# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Li Baolong' _publ_contact_author_email LIBAOLONG@SUDA.EDU.CN _publ_section_title ; Solvent-controlled assembly of supramolecular isomers: 2D (4,4) network, 1D ribbons of ring, and both 2D (4,4) networks and 1D ribbons of rings polycatenated in a 3D array ; loop_ _publ_author_name 'Li Baolong' 'Xun-Gao Liu' 'Yong Zhang' 'Xia Zhu' data_[Mn(btb)2(NCS)2](CH2Cl2)(1) _database_code_depnum_ccdc_archive 'CCDC 714832' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H26 Cl2 Mn N14 S2' _chemical_formula_weight 640.50 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' Mn Mn 0.3368 0.7283 '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' S S 0.1246 0.1234 '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' _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 8.4645(18) _cell_length_b 9.117(2) _cell_length_c 11.632(2) _cell_angle_alpha 110.885(6) _cell_angle_beta 90.108(3) _cell_angle_gamma 104.698(5) _cell_volume 807.0(3) _cell_formula_units_Z 1 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 3175 _cell_measurement_theta_min 3.0088 _cell_measurement_theta_max 25.3491 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 329 _exptl_absorpt_coefficient_mu 0.737 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7824 _exptl_absorpt_correction_T_max 0.8726 _exptl_absorpt_process_details Empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'Rigaku Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 7973 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 25.35 _reflns_number_total 2905 _reflns_number_gt 2592 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and Rfactors 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^)+(0.1161P)^2^+2.2976P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2905 _refine_ls_number_parameters 187 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0791 _refine_ls_R_factor_gt 0.0728 _refine_ls_wR_factor_ref 0.2080 _refine_ls_wR_factor_gt 0.2019 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 0.0000 0.0000 0.0000 0.0209(3) Uani 1 2 d S . . S1 S 0.1648(3) 0.58689(17) 0.25003(17) 0.0712(6) Uani 1 1 d . . . N1 N 0.4186(4) -0.1643(4) 0.0792(3) 0.0261(7) Uani 1 1 d . . . N2 N 0.4754(4) -0.0019(4) 0.1518(3) 0.0318(8) Uani 1 1 d . . . N3 N 0.2334(4) -0.0532(4) 0.0453(3) 0.0260(7) Uani 1 1 d . . . N4 N -0.1889(4) 0.0188(4) 0.3555(3) 0.0310(8) Uani 1 1 d . . . N5 N -0.1350(5) -0.1171(5) 0.3320(4) 0.0392(9) Uani 1 1 d . . . N6 N -0.0772(4) -0.0143(4) 0.1833(3) 0.0261(7) Uani 1 1 d . . . N7 N 0.1104(5) 0.2624(4) 0.0926(4) 0.0333(8) Uani 1 1 d . . . C1 C 0.5146(5) -0.2752(5) 0.0855(4) 0.0323(10) Uani 1 1 d . . . H1A H 0.5134 -0.2809 0.1689 0.039 Uiso 1 1 calc R . . H1B H 0.6300 -0.2301 0.0735 0.039 Uiso 1 1 calc R . . C2 C 0.4503(5) -0.4452(5) -0.0099(4) 0.0289(9) Uani 1 1 d . . . H2A H 0.4600 -0.4424 -0.0940 0.035 Uiso 1 1 calc R . . H2B H 0.3329 -0.4892 -0.0022 0.035 Uiso 1 1 calc R . . C3 C 0.3594(5) 0.0571(5) 0.1279(4) 0.0295(9) Uani 1 1 d . . . H3A H 0.3631 0.1692 0.1657 0.035 Uiso 1 1 calc R . . C4 C 0.2758(5) -0.1916(5) 0.0175(4) 0.0285(9) Uani 1 1 d . . . H4A H 0.2128 -0.2951 -0.0384 0.034 Uiso 1 1 calc R . . C5 C -0.2787(6) 0.0759(6) 0.4630(4) 0.0387(11) Uani 1 1 d . . . H5A H -0.2798 0.1897 0.4786 0.046 Uiso 1 1 calc R . . H5B H -0.2212 0.0751 0.5369 0.046 Uiso 1 1 calc R . . C6 C -0.4544(5) -0.0303(6) 0.4435(4) 0.0350(10) Uani 1 1 d . . . H6A H -0.4538 -0.1443 0.4277 0.042 Uiso 1 1 calc R . . H6B H -0.5125 -0.0289 0.3701 0.042 Uiso 1 1 calc R . . C7 C -0.0698(6) -0.1307(6) 0.2274(4) 0.0348(10) Uani 1 1 d . . . H7A H -0.0212 -0.2161 0.1861 0.042 Uiso 1 1 calc R . . C8 C -0.1545(5) 0.0769(5) 0.2666(4) 0.0273(9) Uani 1 1 d . . . H8A H -0.1812 0.1703 0.2629 0.033 Uiso 1 1 calc R . . C9 C 0.1314(5) 0.3970(5) 0.1579(4) 0.0300(9) Uani 1 1 d . . . Cl1 Cl 0.2557(4) 0.2660(4) 0.4176(3) 0.0641(8) Uani 0.50 1 d P . . Cl2 Cl 0.3272(5) 0.5581(5) 0.6432(4) 0.0863(11) Uani 0.50 1 d P . . C10 C 0.1881(15) 0.3871(15) 0.5210(15) 0.071(4) Uani 0.50 1 d P . . H10B H 0.1123 0.3231 0.5614 0.085 Uiso 0.50 1 calc PR . . H10A H 0.1209 0.4331 0.4806 0.085 Uiso 0.50 1 calc PR . . 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 0.0204(5) 0.0203(5) 0.0227(5) 0.0070(3) 0.0052(3) 0.0077(3) S1 0.1018(14) 0.0279(7) 0.0682(10) -0.0001(7) 0.0297(9) 0.0170(8) N1 0.0234(17) 0.0289(18) 0.0296(17) 0.0122(15) 0.0047(13) 0.0113(14) N2 0.0302(18) 0.0253(18) 0.037(2) 0.0062(15) -0.0016(15) 0.0095(14) N3 0.0218(16) 0.0292(18) 0.0308(18) 0.0125(15) 0.0054(14) 0.0116(13) N4 0.0305(19) 0.036(2) 0.0260(18) 0.0106(15) 0.0099(14) 0.0088(15) N5 0.048(2) 0.043(2) 0.037(2) 0.0207(18) 0.0153(18) 0.0200(19) N6 0.0249(17) 0.0300(18) 0.0241(17) 0.0098(14) 0.0067(13) 0.0088(14) N7 0.037(2) 0.0221(19) 0.037(2) 0.0075(16) 0.0031(16) 0.0071(15) C1 0.027(2) 0.031(2) 0.041(2) 0.0109(19) 0.0013(18) 0.0162(18) C2 0.026(2) 0.030(2) 0.032(2) 0.0107(18) 0.0021(16) 0.0119(17) C3 0.030(2) 0.026(2) 0.033(2) 0.0097(18) 0.0023(17) 0.0106(17) C4 0.0214(19) 0.031(2) 0.034(2) 0.0113(18) 0.0030(16) 0.0106(16) C5 0.041(3) 0.042(3) 0.027(2) 0.006(2) 0.0151(19) 0.008(2) C6 0.034(2) 0.044(3) 0.025(2) 0.0091(19) 0.0098(18) 0.014(2) C7 0.037(2) 0.040(3) 0.035(2) 0.016(2) 0.0133(19) 0.020(2) C8 0.026(2) 0.029(2) 0.026(2) 0.0084(17) 0.0065(16) 0.0090(16) C9 0.029(2) 0.029(2) 0.035(2) 0.013(2) 0.0066(17) 0.0104(17) Cl1 0.076(2) 0.069(2) 0.0423(14) 0.0211(14) 0.0097(14) 0.0120(16) Cl2 0.085(3) 0.074(2) 0.086(3) 0.014(2) -0.014(2) 0.0212(19) C10 0.054(7) 0.050(7) 0.123(12) 0.059(8) -0.027(7) -0.003(5) _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 N7 2.187(4) 2 ? Mn1 N7 2.187(4) . ? Mn1 N3 2.254(3) 2 ? Mn1 N3 2.254(3) . ? Mn1 N6 2.269(3) 2 ? Mn1 N6 2.269(3) . ? S1 C9 1.628(4) . ? N1 C4 1.325(5) . ? N1 N2 1.372(5) . ? N1 C1 1.468(5) . ? N2 C3 1.306(6) . ? N3 C4 1.329(5) . ? N3 C3 1.354(5) . ? N4 C8 1.322(5) . ? N4 N5 1.365(5) . ? N4 C5 1.467(5) . ? N5 C7 1.315(6) . ? N6 C8 1.328(5) . ? N6 C7 1.347(6) . ? N7 C9 1.158(6) . ? C1 C2 1.508(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C2 1.534(8) 2_645 ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9500 . ? C4 H4A 0.9500 . ? C5 C6 1.520(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C6 1.526(8) 2_456 ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9500 . ? C8 H8A 0.9500 . ? Cl1 C10 1.539(16) . ? Cl2 C10 1.822(14) . ? C10 H10B 0.9900 . ? C10 H10A 0.9900 . ? 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 N7 Mn1 N7 180.00(12) 2 . ? N7 Mn1 N3 91.13(13) 2 2 ? N7 Mn1 N3 88.87(13) . 2 ? N7 Mn1 N3 88.87(13) 2 . ? N7 Mn1 N3 91.13(13) . . ? N3 Mn1 N3 180.00(17) 2 . ? N7 Mn1 N6 89.65(13) 2 2 ? N7 Mn1 N6 90.35(13) . 2 ? N3 Mn1 N6 87.01(12) 2 2 ? N3 Mn1 N6 92.99(12) . 2 ? N7 Mn1 N6 90.35(13) 2 . ? N7 Mn1 N6 89.65(13) . . ? N3 Mn1 N6 92.99(12) 2 . ? N3 Mn1 N6 87.01(12) . . ? N6 Mn1 N6 180.0(3) 2 . ? C4 N1 N2 109.8(3) . . ? C4 N1 C1 131.6(4) . . ? N2 N1 C1 118.5(3) . . ? C3 N2 N1 102.2(3) . . ? C4 N3 C3 102.8(3) . . ? C4 N3 Mn1 132.1(3) . . ? C3 N3 Mn1 124.4(3) . . ? C8 N4 N5 109.9(3) . . ? C8 N4 C5 129.0(4) . . ? N5 N4 C5 121.0(4) . . ? C7 N5 N4 102.2(4) . . ? C8 N6 C7 102.9(3) . . ? C8 N6 Mn1 129.6(3) . . ? C7 N6 Mn1 127.2(3) . . ? C9 N7 Mn1 161.6(3) . . ? N1 C1 C2 113.0(3) . . ? N1 C1 H1A 109.0 . . ? C2 C1 H1A 109.0 . . ? N1 C1 H1B 109.0 . . ? C2 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? C1 C2 C2 109.2(4) . 2_645 ? C1 C2 H2A 109.8 . . ? C2 C2 H2A 109.8 2_645 . ? C1 C2 H2B 109.8 . . ? C2 C2 H2B 109.8 2_645 . ? H2A C2 H2B 108.3 . . ? N2 C3 N3 115.1(4) . . ? N2 C3 H3A 122.4 . . ? N3 C3 H3A 122.4 . . ? N1 C4 N3 110.0(4) . . ? N1 C4 H4A 125.0 . . ? N3 C4 H4A 125.0 . . ? N4 C5 C6 111.9(4) . . ? N4 C5 H5A 109.2 . . ? C6 C5 H5A 109.2 . . ? N4 C5 H5B 109.2 . . ? C6 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? C5 C6 C6 111.1(5) . 2_456 ? C5 C6 H6A 109.4 . . ? C6 C6 H6A 109.4 2_456 . ? C5 C6 H6B 109.4 . . ? C6 C6 H6B 109.4 2_456 . ? H6A C6 H6B 108.0 . . ? N5 C7 N6 114.8(4) . . ? N5 C7 H7A 122.6 . . ? N6 C7 H7A 122.6 . . ? N4 C8 N6 110.1(4) . . ? N4 C8 H8A 124.9 . . ? N6 C8 H8A 124.9 . . ? N7 C9 S1 178.9(4) . . ? Cl1 C10 Cl2 120.5(8) . . ? Cl1 C10 H10B 107.2 . . ? Cl2 C10 H10B 107.2 . . ? Cl1 C10 H10A 107.2 . . ? Cl2 C10 H10A 107.2 . . ? H10B C10 H10A 106.8 . . ? 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 C4 N1 N2 C3 0.2(4) . . . . ? C1 N1 N2 C3 -177.1(4) . . . . ? N7 Mn1 N3 C4 2.7(4) 2 . . . ? N7 Mn1 N3 C4 -177.3(4) . . . . ? N6 Mn1 N3 C4 -86.9(4) 2 . . . ? N6 Mn1 N3 C4 93.1(4) . . . . ? N7 Mn1 N3 C3 -166.5(3) 2 . . . ? N7 Mn1 N3 C3 13.5(3) . . . . ? N6 Mn1 N3 C3 103.9(3) 2 . . . ? N6 Mn1 N3 C3 -76.1(3) . . . . ? C8 N4 N5 C7 0.1(5) . . . . ? C5 N4 N5 C7 177.0(4) . . . . ? N7 Mn1 N6 C8 -130.9(4) 2 . . . ? N7 Mn1 N6 C8 49.1(4) . . . . ? N3 Mn1 N6 C8 -39.7(4) 2 . . . ? N3 Mn1 N6 C8 140.3(4) . . . . ? N7 Mn1 N6 C7 41.6(4) 2 . . . ? N7 Mn1 N6 C7 -138.4(4) . . . . ? N3 Mn1 N6 C7 132.7(4) 2 . . . ? N3 Mn1 N6 C7 -47.3(4) . . . . ? N3 Mn1 N7 C9 53.5(11) 2 . . . ? N3 Mn1 N7 C9 -126.5(11) . . . . ? N6 Mn1 N7 C9 140.5(11) 2 . . . ? N6 Mn1 N7 C9 -39.5(11) . . . . ? C4 N1 C1 C2 10.5(7) . . . . ? N2 N1 C1 C2 -172.8(4) . . . . ? N1 C1 C2 C2 -175.8(4) . . . 2_645 ? N1 N2 C3 N3 -0.5(5) . . . . ? C4 N3 C3 N2 0.6(5) . . . . ? Mn1 N3 C3 N2 172.4(3) . . . . ? N2 N1 C4 N3 0.2(5) . . . . ? C1 N1 C4 N3 177.1(4) . . . . ? C3 N3 C4 N1 -0.5(5) . . . . ? Mn1 N3 C4 N1 -171.3(3) . . . . ? C8 N4 C5 C6 101.3(5) . . . . ? N5 N4 C5 C6 -74.9(5) . . . . ? N4 C5 C6 C6 179.7(5) . . . 2_456 ? N4 N5 C7 N6 0.3(5) . . . . ? C8 N6 C7 N5 -0.7(5) . . . . ? Mn1 N6 C7 N5 -174.7(3) . . . . ? N5 N4 C8 N6 -0.6(5) . . . . ? C5 N4 C8 N6 -177.1(4) . . . . ? C7 N6 C8 N4 0.7(5) . . . . ? Mn1 N6 C8 N4 174.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.854 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.118 ###====== data_[Mn(btb)2(NCS)2](CH3NO2)2(2) _database_code_depnum_ccdc_archive 'CCDC 714833' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H30 Mn N16 O4 S2' _chemical_formula_weight 677.66 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' Mn Mn 0.3368 0.7283 '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' S S 0.1246 0.1234 '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' _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 8.6873(10) _cell_length_b 8.9324(11) _cell_length_c 10.5653(15) _cell_angle_alpha 82.685(8) _cell_angle_beta 84.302(9) _cell_angle_gamma 70.617(6) _cell_volume 765.66(17) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2717 _cell_measurement_theta_min 3.0677 _cell_measurement_theta_max 25.3491 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 351 _exptl_absorpt_coefficient_mu 0.624 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8349 _exptl_absorpt_correction_T_max 0.9402 _exptl_absorpt_process_details Empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 7599 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0322 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 25.34 _reflns_number_total 2791 _reflns_number_gt 2387 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and Rfactors 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^)+(0.0446P)^2^+0.3811P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2791 _refine_ls_number_parameters 197 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.0940 _refine_ls_wR_factor_gt 0.0882 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 0.0000 0.5000 0.0000 0.01930(15) Uani 1 2 d S . . S1 S 0.55201(8) 0.18429(10) 0.12975(6) 0.0421(2) Uani 1 1 d . . . O1 O 0.0794(3) 0.2804(3) 0.5267(3) 0.0856(9) Uani 1 1 d . . . O2 O 0.3349(3) 0.1845(2) 0.5505(2) 0.0549(6) Uani 1 1 d . . . N1 N 0.1907(2) 0.8265(2) 0.16464(17) 0.0230(4) Uani 1 1 d . . . N2 N 0.0328(2) 0.9220(2) 0.16701(19) 0.0299(5) Uani 1 1 d . . . N3 N 0.0578(2) 0.6884(2) 0.09464(17) 0.0238(4) Uani 1 1 d . . . N4 N 0.2313(2) 0.6982(2) 0.66069(17) 0.0226(4) Uani 1 1 d . . . N5 N 0.3182(3) 0.5418(2) 0.6500(2) 0.0354(5) Uani 1 1 d . . . N6 N 0.1346(2) 0.5668(2) 0.81823(17) 0.0234(4) Uani 1 1 d . . . N7 N 0.2328(2) 0.3204(2) 0.05316(19) 0.0302(5) Uani 1 1 d . . . N8 N 0.2183(3) 0.2758(3) 0.4969(2) 0.0377(5) Uani 1 1 d . . . C1 C 0.3198(3) 0.8815(3) 0.2015(2) 0.0286(5) Uani 1 1 d . . . H1A H 0.3249 0.9758 0.1430 0.034 Uiso 1 1 calc R . . H1B H 0.4265 0.7963 0.1925 0.034 Uiso 1 1 calc R . . C2 C 0.2903(3) 0.9252(3) 0.3387(2) 0.0254(5) Uani 1 1 d . . . H2A H 0.3800 0.9615 0.3594 0.030 Uiso 1 1 calc R . . H2B H 0.1868 1.0149 0.3463 0.030 Uiso 1 1 calc R . . C3 C 0.2810(3) 0.7855(3) 0.4343(2) 0.0255(5) Uani 1 1 d . . . H3A H 0.1868 0.7538 0.4170 0.031 Uiso 1 1 calc R . . H3B H 0.3815 0.6936 0.4228 0.031 Uiso 1 1 calc R . . C4 C 0.2624(3) 0.8257(3) 0.5714(2) 0.0261(5) Uani 1 1 d . . . H4A H 0.3635 0.8426 0.5928 0.031 Uiso 1 1 calc R . . H4B H 0.1708 0.9262 0.5804 0.031 Uiso 1 1 calc R . . C5 C -0.0418(3) 0.8343(3) 0.1241(2) 0.0281(5) Uani 1 1 d . . . H5A H -0.1563 0.8700 0.1144 0.034 Uiso 1 1 calc R . . C6 C 0.2039(3) 0.6887(3) 0.1217(2) 0.0239(5) Uani 1 1 d . . . H6A H 0.3031 0.6032 0.1119 0.029 Uiso 1 1 calc R . . C7 C 0.2543(3) 0.4694(3) 0.7460(2) 0.0329(6) Uani 1 1 d . . . H7A H 0.2894 0.3566 0.7636 0.040 Uiso 1 1 calc R . . C8 C 0.1248(3) 0.7103(3) 0.7607(2) 0.0226(5) Uani 1 1 d . . . H8A H 0.0518 0.8079 0.7875 0.027 Uiso 1 1 calc R . . C9 C 0.3661(3) 0.2637(3) 0.0836(2) 0.0231(5) Uani 1 1 d . . . C10 C 0.2468(4) 0.3860(4) 0.3892(3) 0.0501(8) Uani 1 1 d . . . H10A H 0.1421 0.4641 0.3648 0.075 Uiso 1 1 calc R . . H10B H 0.3000 0.3260 0.3166 0.075 Uiso 1 1 calc R . . H10C H 0.3174 0.4415 0.4143 0.075 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 0.0213(3) 0.0192(3) 0.0177(2) -0.00333(18) -0.00190(18) -0.0062(2) S1 0.0229(3) 0.0705(5) 0.0316(4) -0.0089(3) -0.0047(3) -0.0112(3) O1 0.0382(13) 0.091(2) 0.123(2) 0.0141(17) 0.0118(14) -0.0291(14) O2 0.0524(13) 0.0403(11) 0.0701(15) -0.0016(11) -0.0182(11) -0.0098(10) N1 0.0279(10) 0.0243(10) 0.0195(9) -0.0038(8) -0.0027(8) -0.0111(9) N2 0.0339(12) 0.0239(10) 0.0326(11) -0.0083(9) -0.0056(9) -0.0075(9) N3 0.0267(10) 0.0232(10) 0.0229(10) -0.0052(8) -0.0019(8) -0.0089(9) N4 0.0253(10) 0.0216(9) 0.0209(9) -0.0027(8) -0.0008(8) -0.0076(8) N5 0.0406(12) 0.0248(11) 0.0313(11) -0.0024(9) 0.0103(10) -0.0016(10) N6 0.0249(10) 0.0230(10) 0.0216(9) -0.0039(8) 0.0025(8) -0.0073(8) N7 0.0292(11) 0.0263(11) 0.0323(11) -0.0024(9) -0.0076(9) -0.0038(9) N8 0.0355(13) 0.0363(12) 0.0439(13) -0.0137(11) 0.0033(11) -0.0131(11) C1 0.0356(13) 0.0356(13) 0.0234(12) -0.0038(10) -0.0017(10) -0.0229(12) C2 0.0309(13) 0.0282(12) 0.0220(12) -0.0027(10) -0.0051(10) -0.0153(11) C3 0.0304(12) 0.0258(12) 0.0230(12) -0.0024(10) -0.0010(10) -0.0130(11) C4 0.0316(13) 0.0261(12) 0.0234(12) -0.0008(10) -0.0012(10) -0.0139(11) C5 0.0286(13) 0.0233(12) 0.0316(13) -0.0080(10) -0.0060(10) -0.0039(10) C6 0.0277(12) 0.0224(11) 0.0225(11) -0.0047(9) 0.0000(9) -0.0088(10) C7 0.0386(14) 0.0231(12) 0.0302(13) -0.0026(10) 0.0071(11) -0.0034(11) C8 0.0251(12) 0.0221(11) 0.0208(11) -0.0046(9) -0.0006(9) -0.0072(10) C9 0.0300(13) 0.0245(12) 0.0176(11) -0.0044(9) 0.0013(10) -0.0125(11) C10 0.065(2) 0.0450(17) 0.0381(16) -0.0064(13) 0.0084(14) -0.0176(16) _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 N7 2.196(2) 2_565 ? Mn1 N7 2.196(2) . ? Mn1 N6 2.2667(18) 1_554 ? Mn1 N6 2.2667(18) 2_566 ? Mn1 N3 2.2740(17) . ? Mn1 N3 2.2740(17) 2_565 ? S1 C9 1.630(2) . ? O1 N8 1.204(3) . ? O2 N8 1.208(3) . ? N1 C6 1.331(3) . ? N1 N2 1.354(3) . ? N1 C1 1.467(3) . ? N2 C5 1.314(3) . ? N3 C6 1.330(3) . ? N3 C5 1.358(3) . ? N4 C8 1.324(3) . ? N4 N5 1.363(3) . ? N4 C4 1.463(3) . ? N5 C7 1.310(3) . ? N6 C8 1.326(3) . ? N6 C7 1.353(3) . ? N6 Mn1 2.2667(18) 1_556 ? N7 C9 1.159(3) . ? N8 C10 1.465(4) . ? C1 C2 1.524(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.521(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.517(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 H8A 0.9500 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Mn1 N7 180.00(15) 2_565 . ? N7 Mn1 N6 92.56(7) 2_565 1_554 ? N7 Mn1 N6 87.44(7) . 1_554 ? N7 Mn1 N6 87.44(7) 2_565 2_566 ? N7 Mn1 N6 92.56(7) . 2_566 ? N6 Mn1 N6 180.0 1_554 2_566 ? N7 Mn1 N3 88.68(7) 2_565 . ? N7 Mn1 N3 91.32(7) . . ? N6 Mn1 N3 88.79(6) 1_554 . ? N6 Mn1 N3 91.21(6) 2_566 . ? N7 Mn1 N3 91.32(7) 2_565 2_565 ? N7 Mn1 N3 88.68(7) . 2_565 ? N6 Mn1 N3 91.21(6) 1_554 2_565 ? N6 Mn1 N3 88.79(6) 2_566 2_565 ? N3 Mn1 N3 180.00(8) . 2_565 ? C6 N1 N2 110.05(18) . . ? C6 N1 C1 128.9(2) . . ? N2 N1 C1 120.98(18) . . ? C5 N2 N1 102.67(18) . . ? C6 N3 C5 102.60(18) . . ? C6 N3 Mn1 127.48(15) . . ? C5 N3 Mn1 129.54(15) . . ? C8 N4 N5 109.86(18) . . ? C8 N4 C4 128.62(19) . . ? N5 N4 C4 121.51(18) . . ? C7 N5 N4 102.17(19) . . ? C8 N6 C7 102.46(18) . . ? C8 N6 Mn1 129.17(15) . 1_556 ? C7 N6 Mn1 128.23(15) . 1_556 ? C9 N7 Mn1 160.93(19) . . ? O1 N8 O2 123.5(3) . . ? O1 N8 C10 118.1(3) . . ? O2 N8 C10 118.4(2) . . ? N1 C1 C2 111.91(18) . . ? N1 C1 H1A 109.2 . . ? C2 C1 H1A 109.2 . . ? N1 C1 H1B 109.2 . . ? C2 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? C3 C2 C1 112.18(19) . . ? C3 C2 H2A 109.2 . . ? C1 C2 H2A 109.2 . . ? C3 C2 H2B 109.2 . . ? C1 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? C4 C3 C2 112.26(18) . . ? C4 C3 H3A 109.2 . . ? C2 C3 H3A 109.2 . . ? C4 C3 H3B 109.2 . . ? C2 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? N4 C4 C3 111.37(18) . . ? N4 C4 H4A 109.4 . . ? C3 C4 H4A 109.4 . . ? N4 C4 H4B 109.4 . . ? C3 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? N2 C5 N3 114.7(2) . . ? N2 C5 H5A 122.7 . . ? N3 C5 H5A 122.7 . . ? N3 C6 N1 110.0(2) . . ? N3 C6 H6A 125.0 . . ? N1 C6 H6A 125.0 . . ? N5 C7 N6 115.2(2) . . ? N5 C7 H7A 122.4 . . ? N6 C7 H7A 122.4 . . ? N4 C8 N6 110.3(2) . . ? N4 C8 H8A 124.8 . . ? N6 C8 H8A 124.8 . . ? N7 C9 S1 178.7(2) . . ? N8 C10 H10A 109.5 . . ? N8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 N1 N2 C5 -0.1(2) . . . . ? C1 N1 N2 C5 177.77(19) . . . . ? N7 Mn1 N3 C6 -158.83(19) 2_565 . . . ? N7 Mn1 N3 C6 21.17(19) . . . . ? N6 Mn1 N3 C6 -66.24(19) 1_554 . . . ? N6 Mn1 N3 C6 113.76(19) 2_566 . . . ? N7 Mn1 N3 C5 12.9(2) 2_565 . . . ? N7 Mn1 N3 C5 -167.1(2) . . . . ? N6 Mn1 N3 C5 105.4(2) 1_554 . . . ? N6 Mn1 N3 C5 -74.6(2) 2_566 . . . ? C8 N4 N5 C7 0.9(3) . . . . ? C4 N4 N5 C7 179.7(2) . . . . ? N6 Mn1 N7 C9 68.1(6) 1_554 . . . ? N6 Mn1 N7 C9 -111.9(6) 2_566 . . . ? N3 Mn1 N7 C9 -20.7(6) . . . . ? N3 Mn1 N7 C9 159.3(6) 2_565 . . . ? C6 N1 C1 C2 -122.9(2) . . . . ? N2 N1 C1 C2 59.7(3) . . . . ? N1 C1 C2 C3 58.8(3) . . . . ? C1 C2 C3 C4 176.3(2) . . . . ? C8 N4 C4 C3 -136.8(2) . . . . ? N5 N4 C4 C3 44.6(3) . . . . ? C2 C3 C4 N4 172.22(18) . . . . ? N1 N2 C5 N3 0.2(3) . . . . ? C6 N3 C5 N2 -0.2(3) . . . . ? Mn1 N3 C5 N2 -173.41(15) . . . . ? C5 N3 C6 N1 0.1(2) . . . . ? Mn1 N3 C6 N1 173.52(14) . . . . ? N2 N1 C6 N3 0.0(3) . . . . ? C1 N1 C6 N3 -177.65(19) . . . . ? N4 N5 C7 N6 -0.7(3) . . . . ? C8 N6 C7 N5 0.3(3) . . . . ? Mn1 N6 C7 N5 -175.62(17) 1_556 . . . ? N5 N4 C8 N6 -0.7(3) . . . . ? C4 N4 C8 N6 -179.5(2) . . . . ? C7 N6 C8 N4 0.3(2) . . . . ? Mn1 N6 C8 N4 176.15(13) 1_556 . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.334 _refine_diff_density_min -0.457 _refine_diff_density_rms 0.053 ###====== data_[2D-Mn(btb)2(NCS)2][1D-Mn(btb)2(NCS)2](3) _database_code_depnum_ccdc_archive 'CCDC 714834' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H48 Mn2 N28 S4' _chemical_formula_weight 1111.14 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' Mn Mn 0.3368 0.7283 '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' S S 0.1246 0.1234 '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 9.0938(17) _cell_length_b 10.587(2) _cell_length_c 13.567(3) _cell_angle_alpha 103.854(4) _cell_angle_beta 100.129(5) _cell_angle_gamma 99.920(4) _cell_volume 1216.7(5) _cell_formula_units_Z 1 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 4935 _cell_measurement_theta_min 3.1052 _cell_measurement_theta_max 25.3491 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 574 _exptl_absorpt_coefficient_mu 0.753 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7785 _exptl_absorpt_correction_T_max 0.8827 _exptl_absorpt_process_details Empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'Rigaku Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12168 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 25.35 _reflns_number_total 4440 _reflns_number_gt 3951 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and Rfactors 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^)+(0.0325P)^2^+0.5106P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4440 _refine_ls_number_parameters 319 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0722 _refine_ls_wR_factor_gt 0.0693 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 0.0000 1.0000 0.5000 0.01793(10) Uani 1 2 d S . . Mn2 Mn 1.0000 0.5000 1.0000 0.01897(10) Uani 1 2 d S . . S1 S -0.41579(6) 0.62363(5) 0.26838(4) 0.03142(13) Uani 1 1 d . . . S2 S 1.10509(6) 0.60221(5) 0.67582(4) 0.03300(14) Uani 1 1 d . . . N1 N 0.29709(16) 0.70601(15) 0.47147(12) 0.0213(3) Uani 1 1 d . . . N2 N 0.40759(17) 0.81955(15) 0.49354(13) 0.0255(4) Uani 1 1 d . . . N3 N 0.17525(17) 0.86769(15) 0.49169(12) 0.0214(3) Uani 1 1 d . . . N4 N 0.01580(17) 0.91486(15) 0.80117(12) 0.0235(3) Uani 1 1 d . . . N5 N -0.12856(18) 0.83964(17) 0.75668(13) 0.0291(4) Uani 1 1 d . . . N6 N -0.03938(17) 0.94855(15) 0.64791(12) 0.0225(3) Uani 1 1 d . . . N7 N -0.18203(18) 0.82814(16) 0.40680(14) 0.0303(4) Uani 1 1 d . . . N8 N 0.62702(17) 0.68085(15) 0.89527(12) 0.0222(3) Uani 1 1 d . . . N9 N 0.6036(2) 0.69440(18) 0.99303(13) 0.0336(4) Uani 1 1 d . . . N10 N 0.79992(17) 0.59530(15) 0.97152(12) 0.0220(3) Uani 1 1 d . . . N11 N 0.63776(17) 1.15259(15) 0.81987(12) 0.0233(3) Uani 1 1 d . . . N12 N 0.73206(19) 1.13366(16) 0.75265(13) 0.0301(4) Uani 1 1 d . . . N13 N 0.84419(17) 1.30945(15) 0.89245(12) 0.0230(3) Uani 1 1 d . . . N14 N 1.07287(19) 0.54225(17) 0.86171(14) 0.0314(4) Uani 1 1 d . . . C1 C 0.3285(2) 0.91325(19) 0.50515(15) 0.0245(4) Uani 1 1 d . . . H1A H 0.3751 1.0055 0.5216 0.029 Uiso 1 1 calc R . . C2 C 0.1605(2) 0.73621(18) 0.47012(14) 0.0219(4) Uani 1 1 d . . . H2A H 0.0662 0.6730 0.4558 0.026 Uiso 1 1 calc R . . C3 C 0.3337(2) 0.57370(18) 0.44496(15) 0.0253(4) Uani 1 1 d . . . H3A H 0.3466 0.5517 0.3723 0.030 Uiso 1 1 calc R . . H3B H 0.2467 0.5060 0.4488 0.030 Uiso 1 1 calc R . . C4 C 0.4781(2) 0.56668(18) 0.51678(15) 0.0256(4) Uani 1 1 d . . . H4A H 0.4621 0.5809 0.5886 0.031 Uiso 1 1 calc R . . H4B H 0.5634 0.6392 0.5175 0.031 Uiso 1 1 calc R . . C5 C -0.1555(2) 0.86423(19) 0.66536(15) 0.0272(4) Uani 1 1 d . . . H5A H -0.2496 0.8256 0.6153 0.033 Uiso 1 1 calc R . . C6 C 0.0660(2) 0.97776(19) 0.73564(14) 0.0239(4) Uani 1 1 d . . . H6A H 0.1639 1.0357 0.7498 0.029 Uiso 1 1 calc R . . C7 C 0.1021(2) 0.9065(2) 0.90069(15) 0.0301(5) Uani 1 1 d . . . H7A H 0.2008 0.9731 0.9218 0.036 Uiso 1 1 calc R . . H7B H 0.1251 0.8169 0.8909 0.036 Uiso 1 1 calc R . . C8 C 0.0163(2) 0.93105(18) 0.98703(14) 0.0248(4) Uani 1 1 d . . . H8A H -0.0820 0.8639 0.9660 0.030 Uiso 1 1 calc R . . H8B H 0.0774 0.9183 1.0505 0.030 Uiso 1 1 calc R . . C9 C -0.2788(2) 0.74146(18) 0.35021(15) 0.0225(4) Uani 1 1 d . . . C10 C 0.7098(2) 0.6407(2) 1.03526(16) 0.0323(5) Uani 1 1 d . . . H10A H 0.7222 0.6344 1.1048 0.039 Uiso 1 1 calc R . . C11 C 0.7426(2) 0.62222(17) 0.88378(15) 0.0220(4) Uani 1 1 d . . . H11A H 0.7793 0.6022 0.8217 0.026 Uiso 1 1 calc R . . C12 C 0.8536(2) 1.23041(19) 0.79982(15) 0.0277(4) Uani 1 1 d . . . H12A H 0.9414 1.2440 0.7713 0.033 Uiso 1 1 calc R . . C13 C 0.7050(2) 1.25684(18) 0.90086(15) 0.0233(4) Uani 1 1 d . . . H13A H 0.6601 1.2895 0.9572 0.028 Uiso 1 1 calc R . . C14 C 0.5335(2) 0.72879(18) 0.81963(15) 0.0266(4) Uani 1 1 d . . . H14A H 0.4247 0.6831 0.8079 0.032 Uiso 1 1 calc R . . H14B H 0.5648 0.7056 0.7524 0.032 Uiso 1 1 calc R . . C15 C 0.5485(2) 0.87827(18) 0.85535(15) 0.0249(4) Uani 1 1 d . . . H15A H 0.6582 0.9242 0.8787 0.030 Uiso 1 1 calc R . . H15B H 0.4993 0.9007 0.9149 0.030 Uiso 1 1 calc R . . C16 C 0.4718(2) 0.92494(18) 0.76578(15) 0.0259(4) Uani 1 1 d . . . H16A H 0.5205 0.8999 0.7064 0.031 Uiso 1 1 calc R . . H16B H 0.3626 0.8774 0.7429 0.031 Uiso 1 1 calc R . . C17 C 0.4808(2) 1.07438(18) 0.79268(17) 0.0288(4) Uani 1 1 d . . . H17A H 0.4224 1.0956 0.7323 0.035 Uiso 1 1 calc R . . H17B H 0.4321 1.1000 0.8520 0.035 Uiso 1 1 calc R . . C18 C 1.0863(2) 0.56514(18) 0.78345(15) 0.0237(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.01759(19) 0.0192(2) 0.0187(2) 0.00664(16) 0.00455(15) 0.00627(16) Mn2 0.0180(2) 0.0189(2) 0.0212(2) 0.00790(16) 0.00364(15) 0.00495(16) S1 0.0362(3) 0.0239(3) 0.0272(3) 0.0029(2) 0.0034(2) -0.0017(2) S2 0.0365(3) 0.0394(3) 0.0245(3) 0.0141(2) 0.0072(2) 0.0048(2) N1 0.0199(8) 0.0190(8) 0.0257(9) 0.0060(7) 0.0054(6) 0.0063(6) N2 0.0199(8) 0.0205(8) 0.0357(10) 0.0053(7) 0.0076(7) 0.0059(7) N3 0.0204(8) 0.0228(8) 0.0249(9) 0.0096(7) 0.0082(6) 0.0077(6) N4 0.0245(8) 0.0271(9) 0.0190(8) 0.0058(7) 0.0047(6) 0.0073(7) N5 0.0281(9) 0.0314(9) 0.0272(9) 0.0103(8) 0.0070(7) 0.0014(7) N6 0.0227(8) 0.0251(8) 0.0212(8) 0.0070(7) 0.0068(6) 0.0067(7) N7 0.0273(9) 0.0255(9) 0.0348(10) 0.0069(8) 0.0024(8) 0.0040(8) N8 0.0222(8) 0.0207(8) 0.0244(9) 0.0076(7) 0.0031(6) 0.0069(7) N9 0.0366(10) 0.0456(11) 0.0314(10) 0.0183(9) 0.0161(8) 0.0237(9) N10 0.0230(8) 0.0207(8) 0.0247(9) 0.0089(7) 0.0054(6) 0.0073(7) N11 0.0222(8) 0.0185(8) 0.0298(9) 0.0072(7) 0.0055(7) 0.0059(6) N12 0.0337(9) 0.0267(9) 0.0277(9) 0.0041(7) 0.0081(7) 0.0050(8) N13 0.0229(8) 0.0208(8) 0.0243(9) 0.0052(7) 0.0047(6) 0.0050(7) N14 0.0333(9) 0.0345(10) 0.0311(10) 0.0142(8) 0.0119(8) 0.0087(8) C1 0.0224(9) 0.0221(10) 0.0294(11) 0.0068(8) 0.0070(8) 0.0052(8) C2 0.0190(9) 0.0242(10) 0.0250(10) 0.0099(8) 0.0057(7) 0.0067(8) C3 0.0259(10) 0.0186(9) 0.0290(11) 0.0017(8) 0.0029(8) 0.0089(8) C4 0.0283(10) 0.0223(10) 0.0242(10) 0.0029(8) 0.0009(8) 0.0110(8) C5 0.0267(10) 0.0296(11) 0.0231(10) 0.0070(9) 0.0047(8) 0.0019(8) C6 0.0202(9) 0.0269(10) 0.0252(10) 0.0077(8) 0.0058(8) 0.0057(8) C7 0.0339(11) 0.0367(11) 0.0215(10) 0.0085(9) 0.0018(8) 0.0167(9) C8 0.0317(10) 0.0222(10) 0.0209(10) 0.0085(8) 0.0033(8) 0.0059(8) C9 0.0256(10) 0.0225(10) 0.0242(10) 0.0114(8) 0.0072(8) 0.0092(8) C10 0.0377(12) 0.0429(12) 0.0276(11) 0.0174(10) 0.0133(9) 0.0217(10) C11 0.0230(9) 0.0192(9) 0.0234(10) 0.0046(8) 0.0048(7) 0.0056(8) C12 0.0296(10) 0.0260(10) 0.0297(11) 0.0085(9) 0.0103(8) 0.0070(9) C13 0.0242(10) 0.0185(9) 0.0266(10) 0.0050(8) 0.0046(8) 0.0061(8) C14 0.0244(10) 0.0230(10) 0.0289(11) 0.0070(8) -0.0034(8) 0.0060(8) C15 0.0247(10) 0.0218(10) 0.0256(10) 0.0048(8) 0.0002(8) 0.0062(8) C16 0.0236(10) 0.0196(9) 0.0293(11) 0.0054(8) -0.0041(8) 0.0030(8) C17 0.0206(9) 0.0219(10) 0.0398(12) 0.0083(9) -0.0027(8) 0.0040(8) C18 0.0195(9) 0.0215(9) 0.0291(11) 0.0063(8) 0.0052(8) 0.0032(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 N7 2.1849(17) 2_576 ? Mn1 N7 2.1849(17) . ? Mn1 N6 2.2718(16) . ? Mn1 N6 2.2718(16) 2_576 ? Mn1 N3 2.2960(14) 2_576 ? Mn1 N3 2.2960(15) . ? Mn2 N14 2.2128(17) 2_767 ? Mn2 N14 2.2128(17) . ? Mn2 N10 2.2472(15) 2_767 ? Mn2 N10 2.2472(15) . ? Mn2 N13 2.2550(16) 2_777 ? Mn2 N13 2.2550(16) 1_545 ? S1 C9 1.630(2) . ? S2 C18 1.629(2) . ? N1 C2 1.333(2) . ? N1 N2 1.360(2) . ? N1 C3 1.471(2) . ? N2 C1 1.318(2) . ? N3 C2 1.330(2) . ? N3 C1 1.358(2) . ? N4 C6 1.328(2) . ? N4 N5 1.361(2) . ? N4 C7 1.468(2) . ? N5 C5 1.316(2) . ? N6 C6 1.323(2) . ? N6 C5 1.354(2) . ? N7 C9 1.163(2) . ? N8 C11 1.323(2) . ? N8 N9 1.358(2) . ? N8 C14 1.458(2) . ? N9 C10 1.317(3) . ? N10 C11 1.329(2) . ? N10 C10 1.355(2) . ? N11 C13 1.323(2) . ? N11 N12 1.362(2) . ? N11 C17 1.456(2) . ? N12 C12 1.315(3) . ? N13 C13 1.328(2) . ? N13 C12 1.359(2) . ? N13 Mn2 2.2550(15) 1_565 ? N14 C18 1.166(2) . ? C1 H1A 0.9500 . ? C2 H2A 0.9500 . ? C3 C4 1.516(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C4 1.520(3) 2_666 ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C8 1.514(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C8 1.511(4) 2_577 ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C15 1.514(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.522(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.520(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? 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 N7 Mn1 N7 180.0 2_576 . ? N7 Mn1 N6 89.92(6) 2_576 . ? N7 Mn1 N6 90.08(6) . . ? N7 Mn1 N6 90.08(6) 2_576 2_576 ? N7 Mn1 N6 89.92(6) . 2_576 ? N6 Mn1 N6 180.0 . 2_576 ? N7 Mn1 N3 89.98(6) 2_576 2_576 ? N7 Mn1 N3 90.02(6) . 2_576 ? N6 Mn1 N3 91.30(5) . 2_576 ? N6 Mn1 N3 88.70(5) 2_576 2_576 ? N7 Mn1 N3 90.02(6) 2_576 . ? N7 Mn1 N3 89.98(6) . . ? N6 Mn1 N3 88.70(5) . . ? N6 Mn1 N3 91.30(5) 2_576 . ? N3 Mn1 N3 180.000(1) 2_576 . ? N14 Mn2 N14 180.000(1) 2_767 . ? N14 Mn2 N10 90.75(6) 2_767 2_767 ? N14 Mn2 N10 89.25(6) . 2_767 ? N14 Mn2 N10 89.25(6) 2_767 . ? N14 Mn2 N10 90.75(6) . . ? N10 Mn2 N10 180.000(1) 2_767 . ? N14 Mn2 N13 87.84(6) 2_767 2_777 ? N14 Mn2 N13 92.16(6) . 2_777 ? N10 Mn2 N13 86.35(6) 2_767 2_777 ? N10 Mn2 N13 93.65(6) . 2_777 ? N14 Mn2 N13 92.16(6) 2_767 1_545 ? N14 Mn2 N13 87.84(6) . 1_545 ? N10 Mn2 N13 93.65(6) 2_767 1_545 ? N10 Mn2 N13 86.35(6) . 1_545 ? N13 Mn2 N13 180.0 2_777 1_545 ? C2 N1 N2 109.87(14) . . ? C2 N1 C3 128.80(15) . . ? N2 N1 C3 121.11(14) . . ? C1 N2 N1 102.50(14) . . ? C2 N3 C1 102.67(15) . . ? C2 N3 Mn1 132.49(12) . . ? C1 N3 Mn1 124.79(12) . . ? C6 N4 N5 109.71(15) . . ? C6 N4 C7 128.15(16) . . ? N5 N4 C7 121.61(15) . . ? C5 N5 N4 102.13(15) . . ? C6 N6 C5 102.38(16) . . ? C6 N6 Mn1 125.13(12) . . ? C5 N6 Mn1 131.38(13) . . ? C9 N7 Mn1 174.19(16) . . ? C11 N8 N9 110.10(15) . . ? C11 N8 C14 128.44(16) . . ? N9 N8 C14 121.45(15) . . ? C10 N9 N8 102.42(15) . . ? C11 N10 C10 102.69(15) . . ? C11 N10 Mn2 126.45(12) . . ? C10 N10 Mn2 130.86(13) . . ? C13 N11 N12 109.94(15) . . ? C13 N11 C17 128.65(17) . . ? N12 N11 C17 120.97(16) . . ? C12 N12 N11 102.30(15) . . ? C13 N13 C12 102.36(16) . . ? C13 N13 Mn2 125.50(13) . 1_565 ? C12 N13 Mn2 131.63(13) . 1_565 ? C18 N14 Mn2 168.81(15) . . ? N2 C1 N3 114.78(17) . . ? N2 C1 H1A 122.6 . . ? N3 C1 H1A 122.6 . . ? N3 C2 N1 110.17(16) . . ? N3 C2 H2A 124.9 . . ? N1 C2 H2A 124.9 . . ? N1 C3 C4 112.64(15) . . ? N1 C3 H3A 109.1 . . ? C4 C3 H3A 109.1 . . ? N1 C3 H3B 109.1 . . ? C4 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? C3 C4 C4 112.12(19) . 2_666 ? C3 C4 H4A 109.2 . . ? C4 C4 H4A 109.2 2_666 . ? C3 C4 H4B 109.2 . . ? C4 C4 H4B 109.2 2_666 . ? H4A C4 H4B 107.9 . . ? N5 C5 N6 115.14(17) . . ? N5 C5 H5A 122.4 . . ? N6 C5 H5A 122.4 . . ? N6 C6 N4 110.64(16) . . ? N6 C6 H6A 124.7 . . ? N4 C6 H6A 124.7 . . ? N4 C7 C8 112.90(16) . . ? N4 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? N4 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C8 C8 C7 113.4(2) 2_577 . ? C8 C8 H8A 108.9 2_577 . ? C7 C8 H8A 108.9 . . ? C8 C8 H8B 108.9 2_577 . ? C7 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? N7 C9 S1 177.93(17) . . ? N9 C10 N10 114.58(18) . . ? N9 C10 H10A 122.7 . . ? N10 C10 H10A 122.7 . . ? N8 C11 N10 110.21(16) . . ? N8 C11 H11A 124.9 . . ? N10 C11 H11A 124.9 . . ? N12 C12 N13 114.87(17) . . ? N12 C12 H12A 122.6 . . ? N13 C12 H12A 122.6 . . ? N11 C13 N13 110.52(17) . . ? N11 C13 H13A 124.7 . . ? N13 C13 H13A 124.7 . . ? N8 C14 C15 112.28(15) . . ? N8 C14 H14A 109.1 . . ? C15 C14 H14A 109.1 . . ? N8 C14 H14B 109.1 . . ? C15 C14 H14B 109.1 . . ? H14A C14 H14B 107.9 . . ? C14 C15 C16 109.48(15) . . ? C14 C15 H15A 109.8 . . ? C16 C15 H15A 109.8 . . ? C14 C15 H15B 109.8 . . ? C16 C15 H15B 109.8 . . ? H15A C15 H15B 108.2 . . ? C17 C16 C15 114.08(16) . . ? C17 C16 H16A 108.7 . . ? C15 C16 H16A 108.7 . . ? C17 C16 H16B 108.7 . . ? C15 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? N11 C17 C16 112.61(15) . . ? N11 C17 H17A 109.1 . . ? C16 C17 H17A 109.1 . . ? N11 C17 H17B 109.1 . . ? C16 C17 H17B 109.1 . . ? H17A C17 H17B 107.8 . . ? N14 C18 S2 178.11(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 N1 N2 C1 0.5(2) . . . . ? C3 N1 N2 C1 175.59(16) . . . . ? N7 Mn1 N3 C2 160.67(17) 2_576 . . . ? N7 Mn1 N3 C2 -19.33(17) . . . . ? N6 Mn1 N3 C2 70.76(17) . . . . ? N6 Mn1 N3 C2 -109.24(17) 2_576 . . . ? N7 Mn1 N3 C1 -22.43(15) 2_576 . . . ? N7 Mn1 N3 C1 157.57(15) . . . . ? N6 Mn1 N3 C1 -112.34(15) . . . . ? N6 Mn1 N3 C1 67.66(15) 2_576 . . . ? C6 N4 N5 C5 -0.3(2) . . . . ? C7 N4 N5 C5 -172.61(16) . . . . ? N7 Mn1 N6 C6 -27.83(15) 2_576 . . . ? N7 Mn1 N6 C6 152.17(15) . . . . ? N3 Mn1 N6 C6 -117.81(15) 2_576 . . . ? N3 Mn1 N6 C6 62.19(15) . . . . ? N7 Mn1 N6 C5 166.41(17) 2_576 . . . ? N7 Mn1 N6 C5 -13.59(17) . . . . ? N3 Mn1 N6 C5 76.43(17) 2_576 . . . ? N3 Mn1 N6 C5 -103.57(17) . . . . ? C11 N8 N9 C10 -0.2(2) . . . . ? C14 N8 N9 C10 -179.53(17) . . . . ? N14 Mn2 N10 C11 -163.55(15) 2_767 . . . ? N14 Mn2 N10 C11 16.45(15) . . . . ? N13 Mn2 N10 C11 108.66(15) 2_777 . . . ? N13 Mn2 N10 C11 -71.34(15) 1_545 . . . ? N14 Mn2 N10 C10 17.41(18) 2_767 . . . ? N14 Mn2 N10 C10 -162.59(18) . . . . ? N13 Mn2 N10 C10 -70.37(18) 2_777 . . . ? N13 Mn2 N10 C10 109.63(18) 1_545 . . . ? C13 N11 N12 C12 0.4(2) . . . . ? C17 N11 N12 C12 173.45(16) . . . . ? N10 Mn2 N14 C18 156.9(8) 2_767 . . . ? N10 Mn2 N14 C18 -23.1(8) . . . . ? N13 Mn2 N14 C18 -116.8(8) 2_777 . . . ? N13 Mn2 N14 C18 63.2(8) 1_545 . . . ? N1 N2 C1 N3 -0.2(2) . . . . ? C2 N3 C1 N2 -0.1(2) . . . . ? Mn1 N3 C1 N2 -177.75(12) . . . . ? C1 N3 C2 N1 0.4(2) . . . . ? Mn1 N3 C2 N1 177.80(12) . . . . ? N2 N1 C2 N3 -0.6(2) . . . . ? C3 N1 C2 N3 -175.20(17) . . . . ? C2 N1 C3 C4 -141.12(19) . . . . ? N2 N1 C3 C4 44.8(2) . . . . ? N1 C3 C4 C4 -175.3(2) . . . 2_666 ? N4 N5 C5 N6 0.4(2) . . . . ? C6 N6 C5 N5 -0.2(2) . . . . ? Mn1 N6 C5 N5 167.87(13) . . . . ? C5 N6 C6 N4 0.0(2) . . . . ? Mn1 N6 C6 N4 -169.11(11) . . . . ? N5 N4 C6 N6 0.2(2) . . . . ? C7 N4 C6 N6 171.84(17) . . . . ? C6 N4 C7 C8 134.41(19) . . . . ? N5 N4 C7 C8 -54.9(2) . . . . ? N4 C7 C8 C8 -62.2(3) . . . 2_577 ? N8 N9 C10 N10 0.6(2) . . . . ? C11 N10 C10 N9 -0.7(2) . . . . ? Mn2 N10 C10 N9 178.47(14) . . . . ? N9 N8 C11 N10 -0.2(2) . . . . ? C14 N8 C11 N10 179.02(16) . . . . ? C10 N10 C11 N8 0.5(2) . . . . ? Mn2 N10 C11 N8 -178.71(11) . . . . ? N11 N12 C12 N13 0.3(2) . . . . ? C13 N13 C12 N12 -0.8(2) . . . . ? Mn2 N13 C12 N12 -172.75(13) 1_565 . . . ? N12 N11 C13 N13 -0.9(2) . . . . ? C17 N11 C13 N13 -173.31(17) . . . . ? C12 N13 C13 N11 1.0(2) . . . . ? Mn2 N13 C13 N11 173.63(11) 1_565 . . . ? C11 N8 C14 C15 -117.4(2) . . . . ? N9 N8 C14 C15 61.7(2) . . . . ? N8 C14 C15 C16 169.91(16) . . . . ? C14 C15 C16 C17 -179.62(16) . . . . ? C13 N11 C17 C16 -131.7(2) . . . . ? N12 N11 C17 C16 56.7(2) . . . . ? C15 C16 C17 N11 62.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.230 _refine_diff_density_min -0.267 _refine_diff_density_rms 0.048 ###======