# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # 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_1_HT _audit_creation_date 2013-11-28T21:59:16-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'Compound X' _chemical_formula_moiety 'C80 H40 Fe9 N48 O34 W6' _chemical_formula_sum 'C84.5 H145.5 Fe9 N48 O36.5 W6' _chemical_formula_weight 4024.01 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.8360(5) _cell_length_b 19.5840(5) _cell_length_c 32.8010(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 113.6570(11) _cell_angle_gamma 90.000(5) _cell_volume 16967.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 170635 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.553 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7612 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.86 _exptl_absorpt_correction_type none _shelx_estimated_absorpt_T_min 0.323 _shelx_estimated_absorpt_T_max 0.475 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.0365911 _diffrn_orient_matrix_ub_12 -0.0010691 _diffrn_orient_matrix_ub_13 0.0207098 _diffrn_orient_matrix_ub_21 0.0075367 _diffrn_orient_matrix_ub_22 0.0352644 _diffrn_orient_matrix_ub_23 -0.0185389 _diffrn_orient_matrix_ub_31 -0.00614 _diffrn_orient_matrix_ub_32 0.0369151 _diffrn_orient_matrix_ub_33 0.0183097 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.1347 _diffrn_reflns_number 180401 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 30.037 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.997 _reflns_number_total 24774 _reflns_number_gt 17790 _reflns_threshold_expression 'I > 2\s(I)' #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-2012 (Sheldrick, 2012)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; DFIX 1.450 0.020 O43 C44 DFIX 1.400 0.020 O51 C52A DFIX 1.400 0.020 O51 C52B DFIX 1.400 0.020 O1 C1 DFIX 1.400 0.020 O4 C4 DFIX 1.400 0.020 O2 C2 DFIX 1.400 0.020 O6 C6 DFIX 1.400 0.020 O7 C7 DFIX 1.400 0.020 O8 C8 DFIX 1.400 0.020 O10 C10 DFIX 1.400 0.020 O1S C1S ISOR 0.01 C44 C52B C52A DELU 0.01 O75 C76 Distances C-O in some methanol molecules were restrained to prevent proper geometry.Isotropic refinement of non-hydrogen atoms of solvent molecules and ISOR restraints on C atoms of some terminal methanols were used to ensure the convergence of the refinement process. ; _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^)+(0.0738P)^2^+4.1628P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.000008(6) _refine_ls_number_reflns 24774 _refine_ls_number_parameters 818 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0768 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1343 _refine_ls_wR_factor_gt 0.1204 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.01 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.006 _refine_diff_density_min -2.65 _refine_diff_density_rms 0.227 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.849 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_disorder_assembly _atom_site_disorder_group W1 W -0.07862(2) 0.33469(2) 0.11903(2) 0.03171(6) Uani 1 d . . W2 W -0.17790(2) 0.16140(2) 0.26603(2) 0.02640(6) Uani 1 d . . W3 W -0.06044(2) -0.04740(2) 0.12595(2) 0.02951(6) Uani 1 d . . Fe1 Fe 0 0.14968(4) 0.25 0.01896(17) Uani 1 d . . Fe2 Fe -0.10647(3) 0.41650(4) 0.26526(3) 0.03343(17) Uani 1 d . . Fe3 Fe -0.12881(3) -0.10368(4) 0.25418(2) 0.03188(16) Uani 1 d . . Fe4 Fe 0.02878(3) 0.15228(4) 0.06875(2) 0.03522(17) Uani 1 d . . Fe5 Fe -0.21487(3) 0.13145(4) 0.09263(2) 0.03545(17) Uani 1 d . . C11 C -0.0465(2) 0.2590(2) 0.17075(16) 0.0311(10) Uani 1 d . . N11 N -0.02812(17) 0.2213(2) 0.19893(14) 0.0347(9) Uani 1 d . . C12 C -0.0904(2) 0.3713(3) 0.1764(2) 0.0392(12) Uani 1 d . . N12 N -0.09604(19) 0.3878(3) 0.20716(17) 0.0468(12) Uani 1 d . . C32 C -0.0136(2) -0.0769(3) 0.32601(17) 0.0352(11) Uani 1 d . . N32 N -0.05337(18) -0.0911(2) 0.30138(16) 0.0424(11) Uani 1 d . . C14 C -0.0336(2) 0.2685(3) 0.09737(17) 0.0382(12) Uani 1 d . . N14 N -0.01061(19) 0.2312(3) 0.08627(15) 0.0457(12) Uani 1 d . . C15 C -0.1368(2) 0.2599(3) 0.10922(19) 0.0426(13) Uani 1 d . . N15 N -0.16776(19) 0.2182(3) 0.10206(18) 0.0525(13) Uani 1 d . . C16 C -0.1426(5) 0.4020(6) 0.0976(3) 0.121(5) Uani 1 d . . N16 N -0.1758(5) 0.4374(7) 0.0866(3) 0.196(7) Uani 1 d . . C17 C -0.1182(2) 0.3240(3) 0.04732(19) 0.0459(14) Uani 1 d . . N17 N -0.1405(2) 0.3168(3) 0.00960(18) 0.0673(17) Uani 1 d . . C18 C -0.0533(4) 0.4159(5) 0.0904(3) 0.105(4) Uani 1 d . . N18 N -0.0384(5) 0.4602(6) 0.0763(3) 0.187(6) Uani 1 d . . C21 C -0.1076(2) 0.1571(2) 0.25707(17) 0.0313(10) Uani 1 d . . N21 N -0.07055(17) 0.1533(2) 0.25337(15) 0.0337(9) Uani 1 d . . C22 C -0.1496(2) 0.2641(3) 0.26932(18) 0.0353(11) Uani 1 d . . N22 N -0.13636(19) 0.3186(2) 0.26902(19) 0.0469(12) Uani 1 d . . C23 C -0.15719(19) 0.0547(3) 0.26552(18) 0.0335(11) Uani 1 d . . N23 N -0.14647(19) -0.0005(2) 0.26341(17) 0.0430(11) Uani 1 d . . C24 C 0.1198(2) 0.1495(3) 0.16793(18) 0.0358(12) Uani 1 d . . N24 N 0.0874(2) 0.1464(3) 0.13359(17) 0.0486(13) Uani 1 d . . C25 C -0.1982(2) 0.1439(3) 0.19630(18) 0.0338(11) Uani 1 d . . N25 N -0.20694(18) 0.1362(3) 0.15938(16) 0.0430(11) Uani 1 d . . C26 C -0.2389(2) 0.0980(3) 0.2641(2) 0.0515(16) Uani 1 d . . N26 N -0.2722(3) 0.0634(3) 0.2625(3) 0.089(3) Uani 1 d . . C27 C -0.2028(2) 0.2058(4) 0.3140(2) 0.0539(17) Uani 1 d . . N27 N -0.2159(3) 0.2300(4) 0.3394(2) 0.091(2) Uani 1 d . . C28 C -0.2439(2) 0.2234(3) 0.22917(18) 0.0381(12) Uani 1 d . . N28 N -0.2777(2) 0.2582(3) 0.21054(19) 0.0546(14) Uani 1 d . . C31 C -0.03469(19) 0.0317(3) 0.17579(17) 0.0326(11) Uani 1 d . . N31 N -0.02193(17) 0.0738(2) 0.20200(15) 0.0344(9) Uani 1 d . . C13 C 0.0056(2) 0.3696(3) 0.33558(18) 0.0357(11) Uani 1 d . . N13 N -0.03328(19) 0.3881(3) 0.31060(17) 0.0467(12) Uani 1 d . . C33 C -0.0915(2) -0.0726(3) 0.17404(18) 0.0365(11) Uani 1 d . . N33 N -0.10699(19) -0.0830(3) 0.20047(16) 0.0450(11) Uani 1 d . . C34 C -0.0311(2) 0.0333(3) 0.09763(17) 0.0379(12) Uani 1 d . . N34 N -0.01371(19) 0.0746(3) 0.08401(16) 0.0439(11) Uani 1 d . . C35 C -0.1207(2) 0.0270(3) 0.11198(18) 0.0421(13) Uani 1 d . . N35 N -0.1526(2) 0.0645(3) 0.10549(17) 0.0522(13) Uani 1 d . . C36 C -0.0703(3) -0.1557(3) 0.1275(3) 0.067(2) Uani 1 d . . N36 N -0.0744(4) -0.2142(4) 0.1291(3) 0.110(3) Uani 1 d . . C37 C -0.1200(3) -0.0681(5) 0.0625(3) 0.091(3) Uani 1 d . . N37 N -0.1512(4) -0.0801(6) 0.0297(3) 0.174(6) Uani 1 d . . C38 C -0.0236(3) -0.0944(3) 0.0870(2) 0.0486(15) Uani 1 d . . N38 N -0.0040(3) -0.1187(3) 0.0662(2) 0.0700(18) Uani 1 d . . O41 O -0.02427(18) 0.1544(3) 0.00178(14) 0.0598(13) Uani 1 d . . C42 C -0.0743(4) 0.1746(6) -0.0157(3) 0.125(5) Uani 1 d . . H42A H -0.0881 0.17 -0.0475 0.187 Uiso 1 calc . . H42B H -0.0764 0.2215 -0.008 0.187 Uiso 1 calc . . H42C H -0.0931 0.1465 -0.0037 0.187 Uiso 1 calc . . O43 O 0.0702(2) 0.2260(3) 0.05040(18) 0.0774(16) Uani 1 d . . O45 O 0.06954(19) 0.0810(3) 0.04687(17) 0.0651(13) Uani 1 d . . C46 C 0.0703(7) 0.0112(5) 0.0460(7) 0.223(10) Uani 1 d . . H46A H 0.0932 -0.0037 0.0331 0.334 Uiso 1 calc . . H46B H 0.0369 -0.0056 0.0285 0.334 Uiso 1 calc . . H46C H 0.0815 -0.0061 0.0758 0.334 Uiso 1 calc . . O51 O -0.2315(2) 0.1253(3) 0.02335(16) 0.0737(15) Uani 1 d . . C52A C -0.1955(8) 0.1250(13) 0.0041(7) 0.118(9) Uani 0.546(18) d A 1 H52A H -0.2126 0.1222 -0.0277 0.177 Uiso 0.546(18) calc A 1 H52B H -0.1734 0.0864 0.0149 0.177 Uiso 0.546(18) calc A 1 H52C H -0.1759 0.1663 0.012 0.177 Uiso 0.546(18) calc A 1 C52B C -0.2321(9) 0.1842(11) -0.0036(6) 0.095(8) Uani 0.454(18) d A 2 H52D H -0.2402 0.1699 -0.0336 0.143 Uiso 0.454(18) calc A 2 H52E H -0.1994 0.2056 0.0082 0.143 Uiso 0.454(18) calc A 2 H52F H -0.2572 0.2161 -0.0031 0.143 Uiso 0.454(18) calc A 2 O53 O -0.28015(17) 0.1945(2) 0.07278(14) 0.0558(11) Uani 1 d . . C54 C -0.2883(3) 0.2505(5) 0.0966(3) 0.084(3) Uani 1 d . . H54A H -0.3217 0.2684 0.0806 0.126 Uiso 1 calc . . H54B H -0.2637 0.2854 0.0997 0.126 Uiso 1 calc . . H54C H -0.2849 0.2354 0.1255 0.126 Uiso 1 calc . . O55 O -0.2625(2) 0.0450(2) 0.08089(19) 0.0728(15) Uani 1 d . . C56 C -0.2488(5) -0.0152(6) 0.1101(4) 0.150(5) Uani 1 d . . H56A H -0.2753 -0.0487 0.0989 0.225 Uiso 1 calc . . H56B H -0.2444 -0.002 0.1396 0.225 Uiso 1 calc . . H56C H -0.2178 -0.0343 0.1108 0.225 Uiso 1 calc . . O61 O -0.1222(2) 0.4530(3) 0.32012(18) 0.0684(14) Uani 1 d . . C62 C -0.1085(4) 0.4139(6) 0.3606(3) 0.104(3) Uani 1 d . . H62A H -0.1187 0.4381 0.3811 0.156 Uiso 1 calc . . H62B H -0.0724 0.4073 0.3737 0.156 Uiso 1 calc . . H62C H -0.1251 0.3704 0.3539 0.156 Uiso 1 calc . . O63 O -0.17916(17) 0.4517(2) 0.22346(17) 0.0601(13) Uani 1 d . . C64 C -0.2149(3) 0.4180(5) 0.1856(3) 0.081(2) Uani 1 d . . H64A H -0.2446 0.4459 0.1724 0.122 Uiso 1 calc . . H64B H -0.224 0.375 0.1944 0.122 Uiso 1 calc . . H64C H -0.2003 0.4104 0.1643 0.122 Uiso 1 calc . . O65 O -0.0817(2) 0.5169(2) 0.2609(2) 0.0782(16) Uani 1 d . . C66 C -0.0383(6) 0.5518(7) 0.2914(6) 0.202(9) Uani 1 d . . H66A H -0.0384 0.598 0.2816 0.303 Uiso 1 calc . . H66B H -0.0082 0.5292 0.2927 0.303 Uiso 1 calc . . H66C H -0.0389 0.5518 0.3204 0.303 Uiso 1 calc . . O71 O -0.20439(15) -0.1179(2) 0.20775(15) 0.0532(11) Uani 1 d . . C72 C -0.2486(3) -0.0976(4) 0.2124(3) 0.066(2) Uani 1 d . . H72A H -0.2777 -0.114 0.1875 0.099 Uiso 1 calc . . H72B H -0.2498 -0.0487 0.2136 0.099 Uiso 1 calc . . H72C H -0.2488 -0.1164 0.2394 0.099 Uiso 1 calc . . O73 O -0.15310(18) -0.1351(2) 0.30545(14) 0.0529(11) Uani 1 d . . C74 C -0.1366(3) -0.1112(6) 0.3484(3) 0.101(4) Uani 1 d . . H74A H -0.1537 -0.1351 0.3639 0.152 Uiso 1 calc . . H74B H -0.1437 -0.0632 0.348 0.152 Uiso 1 calc . . H74C H -0.1007 -0.1184 0.3634 0.152 Uiso 1 calc . . O75 O -0.1149(2) -0.2090(2) 0.24992(19) 0.0727(15) Uani 1 d . . C76 C -0.1430(6) -0.2621(7) 0.2225(7) 0.229(10) Uani 1 d . . H76A H -0.1252 -0.3045 0.2322 0.344 Uiso 1 calc . . H76B H -0.1477 -0.2532 0.1923 0.344 Uiso 1 calc . . H76C H -0.1754 -0.2651 0.2242 0.344 Uiso 1 calc . . O1 O -0.1119(4) 0.5805(6) 0.3513(4) 0.177(4) Uiso 1 d . . C1 C -0.1528(8) 0.6063(12) 0.3582(8) 0.287(12) Uiso 1 d . . H1A H -0.1758 0.5699 0.3565 0.43 Uiso 1 calc . . H1B H -0.1698 0.6398 0.3359 0.43 Uiso 1 calc . . H1C H -0.1411 0.6271 0.3871 0.43 Uiso 1 calc . . O2 O -0.1097(6) 0.5850(8) 0.1860(5) 0.114(5) Uiso 0.5 d . . O5 O -0.2380(3) -0.1763(4) 0.1278(3) 0.124(3) Uiso 1 d . . C5 C -0.2114(7) -0.1977(9) 0.1004(6) 0.203(7) Uiso 1 d . . H5A H -0.2322 -0.229 0.0779 0.304 Uiso 1 calc . . H5B H -0.1803 -0.2198 0.1188 0.304 Uiso 1 calc . . H5C H -0.2041 -0.1585 0.0864 0.304 Uiso 1 calc . . C44 C 0.0914(8) 0.2874(9) 0.0733(7) 0.287(12) Uani 1 d . . H44A H 0.1079 0.3116 0.0574 0.43 Uiso 1 calc . . H44B H 0.1156 0.2768 0.1027 0.43 Uiso 1 calc . . H44C H 0.065 0.3153 0.0752 0.43 Uiso 1 calc . . C2 C -0.1585(8) 0.5870(14) 0.1613(8) 0.146(10) Uiso 0.5 d . . H2A H -0.1733 0.5435 0.1623 0.219 Uiso 0.5 calc . . H2B H -0.1639 0.5974 0.1311 0.219 Uiso 0.5 calc . . H2C H -0.1739 0.6216 0.1724 0.219 Uiso 0.5 calc . . O4 O -0.0795(12) -0.2859(16) 0.3238(11) 0.270(14) Uiso 0.5 d . . C4 C -0.0409(13) -0.2693(17) 0.3667(11) 0.183(13) Uiso 0.5 d . . O3 O 0.1716(10) 0.1021(12) 0.0668(8) 0.189(9) Uiso 0.5 d . . C3 C 0.2079(12) 0.0715(16) 0.0950(11) 0.170(12) Uiso 0.5 d . . H3A H 0.1963 0.0448 0.1136 0.255 Uiso 0.5 calc . . H3B H 0.2325 0.1041 0.1129 0.255 Uiso 0.5 calc . . H3C H 0.223 0.0421 0.0803 0.255 Uiso 0.5 calc . . O6 O -0.2443(12) 0.5083(16) 0.0147(10) 0.260(13) Uiso 0.5 d . . C6 C -0.2087(14) 0.5525(18) 0.0109(14) 0.200(16) Uiso 0.5 d . . O7 O -0.3699(15) 0.029(2) 0.0389(13) 0.340(19) Uiso 0.5 d . . C7 C -0.3488(14) -0.0020(19) 0.0123(12) 0.194(14) Uiso 0.5 d . . O8 O 0.1487(16) 0.215(2) 0.0178(14) 0.35(2) Uiso 0.5 d . . C8 C 0.1161(16) 0.248(2) -0.0209(14) 0.228(18) Uiso 0.5 d . . O9 O -0.0315(9) 0.5673(12) 0.4322(9) 0.201(10) Uiso 0.5 d . . C9 C -0.027(2) 0.584(3) 0.474(2) 0.32(3) Uiso 0.5 d . . O10 O 0 -0.2467(14) 0.25 0.162(10) Uiso 0.5 d . . C10 C -0.0202(13) -0.2620(18) 0.2801(10) 0.080(10) Uiso 0.25 d . . O1S O -0.0613(12) 0.6454(14) 0.1444(11) 0.235(12) Uiso 0.5 d . . C1S C -0.073(2) 0.622(3) 0.1018(13) 0.27(2) Uiso 0.5 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 0.03662(12) 0.03008(11) 0.02483(10) 0.00360(7) 0.00855(9) 0.00513(8) W2 0.02394(10) 0.02837(11) 0.02840(10) -0.00095(7) 0.01207(8) -0.00087(7) W3 0.03160(11) 0.03176(11) 0.02479(10) -0.00500(7) 0.01091(8) -0.00104(8) Fe1 0.0182(4) 0.0214(4) 0.0174(4) 0 0.0072(3) 0 Fe2 0.0320(4) 0.0281(4) 0.0418(4) -0.0046(3) 0.0164(3) 0.0028(3) Fe3 0.0337(4) 0.0295(4) 0.0345(4) -0.0013(3) 0.0158(3) -0.0048(3) Fe4 0.0404(4) 0.0426(4) 0.0248(4) -0.0010(3) 0.0153(3) 0.0003(3) Fe5 0.0287(4) 0.0462(5) 0.0265(4) 0.0026(3) 0.0059(3) 0.0030(3) C11 0.036(3) 0.026(2) 0.029(2) 0.0011(19) 0.011(2) 0.001(2) N11 0.037(2) 0.033(2) 0.030(2) 0.0021(18) 0.0095(19) 0.0003(19) C12 0.032(3) 0.040(3) 0.043(3) -0.005(2) 0.012(2) 0.001(2) N12 0.045(3) 0.054(3) 0.044(3) -0.007(2) 0.021(2) 0.006(2) C32 0.039(3) 0.037(3) 0.030(3) 0.002(2) 0.014(2) -0.005(2) N32 0.041(3) 0.043(3) 0.042(3) 0.002(2) 0.015(2) -0.008(2) C14 0.042(3) 0.044(3) 0.028(3) 0.000(2) 0.013(2) -0.002(2) N14 0.049(3) 0.057(3) 0.032(2) -0.002(2) 0.017(2) 0.005(2) C15 0.039(3) 0.049(3) 0.038(3) 0.006(3) 0.013(3) 0.004(3) N15 0.037(3) 0.063(3) 0.049(3) 0.011(3) 0.009(2) -0.005(3) C16 0.161(10) 0.139(9) 0.064(6) 0.033(6) 0.046(6) 0.117(8) N16 0.232(13) 0.254(14) 0.105(8) 0.063(8) 0.072(8) 0.205(12) C17 0.046(4) 0.055(4) 0.027(3) 0.007(2) 0.004(3) 0.006(3) N17 0.062(4) 0.088(4) 0.032(3) -0.006(3) -0.001(3) 0.003(3) C18 0.146(9) 0.081(6) 0.046(4) 0.022(4) -0.004(5) -0.053(6) N18 0.232(13) 0.151(9) 0.092(7) 0.065(6) -0.026(7) -0.108(9) C21 0.032(3) 0.029(3) 0.032(3) -0.001(2) 0.013(2) -0.001(2) N21 0.031(2) 0.038(2) 0.033(2) -0.0021(18) 0.0138(19) 0.0005(18) C22 0.029(3) 0.034(3) 0.041(3) -0.003(2) 0.012(2) 0.001(2) N22 0.039(3) 0.033(3) 0.068(4) -0.004(2) 0.021(3) -0.001(2) C23 0.028(3) 0.030(3) 0.042(3) 0.000(2) 0.013(2) -0.003(2) N23 0.047(3) 0.035(3) 0.049(3) 0.000(2) 0.022(2) -0.003(2) C24 0.033(3) 0.045(3) 0.032(3) 0.001(2) 0.016(2) -0.001(2) N24 0.047(3) 0.066(4) 0.031(3) 0.001(2) 0.013(2) 0.000(3) C25 0.029(3) 0.041(3) 0.033(3) 0.004(2) 0.013(2) 0.006(2) N25 0.038(3) 0.058(3) 0.029(2) 0.002(2) 0.010(2) 0.008(2) C26 0.043(3) 0.038(3) 0.080(5) 0.003(3) 0.031(3) 0.003(3) N26 0.064(4) 0.052(4) 0.170(8) 0.002(4) 0.066(5) -0.016(3) C27 0.050(4) 0.071(5) 0.045(4) -0.004(3) 0.024(3) 0.016(3) N27 0.084(5) 0.137(7) 0.065(4) -0.021(4) 0.045(4) 0.024(5) C28 0.034(3) 0.039(3) 0.038(3) -0.003(2) 0.012(2) 0.001(2) N28 0.042(3) 0.057(3) 0.061(3) 0.000(3) 0.016(3) 0.018(3) C31 0.031(3) 0.037(3) 0.030(3) 0.000(2) 0.012(2) 0.002(2) N31 0.037(2) 0.033(2) 0.033(2) -0.0040(19) 0.013(2) -0.0002(19) C13 0.037(3) 0.034(3) 0.036(3) -0.007(2) 0.014(2) 0.000(2) N13 0.039(3) 0.052(3) 0.050(3) -0.010(2) 0.019(3) 0.000(2) C33 0.040(3) 0.034(3) 0.037(3) -0.003(2) 0.017(2) -0.004(2) N33 0.051(3) 0.046(3) 0.041(3) 0.001(2) 0.021(2) -0.003(2) C34 0.044(3) 0.045(3) 0.028(3) -0.003(2) 0.017(2) 0.002(3) N34 0.053(3) 0.047(3) 0.038(3) -0.003(2) 0.023(2) -0.006(2) C35 0.038(3) 0.055(4) 0.032(3) 0.000(3) 0.013(2) 0.006(3) N35 0.045(3) 0.066(4) 0.038(3) 0.003(2) 0.008(2) 0.015(3) C36 0.105(6) 0.040(4) 0.090(6) -0.019(3) 0.073(6) -0.015(4) N36 0.180(9) 0.045(4) 0.152(8) -0.024(4) 0.114(8) -0.018(5) C37 0.067(5) 0.089(6) 0.066(5) -0.050(5) -0.026(4) 0.030(4) N37 0.136(9) 0.191(11) 0.099(7) -0.085(7) -0.052(6) 0.069(8) C38 0.069(4) 0.047(3) 0.038(3) -0.004(3) 0.029(3) -0.001(3) N38 0.104(5) 0.064(4) 0.063(4) -0.014(3) 0.056(4) 0.004(4) O41 0.058(3) 0.093(4) 0.027(2) -0.003(2) 0.016(2) 0.019(3) C42 0.081(7) 0.212(13) 0.055(5) -0.034(7) 0.001(5) 0.068(8) O43 0.107(5) 0.069(3) 0.071(4) -0.002(3) 0.052(3) -0.027(3) O45 0.069(3) 0.063(3) 0.075(3) -0.013(3) 0.041(3) 0.007(3) C46 0.33(2) 0.057(7) 0.42(3) -0.011(11) 0.31(2) 0.007(10) O51 0.075(4) 0.103(4) 0.037(3) 0.005(3) 0.017(3) -0.005(3) C52A 0.126(15) 0.155(17) 0.087(12) 0.009(11) 0.058(11) -0.018(12) C52B 0.098(14) 0.125(15) 0.063(11) 0.038(10) 0.033(10) -0.016(11) O53 0.048(3) 0.065(3) 0.039(2) -0.002(2) 0.001(2) 0.014(2) C54 0.089(6) 0.098(7) 0.057(5) 0.003(4) 0.020(5) 0.042(5) O55 0.075(4) 0.058(3) 0.080(4) -0.003(3) 0.025(3) -0.021(3) C56 0.186(14) 0.097(9) 0.125(10) 0.033(8) 0.018(10) -0.035(9) O61 0.074(4) 0.077(4) 0.067(3) -0.018(3) 0.041(3) -0.001(3) C62 0.099(8) 0.153(10) 0.072(6) -0.030(6) 0.048(6) -0.015(7) O63 0.044(3) 0.062(3) 0.067(3) -0.001(2) 0.014(2) 0.020(2) C64 0.054(5) 0.094(6) 0.081(6) -0.002(5) 0.012(4) 0.001(4) O65 0.081(4) 0.043(3) 0.109(5) -0.002(3) 0.035(4) -0.020(3) C66 0.184(16) 0.142(13) 0.220(18) 0.018(12) 0.017(14) -0.093(12) O71 0.035(2) 0.066(3) 0.053(3) -0.010(2) 0.011(2) -0.001(2) C72 0.044(4) 0.080(5) 0.075(5) 0.011(4) 0.024(4) -0.001(4) O73 0.064(3) 0.063(3) 0.038(2) -0.002(2) 0.027(2) -0.026(2) C74 0.085(6) 0.170(10) 0.054(5) -0.025(6) 0.032(5) -0.068(7) O75 0.085(4) 0.039(3) 0.097(4) -0.006(3) 0.039(3) 0.001(2) C76 0.144(13) 0.121(11) 0.40(3) -0.121(14) 0.086(16) 0.000(9) C44 0.285(18) 0.282(18) 0.313(19) 0.029(15) 0.141(15) -0.093(15) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C18 2.120(8) . ? W1 C16 2.143(8) . ? W1 C13 2.144(6) 2 ? W1 C14 2.146(6) . ? W1 C15 2.151(6) . ? W1 C11 2.162(5) . ? W1 C12 2.164(6) . ? W1 C17 2.174(6) . ? W2 C26 2.133(6) . ? W2 C25 2.149(5) . ? W2 C24 2.154(6) 2 ? W2 C22 2.156(5) . ? W2 C27 2.157(6) . ? W2 C21 2.163(5) . ? W2 C28 2.171(6) . ? W2 C23 2.174(5) . ? W3 C37 2.140(7) . ? W3 C36 2.143(7) . ? W3 C31 2.157(5) . ? W3 C33 2.160(5) . ? W3 C32 2.163(6) 2 ? W3 C38 2.168(6) . ? W3 C34 2.170(6) . ? W3 C35 2.171(6) . ? Fe1 N31 2.071(4) 2 ? Fe1 N31 2.071(4) . ? Fe1 N21 2.082(4) . ? Fe1 N21 2.082(4) 2 ? Fe1 N11 2.083(4) 2 ? Fe1 N11 2.083(4) . ? Fe2 O63 2.108(4) . ? Fe2 N13 2.111(5) . ? Fe2 O65 2.115(5) . ? Fe2 N12 2.121(5) . ? Fe2 N22 2.126(5) . ? Fe2 O61 2.148(5) . ? Fe3 O75 2.117(5) . ? Fe3 O71 2.117(4) . ? Fe3 N32 2.118(5) . ? Fe3 N33 2.134(5) . ? Fe3 N23 2.135(5) . ? Fe3 O73 2.155(4) . ? Fe4 O43 2.109(5) . ? Fe4 O41 2.115(4) . ? Fe4 N24 2.124(5) . ? Fe4 O45 2.127(4) . ? Fe4 N14 2.128(5) . ? Fe4 N34 2.135(5) . ? Fe5 N25 2.110(5) . ? Fe5 O55 2.117(5) . ? Fe5 N15 2.120(5) . ? Fe5 O53 2.124(4) . ? Fe5 N35 2.125(5) . ? Fe5 O51 2.129(5) . ? C11 N11 1.134(6) . ? C12 N12 1.132(7) . ? C32 N32 1.140(7) . ? C32 W3 2.163(6) 2 ? C14 N14 1.141(7) . ? C15 N15 1.163(7) . ? C16 N16 1.120(10) . ? C17 N17 1.151(7) . ? C18 N18 1.145(11) . ? C21 N21 1.126(7) . ? C22 N22 1.135(7) . ? C23 N23 1.135(6) . ? C24 N24 1.140(7) . ? C24 W2 2.155(6) 2 ? C25 N25 1.144(7) . ? C26 N26 1.159(8) . ? C27 N27 1.147(8) . ? C28 N28 1.144(7) . ? C31 N31 1.140(6) . ? C13 N13 1.151(7) . ? C13 W1 2.144(6) 2 ? C33 N33 1.142(7) . ? C34 N34 1.133(7) . ? C35 N35 1.127(7) . ? C36 N36 1.157(9) . ? C37 N37 1.117(9) . ? C38 N38 1.148(7) . ? O41 C42 1.379(9) . ? O43 C44 1.419(15) . ? O45 C46 1.367(11) . ? O51 C52A 1.418(14) . ? O51 C52B 1.449(14) . ? O53 C54 1.417(9) . ? O55 C56 1.469(11) . ? O61 C62 1.443(11) . ? O63 C64 1.420(9) . ? O65 C66 1.426(13) . ? O71 C72 1.402(7) . ? O73 C74 1.377(9) . ? O75 C76 1.401(13) . ? O1 C1 1.381(15) . ? O2 C2 1.313(16) . ? O5 C5 1.459(17) . ? O4 C4 1.437(18) . ? O3 C3 1.24(3) . ? O6 C6 1.386(18) . ? O7 C7 1.392(19) . ? O8 C8 1.399(19) . ? O9 C9 1.36(6) . ? O10 C10 1.365(18) . ? O10 C10 1.365(18) 2 ? O1S C1S 1.381(19) . ? 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 C18 W1 C16 78.3(5) . . ? C18 W1 C13 69.7(3) . 2 ? C16 W1 C13 120.5(4) . 2 ? C18 W1 C14 86.8(4) . . ? C16 W1 C14 144.8(3) . . ? C13 W1 C14 82.4(2) 2 . ? C18 W1 C15 146.1(3) . . ? C16 W1 C15 81.5(4) . . ? C13 W1 C15 144.1(2) 2 . ? C14 W1 C15 94.5(2) . . ? C18 W1 C11 138.3(3) . . ? C16 W1 C11 136.1(3) . . ? C13 W1 C11 71.43(19) 2 . ? C14 W1 C11 73.72(19) . . ? C15 W1 C11 73.4(2) . . ? C18 W1 C12 109.8(3) . . ? C16 W1 C12 70.6(3) . . ? C13 W1 C12 75.1(2) 2 . ? C14 W1 C12 144.5(2) . . ? C15 W1 C12 88.3(2) . . ? C11 W1 C12 73.3(2) . . ? C18 W1 C17 73.5(3) . . ? C16 W1 C17 72.2(3) . . ? C13 W1 C17 136.4(2) 2 . ? C14 W1 C17 73.0(2) . . ? C15 W1 C17 74.6(2) . . ? C11 W1 C17 131.1(2) . . ? C12 W1 C17 140.9(2) . . ? C26 W2 C25 90.4(2) . . ? C26 W2 C24 105.5(2) . 2 ? C25 W2 C24 145.34(19) . 2 ? C26 W2 C22 146.6(2) . . ? C25 W2 C22 97.9(2) . . ? C24 W2 C22 85.7(2) 2 . ? C26 W2 C27 75.2(3) . . ? C25 W2 C27 144.4(2) . . ? C24 W2 C27 70.3(2) 2 . ? C22 W2 C27 79.4(2) . . ? C26 W2 C21 141.3(2) . . ? C25 W2 C21 73.67(19) . . ? C24 W2 C21 74.9(2) 2 . ? C22 W2 C21 71.76(19) . . ? C27 W2 C21 135.9(2) . . ? C26 W2 C28 77.3(2) . . ? C25 W2 C28 72.1(2) . . ? C24 W2 C28 140.8(2) 2 . ? C22 W2 C28 74.7(2) . . ? C27 W2 C28 73.0(2) . . ? C21 W2 C28 127.3(2) . . ? C26 W2 C23 70.5(2) . . ? C25 W2 C23 78.3(2) . . ? C24 W2 C23 78.4(2) 2 . ? C22 W2 C23 142.83(19) . . ? C27 W2 C23 124.5(2) . . ? C21 W2 C23 71.74(18) . . ? C28 W2 C23 135.7(2) . . ? C37 W3 C36 76.9(4) . . ? C37 W3 C31 140.5(2) . . ? C36 W3 C31 134.5(3) . . ? C37 W3 C33 105.1(3) . . ? C36 W3 C33 70.0(2) . . ? C31 W3 C33 74.25(19) . . ? C37 W3 C32 146.2(2) . 2 ? C36 W3 C32 79.6(3) . 2 ? C31 W3 C32 72.60(19) . 2 ? C33 W3 C32 89.1(2) . 2 ? C37 W3 C38 74.8(3) . . ? C36 W3 C38 72.2(2) . . ? C31 W3 C38 130.6(2) . . ? C33 W3 C38 141.1(2) . . ? C32 W3 C38 75.0(2) 2 . ? C37 W3 C34 91.1(3) . . ? C36 W3 C34 144.0(2) . . ? C31 W3 C34 74.11(19) . . ? C33 W3 C34 145.7(2) . . ? C32 W3 C34 93.8(2) 2 . ? C38 W3 C34 71.9(2) . . ? C37 W3 C35 70.1(2) . . ? C36 W3 C35 124.5(3) . . ? C31 W3 C35 71.4(2) . . ? C33 W3 C35 77.1(2) . . ? C32 W3 C35 143.7(2) 2 . ? C38 W3 C35 134.5(2) . . ? C34 W3 C35 80.7(2) . . ? N31 Fe1 N31 88.3(2) 2 . ? N31 Fe1 N21 89.47(17) 2 . ? N31 Fe1 N21 93.33(17) . . ? N31 Fe1 N21 93.33(17) 2 2 ? N31 Fe1 N21 89.47(17) . 2 ? N21 Fe1 N21 176.1(2) . 2 ? N31 Fe1 N11 88.28(18) 2 2 ? N31 Fe1 N11 174.87(17) . 2 ? N21 Fe1 N11 90.45(17) . 2 ? N21 Fe1 N11 86.93(17) 2 2 ? N31 Fe1 N11 174.87(17) 2 . ? N31 Fe1 N11 88.28(18) . . ? N21 Fe1 N11 86.93(17) . . ? N21 Fe1 N11 90.44(17) 2 . ? N11 Fe1 N11 95.4(2) 2 . ? O63 Fe2 N13 175.29(19) . . ? O63 Fe2 O65 85.8(2) . . ? N13 Fe2 O65 91.3(2) . . ? O63 Fe2 N12 87.99(19) . . ? N13 Fe2 N12 95.80(19) . . ? O65 Fe2 N12 90.7(2) . . ? O63 Fe2 N22 90.70(19) . . ? N13 Fe2 N22 92.0(2) . . ? O65 Fe2 N22 176.0(2) . . ? N12 Fe2 N22 91.1(2) . . ? O63 Fe2 O61 86.9(2) . . ? N13 Fe2 O61 89.2(2) . . ? O65 Fe2 O61 86.4(2) . . ? N12 Fe2 O61 174.3(2) . . ? N22 Fe2 O61 91.4(2) . . ? O75 Fe3 O71 89.6(2) . . ? O75 Fe3 N32 89.7(2) . . ? O71 Fe3 N32 178.87(19) . . ? O75 Fe3 N33 90.2(2) . . ? O71 Fe3 N33 89.46(19) . . ? N32 Fe3 N33 91.42(19) . . ? O75 Fe3 N23 173.8(2) . . ? O71 Fe3 N23 89.49(18) . . ? N32 Fe3 N23 91.12(19) . . ? N33 Fe3 N23 95.95(19) . . ? O75 Fe3 O73 84.4(2) . . ? O71 Fe3 O73 87.75(18) . . ? N32 Fe3 O73 91.31(18) . . ? N33 Fe3 O73 173.96(18) . . ? N23 Fe3 O73 89.37(18) . . ? O43 Fe4 O41 86.9(2) . . ? O43 Fe4 N24 90.5(2) . . ? O41 Fe4 N24 174.23(19) . . ? O43 Fe4 O45 84.3(2) . . ? O41 Fe4 O45 85.95(19) . . ? N24 Fe4 O45 88.7(2) . . ? O43 Fe4 N14 90.3(2) . . ? O41 Fe4 N14 91.40(18) . . ? N24 Fe4 N14 93.8(2) . . ? O45 Fe4 N14 174.1(2) . . ? O43 Fe4 N34 176.8(2) . . ? O41 Fe4 N34 90.8(2) . . ? N24 Fe4 N34 91.6(2) . . ? O45 Fe4 N34 93.3(2) . . ? N14 Fe4 N34 92.0(2) . . ? N25 Fe5 O55 90.9(2) . . ? N25 Fe5 N15 91.0(2) . . ? O55 Fe5 N15 178.1(2) . . ? N25 Fe5 O53 90.35(18) . . ? O55 Fe5 O53 88.8(2) . . ? N15 Fe5 O53 90.9(2) . . ? N25 Fe5 N35 95.19(19) . . ? O55 Fe5 N35 88.7(2) . . ? N15 Fe5 N35 91.4(2) . . ? O53 Fe5 N35 173.96(19) . . ? N25 Fe5 O51 173.7(2) . . ? O55 Fe5 O51 84.7(2) . . ? N15 Fe5 O51 93.4(2) . . ? O53 Fe5 O51 85.0(2) . . ? N35 Fe5 O51 89.3(2) . . ? N11 C11 W1 177.0(5) . . ? C11 N11 Fe1 175.6(4) . . ? N12 C12 W1 177.1(5) . . ? C12 N12 Fe2 178.8(5) . . ? N32 C32 W3 177.7(5) . 2 ? C32 N32 Fe3 172.6(5) . . ? N14 C14 W1 177.3(5) . . ? C14 N14 Fe4 173.2(5) . . ? N15 C15 W1 176.4(5) . . ? C15 N15 Fe5 171.2(5) . . ? N16 C16 W1 179.5(16) . . ? N17 C17 W1 177.3(6) . . ? N18 C18 W1 177.6(9) . . ? N21 C21 W2 177.8(5) . . ? C21 N21 Fe1 176.6(5) . . ? N22 C22 W2 176.7(5) . . ? C22 N22 Fe2 173.9(5) . . ? N23 C23 W2 177.0(5) . . ? C23 N23 Fe3 175.7(5) . . ? N24 C24 W2 175.7(5) . 2 ? C24 N24 Fe4 173.7(5) . . ? N25 C25 W2 176.8(5) . . ? C25 N25 Fe5 172.1(5) . . ? N26 C26 W2 179.1(7) . . ? N27 C27 W2 179.4(8) . . ? N28 C28 W2 177.4(6) . . ? N31 C31 W3 178.8(5) . . ? C31 N31 Fe1 178.8(5) . . ? N13 C13 W1 178.8(5) . 2 ? C13 N13 Fe2 176.6(5) . . ? N33 C33 W3 176.7(5) . . ? C33 N33 Fe3 174.6(5) . . ? N34 C34 W3 177.1(5) . . ? C34 N34 Fe4 170.7(5) . . ? N35 C35 W3 177.9(6) . . ? C35 N35 Fe5 177.5(6) . . ? N36 C36 W3 178.3(10) . . ? N37 C37 W3 178.6(13) . . ? N38 C38 W3 179.3(6) . . ? C42 O41 Fe4 129.5(5) . . ? C44 O43 Fe4 127.0(9) . . ? C46 O45 Fe4 132.8(6) . . ? C52A O51 Fe5 125.8(10) . . ? C52B O51 Fe5 123.2(10) . . ? C54 O53 Fe5 127.0(4) . . ? C56 O55 Fe5 122.6(6) . . ? C62 O61 Fe2 121.4(5) . . ? C64 O63 Fe2 126.9(4) . . ? C66 O65 Fe2 128.6(7) . . ? C72 O71 Fe3 127.1(4) . . ? C74 O73 Fe3 127.9(4) . . ? C76 O75 Fe3 133.6(7) . . ? C10 O10 C10 155(4) . 2 ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF _database_code_depnum_ccdc_archive 'CCDC 966455' ####################################################################### # # 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_1_LT _audit_creation_date 2013-11-28T21:18:09-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'Compound X' _chemical_formula_moiety 'C72 H72 Fe9 N48 O24 W6' _chemical_formula_sum 'C90 H168 Fe9 N48 O42 W6' _chemical_formula_weight 4200.24 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.3480(4) _cell_length_b 19.0770(3) _cell_length_c 32.3450(5) _cell_angle_alpha 90 _cell_angle_beta 113.6570(10) _cell_angle_gamma 90 _cell_volume 16022.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 89741 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.718 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8004 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.153 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3070 _exptl_absorpt_correction_T_max 0.4573 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 140(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.0219031 _diffrn_orient_matrix_ub_12 0.0411763 _diffrn_orient_matrix_ub_13 0.0001638 _diffrn_orient_matrix_ub_21 -0.0315444 _diffrn_orient_matrix_ub_22 0.0297715 _diffrn_orient_matrix_ub_23 -0.013589 _diffrn_orient_matrix_ub_31 0.002892 _diffrn_orient_matrix_ub_32 0.0128762 _diffrn_orient_matrix_ub_33 0.030896 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.1217 _diffrn_reflns_number 57634 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.325 _diffrn_reflns_theta_max 27.502 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_Laue_measured_fraction_full 0.989 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_point_group_measured_fraction_full 0.989 _diffrn_reflns_point_group_measured_fraction_max 0.989 _reflns_number_total 18205 _reflns_number_gt 14691 _reflns_threshold_expression 'I > 2\s(I)' #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-2012 (Sheldrick, 2012)' _computing_molecular_graphics 'Ortep (Johnson, 1976)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; DFIX 1.400 0.020 O3 C3 DFIX 1.400 0.020 O9 C9 DFIX 1.400 0.020 O1 C1 DFIX 1.400 0.020 O1S C1S DFIX 1.400 0.020 O4 C4 DFIX 1.400 0.020 O2 C2 DFIX 1.400 0.020 O10 C10 DFIX 1.400 0.020 O5 C5 DFIX 1.400 0.020 O2S C2S DFIX 1.400 0.020 O6 C6 DFIX 1.400 0.020 O7 C7 DFIX 1.400 0.020 O8 C8 DELU 0.01 C52 O51 ISOR 0.01 C52 Distances C-O in some methanol molecules were restrained to prevent proper geometry.Isotropic refinement of non-hydrogen atoms of solvent molecules and ISOR restraints on C atoms of some terminal methanols were used to ensure the convergence of the refinement process. ; _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^)+(0.0980P)^2^+162.8645P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 18205 _refine_ls_number_parameters 831 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0741 _refine_ls_R_factor_gt 0.0569 _refine_ls_wR_factor_ref 0.1747 _refine_ls_wR_factor_gt 0.1562 _refine_ls_goodness_of_fit_gt 307.679 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 3.284 _refine_diff_density_min -3.839 _refine_diff_density_rms 0.395 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' W W -0.849 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_disorder_assembly _atom_site_disorder_group W1 W -0.07580(2) 0.34649(2) 0.11744(2) 0.01994(10) Uani 1 d . . W2 W 0.17953(2) 0.17597(2) 0.23377(2) 0.01607(9) Uani 1 d . . W3 W -0.06141(2) -0.04147(2) 0.12402(2) 0.01599(9) Uani 1 d . . Fe1 Fe 0 0.15774(7) 0.25 0.0117(3) Uani 1 d . . Fe2 Fe 0.10717(4) 0.43232(6) 0.23788(4) 0.0190(2) Uani 1 d . . Fe5 Fe -0.21518(5) 0.14313(6) 0.09258(4) 0.0225(3) Uani 1 d . . Fe3 Fe 0.12962(4) -0.09580(6) 0.24628(4) 0.0178(2) Uani 1 d . . Fe4 Fe 0.03097(5) 0.15801(6) 0.06889(4) 0.0216(3) Uani 1 d . . C16 C -0.1344(6) 0.4252(7) 0.0945(3) 0.063(4) Uani 1 d . . N16 N -0.1684(6) 0.4651(7) 0.0814(4) 0.096(5) Uani 1 d . . N28 N 0.2822(3) 0.2714(5) 0.2941(3) 0.043(2) Uani 1 d . . C18 C -0.0424(4) 0.4240(5) 0.0874(3) 0.044(3) Uani 1 d . . N18 N -0.0250(5) 0.4639(6) 0.0713(4) 0.079(4) Uani 1 d . . C17 C -0.1158(3) 0.3326(4) 0.0450(2) 0.0233(17) Uani 1 d . . N17 N -0.1384(3) 0.3241(5) 0.0068(3) 0.039(2) Uani 1 d . . C11 C -0.0460(3) 0.2679(4) 0.1692(3) 0.0202(16) Uani 1 d . . N11 N -0.0281(3) 0.2297(3) 0.1992(2) 0.0197(13) Uani 1 d . . C13 C -0.0028(3) 0.3846(4) 0.1657(3) 0.0236(17) Uani 1 d . . N13 N 0.0349(3) 0.4038(4) 0.1926(2) 0.0230(14) Uani 1 d . . C15 C -0.1379(3) 0.2744(5) 0.1068(3) 0.0276(19) Uani 1 d . . N15 N -0.1697(3) 0.2327(4) 0.1004(2) 0.0288(16) Uani 1 d . . C12 C -0.0905(3) 0.3840(4) 0.1743(3) 0.0216(16) Uani 1 d . . N12 N -0.0955(3) 0.4027(4) 0.2057(2) 0.0282(16) Uani 1 d . . C14 C -0.0303(3) 0.2752(4) 0.0972(2) 0.0184(15) Uani 1 d . . N14 N -0.0077(3) 0.2360(4) 0.0860(2) 0.0269(16) Uani 1 d . . C28 C 0.2468(3) 0.2371(4) 0.2730(3) 0.0259(18) Uani 1 d . . C26 C 0.2408(4) 0.1109(5) 0.2325(3) 0.033(2) Uani 1 d . . N26 N 0.2733(4) 0.0751(5) 0.2314(4) 0.054(3) Uani 1 d . . C27 C 0.2063(3) 0.2312(5) 0.1873(3) 0.0300(19) Uani 1 d . . N27 N 0.2192(4) 0.2600(5) 0.1638(3) 0.051(2) Uani 1 d . . C21 C 0.1080(3) 0.1706(4) 0.2416(2) 0.0165(15) Uani 1 d . . N21 N 0.0704(3) 0.1655(3) 0.2459(2) 0.0196(14) Uani 1 d . . C22 C 0.1509(3) 0.2796(4) 0.2333(3) 0.0190(15) Uani 1 d . . N22 N 0.1370(3) 0.3360(3) 0.2335(3) 0.0247(15) Uani 1 d . . C25 C 0.2000(3) 0.1564(4) 0.3041(3) 0.0207(17) Uani 1 d . . N25 N 0.2077(3) 0.1474(4) 0.3414(2) 0.0268(16) Uani 1 d . . C23 C 0.1590(3) 0.0667(4) 0.2354(3) 0.0209(16) Uani 1 d . . N23 N 0.1482(3) 0.0099(3) 0.2385(2) 0.0224(14) Uani 1 d . . C24 C 0.1223(3) 0.1607(4) 0.1664(3) 0.0183(16) Uani 1 d . . N24 N 0.0907(3) 0.1565(4) 0.1313(2) 0.0238(15) Uani 1 d . . C36 C -0.0706(4) -0.1538(5) 0.1254(3) 0.033(2) Uani 1 d . . N36 N -0.0746(5) -0.2141(5) 0.1267(3) 0.061(3) Uani 1 d . . C38 C -0.0234(3) -0.0899(5) 0.0835(3) 0.0257(18) Uani 1 d . . N38 N -0.0050(3) -0.1136(4) 0.0621(3) 0.0351(19) Uani 1 d . . C37 C -0.1236(4) -0.0644(5) 0.0599(3) 0.036(2) Uani 1 d . . N37 N -0.1574(4) -0.0751(5) 0.0263(3) 0.055(3) Uani 1 d . . C31 C -0.0337(3) 0.0373(4) 0.1760(2) 0.0184(15) Uani 1 d . . N31 N -0.0214(3) 0.0801(3) 0.2024(2) 0.0199(14) Uani 1 d . . C33 C -0.0960(3) -0.0660(4) 0.1703(3) 0.0211(16) Uani 1 d . . N33 N -0.1126(3) -0.0774(4) 0.1973(2) 0.0250(15) Uani 1 d . . C35 C -0.1208(4) 0.0368(4) 0.1101(3) 0.0250(18) Uani 1 d . . N35 N -0.1527(3) 0.0780(4) 0.1044(2) 0.0305(17) Uani 1 d . . C32 C 0.0126(3) -0.0724(4) 0.1731(2) 0.0188(15) Uani 1 d . . N32 N 0.0532(3) -0.0869(4) 0.1998(2) 0.0254(15) Uani 1 d . . C34 C -0.0293(3) 0.0391(4) 0.0971(2) 0.0204(16) Uani 1 d . . N34 N -0.0094(3) 0.0813(4) 0.0842(2) 0.0245(15) Uani 1 d . . O63 O 0.1771(3) 0.4683(4) 0.2799(2) 0.0355(15) Uani 1 d . . C64 C 0.2142(5) 0.4306(9) 0.3213(5) 0.084(5) Uani 1 d . . H64A H 0.2453 0.4591 0.3358 0.126 Uiso 1 calc . . H64B H 0.2236 0.3853 0.3123 0.126 Uiso 1 calc . . H64C H 0.1979 0.4228 0.3424 0.126 Uiso 1 calc . . O61 O 0.1230(3) 0.4674(3) 0.1847(2) 0.0316(14) Uani 1 d . . C62 C 0.1115(5) 0.4284(8) 0.1439(4) 0.063(4) Uani 1 d . . H62A H 0.1224 0.4552 0.1235 0.094 Uiso 1 calc . . H62B H 0.0744 0.4196 0.1294 0.094 Uiso 1 calc . . H62C H 0.13 0.3836 0.1511 0.094 Uiso 1 calc . . O65 O 0.0828(3) 0.5313(3) 0.2411(2) 0.0414(17) Uani 1 d . . C66 C 0.0351(8) 0.5642(9) 0.2068(7) 0.110(7) Uani 1 d . . H66A H 0.0319 0.6123 0.2159 0.164 Uiso 1 calc . . H66B H 0.0048 0.537 0.2047 0.164 Uiso 1 calc . . H66C H 0.0372 0.5647 0.1773 0.164 Uiso 1 calc . . O55 O -0.2595(3) 0.0526(4) 0.0835(3) 0.0435(17) Uani 1 d . . C56 C -0.2423(7) -0.0075(7) 0.1140(6) 0.094(6) Uani 1 d . . H56A H -0.2686 -0.0443 0.1039 0.141 Uiso 1 calc . . H56B H -0.2369 0.0072 0.1447 0.141 Uiso 1 calc . . H56C H -0.21 -0.0256 0.114 0.141 Uiso 1 calc . . O53 O -0.2826(3) 0.2007(4) 0.07327(19) 0.0339(15) Uani 1 d . . C54 C -0.2941(8) 0.2640(14) 0.0997(6) 0.143(10) Uani 1 d . . H54A H -0.3292 0.2814 0.0826 0.214 Uiso 1 calc . . H54B H -0.2694 0.3019 0.1034 0.214 Uiso 1 calc . . H54C H -0.291 0.2479 0.1295 0.214 Uiso 1 calc . . O51 O -0.2328(3) 0.1353(4) 0.0234(2) 0.0432(17) Uani 1 d . . C52 C -0.2298(11) 0.1808(13) -0.0049(7) 0.142(9) Uani 1 d . . O71 O 0.2094(2) -0.1131(3) 0.2882(2) 0.0310(14) Uani 1 d . . C72 C 0.2505(4) -0.0811(5) 0.2817(4) 0.043(3) Uani 1 d . . H72A H 0.2832 -0.0972 0.305 0.065 Uiso 1 calc . . H72B H 0.2479 -0.0301 0.2837 0.065 Uiso 1 calc . . H72C H 0.2491 -0.0936 0.2518 0.065 Uiso 1 calc . . O75 O 0.1193(3) -0.2049(3) 0.2500(2) 0.0443(18) Uani 1 d . . C76 C 0.1412(8) -0.2539(9) 0.2834(7) 0.123(8) Uani 1 d . . H76A H 0.1263 -0.3001 0.2724 0.184 Uiso 1 calc . . H76B H 0.1343 -0.2412 0.3099 0.184 Uiso 1 calc . . H76C H 0.1784 -0.2553 0.2919 0.184 Uiso 1 calc . . O73 O 0.1501(3) -0.1224(3) 0.1916(2) 0.0354(15) Uani 1 d . . C74 C 0.1364(4) -0.0846(6) 0.1503(3) 0.044(3) Uani 1 d . . H74A H 0.1509 -0.1083 0.1311 0.066 Uiso 1 calc . . H74B H 0.1501 -0.0369 0.1568 0.066 Uiso 1 calc . . H74C H 0.0988 -0.0829 0.1346 0.066 Uiso 1 calc . . O45 O 0.0712(3) 0.0898(3) 0.0466(2) 0.0347(15) Uani 1 d . . C46 C 0.0695(7) 0.0176(7) 0.0419(5) 0.076(5) Uani 1 d . . H46A H 0.095 0.0027 0.0304 0.113 Uiso 1 calc . . H46B H 0.035 0.0034 0.0206 0.113 Uiso 1 calc . . H46C H 0.0771 -0.0043 0.0713 0.113 Uiso 1 calc . . O41 O -0.0223(3) 0.1574(3) 0.0034(2) 0.0339(15) Uani 1 d . . C42 C -0.0751(5) 0.1721(8) -0.0133(4) 0.073(5) Uani 1 d . . H42A H -0.0902 0.1676 -0.0463 0.11 Uiso 1 calc . . H42B H -0.0802 0.22 -0.005 0.11 Uiso 1 calc . . H42C H -0.0919 0.1389 -0.0004 0.11 Uiso 1 calc . . O43 O 0.0685(3) 0.2316(3) 0.0478(2) 0.0392(17) Uani 1 d . . C44 C 0.0955(7) 0.2899(7) 0.0715(5) 0.082(5) Uani 1 d . . H44A H 0.1094 0.3159 0.0528 0.123 Uiso 1 calc . . H44B H 0.1238 0.2746 0.0993 0.123 Uiso 1 calc . . H44C H 0.0721 0.3202 0.0791 0.123 Uiso 1 calc . . O3 O 0.1629(4) 0.1268(8) 0.0558(4) 0.109(5) Uani 1 d . . C3 C 0.2050(6) 0.1035(12) 0.0931(5) 0.109(7) Uani 1 d . . H3B H 0.2364 0.1253 0.0934 0.164 Uiso 1 calc . . H3C H 0.2077 0.0525 0.0916 0.164 Uiso 1 calc . . H3A H 0.2006 0.1164 0.1207 0.164 Uiso 1 calc . . O9 O 0.0423(6) 0.5674(7) 0.0644(5) 0.119(5) Uiso 1 d . . C9 C 0.0234(8) 0.6166(10) 0.0287(6) 0.109(6) Uiso 1 d . . H9A H -0.01 0.6345 0.0262 0.163 Uiso 1 calc . . H9B H 0.0194 0.5938 0.0003 0.163 Uiso 1 calc . . H9C H 0.0478 0.6556 0.0348 0.163 Uiso 1 calc . . O1 O 0.1152(5) 0.5904(6) 0.1502(4) 0.091(3) Uiso 1 d . . C1 C 0.1612(9) 0.6076(15) 0.1448(9) 0.165(11) Uiso 1 d . . H1C H 0.1596 0.6564 0.1349 0.247 Uiso 1 calc . . H1B H 0.165 0.5767 0.1221 0.247 Uiso 1 calc . . H1A H 0.1908 0.6016 0.1736 0.247 Uiso 1 calc . . O1S O -0.0598(6) -0.3531(7) 0.1438(5) 0.118(5) Uiso 1 d . . C1S C -0.0626(12) -0.3881(15) 0.1041(8) 0.163(10) Uiso 1 d . . O4 O 0.0853(6) -0.2872(8) 0.1778(5) 0.139(5) Uiso 1 d . . C4 C 0.0572(7) -0.2574(10) 0.1341(6) 0.106(6) Uiso 1 d . . H4B H 0.047 -0.2093 0.1375 0.159 Uiso 1 calc . . H4A H 0.0263 -0.2856 0.1179 0.159 Uiso 1 calc . . H4C H 0.079 -0.2569 0.117 0.159 Uiso 1 calc . . O2 O -0.1120(6) -0.4081(7) 0.1849(4) 0.107(4) Uiso 1 d . . C2 C -0.1630(8) -0.4038(15) 0.1556(8) 0.170(11) Uiso 1 d . . H2B H -0.1798 -0.4491 0.1544 0.255 Uiso 1 calc . . H2C H -0.1654 -0.3913 0.1255 0.255 Uiso 1 calc . . H2A H -0.1801 -0.3677 0.1663 0.255 Uiso 1 calc . . O10 O 0 -0.2240(15) 0.25 0.184(11) Uiso 1 d . . C10 C 0.0216(10) -0.2522(13) 0.2228(8) 0.057(6) Uiso 0.5 d . . H10C H 0.0533 -0.2771 0.2413 0.086 Uiso 0.5 calc . . H10B H 0.0297 -0.2146 0.206 0.086 Uiso 0.5 calc . . H10A H -0.0027 -0.285 0.2015 0.086 Uiso 0.5 calc . . O5 O 0.2367(6) 0.3113(9) 0.0878(5) 0.053(4) Uiso 0.5 d . . C5 C 0.2911(7) 0.3123(12) 0.1006(7) 0.043(5) Uiso 0.5 d . . H5B H 0.3067 0.3476 0.1242 0.065 Uiso 0.5 calc . . H5C H 0.2985 0.3238 0.0743 0.065 Uiso 0.5 calc . . H5A H 0.3054 0.2661 0.1122 0.065 Uiso 0.5 calc . . O2S O 0.1786(7) 0.2855(9) 0.0002(6) 0.061(5) Uiso 0.5 d . . C2S C 0.2011(13) 0.3273(15) -0.0230(11) 0.081(9) Uiso 0.5 d . . H2SB H 0.2008 0.3765 -0.0143 0.122 Uiso 0.5 calc . . H2SC H 0.1814 0.3224 -0.0556 0.122 Uiso 0.5 calc . . H2SA H 0.2367 0.3122 -0.0151 0.122 Uiso 0.5 calc . . O6 O -0.2429(8) 0.5052(11) 0.0005(7) 0.077(6) Uiso 0.5 d . . C6 C -0.2704(9) 0.4718(13) 0.0214(8) 0.055(6) Uiso 0.5 d . . H6C H -0.2517 0.4753 0.0542 0.082 Uiso 0.5 calc . . H6B H -0.2748 0.4223 0.0125 0.082 Uiso 0.5 calc . . H6A H -0.3042 0.4939 0.0124 0.082 Uiso 0.5 calc . . O7 O -0.3713(9) -0.0305(11) 0.0178(7) 0.081(6) Uiso 0.5 d . . C7 C -0.3572(16) 0.0256(16) 0.0461(11) 0.105(12) Uiso 0.5 d . . H7A H -0.3298 0.0117 0.0749 0.158 Uiso 0.5 calc . . H7B H -0.387 0.0423 0.0514 0.158 Uiso 0.5 calc . . H7C H -0.3447 0.0631 0.0324 0.158 Uiso 0.5 calc . . O8 O 0.0830(5) 0.2430(7) -0.0255(4) 0.032(3) Uiso 0.5 d . . C8 C 0.041(2) 0.286(4) -0.030(3) 0.28(4) Uiso 0.5 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 0.02567(19) 0.01810(17) 0.01274(15) 0.00265(11) 0.00424(13) 0.00397(12) W2 0.01404(16) 0.01733(16) 0.01912(16) 0.00160(11) 0.00904(13) 0.00124(11) W3 0.01831(17) 0.01734(16) 0.01217(14) -0.00292(10) 0.00594(12) 0.00107(11) Fe1 0.0124(7) 0.0131(7) 0.0101(6) 0 0.0051(6) 0 Fe2 0.0178(6) 0.0172(5) 0.0228(5) 0.0026(4) 0.0091(5) -0.0011(4) Fe5 0.0201(6) 0.0269(6) 0.0163(5) -0.0018(4) 0.0029(5) 0.0044(5) Fe3 0.0184(6) 0.0170(5) 0.0195(5) 0.0008(4) 0.0092(5) 0.0024(4) Fe4 0.0267(6) 0.0262(6) 0.0145(5) 0.0003(4) 0.0108(5) -0.0003(5) C16 0.095(11) 0.065(8) 0.026(5) 0.014(5) 0.019(6) 0.041(8) N16 0.135(13) 0.096(10) 0.073(8) 0.037(7) 0.059(8) 0.094(10) N28 0.033(5) 0.045(5) 0.046(5) 0.002(4) 0.010(4) -0.021(4) C18 0.043(6) 0.039(6) 0.033(5) 0.011(4) -0.003(5) -0.019(5) N18 0.085(9) 0.079(8) 0.052(6) 0.031(6) 0.007(6) -0.028(7) C17 0.020(4) 0.033(4) 0.009(3) 0.004(3) -0.003(3) 0.005(3) N17 0.036(5) 0.050(5) 0.026(4) 0.002(3) 0.007(4) 0.004(4) C11 0.018(4) 0.023(4) 0.018(4) 0.003(3) 0.005(3) 0.006(3) N11 0.021(3) 0.020(3) 0.018(3) 0.003(2) 0.008(3) 0.001(3) C13 0.025(4) 0.028(4) 0.024(4) 0.011(3) 0.017(4) 0.007(4) N13 0.018(4) 0.030(4) 0.021(3) 0.005(3) 0.008(3) -0.002(3) C15 0.019(4) 0.039(5) 0.021(4) 0.006(3) 0.004(3) 0.010(4) N15 0.018(4) 0.041(4) 0.019(3) 0.008(3) -0.001(3) -0.001(3) C12 0.023(4) 0.018(4) 0.022(4) 0.001(3) 0.008(3) -0.007(3) N12 0.023(4) 0.035(4) 0.025(4) -0.002(3) 0.007(3) 0.004(3) C14 0.020(4) 0.021(4) 0.013(3) 0.002(3) 0.004(3) 0.006(3) N14 0.032(4) 0.031(4) 0.018(3) 0.000(3) 0.009(3) -0.003(3) C28 0.023(4) 0.021(4) 0.033(4) 0.010(3) 0.011(4) 0.000(3) C26 0.030(5) 0.029(5) 0.050(6) 0.004(4) 0.029(5) -0.001(4) N26 0.042(6) 0.042(5) 0.091(8) 0.008(5) 0.042(6) 0.004(4) C27 0.026(5) 0.035(5) 0.034(5) 0.009(4) 0.017(4) 0.003(4) N27 0.047(6) 0.073(7) 0.046(5) 0.013(5) 0.033(5) -0.007(5) C21 0.021(4) 0.018(4) 0.014(3) -0.006(3) 0.011(3) 0.001(3) N21 0.024(4) 0.019(3) 0.014(3) 0.000(2) 0.006(3) 0.004(3) C22 0.019(4) 0.018(4) 0.021(4) 0.004(3) 0.008(3) -0.001(3) N22 0.025(4) 0.017(3) 0.033(4) 0.003(3) 0.012(3) -0.001(3) C25 0.015(4) 0.024(4) 0.017(4) 0.003(3) -0.001(3) -0.007(3) N25 0.021(4) 0.036(4) 0.020(3) -0.001(3) 0.005(3) -0.012(3) C23 0.017(4) 0.026(4) 0.018(4) -0.001(3) 0.006(3) 0.001(3) N23 0.026(4) 0.017(3) 0.026(3) 0.001(3) 0.013(3) 0.003(3) C24 0.020(4) 0.022(4) 0.022(4) 0.002(3) 0.017(3) 0.003(3) N24 0.026(4) 0.026(4) 0.021(4) -0.002(3) 0.012(3) -0.001(3) C36 0.045(6) 0.034(6) 0.028(5) -0.004(4) 0.022(4) -0.001(4) N36 0.112(10) 0.025(5) 0.066(6) -0.009(4) 0.057(7) -0.002(5) C38 0.027(5) 0.031(5) 0.024(4) 0.002(3) 0.015(4) 0.003(4) N38 0.053(5) 0.033(4) 0.029(4) -0.004(3) 0.027(4) 0.009(4) C37 0.025(5) 0.048(6) 0.028(5) -0.012(4) 0.003(4) 0.002(4) N37 0.046(6) 0.065(7) 0.037(5) -0.023(4) -0.002(4) 0.006(5) C31 0.018(4) 0.022(4) 0.013(3) -0.002(3) 0.004(3) -0.001(3) N31 0.023(4) 0.019(3) 0.018(3) 0.002(3) 0.008(3) 0.005(3) C33 0.023(4) 0.024(4) 0.019(4) -0.006(3) 0.011(3) 0.000(3) N33 0.026(4) 0.025(4) 0.027(4) -0.001(3) 0.014(3) 0.000(3) C35 0.031(5) 0.026(4) 0.014(4) -0.003(3) 0.005(3) 0.000(4) N35 0.030(4) 0.025(4) 0.027(4) -0.006(3) 0.000(3) 0.005(3) C32 0.020(4) 0.024(4) 0.018(4) -0.006(3) 0.014(3) -0.003(3) N32 0.021(4) 0.026(4) 0.029(4) -0.003(3) 0.010(3) 0.004(3) C34 0.026(4) 0.022(4) 0.014(3) -0.006(3) 0.007(3) -0.003(3) N34 0.027(4) 0.028(4) 0.020(3) -0.001(3) 0.011(3) 0.000(3) O63 0.026(4) 0.041(4) 0.038(4) -0.004(3) 0.011(3) -0.011(3) C64 0.038(7) 0.112(13) 0.098(12) -0.011(10) 0.022(8) -0.023(8) O61 0.034(4) 0.034(3) 0.038(3) 0.006(3) 0.026(3) 0.002(3) C62 0.054(8) 0.093(10) 0.045(7) 0.006(7) 0.025(6) -0.005(7) O65 0.052(5) 0.025(3) 0.050(4) 0.003(3) 0.024(4) 0.010(3) C66 0.095(15) 0.073(12) 0.156(19) -0.008(12) 0.047(14) 0.020(11) O55 0.034(4) 0.031(4) 0.061(5) 0.000(3) 0.015(4) 0.002(3) C56 0.104(14) 0.050(9) 0.110(13) 0.027(8) 0.025(11) -0.012(9) O53 0.032(4) 0.040(4) 0.020(3) -0.008(3) 0.001(3) 0.007(3) C54 0.084(14) 0.25(3) 0.068(11) 0.072(15) -0.001(10) 0.028(17) O51 0.049(5) 0.050(4) 0.027(3) -0.007(3) 0.011(3) 0.008(4) C52 0.180(18) 0.168(16) 0.081(11) 0.020(10) 0.054(12) -0.052(14) O71 0.024(3) 0.034(3) 0.032(3) 0.007(3) 0.008(3) 0.005(3) C72 0.034(6) 0.036(6) 0.061(7) -0.011(5) 0.021(5) -0.002(5) O75 0.058(5) 0.023(3) 0.050(4) 0.001(3) 0.019(4) -0.011(3) C76 0.110(17) 0.072(12) 0.148(18) 0.040(12) 0.013(14) 0.008(11) O73 0.045(4) 0.039(4) 0.029(3) 0.002(3) 0.022(3) 0.013(3) C74 0.046(6) 0.060(7) 0.035(5) 0.014(5) 0.026(5) 0.019(5) O45 0.041(4) 0.037(4) 0.034(3) -0.008(3) 0.024(3) 0.006(3) C46 0.107(13) 0.057(8) 0.098(11) 0.021(8) 0.078(10) 0.025(8) O41 0.031(4) 0.053(4) 0.020(3) -0.006(3) 0.012(3) 0.006(3) C42 0.057(8) 0.115(12) 0.041(7) -0.018(7) 0.012(6) 0.040(8) O43 0.059(5) 0.031(4) 0.036(4) -0.003(3) 0.028(3) -0.015(3) C44 0.136(16) 0.055(8) 0.067(9) -0.006(7) 0.055(10) -0.029(9) O3 0.061(7) 0.194(14) 0.082(8) -0.052(9) 0.041(6) -0.024(8) C3 0.051(9) 0.21(2) 0.066(10) -0.039(13) 0.019(8) -0.002(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C16 2.140(12) . ? W1 C15 2.149(10) . ? W1 C14 2.149(8) . ? W1 C11 2.152(7) . ? W1 C13 2.158(9) . ? W1 C12 2.162(8) . ? W1 C17 2.172(7) . ? W1 C18 2.183(10) . ? W2 C22 2.135(8) . ? W2 C25 2.142(8) . ? W2 C21 2.144(8) . ? W2 C26 2.149(9) . ? W2 C24 2.152(8) . ? W2 C28 2.161(9) . ? W2 C23 2.170(8) . ? W2 C27 2.207(9) . ? W3 C34 2.141(8) . ? W3 C32 2.144(8) . ? W3 C33 2.147(8) . ? W3 C31 2.156(7) . ? W3 C35 2.158(9) . ? W3 C37 2.160(9) . ? W3 C36 2.161(9) . ? W3 C38 2.206(8) . ? Fe1 N11 2.042(6) . ? Fe1 N11 2.042(6) 2 ? Fe1 N31 2.045(6) 2 ? Fe1 N31 2.045(6) . ? Fe1 N21 2.058(7) . ? Fe1 N21 2.058(7) 2 ? Fe2 O63 2.020(6) . ? Fe2 O65 2.027(7) . ? Fe2 N22 2.051(7) . ? Fe2 O61 2.055(6) . ? Fe2 N13 2.057(7) . ? Fe2 N12 2.058(7) 2 ? Fe5 N25 2.062(7) 2 ? Fe5 N35 2.069(8) . ? Fe5 O53 2.072(7) . ? Fe5 O55 2.087(7) . ? Fe5 O51 2.092(7) . ? Fe5 N15 2.094(8) . ? Fe3 N32 2.091(7) . ? Fe3 N33 2.095(7) 2 ? Fe3 O75 2.112(7) . ? Fe3 N23 2.125(7) . ? Fe3 O73 2.133(6) . ? Fe3 O71 2.146(6) . ? Fe4 N34 2.037(7) . ? Fe4 O43 2.038(6) . ? Fe4 O45 2.042(6) . ? Fe4 O41 2.049(6) . ? Fe4 N24 2.050(7) . ? Fe4 N14 2.052(8) . ? C16 N16 1.165(15) . ? N28 C28 1.161(11) . ? C18 N18 1.142(14) . ? C17 N17 1.151(11) . ? C11 N11 1.155(10) . ? C13 N13 1.133(11) . ? C15 N15 1.158(11) . ? C12 N12 1.141(10) . ? N12 Fe2 2.059(7) 2 ? C14 N14 1.134(10) . ? C26 N26 1.159(13) . ? C27 N27 1.110(12) . ? C21 N21 1.133(11) . ? C22 N22 1.146(10) . ? C25 N25 1.149(10) . ? N25 Fe5 2.063(7) 2 ? C23 N23 1.141(10) . ? C24 N24 1.131(11) . ? C36 N36 1.158(12) . ? C38 N38 1.117(11) . ? C37 N37 1.143(12) . ? C31 N31 1.130(10) . ? C33 N33 1.165(10) . ? N33 Fe3 2.095(7) 2 ? C35 N35 1.157(11) . ? C32 N32 1.160(10) . ? C34 N34 1.154(11) . ? O63 C64 1.511(17) . ? C64 H64A 0.98 . ? C64 H64B 0.98 . ? C64 H64C 0.98 . ? O61 C62 1.435(13) . ? C62 H62A 0.98 . ? C62 H62B 0.98 . ? C62 H62C 0.98 . ? O65 C66 1.501(19) . ? C66 H66A 0.98 . ? C66 H66B 0.98 . ? C66 H66C 0.98 . ? O55 C56 1.462(15) . ? C56 H56A 0.98 . ? C56 H56B 0.98 . ? C56 H56C 0.98 . ? O53 C54 1.59(3) . ? C54 H54A 0.98 . ? C54 H54B 0.98 . ? C54 H54C 0.98 . ? O51 C52 1.29(2) . ? O71 C72 1.405(12) . ? C72 H72A 0.98 . ? C72 H72B 0.98 . ? C72 H72C 0.98 . ? O75 C76 1.373(17) . ? C76 H76A 0.98 . ? C76 H76B 0.98 . ? C76 H76C 0.98 . ? O73 C74 1.428(11) . ? C74 H74A 0.98 . ? C74 H74B 0.98 . ? C74 H74C 0.98 . ? O45 C46 1.383(14) . ? C46 H46A 0.98 . ? C46 H46B 0.98 . ? C46 H46C 0.98 . ? O41 C42 1.402(14) . ? C42 H42A 0.98 . ? C42 H42B 0.98 . ? C42 H42C 0.98 . ? O43 C44 1.392(14) . ? C44 H44A 0.98 . ? C44 H44B 0.98 . ? C44 H44C 0.98 . ? O3 C3 1.385(14) . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? C3 H3A 0.98 . ? O9 C9 1.417(15) . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? O1 C1 1.423(16) . ? C1 H1C 0.98 . ? C1 H1B 0.98 . ? C1 H1A 0.98 . ? O1S C1S 1.420(17) . ? O4 C4 1.433(15) . ? C4 H4B 0.98 . ? C4 H4A 0.98 . ? C4 H4C 0.98 . ? O2 C2 1.375(16) . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C2 H2A 0.98 . ? O10 C10 1.368(16) 2 ? O10 C10 1.368(16) . ? C10 H10C 0.98 . ? C10 H10B 0.98 . ? C10 H10A 0.98 . ? O5 C5 1.426(16) . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C5 H5A 0.98 . ? O2S C2S 1.409(18) . ? C2S H2SB 0.98 . ? C2S H2SC 0.98 . ? C2S H2SA 0.98 . ? O6 C6 1.377(17) . ? C6 H6C 0.98 . ? C6 H6B 0.98 . ? C6 H6A 0.98 . ? O7 C7 1.358(18) . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? O8 C8 1.40(2) . ? 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 C16 W1 C15 85.5(5) . . ? C16 W1 C14 144.7(3) . . ? C15 W1 C14 95.7(3) . . ? C16 W1 C11 140.1(4) . . ? C15 W1 C11 73.7(3) . . ? C14 W1 C11 72.5(3) . . ? C16 W1 C13 113.6(5) . . ? C15 W1 C13 144.8(3) . . ? C14 W1 C13 85.1(3) . . ? C11 W1 C13 73.0(3) . . ? C16 W1 C12 71.0(4) . . ? C15 W1 C12 85.6(3) . . ? C14 W1 C12 144.3(3) . . ? C11 W1 C12 73.7(3) . . ? C13 W1 C12 74.3(3) . . ? C16 W1 C17 73.5(4) . . ? C15 W1 C17 73.2(3) . . ? C14 W1 C17 73.2(3) . . ? C11 W1 C17 128.8(3) . . ? C13 W1 C17 139.1(3) . . ? C12 W1 C17 139.7(3) . . ? C16 W1 C18 77.6(5) . . ? C15 W1 C18 146.7(3) . . ? C14 W1 C18 82.7(4) . . ? C11 W1 C18 135.5(4) . . ? C13 W1 C18 68.4(3) . . ? C12 W1 C18 114.8(4) . . ? C17 W1 C18 74.6(3) . . ? C22 W2 C25 96.3(3) . . ? C22 W2 C21 70.8(3) . . ? C25 W2 C21 74.5(3) . . ? C22 W2 C26 147.4(3) . . ? C25 W2 C26 92.5(3) . . ? C21 W2 C26 141.7(3) . . ? C22 W2 C24 89.4(3) . . ? C25 W2 C24 145.5(3) . . ? C21 W2 C24 75.4(3) . . ? C26 W2 C24 100.9(3) . . ? C22 W2 C28 75.4(3) . . ? C25 W2 C28 70.8(3) . . ? C21 W2 C28 127.6(3) . . ? C26 W2 C28 78.1(3) . . ? C24 W2 C28 142.9(3) . . ? C22 W2 C23 141.7(3) . . ? C25 W2 C23 76.6(3) . . ? C21 W2 C23 71.1(3) . . ? C26 W2 C23 70.9(3) . . ? C24 W2 C23 78.1(3) . . ? C28 W2 C23 133.3(3) . . ? C22 W2 C27 77.7(3) . . ? C25 W2 C27 141.9(3) . . ? C21 W2 C27 134.7(3) . . ? C26 W2 C27 76.1(3) . . ? C24 W2 C27 72.6(3) . . ? C28 W2 C27 71.2(3) . . ? C23 W2 C27 130.1(3) . . ? C34 W3 C32 92.8(3) . . ? C34 W3 C33 145.9(3) . . ? C32 W3 C33 90.5(3) . . ? C34 W3 C31 74.7(3) . . ? C32 W3 C31 70.9(3) . . ? C33 W3 C31 74.5(3) . . ? C34 W3 C35 80.9(3) . . ? C32 W3 C35 142.6(3) . . ? C33 W3 C35 76.1(3) . . ? C31 W3 C35 71.9(3) . . ? C34 W3 C37 94.1(4) . . ? C32 W3 C37 146.6(3) . . ? C33 W3 C37 101.5(4) . . ? C31 W3 C37 142.4(3) . . ? C35 W3 C37 70.8(3) . . ? C34 W3 C36 142.6(3) . . ? C32 W3 C36 78.6(3) . . ? C33 W3 C36 71.2(3) . . ? C31 W3 C36 133.2(3) . . ? C35 W3 C36 126.9(4) . . ? C37 W3 C36 76.1(4) . . ? C34 W3 C38 70.8(3) . . ? C32 W3 C38 76.0(3) . . ? C33 W3 C38 142.4(3) . . ? C31 W3 C38 130.1(3) . . ? C35 W3 C38 133.8(3) . . ? C37 W3 C38 75.5(3) . . ? C36 W3 C38 71.8(3) . . ? N11 Fe1 N11 95.5(4) . 2 ? N11 Fe1 N31 174.2(3) . 2 ? N11 Fe1 N31 88.8(3) 2 2 ? N11 Fe1 N31 88.8(3) . . ? N11 Fe1 N31 174.2(3) 2 . ? N31 Fe1 N31 87.1(4) 2 . ? N11 Fe1 N21 88.5(3) . . ? N11 Fe1 N21 85.9(3) 2 . ? N31 Fe1 N21 95.6(3) 2 . ? N31 Fe1 N21 90.4(3) . . ? N11 Fe1 N21 85.9(3) . 2 ? N11 Fe1 N21 88.5(3) 2 2 ? N31 Fe1 N21 90.4(3) 2 2 ? N31 Fe1 N21 95.6(3) . 2 ? N21 Fe1 N21 171.7(4) . 2 ? O63 Fe2 O65 85.0(3) . . ? O63 Fe2 N22 91.8(3) . . ? O65 Fe2 N22 175.0(3) . . ? O63 Fe2 O61 88.2(3) . . ? O65 Fe2 O61 86.1(3) . . ? N22 Fe2 O61 90.1(3) . . ? O63 Fe2 N13 175.2(3) . . ? O65 Fe2 N13 91.1(3) . . ? N22 Fe2 N13 92.0(3) . . ? O61 Fe2 N13 88.8(3) . . ? O63 Fe2 N12 87.7(3) . 2 ? O65 Fe2 N12 91.8(3) . 2 ? N22 Fe2 N12 91.8(3) . 2 ? O61 Fe2 N12 175.5(3) . 2 ? N13 Fe2 N12 95.2(3) . 2 ? N25 Fe5 N35 96.2(3) 2 . ? N25 Fe5 O53 89.4(3) 2 . ? N35 Fe5 O53 172.6(3) . . ? N25 Fe5 O55 89.1(3) 2 . ? N35 Fe5 O55 87.2(3) . . ? O53 Fe5 O55 88.1(3) . . ? N25 Fe5 O51 172.5(3) 2 . ? N35 Fe5 O51 88.6(3) . . ? O53 Fe5 O51 85.4(3) . . ? O55 Fe5 O51 85.3(3) . . ? N25 Fe5 N15 92.3(3) 2 . ? N35 Fe5 N15 91.6(3) . . ? O53 Fe5 N15 93.0(3) . . ? O55 Fe5 N15 178.3(3) . . ? O51 Fe5 N15 93.4(3) . . ? N32 Fe3 N33 94.5(3) . 2 ? N32 Fe3 O75 89.7(3) . . ? N33 Fe3 O75 91.7(3) 2 . ? N32 Fe3 N23 94.2(3) . . ? N33 Fe3 N23 95.7(3) 2 . ? O75 Fe3 N23 171.4(3) . . ? N32 Fe3 O73 88.4(3) . . ? N33 Fe3 O73 175.2(3) 2 . ? O75 Fe3 O73 84.4(3) . . ? N23 Fe3 O73 88.0(3) . . ? N32 Fe3 O71 173.1(3) . . ? N33 Fe3 O71 91.6(3) 2 . ? O75 Fe3 O71 87.0(3) . . ? N23 Fe3 O71 88.4(3) . . ? O73 Fe3 O71 85.3(3) . . ? N34 Fe4 O43 174.9(3) . . ? N34 Fe4 O45 94.3(3) . . ? O43 Fe4 O45 83.1(3) . . ? N34 Fe4 O41 89.7(3) . . ? O43 Fe4 O41 85.7(3) . . ? O45 Fe4 O41 85.2(3) . . ? N34 Fe4 N24 94.2(3) . . ? O43 Fe4 N24 90.1(3) . . ? O45 Fe4 N24 88.9(3) . . ? O41 Fe4 N24 173.1(3) . . ? N34 Fe4 N14 92.5(3) . . ? O43 Fe4 N14 89.9(3) . . ? O45 Fe4 N14 172.6(3) . . ? O41 Fe4 N14 91.8(3) . . ? N24 Fe4 N14 93.6(3) . . ? N16 C16 W1 176.1(15) . . ? N18 C18 W1 179.0(12) . . ? N17 C17 W1 177.5(9) . . ? N11 C11 W1 174.9(7) . . ? C11 N11 Fe1 176.5(7) . . ? N13 C13 W1 177.0(7) . . ? C13 N13 Fe2 173.8(7) . . ? N15 C15 W1 176.1(8) . . ? C15 N15 Fe5 168.6(7) . . ? N12 C12 W1 176.2(8) . . ? C12 N12 Fe2 177.2(7) . 2 ? N14 C14 W1 177.7(7) . . ? C14 N14 Fe4 174.5(7) . . ? N28 C28 W2 178.3(9) . . ? N26 C26 W2 179.0(11) . . ? N27 C27 W2 178.7(9) . . ? N21 C21 W2 177.8(7) . . ? C21 N21 Fe1 176.8(6) . . ? N22 C22 W2 178.1(7) . . ? C22 N22 Fe2 173.4(7) . . ? N25 C25 W2 175.4(8) . . ? C25 N25 Fe5 172.0(8) . 2 ? N23 C23 W2 176.3(7) . . ? C23 N23 Fe3 178.3(7) . . ? N24 C24 W2 175.6(7) . . ? C24 N24 Fe4 174.5(7) . . ? N36 C36 W3 178.8(12) . . ? N38 C38 W3 178.3(8) . . ? N37 C37 W3 177.9(10) . . ? N31 C31 W3 176.7(7) . . ? C31 N31 Fe1 179.4(7) . . ? N33 C33 W3 176.2(7) . . ? C33 N33 Fe3 170.3(7) . 2 ? N35 C35 W3 177.0(7) . . ? C35 N35 Fe5 174.0(8) . . ? N32 C32 W3 177.8(7) . . ? C32 N32 Fe3 170.3(7) . . ? N34 C34 W3 176.2(8) . . ? C34 N34 Fe4 173.5(7) . . ? C64 O63 Fe2 125.5(7) . . ? O63 C64 H64A 109.5 . . ? O63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? O63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C62 O61 Fe2 123.7(7) . . ? O61 C62 H62A 109.5 . . ? O61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? O61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C66 O65 Fe2 125.3(8) . . ? O65 C66 H66A 109.5 . . ? O65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? O65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C56 O55 Fe5 122.4(8) . . ? O55 C56 H56A 109.5 . . ? O55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? O55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C54 O53 Fe5 127.3(7) . . ? O53 C54 H54A 109.5 . . ? O53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? O53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C52 O51 Fe5 131.0(12) . . ? C72 O71 Fe3 124.4(6) . . ? O71 C72 H72A 109.5 . . ? O71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? O71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C76 O75 Fe3 133.3(10) . . ? O75 C76 H76A 109.5 . . ? O75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? O75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C74 O73 Fe3 126.4(6) . . ? O73 C74 H74A 109.5 . . ? O73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? O73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C46 O45 Fe4 132.4(7) . . ? O45 C46 H46A 109.5 . . ? O45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? O45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C42 O41 Fe4 128.9(6) . . ? O41 C42 H42A 109.5 . . ? O41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? O41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 O43 Fe4 127.7(7) . . ? O43 C44 H44A 109.5 . . ? O43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? O43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O3 C3 H3B 109.5 . . ? O3 C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O3 C3 H3A 109.5 . . ? H3B C3 H3A 109.5 . . ? H3C C3 H3A 109.5 . . ? O9 C9 H9A 109.5 . . ? O9 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O9 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O1 C1 H1C 109.5 . . ? O1 C1 H1B 109.5 . . ? H1C C1 H1B 109.5 . . ? O1 C1 H1A 109.5 . . ? H1C C1 H1A 109.5 . . ? H1B C1 H1A 109.5 . . ? O4 C4 H4B 109.5 . . ? O4 C4 H4A 109.5 . . ? H4B C4 H4A 109.5 . . ? O4 C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? O2 C2 H2B 109.5 . . ? O2 C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O2 C2 H2A 109.5 . . ? H2B C2 H2A 109.5 . . ? H2C C2 H2A 109.5 . . ? C10 O10 C10 134(3) 2 . ? O10 C10 H10C 109.5 . . ? O10 C10 H10B 109.5 . . ? H10C C10 H10B 109.5 . . ? O10 C10 H10A 109.5 . . ? H10C C10 H10A 109.5 . . ? H10B C10 H10A 109.5 . . ? O5 C5 H5B 109.5 . . ? O5 C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O5 C5 H5A 109.5 . . ? H5B C5 H5A 109.5 . . ? H5C C5 H5A 109.5 . . ? O2S C2S H2SB 109.5 . . ? O2S C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? O2S C2S H2SA 109.5 . . ? H2SB C2S H2SA 109.5 . . ? H2SC C2S H2SA 109.5 . . ? O6 C6 H6C 109.5 . . ? O6 C6 H6B 109.5 . . ? H6C C6 H6B 109.5 . . ? O6 C6 H6A 109.5 . . ? H6C C6 H6A 109.5 . . ? H6B C6 H6A 109.5 . . ? O7 C7 H7A 109.5 . . ? O7 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O7 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF _database_code_depnum_ccdc_archive 'CCDC 966456'