# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry # and the Centre National de la Recherche Scientifique 1999 # CCDC Number: 440/133 data_js9809 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H58 N4 O22' _chemical_formula_weight 1283.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.742(2) _cell_length_b 17.522(2) _cell_length_c 21.814(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.080(10) _cell_angle_gamma 90.00 _cell_volume 6015.9(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 18350 _cell_measurement_theta_min 1.52 _cell_measurement_theta_max 27.44 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2680 _exptl_absorpt_coefficient_mu 0.107 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.9883 _exptl_absorpt_correction_T_max 0.9894 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6883 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35854 _diffrn_reflns_av_R_equivalents 0.0529 _diffrn_reflns_av_sigmaI/netI 0.0671 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.48 _diffrn_reflns_theta_max 27.58 _reflns_number_total 13503 _reflns_number_gt 7535 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'TEXSAN 1.7.1 (MSC, 1996)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13503 _refine_ls_number_parameters 902 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1261 _refine_ls_R_factor_gt 0.0751 _refine_ls_wR_factor_ref 0.2145 _refine_ls_wR_factor_gt 0.1946 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_restrained_S_all 1.163 _refine_ls_shift/su_max 3.104 _refine_ls_shift/su_mean 0.086 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.57634(13) -0.33210(15) 0.11094(10) 0.0739(7) Uani 1 d . . . O2 O 0.55977(19) -0.07290(19) 0.10974(12) 0.1005(10) Uani 1 d . . . O3 O 0.89845(15) -0.31712(19) 0.26116(14) 0.0991(10) Uani 1 d . . . O4 O 0.89386(14) -0.05667(16) 0.25270(10) 0.0806(7) Uani 1 d . . . O5 O 0.33983(13) -0.30644(15) 0.36331(11) 0.0720(6) Uani 1 d . . . O6 O 0.32290(13) -0.04614(15) 0.35524(11) 0.0759(7) Uani 1 d . . . O7 O 0.66159(14) -0.27955(15) 0.51738(11) 0.0786(7) Uani 1 d . . . O8 O 0.64592(16) -0.02088(16) 0.50225(10) 0.0775(7) Uani 1 d . . . N1 N 0.55256(18) -0.2037(2) 0.09901(11) 0.0731(9) Uani 1 d . . . N2 N 0.91544(15) -0.18744(19) 0.26509(12) 0.0674(8) Uani 1 d . . . N3 N 0.31047(15) -0.17753(17) 0.35352(13) 0.0662(8) Uani 1 d . . . N4 N 0.66794(16) -0.14874(18) 0.52253(10) 0.0620(7) Uani 1 d . . . C1 C 0.2365(2) -0.1828(2) 0.3120(2) 0.0899(13) Uani 1 d . . . H1A H 0.1997 -0.1374 0.3170 0.108 Uiso 1 calc R . . H1B H 0.2028 -0.2288 0.3217 0.108 Uiso 1 calc R . . C2 C 0.2660(2) -0.1871(2) 0.2481(2) 0.0822(13) Uani 1 d . . . C3 C 0.3010(2) -0.1922(2) 0.2012(2) 0.0847(14) Uani 1 d . . . C4 C 0.3510(2) -0.2007(2) 0.15045(18) 0.0872(14) Uani 1 d . . . C5 C 0.4015(2) -0.2055(2) 0.11151(18) 0.0883(14) Uani 1 d . . . C6 C 0.4699(2) -0.2095(3) 0.06747(16) 0.0942(14) Uani 1 d . . . H6A H 0.4637 -0.1674 0.0374 0.113 Uiso 1 calc R . . H6B H 0.4664 -0.2584 0.0449 0.113 Uiso 1 calc R . . C7 C 0.5890(2) -0.1348(3) 0.11869(14) 0.0715(10) Uani 1 d . . . C8 C 0.66963(19) -0.1570(2) 0.15165(12) 0.0595(9) Uani 1 d . . . C9 C 0.7329(2) -0.1123(2) 0.17890(12) 0.0649(9) Uani 1 d . . . H9 H 0.7317 -0.0581 0.1775 0.078 Uiso 1 calc R . . C10 C 0.79741(18) -0.1519(2) 0.20809(12) 0.0577(8) Uani 1 d . . . C11 C 0.87310(19) -0.1234(2) 0.24374(13) 0.0619(9) Uani 1 d . . . C12 C 0.87578(19) -0.2545(3) 0.24798(16) 0.0702(11) Uani 1 d . . . C13 C 0.79941(17) -0.2298(2) 0.20979(13) 0.0617(9) Uani 1 d . . . C14 C 0.73822(18) -0.2754(2) 0.18219(14) 0.0621(9) Uani 1 d . . . H14 H 0.7406 -0.3296 0.1832 0.075 Uiso 1 calc R . . C15 C 0.67373(18) -0.2360(2) 0.15311(12) 0.0584(9) Uani 1 d . . . C16 C 0.5962(2) -0.2664(2) 0.11911(13) 0.0634(10) Uani 1 d . . . C17 C 0.98579(19) -0.1844(2) 0.31027(16) 0.0802(11) Uani 1 d . . . H17A H 1.0203 -0.2316 0.3077 0.096 Uiso 1 calc R . . H17B H 1.0230 -0.1403 0.3015 0.096 Uiso 1 calc R . . C18 C 0.95106(18) -0.1770(2) 0.37203(16) 0.0676(9) Uani 1 d . . . C19 C 0.91358(18) -0.17013(19) 0.41784(15) 0.0609(8) Uani 1 d . . . C20 C 0.86456(19) -0.16109(19) 0.46830(14) 0.0609(8) Uani 1 d . . . C21 C 0.8175(2) -0.1528(2) 0.50951(13) 0.0649(9) Uani 1 d . . . C22 C 0.7506(2) -0.1416(2) 0.55416(13) 0.0728(10) Uani 1 d . . . H22A H 0.7560 -0.0905 0.5731 0.087 Uiso 1 calc R . . H22B H 0.7556 -0.1804 0.5870 0.087 Uiso 1 calc R . . C23 C 0.6255(2) -0.0869(2) 0.49732(12) 0.0596(8) Uani 1 d . . . C24 C 0.55088(18) -0.11990(19) 0.46312(11) 0.0525(7) Uani 1 d . . . C25 C 0.48617(18) -0.08197(19) 0.43211(12) 0.0533(7) Uani 1 d . . . H25 H 0.4833 -0.0279 0.4293 0.064 Uiso 1 calc R . . C26 C 0.42634(17) -0.12929(18) 0.40571(12) 0.0504(7) Uani 1 d . . . C27 C 0.34793(18) -0.1093(2) 0.36886(14) 0.0616(9) Uani 1 d . . . C28 C 0.35682(18) -0.2406(2) 0.37333(14) 0.0596(8) Uani 1 d . . . C29 C 0.43089(17) -0.20811(18) 0.40853(12) 0.0522(7) Uani 1 d . . . C30 C 0.49612(17) -0.24573(19) 0.43987(12) 0.0529(7) Uani 1 d . . . H30 H 0.4995 -0.2998 0.4422 0.063 Uiso 1 calc R . . C31 C 0.55513(18) -0.19893(19) 0.46708(11) 0.0515(7) Uani 1 d . . . C32 C 0.63341(19) -0.2178(2) 0.50458(13) 0.0594(8) Uani 1 d . . . O9 O 0.17713(14) -0.15412(14) 0.47853(9) 0.0677(6) Uani 1 d . . . O10 O 0.11764(14) -0.02505(14) 0.40857(11) 0.0824(8) Uani 1 d . . . O11 O 0.15644(13) 0.08027(11) 0.31603(8) 0.0563(5) Uani 1 d . . . O12 O 0.34816(18) 0.0975(2) 0.22658(13) 0.1060(10) Uani 1 d . . . O13 O 0.48927(14) -0.05276(19) 0.26014(12) 0.0864(8) Uani 1 d . . . O16 O 0.72399(12) -0.48019(12) 0.54762(9) 0.0574(5) Uani 1 d . . . O17 O 0.54707(11) -0.46035(12) 0.57726(8) 0.0530(5) Uani 1 d . . . O18 O 0.40527(11) -0.36288(11) 0.57536(8) 0.0508(5) Uani 1 d . . . O19 O 0.45356(17) -0.13445(15) 0.59918(11) 0.0843(7) Uani 1 d . . . O20 O 0.48269(13) -0.25264(13) 0.62722(10) 0.0669(6) Uani 1 d . . . O21 O 0.1354(6) -0.2609(6) 0.4049(3) 0.060(2) Uani 0.50 d PD A 1 O21' O 0.1230(9) -0.2850(7) 0.3985(4) 0.101(4) Uani 0.50 d PD A 2 O22 O 0.12040(14) -0.36754(16) 0.46660(11) 0.0779(7) Uani 1 d . . . C33 C 0.23703(17) -0.20220(18) 0.50194(11) 0.0497(7) Uani 1 d . . . C34 C 0.22627(16) -0.27922(19) 0.48869(11) 0.0489(7) Uani 1 d . . . C35 C 0.28261(15) -0.33290(17) 0.51236(11) 0.0452(6) Uani 1 d . . . H35 H 0.2744 -0.3853 0.5029 0.054 Uiso 1 calc R . . C36 C 0.35103(15) -0.31123(16) 0.54981(10) 0.0401(6) Uani 1 d . . . C37 C 0.36367(15) -0.23365(16) 0.56205(10) 0.0420(6) Uani 1 d . . . C38 C 0.30636(17) -0.18011(17) 0.53762(11) 0.0480(7) Uani 1 d . . . H38 H 0.3153 -0.1274 0.5457 0.058 Uiso 1 calc R . . C39 C 0.1763(2) -0.0776(2) 0.50030(15) 0.0681(9) Uani 1 d . . . H39A H 0.2292 -0.0510 0.4889 0.082 Uiso 1 calc R . . H39B H 0.1720 -0.0769 0.5455 0.082 Uiso 1 calc R . . C40 C 0.1005(2) -0.0391(2) 0.47119(15) 0.0680(9) Uani 1 d . . . H40A H 0.0498 -0.0722 0.4746 0.082 Uiso 1 calc R . . H40B H 0.0890 0.0096 0.4924 0.082 Uiso 1 calc R . . C41 C 0.05653(19) 0.02150(18) 0.37989(15) 0.0635(9) Uani 1 d . . . H41A H 0.0526 0.0710 0.4015 0.076 Uiso 1 calc R . . H41B H 0.0001 -0.0035 0.3804 0.076 Uiso 1 calc R . . C42 C 0.08353(18) 0.03357(17) 0.31570(14) 0.0579(8) Uani 1 d . . . H42A H 0.0964 -0.0161 0.2964 0.069 Uiso 1 calc R . . H42B H 0.0372 0.0583 0.2917 0.069 Uiso 1 calc R . . C43 C 0.2027(2) 0.0741(2) 0.26183(14) 0.0648(9) Uani 1 d . . . H43A H 0.1739 0.1028 0.2283 0.078 Uiso 1 calc R . . H43B H 0.2073 0.0200 0.2494 0.078 Uiso 1 calc R . . C44 C 0.2946(2) 0.1088(2) 0.27556(15) 0.0731(10) Uani 1 d . . . H44A H 0.2894 0.1642 0.2837 0.088 Uiso 1 calc R . . H44B H 0.3194 0.0844 0.3127 0.088 Uiso 1 calc R . . C45 C 0.3841(3) 0.0247(3) 0.22641(19) 0.0884(12) Uani 1 d . . . H45A H 0.3931 0.0082 0.1836 0.106 Uiso 1 calc R . . H45B H 0.3447 -0.0120 0.2455 0.106 Uiso 1 calc R . . C46 C 0.4667(2) 0.0244(3) 0.26084(17) 0.0844(12) Uani 1 d . . . H46A H 0.5095 0.0562 0.2400 0.101 Uiso 1 calc R . . H46B H 0.4600 0.0432 0.3033 0.101 Uiso 1 calc R . . C47 C 0.56215(18) -0.0754(3) 0.28846(13) 0.0701(10) Uani 1 d . . . C48 C 0.57175(17) -0.1555(2) 0.28909(12) 0.0635(10) Uani 1 d . . . C49 C 0.51018(19) -0.2051(3) 0.26202(14) 0.0728(11) Uani 1 d . . . H49 H 0.4610 -0.1842 0.2426 0.087 Uiso 1 calc R . . C50 C 0.5208(2) -0.2820(3) 0.26361(15) 0.0808(12) Uani 1 d . . . H50 H 0.4794 -0.3145 0.2451 0.097 Uiso 1 calc R . . C51 C 0.5923(2) -0.3131(2) 0.29235(15) 0.0807(11) Uani 1 d . . . H51 H 0.5993 -0.3669 0.2938 0.097 Uiso 1 calc R . . C52 C 0.6523(2) -0.2671(3) 0.31847(13) 0.0753(11) Uani 1 d . . . C53 C 0.64404(18) -0.1867(2) 0.31822(11) 0.0629(10) Uani 1 d . . . C54 C 0.70466(19) -0.1363(3) 0.34600(12) 0.0673(10) Uani 1 d . . . H54 H 0.7537 -0.1565 0.3662 0.081 Uiso 1 calc R . . C55 C 0.69284(19) -0.0599(3) 0.34377(14) 0.0705(10) Uani 1 d . . . H55 H 0.7344 -0.0273 0.3620 0.085 Uiso 1 calc R . . C56 C 0.62087(19) -0.0276(2) 0.31532(14) 0.0691(10) Uani 1 d . . . H56 H 0.6130 0.0261 0.3147 0.083 Uiso 1 calc R . . O14 O 0.72593(17) -0.29232(16) 0.34650(11) 0.0901(8) Uani 1 d DU . . C57' C 0.7582(5) -0.3657(4) 0.3417(5) 0.109(4) Uani 0.40 d PDU B 2 H57C H 0.7639 -0.3758 0.2973 0.130 Uiso 0.40 calc PR B 2 H57D H 0.7132 -0.4004 0.3562 0.130 Uiso 0.40 calc PR B 2 C58' C 0.8426(5) -0.3929(5) 0.3729(3) 0.070(2) Uani 0.40 d PD B 2 H58C H 0.8531 -0.4468 0.3618 0.084 Uiso 0.40 calc PR B 2 H58D H 0.8903 -0.3620 0.3575 0.084 Uiso 0.40 calc PR B 2 O15' O 0.8399(4) -0.3865(4) 0.4345(3) 0.0758(17) Uani 0.40 d PD B 2 C59' C 0.7841(7) -0.4353(9) 0.4612(4) 0.103(5) Uani 0.40 d PD B 2 H59C H 0.7924 -0.4873 0.4446 0.124 Uiso 0.40 calc PR B 2 H59D H 0.7253 -0.4191 0.4509 0.124 Uiso 0.40 calc PR B 2 C60' C 0.7968(2) -0.4369(2) 0.53226(15) 0.0732(9) Uani 0.40 d PD B 2 H60C H 0.8502 -0.4628 0.5448 0.088 Uiso 0.40 calc PR B 2 H60D H 0.7954 -0.3850 0.5502 0.088 Uiso 0.40 calc PR B 2 C57 C 0.7178(4) -0.3656(3) 0.3607(3) 0.090(2) Uani 0.60 d PDU B 1 H57A H 0.7262 -0.3989 0.3247 0.108 Uiso 0.60 calc PR B 1 H57B H 0.6617 -0.3765 0.3786 0.108 Uiso 0.60 calc PR B 1 C58 C 0.7889(4) -0.3743(4) 0.4076(3) 0.0724(16) Uani 0.60 d P B 1 H58A H 0.8444 -0.3621 0.3893 0.087 Uiso 0.60 calc PR B 1 H58B H 0.7800 -0.3401 0.4430 0.087 Uiso 0.60 calc PR B 1 O15 O 0.7862(3) -0.4502(2) 0.42557(17) 0.0570(10) Uani 0.60 d P B 1 C59 C 0.8375(4) -0.4680(4) 0.4755(3) 0.0667(15) Uani 0.60 d P B 1 H59A H 0.8945 -0.4452 0.4706 0.080 Uiso 0.60 calc PR B 1 H59B H 0.8441 -0.5240 0.4789 0.080 Uiso 0.60 calc PR B 1 C60 C 0.7968(2) -0.4369(2) 0.53226(15) 0.0732(9) Uani 0.60 d P B 1 H60A H 0.8383 -0.4381 0.5669 0.088 Uiso 0.60 calc PR B 1 H60B H 0.7801 -0.3831 0.5252 0.088 Uiso 0.60 calc PR B 1 C61 C 0.69263(19) -0.4573(2) 0.60489(13) 0.0707(10) Uani 1 d . . . H61A H 0.6862 -0.4011 0.6057 0.085 Uiso 1 calc R . . H61B H 0.7336 -0.4720 0.6378 0.085 Uiso 1 calc R . . C62 C 0.60982(19) -0.4936(2) 0.61593(12) 0.0655(9) Uani 1 d . . . H62A H 0.6135 -0.5491 0.6076 0.079 Uiso 1 calc R . . H62B H 0.5943 -0.4867 0.6593 0.079 Uiso 1 calc R . . C63 C 0.46421(18) -0.48570(19) 0.59103(15) 0.0624(8) Uani 1 d . . . H63A H 0.4540 -0.4793 0.6354 0.075 Uiso 1 calc R . . H63B H 0.4583 -0.5405 0.5808 0.075 Uiso 1 calc R . . C64 C 0.40088(17) -0.44024(17) 0.55463(14) 0.0553(7) Uani 1 d . . . H64A H 0.4139 -0.4429 0.5105 0.066 Uiso 1 calc R . . H64B H 0.3430 -0.4608 0.5605 0.066 Uiso 1 calc R . . C65 C 0.43674(18) -0.20129(19) 0.59767(12) 0.0503(7) Uani 1 d . . . C66 C 0.55689(19) -0.2249(2) 0.65973(15) 0.0732(10) Uani 1 d . . . H66A H 0.5864 -0.2677 0.6797 0.088 Uiso 1 calc R . . H66B H 0.5397 -0.1879 0.6909 0.088 Uiso 1 calc R . . H66C H 0.5950 -0.2001 0.6308 0.088 Uiso 1 calc R . . C67 C 0.15490(19) -0.3029(2) 0.44757(13) 0.0641(9) Uani 1 d D . . C68 C 0.0595(7) -0.3873(7) 0.4200(7) 0.064(3) Uani 0.50 d P C 1 H68A H 0.0310 -0.4349 0.4312 0.077 Uiso 0.50 calc PR C 1 H68B H 0.0883 -0.3942 0.3809 0.077 Uiso 0.50 calc PR C 1 H68C H 0.0173 -0.3464 0.4158 0.077 Uiso 0.50 calc PR C 1 C68' C 0.0462(11) -0.4132(11) 0.4374(9) 0.120(7) Uani 0.50 d P C 2 H68D H 0.0345 -0.4581 0.4626 0.144 Uiso 0.50 calc PR C 2 H68E H 0.0615 -0.4295 0.3961 0.144 Uiso 0.50 calc PR C 2 H68F H -0.0046 -0.3808 0.4349 0.144 Uiso 0.50 calc PR C 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 O1 0.0532(13) 0.1020(19) 0.0668(14) -0.0374(13) 0.0109(10) -0.0345(13) O2 0.104(2) 0.114(2) 0.0820(18) 0.0417(17) -0.0277(15) -0.0449(18) O3 0.0413(14) 0.112(2) 0.143(3) -0.062(2) -0.0029(14) 0.0144(14) O4 0.0612(14) 0.110(2) 0.0702(15) -0.0219(13) 0.0035(11) -0.0445(14) O5 0.0470(13) 0.0861(19) 0.0832(16) 0.0163(13) 0.0093(11) -0.0025(12) O6 0.0493(13) 0.0966(18) 0.0821(16) 0.0381(13) 0.0083(11) 0.0238(12) O7 0.0603(14) 0.0950(19) 0.0802(16) 0.0333(13) -0.0032(12) 0.0181(13) O8 0.0821(17) 0.0892(19) 0.0604(14) -0.0230(13) -0.0184(12) 0.0213(14) N1 0.0643(17) 0.112(3) 0.0428(14) 0.0156(15) -0.0134(12) -0.0427(18) N2 0.0368(14) 0.104(2) 0.0617(16) -0.0327(15) 0.0063(12) -0.0094(14) N3 0.0322(13) 0.089(2) 0.0773(18) 0.0311(15) 0.0025(12) 0.0009(13) N4 0.0570(16) 0.094(2) 0.0350(12) 0.0037(13) -0.0038(11) 0.0181(15) C1 0.0300(16) 0.118(3) 0.121(3) 0.053(3) -0.0132(18) -0.0043(17) C2 0.0380(18) 0.101(3) 0.106(3) 0.063(2) -0.0304(19) -0.0282(17) C3 0.0445(19) 0.112(3) 0.097(3) 0.067(2) -0.037(2) -0.0428(19) C4 0.056(2) 0.124(3) 0.079(2) 0.063(2) -0.042(2) -0.052(2) C5 0.065(2) 0.128(3) 0.071(2) 0.050(2) -0.040(2) -0.054(2) C6 0.084(3) 0.143(4) 0.0550(19) 0.031(2) -0.0280(19) -0.057(3) C7 0.076(2) 0.094(3) 0.0443(17) 0.0183(18) -0.0026(16) -0.044(2) C8 0.0510(17) 0.094(3) 0.0336(14) -0.0041(14) 0.0082(12) -0.0354(16) C9 0.063(2) 0.094(2) 0.0384(15) -0.0070(15) 0.0143(14) -0.0415(18) C10 0.0397(16) 0.095(3) 0.0392(14) -0.0201(15) 0.0105(12) -0.0244(16) C11 0.0400(16) 0.103(3) 0.0435(16) -0.0210(17) 0.0113(13) -0.0329(18) C12 0.0296(16) 0.105(3) 0.077(2) -0.050(2) 0.0136(14) -0.0099(18) C13 0.0381(16) 0.096(3) 0.0517(16) -0.0381(16) 0.0174(13) -0.0166(16) C14 0.0359(15) 0.092(2) 0.0585(18) -0.0356(17) 0.0140(14) -0.0130(16) C15 0.0418(16) 0.097(3) 0.0373(14) -0.0237(15) 0.0168(12) -0.0320(16) C16 0.0492(18) 0.104(3) 0.0378(15) -0.0179(17) 0.0121(13) -0.0385(19) C17 0.0303(16) 0.130(3) 0.080(2) -0.043(2) 0.0004(15) -0.0109(17) C18 0.0309(15) 0.103(3) 0.069(2) -0.0322(19) -0.0108(14) 0.0024(15) C19 0.0390(16) 0.084(2) 0.0589(18) -0.0177(16) -0.0179(14) 0.0107(15) C20 0.0495(18) 0.086(2) 0.0466(16) -0.0097(15) -0.0205(14) 0.0174(16) C21 0.062(2) 0.089(3) 0.0429(16) -0.0073(16) -0.0188(15) 0.0227(17) C22 0.067(2) 0.113(3) 0.0376(15) 0.0014(17) -0.0139(14) 0.019(2) C23 0.062(2) 0.082(3) 0.0345(14) -0.0078(15) 0.0007(13) 0.0210(18) C24 0.0513(16) 0.080(2) 0.0265(12) 0.0022(13) 0.0081(11) 0.0190(15) C25 0.0541(18) 0.071(2) 0.0350(13) 0.0050(13) 0.0090(12) 0.0201(15) C26 0.0411(15) 0.074(2) 0.0369(14) 0.0124(13) 0.0120(12) 0.0148(14) C27 0.0387(16) 0.093(3) 0.0540(17) 0.0285(17) 0.0140(13) 0.0201(18) C28 0.0332(15) 0.086(3) 0.0600(18) 0.0239(17) 0.0137(13) 0.0080(16) C29 0.0395(15) 0.077(2) 0.0406(14) 0.0170(13) 0.0137(12) 0.0134(14) C30 0.0453(16) 0.068(2) 0.0454(15) 0.0175(14) 0.0136(13) 0.0132(14) C31 0.0446(16) 0.078(2) 0.0319(13) 0.0126(13) 0.0101(11) 0.0202(15) C32 0.0516(18) 0.088(3) 0.0388(15) 0.0182(16) 0.0070(13) 0.0189(18) O9 0.0649(14) 0.0874(17) 0.0509(12) 0.0185(11) 0.0000(10) 0.0354(12) O10 0.0605(14) 0.1005(18) 0.0874(16) 0.0576(14) 0.0337(12) 0.0426(13) O11 0.0586(13) 0.0622(13) 0.0482(11) 0.0061(9) -0.0003(9) -0.0124(10) O12 0.0743(18) 0.159(3) 0.0845(19) 0.0483(19) -0.0056(15) -0.0397(19) O13 0.0398(13) 0.130(2) 0.0892(17) -0.0423(16) -0.0098(12) 0.0006(14) O16 0.0471(11) 0.0723(14) 0.0531(11) -0.0097(10) 0.0062(9) 0.0062(10) O17 0.0349(10) 0.0783(14) 0.0458(10) 0.0039(9) -0.0011(8) 0.0179(9) O18 0.0380(10) 0.0670(13) 0.0470(10) -0.0057(9) -0.0085(8) 0.0191(9) O19 0.106(2) 0.0769(18) 0.0691(15) 0.0077(13) -0.0243(14) -0.0209(15) O20 0.0437(12) 0.0831(16) 0.0729(14) 0.0023(12) -0.0225(10) -0.0066(11) O21 0.027(3) 0.126(6) 0.025(3) -0.003(3) -0.019(2) 0.008(4) O21' 0.058(5) 0.187(10) 0.058(4) -0.015(5) -0.030(3) -0.008(5) O22 0.0480(13) 0.104(2) 0.0804(16) -0.0301(15) -0.0202(12) 0.0111(13) C33 0.0430(15) 0.074(2) 0.0325(13) 0.0100(13) 0.0061(11) 0.0203(14) C34 0.0331(13) 0.085(2) 0.0290(12) -0.0007(13) 0.0030(10) 0.0179(14) C35 0.0324(13) 0.0665(19) 0.0368(13) -0.0057(12) 0.0018(10) 0.0110(12) C36 0.0299(12) 0.0617(18) 0.0289(11) 0.0004(11) 0.0033(9) 0.0125(12) C37 0.0373(14) 0.0616(19) 0.0273(11) 0.0047(11) 0.0061(10) 0.0046(12) C38 0.0505(16) 0.0605(18) 0.0333(13) 0.0116(12) 0.0088(12) 0.0095(13) C39 0.0558(19) 0.075(2) 0.074(2) 0.0329(18) 0.0218(16) 0.0174(16) C40 0.0509(18) 0.078(2) 0.076(2) 0.0321(17) 0.0237(16) 0.0213(16) C41 0.0476(17) 0.060(2) 0.084(2) 0.0230(16) 0.0105(16) 0.0160(14) C42 0.0459(17) 0.0515(18) 0.076(2) 0.0138(15) -0.0055(14) -0.0044(14) C43 0.064(2) 0.079(2) 0.0511(17) 0.0044(15) -0.0045(15) -0.0140(17) C44 0.101(3) 0.063(2) 0.0551(19) 0.0089(16) 0.0015(19) -0.0158(19) C45 0.071(3) 0.113(4) 0.080(3) 0.019(2) -0.007(2) -0.005(2) C46 0.0422(19) 0.138(4) 0.072(2) 0.008(2) -0.0075(16) -0.030(2) C47 0.0295(15) 0.134(4) 0.0466(17) -0.0275(19) 0.0037(12) -0.0113(17) C48 0.0323(15) 0.123(3) 0.0355(14) -0.0247(16) 0.0103(11) -0.0216(17) C49 0.0333(16) 0.141(4) 0.0450(17) -0.025(2) 0.0084(12) -0.0242(19) C50 0.053(2) 0.140(4) 0.0497(18) -0.024(2) 0.0126(16) -0.046(2) C51 0.074(2) 0.117(3) 0.0509(18) 0.0098(19) 0.0006(17) -0.046(2) C52 0.061(2) 0.126(3) 0.0388(16) 0.0183(18) -0.0011(14) -0.039(2) C53 0.0360(15) 0.126(3) 0.0273(13) -0.0032(16) 0.0054(11) -0.0269(17) C54 0.0405(16) 0.128(3) 0.0329(14) -0.0011(17) -0.0023(12) -0.0257(19) C55 0.0423(18) 0.123(3) 0.0467(17) -0.0134(19) 0.0033(13) -0.0293(19) C56 0.0394(17) 0.113(3) 0.0552(18) -0.0206(18) 0.0052(14) -0.0159(17) O14 0.0904(19) 0.108(2) 0.0706(15) 0.0394(15) -0.0286(14) -0.0387(16) C57' 0.057(6) 0.139(7) 0.130(8) 0.112(7) -0.018(5) -0.051(5) C58' 0.040(4) 0.103(7) 0.066(5) 0.039(5) 0.003(4) 0.032(4) O15' 0.040(3) 0.101(5) 0.086(4) 0.022(3) -0.005(3) 0.005(3) C59' 0.049(6) 0.190(15) 0.071(7) 0.008(9) 0.014(6) -0.021(7) C60' 0.072(2) 0.085(3) 0.063(2) -0.0060(18) 0.0068(17) -0.0079(19) C57 0.057(4) 0.128(6) 0.085(4) 0.048(4) -0.012(3) -0.054(4) C58 0.048(3) 0.089(5) 0.080(4) 0.015(3) -0.007(3) 0.001(3) O15 0.064(2) 0.057(2) 0.050(2) 0.0083(19) 0.001(2) 0.0019(18) C59 0.037(3) 0.094(4) 0.070(4) 0.000(3) 0.005(3) 0.007(3) C60 0.072(2) 0.085(3) 0.063(2) -0.0060(18) 0.0068(17) -0.0079(19) C61 0.0440(17) 0.126(3) 0.0419(16) -0.0088(17) -0.0109(13) 0.0207(18) C62 0.0474(17) 0.112(3) 0.0372(14) 0.0094(16) -0.0027(12) 0.0268(17) C63 0.0406(16) 0.072(2) 0.075(2) 0.0078(16) 0.0095(14) 0.0186(14) C64 0.0362(15) 0.063(2) 0.0672(19) -0.0041(15) 0.0014(13) 0.0148(13) C65 0.0512(17) 0.066(2) 0.0336(13) 0.0050(13) 0.0038(12) -0.0070(15) C66 0.0412(17) 0.111(3) 0.067(2) -0.0071(19) -0.0131(15) -0.0147(17) C67 0.0338(15) 0.111(3) 0.0471(17) -0.0201(19) 0.0001(13) 0.0224(18) C68 0.036(5) 0.080(7) 0.076(6) -0.023(5) -0.008(4) -0.007(5) C68' 0.077(7) 0.162(16) 0.122(14) -0.043(9) -0.007(8) -0.055(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 O1 C16 1.205(4) . ? O2 C7 1.192(5) . ? O3 C12 1.188(5) . ? O4 C11 1.229(4) . ? O5 C28 1.202(4) . ? O6 C27 1.210(4) . ? O7 C32 1.201(4) . ? O8 C23 1.206(4) . ? N1 C16 1.365(5) . ? N1 C7 1.400(4) . ? N1 C6 1.464(4) . ? N2 C12 1.378(4) . ? N2 C11 1.381(5) . ? N2 C17 1.470(4) . ? N3 C27 1.372(5) . ? N3 C28 1.389(4) . ? N3 C1 1.465(4) . ? N4 C32 1.380(4) . ? N4 C23 1.381(4) . ? N4 C22 1.466(4) . ? C1 C2 1.480(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.174(6) . ? C3 C4 1.378(7) . ? C4 C5 1.177(6) . ? C5 C6 1.458(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.499(5) . ? C8 C15 1.386(5) . ? C8 C9 1.392(4) . ? C9 C10 1.376(5) . ? C9 H9 0.9500 . ? C10 C13 1.365(5) . ? C10 C11 1.496(4) . ? C12 C13 1.513(5) . ? C13 C14 1.381(4) . ? C14 C15 1.373(5) . ? C14 H14 0.9500 . ? C15 C16 1.513(4) . ? C17 C18 1.469(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.176(4) . ? C19 C20 1.365(5) . ? C20 C21 1.184(4) . ? C21 C22 1.462(5) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.495(4) . ? C24 C25 1.382(4) . ? C24 C31 1.389(4) . ? C25 C26 1.373(4) . ? C25 H25 0.9500 . ? C26 C29 1.384(4) . ? C26 C27 1.502(4) . ? C28 C29 1.497(4) . ? C29 C30 1.389(4) . ? C30 C31 1.366(4) . ? C30 H30 0.9500 . ? C31 C32 1.503(4) . ? O9 C33 1.357(3) . ? O9 C39 1.422(4) . ? O10 C41 1.400(3) . ? O10 C40 1.419(4) . ? O11 C43 1.404(3) . ? O11 C42 1.410(3) . ? O12 C44 1.388(4) . ? O12 C45 1.396(5) . ? O13 C47 1.352(4) . ? O13 C46 1.399(5) . ? O16 C61 1.410(3) . ? O16 C60' 1.420(4) . ? O17 C62 1.413(3) . ? O17 C63 1.416(3) . ? O18 C36 1.357(3) . ? O18 C64 1.430(3) . ? O19 C65 1.201(4) . ? O20 C65 1.316(4) . ? O20 C66 1.440(3) . ? O21 C67 1.221(5) . ? O21' C67 1.215(5) . ? O22 C67 1.326(4) . ? O22 C68 1.427(15) . ? O22 C68' 1.543(17) . ? C33 C38 1.384(4) . ? C33 C34 1.390(4) . ? C34 C35 1.386(4) . ? C34 C67 1.484(4) . ? C35 C36 1.392(3) . ? C35 H35 0.9500 . ? C36 C37 1.399(4) . ? C37 C38 1.400(4) . ? C37 C65 1.488(4) . ? C38 H38 0.9500 . ? C39 C40 1.502(4) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.486(4) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.592(5) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.490(5) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C56 1.370(4) . ? C47 C48 1.413(5) . ? C48 C53 1.404(5) . ? C48 C49 1.422(4) . ? C49 C50 1.357(5) . ? C49 H49 0.9500 . ? C50 C51 1.390(5) . ? C50 H50 0.9500 . ? C51 C52 1.359(5) . ? C51 H51 0.9500 . ? C52 O14 1.373(4) . ? C52 C53 1.414(5) . ? C53 C54 1.427(4) . ? C54 C55 1.351(5) . ? C54 H54 0.9500 . ? C55 C56 1.401(5) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? O14 C57 1.327(4) . ? O14 C57' 1.387(5) . ? C57' C58' 1.557(8) . ? C57' H57C 0.9900 . ? C57' H57D 0.9900 . ? C58' O15' 1.349(5) . ? C58' H58C 0.9900 . ? C58' H58D 0.9900 . ? O15' C59' 1.363(13) . ? C59' C60' 1.560(8) . ? C59' H59C 0.9900 . ? C59' H59D 0.9900 . ? C60' H60C 0.9900 . ? C60' H60D 0.9900 . ? C57 C58 1.510(9) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 O15 1.387(7) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? O15 C59 1.379(7) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C61 C62 1.474(5) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.493(4) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C68' H68D 0.9800 . ? C68' H68E 0.9800 . ? C68' H68F 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 C16 N1 C7 113.3(3) . . ? C16 N1 C6 122.2(3) . . ? C7 N1 C6 124.0(4) . . ? C12 N2 C11 112.8(3) . . ? C12 N2 C17 123.0(3) . . ? C11 N2 C17 123.4(3) . . ? C27 N3 C28 113.4(3) . . ? C27 N3 C1 122.6(3) . . ? C28 N3 C1 123.3(3) . . ? C32 N4 C23 112.9(3) . . ? C32 N4 C22 123.3(3) . . ? C23 N4 C22 122.6(3) . . ? N3 C1 C2 109.0(3) . . ? N3 C1 H1A 109.9 . . ? C2 C1 H1A 109.9 . . ? N3 C1 H1B 109.9 . . ? C2 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? C3 C2 C1 170.2(3) . . ? C2 C3 C4 172.8(3) . . ? C5 C4 C3 172.2(3) . . ? C4 C5 C6 174.8(3) . . ? C5 C6 N1 110.3(3) . . ? C5 C6 H6A 109.6 . . ? N1 C6 H6A 109.6 . . ? C5 C6 H6B 109.6 . . ? N1 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? O2 C7 N1 125.4(4) . . ? O2 C7 C8 129.4(3) . . ? N1 C7 C8 105.2(3) . . ? C15 C8 C9 121.3(3) . . ? C15 C8 C7 108.0(3) . . ? C9 C8 C7 130.7(4) . . ? C10 C9 C8 115.4(3) . . ? C10 C9 H9 122.3 . . ? C8 C9 H9 122.3 . . ? C13 C10 C9 122.2(3) . . ? C13 C10 C11 107.5(3) . . ? C9 C10 C11 130.2(3) . . ? O4 C11 N2 126.4(3) . . ? O4 C11 C10 127.4(4) . . ? N2 C11 C10 106.2(3) . . ? O3 C12 N2 126.1(3) . . ? O3 C12 C13 129.0(3) . . ? N2 C12 C13 104.9(4) . . ? C10 C13 C14 123.5(3) . . ? C10 C13 C12 108.6(3) . . ? C14 C13 C12 127.9(4) . . ? C15 C14 C13 114.4(3) . . ? C15 C14 H14 122.8 . . ? C13 C14 H14 122.8 . . ? C14 C15 C8 123.1(3) . . ? C14 C15 C16 129.2(3) . . ? C8 C15 C16 107.7(3) . . ? O1 C16 N1 126.4(3) . . ? O1 C16 C15 127.9(4) . . ? N1 C16 C15 105.7(3) . . ? C18 C17 N2 109.2(2) . . ? C18 C17 H17A 109.8 . . ? N2 C17 H17A 109.8 . . ? C18 C17 H17B 109.8 . . ? N2 C17 H17B 109.8 . . ? H17A C17 H17B 108.3 . . ? C19 C18 C17 171.7(3) . . ? C18 C19 C20 175.6(3) . . ? C21 C20 C19 175.7(3) . . ? C20 C21 C22 172.4(3) . . ? C21 C22 N4 108.6(2) . . ? C21 C22 H22A 109.9 . . ? N4 C22 H22A 110.0 . . ? C21 C22 H22B 110.0 . . ? N4 C22 H22B 110.0 . . ? H22A C22 H22B 108.3 . . ? O8 C23 N4 126.2(3) . . ? O8 C23 C24 128.4(3) . . ? N4 C23 C24 105.4(3) . . ? C25 C24 C31 123.0(3) . . ? C25 C24 C23 128.5(3) . . ? C31 C24 C23 108.5(3) . . ? C26 C25 C24 114.1(3) . . ? C26 C25 H25 123.0 . . ? C24 C25 H25 123.0 . . ? C25 C26 C29 123.3(3) . . ? C25 C26 C27 129.3(3) . . ? C29 C26 C27 107.3(3) . . ? O6 C27 N3 126.9(3) . . ? O6 C27 C26 127.3(4) . . ? N3 C27 C26 105.8(3) . . ? O5 C28 N3 126.4(3) . . ? O5 C28 C29 128.8(3) . . ? N3 C28 C29 104.8(3) . . ? C26 C29 C30 122.2(3) . . ? C26 C29 C28 108.5(3) . . ? C30 C29 C28 129.3(3) . . ? C31 C30 C29 114.8(3) . . ? C31 C30 H30 122.6 . . ? C29 C30 H30 122.6 . . ? C30 C31 C24 122.7(3) . . ? C30 C31 C32 130.4(3) . . ? C24 C31 C32 106.9(3) . . ? O7 C32 N4 125.6(3) . . ? O7 C32 C31 128.3(4) . . ? N4 C32 C31 106.0(3) . . ? C33 O9 C39 118.0(3) . . ? C41 O10 C40 112.9(2) . . ? C43 O11 C42 112.7(2) . . ? C44 O12 C45 112.7(3) . . ? C47 O13 C46 119.5(3) . . ? C61 O16 C60' 110.8(2) . . ? C62 O17 C63 112.4(2) . . ? C36 O18 C64 118.4(2) . . ? C65 O20 C66 116.3(3) . . ? C67 O22 C68 105.0(5) . . ? C67 O22 C68' 128.7(7) . . ? C68 O22 C68' 24.1(8) . . ? O9 C33 C38 125.0(3) . . ? O9 C33 C34 116.3(3) . . ? C38 C33 C34 118.7(2) . . ? C35 C34 C33 120.5(2) . . ? C35 C34 C67 120.5(3) . . ? C33 C34 C67 119.0(3) . . ? C34 C35 C36 121.1(3) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? O18 C36 C35 122.2(3) . . ? O18 C36 C37 118.9(2) . . ? C35 C36 C37 118.9(2) . . ? C36 C37 C38 119.4(2) . . ? C36 C37 C65 125.1(2) . . ? C38 C37 C65 115.4(3) . . ? C33 C38 C37 121.5(3) . . ? C33 C38 H38 119.2 . . ? C37 C38 H38 119.3 . . ? O9 C39 C40 107.1(3) . . ? O9 C39 H39A 110.3 . . ? C40 C39 H39A 110.3 . . ? O9 C39 H39B 110.3 . . ? C40 C39 H39B 110.3 . . ? H39A C39 H39B 108.5 . . ? O10 C40 C39 108.7(2) . . ? O10 C40 H40A 109.9 . . ? C39 C40 H40A 109.9 . . ? O10 C40 H40B 110.0 . . ? C39 C40 H40B 109.9 . . ? H40A C40 H40B 108.3 . . ? O10 C41 C42 107.3(2) . . ? O10 C41 H41A 110.2 . . ? C42 C41 H41A 110.2 . . ? O10 C41 H41B 110.3 . . ? C42 C41 H41B 110.3 . . ? H41A C41 H41B 108.5 . . ? O11 C42 C41 109.0(3) . . ? O11 C42 H42A 109.9 . . ? C41 C42 H42A 109.9 . . ? O11 C42 H42B 109.9 . . ? C41 C42 H42B 109.9 . . ? H42A C42 H42B 108.3 . . ? O11 C43 C44 107.2(2) . . ? O11 C43 H43A 110.3 . . ? C44 C43 H43A 110.3 . . ? O11 C43 H43B 110.3 . . ? C44 C43 H43B 110.3 . . ? H43A C43 H43B 108.5 . . ? O12 C44 C43 111.3(3) . . ? O12 C44 H44A 109.4 . . ? C43 C44 H44A 109.4 . . ? O12 C44 H44B 109.4 . . ? C43 C44 H44B 109.4 . . ? H44A C44 H44B 108.0 . . ? O12 C45 C46 110.5(4) . . ? O12 C45 H45A 109.5 . . ? C46 C45 H45A 109.6 . . ? O12 C45 H45B 109.5 . . ? C46 C45 H45B 109.5 . . ? H45A C45 H45B 108.1 . . ? O13 C46 C45 102.5(3) . . ? O13 C46 H46A 111.3 . . ? C45 C46 H46A 111.3 . . ? O13 C46 H46B 111.3 . . ? C45 C46 H46B 111.3 . . ? H46A C46 H46B 109.2 . . ? O13 C47 C56 125.2(4) . . ? O13 C47 C48 112.7(3) . . ? C56 C47 C48 122.1(3) . . ? C53 C48 C47 118.5(3) . . ? C53 C48 C49 119.4(4) . . ? C47 C48 C49 122.1(3) . . ? C50 C49 C48 120.9(4) . . ? C50 C49 H49 119.6 . . ? C48 C49 H49 119.5 . . ? C49 C50 C51 120.0(3) . . ? C49 C50 H50 120.0 . . ? C51 C50 H50 120.0 . . ? C52 C51 C50 120.4(4) . . ? C52 C51 H51 119.8 . . ? C50 C51 H51 119.8 . . ? C51 C52 O14 124.7(4) . . ? C51 C52 C53 121.7(4) . . ? O14 C52 C53 113.5(3) . . ? C48 C53 C52 117.6(3) . . ? C48 C53 C54 118.7(4) . . ? C52 C53 C54 123.7(3) . . ? C55 C54 C53 120.5(3) . . ? C55 C54 H54 119.8 . . ? C53 C54 H54 119.8 . . ? C54 C55 C56 121.7(3) . . ? C54 C55 H55 119.2 . . ? C56 C55 H55 119.2 . . ? C47 C56 C55 118.5(4) . . ? C47 C56 H56 120.8 . . ? C55 C56 H56 120.8 . . ? C57 O14 C52 109.3(4) . . ? C57 O14 C57' 32.7(4) . . ? C52 O14 C57' 124.9(5) . . ? O14 C57' C58' 124.1(7) . . ? O14 C57' H57C 106.2 . . ? C58' C57' H57C 106.2 . . ? O14 C57' H57D 106.3 . . ? C58' C57' H57D 106.4 . . ? H57C C57' H57D 106.5 . . ? O15' C58' C57' 111.6(6) . . ? O15' C58' H58C 109.2 . . ? C57' C58' H58C 109.6 . . ? O15' C58' H58D 109.3 . . ? C57' C58' H58D 109.1 . . ? H58C C58' H58D 107.9 . . ? C58' O15' C59' 113.9(7) . . ? O15' C59' C60' 111.4(8) . . ? O15' C59' H59C 109.3 . . ? C60' C59' H59C 109.4 . . ? O15' C59' H59D 109.3 . . ? C60' C59' H59D 109.3 . . ? H59C C59' H59D 108.0 . . ? O16 C60' C59' 99.0(5) . . ? O16 C60' H60C 112.0 . . ? C59' C60' H60C 112.0 . . ? O16 C60' H60D 112.0 . . ? C59' C60' H60D 112.0 . . ? H60C C60' H60D 109.7 . . ? O14 C57 C58 100.5(5) . . ? O14 C57 H57A 112.1 . . ? C58 C57 H57A 112.0 . . ? O14 C57 H57B 111.3 . . ? C58 C57 H57B 111.3 . . ? H57A C57 H57B 109.4 . . ? O15 C58 C57 105.2(5) . . ? O15 C58 H58A 110.7 . . ? C57 C58 H58A 110.4 . . ? O15 C58 H58B 110.6 . . ? C57 C58 H58B 111.1 . . ? H58A C58 H58B 108.8 . . ? C59 O15 C58 114.8(5) . . ? O15 C59 H59A 110.1 . . ? O15 C59 H59B 110.0 . . ? H59A C59 H59B 108.4 . . ? O16 C61 C62 110.3(3) . . ? O16 C61 H61A 109.6 . . ? C62 C61 H61A 109.6 . . ? O16 C61 H61B 109.6 . . ? C62 C61 H61B 109.6 . . ? H61A C61 H61B 108.1 . . ? O17 C62 C61 109.6(3) . . ? O17 C62 H62A 109.8 . . ? C61 C62 H62A 109.8 . . ? O17 C62 H62B 109.8 . . ? C61 C62 H62B 109.8 . . ? H62A C62 H62B 108.2 . . ? O17 C63 C64 109.2(2) . . ? O17 C63 H63A 109.8 . . ? C64 C63 H63A 109.8 . . ? O17 C63 H63B 109.9 . . ? C64 C63 H63B 109.9 . . ? H63A C63 H63B 108.3 . . ? O18 C64 C63 108.0(2) . . ? O18 C64 H64A 110.1 . . ? C63 C64 H64A 110.1 . . ? O18 C64 H64B 110.1 . . ? C63 C64 H64B 110.1 . . ? H64A C64 H64B 108.4 . . ? O19 C65 O20 122.3(3) . . ? O19 C65 C37 123.6(3) . . ? O20 C65 C37 114.1(3) . . ? O20 C66 H66A 109.5 . . ? O20 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? O20 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? O21' C67 O21 23.0(9) . . ? O21' C67 O22 109.3(6) . . ? O21 C67 O22 130.9(6) . . ? O21' C67 C34 139.1(7) . . ? O21 C67 C34 117.9(6) . . ? O22 C67 C34 111.1(3) . . ? O22 C68 H68A 109.4 . . ? O22 C68 H68B 109.4 . . ? H68A C68 H68B 109.5 . . ? O22 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? O22 C68' H68D 109.3 . . ? O22 C68' H68E 109.7 . . ? H68D C68' H68E 109.5 . . ? O22 C68' H68F 109.4 . . ? H68D C68' H68F 109.5 . . ? H68E C68' H68F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C27 N3 C1 C2 86.9(4) . . . . ? C28 N3 C1 C2 -82.8(4) . . . . ? N3 C1 C2 C3 12(3) . . . . ? C1 C2 C3 C4 6(6) . . . . ? C2 C3 C4 C5 -29(6) . . . . ? C3 C4 C5 C6 2(8) . . . . ? C4 C5 C6 N1 9(5) . . . . ? C16 N1 C6 C5 91.1(4) . . . . ? C7 N1 C6 C5 -80.0(4) . . . . ? C16 N1 C7 O2 -175.7(3) . . . . ? C6 N1 C7 O2 -3.9(5) . . . . ? C16 N1 C7 C8 4.6(3) . . . . ? C6 N1 C7 C8 176.5(3) . . . . ? O2 C7 C8 C15 176.6(3) . . . . ? N1 C7 C8 C15 -3.7(3) . . . . ? O2 C7 C8 C9 -2.1(6) . . . . ? N1 C7 C8 C9 177.5(3) . . . . ? C15 C8 C9 C10 -1.5(4) . . . . ? C7 C8 C9 C10 177.1(3) . . . . ? C8 C9 C10 C13 0.4(4) . . . . ? C8 C9 C10 C11 -177.5(2) . . . . ? C12 N2 C11 O4 179.2(3) . . . . ? C17 N2 C11 O4 9.8(4) . . . . ? C12 N2 C11 C10 -0.5(3) . . . . ? C17 N2 C11 C10 -170.0(2) . . . . ? C13 C10 C11 O4 179.7(3) . . . . ? C9 C10 C11 O4 -2.1(5) . . . . ? C13 C10 C11 N2 -0.5(3) . . . . ? C9 C10 C11 N2 177.7(3) . . . . ? C11 N2 C12 O3 -178.8(3) . . . . ? C17 N2 C12 O3 -9.3(5) . . . . ? C11 N2 C12 C13 1.3(3) . . . . ? C17 N2 C12 C13 170.8(2) . . . . ? C9 C10 C13 C14 0.7(4) . . . . ? C11 C10 C13 C14 179.1(2) . . . . ? C9 C10 C13 C12 -177.1(2) . . . . ? C11 C10 C13 C12 1.3(3) . . . . ? O3 C12 C13 C10 178.5(3) . . . . ? N2 C12 C13 C10 -1.6(3) . . . . ? O3 C12 C13 C14 0.8(5) . . . . ? N2 C12 C13 C14 -179.3(3) . . . . ? C10 C13 C14 C15 -0.8(4) . . . . ? C12 C13 C14 C15 176.6(2) . . . . ? C13 C14 C15 C8 -0.3(4) . . . . ? C13 C14 C15 C16 -179.1(2) . . . . ? C9 C8 C15 C14 1.5(4) . . . . ? C7 C8 C15 C14 -177.3(2) . . . . ? C9 C8 C15 C16 -179.5(2) . . . . ? C7 C8 C15 C16 1.7(3) . . . . ? C7 N1 C16 O1 176.5(3) . . . . ? C6 N1 C16 O1 4.5(5) . . . . ? C7 N1 C16 C15 -3.6(3) . . . . ? C6 N1 C16 C15 -175.6(3) . . . . ? C14 C15 C16 O1 -0.1(4) . . . . ? C8 C15 C16 O1 -179.1(3) . . . . ? C14 C15 C16 N1 180.0(3) . . . . ? C8 C15 C16 N1 1.0(3) . . . . ? C12 N2 C17 C18 -87.8(4) . . . . ? C11 N2 C17 C18 80.5(4) . . . . ? N2 C17 C18 C19 -6(3) . . . . ? C17 C18 C19 C20 -5(7) . . . . ? C18 C19 C20 C21 5(9) . . . . ? C19 C20 C21 C22 -1(8) . . . . ? C20 C21 C22 N4 12(3) . . . . ? C32 N4 C22 C21 75.6(4) . . . . ? C23 N4 C22 C21 -91.2(3) . . . . ? C32 N4 C23 O8 -174.7(3) . . . . ? C22 N4 C23 O8 -6.6(5) . . . . ? C32 N4 C23 C24 4.9(3) . . . . ? C22 N4 C23 C24 172.9(2) . . . . ? O8 C23 C24 C25 -3.7(5) . . . . ? N4 C23 C24 C25 176.7(2) . . . . ? O8 C23 C24 C31 176.6(3) . . . . ? N4 C23 C24 C31 -3.0(3) . . . . ? C31 C24 C25 C26 0.2(4) . . . . ? C23 C24 C25 C26 -179.5(2) . . . . ? C24 C25 C26 C29 -1.3(4) . . . . ? C24 C25 C26 C27 180.0(2) . . . . ? C28 N3 C27 O6 176.9(3) . . . . ? C1 N3 C27 O6 6.2(5) . . . . ? C28 N3 C27 C26 -2.9(3) . . . . ? C1 N3 C27 C26 -173.6(3) . . . . ? C25 C26 C27 O6 0.3(5) . . . . ? C29 C26 C27 O6 -178.5(3) . . . . ? C25 C26 C27 N3 -179.9(3) . . . . ? C29 C26 C27 N3 1.3(3) . . . . ? C27 N3 C28 O5 -176.3(3) . . . . ? C1 N3 C28 O5 -5.7(5) . . . . ? C27 N3 C28 C29 3.2(3) . . . . ? C1 N3 C28 C29 173.8(3) . . . . ? C25 C26 C29 C30 1.5(4) . . . . ? C27 C26 C29 C30 -179.6(2) . . . . ? C25 C26 C29 C28 -178.3(2) . . . . ? C27 C26 C29 C28 0.6(3) . . . . ? O5 C28 C29 C26 177.3(3) . . . . ? N3 C28 C29 C26 -2.3(3) . . . . ? O5 C28 C29 C30 -2.5(5) . . . . ? N3 C28 C29 C30 177.9(2) . . . . ? C26 C29 C30 C31 -0.4(4) . . . . ? C28 C29 C30 C31 179.4(2) . . . . ? C29 C30 C31 C24 -0.8(4) . . . . ? C29 C30 C31 C32 179.7(2) . . . . ? C25 C24 C31 C30 0.9(4) . . . . ? C23 C24 C31 C30 -179.4(2) . . . . ? C25 C24 C31 C32 -179.5(2) . . . . ? C23 C24 C31 C32 0.2(3) . . . . ? C23 N4 C32 O7 175.5(3) . . . . ? C22 N4 C32 O7 7.6(4) . . . . ? C23 N4 C32 C31 -4.8(3) . . . . ? C22 N4 C32 C31 -172.8(2) . . . . ? C30 C31 C32 O7 1.9(5) . . . . ? C24 C31 C32 O7 -177.7(3) . . . . ? C30 C31 C32 N4 -177.8(3) . . . . ? C24 C31 C32 N4 2.6(3) . . . . ? C39 O9 C33 C38 -11.5(4) . . . . ? C39 O9 C33 C34 168.2(2) . . . . ? O9 C33 C34 C35 -177.8(2) . . . . ? C38 C33 C34 C35 1.9(4) . . . . ? O9 C33 C34 C67 3.8(3) . . . . ? C38 C33 C34 C67 -176.6(2) . . . . ? C33 C34 C35 C36 0.0(4) . . . . ? C67 C34 C35 C36 178.4(2) . . . . ? C64 O18 C36 C35 11.2(3) . . . . ? C64 O18 C36 C37 -169.6(2) . . . . ? C34 C35 C36 O18 177.5(2) . . . . ? C34 C35 C36 C37 -1.7(3) . . . . ? O18 C36 C37 C38 -177.8(2) . . . . ? C35 C36 C37 C38 1.5(3) . . . . ? O18 C36 C37 C65 4.9(3) . . . . ? C35 C36 C37 C65 -175.8(2) . . . . ? O9 C33 C38 C37 177.5(2) . . . . ? C34 C33 C38 C37 -2.1(4) . . . . ? C36 C37 C38 C33 0.5(3) . . . . ? C65 C37 C38 C33 178.0(2) . . . . ? C33 O9 C39 C40 -175.5(2) . . . . ? C41 O10 C40 C39 -170.4(3) . . . . ? O9 C39 C40 O10 -73.6(3) . . . . ? C40 O10 C41 C42 178.2(3) . . . . ? C43 O11 C42 C41 159.8(2) . . . . ? O10 C41 C42 O11 -69.7(3) . . . . ? C42 O11 C43 C44 -163.6(2) . . . . ? C45 O12 C44 C43 -81.7(4) . . . . ? O11 C43 C44 O12 173.3(3) . . . . ? C44 O12 C45 C46 -91.0(4) . . . . ? C47 O13 C46 C45 -179.2(3) . . . . ? O12 C45 C46 O13 175.4(3) . . . . ? C46 O13 C47 C56 -4.6(5) . . . . ? C46 O13 C47 C48 174.0(3) . . . . ? O13 C47 C48 C53 -178.8(2) . . . . ? C56 C47 C48 C53 -0.1(4) . . . . ? O13 C47 C48 C49 0.4(4) . . . . ? C56 C47 C48 C49 179.0(3) . . . . ? C53 C48 C49 C50 -0.5(4) . . . . ? C47 C48 C49 C50 -179.6(3) . . . . ? C48 C49 C50 C51 0.4(5) . . . . ? C49 C50 C51 C52 -0.6(5) . . . . ? C50 C51 C52 O14 -178.3(3) . . . . ? C50 C51 C52 C53 0.9(5) . . . . ? C47 C48 C53 C52 179.8(2) . . . . ? C49 C48 C53 C52 0.7(4) . . . . ? C47 C48 C53 C54 0.1(4) . . . . ? C49 C48 C53 C54 -179.1(2) . . . . ? C51 C52 C53 C48 -0.9(4) . . . . ? O14 C52 C53 C48 178.4(2) . . . . ? C51 C52 C53 C54 178.8(3) . . . . ? O14 C52 C53 C54 -1.9(4) . . . . ? C48 C53 C54 C55 -0.6(4) . . . . ? C52 C53 C54 C55 179.7(3) . . . . ? C53 C54 C55 C56 1.0(4) . . . . ? O13 C47 C56 C55 179.0(3) . . . . ? C48 C47 C56 C55 0.5(4) . . . . ? C54 C55 C56 C47 -1.0(4) . . . . ? C51 C52 O14 C57 -18.8(5) . . . . ? C53 C52 O14 C57 161.9(4) . . . . ? C51 C52 O14 C57' 13.7(7) . . . . ? C53 C52 O14 C57' -165.5(5) . . . . ? C57 O14 C57' C58' -110.9(14) . . . . ? C52 O14 C57' C58' 178.9(5) . . . . ? O14 C57' C58' O15' 60.6(11) . . . . ? C57' C58' O15' C59' 67.8(11) . . . . ? C58' O15' C59' C60' 168.6(8) . . . . ? C61 O16 C60' C59' -147.7(6) . . . . ? O15' C59' C60' O16 170.8(9) . . . . ? C52 O14 C57 C58 -162.1(4) . . . . ? C57' O14 C57 C58 72.9(10) . . . . ? O14 C57 C58 O15 -179.8(5) . . . . ? C57 C58 O15 C59 -170.2(5) . . . . ? C60' O16 C61 C62 171.0(3) . . . . ? C63 O17 C62 C61 -172.4(3) . . . . ? O16 C61 C62 O17 -71.8(3) . . . . ? C62 O17 C63 C64 172.1(3) . . . . ? C36 O18 C64 C63 -178.0(2) . . . . ? O17 C63 C64 O18 -65.6(3) . . . . ? C66 O20 C65 O19 -2.5(4) . . . . ? C66 O20 C65 C37 176.7(2) . . . . ? C36 C37 C65 O19 167.4(3) . . . . ? C38 C37 C65 O19 -9.9(4) . . . . ? C36 C37 C65 O20 -11.8(3) . . . . ? C38 C37 C65 O20 170.9(2) . . . . ? C68 O22 C67 O21' -0.3(10) . . . . ? C68' O22 C67 O21' -5.1(13) . . . . ? C68 O22 C67 O21 9.0(10) . . . . ? C68' O22 C67 O21 4.2(13) . . . . ? C68 O22 C67 C34 -174.2(5) . . . . ? C68' O22 C67 C34 -179.0(10) . . . . ? C35 C34 C67 O21' -131.1(13) . . . . ? C33 C34 C67 O21' 47.3(13) . . . . ? C35 C34 C67 O21 -142.7(7) . . . . ? C33 C34 C67 O21 35.8(7) . . . . ? C35 C34 C67 O22 40.0(3) . . . . ? C33 C34 C67 O22 -141.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.852 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.852 _refine_diff_density_max 0.743 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.056