Electronic Supplementary Material for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full J.Mater.Chem. _journal_coden_cambridge 1145 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name G.Aromi U.Behrens S.K.Chandra H.-K.Fun B.K.Ghosh T.K.Karmakar ; T.Mallah ; X.Solans A.Usman _publ_contact_author_name 'Guillem Aromi' _publ_contact_author_email GUILLEM.AROMI@QI.UB.ES data_tm45m _database_code_depnum_ccdc_archive 'CCDC 279584' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H42 Mn2 N15, 3(Cl O4)' _chemical_formula_sum 'C42 H42 Cl3 Mn2 N15 O12' _chemical_formula_weight 1165.12 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 19.5706(3) _cell_length_b 20.7246(5) _cell_length_c 14.1497(3) _cell_angle_alpha 90.00 _cell_angle_beta 118.309(1) _cell_angle_gamma 90.00 _cell_volume 5052.65(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6523 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 28.37 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2408 _exptl_absorpt_coefficient_mu 0.734 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7104 _exptl_absorpt_correction_T_max 0.8321 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The data collection covered over a hemisphere of reciprocal space by a combination of three sets of exposures; each set had a different \f angle (0, 88 and 180\%) for the crystal and each exposure of 30s covered 0.3\% in \w. The crystal-to-detector distance was 5 cm and the detector swing angle was -35\%. Crystal decay was monitored by repeating fifty initial frames at the end of data collection and analysing the intensity of duplicate reflections, and was found to be negligible. ; _diffrn_ambient_temperature 183(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 ; Siemens SMART CCD area detector 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_% negligible _diffrn_reflns_number 14878 _diffrn_reflns_av_R_equivalents 0.1317 _diffrn_reflns_av_sigmaI/netI 0.1672 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 28.31 _reflns_number_total 6147 _reflns_number_gt 2503 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 1997)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material ; SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 1990) ; _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^)+(0.1192P)^2^] 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 SHELXL _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6147 _refine_ls_number_parameters 337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1684 _refine_ls_R_factor_gt 0.0877 _refine_ls_wR_factor_ref 0.2506 _refine_ls_wR_factor_gt 0.2214 _refine_ls_goodness_of_fit_ref 0.876 _refine_ls_restrained_S_all 0.876 _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 0.26670(4) 0.25033(3) 0.24139(6) 0.0538(3) Uani 1 1 d . . . Cl1 Cl 0.30724(11) -0.00130(8) 0.03717(14) 0.0868(5) Uani 1 1 d . . . Cl2 Cl 0.0000 0.11423(11) 0.2500 0.0835(7) Uani 1 2 d S . . O1 O 0.2474(8) 0.0325(8) 0.0179(9) 0.346(8) Uani 1 1 d . . . O2 O 0.3217(6) 0.0149(4) -0.0450(6) 0.233(4) Uani 1 1 d . . . O3 O 0.3697(6) 0.0159(3) 0.1359(6) 0.235(5) Uani 1 1 d . . . O4 O 0.3006(5) -0.0691(3) 0.0323(6) 0.184(3) Uani 1 1 d . . . O5 O 0.0020(6) 0.0829(4) 0.1727(7) 0.245(5) Uani 1 1 d . . . O7 O 0.0568(6) 0.1573(5) 0.2983(5) 0.267(5) Uani 1 1 d . . . N1 N 0.2931(2) 0.14189(18) 0.2798(3) 0.0613(11) Uani 1 1 d . . . N2 N 0.1550(3) 0.19452(19) 0.1582(4) 0.0656(11) Uani 1 1 d . . . N3 N 0.2917(3) 0.2762(2) 0.4114(4) 0.0660(12) Uani 1 1 d . . . N4 N 0.3215(2) 0.34927(18) 0.2759(3) 0.0527(10) Uani 1 1 d . . . N5 N 0.2681(3) 0.2520(3) 0.0878(4) 0.0901(17) Uani 1 1 d . . . N8 N 0.4147(2) 0.2220(2) 0.3311(3) 0.0539(10) Uani 1 1 d . . . N7 N 0.1433(3) 0.3210(2) 0.1868(3) 0.0644(11) Uani 1 1 d . . . N6 N 0.2500 0.2500 0.0000 0.0494(13) Uani 1 2 d S . . C1 C 0.4762(3) 0.2616(3) 0.3564(4) 0.0649(14) Uani 1 1 d . . . H1A H 0.4686 0.3060 0.3507 0.078 Uiso 1 1 calc R . . C2 C 0.5490(3) 0.2374(3) 0.3902(4) 0.0720(16) Uani 1 1 d . . . H2A H 0.5900 0.2655 0.4056 0.086 Uiso 1 1 calc R . . C3 C 0.5624(3) 0.1722(3) 0.4019(4) 0.0765(17) Uani 1 1 d . . . H3A H 0.6122 0.1557 0.4264 0.092 Uiso 1 1 calc R . . C4 C 0.5011(3) 0.1321(3) 0.3767(4) 0.0729(16) Uani 1 1 d . . . H4A H 0.5082 0.0876 0.3827 0.087 Uiso 1 1 calc R . . C5 C 0.4274(3) 0.1587(3) 0.3418(4) 0.0582(13) Uani 1 1 d . . . C6 C 0.3601(3) 0.1181(3) 0.3127(4) 0.0687(15) Uani 1 1 d . . . H6A H 0.3663 0.0735 0.3184 0.082 Uiso 1 1 calc R . . C7 C 0.2260(3) 0.0988(3) 0.2453(6) 0.0862(19) Uani 1 1 d . . . H7B H 0.2077 0.0984 0.2981 0.103 Uiso 1 1 calc R . . H7C H 0.2398 0.0552 0.2363 0.103 Uiso 1 1 calc R . . C8 C 0.1646(4) 0.1249(3) 0.1405(5) 0.0848(18) Uani 1 1 d . . . H8B H 0.1802 0.1201 0.0853 0.102 Uiso 1 1 calc R . . H8C H 0.1161 0.1019 0.1180 0.102 Uiso 1 1 calc R . . C9 C 0.0885(3) 0.2179(3) 0.1302(4) 0.0660(14) Uani 1 1 d . . . H9A H 0.0450 0.1914 0.0986 0.079 Uiso 1 1 calc R . . C10 C 0.0797(3) 0.2848(2) 0.1467(4) 0.0538(12) Uani 1 1 d . . . C11 C 0.0067(3) 0.3108(3) 0.1154(4) 0.0655(14) Uani 1 1 d . . . H11A H -0.0371 0.2846 0.0862 0.079 Uiso 1 1 calc R . . C12 C 0.0003(4) 0.3748(3) 0.1281(5) 0.0827(18) Uani 1 1 d . . . H12A H -0.0477 0.3934 0.1096 0.099 Uiso 1 1 calc R . . C13 C 0.0662(4) 0.4118(3) 0.1688(5) 0.0869(19) Uani 1 1 d . . . H13A H 0.0635 0.4560 0.1775 0.104 Uiso 1 1 calc R . . C14 C 0.1361(4) 0.3830(3) 0.1966(5) 0.0818(17) Uani 1 1 d . . . H14A H 0.1803 0.4087 0.2237 0.098 Uiso 1 1 calc R . . C15 C 0.3375(3) 0.3852(3) 0.2096(5) 0.0748(16) Uani 1 1 d . . . H15A H 0.3186 0.3731 0.1383 0.090 Uiso 1 1 calc R . . C16 C 0.3829(4) 0.4410(3) 0.2491(7) 0.096(2) Uani 1 1 d . . . H16A H 0.3958 0.4650 0.2043 0.115 Uiso 1 1 calc R . . C17 C 0.4078(4) 0.4600(3) 0.3505(7) 0.100(2) Uani 1 1 d . . . H17A H 0.4381 0.4970 0.3759 0.120 Uiso 1 1 calc R . . C18 C 0.3891(4) 0.4258(3) 0.4158(5) 0.0835(17) Uani 1 1 d . . . H18A H 0.4048 0.4389 0.4860 0.100 Uiso 1 1 calc R . . C19 C 0.3458(3) 0.3706(2) 0.3743(4) 0.0554(12) Uani 1 1 d . . . C20 C 0.3246(3) 0.3299(3) 0.4445(4) 0.0699(15) Uani 1 1 d . . . H20A H 0.3357 0.3445 0.5125 0.084 Uiso 1 1 calc R . . C21 C 0.2759(6) 0.2358(3) 0.4842(8) 0.148(4) Uani 1 1 d . . . H21A H 0.2544 0.1950 0.4491 0.222 Uiso 1 1 d R . . H21B H 0.3246 0.2267 0.5479 0.222 Uiso 1 1 d 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 Mn1 0.0540(5) 0.0540(5) 0.0663(5) 0.0000(3) 0.0390(4) -0.0060(3) Cl1 0.0967(13) 0.0769(11) 0.0858(11) 0.0127(8) 0.0425(10) 0.0148(9) Cl2 0.0817(16) 0.0714(14) 0.1159(18) 0.000 0.0621(14) 0.000 O1 0.305(13) 0.495(19) 0.263(12) 0.102(10) 0.155(10) 0.293(13) O2 0.311(11) 0.291(10) 0.151(6) -0.011(6) 0.155(7) -0.089(8) O3 0.317(11) 0.158(6) 0.135(6) -0.018(4) 0.030(7) -0.051(7) O4 0.187(8) 0.113(5) 0.225(7) -0.010(4) 0.075(6) -0.025(5) O5 0.318(13) 0.188(7) 0.221(7) -0.086(6) 0.121(8) 0.068(7) O7 0.292(11) 0.380(11) 0.132(6) -0.048(6) 0.103(6) -0.228(10) N1 0.050(3) 0.050(2) 0.088(3) -0.002(2) 0.036(2) -0.0011(19) N2 0.059(3) 0.057(3) 0.093(3) -0.003(2) 0.045(2) -0.003(2) N3 0.084(3) 0.055(2) 0.096(3) 0.007(2) 0.072(3) 0.004(2) N4 0.047(2) 0.055(2) 0.066(3) 0.014(2) 0.035(2) 0.0002(18) N5 0.078(4) 0.140(5) 0.065(3) -0.002(3) 0.045(3) 0.006(3) N8 0.042(2) 0.067(3) 0.062(2) 0.010(2) 0.032(2) 0.0071(19) N7 0.052(3) 0.054(3) 0.089(3) 0.000(2) 0.035(2) 0.009(2) N6 0.030(3) 0.063(3) 0.064(4) 0.000(3) 0.030(3) -0.006(2) C1 0.049(3) 0.082(4) 0.070(3) 0.009(3) 0.034(3) 0.001(3) C2 0.045(3) 0.110(5) 0.069(3) 0.005(3) 0.034(3) 0.002(3) C3 0.040(3) 0.122(5) 0.071(4) 0.012(3) 0.030(3) 0.019(3) C4 0.067(4) 0.080(4) 0.078(4) 0.007(3) 0.039(3) 0.029(3) C5 0.056(3) 0.070(3) 0.058(3) 0.007(2) 0.035(3) 0.016(3) C6 0.069(4) 0.056(3) 0.090(4) 0.009(3) 0.045(3) 0.015(3) C7 0.073(4) 0.049(3) 0.149(6) 0.007(3) 0.063(4) 0.001(3) C8 0.077(4) 0.054(3) 0.129(5) -0.010(3) 0.054(4) -0.006(3) C9 0.046(3) 0.072(4) 0.087(4) 0.012(3) 0.037(3) -0.004(3) C10 0.047(3) 0.058(3) 0.068(3) -0.001(2) 0.038(3) -0.001(2) C11 0.049(3) 0.083(4) 0.072(3) 0.006(3) 0.035(3) 0.008(3) C12 0.072(4) 0.103(5) 0.078(4) 0.002(4) 0.040(3) 0.029(4) C13 0.085(5) 0.064(4) 0.103(5) -0.003(3) 0.037(4) 0.023(3) C14 0.067(4) 0.067(4) 0.103(4) -0.017(3) 0.033(4) -0.001(3) C15 0.078(4) 0.072(4) 0.092(4) 0.032(3) 0.055(3) 0.010(3) C16 0.098(5) 0.062(4) 0.150(7) 0.037(4) 0.076(5) -0.004(4) C17 0.096(6) 0.063(4) 0.145(7) 0.000(4) 0.060(5) -0.024(3) C18 0.079(4) 0.072(4) 0.098(4) -0.007(3) 0.042(4) -0.013(3) C19 0.047(3) 0.057(3) 0.067(3) 0.002(2) 0.030(2) -0.004(2) C20 0.088(4) 0.071(4) 0.076(4) -0.006(3) 0.060(3) 0.003(3) C21 0.238(11) 0.108(6) 0.232(10) 0.051(6) 0.221(10) 0.047(6) _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 N5 2.186(5) . ? Mn1 N2 2.250(4) . ? Mn1 N4 2.258(4) . ? Mn1 N3 2.279(4) . ? Mn1 N1 2.312(4) . ? Cl1 O1 1.277(8) . ? Cl1 O2 1.362(6) . ? Cl1 O3 1.398(7) . ? Cl1 O4 1.410(6) . ? Cl2 O5 1.288(6) . ? Cl2 O5 1.288(6) 2 ? Cl2 O7 1.333(7) . ? Cl2 O7 1.333(6) 2 ? N1 C6 1.264(6) . ? N1 C7 1.467(6) . ? N2 C9 1.263(6) . ? N2 C8 1.491(6) . ? N3 C20 1.260(6) . ? N3 C21 1.471(7) . ? N4 C19 1.318(6) . ? N4 C15 1.344(6) . ? N5 N6 1.120(5) . ? N8 C5 1.331(6) . ? N8 C1 1.356(6) . ? N7 C14 1.308(6) . ? N7 C10 1.328(6) . ? N6 N5 1.120(5) 7 ? C1 C2 1.365(8) . ? C1 H1A 0.9300 . ? C2 C3 1.373(7) . ? C2 H2A 0.9300 . ? C3 C4 1.360(8) . ? C3 H3A 0.9300 . ? C4 C5 1.398(7) . ? C4 H4A 0.9300 . ? C5 C6 1.449(7) . ? C6 H6A 0.9300 . ? C7 C8 1.499(8) . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 C10 1.429(8) . ? C9 H9A 0.9300 . ? C10 C11 1.389(6) . ? C11 C12 1.353(8) . ? C11 H11A 0.9300 . ? C12 C13 1.370(9) . ? C12 H12A 0.9300 . ? C13 C14 1.367(8) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 C16 1.402(8) . ? C15 H15A 0.9300 . ? C16 C17 1.337(9) . ? C16 H16A 0.9300 . ? C17 C18 1.346(8) . ? C17 H17A 0.9300 . ? C18 C19 1.378(7) . ? C18 H18A 0.9300 . ? C19 C20 1.504(7) . ? C20 H20A 0.9300 . ? C21 C21 1.415(12) 7_556 ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? 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 N5 Mn1 N2 87.42(18) . . ? N5 Mn1 N4 88.36(17) . . ? N2 Mn1 N4 145.52(15) . . ? N5 Mn1 N3 161.33(19) . . ? N2 Mn1 N3 110.02(16) . . ? N4 Mn1 N3 73.51(15) . . ? N5 Mn1 N1 98.18(17) . . ? N2 Mn1 N1 71.16(15) . . ? N4 Mn1 N1 143.26(16) . . ? N3 Mn1 N1 93.93(15) . . ? O1 Cl1 O2 102.8(7) . . ? O1 Cl1 O3 110.6(8) . . ? O2 Cl1 O3 110.7(6) . . ? O1 Cl1 O4 118.8(9) . . ? O2 Cl1 O4 104.8(5) . . ? O3 Cl1 O4 108.7(4) . . ? O5 Cl2 O5 119.5(9) . 2 ? O5 Cl2 O7 114.8(7) . . ? O5 Cl2 O7 104.8(5) 2 . ? O5 Cl2 O7 104.8(5) . 2 ? O5 Cl2 O7 114.8(7) 2 2 ? O7 Cl2 O7 96.0(11) . 2 ? C6 N1 C7 119.6(4) . . ? C6 N1 Mn1 122.9(4) . . ? C7 N1 Mn1 116.6(3) . . ? C9 N2 C8 120.8(5) . . ? C9 N2 Mn1 124.6(4) . . ? C8 N2 Mn1 114.6(3) . . ? C20 N3 C21 118.8(6) . . ? C20 N3 Mn1 114.7(3) . . ? C21 N3 Mn1 126.5(5) . . ? C19 N4 C15 117.7(4) . . ? C19 N4 Mn1 115.4(3) . . ? C15 N4 Mn1 126.6(4) . . ? N6 N5 Mn1 163.0(4) . . ? C5 N8 C1 118.1(4) . . ? C14 N7 C10 118.3(5) . . ? N5 N6 N5 180.0(6) 7 . ? N8 C1 C2 121.2(5) . . ? N8 C1 H1A 119.4 . . ? C2 C1 H1A 119.4 . . ? C1 C2 C3 120.8(5) . . ? C1 C2 H2A 119.6 . . ? C3 C2 H2A 119.6 . . ? C4 C3 C2 118.4(5) . . ? C4 C3 H3A 120.8 . . ? C2 C3 H3A 120.8 . . ? C3 C4 C5 119.0(5) . . ? C3 C4 H4A 120.5 . . ? C5 C4 H4A 120.5 . . ? N8 C5 C4 122.4(5) . . ? N8 C5 C6 116.4(4) . . ? C4 C5 C6 121.2(5) . . ? N1 C6 C5 121.5(5) . . ? N1 C6 H6A 119.3 . . ? C5 C6 H6A 119.3 . . ? N1 C7 C8 106.3(4) . . ? N1 C7 H7B 110.5 . . ? C8 C7 H7B 110.5 . . ? N1 C7 H7C 110.5 . . ? C8 C7 H7C 110.5 . . ? H7B C7 H7C 108.7 . . ? N2 C8 C7 106.8(5) . . ? N2 C8 H8B 110.4 . . ? C7 C8 H8B 110.4 . . ? N2 C8 H8C 110.4 . . ? C7 C8 H8C 110.4 . . ? H8B C8 H8C 108.6 . . ? N2 C9 C10 120.4(5) . . ? N2 C9 H9A 119.8 . . ? C10 C9 H9A 119.8 . . ? N7 C10 C11 122.1(5) . . ? N7 C10 C9 117.2(4) . . ? C11 C10 C9 120.7(5) . . ? C12 C11 C10 118.9(5) . . ? C12 C11 H11A 120.5 . . ? C10 C11 H11A 120.5 . . ? C11 C12 C13 118.5(6) . . ? C11 C12 H12A 120.8 . . ? C13 C12 H12A 120.8 . . ? C14 C13 C12 119.4(6) . . ? C14 C13 H13A 120.3 . . ? C12 C13 H13A 120.3 . . ? N7 C14 C13 122.9(6) . . ? N7 C14 H14A 118.6 . . ? C13 C14 H14A 118.6 . . ? N4 C15 C16 119.5(6) . . ? N4 C15 H15A 120.3 . . ? C16 C15 H15A 120.3 . . ? C17 C16 C15 120.7(6) . . ? C17 C16 H16A 119.7 . . ? C15 C16 H16A 119.7 . . ? C16 C17 C18 120.1(6) . . ? C16 C17 H17A 119.9 . . ? C18 C17 H17A 119.9 . . ? C17 C18 C19 117.2(6) . . ? C17 C18 H18A 121.4 . . ? C19 C18 H18A 121.4 . . ? N4 C19 C18 124.7(5) . . ? N4 C19 C20 115.9(4) . . ? C18 C19 C20 119.4(5) . . ? N3 C20 C19 120.1(5) . . ? N3 C20 H20A 119.9 . . ? C19 C20 H20A 119.9 . . ? C21 C21 N3 113.9(8) 7_556 . ? C21 C21 H21A 108.8 7_556 . ? N3 C21 H21A 108.8 . . ? C21 C21 H21B 108.8 7_556 . ? N3 C21 H21B 108.7 . . ? H21A C21 H21B 107.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Mn1 N1 C6 75.8(5) . . . . ? N2 Mn1 N1 C6 160.2(5) . . . . ? N4 Mn1 N1 C6 -22.5(6) . . . . ? N3 Mn1 N1 C6 -90.0(4) . . . . ? N5 Mn1 N1 C7 -93.0(4) . . . . ? N2 Mn1 N1 C7 -8.6(4) . . . . ? N4 Mn1 N1 C7 168.7(4) . . . . ? N3 Mn1 N1 C7 101.2(4) . . . . ? N5 Mn1 N2 C9 -104.3(5) . . . . ? N4 Mn1 N2 C9 -21.0(6) . . . . ? N3 Mn1 N2 C9 68.8(5) . . . . ? N1 Mn1 N2 C9 156.1(5) . . . . ? N5 Mn1 N2 C8 77.6(4) . . . . ? N4 Mn1 N2 C8 160.9(3) . . . . ? N3 Mn1 N2 C8 -109.2(4) . . . . ? N1 Mn1 N2 C8 -21.9(4) . . . . ? N5 Mn1 N3 C20 12.6(8) . . . . ? N2 Mn1 N3 C20 -145.5(4) . . . . ? N4 Mn1 N3 C20 -1.7(4) . . . . ? N1 Mn1 N3 C20 143.1(4) . . . . ? N5 Mn1 N3 C21 -165.0(6) . . . . ? N2 Mn1 N3 C21 36.8(6) . . . . ? N4 Mn1 N3 C21 -179.4(6) . . . . ? N1 Mn1 N3 C21 -34.5(6) . . . . ? N5 Mn1 N4 C19 -170.4(4) . . . . ? N2 Mn1 N4 C19 106.5(4) . . . . ? N3 Mn1 N4 C19 5.0(3) . . . . ? N1 Mn1 N4 C19 -68.9(4) . . . . ? N5 Mn1 N4 C15 3.4(4) . . . . ? N2 Mn1 N4 C15 -79.6(5) . . . . ? N3 Mn1 N4 C15 178.9(4) . . . . ? N1 Mn1 N4 C15 105.0(5) . . . . ? N2 Mn1 N5 N6 20.6(14) . . . . ? N4 Mn1 N5 N6 -125.1(14) . . . . ? N3 Mn1 N5 N6 -138.9(12) . . . . ? N1 Mn1 N5 N6 91.2(14) . . . . ? C5 N8 C1 C2 1.1(7) . . . . ? N8 C1 C2 C3 -1.5(8) . . . . ? C1 C2 C3 C4 1.4(8) . . . . ? C2 C3 C4 C5 -1.0(8) . . . . ? C1 N8 C5 C4 -0.8(7) . . . . ? C1 N8 C5 C6 -179.3(4) . . . . ? C3 C4 C5 N8 0.7(8) . . . . ? C3 C4 C5 C6 179.2(5) . . . . ? C7 N1 C6 C5 176.4(5) . . . . ? Mn1 N1 C6 C5 7.9(7) . . . . ? N8 C5 C6 N1 -0.5(8) . . . . ? C4 C5 C6 N1 -179.1(5) . . . . ? C6 N1 C7 C8 -133.2(5) . . . . ? Mn1 N1 C7 C8 36.0(6) . . . . ? C9 N2 C8 C7 -129.6(5) . . . . ? Mn1 N2 C8 C7 48.5(5) . . . . ? N1 C7 C8 N2 -52.4(6) . . . . ? C8 N2 C9 C10 -179.5(5) . . . . ? Mn1 N2 C9 C10 2.6(7) . . . . ? C14 N7 C10 C11 -0.1(7) . . . . ? C14 N7 C10 C9 176.0(5) . . . . ? N2 C9 C10 N7 3.5(7) . . . . ? N2 C9 C10 C11 179.6(5) . . . . ? N7 C10 C11 C12 -1.2(7) . . . . ? C9 C10 C11 C12 -177.2(5) . . . . ? C10 C11 C12 C13 1.7(8) . . . . ? C11 C12 C13 C14 -0.9(9) . . . . ? C10 N7 C14 C13 0.9(9) . . . . ? C12 C13 C14 N7 -0.4(10) . . . . ? C19 N4 C15 C16 4.0(8) . . . . ? Mn1 N4 C15 C16 -169.8(4) . . . . ? N4 C15 C16 C17 -2.6(10) . . . . ? C15 C16 C17 C18 -0.3(11) . . . . ? C16 C17 C18 C19 1.6(10) . . . . ? C15 N4 C19 C18 -2.8(8) . . . . ? Mn1 N4 C19 C18 171.7(5) . . . . ? C15 N4 C19 C20 178.2(4) . . . . ? Mn1 N4 C19 C20 -7.3(5) . . . . ? C17 C18 C19 N4 -0.1(9) . . . . ? C17 C18 C19 C20 178.9(6) . . . . ? C21 N3 C20 C19 176.4(5) . . . . ? Mn1 N3 C20 C19 -1.4(7) . . . . ? N4 C19 C20 N3 6.1(8) . . . . ? C18 C19 C20 N3 -173.0(5) . . . . ? C20 N3 C21 C21 63.0(15) . . . 7_556 ? Mn1 N3 C21 C21 -119.5(11) . . . 7_556 ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.730 _refine_diff_density_min -0.699 _refine_diff_density_rms 0.142 data_tm28m _database_code_depnum_ccdc_archive 'CCDC 279585' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(F6 P), C30 H32 Mn2 N14' _chemical_formula_sum 'C30 H32 F12 Mn2 N14 P2' _chemical_formula_weight 988.52 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.4938(1) _cell_length_b 16.1284(2) _cell_length_c 12.8164(1) _cell_angle_alpha 90.00 _cell_angle_beta 94.5494(2) _cell_angle_gamma 90.00 _cell_volume 1956.26(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.03 _cell_measurement_theta_max 29.64 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.678 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 996 _exptl_absorpt_coefficient_mu 0.830 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6915 _exptl_absorpt_correction_T_max 0.8516 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The data collection covered over a hemisphere of reciprocal space by a combination of three sets of exposures; each set had a different \f angle (0, 88 and 180\%) for the crystal and each exposure of 10s covered 0.3\% in \w. The crystal-to-detector distance was 4 cm and the detector swing angle was -35\%. Crystal decay was monitored by repeating fifty initial frames at the end of data collection and analysing the intensity of duplicate reflections, and was found to be negligible. ; _diffrn_ambient_temperature 183(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 ; Siemens SMART CCD area detector 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_% negligible _diffrn_reflns_number 13359 _diffrn_reflns_av_R_equivalents 0.1014 _diffrn_reflns_av_sigmaI/netI 0.1098 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 28.00 _reflns_number_total 4680 _reflns_number_gt 3319 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 1997)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material ; SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 1990) ; _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^)+(0.0000P)^2^+0.0000P] 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 SHELXL _refine_ls_extinction_coef 0.0118(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4680 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0685 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1036 _refine_ls_wR_factor_gt 0.0980 _refine_ls_goodness_of_fit_ref 0.927 _refine_ls_restrained_S_all 0.927 _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 0.37275(4) 0.04888(2) 0.67849(3) 0.01725(12) Uani 1 1 d . . . P1 P 0.93682(7) 0.19389(5) 0.96299(5) 0.02665(18) Uani 1 1 d . . . F1 F 0.81764(19) 0.12419(12) 0.96311(14) 0.0565(5) Uani 1 1 d . . . F2 F 0.87559(18) 0.22252(12) 0.84799(12) 0.0500(5) Uani 1 1 d . . . F3 F 0.83164(17) 0.25714(12) 1.01442(14) 0.0495(5) Uani 1 1 d . . . F4 F 1.05374(17) 0.26521(12) 0.96397(14) 0.0518(5) Uani 1 1 d . . . F5 F 0.99718(17) 0.16618(11) 1.07775(11) 0.0427(4) Uani 1 1 d . . . F6 F 1.04246(18) 0.13148(12) 0.91274(12) 0.0522(5) Uani 1 1 d . . . N1 N 0.40716(19) 0.17688(12) 0.75705(15) 0.0198(4) Uani 1 1 d . . . N2 N 0.16358(19) 0.11471(13) 0.66664(15) 0.0221(4) Uani 1 1 d . . . N3 N 0.2308(2) -0.05281(12) 0.73577(15) 0.0217(4) Uani 1 1 d . . . N4 N 0.4993(2) -0.02204(13) 0.80923(15) 0.0214(4) Uani 1 1 d . . . N5 N 0.5802(2) 0.07754(16) 0.61391(17) 0.0368(6) Uani 1 1 d . . . N6 N 0.3156(2) -0.01222(15) 0.52364(16) 0.0347(6) Uani 1 1 d . . . N7 N 0.3701(2) -0.04434(13) 0.45551(15) 0.0225(4) Uani 1 1 d . . . C1 C 0.5269(3) 0.20798(15) 0.8034(2) 0.0264(6) Uani 1 1 d . . . H1A H 0.6101 0.1781 0.7994 0.032 Uiso 1 1 calc R . . C2 C 0.5330(3) 0.28285(15) 0.85732(19) 0.0271(6) Uani 1 1 d . . . H2A H 0.6181 0.3019 0.8895 0.032 Uiso 1 1 calc R . . C3 C 0.4107(3) 0.32853(16) 0.8623(2) 0.0292(6) Uani 1 1 d . . . H3A H 0.4116 0.3785 0.8985 0.035 Uiso 1 1 calc R . . C4 C 0.2871(3) 0.29847(15) 0.81242(19) 0.0262(6) Uani 1 1 d . . . H4A H 0.2038 0.3287 0.8133 0.031 Uiso 1 1 calc R . . C5 C 0.2878(2) 0.22279(14) 0.76090(17) 0.0198(5) Uani 1 1 d . . . C6 C 0.1584(2) 0.18573(15) 0.71052(18) 0.0227(5) Uani 1 1 d . . . H6B H 0.0729 0.2139 0.7105 0.027 Uiso 1 1 calc R . . C7 C 0.0303(3) 0.07665(17) 0.6241(2) 0.0304(6) Uani 1 1 d . . . H7A H 0.0404 0.0575 0.5534 0.036 Uiso 1 1 calc R . . H7B H -0.0444 0.1178 0.6213 0.036 Uiso 1 1 calc R . . C8 C -0.0100(2) 0.00411(17) 0.6912(2) 0.0289(6) Uani 1 1 d . . . H8A H -0.1052 -0.0131 0.6678 0.035 Uiso 1 1 calc R . . H8B H -0.0116 0.0232 0.7629 0.035 Uiso 1 1 calc R . . C9 C 0.0867(2) -0.07160(16) 0.69025(19) 0.0262(6) Uani 1 1 d . . . H9A H 0.0473 -0.1161 0.7297 0.031 Uiso 1 1 calc R . . H9B H 0.0912 -0.0905 0.6187 0.031 Uiso 1 1 calc R . . C10 C 0.2860(3) -0.10107(17) 0.80658(18) 0.0275(6) Uani 1 1 d . . . H10A H 0.2341 -0.1450 0.8307 0.033 Uiso 1 1 calc R . . C11 C 0.4320(2) -0.08691(16) 0.84976(18) 0.0246(5) Uani 1 1 d . . . C12 C 0.4968(3) -0.13943(19) 0.9243(2) 0.0364(7) Uani 1 1 d . . . H12A H 0.4474 -0.1836 0.9504 0.044 Uiso 1 1 calc R . . C13 C 0.6373(3) -0.12509(19) 0.9596(2) 0.0385(7) Uani 1 1 d . . . H13A H 0.6837 -0.1600 1.0088 0.046 Uiso 1 1 calc R . . C14 C 0.7059(3) -0.05844(17) 0.9204(2) 0.0347(7) Uani 1 1 d . . . H14A H 0.7989 -0.0466 0.9441 0.042 Uiso 1 1 calc R . . C15 C 0.6341(3) -0.00868(16) 0.8446(2) 0.0296(6) Uani 1 1 d . . . H15A H 0.6819 0.0357 0.8174 0.036 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 Mn1 0.01780(19) 0.0168(2) 0.01726(19) -0.00139(14) 0.00240(13) 0.00087(15) P1 0.0222(3) 0.0312(4) 0.0263(3) -0.0020(3) 0.0005(3) -0.0010(3) F1 0.0595(12) 0.0542(12) 0.0546(11) -0.0064(9) -0.0036(9) -0.0324(10) F2 0.0396(10) 0.0754(14) 0.0339(9) 0.0111(9) -0.0041(8) 0.0120(9) F3 0.0362(9) 0.0533(12) 0.0602(11) -0.0134(9) 0.0117(8) 0.0102(8) F4 0.0385(10) 0.0565(12) 0.0614(11) 0.0028(10) 0.0098(9) -0.0215(9) F5 0.0419(9) 0.0601(12) 0.0256(8) 0.0000(8) -0.0012(7) 0.0010(9) F6 0.0570(11) 0.0635(13) 0.0355(9) -0.0119(9) -0.0002(8) 0.0305(10) N1 0.0203(10) 0.0156(10) 0.0233(10) 0.0000(8) 0.0005(8) 0.0012(8) N2 0.0197(10) 0.0208(11) 0.0248(10) 0.0002(9) -0.0034(8) 0.0005(9) N3 0.0182(10) 0.0253(11) 0.0214(10) 0.0024(9) 0.0000(8) -0.0029(9) N4 0.0213(10) 0.0203(11) 0.0221(10) -0.0022(9) -0.0014(8) 0.0018(9) N5 0.0317(12) 0.0513(16) 0.0295(12) -0.0173(11) 0.0164(10) -0.0120(11) N6 0.0327(12) 0.0492(16) 0.0235(11) -0.0178(11) 0.0107(10) -0.0100(11) N7 0.0184(10) 0.0254(11) 0.0234(10) 0.0008(9) -0.0007(8) -0.0077(9) C1 0.0222(13) 0.0185(13) 0.0376(14) 0.0011(11) -0.0035(11) -0.0001(10) C2 0.0291(14) 0.0184(13) 0.0325(14) 0.0004(11) -0.0055(11) -0.0066(11) C3 0.0378(15) 0.0160(13) 0.0343(14) -0.0051(11) 0.0057(12) -0.0051(11) C4 0.0272(13) 0.0160(12) 0.0359(14) -0.0013(11) 0.0059(11) 0.0049(10) C5 0.0241(12) 0.0142(12) 0.0217(12) 0.0021(9) 0.0046(10) 0.0007(10) C6 0.0188(12) 0.0230(13) 0.0264(12) 0.0038(11) 0.0012(10) 0.0053(10) C7 0.0226(13) 0.0276(14) 0.0386(15) -0.0044(12) -0.0115(11) -0.0011(11) C8 0.0140(12) 0.0401(17) 0.0319(14) -0.0050(12) -0.0036(10) -0.0063(11) C9 0.0205(12) 0.0304(15) 0.0268(13) 0.0037(11) -0.0041(10) -0.0080(11) C10 0.0257(13) 0.0309(15) 0.0262(13) 0.0081(12) 0.0043(10) -0.0046(11) C11 0.0228(12) 0.0303(14) 0.0205(12) 0.0029(11) 0.0009(10) 0.0019(11) C12 0.0316(15) 0.0455(18) 0.0315(15) 0.0176(13) -0.0011(12) -0.0014(13) C13 0.0352(16) 0.0450(19) 0.0338(15) 0.0107(14) -0.0067(12) 0.0086(14) C14 0.0249(14) 0.0356(16) 0.0412(16) -0.0033(13) -0.0127(12) 0.0051(12) C15 0.0268(13) 0.0217(14) 0.0388(15) -0.0017(12) -0.0063(12) 0.0007(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 N5 2.244(2) . ? Mn1 N6 2.244(2) . ? Mn1 N2 2.2464(19) . ? Mn1 N3 2.281(2) . ? Mn1 N4 2.2892(19) . ? Mn1 N1 2.3087(19) . ? P1 F6 1.5926(17) . ? P1 F1 1.5950(18) . ? P1 F4 1.5980(18) . ? P1 F5 1.5993(16) . ? P1 F3 1.6052(18) . ? P1 F2 1.6086(16) . ? N1 C1 1.338(3) . ? N1 C5 1.358(3) . ? N2 C6 1.279(3) . ? N2 C7 1.472(3) . ? N3 C10 1.276(3) . ? N3 C9 1.475(3) . ? N4 C15 1.341(3) . ? N4 C11 1.351(3) . ? N5 N7 1.170(3) 3_656 ? N6 N7 1.170(3) . ? N7 N5 1.170(3) 3_656 ? C1 C2 1.390(3) . ? C1 H1A 0.9300 . ? C2 C3 1.381(4) . ? C2 H2A 0.9300 . ? C3 C4 1.378(3) . ? C3 H3A 0.9300 . ? C4 C5 1.388(3) . ? C4 H4A 0.9300 . ? C5 C6 1.469(3) . ? C6 H6B 0.9300 . ? C7 C8 1.519(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.528(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.469(3) . ? C10 H10A 0.9300 . ? C11 C12 1.384(3) . ? C12 C13 1.393(4) . ? C12 H12A 0.9300 . ? C13 C14 1.373(4) . ? C13 H13A 0.9300 . ? C14 C15 1.396(4) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? 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 N5 Mn1 N6 85.52(8) . . ? N5 Mn1 N2 132.42(9) . . ? N6 Mn1 N2 89.85(8) . . ? N5 Mn1 N3 145.60(9) . . ? N6 Mn1 N3 82.03(8) . . ? N2 Mn1 N3 79.62(7) . . ? N5 Mn1 N4 87.01(8) . . ? N6 Mn1 N4 120.27(8) . . ? N2 Mn1 N4 134.08(7) . . ? N3 Mn1 N4 72.21(7) . . ? N5 Mn1 N1 83.04(8) . . ? N6 Mn1 N1 142.61(8) . . ? N2 Mn1 N1 72.58(7) . . ? N3 Mn1 N1 124.71(7) . . ? N4 Mn1 N1 94.57(7) . . ? F6 P1 F1 91.40(11) . . ? F6 P1 F4 89.93(11) . . ? F1 P1 F4 178.66(11) . . ? F6 P1 F5 90.23(9) . . ? F1 P1 F5 90.27(10) . . ? F4 P1 F5 89.77(9) . . ? F6 P1 F3 179.42(10) . . ? F1 P1 F3 89.03(10) . . ? F4 P1 F3 89.64(10) . . ? F5 P1 F3 89.38(9) . . ? F6 P1 F2 90.25(9) . . ? F1 P1 F2 89.90(10) . . ? F4 P1 F2 90.05(10) . . ? F5 P1 F2 179.49(11) . . ? F3 P1 F2 90.14(10) . . ? C1 N1 C5 117.5(2) . . ? C1 N1 Mn1 127.94(16) . . ? C5 N1 Mn1 114.44(15) . . ? C6 N2 C7 118.3(2) . . ? C6 N2 Mn1 117.27(15) . . ? C7 N2 Mn1 123.88(16) . . ? C10 N3 C9 118.1(2) . . ? C10 N3 Mn1 116.58(16) . . ? C9 N3 Mn1 124.99(15) . . ? C15 N4 C11 117.5(2) . . ? C15 N4 Mn1 126.78(17) . . ? C11 N4 Mn1 115.56(15) . . ? N7 N5 Mn1 127.27(18) 3_656 . ? N7 N6 Mn1 139.85(18) . . ? N5 N7 N6 177.6(2) 3_656 . ? N1 C1 C2 123.1(2) . . ? N1 C1 H1A 118.4 . . ? C2 C1 H1A 118.4 . . ? C3 C2 C1 119.0(2) . . ? C3 C2 H2A 120.5 . . ? C1 C2 H2A 120.5 . . ? C4 C3 C2 118.6(2) . . ? C4 C3 H3A 120.7 . . ? C2 C3 H3A 120.7 . . ? C3 C4 C5 119.6(2) . . ? C3 C4 H4A 120.2 . . ? C5 C4 H4A 120.2 . . ? N1 C5 C4 122.1(2) . . ? N1 C5 C6 115.7(2) . . ? C4 C5 C6 122.1(2) . . ? N2 C6 C5 119.9(2) . . ? N2 C6 H6B 120.1 . . ? C5 C6 H6B 120.1 . . ? N2 C7 C8 111.09(19) . . ? N2 C7 H7A 109.4 . . ? C8 C7 H7A 109.4 . . ? N2 C7 H7B 109.4 . . ? C8 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? C7 C8 C9 115.6(2) . . ? C7 C8 H8A 108.4 . . ? C9 C8 H8A 108.4 . . ? C7 C8 H8B 108.4 . . ? C9 C8 H8B 108.4 . . ? H8A C8 H8B 107.4 . . ? N3 C9 C8 111.8(2) . . ? N3 C9 H9A 109.3 . . ? C8 C9 H9A 109.3 . . ? N3 C9 H9B 109.3 . . ? C8 C9 H9B 109.3 . . ? H9A C9 H9B 107.9 . . ? N3 C10 C11 119.7(2) . . ? N3 C10 H10A 120.2 . . ? C11 C10 H10A 120.2 . . ? N4 C11 C12 122.8(2) . . ? N4 C11 C10 115.9(2) . . ? C12 C11 C10 121.3(2) . . ? C11 C12 C13 119.0(3) . . ? C11 C12 H12A 120.5 . . ? C13 C12 H12A 120.5 . . ? C14 C13 C12 118.8(3) . . ? C14 C13 H13A 120.6 . . ? C12 C13 H13A 120.6 . . ? C13 C14 C15 119.0(2) . . ? C13 C14 H14A 120.5 . . ? C15 C14 H14A 120.5 . . ? N4 C15 C14 122.9(3) . . ? N4 C15 H15A 118.5 . . ? C14 C15 H15A 118.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Mn1 N1 C1 -42.4(2) . . . . ? N6 Mn1 N1 C1 -115.5(2) . . . . ? N2 Mn1 N1 C1 179.0(2) . . . . ? N3 Mn1 N1 C1 115.5(2) . . . . ? N4 Mn1 N1 C1 44.0(2) . . . . ? N5 Mn1 N1 C5 141.85(17) . . . . ? N6 Mn1 N1 C5 68.7(2) . . . . ? N2 Mn1 N1 C5 3.20(15) . . . . ? N3 Mn1 N1 C5 -60.25(18) . . . . ? N4 Mn1 N1 C5 -131.74(16) . . . . ? N5 Mn1 N2 C6 -66.1(2) . . . . ? N6 Mn1 N2 C6 -149.87(19) . . . . ? N3 Mn1 N2 C6 128.21(18) . . . . ? N4 Mn1 N2 C6 75.8(2) . . . . ? N1 Mn1 N2 C6 -3.41(17) . . . . ? N5 Mn1 N2 C7 122.29(19) . . . . ? N6 Mn1 N2 C7 38.51(19) . . . . ? N3 Mn1 N2 C7 -43.41(19) . . . . ? N4 Mn1 N2 C7 -95.8(2) . . . . ? N1 Mn1 N2 C7 -175.0(2) . . . . ? N5 Mn1 N3 C10 53.0(2) . . . . ? N6 Mn1 N3 C10 122.82(19) . . . . ? N2 Mn1 N3 C10 -145.86(19) . . . . ? N4 Mn1 N3 C10 -2.59(18) . . . . ? N1 Mn1 N3 C10 -85.67(19) . . . . ? N5 Mn1 N3 C9 -120.7(2) . . . . ? N6 Mn1 N3 C9 -50.87(19) . . . . ? N2 Mn1 N3 C9 40.44(18) . . . . ? N4 Mn1 N3 C9 -176.3(2) . . . . ? N1 Mn1 N3 C9 100.63(19) . . . . ? N5 Mn1 N4 C15 25.9(2) . . . . ? N6 Mn1 N4 C15 109.0(2) . . . . ? N2 Mn1 N4 C15 -126.9(2) . . . . ? N3 Mn1 N4 C15 178.1(2) . . . . ? N1 Mn1 N4 C15 -56.8(2) . . . . ? N5 Mn1 N4 C11 -149.92(18) . . . . ? N6 Mn1 N4 C11 -66.88(19) . . . . ? N2 Mn1 N4 C11 57.2(2) . . . . ? N3 Mn1 N4 C11 2.27(16) . . . . ? N1 Mn1 N4 C11 127.32(17) . . . . ? N6 Mn1 N5 N7 -20.6(2) . . . 3_656 ? N2 Mn1 N5 N7 -106.3(3) . . . 3_656 ? N3 Mn1 N5 N7 48.3(3) . . . 3_656 ? N4 Mn1 N5 N7 100.1(3) . . . 3_656 ? N1 Mn1 N5 N7 -164.9(3) . . . 3_656 ? N5 Mn1 N6 N7 26.2(3) . . . . ? N2 Mn1 N6 N7 158.8(3) . . . . ? N3 Mn1 N6 N7 -121.7(3) . . . . ? N4 Mn1 N6 N7 -57.7(3) . . . . ? N1 Mn1 N6 N7 98.6(3) . . . . ? Mn1 N6 N7 N5 166(7) . . . 3_656 ? C5 N1 C1 C2 2.1(4) . . . . ? Mn1 N1 C1 C2 -173.58(18) . . . . ? N1 C1 C2 C3 -1.1(4) . . . . ? C1 C2 C3 C4 -0.7(4) . . . . ? C2 C3 C4 C5 1.5(4) . . . . ? C1 N1 C5 C4 -1.3(3) . . . . ? Mn1 N1 C5 C4 174.95(18) . . . . ? C1 N1 C5 C6 -179.0(2) . . . . ? Mn1 N1 C5 C6 -2.8(2) . . . . ? C3 C4 C5 N1 -0.5(4) . . . . ? C3 C4 C5 C6 177.1(2) . . . . ? C7 N2 C6 C5 175.3(2) . . . . ? Mn1 N2 C6 C5 3.2(3) . . . . ? N1 C5 C6 N2 -0.2(3) . . . . ? C4 C5 C6 N2 -177.9(2) . . . . ? C6 N2 C7 C8 -107.7(3) . . . . ? Mn1 N2 C7 C8 63.8(3) . . . . ? N2 C7 C8 C9 -67.7(3) . . . . ? C10 N3 C9 C8 129.4(2) . . . . ? Mn1 N3 C9 C8 -57.0(3) . . . . ? C7 C8 C9 N3 64.3(3) . . . . ? C9 N3 C10 C11 176.8(2) . . . . ? Mn1 N3 C10 C11 2.6(3) . . . . ? C15 N4 C11 C12 -0.7(4) . . . . ? Mn1 N4 C11 C12 175.6(2) . . . . ? C15 N4 C11 C10 -178.1(2) . . . . ? Mn1 N4 C11 C10 -1.8(3) . . . . ? N3 C10 C11 N4 -0.5(4) . . . . ? N3 C10 C11 C12 -178.0(2) . . . . ? N4 C11 C12 C13 0.2(4) . . . . ? C10 C11 C12 C13 177.5(3) . . . . ? C11 C12 C13 C14 1.1(4) . . . . ? C12 C13 C14 C15 -1.8(4) . . . . ? C11 N4 C15 C14 -0.1(4) . . . . ? Mn1 N4 C15 C14 -175.9(2) . . . . ? C13 C14 C15 N4 1.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.541 _refine_diff_density_min -0.900 _refine_diff_density_rms 0.148 data_T-Mn65a _database_code_depnum_ccdc_archive 'CCDC 279586' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H18 Cl Mn N7 O4' _chemical_formula_weight 462.76 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 orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 12.5606(6) _cell_length_b 17.2500(8) _cell_length_c 18.1617(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3935.1(3) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 0.846 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7284 _exptl_absorpt_correction_T_max 0.9202 _exptl_absorpt_process_details 'SADABS (Bruker axs)' _exptl_special_details ; How were the crystals grown ? Please, fill in ! ; _diffrn_ambient_temperature 153(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 scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% 0 _diffrn_reflns_number 44314 _diffrn_reflns_av_R_equivalents 0.0592 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4509 _reflns_number_gt 3109 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker axs)' _computing_cell_refinement 'SMART (Bruker axs)' _computing_data_reduction 'SAINT (Bruker axs)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V5.10 NT (Sheldrick, 1998)' _computing_publication_material 'SHELXTL V5.10 NT (Sheldrick, 1998)' _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^)+(0.0998P)^2^+0.0000P] 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 4509 _refine_ls_number_parameters 273 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0849 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1637 _refine_ls_wR_factor_gt 0.1502 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 0.5000 0.73528(4) 0.7500 0.02072(19) Uani 1 2 d S . . Mn2 Mn 0.5000 0.53408(4) 0.7500 0.02223(19) Uani 1 2 d S . . N1 N 0.5542(2) 0.63350(14) 0.68228(13) 0.0240(6) Uani 1 1 d . . . N2 N 0.5461(2) 0.63369(16) 0.61589(16) 0.0317(7) Uani 1 1 d . . . N3 N 0.5388(3) 0.6351(2) 0.55313(16) 0.0491(9) Uani 1 1 d . . . N4 N 0.4666(2) 0.80555(17) 0.85378(16) 0.0338(7) Uani 1 1 d . . . N5 N 0.5414(2) 0.44453(19) 0.66500(18) 0.0402(8) Uani 1 1 d . . . N6 N 0.6578(2) 0.75309(15) 0.80539(14) 0.0247(6) Uani 1 1 d . . . N7 N 0.3500(2) 0.51443(15) 0.68381(14) 0.0251(6) Uani 1 1 d . . . C1 C 0.5441(3) 0.8038(2) 0.8993(2) 0.0376(9) Uani 1 1 d . . . H1 H 0.5332 0.8196 0.9488 0.045 Uiso 1 1 calc R . . C2 C 0.6493(3) 0.7776(2) 0.87586(19) 0.0322(8) Uani 1 1 d . . . C3 C 0.7357(3) 0.7774(2) 0.9240(2) 0.0417(9) Uani 1 1 d . . . H3 H 0.7268 0.7919 0.9741 0.050 Uiso 1 1 calc R . . C4 C 0.8338(3) 0.7558(2) 0.8978(2) 0.0411(9) Uani 1 1 d . . . H4 H 0.8942 0.7570 0.9292 0.049 Uiso 1 1 calc R . . C5 C 0.8439(3) 0.7323(2) 0.8253(2) 0.0334(8) Uani 1 1 d . . . H5 H 0.9111 0.7175 0.8059 0.040 Uiso 1 1 calc R . . C6 C 0.7534(3) 0.73099(19) 0.78185(18) 0.0297(7) Uani 1 1 d . . . H6 H 0.7599 0.7133 0.7325 0.036 Uiso 1 1 calc R . . C7 C 0.3627(3) 0.8334(2) 0.8809(2) 0.0418(9) Uani 1 1 d . . . H7A H 0.3642 0.8387 0.9351 0.050 Uiso 1 1 calc R . . H7B H 0.3059 0.7961 0.8676 0.050 Uiso 1 1 calc R . . C8 C 0.3414(3) 0.9107(2) 0.8456(2) 0.0490(10) Uani 1 1 d . . . H8A H 0.3456 0.9051 0.7915 0.059 Uiso 1 1 calc R . . H8B H 0.3972 0.9478 0.8611 0.059 Uiso 1 1 calc R . . C9 C 0.2292(3) 0.9446(2) 0.8667(2) 0.0489(10) Uani 1 1 d . . . H9A H 0.2228 0.9470 0.9210 0.059 Uiso 1 1 calc R . . H9B H 0.2229 0.9980 0.8473 0.059 Uiso 1 1 calc R . . C10 C 0.1415(3) 0.8964(2) 0.8365(2) 0.0467(10) Uani 1 1 d . . . H10A H 0.1308 0.8500 0.8677 0.056 Uiso 1 1 calc R . . H10B H 0.1596 0.8790 0.7861 0.056 Uiso 1 1 calc R . . C11 C 0.4703(3) 0.4350(3) 0.6153(2) 0.0459(10) Uani 1 1 d . . . H11 H 0.4845 0.4021 0.5745 0.055 Uiso 1 1 calc R . . C12 C 0.3663(3) 0.4747(2) 0.62068(19) 0.0343(8) Uani 1 1 d . . . C13 C 0.2883(3) 0.4667(2) 0.5683(2) 0.0445(10) Uani 1 1 d . . . H13 H 0.3025 0.4397 0.5238 0.053 Uiso 1 1 calc R . . C14 C 0.1889(3) 0.4985(2) 0.5811(2) 0.0477(10) Uani 1 1 d . . . H14 H 0.1342 0.4946 0.5452 0.057 Uiso 1 1 calc R . . C15 C 0.1703(3) 0.5361(2) 0.6472(2) 0.0440(10) Uani 1 1 d . . . H15 H 0.1020 0.5564 0.6587 0.053 Uiso 1 1 calc R . . C16 C 0.2542(3) 0.54332(19) 0.6962(2) 0.0335(8) Uani 1 1 d . . . H16 H 0.2422 0.5704 0.7410 0.040 Uiso 1 1 calc R . . Cl2 Cl 0.89134(6) 0.63819(5) 0.60732(4) 0.0280(2) Uani 1 1 d . . . O1 O 0.9194(2) 0.61973(17) 0.68149(13) 0.0476(7) Uani 1 1 d . . . O2 O 0.9479(3) 0.5900(2) 0.55809(14) 0.0618(9) Uani 1 1 d . . . O3 O 0.7796(2) 0.63017(18) 0.59589(19) 0.0629(9) Uani 1 1 d . . . O4 O 0.9177(3) 0.71738(17) 0.59194(19) 0.0672(9) 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 0.0171(3) 0.0241(4) 0.0209(3) 0.000 -0.0024(2) 0.000 Mn2 0.0162(3) 0.0236(4) 0.0268(4) 0.000 -0.0036(2) 0.000 N1 0.0260(15) 0.0303(15) 0.0155(12) -0.0006(10) 0.0008(10) -0.0005(11) N2 0.0274(16) 0.0345(17) 0.0332(17) -0.0030(13) 0.0003(12) 0.0040(13) N3 0.063(2) 0.067(3) 0.0167(15) -0.0040(14) -0.0019(14) 0.0098(18) N4 0.0257(15) 0.0351(17) 0.0405(17) -0.0141(13) -0.0018(12) 0.0064(13) N5 0.0237(15) 0.0420(19) 0.0548(19) -0.0209(15) -0.0002(14) 0.0050(14) N6 0.0189(14) 0.0274(15) 0.0279(14) -0.0056(11) -0.0022(10) 0.0031(11) N7 0.0189(13) 0.0291(15) 0.0274(13) -0.0053(11) -0.0034(10) 0.0018(11) C1 0.0297(19) 0.050(2) 0.0332(19) -0.0158(16) -0.0049(15) 0.0067(17) C2 0.0261(18) 0.038(2) 0.0327(18) -0.0092(15) -0.0061(14) 0.0019(15) C3 0.038(2) 0.052(3) 0.0347(19) -0.0141(17) -0.0112(16) 0.0040(18) C4 0.029(2) 0.046(2) 0.048(2) -0.0070(18) -0.0188(16) 0.0049(17) C5 0.0227(18) 0.034(2) 0.043(2) -0.0020(16) -0.0057(15) 0.0037(14) C6 0.0239(17) 0.0346(19) 0.0307(17) -0.0031(14) 0.0002(14) 0.0016(15) C7 0.037(2) 0.049(2) 0.040(2) -0.0054(18) 0.0014(16) 0.0136(18) C8 0.035(2) 0.046(3) 0.066(3) 0.003(2) -0.0005(19) -0.0014(18) C9 0.050(3) 0.044(2) 0.053(2) -0.0092(19) -0.0121(19) 0.0103(19) C10 0.036(2) 0.043(2) 0.061(3) 0.007(2) -0.0006(19) 0.0024(18) C11 0.034(2) 0.057(3) 0.047(2) -0.028(2) 0.0037(17) 0.0026(19) C12 0.0287(19) 0.038(2) 0.0366(18) -0.0107(16) -0.0018(14) -0.0012(15) C13 0.044(2) 0.054(3) 0.035(2) -0.0130(18) -0.0110(17) -0.0023(19) C14 0.040(2) 0.047(2) 0.056(2) -0.003(2) -0.0259(19) -0.0012(19) C15 0.0254(19) 0.039(2) 0.068(3) -0.0094(19) -0.0168(17) 0.0076(16) C16 0.0220(17) 0.033(2) 0.046(2) -0.0080(15) -0.0060(15) 0.0046(14) Cl2 0.0195(4) 0.0393(5) 0.0251(4) -0.0002(3) -0.0009(3) -0.0008(3) O1 0.0402(16) 0.082(2) 0.0210(12) 0.0028(12) -0.0015(11) 0.0073(14) O2 0.077(2) 0.075(2) 0.0332(15) -0.0116(15) -0.0025(14) 0.0355(19) O3 0.0266(16) 0.092(3) 0.070(2) 0.0182(17) -0.0117(14) -0.0106(14) O4 0.065(2) 0.0442(19) 0.092(2) 0.0117(17) -0.0135(18) -0.0104(15) _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 N6 2.244(2) . ? Mn1 N6 2.244(2) 3_656 ? Mn1 N1 2.249(3) . ? Mn1 N1 2.249(3) 3_656 ? Mn1 N4 2.280(3) . ? Mn1 N4 2.280(3) 3_656 ? Mn2 N1 2.217(3) . ? Mn2 N1 2.217(3) 3_656 ? Mn2 N5 2.245(3) . ? Mn2 N5 2.245(3) 3_656 ? Mn2 N7 2.260(2) . ? Mn2 N7 2.260(2) 3_656 ? N1 N2 1.210(4) . ? N2 N3 1.144(4) . ? N4 C1 1.277(4) . ? N4 C7 1.475(4) . ? N5 C11 1.281(5) . ? N5 C10 1.507(5) 6_657 ? N6 C6 1.330(4) . ? N6 C2 1.352(4) . ? N7 C16 1.323(4) . ? N7 C12 1.351(4) . ? C1 C2 1.459(5) . ? C2 C3 1.393(5) . ? C3 C4 1.371(5) . ? C4 C5 1.385(5) . ? C5 C6 1.383(4) . ? C7 C8 1.504(6) . ? C8 C9 1.572(5) . ? C9 C10 1.484(5) . ? C10 N5 1.507(5) 6_567 ? C11 C12 1.478(5) . ? C12 C13 1.372(5) . ? C13 C14 1.384(6) . ? C14 C15 1.384(5) . ? C15 C16 1.384(5) . ? Cl2 O2 1.413(3) . ? Cl2 O3 1.426(3) . ? Cl2 O1 1.428(2) . ? Cl2 O4 1.433(3) . ? 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 N6 Mn1 N6 164.26(14) . 3_656 ? N6 Mn1 N1 94.85(9) . . ? N6 Mn1 N1 97.42(10) 3_656 . ? N6 Mn1 N1 97.42(10) . 3_656 ? N6 Mn1 N1 94.85(9) 3_656 3_656 ? N1 Mn1 N1 77.37(13) . 3_656 ? N6 Mn1 N4 73.69(10) . . ? N6 Mn1 N4 97.77(10) 3_656 . ? N1 Mn1 N4 157.34(10) . . ? N1 Mn1 N4 84.68(10) 3_656 . ? N6 Mn1 N4 97.77(10) . 3_656 ? N6 Mn1 N4 73.69(10) 3_656 3_656 ? N1 Mn1 N4 84.68(10) . 3_656 ? N1 Mn1 N4 157.34(10) 3_656 3_656 ? N4 Mn1 N4 115.76(16) . 3_656 ? N1 Mn2 N1 78.69(13) . 3_656 ? N1 Mn2 N5 94.57(11) . . ? N1 Mn2 N5 169.96(11) 3_656 . ? N1 Mn2 N5 169.96(11) . 3_656 ? N1 Mn2 N5 94.57(11) 3_656 3_656 ? N5 Mn2 N5 93.03(18) . 3_656 ? N1 Mn2 N7 94.41(10) . . ? N1 Mn2 N7 98.93(9) 3_656 . ? N5 Mn2 N7 73.98(10) . . ? N5 Mn2 N7 93.98(10) 3_656 . ? N1 Mn2 N7 98.93(10) . 3_656 ? N1 Mn2 N7 94.41(10) 3_656 3_656 ? N5 Mn2 N7 93.98(10) . 3_656 ? N5 Mn2 N7 73.98(10) 3_656 3_656 ? N7 Mn2 N7 162.75(14) . 3_656 ? N2 N1 Mn2 121.9(2) . . ? N2 N1 Mn1 121.2(2) . . ? Mn2 N1 Mn1 101.97(10) . . ? N3 N2 N1 178.9(4) . . ? C1 N4 C7 117.8(3) . . ? C1 N4 Mn1 112.4(2) . . ? C7 N4 Mn1 127.7(2) . . ? C11 N5 C10 119.9(3) . 6_657 ? C11 N5 Mn2 114.3(2) . . ? C10 N5 Mn2 125.8(2) 6_657 . ? C6 N6 C2 117.7(3) . . ? C6 N6 Mn1 127.9(2) . . ? C2 N6 Mn1 113.4(2) . . ? C16 N7 C12 118.2(3) . . ? C16 N7 Mn2 127.7(2) . . ? C12 N7 Mn2 113.7(2) . . ? N4 C1 C2 120.6(3) . . ? N6 C2 C3 122.1(3) . . ? N6 C2 C1 116.4(3) . . ? C3 C2 C1 121.6(3) . . ? C4 C3 C2 118.9(3) . . ? C3 C4 C5 119.4(3) . . ? C6 C5 C4 118.2(3) . . ? N6 C6 C5 123.6(3) . . ? N4 C7 C8 107.7(3) . . ? C7 C8 C9 112.7(3) . . ? C10 C9 C8 111.6(3) . . ? C9 C10 N5 108.5(3) . 6_567 ? N5 C11 C12 120.7(3) . . ? N7 C12 C13 122.1(3) . . ? N7 C12 C11 115.1(3) . . ? C13 C12 C11 122.6(3) . . ? C12 C13 C14 119.2(3) . . ? C13 C14 C15 118.9(3) . . ? C16 C15 C14 118.1(3) . . ? N7 C16 C15 123.3(3) . . ? O2 Cl2 O3 110.3(2) . . ? O2 Cl2 O1 109.96(17) . . ? O3 Cl2 O1 111.01(18) . . ? O2 Cl2 O4 108.7(2) . . ? O3 Cl2 O4 106.97(19) . . ? O1 Cl2 O4 109.83(19) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.947 _refine_diff_density_min -0.436 _refine_diff_density_rms 0.119 #=========================================================================== #eof #End of Crystallographic Information File