# Electronic Supplementary Material (ESI) for CrystEngComm # 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_CCDC931656 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H74 N48 O25 Rb2, 2Cl, 70(H2 O)' _chemical_formula_sum 'C72 H214 Cl2 N48 O95 Rb2' _chemical_formula_weight 3514.75 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' Rb Rb -0.9393 2.9676 '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' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 21.830(14) _cell_length_b 21.830(14) _cell_length_c 52.55(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 21688(25) _cell_formula_units_Z 6 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.615 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 11100 _exptl_absorpt_coefficient_mu 0.845 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8425 _exptl_absorpt_correction_T_max 0.8837 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex2 CCD Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53173 _diffrn_reflns_av_R_equivalents 0.0900 _diffrn_reflns_av_sigmaI/netI 0.0988 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -63 _diffrn_reflns_limit_l_max 64 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 25.99 _reflns_number_total 9361 _reflns_number_gt 3921 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1549P)^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 9361 _refine_ls_number_parameters 446 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1603 _refine_ls_R_factor_gt 0.0845 _refine_ls_wR_factor_ref 0.2826 _refine_ls_wR_factor_gt 0.2539 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.959 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.6667 0.3333 0.2907(4) 0.467(10) Uiso 1 3 d S . . Cl2 Cl 0.5320(8) 0.4218(9) 0.3163(3) 0.127(8) Uiso 0.169(8) 1 d P A 1 Cl2' Cl 0.5046(10) 0.4619(11) 0.3144(4) 0.152(9) Uiso 0.165(8) 1 d P A 2 O1W O 0.6667 0.3333 0.1581(7) 0.45(2) Uiso 1 3 d S . . Rb1 Rb 0.0000 0.0000 0.23243(2) 0.0727(4) Uani 1 3 d S . . Rb2 Rb 0.6667 0.3333 0.21971(3) 0.0807(4) Uani 1 3 d S . . C1 C 0.3977(3) -0.0499(3) 0.20057(17) 0.079(2) Uani 1 1 d . . . C2 C 0.5203(3) 0.0099(3) 0.19403(14) 0.0675(19) Uani 1 1 d . . . H2 H 0.5513 -0.0110 0.1938 0.081 Uiso 1 1 calc R . . C3 C 0.5030(3) 0.0227(3) 0.22142(13) 0.0588(16) Uani 1 1 d . . . H3 H 0.5209 0.0025 0.2343 0.071 Uiso 1 1 calc R . . C4 C 0.5681(3) 0.1306(3) 0.20057(14) 0.0641(17) Uani 1 1 d . . . C5 C 0.3850(3) -0.0292(3) 0.24412(13) 0.0703(17) Uani 1 1 d . . . H5A H 0.4076 -0.0432 0.2572 0.084 Uiso 1 1 calc R . . H5B H 0.3378 -0.0698 0.2410 0.084 Uiso 1 1 calc R . . C6 C 0.5473(3) 0.1336(3) 0.24695(14) 0.0700(18) Uani 1 1 d . . . H6A H 0.5888 0.1811 0.2455 0.084 Uiso 1 1 calc R . . H6B H 0.5578 0.1080 0.2600 0.084 Uiso 1 1 calc R . . C7 C 0.3123(3) 0.0244(3) 0.25628(12) 0.0603(15) Uani 1 1 d . . . C8 C 0.4307(3) 0.0845(3) 0.26892(12) 0.0593(15) Uani 1 1 d . . . H8 H 0.4485 0.0651 0.2822 0.071 Uiso 1 1 calc R . . C9 C 0.3925(3) 0.1212(3) 0.28121(12) 0.0582(15) Uani 1 1 d . . . H9 H 0.3952 0.1221 0.3000 0.070 Uiso 1 1 calc R . . C10 C 0.4891(3) 0.2035(3) 0.25677(12) 0.0608(16) Uani 1 1 d . . . C11 C 0.2597(3) 0.0781(3) 0.28349(13) 0.0632(16) Uani 1 1 d . . . H11A H 0.2650 0.0782 0.3020 0.076 Uiso 1 1 calc R . . H11B H 0.2166 0.0342 0.2789 0.076 Uiso 1 1 calc R . . C12 C 0.4228(3) 0.2493(3) 0.28156(13) 0.0644(17) Uani 1 1 d . . . H12A H 0.4220 0.2444 0.3001 0.077 Uiso 1 1 calc R . . H12B H 0.4645 0.2945 0.2771 0.077 Uiso 1 1 calc R . . C13 C 0.1885(3) 0.1269(3) 0.26518(12) 0.0612(15) Uani 1 1 d . . . C14 C 0.2918(3) 0.2075(3) 0.28652(12) 0.0607(15) Uani 1 1 d . . . H14 H 0.2974 0.2065 0.3052 0.073 Uiso 1 1 calc R . . C15 C 0.2514(3) 0.2439(3) 0.27957(11) 0.0618(16) Uani 1 1 d . . . H15 H 0.2386 0.2616 0.2949 0.074 Uiso 1 1 calc R . . C16 C 0.3638(3) 0.3065(3) 0.26090(12) 0.0621(16) Uani 1 1 d . . . C17 C 0.1288(3) 0.1985(3) 0.25975(12) 0.0657(17) Uani 1 1 d . . . H17A H 0.0862 0.1518 0.2586 0.079 Uiso 1 1 calc R . . H17B H 0.1211 0.2250 0.2732 0.079 Uiso 1 1 calc R . . C18 C 0.2888(3) 0.3613(3) 0.25646(15) 0.080(2) Uani 1 1 d . . . H18A H 0.2664 0.3711 0.2709 0.096 Uiso 1 1 calc R . . H18B H 0.3349 0.4036 0.2536 0.096 Uiso 1 1 calc R . . C19 C 0.1056(3) 0.2033(3) 0.21397(14) 0.0626(16) Uani 1 1 d . . . C20 C 0.1701(3) 0.3108(3) 0.23445(14) 0.0608(17) Uani 1 1 d . . . H20 H 0.1513 0.3285 0.2480 0.073 Uiso 1 1 calc R . . C21 C 0.1494(3) 0.3234(3) 0.20842(14) 0.0655(19) Uani 1 1 d . . . H21 H 0.1180 0.3439 0.2093 0.079 Uiso 1 1 calc R . . C22 C 0.2722(4) 0.3874(3) 0.21217(17) 0.080(2) Uani 1 1 d . . . C23 C 0.5944(3) 0.0957(3) 0.15890(14) 0.076(2) Uani 1 1 d . . . H23A H 0.6315 0.1456 0.1587 0.091 Uiso 1 1 calc R . . H23B H 0.6178 0.0673 0.1585 0.091 Uiso 1 1 calc R . . C24 C 0.4410(3) -0.0788(3) 0.15879(16) 0.086(2) Uani 1 1 d . . . H24A H 0.4756 -0.0949 0.1584 0.103 Uiso 1 1 calc R . . H24B H 0.3937 -0.1208 0.1588 0.103 Uiso 1 1 calc R . . N1 N 0.4509(3) -0.0372(3) 0.18285(13) 0.0899(13) Uani 1 1 d . . . N2 N 0.4252(2) -0.0135(2) 0.22130(10) 0.0614(13) Uani 1 1 d . . . N3 N 0.5546(2) 0.0811(2) 0.18297(10) 0.0589(12) Uani 1 1 d . . . N4 N 0.5372(2) 0.0983(2) 0.22334(11) 0.0609(13) Uani 1 1 d . . . N5 N 0.3771(2) 0.0287(2) 0.25398(9) 0.0595(12) Uani 1 1 d . . . N6 N 0.3193(2) 0.0783(2) 0.27176(9) 0.0576(12) Uani 1 1 d . . . N7 N 0.4880(2) 0.1401(2) 0.25534(9) 0.0581(12) Uani 1 1 d . . . N8 N 0.4295(3) 0.1922(3) 0.27004(12) 0.0899(13) Uani 1 1 d . . . N9 N 0.2508(2) 0.1379(2) 0.27635(9) 0.0601(12) Uani 1 1 d . . . N10 N 0.1890(2) 0.1898(3) 0.26668(9) 0.0641(13) Uani 1 1 d . . . N11 N 0.3610(2) 0.2503(2) 0.27371(10) 0.0620(13) Uani 1 1 d . . . N12 N 0.2994(2) 0.3019(2) 0.26305(10) 0.0637(13) Uani 1 1 d . . . N13 N 0.1394(2) 0.2346(2) 0.23617(10) 0.0562(12) Uani 1 1 d . . . N14 N 0.1136(2) 0.2520(2) 0.19664(10) 0.0584(12) Uani 1 1 d . . . N15 N 0.2465(2) 0.3484(3) 0.23467(13) 0.0756(16) Uani 1 1 d . . . N16 N 0.2176(3) 0.3720(2) 0.19659(12) 0.0686(14) Uani 1 1 d . . . O1 O 0.3345(2) -0.0911(3) 0.19502(10) 0.1038(18) Uani 1 1 d . . . O2 O 0.2568(2) -0.0205(2) 0.24697(8) 0.0715(12) Uani 1 1 d . . . O3 O 0.14144(19) 0.0713(2) 0.25622(8) 0.0693(12) Uani 1 1 d . . . O4 O 0.0707(2) 0.1375(2) 0.21064(8) 0.0757(12) Uani 1 1 d . . . O5 O 0.6018(2) 0.1953(2) 0.19790(9) 0.0815(13) Uani 1 1 d . . . O6 O 0.5338(2) 0.2601(2) 0.24797(9) 0.0748(12) Uani 1 1 d . . . O7 O 0.4144(2) 0.3519(2) 0.24940(10) 0.0794(13) Uani 1 1 d . . . O8 O 0.3360(2) 0.4321(2) 0.20804(11) 0.0986(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rb1 0.0444(4) 0.0444(4) 0.1293(10) 0.000 0.000 0.02218(19) Rb2 0.0486(4) 0.0486(4) 0.1450(12) 0.000 0.000 0.0243(2) C1 0.043(4) 0.046(3) 0.144(7) -0.001(4) 0.040(4) 0.019(3) C2 0.032(3) 0.044(3) 0.124(6) 0.013(3) 0.015(3) 0.017(3) C3 0.039(3) 0.049(3) 0.088(5) 0.019(3) 0.000(3) 0.021(3) C4 0.038(3) 0.045(4) 0.095(5) 0.007(4) -0.014(3) 0.010(3) C5 0.060(4) 0.055(4) 0.092(5) 0.007(3) -0.002(4) 0.026(3) C6 0.034(3) 0.050(3) 0.116(6) 0.000(4) -0.016(3) 0.013(3) C7 0.040(3) 0.053(4) 0.076(4) 0.012(3) 0.002(3) 0.014(3) C8 0.048(3) 0.050(3) 0.079(4) 0.009(3) -0.002(3) 0.024(3) C9 0.045(3) 0.043(3) 0.079(4) 0.005(3) -0.001(3) 0.016(3) C10 0.035(3) 0.064(4) 0.078(4) 0.009(3) -0.001(3) 0.020(3) C11 0.048(3) 0.049(3) 0.084(4) 0.010(3) 0.012(3) 0.017(3) C12 0.043(3) 0.049(3) 0.097(5) -0.027(3) -0.027(3) 0.020(3) C13 0.054(4) 0.052(4) 0.075(4) 0.010(3) 0.012(3) 0.024(3) C14 0.048(3) 0.059(4) 0.068(4) -0.007(3) -0.007(3) 0.021(3) C15 0.047(3) 0.058(4) 0.072(4) -0.018(3) 0.003(3) 0.020(3) C16 0.036(3) 0.050(4) 0.088(5) -0.012(3) -0.008(3) 0.012(3) C17 0.045(3) 0.057(4) 0.085(5) 0.004(3) 0.008(3) 0.018(3) C18 0.055(4) 0.045(4) 0.127(6) -0.003(4) -0.008(4) 0.014(3) C19 0.039(3) 0.048(4) 0.104(5) 0.003(4) 0.008(3) 0.023(3) C20 0.038(3) 0.042(3) 0.107(5) -0.007(3) 0.002(3) 0.024(3) C21 0.039(3) 0.035(3) 0.119(6) -0.001(3) 0.024(3) 0.016(3) C22 0.050(4) 0.044(4) 0.144(7) -0.013(4) 0.013(5) 0.021(3) C23 0.032(3) 0.049(4) 0.131(6) 0.014(4) -0.007(4) 0.009(3) C24 0.061(4) 0.040(3) 0.149(7) -0.008(4) 0.027(4) 0.020(3) N1 0.060(2) 0.064(3) 0.133(4) -0.009(3) -0.001(2) 0.022(2) N2 0.040(3) 0.047(3) 0.079(4) -0.009(3) 0.014(3) 0.008(2) N3 0.042(3) 0.044(3) 0.086(4) 0.013(3) 0.001(3) 0.018(2) N4 0.039(3) 0.047(3) 0.088(4) 0.001(3) -0.008(3) 0.015(2) N5 0.041(3) 0.046(3) 0.078(3) -0.005(2) -0.001(2) 0.012(2) N6 0.041(3) 0.047(3) 0.077(3) -0.010(2) -0.004(2) 0.016(2) N7 0.038(3) 0.048(3) 0.079(3) 0.012(2) 0.004(2) 0.014(2) N8 0.060(2) 0.064(3) 0.133(4) -0.009(3) -0.001(2) 0.022(2) N9 0.035(2) 0.053(3) 0.087(3) -0.002(3) -0.006(2) 0.018(2) N10 0.041(3) 0.058(3) 0.085(4) 0.003(3) 0.010(2) 0.019(2) N11 0.043(3) 0.043(3) 0.093(4) -0.003(3) -0.007(3) 0.016(2) N12 0.045(3) 0.044(3) 0.100(4) -0.013(3) -0.002(3) 0.020(2) N13 0.042(3) 0.039(3) 0.082(4) -0.001(3) 0.010(3) 0.015(2) N14 0.034(2) 0.037(3) 0.094(4) 0.009(3) 0.001(3) 0.010(2) N15 0.035(3) 0.046(3) 0.140(5) 0.013(3) 0.003(3) 0.016(2) N16 0.046(3) 0.035(3) 0.113(4) 0.007(3) 0.016(3) 0.012(2) O1 0.039(2) 0.082(3) 0.155(5) -0.049(3) 0.010(3) 0.004(2) O2 0.052(2) 0.055(2) 0.093(3) -0.010(2) -0.004(2) 0.015(2) O3 0.044(2) 0.046(2) 0.107(3) -0.014(2) -0.016(2) 0.0143(19) O4 0.065(3) 0.038(2) 0.101(3) 0.006(2) 0.005(2) 0.008(2) O5 0.063(3) 0.051(3) 0.101(3) 0.004(2) -0.005(2) 0.007(2) O6 0.048(2) 0.045(2) 0.115(3) 0.012(2) -0.002(2) 0.010(2) O7 0.041(2) 0.049(2) 0.138(4) 0.008(3) 0.002(2) 0.015(2) O8 0.042(2) 0.055(3) 0.183(5) 0.006(3) 0.022(3) 0.014(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 Rb2 3.728(19) . ? O1W Rb1 3.00(4) 13 ? O1W Rb2 3.24(4) . ? Rb1 O4 2.842(4) 2 ? Rb1 O4 2.842(4) 3 ? Rb1 O4 2.842(4) . ? Rb1 O3 2.952(4) . ? Rb1 O3 2.952(4) 3 ? Rb1 O3 2.952(4) 2 ? Rb1 O1W 3.00(4) 13 ? Rb2 O5 2.852(5) . ? Rb2 O5 2.852(5) 2_655 ? Rb2 O5 2.852(5) 3_665 ? Rb2 O6 2.921(4) 2_655 ? Rb2 O6 2.921(4) . ? Rb2 O6 2.921(4) 3_665 ? C1 O1 1.248(8) . ? C1 N2 1.306(9) . ? C1 N1 1.403(8) . ? C2 N1 1.463(8) . ? C2 N3 1.466(7) . ? C2 C3 1.548(9) . ? C2 H2 0.9900 . ? C3 N4 1.434(7) . ? C3 N2 1.471(6) . ? C3 H3 0.9900 . ? C4 O5 1.230(7) . ? C4 N3 1.340(8) . ? C4 N4 1.382(8) . ? C5 N2 1.423(8) . ? C5 N5 1.455(7) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.418(8) . ? C6 N7 1.440(7) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.216(6) . ? C7 N5 1.375(7) . ? C7 N6 1.374(7) . ? C8 N7 1.425(7) . ? C8 N5 1.430(7) . ? C8 C9 1.558(8) . ? C8 H8 0.9900 . ? C9 N8 1.465(7) . ? C9 N6 1.476(7) . ? C9 H9 0.9900 . ? C10 O6 1.220(7) . ? C10 N7 1.376(7) . ? C10 N8 1.385(8) . ? C11 N6 1.439(7) . ? C11 N9 1.461(7) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.421(7) . ? C12 N8 1.457(7) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.226(7) . ? C13 N10 1.368(7) . ? C13 N9 1.389(7) . ? C14 N9 1.427(7) . ? C14 N11 1.482(7) . ? C14 C15 1.498(8) . ? C14 H14 0.9900 . ? C15 N10 1.450(7) . ? C15 N12 1.459(7) . ? C15 H15 0.9900 . ? C16 O7 1.213(7) . ? C16 N12 1.363(7) . ? C16 N11 1.374(7) . ? C17 N13 1.425(7) . ? C17 N10 1.464(7) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N15 1.407(8) . ? C18 N12 1.469(8) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.256(7) . ? C19 N14 1.344(7) . ? C19 N13 1.367(8) . ? C20 N15 1.445(7) . ? C20 N13 1.451(6) . ? C20 C21 1.509(9) . ? C20 H20 0.9900 . ? C21 N16 1.466(7) . ? C21 N14 1.484(7) . ? C21 H21 0.9900 . ? C22 O8 1.256(7) . ? C22 N16 1.344(9) . ? C22 N15 1.400(9) . ? C23 N14 1.412(7) 13 ? C23 N3 1.476(8) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N16 1.410(9) 13 ? C24 N1 1.509(9) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? N14 C23 1.412(7) 13 ? N16 C24 1.410(9) 13 ? 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 Rb1 O1W Rb2 180.0 13 . ? O4 Rb1 O4 104.85(11) 2 3 ? O4 Rb1 O4 104.85(11) 2 . ? O4 Rb1 O4 104.85(11) 3 . ? O4 Rb1 O3 178.29(12) 2 . ? O4 Rb1 O3 76.80(12) 3 . ? O4 Rb1 O3 74.99(12) . . ? O4 Rb1 O3 76.80(12) 2 3 ? O4 Rb1 O3 74.99(12) 3 3 ? O4 Rb1 O3 178.29(12) . 3 ? O3 Rb1 O3 103.35(10) . 3 ? O4 Rb1 O3 74.99(12) 2 2 ? O4 Rb1 O3 178.29(12) 3 2 ? O4 Rb1 O3 76.80(12) . 2 ? O3 Rb1 O3 103.35(10) . 2 ? O3 Rb1 O3 103.35(10) 3 2 ? O4 Rb1 O1W 66.23(9) 2 13 ? O4 Rb1 O1W 66.23(9) 3 13 ? O4 Rb1 O1W 66.23(9) . 13 ? O3 Rb1 O1W 115.06(9) . 13 ? O3 Rb1 O1W 115.06(9) 3 13 ? O3 Rb1 O1W 115.06(9) 2 13 ? O5 Rb2 O5 104.93(11) . 2_655 ? O5 Rb2 O5 104.93(11) . 3_665 ? O5 Rb2 O5 104.93(11) 2_655 3_665 ? O5 Rb2 O6 80.02(12) . 2_655 ? O5 Rb2 O6 78.10(12) 2_655 2_655 ? O5 Rb2 O6 173.03(13) 3_665 2_655 ? O5 Rb2 O6 78.10(12) . . ? O5 Rb2 O6 173.03(13) 2_655 . ? O5 Rb2 O6 80.02(12) 3_665 . ? O6 Rb2 O6 96.45(12) 2_655 . ? O5 Rb2 O6 173.03(13) . 3_665 ? O5 Rb2 O6 80.02(12) 2_655 3_665 ? O5 Rb2 O6 78.10(12) 3_665 3_665 ? O6 Rb2 O6 96.45(12) 2_655 3_665 ? O6 Rb2 O6 96.45(12) . 3_665 ? O5 Rb2 O1W 66.30(9) . . ? O5 Rb2 O1W 66.30(9) 2_655 . ? O5 Rb2 O1W 66.30(9) 3_665 . ? O6 Rb2 O1W 120.56(9) 2_655 . ? O6 Rb2 O1W 120.56(9) . . ? O6 Rb2 O1W 120.56(9) 3_665 . ? O5 Rb2 Cl1 113.70(9) . . ? O5 Rb2 Cl1 113.70(9) 2_655 . ? O5 Rb2 Cl1 113.70(9) 3_665 . ? O6 Rb2 Cl1 59.44(9) 2_655 . ? O6 Rb2 Cl1 59.44(9) . . ? O6 Rb2 Cl1 59.44(9) 3_665 . ? O1W Rb2 Cl1 180.000(2) . . ? O1 C1 N2 129.8(6) . . ? O1 C1 N1 119.7(7) . . ? N2 C1 N1 110.5(6) . . ? N1 C2 N3 112.7(5) . . ? N1 C2 C3 103.9(5) . . ? N3 C2 C3 102.7(5) . . ? N1 C2 H2 112.3 . . ? N3 C2 H2 112.3 . . ? C3 C2 H2 112.3 . . ? N4 C3 N2 114.5(4) . . ? N4 C3 C2 103.9(5) . . ? N2 C3 C2 102.6(5) . . ? N4 C3 H3 111.7 . . ? N2 C3 H3 111.7 . . ? C2 C3 H3 111.7 . . ? O5 C4 N3 127.7(7) . . ? O5 C4 N4 123.0(6) . . ? N3 C4 N4 109.4(5) . . ? N2 C5 N5 114.6(5) . . ? N2 C5 H5A 108.6 . . ? N5 C5 H5A 108.6 . . ? N2 C5 H5B 108.6 . . ? N5 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? N4 C6 N7 114.6(5) . . ? N4 C6 H6A 108.6 . . ? N7 C6 H6A 108.6 . . ? N4 C6 H6B 108.6 . . ? N7 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? O2 C7 N5 126.5(6) . . ? O2 C7 N6 124.7(5) . . ? N5 C7 N6 108.8(5) . . ? N7 C8 N5 116.6(5) . . ? N7 C8 C9 103.7(4) . . ? N5 C8 C9 104.1(4) . . ? N7 C8 H8 110.7 . . ? N5 C8 H8 110.7 . . ? C9 C8 H8 110.7 . . ? N8 C9 N6 112.6(5) . . ? N8 C9 C8 103.0(5) . . ? N6 C9 C8 102.9(4) . . ? N8 C9 H9 112.5 . . ? N6 C9 H9 112.5 . . ? C8 C9 H9 112.5 . . ? O6 C10 N7 126.9(5) . . ? O6 C10 N8 125.3(6) . . ? N7 C10 N8 107.8(5) . . ? N6 C11 N9 114.3(5) . . ? N6 C11 H11A 108.7 . . ? N9 C11 H11A 108.7 . . ? N6 C11 H11B 108.7 . . ? N9 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? N11 C12 N8 113.2(5) . . ? N11 C12 H12A 108.9 . . ? N8 C12 H12A 108.9 . . ? N11 C12 H12B 108.9 . . ? N8 C12 H12B 108.9 . . ? H12A C12 H12B 107.8 . . ? O3 C13 N10 126.7(6) . . ? O3 C13 N9 126.6(5) . . ? N10 C13 N9 106.7(5) . . ? N9 C14 N11 113.5(5) . . ? N9 C14 C15 104.6(4) . . ? N11 C14 C15 103.9(5) . . ? N9 C14 H14 111.5 . . ? N11 C14 H14 111.5 . . ? C15 C14 H14 111.5 . . ? N10 C15 N12 113.9(5) . . ? N10 C15 C14 104.1(5) . . ? N12 C15 C14 104.3(4) . . ? N10 C15 H15 111.4 . . ? N12 C15 H15 111.4 . . ? C14 C15 H15 111.4 . . ? O7 C16 N12 125.8(6) . . ? O7 C16 N11 126.1(5) . . ? N12 C16 N11 108.1(5) . . ? N13 C17 N10 112.5(5) . . ? N13 C17 H17A 109.1 . . ? N10 C17 H17A 109.1 . . ? N13 C17 H17B 109.1 . . ? N10 C17 H17B 109.1 . . ? H17A C17 H17B 107.8 . . ? N15 C18 N12 113.0(5) . . ? N15 C18 H18A 109.0 . . ? N12 C18 H18A 109.0 . . ? N15 C18 H18B 109.0 . . ? N12 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? O4 C19 N14 125.1(6) . . ? O4 C19 N13 123.9(6) . . ? N14 C19 N13 111.0(5) . . ? N15 C20 N13 113.0(4) . . ? N15 C20 C21 105.7(5) . . ? N13 C20 C21 104.8(5) . . ? N15 C20 H20 111.0 . . ? N13 C20 H20 111.0 . . ? C21 C20 H20 111.0 . . ? N16 C21 N14 113.2(5) . . ? N16 C21 C20 103.2(5) . . ? N14 C21 C20 103.6(5) . . ? N16 C21 H21 112.1 . . ? N14 C21 H21 112.1 . . ? C20 C21 H21 112.1 . . ? O8 C22 N16 126.1(8) . . ? O8 C22 N15 124.8(7) . . ? N16 C22 N15 109.0(6) . . ? N14 C23 N3 114.7(5) 13 . ? N14 C23 H23A 108.6 13 . ? N3 C23 H23A 108.6 . . ? N14 C23 H23B 108.6 13 . ? N3 C23 H23B 108.6 . . ? H23A C23 H23B 107.6 . . ? N16 C24 N1 112.2(5) 13 . ? N16 C24 H24A 109.2 13 . ? N1 C24 H24A 109.2 . . ? N16 C24 H24B 109.2 13 . ? N1 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? C1 N1 C2 109.7(6) . . ? C1 N1 C24 125.6(6) . . ? C2 N1 C24 123.1(5) . . ? C1 N2 C5 121.0(5) . . ? C1 N2 C3 112.7(5) . . ? C5 N2 C3 122.3(5) . . ? C4 N3 C2 111.8(5) . . ? C4 N3 C23 123.3(5) . . ? C2 N3 C23 120.2(5) . . ? C4 N4 C6 125.2(5) . . ? C4 N4 C3 111.5(5) . . ? C6 N4 C3 122.5(5) . . ? C7 N5 C8 112.8(5) . . ? C7 N5 C5 122.5(5) . . ? C8 N5 C5 122.2(5) . . ? C7 N6 C11 122.5(5) . . ? C7 N6 C9 111.4(4) . . ? C11 N6 C9 123.3(5) . . ? C10 N7 C8 113.4(5) . . ? C10 N7 C6 123.6(4) . . ? C8 N7 C6 121.2(5) . . ? C10 N8 C12 122.8(5) . . ? C10 N8 C9 111.3(5) . . ? C12 N8 C9 120.1(6) . . ? C13 N9 C14 112.3(5) . . ? C13 N9 C11 120.7(5) . . ? C14 N9 C11 124.3(5) . . ? C13 N10 C15 112.2(5) . . ? C13 N10 C17 123.9(5) . . ? C15 N10 C17 123.2(5) . . ? C16 N11 C12 122.5(5) . . ? C16 N11 C14 111.1(5) . . ? C12 N11 C14 122.4(5) . . ? C16 N12 C15 112.4(5) . . ? C16 N12 C18 121.9(5) . . ? C15 N12 C18 122.9(5) . . ? C19 N13 C17 124.6(5) . . ? C19 N13 C20 110.2(5) . . ? C17 N13 C20 122.9(5) . . ? C19 N14 C23 124.6(5) . 13 ? C19 N14 C21 109.9(5) . . ? C23 N14 C21 121.4(5) 13 . ? C22 N15 C18 122.8(5) . . ? C22 N15 C20 109.7(6) . . ? C18 N15 C20 125.1(6) . . ? C22 N16 C24 121.7(6) . 13 ? C22 N16 C21 112.1(6) . . ? C24 N16 C21 124.4(6) 13 . ? C13 O3 Rb1 145.3(4) . . ? C19 O4 Rb1 148.2(4) . . ? C4 O5 Rb2 149.6(5) . . ? C10 O6 Rb2 145.1(4) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.067 _refine_diff_density_min -0.669 _refine_diff_density_rms 0.090 # 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 0.000 0.000 0.000 138 48 ' ' 2 -0.004 0.469 -0.001 6399 3007 ' ' 3 -0.167 0.667 0.167 356 113 ' ' 4 0.000 0.500 0.500 356 116 ' ' 5 0.167 0.333 0.833 356 113 ' ' 6 0.167 0.833 0.833 356 116 ' ' 7 0.333 0.167 0.167 357 116 ' ' 8 0.333 0.667 0.667 134 48 ' ' 9 0.500 1.000 0.500 356 113 ' ' 10 0.500 0.500 0.500 356 116 ' ' 11 0.667 0.833 0.833 357 116 ' ' 12 0.667 0.333 0.333 134 48 ' ' 13 0.833 0.167 0.167 356 116 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 931656' ####################################################################### # # 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_CCDC931657 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H74 N48 O25 Rb2, 2Cl, 68(H2 O)' _chemical_formula_sum 'C72 H210 Cl2 N48 O93 Rb2' _chemical_formula_weight 3478.72 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' Rb Rb -0.9393 2.9676 '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' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 21.7553(14) _cell_length_b 21.7553(14) _cell_length_c 52.070(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 21343(2) _cell_formula_units_Z 6 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.624 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10980 _exptl_absorpt_coefficient_mu 0.857 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7594 _exptl_absorpt_correction_T_max 0.7892 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex2 CCD Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52620 _diffrn_reflns_av_R_equivalents 0.0671 _diffrn_reflns_av_sigmaI/netI 0.0657 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -63 _diffrn_reflns_limit_l_max 63 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 25.99 _reflns_number_total 9246 _reflns_number_gt 4905 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1455P)^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 9246 _refine_ls_number_parameters 452 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1165 _refine_ls_R_factor_gt 0.0708 _refine_ls_wR_factor_ref 0.2347 _refine_ls_wR_factor_gt 0.2120 _refine_ls_goodness_of_fit_ref 0.951 _refine_ls_restrained_S_all 0.951 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.0000 0.0000 0.04452(19) 0.300(4) Uiso 1 3 d S . . Cl2 Cl 0.3319(5) -0.0400(6) 0.0181(2) 0.127(5) Uiso 0.224(8) 1 d P A 1 Cl2' Cl 0.3373(9) -0.0027(11) 0.0059(4) 0.109(9) Uiso 0.110(8) 1 d P A 2 O1W O 0.6667 0.3333 0.1611(7) 0.457(19) Uiso 1 3 d S . . Rb1 Rb 0.0000 0.0000 0.113479(19) 0.0693(3) Uani 1 3 d S . . Rb2 Rb 0.6667 0.3333 0.099714(18) 0.0650(3) Uani 1 3 d S . . C1 C 0.3971(2) 0.4478(2) 0.19911(11) 0.0630(13) Uani 1 1 d . . . C2 C 0.5028(2) 0.4813(2) 0.22045(10) 0.0566(12) Uani 1 1 d . . . H2 H 0.5203 0.5197 0.2332 0.068 Uiso 1 1 calc R . . C3 C 0.5199(2) 0.5103(2) 0.19281(9) 0.0517(11) Uani 1 1 d . . . H3 H 0.5510 0.5620 0.1923 0.062 Uiso 1 1 calc R . . C4 C 0.5682(2) 0.4371(2) 0.19992(9) 0.0536(11) Uani 1 1 d . . . C5 C 0.4405(2) 0.5179(3) 0.15914(11) 0.0675(14) Uani 1 1 d . . . H5A H 0.3934 0.5123 0.1594 0.081 Uiso 1 1 calc R . . H5B H 0.4746 0.5684 0.1589 0.081 Uiso 1 1 calc R . . C6 C 0.5942(2) 0.4983(3) 0.15796(9) 0.0596(12) Uani 1 1 d . . . H6A H 0.6177 0.5497 0.1575 0.071 Uiso 1 1 calc R . . H6B H 0.6307 0.4850 0.1576 0.071 Uiso 1 1 calc R . . C7 C 0.3926(2) 0.4472(2) 0.11938(12) 0.0687(15) Uani 1 1 d . . . C8 C 0.5162(2) 0.5064(2) 0.12405(10) 0.0546(12) Uani 1 1 d . . . H8 H 0.5474 0.5580 0.1232 0.066 Uiso 1 1 calc R . . C9 C 0.49602(19) 0.4736(2) 0.09767(9) 0.0461(10) Uani 1 1 d . . . H9 H 0.5150 0.5101 0.0843 0.055 Uiso 1 1 calc R . . C10 C 0.5605(2) 0.4301(2) 0.11791(9) 0.0486(11) Uani 1 1 d . . . C11 C 0.3768(2) 0.4052(2) 0.07477(11) 0.0668(14) Uani 1 1 d . . . H11A H 0.3997 0.4369 0.0604 0.080 Uiso 1 1 calc R . . H11B H 0.3307 0.4011 0.0772 0.080 Uiso 1 1 calc R . . C12 C 0.5365(2) 0.4006(2) 0.07267(9) 0.0513(11) Uani 1 1 d . . . H12A H 0.5783 0.3958 0.0741 0.062 Uiso 1 1 calc R . . H12B H 0.5452 0.4347 0.0592 0.062 Uiso 1 1 calc R . . C13 C 0.3024(2) 0.2750(2) 0.07100(9) 0.0512(11) Uani 1 1 d . . . C14 C 0.4148(2) 0.3260(2) 0.05223(9) 0.0530(11) Uani 1 1 d . . . H14 H 0.4273 0.3559 0.0369 0.064 Uiso 1 1 calc R . . C15 C 0.3730(2) 0.2464(2) 0.04542(9) 0.0533(11) Uani 1 1 d . . . H15 H 0.3669 0.2386 0.0268 0.064 Uiso 1 1 calc R . . C16 C 0.4774(2) 0.2705(2) 0.06658(8) 0.0498(10) Uani 1 1 d . . . C17 C 0.2416(2) 0.1573(2) 0.05069(10) 0.0573(12) Uani 1 1 d . . . H17A H 0.2421 0.1531 0.0321 0.069 Uiso 1 1 calc R . . H17B H 0.2001 0.1605 0.0552 0.069 Uiso 1 1 calc R . . C18 C 0.4066(2) 0.1503(2) 0.04852(9) 0.0508(11) Uani 1 1 d . . . H18A H 0.4494 0.1492 0.0529 0.061 Uiso 1 1 calc R . . H18B H 0.4008 0.1455 0.0300 0.061 Uiso 1 1 calc R . . C19 C 0.1777(2) 0.0474(2) 0.07590(8) 0.0490(10) Uani 1 1 d . . . C20 C 0.2737(2) 0.0609(2) 0.05191(8) 0.0477(10) Uani 1 1 d . . . H20 H 0.2712 0.0589 0.0331 0.057 Uiso 1 1 calc R . . C21 C 0.2351(2) -0.0141(2) 0.06376(9) 0.0519(11) Uani 1 1 d . . . H21 H 0.2176 -0.0507 0.0504 0.062 Uiso 1 1 calc R . . C22 C 0.3538(2) 0.0432(2) 0.07620(8) 0.0499(10) Uani 1 1 d . . . C23 C 0.1174(2) -0.0817(2) 0.08696(10) 0.0604(13) Uani 1 1 d . . . H23A H 0.0769 -0.0748 0.0889 0.072 Uiso 1 1 calc R . . H23B H 0.1052 -0.1183 0.0741 0.072 Uiso 1 1 calc R . . C24 C 0.2820(2) -0.0816(2) 0.08878(9) 0.0581(12) Uani 1 1 d . . . H24A H 0.3289 -0.0752 0.0917 0.070 Uiso 1 1 calc R . . H24B H 0.2587 -0.1184 0.0759 0.070 Uiso 1 1 calc R . . N1 N 0.42505(17) 0.43865(18) 0.22063(8) 0.0538(9) Uani 1 1 d . . . N2 N 0.45062(17) 0.48800(19) 0.18220(8) 0.0550(9) Uani 1 1 d . . . N3 N 0.53742(16) 0.43910(18) 0.22299(8) 0.0502(9) Uani 1 1 d . . . N4 N 0.55348(17) 0.47267(18) 0.18233(7) 0.0511(9) Uani 1 1 d . . . N5 N 0.44823(18) 0.48672(19) 0.13622(8) 0.0573(10) Uani 1 1 d . . . N6 N 0.41923(18) 0.43572(18) 0.09769(9) 0.0625(11) Uani 1 1 d . . . N7 N 0.55150(16) 0.47080(17) 0.13609(7) 0.0490(9) Uani 1 1 d . . . N8 N 0.52715(17) 0.42782(17) 0.09608(7) 0.0463(8) Uani 1 1 d . . . N9 N 0.36721(18) 0.33585(18) 0.06879(8) 0.0585(10) Uani 1 1 d . . . N10 N 0.30473(16) 0.22189(18) 0.05862(7) 0.0511(9) Uani 1 1 d . . . N11 N 0.47792(17) 0.33380(18) 0.06532(7) 0.0506(9) Uani 1 1 d . . . N12 N 0.41465(16) 0.21811(17) 0.05632(7) 0.0484(8) Uani 1 1 d . . . N13 N 0.23565(17) 0.09359(18) 0.06230(7) 0.0514(9) Uani 1 1 d . . . N14 N 0.17757(17) -0.01585(18) 0.07765(7) 0.0542(9) Uani 1 1 d . . . N15 N 0.34588(16) 0.09038(17) 0.06077(7) 0.0483(8) Uani 1 1 d . . . N16 N 0.28937(17) -0.01571(18) 0.07889(7) 0.0506(9) Uani 1 1 d . . . O1 O 0.33363(16) 0.4261(2) 0.19461(8) 0.0914(13) Uani 1 1 d . . . O2 O 0.32990(16) 0.42981(17) 0.12358(8) 0.0803(11) Uani 1 1 d . . . O3 O 0.25146(15) 0.27056(16) 0.08274(7) 0.0697(9) Uani 1 1 d . . . O4 O 0.13289(15) 0.05908(16) 0.08528(7) 0.0658(9) Uani 1 1 d . . . O5 O 0.60241(16) 0.40706(17) 0.19719(6) 0.0660(9) Uani 1 1 d . . . O6 O 0.59550(15) 0.40014(17) 0.12188(6) 0.0607(8) Uani 1 1 d . . . O7 O 0.52445(14) 0.26214(16) 0.07607(6) 0.0575(8) Uani 1 1 d . . . O8 O 0.41017(14) 0.05438(16) 0.08559(6) 0.0586(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rb1 0.0435(3) 0.0435(3) 0.1210(8) 0.000 0.000 0.02174(15) Rb2 0.0440(3) 0.0440(3) 0.1071(7) 0.000 0.000 0.02200(15) C1 0.039(3) 0.051(3) 0.101(4) 0.023(3) 0.011(3) 0.024(2) C2 0.032(2) 0.038(2) 0.093(4) -0.012(2) -0.002(2) 0.0119(19) C3 0.029(2) 0.032(2) 0.089(3) 0.002(2) 0.010(2) 0.0112(17) C4 0.030(2) 0.044(2) 0.080(3) -0.012(2) -0.010(2) 0.013(2) C5 0.049(3) 0.049(3) 0.111(4) 0.020(3) 0.021(3) 0.029(2) C6 0.032(2) 0.064(3) 0.083(3) -0.009(3) 0.000(2) 0.024(2) C7 0.040(3) 0.044(3) 0.125(5) 0.038(3) 0.021(3) 0.023(2) C8 0.033(2) 0.032(2) 0.103(4) 0.012(2) 0.017(2) 0.0186(18) C9 0.033(2) 0.033(2) 0.067(3) 0.0023(19) -0.0004(19) 0.0118(17) C10 0.032(2) 0.032(2) 0.075(3) -0.003(2) 0.008(2) 0.0115(18) C11 0.042(3) 0.051(3) 0.117(4) -0.007(3) -0.009(3) 0.031(2) C12 0.034(2) 0.052(3) 0.068(3) 0.011(2) 0.008(2) 0.021(2) C13 0.028(2) 0.053(3) 0.076(3) 0.001(2) -0.010(2) 0.023(2) C14 0.039(2) 0.054(3) 0.067(3) 0.010(2) 0.001(2) 0.024(2) C15 0.045(2) 0.056(3) 0.055(3) 0.006(2) 0.000(2) 0.021(2) C16 0.047(3) 0.056(3) 0.051(3) 0.001(2) 0.005(2) 0.029(2) C17 0.036(2) 0.058(3) 0.078(3) -0.008(2) -0.017(2) 0.024(2) C18 0.037(2) 0.046(2) 0.067(3) 0.004(2) 0.007(2) 0.0192(19) C19 0.033(2) 0.049(3) 0.058(3) -0.014(2) -0.017(2) 0.016(2) C20 0.042(2) 0.048(2) 0.052(3) -0.0030(19) -0.0048(19) 0.022(2) C21 0.037(2) 0.043(2) 0.074(3) -0.009(2) -0.001(2) 0.020(2) C22 0.040(2) 0.055(3) 0.057(3) -0.004(2) 0.005(2) 0.026(2) C23 0.023(2) 0.050(3) 0.099(4) -0.015(3) -0.010(2) 0.0114(19) C24 0.050(3) 0.054(3) 0.085(3) 0.004(2) 0.006(2) 0.037(2) N1 0.0293(17) 0.050(2) 0.082(3) 0.0207(19) 0.0119(18) 0.0199(16) N2 0.038(2) 0.050(2) 0.081(3) 0.0182(19) 0.0141(18) 0.0254(17) N3 0.0289(17) 0.045(2) 0.076(3) -0.0040(18) -0.0030(17) 0.0177(16) N4 0.0392(19) 0.049(2) 0.068(2) -0.0078(18) 0.0017(17) 0.0240(17) N5 0.037(2) 0.050(2) 0.090(3) 0.010(2) 0.0125(19) 0.0252(18) N6 0.0318(19) 0.041(2) 0.112(3) -0.008(2) 0.002(2) 0.0167(17) N7 0.0318(17) 0.0370(18) 0.080(2) -0.0068(17) -0.0043(17) 0.0183(15) N8 0.0402(19) 0.0397(19) 0.063(2) 0.0025(16) -0.0004(17) 0.0230(16) N9 0.0384(19) 0.039(2) 0.100(3) 0.0022(19) -0.0082(19) 0.0206(17) N10 0.0308(18) 0.047(2) 0.075(2) -0.0018(18) -0.0045(16) 0.0191(16) N11 0.0379(19) 0.044(2) 0.070(2) 0.0035(17) 0.0010(17) 0.0203(17) N12 0.0300(17) 0.0435(19) 0.068(2) 0.0051(17) 0.0013(16) 0.0155(16) N13 0.0305(18) 0.049(2) 0.072(2) 0.0004(18) -0.0042(17) 0.0179(16) N14 0.0327(18) 0.043(2) 0.080(3) -0.0086(18) -0.0038(17) 0.0138(16) N15 0.0325(18) 0.047(2) 0.066(2) 0.0028(17) -0.0030(16) 0.0198(16) N16 0.0337(19) 0.049(2) 0.065(2) -0.0007(17) -0.0007(16) 0.0178(17) O1 0.0311(18) 0.100(3) 0.133(3) 0.052(2) 0.0092(19) 0.0250(18) O2 0.0357(18) 0.061(2) 0.140(3) 0.020(2) 0.0176(19) 0.0205(16) O3 0.0367(17) 0.0553(19) 0.116(3) -0.0098(18) -0.0007(17) 0.0223(15) O4 0.0352(16) 0.061(2) 0.105(3) -0.0057(18) 0.0017(16) 0.0265(15) O5 0.0537(19) 0.074(2) 0.087(2) -0.0149(18) -0.0086(16) 0.0446(18) O6 0.0519(18) 0.070(2) 0.079(2) -0.0091(17) -0.0014(15) 0.0439(17) O7 0.0357(15) 0.0586(18) 0.084(2) -0.0092(16) -0.0111(15) 0.0275(15) O8 0.0381(16) 0.068(2) 0.075(2) 0.0091(16) -0.0022(15) 0.0304(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 Rb1 3.591(10) . ? O1W Rb1 3.06(3) 13 ? O1W Rb2 3.19(3) . ? Rb1 O5 2.857(3) 13 ? Rb1 O5 2.857(3) 14_455 ? Rb1 O5 2.857(3) 15_445 ? Rb1 O4 2.907(3) 2 ? Rb1 O4 2.907(3) 3 ? Rb1 O4 2.907(3) . ? Rb1 O1W 3.06(3) 13 ? Rb2 O6 2.845(3) 3_665 ? Rb2 O6 2.845(3) 2_655 ? Rb2 O6 2.845(3) . ? Rb2 O7 2.949(3) 2_655 ? Rb2 O7 2.949(3) 3_665 ? Rb2 O7 2.949(3) . ? C1 O1 1.237(5) . ? C1 N1 1.337(6) . ? C1 N2 1.370(6) . ? C2 N3 1.457(5) . ? C2 N1 1.466(5) . ? C2 C3 1.541(7) . ? C2 H2 0.9800 . ? C3 N2 1.442(5) . ? C3 N4 1.450(5) . ? C3 H3 0.9800 . ? C4 O5 1.219(5) . ? C4 N4 1.338(6) . ? C4 N3 1.387(6) . ? C5 N5 1.424(6) . ? C5 N2 1.434(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N7 1.401(5) . ? C6 N4 1.488(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 O2 1.240(5) . ? C7 N6 1.348(7) . ? C7 N5 1.390(7) . ? C8 N5 1.462(5) . ? C8 N7 1.475(5) . ? C8 C9 1.508(7) . ? C8 H8 0.9800 . ? C9 N6 1.447(5) . ? C9 N8 1.461(5) . ? C9 H9 0.9800 . ? C10 O6 1.242(5) . ? C10 N8 1.337(5) . ? C10 N7 1.376(5) . ? C11 N6 1.450(6) . ? C11 N9 1.451(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N8 1.414(5) . ? C12 N11 1.424(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 O3 1.227(5) . ? C13 N10 1.345(5) . ? C13 N9 1.374(5) . ? C14 N9 1.444(6) . ? C14 N11 1.464(5) . ? C14 C15 1.541(6) . ? C14 H14 0.9800 . ? C15 N12 1.442(5) . ? C15 N10 1.473(5) . ? C15 H15 0.9800 . ? C16 O7 1.228(5) . ? C16 N11 1.375(5) . ? C16 N12 1.376(5) . ? C17 N10 1.450(5) . ? C17 N13 1.457(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 N12 1.454(5) . ? C18 N15 1.458(5) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 O4 1.226(5) . ? C19 N13 1.354(5) . ? C19 N14 1.378(5) . ? C20 N13 1.440(5) . ? C20 N15 1.443(5) . ? C20 C21 1.542(6) . ? C20 H20 0.9800 . ? C21 N14 1.429(5) . ? C21 N16 1.435(5) . ? C21 H21 0.9800 . ? C22 O8 1.227(5) . ? C22 N16 1.353(5) . ? C22 N15 1.380(5) . ? C23 N3 1.400(6) 13 ? C23 N14 1.458(5) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 N16 1.455(5) . ? C24 N1 1.462(6) 13 ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? N1 C24 1.462(6) 13 ? N3 C23 1.400(6) 13 ? O5 Rb1 2.857(3) 13 ? 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 Rb1 O1W Rb2 180.0 13 . ? O5 Rb1 O5 104.12(8) 13 14_455 ? O5 Rb1 O5 104.12(8) 13 15_445 ? O5 Rb1 O5 104.12(8) 14_455 15_445 ? O5 Rb1 O4 173.94(9) 13 2 ? O5 Rb1 O4 78.42(9) 14_455 2 ? O5 Rb1 O4 80.35(9) 15_445 2 ? O5 Rb1 O4 80.35(9) 13 3 ? O5 Rb1 O4 173.93(9) 14_455 3 ? O5 Rb1 O4 78.42(9) 15_445 3 ? O4 Rb1 O4 96.73(9) 2 3 ? O5 Rb1 O4 78.42(9) 13 . ? O5 Rb1 O4 80.35(9) 14_455 . ? O5 Rb1 O4 173.93(10) 15_445 . ? O4 Rb1 O4 96.73(9) 2 . ? O4 Rb1 O4 96.73(9) 3 . ? O5 Rb1 O1W 65.60(7) 13 13 ? O5 Rb1 O1W 65.60(7) 14_455 13 ? O5 Rb1 O1W 65.60(7) 15_445 13 ? O4 Rb1 O1W 120.34(7) 2 13 ? O4 Rb1 O1W 120.34(7) 3 13 ? O4 Rb1 O1W 120.34(7) . 13 ? O5 Rb1 Cl1 114.40(7) 13 . ? O5 Rb1 Cl1 114.40(7) 14_455 . ? O5 Rb1 Cl1 114.40(7) 15_445 . ? O4 Rb1 Cl1 59.66(7) 2 . ? O4 Rb1 Cl1 59.66(7) 3 . ? O4 Rb1 Cl1 59.66(7) . . ? O1W Rb1 Cl1 180.0 13 . ? O6 Rb2 O6 104.66(8) 3_665 2_655 ? O6 Rb2 O6 104.66(8) 3_665 . ? O6 Rb2 O6 104.66(8) 2_655 . ? O6 Rb2 O7 76.52(9) 3_665 2_655 ? O6 Rb2 O7 75.03(8) 2_655 2_655 ? O6 Rb2 O7 178.83(9) . 2_655 ? O6 Rb2 O7 75.03(8) 3_665 3_665 ? O6 Rb2 O7 178.83(9) 2_655 3_665 ? O6 Rb2 O7 76.52(9) . 3_665 ? O7 Rb2 O7 103.80(7) 2_655 3_665 ? O6 Rb2 O7 178.83(9) 3_665 . ? O6 Rb2 O7 76.52(9) 2_655 . ? O6 Rb2 O7 75.03(8) . . ? O7 Rb2 O7 103.80(7) 2_655 . ? O7 Rb2 O7 103.80(7) 3_665 . ? O6 Rb2 O1W 66.06(7) 3_665 . ? O6 Rb2 O1W 66.06(7) 2_655 . ? O6 Rb2 O1W 66.06(7) . . ? O7 Rb2 O1W 114.68(6) 2_655 . ? O7 Rb2 O1W 114.68(6) 3_665 . ? O7 Rb2 O1W 114.68(6) . . ? O1 C1 N1 127.3(4) . . ? O1 C1 N2 123.5(5) . . ? N1 C1 N2 109.2(4) . . ? N3 C2 N1 113.4(3) . . ? N3 C2 C3 104.3(4) . . ? N1 C2 C3 103.4(4) . . ? N3 C2 H2 111.8 . . ? N1 C2 H2 111.8 . . ? C3 C2 H2 111.8 . . ? N2 C3 N4 113.7(4) . . ? N2 C3 C2 102.8(3) . . ? N4 C3 C2 102.0(3) . . ? N2 C3 H3 112.5 . . ? N4 C3 H3 112.5 . . ? C2 C3 H3 112.5 . . ? O5 C4 N4 128.1(5) . . ? O5 C4 N3 123.5(4) . . ? N4 C4 N3 108.4(4) . . ? N5 C5 N2 113.9(4) . . ? N5 C5 H5A 108.8 . . ? N2 C5 H5A 108.8 . . ? N5 C5 H5B 108.8 . . ? N2 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? N7 C6 N4 112.9(3) . . ? N7 C6 H6A 109.0 . . ? N4 C6 H6A 109.0 . . ? N7 C6 H6B 109.0 . . ? N4 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? O2 C7 N6 126.9(5) . . ? O2 C7 N5 124.2(5) . . ? N6 C7 N5 108.8(4) . . ? N5 C8 N7 112.2(3) . . ? N5 C8 C9 104.1(3) . . ? N7 C8 C9 104.1(3) . . ? N5 C8 H8 112.0 . . ? N7 C8 H8 112.0 . . ? C9 C8 H8 112.0 . . ? N6 C9 N8 114.1(3) . . ? N6 C9 C8 104.4(3) . . ? N8 C9 C8 104.4(3) . . ? N6 C9 H9 111.2 . . ? N8 C9 H9 111.2 . . ? C8 C9 H9 111.2 . . ? O6 C10 N8 125.9(4) . . ? O6 C10 N7 123.1(4) . . ? N8 C10 N7 111.0(4) . . ? N6 C11 N9 112.4(4) . . ? N6 C11 H11A 109.1 . . ? N9 C11 H11A 109.1 . . ? N6 C11 H11B 109.1 . . ? N9 C11 H11B 109.1 . . ? H11A C11 H11B 107.9 . . ? N8 C12 N11 114.6(3) . . ? N8 C12 H12A 108.6 . . ? N11 C12 H12A 108.6 . . ? N8 C12 H12B 108.6 . . ? N11 C12 H12B 108.6 . . ? H12A C12 H12B 107.6 . . ? O3 C13 N10 126.3(4) . . ? O3 C13 N9 124.6(4) . . ? N10 C13 N9 109.1(4) . . ? N9 C14 N11 113.9(4) . . ? N9 C14 C15 103.9(3) . . ? N11 C14 C15 103.3(3) . . ? N9 C14 H14 111.7 . . ? N11 C14 H14 111.7 . . ? C15 C14 H14 111.7 . . ? N12 C15 N10 113.4(3) . . ? N12 C15 C14 104.2(3) . . ? N10 C15 C14 102.8(3) . . ? N12 C15 H15 112.0 . . ? N10 C15 H15 112.0 . . ? C14 C15 H15 112.0 . . ? O7 C16 N11 125.3(4) . . ? O7 C16 N12 126.1(4) . . ? N11 C16 N12 108.5(4) . . ? N10 C17 N13 113.3(3) . . ? N10 C17 H17A 108.9 . . ? N13 C17 H17A 108.9 . . ? N10 C17 H17B 108.9 . . ? N13 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? N12 C18 N15 112.4(3) . . ? N12 C18 H18A 109.1 . . ? N15 C18 H18A 109.1 . . ? N12 C18 H18B 109.1 . . ? N15 C18 H18B 109.1 . . ? H18A C18 H18B 107.9 . . ? O4 C19 N13 126.7(4) . . ? O4 C19 N14 125.1(4) . . ? N13 C19 N14 108.2(4) . . ? N13 C20 N15 115.3(3) . . ? N13 C20 C21 103.2(3) . . ? N15 C20 C21 103.8(3) . . ? N13 C20 H20 111.3 . . ? N15 C20 H20 111.3 . . ? C21 C20 H20 111.3 . . ? N14 C21 N16 116.2(4) . . ? N14 C21 C20 103.8(3) . . ? N16 C21 C20 103.0(3) . . ? N14 C21 H21 111.1 . . ? N16 C21 H21 111.1 . . ? C20 C21 H21 111.1 . . ? O8 C22 N16 127.3(4) . . ? O8 C22 N15 124.6(4) . . ? N16 C22 N15 108.1(3) . . ? N3 C23 N14 114.4(3) 13 . ? N3 C23 H23A 108.6 13 . ? N14 C23 H23A 108.6 . . ? N3 C23 H23B 108.6 13 . ? N14 C23 H23B 108.6 . . ? H23A C23 H23B 107.6 . . ? N16 C24 N1 113.6(3) . 13 ? N16 C24 H24A 108.9 . . ? N1 C24 H24A 108.9 13 . ? N16 C24 H24B 108.9 . . ? N1 C24 H24B 108.9 13 . ? H24A C24 H24B 107.7 . . ? C1 N1 C24 121.9(3) . 13 ? C1 N1 C2 111.5(4) . . ? C24 N1 C2 121.9(4) 13 . ? C1 N2 C5 123.6(4) . . ? C1 N2 C3 112.4(4) . . ? C5 N2 C3 122.6(3) . . ? C4 N3 C23 124.0(4) . 13 ? C4 N3 C2 110.6(4) . . ? C23 N3 C2 124.4(4) 13 . ? C4 N4 C3 113.8(4) . . ? C4 N4 C6 122.0(4) . . ? C3 N4 C6 118.9(4) . . ? C7 N5 C5 123.4(4) . . ? C7 N5 C8 110.3(4) . . ? C5 N5 C8 124.5(4) . . ? C7 N6 C9 112.0(4) . . ? C7 N6 C11 122.7(4) . . ? C9 N6 C11 123.3(4) . . ? C10 N7 C6 123.8(3) . . ? C10 N7 C8 109.0(4) . . ? C6 N7 C8 122.0(3) . . ? C10 N8 C12 124.0(3) . . ? C10 N8 C9 110.8(3) . . ? C12 N8 C9 123.2(3) . . ? C13 N9 C14 111.9(4) . . ? C13 N9 C11 122.0(4) . . ? C14 N9 C11 122.8(4) . . ? C13 N10 C17 123.0(3) . . ? C13 N10 C15 112.1(3) . . ? C17 N10 C15 120.8(4) . . ? C16 N11 C12 124.4(3) . . ? C16 N11 C14 111.6(3) . . ? C12 N11 C14 123.5(3) . . ? C16 N12 C15 112.0(3) . . ? C16 N12 C18 121.0(3) . . ? C15 N12 C18 122.7(3) . . ? C19 N13 C20 112.5(3) . . ? C19 N13 C17 122.0(3) . . ? C20 N13 C17 120.9(4) . . ? C19 N14 C21 112.0(3) . . ? C19 N14 C23 123.8(4) . . ? C21 N14 C23 122.6(3) . . ? C22 N15 C20 111.6(3) . . ? C22 N15 C18 121.7(3) . . ? C20 N15 C18 123.7(3) . . ? C22 N16 C21 113.3(3) . . ? C22 N16 C24 121.5(4) . . ? C21 N16 C24 122.2(3) . . ? C19 O4 Rb1 145.9(3) . . ? C4 O5 Rb1 148.6(3) . 13 ? C10 O6 Rb2 146.4(3) . . ? C16 O7 Rb2 145.4(3) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.036 _refine_diff_density_min -0.622 _refine_diff_density_rms 0.082 # 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 -0.046 0.324 -0.001 6650 3091 ' ' 2 -0.167 0.167 0.167 354 111 ' ' 3 0.000 0.500 0.500 353 112 ' ' 4 0.167 0.833 0.833 354 111 ' ' 5 0.167 0.333 0.833 354 113 ' ' 6 0.333 0.167 0.167 354 112 ' ' 7 0.500 0.500 0.500 352 111 ' ' 8 0.500 0.000 0.500 352 112 ' ' 9 0.667 0.833 0.833 354 112 ' ' 10 0.833 0.667 0.167 354 113 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 931657' ####################################################################### # # 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_p _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H212 Cl2 N48 O94 Rb2' _chemical_formula_weight 3496.74 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 21.755(5) _cell_length_b 21.755(5) _cell_length_c 52.173(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 21384(8) _cell_formula_units_Z 6 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 11040 _exptl_absorpt_coefficient_mu 0.856 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8018 _exptl_absorpt_correction_T_max 0.8542 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 82645 _diffrn_reflns_av_R_equivalents 0.1111 _diffrn_reflns_av_sigmaI/netI 0.0793 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -56 _diffrn_reflns_limit_l_max 63 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 25.99 _reflns_number_total 9328 _reflns_number_gt 4782 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1144P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9328 _refine_ls_number_parameters 452 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1237 _refine_ls_R_factor_gt 0.0654 _refine_ls_wR_factor_ref 0.1966 _refine_ls_wR_factor_gt 0.1793 _refine_ls_goodness_of_fit_ref 0.906 _refine_ls_restrained_S_all 0.906 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 1.3333 0.6667 0.1242(2) 0.404(6) Uiso 1 3 d S . . Cl2 Cl 0.9965(6) 0.3004(7) 0.1503(2) 0.178(5) Uiso 0.247(6) 1 d P A 1 Cl2' Cl 1.0021(9) 0.3406(10) 0.1654(4) 0.108(9) Uiso 0.086(6) 1 d P A 2 O1W O 0.6667 0.3333 0.0060(3) 0.249(6) Uiso 1 3 d S . . Rb1 Rb 0.6667 0.3333 0.066431(16) 0.0695(3) Uani 1 3 d S . . Rb2 Rb 1.3333 0.6667 0.052559(18) 0.0792(3) Uani 1 3 d S . . C1 C 0.9363(2) 0.7189(2) -0.03301(11) 0.0754(13) Uani 1 1 d . . . C2 C 0.83113(19) 0.64518(19) -0.05377(9) 0.0632(11) Uani 1 1 d . . . H2 H 0.8136 0.6657 -0.0666 0.076 Uiso 1 1 calc R . . C3 C 0.81351(18) 0.65733(19) -0.02680(10) 0.0679(13) Uani 1 1 d . . . H3 H 0.7825 0.6779 -0.0267 0.081 Uiso 1 1 calc R . . C4 C 0.76487(18) 0.5358(2) -0.03356(9) 0.0608(11) Uani 1 1 d . . . C5 C 0.8928(2) 0.7452(2) 0.00795(11) 0.0851(15) Uani 1 1 d . . . H5A H 0.9399 0.7868 0.0079 0.102 Uiso 1 1 calc R . . H5B H 0.8587 0.7615 0.0083 0.102 Uiso 1 1 calc R . . C6 C 0.7384(2) 0.5704(2) 0.00816(10) 0.0754(13) Uani 1 1 d . . . H6A H 0.7144 0.5979 0.0087 0.090 Uiso 1 1 calc R . . H6B H 0.7023 0.5206 0.0084 0.090 Uiso 1 1 calc R . . C7 C 0.9402(2) 0.7228(2) 0.04604(11) 0.0789(14) Uani 1 1 d . . . C8 C 0.81685(19) 0.65660(18) 0.04240(10) 0.0675(13) Uani 1 1 d . . . H8 H 0.7853 0.6766 0.0431 0.081 Uiso 1 1 calc R . . C9 C 0.83674(19) 0.64405(19) 0.06905(9) 0.0630(11) Uani 1 1 d . . . H9 H 0.8179 0.6618 0.0824 0.076 Uiso 1 1 calc R . . C10 C 0.77115(19) 0.5366(2) 0.04843(9) 0.0633(11) Uani 1 1 d . . . C11 C 0.9570(2) 0.6948(2) 0.09079(10) 0.0799(13) Uani 1 1 d . . . H11A H 0.9353 0.7046 0.1053 0.096 Uiso 1 1 calc R . . H11B H 1.0033 0.7362 0.0880 0.096 Uiso 1 1 calc R . . C12 C 0.79629(19) 0.5316(2) 0.09376(9) 0.0669(11) Uani 1 1 d . . . H12A H 0.7542 0.4850 0.0923 0.080 Uiso 1 1 calc R . . H12B H 0.7879 0.5570 0.1073 0.080 Uiso 1 1 calc R . . C13 C 1.0305(2) 0.6389(2) 0.09538(9) 0.0669(11) Uani 1 1 d . . . C14 C 0.9181(2) 0.5789(2) 0.11379(9) 0.0704(12) Uani 1 1 d . . . H14 H 0.9057 0.5968 0.1290 0.084 Uiso 1 1 calc R . . C15 C 0.9592(2) 0.5401(2) 0.12046(8) 0.0627(10) Uani 1 1 d . . . H15 H 0.9655 0.5389 0.1390 0.075 Uiso 1 1 calc R . . C16 C 0.8558(2) 0.4610(2) 0.09950(8) 0.0581(10) Uani 1 1 d . . . C17 C 1.09154(19) 0.5824(2) 0.11513(9) 0.0701(12) Uani 1 1 d . . . H17A H 1.1331 0.6269 0.1103 0.084 Uiso 1 1 calc R . . H17B H 1.0914 0.5788 0.1337 0.084 Uiso 1 1 calc R . . C18 C 0.9280(2) 0.4107(2) 0.11753(9) 0.0674(11) Uani 1 1 d . . . H18A H 0.9343 0.4113 0.1360 0.081 Uiso 1 1 calc R . . H18B H 0.8853 0.3666 0.1132 0.081 Uiso 1 1 calc R . . C19 C 1.1557(2) 0.5372(2) 0.09045(8) 0.0624(10) Uani 1 1 d . . . C20 C 1.05945(19) 0.45497(19) 0.11477(8) 0.0611(10) Uani 1 1 d . . . H20 H 1.0615 0.4553 0.1335 0.073 Uiso 1 1 calc R . . C21 C 1.09824(19) 0.4173(2) 0.10256(9) 0.0638(11) Uani 1 1 d . . . H21 H 1.1157 0.3979 0.1158 0.077 Uiso 1 1 calc R . . C22 C 0.9796(2) 0.3576(2) 0.08976(8) 0.0577(10) Uani 1 1 d . . . C23 C 1.21445(19) 0.4671(2) 0.08024(10) 0.0761(13) Uani 1 1 d . . . H23A H 1.2246 0.4412 0.0931 0.091 Uiso 1 1 calc R . . H23B H 1.2558 0.5141 0.0789 0.091 Uiso 1 1 calc R . . C24 C 1.0505(2) 0.3033(2) 0.07792(10) 0.0745(12) Uani 1 1 d . . . H24A H 1.0035 0.2633 0.0748 0.089 Uiso 1 1 calc R . . H24B H 1.0728 0.2892 0.0910 0.089 Uiso 1 1 calc R . . N1 N 0.90751(16) 0.67991(17) -0.05401(7) 0.0649(9) Uani 1 1 d . . . N2 N 0.88300(16) 0.70526(16) -0.01588(7) 0.0644(9) Uani 1 1 d . . . N3 N 0.79565(16) 0.56825(17) -0.05610(8) 0.0633(9) Uani 1 1 d . . . N4 N 0.77887(15) 0.58603(16) -0.01588(7) 0.0618(9) Uani 1 1 d . . . N5 N 0.88477(17) 0.70553(16) 0.03051(8) 0.0667(9) Uani 1 1 d . . . N6 N 0.91392(17) 0.68353(17) 0.06851(9) 0.0750(11) Uani 1 1 d . . . N7 N 0.78213(15) 0.58624(15) 0.03051(7) 0.0617(9) Uani 1 1 d . . . N8 N 0.80613(16) 0.56828(15) 0.07054(7) 0.0585(8) Uani 1 1 d . . . N9 N 0.96611(16) 0.63501(15) 0.09700(7) 0.0654(9) Uani 1 1 d . . . N10 N 1.02869(15) 0.58421(16) 0.10724(7) 0.0662(9) Uani 1 1 d . . . N11 N 0.85615(15) 0.52286(16) 0.10092(6) 0.0602(8) Uani 1 1 d . . . N12 N 0.91805(15) 0.47071(16) 0.11029(7) 0.0624(9) Uani 1 1 d . . . N13 N 1.09709(16) 0.52519(16) 0.10426(7) 0.0650(9) Uani 1 1 d . . . N14 N 1.15576(16) 0.47411(16) 0.08891(7) 0.0653(9) Uani 1 1 d . . . N15 N 0.98725(15) 0.41208(16) 0.10527(6) 0.0597(8) Uani 1 1 d . . . N16 N 1.04373(16) 0.36235(16) 0.08757(6) 0.0606(8) Uani 1 1 d . . . O1 O 0.99850(15) 0.75875(18) -0.02850(8) 0.1114(14) Uani 1 1 d . . . O2 O 1.00204(15) 0.76654(16) 0.04256(8) 0.1036(12) Uani 1 1 d . . . O3 O 1.08116(15) 0.68545(15) 0.08323(7) 0.0863(9) Uani 1 1 d . . . O4 O 1.20029(14) 0.59338(14) 0.08122(6) 0.0761(8) Uani 1 1 d . . . O5 O 0.73143(15) 0.47190(14) -0.03081(6) 0.0793(9) Uani 1 1 d . . . O6 O 0.73749(14) 0.47188(13) 0.04433(6) 0.0741(8) Uani 1 1 d . . . O7 O 0.80889(13) 0.40550(14) 0.09025(6) 0.0698(8) Uani 1 1 d . . . O8 O 0.92358(14) 0.31211(14) 0.08066(6) 0.0745(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rb1 0.0444(2) 0.0444(2) 0.1196(7) 0.000 0.000 0.02220(12) Rb2 0.0504(3) 0.0504(3) 0.1370(8) 0.000 0.000 0.02519(13) C1 0.050(2) 0.053(2) 0.116(4) -0.003(3) 0.013(3) 0.020(2) C2 0.047(2) 0.048(2) 0.095(3) 0.012(2) 0.005(2) 0.0244(17) C3 0.0382(19) 0.044(2) 0.119(4) 0.014(2) 0.019(2) 0.0187(16) C4 0.0336(18) 0.049(2) 0.093(3) 0.006(2) -0.005(2) 0.0149(17) C5 0.073(3) 0.040(2) 0.132(5) -0.002(3) 0.026(3) 0.020(2) C6 0.042(2) 0.058(2) 0.117(4) 0.020(3) 0.010(3) 0.0190(18) C7 0.055(3) 0.050(2) 0.131(4) -0.010(3) 0.021(3) 0.026(2) C8 0.045(2) 0.0368(18) 0.120(4) -0.002(2) 0.016(2) 0.0194(16) C9 0.050(2) 0.047(2) 0.095(3) -0.002(2) -0.004(2) 0.0267(18) C10 0.046(2) 0.050(2) 0.093(3) 0.015(2) 0.019(2) 0.0229(18) C11 0.057(2) 0.048(2) 0.122(4) -0.002(2) -0.011(3) 0.0167(19) C12 0.045(2) 0.061(2) 0.085(3) -0.002(2) 0.000(2) 0.0191(18) C13 0.039(2) 0.059(2) 0.087(3) -0.010(2) -0.005(2) 0.0123(19) C14 0.056(2) 0.069(3) 0.078(3) -0.017(2) 0.001(2) 0.026(2) C15 0.056(2) 0.070(3) 0.064(3) -0.011(2) -0.004(2) 0.033(2) C16 0.049(2) 0.051(2) 0.067(3) -0.002(2) 0.005(2) 0.0199(19) C17 0.042(2) 0.062(2) 0.098(3) -0.012(2) -0.019(2) 0.0199(18) C18 0.048(2) 0.061(2) 0.085(3) 0.009(2) 0.014(2) 0.0212(19) C19 0.044(2) 0.061(2) 0.079(3) 0.001(2) -0.009(2) 0.0230(19) C20 0.052(2) 0.056(2) 0.068(3) 0.009(2) -0.0023(19) 0.0215(18) C21 0.043(2) 0.056(2) 0.086(3) 0.014(2) 0.002(2) 0.0193(18) C22 0.048(2) 0.055(2) 0.057(3) 0.004(2) 0.0060(19) 0.0162(19) C23 0.036(2) 0.063(2) 0.126(4) -0.001(3) -0.017(2) 0.0224(18) C24 0.054(2) 0.047(2) 0.105(4) 0.003(2) -0.001(2) 0.0123(18) N1 0.0423(17) 0.0536(18) 0.088(3) -0.0063(19) 0.0096(18) 0.0157(15) N2 0.0510(18) 0.0523(18) 0.087(3) -0.0012(18) 0.0155(18) 0.0233(15) N3 0.0451(17) 0.0510(18) 0.088(3) 0.004(2) -0.0075(18) 0.0198(15) N4 0.0473(17) 0.0473(18) 0.081(2) 0.0077(18) -0.0004(18) 0.0164(14) N5 0.0488(19) 0.0463(17) 0.096(3) 0.0045(19) 0.0133(19) 0.0170(15) N6 0.0441(18) 0.0540(19) 0.125(3) 0.011(2) 0.002(2) 0.0235(16) N7 0.0451(17) 0.0435(17) 0.086(2) -0.0008(18) -0.0070(17) 0.0140(14) N8 0.0524(18) 0.0450(17) 0.072(2) -0.0019(18) 0.0050(18) 0.0199(14) N9 0.0450(17) 0.0425(16) 0.105(3) -0.0033(18) 0.0001(18) 0.0193(14) N10 0.0441(17) 0.0479(18) 0.095(3) 0.0000(18) -0.0070(17) 0.0140(15) N11 0.0426(16) 0.0553(18) 0.077(2) 0.0009(17) 0.0049(16) 0.0199(14) N12 0.0404(16) 0.0544(18) 0.082(2) 0.0008(17) -0.0024(16) 0.0158(14) N13 0.0434(17) 0.0518(18) 0.091(3) -0.0070(18) -0.0109(17) 0.0167(14) N14 0.0491(18) 0.0542(19) 0.083(2) 0.0080(17) -0.0022(17) 0.0186(15) N15 0.0485(17) 0.0507(17) 0.073(2) -0.0055(17) -0.0057(16) 0.0194(14) N16 0.0475(18) 0.0550(18) 0.067(2) -0.0085(16) -0.0004(16) 0.0166(15) O1 0.0440(17) 0.085(2) 0.158(3) -0.050(2) 0.0209(19) -0.0028(15) O2 0.0445(16) 0.0643(18) 0.182(4) 0.001(2) 0.029(2) 0.0119(14) O3 0.0525(16) 0.0551(16) 0.137(3) 0.0106(18) -0.0017(18) 0.0167(14) O4 0.0488(15) 0.0526(16) 0.113(2) 0.0114(16) 0.0035(16) 0.0153(13) O5 0.0654(17) 0.0494(16) 0.102(2) 0.0058(16) -0.0037(16) 0.0127(14) O6 0.0644(16) 0.0377(14) 0.102(2) 0.0046(14) -0.0033(16) 0.0121(12) O7 0.0487(15) 0.0562(16) 0.093(2) -0.0006(15) -0.0063(14) 0.0173(13) O8 0.0552(16) 0.0618(17) 0.087(2) -0.0127(15) 0.0022(15) 0.0149(14) _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 Cl1 Rb2 3.737(12) . ? O1W Rb2 3.056(15) 10_765 ? O1W Rb1 3.152(14) . ? Rb1 O6 2.854(3) 3_665 ? Rb1 O6 2.854(3) 2_655 ? Rb1 O6 2.854(3) . ? Rb1 O7 2.954(3) . ? Rb1 O7 2.954(3) 3_665 ? Rb1 O7 2.954(3) 2_655 ? Rb2 O5 2.848(3) 12_655 ? Rb2 O5 2.848(3) 11_665 ? Rb2 O5 2.848(3) 10_765 ? Rb2 O4 2.923(3) 3_775 ? Rb2 O4 2.923(3) . ? Rb2 O4 2.923(3) 2_755 ? Rb2 O1W 3.056(15) 10_765 ? C1 O1 1.211(5) . ? C1 N1 1.334(6) . ? C1 N2 1.374(5) . ? C2 N1 1.441(5) . ? C2 N3 1.456(5) . ? C2 C3 1.516(6) . ? C2 H2 0.9800 . ? C3 N2 1.456(5) . ? C3 N4 1.459(5) . ? C3 H3 0.9800 . ? C4 O5 1.213(4) . ? C4 N4 1.344(5) . ? C4 N3 1.363(5) . ? C5 N5 1.417(6) . ? C5 N2 1.470(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N7 1.434(5) . ? C6 N4 1.472(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 O2 1.212(5) . ? C7 N5 1.341(6) . ? C7 N6 1.393(6) . ? C8 N5 1.459(5) . ? C8 N7 1.464(5) . ? C8 C9 1.521(6) . ? C8 H8 0.9800 . ? C9 N8 1.438(5) . ? C9 N6 1.454(5) . ? C9 H9 0.9800 . ? C10 O6 1.237(4) . ? C10 N7 1.357(5) . ? C10 N8 1.364(5) . ? C11 N6 1.435(6) . ? C11 N9 1.447(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N8 1.408(5) . ? C12 N11 1.455(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 O3 1.235(5) . ? C13 N10 1.324(5) . ? C13 N9 1.364(5) . ? C14 N9 1.440(5) . ? C14 N11 1.453(5) . ? C14 C15 1.547(6) . ? C14 H14 0.9800 . ? C15 N12 1.418(5) . ? C15 N10 1.493(5) . ? C15 H15 0.9800 . ? C16 O7 1.225(4) . ? C16 N11 1.345(5) . ? C16 N12 1.381(5) . ? C17 N13 1.428(5) . ? C17 N10 1.447(5) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 N15 1.426(5) . ? C18 N12 1.475(5) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 O4 1.217(5) . ? C19 N13 1.371(5) . ? C19 N14 1.375(5) . ? C20 N13 1.433(5) . ? C20 N15 1.455(5) . ? C20 C21 1.575(6) . ? C20 H20 0.9800 . ? C21 N16 1.425(5) . ? C21 N14 1.433(5) . ? C21 H21 0.9800 . ? C22 O8 1.219(4) . ? C22 N16 1.351(5) . ? C22 N15 1.375(5) . ? C23 N14 1.433(5) . ? C23 N3 1.434(6) 10_765 ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 N16 1.454(5) . ? C24 N1 1.480(6) 10_765 ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? N1 C24 1.480(6) 10_765 ? N3 C23 1.434(6) 10_765 ? O5 Rb2 2.848(3) 10_765 ? 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 Rb2 O1W Rb1 180.0 10_765 . ? O6 Rb1 O6 104.77(7) 3_665 2_655 ? O6 Rb1 O6 104.77(7) 3_665 . ? O6 Rb1 O6 104.77(7) 2_655 . ? O6 Rb1 O7 76.74(8) 3_665 . ? O6 Rb1 O7 178.47(8) 2_655 . ? O6 Rb1 O7 74.92(8) . . ? O6 Rb1 O7 74.92(8) 3_665 3_665 ? O6 Rb1 O7 76.74(8) 2_655 3_665 ? O6 Rb1 O7 178.47(8) . 3_665 ? O7 Rb1 O7 103.56(7) . 3_665 ? O6 Rb1 O7 178.47(8) 3_665 2_655 ? O6 Rb1 O7 74.92(8) 2_655 2_655 ? O6 Rb1 O7 76.74(8) . 2_655 ? O7 Rb1 O7 103.56(7) . 2_655 ? O7 Rb1 O7 103.56(7) 3_665 2_655 ? O6 Rb1 O1W 66.16(6) 3_665 . ? O6 Rb1 O1W 66.16(6) 2_655 . ? O6 Rb1 O1W 66.16(6) . . ? O7 Rb1 O1W 114.88(6) . . ? O7 Rb1 O1W 114.88(6) 3_665 . ? O7 Rb1 O1W 114.88(6) 2_655 . ? O5 Rb2 O5 105.18(7) 12_655 11_665 ? O5 Rb2 O5 105.18(7) 12_655 10_765 ? O5 Rb2 O5 105.18(7) 11_665 10_765 ? O5 Rb2 O4 78.21(8) 12_655 3_775 ? O5 Rb2 O4 79.88(8) 11_665 3_775 ? O5 Rb2 O4 172.62(9) 10_765 3_775 ? O5 Rb2 O4 79.88(8) 12_655 . ? O5 Rb2 O4 172.62(9) 11_665 . ? O5 Rb2 O4 78.21(8) 10_765 . ? O4 Rb2 O4 96.15(8) 3_775 . ? O5 Rb2 O4 172.62(9) 12_655 2_755 ? O5 Rb2 O4 78.21(8) 11_665 2_755 ? O5 Rb2 O4 79.88(8) 10_765 2_755 ? O4 Rb2 O4 96.15(8) 3_775 2_755 ? O4 Rb2 O4 96.15(8) . 2_755 ? O5 Rb2 O1W 66.52(6) 12_655 10_765 ? O5 Rb2 O1W 66.52(6) 11_665 10_765 ? O5 Rb2 O1W 66.52(6) 10_765 10_765 ? O4 Rb2 O1W 120.78(6) 3_775 10_765 ? O4 Rb2 O1W 120.78(6) . 10_765 ? O4 Rb2 O1W 120.78(6) 2_755 10_765 ? O5 Rb2 Cl1 113.48(6) 12_655 . ? O5 Rb2 Cl1 113.48(6) 11_665 . ? O5 Rb2 Cl1 113.48(6) 10_765 . ? O4 Rb2 Cl1 59.22(6) 3_775 . ? O4 Rb2 Cl1 59.22(6) . . ? O4 Rb2 Cl1 59.22(6) 2_755 . ? O1W Rb2 Cl1 180.000(1) 10_765 . ? O1 C1 N1 128.1(4) . . ? O1 C1 N2 123.3(5) . . ? N1 C1 N2 108.7(4) . . ? N1 C2 N3 114.3(3) . . ? N1 C2 C3 104.0(3) . . ? N3 C2 C3 104.1(3) . . ? N1 C2 H2 111.3 . . ? N3 C2 H2 111.3 . . ? C3 C2 H2 111.3 . . ? N2 C3 N4 114.1(3) . . ? N2 C3 C2 103.0(3) . . ? N4 C3 C2 102.6(3) . . ? N2 C3 H3 112.1 . . ? N4 C3 H3 112.1 . . ? C2 C3 H3 112.1 . . ? O5 C4 N4 127.8(4) . . ? O5 C4 N3 123.6(4) . . ? N4 C4 N3 108.5(3) . . ? N5 C5 N2 113.9(3) . . ? N5 C5 H5A 108.8 . . ? N2 C5 H5A 108.8 . . ? N5 C5 H5B 108.8 . . ? N2 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? N7 C6 N4 112.9(3) . . ? N7 C6 H6A 109.0 . . ? N4 C6 H6A 109.0 . . ? N7 C6 H6B 109.0 . . ? N4 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? O2 C7 N5 128.2(5) . . ? O2 C7 N6 124.2(5) . . ? N5 C7 N6 107.5(4) . . ? N5 C8 N7 112.8(3) . . ? N5 C8 C9 104.2(3) . . ? N7 C8 C9 104.1(3) . . ? N5 C8 H8 111.8 . . ? N7 C8 H8 111.8 . . ? C9 C8 H8 111.8 . . ? N8 C9 N6 114.5(3) . . ? N8 C9 C8 104.2(3) . . ? N6 C9 C8 103.0(3) . . ? N8 C9 H9 111.6 . . ? N6 C9 H9 111.6 . . ? C8 C9 H9 111.6 . . ? O6 C10 N7 123.7(4) . . ? O6 C10 N8 125.8(4) . . ? N7 C10 N8 110.4(3) . . ? N6 C11 N9 113.5(3) . . ? N6 C11 H11A 108.9 . . ? N9 C11 H11A 108.9 . . ? N6 C11 H11B 108.9 . . ? N9 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? N8 C12 N11 113.8(3) . . ? N8 C12 H12A 108.8 . . ? N11 C12 H12A 108.8 . . ? N8 C12 H12B 108.8 . . ? N11 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? O3 C13 N10 126.2(4) . . ? O3 C13 N9 123.3(4) . . ? N10 C13 N9 110.3(4) . . ? N9 C14 N11 113.9(4) . . ? N9 C14 C15 103.1(3) . . ? N11 C14 C15 101.1(3) . . ? N9 C14 H14 112.6 . . ? N11 C14 H14 112.6 . . ? C15 C14 H14 112.6 . . ? N12 C15 N10 114.1(3) . . ? N12 C15 C14 105.5(3) . . ? N10 C15 C14 102.8(3) . . ? N12 C15 H15 111.3 . . ? N10 C15 H15 111.3 . . ? C14 C15 H15 111.3 . . ? O7 C16 N11 126.3(4) . . ? O7 C16 N12 125.6(4) . . ? N11 C16 N12 108.1(3) . . ? N13 C17 N10 113.8(3) . . ? N13 C17 H17A 108.8 . . ? N10 C17 H17A 108.8 . . ? N13 C17 H17B 108.8 . . ? N10 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? N15 C18 N12 113.4(3) . . ? N15 C18 H18A 108.9 . . ? N12 C18 H18A 108.9 . . ? N15 C18 H18B 108.9 . . ? N12 C18 H18B 108.9 . . ? H18A C18 H18B 107.7 . . ? O4 C19 N13 126.7(4) . . ? O4 C19 N14 125.5(4) . . ? N13 C19 N14 107.8(3) . . ? N13 C20 N15 114.3(3) . . ? N13 C20 C21 103.3(3) . . ? N15 C20 C21 102.5(3) . . ? N13 C20 H20 112.0 . . ? N15 C20 H20 112.0 . . ? C21 C20 H20 112.0 . . ? N16 C21 N14 116.9(4) . . ? N16 C21 C20 102.8(3) . . ? N14 C21 C20 102.5(3) . . ? N16 C21 H21 111.3 . . ? N14 C21 H21 111.3 . . ? C20 C21 H21 111.3 . . ? O8 C22 N16 127.2(4) . . ? O8 C22 N15 124.8(4) . . ? N16 C22 N15 108.0(3) . . ? N14 C23 N3 115.4(3) . 10_765 ? N14 C23 H23A 108.4 . . ? N3 C23 H23A 108.4 10_765 . ? N14 C23 H23B 108.4 . . ? N3 C23 H23B 108.4 10_765 . ? H23A C23 H23B 107.5 . . ? N16 C24 N1 113.4(3) . 10_765 ? N16 C24 H24A 108.9 . . ? N1 C24 H24A 108.9 10_765 . ? N16 C24 H24B 108.9 . . ? N1 C24 H24B 108.9 10_765 . ? H24A C24 H24B 107.7 . . ? C1 N1 C2 112.2(3) . . ? C1 N1 C24 120.0(3) . 10_765 ? C2 N1 C24 123.0(4) . 10_765 ? C1 N2 C3 111.2(4) . . ? C1 N2 C5 124.4(4) . . ? C3 N2 C5 123.1(3) . . ? C4 N3 C23 125.2(3) . 10_765 ? C4 N3 C2 111.4(4) . . ? C23 N3 C2 122.7(4) 10_765 . ? C4 N4 C3 112.5(4) . . ? C4 N4 C6 122.1(3) . . ? C3 N4 C6 120.6(3) . . ? C7 N5 C5 120.8(4) . . ? C7 N5 C8 112.8(4) . . ? C5 N5 C8 124.7(4) . . ? C7 N6 C11 123.0(4) . . ? C7 N6 C9 112.1(4) . . ? C11 N6 C9 123.2(4) . . ? C10 N7 C6 122.5(3) . . ? C10 N7 C8 109.5(4) . . ? C6 N7 C8 121.9(3) . . ? C10 N8 C12 123.6(3) . . ? C10 N8 C9 110.9(3) . . ? C12 N8 C9 123.3(4) . . ? C13 N9 C14 112.2(3) . . ? C13 N9 C11 122.0(3) . . ? C14 N9 C11 122.0(3) . . ? C13 N10 C17 123.5(3) . . ? C13 N10 C15 111.1(3) . . ? C17 N10 C15 121.2(3) . . ? C16 N11 C14 113.8(3) . . ? C16 N11 C12 124.0(3) . . ? C14 N11 C12 121.6(3) . . ? C16 N12 C15 111.4(3) . . ? C16 N12 C18 122.3(3) . . ? C15 N12 C18 123.5(3) . . ? C19 N13 C17 121.3(3) . . ? C19 N13 C20 112.7(3) . . ? C17 N13 C20 121.7(4) . . ? C19 N14 C21 113.3(3) . . ? C19 N14 C23 124.8(3) . . ? C21 N14 C23 120.4(3) . . ? C22 N15 C18 121.8(3) . . ? C22 N15 C20 112.3(3) . . ? C18 N15 C20 122.4(3) . . ? C22 N16 C21 114.3(3) . . ? C22 N16 C24 121.2(3) . . ? C21 N16 C24 121.5(3) . . ? C19 O4 Rb2 145.6(3) . . ? C4 O5 Rb2 149.5(3) . 10_765 ? C10 O6 Rb1 146.2(3) . . ? C16 O7 Rb1 145.6(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.791 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.067 _database_code_depnum_ccdc_archive 'CCDC 946730' ####################################################################### # # 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_CCDC931659 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H74 N48 O25 Rb2, 2Cl, 72(H2 O)' _chemical_formula_sum 'C72 H218 Cl2 N48 O97 Rb2' _chemical_formula_weight 3550.78 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' Rb Rb -0.9393 2.9676 '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' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 21.879(8) _cell_length_b 21.879(8) _cell_length_c 52.67(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 21832(19) _cell_formula_units_Z 6 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.620 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 11220 _exptl_absorpt_coefficient_mu 0.841 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8300 _exptl_absorpt_correction_T_max 0.8702 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex2 CCD Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52887 _diffrn_reflns_av_R_equivalents 0.0926 _diffrn_reflns_av_sigmaI/netI 0.1039 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -64 _diffrn_reflns_limit_l_max 62 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9398 _reflns_number_gt 4122 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1539P)^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 SHELXL _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9398 _refine_ls_number_parameters 445 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1532 _refine_ls_R_factor_gt 0.0894 _refine_ls_wR_factor_ref 0.2640 _refine_ls_wR_factor_gt 0.2440 _refine_ls_goodness_of_fit_ref 0.915 _refine_ls_restrained_S_all 0.915 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.3333 0.6667 0.12427(14) 0.393(4) Uiso 1 3 d S . . Cl2 Cl -0.3333 0.3333 0.2602(3) 0.431(7) Uiso 1 3 d S . . O1W O 0.3333 0.6667 -0.0062(5) 0.296(7) Uiso 1 3 d S . . Rb1 Rb -0.3333 0.3333 0.066349(12) 0.07132(17) Uani 1 3 d S . . Rb2 Rb 0.3333 0.6667 0.052710(13) 0.0811(2) Uani 1 3 d S . . C1 C -0.02133(13) 0.35775(14) 0.09005(5) 0.0605(9) Uani 1 1 d . . . C2 C 0.09707(12) 0.41650(13) 0.10284(6) 0.0668(10) Uani 1 1 d . . . H2 H 0.1155 0.3968 0.1157 0.080 Uiso 1 1 calc R . . C3 C 0.05777(14) 0.45563(13) 0.11595(6) 0.0686(10) Uani 1 1 d . . . H3 H 0.0594 0.4561 0.1347 0.082 Uiso 1 1 calc R . . C4 C 0.15423(13) 0.53723(15) 0.09060(6) 0.0716(10) Uani 1 1 d . . . C5 C -0.07088(15) 0.41020(15) 0.11796(6) 0.0745(11) Uani 1 1 d . . . H5A H -0.0622 0.4127 0.1363 0.089 Uiso 1 1 calc R . . H5B H -0.1139 0.3653 0.1144 0.089 Uiso 1 1 calc R . . C6 C 0.09202(13) 0.58423(14) 0.11525(8) 0.0821(11) Uani 1 1 d . . . H6A H 0.0931 0.5823 0.1338 0.099 Uiso 1 1 calc R . . H6B H 0.1331 0.6286 0.1098 0.099 Uiso 1 1 calc R . . C7 C -0.14402(14) 0.46121(14) 0.09940(6) 0.0638(9) Uani 1 1 d . . . C8 C -0.04194(14) 0.53979(15) 0.12031(6) 0.0691(9) Uani 1 1 d . . . H8 H -0.0356 0.5383 0.1389 0.083 Uiso 1 1 calc R . . C9 C -0.08344(16) 0.57819(18) 0.11415(7) 0.0857(12) Uani 1 1 d . . . H9 H -0.0963 0.5962 0.1293 0.103 Uiso 1 1 calc R . . C10 C 0.03063(15) 0.63851(16) 0.09570(6) 0.0745(11) Uani 1 1 d . . . C11 C -0.20369(13) 0.53268(15) 0.09344(7) 0.0760(11) Uani 1 1 d . . . H11A H -0.2468 0.4865 0.0924 0.091 Uiso 1 1 calc R . . H11B H -0.2106 0.5598 0.1068 0.091 Uiso 1 1 calc R . . C12 C -0.04353(17) 0.69529(16) 0.09173(8) 0.0992(14) Uani 1 1 d . . . H12A H 0.0024 0.7383 0.0897 0.119 Uiso 1 1 calc R . . H12B H -0.0673 0.7020 0.1063 0.119 Uiso 1 1 calc R . . C13 C -0.23088(12) 0.53615(14) 0.04799(6) 0.0647(10) Uani 1 1 d . . . C14 C -0.16496(15) 0.64446(14) 0.06969(7) 0.0777(11) Uani 1 1 d . . . H14 H -0.1849 0.6612 0.0831 0.093 Uiso 1 1 calc R . . C15 C -0.18073(15) 0.65914(13) 0.04179(7) 0.0759(11) Uani 1 1 d . . . H15 H -0.2122 0.6795 0.0417 0.091 Uiso 1 1 calc R . . C16 C -0.06076(14) 0.72265(14) 0.04661(7) 0.0802(11) Uani 1 1 d . . . C17 C -0.26244(15) 0.56735(17) 0.00722(7) 0.0886(12) Uani 1 1 d . . . H17A H -0.2971 0.5168 0.0076 0.106 Uiso 1 1 calc R . . H17B H -0.2881 0.5934 0.0075 0.106 Uiso 1 1 calc R . . C18 C -0.10690(17) 0.74602(15) 0.00826(7) 0.0924(12) Uani 1 1 d . . . H18A H -0.0595 0.7877 0.0083 0.111 Uiso 1 1 calc R . . H18B H -0.1412 0.7624 0.0087 0.111 Uiso 1 1 calc R . . C19 C -0.23461(12) 0.53522(14) -0.03391(6) 0.0594(9) Uani 1 1 d . . . C20 C -0.18477(14) 0.65908(14) -0.02697(6) 0.0717(10) Uani 1 1 d . . . H20 H -0.2161 0.6797 -0.0266 0.086 Uiso 1 1 calc R . . C21 C -0.17008(13) 0.64454(13) -0.05385(6) 0.0644(10) Uani 1 1 d . . . H21 H -0.1887 0.6648 -0.0664 0.077 Uiso 1 1 calc R . . C22 C -0.06482(15) 0.71872(15) -0.03355(7) 0.0830(12) Uani 1 1 d . . . C23 C 0.21311(14) 0.46560(16) 0.08091(8) 0.0964(14) Uani 1 1 d . . . H23A H 0.2205 0.4381 0.0940 0.116 Uiso 1 1 calc R . . H23B H 0.2558 0.5122 0.0803 0.116 Uiso 1 1 calc R . . C24 C 0.05031(16) 0.30260(15) 0.07796(8) 0.0956(14) Uani 1 1 d . . . H24A H 0.0728 0.2886 0.0910 0.115 Uiso 1 1 calc R . . H24B H 0.0029 0.2624 0.0751 0.115 Uiso 1 1 calc R . . N1 N 0.04314(12) 0.36333(12) 0.08810(5) 0.0736(8) Uani 1 1 d . . . N2 N -0.01471(11) 0.41103(12) 0.10540(5) 0.0724(8) Uani 1 1 d . . . N3 N 0.15384(12) 0.47480(12) 0.08878(6) 0.0800(10) Uani 1 1 d . . . N4 N 0.09753(12) 0.52472(13) 0.10466(6) 0.0869(10) Uani 1 1 d . . . N5 N -0.08286(11) 0.47059(12) 0.11034(5) 0.0696(8) Uani 1 1 d . . . N6 N -0.14399(11) 0.52234(12) 0.10059(5) 0.0668(8) Uani 1 1 d . . . N7 N 0.02771(12) 0.58412(12) 0.10744(6) 0.0791(9) Uani 1 1 d . . . N8 N -0.03247(11) 0.63478(11) 0.09678(5) 0.0708(8) Uani 1 1 d . . . N9 N -0.19339(11) 0.56873(10) 0.06968(5) 0.0677(8) Uani 1 1 d . . . N10 N -0.21616(12) 0.58630(11) 0.02967(5) 0.0677(8) Uani 1 1 d . . . N11 N -0.08667(12) 0.68436(12) 0.06841(7) 0.0961(11) Uani 1 1 d . . . N12 N -0.11524(12) 0.70529(12) 0.03063(6) 0.0766(9) Uani 1 1 d . . . N13 N -0.22053(12) 0.58424(12) -0.01589(5) 0.0734(9) Uani 1 1 d . . . N14 N -0.20542(11) 0.56930(11) -0.05620(5) 0.0756(9) Uani 1 1 d . . . N15 N -0.11701(11) 0.70514(13) -0.01584(5) 0.0763(9) Uani 1 1 d . . . N16 N -0.09066(11) 0.68316(13) -0.05453(6) 0.0820(9) Uani 1 1 d . . . O1 O -0.07547(10) 0.31363(11) 0.08090(4) 0.0813(8) Uani 1 1 d . . . O2 O -0.19142(9) 0.40535(10) 0.09005(4) 0.0742(7) Uani 1 1 d . . . O3 O -0.26277(10) 0.47211(9) 0.04433(4) 0.0761(7) Uani 1 1 d . . . O4 O -0.26710(11) 0.47207(9) -0.03087(4) 0.0843(8) Uani 1 1 d . . . O5 O 0.20005(9) 0.59419(10) 0.08145(5) 0.0799(7) Uani 1 1 d . . . O6 O 0.08100(11) 0.68469(10) 0.08314(5) 0.0969(9) Uani 1 1 d . . . O7 O 0.00110(10) 0.76780(11) 0.04262(6) 0.1183(11) Uani 1 1 d . . . O8 O -0.00237(11) 0.75859(12) -0.02862(6) 0.1375(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rb1 0.04442(15) 0.04442(15) 0.1251(5) 0.000 0.000 0.02221(8) Rb2 0.04844(17) 0.04844(17) 0.1463(5) 0.000 0.000 0.02422(8) C1 0.0436(12) 0.0589(14) 0.0617(18) -0.0040(14) -0.0017(13) 0.0128(11) C2 0.0344(11) 0.0538(13) 0.102(2) 0.0267(15) 0.0055(14) 0.0142(10) C3 0.0717(14) 0.0545(13) 0.079(2) 0.0142(14) 0.0114(15) 0.0315(11) C4 0.0405(12) 0.0691(15) 0.100(2) 0.0122(16) -0.0036(14) 0.0232(11) C5 0.0759(16) 0.0593(15) 0.079(2) 0.0044(15) 0.0136(16) 0.0269(12) C6 0.0416(11) 0.0617(14) 0.145(3) -0.0076(17) -0.0215(16) 0.0273(10) C7 0.0607(14) 0.0521(13) 0.0712(19) -0.0060(13) 0.0016(14) 0.0226(11) C8 0.0739(13) 0.0885(15) 0.0621(19) -0.0047(14) 0.0019(14) 0.0534(11) C9 0.0804(17) 0.0924(19) 0.083(2) -0.0091(18) -0.0015(17) 0.0423(14) C10 0.0518(15) 0.0671(17) 0.077(2) -0.0104(16) -0.0147(15) 0.0090(13) C11 0.0306(12) 0.0629(16) 0.114(3) 0.0005(17) 0.0052(15) 0.0082(11) C12 0.0627(17) 0.0530(17) 0.155(3) 0.005(2) -0.022(2) 0.0089(14) C13 0.0373(11) 0.0575(14) 0.091(2) 0.0010(14) 0.0124(14) 0.0175(10) C14 0.0686(16) 0.0400(13) 0.114(3) -0.0042(15) -0.0025(18) 0.0190(11) C15 0.0636(14) 0.0343(12) 0.124(3) 0.0118(15) 0.0118(17) 0.0199(10) C16 0.0696(13) 0.0600(13) 0.124(3) 0.0071(15) 0.0295(16) 0.0418(10) C17 0.0525(15) 0.0747(17) 0.125(3) 0.0342(18) 0.0123(18) 0.0214(13) C18 0.0801(17) 0.0471(14) 0.143(3) -0.0047(17) 0.0364(19) 0.0264(12) C19 0.0308(10) 0.0661(14) 0.0702(19) 0.0071(14) -0.0040(12) 0.0159(10) C20 0.0518(13) 0.0396(12) 0.115(3) 0.0136(15) 0.0225(16) 0.0160(10) C21 0.0510(13) 0.0372(12) 0.093(2) 0.0097(14) 0.0028(15) 0.0130(10) C22 0.0586(16) 0.0526(15) 0.120(3) -0.0241(17) -0.0055(18) 0.0144(12) C23 0.0404(12) 0.0711(16) 0.178(4) 0.013(2) -0.0045(18) 0.0280(11) C24 0.0609(16) 0.0401(14) 0.166(3) 0.0137(19) 0.024(2) 0.0106(12) N1 0.0680(12) 0.0630(12) 0.0863(18) -0.0147(12) -0.0164(13) 0.0301(10) N2 0.0531(11) 0.0636(12) 0.0969(19) -0.0008(13) 0.0052(13) 0.0266(9) N3 0.0521(12) 0.0497(12) 0.118(2) 0.0005(14) -0.0006(14) 0.0104(10) N4 0.0451(11) 0.0638(13) 0.144(2) -0.0222(15) -0.0274(14) 0.0210(9) N5 0.0389(10) 0.0580(12) 0.0948(18) 0.0016(13) -0.0107(12) 0.0114(9) N6 0.0403(10) 0.0590(12) 0.0883(17) 0.0031(12) 0.0065(12) 0.0152(9) N7 0.0663(12) 0.0502(11) 0.114(2) -0.0067(13) -0.0079(14) 0.0243(10) N8 0.0400(10) 0.0432(10) 0.117(2) -0.0002(12) 0.0009(13) 0.0116(8) N9 0.0690(12) 0.0385(10) 0.0875(17) 0.0040(11) 0.0257(12) 0.0209(9) N10 0.0623(12) 0.0382(10) 0.0896(17) -0.0077(12) -0.0075(13) 0.0153(9) N11 0.0562(12) 0.0507(12) 0.180(3) 0.0103(16) 0.0043(17) 0.0253(9) N12 0.0585(12) 0.0508(11) 0.115(2) 0.0001(13) 0.0025(14) 0.0231(9) N13 0.0687(14) 0.0539(12) 0.0741(16) 0.0061(12) -0.0065(13) 0.0129(11) N14 0.0592(11) 0.0473(11) 0.111(2) -0.0053(13) -0.0243(13) 0.0198(9) N15 0.0436(10) 0.0803(14) 0.0958(19) -0.0014(14) 0.0129(12) 0.0240(10) N16 0.0504(10) 0.0715(13) 0.124(2) -0.0034(14) 0.0143(14) 0.0306(9) O1 0.0685(11) 0.0708(11) 0.0878(15) -0.0060(11) 0.0051(11) 0.0223(9) O2 0.0504(9) 0.0554(10) 0.1006(15) 0.0043(10) -0.0067(10) 0.0144(8) O3 0.0699(11) 0.0338(8) 0.1019(15) 0.0032(10) -0.0037(11) 0.0088(8) O4 0.0741(12) 0.0410(9) 0.1141(17) 0.0067(11) -0.0001(12) 0.0109(9) O5 0.0505(9) 0.0572(10) 0.1246(17) 0.0109(11) 0.0063(11) 0.0213(7) O6 0.0566(11) 0.0458(10) 0.161(2) 0.0020(13) 0.0038(14) 0.0053(9) O7 0.0395(10) 0.0685(12) 0.224(3) -0.0157(16) 0.0229(14) 0.0100(9) O8 0.0390(11) 0.0970(14) 0.212(2) -0.0901(15) 0.0320(13) -0.0143(11) _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 Cl1 Rb2 3.769(8) . ? O1W Rb2 3.10(3) . ? O1W Rb1 3.17(3) 10_565 ? Rb1 O3 2.874(2) 3_455 ? Rb1 O3 2.874(2) 2_565 ? Rb1 O3 2.874(2) . ? Rb1 O2 2.965(2) . ? Rb1 O2 2.965(2) 3_455 ? Rb1 O2 2.965(2) 2_565 ? Rb1 O1W 3.17(3) 10_565 ? Rb2 O4 2.870(2) 12_665 ? Rb2 O4 2.870(2) 11 ? Rb2 O4 2.870(2) 10_565 ? Rb2 O5 2.947(2) 3_565 ? Rb2 O5 2.947(2) . ? Rb2 O5 2.947(2) 2_665 ? C1 O1 1.193(3) . ? C1 N1 1.358(4) . ? C1 N2 1.365(4) . ? C2 N1 1.406(3) . ? C2 N3 1.461(3) . ? C2 C3 1.638(5) . ? C2 H2 0.9900 . ? C3 N4 1.442(4) . ? C3 N2 1.493(3) . ? C3 H3 0.9900 . ? C4 O5 1.241(3) . ? C4 N4 1.350(4) . ? C4 N3 1.365(4) . ? C5 N2 1.388(4) . ? C5 N5 1.524(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.465(4) . ? C6 N4 1.476(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.243(3) . ? C7 N6 1.339(4) . ? C7 N5 1.375(4) . ? C8 N5 1.419(3) . ? C8 N7 1.498(4) . ? C8 C9 1.549(5) . ? C8 H8 0.9900 . ? C9 N6 1.463(4) . ? C9 N8 1.494(4) . ? C9 H9 0.9900 . ? C10 O6 1.249(3) . ? C10 N7 1.314(4) . ? C10 N8 1.343(4) . ? C11 N9 1.435(4) . ? C11 N6 1.481(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N8 1.484(5) . ? C12 N11 1.494(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.229(3) . ? C13 N10 1.373(4) . ? C13 N9 1.379(4) . ? C14 N9 1.450(3) . ? C14 N11 1.485(4) . ? C14 C15 1.579(5) . ? C14 H14 0.9900 . ? C15 N12 1.404(4) . ? C15 N10 1.521(4) . ? C15 H15 0.9900 . ? C16 O7 1.231(3) . ? C16 N12 1.349(4) . ? C16 N11 1.366(5) . ? C17 N13 1.456(4) . ? C17 N10 1.475(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N12 1.433(5) . ? C18 N15 1.504(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.207(3) . ? C19 N13 1.347(4) . ? C19 N14 1.366(4) . ? C20 N15 1.436(3) . ? C20 C21 1.520(5) . ? C20 N13 1.534(4) . ? C20 H20 0.9900 . ? C21 N14 1.432(3) . ? C21 N16 1.506(3) . ? C21 H21 0.9900 . ? C22 O8 1.226(3) . ? C22 N16 1.306(4) . ? C22 N15 1.387(4) . ? C23 N3 1.468(4) . ? C23 N14 1.475(5) 10_565 ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N16 1.457(5) 10_565 ? C24 N1 1.511(4) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? N14 C23 1.475(5) 10_565 ? N16 C24 1.457(5) 10_565 ? O4 Rb2 2.870(2) 10_565 ? 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 Rb2 O1W Rb1 180.0 . 10_565 ? O3 Rb1 O3 104.82(5) 3_455 2_565 ? O3 Rb1 O3 104.82(5) 3_455 . ? O3 Rb1 O3 104.82(5) 2_565 . ? O3 Rb1 O2 76.60(7) 3_455 . ? O3 Rb1 O2 178.54(6) 2_565 . ? O3 Rb1 O2 75.04(6) . . ? O3 Rb1 O2 75.04(6) 3_455 3_455 ? O3 Rb1 O2 76.60(7) 2_565 3_455 ? O3 Rb1 O2 178.54(6) . 3_455 ? O2 Rb1 O2 103.54(5) . 3_455 ? O3 Rb1 O2 178.54(6) 3_455 2_565 ? O3 Rb1 O2 75.04(6) 2_565 2_565 ? O3 Rb1 O2 76.60(7) . 2_565 ? O2 Rb1 O2 103.54(5) . 2_565 ? O2 Rb1 O2 103.54(5) 3_455 2_565 ? O3 Rb1 O1W 66.20(5) 3_455 10_565 ? O3 Rb1 O1W 66.20(5) 2_565 10_565 ? O3 Rb1 O1W 66.20(5) . 10_565 ? O2 Rb1 O1W 114.90(5) . 10_565 ? O2 Rb1 O1W 114.90(5) 3_455 10_565 ? O2 Rb1 O1W 114.90(5) 2_565 10_565 ? O4 Rb2 O4 105.02(6) 12_665 11 ? O4 Rb2 O4 105.02(6) 12_665 10_565 ? O4 Rb2 O4 105.02(6) 11 10_565 ? O4 Rb2 O5 78.24(6) 12_665 3_565 ? O4 Rb2 O5 80.18(7) 11 3_565 ? O4 Rb2 O5 172.61(7) 10_565 3_565 ? O4 Rb2 O5 80.18(7) 12_665 . ? O4 Rb2 O5 172.61(7) 11 . ? O4 Rb2 O5 78.24(6) 10_565 . ? O5 Rb2 O5 95.98(7) 3_565 . ? O4 Rb2 O5 172.61(7) 12_665 2_665 ? O4 Rb2 O5 78.24(7) 11 2_665 ? O4 Rb2 O5 80.18(7) 10_565 2_665 ? O5 Rb2 O5 95.98(7) 3_565 2_665 ? O5 Rb2 O5 95.98(7) . 2_665 ? O4 Rb2 O1W 66.38(5) 12_665 . ? O4 Rb2 O1W 66.38(5) 11 . ? O4 Rb2 O1W 66.38(5) 10_565 . ? O5 Rb2 O1W 120.91(5) 3_565 . ? O5 Rb2 O1W 120.91(5) . . ? O5 Rb2 O1W 120.91(5) 2_665 . ? O4 Rb2 Cl1 113.62(5) 12_665 . ? O4 Rb2 Cl1 113.62(5) 11 . ? O4 Rb2 Cl1 113.62(5) 10_565 . ? O5 Rb2 Cl1 59.09(5) 3_565 . ? O5 Rb2 Cl1 59.09(5) . . ? O5 Rb2 Cl1 59.09(5) 2_665 . ? O1W Rb2 Cl1 180.000(1) . . ? O1 C1 N1 127.5(3) . . ? O1 C1 N2 124.6(3) . . ? N1 C1 N2 107.8(2) . . ? N1 C2 N3 116.0(3) . . ? N1 C2 C3 102.9(2) . . ? N3 C2 C3 101.3(2) . . ? N1 C2 H2 111.9 . . ? N3 C2 H2 111.9 . . ? C3 C2 H2 111.9 . . ? N4 C3 N2 114.7(3) . . ? N4 C3 C2 100.1(2) . . ? N2 C3 C2 99.5(2) . . ? N4 C3 H3 113.6 . . ? N2 C3 H3 113.6 . . ? C2 C3 H3 113.6 . . ? O5 C4 N4 128.0(3) . . ? O5 C4 N3 125.1(3) . . ? N4 C4 N3 106.9(2) . . ? N2 C5 N5 113.5(2) . . ? N2 C5 H5A 108.9 . . ? N5 C5 H5A 108.9 . . ? N2 C5 H5B 108.9 . . ? N5 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? N7 C6 N4 113.3(2) . . ? N7 C6 H6A 108.9 . . ? N4 C6 H6A 108.9 . . ? N7 C6 H6B 108.9 . . ? N4 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N6 125.8(3) . . ? O2 C7 N5 125.7(3) . . ? N6 C7 N5 108.5(2) . . ? N5 C8 N7 114.7(3) . . ? N5 C8 C9 105.8(2) . . ? N7 C8 C9 103.7(2) . . ? N5 C8 H8 110.7 . . ? N7 C8 H8 110.7 . . ? C9 C8 H8 110.7 . . ? N6 C9 N8 112.5(3) . . ? N6 C9 C8 100.4(3) . . ? N8 C9 C8 100.4(3) . . ? N6 C9 H9 114.0 . . ? N8 C9 H9 114.0 . . ? C8 C9 H9 114.0 . . ? O6 C10 N7 127.3(3) . . ? O6 C10 N8 122.4(3) . . ? N7 C10 N8 110.0(2) . . ? N9 C11 N6 113.4(2) . . ? N9 C11 H11A 108.9 . . ? N6 C11 H11A 108.9 . . ? N9 C11 H11B 108.9 . . ? N6 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? N8 C12 N11 112.1(3) . . ? N8 C12 H12A 109.2 . . ? N11 C12 H12A 109.2 . . ? N8 C12 H12B 109.2 . . ? N11 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? O3 C13 N10 125.0(3) . . ? O3 C13 N9 124.8(3) . . ? N10 C13 N9 109.2(2) . . ? N9 C14 N11 112.4(3) . . ? N9 C14 C15 102.7(2) . . ? N11 C14 C15 98.2(3) . . ? N9 C14 H14 114.0 . . ? N11 C14 H14 114.0 . . ? C15 C14 H14 114.0 . . ? N12 C15 N10 112.4(3) . . ? N12 C15 C14 106.7(3) . . ? N10 C15 C14 103.1(2) . . ? N12 C15 H15 111.4 . . ? N10 C15 H15 111.4 . . ? C14 C15 H15 111.4 . . ? O7 C16 N12 125.6(3) . . ? O7 C16 N11 126.0(3) . . ? N12 C16 N11 108.3(2) . . ? N13 C17 N10 110.0(2) . . ? N13 C17 H17A 109.7 . . ? N10 C17 H17A 109.7 . . ? N13 C17 H17B 109.7 . . ? N10 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? N12 C18 N15 112.9(3) . . ? N12 C18 H18A 109.0 . . ? N15 C18 H18A 109.0 . . ? N12 C18 H18B 109.0 . . ? N15 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? O4 C19 N13 126.0(3) . . ? O4 C19 N14 125.8(3) . . ? N13 C19 N14 108.2(2) . . ? N15 C20 C21 106.0(2) . . ? N15 C20 N13 113.0(3) . . ? C21 C20 N13 100.3(2) . . ? N15 C20 H20 112.3 . . ? C21 C20 H20 112.3 . . ? N13 C20 H20 112.3 . . ? N14 C21 N16 116.8(3) . . ? N14 C21 C20 105.8(2) . . ? N16 C21 C20 102.1(2) . . ? N14 C21 H21 110.5 . . ? N16 C21 H21 110.5 . . ? C20 C21 H21 110.5 . . ? O8 C22 N16 126.8(3) . . ? O8 C22 N15 121.0(3) . . ? N16 C22 N15 112.1(2) . . ? N3 C23 N14 116.1(3) . 10_565 ? N3 C23 H23A 108.3 . . ? N14 C23 H23A 108.3 10_565 . ? N3 C23 H23B 108.3 . . ? N14 C23 H23B 108.3 10_565 . ? H23A C23 H23B 107.4 . . ? N16 C24 N1 115.4(3) 10_565 . ? N16 C24 H24A 108.4 10_565 . ? N1 C24 H24A 108.4 . . ? N16 C24 H24B 108.4 10_565 . ? N1 C24 H24B 108.4 . . ? H24A C24 H24B 107.5 . . ? C1 N1 C2 115.9(3) . . ? C1 N1 C24 120.5(2) . . ? C2 N1 C24 120.6(3) . . ? C1 N2 C5 123.8(2) . . ? C1 N2 C3 113.8(3) . . ? C5 N2 C3 118.4(3) . . ? C4 N3 C2 114.5(3) . . ? C4 N3 C23 126.4(2) . . ? C2 N3 C23 116.6(3) . . ? C4 N4 C3 116.7(3) . . ? C4 N4 C6 120.0(2) . . ? C3 N4 C6 119.8(3) . . ? C7 N5 C8 111.2(3) . . ? C7 N5 C5 123.9(2) . . ? C8 N5 C5 122.5(2) . . ? C7 N6 C9 113.9(3) . . ? C7 N6 C11 125.5(2) . . ? C9 N6 C11 119.7(3) . . ? C10 N7 C6 121.3(2) . . ? C10 N7 C8 111.9(3) . . ? C6 N7 C8 122.7(3) . . ? C10 N8 C12 124.0(2) . . ? C10 N8 C9 113.3(3) . . ? C12 N8 C9 117.5(3) . . ? C13 N9 C11 123.3(2) . . ? C13 N9 C14 113.3(3) . . ? C11 N9 C14 119.2(3) . . ? C13 N10 C17 119.0(2) . . ? C13 N10 C15 109.6(2) . . ? C17 N10 C15 123.3(3) . . ? C16 N11 C14 113.7(3) . . ? C16 N11 C12 123.9(2) . . ? C14 N11 C12 120.5(3) . . ? C16 N12 C15 112.5(3) . . ? C16 N12 C18 121.2(2) . . ? C15 N12 C18 123.9(3) . . ? C19 N13 C17 121.5(2) . . ? C19 N13 C20 111.9(2) . . ? C17 N13 C20 120.6(3) . . ? C19 N14 C21 112.9(3) . . ? C19 N14 C23 125.1(2) . 10_565 ? C21 N14 C23 121.8(3) . 10_565 ? C22 N15 C20 109.1(3) . . ? C22 N15 C18 125.4(2) . . ? C20 N15 C18 123.7(3) . . ? C22 N16 C24 123.6(2) . 10_565 ? C22 N16 C21 110.4(3) . . ? C24 N16 C21 123.1(3) 10_565 . ? C7 O2 Rb1 145.8(2) . . ? C13 O3 Rb1 147.2(2) . . ? C19 O4 Rb2 148.7(2) . 10_565 ? C4 O5 Rb2 145.6(2) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.532 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.091 # 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 -0.046 -0.042 -0.001 7458 2918 ' ' 2 0.000 0.500 0.000 356 155 ' ' 3 0.167 0.333 0.333 358 153 ' ' 4 0.167 0.833 0.333 358 154 ' ' 5 -0.167 0.167 0.667 358 154 ' ' 6 -0.167 0.667 0.667 358 153 ' ' 7 0.333 0.167 0.667 358 155 ' ' 8 0.500 1.000 1.000 356 153 ' ' 9 0.500 0.500 0.000 356 154 ' ' 10 0.667 0.833 0.333 358 155 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 931659' ####################################################################### # # 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_CCDC931660 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C144 H380 Cl24 In6 N96 Na2 O164' _chemical_formula_weight 7667.14 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' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P -3' _symmetry_space_group_name_Hall '-P 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 22.174(3) _cell_length_b 22.174(3) _cell_length_c 18.102(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 7708(3) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.652 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3952 _exptl_absorpt_coefficient_mu 0.770 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7851 _exptl_absorpt_correction_T_max 0.8132 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex2 CCD Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46011 _diffrn_reflns_av_R_equivalents 0.0527 _diffrn_reflns_av_sigmaI/netI 0.0651 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 27.66 _reflns_number_total 11851 _reflns_number_gt 6496 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1105P)^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 11851 _refine_ls_number_parameters 508 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0983 _refine_ls_R_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.1829 _refine_ls_wR_factor_gt 0.1701 _refine_ls_goodness_of_fit_ref 0.940 _refine_ls_restrained_S_all 0.940 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O3W O 0.1742(4) 0.0682(3) 0.2693(4) 0.197(3) Uani 1 1 d . . . O1W O 0.46804(15) 0.69301(18) -0.04800(13) 0.0649(9) Uani 1 1 d . . . O2W O 0.5214(2) 0.71983(19) 0.12256(16) 0.0793(10) Uani 1 1 d . . . In1 In 0.58582(2) 0.755143(18) 0.018415(15) 0.07125(16) Uani 1 1 d . . . Cl1 Cl 0.58389(7) 0.64245(6) 0.02140(6) 0.0643(3) Uani 1 1 d . . . Cl2 Cl 0.65252(8) 0.79185(7) -0.09827(6) 0.0842(4) Uani 1 1 d . . . Cl3 Cl 0.68741(9) 0.80938(8) 0.10264(8) 0.0976(5) Uani 1 1 d . . . Cl4 Cl 0.57364(14) 0.86027(9) 0.02423(8) 0.1385(9) Uani 1 1 d . . . Na1 Na 0.6667 0.3333 0.31089(19) 0.0644(8) Uani 1 3 d S . . C1 C 0.2669(2) 0.29588(18) 0.6587(2) 0.0428(8) Uani 1 1 d . . . C2 C 0.22692(18) 0.36367(18) 0.71494(18) 0.0380(8) Uani 1 1 d . . . H2 H 0.1920 0.3436 0.7550 0.046 Uiso 1 1 calc R . . C3 C 0.19295(18) 0.34004(18) 0.63817(18) 0.0373(8) Uani 1 1 d . . . H3 H 0.1415 0.3134 0.6415 0.045 Uiso 1 1 calc R . . C4 C 0.25174(18) 0.46184(19) 0.6446(2) 0.0405(8) Uani 1 1 d . . . C5 C 0.1846(2) 0.24611(19) 0.55310(18) 0.0414(8) Uani 1 1 d . . . H5A H 0.1983 0.2105 0.5568 0.050 Uiso 1 1 calc R . . H5B H 0.1343 0.2233 0.5614 0.050 Uiso 1 1 calc R . . C6 C 0.1819(2) 0.4096(2) 0.5339(2) 0.0479(10) Uani 1 1 d . . . H6A H 0.1938 0.4581 0.5267 0.057 Uiso 1 1 calc R . . H6B H 0.1316 0.3819 0.5421 0.057 Uiso 1 1 calc R . . C7 C 0.22996(18) 0.25388(19) 0.42779(18) 0.0395(8) Uani 1 1 d . . . C8 C 0.16657(19) 0.31138(19) 0.44810(18) 0.0402(8) Uani 1 1 d . . . H8 H 0.1160 0.2869 0.4588 0.048 Uiso 1 1 calc R . . C9 C 0.18106(19) 0.3122(2) 0.36420(18) 0.0402(8) Uani 1 1 d . . . H9 H 0.1374 0.2869 0.3354 0.048 Uiso 1 1 calc R . . C10 C 0.2270(2) 0.4262(2) 0.4061(2) 0.0499(10) Uani 1 1 d . . . C11 C 0.23847(19) 0.25620(19) 0.29154(19) 0.0429(8) Uani 1 1 d . . . H11A H 0.2469 0.2176 0.3015 0.052 Uiso 1 1 calc R . . H11B H 0.1977 0.2386 0.2591 0.052 Uiso 1 1 calc R . . C12 C 0.2310(2) 0.4117(2) 0.27091(19) 0.0508(10) Uani 1 1 d . . . H12A H 0.1905 0.3811 0.2405 0.061 Uiso 1 1 calc R . . H12B H 0.2355 0.4579 0.2711 0.061 Uiso 1 1 calc R . . C13 C 0.36213(19) 0.31671(18) 0.25576(18) 0.0389(8) Uani 1 1 d . . . C14 C 0.29450(18) 0.35841(19) 0.20298(18) 0.0401(8) Uani 1 1 d . . . H14 H 0.2564 0.3346 0.1665 0.048 Uiso 1 1 calc R . . C15 C 0.36659(18) 0.39378(19) 0.16534(18) 0.0398(8) Uani 1 1 d . . . H15 H 0.3633 0.3810 0.1125 0.048 Uiso 1 1 calc R . . C16 C 0.3478(2) 0.4788(2) 0.2164(2) 0.0471(9) Uani 1 1 d . . . C17 C 0.46611(18) 0.36878(19) 0.1774(2) 0.0436(9) Uani 1 1 d . . . H17A H 0.4704 0.3310 0.2000 0.052 Uiso 1 1 calc R . . H17B H 0.4589 0.3594 0.1243 0.052 Uiso 1 1 calc R . . C18 C 0.4504(2) 0.5203(2) 0.1345(2) 0.0521(10) Uani 1 1 d . . . H18A H 0.4469 0.5066 0.0825 0.063 Uiso 1 1 calc R . . H18B H 0.4484 0.5635 0.1366 0.063 Uiso 1 1 calc R . . C19 C 0.58746(18) 0.43585(19) 0.21966(19) 0.0400(8) Uani 1 1 d . . . C20 C 0.54943(19) 0.49402(18) 0.14146(19) 0.0410(8) Uani 1 1 d . . . H20 H 0.5419 0.4816 0.0884 0.049 Uiso 1 1 calc R . . C21 C 0.62715(18) 0.54206(18) 0.15956(18) 0.0388(8) Uani 1 1 d . . . H21 H 0.6560 0.5590 0.1143 0.047 Uiso 1 1 calc R . . C22 C 0.5634(2) 0.5953(2) 0.19499(18) 0.0443(9) Uani 1 1 d . . . C23 C 0.28574(18) 0.48295(19) 0.7763(2) 0.0399(8) Uani 1 1 d . . . H23A H 0.2548 0.4593 0.8182 0.048 Uiso 1 1 calc R . . H23B H 0.2844 0.5257 0.7667 0.048 Uiso 1 1 calc R . . C24 C 0.3099(2) 0.33553(19) 0.7846(2) 0.0501(10) Uani 1 1 d . . . H24A H 0.2778 0.3242 0.8263 0.060 Uiso 1 1 calc R . . H24B H 0.3214 0.2984 0.7804 0.060 Uiso 1 1 calc R . . N1 N 0.27512(16) 0.33763(15) 0.71714(16) 0.0429(7) Uani 1 1 d . . . N2 N 0.22022(15) 0.29804(15) 0.61064(15) 0.0404(7) Uani 1 1 d . . . N3 N 0.25953(15) 0.43864(14) 0.71244(15) 0.0383(7) Uani 1 1 d . . . N4 N 0.21743(16) 0.40534(15) 0.59861(15) 0.0404(7) Uani 1 1 d . . . N5 N 0.19998(16) 0.27524(15) 0.47972(15) 0.0407(7) Uani 1 1 d . . . N6 N 0.22251(15) 0.27790(16) 0.36013(15) 0.0410(7) Uani 1 1 d . . . N7 N 0.19965(17) 0.38476(16) 0.46658(15) 0.0464(8) Uani 1 1 d . . . N8 N 0.21862(17) 0.38491(17) 0.34619(15) 0.0470(8) Uani 1 1 d . . . N9 N 0.29736(15) 0.30953(15) 0.25327(15) 0.0403(7) Uani 1 1 d . . . N10 N 0.40530(15) 0.36821(15) 0.20803(15) 0.0379(7) Uani 1 1 d . . . N11 N 0.29285(17) 0.41666(17) 0.23755(16) 0.0471(8) Uani 1 1 d . . . N12 N 0.39121(16) 0.46608(16) 0.17481(17) 0.0457(7) Uani 1 1 d . . . N13 N 0.53024(15) 0.43312(15) 0.18825(16) 0.0405(7) Uani 1 1 d . . . N14 N 0.64422(15) 0.49854(15) 0.20319(16) 0.0412(7) Uani 1 1 d . . . N15 N 0.51711(16) 0.53369(16) 0.16345(18) 0.0468(8) Uani 1 1 d . . . N16 N 0.62645(16) 0.59857(16) 0.20024(16) 0.0448(7) Uani 1 1 d . . . O1 O 0.29726(15) 0.26250(15) 0.64867(16) 0.0602(8) Uani 1 1 d . . . O2 O 0.25714(15) 0.21934(15) 0.43834(14) 0.0533(7) Uani 1 1 d . . . O3 O 0.37941(14) 0.28285(13) 0.29559(15) 0.0516(7) Uani 1 1 d . . . O4 O 0.58704(14) 0.38860(14) 0.25502(16) 0.0540(7) Uani 1 1 d . . . O5 O 0.27188(16) 0.52281(14) 0.62878(15) 0.0558(7) Uani 1 1 d . . . O6 O 0.25386(19) 0.49004(17) 0.40581(17) 0.0729(9) Uani 1 1 d . . . O7 O 0.35720(18) 0.53711(16) 0.23130(18) 0.0717(9) Uani 1 1 d . . . O8 O 0.55013(15) 0.64022(14) 0.21654(15) 0.0543(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O3W 0.210(6) 0.113(4) 0.236(7) -0.019(4) -0.151(6) 0.057(4) O1W 0.077(2) 0.131(3) 0.0332(13) -0.0177(15) -0.0009(13) 0.087(2) O2W 0.129(3) 0.108(3) 0.0443(16) 0.0014(16) 0.0055(17) 0.091(3) In1 0.1349(4) 0.0686(3) 0.03602(18) 0.00174(13) 0.00204(17) 0.0702(2) Cl1 0.1050(9) 0.0626(7) 0.0445(5) 0.0078(5) 0.0154(5) 0.0564(7) Cl2 0.1087(10) 0.0727(8) 0.0450(6) 0.0083(5) -0.0008(6) 0.0258(7) Cl3 0.1325(13) 0.0934(10) 0.0637(8) -0.0099(7) -0.0075(8) 0.0541(10) Cl4 0.311(3) 0.1189(13) 0.0608(8) -0.0160(8) -0.0285(12) 0.1637(18) Na1 0.0385(9) 0.0385(9) 0.116(3) 0.000 0.000 0.0193(5) C1 0.046(2) 0.033(2) 0.046(2) -0.0004(16) -0.0045(16) 0.0178(18) C2 0.040(2) 0.040(2) 0.0328(17) -0.0007(14) 0.0021(14) 0.0193(17) C3 0.040(2) 0.040(2) 0.0370(17) -0.0011(15) 0.0009(15) 0.0235(17) C4 0.038(2) 0.042(2) 0.046(2) -0.0006(16) 0.0053(16) 0.0235(18) C5 0.053(2) 0.043(2) 0.0328(17) -0.0025(15) -0.0030(15) 0.0268(19) C6 0.067(3) 0.058(2) 0.0383(19) -0.0006(17) 0.0022(17) 0.046(2) C7 0.041(2) 0.044(2) 0.0362(18) 0.0000(15) 0.0034(15) 0.0226(18) C8 0.041(2) 0.050(2) 0.0330(17) 0.0007(15) -0.0003(14) 0.0254(18) C9 0.041(2) 0.056(2) 0.0359(18) 0.0003(16) 0.0022(15) 0.0330(19) C10 0.062(3) 0.061(3) 0.042(2) 0.0066(18) 0.0075(18) 0.043(2) C11 0.044(2) 0.043(2) 0.0411(19) -0.0022(16) 0.0065(16) 0.0215(18) C12 0.056(2) 0.076(3) 0.0371(19) 0.0122(18) 0.0082(17) 0.045(2) C13 0.042(2) 0.037(2) 0.0406(18) -0.0075(15) -0.0025(15) 0.0215(17) C14 0.038(2) 0.049(2) 0.0324(17) -0.0009(15) -0.0001(14) 0.0211(18) C15 0.042(2) 0.050(2) 0.0315(16) -0.0011(15) -0.0022(14) 0.0262(18) C16 0.055(2) 0.058(3) 0.0394(18) 0.0084(18) 0.0033(17) 0.037(2) C17 0.042(2) 0.039(2) 0.048(2) -0.0114(16) -0.0039(16) 0.0191(18) C18 0.050(2) 0.055(2) 0.050(2) 0.0204(19) 0.0012(18) 0.026(2) C19 0.036(2) 0.045(2) 0.0382(18) -0.0043(16) 0.0014(15) 0.0194(18) C20 0.045(2) 0.043(2) 0.0327(17) 0.0054(15) -0.0003(15) 0.0199(18) C21 0.043(2) 0.039(2) 0.0339(16) 0.0063(14) 0.0053(15) 0.0194(17) C22 0.054(2) 0.049(2) 0.0331(17) 0.0076(16) -0.0019(16) 0.028(2) C23 0.0323(19) 0.039(2) 0.050(2) -0.0057(16) -0.0003(15) 0.0194(17) C24 0.063(3) 0.038(2) 0.046(2) 0.0034(16) -0.0160(18) 0.022(2) N1 0.0489(18) 0.0436(18) 0.0410(16) -0.0049(13) -0.0103(13) 0.0268(15) N2 0.0489(18) 0.0480(18) 0.0346(14) -0.0079(13) -0.0045(13) 0.0319(16) N3 0.0439(17) 0.0346(16) 0.0377(15) -0.0015(12) -0.0012(13) 0.0205(14) N4 0.0508(19) 0.0409(17) 0.0347(15) -0.0024(13) 0.0009(13) 0.0268(15) N5 0.0533(19) 0.0485(18) 0.0320(14) 0.0035(13) 0.0033(13) 0.0341(16) N6 0.0449(18) 0.0507(18) 0.0339(14) -0.0021(13) 0.0030(12) 0.0287(15) N7 0.065(2) 0.0483(19) 0.0335(15) 0.0020(13) 0.0033(14) 0.0337(17) N8 0.062(2) 0.059(2) 0.0328(15) 0.0089(14) 0.0057(14) 0.0399(18) N9 0.0393(17) 0.0418(17) 0.0397(15) 0.0010(13) 0.0025(13) 0.0203(14) N10 0.0370(16) 0.0423(17) 0.0380(15) 0.0030(13) 0.0016(12) 0.0224(14) N11 0.060(2) 0.057(2) 0.0385(16) 0.0096(14) 0.0098(14) 0.0408(18) N12 0.0438(18) 0.048(2) 0.0481(17) 0.0077(14) 0.0017(14) 0.0253(16) N13 0.0361(17) 0.0387(17) 0.0447(16) 0.0011(13) -0.0041(13) 0.0171(14) N14 0.0368(17) 0.0399(17) 0.0449(16) 0.0031(13) -0.0033(13) 0.0177(14) N15 0.0458(19) 0.0428(19) 0.0552(19) 0.0045(15) -0.0074(15) 0.0248(16) N16 0.051(2) 0.0446(18) 0.0393(16) -0.0009(13) -0.0088(14) 0.0239(16) O1 0.072(2) 0.0635(18) 0.0706(19) -0.0137(14) -0.0165(15) 0.0526(17) O2 0.0696(19) 0.0660(18) 0.0472(15) 0.0060(13) 0.0077(13) 0.0510(17) O3 0.0544(17) 0.0486(16) 0.0605(16) 0.0120(13) 0.0040(13) 0.0323(14) O4 0.0492(16) 0.0416(15) 0.0721(18) 0.0141(13) -0.0064(13) 0.0234(13) O5 0.075(2) 0.0397(16) 0.0540(16) 0.0047(12) -0.0005(14) 0.0301(15) O6 0.112(3) 0.053(2) 0.0619(19) 0.0144(15) 0.0157(17) 0.0472(19) O7 0.094(2) 0.059(2) 0.079(2) 0.0079(16) 0.0129(18) 0.0513(19) O8 0.0642(18) 0.0576(18) 0.0515(16) 0.0044(13) -0.0014(13) 0.0382(16) _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 O1W In1 2.562(3) . ? O2W In1 2.255(3) . ? In1 Cl2 2.4714(14) . ? In1 Cl3 2.4772(17) . ? In1 Cl1 2.4783(11) . ? In1 Cl4 2.4795(14) . ? Na1 O4 2.794(3) 2_655 ? Na1 O4 2.794(3) 3_665 ? Na1 O4 2.794(3) . ? Na1 O5 2.980(3) 6_656 ? Na1 O5 2.980(3) 4_666 ? Na1 O5 2.980(3) 5_556 ? C1 O1 1.237(4) . ? C1 N1 1.357(5) . ? C1 N2 1.372(5) . ? C2 N3 1.444(4) . ? C2 N1 1.447(5) . ? C2 C3 1.542(5) . ? C2 H2 0.9900 . ? C3 N2 1.430(4) . ? C3 N4 1.455(4) . ? C3 H3 0.9900 . ? C4 O5 1.227(4) . ? C4 N4 1.374(5) . ? C4 N3 1.376(4) . ? C5 N5 1.441(4) . ? C5 N2 1.458(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.440(5) . ? C6 N7 1.470(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.203(4) . ? C7 N5 1.366(4) . ? C7 N6 1.378(4) . ? C8 N7 1.451(5) . ? C8 N5 1.453(4) . ? C8 C9 1.551(5) . ? C8 H8 0.9900 . ? C9 N8 1.435(5) . ? C9 N6 1.458(4) . ? C9 H9 0.9900 . ? C10 O6 1.231(5) . ? C10 N7 1.362(5) . ? C10 N8 1.370(5) . ? C11 N9 1.428(4) . ? C11 N6 1.438(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.452(5) . ? C12 N8 1.457(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.232(4) . ? C13 N9 1.364(5) . ? C13 N10 1.369(4) . ? C14 N9 1.441(4) . ? C14 N11 1.452(5) . ? C14 C15 1.543(5) . ? C14 H14 0.9900 . ? C15 N12 1.422(5) . ? C15 N10 1.464(4) . ? C15 H15 0.9900 . ? C16 O7 1.232(5) . ? C16 N12 1.358(5) . ? C16 N11 1.361(5) . ? C17 N13 1.438(4) . ? C17 N10 1.452(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N15 1.454(5) . ? C18 N12 1.458(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.224(4) . ? C19 N13 1.364(4) . ? C19 N14 1.362(5) . ? C20 N15 1.441(5) . ? C20 N13 1.465(4) . ? C20 C21 1.542(5) . ? C20 H20 0.9900 . ? C21 N14 1.437(4) . ? C21 N16 1.460(4) . ? C21 H21 0.9900 . ? C22 O8 1.235(4) . ? C22 N15 1.358(5) . ? C22 N16 1.366(5) . ? C23 N3 1.439(4) . ? C23 N14 1.442(4) 4_666 ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N16 1.463(5) 4_666 ? C24 N1 1.457(4) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? N14 C23 1.442(4) 4_666 ? N16 C24 1.463(5) 4_666 ? O5 Na1 2.980(3) 4_666 ? 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 O2W In1 Cl2 177.98(10) . . ? O2W In1 Cl3 85.31(10) . . ? Cl2 In1 Cl3 96.72(5) . . ? O2W In1 Cl1 86.72(8) . . ? Cl2 In1 Cl1 93.24(4) . . ? Cl3 In1 Cl1 91.67(5) . . ? O2W In1 Cl4 86.75(9) . . ? Cl2 In1 Cl4 93.17(6) . . ? Cl3 In1 Cl4 91.00(6) . . ? Cl1 In1 Cl4 172.72(6) . . ? O2W In1 O1W 84.69(11) . . ? Cl2 In1 O1W 93.29(7) . . ? Cl3 In1 O1W 169.99(7) . . ? Cl1 In1 O1W 88.22(8) . . ? Cl4 In1 O1W 87.97(8) . . ? O4 Na1 O4 107.66(10) 2_655 3_665 ? O4 Na1 O4 107.66(10) 2_655 . ? O4 Na1 O4 107.66(10) 3_665 . ? O4 Na1 O5 71.58(8) 2_655 6_656 ? O4 Na1 O5 73.39(8) 3_665 6_656 ? O4 Na1 O5 178.89(9) . 6_656 ? O4 Na1 O5 178.89(9) 2_655 4_666 ? O4 Na1 O5 71.58(8) 3_665 4_666 ? O4 Na1 O5 73.39(8) . 4_666 ? O5 Na1 O5 107.37(9) 6_656 4_666 ? O4 Na1 O5 73.39(8) 2_655 5_556 ? O4 Na1 O5 178.89(9) 3_665 5_556 ? O4 Na1 O5 71.58(8) . 5_556 ? O5 Na1 O5 107.37(9) 6_656 5_556 ? O5 Na1 O5 107.37(9) 4_666 5_556 ? O1 C1 N1 126.5(3) . . ? O1 C1 N2 125.0(3) . . ? N1 C1 N2 108.4(3) . . ? N3 C2 N1 114.5(3) . . ? N3 C2 C3 104.0(3) . . ? N1 C2 C3 102.8(3) . . ? N3 C2 H2 111.6 . . ? N1 C2 H2 111.6 . . ? C3 C2 H2 111.6 . . ? N2 C3 N4 114.1(3) . . ? N2 C3 C2 104.0(3) . . ? N4 C3 C2 103.3(3) . . ? N2 C3 H3 111.7 . . ? N4 C3 H3 111.7 . . ? C2 C3 H3 111.7 . . ? O5 C4 N4 126.5(3) . . ? O5 C4 N3 125.1(3) . . ? N4 C4 N3 108.4(3) . . ? N5 C5 N2 113.0(3) . . ? N5 C5 H5A 109.0 . . ? N2 C5 H5A 109.0 . . ? N5 C5 H5B 109.0 . . ? N2 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? N4 C6 N7 113.1(3) . . ? N4 C6 H6A 109.0 . . ? N7 C6 H6A 109.0 . . ? N4 C6 H6B 109.0 . . ? N7 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? O2 C7 N5 126.7(3) . . ? O2 C7 N6 125.6(3) . . ? N5 C7 N6 107.7(3) . . ? N7 C8 N5 114.6(3) . . ? N7 C8 C9 103.1(3) . . ? N5 C8 C9 103.4(3) . . ? N7 C8 H8 111.7 . . ? N5 C8 H8 111.7 . . ? C9 C8 H8 111.7 . . ? N8 C9 N6 114.3(3) . . ? N8 C9 C8 103.6(3) . . ? N6 C9 C8 103.0(3) . . ? N8 C9 H9 111.8 . . ? N6 C9 H9 111.8 . . ? C8 C9 H9 111.8 . . ? O6 C10 N7 125.1(4) . . ? O6 C10 N8 126.3(4) . . ? N7 C10 N8 108.6(3) . . ? N9 C11 N6 114.7(3) . . ? N9 C11 H11A 108.6 . . ? N6 C11 H11A 108.6 . . ? N9 C11 H11B 108.6 . . ? N6 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? N11 C12 N8 113.5(3) . . ? N11 C12 H12A 108.9 . . ? N8 C12 H12A 108.9 . . ? N11 C12 H12B 108.9 . . ? N8 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? O3 C13 N9 125.3(3) . . ? O3 C13 N10 125.2(3) . . ? N9 C13 N10 109.4(3) . . ? N9 C14 N11 115.3(3) . . ? N9 C14 C15 103.7(3) . . ? N11 C14 C15 102.6(3) . . ? N9 C14 H14 111.5 . . ? N11 C14 H14 111.5 . . ? C15 C14 H14 111.5 . . ? N12 C15 N10 113.8(3) . . ? N12 C15 C14 103.6(3) . . ? N10 C15 C14 103.2(3) . . ? N12 C15 H15 111.8 . . ? N10 C15 H15 111.8 . . ? C14 C15 H15 111.8 . . ? O7 C16 N12 125.0(4) . . ? O7 C16 N11 126.6(4) . . ? N12 C16 N11 108.3(3) . . ? N13 C17 N10 114.2(3) . . ? N13 C17 H17A 108.7 . . ? N10 C17 H17A 108.7 . . ? N13 C17 H17B 108.7 . . ? N10 C17 H17B 108.7 . . ? H17A C17 H17B 107.6 . . ? N15 C18 N12 113.1(3) . . ? N15 C18 H18A 109.0 . . ? N12 C18 H18A 109.0 . . ? N15 C18 H18B 109.0 . . ? N12 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? O4 C19 N13 124.8(3) . . ? O4 C19 N14 126.6(3) . . ? N13 C19 N14 108.6(3) . . ? N15 C20 N13 113.5(3) . . ? N15 C20 C21 104.2(3) . . ? N13 C20 C21 102.9(3) . . ? N15 C20 H20 111.9 . . ? N13 C20 H20 111.9 . . ? C21 C20 H20 111.9 . . ? N14 C21 N16 114.7(3) . . ? N14 C21 C20 103.4(3) . . ? N16 C21 C20 102.3(3) . . ? N14 C21 H21 111.9 . . ? N16 C21 H21 111.9 . . ? C20 C21 H21 111.9 . . ? O8 C22 N15 125.3(4) . . ? O8 C22 N16 125.9(4) . . ? N15 C22 N16 108.8(3) . . ? N3 C23 N14 114.2(3) . 4_666 ? N3 C23 H23A 108.7 . . ? N14 C23 H23A 108.7 4_666 . ? N3 C23 H23B 108.7 . . ? N14 C23 H23B 108.7 4_666 . ? H23A C23 H23B 107.6 . . ? N16 C24 N1 112.8(3) 4_666 . ? N16 C24 H24A 109.0 4_666 . ? N1 C24 H24A 109.0 . . ? N16 C24 H24B 109.0 4_666 . ? N1 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? C1 N1 C2 112.2(3) . . ? C1 N1 C24 121.6(3) . . ? C2 N1 C24 122.9(3) . . ? C1 N2 C3 112.0(3) . . ? C1 N2 C5 123.1(3) . . ? C3 N2 C5 121.7(3) . . ? C4 N3 C23 123.1(3) . . ? C4 N3 C2 112.0(3) . . ? C23 N3 C2 124.0(3) . . ? C4 N4 C6 120.3(3) . . ? C4 N4 C3 111.7(3) . . ? C6 N4 C3 121.4(3) . . ? C7 N5 C5 121.7(3) . . ? C7 N5 C8 113.0(3) . . ? C5 N5 C8 122.6(3) . . ? C7 N6 C11 122.7(3) . . ? C7 N6 C9 112.7(3) . . ? C11 N6 C9 122.9(3) . . ? C10 N7 C8 112.1(3) . . ? C10 N7 C6 121.8(3) . . ? C8 N7 C6 122.1(3) . . ? C10 N8 C9 112.4(3) . . ? C10 N8 C12 122.2(3) . . ? C9 N8 C12 123.8(3) . . ? C13 N9 C11 123.6(3) . . ? C13 N9 C14 111.9(3) . . ? C11 N9 C14 124.3(3) . . ? C13 N10 C17 120.5(3) . . ? C13 N10 C15 110.8(3) . . ? C17 N10 C15 121.1(3) . . ? C16 N11 C12 121.9(3) . . ? C16 N11 C14 111.8(3) . . ? C12 N11 C14 123.7(3) . . ? C16 N12 C15 112.9(3) . . ? C16 N12 C18 123.1(3) . . ? C15 N12 C18 123.4(3) . . ? C19 N13 C17 122.5(3) . . ? C19 N13 C20 111.4(3) . . ? C17 N13 C20 121.5(3) . . ? C19 N14 C21 112.7(3) . . ? C19 N14 C23 123.2(3) . 4_666 ? C21 N14 C23 123.9(3) . 4_666 ? C22 N15 C20 111.9(3) . . ? C22 N15 C18 122.5(3) . . ? C20 N15 C18 122.8(3) . . ? C22 N16 C24 121.1(3) . 4_666 ? C22 N16 C21 111.7(3) . . ? C24 N16 C21 122.2(3) 4_666 . ? C19 O4 Na1 146.0(2) . . ? C4 O5 Na1 144.5(2) . 4_666 ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.66 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 2.135 _refine_diff_density_min -0.964 _refine_diff_density_rms 0.091 # 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 0.000 0.000 -0.005 1178 499 ' ' 2 0.314 0.662 0.500 1611 480 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 931660' ####################################################################### # # 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_CCDC931661 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C144 H446 Cl8 N96 O199 Sr4' _chemical_formula_weight 7342.05 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' Sr Sr -1.5307 3.2498 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 18.733(6) _cell_length_b 21.701(7) _cell_length_c 22.301(7) _cell_angle_alpha 118.963(4) _cell_angle_beta 90.299(5) _cell_angle_gamma 104.709(5) _cell_volume 7583(4) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3862 _exptl_absorpt_coefficient_mu 0.903 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8330 _exptl_absorpt_correction_T_max 0.8916 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex2 CCD Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 69347 _diffrn_reflns_av_R_equivalents 0.0713 _diffrn_reflns_av_sigmaI/netI 0.1386 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 25.00 _reflns_number_total 25594 _reflns_number_gt 12059 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1364P)^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 25594 _refine_ls_number_parameters 1487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1384 _refine_ls_R_factor_gt 0.0835 _refine_ls_wR_factor_ref 0.2491 _refine_ls_wR_factor_gt 0.2258 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.968 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl -0.55384(12) -0.10603(18) -0.12679(14) 0.1165(10) Uani 1 1 d . . . Cl2 Cl 0.5175(4) 1.0550(5) 0.6869(4) 0.169(3) Uani 0.50 1 d P . . Cl3 Cl 0.3560(4) 0.2837(5) 0.3862(4) 0.167(3) Uani 0.50 1 d P . . Cl4 Cl -0.4342(4) -0.2173(5) -0.2965(4) 0.178(3) Uani 0.50 1 d P . . Cl5 Cl 0.5363(4) 0.6588(6) 0.4725(5) 0.184(4) Uani 0.50 1 d P . . Cl6 Cl 0.2343(8) 0.4568(4) 0.1097(5) 0.260(7) Uani 0.50 1 d P . . Cl7 Cl 0.4473(6) 0.4285(4) 0.2811(6) 0.283(8) Uani 0.50 1 d P . . O11W O 0.0917(7) 0.8813(6) 0.7211(6) 0.112(5) Uani 0.50 1 d P . . O12W O 0.2092(8) 0.8901(9) 0.7631(6) 0.124(5) Uani 0.50 1 d P . . O1W O 0.2026(3) 0.2267(2) 0.3705(2) 0.0528(13) Uani 1 1 d . . . O2W O 0.1202(4) 0.4362(3) 0.5203(3) 0.093(2) Uani 1 1 d . . . O3W O 0.1089(3) 0.4128(3) 0.3796(3) 0.0649(14) Uani 1 1 d . . . O4W O -0.0221(5) 0.8256(5) 0.6493(5) 0.164(4) Uani 1 1 d . . . O5W O -0.0193(4) 0.3122(7) 0.4364(6) 0.208(5) Uani 1 1 d . . . O6W O 0.3265(3) 0.8398(2) 0.7330(2) 0.0738(16) Uani 1 1 d . . . O7W O 0.3566(4) 1.0067(4) 0.7887(4) 0.124(3) Uani 1 1 d . . . O8W O 0.3821(4) 0.9201(4) 0.6238(4) 0.125(3) Uani 1 1 d . . . O9W O 0.1600(4) 0.7814(4) 0.6656(3) 0.129(3) Uani 1 1 d . . . O10W O 0.1607(6) 0.8894(4) 0.5950(6) 0.224(6) Uani 1 1 d . . . Sr1 Sr 0.11415(4) 0.31090(4) 0.40564(3) 0.0448(2) Uani 1 1 d . . . Sr2 Sr 0.26483(4) 0.89711(4) 0.67424(4) 0.0561(2) Uani 1 1 d . . . C1 C 0.2889(3) 0.1663(3) 0.1960(3) 0.0342(15) Uani 1 1 d . . . C2 C 0.3745(3) 0.1689(3) 0.1218(3) 0.0345(15) Uani 1 1 d . . . H2 H 0.4278 0.1836 0.1390 0.041 Uiso 1 1 calc R . . C3 C 0.3447(3) 0.2351(3) 0.1467(3) 0.0345(15) Uani 1 1 d . . . H3 H 0.3852 0.2815 0.1691 0.041 Uiso 1 1 calc R . . C4 C 0.3199(3) 0.1651(3) 0.0251(3) 0.0408(16) Uani 1 1 d . . . C5 C 0.2667(3) 0.2883(3) 0.2427(3) 0.0369(15) Uani 1 1 d . . . H5A H 0.3059 0.3346 0.2608 0.044 Uiso 1 1 calc R . . H5B H 0.2543 0.2810 0.2814 0.044 Uiso 1 1 calc R . . C6 C 0.2842(4) 0.2798(4) 0.0771(3) 0.0433(17) Uani 1 1 d . . . H6A H 0.3219 0.3268 0.1053 0.052 Uiso 1 1 calc R . . H6B H 0.2815 0.2690 0.0294 0.052 Uiso 1 1 calc R . . C7 C 0.1346(3) 0.2829(3) 0.2336(3) 0.0345(15) Uani 1 1 d . . . C8 C 0.2070(3) 0.3310(3) 0.1735(3) 0.0315(14) Uani 1 1 d . . . H8 H 0.2462 0.3784 0.1959 0.038 Uiso 1 1 calc R . . C9 C 0.1282(3) 0.3408(3) 0.1701(3) 0.0349(15) Uani 1 1 d . . . H9 H 0.1303 0.3929 0.1942 0.042 Uiso 1 1 calc R . . C10 C 0.1547(4) 0.2771(3) 0.0570(3) 0.0417(16) Uani 1 1 d . . . C11 C 0.0190(3) 0.3161(3) 0.2289(3) 0.0349(15) Uani 1 1 d . . . H11A H 0.0247 0.3685 0.2512 0.042 Uiso 1 1 calc R . . H11B H 0.0102 0.3015 0.2637 0.042 Uiso 1 1 calc R . . C12 C 0.0449(3) 0.3237(3) 0.0696(3) 0.0359(15) Uani 1 1 d . . . H12A H 0.0516 0.3762 0.0972 0.043 Uiso 1 1 calc R . . H12B H 0.0502 0.3121 0.0223 0.043 Uiso 1 1 calc R . . C13 C -0.1057(3) 0.2322(4) 0.1789(3) 0.0355(15) Uani 1 1 d . . . C14 C -0.0638(3) 0.3058(3) 0.1329(3) 0.0332(15) Uani 1 1 d . . . H14 H -0.0545 0.3593 0.1601 0.040 Uiso 1 1 calc R . . C15 C -0.1480(3) 0.2653(3) 0.1044(3) 0.0347(15) Uani 1 1 d . . . H15 H -0.1783 0.2994 0.1174 0.042 Uiso 1 1 calc R . . C16 C -0.0815(4) 0.2392(3) 0.0113(3) 0.0351(15) Uani 1 1 d . . . C17 C -0.2416(4) 0.1803(4) 0.1365(3) 0.062(2) Uani 1 1 d . . . H17A H -0.2413 0.1698 0.1741 0.075 Uiso 1 1 calc R . . H17B H -0.2730 0.2123 0.1455 0.075 Uiso 1 1 calc R . . C18 C -0.2180(4) 0.1910(3) -0.0201(3) 0.0417(17) Uani 1 1 d . . . H18A H -0.2493 0.2236 -0.0035 0.050 Uiso 1 1 calc R . . H18B H -0.2052 0.1860 -0.0640 0.050 Uiso 1 1 calc R . . C19 C -0.2986(3) 0.0479(4) 0.0716(3) 0.0463(18) Uani 1 1 d . . . C20 C -0.3111(3) 0.1089(4) 0.0120(3) 0.0421(17) Uani 1 1 d . . . H20 H -0.3437 0.1409 0.0249 0.051 Uiso 1 1 calc R . . C21 C -0.3548(3) 0.0270(3) -0.0312(3) 0.0283(13) Uani 1 1 d . . . H21 H -0.4078 0.0206 -0.0423 0.034 Uiso 1 1 calc R . . C22 C -0.2649(4) 0.0576(3) -0.0928(3) 0.0368(16) Uani 1 1 d . . . C23 C -0.3880(4) -0.0737(3) -0.0005(3) 0.0424(16) Uani 1 1 d . . . H23A H -0.4390 -0.0833 -0.0191 0.051 Uiso 1 1 calc R . . H23B H -0.3887 -0.0725 0.0436 0.051 Uiso 1 1 calc R . . C24 C -0.3485(4) -0.0691(3) -0.1548(3) 0.0419(16) Uani 1 1 d . . . H24A H -0.3285 -0.0656 -0.1934 0.050 Uiso 1 1 calc R . . H24B H -0.4025 -0.0817 -0.1640 0.050 Uiso 1 1 calc R . . C25 C -0.1652(3) 0.4723(3) 0.2659(3) 0.0353(15) Uani 1 1 d . . . C26 C -0.2275(3) 0.5600(3) 0.3228(3) 0.0275(13) Uani 1 1 d . . . H26 H -0.2710 0.5592 0.2975 0.033 Uiso 1 1 calc R . . C27 C -0.1548(3) 0.5960(3) 0.3077(3) 0.0314(14) Uani 1 1 d . . . H27 H -0.1626 0.6188 0.2805 0.038 Uiso 1 1 calc R . . C28 C -0.1570(4) 0.6572(3) 0.4277(3) 0.0345(15) Uani 1 1 d . . . C29 C -0.0642(3) 0.5386(3) 0.2293(3) 0.0328(14) Uani 1 1 d . . . H29A H -0.0735 0.5636 0.2053 0.039 Uiso 1 1 calc R . . H29B H -0.0663 0.4886 0.1947 0.039 Uiso 1 1 calc R . . C30 C -0.0487(3) 0.7114(3) 0.3882(3) 0.0389(16) Uani 1 1 d . . . H30A H -0.0425 0.7523 0.4350 0.047 Uiso 1 1 calc R . . H30B H -0.0582 0.7279 0.3563 0.047 Uiso 1 1 calc R . . C31 C 0.0646(3) 0.5412(3) 0.2612(3) 0.0333(14) Uani 1 1 d . . . C32 C 0.0410(3) 0.6541(3) 0.3077(3) 0.0303(14) Uani 1 1 d . . . H32 H 0.0305 0.6762 0.2806 0.036 Uiso 1 1 calc R . . C33 C 0.1249(3) 0.6676(3) 0.3235(3) 0.0345(15) Uani 1 1 d . . . H33 H 0.1537 0.6927 0.3009 0.041 Uiso 1 1 calc R . . C34 C 0.0804(4) 0.7253(3) 0.4278(4) 0.0437(17) Uani 1 1 d . . . C35 C 0.2006(3) 0.5764(3) 0.2858(3) 0.0359(15) Uani 1 1 d . . . H35A H 0.1916 0.5256 0.2493 0.043 Uiso 1 1 calc R . . H35B H 0.2321 0.6075 0.2704 0.043 Uiso 1 1 calc R . . C36 C 0.2190(3) 0.7510(3) 0.4339(3) 0.0381(16) Uani 1 1 d . . . H36A H 0.2486 0.7672 0.4058 0.046 Uiso 1 1 calc R . . H36B H 0.2184 0.7945 0.4770 0.046 Uiso 1 1 calc R . . C37 C 0.2491(3) 0.5295(3) 0.3530(3) 0.0303(14) Uani 1 1 d . . . C38 C 0.2904(3) 0.6571(3) 0.3980(3) 0.0335(14) Uani 1 1 d . . . H38 H 0.3240 0.6807 0.3766 0.040 Uiso 1 1 calc R . . C39 C 0.3341(3) 0.6365(3) 0.4422(3) 0.0309(14) Uani 1 1 d . . . H39 H 0.3878 0.6489 0.4404 0.037 Uiso 1 1 calc R . . C40 C 0.2743(3) 0.7225(3) 0.5146(3) 0.0383(15) Uani 1 1 d . . . C41 C 0.3345(3) 0.5119(3) 0.4227(3) 0.0374(16) Uani 1 1 d . . . H41A H 0.3880 0.5287 0.4242 0.045 Uiso 1 1 calc R . . H41B H 0.3161 0.4620 0.3838 0.045 Uiso 1 1 calc R . . C42 C 0.3614(3) 0.6922(3) 0.5732(3) 0.0384(16) Uani 1 1 d . . . H42A H 0.4133 0.6998 0.5665 0.046 Uiso 1 1 calc R . . H42B H 0.3577 0.7369 0.6134 0.046 Uiso 1 1 calc R . . C43 C 0.2869(3) 0.4472(3) 0.4859(3) 0.0316(14) Uani 1 1 d . . . C44 C 0.3638(3) 0.5689(3) 0.5536(3) 0.0303(14) Uani 1 1 d . . . H44 H 0.4173 0.5813 0.5510 0.036 Uiso 1 1 calc R . . C45 C 0.3445(3) 0.5329(3) 0.5994(3) 0.0328(14) Uani 1 1 d . . . H45 H 0.3896 0.5342 0.6230 0.039 Uiso 1 1 calc R . . C46 C 0.3041(3) 0.6370(3) 0.6432(3) 0.0386(16) Uani 1 1 d . . . C47 C 0.2860(3) 0.3987(3) 0.5650(3) 0.0319(14) Uani 1 1 d . . . H47A H 0.3304 0.4046 0.5922 0.038 Uiso 1 1 calc R . . H47B H 0.2764 0.3524 0.5217 0.038 Uiso 1 1 calc R . . C48 C 0.2878(4) 0.5732(4) 0.7093(3) 0.0445(17) Uani 1 1 d . . . H48A H 0.2809 0.6196 0.7440 0.053 Uiso 1 1 calc R . . H48B H 0.3312 0.5674 0.7275 0.053 Uiso 1 1 calc R . . C49 C 0.2910(4) 0.9789(4) 0.4806(4) 0.0439(17) Uani 1 1 d . . . C50 C 0.3332(3) 1.0468(3) 0.4240(3) 0.0317(14) Uani 1 1 d . . . H50 H 0.3755 1.0399 0.3984 0.038 Uiso 1 1 calc R . . C51 C 0.3590(4) 1.0951(3) 0.5008(3) 0.0365(15) Uani 1 1 d . . . H51 H 0.4133 1.1166 0.5121 0.044 Uiso 1 1 calc R . . C52 C 0.2851(3) 1.1459(3) 0.4628(3) 0.0337(14) Uani 1 1 d . . . C53 C 0.3592(4) 1.0627(4) 0.5961(3) 0.0457(17) Uani 1 1 d . . . H53A H 0.4126 1.0859 0.6055 0.055 Uiso 1 1 calc R . . H53B H 0.3508 1.0161 0.5948 0.055 Uiso 1 1 calc R . . C54 C 0.3397(4) 1.2207(3) 0.5867(3) 0.0382(15) Uani 1 1 d . . . H54A H 0.3936 1.2395 0.5984 0.046 Uiso 1 1 calc R . . H54B H 0.3219 1.2570 0.5827 0.046 Uiso 1 1 calc R . . C55 C 0.2852(4) 1.0858(4) 0.6910(3) 0.0413(17) Uani 1 1 d . . . C56 C 0.3431(3) 1.1880(3) 0.6809(3) 0.0385(16) Uani 1 1 d . . . H56 H 0.3971 1.2118 0.6926 0.046 Uiso 1 1 calc R . . C57 C 0.3047(3) 1.2108(4) 0.7482(3) 0.0412(16) Uani 1 1 d . . . H57 H 0.3416 1.2427 0.7904 0.049 Uiso 1 1 calc R . . C58 C 0.2621(3) 1.2523(3) 0.6779(3) 0.0379(15) Uani 1 1 d . . . C59 C 0.2366(4) 1.1389(4) 0.8009(4) 0.0499(18) Uani 1 1 d . . . H59A H 0.2685 1.1776 0.8439 0.060 Uiso 1 1 calc R . . H59B H 0.2355 1.0920 0.7967 0.060 Uiso 1 1 calc R . . C60 C 0.2226(3) 1.2969(3) 0.7943(3) 0.0365(15) Uani 1 1 d . . . H60A H 0.2563 1.3227 0.8378 0.044 Uiso 1 1 calc R . . H60B H 0.2132 1.3336 0.7849 0.044 Uiso 1 1 calc R . . C61 C 0.0978(4) 1.0880(4) 0.7871(4) 0.0497(18) Uani 1 1 d . . . C62 C 0.1458(3) 1.2172(3) 0.8403(3) 0.0362(15) Uani 1 1 d . . . H62 H 0.1758 1.2488 0.8865 0.043 Uiso 1 1 calc R . . C63 C 0.0619(3) 1.1959(3) 0.8445(3) 0.0368(15) Uani 1 1 d . . . H63 H 0.0528 1.2165 0.8927 0.044 Uiso 1 1 calc R . . C64 C 0.0868(3) 1.2651(3) 0.7880(3) 0.0286(14) Uani 1 1 d . . . C65 C -0.0298(3) 1.0730(3) 0.8134(3) 0.0368(15) Uani 1 1 d . . . H65A H -0.0242 1.0255 0.8022 0.044 Uiso 1 1 calc R . . H65B H -0.0388 1.0969 0.8611 0.044 Uiso 1 1 calc R . . C66 C -0.0412(3) 1.2371(3) 0.8127(3) 0.0356(15) Uani 1 1 d . . . H66A H -0.0515 1.2544 0.8598 0.043 Uiso 1 1 calc R . . H66B H -0.0431 1.2743 0.8009 0.043 Uiso 1 1 calc R . . C67 C -0.1388(3) 0.9915(3) 0.7244(3) 0.0334(14) Uani 1 1 d . . . C68 C -0.1328(3) 1.1164(3) 0.7864(3) 0.0313(14) Uani 1 1 d . . . H68 H -0.1401 1.1397 0.8352 0.038 Uiso 1 1 calc R . . C69 C -0.2070(3) 1.0728(3) 0.7376(3) 0.0355(15) Uani 1 1 d . . . H69 H -0.2501 1.0784 0.7624 0.043 Uiso 1 1 calc R . . C70 C -0.1413(3) 1.1617(3) 0.7118(3) 0.0354(15) Uani 1 1 d . . . C71 C 0.2696(3) 1.0664(3) 0.3348(3) 0.0374(15) Uani 1 1 d . . . H71A H 0.3111 1.0561 0.3096 0.045 Uiso 1 1 calc R . . H71B H 0.2608 1.1090 0.3358 0.045 Uiso 1 1 calc R . . C72 C -0.2680(3) 1.0911(3) 0.6477(3) 0.0408(16) Uani 1 1 d . . . H72A H -0.3100 1.0928 0.6731 0.049 Uiso 1 1 calc R . . H72B H -0.2592 1.1311 0.6378 0.049 Uiso 1 1 calc R . . N1 N 0.3287(3) 0.1272(3) 0.1501(2) 0.0325(12) Uani 1 1 d . . . N2 N 0.2950(3) 0.2300(3) 0.1953(2) 0.0372(13) Uani 1 1 d . . . N3 N 0.3597(3) 0.1329(3) 0.0474(2) 0.0420(13) Uani 1 1 d . . . N4 N 0.3066(3) 0.2226(3) 0.0821(2) 0.0375(12) Uani 1 1 d . . . N5 N 0.2020(3) 0.2941(2) 0.2132(2) 0.0323(12) Uani 1 1 d . . . N6 N 0.0872(3) 0.3031(3) 0.2038(2) 0.0330(12) Uani 1 1 d . . . N7 N 0.2125(3) 0.2860(3) 0.0997(2) 0.0345(12) Uani 1 1 d . . . N8 N 0.1034(3) 0.3057(3) 0.0964(2) 0.0329(12) Uani 1 1 d . . . N9 N -0.0451(3) 0.2769(3) 0.1753(2) 0.0337(12) Uani 1 1 d . . . N10 N -0.1639(3) 0.2206(3) 0.1368(3) 0.0437(14) Uani 1 1 d . . . N11 N -0.0290(3) 0.2847(3) 0.0705(2) 0.0338(12) Uani 1 1 d . . . N12 N -0.1482(3) 0.2251(3) 0.0307(2) 0.0357(12) Uani 1 1 d . . . N13 N -0.2739(3) 0.1127(3) 0.0731(2) 0.0419(13) Uani 1 1 d . . . N14 N -0.3446(3) -0.0033(3) 0.0111(2) 0.0368(13) Uani 1 1 d . . . N15 N -0.2589(3) 0.1212(3) -0.0309(2) 0.0362(12) Uani 1 1 d . . . N16 N -0.3209(3) 0.0015(3) -0.0924(2) 0.0349(12) Uani 1 1 d . . . N17 N -0.2235(3) 0.4857(2) 0.3008(2) 0.0321(12) Uani 1 1 d . . . N18 N -0.1205(3) 0.5366(2) 0.2709(2) 0.0320(12) Uani 1 1 d . . . N19 N -0.2228(3) 0.6053(2) 0.3972(2) 0.0338(12) Uani 1 1 d . . . N20 N -0.1121(3) 0.6513(2) 0.3781(2) 0.0294(11) Uani 1 1 d . . . N21 N 0.0104(3) 0.5764(2) 0.2703(2) 0.0323(12) Uani 1 1 d . . . N22 N 0.1307(3) 0.5929(2) 0.2955(2) 0.0309(12) Uani 1 1 d . . . N23 N 0.0198(3) 0.6900(2) 0.3769(2) 0.0340(12) Uani 1 1 d . . . N24 N 0.1427(3) 0.7111(3) 0.3973(3) 0.0387(13) Uani 1 1 d . . . N25 N 0.2397(3) 0.5869(2) 0.3464(2) 0.0309(12) Uani 1 1 d . . . N26 N 0.3001(3) 0.5587(2) 0.4113(2) 0.0345(12) Uani 1 1 d . . . N27 N 0.2531(3) 0.7076(3) 0.4486(2) 0.0363(12) Uani 1 1 d . . . N28 N 0.3168(3) 0.6804(2) 0.5120(2) 0.0353(12) Uani 1 1 d . . . N29 N 0.3201(2) 0.5111(2) 0.4865(2) 0.0290(11) Uani 1 1 d . . . N30 N 0.3004(3) 0.4575(2) 0.5501(2) 0.0293(11) Uani 1 1 d . . . N31 N 0.3391(3) 0.6327(2) 0.5870(2) 0.0337(12) Uani 1 1 d . . . N32 N 0.3026(3) 0.5772(3) 0.6484(2) 0.0359(12) Uani 1 1 d . . . N33 N 0.2870(3) 0.9772(3) 0.4164(2) 0.0355(12) Uani 1 1 d . . . N34 N 0.3314(3) 1.0487(3) 0.5301(2) 0.0353(12) Uani 1 1 d . . . N35 N 0.2902(3) 1.0842(2) 0.4055(2) 0.0339(12) Uani 1 1 d . . . N36 N 0.3195(3) 1.1517(2) 0.5197(2) 0.0345(12) Uani 1 1 d . . . N37 N 0.3259(3) 1.1090(3) 0.6522(2) 0.0374(13) Uani 1 1 d . . . N38 N 0.2680(3) 1.1432(3) 0.7437(3) 0.0378(13) Uani 1 1 d . . . N39 N 0.3087(3) 1.2109(3) 0.6417(2) 0.0333(12) Uani 1 1 d . . . N40 N 0.2581(3) 1.2504(3) 0.7389(2) 0.0380(13) Uani 1 1 d . . . N41 N 0.1605(3) 1.1462(3) 0.8041(3) 0.0381(13) Uani 1 1 d . . . N42 N 0.0386(3) 1.1165(3) 0.8081(3) 0.0383(13) Uani 1 1 d . . . N43 N 0.1527(3) 1.2548(3) 0.8013(2) 0.0355(12) Uani 1 1 d . . . N44 N 0.0330(3) 1.2296(3) 0.8101(2) 0.0347(12) Uani 1 1 d . . . N45 N -0.0933(3) 1.0612(3) 0.7698(3) 0.0374(13) Uani 1 1 d . . . N46 N -0.2034(3) 0.9965(2) 0.7022(2) 0.0323(12) Uani 1 1 d . . . N47 N -0.0988(3) 1.1702(3) 0.7670(2) 0.0370(13) Uani 1 1 d . . . N48 N -0.2030(3) 1.1025(3) 0.6907(2) 0.0380(13) Uani 1 1 d . . . O1 O 0.2516(2) 0.1494(2) 0.2338(2) 0.0418(11) Uani 1 1 d . . . O2 O 0.1183(2) 0.2594(2) 0.2740(2) 0.0396(10) Uani 1 1 d . . . O3 O -0.1058(3) 0.1987(3) 0.2133(2) 0.0589(13) Uani 1 1 d . . . O4 O -0.2809(3) 0.0375(3) 0.1195(2) 0.0646(14) Uani 1 1 d . . . O5 O 0.3008(3) 0.1461(3) -0.0353(2) 0.0639(14) Uani 1 1 d . . . O6 O 0.1495(3) 0.2475(3) -0.0062(2) 0.0523(12) Uani 1 1 d . . . O7 O -0.0659(2) 0.2179(2) -0.0485(2) 0.0422(11) Uani 1 1 d . . . O8 O -0.2284(2) 0.0522(2) -0.1396(2) 0.0446(11) Uani 1 1 d . . . O9 O -0.1513(2) 0.4122(2) 0.2365(2) 0.0489(12) Uani 1 1 d . . . O10 O 0.0532(2) 0.4741(2) 0.2262(2) 0.0455(11) Uani 1 1 d . . . O11 O 0.2167(2) 0.4661(2) 0.3151(2) 0.0422(11) Uani 1 1 d . . . O12 O 0.2521(2) 0.3894(2) 0.4347(2) 0.0368(10) Uani 1 1 d . . . O13 O -0.1387(2) 0.7039(2) 0.49002(19) 0.0357(10) Uani 1 1 d . . . O14 O 0.0799(2) 0.7629(2) 0.4896(2) 0.0507(12) Uani 1 1 d . . . O15 O 0.2587(2) 0.7696(2) 0.5676(2) 0.0506(12) Uani 1 1 d . . . O16 O 0.2804(2) 0.6879(2) 0.6822(2) 0.0464(11) Uani 1 1 d . . . O17 O 0.2641(3) 0.9253(3) 0.4869(2) 0.0569(13) Uani 1 1 d . . . O18 O 0.2674(3) 1.0223(3) 0.6791(3) 0.0592(13) Uani 1 1 d . . . O19 O 0.0944(2) 1.0230(2) 0.7597(3) 0.0568(13) Uani 1 1 d . . . O20 O -0.1235(2) 0.9337(2) 0.7061(2) 0.0423(11) Uani 1 1 d . . . O21 O 0.2543(2) 1.1894(2) 0.4634(2) 0.0478(12) Uani 1 1 d . . . O22 O 0.2303(3) 1.2827(2) 0.6588(2) 0.0485(12) Uani 1 1 d . . . O23 O 0.0779(2) 1.3007(2) 0.7614(2) 0.0470(11) Uani 1 1 d . . . O24 O -0.1269(2) 1.2004(2) 0.6850(2) 0.0497(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0507(13) 0.183(3) 0.106(2) 0.061(2) 0.0282(13) 0.0413(16) Cl2 0.141(6) 0.219(8) 0.142(6) 0.093(6) 0.018(5) 0.039(6) Cl3 0.150(6) 0.208(8) 0.182(7) 0.110(7) 0.075(6) 0.089(6) Cl4 0.122(5) 0.204(8) 0.137(6) 0.032(6) -0.001(5) 0.051(5) Cl5 0.081(4) 0.297(11) 0.229(9) 0.168(9) 0.049(5) 0.068(6) Cl6 0.437(18) 0.115(6) 0.201(9) 0.089(6) 0.168(11) 0.018(8) Cl7 0.224(10) 0.087(5) 0.298(12) -0.036(6) 0.139(9) -0.051(6) O11W 0.099(9) 0.064(8) 0.093(9) -0.005(7) -0.054(8) -0.007(7) O12W 0.108(10) 0.176(14) 0.075(9) 0.036(9) 0.014(8) 0.079(10) O1W 0.094(4) 0.041(3) 0.026(2) 0.011(2) 0.012(2) 0.036(3) O2W 0.158(6) 0.111(5) 0.058(3) 0.050(3) 0.049(4) 0.097(4) O3W 0.071(3) 0.056(3) 0.071(3) 0.035(3) 0.002(3) 0.019(3) O4W 0.121(6) 0.137(7) 0.207(9) 0.106(7) -0.017(6) -0.045(5) O5W 0.080(6) 0.316(14) 0.266(12) 0.161(11) 0.088(7) 0.083(7) O6W 0.132(5) 0.045(3) 0.042(3) 0.018(2) 0.011(3) 0.029(3) O7W 0.132(6) 0.118(6) 0.102(5) 0.061(5) -0.016(5) -0.003(5) O8W 0.094(5) 0.097(5) 0.203(8) 0.081(5) 0.062(5) 0.045(4) O9W 0.145(6) 0.112(5) 0.091(5) 0.036(4) 0.065(5) 0.003(5) O10W 0.234(10) 0.075(5) 0.258(11) 0.009(6) -0.178(9) 0.040(6) Sr1 0.0490(4) 0.0555(4) 0.0364(4) 0.0261(3) 0.0098(3) 0.0190(3) Sr2 0.0669(5) 0.0498(4) 0.0520(4) 0.0241(4) 0.0105(4) 0.0207(4) C1 0.024(3) 0.038(4) 0.031(4) 0.010(3) -0.001(3) 0.009(3) C2 0.029(3) 0.049(4) 0.027(3) 0.017(3) 0.009(3) 0.020(3) C3 0.025(3) 0.046(4) 0.038(4) 0.025(3) 0.010(3) 0.012(3) C4 0.039(4) 0.049(4) 0.030(4) 0.014(3) 0.012(3) 0.018(3) C5 0.043(4) 0.047(4) 0.025(3) 0.017(3) 0.009(3) 0.023(3) C6 0.050(4) 0.065(5) 0.040(4) 0.037(4) 0.025(3) 0.032(4) C7 0.038(4) 0.041(4) 0.024(3) 0.011(3) 0.005(3) 0.022(3) C8 0.036(3) 0.034(3) 0.027(3) 0.015(3) 0.013(3) 0.017(3) C9 0.033(3) 0.042(4) 0.028(3) 0.015(3) 0.005(3) 0.014(3) C10 0.047(4) 0.039(4) 0.044(4) 0.025(3) 0.014(3) 0.012(3) C11 0.032(3) 0.047(4) 0.025(3) 0.018(3) 0.007(3) 0.013(3) C12 0.040(4) 0.044(4) 0.037(4) 0.026(3) 0.007(3) 0.020(3) C13 0.022(3) 0.049(4) 0.025(3) 0.012(3) 0.006(3) 0.009(3) C14 0.036(3) 0.036(3) 0.024(3) 0.005(3) 0.009(3) 0.027(3) C15 0.028(3) 0.038(4) 0.021(3) 0.003(3) 0.003(3) 0.008(3) C16 0.045(4) 0.027(3) 0.020(3) 0.004(3) -0.008(3) 0.007(3) C17 0.038(4) 0.091(6) 0.020(3) 0.009(4) 0.016(3) -0.001(4) C18 0.057(4) 0.036(4) 0.027(3) 0.013(3) -0.005(3) 0.012(3) C19 0.023(4) 0.074(5) 0.041(4) 0.030(4) 0.020(3) 0.014(4) C20 0.040(4) 0.053(4) 0.025(3) 0.013(3) 0.005(3) 0.015(3) C21 0.032(3) 0.028(3) 0.018(3) 0.007(3) 0.002(3) 0.007(3) C22 0.045(4) 0.034(4) 0.025(4) 0.009(3) 0.002(3) 0.014(3) C23 0.050(4) 0.039(4) 0.049(4) 0.027(3) 0.029(3) 0.019(3) C24 0.054(4) 0.041(4) 0.030(3) 0.019(3) 0.007(3) 0.009(3) C25 0.039(4) 0.040(4) 0.027(3) 0.016(3) 0.008(3) 0.013(3) C26 0.034(3) 0.027(3) 0.024(3) 0.013(3) 0.011(3) 0.011(3) C27 0.045(4) 0.029(3) 0.021(3) 0.012(3) 0.006(3) 0.014(3) C28 0.049(4) 0.035(4) 0.033(4) 0.024(3) 0.012(3) 0.020(3) C29 0.034(4) 0.037(4) 0.022(3) 0.013(3) 0.014(3) 0.006(3) C30 0.037(4) 0.031(4) 0.038(4) 0.013(3) 0.003(3) 0.002(3) C31 0.040(4) 0.037(4) 0.033(3) 0.023(3) 0.017(3) 0.017(3) C32 0.028(3) 0.028(3) 0.034(3) 0.016(3) 0.003(3) 0.006(3) C33 0.044(4) 0.021(3) 0.038(4) 0.015(3) 0.005(3) 0.007(3) C34 0.050(4) 0.031(4) 0.055(5) 0.029(4) 0.004(4) 0.004(3) C35 0.045(4) 0.039(4) 0.034(3) 0.021(3) 0.016(3) 0.020(3) C36 0.039(4) 0.020(3) 0.040(4) 0.008(3) -0.008(3) 0.002(3) C37 0.047(4) 0.020(3) 0.025(3) 0.012(3) 0.014(3) 0.007(3) C38 0.040(4) 0.022(3) 0.035(3) 0.014(3) 0.004(3) 0.004(3) C39 0.029(3) 0.034(4) 0.032(3) 0.018(3) 0.007(3) 0.010(3) C40 0.038(4) 0.034(4) 0.036(4) 0.016(3) 0.005(3) 0.005(3) C41 0.046(4) 0.049(4) 0.024(3) 0.016(3) 0.016(3) 0.028(3) C42 0.039(4) 0.035(4) 0.029(3) 0.010(3) 0.000(3) 0.004(3) C43 0.036(4) 0.038(4) 0.027(4) 0.017(3) 0.010(3) 0.022(3) C44 0.018(3) 0.045(4) 0.036(3) 0.027(3) 0.007(3) 0.010(3) C45 0.024(3) 0.040(4) 0.035(3) 0.019(3) 0.006(3) 0.009(3) C46 0.036(4) 0.036(4) 0.038(4) 0.013(3) 0.001(3) 0.012(3) C47 0.033(3) 0.037(4) 0.034(3) 0.019(3) 0.017(3) 0.021(3) C48 0.059(5) 0.052(4) 0.022(3) 0.018(3) 0.013(3) 0.017(4) C49 0.049(4) 0.051(5) 0.057(5) 0.039(4) 0.018(4) 0.028(4) C50 0.032(3) 0.033(4) 0.035(3) 0.021(3) 0.006(3) 0.009(3) C51 0.046(4) 0.026(3) 0.043(4) 0.020(3) 0.010(3) 0.014(3) C52 0.038(4) 0.035(4) 0.035(4) 0.026(3) 0.011(3) 0.005(3) C53 0.058(4) 0.055(4) 0.035(4) 0.024(3) 0.007(3) 0.030(4) C54 0.057(4) 0.020(3) 0.028(3) 0.011(3) 0.011(3) -0.001(3) C55 0.042(4) 0.057(5) 0.043(4) 0.034(4) 0.010(3) 0.025(4) C56 0.033(4) 0.049(4) 0.042(4) 0.032(3) 0.004(3) 0.008(3) C57 0.029(3) 0.058(5) 0.036(4) 0.027(3) 0.004(3) 0.007(3) C58 0.046(4) 0.030(4) 0.032(4) 0.015(3) -0.001(3) 0.003(3) C59 0.055(4) 0.066(5) 0.055(4) 0.043(4) 0.019(4) 0.031(4) C60 0.042(4) 0.035(4) 0.033(3) 0.020(3) 0.007(3) 0.006(3) C61 0.062(5) 0.071(6) 0.052(4) 0.051(4) 0.026(4) 0.031(5) C62 0.032(4) 0.052(4) 0.035(3) 0.031(3) 0.007(3) 0.008(3) C63 0.035(4) 0.059(4) 0.030(3) 0.030(3) 0.011(3) 0.020(3) C64 0.031(3) 0.026(3) 0.029(3) 0.014(3) 0.002(3) 0.007(3) C65 0.033(4) 0.039(4) 0.041(4) 0.022(3) 0.007(3) 0.012(3) C66 0.033(3) 0.038(4) 0.046(4) 0.025(3) 0.016(3) 0.018(3) C67 0.044(4) 0.034(4) 0.022(3) 0.018(3) 0.001(3) 0.002(3) C68 0.042(4) 0.026(3) 0.031(3) 0.017(3) 0.012(3) 0.012(3) C69 0.033(3) 0.038(4) 0.042(4) 0.020(3) 0.007(3) 0.019(3) C70 0.045(4) 0.023(3) 0.040(4) 0.016(3) -0.003(3) 0.010(3) C71 0.043(4) 0.043(4) 0.039(4) 0.033(3) 0.009(3) 0.007(3) C72 0.037(4) 0.035(4) 0.041(4) 0.016(3) -0.010(3) 0.002(3) N1 0.038(3) 0.037(3) 0.032(3) 0.020(2) 0.019(2) 0.019(2) N2 0.048(3) 0.048(3) 0.026(3) 0.020(3) 0.020(2) 0.027(3) N3 0.050(3) 0.050(3) 0.034(3) 0.019(3) 0.021(3) 0.030(3) N4 0.040(3) 0.051(3) 0.033(3) 0.027(3) 0.014(2) 0.017(3) N5 0.041(3) 0.033(3) 0.029(3) 0.017(2) 0.005(2) 0.017(2) N6 0.030(3) 0.050(3) 0.022(3) 0.021(2) 0.009(2) 0.011(2) N7 0.033(3) 0.054(3) 0.029(3) 0.024(3) 0.015(2) 0.026(3) N8 0.039(3) 0.044(3) 0.016(2) 0.015(2) 0.007(2) 0.014(3) N9 0.032(3) 0.045(3) 0.026(3) 0.021(2) 0.000(2) 0.008(3) N10 0.033(3) 0.063(4) 0.035(3) 0.028(3) 0.014(3) 0.006(3) N11 0.036(3) 0.039(3) 0.021(3) 0.014(2) 0.003(2) 0.006(2) N12 0.031(3) 0.039(3) 0.027(3) 0.011(2) 0.007(2) 0.008(2) N13 0.041(3) 0.049(4) 0.021(3) 0.013(3) 0.002(2) -0.002(3) N14 0.036(3) 0.045(3) 0.019(3) 0.008(2) 0.009(2) 0.012(3) N15 0.044(3) 0.028(3) 0.025(3) 0.010(2) 0.006(2) -0.001(2) N16 0.038(3) 0.037(3) 0.018(3) 0.006(2) 0.007(2) 0.008(3) N17 0.032(3) 0.022(3) 0.034(3) 0.010(2) 0.009(2) 0.002(2) N18 0.034(3) 0.024(3) 0.035(3) 0.012(2) 0.012(2) 0.009(2) N19 0.040(3) 0.027(3) 0.031(3) 0.013(2) -0.002(2) 0.007(2) N20 0.033(3) 0.026(3) 0.025(3) 0.011(2) 0.006(2) 0.006(2) N21 0.032(3) 0.025(3) 0.035(3) 0.013(2) 0.012(2) 0.005(2) N22 0.030(3) 0.023(3) 0.032(3) 0.009(2) 0.000(2) 0.006(2) N23 0.029(3) 0.030(3) 0.039(3) 0.015(2) 0.000(2) 0.008(2) N24 0.037(3) 0.028(3) 0.049(3) 0.018(3) 0.003(3) 0.009(2) N25 0.038(3) 0.027(3) 0.025(3) 0.011(2) 0.003(2) 0.009(2) N26 0.051(3) 0.022(3) 0.032(3) 0.013(2) 0.004(2) 0.014(2) N27 0.039(3) 0.031(3) 0.031(3) 0.009(2) 0.004(2) 0.013(2) N28 0.046(3) 0.027(3) 0.027(3) 0.008(2) 0.010(2) 0.011(2) N29 0.025(3) 0.027(3) 0.032(3) 0.013(2) 0.006(2) 0.007(2) N30 0.035(3) 0.019(3) 0.034(3) 0.014(2) 0.009(2) 0.010(2) N31 0.046(3) 0.023(3) 0.032(3) 0.016(2) 0.008(2) 0.004(2) N32 0.049(3) 0.024(3) 0.025(3) 0.009(2) 0.008(2) 0.002(2) N33 0.038(3) 0.035(3) 0.037(3) 0.022(3) 0.002(2) 0.009(2) N34 0.051(3) 0.031(3) 0.031(3) 0.020(3) 0.003(2) 0.015(3) N35 0.041(3) 0.028(3) 0.034(3) 0.015(2) 0.004(2) 0.012(2) N36 0.055(3) 0.033(3) 0.028(3) 0.022(2) 0.017(2) 0.019(3) N37 0.046(3) 0.042(3) 0.038(3) 0.028(3) 0.017(3) 0.017(3) N38 0.042(3) 0.050(4) 0.046(3) 0.039(3) 0.025(3) 0.020(3) N39 0.039(3) 0.035(3) 0.033(3) 0.020(2) 0.019(2) 0.015(2) N40 0.042(3) 0.052(3) 0.038(3) 0.033(3) 0.022(2) 0.020(3) N41 0.036(3) 0.045(3) 0.053(3) 0.036(3) 0.016(3) 0.017(3) N42 0.033(3) 0.036(3) 0.052(3) 0.026(3) 0.009(3) 0.012(3) N43 0.041(3) 0.041(3) 0.042(3) 0.033(3) 0.022(2) 0.015(3) N44 0.036(3) 0.041(3) 0.041(3) 0.031(3) 0.010(2) 0.009(3) N45 0.036(3) 0.039(3) 0.048(3) 0.028(3) 0.004(3) 0.015(3) N46 0.047(3) 0.025(3) 0.032(3) 0.019(2) 0.006(2) 0.011(2) N47 0.039(3) 0.034(3) 0.040(3) 0.020(3) 0.000(2) 0.010(3) N48 0.044(3) 0.034(3) 0.042(3) 0.024(3) 0.000(3) 0.009(3) O1 0.048(3) 0.045(3) 0.037(3) 0.024(2) 0.019(2) 0.015(2) O2 0.052(3) 0.047(3) 0.030(2) 0.024(2) 0.009(2) 0.020(2) O3 0.059(3) 0.074(3) 0.050(3) 0.044(3) 0.012(2) 0.003(3) O4 0.057(3) 0.093(4) 0.046(3) 0.043(3) 0.000(2) 0.009(3) O5 0.090(4) 0.085(4) 0.036(3) 0.035(3) 0.027(3) 0.046(3) O6 0.067(3) 0.078(3) 0.017(2) 0.021(2) 0.016(2) 0.035(3) O7 0.049(3) 0.051(3) 0.020(2) 0.016(2) 0.007(2) 0.009(2) O8 0.058(3) 0.038(3) 0.037(3) 0.019(2) 0.026(2) 0.011(2) O9 0.060(3) 0.026(2) 0.049(3) 0.011(2) 0.016(2) 0.010(2) O10 0.051(3) 0.024(2) 0.054(3) 0.015(2) 0.011(2) 0.010(2) O11 0.072(3) 0.028(2) 0.025(2) 0.009(2) 0.013(2) 0.020(2) O12 0.042(2) 0.032(2) 0.037(3) 0.017(2) 0.014(2) 0.013(2) O13 0.049(3) 0.040(2) 0.019(2) 0.015(2) 0.0056(19) 0.014(2) O14 0.048(3) 0.052(3) 0.024(2) 0.004(2) -0.002(2) 0.004(2) O15 0.051(3) 0.045(3) 0.035(3) 0.004(2) 0.007(2) 0.016(2) O16 0.064(3) 0.029(2) 0.039(3) 0.014(2) 0.022(2) 0.007(2) O17 0.080(4) 0.043(3) 0.056(3) 0.035(3) 0.003(3) 0.010(3) O18 0.069(3) 0.047(3) 0.082(4) 0.048(3) 0.017(3) 0.019(3) O19 0.056(3) 0.038(3) 0.087(4) 0.032(3) 0.026(3) 0.030(2) O20 0.058(3) 0.030(2) 0.044(3) 0.020(2) 0.003(2) 0.018(2) O21 0.067(3) 0.046(3) 0.050(3) 0.031(2) 0.011(2) 0.033(2) O22 0.069(3) 0.050(3) 0.046(3) 0.033(2) 0.012(2) 0.030(3) O23 0.050(3) 0.050(3) 0.058(3) 0.041(3) 0.010(2) 0.014(2) O24 0.062(3) 0.036(3) 0.052(3) 0.029(2) -0.007(2) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O12W Sr2 2.296(15) . ? O1W Sr1 2.620(4) . ? O2W Sr1 2.655(5) . ? O3W Sr1 2.568(5) . ? O4W Sr1 2.668(7) 2_566 ? O5W Sr1 2.600(7) . ? O6W Sr2 2.626(5) . ? O7W Sr2 2.669(7) . ? O8W Sr2 2.520(7) . ? O9W Sr2 2.688(7) . ? O10W Sr2 2.544(7) . ? Sr1 O13 2.553(4) 2_566 ? Sr1 O12 2.584(4) . ? Sr1 O2 2.595(4) . ? Sr1 O4W 2.668(7) 2_566 ? Sr2 O15 2.605(4) . ? Sr2 O18 2.654(5) . ? C1 O1 1.228(7) . ? C1 N1 1.346(7) . ? C1 N2 1.364(8) . ? C2 N3 1.439(7) . ? C2 N1 1.456(7) . ? C2 C3 1.524(8) . ? C2 H2 0.9800 . ? C3 N2 1.460(7) . ? C3 N4 1.472(7) . ? C3 H3 0.9800 . ? C4 O5 1.223(7) . ? C4 N4 1.365(7) . ? C4 N3 1.373(8) . ? C5 N2 1.432(7) . ? C5 N5 1.437(7) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N7 1.452(7) . ? C6 N4 1.460(7) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 O2 1.239(7) . ? C7 N5 1.348(8) . ? C7 N6 1.379(7) . ? C8 N5 1.444(7) . ? C8 N7 1.473(7) . ? C8 C9 1.551(7) . ? C8 H8 0.9800 . ? C9 N8 1.449(7) . ? C9 N6 1.450(7) . ? C9 H9 0.9800 . ? C10 O6 1.224(7) . ? C10 N7 1.350(7) . ? C10 N8 1.365(7) . ? C11 N6 1.437(7) . ? C11 N9 1.441(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N11 1.434(7) . ? C12 N8 1.465(7) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 O3 1.288(7) . ? C13 N10 1.323(7) . ? C13 N9 1.324(8) . ? C14 N9 1.446(7) . ? C14 N11 1.453(7) . ? C14 C15 1.552(8) . ? C14 H14 0.9800 . ? C15 N12 1.438(7) . ? C15 N10 1.446(8) . ? C15 H15 0.9800 . ? C16 O7 1.244(7) . ? C16 N12 1.335(8) . ? C16 N11 1.385(7) . ? C17 N13 1.431(8) . ? C17 N10 1.493(8) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 N15 1.413(7) . ? C18 N12 1.491(7) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 O4 1.254(8) . ? C19 N13 1.348(8) . ? C19 N14 1.359(8) . ? C20 N15 1.438(8) . ? C20 N13 1.483(8) . ? C20 C21 1.533(8) . ? C20 H20 0.9800 . ? C21 N14 1.423(7) . ? C21 N16 1.424(7) . ? C21 H21 0.9800 . ? C22 O8 1.226(7) . ? C22 N15 1.377(7) . ? C22 N16 1.393(8) . ? C23 N14 1.430(8) . ? C23 N3 1.441(7) 2 ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 N16 1.440(7) . ? C24 N1 1.450(7) 2 ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 O9 1.242(7) . ? C25 N17 1.353(7) . ? C25 N18 1.384(8) . ? C26 N19 1.450(7) . ? C26 N17 1.464(7) . ? C26 C27 1.516(8) . ? C26 H26 0.9800 . ? C27 N18 1.466(7) . ? C27 N20 1.490(7) . ? C27 H27 0.9800 . ? C28 O13 1.238(7) . ? C28 N19 1.340(7) . ? C28 N20 1.370(7) . ? C29 N18 1.415(7) . ? C29 N21 1.461(7) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 N20 1.445(7) . ? C30 N23 1.457(7) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 O10 1.231(7) . ? C31 N22 1.352(7) . ? C31 N21 1.379(7) . ? C32 N21 1.418(7) . ? C32 N23 1.464(7) . ? C32 C33 1.529(8) . ? C32 H32 0.9800 . ? C33 N24 1.430(7) . ? C33 N22 1.463(7) . ? C33 H33 0.9800 . ? C34 O14 1.216(7) . ? C34 N23 1.366(8) . ? C34 N24 1.381(8) . ? C35 N25 1.422(7) . ? C35 N22 1.435(7) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 N27 1.416(7) . ? C36 N24 1.460(7) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 O11 1.192(6) . ? C37 N26 1.372(7) . ? C37 N25 1.376(7) . ? C38 N25 1.451(7) . ? C38 N27 1.470(7) . ? C38 C39 1.563(8) . ? C38 H38 0.9800 . ? C39 N26 1.434(7) . ? C39 N28 1.471(7) . ? C39 H39 0.9800 . ? C40 O15 1.230(7) . ? C40 N28 1.339(7) . ? C40 N27 1.376(7) . ? C41 N26 1.448(7) . ? C41 N29 1.458(7) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 N31 1.432(7) . ? C42 N28 1.470(7) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 O12 1.221(6) . ? C43 N30 1.351(7) . ? C43 N29 1.359(7) . ? C44 N31 1.421(7) . ? C44 N29 1.459(7) . ? C44 C45 1.555(8) . ? C44 H44 0.9800 . ? C45 N32 1.452(7) . ? C45 N30 1.460(7) . ? C45 H45 0.9800 . ? C46 O16 1.224(7) . ? C46 N32 1.350(8) . ? C46 N31 1.391(8) . ? C47 N30 1.431(7) . ? C47 N19 1.466(7) 2_566 ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 N32 1.427(7) . ? C48 N17 1.440(8) 2_566 ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 O17 1.220(7) . ? C49 N34 1.369(8) . ? C49 N33 1.415(8) . ? C50 N35 1.459(7) . ? C50 N33 1.464(7) . ? C50 C51 1.503(8) . ? C50 H50 0.9800 . ? C51 N34 1.444(7) . ? C51 N36 1.482(7) . ? C51 H51 0.9800 . ? C52 O21 1.222(7) . ? C52 N36 1.354(7) . ? C52 N35 1.358(7) . ? C53 N34 1.418(7) . ? C53 N37 1.438(7) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 N39 1.443(7) . ? C54 N36 1.469(7) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 O18 1.222(7) . ? C55 N37 1.348(8) . ? C55 N38 1.350(8) . ? C56 N39 1.419(7) . ? C56 N37 1.452(8) . ? C56 C57 1.577(8) . ? C56 H56 0.9800 . ? C57 N38 1.407(8) . ? C57 N40 1.449(7) . ? C57 H57 0.9800 . ? C58 O22 1.199(7) . ? C58 N40 1.381(7) . ? C58 N39 1.387(7) . ? C59 N38 1.442(8) . ? C59 N41 1.472(8) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 N43 1.451(7) . ? C60 N40 1.460(7) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 O19 1.219(8) . ? C61 N41 1.379(8) . ? C61 N42 1.380(8) . ? C62 N43 1.439(7) . ? C62 N41 1.455(7) . ? C62 C63 1.538(8) . ? C62 H62 0.9800 . ? C63 N42 1.442(7) . ? C63 N44 1.468(7) . ? C63 H63 0.9800 . ? C64 O23 1.218(6) . ? C64 N44 1.352(7) . ? C64 N43 1.366(7) . ? C65 N45 1.420(7) . ? C65 N42 1.430(7) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 N47 1.438(7) . ? C66 N44 1.438(7) . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C67 O20 1.228(7) . ? C67 N46 1.354(7) . ? C67 N45 1.375(7) . ? C68 N47 1.439(7) . ? C68 N45 1.464(7) . ? C68 C69 1.528(8) . ? C68 H68 0.9800 . ? C69 N48 1.463(7) . ? C69 N46 1.470(7) . ? C69 H69 0.9800 . ? C70 O24 1.228(7) . ? C70 N48 1.364(8) . ? C70 N47 1.372(7) . ? C71 N35 1.454(7) . ? C71 N46 1.458(7) 2_576 ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C72 N33 1.429(7) 2_576 ? C72 N48 1.440(7) . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? N1 C24 1.450(7) 2 ? N3 C23 1.441(7) 2 ? N17 C48 1.440(8) 2_566 ? N19 C47 1.466(7) 2_566 ? N33 C72 1.429(7) 2_576 ? N46 C71 1.458(7) 2_576 ? O13 Sr1 2.553(4) 2_566 ? 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 O13 Sr1 O3W 139.09(14) 2_566 . ? O13 Sr1 O12 87.30(13) 2_566 . ? O3W Sr1 O12 76.76(14) . . ? O13 Sr1 O2 145.91(12) 2_566 . ? O3W Sr1 O2 72.72(14) . . ? O12 Sr1 O2 90.82(13) . . ? O13 Sr1 O5W 87.1(3) 2_566 . ? O3W Sr1 O5W 85.0(3) . . ? O12 Sr1 O5W 144.7(3) . . ? O2 Sr1 O5W 112.4(3) . . ? O13 Sr1 O1W 74.45(12) 2_566 . ? O3W Sr1 O1W 130.79(16) . . ? O12 Sr1 O1W 69.49(13) . . ? O2 Sr1 O1W 73.05(12) . . ? O5W Sr1 O1W 141.2(3) . . ? O13 Sr1 O2W 71.56(14) 2_566 . ? O3W Sr1 O2W 68.02(16) . . ? O12 Sr1 O2W 75.21(17) . . ? O2 Sr1 O2W 140.34(15) . . ? O5W Sr1 O2W 69.9(3) . . ? O1W Sr1 O2W 131.43(16) . . ? O13 Sr1 O4W 84.2(2) 2_566 2_566 ? O3W Sr1 O4W 128.9(2) . 2_566 ? O12 Sr1 O4W 144.9(2) . 2_566 ? O2 Sr1 O4W 78.0(2) . 2_566 ? O5W Sr1 O4W 68.8(4) . 2_566 ? O1W Sr1 O4W 75.4(2) . 2_566 ? O2W Sr1 O4W 132.7(3) . 2_566 ? O12W Sr2 O8W 149.1(4) . . ? O12W Sr2 O10W 105.2(5) . . ? O8W Sr2 O10W 105.3(4) . . ? O12W Sr2 O15 114.1(4) . . ? O8W Sr2 O15 75.03(19) . . ? O10W Sr2 O15 82.0(2) . . ? O12W Sr2 O6W 64.6(3) . . ? O8W Sr2 O6W 90.1(2) . . ? O10W Sr2 O6W 151.4(2) . . ? O15 Sr2 O6W 78.99(14) . . ? O12W Sr2 O18 110.5(4) . . ? O8W Sr2 O18 79.08(18) . . ? O10W Sr2 O18 64.1(2) . . ? O15 Sr2 O18 129.44(15) . . ? O6W Sr2 O18 143.83(15) . . ? O12W Sr2 O7W 75.8(4) . . ? O8W Sr2 O7W 79.6(3) . . ? O10W Sr2 O7W 134.1(2) . . ? O15 Sr2 O7W 140.8(2) . . ? O6W Sr2 O7W 71.55(19) . . ? O18 Sr2 O7W 72.58(19) . . ? O12W Sr2 O9W 52.9(4) . . ? O8W Sr2 O9W 138.0(2) . . ? O10W Sr2 O9W 80.9(3) . . ? O15 Sr2 O9W 64.61(17) . . ? O6W Sr2 O9W 71.7(2) . . ? O18 Sr2 O9W 136.4(2) . . ? O7W Sr2 O9W 125.9(2) . . ? O1 C1 N1 127.0(6) . . ? O1 C1 N2 122.9(5) . . ? N1 C1 N2 110.1(6) . . ? N3 C2 N1 113.4(5) . . ? N3 C2 C3 104.1(4) . . ? N1 C2 C3 102.4(4) . . ? N3 C2 H2 112.1 . . ? N1 C2 H2 112.1 . . ? C3 C2 H2 112.1 . . ? N2 C3 N4 114.5(4) . . ? N2 C3 C2 104.8(5) . . ? N4 C3 C2 103.0(5) . . ? N2 C3 H3 111.4 . . ? N4 C3 H3 111.4 . . ? C2 C3 H3 111.4 . . ? O5 C4 N4 126.0(6) . . ? O5 C4 N3 125.9(6) . . ? N4 C4 N3 108.1(5) . . ? N2 C5 N5 114.5(5) . . ? N2 C5 H5A 108.6 . . ? N5 C5 H5A 108.6 . . ? N2 C5 H5B 108.6 . . ? N5 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? N7 C6 N4 112.6(5) . . ? N7 C6 H6A 109.1 . . ? N4 C6 H6A 109.1 . . ? N7 C6 H6B 109.1 . . ? N4 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? O2 C7 N5 125.2(5) . . ? O2 C7 N6 125.2(6) . . ? N5 C7 N6 109.5(5) . . ? N5 C8 N7 115.3(4) . . ? N5 C8 C9 103.1(5) . . ? N7 C8 C9 102.2(4) . . ? N5 C8 H8 111.8 . . ? N7 C8 H8 111.8 . . ? C9 C8 H8 111.8 . . ? N8 C9 N6 114.7(5) . . ? N8 C9 C8 103.3(4) . . ? N6 C9 C8 103.8(4) . . ? N8 C9 H9 111.5 . . ? N6 C9 H9 111.5 . . ? C8 C9 H9 111.5 . . ? O6 C10 N7 125.2(6) . . ? O6 C10 N8 126.5(6) . . ? N7 C10 N8 108.2(5) . . ? N6 C11 N9 113.4(4) . . ? N6 C11 H11A 108.9 . . ? N9 C11 H11A 108.9 . . ? N6 C11 H11B 108.9 . . ? N9 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? N11 C12 N8 113.0(5) . . ? N11 C12 H12A 109.0 . . ? N8 C12 H12A 109.0 . . ? N11 C12 H12B 109.0 . . ? N8 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? O3 C13 N10 124.6(6) . . ? O3 C13 N9 123.9(5) . . ? N10 C13 N9 111.1(6) . . ? N9 C14 N11 114.4(4) . . ? N9 C14 C15 104.4(5) . . ? N11 C14 C15 103.3(4) . . ? N9 C14 H14 111.4 . . ? N11 C14 H14 111.4 . . ? C15 C14 H14 111.4 . . ? N12 C15 N10 114.9(5) . . ? N12 C15 C14 102.6(4) . . ? N10 C15 C14 100.8(4) . . ? N12 C15 H15 112.5 . . ? N10 C15 H15 112.5 . . ? C14 C15 H15 112.5 . . ? O7 C16 N12 128.5(5) . . ? O7 C16 N11 123.4(6) . . ? N12 C16 N11 108.0(5) . . ? N13 C17 N10 114.4(5) . . ? N13 C17 H17A 108.7 . . ? N10 C17 H17A 108.7 . . ? N13 C17 H17B 108.7 . . ? N10 C17 H17B 108.7 . . ? H17A C17 H17B 107.6 . . ? N15 C18 N12 113.1(5) . . ? N15 C18 H18A 109.0 . . ? N12 C18 H18A 109.0 . . ? N15 C18 H18B 109.0 . . ? N12 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? O4 C19 N13 124.1(6) . . ? O4 C19 N14 125.8(7) . . ? N13 C19 N14 110.1(6) . . ? N15 C20 N13 112.3(5) . . ? N15 C20 C21 104.5(4) . . ? N13 C20 C21 102.2(5) . . ? N15 C20 H20 112.4 . . ? N13 C20 H20 112.4 . . ? C21 C20 H20 112.4 . . ? N14 C21 N16 114.9(5) . . ? N14 C21 C20 104.9(4) . . ? N16 C21 C20 103.7(5) . . ? N14 C21 H21 111.0 . . ? N16 C21 H21 111.0 . . ? C20 C21 H21 111.0 . . ? O8 C22 N15 125.9(6) . . ? O8 C22 N16 126.8(5) . . ? N15 C22 N16 107.3(5) . . ? N14 C23 N3 113.0(5) . 2 ? N14 C23 H23A 109.0 . . ? N3 C23 H23A 109.0 2 . ? N14 C23 H23B 109.0 . . ? N3 C23 H23B 109.0 2 . ? H23A C23 H23B 107.8 . . ? N16 C24 N1 112.7(5) . 2 ? N16 C24 H24A 109.1 . . ? N1 C24 H24A 109.1 2 . ? N16 C24 H24B 109.1 . . ? N1 C24 H24B 109.1 2 . ? H24A C24 H24B 107.8 . . ? O9 C25 N17 125.5(6) . . ? O9 C25 N18 124.4(6) . . ? N17 C25 N18 110.1(5) . . ? N19 C26 N17 113.4(4) . . ? N19 C26 C27 103.3(4) . . ? N17 C26 C27 103.6(4) . . ? N19 C26 H26 111.9 . . ? N17 C26 H26 111.9 . . ? C27 C26 H26 111.9 . . ? N18 C27 N20 111.5(4) . . ? N18 C27 C26 104.9(4) . . ? N20 C27 C26 103.3(4) . . ? N18 C27 H27 112.2 . . ? N20 C27 H27 112.2 . . ? C26 C27 H27 112.2 . . ? O13 C28 N19 126.8(6) . . ? O13 C28 N20 124.4(6) . . ? N19 C28 N20 108.8(5) . . ? N18 C29 N21 112.1(4) . . ? N18 C29 H29A 109.2 . . ? N21 C29 H29A 109.2 . . ? N18 C29 H29B 109.2 . . ? N21 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? N20 C30 N23 111.9(5) . . ? N20 C30 H30A 109.2 . . ? N23 C30 H30A 109.2 . . ? N20 C30 H30B 109.2 . . ? N23 C30 H30B 109.2 . . ? H30A C30 H30B 107.9 . . ? O10 C31 N22 127.2(5) . . ? O10 C31 N21 124.5(6) . . ? N22 C31 N21 108.3(5) . . ? N21 C32 N23 114.3(5) . . ? N21 C32 C33 105.0(4) . . ? N23 C32 C33 102.9(4) . . ? N21 C32 H32 111.4 . . ? N23 C32 H32 111.4 . . ? C33 C32 H32 111.4 . . ? N24 C33 N22 113.4(5) . . ? N24 C33 C32 105.1(5) . . ? N22 C33 C32 102.4(4) . . ? N24 C33 H33 111.8 . . ? N22 C33 H33 111.8 . . ? C32 C33 H33 111.8 . . ? O14 C34 N23 126.0(6) . . ? O14 C34 N24 125.6(6) . . ? N23 C34 N24 108.4(6) . . ? N25 C35 N22 113.8(5) . . ? N25 C35 H35A 108.8 . . ? N22 C35 H35A 108.8 . . ? N25 C35 H35B 108.8 . . ? N22 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? N27 C36 N24 112.6(5) . . ? N27 C36 H36A 109.1 . . ? N24 C36 H36A 109.1 . . ? N27 C36 H36B 109.1 . . ? N24 C36 H36B 109.1 . . ? H36A C36 H36B 107.8 . . ? O11 C37 N26 127.0(5) . . ? O11 C37 N25 125.0(5) . . ? N26 C37 N25 108.0(5) . . ? N25 C38 N27 113.9(5) . . ? N25 C38 C39 103.6(4) . . ? N27 C38 C39 103.5(4) . . ? N25 C38 H38 111.7 . . ? N27 C38 H38 111.7 . . ? C39 C38 H38 111.7 . . ? N26 C39 N28 114.2(5) . . ? N26 C39 C38 102.8(4) . . ? N28 C39 C38 102.2(4) . . ? N26 C39 H39 112.3 . . ? N28 C39 H39 112.3 . . ? C38 C39 H39 112.3 . . ? O15 C40 N28 125.8(6) . . ? O15 C40 N27 124.6(6) . . ? N28 C40 N27 109.6(5) . . ? N26 C41 N29 113.4(4) . . ? N26 C41 H41A 108.9 . . ? N29 C41 H41A 108.9 . . ? N26 C41 H41B 108.9 . . ? N29 C41 H41B 108.9 . . ? H41A C41 H41B 107.7 . . ? N31 C42 N28 114.0(5) . . ? N31 C42 H42A 108.8 . . ? N28 C42 H42A 108.8 . . ? N31 C42 H42B 108.8 . . ? N28 C42 H42B 108.8 . . ? H42A C42 H42B 107.7 . . ? O12 C43 N30 125.6(6) . . ? O12 C43 N29 125.2(5) . . ? N30 C43 N29 109.2(5) . . ? N31 C44 N29 115.1(4) . . ? N31 C44 C45 103.5(4) . . ? N29 C44 C45 102.0(4) . . ? N31 C44 H44 111.8 . . ? N29 C44 H44 111.8 . . ? C45 C44 H44 111.8 . . ? N32 C45 N30 114.3(4) . . ? N32 C45 C44 103.4(4) . . ? N30 C45 C44 103.6(4) . . ? N32 C45 H45 111.6 . . ? N30 C45 H45 111.6 . . ? C44 C45 H45 111.6 . . ? O16 C46 N32 126.1(6) . . ? O16 C46 N31 124.9(6) . . ? N32 C46 N31 109.0(5) . . ? N30 C47 N19 114.1(4) . 2_566 ? N30 C47 H47A 108.7 . . ? N19 C47 H47A 108.7 2_566 . ? N30 C47 H47B 108.7 . . ? N19 C47 H47B 108.7 2_566 . ? H47A C47 H47B 107.6 . . ? N32 C48 N17 114.8(5) . 2_566 ? N32 C48 H48A 108.6 . . ? N17 C48 H48A 108.6 2_566 . ? N32 C48 H48B 108.6 . . ? N17 C48 H48B 108.6 2_566 . ? H48A C48 H48B 107.5 . . ? O17 C49 N34 128.9(6) . . ? O17 C49 N33 123.6(6) . . ? N34 C49 N33 107.4(6) . . ? N35 C50 N33 112.8(4) . . ? N35 C50 C51 105.5(4) . . ? N33 C50 C51 104.0(5) . . ? N35 C50 H50 111.4 . . ? N33 C50 H50 111.4 . . ? C51 C50 H50 111.4 . . ? N34 C51 N36 111.6(5) . . ? N34 C51 C50 105.5(5) . . ? N36 C51 C50 102.2(4) . . ? N34 C51 H51 112.3 . . ? N36 C51 H51 112.3 . . ? C50 C51 H51 112.3 . . ? O21 C52 N36 125.1(6) . . ? O21 C52 N35 125.6(5) . . ? N36 C52 N35 109.3(5) . . ? N34 C53 N37 114.4(5) . . ? N34 C53 H53A 108.7 . . ? N37 C53 H53A 108.7 . . ? N34 C53 H53B 108.7 . . ? N37 C53 H53B 108.7 . . ? H53A C53 H53B 107.6 . . ? N39 C54 N36 112.3(5) . . ? N39 C54 H54A 109.1 . . ? N36 C54 H54A 109.1 . . ? N39 C54 H54B 109.1 . . ? N36 C54 H54B 109.1 . . ? H54A C54 H54B 107.9 . . ? O18 C55 N37 123.9(6) . . ? O18 C55 N38 126.6(7) . . ? N37 C55 N38 109.5(6) . . ? N39 C56 N37 115.9(5) . . ? N39 C56 C57 105.1(5) . . ? N37 C56 C57 101.4(5) . . ? N39 C56 H56 111.3 . . ? N37 C56 H56 111.3 . . ? C57 C56 H56 111.3 . . ? N38 C57 N40 117.0(5) . . ? N38 C57 C56 103.8(5) . . ? N40 C57 C56 101.0(5) . . ? N38 C57 H57 111.4 . . ? N40 C57 H57 111.4 . . ? C56 C57 H57 111.4 . . ? O22 C58 N40 126.8(6) . . ? O22 C58 N39 126.0(6) . . ? N40 C58 N39 107.2(5) . . ? N38 C59 N41 112.7(5) . . ? N38 C59 H59A 109.1 . . ? N41 C59 H59A 109.1 . . ? N38 C59 H59B 109.1 . . ? N41 C59 H59B 109.1 . . ? H59A C59 H59B 107.8 . . ? N43 C60 N40 112.2(5) . . ? N43 C60 H60A 109.2 . . ? N40 C60 H60A 109.2 . . ? N43 C60 H60B 109.2 . . ? N40 C60 H60B 109.2 . . ? H60A C60 H60B 107.9 . . ? O19 C61 N41 126.9(6) . . ? O19 C61 N42 125.6(7) . . ? N41 C61 N42 107.5(6) . . ? N43 C62 N41 114.1(5) . . ? N43 C62 C63 104.7(4) . . ? N41 C62 C63 102.8(5) . . ? N43 C62 H62 111.6 . . ? N41 C62 H62 111.6 . . ? C63 C62 H62 111.6 . . ? N42 C63 N44 115.6(5) . . ? N42 C63 C62 104.6(5) . . ? N44 C63 C62 101.7(5) . . ? N42 C63 H63 111.4 . . ? N44 C63 H63 111.4 . . ? C62 C63 H63 111.4 . . ? O23 C64 N44 125.7(5) . . ? O23 C64 N43 126.0(6) . . ? N44 C64 N43 108.3(5) . . ? N45 C65 N42 114.6(5) . . ? N45 C65 H65A 108.6 . . ? N42 C65 H65A 108.6 . . ? N45 C65 H65B 108.6 . . ? N42 C65 H65B 108.6 . . ? H65A C65 H65B 107.6 . . ? N47 C66 N44 114.3(5) . . ? N47 C66 H66A 108.7 . . ? N44 C66 H66A 108.7 . . ? N47 C66 H66B 108.7 . . ? N44 C66 H66B 108.7 . . ? H66A C66 H66B 107.6 . . ? O20 C67 N46 125.0(5) . . ? O20 C67 N45 125.9(5) . . ? N46 C67 N45 109.1(5) . . ? N47 C68 N45 113.3(5) . . ? N47 C68 C69 104.1(4) . . ? N45 C68 C69 103.9(4) . . ? N47 C68 H68 111.7 . . ? N45 C68 H68 111.7 . . ? C69 C68 H68 111.7 . . ? N48 C69 N46 112.1(5) . . ? N48 C69 C68 103.5(5) . . ? N46 C69 C68 103.4(4) . . ? N48 C69 H69 112.4 . . ? N46 C69 H69 112.4 . . ? C68 C69 H69 112.4 . . ? O24 C70 N48 125.0(5) . . ? O24 C70 N47 126.2(6) . . ? N48 C70 N47 108.8(5) . . ? N35 C71 N46 113.4(5) . 2_576 ? N35 C71 H71A 108.9 . . ? N46 C71 H71A 108.9 2_576 . ? N35 C71 H71B 108.9 . . ? N46 C71 H71B 108.9 2_576 . ? H71A C71 H71B 107.7 . . ? N33 C72 N48 113.5(5) 2_576 . ? N33 C72 H72A 108.9 2_576 . ? N48 C72 H72A 108.9 . . ? N33 C72 H72B 108.9 2_576 . ? N48 C72 H72B 108.9 . . ? H72A C72 H72B 107.7 . . ? C1 N1 C24 120.2(5) . 2 ? C1 N1 C2 111.8(5) . . ? C24 N1 C2 122.3(5) 2 . ? C1 N2 C5 125.1(5) . . ? C1 N2 C3 109.8(5) . . ? C5 N2 C3 124.5(5) . . ? C4 N3 C2 112.4(5) . . ? C4 N3 C23 122.6(5) . 2 ? C2 N3 C23 124.8(5) . 2 ? C4 N4 C6 121.2(5) . . ? C4 N4 C3 111.7(5) . . ? C6 N4 C3 122.9(5) . . ? C7 N5 C5 123.1(5) . . ? C7 N5 C8 112.4(5) . . ? C5 N5 C8 122.5(5) . . ? C7 N6 C11 122.4(5) . . ? C7 N6 C9 110.4(5) . . ? C11 N6 C9 121.5(5) . . ? C10 N7 C6 121.5(5) . . ? C10 N7 C8 112.8(5) . . ? C6 N7 C8 120.9(5) . . ? C10 N8 C9 112.9(5) . . ? C10 N8 C12 121.8(5) . . ? C9 N8 C12 121.5(5) . . ? C13 N9 C11 122.2(5) . . ? C13 N9 C14 110.4(5) . . ? C11 N9 C14 121.8(5) . . ? C13 N10 C15 113.0(5) . . ? C13 N10 C17 122.9(6) . . ? C15 N10 C17 122.5(5) . . ? C16 N11 C12 122.5(5) . . ? C16 N11 C14 111.5(5) . . ? C12 N11 C14 123.1(5) . . ? C16 N12 C15 114.2(5) . . ? C16 N12 C18 120.7(5) . . ? C15 N12 C18 122.2(5) . . ? C19 N13 C17 121.6(6) . . ? C19 N13 C20 110.6(5) . . ? C17 N13 C20 123.2(6) . . ? C19 N14 C21 111.6(5) . . ? C19 N14 C23 122.4(6) . . ? C21 N14 C23 124.9(5) . . ? C22 N15 C18 121.7(5) . . ? C22 N15 C20 111.9(5) . . ? C18 N15 C20 125.1(5) . . ? C22 N16 C21 112.6(5) . . ? C22 N16 C24 120.1(5) . . ? C21 N16 C24 126.0(5) . . ? C25 N17 C48 121.6(5) . 2_566 ? C25 N17 C26 111.0(5) . . ? C48 N17 C26 122.4(5) 2_566 . ? C25 N18 C29 123.7(5) . . ? C25 N18 C27 109.5(5) . . ? C29 N18 C27 124.2(5) . . ? C28 N19 C26 113.4(5) . . ? C28 N19 C47 122.3(5) . 2_566 ? C26 N19 C47 123.9(5) . 2_566 ? C28 N20 C30 122.4(5) . . ? C28 N20 C27 110.3(5) . . ? C30 N20 C27 121.0(5) . . ? C31 N21 C32 111.8(5) . . ? C31 N21 C29 122.4(5) . . ? C32 N21 C29 123.5(4) . . ? C31 N22 C35 122.4(5) . . ? C31 N22 C33 112.0(4) . . ? C35 N22 C33 122.6(5) . . ? C34 N23 C30 121.6(5) . . ? C34 N23 C32 111.8(5) . . ? C30 N23 C32 122.0(4) . . ? C34 N24 C33 111.6(5) . . ? C34 N24 C36 123.4(5) . . ? C33 N24 C36 123.2(5) . . ? C37 N25 C35 123.0(5) . . ? C37 N25 C38 111.9(4) . . ? C35 N25 C38 123.0(5) . . ? C37 N26 C39 113.4(4) . . ? C37 N26 C41 120.3(5) . . ? C39 N26 C41 122.4(5) . . ? C40 N27 C36 124.0(5) . . ? C40 N27 C38 111.1(5) . . ? C36 N27 C38 122.3(5) . . ? C40 N28 C42 123.9(5) . . ? C40 N28 C39 113.2(5) . . ? C42 N28 C39 120.3(5) . . ? C43 N29 C41 121.4(5) . . ? C43 N29 C44 112.7(5) . . ? C41 N29 C44 121.7(5) . . ? C43 N30 C47 123.7(5) . . ? C43 N30 C45 111.9(5) . . ? C47 N30 C45 123.4(5) . . ? C46 N31 C44 111.9(5) . . ? C46 N31 C42 123.9(5) . . ? C44 N31 C42 123.0(5) . . ? C46 N32 C48 122.8(5) . . ? C46 N32 C45 111.5(5) . . ? C48 N32 C45 121.7(5) . . ? C49 N33 C72 120.9(5) . 2_576 ? C49 N33 C50 110.6(5) . . ? C72 N33 C50 123.5(5) 2_576 . ? C49 N34 C53 120.0(5) . . ? C49 N34 C51 112.1(5) . . ? C53 N34 C51 125.3(5) . . ? C52 N35 C71 124.2(5) . . ? C52 N35 C50 110.6(4) . . ? C71 N35 C50 124.0(5) . . ? C52 N36 C54 122.0(5) . . ? C52 N36 C51 111.7(5) . . ? C54 N36 C51 122.3(5) . . ? C55 N37 C53 123.2(5) . . ? C55 N37 C56 112.2(5) . . ? C53 N37 C56 123.7(5) . . ? C55 N38 C57 112.5(5) . . ? C55 N38 C59 122.3(5) . . ? C57 N38 C59 122.2(5) . . ? C58 N39 C56 112.2(5) . . ? C58 N39 C54 118.4(5) . . ? C56 N39 C54 124.2(5) . . ? C58 N40 C57 113.9(5) . . ? C58 N40 C60 122.0(5) . . ? C57 N40 C60 123.0(5) . . ? C61 N41 C62 112.8(5) . . ? C61 N41 C59 123.1(5) . . ? C62 N41 C59 122.6(5) . . ? C61 N42 C65 120.7(5) . . ? C61 N42 C63 112.2(5) . . ? C65 N42 C63 123.9(5) . . ? C64 N43 C62 111.9(5) . . ? C64 N43 C60 120.5(5) . . ? C62 N43 C60 125.1(5) . . ? C64 N44 C66 123.0(5) . . ? C64 N44 C63 113.1(5) . . ? C66 N44 C63 122.7(5) . . ? C67 N45 C65 121.7(5) . . ? C67 N45 C68 111.1(5) . . ? C65 N45 C68 123.1(5) . . ? C67 N46 C71 123.4(5) . 2_576 ? C67 N46 C69 111.9(5) . . ? C71 N46 C69 122.2(5) 2_576 . ? C70 N47 C66 122.8(5) . . ? C70 N47 C68 111.9(5) . . ? C66 N47 C68 122.6(5) . . ? C70 N48 C72 122.0(5) . . ? C70 N48 C69 111.2(5) . . ? C72 N48 C69 122.3(5) . . ? C7 O2 Sr1 138.7(4) . . ? C43 O12 Sr1 131.8(4) . . ? C28 O13 Sr1 130.3(4) . 2_566 ? C40 O15 Sr2 160.7(4) . . ? C55 O18 Sr2 164.2(4) . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.978 _refine_diff_density_min -0.985 _refine_diff_density_rms 0.105 # 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 0.000 0.000 0.000 401 118 ' ' 2 0.000 0.000 0.500 358 136 ' ' 3 -0.002 0.479 0.979 2085 931 ' ' 4 0.000 0.500 0.500 219 74 ' ' 5 0.500 0.500 0.500 44 27 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 931661'