# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Javier Ruiz' 'M Rosario Diaz' 'Santiago Garcia-Granda' 'Roberto Quesada' 'Victor Riera' _publ_contact_author_name 'Dr Javier Ruiz' _publ_contact_author_address ; Quimica Organica e Inorganica Universidad de Oviedo Julian Clavería s/n Oviedo Spain 33071 SPAIN ; _publ_contact_author_email JRUIZ@SAURON.QUIMICA.UNIOVI.ES _publ_requested_journal 'Chemical Communications' _publ_section_title ; Dithiocarbamyl-substituted diphosphanylmethanide complexes of manganese(I): A new type of ambivalent metalloligands. ; data_2 _database_code_CSD 210265 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C32 H26 Mn N O4 P2 S2' _chemical_formula_sum 'C32 H26 Mn N O4 P2 S2' _chemical_formula_weight 669.54 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' O O 0.0106 0.0060 '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' 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 10.5648(7) _cell_length_b 11.6965(6) _cell_length_c 15.0420(10) _cell_angle_alpha 95.264(5) _cell_angle_beta 104.315(4) _cell_angle_gamma 115.24(4) _cell_volume 1587.29(64) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 3 _cell_measurement_theta_max 10 _exptl_crystal_description Prismatic _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 0.685 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Enraf-Nonius CAD4' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 3.82 _diffrn_reflns_number 5620 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0808 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max -1 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 25.98 _reflns_number_total 5620 _reflns_number_gt 3245 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; Nonius CAD-4 Diffractometer Control Software. Data collection with profile analysis over all refelctions (Lehmen and Larsen, 1974; Grant and Gable, 1978) ; _computing_cell_refinement 'CRYSDA (Beurskens et al, 1992)' _computing_data_reduction 'THE REFLEX (local program)' _computing_structure_solution ; Direct Methods using SHELXS97 (Sheldrick,1997). ; _computing_structure_refinement ; Anisotropic least-square carried out with SHELXS-97 (Sheldrick, 1997). Geometric calculations made with PARST (Nardelli, 1983). ; _computing_molecular_graphics ; EUCLID (Speck, 1982) ; _computing_publication_material ; All calculations are made at the University of Oviedo on the Scientific Computer Centre and X-Ray group ALPHA/AXP-compututer ; _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^)+(0.0452P)^2^+0.3971P] 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 5620 _refine_ls_number_parameters 474 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1148 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.1097 _refine_ls_wR_factor_gt 0.0902 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.50670(6) 0.29599(6) 0.60580(4) 0.04039(17) Uani 1 d . . . P1 P 0.40345(10) 0.15503(9) 0.69946(6) 0.0363(2) Uani 1 d . . . P2 P 0.66389(10) 0.37215(9) 0.76043(6) 0.0378(2) Uani 1 d . . . S1 S 0.56909(10) 0.22455(10) 0.91522(6) 0.0420(2) Uani 1 d . . . S2 S 0.77786(13) 0.11687(13) 0.89209(8) 0.0677(3) Uani 1 d . . . N1 N 0.7071(3) 0.1467(3) 1.0453(2) 0.0513(8) Uani 1 d . . . O1 O 0.6999(4) 0.5162(3) 0.5409(2) 0.0816(10) Uani 1 d . . . O2 O 0.2747(4) 0.1762(4) 0.4192(2) 0.0895(11) Uani 1 d . . . O3 O 0.6428(3) 0.1277(3) 0.5651(2) 0.0630(8) Uani 1 d . . . O4 O 0.3639(3) 0.4512(3) 0.6594(2) 0.0702(9) Uani 1 d . . . C10 C 0.6240(5) 0.4296(4) 0.5642(3) 0.0548(10) Uani 1 d . . . C20 C 0.3631(5) 0.2190(4) 0.4915(3) 0.0566(10) Uani 1 d . . . C30 C 0.5925(4) 0.1931(4) 0.5806(2) 0.0463(9) Uani 1 d . . . C40 C 0.4176(4) 0.3910(4) 0.6388(3) 0.0502(10) Uani 1 d . . . C1 C 0.5571(4) 0.2384(3) 0.7996(2) 0.0363(8) Uani 1 d . . . C2 C 0.6917(4) 0.1571(4) 0.9569(2) 0.0415(8) Uani 1 d . . . C3 C 0.6213(7) 0.1719(7) 1.1005(4) 0.0681(14) Uani 1 d . . . H3A H 0.578(7) 0.108(7) 1.130(5) 0.15(3) Uiso 1 d . . . H3B H 0.591(6) 0.227(6) 1.091(4) 0.11(2) Uiso 1 d . . . H3C H 0.703(7) 0.232(7) 1.159(6) 0.16(3) Uiso 1 d . . . C4 C 0.8137(6) 0.1067(7) 1.0957(4) 0.0862(17) Uani 1 d . . . H4A H 0.7888 0.0775 1.1495 0.14(2) Uiso 1 calc R . . H4B H 0.9111 0.1790 1.1160 0.18(4) Uiso 1 calc R . . H4C H 0.8111 0.0374 1.0545 0.16(3) Uiso 1 calc R . . C11 C 0.3517(4) -0.0178(4) 0.6701(2) 0.0411(9) Uani 1 d . . . C12 C 0.2066(5) -0.1142(4) 0.6302(3) 0.0619(12) Uani 1 d . . . H12 H 0.126(4) -0.096(4) 0.614(3) 0.059(12) Uiso 1 d . . . C13 C 0.1755(7) -0.2440(5) 0.6086(4) 0.0827(16) Uani 1 d . . . H13 H 0.076(5) -0.302(5) 0.580(3) 0.075(15) Uiso 1 d . . . C14 C 0.2859(8) -0.2775(6) 0.6266(4) 0.0818(17) Uani 1 d . . . H14 H 0.259(5) -0.368(5) 0.611(3) 0.082(14) Uiso 1 d . . . C15 C 0.4279(7) -0.1840(5) 0.6664(4) 0.0688(14) Uani 1 d . . . H15 H 0.505(5) -0.202(5) 0.688(4) 0.093(18) Uiso 1 d . . . C16 C 0.4627(5) -0.0544(4) 0.6883(3) 0.0530(10) Uani 1 d . . . H16 H 0.568(4) 0.016(4) 0.724(2) 0.043(10) Uiso 1 d . . . C21 C 0.2326(4) 0.1509(4) 0.7103(2) 0.0407(8) Uani 1 d . . . C22 C 0.2075(4) 0.1585(4) 0.7961(3) 0.0460(9) Uani 1 d . . . H22 H 0.284(4) 0.177(3) 0.850(3) 0.042(10) Uiso 1 d . . . C23 C 0.0734(5) 0.1462(4) 0.8014(3) 0.0578(11) Uani 1 d . . . H23 H 0.058(4) 0.148(4) 0.863(3) 0.057(11) Uiso 1 d . . . C24 C -0.0364(5) 0.1272(4) 0.7211(3) 0.0575(12) Uani 1 d . . . H24 H -0.126(4) 0.121(4) 0.725(3) 0.063(12) Uiso 1 d . . . C25 C -0.0130(5) 0.1207(5) 0.6361(3) 0.0636(12) Uani 1 d . . . H25 H -0.083(4) 0.106(4) 0.576(3) 0.066(12) Uiso 1 d . . . C26 C 0.1205(4) 0.1321(5) 0.6304(3) 0.0573(11) Uani 1 d . . . H26 H 0.136(4) 0.126(4) 0.572(3) 0.057(11) Uiso 1 d . . . C31 C 0.6830(4) 0.5238(4) 0.8213(3) 0.0473(9) Uani 1 d . . . C32 C 0.5977(5) 0.5252(5) 0.8776(3) 0.0577(11) Uani 1 d . . . H32 H 0.531(4) 0.447(4) 0.884(2) 0.039(10) Uiso 1 d . . . C33 C 0.6070(7) 0.6402(6) 0.9180(4) 0.0771(16) Uani 1 d . . . H33 H 0.550(5) 0.629(4) 0.955(3) 0.076(15) Uiso 1 d . . . C34 C 0.6976(7) 0.7551(7) 0.9010(5) 0.094(2) Uani 1 d . . . H34 H 0.697(6) 0.822(6) 0.924(4) 0.096(18) Uiso 1 d . . . C35 C 0.7796(6) 0.7553(5) 0.8440(5) 0.099(2) Uani 1 d . . . H35 H 0.851(5) 0.837(5) 0.840(3) 0.084(15) Uiso 1 d . . . C36 C 0.7744(6) 0.6412(5) 0.8048(4) 0.0790(16) Uani 1 d . . . H36 H 0.829(5) 0.641(4) 0.767(3) 0.078(15) Uiso 1 d . . . C41 C 0.8570(4) 0.4100(4) 0.7825(3) 0.0451(9) Uani 1 d . . . C42 C 0.9192(5) 0.4194(5) 0.7111(4) 0.0594(12) Uani 1 d . . . H42 H 0.861(4) 0.404(4) 0.653(3) 0.045(11) Uiso 1 d . . . C43 C 1.0649(6) 0.4490(5) 0.7295(5) 0.0787(17) Uani 1 d . . . H43 H 1.102(5) 0.449(5) 0.687(4) 0.091(19) Uiso 1 d . . . C44 C 1.1521(6) 0.4708(5) 0.8192(5) 0.0827(18) Uani 1 d . . . H44 H 1.247(6) 0.486(5) 0.829(4) 0.102(18) Uiso 1 d . . . C45 C 1.0936(6) 0.4625(6) 0.8905(5) 0.0904(19) Uani 1 d . . . H45 H 1.138(5) 0.466(5) 0.947(3) 0.064(15) Uiso 1 d . . . C46 C 0.9457(5) 0.4316(5) 0.8729(3) 0.0692(14) Uani 1 d . . . H46 H 0.904(4) 0.420(4) 0.922(3) 0.072(14) Uiso 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 0.0528(3) 0.0472(4) 0.0331(3) 0.0143(3) 0.0186(2) 0.0302(3) P1 0.0429(5) 0.0429(6) 0.0318(5) 0.0106(4) 0.0161(4) 0.0251(5) P2 0.0440(5) 0.0415(6) 0.0370(5) 0.0102(4) 0.0178(4) 0.0250(5) S1 0.0505(5) 0.0582(6) 0.0321(5) 0.0150(4) 0.0182(4) 0.0346(5) S2 0.0768(8) 0.0995(10) 0.0623(7) 0.0250(7) 0.0323(6) 0.0655(8) N1 0.063(2) 0.059(2) 0.0392(19) 0.0215(16) 0.0149(15) 0.0335(18) O1 0.105(3) 0.076(2) 0.080(2) 0.050(2) 0.048(2) 0.041(2) O2 0.092(2) 0.104(3) 0.046(2) 0.0039(19) 0.0005(18) 0.036(2) O3 0.081(2) 0.067(2) 0.0659(19) 0.0160(16) 0.0356(16) 0.0503(18) O4 0.090(2) 0.084(2) 0.071(2) 0.0235(18) 0.0309(17) 0.067(2) C10 0.071(3) 0.064(3) 0.045(2) 0.022(2) 0.022(2) 0.041(2) C20 0.066(3) 0.062(3) 0.050(3) 0.015(2) 0.025(2) 0.032(2) C30 0.057(2) 0.056(3) 0.037(2) 0.0187(19) 0.0231(18) 0.029(2) C40 0.060(2) 0.064(3) 0.039(2) 0.019(2) 0.0152(19) 0.038(2) C1 0.0430(19) 0.043(2) 0.0287(18) 0.0104(16) 0.0147(15) 0.0228(17) C2 0.039(2) 0.046(2) 0.042(2) 0.0165(18) 0.0132(16) 0.0213(18) C3 0.100(4) 0.078(4) 0.046(3) 0.026(3) 0.037(3) 0.049(4) C4 0.101(5) 0.119(5) 0.058(3) 0.038(3) 0.009(3) 0.074(4) C11 0.058(2) 0.040(2) 0.0335(19) 0.0119(17) 0.0237(17) 0.024(2) C12 0.065(3) 0.052(3) 0.063(3) 0.005(2) 0.019(2) 0.024(3) C13 0.089(4) 0.048(3) 0.090(4) 0.002(3) 0.033(3) 0.013(3) C14 0.135(6) 0.052(4) 0.089(4) 0.024(3) 0.068(4) 0.051(4) C15 0.107(4) 0.073(4) 0.069(3) 0.032(3) 0.054(3) 0.062(4) C16 0.075(3) 0.059(3) 0.047(2) 0.018(2) 0.032(2) 0.042(3) C21 0.043(2) 0.046(2) 0.038(2) 0.0092(17) 0.0148(16) 0.0247(18) C22 0.047(2) 0.058(3) 0.042(2) 0.014(2) 0.0173(19) 0.030(2) C23 0.060(3) 0.074(3) 0.059(3) 0.022(2) 0.034(2) 0.039(2) C24 0.044(2) 0.075(3) 0.064(3) 0.017(2) 0.022(2) 0.033(2) C25 0.047(2) 0.087(4) 0.057(3) 0.016(3) 0.009(2) 0.036(2) C26 0.050(2) 0.079(3) 0.045(3) 0.013(2) 0.016(2) 0.032(2) C31 0.049(2) 0.047(2) 0.049(2) 0.0052(19) 0.0119(18) 0.028(2) C32 0.072(3) 0.058(3) 0.055(3) 0.006(2) 0.023(2) 0.041(3) C33 0.098(4) 0.088(5) 0.068(3) 0.003(3) 0.030(3) 0.065(4) C34 0.086(4) 0.065(4) 0.128(5) -0.015(4) 0.017(4) 0.050(4) C35 0.075(4) 0.039(3) 0.177(7) 0.007(4) 0.046(4) 0.020(3) C36 0.068(3) 0.046(3) 0.126(5) 0.005(3) 0.048(3) 0.023(3) C41 0.045(2) 0.041(2) 0.057(3) 0.0108(19) 0.0204(19) 0.0251(18) C42 0.058(3) 0.070(3) 0.074(3) 0.033(3) 0.039(3) 0.038(3) C43 0.063(3) 0.079(4) 0.119(5) 0.038(4) 0.058(4) 0.036(3) C44 0.040(3) 0.065(3) 0.135(6) -0.001(3) 0.030(3) 0.022(3) C45 0.054(3) 0.111(5) 0.086(4) -0.011(4) -0.001(3) 0.039(3) C46 0.047(3) 0.096(4) 0.056(3) -0.003(3) 0.009(2) 0.034(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 C10 1.811(5) . ? Mn1 C20 1.824(5) . ? Mn1 C40 1.841(4) . ? Mn1 C30 1.851(4) . ? Mn1 P2 2.3259(12) . ? Mn1 P1 2.3548(12) . ? P1 C1 1.740(4) . ? P1 C11 1.831(4) . ? P1 C21 1.832(3) . ? P1 P2 2.688(2) . ? P2 C1 1.749(4) . ? P2 C31 1.825(4) . ? P2 C41 1.826(4) . ? S1 C1 1.740(3) . ? S1 C2 1.804(3) . ? S2 C2 1.650(3) . ? N1 C2 1.322(4) . ? N1 C3 1.467(6) . ? N1 C4 1.468(5) . ? O1 C10 1.141(5) . ? O2 C20 1.143(5) . ? O3 C30 1.139(4) . ? O4 C40 1.141(4) . ? C11 C16 1.388(5) . ? C11 C12 1.389(6) . ? C12 C13 1.396(7) . ? C13 C14 1.357(7) . ? C14 C15 1.357(8) . ? C15 C16 1.384(6) . ? C21 C22 1.383(5) . ? C21 C26 1.386(5) . ? C22 C23 1.386(5) . ? C23 C24 1.375(6) . ? C24 C25 1.362(6) . ? C25 C26 1.384(5) . ? C31 C32 1.384(5) . ? C31 C36 1.390(6) . ? C32 C33 1.378(6) . ? C33 C34 1.370(9) . ? C34 C35 1.362(9) . ? C35 C36 1.381(7) . ? C41 C46 1.377(6) . ? C41 C42 1.381(6) . ? C42 C43 1.373(6) . ? C43 C44 1.362(8) . ? C44 C45 1.356(8) . ? C45 C46 1.393(6) . ? 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 C10 Mn1 C20 94.14(19) . . ? C10 Mn1 C40 90.09(18) . . ? C20 Mn1 C40 91.13(17) . . ? C10 Mn1 C30 94.24(17) . . ? C20 Mn1 C30 90.83(18) . . ? C40 Mn1 C30 175.12(16) . . ? C10 Mn1 P2 94.36(14) . . ? C20 Mn1 P2 171.33(13) . . ? C40 Mn1 P2 87.17(12) . . ? C30 Mn1 P2 90.24(12) . . ? C10 Mn1 P1 164.42(14) . . ? C20 Mn1 P1 101.36(14) . . ? C40 Mn1 P1 88.13(12) . . ? C30 Mn1 P1 87.10(11) . . ? P2 Mn1 P1 70.10(5) . . ? C1 P1 C11 112.10(17) . . ? C1 P1 C21 115.01(15) . . ? C11 P1 C21 102.03(17) . . ? C1 P1 Mn1 93.94(12) . . ? C11 P1 Mn1 121.41(11) . . ? C21 P1 Mn1 113.07(12) . . ? C1 P1 P2 39.73(12) . . ? C11 P1 P2 133.39(12) . . ? C21 P1 P2 122.74(12) . . ? Mn1 P1 P2 54.45(4) . . ? C1 P2 C31 112.33(17) . . ? C1 P2 C41 116.09(16) . . ? C31 P2 C41 101.25(18) . . ? C1 P2 Mn1 94.69(12) . . ? C31 P2 Mn1 114.60(13) . . ? C41 P2 Mn1 118.62(13) . . ? C1 P2 P1 39.48(11) . . ? C31 P2 P1 121.57(13) . . ? C41 P2 P1 135.63(13) . . ? Mn1 P2 P1 55.46(4) . . ? C1 S1 C2 110.02(16) . . ? C2 N1 C3 124.2(3) . . ? C2 N1 C4 121.1(3) . . ? C3 N1 C4 114.7(4) . . ? O1 C10 Mn1 177.8(4) . . ? O2 C20 Mn1 176.9(4) . . ? O3 C30 Mn1 178.7(4) . . ? O4 C40 Mn1 179.2(4) . . ? S1 C1 P1 127.6(2) . . ? S1 C1 P2 127.8(2) . . ? P1 C1 P2 100.79(17) . . ? N1 C2 S2 124.1(3) . . ? N1 C2 S1 112.6(3) . . ? S2 C2 S1 123.3(2) . . ? C16 C11 C12 118.2(4) . . ? C16 C11 P1 118.5(3) . . ? C12 C11 P1 123.3(3) . . ? C11 C12 C13 120.1(5) . . ? C14 C13 C12 120.7(6) . . ? C13 C14 C15 119.7(5) . . ? C14 C15 C16 121.2(5) . . ? C15 C16 C11 120.2(5) . . ? C22 C21 C26 118.0(3) . . ? C22 C21 P1 121.9(3) . . ? C26 C21 P1 120.0(3) . . ? C21 C22 C23 120.7(4) . . ? C24 C23 C22 120.2(4) . . ? C25 C24 C23 119.9(4) . . ? C24 C25 C26 120.1(4) . . ? C25 C26 C21 121.1(4) . . ? C32 C31 C36 117.9(4) . . ? C32 C31 P2 121.6(3) . . ? C36 C31 P2 120.1(3) . . ? C33 C32 C31 120.7(5) . . ? C34 C33 C32 120.6(5) . . ? C35 C34 C33 119.5(5) . . ? C34 C35 C36 120.6(6) . . ? C35 C36 C31 120.6(5) . . ? C46 C41 C42 118.0(4) . . ? C46 C41 P2 119.9(3) . . ? C42 C41 P2 122.1(3) . . ? C43 C42 C41 121.0(5) . . ? C44 C43 C42 120.6(5) . . ? C45 C44 C43 119.4(5) . . ? C44 C45 C46 120.7(6) . . ? C41 C46 C45 120.2(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 C10 Mn1 P1 C1 -8.7(5) . . . . ? C20 Mn1 P1 C1 176.94(17) . . . . ? C40 Mn1 P1 C1 -92.29(16) . . . . ? C30 Mn1 P1 C1 86.67(16) . . . . ? P2 Mn1 P1 C1 -4.63(11) . . . . ? C10 Mn1 P1 C11 -127.6(5) . . . . ? C20 Mn1 P1 C11 57.99(19) . . . . ? C40 Mn1 P1 C11 148.76(19) . . . . ? C30 Mn1 P1 C11 -32.27(19) . . . . ? P2 Mn1 P1 C11 -123.57(15) . . . . ? C10 Mn1 P1 C21 110.6(5) . . . . ? C20 Mn1 P1 C21 -63.72(18) . . . . ? C40 Mn1 P1 C21 27.05(18) . . . . ? C30 Mn1 P1 C21 -153.99(17) . . . . ? P2 Mn1 P1 C21 114.71(13) . . . . ? C10 Mn1 P1 P2 -4.1(5) . . . . ? C20 Mn1 P1 P2 -178.44(13) . . . . ? C40 Mn1 P1 P2 -87.66(13) . . . . ? C30 Mn1 P1 P2 91.30(12) . . . . ? C10 Mn1 P2 C1 -176.49(16) . . . . ? C40 Mn1 P2 C1 93.64(17) . . . . ? C30 Mn1 P2 C1 -82.22(16) . . . . ? P1 Mn1 P2 C1 4.61(11) . . . . ? C10 Mn1 P2 C31 66.33(19) . . . . ? C40 Mn1 P2 C31 -23.54(19) . . . . ? C30 Mn1 P2 C31 160.60(18) . . . . ? P1 Mn1 P2 C31 -112.57(15) . . . . ? C10 Mn1 P2 C41 -53.29(19) . . . . ? C40 Mn1 P2 C41 -143.16(19) . . . . ? C30 Mn1 P2 C41 40.98(18) . . . . ? P1 Mn1 P2 C41 127.81(14) . . . . ? C10 Mn1 P2 P1 178.90(12) . . . . ? C40 Mn1 P2 P1 89.03(13) . . . . ? C30 Mn1 P2 P1 -86.83(12) . . . . ? C11 P1 P2 C1 -70.9(2) . . . . ? C21 P1 P2 C1 90.7(2) . . . . ? Mn1 P1 P2 C1 -172.77(17) . . . . ? C1 P1 P2 C31 -87.4(2) . . . . ? C11 P1 P2 C31 -158.3(2) . . . . ? C21 P1 P2 C31 3.3(2) . . . . ? Mn1 P1 P2 C31 99.80(15) . . . . ? C1 P1 P2 C41 75.4(2) . . . . ? C11 P1 P2 C41 4.5(2) . . . . ? C21 P1 P2 C41 166.2(2) . . . . ? Mn1 P1 P2 C41 -97.35(18) . . . . ? C1 P1 P2 Mn1 172.77(17) . . . . ? C11 P1 P2 Mn1 101.88(15) . . . . ? C21 P1 P2 Mn1 -96.50(13) . . . . ? C2 S1 C1 P1 114.0(2) . . . . ? C2 S1 C1 P2 -92.0(3) . . . . ? C11 P1 C1 S1 -68.5(3) . . . . ? C21 P1 C1 S1 47.5(3) . . . . ? Mn1 P1 C1 S1 165.3(2) . . . . ? P2 P1 C1 S1 159.4(3) . . . . ? C11 P1 C1 P2 132.18(16) . . . . ? C21 P1 C1 P2 -111.86(17) . . . . ? Mn1 P1 C1 P2 5.89(14) . . . . ? C31 P2 C1 S1 -46.2(3) . . . . ? C41 P2 C1 S1 69.6(3) . . . . ? Mn1 P2 C1 S1 -165.3(2) . . . . ? P1 P2 C1 S1 -159.3(3) . . . . ? C31 P2 C1 P1 113.06(17) . . . . ? C41 P2 C1 P1 -131.10(17) . . . . ? Mn1 P2 C1 P1 -5.97(14) . . . . ? C3 N1 C2 S2 -174.6(4) . . . . ? C4 N1 C2 S2 4.9(6) . . . . ? C3 N1 C2 S1 6.9(6) . . . . ? C4 N1 C2 S1 -173.6(4) . . . . ? C1 S1 C2 N1 178.8(3) . . . . ? C1 S1 C2 S2 0.3(3) . . . . ? C1 P1 C11 C16 -34.1(3) . . . . ? C21 P1 C11 C16 -157.7(3) . . . . ? Mn1 P1 C11 C16 75.5(3) . . . . ? P2 P1 C11 C16 6.6(4) . . . . ? C1 P1 C11 C12 146.1(3) . . . . ? C21 P1 C11 C12 22.5(4) . . . . ? Mn1 P1 C11 C12 -104.3(3) . . . . ? P2 P1 C11 C12 -173.2(3) . . . . ? C16 C11 C12 C13 -0.6(6) . . . . ? P1 C11 C12 C13 179.2(4) . . . . ? C11 C12 C13 C14 0.3(8) . . . . ? C12 C13 C14 C15 0.3(8) . . . . ? C13 C14 C15 C16 -0.7(7) . . . . ? C14 C15 C16 C11 0.4(7) . . . . ? C12 C11 C16 C15 0.2(6) . . . . ? P1 C11 C16 C15 -179.6(3) . . . . ? C1 P1 C21 C22 -27.6(4) . . . . ? C11 P1 C21 C22 94.0(4) . . . . ? Mn1 P1 C21 C22 -133.9(3) . . . . ? P2 P1 C21 C22 -72.5(4) . . . . ? C1 P1 C21 C26 156.2(3) . . . . ? C11 P1 C21 C26 -82.2(4) . . . . ? Mn1 P1 C21 C26 49.9(4) . . . . ? P2 P1 C21 C26 111.3(3) . . . . ? C26 C21 C22 C23 0.7(6) . . . . ? P1 C21 C22 C23 -175.6(3) . . . . ? C21 C22 C23 C24 -0.5(6) . . . . ? C22 C23 C24 C25 -0.2(7) . . . . ? C23 C24 C25 C26 0.6(7) . . . . ? C24 C25 C26 C21 -0.4(7) . . . . ? C22 C21 C26 C25 -0.3(6) . . . . ? P1 C21 C26 C25 176.1(3) . . . . ? C1 P2 C31 C32 -11.7(4) . . . . ? C41 P2 C31 C32 -136.2(4) . . . . ? Mn1 P2 C31 C32 94.9(4) . . . . ? P1 P2 C31 C32 31.7(4) . . . . ? C1 P2 C31 C36 174.6(4) . . . . ? C41 P2 C31 C36 50.1(4) . . . . ? Mn1 P2 C31 C36 -78.8(4) . . . . ? P1 P2 C31 C36 -142.0(3) . . . . ? C36 C31 C32 C33 -1.9(7) . . . . ? P2 C31 C32 C33 -175.8(4) . . . . ? C31 C32 C33 C34 2.0(8) . . . . ? C32 C33 C34 C35 -0.4(9) . . . . ? C33 C34 C35 C36 -1.2(10) . . . . ? C34 C35 C36 C31 1.3(10) . . . . ? C32 C31 C36 C35 0.3(8) . . . . ? P2 C31 C36 C35 174.2(5) . . . . ? C1 P2 C41 C46 -56.1(4) . . . . ? C31 P2 C41 C46 65.8(4) . . . . ? Mn1 P2 C41 C46 -167.9(3) . . . . ? P1 P2 C41 C46 -99.3(4) . . . . ? C1 P2 C41 C42 124.7(4) . . . . ? C31 P2 C41 C42 -113.4(4) . . . . ? Mn1 P2 C41 C42 12.9(4) . . . . ? P1 P2 C41 C42 81.5(4) . . . . ? C46 C41 C42 C43 0.2(7) . . . . ? P2 C41 C42 C43 179.4(4) . . . . ? C41 C42 C43 C44 -0.5(8) . . . . ? C42 C43 C44 C45 0.3(8) . . . . ? C43 C44 C45 C46 0.1(9) . . . . ? C42 C41 C46 C45 0.2(7) . . . . ? P2 C41 C46 C45 -179.0(4) . . . . ? C44 C45 C46 C41 -0.4(9) . . . . ? loop_ _publ_manuscript_incl_extra_item '_geom_bond_atom_site_label_D' '_geom_bond_atom_site_label_H' '_geom_contact_atom_site_label_A' '_geom_bond_distance_DH' '_geom_contact_distance_HA' '_geom_contact_distance_DA' '_geom_angle_DHA' '_geom_contact_site_symmetry_A' loop_ _geom_bond_atom_site_label_d _geom_bond_atom_site_label_h _geom_contact_atom_site_label_a _geom_bond_distance_dh _geom_contact_distance_ha _geom_contact_distance_da _geom_angle_dha _geom_contact_site_symmetry_a C3 H3B S1 0.84(8) 2.880(6) 2.59(6) 101.(5) 1_555 C4 H4C S2 0.96(8) 3.011(6) 2.688(1) 100.3(3) 1_555 C16 H16 S2 1.02(3) 3.555(4) 2.67(3) 145.(3) 1_555 C16 H16 O3 1.02(3) 3.255(6) 2.95(4) 98.(2) 1_555 C22 H22 S1 0.92(3) 3.499(5) 2.72(4) 144.(3) 1_555 C26 H26 O2 0.93(5) 3.894(6) 3.00(5) 162.(3) 1_555 C32 H32 S1 0.92(4) 3.510(6) 2.86(5) 128.(3) 1_555 C42 H42 O1 0.88(4) 3.610(7) 2.89(5) 140.(3) 1_555 C42 H42 O3 0.88(4) 3.456(5) 2.98(3) 116.(3) 1_555 _diffrn_measured_fraction_theta_max 0.903 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.903 _refine_diff_density_max 0.259 _refine_diff_density_min -0.231 _refine_diff_density_rms 0.056 #==END #========================================================================== data_4 _database_code_CSD 210266 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C34 H29 Cu Mn N2 O4 P2 S2, 2(C H2 Cl2), B F4' _chemical_formula_sum 'C36 H33 B Cl4 Cu F4 Mn N2 O4 P2 S2' _chemical_formula_weight 1030.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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 10.36890(10) _cell_length_b 12.9100(2) _cell_length_c 16.8117(2) _cell_angle_alpha 101.7570(10) _cell_angle_beta 99.0220(10) _cell_angle_gamma 93.9810(10) _cell_volume 2163.99(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7837 _cell_measurement_theta_min 3 _cell_measurement_theta_max 70 _exptl_crystal_description Prismatic _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 7.355 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.139 _exptl_absorpt_correction_T_max 0.266 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurement Sortav (Blessing 1995) ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7931 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1317 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 68.61 _reflns_number_total 7930 _reflns_number_gt 6386 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD control sofware (Nonius, 1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor, 1997) ; _computing_structure_solution 'DIRDIF-96 (Beurskens, 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0388P)^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 7930 _refine_ls_number_parameters 638 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0614 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1480 _refine_ls_wR_factor_gt 0.1427 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.75409(5) 0.62933(4) 0.31717(3) 0.02843(15) Uani 1 d . . . Mn1 Mn 1.05132(5) 0.84671(4) 0.31118(3) 0.02077(15) Uani 1 d . . . P1 P 1.03856(8) 0.70111(6) 0.37116(4) 0.02055(19) Uani 1 d . . . P2 P 0.93184(8) 0.70411(6) 0.21396(5) 0.02177(19) Uani 1 d . . . S1 S 0.95763(8) 0.47642(6) 0.25430(5) 0.02381(19) Uani 1 d . . . S2 S 0.68584(9) 0.45744(7) 0.30161(6) 0.0332(2) Uani 1 d . . . N1 N 0.8220(3) 0.2966(2) 0.25357(17) 0.0283(6) Uani 1 d . . . N2 N 0.6557(3) 0.7386(2) 0.36111(18) 0.0307(6) Uani 1 d . . . O1 O 1.0498(3) 1.0045(2) 0.20452(16) 0.0426(7) Uani 1 d . . . O2 O 1.2189(3) 0.9709(2) 0.46513(14) 0.0341(6) Uani 1 d . . . O3 O 0.8199(3) 0.9475(2) 0.36616(15) 0.0353(6) Uani 1 d . . . O4 O 1.2967(3) 0.7849(2) 0.24944(15) 0.0353(6) Uani 1 d . . . C10 C 1.0502(4) 0.9442(3) 0.2455(2) 0.0294(7) Uani 1 d . . . C20 C 1.1548(4) 0.9263(2) 0.4047(2) 0.0260(7) Uani 1 d . . . C30 C 0.9040(4) 0.9029(3) 0.34575(19) 0.0274(7) Uani 1 d . . . C40 C 1.2029(4) 0.8052(3) 0.27316(19) 0.0273(7) Uani 1 d . . . C1 C 0.9386(3) 0.6132(2) 0.28278(18) 0.0232(7) Uani 1 d . . . C2 C 0.8160(4) 0.4009(3) 0.26926(19) 0.0261(7) Uani 1 d . . . C3 C 0.7195(5) 0.2224(3) 0.2686(3) 0.0380(9) Uani 1 d . . . H3A H 0.677(6) 0.194(4) 0.221(3) 0.059(16) Uiso 1 d . . . H3B H 0.661(7) 0.252(5) 0.299(4) 0.10(2) Uiso 1 d . . . H3C H 0.762(7) 0.171(5) 0.297(4) 0.084(19) Uiso 1 d . . . C4 C 0.9316(4) 0.2459(3) 0.2231(3) 0.0351(8) Uani 1 d . . . H4A H 0.949(7) 0.268(6) 0.181(4) 0.09(2) Uiso 1 d . . . H4B H 1.009(6) 0.254(4) 0.267(3) 0.067(16) Uiso 1 d . . . H4C H 0.908(6) 0.169(5) 0.185(3) 0.078(18) Uiso 1 d . . . C5 C 0.5951(4) 0.7987(3) 0.3935(2) 0.0282(7) Uani 1 d . . . C6 C 0.5191(5) 0.8748(3) 0.4357(3) 0.0363(9) Uani 1 d . . . H6A H 0.428(6) 0.842(4) 0.433(3) 0.060(15) Uiso 1 d . . . H6B H 0.548(4) 0.890(3) 0.489(3) 0.035(11) Uiso 1 d . . . H6C H 0.512(5) 0.931(4) 0.416(3) 0.056(14) Uiso 1 d . . . C11 C 0.9599(3) 0.7041(2) 0.46129(18) 0.0232(7) Uani 1 d . . . C12 C 0.9141(4) 0.6070(3) 0.47665(19) 0.0256(7) Uani 1 d . . . H12 H 0.932(4) 0.544(3) 0.441(2) 0.019(8) Uiso 1 d . . . C13 C 0.8436(4) 0.6047(3) 0.5394(2) 0.0298(7) Uani 1 d . . . H13 H 0.809(4) 0.535(3) 0.549(2) 0.029(10) Uiso 1 d . . . C14 C 0.8172(4) 0.6987(3) 0.5876(2) 0.0307(7) Uani 1 d . . . H14 H 0.768(4) 0.700(3) 0.629(2) 0.033(10) Uiso 1 d . . . C15 C 0.8651(4) 0.7953(3) 0.5743(2) 0.0334(8) Uani 1 d . . . H15 H 0.840(4) 0.858(4) 0.606(3) 0.042(12) Uiso 1 d . . . C16 C 0.9371(4) 0.7980(3) 0.5112(2) 0.0290(7) Uani 1 d . . . H16 H 0.973(4) 0.867(3) 0.504(2) 0.029(10) Uiso 1 d . . . C21 C 1.1969(3) 0.6548(2) 0.40314(19) 0.0240(7) Uani 1 d . . . C22 C 1.2605(4) 0.6858(3) 0.4847(2) 0.0298(8) Uani 1 d . . . H22 H 1.219(5) 0.720(4) 0.521(3) 0.043(12) Uiso 1 d . . . C23 C 1.3857(4) 0.6592(3) 0.5085(2) 0.0338(8) Uani 1 d . . . H23 H 1.433(5) 0.681(3) 0.564(3) 0.043(12) Uiso 1 d . . . C24 C 1.4487(4) 0.5994(3) 0.4506(2) 0.0332(8) Uani 1 d . . . H24 H 1.525(5) 0.587(3) 0.467(3) 0.038(11) Uiso 1 d . . . C25 C 1.3862(4) 0.5683(3) 0.3698(2) 0.0306(8) Uani 1 d . . . H25 H 1.421(4) 0.529(3) 0.338(2) 0.027(10) Uiso 1 d . . . C26 C 1.2617(4) 0.5953(3) 0.3457(2) 0.0270(7) Uani 1 d . . . H26 H 1.221(4) 0.577(3) 0.293(2) 0.019(9) Uiso 1 d . . . C31 C 1.0078(3) 0.6643(3) 0.12300(19) 0.0255(7) Uani 1 d . . . C32 C 1.0941(4) 0.5879(3) 0.1147(2) 0.0285(7) Uani 1 d . . . H32 H 1.109(4) 0.549(3) 0.152(2) 0.033(10) Uiso 1 d . . . C33 C 1.1590(4) 0.5702(3) 0.0471(2) 0.0325(8) Uani 1 d . . . H33 H 1.221(4) 0.511(3) 0.040(2) 0.032(10) Uiso 1 d . . . C34 C 1.1372(4) 0.6314(3) -0.0110(2) 0.0408(9) Uani 1 d . . . H34 H 1.180(4) 0.623(3) -0.054(3) 0.038(11) Uiso 1 d . . . C35 C 1.0506(6) 0.7071(4) -0.0039(2) 0.0530(12) Uani 1 d . . . H35 H 1.023(6) 0.751(5) -0.043(4) 0.087(19) Uiso 1 d . . . C36 C 0.9843(5) 0.7236(3) 0.0627(2) 0.0417(10) Uani 1 d . . . H36 H 0.920(5) 0.776(4) 0.069(3) 0.062(15) Uiso 1 d . . . C41 C 0.7609(3) 0.7112(3) 0.16963(19) 0.0273(7) Uani 1 d . . . C42 C 0.6771(4) 0.6178(3) 0.1388(2) 0.0306(8) Uani 1 d . . . H42 H 0.702(4) 0.555(4) 0.134(2) 0.035(11) Uiso 1 d . . . C43 C 0.5444(4) 0.6223(3) 0.1124(2) 0.0374(9) Uani 1 d . . . H43 H 0.490(5) 0.558(4) 0.090(3) 0.046(12) Uiso 1 d . . . C44 C 0.4943(4) 0.7199(3) 0.1162(2) 0.0391(9) Uani 1 d . . . H44 H 0.398(5) 0.721(4) 0.101(3) 0.046(12) Uiso 1 d . . . C45 C 0.5785(4) 0.8127(3) 0.1451(2) 0.0378(9) Uani 1 d . . . H45 H 0.549(5) 0.874(4) 0.152(3) 0.042(12) Uiso 1 d . . . C46 C 0.7096(4) 0.8084(3) 0.1712(2) 0.0321(8) Uani 1 d . . . H46 H 0.757(4) 0.865(4) 0.192(3) 0.038(12) Uiso 1 d . . . F1 F 0.3348(3) 1.0332(2) 0.32613(18) 0.0574(7) Uani 1 d . . . F2 F 0.4308(4) 1.0568(2) 0.21723(16) 0.0722(9) Uani 1 d . . . F3 F 0.5516(3) 1.0768(3) 0.3434(2) 0.0736(9) Uani 1 d . . . F4 F 0.4140(3) 1.19681(18) 0.31574(14) 0.0474(6) Uani 1 d . . . B1 B 0.4310(5) 1.0897(3) 0.2991(2) 0.0334(9) Uani 1 d . . . Cl1 Cl 0.24088(13) 0.35599(11) 0.18246(9) 0.0670(3) Uani 1 d . . . Cl2 Cl 0.4297(2) 0.31202(12) 0.07397(9) 0.0897(6) Uani 1 d . . . C7 C 0.3844(5) 0.2956(4) 0.1662(3) 0.0449(10) Uani 1 d . . . H7A H 0.369(5) 0.221(4) 0.163(3) 0.046(12) Uiso 1 d . . . H7B H 0.443(5) 0.328(4) 0.211(3) 0.040(12) Uiso 1 d . . . Cl3 Cl 0.6498(3) 0.10965(15) 0.03201(11) 0.1111(7) Uani 1 d . . . Cl4 Cl 0.8396(3) -0.0371(2) 0.0007(2) 0.1534(11) Uani 1 d . . . C8 C 0.6985(14) -0.0021(10) -0.0271(6) 0.232(9) Uani 1 d . . . H8A H 0.6341 -0.0615 -0.0300 0.279 Uiso 1 calc R . . H8B H 0.6942 0.0093 -0.0827 0.279 Uiso 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 Cu1 0.0292(3) 0.0249(3) 0.0307(3) 0.0026(2) 0.0088(2) 0.0013(2) Mn1 0.0269(3) 0.0188(3) 0.0155(3) 0.00268(19) 0.0032(2) -0.0014(2) P1 0.0268(4) 0.0184(4) 0.0152(4) 0.0024(3) 0.0032(3) -0.0011(3) P2 0.0265(4) 0.0211(4) 0.0157(4) 0.0022(3) 0.0015(3) -0.0006(3) S1 0.0285(4) 0.0195(4) 0.0219(4) 0.0011(3) 0.0059(3) -0.0008(3) S2 0.0308(5) 0.0267(4) 0.0416(5) 0.0041(4) 0.0115(4) -0.0031(3) N1 0.0329(16) 0.0232(14) 0.0281(14) 0.0040(11) 0.0074(12) -0.0026(12) N2 0.0325(17) 0.0276(15) 0.0323(15) 0.0074(12) 0.0073(13) -0.0013(13) O1 0.0601(19) 0.0367(14) 0.0373(14) 0.0216(12) 0.0101(13) 0.0051(13) O2 0.0407(15) 0.0333(13) 0.0215(12) -0.0026(10) -0.0006(11) -0.0040(11) O3 0.0383(15) 0.0342(13) 0.0338(13) 0.0030(10) 0.0111(11) 0.0086(12) O4 0.0354(15) 0.0381(14) 0.0325(13) 0.0026(11) 0.0144(11) 0.0007(11) C10 0.035(2) 0.0278(17) 0.0232(16) 0.0019(14) 0.0059(14) -0.0008(14) C20 0.0362(19) 0.0203(15) 0.0242(17) 0.0067(12) 0.0113(14) 0.0025(14) C30 0.036(2) 0.0226(16) 0.0202(16) 0.0020(12) 0.0026(14) -0.0038(15) C40 0.041(2) 0.0220(15) 0.0146(15) 0.0015(12) 0.0004(14) -0.0057(14) C1 0.0281(17) 0.0210(15) 0.0193(15) 0.0030(12) 0.0041(12) -0.0020(13) C2 0.0323(19) 0.0232(16) 0.0197(15) 0.0031(12) -0.0002(13) -0.0019(13) C3 0.039(2) 0.0277(18) 0.046(2) 0.0071(17) 0.011(2) -0.0067(17) C4 0.044(2) 0.0266(18) 0.034(2) 0.0028(15) 0.0094(17) 0.0016(16) C5 0.0307(19) 0.0252(16) 0.0280(17) 0.0059(13) 0.0058(14) -0.0035(14) C6 0.044(2) 0.0295(19) 0.035(2) 0.0041(16) 0.0103(18) 0.0042(17) C11 0.0280(17) 0.0235(15) 0.0174(15) 0.0051(12) 0.0023(12) 0.0009(13) C12 0.0357(19) 0.0214(15) 0.0185(15) 0.0032(12) 0.0031(13) 0.0015(14) C13 0.037(2) 0.0293(17) 0.0246(17) 0.0092(13) 0.0086(14) -0.0009(15) C14 0.034(2) 0.0382(19) 0.0231(17) 0.0100(14) 0.0088(15) 0.0052(15) C15 0.048(2) 0.0323(18) 0.0219(17) 0.0045(14) 0.0130(16) 0.0088(17) C16 0.041(2) 0.0251(16) 0.0197(16) 0.0043(13) 0.0055(14) 0.0004(15) C21 0.0296(18) 0.0202(14) 0.0213(15) 0.0062(12) 0.0029(13) -0.0048(13) C22 0.037(2) 0.0304(17) 0.0203(17) 0.0044(14) 0.0017(15) -0.0002(15) C23 0.032(2) 0.0392(19) 0.0284(18) 0.0116(15) -0.0046(15) -0.0028(16) C24 0.0228(19) 0.039(2) 0.041(2) 0.0202(16) 0.0024(15) 0.0003(15) C25 0.0306(19) 0.0287(17) 0.0334(19) 0.0061(15) 0.0093(15) 0.0025(15) C26 0.0304(18) 0.0269(16) 0.0225(17) 0.0052(13) 0.0029(14) -0.0004(14) C31 0.0295(18) 0.0272(16) 0.0160(14) 0.0011(12) 0.0008(13) -0.0056(13) C32 0.0295(18) 0.0313(17) 0.0209(16) 0.0012(14) 0.0012(13) -0.0033(14) C33 0.033(2) 0.0350(19) 0.0236(17) -0.0042(14) 0.0049(14) -0.0039(15) C34 0.049(3) 0.051(2) 0.0198(18) -0.0008(16) 0.0129(17) 0.0019(19) C35 0.078(4) 0.064(3) 0.025(2) 0.0184(19) 0.017(2) 0.020(3) C36 0.058(3) 0.048(2) 0.0231(18) 0.0100(16) 0.0105(17) 0.017(2) C41 0.0300(18) 0.0334(17) 0.0175(15) 0.0039(13) 0.0040(13) 0.0027(14) C42 0.036(2) 0.0315(19) 0.0217(17) 0.0040(14) 0.0005(14) -0.0010(16) C43 0.032(2) 0.046(2) 0.0299(19) 0.0070(16) -0.0022(15) -0.0073(17) C44 0.031(2) 0.055(2) 0.0294(19) 0.0082(17) 0.0007(16) 0.0049(18) C45 0.041(2) 0.042(2) 0.0281(19) 0.0039(16) 0.0004(16) 0.0132(18) C46 0.038(2) 0.0303(19) 0.0243(17) 0.0028(14) -0.0013(15) 0.0029(16) F1 0.0476(16) 0.0496(14) 0.0788(18) 0.0190(13) 0.0234(13) -0.0113(12) F2 0.129(3) 0.0533(16) 0.0374(14) 0.0044(12) 0.0273(16) 0.0181(17) F3 0.0466(17) 0.077(2) 0.109(2) 0.0619(18) 0.0001(16) -0.0022(15) F4 0.0649(17) 0.0355(12) 0.0414(13) 0.0062(9) 0.0132(11) -0.0008(11) B1 0.041(2) 0.030(2) 0.029(2) 0.0076(16) 0.0072(17) -0.0067(18) Cl1 0.0547(7) 0.0611(7) 0.0841(9) 0.0085(6) 0.0135(6) 0.0175(6) Cl2 0.1505(17) 0.0714(8) 0.0613(8) 0.0116(7) 0.0649(10) 0.0110(9) C7 0.055(3) 0.044(2) 0.035(2) 0.0085(18) 0.006(2) 0.012(2) Cl3 0.156(2) 0.0820(11) 0.0723(10) -0.0126(8) -0.0159(11) 0.0227(12) Cl4 0.1140(19) 0.174(2) 0.217(3) 0.127(2) 0.0343(18) 0.0627(17) C8 0.284(16) 0.217(12) 0.111(7) -0.101(8) -0.106(9) 0.179(12) _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 Cu1 N2 1.894(3) . ? Cu1 C1 2.095(3) . ? Cu1 S2 2.2317(9) . ? Mn1 C20 1.827(3) . ? Mn1 C10 1.836(3) . ? Mn1 C40 1.859(4) . ? Mn1 C30 1.860(4) . ? Mn1 P1 2.3124(9) . ? Mn1 P2 2.3275(9) . ? P1 C1 1.799(3) . ? P1 C21 1.825(4) . ? P1 C11 1.825(3) . ? P2 C1 1.806(3) . ? P2 C31 1.827(3) . ? P2 C41 1.828(4) . ? S1 C1 1.766(3) . ? S1 C2 1.785(4) . ? S2 C2 1.690(4) . ? N1 C2 1.326(4) . ? N1 C4 1.460(5) . ? N1 C3 1.467(5) . ? N2 C5 1.139(5) . ? O1 C10 1.140(4) . ? O2 C20 1.141(4) . ? O3 C30 1.136(4) . ? O4 C40 1.136(5) . ? C3 H3A 0.85(6) . ? C3 H3B 0.91(7) . ? C3 H3C 0.98(7) . ? C4 H4A 0.85(7) . ? C4 H4B 0.98(6) . ? C4 H4C 1.05(6) . ? C5 C6 1.445(5) . ? C6 H6A 1.00(6) . ? C6 H6B 0.88(4) . ? C6 H6C 0.86(5) . ? C11 C16 1.385(5) . ? C11 C12 1.397(4) . ? C12 C13 1.379(5) . ? C12 H12 0.95(4) . ? C13 C14 1.385(5) . ? C13 H13 0.99(4) . ? C14 C15 1.384(5) . ? C14 H14 0.93(4) . ? C15 C16 1.393(5) . ? C15 H15 0.95(5) . ? C16 H16 0.98(4) . ? C21 C22 1.390(5) . ? C21 C26 1.395(5) . ? C22 C23 1.385(5) . ? C22 H22 0.87(5) . ? C23 C24 1.391(6) . ? C23 H23 0.95(5) . ? C24 C25 1.376(5) . ? C24 H24 0.84(5) . ? C25 C26 1.381(5) . ? C25 H25 0.81(4) . ? C26 H26 0.89(4) . ? C31 C32 1.377(5) . ? C31 C36 1.393(5) . ? C32 C33 1.397(5) . ? C32 H32 0.89(4) . ? C33 C34 1.378(6) . ? C33 H33 1.03(4) . ? C34 C35 1.373(7) . ? C34 H34 0.89(4) . ? C35 C36 1.391(6) . ? C35 H35 0.98(6) . ? C36 H36 0.98(6) . ? C41 C42 1.392(5) . ? C41 C46 1.393(5) . ? C42 C43 1.388(6) . ? C42 H42 0.86(5) . ? C43 C44 1.389(6) . ? C43 H43 0.94(5) . ? C44 C45 1.384(6) . ? C44 H44 0.99(5) . ? C45 C46 1.371(6) . ? C45 H45 0.87(5) . ? C46 H46 0.83(4) . ? F1 B1 1.382(5) . ? F2 B1 1.354(5) . ? F3 B1 1.390(5) . ? F4 B1 1.384(5) . ? Cl1 C7 1.760(5) . ? Cl2 C7 1.737(5) . ? C7 H7A 0.96(5) . ? C7 H7B 0.89(5) . ? Cl3 C8 1.731(8) . ? Cl4 C8 1.590(11) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 C1 138.91(12) . . ? N2 Cu1 S2 122.00(9) . . ? C1 Cu1 S2 98.78(9) . . ? C20 Mn1 C10 99.12(14) . . ? C20 Mn1 C40 88.61(15) . . ? C10 Mn1 C40 86.81(15) . . ? C20 Mn1 C30 89.99(15) . . ? C10 Mn1 C30 87.09(15) . . ? C40 Mn1 C30 173.45(14) . . ? C20 Mn1 P1 91.15(10) . . ? C10 Mn1 P1 169.33(11) . . ? C40 Mn1 P1 90.54(10) . . ? C30 Mn1 P1 95.88(10) . . ? C20 Mn1 P2 162.36(10) . . ? C10 Mn1 P2 98.13(11) . . ? C40 Mn1 P2 88.67(10) . . ? C30 Mn1 P2 94.56(10) . . ? P1 Mn1 P2 71.45(3) . . ? C1 P1 C21 113.75(15) . . ? C1 P1 C11 109.43(15) . . ? C21 P1 C11 102.60(15) . . ? C1 P1 Mn1 95.85(10) . . ? C21 P1 Mn1 114.30(10) . . ? C11 P1 Mn1 121.27(11) . . ? C1 P2 C31 115.38(16) . . ? C1 P2 C41 109.63(15) . . ? C31 P2 C41 103.07(15) . . ? C1 P2 Mn1 95.15(10) . . ? C31 P2 Mn1 113.37(11) . . ? C41 P2 Mn1 120.80(11) . . ? C1 S1 C2 108.91(16) . . ? C2 S2 Cu1 100.53(12) . . ? C2 N1 C4 123.6(3) . . ? C2 N1 C3 122.1(3) . . ? C4 N1 C3 114.3(3) . . ? C5 N2 Cu1 173.2(3) . . ? O1 C10 Mn1 179.8(3) . . ? O2 C20 Mn1 176.0(3) . . ? O3 C30 Mn1 172.6(3) . . ? O4 C40 Mn1 176.5(3) . . ? S1 C1 P1 122.82(19) . . ? S1 C1 P2 124.98(18) . . ? P1 C1 P2 97.45(15) . . ? S1 C1 Cu1 108.81(16) . . ? P1 C1 Cu1 99.11(14) . . ? P2 C1 Cu1 98.56(15) . . ? N1 C2 S2 122.8(3) . . ? N1 C2 S1 114.3(3) . . ? S2 C2 S1 122.90(19) . . ? N1 C3 H3A 104(4) . . ? N1 C3 H3B 116(4) . . ? H3A C3 H3B 107(6) . . ? N1 C3 H3C 108(4) . . ? H3A C3 H3C 113(5) . . ? H3B C3 H3C 108(5) . . ? N1 C4 H4A 111(5) . . ? N1 C4 H4B 112(3) . . ? H4A C4 H4B 113(6) . . ? N1 C4 H4C 116(3) . . ? H4A C4 H4C 88(5) . . ? H4B C4 H4C 115(5) . . ? N2 C5 C6 179.2(4) . . ? C5 C6 H6A 110(3) . . ? C5 C6 H6B 111(3) . . ? H6A C6 H6B 101(4) . . ? C5 C6 H6C 114(3) . . ? H6A C6 H6C 107(5) . . ? H6B C6 H6C 112(4) . . ? C16 C11 C12 119.4(3) . . ? C16 C11 P1 122.6(2) . . ? C12 C11 P1 117.8(2) . . ? C13 C12 C11 120.2(3) . . ? C13 C12 H12 123(2) . . ? C11 C12 H12 117(2) . . ? C12 C13 C14 120.3(3) . . ? C12 C13 H13 120(2) . . ? C14 C13 H13 120(2) . . ? C15 C14 C13 119.8(3) . . ? C15 C14 H14 118(2) . . ? C13 C14 H14 123(2) . . ? C14 C15 C16 120.1(3) . . ? C14 C15 H15 117(3) . . ? C16 C15 H15 123(3) . . ? C11 C16 C15 120.1(3) . . ? C11 C16 H16 121(2) . . ? C15 C16 H16 119(2) . . ? C22 C21 C26 118.4(3) . . ? C22 C21 P1 120.2(3) . . ? C26 C21 P1 121.2(2) . . ? C23 C22 C21 120.9(4) . . ? C23 C22 H22 120(3) . . ? C21 C22 H22 119(3) . . ? C22 C23 C24 119.9(3) . . ? C22 C23 H23 123(3) . . ? C24 C23 H23 117(3) . . ? C25 C24 C23 119.4(4) . . ? C25 C24 H24 123(3) . . ? C23 C24 H24 117(3) . . ? C24 C25 C26 120.8(4) . . ? C24 C25 H25 118(3) . . ? C26 C25 H25 121(3) . . ? C25 C26 C21 120.5(3) . . ? C25 C26 H26 121(2) . . ? C21 C26 H26 118(2) . . ? C32 C31 C36 119.4(3) . . ? C32 C31 P2 124.4(3) . . ? C36 C31 P2 115.9(3) . . ? C31 C32 C33 120.8(3) . . ? C31 C32 H32 121(3) . . ? C33 C32 H32 119(3) . . ? C34 C33 C32 119.2(4) . . ? C34 C33 H33 120(2) . . ? C32 C33 H33 121(2) . . ? C35 C34 C33 120.7(4) . . ? C35 C34 H34 119(3) . . ? C33 C34 H34 121(3) . . ? C34 C35 C36 120.2(4) . . ? C34 C35 H35 128(4) . . ? C36 C35 H35 112(4) . . ? C35 C36 C31 119.8(4) . . ? C35 C36 H36 123(3) . . ? C31 C36 H36 117(3) . . ? C42 C41 C46 118.8(3) . . ? C42 C41 P2 119.5(3) . . ? C46 C41 P2 121.5(3) . . ? C43 C42 C41 120.1(4) . . ? C43 C42 H42 116(3) . . ? C41 C42 H42 124(3) . . ? C42 C43 C44 120.3(4) . . ? C42 C43 H43 119(3) . . ? C44 C43 H43 121(3) . . ? C45 C44 C43 119.4(4) . . ? C45 C44 H44 122(3) . . ? C43 C44 H44 119(3) . . ? C46 C45 C44 120.4(4) . . ? C46 C45 H45 118(3) . . ? C44 C45 H45 121(3) . . ? C45 C46 C41 120.9(4) . . ? C45 C46 H46 118(3) . . ? C41 C46 H46 120(3) . . ? F2 B1 F1 112.8(3) . . ? F2 B1 F4 108.7(3) . . ? F1 B1 F4 109.8(4) . . ? F2 B1 F3 109.7(4) . . ? F1 B1 F3 107.7(3) . . ? F4 B1 F3 108.1(3) . . ? Cl2 C7 Cl1 111.3(3) . . ? Cl2 C7 H7A 107(3) . . ? Cl1 C7 H7A 110(3) . . ? Cl2 C7 H7B 113(3) . . ? Cl1 C7 H7B 103(3) . . ? H7A C7 H7B 112(4) . . ? Cl4 C8 Cl3 118.8(5) . . ? Cl4 C8 H8A 107.6 . . ? Cl3 C8 H8A 107.6 . . ? Cl4 C8 H8B 107.6 . . ? Cl3 C8 H8B 107.6 . . ? H8A C8 H8B 107.0 . . ? 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 C20 Mn1 P1 C1 -179.13(16) . . . . ? C10 Mn1 P1 C1 -15.0(7) . . . . ? C40 Mn1 P1 C1 -90.51(15) . . . . ? C30 Mn1 P1 C1 90.76(15) . . . . ? P2 Mn1 P1 C1 -2.09(11) . . . . ? C20 Mn1 P1 C21 -59.76(16) . . . . ? C10 Mn1 P1 C21 104.4(7) . . . . ? C40 Mn1 P1 C21 28.86(15) . . . . ? C30 Mn1 P1 C21 -149.87(15) . . . . ? P2 Mn1 P1 C21 117.28(12) . . . . ? C20 Mn1 P1 C11 63.90(17) . . . . ? C10 Mn1 P1 C11 -132.0(7) . . . . ? C40 Mn1 P1 C11 152.52(16) . . . . ? C30 Mn1 P1 C11 -26.21(16) . . . . ? P2 Mn1 P1 C11 -119.06(13) . . . . ? C20 Mn1 P2 C1 11.9(4) . . . . ? C10 Mn1 P2 C1 179.69(16) . . . . ? C40 Mn1 P2 C1 93.10(15) . . . . ? C30 Mn1 P2 C1 -92.60(15) . . . . ? P1 Mn1 P2 C1 2.08(11) . . . . ? C20 Mn1 P2 C31 -108.6(4) . . . . ? C10 Mn1 P2 C31 59.18(17) . . . . ? C40 Mn1 P2 C31 -27.41(16) . . . . ? C30 Mn1 P2 C31 146.89(16) . . . . ? P1 Mn1 P2 C31 -118.43(13) . . . . ? C20 Mn1 P2 C41 128.4(4) . . . . ? C10 Mn1 P2 C41 -63.80(17) . . . . ? C40 Mn1 P2 C41 -150.39(16) . . . . ? C30 Mn1 P2 C41 23.91(16) . . . . ? P1 Mn1 P2 C41 118.60(13) . . . . ? N2 Cu1 S2 C2 -175.20(15) . . . . ? C1 Cu1 S2 C2 -0.48(14) . . . . ? C2 S1 C1 P1 112.2(2) . . . . ? C2 S1 C1 P2 -118.0(2) . . . . ? C2 S1 C1 Cu1 -2.50(19) . . . . ? C21 P1 C1 S1 23.3(3) . . . . ? C11 P1 C1 S1 -90.7(2) . . . . ? Mn1 P1 C1 S1 143.15(19) . . . . ? C21 P1 C1 P2 -117.22(16) . . . . ? C11 P1 C1 P2 128.70(15) . . . . ? Mn1 P1 C1 P2 2.58(14) . . . . ? C21 P1 C1 Cu1 142.82(13) . . . . ? C11 P1 C1 Cu1 28.73(17) . . . . ? Mn1 P1 C1 Cu1 -97.38(10) . . . . ? C31 P2 C1 S1 -23.0(3) . . . . ? C41 P2 C1 S1 92.8(2) . . . . ? Mn1 P2 C1 S1 -141.9(2) . . . . ? C31 P2 C1 P1 116.36(16) . . . . ? C41 P2 C1 P1 -127.87(16) . . . . ? Mn1 P2 C1 P1 -2.56(14) . . . . ? C31 P2 C1 Cu1 -143.21(14) . . . . ? C41 P2 C1 Cu1 -27.43(17) . . . . ? Mn1 P2 C1 Cu1 97.87(10) . . . . ? N2 Cu1 C1 S1 175.00(15) . . . . ? S2 Cu1 C1 S1 1.82(15) . . . . ? N2 Cu1 C1 P1 45.6(2) . . . . ? S2 Cu1 C1 P1 -127.57(11) . . . . ? N2 Cu1 C1 P2 -53.4(2) . . . . ? S2 Cu1 C1 P2 133.40(11) . . . . ? C4 N1 C2 S2 178.0(3) . . . . ? C3 N1 C2 S2 -4.3(5) . . . . ? C4 N1 C2 S1 -2.6(4) . . . . ? C3 N1 C2 S1 175.1(3) . . . . ? Cu1 S2 C2 N1 178.3(3) . . . . ? Cu1 S2 C2 S1 -1.1(2) . . . . ? C1 S1 C2 N1 -176.9(2) . . . . ? C1 S1 C2 S2 2.5(3) . . . . ? C1 P1 C11 C16 -128.1(3) . . . . ? C21 P1 C11 C16 110.8(3) . . . . ? Mn1 P1 C11 C16 -18.1(3) . . . . ? C1 P1 C11 C12 47.9(3) . . . . ? C21 P1 C11 C12 -73.2(3) . . . . ? Mn1 P1 C11 C12 157.8(2) . . . . ? C16 C11 C12 C13 1.9(5) . . . . ? P1 C11 C12 C13 -174.2(3) . . . . ? C11 C12 C13 C14 0.2(5) . . . . ? C12 C13 C14 C15 -1.9(6) . . . . ? C13 C14 C15 C16 1.5(6) . . . . ? C12 C11 C16 C15 -2.2(5) . . . . ? P1 C11 C16 C15 173.6(3) . . . . ? C14 C15 C16 C11 0.5(6) . . . . ? C1 P1 C21 C22 -153.7(3) . . . . ? C11 P1 C21 C22 -35.6(3) . . . . ? Mn1 P1 C21 C22 97.6(3) . . . . ? C1 P1 C21 C26 31.6(3) . . . . ? C11 P1 C21 C26 149.7(3) . . . . ? Mn1 P1 C21 C26 -77.1(3) . . . . ? C26 C21 C22 C23 0.7(5) . . . . ? P1 C21 C22 C23 -174.2(3) . . . . ? C21 C22 C23 C24 -1.0(5) . . . . ? C22 C23 C24 C25 0.9(5) . . . . ? C23 C24 C25 C26 -0.4(5) . . . . ? C24 C25 C26 C21 0.1(5) . . . . ? C22 C21 C26 C25 -0.2(5) . . . . ? P1 C21 C26 C25 174.6(3) . . . . ? C1 P2 C31 C32 -16.7(3) . . . . ? C41 P2 C31 C32 -136.1(3) . . . . ? Mn1 P2 C31 C32 91.6(3) . . . . ? C1 P2 C31 C36 169.6(3) . . . . ? C41 P2 C31 C36 50.1(3) . . . . ? Mn1 P2 C31 C36 -82.2(3) . . . . ? C36 C31 C32 C33 0.7(5) . . . . ? P2 C31 C32 C33 -172.9(3) . . . . ? C31 C32 C33 C34 1.0(5) . . . . ? C32 C33 C34 C35 -1.6(6) . . . . ? C33 C34 C35 C36 0.5(7) . . . . ? C34 C35 C36 C31 1.1(7) . . . . ? C32 C31 C36 C35 -1.7(6) . . . . ? P2 C31 C36 C35 172.4(4) . . . . ? C1 P2 C41 C42 -46.0(3) . . . . ? C31 P2 C41 C42 77.3(3) . . . . ? Mn1 P2 C41 C42 -154.9(2) . . . . ? C1 P2 C41 C46 129.3(3) . . . . ? C31 P2 C41 C46 -107.3(3) . . . . ? Mn1 P2 C41 C46 20.4(3) . . . . ? C46 C41 C42 C43 -1.7(5) . . . . ? P2 C41 C42 C43 173.7(3) . . . . ? C41 C42 C43 C44 0.2(5) . . . . ? C42 C43 C44 C45 1.4(6) . . . . ? C43 C44 C45 C46 -1.4(6) . . . . ? C44 C45 C46 C41 -0.2(6) . . . . ? C42 C41 C46 C45 1.7(5) . . . . ? P2 C41 C46 C45 -173.7(3) . . . . ? loop_ _publ_manuscript_incl_extra_item '_geom_bond_atom_site_label_D' '_geom_bond_atom_site_label_H' '_geom_contact_atom_site_label_A' '_geom_bond_distance_DH' '_geom_contact_distance_HA' '_geom_contact_distance_DA' '_geom_angle_DHA' '_geom_contact_site_symmetry_A' loop_ _geom_bond_atom_site_label_d _geom_bond_atom_site_label_h _geom_contact_atom_site_label_a _geom_bond_distance_dh _geom_contact_distance_ha _geom_contact_distance_da _geom_angle_dha _geom_contact_site_symmetry_a C6 H6C F1 0.86(6) 3.492(5) 2.77(6) 143.(5) 1_555 C6 H6C F3 0.86(6) 3.318(6) 2.49(6) 163.(5) 1_555 C3 H3B S2 0.91(8) 3.027(4) 2.63(7) 107.(5) 1_555 C4 H4A S1 0.85(8) 2.900(4) 2.71(7) 94.(5) 1_555 C26 H26 S1 0.89(3) 3.392(3) 2.86(4) 120.(3) 1_555 C32 H32 S1 0.89(5) 3.423(4) 2.75(5) 133.(3) 1_555 C45 H45 F2 0.86(5) 3.667(5) 2.83(5) 162.(4) 1_555 C46 H46 O4 0.83(4) 3.378(4) 2.86(4) 122.(3) 1_555 C7 H7B S2 0.89(4) 3.774(4) 2.94(4) 156.(4) 1_555 C3 H3C F3 0.97(7) 3.056(6) 2.72(7) 101.(4) 1_545 C3 H3B F3 0.91(8) 3.056(6) 2.75(8) 101.(5) 1_545 C4 H4C O1 1.05(5) 3.400(5) 2.71(6) 123.(4) 1_545 C7 H7A F2 0.96(5) 3.409(6) 2.55(5) 149.(4) 1_545 C7 H7A F4 0.96(5) 3.027(6) 2.63(5) 106.(3) 1_545 C3 H3B F4 0.91(8) 3.395(6) 2.68(8) 136.(6) 1_545 C7 H7B F4 0.89(4) 3.027(6) 2.72(5) 102.(3) 1_545 C8 H8B F2 0.97(1) 3.18(1) 2.379(3) 139.(6) 2_665 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 68.61 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.151 _refine_diff_density_min -0.799 _refine_diff_density_rms 0.113 #==END #========================================================================== data_5a _database_code_CSD 210267 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C72 H72 Cu Mn2 N4 O6 P4 S4, 2(C H2 Cl2), 3(B F4)' _chemical_formula_sum 'C74 H76 B3 Cl4 Cu F12 Mn2 N4 O6 P4 S4' _chemical_formula_weight 1945.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1163(3) _cell_length_b 19.3279(8) _cell_length_c 21.7730(10) _cell_angle_alpha 69.660(3) _cell_angle_beta 79.268(3) _cell_angle_gamma 84.282(2) _cell_volume 4306.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15740 _cell_measurement_theta_min 3 _cell_measurement_theta_max 68 _exptl_crystal_description Prismatic _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.075 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.025 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.500 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1980 _exptl_absorpt_coefficient_mu 6.054 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.597 _exptl_absorpt_correction_T_max 0.860 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurement Sortav (Blessing 1995) ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15759 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1284 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 68.35 _reflns_number_total 15758 _reflns_number_gt 11111 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD control sofware (Nonius, 1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction ; 'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)' ; _computing_structure_solution 'DIRDIF-96 (Beurskens, 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0318P)^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 15758 _refine_ls_number_parameters 1224 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0695 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1438 _refine_ls_wR_factor_gt 0.1375 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.913 _refine_ls_shift/su_max 0.002 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.37966(5) 0.82760(3) 0.07035(3) 0.02535(13) Uani 1 d . . . Cu1 Cu 0.5000 0.5000 0.0000 0.0457(2) Uani 1 d S . . P1 P 0.42214(8) 0.79766(5) -0.02571(4) 0.02585(19) Uani 1 d . . . P2 P 0.39347(8) 0.70142(5) 0.10290(4) 0.02612(19) Uani 1 d . . . S1 S 0.25629(8) 0.66456(5) 0.01090(5) 0.03072(19) Uani 1 d . . . S2 S 0.44783(9) 0.59874(5) -0.07651(5) 0.0356(2) Uani 1 d . . . N1 N 0.1023(3) 0.82184(18) 0.06728(16) 0.0312(7) Uani 1 d . . . N2 N 0.2079(3) 0.61303(18) -0.07658(17) 0.0357(7) Uani 1 d . . . O1 O 0.6451(2) 0.83225(16) 0.07112(14) 0.0379(6) Uani 1 d . . . O2 O 0.3596(3) 0.82041(16) 0.21057(14) 0.0397(6) Uani 1 d . . . O3 O 0.3535(3) 0.99161(15) 0.01349(15) 0.0405(7) Uani 1 d . . . C10 C 0.5435(4) 0.8308(2) 0.06980(18) 0.0307(8) Uani 1 d . . . C20 C 0.3590(3) 0.8256(2) 0.1568(2) 0.0326(8) Uani 1 d . . . C30 C 0.3638(3) 0.9284(2) 0.03424(19) 0.0332(8) Uani 1 d . . . C1 C 0.3970(3) 0.6960(2) 0.01883(18) 0.0286(7) Uani 1 d . . . H1 H 0.448(4) 0.665(2) 0.007(2) 0.025(10) Uiso 1 d . . . C2 C 0.2991(3) 0.62227(19) -0.05062(18) 0.0301(8) Uani 1 d . . . C3 C 0.2228(5) 0.5693(3) -0.1215(3) 0.0500(11) Uani 1 d . . . H3A H 0.2454 0.6011 -0.1665 0.063(16) Uiso 1 calc R . . H3B H 0.1470 0.5469 -0.1171 0.08(2) Uiso 1 calc R . . H3C H 0.2857 0.5315 -0.1100 0.070(18) Uiso 1 calc R . . C4 C 0.0833(4) 0.6422(3) -0.0623(3) 0.0483(11) Uani 1 d . . . H4A H 0.0863 0.6919 -0.0629 0.053(14) Uiso 1 calc R . . H4B H 0.0447 0.6121 -0.0192 0.09(2) Uiso 1 calc R . . H4C H 0.0372 0.6417 -0.0953 0.059(15) Uiso 1 calc R . . C5 C 0.2049(3) 0.8228(2) 0.06971(17) 0.0293(8) Uani 1 d . . . C6 C -0.0291(3) 0.8236(2) 0.0644(2) 0.0329(8) Uani 1 d . . . C7 C -0.0443(4) 0.7784(3) 0.0220(3) 0.0445(10) Uani 1 d . . . H7A H -0.017(4) 0.729(3) 0.042(2) 0.038(12) Uiso 1 d . . . H7B H -0.003(5) 0.799(3) -0.018(3) 0.058(16) Uiso 1 d . . . H7C H -0.134(5) 0.781(3) 0.018(2) 0.042(12) Uiso 1 d . . . C8 C -0.0679(4) 0.9040(3) 0.0323(3) 0.0504(12) Uani 1 d . . . H8A H -0.1537 0.9075 0.0297 0.040(12) Uiso 1 calc R . . H8B H -0.0218 0.9231 -0.0115 0.08(2) Uiso 1 calc R . . H8C H -0.0528 0.9322 0.0585 0.08(2) Uiso 1 calc R . . C9 C -0.0936(4) 0.7898(3) 0.1348(2) 0.0500(12) Uani 1 d . . . H9A H -0.0639 0.7397 0.1529 0.039(12) Uiso 1 calc R . . H9B H -0.1802 0.7907 0.1352 0.038(11) Uiso 1 calc R . . H9C H -0.0776 0.8176 0.1612 0.078(19) Uiso 1 calc R . . C11 C 0.5798(3) 0.8091(2) -0.06921(17) 0.0302(8) Uani 1 d . . . C12 C 0.6523(3) 0.7542(2) -0.08809(19) 0.0321(8) Uani 1 d . . . H12 H 0.626(3) 0.709(2) -0.0795(18) 0.019(9) Uiso 1 d . . . C13 C 0.7732(4) 0.7689(2) -0.1207(2) 0.0393(9) Uani 1 d . . . H13 H 0.821(4) 0.726(3) -0.128(2) 0.038(12) Uiso 1 d . . . C14 C 0.8192(4) 0.8369(3) -0.1336(2) 0.0410(10) Uani 1 d . . . H14 H 0.894(6) 0.849(3) -0.156(3) 0.072(18) Uiso 1 d . . . C15 C 0.7484(4) 0.8921(2) -0.1153(2) 0.0400(9) Uani 1 d . . . H15 H 0.780(4) 0.939(3) -0.126(2) 0.032(11) Uiso 1 d . . . C16 C 0.6288(4) 0.8775(2) -0.08312(19) 0.0341(8) Uani 1 d . . . H16 H 0.585(4) 0.918(2) -0.0699(19) 0.024(9) Uiso 1 d . . . C21 C 0.3317(3) 0.8288(2) -0.09258(18) 0.0305(8) Uani 1 d . . . C22 C 0.2438(3) 0.8860(2) -0.09530(19) 0.0339(8) Uani 1 d . . . H22 H 0.2301 0.9076 -0.0624 0.037(11) Uiso 1 calc R . . C23 C 0.1766(4) 0.9106(3) -0.1471(2) 0.0446(10) Uani 1 d . . . H23 H 0.130(5) 0.956(3) -0.147(3) 0.053(14) Uiso 1 d . . . C24 C 0.1966(4) 0.8779(3) -0.1959(2) 0.0492(11) Uani 1 d . . . H24 H 0.153(5) 0.897(3) -0.230(3) 0.055(15) Uiso 1 d . . . C25 C 0.2833(4) 0.8216(3) -0.1935(2) 0.0443(10) Uani 1 d . . . H25 H 0.294(5) 0.799(3) -0.225(3) 0.046(13) Uiso 1 d . . . C26 C 0.3529(4) 0.7974(2) -0.14224(19) 0.0350(8) Uani 1 d . . . H26 H 0.401(4) 0.758(2) -0.1378(19) 0.022(9) Uiso 1 d . . . C31 C 0.5326(3) 0.6553(2) 0.13212(18) 0.0302(8) Uani 1 d . . . C32 C 0.6378(3) 0.6437(2) 0.09036(19) 0.0322(8) Uani 1 d . . . H32 H 0.6361 0.6552 0.0453 0.024(9) Uiso 1 calc R . . C33 C 0.7452(4) 0.6150(2) 0.1153(2) 0.0385(9) Uani 1 d . . . H33 H 0.814(5) 0.604(3) 0.084(2) 0.040(12) Uiso 1 d . . . C34 C 0.7492(4) 0.5986(2) 0.1821(2) 0.0441(10) Uani 1 d . . . H34 H 0.826(5) 0.576(3) 0.202(3) 0.058(15) Uiso 1 d . . . C35 C 0.6447(5) 0.6097(3) 0.2240(3) 0.0530(12) Uani 1 d . . . H35 H 0.643(7) 0.605(4) 0.270(4) 0.10(2) Uiso 1 d . . . C36 C 0.5370(4) 0.6379(3) 0.1995(2) 0.0452(10) Uani 1 d . . . H36 H 0.463(4) 0.650(2) 0.227(2) 0.037(11) Uiso 1 d . . . C41 C 0.2727(3) 0.6460(2) 0.16231(17) 0.0303(8) Uani 1 d . . . C42 C 0.1859(3) 0.6772(2) 0.20135(19) 0.0322(8) Uani 1 d . . . H42 H 0.185(3) 0.729(2) 0.1980(17) 0.017(8) Uiso 1 d . . . C43 C 0.0982(4) 0.6324(2) 0.2488(2) 0.0389(9) Uani 1 d . . . H43 H 0.0407 0.6525 0.2755 0.028(10) Uiso 1 calc R . . C44 C 0.0957(4) 0.5589(3) 0.2565(2) 0.0450(10) Uani 1 d . . . H44 H 0.032(5) 0.524(3) 0.287(3) 0.051(14) Uiso 1 d . . . C45 C 0.1803(4) 0.5287(3) 0.2177(2) 0.0455(10) Uani 1 d . . . H45 H 0.176(4) 0.476(3) 0.224(2) 0.043(12) Uiso 1 d . . . C46 C 0.2705(4) 0.5717(2) 0.1705(2) 0.0363(9) Uani 1 d . . . H46 H 0.326(4) 0.550(2) 0.146(2) 0.031(11) Uiso 1 d . . . Mn1' Mn 0.39718(5) 0.86129(3) -0.46957(3) 0.02675(14) Uani 1 d . . . Cu1' Cu 0.5000 0.5000 -0.5000 0.0553(3) Uani 1 d S . . P1' P 0.40439(8) 0.74540(5) -0.39121(5) 0.02789(19) Uani 1 d . . . P2' P 0.43800(8) 0.77806(5) -0.52698(4) 0.02698(19) Uani 1 d . . . S1' S 0.62782(8) 0.66777(5) -0.45291(5) 0.03111(19) Uani 1 d . . . S2' S 0.49256(9) 0.52366(5) -0.40879(5) 0.0389(2) Uani 1 d . . . N1' N 0.6794(3) 0.85950(18) -0.47896(17) 0.0350(7) Uani 1 d . . . N2' N 0.7330(3) 0.53678(18) -0.41960(17) 0.0348(7) Uani 1 d . . . O1' O 0.1324(2) 0.85537(17) -0.47087(16) 0.0442(7) Uani 1 d . . . O2' O 0.3338(3) 0.94170(18) -0.37236(16) 0.0471(7) Uani 1 d . . . O3' O 0.4088(3) 1.00276(15) -0.58276(15) 0.0420(7) Uani 1 d . . . C1' C 0.4693(3) 0.6973(2) -0.45240(18) 0.0290(8) Uani 1 d . . . H1' H 0.434(4) 0.666(2) -0.4507(19) 0.019(10) Uiso 1 d . . . C2' C 0.6251(4) 0.5703(2) -0.42633(19) 0.0325(8) Uani 1 d . . . C3' C 0.7495(5) 0.4565(2) -0.4024(3) 0.0479(11) Uani 1 d . . . H3'A H 0.734(5) 0.443(3) -0.439(3) 0.061(16) Uiso 1 d . . . H3'B H 0.822(6) 0.441(3) -0.390(3) 0.056(15) Uiso 1 d . . . H3'C H 0.689(6) 0.434(3) -0.367(3) 0.071(18) Uiso 1 d . . . C4' C 0.8454(4) 0.5787(3) -0.4373(2) 0.0442(10) Uani 1 d . . . H4'A H 0.8388 0.6104 -0.4112 0.044(13) Uiso 1 calc R . . H4'B H 0.8560 0.6080 -0.4836 0.051(14) Uiso 1 calc R . . H4'C H 0.9147 0.5449 -0.4286 0.10(2) Uiso 1 calc R . . C5' C 0.5750(4) 0.8608(2) -0.47422(19) 0.0324(8) Uani 1 d . . . C6' C 0.8139(3) 0.8556(2) -0.4832(2) 0.0397(9) Uani 1 d . . . C7' C 0.8535(4) 0.9323(2) -0.4949(3) 0.0474(11) Uani 1 d . . . H7'A H 0.8229 0.9460 -0.4563 0.044(13) Uiso 1 calc R . . H7'B H 0.8213 0.9667 -0.5325 0.076(19) Uiso 1 calc R . . H7'C H 0.9413 0.9330 -0.5035 0.056(14) Uiso 1 calc R . . C8' C 0.8695(4) 0.8294(3) -0.5407(3) 0.0601(14) Uani 1 d . . . H8'A H 0.9572 0.8290 -0.5460 0.035(11) Uiso 1 calc R . . H8'B H 0.8427 0.8623 -0.5806 0.057(16) Uiso 1 calc R . . H8'C H 0.8436 0.7805 -0.5320 0.072(18) Uiso 1 calc R . . C9' C 0.8422(5) 0.8005(3) -0.4177(3) 0.0650(16) Uani 1 d . . . H9'A H 0.8121 0.7532 -0.4114 0.066(17) Uiso 1 calc R . . H9'B H 0.8031 0.8173 -0.3820 0.09(2) Uiso 1 calc R . . H9'C H 0.9292 0.7961 -0.4184 0.11(3) Uiso 1 calc R . . C10' C 0.2341(4) 0.8573(2) -0.46975(18) 0.0323(8) Uani 1 d . . . C20' C 0.3623(4) 0.9104(2) -0.4095(2) 0.0370(9) Uani 1 d . . . C30' C 0.4053(3) 0.9476(2) -0.5409(2) 0.0342(8) Uani 1 d . . . C11' C 0.2610(3) 0.7021(2) -0.34537(18) 0.0329(8) Uani 1 d . . . C12' C 0.1754(4) 0.7444(2) -0.3168(2) 0.0376(9) Uani 1 d . . . H12' H 0.187(3) 0.799(2) -0.3232(18) 0.020(9) Uiso 1 d . . . C13' C 0.0674(4) 0.7125(3) -0.2774(2) 0.0469(11) Uani 1 d . . . H13' H 0.010(5) 0.741(3) -0.255(3) 0.059(15) Uiso 1 d . . . C14' C 0.0455(4) 0.6399(3) -0.2670(2) 0.0504(11) Uani 1 d . . . H14' H -0.035(5) 0.619(3) -0.244(3) 0.050(13) Uiso 1 d . . . C15' C 0.1301(5) 0.5985(3) -0.2956(2) 0.0479(11) Uani 1 d . . . H15' H 0.120(4) 0.551(3) -0.292(2) 0.035(11) Uiso 1 d . . . C16' C 0.2387(4) 0.6289(2) -0.3341(2) 0.0397(9) Uani 1 d . . . H16' H 0.293(4) 0.600(3) -0.355(2) 0.041(12) Uiso 1 d . . . C21' C 0.5008(3) 0.7222(2) -0.32736(19) 0.0337(8) Uani 1 d . . . C22' C 0.5490(4) 0.7776(3) -0.3131(2) 0.0409(9) Uani 1 d . . . H22' H 0.5343 0.8270 -0.3370 0.042(12) Uiso 1 calc R . . C23' C 0.6193(4) 0.7582(3) -0.2627(2) 0.0486(11) Uani 1 d . . . H23' H 0.6507 0.7950 -0.2524 0.051(14) Uiso 1 calc R . . C24' C 0.6427(4) 0.6858(3) -0.2281(2) 0.0519(12) Uani 1 d . . . H24' H 0.6920 0.6736 -0.1954 0.08(2) Uiso 1 calc R . . C25' C 0.5943(5) 0.6307(3) -0.2412(2) 0.0502(12) Uani 1 d . . . H25' H 0.603(5) 0.582(3) -0.220(3) 0.061(16) Uiso 1 d . . . C26' C 0.5226(4) 0.6485(2) -0.2915(2) 0.0416(10) Uani 1 d . . . H26' H 0.487(3) 0.608(2) -0.2975(18) 0.017(9) Uiso 1 d . . . C31' C 0.3131(3) 0.7508(2) -0.55591(19) 0.0309(8) Uani 1 d . . . C32' C 0.2957(4) 0.7850(3) -0.6209(2) 0.0499(11) Uani 1 d . . . H32' H 0.340(4) 0.826(3) -0.651(2) 0.039(12) Uiso 1 d . . . C33' C 0.1963(5) 0.7703(3) -0.6436(2) 0.0554(13) Uani 1 d . . . H33' H 0.1858 0.7946 -0.6874 0.074(18) Uiso 1 calc R . . C34' C 0.1132(4) 0.7201(3) -0.6018(2) 0.0422(10) Uani 1 d . . . H34' H 0.0466 0.7100 -0.6172 0.047(13) Uiso 1 calc R . . C35' C 0.1291(4) 0.6847(2) -0.5370(2) 0.0453(10) Uani 1 d . . . H35' H 0.0728 0.6506 -0.5084 0.053(14) Uiso 1 calc R . . C36' C 0.2286(4) 0.6995(2) -0.5141(2) 0.0389(9) Uani 1 d . . . H36' H 0.2389 0.6749 -0.4702 0.045(13) Uiso 1 calc R . . C41' C 0.5653(3) 0.7895(2) -0.59437(19) 0.0327(8) Uani 1 d . . . C42' C 0.6143(4) 0.8585(2) -0.6282(2) 0.0362(9) Uani 1 d . . . H42' H 0.584(4) 0.898(2) -0.615(2) 0.030(10) Uiso 1 d . . . C43' C 0.7105(4) 0.8679(3) -0.6808(2) 0.0489(11) Uani 1 d . . . H43' H 0.728(5) 0.916(3) -0.701(3) 0.052(14) Uiso 1 d . . . C44' C 0.7598(5) 0.8081(3) -0.6984(2) 0.0534(12) Uani 1 d . . . H44' H 0.832(6) 0.817(3) -0.732(3) 0.065(16) Uiso 1 d . . . C45' C 0.7115(5) 0.7390(3) -0.6660(2) 0.0513(11) Uani 1 d . . . H45' H 0.732(5) 0.696(3) -0.683(2) 0.048(13) Uiso 1 d . . . C46' C 0.6131(4) 0.7296(2) -0.6144(2) 0.0404(9) Uani 1 d . . . H46' H 0.582(5) 0.679(3) -0.593(2) 0.045(13) Uiso 1 d . . . Cl1 Cl 0.15593(16) 0.95510(9) 0.37056(8) 0.0763(4) Uani 1 d . . . Cl2 Cl 0.0166(2) 1.09320(11) 0.33356(10) 0.1026(7) Uani 1 d . . . C40 C 0.1121(8) 1.0286(4) 0.3061(3) 0.0810(19) Uani 1 d . . . H40A H 0.0695 1.0105 0.2800 0.097 Uiso 1 calc R . . H40B H 0.1846 1.0527 0.2775 0.097 Uiso 1 calc R . . Cl3 Cl 0.56864(12) 0.95629(7) 0.15397(6) 0.0558(3) Uani 1 d . . . Cl4 Cl 0.48919(16) 1.03720(8) 0.24650(7) 0.0705(4) Uani 1 d . . . C50 C 0.4640(5) 0.9611(3) 0.2241(3) 0.0545(12) Uani 1 d . . . H50A H 0.486(5) 0.917(3) 0.262(3) 0.067(17) Uiso 1 d . . . H50B H 0.372(5) 0.964(3) 0.215(3) 0.055(14) Uiso 1 d . . . F1 F 0.0959(3) 0.50504(16) 0.06730(18) 0.0705(9) Uani 1 d . . . F2 F 0.2047(3) 0.42283(19) 0.02354(14) 0.0690(8) Uani 1 d . . . F3 F 0.1370(2) 0.38975(14) 0.13353(12) 0.0491(6) Uani 1 d . . . F4 F 0.2892(2) 0.46955(15) 0.08683(15) 0.0541(7) Uani 1 d . . . B1 B 0.1807(4) 0.4472(3) 0.0770(2) 0.0370(10) Uani 1 d . . . F5 F 0.0763(2) 0.84502(13) 0.21565(13) 0.0457(6) Uani 1 d . . . F6 F 0.0732(3) 0.95637(16) 0.13365(14) 0.0634(8) Uani 1 d . . . F7 F -0.0255(2) 0.94377(16) 0.23774(15) 0.0564(7) Uani 1 d . . . F8 F 0.1815(2) 0.93948(14) 0.21608(14) 0.0484(6) Uani 1 d . . . B2 B 0.0756(4) 0.9204(3) 0.2004(2) 0.0361(10) Uani 1 d . . . F9 F 0.8597(3) 0.46656(15) 0.42301(17) 0.0657(8) Uani 1 d . . . F10 F 0.9274(2) 0.57824(18) 0.40602(15) 0.0589(7) Uani 1 d . . . F11 F 0.8128(3) 0.56331(17) 0.33661(13) 0.0552(7) Uani 1 d . . . F12 F 0.7255(2) 0.55669(15) 0.44083(13) 0.0488(6) Uani 1 d . . . B3 B 0.8320(4) 0.5408(2) 0.4019(2) 0.0332(9) Uani 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 0.0226(3) 0.0235(3) 0.0306(3) -0.0084(2) -0.0070(2) -0.0013(2) Cu1 0.0531(5) 0.0342(5) 0.0556(6) -0.0177(4) -0.0250(4) 0.0121(4) P1 0.0254(4) 0.0250(4) 0.0266(4) -0.0063(3) -0.0073(3) -0.0012(3) P2 0.0259(4) 0.0236(4) 0.0284(4) -0.0067(3) -0.0070(3) -0.0015(3) S1 0.0265(4) 0.0333(5) 0.0357(5) -0.0143(4) -0.0068(3) -0.0034(3) S2 0.0340(5) 0.0339(5) 0.0401(5) -0.0149(4) -0.0048(4) 0.0003(4) N1 0.0188(15) 0.0379(17) 0.0371(17) -0.0116(14) -0.0067(12) -0.0014(12) N2 0.0363(18) 0.0349(17) 0.0413(18) -0.0160(14) -0.0138(14) -0.0006(14) O1 0.0226(13) 0.0434(16) 0.0485(16) -0.0128(13) -0.0115(11) -0.0030(11) O2 0.0400(15) 0.0492(17) 0.0320(15) -0.0156(12) -0.0049(11) -0.0055(13) O3 0.0419(16) 0.0249(15) 0.0524(17) -0.0098(12) -0.0088(13) -0.0009(11) C10 0.040(2) 0.0243(17) 0.0267(18) -0.0064(14) -0.0081(15) 0.0014(15) C20 0.0250(18) 0.0270(19) 0.045(2) -0.0110(16) -0.0059(15) -0.0021(14) C30 0.0270(18) 0.040(2) 0.037(2) -0.0165(17) -0.0093(15) -0.0047(16) C1 0.0277(18) 0.0268(18) 0.0317(19) -0.0086(15) -0.0096(14) 0.0018(15) C2 0.0336(19) 0.0225(17) 0.0323(19) -0.0043(14) -0.0087(15) -0.0037(14) C3 0.054(3) 0.054(3) 0.056(3) -0.032(2) -0.019(2) 0.000(2) C4 0.035(2) 0.058(3) 0.061(3) -0.025(2) -0.022(2) 0.003(2) C5 0.035(2) 0.0273(18) 0.0254(17) -0.0080(14) -0.0051(14) -0.0014(14) C6 0.0188(17) 0.038(2) 0.043(2) -0.0129(17) -0.0078(15) -0.0020(14) C7 0.034(2) 0.053(3) 0.052(3) -0.023(2) -0.010(2) -0.002(2) C8 0.029(2) 0.043(2) 0.081(4) -0.019(2) -0.017(2) -0.0003(18) C9 0.031(2) 0.079(4) 0.041(2) -0.019(2) -0.0054(18) -0.012(2) C11 0.0348(19) 0.0289(18) 0.0246(17) -0.0038(14) -0.0096(14) -0.0011(15) C12 0.0280(19) 0.032(2) 0.036(2) -0.0085(16) -0.0083(15) -0.0021(15) C13 0.033(2) 0.043(2) 0.037(2) -0.0103(18) -0.0032(16) 0.0032(18) C14 0.029(2) 0.051(3) 0.037(2) -0.0076(18) -0.0035(17) -0.0049(18) C15 0.038(2) 0.035(2) 0.043(2) -0.0065(18) -0.0036(17) -0.0112(18) C16 0.035(2) 0.030(2) 0.033(2) -0.0066(16) -0.0042(16) -0.0016(16) C21 0.0260(17) 0.0310(19) 0.0305(18) -0.0031(15) -0.0075(14) -0.0031(14) C22 0.0320(19) 0.034(2) 0.0327(19) -0.0064(16) -0.0068(15) -0.0004(15) C23 0.033(2) 0.049(3) 0.043(2) -0.0018(19) -0.0150(18) 0.0053(19) C24 0.043(2) 0.065(3) 0.033(2) -0.002(2) -0.0188(19) -0.002(2) C25 0.048(3) 0.055(3) 0.032(2) -0.013(2) -0.0121(18) -0.005(2) C26 0.039(2) 0.033(2) 0.033(2) -0.0091(16) -0.0115(16) 0.0006(18) C31 0.0325(19) 0.0249(18) 0.0324(19) -0.0070(14) -0.0080(15) -0.0023(14) C32 0.0314(19) 0.0318(19) 0.032(2) -0.0074(15) -0.0099(15) 0.0002(15) C33 0.030(2) 0.037(2) 0.048(2) -0.0129(18) -0.0104(18) 0.0029(16) C34 0.037(2) 0.039(2) 0.053(3) -0.0040(19) -0.023(2) 0.0007(18) C35 0.050(3) 0.066(3) 0.040(3) -0.011(2) -0.020(2) 0.005(2) C36 0.036(2) 0.066(3) 0.032(2) -0.012(2) -0.0122(17) 0.003(2) C41 0.0333(19) 0.0318(19) 0.0242(17) -0.0047(14) -0.0089(14) -0.0031(15) C42 0.0308(19) 0.032(2) 0.0322(19) -0.0078(15) -0.0071(15) -0.0029(15) C43 0.036(2) 0.044(2) 0.034(2) -0.0117(17) -0.0010(16) -0.0047(17) C44 0.041(2) 0.044(2) 0.043(2) -0.0046(19) -0.0036(19) -0.0144(19) C45 0.047(3) 0.033(2) 0.051(3) -0.0090(19) -0.002(2) -0.0108(19) C46 0.038(2) 0.0272(19) 0.041(2) -0.0093(17) -0.0013(17) -0.0034(16) Mn1' 0.0225(3) 0.0256(3) 0.0328(3) -0.0099(2) -0.0065(2) 0.0005(2) Cu1' 0.0716(7) 0.0375(5) 0.0736(7) -0.0265(5) -0.0437(6) 0.0098(4) P1' 0.0253(4) 0.0277(4) 0.0298(5) -0.0083(4) -0.0057(3) 0.0006(3) P2' 0.0257(4) 0.0243(4) 0.0294(4) -0.0070(3) -0.0048(3) -0.0011(3) S1' 0.0260(4) 0.0266(4) 0.0398(5) -0.0099(4) -0.0063(3) 0.0002(3) S2' 0.0330(5) 0.0282(5) 0.0541(6) -0.0123(4) -0.0058(4) -0.0032(4) N1' 0.0215(16) 0.0385(18) 0.0477(19) -0.0167(15) -0.0076(13) -0.0029(13) N2' 0.0337(17) 0.0308(16) 0.0405(18) -0.0114(14) -0.0112(14) 0.0042(13) O1' 0.0231(14) 0.0517(18) 0.0567(18) -0.0159(14) -0.0102(12) 0.0017(12) O2' 0.0443(17) 0.0535(18) 0.0530(18) -0.0319(16) -0.0079(14) 0.0056(14) O3' 0.0434(16) 0.0276(14) 0.0478(17) -0.0050(13) -0.0049(13) -0.0014(12) C1' 0.0286(19) 0.0238(18) 0.033(2) -0.0053(15) -0.0071(15) -0.0066(15) C2' 0.034(2) 0.035(2) 0.0312(19) -0.0130(15) -0.0110(15) 0.0008(16) C3' 0.044(3) 0.030(2) 0.068(3) -0.013(2) -0.016(2) 0.0075(19) C4' 0.028(2) 0.045(2) 0.063(3) -0.020(2) -0.0155(19) 0.0040(17) C5' 0.038(2) 0.0264(18) 0.036(2) -0.0124(15) -0.0089(16) -0.0013(15) C6' 0.0201(18) 0.037(2) 0.062(3) -0.0159(19) -0.0075(17) 0.0011(15) C7' 0.034(2) 0.038(2) 0.072(3) -0.021(2) -0.013(2) -0.0003(18) C8' 0.030(2) 0.074(4) 0.091(4) -0.048(3) -0.003(2) -0.003(2) C9' 0.037(3) 0.055(3) 0.085(4) 0.005(3) -0.019(3) -0.007(2) C10' 0.038(2) 0.0274(18) 0.0306(19) -0.0090(15) -0.0074(15) 0.0040(15) C20' 0.031(2) 0.032(2) 0.048(2) -0.0120(18) -0.0102(17) 0.0001(16) C30' 0.0259(18) 0.032(2) 0.045(2) -0.0145(18) -0.0074(16) 0.0048(15) C11' 0.0313(19) 0.035(2) 0.0293(19) -0.0081(15) -0.0032(15) -0.0001(15) C12' 0.036(2) 0.040(2) 0.036(2) -0.0127(17) -0.0050(16) -0.0009(17) C13' 0.032(2) 0.065(3) 0.044(2) -0.024(2) 0.0037(18) -0.002(2) C14' 0.039(2) 0.064(3) 0.045(3) -0.017(2) 0.0068(19) -0.014(2) C15' 0.051(3) 0.048(3) 0.045(2) -0.016(2) 0.000(2) -0.018(2) C16' 0.042(2) 0.039(2) 0.035(2) -0.0113(17) 0.0009(17) -0.0054(18) C21' 0.0270(18) 0.042(2) 0.0308(19) -0.0131(16) -0.0032(14) 0.0035(15) C22' 0.036(2) 0.050(3) 0.040(2) -0.0186(19) -0.0093(17) -0.0003(18) C23' 0.040(2) 0.070(3) 0.044(2) -0.025(2) -0.0153(19) -0.004(2) C24' 0.042(2) 0.077(3) 0.036(2) -0.018(2) -0.0120(19) 0.007(2) C25' 0.049(3) 0.057(3) 0.037(2) -0.007(2) -0.0129(19) 0.014(2) C26' 0.045(2) 0.038(2) 0.038(2) -0.0099(18) -0.0070(18) 0.0056(18) C31' 0.0322(19) 0.0290(18) 0.0328(19) -0.0115(15) -0.0082(15) 0.0022(15) C32' 0.044(3) 0.061(3) 0.037(2) -0.002(2) -0.0096(19) -0.015(2) C33' 0.047(3) 0.081(4) 0.036(2) -0.011(2) -0.016(2) -0.009(2) C34' 0.031(2) 0.053(3) 0.050(2) -0.024(2) -0.0135(18) 0.0019(18) C35' 0.036(2) 0.040(2) 0.056(3) -0.006(2) -0.0145(19) -0.0090(18) C36' 0.036(2) 0.040(2) 0.038(2) -0.0041(17) -0.0157(17) -0.0065(17) C41' 0.0315(19) 0.0321(19) 0.0332(19) -0.0078(15) -0.0095(15) 0.0003(15) C42' 0.035(2) 0.031(2) 0.040(2) -0.0109(17) -0.0022(16) -0.0026(16) C43' 0.047(3) 0.049(3) 0.043(2) -0.009(2) 0.005(2) -0.014(2) C44' 0.048(3) 0.065(3) 0.044(3) -0.022(2) 0.006(2) 0.002(2) C45' 0.055(3) 0.049(3) 0.046(3) -0.018(2) 0.002(2) 0.007(2) C46' 0.045(2) 0.037(2) 0.037(2) -0.0128(18) -0.0030(17) 0.0032(18) Cl1 0.0897(11) 0.0682(9) 0.0709(9) -0.0187(7) -0.0265(8) 0.0057(8) Cl2 0.1318(16) 0.1071(13) 0.1037(13) -0.0735(11) -0.0694(12) 0.0713(12) C40 0.114(5) 0.069(4) 0.068(4) -0.036(3) -0.024(4) 0.030(4) Cl3 0.0574(7) 0.0501(6) 0.0587(7) -0.0169(5) -0.0050(5) -0.0111(5) Cl4 0.0983(11) 0.0642(8) 0.0532(7) -0.0227(6) -0.0058(7) -0.0241(7) C50 0.057(3) 0.054(3) 0.052(3) -0.014(2) -0.007(2) -0.015(2) F1 0.0555(17) 0.0521(17) 0.097(2) -0.0129(16) -0.0272(16) 0.0139(14) F2 0.082(2) 0.089(2) 0.0426(15) -0.0298(15) -0.0029(14) -0.0167(18) F3 0.0536(15) 0.0478(14) 0.0419(13) -0.0088(11) -0.0053(11) -0.0111(12) F4 0.0349(13) 0.0545(16) 0.0805(19) -0.0334(14) -0.0047(12) -0.0061(11) B1 0.040(2) 0.036(2) 0.039(2) -0.0144(19) -0.0106(19) -0.0011(19) F5 0.0499(14) 0.0353(12) 0.0559(15) -0.0137(11) -0.0207(12) -0.0031(10) F6 0.090(2) 0.0540(17) 0.0450(15) -0.0096(13) -0.0215(15) -0.0054(15) F7 0.0392(14) 0.0596(17) 0.0694(18) -0.0233(14) -0.0058(12) 0.0040(12) F8 0.0394(13) 0.0433(14) 0.0683(17) -0.0222(12) -0.0144(12) -0.0048(10) B2 0.038(2) 0.034(2) 0.039(2) -0.0120(19) -0.0105(19) -0.0015(18) F9 0.070(2) 0.0404(15) 0.080(2) -0.0105(14) -0.0220(16) 0.0097(13) F10 0.0372(14) 0.084(2) 0.0642(17) -0.0328(15) -0.0041(12) -0.0187(13) F11 0.0517(15) 0.0751(19) 0.0406(14) -0.0213(13) -0.0185(12) 0.0171(13) F12 0.0391(13) 0.0631(16) 0.0488(14) -0.0269(12) -0.0002(11) -0.0059(12) B3 0.028(2) 0.033(2) 0.037(2) -0.0098(18) -0.0047(17) -0.0017(17) _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 C10 1.826(4) . ? Mn1 C30 1.834(4) . ? Mn1 C20 1.840(4) . ? Mn1 C5 1.957(4) . ? Mn1 P2 2.2887(10) . ? Mn1 P1 2.3135(11) . ? Cu1 S2 2.1639(10) 2_665 ? Cu1 S2 2.1640(10) . ? P1 C21 1.819(4) . ? P1 C11 1.825(4) . ? P1 C1 1.888(4) . ? P2 C31 1.813(4) . ? P2 C41 1.817(4) . ? P2 C1 1.863(4) . ? S1 C2 1.771(4) . ? S1 C1 1.791(4) . ? S2 C2 1.714(4) . ? N1 C5 1.154(5) . ? N1 C6 1.470(4) . ? N2 C2 1.304(5) . ? N2 C4 1.463(6) . ? N2 C3 1.478(6) . ? O1 C10 1.139(5) . ? O2 C20 1.141(5) . ? O3 C30 1.148(5) . ? C1 H1 0.86(4) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C6 C9 1.509(6) . ? C6 C7 1.515(6) . ? C6 C8 1.521(6) . ? C7 H7A 0.94(5) . ? C7 H7B 0.89(6) . ? C7 H7C 1.01(5) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C11 C16 1.392(5) . ? C11 C12 1.396(6) . ? C12 C13 1.403(6) . ? C12 H12 0.90(4) . ? C13 C14 1.376(7) . ? C13 H13 0.98(5) . ? C14 C15 1.389(7) . ? C14 H14 0.89(7) . ? C15 C16 1.389(6) . ? C15 H15 0.94(5) . ? C16 H16 0.98(4) . ? C21 C26 1.388(6) . ? C21 C22 1.393(6) . ? C22 C23 1.388(6) . ? C22 H22 0.9300 . ? C23 C24 1.388(7) . ? C23 H23 0.97(6) . ? C24 C25 1.372(7) . ? C24 H24 0.91(6) . ? C25 C26 1.396(6) . ? C25 H25 0.93(5) . ? C26 H26 0.88(4) . ? C31 C32 1.393(6) . ? C31 C36 1.396(6) . ? C32 C33 1.389(5) . ? C32 H32 0.9300 . ? C33 C34 1.386(7) . ? C33 H33 0.98(5) . ? C34 C35 1.384(7) . ? C34 H34 1.02(6) . ? C35 C36 1.386(6) . ? C35 H35 0.98(8) . ? C36 H36 0.97(5) . ? C41 C46 1.386(6) . ? C41 C42 1.397(6) . ? C42 C43 1.392(5) . ? C42 H42 0.97(4) . ? C43 C44 1.374(6) . ? C43 H43 0.9300 . ? C44 C45 1.370(7) . ? C44 H44 1.00(5) . ? C45 C46 1.393(6) . ? C45 H45 0.99(5) . ? C46 H46 0.91(5) . ? Mn1' C10' 1.823(4) . ? Mn1' C20' 1.835(4) . ? Mn1' C30' 1.838(4) . ? Mn1' C5' 1.960(4) . ? Mn1' P1' 2.3007(10) . ? Mn1' P2' 2.3234(11) . ? Cu1' S2' 2.1731(11) 2_664 ? Cu1' S2' 2.1732(11) . ? P1' C21' 1.818(4) . ? P1' C11' 1.825(4) . ? P1' C1' 1.879(4) . ? P2' C41' 1.808(4) . ? P2' C31' 1.818(4) . ? P2' C1' 1.880(4) . ? S1' C2' 1.769(4) . ? S1' C1' 1.797(4) . ? S2' C2' 1.716(4) . ? N1' C5' 1.144(5) . ? N1' C6' 1.477(5) . ? N2' C2' 1.314(5) . ? N2' C3' 1.465(6) . ? N2' C4' 1.473(5) . ? O1' C10' 1.140(5) . ? O2' C20' 1.151(5) . ? O3' C30' 1.135(5) . ? C1' H1' 0.75(4) . ? C3' H3'A 0.97(6) . ? C3' H3'B 0.89(6) . ? C3' H3'C 0.93(7) . ? C4' H4'A 0.9600 . ? C4' H4'B 0.9600 . ? C4' H4'C 0.9600 . ? C6' C7' 1.511(6) . ? C6' C8' 1.516(7) . ? C6' C9' 1.519(7) . ? C7' H7'A 0.9600 . ? C7' H7'B 0.9600 . ? C7' H7'C 0.9600 . ? C8' H8'A 0.9600 . ? C8' H8'B 0.9600 . ? C8' H8'C 0.9600 . ? C9' H9'A 0.9600 . ? C9' H9'B 0.9600 . ? C9' H9'C 0.9600 . ? C11' C16' 1.388(6) . ? C11' C12' 1.392(6) . ? C12' C13' 1.397(6) . ? C12' H12' 1.03(4) . ? C13' C14' 1.380(7) . ? C13' H13' 0.98(6) . ? C14' C15' 1.375(7) . ? C14' H14' 0.99(5) . ? C15' C16' 1.389(6) . ? C15' H15' 0.92(5) . ? C16' H16' 0.95(5) . ? C21' C26' 1.388(6) . ? C21' C22' 1.393(6) . ? C22' C23' 1.389(6) . ? C22' H22' 0.9300 . ? C23' C24' 1.365(7) . ? C23' H23' 0.9300 . ? C24' C25' 1.374(8) . ? C24' H24' 0.9300 . ? C25' C26' 1.400(6) . ? C25' H25' 0.90(6) . ? C26' H26' 0.98(4) . ? C31' C32' 1.380(6) . ? C31' C36' 1.391(6) . ? C32' C33' 1.381(6) . ? C32' H32' 0.95(5) . ? C33' C34' 1.369(7) . ? C33' H33' 0.9300 . ? C34' C35' 1.375(6) . ? C34' H34' 0.9300 . ? C35' C36' 1.387(6) . ? C35' H35' 0.9300 . ? C36' H36' 0.9300 . ? C41' C42' 1.390(6) . ? C41' C46' 1.399(6) . ? C42' C43' 1.388(6) . ? C42' H42' 0.92(5) . ? C43' C44' 1.374(8) . ? C43' H43' 0.90(5) . ? C44' C45' 1.383(8) . ? C44' H44' 0.96(6) . ? C45' C46' 1.390(6) . ? C45' H45' 1.01(5) . ? C46' H46' 0.98(5) . ? Cl1 C40 1.720(6) . ? Cl2 C40 1.750(6) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? Cl3 C50 1.763(6) . ? Cl4 C50 1.765(6) . ? C50 H50A 1.01(6) . ? C50 H50B 1.07(6) . ? F1 B1 1.372(6) . ? F2 B1 1.375(6) . ? F3 B1 1.384(5) . ? F4 B1 1.397(5) . ? F5 B2 1.377(5) . ? F6 B2 1.380(5) . ? F7 B2 1.393(6) . ? F8 B2 1.401(5) . ? F9 B3 1.369(5) . ? F10 B3 1.375(5) . ? F11 B3 1.386(5) . ? F12 B3 1.396(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 Mn1 C30 92.24(16) . . ? C10 Mn1 C20 86.11(16) . . ? C30 Mn1 C20 95.15(17) . . ? C10 Mn1 C5 178.74(16) . . ? C30 Mn1 C5 88.41(16) . . ? C20 Mn1 C5 94.91(16) . . ? C10 Mn1 P2 90.77(12) . . ? C30 Mn1 P2 172.60(12) . . ? C20 Mn1 P2 91.80(12) . . ? C5 Mn1 P2 88.45(11) . . ? C10 Mn1 P1 90.08(12) . . ? C30 Mn1 P1 99.81(13) . . ? C20 Mn1 P1 164.69(12) . . ? C5 Mn1 P1 88.75(11) . . ? P2 Mn1 P1 73.42(4) . . ? S2 Cu1 S2 180.0 2_665 . ? C21 P1 C11 103.51(16) . . ? C21 P1 C1 107.68(16) . . ? C11 P1 C1 108.66(17) . . ? C21 P1 Mn1 125.22(13) . . ? C11 P1 Mn1 116.05(13) . . ? C1 P1 Mn1 94.32(12) . . ? C31 P2 C41 103.50(17) . . ? C31 P2 C1 107.36(18) . . ? C41 P2 C1 110.69(17) . . ? C31 P2 Mn1 117.79(12) . . ? C41 P2 Mn1 120.87(13) . . ? C1 P2 Mn1 95.84(12) . . ? C2 S1 C1 104.37(18) . . ? C2 S2 Cu1 107.40(12) . . ? C5 N1 C6 177.7(4) . . ? C2 N2 C4 123.5(4) . . ? C2 N2 C3 121.7(4) . . ? C4 N2 C3 114.8(3) . . ? O1 C10 Mn1 178.3(3) . . ? O2 C20 Mn1 172.0(3) . . ? O3 C30 Mn1 178.0(4) . . ? S1 C1 P2 112.1(2) . . ? S1 C1 P1 114.92(19) . . ? P2 C1 P1 94.35(18) . . ? S1 C1 H1 100(3) . . ? P2 C1 H1 118(3) . . ? P1 C1 H1 118(3) . . ? N2 C2 S2 122.6(3) . . ? N2 C2 S1 114.1(3) . . ? S2 C2 S1 123.3(2) . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 Mn1 177.7(3) . . ? N1 C6 C9 106.9(3) . . ? N1 C6 C7 107.3(3) . . ? C9 C6 C7 111.4(4) . . ? N1 C6 C8 107.0(3) . . ? C9 C6 C8 113.2(4) . . ? C7 C6 C8 110.8(4) . . ? C6 C7 H7A 110(3) . . ? C6 C7 H7B 109(4) . . ? H7A C7 H7B 112(5) . . ? C6 C7 H7C 108(3) . . ? H7A C7 H7C 111(4) . . ? H7B C7 H7C 108(5) . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C16 C11 C12 119.4(4) . . ? C16 C11 P1 116.2(3) . . ? C12 C11 P1 124.4(3) . . ? C11 C12 C13 119.6(4) . . ? C11 C12 H12 123(2) . . ? C13 C12 H12 118(2) . . ? C14 C13 C12 119.8(4) . . ? C14 C13 H13 125(3) . . ? C12 C13 H13 115(3) . . ? C13 C14 C15 121.4(4) . . ? C13 C14 H14 122(4) . . ? C15 C14 H14 116(4) . . ? C14 C15 C16 118.6(4) . . ? C14 C15 H15 120(3) . . ? C16 C15 H15 121(3) . . ? C15 C16 C11 121.2(4) . . ? C15 C16 H16 115(2) . . ? C11 C16 H16 124(2) . . ? C26 C21 C22 119.8(4) . . ? C26 C21 P1 120.1(3) . . ? C22 C21 P1 120.1(3) . . ? C23 C22 C21 119.9(4) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 120.0(4) . . ? C22 C23 H23 111(3) . . ? C24 C23 H23 128(3) . . ? C25 C24 C23 120.3(4) . . ? C25 C24 H24 122(4) . . ? C23 C24 H24 118(4) . . ? C24 C25 C26 120.1(5) . . ? C24 C25 H25 120(3) . . ? C26 C25 H25 120(3) . . ? C21 C26 C25 119.8(4) . . ? C21 C26 H26 120(3) . . ? C25 C26 H26 120(3) . . ? C32 C31 C36 118.9(4) . . ? C32 C31 P2 123.7(3) . . ? C36 C31 P2 117.1(3) . . ? C33 C32 C31 120.6(4) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C34 C33 C32 120.1(4) . . ? C34 C33 H33 124(3) . . ? C32 C33 H33 116(3) . . ? C35 C34 C33 119.5(4) . . ? C35 C34 H34 119(3) . . ? C33 C34 H34 121(3) . . ? C34 C35 C36 120.7(4) . . ? C34 C35 H35 124(5) . . ? C36 C35 H35 115(5) . . ? C35 C36 C31 120.2(4) . . ? C35 C36 H36 123(3) . . ? C31 C36 H36 117(3) . . ? C46 C41 C42 120.3(3) . . ? C46 C41 P2 119.3(3) . . ? C42 C41 P2 120.3(3) . . ? C43 C42 C41 119.0(4) . . ? C43 C42 H42 118(2) . . ? C41 C42 H42 123(2) . . ? C44 C43 C42 120.6(4) . . ? C44 C43 H43 119.7 . . ? C42 C43 H43 119.7 . . ? C45 C44 C43 120.2(4) . . ? C45 C44 H44 115(3) . . ? C43 C44 H44 125(3) . . ? C44 C45 C46 120.6(4) . . ? C44 C45 H45 119(3) . . ? C46 C45 H45 121(3) . . ? C41 C46 C45 119.3(4) . . ? C41 C46 H46 122(3) . . ? C45 C46 H46 119(3) . . ? C10' Mn1' C20' 90.37(17) . . ? C10' Mn1' C30' 90.42(16) . . ? C20' Mn1' C30' 92.71(18) . . ? C10' Mn1' C5' 175.31(17) . . ? C20' Mn1' C5' 94.31(17) . . ? C30' Mn1' C5' 89.67(16) . . ? C10' Mn1' P1' 92.66(12) . . ? C20' Mn1' P1' 95.32(13) . . ? C30' Mn1' P1' 171.38(13) . . ? C5' Mn1' P1' 86.61(11) . . ? C10' Mn1' P2' 89.32(12) . . ? C20' Mn1' P2' 168.56(13) . . ? C30' Mn1' P2' 98.73(13) . . ? C5' Mn1' P2' 86.03(11) . . ? P1' Mn1' P2' 73.28(4) . . ? S2' Cu1' S2' 180.0 2_664 . ? C21' P1' C11' 102.82(17) . . ? C21' P1' C1' 109.05(17) . . ? C11' P1' C1' 107.28(18) . . ? C21' P1' Mn1' 122.24(14) . . ? C11' P1' Mn1' 118.99(13) . . ? C1' P1' Mn1' 95.24(12) . . ? C41' P2' C31' 104.59(18) . . ? C41' P2' C1' 110.58(17) . . ? C31' P2' C1' 105.28(17) . . ? C41' P2' Mn1' 121.19(13) . . ? C31' P2' Mn1' 119.12(13) . . ? C1' P2' Mn1' 94.46(13) . . ? C2' S1' C1' 103.98(18) . . ? C2' S2' Cu1' 100.89(14) . . ? C5' N1' C6' 178.1(4) . . ? C2' N2' C3' 121.6(4) . . ? C2' N2' C4' 121.4(3) . . ? C3' N2' C4' 116.5(3) . . ? S1' C1' P1' 115.3(2) . . ? S1' C1' P2' 114.6(2) . . ? P1' C1' P2' 94.47(18) . . ? S1' C1' H1' 108(3) . . ? P1' C1' H1' 115(3) . . ? P2' C1' H1' 108(3) . . ? N2' C2' S2' 122.9(3) . . ? N2' C2' S1' 114.1(3) . . ? S2' C2' S1' 122.9(2) . . ? N2' C3' H3'A 109(3) . . ? N2' C3' H3'B 111(4) . . ? H3'A C3' H3'B 115(5) . . ? N2' C3' H3'C 110(4) . . ? H3'A C3' H3'C 104(5) . . ? H3'B C3' H3'C 108(5) . . ? N2' C4' H4'A 109.5 . . ? N2' C4' H4'B 109.5 . . ? H4'A C4' H4'B 109.5 . . ? N2' C4' H4'C 109.5 . . ? H4'A C4' H4'C 109.5 . . ? H4'B C4' H4'C 109.5 . . ? N1' C5' Mn1' 177.4(4) . . ? N1' C6' C7' 107.4(3) . . ? N1' C6' C8' 107.8(4) . . ? C7' C6' C8' 111.0(4) . . ? N1' C6' C9' 106.7(3) . . ? C7' C6' C9' 112.4(4) . . ? C8' C6' C9' 111.1(4) . . ? C6' C7' H7'A 109.5 . . ? C6' C7' H7'B 109.5 . . ? H7'A C7' H7'B 109.5 . . ? C6' C7' H7'C 109.5 . . ? H7'A C7' H7'C 109.5 . . ? H7'B C7' H7'C 109.5 . . ? C6' C8' H8'A 109.5 . . ? C6' C8' H8'B 109.5 . . ? H8'A C8' H8'B 109.5 . . ? C6' C8' H8'C 109.5 . . ? H8'A C8' H8'C 109.5 . . ? H8'B C8' H8'C 109.5 . . ? C6' C9' H9'A 109.5 . . ? C6' C9' H9'B 109.5 . . ? H9'A C9' H9'B 109.5 . . ? C6' C9' H9'C 109.5 . . ? H9'A C9' H9'C 109.5 . . ? H9'B C9' H9'C 109.5 . . ? O1' C10' Mn1' 179.0(3) . . ? O2' C20' Mn1' 176.2(4) . . ? O3' C30' Mn1' 176.5(4) . . ? C16' C11' C12' 119.8(4) . . ? C16' C11' P1' 123.2(3) . . ? C12' C11' P1' 116.8(3) . . ? C11' C12' C13' 119.3(4) . . ? C11' C12' H12' 124(2) . . ? C13' C12' H12' 117(2) . . ? C14' C13' C12' 120.5(4) . . ? C14' C13' H13' 120(3) . . ? C12' C13' H13' 119(3) . . ? C15' C14' C13' 120.0(4) . . ? C15' C14' H14' 119(3) . . ? C13' C14' H14' 120(3) . . ? C14' C15' C16' 120.3(5) . . ? C14' C15' H15' 125(3) . . ? C16' C15' H15' 115(3) . . ? C11' C16' C15' 120.0(4) . . ? C11' C16' H16' 122(3) . . ? C15' C16' H16' 118(3) . . ? C26' C21' C22' 120.3(4) . . ? C26' C21' P1' 119.1(3) . . ? C22' C21' P1' 120.5(3) . . ? C23' C22' C21' 119.2(4) . . ? C23' C22' H22' 120.4 . . ? C21' C22' H22' 120.4 . . ? C24' C23' C22' 120.6(5) . . ? C24' C23' H23' 119.7 . . ? C22' C23' H23' 119.7 . . ? C23' C24' C25' 120.6(4) . . ? C23' C24' H24' 119.7 . . ? C25' C24' H24' 119.7 . . ? C24' C25' C26' 120.1(5) . . ? C24' C25' H25' 127(4) . . ? C26' C25' H25' 113(4) . . ? C21' C26' C25' 119.1(5) . . ? C21' C26' H26' 124(2) . . ? C25' C26' H26' 117(2) . . ? C32' C31' C36' 117.7(4) . . ? C32' C31' P2' 119.5(3) . . ? C36' C31' P2' 122.7(3) . . ? C31' C32' C33' 121.4(4) . . ? C31' C32' H32' 124(3) . . ? C33' C32' H32' 114(3) . . ? C34' C33' C32' 120.3(4) . . ? C34' C33' H33' 119.8 . . ? C32' C33' H33' 119.8 . . ? C33' C34' C35' 119.5(4) . . ? C33' C34' H34' 120.3 . . ? C35' C34' H34' 120.3 . . ? C34' C35' C36' 120.3(4) . . ? C34' C35' H35' 119.9 . . ? C36' C35' H35' 119.9 . . ? C35' C36' C31' 120.8(4) . . ? C35' C36' H36' 119.6 . . ? C31' C36' H36' 119.6 . . ? C42' C41' C46' 119.3(4) . . ? C42' C41' P2' 120.2(3) . . ? C46' C41' P2' 120.4(3) . . ? C43' C42' C41' 120.5(4) . . ? C43' C42' H42' 120(3) . . ? C41' C42' H42' 120(3) . . ? C44' C43' C42' 119.7(4) . . ? C44' C43' H43' 129(3) . . ? C42' C43' H43' 112(3) . . ? C43' C44' C45' 120.8(4) . . ? C43' C44' H44' 116(3) . . ? C45' C44' H44' 123(3) . . ? C44' C45' C46' 119.8(5) . . ? C44' C45' H45' 124(3) . . ? C46' C45' H45' 115(3) . . ? C45' C46' C41' 119.8(4) . . ? C45' C46' H46' 117(3) . . ? C41' C46' H46' 123(3) . . ? Cl1 C40 Cl2 112.4(4) . . ? Cl1 C40 H40A 109.1 . . ? Cl2 C40 H40A 109.1 . . ? Cl1 C40 H40B 109.1 . . ? Cl2 C40 H40B 109.1 . . ? H40A C40 H40B 107.8 . . ? Cl3 C50 Cl4 111.8(3) . . ? Cl3 C50 H50A 105(3) . . ? Cl4 C50 H50A 104(3) . . ? Cl3 C50 H50B 110(3) . . ? Cl4 C50 H50B 111(3) . . ? H50A C50 H50B 115(4) . . ? F1 B1 F2 111.2(4) . . ? F1 B1 F3 109.4(4) . . ? F2 B1 F3 109.4(4) . . ? F1 B1 F4 109.4(4) . . ? F2 B1 F4 109.3(4) . . ? F3 B1 F4 108.0(4) . . ? F5 B2 F6 110.9(4) . . ? F5 B2 F7 110.2(4) . . ? F6 B2 F7 109.7(4) . . ? F5 B2 F8 109.4(3) . . ? F6 B2 F8 108.6(4) . . ? F7 B2 F8 108.0(4) . . ? F9 B3 F10 109.6(4) . . ? F9 B3 F11 109.1(4) . . ? F10 B3 F11 109.5(3) . . ? F9 B3 F12 110.3(3) . . ? F10 B3 F12 109.5(4) . . ? F11 B3 F12 108.7(3) . . ? 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 C10 Mn1 P1 C21 -144.03(18) . . . . ? C30 Mn1 P1 C21 -51.74(19) . . . . ? C20 Mn1 P1 C21 140.6(5) . . . . ? C5 Mn1 P1 C21 36.43(18) . . . . ? P2 Mn1 P1 C21 125.19(15) . . . . ? C10 Mn1 P1 C11 -12.47(17) . . . . ? C30 Mn1 P1 C11 79.82(17) . . . . ? C20 Mn1 P1 C11 -87.9(5) . . . . ? C5 Mn1 P1 C11 167.99(17) . . . . ? P2 Mn1 P1 C11 -103.25(13) . . . . ? C10 Mn1 P1 C1 100.74(16) . . . . ? C30 Mn1 P1 C1 -166.97(16) . . . . ? C20 Mn1 P1 C1 25.4(5) . . . . ? C5 Mn1 P1 C1 -78.80(16) . . . . ? P2 Mn1 P1 C1 9.96(12) . . . . ? C10 Mn1 P2 C31 13.16(18) . . . . ? C20 Mn1 P2 C31 -72.96(18) . . . . ? C5 Mn1 P2 C31 -167.83(18) . . . . ? P1 Mn1 P2 C31 103.02(15) . . . . ? C10 Mn1 P2 C41 141.67(18) . . . . ? C20 Mn1 P2 C41 55.54(18) . . . . ? C5 Mn1 P2 C41 -39.33(18) . . . . ? P1 Mn1 P2 C41 -128.48(14) . . . . ? C10 Mn1 P2 C1 -99.98(17) . . . . ? C20 Mn1 P2 C1 173.90(16) . . . . ? C5 Mn1 P2 C1 79.03(16) . . . . ? P1 Mn1 P2 C1 -10.12(12) . . . . ? C2 S1 C1 P2 -153.01(19) . . . . ? C2 S1 C1 P1 100.8(2) . . . . ? C31 P2 C1 S1 131.3(2) . . . . ? C41 P2 C1 S1 19.0(3) . . . . ? Mn1 P2 C1 S1 -107.20(18) . . . . ? C31 P2 C1 P1 -109.58(17) . . . . ? C41 P2 C1 P1 138.11(16) . . . . ? Mn1 P2 C1 P1 11.95(14) . . . . ? C21 P1 C1 S1 -24.1(3) . . . . ? C11 P1 C1 S1 -135.6(2) . . . . ? Mn1 P1 C1 S1 105.1(2) . . . . ? C21 P1 C1 P2 -140.93(17) . . . . ? C11 P1 C1 P2 107.58(18) . . . . ? Mn1 P1 C1 P2 -11.79(14) . . . . ? C4 N2 C2 S2 -170.9(3) . . . . ? C3 N2 C2 S2 11.4(5) . . . . ? C4 N2 C2 S1 6.7(5) . . . . ? C3 N2 C2 S1 -171.1(3) . . . . ? Cu1 S2 C2 N2 -106.8(3) . . . . ? Cu1 S2 C2 S1 75.9(2) . . . . ? C1 S1 C2 N2 -162.7(3) . . . . ? C1 S1 C2 S2 14.8(3) . . . . ? C21 P1 C11 C16 89.3(3) . . . . ? C1 P1 C11 C16 -156.5(3) . . . . ? Mn1 P1 C11 C16 -51.8(3) . . . . ? C21 P1 C11 C12 -91.4(3) . . . . ? C1 P1 C11 C12 22.8(4) . . . . ? Mn1 P1 C11 C12 127.5(3) . . . . ? C16 C11 C12 C13 0.1(5) . . . . ? P1 C11 C12 C13 -179.2(3) . . . . ? C11 C12 C13 C14 0.1(6) . . . . ? C12 C13 C14 C15 -0.1(6) . . . . ? C13 C14 C15 C16 0.0(6) . . . . ? C14 C15 C16 C11 0.1(6) . . . . ? C12 C11 C16 C15 -0.2(6) . . . . ? P1 C11 C16 C15 179.2(3) . . . . ? C11 P1 C21 C26 55.0(3) . . . . ? C1 P1 C21 C26 -59.9(3) . . . . ? Mn1 P1 C21 C26 -168.7(3) . . . . ? C11 P1 C21 C22 -122.8(3) . . . . ? C1 P1 C21 C22 122.2(3) . . . . ? Mn1 P1 C21 C22 13.4(4) . . . . ? C26 C21 C22 C23 0.8(6) . . . . ? P1 C21 C22 C23 178.7(3) . . . . ? C21 C22 C23 C24 0.4(6) . . . . ? C22 C23 C24 C25 -0.5(7) . . . . ? C23 C24 C25 C26 -0.7(7) . . . . ? C22 C21 C26 C25 -2.0(6) . . . . ? P1 C21 C26 C25 -179.9(3) . . . . ? C24 C25 C26 C21 1.9(7) . . . . ? C41 P2 C31 C32 138.2(3) . . . . ? C1 P2 C31 C32 21.0(4) . . . . ? Mn1 P2 C31 C32 -85.5(3) . . . . ? C41 P2 C31 C36 -48.7(4) . . . . ? C1 P2 C31 C36 -165.8(3) . . . . ? Mn1 P2 C31 C36 87.6(3) . . . . ? C36 C31 C32 C33 0.2(6) . . . . ? P2 C31 C32 C33 173.2(3) . . . . ? C31 C32 C33 C34 -0.9(6) . . . . ? C32 C33 C34 C35 1.3(7) . . . . ? C33 C34 C35 C36 -1.0(8) . . . . ? C34 C35 C36 C31 0.3(8) . . . . ? C32 C31 C36 C35 0.1(7) . . . . ? P2 C31 C36 C35 -173.4(4) . . . . ? C31 P2 C41 C46 -58.9(3) . . . . ? C1 P2 C41 C46 55.8(4) . . . . ? Mn1 P2 C41 C46 166.5(3) . . . . ? C31 P2 C41 C42 118.4(3) . . . . ? C1 P2 C41 C42 -126.9(3) . . . . ? Mn1 P2 C41 C42 -16.2(4) . . . . ? C46 C41 C42 C43 0.5(6) . . . . ? P2 C41 C42 C43 -176.8(3) . . . . ? C41 C42 C43 C44 -0.9(6) . . . . ? C42 C43 C44 C45 0.3(7) . . . . ? C43 C44 C45 C46 0.8(7) . . . . ? C42 C41 C46 C45 0.5(6) . . . . ? P2 C41 C46 C45 177.8(3) . . . . ? C44 C45 C46 C41 -1.2(7) . . . . ? C10' Mn1' P1' C21' -143.96(19) . . . . ? C20' Mn1' P1' C21' -53.35(19) . . . . ? C5' Mn1' P1' C21' 40.67(19) . . . . ? P2' Mn1' P1' C21' 127.54(15) . . . . ? C10' Mn1' P1' C11' -13.48(19) . . . . ? C20' Mn1' P1' C11' 77.1(2) . . . . ? C5' Mn1' P1' C11' 171.16(19) . . . . ? P2' Mn1' P1' C11' -101.97(15) . . . . ? C10' Mn1' P1' C1' 99.59(17) . . . . ? C20' Mn1' P1' C1' -169.79(17) . . . . ? C5' Mn1' P1' C1' -75.77(16) . . . . ? P2' Mn1' P1' C1' 11.10(12) . . . . ? C10' Mn1' P2' C41' 138.59(18) . . . . ? C20' Mn1' P2' C41' -132.9(7) . . . . ? C30' Mn1' P2' C41' 48.27(19) . . . . ? C5' Mn1' P2' C41' -40.79(18) . . . . ? P1' Mn1' P2' C41' -128.43(15) . . . . ? C10' Mn1' P2' C31' 6.19(18) . . . . ? C20' Mn1' P2' C31' 94.7(7) . . . . ? C30' Mn1' P2' C31' -84.13(18) . . . . ? C5' Mn1' P2' C31' -173.18(18) . . . . ? P1' Mn1' P2' C31' 99.17(14) . . . . ? C10' Mn1' P2' C1' -104.06(17) . . . . ? C20' Mn1' P2' C1' -15.5(7) . . . . ? C30' Mn1' P2' C1' 165.62(17) . . . . ? C5' Mn1' P2' C1' 76.57(16) . . . . ? P1' Mn1' P2' C1' -11.08(12) . . . . ? C2' S1' C1' P1' 115.5(2) . . . . ? C2' S1' C1' P2' -136.4(2) . . . . ? C21' P1' C1' S1' -20.0(3) . . . . ? C11' P1' C1' S1' -130.7(2) . . . . ? Mn1' P1' C1' S1' 106.72(19) . . . . ? C21' P1' C1' P2' -139.97(17) . . . . ? C11' P1' C1' P2' 109.35(18) . . . . ? Mn1' P1' C1' P2' -13.21(14) . . . . ? C41' P2' C1' S1' 18.4(3) . . . . ? C31' P2' C1' S1' 130.8(2) . . . . ? Mn1' P2' C1' S1' -107.4(2) . . . . ? C41' P2' C1' P1' 138.81(17) . . . . ? C31' P2' C1' P1' -108.77(18) . . . . ? Mn1' P2' C1' P1' 13.06(14) . . . . ? C3' N2' C2' S2' 5.9(6) . . . . ? C4' N2' C2' S2' 177.9(3) . . . . ? C3' N2' C2' S1' -175.7(4) . . . . ? C4' N2' C2' S1' -3.7(5) . . . . ? Cu1' S2' C2' N2' -82.2(3) . . . . ? Cu1' S2' C2' S1' 99.6(2) . . . . ? C1' S1' C2' N2' -176.4(3) . . . . ? C1' S1' C2' S2' 1.9(3) . . . . ? C21' P1' C11' C16' -86.1(4) . . . . ? C1' P1' C11' C16' 28.8(4) . . . . ? Mn1' P1' C11' C16' 135.2(3) . . . . ? C21' P1' C11' C12' 89.1(3) . . . . ? C1' P1' C11' C12' -156.0(3) . . . . ? Mn1' P1' C11' C12' -49.7(3) . . . . ? C16' C11' C12' C13' -0.4(6) . . . . ? P1' C11' C12' C13' -175.7(3) . . . . ? C11' C12' C13' C14' -0.2(7) . . . . ? C12' C13' C14' C15' -0.1(7) . . . . ? C13' C14' C15' C16' 1.1(7) . . . . ? C12' C11' C16' C15' 1.4(6) . . . . ? P1' C11' C16' C15' 176.4(3) . . . . ? C14' C15' C16' C11' -1.7(7) . . . . ? C11' P1' C21' C26' 57.6(4) . . . . ? C1' P1' C21' C26' -56.1(4) . . . . ? Mn1' P1' C21' C26' -165.5(3) . . . . ? C11' P1' C21' C22' -120.4(3) . . . . ? C1' P1' C21' C22' 126.0(3) . . . . ? Mn1' P1' C21' C22' 16.6(4) . . . . ? C26' C21' C22' C23' 0.2(6) . . . . ? P1' C21' C22' C23' 178.1(3) . . . . ? C21' C22' C23' C24' 1.0(7) . . . . ? C22' C23' C24' C25' -1.9(7) . . . . ? C23' C24' C25' C26' 1.6(7) . . . . ? C22' C21' C26' C25' -0.5(6) . . . . ? P1' C21' C26' C25' -178.4(3) . . . . ? C24' C25' C26' C21' -0.4(7) . . . . ? C41' P2' C31' C32' -41.2(4) . . . . ? C1' P2' C31' C32' -157.8(4) . . . . ? Mn1' P2' C31' C32' 98.0(4) . . . . ? C41' P2' C31' C36' 142.8(4) . . . . ? C1' P2' C31' C36' 26.2(4) . . . . ? Mn1' P2' C31' C36' -78.0(4) . . . . ? C36' C31' C32' C33' 1.5(7) . . . . ? P2' C31' C32' C33' -174.7(4) . . . . ? C31' C32' C33' C34' -1.0(9) . . . . ? C32' C33' C34' C35' 0.4(8) . . . . ? C33' C34' C35' C36' -0.2(7) . . . . ? C34' C35' C36' C31' 0.7(7) . . . . ? C32' C31' C36' C35' -1.3(7) . . . . ? P2' C31' C36' C35' 174.8(4) . . . . ? C31' P2' C41' C42' 115.8(3) . . . . ? C1' P2' C41' C42' -131.3(3) . . . . ? Mn1' P2' C41' C42' -22.4(4) . . . . ? C31' P2' C41' C46' -62.3(4) . . . . ? C1' P2' C41' C46' 50.6(4) . . . . ? Mn1' P2' C41' C46' 159.6(3) . . . . ? C46' C41' C42' C43' -0.6(6) . . . . ? P2' C41' C42' C43' -178.7(4) . . . . ? C41' C42' C43' C44' -1.9(7) . . . . ? C42' C43' C44' C45' 2.7(8) . . . . ? C43' C44' C45' C46' -1.0(8) . . . . ? C44' C45' C46' C41' -1.5(7) . . . . ? C42' C41' C46' C45' 2.3(6) . . . . ? P2' C41' C46' C45' -179.6(4) . . . . ? loop_ _publ_manuscript_incl_extra_item '_geom_bond_atom_site_label_D' '_geom_bond_atom_site_label_H' '_geom_contact_atom_site_label_A' '_geom_bond_distance_DH' '_geom_contact_distance_HA' '_geom_contact_distance_DA' '_geom_angle_DHA' '_geom_contact_site_symmetry_A' loop_ _geom_bond_atom_site_label_d _geom_bond_atom_site_label_h _geom_contact_atom_site_label_a _geom_bond_distance_dh _geom_contact_distance_ha _geom_contact_distance_da _geom_angle_dha _geom_contact_site_symmetry_a C1 H1 S2 0.87(4) 3.197(5) 2.55(5) 132.(4) 1_555 C3 H3C S2 0.960(5) 3.020(6) 2.661(1) 102.7(3) 1_555 C3 H3C F2 0.960(5) 3.418(5) 2.972(3) 109.8(3) 1_555 C4 H4A S1 0.960(6) 2.865(6) 2.603(1) 95.8(3) 1_555 C4 H4B F1 0.960(4) 3.143(5) 2.368(3) 137.5(3) 1_555 C8 H8C F6 0.960(6) 3.393(7) 2.524(4) 150.5(3) 1_555 C9 H9C F5 0.960(6) 3.278(7) 2.446(3) 144.8(3) 1_555 C22 H22 N1 0.930(5) 3.436(5) 2.909(3) 117.2(2) 1_555 C26 H26 S2 0.88(4) 3.720(4) 2.93(4) 151.(4) 1_555 C34 H34 F11 1.02(6) 3.387(6) 2.84(6) 114.(4) 1_555 C35 H35 F11 0.98(9) 3.187(6) 2.49(9) 128.(6) 1_555 C42 H42 O2 0.97(4) 3.610(6) 2.86(4) 134.(3) 1_555 C42 H42 F5 0.97(4) 3.447(5) 2.56(4) 152.(3) 1_555 C46 H46 F4 0.91(5) 3.088(6) 2.44(5) 129.(4) 1_555 C1' H1' S2' 0.75(5) 3.151(4) 2.63(4) 129.(4) 1_555 C3' H3'C S2' 0.93(6) 3.024(5) 2.74(6) 99.(5) 1_555 C4' H4'A S1' 0.960(6) 2.829(4) 2.670(1) 89.4(3) 1_555 C4' H4'B S1' 0.960(5) 2.829(4) 2.746(1) 85.0(3) 1_555 C16' H16' S2' 0.95(5) 3.767(5) 2.83(5) 168.(4.) 1_555 C22' H22' O2' 0.930(4) 3.773(5) 2.990(3) 142.9(3) 1_555 C42' H42' O3' 0.92(5) 3.711(5) 2.84(5) 159.(4) 1_555 C40 H40A F7 0.970(9) 3.207(9) 2.254(4) 167.1(4) 1_555 C40 H40A F8 0.970(9) 2.987(8) 2.390(3) 119.3(4) 1_555 C40 H40B F8 0.970(7) 2.987(8) 2.940(3) 83.3(4) 1_555 C50 H50B O2 1.07(6) 3.184(8) 2.82(6) 100.(3) 1_555 C50 H50B F8 1.07(6) 3.253(7) 2.21(6) 165.(5) 1_555 C4 H4C F3 0.960(6) 3.342(7) 2.450(3) 154.5(3) 2_565 C14' H14' F3 0.99(5) 3.125(5) 2.41(5) 129.(4) 2_565 C8 H8A O1 0.960(5) 3.446(5) 2.629(3) 143.2(3) 1_455 C44 H44 F11 1.00(5) 3.309(5) 2.63(5) 125.(4) 1_455 C7 H7C O1 1.01(5) 3.582(5) 2.76(5) 139.(4) 1_455 C9 H9B O1 0.960(5) 3.357(5) 2.506(3) 147.7(3) 1_455 C32 H32 F2 0.930(4) 3.319(5) 2.776(4) 118.3(2) 2_665 C15' H15' F11 0.92(5) 3.510(7) 2.68(6) 150.(4) 2_665 C33 H33 F2 0.98(5) 3.288(6) 2.61(6) 126.(3) 2_665 C13 H13 F3 0.98(5) 3.218(6) 2.28(5) 160.(4) 2_665 C24' H24' F3 0.930(5) 3.383(6) 2.505(3) 157.6(3) 2_665 C35' H35' F9 0.930(4) 3.117(5) 2.529(3) 121.4(3) 2_665 C46' H46' F12 0.98(5) 3.333(5) 2.68(5) 124.(4) 1_554 C33' H33' O2 0.930(5) 3.222(5) 2.595(3) 125.2(3) 1_554 C33' H33' F5 0.930(5) 3.365(6) 2.485(3) 157.9(3) 1_554 C4' H4'B F10 0.960(5) 3.366(6) 2.627(4) 134.1(3) 1_554 C3' H3'A F12 0.97(7) 3.333(6) 2.78(5) 117.(4) 1_554 C45' H45' F11 1.01(6) 3.454(6) 2.54(5) 149.(4) 1_554 C7' H7'C O1' 0.960(4) 3.353(5) 2.541(3) 142.5(3) 1_655 C9' H9'C O1' 0.960(5) 3.363(6) 2.523(3) 146.2(3) 1_655 C44' H44' F5 0.96(6) 3.676(6) 2.77(6) 156.(5) 1_654 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 68.35 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.170 _refine_diff_density_min -0.893 _refine_diff_density_rms 0.112 #==END