# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email xyhuang@fjirsm.ac.cn _publ_contact_author_name 'Huang, Xiao-ying' loop_ _publ_author_name 'Zai-Lai Xie' 'Mei-Ling Feng' 'Bin Tan' 'Yong Wang' A.Taubert 'Xiao-Ying Huang' data_compound-1 _database_code_depnum_ccdc_archive 'CCDC 800121' #TrackingRef '- compound-1-bt2-20f(zx3-39b).cif' _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point 'C42 H37 Cd3 F N7 O8, B1 F4' _chemical_formula_moiety 'C42 H37 Cd3 F N7 O8 B1 F4' _chemical_formula_sum 'C42 H37 B Cd3 F5 N7 O8' _chemical_formula_weight 1210.80 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'A m a 2' _symmetry_space_group_name_Hall 'A 2 -2a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y, z' 'x+1/2, -y, z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 20.6365(4) _cell_length_b 18.1133(4) _cell_length_c 12.6984(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4746.60(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12652 _cell_measurement_theta_min 2.4510 _cell_measurement_theta_max 28.8431 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.694 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2384 _exptl_absorpt_coefficient_mu 1.408 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.71057 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2083 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10835 _diffrn_reflns_av_R_equivalents 0.0145 _diffrn_reflns_av_sigmaI/netI 0.0167 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 25.99 _reflns_number_total 4665 _reflns_number_gt 4484 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND. Version 3.0. Crystal Impact' _computing_publication_material 'Windows Word 2003' _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^)+(0.0510P)^2^+19.4920P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(4) _refine_ls_number_reflns 4665 _refine_ls_number_parameters 409 _refine_ls_number_restraints 1081 _refine_ls_R_factor_all 0.0348 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0882 _refine_ls_wR_factor_gt 0.0874 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.074 _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 Cd1 Cd 0.339689(14) 0.684399(17) 0.45573(10) 0.02226(9) Uani 1 1 d . . . Cd2 Cd 0.2500 0.67072(3) 0.73003(10) 0.02818(13) Uani 1 2 d S . . F1 F 0.2500 0.6618(2) 0.5541(3) 0.0249(8) Uani 1 2 d S . . O1 O 0.3608(2) 0.6665(3) 0.7404(5) 0.0629(13) Uani 1 1 d U A . O2 O 0.3984(2) 0.7230(3) 0.5958(3) 0.0562(13) Uani 1 1 d . A . N1 N 0.5678(2) 0.7790(3) 0.8620(4) 0.0351(10) Uani 1 1 d . . . C1 C 0.4009(3) 0.7045(4) 0.6887(5) 0.0463(12) Uani 1 1 d U . . C2 C 0.4606(3) 0.7293(3) 0.7506(4) 0.0402(12) Uani 1 1 d U A . C3 C 0.4835(3) 0.6902(3) 0.8360(5) 0.0405(12) Uani 1 1 d U . . H3A H 0.4631 0.6472 0.8582 0.049 Uiso 1 1 calc R A . C4 C 0.5373(3) 0.7167(4) 0.8875(5) 0.0403(12) Uani 1 1 d U A . H4A H 0.5535 0.6894 0.9437 0.048 Uiso 1 1 calc R . . C5 C 0.5457(3) 0.8160(3) 0.7785(5) 0.0428(13) Uani 1 1 d U A . H5A H 0.5674 0.8586 0.7576 0.051 Uiso 1 1 calc R . . C6 C 0.4922(3) 0.7937(4) 0.7221(5) 0.0469(12) Uani 1 1 d U . . H6A H 0.4774 0.8215 0.6655 0.056 Uiso 1 1 calc R A . O3 O 0.3056(5) 0.6356(6) 0.2991(7) 0.032(2) Uani 0.50 1 d P . . O4 O 0.2020(6) 0.6693(7) 0.2923(9) 0.043(3) Uani 0.50 1 d PU . . C7 C 0.2500 0.6546(5) 0.2523(6) 0.0453(17) Uani 1 2 d SU . . C8 C 0.2500 0.6650(5) 0.1338(8) 0.0551(19) Uani 1 2 d SDU . . C9 C 0.1959(4) 0.6379(5) 0.0779(7) 0.052(2) Uani 0.50 1 d PDU . . H9A H 0.1608 0.6146 0.1149 0.062 Uiso 0.50 1 d PR A . C10 C 0.1982(4) 0.6460(5) -0.0319(8) 0.054(2) Uani 0.50 1 d PDU . . H10A H 0.1616 0.6276 -0.0706 0.065 Uiso 0.50 1 d PR . . N2 N 0.2500 0.6783(5) -0.0836(8) 0.073(3) Uani 1 2 d SDU . . C11 C 0.2972(4) 0.7012(6) -0.0224(8) 0.061(2) Uani 0.50 1 d PDU . . H11A H 0.3323 0.7225 -0.0615 0.073 Uiso 0.50 1 d PR . . C12 C 0.3021(4) 0.6973(6) 0.0853(8) 0.063(2) Uani 0.50 1 d PDU . . H12A H 0.3348 0.7256 0.1207 0.075 Uiso 0.50 1 d PR A . O5 O 0.3035(2) 0.7993(3) 0.4231(4) 0.0574(13) Uani 1 1 d U A . N3 N 0.2500 1.0453(4) 0.2716(5) 0.0343(14) Uani 1 2 d S . . C13 C 0.2500 0.8267(5) 0.4057(9) 0.0452(17) Uani 1 2 d SU . . C14 C 0.2500 0.9024(5) 0.3563(8) 0.0466(17) Uani 1 2 d SU . . C15 C 0.1944(4) 0.9398(5) 0.3385(8) 0.0701(19) Uani 1 1 d U . . H15A H 0.1536 0.9160 0.3506 0.084 Uiso 1 1 d R A . C16 C 0.1965(3) 1.0109(4) 0.2985(8) 0.0676(18) Uani 1 1 d U A . H16A H 0.1561 1.0363 0.2891 0.081 Uiso 1 1 d R . . N4A N 0.3752(7) 0.5582(19) 0.4793(17) 0.043(4) Uani 0.50 1 d PD A 1 C17A C 0.3795(7) 0.5119(7) 0.4082(15) 0.0713(16) Uani 0.50 1 d PDU A 1 H17A H 0.3703 0.5277 0.3402 0.086 Uiso 0.50 1 calc PR A 1 C18A C 0.3967(6) 0.4391(7) 0.4204(13) 0.0730(16) Uani 0.50 1 d PDU A 1 H18A H 0.3989 0.4081 0.3622 0.088 Uiso 0.50 1 calc PR A 1 C19A C 0.4108(6) 0.4124(8) 0.5192(11) 0.0728(16) Uani 0.50 1 d PDU A 1 C20A C 0.4057(7) 0.4649(9) 0.5973(14) 0.0742(17) Uani 0.50 1 d PDU A 1 H20A H 0.4142 0.4514 0.6665 0.089 Uiso 0.50 1 calc PR A 1 C21A C 0.3891(7) 0.5335(9) 0.5772(15) 0.0708(16) Uani 0.50 1 d PDU A 1 H21A H 0.3869 0.5667 0.6330 0.085 Uiso 0.50 1 calc PR A 1 C22A C 0.4300(9) 0.3355(10) 0.5399(17) 0.081(2) Uani 0.50 1 d PDU A 1 H22A H 0.4369 0.3290 0.6141 0.122 Uiso 0.50 1 calc PR A 1 H22B H 0.4692 0.3246 0.5025 0.122 Uiso 0.50 1 calc PR A 1 H22C H 0.3962 0.3028 0.5167 0.122 Uiso 0.50 1 calc PR A 1 N4B N 0.3560(9) 0.562(2) 0.4788(14) 0.043(4) Uani 0.50 1 d PD A 2 C17B C 0.3053(8) 0.5111(7) 0.4741(11) 0.0713(16) Uani 0.50 1 d PDU A 2 H17B H 0.2646 0.5271 0.4524 0.086 Uiso 0.50 1 calc PR A 2 C18B C 0.3135(8) 0.4380(7) 0.5004(9) 0.0730(16) Uani 0.50 1 d PDU A 2 H18B H 0.2782 0.4063 0.4959 0.088 Uiso 0.50 1 calc PR A 2 C19B C 0.3719(7) 0.4104(9) 0.5329(9) 0.0728(16) Uani 0.50 1 d PDU A 2 C20B C 0.4233(9) 0.4585(9) 0.5388(11) 0.0742(17) Uani 0.50 1 d PDU A 2 H20B H 0.4640 0.4425 0.5605 0.089 Uiso 0.50 1 calc PR A 2 C21B C 0.4124(10) 0.5326(9) 0.5110(13) 0.0708(16) Uani 0.50 1 d PDU A 2 H21B H 0.4477 0.5644 0.5153 0.085 Uiso 0.50 1 calc PR A 2 C22B C 0.3682(11) 0.3253(10) 0.5581(15) 0.081(2) Uani 0.50 1 d PDU A 2 H22D H 0.3246 0.3082 0.5481 0.122 Uiso 0.50 1 calc PR A 2 H22E H 0.3811 0.3169 0.6297 0.122 Uiso 0.50 1 calc PR A 2 H22F H 0.3968 0.2989 0.5117 0.122 Uiso 0.50 1 calc PR A 2 N5 N 0.2683(4) 0.7998(5) 0.7246(8) 0.039(2) Uani 0.50 1 d PD . . C23 C 0.3272(7) 0.8261(8) 0.7621(10) 0.057(2) Uani 0.50 1 d PDU . . H23A H 0.3521 0.7953 0.8044 0.068 Uiso 0.50 1 calc PR A . C24 C 0.3502(7) 0.8949(8) 0.7398(11) 0.060(2) Uani 0.50 1 d PDU A . H24A H 0.3896 0.9118 0.7659 0.071 Uiso 0.50 1 calc PR . . C25 C 0.3101(8) 0.9389(9) 0.6743(11) 0.068(3) Uani 0.50 1 d PDU . . C26 C 0.2500 0.9141(6) 0.6367(9) 0.0623(19) Uani 1 2 d SDU . . H26A H 0.2321 0.9463 0.5896 0.075 Uiso 0.50 1 d PR . . C27 C 0.2342(6) 0.8457(7) 0.6642(9) 0.056(2) Uani 0.50 1 d PDU . . H27A H 0.1956 0.8302 0.6342 0.068 Uiso 0.50 1 d PR A . C28 C 0.3378(9) 1.0122(10) 0.6407(17) 0.080(4) Uani 0.50 1 d PU A . H28A H 0.3784 1.0202 0.6759 0.120 Uiso 0.50 1 calc PR . . H28B H 0.3081 1.0509 0.6589 0.120 Uiso 0.50 1 calc PR . . H28C H 0.3446 1.0120 0.5659 0.120 Uiso 0.50 1 calc PR . . B1 B 0.5158(9) 0.4931(10) 0.0447(15) 0.265(8) Uani 0.50 1 d PDU . 1 F2 F 0.4883(15) 0.5633(12) 0.035(2) 0.239(8) Uani 0.50 1 d PDU . 1 F3 F 0.5637(11) 0.4841(17) -0.032(2) 0.276(9) Uani 0.50 1 d PDU . 1 F4 F 0.4683(14) 0.4392(15) 0.031(2) 0.259(9) Uani 0.50 1 d PDU . 1 F5 F 0.5427(12) 0.4862(16) 0.1453(17) 0.280(9) Uani 0.50 1 d PDU . 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.01835(14) 0.03115(16) 0.01729(15) 0.00382(14) 0.00060(14) -0.00218(12) Cd2 0.0384(3) 0.0311(2) 0.0151(2) 0.0043(2) 0.000 0.000 F1 0.0225(19) 0.035(2) 0.0172(18) 0.0001(15) 0.000 0.000 O1 0.050(2) 0.088(3) 0.050(3) 0.031(2) -0.020(2) -0.036(2) O2 0.058(3) 0.079(3) 0.032(2) 0.014(2) -0.022(2) -0.036(3) N1 0.022(2) 0.053(3) 0.030(2) -0.002(2) -0.0068(18) -0.003(2) C1 0.042(2) 0.056(3) 0.041(2) 0.011(2) -0.013(2) -0.018(2) C2 0.034(2) 0.056(3) 0.030(2) 0.007(2) -0.0105(19) -0.016(2) C3 0.037(3) 0.052(3) 0.033(2) 0.008(2) -0.012(2) -0.017(2) C4 0.035(2) 0.051(3) 0.035(2) 0.010(2) -0.014(2) -0.011(2) C5 0.037(3) 0.054(3) 0.037(3) 0.011(2) -0.010(2) -0.016(2) C6 0.045(2) 0.058(2) 0.038(2) 0.014(2) -0.016(2) -0.015(2) O3 0.046(5) 0.033(5) 0.016(4) -0.005(4) -0.009(3) 0.013(4) O4 0.045(4) 0.055(5) 0.030(4) -0.002(4) 0.010(3) 0.006(4) C7 0.059(3) 0.051(3) 0.026(3) -0.003(3) 0.000 0.000 C8 0.075(4) 0.058(4) 0.032(3) -0.003(3) 0.000 0.000 C9 0.066(4) 0.056(4) 0.034(4) 0.000(4) 0.006(4) -0.001(4) C10 0.071(4) 0.057(4) 0.035(4) -0.001(4) 0.005(4) 0.005(4) N2 0.100(5) 0.072(4) 0.049(4) 0.010(3) 0.000 0.000 C11 0.078(4) 0.066(4) 0.039(4) -0.002(4) 0.011(4) -0.018(4) C12 0.080(5) 0.067(4) 0.042(4) -0.001(4) 0.007(4) -0.013(4) O5 0.045(2) 0.044(2) 0.084(3) 0.028(2) 0.011(2) 0.0082(18) N3 0.038(3) 0.035(3) 0.030(3) 0.009(3) 0.000 0.000 C13 0.042(3) 0.038(3) 0.056(3) 0.008(3) 0.000 0.000 C14 0.041(3) 0.041(3) 0.057(4) 0.010(3) 0.000 0.000 C15 0.047(3) 0.055(3) 0.109(4) 0.033(3) -0.011(3) -0.011(3) C16 0.037(3) 0.056(3) 0.109(4) 0.037(3) -0.008(3) -0.006(3) N4A 0.042(10) 0.037(4) 0.050(4) 0.005(3) 0.012(6) 0.020(9) C17A 0.082(3) 0.058(3) 0.075(3) 0.003(3) -0.001(3) 0.000(3) C18A 0.084(3) 0.059(3) 0.077(3) 0.000(3) -0.001(3) 0.000(3) C19A 0.083(3) 0.058(3) 0.077(3) 0.003(3) -0.001(3) 0.001(3) C20A 0.084(3) 0.061(3) 0.078(3) 0.003(3) -0.001(3) 0.003(3) C21A 0.080(3) 0.058(3) 0.074(3) 0.003(3) -0.002(3) 0.001(3) C22A 0.093(4) 0.065(4) 0.087(4) 0.002(4) 0.000(4) 0.007(4) N4B 0.042(10) 0.037(4) 0.050(4) 0.005(3) 0.012(6) 0.020(9) C17B 0.082(3) 0.058(3) 0.075(3) 0.003(3) -0.001(3) 0.000(3) C18B 0.084(3) 0.059(3) 0.077(3) 0.000(3) -0.001(3) 0.000(3) C19B 0.083(3) 0.058(3) 0.077(3) 0.003(3) -0.001(3) 0.001(3) C20B 0.084(3) 0.061(3) 0.078(3) 0.003(3) -0.001(3) 0.003(3) C21B 0.080(3) 0.058(3) 0.074(3) 0.003(3) -0.002(3) 0.001(3) C22B 0.093(4) 0.065(4) 0.087(4) 0.002(4) 0.000(4) 0.007(4) N5 0.028(6) 0.049(4) 0.039(4) 0.000(5) -0.001(4) -0.009(3) C23 0.057(4) 0.056(4) 0.056(4) 0.001(3) -0.005(3) -0.007(3) C24 0.060(4) 0.059(4) 0.060(4) 0.001(3) -0.005(3) -0.008(3) C25 0.074(5) 0.063(4) 0.068(5) -0.001(4) 0.002(4) -0.002(4) C26 0.069(4) 0.055(3) 0.063(4) 0.001(3) 0.000 0.000 C27 0.061(4) 0.052(4) 0.056(4) -0.001(4) -0.004(4) -0.007(4) C28 0.090(7) 0.070(6) 0.081(6) 0.002(6) -0.002(6) -0.005(6) B1 0.266(9) 0.260(9) 0.268(9) 0.000(6) -0.001(6) 0.000(6) F2 0.243(11) 0.226(10) 0.248(10) 0.009(7) -0.003(8) -0.009(8) F3 0.276(11) 0.273(11) 0.279(11) -0.003(8) 0.005(8) 0.000(8) F4 0.267(11) 0.244(11) 0.265(10) -0.007(8) -0.001(8) 0.000(8) F5 0.282(11) 0.280(11) 0.279(11) 0.002(8) -0.006(8) 0.006(8) _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 Cd1 O5 2.249(4) . ? Cd1 O2 2.262(4) . ? Cd1 O4 2.263(11) 3 ? Cd1 N4B 2.26(4) . ? Cd1 F1 2.271(2) . ? Cd1 O3 2.288(9) . ? Cd1 N1 2.346(4) 6_664 ? Cd1 N4A 2.42(4) . ? Cd2 F1 2.239(4) . ? Cd2 O1 2.292(5) . ? Cd2 O1 2.292(5) 3 ? Cd2 N3 2.333(7) 5_545 ? Cd2 N5 2.370(9) . ? Cd2 N5 2.370(9) 3 ? Cd2 N2 2.371(10) 1_556 ? F1 Cd1 2.271(2) 3 ? O1 C1 1.260(8) . ? O2 C1 1.228(7) . ? N1 C4 1.331(8) . ? N1 C5 1.334(8) . ? N1 Cd1 2.346(4) 6_665 ? C1 C2 1.529(7) . ? C2 C3 1.378(8) . ? C2 C6 1.385(8) . ? C3 C4 1.376(8) . ? C3 H3A 0.9300 . ? C4 H4A 0.9300 . ? C5 C6 1.378(8) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? O3 O4 0.637(10) 3 ? O3 C7 1.336(10) . ? O4 O3 0.637(10) 3 ? O4 C7 1.144(12) . ? O4 Cd1 2.263(11) 3 ? C7 O4 1.144(12) 3 ? C7 O3 1.336(10) 3 ? C7 C8 1.517(12) . ? C8 C12 1.370(5) . ? C8 C12 1.370(5) 3 ? C8 C9 1.412(5) 3 ? C8 C9 1.412(5) . ? C9 C12 1.081(14) 3 ? C9 C10 1.402(5) . ? C9 C11 1.719(15) 3 ? C9 H9A 0.9600 . ? C10 C11 1.011(14) 3 ? C10 N2 1.385(5) . ? C10 C12 1.755(15) 3 ? C10 H10A 0.9599 . ? N2 C11 1.313(5) . ? N2 C11 1.313(5) 3 ? N2 C10 1.385(5) 3 ? N2 Cd2 2.371(10) 1_554 ? C11 C10 1.011(14) 3 ? C11 C12 1.373(5) . ? C11 C9 1.719(15) 3 ? C11 C11 1.948(18) 3 ? C11 H11A 0.9601 . ? C12 C9 1.081(14) 3 ? C12 C10 1.755(15) 3 ? C12 H12A 0.9599 . ? O5 C13 1.231(6) . ? N3 C16 1.312(8) 3 ? N3 C16 1.312(8) . ? N3 Cd2 2.333(6) 5_554 ? C13 O5 1.231(6) 3 ? C13 C14 1.508(12) . ? C14 C15 1.351(9) 3 ? C14 C15 1.351(9) . ? C15 C16 1.385(10) . ? C15 H15A 0.9599 . ? C16 H16A 0.9601 . ? N4A C17A 1.24(3) . ? N4A C21A 1.35(3) . ? C17A C18A 1.374(10) . ? C17A H17A 0.9300 . ? C18A C19A 1.375(10) . ? C18A H18A 0.9300 . ? C19A C20A 1.379(10) . ? C19A C22A 1.47(2) . ? C20A C21A 1.31(2) . ? C20A H20A 0.9300 . ? C21A H21A 0.9300 . ? C22A H22A 0.9600 . ? C22A H22B 0.9600 . ? C22A H22C 0.9600 . ? N4B C21B 1.34(3) . ? N4B C17B 1.39(3) . ? C17B C18B 1.376(10) . ? C17B H17B 0.9300 . ? C18B C19B 1.368(10) . ? C18B H18B 0.9300 . ? C19B C20B 1.375(10) . ? C19B C22B 1.58(2) . ? C20B C21B 1.40(2) . ? C20B H20B 0.9300 . ? C21B H21B 0.9300 . ? C22B H22D 0.9600 . ? C22B H22E 0.9600 . ? C22B H22F 0.9600 . ? N5 N5 0.755(15) 3 ? N5 C27 1.132(15) 3 ? N5 C27 1.332(16) . ? N5 C23 1.389(18) . ? C23 C24 1.36(2) . ? C23 C27 1.81(2) 3 ? C23 H23A 0.9300 . ? C24 C25 1.42(2) . ? C24 H24A 0.9300 . ? C25 C26 1.402(18) . ? C25 C28 1.51(2) . ? C25 C27 1.92(2) 3 ? C26 C27 1.329(16) 3 ? C26 C27 1.329(16) . ? C26 C25 1.402(18) 3 ? C26 H26A 0.9135 . ? C27 C27 0.65(3) 3 ? C27 N5 1.132(15) 3 ? C27 C23 1.81(2) 3 ? C27 C25 1.92(2) 3 ? C27 H27A 0.9272 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? B1 B1 0.70(4) 2_665 ? B1 F2 1.03(4) 2_665 ? B1 F4 1.28(4) 2_665 ? B1 F4 1.395(10) . ? B1 F3 1.398(10) . ? B1 F2 1.398(10) . ? B1 F5 1.399(10) . ? B1 F5 1.80(3) 2_665 ? B1 F3 1.95(3) 2_665 ? F2 F4 0.90(3) 2_665 ? F2 B1 1.03(4) 2_665 ? F2 F3 1.62(3) 2_665 ? F3 F2 1.62(3) 2_665 ? F3 F4 1.74(4) 2_665 ? F3 B1 1.95(3) 2_665 ? F4 F2 0.90(3) 2_665 ? F4 B1 1.28(4) 2_665 ? F4 F3 1.74(4) 2_665 ? F5 B1 1.80(3) 2_665 ? 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 O5 Cd1 O2 92.1(2) . . ? O5 Cd1 O4 79.4(4) . 3 ? O2 Cd1 O4 164.1(3) . 3 ? O5 Cd1 N4B 168.6(5) . . ? O2 Cd1 N4B 97.0(5) . . ? O4 Cd1 N4B 93.3(6) 3 . ? O5 Cd1 F1 89.88(15) . . ? O2 Cd1 F1 93.40(15) . . ? O4 Cd1 F1 99.9(3) 3 . ? N4B Cd1 F1 82.7(4) . . ? O5 Cd1 O3 95.5(3) . . ? O2 Cd1 O3 165.4(3) . . ? O4 Cd1 O3 16.1(3) 3 . ? N4B Cd1 O3 77.3(5) . . ? F1 Cd1 O3 99.1(3) . . ? O5 Cd1 N1 85.13(17) . 6_664 ? O2 Cd1 N1 82.88(18) . 6_664 ? O4 Cd1 N1 83.0(3) 3 6_664 ? N4B Cd1 N1 102.8(4) . 6_664 ? F1 Cd1 N1 173.65(16) . 6_664 ? O3 Cd1 N1 85.3(3) . 6_664 ? O5 Cd1 N4A 176.0(5) . . ? O2 Cd1 N4A 91.9(5) . . ? O4 Cd1 N4A 96.6(6) 3 . ? N4B Cd1 N4A 9.1(8) . . ? F1 Cd1 N4A 90.5(4) . . ? O3 Cd1 N4A 80.5(6) . . ? N1 Cd1 N4A 94.8(4) 6_664 . ? F1 Cd2 O1 93.15(15) . . ? F1 Cd2 O1 93.15(15) . 3 ? O1 Cd2 O1 172.4(2) . 3 ? F1 Cd2 N3 99.0(2) . 5_545 ? O1 Cd2 N3 87.39(13) . 5_545 ? O1 Cd2 N3 87.39(13) 3 5_545 ? F1 Cd2 N5 92.4(3) . . ? O1 Cd2 N5 82.9(2) . . ? O1 Cd2 N5 101.2(2) 3 . ? N3 Cd2 N5 165.4(3) 5_545 . ? F1 Cd2 N5 92.4(3) . 3 ? O1 Cd2 N5 101.2(2) . 3 ? O1 Cd2 N5 82.9(2) 3 3 ? N3 Cd2 N5 165.4(3) 5_545 3 ? N5 Cd2 N5 18.3(4) . 3 ? F1 Cd2 N2 179.2(2) . 1_556 ? O1 Cd2 N2 86.82(15) . 1_556 ? O1 Cd2 N2 86.82(15) 3 1_556 ? N3 Cd2 N2 80.2(3) 5_545 1_556 ? N5 Cd2 N2 88.4(3) . 1_556 ? N5 Cd2 N2 88.4(3) 3 1_556 ? Cd2 F1 Cd1 122.41(9) . 3 ? Cd2 F1 Cd1 122.41(9) . . ? Cd1 F1 Cd1 109.21(16) 3 . ? C1 O1 Cd2 127.3(4) . . ? C1 O2 Cd1 133.9(4) . . ? C4 N1 C5 117.3(5) . . ? C4 N1 Cd1 120.0(4) . 6_665 ? C5 N1 Cd1 122.6(4) . 6_665 ? O2 C1 O1 128.5(6) . . ? O2 C1 C2 116.6(5) . . ? O1 C1 C2 114.9(5) . . ? C3 C2 C6 118.5(5) . . ? C3 C2 C1 122.0(5) . . ? C6 C2 C1 119.5(5) . . ? C4 C3 C2 118.2(5) . . ? C4 C3 H3A 120.9 . . ? C2 C3 H3A 120.9 . . ? N1 C4 C3 124.1(5) . . ? N1 C4 H4A 118.0 . . ? C3 C4 H4A 118.0 . . ? N1 C5 C6 122.6(5) . . ? N1 C5 H5A 118.7 . . ? C6 C5 H5A 118.7 . . ? C5 C6 C2 119.3(6) . . ? C5 C6 H6A 120.3 . . ? C2 C6 H6A 120.3 . . ? O4 O3 C7 58.8(15) 3 . ? O4 O3 Cd1 79.8(15) 3 . ? C7 O3 Cd1 123.4(7) . . ? O3 O4 C7 92.8(18) 3 . ? O3 O4 Cd1 84.2(16) 3 3 ? C7 O4 Cd1 139.9(10) . 3 ? O4 C7 O4 119.8(15) 3 . ? O4 C7 O3 28.4(6) 3 . ? O4 C7 O3 127.2(9) . . ? O4 C7 O3 127.2(9) 3 3 ? O4 C7 O3 28.4(6) . 3 ? O3 C7 O3 118.2(11) . 3 ? O4 C7 C8 114.3(8) 3 . ? O4 C7 C8 114.3(7) . . ? O3 C7 C8 118.2(5) . . ? O3 C7 C8 118.2(5) 3 . ? C12 C8 C12 103.3(10) . 3 ? C12 C8 C9 45.7(6) . 3 ? C12 C8 C9 122.9(10) 3 3 ? C12 C8 C9 122.9(10) . . ? C12 C8 C9 45.7(6) 3 . ? C9 C8 C9 104.6(9) 3 . ? C12 C8 C7 119.9(7) . . ? C12 C8 C7 119.9(7) 3 . ? C9 C8 C7 117.1(6) 3 . ? C9 C8 C7 117.1(6) . . ? C12 C9 C10 88.9(9) 3 . ? C12 C9 C8 65.1(5) 3 . ? C10 C9 C8 115.9(10) . . ? C12 C9 C11 53.0(7) 3 3 ? C10 C9 C11 36.0(5) . 3 ? C8 C9 C11 94.3(8) . 3 ? C12 C9 H9A 115.1 3 . ? C10 C9 H9A 123.9 . . ? C8 C9 H9A 120.1 . . ? C11 C9 H9A 135.9 3 . ? C11 C10 N2 64.3(5) 3 . ? C11 C10 C9 89.3(9) 3 . ? N2 C10 C9 122.8(11) . . ? C11 C10 C12 51.3(7) 3 3 ? N2 C10 C12 100.4(8) . 3 ? C9 C10 C12 38.0(5) . 3 ? C11 C10 H10A 118.6 3 . ? N2 C10 H10A 120.7 . . ? C9 C10 H10A 116.5 . . ? C12 C10 H10A 128.0 3 . ? C11 N2 C11 95.7(11) . 3 ? C11 N2 C10 43.9(6) . 3 ? C11 N2 C10 115.2(11) 3 3 ? C11 N2 C10 115.2(11) . . ? C11 N2 C10 43.9(6) 3 . ? C10 N2 C10 101.2(10) 3 . ? C11 N2 Cd2 127.5(7) . 1_554 ? C11 N2 Cd2 127.5(7) 3 1_554 ? C10 N2 Cd2 116.7(6) 3 1_554 ? C10 N2 Cd2 116.7(6) . 1_554 ? C10 C11 N2 71.8(5) 3 . ? C10 C11 C12 93.6(9) 3 . ? N2 C11 C12 128.9(12) . . ? C10 C11 C9 54.7(7) 3 3 ? N2 C11 C9 106.8(9) . 3 ? C12 C11 C9 39.0(5) . 3 ? C10 C11 C11 95.4(6) 3 3 ? N2 C11 C11 42.1(5) . 3 ? C12 C11 C11 94.2(5) . 3 ? C9 C11 C11 94.8(4) 3 3 ? C10 C11 H11A 105.3 3 . ? N2 C11 H11A 112.4 . . ? C12 C11 H11A 118.8 . . ? C9 C11 H11A 126.1 3 . ? C11 C11 H11A 139.0 3 . ? C9 C12 C8 69.2(5) 3 . ? C9 C12 C11 88.1(9) 3 . ? C8 C12 C11 114.3(11) . . ? C9 C12 C10 53.0(6) 3 3 ? C8 C12 C10 98.8(8) . 3 ? C11 C12 C10 35.1(5) . 3 ? C9 C12 H12A 123.0 3 . ? C8 C12 H12A 124.7 . . ? C11 C12 H12A 119.4 . . ? C10 C12 H12A 133.0 3 . ? C13 O5 Cd1 134.7(5) . . ? C16 N3 C16 114.5(8) 3 . ? C16 N3 Cd2 121.4(4) 3 5_554 ? C16 N3 Cd2 121.4(4) . 5_554 ? O5 C13 O5 127.6(8) . 3 ? O5 C13 C14 116.2(4) . . ? O5 C13 C14 116.2(4) 3 . ? C15 C14 C15 116.2(9) 3 . ? C15 C14 C13 121.7(4) 3 . ? C15 C14 C13 121.7(4) . . ? C14 C15 C16 120.1(7) . . ? C14 C15 H15A 119.6 . . ? C16 C15 H15A 120.3 . . ? N3 C16 C15 124.2(7) . . ? N3 C16 H16A 118.1 . . ? C15 C16 H16A 117.7 . . ? C17A N4A C21A 116(3) . . ? C17A N4A Cd1 125(2) . . ? C21A N4A Cd1 119.4(17) . . ? N4A C17A C18A 126(2) . . ? N4A C17A H17A 117.0 . . ? C18A C17A H17A 117.0 . . ? C17A C18A C19A 119.7(16) . . ? C17A C18A H18A 120.2 . . ? C19A C18A H18A 120.2 . . ? C18A C19A C20A 113.4(15) . . ? C18A C19A C22A 123.6(14) . . ? C20A C19A C22A 123.0(15) . . ? C21A C20A C19A 122.2(17) . . ? C21A C20A H20A 118.9 . . ? C19A C20A H20A 118.9 . . ? C20A C21A N4A 123(2) . . ? C20A C21A H21A 118.4 . . ? N4A C21A H21A 118.4 . . ? C19A C22A H22A 109.5 . . ? C19A C22A H22B 109.5 . . ? H22A C22A H22B 109.5 . . ? C19A C22A H22C 109.5 . . ? H22A C22A H22C 109.5 . . ? H22B C22A H22C 109.5 . . ? C21B N4B C17B 114(3) . . ? C21B N4B Cd1 123.8(19) . . ? C17B N4B Cd1 121.9(16) . . ? C18B C17B N4B 122.1(19) . . ? C18B C17B H17B 119.0 . . ? N4B C17B H17B 119.0 . . ? C19B C18B C17B 122.3(16) . . ? C19B C18B H18B 118.9 . . ? C17B C18B H18B 118.9 . . ? C18B C19B C20B 117.6(16) . . ? C18B C19B C22B 112.1(13) . . ? C20B C19B C22B 130.3(15) . . ? C19B C20B C21B 118.0(17) . . ? C19B C20B H20B 121.0 . . ? C21B C20B H20B 121.0 . . ? N4B C21B C20B 126(2) . . ? N4B C21B H21B 116.9 . . ? C20B C21B H21B 116.9 . . ? C19B C22B H22D 109.5 . . ? C19B C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? C19B C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? N5 N5 C27 87.4(8) 3 3 ? N5 N5 C27 58.1(6) 3 . ? C27 N5 C27 29.2(11) 3 . ? N5 N5 C23 151.0(4) 3 . ? C27 N5 C23 91.2(10) 3 . ? C27 N5 C23 116.4(11) . . ? N5 N5 Cd2 80.83(19) 3 . ? C27 N5 Cd2 137.4(7) 3 . ? C27 N5 Cd2 123.2(7) . . ? C23 N5 Cd2 117.9(8) . . ? C24 C23 N5 123.2(15) . . ? C24 C23 C27 85.6(11) . 3 ? N5 C23 C27 38.7(7) . 3 ? C24 C23 H23A 118.4 . . ? N5 C23 H23A 118.4 . . ? C27 C23 H23A 154.4 3 . ? C23 C24 C25 115.5(15) . . ? C23 C24 H24A 122.2 . . ? C25 C24 H24A 122.2 . . ? C26 C25 C24 122.5(15) . . ? C26 C25 C28 121.4(16) . . ? C24 C25 C28 116.0(15) . . ? C26 C25 C27 43.7(7) . 3 ? C24 C25 C27 79.9(11) . 3 ? C28 C25 C27 159.1(14) . 3 ? C27 C26 C27 28.4(11) 3 . ? C27 C26 C25 89.5(9) 3 . ? C27 C26 C25 115.1(11) . . ? C27 C26 C25 115.1(11) 3 3 ? C27 C26 C25 89.5(9) . 3 ? C25 C26 C25 124.3(10) . 3 ? C27 C26 H26A 150.1 3 . ? C27 C26 H26A 131.9 . . ? C25 C26 H26A 112.2 . . ? C25 C26 H26A 70.2 3 . ? C27 C27 N5 92.6(8) 3 3 ? C27 C27 C26 75.8(6) 3 . ? N5 C27 C26 151.0(11) 3 . ? C27 C27 N5 58.1(6) 3 . ? N5 C27 N5 34.5(8) 3 . ? C26 C27 N5 127.2(11) . . ? C27 C27 C23 134.4(6) 3 3 ? N5 C27 C23 50.1(7) 3 3 ? C26 C27 C23 122.4(8) . 3 ? N5 C27 C23 81.5(8) . 3 ? C27 C27 C25 118.4(6) 3 3 ? N5 C27 C25 125.2(9) 3 3 ? C26 C27 C25 46.8(7) . 3 ? N5 C27 C25 139.4(8) . 3 ? C23 C27 C25 78.1(8) 3 3 ? C27 C27 H27A 149.3 3 . ? N5 C27 H27A 91.0 3 . ? C26 C27 H27A 112.6 . . ? N5 C27 H27A 120.1 . . ? C23 C27 H27A 67.7 3 . ? C25 C27 H27A 83.4 3 . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? B1 B1 F2 106(4) 2_665 2_665 ? B1 B1 F4 84(3) 2_665 2_665 ? F2 B1 F4 162(2) 2_665 2_665 ? B1 B1 F4 66(3) 2_665 . ? F2 B1 F4 40.1(19) 2_665 . ? F4 B1 F4 146.4(18) 2_665 . ? B1 B1 F3 134.6(12) 2_665 . ? F2 B1 F3 81.8(19) 2_665 . ? F4 B1 F3 80.6(17) 2_665 . ? F4 B1 F3 109.2(8) . . ? B1 B1 F2 45(3) 2_665 . ? F2 B1 F2 149(2) 2_665 . ? F4 B1 F2 38.9(15) 2_665 . ? F4 B1 F2 109.9(8) . . ? F3 B1 F2 109.4(8) . . ? B1 B1 F5 113.8(10) 2_665 . ? F2 B1 F5 93(2) 2_665 . ? F4 B1 F5 96.2(19) 2_665 . ? F4 B1 F5 109.2(8) . . ? F3 B1 F5 110.2(8) . . ? F2 B1 F5 109.0(8) . . ? B1 B1 F5 45.4(10) 2_665 2_665 ? F2 B1 F5 104(2) 2_665 2_665 ? F4 B1 F5 93.9(18) 2_665 2_665 ? F4 B1 F5 76.2(18) . 2_665 ? F3 B1 F5 174.3(19) . 2_665 ? F2 B1 F5 66.4(17) . 2_665 ? F5 B1 F5 68.7(16) . 2_665 ? B1 B1 F3 30.6(9) 2_665 2_665 ? F2 B1 F3 95(2) 2_665 2_665 ? F4 B1 F3 86.8(17) 2_665 2_665 ? F4 B1 F3 59.7(13) . 2_665 ? F3 B1 F3 105.8(16) . 2_665 ? F2 B1 F3 54.6(13) . 2_665 ? F5 B1 F3 143.9(17) . 2_665 ? F5 B1 F3 75.3(13) 2_665 2_665 ? F4 F2 B1 92(3) 2_665 2_665 ? F4 F2 B1 64(2) 2_665 . ? B1 F2 B1 29(2) 2_665 . ? F4 F2 F3 127(3) 2_665 2_665 ? B1 F2 F3 59.0(17) 2_665 2_665 ? B1 F2 F3 80.5(15) . 2_665 ? B1 F3 F2 39.2(13) . 2_665 ? B1 F3 F4 46.7(12) . 2_665 ? F2 F3 F4 85.9(12) 2_665 2_665 ? B1 F3 B1 14.8(7) . 2_665 ? F2 F3 B1 44.9(8) 2_665 2_665 ? F4 F3 B1 43.9(8) 2_665 2_665 ? F2 F4 B1 78(2) 2_665 2_665 ? F2 F4 B1 48(2) 2_665 . ? B1 F4 B1 29.9(17) 2_665 . ? F2 F4 F3 116(3) 2_665 2_665 ? B1 F4 F3 52.6(14) 2_665 2_665 ? B1 F4 F3 76.4(14) . 2_665 ? B1 F5 B1 20.8(10) . 2_665 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.930 _refine_diff_density_min -0.825 _refine_diff_density_rms 0.099 # Attachment '- compound-2-zx3-47a.cif' # Supplementary Material (ESI) for Chemical Communications data_compound-2 _database_code_depnum_ccdc_archive 'CCDC 800122' #TrackingRef '- compound-2-zx3-47a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H42 Cd3 F N9 O6, C10 H8 N2, 2 (BF4), 2(H2O)' _chemical_formula_sum 'C60 H54 B2 Cd3 F9 N11 O8' _chemical_formula_weight 1586.96 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.028(6) _cell_length_b 12.607(3) _cell_length_c 23.179(6) _cell_angle_alpha 90.00 _cell_angle_beta 103.760(5) _cell_angle_gamma 90.00 _cell_volume 6252(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7859 _cell_measurement_theta_min 3.1051 _cell_measurement_theta_max 27.4797 _exptl_crystal_description Lathe _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.686 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3160 _exptl_absorpt_coefficient_mu 1.101 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8766 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku/MSC Inc., 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 20977 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0238 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 25.90 _reflns_number_total 6031 _reflns_number_gt 5689 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND. Version 3.0. Crystal Impact' _computing_publication_material 'Windows Word 2003' _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^)+(0.0400P)^2^+8.5000P] 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 6031 _refine_ls_number_parameters 460 _refine_ls_number_restraints 172 _refine_ls_R_factor_all 0.0291 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0703 _refine_ls_wR_factor_gt 0.0683 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.113 _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 Cd1 Cd 0.5000 0.400808(18) 0.2500 0.01901(8) Uani 1 2 d S . . Cd2 Cd 0.597525(8) 0.667749(13) 0.270600(8) 0.02014(7) Uani 1 1 d . . . F1 F 0.5000 0.58244(15) 0.2500 0.0239(4) Uani 1 2 d S . . O1 O 0.59944(8) 0.38252(16) 0.24409(10) 0.0384(5) Uani 1 1 d . . . O2 O 0.65759(9) 0.52158(15) 0.28069(10) 0.0382(5) Uani 1 1 d . . . O3 O 0.55083(9) 0.82607(14) 0.27125(10) 0.0367(5) Uani 1 1 d . . . N1 N 0.81147(10) 0.26637(18) 0.23330(10) 0.0291(5) Uani 1 1 d . . . N2 N 0.5000 1.2110(2) 0.2500 0.0291(7) Uani 1 2 d S . . N3 N 0.52603(12) 0.38746(19) 0.35514(10) 0.0322(5) Uani 1 1 d . . . N4 N 0.58441(11) 0.3347(2) 0.66716(11) 0.0357(6) Uani 1 1 d . . . N5 N 0.62946(11) 0.68454(19) 0.37386(11) 0.0313(5) Uani 1 1 d . . . C1 C 0.64994(11) 0.4311(2) 0.25909(11) 0.0218(5) Uani 1 1 d . . . C2 C 0.70679(11) 0.3728(2) 0.25005(11) 0.0236(5) Uani 1 1 d . . . C3 C 0.70129(12) 0.2764(2) 0.22155(13) 0.0321(6) Uani 1 1 d . . . H3A H 0.6623 0.2452 0.2078 0.039 Uiso 1 1 calc R . . C4 C 0.75467(12) 0.2266(2) 0.21371(13) 0.0320(6) Uani 1 1 d . . . H4A H 0.7505 0.1620 0.1937 0.038 Uiso 1 1 calc R . . C5 C 0.81626(13) 0.3597(3) 0.26114(17) 0.0443(8) Uani 1 1 d . . . H5A H 0.8559 0.3886 0.2752 0.053 Uiso 1 1 calc R . . C6 C 0.76581(13) 0.4153(2) 0.27009(16) 0.0426(8) Uani 1 1 d . . . H6A H 0.7712 0.4805 0.2893 0.051 Uiso 1 1 calc R . . C7 C 0.5000 0.8706(3) 0.2500 0.0270(8) Uani 1 2 d S . . C8 C 0.5000 0.9901(3) 0.2500 0.0262(8) Uani 1 2 d S . . C9 C 0.55313(12) 1.0464(2) 0.27673(14) 0.0331(6) Uani 1 1 d . . . H9A H 0.5896 1.0111 0.2953 0.040 Uiso 1 1 calc R . . C10 C 0.55113(13) 1.1554(2) 0.27542(14) 0.0341(6) Uani 1 1 d . . . H10A H 0.5873 1.1925 0.2932 0.041 Uiso 1 1 calc R . . C11 C 0.58195(15) 0.3553(3) 0.38701(13) 0.0386(7) Uani 1 1 d . . . H11A H 0.6131 0.3425 0.3670 0.046 Uiso 1 1 calc R . . C12 C 0.59608(15) 0.3400(3) 0.44738(14) 0.0405(7) Uani 1 1 d . . . H12A H 0.6359 0.3181 0.4672 0.049 Uiso 1 1 calc R . . C13 C 0.55048(14) 0.3574(2) 0.47841(13) 0.0352(6) Uani 1 1 d . . . C14 C 0.49217(15) 0.3892(3) 0.44546(14) 0.0461(8) Uani 1 1 d . . . H14A H 0.4599 0.4009 0.4642 0.055 Uiso 1 1 calc R . . C15 C 0.48211(15) 0.4032(3) 0.38527(13) 0.0432(8) Uani 1 1 d . . . H15A H 0.4426 0.4248 0.3643 0.052 Uiso 1 1 calc R . . C16 C 0.56288(14) 0.3453(3) 0.54345(13) 0.0366(7) Uani 1 1 d . . . C17 C 0.62066(14) 0.3718(3) 0.58020(13) 0.0411(7) Uani 1 1 d . . . H17A H 0.6534 0.3932 0.5639 0.049 Uiso 1 1 calc R . . C18 C 0.62876(14) 0.3658(3) 0.64071(14) 0.0410(7) Uani 1 1 d . . . H18A H 0.6675 0.3845 0.6646 0.049 Uiso 1 1 calc R . . C19 C 0.52975(14) 0.3056(3) 0.63172(14) 0.0463(8) Uani 1 1 d . . . H19A H 0.4985 0.2810 0.6492 0.056 Uiso 1 1 calc R . . C20 C 0.51749(15) 0.3102(3) 0.57101(14) 0.0481(8) Uani 1 1 d . . . H20A H 0.4785 0.2897 0.5483 0.058 Uiso 1 1 calc R . . C21 C 0.65240(17) 0.6033(3) 0.40887(14) 0.0456(8) Uani 1 1 d . . . H21A H 0.6554 0.5377 0.3914 0.055 Uiso 1 1 calc R . . C22 C 0.6719(2) 0.6114(3) 0.46968(16) 0.0593(10) Uani 1 1 d . . . H22A H 0.6867 0.5516 0.4921 0.071 Uiso 1 1 calc R . . C23 C 0.66978(17) 0.7070(3) 0.49751(15) 0.0518(9) Uani 1 1 d . . . C24 C 0.64847(18) 0.7926(3) 0.46079(16) 0.0543(9) Uani 1 1 d . . . H24A H 0.6473 0.8597 0.4771 0.065 Uiso 1 1 calc R . . C25 C 0.62897(15) 0.7790(3) 0.40022(14) 0.0410(7) Uani 1 1 d . . . H25A H 0.6149 0.8378 0.3766 0.049 Uiso 1 1 calc R . . C26 C 0.6899(2) 0.7178(5) 0.56396(17) 0.0799(14) Uani 1 1 d . . . H26B H 0.7017 0.7900 0.5741 0.120 Uiso 1 1 calc R . . H26C H 0.7250 0.6720 0.5790 0.120 Uiso 1 1 calc R . . H26D H 0.6560 0.6983 0.5812 0.120 Uiso 1 1 calc R . . N6 N 0.3850(2) 0.0590(4) 0.3673(2) 0.0935(13) Uani 1 1 d . . . C27 C 0.3730(3) -0.0024(5) 0.4089(3) 0.0973(17) Uani 1 1 d . . . H26A H 0.3331 -0.0308 0.4029 0.117 Uiso 1 1 calc R . . C28 C 0.4166(2) -0.0281(4) 0.4621(2) 0.0836(14) Uani 1 1 d . . . H27A H 0.4052 -0.0718 0.4900 0.100 Uiso 1 1 calc R . . C29 C 0.47610(19) 0.0121(3) 0.47214(18) 0.0596(10) Uani 1 1 d . . . C30 C 0.4889(3) 0.0747(5) 0.4282(2) 0.0862(15) Uani 1 1 d . . . H30A H 0.5288 0.1022 0.4320 0.103 Uiso 1 1 calc R . . C31 C 0.4425(3) 0.0968(5) 0.3782(2) 0.0967(17) Uani 1 1 d . . . H31A H 0.4525 0.1418 0.3500 0.116 Uiso 1 1 calc R . . B1 B 0.70074(19) 0.0916(4) 0.4059(2) 0.0802(15) Uani 1 1 d DU . . F1A F 0.6467(3) 0.0469(11) 0.4085(5) 0.112(3) Uani 0.514(19) 1 d PDU A 1 F2A F 0.6890(6) 0.1723(8) 0.3677(5) 0.137(4) Uani 0.514(19) 1 d PDU A 1 F3A F 0.7300(7) 0.1305(12) 0.4593(4) 0.173(5) Uani 0.514(19) 1 d PDU A 1 F4A F 0.7382(6) 0.0210(9) 0.3897(6) 0.161(4) Uani 0.514(19) 1 d PDU A 1 F1B F 0.6447(3) 0.1034(15) 0.4157(5) 0.123(4) Uani 0.486(19) 1 d PDU A 2 F2B F 0.7108(7) 0.1683(10) 0.3690(5) 0.153(5) Uani 0.486(19) 1 d PDU A 2 F3B F 0.7467(3) 0.0963(11) 0.4547(3) 0.113(4) Uani 0.486(19) 1 d PDU A 2 F4B F 0.7037(9) -0.0019(8) 0.3785(5) 0.172(4) Uani 0.486(19) 1 d PDU A 2 O1W O 0.7436(3) 0.3725(5) 0.4173(3) 0.163(2) Uani 1 1 d . . . H1A H 0.7218 0.3162 0.4125 0.196 Uiso 1 1 d R . . H1B H 0.7496 0.3720 0.4549 0.196 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.01675(13) 0.01636(13) 0.02460(14) 0.000 0.00624(10) 0.000 Cd2 0.01739(11) 0.01842(11) 0.02543(11) -0.00118(6) 0.00673(8) -0.00069(6) F1 0.0197(10) 0.0179(10) 0.0350(11) 0.000 0.0082(9) 0.000 O1 0.0186(9) 0.0355(11) 0.0635(14) -0.0090(10) 0.0147(9) -0.0004(8) O2 0.0268(10) 0.0278(10) 0.0594(14) -0.0109(9) 0.0086(9) 0.0072(8) O3 0.0262(10) 0.0187(9) 0.0615(14) 0.0015(9) 0.0030(10) 0.0047(7) N1 0.0224(11) 0.0295(12) 0.0361(12) -0.0028(10) 0.0083(10) 0.0062(9) N2 0.0304(16) 0.0170(15) 0.0391(18) 0.000 0.0067(14) 0.000 N3 0.0377(13) 0.0335(13) 0.0249(12) -0.0009(10) 0.0064(10) -0.0005(10) N4 0.0291(13) 0.0523(16) 0.0272(12) 0.0045(11) 0.0093(10) 0.0041(10) N5 0.0328(13) 0.0327(13) 0.0281(12) -0.0021(10) 0.0065(10) -0.0017(10) C1 0.0201(12) 0.0237(12) 0.0221(12) 0.0022(10) 0.0057(10) 0.0063(9) C2 0.0189(12) 0.0271(13) 0.0259(13) -0.0006(10) 0.0072(10) 0.0037(10) C3 0.0190(12) 0.0303(15) 0.0460(16) -0.0076(12) 0.0058(12) 0.0010(10) C4 0.0253(13) 0.0258(14) 0.0442(16) -0.0094(12) 0.0067(12) 0.0035(10) C5 0.0197(14) 0.0399(17) 0.073(2) -0.0181(16) 0.0096(14) -0.0015(12) C6 0.0272(14) 0.0298(15) 0.072(2) -0.0205(15) 0.0146(15) -0.0016(11) C7 0.0254(19) 0.0266(19) 0.031(2) 0.000 0.0105(16) 0.000 C8 0.0228(18) 0.0262(19) 0.0295(19) 0.000 0.0060(15) 0.000 C9 0.0259(14) 0.0213(13) 0.0479(17) -0.0013(12) 0.0004(13) 0.0000(10) C10 0.0281(15) 0.0197(13) 0.0497(18) -0.0021(12) -0.0006(13) -0.0020(10) C11 0.0368(16) 0.0509(18) 0.0311(15) 0.0005(13) 0.0143(13) -0.0004(14) C12 0.0336(16) 0.059(2) 0.0292(16) 0.0032(14) 0.0070(13) 0.0037(14) C13 0.0386(16) 0.0392(16) 0.0288(15) -0.0002(12) 0.0102(13) -0.0013(13) C14 0.0385(17) 0.068(2) 0.0345(17) 0.0010(15) 0.0140(14) 0.0104(15) C15 0.0401(17) 0.061(2) 0.0285(15) 0.0008(14) 0.0081(13) 0.0135(15) C16 0.0339(16) 0.0495(18) 0.0276(15) 0.0013(13) 0.0100(13) 0.0014(13) C17 0.0309(15) 0.064(2) 0.0308(16) 0.0047(15) 0.0112(13) -0.0036(14) C18 0.0295(15) 0.062(2) 0.0310(16) 0.0037(14) 0.0061(13) -0.0038(14) C19 0.0294(16) 0.078(2) 0.0329(16) 0.0058(16) 0.0099(13) -0.0055(15) C20 0.0344(17) 0.079(3) 0.0306(16) 0.0036(16) 0.0071(14) -0.0099(16) C21 0.064(2) 0.0369(17) 0.0326(16) 0.0030(13) 0.0051(16) 0.0012(15) C22 0.075(3) 0.060(2) 0.0380(19) 0.0119(17) 0.0047(19) 0.002(2) C23 0.0438(19) 0.077(3) 0.0345(17) -0.0085(17) 0.0083(15) -0.0062(18) C24 0.056(2) 0.059(2) 0.045(2) -0.0227(18) 0.0055(17) -0.0042(18) C25 0.0453(18) 0.0370(17) 0.0371(17) -0.0056(13) 0.0023(14) 0.0011(13) C26 0.076(3) 0.125(4) 0.034(2) -0.011(2) 0.004(2) -0.003(3) N6 0.090(3) 0.108(4) 0.078(3) 0.002(3) 0.012(3) -0.005(3) C27 0.075(3) 0.110(5) 0.097(4) 0.012(3) 0.000(3) -0.019(3) C28 0.073(3) 0.087(3) 0.091(4) 0.010(3) 0.020(3) -0.009(3) C29 0.062(2) 0.054(2) 0.065(2) -0.0094(19) 0.019(2) -0.0010(18) C30 0.081(3) 0.113(4) 0.067(3) 0.008(3) 0.021(3) -0.022(3) C31 0.107(4) 0.114(5) 0.069(3) 0.013(3) 0.021(3) -0.014(4) B1 0.050(3) 0.085(4) 0.097(4) 0.001(3) 0.000(3) -0.002(3) F1A 0.077(4) 0.128(7) 0.133(6) -0.008(6) 0.026(4) -0.033(4) F2A 0.096(7) 0.129(7) 0.160(8) 0.059(6) -0.020(5) 0.002(5) F3A 0.163(9) 0.210(10) 0.111(7) -0.036(7) -0.039(7) -0.007(8) F4A 0.095(7) 0.131(7) 0.259(10) -0.042(7) 0.043(7) 0.003(5) F1B 0.066(4) 0.150(10) 0.155(7) -0.011(7) 0.031(4) 0.012(5) F2B 0.129(10) 0.183(9) 0.135(7) 0.080(7) 0.009(7) -0.028(7) F3B 0.041(3) 0.195(9) 0.096(5) 0.043(5) 0.000(3) 0.015(4) F4B 0.148(9) 0.127(7) 0.232(9) -0.058(6) 0.027(8) 0.000(7) O1W 0.181(5) 0.136(4) 0.190(6) 0.022(4) 0.077(5) -0.018(4) _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 Cd1 O1 2.2389(18) . ? Cd1 O1 2.2389(18) 2_655 ? Cd1 F1 2.290(2) . ? Cd1 N3 2.373(2) . ? Cd1 N3 2.373(2) 2_655 ? Cd1 N2 2.392(3) 1_545 ? Cd2 O3 2.2472(18) . ? Cd2 O2 2.2481(19) . ? Cd2 N5 2.338(2) . ? Cd2 N4 2.346(3) 6_565 ? Cd2 F1 2.3477(10) . ? Cd2 N1 2.379(2) 4_655 ? F1 Cd2 2.3477(10) 2_655 ? O1 C1 1.245(3) . ? O2 C1 1.241(3) . ? O3 C7 1.245(3) . ? N1 C4 1.324(3) . ? N1 C5 1.334(4) . ? N1 Cd2 2.379(2) 4_645 ? N2 C10 1.339(3) . ? N2 C10 1.339(3) 2_655 ? N2 Cd1 2.392(3) 1_565 ? N3 C15 1.336(4) . ? N3 C11 1.340(4) . ? N4 C18 1.330(4) . ? N4 C19 1.337(4) . ? N4 Cd2 2.346(3) 6_566 ? N5 C21 1.330(4) . ? N5 C25 1.339(4) . ? C1 C2 1.509(3) . ? C2 C3 1.374(4) . ? C2 C6 1.381(4) . ? C3 C4 1.383(4) . ? C3 H3A 0.9300 . ? C4 H4A 0.9300 . ? C5 C6 1.370(4) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 O3 1.245(3) 2_655 ? C7 C8 1.507(5) . ? C8 C9 1.383(3) . ? C8 C9 1.383(3) 2_655 ? C9 C10 1.375(4) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.373(4) . ? C11 H11A 0.9300 . ? C12 C13 1.385(4) . ? C12 H12A 0.9300 . ? C13 C14 1.388(4) . ? C13 C16 1.475(4) . ? C14 C15 1.371(4) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 C20 1.381(4) . ? C16 C17 1.393(4) . ? C17 C18 1.373(4) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 C20 1.369(4) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C22 1.376(5) . ? C21 H21A 0.9300 . ? C22 C23 1.373(6) . ? C22 H22A 0.9300 . ? C23 C24 1.385(6) . ? C23 C26 1.504(5) . ? C24 C25 1.378(5) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C26 H26D 0.9600 . ? N6 C27 1.311(7) . ? N6 C31 1.320(7) . ? C27 C28 1.408(7) . ? C27 H26A 0.9300 . ? C28 C29 1.372(6) . ? C28 H27A 0.9300 . ? C29 C30 1.370(6) . ? C29 C29 1.491(8) 5_656 ? C30 C31 1.378(7) . ? C30 H30A 0.9300 . ? C31 H31A 0.9300 . ? B1 F1B 1.315(6) . ? B1 F4A 1.327(6) . ? B1 F3B 1.328(6) . ? B1 F1A 1.331(6) . ? B1 F2A 1.333(6) . ? B1 F3A 1.344(6) . ? B1 F2B 1.345(6) . ? B1 F4B 1.349(6) . ? O1W H1A 0.8500 . ? O1W H1B 0.8501 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cd1 O1 168.18(10) . 2_655 ? O1 Cd1 F1 95.91(5) . . ? O1 Cd1 F1 95.91(5) 2_655 . ? O1 Cd1 N3 93.13(8) . . ? O1 Cd1 N3 86.03(8) 2_655 . ? F1 Cd1 N3 94.07(6) . . ? O1 Cd1 N3 86.03(8) . 2_655 ? O1 Cd1 N3 93.13(8) 2_655 2_655 ? F1 Cd1 N3 94.07(6) . 2_655 ? N3 Cd1 N3 171.87(12) . 2_655 ? O1 Cd1 N2 84.09(5) . 1_545 ? O1 Cd1 N2 84.09(5) 2_655 1_545 ? F1 Cd1 N2 180.0 . 1_545 ? N3 Cd1 N2 85.93(6) . 1_545 ? N3 Cd1 N2 85.93(6) 2_655 1_545 ? O3 Cd2 O2 170.55(8) . . ? O3 Cd2 N5 86.53(8) . . ? O2 Cd2 N5 86.64(8) . . ? O3 Cd2 N4 94.21(9) . 6_565 ? O2 Cd2 N4 91.25(9) . 6_565 ? N5 Cd2 N4 168.91(8) . 6_565 ? O3 Cd2 F1 90.57(7) . . ? O2 Cd2 F1 97.65(7) . . ? N5 Cd2 F1 106.71(6) . . ? N4 Cd2 F1 84.36(6) 6_565 . ? O3 Cd2 N1 85.83(8) . 4_655 ? O2 Cd2 N1 87.25(8) . 4_655 ? N5 Cd2 N1 86.59(8) . 4_655 ? N4 Cd2 N1 82.43(8) 6_565 4_655 ? F1 Cd2 N1 166.01(6) . 4_655 ? Cd1 F1 Cd2 117.26(4) . . ? Cd1 F1 Cd2 117.26(4) . 2_655 ? Cd2 F1 Cd2 125.47(8) . 2_655 ? C1 O1 Cd1 138.98(17) . . ? C1 O2 Cd2 133.74(17) . . ? C7 O3 Cd2 140.2(2) . . ? C4 N1 C5 117.4(2) . . ? C4 N1 Cd2 121.68(17) . 4_645 ? C5 N1 Cd2 120.60(18) . 4_645 ? C10 N2 C10 116.8(3) . 2_655 ? C10 N2 Cd1 121.60(16) . 1_565 ? C10 N2 Cd1 121.60(16) 2_655 1_565 ? C15 N3 C11 116.2(3) . . ? C15 N3 Cd1 119.9(2) . . ? C11 N3 Cd1 123.61(19) . . ? C18 N4 C19 116.8(3) . . ? C18 N4 Cd2 123.3(2) . 6_566 ? C19 N4 Cd2 119.88(19) . 6_566 ? C21 N5 C25 116.7(3) . . ? C21 N5 Cd2 122.2(2) . . ? C25 N5 Cd2 121.0(2) . . ? O2 C1 O1 126.3(2) . . ? O2 C1 C2 117.8(2) . . ? O1 C1 C2 115.9(2) . . ? C3 C2 C6 118.2(2) . . ? C3 C2 C1 121.1(2) . . ? C6 C2 C1 120.7(2) . . ? C2 C3 C4 119.0(2) . . ? C2 C3 H3A 120.5 . . ? C4 C3 H3A 120.5 . . ? N1 C4 C3 123.1(3) . . ? N1 C4 H4A 118.4 . . ? C3 C4 H4A 118.4 . . ? N1 C5 C6 123.4(3) . . ? N1 C5 H5A 118.3 . . ? C6 C5 H5A 118.3 . . ? C5 C6 C2 118.9(3) . . ? C5 C6 H6A 120.5 . . ? C2 C6 H6A 120.5 . . ? O3 C7 O3 126.4(4) . 2_655 ? O3 C7 C8 116.81(18) . . ? O3 C7 C8 116.81(18) 2_655 . ? C9 C8 C9 118.3(3) . 2_655 ? C9 C8 C7 120.87(17) . . ? C9 C8 C7 120.87(17) 2_655 . ? C10 C9 C8 118.9(3) . . ? C10 C9 H9A 120.5 . . ? C8 C9 H9A 120.5 . . ? N2 C10 C9 123.5(3) . . ? N2 C10 H10A 118.2 . . ? C9 C10 H10A 118.2 . . ? N3 C11 C12 124.1(3) . . ? N3 C11 H11A 118.0 . . ? C12 C11 H11A 118.0 . . ? C11 C12 C13 119.4(3) . . ? C11 C12 H12A 120.3 . . ? C13 C12 H12A 120.3 . . ? C12 C13 C14 116.8(3) . . ? C12 C13 C16 122.3(3) . . ? C14 C13 C16 121.0(3) . . ? C15 C14 C13 120.1(3) . . ? C15 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? N3 C15 C14 123.4(3) . . ? N3 C15 H15A 118.3 . . ? C14 C15 H15A 118.3 . . ? C20 C16 C17 116.8(3) . . ? C20 C16 C13 121.9(3) . . ? C17 C16 C13 121.3(3) . . ? C18 C17 C16 119.3(3) . . ? C18 C17 H17A 120.4 . . ? C16 C17 H17A 120.4 . . ? N4 C18 C17 123.8(3) . . ? N4 C18 H18A 118.1 . . ? C17 C18 H18A 118.1 . . ? N4 C19 C20 123.2(3) . . ? N4 C19 H19A 118.4 . . ? C20 C19 H19A 118.4 . . ? C19 C20 C16 120.1(3) . . ? C19 C20 H20A 120.0 . . ? C16 C20 H20A 120.0 . . ? N5 C21 C22 123.3(3) . . ? N5 C21 H21A 118.4 . . ? C22 C21 H21A 118.4 . . ? C23 C22 C21 120.6(4) . . ? C23 C22 H22A 119.7 . . ? C21 C22 H22A 119.7 . . ? C22 C23 C24 116.1(3) . . ? C22 C23 C26 121.7(4) . . ? C24 C23 C26 122.2(4) . . ? C25 C24 C23 120.5(3) . . ? C25 C24 H24A 119.8 . . ? C23 C24 H24A 119.8 . . ? N5 C25 C24 122.8(3) . . ? N5 C25 H25A 118.6 . . ? C24 C25 H25A 118.6 . . ? C23 C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C26 H26D 109.5 . . ? H26B C26 H26D 109.5 . . ? H26C C26 H26D 109.5 . . ? C27 N6 C31 115.1(5) . . ? N6 C27 C28 124.4(5) . . ? N6 C27 H26A 117.8 . . ? C28 C27 H26A 117.8 . . ? C29 C28 C27 119.3(5) . . ? C29 C28 H27A 120.4 . . ? C27 C28 H27A 120.4 . . ? C30 C29 C28 116.3(4) . . ? C30 C29 C29 122.3(5) . 5_656 ? C28 C29 C29 121.4(5) . 5_656 ? C29 C30 C31 120.0(5) . . ? C29 C30 H30A 120.0 . . ? C31 C30 H30A 120.0 . . ? N6 C31 C30 125.0(5) . . ? N6 C31 H31A 117.5 . . ? C30 C31 H31A 117.5 . . ? F1B B1 F4A 142.8(6) . . ? F1B B1 F3B 113.9(6) . . ? F4A B1 F3B 82.6(7) . . ? F1B B1 F1A 32.3(5) . . ? F4A B1 F1A 110.5(5) . . ? F3B B1 F1A 119.4(8) . . ? F1B B1 F2A 89.2(8) . . ? F4A B1 F2A 111.1(6) . . ? F3B B1 F2A 121.3(9) . . ? F1A B1 F2A 108.6(5) . . ? F1B B1 F3A 93.7(8) . . ? F4A B1 F3A 108.1(5) . . ? F3B B1 F3A 25.6(7) . . ? F1A B1 F3A 110.6(6) . . ? F2A B1 F3A 107.9(6) . . ? F1B B1 F2B 109.4(6) . . ? F4A B1 F2B 95.4(10) . . ? F3B B1 F2B 107.6(5) . . ? F1A B1 F2B 128.1(8) . . ? F2A B1 F2B 20.5(9) . . ? F3A B1 F2B 102.0(11) . . ? F1B B1 F4B 109.4(5) . . ? F4A B1 F4B 34.6(5) . . ? F3B B1 F4B 109.1(6) . . ? F1A B1 F4B 78.1(6) . . ? F2A B1 F4B 112.2(11) . . ? F3A B1 F4B 133.4(9) . . ? F2B B1 F4B 107.1(6) . . ? H1A O1W H1B 94.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Cd1 F1 Cd2 -16.27(6) . . . . ? O1 Cd1 F1 Cd2 163.73(6) 2_655 . . . ? N3 Cd1 F1 Cd2 77.31(6) . . . . ? N3 Cd1 F1 Cd2 -102.69(6) 2_655 . . . ? N2 Cd1 F1 Cd2 -103(51) 1_545 . . . ? O1 Cd1 F1 Cd2 163.73(6) . . . 2_655 ? O1 Cd1 F1 Cd2 -16.27(6) 2_655 . . 2_655 ? N3 Cd1 F1 Cd2 -102.69(6) . . . 2_655 ? N3 Cd1 F1 Cd2 77.31(6) 2_655 . . 2_655 ? N2 Cd1 F1 Cd2 77(51) 1_545 . . 2_655 ? O3 Cd2 F1 Cd1 -173.78(6) . . . . ? O2 Cd2 F1 Cd1 1.55(6) . . . . ? N5 Cd2 F1 Cd1 -87.23(6) . . . . ? N4 Cd2 F1 Cd1 92.05(6) 6_565 . . . ? N1 Cd2 F1 Cd1 111.3(3) 4_655 . . . ? O3 Cd2 F1 Cd2 6.22(6) . . . 2_655 ? O2 Cd2 F1 Cd2 -178.45(6) . . . 2_655 ? N5 Cd2 F1 Cd2 92.77(6) . . . 2_655 ? N4 Cd2 F1 Cd2 -87.95(6) 6_565 . . 2_655 ? N1 Cd2 F1 Cd2 -68.7(3) 4_655 . . 2_655 ? O1 Cd1 O1 C1 -150.8(3) 2_655 . . . ? F1 Cd1 O1 C1 29.2(3) . . . . ? N3 Cd1 O1 C1 -65.2(3) . . . . ? N3 Cd1 O1 C1 122.9(3) 2_655 . . . ? N2 Cd1 O1 C1 -150.8(3) 1_545 . . . ? O3 Cd2 O2 C1 179(11) . . . . ? N5 Cd2 O2 C1 135.6(3) . . . . ? N4 Cd2 O2 C1 -55.3(3) 6_565 . . . ? F1 Cd2 O2 C1 29.2(3) . . . . ? N1 Cd2 O2 C1 -137.6(3) 4_655 . . . ? O2 Cd2 O3 C7 -176.6(4) . . . . ? N5 Cd2 O3 C7 -132.8(3) . . . . ? N4 Cd2 O3 C7 58.3(3) 6_565 . . . ? F1 Cd2 O3 C7 -26.1(2) . . . . ? N1 Cd2 O3 C7 140.4(3) 4_655 . . . ? O1 Cd1 N3 C15 173.9(2) . . . . ? O1 Cd1 N3 C15 -17.9(2) 2_655 . . . ? F1 Cd1 N3 C15 77.7(2) . . . . ? N3 Cd1 N3 C15 -102.3(2) 2_655 . . . ? N2 Cd1 N3 C15 -102.3(2) 1_545 . . . ? O1 Cd1 N3 C11 -12.3(2) . . . . ? O1 Cd1 N3 C11 155.9(2) 2_655 . . . ? F1 Cd1 N3 C11 -108.5(2) . . . . ? N3 Cd1 N3 C11 71.5(2) 2_655 . . . ? N2 Cd1 N3 C11 71.5(2) 1_545 . . . ? O3 Cd2 N5 C21 166.3(3) . . . . ? O2 Cd2 N5 C21 -20.2(3) . . . . ? N4 Cd2 N5 C21 -99.5(5) 6_565 . . . ? F1 Cd2 N5 C21 76.8(3) . . . . ? N1 Cd2 N5 C21 -107.7(3) 4_655 . . . ? O3 Cd2 N5 C25 -17.8(2) . . . . ? O2 Cd2 N5 C25 155.6(2) . . . . ? N4 Cd2 N5 C25 76.3(5) 6_565 . . . ? F1 Cd2 N5 C25 -107.4(2) . . . . ? N1 Cd2 N5 C25 68.2(2) 4_655 . . . ? Cd2 O2 C1 O1 -31.0(4) . . . . ? Cd2 O2 C1 C2 149.34(19) . . . . ? Cd1 O1 C1 O2 -7.4(5) . . . . ? Cd1 O1 C1 C2 172.31(19) . . . . ? O2 C1 C2 C3 -174.1(3) . . . . ? O1 C1 C2 C3 6.2(4) . . . . ? O2 C1 C2 C6 5.6(4) . . . . ? O1 C1 C2 C6 -174.1(3) . . . . ? C6 C2 C3 C4 -0.5(4) . . . . ? C1 C2 C3 C4 179.3(3) . . . . ? C5 N1 C4 C3 -0.9(5) . . . . ? Cd2 N1 C4 C3 172.2(2) 4_645 . . . ? C2 C3 C4 N1 1.2(5) . . . . ? C4 N1 C5 C6 -0.1(5) . . . . ? Cd2 N1 C5 C6 -173.3(3) 4_645 . . . ? N1 C5 C6 C2 0.7(6) . . . . ? C3 C2 C6 C5 -0.4(5) . . . . ? C1 C2 C6 C5 179.8(3) . . . . ? Cd2 O3 C7 O3 18.55(18) . . . 2_655 ? Cd2 O3 C7 C8 -161.45(18) . . . . ? O3 C7 C8 C9 -4.96(19) . . . . ? O3 C7 C8 C9 175.04(19) 2_655 . . . ? O3 C7 C8 C9 175.04(19) . . . 2_655 ? O3 C7 C8 C9 -4.96(19) 2_655 . . 2_655 ? C9 C8 C9 C10 -0.3(2) 2_655 . . . ? C7 C8 C9 C10 179.7(2) . . . . ? C10 N2 C10 C9 -0.4(2) 2_655 . . . ? Cd1 N2 C10 C9 179.6(2) 1_565 . . . ? C8 C9 C10 N2 0.7(4) . . . . ? C15 N3 C11 C12 -1.1(5) . . . . ? Cd1 N3 C11 C12 -175.1(2) . . . . ? N3 C11 C12 C13 0.6(5) . . . . ? C11 C12 C13 C14 0.5(5) . . . . ? C11 C12 C13 C16 -178.3(3) . . . . ? C12 C13 C14 C15 -0.9(5) . . . . ? C16 C13 C14 C15 178.0(3) . . . . ? C11 N3 C15 C14 0.7(5) . . . . ? Cd1 N3 C15 C14 174.9(3) . . . . ? C13 C14 C15 N3 0.3(6) . . . . ? C12 C13 C16 C20 -147.0(4) . . . . ? C14 C13 C16 C20 34.3(5) . . . . ? C12 C13 C16 C17 35.0(5) . . . . ? C14 C13 C16 C17 -143.8(3) . . . . ? C20 C16 C17 C18 -2.4(5) . . . . ? C13 C16 C17 C18 175.7(3) . . . . ? C19 N4 C18 C17 1.7(5) . . . . ? Cd2 N4 C18 C17 -177.2(3) 6_566 . . . ? C16 C17 C18 N4 0.7(5) . . . . ? C18 N4 C19 C20 -2.4(5) . . . . ? Cd2 N4 C19 C20 176.5(3) 6_566 . . . ? N4 C19 C20 C16 0.7(6) . . . . ? C17 C16 C20 C19 1.8(5) . . . . ? C13 C16 C20 C19 -176.4(3) . . . . ? C25 N5 C21 C22 3.5(5) . . . . ? Cd2 N5 C21 C22 179.5(3) . . . . ? N5 C21 C22 C23 -1.5(6) . . . . ? C21 C22 C23 C24 -1.4(6) . . . . ? C21 C22 C23 C26 179.1(4) . . . . ? C22 C23 C24 C25 2.1(6) . . . . ? C26 C23 C24 C25 -178.4(4) . . . . ? C21 N5 C25 C24 -2.7(5) . . . . ? Cd2 N5 C25 C24 -178.8(3) . . . . ? C23 C24 C25 N5 0.0(6) . . . . ? C31 N6 C27 C28 0.2(9) . . . . ? N6 C27 C28 C29 -0.4(10) . . . . ? C27 C28 C29 C30 -0.8(8) . . . . ? C27 C28 C29 C29 179.6(5) . . . 5_656 ? C28 C29 C30 C31 2.0(8) . . . . ? C29 C29 C30 C31 -178.3(5) 5_656 . . . ? C27 N6 C31 C30 1.2(10) . . . . ? C29 C30 C31 N6 -2.4(10) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1B F3A 0.85 1.93 2.780(11) 175.6 7_656 O1W H1B F3B 0.85 2.11 2.949(10) 167.0 7_656 O1W H1A F2B 0.85 2.11 2.832(16) 143.1 . O1W H1A F2A 0.85 2.13 2.912(15) 153.2 . _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.90 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.963 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.069 # Attachment '- compound-3-zx3-10a-y.cif' # Supplementary Material (ESI) for Chemical Communications data_compound-3 _database_code_depnum_ccdc_archive 'CCDC 800123' #TrackingRef '- compound-3-zx3-10a-y.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H36 Cd3 F N9 O6, C10 H8 N2, 2(B F4), 2(H2 O)' _chemical_formula_sum 'C58 H48 B2 Cd3 F9 N11 O8' _chemical_formula_weight 1556.89 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.892(10) _cell_length_b 12.609(5) _cell_length_c 23.263(10) _cell_angle_alpha 90.00 _cell_angle_beta 102.894(7) _cell_angle_gamma 90.00 _cell_volume 6260(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6248 _cell_measurement_theta_min 3.1039 _cell_measurement_theta_max 27.4797 _exptl_crystal_description Lathe _exptl_crystal_colour Orange _exptl_crystal_size_max 0.1000 _exptl_crystal_size_mid 0.0800 _exptl_crystal_size_min 0.0800 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.652 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3088 _exptl_absorpt_coefficient_mu 1.098 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8457 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku/MSC Inc., 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 20617 _diffrn_reflns_av_R_equivalents 0.0640 _diffrn_reflns_av_sigmaI/netI 0.0658 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 25.75 _reflns_number_total 5764 _reflns_number_gt 4714 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND. Version 3.0. Crystal Impact' _computing_publication_material 'Windows Word 2003' _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^)+(0.0350P)^2^+26.0000P] 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 5764 _refine_ls_number_parameters 469 _refine_ls_number_restraints 278 _refine_ls_R_factor_all 0.0671 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1090 _refine_ls_wR_factor_gt 0.0987 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.001 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 Cd1 Cd 0.0000 0.40863(4) 0.2500 0.02124(15) Uani 1 2 d S . . Cd2 Cd 0.094497(15) 0.67684(3) 0.265455(17) 0.02198(12) Uani 1 1 d . . . O1 O 0.09957(16) 0.3926(3) 0.2438(2) 0.0416(11) Uani 1 1 d . . . O2 O 0.15601(17) 0.5336(3) 0.2768(2) 0.0438(11) Uani 1 1 d . . . O3 O 0.05068(16) 0.8352(3) 0.27186(19) 0.0384(10) Uani 1 1 d . . . F1 F 0.0000 0.5904(3) 0.2500 0.0257(9) Uani 1 2 d S . . N1 N 0.31472(19) 0.2734(4) 0.2416(2) 0.0340(11) Uani 1 1 d . . . N2 N 0.0000 1.2199(4) 0.2500 0.0262(14) Uani 1 2 d S . . N3 N 0.0249(2) 0.3967(3) 0.3542(2) 0.0335(11) Uani 1 1 d . . . N4 N 0.0781(2) 0.3256(4) 0.6623(2) 0.0386(12) Uani 1 1 d . . . N5 N 0.1357(2) 0.6979(4) 0.3691(2) 0.0336(11) Uani 1 1 d . . . C1 C 0.1497(2) 0.4404(4) 0.2582(2) 0.0251(11) Uani 1 1 d . . . C2 C 0.2073(2) 0.3825(4) 0.2526(3) 0.0300(13) Uani 1 1 d . . . C3 C 0.2035(2) 0.2899(5) 0.2213(3) 0.0406(15) Uani 1 1 d . . . H3A H 0.1645 0.2620 0.2034 0.049 Uiso 1 1 calc R . . C4 C 0.2577(2) 0.2380(4) 0.2166(3) 0.0411(16) Uani 1 1 d . . . H4A H 0.2542 0.1755 0.1949 0.049 Uiso 1 1 calc R . . C5 C 0.3180(2) 0.3638(5) 0.2706(3) 0.0434(16) Uani 1 1 d . . . H5A H 0.3575 0.3906 0.2875 0.052 Uiso 1 1 calc R . . C6 C 0.2668(2) 0.4202(5) 0.2773(3) 0.0420(16) Uani 1 1 d . . . H6A H 0.2719 0.4835 0.2983 0.050 Uiso 1 1 calc R . . C7 C 0.0000 0.8803(6) 0.2500 0.0257(16) Uani 1 2 d S . . C8 C 0.0000 0.9991(5) 0.2500 0.0262(16) Uani 1 2 d S . . C9 C 0.0537(2) 1.0555(4) 0.2741(3) 0.0356(14) Uani 1 1 d . . . H9A H 0.0906 1.0202 0.2909 0.043 Uiso 1 1 calc R . . C10 C 0.0520(3) 1.1644(4) 0.2728(3) 0.0383(15) Uani 1 1 d . . . H10A H 0.0886 1.2015 0.2885 0.046 Uiso 1 1 calc R . . C11 C 0.0812(3) 0.3654(5) 0.3851(3) 0.0412(15) Uani 1 1 d . . . H11A H 0.1133 0.3557 0.3653 0.049 Uiso 1 1 calc R . . C12 C 0.0933(3) 0.3469(5) 0.4447(3) 0.0465(16) Uani 1 1 d . . . H12A H 0.1332 0.3257 0.4645 0.056 Uiso 1 1 calc R . . C13 C 0.0466(3) 0.3597(5) 0.4752(3) 0.0378(14) Uani 1 1 d . . . C14 C -0.0108(3) 0.3904(6) 0.4433(3) 0.0546(19) Uani 1 1 d . . . H14A H -0.0438 0.3989 0.4620 0.066 Uiso 1 1 calc R . . C15 C -0.0201(3) 0.4088(5) 0.3841(3) 0.0494(17) Uani 1 1 d . . . H15A H -0.0596 0.4307 0.3637 0.059 Uiso 1 1 calc R . . C16 C 0.0585(3) 0.3430(5) 0.5398(3) 0.0427(15) Uani 1 1 d . . . C17 C 0.1151(3) 0.3674(6) 0.5765(3) 0.0488(17) Uani 1 1 d . . . H17A H 0.1479 0.3913 0.5605 0.059 Uiso 1 1 calc R . . C18 C 0.1238(3) 0.3569(5) 0.6359(3) 0.0454(16) Uani 1 1 d . . . H18A H 0.1631 0.3722 0.6593 0.055 Uiso 1 1 calc R . . C19 C 0.0237(3) 0.2996(6) 0.6269(3) 0.0490(17) Uani 1 1 d . . . H19A H -0.0081 0.2748 0.6440 0.059 Uiso 1 1 calc R . . C20 C 0.0118(3) 0.3072(6) 0.5667(3) 0.0522(18) Uani 1 1 d . . . H20A H -0.0273 0.2885 0.5440 0.063 Uiso 1 1 calc R . . C21 C 0.1660(3) 0.6205(5) 0.4019(3) 0.0512(18) Uani 1 1 d . . . H21A H 0.1569 0.5510 0.3895 0.061 Uiso 1 1 calc R . . C22 C 0.2103(3) 0.6372(5) 0.4536(3) 0.0559(19) Uani 1 1 d . . . H22A H 0.2299 0.5796 0.4750 0.067 Uiso 1 1 calc R . . C23 C 0.2255(3) 0.7389(5) 0.4733(3) 0.0425(15) Uani 1 1 d . . . C24 C 0.1925(3) 0.8180(5) 0.4394(3) 0.063(2) Uani 1 1 d . . . H24A H 0.1998 0.8883 0.4510 0.076 Uiso 1 1 calc R . . C25 C 0.1488(3) 0.7952(5) 0.3887(3) 0.059(2) Uani 1 1 d . . . H25A H 0.1275 0.8512 0.3671 0.070 Uiso 1 1 calc R . . N6A N 0.3835(6) 0.5852(13) 0.3753(6) 0.097(3) Uani 0.667(14) 1 d PDU A 1 C26A C 0.3690(7) 0.5240(14) 0.4159(7) 0.096(2) Uani 0.667(14) 1 d PDU A 1 H26A H 0.3270 0.5058 0.4119 0.115 Uiso 0.667(14) 1 calc PR A 1 C27A C 0.4119(7) 0.4846(14) 0.4648(7) 0.092(3) Uani 0.667(14) 1 d PU A 1 H27A H 0.3994 0.4365 0.4902 0.110 Uiso 0.667(14) 1 calc PR A 1 N6B N 0.3895(11) 0.640(2) 0.3892(13) 0.097(3) Uani 0.333(14) 1 d PDU A 2 C26B C 0.3760(14) 0.592(3) 0.4355(13) 0.096(2) Uani 0.333(14) 1 d PDU A 2 H26B H 0.3341 0.5927 0.4378 0.115 Uiso 0.333(14) 1 calc PR A 2 C27B C 0.4176(14) 0.541(3) 0.4813(14) 0.092(3) Uani 0.333(14) 1 d PDU A 2 H27B H 0.4053 0.5222 0.5156 0.110 Uiso 0.333(14) 1 calc PR A 2 C28 C 0.4763(4) 0.5199(7) 0.4749(4) 0.071(2) Uani 1 1 d . . . C29 C 0.4919(4) 0.5758(7) 0.4294(4) 0.083(3) Uani 1 1 d . A . H29A H 0.5337 0.5881 0.4293 0.099 Uiso 1 1 calc R . . C30 C 0.4455(6) 0.6136(9) 0.3839(4) 0.112(4) Uani 1 1 d D . . H30A H 0.4568 0.6610 0.3574 0.135 Uiso 1 1 calc R A 1 B1 B 0.2037(3) 0.1051(5) 0.3991(3) 0.104(3) Uani 1 1 d DU . . F1A F 0.1461(3) 0.0912(12) 0.4086(6) 0.132(5) Uani 0.654(16) 1 d PDU B 1 F2A F 0.2100(7) 0.2048(6) 0.3815(6) 0.147(5) Uani 0.654(16) 1 d PDU B 1 F3A F 0.2471(3) 0.0844(11) 0.4485(4) 0.109(4) Uani 0.654(16) 1 d PDU B 1 F4A F 0.2124(7) 0.0374(9) 0.3565(5) 0.151(4) Uani 0.654(16) 1 d PDU B 1 F1B F 0.1487(5) 0.0565(15) 0.3977(9) 0.093(5) Uani 0.346(16) 1 d PDU B 2 F2B F 0.1949(10) 0.1825(14) 0.3583(9) 0.126(6) Uani 0.346(16) 1 d PDU B 2 F3B F 0.2258(11) 0.148(2) 0.4526(6) 0.154(7) Uani 0.346(16) 1 d PDU B 2 F4B F 0.2450(8) 0.0341(12) 0.3875(12) 0.128(5) Uani 0.346(16) 1 d PDU B 2 O1W O 0.2512(6) 0.3856(8) 0.4276(5) 0.159(5) Uani 0.75 1 d P . . H1A H 0.2384 0.3259 0.4127 0.239 Uiso 0.75 1 d PR . . H1B H 0.2299 0.3878 0.4540 0.239 Uiso 0.75 1 d PR . . O2W O 0.3373(15) 0.875(3) 0.4127(15) 0.163(15) Uani 0.25 1 d P . . H2A H 0.3005 0.8796 0.4187 0.244 Uiso 0.25 1 d PR . . H2B H 0.3577 0.9100 0.4420 0.244 Uiso 0.25 1 d PR . . 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 Cd1 0.0178(2) 0.0183(3) 0.0277(3) 0.000 0.0053(2) 0.000 Cd2 0.01634(18) 0.02048(19) 0.0284(3) -0.00176(15) 0.00338(15) -0.00140(13) O1 0.0185(18) 0.036(2) 0.072(3) -0.010(2) 0.0137(19) -0.0004(16) O2 0.0267(19) 0.031(2) 0.073(3) -0.018(2) 0.009(2) 0.0050(16) O3 0.030(2) 0.0198(18) 0.059(3) -0.0036(18) -0.0039(19) 0.0050(15) F1 0.0165(18) 0.0173(19) 0.042(3) 0.000 0.0048(18) 0.000 N1 0.020(2) 0.031(2) 0.049(3) -0.006(2) 0.004(2) 0.0075(18) N2 0.029(3) 0.019(3) 0.026(4) 0.000 -0.004(3) 0.000 N3 0.041(3) 0.031(2) 0.026(3) -0.001(2) 0.003(2) -0.001(2) N4 0.031(2) 0.061(3) 0.025(3) 0.005(2) 0.008(2) 0.005(2) N5 0.033(2) 0.036(3) 0.028(3) -0.003(2) -0.001(2) 0.000(2) C1 0.018(2) 0.029(3) 0.027(3) 0.003(2) 0.002(2) 0.005(2) C2 0.024(2) 0.024(3) 0.043(4) 0.001(2) 0.007(2) 0.001(2) C3 0.021(3) 0.042(3) 0.056(4) -0.013(3) 0.003(3) -0.001(2) C4 0.027(3) 0.033(3) 0.063(5) -0.021(3) 0.009(3) 0.003(2) C5 0.019(3) 0.047(4) 0.063(5) -0.012(3) 0.005(3) 0.000(2) C6 0.027(3) 0.035(3) 0.063(5) -0.015(3) 0.006(3) 0.001(2) C7 0.027(4) 0.027(4) 0.023(5) 0.000 0.005(3) 0.000 C8 0.026(4) 0.023(4) 0.028(5) 0.000 0.002(3) 0.000 C9 0.021(3) 0.024(3) 0.056(4) 0.002(3) -0.003(3) -0.002(2) C10 0.032(3) 0.024(3) 0.052(4) -0.002(3) -0.004(3) -0.006(2) C11 0.037(3) 0.056(4) 0.032(4) 0.001(3) 0.010(3) -0.003(3) C12 0.037(3) 0.072(5) 0.029(4) 0.005(3) 0.003(3) 0.002(3) C13 0.039(3) 0.049(4) 0.024(4) 0.000(3) 0.006(3) 0.000(3) C14 0.045(4) 0.089(5) 0.030(4) 0.002(4) 0.010(3) 0.010(4) C15 0.044(4) 0.074(5) 0.030(4) 0.004(3) 0.006(3) 0.013(3) C16 0.037(3) 0.058(4) 0.033(4) 0.000(3) 0.008(3) 0.005(3) C17 0.039(3) 0.080(5) 0.030(4) 0.008(3) 0.012(3) 0.002(3) C18 0.030(3) 0.073(5) 0.032(4) 0.007(3) 0.004(3) 0.003(3) C19 0.034(3) 0.083(5) 0.033(4) 0.003(3) 0.013(3) -0.009(3) C20 0.033(3) 0.093(6) 0.027(4) 0.001(3) 0.000(3) -0.007(3) C21 0.062(4) 0.034(3) 0.046(5) 0.006(3) -0.012(3) -0.013(3) C22 0.073(5) 0.037(3) 0.044(5) 0.008(3) -0.016(4) -0.007(3) C23 0.049(4) 0.044(4) 0.028(4) 0.000(3) -0.005(3) 0.000(3) C24 0.077(5) 0.035(4) 0.055(5) -0.007(3) -0.033(4) 0.012(3) C25 0.072(5) 0.043(4) 0.045(5) -0.008(3) -0.022(4) 0.010(3) N6A 0.091(4) 0.103(5) 0.092(4) 0.004(4) 0.009(4) 0.010(4) C26A 0.087(4) 0.105(4) 0.094(4) 0.006(4) 0.014(3) 0.004(4) C27A 0.083(4) 0.101(5) 0.091(4) 0.011(4) 0.017(4) 0.003(4) N6B 0.091(4) 0.103(5) 0.092(4) 0.004(4) 0.009(4) 0.010(4) C26B 0.087(4) 0.105(4) 0.094(4) 0.006(4) 0.014(3) 0.004(4) C27B 0.083(4) 0.101(5) 0.091(4) 0.011(4) 0.017(4) 0.003(4) C28 0.065(5) 0.086(6) 0.063(6) 0.015(5) 0.018(4) 0.009(4) C29 0.075(6) 0.104(7) 0.069(7) 0.022(5) 0.017(5) 0.000(5) C30 0.145(10) 0.120(9) 0.067(8) 0.038(6) 0.013(7) 0.016(8) B1 0.079(6) 0.114(7) 0.110(7) -0.002(6) 0.003(6) -0.011(6) F1A 0.074(6) 0.173(10) 0.151(9) -0.003(8) 0.030(6) -0.006(6) F2A 0.168(10) 0.101(7) 0.154(10) 0.022(7) 0.000(8) -0.039(7) F3A 0.053(4) 0.156(9) 0.102(6) 0.027(6) -0.013(4) 0.000(5) F4A 0.152(10) 0.168(9) 0.126(9) -0.038(7) 0.016(8) 0.017(8) F1B 0.047(8) 0.118(11) 0.107(10) -0.007(9) -0.002(8) -0.010(8) F2B 0.130(11) 0.106(11) 0.121(13) 0.038(10) -0.017(10) -0.038(10) F3B 0.141(12) 0.176(14) 0.119(11) -0.017(11) -0.031(11) 0.002(12) F4B 0.079(9) 0.152(10) 0.148(12) -0.002(10) 0.014(9) 0.008(9) O1W 0.216(13) 0.098(8) 0.184(12) -0.012(8) 0.085(10) -0.024(8) O2W 0.11(2) 0.24(4) 0.12(3) -0.05(3) 0.00(2) -0.02(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1 2.226(3) 2 ? Cd1 O1 2.226(3) . ? Cd1 F1 2.292(4) . ? Cd1 N3 2.368(5) 2 ? Cd1 N3 2.368(5) . ? Cd1 N2 2.380(6) 1_545 ? Cd2 O2 2.233(4) . ? Cd2 O3 2.234(3) . ? Cd2 F1 2.2945(19) . ? Cd2 N4 2.345(5) 6_565 ? Cd2 N1 2.367(4) 4 ? Cd2 N5 2.394(5) . ? O1 C1 1.232(6) . ? O2 C1 1.249(6) . ? O3 C7 1.250(5) . ? F1 Cd2 2.2945(19) 2 ? N1 C5 1.319(7) . ? N1 C4 1.331(7) . ? N1 Cd2 2.367(4) 4_545 ? N2 C10 1.340(6) . ? N2 C10 1.340(6) 2 ? N2 Cd1 2.380(6) 1_565 ? N3 C15 1.336(7) . ? N3 C11 1.339(7) . ? N4 C19 1.329(7) . ? N4 C18 1.345(7) . ? N4 Cd2 2.345(5) 6_566 ? N5 C25 1.317(8) . ? N5 C21 1.322(7) . ? C1 C2 1.488(7) . ? C2 C3 1.368(8) . ? C2 C6 1.385(7) . ? C3 C4 1.382(7) . ? C3 H3A 0.9300 . ? C4 H4A 0.9300 . ? C5 C6 1.366(7) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 O3 1.250(5) 2 ? C7 C8 1.498(10) . ? C8 C9 1.381(6) . ? C8 C9 1.381(6) 2 ? C9 C10 1.374(7) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.372(8) . ? C11 H11A 0.9300 . ? C12 C13 1.378(8) . ? C12 H12A 0.9300 . ? C13 C14 1.365(8) . ? C13 C16 1.483(9) . ? C14 C15 1.367(9) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 C17 1.373(8) . ? C16 C20 1.388(9) . ? C17 C18 1.359(9) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 C20 1.368(9) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C22 1.382(8) . ? C21 H21A 0.9300 . ? C22 C23 1.378(9) . ? C22 H22A 0.9300 . ? C23 C24 1.372(8) . ? C23 C23 1.478(11) 7_566 ? C24 C25 1.372(9) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? N6A C26A 1.314(14) . ? N6A C30 1.374(17) . ? C26A C27A 1.394(18) . ? C26A H26A 0.9300 . ? C27A C28 1.448(18) . ? C27A H27A 0.9300 . ? N6B C30 1.302(17) . ? N6B C26B 1.326(18) . ? C26B C27B 1.395(18) . ? C26B H26B 0.9300 . ? C27B C28 1.35(3) . ? C27B H27B 0.9300 . ? C28 C29 1.377(11) . ? C28 C28 1.465(15) 5_666 ? C29 C30 1.378(12) . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? B1 F1A 1.339(7) . ? B1 F2A 1.340(7) . ? B1 F4B 1.343(7) . ? B1 F3A 1.344(6) . ? B1 F3B 1.344(7) . ? B1 F1B 1.345(7) . ? B1 F2B 1.345(7) . ? B1 F4A 1.354(7) . ? O1W H1A 0.8500 . ? O1W H1B 0.8500 . ? O2W H2A 0.8501 . ? O2W H2B 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cd1 O1 169.6(2) 2 . ? O1 Cd1 F1 95.22(10) 2 . ? O1 Cd1 F1 95.22(10) . . ? O1 Cd1 N3 93.16(16) 2 2 ? O1 Cd1 N3 86.18(16) . 2 ? F1 Cd1 N3 93.65(11) . 2 ? O1 Cd1 N3 86.18(16) 2 . ? O1 Cd1 N3 93.16(16) . . ? F1 Cd1 N3 93.65(11) . . ? N3 Cd1 N3 172.7(2) 2 . ? O1 Cd1 N2 84.78(10) 2 1_545 ? O1 Cd1 N2 84.78(10) . 1_545 ? F1 Cd1 N2 180.000(1) . 1_545 ? N3 Cd1 N2 86.35(11) 2 1_545 ? N3 Cd1 N2 86.35(11) . 1_545 ? O2 Cd2 O3 166.26(14) . . ? O2 Cd2 F1 97.66(13) . . ? O3 Cd2 F1 92.83(12) . . ? O2 Cd2 N4 93.51(17) . 6_565 ? O3 Cd2 N4 96.30(17) . 6_565 ? F1 Cd2 N4 84.64(11) . 6_565 ? O2 Cd2 N1 86.01(15) . 4 ? O3 Cd2 N1 85.69(15) . 4 ? F1 Cd2 N1 167.14(12) . 4 ? N4 Cd2 N1 82.83(16) 6_565 4 ? O2 Cd2 N5 83.62(16) . . ? O3 Cd2 N5 84.52(15) . . ? F1 Cd2 N5 109.55(11) . . ? N4 Cd2 N5 165.75(16) 6_565 . ? N1 Cd2 N5 83.05(16) 4 . ? C1 O1 Cd1 139.9(4) . . ? C1 O2 Cd2 134.7(3) . . ? C7 O3 Cd2 137.3(4) . . ? Cd1 F1 Cd2 118.36(8) . . ? Cd1 F1 Cd2 118.36(8) . 2 ? Cd2 F1 Cd2 123.28(16) . 2 ? C5 N1 C4 116.9(4) . . ? C5 N1 Cd2 121.9(3) . 4_545 ? C4 N1 Cd2 121.2(4) . 4_545 ? C10 N2 C10 117.1(6) . 2 ? C10 N2 Cd1 121.5(3) . 1_565 ? C10 N2 Cd1 121.5(3) 2 1_565 ? C15 N3 C11 116.9(5) . . ? C15 N3 Cd1 119.8(4) . . ? C11 N3 Cd1 122.8(4) . . ? C19 N4 C18 116.3(5) . . ? C19 N4 Cd2 122.9(4) . 6_566 ? C18 N4 Cd2 120.8(4) . 6_566 ? C25 N5 C21 116.5(5) . . ? C25 N5 Cd2 117.1(4) . . ? C21 N5 Cd2 121.8(4) . . ? O1 C1 O2 125.2(5) . . ? O1 C1 C2 117.2(5) . . ? O2 C1 C2 117.5(4) . . ? C3 C2 C6 117.0(5) . . ? C3 C2 C1 120.8(5) . . ? C6 C2 C1 122.1(5) . . ? C2 C3 C4 119.6(5) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? N1 C4 C3 123.1(5) . . ? N1 C4 H4A 118.5 . . ? C3 C4 H4A 118.5 . . ? N1 C5 C6 123.8(5) . . ? N1 C5 H5A 118.1 . . ? C6 C5 H5A 118.1 . . ? C5 C6 C2 119.6(5) . . ? C5 C6 H6A 120.2 . . ? C2 C6 H6A 120.2 . . ? O3 C7 O3 125.8(7) . 2 ? O3 C7 C8 117.1(3) . . ? O3 C7 C8 117.1(3) 2 . ? C9 C8 C9 118.0(7) . 2 ? C9 C8 C7 121.0(3) . . ? C9 C8 C7 121.0(3) 2 . ? C10 C9 C8 119.2(5) . . ? C10 C9 H9A 120.4 . . ? C8 C9 H9A 120.4 . . ? N2 C10 C9 123.2(5) . . ? N2 C10 H10A 118.4 . . ? C9 C10 H10A 118.4 . . ? N3 C11 C12 122.6(6) . . ? N3 C11 H11A 118.7 . . ? C12 C11 H11A 118.7 . . ? C11 C12 C13 120.1(6) . . ? C11 C12 H12A 119.9 . . ? C13 C12 H12A 119.9 . . ? C14 C13 C12 116.9(6) . . ? C14 C13 C16 121.5(6) . . ? C12 C13 C16 121.5(5) . . ? C13 C14 C15 120.5(6) . . ? C13 C14 H14A 119.7 . . ? C15 C14 H14A 119.7 . . ? N3 C15 C14 122.9(6) . . ? N3 C15 H15A 118.6 . . ? C14 C15 H15A 118.6 . . ? C17 C16 C20 116.5(6) . . ? C17 C16 C13 121.9(6) . . ? C20 C16 C13 121.5(6) . . ? C18 C17 C16 120.8(6) . . ? C18 C17 H17A 119.6 . . ? C16 C17 H17A 119.6 . . ? N4 C18 C17 122.9(6) . . ? N4 C18 H18A 118.5 . . ? C17 C18 H18A 118.5 . . ? N4 C19 C20 123.9(6) . . ? N4 C19 H19A 118.0 . . ? C20 C19 H19A 118.0 . . ? C19 C20 C16 119.5(6) . . ? C19 C20 H20A 120.3 . . ? C16 C20 H20A 120.3 . . ? N5 C21 C22 123.6(6) . . ? N5 C21 H21A 118.2 . . ? C22 C21 H21A 118.2 . . ? C23 C22 C21 120.0(6) . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C24 C23 C22 115.4(6) . . ? C24 C23 C23 122.5(7) . 7_566 ? C22 C23 C23 122.1(7) . 7_566 ? C23 C24 C25 121.2(6) . . ? C23 C24 H24A 119.4 . . ? C25 C24 H24A 119.4 . . ? N5 C25 C24 123.3(6) . . ? N5 C25 H25A 118.4 . . ? C24 C25 H25A 118.4 . . ? C26A N6A C30 116.1(13) . . ? N6A C26A C27A 124.6(15) . . ? N6A C26A H26A 117.7 . . ? C27A C26A H26A 117.7 . . ? C26A C27A C28 118.6(14) . . ? C26A C27A H27A 120.7 . . ? C28 C27A H27A 120.7 . . ? C30 N6B C26B 110(2) . . ? N6B C26B C27B 127(3) . . ? N6B C26B H26B 116.5 . . ? C27B C26B H26B 116.5 . . ? C28 C27B C26B 119(3) . . ? C28 C27B H27B 120.5 . . ? C26B C27B H27B 120.5 . . ? C27B C28 C29 112.7(15) . . ? C27B C28 C27A 33.3(14) . . ? C29 C28 C27A 115.5(9) . . ? C27B C28 C28 120.1(15) . 5_666 ? C29 C28 C28 122.4(10) . 5_666 ? C27A C28 C28 121.0(11) . 5_666 ? C30 C29 C28 120.1(9) . . ? C30 C29 H29A 119.9 . . ? C28 C29 H29A 119.9 . . ? N6B C30 N6A 32.9(13) . . ? N6B C30 C29 124.3(16) . . ? N6A C30 C29 123.8(11) . . ? N6B C30 H30A 107.1 . . ? N6A C30 H30A 118.1 . . ? C29 C30 H30A 118.1 . . ? F1A B1 F2A 109.8(6) . . ? F1A B1 F4B 130.4(11) . . ? F2A B1 F4B 116.3(13) . . ? F1A B1 F3A 110.2(6) . . ? F2A B1 F3A 110.0(6) . . ? F4B B1 F3A 70.3(9) . . ? F1A B1 F3B 93.3(11) . . ? F2A B1 F3B 82.3(10) . . ? F4B B1 F3B 109.5(6) . . ? F3A B1 F3B 41.0(9) . . ? F1A B1 F1B 22.1(11) . . ? F2A B1 F1B 125.0(12) . . ? F4B B1 F1B 109.4(6) . . ? F3A B1 F1B 113.0(11) . . ? F3B B1 F1B 109.9(6) . . ? F1A B1 F2B 102.7(13) . . ? F2A B1 F2B 27.2(10) . . ? F4B B1 F2B 109.7(6) . . ? F3A B1 F2B 134.9(10) . . ? F3B B1 F2B 109.1(6) . . ? F1B B1 F2B 109.2(6) . . ? F1A B1 F4A 109.3(6) . . ? F2A B1 F4A 109.1(6) . . ? F4B B1 F4A 38.8(8) . . ? F3A B1 F4A 108.4(6) . . ? F3B B1 F4A 148.3(9) . . ? F1B B1 F4A 88.1(10) . . ? F2B B1 F4A 87.8(11) . . ? H1A O1W H1B 98.0 . . ? H2A O2W H2B 100.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1A F2A 0.85 1.74 2.594(15) 178.3 . O1W H1A F2B 0.85 2.29 3.13(3) 169.7 . O1W H1B F3B 0.85 2.22 2.753(19) 120.8 7_556 O1W H1B F3A 0.85 2.24 2.900(16) 134.6 7_556 _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 25.75 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.974 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.113