# 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_mer27squeeze-sr _audit_creation_date 2013-05-14 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:59:47, GUI svn.r4466) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C54 H60 Fe5 N12 O22, 5(Cl O4), 3(C2 H3 N), 4(H2 O)' _chemical_formula_sum 'C60 H77 Cl5 Fe5 N15 O46' _chemical_formula_weight 2200.82 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 16.2556(2) _cell_length_b 22.8571(4) _cell_length_c 25.5874(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.0441(15) _cell_angle_gamma 90.00 _cell_volume 9297.9(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 16167 _cell_measurement_temperature 120.02(10) _cell_measurement_theta_max 73.6676 _cell_measurement_theta_min 2.7772 _exptl_absorpt_coefficient_mu 8.284 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.50254 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 4364 _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_special_details ; Despite screening several crystals the diffraction at high angle was always weak. This is probably due to the disordered anions and solvent molecules present in the crystal lattice. ; _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_unetI/netI 0.0612 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 56674 _diffrn_reflns_theta_full 66.99 _diffrn_reflns_theta_max 66.99 _diffrn_reflns_theta_min 2.78 _diffrn_ambient_temperature 120.02(10) _diffrn_detector_area_resol_mean 10.6501 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -49.00 36.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - -39.9063 37.0000 150.0000 85 #__ type_ start__ end____ width___ exp.time_ 2 omega -114.00 -10.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - -39.9063 -57.0000 0.0000 104 #__ type_ start__ end____ width___ exp.time_ 3 omega 66.00 96.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 39.9063 -125.0000 90.0000 30 #__ type_ start__ end____ width___ exp.time_ 4 omega 35.00 62.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 39.9063 -125.0000 -150.0000 27 #__ type_ start__ end____ width___ exp.time_ 5 omega 32.00 88.00 1.0000 45.0000 omega____ theta____ kappa____ phi______ frames - 107.7801 -30.0000 -120.0000 56 #__ type_ start__ end____ width___ exp.time_ 6 omega 52.00 91.00 1.0000 45.0000 omega____ theta____ kappa____ phi______ frames - 107.7801 -35.0000 -79.0000 39 #__ type_ start__ end____ width___ exp.time_ 7 omega 85.00 141.00 1.0000 45.0000 omega____ theta____ kappa____ phi______ frames - 107.7801 45.0000 90.0000 56 #__ type_ start__ end____ width___ exp.time_ 8 omega 57.00 93.00 1.0000 45.0000 omega____ theta____ kappa____ phi______ frames - 107.7801 -45.0000 -30.0000 36 #__ type_ start__ end____ width___ exp.time_ 9 omega 37.00 105.00 1.0000 45.0000 omega____ theta____ kappa____ phi______ frames - 107.7801 -94.0000 -150.0000 68 #__ type_ start__ end____ width___ exp.time_ 10 omega 42.00 80.00 1.0000 45.0000 omega____ theta____ kappa____ phi______ frames - 107.7801 -30.0000 120.0000 38 #__ type_ start__ end____ width___ exp.time_ 11 omega 33.00 99.00 1.0000 45.0000 omega____ theta____ kappa____ phi______ frames - 107.7801 -45.0000 -180.0000 66 #__ type_ start__ end____ width___ exp.time_ 12 omega 79.00 169.00 1.0000 45.0000 omega____ theta____ kappa____ phi______ frames - 107.7801 30.0000 -180.0000 90 #__ type_ start__ end____ width___ exp.time_ 13 omega -119.00 -6.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - -39.9063 -77.0000 -180.0000 113 #__ type_ start__ end____ width___ exp.time_ 14 omega -114.00 -10.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - -39.9063 -57.0000 -120.0000 104 #__ type_ start__ end____ width___ exp.time_ 15 omega -49.00 36.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - -39.9063 37.0000 -60.0000 85 #__ type_ start__ end____ width___ exp.time_ 16 omega 77.00 168.00 1.0000 45.0000 omega____ theta____ kappa____ phi______ frames - 107.7801 30.0000 0.0000 91 #__ type_ start__ end____ width___ exp.time_ 17 omega 77.00 178.00 1.0000 45.0000 omega____ theta____ kappa____ phi______ frames - 107.7801 61.0000 -90.0000 101 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0042662000 _diffrn_orient_matrix_UB_12 -0.0302261000 _diffrn_orient_matrix_UB_13 0.0531886000 _diffrn_orient_matrix_UB_21 0.0968281000 _diffrn_orient_matrix_UB_22 -0.0005435000 _diffrn_orient_matrix_UB_23 0.0155422000 _diffrn_orient_matrix_UB_31 -0.0012794000 _diffrn_orient_matrix_UB_32 0.0602070000 _diffrn_orient_matrix_UB_33 0.0268362000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'SuperNova (Cu) X-ray Source' _reflns_number_gt 10965 _reflns_number_total 16567 _reflns_odcompleteness_completeness 99.91 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XLMP, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 1.402 _refine_diff_density_min -1.684 _refine_diff_density_rms 0.164 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.195 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 1199 _refine_ls_number_reflns 16567 _refine_ls_number_restraints 137 _refine_ls_R_factor_all 0.1325 _refine_ls_R_factor_gt 0.0998 _refine_ls_restrained_S_all 1.201 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3016 _refine_ls_wR_factor_ref 0.3250 _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. Despite varying the parameters of the absorption correction and the weighting scheme no significant improvement could be made to the final wR2 value. This high value is probably due to the weak high angle data caused by solvent/anion disorder and the presence of solvent accessible voids. All of the ClO4 anions were restrained (DFIX) to follow the tetrahedral geometry expected for ClO4 and five of them had their thermal parameters constrained to be roughly equal (EDAP). All MeCN solvent molecules were restrained (DFIX), while one MeCN solvent molecule also had its thermal parameters constrained to be roughly equal (EDAP). Two H2O molecules were also constrained using EDAP (O19 and O50). Three solvent water molecules (O19, O50 and O51) and two perchlorate anions (Cl3 and Cl7) were refined isotropically.Attempts were made to model the remaining residual electron density, however, no satisfactory model could be found and so the residual electron density was removed using the SQUEEZE protocol inside PLATON (128 electrons per unit cell). These were modelled as 4 MeCN and 4 H2O solvent molecules per unit cell and have been included in the molecular formula and molecular weight. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H,H) groups 2. Restrained distances O26-O27 = O26-O28 = O26-O29 = O27-O28 = O27-O29 = O28-O29 2.29 with sigma of 0.02 N15-C60 1.15 with sigma of 0.02 N25-C62 1.15 with sigma of 0.02 N19-C58 1.15 with sigma of 0.02 O46-O47 = O46-O48 = O46-O49 = O47-O48 = O47-O49 = O48-O49 2.29 with sigma of 0.02 C63-C62 1.45 with sigma of 0.02 C60-C61 1.45 with sigma of 0.02 C58-C59 1.45 with sigma of 0.02 H2BA-H64A 2 with sigma of 0.02 C28-C29 1.39 with sigma of 0.02 C29-C30 1.39 with sigma of 0.02 C30-C31 1.39 with sigma of 0.02 N7-C28 1.39 with sigma of 0.02 N7-C32 1.39 with sigma of 0.02 C32-C1B 1.39 with sigma of 0.02 C1B-C1A 1.39 with sigma of 0.02 C1A-C1D 1.39 with sigma of 0.02 C1D-C28 1.39 with sigma of 0.02 C31-C1C 1.39 with sigma of 0.02 C1C-N7 1.39 with sigma of 0.02 Cl10-O56 = Cl10-O53 = Cl10-O1F = Cl10-O1J 1.44 with sigma of 0.02 Cl4-O37 = Cl4-O35 = Cl4-O31 = Cl4-O32 = Cl4-O33 = Cl4-O30 = Cl4-O34 = Cl4-O36 1.44 with sigma of 0.02 Cl7-O46 = Cl7-O47 = Cl7-O48 = Cl7-O49 1.44 with sigma of 0.02 Cl7-O48 = Cl7-O46 = Cl7-O49 = Cl7-O47 1.44 with sigma of 0.02 Cl3-O26 = Cl3-O27 = Cl3-O28 = Cl3-O29 1.44 with sigma of 0.02 Cl3-O26 = Cl3-O27 = Cl3-O29 = Cl3-O28 1.44 with sigma of 0.02 Cl2-O22 = Cl2-O23 = Cl2-O20 = Cl2-O21 1.44 with sigma of 0.02 Cl1-O22 = Cl1-O23 = Cl1-O24 = Cl1-O25 1.44 with sigma of 0.02 Cl9-O1D 1.44 with sigma of 0.02 Cl9-O24 1.44 with sigma of 0.02 Cl9-O22 = Cl9-O1C 1.44 with sigma of 0.02 Cl6-O45 = Cl6-O42 = Cl6-O44 = Cl6-O43 1.44 with sigma of 0.02 Cl8-O54 = Cl8-O55 = Cl8-O1H = Cl8-O1I 1.44 with sigma of 0.02 Cl5-O41 = Cl5-O39 = Cl5-O38 = Cl5-O40 1.44 with sigma of 0.02 O22-O1C 2.3 with sigma of 0.04 3. Uiso/Uaniso restraints and constraints C30 \\sim C29: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0. Cl1 \\sim O24 \\sim O22 \\sim O25 \\sim O23: within 1.7A with sigma of 0.04 and Cl6 \\sim O45 \\sim O44 \\sim O42 \\sim O43: within 1.7A with sigma of 0.04 and Uanis(O34) = Uanis(O35) Uanis(O31) = Uanis(O30) Uanis(O32) = Uanis(O33) Uanis(O36) = Uanis(O37) Uiso(N25) = Uiso(C62) = Uiso(C63) Uanis(N14) = Uanis(C1C) Uanis(Cl10) = Uanis(O1F) = Uanis(O53) = Uanis(O56) = Uanis(O1J) Uiso(O48) = Uiso(Cl7) = Uiso(O47) = Uiso(O49) = Uiso(O46) Uiso(O27) = Uiso(O26) = Uiso(O28) = Uiso(Cl3) = Uiso(O29) Uanis(Cl1) = Uanis(O22) = Uanis(O24) = Uanis(O25) = Uanis(Cl2) = Uanis(Cl9) = Ua Uanis(O45) = Uanis(Cl6) = Uanis(O44) = Uanis(O42) = Uanis(O43) Uanis(Cl8) = Uanis(O1I) = Uanis(O1H) = Uanis(O54) = Uanis(O55) 4. Others Fixed Sof: O37(0.25) N8(0.6) H8(0.6) O35(0.75) O31(0.75) C32(0.6) O54(0.5) H28A(0.5) H28(0.5) O55(0.5) C31(0.4) H31(0.4) Cl5(0.5) O41(0.5) O39(0.5) O38(0.5) O40(0.5) Cl1(0.4) O23(0.8) O24(0.6) Cl6(0.5) O45(0.5) Cl2(0.4) N13(0.5) C65(0.5) C64(0.5) H64A(0.5) H64B(0.5) H64C(0.5) N15(0.5) C60(0.5) C61(0.5) H61A(0.5) H61B(0.5) H61C(0.5) N19(0.5) C58(0.5) C59(0.5) H59A(0.5) H59B(0.5) H59C(0.5) O25(0.4) O20(0.4) O21(0.4) C29(0.4) H29(0.4) C30(0.4) H30(0.4) O32(0.75) O42(0.5) O56(0.5) Cl8(0.5) O33(0.25) O30(0.25) O34(0.25) O36(0.75) O53(0.5) O50(0.5) Cl3(0.5) O48(0.5) Cl7(0.5) O46(0.5) O26(0.5) O49(0.5) O27(0.5) O29(0.5) O44(0.5) O43(0.5) O47(0.5) N25(0.5) C62(0.5) C63(0.5) H63A(0.5) H63B(0.5) H63C(0.5) O28(0.5) C1A(0.6) H1A(0.6) C1B(0.6) H1B(0.6) C1C(0.4) C1D(0.6) H1D(0.6) N14(0.4) H14(0.4) Cl9(0.2) O1C(0.2) O1D(0.2) O1E(0.5) H1EA(0.5) H1EB(0.5) O1F(0.5) Cl10(0.5) O1H(0.5) O1I(0.5) O1J(0.5) Fixed Uiso: Cl3(0.12) O48(0.12) Cl7(0.12) O46(0.12) O26(0.12) O49(0.12) O27(0.12) O29(0.12) O47(0.12) O28(0.12) 5.a Riding coordinates: N14(H14) 5.b Free rotating group: O52(H52C,H52D), O51(H51A,H51B), O1E(H1EA,H1EB) 5.c Rotating group: O1B(H1BA,H1BB), O3B(H3BA,H3BB), O2B(H2BA,H2BB) 5.d Secondary CH2 refined with riding coordinates: C26(H26A,H26B), C17(H17A,H17B), C8(H8A,H8B), C7(H7A,H7B), C44(H44A,H44B), C43(H43A,H43B), C16(H16A,H16B), C52(H52A,H52B), C53(H53A,H53B), C25(H25A,H25B), C34(H34A,H34B), C35(H35A,H35B) 5.e Aromatic/amide H refined with riding coordinates: N10(H10), N6(H6), N4(H4), N2(H2), N12(H12), N8(H8), C40(H40), C19(H19), C21(H21), C1(H1), C22(H22), C38(H38), C37(H37), C2(H2A), C4(H4A), C20(H20), C49(H49), C39(H39), C13(H13), C3(H3), C48(H48), C12(H12A), C46(H46), C11(H11), C10(H10A), C28(H28A), C28(H28), C47(H47), C31(H31), C29(H29), C30(H30), C1A(H1A), C1B(H1B), C1D(H1D) 5.f Idealised Me refined as rotating group: C64(H64A,H64B,H64C), C61(H61A,H61B,H61C), C59(H59A,H59B,H59C), C63(H63A,H63B, H63C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.78987(2) 0.434711(14) 0.430920(13) 0.02373(8) Uani 1 1 d . . . Fe2 Fe 0.67221(2) 0.437500(14) 0.309588(13) 0.02567(9) Uani 1 1 d . . . Fe3 Fe 0.87945(2) 0.440972(14) 0.327900(13) 0.02532(9) Uani 1 1 d . . . Fe4 Fe 0.75506(2) 0.690247(16) 0.331479(14) 0.03595(10) Uani 1 1 d . . . Fe5 Fe 0.77740(3) 0.185992(18) 0.323089(17) 0.04546(12) Uani 1 1 d . B . O1A O 0.77965(8) 0.43763(6) 0.35552(6) 0.0257(4) Uani 1 1 d . . . O3 O 0.83709(9) 0.49926(7) 0.27009(6) 0.0352(5) Uani 1 1 d . . . O15 O 0.84527(9) 0.37876(7) 0.27239(6) 0.0358(5) Uani 1 1 d . . . O1B O 0.55581(10) 0.43919(7) 0.25665(7) 0.0376(5) Uani 1 1 d . . . H1BA H 0.5230 0.4089 0.2612 0.056 Uiso 1 1 d R . . H1BB H 0.5621 0.4369 0.2228 0.056 Uiso 1 1 d R . . O2 O 0.69691(10) 0.50143(7) 0.26148(6) 0.0350(5) Uani 1 1 d . . . O3B O 0.98977(9) 0.44604(6) 0.29887(6) 0.0316(4) Uani 1 1 d . . . H3BA H 0.9844 0.4265 0.2699 0.047 Uiso 1 1 d R . . H3BB H 1.0303 0.4325 0.3224 0.047 Uiso 1 1 d R . . O12 O 0.69728(10) 0.37674(7) 0.42947(6) 0.0380(5) Uani 1 1 d . . . O2B O 0.80103(9) 0.43176(7) 0.51364(6) 0.0323(4) Uani 1 1 d . . . H2BA H 0.7756 0.4009 0.5233 0.048 Uiso 1 1 d RD . . H2BB H 0.7781 0.4629 0.5247 0.048 Uiso 1 1 d R . . O6 O 0.70920(10) 0.50168(7) 0.43155(6) 0.0369(5) Uani 1 1 d . . . O7 O 0.86012(10) 0.64027(7) 0.36834(6) 0.0336(4) Uani 1 1 d . . . O8 O 0.92870(9) 0.51061(7) 0.37391(6) 0.0308(4) Uani 1 1 d . . . O18 O 0.87031(10) 0.36733(7) 0.44274(6) 0.0362(5) Uani 1 1 d . . . O5 O 0.62038(9) 0.49579(7) 0.35265(6) 0.0333(4) Uani 1 1 d . . . O17 O 0.94064(9) 0.37975(7) 0.37780(6) 0.0331(4) Uani 1 1 d . . . O1 O 0.72670(11) 0.63261(7) 0.26784(6) 0.0397(5) Uani 1 1 d . . . O4 O 0.68329(10) 0.64898(7) 0.37917(6) 0.0362(5) Uani 1 1 d . . . O9 O 0.88429(10) 0.49072(7) 0.44836(6) 0.0342(4) Uani 1 1 d . . . N10 N 0.98984(12) 0.19059(9) 0.33697(8) 0.0406(6) Uani 1 1 d . . . H10 H 1.0431 0.1861 0.3484 0.049 Uiso 1 1 calc R . . O11 O 0.62360(10) 0.37218(7) 0.34598(6) 0.0367(5) Uani 1 1 d . . . O13 O 0.74208(11) 0.24579(8) 0.26228(7) 0.0476(5) Uani 1 1 d . . . O14 O 0.70447(9) 0.38003(7) 0.25699(6) 0.0341(4) Uani 1 1 d . . . O16 O 0.87863(10) 0.24074(7) 0.35663(7) 0.0451(5) Uani 1 1 d . . . O10 O 0.70051(11) 0.22431(7) 0.36964(7) 0.0438(5) Uani 1 1 d . B . N6 N 0.96686(14) 0.69428(9) 0.34737(8) 0.0424(6) Uani 1 1 d . . . H6 H 1.0195 0.7013 0.3588 0.051 Uiso 1 1 calc R . . C18 C 0.64511(13) 0.51669(9) 0.39848(8) 0.0273(6) Uani 1 1 d . . . C26 C 0.96561(14) 0.57545(9) 0.44826(8) 0.0293(6) Uani 1 1 d . . . H26A H 1.0109 0.5625 0.4769 0.035 Uiso 1 1 calc R . . H26B H 0.9258 0.5968 0.4644 0.035 Uiso 1 1 calc R . . N1 N 0.64088(13) 0.73445(9) 0.28967(8) 0.0430(6) Uani 1 1 d . . . N3 N 0.78943(13) 0.75018(9) 0.40077(9) 0.0442(6) Uani 1 1 d . . . C27 C 0.92223(13) 0.52247(9) 0.42127(8) 0.0252(5) Uani 1 1 d . . . N5 N 0.84554(14) 0.72976(9) 0.28856(8) 0.0392(6) Uani 1 1 d . . . C15 C 0.68812(14) 0.64954(10) 0.42737(9) 0.0333(6) Uani 1 1 d . . . C17 C 0.59068(13) 0.56343(10) 0.41728(9) 0.0314(6) Uani 1 1 d . . . H17A H 0.5585 0.5835 0.3863 0.038 Uiso 1 1 calc R . . H17B H 0.5511 0.5444 0.4353 0.038 Uiso 1 1 calc R . . C8 C 0.75729(15) 0.55126(11) 0.19695(8) 0.0351(7) Uani 1 1 d . . . H8A H 0.7595 0.5254 0.1672 0.042 Uiso 1 1 calc R . . H8B H 0.8054 0.5772 0.2015 0.042 Uiso 1 1 calc R . . N9 N 0.86878(14) 0.14840(9) 0.27942(9) 0.0475(7) Uani 1 1 d . . . C54 C 0.77228(14) 0.36451(10) 0.24608(8) 0.0298(6) Uani 1 1 d . . . N4 N 0.73526(13) 0.68844(10) 0.46113(8) 0.0440(6) Uani 1 1 d . . . H4 H 0.7385 0.6812 0.4945 0.053 Uiso 1 1 calc R . . N11 N 0.66700(15) 0.13849(9) 0.28028(10) 0.0542(7) Uani 1 1 d . . . C45 C 0.92522(13) 0.35289(9) 0.41818(8) 0.0273(6) Uani 1 1 d . . . C7 C 0.67717(16) 0.58756(12) 0.18347(10) 0.0426(7) Uani 1 1 d . . . H7A H 0.6744 0.6070 0.1495 0.051 Uiso 1 1 calc R . . H7B H 0.6288 0.5619 0.1799 0.051 Uiso 1 1 calc R . . C9 C 0.76358(15) 0.51513(10) 0.24682(9) 0.0331(6) Uani 1 1 d . . . C14 C 0.77941(15) 0.73830(12) 0.45077(9) 0.0404(7) Uani 1 1 d . . . C36 C 0.64208(13) 0.35479(10) 0.39354(9) 0.0313(6) Uani 1 1 d . B . C44 C 0.98073(14) 0.30243(10) 0.44026(9) 0.0328(6) Uani 1 1 d . . . H44A H 0.9481 0.2749 0.4565 0.039 Uiso 1 1 calc R . . H44B H 1.0259 0.3169 0.4682 0.039 Uiso 1 1 calc R . . N2 N 0.61040(14) 0.67196(10) 0.21487(9) 0.0530(7) Uani 1 1 d . . . H2 H 0.5769 0.6670 0.1844 0.064 Uiso 1 1 calc R . . C43 C 1.01858(15) 0.27042(11) 0.39961(11) 0.0448(7) Uani 1 1 d . . . H43A H 1.0643 0.2460 0.4181 0.054 Uiso 1 1 calc R . . H43B H 1.0420 0.2987 0.3785 0.054 Uiso 1 1 calc R . . C24 C 0.93616(15) 0.65089(10) 0.37450(9) 0.0333(6) Uani 1 1 d . . . O37 O 0.2461(3) 0.4560(3) 0.4354(3) 0.0486(7) Uani 0.25 1 d PD A 2 C16 C 0.63986(14) 0.60791(10) 0.45437(9) 0.0318(6) Uani 1 1 d . . . H16A H 0.6013 0.6300 0.4711 0.038 Uiso 1 1 calc R . . H16B H 0.6788 0.5876 0.4824 0.038 Uiso 1 1 calc R . . C6 C 0.67381(16) 0.63275(11) 0.22599(9) 0.0379(7) Uani 1 1 d . . . C51 C 0.69259(15) 0.24378(11) 0.21917(11) 0.0419(7) Uani 1 1 d . . . C52 C 0.69212(15) 0.29288(11) 0.17941(10) 0.0435(7) Uani 1 1 d . . . H52A H 0.6419 0.3164 0.1777 0.052 Uiso 1 1 calc R . . H52B H 0.6900 0.2763 0.1443 0.052 Uiso 1 1 calc R . . C42 C 0.95452(15) 0.23200(10) 0.36207(10) 0.0394(7) Uani 1 1 d . . . C53 C 0.77018(16) 0.33245(12) 0.19438(10) 0.0446(8) Uani 1 1 d . . . H53A H 0.8205 0.3087 0.1977 0.054 Uiso 1 1 calc R . . H53B H 0.7700 0.3606 0.1660 0.054 Uiso 1 1 calc R . . N12 N 0.63620(14) 0.20061(10) 0.20483(10) 0.0544(7) Uani 1 1 d . . . H12 H 0.6079 0.2026 0.1725 0.065 Uiso 1 1 calc R . . C41 C 0.95351(16) 0.15354(11) 0.29507(10) 0.0406(7) Uani 1 1 d . . . N8 N 0.7574(2) 0.18997(13) 0.45458(12) 0.0366(10) Uani 0.60 1 d P B 1 H8 H 0.7569 0.1969 0.4875 0.044 Uiso 0.60 1 calc PR B 1 C33 C 0.7076(2) 0.22533(12) 0.41971(11) 0.0569(9) Uani 1 1 d . . . C40 C 1.00776(17) 0.12174(10) 0.26935(11) 0.0442(8) Uani 1 1 d . . . H40 H 1.0657 0.1254 0.2809 0.053 Uiso 1 1 calc R . . O35 O 0.12011(15) 0.48410(10) 0.41814(10) 0.0512(7) Uani 0.75 1 d PD A 1 C25 C 1.00161(14) 0.61691(9) 0.41344(9) 0.0324(6) Uani 1 1 d . . . H25A H 1.0358 0.5949 0.3935 0.039 Uiso 1 1 calc R . . H25B H 1.0383 0.6444 0.4361 0.039 Uiso 1 1 calc R . . C23 C 0.92888(16) 0.72936(10) 0.30473(9) 0.0372(7) Uani 1 1 d . . . C34 C 0.64899(19) 0.25946(11) 0.44624(10) 0.0471(8) Uani 1 1 d . B . H34A H 0.6818 0.2805 0.4765 0.056 Uiso 1 1 calc R . . H34B H 0.6127 0.2323 0.4599 0.056 Uiso 1 1 calc R . . N7 N 0.81929(16) 0.12991(10) 0.39425(9) 0.0586(8) Uani 1 1 d D . . C19 C 0.81407(18) 0.76278(11) 0.24483(10) 0.0470(8) Uani 1 1 d . . . H19 H 0.7562 0.7622 0.2320 0.056 Uiso 1 1 calc R . . C21 C 0.9446(2) 0.79773(12) 0.23822(11) 0.0580(10) Uani 1 1 d . . . H21 H 0.9782 0.8224 0.2227 0.070 Uiso 1 1 calc R . . C35 C 0.59431(14) 0.30315(10) 0.40927(9) 0.0338(6) Uani 1 1 d . . . H35A H 0.5666 0.2829 0.3771 0.041 Uiso 1 1 calc R B . H35B H 0.5510 0.3176 0.4269 0.041 Uiso 1 1 calc R . . C1 C 0.6151(2) 0.77885(13) 0.31731(13) 0.0602(10) Uani 1 1 d . . . H1 H 0.6485 0.7896 0.3500 0.072 Uiso 1 1 calc R . . C22 C 0.97980(19) 0.76345(11) 0.27998(11) 0.0533(8) Uani 1 1 d . . . H22 H 1.0379 0.7628 0.2920 0.064 Uiso 1 1 calc R . . C38 C 0.8906(2) 0.08179(12) 0.21033(11) 0.0560(9) Uani 1 1 d . . . H38 H 0.8668 0.0595 0.1806 0.067 Uiso 1 1 calc R . . O31 O 0.15156(15) 0.38732(11) 0.45189(9) 0.0522(8) Uani 0.75 1 d PD A 1 C32 C 0.8109(3) 0.14293(17) 0.44638(12) 0.0414(12) Uani 0.60 1 d PD B 1 C5 C 0.59003(17) 0.71887(11) 0.24424(10) 0.0465(8) Uani 1 1 d . . . C37 C 0.84044(19) 0.11241(12) 0.23876(12) 0.0556(9) Uani 1 1 d . . . H37 H 0.7825 0.1074 0.2286 0.067 Uiso 1 1 calc R . . C2 C 0.5400(2) 0.80923(14) 0.29857(13) 0.0634(10) Uani 1 1 d . . . H2A H 0.5257 0.8410 0.3175 0.076 Uiso 1 1 calc R . . C4 C 0.51237(18) 0.74465(12) 0.22543(12) 0.0521(9) Uani 1 1 d . . . H4A H 0.4769 0.7302 0.1949 0.063 Uiso 1 1 calc R . . C20 C 0.86013(19) 0.79612(12) 0.21890(11) 0.0507(9) Uani 1 1 d . . . H20 H 0.8353 0.8174 0.1888 0.061 Uiso 1 1 calc R . . C49 C 0.54135(19) 0.12445(12) 0.21384(13) 0.0603(10) Uani 1 1 d . . . H49 H 0.5070 0.1372 0.1821 0.072 Uiso 1 1 calc R . . C39 C 0.9756(2) 0.08531(12) 0.22730(11) 0.0513(9) Uani 1 1 d . . . H39 H 1.0112 0.0635 0.2108 0.062 Uiso 1 1 calc R . . C13 C 0.81210(17) 0.77374(13) 0.49430(12) 0.0538(9) Uani 1 1 d . . . H13 H 0.8048 0.7639 0.5283 0.065 Uiso 1 1 calc R . . C3 C 0.48783(19) 0.79180(13) 0.25219(12) 0.0633(9) Uani 1 1 d . . . H3 H 0.4374 0.8111 0.2391 0.076 Uiso 1 1 calc R . . C48 C 0.5169(2) 0.07745(14) 0.23982(15) 0.0744(12) Uani 1 1 d . . . H48 H 0.4674 0.0573 0.2260 0.089 Uiso 1 1 calc R . . C12 C 0.8547(2) 0.82287(15) 0.48653(14) 0.0669(11) Uani 1 1 d . . . H12A H 0.8760 0.8477 0.5149 0.080 Uiso 1 1 calc R . . O54 O 0.8190(3) 0.3097(2) 0.54134(16) 0.1048(6) Uani 0.50 1 d PD C 2 C46 C 0.6430(2) 0.09274(14) 0.30704(14) 0.0753(12) Uani 1 1 d . . . H46 H 0.6768 0.0820 0.3396 0.090 Uiso 1 1 calc R . . C50 C 0.61659(18) 0.15379(11) 0.23378(11) 0.0505(8) Uani 1 1 d . . . C11 C 0.8662(2) 0.83557(14) 0.43498(13) 0.0702(10) Uani 1 1 d . . . H11 H 0.8970 0.8682 0.4286 0.084 Uiso 1 1 calc R . . C10 C 0.8309(2) 0.79858(13) 0.39407(14) 0.0616(10) Uani 1 1 d . . . H10A H 0.8364 0.8081 0.3596 0.074 Uiso 1 1 calc R . . C28 C 0.8695(2) 0.08454(12) 0.38925(12) 0.0687(11) Uani 1 1 d D B . H28A H 0.8532 0.0628 0.3581 0.082 Uiso 0.50 1 calc PR D 2 H28 H 0.8749 0.0722 0.3555 0.082 Uiso 0.50 1 calc PR D 1 C47 C 0.5692(3) 0.06079(14) 0.28786(18) 0.0859(15) Uani 1 1 d . . . H47 H 0.5553 0.0290 0.3069 0.103 Uiso 1 1 calc R . . O55 O 0.9069(3) 0.2543(3) 0.56559(17) 0.1048(6) Uani 0.50 1 d PD C 2 C31 C 0.9010(3) 0.1383(2) 0.4780(2) 0.051(2) Uani 0.40 1 d PD B 2 H31 H 0.9121 0.1575 0.5108 0.062 Uiso 0.40 1 calc PR B 2 Cl5 Cl 0.34626(6) 0.26876(5) 0.40711(4) 0.0365(3) Uani 0.50 1 d PD E 1 O41 O 0.3309(2) 0.20725(14) 0.40729(17) 0.0561(13) Uani 0.50 1 d PD E 1 O39 O 0.3636(2) 0.28941(19) 0.35831(12) 0.0594(12) Uani 0.50 1 d PD E 1 O38 O 0.27206(19) 0.29601(15) 0.41674(12) 0.0403(10) Uani 0.50 1 d PD E 1 O40 O 0.4139(2) 0.28273(19) 0.45196(14) 0.0594(13) Uani 0.50 1 d PD E 1 Cl1 Cl 0.03033(17) 0.94443(10) 0.34953(8) 0.0891(4) Uani 0.40 1 d PDU F 2 O22 O -0.00156(18) 0.93094(11) 0.39228(8) 0.0891(4) Uani 1 1 d DU . . O23 O 0.0281(2) 0.90843(15) 0.30479(10) 0.0891(4) Uani 0.80 1 d PDU F 1 O24 O 0.1224(2) 0.94420(18) 0.37069(15) 0.0891(4) Uani 0.60 1 d PDU F 2 Cl6 Cl 0.48938(13) 0.24627(10) 0.56008(9) 0.1034(7) Uani 0.50 1 d PDU G 2 O45 O 0.5399(3) 0.2836(2) 0.5962(2) 0.1034(7) Uani 0.50 1 d PDU G 2 Cl2 Cl -0.02417(17) 0.93121(10) 0.33712(8) 0.0891(4) Uani 0.40 1 d PD F 1 N13 N 0.6760(3) 0.4327(2) 0.6422(2) 0.0625(14) Uiso 0.50 1 d P H 2 C65 C 0.6498(3) 0.4190(2) 0.5976(2) 0.0463(12) Uiso 0.50 1 d P H 2 C64 C 0.6123(3) 0.4094(3) 0.5392(2) 0.0595(15) Uiso 0.50 1 d P H 2 H64A H 0.6535 0.4181 0.5185 0.089 Uiso 0.50 1 calc PRD H 2 H64B H 0.5645 0.4346 0.5285 0.089 Uiso 0.50 1 calc PR H 2 H64C H 0.5949 0.3694 0.5336 0.089 Uiso 0.50 1 calc PR H 2 N15 N 0.3888(3) 0.4250(3) 0.2649(3) 0.0820(18) Uiso 0.50 1 d PD I 2 C60 C 0.3186(2) 0.4333(3) 0.2646(3) 0.074(2) Uiso 0.50 1 d PD I 2 C61 C 0.2347(3) 0.4444(4) 0.2717(3) 0.096(3) Uiso 0.50 1 d PD I 2 H61A H 0.1977 0.4488 0.2374 0.144 Uiso 0.50 1 calc PR I 2 H61B H 0.2341 0.4796 0.2921 0.144 Uiso 0.50 1 calc PR I 2 H61C H 0.2161 0.4121 0.2903 0.144 Uiso 0.50 1 calc PR I 2 N19 N 0.4241(4) 0.4313(3) 0.3750(2) 0.091(2) Uiso 0.50 1 d PD J 1 C58 C 0.4520(5) 0.4354(4) 0.41860(18) 0.095(3) Uiso 0.50 1 d PD J 1 C59 C 0.5037(6) 0.4301(5) 0.4708(3) 0.140(5) Uiso 0.50 1 d PD J 1 H59A H 0.5530 0.4076 0.4689 0.211 Uiso 0.50 1 calc PR J 1 H59B H 0.4728 0.4107 0.4939 0.211 Uiso 0.50 1 calc PR J 1 H59C H 0.5202 0.4683 0.4847 0.211 Uiso 0.50 1 calc PR J 1 O25 O 0.0135(5) 1.0039(2) 0.3365(2) 0.0891(4) Uani 0.40 1 d PDU F 2 O20 O -0.0925(3) 0.8917(3) 0.3271(2) 0.0891(4) Uani 0.40 1 d PD F 1 O21 O -0.0596(4) 0.9857(2) 0.3172(2) 0.0891(4) Uani 0.40 1 d PD F 1 C29 C 0.9409(4) 0.0654(3) 0.4230(2) 0.075(3) Uani 0.40 1 d PDU B 2 H29 H 0.9787 0.0393 0.4132 0.090 Uiso 0.40 1 calc PR B 2 C30 C 0.9505(3) 0.0895(2) 0.4738(2) 0.066(2) Uani 0.40 1 d PDU B 2 H30 H 0.9875 0.0739 0.5032 0.079 Uiso 0.40 1 calc PR B 2 Cl4 Cl 0.16667(4) 0.42862(3) 0.41449(2) 0.04108(16) Uani 1 1 d D . . O32 O 0.13577(15) 0.40560(11) 0.36116(9) 0.0517(6) Uani 0.75 1 d PD A 1 O42 O 0.5445(3) 0.2026(2) 0.5517(2) 0.1034(7) Uani 0.50 1 d PDU G 2 O56 O 0.8481(3) 0.27961(13) 0.63397(12) 0.0479(3) Uani 0.50 1 d PD K 1 Cl8 Cl 0.82531(12) 0.26328(10) 0.58058(6) 0.1048(6) Uani 0.50 1 d PD C 2 O33 O 0.1503(5) 0.4156(3) 0.35802(19) 0.0517(6) Uani 0.25 1 d PD A 2 O30 O 0.1968(4) 0.3696(2) 0.4310(3) 0.0522(8) Uani 0.25 1 d PD A 2 O34 O 0.1018(3) 0.4666(3) 0.4265(3) 0.0512(7) Uani 0.25 1 d PD A 2 O36 O 0.25404(14) 0.44381(11) 0.42194(10) 0.0486(7) Uani 0.75 1 d PD A 1 O53 O 0.7687(2) 0.22035(12) 0.56789(13) 0.0479(3) Uani 0.50 1 d PD K 1 O50 O 0.3241(4) 0.4664(3) 0.0667(2) 0.1001(18) Uiso 0.50 1 d P L 1 O52 O 0.83875(13) 0.83403(10) 0.62794(9) 0.0675(7) Uani 1 1 d G . . H52C H 0.8545 0.8546 0.6041 0.101 Uiso 1 1 d G . . H52D H 0.7979 0.8125 0.6136 0.101 Uiso 1 1 d G . . Cl3 Cl 0.41582(14) 0.90930(10) 0.57915(9) 0.120 Uiso 0.50 1 d PD M 2 O48 O 0.5013(3) 0.15616(16) 0.38812(15) 0.120 Uiso 0.50 1 d PD N 1 Cl7 Cl 0.51990(14) 0.11213(10) 0.42683(9) 0.120 Uiso 0.50 1 d PD N 1 O51 O 0.8438(2) 0.94786(16) 0.57988(15) 0.1343(13) Uiso 1 1 d G . . H51A H 0.8368 0.9848 0.5792 0.202 Uiso 1 1 d G . . H51B H 0.7961 0.9311 0.5762 0.202 Uiso 1 1 d G . . O46 O 0.4558(2) 0.1107(2) 0.45812(15) 0.120 Uiso 0.50 1 d PD N 1 O26 O 0.33253(19) 0.8903(2) 0.5735(2) 0.120 Uiso 0.50 1 d PD M 2 O49 O 0.5184(4) 0.05506(13) 0.40455(19) 0.120 Uiso 0.50 1 d PD N 1 O27 O 0.4216(3) 0.96735(13) 0.59832(19) 0.120 Uiso 0.50 1 d PD M 2 O29 O 0.4687(3) 0.86714(17) 0.61296(18) 0.120 Uiso 0.50 1 d PD M 2 O44 O 0.4828(4) 0.2716(3) 0.50700(18) 0.1034(7) Uani 0.50 1 d PDU G 2 O43 O 0.4060(3) 0.2235(3) 0.5579(2) 0.1034(7) Uani 0.50 1 d PDU G 2 O47 O 0.5958(2) 0.1264(2) 0.46453(18) 0.120 Uiso 0.50 1 d PD N 1 N25 N 0.3838(3) 0.4249(3) 0.2417(4) 0.1101(17) Uiso 0.50 1 d PD O 1 C62 C 0.3107(3) 0.4299(4) 0.2335(4) 0.1101(17) Uiso 0.50 1 d PD O 1 C63 C 0.2210(3) 0.4398(4) 0.2197(4) 0.1101(17) Uiso 0.50 1 d PD O 1 H63A H 0.2061 0.4555 0.1842 0.165 Uiso 0.50 1 calc PR O 1 H63B H 0.2054 0.4671 0.2445 0.165 Uiso 0.50 1 calc PR O 1 H63C H 0.1920 0.4035 0.2213 0.165 Uiso 0.50 1 calc PR O 1 O28 O 0.4358(3) 0.9105(2) 0.52677(12) 0.120 Uiso 0.50 1 d PD M 2 C1A C 0.9104(3) 0.0741(2) 0.48571(16) 0.0890(18) Uani 0.60 1 d PD B 1 H1A H 0.9410 0.0538 0.5148 0.107 Uiso 0.60 1 calc PR B 1 C1B C 0.8622(3) 0.1222(2) 0.49370(19) 0.088(2) Uani 0.60 1 d PD B 1 H1B H 0.8638 0.1389 0.5270 0.106 Uiso 0.60 1 calc PR B 1 C1C C 0.8376(4) 0.1618(2) 0.43926(19) 0.0568(15) Uani 0.40 1 d PD B 2 C1D C 0.9127(3) 0.0565(2) 0.43400(15) 0.0699(18) Uani 0.60 1 d PD B 1 H1D H 0.9451 0.0241 0.4296 0.084 Uiso 0.60 1 calc PR B 1 N14 N 0.7906(4) 0.2068(2) 0.4482(2) 0.0568(15) Uani 0.40 1 d P B 2 H14 H 0.7857 0.2031 0.4809 0.068 Uiso 0.40 1 d PR B 2 Cl9 Cl 0.0336(2) 0.92721(18) 0.34886(14) 0.0891(4) Uani 0.20 1 d PD F 3 O1C O 0.0662(6) 0.8670(3) 0.3601(4) 0.0891(4) Uani 0.20 1 d PD F 3 O1D O -0.0287(6) 0.9196(6) 0.2999(3) 0.0891(4) Uani 0.20 1 d PD F 3 O1E O 0.5071(2) 0.28802(19) 0.60140(14) 0.0592(12) Uani 0.50 1 d PG P 1 H1EA H 0.5349 0.3156 0.5911 0.089 Uiso 0.50 1 d PG P 1 H1EB H 0.5177 0.2561 0.5870 0.089 Uiso 0.50 1 d PG P 1 O1F O 0.7746(2) 0.32426(12) 0.55850(13) 0.0479(3) Uani 0.50 1 d PD K 1 Cl10 Cl 0.81622(9) 0.27272(5) 0.57892(5) 0.0479(3) Uani 0.50 1 d PD K 1 O1H O 0.7603(3) 0.2204(2) 0.57036(18) 0.1048(6) Uani 0.50 1 d PD C 2 O1I O 0.8523(4) 0.2842(3) 0.63314(15) 0.1048(6) Uani 0.50 1 d PD C 2 O1J O 0.8791(2) 0.25966(13) 0.54673(12) 0.0479(3) Uani 0.50 1 d PD K 1 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 0.02566(14) 0.01946(15) 0.02285(14) -0.00096(13) -0.00230(12) 0.00082(13) Fe2 0.02583(14) 0.02324(16) 0.02431(14) -0.00211(13) -0.00309(12) 0.00197(13) Fe3 0.02569(14) 0.02368(16) 0.02316(14) -0.00243(13) -0.00278(12) 0.00104(13) Fe4 0.04837(18) 0.02543(18) 0.03329(17) 0.00610(15) 0.00682(15) 0.00504(16) Fe5 0.0422(2) 0.03128(19) 0.0527(2) -0.01642(18) -0.01343(18) 0.00653(17) O1A 0.0210(6) 0.0236(7) 0.0304(7) -0.0107(6) 0.0003(5) 0.0008(5) O3 0.0336(7) 0.0350(8) 0.0341(7) 0.0030(7) 0.0003(6) 0.0048(7) O15 0.0290(7) 0.0378(9) 0.0364(8) -0.0133(7) -0.0025(6) -0.0005(7) O1B 0.0347(8) 0.0317(9) 0.0410(8) -0.0026(7) -0.0043(7) 0.0002(7) O2 0.0347(7) 0.0300(8) 0.0331(8) 0.0051(7) -0.0096(7) 0.0017(7) O3B 0.0351(7) 0.0332(8) 0.0235(7) 0.0012(6) -0.0005(6) 0.0028(7) O12 0.0412(8) 0.0430(9) 0.0261(7) -0.0071(7) -0.0013(6) -0.0196(7) O2B 0.0384(7) 0.0284(8) 0.0273(7) -0.0026(6) 0.0004(6) -0.0063(7) O6 0.0404(7) 0.0406(9) 0.0270(7) -0.0034(7) 0.0007(6) 0.0195(7) O7 0.0422(8) 0.0281(8) 0.0287(7) 0.0038(6) 0.0034(6) -0.0044(7) O8 0.0321(7) 0.0298(8) 0.0283(7) -0.0061(6) 0.0009(6) -0.0066(6) O18 0.0381(8) 0.0333(8) 0.0348(8) -0.0003(7) 0.0021(6) 0.0100(7) O5 0.0339(7) 0.0316(8) 0.0288(7) -0.0025(7) -0.0064(6) 0.0070(7) O17 0.0275(7) 0.0380(9) 0.0298(7) 0.0068(7) -0.0031(6) 0.0060(7) O1 0.0475(9) 0.0330(9) 0.0328(8) 0.0022(7) -0.0054(7) 0.0040(7) O4 0.0522(9) 0.0300(8) 0.0246(7) -0.0008(6) 0.0037(6) 0.0012(7) O9 0.0378(7) 0.0299(8) 0.0314(7) 0.0017(7) -0.0013(6) -0.0094(7) N10 0.0328(9) 0.0369(11) 0.0481(11) -0.0128(9) -0.0008(8) 0.0144(8) O11 0.0339(7) 0.0308(8) 0.0382(8) 0.0063(7) -0.0094(7) -0.0012(7) O13 0.0417(9) 0.0378(9) 0.0520(10) -0.0148(8) -0.0165(8) 0.0021(8) O14 0.0276(7) 0.0384(9) 0.0312(7) -0.0108(7) -0.0058(6) 0.0061(7) O16 0.0344(8) 0.0319(8) 0.0598(10) -0.0187(8) -0.0112(8) 0.0099(7) O10 0.0507(9) 0.0258(8) 0.0471(9) -0.0060(8) -0.0078(8) 0.0041(8) N6 0.0522(11) 0.0291(10) 0.0409(10) 0.0104(9) -0.0017(9) -0.0112(9) C18 0.0295(9) 0.0215(10) 0.0296(10) 0.0021(9) 0.0034(8) 0.0021(8) C26 0.0339(10) 0.0256(11) 0.0245(10) 0.0008(9) -0.0029(8) -0.0011(9) N1 0.0518(11) 0.0319(10) 0.0456(11) 0.0142(9) 0.0113(9) 0.0139(9) N3 0.0470(11) 0.0366(11) 0.0492(11) -0.0002(10) 0.0107(9) -0.0041(9) C27 0.0270(9) 0.0188(10) 0.0250(9) 0.0009(8) -0.0053(8) -0.0017(8) N5 0.0596(11) 0.0267(10) 0.0308(9) 0.0074(8) 0.0081(8) 0.0006(9) C15 0.0327(10) 0.0217(10) 0.0417(12) 0.0023(10) -0.0010(9) 0.0118(9) C17 0.0261(9) 0.0368(12) 0.0285(10) 0.0014(9) -0.0010(8) 0.0088(9) C8 0.0440(12) 0.0382(13) 0.0199(9) 0.0001(9) -0.0006(9) 0.0024(10) N9 0.0539(12) 0.0297(10) 0.0514(12) -0.0158(9) -0.0065(10) 0.0115(9) C54 0.0343(10) 0.0274(11) 0.0243(9) -0.0103(9) -0.0019(8) 0.0021(9) N4 0.0484(11) 0.0497(13) 0.0271(9) 0.0025(9) -0.0077(9) -0.0067(10) N11 0.0540(12) 0.0337(11) 0.0620(13) -0.0237(10) -0.0173(11) 0.0072(10) C45 0.0345(10) 0.0168(9) 0.0254(9) -0.0083(8) -0.0059(8) -0.0018(8) C7 0.0478(13) 0.0441(14) 0.0307(11) 0.0067(11) -0.0038(10) -0.0029(12) C9 0.0391(11) 0.0206(10) 0.0336(11) -0.0007(9) -0.0064(9) -0.0048(9) C14 0.0402(11) 0.0470(14) 0.0339(11) 0.0024(11) 0.0072(9) 0.0069(11) C36 0.0296(10) 0.0306(11) 0.0316(10) -0.0027(9) 0.0015(9) 0.0030(9) C44 0.0315(10) 0.0259(11) 0.0343(11) -0.0033(9) -0.0083(9) 0.0050(9) N2 0.0532(12) 0.0563(13) 0.0455(12) 0.0118(11) 0.0008(10) 0.0220(11) C43 0.0359(11) 0.0362(13) 0.0539(14) -0.0167(12) -0.0099(11) 0.0124(10) C24 0.0436(11) 0.0256(11) 0.0269(10) -0.0007(9) -0.0010(9) -0.0070(10) O37 0.0380(10) 0.0575(14) 0.0437(13) -0.0111(11) -0.0068(10) -0.0105(9) C16 0.0375(10) 0.0252(11) 0.0321(10) -0.0004(9) 0.0056(8) 0.0108(9) C6 0.0485(12) 0.0312(12) 0.0328(11) 0.0086(10) 0.0055(10) 0.0002(11) C51 0.0358(11) 0.0318(12) 0.0517(13) -0.0184(11) -0.0058(11) 0.0039(10) C52 0.0345(11) 0.0482(14) 0.0422(12) -0.0208(11) -0.0050(10) 0.0071(11) C42 0.0404(12) 0.0322(12) 0.0379(11) -0.0149(10) -0.0093(10) 0.0103(10) C53 0.0449(13) 0.0473(14) 0.0385(12) -0.0208(11) 0.0013(10) -0.0008(12) N12 0.0441(12) 0.0494(13) 0.0579(13) -0.0260(11) -0.0162(11) -0.0039(10) C41 0.0505(13) 0.0279(12) 0.0400(12) -0.0050(10) 0.0014(11) 0.0084(11) N8 0.0612(19) 0.0164(14) 0.0254(14) -0.0014(12) -0.0064(14) 0.0124(14) C33 0.0791(19) 0.0322(13) 0.0446(14) -0.0128(12) -0.0211(14) 0.0036(14) C40 0.0549(13) 0.0273(12) 0.0489(13) -0.0008(11) 0.0075(11) 0.0168(11) O35 0.0476(12) 0.0427(13) 0.0594(12) -0.0126(11) 0.0022(10) -0.0005(11) C25 0.0421(11) 0.0216(10) 0.0291(10) 0.0021(9) -0.0027(9) -0.0066(9) C23 0.0513(12) 0.0260(11) 0.0337(11) 0.0013(10) 0.0076(10) -0.0029(10) C34 0.0749(17) 0.0280(12) 0.0325(12) -0.0045(10) -0.0021(12) -0.0006(13) N7 0.0706(15) 0.0421(13) 0.0536(13) -0.0047(11) -0.0091(12) 0.0150(12) C19 0.0591(15) 0.0350(13) 0.0411(13) 0.0143(11) -0.0032(12) 0.0081(12) C21 0.099(2) 0.0280(13) 0.0420(14) 0.0058(11) 0.0040(15) -0.0186(14) C35 0.0379(11) 0.0269(11) 0.0335(11) -0.0043(9) 0.0004(9) -0.0034(9) C1 0.0716(17) 0.0466(16) 0.0643(17) 0.0145(14) 0.0187(14) 0.0179(14) C22 0.0721(16) 0.0351(13) 0.0508(14) 0.0069(12) 0.0083(13) -0.0255(12) C38 0.0795(19) 0.0399(14) 0.0381(13) -0.0142(12) -0.0119(14) 0.0143(14) O31 0.0496(12) 0.0608(15) 0.0436(12) 0.0071(11) 0.0042(10) -0.0078(12) C32 0.063(2) 0.032(2) 0.0243(17) 0.0048(16) -0.0010(17) 0.0159(19) C5 0.0592(14) 0.0354(13) 0.0457(12) 0.0206(11) 0.0127(11) 0.0200(11) C37 0.0602(16) 0.0412(15) 0.0555(16) -0.0137(13) -0.0105(14) 0.0092(13) C2 0.0696(17) 0.0581(18) 0.0644(17) 0.0184(15) 0.0180(14) 0.0258(14) C4 0.0603(15) 0.0408(14) 0.0539(15) 0.0161(12) 0.0091(13) 0.0166(12) C20 0.0656(16) 0.0362(14) 0.0479(14) 0.0132(12) 0.0062(13) 0.0046(13) C49 0.0581(16) 0.0371(14) 0.0714(18) -0.0209(13) -0.0196(15) -0.0001(13) C39 0.0804(17) 0.0336(13) 0.0392(12) -0.0079(11) 0.0109(12) 0.0135(13) C13 0.0489(14) 0.0541(17) 0.0519(15) -0.0057(14) -0.0041(13) -0.0138(13) C3 0.0670(15) 0.0583(15) 0.0692(16) 0.0392(13) 0.0249(13) 0.0376(13) C48 0.075(2) 0.0428(16) 0.088(2) -0.0168(16) -0.0220(19) -0.0151(15) C12 0.076(2) 0.0586(19) 0.0633(18) -0.0104(16) 0.0079(16) -0.0134(17) O54 0.1159(9) 0.1535(13) 0.0390(6) -0.0064(7) 0.0020(6) -0.0783(8) C46 0.090(2) 0.0389(16) 0.076(2) -0.0140(15) -0.0329(18) -0.0139(16) C50 0.0521(14) 0.0328(13) 0.0545(15) -0.0197(11) -0.0161(13) 0.0004(12) C11 0.100(2) 0.0473(16) 0.0715(17) -0.0161(15) 0.0379(15) -0.0328(15) C10 0.0826(19) 0.0371(15) 0.0686(17) -0.0086(14) 0.0235(15) -0.0077(14) C28 0.097(2) 0.0468(16) 0.0532(17) -0.0101(14) -0.0058(17) 0.0260(16) C47 0.085(2) 0.0432(18) 0.111(3) -0.0044(19) -0.023(2) -0.0138(17) O55 0.1159(9) 0.1535(13) 0.0390(6) -0.0064(7) 0.0020(6) -0.0783(8) C31 0.056(4) 0.054(4) 0.037(3) -0.002(3) -0.005(3) 0.009(3) Cl5 0.0384(5) 0.0400(5) 0.0312(4) -0.0198(4) 0.0077(4) -0.0213(4) O41 0.059(2) 0.0286(18) 0.082(3) -0.0143(18) 0.0183(19) -0.0148(16) O39 0.0552(18) 0.100(3) 0.0256(14) -0.0207(18) 0.0145(13) -0.0331(19) O38 0.0492(17) 0.0412(18) 0.0285(15) 0.0082(14) 0.0035(14) 0.0022(15) O40 0.055(2) 0.078(3) 0.0400(18) -0.0171(19) -0.0003(17) -0.026(2) Cl1 0.1308(10) 0.0906(7) 0.0491(4) 0.0044(5) 0.0261(5) 0.0031(8) O22 0.1308(10) 0.0906(7) 0.0491(4) 0.0044(5) 0.0261(5) 0.0031(8) O23 0.1308(10) 0.0906(7) 0.0491(4) 0.0044(5) 0.0261(5) 0.0031(8) O24 0.1308(10) 0.0906(7) 0.0491(4) 0.0044(5) 0.0261(5) 0.0031(8) Cl6 0.0918(10) 0.1155(13) 0.0977(12) 0.0037(11) 0.0078(10) 0.0306(9) O45 0.0918(10) 0.1155(13) 0.0977(12) 0.0037(11) 0.0078(10) 0.0306(9) Cl2 0.1308(10) 0.0906(7) 0.0491(4) 0.0044(5) 0.0261(5) 0.0031(8) O25 0.1308(10) 0.0906(7) 0.0491(4) 0.0044(5) 0.0261(5) 0.0031(8) O20 0.1308(10) 0.0906(7) 0.0491(4) 0.0044(5) 0.0261(5) 0.0031(8) O21 0.1308(10) 0.0906(7) 0.0491(4) 0.0044(5) 0.0261(5) 0.0031(8) C29 0.063(4) 0.090(6) 0.070(5) -0.006(4) 0.013(4) -0.029(4) C30 0.025(3) 0.082(5) 0.083(5) -0.020(4) -0.004(3) 0.013(3) Cl4 0.0398(3) 0.0470(3) 0.0309(2) -0.0083(2) -0.0054(2) -0.0013(3) O32 0.0505(11) 0.0565(12) 0.0383(9) -0.0159(9) -0.0128(9) 0.0162(10) O42 0.0918(10) 0.1155(13) 0.0977(12) 0.0037(11) 0.0078(10) 0.0306(9) O56 0.0851(7) 0.0183(4) 0.0313(4) 0.0093(4) -0.0086(5) -0.0219(5) Cl8 0.1159(9) 0.1535(13) 0.0390(6) -0.0064(7) 0.0020(6) -0.0783(8) O33 0.0505(11) 0.0565(12) 0.0383(9) -0.0159(9) -0.0128(9) 0.0162(10) O30 0.0496(12) 0.0608(15) 0.0436(12) 0.0071(11) 0.0042(10) -0.0078(12) O34 0.0476(12) 0.0427(13) 0.0594(12) -0.0126(11) 0.0022(10) -0.0005(11) O36 0.0380(10) 0.0575(14) 0.0437(13) -0.0111(11) -0.0068(10) -0.0105(9) O53 0.0851(7) 0.0183(4) 0.0313(4) 0.0093(4) -0.0086(5) -0.0219(5) O52 0.0522(11) 0.0745(14) 0.0685(13) -0.0170(12) -0.0043(10) 0.0069(11) O44 0.0918(10) 0.1155(13) 0.0977(12) 0.0037(11) 0.0078(10) 0.0306(9) O43 0.0918(10) 0.1155(13) 0.0977(12) 0.0037(11) 0.0078(10) 0.0306(9) C1A 0.117(3) 0.098(3) 0.040(3) 0.002(2) -0.010(3) 0.087(2) C1B 0.116(4) 0.095(4) 0.047(3) 0.016(3) 0.000(3) 0.062(3) C1C 0.087(3) 0.034(2) 0.036(2) -0.0108(19) -0.018(2) -0.004(2) C1D 0.086(3) 0.058(3) 0.065(3) 0.003(3) 0.015(3) 0.045(2) N14 0.087(3) 0.034(2) 0.036(2) -0.0108(19) -0.018(2) -0.004(2) Cl9 0.1308(10) 0.0906(7) 0.0491(4) 0.0044(5) 0.0261(5) 0.0031(8) O1C 0.1308(10) 0.0906(7) 0.0491(4) 0.0044(5) 0.0261(5) 0.0031(8) O1D 0.1308(10) 0.0906(7) 0.0491(4) 0.0044(5) 0.0261(5) 0.0031(8) O1E 0.0367(16) 0.091(3) 0.0386(18) -0.0018(19) -0.0170(15) 0.0412(16) O1F 0.0851(7) 0.0183(4) 0.0313(4) 0.0093(4) -0.0086(5) -0.0219(5) Cl10 0.0851(7) 0.0183(4) 0.0313(4) 0.0093(4) -0.0086(5) -0.0219(5) O1H 0.1159(9) 0.1535(13) 0.0390(6) -0.0064(7) 0.0020(6) -0.0783(8) O1I 0.1159(9) 0.1535(13) 0.0390(6) -0.0064(7) 0.0020(6) -0.0783(8) O1J 0.0851(7) 0.0183(4) 0.0313(4) 0.0093(4) -0.0086(5) -0.0219(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1A 1.9027(15) . ? Fe1 O12 1.9998(17) . ? Fe1 O2B 2.0873(15) . ? Fe1 O6 2.0179(16) . ? Fe1 O18 2.0021(16) . ? Fe1 O9 1.9768(16) . ? Fe2 O1A 1.8907(13) . ? Fe2 O1B 2.0849(15) . ? Fe2 O2 2.0045(16) . ? Fe2 O5 2.0215(16) . ? Fe2 O11 2.0070(17) . ? Fe2 O14 2.0263(16) . ? Fe3 O1A 1.9015(15) . ? Fe3 O3 2.0030(16) . ? Fe3 O15 2.0046(16) . ? Fe3 O3B 2.0826(17) . ? Fe3 O8 2.0413(15) . ? Fe3 O17 2.0119(15) . ? Fe4 O7 2.1069(15) . ? Fe4 O1 2.0704(16) . ? Fe4 O4 2.0818(18) . ? Fe4 N1 2.187(2) . ? Fe4 N3 2.218(2) . ? Fe4 N5 2.204(2) . ? Fe5 O13 2.0606(18) . ? Fe5 O16 2.1026(16) . ? Fe5 O10 2.090(2) . ? Fe5 N9 2.210(2) . ? Fe5 N11 2.186(2) . ? Fe5 N7 2.215(2) . ? O3 C9 1.272(3) . ? O15 C54 1.278(2) . ? O1B H1BA 0.8969 . ? O1B H1BB 0.8941 . ? O2 C9 1.258(3) . ? O3B H3BA 0.8533 . ? O3B H3BB 0.8523 . ? O12 C36 1.248(2) . ? O2B H2BA 0.8787 . ? O2B H2BB 0.8768 . ? O6 C18 1.245(2) . ? O7 C24 1.237(3) . ? O8 C27 1.267(3) . ? O18 C45 1.239(3) . ? O5 C18 1.252(3) . ? O17 C45 1.271(3) . ? O1 C6 1.225(3) . ? O4 C15 1.219(3) . ? O9 C27 1.251(3) . ? N10 H10 0.8600 . ? N10 C42 1.339(3) . ? N10 C41 1.397(3) . ? O11 C36 1.256(3) . ? O13 C51 1.223(3) . ? O14 C54 1.244(3) . ? O16 C42 1.229(3) . ? O10 C33 1.262(3) . ? N6 H6 0.8600 . ? N6 C24 1.364(3) . ? N6 C23 1.390(3) . ? C18 C17 1.527(3) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 C27 1.496(3) . ? C26 C25 1.501(3) . ? N1 C1 1.353(4) . ? N1 C5 1.327(3) . ? N3 C14 1.351(3) . ? N3 C10 1.325(4) . ? N5 C23 1.331(3) . ? N5 C19 1.358(3) . ? C15 N4 1.359(3) . ? C15 C16 1.491(3) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 C16 1.502(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 C7 1.522(4) . ? C8 C9 1.505(3) . ? N9 C41 1.357(3) . ? N9 C37 1.331(3) . ? C54 C53 1.506(3) . ? N4 H4 0.8600 . ? N4 C14 1.401(3) . ? N11 C46 1.352(4) . ? N11 C50 1.343(3) . ? C45 C44 1.500(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 C6 1.510(4) . ? C14 C13 1.390(4) . ? C36 C35 1.513(3) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C44 C43 1.504(4) . ? N2 H2 0.8600 . ? N2 C6 1.351(3) . ? N2 C5 1.388(4) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 C42 1.536(3) . ? C24 C25 1.512(3) . ? O37 Cl4 1.434(5) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C51 C52 1.514(4) . ? C51 N12 1.345(3) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C52 C53 1.540(4) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? N12 H12 0.8600 . ? N12 C50 1.376(4) . ? C41 C40 1.407(4) . ? N8 H8 0.8600 . ? N8 C33 1.343(4) . ? N8 C32 1.426(5) . ? N8 H14 0.7907 . ? C33 C34 1.499(4) . ? C33 N14 1.457(7) . ? C40 H40 0.9300 . ? C40 C39 1.375(4) . ? O35 Cl4 1.490(2) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C23 C22 1.383(4) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 C35 1.527(3) . ? N7 C32 1.401(4) . ? N7 C28 1.342(4) . ? N7 C1C 1.343(5) . ? C19 H19 0.9300 . ? C19 C20 1.337(4) . ? C21 H21 0.9300 . ? C21 C22 1.352(4) . ? C21 C20 1.360(4) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C1 H1 0.9300 . ? C1 C2 1.400(4) . ? C22 H22 0.9300 . ? C38 H38 0.9300 . ? C38 C37 1.390(5) . ? C38 C39 1.362(4) . ? O31 Cl4 1.402(3) . ? C32 C1B 1.402(5) . ? C5 C4 1.385(4) . ? C37 H37 0.9300 . ? C2 H2A 0.9300 . ? C2 C3 1.366(4) . ? C4 H4A 0.9300 . ? C4 C3 1.380(4) . ? C20 H20 0.9300 . ? C49 H49 0.9300 . ? C49 C48 1.365(5) . ? C49 C50 1.395(4) . ? C39 H39 0.9300 . ? C13 H13 0.9300 . ? C13 C12 1.356(5) . ? C3 H3 0.9300 . ? C48 H48 0.9300 . ? C48 C47 1.393(5) . ? C12 H12A 0.9300 . ? C12 C11 1.401(5) . ? O54 Cl8 1.449(5) . ? C46 H46 0.9300 . ? C46 C47 1.403(5) . ? C11 H11 0.9300 . ? C11 C10 1.375(4) . ? C10 H10A 0.9300 . ? C28 H28A 0.9300 . ? C28 H28 0.9300 . ? C28 C29 1.366(6) . ? C28 C1D 1.371(5) . ? C47 H47 0.9300 . ? O55 Cl8 1.470(5) . ? C31 H31 0.9300 . ? C31 C30 1.393(7) . ? C31 C1C 1.381(7) . ? Cl5 O41 1.428(3) . ? Cl5 O39 1.417(4) . ? Cl5 O38 1.424(3) . ? Cl5 O40 1.449(3) . ? Cl1 O22 1.341(3) . ? Cl1 O24 1.481(4) . ? Cl1 O25 1.414(5) . ? O22 Cl2 1.382(3) . ? O22 Cl9 1.354(5) . ? O23 Cl2 1.403(4) . ? Cl6 O45 1.392(5) . ? Cl6 O42 1.387(6) . ? Cl6 O44 1.460(5) . ? Cl6 O43 1.443(5) . ? Cl6 H1EB 0.7783 . ? O45 H1EA 0.7452 . ? O45 H1EB 0.7376 . ? Cl2 O20 1.412(6) . ? Cl2 O21 1.421(6) . ? N13 C65 1.175(8) . ? C65 C64 1.506(8) . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? N15 C60 1.156(6) . ? C60 C61 1.437(7) . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? N19 C58 1.118(7) . ? C58 C59 1.428(8) . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C29 H29 0.9300 . ? C29 C30 1.389(8) . ? C30 H30 0.9300 . ? Cl4 O32 1.451(2) . ? Cl4 O33 1.445(5) . ? Cl4 O30 1.467(5) . ? Cl4 O34 1.448(6) . ? Cl4 O36 1.436(2) . ? O56 Cl10 1.405(3) . ? Cl8 O1H 1.424(5) . ? Cl8 O1I 1.408(4) . ? O53 Cl10 1.421(3) . ? O52 H52C 0.8511 . ? O52 H52D 0.8473 . ? Cl3 O26 1.400(4) . ? Cl3 O27 1.411(4) . ? Cl3 O29 1.451(4) . ? Cl3 O28 1.444(4) . ? O48 Cl7 1.400(4) . ? Cl7 O46 1.440(4) . ? Cl7 O49 1.422(4) . ? Cl7 O47 1.437(4) . ? O51 H51A 0.8509 . ? O51 H51B 0.8516 . ? N25 C62 1.169(7) . ? C62 C63 1.444(7) . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C1A H1A 0.9300 . ? C1A C1B 1.389(7) . ? C1A C1D 1.391(6) . ? C1B H1B 0.9300 . ? C1C N14 1.328(9) . ? C1D H1D 0.9300 . ? N14 H14 0.8601 . ? Cl9 O1C 1.481(7) . ? Cl9 O1D 1.448(8) . ? O1E H1EA 0.8502 . ? O1E H1EB 0.8504 . ? O1F Cl10 1.404(3) . ? Cl10 O1J 1.471(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A Fe1 O12 95.64(6) . . ? O1A Fe1 O2B 179.84(7) . . ? O1A Fe1 O6 93.56(6) . . ? O1A Fe1 O18 95.52(6) . . ? O1A Fe1 O9 96.06(6) . . ? O12 Fe1 O2B 84.45(6) . . ? O12 Fe1 O6 90.86(7) . . ? O12 Fe1 O18 87.61(7) . . ? O6 Fe1 O2B 86.30(6) . . ? O18 Fe1 O2B 84.61(6) . . ? O18 Fe1 O6 170.89(7) . . ? O9 Fe1 O12 168.28(6) . . ? O9 Fe1 O2B 83.85(6) . . ? O9 Fe1 O6 88.98(6) . . ? O9 Fe1 O18 90.70(6) . . ? O1A Fe2 O1B 177.68(7) . . ? O1A Fe2 O2 95.92(6) . . ? O1A Fe2 O5 95.52(6) . . ? O1A Fe2 O11 96.59(6) . . ? O1A Fe2 O14 94.61(6) . . ? O2 Fe2 O1B 81.86(6) . . ? O2 Fe2 O5 90.80(7) . . ? O2 Fe2 O11 167.42(6) . . ? O2 Fe2 O14 87.25(7) . . ? O5 Fe2 O1B 85.24(6) . . ? O5 Fe2 O14 169.83(6) . . ? O11 Fe2 O1B 85.61(6) . . ? O11 Fe2 O5 89.32(7) . . ? O11 Fe2 O14 90.42(7) . . ? O14 Fe2 O1B 84.61(6) . . ? O1A Fe3 O3 96.47(6) . . ? O1A Fe3 O15 95.91(6) . . ? O1A Fe3 O3B 178.75(6) . . ? O1A Fe3 O8 94.55(6) . . ? O1A Fe3 O17 94.78(6) . . ? O3 Fe3 O15 86.95(6) . . ? O3 Fe3 O3B 83.60(6) . . ? O3 Fe3 O8 86.57(6) . . ? O3 Fe3 O17 168.39(7) . . ? O15 Fe3 O3B 85.34(6) . . ? O15 Fe3 O8 168.25(7) . . ? O15 Fe3 O17 89.05(6) . . ? O8 Fe3 O3B 84.21(6) . . ? O17 Fe3 O3B 85.21(6) . . ? O17 Fe3 O8 95.39(6) . . ? O7 Fe4 N1 174.58(7) . . ? O7 Fe4 N3 86.08(7) . . ? O7 Fe4 N5 83.24(7) . . ? O1 Fe4 O7 91.93(6) . . ? O1 Fe4 O4 96.47(7) . . ? O1 Fe4 N1 83.24(7) . . ? O1 Fe4 N3 178.00(7) . . ? O1 Fe4 N5 86.05(7) . . ? O4 Fe4 O7 89.60(6) . . ? O4 Fe4 N1 88.50(8) . . ? O4 Fe4 N3 83.67(7) . . ? O4 Fe4 N5 172.50(7) . . ? N1 Fe4 N3 98.75(8) . . ? N1 Fe4 N5 98.83(8) . . ? N5 Fe4 N3 93.57(8) . . ? O13 Fe5 O16 89.11(7) . . ? O13 Fe5 O10 92.69(7) . . ? O13 Fe5 N9 89.25(8) . . ? O13 Fe5 N11 83.16(8) . . ? O13 Fe5 N7 173.81(8) . . ? O16 Fe5 N9 83.48(8) . . ? O16 Fe5 N11 172.24(8) . . ? O16 Fe5 N7 85.91(8) . . ? O10 Fe5 O16 91.61(7) . . ? O10 Fe5 N9 174.70(7) . . ? O10 Fe5 N11 88.15(8) . . ? O10 Fe5 N7 83.79(8) . . ? N9 Fe5 N7 93.83(9) . . ? N11 Fe5 N9 96.98(9) . . ? N11 Fe5 N7 101.77(9) . . ? Fe2 O1A Fe1 120.27(8) . . ? Fe2 O1A Fe3 121.20(8) . . ? Fe3 O1A Fe1 118.52(7) . . ? C9 O3 Fe3 132.86(16) . . ? C54 O15 Fe3 130.06(15) . . ? Fe2 O1B H1BA 112.7 . . ? Fe2 O1B H1BB 110.9 . . ? H1BA O1B H1BB 105.7 . . ? C9 O2 Fe2 131.30(14) . . ? Fe3 O3B H3BA 109.9 . . ? Fe3 O3B H3BB 108.9 . . ? H3BA O3B H3BB 110.3 . . ? C36 O12 Fe1 134.64(16) . . ? Fe1 O2B H2BA 111.3 . . ? Fe1 O2B H2BB 110.3 . . ? H2BA O2B H2BB 107.8 . . ? C18 O6 Fe1 131.02(14) . . ? C24 O7 Fe4 130.22(15) . . ? C27 O8 Fe3 128.13(14) . . ? C45 O18 Fe1 130.19(14) . . ? C18 O5 Fe2 132.30(14) . . ? C45 O17 Fe3 134.16(14) . . ? C6 O1 Fe4 133.32(16) . . ? C15 O4 Fe4 131.48(15) . . ? C27 O9 Fe1 134.40(13) . . ? C42 N10 H10 115.0 . . ? C42 N10 C41 129.9(2) . . ? C41 N10 H10 115.0 . . ? C36 O11 Fe2 130.35(14) . . ? C51 O13 Fe5 133.10(17) . . ? C54 O14 Fe2 134.28(14) . . ? C42 O16 Fe5 129.15(16) . . ? C33 O10 Fe5 130.35(18) . . ? C24 N6 H6 114.0 . . ? C24 N6 C23 132.0(2) . . ? C23 N6 H6 114.0 . . ? O6 C18 O5 126.2(2) . . ? O6 C18 C17 115.85(18) . . ? O5 C18 C17 117.90(17) . . ? H26A C26 H26B 107.4 . . ? C27 C26 H26A 108.2 . . ? C27 C26 H26B 108.2 . . ? C27 C26 C25 116.22(18) . . ? C25 C26 H26A 108.2 . . ? C25 C26 H26B 108.2 . . ? C1 N1 Fe4 114.51(17) . . ? C5 N1 Fe4 127.92(18) . . ? C5 N1 C1 117.1(2) . . ? C14 N3 Fe4 124.96(17) . . ? C10 N3 Fe4 117.5(2) . . ? C10 N3 C14 117.1(2) . . ? O8 C27 C26 119.30(19) . . ? O9 C27 O8 123.67(19) . . ? O9 C27 C26 116.95(19) . . ? C23 N5 Fe4 125.72(16) . . ? C23 N5 C19 116.3(2) . . ? C19 N5 Fe4 117.54(18) . . ? O4 C15 N4 123.9(2) . . ? O4 C15 C16 122.2(2) . . ? N4 C15 C16 113.8(2) . . ? C18 C17 H17A 108.8 . . ? C18 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? C16 C17 C18 113.92(18) . . ? C16 C17 H17A 108.8 . . ? C16 C17 H17B 108.8 . . ? H8A C8 H8B 107.7 . . ? C7 C8 H8A 108.9 . . ? C7 C8 H8B 108.9 . . ? C9 C8 H8A 108.9 . . ? C9 C8 H8B 108.9 . . ? C9 C8 C7 113.3(2) . . ? C41 N9 Fe5 124.40(17) . . ? C37 N9 Fe5 118.4(2) . . ? C37 N9 C41 116.7(2) . . ? O15 C54 C53 115.8(2) . . ? O14 C54 O15 125.3(2) . . ? O14 C54 C53 118.50(18) . . ? C15 N4 H4 114.5 . . ? C15 N4 C14 130.9(2) . . ? C14 N4 H4 114.5 . . ? C46 N11 Fe5 115.10(19) . . ? C50 N11 Fe5 126.88(19) . . ? C50 N11 C46 117.6(2) . . ? O18 C45 O17 124.67(19) . . ? O18 C45 C44 117.0(2) . . ? O17 C45 C44 118.2(2) . . ? C8 C7 H7A 109.3 . . ? C8 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? C6 C7 C8 111.57(19) . . ? C6 C7 H7A 109.3 . . ? C6 C7 H7B 109.3 . . ? O3 C9 C8 116.4(2) . . ? O2 C9 O3 125.0(2) . . ? O2 C9 C8 118.61(19) . . ? N3 C14 N4 120.7(2) . . ? N3 C14 C13 122.7(3) . . ? C13 C14 N4 116.6(2) . . ? O12 C36 O11 125.2(2) . . ? O12 C36 C35 116.60(19) . . ? O11 C36 C35 118.20(18) . . ? C45 C44 H44A 108.6 . . ? C45 C44 H44B 108.6 . . ? C45 C44 C43 114.47(19) . . ? H44A C44 H44B 107.6 . . ? C43 C44 H44A 108.6 . . ? C43 C44 H44B 108.6 . . ? C6 N2 H2 114.5 . . ? C6 N2 C5 131.0(2) . . ? C5 N2 H2 114.5 . . ? C44 C43 H43A 109.0 . . ? C44 C43 H43B 109.0 . . ? C44 C43 C42 112.9(2) . . ? H43A C43 H43B 107.8 . . ? C42 C43 H43A 109.0 . . ? C42 C43 H43B 109.0 . . ? O7 C24 N6 122.7(2) . . ? O7 C24 C25 122.0(2) . . ? N6 C24 C25 115.3(2) . . ? C15 C16 C17 113.65(19) . . ? C15 C16 H16A 108.8 . . ? C15 C16 H16B 108.8 . . ? C17 C16 H16A 108.8 . . ? C17 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? O1 C6 C7 120.2(2) . . ? O1 C6 N2 123.5(2) . . ? N2 C6 C7 116.3(2) . . ? O13 C51 C52 119.2(2) . . ? O13 C51 N12 123.8(2) . . ? N12 C51 C52 116.9(2) . . ? C51 C52 H52A 109.1 . . ? C51 C52 H52B 109.1 . . ? C51 C52 C53 112.32(19) . . ? H52A C52 H52B 107.9 . . ? C53 C52 H52A 109.1 . . ? C53 C52 H52B 109.1 . . ? N10 C42 C43 113.7(2) . . ? O16 C42 N10 125.6(2) . . ? O16 C42 C43 120.8(2) . . ? C54 C53 C52 111.7(2) . . ? C54 C53 H53A 109.3 . . ? C54 C53 H53B 109.3 . . ? C52 C53 H53A 109.3 . . ? C52 C53 H53B 109.3 . . ? H53A C53 H53B 107.9 . . ? C51 N12 H12 114.9 . . ? C51 N12 C50 130.2(2) . . ? C50 N12 H12 114.9 . . ? N10 C41 C40 117.8(2) . . ? N9 C41 N10 121.3(2) . . ? N9 C41 C40 120.9(2) . . ? H8 N8 H14 38.6 . . ? C33 N8 H8 114.4 . . ? C33 N8 C32 131.1(3) . . ? C33 N8 H14 120.1 . . ? C32 N8 H8 114.4 . . ? C32 N8 H14 98.4 . . ? O10 C33 N8 125.3(3) . . ? O10 C33 C34 122.5(2) . . ? O10 C33 N14 112.4(4) . . ? N8 C33 C34 111.4(3) . . ? N8 C33 N14 29.0(3) . . ? N14 C33 C34 122.3(3) . . ? C41 C40 H40 119.8 . . ? C39 C40 C41 120.4(3) . . ? C39 C40 H40 119.8 . . ? C26 C25 C24 114.1(2) . . ? C26 C25 H25A 108.7 . . ? C26 C25 H25B 108.7 . . ? C24 C25 H25A 108.7 . . ? C24 C25 H25B 108.7 . . ? H25A C25 H25B 107.6 . . ? N5 C23 N6 120.3(2) . . ? N5 C23 C22 121.4(2) . . ? C22 C23 N6 118.3(2) . . ? C33 C34 H34A 108.8 . . ? C33 C34 H34B 108.8 . . ? C33 C34 C35 113.7(2) . . ? H34A C34 H34B 107.7 . . ? C35 C34 H34A 108.8 . . ? C35 C34 H34B 108.8 . . ? C32 N7 Fe5 125.8(2) . . ? C28 N7 Fe5 117.2(2) . . ? C28 N7 C32 115.9(3) . . ? C28 N7 C1C 118.1(3) . . ? C1C N7 Fe5 111.5(3) . . ? C1C N7 C32 27.9(3) . . ? N5 C19 H19 117.6 . . ? C20 C19 N5 124.9(3) . . ? C20 C19 H19 117.6 . . ? C22 C21 H21 120.0 . . ? C22 C21 C20 120.0(3) . . ? C20 C21 H21 120.0 . . ? C36 C35 C34 114.2(2) . . ? C36 C35 H35A 108.7 . . ? C36 C35 H35B 108.7 . . ? C34 C35 H35A 108.7 . . ? C34 C35 H35B 108.7 . . ? H35A C35 H35B 107.6 . . ? N1 C1 H1 118.8 . . ? N1 C1 C2 122.4(3) . . ? C2 C1 H1 118.8 . . ? C23 C22 H22 120.2 . . ? C21 C22 C23 119.6(3) . . ? C21 C22 H22 120.2 . . ? C37 C38 H38 121.0 . . ? C39 C38 H38 121.0 . . ? C39 C38 C37 118.1(3) . . ? N7 C32 N8 119.0(3) . . ? N7 C32 C1B 126.3(4) . . ? C1B C32 N8 113.5(3) . . ? N1 C5 N2 120.4(2) . . ? N1 C5 C4 123.1(3) . . ? C4 C5 N2 116.3(2) . . ? N9 C37 C38 125.1(3) . . ? N9 C37 H37 117.4 . . ? C38 C37 H37 117.4 . . ? C1 C2 H2A 120.3 . . ? C3 C2 C1 119.5(3) . . ? C3 C2 H2A 120.3 . . ? C5 C4 H4A 120.1 . . ? C3 C4 C5 119.8(2) . . ? C3 C4 H4A 120.1 . . ? C19 C20 C21 117.6(3) . . ? C19 C20 H20 121.2 . . ? C21 C20 H20 121.2 . . ? C48 C49 H49 119.3 . . ? C48 C49 C50 121.5(3) . . ? C50 C49 H49 119.3 . . ? C40 C39 H39 120.7 . . ? C38 C39 C40 118.7(3) . . ? C38 C39 H39 120.7 . . ? C14 C13 H13 120.4 . . ? C12 C13 C14 119.1(3) . . ? C12 C13 H13 120.4 . . ? C2 C3 C4 117.9(3) . . ? C2 C3 H3 121.1 . . ? C4 C3 H3 121.1 . . ? C49 C48 H48 121.3 . . ? C49 C48 C47 117.3(3) . . ? C47 C48 H48 121.3 . . ? C13 C12 H12A 120.6 . . ? C13 C12 C11 118.8(3) . . ? C11 C12 H12A 120.6 . . ? N11 C46 H46 118.6 . . ? N11 C46 C47 122.8(3) . . ? C47 C46 H46 118.6 . . ? N11 C50 N12 120.8(2) . . ? N11 C50 C49 121.7(3) . . ? N12 C50 C49 117.4(2) . . ? C12 C11 H11 120.9 . . ? C10 C11 C12 118.2(3) . . ? C10 C11 H11 120.9 . . ? N3 C10 C11 123.9(3) . . ? N3 C10 H10A 118.0 . . ? C11 C10 H10A 118.0 . . ? N7 C28 H28A 115.1 . . ? N7 C28 H28 120.1 . . ? N7 C28 C29 129.8(4) . . ? N7 C28 C1D 119.8(3) . . ? H28A C28 H28 26.7 . . ? C29 C28 H28A 115.1 . . ? C29 C28 H28 104.9 . . ? C29 C28 C1D 26.2(4) . . ? C1D C28 H28A 118.1 . . ? C1D C28 H28 120.1 . . ? C48 C47 C46 119.0(3) . . ? C48 C47 H47 120.5 . . ? C46 C47 H47 120.5 . . ? C30 C31 H31 116.1 . . ? C1C C31 H31 116.1 . . ? C1C C31 C30 127.8(5) . . ? O41 Cl5 O40 108.6(2) . . ? O39 Cl5 O41 113.4(3) . . ? O39 Cl5 O38 109.8(2) . . ? O39 Cl5 O40 111.5(2) . . ? O38 Cl5 O41 106.0(2) . . ? O38 Cl5 O40 107.3(2) . . ? O22 Cl1 O24 103.5(2) . . ? O22 Cl1 O25 109.0(3) . . ? O25 Cl1 O24 102.8(4) . . ? Cl1 O22 Cl2 39.78(16) . . ? Cl1 O22 Cl9 17.0(2) . . ? Cl9 O22 Cl2 39.7(2) . . ? O45 Cl6 O44 107.0(4) . . ? O45 Cl6 O43 131.8(4) . . ? O45 Cl6 H1EB 22.7 . . ? O42 Cl6 O45 103.5(3) . . ? O42 Cl6 O44 93.8(4) . . ? O42 Cl6 O43 111.5(4) . . ? O42 Cl6 H1EB 93.6 . . ? O44 Cl6 H1EB 128.6 . . ? O43 Cl6 O44 102.8(3) . . ? O43 Cl6 H1EB 121.1 . . ? Cl6 O45 H1EA 117.3 . . ? Cl6 O45 H1EB 24.0 . . ? O22 Cl2 O23 122.4(2) . . ? O22 Cl2 O20 102.4(3) . . ? O22 Cl2 O21 111.8(3) . . ? O23 Cl2 O20 101.9(3) . . ? O23 Cl2 O21 111.3(3) . . ? O20 Cl2 O21 104.5(4) . . ? N13 C65 C64 172.6(6) . . ? C65 C64 H64A 109.5 . . ? C65 C64 H64B 109.5 . . ? C65 C64 H64C 109.5 . . ? H64A C64 H64B 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? N15 C60 C61 172.5(8) . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61B 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? N19 C58 C59 164.7(9) . . ? C28 C29 H29 123.8 . . ? C28 C29 C30 112.3(5) . . ? C30 C29 H29 123.8 . . ? C31 C30 H30 122.1 . . ? C29 C30 C31 115.8(5) . . ? C29 C30 H30 122.1 . . ? O37 Cl4 O35 92.0(3) . . ? O37 Cl4 O32 128.1(3) . . ? O37 Cl4 O33 115.3(4) . . ? O37 Cl4 O30 94.2(4) . . ? O37 Cl4 O34 107.3(4) . . ? O37 Cl4 O36 19.3(3) . . ? O31 Cl4 O37 108.1(3) . . ? O31 Cl4 O35 111.51(16) . . ? O31 Cl4 O32 108.80(15) . . ? O31 Cl4 O33 121.5(3) . . ? O31 Cl4 O30 43.9(3) . . ? O31 Cl4 O34 91.1(3) . . ? O31 Cl4 O36 112.43(14) . . ? O32 Cl4 O35 106.68(14) . . ? O32 Cl4 O30 88.1(3) . . ? O33 Cl4 O35 104.4(3) . . ? O33 Cl4 O32 13.9(3) . . ? O33 Cl4 O30 94.6(4) . . ? O33 Cl4 O34 110.3(4) . . ? O30 Cl4 O35 155.2(3) . . ? O34 Cl4 O35 22.2(3) . . ? O34 Cl4 O32 107.0(3) . . ? O34 Cl4 O30 134.7(4) . . ? O36 Cl4 O35 106.70(14) . . ? O36 Cl4 O32 110.56(15) . . ? O36 Cl4 O33 98.8(3) . . ? O36 Cl4 O30 85.6(3) . . ? O36 Cl4 O34 124.8(3) . . ? O54 Cl8 O55 81.9(3) . . ? O1H Cl8 O54 115.7(3) . . ? O1H Cl8 O55 122.1(3) . . ? O1I Cl8 O54 112.1(3) . . ? O1I Cl8 O55 100.3(3) . . ? O1I Cl8 O1H 118.7(3) . . ? H52C O52 H52D 109.6 . . ? O26 Cl3 O27 108.7(3) . . ? O26 Cl3 O29 107.2(3) . . ? O26 Cl3 O28 108.0(3) . . ? O27 Cl3 O29 115.4(3) . . ? O27 Cl3 O28 107.0(3) . . ? O28 Cl3 O29 110.2(3) . . ? O48 Cl7 O46 109.6(3) . . ? O48 Cl7 O49 113.1(3) . . ? O48 Cl7 O47 109.8(3) . . ? O49 Cl7 O46 104.4(3) . . ? O49 Cl7 O47 114.7(3) . . ? O47 Cl7 O46 104.6(3) . . ? H51A O51 H51B 109.3 . . ? N25 C62 C63 174.8(11) . . ? C1B C1A H1A 120.1 . . ? C1B C1A C1D 119.8(4) . . ? C1D C1A H1A 120.1 . . ? C32 C1B H1B 123.5 . . ? C1A C1B C32 113.1(4) . . ? C1A C1B H1B 123.5 . . ? N7 C1C C31 113.7(5) . . ? N14 C1C N7 122.4(5) . . ? N14 C1C C31 123.2(5) . . ? C28 C1D C1A 123.2(4) . . ? C28 C1D H1D 118.4 . . ? C1A C1D H1D 118.4 . . ? C33 N14 H14 104.5 . . ? C1C N14 C33 130.1(5) . . ? C1C N14 H14 105.3 . . ? O22 Cl9 O1C 95.4(5) . . ? O22 Cl9 O1D 112.2(5) . . ? O1D Cl9 O1C 102.4(7) . . ? O56 Cl10 O53 111.4(2) . . ? O56 Cl10 O1J 115.5(2) . . ? O53 Cl10 O1J 97.5(2) . . ? O1F Cl10 O56 109.1(2) . . ? O1F Cl10 O53 115.7(2) . . ? O1F Cl10 O1J 107.4(2) . . ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.380 0.564 0.914 89 30 ' ' 2 0.380 0.936 0.414 88 30 ' ' 3 0.311 0.130 0.498 10 2 ' ' 4 0.311 0.370 0.998 10 2 ' ' 5 0.620 0.064 0.586 89 30 ' ' 6 0.619 0.436 0.086 88 30 ' ' 7 0.689 0.630 0.002 10 2 ' ' 8 0.688 0.870 0.502 10 2 ' ' _platon_squeeze_details ; ; _iucr_refine_instructions_details ; TITL MER27 in P21/c #14 CELL 1.54184 16.255641 22.857152 25.587356 90 102.0441 90 ZERR 4 0.000246 0.000374 0.000368 0 0.0015 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl Fe N O UNIT 232 284 20 20 56 180 DFIX 2.29 O26 O27 O26 O28 O26 O29 O27 O28 O27 O29 O28 O29 DFIX 1.15 N15 C60 DFIX 1.15 N25 C62 DFIX 1.15 N19 C58 DFIX 2.29 O46 O47 O46 O48 O46 O49 O47 O48 O47 O49 O48 O49 DFIX 1.45 C63 C62 DFIX 1.45 C60 C61 DFIX 1.45 C58 C59 DFIX 2 H2Ba H64a DFIX 1.39 C28 C29 DFIX 1.39 C29 C30 DFIX 1.39 C30 C31 DFIX 1.39 N7 C28 DFIX 1.39 N7 C32 DFIX 1.39 C32 C1B DFIX 1.39 C1B C1A DFIX 1.39 C1A C1D DFIX 1.39 C1D C28 DFIX 1.39 C31 C1C DFIX 1.39 C1C N7 DFIX 1.44 Cl10 O56 Cl10 O53 Cl10 O1F Cl10 O1J DFIX 1.44 Cl4 O37 Cl4 O35 Cl4 O31 Cl4 O32 Cl4 O33 Cl4 O30 Cl4 O34 Cl4 O36 DFIX 1.44 Cl7 O46 Cl7 O47 Cl7 O48 Cl7 O49 DFIX 1.44 Cl7 O48 Cl7 O46 Cl7 O49 Cl7 O47 DFIX 1.44 Cl3 O26 Cl3 O27 Cl3 O28 Cl3 O29 DFIX 1.44 Cl3 O26 Cl3 O27 Cl3 O29 Cl3 O28 DFIX 1.44 Cl2 O22 Cl2 O23 Cl2 O20 Cl2 O21 DFIX 1.44 Cl1 O22 Cl1 O23 Cl1 O24 Cl1 O25 DFIX 1.44 Cl9 O1D DFIX 1.44 Cl9 O24 DFIX 1.44 Cl9 O22 Cl9 O1C DFIX 1.44 Cl6 O45 Cl6 O42 Cl6 O44 Cl6 O43 DFIX 1.44 Cl8 O54 Cl8 O55 Cl8 O1H Cl8 O1I DFIX 1.44 Cl5 O41 Cl5 O39 Cl5 O38 Cl5 O40 DANG 2.3 O22 O1C SIMU C30 C29 SIMU Cl1 O24 O22 O25 O23 SIMU Cl6 O45 O44 O42 O43 EADP O34 O35 EADP O31 O30 EADP O32 O33 EADP O36 O37 EADP N25 C62 C63 EADP N14 C1C EADP Cl10 O1F O53 O56 O1J EADP O48 Cl7 O47 O49 O46 EADP O27 O26 O28 Cl3 O29 EADP Cl1 O22 O24 O25 Cl2 Cl9 O23 O20 O21 O1C O1D EADP O45 Cl6 O44 O42 O43 EADP Cl8 O1I O1H O54 O55 L.S. 10 0 0 511 PLAN 20 DAMP 10000 REM reset to P21/c #14 BOND $H more -1 fmap 2 acta OMIT -2 134 REM D:/Structures/MER27/MER27/Squeeze/mer27squeeze-sr.hkl WGHT 0.200000 FVAR 1.29147 FE1 4 0.789869 0.434711 0.430920 11.00000 0.02566 0.01946 = 0.02285 -0.00096 -0.00230 0.00082 FE2 4 0.672211 0.437500 0.309588 11.00000 0.02583 0.02324 = 0.02431 -0.00211 -0.00309 0.00197 FE3 4 0.879450 0.440972 0.327900 11.00000 0.02569 0.02368 = 0.02316 -0.00243 -0.00278 0.00104 FE4 4 0.755060 0.690247 0.331479 11.00000 0.04837 0.02543 = 0.03329 0.00610 0.00682 0.00504 FE5 4 0.777399 0.185992 0.323089 11.00000 0.04219 0.03128 = 0.05274 -0.01642 -0.01343 0.00653 O1A 6 0.779647 0.437628 0.355521 11.00000 0.02096 0.02358 = 0.03037 -0.01066 0.00026 0.00082 O3 6 0.837090 0.499262 0.270093 11.00000 0.03359 0.03500 = 0.03407 0.00297 0.00030 0.00485 O15 6 0.845271 0.378762 0.272392 11.00000 0.02898 0.03777 = 0.03644 -0.01331 -0.00253 -0.00045 O1B 6 0.555810 0.439188 0.256652 11.00000 0.03472 0.03166 = 0.04102 -0.00264 -0.00431 0.00023 AFIX 7 H1BA 2 0.522981 0.408867 0.261192 11.00000 -1.50000 H1BB 2 0.562050 0.436878 0.222812 11.00000 -1.50000 AFIX 0 O2 6 0.696911 0.501429 0.261480 11.00000 0.03472 0.03002 = 0.03312 0.00507 -0.00962 0.00174 O3B 6 0.989771 0.446039 0.298870 11.00000 0.03509 0.03321 = 0.02353 0.00118 -0.00051 0.00279 AFIX 7 H3BA 2 0.984352 0.426506 0.269931 11.00000 -1.50000 H3BB 2 1.030302 0.432482 0.322371 11.00000 -1.50000 AFIX 0 O12 6 0.697279 0.376740 0.429470 11.00000 0.04122 0.04296 = 0.02610 -0.00712 -0.00126 -0.01963 O2B 6 0.801032 0.431762 0.513638 11.00000 0.03838 0.02835 = 0.02733 -0.00260 0.00037 -0.00630 AFIX 7 H2BA 2 0.775637 0.400874 0.523278 11.00000 -1.50000 H2BB 2 0.778146 0.462903 0.524679 11.00000 -1.50000 AFIX 0 O6 6 0.709197 0.501681 0.431553 11.00000 0.04036 0.04057 = 0.02696 -0.00338 0.00067 0.01951 O7 6 0.860121 0.640270 0.368340 11.00000 0.04216 0.02808 = 0.02875 0.00383 0.00342 -0.00439 O8 6 0.928699 0.510610 0.373909 11.00000 0.03205 0.02977 = 0.02835 -0.00608 0.00092 -0.00661 O18 6 0.870307 0.367329 0.442742 11.00000 0.03814 0.03332 = 0.03476 -0.00028 0.00214 0.00995 O5 6 0.620380 0.495788 0.352651 11.00000 0.03388 0.03161 = 0.02884 -0.00250 -0.00640 0.00700 O17 6 0.940641 0.379751 0.377798 11.00000 0.02746 0.03803 = 0.02978 0.00682 -0.00312 0.00600 O1 6 0.726700 0.632608 0.267841 11.00000 0.04746 0.03296 = 0.03279 0.00217 -0.00544 0.00400 O4 6 0.683292 0.648980 0.379170 11.00000 0.05217 0.03000 = 0.02460 -0.00078 0.00367 0.00124 O9 6 0.884288 0.490717 0.448362 11.00000 0.03776 0.02986 = 0.03141 0.00167 -0.00128 -0.00942 N10 5 0.989840 0.190589 0.336970 11.00000 0.03284 0.03688 = 0.04815 -0.01278 -0.00077 0.01437 AFIX 43 H10 2 1.043087 0.186105 0.348400 11.00000 -1.20000 AFIX 0 O11 6 0.623599 0.372178 0.345983 11.00000 0.03386 0.03080 = 0.03819 0.00632 -0.00938 -0.00122 O13 6 0.742083 0.245791 0.262278 11.00000 0.04167 0.03779 = 0.05195 -0.01482 -0.01646 0.00206 O14 6 0.704466 0.380031 0.256993 11.00000 0.02759 0.03844 = 0.03115 -0.01075 -0.00579 0.00610 O16 6 0.878631 0.240741 0.356628 11.00000 0.03435 0.03190 = 0.05984 -0.01874 -0.01119 0.00986 O10 6 0.700509 0.224311 0.369640 11.00000 0.05071 0.02581 = 0.04712 -0.00603 -0.00777 0.00411 N6 5 0.966861 0.694282 0.347371 11.00000 0.05224 0.02911 = 0.04091 0.01036 -0.00171 -0.01116 AFIX 43 H6 2 1.019544 0.701258 0.358759 11.00000 -1.20000 AFIX 0 C18 1 0.645110 0.516690 0.398478 11.00000 0.02955 0.02147 = 0.02965 0.00214 0.00336 0.00213 C26 1 0.965609 0.575451 0.448259 11.00000 0.03393 0.02557 = 0.02449 0.00078 -0.00286 -0.00113 AFIX 23 H26A 2 1.010858 0.562542 0.476923 11.00000 -1.20000 H26B 2 0.925807 0.596833 0.464447 11.00000 -1.20000 AFIX 0 N1 5 0.640879 0.734451 0.289671 11.00000 0.05183 0.03193 = 0.04561 0.01423 0.01125 0.01390 N3 5 0.789432 0.750183 0.400770 11.00000 0.04697 0.03662 = 0.04923 -0.00022 0.01068 -0.00406 C27 1 0.922230 0.522470 0.421270 11.00000 0.02705 0.01884 = 0.02502 0.00087 -0.00531 -0.00169 N5 5 0.845542 0.729759 0.288560 11.00000 0.05957 0.02670 = 0.03080 0.00744 0.00805 0.00056 C15 1 0.688122 0.649539 0.427369 11.00000 0.03270 0.02175 = 0.04166 0.00231 -0.00098 0.01181 C17 1 0.590683 0.563428 0.417278 11.00000 0.02613 0.03676 = 0.02850 0.00136 -0.00103 0.00884 AFIX 23 H17A 2 0.558520 0.583501 0.386251 11.00000 -1.20000 H17B 2 0.551059 0.544393 0.435303 11.00000 -1.20000 AFIX 0 C8 1 0.757288 0.551259 0.196949 11.00000 0.04404 0.03825 = 0.01990 0.00014 -0.00058 0.00237 AFIX 23 H8A 2 0.759523 0.525431 0.167198 11.00000 -1.20000 H8B 2 0.805438 0.577240 0.201470 11.00000 -1.20000 AFIX 0 N9 5 0.868779 0.148398 0.279419 11.00000 0.05385 0.02969 = 0.05143 -0.01585 -0.00649 0.01148 C54 1 0.772277 0.364507 0.246079 11.00000 0.03427 0.02742 = 0.02427 -0.01027 -0.00189 0.00206 N4 5 0.735259 0.688441 0.461127 11.00000 0.04842 0.04974 = 0.02714 0.00247 -0.00771 -0.00666 AFIX 43 H4 2 0.738539 0.681232 0.494487 11.00000 -1.20000 AFIX 0 N11 5 0.667002 0.138490 0.280279 11.00000 0.05403 0.03373 = 0.06205 -0.02368 -0.01731 0.00724 C45 1 0.925223 0.352888 0.418182 11.00000 0.03449 0.01681 = 0.02535 -0.00826 -0.00594 -0.00183 C7 1 0.677170 0.587557 0.183468 11.00000 0.04776 0.04413 = 0.03073 0.00669 -0.00382 -0.00293 AFIX 23 H7A 2 0.674415 0.607032 0.149464 11.00000 -1.20000 H7B 2 0.628778 0.561908 0.179907 11.00000 -1.20000 AFIX 0 C9 1 0.763582 0.515131 0.246818 11.00000 0.03908 0.02059 = 0.03355 -0.00067 -0.00640 -0.00478 C14 1 0.779411 0.738301 0.450772 11.00000 0.04021 0.04695 = 0.03394 0.00240 0.00720 0.00689 C36 1 0.642079 0.354788 0.393539 11.00000 0.02963 0.03057 = 0.03163 -0.00267 0.00149 0.00298 C44 1 0.980731 0.302431 0.440260 11.00000 0.03154 0.02590 = 0.03426 -0.00332 -0.00829 0.00499 AFIX 23 H44A 2 0.948093 0.274925 0.456479 11.00000 -1.20000 H44B 2 1.025905 0.316861 0.468230 11.00000 -1.20000 AFIX 0 N2 5 0.610397 0.671960 0.214872 11.00000 0.05319 0.05625 = 0.04545 0.01180 0.00082 0.02201 AFIX 43 H2 2 0.576924 0.667028 0.184402 11.00000 -1.20000 AFIX 0 C43 1 1.018577 0.270418 0.399609 11.00000 0.03594 0.03620 = 0.05390 -0.01673 -0.00988 0.01238 AFIX 23 H43A 2 1.064297 0.245981 0.418067 11.00000 -1.20000 H43B 2 1.041971 0.298703 0.378473 11.00000 -1.20000 AFIX 0 C24 1 0.936161 0.650887 0.374498 11.00000 0.04364 0.02565 = 0.02693 -0.00068 -0.00103 -0.00701 PART 2 O37 6 0.246069 0.456021 0.435409 10.25000 0.03801 0.05748 = 0.04370 -0.01113 -0.00677 -0.01054 PART 0 C16 1 0.639860 0.607910 0.454368 11.00000 0.03747 0.02522 = 0.03211 -0.00036 0.00559 0.01077 AFIX 23 H16A 2 0.601333 0.629972 0.471072 11.00000 -1.20000 H16B 2 0.678780 0.587622 0.482418 11.00000 -1.20000 AFIX 0 C6 1 0.673807 0.632750 0.225992 11.00000 0.04849 0.03121 = 0.03279 0.00860 0.00550 0.00019 C51 1 0.692593 0.243780 0.219171 11.00000 0.03576 0.03178 = 0.05168 -0.01838 -0.00582 0.00388 C52 1 0.692122 0.292879 0.179408 11.00000 0.03451 0.04823 = 0.04223 -0.02077 -0.00497 0.00708 AFIX 23 H52A 2 0.641926 0.316374 0.177650 11.00000 -1.20000 H52B 2 0.690019 0.276300 0.144257 11.00000 -1.20000 AFIX 0 C42 1 0.954519 0.232002 0.362069 11.00000 0.04043 0.03221 = 0.03794 -0.01487 -0.00930 0.01027 C53 1 0.770182 0.332448 0.194379 11.00000 0.04492 0.04725 = 0.03853 -0.02078 0.00130 -0.00083 AFIX 23 H53A 2 0.820513 0.308750 0.197727 11.00000 -1.20000 H53B 2 0.769985 0.360633 0.166012 11.00000 -1.20000 AFIX 0 N12 5 0.636200 0.200609 0.204831 11.00000 0.04413 0.04941 = 0.05791 -0.02597 -0.01621 -0.00392 AFIX 43 H12 2 0.607942 0.202564 0.172479 11.00000 -1.20000 AFIX 0 C41 1 0.953510 0.153537 0.295068 11.00000 0.05052 0.02788 = 0.04002 -0.00501 0.00141 0.00835 PART 1 N8 5 0.757354 0.189966 0.454577 10.60000 0.06123 0.01641 = 0.02544 -0.00138 -0.00641 0.01240 AFIX 43 H8 2 0.756873 0.196878 0.487550 10.60000 -1.20000 AFIX 0 PART 0 C33 1 0.707579 0.225332 0.419712 11.00000 0.07912 0.03221 = 0.04461 -0.01279 -0.02108 0.00362 C40 1 1.007756 0.121742 0.269350 11.00000 0.05488 0.02735 = 0.04889 -0.00084 0.00750 0.01677 AFIX 43 H40 2 1.065688 0.125404 0.280873 11.00000 -1.20000 AFIX 0 PART 1 O35 6 0.120106 0.484100 0.418138 10.75000 0.04763 0.04275 = 0.05944 -0.01264 0.00216 -0.00047 PART 0 C25 1 1.001608 0.616908 0.413442 11.00000 0.04213 0.02160 = 0.02911 0.00213 -0.00271 -0.00658 AFIX 23 H25A 2 1.035751 0.594860 0.393490 11.00000 -1.20000 H25B 2 1.038263 0.644379 0.436085 11.00000 -1.20000 AFIX 0 C23 1 0.928877 0.729360 0.304731 11.00000 0.05131 0.02596 = 0.03368 0.00131 0.00757 -0.00286 C34 1 0.648989 0.259458 0.446238 11.00000 0.07489 0.02801 = 0.03248 -0.00446 -0.00215 -0.00064 AFIX 23 H34A 2 0.681831 0.280462 0.476451 11.00000 -1.20000 H34B 2 0.612708 0.232333 0.459918 11.00000 -1.20000 AFIX 0 N7 5 0.819292 0.129911 0.394251 11.00000 0.07060 0.04205 = 0.05357 -0.00466 -0.00907 0.01500 C19 1 0.814070 0.762782 0.244830 11.00000 0.05911 0.03497 = 0.04112 0.01431 -0.00316 0.00810 AFIX 43 H19 2 0.756180 0.762168 0.231957 11.00000 -1.20000 AFIX 0 C21 1 0.944629 0.797732 0.238221 11.00000 0.09927 0.02799 = 0.04204 0.00583 0.00405 -0.01861 AFIX 43 H21 2 0.978229 0.822420 0.222704 11.00000 -1.20000 AFIX 0 C35 1 0.594308 0.303152 0.409269 11.00000 0.03787 0.02689 = 0.03353 -0.00425 0.00038 -0.00337 AFIX 23 H35A 2 0.566568 0.282872 0.377098 11.00000 -1.20000 H35B 2 0.550962 0.317612 0.426867 11.00000 -1.20000 AFIX 0 C1 1 0.615089 0.778852 0.317310 11.00000 0.07161 0.04663 = 0.06431 0.01452 0.01873 0.01794 AFIX 43 H1 2 0.648519 0.789595 0.349983 11.00000 -1.20000 AFIX 0 C22 1 0.979798 0.763451 0.279982 11.00000 0.07210 0.03512 = 0.05079 0.00686 0.00828 -0.02553 AFIX 43 H22 2 1.037877 0.762802 0.291990 11.00000 -1.20000 AFIX 0 C38 1 0.890583 0.081790 0.210327 11.00000 0.07948 0.03991 = 0.03806 -0.01419 -0.01187 0.01434 AFIX 43 H38 2 0.866777 0.059541 0.180577 11.00000 -1.20000 AFIX 0 PART 1 O31 6 0.151561 0.387322 0.451893 10.75000 0.04963 0.06085 = 0.04357 0.00707 0.00422 -0.00777 C32 1 0.810864 0.142934 0.446377 10.60000 0.06347 0.03215 = 0.02429 0.00477 -0.00099 0.01589 PART 0 C5 1 0.590032 0.718869 0.244242 11.00000 0.05923 0.03542 = 0.04575 0.02056 0.01266 0.01997 C37 1 0.840439 0.112409 0.238758 11.00000 0.06022 0.04117 = 0.05552 -0.01375 -0.01049 0.00919 AFIX 43 H37 2 0.782534 0.107357 0.228574 11.00000 -1.20000 AFIX 0 C2 1 0.539968 0.809230 0.298571 11.00000 0.06962 0.05811 = 0.06436 0.01836 0.01801 0.02577 AFIX 43 H2A 2 0.525669 0.841025 0.317542 11.00000 -1.20000 AFIX 0 C4 1 0.512371 0.744648 0.225428 11.00000 0.06033 0.04084 = 0.05386 0.01606 0.00909 0.01661 AFIX 43 H4A 2 0.476893 0.730220 0.194859 11.00000 -1.20000 AFIX 0 C20 1 0.860132 0.796118 0.218901 11.00000 0.06559 0.03625 = 0.04789 0.01321 0.00624 0.00465 AFIX 43 H20 2 0.835281 0.817416 0.188761 11.00000 -1.20000 AFIX 0 C49 1 0.541351 0.124448 0.213840 11.00000 0.05807 0.03713 = 0.07139 -0.02086 -0.01958 -0.00013 AFIX 43 H49 2 0.507048 0.137188 0.182140 11.00000 -1.20000 AFIX 0 C39 1 0.975610 0.085310 0.227299 11.00000 0.08037 0.03359 = 0.03917 -0.00795 0.01095 0.01347 AFIX 43 H39 2 1.011219 0.063495 0.210764 11.00000 -1.20000 AFIX 0 C13 1 0.812101 0.773741 0.494298 11.00000 0.04892 0.05415 = 0.05191 -0.00567 -0.00407 -0.01385 AFIX 43 H13 2 0.804828 0.763882 0.528306 11.00000 -1.20000 AFIX 0 C3 1 0.487830 0.791799 0.252192 11.00000 0.06699 0.05834 = 0.06918 0.03923 0.02491 0.03756 AFIX 43 H3 2 0.437385 0.811102 0.239069 11.00000 -1.20000 AFIX 0 C48 1 0.516948 0.077447 0.239818 11.00000 0.07532 0.04276 = 0.08808 -0.01675 -0.02198 -0.01511 AFIX 43 H48 2 0.467446 0.057347 0.225998 11.00000 -1.20000 AFIX 0 C12 1 0.854729 0.822871 0.486531 11.00000 0.07595 0.05858 = 0.06330 -0.01042 0.00794 -0.01344 AFIX 43 H12A 2 0.875958 0.847707 0.514935 11.00000 -1.20000 AFIX 0 PART 2 O54 6 0.818982 0.309669 0.541336 10.50000 0.11587 0.15350 = 0.03899 -0.00643 0.00204 -0.07827 PART 0 C46 1 0.642969 0.092738 0.307042 11.00000 0.08951 0.03886 = 0.07564 -0.01400 -0.03289 -0.01391 AFIX 43 H46 2 0.676819 0.081973 0.339569 11.00000 -1.20000 AFIX 0 C50 1 0.616589 0.153790 0.233781 11.00000 0.05214 0.03284 = 0.05449 -0.01972 -0.01613 0.00035 C11 1 0.866241 0.835573 0.434979 11.00000 0.10042 0.04728 = 0.07145 -0.01610 0.03786 -0.03284 AFIX 43 H11 2 0.896971 0.868158 0.428600 11.00000 -1.20000 AFIX 0 C10 1 0.830892 0.798576 0.394068 11.00000 0.08261 0.03707 = 0.06861 -0.00863 0.02353 -0.00772 AFIX 43 H10A 2 0.836412 0.808087 0.359627 11.00000 -1.20000 AFIX 0 C28 1 0.869483 0.084538 0.389249 11.00000 0.09673 0.04685 = 0.05324 -0.01014 -0.00581 0.02604 PART 2 AFIX 43 H28A 2 0.853206 0.062834 0.358059 10.50000 -1.20000 AFIX 43 PART 0 PART 1 H28 2 0.874945 0.072154 0.355519 10.50000 -1.20000 AFIX 0 PART 0 C47 1 0.569151 0.060790 0.287858 11.00000 0.08463 0.04319 = 0.11081 -0.00436 -0.02343 -0.01384 AFIX 43 H47 2 0.555266 0.028951 0.306938 11.00000 -1.20000 AFIX 0 PART 2 O55 6 0.906939 0.254312 0.565594 10.50000 0.11587 0.15350 = 0.03899 -0.00643 0.00204 -0.07827 C31 1 0.901044 0.138334 0.477957 10.40000 0.05571 0.05440 = 0.03721 -0.00181 -0.00534 0.00906 AFIX 43 H31 2 0.912145 0.157464 0.510756 10.40000 -1.20000 AFIX 0 PART 0 PART 1 CL5 3 0.346260 0.268763 0.407110 10.50000 0.03840 0.03999 = 0.03118 -0.01983 0.00770 -0.02128 O41 6 0.330927 0.207251 0.407290 10.50000 0.05942 0.02865 = 0.08182 -0.01429 0.01830 -0.01475 O39 6 0.363608 0.289408 0.358309 10.50000 0.05518 0.10008 = 0.02558 -0.02069 0.01454 -0.03308 O38 6 0.272061 0.296012 0.416739 10.50000 0.04916 0.04121 = 0.02853 0.00824 0.00354 0.00216 O40 6 0.413887 0.282727 0.451956 10.50000 0.05534 0.07850 = 0.03997 -0.01713 -0.00027 -0.02570 PART 0 PART 2 CL1 3 0.030333 0.944431 0.349528 10.40000 0.13076 0.09063 = 0.04907 0.00444 0.02609 0.00305 PART 0 O22 6 -0.001559 0.930941 0.392279 11.00000 0.13076 0.09063 = 0.04907 0.00444 0.02609 0.00305 PART 1 O23 6 0.028066 0.908431 0.304792 10.80000 0.13076 0.09063 = 0.04907 0.00444 0.02609 0.00305 PART 0 PART 2 O24 6 0.122379 0.944201 0.370691 10.60000 0.13076 0.09063 = 0.04907 0.00444 0.02609 0.00305 CL6 3 0.489381 0.246269 0.560079 10.50000 0.09183 0.11552 = 0.09775 0.00370 0.00777 0.03064 O45 6 0.539895 0.283600 0.596161 10.50000 0.09183 0.11552 = 0.09775 0.00370 0.00777 0.03064 PART 0 PART 1 CL2 3 -0.024168 0.931209 0.337119 10.40000 0.13076 0.09063 = 0.04907 0.00444 0.02609 0.00305 PART 0 PART 2 N13 5 0.675977 0.432720 0.642230 10.50000 0.06245 C65 1 0.649820 0.418998 0.597580 10.50000 0.04632 C64 1 0.612281 0.409399 0.539240 10.50000 0.05953 AFIX 137 H64A 2 0.653550 0.418129 0.518455 10.50000 -1.50000 H64B 2 0.564498 0.434594 0.528469 10.50000 -1.50000 H64C 2 0.594869 0.369354 0.533613 10.50000 -1.50000 AFIX 0 N15 5 0.388838 0.424962 0.264877 10.50000 0.08199 C60 1 0.318639 0.433350 0.264600 10.50000 0.07396 C61 1 0.234660 0.444377 0.271707 10.50000 0.09609 AFIX 137 H61A 2 0.197671 0.448817 0.237414 10.50000 -1.50000 H61B 2 0.234078 0.479559 0.292119 10.50000 -1.50000 H61C 2 0.216112 0.412124 0.290337 10.50000 -1.50000 AFIX 0 PART 0 PART 1 N19 5 0.424077 0.431292 0.374957 10.50000 0.09128 C58 1 0.451965 0.435373 0.418597 10.50000 0.09479 C59 1 0.503739 0.430052 0.470819 10.50000 0.14045 AFIX 137 H59A 2 0.552979 0.407635 0.468939 10.50000 -1.50000 H59B 2 0.472838 0.410668 0.493911 10.50000 -1.50000 H59C 2 0.520204 0.468274 0.484713 10.50000 -1.50000 AFIX 0 PART 0 PART 2 O25 6 0.013471 1.003938 0.336499 10.40000 0.13076 0.09063 = 0.04907 0.00444 0.02609 0.00305 PART 0 PART 1 O20 6 -0.092470 0.891742 0.327098 10.40000 0.13076 0.09063 = 0.04907 0.00444 0.02609 0.00305 O21 6 -0.059562 0.985699 0.317190 10.40000 0.13076 0.09063 = 0.04907 0.00444 0.02609 0.00305 PART 0 PART 2 C29 1 0.940875 0.065404 0.423042 10.40000 0.06267 0.09040 = 0.07018 -0.00620 0.01261 -0.02910 AFIX 43 H29 2 0.978747 0.039253 0.413174 10.40000 -1.20000 AFIX 0 C30 1 0.950452 0.089452 0.473804 10.40000 0.02456 0.08233 = 0.08308 -0.01980 -0.00378 0.01342 AFIX 43 H30 2 0.987512 0.073900 0.503168 10.40000 -1.20000 AFIX 0 PART 0 CL4 3 0.166667 0.428622 0.414489 11.00000 0.03976 0.04702 = 0.03086 -0.00825 -0.00545 -0.00133 PART 1 O32 6 0.135771 0.405602 0.361158 10.75000 0.05051 0.05653 = 0.03830 -0.01591 -0.01279 0.01620 PART 0 PART 2 O42 6 0.544466 0.202612 0.551683 10.50000 0.09183 0.11552 = 0.09775 0.00370 0.00777 0.03064 PART 0 PART 1 O56 6 0.848092 0.279611 0.633969 10.50000 0.08509 0.01832 = 0.03126 0.00930 -0.00864 -0.02186 PART 0 PART 2 CL8 3 0.825313 0.263277 0.580579 10.50000 0.11587 0.15350 = 0.03899 -0.00643 0.00204 -0.07827 O33 6 0.150313 0.415578 0.358021 10.25000 0.05051 0.05653 = 0.03830 -0.01591 -0.01279 0.01620 O30 6 0.196769 0.369599 0.431042 10.25000 0.04963 0.06085 = 0.04357 0.00707 0.00422 -0.00777 O34 6 0.101752 0.466609 0.426526 10.25000 0.04763 0.04275 = 0.05944 -0.01264 0.00216 -0.00047 PART 0 PART 1 O36 6 0.254041 0.443807 0.421940 10.75000 0.03801 0.05748 = 0.04370 -0.01113 -0.00677 -0.01054 O53 6 0.768704 0.220348 0.567887 10.50000 0.08509 0.01832 = 0.03126 0.00930 -0.00864 -0.02186 O50 6 0.324101 0.466372 0.066730 10.50000 0.10009 PART 0 AFIX 6 O52 6 0.838752 0.834029 0.627939 11.00000 0.05222 0.07445 = 0.06853 -0.01698 -0.00425 0.00685 H52C 2 0.854461 0.854580 0.604060 11.00000 -1.50000 H52D 2 0.797864 0.812467 0.613559 11.00000 -1.50000 AFIX 0 PART 2 CL3 3 0.415819 0.909300 0.579151 10.50000 10.12000 PART 0 PART 1 O48 6 0.501327 0.156162 0.388120 10.50000 10.12000 CL7 3 0.519899 0.112131 0.426832 10.50000 10.12000 PART 0 AFIX 6 O51 6 0.843761 0.947863 0.579881 11.00000 0.13434 H51A 2 0.836810 0.984772 0.579194 11.00000 -1.50000 H51B 2 0.796142 0.931061 0.576247 11.00000 -1.50000 AFIX 0 PART 1 O46 6 0.455830 0.110702 0.458119 10.50000 10.12000 PART 0 PART 2 O26 6 0.332528 0.890310 0.573472 10.50000 10.12000 PART 0 PART 1 O49 6 0.518422 0.055058 0.404551 10.50000 10.12000 PART 0 PART 2 O27 6 0.421611 0.967349 0.598319 10.50000 10.12000 O29 6 0.468728 0.867141 0.612959 10.50000 10.12000 O44 6 0.482823 0.271631 0.506998 10.50000 0.09183 0.11552 = 0.09775 0.00370 0.00777 0.03064 O43 6 0.405951 0.223471 0.557920 10.50000 0.09183 0.11552 = 0.09775 0.00370 0.00777 0.03064 PART 0 PART 1 O47 6 0.595848 0.126441 0.464528 10.50000 10.12000 N25 5 0.383822 0.424857 0.241657 10.50000 0.11012 C62 1 0.310678 0.429857 0.233517 10.50000 0.11012 C63 1 0.221049 0.439819 0.219710 10.50000 0.11012 AFIX 137 H63A 2 0.206122 0.455499 0.184184 10.50000 -1.50000 H63B 2 0.205423 0.467081 0.244477 10.50000 -1.50000 H63C 2 0.192007 0.403500 0.221289 10.50000 -1.50000 AFIX 0 PART 0 PART 2 O28 6 0.435778 0.910511 0.526772 10.50000 10.12000 PART 0 PART 1 C1A 1 0.910354 0.074136 0.485707 10.60000 0.11684 0.09824 = 0.04038 0.00204 -0.01011 0.08697 AFIX 43 H1A 2 0.940978 0.053795 0.514844 10.60000 -1.20000 AFIX 0 C1B 1 0.862183 0.122200 0.493704 10.60000 0.11589 0.09464 = 0.04710 0.01576 0.00024 0.06206 AFIX 43 H1B 2 0.863803 0.138918 0.527040 10.60000 -1.20000 AFIX 0 PART 0 PART 2 C1C 1 0.837569 0.161822 0.439256 10.40000 0.08705 0.03373 = 0.03600 -0.01081 -0.01831 -0.00358 PART 0 PART 1 C1D 1 0.912678 0.056497 0.433999 10.60000 0.08579 0.05836 = 0.06493 0.00275 0.01454 0.04486 AFIX 43 H1D 2 0.945133 0.024086 0.429571 10.60000 -1.20000 AFIX 0 PART 0 PART 2 N14 5 0.790608 0.206782 0.448211 10.40000 0.08705 0.03373 = 0.03600 -0.01081 -0.01831 -0.00358 AFIX 3 H14 2 0.785698 0.203062 0.480871 10.40000 -1.20000 AFIX 0 PART 0 PART 3 CL9 3 0.033640 0.927211 0.348862 10.20000 0.13076 0.09063 = 0.04907 0.00444 0.02609 0.00305 O1C 6 0.066226 0.866999 0.360092 10.20000 0.13076 0.09063 = 0.04907 0.00444 0.02609 0.00305 O1D 6 -0.028710 0.919617 0.299933 10.20000 0.13076 0.09063 = 0.04907 0.00444 0.02609 0.00305 PART 0 PART 1 AFIX 6 O1E 6 0.507082 0.288018 0.601401 10.50000 0.03675 0.09132 = 0.03865 -0.00182 -0.01696 0.04117 H1EA 2 0.534908 0.315638 0.591078 10.50000 -1.50000 H1EB 2 0.517711 0.256118 0.587031 10.50000 -1.50000 AFIX 0 O1F 6 0.774572 0.324260 0.558500 10.50000 0.08509 0.01832 = 0.03126 0.00930 -0.00864 -0.02186 CL10 3 0.816223 0.272717 0.578916 10.50000 0.08509 0.01832 = 0.03126 0.00930 -0.00864 -0.02186 PART 0 PART 2 O1H 6 0.760346 0.220402 0.570365 10.50000 0.11587 0.15350 = 0.03899 -0.00643 0.00204 -0.07827 O1I 6 0.852273 0.284200 0.633138 10.50000 0.11587 0.15350 = 0.03899 -0.00643 0.00204 -0.07827 PART 0 PART 1 O1J 6 0.879136 0.259656 0.546731 10.50000 0.08509 0.01832 = 0.03126 0.00930 -0.00864 -0.02186 HKLF 4 REM MER27 in P21/c #14 REM R1 = 0.0998 for 10965 Fo > 4sig(Fo) and 0.1325 for all 16567 data REM 1199 parameters refined using 137 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 1.402, deepest hole -1.684, 1-sigma level 0.164 Q1 1 0.2564 0.4561 0.1201 11.00000 0.05 1.40 Q2 1 0.2371 0.4487 0.1734 11.00000 0.05 1.34 Q3 1 0.4803 0.4318 0.4405 11.00000 0.05 1.29 Q4 1 0.3379 0.2863 0.3935 11.00000 0.05 1.29 Q5 1 0.3532 0.1423 0.5660 11.00000 0.05 1.22 Q6 1 0.3217 0.4420 0.0816 11.00000 0.05 1.15 Q7 1 0.4482 0.1878 0.5459 11.00000 0.05 1.10 Q8 1 0.6687 0.6985 0.3084 11.00000 0.05 1.07 Q9 1 0.1726 0.4655 0.0215 11.00000 0.05 1.03 Q10 1 0.7125 0.3020 0.5835 11.00000 0.05 0.99 Q11 1 0.4776 0.0675 0.4485 11.00000 0.05 0.98 Q12 1 0.2689 0.4793 0.0894 11.00000 0.05 0.96 Q13 1 0.2183 0.4657 0.0675 11.00000 0.05 0.95 Q14 1 0.3738 0.0772 0.4818 11.00000 0.05 0.94 Q15 1 0.3505 0.3216 0.3532 11.00000 0.05 0.93 Q16 1 0.6646 0.4596 0.6568 11.00000 0.05 0.93 Q17 1 0.7804 0.7000 0.4358 11.00000 0.05 0.87 Q18 1 0.7455 0.1857 0.3281 11.00000 0.05 0.85 Q19 1 0.7955 0.6877 0.3280 11.00000 0.05 0.82 Q20 1 0.6860 0.4216 0.6297 11.00000 0.05 0.81 REM The information below was added by Olex2. REM REM R1 = 0.0998 for 10965 Fo > 4sig(Fo) and 0.1325 for all 56674 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.40, deepest hole -1.68 REM Mean Shift 0.001, Max Shift 0. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1325 REM R1_gt = 0.0998 REM wR_ref = 0.3250 REM GOOF = 1.195 REM Shift_max = 0 REM Shift_mean = 0.001 REM Reflections_all = 56674 REM Reflections_gt = 10965 REM Parameters = n/a REM Hole = 1.40 REM Peak = -1.68 REM Flack = n/a ; _database_code_depnum_ccdc_archive 'CCDC 939536' ####################################################################### # # 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_merm _audit_creation_date 2013-05-14 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:59:47, GUI svn.r4466) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C74.5 H89 Co8 N16 O33, 3(Cl O4), 5(C H4 O), 2(H2 O)' _chemical_formula_sum 'C79.50 H113 Cl3 Co8 N16 O52' _chemical_formula_weight 2702.65 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y, -z+1/2' 3 'x+1/2, y+1/2, z' 4 '-x+1/2, y+1/2, -z+1/2' 5 '-x, -y, -z' 6 'x, -y, z-1/2' 7 '-x+1/2, -y+1/2, -z' 8 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.9059(4) _cell_length_b 14.9866(2) _cell_length_c 27.3422(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.2539(15) _cell_angle_gamma 90.00 _cell_volume 10612.8(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10240 _cell_measurement_temperature 120.01(10) _cell_measurement_theta_max 29.2834 _cell_measurement_theta_min 2.6995 _exptl_absorpt_coefficient_mu 1.398 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.91003 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description irregular _exptl_crystal_F_000 5540 _exptl_crystal_size_max 0.149 _exptl_crystal_size_mid 0.113 _exptl_crystal_size_min 0.09 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_unetI/netI 0.0338 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 20971 _diffrn_reflns_theta_full 25.05 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_theta_min 2.72 _diffrn_ambient_temperature 120.01(10) _diffrn_detector_area_resol_mean 10.6501 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -20.00 7.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 13.9943 -94.0000 -81.0000 27 #__ type_ start__ end____ width___ exp.time_ 2 omega -37.00 46.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 13.9943 -57.0000 -90.0000 83 #__ type_ start__ end____ width___ exp.time_ 3 omega 1.00 93.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 13.9943 37.0000 90.0000 92 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0014615000 _diffrn_orient_matrix_UB_12 0.0395864000 _diffrn_orient_matrix_UB_13 0.0141192000 _diffrn_orient_matrix_UB_21 -0.0168092000 _diffrn_orient_matrix_UB_22 0.0190954000 _diffrn_orient_matrix_UB_23 -0.0179508000 _diffrn_orient_matrix_UB_31 -0.0215750000 _diffrn_orient_matrix_UB_32 -0.0175612000 _diffrn_orient_matrix_UB_33 0.0123105000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'SuperNova (Mo) X-ray Source' _diffrn_source_current n/a _diffrn_source_voltage n/a _reflns_number_gt 8002 _reflns_number_total 9391 _reflns_odcompleteness_completeness 99.82 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XLMP, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 1.563 _refine_diff_density_min -1.332 _refine_diff_density_rms 0.089 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 777 _refine_ls_number_reflns 9391 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.0481 _refine_ls_restrained_S_all 5.185 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0166P)^2^+97.1309P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0978 _refine_ls_wR_factor_ref 0.1029 _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. The alcohol hydrogens on the coordinating methanols were located in the electron density map before being restrained to a distance of 0.84 A. The oxygens of the the disordered water (O13) and methanol (O19) were constrained to have the same position and thermal parameters. The C-O distance in this methanol was fixed at 1.5 A, and the alcohol hydrogen was encouraged to point away from the CH3 with an antibumping restraint. The perchlorate anions were restrained to have chemically sensible bond lengths and geometries (DFIX and DANG). The thermal parameters of the oxygen atoms O1C, O1D and O17 were constrained to be roughly equal (EDAP). ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, {H2H,H1H} of O2A, H14 of O16, H19A of O19, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups, {H13A,H13B} of O13, H1B of O1B, H2B of O2B, {H2AA, H2AB} of O2A, H16 of O16 2. Shared sites {O13, O19} 3. Restrained distances O1H-H1H 0.84 with sigma of 0.02 H2H-O2H 0.84 with sigma of 0.02 C13-H16 2 with sigma of 0.02 H14-O14 0.84 with sigma of 0.02 C1A-H19A 2.1 with sigma of 0.02 C1A-O19 1.5 with sigma of 0.005 Cl20-O22A = Cl20-O21A = Cl20-O15 = Cl20-O18 1.44 with sigma of 0.005 Cl10-O14A = Cl10-O12A = Cl10-O13A = Cl10-O11A = Cl10-O17 = Cl10-O1C = Cl10-O1D 1.44 with sigma of 0.005 O1D-O1C 2.3 with sigma of 0.01 O12A-O1C 2.3 with sigma of 0.04 O17-O1D 2.3 with sigma of 0.01 4. Uiso/Uaniso restraints and constraints Uanis(O13) = Uanis(O19) Uanis(O17) = Uanis(O1C) = Uanis(O1D) 5. Others Fixed Sof: O13(0.75) H13A(0.75) H13B(0.75) O14A(0.7) Cl20(0.5) O13A(0.7) O11A(0.7) O15(0.5) O16(0.5) H16(0.5) O18(0.5) O19(0.25) H19A(0.25) C1A(0.25) H1AA(0.25) H1AB(0.25) H1AC(0.25) C1C(0.5) H1CA(0.5) H1CB(0.5) H1CC(0.5) O17(0.3) O1C(0.3) O1D(0.3) 6.a Free rotating group: O2A(H2H,H1H,H2AA,H2AB), O16(H14,H16) 6.b Rotating group: O13(H13A,H13B) 6.c Secondary CH2 refined with riding coordinates: C17(H17A,H17B), C35(H35A,H35B), C16(H16A,H16B), C25(H25A,H25B), C34(H34A, H34B), C26(H26A,H26B), C8(H8A,H8B), C7(H7A,H7B) 6.d Aromatic/amide H refined with riding coordinates: N4(H4), N6(H6), N8(H8), C11(H11), C1(H1), C28(H28), C13(H13), N2(H2), C31(H31), C30(H30), C12(H12), C10(H10), C19(H19), C21(H21), C29(H29), C2(H2A), C22(H22), C20(H20), C3(H3), C4(H4A) 6.e Idealised Me refined as rotating group: C38(H38A,H38B,H38C), C1B(H1BA,H1BB,H1BC), C2B(H2BA,H2BB,H2BC), C1A(H1AA,H1AB, H1AC), C1C(H1CA,H1CB,H1CC) 6.f Idealised tetrahedral OH refined as rotating group: O1B(H1B), O2B(H2B) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Co2 Co 0.43373(4) 0.16507(7) 0.29601(3) 0.0146(3) Uani 1 1 d . . . Co3 Co 0.44820(4) 0.17400(7) 0.18624(3) 0.0143(2) Uani 1 1 d . . . Co1 Co 0.44764(4) 0.33986(8) 0.35543(4) 0.0221(3) Uani 1 1 d . . . Co4 Co 0.38847(4) -0.00565(7) 0.19668(4) 0.0159(3) Uani 1 1 d . . . Cl10 Cl 0.30064(10) 0.4967(2) 0.45728(8) 0.0630(9) Uani 1 1 d D . . O8 O 0.4021(2) 0.1741(4) 0.12318(18) 0.0193(14) Uani 1 1 d . . . O11 O 0.3676(2) 0.1660(4) 0.33788(19) 0.0216(15) Uani 1 1 d . A . O5 O 0.45091(19) 0.0422(4) 0.32552(19) 0.0195(14) Uani 1 1 d . . . O2 O 0.4180(2) 0.2985(4) 0.20148(19) 0.0201(14) Uani 1 1 d . A . O2H O 0.39517(19) 0.1151(3) 0.23372(18) 0.0164(13) Uani 1 1 d D . . O6 O 0.46335(19) 0.0359(3) 0.17453(19) 0.0181(14) Uani 1 1 d . . . O1H O 0.48612(19) 0.2208(4) 0.34813(18) 0.0178(14) Uani 1 1 d D . . O4 O 0.4195(2) -0.0839(3) 0.25175(19) 0.0196(14) Uani 1 1 d . . . O1 O 0.5029(2) 0.4200(4) 0.3268(2) 0.0252(16) Uani 1 1 d . A . O12 O 0.3838(2) 0.2838(4) 0.3861(2) 0.0308(17) Uani 1 1 d . A . O14 O 0.3873(2) -0.1227(4) 0.1507(2) 0.0255(16) Uani 1 1 d D . . O9 O 0.3564(2) 0.0488(4) 0.13324(19) 0.0217(15) Uani 1 1 d . . . C18 C 0.4926(3) -0.0004(5) 0.3275(3) 0.0168(19) Uani 1 1 d . . . O3 O 0.4219(2) 0.3032(3) 0.28284(19) 0.0200(14) Uani 1 1 d . A . O7 O 0.4057(2) 0.1680(5) -0.0416(2) 0.039(2) Uani 1 1 d . . . C36 C 0.3686(3) 0.1175(5) 0.1101(3) 0.018(2) Uani 1 1 d . . . N4 N 0.3502(2) -0.0881(5) 0.3020(2) 0.0221(18) Uani 1 1 d . . . H4 H 0.3424 -0.0874 0.3332 0.027 Uiso 1 1 calc R . . N6 N 0.2682(3) 0.1375(5) 0.3016(3) 0.028(2) Uani 1 1 d . . . H6 H 0.3020 0.1419 0.3045 0.034 Uiso 1 1 calc R . . N3 N 0.3156(2) -0.0467(4) 0.2239(2) 0.0183(17) Uani 1 1 d . . . O13 O 0.4001(3) 0.4573(4) 0.3572(2) 0.047(2) Uani 0.75 1 d P A 1 H13A H 0.3764 0.4449 0.3741 0.071 Uiso 0.75 1 d PR A 1 H13B H 0.4176 0.5003 0.3649 0.071 Uiso 0.75 1 d PR A 1 N8 N 0.4494(3) 0.1708(5) 0.0316(2) 0.0251(19) Uani 1 1 d . . . H8 H 0.4467 0.1903 0.0618 0.030 Uiso 1 1 calc R . . O1A O 0.5000 0.1674(7) 0.2500 0.035(3) Uani 1 2 d S . . O10 O 0.1973(2) 0.1027(5) 0.3448(3) 0.041(2) Uani 1 1 d . . . C11 C 0.2258(3) -0.0747(6) 0.2054(3) 0.027(2) Uani 1 1 d . . . H11 H 0.1979 -0.0742 0.1824 0.033 Uiso 1 1 calc R . . C17 C 0.4892(3) -0.1002(5) 0.3310(3) 0.022(2) Uani 1 1 d . . . H17A H 0.5092 -0.1207 0.3602 0.026 Uiso 1 1 calc R . . H17B H 0.5048 -0.1273 0.3018 0.026 Uiso 1 1 calc R . . C15 C 0.4009(3) -0.0973(5) 0.2923(3) 0.021(2) Uani 1 1 d . . . C27 C 0.3566(3) 0.2190(6) 0.3720(3) 0.025(2) Uani 1 1 d . . . N5 N 0.2846(3) 0.1727(5) 0.2224(3) 0.030(2) Uani 1 1 d . . . C6 C 0.5458(3) 0.4392(5) 0.3447(3) 0.026(2) Uani 1 1 d . . . N1 N 0.4820(3) 0.3704(5) 0.4258(3) 0.029(2) Uani 1 1 d . A . C1 C 0.4556(4) 0.3476(6) 0.4659(3) 0.035(3) Uani 1 1 d . . . H1 H 0.4215 0.3253 0.4615 0.042 Uiso 1 1 calc R A . N7 N 0.5269(3) 0.1199(5) 0.0608(2) 0.0246(19) Uani 1 1 d . . . C33 C 0.4066(3) 0.1815(6) 0.0024(3) 0.026(2) Uani 1 1 d . . . C28 C 0.5731(3) 0.0838(6) 0.0548(3) 0.030(2) Uani 1 1 d . . . H28 H 0.5944 0.0742 0.0830 0.036 Uiso 1 1 calc R . . C14 C 0.3084(3) -0.0794(5) 0.2689(3) 0.020(2) Uani 1 1 d . . . C13 C 0.2607(3) -0.1060(6) 0.2849(3) 0.028(2) Uani 1 1 d D . . H13 H 0.2565 -0.1246 0.3178 0.034 Uiso 1 1 calc R . . N2 N 0.5585(3) 0.4319(5) 0.3928(3) 0.031(2) Uani 1 1 d . A . H2 H 0.5905 0.4471 0.4004 0.037 Uiso 1 1 calc R . . C5 C 0.5292(3) 0.4042(6) 0.4325(3) 0.030(2) Uani 1 1 d . . . C31 C 0.5125(3) 0.1099(7) -0.0262(3) 0.033(3) Uani 1 1 d . . . H31 H 0.4903 0.1191 -0.0538 0.039 Uiso 1 1 calc R . . C35 C 0.3387(3) 0.1343(6) 0.0623(3) 0.021(2) Uani 1 1 d . . . H35A H 0.3025 0.1482 0.0702 0.026 Uiso 1 1 calc R . . H35B H 0.3384 0.0785 0.0430 0.026 Uiso 1 1 calc R . . C30 C 0.5608(3) 0.0731(7) -0.0314(3) 0.034(3) Uani 1 1 d . . . H30 H 0.5726 0.0572 -0.0629 0.040 Uiso 1 1 calc R . . C23 C 0.2476(4) 0.1521(6) 0.2543(3) 0.029(2) Uani 1 1 d . . . C24 C 0.2439(3) 0.1178(6) 0.3431(3) 0.029(2) Uani 1 1 d . A . C32 C 0.4972(3) 0.1331(6) 0.0205(3) 0.025(2) Uani 1 1 d . . . C16 C 0.4336(3) -0.1313(6) 0.3346(3) 0.026(2) Uani 1 1 d . . . H16A H 0.4326 -0.1974 0.3350 0.032 Uiso 1 1 calc R . . H16B H 0.4191 -0.1096 0.3657 0.032 Uiso 1 1 calc R . . C12 C 0.2193(3) -0.1053(6) 0.2527(3) 0.032(3) Uani 1 1 d . . . H12 H 0.1865 -0.1256 0.2627 0.038 Uiso 1 1 calc R . . C25 C 0.2788(3) 0.1155(7) 0.3886(3) 0.032(3) Uani 1 1 d . . . H25A H 0.3046 0.0674 0.3848 0.039 Uiso 1 1 calc R A . H25B H 0.2577 0.1004 0.4172 0.039 Uiso 1 1 calc R . . C10 C 0.2740(3) -0.0452(5) 0.1929(3) 0.022(2) Uani 1 1 d . . . H10 H 0.2784 -0.0225 0.1608 0.026 Uiso 1 1 calc R . . C34 C 0.3592(3) 0.2094(6) 0.0302(3) 0.025(2) Uani 1 1 d . . . H34A H 0.3318 0.2280 0.0066 0.030 Uiso 1 1 calc R . . H34B H 0.3680 0.2614 0.0511 0.030 Uiso 1 1 calc R . . C19 C 0.2693(4) 0.1881(7) 0.1761(3) 0.044(3) Uani 1 1 d . . . H19 H 0.2949 0.2034 0.1532 0.053 Uiso 1 1 calc R . . C21 C 0.1817(4) 0.1627(7) 0.1932(4) 0.055(3) Uani 1 1 d . . . H21 H 0.1464 0.1592 0.1831 0.066 Uiso 1 1 calc R . . C29 C 0.5921(3) 0.0593(7) 0.0098(3) 0.034(3) Uani 1 1 d . . . H29 H 0.6255 0.0338 0.0072 0.041 Uiso 1 1 calc R . . C2 C 0.4755(4) 0.3550(7) 0.5128(4) 0.045(3) Uani 1 1 d . A . H2A H 0.4557 0.3381 0.5402 0.054 Uiso 1 1 calc R . . O14A O 0.2754(3) 0.4719(9) 0.4129(3) 0.067(4) Uani 0.70 1 d PD B 1 C38 C 0.3803(4) -0.2116(6) 0.1695(4) 0.047(3) Uani 1 1 d . . . H38A H 0.4060 -0.2233 0.1955 0.071 Uiso 1 1 calc R . . H38B H 0.3845 -0.2550 0.1430 0.071 Uiso 1 1 calc R . . H38C H 0.3455 -0.2171 0.1827 0.071 Uiso 1 1 calc R . . C26 C 0.3071(3) 0.2034(7) 0.3989(3) 0.034(3) Uani 1 1 d . A . H26A H 0.2832 0.2531 0.3908 0.041 Uiso 1 1 calc R . . H26B H 0.3151 0.2066 0.4344 0.041 Uiso 1 1 calc R . . C22 C 0.1957(4) 0.1473(6) 0.2417(4) 0.041(3) Uani 1 1 d . . . H22 H 0.1706 0.1340 0.2654 0.049 Uiso 1 1 calc R . . C20 C 0.2187(4) 0.1830(7) 0.1597(4) 0.055(3) Uani 1 1 d . . . H20 H 0.2097 0.1932 0.1263 0.066 Uiso 1 1 calc R . . C3 C 0.5254(4) 0.3878(8) 0.5188(4) 0.051(3) Uani 1 1 d . . . H3 H 0.5405 0.3932 0.5507 0.061 Uiso 1 1 calc R A . O12A O 0.2932(4) 0.5890(5) 0.4673(4) 0.083(3) Uani 1 1 d D B . Cl20 Cl 0.48270(16) 0.6668(3) 0.28116(17) 0.0427(14) Uani 0.50 1 d PD . 2 O22A O 0.5000 0.5932(5) 0.2500 0.048(3) Uani 1 2 d SD . 2 O21A O 0.5000 0.7425(6) 0.2500 0.111(7) Uani 1 2 d SD . 2 O1B O 0.8216(2) 0.3792(5) 0.4012(2) 0.041(2) Uani 1 1 d . . . H1B H 0.8465 0.3657 0.4199 0.062 Uiso 1 1 calc R . . C1B C 0.7744(4) 0.3778(9) 0.4280(4) 0.060(4) Uani 1 1 d . . . H1BA H 0.7777 0.4177 0.4563 0.090 Uiso 1 1 calc R . . H1BB H 0.7677 0.3169 0.4393 0.090 Uiso 1 1 calc R . . H1BC H 0.7458 0.3977 0.4067 0.090 Uiso 1 1 calc R . . O2B O 0.6814(3) 0.8674(8) 0.4252(3) 0.098(4) Uani 1 1 d . . . H2B H 0.7099 0.8942 0.4268 0.147 Uiso 1 1 calc R . . C2B C 0.6841(5) 0.7907(11) 0.4537(4) 0.094(5) Uani 1 1 d . . . H2BA H 0.7150 0.7931 0.4750 0.141 Uiso 1 1 calc R . . H2BB H 0.6860 0.7382 0.4324 0.141 Uiso 1 1 calc R . . H2BC H 0.6533 0.7866 0.4737 0.141 Uiso 1 1 calc R . . C4 C 0.5529(4) 0.4124(7) 0.4787(3) 0.044(3) Uani 1 1 d . A . H4A H 0.5871 0.4345 0.4822 0.052 Uiso 1 1 calc R . . O13A O 0.3564(3) 0.4964(9) 0.4472(4) 0.070(4) Uani 0.70 1 d PD B 1 O11A O 0.2913(6) 0.4432(9) 0.4981(3) 0.107(6) Uani 0.70 1 d PD B 1 C9 C 0.4190(3) 0.3400(5) 0.2410(3) 0.019(2) Uani 1 1 d . . . C8 C 0.4172(3) 0.4412(5) 0.2391(3) 0.026(2) Uani 1 1 d . . . H8A H 0.3873 0.4624 0.2577 0.031 Uiso 1 1 calc R . . H8B H 0.4489 0.4654 0.2550 0.031 Uiso 1 1 calc R . . C7 C 0.5871(3) 0.4763(6) 0.3129(3) 0.029(2) Uani 1 1 d . . . H7A H 0.6214 0.4603 0.3270 0.035 Uiso 1 1 calc R . . H7B H 0.5845 0.5422 0.3124 0.035 Uiso 1 1 calc R . . O2A O 0.3503(3) 0.4832(9) 0.5820(3) 0.124(4) Uani 1 1 d G . . H2H H 0.3671 0.1426 0.2336 0.149 Uiso 1 1 d GD . . H1H H 0.4922 0.1929 0.3739 0.149 Uiso 1 1 d GD . . H2AA H 0.3310 0.4640 0.6046 0.187 Uiso 1 1 d G . . H2AB H 0.3355 0.4740 0.5544 0.187 Uiso 1 1 d G . . O15 O 0.4276(4) 0.6669(17) 0.2760(10) 0.128(9) Uani 0.50 1 d PD C 2 O16 O 0.4517(5) 0.6208(8) 0.3322(5) 0.034(4) Uani 0.50 1 d PG D 1 H14 H 0.3633 -0.1168 0.1307 0.041 Uiso 1 1 d GD . . H16 H 0.4432 0.5683 0.3211 0.051 Uiso 0.50 1 d PGD D 1 O18 O 0.5030(6) 0.6685(11) 0.3303(3) 0.064(6) Uani 0.50 1 d PD E 2 O19 O 0.4001(3) 0.4573(4) 0.3572(2) 0.047(2) Uani 0.25 1 d PD A 2 H19A H 0.381(5) 0.411(3) 0.372(9) 0.057 Uiso 0.25 1 d PD F 2 C1A C 0.4047(15) 0.5435(8) 0.3838(8) 0.054(14) Uani 0.25 1 d PD A 2 H1AA H 0.4319 0.5797 0.3692 0.080 Uiso 0.25 1 calc PR A 2 H1AB H 0.4136 0.5320 0.4183 0.080 Uiso 0.25 1 calc PR A 2 H1AC H 0.3718 0.5755 0.3815 0.080 Uiso 0.25 1 calc PR A 2 C1C C 0.4951(8) 0.6590(13) 0.3611(7) 0.036(5) Uani 0.50 1 d P D 1 H1CA H 0.5157 0.6975 0.3400 0.055 Uiso 0.50 1 calc PR D 1 H1CB H 0.5169 0.6106 0.3741 0.055 Uiso 0.50 1 calc PR D 1 H1CC H 0.4817 0.6941 0.3882 0.055 Uiso 0.50 1 calc PR D 1 O17 O 0.2527(4) 0.4609(15) 0.4786(5) 0.064(5) Uani 0.30 1 d PD B 2 O1C O 0.3347(5) 0.4380(10) 0.4843(5) 0.064(5) Uani 0.30 1 d PD B 2 O1D O 0.2972(8) 0.4597(14) 0.4085(3) 0.064(5) Uani 0.30 1 d PD 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 Co2 0.0136(5) 0.0165(5) 0.0137(4) -0.0007(4) -0.0016(4) 0.0017(4) Co3 0.0137(4) 0.0157(5) 0.0134(4) 0.0002(4) -0.0013(4) -0.0027(4) Co1 0.0163(5) 0.0255(5) 0.0243(5) -0.0108(5) -0.0044(4) 0.0059(5) Co4 0.0147(5) 0.0154(5) 0.0175(5) -0.0006(4) -0.0001(4) -0.0030(4) Cl10 0.0544(15) 0.108(2) 0.0260(12) -0.0140(14) -0.0077(11) 0.0348(16) O8 0.018(3) 0.024(3) 0.016(2) 0.000(2) -0.003(2) -0.004(2) O11 0.019(3) 0.028(3) 0.018(3) -0.001(2) 0.002(2) 0.002(3) O5 0.015(2) 0.022(3) 0.022(3) 0.003(2) 0.001(2) 0.002(2) O2 0.022(3) 0.018(3) 0.021(3) 0.002(2) -0.005(2) 0.001(2) O2H 0.016(2) 0.018(3) 0.015(2) -0.001(2) -0.001(2) -0.001(2) O6 0.016(2) 0.018(3) 0.021(3) -0.002(2) 0.001(2) -0.003(2) O1H 0.016(2) 0.022(3) 0.016(2) -0.004(2) -0.002(2) 0.005(2) O4 0.017(3) 0.017(3) 0.025(3) 0.003(2) 0.001(2) 0.000(2) O1 0.020(3) 0.020(3) 0.035(3) -0.007(3) -0.010(2) 0.003(2) O12 0.020(3) 0.047(4) 0.025(3) -0.014(3) 0.000(2) 0.004(3) O14 0.020(3) 0.027(3) 0.030(3) -0.010(3) -0.001(2) -0.004(3) O9 0.019(3) 0.026(3) 0.020(3) 0.001(2) -0.002(2) -0.006(2) C18 0.015(3) 0.021(4) 0.014(3) 0.004(3) 0.001(3) 0.000(3) O3 0.021(3) 0.017(3) 0.022(3) -0.003(2) -0.005(2) 0.004(2) O7 0.031(3) 0.070(5) 0.015(3) -0.003(3) -0.001(2) -0.003(3) C36 0.014(3) 0.024(4) 0.015(3) -0.003(3) 0.002(3) 0.000(3) N4 0.017(3) 0.028(4) 0.021(3) 0.005(3) 0.001(3) -0.002(3) N6 0.020(3) 0.032(4) 0.031(4) 0.000(3) -0.004(3) -0.001(3) N3 0.017(3) 0.016(3) 0.022(3) 0.000(3) 0.000(3) 0.000(3) O13 0.042(4) 0.051(4) 0.048(4) -0.026(3) -0.019(3) 0.030(3) N8 0.022(3) 0.037(4) 0.016(3) -0.004(3) 0.000(3) -0.003(3) O1A 0.013(4) 0.081(7) 0.012(4) 0.000 -0.001(3) 0.000 O10 0.021(3) 0.051(4) 0.050(4) -0.001(3) 0.003(3) -0.002(3) C11 0.016(4) 0.030(4) 0.035(5) 0.004(4) -0.004(4) -0.001(4) C17 0.018(4) 0.022(4) 0.026(4) 0.008(3) 0.000(3) 0.001(3) C15 0.022(4) 0.014(4) 0.026(4) 0.005(3) -0.001(3) -0.004(3) C27 0.019(4) 0.040(5) 0.016(4) -0.002(4) -0.003(3) 0.011(4) N5 0.039(4) 0.026(4) 0.024(3) -0.007(3) -0.003(3) 0.013(3) C6 0.024(4) 0.015(4) 0.038(5) -0.011(4) -0.010(4) 0.005(4) N1 0.028(4) 0.031(4) 0.028(4) -0.013(3) -0.007(3) 0.010(3) C1 0.032(5) 0.041(5) 0.031(5) -0.015(4) -0.004(4) 0.010(4) N7 0.017(3) 0.034(4) 0.022(3) -0.005(3) 0.001(3) -0.004(3) C33 0.028(4) 0.032(5) 0.018(4) 0.002(4) 0.000(3) -0.005(4) C28 0.025(4) 0.037(5) 0.028(4) -0.007(4) -0.003(4) -0.004(4) C14 0.019(4) 0.015(4) 0.026(4) 0.005(3) -0.001(3) 0.000(3) C13 0.021(4) 0.030(4) 0.034(5) 0.013(4) 0.001(4) 0.003(4) N2 0.023(4) 0.032(4) 0.037(4) -0.010(3) -0.012(3) -0.001(3) C5 0.030(4) 0.026(4) 0.035(5) -0.014(4) -0.011(4) 0.007(4) C31 0.031(5) 0.049(5) 0.018(4) -0.007(4) 0.003(4) -0.008(4) C35 0.020(4) 0.030(4) 0.014(4) -0.003(3) -0.003(3) -0.002(4) C30 0.029(4) 0.045(5) 0.027(4) -0.009(4) 0.010(4) -0.007(4) C23 0.034(4) 0.021(4) 0.033(4) -0.010(4) -0.011(4) 0.008(4) C24 0.024(4) 0.023(4) 0.040(5) -0.001(4) 0.001(4) 0.005(4) C32 0.023(4) 0.032(4) 0.022(4) -0.002(4) 0.004(3) -0.009(4) C16 0.023(4) 0.025(4) 0.032(4) 0.014(4) -0.002(4) -0.002(4) C12 0.015(4) 0.033(5) 0.047(5) 0.014(4) 0.004(4) -0.002(4) C25 0.022(4) 0.047(5) 0.028(4) 0.006(4) 0.007(4) 0.003(4) C10 0.019(4) 0.023(4) 0.023(4) -0.001(3) -0.001(3) 0.001(4) C34 0.022(4) 0.034(5) 0.018(4) 0.000(4) -0.004(3) 0.001(4) C19 0.066(6) 0.041(5) 0.024(4) -0.009(4) -0.008(4) 0.031(5) C21 0.055(6) 0.045(6) 0.063(6) -0.029(5) -0.035(5) 0.021(5) C29 0.022(4) 0.045(5) 0.036(5) -0.012(4) 0.006(4) -0.003(4) C2 0.045(6) 0.058(6) 0.030(5) -0.011(5) -0.006(4) 0.011(5) O14A 0.032(5) 0.139(11) 0.029(5) 0.006(6) -0.009(4) -0.034(6) C38 0.053(6) 0.023(5) 0.066(7) -0.009(5) -0.009(5) -0.002(5) C26 0.022(4) 0.059(6) 0.022(4) -0.006(4) 0.002(3) 0.005(5) C22 0.037(5) 0.033(5) 0.053(6) -0.016(4) -0.016(4) 0.008(4) C20 0.071(7) 0.054(6) 0.038(5) -0.020(5) -0.026(5) 0.037(5) C3 0.045(6) 0.073(7) 0.034(5) -0.017(5) -0.019(4) 0.008(6) O12A 0.063(5) 0.097(7) 0.090(7) -0.016(6) 0.016(5) 0.016(5) Cl20 0.035(2) 0.027(2) 0.066(3) -0.018(2) -0.005(2) 0.006(2) O22A 0.048(5) 0.019(4) 0.080(7) 0.000 0.029(5) 0.000 O21A 0.217(18) 0.019(6) 0.096(10) 0.000 -0.040(11) 0.000 O1B 0.026(3) 0.073(5) 0.025(3) 0.013(3) 0.003(3) 0.003(3) C1B 0.043(6) 0.087(9) 0.049(6) 0.013(6) 0.011(5) 0.007(6) O2B 0.045(4) 0.184(9) 0.064(5) 0.076(5) -0.018(4) -0.021(6) C2B 0.079(7) 0.160(11) 0.044(6) 0.040(7) 0.022(6) 0.084(7) C4 0.041(5) 0.053(6) 0.037(5) -0.017(5) -0.016(4) 0.006(5) O13A 0.032(5) 0.106(9) 0.072(7) -0.048(6) -0.009(5) 0.013(6) O11A 0.150(13) 0.139(13) 0.032(6) 0.019(8) -0.018(7) -0.057(11) C9 0.013(3) 0.018(4) 0.026(4) -0.001(3) -0.005(3) 0.000(3) C8 0.025(4) 0.016(4) 0.036(4) -0.001(4) -0.012(4) 0.001(4) C7 0.021(4) 0.018(4) 0.047(5) -0.007(4) -0.011(4) -0.001(4) O2A 0.076(5) 0.261(11) 0.036(4) 0.013(6) -0.020(4) -0.108(6) O15 0.039(10) 0.157(19) 0.19(2) -0.093(15) 0.008(12) 0.013(12) O16 0.033(6) 0.017(6) 0.053(8) 0.000(6) 0.015(6) -0.004(5) O18 0.096(12) 0.054(9) 0.044(8) 0.009(8) 0.011(9) 0.011(10) O19 0.042(4) 0.051(4) 0.048(4) -0.026(3) -0.019(3) 0.030(3) C1A 0.028(19) 0.08(3) 0.05(2) 0.00(2) -0.008(18) 0.02(2) C1C 0.045(11) 0.025(9) 0.039(10) 0.002(8) -0.001(9) 0.005(9) O17 0.055(8) 0.120(13) 0.018(6) -0.006(8) -0.004(6) 0.037(9) O1C 0.055(8) 0.120(13) 0.018(6) -0.006(8) -0.004(6) 0.037(9) O1D 0.055(8) 0.120(13) 0.018(6) -0.006(8) -0.004(6) 0.037(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 Co2 O11 2.081(5) . ? Co2 O5 2.056(5) . ? Co2 O2H 2.094(5) . ? Co2 O1H 2.118(5) . ? Co2 O3 2.122(5) . ? Co2 O1A 2.1507(10) . ? Co3 O8 2.076(5) . ? Co3 O2 2.070(5) . ? Co3 O2H 2.105(5) . ? Co3 O6 2.132(5) . ? Co3 O1H 2.083(5) 2_655 ? Co3 O1A 2.1788(11) . ? Co1 O1H 2.055(5) . ? Co1 O1 2.038(6) . ? Co1 O12 2.051(6) . ? Co1 O3 2.151(5) . ? Co1 O13 2.149(6) . ? Co1 N1 2.150(7) . ? Co4 O2H 2.079(5) . ? Co4 O6 2.138(5) . ? Co4 O4 2.059(5) . ? Co4 O14 2.157(6) . ? Co4 O9 2.074(5) . ? Co4 N3 2.134(6) . ? Cl10 O14A 1.415(8) . ? Cl10 O12A 1.424(8) . ? Cl10 O13A 1.476(8) . ? Cl10 O11A 1.400(10) . ? Cl10 O17 1.482(13) . ? Cl10 O1C 1.438(13) . ? Cl10 O1D 1.445(11) . ? O8 C36 1.259(9) . ? O11 C27 1.263(10) . ? O5 C18 1.255(9) . ? O2 C9 1.246(9) . ? O2H H2H 0.8349 . ? O6 C18 1.266(9) 2_655 ? O1H Co3 2.083(5) 2_655 ? O1H H1H 0.8316 . ? O4 C15 1.235(10) . ? O1 C6 1.237(10) . ? O12 C27 1.256(11) . ? O14 C38 1.441(11) . ? O14 H14 0.8236 . ? O9 C36 1.253(10) . ? C18 O6 1.266(9) 2_655 ? C18 C17 1.503(11) . ? O3 C9 1.272(9) . ? O7 C33 1.222(10) . ? C36 C35 1.525(10) . ? N4 H4 0.8800 . ? N4 C15 1.354(10) . ? N4 C14 1.403(10) . ? N6 H6 0.8800 . ? N6 C23 1.406(11) . ? N6 C24 1.342(11) . ? N3 C14 1.340(10) . ? N3 C10 1.358(10) . ? O13 H13A 0.8006 . ? O13 H13B 0.8136 . ? O13 H19A 0.93(15) . ? N8 H8 0.8800 . ? N8 C33 1.362(10) . ? N8 C32 1.400(11) . ? O1A Co2 2.1507(10) 2_655 ? O1A Co3 2.1788(11) 2_655 ? O10 C24 1.232(11) . ? C11 H11 0.9500 . ? C11 C12 1.384(13) . ? C11 C10 1.374(11) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C17 C16 1.521(11) . ? C15 C16 1.508(11) . ? C27 C26 1.508(12) . ? N5 C23 1.346(12) . ? N5 C19 1.338(11) . ? C6 N2 1.354(11) . ? C6 C7 1.500(12) . ? N1 C1 1.348(12) . ? N1 C5 1.332(11) . ? C1 H1 0.9500 . ? C1 C2 1.377(13) . ? N7 C28 1.326(11) . ? N7 C32 1.345(10) . ? C33 C34 1.515(12) . ? C28 H28 0.9500 . ? C28 C29 1.385(13) . ? C14 C13 1.378(11) . ? C13 H13 0.9500 . ? C13 C12 1.373(12) . ? N2 H2 0.8800 . ? N2 C5 1.404(12) . ? C5 C4 1.398(13) . ? C31 H31 0.9500 . ? C31 C30 1.377(13) . ? C31 C32 1.389(12) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C35 C34 1.529(12) . ? C30 H30 0.9500 . ? C30 C29 1.388(13) . ? C23 C22 1.383(13) . ? C24 C25 1.521(12) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C12 H12 0.9500 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C25 C26 1.532(14) . ? C10 H10 0.9500 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C19 H19 0.9500 . ? C19 C20 1.379(15) . ? C21 H21 0.9500 . ? C21 C22 1.386(15) . ? C21 C20 1.376(16) . ? C29 H29 0.9500 . ? C2 H2A 0.9500 . ? C2 C3 1.391(15) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C22 H22 0.9500 . ? C20 H20 0.9500 . ? C3 H3 0.9500 . ? C3 C4 1.369(15) . ? Cl20 Cl20 1.943(9) 2_655 ? Cl20 O22A 1.469(7) . ? Cl20 O21A 1.494(8) . ? Cl20 O15 1.432(10) . ? Cl20 O18 1.432(11) . ? O22A Cl20 1.469(7) 2_655 ? O21A Cl20 1.494(8) 2_655 ? O1B H1B 0.8400 . ? O1B C1B 1.441(13) . ? C1B H1BA 0.9800 . ? C1B H1BB 0.9800 . ? C1B H1BC 0.9800 . ? O2B H2B 0.8400 . ? O2B C2B 1.390(18) . ? C2B H2BA 0.9800 . ? C2B H2BB 0.9800 . ? C2B H2BC 0.9800 . ? C4 H4A 0.9500 . ? C9 C8 1.517(11) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 C7 1.517(12) 2_655 ? C7 C8 1.517(12) 2_655 ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? O2A H2AA 0.8538 . ? O2A H2AB 0.8507 . ? O16 H16 0.8699 . ? O16 C1C 1.48(2) . ? C1A H13B 0.8960 . ? C1A H1AA 0.9800 . ? C1A H1AB 0.9800 . ? C1A H1AC 0.9800 . ? C1C H1CA 0.9800 . ? C1C H1CB 0.9800 . ? C1C H1CC 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 O11 Co2 O2H 93.8(2) . . ? O11 Co2 O1H 98.6(2) . . ? O11 Co2 O3 88.3(2) . . ? O11 Co2 O1A 177.2(2) . . ? O5 Co2 O11 87.9(2) . . ? O5 Co2 O2H 95.4(2) . . ? O5 Co2 O1H 87.7(2) . . ? O5 Co2 O3 165.9(2) . . ? O5 Co2 O1A 94.3(3) . . ? O2H Co2 O1H 167.3(2) . . ? O2H Co2 O3 98.4(2) . . ? O2H Co2 O1A 84.43(17) . . ? O1H Co2 O3 79.5(2) . . ? O1H Co2 O1A 83.06(18) . . ? O3 Co2 O1A 89.9(3) . . ? O8 Co3 O2H 98.1(2) . . ? O8 Co3 O6 88.9(2) . . ? O8 Co3 O1H 94.9(2) . 2_655 ? O8 Co3 O1A 176.1(2) . . ? O2 Co3 O8 87.3(2) . . ? O2 Co3 O2H 89.9(2) . . ? O2 Co3 O6 167.7(2) . . ? O2 Co3 O1H 95.9(2) . 2_655 ? O2 Co3 O1A 96.2(3) . . ? O2H Co3 O6 79.1(2) . . ? O2H Co3 O1A 83.48(18) . . ? O6 Co3 O1A 88.0(3) . . ? O1H Co3 O2H 165.9(2) 2_655 . ? O1H Co3 O6 96.0(2) 2_655 . ? O1H Co3 O1A 83.19(17) 2_655 . ? O1H Co1 O3 80.2(2) . . ? O1H Co1 O13 172.9(2) . . ? O1H Co1 N1 94.6(2) . . ? O1 Co1 O1H 97.4(2) . . ? O1 Co1 O12 168.0(2) . . ? O1 Co1 O3 90.1(2) . . ? O1 Co1 O13 86.2(2) . . ? O1 Co1 N1 86.4(3) . . ? O12 Co1 O1H 94.7(2) . . ? O12 Co1 O3 92.1(2) . . ? O12 Co1 O13 81.9(3) . . ? O12 Co1 N1 92.5(3) . . ? O13 Co1 O3 93.6(2) . . ? O13 Co1 N1 91.8(3) . . ? N1 Co1 O3 173.3(2) . . ? O2H Co4 O6 79.5(2) . . ? O2H Co4 O14 172.4(2) . . ? O2H Co4 N3 98.4(2) . . ? O6 Co4 O14 94.2(2) . . ? O4 Co4 O2H 96.5(2) . . ? O4 Co4 O6 91.7(2) . . ? O4 Co4 O14 87.9(2) . . ? O4 Co4 O9 168.2(2) . . ? O4 Co4 N3 85.1(2) . . ? O9 Co4 O2H 95.3(2) . . ? O9 Co4 O6 89.8(2) . . ? O9 Co4 O14 80.4(2) . . ? O9 Co4 N3 93.7(2) . . ? N3 Co4 O6 176.0(2) . . ? N3 Co4 O14 88.2(2) . . ? O14A Cl10 O12A 111.0(7) . . ? O14A Cl10 O13A 105.9(6) . . ? O14A Cl10 O17 82.4(7) . . ? O14A Cl10 O1C 123.1(8) . . ? O14A Cl10 O1D 24.5(9) . . ? O12A Cl10 O13A 100.1(7) . . ? O12A Cl10 O17 99.1(9) . . ? O12A Cl10 O1C 125.4(8) . . ? O12A Cl10 O1D 123.0(9) . . ? O11A Cl10 O14A 116.7(8) . . ? O11A Cl10 O12A 112.2(7) . . ? O11A Cl10 O13A 109.6(9) . . ? O11A Cl10 O17 47.0(9) . . ? O11A Cl10 O1C 49.8(9) . . ? O11A Cl10 O1D 120.5(10) . . ? O17 Cl10 O13A 154.6(9) . . ? O1C Cl10 O13A 60.2(8) . . ? O1C Cl10 O17 94.9(9) . . ? O1C Cl10 O1D 105.3(10) . . ? O1D Cl10 O13A 82.3(9) . . ? O1D Cl10 O17 100.8(10) . . ? C36 O8 Co3 128.0(5) . . ? C27 O11 Co2 127.8(5) . . ? C18 O5 Co2 130.6(5) . . ? C9 O2 Co3 128.6(5) . . ? Co2 O2H Co3 92.6(2) . . ? Co2 O2H H2H 103.0 . . ? Co3 O2H H2H 111.8 . . ? Co4 O2H Co2 137.8(3) . . ? Co4 O2H Co3 96.5(2) . . ? Co4 O2H H2H 111.4 . . ? Co3 O6 Co4 94.0(2) . . ? C18 O6 Co3 126.3(5) 2_655 . ? C18 O6 Co4 135.3(5) 2_655 . ? Co2 O1H H1H 118.5 . . ? Co3 O1H Co2 94.7(2) 2_655 . ? Co3 O1H H1H 94.1 2_655 . ? Co1 O1H Co2 95.9(2) . . ? Co1 O1H Co3 137.6(3) . 2_655 ? Co1 O1H H1H 116.0 . . ? C15 O4 Co4 126.5(5) . . ? C6 O1 Co1 128.2(6) . . ? C27 O12 Co1 130.1(5) . . ? Co4 O14 H14 107.5 . . ? C38 O14 Co4 123.0(6) . . ? C38 O14 H14 103.6 . . ? C36 O9 Co4 130.2(5) . . ? O5 C18 O6 123.8(7) . 2_655 ? O5 C18 C17 117.2(7) . . ? O6 C18 C17 119.0(7) 2_655 . ? Co2 O3 Co1 93.0(2) . . ? C9 O3 Co2 125.6(5) . . ? C9 O3 Co1 136.9(5) . . ? O8 C36 C35 117.8(7) . . ? O9 C36 O8 126.1(7) . . ? O9 C36 C35 116.1(7) . . ? C15 N4 H4 115.8 . . ? C15 N4 C14 128.3(7) . . ? C14 N4 H4 115.8 . . ? C23 N6 H6 115.3 . . ? C24 N6 H6 115.3 . . ? C24 N6 C23 129.5(7) . . ? C14 N3 Co4 124.6(5) . . ? C14 N3 C10 117.0(7) . . ? C10 N3 Co4 118.3(5) . . ? Co1 O13 H13A 105.7 . . ? Co1 O13 H13B 109.9 . . ? Co1 O13 H19A 73(8) . . ? H13A O13 H19A 34.1 . . ? H13B O13 H19A 139.9 . . ? C33 N8 H8 115.3 . . ? C33 N8 C32 129.4(7) . . ? C32 N8 H8 115.3 . . ? Co2 O1A Co2 178.1(6) . 2_655 ? Co2 O1A Co3 89.04(4) . . ? Co2 O1A Co3 91.04(4) 2_655 . ? Co2 O1A Co3 89.04(4) 2_655 2_655 ? Co2 O1A Co3 91.04(4) . 2_655 ? Co3 O1A Co3 174.8(6) . 2_655 ? C12 C11 H11 121.0 . . ? C10 C11 H11 121.0 . . ? C10 C11 C12 118.0(8) . . ? C18 C17 H17A 109.3 . . ? C18 C17 H17B 109.3 . . ? C18 C17 C16 111.5(7) . . ? H17A C17 H17B 108.0 . . ? C16 C17 H17A 109.3 . . ? C16 C17 H17B 109.3 . . ? O4 C15 N4 124.1(7) . . ? O4 C15 C16 121.3(7) . . ? N4 C15 C16 114.4(7) . . ? O11 C27 C26 118.1(8) . . ? O12 C27 O11 125.4(7) . . ? O12 C27 C26 116.5(7) . . ? C19 N5 C23 116.8(8) . . ? O1 C6 N2 124.2(8) . . ? O1 C6 C7 120.2(8) . . ? N2 C6 C7 115.5(7) . . ? C1 N1 Co1 117.8(6) . . ? C5 N1 Co1 124.4(6) . . ? C5 N1 C1 117.6(7) . . ? N1 C1 H1 118.2 . . ? N1 C1 C2 123.5(9) . . ? C2 C1 H1 118.2 . . ? C28 N7 C32 117.3(7) . . ? O7 C33 N8 123.6(8) . . ? O7 C33 C34 122.9(8) . . ? N8 C33 C34 113.4(7) . . ? N7 C28 H28 118.0 . . ? N7 C28 C29 124.0(8) . . ? C29 C28 H28 118.0 . . ? N3 C14 N4 120.3(7) . . ? N3 C14 C13 122.8(7) . . ? C13 C14 N4 116.9(7) . . ? C14 C13 H13 120.4 . . ? C12 C13 C14 119.1(8) . . ? C12 C13 H13 120.4 . . ? C6 N2 H2 114.7 . . ? C6 N2 C5 130.6(7) . . ? C5 N2 H2 114.7 . . ? N1 C5 N2 121.1(8) . . ? N1 C5 C4 122.8(9) . . ? C4 C5 N2 116.0(8) . . ? C30 C31 H31 120.9 . . ? C30 C31 C32 118.2(8) . . ? C32 C31 H31 120.9 . . ? C36 C35 H35A 108.3 . . ? C36 C35 H35B 108.3 . . ? C36 C35 C34 115.9(7) . . ? H35A C35 H35B 107.4 . . ? C34 C35 H35A 108.3 . . ? C34 C35 H35B 108.3 . . ? C31 C30 H30 120.3 . . ? C31 C30 C29 119.5(8) . . ? C29 C30 H30 120.3 . . ? N5 C23 N6 111.7(8) . . ? N5 C23 C22 123.6(8) . . ? C22 C23 N6 124.7(8) . . ? N6 C24 C25 114.5(7) . . ? O10 C24 N6 123.5(8) . . ? O10 C24 C25 122.0(8) . . ? N7 C32 N8 111.9(7) . . ? N7 C32 C31 123.1(8) . . ? C31 C32 N8 124.9(7) . . ? C17 C16 H16A 109.4 . . ? C17 C16 H16B 109.4 . . ? C15 C16 C17 111.3(7) . . ? C15 C16 H16A 109.4 . . ? C15 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? C11 C12 H12 120.3 . . ? C13 C12 C11 119.4(8) . . ? C13 C12 H12 120.3 . . ? C24 C25 H25A 108.8 . . ? C24 C25 H25B 108.8 . . ? C24 C25 C26 113.8(8) . . ? H25A C25 H25B 107.7 . . ? C26 C25 H25A 108.8 . . ? C26 C25 H25B 108.8 . . ? N3 C10 C11 123.5(8) . . ? N3 C10 H10 118.2 . . ? C11 C10 H10 118.2 . . ? C33 C34 C35 112.3(7) . . ? C33 C34 H34A 109.1 . . ? C33 C34 H34B 109.1 . . ? C35 C34 H34A 109.1 . . ? C35 C34 H34B 109.1 . . ? H34A C34 H34B 107.9 . . ? N5 C19 H19 118.0 . . ? N5 C19 C20 124.1(10) . . ? C20 C19 H19 118.0 . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C20 C21 C22 120.2(10) . . ? C28 C29 C30 117.8(8) . . ? C28 C29 H29 121.1 . . ? C30 C29 H29 121.1 . . ? C1 C2 H2A 121.1 . . ? C1 C2 C3 117.8(9) . . ? C3 C2 H2A 121.1 . . ? O14 C38 H38A 109.5 . . ? O14 C38 H38B 109.5 . . ? O14 C38 H38C 109.5 . . ? H38A C38 H38B 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C27 C26 C25 116.9(8) . . ? C27 C26 H26A 108.1 . . ? C27 C26 H26B 108.1 . . ? C25 C26 H26A 108.1 . . ? C25 C26 H26B 108.1 . . ? H26A C26 H26B 107.3 . . ? C23 C22 C21 117.5(10) . . ? C23 C22 H22 121.2 . . ? C21 C22 H22 121.2 . . ? C19 C20 H20 121.1 . . ? C21 C20 C19 117.8(10) . . ? C21 C20 H20 121.1 . . ? C2 C3 H3 120.0 . . ? C4 C3 C2 119.9(9) . . ? C4 C3 H3 120.0 . . ? O22A Cl20 Cl20 48.6(3) . 2_655 ? O22A Cl20 O21A 98.1(4) . . ? O21A Cl20 Cl20 49.4(3) . 2_655 ? O15 Cl20 Cl20 113.1(11) . 2_655 ? O15 Cl20 O22A 105.1(10) . . ? O15 Cl20 O21A 104.7(11) . . ? O18 Cl20 Cl20 131.0(7) . 2_655 ? O18 Cl20 O22A 116.6(7) . . ? O18 Cl20 O21A 114.4(7) . . ? O18 Cl20 O15 115.9(13) . . ? Cl20 O22A Cl20 82.8(5) 2_655 . ? Cl20 O21A Cl20 81.1(6) 2_655 . ? C1B O1B H1B 109.5 . . ? O1B C1B H1BA 109.5 . . ? O1B C1B H1BB 109.5 . . ? O1B C1B H1BC 109.5 . . ? H1BA C1B H1BB 109.5 . . ? H1BA C1B H1BC 109.5 . . ? H1BB C1B H1BC 109.5 . . ? C2B O2B H2B 109.5 . . ? O2B C2B H2BA 109.5 . . ? O2B C2B H2BB 109.5 . . ? O2B C2B H2BC 109.5 . . ? H2BA C2B H2BB 109.5 . . ? H2BA C2B H2BC 109.5 . . ? H2BB C2B H2BC 109.5 . . ? C5 C4 H4A 120.9 . . ? C3 C4 C5 118.3(9) . . ? C3 C4 H4A 120.9 . . ? O2 C9 O3 124.3(7) . . ? O2 C9 C8 118.0(7) . . ? O3 C9 C8 117.7(7) . . ? C9 C8 H8A 109.1 . . ? C9 C8 H8B 109.1 . . ? H8A C8 H8B 107.9 . . ? C7 C8 C9 112.3(7) 2_655 . ? C7 C8 H8A 109.1 2_655 . ? C7 C8 H8B 109.1 2_655 . ? C6 C7 C8 112.0(7) . 2_655 ? C6 C7 H7A 109.2 . . ? C6 C7 H7B 109.2 . . ? C8 C7 H7A 109.2 2_655 . ? C8 C7 H7B 109.2 2_655 . ? H7A C7 H7B 107.9 . . ? H2AA O2A H2AB 109.2 . . ? H1AA C1A H1AB 109.5 . . ? H1AA C1A H1AC 109.5 . . ? H1AB C1A H1AC 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4 O1B 0.88 2.01 2.867(9) 164.6 3_445 N6 H6 O11 0.88 1.95 2.772(9) 155.9 . O13 H13A O13A 0.80 2.21 2.794(13) 129.7 . O13 H13B O16 0.81 2.21 2.879(13) 140.1 . N8 H8 O8 0.88 2.07 2.813(8) 141.1 . N2 H2 O2A 0.88 1.91 2.756(12) 161.5 5_666 O1B H1B O7 0.84 1.91 2.747(9) 175.7 8_556 O2A H2AA O10 0.85 1.87 2.699(12) 164.0 7_556 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Co2 O11 C27 O12 2.1(12) . . . . ? Co2 O11 C27 C26 -177.0(5) . . . . ? Co2 O5 C18 O6 24.2(11) . . . 2_655 ? Co2 O5 C18 C17 -154.2(5) . . . . ? Co2 O3 C9 O2 7.0(10) . . . . ? Co2 O3 C9 C8 -172.4(5) . . . . ? Co3 O8 C36 O9 0.3(11) . . . . ? Co3 O8 C36 C35 178.4(5) . . . . ? Co3 O2 C9 O3 -26.9(11) . . . . ? Co3 O2 C9 C8 152.5(5) . . . . ? Co1 O1 C6 N2 -20.5(12) . . . . ? Co1 O1 C6 C7 161.9(6) . . . . ? Co1 O12 C27 O11 10.1(13) . . . . ? Co1 O12 C27 C26 -170.8(6) . . . . ? Co1 O3 C9 O2 156.2(6) . . . . ? Co1 O3 C9 C8 -23.2(11) . . . . ? Co1 N1 C1 C2 173.0(8) . . . . ? Co1 N1 C5 N2 7.1(12) . . . . ? Co1 N1 C5 C4 -171.4(7) . . . . ? Co4 O4 C15 N4 22.9(11) . . . . ? Co4 O4 C15 C16 -160.9(6) . . . . ? Co4 O9 C36 O8 -6.0(12) . . . . ? Co4 O9 C36 C35 175.8(5) . . . . ? Co4 N3 C14 N4 0.6(10) . . . . ? Co4 N3 C14 C13 -179.4(6) . . . . ? Co4 N3 C10 C11 176.2(7) . . . . ? O8 Co3 O2 C9 163.8(6) . . . . ? O8 Co3 O2H Co2 -159.2(2) . . . . ? O8 Co3 O2H Co4 62.1(2) . . . . ? O8 Co3 O6 Co4 -74.2(2) . . . . ? O8 Co3 O6 C18 126.5(6) . . . 2_655 ? O8 Co3 O1A Co2 -138(4) . . . . ? O8 Co3 O1A Co2 40(4) . . . 2_655 ? O8 Co3 O1A Co3 131(4) . . . 2_655 ? O8 C36 C35 C34 11.0(10) . . . . ? O11 Co2 O5 C18 -162.1(6) . . . . ? O11 Co2 O2H Co3 153.2(2) . . . . ? O11 Co2 O2H Co4 -104.1(4) . . . . ? O11 Co2 O1H Co3 160.4(2) . . . 2_655 ? O11 Co2 O1H Co1 -60.7(2) . . . . ? O11 Co2 O3 Co1 74.6(2) . . . . ? O11 Co2 O3 C9 -125.9(6) . . . . ? O11 Co2 O1A Co2 -118(6) . . . 2_655 ? O11 Co2 O1A Co3 149(6) . . . 2_655 ? O11 Co2 O1A Co3 -26(7) . . . . ? O11 C27 C26 C25 10.1(11) . . . . ? O5 Co2 O11 C27 116.1(7) . . . . ? O5 Co2 O2H Co3 -118.5(2) . . . . ? O5 Co2 O2H Co4 -15.9(4) . . . . ? O5 Co2 O1H Co3 72.9(2) . . . 2_655 ? O5 Co2 O1H Co1 -148.2(2) . . . . ? O5 Co2 O3 Co1 0.3(10) . . . . ? O5 Co2 O3 C9 159.8(8) . . . . ? O5 Co2 O1A Co2 26.23(15) . . . 2_655 ? O5 Co2 O1A Co3 118.8(3) . . . . ? O5 Co2 O1A Co3 -66.4(3) . . . 2_655 ? O5 C18 C17 C16 -3.4(10) . . . . ? O2 Co3 O8 C36 -123.4(6) . . . . ? O2 Co3 O2H Co2 -71.9(2) . . . . ? O2 Co3 O2H Co4 149.4(2) . . . . ? O2 Co3 O6 Co4 -2.3(11) . . . . ? O2 Co3 O6 C18 -161.6(9) . . . 2_655 ? O2 Co3 O1A Co2 -116.3(3) . . . 2_655 ? O2 Co3 O1A Co2 65.5(3) . . . . ? O2 Co3 O1A Co3 -25.47(15) . . . 2_655 ? O2 C9 C8 C7 1.5(10) . . . 2_655 ? O2H Co2 O11 C27 -148.7(6) . . . . ? O2H Co2 O5 C18 104.3(6) . . . . ? O2H Co2 O1H Co3 -31.5(10) . . . 2_655 ? O2H Co2 O1H Co1 107.4(9) . . . . ? O2H Co2 O3 Co1 168.14(19) . . . . ? O2H Co2 O3 C9 -32.4(6) . . . . ? O2H Co2 O1A Co2 -68.77(15) . . . 2_655 ? O2H Co2 O1A Co3 -161.4(3) . . . 2_655 ? O2H Co2 O1A Co3 23.8(3) . . . . ? O2H Co3 O8 C36 -33.8(6) . . . . ? O2H Co3 O2 C9 65.7(6) . . . . ? O2H Co3 O6 Co4 24.33(19) . . . . ? O2H Co3 O6 C18 -135.0(6) . . . 2_655 ? O2H Co3 O1A Co2 -23.7(3) . . . . ? O2H Co3 O1A Co2 154.4(4) . . . 2_655 ? O2H Co3 O1A Co3 -114.70(15) . . . 2_655 ? O2H Co4 O6 Co3 -24.61(19) . . . . ? O2H Co4 O6 C18 131.6(7) . . . 2_655 ? O2H Co4 O4 C15 65.4(6) . . . . ? O2H Co4 O14 C38 156.2(15) . . . . ? O2H Co4 O9 C36 43.9(7) . . . . ? O2H Co4 N3 C14 -75.8(6) . . . . ? O2H Co4 N3 C10 108.5(6) . . . . ? O6 Co3 O8 C36 45.0(6) . . . . ? O6 Co3 O2 C9 91.7(11) . . . . ? O6 Co3 O2H Co2 113.5(2) . . . . ? O6 Co3 O2H Co4 -25.17(19) . . . . ? O6 Co3 O1A Co2 75.2(3) . . . 2_655 ? O6 Co3 O1A Co2 -102.9(3) . . . . ? O6 Co3 O1A Co3 166.08(14) . . . 2_655 ? O6 Co4 O2H Co2 -76.1(4) . . . . ? O6 Co4 O2H Co3 25.06(19) . . . . ? O6 Co4 O4 C15 145.1(6) . . . . ? O6 Co4 O14 C38 122.9(7) . . . . ? O6 Co4 O9 C36 -35.5(7) . . . . ? O6 Co4 N3 C14 -18(4) . . . . ? O6 Co4 N3 C10 166(3) . . . . ? O6 C18 C17 C16 178.2(7) 2_655 . . . ? O1H Co2 O11 C27 28.7(7) . . . . ? O1H Co2 O5 C18 -63.4(6) . . . . ? O1H Co2 O2H Co3 -15.0(10) . . . . ? O1H Co2 O2H Co4 87.6(10) . . . . ? O1H Co2 O3 Co1 -24.55(19) . . . . ? O1H Co2 O3 C9 134.9(6) . . . . ? O1H Co2 O1A Co2 113.36(16) . . . 2_655 ? O1H Co2 O1A Co3 -154.1(3) . . . . ? O1H Co2 O1A Co3 20.7(3) . . . 2_655 ? O1H Co3 O8 C36 140.9(6) 2_655 . . . ? O1H Co3 O2 C9 -101.5(6) 2_655 . . . ? O1H Co3 O2H Co2 43.0(9) 2_655 . . . ? O1H Co3 O2H Co4 -95.7(8) 2_655 . . . ? O1H Co3 O6 Co4 -168.99(19) 2_655 . . . ? O1H Co3 O6 C18 31.7(6) 2_655 . . 2_655 ? O1H Co3 O1A Co2 -21.1(3) 2_655 . . 2_655 ? O1H Co3 O1A Co2 160.8(3) 2_655 . . . ? O1H Co3 O1A Co3 69.79(15) 2_655 . . 2_655 ? O1H Co1 O1 C6 -69.5(7) . . . . ? O1H Co1 O12 C27 -50.7(7) . . . . ? O1H Co1 O3 Co2 25.3(2) . . . . ? O1H Co1 O3 C9 -130.0(7) . . . . ? O1H Co1 N1 C1 -95.0(7) . . . . ? O1H Co1 N1 C5 79.7(7) . . . . ? O4 Co4 O2H Co2 14.5(4) . . . . ? O4 Co4 O2H Co3 115.6(2) . . . . ? O4 Co4 O6 Co3 -120.9(2) . . . . ? O4 Co4 O6 C18 35.3(7) . . . 2_655 ? O4 Co4 O14 C38 31.3(7) . . . . ? O4 Co4 O9 C36 -133.3(10) . . . . ? O4 Co4 N3 C14 20.0(6) . . . . ? O4 Co4 N3 C10 -155.6(6) . . . . ? O4 C15 C16 C17 30.2(11) . . . . ? O1 Co1 O1H Co2 -114.3(2) . . . . ? O1 Co1 O1H Co3 -10.8(4) . . . 2_655 ? O1 Co1 O12 C27 130.1(11) . . . . ? O1 Co1 O3 Co2 122.7(2) . . . . ? O1 Co1 O3 C9 -32.6(7) . . . . ? O1 Co1 N1 C1 167.9(7) . . . . ? O1 Co1 N1 C5 -17.4(7) . . . . ? O1 C6 N2 C5 -0.9(14) . . . . ? O1 C6 C7 C8 -31.1(11) . . . 2_655 ? O12 Co1 O1H Co2 65.8(2) . . . . ? O12 Co1 O1H Co3 169.4(4) . . . 2_655 ? O12 Co1 O1 C6 109.7(12) . . . . ? O12 Co1 O3 Co2 -69.1(2) . . . . ? O12 Co1 O3 C9 135.6(7) . . . . ? O12 Co1 N1 C1 -0.1(7) . . . . ? O12 Co1 N1 C5 174.6(7) . . . . ? O12 C27 C26 C25 -169.1(7) . . . . ? O14 Co4 O2H Co2 -110.0(15) . . . . ? O14 Co4 O2H Co3 -8.8(17) . . . . ? O14 Co4 O6 Co3 151.1(2) . . . . ? O14 Co4 O6 C18 -52.7(7) . . . 2_655 ? O14 Co4 O4 C15 -120.8(6) . . . . ? O14 Co4 O9 C36 -129.8(7) . . . . ? O14 Co4 N3 C14 108.0(6) . . . . ? O14 Co4 N3 C10 -67.6(6) . . . . ? O9 Co4 O2H Co2 -165.0(4) . . . . ? O9 Co4 O2H Co3 -63.8(2) . . . . ? O9 Co4 O6 Co3 70.8(2) . . . . ? O9 Co4 O6 C18 -133.0(7) . . . 2_655 ? O9 Co4 O4 C15 -117.3(11) . . . . ? O9 Co4 O14 C38 -148.0(7) . . . . ? O9 Co4 N3 C14 -171.7(6) . . . . ? O9 Co4 N3 C10 12.6(6) . . . . ? O9 C36 C35 C34 -170.7(7) . . . . ? C18 C17 C16 C15 55.8(9) . . . . ? O3 Co2 O11 C27 -50.3(6) . . . . ? O3 Co2 O5 C18 -87.8(11) . . . . ? O3 Co2 O2H Co3 64.4(2) . . . . ? O3 Co2 O2H Co4 167.1(4) . . . . ? O3 Co2 O1H Co3 -113.0(2) . . . 2_655 ? O3 Co2 O1H Co1 25.9(2) . . . . ? O3 Co2 O1A Co2 -167.24(15) . . . 2_655 ? O3 Co2 O1A Co3 100.1(3) . . . 2_655 ? O3 Co2 O1A Co3 -74.7(3) . . . . ? O3 Co1 O1H Co2 -25.4(2) . . . . ? O3 Co1 O1H Co3 78.1(4) . . . 2_655 ? O3 Co1 O1 C6 -149.7(7) . . . . ? O3 Co1 O12 C27 29.7(7) . . . . ? O3 Co1 N1 C1 -133(2) . . . . ? O3 Co1 N1 C5 42(3) . . . . ? O3 C9 C8 C7 -179.0(7) . . . 2_655 ? O7 C33 C34 C35 108.0(10) . . . . ? C36 C35 C34 C33 77.2(9) . . . . ? N4 C15 C16 C17 -153.2(7) . . . . ? N4 C14 C13 C12 -175.1(8) . . . . ? N6 C23 C22 C21 -179.3(9) . . . . ? N6 C24 C25 C26 58.6(10) . . . . ? N3 Co4 O2H Co2 100.5(4) . . . . ? N3 Co4 O2H Co3 -158.3(2) . . . . ? N3 Co4 O6 Co3 -83(3) . . . . ? N3 Co4 O6 C18 73(3) . . . 2_655 ? N3 Co4 O4 C15 -32.5(6) . . . . ? N3 Co4 O14 C38 -53.9(7) . . . . ? N3 Co4 O9 C36 142.7(7) . . . . ? N3 C14 C13 C12 4.8(13) . . . . ? O13 Co1 O1H Co2 5(2) . . . . ? O13 Co1 O1H Co3 108.6(19) . . . 2_655 ? O13 Co1 O1 C6 116.7(7) . . . . ? O13 Co1 O12 C27 123.0(7) . . . . ? O13 Co1 O3 Co2 -151.1(2) . . . . ? O13 Co1 O3 C9 53.6(7) . . . . ? O13 Co1 N1 C1 81.8(7) . . . . ? O13 Co1 N1 C5 -103.5(7) . . . . ? N8 C33 C34 C35 -70.5(9) . . . . ? O1A Co2 O11 C27 -99(6) . . . . ? O1A Co2 O5 C18 19.5(6) . . . . ? O1A Co2 O2H Co3 -24.7(3) . . . . ? O1A Co2 O2H Co4 78.0(4) . . . . ? O1A Co2 O1H Co3 -21.8(3) . . . 2_655 ? O1A Co2 O1H Co1 117.1(3) . . . . ? O1A Co2 O3 Co1 -107.51(17) . . . . ? O1A Co2 O3 C9 52.0(6) . . . . ? O1A Co3 O8 C36 80(4) . . . . ? O1A Co3 O2 C9 -17.8(6) . . . . ? O1A Co3 O2H Co2 24.4(3) . . . . ? O1A Co3 O2H Co4 -114.3(3) . . . . ? O1A Co3 O6 Co4 108.08(17) . . . . ? O1A Co3 O6 C18 -51.3(6) . . . 2_655 ? O10 C24 C25 C26 -121.4(9) . . . . ? C15 N4 C14 N3 -25.1(12) . . . . ? C15 N4 C14 C13 154.8(8) . . . . ? N5 C23 C22 C21 1.5(14) . . . . ? N5 C19 C20 C21 1.4(16) . . . . ? C6 N2 C5 N1 7.2(14) . . . . ? C6 N2 C5 C4 -174.2(9) . . . . ? N1 Co1 O1H Co2 158.7(2) . . . . ? N1 Co1 O1H Co3 -97.7(4) . . . 2_655 ? N1 Co1 O1 C6 24.6(7) . . . . ? N1 Co1 O12 C27 -145.5(7) . . . . ? N1 Co1 O3 Co2 64(2) . . . . ? N1 Co1 O3 C9 -91(2) . . . . ? N1 C1 C2 C3 0.1(16) . . . . ? N1 C5 C4 C3 -2.6(15) . . . . ? C1 N1 C5 N2 -178.2(8) . . . . ? C1 N1 C5 C4 3.3(13) . . . . ? C1 C2 C3 C4 0.6(17) . . . . ? N7 C28 C29 C30 -0.2(15) . . . . ? C33 N8 C32 N7 -169.0(8) . . . . ? C33 N8 C32 C31 9.6(15) . . . . ? C28 N7 C32 N8 179.5(8) . . . . ? C28 N7 C32 C31 0.9(13) . . . . ? C14 N4 C15 O4 13.4(13) . . . . ? C14 N4 C15 C16 -163.1(7) . . . . ? C14 N3 C10 C11 0.2(12) . . . . ? C14 C13 C12 C11 -2.5(13) . . . . ? N2 C6 C7 C8 151.1(7) . . . 2_655 ? N2 C5 C4 C3 178.8(9) . . . . ? C5 N1 C1 C2 -2.0(14) . . . . ? C31 C30 C29 C28 -0.2(14) . . . . ? C30 C31 C32 N8 -179.7(9) . . . . ? C30 C31 C32 N7 -1.3(14) . . . . ? C23 N6 C24 O10 5.6(15) . . . . ? C23 N6 C24 C25 -174.4(8) . . . . ? C23 N5 C19 C20 -0.8(14) . . . . ? C24 N6 C23 N5 178.4(8) . . . . ? C24 N6 C23 C22 -0.8(14) . . . . ? C24 C25 C26 C27 -83.7(10) . . . . ? C32 N8 C33 O7 -9.1(15) . . . . ? C32 N8 C33 C34 169.3(8) . . . . ? C32 N7 C28 C29 -0.1(13) . . . . ? C32 C31 C30 C29 0.9(14) . . . . ? C12 C11 C10 N3 1.9(13) . . . . ? C10 N3 C14 N4 176.3(7) . . . . ? C10 N3 C14 C13 -3.7(11) . . . . ? C10 C11 C12 C13 -0.7(13) . . . . ? C19 N5 C23 N6 -180.0(8) . . . . ? C19 N5 C23 C22 -0.7(13) . . . . ? C2 C3 C4 C5 0.5(17) . . . . ? C22 C21 C20 C19 -0.6(16) . . . . ? C20 C21 C22 C23 -0.8(15) . . . . ? O22A Cl20 O21A Cl20 0.0 . . . 2_655 ? O21A Cl20 O22A Cl20 -0.001(1) . . . 2_655 ? C7 C6 N2 C5 176.9(8) . . . . ? O15 Cl20 O22A Cl20 107.7(12) . . . 2_655 ? O15 Cl20 O21A Cl20 -108.0(11) . . . 2_655 ? O18 Cl20 O22A Cl20 -122.5(8) . . . 2_655 ? O18 Cl20 O21A Cl20 124.1(8) . . . 2_655 ? _database_code_depnum_ccdc_archive 'CCDC 939537' ####################################################################### # # 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_meru _audit_creation_date 2013-05-14 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:59:47, GUI svn.r4466) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C37 H38 Cu6 N8 O20, C H4 O' _chemical_formula_sum 'C38 H42 Cu6 N8 O21' _chemical_formula_weight 1328.04 _chemical_melting_point ? _chemical_oxdiff_formula C9H10N2O3Cu1 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y, -z+1/2' 3 'x+1/2, y+1/2, z' 4 '-x+1/2, y+1/2, -z+1/2' 5 '-x, -y, -z' 6 'x, -y, z-1/2' 7 '-x+1/2, -y+1/2, -z' 8 'x+1/2, -y+1/2, z-1/2' _cell_length_a 41.7229(8) _cell_length_b 13.7165(3) _cell_length_c 15.3592(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.5503(18) _cell_angle_gamma 90.00 _cell_volume 8786.7(3) _cell_formula_units_Z 8 _cell_measurement_reflns_used 8118 _cell_measurement_temperature 120.01(10) _cell_measurement_theta_max 73.7720 _cell_measurement_theta_min 2.8757 _exptl_absorpt_coefficient_mu 4.009 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.89968 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour green _exptl_crystal_colour_primary green _exptl_crystal_density_diffrn 2.008 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 5344 _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.06 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_unetI/netI 0.0375 _diffrn_reflns_limit_h_max 51 _diffrn_reflns_limit_h_min -50 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 17949 _diffrn_reflns_theta_full 72.48 _diffrn_reflns_theta_max 72.48 _diffrn_reflns_theta_min 3.39 _diffrn_ambient_temperature 120.01(10) _diffrn_detector_area_resol_mean 10.6501 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 14.00 39.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -39.9063 77.0000 120.0000 25 #__ type_ start__ end____ width___ exp.time_ 2 omega -116.00 -9.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -39.9063 -72.0000 118.0000 107 #__ type_ start__ end____ width___ exp.time_ 3 omega -71.00 -45.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -39.9063 77.0000 120.0000 26 #__ type_ start__ end____ width___ exp.time_ 4 omega -65.00 21.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -39.9063 57.0000 -90.0000 86 #__ type_ start__ end____ width___ exp.time_ 5 omega 126.00 177.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 107.7801 30.0000 -60.0000 51 #__ type_ start__ end____ width___ exp.time_ 6 omega 40.00 99.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 107.7801 -45.0000 120.0000 59 #__ type_ start__ end____ width___ exp.time_ 7 omega 105.00 176.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 107.7801 45.0000 -180.0000 71 #__ type_ start__ end____ width___ exp.time_ 8 omega 152.00 178.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 107.7801 125.0000 0.0000 26 #__ type_ start__ end____ width___ exp.time_ 9 omega 39.00 91.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 107.7801 -30.0000 0.0000 52 #__ type_ start__ end____ width___ exp.time_ 10 omega 98.00 124.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 107.7801 125.0000 0.0000 26 #__ type_ start__ end____ width___ exp.time_ 11 omega 37.00 89.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 107.7801 -30.0000 -150.0000 52 #__ type_ start__ end____ width___ exp.time_ 12 omega 100.00 177.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 107.7801 125.0000 120.0000 77 #__ type_ start__ end____ width___ exp.time_ 13 omega 34.00 98.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 107.7801 -45.0000 -180.0000 64 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0296373000 _diffrn_orient_matrix_UB_12 -0.0543616000 _diffrn_orient_matrix_UB_13 0.0328080000 _diffrn_orient_matrix_UB_21 0.0017585000 _diffrn_orient_matrix_UB_22 -0.0711652000 _diffrn_orient_matrix_UB_23 -0.0773148000 _diffrn_orient_matrix_UB_31 0.0219794000 _diffrn_orient_matrix_UB_32 -0.0676449000 _diffrn_orient_matrix_UB_33 0.0550257000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'SuperNova (Cu) X-ray Source' _reflns_number_gt 7420 _reflns_number_total 8599 _reflns_odcompleteness_completeness 99.91 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XLMP, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.931 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.096 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 688 _refine_ls_number_reflns 8599 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0338 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+13.2663P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0881 _refine_ls_wR_factor_ref 0.0940 _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. The O-H hydrogens were located in the electron difference map. The O-H distances were allowed to refine at a fixed distance of 0.84A, with a thermal parameter 1.5 times the atom they were riding on. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups, All O(H,H) groups 2. Restrained distances O50-H50 = O65-H65 = O3-H3A = O3-H3B 0.84 with sigma of 0.01 O35-H35A = O35-H35B 0.84 with sigma of 0.02 O28-H28A = O28-H28B 0.84 with sigma of 0.02 3.a Ternary CH refined with riding coordinates: C34(H34), C38(H38), C41(H41), C43(H43) 3.b Secondary CH2 refined with riding coordinates: C51(H51A,H51B), C52(H52A,H52B), C54(H54A,H54B), C62(H62A,H62B) 3.c Aromatic/amide H refined with riding coordinates: C33(H33), C36(H36), C37(H37), C39(H39), C46(H46), C48(H48), C53(H53), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60), C61(H61), C63(H63), C64(H64) 3.d Idealised Me refined as rotating group: C69(H69A,H69B,H69C), C1(H1A,H1B,H1C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Cu1 Cu 0.658043(9) 0.83753(3) 0.08793(3) 0.01519(10) Uani 1 1 d . . . Cu5 Cu 0.544135(9) 0.77775(3) 0.25608(2) 0.01400(10) Uani 1 1 d . . . Cu2 Cu 0.699567(10) 0.76390(3) 0.23939(3) 0.01530(10) Uani 1 1 d . . . Cu4 Cu 0.588173(9) 0.94728(3) 0.31043(2) 0.01359(10) Uani 1 1 d . . . Cu6 Cu 0.581906(10) 0.60236(3) 0.19343(3) 0.01511(10) Uani 1 1 d . . . Cu3 Cu 0.662185(10) 0.69377(3) 0.39656(3) 0.01629(10) Uani 1 1 d . . . O1 O 0.69596(5) 0.87268(14) 0.15980(13) 0.0162(4) Uani 1 1 d . . . O2 O 0.69684(5) 0.65553(15) 0.31858(12) 0.0171(4) Uani 1 1 d . . . O3 O 0.58735(5) 1.06665(17) 0.41710(14) 0.0241(5) Uani 1 1 d D . . H3A H 0.6011(8) 1.108(2) 0.432(3) 0.036 Uiso 1 1 d D . . H3B H 0.5723(7) 1.079(3) 0.450(2) 0.036 Uiso 1 1 d D . . O4 O 0.61131(5) 0.68824(15) 0.12998(13) 0.0177(4) Uani 1 1 d . . . O5 O 0.61843(5) 0.85787(16) 0.37145(13) 0.0188(4) Uani 1 1 d . . . O6 O 0.55172(4) 0.87055(14) 0.34863(12) 0.0144(4) Uani 1 1 d . . . O7 O 0.54559(5) 0.68501(14) 0.16149(12) 0.0154(4) Uani 1 1 d . . . O8 O 0.63021(5) 0.90938(15) 0.16596(13) 0.0181(4) Uani 1 1 d . . . N9 N 0.53983(6) 0.87529(17) 0.16592(15) 0.0154(4) Uani 1 1 d . . . N10 N 0.54223(6) 0.68086(18) 0.34750(15) 0.0161(5) Uani 1 1 d . . . N11 N 0.70129(6) 0.66612(18) 0.14874(16) 0.0170(5) Uani 1 1 d . . . O12 O 0.62507(5) 1.02055(15) 0.26958(13) 0.0168(4) Uani 1 1 d . . . O13 O 0.70321(5) 0.49792(16) 0.13448(14) 0.0236(4) Uani 1 1 d . . . O14 O 0.62710(5) 0.74225(15) 0.46948(13) 0.0189(4) Uani 1 1 d . . . O15 O 0.61974(5) 0.79200(15) 0.02252(13) 0.0178(4) Uani 1 1 d . . . N16 N 0.70430(6) 0.86127(18) 0.33012(16) 0.0173(5) Uani 1 1 d . . . O17 O 0.63096(5) 0.62765(15) 0.32207(13) 0.0195(4) Uani 1 1 d . . . O18 O 0.53687(5) 0.88721(16) 0.01558(13) 0.0212(4) Uani 1 1 d . . . O19 O 0.61871(5) 0.51815(15) 0.22139(13) 0.0184(4) Uani 1 1 d . . . O20 O 0.54133(5) 0.67402(16) 0.49841(13) 0.0219(4) Uani 1 1 d . . . N21 N 0.69333(6) 0.77898(19) 0.45992(16) 0.0183(5) Uani 1 1 d . . . C22 C 0.61095(7) 0.8136(2) 0.44010(18) 0.0167(5) Uani 1 1 d . . . C23 C 0.63751(7) 0.5521(2) 0.27914(19) 0.0177(6) Uani 1 1 d . . . N24 N 0.55517(6) 0.53358(18) 0.28120(15) 0.0170(5) Uani 1 1 d . . . N25 N 0.55846(6) 1.02057(18) 0.22942(15) 0.0160(5) Uani 1 1 d . . . C26 C 0.53705(7) 0.9772(2) 0.17574(17) 0.0153(5) Uani 1 1 d . . . C27 C 0.54400(6) 0.7185(2) 0.42852(19) 0.0168(5) Uani 1 1 d . . . O28 O 0.57330(7) 0.47840(19) 0.08486(17) 0.0326(5) Uani 1 1 d D . . C29 C 0.53970(6) 0.8402(2) 0.08429(18) 0.0165(5) Uani 1 1 d . . . C30 C 0.53691(7) 0.5801(2) 0.33885(18) 0.0172(5) Uani 1 1 d . . . N31 N 0.68627(6) 0.74783(18) 0.02035(16) 0.0183(5) Uani 1 1 d . . . C32 C 0.70119(7) 0.5735(2) 0.17741(19) 0.0182(6) Uani 1 1 d . . . C33 C 0.72975(7) 0.6352(2) 0.0137(2) 0.0214(6) Uani 1 1 d . . . H33 H 0.7441 0.5917 0.0430 0.026 Uiso 1 1 calc R . . C34 C 0.54298(6) 0.7291(2) 0.07869(17) 0.0151(5) Uani 1 1 d . . . H34 H 0.5228 0.7041 0.0502 0.018 Uiso 1 1 calc R . . O35 O 0.66091(5) 0.96727(18) -0.02017(15) 0.0253(5) Uani 1 1 d D . . C36 C 0.69917(8) 0.7620(2) 0.54559(19) 0.0227(6) Uani 1 1 d . . . H36 H 0.6860 0.7167 0.5748 0.027 Uiso 1 1 calc R . . C37 C 0.51340(7) 1.0312(2) 0.13039(18) 0.0182(5) Uani 1 1 d . . . H37 H 0.4972 0.9990 0.0968 0.022 Uiso 1 1 calc R . . C38 C 0.69772(7) 0.5640(2) 0.27627(19) 0.0186(6) Uani 1 1 d . . . H38 H 0.7173 0.5294 0.2992 0.022 Uiso 1 1 calc R . . C39 C 0.72361(8) 0.8080(3) 0.5922(2) 0.0271(7) Uani 1 1 d . . . H39 H 0.7271 0.7952 0.6525 0.033 Uiso 1 1 calc R . . O40 O 0.70629(6) 1.02897(16) 0.34639(14) 0.0250(5) Uani 1 1 d . . . C41 C 0.69915(7) 0.9642(2) 0.20230(18) 0.0170(5) Uani 1 1 d . . . H41 H 0.7189 0.9961 0.1800 0.020 Uiso 1 1 calc R . . C42 C 0.70576(7) 0.6820(2) 0.05979(19) 0.0177(5) Uani 1 1 d . . . C43 C 0.55090(7) 0.8278(2) 0.43245(18) 0.0161(5) Uani 1 1 d . . . H43 H 0.5328 0.8589 0.4635 0.019 Uiso 1 1 calc R . . C44 C 0.70381(7) 0.9536(2) 0.30165(19) 0.0180(6) Uani 1 1 d . . . C45 C 0.63989(6) 0.9843(2) 0.20651(18) 0.0151(5) Uani 1 1 d . . . C46 C 0.51433(7) 0.5292(2) 0.38677(19) 0.0197(6) Uani 1 1 d . . . H46 H 0.5005 0.5636 0.4242 0.024 Uiso 1 1 calc R . . C47 C 0.60269(7) 0.7287(2) 0.05990(18) 0.0151(5) Uani 1 1 d . . . C48 C 0.53763(8) 1.1760(2) 0.1855(2) 0.0225(6) Uani 1 1 d . . . H48 H 0.5392 1.2451 0.1869 0.027 Uiso 1 1 calc R . . C49 C 0.71127(7) 0.8452(2) 0.41890(19) 0.0182(6) Uani 1 1 d . . . O50 O 0.66743(7) 0.56111(19) 0.49375(17) 0.0353(6) Uani 1 1 d D . . H50 H 0.6818(9) 0.547(4) 0.531(3) 0.053 Uiso 1 1 d D . . C51 C 0.67077(7) 1.0325(2) 0.18128(19) 0.0177(5) Uani 1 1 d . . . H51A H 0.6736 1.0945 0.2137 0.021 Uiso 1 1 calc R . . H51B H 0.6700 1.0476 0.1182 0.021 Uiso 1 1 calc R . . C52 C 0.57062(7) 0.7023(2) 0.01834(18) 0.0169(5) Uani 1 1 d . . . H52A H 0.5700 0.6315 0.0060 0.020 Uiso 1 1 calc R . . H52B H 0.5678 0.7374 -0.0377 0.020 Uiso 1 1 calc R . . C53 C 0.53255(8) 0.3812(2) 0.3246(2) 0.0244(6) Uani 1 1 d . . . H53 H 0.5324 0.3120 0.3211 0.029 Uiso 1 1 calc R . . C54 C 0.58153(7) 0.8458(2) 0.48784(18) 0.0170(5) Uani 1 1 d . . . H54A H 0.5833 0.9161 0.5018 0.020 Uiso 1 1 calc R . . H54B H 0.5803 0.8095 0.5433 0.020 Uiso 1 1 calc R . . C55 C 0.73269(8) 0.6522(2) -0.0744(2) 0.0255(6) Uani 1 1 d . . . H55 H 0.7491 0.6215 -0.1062 0.031 Uiso 1 1 calc R . . C56 C 0.55883(7) 1.1190(2) 0.23360(19) 0.0192(6) Uani 1 1 d . . . H56 H 0.5742 1.1501 0.2710 0.023 Uiso 1 1 calc R . . C57 C 0.68880(8) 0.7628(2) -0.0667(2) 0.0230(6) Uani 1 1 d . . . H57 H 0.6747 0.8079 -0.0948 0.028 Uiso 1 1 calc R . . C58 C 0.55305(7) 0.4353(2) 0.2754(2) 0.0217(6) Uani 1 1 d . . . H58 H 0.5663 0.4023 0.2355 0.026 Uiso 1 1 calc R . . C59 C 0.51206(7) 0.4297(2) 0.3798(2) 0.0233(6) Uani 1 1 d . . . H59 H 0.4967 0.3946 0.4120 0.028 Uiso 1 1 calc R . . C60 C 0.71103(8) 0.7153(3) -0.1154(2) 0.0273(7) Uani 1 1 d . . . H60 H 0.7116 0.7255 -0.1765 0.033 Uiso 1 1 calc R . . C61 C 0.74265(7) 0.8728(2) 0.5493(2) 0.0259(7) Uani 1 1 d . . . H61 H 0.7599 0.9043 0.5797 0.031 Uiso 1 1 calc R . . C62 C 0.66902(7) 0.4994(2) 0.2964(2) 0.0203(6) Uani 1 1 d . . . H62A H 0.6697 0.4398 0.2601 0.024 Uiso 1 1 calc R . . H62B H 0.6704 0.4791 0.3583 0.024 Uiso 1 1 calc R . . C63 C 0.51403(7) 1.1308(2) 0.13521(19) 0.0203(6) Uani 1 1 d . . . H63 H 0.4984 1.1685 0.1043 0.024 Uiso 1 1 calc R . . C64 C 0.73681(7) 0.8922(2) 0.4621(2) 0.0222(6) Uani 1 1 d . . . H64 H 0.7499 0.9368 0.4320 0.027 Uiso 1 1 calc R . . C69 C 0.64207(10) 0.4976(3) 0.5046(3) 0.0424(9) Uani 1 1 d . . . H69A H 0.6228 0.5236 0.4749 0.064 Uiso 1 1 calc R . . H69B H 0.6381 0.4902 0.5669 0.064 Uiso 1 1 calc R . . H69C H 0.6473 0.4339 0.4798 0.064 Uiso 1 1 calc R . . O65 O 0.61114(8) 0.6810(2) 0.63511(19) 0.0498(8) Uani 1 1 d D . . H65 H 0.6159(15) 0.709(4) 0.588(2) 0.075 Uiso 1 1 d D . . C1 C 0.62918(11) 0.7217(3) 0.7050(3) 0.0495(10) Uani 1 1 d . . . H1A H 0.6519 0.7054 0.6988 0.074 Uiso 1 1 calc R . . H1B H 0.6216 0.6954 0.7601 0.074 Uiso 1 1 calc R . . H1C H 0.6266 0.7928 0.7047 0.074 Uiso 1 1 calc R . . H28A H 0.5910(5) 0.4564(18) 0.0653(15) -0.011(5) Uiso 1 1 d D . . H28B H 0.5608(10) 0.440(3) 0.058(3) 0.049(14) Uiso 1 1 d D . . H35A H 0.6448(9) 0.994(4) -0.043(3) 0.054(15) Uiso 1 1 d D . . H35B H 0.6751(11) 0.963(5) -0.056(3) 0.072(19) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01387(19) 0.0160(2) 0.01573(19) -0.00167(15) 0.00152(14) 0.00081(15) Cu5 0.01600(19) 0.0130(2) 0.01294(19) 0.00204(14) -0.00088(14) -0.00064(15) Cu2 0.01600(19) 0.0141(2) 0.0157(2) -0.00351(15) -0.00060(14) 0.00062(15) Cu4 0.01263(18) 0.0147(2) 0.01342(19) 0.00148(14) 0.00074(14) 0.00028(15) Cu6 0.01541(19) 0.0139(2) 0.0159(2) 0.00212(15) -0.00164(14) -0.00065(15) Cu3 0.01490(19) 0.0178(2) 0.0160(2) -0.00067(15) -0.00267(15) 0.00106(16) O1 0.0163(9) 0.0137(9) 0.0188(9) -0.0034(7) 0.0006(7) 0.0006(7) O2 0.0178(9) 0.0171(10) 0.0162(9) -0.0033(7) -0.0006(7) 0.0009(8) O3 0.0253(11) 0.0245(11) 0.0229(11) -0.0095(9) 0.0049(8) -0.0048(9) O4 0.0146(9) 0.0181(10) 0.0205(10) 0.0029(8) -0.0014(7) -0.0012(8) O5 0.0154(9) 0.0228(10) 0.0182(9) 0.0052(8) 0.0026(7) 0.0024(8) O6 0.0161(9) 0.0146(9) 0.0123(9) 0.0020(7) -0.0005(7) -0.0011(7) O7 0.0176(9) 0.0143(9) 0.0143(9) 0.0030(7) -0.0008(7) -0.0016(7) O8 0.0162(9) 0.0178(10) 0.0203(10) -0.0022(8) 0.0034(7) -0.0005(8) N9 0.0185(11) 0.0141(11) 0.0134(11) 0.0007(9) -0.0031(8) 0.0009(9) N10 0.0180(11) 0.0137(11) 0.0167(11) 0.0031(9) 0.0008(9) -0.0010(9) N11 0.0165(11) 0.0156(12) 0.0189(11) -0.0023(9) -0.0013(9) 0.0022(9) O12 0.0160(9) 0.0154(9) 0.0193(9) -0.0010(8) 0.0043(7) -0.0002(8) O13 0.0275(11) 0.0172(10) 0.0260(11) -0.0067(8) 0.0001(8) 0.0024(9) O14 0.0179(9) 0.0214(10) 0.0172(9) 0.0040(8) -0.0013(7) 0.0022(8) O15 0.0183(9) 0.0191(10) 0.0160(9) 0.0015(8) 0.0009(7) -0.0011(8) N16 0.0167(11) 0.0174(12) 0.0179(11) -0.0046(9) -0.0001(9) -0.0008(9) O17 0.0180(9) 0.0207(10) 0.0196(10) -0.0004(8) -0.0028(7) 0.0020(8) O18 0.0256(10) 0.0240(11) 0.0141(9) 0.0045(8) -0.0007(8) 0.0041(9) O19 0.0174(9) 0.0159(10) 0.0216(10) 0.0009(8) -0.0046(7) -0.0020(8) O20 0.0270(11) 0.0232(11) 0.0157(10) 0.0061(8) 0.0016(8) -0.0049(9) N21 0.0181(11) 0.0205(12) 0.0161(11) -0.0030(9) -0.0020(9) 0.0044(10) C22 0.0167(13) 0.0187(14) 0.0147(12) 0.0000(10) -0.0021(10) -0.0021(11) C23 0.0193(13) 0.0146(13) 0.0192(13) 0.0060(10) 0.0004(10) -0.0024(11) N24 0.0199(11) 0.0138(11) 0.0171(11) 0.0026(9) -0.0027(9) -0.0005(9) N25 0.0171(11) 0.0142(11) 0.0167(11) 0.0011(9) 0.0012(8) -0.0003(9) C26 0.0162(12) 0.0145(13) 0.0151(12) 0.0041(10) 0.0001(10) 0.0000(10) C27 0.0122(12) 0.0186(14) 0.0197(14) 0.0016(11) 0.0013(10) -0.0010(10) O28 0.0380(14) 0.0249(12) 0.0345(13) -0.0064(10) -0.0057(11) -0.0022(11) C29 0.0124(12) 0.0200(14) 0.0169(13) 0.0021(11) -0.0010(9) 0.0002(10) C30 0.0162(13) 0.0174(14) 0.0180(13) 0.0036(11) -0.0042(10) -0.0003(11) N31 0.0163(11) 0.0197(12) 0.0188(12) -0.0039(9) 0.0011(9) -0.0001(9) C32 0.0140(12) 0.0188(14) 0.0216(14) -0.0043(11) -0.0030(10) 0.0023(11) C33 0.0200(14) 0.0163(14) 0.0282(15) -0.0040(12) 0.0039(11) -0.0001(11) C34 0.0151(12) 0.0172(13) 0.0129(12) 0.0000(10) -0.0026(10) 0.0002(10) O35 0.0227(11) 0.0287(12) 0.0246(11) 0.0039(9) 0.0014(9) 0.0022(9) C36 0.0250(15) 0.0256(16) 0.0174(14) -0.0037(12) 0.0000(11) 0.0065(12) C37 0.0194(13) 0.0191(14) 0.0162(13) 0.0022(11) 0.0004(10) 0.0032(11) C38 0.0179(13) 0.0168(14) 0.0207(14) -0.0011(11) -0.0054(10) 0.0024(11) C39 0.0330(17) 0.0333(18) 0.0148(13) -0.0076(12) -0.0050(12) 0.0130(14) O40 0.0321(12) 0.0170(10) 0.0260(11) -0.0072(9) 0.0003(9) -0.0004(9) C41 0.0153(12) 0.0162(13) 0.0197(13) -0.0032(11) 0.0038(10) -0.0026(10) C42 0.0180(13) 0.0153(13) 0.0197(13) -0.0048(11) 0.0006(10) -0.0031(11) C43 0.0151(12) 0.0179(14) 0.0155(13) 0.0028(10) 0.0037(10) 0.0007(10) C44 0.0130(12) 0.0172(14) 0.0239(14) -0.0041(11) 0.0010(10) -0.0016(10) C45 0.0134(12) 0.0149(13) 0.0172(12) 0.0027(10) 0.0007(10) 0.0023(10) C46 0.0171(13) 0.0190(14) 0.0230(14) 0.0028(11) -0.0005(11) -0.0021(11) C47 0.0162(12) 0.0125(13) 0.0166(13) -0.0019(10) 0.0015(10) 0.0009(10) C48 0.0279(15) 0.0174(14) 0.0225(14) 0.0006(11) 0.0032(11) 0.0022(12) C49 0.0157(13) 0.0194(14) 0.0194(13) -0.0057(11) -0.0022(10) 0.0025(11) O50 0.0442(15) 0.0303(13) 0.0309(13) 0.0130(10) -0.0113(11) -0.0056(11) C51 0.0176(13) 0.0139(13) 0.0219(13) 0.0001(10) 0.0067(10) -0.0003(11) C52 0.0175(13) 0.0177(13) 0.0153(12) -0.0014(10) -0.0008(10) -0.0014(11) C53 0.0323(16) 0.0153(14) 0.0254(15) 0.0031(11) -0.0050(12) -0.0042(12) C54 0.0168(13) 0.0198(14) 0.0146(12) 0.0016(10) 0.0021(10) 0.0002(11) C55 0.0235(15) 0.0209(15) 0.0327(17) -0.0074(12) 0.0108(12) -0.0038(12) C56 0.0216(14) 0.0159(14) 0.0202(13) -0.0001(11) 0.0015(10) -0.0018(11) C57 0.0269(15) 0.0225(15) 0.0196(14) -0.0015(11) 0.0020(11) -0.0008(12) C58 0.0250(14) 0.0169(14) 0.0230(14) 0.0024(11) -0.0015(11) 0.0007(12) C59 0.0230(14) 0.0246(15) 0.0221(15) 0.0066(12) -0.0009(11) -0.0067(12) C60 0.0329(17) 0.0296(17) 0.0197(15) -0.0038(12) 0.0063(12) -0.0034(14) C61 0.0199(14) 0.0269(16) 0.0304(16) -0.0153(13) -0.0084(12) 0.0062(12) C62 0.0177(13) 0.0162(14) 0.0266(15) 0.0034(11) -0.0043(11) 0.0009(11) C63 0.0244(14) 0.0199(14) 0.0167(13) 0.0034(11) 0.0009(11) 0.0085(12) C64 0.0188(13) 0.0208(15) 0.0267(15) -0.0099(12) -0.0024(11) 0.0027(12) C69 0.037(2) 0.049(2) 0.040(2) 0.0131(18) 0.0051(16) -0.0035(18) O65 0.063(2) 0.0511(18) 0.0352(15) 0.0133(13) -0.0042(13) -0.0184(16) C1 0.042(2) 0.042(2) 0.064(3) 0.004(2) 0.005(2) -0.0020(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 Cu2 3.0357(6) . ? Cu1 O1 1.964(2) . ? Cu1 O8 1.957(2) . ? Cu1 O15 1.966(2) . ? Cu1 N31 2.011(2) . ? Cu1 O35 2.439(2) . ? Cu5 Cu6 3.0461(6) . ? Cu5 O6 1.9279(19) . ? Cu5 O7 1.933(2) . ? Cu5 N9 1.930(2) . ? Cu5 N10 1.937(2) . ? Cu2 O1 1.932(2) . ? Cu2 O2 1.926(2) . ? Cu2 N11 1.936(2) . ? Cu2 N16 1.937(2) . ? Cu4 O3 2.317(2) . ? Cu4 O5 1.978(2) . ? Cu4 O6 1.9527(19) . ? Cu4 O12 1.956(2) . ? Cu4 N25 2.003(2) . ? Cu6 O4 1.977(2) . ? Cu6 O7 1.945(2) . ? Cu6 O19 1.960(2) . ? Cu6 N24 2.008(2) . ? Cu6 O28 2.402(2) . ? Cu3 O2 1.973(2) . ? Cu3 O14 1.982(2) . ? Cu3 O17 1.936(2) . ? Cu3 N21 1.983(2) . ? Cu3 O50 2.360(2) . ? O1 C41 1.420(3) . ? O2 C38 1.415(3) . ? O3 H3A 0.837(10) . ? O3 H3B 0.838(10) . ? O4 C47 1.255(4) . ? O5 C22 1.264(4) . ? O6 C43 1.416(3) . ? O7 C34 1.410(3) . ? O8 C45 1.262(4) . ? N9 C26 1.411(4) . ? N9 C29 1.343(4) . ? N10 C27 1.347(4) . ? N10 C30 1.406(4) . ? N11 C32 1.344(4) . ? N11 C42 1.401(4) . ? O12 C45 1.265(4) . ? O13 C32 1.233(4) . ? O14 C22 1.264(4) . ? O15 C47 1.270(4) . ? N16 C44 1.340(4) . ? N16 C49 1.404(4) . ? O17 C23 1.262(4) . ? O18 C29 1.240(4) . ? O19 C23 1.258(4) . ? O20 C27 1.242(4) . ? N21 C36 1.352(4) . ? N21 C49 1.345(4) . ? C22 C54 1.513(4) . ? C23 C62 1.518(4) . ? N24 C30 1.345(4) . ? N24 C58 1.354(4) . ? N25 C26 1.339(4) . ? N25 C56 1.352(4) . ? C26 C37 1.404(4) . ? C27 C43 1.527(4) . ? O28 H28A 0.858(17) . ? O28 H28B 0.84(2) . ? C29 C34 1.532(4) . ? C30 C46 1.398(4) . ? N31 C42 1.348(4) . ? N31 C57 1.360(4) . ? C32 C38 1.535(4) . ? C33 H33 0.9500 . ? C33 C42 1.397(4) . ? C33 C55 1.382(5) . ? C34 H34 1.0000 . ? C34 C52 1.543(4) . ? O35 H35A 0.84(2) . ? O35 H35B 0.82(2) . ? C36 H36 0.9500 . ? C36 C39 1.383(5) . ? C37 H37 0.9500 . ? C37 C63 1.368(4) . ? C38 H38 1.0000 . ? C38 C62 1.528(4) . ? C39 H39 0.9500 . ? C39 C61 1.372(5) . ? O40 C44 1.244(4) . ? C41 H41 1.0000 . ? C41 C44 1.540(4) . ? C41 C51 1.537(4) . ? C43 H43 1.0000 . ? C43 C54 1.536(4) . ? C45 C51 1.508(4) . ? C46 H46 0.9500 . ? C46 C59 1.373(4) . ? C47 C52 1.511(4) . ? C48 H48 0.9500 . ? C48 C56 1.380(4) . ? C48 C63 1.382(4) . ? C49 C64 1.398(4) . ? O50 H50 0.839(10) . ? O50 C69 1.384(5) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 H53 0.9500 . ? C53 C58 1.375(4) . ? C53 C59 1.390(5) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 H55 0.9500 . ? C55 C60 1.390(5) . ? C56 H56 0.9500 . ? C57 H57 0.9500 . ? C57 C60 1.372(5) . ? C58 H58 0.9500 . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 H61 0.9500 . ? C61 C64 1.381(5) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? O65 H65 0.847(10) . ? O65 C1 1.409(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 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 O1 Cu1 Cu2 38.45(6) . . ? O1 Cu1 O15 174.91(9) . . ? O1 Cu1 N31 88.07(9) . . ? O1 Cu1 O35 98.62(8) . . ? O8 Cu1 Cu2 91.95(6) . . ? O8 Cu1 O1 90.83(8) . . ? O8 Cu1 O15 89.16(9) . . ? O8 Cu1 N31 171.68(10) . . ? O8 Cu1 O35 95.18(8) . . ? O15 Cu1 Cu2 136.47(6) . . ? O15 Cu1 N31 91.21(9) . . ? O15 Cu1 O35 86.45(8) . . ? N31 Cu1 Cu2 82.07(7) . . ? N31 Cu1 O35 93.14(9) . . ? O35 Cu1 Cu2 136.63(6) . . ? O6 Cu5 Cu6 132.71(6) . . ? O6 Cu5 O7 168.72(8) . . ? O6 Cu5 N9 94.68(9) . . ? O6 Cu5 N10 85.85(9) . . ? O7 Cu5 Cu6 38.36(6) . . ? O7 Cu5 N10 95.51(9) . . ? N9 Cu5 Cu6 111.08(7) . . ? N9 Cu5 O7 85.48(9) . . ? N9 Cu5 N10 172.27(10) . . ? N10 Cu5 Cu6 73.67(7) . . ? O1 Cu2 Cu1 39.21(6) . . ? O1 Cu2 N11 94.80(9) . . ? O1 Cu2 N16 85.84(9) . . ? O2 Cu2 Cu1 134.30(6) . . ? O2 Cu2 O1 172.14(8) . . ? O2 Cu2 N11 85.61(9) . . ? O2 Cu2 N16 94.85(10) . . ? N11 Cu2 Cu1 73.19(7) . . ? N11 Cu2 N16 172.02(10) . . ? N16 Cu2 Cu1 111.53(7) . . ? O5 Cu4 O3 97.15(9) . . ? O5 Cu4 N25 169.08(9) . . ? O6 Cu4 O3 98.16(8) . . ? O6 Cu4 O5 90.90(8) . . ? O6 Cu4 O12 178.08(9) . . ? O6 Cu4 N25 89.03(9) . . ? O12 Cu4 O3 83.71(8) . . ? O12 Cu4 O5 88.44(9) . . ? O12 Cu4 N25 91.27(9) . . ? N25 Cu4 O3 93.66(9) . . ? O4 Cu6 Cu5 91.05(6) . . ? O4 Cu6 N24 166.99(9) . . ? O4 Cu6 O28 99.36(9) . . ? O7 Cu6 Cu5 38.10(6) . . ? O7 Cu6 O4 91.02(8) . . ? O7 Cu6 O19 178.04(9) . . ? O7 Cu6 N24 90.01(9) . . ? O7 Cu6 O28 97.86(9) . . ? O19 Cu6 Cu5 143.63(6) . . ? O19 Cu6 O4 88.07(8) . . ? O19 Cu6 N24 91.27(9) . . ? O19 Cu6 O28 80.58(9) . . ? N24 Cu6 Cu5 81.81(7) . . ? N24 Cu6 O28 93.34(10) . . ? O28 Cu6 Cu5 135.20(7) . . ? O2 Cu3 O14 175.33(9) . . ? O2 Cu3 N21 88.47(9) . . ? O2 Cu3 O50 97.01(10) . . ? O14 Cu3 N21 90.52(9) . . ? O14 Cu3 O50 87.62(9) . . ? O17 Cu3 O2 90.53(9) . . ? O17 Cu3 O14 89.75(9) . . ? O17 Cu3 N21 170.95(10) . . ? O17 Cu3 O50 93.56(9) . . ? N21 Cu3 O50 95.49(10) . . ? Cu2 O1 Cu1 102.35(9) . . ? C41 O1 Cu1 122.66(17) . . ? C41 O1 Cu2 112.78(16) . . ? Cu2 O2 Cu3 103.60(9) . . ? C38 O2 Cu2 113.10(17) . . ? C38 O2 Cu3 122.91(18) . . ? Cu4 O3 H3A 131(3) . . ? Cu4 O3 H3B 127(3) . . ? H3A O3 H3B 102(4) . . ? C47 O4 Cu6 121.27(18) . . ? C22 O5 Cu4 121.65(18) . . ? Cu5 O6 Cu4 104.36(9) . . ? C43 O6 Cu5 112.91(17) . . ? C43 O6 Cu4 122.32(16) . . ? Cu5 O7 Cu6 103.55(9) . . ? C34 O7 Cu5 113.09(17) . . ? C34 O7 Cu6 121.23(17) . . ? C45 O8 Cu1 121.66(18) . . ? C26 N9 Cu5 128.05(19) . . ? C29 N9 Cu5 114.8(2) . . ? C29 N9 C26 117.2(2) . . ? C27 N10 Cu5 113.8(2) . . ? C27 N10 C30 118.0(2) . . ? C30 N10 Cu5 128.01(19) . . ? C32 N11 Cu2 114.74(19) . . ? C32 N11 C42 117.9(2) . . ? C42 N11 Cu2 127.0(2) . . ? C45 O12 Cu4 116.67(18) . . ? C22 O14 Cu3 116.91(18) . . ? C47 O15 Cu1 116.35(18) . . ? C44 N16 Cu2 114.63(19) . . ? C44 N16 C49 117.8(2) . . ? C49 N16 Cu2 127.3(2) . . ? C23 O17 Cu3 122.78(19) . . ? C23 O19 Cu6 113.96(19) . . ? C36 N21 Cu3 118.3(2) . . ? C49 N21 Cu3 122.28(19) . . ? C49 N21 C36 119.0(3) . . ? O5 C22 O14 121.9(3) . . ? O5 C22 C54 119.1(3) . . ? O14 C22 C54 119.0(2) . . ? O17 C23 C62 119.9(3) . . ? O19 C23 O17 122.2(3) . . ? O19 C23 C62 117.9(3) . . ? C30 N24 Cu6 123.7(2) . . ? C30 N24 C58 118.6(3) . . ? C58 N24 Cu6 117.4(2) . . ? C26 N25 Cu4 123.44(19) . . ? C26 N25 C56 118.7(2) . . ? C56 N25 Cu4 117.8(2) . . ? N25 C26 N9 116.8(2) . . ? N25 C26 C37 121.3(3) . . ? C37 C26 N9 121.9(3) . . ? N10 C27 C43 114.7(2) . . ? O20 C27 N10 127.3(3) . . ? O20 C27 C43 118.0(3) . . ? Cu6 O28 H28A 112.2(17) . . ? Cu6 O28 H28B 150(4) . . ? H28A O28 H28B 98(4) . . ? N9 C29 C34 114.3(2) . . ? O18 C29 N9 127.3(3) . . ? O18 C29 C34 118.4(3) . . ? N24 C30 N10 116.0(3) . . ? N24 C30 C46 120.8(3) . . ? C46 C30 N10 123.2(3) . . ? C42 N31 Cu1 122.2(2) . . ? C42 N31 C57 118.8(3) . . ? C57 N31 Cu1 118.5(2) . . ? N11 C32 C38 114.0(2) . . ? O13 C32 N11 128.2(3) . . ? O13 C32 C38 117.8(3) . . ? C42 C33 H33 119.9 . . ? C55 C33 H33 119.9 . . ? C55 C33 C42 120.2(3) . . ? O7 C34 C29 112.4(2) . . ? O7 C34 H34 106.9 . . ? O7 C34 C52 113.5(2) . . ? C29 C34 H34 106.9 . . ? C29 C34 C52 109.9(2) . . ? C52 C34 H34 106.9 . . ? Cu1 O35 H35A 124(4) . . ? Cu1 O35 H35B 117(4) . . ? H35A O35 H35B 109(5) . . ? N21 C36 H36 118.8 . . ? N21 C36 C39 122.4(3) . . ? C39 C36 H36 118.8 . . ? C26 C37 H37 120.4 . . ? C63 C37 C26 119.2(3) . . ? C63 C37 H37 120.4 . . ? O2 C38 C32 112.5(2) . . ? O2 C38 H38 106.9 . . ? O2 C38 C62 113.0(2) . . ? C32 C38 H38 106.9 . . ? C62 C38 C32 110.2(2) . . ? C62 C38 H38 106.9 . . ? C36 C39 H39 120.8 . . ? C61 C39 C36 118.4(3) . . ? C61 C39 H39 120.8 . . ? O1 C41 H41 107.3 . . ? O1 C41 C44 112.3(2) . . ? O1 C41 C51 112.3(2) . . ? C44 C41 H41 107.3 . . ? C51 C41 H41 107.3 . . ? C51 C41 C44 110.0(2) . . ? N31 C42 N11 116.6(3) . . ? N31 C42 C33 120.8(3) . . ? C33 C42 N11 122.6(3) . . ? O6 C43 C27 112.3(2) . . ? O6 C43 H43 107.1 . . ? O6 C43 C54 113.4(2) . . ? C27 C43 H43 107.1 . . ? C27 C43 C54 109.5(2) . . ? C54 C43 H43 107.1 . . ? N16 C44 C41 114.4(2) . . ? O40 C44 N16 127.2(3) . . ? O40 C44 C41 118.4(3) . . ? O8 C45 O12 122.8(3) . . ? O8 C45 C51 119.6(2) . . ? O12 C45 C51 117.6(2) . . ? C30 C46 H46 120.0 . . ? C59 C46 C30 120.1(3) . . ? C59 C46 H46 120.0 . . ? O4 C47 O15 122.6(3) . . ? O4 C47 C52 119.1(2) . . ? O15 C47 C52 118.3(2) . . ? C56 C48 H48 120.6 . . ? C56 C48 C63 118.8(3) . . ? C63 C48 H48 120.6 . . ? N21 C49 N16 117.2(2) . . ? N21 C49 C64 121.1(3) . . ? C64 C49 N16 121.6(3) . . ? Cu3 O50 H50 131(4) . . ? C69 O50 Cu3 120.2(2) . . ? C69 O50 H50 108(4) . . ? C41 C51 H51A 109.7 . . ? C41 C51 H51B 109.7 . . ? C45 C51 C41 109.7(2) . . ? C45 C51 H51A 109.7 . . ? C45 C51 H51B 109.7 . . ? H51A C51 H51B 108.2 . . ? C34 C52 H52A 109.5 . . ? C34 C52 H52B 109.5 . . ? C47 C52 C34 110.9(2) . . ? C47 C52 H52A 109.5 . . ? C47 C52 H52B 109.5 . . ? H52A C52 H52B 108.0 . . ? C58 C53 H53 120.7 . . ? C58 C53 C59 118.6(3) . . ? C59 C53 H53 120.7 . . ? C22 C54 C43 111.0(2) . . ? C22 C54 H54A 109.4 . . ? C22 C54 H54B 109.4 . . ? C43 C54 H54A 109.4 . . ? C43 C54 H54B 109.4 . . ? H54A C54 H54B 108.0 . . ? C33 C55 H55 120.8 . . ? C33 C55 C60 118.4(3) . . ? C60 C55 H55 120.8 . . ? N25 C56 C48 122.3(3) . . ? N25 C56 H56 118.9 . . ? C48 C56 H56 118.9 . . ? N31 C57 H57 118.8 . . ? N31 C57 C60 122.4(3) . . ? C60 C57 H57 118.8 . . ? N24 C58 C53 122.8(3) . . ? N24 C58 H58 118.6 . . ? C53 C58 H58 118.6 . . ? C46 C59 C53 118.8(3) . . ? C46 C59 H59 120.6 . . ? C53 C59 H59 120.6 . . ? C55 C60 H60 120.4 . . ? C57 C60 C55 119.3(3) . . ? C57 C60 H60 120.4 . . ? C39 C61 H61 120.0 . . ? C39 C61 C64 120.1(3) . . ? C64 C61 H61 120.0 . . ? C23 C62 C38 111.6(2) . . ? C23 C62 H62A 109.3 . . ? C23 C62 H62B 109.3 . . ? C38 C62 H62A 109.3 . . ? C38 C62 H62B 109.3 . . ? H62A C62 H62B 108.0 . . ? C37 C63 C48 119.4(3) . . ? C37 C63 H63 120.3 . . ? C48 C63 H63 120.3 . . ? C49 C64 H64 120.5 . . ? C61 C64 C49 119.0(3) . . ? C61 C64 H64 120.5 . . ? O50 C69 H69A 109.5 . . ? O50 C69 H69B 109.5 . . ? O50 C69 H69C 109.5 . . ? H69A C69 H69B 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C1 O65 H65 110(4) . . ? O65 C1 H1A 109.5 . . ? O65 C1 H1B 109.5 . . ? O65 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? _database_code_depnum_ccdc_archive 'CCDC 939538'