Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Yu-Bin Dong' 'Ru-Qi Huang' 'Guo-Xia Jin' 'Jian-Ping Ma' _publ_contact_author_name 'Prof Yu-Bin Dong' _publ_contact_author_address ; College of Chemistry, Chemical Engineering & Materials Science Shandong Normal University Wenhua east road 88# Jinan Shandong 250014 CHINA ; _publ_contact_author_email YUBINDONG@SDNU.EDU.CN _publ_section_title ; New Ag(I) Inorganic-Organic Coordination Polymers and M(II) (M = Co(II) and Mn(II)) Molecular Complexes Generated from New Type of Fulvene Ligands ; data_3 _database_code_CSD 210651 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H30 Ag0.5 F6 N2 O2 P' _chemical_formula_weight 1243.99 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' Ag Ag -0.8971 1.1015 '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' _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 8.209(3) _cell_length_b 11.951(4) _cell_length_c 15.384(5) _cell_angle_alpha 103.007(6) _cell_angle_beta 94.673(6) _cell_angle_gamma 94.643(6) _cell_volume 1458.0(8) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1008 _cell_measurement_theta_min 2.503 _cell_measurement_theta_max 19.418 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 374.5 _exptl_absorpt_coefficient_mu 0.250 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8778 _exptl_absorpt_correction_T_max 0.9443 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8470 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.1689 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 26.37 _reflns_number_total 5773 _reflns_number_gt 1868 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0407P)^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 5773 _refine_ls_number_parameters 382 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1804 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1211 _refine_ls_wR_factor_gt 0.0951 _refine_ls_goodness_of_fit_ref 0.740 _refine_ls_restrained_S_all 0.740 _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 Ag1 Ag 1.0000 0.0000 1.0000 0.1357(4) Uani 1 2 d S . . F1 F 0.0137(5) 0.6330(3) 0.0252(2) 0.1581(16) Uani 1 1 d . . . F2 F 0.0965(5) 0.5018(4) -0.0822(3) 0.1697(16) Uani 1 1 d . . . F3 F 0.1599(4) 0.4977(3) 0.0608(2) 0.1379(13) Uani 1 1 d . . . N1 N 0.9964(5) 0.0830(3) 0.8864(2) 0.0757(12) Uani 1 1 d . . . N2 N 0.2889(5) -0.0726(4) -0.0265(3) 0.0917(14) Uani 1 1 d . . . O1 O 0.7245(4) -0.0769(3) 0.51254(18) 0.0807(10) Uani 1 1 d . . . H1 H 0.7137 -0.1191 0.4620 0.121 Uiso 1 1 calc R . . O2 O 0.6802(4) -0.1919(2) 0.35599(18) 0.0738(9) Uani 1 1 d . . . P1 P 0.0000 0.5000 0.0000 0.0856(7) Uani 1 2 d S . . C1 C 0.7571(5) 0.0291(4) 0.5076(3) 0.0563(12) Uani 1 1 d . . . C2 C 0.7694(5) 0.0626(3) 0.4266(3) 0.0506(11) Uani 1 1 d . . . C3 C 0.8315(5) 0.1761(3) 0.4217(3) 0.0503(11) Uani 1 1 d . . . H3 H 0.8659 0.2372 0.4708 0.060 Uiso 1 1 calc R . . C4 C 0.8326(5) 0.1811(3) 0.3328(3) 0.0474(11) Uani 1 1 d . . . C5 C 0.7717(5) 0.0714(4) 0.2801(3) 0.0516(11) Uani 1 1 d . . . H5 H 0.7599 0.0522 0.2178 0.062 Uiso 1 1 calc R . . C6 C 0.7312(5) -0.0054(4) 0.3334(3) 0.0488(11) Uani 1 1 d . . . C7 C 0.6786(5) -0.1242(4) 0.3035(3) 0.0532(11) Uani 1 1 d . . . C8 C 0.7784(5) 0.1110(4) 0.5961(3) 0.0530(12) Uani 1 1 d . . . C9 C 0.8565(5) 0.0791(4) 0.6678(3) 0.0524(11) Uani 1 1 d . . . H9 H 0.8983 0.0078 0.6596 0.063 Uiso 1 1 calc R . . C10 C 0.8732(5) 0.1517(4) 0.7514(3) 0.0518(12) Uani 1 1 d . . . C11 C 0.8117(6) 0.2581(4) 0.7655(3) 0.0668(13) Uani 1 1 d . . . H11 H 0.8257 0.3076 0.8222 0.080 Uiso 1 1 calc R . . C12 C 0.7301(6) 0.2895(4) 0.6950(3) 0.0716(14) Uani 1 1 d . . . H12 H 0.6870 0.3603 0.7040 0.086 Uiso 1 1 calc R . . C13 C 0.7116(5) 0.2169(5) 0.6109(3) 0.0697(14) Uani 1 1 d . . . H13 H 0.6543 0.2384 0.5636 0.084 Uiso 1 1 calc R . . C14 C 0.9447(6) 0.1153(4) 0.8265(3) 0.0630(13) Uani 1 1 d . . . C15 C 0.6205(5) -0.1771(4) 0.2086(3) 0.0513(11) Uani 1 1 d . . . C16 C 0.5245(5) -0.1209(4) 0.1568(3) 0.0570(12) Uani 1 1 d . . . H16 H 0.5014 -0.0457 0.1801 0.068 Uiso 1 1 calc R . . C17 C 0.4636(5) -0.1780(4) 0.0701(3) 0.0564(12) Uani 1 1 d . . . C18 C 0.4970(6) -0.2890(5) 0.0340(3) 0.0734(14) Uani 1 1 d . . . H18 H 0.4565 -0.3259 -0.0245 0.088 Uiso 1 1 calc R . . C19 C 0.5917(7) -0.3446(4) 0.0861(4) 0.0824(16) Uani 1 1 d . . . H19 H 0.6149 -0.4198 0.0629 0.099 Uiso 1 1 calc R . . C20 C 0.6508(6) -0.2888(4) 0.1716(3) 0.0676(14) Uani 1 1 d . . . H20 H 0.7137 -0.3273 0.2062 0.081 Uiso 1 1 calc R . . C21 C 0.3639(6) -0.1194(4) 0.0166(3) 0.0649(13) Uani 1 1 d . . . C22 C 0.8990(5) 0.2816(3) 0.2962(3) 0.0528(11) Uani 1 1 d . . . C23 C 1.0451(5) 0.2451(3) 0.2456(3) 0.0501(11) Uani 1 1 d . . . C24 C 1.1731(6) 0.2005(3) 0.2876(3) 0.0583(12) Uani 1 1 d . . . H24 H 1.1667 0.1934 0.3462 0.070 Uiso 1 1 calc R . . C25 C 1.3085(6) 0.1666(4) 0.2455(4) 0.0706(14) Uani 1 1 d . . . H25 H 1.3920 0.1372 0.2755 0.085 Uiso 1 1 calc R . . C26 C 1.3195(6) 0.1764(4) 0.1596(4) 0.0823(15) Uani 1 1 d . . . H26 H 1.4097 0.1526 0.1302 0.099 Uiso 1 1 calc R . . C27 C 1.1973(8) 0.2213(4) 0.1170(3) 0.0817(15) Uani 1 1 d . . . H27 H 1.2063 0.2297 0.0589 0.098 Uiso 1 1 calc R . . C28 C 1.0606(6) 0.2546(4) 0.1588(3) 0.0667(13) Uani 1 1 d . . . H28 H 0.9780 0.2839 0.1281 0.080 Uiso 1 1 calc R . . C29 C 0.7574(5) 0.3091(4) 0.2344(3) 0.0790(15) Uani 1 1 d . . . H29A H 0.7943 0.3729 0.2102 0.118 Uiso 1 1 calc R . . H29B H 0.6665 0.3287 0.2684 0.118 Uiso 1 1 calc R . . H29C H 0.7233 0.2427 0.1863 0.118 Uiso 1 1 calc R . . C30 C 0.9540(6) 0.3870(3) 0.3742(3) 0.0671(13) Uani 1 1 d . . . H30A H 0.8626 0.4042 0.4095 0.080 Uiso 1 1 calc R . . H30B H 1.0417 0.3678 0.4128 0.080 Uiso 1 1 calc R . . C31 C 1.0129(8) 0.4922(5) 0.3437(4) 0.148(3) Uani 1 1 d . . . H31A H 1.0459 0.5548 0.3949 0.221 Uiso 1 1 calc R . . H31B H 0.9257 0.5131 0.3068 0.221 Uiso 1 1 calc R . . H31C H 1.1047 0.4763 0.3096 0.221 Uiso 1 1 calc R . . C32 C 0.5407(8) 0.5497(8) 0.4313(6) 0.108(2) Uani 1 1 d . . . H32 H 0.5673 0.5829 0.3844 0.130 Uiso 1 1 calc R . . C33 C 0.4576(9) 0.4426(8) 0.4141(5) 0.121(2) Uani 1 1 d . . . H33 H 0.4284 0.4022 0.3550 0.145 Uiso 1 1 calc R . . C34 C 0.4161(8) 0.3928(5) 0.4832(8) 0.122(3) Uani 1 1 d . . . H34 H 0.3585 0.3198 0.4705 0.146 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 Ag1 0.1099(6) 0.2339(9) 0.1182(6) 0.1311(6) 0.0330(4) 0.0669(6) F1 0.246(4) 0.075(2) 0.134(3) 0.013(2) -0.063(3) 0.020(2) F2 0.185(4) 0.224(4) 0.146(3) 0.096(3) 0.070(3) 0.088(3) F3 0.142(3) 0.124(2) 0.135(3) 0.019(2) -0.052(2) 0.037(2) N1 0.097(3) 0.085(3) 0.053(3) 0.028(2) 0.004(2) 0.023(2) N2 0.089(3) 0.116(4) 0.068(3) 0.015(3) -0.011(2) 0.032(3) O1 0.121(3) 0.068(2) 0.055(2) 0.0311(18) -0.0032(18) -0.014(2) O2 0.107(3) 0.0584(19) 0.057(2) 0.0272(17) -0.0056(18) -0.0069(17) P1 0.111(2) 0.0714(17) 0.0739(16) 0.0194(13) -0.0073(15) 0.0171(13) C1 0.059(3) 0.067(3) 0.047(3) 0.024(3) 0.003(2) 0.003(3) C2 0.055(3) 0.050(3) 0.045(3) 0.015(2) -0.001(2) -0.004(2) C3 0.058(3) 0.053(3) 0.039(3) 0.012(2) 0.004(2) 0.000(2) C4 0.053(3) 0.047(3) 0.043(3) 0.014(2) 0.005(2) 0.000(2) C5 0.045(3) 0.070(3) 0.044(3) 0.024(3) 0.002(2) 0.002(2) C6 0.048(3) 0.062(3) 0.041(3) 0.023(3) 0.001(2) 0.004(2) C7 0.058(3) 0.045(3) 0.057(3) 0.016(3) 0.005(2) 0.002(2) C8 0.065(3) 0.064(3) 0.037(3) 0.024(3) 0.009(2) 0.013(3) C9 0.062(3) 0.061(3) 0.041(3) 0.022(3) 0.011(2) 0.013(2) C10 0.058(3) 0.065(3) 0.041(3) 0.027(3) 0.010(2) 0.011(3) C11 0.084(4) 0.074(4) 0.045(3) 0.018(3) 0.013(3) 0.008(3) C12 0.094(4) 0.073(3) 0.057(4) 0.029(3) 0.013(3) 0.022(3) C13 0.073(4) 0.098(4) 0.051(3) 0.039(3) 0.011(3) 0.020(3) C14 0.074(3) 0.068(3) 0.049(3) 0.017(3) 0.006(3) 0.011(3) C15 0.050(3) 0.057(3) 0.046(3) 0.015(3) 0.003(2) -0.002(2) C16 0.061(3) 0.058(3) 0.054(3) 0.014(3) 0.013(2) 0.005(2) C17 0.050(3) 0.071(3) 0.046(3) 0.009(3) 0.011(2) 0.007(3) C18 0.084(4) 0.077(4) 0.052(3) 0.000(3) 0.003(3) 0.011(3) C19 0.109(5) 0.060(3) 0.073(4) 0.002(3) 0.008(3) 0.014(3) C20 0.080(4) 0.055(3) 0.065(4) 0.012(3) 0.002(3) 0.005(3) C21 0.054(3) 0.085(4) 0.050(3) 0.005(3) 0.002(2) 0.008(3) C22 0.061(3) 0.056(3) 0.049(3) 0.024(2) 0.011(2) 0.008(3) C23 0.059(3) 0.049(3) 0.042(3) 0.012(2) 0.003(2) -0.001(2) C24 0.069(3) 0.056(3) 0.051(3) 0.014(2) 0.007(3) 0.004(3) C25 0.067(4) 0.071(4) 0.073(4) 0.014(3) 0.009(3) 0.013(3) C26 0.065(4) 0.091(4) 0.088(5) 0.011(4) 0.022(3) 0.004(3) C27 0.095(5) 0.098(4) 0.053(3) 0.022(3) 0.018(3) -0.011(4) C28 0.063(3) 0.081(4) 0.060(3) 0.028(3) 0.005(3) 0.001(3) C29 0.080(4) 0.089(3) 0.081(4) 0.050(3) 0.006(3) 0.009(3) C30 0.097(4) 0.041(3) 0.066(3) 0.017(3) 0.018(3) -0.004(3) C31 0.182(7) 0.125(5) 0.129(6) 0.025(5) 0.028(5) -0.021(5) C32 0.091(5) 0.111(6) 0.120(7) 0.031(5) -0.015(4) 0.008(4) C33 0.117(6) 0.091(6) 0.129(7) -0.011(5) -0.034(5) 0.011(5) C34 0.131(6) 0.066(4) 0.157(8) 0.030(6) -0.040(6) -0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.193(4) . ? Ag1 N1 2.193(4) 2_757 ? Ag1 N2 2.622(4) 2_656 ? Ag1 N2 2.622(4) 1_656 ? F1 P1 1.542(3) . ? F2 P1 1.549(4) . ? F3 P1 1.555(3) . ? N1 C14 1.141(4) . ? N2 C21 1.136(5) . ? N2 Ag1 2.622(4) 1_454 ? O1 C1 1.293(4) . ? O2 C7 1.265(4) . ? P1 F1 1.542(3) 2_565 ? P1 F2 1.549(4) 2_565 ? P1 F3 1.555(3) 2_565 ? C1 C2 1.401(5) . ? C1 C8 1.475(5) . ? C2 C3 1.431(5) . ? C2 C6 1.475(5) . ? C3 C4 1.383(5) . ? C4 C5 1.405(5) . ? C4 C22 1.519(5) . ? C5 C6 1.400(5) . ? C6 C7 1.410(5) . ? C7 C15 1.477(5) . ? C8 C9 1.374(5) . ? C8 C13 1.400(5) . ? C9 C10 1.369(5) . ? C10 C11 1.384(5) . ? C10 C14 1.423(5) . ? C11 C12 1.368(5) . ? C12 C13 1.375(5) . ? C15 C20 1.379(5) . ? C15 C16 1.390(5) . ? C16 C17 1.386(5) . ? C17 C18 1.376(5) . ? C17 C21 1.443(6) . ? C18 C19 1.383(6) . ? C19 C20 1.364(6) . ? C22 C23 1.523(6) . ? C22 C30 1.539(5) . ? C22 C29 1.543(5) . ? C23 C28 1.381(5) . ? C23 C24 1.393(5) . ? C24 C25 1.375(6) . ? C25 C26 1.362(6) . ? C26 C27 1.365(6) . ? C27 C28 1.380(6) . ? C30 C31 1.497(6) . ? C32 C34 1.343(8) 2_666 ? C32 C33 1.361(8) . ? C33 C34 1.381(9) . ? C34 C32 1.343(8) 2_666 ? 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 N1 Ag1 N1 180.000(1) . 2_757 ? N1 Ag1 N2 86.79(14) . 2_656 ? N1 Ag1 N2 93.21(14) 2_757 2_656 ? N1 Ag1 N2 93.21(14) . 1_656 ? N1 Ag1 N2 86.79(14) 2_757 1_656 ? N2 Ag1 N2 180.00(18) 2_656 1_656 ? C14 N1 Ag1 159.0(4) . . ? C21 N2 Ag1 127.1(4) . 1_454 ? F1 P1 F1 180.0 . 2_565 ? F1 P1 F2 89.2(2) . 2_565 ? F1 P1 F2 90.8(2) 2_565 2_565 ? F1 P1 F2 90.8(2) . . ? F1 P1 F2 89.2(2) 2_565 . ? F2 P1 F2 180.0(3) 2_565 . ? F1 P1 F3 88.00(17) . 2_565 ? F1 P1 F3 92.00(17) 2_565 2_565 ? F2 P1 F3 92.0(2) 2_565 2_565 ? F2 P1 F3 88.0(2) . 2_565 ? F1 P1 F3 92.00(17) . . ? F1 P1 F3 88.00(17) 2_565 . ? F2 P1 F3 88.0(2) 2_565 . ? F2 P1 F3 92.0(2) . . ? F3 P1 F3 180.0(3) 2_565 . ? O1 C1 C2 123.5(4) . . ? O1 C1 C8 112.9(4) . . ? C2 C1 C8 123.6(4) . . ? C1 C2 C3 123.3(4) . . ? C1 C2 C6 129.9(4) . . ? C3 C2 C6 106.7(3) . . ? C4 C3 C2 109.5(4) . . ? C3 C4 C5 107.4(3) . . ? C3 C4 C22 127.6(4) . . ? C5 C4 C22 124.8(4) . . ? C6 C5 C4 111.4(4) . . ? C5 C6 C7 126.8(4) . . ? C5 C6 C2 105.0(3) . . ? C7 C6 C2 128.0(4) . . ? O2 C7 C6 122.1(4) . . ? O2 C7 C15 116.1(4) . . ? C6 C7 C15 121.8(4) . . ? C9 C8 C13 118.7(4) . . ? C9 C8 C1 119.0(4) . . ? C13 C8 C1 122.1(4) . . ? C10 C9 C8 120.3(4) . . ? C9 C10 C11 120.9(4) . . ? C9 C10 C14 120.1(4) . . ? C11 C10 C14 118.8(4) . . ? C12 C11 C10 119.2(4) . . ? C11 C12 C13 120.4(4) . . ? C12 C13 C8 120.4(4) . . ? N1 C14 C10 177.1(5) . . ? C20 C15 C16 118.4(4) . . ? C20 C15 C7 119.6(4) . . ? C16 C15 C7 121.8(4) . . ? C17 C16 C15 119.3(4) . . ? C18 C17 C16 121.4(4) . . ? C18 C17 C21 119.5(4) . . ? C16 C17 C21 119.1(5) . . ? C17 C18 C19 119.0(4) . . ? C20 C19 C18 119.7(5) . . ? C19 C20 C15 122.2(4) . . ? N2 C21 C17 178.2(5) . . ? C4 C22 C23 108.0(3) . . ? C4 C22 C30 109.6(3) . . ? C23 C22 C30 109.9(4) . . ? C4 C22 C29 106.9(3) . . ? C23 C22 C29 112.2(3) . . ? C30 C22 C29 110.1(3) . . ? C28 C23 C24 116.7(4) . . ? C28 C23 C22 123.6(4) . . ? C24 C23 C22 119.8(4) . . ? C25 C24 C23 122.4(4) . . ? C26 C25 C24 119.4(4) . . ? C25 C26 C27 119.6(5) . . ? C26 C27 C28 121.1(5) . . ? C27 C28 C23 120.8(4) . . ? C31 C30 C22 113.1(4) . . ? C34 C32 C33 119.2(6) 2_666 . ? C32 C33 C34 121.0(6) . . ? C32 C34 C33 119.8(6) 2_666 . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.435 _refine_diff_density_min -0.422 _refine_diff_density_rms 0.047 data_4 _database_code_CSD 210652 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H38 Ag0.5 F6 N2 O2 Sb' _chemical_formula_weight 1412.89 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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' _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 8.148(3) _cell_length_b 13.607(4) _cell_length_c 15.390(5) _cell_angle_alpha 108.439(5) _cell_angle_beta 94.268(6) _cell_angle_gamma 94.948(6) _cell_volume 1603.3(9) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 869 _cell_measurement_theta_min 2.524 _cell_measurement_theta_max 16.462 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 460.5 _exptl_absorpt_coefficient_mu 0.620 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7830 _exptl_absorpt_correction_T_max 0.9442 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8529 _diffrn_reflns_av_R_equivalents 0.0550 _diffrn_reflns_av_sigmaI/netI 0.1916 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5603 _reflns_number_gt 1792 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0894P)^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 5603 _refine_ls_number_parameters 409 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1958 _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.2012 _refine_ls_wR_factor_gt 0.1375 _refine_ls_goodness_of_fit_ref 0.789 _refine_ls_restrained_S_all 0.804 _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 Sb1 Sb 0.5000 0.5000 0.5000 0.1191(6) Uani 1 2 d SD . . Ag1 Ag 1.5000 1.0000 0.5000 0.1323(7) Uani 1 2 d S . . F1 F 0.7006(10) 0.5276(7) 0.5599(8) 0.275(6) Uani 1 1 d D . . F2 F 0.4777(13) 0.3647(6) 0.5035(7) 0.254(6) Uani 1 1 d D . . F3 F 0.5798(17) 0.4509(10) 0.3903(6) 0.313(7) Uani 1 1 d D . . N1 N 1.2123(10) 1.0616(6) 0.5364(5) 0.081(2) Uani 1 1 d . . . N2 N 0.5103(10) 0.9289(6) -0.3905(5) 0.083(3) Uani 1 1 d . . . O1 O 0.8214(8) 1.1694(4) 0.1647(3) 0.0769(19) Uani 1 1 d . . . O2 O 0.7783(8) 1.0694(4) 0.0001(3) 0.0777(19) Uani 1 1 d . . . H2 H 0.7888 1.1063 0.0543 0.116 Uiso 1 1 calc R . . C1 C 0.8232(10) 1.1071(7) 0.2096(5) 0.051(2) Uani 1 1 d . . . C2 C 0.7679(10) 0.9985(6) 0.1698(5) 0.049(2) Uani 1 1 d . . . C3 C 0.7259(9) 0.9295(6) 0.2170(5) 0.047(2) Uani 1 1 d . . . H3 H 0.7385 0.9463 0.2807 0.056 Uiso 1 1 calc R . . C4 C 0.6613(9) 0.8305(6) 0.1546(5) 0.0442(19) Uani 1 1 d . . . C5 C 0.6669(9) 0.8363(6) 0.0675(5) 0.050(2) Uani 1 1 d . . . H5 H 0.6341 0.7812 0.0134 0.060 Uiso 1 1 calc R . . C6 C 0.7301(9) 0.9388(6) 0.0717(5) 0.047(2) Uani 1 1 d . . . C7 C 0.7447(10) 0.9718(7) -0.0052(5) 0.055(2) Uani 1 1 d . . . C8 C 0.8816(10) 1.1549(6) 0.3087(5) 0.050(2) Uani 1 1 d . . . C9 C 0.9774(9) 1.1043(6) 0.3571(5) 0.053(2) Uani 1 1 d . . . H9 H 0.9978 1.0360 0.3283 0.063 Uiso 1 1 calc R . . C10 C 1.0410(10) 1.1552(7) 0.4468(5) 0.053(2) Uani 1 1 d . . . C11 C 1.0185(12) 1.2589(7) 0.4901(6) 0.076(3) Uani 1 1 d . . . H11 H 1.0665 1.2942 0.5499 0.091 Uiso 1 1 calc R . . C12 C 0.9249(13) 1.3075(7) 0.4431(6) 0.080(3) Uani 1 1 d . . . H12 H 0.9053 1.3760 0.4719 0.096 Uiso 1 1 calc R . . C13 C 0.8595(11) 1.2569(7) 0.3541(6) 0.068(3) Uani 1 1 d . . . H13 H 0.7980 1.2925 0.3231 0.081 Uiso 1 1 calc R . . C14 C 1.1390(11) 1.1032(7) 0.4964(5) 0.061(2) Uani 1 1 d . . . C15 C 0.7254(10) 0.8995(7) -0.1009(5) 0.055(2) Uani 1 1 d . . . C16 C 0.6485(9) 0.9315(6) -0.1691(5) 0.051(2) Uani 1 1 d . . . H16 H 0.6077 0.9959 -0.1537 0.062 Uiso 1 1 calc R . . C17 C 0.6326(10) 0.8678(6) -0.2598(5) 0.051(2) Uani 1 1 d . . . C18 C 0.6933(11) 0.7709(7) -0.2837(5) 0.067(3) Uani 1 1 d . . . H18 H 0.6805 0.7274 -0.3446 0.080 Uiso 1 1 calc R . . C19 C 0.7726(12) 0.7408(7) -0.2154(6) 0.075(3) Uani 1 1 d . . . H19 H 0.8159 0.6772 -0.2306 0.089 Uiso 1 1 calc R . . C20 C 0.7879(11) 0.8041(7) -0.1254(6) 0.067(3) Uani 1 1 d . . . H20 H 0.8410 0.7827 -0.0800 0.080 Uiso 1 1 calc R . . C21 C 0.5606(11) 0.9020(6) -0.3328(6) 0.059(2) Uani 1 1 d . . . C22 C 0.5976(10) 0.7372(6) 0.1818(5) 0.052(2) Uani 1 1 d . . . C23 C 0.4498(10) 0.7693(6) 0.2364(5) 0.052(2) Uani 1 1 d . . . C24 C 0.3208(11) 0.8041(6) 0.1958(6) 0.063(2) Uani 1 1 d . . . H24 H 0.3263 0.8078 0.1368 0.076 Uiso 1 1 calc R . . C25 C 0.1834(12) 0.8337(7) 0.2405(8) 0.083(3) Uani 1 1 d . . . H25 H 0.0974 0.8566 0.2115 0.099 Uiso 1 1 calc R . . C26 C 0.1744(14) 0.8294(8) 0.3262(9) 0.094(3) Uani 1 1 d . . . H26 H 0.0814 0.8486 0.3562 0.112 Uiso 1 1 calc R . . C27 C 0.3018(17) 0.7969(9) 0.3692(7) 0.096(4) Uani 1 1 d . . . H27 H 0.2971 0.7968 0.4294 0.116 Uiso 1 1 calc R . . C28 C 0.4373(12) 0.7642(7) 0.3238(6) 0.068(3) Uani 1 1 d . . . H28 H 0.5204 0.7385 0.3522 0.081 Uiso 1 1 calc R . . C29 C 0.7365(11) 0.7109(7) 0.2401(6) 0.077(3) Uani 1 1 d . . . H29A H 0.6971 0.6520 0.2575 0.115 Uiso 1 1 calc R . . H29B H 0.7707 0.7697 0.2945 0.115 Uiso 1 1 calc R . . H29C H 0.8289 0.6944 0.2050 0.115 Uiso 1 1 calc R . . C30 C 0.5417(11) 0.6407(6) 0.0971(5) 0.073(3) Uani 1 1 d . . . H30A H 0.5025 0.5834 0.1167 0.109 Uiso 1 1 calc R . . H30B H 0.6336 0.6226 0.0619 0.109 Uiso 1 1 calc R . . H30C H 0.4542 0.6557 0.0596 0.109 Uiso 1 1 calc R . . C31 C 0.167(2) 0.5805(16) 0.835(2) 0.210(16) Uani 1 1 d D . . C32 C 0.084(4) 0.594(2) 0.9123(18) 0.28(2) Uani 1 1 d D . . H32 H 0.1408 0.6352 0.9684 0.337 Uiso 1 1 calc R . . C33 C -0.073(4) 0.553(4) 0.9145(18) 0.33(3) Uani 1 1 d D . . H33 H -0.1258 0.5638 0.9679 0.401 Uiso 1 1 calc R . . C34 C -0.145(3) 0.495(2) 0.828(2) 0.27(2) Uani 1 1 d D . . H34 H -0.2532 0.4632 0.8217 0.323 Uiso 1 1 calc R . . C35 C -0.067(3) 0.4797(11) 0.7509(15) 0.196(12) Uani 1 1 d D . . H35 H -0.1254 0.4387 0.6951 0.235 Uiso 1 1 calc R . . C36 C 0.083(3) 0.5185(14) 0.7494(13) 0.154(6) Uani 1 1 d D . . H36 H 0.1330 0.5060 0.6950 0.185 Uiso 1 1 calc R . . C37 C 0.313(4) 0.6111(18) 0.8361(17) 0.316(17) Uani 1 1 d . . . H37A H 0.3451 0.5873 0.7748 0.474 Uiso 1 1 calc R . . H37B H 0.3797 0.5840 0.8753 0.474 Uiso 1 1 calc R . . H37C H 0.3290 0.6859 0.8592 0.474 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 Sb1 0.0946(10) 0.1052(11) 0.1178(10) -0.0182(7) -0.0203(8) 0.0325(8) Ag1 0.1012(11) 0.2409(18) 0.1278(11) 0.1393(12) 0.0406(8) 0.0848(11) F1 0.135(8) 0.161(8) 0.398(14) -0.065(9) -0.111(9) 0.032(6) F2 0.311(14) 0.126(7) 0.293(12) 0.064(7) -0.119(10) 0.003(8) F3 0.349(17) 0.338(16) 0.186(9) -0.024(10) 0.110(10) 0.034(13) N1 0.078(6) 0.102(7) 0.058(5) 0.017(4) -0.001(4) 0.026(5) N2 0.115(7) 0.091(6) 0.056(5) 0.034(4) 0.005(5) 0.037(5) O1 0.123(6) 0.048(4) 0.060(4) 0.026(3) -0.012(3) -0.005(4) O2 0.128(6) 0.052(4) 0.052(3) 0.022(3) -0.003(3) -0.004(4) C1 0.050(5) 0.052(6) 0.051(5) 0.020(5) -0.002(4) 0.002(5) C2 0.055(6) 0.048(5) 0.042(5) 0.012(4) -0.009(4) 0.007(5) C3 0.049(5) 0.053(5) 0.039(5) 0.017(4) -0.003(4) 0.009(4) C4 0.046(5) 0.050(5) 0.041(5) 0.017(4) 0.008(4) 0.015(4) C5 0.046(5) 0.050(6) 0.050(5) 0.013(4) 0.000(4) 0.008(5) C6 0.048(5) 0.053(5) 0.044(5) 0.021(4) -0.001(4) 0.007(4) C7 0.057(6) 0.059(6) 0.049(5) 0.024(5) -0.008(4) 0.004(5) C8 0.053(6) 0.049(5) 0.045(5) 0.013(4) -0.001(4) 0.004(4) C9 0.055(6) 0.054(5) 0.042(5) 0.008(4) 0.001(4) 0.008(5) C10 0.053(6) 0.054(6) 0.046(5) 0.011(5) 0.000(4) -0.001(5) C11 0.092(8) 0.077(7) 0.050(5) 0.011(5) -0.014(5) 0.011(6) C12 0.121(9) 0.051(6) 0.055(6) -0.001(5) 0.003(6) 0.024(6) C13 0.090(7) 0.055(6) 0.055(6) 0.015(5) -0.006(5) 0.007(5) C14 0.063(7) 0.072(7) 0.039(5) 0.009(5) -0.003(5) 0.011(5) C15 0.063(6) 0.067(6) 0.036(5) 0.019(4) 0.002(4) 0.012(5) C16 0.066(6) 0.051(5) 0.042(5) 0.020(4) 0.003(4) 0.013(5) C17 0.057(6) 0.058(6) 0.040(5) 0.022(4) -0.005(4) 0.005(5) C18 0.095(8) 0.057(6) 0.046(5) 0.011(4) 0.015(5) 0.016(6) C19 0.104(8) 0.070(6) 0.058(6) 0.022(5) 0.016(5) 0.042(6) C20 0.081(7) 0.066(6) 0.066(6) 0.034(5) 0.013(5) 0.030(6) C21 0.070(7) 0.057(6) 0.049(5) 0.014(4) 0.013(5) 0.011(5) C22 0.050(6) 0.049(5) 0.063(5) 0.027(5) 0.003(4) 0.007(5) C23 0.049(6) 0.046(5) 0.057(6) 0.016(4) 0.003(5) -0.001(4) C24 0.055(6) 0.072(6) 0.063(6) 0.023(5) 0.010(5) 0.010(5) C25 0.063(7) 0.080(7) 0.103(9) 0.028(6) 0.005(7) 0.003(6) C26 0.074(9) 0.095(8) 0.094(9) 0.003(7) 0.026(7) 0.000(7) C27 0.108(10) 0.104(9) 0.057(7) 0.005(6) 0.018(7) -0.026(8) C28 0.061(6) 0.087(7) 0.056(6) 0.028(5) 0.001(5) 0.002(6) C29 0.080(7) 0.068(6) 0.093(7) 0.039(5) 0.005(6) 0.015(6) C30 0.090(7) 0.050(6) 0.075(6) 0.014(5) 0.018(5) 0.005(5) C31 0.104(15) 0.101(16) 0.44(4) 0.15(2) -0.11(3) -0.037(13) C32 0.40(5) 0.35(4) 0.24(2) 0.23(3) 0.14(3) 0.26(4) C33 0.33(5) 0.40(6) 0.43(5) 0.30(5) 0.10(4) 0.18(5) C34 0.21(3) 0.25(3) 0.49(5) 0.26(4) 0.19(4) 0.10(2) C35 0.106(14) 0.055(9) 0.40(3) 0.067(14) -0.086(19) -0.009(11) C36 0.147(17) 0.074(12) 0.25(2) 0.069(13) -0.028(15) 0.036(11) C37 0.50(5) 0.16(2) 0.29(3) 0.11(2) -0.11(3) 0.08(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sb1 F1 1.764(7) . ? Sb1 F1 1.764(7) 2_666 ? Sb1 F3 1.801(8) 2_666 ? Sb1 F3 1.801(8) . ? Sb1 F2 1.853(7) 2_666 ? Sb1 F2 1.853(7) . ? Ag1 N2 2.192(7) 1_656 ? Ag1 N2 2.192(7) 2_775 ? Ag1 N1 2.597(8) . ? Ag1 N1 2.597(8) 2_876 ? N1 C14 1.131(9) . ? N2 C21 1.127(9) . ? N2 Ag1 2.192(7) 1_454 ? O1 C1 1.252(8) . ? O2 C7 1.308(8) . ? C1 C2 1.426(10) . ? C1 C8 1.479(10) . ? C2 C3 1.392(9) . ? C2 C6 1.465(9) . ? C3 C4 1.413(10) . ? C4 C5 1.371(9) . ? C4 C22 1.521(10) . ? C5 C6 1.425(10) . ? C6 C7 1.402(9) . ? C7 C15 1.478(10) . ? C8 C13 1.376(10) . ? C8 C9 1.404(9) . ? C9 C10 1.370(10) . ? C10 C11 1.391(10) . ? C10 C14 1.440(11) . ? C11 C12 1.360(10) . ? C12 C13 1.367(11) . ? C15 C20 1.386(10) . ? C15 C16 1.386(9) . ? C16 C17 1.381(9) . ? C17 C18 1.397(10) . ? C17 C21 1.449(11) . ? C18 C19 1.381(10) . ? C19 C20 1.371(10) . ? C22 C29 1.529(10) . ? C22 C30 1.535(10) . ? C22 C23 1.535(10) . ? C23 C24 1.376(10) . ? C23 C28 1.380(10) . ? C24 C25 1.380(12) . ? C25 C26 1.346(12) . ? C26 C27 1.369(13) . ? C27 C28 1.381(13) . ? C31 C37 1.22(3) . ? C31 C32 1.387(17) . ? C31 C36 1.404(16) . ? C32 C33 1.356(19) . ? C33 C34 1.375(18) . ? C34 C35 1.353(16) . ? C35 C36 1.297(14) . ? 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 F1 Sb1 F1 180.000(1) . 2_666 ? F1 Sb1 F3 87.9(5) . 2_666 ? F1 Sb1 F3 92.1(5) 2_666 2_666 ? F1 Sb1 F3 92.1(5) . . ? F1 Sb1 F3 87.9(5) 2_666 . ? F3 Sb1 F3 180.0(3) 2_666 . ? F1 Sb1 F2 87.6(4) . 2_666 ? F1 Sb1 F2 92.4(4) 2_666 2_666 ? F3 Sb1 F2 88.0(5) 2_666 2_666 ? F3 Sb1 F2 92.0(5) . 2_666 ? F1 Sb1 F2 92.4(4) . . ? F1 Sb1 F2 87.6(4) 2_666 . ? F3 Sb1 F2 92.0(5) 2_666 . ? F3 Sb1 F2 88.0(5) . . ? F2 Sb1 F2 180.000(2) 2_666 . ? N2 Ag1 N2 180.000(2) 1_656 2_775 ? N2 Ag1 N1 92.5(3) 1_656 . ? N2 Ag1 N1 87.5(3) 2_775 . ? N2 Ag1 N1 87.5(3) 1_656 2_876 ? N2 Ag1 N1 92.5(3) 2_775 2_876 ? N1 Ag1 N1 180.0(3) . 2_876 ? C14 N1 Ag1 124.6(7) . . ? C21 N2 Ag1 160.8(8) . 1_454 ? O1 C1 C2 123.1(7) . . ? O1 C1 C8 115.1(7) . . ? C2 C1 C8 121.8(7) . . ? C3 C2 C1 126.6(7) . . ? C3 C2 C6 105.9(7) . . ? C1 C2 C6 127.3(7) . . ? C2 C3 C4 110.7(6) . . ? C5 C4 C3 107.0(7) . . ? C5 C4 C22 127.8(7) . . ? C3 C4 C22 125.2(7) . . ? C4 C5 C6 110.3(7) . . ? C7 C6 C5 124.6(7) . . ? C7 C6 C2 129.4(8) . . ? C5 C6 C2 106.0(6) . . ? O2 C7 C6 123.6(7) . . ? O2 C7 C15 112.9(6) . . ? C6 C7 C15 123.4(8) . . ? C13 C8 C9 117.3(7) . . ? C13 C8 C1 120.0(7) . . ? C9 C8 C1 122.3(7) . . ? C10 C9 C8 120.2(7) . . ? C9 C10 C11 121.0(8) . . ? C9 C10 C14 120.2(8) . . ? C11 C10 C14 118.8(8) . . ? C12 C11 C10 118.6(8) . . ? C11 C12 C13 120.7(8) . . ? C12 C13 C8 122.1(8) . . ? N1 C14 C10 178.2(10) . . ? C20 C15 C16 119.2(7) . . ? C20 C15 C7 122.7(7) . . ? C16 C15 C7 118.1(7) . . ? C17 C16 C15 120.0(7) . . ? C16 C17 C18 120.5(7) . . ? C16 C17 C21 120.9(7) . . ? C18 C17 C21 118.5(7) . . ? C19 C18 C17 119.0(7) . . ? C20 C19 C18 120.4(8) . . ? C19 C20 C15 121.0(7) . . ? N2 C21 C17 177.5(10) . . ? C4 C22 C29 109.0(7) . . ? C4 C22 C30 111.7(6) . . ? C29 C22 C30 108.3(6) . . ? C4 C22 C23 106.4(6) . . ? C29 C22 C23 111.6(6) . . ? C30 C22 C23 109.8(7) . . ? C24 C23 C28 117.7(8) . . ? C24 C23 C22 118.5(7) . . ? C28 C23 C22 123.8(8) . . ? C23 C24 C25 121.8(8) . . ? C26 C25 C24 119.7(10) . . ? C25 C26 C27 120.1(10) . . ? C26 C27 C28 120.4(9) . . ? C23 C28 C27 120.2(9) . . ? C37 C31 C32 125(3) . . ? C37 C31 C36 117(3) . . ? C32 C31 C36 118(2) . . ? C33 C32 C31 127(3) . . ? C32 C33 C34 111(3) . . ? C35 C34 C33 123.7(19) . . ? C36 C35 C34 124.6(16) . . ? C35 C36 C31 116.0(17) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.462 _refine_diff_density_min -0.563 _refine_diff_density_rms 0.102 data_6 _database_code_CSD 210654 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H27 Mn0.5 N2 O3' _chemical_formula_weight 1030.05 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6786(4) _cell_length_b 10.8010(5) _cell_length_c 14.5929(7) _cell_angle_alpha 99.7260(10) _cell_angle_beta 93.6690(10) _cell_angle_gamma 94.2720(10) _cell_volume 1340.41(11) _cell_formula_units_Z 1 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 8825 _cell_measurement_theta_min 2.360 _cell_measurement_theta_max 26.394 _exptl_crystal_description bar _exptl_crystal_colour orange _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 269.5 _exptl_absorpt_coefficient_mu 0.152 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7546 _exptl_absorpt_correction_T_max 0.9422 _exptl_absorpt_process_details '(SADABS, Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12415 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 26.39 _reflns_number_total 5475 _reflns_number_gt 4368 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART NT V5.625 (Bruker, 1998)' _computing_cell_refinement 'SAINT+ NT V6.22 (Bruker, 2001)' _computing_data_reduction 'SAINT+ NT V6.22' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V6.1 (Sheldrick, 2000)' _computing_publication_material 'SHELXTL V6.1' _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^)+(0.0604P)^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 5475 _refine_ls_number_parameters 366 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0504 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.1067 _refine_ls_wR_factor_gt 0.1036 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.033 _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 Mn Mn 0.0000 0.0000 0.0000 0.02811(12) Uani 1 2 d S . . C1 C 0.26633(19) 0.14994(15) 0.37094(11) 0.0253(4) Uani 1 1 d . . . C2 C 0.15686(19) 0.21068(15) 0.32554(11) 0.0256(4) Uani 1 1 d . . . H2 H 0.1332 0.2950 0.3456 0.031 Uiso 1 1 calc R . . C3 C 0.08528(19) 0.12941(15) 0.24509(11) 0.0248(3) Uani 1 1 d . . . C4 C 0.15470(19) 0.01035(15) 0.24251(11) 0.0250(4) Uani 1 1 d . A . C5 C 0.26189(19) 0.02633(15) 0.32075(11) 0.0264(4) Uani 1 1 d . . . H5 H 0.3227 -0.0372 0.3374 0.032 Uiso 1 1 calc R . . C6 C -0.0364(2) 0.16353(15) 0.18752(11) 0.0258(4) Uani 1 1 d . . . C7 C -0.0988(2) 0.28957(15) 0.21253(12) 0.0277(4) Uani 1 1 d . . . C8 C -0.1589(2) 0.32734(18) 0.29777(13) 0.0368(4) Uani 1 1 d . . . H8 H -0.1556 0.2748 0.3438 0.044 Uiso 1 1 calc R . . C9 C -0.2237(3) 0.4414(2) 0.31585(15) 0.0499(6) Uani 1 1 d . . . H9 H -0.2663 0.4660 0.3739 0.060 Uiso 1 1 calc R . . C10 C -0.2269(3) 0.51958(19) 0.25055(16) 0.0510(6) Uani 1 1 d . . . H10 H -0.2703 0.5983 0.2635 0.061 Uiso 1 1 calc R . . C11 C -0.1660(2) 0.48190(17) 0.16536(14) 0.0408(5) Uani 1 1 d . . . C12 C -0.1048(2) 0.36618(16) 0.14531(12) 0.0318(4) Uani 1 1 d . . . H12 H -0.0673 0.3396 0.0860 0.038 Uiso 1 1 calc R . . C13 C -0.1653(3) 0.56589(19) 0.09788(17) 0.0548(6) Uani 1 1 d . . . C14 C 0.1383(2) -0.10293(15) 0.17460(11) 0.0269(4) Uani 1 1 d . . . C15 C 0.1843(2) -0.22337(15) 0.20298(12) 0.0294(4) Uani 0.671(3) 1 d P A 1 C16 C 0.2591(2) -0.30561(17) 0.14078(14) 0.0399(5) Uani 0.671(3) 1 d P A 1 H16 H 0.2838 -0.2836 0.0828 0.048 Uiso 0.671(3) 1 calc PR A 1 C17 C 0.2984(3) -0.42048(19) 0.16290(17) 0.0544(6) Uani 0.671(3) 1 d P A 1 H17 H 0.3529 -0.4753 0.1211 0.065 Uiso 0.671(3) 1 calc PR A 1 C18 C 0.2578(3) -0.45436(19) 0.24599(18) 0.0562(7) Uani 0.671(3) 1 d P A 1 H18 H 0.2833 -0.5330 0.2609 0.067 Uiso 0.671(3) 1 calc PR A 1 C19 C 0.1802(2) -0.37387(19) 0.30727(15) 0.0462(5) Uani 0.671(3) 1 d P A 1 C20 C 0.1444(2) -0.25741(17) 0.28625(13) 0.0362(4) Uani 0.671(3) 1 d P A 1 H20 H 0.0928 -0.2016 0.3290 0.043 Uiso 0.671(3) 1 calc PR A 1 C21 C 0.1319(4) -0.3962(3) 0.4012(2) 0.0527(10) Uani 0.671(3) 1 d P A 1 N2 N 0.0985(5) -0.4148(3) 0.4722(2) 0.0897(14) Uani 0.671(3) 1 d P A 1 C15A C 0.1843(2) -0.22337(15) 0.20298(12) 0.0294(4) Uani 0.329(3) 1 d P A 2 C16A C 0.2591(2) -0.30561(17) 0.14078(14) 0.0399(5) Uani 0.329(3) 1 d P A 2 H16A H 0.2838 -0.2836 0.0828 0.048 Uiso 0.329(3) 1 calc PR A 2 C17A C 0.2984(3) -0.42048(19) 0.16290(17) 0.0544(6) Uani 0.329(3) 1 d PD A 2 C18A C 0.2578(3) -0.45436(19) 0.24599(18) 0.0562(7) Uani 0.329(3) 1 d P A 2 H18A H 0.2833 -0.5330 0.2609 0.067 Uiso 0.329(3) 1 calc PR A 2 C19A C 0.1802(2) -0.37387(19) 0.30727(15) 0.0462(5) Uani 0.329(3) 1 d P A 2 H19A H 0.1511 -0.3979 0.3639 0.055 Uiso 0.329(3) 1 calc PR A 2 C20A C 0.1444(2) -0.25741(17) 0.28625(13) 0.0362(4) Uani 0.329(3) 1 d P A 2 H20A H 0.0928 -0.2016 0.3290 0.043 Uiso 0.329(3) 1 calc PR A 2 C21A C 0.4153(7) -0.4807(5) 0.0921(4) 0.0458(17) Uani 0.329(3) 1 d PD A 2 N2A N 0.4946(7) -0.5339(5) 0.0395(4) 0.0595(18) Uani 0.329(3) 1 d PD . 2 C22 C 0.37565(19) 0.20588(15) 0.45589(12) 0.0271(4) Uani 1 1 d . . . C23 C 0.32760(19) 0.16084(15) 0.54531(11) 0.0262(4) Uani 1 1 d . . . C24 C 0.4184(2) 0.20034(16) 0.62917(12) 0.0323(4) Uani 1 1 d . . . H24 H 0.5090 0.2558 0.6303 0.039 Uiso 1 1 calc R . . C25 C 0.3796(2) 0.16074(17) 0.71055(12) 0.0356(4) Uani 1 1 d . . . H25 H 0.4434 0.1894 0.7666 0.043 Uiso 1 1 calc R . . C26 C 0.2491(2) 0.07984(18) 0.71100(12) 0.0352(4) Uani 1 1 d . . . H26 H 0.2222 0.0525 0.7669 0.042 Uiso 1 1 calc R . . C27 C 0.1583(2) 0.03938(18) 0.62863(12) 0.0359(4) Uani 1 1 d . . . H27 H 0.0684 -0.0167 0.6278 0.043 Uiso 1 1 calc R . . C28 C 0.1970(2) 0.07961(17) 0.54730(12) 0.0306(4) Uani 1 1 d . . . H28 H 0.1326 0.0509 0.4915 0.037 Uiso 1 1 calc R . . C29 C 0.5395(2) 0.16771(18) 0.43625(13) 0.0365(4) Uani 1 1 d . . . H29A H 0.5693 0.1947 0.3785 0.055 Uiso 1 1 calc R . . H29B H 0.5400 0.0759 0.4295 0.055 Uiso 1 1 calc R . . H29C H 0.6133 0.2083 0.4882 0.055 Uiso 1 1 calc R . . C30 C 0.3792(2) 0.35068(16) 0.47148(14) 0.0394(5) Uani 1 1 d . . . H30A H 0.2762 0.3763 0.4858 0.059 Uiso 1 1 calc R . . H30B H 0.4090 0.3809 0.4149 0.059 Uiso 1 1 calc R . . H30C H 0.4547 0.3870 0.5237 0.059 Uiso 1 1 calc R . . C31 C 0.3614(3) 0.1184(2) 0.03405(19) 0.0585(6) Uani 1 1 d . . . H31A H 0.4068 0.1358 -0.0235 0.070 Uiso 1 1 calc R . . H31B H 0.3678 0.0278 0.0362 0.070 Uiso 1 1 calc R . . C32 C 0.4531(3) 0.1928(4) 0.1146(2) 0.1013(11) Uani 1 1 d . . . H32A H 0.4001 0.1868 0.1712 0.152 Uiso 1 1 calc R . . H32B H 0.4657 0.2812 0.1065 0.152 Uiso 1 1 calc R . . H32C H 0.5553 0.1605 0.1202 0.152 Uiso 1 1 calc R . . N1 N -0.1658(3) 0.63309(19) 0.04547(17) 0.0783(7) Uani 1 1 d . . . O1 O -0.10046(14) 0.09710(11) 0.11377(8) 0.0307(3) Uani 1 1 d . . . O2 O 0.09191(16) -0.11302(11) 0.09048(8) 0.0349(3) Uani 1 1 d . A . O3 O 0.20151(15) 0.14359(12) 0.02928(9) 0.0364(3) Uani 1 1 d D . . H3 H 0.199(3) 0.214(2) 0.0033(18) 0.085(9) Uiso 1 1 d 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 Mn 0.0394(2) 0.0223(2) 0.0230(2) 0.00350(14) 0.00124(16) 0.00697(16) C1 0.0275(9) 0.0224(8) 0.0269(8) 0.0055(7) 0.0047(7) 0.0026(7) C2 0.0304(9) 0.0201(8) 0.0273(8) 0.0043(6) 0.0067(7) 0.0049(7) C3 0.0318(9) 0.0211(8) 0.0230(8) 0.0059(6) 0.0056(7) 0.0054(7) C4 0.0303(9) 0.0212(8) 0.0252(8) 0.0063(6) 0.0054(7) 0.0048(7) C5 0.0287(9) 0.0218(8) 0.0301(9) 0.0065(7) 0.0043(7) 0.0057(7) C6 0.0313(9) 0.0242(8) 0.0237(8) 0.0060(7) 0.0082(7) 0.0050(7) C7 0.0284(9) 0.0257(9) 0.0285(9) 0.0028(7) 0.0000(7) 0.0053(7) C8 0.0405(11) 0.0401(11) 0.0311(9) 0.0042(8) 0.0037(8) 0.0148(9) C9 0.0537(13) 0.0563(13) 0.0384(11) -0.0053(10) 0.0032(10) 0.0279(11) C10 0.0591(14) 0.0347(11) 0.0551(13) -0.0073(10) -0.0116(11) 0.0251(10) C11 0.0464(12) 0.0265(9) 0.0477(12) 0.0057(8) -0.0111(9) 0.0067(8) C12 0.0359(10) 0.0268(9) 0.0323(9) 0.0046(7) -0.0016(8) 0.0052(7) C13 0.0694(16) 0.0283(11) 0.0651(15) 0.0101(10) -0.0151(12) 0.0068(10) C14 0.0310(9) 0.0235(8) 0.0275(9) 0.0058(7) 0.0034(7) 0.0061(7) C15 0.0329(9) 0.0209(8) 0.0331(9) 0.0039(7) -0.0056(7) 0.0025(7) C16 0.0498(12) 0.0285(9) 0.0390(10) -0.0012(8) -0.0058(9) 0.0126(9) C17 0.0685(15) 0.0297(10) 0.0595(14) -0.0060(10) -0.0202(12) 0.0206(10) C18 0.0703(16) 0.0218(10) 0.0723(16) 0.0122(10) -0.0346(13) 0.0012(10) C19 0.0498(12) 0.0368(11) 0.0518(12) 0.0211(10) -0.0197(10) -0.0079(9) C20 0.0379(11) 0.0325(10) 0.0374(10) 0.0102(8) -0.0092(8) -0.0008(8) C21 0.076(2) 0.0337(17) 0.048(2) 0.0145(14) -0.0167(17) 0.0046(16) N2 0.158(4) 0.078(2) 0.0425(18) 0.0320(17) -0.002(2) 0.026(2) C15A 0.0329(9) 0.0209(8) 0.0331(9) 0.0039(7) -0.0056(7) 0.0025(7) C16A 0.0498(12) 0.0285(9) 0.0390(10) -0.0012(8) -0.0058(9) 0.0126(9) C17A 0.0685(15) 0.0297(10) 0.0595(14) -0.0060(10) -0.0202(12) 0.0206(10) C18A 0.0703(16) 0.0218(10) 0.0723(16) 0.0122(10) -0.0346(13) 0.0012(10) C19A 0.0498(12) 0.0368(11) 0.0518(12) 0.0211(10) -0.0197(10) -0.0079(9) C20A 0.0379(11) 0.0325(10) 0.0374(10) 0.0102(8) -0.0092(8) -0.0008(8) C21A 0.042(4) 0.029(3) 0.062(4) -0.002(3) -0.010(3) 0.009(3) N2A 0.050(4) 0.047(4) 0.077(4) -0.005(3) -0.002(3) 0.010(3) C22 0.0278(9) 0.0217(8) 0.0314(9) 0.0039(7) 0.0013(7) 0.0011(7) C23 0.0265(9) 0.0222(8) 0.0296(9) 0.0011(7) 0.0016(7) 0.0078(7) C24 0.0308(9) 0.0276(9) 0.0362(10) 0.0006(7) -0.0020(8) 0.0025(7) C25 0.0398(11) 0.0364(10) 0.0281(9) -0.0007(8) -0.0054(8) 0.0084(8) C26 0.0369(10) 0.0424(11) 0.0274(9) 0.0060(8) 0.0033(8) 0.0093(9) C27 0.0290(10) 0.0465(11) 0.0326(10) 0.0093(8) 0.0021(8) 0.0005(8) C28 0.0261(9) 0.0368(10) 0.0278(9) 0.0042(7) -0.0021(7) 0.0023(7) C29 0.0287(10) 0.0397(10) 0.0402(10) 0.0057(8) 0.0031(8) -0.0011(8) C30 0.0506(12) 0.0232(9) 0.0420(11) 0.0048(8) -0.0065(9) -0.0016(8) C31 0.0434(13) 0.0478(13) 0.0856(18) 0.0129(12) 0.0048(12) 0.0094(10) C32 0.0514(17) 0.146(3) 0.099(2) 0.014(2) -0.0136(17) -0.0033(19) N1 0.114(2) 0.0373(11) 0.0855(16) 0.0270(11) -0.0192(14) 0.0080(12) O1 0.0378(7) 0.0285(6) 0.0254(6) 0.0010(5) 0.0009(5) 0.0092(5) O2 0.0547(8) 0.0239(6) 0.0265(6) 0.0031(5) 0.0007(6) 0.0116(6) O3 0.0395(7) 0.0288(7) 0.0423(7) 0.0096(6) 0.0018(6) 0.0051(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 Mn O1 2.0856(11) 2 ? Mn O1 2.0856(11) . ? Mn O2 2.1035(12) . ? Mn O2 2.1035(12) 2 ? Mn O3 2.2187(13) 2 ? Mn O3 2.2187(13) . ? C1 C2 1.390(2) . ? C1 C5 1.407(2) . ? C1 C22 1.521(2) . ? C2 C3 1.418(2) . ? C3 C6 1.416(2) . ? C3 C4 1.456(2) . ? C4 C5 1.404(2) . ? C4 C14 1.430(2) . ? C6 O1 1.2591(19) . ? C6 C7 1.499(2) . ? C7 C12 1.387(2) . ? C7 C8 1.389(2) . ? C8 C9 1.384(3) . ? C9 C10 1.376(3) . ? C10 C11 1.391(3) . ? C11 C12 1.388(2) . ? C11 C13 1.447(3) . ? C13 N1 1.140(3) . ? C14 O2 1.251(2) . ? C14 C15 1.504(2) . ? C15 C20 1.385(3) . ? C15 C16 1.387(3) . ? C16 C17 1.394(3) . ? C17 C18 1.383(4) . ? C18 C19 1.382(3) . ? C19 C20 1.396(3) . ? C19 C21 1.511(4) . ? C21 N2 1.139(5) . ? C21A N2A 1.171(6) . ? N2A N2A 1.470(12) 2_645 ? C22 C23 1.538(2) . ? C22 C30 1.540(2) . ? C22 C29 1.541(2) . ? C23 C28 1.385(2) . ? C23 C24 1.397(2) . ? C24 C25 1.381(3) . ? C25 C26 1.379(3) . ? C26 C27 1.381(2) . ? C27 C28 1.383(2) . ? C31 O3 1.433(3) . ? C31 C32 1.459(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn O1 180.00(9) 2 . ? O1 Mn O2 92.25(5) 2 . ? O1 Mn O2 87.75(5) . . ? O1 Mn O2 87.75(5) 2 2 ? O1 Mn O2 92.25(5) . 2 ? O2 Mn O2 180.00(6) . 2 ? O1 Mn O3 88.73(5) 2 2 ? O1 Mn O3 91.27(5) . 2 ? O2 Mn O3 86.38(5) . 2 ? O2 Mn O3 93.62(5) 2 2 ? O1 Mn O3 91.27(5) 2 . ? O1 Mn O3 88.73(5) . . ? O2 Mn O3 93.62(5) . . ? O2 Mn O3 86.38(5) 2 . ? O3 Mn O3 180.00(9) 2 . ? C2 C1 C5 106.68(15) . . ? C2 C1 C22 127.41(14) . . ? C5 C1 C22 125.86(15) . . ? C1 C2 C3 110.63(14) . . ? C6 C3 C2 123.29(14) . . ? C6 C3 C4 130.76(15) . . ? C2 C3 C4 105.78(14) . . ? C5 C4 C14 121.64(15) . . ? C5 C4 C3 106.60(14) . . ? C14 C4 C3 131.55(15) . . ? C4 C5 C1 110.26(15) . . ? O1 C6 C3 126.01(15) . . ? O1 C6 C7 114.18(14) . . ? C3 C6 C7 119.80(14) . . ? C12 C7 C8 119.78(16) . . ? C12 C7 C6 118.03(15) . . ? C8 C7 C6 122.06(15) . . ? C9 C8 C7 120.14(18) . . ? C10 C9 C8 120.61(19) . . ? C9 C10 C11 119.19(18) . . ? C12 C11 C10 120.79(18) . . ? C12 C11 C13 120.10(19) . . ? C10 C11 C13 119.10(19) . . ? C7 C12 C11 119.45(17) . . ? N1 C13 C11 179.1(3) . . ? O2 C14 C4 126.33(15) . . ? O2 C14 C15 114.60(14) . . ? C4 C14 C15 119.05(14) . . ? C20 C15 C16 119.67(17) . . ? C20 C15 C14 121.63(16) . . ? C16 C15 C14 118.55(16) . . ? C15 C16 C17 120.4(2) . . ? C18 C17 C16 119.7(2) . . ? C19 C18 C17 120.05(18) . . ? C18 C19 C20 120.2(2) . . ? C18 C19 C21 126.1(2) . . ? C20 C19 C21 113.6(2) . . ? C15 C20 C19 119.90(19) . . ? N2 C21 C19 178.3(4) . . ? C21A N2A N2A 108.1(7) . 2_645 ? C1 C22 C23 112.72(13) . . ? C1 C22 C30 109.39(14) . . ? C23 C22 C30 108.46(14) . . ? C1 C22 C29 108.15(14) . . ? C23 C22 C29 109.38(14) . . ? C30 C22 C29 108.67(15) . . ? C28 C23 C24 116.97(16) . . ? C28 C23 C22 122.98(15) . . ? C24 C23 C22 120.05(15) . . ? C25 C24 C23 121.61(17) . . ? C26 C25 C24 120.48(17) . . ? C25 C26 C27 118.69(17) . . ? C26 C27 C28 120.71(17) . . ? C27 C28 C23 121.53(16) . . ? O3 C31 C32 113.6(2) . . ? C6 O1 Mn 129.40(11) . . ? C14 O2 Mn 138.50(11) . . ? C31 O3 Mn 125.90(12) . . ? 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 C5 C1 C2 C3 -1.87(19) . . . . ? C22 C1 C2 C3 175.74(15) . . . . ? C1 C2 C3 C6 176.78(16) . . . . ? C1 C2 C3 C4 0.96(18) . . . . ? C6 C3 C4 C5 -175.06(17) . . . . ? C2 C3 C4 C5 0.33(17) . . . . ? C6 C3 C4 C14 10.2(3) . . . . ? C2 C3 C4 C14 -174.40(17) . . . . ? C14 C4 C5 C1 173.87(15) . . . . ? C3 C4 C5 C1 -1.50(19) . . . . ? C2 C1 C5 C4 2.09(19) . . . . ? C22 C1 C5 C4 -175.57(15) . . . . ? C2 C3 C6 O1 177.44(15) . . . . ? C4 C3 C6 O1 -7.9(3) . . . . ? C2 C3 C6 C7 -2.0(2) . . . . ? C4 C3 C6 C7 172.68(16) . . . . ? O1 C6 C7 C12 -52.7(2) . . . . ? C3 C6 C7 C12 126.79(17) . . . . ? O1 C6 C7 C8 123.12(18) . . . . ? C3 C6 C7 C8 -57.4(2) . . . . ? C12 C7 C8 C9 -0.4(3) . . . . ? C6 C7 C8 C9 -176.19(18) . . . . ? C7 C8 C9 C10 -1.1(3) . . . . ? C8 C9 C10 C11 0.8(3) . . . . ? C9 C10 C11 C12 1.1(3) . . . . ? C9 C10 C11 C13 -178.1(2) . . . . ? C8 C7 C12 C11 2.3(3) . . . . ? C6 C7 C12 C11 178.19(16) . . . . ? C10 C11 C12 C7 -2.6(3) . . . . ? C13 C11 C12 C7 176.61(18) . . . . ? C12 C11 C13 N1 175(100) . . . . ? C10 C11 C13 N1 -6(18) . . . . ? C5 C4 C14 O2 -153.31(18) . . . . ? C3 C4 C14 O2 20.8(3) . . . . ? C5 C4 C14 C15 24.8(2) . . . . ? C3 C4 C14 C15 -161.18(17) . . . . ? O2 C14 C15 C20 -138.04(17) . . . . ? C4 C14 C15 C20 43.7(2) . . . . ? O2 C14 C15 C16 37.5(2) . . . . ? C4 C14 C15 C16 -140.78(17) . . . . ? C20 C15 C16 C17 -1.9(3) . . . . ? C14 C15 C16 C17 -177.54(18) . . . . ? C15 C16 C17 C18 2.2(3) . . . . ? C16 C17 C18 C19 -0.8(3) . . . . ? C17 C18 C19 C20 -0.9(3) . . . . ? C17 C18 C19 C21 -178.4(2) . . . . ? C16 C15 C20 C19 0.2(3) . . . . ? C14 C15 C20 C19 175.72(16) . . . . ? C18 C19 C20 C15 1.2(3) . . . . ? C21 C19 C20 C15 179.0(2) . . . . ? C18 C19 C21 N2 29(14) . . . . ? C20 C19 C21 N2 -149(13) . . . . ? C2 C1 C22 C23 106.21(19) . . . . ? C5 C1 C22 C23 -76.6(2) . . . . ? C2 C1 C22 C30 -14.5(2) . . . . ? C5 C1 C22 C30 162.64(17) . . . . ? C2 C1 C22 C29 -132.74(18) . . . . ? C5 C1 C22 C29 44.4(2) . . . . ? C1 C22 C23 C28 -1.0(2) . . . . ? C30 C22 C23 C28 120.30(18) . . . . ? C29 C22 C23 C28 -121.32(17) . . . . ? C1 C22 C23 C24 178.04(14) . . . . ? C30 C22 C23 C24 -60.7(2) . . . . ? C29 C22 C23 C24 57.7(2) . . . . ? C28 C23 C24 C25 -0.2(2) . . . . ? C22 C23 C24 C25 -179.32(15) . . . . ? C23 C24 C25 C26 0.3(3) . . . . ? C24 C25 C26 C27 0.0(3) . . . . ? C25 C26 C27 C28 -0.3(3) . . . . ? C26 C27 C28 C23 0.3(3) . . . . ? C24 C23 C28 C27 0.0(3) . . . . ? C22 C23 C28 C27 179.00(16) . . . . ? C3 C6 O1 Mn -48.2(2) . . . . ? C7 C6 O1 Mn 131.32(13) . . . . ? O1 Mn O1 C6 -110(100) 2 . . . ? O2 Mn O1 C6 64.18(14) . . . . ? O2 Mn O1 C6 -115.82(14) 2 . . . ? O3 Mn O1 C6 150.51(14) 2 . . . ? O3 Mn O1 C6 -29.49(14) . . . . ? C4 C14 O2 Mn -5.8(3) . . . . ? C15 C14 O2 Mn 176.08(12) . . . . ? O1 Mn O2 C14 148.76(19) 2 . . . ? O1 Mn O2 C14 -31.24(19) . . . . ? O2 Mn O2 C14 -76(100) 2 . . . ? O3 Mn O2 C14 -122.66(19) 2 . . . ? O3 Mn O2 C14 57.34(19) . . . . ? C32 C31 O3 Mn -133.9(2) . . . . ? O1 Mn O3 C31 -47.86(17) 2 . . . ? O1 Mn O3 C31 132.14(17) . . . . ? O2 Mn O3 C31 44.47(17) . . . . ? O2 Mn O3 C31 -135.53(17) 2 . . . ? O3 Mn O3 C31 -173.76(16) 2 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 N1 0.903(17) 1.942(18) 2.839(2) 172(3) 2_565 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.313 _refine_diff_density_min -0.475 _refine_diff_density_rms 0.055