 30 . . . ? C3 N4 C5 C6 -179.4(5) . . . . ? Fe1 N4 C5 C6 2.6(7) . . . . ? N4 C5 C6 C10 175.9(7) . . . . ? N4 C5 C6 N7 -1.2(8) . . . . ? C10 C6 N7 C8 0.0(7) . . . . ? C5 C6 N7 C8 177.9(5) . . . . ? C10 C6 N7 Fe1 -178.7(4) . . . . ? C5 C6 N7 Fe1 -0.8(6) . . . . ? N7 Fe1 N7 C8 3.7(7) 84 . . . ? N7 Fe1 N7 C8 96.8(5) 30 . . . ? N4 Fe1 N7 C8 -76.7(6) 84 . . . ? N4 Fe1 N7 C8 -176.5(6) . . . . ? N4 Fe1 N7 C8 95.2(18) 30 . . . ? N7 Fe1 N7 C6 -178.2(4) 84 . . . ? N7 Fe1 N7 C6 -85.1(5) 30 . . . ? N4 Fe1 N7 C6 101.4(4) 84 . . . ? N4 Fe1 N7 C6 1.7(4) . . . . ? N4 Fe1 N7 C6 -86.7(18) 30 . . . ? C6 N7 C8 N9 0.2(7) . . . . ? Fe1 N7 C8 N9 178.4(5) . . . . ? N7 C8 N9 C10 -0.4(7) . . . . ? N7 C6 C10 N9 -0.2(7) . . . . ? C5 C6 C10 N9 -177.4(7) . . . . ? N7 C6 C10 C11 -179.8(7) . . . . ? C5 C6 C10 C11 3.1(13) . . . . ? C8 N9 C10 C6 0.4(7) . . . . ? C8 N9 C10 C11 179.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.790 _refine_diff_density_min -0.583 _refine_diff_density_rms 0.079 _exptl_crystal_id 'Greg Brawer DZ3' _diffrn_measurement_total_frames-CCD 1868 _diffrn_measurement_details NFRAMES=606,606,606,50 _diffrn_measurement_frame_width-CCD 0.3 _diffrn_detector_distance-CCD 4.890 _diffrn_source_voltage 50 _diffrn_source_current 40 _diffrn_measurement_frame_time-CCD 23 _diffrn_measurement_total_time-CCD 15.6 _diffrn_measurement_frame_size-CCD 512 _chemical_absolute_configuration ad _diffrn_orient_matrix_type standard _diffrn_orient_matrix_UB_11 -0.0034604 _diffrn_orient_matrix_UB_12 -0.0295793 _diffrn_orient_matrix_UB_13 -0.0157210 _diffrn_orient_matrix_UB_21 -0.0334632 _diffrn_orient_matrix_UB_22 0.0021847 _diffrn_orient_matrix_UB_23 0.0032623 _diffrn_orient_matrix_UB_31 -0.0018472 _diffrn_orient_matrix_UB_32 0.0159527 _diffrn_orient_matrix_UB_33 -0.0296138 _symmetry_space_group_name_Hall 'F -4c 2 3' _diffrn_measurement_specimen_support 'glass capillary' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker Smart1000' _reflns_Friedel_coverage 0.882 #_______________________________________________________________________________ # #===END #===END data_1232 _database_code_depnum_ccdc_archive 'CCDC 277554' _audit_creation_method 'SHELXL-97 & ZCIF' _chemical_name_systematic ; Mn-complex perchlorate ; _chemical_name_common 'Mn-complex perchlorate' _chemical_formula_moiety 'C24 H36 Mn N10, 2(Cl O4)' _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 11.8154(5) _cell_length_b 12.2056(6) _cell_length_c 12.3982(6) _cell_angle_alpha 78.863(1) _cell_angle_beta 70.789(1) _cell_angle_gamma 67.400(1) _cell_volume 1554.20(13) _cell_formula_units_Z 2 _cell_measurement_temperature 233(2) _cell_measurement_reflns_used 4886 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 29.1 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method not_measured _exptl_crystal_F_000 746 _exptl_absorpt_coefficient_mu 0.660 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.773 _exptl_absorpt_correction_T_max 0.848 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _diffrn_ambient_temperature 233(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 'three-circle diffractometer' _diffrn_measurement_method '/w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_decay_% -0.05 _diffrn_reflns_number 14610 _diffrn_reflns_av_R_equivalents 0.0206 _diffrn_reflns_av_sigmaI/netI 0.0249 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7042 _reflns_number_gt 6321 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Platon (Spek, 1990)' _computing_publication_material SHELXL-97 _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. Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 0.0580 (0.0114) x + 11.2899 (0.0045) y + 1.0935 (0.0127) z = 4.0063 (0.0059) * 0.0025 (0.0011) N12 * 0.0019 (0.0012) N13 * -0.0013 (0.0011) C15 * -0.0028 (0.0012) C16 * -0.0003 (0.0011) C17 -0.1351 (0.0036) N11 0.0045 (0.0051) C13 -0.0018 (0.0033) C14 -0.0220 (0.0038) C18 -0.3263 (0.0032) Mn1 Rms deviation of fitted atoms = 0.0020 - 7.5377 (0.0085) x + 0.4678 (0.0126) y + 5.9163 (0.0102) z = 1.0311 (0.0092) Angle to previous plane (with approximate esd) = 71.66 ( 0.09 ) * 0.0025 (0.0011) N22 * 0.0010 (0.0012) N23 * -0.0019 (0.0011) C25 * -0.0022 (0.0012) C26 * 0.0006 (0.0012) C27 -0.0980 (0.0036) N21 0.0829 (0.0051) C23 0.0300 (0.0033) C24 -0.0456 (0.0040) C28 -0.3499 (0.0033) Mn1 Rms deviation of fitted atoms = 0.0018 5.8006 (0.0108) x + 5.5803 (0.0100) y + 11.8497 (0.0035) z = 6.3201 (0.0057) Angle to previous plane (with approximate esd) = 69.14 ( 0.07 ) * 0.0020 (0.0011) N32 * 0.0000 (0.0012) N33 * -0.0020 (0.0011) C35 * -0.0013 (0.0012) C36 * 0.0013 (0.0011) C37 -0.0887 (0.0036) N31 0.0441 (0.0052) C33 0.0070 (0.0033) C34 -0.0207 (0.0039) C38 -0.2347 (0.0033) Mn1 Rms deviation of fitted atoms = 0.0015 ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.015P)^2^+1.615P], P=(max(Fo^2^,0)+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_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7042 _refine_ls_number_parameters 482 _refine_ls_number_restraints 108 _refine_ls_R_factor_all 0.0411 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0836 _refine_ls_wR_factor_gt 0.0809 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.001 _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 Mn1 Mn 0.16002(2) 0.29650(2) 0.29559(2) 0.02703(7) Uani 1 1 d . . . N1 N 0.28043(15) 0.14393(13) 0.14962(13) 0.0310(3) Uani 1 1 d . . . N11 N 0.01646(15) 0.32383(13) 0.19590(13) 0.0309(3) Uani 1 1 d . . . N12 N -0.03953(15) 0.31380(14) 0.42829(14) 0.0339(3) Uani 1 1 d . . . N13 N -0.21219(17) 0.30178(15) 0.56103(16) 0.0419(4) Uani 1 1 d . . . H13 H -0.2639 0.2958 0.6288 0.059(8) Uiso 1 1 calc R . . C11 C 0.27777(19) 0.20182(19) 0.03270(16) 0.0375(4) Uani 1 1 d . . . H11A H 0.3405 0.1452 -0.0232 0.047(6) Uiso 1 1 calc R . . H11B H 0.3058 0.2702 0.0213 0.033(5) Uiso 1 1 calc R . . C12 C 0.1498(2) 0.24490(19) 0.00607(17) 0.0389(4) Uani 1 1 d . . . H12A H 0.1638 0.2684 -0.0761 0.044(6) Uiso 1 1 calc R . . H12B H 0.1187 0.1780 0.0224 0.048(7) Uiso 1 1 calc R . . C13 C 0.0462(2) 0.34812(18) 0.07128(17) 0.0385(4) Uani 1 1 d . . . H13A H 0.0733 0.4177 0.0499 0.044(6) Uiso 1 1 calc R . . H13B H -0.0316 0.3680 0.0483 0.049(7) Uiso 1 1 calc R . . C14 C -0.09704(18) 0.33069(17) 0.25295(17) 0.0346(4) Uani 1 1 d . . . H14 H -0.1587 0.3432 0.2153 0.038(6) Uiso 1 1 calc R . . C15 C -0.12963(17) 0.31891(16) 0.37679(17) 0.0324(4) Uani 1 1 d . . . C16 C -0.0926(2) 0.30293(18) 0.53851(18) 0.0403(4) Uani 1 1 d . . . H16 H -0.0528 0.2967 0.5949 0.056(7) Uiso 1 1 calc R . . C17 C -0.23785(18) 0.31161(17) 0.45888(19) 0.0382(4) Uani 1 1 d . . . C18 C -0.3611(2) 0.3109(2) 0.4524(3) 0.0565(6) Uani 1 1 d . . . H18A H -0.3750 0.2386 0.4923 0.115(13) Uiso 1 1 calc R . . H18B H -0.3584 0.3144 0.3728 0.077(10) Uiso 1 1 calc R . . H18C H -0.4304 0.3794 0.4879 0.098(11) Uiso 1 1 calc R . . N21 N 0.20076(15) 0.11623(13) 0.40431(13) 0.0311(3) Uani 1 1 d . . . N22 N 0.23204(15) 0.31234(14) 0.44566(14) 0.0321(3) Uani 1 1 d . . . N23 N 0.32637(16) 0.33026(16) 0.56417(15) 0.0387(4) Uani 1 1 d . . . H23 H 0.3561 0.3631 0.5998 0.053(7) Uiso 1 1 calc R . . C21 C 0.2238(2) 0.04880(17) 0.17161(18) 0.0372(4) Uani 1 1 d . . . H21A H 0.2640 0.0009 0.1052 0.048(7) Uiso 1 1 calc R . . H21B H 0.1329 0.0872 0.1763 0.032(5) Uiso 1 1 calc R . . C22 C 0.2356(2) -0.03538(17) 0.27870(18) 0.0394(4) Uani 1 1 d . . . H22A H 0.2071 -0.1002 0.2764 0.051(7) Uiso 1 1 calc R . . H22B H 0.3260 -0.0706 0.2767 0.048(7) Uiso 1 1 calc R . . C23 C 0.1606(2) 0.02109(17) 0.39119(18) 0.0384(4) Uani 1 1 d . . . H23A H 0.0695 0.0538 0.3955 0.046(6) Uiso 1 1 calc R . . H23B H 0.1719 -0.0402 0.4546 0.042(6) Uiso 1 1 calc R . . C24 C 0.24750(18) 0.10478(16) 0.48640(16) 0.0327(4) Uani 1 1 d . . . H24 H 0.2646 0.0332 0.5329 0.035(5) Uiso 1 1 calc R . . C25 C 0.27392(17) 0.20409(16) 0.50683(16) 0.0307(4) Uani 1 1 d . . . C26 C 0.26616(19) 0.38524(18) 0.48257(18) 0.0381(4) Uani 1 1 d . . . H26 H 0.2507 0.4656 0.4556 0.045(6) Uiso 1 1 calc R . . C27 C 0.33266(18) 0.21396(18) 0.58131(17) 0.0358(4) Uani 1 1 d . . . C28 C 0.3976(3) 0.1258(2) 0.6632(2) 0.0551(6) Uani 1 1 d . . . H28A H 0.3842 0.0512 0.6676 0.102(12) Uiso 1 1 calc R . . H28B H 0.3623 0.1562 0.7384 0.119(14) Uiso 1 1 calc R . . H28C H 0.4884 0.1125 0.6366 0.107(12) Uiso 1 1 calc R . . N31 N 0.33940(14) 0.34430(14) 0.19759(14) 0.0318(3) Uani 1 1 d . . . N32 N 0.09585(15) 0.50544(14) 0.24858(14) 0.0323(3) Uani 1 1 d . . . N33 N 0.02632(17) 0.69614(14) 0.19264(15) 0.0384(4) Uani 1 1 d . . . H33 H -0.0268 0.7680 0.1848 0.055(7) Uiso 1 1 calc R . . C31 C 0.41647(18) 0.08619(17) 0.15127(18) 0.0374(4) Uani 1 1 d . . . H31A H 0.4553 0.0173 0.1051 0.044(6) Uiso 1 1 calc R . . H31B H 0.4173 0.0557 0.2303 0.038(6) Uiso 1 1 calc R . . C32 C 0.50134(18) 0.16165(19) 0.10853(18) 0.0402(4) Uani 1 1 d . . . H32A H 0.4949 0.1986 0.0322 0.044(6) Uiso 1 1 calc R . . H32B H 0.5902 0.1093 0.1005 0.046(6) Uiso 1 1 calc R . . C33 C 0.46964(18) 0.25901(19) 0.18520(19) 0.0398(4) Uani 1 1 d . . . H33A H 0.4788 0.2227 0.2610 0.035(5) Uiso 1 1 calc R . . H33B H 0.5305 0.3013 0.1526 0.045(6) Uiso 1 1 calc R . . C34 C 0.32536(18) 0.45232(17) 0.16167(16) 0.0326(4) Uani 1 1 d . . . H34 H 0.3969 0.4749 0.1224 0.040(6) Uiso 1 1 calc R . . C35 C 0.19794(18) 0.53994(16) 0.18202(15) 0.0302(4) Uani 1 1 d . . . C36 C -0.00516(19) 0.60180(17) 0.25237(18) 0.0376(4) Uani 1 1 d . . . H36 H -0.0892 0.6050 0.2917 0.041(6) Uiso 1 1 calc R . . C37 C 0.15612(19) 0.65889(17) 0.14675(17) 0.0348(4) Uani 1 1 d . . . C38 C 0.2247(3) 0.7391(2) 0.0735(2) 0.0542(6) Uani 1 1 d . . . H38A H 0.2165 0.7493 -0.0034 0.102(12) Uiso 1 1 calc R . . H38B H 0.3144 0.7044 0.0710 0.098(12) Uiso 1 1 calc R . . H38C H 0.1880 0.8160 0.1053 0.131(15) Uiso 1 1 calc R . . Cl1 Cl 0.13036(5) 0.97173(5) 0.78871(5) 0.04491(13) Uani 1 1 d . . . O11 O 0.0724(2) 0.8975(2) 0.87209(19) 0.0814(7) Uani 1 1 d . . . O12 O 0.0515(2) 1.0343(2) 0.71334(18) 0.0778(6) Uani 1 1 d . . . O13 O 0.1423(2) 1.05951(16) 0.84184(19) 0.0692(5) Uani 1 1 d . . . O14 O 0.2547(2) 0.90376(18) 0.72314(19) 0.0764(6) Uani 1 1 d . . . Cl2 Cl 0.54360(5) 0.59243(5) 0.21690(5) 0.04800(13) Uani 0.438(15) 1 d PDU A 1 O21 O 0.5759(12) 0.5644(9) 0.1037(5) 0.0626(18) Uani 0.438(15) 1 d PDU A 1 O22 O 0.6497(10) 0.5936(13) 0.2433(13) 0.106(3) Uani 0.438(15) 1 d PDU A 1 O23 O 0.4882(9) 0.5063(7) 0.2923(7) 0.087(2) Uani 0.438(15) 1 d PDU A 1 O24 O 0.4440(7) 0.7037(6) 0.2387(8) 0.086(2) Uani 0.438(15) 1 d PDU A 1 Cl3 Cl 0.54360(5) 0.59243(5) 0.21690(5) 0.04800(13) Uani 0.562(15) 1 d PDU A 2 O31 O 0.5956(10) 0.5373(10) 0.1133(6) 0.092(2) Uani 0.562(15) 1 d PDU A 2 O32 O 0.6456(6) 0.5647(7) 0.2641(9) 0.0682(16) Uani 0.562(15) 1 d PDU A 2 O33 O 0.4483(8) 0.5480(11) 0.2908(6) 0.109(2) Uani 0.562(15) 1 d PDU A 2 O34 O 0.4896(13) 0.7188(5) 0.1961(11) 0.135(3) Uani 0.562(15) 1 d PDU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.02616(13) 0.02622(13) 0.02982(14) 0.00075(10) -0.01045(10) -0.00945(10) N1 0.0309(8) 0.0287(7) 0.0326(8) -0.0032(6) -0.0115(6) -0.0067(6) N11 0.0308(8) 0.0287(7) 0.0340(8) -0.0015(6) -0.0132(6) -0.0079(6) N12 0.0303(8) 0.0333(8) 0.0380(9) -0.0025(7) -0.0106(7) -0.0103(6) N13 0.0395(9) 0.0352(9) 0.0415(10) -0.0015(7) -0.0006(8) -0.0127(7) C11 0.0375(10) 0.0412(11) 0.0302(9) -0.0044(8) -0.0098(8) -0.0089(8) C12 0.0453(11) 0.0443(11) 0.0294(9) -0.0009(8) -0.0162(8) -0.0141(9) C13 0.0393(10) 0.0396(10) 0.0358(10) 0.0033(8) -0.0187(8) -0.0090(8) C14 0.0297(9) 0.0321(9) 0.0448(11) -0.0055(8) -0.0163(8) -0.0077(7) C15 0.0275(9) 0.0266(8) 0.0432(10) -0.0042(7) -0.0106(8) -0.0083(7) C16 0.0395(11) 0.0394(11) 0.0387(11) -0.0025(8) -0.0107(9) -0.0105(9) C17 0.0300(9) 0.0291(9) 0.0526(12) -0.0070(8) -0.0059(8) -0.0100(7) C18 0.0323(11) 0.0606(15) 0.0766(18) -0.0127(13) -0.0054(11) -0.0208(11) N21 0.0354(8) 0.0276(7) 0.0320(8) -0.0007(6) -0.0118(6) -0.0114(6) N22 0.0318(8) 0.0306(8) 0.0355(8) -0.0009(6) -0.0131(6) -0.0103(6) N23 0.0340(8) 0.0463(10) 0.0439(9) -0.0087(8) -0.0132(7) -0.0180(7) C21 0.0445(11) 0.0309(9) 0.0405(11) -0.0060(8) -0.0174(9) -0.0114(8) C22 0.0493(12) 0.0260(9) 0.0478(12) -0.0025(8) -0.0206(10) -0.0127(8) C23 0.0500(12) 0.0316(9) 0.0412(11) 0.0025(8) -0.0176(9) -0.0207(9) C24 0.0347(9) 0.0285(9) 0.0334(9) 0.0016(7) -0.0131(8) -0.0083(7) C25 0.0288(9) 0.0322(9) 0.0304(9) -0.0008(7) -0.0103(7) -0.0090(7) C26 0.0362(10) 0.0349(10) 0.0458(11) -0.0048(8) -0.0123(9) -0.0137(8) C27 0.0295(9) 0.0434(11) 0.0367(10) -0.0020(8) -0.0128(8) -0.0125(8) C28 0.0566(15) 0.0650(16) 0.0574(15) 0.0115(12) -0.0377(12) -0.0249(12) N31 0.0268(7) 0.0334(8) 0.0350(8) -0.0039(6) -0.0082(6) -0.0098(6) N32 0.0300(8) 0.0299(8) 0.0369(8) -0.0017(6) -0.0079(6) -0.0119(6) N33 0.0415(9) 0.0284(8) 0.0462(10) -0.0022(7) -0.0192(8) -0.0076(7) C31 0.0311(9) 0.0329(9) 0.0413(11) -0.0078(8) -0.0110(8) -0.0007(8) C32 0.0261(9) 0.0435(11) 0.0425(11) -0.0083(9) -0.0066(8) -0.0030(8) C33 0.0268(9) 0.0423(11) 0.0482(12) -0.0057(9) -0.0110(8) -0.0082(8) C34 0.0309(9) 0.0385(10) 0.0313(9) -0.0025(7) -0.0067(7) -0.0169(8) C35 0.0338(9) 0.0301(9) 0.0300(9) -0.0009(7) -0.0096(7) -0.0148(7) C36 0.0331(10) 0.0358(10) 0.0431(11) -0.0039(8) -0.0098(8) -0.0115(8) C37 0.0432(10) 0.0324(9) 0.0343(10) 0.0009(7) -0.0156(8) -0.0167(8) C38 0.0669(16) 0.0443(13) 0.0582(15) 0.0152(11) -0.0225(12) -0.0316(12) Cl1 0.0512(3) 0.0394(3) 0.0496(3) -0.0022(2) -0.0189(2) -0.0181(2) O11 0.1005(17) 0.0881(15) 0.0798(14) 0.0296(12) -0.0391(13) -0.0638(14) O12 0.0701(13) 0.0977(16) 0.0719(13) 0.0153(12) -0.0395(11) -0.0297(12) O13 0.0738(13) 0.0519(10) 0.0935(15) -0.0217(10) -0.0320(11) -0.0196(9) O14 0.0689(13) 0.0574(11) 0.0864(15) -0.0231(10) -0.0175(11) 0.0002(10) Cl2 0.0482(3) 0.0535(3) 0.0420(3) -0.0126(2) -0.0161(2) -0.0101(2) O21 0.084(5) 0.084(4) 0.0343(17) -0.001(2) -0.017(2) -0.046(3) O22 0.086(4) 0.130(8) 0.132(7) -0.061(6) -0.063(5) -0.017(3) O23 0.105(5) 0.075(3) 0.054(3) 0.020(3) -0.009(3) -0.024(3) O24 0.060(3) 0.064(2) 0.082(4) 0.003(2) 0.012(3) 0.001(2) Cl3 0.0482(3) 0.0535(3) 0.0420(3) -0.0126(2) -0.0161(2) -0.0101(2) O31 0.082(4) 0.134(5) 0.067(3) -0.059(4) 0.009(2) -0.047(4) O32 0.052(2) 0.066(3) 0.096(4) -0.023(2) -0.036(2) -0.0089(19) O33 0.067(4) 0.200(6) 0.081(3) -0.061(4) 0.021(2) -0.079(5) O34 0.155(7) 0.0704(18) 0.133(7) -0.014(3) -0.068(5) 0.038(3) _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 Mn1 N31 2.3001(15) . ? Mn1 N11 2.3026(15) . ? Mn1 N21 2.3145(15) . ? Mn1 N12 2.3471(16) . ? Mn1 N22 2.3517(16) . ? Mn1 N32 2.3767(15) . ? Mn1 N1 2.5176(15) . ? N1 C11 1.490(2) . ? N1 C21 1.492(2) . ? N1 C31 1.492(2) . ? N11 C14 1.272(2) . ? N11 C13 1.464(2) . ? N12 C16 1.307(3) . ? N12 C15 1.388(2) . ? N13 C16 1.353(3) . ? N13 C17 1.370(3) . ? N13 H13 0.8700 . ? C11 C12 1.524(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 C13 1.515(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 C15 1.447(3) . ? C14 H14 0.9400 . ? C15 C17 1.369(3) . ? C16 H16 0.9400 . ? C17 C18 1.488(3) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? N21 C24 1.271(2) . ? N21 C23 1.466(2) . ? N22 C26 1.311(2) . ? N22 C25 1.387(2) . ? N23 C26 1.351(3) . ? N23 C27 1.371(3) . ? N23 H23 0.8700 . ? C21 C22 1.524(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C22 C23 1.515(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 C25 1.446(3) . ? C24 H24 0.9400 . ? C25 C27 1.370(3) . ? C26 H26 0.9400 . ? C27 C28 1.494(3) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? N31 C34 1.272(2) . ? N31 C33 1.466(2) . ? N32 C36 1.310(2) . ? N32 C35 1.384(2) . ? N33 C36 1.353(3) . ? N33 C37 1.368(3) . ? N33 H33 0.8700 . ? C31 C32 1.519(3) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C32 C33 1.522(3) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C34 C35 1.446(3) . ? C34 H34 0.9400 . ? C35 C37 1.374(3) . ? C36 H36 0.9400 . ? C37 C38 1.491(3) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C38 H38C 0.9700 . ? Cl1 O11 1.416(2) . ? Cl1 O14 1.430(2) . ? Cl1 O13 1.4323(18) . ? Cl1 O12 1.4409(19) . ? Cl2 O22 1.402(6) . ? Cl2 O21 1.402(5) . ? Cl2 O24 1.417(5) . ? Cl2 O23 1.467(5) . ? 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 N31 Mn1 N11 117.05(6) . . ? N31 Mn1 N21 114.05(6) . . ? N11 Mn1 N21 112.70(5) . . ? N31 Mn1 N12 157.94(6) . . ? N11 Mn1 N12 71.75(6) . . ? N21 Mn1 N12 77.01(6) . . ? N31 Mn1 N22 77.99(6) . . ? N11 Mn1 N22 157.60(6) . . ? N21 Mn1 N22 71.36(5) . . ? N12 Mn1 N22 88.50(6) . . ? N31 Mn1 N32 71.56(5) . . ? N11 Mn1 N32 78.57(5) . . ? N21 Mn1 N32 159.90(6) . . ? N12 Mn1 N32 91.81(5) . . ? N22 Mn1 N32 91.96(5) . . ? N31 Mn1 N1 76.70(5) . . ? N11 Mn1 N1 76.45(5) . . ? N21 Mn1 N1 75.85(5) . . ? N12 Mn1 N1 125.29(5) . . ? N22 Mn1 N1 124.96(5) . . ? N32 Mn1 N1 123.92(5) . . ? C11 N1 C21 107.92(15) . . ? C11 N1 C31 108.35(15) . . ? C21 N1 C31 108.05(14) . . ? C11 N1 Mn1 110.06(11) . . ? C21 N1 Mn1 111.81(11) . . ? C31 N1 Mn1 110.54(11) . . ? C14 N11 C13 118.95(16) . . ? C14 N11 Mn1 118.07(13) . . ? C13 N11 Mn1 122.53(12) . . ? C16 N12 C15 105.62(17) . . ? C16 N12 Mn1 140.93(14) . . ? C15 N12 Mn1 112.43(12) . . ? C16 N13 C17 108.26(17) . . ? C16 N13 H13 125.9 . . ? C17 N13 H13 125.9 . . ? N1 C11 C12 116.50(17) . . ? N1 C11 H11A 108.2 . . ? C12 C11 H11A 108.2 . . ? N1 C11 H11B 108.2 . . ? C12 C11 H11B 108.2 . . ? H11A C11 H11B 107.3 . . ? C13 C12 C11 115.63(17) . . ? C13 C12 H12A 108.4 . . ? C11 C12 H12A 108.4 . . ? C13 C12 H12B 108.4 . . ? C11 C12 H12B 108.4 . . ? H12A C12 H12B 107.4 . . ? N11 C13 C12 113.62(16) . . ? N11 C13 H13A 108.8 . . ? C12 C13 H13A 108.8 . . ? N11 C13 H13B 108.8 . . ? C12 C13 H13B 108.8 . . ? H13A C13 H13B 107.7 . . ? N11 C14 C15 118.91(17) . . ? N11 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? C17 C15 N12 109.91(18) . . ? C17 C15 C14 131.84(18) . . ? N12 C15 C14 118.25(16) . . ? N12 C16 N13 111.26(19) . . ? N12 C16 H16 124.4 . . ? N13 C16 H16 124.4 . . ? C15 C17 N13 104.95(17) . . ? C15 C17 C18 132.7(2) . . ? N13 C17 C18 122.4(2) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C24 N21 C23 118.85(16) . . ? C24 N21 Mn1 118.18(12) . . ? C23 N21 Mn1 122.53(12) . . ? C26 N22 C25 105.18(16) . . ? C26 N22 Mn1 141.11(14) . . ? C25 N22 Mn1 112.54(11) . . ? C26 N23 C27 108.35(16) . . ? C26 N23 H23 125.8 . . ? C27 N23 H23 125.8 . . ? N1 C21 C22 117.02(16) . . ? N1 C21 H21A 108.0 . . ? C22 C21 H21A 108.0 . . ? N1 C21 H21B 108.0 . . ? C22 C21 H21B 108.0 . . ? H21A C21 H21B 107.3 . . ? C23 C22 C21 115.23(16) . . ? C23 C22 H22A 108.5 . . ? C21 C22 H22A 108.5 . . ? C23 C22 H22B 108.5 . . ? C21 C22 H22B 108.5 . . ? H22A C22 H22B 107.5 . . ? N21 C23 C22 112.28(17) . . ? N21 C23 H23A 109.1 . . ? C22 C23 H23A 109.1 . . ? N21 C23 H23B 109.1 . . ? C22 C23 H23B 109.1 . . ? H23A C23 H23B 107.9 . . ? N21 C24 C25 118.71(17) . . ? N21 C24 H24 120.6 . . ? C25 C24 H24 120.6 . . ? C27 C25 N22 110.34(17) . . ? C27 C25 C24 131.33(17) . . ? N22 C25 C24 118.30(16) . . ? N22 C26 N23 111.47(18) . . ? N22 C26 H26 124.3 . . ? N23 C26 H26 124.3 . . ? C25 C27 N23 104.66(17) . . ? C25 C27 C28 132.5(2) . . ? N23 C27 C28 122.76(19) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C34 N31 C33 118.15(16) . . ? C34 N31 Mn1 118.40(12) . . ? C33 N31 Mn1 123.11(12) . . ? C36 N32 C35 105.10(16) . . ? C36 N32 Mn1 142.58(13) . . ? C35 N32 Mn1 111.78(11) . . ? C36 N33 C37 108.16(16) . . ? C36 N33 H33 125.9 . . ? C37 N33 H33 125.9 . . ? N1 C31 C32 117.65(16) . . ? N1 C31 H31A 107.9 . . ? C32 C31 H31A 107.9 . . ? N1 C31 H31B 107.9 . . ? C32 C31 H31B 107.9 . . ? H31A C31 H31B 107.2 . . ? C31 C32 C33 114.74(17) . . ? C31 C32 H32A 108.6 . . ? C33 C32 H32A 108.6 . . ? C31 C32 H32B 108.6 . . ? C33 C32 H32B 108.6 . . ? H32A C32 H32B 107.6 . . ? N31 C33 C32 111.92(16) . . ? N31 C33 H33A 109.2 . . ? C32 C33 H33A 109.2 . . ? N31 C33 H33B 109.2 . . ? C32 C33 H33B 109.2 . . ? H33A C33 H33B 107.9 . . ? N31 C34 C35 119.14(17) . . ? N31 C34 H34 120.4 . . ? C35 C34 H34 120.4 . . ? C37 C35 N32 110.40(17) . . ? C37 C35 C34 130.83(17) . . ? N32 C35 C34 118.77(16) . . ? N32 C36 N33 111.66(18) . . ? N32 C36 H36 124.2 . . ? N33 C36 H36 124.2 . . ? N33 C37 C35 104.68(17) . . ? N33 C37 C38 123.04(19) . . ? C35 C37 C38 132.3(2) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O11 Cl1 O14 111.07(15) . . ? O11 Cl1 O13 110.74(14) . . ? O14 Cl1 O13 108.51(13) . . ? O11 Cl1 O12 109.67(13) . . ? O14 Cl1 O12 109.49(14) . . ? O13 Cl1 O12 107.26(13) . . ? O22 Cl2 O21 111.3(6) . . ? O22 Cl2 O24 109.1(6) . . ? O21 Cl2 O24 112.1(5) . . ? O22 Cl2 O23 112.5(6) . . ? O21 Cl2 O23 107.8(5) . . ? O24 Cl2 O23 103.9(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 N31 Mn1 N1 C11 -69.88(12) . . . . ? N11 Mn1 N1 C11 52.65(12) . . . . ? N21 Mn1 N1 C11 170.69(13) . . . . ? N12 Mn1 N1 C11 108.23(12) . . . . ? N22 Mn1 N1 C11 -134.65(12) . . . . ? N32 Mn1 N1 C11 -13.28(14) . . . . ? N31 Mn1 N1 C21 170.19(12) . . . . ? N11 Mn1 N1 C21 -67.28(12) . . . . ? N21 Mn1 N1 C21 50.76(11) . . . . ? N12 Mn1 N1 C21 -11.70(14) . . . . ? N22 Mn1 N1 C21 105.42(12) . . . . ? N32 Mn1 N1 C21 -133.21(11) . . . . ? N31 Mn1 N1 C31 49.78(12) . . . . ? N11 Mn1 N1 C31 172.31(13) . . . . ? N21 Mn1 N1 C31 -69.66(12) . . . . ? N12 Mn1 N1 C31 -132.11(12) . . . . ? N22 Mn1 N1 C31 -15.00(14) . . . . ? N32 Mn1 N1 C31 106.37(12) . . . . ? N31 Mn1 N11 C14 -160.67(13) . . . . ? N21 Mn1 N11 C14 64.12(15) . . . . ? N12 Mn1 N11 C14 -2.64(13) . . . . ? N22 Mn1 N11 C14 -31.9(2) . . . . ? N32 Mn1 N11 C14 -98.42(14) . . . . ? N1 Mn1 N11 C14 132.21(15) . . . . ? N31 Mn1 N11 C13 11.58(16) . . . . ? N21 Mn1 N11 C13 -123.62(14) . . . . ? N12 Mn1 N11 C13 169.61(15) . . . . ? N22 Mn1 N11 C13 140.32(16) . . . . ? N32 Mn1 N11 C13 73.83(14) . . . . ? N1 Mn1 N11 C13 -55.54(14) . . . . ? N31 Mn1 N12 C16 -70.6(3) . . . . ? N11 Mn1 N12 C16 172.0(2) . . . . ? N21 Mn1 N12 C16 52.4(2) . . . . ? N22 Mn1 N12 C16 -18.8(2) . . . . ? N32 Mn1 N12 C16 -110.7(2) . . . . ? N1 Mn1 N12 C16 114.3(2) . . . . ? N31 Mn1 N12 C15 123.39(16) . . . . ? N11 Mn1 N12 C15 5.91(12) . . . . ? N21 Mn1 N12 C15 -113.63(13) . . . . ? N22 Mn1 N12 C15 175.16(12) . . . . ? N32 Mn1 N12 C15 83.25(12) . . . . ? N1 Mn1 N12 C15 -51.70(14) . . . . ? C21 N1 C11 C12 51.6(2) . . . . ? C31 N1 C11 C12 168.39(17) . . . . ? Mn1 N1 C11 C12 -70.63(18) . . . . ? N1 C11 C12 C13 67.6(2) . . . . ? C14 N11 C13 C12 -121.2(2) . . . . ? Mn1 N11 C13 C12 66.6(2) . . . . ? C11 C12 C13 N11 -58.1(2) . . . . ? C13 N11 C14 C15 -173.65(16) . . . . ? Mn1 N11 C14 C15 -1.1(2) . . . . ? C16 N12 C15 C17 0.4(2) . . . . ? Mn1 N12 C15 C17 171.32(12) . . . . ? C16 N12 C15 C14 -179.77(17) . . . . ? Mn1 N12 C15 C14 -8.8(2) . . . . ? N11 C14 C15 C17 -173.18(19) . . . . ? N11 C14 C15 N12 7.0(3) . . . . ? C15 N12 C16 N13 -0.5(2) . . . . ? Mn1 N12 C16 N13 -167.16(15) . . . . ? C17 N13 C16 N12 0.5(2) . . . . ? N12 C15 C17 N13 -0.1(2) . . . . ? C14 C15 C17 N13 -179.91(19) . . . . ? N12 C15 C17 C18 -179.0(2) . . . . ? C14 C15 C17 C18 1.2(4) . . . . ? C16 N13 C17 C15 -0.2(2) . . . . ? C16 N13 C17 C18 178.8(2) . . . . ? N31 Mn1 N21 C24 63.19(15) . . . . ? N11 Mn1 N21 C24 -160.22(14) . . . . ? N12 Mn1 N21 C24 -96.63(15) . . . . ? N22 Mn1 N21 C24 -3.79(14) . . . . ? N32 Mn1 N21 C24 -39.0(2) . . . . ? N1 Mn1 N21 C24 131.33(15) . . . . ? N31 Mn1 N21 C23 -124.48(14) . . . . ? N11 Mn1 N21 C23 12.11(16) . . . . ? N12 Mn1 N21 C23 75.70(15) . . . . ? N22 Mn1 N21 C23 168.54(16) . . . . ? N32 Mn1 N21 C23 133.29(17) . . . . ? N1 Mn1 N21 C23 -56.34(14) . . . . ? N31 Mn1 N22 C26 51.8(2) . . . . ? N11 Mn1 N22 C26 -83.0(3) . . . . ? N21 Mn1 N22 C26 172.6(2) . . . . ? N12 Mn1 N22 C26 -110.6(2) . . . . ? N32 Mn1 N22 C26 -18.9(2) . . . . ? N1 Mn1 N22 C26 116.0(2) . . . . ? N31 Mn1 N22 C25 -113.23(13) . . . . ? N11 Mn1 N22 C25 112.01(16) . . . . ? N21 Mn1 N22 C25 7.53(12) . . . . ? N12 Mn1 N22 C25 84.32(13) . . . . ? N32 Mn1 N22 C25 176.08(12) . . . . ? N1 Mn1 N22 C25 -49.06(14) . . . . ? C11 N1 C21 C22 170.66(17) . . . . ? C31 N1 C21 C22 53.7(2) . . . . ? Mn1 N1 C21 C22 -68.17(19) . . . . ? N1 C21 C22 C23 67.1(2) . . . . ? C24 N21 C23 C22 -117.9(2) . . . . ? Mn1 N21 C23 C22 69.8(2) . . . . ? C21 C22 C23 N21 -60.6(2) . . . . ? C23 N21 C24 C25 -173.24(17) . . . . ? Mn1 N21 C24 C25 -0.6(2) . . . . ? C26 N22 C25 C27 0.4(2) . . . . ? Mn1 N22 C25 C27 170.77(13) . . . . ? C26 N22 C25 C24 178.73(17) . . . . ? Mn1 N22 C25 C24 -10.9(2) . . . . ? N21 C24 C25 C27 -174.0(2) . . . . ? N21 C24 C25 N22 8.2(3) . . . . ? C25 N22 C26 N23 -0.5(2) . . . . ? Mn1 N22 C26 N23 -166.16(15) . . . . ? C27 N23 C26 N22 0.3(2) . . . . ? N22 C25 C27 N23 -0.2(2) . . . . ? C24 C25 C27 N23 -178.24(19) . . . . ? N22 C25 C27 C28 -177.7(2) . . . . ? C24 C25 C27 C28 4.3(4) . . . . ? C26 N23 C27 C25 0.0(2) . . . . ? C26 N23 C27 C28 177.8(2) . . . . ? N11 Mn1 N31 C34 64.24(15) . . . . ? N21 Mn1 N31 C34 -161.14(13) . . . . ? N12 Mn1 N31 C34 -44.7(2) . . . . ? N22 Mn1 N31 C34 -98.07(15) . . . . ? N32 Mn1 N31 C34 -1.88(14) . . . . ? N1 Mn1 N31 C34 131.22(15) . . . . ? N11 Mn1 N31 C33 -122.53(14) . . . . ? N21 Mn1 N31 C33 12.09(16) . . . . ? N12 Mn1 N31 C33 128.56(17) . . . . ? N22 Mn1 N31 C33 75.16(15) . . . . ? N32 Mn1 N31 C33 171.35(16) . . . . ? N1 Mn1 N31 C33 -55.55(14) . . . . ? N31 Mn1 N32 C36 174.2(2) . . . . ? N11 Mn1 N32 C36 50.4(2) . . . . ? N21 Mn1 N32 C36 -76.0(3) . . . . ? N12 Mn1 N32 C36 -20.6(2) . . . . ? N22 Mn1 N32 C36 -109.2(2) . . . . ? N1 Mn1 N32 C36 115.3(2) . . . . ? N31 Mn1 N32 C35 4.42(12) . . . . ? N11 Mn1 N32 C35 -119.40(13) . . . . ? N21 Mn1 N32 C35 114.24(17) . . . . ? N12 Mn1 N32 C35 169.63(12) . . . . ? N22 Mn1 N32 C35 81.06(12) . . . . ? N1 Mn1 N32 C35 -54.49(14) . . . . ? C11 N1 C31 C32 51.8(2) . . . . ? C21 N1 C31 C32 168.49(17) . . . . ? Mn1 N1 C31 C32 -68.88(19) . . . . ? N1 C31 C32 C33 69.2(2) . . . . ? C34 N31 C33 C32 -117.9(2) . . . . ? Mn1 N31 C33 C32 68.8(2) . . . . ? C31 C32 C33 N31 -60.7(2) . . . . ? C33 N31 C34 C35 -174.58(17) . . . . ? Mn1 N31 C34 C35 -1.0(2) . . . . ? C36 N32 C35 C37 0.4(2) . . . . ? Mn1 N32 C35 C37 173.98(12) . . . . ? C36 N32 C35 C34 179.70(17) . . . . ? Mn1 N32 C35 C34 -6.7(2) . . . . ? N31 C34 C35 C37 -175.35(19) . . . . ? N31 C34 C35 N32 5.5(3) . . . . ? C35 N32 C36 N33 -0.3(2) . . . . ? Mn1 N32 C36 N33 -170.49(15) . . . . ? C37 N33 C36 N32 0.1(2) . . . . ? C36 N33 C37 C35 0.1(2) . . . . ? C36 N33 C37 C38 178.9(2) . . . . ? N32 C35 C37 N33 -0.3(2) . . . . ? C34 C35 C37 N33 -179.50(19) . . . . ? N32 C35 C37 C38 -179.0(2) . . . . ? C34 C35 C37 C38 1.9(4) . . . . ? 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 N13 H13 O24 0.87 2.22 3.045(7) 158.7 2_566 N13 H13 O33 0.87 2.34 2.918(10) 123.9 2_566 N23 H23 O32 0.87 2.04 2.852(9) 154.7 2_666 N23 H23 O22 0.87 2.09 2.854(12) 146.7 2_666 N33 H33 O13 0.87 2.05 2.924(3) 176.2 2_576 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.555 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.054 _exptl_crystal_id 'Brewer LLC21' _diffrn_measurement_total_frames-CCD 1907 _diffrn_measurement_details NFRAMES=645,606,606,50 _diffrn_measurement_frame_width-CCD 0.30 _diffrn_detector_distance-CCD 4.99 _diffrn_source_voltage 50 _diffrn_source_current 35 _diffrn_measurement_frame_time-CCD 15 _diffrn_measurement_total_time-CCD 11.7 _diffrn_measurement_frame_size-CCD 512 _diffrn_orient_matrix_type standard _diffrn_orient_matrix_UB_11 -0.0353365 _diffrn_orient_matrix_UB_12 -0.0329681 _diffrn_orient_matrix_UB_13 0.0788239 _diffrn_orient_matrix_UB_21 -0.0166345 _diffrn_orient_matrix_UB_22 0.0759628 _diffrn_orient_matrix_UB_23 0.0314922 _diffrn_orient_matrix_UB_31 -0.0871852 _diffrn_orient_matrix_UB_32 0.0326304 _diffrn_orient_matrix_UB_33 -0.0115499 _symmetry_space_group_name_Hall '-P 1' _diffrn_measurement_specimen_support 'glass capillary' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker Smart1000' #_______________________________________________________________________________ # _publ_section_references ; Bruker (1999). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Spek, A. L. (1990). Acta Cryst., A46, C-34. Sheldrick, G. M. (1990). Acta Cryst. A46, 467-473. Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany. Sheldrick, G. M. (1997). SHELXL-97. University of G\"ottingen, Germany. ;