# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_msb422_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H40 Mo N O8 P2' _chemical_formula_sum 'C43 H40 Mo N O8 P2' _chemical_formula_weight 856.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/a _symmetry_space_group_name_Hall '-I 4ad' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 21.060(2) _cell_length_b 21.060(2) _cell_length_c 17.7326(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7864.6(14) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2749 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 26.76 _exptl_crystal_description Slab _exptl_crystal_colour colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3528 _exptl_absorpt_coefficient_mu 0.470 _exptl_absorpt_correction_type 'integration numerical gaussian' _exptl_absorpt_correction_T_min 0.8532 _exptl_absorpt_correction_T_max 0.9545 _exptl_absorpt_process_details 'TWINABS (Sheldrick, 2008b)' _exptl_special_details ; The diffraction data were collected in three sets of 606 frames (0.3 deg. width in omega) at phi = 0, 120 and 240 deg. A scan time of 50 sec/frame was used. From 3538 reflections having I/\s(I) > 15 and chosen from the fulldata set, it was determined that the crystal was comprised of two comp0onents rotated by 173.8 deg about an axis slightly offset from c (CELL_NOW (Sheldrick, 2008a)). Integration of the raw data was accomplished withthe multi-component version of SAINT using the two- component control file generated by CELL_NOW. ; _diffrn_ambient_temperature 100(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 'Bruker APEX-I CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 133140 _diffrn_reflns_av_R_equivalents 0.0622 _diffrn_reflns_av_sigmaI/netI 0.0382 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 27.91 _reflns_number_total 12904 _reflns_number_gt 9334 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2009)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2009a)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS 2009a)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008)' _computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008)' _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. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. The portion of the allyl substituent consisting of C8 and C9 is disordered over two equally populated sites because of the 4-bar crystallographic symmetry imposed on the molecule. This was modeled with the geometries of the two sites constrained to be essentially the same as the ordered allyl substituent. The final refinement was performed with the full 2-component data set. ; _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^)+(0.0534P)^2^+9.9389P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00012(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12904 _refine_ls_number_parameters 261 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0755 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1265 _refine_ls_wR_factor_gt 0.1101 _refine_ls_goodness_of_fit_ref 1.712 _refine_ls_restrained_S_all 1.716 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.5000 0.2500 0.037651(18) 0.02637(13) Uani 1 2 d S . . P1 P 0.44980(4) 0.21330(3) 0.15390(4) 0.02342(17) Uani 1 1 d . . . O1 O 0.44344(10) 0.14024(10) 0.18081(11) 0.0263(4) Uani 1 1 d . . . O2 O 0.38293(10) 0.23620(10) 0.18908(11) 0.0270(4) Uani 1 1 d . . . O3 O 0.40560(13) 0.36658(11) 0.01467(13) 0.0409(6) Uani 1 1 d . . . O4 O 0.58544(13) 0.32131(13) -0.08182(13) 0.0445(6) Uani 1 1 d . . . N1 N 0.5000 0.2500 0.21492(17) 0.0208(6) Uani 1 2 d S . . C1 C 0.48617(14) 0.09248(14) 0.15851(16) 0.0263(6) Uani 1 1 d . A . C2 C 0.54655(15) 0.09107(15) 0.18908(17) 0.0301(6) Uani 1 1 d . . . H2 H 0.5608 0.1248 0.2204 0.036 Uiso 1 1 calc R . . C3 C 0.58595(17) 0.04017(16) 0.17370(19) 0.0368(7) Uani 1 1 d . . . H3 H 0.6278 0.0391 0.1936 0.044 Uiso 1 1 calc R . . C4 C 0.56413(19) -0.00908(17) 0.1292(2) 0.0405(8) Uani 1 1 d . . . H4 H 0.5905 -0.0448 0.1201 0.049 Uiso 1 1 calc R . . C5 C 0.50406(19) -0.00648(16) 0.0980(2) 0.0393(8) Uani 1 1 d . A . H5 H 0.4899 -0.0405 0.0671 0.047 Uiso 1 1 calc R . . C6 C 0.46363(16) 0.04503(15) 0.11097(16) 0.0308(6) Uani 1 1 d . . . C7 C 0.39708(17) 0.04657(18) 0.07856(18) 0.0414(8) Uani 0.50 1 d PD A 1 H7A H 0.3883 0.0899 0.0596 0.050 Uiso 0.50 1 calc PR A 1 H7B H 0.3952 0.0173 0.0350 0.050 Uiso 0.50 1 calc PR A 1 C8 C 0.3460(3) 0.0285(4) 0.1335(4) 0.0463(13) Uani 0.50 1 d PD A 1 H8 H 0.3340 0.0565 0.1731 0.056 Uiso 0.50 1 calc PR A 1 C9 C 0.3184(5) -0.0265(4) 0.1256(8) 0.077(2) Uani 0.50 1 d PD A 1 H9A H 0.3308 -0.0540 0.0857 0.092 Uiso 0.50 1 calc PR A 1 H9B H 0.2859 -0.0391 0.1596 0.092 Uiso 0.50 1 calc PR A 1 C7A C 0.39708(17) 0.04657(18) 0.07856(18) 0.0414(8) Uani 0.50 1 d PD A 2 H7A1 H 0.3779 0.0891 0.0853 0.050 Uiso 0.50 1 calc PR A 2 H7A2 H 0.3978 0.0364 0.0241 0.050 Uiso 0.50 1 calc PR A 2 C8A C 0.3598(3) -0.0029(3) 0.1215(4) 0.0463(13) Uani 0.50 1 d PD A 2 H8A H 0.3799 -0.0433 0.1242 0.056 Uiso 0.50 1 calc PR A 2 C9A C 0.3056(4) 0.0000(6) 0.1552(8) 0.077(2) Uani 0.50 1 d PD A 2 H9A1 H 0.2822 0.0385 0.1553 0.092 Uiso 0.50 1 calc PR A 2 H9A2 H 0.2890 -0.0365 0.1799 0.092 Uiso 0.50 1 calc PR A 2 C10 C 0.32544(15) 0.21020(15) 0.16246(19) 0.0323(7) Uani 1 1 d . . . C11 C 0.30994(19) 0.21804(18) 0.0870(2) 0.0447(9) Uani 1 1 d . . . H11 H 0.3384 0.2389 0.0536 0.054 Uiso 1 1 calc R . . C12 C 0.2524(2) 0.1950(2) 0.0613(3) 0.0611(13) Uani 1 1 d . . . H12 H 0.2412 0.1993 0.0097 0.073 Uiso 1 1 calc R . . C13 C 0.2119(2) 0.1662(2) 0.1103(3) 0.0682(15) Uani 1 1 d . . . H13 H 0.1720 0.1513 0.0926 0.082 Uiso 1 1 calc R . . C14 C 0.22787(19) 0.15825(18) 0.1858(3) 0.0549(11) Uani 1 1 d . . . H14 H 0.1989 0.1379 0.2190 0.066 Uiso 1 1 calc R . . C15 C 0.28627(16) 0.17990(15) 0.2135(2) 0.0361(8) Uani 1 1 d . . . C16 C 0.30494(15) 0.17020(15) 0.2949(2) 0.0356(7) Uani 1 1 d . . . H16A H 0.3515 0.1644 0.2975 0.043 Uiso 1 1 calc R . . H16B H 0.2943 0.2091 0.3236 0.043 Uiso 1 1 calc R . . C17 C 0.27335(16) 0.11429(16) 0.3321(2) 0.0406(8) Uani 1 1 d . . . H17 H 0.2794 0.0737 0.3099 0.049 Uiso 1 1 calc R . . C18 C 0.23839(18) 0.11728(19) 0.3925(2) 0.0476(9) Uani 1 1 d . . . H18A H 0.2312 0.1570 0.4164 0.057 Uiso 1 1 calc R . . H18B H 0.2200 0.0797 0.4127 0.057 Uiso 1 1 calc R . . C19 C 0.5000 0.2500 0.2961(2) 0.0210(7) Uani 1 2 d S . . C20 C 0.4825(3) 0.1960(3) 0.3351(3) 0.0227(7) Uani 0.50 1 d P . . H20 H 0.4723 0.1593 0.3102 0.027 Uiso 1 1 d R . . C20A C 0.4465(3) 0.2689(3) 0.3365(3) 0.0227(7) Uani 0.50 1 d P . . H20A H 0.4076 0.2784 0.3094 0.027 Uiso 1 1 d R . . C21 C 0.43953(17) 0.32591(15) 0.02729(16) 0.0321(7) Uani 1 1 d . . . C22 C 0.55439(17) 0.29478(15) -0.03950(17) 0.0335(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0418(2) 0.0266(2) 0.01068(16) 0.000 0.000 0.00366(15) P1 0.0310(4) 0.0265(4) 0.0128(3) -0.0011(3) -0.0026(3) 0.0033(3) O1 0.0307(11) 0.0273(10) 0.0209(9) -0.0004(8) 0.0001(8) 0.0028(8) O2 0.0280(10) 0.0326(11) 0.0204(9) -0.0054(8) -0.0052(8) 0.0028(8) O3 0.0561(15) 0.0375(13) 0.0291(12) 0.0022(10) -0.0067(11) 0.0120(11) O4 0.0600(16) 0.0487(15) 0.0249(12) 0.0061(10) 0.0046(11) -0.0080(12) N1 0.0253(16) 0.0251(16) 0.0120(14) 0.000 0.000 0.0002(13) C1 0.0344(15) 0.0251(14) 0.0195(13) 0.0023(11) 0.0038(11) 0.0027(12) C2 0.0335(16) 0.0298(15) 0.0272(15) -0.0001(12) 0.0012(12) -0.0013(12) C3 0.0367(17) 0.0387(18) 0.0348(17) 0.0059(14) 0.0015(14) 0.0059(14) C4 0.051(2) 0.0323(17) 0.0380(18) 0.0001(14) 0.0055(15) 0.0117(15) C5 0.058(2) 0.0299(16) 0.0303(16) -0.0058(13) 0.0030(15) -0.0004(15) C6 0.0413(17) 0.0317(15) 0.0194(13) 0.0000(11) 0.0010(12) -0.0032(13) C7 0.048(2) 0.048(2) 0.0288(16) -0.0081(14) -0.0070(14) -0.0053(16) C8 0.039(3) 0.047(4) 0.052(3) -0.009(3) 0.004(2) 0.006(3) C9 0.055(5) 0.059(6) 0.116(9) -0.003(5) 0.029(4) -0.006(4) C7A 0.048(2) 0.048(2) 0.0288(16) -0.0081(14) -0.0070(14) -0.0053(16) C8A 0.039(3) 0.047(4) 0.052(3) -0.009(3) 0.004(2) 0.006(3) C9A 0.055(5) 0.059(6) 0.116(9) -0.003(5) 0.029(4) -0.006(4) C10 0.0322(16) 0.0289(15) 0.0357(17) -0.0086(13) -0.0152(13) 0.0088(12) C11 0.051(2) 0.0435(19) 0.0391(19) -0.0119(16) -0.0227(16) 0.0175(16) C12 0.074(3) 0.046(2) 0.064(3) -0.017(2) -0.047(3) 0.016(2) C13 0.062(3) 0.040(2) 0.103(4) -0.006(2) -0.059(3) -0.001(2) C14 0.041(2) 0.0322(19) 0.092(3) 0.003(2) -0.030(2) -0.0048(15) C15 0.0304(16) 0.0236(15) 0.054(2) -0.0024(14) -0.0157(15) 0.0045(12) C16 0.0282(15) 0.0282(16) 0.050(2) 0.0042(14) -0.0060(14) 0.0016(12) C17 0.0328(17) 0.0291(16) 0.060(2) 0.0005(15) 0.0030(16) 0.0012(13) C18 0.042(2) 0.0398(19) 0.061(2) 0.0005(17) 0.0061(18) 0.0008(16) C19 0.0251(19) 0.0254(19) 0.0123(16) 0.000 0.000 0.0003(15) C20 0.0263(19) 0.0263(19) 0.0155(18) -0.0016(14) -0.0010(14) -0.0002(15) C20A 0.0263(19) 0.0263(19) 0.0155(18) -0.0016(14) -0.0010(14) -0.0002(15) C21 0.0481(19) 0.0335(16) 0.0146(13) -0.0004(11) -0.0020(12) -0.0009(14) C22 0.050(2) 0.0338(16) 0.0170(13) -0.0011(12) -0.0027(13) 0.0035(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C22 2.018(3) . ? Mo1 C22 2.018(3) 6_554 ? Mo1 C21 2.052(3) . ? Mo1 C21 2.052(3) 6_554 ? Mo1 P1 2.4422(8) . ? Mo1 P1 2.4423(8) 6_554 ? P1 O2 1.614(2) . ? P1 O1 1.616(2) . ? P1 N1 1.699(2) . ? O1 C1 1.406(3) . ? O2 C10 1.410(4) . ? O3 C21 1.138(4) . ? O4 C22 1.142(4) . ? N1 C19 1.439(5) . ? N1 P1 1.699(2) 6_554 ? C1 C2 1.383(4) . ? C1 C6 1.391(4) . ? C2 C3 1.383(5) . ? C2 H2 0.9500 . ? C3 C4 1.381(5) . ? C3 H3 0.9500 . ? C4 C5 1.382(5) . ? C4 H4 0.9500 . ? C5 C6 1.398(5) . ? C5 H5 0.9500 . ? C6 C7 1.515(5) . ? C7 C8 1.501(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.304(5) . ? C8 H8 0.9500 . ? C9 H9A 0.9500 . ? C9 H9B 0.9500 . ? C8A C9A 1.291(5) . ? C8A H8A 0.9500 . ? C9A H9A1 0.9500 . ? C9A H9A2 0.9500 . ? C10 C15 1.381(5) . ? C10 C11 1.387(5) . ? C11 C12 1.382(6) . ? C11 H11 0.9500 . ? C12 C13 1.360(8) . ? C12 H12 0.9500 . ? C13 C14 1.392(7) . ? C13 H13 0.9500 . ? C14 C15 1.401(5) . ? C14 H14 0.9500 . ? C15 C16 1.509(5) . ? C16 C17 1.505(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.301(5) . ? C17 H17 0.9500 . ? C18 H18A 0.9500 . ? C18 H18B 0.9500 . ? C19 C20 1.381(6) . ? C19 C20 1.381(6) 6_554 ? C19 C20A 1.393(6) . ? C19 C20A 1.393(6) 6_554 ? C20 C20A 1.390(7) 16_656 ? C20 H20 0.9158 . ? C20A C20 1.390(7) 11_666 ? C20A H20A 0.9713 . ? 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 C22 Mo1 C22 94.64(18) . 6_554 ? C22 Mo1 C21 85.84(13) . . ? C22 Mo1 C21 87.20(13) 6_554 . ? C22 Mo1 C21 87.20(13) . 6_554 ? C22 Mo1 C21 85.84(13) 6_554 6_554 ? C21 Mo1 C21 169.73(16) . 6_554 ? C22 Mo1 P1 164.96(9) . . ? C22 Mo1 P1 100.29(9) 6_554 . ? C21 Mo1 P1 93.07(9) . . ? C21 Mo1 P1 95.60(8) 6_554 . ? C22 Mo1 P1 100.29(9) . 6_554 ? C22 Mo1 P1 164.96(9) 6_554 6_554 ? C21 Mo1 P1 95.60(8) . 6_554 ? C21 Mo1 P1 93.07(9) 6_554 6_554 ? P1 Mo1 P1 64.86(4) . 6_554 ? O2 P1 O1 95.62(11) . . ? O2 P1 N1 99.26(9) . . ? O1 P1 N1 107.26(10) . . ? O2 P1 Mo1 127.55(8) . . ? O1 P1 Mo1 125.89(8) . . ? N1 P1 Mo1 97.13(9) . . ? C1 O1 P1 123.00(18) . . ? C10 O2 P1 120.26(18) . . ? C19 N1 P1 129.56(8) . . ? C19 N1 P1 129.56(8) . 6_554 ? P1 N1 P1 100.88(16) . 6_554 ? C2 C1 C6 122.4(3) . . ? C2 C1 O1 119.6(3) . . ? C6 C1 O1 117.8(3) . . ? C1 C2 C3 119.4(3) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C4 C3 C2 119.7(3) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 120.2(3) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C4 C5 C6 121.5(3) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C1 C6 C5 116.7(3) . . ? C1 C6 C7 122.0(3) . . ? C5 C6 C7 121.2(3) . . ? C8 C7 C6 114.3(4) . . ? C8 C7 H7A 108.7 . . ? C6 C7 H7A 108.7 . . ? C8 C7 H7B 108.7 . . ? C6 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C9 C8 C7 118.3(7) . . ? C9 C8 H8 120.9 . . ? C7 C8 H8 120.9 . . ? C8 C9 H9A 120.0 . . ? C8 C9 H9B 120.0 . . ? H9A C9 H9B 120.0 . . ? C9A C8A H8A 114.3 . . ? C8A C9A H9A1 120.0 . . ? C8A C9A H9A2 120.0 . . ? H9A1 C9A H9A2 120.0 . . ? C15 C10 C11 123.2(3) . . ? C15 C10 O2 118.2(3) . . ? C11 C10 O2 118.6(3) . . ? C12 C11 C10 118.8(4) . . ? C12 C11 H11 120.6 . . ? C10 C11 H11 120.6 . . ? C13 C12 C11 119.8(4) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C14 121.1(4) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C13 C14 C15 120.7(4) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C10 C15 C14 116.4(4) . . ? C10 C15 C16 122.3(3) . . ? C14 C15 C16 121.3(4) . . ? C17 C16 C15 114.2(3) . . ? C17 C16 H16A 108.7 . . ? C15 C16 H16A 108.7 . . ? C17 C16 H16B 108.7 . . ? C15 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? C18 C17 C16 125.0(3) . . ? C18 C17 H17 117.5 . . ? C16 C17 H17 117.5 . . ? C17 C18 H18A 120.0 . . ? C17 C18 H18B 120.0 . . ? H18A C18 H18B 120.0 . . ? C20 C19 C20 119.9(5) . 6_554 ? C20 C19 C20A 76.3(3) . . ? C20 C19 C20A 73.8(3) 6_554 . ? C20 C19 C20A 73.8(3) . 6_554 ? C20 C19 C20A 76.3(3) 6_554 6_554 ? C20A C19 C20A 118.0(5) . 6_554 ? C20 C19 N1 120.1(3) . . ? C20 C19 N1 120.1(3) 6_554 . ? C20A C19 N1 121.0(3) . . ? C20A C19 N1 121.0(3) 6_554 . ? C19 C20 C20A 120.0(5) . 16_656 ? C19 C20 H20 121.1 . . ? C20A C20 H20 118.8 16_656 . ? C20A C20 H20 126.4 6_554 . ? C20 C20A C19 121.0(5) 11_666 . ? C20 C20A H20A 119.5 11_666 . ? C19 C20A H20A 119.1 . . ? O3 C21 Mo1 173.7(3) . . ? O4 C22 Mo1 178.2(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.91 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.360 _refine_diff_density_min -1.419 _refine_diff_density_rms 0.092 _database_code_depnum_ccdc_archive 'CCDC 955814' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_msb423_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H38 N O8 P2 W' _chemical_formula_sum 'C43 H38 N O8 P2 W' _chemical_formula_weight 945.54 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' 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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/a _symmetry_space_group_name_Hall '-I 4ad' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 21.0377(17) _cell_length_b 21.0377(17) _cell_length_c 17.7433(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7852.9(11) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9698 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 29.13 _exptl_crystal_description Parallelepiped _exptl_crystal_colour colourless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3768 _exptl_absorpt_coefficient_mu 3.078 _exptl_absorpt_correction_type 'integration numerical Gaussian' _exptl_absorpt_correction_T_min 0.4650 _exptl_absorpt_correction_T_max 0.7127 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008a)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in omega, colllected at phi = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in phi, collected at omega = -30.00 and 210.00 deg. The scan time was 15 sec/frame. ; _diffrn_ambient_temperature 100(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 'Bruker APEX-I CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 70156 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_sigmaI/netI 0.0192 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 29.17 _reflns_number_total 5271 _reflns_number_gt 4445 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2009)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2009a)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS 2009a)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008)' _computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008)' _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. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. The allyl group attached to C6 is disordered over two equally populated sites having C7 in common as a result of the -4 crystallographic symmetry imposed. The geometry of this substituent was constrained to be that of the ordered allyl substituent. The -4 symmetry also occasions a smaller amount of disorder in one of the phenyl rings as indicated by the elongated displacement ellipsoids but it did not seem to model this further. ; _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^)+(0.0259P)^2^+24.1691P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5271 _refine_ls_number_parameters 259 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0645 _refine_ls_wR_factor_gt 0.0595 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.5000 0.2500 0.037758(7) 0.02921(5) Uani 1 2 d S . . P1 P 0.44997(3) 0.21344(3) 0.15368(3) 0.02440(13) Uani 1 1 d . . . O1 O 0.44341(8) 0.14018(8) 0.17994(10) 0.0263(4) Uani 1 1 d . . . O2 O 0.38289(8) 0.23646(9) 0.18824(10) 0.0285(4) Uani 1 1 d . . . O3 O 0.40559(12) 0.36627(10) 0.01452(12) 0.0454(5) Uani 1 1 d . . . O4 O 0.58553(12) 0.32190(11) -0.08092(12) 0.0481(6) Uani 1 1 d . . . N1 N 0.5000 0.2500 0.21497(14) 0.0203(5) Uani 1 2 d S . . C1 C 0.48597(13) 0.09210(12) 0.15783(14) 0.0272(5) Uani 1 1 d . A . C2 C 0.54652(13) 0.09110(13) 0.18815(16) 0.0316(5) Uani 1 1 d . . . H2 H 0.5608 0.1251 0.2190 0.038 Uiso 1 1 calc R . . C3 C 0.58615(15) 0.04021(14) 0.17321(17) 0.0379(6) Uani 1 1 d . . . H3 H 0.6280 0.0392 0.1933 0.046 Uiso 1 1 calc R . . C4 C 0.56429(17) -0.00940(14) 0.12867(18) 0.0425(7) Uani 1 1 d . . . H4 H 0.5908 -0.0451 0.1193 0.051 Uiso 1 1 calc R . . C5 C 0.50389(17) -0.00701(14) 0.09778(18) 0.0413(7) Uani 1 1 d . A . H5 H 0.4897 -0.0412 0.0670 0.050 Uiso 1 1 calc R . . C6 C 0.46320(14) 0.04441(13) 0.11073(15) 0.0321(6) Uani 1 1 d . . . C7 C 0.39676(15) 0.04556(16) 0.07837(16) 0.0429(7) Uani 0.50 1 d PD A 1 H7A H 0.3880 0.0887 0.0587 0.051 Uiso 0.50 1 calc PR A 1 H7B H 0.3949 0.0157 0.0353 0.051 Uiso 0.50 1 calc PR A 1 C8 C 0.3457(3) 0.0282(3) 0.1334(4) 0.0477(12) Uani 0.50 1 d PD A 1 H8 H 0.3337 0.0567 0.1724 0.057 Uiso 0.50 1 calc PR A 1 C9 C 0.3183(5) -0.0269(4) 0.1263(7) 0.078(2) Uani 0.50 1 d PD A 1 H9A H 0.3308 -0.0549 0.0870 0.094 Uiso 0.50 1 calc PR A 1 H9B H 0.2857 -0.0391 0.1604 0.094 Uiso 0.50 1 calc PR A 1 C7A C 0.39676(15) 0.04556(16) 0.07837(16) 0.0429(7) Uani 0.50 1 d PD A 2 H7A1 H 0.3976 0.0352 0.0239 0.051 Uiso 0.50 1 calc PR A 2 H7A2 H 0.3774 0.0881 0.0849 0.051 Uiso 0.50 1 calc PR A 2 C8A C 0.3592(3) -0.0042(3) 0.1216(4) 0.0477(12) Uani 0.50 1 d PD A 2 H8A H 0.3776 -0.0455 0.1220 0.057 Uiso 0.50 1 calc PR A 2 C9A C 0.3062(4) 0.0009(5) 0.1579(6) 0.078(2) Uani 0.50 1 d PD A 2 H9A1 H 0.2849 0.0407 0.1601 0.094 Uiso 0.50 1 calc PR A 2 H9A2 H 0.2885 -0.0351 0.1825 0.094 Uiso 0.50 1 calc PR A 2 C10 C 0.32546(14) 0.21033(13) 0.16187(17) 0.0360(6) Uani 1 1 d . . . C11 C 0.30981(18) 0.21783(17) 0.0865(2) 0.0521(9) Uani 1 1 d . . . H11 H 0.3382 0.2384 0.0528 0.062 Uiso 1 1 calc R . . C12 C 0.2521(2) 0.1948(2) 0.0613(3) 0.0725(15) Uani 1 1 d . . . H12 H 0.2406 0.1992 0.0098 0.087 Uiso 1 1 calc R . . C13 C 0.2116(2) 0.1658(2) 0.1104(3) 0.0807(17) Uani 1 1 d . . . H13 H 0.1718 0.1506 0.0928 0.097 Uiso 1 1 calc R . . C14 C 0.22767(18) 0.15809(16) 0.1862(3) 0.0628(12) Uani 1 1 d . . . H14 H 0.1986 0.1381 0.2196 0.075 Uiso 1 1 calc R . . C15 C 0.28651(14) 0.17968(13) 0.2133(2) 0.0399(7) Uani 1 1 d . . . C16 C 0.30535(13) 0.17032(14) 0.29450(18) 0.0378(6) Uani 1 1 d . . . H16A H 0.3520 0.1645 0.2971 0.045 Uiso 1 1 calc R . . H16B H 0.2947 0.2093 0.3230 0.045 Uiso 1 1 calc R . . C17 C 0.27381(14) 0.11447(15) 0.3321(2) 0.0444(8) Uani 1 1 d . . . H17 H 0.2797 0.0738 0.3098 0.053 Uiso 1 1 calc R . . C18 C 0.23893(17) 0.11743(18) 0.3929(2) 0.0526(9) Uani 1 1 d . . . H18A H 0.2319 0.1572 0.4169 0.063 Uiso 1 1 calc R . . H18B H 0.2206 0.0798 0.4132 0.063 Uiso 1 1 calc R . . C19 C 0.5000 0.2500 0.29610(17) 0.0213(6) Uani 1 2 d S . . C20 C 0.4823(2) 0.1959(2) 0.3353(3) 0.0232(6) Uani 0.50 1 d P . . H20 H 0.4700 0.1618 0.3108 0.028 Uiso 0.50 1 d PR . . C20A C 0.4466(2) 0.2688(2) 0.3363(3) 0.0232(6) Uani 0.50 1 d P . . H20A H 0.4132 0.2842 0.3076 0.028 Uiso 0.50 1 d PR . . C21 C 0.43951(16) 0.32547(14) 0.02689(15) 0.0355(6) Uani 1 1 d . . . C22 C 0.55438(16) 0.29542(14) -0.03873(15) 0.0370(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.05087(10) 0.02623(8) 0.01054(7) 0.000 0.000 0.00336(6) P1 0.0350(3) 0.0256(3) 0.0127(2) -0.0007(2) -0.0031(2) 0.0035(2) O1 0.0325(9) 0.0259(8) 0.0204(8) 0.0008(7) -0.0002(7) 0.0029(7) O2 0.0306(9) 0.0329(9) 0.0221(8) -0.0065(7) -0.0073(7) 0.0057(7) O3 0.0664(15) 0.0395(12) 0.0301(11) 0.0010(9) -0.0080(10) 0.0115(11) O4 0.0663(15) 0.0509(13) 0.0271(11) 0.0068(9) 0.0051(10) -0.0066(11) N1 0.0263(14) 0.0233(13) 0.0112(12) 0.000 0.000 0.0037(11) C1 0.0374(14) 0.0239(12) 0.0202(11) 0.0024(9) 0.0032(10) 0.0015(10) C2 0.0354(14) 0.0301(13) 0.0293(13) 0.0001(11) 0.0006(11) 0.0004(11) C3 0.0388(15) 0.0388(15) 0.0363(15) 0.0038(12) 0.0021(12) 0.0075(12) C4 0.0561(19) 0.0328(14) 0.0387(16) 0.0025(12) 0.0070(14) 0.0126(13) C5 0.061(2) 0.0312(14) 0.0317(15) -0.0042(12) 0.0041(14) 0.0001(13) C6 0.0433(15) 0.0308(13) 0.0221(12) 0.0001(10) 0.0015(11) -0.0023(11) C7 0.0497(18) 0.0488(18) 0.0300(15) -0.0089(13) -0.0072(13) -0.0058(14) C8 0.041(3) 0.045(3) 0.057(3) -0.013(3) 0.001(2) 0.003(2) C9 0.063(4) 0.060(5) 0.111(7) -0.014(4) 0.028(4) -0.013(4) C7A 0.0497(18) 0.0488(18) 0.0300(15) -0.0089(13) -0.0072(13) -0.0058(14) C8A 0.041(3) 0.045(3) 0.057(3) -0.013(3) 0.001(2) 0.003(2) C9A 0.063(4) 0.060(5) 0.111(7) -0.014(4) 0.028(4) -0.013(4) C10 0.0362(14) 0.0309(14) 0.0409(16) -0.0096(12) -0.0194(12) 0.0093(11) C11 0.064(2) 0.0505(19) 0.0415(18) -0.0148(15) -0.0290(16) 0.0223(16) C12 0.086(3) 0.054(2) 0.077(3) -0.024(2) -0.061(3) 0.023(2) C13 0.071(3) 0.045(2) 0.125(4) -0.011(2) -0.072(3) -0.0007(19) C14 0.0459(19) 0.0345(17) 0.108(3) 0.0000(19) -0.039(2) -0.0035(14) C15 0.0340(14) 0.0236(13) 0.062(2) -0.0035(12) -0.0182(14) 0.0048(11) C16 0.0284(13) 0.0295(14) 0.0555(19) 0.0043(12) -0.0077(12) 0.0016(11) C17 0.0339(15) 0.0322(15) 0.067(2) 0.0007(14) 0.0038(15) 0.0018(12) C18 0.0434(18) 0.0438(18) 0.071(2) -0.0026(17) 0.0058(17) -0.0018(14) C19 0.0266(16) 0.0253(16) 0.0118(13) 0.000 0.000 0.0001(13) C20 0.0270(16) 0.0279(16) 0.0146(15) -0.0008(12) 0.0011(12) 0.0009(13) C20A 0.0270(16) 0.0279(16) 0.0146(15) -0.0008(12) 0.0011(12) 0.0009(13) C21 0.0563(18) 0.0330(14) 0.0170(12) 0.0002(10) -0.0037(11) 0.0019(12) C22 0.0606(19) 0.0336(14) 0.0167(12) 0.0009(10) -0.0011(12) 0.0023(13) _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 W1 C22 2.016(3) . ? W1 C22 2.016(3) 6_554 ? W1 C21 2.044(3) 6_554 ? W1 C21 2.044(3) . ? W1 P1 2.4351(7) 6_554 ? W1 P1 2.4352(7) . ? P1 O2 1.6130(19) . ? P1 O1 1.6160(18) . ? P1 N1 1.6976(18) . ? O1 C1 1.407(3) . ? O2 C10 1.407(3) . ? O3 C21 1.138(4) . ? O4 C22 1.140(4) . ? N1 C19 1.439(4) . ? N1 P1 1.6976(17) 6_554 ? C1 C2 1.383(4) . ? C1 C6 1.391(4) . ? C2 C3 1.383(4) . ? C2 H2 0.9500 . ? C3 C4 1.388(4) . ? C3 H3 0.9500 . ? C4 C5 1.385(5) . ? C4 H4 0.9500 . ? C5 C6 1.398(4) . ? C5 H5 0.9500 . ? C6 C7 1.511(4) . ? C7 C8 1.496(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.301(5) . ? C8 H8 0.9500 . ? C9 H9A 0.9500 . ? C9 H9B 0.9500 . ? C8A C9A 1.293(5) . ? C8A H8A 0.9500 . ? C9A H9A1 0.9500 . ? C9A H9A2 0.9500 . ? C10 C15 1.385(5) . ? C10 C11 1.387(4) . ? C11 C12 1.381(5) . ? C11 H11 0.9500 . ? C12 C13 1.362(7) . ? C12 H12 0.9500 . ? C13 C14 1.396(7) . ? C13 H13 0.9500 . ? C14 C15 1.403(4) . ? C14 H14 0.9500 . ? C15 C16 1.508(4) . ? C16 C17 1.505(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.307(5) . ? C17 H17 0.9500 . ? C18 H18A 0.9500 . ? C18 H18B 0.9500 . ? C19 C20 1.385(5) . ? C19 C20 1.385(5) 6_554 ? C19 C20A 1.389(5) 6_554 ? C19 C20A 1.389(5) . ? C20 C20A 1.391(6) 16_656 ? C20 C20A 1.671(7) 6_554 ? C20 H20 0.8774 . ? C20A C20 1.391(6) 11_666 ? C20A C20 1.671(7) 6_554 ? C20A H20A 0.9250 . ? 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 C22 W1 C22 95.37(16) . 6_554 ? C22 W1 C21 87.21(12) . 6_554 ? C22 W1 C21 85.50(12) 6_554 6_554 ? C22 W1 C21 85.50(12) . . ? C22 W1 C21 87.21(12) 6_554 . ? C21 W1 C21 169.17(15) 6_554 . ? C22 W1 P1 100.00(8) . 6_554 ? C22 W1 P1 164.50(8) 6_554 6_554 ? C21 W1 P1 93.21(8) 6_554 6_554 ? C21 W1 P1 95.94(8) . 6_554 ? C22 W1 P1 164.50(8) . . ? C22 W1 P1 100.00(8) 6_554 . ? C21 W1 P1 95.94(8) 6_554 . ? C21 W1 P1 93.21(8) . . ? P1 W1 P1 64.73(3) 6_554 . ? O2 P1 O1 95.85(10) . . ? O2 P1 N1 99.37(8) . . ? O1 P1 N1 107.48(8) . . ? O2 P1 W1 127.18(7) . . ? O1 P1 W1 125.57(7) . . ? N1 P1 W1 97.47(7) . . ? C1 O1 P1 123.44(16) . . ? C10 O2 P1 120.49(17) . . ? C19 N1 P1 129.84(7) . . ? C19 N1 P1 129.84(7) . 6_554 ? P1 N1 P1 100.33(14) . 6_554 ? C2 C1 C6 122.7(2) . . ? C2 C1 O1 119.3(2) . . ? C6 C1 O1 117.8(2) . . ? C3 C2 C1 119.5(3) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 119.5(3) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 120.1(3) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 121.7(3) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C1 C6 C5 116.5(3) . . ? C1 C6 C7 122.4(3) . . ? C5 C6 C7 121.1(3) . . ? C8 C7 C6 114.3(4) . . ? C8 C7 H7A 108.7 . . ? C6 C7 H7A 108.7 . . ? C8 C7 H7B 108.7 . . ? C6 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C9 C8 C7 118.2(6) . . ? C9 C8 H8 120.9 . . ? C7 C8 H8 120.9 . . ? C8 C9 H9A 120.0 . . ? C8 C9 H9B 120.0 . . ? H9A C9 H9B 120.0 . . ? C9A C8A H8A 115.0 . . ? C8A C9A H9A1 120.0 . . ? C8A C9A H9A2 120.0 . . ? H9A1 C9A H9A2 120.0 . . ? C15 C10 C11 123.2(3) . . ? C15 C10 O2 118.1(3) . . ? C11 C10 O2 118.7(3) . . ? C12 C11 C10 118.7(4) . . ? C12 C11 H11 120.6 . . ? C10 C11 H11 120.6 . . ? C13 C12 C11 120.0(4) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 121.1(4) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? C13 C14 C15 120.4(4) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C10 C15 C14 116.5(3) . . ? C10 C15 C16 122.3(3) . . ? C14 C15 C16 121.1(3) . . ? C17 C16 C15 114.2(3) . . ? C17 C16 H16A 108.7 . . ? C15 C16 H16A 108.7 . . ? C17 C16 H16B 108.7 . . ? C15 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? C18 C17 C16 125.2(3) . . ? C18 C17 H17 117.4 . . ? C16 C17 H17 117.4 . . ? C17 C18 H18A 120.0 . . ? C17 C18 H18B 120.0 . . ? H18A C18 H18B 120.0 . . ? C20 C19 C20 119.7(4) . 6_554 ? C20 C19 C20A 74.1(3) . 6_554 ? C20 C19 C20A 76.0(3) 6_554 6_554 ? C20 C19 C20A 76.0(3) . . ? C20 C19 C20A 74.1(3) 6_554 . ? C20A C19 C20A 118.2(4) 6_554 . ? C20 C19 N1 120.2(2) . . ? C20 C19 N1 120.2(2) 6_554 . ? C20A C19 N1 120.9(2) 6_554 . ? C20A C19 N1 120.9(2) . . ? C19 C20 C20A 119.9(4) . 16_656 ? C19 C20 C20A 53.1(2) . 6_554 ? C20A C20 C20A 90.0(4) 16_656 6_554 ? C19 C20 H20 120.1 . . ? C20A C20 H20 119.9 16_656 . ? C20A C20 H20 129.2 6_554 . ? C19 C20A C20 121.1(4) . 11_666 ? C19 C20A C20 52.8(2) . 6_554 ? C20 C20A C20 91.6(4) 11_666 6_554 ? C19 C20A H20A 115.4 . . ? C20 C20A H20A 123.3 11_666 . ? C20 C20A H20A 121.2 6_554 . ? O3 C21 W1 174.2(2) . . ? O4 C22 W1 178.7(3) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 29.17 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.262 _refine_diff_density_min -1.320 _refine_diff_density_rms 0.083 _database_code_depnum_ccdc_archive 'CCDC 955815' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_msb429_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C102 H94 Fe4 N2 O12 P4' _chemical_formula_sum 'C102 H94 Fe4 N2 O12 P4' _chemical_formula_weight 1887.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.222(5) _cell_length_b 15.757(6) _cell_length_c 20.793(8) _cell_angle_alpha 93.652(6) _cell_angle_beta 98.092(6) _cell_angle_gamma 115.125(5) _cell_volume 4428(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 275 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 16.18 _exptl_crystal_description Slab _exptl_crystal_colour red _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960 _exptl_absorpt_coefficient_mu 0.780 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5752 _exptl_absorpt_correction_T_max 0.9212 _exptl_absorpt_process_details 'TWINABS (Sheldrick, 2008b)' _exptl_special_details ; The diffraction data were collected in three sets of 606 frames (0.3 deg. width in omega) at phi = 0, 120 and 240 deg. A scan time of 120 sec/frame was used. The crystal was determined to consist of two major components (CELL_NOW (Sheldrick, 2008a)) related by a 131 deg. rotation about the real axis -0.859, 0.577, 1.000. Integration of the raw data was accomplished with the multi-component version of SAINT and the two-component control file written by CELL_NOW. ; _diffrn_ambient_temperature 100(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 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 33586 _diffrn_reflns_av_R_equivalents 0.0696 _diffrn_reflns_av_sigmaI/netI 0.5277 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.00 _diffrn_reflns_theta_max 25.05 _reflns_number_total 15591 _reflns_number_gt 4178 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2009)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2009a)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS 2009a)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008)' _computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008)' _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. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. Several of the allyl substituents are disordered over two approximately equal sites. These were refined with restraints to approximate the geometry of the ordered allyl groups. One phenyl ring is also disordered over two sites and the components of this disorder were treated as rigid groups with ideal geometry. Because of the limited data the displacement parameters for the light atoms were loosely restrained to approximate isotropic behavior ; _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^)+(0.0747P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15591 _refine_ls_number_parameters 1151 _refine_ls_number_restraints 948 _refine_ls_R_factor_all 0.3595 _refine_ls_R_factor_gt 0.1177 _refine_ls_wR_factor_ref 0.2858 _refine_ls_wR_factor_gt 0.1936 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.928 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.04998(17) 0.57924(15) 0.18735(12) 0.0386(7) Uani 1 1 d . . . Fe2 Fe 0.19933(16) 0.62411(14) 0.13429(11) 0.0276(6) Uani 1 1 d . . . Fe3 Fe 0.25421(17) 1.34729(14) 0.38663(11) 0.0319(7) Uani 1 1 d . . . Fe4 Fe 0.40031(17) 1.41418(14) 0.33033(11) 0.0308(7) Uani 1 1 d . . . P1 P 0.0905(3) 0.7180(3) 0.2325(2) 0.0292(11) Uani 1 1 d . A . P2 P 0.2435(3) 0.7710(3) 0.15295(19) 0.0222(10) Uani 1 1 d . A . P3 P 0.2072(3) 1.2055(3) 0.3459(2) 0.0308(11) Uani 1 1 d . . . P4 P 0.3928(3) 1.2814(3) 0.29752(19) 0.0253(11) Uani 1 1 d . . . O1 O 0.0264(8) 0.6119(7) 0.0498(6) 0.045(3) Uani 1 1 d U . . O2 O 0.2267(7) 0.5991(6) 0.2728(5) 0.030(3) Uani 1 1 d U . . O3 O 0.0135(7) 0.7635(6) 0.2350(5) 0.029(3) Uani 1 1 d DU . . O4 O 0.1361(7) 0.7442(6) 0.3108(5) 0.033(3) Uani 1 1 d U . . O5 O 0.2223(7) 0.8310(6) 0.0973(4) 0.027(2) Uani 1 1 d U . . O6 O 0.3603(6) 0.8451(6) 0.1761(4) 0.022(2) Uani 1 1 d U . . O7 O 0.1698(7) 1.1164(6) 0.3870(5) 0.034(3) Uani 1 1 d U . . O8 O 0.1105(7) 1.1589(7) 0.2860(5) 0.035(3) Uani 1 1 d U . . O9 O 0.4678(6) 1.2411(6) 0.3316(4) 0.022(2) Uani 1 1 d U . . O10 O 0.4078(7) 1.2587(6) 0.2233(4) 0.024(2) Uani 1 1 d U . . O11 O 0.4441(8) 1.3767(7) 0.4623(5) 0.038(3) Uani 1 1 d U . . O12 O 0.2072(8) 1.3751(7) 0.2522(5) 0.042(3) Uani 1 1 d U . . N1 N 0.1877(7) 0.8043(7) 0.2088(5) 0.016(3) Uani 1 1 d U . . N2 N 0.2861(8) 1.1860(7) 0.3048(5) 0.017(3) Uani 1 1 d U A . C1 C -0.0841(14) 0.5170(12) 0.2180(9) 0.063(6) Uani 1 1 d U . . H1 H -0.1108 0.5537 0.2386 0.075 Uiso 1 1 calc R . . C2 C -0.0217(13) 0.4833(11) 0.2518(9) 0.049(5) Uani 1 1 d U . . H2 H 0.0003 0.4915 0.2979 0.059 Uiso 1 1 calc R . . C3 C 0.0011(12) 0.4348(10) 0.2028(8) 0.048(5) Uani 1 1 d U . . H3 H 0.0425 0.4036 0.2097 0.058 Uiso 1 1 calc R . . C4 C -0.0482(12) 0.4402(11) 0.1411(9) 0.050(5) Uani 1 1 d U . . H4 H -0.0446 0.4136 0.0998 0.060 Uiso 1 1 calc R . . C5 C -0.1020(12) 0.4901(11) 0.1506(9) 0.048(5) Uani 1 1 d U . . H5 H -0.1429 0.5034 0.1179 0.058 Uiso 1 1 calc R . . C6 C 0.0703(12) 0.6109(11) 0.1011(9) 0.038(5) Uani 1 1 d U . . C7 C 0.1810(11) 0.6052(10) 0.2214(8) 0.031(4) Uani 1 1 d U . . C8 C 0.1791(12) 0.4969(11) 0.0777(7) 0.037(4) Uani 1 1 d U . . H8 H 0.1181 0.4419 0.0646 0.045 Uiso 1 1 calc R . . C9 C 0.2175(12) 0.5710(11) 0.0421(8) 0.039(4) Uani 1 1 d U . . H9 H 0.1871 0.5748 -0.0001 0.047 Uiso 1 1 calc R . . C10 C 0.3044(12) 0.6373(11) 0.0763(8) 0.036(4) Uani 1 1 d U . . H10 H 0.3435 0.6961 0.0629 0.043 Uiso 1 1 calc R . . C11 C 0.3282(11) 0.6050(10) 0.1362(8) 0.035(4) Uani 1 1 d U . . H11 H 0.3870 0.6369 0.1681 0.042 Uiso 1 1 calc R . . C12 C 0.2493(11) 0.5179(9) 0.1392(7) 0.030(4) Uani 1 1 d U . . H12 H 0.2426 0.4805 0.1739 0.036 Uiso 1 1 calc R . . C13 C -0.0373(11) 0.7892(12) 0.1808(7) 0.027(6) Uani 0.599(8) 1 d PGDU A 1 C14 C -0.0986(12) 0.8291(12) 0.1965(6) 0.026(5) Uani 0.599(8) 1 d PGDU A 1 C15 C -0.1497(12) 0.8559(12) 0.1474(9) 0.062(8) Uani 0.599(8) 1 d PGU A 1 H15 H -0.1916 0.8831 0.1582 0.075 Uiso 0.599(8) 1 calc PR A 1 C16 C -0.1394(13) 0.8427(14) 0.0827(8) 0.079(9) Uani 0.599(8) 1 d PGU A 1 H16 H -0.1743 0.8610 0.0491 0.095 Uiso 0.599(8) 1 calc PR A 1 C17 C -0.0781(13) 0.8027(13) 0.0669(6) 0.054(8) Uani 0.599(8) 1 d PGU A 1 H17 H -0.0711 0.7937 0.0227 0.065 Uiso 0.599(8) 1 calc PR A 1 C18 C -0.0270(11) 0.7760(11) 0.1160(8) 0.025(6) Uani 0.599(8) 1 d PGU A 1 H18 H 0.0149 0.7487 0.1053 0.029 Uiso 0.599(8) 1 calc PR A 1 C19 C -0.1152(19) 0.8426(19) 0.2655(9) 0.049(7) Uani 0.599(8) 1 d PDU A 1 H19A H -0.0542 0.8558 0.2969 0.059 Uiso 0.599(8) 1 calc PR A 1 H19B H -0.1295 0.8980 0.2713 0.059 Uiso 0.599(8) 1 calc PR A 1 C20 C -0.200(2) 0.7566(19) 0.2806(16) 0.068(9) Uani 0.599(8) 1 d PDU A 1 H20A H -0.2115 0.7563 0.3243 0.082 Uiso 0.599(8) 1 calc PR A 1 C21 C -0.258(2) 0.682(2) 0.2376(16) 0.086(10) Uani 0.599(8) 1 d PDU A 1 H21A H -0.2481 0.6797 0.1935 0.103 Uiso 0.599(8) 1 calc PR A 1 H21B H -0.3096 0.6301 0.2506 0.103 Uiso 0.599(8) 1 calc PR A 1 C13A C -0.0618(15) 0.7497(18) 0.1891(10) 0.027(6) Uani 0.401(8) 1 d PGDU A 2 C14A C -0.1401(18) 0.7642(18) 0.2060(9) 0.026(5) Uani 0.401(8) 1 d PGDU A 2 C15A C -0.2124(16) 0.764(2) 0.1572(13) 0.062(8) Uani 0.401(8) 1 d PGU A 2 H15A H -0.2659 0.7743 0.1687 0.075 Uiso 0.401(8) 1 calc PR A 2 C16A C -0.2065(18) 0.750(2) 0.0916(11) 0.079(9) Uani 0.401(8) 1 d PGU A 2 H16A H -0.2560 0.7505 0.0583 0.095 Uiso 0.401(8) 1 calc PR A 2 C17A C -0.128(2) 0.736(2) 0.0747(8) 0.054(8) Uani 0.401(8) 1 d PGU A 2 H17A H -0.1242 0.7262 0.0299 0.065 Uiso 0.401(8) 1 calc PR A 2 C18A C -0.0559(15) 0.7355(18) 0.1235(12) 0.025(6) Uani 0.401(8) 1 d PGU A 2 H18A H -0.0024 0.7257 0.1120 0.029 Uiso 0.401(8) 1 calc PR A 2 C19A C -0.142(4) 0.781(3) 0.2779(11) 0.049(7) Uani 0.401(8) 1 d PDU A 2 H19C H -0.0736 0.8139 0.3024 0.059 Uiso 0.401(8) 1 calc PR A 2 H19D H -0.1737 0.8240 0.2836 0.059 Uiso 0.401(8) 1 calc PR A 2 C20A C -0.196(3) 0.694(3) 0.308(2) 0.068(9) Uani 0.401(8) 1 d PDU A 2 H20B H -0.2013 0.7033 0.3527 0.082 Uiso 0.401(8) 1 calc PR A 2 C21A C -0.236(3) 0.608(3) 0.278(3) 0.086(10) Uani 0.401(8) 1 d PDU A 2 H21C H -0.2324 0.5956 0.2338 0.103 Uiso 0.401(8) 1 calc PR A 2 H21D H -0.2688 0.5566 0.3015 0.103 Uiso 0.401(8) 1 calc PR A 2 C22 C 0.0888(14) 0.6992(12) 0.3610(9) 0.050(5) Uani 1 1 d U A . C23 C 0.1566(16) 0.6929(12) 0.4127(9) 0.055(5) Uani 1 1 d U . . C24 C 0.1054(19) 0.6493(15) 0.4666(11) 0.088(7) Uani 1 1 d U A . H24 H 0.1428 0.6441 0.5055 0.105 Uiso 1 1 calc R . . C25 C 0.0093(18) 0.6181(14) 0.4611(11) 0.080(7) Uani 1 1 d U . . H25 H -0.0198 0.5855 0.4952 0.096 Uiso 1 1 calc R A . C26 C -0.0501(15) 0.6276(12) 0.4131(10) 0.063(6) Uani 1 1 d U A . H26 H -0.1179 0.6071 0.4151 0.075 Uiso 1 1 calc R . . C27 C -0.0125(14) 0.6688(11) 0.3579(9) 0.055(5) Uani 1 1 d U . . H27 H -0.0535 0.6752 0.3215 0.066 Uiso 1 1 calc R A . C28 C 0.2587(15) 0.7250(13) 0.4134(9) 0.075(6) Uani 0.507(14) 1 d PDU A 1 H28A H 0.2715 0.7237 0.3680 0.090 Uiso 0.507(14) 1 calc PR A 1 H28B H 0.2833 0.6841 0.4365 0.090 Uiso 0.507(14) 1 calc PR A 1 C29 C 0.308(2) 0.8218(16) 0.4476(14) 0.046(7) Uani 0.507(14) 1 d PDU A 1 H29 H 0.2904 0.8674 0.4292 0.055 Uiso 0.507(14) 1 calc PR A 1 C30 C 0.374(2) 0.850(2) 0.5010(14) 0.052(8) Uani 0.507(14) 1 d PDU A 1 H30A H 0.3930 0.8069 0.5209 0.062 Uiso 0.507(14) 1 calc PR A 1 H30B H 0.4021 0.9147 0.5203 0.062 Uiso 0.507(14) 1 calc PR A 1 C28A C 0.2587(15) 0.7250(13) 0.4134(9) 0.075(6) Uani 0.493(14) 1 d PDU A 2 H28C H 0.2792 0.7886 0.3995 0.090 Uiso 0.493(14) 1 calc PR A 2 H28D H 0.2610 0.6846 0.3758 0.090 Uiso 0.493(14) 1 calc PR A 2 C29A C 0.3457(18) 0.737(2) 0.4648(14) 0.046(7) Uani 0.493(14) 1 d PDU A 2 H29A H 0.3424 0.6761 0.4706 0.055 Uiso 0.493(14) 1 calc PR A 2 C30A C 0.425(2) 0.802(2) 0.5043(15) 0.052(8) Uani 0.493(14) 1 d PDU A 2 H30C H 0.4388 0.8673 0.5046 0.062 Uiso 0.493(14) 1 calc PR A 2 H30D H 0.4670 0.7848 0.5324 0.062 Uiso 0.493(14) 1 calc PR A 2 C31 C 0.2596(10) 0.8433(9) 0.0387(7) 0.021(4) Uani 1 1 d U . . C32 C 0.3380(10) 0.9313(9) 0.0330(7) 0.024(4) Uani 1 1 d U . . C33 C 0.3673(11) 0.9397(10) -0.0270(7) 0.032(4) Uani 1 1 d U . . H33 H 0.4186 0.9977 -0.0335 0.038 Uiso 1 1 calc R . . C34 C 0.3229(11) 0.8641(10) -0.0792(7) 0.036(4) Uani 1 1 d U . . H34 H 0.3468 0.8706 -0.1192 0.043 Uiso 1 1 calc R . . C35 C 0.2451(11) 0.7812(10) -0.0720(7) 0.037(4) Uani 1 1 d U . . H35 H 0.2135 0.7316 -0.1079 0.045 Uiso 1 1 calc R . . C36 C 0.2135(10) 0.7700(10) -0.0137(7) 0.025(4) Uani 1 1 d U . . H36 H 0.1601 0.7126 -0.0087 0.030 Uiso 1 1 calc R . . C37 C 0.3797(11) 1.0114(10) 0.0879(7) 0.033(4) Uani 1 1 d U . . H37A H 0.4499 1.0513 0.0865 0.039 Uiso 1 1 calc R . . H37B H 0.3769 0.9857 0.1302 0.039 Uiso 1 1 calc R . . C38 C 0.3251(13) 1.0720(12) 0.0848(9) 0.055(5) Uani 1 1 d U . . H38 H 0.3491 1.1239 0.1188 0.066 Uiso 1 1 calc R . . C39 C 0.2498(15) 1.0630(14) 0.0421(11) 0.085(7) Uani 1 1 d U . . H39A H 0.2220 1.0126 0.0067 0.102 Uiso 1 1 calc R . . H39B H 0.2225 1.1068 0.0461 0.102 Uiso 1 1 calc R . . C40 C 0.4272(11) 0.8276(9) 0.2168(7) 0.024(4) Uani 1 1 d U . . C41 C 0.5176(12) 0.8469(11) 0.2004(8) 0.038(4) Uani 1 1 d U C . C42 C 0.5890(13) 0.8336(11) 0.2442(9) 0.056(5) Uani 1 1 d U . . H42 H 0.6525 0.8485 0.2342 0.068 Uiso 1 1 calc R . . C43 C 0.5644(14) 0.7978(12) 0.3032(9) 0.057(5) Uani 1 1 d U . . H43 H 0.6113 0.7872 0.3326 0.068 Uiso 1 1 calc R . . C44 C 0.4729(12) 0.7780(10) 0.3183(8) 0.040(4) Uani 1 1 d U . . H44 H 0.4559 0.7539 0.3578 0.048 Uiso 1 1 calc R . . C45 C 0.4073(12) 0.7944(10) 0.2749(7) 0.035(4) Uani 1 1 d U . . H45 H 0.3447 0.7819 0.2856 0.042 Uiso 1 1 calc R . . C46 C 0.5450(12) 0.8845(11) 0.1383(8) 0.049(5) Uani 1 1 d U . . H46A H 0.6021 0.9477 0.1500 0.059 Uiso 1 1 calc R B 1 H46B H 0.4892 0.8936 0.1146 0.059 Uiso 1 1 calc R B 1 C47 C 0.5709(13) 0.8255(13) 0.0920(9) 0.055(5) Uani 0.50(2) 1 d PDU C 1 H47A H 0.5927 0.8507 0.0538 0.066 Uiso 0.50(2) 1 calc PR C 1 C48 C 0.566(3) 0.742(2) 0.100(2) 0.093(11) Uani 0.50(2) 1 d PDU C 1 H48A H 0.5445 0.7146 0.1380 0.111 Uiso 0.50(2) 1 calc PR C 1 H48B H 0.5836 0.7090 0.0687 0.111 Uiso 0.50(2) 1 calc PR C 1 C47A C 0.5709(13) 0.8255(13) 0.0920(9) 0.055(5) Uani 0.50(2) 1 d PDU C 2 H47B H 0.6212 0.8082 0.1095 0.066 Uiso 0.50(2) 1 calc PR C 2 C48A C 0.531(3) 0.795(3) 0.0297(13) 0.093(11) Uani 0.50(2) 1 d PDU C 2 H48C H 0.4804 0.8108 0.0099 0.111 Uiso 0.50(2) 1 calc PR C 2 H48D H 0.5526 0.7582 0.0044 0.111 Uiso 0.50(2) 1 calc PR C 2 C49 C 0.2162(10) 0.9024(9) 0.2312(7) 0.020(4) Uani 1 1 d U A . C50 C 0.2849(10) 0.9479(9) 0.2913(7) 0.022(4) Uani 1 1 d U . . H50 H 0.3148 0.9152 0.3160 0.026 Uiso 1 1 calc R A . C51 C 0.3060(10) 1.0388(10) 0.3119(7) 0.022(4) Uani 1 1 d U A . H51 H 0.3514 1.0682 0.3519 0.026 Uiso 1 1 calc R . . C52 C 0.2680(11) 1.0908(10) 0.2802(7) 0.028(4) Uani 1 1 d U . . C53 C 0.2007(11) 1.0464(9) 0.2201(7) 0.032(4) Uani 1 1 d U A . H53 H 0.1699 1.0796 0.1968 0.039 Uiso 1 1 calc R . . C54 C 0.1797(11) 0.9534(10) 0.1952(7) 0.028(4) Uani 1 1 d U . . H54 H 0.1398 0.9260 0.1531 0.034 Uiso 1 1 calc R A . C55 C 0.2221(12) 1.0934(11) 0.4364(8) 0.036(4) Uani 1 1 d U D . C56 C 0.1808(14) 0.9989(13) 0.4464(9) 0.060(5) Uani 1 1 d U . . C57 C 0.234(2) 0.9711(19) 0.4934(13) 0.125(10) Uani 1 1 d U D . H57 H 0.2113 0.9057 0.4972 0.150 Uiso 1 1 calc R . . C58 C 0.319(3) 1.036(2) 0.5348(17) 0.176(13) Uani 1 1 d U . . H58 H 0.3517 1.0179 0.5697 0.211 Uiso 1 1 calc R D . C59 C 0.356(2) 1.132(2) 0.5227(13) 0.133(10) Uani 1 1 d U D . H59 H 0.4146 1.1780 0.5499 0.160 Uiso 1 1 calc R . . C60 C 0.3093(13) 1.1612(13) 0.4737(9) 0.062(6) Uani 1 1 d U . . H60 H 0.3360 1.2252 0.4656 0.075 Uiso 1 1 calc R D . C61 C 0.0860(11) 0.9273(10) 0.4043(7) 0.037(4) Uani 0.53(2) 1 d PDU D 1 H61A H 0.0869 0.9390 0.3582 0.044 Uiso 0.53(2) 1 calc PR D 1 H61B H 0.0821 0.8633 0.4070 0.044 Uiso 0.53(2) 1 calc PR D 1 C62 C -0.0040(17) 0.930(2) 0.4237(15) 0.053(8) Uani 0.53(2) 1 d PDU D 1 H62A H -0.0089 0.9873 0.4194 0.063 Uiso 0.53(2) 1 calc PR D 1 C63 C -0.0760(15) 0.8670(15) 0.4454(11) 0.093(8) Uani 0.53(2) 1 d PDU D 1 H63A H -0.0769 0.8073 0.4512 0.112 Uiso 0.53(2) 1 calc PR D 1 H63B H -0.1282 0.8803 0.4555 0.112 Uiso 0.53(2) 1 calc PR D 1 C61A C 0.0860(11) 0.9273(10) 0.4043(7) 0.037(4) Uani 0.47(2) 1 d PDU D 2 H61C H 0.0588 0.9589 0.3731 0.044 Uiso 0.47(2) 1 calc PR D 2 H61D H 0.0982 0.8794 0.3789 0.044 Uiso 0.47(2) 1 calc PR D 2 C62A C 0.0146(18) 0.881(2) 0.4479(15) 0.053(8) Uani 0.47(2) 1 d PDU D 2 H62B H 0.0399 0.8578 0.4834 0.063 Uiso 0.47(2) 1 calc PR D 2 C63A C -0.0760(15) 0.8670(15) 0.4454(11) 0.093(8) Uani 0.47(2) 1 d PDU D 2 H63C H -0.1070 0.8880 0.4113 0.112 Uiso 0.47(2) 1 calc PR D 2 H63D H -0.1115 0.8357 0.4776 0.112 Uiso 0.47(2) 1 calc PR D 2 C64 C 0.0107(14) 1.1416(12) 0.2860(10) 0.054(5) Uani 1 1 d U E . C65 C -0.0394(16) 1.1546(13) 0.2280(11) 0.072(6) Uani 1 1 d U . . C66 C -0.1420(18) 1.1267(15) 0.2286(13) 0.098(8) Uani 1 1 d U E . H66 H -0.1827 1.1280 0.1900 0.118 Uiso 1 1 calc R . . C67 C -0.182(2) 1.0993(18) 0.2799(15) 0.115(9) Uani 1 1 d U . . H67 H -0.2499 1.0856 0.2773 0.138 Uiso 1 1 calc R E . C68 C -0.1356(17) 1.0898(14) 0.3340(12) 0.087(7) Uani 1 1 d U E . H68 H -0.1682 1.0693 0.3698 0.104 Uiso 1 1 calc R . . C69 C -0.0293(13) 1.1121(11) 0.3384(9) 0.052(5) Uani 1 1 d U . . H69 H 0.0082 1.1056 0.3767 0.063 Uiso 1 1 calc R E . C70 C 0.0090(15) 1.1855(13) 0.1728(9) 0.078(7) Uani 0.605(14) 1 d PDU E 1 H70A H 0.0799 1.2270 0.1894 0.093 Uiso 0.605(14) 1 calc PR E 1 H70B H -0.0197 1.2233 0.1495 0.093 Uiso 0.605(14) 1 calc PR E 1 C71 C 0.000(2) 1.1071(17) 0.1264(13) 0.045(7) Uani 0.605(14) 1 d PDU E 1 H71A H 0.0248 1.1180 0.0869 0.054 Uiso 0.605(14) 1 calc PR E 1 C72 C -0.044(3) 1.022(2) 0.141(2) 0.140(15) Uani 0.605(14) 1 d PDU E 1 H72A H -0.0692 1.0126 0.1808 0.168 Uiso 0.605(14) 1 calc PR E 1 H72B H -0.0519 0.9694 0.1121 0.168 Uiso 0.605(14) 1 calc PR E 1 C70A C 0.0090(15) 1.1855(13) 0.1728(9) 0.078(7) Uani 0.395(14) 1 d PDU E 2 H70C H 0.0482 1.1490 0.1712 0.093 Uiso 0.395(14) 1 calc PR E 2 H70D H 0.0581 1.2512 0.1901 0.093 Uiso 0.395(14) 1 calc PR E 2 C71A C -0.020(3) 1.191(3) 0.1017(12) 0.045(7) Uani 0.395(14) 1 d PDU E 2 H71B H -0.0286 1.2461 0.0940 0.054 Uiso 0.395(14) 1 calc PR E 2 C72A C -0.034(5) 1.135(4) 0.048(3) 0.140(15) Uani 0.395(14) 1 d PDU E 2 H72C H -0.0267 1.0781 0.0511 0.168 Uiso 0.395(14) 1 calc PR E 2 H72D H -0.0522 1.1502 0.0065 0.168 Uiso 0.395(14) 1 calc PR E 2 C73 C 0.5694(11) 1.2853(9) 0.3361(7) 0.025(4) Uani 1 1 d U . . C74 C 0.6171(11) 1.2568(10) 0.2948(7) 0.026(4) Uani 1 1 d U . . C75 C 0.7177(11) 1.3002(10) 0.3031(7) 0.032(4) Uani 1 1 d U . . H75 H 0.7507 1.2788 0.2752 0.039 Uiso 1 1 calc R . . C76 C 0.7720(11) 1.3764(10) 0.3531(7) 0.034(4) Uani 1 1 d U . . H76 H 0.8417 1.4088 0.3572 0.041 Uiso 1 1 calc R . . C77 C 0.7264(11) 1.4052(10) 0.3962(7) 0.036(4) Uani 1 1 d U . . H77 H 0.7642 1.4561 0.4305 0.043 Uiso 1 1 calc R . . C78 C 0.6249(11) 1.3592(10) 0.3891(7) 0.032(4) Uani 1 1 d U . . H78 H 0.5923 1.3767 0.4195 0.038 Uiso 1 1 calc R . . C79 C 0.5577(11) 1.1685(10) 0.2436(7) 0.037(4) Uani 1 1 d U . . H79A H 0.4921 1.1660 0.2276 0.044 Uiso 1 1 calc R . . H79B H 0.5920 1.1750 0.2059 0.044 Uiso 1 1 calc R . . C80 C 0.5428(10) 1.0774(10) 0.2678(7) 0.025(4) Uani 1 1 d U . . H80 H 0.5051 1.0223 0.2367 0.030 Uiso 1 1 calc R . . C81 C 0.5739(12) 1.0622(11) 0.3253(8) 0.048(5) Uani 1 1 d U . . H81A H 0.6121 1.1139 0.3590 0.058 Uiso 1 1 calc R . . H81B H 0.5585 0.9994 0.3337 0.058 Uiso 1 1 calc R . . C82 C 0.3699(13) 1.2952(11) 0.1695(8) 0.034(4) Uani 1 1 d U F . C83 C 0.4397(15) 1.3425(13) 0.1335(9) 0.058(5) Uani 1 1 d U . . C84 C 0.4096(16) 1.3784(13) 0.0769(9) 0.066(6) Uani 1 1 d U F . H84 H 0.4555 1.4135 0.0509 0.080 Uiso 1 1 calc R . . C85 C 0.3120(17) 1.3600(14) 0.0621(10) 0.071(6) Uani 1 1 d U . . C86 C 0.2409(14) 1.3087(12) 0.0966(9) 0.056(5) Uani 1 1 d U F . C87 C 0.2794(15) 1.2783(12) 0.1527(9) 0.059(5) Uani 1 1 d U . . H87 H 0.2345 1.2430 0.1792 0.071 Uiso 1 1 calc R F . C88 C 0.5481(13) 1.3635(11) 0.1468(9) 0.056(5) Uani 0.652(13) 1 d PDU F 1 H88A H 0.5678 1.3581 0.1932 0.067 Uiso 0.652(13) 1 calc PR F 1 H88B H 0.5578 1.3159 0.1190 0.067 Uiso 0.652(13) 1 calc PR F 1 C89 C 0.6112(17) 1.4586(15) 0.1332(12) 0.045(6) Uani 0.652(13) 1 d PDU F 1 H89 H 0.6128 1.5117 0.1586 0.055 Uiso 0.652(13) 1 calc PR F 1 C90 C 0.6644(19) 1.473(2) 0.0883(12) 0.064(8) Uani 0.652(13) 1 d PDU F 1 H90A H 0.6639 1.4212 0.0623 0.076 Uiso 0.652(13) 1 calc PR F 1 H90B H 0.7041 1.5361 0.0813 0.076 Uiso 0.652(13) 1 calc PR F 1 C88A C 0.5481(13) 1.3635(11) 0.1468(9) 0.056(5) Uani 0.348(13) 1 d PDU F 2 H88C H 0.5828 1.4312 0.1418 0.067 Uiso 0.348(13) 1 calc PR F 2 H88D H 0.5624 1.3607 0.1943 0.067 Uiso 0.348(13) 1 calc PR F 2 C89A C 0.606(3) 1.320(3) 0.118(2) 0.045(6) Uani 0.348(13) 1 d PDU F 2 H89A H 0.6712 1.3329 0.1384 0.055 Uiso 0.348(13) 1 calc PR F 2 C90A C 0.563(4) 1.263(3) 0.063(2) 0.064(8) Uani 0.348(13) 1 d PDU F 2 H90C H 0.4975 1.2519 0.0437 0.076 Uiso 0.348(13) 1 calc PR F 2 H90D H 0.5960 1.2336 0.0423 0.076 Uiso 0.348(13) 1 calc PR F 2 C91 C 0.5317(12) 1.4914(11) 0.2983(8) 0.043(5) Uani 1 1 d U . . H91 H 0.5689 1.4627 0.2814 0.051 Uiso 1 1 calc R . . C92 C 0.4536(12) 1.5043(9) 0.2610(8) 0.034(4) Uani 1 1 d U . . H92 H 0.4300 1.4856 0.2152 0.041 Uiso 1 1 calc R . . C93 C 0.4175(12) 1.5492(10) 0.3033(8) 0.042(5) Uani 1 1 d U . . H93 H 0.3671 1.5686 0.2913 0.050 Uiso 1 1 calc R . . C94 C 0.4714(11) 1.5601(10) 0.3683(7) 0.034(4) Uani 1 1 d U . . H94 H 0.4597 1.5847 0.4074 0.041 Uiso 1 1 calc R . . C95 C 0.5447(12) 1.5282(10) 0.3642(8) 0.039(4) Uani 1 1 d U . . H95 H 0.5935 1.5310 0.3993 0.047 Uiso 1 1 calc R . . C96 C 0.3881(11) 1.3728(10) 0.4129(8) 0.029(4) Uani 1 1 d U . . C97 C 0.2655(12) 1.3743(10) 0.2993(8) 0.033(4) Uani 1 1 d U . . C98 C 0.1414(12) 1.3160(12) 0.4417(8) 0.046(5) Uani 1 1 d U . . H98 H 0.0968 1.2533 0.4458 0.055 Uiso 1 1 calc R . . C99 C 0.1248(13) 1.3670(12) 0.3934(9) 0.053(5) Uani 1 1 d U . . H99 H 0.0690 1.3472 0.3592 0.063 Uiso 1 1 calc R . . C100 C 0.2101(13) 1.4558(12) 0.4065(9) 0.054(5) Uani 1 1 d U . . H100 H 0.2208 1.5068 0.3817 0.064 Uiso 1 1 calc R . . C101 C 0.2753(13) 1.4569(11) 0.4607(8) 0.045(5) Uani 1 1 d U . . H101 H 0.3376 1.5080 0.4790 0.053 Uiso 1 1 calc R . . C102 C 0.2330(11) 1.3692(10) 0.4839(8) 0.036(4) Uani 1 1 d U . . H102 H 0.2605 1.3496 0.5206 0.043 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0350(16) 0.0189(13) 0.0483(17) -0.0068(12) 0.0232(14) -0.0040(12) Fe2 0.0343(15) 0.0184(12) 0.0312(15) 0.0004(11) 0.0155(12) 0.0101(11) Fe3 0.0464(17) 0.0202(13) 0.0270(15) -0.0020(11) 0.0122(13) 0.0116(12) Fe4 0.0453(17) 0.0172(13) 0.0237(14) -0.0003(11) 0.0120(12) 0.0065(12) P1 0.029(3) 0.021(2) 0.028(3) -0.009(2) 0.011(2) 0.003(2) P2 0.023(2) 0.021(2) 0.024(2) 0.0042(19) 0.008(2) 0.010(2) P3 0.031(3) 0.022(2) 0.034(3) -0.002(2) 0.005(2) 0.008(2) P4 0.029(3) 0.024(2) 0.016(2) -0.0032(18) 0.004(2) 0.007(2) O1 0.034(6) 0.043(6) 0.049(7) -0.009(5) 0.005(5) 0.011(5) O2 0.045(6) 0.014(5) 0.029(6) 0.000(4) 0.013(5) 0.010(4) O3 0.018(5) 0.032(5) 0.035(6) -0.009(4) 0.005(4) 0.011(4) O4 0.042(6) 0.027(5) 0.028(6) 0.011(4) 0.021(5) 0.009(5) O5 0.032(5) 0.022(5) 0.025(5) -0.002(4) -0.001(5) 0.013(4) O6 0.020(5) 0.019(5) 0.030(5) 0.009(4) -0.001(4) 0.014(4) O7 0.033(6) 0.025(5) 0.039(6) 0.006(5) 0.008(5) 0.008(5) O8 0.029(6) 0.033(5) 0.041(6) 0.004(5) -0.007(5) 0.017(5) O9 0.019(5) 0.021(5) 0.018(5) -0.001(4) 0.003(4) 0.001(4) O10 0.040(6) 0.023(5) 0.008(5) -0.003(4) -0.003(4) 0.017(4) O11 0.039(6) 0.035(6) 0.032(6) -0.001(5) 0.017(5) 0.007(5) O12 0.050(6) 0.034(6) 0.042(6) 0.005(5) 0.008(5) 0.019(5) N1 0.010(6) 0.024(6) 0.012(6) -0.002(5) 0.005(5) 0.004(5) N2 0.025(6) 0.013(5) 0.010(5) 0.000(4) 0.001(5) 0.007(5) C1 0.054(9) 0.057(9) 0.062(9) -0.008(7) 0.036(8) 0.004(7) C2 0.046(8) 0.035(8) 0.049(8) 0.004(7) 0.033(7) -0.006(6) C3 0.053(9) 0.031(8) 0.054(9) -0.003(7) 0.033(7) 0.007(6) C4 0.042(8) 0.043(8) 0.057(9) -0.011(7) 0.026(7) 0.007(7) C5 0.050(8) 0.034(8) 0.052(9) -0.003(7) 0.021(7) 0.008(7) C6 0.032(8) 0.032(7) 0.042(8) -0.008(6) 0.013(7) 0.004(6) C7 0.032(8) 0.016(7) 0.043(8) -0.006(6) 0.015(7) 0.007(6) C8 0.039(8) 0.035(7) 0.035(8) -0.004(6) 0.015(7) 0.012(6) C9 0.048(8) 0.043(8) 0.028(8) 0.001(6) 0.007(7) 0.022(7) C10 0.046(8) 0.027(7) 0.041(8) 0.012(6) 0.026(7) 0.016(6) C11 0.037(8) 0.030(7) 0.042(8) 0.002(6) 0.002(6) 0.020(6) C12 0.043(8) 0.011(6) 0.032(7) -0.003(6) 0.010(6) 0.008(6) C13 0.023(8) 0.025(9) 0.027(8) -0.009(6) 0.005(6) 0.008(6) C14 0.021(8) 0.030(8) 0.024(8) -0.001(6) 0.004(6) 0.009(6) C15 0.057(10) 0.066(10) 0.067(10) 0.004(7) 0.005(7) 0.032(7) C16 0.076(11) 0.088(11) 0.080(11) 0.009(7) 0.014(7) 0.042(7) C17 0.051(10) 0.060(10) 0.052(9) -0.003(6) 0.013(7) 0.025(7) C18 0.019(8) 0.026(9) 0.025(8) 0.004(6) 0.002(6) 0.008(6) C19 0.048(9) 0.044(10) 0.054(9) 0.009(6) 0.004(6) 0.022(7) C20 0.070(11) 0.069(11) 0.070(11) 0.007(7) 0.020(7) 0.033(7) C21 0.083(12) 0.085(12) 0.087(12) 0.015(7) 0.020(7) 0.032(7) C13A 0.023(8) 0.025(9) 0.027(8) -0.009(6) 0.005(6) 0.008(6) C14A 0.021(8) 0.030(8) 0.024(8) -0.001(6) 0.004(6) 0.009(6) C15A 0.057(10) 0.066(10) 0.067(10) 0.004(7) 0.005(7) 0.032(7) C16A 0.076(11) 0.088(11) 0.080(11) 0.009(7) 0.014(7) 0.042(7) C17A 0.051(10) 0.060(10) 0.052(9) -0.003(6) 0.013(7) 0.025(7) C18A 0.019(8) 0.026(9) 0.025(8) 0.004(6) 0.002(6) 0.008(6) C19A 0.048(9) 0.044(10) 0.054(9) 0.009(6) 0.004(6) 0.022(7) C20A 0.070(11) 0.069(11) 0.070(11) 0.007(7) 0.020(7) 0.033(7) C21A 0.083(12) 0.085(12) 0.087(12) 0.015(7) 0.020(7) 0.032(7) C22 0.058(9) 0.040(8) 0.052(9) -0.004(7) 0.013(7) 0.022(7) C23 0.084(10) 0.038(8) 0.052(9) 0.003(7) 0.029(8) 0.030(7) C24 0.117(11) 0.080(10) 0.087(11) 0.012(8) 0.016(8) 0.064(9) C25 0.101(11) 0.060(9) 0.077(10) 0.018(8) 0.040(8) 0.026(8) C26 0.073(10) 0.048(9) 0.067(9) -0.013(7) 0.036(8) 0.023(7) C27 0.066(9) 0.035(8) 0.058(9) -0.010(7) 0.033(7) 0.011(7) C28 0.084(9) 0.075(8) 0.074(9) 0.011(6) 0.007(6) 0.044(6) C29 0.044(9) 0.040(9) 0.049(9) 0.014(6) 0.001(6) 0.015(6) C30 0.051(9) 0.053(9) 0.055(9) 0.007(7) 0.010(7) 0.025(6) C28A 0.084(9) 0.075(8) 0.074(9) 0.011(6) 0.007(6) 0.044(6) C29A 0.044(9) 0.040(9) 0.049(9) 0.014(6) 0.001(6) 0.015(6) C30A 0.051(9) 0.053(9) 0.055(9) 0.007(7) 0.010(7) 0.025(6) C31 0.028(7) 0.022(7) 0.014(7) 0.005(5) 0.004(6) 0.013(6) C32 0.033(7) 0.023(7) 0.023(7) 0.007(6) 0.014(6) 0.016(6) C33 0.037(8) 0.034(7) 0.024(7) 0.005(6) 0.012(6) 0.012(6) C34 0.040(8) 0.035(7) 0.028(7) 0.006(6) 0.003(6) 0.013(6) C35 0.039(8) 0.032(7) 0.028(7) 0.006(6) 0.004(6) 0.004(6) C36 0.021(7) 0.025(7) 0.032(7) 0.002(6) 0.008(6) 0.011(6) C37 0.039(8) 0.027(7) 0.035(8) 0.008(6) 0.011(6) 0.016(6) C38 0.069(9) 0.038(8) 0.056(9) 0.000(7) 0.001(7) 0.025(7) C39 0.098(11) 0.079(10) 0.094(11) 0.007(8) 0.012(8) 0.056(8) C40 0.028(7) 0.015(6) 0.023(7) -0.005(6) -0.002(6) 0.008(6) C41 0.032(8) 0.039(8) 0.046(8) 0.012(6) 0.006(7) 0.019(6) C42 0.044(9) 0.047(8) 0.069(9) 0.013(7) 0.009(7) 0.013(7) C43 0.056(9) 0.057(9) 0.058(9) 0.006(7) -0.007(7) 0.031(7) C44 0.040(8) 0.031(7) 0.039(8) 0.012(6) 0.002(7) 0.007(6) C45 0.038(8) 0.034(7) 0.028(8) -0.008(6) 0.001(7) 0.015(6) C46 0.044(8) 0.054(8) 0.051(9) 0.004(7) 0.020(7) 0.021(7) C47 0.062(8) 0.055(7) 0.051(8) 0.009(6) 0.011(6) 0.027(6) C48 0.091(12) 0.093(12) 0.094(12) 0.011(7) 0.014(7) 0.042(8) C47A 0.062(8) 0.055(7) 0.051(8) 0.009(6) 0.011(6) 0.027(6) C48A 0.091(12) 0.093(12) 0.094(12) 0.011(7) 0.014(7) 0.042(8) C49 0.015(7) 0.016(6) 0.027(7) 0.000(6) 0.005(6) 0.005(5) C50 0.023(7) 0.018(6) 0.023(7) 0.006(6) 0.001(6) 0.009(6) C51 0.015(7) 0.026(7) 0.019(7) -0.003(6) -0.002(6) 0.007(6) C52 0.034(8) 0.021(7) 0.026(7) -0.001(6) -0.002(6) 0.013(6) C53 0.052(8) 0.016(6) 0.034(8) -0.003(6) 0.002(6) 0.023(6) C54 0.036(8) 0.025(7) 0.024(7) -0.003(6) 0.004(6) 0.017(6) C55 0.043(8) 0.028(7) 0.031(8) 0.013(6) 0.022(7) 0.006(6) C56 0.060(9) 0.052(9) 0.055(9) 0.024(7) 0.001(7) 0.013(7) C57 0.127(13) 0.113(12) 0.117(12) 0.044(9) 0.000(9) 0.039(9) C58 0.184(16) 0.163(15) 0.167(15) 0.061(10) 0.000(9) 0.066(10) C59 0.131(13) 0.120(12) 0.121(13) 0.042(9) -0.002(9) 0.033(9) C60 0.059(9) 0.064(9) 0.045(9) 0.024(7) 0.009(7) 0.008(7) C61 0.042(7) 0.035(6) 0.030(7) 0.010(5) 0.004(5) 0.013(5) C62 0.054(10) 0.050(10) 0.051(10) 0.008(6) 0.007(7) 0.021(7) C63 0.092(10) 0.100(10) 0.091(10) 0.013(6) 0.021(7) 0.044(7) C61A 0.042(7) 0.035(6) 0.030(7) 0.010(5) 0.004(5) 0.013(5) C62A 0.054(10) 0.050(10) 0.051(10) 0.008(6) 0.007(7) 0.021(7) C63A 0.092(10) 0.100(10) 0.091(10) 0.013(6) 0.021(7) 0.044(7) C64 0.056(9) 0.038(8) 0.063(9) 0.004(7) 0.007(8) 0.018(7) C65 0.068(10) 0.059(9) 0.088(10) 0.011(8) -0.003(8) 0.032(8) C66 0.099(11) 0.089(11) 0.112(12) 0.023(9) -0.002(9) 0.052(9) C67 0.109(12) 0.113(12) 0.130(13) 0.011(9) 0.019(9) 0.057(9) C68 0.085(11) 0.074(10) 0.103(11) 0.010(8) 0.022(8) 0.036(8) C69 0.045(9) 0.043(8) 0.071(9) 0.007(7) 0.000(7) 0.026(7) C70 0.083(9) 0.072(8) 0.073(9) 0.024(6) -0.008(6) 0.033(6) C71 0.052(9) 0.041(9) 0.047(9) 0.007(6) 0.012(6) 0.023(6) C72 0.138(16) 0.143(16) 0.137(16) 0.017(7) 0.026(8) 0.059(9) C70A 0.083(9) 0.072(8) 0.073(9) 0.024(6) -0.008(6) 0.033(6) C71A 0.052(9) 0.041(9) 0.047(9) 0.007(6) 0.012(6) 0.023(6) C72A 0.138(16) 0.143(16) 0.137(16) 0.017(7) 0.026(8) 0.059(9) C73 0.035(8) 0.014(6) 0.028(7) 0.002(6) 0.007(6) 0.013(6) C74 0.034(8) 0.030(7) 0.026(7) 0.010(6) 0.009(6) 0.022(6) C75 0.042(8) 0.027(7) 0.032(8) -0.003(6) 0.014(6) 0.016(6) C76 0.031(7) 0.039(8) 0.028(7) 0.009(6) 0.016(6) 0.006(6) C77 0.031(8) 0.030(7) 0.031(7) 0.007(6) 0.006(6) -0.001(6) C78 0.030(8) 0.031(7) 0.030(7) -0.008(6) 0.010(6) 0.009(6) C79 0.040(8) 0.041(8) 0.035(8) -0.002(6) 0.000(6) 0.025(6) C80 0.020(7) 0.020(7) 0.032(7) -0.001(6) -0.004(6) 0.009(6) C81 0.058(9) 0.036(8) 0.047(8) 0.011(7) -0.001(7) 0.019(7) C82 0.041(8) 0.037(8) 0.023(7) -0.012(6) 0.011(7) 0.018(6) C83 0.071(9) 0.057(9) 0.055(9) 0.000(7) 0.012(8) 0.038(7) C84 0.090(10) 0.072(9) 0.044(9) 0.013(7) 0.030(8) 0.035(8) C85 0.082(10) 0.076(10) 0.064(10) 0.008(8) 0.009(8) 0.044(8) C86 0.071(9) 0.054(8) 0.056(9) 0.013(7) -0.001(7) 0.044(7) C87 0.071(9) 0.050(9) 0.061(9) -0.002(7) 0.005(8) 0.035(7) C88 0.066(8) 0.053(7) 0.050(8) 0.001(6) 0.021(6) 0.025(6) C89 0.047(9) 0.046(8) 0.048(9) 0.000(6) 0.015(6) 0.024(6) C90 0.064(10) 0.063(10) 0.064(10) 0.011(6) 0.013(7) 0.028(7) C88A 0.066(8) 0.053(7) 0.050(8) 0.001(6) 0.021(6) 0.025(6) C89A 0.047(9) 0.046(8) 0.048(9) 0.000(6) 0.015(6) 0.024(6) C90A 0.064(10) 0.063(10) 0.064(10) 0.011(6) 0.013(7) 0.028(7) C91 0.042(8) 0.040(8) 0.045(8) 0.001(6) 0.029(7) 0.012(6) C92 0.048(8) 0.020(7) 0.026(7) -0.001(6) 0.014(7) 0.005(6) C93 0.050(8) 0.032(7) 0.037(8) -0.003(6) 0.014(7) 0.010(6) C94 0.045(8) 0.031(7) 0.025(7) 0.005(6) 0.011(6) 0.013(6) C95 0.045(8) 0.023(7) 0.043(8) 0.008(6) 0.011(7) 0.007(6) C96 0.024(7) 0.025(7) 0.027(7) 0.000(6) 0.006(6) 0.001(6) C97 0.047(8) 0.017(7) 0.030(8) 0.004(6) 0.011(7) 0.009(6) C98 0.034(8) 0.046(8) 0.056(9) -0.002(7) 0.015(7) 0.016(7) C99 0.056(9) 0.048(8) 0.059(9) 0.002(7) 0.013(7) 0.027(7) C100 0.061(9) 0.044(8) 0.061(9) 0.002(7) 0.016(7) 0.028(7) C101 0.058(9) 0.029(7) 0.045(8) -0.008(6) 0.022(7) 0.016(7) C102 0.041(8) 0.031(7) 0.035(8) 0.001(6) 0.018(7) 0.013(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C7 1.875(17) . ? Fe1 C6 1.922(17) . ? Fe1 C1 2.068(17) . ? Fe1 P1 2.115(5) . ? Fe1 C4 2.123(16) . ? Fe1 C5 2.125(17) . ? Fe1 C2 2.131(15) . ? Fe1 C3 2.136(16) . ? Fe1 Fe2 2.515(3) . ? Fe2 C7 1.895(16) . ? Fe2 C6 1.905(18) . ? Fe2 C10 2.084(14) . ? Fe2 C11 2.103(15) . ? Fe2 P2 2.110(4) . ? Fe2 C12 2.113(14) . ? Fe2 C8 2.138(15) . ? Fe2 C9 2.142(15) . ? Fe3 C96 1.892(16) . ? Fe3 C97 1.906(16) . ? Fe3 C98 2.099(16) . ? Fe3 P3 2.110(5) . ? Fe3 C102 2.121(14) . ? Fe3 C100 2.123(17) . ? Fe3 C101 2.124(15) . ? Fe3 C99 2.142(17) . ? Fe3 Fe4 2.515(3) . ? Fe4 C97 1.871(17) . ? Fe4 C96 1.881(16) . ? Fe4 C91 2.082(15) . ? Fe4 C92 2.089(14) . ? Fe4 P4 2.109(5) . ? Fe4 C94 2.121(15) . ? Fe4 C95 2.145(16) . ? Fe4 C93 2.152(16) . ? P1 O3 1.618(10) . ? P1 O4 1.630(10) . ? P1 N1 1.692(10) . ? P2 O5 1.621(10) . ? P2 O6 1.638(9) . ? P2 N1 1.708(10) . ? P3 O7 1.623(10) . ? P3 O8 1.645(10) . ? P3 N2 1.685(11) . ? P4 O9 1.629(10) . ? P4 O10 1.630(9) . ? P4 N2 1.716(11) . ? O1 C6 1.181(18) . ? O2 C7 1.222(17) . ? O3 C13A 1.314(16) . ? O3 C13 1.454(14) . ? O4 C22 1.407(18) . ? O5 C31 1.406(15) . ? O6 C40 1.361(16) . ? O7 C55 1.373(18) . ? O8 C64 1.43(2) . ? O9 C73 1.387(16) . ? O10 C82 1.448(18) . ? O11 C96 1.219(16) . ? O12 C97 1.231(17) . ? N1 C49 1.441(15) . ? N2 C52 1.449(16) . ? C1 C5 1.39(2) . ? C1 C2 1.40(2) . ? C1 H1 0.9500 . ? C2 C3 1.40(2) . ? C2 H2 0.9500 . ? C3 C4 1.42(2) . ? C3 H3 0.9500 . ? C4 C5 1.38(2) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C8 C9 1.380(19) . ? C8 C12 1.47(2) . ? C8 H8 0.9500 . ? C9 C10 1.35(2) . ? C9 H9 0.9500 . ? C10 C11 1.43(2) . ? C10 H10 0.9500 . ? C11 C12 1.401(18) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C14 C15 1.3900 . ? C14 C19 1.510(11) . ? C15 C16 1.3900 . ? C15 H15 0.9500 . ? C16 C17 1.3900 . ? C16 H16 0.9500 . ? C17 C18 1.3900 . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.508(18) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.314(17) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C21 H21B 0.9500 . ? C13A C14A 1.3900 . ? C13A C18A 1.3900 . ? C14A C15A 1.3900 . ? C14A C19A 1.511(12) . ? C15A C16A 1.3900 . ? C15A H15A 0.9500 . ? C16A C17A 1.3900 . ? C16A H16A 0.9500 . ? C17A C18A 1.3900 . ? C17A H17A 0.9500 . ? C18A H18A 0.9500 . ? C19A C20A 1.492(18) . ? C19A H19C 0.9900 . ? C19A H19D 0.9900 . ? C20A C21A 1.303(18) . ? C20A H20B 0.9500 . ? C21A H21C 0.9500 . ? C21A H21D 0.9500 . ? C22 C27 1.40(2) . ? C22 C23 1.42(2) . ? C23 C28 1.41(2) . ? C23 C24 1.49(2) . ? C24 C25 1.32(3) . ? C24 H24 0.9500 . ? C25 C26 1.31(3) . ? C25 H25 0.9500 . ? C26 C27 1.43(2) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.461(17) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.295(17) . ? C29 H29 0.9500 . ? C30 H30A 0.9500 . ? C30 H30B 0.9500 . ? C29A C30A 1.322(17) . ? C29A H29A 0.9500 . ? C30A H30C 0.9500 . ? C30A H30D 0.9500 . ? C31 C36 1.396(17) . ? C31 C32 1.420(17) . ? C32 C33 1.379(17) . ? C32 C37 1.494(18) . ? C33 C34 1.413(18) . ? C33 H33 0.9500 . ? C34 C35 1.375(18) . ? C34 H34 0.9500 . ? C35 C36 1.362(18) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.51(2) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.30(2) . ? C38 H38 0.9500 . ? C39 H39A 0.9500 . ? C39 H39B 0.9500 . ? C40 C45 1.369(19) . ? C40 C41 1.376(19) . ? C41 C42 1.41(2) . ? C41 C46 1.49(2) . ? C42 C43 1.41(2) . ? C42 H42 0.9500 . ? C43 C44 1.38(2) . ? C43 H43 0.9500 . ? C44 C45 1.37(2) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.50(2) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.308(17) . ? C47 H47A 0.9500 . ? C48 H48A 0.9500 . ? C48 H48B 0.9500 . ? C48A H48C 0.9500 . ? C48A H48D 0.9500 . ? C49 C54 1.362(18) . ? C49 C50 1.432(17) . ? C50 C51 1.353(17) . ? C50 H50 0.9500 . ? C51 C52 1.343(18) . ? C51 H51 0.9500 . ? C52 C53 1.421(19) . ? C53 C54 1.407(17) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C60 1.38(2) . ? C55 C56 1.39(2) . ? C56 C57 1.39(3) . ? C56 C61 1.50(2) . ? C57 C58 1.38(3) . ? C57 H57 0.9500 . ? C58 C59 1.42(3) . ? C58 H58 0.9500 . ? C59 C60 1.37(3) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C62 1.497(17) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.286(17) . ? C62 H62A 0.9500 . ? C63 H63A 0.9500 . ? C63 H63B 0.9500 . ? C62A H62B 0.9500 . ? C64 C69 1.34(2) . ? C64 C65 1.41(3) . ? C65 C66 1.43(3) . ? C65 C70 1.45(2) . ? C66 C67 1.31(3) . ? C66 H66 0.9500 . ? C67 C68 1.29(3) . ? C67 H67 0.9500 . ? C68 C69 1.49(2) . ? C68 H68 0.9500 . ? C69 H69 0.9500 . ? C70 C71 1.461(16) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.297(18) . ? C71 H71A 0.9500 . ? C72 H72A 0.9500 . ? C72 H72B 0.9500 . ? C71A C72A 1.311(18) . ? C71A H71B 0.9500 . ? C72A H72C 0.9500 . ? C72A H72D 0.9500 . ? C73 C74 1.366(18) . ? C73 C78 1.423(18) . ? C74 C75 1.365(19) . ? C74 C79 1.536(19) . ? C75 C76 1.401(18) . ? C75 H75 0.9500 . ? C76 C77 1.371(18) . ? C76 H76 0.9500 . ? C77 C78 1.381(18) . ? C77 H77 0.9500 . ? C78 H78 0.9500 . ? C79 C80 1.488(18) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 C81 1.297(19) . ? C80 H80 0.9500 . ? C81 H81A 0.9500 . ? C81 H81B 0.9500 . ? C82 C87 1.28(2) . ? C82 C83 1.37(2) . ? C83 C84 1.44(2) . ? C83 C88 1.52(2) . ? C84 C85 1.37(2) . ? C84 H84 0.9500 . ? C85 C86 1.37(2) . ? C86 C87 1.43(2) . ? C87 H87 0.9500 . ? C88 C89 1.469(16) . ? C88 H88A 0.9900 . ? C88 H88B 0.9900 . ? C89 C90 1.289(17) . ? C89 H89 0.9500 . ? C90 H90A 0.9500 . ? C90 H90B 0.9500 . ? C89A C90A 1.300(18) . ? C89A H89A 0.9500 . ? C90A H90C 0.9500 . ? C90A H90D 0.9500 . ? C91 C95 1.41(2) . ? C91 C92 1.42(2) . ? C91 H91 0.9500 . ? C92 C93 1.400(19) . ? C92 H92 0.9500 . ? C93 C94 1.44(2) . ? C93 H93 0.9500 . ? C94 C95 1.42(2) . ? C94 H94 0.9500 . ? C95 H95 0.9500 . ? C98 C99 1.39(2) . ? C98 C102 1.41(2) . ? C98 H98 0.9500 . ? C99 C100 1.42(2) . ? C99 H99 0.9500 . ? C100 C101 1.39(2) . ? C100 H100 0.9500 . ? C101 C102 1.405(19) . ? C101 H101 0.9500 . ? C102 H102 0.9500 . ? 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 C7 Fe1 C6 96.8(7) . . ? C7 Fe1 C1 135.8(8) . . ? C6 Fe1 C1 126.7(8) . . ? C7 Fe1 P1 84.4(4) . . ? C6 Fe1 P1 96.8(5) . . ? C1 Fe1 P1 96.2(5) . . ? C7 Fe1 C4 118.5(7) . . ? C6 Fe1 C4 86.9(7) . . ? C1 Fe1 C4 63.6(6) . . ? P1 Fe1 C4 156.3(5) . . ? C7 Fe1 C5 154.9(7) . . ? C6 Fe1 C5 90.8(7) . . ? C1 Fe1 C5 38.7(6) . . ? P1 Fe1 C5 118.4(5) . . ? C4 Fe1 C5 37.9(6) . . ? C7 Fe1 C2 98.8(7) . . ? C6 Fe1 C2 151.9(7) . . ? C1 Fe1 C2 39.0(6) . . ? P1 Fe1 C2 107.8(5) . . ? C4 Fe1 C2 65.1(6) . . ? C5 Fe1 C2 65.8(7) . . ? C7 Fe1 C3 90.8(7) . . ? C6 Fe1 C3 118.4(6) . . ? C1 Fe1 C3 63.9(7) . . ? P1 Fe1 C3 144.7(5) . . ? C4 Fe1 C3 38.9(6) . . ? C5 Fe1 C3 64.7(7) . . ? C2 Fe1 C3 38.4(5) . . ? C7 Fe1 Fe2 48.5(5) . . ? C6 Fe1 Fe2 48.6(5) . . ? C1 Fe1 Fe2 168.3(5) . . ? P1 Fe1 Fe2 95.12(14) . . ? C4 Fe1 Fe2 104.7(4) . . ? C5 Fe1 Fe2 131.5(4) . . ? C2 Fe1 Fe2 138.4(5) . . ? C3 Fe1 Fe2 107.6(4) . . ? C7 Fe2 C6 96.8(7) . . ? C7 Fe2 C10 138.7(7) . . ? C6 Fe2 C10 124.0(7) . . ? C7 Fe2 C11 99.2(7) . . ? C6 Fe2 C11 157.7(6) . . ? C10 Fe2 C11 40.0(5) . . ? C7 Fe2 P2 93.3(4) . . ? C6 Fe2 P2 87.2(5) . . ? C10 Fe2 P2 94.5(4) . . ? C11 Fe2 P2 107.2(4) . . ? C7 Fe2 C12 84.6(6) . . ? C6 Fe2 C12 128.6(6) . . ? C10 Fe2 C12 66.1(6) . . ? C11 Fe2 C12 38.8(5) . . ? P2 Fe2 C12 144.2(4) . . ? C7 Fe2 C8 111.5(6) . . ? C6 Fe2 C8 94.6(6) . . ? C10 Fe2 C8 63.7(6) . . ? C11 Fe2 C8 65.1(6) . . ? P2 Fe2 C8 154.7(4) . . ? C12 Fe2 C8 40.3(5) . . ? C7 Fe2 C9 148.2(6) . . ? C6 Fe2 C9 94.0(7) . . ? C10 Fe2 C9 37.1(5) . . ? C11 Fe2 C9 64.5(6) . . ? P2 Fe2 C9 117.1(5) . . ? C12 Fe2 C9 65.5(6) . . ? C8 Fe2 C9 37.6(5) . . ? C7 Fe2 Fe1 47.8(5) . . ? C6 Fe2 Fe1 49.2(5) . . ? C10 Fe2 Fe1 168.3(4) . . ? C11 Fe2 Fe1 142.1(4) . . ? P2 Fe2 Fe1 94.60(14) . . ? C12 Fe2 Fe1 109.6(4) . . ? C8 Fe2 Fe1 105.6(4) . . ? C9 Fe2 Fe1 131.3(4) . . ? C96 Fe3 C97 95.2(7) . . ? C96 Fe3 C98 130.2(7) . . ? C97 Fe3 C98 134.2(7) . . ? C96 Fe3 P3 95.3(5) . . ? C97 Fe3 P3 84.9(4) . . ? C98 Fe3 P3 94.8(5) . . ? C96 Fe3 C102 94.0(6) . . ? C97 Fe3 C102 156.0(6) . . ? C98 Fe3 C102 39.0(6) . . ? P3 Fe3 C102 116.3(4) . . ? C96 Fe3 C100 119.2(7) . . ? C97 Fe3 C100 91.9(7) . . ? C98 Fe3 C100 63.5(7) . . ? P3 Fe3 C100 145.5(5) . . ? C102 Fe3 C100 64.3(7) . . ? C96 Fe3 C101 88.9(7) . . ? C97 Fe3 C101 119.4(6) . . ? C98 Fe3 C101 64.4(6) . . ? P3 Fe3 C101 154.9(5) . . ? C102 Fe3 C101 38.6(5) . . ? C100 Fe3 C101 38.1(6) . . ? C96 Fe3 C99 154.2(7) . . ? C97 Fe3 C99 98.5(7) . . ? C98 Fe3 C99 38.1(6) . . ? P3 Fe3 C99 107.5(5) . . ? C102 Fe3 C99 65.5(7) . . ? C100 Fe3 C99 39.0(6) . . ? C101 Fe3 C99 65.3(7) . . ? C96 Fe3 Fe4 48.0(5) . . ? C97 Fe3 Fe4 47.7(5) . . ? C98 Fe3 Fe4 169.9(5) . . ? P3 Fe3 Fe4 95.27(15) . . ? C102 Fe3 Fe4 133.9(4) . . ? C100 Fe3 Fe4 107.8(5) . . ? C101 Fe3 Fe4 105.7(5) . . ? C99 Fe3 Fe4 137.7(5) . . ? C97 Fe4 C96 96.8(7) . . ? C97 Fe4 C91 136.6(7) . . ? C96 Fe4 C91 126.3(7) . . ? C97 Fe4 C92 97.6(7) . . ? C96 Fe4 C92 158.8(6) . . ? C91 Fe4 C92 39.8(6) . . ? C97 Fe4 P4 92.7(5) . . ? C96 Fe4 P4 86.7(5) . . ? C91 Fe4 P4 94.4(5) . . ? C92 Fe4 P4 108.1(4) . . ? C97 Fe4 C94 111.1(6) . . ? C96 Fe4 C94 94.7(6) . . ? C91 Fe4 C94 65.4(6) . . ? C92 Fe4 C94 65.6(6) . . ? P4 Fe4 C94 155.8(5) . . ? C97 Fe4 C95 148.9(6) . . ? C96 Fe4 C95 94.3(6) . . ? C91 Fe4 C95 38.8(5) . . ? C92 Fe4 C95 65.7(6) . . ? P4 Fe4 C95 117.0(5) . . ? C94 Fe4 C95 38.8(5) . . ? C97 Fe4 C93 85.2(6) . . ? C96 Fe4 C93 128.1(6) . . ? C91 Fe4 C93 65.4(6) . . ? C92 Fe4 C93 38.5(5) . . ? P4 Fe4 C93 145.2(4) . . ? C94 Fe4 C93 39.3(5) . . ? C95 Fe4 C93 65.2(6) . . ? C97 Fe4 Fe3 48.8(5) . . ? C96 Fe4 Fe3 48.4(5) . . ? C91 Fe4 Fe3 168.9(4) . . ? C92 Fe4 Fe3 140.8(5) . . ? P4 Fe4 Fe3 94.87(14) . . ? C94 Fe4 Fe3 104.1(4) . . ? C95 Fe4 Fe3 130.5(4) . . ? C93 Fe4 Fe3 109.1(4) . . ? O3 P1 O4 95.4(5) . . ? O3 P1 N1 103.4(5) . . ? O4 P1 N1 96.1(5) . . ? O3 P1 Fe1 123.6(4) . . ? O4 P1 Fe1 118.1(4) . . ? N1 P1 Fe1 115.3(4) . . ? O5 P2 O6 94.6(5) . . ? O5 P2 N1 95.8(5) . . ? O6 P2 N1 103.4(5) . . ? O5 P2 Fe2 122.6(4) . . ? O6 P2 Fe2 120.6(4) . . ? N1 P2 Fe2 115.1(4) . . ? O7 P3 O8 95.2(5) . . ? O7 P3 N2 103.0(5) . . ? O8 P3 N2 96.8(5) . . ? O7 P3 Fe3 124.0(4) . . ? O8 P3 Fe3 117.7(4) . . ? N2 P3 Fe3 115.2(4) . . ? O9 P4 O10 94.2(5) . . ? O9 P4 N2 96.0(5) . . ? O10 P4 N2 103.8(5) . . ? O9 P4 Fe4 123.3(4) . . ? O10 P4 Fe4 120.3(4) . . ? N2 P4 Fe4 114.7(4) . . ? C13A O3 P1 126.8(13) . . ? C13 O3 P1 127.9(9) . . ? C22 O4 P1 126.1(10) . . ? C31 O5 P2 125.8(8) . . ? C40 O6 P2 124.6(8) . . ? C55 O7 P3 129.6(10) . . ? C64 O8 P3 129.8(11) . . ? C73 O9 P4 124.3(8) . . ? C82 O10 P4 120.2(8) . . ? C49 N1 P1 120.3(8) . . ? C49 N1 P2 121.9(9) . . ? P1 N1 P2 117.6(6) . . ? C52 N2 P3 121.0(9) . . ? C52 N2 P4 120.7(9) . . ? P3 N2 P4 118.2(6) . . ? C5 C1 C2 111.9(17) . . ? C5 C1 Fe1 72.9(10) . . ? C2 C1 Fe1 73.0(10) . . ? C5 C1 H1 124.1 . . ? C2 C1 H1 124.1 . . ? Fe1 C1 H1 121.6 . . ? C1 C2 C3 104.9(17) . . ? C1 C2 Fe1 68.1(10) . . ? C3 C2 Fe1 71.0(9) . . ? C1 C2 H2 127.5 . . ? C3 C2 H2 127.5 . . ? Fe1 C2 H2 125.0 . . ? C2 C3 C4 108.2(17) . . ? C2 C3 Fe1 70.6(9) . . ? C4 C3 Fe1 70.1(10) . . ? C2 C3 H3 125.9 . . ? C4 C3 H3 125.9 . . ? Fe1 C3 H3 125.1 . . ? C5 C4 C3 109.2(16) . . ? C5 C4 Fe1 71.1(10) . . ? C3 C4 Fe1 71.0(9) . . ? C5 C4 H4 125.4 . . ? C3 C4 H4 125.4 . . ? Fe1 C4 H4 124.0 . . ? C4 C5 C1 105.7(18) . . ? C4 C5 Fe1 70.9(10) . . ? C1 C5 Fe1 68.4(10) . . ? C4 C5 H5 127.1 . . ? C1 C5 H5 127.1 . . ? Fe1 C5 H5 125.1 . . ? O1 C6 Fe2 136.2(13) . . ? O1 C6 Fe1 141.1(13) . . ? Fe2 C6 Fe1 82.2(8) . . ? O2 C7 Fe1 136.9(12) . . ? O2 C7 Fe2 138.7(12) . . ? Fe1 C7 Fe2 83.7(7) . . ? C9 C8 C12 107.9(14) . . ? C9 C8 Fe2 71.3(9) . . ? C12 C8 Fe2 68.9(8) . . ? C9 C8 H8 126.1 . . ? C12 C8 H8 126.1 . . ? Fe2 C8 H8 125.3 . . ? C10 C9 C8 109.7(15) . . ? C10 C9 Fe2 69.1(9) . . ? C8 C9 Fe2 71.1(9) . . ? C10 C9 H9 125.1 . . ? C8 C9 H9 125.1 . . ? Fe2 C9 H9 126.3 . . ? C9 C10 C11 109.1(14) . . ? C9 C10 Fe2 73.8(9) . . ? C11 C10 Fe2 70.7(8) . . ? C9 C10 H10 125.5 . . ? C11 C10 H10 125.5 . . ? Fe2 C10 H10 121.7 . . ? C12 C11 C10 107.7(14) . . ? C12 C11 Fe2 71.0(9) . . ? C10 C11 Fe2 69.3(9) . . ? C12 C11 H11 126.1 . . ? C10 C11 H11 126.1 . . ? Fe2 C11 H11 125.2 . . ? C11 C12 C8 105.5(13) . . ? C11 C12 Fe2 70.2(8) . . ? C8 C12 Fe2 70.8(9) . . ? C11 C12 H12 127.3 . . ? C8 C12 H12 127.3 . . ? Fe2 C12 H12 123.5 . . ? C14 C13 C18 120.0 . . ? C14 C13 O3 116.4(12) . . ? C18 C13 O3 123.6(12) . . ? C13 C14 C15 120.0 . . ? C13 C14 C19 122.6(16) . . ? C15 C14 C19 117.4(16) . . ? C16 C15 C14 120.0 . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 120.0 . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C16 C17 C18 120.0 . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C13 120.0 . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? C20 C19 C14 112(2) . . ? C20 C19 H19A 109.2 . . ? C14 C19 H19A 109.2 . . ? C20 C19 H19B 109.2 . . ? C14 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? C21 C20 C19 125(3) . . ? C21 C20 H20A 117.7 . . ? C19 C20 H20A 117.7 . . ? C20 C21 H21A 120.0 . . ? C20 C21 H21B 120.0 . . ? H21A C21 H21B 120.0 . . ? O3 C13A C14A 119.5(19) . . ? O3 C13A C18A 119.8(19) . . ? C14A C13A C18A 120.0 . . ? C15A C14A C13A 120.0 . . ? C15A C14A C19A 122(3) . . ? C13A C14A C19A 118(3) . . ? C16A C15A C14A 120.0 . . ? C16A C15A H15A 120.0 . . ? C14A C15A H15A 120.0 . . ? C15A C16A C17A 120.0 . . ? C15A C16A H16A 120.0 . . ? C17A C16A H16A 120.0 . . ? C18A C17A C16A 120.0 . . ? C18A C17A H17A 120.0 . . ? C16A C17A H17A 120.0 . . ? C17A C18A C13A 120.0 . . ? C17A C18A H18A 120.0 . . ? C13A C18A H18A 120.0 . . ? C20A C19A C14A 115(3) . . ? C20A C19A H19C 108.4 . . ? C14A C19A H19C 108.4 . . ? C20A C19A H19D 108.4 . . ? C14A C19A H19D 108.4 . . ? H19C C19A H19D 107.5 . . ? C21A C20A C19A 126(4) . . ? C21A C20A H20B 117.2 . . ? C19A C20A H20B 117.2 . . ? C20A C21A H21C 120.0 . . ? C20A C21A H21D 120.0 . . ? H21C C21A H21D 120.0 . . ? C27 C22 O4 121.3(18) . . ? C27 C22 C23 126.9(19) . . ? O4 C22 C23 111.8(16) . . ? C28 C23 C22 124.6(18) . . ? C28 C23 C24 125(2) . . ? C22 C23 C24 110.6(19) . . ? C25 C24 C23 121(2) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C26 C25 C24 126(2) . . ? C26 C25 H25 116.9 . . ? C24 C25 H25 116.9 . . ? C25 C26 C27 120(2) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C22 C27 C26 115(2) . . ? C22 C27 H27 122.3 . . ? C26 C27 H27 122.3 . . ? C23 C28 C29 106.8(19) . . ? C23 C28 H28A 110.4 . . ? C29 C28 H28A 110.4 . . ? C23 C28 H28B 110.4 . . ? C29 C28 H28B 110.4 . . ? H28A C28 H28B 108.6 . . ? C30 C29 C28 125(3) . . ? C30 C29 H29 117.4 . . ? C28 C29 H29 117.4 . . ? C29 C30 H30A 120.0 . . ? C29 C30 H30B 120.0 . . ? H30A C30 H30B 120.0 . . ? C30A C29A H29A 109.3 . . ? C29A C30A H30C 120.0 . . ? C29A C30A H30D 120.0 . . ? H30C C30A H30D 120.0 . . ? C36 C31 O5 118.3(12) . . ? C36 C31 C32 122.1(13) . . ? O5 C31 C32 119.4(12) . . ? C33 C32 C31 116.1(13) . . ? C33 C32 C37 122.9(13) . . ? C31 C32 C37 120.8(12) . . ? C32 C33 C34 121.6(14) . . ? C32 C33 H33 119.2 . . ? C34 C33 H33 119.2 . . ? C35 C34 C33 120.2(14) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C36 C35 C34 120.1(15) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C31 119.9(14) . . ? C35 C36 H36 120.1 . . ? C31 C36 H36 120.1 . . ? C32 C37 C38 112.7(13) . . ? C32 C37 H37A 109.1 . . ? C38 C37 H37A 109.1 . . ? C32 C37 H37B 109.1 . . ? C38 C37 H37B 109.1 . . ? H37A C37 H37B 107.8 . . ? C39 C38 C37 128.9(18) . . ? C39 C38 H38 115.6 . . ? C37 C38 H38 115.6 . . ? C38 C39 H39A 120.0 . . ? C38 C39 H39B 120.0 . . ? H39A C39 H39B 120.0 . . ? O6 C40 C45 121.0(14) . . ? O6 C40 C41 119.5(14) . . ? C45 C40 C41 119.4(16) . . ? C40 C41 C42 119.5(16) . . ? C40 C41 C46 122.4(16) . . ? C42 C41 C46 118.0(16) . . ? C41 C42 C43 118.9(17) . . ? C41 C42 H42 120.5 . . ? C43 C42 H42 120.5 . . ? C44 C43 C42 120.6(18) . . ? C44 C43 H43 119.7 . . ? C42 C43 H43 119.7 . . ? C45 C44 C43 118.1(16) . . ? C45 C44 H44 121.0 . . ? C43 C44 H44 121.0 . . ? C44 C45 C40 123.4(16) . . ? C44 C45 H45 118.3 . . ? C40 C45 H45 118.3 . . ? C41 C46 C47 116.7(15) . . ? C41 C46 H46A 108.1 . . ? C47 C46 H46A 108.1 . . ? C41 C46 H46B 108.1 . . ? C47 C46 H46B 108.1 . . ? H46A C46 H46B 107.3 . . ? C48 C47 C46 125(3) . . ? C48 C47 H47A 117.5 . . ? C46 C47 H47A 117.5 . . ? C47 C48 H48A 120.0 . . ? C47 C48 H48B 120.0 . . ? H48A C48 H48B 120.0 . . ? H48C C48A H48D 120.0 . . ? C54 C49 C50 119.1(13) . . ? C54 C49 N1 120.7(13) . . ? C50 C49 N1 120.2(12) . . ? C51 C50 C49 118.1(13) . . ? C51 C50 H50 121.0 . . ? C49 C50 H50 121.0 . . ? C52 C51 C50 125.2(14) . . ? C52 C51 H51 117.4 . . ? C50 C51 H51 117.4 . . ? C51 C52 C53 117.1(13) . . ? C51 C52 N2 124.7(13) . . ? C53 C52 N2 118.1(13) . . ? C54 C53 C52 119.8(14) . . ? C54 C53 H53 120.1 . . ? C52 C53 H53 120.1 . . ? C49 C54 C53 120.4(14) . . ? C49 C54 H54 119.8 . . ? C53 C54 H54 119.8 . . ? O7 C55 C60 121.0(14) . . ? O7 C55 C56 115.8(15) . . ? C60 C55 C56 123.2(17) . . ? C55 C56 C57 118(2) . . ? C55 C56 C61 121.3(16) . . ? C57 C56 C61 120.7(19) . . ? C58 C57 C56 122(3) . . ? C58 C57 H57 119.2 . . ? C56 C57 H57 119.2 . . ? C57 C58 C59 117(3) . . ? C57 C58 H58 121.5 . . ? C59 C58 H58 121.5 . . ? C60 C59 C58 123(3) . . ? C60 C59 H59 118.5 . . ? C58 C59 H59 118.5 . . ? C59 C60 C55 117(2) . . ? C59 C60 H60 121.5 . . ? C55 C60 H60 121.5 . . ? C62 C61 C56 113.4(17) . . ? C62 C61 H61A 108.9 . . ? C56 C61 H61A 108.9 . . ? C62 C61 H61B 108.9 . . ? C56 C61 H61B 108.9 . . ? H61A C61 H61B 107.7 . . ? C63 C62 C61 131(2) . . ? C63 C62 H62A 114.6 . . ? C61 C62 H62A 114.6 . . ? C62 C63 H63A 120.0 . . ? C62 C63 H63B 120.0 . . ? H63A C63 H63B 120.0 . . ? C69 C64 C65 125(2) . . ? C69 C64 O8 119.4(18) . . ? C65 C64 O8 115.5(18) . . ? C64 C65 C66 113(2) . . ? C64 C65 C70 122(2) . . ? C66 C65 C70 125(2) . . ? C67 C66 C65 123(3) . . ? C67 C66 H66 118.4 . . ? C65 C66 H66 118.4 . . ? C68 C67 C66 124(3) . . ? C68 C67 H67 118.0 . . ? C66 C67 H67 118.0 . . ? C67 C68 C69 118(2) . . ? C67 C68 H68 120.9 . . ? C69 C68 H68 120.9 . . ? C64 C69 C68 117(2) . . ? C64 C69 H69 121.6 . . ? C68 C69 H69 121.6 . . ? C65 C70 C71 113.2(18) . . ? C65 C70 H70A 108.9 . . ? C71 C70 H70A 108.9 . . ? C65 C70 H70B 108.9 . . ? C71 C70 H70B 108.9 . . ? H70A C70 H70B 107.8 . . ? C72 C71 C70 118(3) . . ? C72 C71 H71A 121.2 . . ? C70 C71 H71A 121.2 . . ? C71 C72 H72A 120.0 . . ? C71 C72 H72B 120.0 . . ? H72A C72 H72B 120.0 . . ? C72A C71A H71B 114.1 . . ? C71A C72A H72C 120.0 . . ? C71A C72A H72D 120.0 . . ? H72C C72A H72D 120.0 . . ? C74 C73 O9 122.9(13) . . ? C74 C73 C78 119.9(14) . . ? O9 C73 C78 117.1(12) . . ? C75 C74 C73 120.6(14) . . ? C75 C74 C79 119.7(13) . . ? C73 C74 C79 119.4(14) . . ? C74 C75 C76 119.5(14) . . ? C74 C75 H75 120.3 . . ? C76 C75 H75 120.3 . . ? C77 C76 C75 121.2(15) . . ? C77 C76 H76 119.4 . . ? C75 C76 H76 119.4 . . ? C76 C77 C78 119.2(15) . . ? C76 C77 H77 120.4 . . ? C78 C77 H77 120.4 . . ? C77 C78 C73 119.5(14) . . ? C77 C78 H78 120.3 . . ? C73 C78 H78 120.3 . . ? C80 C79 C74 114.8(12) . . ? C80 C79 H79A 108.6 . . ? C74 C79 H79A 108.6 . . ? C80 C79 H79B 108.6 . . ? C74 C79 H79B 108.6 . . ? H79A C79 H79B 107.5 . . ? C81 C80 C79 129.4(14) . . ? C81 C80 H80 115.3 . . ? C79 C80 H80 115.3 . . ? C80 C81 H81A 120.0 . . ? C80 C81 H81B 120.0 . . ? H81A C81 H81B 120.0 . . ? C87 C82 C83 122.3(19) . . ? C87 C82 O10 124.7(17) . . ? C83 C82 O10 112.7(15) . . ? C82 C83 C84 117.8(18) . . ? C82 C83 C88 127.2(18) . . ? C84 C83 C88 115.0(18) . . ? C85 C84 C83 117.3(19) . . ? C85 C84 H84 121.4 . . ? C83 C84 H84 121.4 . . ? C84 C85 C86 125(2) . . ? C85 C86 C87 113.1(18) . . ? C82 C87 C86 125(2) . . ? C82 C87 H87 117.7 . . ? C86 C87 H87 117.7 . . ? C89 C88 C83 111.7(17) . . ? C89 C88 H88A 109.3 . . ? C83 C88 H88A 109.3 . . ? C89 C88 H88B 109.3 . . ? C83 C88 H88B 109.3 . . ? H88A C88 H88B 107.9 . . ? C90 C89 C88 123(2) . . ? C90 C89 H89 118.5 . . ? C88 C89 H89 118.5 . . ? C89 C90 H90A 120.0 . . ? C89 C90 H90B 120.0 . . ? H90A C90 H90B 120.0 . . ? C90A C89A H89A 121.9 . . ? C89A C90A H90C 120.0 . . ? C89A C90A H90D 120.0 . . ? H90C C90A H90D 120.0 . . ? C95 C91 C92 108.8(15) . . ? C95 C91 Fe4 73.0(9) . . ? C92 C91 Fe4 70.3(9) . . ? C95 C91 H91 125.6 . . ? C92 C91 H91 125.6 . . ? Fe4 C91 H91 122.7 . . ? C93 C92 C91 108.5(15) . . ? C93 C92 Fe4 73.2(9) . . ? C91 C92 Fe4 69.8(9) . . ? C93 C92 H92 125.8 . . ? C91 C92 H92 125.8 . . ? Fe4 C92 H92 122.9 . . ? C92 C93 C94 106.9(15) . . ? C92 C93 Fe4 68.3(9) . . ? C94 C93 Fe4 69.2(9) . . ? C92 C93 H93 126.5 . . ? C94 C93 H93 126.5 . . ? Fe4 C93 H93 127.5 . . ? C95 C94 C93 108.6(14) . . ? C95 C94 Fe4 71.6(9) . . ? C93 C94 Fe4 71.5(9) . . ? C95 C94 H94 125.7 . . ? C93 C94 H94 125.7 . . ? Fe4 C94 H94 122.9 . . ? C91 C95 C94 107.1(15) . . ? C91 C95 Fe4 68.2(9) . . ? C94 C95 Fe4 69.7(9) . . ? C91 C95 H95 126.5 . . ? C94 C95 H95 126.5 . . ? Fe4 C95 H95 127.2 . . ? O11 C96 Fe4 136.5(12) . . ? O11 C96 Fe3 138.8(12) . . ? Fe4 C96 Fe3 83.6(7) . . ? O12 C97 Fe4 142.1(12) . . ? O12 C97 Fe3 133.5(12) . . ? Fe4 C97 Fe3 83.5(7) . . ? C99 C98 C102 111.3(16) . . ? C99 C98 Fe3 72.6(10) . . ? C102 C98 Fe3 71.3(9) . . ? C99 C98 H98 124.4 . . ? C102 C98 H98 124.4 . . ? Fe3 C98 H98 123.2 . . ? C98 C99 C100 104.7(17) . . ? C98 C99 Fe3 69.3(10) . . ? C100 C99 Fe3 69.8(10) . . ? C98 C99 H99 127.7 . . ? C100 C99 H99 127.7 . . ? Fe3 C99 H99 124.9 . . ? C101 C100 C99 110.0(17) . . ? C101 C100 Fe3 71.0(10) . . ? C99 C100 Fe3 71.2(10) . . ? C101 C100 H100 125.0 . . ? C99 C100 H100 125.0 . . ? Fe3 C100 H100 124.4 . . ? C100 C101 C102 107.9(16) . . ? C100 C101 Fe3 70.9(10) . . ? C102 C101 Fe3 70.6(8) . . ? C100 C101 H101 126.0 . . ? C102 C101 H101 126.0 . . ? Fe3 C101 H101 124.1 . . ? C101 C102 C98 106.1(16) . . ? C101 C102 Fe3 70.8(9) . . ? C98 C102 Fe3 69.7(9) . . ? C101 C102 H102 126.9 . . ? C98 C102 H102 126.9 . . ? Fe3 C102 H102 124.3 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.866 _refine_diff_density_min -0.588 _refine_diff_density_rms 0.134 _database_code_depnum_ccdc_archive 'CCDC 955816' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_msb429a_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C102 H96 Fe4 N2 O12 P4' _chemical_formula_sum 'C102 H96 Fe4 N2 O12 P4' _chemical_formula_weight 1889.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.694(4) _cell_length_b 24.793(6) _cell_length_c 24.102(6) _cell_angle_alpha 90.00 _cell_angle_beta 108.831(3) _cell_angle_gamma 90.00 _cell_volume 8876(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9964 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 27.44 _exptl_crystal_description Plate _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.414 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3928 _exptl_absorpt_coefficient_mu 0.778 _exptl_absorpt_correction_type 'integration numerical gaussian' _exptl_absorpt_correction_T_min 0.8492 _exptl_absorpt_correction_T_max 0.9404 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008a)' _exptl_special_details ; The diffraction data were collected in three sets of 606 frames (0.3 deg. width in omega) at phi = 0, 120 and 240 deg. A scan time of 70 sec/frame was used. ; _diffrn_ambient_temperature 100(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 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 76855 _diffrn_reflns_av_R_equivalents 0.0937 _diffrn_reflns_av_sigmaI/netI 0.0951 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 27.53 _reflns_number_total 20295 _reflns_number_gt 11945 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2009)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2009a)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS 2009a)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008)' _computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008)' _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. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. The terminal carbon atom of the allyl group C100, C101, c102 is disordered over two sites in a 73/27 ratio. The two sites were refined subject to restraints that the geometries of the two components of the disorder be equivalent. ; _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^)+(0.0704P)^2^+1.7918P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20295 _refine_ls_number_parameters 1116 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1254 _refine_ls_R_factor_gt 0.0650 _refine_ls_wR_factor_ref 0.1654 _refine_ls_wR_factor_gt 0.1362 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 1.01980(4) 0.31731(2) 0.22493(3) 0.01615(14) Uani 1 1 d . . . Fe2 Fe 1.03090(4) 0.21610(2) 0.22187(3) 0.01475(14) Uani 1 1 d . . . Fe3 Fe 0.25145(4) 0.31755(2) 0.02446(3) 0.01486(14) Uani 1 1 d . . . Fe4 Fe 0.23958(4) 0.21611(2) 0.02491(3) 0.01354(13) Uani 1 1 d . . . P1 P 0.87977(7) 0.32038(4) 0.17895(5) 0.0134(2) Uani 1 1 d . . . P2 P 0.89044(7) 0.20350(4) 0.19196(5) 0.0131(2) Uani 1 1 d . . . P3 P 0.39277(7) 0.31938(4) 0.06468(5) 0.0131(2) Uani 1 1 d . . . P4 P 0.37987(7) 0.20295(4) 0.04650(5) 0.0126(2) Uani 1 1 d . . . O1 O 1.02849(19) 0.27424(12) 0.11584(12) 0.0189(7) Uani 1 1 d . . . O2 O 1.0111(2) 0.25979(12) 0.32874(13) 0.0232(7) Uani 1 1 d . . . O3 O 0.84811(18) 0.33972(11) 0.11040(12) 0.0153(6) Uani 1 1 d . . . O4 O 0.80951(19) 0.35927(11) 0.19714(12) 0.0176(6) Uani 1 1 d . . . O5 O 0.84765(19) 0.15860(11) 0.14134(12) 0.0163(6) Uani 1 1 d . . . O6 O 0.83653(18) 0.18268(11) 0.23535(12) 0.0154(6) Uani 1 1 d . . . O7 O 0.25161(19) 0.27169(11) 0.13455(12) 0.0184(6) Uani 1 1 d . . . O8 O 0.2453(2) 0.26192(12) -0.08418(13) 0.0208(7) Uani 1 1 d . . . O9 O 0.46040(19) 0.35899(11) 0.04424(12) 0.0152(6) Uani 1 1 d . . . O10 O 0.43309(19) 0.33520(11) 0.13354(12) 0.0150(6) Uani 1 1 d . . . O11 O 0.42726(18) 0.18635(11) -0.00195(12) 0.0144(6) Uani 1 1 d . . . O12 O 0.42922(18) 0.15582(11) 0.09299(12) 0.0145(6) Uani 1 1 d . . . N1 N 0.8268(2) 0.25963(13) 0.16808(15) 0.0142(7) Uani 1 1 d . . . N2 N 0.4444(2) 0.25851(13) 0.07083(14) 0.0124(7) Uani 1 1 d . . . C1 C 1.0348(3) 0.40111(18) 0.2411(2) 0.0273(11) Uani 1 1 d . . . H1 H 0.9859 0.4256 0.2343 0.033 Uiso 1 1 calc R . . C2 C 1.0766(3) 0.37313(18) 0.2939(2) 0.0262(11) Uani 1 1 d . . . H2 H 1.0618 0.3757 0.3290 0.031 Uiso 1 1 calc R . . C3 C 1.1443(3) 0.34065(19) 0.2846(2) 0.0285(11) Uani 1 1 d . . . H3 H 1.1826 0.3169 0.3126 0.034 Uiso 1 1 calc R . . C4 C 1.1464(3) 0.34905(19) 0.2269(2) 0.0280(11) Uani 1 1 d . . . H4 H 1.1865 0.3324 0.2098 0.034 Uiso 1 1 calc R . . C5 C 1.0785(3) 0.38643(19) 0.1996(2) 0.0291(11) Uani 1 1 d . . . H5 H 1.0642 0.3996 0.1607 0.035 Uiso 1 1 calc R . . C6 C 1.0233(3) 0.27017(17) 0.16346(19) 0.0180(9) Uani 1 1 d . . . C7 C 1.0128(3) 0.26266(17) 0.27913(18) 0.0182(9) Uani 1 1 d . . . C8 C 1.0613(3) 0.13372(17) 0.2366(2) 0.0224(10) Uani 1 1 d . . . H8 H 1.0172 0.1072 0.2358 0.027 Uiso 1 1 calc R . . C9 C 1.0866(3) 0.15124(17) 0.1876(2) 0.0211(10) Uani 1 1 d . . . H9 H 1.0633 0.1381 0.1485 0.025 Uiso 1 1 calc R . . C10 C 1.1528(3) 0.19182(17) 0.2080(2) 0.0204(10) Uani 1 1 d . . . H10 H 1.1815 0.2110 0.1848 0.024 Uiso 1 1 calc R . . C11 C 1.1691(3) 0.19896(19) 0.2688(2) 0.0235(10) Uani 1 1 d . . . H11 H 1.2103 0.2238 0.2934 0.028 Uiso 1 1 calc R . . C12 C 1.1135(3) 0.16272(18) 0.2866(2) 0.0234(10) Uani 1 1 d . . . H12 H 1.1115 0.1586 0.3253 0.028 Uiso 1 1 calc R . . C13 C 0.8691(3) 0.38888(16) 0.08921(18) 0.0170(9) Uani 1 1 d . . . C14 C 0.8858(3) 0.38761(18) 0.03553(19) 0.0206(9) Uani 1 1 d . . . C15 C 0.9033(3) 0.43672(19) 0.0131(2) 0.0277(11) Uani 1 1 d . . . H15 H 0.9140 0.4371 -0.0235 0.033 Uiso 1 1 calc R . . C16 C 0.9054(3) 0.48513(19) 0.0426(2) 0.0278(11) Uani 1 1 d . . . H16 H 0.9188 0.5179 0.0267 0.033 Uiso 1 1 calc R . . C17 C 0.8880(3) 0.48501(18) 0.0952(2) 0.0257(11) Uani 1 1 d . . . H17 H 0.8891 0.5179 0.1156 0.031 Uiso 1 1 calc R . . C18 C 0.8688(3) 0.43713(17) 0.11840(19) 0.0211(10) Uani 1 1 d . . . H18 H 0.8554 0.4373 0.1541 0.025 Uiso 1 1 calc R . . C19 C 0.8796(3) 0.33609(18) 0.00115(19) 0.0219(10) Uani 1 1 d . . . H19A H 0.9179 0.3393 -0.0243 0.026 Uiso 1 1 calc R . . H19B H 0.9033 0.3059 0.0287 0.026 Uiso 1 1 calc R . . C20 C 0.7855(3) 0.32343(19) -0.0359(2) 0.0276(11) Uani 1 1 d . . . H20 H 0.7410 0.3210 -0.0171 0.033 Uiso 1 1 calc R . . C21 C 0.7596(4) 0.3153(2) -0.0933(2) 0.0410(14) Uani 1 1 d . . . H21A H 0.8023 0.3174 -0.1136 0.049 Uiso 1 1 calc R . . H21B H 0.6984 0.3074 -0.1141 0.049 Uiso 1 1 calc R . . C22 C 0.7851(3) 0.35873(17) 0.24772(18) 0.0183(9) Uani 1 1 d . . . C23 C 0.7214(3) 0.39799(19) 0.2492(2) 0.0246(10) Uani 1 1 d . . . C24 C 0.6908(4) 0.3974(2) 0.2975(2) 0.0464(15) Uani 1 1 d . . . H24 H 0.6470 0.4231 0.2995 0.056 Uiso 1 1 calc R . . C25 C 0.7222(5) 0.3607(3) 0.3424(3) 0.0550(18) Uani 1 1 d . . . H25 H 0.7000 0.3610 0.3747 0.066 Uiso 1 1 calc R . . C26 C 0.7869(4) 0.3231(2) 0.3398(2) 0.0446(15) Uani 1 1 d . . . H26 H 0.8096 0.2979 0.3708 0.054 Uiso 1 1 calc R . . C27 C 0.8183(3) 0.32233(18) 0.29219(19) 0.0247(10) Uani 1 1 d . . . H27 H 0.8625 0.2968 0.2905 0.030 Uiso 1 1 calc R . . C28 C 0.6879(3) 0.4398(2) 0.2022(2) 0.0321(12) Uani 1 1 d . . . H28A H 0.6256 0.4498 0.1995 0.039 Uiso 1 1 calc R . . H28B H 0.6858 0.4237 0.1642 0.039 Uiso 1 1 calc R . . C29 C 0.7445(4) 0.4902(2) 0.2120(3) 0.0400(14) Uani 1 1 d . . . H29 H 0.7263 0.5176 0.1830 0.048 Uiso 1 1 calc R . . C30 C 0.8164(4) 0.4996(2) 0.2570(3) 0.0561(18) Uani 1 1 d . . . H30A H 0.8371 0.4733 0.2871 0.067 Uiso 1 1 calc R . . H30B H 0.8480 0.5327 0.2596 0.067 Uiso 1 1 calc R . . C31 C 0.8737(3) 0.15105(18) 0.09101(18) 0.0188(9) Uani 1 1 d . . . C32 C 0.8921(3) 0.09808(19) 0.0777(2) 0.0234(10) Uani 1 1 d . . . C33 C 0.9121(3) 0.09115(19) 0.0256(2) 0.0285(11) Uani 1 1 d . . . H33 H 0.9257 0.0560 0.0152 0.034 Uiso 1 1 calc R . . C34 C 0.9126(3) 0.1336(2) -0.0112(2) 0.0278(11) Uani 1 1 d . . . H34 H 0.9255 0.1275 -0.0466 0.033 Uiso 1 1 calc R . . C35 C 0.8944(3) 0.18500(19) 0.00344(19) 0.0233(10) Uani 1 1 d . . . H35 H 0.8956 0.2145 -0.0215 0.028 Uiso 1 1 calc R . . C36 C 0.8742(3) 0.19376(18) 0.05503(18) 0.0200(9) Uani 1 1 d . . . H36 H 0.8608 0.2291 0.0651 0.024 Uiso 1 1 calc R . . C37 C 0.8892(3) 0.05035(18) 0.1168(2) 0.0303(12) Uani 1 1 d . . . H37A H 0.8907 0.0637 0.1558 0.036 Uiso 1 1 calc R . . H37B H 0.8320 0.0304 0.0995 0.036 Uiso 1 1 calc R . . C38 C 0.9656(5) 0.0135(2) 0.1237(3) 0.0549(17) Uani 1 1 d . . . H38 H 1.0240 0.0264 0.1449 0.066 Uiso 1 1 calc R . . C39 C 0.9593(6) -0.0364(2) 0.1025(3) 0.068(2) Uani 1 1 d . . . H39A H 0.9021 -0.0508 0.0810 0.082 Uiso 1 1 calc R . . H39B H 1.0120 -0.0576 0.1089 0.082 Uiso 1 1 calc R . . C40 C 0.8556(3) 0.13470(16) 0.26794(18) 0.0155(9) Uani 1 1 d . . . C41 C 0.8008(3) 0.08993(17) 0.24822(19) 0.0195(9) Uani 1 1 d . . . C42 C 0.8207(3) 0.04309(19) 0.2828(2) 0.0282(11) Uani 1 1 d . . . H42 H 0.7854 0.0116 0.2701 0.034 Uiso 1 1 calc R . . C43 C 0.8909(3) 0.04225(18) 0.3350(2) 0.0282(11) Uani 1 1 d . . . H43 H 0.9040 0.0101 0.3576 0.034 Uiso 1 1 calc R . . C44 C 0.9428(3) 0.08836(17) 0.35486(19) 0.0206(9) Uani 1 1 d . . . H44 H 0.9901 0.0880 0.3914 0.025 Uiso 1 1 calc R . . C45 C 0.9250(3) 0.13461(17) 0.32090(19) 0.0187(9) Uani 1 1 d . . . H45 H 0.9601 0.1662 0.3339 0.022 Uiso 1 1 calc R . . C46 C 0.7191(3) 0.09178(18) 0.1939(2) 0.0241(10) Uani 1 1 d . . . H46A H 0.7313 0.1166 0.1652 0.029 Uiso 1 1 calc R . . H46B H 0.7088 0.0554 0.1760 0.029 Uiso 1 1 calc R . . C47 C 0.6351(3) 0.1100(2) 0.2056(2) 0.0272(11) Uani 1 1 d . . . H47 H 0.5829 0.1141 0.1722 0.033 Uiso 1 1 calc R . . C48 C 0.6251(3) 0.1208(2) 0.2562(2) 0.0342(12) Uani 1 1 d . . . H48A H 0.6748 0.1174 0.2912 0.041 Uiso 1 1 calc R . . H48B H 0.5682 0.1320 0.2580 0.041 Uiso 1 1 calc R . . C49 C 0.7292(3) 0.25666(16) 0.14308(18) 0.0148(9) Uani 1 1 d . . . C50 C 0.6877(3) 0.26025(17) 0.08229(18) 0.0158(9) Uani 1 1 d . . . H50 H 0.7234 0.2633 0.0572 0.019 Uiso 1 1 calc R . . C51 C 0.5948(3) 0.25932(16) 0.05870(18) 0.0151(9) Uani 1 1 d . . . H51 H 0.5671 0.2612 0.0174 0.018 Uiso 1 1 calc R . . C52 C 0.5418(3) 0.25557(15) 0.09503(18) 0.0138(8) Uani 1 1 d . . . C53 C 0.5831(3) 0.25079(15) 0.15515(18) 0.0144(8) Uani 1 1 d . . . H53 H 0.5471 0.2475 0.1800 0.017 Uiso 1 1 calc R . . C54 C 0.6764(3) 0.25079(16) 0.17938(18) 0.0154(9) Uani 1 1 d . . . H54 H 0.7041 0.2468 0.2205 0.019 Uiso 1 1 calc R . . C55 C 0.1247(3) 0.34457(18) -0.0307(2) 0.0249(11) Uani 1 1 d . . . H55 H 0.0837 0.3229 -0.0598 0.030 Uiso 1 1 calc R . . C56 C 0.1273(3) 0.34920(18) 0.0283(2) 0.0263(11) Uani 1 1 d . . . H56 H 0.0883 0.3316 0.0455 0.032 Uiso 1 1 calc R . . C57 C 0.1986(3) 0.38481(18) 0.0570(2) 0.0253(10) Uani 1 1 d . . . H57 H 0.2160 0.3953 0.0971 0.030 Uiso 1 1 calc R . . C58 C 0.2394(3) 0.40208(17) 0.0150(2) 0.0239(10) Uani 1 1 d . . . H58 H 0.2891 0.4260 0.0223 0.029 Uiso 1 1 calc R . . C59 C 0.1932(3) 0.37748(18) -0.0394(2) 0.0252(10) Uani 1 1 d . . . H59 H 0.2057 0.3821 -0.0752 0.030 Uiso 1 1 calc R . . C60 C 0.2528(3) 0.26853(16) 0.08575(18) 0.0147(8) Uani 1 1 d . . . C61 C 0.2504(3) 0.26374(17) -0.03371(18) 0.0166(9) Uani 1 1 d . . . C62 C 0.1195(3) 0.19359(17) 0.04231(19) 0.0200(9) Uani 1 1 d . . . H62 H 0.0927 0.2134 0.0661 0.024 Uiso 1 1 calc R . . C63 C 0.1845(3) 0.15225(17) 0.06143(19) 0.0195(9) Uani 1 1 d . . . H63 H 0.2088 0.1391 0.1004 0.023 Uiso 1 1 calc R . . C64 C 0.2070(3) 0.13383(16) 0.0117(2) 0.0215(10) Uani 1 1 d . . . H64 H 0.2501 0.1068 0.0120 0.026 Uiso 1 1 calc R . . C65 C 0.1538(3) 0.16300(19) -0.0379(2) 0.0261(11) Uani 1 1 d . . . H65 H 0.1535 0.1583 -0.0770 0.031 Uiso 1 1 calc R . . C66 C 0.1014(3) 0.20012(19) -0.0189(2) 0.0235(10) Uani 1 1 d . . . H66 H 0.0606 0.2254 -0.0430 0.028 Uiso 1 1 calc R . . C67 C 0.4732(3) 0.36152(16) -0.01035(18) 0.0176(9) Uani 1 1 d . . . C68 C 0.5522(3) 0.38769(18) -0.0110(2) 0.0230(10) Uani 1 1 d . . . C69 C 0.5661(3) 0.3925(2) -0.0649(2) 0.0330(12) Uani 1 1 d . . . H69 H 0.6187 0.4103 -0.0668 0.040 Uiso 1 1 calc R . . C70 C 0.5058(4) 0.3723(2) -0.1159(2) 0.0406(14) Uani 1 1 d . . . H70 H 0.5166 0.3765 -0.1523 0.049 Uiso 1 1 calc R . . C71 C 0.4297(4) 0.3459(2) -0.1135(2) 0.0331(12) Uani 1 1 d . . . H71 H 0.3885 0.3311 -0.1483 0.040 Uiso 1 1 calc R . . C72 C 0.4129(3) 0.34074(18) -0.06097(19) 0.0237(10) Uani 1 1 d . . . H72 H 0.3599 0.3230 -0.0596 0.028 Uiso 1 1 calc R . . C73 C 0.6182(3) 0.41084(19) 0.0441(2) 0.0260(11) Uani 1 1 d . . . H73A H 0.6185 0.3883 0.0781 0.031 Uiso 1 1 calc R . . H73B H 0.6795 0.4102 0.0409 0.031 Uiso 1 1 calc R . . C74 C 0.5937(3) 0.4676(2) 0.0540(2) 0.0294(11) Uani 1 1 d . . . H74 H 0.5365 0.4735 0.0584 0.035 Uiso 1 1 calc R . . C75 C 0.6453(4) 0.5097(2) 0.0569(3) 0.0443(15) Uani 1 1 d . . . H75A H 0.7030 0.5054 0.0526 0.053 Uiso 1 1 calc R . . H75B H 0.6250 0.5445 0.0632 0.053 Uiso 1 1 calc R . . C76 C 0.4256(3) 0.38243(17) 0.16320(19) 0.0201(9) Uani 1 1 d . . . C77 C 0.4247(3) 0.37519(18) 0.2203(2) 0.0250(10) Uani 1 1 d . . . C78 C 0.4234(4) 0.4214(2) 0.2528(2) 0.0326(12) Uani 1 1 d . . . H78 H 0.4237 0.4178 0.2921 0.039 Uiso 1 1 calc R . . C79 C 0.4217(4) 0.4725(2) 0.2292(2) 0.0365(13) Uani 1 1 d . . . H79 H 0.4210 0.5034 0.2524 0.044 Uiso 1 1 calc R . . C80 C 0.4210(3) 0.47876(19) 0.1720(2) 0.0320(12) Uani 1 1 d . . . H80 H 0.4180 0.5138 0.1555 0.038 Uiso 1 1 calc R . . C81 C 0.4247(3) 0.43328(17) 0.1388(2) 0.0226(10) Uani 1 1 d . . . H81 H 0.4266 0.4370 0.0999 0.027 Uiso 1 1 calc R . . C82 C 0.4289(4) 0.31862(19) 0.2455(2) 0.0303(11) Uani 1 1 d . . . H82A H 0.3865 0.2955 0.2157 0.036 Uiso 1 1 calc R . . H82B H 0.4902 0.3042 0.2520 0.036 Uiso 1 1 calc R . . C83 C 0.4082(4) 0.3131(2) 0.3013(2) 0.0400(13) Uani 1 1 d . . . H83 H 0.3563 0.3310 0.3042 0.048 Uiso 1 1 calc R . . C84 C 0.4571(5) 0.2850(2) 0.3469(2) 0.060(2) Uani 1 1 d . . . H84A H 0.5094 0.2667 0.3454 0.071 Uiso 1 1 calc R . . H84B H 0.4400 0.2832 0.3812 0.071 Uiso 1 1 calc R . . C85 C 0.4131(3) 0.13741(16) -0.03276(18) 0.0155(9) Uani 1 1 d . . . C86 C 0.4799(3) 0.09822(17) -0.01808(18) 0.0171(9) Uani 1 1 d . . . C87 C 0.4650(3) 0.05235(17) -0.05361(19) 0.0217(10) Uani 1 1 d . . . H87 H 0.5095 0.0248 -0.0452 0.026 Uiso 1 1 calc R . . C88 C 0.3866(3) 0.04595(18) -0.1011(2) 0.0242(10) Uani 1 1 d . . . H88 H 0.3780 0.0141 -0.1243 0.029 Uiso 1 1 calc R . . C89 C 0.3217(3) 0.08533(18) -0.11468(19) 0.0229(10) Uani 1 1 d . . . H89 H 0.2680 0.0808 -0.1469 0.027 Uiso 1 1 calc R . . C90 C 0.3351(3) 0.13197(17) -0.08092(18) 0.0195(9) Uani 1 1 d . . . H90 H 0.2915 0.1600 -0.0906 0.023 Uiso 1 1 calc R . . C91 C 0.5664(3) 0.10495(18) 0.03187(19) 0.0218(10) Uani 1 1 d . . . H91A H 0.5535 0.1249 0.0638 0.026 Uiso 1 1 calc R . . H91B H 0.5891 0.0688 0.0471 0.026 Uiso 1 1 calc R . . C92 C 0.6387(3) 0.1341(2) 0.0160(2) 0.0324(12) Uani 1 1 d . . . H92 H 0.6941 0.1390 0.0467 0.039 Uiso 1 1 calc R . . C93 C 0.6346(4) 0.1534(3) -0.0350(3) 0.0478(16) Uani 1 1 d . . . H93A H 0.5809 0.1497 -0.0673 0.057 Uiso 1 1 calc R . . H93B H 0.6853 0.1713 -0.0398 0.057 Uiso 1 1 calc R . . C94 C 0.4021(3) 0.14120(16) 0.14134(17) 0.0147(8) Uani 1 1 d . . . C95 C 0.3926(3) 0.08690(17) 0.15096(19) 0.0197(9) Uani 1 1 d . B . C96 C 0.3680(3) 0.07314(18) 0.2001(2) 0.0245(10) Uani 1 1 d . . . H96 H 0.3603 0.0362 0.2080 0.029 Uiso 1 1 calc R . . C97 C 0.3546(3) 0.11235(19) 0.23756(19) 0.0247(10) Uani 1 1 d . . . H97 H 0.3371 0.1022 0.2703 0.030 Uiso 1 1 calc R . . C98 C 0.3667(3) 0.16641(17) 0.22719(18) 0.0195(9) Uani 1 1 d . . . H98 H 0.3574 0.1934 0.2527 0.023 Uiso 1 1 calc R . . C99 C 0.3923(3) 0.18064(17) 0.17984(17) 0.0154(8) Uani 1 1 d . . . H99 H 0.4034 0.2174 0.1734 0.018 Uiso 1 1 calc R . . C100 C 0.4080(3) 0.04277(17) 0.11133(19) 0.0221(10) Uani 1 1 d D . . H10A H 0.4257 0.0599 0.0796 0.027 Uiso 1 1 calc R A 1 H10B H 0.4591 0.0201 0.1345 0.027 Uiso 1 1 calc R A 1 C101 C 0.3283(3) 0.00676(18) 0.0840(2) 0.0289(11) Uani 0.726(7) 1 d PD B 1 H101 H 0.3005 -0.0101 0.1092 0.035 Uiso 0.726(7) 1 calc PR B 1 C102 C 0.2948(5) -0.0028(3) 0.0276(3) 0.0335(16) Uiso 0.726(7) 1 d PD B 1 H10C H 0.3210 0.0134 0.0013 0.040 Uiso 0.726(7) 1 calc PR B 1 H10D H 0.2442 -0.0260 0.0130 0.040 Uiso 0.726(7) 1 calc PR B 1 C10A C 0.3283(3) 0.00676(18) 0.0840(2) 0.0289(11) Uani 0.274(7) 1 d PD B 2 H10E H 0.3360 -0.0201 0.0580 0.035 Uiso 0.274(7) 1 calc PR B 2 C11A C 0.2499(9) 0.0080(7) 0.0918(8) 0.0335(16) Uiso 0.274(7) 1 d PD B 2 H11A H 0.2381 0.0340 0.1173 0.040 Uiso 0.274(7) 1 calc PR B 2 H11B H 0.2046 -0.0171 0.0719 0.040 Uiso 0.274(7) 1 calc PR B 2 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 Fe1 0.0136(3) 0.0142(3) 0.0185(3) -0.0012(2) 0.0021(2) -0.0020(2) Fe2 0.0115(3) 0.0144(3) 0.0174(3) -0.0005(2) 0.0033(2) 0.0011(2) Fe3 0.0128(3) 0.0120(3) 0.0185(3) 0.0018(2) 0.0032(2) 0.0019(2) Fe4 0.0113(3) 0.0128(3) 0.0160(3) 0.0000(2) 0.0035(2) -0.0006(2) P1 0.0141(5) 0.0110(5) 0.0152(5) -0.0007(4) 0.0049(4) -0.0004(4) P2 0.0117(5) 0.0132(5) 0.0140(5) -0.0005(4) 0.0033(4) 0.0004(4) P3 0.0142(5) 0.0100(5) 0.0155(5) 0.0005(4) 0.0052(4) 0.0004(4) P4 0.0131(5) 0.0105(5) 0.0141(5) 0.0002(4) 0.0042(4) 0.0007(4) O1 0.0170(16) 0.0222(17) 0.0184(15) 0.0058(13) 0.0071(13) 0.0015(13) O2 0.0289(18) 0.0225(17) 0.0176(16) -0.0002(13) 0.0067(14) 0.0015(14) O3 0.0170(15) 0.0116(14) 0.0181(15) 0.0029(11) 0.0069(12) -0.0001(12) O4 0.0212(16) 0.0151(15) 0.0200(15) 0.0001(12) 0.0114(13) 0.0030(12) O5 0.0181(16) 0.0142(14) 0.0178(15) -0.0018(12) 0.0075(12) -0.0013(12) O6 0.0164(15) 0.0123(14) 0.0183(15) 0.0034(12) 0.0071(12) 0.0021(12) O7 0.0194(16) 0.0186(16) 0.0192(16) 0.0004(12) 0.0089(13) 0.0004(13) O8 0.0236(17) 0.0186(16) 0.0178(16) 0.0023(13) 0.0033(13) -0.0037(13) O9 0.0182(15) 0.0131(14) 0.0152(14) 0.0003(11) 0.0065(12) -0.0027(12) O10 0.0178(15) 0.0120(14) 0.0150(14) -0.0022(11) 0.0050(12) 0.0013(12) O11 0.0184(15) 0.0123(14) 0.0146(14) -0.0016(11) 0.0084(12) -0.0009(12) O12 0.0160(15) 0.0133(14) 0.0152(14) 0.0036(11) 0.0065(12) 0.0030(12) N1 0.0102(17) 0.0113(17) 0.0203(18) -0.0011(14) 0.0037(14) 0.0001(14) N2 0.0137(17) 0.0091(16) 0.0138(17) -0.0006(13) 0.0035(14) 0.0026(13) C1 0.021(2) 0.015(2) 0.040(3) -0.007(2) 0.003(2) -0.0040(19) C2 0.027(3) 0.018(2) 0.027(3) -0.0085(19) -0.001(2) -0.002(2) C3 0.017(2) 0.021(2) 0.037(3) 0.000(2) -0.005(2) -0.0067(19) C4 0.013(2) 0.025(3) 0.044(3) -0.004(2) 0.007(2) -0.0080(19) C5 0.024(3) 0.025(3) 0.034(3) 0.003(2) 0.003(2) -0.008(2) C6 0.012(2) 0.017(2) 0.024(2) 0.0029(18) 0.0050(18) -0.0014(17) C7 0.015(2) 0.018(2) 0.018(2) 0.0006(17) 0.0009(17) -0.0017(18) C8 0.014(2) 0.016(2) 0.038(3) 0.007(2) 0.010(2) 0.0065(18) C9 0.021(2) 0.017(2) 0.023(2) -0.0024(18) 0.0034(19) 0.0047(18) C10 0.013(2) 0.022(2) 0.028(2) 0.0032(19) 0.0093(18) 0.0078(18) C11 0.011(2) 0.027(2) 0.030(3) -0.003(2) 0.0025(19) 0.0032(19) C12 0.020(2) 0.029(3) 0.021(2) 0.0080(19) 0.0052(19) 0.011(2) C13 0.016(2) 0.012(2) 0.023(2) 0.0057(17) 0.0056(18) 0.0007(17) C14 0.018(2) 0.024(2) 0.020(2) 0.0058(18) 0.0059(18) 0.0015(19) C15 0.025(3) 0.031(3) 0.029(3) 0.004(2) 0.012(2) -0.001(2) C16 0.030(3) 0.019(2) 0.033(3) 0.008(2) 0.009(2) -0.003(2) C17 0.025(3) 0.018(2) 0.032(3) -0.001(2) 0.006(2) -0.0025(19) C18 0.020(2) 0.020(2) 0.021(2) 0.0042(18) 0.0030(19) 0.0037(18) C19 0.021(2) 0.026(2) 0.021(2) 0.0031(19) 0.0097(19) 0.0032(19) C20 0.027(3) 0.026(3) 0.030(3) 0.005(2) 0.009(2) 0.001(2) C21 0.039(3) 0.049(4) 0.031(3) 0.001(3) 0.007(3) -0.003(3) C22 0.019(2) 0.020(2) 0.015(2) -0.0050(17) 0.0057(18) -0.0036(18) C23 0.025(2) 0.028(3) 0.022(2) -0.0031(19) 0.009(2) 0.004(2) C24 0.051(4) 0.055(4) 0.043(3) -0.001(3) 0.028(3) 0.013(3) C25 0.083(5) 0.066(4) 0.034(3) 0.010(3) 0.043(3) 0.025(4) C26 0.067(4) 0.046(3) 0.027(3) 0.007(3) 0.024(3) 0.010(3) C27 0.031(3) 0.021(2) 0.025(2) 0.0005(19) 0.013(2) 0.005(2) C28 0.034(3) 0.031(3) 0.031(3) -0.004(2) 0.010(2) 0.015(2) C29 0.060(4) 0.019(3) 0.046(3) -0.006(2) 0.023(3) 0.007(3) C30 0.066(5) 0.034(3) 0.068(5) -0.008(3) 0.022(4) -0.017(3) C31 0.010(2) 0.029(2) 0.017(2) -0.0068(18) 0.0035(17) -0.0032(18) C32 0.016(2) 0.027(2) 0.026(2) -0.006(2) 0.0054(19) -0.0034(19) C33 0.028(3) 0.024(3) 0.034(3) -0.012(2) 0.011(2) 0.000(2) C34 0.023(3) 0.035(3) 0.027(3) -0.011(2) 0.011(2) -0.007(2) C35 0.020(2) 0.029(3) 0.024(2) -0.002(2) 0.0105(19) -0.005(2) C36 0.016(2) 0.024(2) 0.020(2) -0.0043(18) 0.0058(18) -0.0031(18) C37 0.039(3) 0.015(2) 0.037(3) -0.002(2) 0.011(2) 0.006(2) C38 0.059(4) 0.026(3) 0.078(5) 0.002(3) 0.019(4) 0.008(3) C39 0.119(7) 0.029(3) 0.070(5) 0.002(3) 0.048(5) 0.018(4) C40 0.013(2) 0.016(2) 0.018(2) 0.0024(17) 0.0054(17) 0.0001(17) C41 0.015(2) 0.021(2) 0.022(2) -0.0028(18) 0.0060(18) -0.0023(18) C42 0.028(3) 0.019(2) 0.035(3) 0.004(2) 0.006(2) -0.006(2) C43 0.029(3) 0.016(2) 0.036(3) 0.009(2) 0.005(2) 0.003(2) C44 0.020(2) 0.020(2) 0.020(2) 0.0050(18) 0.0027(18) 0.0016(18) C45 0.016(2) 0.017(2) 0.022(2) 0.0006(17) 0.0052(18) -0.0031(17) C46 0.018(2) 0.023(2) 0.027(2) -0.0011(19) 0.001(2) -0.0091(19) C47 0.017(2) 0.037(3) 0.023(2) 0.012(2) -0.0007(19) -0.003(2) C48 0.020(3) 0.046(3) 0.034(3) 0.007(2) 0.006(2) 0.003(2) C49 0.012(2) 0.012(2) 0.019(2) 0.0009(16) 0.0027(17) 0.0000(16) C50 0.011(2) 0.019(2) 0.016(2) -0.0064(17) 0.0034(16) -0.0016(17) C51 0.018(2) 0.013(2) 0.014(2) -0.0009(16) 0.0042(17) 0.0001(17) C52 0.011(2) 0.0096(19) 0.021(2) 0.0003(16) 0.0060(17) 0.0021(15) C53 0.018(2) 0.0089(18) 0.020(2) -0.0008(16) 0.0116(18) -0.0004(16) C54 0.015(2) 0.013(2) 0.017(2) 0.0000(16) 0.0030(17) 0.0000(16) C55 0.015(2) 0.020(2) 0.033(3) 0.005(2) -0.003(2) 0.0039(18) C56 0.018(2) 0.022(2) 0.040(3) 0.010(2) 0.010(2) 0.0093(19) C57 0.028(3) 0.020(2) 0.026(2) 0.0021(19) 0.007(2) 0.013(2) C58 0.023(2) 0.011(2) 0.036(3) 0.0055(19) 0.007(2) 0.0044(18) C59 0.023(2) 0.021(2) 0.026(2) 0.0070(19) 0.000(2) 0.0065(19) C60 0.012(2) 0.0113(19) 0.021(2) 0.0026(17) 0.0052(17) -0.0013(16) C61 0.010(2) 0.018(2) 0.019(2) 0.0012(17) 0.0010(17) 0.0002(17) C62 0.013(2) 0.022(2) 0.025(2) -0.0026(18) 0.0052(18) -0.0044(18) C63 0.017(2) 0.021(2) 0.022(2) 0.0016(18) 0.0076(18) -0.0053(18) C64 0.022(2) 0.009(2) 0.038(3) -0.0043(18) 0.016(2) -0.0058(17) C65 0.026(3) 0.029(3) 0.023(2) -0.009(2) 0.008(2) -0.018(2) C66 0.011(2) 0.026(2) 0.029(2) 0.006(2) 0.0007(19) -0.0062(18) C67 0.022(2) 0.014(2) 0.018(2) 0.0027(17) 0.0077(18) -0.0011(18) C68 0.021(2) 0.023(2) 0.023(2) 0.0042(19) 0.0056(19) 0.0005(19) C69 0.030(3) 0.043(3) 0.031(3) 0.007(2) 0.017(2) -0.006(2) C70 0.051(4) 0.051(4) 0.025(3) 0.002(2) 0.020(3) -0.010(3) C71 0.046(3) 0.031(3) 0.027(3) -0.002(2) 0.018(2) -0.008(2) C72 0.031(3) 0.020(2) 0.022(2) -0.0033(18) 0.011(2) -0.008(2) C73 0.019(2) 0.029(3) 0.029(3) 0.009(2) 0.007(2) -0.003(2) C74 0.023(3) 0.033(3) 0.028(3) 0.006(2) 0.002(2) -0.002(2) C75 0.030(3) 0.031(3) 0.061(4) 0.016(3) 0.000(3) -0.002(2) C76 0.017(2) 0.017(2) 0.025(2) -0.0083(18) 0.0055(19) 0.0019(18) C77 0.028(3) 0.023(2) 0.025(2) -0.0079(19) 0.010(2) -0.002(2) C78 0.046(3) 0.028(3) 0.029(3) -0.012(2) 0.019(2) -0.002(2) C79 0.050(3) 0.023(3) 0.037(3) -0.016(2) 0.015(3) -0.003(2) C80 0.039(3) 0.012(2) 0.041(3) -0.002(2) 0.008(3) 0.001(2) C81 0.026(2) 0.019(2) 0.023(2) -0.0016(19) 0.008(2) 0.0024(19) C82 0.049(3) 0.023(2) 0.023(2) -0.004(2) 0.017(2) -0.008(2) C83 0.054(4) 0.032(3) 0.034(3) -0.005(2) 0.016(3) -0.003(3) C84 0.109(6) 0.037(3) 0.031(3) 0.000(3) 0.021(4) 0.012(4) C85 0.018(2) 0.011(2) 0.019(2) -0.0010(16) 0.0080(18) -0.0021(17) C86 0.018(2) 0.016(2) 0.018(2) -0.0008(17) 0.0069(18) -0.0010(17) C87 0.022(2) 0.017(2) 0.026(2) -0.0023(18) 0.008(2) 0.0040(18) C88 0.026(3) 0.017(2) 0.027(2) -0.0075(19) 0.005(2) -0.0005(19) C89 0.022(2) 0.025(2) 0.019(2) -0.0068(18) 0.0015(19) 0.0003(19) C90 0.022(2) 0.017(2) 0.021(2) 0.0011(17) 0.0081(19) 0.0028(18) C91 0.021(2) 0.021(2) 0.021(2) -0.0041(18) 0.0019(19) 0.0046(19) C92 0.013(2) 0.044(3) 0.037(3) -0.014(2) 0.004(2) 0.000(2) C93 0.033(3) 0.071(4) 0.045(4) -0.023(3) 0.021(3) -0.025(3) C94 0.011(2) 0.017(2) 0.017(2) 0.0050(16) 0.0057(17) 0.0041(16) C95 0.020(2) 0.018(2) 0.022(2) 0.0009(18) 0.0080(19) 0.0005(18) C96 0.032(3) 0.016(2) 0.030(3) 0.0030(19) 0.015(2) 0.002(2) C97 0.030(3) 0.027(3) 0.020(2) 0.0074(19) 0.013(2) 0.003(2) C98 0.026(2) 0.021(2) 0.015(2) -0.0026(17) 0.0107(19) -0.0024(19) C99 0.014(2) 0.014(2) 0.018(2) -0.0017(17) 0.0051(17) -0.0004(17) C100 0.026(3) 0.016(2) 0.024(2) 0.0000(18) 0.009(2) 0.0000(19) C101 0.033(3) 0.017(2) 0.037(3) -0.004(2) 0.011(2) -0.007(2) C10A 0.033(3) 0.017(2) 0.037(3) -0.004(2) 0.011(2) -0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C6 1.902(4) . ? Fe1 C7 1.910(4) . ? Fe1 C3 2.099(4) . ? Fe1 C1 2.113(4) . ? Fe1 P1 2.1192(13) . ? Fe1 C4 2.123(4) . ? Fe1 C2 2.125(4) . ? Fe1 C5 2.126(5) . ? Fe1 Fe2 2.5182(10) . ? Fe2 C7 1.890(4) . ? Fe2 C6 1.919(4) . ? Fe2 C8 2.101(4) . ? Fe2 P2 2.1097(13) . ? Fe2 C9 2.121(4) . ? Fe2 C10 2.132(4) . ? Fe2 C12 2.135(4) . ? Fe2 C11 2.140(4) . ? Fe3 C60 1.908(4) . ? Fe3 C61 1.932(4) . ? Fe3 C58 2.110(4) . ? Fe3 C55 2.114(4) . ? Fe3 P3 2.1147(13) . ? Fe3 C57 2.123(4) . ? Fe3 C59 2.123(4) . ? Fe3 C56 2.130(4) . ? Fe3 Fe4 2.5221(10) . ? Fe4 C61 1.891(4) . ? Fe4 C60 1.920(4) . ? Fe4 C64 2.102(4) . ? Fe4 P4 2.1178(13) . ? Fe4 C66 2.120(4) . ? Fe4 C63 2.126(4) . ? Fe4 C65 2.126(4) . ? Fe4 C62 2.133(4) . ? P1 O4 1.628(3) . ? P1 O3 1.636(3) . ? P1 N1 1.700(3) . ? P2 O6 1.627(3) . ? P2 O5 1.628(3) . ? P2 N1 1.701(3) . ? P3 O10 1.622(3) . ? P3 O9 1.634(3) . ? P3 N2 1.697(3) . ? P4 O11 1.627(3) . ? P4 O12 1.631(3) . ? P4 N2 1.698(3) . ? O1 C6 1.181(5) . ? O2 C7 1.207(5) . ? O3 C13 1.401(5) . ? O4 C22 1.391(5) . ? O5 C31 1.412(5) . ? O6 C40 1.404(5) . ? O7 C60 1.185(5) . ? O8 C61 1.194(5) . ? O9 C67 1.396(5) . ? O10 C76 1.397(5) . ? O11 C85 1.402(5) . ? O12 C94 1.411(5) . ? N1 C49 1.456(5) . ? N2 C52 1.451(5) . ? C1 C2 1.411(6) . ? C1 C5 1.430(7) . ? C1 H1 0.9500 . ? C2 C3 1.407(7) . ? C2 H2 0.9500 . ? C3 C4 1.417(7) . ? C3 H3 0.9500 . ? C4 C5 1.405(6) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C8 C12 1.414(6) . ? C8 C9 1.431(6) . ? C8 H8 0.9500 . ? C9 C10 1.415(6) . ? C9 H9 0.9500 . ? C10 C11 1.414(6) . ? C10 H10 0.9500 . ? C11 C12 1.412(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.389(6) . ? C13 C14 1.401(6) . ? C14 C15 1.395(6) . ? C14 C19 1.509(6) . ? C15 C16 1.390(7) . ? C15 H15 0.9500 . ? C16 C17 1.381(7) . ? C16 H16 0.9500 . ? C17 C18 1.386(6) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.493(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.324(7) . ? C20 H20 0.9500 . ? C21 H21A 0.9500 . ? C21 H21B 0.9500 . ? C22 C27 1.369(6) . ? C22 C23 1.404(6) . ? C23 C24 1.395(7) . ? C23 C28 1.500(6) . ? C24 C25 1.378(8) . ? C24 H24 0.9500 . ? C25 C26 1.394(8) . ? C25 H25 0.9500 . ? C26 C27 1.388(7) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.507(7) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.309(8) . ? C29 H29 0.9500 . ? C30 H30A 0.9500 . ? C30 H30B 0.9500 . ? C31 C36 1.370(6) . ? C31 C32 1.404(6) . ? C32 C33 1.400(6) . ? C32 C37 1.523(6) . ? C33 C34 1.379(7) . ? C33 H33 0.9500 . ? C34 C35 1.376(6) . ? C34 H34 0.9500 . ? C35 C36 1.396(6) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.475(7) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.328(8) . ? C38 H38 0.9500 . ? C39 H39A 0.9500 . ? C39 H39B 0.9500 . ? C40 C45 1.385(6) . ? C40 C41 1.391(6) . ? C41 C42 1.405(6) . ? C41 C46 1.508(6) . ? C42 C43 1.379(6) . ? C42 H42 0.9500 . ? C43 C44 1.396(6) . ? C43 H43 0.9500 . ? C44 C45 1.384(6) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.506(6) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.305(7) . ? C47 H47 0.9500 . ? C48 H48A 0.9500 . ? C48 H48B 0.9500 . ? C49 C54 1.392(6) . ? C49 C50 1.401(5) . ? C50 C51 1.383(5) . ? C50 H50 0.9500 . ? C51 C52 1.393(6) . ? C51 H51 0.9500 . ? C52 C53 1.388(6) . ? C53 C54 1.392(6) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C56 1.413(7) . ? C55 C59 1.419(6) . ? C55 H55 0.9500 . ? C56 C57 1.418(7) . ? C56 H56 0.9500 . ? C57 C58 1.428(6) . ? C57 H57 0.9500 . ? C58 C59 1.416(6) . ? C58 H58 0.9500 . ? C59 H59 0.9500 . ? C62 C63 1.414(6) . ? C62 C66 1.418(6) . ? C62 H62 0.9500 . ? C63 C64 1.429(6) . ? C63 H63 0.9500 . ? C64 C65 1.416(6) . ? C64 H64 0.9500 . ? C65 C66 1.406(7) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C67 C72 1.380(6) . ? C67 C68 1.403(6) . ? C68 C69 1.391(6) . ? C68 C73 1.510(6) . ? C69 C70 1.381(7) . ? C69 H69 0.9500 . ? C70 C71 1.380(7) . ? C70 H70 0.9500 . ? C71 C72 1.380(6) . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? C73 C74 1.498(7) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C75 1.308(7) . ? C74 H74 0.9500 . ? C75 H75A 0.9500 . ? C75 H75B 0.9500 . ? C76 C81 1.390(6) . ? C76 C77 1.392(6) . ? C77 C78 1.393(6) . ? C77 C82 1.522(6) . ? C78 C79 1.386(7) . ? C78 H78 0.9500 . ? C79 C80 1.384(7) . ? C79 H79 0.9500 . ? C80 C81 1.395(6) . ? C80 H80 0.9500 . ? C81 H81 0.9500 . ? C82 C83 1.488(7) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 C84 1.318(7) . ? C83 H83 0.9500 . ? C84 H84A 0.9500 . ? C84 H84B 0.9500 . ? C85 C86 1.389(6) . ? C85 C90 1.395(6) . ? C86 C87 1.397(6) . ? C86 C91 1.505(6) . ? C87 C88 1.393(6) . ? C87 H87 0.9500 . ? C88 C89 1.372(6) . ? C88 H88 0.9500 . ? C89 C90 1.390(6) . ? C89 H89 0.9500 . ? C90 H90 0.9500 . ? C91 C92 1.497(7) . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? C92 C93 1.300(7) . ? C92 H92 0.9500 . ? C93 H93A 0.9500 . ? C93 H93B 0.9500 . ? C94 C95 1.382(6) . ? C94 C99 1.390(6) . ? C95 C96 1.402(6) . ? C95 C100 1.522(6) . ? C96 C97 1.388(6) . ? C96 H96 0.9500 . ? C97 C98 1.388(6) . ? C97 H97 0.9500 . ? C98 C99 1.373(6) . ? C98 H98 0.9500 . ? C99 H99 0.9500 . ? C100 C101 1.505(6) . ? C100 H10A 0.9900 . ? C100 H10B 0.9900 . ? C101 C102 1.312(8) . ? C101 H101 0.9500 . ? C102 H10C 0.9500 . ? C102 H10D 0.9500 . ? C11A H11A 0.9500 . ? C11A H11B 0.9500 . ? 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 C6 Fe1 C7 96.84(18) . . ? C6 Fe1 C3 116.66(19) . . ? C7 Fe1 C3 88.46(18) . . ? C6 Fe1 C1 135.92(19) . . ? C7 Fe1 C1 126.82(19) . . ? C3 Fe1 C1 65.10(18) . . ? C6 Fe1 P1 84.28(13) . . ? C7 Fe1 P1 96.00(13) . . ? C3 Fe1 P1 158.00(14) . . ? C1 Fe1 P1 95.52(13) . . ? C6 Fe1 C4 89.04(18) . . ? C7 Fe1 C4 120.49(19) . . ? C3 Fe1 C4 39.21(19) . . ? C1 Fe1 C4 65.39(19) . . ? P1 Fe1 C4 143.45(14) . . ? C6 Fe1 C2 154.07(19) . . ? C7 Fe1 C2 91.69(18) . . ? C3 Fe1 C2 38.92(18) . . ? C1 Fe1 C2 38.90(17) . . ? P1 Fe1 C2 119.21(13) . . ? C4 Fe1 C2 65.66(19) . . ? C6 Fe1 C5 98.49(19) . . ? C7 Fe1 C5 153.38(18) . . ? C3 Fe1 C5 65.21(19) . . ? C1 Fe1 C5 39.42(18) . . ? P1 Fe1 C5 107.06(13) . . ? C4 Fe1 C5 38.61(17) . . ? C2 Fe1 C5 65.68(19) . . ? C6 Fe1 Fe2 49.08(13) . . ? C7 Fe1 Fe2 48.14(13) . . ? C3 Fe1 Fe2 103.70(13) . . ? C1 Fe1 Fe2 168.70(13) . . ? P1 Fe1 Fe2 95.18(4) . . ? C4 Fe1 Fe2 107.27(13) . . ? C2 Fe1 Fe2 131.03(13) . . ? C5 Fe1 Fe2 138.95(14) . . ? C7 Fe2 C6 96.92(19) . . ? C7 Fe2 C8 123.33(18) . . ? C6 Fe2 C8 139.46(19) . . ? C7 Fe2 P2 87.33(13) . . ? C6 Fe2 P2 92.41(13) . . ? C8 Fe2 P2 93.97(12) . . ? C7 Fe2 C9 157.76(18) . . ? C6 Fe2 C9 100.34(18) . . ? C8 Fe2 C9 39.62(17) . . ? P2 Fe2 C9 105.74(13) . . ? C7 Fe2 C10 129.84(18) . . ? C6 Fe2 C10 85.92(18) . . ? C8 Fe2 C10 65.54(17) . . ? P2 Fe2 C10 142.76(13) . . ? C9 Fe2 C10 38.87(16) . . ? C7 Fe2 C12 92.52(18) . . ? C6 Fe2 C12 148.00(18) . . ? C8 Fe2 C12 38.99(17) . . ? P2 Fe2 C12 118.61(13) . . ? C9 Fe2 C12 65.51(17) . . ? C10 Fe2 C12 64.90(17) . . ? C7 Fe2 C11 95.79(18) . . ? C6 Fe2 C11 109.80(18) . . ? C8 Fe2 C11 65.24(17) . . ? P2 Fe2 C11 156.94(13) . . ? C9 Fe2 C11 65.19(17) . . ? C10 Fe2 C11 38.66(16) . . ? C12 Fe2 C11 38.58(17) . . ? C7 Fe2 Fe1 48.83(13) . . ? C6 Fe2 Fe1 48.47(13) . . ? C8 Fe2 Fe1 167.84(13) . . ? P2 Fe2 Fe1 94.76(4) . . ? C9 Fe2 Fe1 143.89(13) . . ? C10 Fe2 Fe1 111.10(12) . . ? C12 Fe2 Fe1 128.87(13) . . ? C11 Fe2 Fe1 104.50(13) . . ? C60 Fe3 C61 96.75(18) . . ? C60 Fe3 C58 134.00(18) . . ? C61 Fe3 C58 128.91(18) . . ? C60 Fe3 C55 117.49(18) . . ? C61 Fe3 C55 88.67(18) . . ? C58 Fe3 C55 65.40(18) . . ? C60 Fe3 P3 84.90(12) . . ? C61 Fe3 P3 96.27(12) . . ? C58 Fe3 P3 94.16(13) . . ? C55 Fe3 P3 156.42(13) . . ? C60 Fe3 C57 97.00(18) . . ? C61 Fe3 C57 153.95(17) . . ? C58 Fe3 C57 39.43(17) . . ? C55 Fe3 C57 65.34(18) . . ? P3 Fe3 C57 106.91(13) . . ? C60 Fe3 C59 154.43(18) . . ? C61 Fe3 C59 93.21(18) . . ? C58 Fe3 C59 39.09(17) . . ? C55 Fe3 C59 39.13(17) . . ? P3 Fe3 C59 117.38(13) . . ? C57 Fe3 C59 65.82(18) . . ? C60 Fe3 C56 89.02(18) . . ? C61 Fe3 C56 119.49(18) . . ? C58 Fe3 C56 65.62(18) . . ? C55 Fe3 C56 38.89(18) . . ? P3 Fe3 C56 144.20(14) . . ? C57 Fe3 C56 38.96(18) . . ? C59 Fe3 C56 65.64(18) . . ? C60 Fe3 Fe4 48.99(12) . . ? C61 Fe3 Fe4 48.02(13) . . ? C58 Fe3 Fe4 170.64(13) . . ? C55 Fe3 Fe4 105.24(13) . . ? P3 Fe3 Fe4 95.02(4) . . ? C57 Fe3 Fe4 138.03(13) . . ? C59 Fe3 Fe4 133.30(13) . . ? C56 Fe3 Fe4 107.30(13) . . ? C61 Fe4 C60 97.72(18) . . ? C61 Fe4 C64 124.71(18) . . ? C60 Fe4 C64 137.16(17) . . ? C61 Fe4 P4 86.71(13) . . ? C60 Fe4 P4 93.98(12) . . ? C64 Fe4 P4 94.03(13) . . ? C61 Fe4 C66 93.98(17) . . ? C60 Fe4 C66 110.33(18) . . ? C64 Fe4 C66 65.40(18) . . ? P4 Fe4 C66 155.31(14) . . ? C61 Fe4 C63 157.10(17) . . ? C60 Fe4 C63 98.39(17) . . ? C64 Fe4 C63 39.50(16) . . ? P4 Fe4 C63 108.24(12) . . ? C66 Fe4 C63 65.13(17) . . ? C61 Fe4 C65 92.53(18) . . ? C60 Fe4 C65 148.23(18) . . ? C64 Fe4 C65 39.14(17) . . ? P4 Fe4 C65 116.66(14) . . ? C66 Fe4 C65 38.66(18) . . ? C63 Fe4 C65 65.46(17) . . ? C61 Fe4 C62 127.50(17) . . ? C60 Fe4 C62 84.91(17) . . ? C64 Fe4 C62 65.71(17) . . ? P4 Fe4 C62 145.67(12) . . ? C66 Fe4 C62 38.94(16) . . ? C63 Fe4 C62 38.78(16) . . ? C65 Fe4 C62 65.23(17) . . ? C61 Fe4 Fe3 49.41(13) . . ? C60 Fe4 Fe3 48.58(12) . . ? C64 Fe4 Fe3 169.04(13) . . ? P4 Fe4 Fe3 94.72(4) . . ? C66 Fe4 Fe3 104.44(13) . . ? C63 Fe4 Fe3 141.70(12) . . ? C65 Fe4 Fe3 130.18(14) . . ? C62 Fe4 Fe3 109.45(12) . . ? O4 P1 O3 94.99(15) . . ? O4 P1 N1 103.06(16) . . ? O3 P1 N1 97.48(16) . . ? O4 P1 Fe1 123.96(12) . . ? O3 P1 Fe1 117.66(11) . . ? N1 P1 Fe1 114.98(12) . . ? O6 P2 O5 95.20(15) . . ? O6 P2 N1 96.11(16) . . ? O5 P2 N1 104.51(16) . . ? O6 P2 Fe2 122.01(11) . . ? O5 P2 Fe2 119.34(11) . . ? N1 P2 Fe2 115.43(12) . . ? O10 P3 O9 94.95(15) . . ? O10 P3 N2 96.20(15) . . ? O9 P3 N2 102.86(16) . . ? O10 P3 Fe3 118.63(12) . . ? O9 P3 Fe3 124.18(11) . . ? N2 P3 Fe3 114.93(12) . . ? O11 P4 O12 94.94(14) . . ? O11 P4 N2 95.35(16) . . ? O12 P4 N2 104.23(16) . . ? O11 P4 Fe4 122.85(11) . . ? O12 P4 Fe4 120.32(11) . . ? N2 P4 Fe4 114.62(12) . . ? C13 O3 P1 126.3(3) . . ? C22 O4 P1 129.3(3) . . ? C31 O5 P2 124.8(3) . . ? C40 O6 P2 124.6(3) . . ? C67 O9 P3 128.1(3) . . ? C76 O10 P3 131.1(3) . . ? C85 O11 P4 124.6(3) . . ? C94 O12 P4 123.3(2) . . ? C49 N1 P1 120.4(3) . . ? C49 N1 P2 121.6(3) . . ? P1 N1 P2 117.9(2) . . ? C52 N2 P3 119.4(3) . . ? C52 N2 P4 122.1(3) . . ? P3 N2 P4 118.5(2) . . ? C2 C1 C5 108.5(4) . . ? C2 C1 Fe1 71.0(3) . . ? C5 C1 Fe1 70.8(3) . . ? C2 C1 H1 125.8 . . ? C5 C1 H1 125.8 . . ? Fe1 C1 H1 124.1 . . ? C3 C2 C1 107.0(4) . . ? C3 C2 Fe1 69.6(3) . . ? C1 C2 Fe1 70.1(3) . . ? C3 C2 H2 126.5 . . ? C1 C2 H2 126.5 . . ? Fe1 C2 H2 125.4 . . ? C2 C3 C4 109.2(4) . . ? C2 C3 Fe1 71.5(3) . . ? C4 C3 Fe1 71.3(3) . . ? C2 C3 H3 125.4 . . ? C4 C3 H3 125.4 . . ? Fe1 C3 H3 123.4 . . ? C5 C4 C3 107.6(4) . . ? C5 C4 Fe1 70.8(3) . . ? C3 C4 Fe1 69.5(3) . . ? C5 C4 H4 126.2 . . ? C3 C4 H4 126.2 . . ? Fe1 C4 H4 125.1 . . ? C4 C5 C1 107.6(4) . . ? C4 C5 Fe1 70.6(3) . . ? C1 C5 Fe1 69.8(3) . . ? C4 C5 H5 126.2 . . ? C1 C5 H5 126.2 . . ? Fe1 C5 H5 125.1 . . ? O1 C6 Fe1 137.1(3) . . ? O1 C6 Fe2 139.9(4) . . ? Fe1 C6 Fe2 82.45(18) . . ? O2 C7 Fe2 138.1(3) . . ? O2 C7 Fe1 138.1(3) . . ? Fe2 C7 Fe1 83.03(18) . . ? C12 C8 C9 108.1(4) . . ? C12 C8 Fe2 71.8(2) . . ? C9 C8 Fe2 70.9(2) . . ? C12 C8 H8 126.0 . . ? C9 C8 H8 126.0 . . ? Fe2 C8 H8 123.0 . . ? C10 C9 C8 107.2(4) . . ? C10 C9 Fe2 71.0(2) . . ? C8 C9 Fe2 69.4(2) . . ? C10 C9 H9 126.4 . . ? C8 C9 H9 126.4 . . ? Fe2 C9 H9 124.8 . . ? C11 C10 C9 108.4(4) . . ? C11 C10 Fe2 70.9(2) . . ? C9 C10 Fe2 70.1(2) . . ? C11 C10 H10 125.8 . . ? C9 C10 H10 125.8 . . ? Fe2 C10 H10 124.7 . . ? C12 C11 C10 108.2(4) . . ? C12 C11 Fe2 70.5(2) . . ? C10 C11 Fe2 70.4(2) . . ? C12 C11 H11 125.9 . . ? C10 C11 H11 125.9 . . ? Fe2 C11 H11 124.8 . . ? C11 C12 C8 108.0(4) . . ? C11 C12 Fe2 70.9(2) . . ? C8 C12 Fe2 69.2(2) . . ? C11 C12 H12 126.0 . . ? C8 C12 H12 126.0 . . ? Fe2 C12 H12 125.5 . . ? C18 C13 O3 121.7(4) . . ? C18 C13 C14 121.3(4) . . ? O3 C13 C14 116.9(4) . . ? C15 C14 C13 117.2(4) . . ? C15 C14 C19 120.8(4) . . ? C13 C14 C19 121.9(4) . . ? C16 C15 C14 122.0(5) . . ? C16 C15 H15 119.0 . . ? C14 C15 H15 119.0 . . ? C17 C16 C15 119.3(4) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C16 C17 C18 120.4(4) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C13 119.8(4) . . ? C17 C18 H18 120.1 . . ? C13 C18 H18 120.1 . . ? C20 C19 C14 112.5(4) . . ? C20 C19 H19A 109.1 . . ? C14 C19 H19A 109.1 . . ? C20 C19 H19B 109.1 . . ? C14 C19 H19B 109.1 . . ? H19A C19 H19B 107.8 . . ? C21 C20 C19 124.6(5) . . ? C21 C20 H20 117.7 . . ? C19 C20 H20 117.7 . . ? C20 C21 H21A 120.0 . . ? C20 C21 H21B 120.0 . . ? H21A C21 H21B 120.0 . . ? C27 C22 O4 123.3(4) . . ? C27 C22 C23 122.1(4) . . ? O4 C22 C23 114.6(4) . . ? C24 C23 C22 117.0(5) . . ? C24 C23 C28 120.4(4) . . ? C22 C23 C28 122.6(4) . . ? C25 C24 C23 121.9(5) . . ? C25 C24 H24 119.0 . . ? C23 C24 H24 119.0 . . ? C24 C25 C26 119.2(5) . . ? C24 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? C27 C26 C25 120.3(5) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C22 C27 C26 119.4(5) . . ? C22 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C23 C28 C29 114.2(4) . . ? C23 C28 H28A 108.7 . . ? C29 C28 H28A 108.7 . . ? C23 C28 H28B 108.7 . . ? C29 C28 H28B 108.7 . . ? H28A C28 H28B 107.6 . . ? C30 C29 C28 125.8(5) . . ? C30 C29 H29 117.1 . . ? C28 C29 H29 117.1 . . ? C29 C30 H30A 120.0 . . ? C29 C30 H30B 120.0 . . ? H30A C30 H30B 120.0 . . ? C36 C31 C32 122.4(4) . . ? C36 C31 O5 120.2(4) . . ? C32 C31 O5 117.2(4) . . ? C33 C32 C31 116.2(4) . . ? C33 C32 C37 121.3(4) . . ? C31 C32 C37 122.5(4) . . ? C34 C33 C32 122.2(4) . . ? C34 C33 H33 118.9 . . ? C32 C33 H33 118.9 . . ? C35 C34 C33 119.8(4) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C34 C35 C36 119.9(4) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C31 C36 C35 119.5(4) . . ? C31 C36 H36 120.2 . . ? C35 C36 H36 120.2 . . ? C38 C37 C32 111.4(4) . . ? C38 C37 H37A 109.3 . . ? C32 C37 H37A 109.3 . . ? C38 C37 H37B 109.3 . . ? C32 C37 H37B 109.3 . . ? H37A C37 H37B 108.0 . . ? C39 C38 C37 125.2(7) . . ? C39 C38 H38 117.4 . . ? C37 C38 H38 117.4 . . ? C38 C39 H39A 120.0 . . ? C38 C39 H39B 120.0 . . ? H39A C39 H39B 120.0 . . ? C45 C40 C41 122.0(4) . . ? C45 C40 O6 118.7(4) . . ? C41 C40 O6 119.2(4) . . ? C40 C41 C42 117.5(4) . . ? C40 C41 C46 122.1(4) . . ? C42 C41 C46 120.3(4) . . ? C43 C42 C41 120.9(4) . . ? C43 C42 H42 119.6 . . ? C41 C42 H42 119.6 . . ? C42 C43 C44 120.4(4) . . ? C42 C43 H43 119.8 . . ? C44 C43 H43 119.8 . . ? C45 C44 C43 119.4(4) . . ? C45 C44 H44 120.3 . . ? C43 C44 H44 120.3 . . ? C44 C45 C40 119.7(4) . . ? C44 C45 H45 120.2 . . ? C40 C45 H45 120.2 . . ? C47 C46 C41 113.3(4) . . ? C47 C46 H46A 108.9 . . ? C41 C46 H46A 108.9 . . ? C47 C46 H46B 108.9 . . ? C41 C46 H46B 108.9 . . ? H46A C46 H46B 107.7 . . ? C48 C47 C46 127.8(4) . . ? C48 C47 H47 116.1 . . ? C46 C47 H47 116.1 . . ? C47 C48 H48A 120.0 . . ? C47 C48 H48B 120.0 . . ? H48A C48 H48B 120.0 . . ? C54 C49 C50 119.6(4) . . ? C54 C49 N1 120.3(4) . . ? C50 C49 N1 120.1(4) . . ? C51 C50 C49 120.1(4) . . ? C51 C50 H50 120.0 . . ? C49 C50 H50 120.0 . . ? C50 C51 C52 120.5(4) . . ? C50 C51 H51 119.8 . . ? C52 C51 H51 119.8 . . ? C53 C52 C51 119.3(4) . . ? C53 C52 N2 120.0(4) . . ? C51 C52 N2 120.7(4) . . ? C52 C53 C54 120.8(4) . . ? C52 C53 H53 119.6 . . ? C54 C53 H53 119.6 . . ? C53 C54 C49 119.7(4) . . ? C53 C54 H54 120.2 . . ? C49 C54 H54 120.2 . . ? C56 C55 C59 109.0(4) . . ? C56 C55 Fe3 71.2(3) . . ? C59 C55 Fe3 70.8(2) . . ? C56 C55 H55 125.5 . . ? C59 C55 H55 125.5 . . ? Fe3 C55 H55 124.1 . . ? C55 C56 C57 107.8(4) . . ? C55 C56 Fe3 69.9(3) . . ? C57 C56 Fe3 70.3(3) . . ? C55 C56 H56 126.1 . . ? C57 C56 H56 126.1 . . ? Fe3 C56 H56 125.3 . . ? C56 C57 C58 107.6(4) . . ? C56 C57 Fe3 70.8(3) . . ? C58 C57 Fe3 69.8(2) . . ? C56 C57 H57 126.2 . . ? C58 C57 H57 126.2 . . ? Fe3 C57 H57 124.8 . . ? C59 C58 C57 108.4(4) . . ? C59 C58 Fe3 70.9(2) . . ? C57 C58 Fe3 70.8(2) . . ? C59 C58 H58 125.8 . . ? C57 C58 H58 125.8 . . ? Fe3 C58 H58 124.1 . . ? C58 C59 C55 107.2(4) . . ? C58 C59 Fe3 70.0(2) . . ? C55 C59 Fe3 70.1(2) . . ? C58 C59 H59 126.4 . . ? C55 C59 H59 126.4 . . ? Fe3 C59 H59 125.2 . . ? O7 C60 Fe3 136.6(3) . . ? O7 C60 Fe4 140.4(3) . . ? Fe3 C60 Fe4 82.44(17) . . ? O8 C61 Fe4 138.2(3) . . ? O8 C61 Fe3 138.4(3) . . ? Fe4 C61 Fe3 82.56(17) . . ? C63 C62 C66 107.6(4) . . ? C63 C62 Fe4 70.3(2) . . ? C66 C62 Fe4 70.0(2) . . ? C63 C62 H62 126.2 . . ? C66 C62 H62 126.2 . . ? Fe4 C62 H62 125.0 . . ? C62 C63 C64 107.8(4) . . ? C62 C63 Fe4 70.9(2) . . ? C64 C63 Fe4 69.3(2) . . ? C62 C63 H63 126.1 . . ? C64 C63 H63 126.1 . . ? Fe4 C63 H63 125.3 . . ? C65 C64 C63 107.8(4) . . ? C65 C64 Fe4 71.4(2) . . ? C63 C64 Fe4 71.2(2) . . ? C65 C64 H64 126.1 . . ? C63 C64 H64 126.1 . . ? Fe4 C64 H64 123.0 . . ? C66 C65 C64 107.9(4) . . ? C66 C65 Fe4 70.4(2) . . ? C64 C65 Fe4 69.5(2) . . ? C66 C65 H65 126.1 . . ? C64 C65 H65 126.1 . . ? Fe4 C65 H65 125.6 . . ? C65 C66 C62 108.8(4) . . ? C65 C66 Fe4 70.9(2) . . ? C62 C66 Fe4 71.0(2) . . ? C65 C66 H66 125.6 . . ? C62 C66 H66 125.6 . . ? Fe4 C66 H66 124.1 . . ? C72 C67 O9 123.3(4) . . ? C72 C67 C68 121.3(4) . . ? O9 C67 C68 115.3(4) . . ? C69 C68 C67 117.1(4) . . ? C69 C68 C73 121.3(4) . . ? C67 C68 C73 121.6(4) . . ? C70 C69 C68 122.1(5) . . ? C70 C69 H69 118.9 . . ? C68 C69 H69 118.9 . . ? C71 C70 C69 119.3(5) . . ? C71 C70 H70 120.4 . . ? C69 C70 H70 120.4 . . ? C70 C71 C72 120.4(5) . . ? C70 C71 H71 119.8 . . ? C72 C71 H71 119.8 . . ? C71 C72 C67 119.8(4) . . ? C71 C72 H72 120.1 . . ? C67 C72 H72 120.1 . . ? C74 C73 C68 111.0(4) . . ? C74 C73 H73A 109.4 . . ? C68 C73 H73A 109.4 . . ? C74 C73 H73B 109.4 . . ? C68 C73 H73B 109.4 . . ? H73A C73 H73B 108.0 . . ? C75 C74 C73 124.9(5) . . ? C75 C74 H74 117.5 . . ? C73 C74 H74 117.5 . . ? C74 C75 H75A 120.0 . . ? C74 C75 H75B 120.0 . . ? H75A C75 H75B 120.0 . . ? C81 C76 C77 122.3(4) . . ? C81 C76 O10 122.3(4) . . ? C77 C76 O10 115.3(4) . . ? C76 C77 C78 117.2(4) . . ? C76 C77 C82 120.1(4) . . ? C78 C77 C82 122.6(4) . . ? C79 C78 C77 121.5(5) . . ? C79 C78 H78 119.2 . . ? C77 C78 H78 119.2 . . ? C80 C79 C78 120.2(4) . . ? C80 C79 H79 119.9 . . ? C78 C79 H79 119.9 . . ? C79 C80 C81 119.6(4) . . ? C79 C80 H80 120.2 . . ? C81 C80 H80 120.2 . . ? C76 C81 C80 119.1(4) . . ? C76 C81 H81 120.5 . . ? C80 C81 H81 120.5 . . ? C83 C82 C77 116.9(4) . . ? C83 C82 H82A 108.1 . . ? C77 C82 H82A 108.1 . . ? C83 C82 H82B 108.1 . . ? C77 C82 H82B 108.1 . . ? H82A C82 H82B 107.3 . . ? C84 C83 C82 124.3(6) . . ? C84 C83 H83 117.8 . . ? C82 C83 H83 117.8 . . ? C83 C84 H84A 120.0 . . ? C83 C84 H84B 120.0 . . ? H84A C84 H84B 120.0 . . ? C86 C85 C90 122.1(4) . . ? C86 C85 O11 119.5(4) . . ? C90 C85 O11 118.1(4) . . ? C85 C86 C87 116.8(4) . . ? C85 C86 C91 122.5(4) . . ? C87 C86 C91 120.7(4) . . ? C88 C87 C86 121.7(4) . . ? C88 C87 H87 119.2 . . ? C86 C87 H87 119.2 . . ? C89 C88 C87 120.4(4) . . ? C89 C88 H88 119.8 . . ? C87 C88 H88 119.8 . . ? C88 C89 C90 119.4(4) . . ? C88 C89 H89 120.3 . . ? C90 C89 H89 120.3 . . ? C89 C90 C85 119.6(4) . . ? C89 C90 H90 120.2 . . ? C85 C90 H90 120.2 . . ? C92 C91 C86 114.3(4) . . ? C92 C91 H91A 108.7 . . ? C86 C91 H91A 108.7 . . ? C92 C91 H91B 108.7 . . ? C86 C91 H91B 108.7 . . ? H91A C91 H91B 107.6 . . ? C93 C92 C91 127.5(5) . . ? C93 C92 H92 116.2 . . ? C91 C92 H92 116.2 . . ? C92 C93 H93A 120.0 . . ? C92 C93 H93B 120.0 . . ? H93A C93 H93B 120.0 . . ? C95 C94 C99 122.1(4) . . ? C95 C94 O12 117.8(4) . . ? C99 C94 O12 119.9(4) . . ? C94 C95 C96 117.0(4) . . ? C94 C95 C100 123.2(4) . . ? C96 C95 C100 119.9(4) . . ? C97 C96 C95 121.3(4) . . ? C97 C96 H96 119.3 . . ? C95 C96 H96 119.3 . . ? C98 C97 C96 120.1(4) . . ? C98 C97 H97 120.0 . . ? C96 C97 H97 120.0 . . ? C99 C98 C97 119.5(4) . . ? C99 C98 H98 120.3 . . ? C97 C98 H98 120.3 . . ? C98 C99 C94 120.0(4) . . ? C98 C99 H99 120.0 . . ? C94 C99 H99 120.0 . . ? C101 C100 C95 115.0(4) . . ? C101 C100 H10A 108.5 . . ? C95 C100 H10A 108.5 . . ? C101 C100 H10B 108.5 . . ? C95 C100 H10B 108.5 . . ? H10A C100 H10B 107.5 . . ? C102 C101 C100 124.0(5) . . ? C102 C101 H101 118.0 . . ? C100 C101 H101 118.0 . . ? C101 C102 H10C 120.0 . . ? C101 C102 H10D 120.0 . . ? H10C C102 H10D 120.0 . . ? H11A C11A H11B 120.0 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.584 _refine_diff_density_min -0.576 _refine_diff_density_rms 0.106 _database_code_depnum_ccdc_archive 'CCDC 955817' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_msb436_0m _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C86 H88 Cl4 Cu4 N6 O8 P4' _chemical_formula_sum 'C86 H88 Cl4 Cu4 N6 O8 P4' _chemical_formula_weight 1853.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1635(8) _cell_length_b 14.0031(10) _cell_length_c 16.8906(13) _cell_angle_alpha 69.0670(10) _cell_angle_beta 73.0430(10) _cell_angle_gamma 82.9680(10) _cell_volume 2147.2(3) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9856 _cell_measurement_theta_min 2.164 _cell_measurement_theta_max 29.136 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.433 _exptl_crystal_F_000 954 _exptl_transmission_factor_min 0.734 _exptl_transmission_factor_max 0.928 _exptl_crystal_size_max 0.230 _exptl_crystal_size_mid 0.164 _exptl_crystal_size_min 0.131 _exptl_absorpt_coefficient_mu 1.234 _shelx_estimated_absorpt_T_min 0.764 _shelx_estimated_absorpt_T_max 0.855 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'TWINABS (Sheldrick, 2009)' _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.85 _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5\% in \w, colllected at \f = 0.00, 90.00 and 180.00\% and 2 sets of 800 frames, each of width 0.45\% in \f, collected at \w = --30.00 and 210.00\%. The scan time was 15 sec/frame. Analysis of 1290 reflections having I/\s(I) > 20 and chosen from the full data set with CELL_NOW (Sheldrick, 2008) showed the crystal to belong to the triclinic system and to be twinned by a 180 \% rotation about c*. The raw data were processed using the multi-component version of SAINT under control of the two-component orientation file generated by CELL_NOW. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3660 _diffrn_reflns_number 58798 _diffrn_reflns_av_unetI/netI 0.0336 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.095 _diffrn_reflns_theta_max 29.232 _diffrn_reflns_theta_full 28.500 _diffrn_measured_fraction_theta_max 0.974 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.974 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.974 _diffrn_reflns_point_group_measured_fraction_full 0.997 _reflns_number_total 19646 _reflns_number_gt 15379 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'APEX2 (Bruker AXS, 2009)' _computing_cell_refinement 'SAINT (Bruker AXS, 2009a)' _computing_data_reduction 'SAINT (Bruker AXS, 2013a)' _computing_structure_solution 'SHELXs (Sheldrick, 2008a)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Putz, 2012)' _computing_publication_material 'SHELXTL (Bruker AXS, 2008)' _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. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. The structure was refined as a 2-component twin. Three of the four independent allyl groups are disordered over two sites. These were refined with restraints that their geometry approximate the ideal. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+1.4103P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 19646 _refine_ls_number_parameters 533 _refine_ls_number_restraints 102 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1177 _refine_ls_wR_factor_gt 0.1077 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.005 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.82497(4) 0.20016(2) 0.37141(2) 0.03191(9) Uani 1 1 d . . . . . Cu2 Cu 0.77878(4) 0.38453(2) 0.39139(2) 0.03056(9) Uani 1 1 d . . . . . Cl1 Cl 0.95516(8) 0.26286(5) 0.44332(5) 0.03984(17) Uani 1 1 d . . . . . Cl2 Cl 0.60569(8) 0.26652(6) 0.42898(6) 0.04693(19) Uani 1 1 d . . . . . P1 P 0.91778(6) 0.26687(4) 0.23076(4) 0.02091(12) Uani 1 1 d . . . . . P2 P 0.86395(6) 0.46545(4) 0.25192(4) 0.02000(12) Uani 1 1 d . . . . . O1 O 0.86362(19) 0.23027(13) 0.16501(12) 0.0283(4) Uani 1 1 d . . . . . O2 O 1.08330(17) 0.25269(12) 0.19423(12) 0.0266(4) Uani 1 1 d . . . . . O3 O 0.77267(19) 0.55582(14) 0.19942(12) 0.0300(4) Uani 1 1 d . . . . . O4 O 1.00976(18) 0.52301(13) 0.22020(11) 0.0263(4) Uani 1 1 d . . . . . N1 N 0.9077(2) 0.39568(14) 0.18410(12) 0.0210(4) Uani 1 1 d . . . . . N2 N 0.7958(3) 0.0525(2) 0.43356(18) 0.0468(7) Uani 1 1 d . . . . . N3 N 0.7227(3) 0.45939(19) 0.47549(16) 0.0395(6) Uani 1 1 d . . . . . C1 C 0.7768(3) 0.1452(2) 0.20107(18) 0.0308(5) Uani 1 1 d . . . . . C2 C 0.8353(3) 0.0485(2) 0.2135(2) 0.0427(7) Uani 1 1 d . . . . . H2 H 0.9324 0.0390 0.2003 0.051 Uiso 1 1 calc R U . . . C3 C 0.7495(4) -0.0346(2) 0.2456(3) 0.0554(9) Uani 1 1 d . . . . . H3 H 0.7878 -0.1018 0.2548 0.066 Uiso 1 1 calc R U . . . C4 C 0.6093(4) -0.0195(3) 0.2641(3) 0.0603(11) Uani 1 1 d . . . . . H4 H 0.5509 -0.0764 0.2857 0.072 Uiso 1 1 calc R U . . . C5 C 0.5527(3) 0.0776(2) 0.2516(3) 0.0503(9) Uani 1 1 d . . . . . H5 H 0.4555 0.0867 0.2651 0.060 Uiso 1 1 calc R U . . . C6 C 0.6357(3) 0.1630(2) 0.2194(2) 0.0356(6) Uani 1 1 d . . . . . C7 C 0.5760(3) 0.2702(2) 0.2052(2) 0.0410(7) Uani 0.712(6) 1 d D . P A 1 H7A H 0.5891 0.2943 0.2507 0.049 Uiso 0.712(6) 1 calc R U P A 1 H7B H 0.6279 0.3159 0.1472 0.049 Uiso 0.712(6) 1 calc R U P A 1 C8 C 0.4275(4) 0.2791(3) 0.2085(3) 0.0399(9) Uani 0.712(6) 1 d D . P A 1 H8 H 0.3991 0.2598 0.1676 0.048 Uiso 0.712(6) 1 calc R U P A 1 C9 C 0.3334(6) 0.3123(7) 0.2655(4) 0.0476(15) Uani 0.712(6) 1 d D . P A 1 H9A H 0.3593 0.3320 0.3071 0.057 Uiso 0.712(6) 1 calc R U P A 1 H9B H 0.2396 0.3166 0.2650 0.057 Uiso 0.712(6) 1 calc R U P A 1 C7A C 0.5760(3) 0.2702(2) 0.2052(2) 0.0410(7) Uani 0.288(6) 1 d D . P A 2 H7A1 H 0.6424 0.3123 0.2104 0.049 Uiso 0.288(6) 1 calc R U P A 2 H7A2 H 0.5671 0.2994 0.1443 0.049 Uiso 0.288(6) 1 calc R U P A 2 C8A C 0.4401(6) 0.2800(8) 0.2661(6) 0.0399(9) Uani 0.288(6) 1 d D . P A 2 H8A H 0.4303 0.2549 0.3277 0.048 Uiso 0.288(6) 1 calc R U P A 2 C9A C 0.3332(12) 0.3227(19) 0.2365(11) 0.0476(15) Uani 0.288(6) 1 d D . P A 2 H9A1 H 0.3420 0.3480 0.1750 0.057 Uiso 0.288(6) 1 calc R U P A 2 H9A2 H 0.2473 0.3282 0.2766 0.057 Uiso 0.288(6) 1 calc R U P A 2 C10 C 1.1401(3) 0.15259(18) 0.21319(18) 0.0281(5) Uani 1 1 d . . . . . C11 C 1.1321(3) 0.0925(2) 0.2999(2) 0.0350(6) Uani 1 1 d . . . . . H11 H 1.0893 0.1185 0.3463 0.042 Uiso 1 1 calc R U . . . C12 C 1.1878(3) -0.0065(2) 0.3178(2) 0.0437(7) Uani 1 1 d . . . . . H12 H 1.1813 -0.0494 0.3768 0.052 Uiso 1 1 calc R U . . . C13 C 1.2523(3) -0.0418(2) 0.2493(3) 0.0459(8) Uani 1 1 d . . . . . H13 H 1.2902 -0.1093 0.2613 0.055 Uiso 1 1 calc R U . . . C14 C 1.2621(3) 0.0201(2) 0.1635(2) 0.0424(7) Uani 1 1 d . . . . . H14 H 1.3080 -0.0053 0.1171 0.051 Uiso 1 1 calc R U . . . C15 C 1.2060(3) 0.1193(2) 0.1431(2) 0.0339(6) Uani 1 1 d . . . . . C16 C 1.2314(13) 0.1940(13) 0.0491(11) 0.040(2) Uani 0.5 1 d D U P B 1 H16A H 1.1522 0.1943 0.0260 0.048 Uiso 0.5 1 calc R U P B 1 H16B H 1.2404 0.2640 0.0483 0.048 Uiso 0.5 1 calc R U P B 1 C17 C 1.3581(14) 0.1640(13) -0.0071(9) 0.074(3) Uani 0.5 1 d D U P B 1 H17 H 1.4376 0.1514 0.0141 0.089 Uiso 0.5 1 calc R U P B 1 C18 C 1.373(2) 0.1528(15) -0.0820(11) 0.086(4) Uani 0.5 1 d D U P B 1 H18A H 1.2969 0.1644 -0.1064 0.103 Uiso 0.5 1 calc R U P B 1 H18B H 1.4601 0.1331 -0.1126 0.103 Uiso 0.5 1 calc R U P B 1 C16A C 1.2025(13) 0.1798(13) 0.0486(11) 0.040(2) Uani 0.5 1 d D U P B 2 H16C H 1.1243 0.1554 0.0376 0.048 Uiso 0.5 1 calc R U P B 2 H16D H 1.1828 0.2524 0.0437 0.048 Uiso 0.5 1 calc R U P B 2 C17A C 1.3263(13) 0.1755(12) -0.0220(9) 0.074(3) Uani 0.5 1 d D U P B 2 H17A H 1.4037 0.2102 -0.0257 0.089 Uiso 0.5 1 calc R U P B 2 C18A C 1.344(2) 0.1312(15) -0.0795(12) 0.086(4) Uani 0.5 1 d D U P B 2 H18A H 1.2711 0.0951 -0.0796 0.103 Uiso 0.5 1 calc R U P B 2 H18B H 1.4306 0.1347 -0.1217 0.103 Uiso 0.5 1 calc R U P B 2 C19 C 0.6592(3) 0.60327(19) 0.24340(17) 0.0284(5) Uani 1 1 d . . . . . C20 C 0.6723(3) 0.6457(2) 0.30252(18) 0.0348(6) Uani 1 1 d . . . . . H20 H 0.7582 0.6431 0.3151 0.042 Uiso 1 1 calc R U . . . C21 C 0.5576(3) 0.6928(2) 0.3438(2) 0.0409(7) Uani 1 1 d . . . . . H21 H 0.5641 0.7208 0.3860 0.049 Uiso 1 1 calc R U . . . C22 C 0.4349(3) 0.6984(2) 0.3231(2) 0.0423(7) Uani 1 1 d . . . . . H22 H 0.3565 0.7300 0.3514 0.051 Uiso 1 1 calc R U . . . C23 C 0.4254(3) 0.6582(2) 0.2612(2) 0.0431(7) Uani 1 1 d . . . . . H23 H 0.3407 0.6644 0.2464 0.052 Uiso 1 1 calc R U . . . C24 C 0.5372(3) 0.6087(2) 0.2200(2) 0.0351(6) Uani 1 1 d . . . . . C25 C 0.5331(3) 0.5635(3) 0.1507(3) 0.0512(8) Uani 1 1 d . . . . . H25A H 0.6094 0.5927 0.0978 0.061 Uiso 1 1 calc R U . . . H25B H 0.5515 0.4889 0.1737 0.061 Uiso 1 1 calc R U . . . C26 C 0.4047(4) 0.5792(3) 0.1229(3) 0.0636(10) Uani 1 1 d . . . . . H26 H 0.3204 0.5622 0.1674 0.076 Uiso 1 1 calc R U . . . C27 C 0.4002(6) 0.6143(4) 0.0427(4) 0.0926(17) Uani 1 1 d . . . . . H27A H 0.4828 0.6320 -0.0033 0.111 Uiso 1 1 calc R U . . . H27B H 0.3142 0.6226 0.0291 0.111 Uiso 1 1 calc R U . . . C28 C 1.0235(2) 0.59291(19) 0.25960(16) 0.0249(5) Uani 1 1 d . . . . . C29 C 1.0280(3) 0.5563(2) 0.34661(18) 0.0312(5) Uani 1 1 d . . . . . H29 H 1.0235 0.4850 0.3786 0.037 Uiso 1 1 calc R U . . . C30 C 1.0393(3) 0.6251(2) 0.3864(2) 0.0381(6) Uani 1 1 d . . . . . H30 H 1.0406 0.6013 0.4463 0.046 Uiso 1 1 calc R U . . . C31 C 1.0485(3) 0.7280(2) 0.3386(2) 0.0391(7) Uani 1 1 d . . . . . H31 H 1.0553 0.7754 0.3658 0.047 Uiso 1 1 calc R U . . . C32 C 1.0479(3) 0.7625(2) 0.2514(2) 0.0383(6) Uani 1 1 d . . . . . H32 H 1.0566 0.8336 0.2190 0.046 Uiso 1 1 calc R U . . . C33 C 1.0350(3) 0.6960(2) 0.20935(18) 0.0314(5) Uani 1 1 d . . . . . C34 C 1.0477(10) 0.7271(8) 0.1166(9) 0.0395(18) Uani 0.5 1 d D U P C 1 H34A H 0.9530 0.7292 0.1110 0.047 Uiso 0.5 1 calc R U P C 1 H34B H 1.0964 0.6700 0.0977 0.047 Uiso 0.5 1 calc R U P C 1 C35 C 1.1124(11) 0.8206(7) 0.0498(6) 0.067(2) Uani 0.5 1 d D U P C 1 H35 H 1.0508 0.8702 0.0239 0.080 Uiso 0.5 1 calc R U P C 1 C36 C 1.2372(12) 0.8458(11) 0.0211(9) 0.123(4) Uani 0.5 1 d D U P C 1 H36A H 1.3053 0.8002 0.0437 0.148 Uiso 0.5 1 calc R U P C 1 H36B H 1.2630 0.9102 -0.0231 0.148 Uiso 0.5 1 calc R U P C 1 C34A C 1.0116(11) 0.7399(8) 0.1133(10) 0.0395(18) Uani 0.5 1 d D U P C 2 H34C H 1.0616 0.6970 0.0780 0.047 Uiso 0.5 1 calc R U P C 2 H34D H 0.9125 0.7409 0.1169 0.047 Uiso 0.5 1 calc R U P C 2 C35A C 1.0646(12) 0.8441(7) 0.0731(6) 0.067(2) Uani 0.5 1 d D U P C 2 H35A H 1.0255 0.8882 0.1059 0.080 Uiso 0.5 1 calc R U P C 2 C36A C 1.1548(13) 0.8849(11) 0.0011(7) 0.123(4) Uani 0.5 1 d D U P C 2 H36C H 1.1988 0.8458 -0.0355 0.148 Uiso 0.5 1 calc R U P C 2 H36D H 1.1780 0.9544 -0.0159 0.148 Uiso 0.5 1 calc R U P C 2 C37 C 0.9567(2) 0.44730(16) 0.08967(14) 0.0201(4) Uani 1 1 d . . . . . C38 C 1.0940(2) 0.47401(18) 0.05053(15) 0.0237(5) Uani 1 1 d . . . . . H38 H 1.1582 0.4561 0.0849 0.028 Uiso 1 1 calc R U . . . C39 C 1.1363(2) 0.52697(18) -0.03905(15) 0.0231(5) Uani 1 1 d . . . . . H39 H 1.2298 0.5458 -0.0660 0.028 Uiso 1 1 calc R U . . . C40 C 0.7656(4) -0.0304(3) 0.4633(3) 0.0532(9) Uani 1 1 d . U . . . C41 C 0.7267(5) -0.1370(3) 0.5003(4) 0.0993(19) Uani 1 1 d . U . . . H41A H 0.6300 -0.1417 0.5030 0.149 Uiso 1 1 calc R U . . . H41B H 0.7392 -0.1667 0.5598 0.149 Uiso 1 1 calc R U . . . H41C H 0.7847 -0.1746 0.4632 0.149 Uiso 1 1 calc R U . . . C42 C 0.7047(3) 0.5101(2) 0.5170(2) 0.0415(7) Uani 1 1 d . . . . . C43 C 0.6858(5) 0.5754(3) 0.5700(3) 0.0619(11) Uani 1 1 d . . . . . H43A H 0.6916 0.5337 0.6295 0.093 Uiso 1 1 calc R U . . . H43B H 0.5953 0.6097 0.5731 0.093 Uiso 1 1 calc R U . . . H43C H 0.7577 0.6268 0.5432 0.093 Uiso 1 1 calc R U . . . 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 0.0405(2) 0.02454(16) 0.02373(15) -0.00331(12) -0.00243(13) -0.00560(13) Cu2 0.03667(19) 0.02921(16) 0.02076(15) -0.00603(12) -0.00199(13) -0.00384(13) Cl1 0.0504(4) 0.0379(4) 0.0402(4) -0.0163(3) -0.0254(3) 0.0086(3) Cl2 0.0299(4) 0.0501(4) 0.0563(5) -0.0231(4) 0.0052(3) -0.0103(3) P1 0.0223(3) 0.0180(3) 0.0213(3) -0.0054(2) -0.0045(2) -0.0035(2) P2 0.0210(3) 0.0192(3) 0.0187(3) -0.0061(2) -0.0040(2) -0.0005(2) O1 0.0319(9) 0.0271(9) 0.0275(9) -0.0098(7) -0.0056(7) -0.0109(7) O2 0.0224(8) 0.0197(8) 0.0341(9) -0.0065(7) -0.0054(7) -0.0006(6) O3 0.0297(10) 0.0306(9) 0.0236(8) -0.0066(7) -0.0052(7) 0.0093(7) O4 0.0251(9) 0.0283(9) 0.0279(9) -0.0137(7) -0.0036(7) -0.0060(7) N1 0.0248(10) 0.0182(9) 0.0182(9) -0.0051(7) -0.0038(7) -0.0027(7) N2 0.0551(17) 0.0318(13) 0.0406(14) 0.0003(11) -0.0062(12) -0.0094(12) N3 0.0493(15) 0.0363(13) 0.0256(11) -0.0086(10) -0.0032(10) 0.0033(11) C1 0.0337(14) 0.0268(12) 0.0351(14) -0.0119(10) -0.0083(11) -0.0103(10) C2 0.0375(16) 0.0345(15) 0.062(2) -0.0215(14) -0.0137(14) -0.0032(12) C3 0.052(2) 0.0289(15) 0.090(3) -0.0219(17) -0.022(2) -0.0044(14) C4 0.047(2) 0.0320(16) 0.099(3) -0.0178(18) -0.015(2) -0.0163(14) C5 0.0345(16) 0.0349(16) 0.081(3) -0.0177(16) -0.0121(16) -0.0113(13) C6 0.0334(14) 0.0275(13) 0.0467(16) -0.0119(12) -0.0099(12) -0.0069(11) C7 0.0330(15) 0.0308(14) 0.0586(19) -0.0130(13) -0.0122(14) -0.0054(11) C8 0.036(2) 0.0375(19) 0.051(2) -0.0159(18) -0.0168(18) -0.0037(16) C9 0.043(2) 0.049(3) 0.052(4) -0.022(4) -0.004(2) -0.0077(17) C7A 0.0330(15) 0.0308(14) 0.0586(19) -0.0130(13) -0.0122(14) -0.0054(11) C8A 0.036(2) 0.0375(19) 0.051(2) -0.0159(18) -0.0168(18) -0.0037(16) C9A 0.043(2) 0.049(3) 0.052(4) -0.022(4) -0.004(2) -0.0077(17) C10 0.0232(12) 0.0201(11) 0.0389(14) -0.0056(10) -0.0106(10) -0.0009(9) C11 0.0334(14) 0.0322(14) 0.0391(15) -0.0070(11) -0.0151(12) -0.0014(11) C12 0.0437(17) 0.0305(14) 0.0525(19) 0.0017(13) -0.0250(15) -0.0032(12) C13 0.0412(17) 0.0245(13) 0.073(2) -0.0115(14) -0.0245(16) 0.0042(12) C14 0.0383(16) 0.0322(15) 0.060(2) -0.0204(14) -0.0145(14) 0.0069(12) C15 0.0295(14) 0.0291(13) 0.0425(15) -0.0119(11) -0.0098(11) 0.0012(10) C16 0.039(4) 0.038(4) 0.0397(17) -0.013(2) -0.007(3) -0.001(3) C17 0.088(5) 0.058(4) 0.054(4) -0.006(3) -0.011(3) 0.021(4) C18 0.121(8) 0.043(7) 0.063(3) -0.020(4) 0.027(4) -0.014(5) C16A 0.039(4) 0.038(4) 0.0397(17) -0.013(2) -0.007(3) -0.001(3) C17A 0.088(5) 0.058(4) 0.054(4) -0.006(3) -0.011(3) 0.021(4) C18A 0.121(8) 0.043(7) 0.063(3) -0.020(4) 0.027(4) -0.014(5) C19 0.0281(13) 0.0225(11) 0.0254(12) -0.0030(9) -0.0024(10) 0.0054(9) C20 0.0357(15) 0.0336(14) 0.0309(13) -0.0092(11) -0.0083(11) 0.0075(11) C21 0.0496(18) 0.0318(14) 0.0325(14) -0.0100(12) -0.0043(13) 0.0119(12) C22 0.0380(16) 0.0290(14) 0.0419(16) -0.0050(12) 0.0030(13) 0.0100(12) C23 0.0297(15) 0.0311(14) 0.061(2) -0.0108(14) -0.0089(14) 0.0060(11) C24 0.0305(14) 0.0259(12) 0.0448(16) -0.0096(11) -0.0086(12) 0.0030(10) C25 0.0386(17) 0.0477(18) 0.078(3) -0.0320(18) -0.0204(17) 0.0066(14) C26 0.051(2) 0.071(3) 0.079(3) -0.038(2) -0.021(2) 0.0060(19) C27 0.101(4) 0.117(4) 0.084(4) -0.042(3) -0.044(3) -0.017(3) C28 0.0221(11) 0.0276(12) 0.0287(12) -0.0136(10) -0.0061(9) -0.0032(9) C29 0.0320(14) 0.0321(13) 0.0326(13) -0.0101(11) -0.0134(11) -0.0030(10) C30 0.0370(15) 0.0509(17) 0.0340(14) -0.0206(13) -0.0106(12) -0.0067(13) C31 0.0356(15) 0.0450(16) 0.0472(17) -0.0284(14) -0.0087(13) -0.0057(12) C32 0.0396(16) 0.0296(13) 0.0490(17) -0.0166(12) -0.0106(13) -0.0057(11) C33 0.0342(14) 0.0286(13) 0.0329(13) -0.0101(11) -0.0093(11) -0.0062(10) C34 0.051(5) 0.033(2) 0.0366(18) 0.0019(19) -0.028(3) -0.009(3) C35 0.101(5) 0.058(4) 0.037(4) -0.006(2) -0.011(3) -0.030(3) C36 0.143(9) 0.118(8) 0.108(6) -0.011(5) -0.036(6) -0.075(7) C34A 0.051(5) 0.033(2) 0.0366(18) 0.0019(19) -0.028(3) -0.009(3) C35A 0.101(5) 0.058(4) 0.037(4) -0.006(2) -0.011(3) -0.030(3) C36A 0.143(9) 0.118(8) 0.108(6) -0.011(5) -0.036(6) -0.075(7) C37 0.0238(11) 0.0173(10) 0.0182(10) -0.0060(8) -0.0037(8) -0.0018(8) C38 0.0223(11) 0.0271(11) 0.0220(11) -0.0074(9) -0.0074(9) -0.0012(9) C39 0.0205(11) 0.0246(11) 0.0231(11) -0.0077(9) -0.0031(9) -0.0041(9) C40 0.0463(19) 0.0354(16) 0.066(2) 0.0022(15) -0.0188(17) -0.0081(14) C41 0.088(3) 0.040(2) 0.150(5) 0.018(3) -0.057(3) -0.023(2) C42 0.0513(18) 0.0355(15) 0.0304(14) -0.0088(12) -0.0074(13) 0.0103(13) C43 0.089(3) 0.047(2) 0.054(2) -0.0297(17) -0.021(2) 0.0246(19) _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 1.970(3) . ? Cu1 P1 2.1746(7) . ? Cu1 Cl2 2.3770(8) . ? Cu1 Cl1 2.4455(8) . ? Cu1 Cu2 2.6894(5) . ? Cu2 N3 1.971(3) . ? Cu2 P2 2.1740(7) . ? Cu2 Cl2 2.3535(8) . ? Cu2 Cl1 2.4469(8) . ? P1 O1 1.6222(18) . ? P1 O2 1.6281(18) . ? P1 N1 1.6944(19) . ? P2 O3 1.6244(18) . ? P2 O4 1.6290(18) . ? P2 N1 1.691(2) . ? O1 C1 1.412(3) . ? O2 C10 1.411(3) . ? O3 C19 1.410(3) . ? O4 C28 1.405(3) . ? N1 C37 1.454(3) . ? N2 C40 1.129(4) . ? N3 C42 1.131(4) . ? C1 C2 1.380(4) . ? C1 C6 1.387(4) . ? C2 C3 1.389(4) . ? C2 H2 0.9500 . ? C3 C4 1.373(5) . ? C3 H3 0.9500 . ? C4 C5 1.378(5) . ? C4 H4 0.9500 . ? C5 C6 1.396(4) . ? C5 H5 0.9500 . ? C6 C7 1.512(4) . ? C7 C8 1.485(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.316(5) . ? C8 H8 0.9500 . ? C9 H9A 0.9500 . ? C9 H9B 0.9500 . ? C8A C9A 1.317(6) . ? C8A H8A 0.9500 . ? C9A H9A1 0.9500 . ? C9A H9A2 0.9500 . ? C10 C15 1.386(4) . ? C10 C11 1.388(4) . ? C11 C12 1.394(4) . ? C11 H11 0.9500 . ? C12 C13 1.378(5) . ? C12 H12 0.9500 . ? C13 C14 1.379(5) . ? C13 H13 0.9500 . ? C14 C15 1.398(4) . ? C14 H14 0.9500 . ? C15 C16 1.525(18) . ? C15 C16A 1.525(18) . ? C16 C17 1.475(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.292(6) . ? C17 H17 0.9500 . ? C18 H18A 0.9500 . ? C18 H18B 0.9500 . ? C16A C17A 1.471(5) . ? C16A H16C 0.9900 . ? C16A H16D 0.9900 . ? C17A C18A 1.289(6) . ? C17A H17A 0.9500 . ? C18A H18A 0.9500 . ? C18A H18B 0.9500 . ? C19 C20 1.375(4) . ? C19 C24 1.393(4) . ? C20 C21 1.395(4) . ? C20 H20 0.9500 . ? C21 C22 1.376(5) . ? C21 H21 0.9500 . ? C22 C23 1.383(5) . ? C22 H22 0.9500 . ? C23 C24 1.395(4) . ? C23 H23 0.9500 . ? C24 C25 1.529(5) . ? C25 C26 1.478(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.279(7) . ? C26 H26 0.9500 . ? C27 H27A 0.9500 . ? C27 H27B 0.9500 . ? C28 C29 1.386(4) . ? C28 C33 1.388(4) . ? C29 C30 1.388(4) . ? C29 H29 0.9500 . ? C30 C31 1.376(4) . ? C30 H30 0.9500 . ? C31 C32 1.378(4) . ? C31 H31 0.9500 . ? C32 C33 1.395(4) . ? C32 H32 0.9500 . ? C33 C34 1.438(15) . ? C33 C34A 1.595(15) . ? C34 C35 1.464(5) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.264(6) . ? C35 H35 0.9500 . ? C36 H36A 0.9500 . ? C36 H36B 0.9500 . ? C34A C35A 1.466(5) . ? C34A H34C 0.9900 . ? C34A H34D 0.9900 . ? C35A C36A 1.276(6) . ? C35A H35A 0.9500 . ? C36A H36C 0.9500 . ? C36A H36D 0.9500 . ? C37 C39 1.387(3) 2_765 ? C37 C38 1.392(3) . ? C38 C39 1.386(3) . ? C38 H38 0.9500 . ? C39 C37 1.387(3) 2_765 ? C39 H39 0.9500 . ? C40 C41 1.452(5) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.455(5) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 P1 123.71(9) . . ? N2 Cu1 Cl2 100.41(9) . . ? P1 Cu1 Cl2 116.97(3) . . ? N2 Cu1 Cl1 108.97(9) . . ? P1 Cu1 Cl1 106.24(3) . . ? Cl2 Cu1 Cl1 97.38(3) . . ? N2 Cu1 Cu2 143.75(9) . . ? P1 Cu1 Cu2 92.44(2) . . ? Cl2 Cu1 Cu2 54.94(2) . . ? Cl1 Cu1 Cu2 56.678(19) . . ? N3 Cu2 P2 120.53(7) . . ? N3 Cu2 Cl2 107.21(8) . . ? P2 Cu2 Cl2 116.63(3) . . ? N3 Cu2 Cl1 103.82(8) . . ? P2 Cu2 Cl1 107.48(3) . . ? Cl2 Cu2 Cl1 97.98(3) . . ? N3 Cu2 Cu1 146.06(7) . . ? P2 Cu2 Cu1 92.98(2) . . ? Cl2 Cu2 Cu1 55.77(2) . . ? Cl1 Cu2 Cu1 56.63(2) . . ? Cu1 Cl1 Cu2 66.69(2) . . ? Cu2 Cl2 Cu1 69.29(2) . . ? O1 P1 O2 100.58(10) . . ? O1 P1 N1 100.90(10) . . ? O2 P1 N1 97.91(9) . . ? O1 P1 Cu1 118.05(7) . . ? O2 P1 Cu1 118.03(7) . . ? N1 P1 Cu1 117.78(7) . . ? O3 P2 O4 100.40(10) . . ? O3 P2 N1 99.79(10) . . ? O4 P2 N1 97.41(9) . . ? O3 P2 Cu2 119.05(7) . . ? O4 P2 Cu2 118.69(7) . . ? N1 P2 Cu2 117.51(7) . . ? C1 O1 P1 118.83(16) . . ? C10 O2 P1 118.30(15) . . ? C19 O3 P2 122.20(16) . . ? C28 O4 P2 118.74(15) . . ? C37 N1 P2 119.46(15) . . ? C37 N1 P1 122.19(15) . . ? P2 N1 P1 117.55(11) . . ? C40 N2 Cu1 170.5(3) . . ? C42 N3 Cu2 171.0(3) . . ? C2 C1 C6 122.7(2) . . ? C2 C1 O1 118.9(2) . . ? C6 C1 O1 118.3(2) . . ? C1 C2 C3 118.7(3) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C4 C3 C2 120.0(3) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.5(3) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C4 C5 C6 121.1(3) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C1 C6 C5 116.9(3) . . ? C1 C6 C7 120.9(2) . . ? C5 C6 C7 122.1(3) . . ? C8 C7 C6 114.1(3) . . ? C8 C7 H7A 108.7 . . ? C6 C7 H7A 108.7 . . ? C8 C7 H7B 108.7 . . ? C6 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C9 C8 C7 123.1(4) . . ? C9 C8 H8 118.4 . . ? C7 C8 H8 118.4 . . ? C8 C9 H9A 120.0 . . ? C8 C9 H9B 120.0 . . ? H9A C9 H9B 120.0 . . ? C9A C8A H8A 119.3 . . ? C8A C9A H9A1 120.0 . . ? C8A C9A H9A2 120.0 . . ? H9A1 C9A H9A2 120.0 . . ? C15 C10 C11 122.5(2) . . ? C15 C10 O2 117.9(2) . . ? C11 C10 O2 119.5(2) . . ? C10 C11 C12 119.0(3) . . ? C10 C11 H11 120.5 . . ? C12 C11 H11 120.5 . . ? C13 C12 C11 119.6(3) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C12 C13 C14 120.5(3) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C13 C14 C15 121.5(3) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C10 C15 C14 116.9(3) . . ? C10 C15 C16 120.0(6) . . ? C14 C15 C16 122.5(6) . . ? C10 C15 C16A 123.0(6) . . ? C14 C15 C16A 119.6(6) . . ? C17 C16 C15 109.9(12) . . ? C17 C16 H16A 109.7 . . ? C15 C16 H16A 109.7 . . ? C17 C16 H16B 109.7 . . ? C15 C16 H16B 109.7 . . ? H16A C16 H16B 108.2 . . ? C18 C17 C16 127.3(10) . . ? C18 C17 H17 116.4 . . ? C16 C17 H17 116.4 . . ? C17 C18 H18A 120.0 . . ? C17 C18 H18B 120.0 . . ? H18A C18 H18B 120.0 . . ? C17A C16A C15 117.6(12) . . ? C17A C16A H16C 107.9 . . ? C15 C16A H16C 107.9 . . ? C17A C16A H16D 107.9 . . ? C15 C16A H16D 107.9 . . ? H16C C16A H16D 107.2 . . ? C18A C17A C16A 129.0(10) . . ? C18A C17A H17A 115.5 . . ? C16A C17A H17A 115.5 . . ? C17A C18A H18A 120.0 . . ? C17A C18A H18B 120.0 . . ? H18A C18A H18B 120.0 . . ? C20 C19 C24 122.8(2) . . ? C20 C19 O3 121.0(2) . . ? C24 C19 O3 116.1(2) . . ? C19 C20 C21 118.9(3) . . ? C19 C20 H20 120.5 . . ? C21 C20 H20 120.5 . . ? C22 C21 C20 119.8(3) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C21 C22 C23 120.2(3) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C24 121.5(3) . . ? C22 C23 H23 119.2 . . ? C24 C23 H23 119.2 . . ? C19 C24 C23 116.6(3) . . ? C19 C24 C25 119.5(3) . . ? C23 C24 C25 123.9(3) . . ? C26 C25 C24 117.1(3) . . ? C26 C25 H25A 108.0 . . ? C24 C25 H25A 108.0 . . ? C26 C25 H25B 108.0 . . ? C24 C25 H25B 108.0 . . ? H25A C25 H25B 107.3 . . ? C27 C26 C25 124.0(5) . . ? C27 C26 H26 118.0 . . ? C25 C26 H26 118.0 . . ? C26 C27 H27A 120.0 . . ? C26 C27 H27B 120.0 . . ? H27A C27 H27B 120.0 . . ? C29 C28 C33 122.4(2) . . ? C29 C28 O4 118.9(2) . . ? C33 C28 O4 118.8(2) . . ? C28 C29 C30 119.1(3) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? C31 C30 C29 119.8(3) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C30 C31 C32 120.1(3) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C31 C32 C33 121.9(3) . . ? C31 C32 H32 119.1 . . ? C33 C32 H32 119.1 . . ? C28 C33 C32 116.7(3) . . ? C28 C33 C34 119.3(6) . . ? C32 C33 C34 123.7(6) . . ? C28 C33 C34A 122.3(5) . . ? C32 C33 C34A 120.3(5) . . ? C33 C34 C35 125.6(11) . . ? C33 C34 H34A 105.9 . . ? C35 C34 H34A 105.9 . . ? C33 C34 H34B 105.9 . . ? C35 C34 H34B 105.9 . . ? H34A C34 H34B 106.2 . . ? C36 C35 C34 130.3(9) . . ? C36 C35 H35 114.9 . . ? C34 C35 H35 114.9 . . ? C35 C36 H36A 120.0 . . ? C35 C36 H36B 120.0 . . ? H36A C36 H36B 120.0 . . ? C35A C34A C33 106.6(10) . . ? C35A C34A H34C 110.4 . . ? C33 C34A H34C 110.4 . . ? C35A C34A H34D 110.4 . . ? C33 C34A H34D 110.4 . . ? H34C C34A H34D 108.6 . . ? C36A C35A C34A 130.3(9) . . ? C36A C35A H35A 114.8 . . ? C34A C35A H35A 114.8 . . ? C35A C36A H36C 120.0 . . ? C35A C36A H36D 120.0 . . ? H36C C36A H36D 120.0 . . ? C39 C37 C38 120.0(2) 2_765 . ? C39 C37 N1 119.1(2) 2_765 . ? C38 C37 N1 120.8(2) . . ? C39 C38 C37 119.4(2) . . ? C39 C38 H38 120.3 . . ? C37 C38 H38 120.3 . . ? C38 C39 C37 120.5(2) . 2_765 ? C38 C39 H39 119.7 . . ? C37 C39 H39 119.7 2_765 . ? N2 C40 C41 179.2(5) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N3 C42 C43 178.4(4) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? _refine_diff_density_max 1.122 _refine_diff_density_min -0.709 _refine_diff_density_rms 0.098 _shelxl_version_number 2013-3 _shelx_res_file ; TITL msb436_0m in P-1 CELL 0.71073 10.1635 14.0031 16.8906 69.067 73.043 82.968 ZERR 1.00 0.0008 0.0010 0.0013 0.001 0.001 0.001 LATT 1 SFAC C H N O P Cl Cu UNIT 86 88 6 8 4 4 4 L.S. 16 OMIT 0 5 3 OMIT 1 5 3 ACTA 57 BOND $H FMAP 2 PLAN 5 SIZE 0.131 0.164 0.23 DFIX 1.477 0.004 C7 C8 C7a C8a C16 C17 C16a C17a C34 C35 C34a C35a DFIX 1.320 0.005 C8 C9 C8a C9a C17 C18 C17a C18a C35 C36 C35a C36a DFIX 2.436 0.008 C7 C9 C7a C9a C16 C18 C16a C18a C34 C36 C34a C36a EADP C36 C36a EADP C35 C35a EADP C34 C34a EADP C18 C18a EADP C17 C17a EADP C16 C16a EXYZ C7 C7a EADP C7 C7a EADP C8 C8a EADP C9 C9a ISOR 0.007 c16 > c18a c34 > C36a C40 ISOR 0.004 C41 TEMP -73 WGHT 0.050900 1.410300 BASF 0.09956 FVAR 0.56422 0.71198 MOLE 1 CU1 7 0.824971 0.200163 0.371413 11.00000 0.04049 0.02454 = 0.02373 -0.00331 -0.00243 -0.00560 CU2 7 0.778776 0.384530 0.391392 11.00000 0.03667 0.02921 = 0.02076 -0.00603 -0.00199 -0.00384 CL1 6 0.955158 0.262858 0.443323 11.00000 0.05043 0.03789 = 0.04020 -0.01626 -0.02540 0.00857 CL2 6 0.605694 0.266519 0.428985 11.00000 0.02995 0.05007 = 0.05633 -0.02311 0.00523 -0.01031 P1 5 0.917777 0.266868 0.230763 11.00000 0.02226 0.01802 = 0.02131 -0.00539 -0.00448 -0.00352 P2 5 0.863946 0.465449 0.251915 11.00000 0.02096 0.01924 = 0.01872 -0.00615 -0.00403 -0.00055 O1 4 0.863622 0.230269 0.165005 11.00000 0.03192 0.02712 = 0.02754 -0.00983 -0.00564 -0.01088 O2 4 1.083301 0.252688 0.194228 11.00000 0.02235 0.01973 = 0.03411 -0.00654 -0.00537 -0.00056 O3 4 0.772674 0.555824 0.199419 11.00000 0.02971 0.03059 = 0.02357 -0.00657 -0.00523 0.00929 O4 4 1.009759 0.523010 0.220203 11.00000 0.02513 0.02830 = 0.02795 -0.01366 -0.00357 -0.00600 N1 3 0.907730 0.395678 0.184097 11.00000 0.02475 0.01824 = 0.01825 -0.00511 -0.00378 -0.00273 N2 3 0.795840 0.052531 0.433555 11.00000 0.05510 0.03184 = 0.04057 0.00032 -0.00624 -0.00938 N3 3 0.722677 0.459388 0.475489 11.00000 0.04931 0.03628 = 0.02563 -0.00864 -0.00322 0.00331 C1 1 0.776768 0.145186 0.201072 11.00000 0.03366 0.02684 = 0.03515 -0.01191 -0.00834 -0.01032 C2 1 0.835332 0.048523 0.213458 11.00000 0.03748 0.03448 = 0.06156 -0.02146 -0.01367 -0.00323 AFIX 43 H2 2 0.932449 0.038968 0.200255 11.00000 -1.20000 AFIX 0 C3 1 0.749517 -0.034584 0.245617 11.00000 0.05244 0.02890 = 0.08960 -0.02195 -0.02220 -0.00435 AFIX 43 H3 2 0.787796 -0.101798 0.254802 11.00000 -1.20000 AFIX 0 C4 1 0.609316 -0.019506 0.264120 11.00000 0.04687 0.03204 = 0.09949 -0.01780 -0.01531 -0.01628 AFIX 43 H4 2 0.550946 -0.076447 0.285725 11.00000 -1.20000 AFIX 0 C5 1 0.552674 0.077634 0.251574 11.00000 0.03451 0.03495 = 0.08066 -0.01770 -0.01213 -0.01134 AFIX 43 H5 2 0.455479 0.086687 0.265081 11.00000 -1.20000 AFIX 0 C6 1 0.635664 0.162951 0.219361 11.00000 0.03337 0.02750 = 0.04669 -0.01188 -0.00992 -0.00693 PART 1 C7 1 0.575993 0.270201 0.205210 21.00000 0.03295 0.03084 = 0.05859 -0.01298 -0.01218 -0.00542 AFIX 23 H7A 2 0.589131 0.294334 0.250740 21.00000 -1.20000 H7B 2 0.627864 0.315872 0.147218 21.00000 -1.20000 AFIX 0 C8 1 0.427489 0.279073 0.208533 21.00000 0.03648 0.03746 = 0.05084 -0.01587 -0.01679 -0.00372 AFIX 43 H8 2 0.399095 0.259832 0.167598 21.00000 -1.20000 AFIX 0 C9 1 0.333408 0.312324 0.265497 21.00000 0.04335 0.04862 = 0.05153 -0.02232 -0.00434 -0.00771 AFIX 93 H9A 2 0.359285 0.332016 0.307083 21.00000 -1.20000 H9B 2 0.239604 0.316640 0.265038 21.00000 -1.20000 PART 2 AFIX 0 C7A 1 0.575993 0.270201 0.205210 -21.00000 0.03295 0.03084 = 0.05859 -0.01298 -0.01218 -0.00542 AFIX 23 H7A1 2 0.642435 0.312283 0.210418 -21.00000 -1.20000 H7A2 2 0.567055 0.299390 0.144254 -21.00000 -1.20000 AFIX 0 C8A 1 0.440137 0.279999 0.266120 -21.00000 0.03648 0.03746 = 0.05084 -0.01587 -0.01679 -0.00372 AFIX 43 H8A 2 0.430257 0.254932 0.327717 -21.00000 -1.20000 AFIX 0 C9A 1 0.333210 0.322696 0.236476 -21.00000 0.04335 0.04862 = 0.05153 -0.02232 -0.00434 -0.00771 AFIX 93 H9A1 2 0.341963 0.348015 0.175004 -21.00000 -1.20000 H9A2 2 0.247308 0.328183 0.276560 -21.00000 -1.20000 PART 0 AFIX 0 C10 1 1.140103 0.152588 0.213193 11.00000 0.02317 0.02005 = 0.03890 -0.00562 -0.01056 -0.00093 C11 1 1.132070 0.092527 0.299890 11.00000 0.03342 0.03218 = 0.03908 -0.00701 -0.01508 -0.00145 AFIX 43 H11 2 1.089283 0.118503 0.346316 11.00000 -1.20000 AFIX 0 C12 1 1.187766 -0.006537 0.317813 11.00000 0.04374 0.03046 = 0.05252 0.00169 -0.02505 -0.00318 AFIX 43 H12 2 1.181307 -0.049411 0.376839 11.00000 -1.20000 AFIX 0 C13 1 1.252259 -0.041840 0.249310 11.00000 0.04123 0.02452 = 0.07279 -0.01154 -0.02449 0.00424 AFIX 43 H13 2 1.290222 -0.109327 0.261320 11.00000 -1.20000 AFIX 0 C14 1 1.262109 0.020053 0.163457 11.00000 0.03828 0.03223 = 0.05962 -0.02036 -0.01448 0.00692 AFIX 43 H14 2 1.308046 -0.005347 0.117106 11.00000 -1.20000 AFIX 0 C15 1 1.206029 0.119294 0.143124 11.00000 0.02955 0.02911 = 0.04252 -0.01188 -0.00977 0.00115 PART 1 C16 1 1.231368 0.194050 0.049063 10.50000 0.03856 0.03778 = 0.03971 -0.01282 -0.00666 -0.00111 AFIX 23 H16A 2 1.152231 0.194289 0.025988 10.50000 -1.20000 H16B 2 1.240432 0.263999 0.048270 10.50000 -1.20000 AFIX 0 C17 1 1.358067 0.164000 -0.007110 10.50000 0.08800 0.05754 = 0.05403 -0.00640 -0.01063 0.02144 AFIX 43 H17 2 1.437618 0.151449 0.014121 10.50000 -1.20000 AFIX 0 C18 1 1.372989 0.152832 -0.081975 10.50000 0.12146 0.04315 = 0.06303 -0.01982 0.02747 -0.01401 AFIX 93 H18A 2 1.296881 0.164381 -0.106398 10.50000 -1.20000 H18B 2 1.460068 0.133073 -0.112587 10.50000 -1.20000 AFIX 0 PART 2 C16A 1 1.202539 0.179770 0.048598 10.50000 0.03856 0.03778 = 0.03971 -0.01282 -0.00666 -0.00111 AFIX 23 H16C 2 1.124320 0.155394 0.037643 10.50000 -1.20000 H16D 2 1.182806 0.252367 0.043689 10.50000 -1.20000 AFIX 0 C17A 1 1.326262 0.175514 -0.021961 10.50000 0.08800 0.05754 = 0.05403 -0.00640 -0.01063 0.02144 AFIX 43 H17A 2 1.403666 0.210234 -0.025655 10.50000 -1.20000 AFIX 0 C18A 1 1.344234 0.131223 -0.079466 10.50000 0.12146 0.04315 = 0.06303 -0.01982 0.02747 -0.01401 AFIX 93 H18A 2 1.271112 0.095073 -0.079601 10.50000 -1.20000 H18B 2 1.430605 0.134722 -0.121723 10.50000 -1.20000 PART 0 AFIX 0 C19 1 0.659180 0.603273 0.243399 11.00000 0.02807 0.02255 = 0.02541 -0.00304 -0.00239 0.00540 C20 1 0.672345 0.645739 0.302517 11.00000 0.03569 0.03357 = 0.03092 -0.00922 -0.00832 0.00746 AFIX 43 H20 2 0.758222 0.643088 0.315069 11.00000 -1.20000 AFIX 0 C21 1 0.557607 0.692765 0.343757 11.00000 0.04961 0.03176 = 0.03248 -0.01004 -0.00425 0.01192 AFIX 43 H21 2 0.564138 0.720829 0.386007 11.00000 -1.20000 AFIX 0 C22 1 0.434906 0.698409 0.323090 11.00000 0.03800 0.02899 = 0.04186 -0.00498 0.00301 0.00997 AFIX 43 H22 2 0.356515 0.730040 0.351414 11.00000 -1.20000 AFIX 0 C23 1 0.425358 0.658167 0.261200 11.00000 0.02967 0.03107 = 0.06069 -0.01082 -0.00889 0.00601 AFIX 43 H23 2 0.340667 0.664356 0.246410 11.00000 -1.20000 AFIX 0 C24 1 0.537208 0.608691 0.219976 11.00000 0.03053 0.02591 = 0.04479 -0.00965 -0.00862 0.00305 C25 1 0.533110 0.563470 0.150689 11.00000 0.03865 0.04774 = 0.07762 -0.03201 -0.02037 0.00664 AFIX 23 H25A 2 0.609448 0.592748 0.097792 11.00000 -1.20000 H25B 2 0.551513 0.488940 0.173731 11.00000 -1.20000 AFIX 0 C26 1 0.404718 0.579180 0.122905 11.00000 0.05145 0.07127 = 0.07892 -0.03753 -0.02129 0.00601 AFIX 43 H26 2 0.320377 0.562154 0.167387 11.00000 -1.20000 AFIX 0 C27 1 0.400193 0.614277 0.042683 11.00000 0.10123 0.11659 = 0.08430 -0.04233 -0.04446 -0.01682 AFIX 93 H27A 2 0.482776 0.632011 -0.003311 11.00000 -1.20000 H27B 2 0.314249 0.622621 0.029068 11.00000 -1.20000 AFIX 0 C28 1 1.023454 0.592911 0.259600 11.00000 0.02205 0.02756 = 0.02865 -0.01357 -0.00608 -0.00317 C29 1 1.028011 0.556280 0.346610 11.00000 0.03198 0.03208 = 0.03260 -0.01013 -0.01341 -0.00304 AFIX 43 H29 2 1.023491 0.484977 0.378647 11.00000 -1.20000 AFIX 0 C30 1 1.039267 0.625129 0.386366 11.00000 0.03703 0.05087 = 0.03399 -0.02057 -0.01061 -0.00668 AFIX 43 H30 2 1.040594 0.601299 0.446323 11.00000 -1.20000 AFIX 0 C31 1 1.048496 0.728027 0.338587 11.00000 0.03557 0.04498 = 0.04722 -0.02838 -0.00873 -0.00568 AFIX 43 H31 2 1.055275 0.775374 0.365778 11.00000 -1.20000 AFIX 0 C32 1 1.047921 0.762489 0.251404 11.00000 0.03958 0.02964 = 0.04900 -0.01661 -0.01059 -0.00575 AFIX 43 H32 2 1.056581 0.833586 0.218994 11.00000 -1.20000 AFIX 0 C33 1 1.034993 0.696011 0.209353 11.00000 0.03419 0.02865 = 0.03288 -0.01008 -0.00929 -0.00617 PART 1 C34 1 1.047689 0.727077 0.116612 10.50000 0.05093 0.03269 = 0.03657 0.00186 -0.02760 -0.00936 AFIX 23 H34A 2 0.952982 0.729198 0.111041 10.50000 -1.20000 H34B 2 1.096359 0.669964 0.097685 10.50000 -1.20000 AFIX 0 C35 1 1.112411 0.820569 0.049795 10.50000 0.10058 0.05765 = 0.03679 -0.00606 -0.01103 -0.02982 AFIX 43 H35 2 1.050818 0.870196 0.023870 10.50000 -1.20000 AFIX 0 C36 1 1.237230 0.845757 0.021114 10.50000 0.14265 0.11771 = 0.10841 -0.01106 -0.03646 -0.07544 AFIX 93 H36A 2 1.305266 0.800250 0.043738 10.50000 -1.20000 H36B 2 1.263014 0.910198 -0.023069 10.50000 -1.20000 PART 2 AFIX 0 C34A 1 1.011594 0.739933 0.113283 10.50000 0.05093 0.03269 = 0.03657 0.00186 -0.02760 -0.00936 AFIX 23 H34C 2 1.061606 0.696980 0.077989 10.50000 -1.20000 H34D 2 0.912483 0.740870 0.116890 10.50000 -1.20000 AFIX 0 C35A 1 1.064605 0.844072 0.073069 10.50000 0.10058 0.05765 = 0.03679 -0.00606 -0.01103 -0.02982 AFIX 43 H35A 2 1.025527 0.888193 0.105867 10.50000 -1.20000 AFIX 0 C36A 1 1.154819 0.884921 0.001077 10.50000 0.14265 0.11771 = 0.10841 -0.01106 -0.03646 -0.07544 AFIX 93 H36C 2 1.198774 0.845834 -0.035539 10.50000 -1.20000 H36D 2 1.178042 0.954426 -0.015916 10.50000 -1.20000 PART 0 AFIX 0 C37 1 0.956695 0.447301 0.089669 11.00000 0.02376 0.01735 = 0.01822 -0.00603 -0.00374 -0.00175 C38 1 1.094029 0.474015 0.050535 11.00000 0.02235 0.02712 = 0.02197 -0.00744 -0.00744 -0.00116 AFIX 43 H38 2 1.158191 0.456102 0.084930 11.00000 -1.20000 AFIX 0 C39 1 1.136331 0.526974 -0.039049 11.00000 0.02046 0.02461 = 0.02307 -0.00768 -0.00306 -0.00409 AFIX 43 H39 2 1.229805 0.545795 -0.065985 11.00000 -1.20000 AFIX 0 C40 1 0.765634 -0.030398 0.463263 11.00000 0.04628 0.03539 = 0.06607 0.00217 -0.01876 -0.00810 C41 1 0.726743 -0.136993 0.500309 11.00000 0.08842 0.03983 = 0.15017 0.01779 -0.05734 -0.02275 AFIX 137 H41A 2 0.630041 -0.141690 0.502954 11.00000 -1.50000 H41B 2 0.739248 -0.166672 0.559756 11.00000 -1.50000 H41C 2 0.784693 -0.174556 0.463220 11.00000 -1.50000 AFIX 0 C42 1 0.704726 0.510136 0.516955 11.00000 0.05126 0.03551 = 0.03036 -0.00878 -0.00742 0.01030 C43 1 0.685814 0.575408 0.570009 11.00000 0.08875 0.04724 = 0.05440 -0.02973 -0.02071 0.02455 AFIX 137 H43A 2 0.691649 0.533700 0.629469 11.00000 -1.50000 H43B 2 0.595330 0.609663 0.573110 11.00000 -1.50000 H43C 2 0.757725 0.626823 0.543182 11.00000 -1.50000 AFIX 0 HKLF 5 REM msb436_0m in P-1 REM R1 = 0.0434 for 15379 Fo > 4sig(Fo) and 0.0592 for all 19646 data REM 533 parameters refined using 102 restraints END WGHT 0.0506 1.4167 REM Highest difference peak 1.122, deepest hole -0.709, 1-sigma level 0.098 Q1 1 1.2601 0.1315 -0.0138 11.00000 0.05 1.12 Q2 1 1.0627 0.9244 0.0265 11.00000 0.05 0.96 Q3 1 1.1646 0.8138 0.0624 11.00000 0.05 0.64 Q4 1 0.4815 0.5387 0.2016 11.00000 0.05 0.54 Q5 1 0.7983 0.4266 0.3254 11.00000 0.05 0.49 ; _shelx_res_checksum 32102 _shelx_hkl_file ; 1 0 0 526.319 16.8087 2 1 0 0 4360.61 131.149 1 2 0 0 466.309 7.60420 1 2 0 0 50.8444 0.90036 2 3 0 0 396.487 5.12836 1 3 0 0 43.3939 0.95908 2 4 0 0 -0.7695 0.35246 2 4 0 0 1.19285 0.43957 1 5 0 0 1800.81 21.1123 1 5 0 0 211.796 3.93668 2 6 0 5 236.052 3.97174 -2 6 0 0 236.052 3.97174 1 7 0 0 13.9961 2.05027 2 7 0 6 80.4211 4.53803 -2 7 0 0 80.4211 4.53803 1 7 0 0 63.5975 3.96594 1 8 0 0 6.01973 1.81935 2 8 0 0 45.9034 3.12986 1 8 0 7 100.030 7.75580 -2 8 0 0 100.030 7.75580 1 9 0 0 10.0721 1.86765 1 9 0 0 -0.9739 1.33395 2 10 0 0 16.4875 3.43538 1 10 0 0 1.88489 2.78565 2 11 0 9 80.0403 6.39393 -2 11 0 0 80.0403 6.39393 1 12 0 10 -0.7996 3.07046 -2 12 0 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4.15784 1 2 11 20 2.30749 4.23449 2 -3 -11 9 35.8640 3.92611 -2 3 11 20 35.8640 3.92611 1 -4 -11 8 2.68623 2.18524 -2 4 11 20 2.68623 2.18524 1 -5 -11 7 1.21761 2.40707 -2 5 11 20 1.21761 2.40707 1 6 11 20 1.39734 1.93549 2 6 11 20 1.39252 2.53924 1 -6 -11 6 -3.9601 4.63666 -2 6 11 20 -3.9601 4.63666 1 7 11 20 1.48046 1.65698 2 7 11 20 8.64678 3.23782 1 8 11 20 1.89365 1.56121 2 8 11 20 8.34983 2.85200 1 -1 12 20 3.29413 2.76447 2 0 12 20 2.11062 1.43105 2 0 12 20 5.30473 1.71168 1 1 12 20 2.62735 3.45800 2 -1 -12 10 50.3168 7.86587 -2 1 12 20 50.3168 7.86587 1 1 12 20 36.9902 4.31825 1 -2 -12 9 -2.3297 2.26444 -2 2 12 20 -2.3297 2.26444 1 -3 -12 8 14.5104 2.71180 -2 3 12 20 14.5104 2.71180 1 -4 -12 7 10.8423 2.84298 -2 4 12 20 10.8423 2.84298 1 5 12 20 0.72195 1.89134 1 5 12 20 2.35960 1.57675 2 6 12 20 5.51281 2.16289 1 6 12 20 3.61948 1.63861 2 7 12 20 -1.5200 1.85678 1 7 12 20 0.10541 3.22169 2 0 13 20 147.151 10.9735 1 -1 -13 9 16.0933 3.17507 -2 1 13 20 16.0933 3.17507 1 -2 -13 8 6.74698 2.24885 -2 2 13 20 6.74698 2.24885 1 -3 -13 7 6.74412 2.87429 -2 3 13 20 6.74412 2.87429 1 4 13 20 11.8501 2.49605 1 4 13 20 0.42312 1.20463 2 5 13 20 0.21395 1.64687 1 5 13 20 0.81549 1.42951 2 6 13 20 5.20819 2.40053 1 -2 -14 7 10.3446 4.09633 -2 2 14 20 10.3446 4.09633 1 3 14 20 1.43097 1.61987 1 4 14 20 18.7096 3.05972 1 -5 -14 5 34.0316 6.32309 -2 5 14 20 34.0316 6.32309 1 -2 1 20 18.6334 2.26235 -2 2 -1 21 18.6334 2.26235 1 -3 1 19 19.7111 2.14354 -2 3 -1 21 19.7111 2.14354 1 3 -1 21 0.77570 3.43318 2 4 -1 21 158.809 8.42675 1 4 -1 21 16.2614 3.57185 2 5 -1 21 13.8415 2.82438 2 -1 0 20 11.4197 2.31454 -2 1 0 21 11.4197 2.31454 1 -2 0 19 64.5792 7.92399 -2 2 0 21 64.5792 7.92399 1 2 0 21 6.64533 1.52526 2 2 0 21 63.1439 4.03930 1 3 0 21 75.9014 3.95706 1 3 0 21 8.08722 1.43156 2 4 0 21 0.65843 1.37311 2 -4 0 18 30.9281 7.26663 -2 4 0 21 30.9281 7.26663 1 4 0 21 28.9994 4.84256 1 -5 0 17 -6.3609 4.30480 -2 5 0 21 -6.3609 4.30480 1 -6 0 16 1.64054 4.42516 -2 6 0 21 1.64054 4.42516 1 0 -1 20 16.8833 2.66395 -2 0 1 21 16.8833 2.66395 1 1 1 21 2.03078 1.48675 2 1 1 21 2.12158 1.45840 1 2 1 21 2.61385 1.12685 1 2 1 21 2.08231 1.35637 2 -3 -1 18 4.00048 2.62135 -2 3 1 21 4.00048 2.62135 1 3 1 21 12.0188 4.81632 1 -4 -1 17 7.78304 1.95524 -2 4 1 21 7.78304 1.95524 1 -5 -1 16 14.7866 2.22590 -2 5 1 21 14.7866 2.22590 1 -6 -1 15 16.0417 3.61451 -2 6 1 21 16.0417 3.61451 1 7 1 21 1.32999 1.26090 2 7 1 21 9.36105 4.66848 1 0 2 21 4.53911 1.33806 2 0 2 21 23.3103 4.03306 1 1 2 21 10.2756 2.11207 2 1 2 21 26.4212 2.96485 1 -2 -2 18 0.56946 2.47308 -2 2 2 21 0.56946 2.47308 1 -3 -2 17 23.7356 2.67153 -2 3 2 21 23.7356 2.67153 1 -4 -2 16 7.77655 2.60008 -2 4 2 21 7.77655 2.60008 1 -5 -2 15 9.51921 3.26327 -2 5 2 21 9.51921 3.26327 1 5 2 21 -1.3290 4.18056 2 6 2 21 5.35037 1.98228 2 6 2 21 -0.7473 1.70049 1 7 2 21 -0.0160 1.48798 1 7 2 21 3.47603 3.00347 2 8 2 21 -2.2241 2.27604 1 -1 3 21 64.1177 7.71757 1 0 -3 19 97.4970 10.0271 -2 0 3 21 97.4970 10.0271 1 0 3 21 86.9733 5.63934 1 0 3 21 9.95836 1.96397 2 -1 -3 18 4.30749 2.15262 -2 1 3 21 4.30749 2.15262 1 -2 -3 17 129.505 5.83743 -2 2 3 21 129.505 5.83743 1 -3 -3 16 39.8819 3.64979 -2 3 3 21 39.8819 3.64979 1 -4 -3 15 9.99827 5.99952 -2 4 3 21 9.99827 5.99952 1 4 3 21 18.1214 4.43835 1 4 3 21 2.45709 4.43729 2 5 3 21 -1.0930 2.05063 1 5 3 21 -0.4118 1.84615 2 6 3 21 0.12752 1.92247 2 6 3 21 12.5558 3.01331 1 -7 -3 13 70.3403 8.54820 -2 7 3 21 70.3403 8.54820 1 7 3 21 42.7181 5.82648 1 -8 -3 12 15.3424 2.99141 -2 8 3 21 15.3424 2.99141 1 -1 4 21 24.1313 5.81429 1 0 -4 18 4.09668 2.00606 -2 0 4 21 4.09668 2.00606 1 -1 -4 17 71.6896 4.41823 -2 1 4 21 71.6896 4.41823 1 -2 -4 16 8.24599 2.70585 -2 2 4 21 8.24599 2.70585 1 3 4 21 106.033 5.61201 1 3 4 21 10.3213 2.96374 2 4 4 21 -2.4262 1.39087 2 4 4 21 0.71128 1.72244 1 5 4 21 139.425 7.69590 1 5 4 21 11.0030 2.94548 2 -6 -4 13 134.145 7.58088 -2 6 4 21 134.145 7.58088 1 -7 -4 12 -4.6111 2.56931 -2 7 4 21 -4.6111 2.56931 1 -8 -4 11 67.3046 5.71712 -2 8 4 21 67.3046 5.71712 1 9 4 21 48.0928 6.07490 1 1 -5 18 2.56929 3.34996 -2 -1 5 21 2.56929 3.34996 1 0 -5 17 3.60512 2.24528 -2 0 5 21 3.60512 2.24528 1 -1 -5 16 -1.0494 2.69975 -2 1 5 21 -1.0494 2.69975 1 2 5 21 9.26344 2.09974 2 2 5 21 88.0950 5.12231 1 3 5 21 4.54360 1.83169 2 3 5 21 48.4533 4.04957 1 4 5 21 63.8546 6.74116 1 -4 -5 14 67.4336 6.12712 -2 4 5 21 67.4336 6.12712 1 -5 -5 13 102.661 5.46224 -2 5 5 21 102.661 5.46224 1 -6 -5 12 4.05142 2.78204 -2 6 5 21 4.05142 2.78204 1 -7 -5 11 213.638 10.0286 -2 7 5 21 213.638 10.0286 1 8 5 21 97.8232 6.72249 1 8 5 21 5.49907 2.13150 2 9 5 21 5.80909 3.12936 1 1 -6 17 21.6908 3.29123 -2 -1 6 21 21.6908 3.29123 1 0 -6 16 13.3635 3.18775 -2 0 6 21 13.3635 3.18775 1 1 6 21 2.44511 1.62054 2 1 6 21 4.70683 2.19839 1 2 6 21 6.81030 1.80964 2 2 6 21 30.3000 3.55177 1 -3 -6 14 0.27247 2.67517 -2 3 6 21 0.27247 2.67517 1 -4 -6 13 17.1711 2.88631 -2 4 6 21 17.1711 2.88631 1 -5 -6 12 1.87628 2.17008 -2 5 6 21 1.87628 2.17008 1 6 6 21 72.2257 7.66248 1 -6 -6 11 83.4039 6.36530 -2 6 6 21 83.4039 6.36530 1 6 6 21 8.41829 4.71430 2 7 6 21 123.013 7.25891 1 7 6 21 8.62973 2.40985 2 8 6 21 2.63485 1.84407 2 8 6 21 9.26478 4.18477 1 -1 7 21 10.5134 3.87085 1 1 -7 16 19.4143 5.80269 -2 -1 7 21 19.4143 5.80269 1 -1 7 21 4.20440 2.75421 2 0 7 21 2.78801 1.63858 2 0 7 21 24.2235 3.25699 1 1 7 21 -0.1850 2.18953 1 1 7 21 3.56850 2.11523 2 -1 -7 15 8.02160 5.98531 -2 1 7 21 8.02160 5.98531 1 -2 -7 14 21.2403 3.26400 -2 2 7 21 21.2403 3.26400 1 -3 -7 13 45.8350 3.75960 -2 3 7 21 45.8350 3.75960 1 -4 -7 12 10.5401 2.86671 -2 4 7 21 10.5401 2.86671 1 -5 -7 11 7.97373 3.76906 -2 5 7 21 7.97373 3.76906 1 5 7 21 -3.1249 2.58318 1 5 7 21 3.05457 4.07473 2 6 7 21 5.38746 2.72058 1 6 7 21 -1.0137 1.66786 2 7 7 21 0.14231 1.85511 2 7 7 21 -0.1372 2.03930 1 -8 -7 9 11.4454 4.18584 -2 8 7 21 11.4454 4.18584 1 -1 8 21 5.37316 3.05904 2 -1 8 21 16.7880 4.86633 1 0 -8 15 7.76941 3.27513 -2 0 8 21 7.76941 3.27513 1 0 8 21 -1.8500 2.96288 1 -1 -8 14 116.386 6.08369 -2 1 8 21 116.386 6.08369 1 -2 -8 13 141.928 6.53896 -2 2 8 21 141.928 6.53896 1 -3 -8 12 4.68813 3.47135 -2 3 8 21 4.68813 3.47135 1 4 8 21 21.2086 2.89404 2 4 8 21 208.058 10.5993 1 5 8 21 3.72470 1.85204 2 5 8 21 71.3985 6.09622 1 6 8 21 2.91666 2.55058 1 -7 -8 9 -2.3878 2.67399 -2 7 8 21 -2.3878 2.67399 1 -8 -8 8 18.6676 4.66021 -2 8 8 21 18.6676 4.66021 1 0 -9 14 120.285 7.63596 -2 0 9 21 120.285 7.63596 1 -1 -9 13 71.5662 6.09110 -2 1 9 21 71.5662 6.09110 1 -2 -9 12 15.0817 4.01105 -2 2 9 21 15.0817 4.01105 1 3 9 21 14.8027 2.24710 2 3 9 21 135.035 8.57989 1 4 9 21 99.7011 7.24646 1 4 9 21 10.8751 2.11445 2 -5 -9 10 15.6615 4.27870 -2 5 9 21 15.6615 4.27870 1 -6 -9 9 66.5214 5.80568 -2 6 9 21 66.5214 5.80568 1 -7 -9 8 14.7285 3.25542 -2 7 9 21 14.7285 3.25542 1 -8 -9 7 13.1676 5.61790 -2 8 9 21 13.1676 5.61790 1 -1 -10 12 25.5124 4.47298 -2 1 10 21 25.5124 4.47298 1 2 10 21 9.28793 2.20079 2 2 10 21 107.432 7.51260 1 3 10 21 3.80598 2.20562 2 3 10 21 74.1497 6.42983 1 -4 -10 10 24.6312 4.63805 -2 4 10 21 24.6312 4.63805 1 -5 -10 9 103.875 7.12421 -2 5 10 21 103.875 7.12421 1 -6 -10 8 26.3829 4.38665 -2 6 10 21 26.3829 4.38665 1 7 10 21 -0.5561 3.56179 2 -7 -10 7 2.04595 3.06984 -2 7 10 21 2.04595 3.06984 1 8 10 21 5.81399 3.63694 2 8 10 21 12.4203 3.05467 1 0 11 21 -3.1179 2.40516 2 1 11 21 2.13171 1.48632 2 1 11 21 21.1342 3.71670 1 2 11 21 -1.8939 2.66726 2 -2 -11 11 12.4768 5.09224 -2 2 11 21 12.4768 5.09224 1 2 11 21 16.8475 4.89121 1 -3 -11 10 6.34447 3.16200 -2 3 11 21 6.34447 3.16200 1 -4 -11 9 34.9160 3.28255 -2 4 11 21 34.9160 3.28255 1 -5 -11 8 2.00037 2.48346 -2 5 11 21 2.00037 2.48346 1 6 11 21 -0.9611 1.69861 2 6 11 21 9.45715 4.21278 1 -6 -11 7 16.1329 3.94852 -2 6 11 21 16.1329 3.94852 1 7 11 21 6.96647 2.91817 2 7 11 21 7.56916 2.76727 1 8 11 21 3.03107 2.74194 2 8 11 21 5.86435 3.36472 1 1 12 21 1.26446 2.99215 2 -2 -12 10 15.8360 4.16927 -2 2 12 21 15.8360 4.16927 1 -3 -12 9 -0.4407 1.62319 -2 3 12 21 -0.4407 1.62319 1 -4 -12 8 9.27628 2.74891 -2 4 12 21 9.27628 2.74891 1 5 12 21 -0.0668 1.69180 1 5 12 21 2.54866 1.64951 2 6 12 21 1.55300 2.32989 1 6 12 21 0.56611 1.44367 2 7 12 21 11.6143 4.19220 1 7 12 21 10.1829 4.12610 2 -2 -13 9 26.4321 4.98022 -2 2 13 21 26.4321 4.98022 1 -3 -13 8 3.33791 4.32248 -2 3 13 21 3.33791 4.32248 1 4 13 21 50.0818 4.65217 1 4 13 21 7.22055 1.55478 2 5 13 21 18.7018 3.34125 1 5 13 21 3.68460 1.10269 2 6 13 21 30.8184 5.35604 1 2 2 22 116.541 10.5484 1 -2 -3 18 161.180 12.2495 -2 2 3 22 161.180 12.2495 1 -3 -3 17 4.13182 4.01173 -2 3 3 22 4.13182 4.01173 1 4 3 22 3.21771 3.46501 2 4 3 22 7.56536 2.81211 1 5 3 22 8.53436 3.30839 2 -1 -4 18 91.6709 9.12470 -2 1 4 22 91.6709 9.12470 1 -2 -4 17 3.29779 2.64764 -2 2 4 22 3.29779 2.64764 1 3 4 22 51.1993 4.53850 1 -3 -4 16 57.9458 8.03432 -2 3 4 22 57.9458 8.03432 1 3 4 22 10.0278 4.38360 2 4 4 22 0.30581 1.48342 1 4 4 22 -2.2907 1.39327 2 5 4 22 44.3671 4.31008 1 5 4 22 5.30351 2.25365 2 -6 -4 14 22.1573 4.24856 -2 6 4 22 22.1573 4.24856 1 -1 -5 17 4.19376 2.64640 -2 1 5 22 4.19376 2.64640 1 2 5 22 34.4918 3.35320 1 2 5 22 4.55831 1.59686 2 3 5 22 2.60652 1.83895 1 3 5 22 -0.2086 1.25718 2 -4 -5 15 30.7767 4.36921 -2 4 5 22 30.7767 4.36921 1 4 5 22 19.0800 4.92434 1 -5 -5 14 3.72538 2.10974 -2 5 5 22 3.72538 2.10974 1 -6 -5 13 90.4548 6.19249 -2 6 5 22 90.4548 6.19249 1 -7 -5 12 140.767 8.08400 -2 7 5 22 140.767 8.08400 1 1 6 22 3.35036 1.98512 1 1 6 22 -0.5498 1.80620 2 2 6 22 -0.9519 1.17662 2 2 6 22 3.11595 1.75072 1 -3 -6 15 17.5482 3.10097 -2 3 6 22 17.5482 3.10097 1 -4 -6 14 20.6536 2.90717 -2 4 6 22 20.6536 2.90717 1 -5 -6 13 0.19120 2.17283 -2 5 6 22 0.19120 2.17283 1 -6 -6 12 19.9753 3.27001 -2 6 6 22 19.9753 3.27001 1 7 6 22 -0.2488 2.03654 1 8 6 22 114.797 9.41334 1 0 7 22 3.77007 2.69878 2 1 7 22 5.86605 3.31988 1 -2 -7 15 12.5449 3.41319 -2 2 7 22 12.5449 3.41319 1 -3 -7 14 61.6259 4.34683 -2 3 7 22 61.6259 4.34683 1 -4 -7 13 66.8185 4.77057 -2 4 7 22 66.8185 4.77057 1 -5 -7 12 15.1591 4.16849 -2 5 7 22 15.1591 4.16849 1 5 7 22 5.21182 3.58651 1 5 7 22 -0.4836 3.06677 2 6 7 22 2.57018 1.53348 1 6 7 22 -0.5986 1.37221 2 7 7 22 -0.6291 2.44208 1 0 8 22 -1.8909 1.96775 2 0 8 22 -1.5018 2.55206 1 -1 -8 15 33.7985 5.76817 -2 1 8 22 33.7985 5.76817 1 -2 -8 14 15.8104 2.47455 -2 2 8 22 15.8104 2.47455 1 -3 -8 13 58.4761 4.39092 -2 3 8 22 58.4761 4.39092 1 4 8 22 2.57613 1.94307 2 4 8 22 41.2611 5.18500 1 5 8 22 2.16830 1.68644 2 5 8 22 35.7964 4.77106 1 6 8 22 129.331 8.28916 1 -7 -8 10 80.9895 6.19201 -2 7 8 22 80.9895 6.19201 1 3 9 22 58.6266 5.38253 1 3 9 22 10.4584 2.10988 2 4 9 22 31.6147 4.40688 1 4 9 22 3.03110 1.57754 2 -5 -9 11 317.354 13.4761 -2 5 9 22 317.354 13.4761 1 -6 -9 10 136.646 8.32410 -2 6 9 22 136.646 8.32410 1 -7 -9 9 4.45181 2.63720 -2 7 9 22 4.45181 2.63720 1 3 10 22 -0.8891 1.21752 2 -5 -10 10 35.7419 4.36722 -2 5 10 22 35.7419 4.36722 1 -6 -10 9 21.6470 3.53088 -2 6 10 22 21.6470 3.53088 1 -7 -10 8 98.0653 9.54987 -2 7 10 22 98.0653 9.54987 1 -5 -11 9 50.3424 6.50522 -2 5 11 22 50.3424 6.50522 1 -6 -11 8 85.7674 5.92589 -2 6 11 22 85.7674 5.92589 1 -4 -12 9 7.80190 4.05691 -2 4 12 22 7.80190 4.05691 1 4 5 23 -3.5018 2.84010 1 -4 -6 15 5.13698 3.47074 -2 4 6 23 5.13698 3.47074 1 -5 -6 14 8.40811 3.76509 -2 5 6 23 8.40811 3.76509 1 -3 -7 15 19.6681 4.24655 -2 3 7 23 19.6681 4.24655 1 -4 -7 14 22.3715 5.09955 -2 4 7 23 22.3715 5.09955 1 5 7 23 4.03378 3.06024 1 -5 -7 13 3.54031 5.10157 -2 5 7 23 3.54031 5.10157 1 -3 -8 14 13.2822 4.35610 -2 3 8 23 13.2822 4.35610 1 4 8 23 27.7773 4.40320 1 4 8 23 2.72953 3.37799 2 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 84111 _database_code_depnum_ccdc_archive 'CCDC 955818' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_msb443_1m _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C86 H88 Br4 Cu4 N6 O8 P4' _chemical_formula_sum 'C86 H88 Br4 Cu4 N6 O8 P4' _chemical_formula_weight 2031.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2115(19) _cell_length_b 13.988(3) _cell_length_c 16.974(4) _cell_angle_alpha 68.746(3) _cell_angle_beta 73.126(2) _cell_angle_gamma 82.826(2) _cell_volume 2161.8(7) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5777 _cell_measurement_theta_min 2.349 _cell_measurement_theta_max 28.278 _exptl_crystal_description slab _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.560 _exptl_crystal_F_000 1026 _exptl_transmission_factor_min 0.251 _exptl_transmission_factor_max 0.431 _exptl_crystal_size_max 0.234 _exptl_crystal_size_mid 0.118 _exptl_crystal_size_min 0.033 _exptl_absorpt_coefficient_mu 2.950 _shelx_estimated_absorpt_T_min 0.545 _shelx_estimated_absorpt_T_max 0.909 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5300 _exptl_absorpt_correction_T_max 0.9089 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008a)' _exptl_special_details ; The diffraction data were collected in three sets of 606 frames (0.3 deg. width in omega) at phi = 0, 120 and 240 deg. A scan time of 30 sec/frame was used. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 26101 _diffrn_reflns_av_unetI/netI 0.0554 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.335 _diffrn_reflns_theta_max 28.323 _diffrn_reflns_theta_full 25.500 _diffrn_measured_fraction_theta_max 0.904 _diffrn_measured_fraction_theta_full 0.984 _diffrn_reflns_Laue_measured_fraction_max 0.904 _diffrn_reflns_Laue_measured_fraction_full 0.984 _diffrn_reflns_point_group_measured_fraction_max 0.904 _diffrn_reflns_point_group_measured_fraction_full 0.984 _reflns_number_total 9728 _reflns_number_gt 7167 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Data were apparently pre-merged, so _diffrn_reflns_number etc. will have to be added later. Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2 (Bruker AXS, 2009)' _computing_cell_refinement 'Bruker SAINT (Bruker AXS 2009a)' _computing_data_reduction 'Bruker SAINT (Bruker AXS 2009a)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Bruker SHELXTL(Bruker AXS 2008)' _computing_publication_material 'Bruker SHELXTL(Bruker AXS 2008)' _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. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. One allyl group and one acetonitrile ligand were disordered over two equally populated sites. These were refined with restraints that the two components of each disorder have approximately the same geometry. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0570P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 9728 _refine_ls_number_parameters 524 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.0711 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1137 _refine_ls_wR_factor_gt 0.1065 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.057 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.70968(4) 0.61399(3) 0.60970(3) 0.02230(11) Uani 1 1 d . . . . . Cu2 Cu 0.66158(5) 0.80102(3) 0.62860(3) 0.02292(11) Uani 1 1 d D . . . . Br1 Br 0.89485(4) 0.73328(3) 0.57077(3) 0.03269(11) Uani 1 1 d . . . . . Br2 Br 0.52399(4) 0.73962(3) 0.55392(2) 0.02642(10) Uani 1 1 d . . . . . P1 P 0.62903(9) 0.53456(7) 0.74997(5) 0.01649(18) Uani 1 1 d . . . . . P2 P 0.57268(9) 0.73499(7) 0.76934(6) 0.01755(19) Uani 1 1 d . . . . . O1 O 0.7239(2) 0.44600(18) 0.80146(15) 0.0219(5) Uani 1 1 d . . . . . O2 O 0.4848(2) 0.47492(17) 0.78470(15) 0.0189(5) Uani 1 1 d . . . . . O3 O 0.6272(2) 0.77362(18) 0.83324(15) 0.0209(5) Uani 1 1 d . . . . . O4 O 0.4083(2) 0.74756(17) 0.80720(15) 0.0206(5) Uani 1 1 d . . . . . N1 N 0.5859(3) 0.6057(2) 0.81614(17) 0.0167(6) Uani 1 1 d . . . . . N2 N 0.7617(3) 0.5386(2) 0.52653(19) 0.0275(7) Uani 1 1 d . . . . . C1 C 0.8383(3) 0.4005(3) 0.7573(2) 0.0202(7) Uani 1 1 d . . . . . C2 C 0.9600(4) 0.3949(3) 0.7807(2) 0.0237(8) Uani 1 1 d . . . . . C3 C 1.0721(4) 0.3461(3) 0.7395(2) 0.0282(9) Uani 1 1 d . . . . . H3 H 1.1560 0.3393 0.7547 0.034 Uiso 1 1 calc R U . . . C4 C 1.0633(4) 0.3074(3) 0.6765(2) 0.0299(9) Uani 1 1 d . . . . . H4 H 1.1418 0.2771 0.6475 0.036 Uiso 1 1 calc R U . . . C5 C 0.9407(4) 0.3127(3) 0.6561(2) 0.0284(9) Uani 1 1 d . . . . . H5 H 0.9349 0.2855 0.6135 0.034 Uiso 1 1 calc R U . . . C6 C 0.8260(4) 0.3577(3) 0.6976(2) 0.0258(8) Uani 1 1 d . . . . . H6 H 0.7405 0.3592 0.6854 0.031 Uiso 1 1 calc R U . . . C7 C 0.9626(4) 0.4394(3) 0.8495(3) 0.0285(8) Uani 1 1 d . . . . . H7A H 0.9405 0.5137 0.8275 0.034 Uiso 1 1 calc R U . . . H7B H 0.8888 0.4076 0.9028 0.034 Uiso 1 1 calc R U . . . C8 C 1.0933(4) 0.4262(3) 0.8752(3) 0.0377(10) Uani 1 1 d . . . . . H8 H 1.1753 0.4478 0.8300 0.045 Uiso 1 1 calc R U . . . C9 C 1.1017(6) 0.3867(4) 0.9559(4) 0.0580(14) Uani 1 1 d . . . . . H9A H 1.0214 0.3644 1.0025 0.070 Uiso 1 1 calc R U . . . H9B H 1.1880 0.3803 0.9682 0.070 Uiso 1 1 calc R U . . . C10 C 0.4713(3) 0.4025(3) 0.7481(2) 0.0197(7) Uani 1 1 d . . . . . C11 C 0.4599(4) 0.2996(3) 0.8007(2) 0.0244(8) Uani 1 1 d D . . . . C12 C 0.4467(4) 0.2302(3) 0.7617(3) 0.0292(9) Uani 1 1 d . . . . . H12 H 0.4371 0.1595 0.7961 0.035 Uiso 1 1 calc R U . . . C13 C 0.4472(4) 0.2613(3) 0.6751(3) 0.0291(9) Uani 1 1 d . . . . . H13 H 0.4405 0.2119 0.6502 0.035 Uiso 1 1 calc R U . . . C14 C 0.4575(4) 0.3642(3) 0.6238(2) 0.0259(8) Uani 1 1 d . . . . . H14 H 0.4579 0.3858 0.5638 0.031 Uiso 1 1 calc R U . . . C15 C 0.4672(4) 0.4361(3) 0.6614(2) 0.0228(8) Uani 1 1 d . . . . . H15 H 0.4709 0.5072 0.6279 0.027 Uiso 1 1 calc R U . . . C16 C 0.4574(17) 0.2706(9) 0.8964(7) 0.0375(18) Uani 0.5 1 d D . P A 1 H16A H 0.5489 0.2820 0.9001 0.045 Uiso 0.5 1 calc R U P A 1 H16B H 0.3909 0.3162 0.9222 0.045 Uiso 0.5 1 calc R U P A 1 C17 C 0.4199(10) 0.1624(7) 0.9488(7) 0.048(2) Uani 0.5 1 d D U P A 1 H17 H 0.4886 0.1097 0.9516 0.058 Uiso 0.5 1 calc R U P A 1 C18 C 0.2906(11) 0.1391(10) 0.9917(10) 0.099(4) Uani 0.5 1 d D U P A 1 H18A H 0.2218 0.1918 0.9889 0.119 Uiso 0.5 1 calc R U P A 1 H18B H 0.2666 0.0698 1.0252 0.119 Uiso 0.5 1 calc R U P A 1 C16A C 0.4734(16) 0.2587(10) 0.8946(7) 0.0375(18) Uani 0.5 1 d D . P A 2 H16C H 0.5641 0.2242 0.8948 0.045 Uiso 0.5 1 calc R U P A 2 H16D H 0.4706 0.3177 0.9143 0.045 Uiso 0.5 1 calc R U P A 2 C17A C 0.3670(10) 0.1862(7) 0.9584(6) 0.048(2) Uani 0.5 1 d D U P A 2 H17A H 0.2747 0.2105 0.9670 0.058 Uiso 0.5 1 calc R U P A 2 C18A C 0.3903(15) 0.0913(7) 1.0039(9) 0.099(4) Uani 0.5 1 d D U P A 2 H18C H 0.4813 0.0642 0.9971 0.119 Uiso 0.5 1 calc R U P A 2 H18D H 0.3162 0.0492 1.0438 0.119 Uiso 0.5 1 calc R U P A 2 C19 C 0.7133(4) 0.8597(3) 0.7957(2) 0.0242(8) Uani 1 1 d . . . . . C20 C 0.8533(4) 0.8417(3) 0.7801(2) 0.0259(8) Uani 1 1 d . . . . . C21 C 0.9360(4) 0.9273(3) 0.7464(3) 0.0354(10) Uani 1 1 d . . . . . H21 H 1.0326 0.9178 0.7351 0.043 Uiso 1 1 calc R U . . . C22 C 0.8797(4) 1.0261(3) 0.7292(3) 0.0434(11) Uani 1 1 d . . . . . H22 H 0.9375 1.0834 0.7061 0.052 Uiso 1 1 calc R U . . . C23 C 0.7394(4) 1.0407(3) 0.7455(3) 0.0412(11) Uani 1 1 d . . . . . H23 H 0.7007 1.1081 0.7340 0.049 Uiso 1 1 calc R U . . . C24 C 0.6551(4) 0.9567(3) 0.7789(3) 0.0322(9) Uani 1 1 d . . . . . H24 H 0.5585 0.9661 0.7899 0.039 Uiso 1 1 calc R U . . . C25 C 0.9129(4) 0.7338(3) 0.7988(3) 0.0284(9) Uani 1 1 d . . . . . H25A H 0.8622 0.6908 0.8582 0.034 Uiso 1 1 calc R U . . . H25B H 0.8975 0.7058 0.7565 0.034 Uiso 1 1 calc R U . . . C26 C 1.0613(4) 0.7238(3) 0.7942(3) 0.0362(10) Uani 1 1 d . . . . . H26 H 1.0909 0.7468 0.8324 0.043 Uiso 1 1 calc R U . . . C27 C 1.1528(4) 0.6864(3) 0.7422(3) 0.0381(10) Uani 1 1 d . . . . . H27A H 1.1271 0.6627 0.7031 0.046 Uiso 1 1 calc R U . . . H27B H 1.2460 0.6825 0.7430 0.046 Uiso 1 1 calc R U . . . C28 C 0.3499(3) 0.8478(3) 0.7894(2) 0.0213(7) Uani 1 1 d . . . . . C29 C 0.2852(4) 0.8789(3) 0.8608(2) 0.0260(8) Uani 1 1 d . . . . . C30 C 0.2261(4) 0.9775(3) 0.8428(3) 0.0298(9) Uani 1 1 d . . . . . H30 H 0.1795 1.0008 0.8899 0.036 Uiso 1 1 calc R U . . . C31 C 0.2339(4) 1.0418(3) 0.7578(3) 0.0320(9) Uani 1 1 d . . . . . H31 H 0.1953 1.1092 0.7470 0.038 Uiso 1 1 calc R U . . . C32 C 0.2980(4) 1.0083(3) 0.6882(3) 0.0284(8) Uani 1 1 d . . . . . H32 H 0.3025 1.0525 0.6298 0.034 Uiso 1 1 calc R U . . . C33 C 0.3556(4) 0.9104(3) 0.7036(2) 0.0245(8) Uani 1 1 d . . . . . H33 H 0.3983 0.8864 0.6563 0.029 Uiso 1 1 calc R U . . . C34 C 0.2785(4) 0.8090(3) 0.9541(3) 0.0352(10) Uani 1 1 d . . . . . H34A H 0.2771 0.7370 0.9573 0.042 Uiso 1 1 calc R U . . . H34B H 0.3631 0.8171 0.9682 0.042 Uiso 1 1 calc R U . . . C35 C 0.1594(6) 0.8273(4) 1.0218(3) 0.0615(16) Uani 1 1 d . . . . . H35 H 0.0745 0.8153 1.0149 0.074 Uiso 1 1 calc R U . . . C36 C 0.1458(7) 0.8547(4) 1.0851(3) 0.0711(19) Uani 1 1 d . . . . . H36A H 0.2242 0.8687 1.0982 0.085 Uiso 1 1 calc R U . . . H36B H 0.0570 0.8616 1.1209 0.085 Uiso 1 1 calc R U . . . C37 C 0.5402(3) 0.5539(2) 0.9106(2) 0.0172(7) Uani 1 1 d . . . . . C38 C 0.6349(3) 0.5276(3) 0.9597(2) 0.0193(7) Uani 1 1 d . . . . . H38 H 0.7276 0.5468 0.9318 0.023 Uiso 1 1 calc R U . . . C39 C 0.5959(3) 0.4737(3) 1.0492(2) 0.0186(7) Uani 1 1 d . . . . . H39 H 0.6612 0.4559 1.0825 0.022 Uiso 1 1 calc R U . . . C40 C 0.7776(4) 0.4891(3) 0.4837(2) 0.0281(8) Uani 1 1 d . . . . . C41 C 0.7981(5) 0.4248(3) 0.4303(3) 0.0380(10) Uani 1 1 d . . . . . H41A H 0.8047 0.4681 0.3693 0.057 Uiso 1 1 calc R U . . . H41B H 0.7205 0.3789 0.4519 0.057 Uiso 1 1 calc R U . . . H41C H 0.8828 0.3839 0.4338 0.057 Uiso 1 1 calc R U . . . N3 N 0.698(4) 0.9482(11) 0.569(2) 0.030(2) Uani 0.5 1 d D U P B 1 C42 C 0.733(2) 1.0308(10) 0.5404(9) 0.029(2) Uani 0.5 1 d D U P B 1 C43 C 0.7849(15) 1.1346(9) 0.5050(8) 0.045(3) Uani 0.5 1 d D U P B 1 H43A H 0.7884 1.1615 0.4425 0.068 Uiso 0.5 1 d R U P B 1 H43B H 0.8766 1.1356 0.5121 0.068 Uiso 0.5 1 d R U P B 1 H43C H 0.7221 1.1774 0.5348 0.068 Uiso 0.5 1 d R U P B 1 N3A N 0.691(4) 0.9477(11) 0.560(2) 0.030(2) Uani 0.5 1 d D U P B 2 C42A C 0.744(2) 1.0245(10) 0.5197(9) 0.029(2) Uani 0.5 1 d D U P B 2 C43A C 0.8099(16) 1.1231(9) 0.4713(8) 0.045(3) Uani 0.5 1 d D U P B 2 H43D H 0.8731 1.1287 0.5031 0.068 Uiso 0.5 1 d R U P B 2 H43E H 0.7426 1.1799 0.4678 0.068 Uiso 0.5 1 d R U P B 2 H43F H 0.8614 1.1261 0.4119 0.068 Uiso 0.5 1 d R U P B 2 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 0.0247(2) 0.0251(2) 0.0160(2) -0.00829(18) -0.00157(17) -0.00217(18) Cu2 0.0257(2) 0.0224(2) 0.0186(2) -0.00661(18) -0.00161(18) -0.00459(18) Br1 0.01968(19) 0.0398(2) 0.0396(2) -0.02077(19) 0.00218(16) -0.00631(16) Br2 0.0301(2) 0.0282(2) 0.02660(19) -0.01278(16) -0.01283(16) 0.00259(15) P1 0.0158(4) 0.0195(4) 0.0155(4) -0.0084(3) -0.0032(3) -0.0004(3) P2 0.0161(4) 0.0188(4) 0.0184(4) -0.0081(4) -0.0024(3) -0.0029(3) O1 0.0194(12) 0.0260(13) 0.0202(12) -0.0102(10) -0.0046(10) 0.0048(10) O2 0.0182(12) 0.0215(12) 0.0206(12) -0.0123(10) -0.0025(10) -0.0040(9) O3 0.0232(13) 0.0230(13) 0.0199(12) -0.0110(10) -0.0031(10) -0.0073(10) O4 0.0160(12) 0.0183(12) 0.0259(13) -0.0081(10) -0.0025(10) -0.0006(9) N1 0.0184(14) 0.0178(14) 0.0138(13) -0.0071(11) -0.0015(11) -0.0017(11) N2 0.0315(18) 0.0293(17) 0.0206(16) -0.0105(14) -0.0027(14) -0.0006(14) C1 0.0184(17) 0.0192(18) 0.0175(17) -0.0043(14) -0.0006(14) 0.0027(14) C2 0.0231(19) 0.0198(18) 0.0238(18) -0.0062(15) -0.0020(15) 0.0011(14) C3 0.0185(18) 0.027(2) 0.033(2) -0.0090(17) -0.0009(16) 0.0008(15) C4 0.026(2) 0.025(2) 0.027(2) -0.0049(16) 0.0021(16) 0.0078(16) C5 0.037(2) 0.025(2) 0.0208(18) -0.0108(15) -0.0041(16) 0.0053(17) C6 0.027(2) 0.0250(19) 0.0229(18) -0.0078(15) -0.0063(16) 0.0044(15) C7 0.025(2) 0.031(2) 0.033(2) -0.0150(17) -0.0081(17) 0.0004(16) C8 0.032(2) 0.040(2) 0.048(3) -0.022(2) -0.014(2) 0.0005(19) C9 0.059(3) 0.065(3) 0.063(3) -0.017(3) -0.037(3) -0.013(3) C10 0.0137(16) 0.0255(19) 0.0231(18) -0.0124(15) -0.0033(14) -0.0034(14) C11 0.0245(19) 0.0253(19) 0.0257(19) -0.0103(16) -0.0052(15) -0.0076(15) C12 0.028(2) 0.028(2) 0.035(2) -0.0150(17) -0.0042(17) -0.0063(16) C13 0.024(2) 0.035(2) 0.037(2) -0.0257(19) -0.0029(17) -0.0026(16) C14 0.0239(19) 0.037(2) 0.0242(19) -0.0176(17) -0.0078(15) -0.0033(16) C15 0.0212(18) 0.0258(19) 0.0268(19) -0.0133(16) -0.0095(15) 0.0012(15) C16 0.060(4) 0.026(3) 0.026(2) -0.008(2) -0.010(2) -0.009(3) C17 0.051(4) 0.036(3) 0.048(3) -0.002(3) -0.012(3) -0.004(3) C18 0.109(7) 0.078(6) 0.109(6) -0.036(5) -0.008(6) -0.039(5) C16A 0.060(4) 0.026(3) 0.026(2) -0.008(2) -0.010(2) -0.009(3) C17A 0.051(4) 0.036(3) 0.048(3) -0.002(3) -0.012(3) -0.004(3) C18A 0.109(7) 0.078(6) 0.109(6) -0.036(5) -0.008(6) -0.039(5) C19 0.0238(19) 0.0240(19) 0.0261(19) -0.0111(15) -0.0021(15) -0.0087(15) C20 0.026(2) 0.0243(19) 0.030(2) -0.0127(16) -0.0058(16) -0.0039(15) C21 0.021(2) 0.033(2) 0.054(3) -0.017(2) -0.0063(19) -0.0056(17) C22 0.033(2) 0.029(2) 0.067(3) -0.017(2) -0.005(2) -0.0150(19) C23 0.035(2) 0.022(2) 0.070(3) -0.022(2) -0.011(2) -0.0026(18) C24 0.024(2) 0.029(2) 0.048(3) -0.0190(19) -0.0079(18) -0.0022(16) C25 0.0221(19) 0.024(2) 0.039(2) -0.0086(17) -0.0081(17) -0.0044(15) C26 0.033(2) 0.035(2) 0.040(2) -0.0110(19) -0.0093(19) -0.0055(18) C27 0.032(2) 0.040(2) 0.048(3) -0.023(2) -0.006(2) -0.0078(19) C28 0.0133(16) 0.0215(18) 0.0314(19) -0.0100(15) -0.0073(15) -0.0028(13) C29 0.0211(18) 0.028(2) 0.030(2) -0.0114(16) -0.0063(16) -0.0012(15) C30 0.0235(19) 0.027(2) 0.040(2) -0.0176(18) -0.0044(17) 0.0029(16) C31 0.027(2) 0.023(2) 0.045(2) -0.0101(18) -0.0110(18) 0.0008(16) C32 0.025(2) 0.029(2) 0.030(2) -0.0029(16) -0.0128(16) -0.0060(16) C33 0.0206(18) 0.029(2) 0.0271(19) -0.0105(16) -0.0095(15) -0.0033(15) C34 0.041(2) 0.031(2) 0.027(2) -0.0122(17) 0.0002(18) 0.0041(18) C35 0.076(4) 0.051(3) 0.038(3) -0.010(2) 0.001(3) 0.016(3) C36 0.102(5) 0.044(3) 0.046(3) -0.022(3) 0.025(3) -0.011(3) C37 0.0208(17) 0.0166(17) 0.0151(16) -0.0095(13) 0.0002(13) -0.0026(13) C38 0.0167(16) 0.0212(18) 0.0206(17) -0.0104(14) 0.0001(14) -0.0048(13) C39 0.0170(17) 0.0231(18) 0.0201(17) -0.0122(14) -0.0050(14) -0.0006(13) C40 0.027(2) 0.028(2) 0.0244(19) -0.0063(17) -0.0054(16) 0.0024(16) C41 0.046(3) 0.037(2) 0.038(2) -0.023(2) -0.011(2) 0.008(2) N3 0.032(3) 0.0288(17) 0.028(4) -0.0063(17) -0.009(3) -0.0055(14) C42 0.028(3) 0.029(2) 0.031(5) -0.009(3) -0.009(4) -0.002(2) C43 0.039(5) 0.030(3) 0.059(7) 0.001(4) -0.021(5) -0.008(3) N3A 0.032(3) 0.0288(17) 0.028(4) -0.0063(17) -0.009(3) -0.0055(14) C42A 0.028(3) 0.029(2) 0.031(5) -0.009(3) -0.009(4) -0.002(2) C43A 0.039(5) 0.030(3) 0.059(7) 0.001(4) -0.021(5) -0.008(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 Cu1 N2 1.973(3) . ? Cu1 P1 2.1805(10) . ? Cu1 Br1 2.4616(7) . ? Cu1 Br2 2.5658(7) . ? Cu1 Cu2 2.7174(8) . ? Cu2 N3 1.966(9) . ? Cu2 N3A 1.971(10) . ? Cu2 P2 2.1760(10) . ? Cu2 Br1 2.5076(7) . ? Cu2 Br2 2.5382(6) . ? P1 O1 1.626(2) . ? P1 O2 1.631(2) . ? P1 N1 1.691(3) . ? P2 O3 1.622(2) . ? P2 O4 1.626(2) . ? P2 N1 1.697(3) . ? O1 C1 1.409(4) . ? O2 C10 1.405(4) . ? O3 C19 1.418(4) . ? O4 C28 1.414(4) . ? N1 C37 1.456(4) . ? N2 C40 1.140(5) . ? C1 C6 1.390(5) . ? C1 C2 1.396(5) . ? C2 C3 1.396(5) . ? C2 C7 1.517(5) . ? C3 C4 1.390(6) . ? C3 H3 0.9500 . ? C4 C5 1.378(6) . ? C4 H4 0.9500 . ? C5 C6 1.386(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.491(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.304(6) . ? C8 H8 0.9500 . ? C9 H9A 0.9500 . ? C9 H9B 0.9500 . ? C10 C15 1.384(5) . ? C10 C11 1.390(5) . ? C11 C12 1.395(5) . ? C11 C16 1.519(12) . ? C11 C16A 1.528(11) . ? C12 C13 1.373(5) . ? C12 H12 0.9500 . ? C13 C14 1.385(5) . ? C13 H13 0.9500 . ? C14 C15 1.398(5) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.483(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.325(5) . ? C17 H17 0.9500 . ? C18 H18A 0.9500 . ? C18 H18B 0.9500 . ? C16A C17A 1.475(4) . ? C16A H16C 0.9900 . ? C16A H16D 0.9900 . ? C17A C18A 1.304(5) . ? C17A H17A 0.9500 . ? C18A H18C 0.9500 . ? C18A H18D 0.9500 . ? C19 C24 1.375(5) . ? C19 C20 1.384(5) . ? C20 C21 1.396(5) . ? C20 C25 1.512(5) . ? C21 C22 1.390(6) . ? C21 H21 0.9500 . ? C22 C23 1.381(6) . ? C22 H22 0.9500 . ? C23 C24 1.390(5) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.486(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.289(6) . ? C26 H26 0.9500 . ? C27 H27A 0.9500 . ? C27 H27B 0.9500 . ? C28 C33 1.389(5) . ? C28 C29 1.393(5) . ? C29 C30 1.399(5) . ? C29 C34 1.516(5) . ? C30 C31 1.381(6) . ? C30 H30 0.9500 . ? C31 C32 1.385(6) . ? C31 H31 0.9500 . ? C32 C33 1.385(5) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.479(6) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.233(7) . ? C35 H35 0.9500 . ? C36 H36A 0.9500 . ? C36 H36B 0.9500 . ? C37 C38 1.387(5) . ? C37 C39 1.392(5) 2_667 ? C38 C39 1.388(5) . ? C38 H38 0.9500 . ? C39 C37 1.392(5) 2_667 ? C39 H39 0.9500 . ? C40 C41 1.453(5) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? N3 C42 1.138(10) . ? C42 C43 1.457(10) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? N3A C42A 1.141(11) . ? C42A C43A 1.458(10) . ? C43A H43D 0.9800 . ? C43A H43E 0.9800 . ? C43A H43F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 P1 121.21(10) . . ? N2 Cu1 Br1 107.25(9) . . ? P1 Cu1 Br1 114.75(3) . . ? N2 Cu1 Br2 102.13(10) . . ? P1 Cu1 Br2 108.22(3) . . ? Br1 Cu1 Br2 100.56(2) . . ? N2 Cu1 Cu2 146.03(9) . . ? P1 Cu1 Cu2 92.19(3) . . ? Br1 Cu1 Cu2 57.665(19) . . ? Br2 Cu1 Cu2 57.341(17) . . ? N3 Cu2 P2 122.4(11) . . ? N3A Cu2 P2 126.5(11) . . ? N3 Cu2 Br1 98.0(11) . . ? N3A Cu2 Br1 98.4(11) . . ? P2 Cu2 Br1 115.87(3) . . ? N3 Cu2 Br2 110.6(10) . . ? N3A Cu2 Br2 105.2(10) . . ? P2 Cu2 Br2 107.49(3) . . ? Br1 Cu2 Br2 100.07(2) . . ? N3 Cu2 Cu1 144.1(11) . . ? N3A Cu2 Cu1 140.6(11) . . ? P2 Cu2 Cu1 92.80(3) . . ? Br1 Cu2 Cu1 56.042(16) . . ? Br2 Cu2 Cu1 58.326(17) . . ? Cu1 Br1 Cu2 66.29(2) . . ? Cu2 Br2 Cu1 64.33(2) . . ? O1 P1 O2 100.62(13) . . ? O1 P1 N1 99.93(13) . . ? O2 P1 N1 97.08(13) . . ? O1 P1 Cu1 118.50(9) . . ? O2 P1 Cu1 118.88(9) . . ? N1 P1 Cu1 117.87(10) . . ? O3 P2 O4 100.34(13) . . ? O3 P2 N1 101.33(14) . . ? O4 P2 N1 98.02(13) . . ? O3 P2 Cu2 118.18(9) . . ? O4 P2 Cu2 118.25(10) . . ? N1 P2 Cu2 117.19(10) . . ? C1 O1 P1 122.4(2) . . ? C10 O2 P1 118.6(2) . . ? C19 O3 P2 119.0(2) . . ? C28 O4 P2 118.3(2) . . ? C37 N1 P1 119.0(2) . . ? C37 N1 P2 122.0(2) . . ? P1 N1 P2 118.24(16) . . ? C40 N2 Cu1 171.9(3) . . ? C6 C1 C2 122.4(3) . . ? C6 C1 O1 120.6(3) . . ? C2 C1 O1 116.8(3) . . ? C1 C2 C3 116.9(3) . . ? C1 C2 C7 118.9(3) . . ? C3 C2 C7 124.2(3) . . ? C4 C3 C2 121.4(4) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C5 C4 C3 120.1(3) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 120.3(4) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C1 118.8(4) . . ? C5 C6 H6 120.6 . . ? C1 C6 H6 120.6 . . ? C8 C7 C2 116.4(3) . . ? C8 C7 H7A 108.2 . . ? C2 C7 H7A 108.2 . . ? C8 C7 H7B 108.2 . . ? C2 C7 H7B 108.2 . . ? H7A C7 H7B 107.3 . . ? C9 C8 C7 123.8(4) . . ? C9 C8 H8 118.1 . . ? C7 C8 H8 118.1 . . ? C8 C9 H9A 120.0 . . ? C8 C9 H9B 120.0 . . ? H9A C9 H9B 120.0 . . ? C15 C10 C11 122.2(3) . . ? C15 C10 O2 119.0(3) . . ? C11 C10 O2 118.8(3) . . ? C10 C11 C12 116.9(3) . . ? C10 C11 C16 118.5(5) . . ? C12 C11 C16 124.5(5) . . ? C10 C11 C16A 123.7(6) . . ? C12 C11 C16A 119.2(6) . . ? C13 C12 C11 121.9(4) . . ? C13 C12 H12 119.0 . . ? C11 C12 H12 119.0 . . ? C12 C13 C14 120.4(3) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C13 C14 C15 119.1(3) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C10 C15 C14 119.3(3) . . ? C10 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C17 C16 C11 113.1(9) . . ? C17 C16 H16A 109.0 . . ? C11 C16 H16A 109.0 . . ? C17 C16 H16B 109.0 . . ? C11 C16 H16B 109.0 . . ? H16A C16 H16B 107.8 . . ? C18 C17 C16 120.1(7) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 H18A 120.0 . . ? C17 C18 H18B 120.0 . . ? H18A C18 H18B 120.0 . . ? C17A C16A C11 114.8(9) . . ? C17A C16A H16C 108.6 . . ? C11 C16A H16C 108.6 . . ? C17A C16A H16D 108.6 . . ? C11 C16A H16D 108.6 . . ? H16C C16A H16D 107.5 . . ? C18A C17A C16A 124.9(8) . . ? C18A C17A H17A 117.5 . . ? C16A C17A H17A 117.5 . . ? C17A C18A H18C 120.0 . . ? C17A C18A H18D 120.0 . . ? H18C C18A H18D 120.0 . . ? C24 C19 C20 122.8(3) . . ? C24 C19 O3 119.2(3) . . ? C20 C19 O3 117.9(3) . . ? C19 C20 C21 117.1(3) . . ? C19 C20 C25 121.0(3) . . ? C21 C20 C25 121.9(3) . . ? C22 C21 C20 121.2(4) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C23 C22 C21 119.9(4) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 119.9(4) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C19 C24 C23 119.1(4) . . ? C19 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? C26 C25 C20 115.4(3) . . ? C26 C25 H25A 108.4 . . ? C20 C25 H25A 108.4 . . ? C26 C25 H25B 108.4 . . ? C20 C25 H25B 108.4 . . ? H25A C25 H25B 107.5 . . ? C27 C26 C25 124.8(4) . . ? C27 C26 H26 117.6 . . ? C25 C26 H26 117.6 . . ? C26 C27 H27A 120.0 . . ? C26 C27 H27B 120.0 . . ? H27A C27 H27B 120.0 . . ? C33 C28 C29 122.4(3) . . ? C33 C28 O4 120.2(3) . . ? C29 C28 O4 117.4(3) . . ? C28 C29 C30 117.0(4) . . ? C28 C29 C34 121.7(3) . . ? C30 C29 C34 121.3(3) . . ? C31 C30 C29 121.3(4) . . ? C31 C30 H30 119.3 . . ? C29 C30 H30 119.3 . . ? C30 C31 C32 120.2(4) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C31 C32 C33 120.1(4) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C32 C33 C28 118.9(3) . . ? C32 C33 H33 120.6 . . ? C28 C33 H33 120.6 . . ? C35 C34 C29 115.2(4) . . ? C35 C34 H34A 108.5 . . ? C29 C34 H34A 108.5 . . ? C35 C34 H34B 108.5 . . ? C29 C34 H34B 108.5 . . ? H34A C34 H34B 107.5 . . ? C36 C35 C34 134.2(7) . . ? C36 C35 H35 112.9 . . ? C34 C35 H35 112.9 . . ? C35 C36 H36A 120.0 . . ? C35 C36 H36B 120.0 . . ? H36A C36 H36B 120.0 . . ? C38 C37 C39 120.1(3) . 2_667 ? C38 C37 N1 119.3(3) . . ? C39 C37 N1 120.5(3) 2_667 . ? C37 C38 C39 120.7(3) . . ? C37 C38 H38 119.6 . . ? C39 C38 H38 119.6 . . ? C38 C39 C37 119.2(3) . 2_667 ? C38 C39 H39 120.4 . . ? C37 C39 H39 120.4 2_667 . ? N2 C40 C41 179.2(4) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C42 N3 Cu2 170(3) . . ? N3 C42 C43 177(3) . . ? C42 C43 H43A 107.3 . . ? C42 C43 H43B 111.7 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.4 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42A N3A Cu2 162(3) . . ? N3A C42A C43A 178(2) . . ? C42A C43A H43D 107.0 . . ? C42A C43A H43E 111.1 . . ? H43D C43A H43E 109.5 . . ? C42A C43A H43F 110.3 . . ? H43D C43A H43F 109.5 . . ? H43E C43A H43F 109.5 . . ? _refine_diff_density_max 0.996 _refine_diff_density_min -0.811 _refine_diff_density_rms 0.108 _shelxl_version_number 2013-3 _shelx_res_file ; TITL msb443_1m in P-1 CELL 0.71073 10.2115 13.9878 16.9741 68.746 73.126 82.826 ZERR 1.00 0.0019 0.0026 0.0036 0.003 0.002 0.002 LATT 1 SFAC C H N O P Br Cu UNIT 86 88 6 8 4 4 4 L.S. 12 OMIT -1 -10 12 ACTA 51 BOND $H FMAP 2 PLAN 5 EADP N3 N3a EADP C16 C16a EADP C17 C17a EADP C18 C18a DFIX 1.477 0.004 C16 C17 C16a C17a DFIX 1.320 0.005 C17 C18 C17a C18a DFIX 2.436 0.008 C16 C18 C16a C18a SADI C11 C17 C11 C17a SADI C11 C16 C11 C16a EADP C42 C42a EADP C43 C43a SADI N3 C42 N3a C42a SADI C42 C43 C42a C43a SADI N3 C43 N3a C43a SADI Cu2 N3 Cu2 N3a SIZE 0.033 0.118 0.234 ISOR 0.006 N3 N3A C17 C18 C17A C18A C42 C42A C43 C43A TEMP -173 WGHT 0.057000 FVAR 0.11850 MOLE 1 CU1 7 0.709678 0.613991 0.609696 11.00000 0.02473 0.02512 = 0.01599 -0.00829 -0.00157 -0.00217 CU2 7 0.661583 0.801018 0.628595 11.00000 0.02566 0.02244 = 0.01855 -0.00661 -0.00161 -0.00459 BR1 6 0.894847 0.733285 0.570768 11.00000 0.01968 0.03982 = 0.03956 -0.02077 0.00218 -0.00631 BR2 6 0.523992 0.739624 0.553921 11.00000 0.03006 0.02820 = 0.02660 -0.01278 -0.01283 0.00259 P1 5 0.629026 0.534557 0.749974 11.00000 0.01582 0.01955 = 0.01550 -0.00842 -0.00317 -0.00037 P2 5 0.572682 0.734994 0.769336 11.00000 0.01610 0.01881 = 0.01842 -0.00810 -0.00236 -0.00291 O1 4 0.723900 0.446002 0.801463 11.00000 0.01942 0.02597 = 0.02022 -0.01020 -0.00462 0.00475 O2 4 0.484795 0.474922 0.784697 11.00000 0.01816 0.02148 = 0.02058 -0.01226 -0.00253 -0.00402 O3 4 0.627239 0.773619 0.833245 11.00000 0.02320 0.02299 = 0.01994 -0.01100 -0.00313 -0.00731 O4 4 0.408328 0.747561 0.807203 11.00000 0.01603 0.01829 = 0.02591 -0.00805 -0.00255 -0.00057 N1 3 0.585928 0.605717 0.816144 11.00000 0.01844 0.01783 = 0.01376 -0.00713 -0.00152 -0.00172 N2 3 0.761672 0.538576 0.526527 11.00000 0.03149 0.02933 = 0.02055 -0.01055 -0.00268 -0.00062 C1 1 0.838329 0.400499 0.757264 11.00000 0.01843 0.01916 = 0.01752 -0.00433 -0.00059 0.00272 C2 1 0.960043 0.394877 0.780688 11.00000 0.02313 0.01975 = 0.02383 -0.00624 -0.00200 0.00111 C3 1 1.072053 0.346142 0.739451 11.00000 0.01853 0.02736 = 0.03303 -0.00900 -0.00089 0.00079 AFIX 43 H3 2 1.156026 0.339344 0.754732 11.00000 -1.20000 AFIX 0 C4 1 1.063258 0.307357 0.676495 11.00000 0.02595 0.02499 = 0.02692 -0.00495 0.00212 0.00784 AFIX 43 H4 2 1.141833 0.277115 0.647457 11.00000 -1.20000 AFIX 0 C5 1 0.940719 0.312713 0.656141 11.00000 0.03740 0.02538 = 0.02075 -0.01085 -0.00415 0.00530 AFIX 43 H5 2 0.934859 0.285476 0.613530 11.00000 -1.20000 AFIX 0 C6 1 0.826000 0.357678 0.697590 11.00000 0.02745 0.02503 = 0.02287 -0.00775 -0.00628 0.00440 AFIX 43 H6 2 0.740467 0.359212 0.685442 11.00000 -1.20000 AFIX 0 C7 1 0.962555 0.439383 0.849491 11.00000 0.02476 0.03117 = 0.03310 -0.01505 -0.00807 0.00041 AFIX 23 H7A 2 0.940497 0.513718 0.827513 11.00000 -1.20000 H7B 2 0.888828 0.407589 0.902819 11.00000 -1.20000 AFIX 0 C8 1 1.093302 0.426173 0.875158 11.00000 0.03220 0.04024 = 0.04818 -0.02204 -0.01365 0.00048 AFIX 43 H8 2 1.175290 0.447774 0.829999 11.00000 -1.20000 AFIX 0 C9 1 1.101667 0.386718 0.955938 11.00000 0.05869 0.06526 = 0.06288 -0.01715 -0.03667 -0.01301 AFIX 93 H9A 2 1.021420 0.364425 1.002497 11.00000 -1.20000 H9B 2 1.188009 0.380260 0.968244 11.00000 -1.20000 AFIX 0 C10 1 0.471345 0.402459 0.748082 11.00000 0.01374 0.02547 = 0.02308 -0.01236 -0.00326 -0.00340 C11 1 0.459942 0.299600 0.800675 11.00000 0.02453 0.02533 = 0.02567 -0.01030 -0.00521 -0.00760 C12 1 0.446744 0.230229 0.761705 11.00000 0.02782 0.02760 = 0.03484 -0.01504 -0.00417 -0.00627 AFIX 43 H12 2 0.437141 0.159462 0.796124 11.00000 -1.20000 AFIX 0 C13 1 0.447234 0.261279 0.675083 11.00000 0.02408 0.03504 = 0.03687 -0.02570 -0.00293 -0.00264 AFIX 43 H13 2 0.440514 0.211856 0.650153 11.00000 -1.20000 AFIX 0 C14 1 0.457467 0.364230 0.623794 11.00000 0.02387 0.03744 = 0.02418 -0.01755 -0.00784 -0.00330 AFIX 43 H14 2 0.457865 0.385756 0.563826 11.00000 -1.20000 AFIX 0 C15 1 0.467205 0.436073 0.661448 11.00000 0.02117 0.02585 = 0.02681 -0.01334 -0.00951 0.00117 AFIX 43 H15 2 0.470940 0.507234 0.627893 11.00000 -1.20000 PART 1 AFIX 0 C16 1 0.457377 0.270561 0.896444 10.50000 0.06047 0.02644 = 0.02579 -0.00765 -0.00999 -0.00900 AFIX 23 H16A 2 0.548869 0.281971 0.900088 10.50000 -1.20000 H16B 2 0.390873 0.316153 0.922167 10.50000 -1.20000 AFIX 0 C17 1 0.419870 0.162368 0.948799 10.50000 0.05073 0.03561 = 0.04759 -0.00156 -0.01233 -0.00376 AFIX 43 H17 2 0.488573 0.109675 0.951592 10.50000 -1.20000 AFIX 0 C18 1 0.290573 0.139119 0.991701 10.50000 0.10917 0.07840 = 0.10920 -0.03624 -0.00754 -0.03850 AFIX 93 H18A 2 0.221840 0.191789 0.988925 10.50000 -1.20000 H18B 2 0.266631 0.069785 1.025227 10.50000 -1.20000 PART 2 AFIX 0 C16A 1 0.473402 0.258747 0.894641 10.50000 0.06047 0.02644 = 0.02579 -0.00765 -0.00999 -0.00900 AFIX 23 H16C 2 0.564099 0.224183 0.894775 10.50000 -1.20000 H16D 2 0.470575 0.317670 0.914334 10.50000 -1.20000 AFIX 0 C17A 1 0.367046 0.186226 0.958413 10.50000 0.05073 0.03561 = 0.04759 -0.00156 -0.01233 -0.00376 AFIX 43 H17A 2 0.274680 0.210535 0.966990 10.50000 -1.20000 AFIX 0 C18A 1 0.390275 0.091296 1.003881 10.50000 0.10917 0.07840 = 0.10920 -0.03624 -0.00754 -0.03850 AFIX 93 H18C 2 0.481307 0.064202 0.997110 10.50000 -1.20000 H18D 2 0.316170 0.049217 1.043784 10.50000 -1.20000 PART 0 AFIX 0 C19 1 0.713289 0.859711 0.795695 11.00000 0.02383 0.02397 = 0.02612 -0.01109 -0.00208 -0.00875 C20 1 0.853306 0.841704 0.780146 11.00000 0.02572 0.02435 = 0.03028 -0.01273 -0.00583 -0.00391 C21 1 0.936047 0.927285 0.746447 11.00000 0.02067 0.03263 = 0.05417 -0.01745 -0.00632 -0.00562 AFIX 43 H21 2 1.032607 0.917827 0.735123 11.00000 -1.20000 AFIX 0 C22 1 0.879686 1.026058 0.729173 11.00000 0.03301 0.02918 = 0.06730 -0.01736 -0.00521 -0.01496 AFIX 43 H22 2 0.937544 1.083414 0.706149 11.00000 -1.20000 AFIX 0 C23 1 0.739422 1.040685 0.745536 11.00000 0.03513 0.02222 = 0.06984 -0.02164 -0.01097 -0.00264 AFIX 43 H23 2 0.700651 1.108113 0.734008 11.00000 -1.20000 AFIX 0 C24 1 0.655061 0.956656 0.778884 11.00000 0.02376 0.02917 = 0.04797 -0.01900 -0.00790 -0.00217 AFIX 43 H24 2 0.558523 0.966068 0.789907 11.00000 -1.20000 AFIX 0 C25 1 0.912927 0.733778 0.798831 11.00000 0.02209 0.02395 = 0.03850 -0.00861 -0.00812 -0.00445 AFIX 23 H25A 2 0.862154 0.690817 0.858162 11.00000 -1.20000 H25B 2 0.897459 0.705826 0.756467 11.00000 -1.20000 AFIX 0 C26 1 1.061304 0.723838 0.794193 11.00000 0.03279 0.03486 = 0.04047 -0.01097 -0.00935 -0.00554 AFIX 43 H26 2 1.090890 0.746781 0.832358 11.00000 -1.20000 AFIX 0 C27 1 1.152828 0.686381 0.742204 11.00000 0.03153 0.03973 = 0.04840 -0.02296 -0.00572 -0.00775 AFIX 93 H27A 2 1.127112 0.662654 0.703095 11.00000 -1.20000 H27B 2 1.246012 0.682497 0.742989 11.00000 -1.20000 AFIX 0 C28 1 0.349927 0.847771 0.789377 11.00000 0.01327 0.02152 = 0.03140 -0.00995 -0.00725 -0.00285 C29 1 0.285152 0.878866 0.860808 11.00000 0.02111 0.02767 = 0.03036 -0.01143 -0.00628 -0.00115 C30 1 0.226057 0.977544 0.842762 11.00000 0.02346 0.02707 = 0.04039 -0.01757 -0.00444 0.00293 AFIX 43 H30 2 0.179545 1.000824 0.889938 11.00000 -1.20000 AFIX 0 C31 1 0.233947 1.041811 0.757772 11.00000 0.02682 0.02305 = 0.04541 -0.01013 -0.01099 0.00077 AFIX 43 H31 2 0.195284 1.109230 0.746974 11.00000 -1.20000 AFIX 0 C32 1 0.298048 1.008308 0.688198 11.00000 0.02487 0.02876 = 0.03042 -0.00290 -0.01280 -0.00595 AFIX 43 H32 2 0.302535 1.052549 0.629843 11.00000 -1.20000 AFIX 0 C33 1 0.355621 0.910379 0.703596 11.00000 0.02062 0.02948 = 0.02705 -0.01054 -0.00952 -0.00331 AFIX 43 H33 2 0.398288 0.886435 0.656278 11.00000 -1.20000 AFIX 0 C34 1 0.278491 0.808993 0.954105 11.00000 0.04148 0.03129 = 0.02719 -0.01220 0.00015 0.00414 AFIX 23 H34A 2 0.277066 0.737038 0.957273 11.00000 -1.20000 H34B 2 0.363099 0.817059 0.968186 11.00000 -1.20000 AFIX 0 C35 1 0.159404 0.827309 1.021766 11.00000 0.07560 0.05107 = 0.03811 -0.01046 0.00096 0.01581 AFIX 43 H35 2 0.074507 0.815345 1.014878 11.00000 -1.20000 AFIX 0 C36 1 0.145837 0.854657 1.085125 11.00000 0.10240 0.04365 = 0.04574 -0.02217 0.02458 -0.01078 AFIX 93 H36A 2 0.224235 0.868737 1.098163 11.00000 -1.20000 H36B 2 0.056986 0.861646 1.120898 11.00000 -1.20000 AFIX 0 C37 1 0.540165 0.553917 0.910579 11.00000 0.02078 0.01659 = 0.01506 -0.00952 0.00020 -0.00261 C38 1 0.634937 0.527637 0.959717 11.00000 0.01671 0.02119 = 0.02056 -0.01041 0.00007 -0.00475 AFIX 43 H38 2 0.727606 0.546769 0.931835 11.00000 -1.20000 AFIX 0 C39 1 0.595860 0.473703 1.049163 11.00000 0.01702 0.02305 = 0.02007 -0.01221 -0.00497 -0.00057 AFIX 43 H39 2 0.661174 0.455856 1.082502 11.00000 -1.20000 AFIX 0 C40 1 0.777582 0.489099 0.483747 11.00000 0.02728 0.02839 = 0.02441 -0.00629 -0.00543 0.00241 C41 1 0.798056 0.424768 0.430336 11.00000 0.04650 0.03652 = 0.03782 -0.02349 -0.01127 0.00846 AFIX 137 H41A 2 0.804689 0.468118 0.369274 11.00000 -1.50000 H41B 2 0.720541 0.378913 0.451872 11.00000 -1.50000 H41C 2 0.882752 0.383868 0.433826 11.00000 -1.50000 PART 1 AFIX 0 N3 3 0.698181 0.948198 0.568732 10.50000 0.03222 0.02878 = 0.02817 -0.00633 -0.00886 -0.00552 C42 1 0.733288 1.030808 0.540450 10.50000 0.02750 0.02950 = 0.03071 -0.00913 -0.00884 -0.00165 C43 1 0.784899 1.134630 0.505048 10.50000 0.03931 0.03014 = 0.05878 0.00111 -0.02079 -0.00800 AFIX 3 H43A 2 0.788418 1.161490 0.442540 10.50000 -1.50000 H43B 2 0.876590 1.135589 0.512089 10.50000 -1.50000 H43C 2 0.722052 1.177423 0.534811 10.50000 -1.50000 PART 2 AFIX 0 N3A 3 0.691339 0.947741 0.559561 10.50000 0.03222 0.02878 = 0.02817 -0.00633 -0.00886 -0.00552 C42A 1 0.743547 1.024503 0.519653 10.50000 0.02750 0.02950 = 0.03071 -0.00913 -0.00884 -0.00165 C43A 1 0.809900 1.123139 0.471277 10.50000 0.03931 0.03014 = 0.05878 0.00111 -0.02079 -0.00800 AFIX 3 H43D 2 0.873073 1.128734 0.503130 10.50000 -1.50000 H43E 2 0.742587 1.179939 0.467849 10.50000 -1.50000 H43F 2 0.861399 1.126110 0.411938 10.50000 -1.50000 PART AFIX 0 HKLF 4 REM msb443_1m in P-1 REM R1 = 0.0454 for 7167 Fo > 4sig(Fo) and 0.0711 for all 9728 data REM 524 parameters refined using 72 restraints END WGHT 0.0570 0.0000 REM Highest difference peak 0.996, deepest hole -0.811, 1-sigma level 0.108 Q1 1 0.2402 0.8721 1.0129 11.00000 0.05 1.00 Q2 1 0.3258 0.1184 1.0129 11.00000 0.05 0.92 Q3 1 0.2715 0.1596 0.9513 11.00000 0.05 0.90 Q4 1 0.4764 0.7020 0.6028 11.00000 0.05 0.80 Q5 1 1.0590 0.7213 0.7311 11.00000 0.05 0.78 ; _shelx_res_checksum 71653 _shelx_hkl_file ; -1 0 -1 193.24 5.16 -2 0 -2 69.44 1.89 -3 0 -3 63.37 2.10 -4 0 -4 34.24 1.02 -5 0 -5 158.43 5.75 -6 0 -6 5.56 0.51 -7 0 -7 6.26 0.42 -8 0 -8 10.83 1.10 -9 0 -9 1.70 0.76 -10 0 -10 0.34 0.55 -11 0 -11 5.26 0.86 -12 0 -12 0.00 1.72 12 1 12 5.78 1.92 11 1 11 0.00 1.60 10 1 10 19.15 1.07 9 1 9 8.01 0.93 8 1 8 22.62 0.92 7 1 7 85.89 2.45 6 1 6 43.33 1.81 5 1 5 71.82 2.06 4 1 4 43.87 1.26 3 1 3 33.31 1.23 2 1 2 5.26 0.21 1 1 1 637.31 21.15 0 1 0 172.67 4.99 -1 1 -1 111.47 3.50 -2 1 -2 93.69 2.54 -3 1 -3 65.79 2.07 -4 1 -4 0.54 0.19 -5 1 -5 56.19 2.12 -6 1 -6 36.17 1.67 -7 1 -7 21.58 0.78 -8 1 -8 22.00 1.18 -9 1 -9 4.76 0.97 -10 1 -10 9.78 0.80 -11 1 -11 1.00 0.73 12 2 12 0.29 1.20 11 2 11 11.17 1.96 10 2 10 1.18 1.05 9 2 9 2.39 0.74 8 2 8 84.66 2.68 7 2 7 0.26 0.28 6 2 6 0.84 0.35 5 2 5 217.11 6.27 4 2 4 0.86 0.18 3 2 3 21.08 2.10 2 2 2 353.32 9.39 1 2 1 16.42 0.61 0 2 0 192.46 5.57 -1 2 -1 5.61 0.23 -2 2 -2 275.83 7.37 -3 2 -3 85.27 2.39 -4 2 -4 0.21 0.19 -5 2 -5 44.15 1.42 -6 2 -6 2.58 0.45 -7 2 -7 50.35 1.94 -8 2 -8 4.85 0.80 -9 2 -9 3.84 0.82 -10 2 -10 0.36 0.54 -11 2 -11 0.58 0.84 -12 2 -12 0.50 1.16 12 3 12 13.94 1.76 11 3 11 1.59 1.85 10 3 10 19.47 1.84 9 3 9 19.07 1.17 8 3 8 18.41 0.83 7 3 7 20.94 0.76 6 3 6 17.34 0.91 5 3 5 107.03 3.00 4 3 4 1.94 0.20 3 3 3 9.57 0.37 2 3 2 54.44 1.90 1 3 1 12.82 0.40 0 3 0 0.29 0.17 -1 3 -1 28.44 0.83 -2 3 -2 199.76 5.40 -3 3 -3 7.68 0.51 -4 3 -4 1.47 0.23 -5 3 -5 40.89 1.58 -6 3 -6 7.52 0.74 -7 3 -7 2.01 0.39 -8 3 -8 61.79 2.42 -9 3 -9 5.80 0.84 -10 3 -10 12.82 0.95 -11 3 -11 2.33 1.02 12 4 12 2.22 1.35 11 4 11 10.20 2.07 10 4 10 1.25 1.05 9 4 9 0.89 0.81 8 4 8 12.82 1.24 7 4 7 22.32 0.79 6 4 6 0.00 0.36 5 4 5 0.61 0.20 4 4 4 2.11 0.19 3 4 3 11.47 1.40 2 4 2 192.12 6.50 1 4 1 89.43 2.43 0 4 0 217.01 6.30 -1 4 -1 23.15 0.71 -2 4 -2 4.57 0.31 -3 4 -3 48.35 1.44 -4 4 -4 28.96 0.93 -5 4 -5 23.01 0.94 -6 4 -6 69.20 3.98 -7 4 -7 6.69 0.66 -8 4 -8 16.11 1.03 -9 4 -9 0.65 0.80 -10 4 -10 3.82 0.95 -11 4 -11 38.64 2.39 12 5 12 0.00 1.27 11 5 11 11.02 2.13 10 5 10 9.21 1.44 9 5 9 4.12 0.91 8 5 8 139.78 5.03 7 5 7 41.82 1.69 6 5 6 21.99 0.75 5 5 5 63.69 1.84 4 5 4 25.30 1.04 3 5 3 442.12 14.92 2 5 2 109.11 3.76 1 5 1 16.21 0.53 0 5 0 17.95 0.64 -1 5 -1 12.67 0.47 -2 5 -2 9.84 0.43 -3 5 -3 41.06 1.56 -4 5 -4 1.93 0.29 -5 5 -5 50.52 1.59 -6 5 -6 4.05 1.87 -7 5 -7 2.84 0.58 -8 5 -8 8.90 0.86 -9 5 -9 1.24 1.09 -10 5 -10 39.16 2.38 12 6 12 0.00 1.21 11 6 11 2.76 1.98 10 6 10 26.14 1.37 9 6 9 62.15 2.57 8 6 8 136.96 4.99 7 6 7 27.75 1.25 6 6 6 30.39 1.38 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_database_code_depnum_ccdc_archive 'CCDC 955819' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_msb435_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C86 H88 Cu4 I4 N6 O8 P4, 2(C2 H3 N)' _chemical_formula_sum 'C90 H94 Cu4 I4 N8 O8 P4' _chemical_formula_weight 2301.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.583(2) _cell_length_b 14.336(3) _cell_length_c 17.250(3) _cell_angle_alpha 100.788(2) _cell_angle_beta 104.252(2) _cell_angle_gamma 104.309(2) _cell_volume 2370.7(8) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9599 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 29.03 _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.612 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1142 _exptl_absorpt_coefficient_mu 2.311 _exptl_absorpt_correction_type 'integration numerical Gaussian' _exptl_absorpt_correction_T_min 0.5147 _exptl_absorpt_correction_T_max 0.7802 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008a)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in omega, colllected at phi = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in phi, collected at omega = -30.00 and 210.00 deg. The scan time was 15 sec/frame. ; _diffrn_ambient_temperature 100(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 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 41560 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 28.12 _reflns_number_total 11466 _reflns_number_gt 10156 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2009)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2009a)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS 2009a)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008)' _computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008)' _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. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. The allyl substituent consisting of C34 - C36 is disordered over two equally populated sites, presumably as a result of the crystallographically-imposed centrosymmetry. These were restrained to approximate the geometries of the ordered allyl substituents ; _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^)+(0.0500P)^2^+5.7981P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11466 _refine_ls_number_parameters 541 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.1031 _refine_ls_wR_factor_gt 0.0987 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.10096(2) 0.247393(15) 0.423791(12) 0.02423(6) Uani 1 1 d . . . I2 I 0.48108(2) 0.224824(18) 0.401608(15) 0.03220(7) Uani 1 1 d . . . Cu1 Cu 0.27602(4) 0.29176(3) 0.33796(2) 0.01923(9) Uani 1 1 d . . . Cu2 Cu 0.22989(4) 0.11477(3) 0.37515(2) 0.02309(9) Uani 1 1 d . . . P1 P 0.16029(8) 0.22569(5) 0.20585(4) 0.01461(14) Uani 1 1 d . . . P2 P 0.13002(8) 0.03341(5) 0.24347(4) 0.01490(14) Uani 1 1 d . . . O1 O 0.2262(2) 0.26692(15) 0.13813(13) 0.0177(4) Uani 1 1 d . . . O2 O 0.0078(2) 0.23393(15) 0.16895(13) 0.0175(4) Uani 1 1 d . . . O3 O -0.0326(2) -0.02955(15) 0.21406(13) 0.0162(4) Uani 1 1 d . . . O4 O 0.1937(2) -0.04906(16) 0.20298(13) 0.0195(4) Uani 1 1 d . . . N1 N 0.1209(3) 0.10023(18) 0.17166(15) 0.0157(5) Uani 1 1 d . . . N2 N 0.3711(3) 0.4375(2) 0.37120(18) 0.0264(6) Uani 1 1 d . . . N3 N 0.2398(3) 0.0343(2) 0.45720(18) 0.0307(7) Uani 1 1 d . . . C1 C 0.3661(3) 0.3222(2) 0.16176(18) 0.0179(6) Uani 1 1 d . . . C2 C 0.4649(3) 0.2775(2) 0.1885(2) 0.0234(6) Uani 1 1 d . . . H2 H 0.4388 0.2104 0.1917 0.028 Uiso 1 1 calc R . . C3 C 0.6024(4) 0.3319(3) 0.2104(2) 0.0287(7) Uani 1 1 d . . . H3 H 0.6710 0.3022 0.2292 0.034 Uiso 1 1 calc R . . C4 C 0.6393(4) 0.4295(3) 0.2048(3) 0.0350(8) Uani 1 1 d . . . H4 H 0.7334 0.4669 0.2197 0.042 Uiso 1 1 calc R . . C5 C 0.5380(4) 0.4729(3) 0.1773(3) 0.0326(8) Uani 1 1 d . . . H5 H 0.5642 0.5400 0.1738 0.039 Uiso 1 1 calc R . . C6 C 0.3994(3) 0.4198(2) 0.1548(2) 0.0225(6) Uani 1 1 d . . . C7 C 0.2879(3) 0.4659(2) 0.1259(2) 0.0281(7) Uani 1 1 d . . . H7A H 0.2210 0.4201 0.0736 0.034 Uiso 1 1 calc R . . H7B H 0.2389 0.4715 0.1678 0.034 Uiso 1 1 calc R . . C8 C 0.3369(4) 0.5668(3) 0.1117(3) 0.0336(8) Uani 1 1 d . . . H8 H 0.3824 0.5717 0.0708 0.040 Uiso 1 1 calc R . . C9 C 0.3219(4) 0.6483(3) 0.1510(3) 0.0406(10) Uani 1 1 d . . . H9A H 0.2770 0.6465 0.1923 0.049 Uiso 1 1 calc R . . H9B H 0.3560 0.7096 0.1384 0.049 Uiso 1 1 calc R . . C10 C -0.0074(3) 0.3287(2) 0.16763(19) 0.0180(6) Uani 1 1 d . . . C11 C 0.0266(3) 0.4010(2) 0.2418(2) 0.0226(6) Uani 1 1 d . . . H11 H 0.0561 0.3862 0.2934 0.027 Uiso 1 1 calc R . . C12 C 0.0168(3) 0.4957(2) 0.2391(2) 0.0271(7) Uani 1 1 d . . . H12 H 0.0410 0.5465 0.2891 0.032 Uiso 1 1 calc R . . C13 C -0.0288(4) 0.5154(3) 0.1629(2) 0.0294(7) Uani 1 1 d . . . H13 H -0.0340 0.5802 0.1609 0.035 Uiso 1 1 calc R . . C14 C -0.0666(3) 0.4410(3) 0.0898(2) 0.0261(7) Uani 1 1 d . . . H14 H -0.1005 0.4549 0.0383 0.031 Uiso 1 1 calc R . . C15 C -0.0558(3) 0.3457(2) 0.0904(2) 0.0200(6) Uani 1 1 d . . . C16 C -0.0902(4) 0.2667(3) 0.0112(2) 0.0251(7) Uani 1 1 d . . . H16A H -0.0179 0.2336 0.0163 0.030 Uiso 1 1 calc R . . H16B H -0.0885 0.2994 -0.0344 0.030 Uiso 1 1 calc R . . C17 C -0.2269(4) 0.1879(3) -0.0123(2) 0.0283(7) Uani 1 1 d . . . H17 H -0.2531 0.1392 -0.0637 0.034 Uiso 1 1 calc R . . C18 C -0.3139(4) 0.1794(3) 0.0305(3) 0.0342(8) Uani 1 1 d . . . H18A H -0.2928 0.2262 0.0824 0.041 Uiso 1 1 calc R . . H18B H -0.3979 0.1265 0.0098 0.041 Uiso 1 1 calc R . . C19 C -0.0777(3) -0.1019(2) 0.25431(18) 0.0175(5) Uani 1 1 d . . . C20 C -0.0758(3) -0.0723(2) 0.3362(2) 0.0223(6) Uani 1 1 d . . . H20 H -0.0476 -0.0035 0.3643 0.027 Uiso 1 1 calc R . . C21 C -0.1157(4) -0.1448(3) 0.3763(2) 0.0291(7) Uani 1 1 d . . . H21 H -0.1140 -0.1256 0.4325 0.035 Uiso 1 1 calc R . . C22 C -0.1579(4) -0.2447(3) 0.3347(2) 0.0292(7) Uani 1 1 d . . . H22 H -0.1829 -0.2942 0.3626 0.035 Uiso 1 1 calc R . . C23 C -0.1638(3) -0.2728(2) 0.2518(2) 0.0237(6) Uani 1 1 d . . . H23 H -0.1959 -0.3417 0.2231 0.028 Uiso 1 1 calc R . . C24 C -0.1235(3) -0.2018(2) 0.20986(19) 0.0188(6) Uani 1 1 d . . . C25 C -0.1340(4) -0.2317(2) 0.1198(2) 0.0255(7) Uani 1 1 d . . . H25A H -0.1165 -0.2968 0.1074 0.031 Uiso 1 1 calc R . . H25B H -0.0619 -0.1818 0.1089 0.031 Uiso 1 1 calc R . . C26 C -0.2709(4) -0.2402(3) 0.0624(2) 0.0367(9) Uani 1 1 d . . . H26 H -0.2787 -0.2507 0.0052 0.044 Uiso 1 1 calc R . . C27 C -0.3779(5) -0.2348(4) 0.0822(3) 0.0568(13) Uani 1 1 d . . . H27A H -0.3758 -0.2244 0.1386 0.068 Uiso 1 1 calc R . . H27B H -0.4596 -0.2413 0.0406 0.068 Uiso 1 1 calc R . . C28 C 0.2880(3) -0.0841(2) 0.25371(19) 0.0192(6) Uani 1 1 d . A . C29 C 0.2421(3) -0.1471(3) 0.3002(2) 0.0256(7) Uani 1 1 d . . . H29 H 0.1485 -0.1657 0.2982 0.031 Uiso 1 1 calc R . . C30 C 0.3352(4) -0.1826(3) 0.3498(2) 0.0310(8) Uani 1 1 d . . . H30 H 0.3055 -0.2254 0.3820 0.037 Uiso 1 1 calc R . . C31 C 0.4707(4) -0.1550(3) 0.3515(2) 0.0306(8) Uani 1 1 d . . . H31 H 0.5349 -0.1774 0.3862 0.037 Uiso 1 1 calc R . . C32 C 0.5132(3) -0.0947(2) 0.3026(2) 0.0263(7) Uani 1 1 d . A . H32 H 0.6059 -0.0787 0.3027 0.032 Uiso 1 1 calc R . . C33 C 0.4232(3) -0.0568(2) 0.2532(2) 0.0213(6) Uani 1 1 d . . . C34 C 0.4713(3) 0.0112(3) 0.2021(2) 0.0307(8) Uani 0.50 1 d PD A 1 H34A H 0.4604 -0.0308 0.1468 0.037 Uiso 0.50 1 calc PR A 1 H34B H 0.4101 0.0530 0.1936 0.037 Uiso 0.50 1 calc PR A 1 C35 C 0.6146(4) 0.0779(5) 0.2368(4) 0.0272(10) Uani 0.50 1 d PD A 1 H35 H 0.6313 0.1326 0.2828 0.033 Uiso 0.50 1 calc PR A 1 C36 C 0.7210(9) 0.0721(8) 0.2131(10) 0.035(2) Uani 0.50 1 d PD A 1 H36A H 0.7116 0.0193 0.1675 0.042 Uiso 0.50 1 calc PR A 1 H36B H 0.8078 0.1206 0.2414 0.042 Uiso 0.50 1 calc PR A 1 C34A C 0.4713(3) 0.0112(3) 0.2021(2) 0.0307(8) Uani 0.50 1 d PD A 2 H34C H 0.4086 -0.0157 0.1445 0.037 Uiso 0.50 1 calc PR A 2 H34D H 0.4630 0.0775 0.2241 0.037 Uiso 0.50 1 calc PR A 2 C35A C 0.6148(5) 0.0251(5) 0.1994(4) 0.0272(10) Uani 0.50 1 d PD A 2 H35A H 0.6294 -0.0310 0.1680 0.033 Uiso 0.50 1 calc PR A 2 C36A C 0.7225(8) 0.1034(6) 0.2342(10) 0.035(2) Uani 0.50 1 d PD A 2 H36C H 0.7153 0.1621 0.2665 0.042 Uiso 0.50 1 calc PR A 2 H36D H 0.8083 0.1018 0.2272 0.042 Uiso 0.50 1 calc PR A 2 C37 C 0.0583(3) 0.0493(2) 0.08377(17) 0.0156(5) Uani 1 1 d . . . C38 C 0.1419(3) 0.0359(2) 0.03427(18) 0.0170(5) Uani 1 1 d . . . H38 H 0.2387 0.0608 0.0578 0.020 Uiso 1 1 calc R . . C39 C 0.0840(3) -0.0137(2) -0.04944(18) 0.0176(5) Uani 1 1 d . . . H39 H 0.1410 -0.0233 -0.0831 0.021 Uiso 1 1 calc R . . C40 C 0.4354(4) 0.5170(3) 0.3791(2) 0.0296(7) Uani 1 1 d . . . C41 C 0.5166(6) 0.6189(3) 0.3890(3) 0.0567(13) Uani 1 1 d . . . H41A H 0.5103 0.6308 0.3343 0.085 Uiso 1 1 calc R . . H41B H 0.6125 0.6289 0.4191 0.085 Uiso 1 1 calc R . . H41C H 0.4817 0.6655 0.4203 0.085 Uiso 1 1 calc R . . C42 C 0.2387(4) -0.0259(3) 0.4920(2) 0.0287(7) Uani 1 1 d . . . C43 C 0.2351(4) -0.1049(3) 0.5346(3) 0.0353(8) Uani 1 1 d . . . H43A H 0.2107 -0.0860 0.5852 0.053 Uiso 1 1 calc R . . H43B H 0.3255 -0.1149 0.5490 0.053 Uiso 1 1 calc R . . H43C H 0.1667 -0.1670 0.4981 0.053 Uiso 1 1 calc R . . N4 N 0.8573(6) 0.3734(4) 0.5537(3) 0.0702(15) Uani 1 1 d . . . C44 C 0.8326(6) 0.4050(4) 0.5063(4) 0.0638(15) Uani 1 1 d . . . C45 C 0.8045(8) 0.4533(5) 0.4351(5) 0.105(3) Uani 1 1 d . . . H45A H 0.8188 0.5244 0.4573 0.158 Uiso 1 1 calc R . . H45B H 0.7097 0.4210 0.3994 0.158 Uiso 1 1 calc R . . H45C H 0.8671 0.4454 0.4026 0.158 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.03292(12) 0.01937(10) 0.02051(11) 0.00686(8) 0.01081(8) 0.00446(8) I2 0.02644(12) 0.03139(13) 0.03559(13) 0.00992(10) 0.00322(9) 0.00880(9) Cu1 0.02366(19) 0.01230(17) 0.01590(17) 0.00237(13) 0.00150(14) 0.00090(14) Cu2 0.0325(2) 0.01531(18) 0.01494(18) 0.00473(14) -0.00021(15) 0.00293(15) P1 0.0170(3) 0.0103(3) 0.0142(3) 0.0040(3) 0.0028(3) 0.0017(3) P2 0.0182(3) 0.0107(3) 0.0137(3) 0.0043(3) 0.0022(3) 0.0028(3) O1 0.0190(10) 0.0142(10) 0.0168(10) 0.0058(8) 0.0044(8) -0.0005(8) O2 0.0190(10) 0.0121(9) 0.0207(10) 0.0062(8) 0.0045(8) 0.0037(8) O3 0.0171(10) 0.0133(9) 0.0180(10) 0.0075(8) 0.0045(8) 0.0025(8) O4 0.0212(11) 0.0196(10) 0.0192(10) 0.0062(8) 0.0030(8) 0.0110(8) N1 0.0204(12) 0.0110(11) 0.0130(11) 0.0044(9) 0.0023(9) 0.0017(9) N2 0.0306(15) 0.0162(13) 0.0248(14) 0.0014(11) 0.0053(11) 0.0003(11) N3 0.0423(18) 0.0230(14) 0.0188(13) 0.0050(11) -0.0006(12) 0.0061(13) C1 0.0172(14) 0.0152(13) 0.0180(13) 0.0026(11) 0.0052(11) 0.0006(11) C2 0.0258(16) 0.0172(14) 0.0284(16) 0.0069(12) 0.0089(13) 0.0075(12) C3 0.0226(16) 0.0298(18) 0.0369(19) 0.0112(15) 0.0097(14) 0.0114(14) C4 0.0182(16) 0.036(2) 0.053(2) 0.0203(18) 0.0112(15) 0.0052(14) C5 0.0242(17) 0.0216(16) 0.052(2) 0.0165(16) 0.0118(16) 0.0016(13) C6 0.0186(14) 0.0175(14) 0.0317(17) 0.0097(12) 0.0078(12) 0.0034(11) C7 0.0228(16) 0.0173(15) 0.043(2) 0.0131(14) 0.0062(14) 0.0039(12) C8 0.0307(18) 0.0261(18) 0.042(2) 0.0174(16) 0.0064(16) 0.0042(14) C9 0.037(2) 0.0233(18) 0.056(3) 0.0160(17) 0.0020(18) 0.0070(15) C10 0.0168(13) 0.0139(13) 0.0247(15) 0.0072(11) 0.0074(11) 0.0044(10) C11 0.0223(15) 0.0219(15) 0.0243(15) 0.0052(12) 0.0081(12) 0.0076(12) C12 0.0248(16) 0.0193(15) 0.0354(18) 0.0002(13) 0.0101(14) 0.0082(13) C13 0.0284(17) 0.0204(16) 0.045(2) 0.0121(15) 0.0133(15) 0.0123(13) C14 0.0247(16) 0.0271(17) 0.0351(18) 0.0171(14) 0.0121(14) 0.0131(13) C15 0.0176(14) 0.0206(15) 0.0242(15) 0.0084(12) 0.0074(11) 0.0071(11) C16 0.0297(17) 0.0330(18) 0.0191(15) 0.0112(13) 0.0083(13) 0.0171(14) C17 0.0340(18) 0.0234(16) 0.0236(16) 0.0033(13) 0.0017(13) 0.0117(14) C18 0.0294(18) 0.0288(18) 0.036(2) 0.0041(15) 0.0051(15) 0.0032(15) C19 0.0180(13) 0.0167(13) 0.0196(14) 0.0094(11) 0.0053(11) 0.0056(11) C20 0.0272(16) 0.0180(14) 0.0208(15) 0.0064(12) 0.0074(12) 0.0045(12) C21 0.0336(18) 0.0326(18) 0.0201(15) 0.0112(14) 0.0093(13) 0.0046(14) C22 0.0350(18) 0.0262(17) 0.0302(18) 0.0180(14) 0.0123(14) 0.0060(14) C23 0.0244(15) 0.0164(14) 0.0299(17) 0.0088(12) 0.0092(13) 0.0030(12) C24 0.0172(14) 0.0161(14) 0.0227(14) 0.0065(11) 0.0056(11) 0.0038(11) C25 0.0330(18) 0.0179(15) 0.0233(16) 0.0033(12) 0.0113(13) 0.0028(13) C26 0.046(2) 0.0307(19) 0.0212(17) 0.0082(14) -0.0006(15) -0.0006(16) C27 0.039(2) 0.073(4) 0.051(3) 0.027(3) -0.003(2) 0.011(2) C28 0.0222(15) 0.0145(13) 0.0187(14) 0.0041(11) 0.0004(11) 0.0077(11) C29 0.0235(16) 0.0252(16) 0.0312(17) 0.0140(14) 0.0073(13) 0.0091(13) C30 0.0346(19) 0.0266(17) 0.0360(19) 0.0196(15) 0.0078(15) 0.0111(14) C31 0.0301(18) 0.0226(16) 0.0360(19) 0.0122(14) -0.0012(14) 0.0107(14) C32 0.0205(15) 0.0200(15) 0.0354(18) 0.0080(13) 0.0012(13) 0.0079(12) C33 0.0226(15) 0.0147(13) 0.0247(15) 0.0061(12) 0.0030(12) 0.0058(11) C34 0.0235(16) 0.0346(19) 0.0384(19) 0.0211(16) 0.0081(14) 0.0093(14) C35 0.032(2) 0.026(3) 0.027(3) 0.0109(19) 0.010(2) 0.011(2) C36 0.030(2) 0.030(6) 0.064(8) 0.025(5) 0.024(3) 0.020(3) C34A 0.0235(16) 0.0346(19) 0.0384(19) 0.0211(16) 0.0081(14) 0.0093(14) C35A 0.032(2) 0.026(3) 0.027(3) 0.0109(19) 0.010(2) 0.011(2) C36A 0.030(2) 0.030(6) 0.064(8) 0.025(5) 0.024(3) 0.020(3) C37 0.0212(14) 0.0077(11) 0.0141(12) 0.0033(10) 0.0016(10) 0.0014(10) C38 0.0161(13) 0.0145(13) 0.0178(13) 0.0051(11) 0.0022(10) 0.0026(10) C39 0.0207(14) 0.0142(13) 0.0173(13) 0.0041(11) 0.0051(11) 0.0049(11) C40 0.0351(19) 0.0185(16) 0.0278(17) 0.0031(13) 0.0029(14) 0.0041(14) C41 0.071(3) 0.0202(19) 0.059(3) 0.0090(19) 0.009(3) -0.009(2) C42 0.0365(19) 0.0232(16) 0.0200(15) 0.0060(13) -0.0003(13) 0.0069(14) C43 0.046(2) 0.0276(18) 0.035(2) 0.0188(16) 0.0086(17) 0.0121(16) N4 0.076(3) 0.062(3) 0.038(2) -0.004(2) -0.008(2) -0.003(3) C44 0.059(3) 0.045(3) 0.058(4) -0.010(3) 0.004(3) -0.004(2) C45 0.083(5) 0.058(4) 0.116(6) 0.017(4) -0.041(4) -0.006(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 I1 Cu1 2.6739(6) . ? I1 Cu2 2.7257(6) . ? I2 Cu2 2.6124(6) . ? I2 Cu1 2.6621(6) . ? Cu1 N2 1.983(3) . ? Cu1 P1 2.1988(9) . ? Cu1 Cu2 2.6907(7) . ? Cu2 N3 1.986(3) . ? Cu2 P2 2.2031(9) . ? P1 O2 1.625(2) . ? P1 O1 1.630(2) . ? P1 N1 1.694(3) . ? P2 O4 1.630(2) . ? P2 O3 1.632(2) . ? P2 N1 1.701(2) . ? O1 C1 1.410(3) . ? O2 C10 1.410(3) . ? O3 C19 1.405(3) . ? O4 C28 1.413(3) . ? N1 C37 1.457(4) . ? N2 C40 1.137(5) . ? N3 C42 1.139(5) . ? C1 C2 1.385(4) . ? C1 C6 1.392(4) . ? C2 C3 1.387(5) . ? C2 H2 0.9500 . ? C3 C4 1.385(5) . ? C3 H3 0.9500 . ? C4 C5 1.397(5) . ? C4 H4 0.9500 . ? C5 C6 1.393(5) . ? C5 H5 0.9500 . ? C6 C7 1.515(5) . ? C7 C8 1.499(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.303(6) . ? C8 H8 0.9500 . ? C9 H9A 0.9500 . ? C9 H9B 0.9500 . ? C10 C11 1.390(4) . ? C10 C15 1.394(4) . ? C11 C12 1.396(5) . ? C11 H11 0.9500 . ? C12 C13 1.390(5) . ? C12 H12 0.9500 . ? C13 C14 1.388(5) . ? C13 H13 0.9500 . ? C14 C15 1.401(4) . ? C14 H14 0.9500 . ? C15 C16 1.502(5) . ? C16 C17 1.504(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.312(5) . ? C17 H17 0.9500 . ? C18 H18A 0.9500 . ? C18 H18B 0.9500 . ? C19 C20 1.390(4) . ? C19 C24 1.391(4) . ? C20 C21 1.391(4) . ? C20 H20 0.9500 . ? C21 C22 1.381(5) . ? C21 H21 0.9500 . ? C22 C23 1.393(5) . ? C22 H22 0.9500 . ? C23 C24 1.398(4) . ? C23 H23 0.9500 . ? C24 C25 1.501(4) . ? C25 C26 1.501(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.277(7) . ? C26 H26 0.9500 . ? C27 H27A 0.9500 . ? C27 H27B 0.9500 . ? C28 C33 1.390(5) . ? C28 C29 1.392(4) . ? C29 C30 1.400(5) . ? C29 H29 0.9500 . ? C30 C31 1.381(5) . ? C30 H30 0.9500 . ? C31 C32 1.388(5) . ? C31 H31 0.9500 . ? C32 C33 1.400(4) . ? C32 H32 0.9500 . ? C33 C34 1.510(4) . ? C34 C35 1.482(4) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.306(5) . ? C35 H35 0.9500 . ? C36 H36A 0.9500 . ? C36 H36B 0.9500 . ? C35A C36A 1.304(5) . ? C35A H35A 0.9500 . ? C36A H36C 0.9500 . ? C36A H36D 0.9500 . ? C37 C38 1.394(4) . ? C37 C39 1.396(4) 2 ? C38 C39 1.390(4) . ? C38 H38 0.9500 . ? C39 C37 1.396(4) 2 ? C39 H39 0.9500 . ? C40 C41 1.455(5) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.458(5) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? N4 C44 1.017(8) . ? C44 C45 1.522(11) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu1 I1 Cu2 59.768(15) . . ? Cu2 I2 Cu1 61.337(18) . . ? N2 Cu1 P1 116.12(9) . . ? N2 Cu1 I2 100.68(9) . . ? P1 Cu1 I2 117.46(3) . . ? N2 Cu1 I1 110.35(9) . . ? P1 Cu1 I1 107.12(3) . . ? I2 Cu1 I1 104.450(19) . . ? N2 Cu1 Cu2 149.74(9) . . ? P1 Cu1 Cu2 93.80(2) . . ? I2 Cu1 Cu2 58.420(15) . . ? I1 Cu1 Cu2 61.072(13) . . ? N3 Cu2 P2 117.28(9) . . ? N3 Cu2 I2 106.07(10) . . ? P2 Cu2 I2 111.75(3) . . ? N3 Cu2 Cu1 151.06(9) . . ? P2 Cu2 Cu1 91.65(3) . . ? I2 Cu2 Cu1 60.242(14) . . ? N3 Cu2 I1 105.62(10) . . ? P2 Cu2 I1 110.79(3) . . ? I2 Cu2 I1 104.37(2) . . ? Cu1 Cu2 I1 59.160(16) . . ? O2 P1 O1 97.71(11) . . ? O2 P1 N1 97.73(12) . . ? O1 P1 N1 103.43(12) . . ? O2 P1 Cu1 120.49(9) . . ? O1 P1 Cu1 117.86(8) . . ? N1 P1 Cu1 116.01(9) . . ? O4 P2 O3 101.55(11) . . ? O4 P2 N1 99.98(12) . . ? O3 P2 N1 97.01(11) . . ? O4 P2 Cu2 117.87(8) . . ? O3 P2 Cu2 118.27(8) . . ? N1 P2 Cu2 118.39(9) . . ? C1 O1 P1 120.18(18) . . ? C10 O2 P1 118.92(18) . . ? C19 O3 P2 118.99(18) . . ? C28 O4 P2 120.99(19) . . ? C37 N1 P1 121.01(18) . . ? C37 N1 P2 120.20(18) . . ? P1 N1 P2 117.93(14) . . ? C40 N2 Cu1 167.7(3) . . ? C42 N3 Cu2 167.7(3) . . ? C2 C1 C6 122.4(3) . . ? C2 C1 O1 119.7(3) . . ? C6 C1 O1 117.9(3) . . ? C1 C2 C3 119.4(3) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C4 C3 C2 119.9(3) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 119.9(3) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C6 C5 C4 121.3(3) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C1 C6 C5 117.2(3) . . ? C1 C6 C7 120.6(3) . . ? C5 C6 C7 122.2(3) . . ? C8 C7 C6 115.0(3) . . ? C8 C7 H7A 108.5 . . ? C6 C7 H7A 108.5 . . ? C8 C7 H7B 108.5 . . ? C6 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? C9 C8 C7 125.1(4) . . ? C9 C8 H8 117.5 . . ? C7 C8 H8 117.5 . . ? C8 C9 H9A 120.0 . . ? C8 C9 H9B 120.0 . . ? H9A C9 H9B 120.0 . . ? C11 C10 C15 122.7(3) . . ? C11 C10 O2 119.8(3) . . ? C15 C10 O2 117.6(3) . . ? C10 C11 C12 118.9(3) . . ? C10 C11 H11 120.5 . . ? C12 C11 H11 120.5 . . ? C13 C12 C11 119.7(3) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C14 C13 C12 120.4(3) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C15 121.3(3) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C10 C15 C14 117.1(3) . . ? C10 C15 C16 121.6(3) . . ? C14 C15 C16 121.3(3) . . ? C15 C16 C17 115.1(3) . . ? C15 C16 H16A 108.5 . . ? C17 C16 H16A 108.5 . . ? C15 C16 H16B 108.5 . . ? C17 C16 H16B 108.5 . . ? H16A C16 H16B 107.5 . . ? C18 C17 C16 126.9(3) . . ? C18 C17 H17 116.5 . . ? C16 C17 H17 116.5 . . ? C17 C18 H18A 120.0 . . ? C17 C18 H18B 120.0 . . ? H18A C18 H18B 120.0 . . ? C20 C19 C24 122.2(3) . . ? C20 C19 O3 119.7(3) . . ? C24 C19 O3 118.1(3) . . ? C19 C20 C21 119.1(3) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? C22 C21 C20 120.0(3) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 120.0(3) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C22 C23 C24 121.3(3) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C19 C24 C23 117.3(3) . . ? C19 C24 C25 121.3(3) . . ? C23 C24 C25 121.4(3) . . ? C24 C25 C26 113.5(3) . . ? C24 C25 H25A 108.9 . . ? C26 C25 H25A 108.9 . . ? C24 C25 H25B 108.9 . . ? C26 C25 H25B 108.9 . . ? H25A C25 H25B 107.7 . . ? C27 C26 C25 127.0(4) . . ? C27 C26 H26 116.5 . . ? C25 C26 H26 116.5 . . ? C26 C27 H27A 120.0 . . ? C26 C27 H27B 120.0 . . ? H27A C27 H27B 120.0 . . ? C33 C28 C29 122.3(3) . . ? C33 C28 O4 118.3(3) . . ? C29 C28 O4 119.3(3) . . ? C28 C29 C30 119.3(3) . . ? C28 C29 H29 120.3 . . ? C30 C29 H29 120.3 . . ? C31 C30 C29 119.5(3) . . ? C31 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? C30 C31 C32 120.2(3) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C31 C32 C33 121.8(3) . . ? C31 C32 H32 119.1 . . ? C33 C32 H32 119.1 . . ? C28 C33 C32 116.8(3) . . ? C28 C33 C34 121.7(3) . . ? C32 C33 C34 121.5(3) . . ? C35 C34 C33 116.3(4) . . ? C35 C34 H34A 108.2 . . ? C33 C34 H34A 108.2 . . ? C35 C34 H34B 108.2 . . ? C33 C34 H34B 108.2 . . ? H34A C34 H34B 107.4 . . ? C36 C35 C34 128.9(7) . . ? C36 C35 H35 115.5 . . ? C34 C35 H35 115.5 . . ? C35 C36 H36A 120.0 . . ? C35 C36 H36B 120.0 . . ? H36A C36 H36B 120.0 . . ? C36A C35A H35A 115.5 . . ? C35A C36A H36C 120.0 . . ? C35A C36A H36D 120.0 . . ? H36C C36A H36D 120.0 . . ? C38 C37 C39 120.2(3) . 2 ? C38 C37 N1 119.4(3) . . ? C39 C37 N1 120.4(3) 2 . ? C39 C38 C37 120.2(3) . . ? C39 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C38 C39 C37 119.6(3) . 2 ? C38 C39 H39 120.2 . . ? C37 C39 H39 120.2 2 . ? N2 C40 C41 179.5(5) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N3 C42 C43 178.5(4) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N4 C44 C45 176.6(8) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.12 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.013 _refine_diff_density_min -2.149 _refine_diff_density_rms 0.121 _database_code_depnum_ccdc_archive 'CCDC 955820' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_msb427_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; \m-{1,4-bis[bis(bis(2-(3-propenyl)phenoxy)phosphino)amino]benzene} tetrakis(chlorogold(I)) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C78 H76 Au4 Cl4 N2 O8 P4' _chemical_formula_sum 'C78 H76 Au4 Cl4 N2 O8 P4' _chemical_formula_weight 2222.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.1051(8) _cell_length_b 15.3140(8) _cell_length_c 18.5847(10) _cell_angle_alpha 90.00 _cell_angle_beta 102.948(1) _cell_angle_gamma 90.00 _cell_volume 3912.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9994 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 29.14 _exptl_crystal_description Plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.887 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2132 _exptl_absorpt_coefficient_mu 7.750 _exptl_absorpt_correction_type 'integration numerical Gaussian' _exptl_absorpt_correction_T_min 0.3914 _exptl_absorpt_correction_T_max 0.5326 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008a)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in omega, colllected at phi = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in phi, collected at omega = -30.00 and 210.00 deg. The scan time was 15 sec/frame. ; _diffrn_ambient_temperature 100(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 'Bruker APEX-I CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 68946 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_sigmaI/netI 0.0252 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 28.50 _reflns_number_total 9896 _reflns_number_gt 8796 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2009)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2009a)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS 2009a)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008)' _computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008)' _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. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. ; _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^)+(0.0133P)^2^+3.0146P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9896 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0243 _refine_ls_R_factor_gt 0.0187 _refine_ls_wR_factor_ref 0.0393 _refine_ls_wR_factor_gt 0.0375 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.912570(7) 0.725961(6) 0.240663(5) 0.01283(3) Uani 1 1 d . . . Au2 Au 0.702538(7) 0.697388(6) 0.277162(5) 0.01376(3) Uani 1 1 d . . . Cl1 Cl 0.87994(5) 0.74591(5) 0.11666(3) 0.02445(15) Uani 1 1 d . . . Cl2 Cl 0.60378(5) 0.80520(5) 0.21902(4) 0.02784(16) Uani 1 1 d . . . P1 P 0.95710(5) 0.69398(4) 0.35872(3) 0.01113(12) Uani 1 1 d . . . P2 P 0.78438(5) 0.58603(4) 0.33488(3) 0.01167(12) Uani 1 1 d . . . O1 O 1.06809(12) 0.66859(11) 0.38848(9) 0.0131(3) Uani 1 1 d . . . O2 O 0.94507(13) 0.76608(11) 0.41737(9) 0.0138(4) Uani 1 1 d . . . O3 O 0.80414(12) 0.50528(11) 0.28567(9) 0.0153(4) Uani 1 1 d . . . O4 O 0.73296(12) 0.53877(11) 0.39256(9) 0.0132(3) Uani 1 1 d . . . N1 N 0.89787(15) 0.60728(13) 0.38361(10) 0.0123(4) Uani 1 1 d . . . C1 C 1.11612(17) 0.59638(16) 0.36562(13) 0.0130(5) Uani 1 1 d . . . C2 C 1.20601(18) 0.57694(16) 0.41135(13) 0.0148(5) Uani 1 1 d . . . C3 C 1.25530(19) 0.50509(17) 0.39174(15) 0.0195(5) Uani 1 1 d . . . H3 H 1.3171 0.4900 0.4215 0.023 Uiso 1 1 calc R . . C4 C 1.2165(2) 0.45483(17) 0.32978(15) 0.0209(6) Uani 1 1 d . . . H4 H 1.2513 0.4059 0.3178 0.025 Uiso 1 1 calc R . . C5 C 1.1271(2) 0.47647(17) 0.28586(14) 0.0196(6) Uani 1 1 d . . . H5 H 1.1007 0.4426 0.2432 0.024 Uiso 1 1 calc R . . C6 C 1.07557(19) 0.54763(17) 0.30374(13) 0.0169(5) Uani 1 1 d . . . H6 H 1.0137 0.5625 0.2740 0.020 Uiso 1 1 calc R . . C7 C 1.24711(18) 0.63043(17) 0.47942(14) 0.0171(5) Uani 1 1 d . . . H7A H 1.1964 0.6372 0.5082 0.021 Uiso 1 1 calc R . . H7B H 1.3022 0.5981 0.5105 0.021 Uiso 1 1 calc R . . C8 C 1.2819(2) 0.71947(18) 0.46321(16) 0.0222(6) Uani 1 1 d . . . H8 H 1.3197 0.7235 0.4270 0.027 Uiso 1 1 calc R . . C9 C 1.2641(2) 0.7921(2) 0.49515(18) 0.0327(7) Uani 1 1 d . . . H9A H 1.2266 0.7908 0.5317 0.039 Uiso 1 1 calc R . . H9B H 1.2888 0.8460 0.4818 0.039 Uiso 1 1 calc R . . C10 C 0.96431(18) 0.85592(15) 0.40700(13) 0.0134(5) Uani 1 1 d . . . C11 C 0.89376(18) 0.91431(16) 0.41798(13) 0.0148(5) Uani 1 1 d . . . C12 C 0.9144(2) 1.00263(17) 0.41184(14) 0.0187(5) Uani 1 1 d . . . H12 H 0.8683 1.0450 0.4192 0.022 Uiso 1 1 calc R . . C13 C 1.0003(2) 1.03011(18) 0.39529(14) 0.0220(6) Uani 1 1 d . . . H13 H 1.0130 1.0907 0.3920 0.026 Uiso 1 1 calc R . . C14 C 1.0679(2) 0.96958(18) 0.38347(15) 0.0221(6) Uani 1 1 d . . . H14 H 1.1263 0.9885 0.3711 0.027 Uiso 1 1 calc R . . C15 C 1.05024(19) 0.88095(18) 0.38969(14) 0.0195(5) Uani 1 1 d . . . H15 H 1.0964 0.8387 0.3822 0.023 Uiso 1 1 calc R . . C16 C 0.80000(19) 0.88163(17) 0.43501(15) 0.0200(5) Uani 1 1 d . . . H16A H 0.7638 0.8481 0.3920 0.024 Uiso 1 1 calc R . . H16B H 0.8160 0.8411 0.4775 0.024 Uiso 1 1 calc R . . C17 C 0.7353(2) 0.9521(2) 0.45250(17) 0.0284(7) Uani 1 1 d . . . H17 H 0.7561 0.9820 0.4981 0.034 Uiso 1 1 calc R . . C18 C 0.6533(2) 0.9755(2) 0.41058(19) 0.0386(8) Uani 1 1 d . . . H18A H 0.6299 0.9471 0.3646 0.046 Uiso 1 1 calc R . . H18B H 0.6165 1.0210 0.4258 0.046 Uiso 1 1 calc R . . C19 C 0.72708(18) 0.47097(17) 0.22997(13) 0.0162(5) Uani 1 1 d . . . C20 C 0.6908(2) 0.38908(18) 0.24114(15) 0.0228(6) Uani 1 1 d . . . C21 C 0.6179(2) 0.3567(2) 0.18402(17) 0.0308(7) Uani 1 1 d . . . H21 H 0.5909 0.3009 0.1895 0.037 Uiso 1 1 calc R . . C22 C 0.5834(2) 0.4031(2) 0.11971(17) 0.0323(7) Uani 1 1 d . . . H22 H 0.5337 0.3791 0.0818 0.039 Uiso 1 1 calc R . . C23 C 0.6216(2) 0.4843(2) 0.11074(15) 0.0272(7) Uani 1 1 d . . . H23 H 0.5976 0.5166 0.0668 0.033 Uiso 1 1 calc R . . C24 C 0.69503(19) 0.51876(18) 0.16598(14) 0.0194(5) Uani 1 1 d . . . H24 H 0.7227 0.5741 0.1599 0.023 Uiso 1 1 calc R . . C25 C 0.7283(2) 0.33501(19) 0.30978(16) 0.0295(7) Uani 1 1 d . . . H25A H 0.7537 0.3745 0.3519 0.035 Uiso 1 1 calc R . . H25B H 0.6739 0.3012 0.3214 0.035 Uiso 1 1 calc R . . C26 C 0.8063(3) 0.2742(3) 0.3006(2) 0.0460(10) Uani 1 1 d . . . H26 H 0.8661 0.2985 0.2947 0.055 Uiso 1 1 calc R . . C27 C 0.7985(4) 0.1890(3) 0.3002(2) 0.0768(17) Uani 1 1 d . . . H27A H 0.7398 0.1625 0.3060 0.092 Uiso 1 1 calc R . . H27B H 0.8515 0.1537 0.2941 0.092 Uiso 1 1 calc R . . C28 C 0.67124(18) 0.58690(16) 0.42832(13) 0.0134(5) Uani 1 1 d . . . C29 C 0.57465(18) 0.56089(17) 0.41650(14) 0.0163(5) Uani 1 1 d . . . C30 C 0.5162(2) 0.60670(18) 0.45476(16) 0.0235(6) Uani 1 1 d . . . H30 H 0.4498 0.5906 0.4483 0.028 Uiso 1 1 calc R . . C31 C 0.5520(2) 0.67491(19) 0.50187(16) 0.0251(6) Uani 1 1 d . . . H31 H 0.5101 0.7052 0.5269 0.030 Uiso 1 1 calc R . . C32 C 0.6488(2) 0.69906(18) 0.51250(15) 0.0223(6) Uani 1 1 d . . . H32 H 0.6737 0.7456 0.5450 0.027 Uiso 1 1 calc R . . C33 C 0.70917(19) 0.65463(17) 0.47525(14) 0.0174(5) Uani 1 1 d . . . H33 H 0.7757 0.6706 0.4819 0.021 Uiso 1 1 calc R . . C34 C 0.53387(19) 0.48881(17) 0.36296(14) 0.0191(5) Uani 1 1 d . . . H34A H 0.5850 0.4442 0.3639 0.023 Uiso 1 1 calc R . . H34B H 0.4794 0.4604 0.3795 0.023 Uiso 1 1 calc R . . C35 C 0.4980(2) 0.52046(19) 0.28477(15) 0.0259(6) Uani 1 1 d . . . H35 H 0.4831 0.4770 0.2474 0.031 Uiso 1 1 calc R . . C36 C 0.4853(2) 0.6019(2) 0.26318(17) 0.0297(7) Uani 1 1 d . . . H36A H 0.4992 0.6478 0.2984 0.036 Uiso 1 1 calc R . . H36B H 0.4623 0.6151 0.2123 0.036 Uiso 1 1 calc R . . C37 C 0.94798(17) 0.55133(16) 0.44375(13) 0.0130(5) Uani 1 1 d . . . C38 C 0.97898(17) 0.58631(16) 0.51374(13) 0.0124(5) Uani 1 1 d . . . H38 H 0.9648 0.6454 0.5229 0.015 Uiso 1 1 calc R . . C39 C 1.03088(17) 0.53486(15) 0.57052(13) 0.0123(5) Uani 1 1 d . . . H39 H 1.0518 0.5583 0.6188 0.015 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01384(5) 0.01305(5) 0.01144(4) 0.00354(3) 0.00250(3) 0.00173(4) Au2 0.01168(5) 0.01327(5) 0.01569(5) 0.00394(3) 0.00174(3) 0.00223(4) Cl1 0.0329(4) 0.0273(4) 0.0129(3) 0.0058(2) 0.0045(3) 0.0107(3) Cl2 0.0192(3) 0.0222(3) 0.0413(4) 0.0166(3) 0.0051(3) 0.0069(3) P1 0.0106(3) 0.0108(3) 0.0119(3) 0.0019(2) 0.0023(2) 0.0014(2) P2 0.0106(3) 0.0125(3) 0.0116(3) 0.0012(2) 0.0019(2) 0.0011(2) O1 0.0100(8) 0.0136(8) 0.0150(8) -0.0007(7) 0.0015(7) 0.0020(7) O2 0.0187(9) 0.0093(8) 0.0143(8) 0.0007(6) 0.0057(7) 0.0014(7) O3 0.0133(9) 0.0164(9) 0.0147(8) -0.0027(7) 0.0000(7) 0.0014(7) O4 0.0135(9) 0.0121(8) 0.0152(8) 0.0007(6) 0.0055(7) 0.0006(7) N1 0.0125(10) 0.0121(10) 0.0118(9) 0.0039(8) 0.0017(8) 0.0006(8) C1 0.0124(12) 0.0115(12) 0.0168(11) 0.0023(9) 0.0073(9) 0.0012(9) C2 0.0138(12) 0.0138(12) 0.0176(12) 0.0036(9) 0.0051(10) -0.0008(10) C3 0.0136(12) 0.0196(14) 0.0256(14) 0.0051(11) 0.0052(11) 0.0014(10) C4 0.0197(14) 0.0161(13) 0.0288(14) 0.0001(11) 0.0094(11) 0.0041(11) C5 0.0261(15) 0.0153(13) 0.0183(13) -0.0018(10) 0.0067(11) -0.0004(11) C6 0.0170(13) 0.0191(13) 0.0139(12) 0.0017(10) 0.0020(10) 0.0031(10) C7 0.0127(12) 0.0181(13) 0.0191(12) 0.0031(10) 0.0003(10) 0.0007(10) C8 0.0161(13) 0.0213(14) 0.0270(14) 0.0008(11) -0.0001(11) -0.0035(11) C9 0.0318(17) 0.0258(16) 0.0392(18) -0.0036(13) 0.0050(14) -0.0048(13) C10 0.0167(12) 0.0096(11) 0.0123(11) 0.0011(9) -0.0005(9) -0.0007(9) C11 0.0182(13) 0.0132(12) 0.0127(11) 0.0010(9) 0.0029(10) 0.0005(10) C12 0.0250(14) 0.0140(13) 0.0162(12) -0.0013(10) 0.0027(10) 0.0009(11) C13 0.0306(16) 0.0157(13) 0.0177(13) 0.0010(10) 0.0015(11) -0.0089(11) C14 0.0185(14) 0.0258(15) 0.0225(13) 0.0030(11) 0.0056(11) -0.0087(11) C15 0.0140(13) 0.0225(14) 0.0219(13) 0.0016(11) 0.0035(10) 0.0004(11) C16 0.0211(14) 0.0174(13) 0.0237(13) 0.0009(10) 0.0095(11) 0.0010(11) C17 0.0270(16) 0.0301(17) 0.0289(15) -0.0037(12) 0.0083(13) 0.0032(13) C18 0.0297(18) 0.044(2) 0.0402(19) 0.0028(16) 0.0043(15) 0.0079(15) C19 0.0136(12) 0.0215(13) 0.0133(11) -0.0047(10) 0.0026(10) 0.0009(10) C20 0.0254(15) 0.0211(14) 0.0231(14) -0.0074(11) 0.0078(11) -0.0011(12) C21 0.0271(16) 0.0282(16) 0.0386(17) -0.0155(13) 0.0103(14) -0.0073(13) C22 0.0230(16) 0.0420(19) 0.0281(16) -0.0160(14) -0.0023(13) -0.0012(14) C23 0.0241(15) 0.0387(18) 0.0170(13) -0.0044(12) 0.0010(11) 0.0099(13) C24 0.0175(13) 0.0251(15) 0.0161(12) -0.0028(10) 0.0050(10) 0.0037(11) C25 0.0421(19) 0.0186(14) 0.0296(15) -0.0020(12) 0.0121(14) -0.0017(13) C26 0.048(2) 0.056(2) 0.0386(19) 0.0115(17) 0.0192(17) 0.0244(19) C27 0.131(5) 0.060(3) 0.044(2) 0.008(2) 0.030(3) 0.065(3) C28 0.0146(12) 0.0141(12) 0.0123(11) 0.0014(9) 0.0045(9) 0.0025(10) C29 0.0147(12) 0.0154(13) 0.0195(12) -0.0001(10) 0.0052(10) -0.0029(10) C30 0.0159(13) 0.0243(15) 0.0320(15) -0.0052(12) 0.0090(12) -0.0053(11) C31 0.0240(15) 0.0265(15) 0.0271(14) -0.0072(12) 0.0109(12) 0.0010(12) C32 0.0238(15) 0.0214(14) 0.0214(13) -0.0063(11) 0.0042(11) -0.0030(11) C33 0.0138(12) 0.0194(13) 0.0187(12) -0.0021(10) 0.0031(10) -0.0015(10) C34 0.0153(13) 0.0175(13) 0.0243(13) -0.0056(10) 0.0042(11) -0.0050(10) C35 0.0248(15) 0.0275(16) 0.0231(14) -0.0072(12) 0.0005(12) -0.0077(12) C36 0.0260(16) 0.0321(17) 0.0284(15) 0.0008(13) 0.0004(12) -0.0060(13) C37 0.0118(12) 0.0130(12) 0.0137(11) 0.0041(9) 0.0020(9) 0.0002(9) C38 0.0117(12) 0.0116(12) 0.0150(11) 0.0006(9) 0.0057(9) 0.0003(9) C39 0.0133(12) 0.0129(12) 0.0101(11) 0.0002(9) 0.0015(9) -0.0022(9) _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 Au1 P1 2.1978(6) . ? Au1 Cl1 2.2674(6) . ? Au1 Au2 3.2138(2) . ? Au2 P2 2.1992(6) . ? Au2 Cl2 2.2714(6) . ? P1 O2 1.5872(17) . ? P1 O1 1.5874(17) . ? P1 N1 1.688(2) . ? P2 O4 1.5961(17) . ? P2 O3 1.5993(18) . ? P2 N1 1.685(2) . ? O1 C1 1.411(3) . ? O2 C10 1.424(3) . ? O3 C19 1.423(3) . ? O4 C28 1.415(3) . ? N1 C37 1.459(3) . ? C1 C6 1.383(3) . ? C1 C2 1.391(3) . ? C2 C3 1.393(4) . ? C2 C7 1.510(3) . ? C3 C4 1.391(4) . ? C3 H3 0.9500 . ? C4 C5 1.380(4) . ? C4 H4 0.9500 . ? C5 C6 1.391(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.502(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.311(4) . ? C8 H8 0.9500 . ? C9 H9A 0.9500 . ? C9 H9B 0.9500 . ? C10 C15 1.376(4) . ? C10 C11 1.387(3) . ? C11 C12 1.393(3) . ? C11 C16 1.512(4) . ? C12 C13 1.381(4) . ? C12 H12 0.9500 . ? C13 C14 1.381(4) . ? C13 H13 0.9500 . ? C14 C15 1.389(4) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.495(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.291(4) . ? C17 H17 0.9500 . ? C18 H18A 0.9500 . ? C18 H18B 0.9500 . ? C19 C24 1.383(3) . ? C19 C20 1.387(4) . ? C20 C21 1.394(4) . ? C20 C25 1.513(4) . ? C21 C22 1.382(4) . ? C21 H21 0.9500 . ? C22 C23 1.380(4) . ? C22 H22 0.9500 . ? C23 C24 1.389(4) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.481(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.308(6) . ? C26 H26 0.9500 . ? C27 H27A 0.9500 . ? C27 H27B 0.9500 . ? C28 C33 1.383(3) . ? C28 C29 1.389(3) . ? C29 C30 1.393(4) . ? C29 C34 1.511(3) . ? C30 C31 1.384(4) . ? C30 H30 0.9500 . ? C31 C32 1.386(4) . ? C31 H31 0.9500 . ? C32 C33 1.390(4) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.508(4) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.310(4) . ? C35 H35 0.9500 . ? C36 H36A 0.9500 . ? C36 H36B 0.9500 . ? C37 C38 1.384(3) . ? C37 C39 1.392(3) 3_766 ? C38 C39 1.387(3) . ? C38 H38 0.9500 . ? C39 C37 1.392(3) 3_766 ? C39 H39 0.9500 . ? 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 P1 Au1 Cl1 172.83(2) . . ? P1 Au1 Au2 80.196(17) . . ? Cl1 Au1 Au2 104.248(19) . . ? P2 Au2 Cl2 174.05(2) . . ? P2 Au2 Au1 78.496(17) . . ? Cl2 Au2 Au1 107.257(19) . . ? O2 P1 O1 100.37(9) . . ? O2 P1 N1 102.90(10) . . ? O1 P1 N1 102.82(10) . . ? O2 P1 Au1 118.69(7) . . ? O1 P1 Au1 116.19(7) . . ? N1 P1 Au1 113.62(7) . . ? O4 P2 O3 101.37(9) . . ? O4 P2 N1 104.28(9) . . ? O3 P2 N1 100.97(10) . . ? O4 P2 Au2 114.29(7) . . ? O3 P2 Au2 117.41(7) . . ? N1 P2 Au2 116.36(7) . . ? C1 O1 P1 126.13(15) . . ? C10 O2 P1 121.75(15) . . ? C19 O3 P2 119.93(15) . . ? C28 O4 P2 119.95(15) . . ? C37 N1 P2 122.49(16) . . ? C37 N1 P1 119.17(16) . . ? P2 N1 P1 118.27(11) . . ? C6 C1 C2 122.9(2) . . ? C6 C1 O1 122.4(2) . . ? C2 C1 O1 114.7(2) . . ? C1 C2 C3 116.7(2) . . ? C1 C2 C7 121.5(2) . . ? C3 C2 C7 121.8(2) . . ? C4 C3 C2 121.8(2) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? C5 C4 C3 119.7(2) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 120.3(2) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C1 C6 C5 118.7(2) . . ? C1 C6 H6 120.6 . . ? C5 C6 H6 120.6 . . ? C8 C7 C2 113.9(2) . . ? C8 C7 H7A 108.8 . . ? C2 C7 H7A 108.8 . . ? C8 C7 H7B 108.8 . . ? C2 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C9 C8 C7 125.1(3) . . ? C9 C8 H8 117.4 . . ? C7 C8 H8 117.4 . . ? C8 C9 H9A 120.0 . . ? C8 C9 H9B 120.0 . . ? H9A C9 H9B 120.0 . . ? C15 C10 C11 123.6(2) . . ? C15 C10 O2 120.4(2) . . ? C11 C10 O2 116.0(2) . . ? C10 C11 C12 116.3(2) . . ? C10 C11 C16 120.5(2) . . ? C12 C11 C16 123.2(2) . . ? C13 C12 C11 121.6(3) . . ? C13 C12 H12 119.2 . . ? C11 C12 H12 119.2 . . ? C14 C13 C12 120.1(3) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 120.0(3) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C10 C15 C14 118.4(3) . . ? C10 C15 H15 120.8 . . ? C14 C15 H15 120.8 . . ? C17 C16 C11 114.3(2) . . ? C17 C16 H16A 108.7 . . ? C11 C16 H16A 108.7 . . ? C17 C16 H16B 108.7 . . ? C11 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? C18 C17 C16 125.2(3) . . ? C18 C17 H17 117.4 . . ? C16 C17 H17 117.4 . . ? C17 C18 H18A 120.0 . . ? C17 C18 H18B 120.0 . . ? H18A C18 H18B 120.0 . . ? C24 C19 C20 123.1(2) . . ? C24 C19 O3 118.6(2) . . ? C20 C19 O3 118.2(2) . . ? C19 C20 C21 116.2(3) . . ? C19 C20 C25 123.3(2) . . ? C21 C20 C25 120.4(3) . . ? C22 C21 C20 122.1(3) . . ? C22 C21 H21 118.9 . . ? C20 C21 H21 118.9 . . ? C23 C22 C21 119.8(3) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 120.0(3) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C19 C24 C23 118.7(3) . . ? C19 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? C26 C25 C20 112.1(3) . . ? C26 C25 H25A 109.2 . . ? C20 C25 H25A 109.2 . . ? C26 C25 H25B 109.2 . . ? C20 C25 H25B 109.2 . . ? H25A C25 H25B 107.9 . . ? C27 C26 C25 124.3(4) . . ? C27 C26 H26 117.8 . . ? C25 C26 H26 117.8 . . ? C26 C27 H27A 120.0 . . ? C26 C27 H27B 120.0 . . ? H27A C27 H27B 120.0 . . ? C33 C28 C29 122.8(2) . . ? C33 C28 O4 119.7(2) . . ? C29 C28 O4 117.5(2) . . ? C28 C29 C30 116.5(2) . . ? C28 C29 C34 121.9(2) . . ? C30 C29 C34 121.5(2) . . ? C31 C30 C29 122.0(3) . . ? C31 C30 H30 119.0 . . ? C29 C30 H30 119.0 . . ? C30 C31 C32 120.0(3) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C31 C32 C33 119.5(2) . . ? C31 C32 H32 120.2 . . ? C33 C32 H32 120.2 . . ? C28 C33 C32 119.2(2) . . ? C28 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? C35 C34 C29 113.3(2) . . ? C35 C34 H34A 108.9 . . ? C29 C34 H34A 108.9 . . ? C35 C34 H34B 108.9 . . ? C29 C34 H34B 108.9 . . ? H34A C34 H34B 107.7 . . ? C36 C35 C34 126.5(3) . . ? C36 C35 H35 116.8 . . ? C34 C35 H35 116.8 . . ? C35 C36 H36A 120.0 . . ? C35 C36 H36B 120.0 . . ? H36A C36 H36B 120.0 . . ? C38 C37 C39 120.7(2) . 3_766 ? C38 C37 N1 119.3(2) . . ? C39 C37 N1 119.9(2) 3_766 . ? C37 C38 C39 119.8(2) . . ? C37 C38 H38 120.1 . . ? C39 C38 H38 120.1 . . ? C38 C39 C37 119.5(2) . 3_766 ? C38 C39 H39 120.2 . . ? C37 C39 H39 120.2 3_766 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.694 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.106 #===END _database_code_depnum_ccdc_archive 'CCDC 955821'