# Copyright The Royal Society of Chemistry, 1998 # CCDC Number: 186/1189 data_GLOBAL # 1. SUBMISSION DETAILS _publ_contact_author_name 'Comba, Peter' _publ_contact_author_address ; Anorganisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg Germany ; _publ_contact_author_phone '049 6221 54-8453' _publ_contact_author_fax '049 6221 54-6617' _publ_contact_author_email 'comba@akcomba.oci.uni-heidelberg.de' _publ_requested_journal 'J. Chem. Soc., Dalton' _publ_requested_coeditor_name ? _publ_contact_letter ; paper (to be) submitted/accepted for publication in J. Chem. Soc., Dalton ; #======================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and Characterization of Manganese(II) Compounds with Tetradentate Ligands Based on the Bispidine Backbone ; loop_ _publ_author_name _publ_author_address 'Comba, Peter' ; Anorganisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; 'Kanellakopulos, Basil' ; Anorganisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; 'Katsichtis, Charis' ; Anorganisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; 'Lienke, Achim' ; Anorganisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; 'Rominger, Frank' ; Organisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; 'Pritzkow, Hans' ; Anorganisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; #======================================================================= # 4. TEXT _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_experimental ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; ; #======================================================================= data_comba11 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H26 Cl2 Mn N4 O6' _chemical_formula_weight 616.35 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 11.577(6) _cell_length_b 11.812(6) _cell_length_c 11.951(6) _cell_angle_alpha 110.71(3) _cell_angle_beta 102.50(3) _cell_angle_gamma 105.15(3) _cell_volume 1386.5(12) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 634 _exptl_absorpt_coefficient_mu 0.716 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.949 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens-Stoe AED2' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 1 _diffrn_reflns_number 4443 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0704 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4443 _reflns_number_gt 3133 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DIF4 (Stoe)' _computing_cell_refinement 'DIF4 (Stoe)' _computing_data_reduction 'REDU4 (Stoe)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (C.K.Johnson, 1965)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Disordered solvent molecule(s) ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0595P)^2^+1.3592P] 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 4443 _refine_ls_number_parameters 367 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0962 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1409 _refine_ls_wR_factor_gt 0.1230 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.23187(6) 0.95790(7) 0.23586(7) 0.0281(2) Uani 1 d . . . Cl1 Cl 0.21845(12) 0.85838(12) 0.38445(12) 0.0393(3) Uani 1 d . . . Cl2 Cl 0.06922(16) 0.77138(15) 0.05474(15) 0.0700(5) Uani 1 d . . . N1 N 0.4001(3) 1.1617(3) 0.3784(3) 0.0233(8) Uani 1 d . . . N2 N 0.2666(3) 1.0852(4) 0.1067(3) 0.0278(9) Uani 1 d . . . N3 N 0.4152(3) 0.9349(3) 0.2264(3) 0.0269(8) Uani 1 d . . . N4 N 0.1443(3) 1.0948(3) 0.3359(3) 0.0275(9) Uani 1 d . . . O1 O 0.5238(3) 1.4442(3) 0.2692(3) 0.0382(8) Uani 1 d . . . O2 O 0.6363(3) 1.2064(4) 0.0991(3) 0.0487(10) Uani 1 d . . . O3 O 0.7244(3) 1.3319(3) 0.3090(3) 0.0388(8) Uani 1 d . . . O4 O 0.3615(3) 1.5235(3) 0.4326(3) 0.0387(8) Uani 1 d . . . O5 O 0.2099(3) 1.4270(3) 0.2403(3) 0.0461(9) Uani 1 d . . . C1 C 0.5104(4) 1.1737(4) 0.3332(4) 0.0233(9) Uani 1 d . . . C2 C 0.5004(4) 1.2206(4) 0.2263(4) 0.0256(10) Uani 1 d . . . C3 C 0.3950(4) 1.1201(5) 0.0976(4) 0.0274(10) Uani 1 d . . . C4 C 0.2366(4) 1.2040(5) 0.1535(4) 0.0284(10) Uani 1 d . . . C5 C 0.3357(4) 1.3098(4) 0.2847(4) 0.0255(10) Uani 1 d . . . C6 C 0.3481(4) 1.2668(4) 0.3956(4) 0.0251(10) Uani 1 d . . . C7 C 0.4641(4) 1.3411(4) 0.2647(4) 0.0257(10) Uani 1 d . . . C8 C 0.5233(4) 1.0401(4) 0.2835(4) 0.0254(10) Uani 1 d . . . C9 C 0.6417(4) 1.0295(5) 0.2943(4) 0.0314(11) Uani 1 d . . . H9 H 0.7168 1.1041 0.3345 0.035(5) Uiso 1 calc R . . C10 C 0.6459(5) 0.9057(5) 0.2442(5) 0.0376(12) Uani 1 d . . . H10 H 0.7246 0.8956 0.2502 0.035(5) Uiso 1 calc R . . C11 C 0.5351(5) 0.7982(5) 0.1859(4) 0.0364(12) Uani 1 d . . . H11 H 0.5365 0.7138 0.1517 0.035(5) Uiso 1 calc R . . C12 C 0.4210(5) 0.8169(4) 0.1786(4) 0.0339(11) Uani 1 d . . . H12 H 0.3447 0.7436 0.1384 0.035(5) Uiso 1 calc R . . C13 C 0.2206(4) 1.2203(4) 0.4116(4) 0.0261(10) Uani 1 d . . . C14 C 0.1862(5) 1.3020(5) 0.5040(5) 0.0371(12) Uani 1 d . . . H14 H 0.2406 1.3892 0.5564 0.035(5) Uiso 1 calc R . . C15 C 0.0699(5) 1.2519(5) 0.5171(5) 0.0435(13) Uani 1 d . . . H15 H 0.0441 1.3050 0.5782 0.035(5) Uiso 1 calc R . . C16 C -0.0075(4) 1.1230(5) 0.4393(5) 0.0377(12) Uani 1 d . . . H16 H -0.0862 1.0869 0.4472 0.035(5) Uiso 1 calc R . . C17 C 0.0326(4) 1.0485(5) 0.3501(4) 0.0322(11) Uani 1 d . . . H17 H -0.0207 0.9611 0.2969 0.035(5) Uiso 1 calc R . . C18 C 0.6264(4) 1.2513(4) 0.2018(4) 0.0310(11) Uani 1 d . . . C19 C 0.8480(5) 1.3646(6) 0.2956(6) 0.0558(16) Uani 1 d . . . H19A H 0.9105 1.4339 0.3753 0.081(9) Uiso 1 calc R . . H19B H 0.8455 1.3935 0.2288 0.081(9) Uiso 1 calc R . . H19C H 0.8714 1.2885 0.2737 0.081(9) Uiso 1 calc R . . C20 C 0.3053(4) 1.4335(4) 0.3293(5) 0.0294(11) Uani 1 d . . . C21 C 0.1743(6) 1.5417(6) 0.2725(6) 0.0613(18) Uani 1 d . . . H21A H 0.0986 1.5242 0.2051 0.081(9) Uiso 1 calc R . . H21B H 0.2436 1.6154 0.2819 0.081(9) Uiso 1 calc R . . H21C H 0.1572 1.5615 0.3518 0.081(9) Uiso 1 calc R . . C22 C 0.4427(4) 1.1601(4) 0.5043(4) 0.0285(10) Uani 1 d . . . H22A H 0.4832 1.0969 0.4978 0.038(6) Uiso 1 calc R . . H22B H 0.3697 1.1365 0.5303 0.038(6) Uiso 1 calc R . . H22C H 0.5030 1.2459 0.5667 0.038(6) Uiso 1 calc R . . C23 C 0.1764(4) 1.0015(5) -0.0258(4) 0.0366(12) Uani 1 d . . . H23A H 0.0901 0.9747 -0.0248 0.038(6) Uiso 1 calc R . . H23B H 0.1968 0.9250 -0.0627 0.038(6) Uiso 1 calc R . . H23C H 0.1835 1.0501 -0.0762 0.038(6) Uiso 1 calc R . . H1 H 0.591(5) 1.233(4) 0.401(4) 0.032(13) Uiso 1 d . . . H3A H 0.397(4) 1.157(4) 0.036(4) 0.027(12) Uiso 1 d . . . H3B H 0.412(4) 1.041(5) 0.067(4) 0.034(13) Uiso 1 d . . . H4A H 0.147(4) 1.173(4) 0.159(4) 0.016(10) Uiso 1 d . . . H4B H 0.235(5) 1.241(5) 0.094(5) 0.042(14) Uiso 1 d . . . H6 H 0.405(4) 1.340(4) 0.469(4) 0.025(12) Uiso 1 d . . . O31 O -0.1727(7) 0.7380(7) 0.1285(7) 0.137(2) Uiso 1 d . . . C32 C -0.0923(14) 0.6075(14) 0.1803(14) 0.175(5) Uiso 1 d . . . C33 C -0.3056(14) 0.5412(14) 0.0485(14) 0.163(5) Uiso 1 d . . . C34 C -0.1945(19) 0.5342(18) 0.0588(18) 0.100(5) Uiso 0.50 d P . . C35 C -0.2255(19) 0.6216(19) 0.1466(19) 0.102(5) Uiso 0.50 d P . . 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 0.0240(4) 0.0246(4) 0.0303(4) 0.0070(3) 0.0099(3) 0.0074(3) Cl1 0.0456(7) 0.0342(6) 0.0478(7) 0.0209(6) 0.0254(6) 0.0175(6) Cl2 0.0631(10) 0.0502(9) 0.0479(9) 0.0078(7) -0.0025(8) -0.0162(8) N1 0.0225(19) 0.0231(19) 0.0238(19) 0.0093(16) 0.0089(16) 0.0083(16) N2 0.024(2) 0.030(2) 0.0237(19) 0.0068(17) 0.0050(17) 0.0103(17) N3 0.030(2) 0.030(2) 0.0239(19) 0.0119(17) 0.0112(17) 0.0129(17) N4 0.024(2) 0.028(2) 0.029(2) 0.0116(18) 0.0089(17) 0.0101(17) O1 0.0359(19) 0.0289(18) 0.051(2) 0.0189(16) 0.0190(17) 0.0078(15) O2 0.041(2) 0.067(3) 0.040(2) 0.0206(19) 0.0239(18) 0.0189(19) O3 0.0230(17) 0.043(2) 0.041(2) 0.0123(17) 0.0119(16) 0.0054(15) O4 0.044(2) 0.0267(18) 0.0349(19) 0.0050(16) 0.0080(17) 0.0131(16) O5 0.048(2) 0.035(2) 0.045(2) 0.0087(17) 0.0010(18) 0.0256(17) C1 0.018(2) 0.027(2) 0.024(2) 0.011(2) 0.007(2) 0.0066(19) C2 0.024(2) 0.030(2) 0.024(2) 0.012(2) 0.0101(19) 0.0099(19) C3 0.030(3) 0.029(3) 0.020(2) 0.008(2) 0.008(2) 0.011(2) C4 0.024(3) 0.031(3) 0.026(2) 0.010(2) 0.006(2) 0.009(2) C5 0.028(2) 0.023(2) 0.026(2) 0.011(2) 0.010(2) 0.0096(19) C6 0.026(2) 0.024(2) 0.025(2) 0.008(2) 0.010(2) 0.011(2) C7 0.028(2) 0.026(2) 0.021(2) 0.0082(19) 0.007(2) 0.010(2) C8 0.027(2) 0.031(2) 0.020(2) 0.012(2) 0.009(2) 0.010(2) C9 0.026(2) 0.036(3) 0.034(3) 0.015(2) 0.011(2) 0.014(2) C10 0.037(3) 0.046(3) 0.043(3) 0.023(3) 0.020(2) 0.025(3) C11 0.048(3) 0.034(3) 0.036(3) 0.015(2) 0.021(2) 0.023(3) C12 0.040(3) 0.025(2) 0.033(3) 0.008(2) 0.014(2) 0.012(2) C13 0.025(2) 0.032(2) 0.026(2) 0.015(2) 0.011(2) 0.012(2) C14 0.039(3) 0.036(3) 0.035(3) 0.011(2) 0.019(2) 0.015(2) C15 0.039(3) 0.047(3) 0.047(3) 0.012(3) 0.025(3) 0.021(3) C16 0.025(3) 0.048(3) 0.049(3) 0.025(3) 0.020(2) 0.016(2) C17 0.023(2) 0.035(3) 0.036(3) 0.015(2) 0.010(2) 0.009(2) C18 0.030(3) 0.033(3) 0.034(3) 0.016(2) 0.013(2) 0.013(2) C19 0.027(3) 0.061(4) 0.071(4) 0.025(3) 0.022(3) 0.006(3) C20 0.025(2) 0.028(3) 0.037(3) 0.014(2) 0.011(2) 0.011(2) C21 0.066(4) 0.050(4) 0.072(4) 0.023(3) 0.013(3) 0.042(3) C22 0.027(2) 0.032(3) 0.026(2) 0.013(2) 0.008(2) 0.011(2) C23 0.032(3) 0.041(3) 0.026(3) 0.008(2) 0.006(2) 0.011(2) _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 N3 2.231(4) . ? Mn1 N4 2.255(4) . ? Mn1 N1 2.388(4) . ? Mn1 Cl2 2.404(2) . ? Mn1 Cl1 2.4616(18) . ? Mn1 N2 2.531(4) . ? N1 C22 1.486(5) . ? N1 C6 1.486(5) . ? N1 C1 1.484(5) . ? N2 C3 1.474(6) . ? N2 C4 1.478(6) . ? N2 C23 1.487(6) . ? N3 C12 1.332(6) . ? N3 C8 1.339(6) . ? N4 C17 1.338(6) . ? N4 C13 1.348(6) . ? O1 C7 1.209(5) . ? O2 C18 1.196(5) . ? O3 C18 1.333(6) . ? O3 C19 1.441(6) . ? O4 C20 1.200(5) . ? O5 C20 1.321(6) . ? O5 C21 1.465(6) . ? C1 C8 1.537(6) . ? C1 C2 1.556(6) . ? C1 H1 0.97(5) . ? C2 C18 1.527(6) . ? C2 C7 1.532(6) . ? C2 C3 1.550(6) . ? C3 H3A 0.98(5) . ? C3 H3B 0.97(5) . ? C4 C5 1.556(6) . ? C4 H4A 1.03(4) . ? C4 H4B 0.95(5) . ? C5 C7 1.527(6) . ? C5 C20 1.531(6) . ? C5 C6 1.572(6) . ? C6 C13 1.513(6) . ? C6 H6 0.93(4) . ? C8 C9 1.392(6) . ? C9 C10 1.390(7) . ? C9 H9 0.9400 . ? C10 C11 1.371(7) . ? C10 H10 0.9400 . ? C11 C12 1.385(7) . ? C11 H11 0.9400 . ? C12 H12 0.9400 . ? C13 C14 1.395(6) . ? C14 C15 1.388(7) . ? C14 H14 0.9400 . ? C15 C16 1.382(7) . ? C15 H15 0.9400 . ? C16 C17 1.375(6) . ? C16 H16 0.9400 . ? C17 H17 0.9400 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? O31 C35 1.463(19) . ? C32 C34 1.45(2) . ? C32 C35 1.58(2) . ? C33 C35 1.19(2) . ? C33 C34 1.29(2) . ? C34 C35 1.37(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 N3 Mn1 N4 144.40(14) . . ? N3 Mn1 N1 72.35(13) . . ? N4 Mn1 N1 72.19(13) . . ? N3 Mn1 Cl2 105.27(11) . . ? N4 Mn1 Cl2 109.92(11) . . ? N1 Mn1 Cl2 166.22(10) . . ? N3 Mn1 Cl1 92.80(10) . . ? N4 Mn1 Cl1 89.54(10) . . ? N1 Mn1 Cl1 98.86(10) . . ? Cl2 Mn1 Cl1 94.79(7) . . ? N3 Mn1 N2 85.47(13) . . ? N4 Mn1 N2 87.87(13) . . ? N1 Mn1 N2 74.01(12) . . ? Cl2 Mn1 N2 92.35(10) . . ? Cl1 Mn1 N2 172.86(9) . . ? C22 N1 C6 107.3(3) . . ? C22 N1 C1 106.7(3) . . ? C6 N1 C1 116.9(3) . . ? C22 N1 Mn1 107.9(3) . . ? C6 N1 Mn1 108.5(3) . . ? C1 N1 Mn1 109.2(2) . . ? C3 N2 C4 109.4(4) . . ? C3 N2 C23 106.3(3) . . ? C4 N2 C23 106.7(3) . . ? C3 N2 Mn1 114.5(3) . . ? C4 N2 Mn1 112.0(3) . . ? C23 N2 Mn1 107.7(3) . . ? C12 N3 C8 119.3(4) . . ? C12 N3 Mn1 120.7(3) . . ? C8 N3 Mn1 119.5(3) . . ? C17 N4 C13 118.6(4) . . ? C17 N4 Mn1 120.6(3) . . ? C13 N4 Mn1 118.0(3) . . ? C18 O3 C19 115.8(4) . . ? C20 O5 C21 115.7(4) . . ? N1 C1 C8 108.3(3) . . ? N1 C1 C2 114.3(3) . . ? C8 C1 C2 108.9(3) . . ? N1 C1 H1 113(3) . . ? C8 C1 H1 105(3) . . ? C2 C1 H1 107(3) . . ? C18 C2 C7 110.5(4) . . ? C18 C2 C3 107.4(4) . . ? C7 C2 C3 104.9(4) . . ? C18 C2 C1 110.3(4) . . ? C7 C2 C1 109.7(3) . . ? C3 C2 C1 113.9(4) . . ? N2 C3 C2 113.2(3) . . ? N2 C3 H3A 109(3) . . ? C2 C3 H3A 108(3) . . ? N2 C3 H3B 108(3) . . ? C2 C3 H3B 110(3) . . ? H3A C3 H3B 109(4) . . ? N2 C4 C5 112.5(4) . . ? N2 C4 H4A 105(2) . . ? C5 C4 H4A 111(2) . . ? N2 C4 H4B 110(3) . . ? C5 C4 H4B 108(3) . . ? H4A C4 H4B 110(4) . . ? C7 C5 C20 109.5(3) . . ? C7 C5 C4 105.9(3) . . ? C20 C5 C4 111.6(4) . . ? C7 C5 C6 108.0(3) . . ? C20 C5 C6 106.7(3) . . ? C4 C5 C6 115.0(4) . . ? N1 C6 C13 107.8(3) . . ? N1 C6 C5 114.0(3) . . ? C13 C6 C5 111.1(4) . . ? N1 C6 H6 108(3) . . ? C13 C6 H6 110(3) . . ? C5 C6 H6 106(3) . . ? O1 C7 C5 124.3(4) . . ? O1 C7 C2 124.7(4) . . ? C5 C7 C2 110.8(3) . . ? N3 C8 C9 121.7(4) . . ? N3 C8 C1 116.9(4) . . ? C9 C8 C1 121.4(4) . . ? C10 C9 C8 118.3(4) . . ? C10 C9 H9 120.9 . . ? C8 C9 H9 120.9 . . ? C11 C10 C9 119.8(4) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C10 C11 C12 118.4(4) . . ? C10 C11 H11 120.8 . . ? C12 C11 H11 120.8 . . ? N3 C12 C11 122.5(4) . . ? N3 C12 H12 118.7 . . ? C11 C12 H12 118.7 . . ? N4 C13 C14 121.7(4) . . ? N4 C13 C6 116.7(4) . . ? C14 C13 C6 121.5(4) . . ? C15 C14 C13 118.7(5) . . ? C15 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? C16 C15 C14 119.2(5) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C17 C16 C15 118.9(4) . . ? C17 C16 H16 120.6 . . ? C15 C16 H16 120.6 . . ? N4 C17 C16 122.9(4) . . ? N4 C17 H17 118.6 . . ? C16 C17 H17 118.6 . . ? O2 C18 O3 124.2(4) . . ? O2 C18 C2 124.0(4) . . ? O3 C18 C2 111.8(4) . . ? O3 C19 H19A 109.5 . . ? O3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O4 C20 O5 125.3(4) . . ? O4 C20 C5 123.4(4) . . ? O5 C20 C5 111.3(4) . . ? O5 C21 H21A 109.5 . . ? O5 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O5 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N1 C22 H22A 109.5 . . ? N1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N2 C23 H23A 109.5 . . ? N2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C34 C32 C35 53.9(11) . . ? C35 C33 C34 67.0(14) . . ? C33 C34 C35 53.0(12) . . ? C33 C34 C32 120.0(17) . . ? C35 C34 C32 67.9(13) . . ? C33 C35 C34 60.0(13) . . ? C33 C35 O31 107.6(16) . . ? C34 C35 O31 100.0(15) . . ? C33 C35 C32 117.4(17) . . ? C34 C35 C32 58.2(12) . . ? O31 C35 C32 92.3(13) . . ? 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 N3 Mn1 N1 C22 -88.4(3) . . . . ? N4 Mn1 N1 C22 88.3(3) . . . . ? Cl2 Mn1 N1 C22 -170.6(3) . . . . ? Cl1 Mn1 N1 C22 1.7(3) . . . . ? N2 Mn1 N1 C22 -178.7(3) . . . . ? N3 Mn1 N1 C6 155.6(3) . . . . ? N4 Mn1 N1 C6 -27.7(2) . . . . ? Cl2 Mn1 N1 C6 73.4(5) . . . . ? Cl1 Mn1 N1 C6 -114.3(2) . . . . ? N2 Mn1 N1 C6 65.3(3) . . . . ? N3 Mn1 N1 C1 27.2(3) . . . . ? N4 Mn1 N1 C1 -156.0(3) . . . . ? Cl2 Mn1 N1 C1 -54.9(6) . . . . ? Cl1 Mn1 N1 C1 117.3(2) . . . . ? N2 Mn1 N1 C1 -63.1(3) . . . . ? N3 Mn1 N2 C3 -12.0(3) . . . . ? N4 Mn1 N2 C3 133.0(3) . . . . ? N1 Mn1 N2 C3 60.9(3) . . . . ? Cl2 Mn1 N2 C3 -117.2(3) . . . . ? Cl1 Mn1 N2 C3 64.2(9) . . . . ? N3 Mn1 N2 C4 -137.2(3) . . . . ? N4 Mn1 N2 C4 7.8(3) . . . . ? N1 Mn1 N2 C4 -64.3(3) . . . . ? Cl2 Mn1 N2 C4 117.7(3) . . . . ? Cl1 Mn1 N2 C4 -61.0(9) . . . . ? N3 Mn1 N2 C23 105.9(3) . . . . ? N4 Mn1 N2 C23 -109.1(3) . . . . ? N1 Mn1 N2 C23 178.8(3) . . . . ? Cl2 Mn1 N2 C23 0.7(3) . . . . ? Cl1 Mn1 N2 C23 -177.9(6) . . . . ? N4 Mn1 N3 C12 156.7(3) . . . . ? N1 Mn1 N3 C12 162.0(4) . . . . ? Cl2 Mn1 N3 C12 -32.2(4) . . . . ? Cl1 Mn1 N3 C12 63.6(3) . . . . ? N2 Mn1 N3 C12 -123.4(3) . . . . ? N4 Mn1 N3 C8 -14.8(4) . . . . ? N1 Mn1 N3 C8 -9.5(3) . . . . ? Cl2 Mn1 N3 C8 156.3(3) . . . . ? Cl1 Mn1 N3 C8 -107.9(3) . . . . ? N2 Mn1 N3 C8 65.1(3) . . . . ? N3 Mn1 N4 C17 -149.0(3) . . . . ? N1 Mn1 N4 C17 -154.3(4) . . . . ? Cl2 Mn1 N4 C17 40.1(4) . . . . ? Cl1 Mn1 N4 C17 -54.9(3) . . . . ? N2 Mn1 N4 C17 131.8(3) . . . . ? N3 Mn1 N4 C13 12.0(4) . . . . ? N1 Mn1 N4 C13 6.7(3) . . . . ? Cl2 Mn1 N4 C13 -158.9(3) . . . . ? Cl1 Mn1 N4 C13 106.2(3) . . . . ? N2 Mn1 N4 C13 -67.2(3) . . . . ? C22 N1 C1 C8 76.9(4) . . . . ? C6 N1 C1 C8 -163.0(3) . . . . ? Mn1 N1 C1 C8 -39.5(4) . . . . ? C22 N1 C1 C2 -161.6(4) . . . . ? C6 N1 C1 C2 -41.5(5) . . . . ? Mn1 N1 C1 C2 82.0(4) . . . . ? N1 C1 C2 C18 170.7(4) . . . . ? C8 C1 C2 C18 -68.0(4) . . . . ? N1 C1 C2 C7 48.8(5) . . . . ? C8 C1 C2 C7 170.1(3) . . . . ? N1 C1 C2 C3 -68.4(5) . . . . ? C8 C1 C2 C3 52.8(5) . . . . ? C4 N2 C3 C2 58.7(5) . . . . ? C23 N2 C3 C2 173.5(4) . . . . ? Mn1 N2 C3 C2 -67.9(4) . . . . ? C18 C2 C3 N2 -177.8(4) . . . . ? C7 C2 C3 N2 -60.2(5) . . . . ? C1 C2 C3 N2 59.7(5) . . . . ? C3 N2 C4 C5 -57.5(5) . . . . ? C23 N2 C4 C5 -172.0(4) . . . . ? Mn1 N2 C4 C5 70.4(4) . . . . ? N2 C4 C5 C7 59.0(5) . . . . ? N2 C4 C5 C20 178.2(4) . . . . ? N2 C4 C5 C6 -60.2(5) . . . . ? C22 N1 C6 C13 -73.2(4) . . . . ? C1 N1 C6 C13 167.1(3) . . . . ? Mn1 N1 C6 C13 43.2(4) . . . . ? C22 N1 C6 C5 163.1(3) . . . . ? C1 N1 C6 C5 43.3(5) . . . . ? Mn1 N1 C6 C5 -80.6(4) . . . . ? C7 C5 C6 N1 -52.0(5) . . . . ? C20 C5 C6 N1 -169.7(3) . . . . ? C4 C5 C6 N1 66.0(5) . . . . ? C7 C5 C6 C13 -174.0(3) . . . . ? C20 C5 C6 C13 68.4(4) . . . . ? C4 C5 C6 C13 -55.9(5) . . . . ? C20 C5 C7 O1 -8.1(6) . . . . ? C4 C5 C7 O1 112.4(5) . . . . ? C6 C5 C7 O1 -123.9(5) . . . . ? C20 C5 C7 C2 177.2(4) . . . . ? C4 C5 C7 C2 -62.3(4) . . . . ? C6 C5 C7 C2 61.3(4) . . . . ? C18 C2 C7 O1 3.2(6) . . . . ? C3 C2 C7 O1 -112.3(5) . . . . ? C1 C2 C7 O1 125.0(5) . . . . ? C18 C2 C7 C5 177.9(4) . . . . ? C3 C2 C7 C5 62.4(4) . . . . ? C1 C2 C7 C5 -60.3(4) . . . . ? C12 N3 C8 C9 0.0(6) . . . . ? Mn1 N3 C8 C9 171.7(3) . . . . ? C12 N3 C8 C1 178.2(4) . . . . ? Mn1 N3 C8 C1 -10.1(5) . . . . ? N1 C1 C8 N3 34.4(5) . . . . ? C2 C1 C8 N3 -90.4(4) . . . . ? N1 C1 C8 C9 -147.4(4) . . . . ? C2 C1 C8 C9 87.8(5) . . . . ? N3 C8 C9 C10 -0.1(7) . . . . ? C1 C8 C9 C10 -178.2(4) . . . . ? C8 C9 C10 C11 0.0(7) . . . . ? C9 C10 C11 C12 0.2(7) . . . . ? C8 N3 C12 C11 0.2(7) . . . . ? Mn1 N3 C12 C11 -171.4(3) . . . . ? C10 C11 C12 N3 -0.3(7) . . . . ? C17 N4 C13 C14 0.2(7) . . . . ? Mn1 N4 C13 C14 -161.2(4) . . . . ? C17 N4 C13 C6 177.6(4) . . . . ? Mn1 N4 C13 C6 16.2(5) . . . . ? N1 C6 C13 N4 -40.8(5) . . . . ? C5 C6 C13 N4 84.7(5) . . . . ? N1 C6 C13 C14 136.5(4) . . . . ? C5 C6 C13 C14 -98.0(5) . . . . ? N4 C13 C14 C15 -0.3(7) . . . . ? C6 C13 C14 C15 -177.5(5) . . . . ? C13 C14 C15 C16 0.5(8) . . . . ? C14 C15 C16 C17 -0.7(8) . . . . ? C13 N4 C17 C16 -0.4(7) . . . . ? Mn1 N4 C17 C16 160.5(4) . . . . ? C15 C16 C17 N4 0.7(8) . . . . ? C19 O3 C18 O2 0.2(7) . . . . ? C19 O3 C18 C2 178.8(4) . . . . ? C7 C2 C18 O2 -111.8(5) . . . . ? C3 C2 C18 O2 2.1(6) . . . . ? C1 C2 C18 O2 126.8(5) . . . . ? C7 C2 C18 O3 69.6(5) . . . . ? C3 C2 C18 O3 -176.5(4) . . . . ? C1 C2 C18 O3 -51.8(5) . . . . ? C21 O5 C20 O4 1.4(7) . . . . ? C21 O5 C20 C5 -179.0(4) . . . . ? C7 C5 C20 O4 -70.0(6) . . . . ? C4 C5 C20 O4 173.0(4) . . . . ? C6 C5 C20 O4 46.7(6) . . . . ? C7 C5 C20 O5 110.4(4) . . . . ? C4 C5 C20 O5 -6.6(5) . . . . ? C6 C5 C20 O5 -132.9(4) . . . . ? C35 C33 C34 C32 11.8(19) . . . . ? C35 C32 C34 C33 -10.1(16) . . . . ? C34 C33 C35 O31 91.6(16) . . . . ? C34 C33 C35 C32 -10.5(17) . . . . ? C32 C34 C35 C33 -169.0(17) . . . . ? C33 C34 C35 O31 -104.6(16) . . . . ? C32 C34 C35 O31 86.4(13) . . . . ? C33 C34 C35 C32 169.0(17) . . . . ? C34 C32 C35 C33 10.7(17) . . . . ? C34 C32 C35 O31 -100.4(15) . . . . ? _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.911 _refine_diff_density_max 0.481 _refine_diff_density_min -0.784 _refine_diff_density_rms 0.075 #======================================================================= data_hk1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H27 Cl2 Mn N4 O3' _chemical_formula_weight 533.33 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 33.5560(9) _cell_length_b 9.4762(3) _cell_length_c 31.4442(9) _cell_angle_alpha 90.00 _cell_angle_beta 109.6190(10) _cell_angle_gamma 90.00 _cell_volume 9418.3(5) _cell_formula_units_Z 16 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description polyhedron _exptl_crystal_colour colorless _exptl_crystal_size_max .19 _exptl_crystal_size_mid .10 _exptl_crystal_size_min .09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4416 _exptl_absorpt_coefficient_mu 0.821 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 0.92 _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34438 _diffrn_reflns_av_R_equivalents 0.1040 _diffrn_reflns_av_sigmaI/netI 0.1093 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.61 _reflns_number_total 8197 _reflns_number_gt 4299 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0360P)^2^+39.5908P] whereP=(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 8197 _refine_ls_number_parameters 623 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1553 _refine_ls_R_factor_gt 0.0617 _refine_ls_wR_factor_ref 0.1401 _refine_ls_wR_factor_gt 0.1082 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 1.871 _refine_ls_shift/su_mean 0.044 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 Mn31 Mn 0.08513(3) 0.67604(9) 0.09767(3) 0.0346(2) Uani 1 1 d . . . Cl31 Cl 0.09282(7) 0.5036(2) 0.04529(6) 0.0801(6) Uani 1 1 d . . . Cl32 Cl 0.06762(5) 0.49279(15) 0.14689(6) 0.0552(5) Uani 1 1 d . . . N32 N 0.09997(15) 0.8802(5) 0.05778(15) 0.0401(13) Uani 1 1 d . . . N31 N 0.08594(13) 0.8642(4) 0.14630(13) 0.0250(10) Uani 1 1 d . . . N33 N 0.01893(13) 0.7516(4) 0.07887(14) 0.0326(11) Uani 1 1 d . . . N34 N 0.15152(13) 0.6882(5) 0.14621(15) 0.0337(11) Uani 1 1 d . . . C31 C 0.06215(17) 1.0624(5) 0.08804(17) 0.0323(14) Uani 1 1 d . A . C32 C 0.06628(18) 0.9897(6) 0.04654(18) 0.0393(15) Uani 1 1 d . . . H2A H 0.0389 0.9453 0.0294 0.047 Uiso 1 1 calc R . . H2B H 0.0726 1.0616 0.0268 0.047 Uiso 1 1 calc R . . C35 C 0.13916(16) 1.0203(6) 0.12713(19) 0.0348(14) Uani 1 1 d . B . C33 C 0.1032(2) 0.8299(7) 0.0142(2) 0.060(2) Uani 1 1 d . . . H3A H 0.1098 0.9098 -0.0021 0.091 Uiso 1 1 calc R . . H3B H 0.0763 0.7876 -0.0041 0.091 Uiso 1 1 calc R . . H3C H 0.1257 0.7592 0.0202 0.091 Uiso 1 1 calc R . . C34 C 0.14056(19) 0.9472(6) 0.0845(2) 0.0462(17) Uani 1 1 d . . . H4A H 0.1484 1.0173 0.0653 0.055 Uiso 1 1 calc R . . H4B H 0.1629 0.8740 0.0931 0.055 Uiso 1 1 calc R . . C36 C 0.12991(16) 0.9218(5) 0.16181(18) 0.0312(14) Uani 1 1 d . . . H6 H 0.1337 0.9780 0.1898 0.037 Uiso 1 1 calc R . . C37 C 0.07672(17) 0.8158(6) 0.18720(17) 0.0346(14) Uani 1 1 d . . . H7A H 0.0481 0.7759 0.1781 0.052 Uiso 1 1 calc R . . H7B H 0.0786 0.8961 0.2074 0.052 Uiso 1 1 calc R . . H7C H 0.0973 0.7437 0.2029 0.052 Uiso 1 1 calc R . . C38 C 0.05092(15) 0.9626(5) 0.12084(17) 0.0266(13) Uani 1 1 d . . . H8 H 0.0440 1.0225 0.1436 0.032 Uiso 1 1 calc R . . C39 C 0.10440(18) 1.1332(6) 0.11386(19) 0.0379(15) Uani 1 1 d . . . H9 H 0.1112 1.2041 0.0937 0.045 Uiso 1 1 calc R . . O31 O 0.10431(12) 1.2018(4) 0.15429(14) 0.0499(11) Uani 1 1 d . . . H1 H 0.0797 1.2014 0.1555 0.075 Uiso 1 1 calc R . . C40 C 0.02671(18) 1.1731(6) 0.0704(2) 0.0455(17) Uani 1 1 d D . . H10A H 0.0373 1.2453 0.0541 0.055 Uiso 0.435(10) 1 calc PR A 1 H10B H 0.0028 1.1251 0.0475 0.055 Uiso 0.435(10) 1 calc PR A 1 H10C H -0.0004 1.1212 0.0581 0.055 Uiso 0.565(10) 1 d PR A 2 H10D H 0.0253 1.2279 0.0966 0.055 Uiso 0.565(10) 1 d PR A 2 O32A O 0.0111(3) 1.2400(9) 0.0968(3) 0.042(3) Uani 0.435(10) 1 d PD A 1 O32B O 0.0285(3) 1.2636(8) 0.0397(2) 0.064(3) Uani 0.565(10) 1 d PD A 2 C41 C 0.1831(2) 1.0898(7) 0.1508(3) 0.061(2) Uani 1 1 d D . . H11A H 0.1854 1.1129 0.1822 0.073 Uiso 0.551(11) 1 calc PR B 1 H11B H 0.2053 1.0197 0.1521 0.073 Uiso 0.551(11) 1 calc PR B 1 H11C H 0.2047 1.0145 0.1566 0.073 Uiso 0.449(11) 1 d PR B 2 H11D H 0.1885 1.1559 0.1289 0.073 Uiso 0.449(11) 1 d PR B 2 O33A O 0.1909(2) 1.2089(8) 0.1307(3) 0.056(3) Uani 0.551(11) 1 d PD B 1 O33B O 0.1892(3) 1.1531(11) 0.1853(4) 0.059(4) Uani 0.449(11) 1 d PD B 2 C42 C 0.01223(17) 0.8731(5) 0.09743(17) 0.0293(13) Uani 1 1 d . . . C43 C -0.02828(18) 0.9142(6) 0.09476(18) 0.0378(15) Uani 1 1 d . . . H13 H -0.0325 0.9999 0.1084 0.045 Uiso 1 1 calc R . . C44 C -0.06231(18) 0.8303(7) 0.07230(19) 0.0456(16) Uani 1 1 d . . . H14 H -0.0902 0.8575 0.0700 0.055 Uiso 1 1 calc R . . C45 C -0.05527(18) 0.7069(6) 0.05335(19) 0.0427(16) Uani 1 1 d . . . H15 H -0.0783 0.6472 0.0377 0.051 Uiso 1 1 calc R . . C46 C -0.01444(18) 0.6702(6) 0.05717(18) 0.0399(15) Uani 1 1 d . . . H16 H -0.0098 0.5843 0.0440 0.048 Uiso 1 1 calc R . . C47 C 0.16033(17) 0.7978(6) 0.17465(18) 0.0326(14) Uani 1 1 d . . . C48 C 0.19556(17) 0.7986(6) 0.2133(2) 0.0436(16) Uani 1 1 d . . . H18 H 0.2006 0.8756 0.2338 0.052 Uiso 1 1 calc R . . C49 C 0.22334(19) 0.6862(7) 0.2218(2) 0.0518(18) Uani 1 1 d . . . H19 H 0.2478 0.6857 0.2481 0.062 Uiso 1 1 calc R . . C50 C 0.21557(19) 0.5753(7) 0.1921(2) 0.0484(17) Uani 1 1 d . . . H20 H 0.2349 0.4987 0.1968 0.058 Uiso 1 1 calc R . . C51 C 0.17901(19) 0.5785(6) 0.1555(2) 0.0437(16) Uani 1 1 d . . . H21 H 0.1726 0.4997 0.1357 0.052 Uiso 1 1 calc R . . Mn1 Mn 0.14938(3) 1.79804(8) -0.15294(3) 0.0322(2) Uani 1 1 d . . . Cl1 Cl 0.15841(6) 1.98501(16) -0.20199(6) 0.0619(5) Uani 1 1 d . . . Cl2 Cl 0.15225(5) 1.97309(15) -0.09121(5) 0.0505(4) Uani 1 1 d . . . N2 N 0.15078(14) 1.6088(4) -0.20492(14) 0.0316(11) Uani 1 1 d . . . N1 N 0.13235(13) 1.5982(4) -0.11851(14) 0.0273(11) Uani 1 1 d . . . N3 N 0.21074(14) 1.7159(5) -0.10601(15) 0.0345(11) Uani 1 1 d . . . N4 N 0.07896(14) 1.7843(5) -0.17511(14) 0.0336(11) Uani 1 1 d . . . C1 C 0.17335(17) 1.4142(5) -0.14690(18) 0.0305(14) Uani 1 1 d . . . C2 C 0.18321(17) 1.5015(5) -0.18303(18) 0.0328(14) Uani 1 1 d . . . H32A H 0.2107 1.5496 -0.1690 0.039 Uiso 1 1 calc R . . H32B H 0.1862 1.4369 -0.2065 0.039 Uiso 1 1 calc R . . C3 C 0.16137(19) 1.6696(6) -0.24316(19) 0.0463(16) Uani 1 1 d . . . H33A H 0.1889 1.7168 -0.2317 0.069 Uiso 1 1 calc R . . H33B H 0.1397 1.7383 -0.2591 0.069 Uiso 1 1 calc R . . H33C H 0.1626 1.5941 -0.2640 0.069 Uiso 1 1 calc R . . C4 C 0.10968(17) 1.5369(6) -0.22348(18) 0.0355(14) Uani 1 1 d . . . H34A H 0.1106 1.4733 -0.2481 0.043 Uiso 1 1 calc R . . H34B H 0.0875 1.6085 -0.2368 0.043 Uiso 1 1 calc R . . C5 C 0.09709(17) 1.4510(6) -0.18909(18) 0.0336(14) Uani 1 1 d . . . C6 C 0.09192(16) 1.5401(5) -0.14994(17) 0.0309(13) Uani 1 1 d . . . H36 H 0.0795 1.4777 -0.1320 0.037 Uiso 1 1 calc R . . C7 C 0.12502(18) 1.6370(6) -0.07631(18) 0.0394(15) Uani 1 1 d . . . H37A H 0.1010 1.7021 -0.0831 0.059 Uiso 1 1 calc R . . H37B H 0.1504 1.6828 -0.0558 0.059 Uiso 1 1 calc R . . H37C H 0.1188 1.5518 -0.0620 0.059 Uiso 1 1 calc R . . C8 C 0.16990(16) 1.5024(5) -0.10685(17) 0.0304(13) Uani 1 1 d . . . H38 H 0.1676 1.4350 -0.0833 0.036 Uiso 1 1 calc R . . C9 C 0.13127(17) 1.3393(6) -0.16884(19) 0.0362(14) Uani 1 1 d . . . H39 H 0.1335 1.2770 -0.1936 0.043 Uiso 1 1 calc R . . O1 O 0.11952(12) 1.2565(4) -0.13752(14) 0.0497(11) Uani 1 1 d . . . H31 H 0.0932 1.2443 -0.1471 0.075 Uiso 1 1 calc R . . C10 C 0.20977(18) 1.3070(6) -0.1271(2) 0.0432(16) Uani 1 1 d . . . H40A H 0.2351 1.3583 -0.1079 0.052 Uiso 1 1 calc R . . H40B H 0.2014 1.2394 -0.1076 0.052 Uiso 1 1 calc R . . O2 O 0.22047(13) 1.2303(4) -0.16069(16) 0.0564(12) Uani 1 1 d . . . H32 H 0.2029 1.1649 -0.1707 0.085 Uiso 1 1 calc R . . C11 C 0.05500(18) 1.3775(7) -0.2155(2) 0.0499(17) Uani 1 1 d . . . H41A H 0.0350 1.4493 -0.2336 0.060 Uiso 1 1 calc R . . H41B H 0.0603 1.3092 -0.2369 0.060 Uiso 1 1 calc R . . O3 O 0.03574(13) 1.3054(5) -0.18819(15) 0.0614(13) Uani 1 1 d . . . H33 H 0.0093 1.3136 -0.1994 0.092 Uiso 1 1 calc R . . C12 C 0.20910(17) 1.5934(6) -0.08531(18) 0.0331(14) Uani 1 1 d . . . C13 C 0.24135(19) 1.5513(7) -0.04616(19) 0.0441(16) Uani 1 1 d . . . H43 H 0.2392 1.4654 -0.0315 0.053 Uiso 1 1 calc R . . C14 C 0.27633(19) 1.6366(7) -0.0291(2) 0.0507(18) Uani 1 1 d . . . H44 H 0.2988 1.6097 -0.0028 0.061 Uiso 1 1 calc R . . C15 C 0.27831(19) 1.7605(7) -0.0507(2) 0.0532(18) Uani 1 1 d . . . H45 H 0.3022 1.8205 -0.0395 0.064 Uiso 1 1 calc R . . C16 C 0.24502(18) 1.7972(6) -0.0889(2) 0.0434(16) Uani 1 1 d . . . H46 H 0.2465 1.8836 -0.1035 0.052 Uiso 1 1 calc R . . C17 C 0.06170(17) 1.6636(6) -0.16752(18) 0.0335(14) Uani 1 1 d . . . C18 C 0.01883(18) 1.6516(7) -0.1745(2) 0.0446(16) Uani 1 1 d . . . H48 H 0.0072 1.5647 -0.1691 0.054 Uiso 1 1 calc R . . C19 C -0.0067(2) 1.7677(8) -0.1894(2) 0.0522(18) Uani 1 1 d . . . H49 H -0.0361 1.7621 -0.1942 0.063 Uiso 1 1 calc R . . C20 C 0.0110(2) 1.8921(8) -0.1972(2) 0.0522(18) Uani 1 1 d . . . H50 H -0.0062 1.9733 -0.2076 0.063 Uiso 1 1 calc R . . C21 C 0.05391(19) 1.8973(6) -0.18988(18) 0.0428(16) Uani 1 1 d . . . H51 H 0.0661 1.9830 -0.1954 0.051 Uiso 1 1 calc R . . C100 C 0.1939(5) 2.2140(10) -0.0214(3) 0.144(5) Uani 1 1 d . . . C101 C 0.1776(3) 2.2307(10) 0.0064(4) 0.087(3) Uani 1 1 d . . . C102 C 0.2008(7) 2.3580(16) 0.0389(5) 0.204(11) Uani 1 1 d . . . C103 C 0.1814(8) 2.415(3) 0.0345(9) 0.349(18) 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 Mn31 0.0328(5) 0.0329(5) 0.0342(5) -0.0075(4) 0.0061(4) 0.0058(4) Cl31 0.1024(17) 0.0707(13) 0.0690(13) -0.0337(11) 0.0314(12) 0.0092(11) Cl32 0.0612(11) 0.0322(9) 0.0691(12) 0.0047(8) 0.0178(9) -0.0014(8) N32 0.044(3) 0.051(3) 0.030(3) 0.005(2) 0.018(3) 0.010(3) N31 0.025(3) 0.022(2) 0.025(3) 0.0020(19) 0.006(2) 0.0025(19) N33 0.030(3) 0.031(3) 0.033(3) -0.008(2) 0.006(2) 0.002(2) N34 0.030(3) 0.037(3) 0.035(3) 0.005(2) 0.012(2) 0.005(2) C31 0.031(3) 0.035(3) 0.026(3) 0.002(3) 0.004(3) 0.005(3) C32 0.044(4) 0.045(4) 0.028(3) 0.008(3) 0.012(3) 0.010(3) C35 0.025(3) 0.036(3) 0.042(4) 0.008(3) 0.010(3) -0.001(3) C33 0.071(5) 0.082(5) 0.037(4) 0.002(4) 0.029(4) 0.027(4) C34 0.044(4) 0.055(4) 0.047(4) 0.022(3) 0.025(3) 0.016(3) C36 0.031(4) 0.035(3) 0.026(3) -0.001(3) 0.008(3) -0.001(3) C37 0.038(4) 0.042(4) 0.026(3) 0.009(3) 0.015(3) 0.003(3) C38 0.024(3) 0.030(3) 0.023(3) -0.007(2) 0.004(2) 0.004(2) C39 0.041(4) 0.032(3) 0.036(4) 0.012(3) 0.006(3) 0.002(3) O31 0.042(3) 0.042(3) 0.055(3) -0.007(2) 0.002(2) 0.000(2) C40 0.034(4) 0.038(4) 0.052(4) 0.002(4) -0.001(3) 0.000(3) O32A 0.038(6) 0.037(6) 0.049(7) 0.004(5) 0.014(5) 0.018(4) O32B 0.084(7) 0.064(6) 0.050(5) 0.039(4) 0.030(5) 0.027(5) C41 0.034(4) 0.050(5) 0.096(7) 0.028(5) 0.020(4) -0.002(3) O33A 0.042(5) 0.049(6) 0.074(6) 0.022(4) 0.014(4) -0.007(4) O33B 0.053(7) 0.066(8) 0.055(8) -0.020(6) 0.015(6) -0.017(5) C42 0.029(3) 0.034(3) 0.025(3) -0.002(3) 0.009(3) 0.005(3) C43 0.032(4) 0.043(4) 0.037(4) -0.007(3) 0.011(3) 0.007(3) C44 0.026(4) 0.072(5) 0.037(4) -0.004(3) 0.009(3) -0.002(3) C45 0.033(4) 0.049(4) 0.041(4) -0.004(3) 0.005(3) -0.008(3) C46 0.034(4) 0.038(4) 0.040(4) -0.009(3) 0.003(3) 0.003(3) C47 0.030(3) 0.035(3) 0.031(3) 0.006(3) 0.008(3) 0.003(3) C48 0.029(4) 0.049(4) 0.047(4) 0.006(3) 0.007(3) -0.001(3) C49 0.030(4) 0.067(5) 0.055(4) 0.019(4) 0.009(3) 0.000(4) C50 0.038(4) 0.052(4) 0.056(4) 0.017(4) 0.017(4) 0.020(3) C51 0.044(4) 0.040(4) 0.053(4) 0.006(3) 0.024(4) 0.016(3) Mn1 0.0332(5) 0.0276(5) 0.0334(5) -0.0008(4) 0.0080(4) 0.0014(4) Cl1 0.1008(15) 0.0344(9) 0.0543(11) 0.0045(8) 0.0309(10) -0.0032(9) Cl2 0.0664(12) 0.0352(9) 0.0432(10) -0.0081(7) 0.0095(8) 0.0104(8) N2 0.034(3) 0.030(3) 0.031(3) 0.000(2) 0.010(2) 0.003(2) N1 0.026(3) 0.031(3) 0.025(3) -0.002(2) 0.009(2) 0.001(2) N3 0.033(3) 0.033(3) 0.035(3) -0.007(2) 0.008(2) -0.004(2) N4 0.032(3) 0.035(3) 0.029(3) -0.005(2) 0.005(2) 0.006(2) C1 0.030(3) 0.023(3) 0.038(3) 0.001(3) 0.010(3) 0.007(2) C2 0.032(3) 0.028(3) 0.041(4) -0.007(3) 0.015(3) 0.003(3) C3 0.062(4) 0.044(4) 0.039(4) 0.002(3) 0.025(3) -0.005(3) C4 0.041(4) 0.031(3) 0.032(3) -0.006(3) 0.007(3) 0.005(3) C5 0.031(3) 0.030(3) 0.039(4) -0.006(3) 0.010(3) -0.004(3) C6 0.031(3) 0.032(3) 0.030(3) 0.000(3) 0.010(3) 0.002(3) C7 0.045(4) 0.047(4) 0.034(4) -0.005(3) 0.023(3) -0.001(3) C8 0.029(3) 0.032(3) 0.029(3) 0.006(3) 0.008(3) 0.004(3) C9 0.039(4) 0.028(3) 0.044(4) -0.006(3) 0.016(3) -0.005(3) O1 0.037(3) 0.044(3) 0.071(3) 0.007(2) 0.021(2) -0.007(2) C10 0.039(4) 0.034(3) 0.054(4) -0.007(3) 0.011(3) 0.003(3) O2 0.048(3) 0.042(3) 0.081(3) -0.008(2) 0.024(3) 0.008(2) C11 0.035(4) 0.054(4) 0.059(5) -0.011(3) 0.014(3) -0.003(3) O3 0.036(3) 0.069(3) 0.078(3) -0.007(3) 0.016(2) -0.020(3) C12 0.033(4) 0.041(4) 0.026(3) -0.001(3) 0.012(3) 0.007(3) C13 0.042(4) 0.049(4) 0.038(4) 0.002(3) 0.009(3) 0.008(3) C14 0.036(4) 0.062(5) 0.043(4) -0.008(4) -0.001(3) 0.013(3) C15 0.032(4) 0.052(4) 0.064(5) -0.020(4) 0.001(4) -0.001(3) C16 0.041(4) 0.038(4) 0.049(4) -0.005(3) 0.013(3) 0.001(3) C17 0.027(4) 0.042(4) 0.030(3) -0.010(3) 0.008(3) -0.002(3) C18 0.031(4) 0.050(4) 0.051(4) -0.015(3) 0.013(3) 0.002(3) C19 0.033(4) 0.073(5) 0.047(4) -0.013(4) 0.009(3) 0.009(4) C20 0.047(5) 0.065(5) 0.040(4) -0.008(3) 0.009(3) 0.029(4) C21 0.047(4) 0.042(4) 0.036(4) -0.003(3) 0.010(3) 0.018(3) C100 0.262(16) 0.062(6) 0.063(7) -0.003(5) -0.003(8) -0.036(8) C101 0.074(6) 0.075(7) 0.136(10) 0.011(7) 0.065(7) 0.012(5) C102 0.41(3) 0.131(11) 0.137(12) 0.084(10) 0.172(15) 0.194(16) C103 0.35(3) 0.38(3) 0.37(3) -0.22(3) 0.19(3) -0.27(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 Mn31 N33 2.217(4) . ? Mn31 N34 2.241(4) . ? Mn31 N31 2.343(4) . ? Mn31 Cl31 2.3946(19) . ? Mn31 N32 2.446(5) . ? Mn31 Cl32 2.5233(18) . ? N32 C34 1.482(7) . ? N32 C32 1.487(6) . ? N32 C33 1.488(7) . ? N31 C37 1.492(6) . ? N31 C36 1.493(6) . ? N31 C38 1.503(6) . ? N33 C46 1.342(6) . ? N33 C42 1.343(6) . ? N34 C47 1.337(6) . ? N34 C51 1.355(7) . ? C31 C32 1.523(7) . ? C31 C39 1.532(7) . ? C31 C38 1.537(7) . ? C31 C40 1.543(7) . ? C35 C34 1.523(8) . ? C35 C39 1.534(7) . ? C35 C36 1.544(7) . ? C35 C41 1.556(8) . ? C36 C47 1.519(7) . ? C38 C42 1.518(7) . ? C39 O31 1.429(6) . ? C40 O32A 1.288(9) . ? C40 O32B 1.306(8) . ? C41 O33B 1.197(10) . ? C41 O33A 1.360(8) . ? C42 C43 1.389(7) . ? C43 C44 1.376(7) . ? C44 C45 1.368(8) . ? C45 C46 1.379(7) . ? C47 C48 1.382(7) . ? C48 C49 1.382(8) . ? C49 C50 1.370(8) . ? C50 C51 1.372(8) . ? Mn1 N3 2.232(4) . ? Mn1 N4 2.232(4) . ? Mn1 N1 2.345(4) . ? Mn1 Cl1 2.4339(18) . ? Mn1 N2 2.437(4) . ? Mn1 Cl2 2.5304(17) . ? N2 C4 1.472(6) . ? N2 C2 1.479(6) . ? N2 C3 1.480(6) . ? N1 C7 1.475(6) . ? N1 C6 1.490(6) . ? N1 C8 1.495(6) . ? N3 C16 1.338(7) . ? N3 C12 1.342(6) . ? N4 C17 1.340(7) . ? N4 C21 1.344(6) . ? C1 C9 1.523(7) . ? C1 C2 1.529(7) . ? C1 C8 1.548(7) . ? C1 C10 1.550(7) . ? C4 C5 1.522(7) . ? C5 C9 1.533(7) . ? C5 C11 1.544(7) . ? C5 C6 1.549(7) . ? C6 C17 1.526(7) . ? C8 C12 1.528(7) . ? C9 O1 1.415(6) . ? C10 O2 1.425(6) . ? C11 O3 1.413(7) . ? C12 C13 1.397(7) . ? C13 C14 1.377(8) . ? C14 C15 1.368(8) . ? C15 C16 1.382(8) . ? C17 C18 1.385(7) . ? C18 C19 1.375(8) . ? C19 C20 1.378(9) . ? C20 C21 1.382(8) . ? C100 C101 1.187(13) . ? C101 C102 1.60(2) . ? C101 C103 1.94(2) . ? C102 C103 0.82(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N33 Mn31 N34 147.44(16) . . ? N33 Mn31 N31 73.70(15) . . ? N34 Mn31 N31 74.05(15) . . ? N33 Mn31 Cl31 111.52(12) . . ? N34 Mn31 Cl31 101.04(13) . . ? N31 Mn31 Cl31 171.02(12) . . ? N33 Mn31 N32 88.06(16) . . ? N34 Mn31 N32 88.94(16) . . ? N31 Mn31 N32 76.89(15) . . ? Cl31 Mn31 N32 95.70(12) . . ? N33 Mn31 Cl32 88.11(12) . . ? N34 Mn31 Cl32 90.03(12) . . ? N31 Mn31 Cl32 94.44(11) . . ? Cl31 Mn31 Cl32 93.06(7) . . ? N32 Mn31 Cl32 171.21(12) . . ? C34 N32 C32 108.4(4) . . ? C34 N32 C33 108.8(5) . . ? C32 N32 C33 106.8(4) . . ? C34 N32 Mn31 110.8(3) . . ? C32 N32 Mn31 113.9(3) . . ? C33 N32 Mn31 108.0(4) . . ? C37 N31 C36 107.4(4) . . ? C37 N31 C38 107.3(4) . . ? C36 N31 C38 117.2(4) . . ? C37 N31 Mn31 111.6(3) . . ? C36 N31 Mn31 106.6(3) . . ? C38 N31 Mn31 106.8(3) . . ? C46 N33 C42 118.7(5) . . ? C46 N33 Mn31 122.7(4) . . ? C42 N33 Mn31 117.4(3) . . ? C47 N34 C51 118.0(5) . . ? C47 N34 Mn31 116.2(3) . . ? C51 N34 Mn31 123.8(4) . . ? C32 C31 C39 108.5(5) . . ? C32 C31 C38 114.2(4) . . ? C39 C31 C38 107.8(4) . . ? C32 C31 C40 106.3(4) . . ? C39 C31 C40 110.9(4) . . ? C38 C31 C40 109.1(5) . . ? N32 C32 C31 113.1(4) . . ? C34 C35 C39 108.8(5) . . ? C34 C35 C36 114.8(5) . . ? C39 C35 C36 107.4(4) . . ? C34 C35 C41 108.0(5) . . ? C39 C35 C41 110.2(5) . . ? C36 C35 C41 107.5(5) . . ? N32 C34 C35 113.6(4) . . ? N31 C36 C47 107.8(4) . . ? N31 C36 C35 113.7(4) . . ? C47 C36 C35 112.2(4) . . ? N31 C38 C42 107.5(4) . . ? N31 C38 C31 114.5(4) . . ? C42 C38 C31 112.4(4) . . ? O31 C39 C31 113.1(5) . . ? O31 C39 C35 107.7(4) . . ? C31 C39 C35 108.8(4) . . ? O32A C40 O32B 106.4(7) . . ? O32A C40 C31 122.2(6) . . ? O32B C40 C31 119.5(6) . . ? O33B C41 O33A 90.2(8) . . ? O33B C41 C35 119.5(8) . . ? O33A C41 C35 115.4(6) . . ? N33 C42 C43 121.2(5) . . ? N33 C42 C38 116.7(5) . . ? C43 C42 C38 122.2(5) . . ? C44 C43 C42 119.7(5) . . ? C45 C44 C43 118.8(6) . . ? C44 C45 C46 119.3(5) . . ? N33 C46 C45 122.3(5) . . ? N34 C47 C48 121.6(5) . . ? N34 C47 C36 116.4(5) . . ? C48 C47 C36 122.0(5) . . ? C47 C48 C49 119.2(6) . . ? C50 C49 C48 119.9(6) . . ? C49 C50 C51 117.8(6) . . ? N34 C51 C50 123.4(6) . . ? N3 Mn1 N4 146.23(17) . . ? N3 Mn1 N1 74.17(16) . . ? N4 Mn1 N1 72.58(16) . . ? N3 Mn1 Cl1 112.90(13) . . ? N4 Mn1 Cl1 100.86(13) . . ? N1 Mn1 Cl1 169.05(11) . . ? N3 Mn1 N2 88.04(15) . . ? N4 Mn1 N2 90.26(15) . . ? N1 Mn1 N2 77.18(14) . . ? Cl1 Mn1 N2 94.36(11) . . ? N3 Mn1 Cl2 86.12(12) . . ? N4 Mn1 Cl2 92.37(12) . . ? N1 Mn1 Cl2 97.34(11) . . ? Cl1 Mn1 Cl2 91.61(6) . . ? N2 Mn1 Cl2 172.91(11) . . ? C4 N2 C2 108.1(4) . . ? C4 N2 C3 107.9(4) . . ? C2 N2 C3 107.8(4) . . ? C4 N2 Mn1 112.3(3) . . ? C2 N2 Mn1 111.7(3) . . ? C3 N2 Mn1 108.8(3) . . ? C7 N1 C6 107.4(4) . . ? C7 N1 C8 108.2(4) . . ? C6 N1 C8 116.3(4) . . ? C7 N1 Mn1 110.7(3) . . ? C6 N1 Mn1 107.5(3) . . ? C8 N1 Mn1 106.7(3) . . ? C16 N3 C12 118.2(5) . . ? C16 N3 Mn1 122.9(4) . . ? C12 N3 Mn1 116.3(4) . . ? C17 N4 C21 119.0(5) . . ? C17 N4 Mn1 118.0(4) . . ? C21 N4 Mn1 122.4(4) . . ? C9 C1 C2 108.3(4) . . ? C9 C1 C8 108.0(4) . . ? C2 C1 C8 113.9(4) . . ? C9 C1 C10 111.3(4) . . ? C2 C1 C10 108.4(4) . . ? C8 C1 C10 106.9(4) . . ? N2 C2 C1 114.1(4) . . ? N2 C4 C5 114.4(4) . . ? C4 C5 C9 108.5(4) . . ? C4 C5 C11 106.3(5) . . ? C9 C5 C11 109.5(4) . . ? C4 C5 C6 113.9(4) . . ? C9 C5 C6 108.3(4) . . ? C11 C5 C6 110.3(4) . . ? N1 C6 C17 107.6(4) . . ? N1 C6 C5 114.1(4) . . ? C17 C6 C5 111.6(4) . . ? N1 C8 C12 107.2(4) . . ? N1 C8 C1 114.5(4) . . ? C12 C8 C1 112.1(4) . . ? O1 C9 C1 112.1(4) . . ? O1 C9 C5 109.1(4) . . ? C1 C9 C5 108.5(4) . . ? O2 C10 C1 113.4(5) . . ? O3 C11 C5 114.4(5) . . ? N3 C12 C13 121.9(5) . . ? N3 C12 C8 116.3(5) . . ? C13 C12 C8 121.8(5) . . ? C14 C13 C12 118.9(6) . . ? C15 C14 C13 119.2(6) . . ? C14 C15 C16 119.1(6) . . ? N3 C16 C15 122.7(6) . . ? N4 C17 C18 122.0(5) . . ? N4 C17 C6 116.4(5) . . ? C18 C17 C6 121.5(5) . . ? C19 C18 C17 118.8(6) . . ? C18 C19 C20 119.4(6) . . ? C19 C20 C21 119.1(6) . . ? N4 C21 C20 121.7(6) . . ? C100 C101 C102 108.9(11) . . ? C100 C101 C103 118.6(11) . . ? C102 C101 C103 24.5(12) . . ? C103 C102 C101 102(3) . . ? C102 C103 C101 54(2) . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 25.61 _diffrn_measured_fraction_theta_full 0.921 _refine_diff_density_max 0.512 _refine_diff_density_min -0.442 _refine_diff_density_rms 0.079