# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_requested_category FM _publ_contact_author_name 'Paul V. Bernhardt' _publ_contact_author_email p.bernhardt@uq.edu.au loop_ _publ_author_name L.Daumann K.Dalle G.Schenk R.McGeary P.Bernhardt D.Ollis L.Gahan data_334kd1 _database_code_depnum_ccdc_archive 'CCDC 830841' #TrackingRef 'supdata.cif' _audit_creation_date 2011-06-17T13:07:59-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C31 H41 N4 O7 Zn2, P F6' _chemical_formula_sum 'C31 H41 F6 N4 O7 P Zn2' _chemical_formula_weight 857.39 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.7745(5) _cell_length_b 14.8184(8) _cell_length_c 23.1270(10) _cell_angle_alpha 90 _cell_angle_beta 102.967(5) _cell_angle_gamma 90 _cell_volume 3598.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3977 _cell_measurement_theta_min 2.9302 _cell_measurement_theta_max 29.1267 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.459 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.89316 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 16.0696 _diffrn_orient_matrix_ub_11 0.0160769011 _diffrn_orient_matrix_ub_12 -0.0125257037 _diffrn_orient_matrix_ub_13 0.0303569723 _diffrn_orient_matrix_ub_21 0.0027876908 _diffrn_orient_matrix_ub_22 0.0463009461 _diffrn_orient_matrix_ub_23 0.0082506942 _diffrn_orient_matrix_ub_31 -0.0655696458 _diffrn_orient_matrix_ub_32 -0.001103936 _diffrn_orient_matrix_ub_33 0.0005099801 _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0456 _diffrn_reflns_av_unetI/netI 0.117 _diffrn_reflns_number 15336 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 6333 _reflns_number_gt 3255 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0317P)^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_number_reflns 6333 _refine_ls_number_parameters 485 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0913 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.0791 _refine_ls_wR_factor_gt 0.0735 _refine_ls_goodness_of_fit_ref 0.79 _refine_ls_restrained_S_all 0.8 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.531 _refine_diff_density_min -0.389 _refine_diff_density_rms 0.06 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7111(4) 0.2198(3) 0.69727(19) 0.0428(12) Uani 1 1 d . . . C2 C 0.6728(4) 0.2874(3) 0.73000(18) 0.0415(12) Uani 1 1 d . . . H2 H 0.7286 0.3066 0.7645 0.05 Uiso 1 1 calc R . . C3 C 0.5536(3) 0.3283(3) 0.71360(17) 0.0331(10) Uani 1 1 d . . . C4 C 0.4684(3) 0.2982(3) 0.66226(17) 0.0315(10) Uani 1 1 d . . . C5 C 0.5043(4) 0.2295(3) 0.62844(17) 0.0334(10) Uani 1 1 d . . . C6 C 0.6253(4) 0.1920(3) 0.64629(18) 0.0430(12) Uani 1 1 d . . . H6 H 0.6494 0.1467 0.6232 0.052 Uiso 1 1 calc R . . C7 C 0.8404(4) 0.1746(3) 0.7168(2) 0.0583(14) Uani 1 1 d . . . H7A H 0.9054 0.2201 0.7253 0.088 Uiso 1 1 d R . . H7B H 0.8557 0.1359 0.6858 0.088 Uiso 1 1 d R . . H7C H 0.842 0.1396 0.7518 0.088 Uiso 1 1 d R . . C8 C 0.5153(3) 0.4011(3) 0.75085(17) 0.0396(12) Uani 1 1 d . . . H8A H 0.5863 0.414 0.7838 0.047 Uiso 1 1 calc R . . H8B H 0.4969 0.4556 0.7272 0.047 Uiso 1 1 calc R . . C9 C 0.2383(4) 0.4419(3) 0.81995(18) 0.0389(11) Uani 1 1 d . . . C10 C 0.2040(4) 0.4637(3) 0.87178(18) 0.0474(13) Uani 1 1 d . . . H10 H 0.2652 0.484 0.9041 0.057 Uiso 1 1 calc R . . C11 C 0.0795(5) 0.4554(3) 0.8761(2) 0.0571(14) Uani 1 1 d . . . H11 H 0.0554 0.4699 0.9112 0.068 Uiso 1 1 calc R . . C12 C -0.0083(4) 0.4255(3) 0.8277(2) 0.0570(14) Uani 1 1 d . . . H12 H -0.0938 0.421 0.829 0.068 Uiso 1 1 calc R . . C13 C 0.0312(4) 0.4021(3) 0.77736(19) 0.0472(13) Uani 1 1 d . . . H13 H -0.0287 0.3795 0.7452 0.057 Uiso 1 1 calc R . . C14 C 0.3703(4) 0.4528(3) 0.81012(17) 0.0417(12) Uani 1 1 d . . . H14A H 0.3761 0.5094 0.7898 0.05 Uiso 1 1 calc R . . H14B H 0.4308 0.4548 0.8481 0.05 Uiso 1 1 calc R . . C15 C 0.4228(4) 0.2944(3) 0.81170(18) 0.0471(12) Uani 1 1 d . . . H15A H 0.374 0.2995 0.842 0.057 Uiso 1 1 calc R . . H15B H 0.5121 0.2909 0.8316 0.057 Uiso 1 1 calc R . . C16 C 0.3858(4) 0.2074(3) 0.77774(19) 0.0514(13) Uani 1 1 d . . . H16A H 0.4451 0.1944 0.7529 0.062 Uiso 1 1 calc R . . H16B H 0.3877 0.1576 0.8051 0.062 Uiso 1 1 calc R . . C17 C 0.1407(4) 0.4600(3) 0.4419(2) 0.0476(13) Uani 1 1 d . . . H17 H 0.1328 0.512 0.4633 0.057 Uiso 1 1 calc R . . C18 C 0.0895(4) 0.4591(4) 0.3816(2) 0.0604(15) Uani 1 1 d . . . H18 H 0.0472 0.5092 0.3624 0.073 Uiso 1 1 calc R . . C19 C 0.1031(4) 0.3816(4) 0.3507(2) 0.0626(15) Uani 1 1 d . . . H19 H 0.0719 0.3794 0.3099 0.075 Uiso 1 1 calc R . . C20 C 0.1632(4) 0.3069(3) 0.38060(19) 0.0502(13) Uani 1 1 d . . . H20 H 0.1703 0.2537 0.3603 0.06 Uiso 1 1 calc R . . C21 C 0.2118(4) 0.3127(3) 0.44028(19) 0.0408(12) Uani 1 1 d . . . C22 C 0.2758(4) 0.2354(3) 0.47731(17) 0.0479(13) Uani 1 1 d . . . H22A H 0.2131 0.2014 0.4925 0.057 Uiso 1 1 calc R . . H22B H 0.3136 0.1953 0.4529 0.057 Uiso 1 1 calc R . . C23 C 0.4851(4) 0.3012(3) 0.50361(18) 0.0461(12) Uani 1 1 d . . . H23A H 0.4533 0.3253 0.4641 0.055 Uiso 1 1 calc R . . H23B H 0.5398 0.2503 0.5003 0.055 Uiso 1 1 calc R . . C24 C 0.5634(4) 0.3728(3) 0.54143(19) 0.0510(12) Uani 1 1 d . . . H24A H 0.615 0.3457 0.577 0.061 Uiso 1 1 calc R . . H24B H 0.6198 0.4015 0.5197 0.061 Uiso 1 1 calc R . . C25 C 0.4129(4) 0.1973(3) 0.57306(17) 0.0420(11) Uani 1 1 d . . . H25A H 0.452 0.1478 0.5562 0.05 Uiso 1 1 calc R . . H25B H 0.3369 0.1742 0.5838 0.05 Uiso 1 1 calc R . . C26 C -0.0923(4) 0.2706(4) 0.57600(19) 0.086(2) Uani 1 1 d . . . H26A H -0.1371 0.2704 0.6075 0.129 Uiso 1 1 calc R . . H26B H -0.0873 0.2101 0.5618 0.129 Uiso 1 1 calc R . . H26C H -0.1368 0.308 0.5442 0.129 Uiso 1 1 calc R . . C27 C 0.0390(4) 0.3067(3) 0.5986(2) 0.0424(12) Uani 1 1 d . . . C28 C 0.2338(4) 0.5439(3) 0.6277(2) 0.0382(11) Uani 1 1 d . . . C29 C 0.2292(5) 0.6449(3) 0.6243(2) 0.0692(15) Uani 1 1 d . . . H29A H 0.2269 0.6637 0.5844 0.104 Uiso 1 1 calc R . . H29B H 0.3035 0.6695 0.6504 0.104 Uiso 1 1 calc R . . H29C H 0.1543 0.6662 0.636 0.104 Uiso 1 1 calc R . . C30 C 0.5442(4) 0.5022(3) 0.5989(2) 0.0635(15) Uani 1 1 d . . . H30A H 0.484 0.5445 0.608 0.095 Uiso 1 1 calc R . . H30B H 0.6059 0.5338 0.5823 0.095 Uiso 1 1 calc R . . H30C H 0.5866 0.4717 0.6344 0.095 Uiso 1 1 calc R . . C31 C 0.2223(5) 0.1411(3) 0.7059(2) 0.0768(17) Uani 1 1 d . . . H31A H 0.1378 0.1505 0.6824 0.115 Uiso 1 1 calc R . . H31B H 0.223 0.089 0.7307 0.115 Uiso 1 1 calc R . . H31C H 0.2799 0.1319 0.6803 0.115 Uiso 1 1 calc R . . N1 N 0.4025(3) 0.3776(2) 0.77453(13) 0.0335(8) Uani 1 1 d . . . N2 N 0.1521(3) 0.4102(2) 0.77243(14) 0.0376(9) Uani 1 1 d . . . N3 N 0.3752(3) 0.2686(2) 0.52714(13) 0.0355(9) Uani 1 1 d . . . N4 N 0.2013(3) 0.3888(3) 0.47049(14) 0.0399(9) Uani 1 1 d . . . O1 O 0.3526(2) 0.33626(18) 0.64648(10) 0.0363(7) Uani 1 1 d . . . O2 O 0.1092(3) 0.3111(2) 0.56312(13) 0.0575(9) Uani 1 1 d . . . O3 O 0.0689(2) 0.3298(2) 0.65250(12) 0.0484(8) Uani 1 1 d . . . O4 O 0.2610(3) 0.2183(2) 0.74220(12) 0.0504(8) Uani 1 1 d . . . O5 O 0.4792(2) 0.4378(2) 0.55694(12) 0.0495(8) Uani 1 1 d . . . O6 O 0.2349(2) 0.50383(19) 0.57945(12) 0.0473(8) Uani 1 1 d . . . O7 O 0.2368(2) 0.50694(19) 0.67603(13) 0.0447(8) Uani 1 1 d . . . P1 P 0.27581(14) 0.92859(11) 0.55124(6) 0.0678(5) Uani 1 1 d . . . F1 F 0.4174(5) 0.9526(6) 0.5522(3) 0.201(4) Uani 0.777(7) 1 d PD A 1 F2 F 0.3320(6) 0.8374(3) 0.5757(3) 0.160(3) Uani 0.777(7) 1 d PD A 1 F3 F 0.1417(6) 0.8950(6) 0.5456(4) 0.174(5) Uani 0.777(7) 1 d PD A 1 F4 F 0.2122(8) 1.0160(4) 0.5240(2) 0.185(4) Uani 0.777(7) 1 d PD A 1 F5 F 0.2983(5) 0.9703(4) 0.61275(17) 0.139(3) Uani 0.777(7) 1 d PD A 1 F6 F 0.2730(4) 0.8897(3) 0.48600(18) 0.1034(19) Uani 0.777(7) 1 d PD A 1 F1' F 0.1290(12) 0.9045(13) 0.5332(8) 0.20(2) Uiso 0.223(7) 1 d PD A 2 F2' F 0.2632(12) 0.8698(10) 0.6104(6) 0.084(6) Uiso 0.223(7) 1 d PD A 2 F3' F 0.4054(11) 0.9575(10) 0.5845(7) 0.097(7) Uiso 0.223(7) 1 d PD A 2 F4' F 0.2899(11) 1.0046(8) 0.5129(5) 0.053(5) Uiso 0.223(7) 1 d PD A 2 F5' F 0.2066(13) 1.0094(9) 0.5907(6) 0.105(7) Uiso 0.223(7) 1 d PD A 2 F6' F 0.3038(18) 0.8532(9) 0.5231(8) 0.159(11) Uiso 0.223(7) 1 d PD A 2 Zn1 Zn 0.27680(4) 0.37639(4) 0.563185(19) 0.03442(14) Uani 1 1 d . . . Zn2 Zn 0.23624(4) 0.37204(4) 0.700213(18) 0.03443(15) 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 C1 0.037(3) 0.046(3) 0.047(3) 0.015(2) 0.012(2) 0.001(2) C2 0.036(3) 0.049(3) 0.038(3) 0.003(2) 0.005(2) -0.001(2) C3 0.028(2) 0.038(3) 0.033(3) 0.005(2) 0.008(2) -0.009(2) C4 0.029(2) 0.036(3) 0.031(3) 0.007(2) 0.011(2) 0.003(2) C5 0.037(2) 0.028(3) 0.036(3) 0.004(2) 0.010(2) 0.005(2) C6 0.055(3) 0.032(3) 0.046(3) 0.008(2) 0.022(2) 0.011(2) C7 0.048(3) 0.055(4) 0.072(3) 0.018(3) 0.015(2) 0.012(3) C8 0.036(2) 0.047(4) 0.033(3) -0.002(2) 0.003(2) -0.004(2) C9 0.047(3) 0.038(3) 0.033(3) -0.003(2) 0.012(2) 0.003(2) C10 0.070(3) 0.043(3) 0.031(3) -0.011(2) 0.015(2) -0.004(3) C11 0.075(3) 0.063(4) 0.043(3) -0.009(3) 0.033(3) 0.000(3) C12 0.049(3) 0.069(4) 0.060(3) -0.003(3) 0.026(3) 0.002(3) C13 0.044(3) 0.056(4) 0.044(3) -0.004(2) 0.014(2) -0.005(2) C14 0.046(3) 0.048(3) 0.029(3) -0.010(2) 0.004(2) -0.004(2) C15 0.050(3) 0.058(4) 0.033(3) 0.006(3) 0.008(2) 0.005(3) C16 0.065(3) 0.042(3) 0.049(3) 0.009(3) 0.017(3) 0.005(3) C17 0.047(3) 0.050(4) 0.047(3) -0.001(3) 0.011(2) 0.002(2) C18 0.049(3) 0.084(5) 0.046(3) 0.009(3) 0.005(3) 0.011(3) C19 0.049(3) 0.100(5) 0.033(3) -0.008(3) -0.003(2) 0.006(3) C20 0.052(3) 0.064(4) 0.033(3) -0.017(3) 0.005(2) 0.001(3) C21 0.039(3) 0.048(3) 0.036(3) -0.002(3) 0.011(2) 0.004(2) C22 0.065(3) 0.042(3) 0.033(3) -0.019(2) 0.004(2) 0.000(3) C23 0.047(3) 0.047(3) 0.047(3) -0.001(3) 0.018(2) 0.015(2) C24 0.045(3) 0.060(3) 0.055(3) 0.015(3) 0.026(2) 0.008(3) C25 0.050(3) 0.029(3) 0.047(3) -0.002(2) 0.011(2) 0.005(2) C26 0.057(3) 0.153(6) 0.045(3) -0.014(3) 0.004(2) -0.049(4) C27 0.035(3) 0.045(3) 0.048(3) 0.001(3) 0.010(2) -0.011(2) C28 0.035(3) 0.036(3) 0.046(3) -0.002(3) 0.014(2) -0.003(2) C29 0.119(4) 0.027(3) 0.070(4) -0.001(3) 0.038(3) 0.002(3) C30 0.065(3) 0.053(4) 0.074(4) -0.012(3) 0.019(3) -0.025(3) C31 0.102(4) 0.054(4) 0.076(4) -0.013(3) 0.022(3) -0.022(3) N1 0.0377(19) 0.036(2) 0.0270(18) -0.0043(19) 0.0073(15) 0.0023(19) N2 0.041(2) 0.043(3) 0.030(2) -0.0047(17) 0.0105(17) -0.0005(17) N3 0.044(2) 0.032(2) 0.030(2) -0.0021(17) 0.0086(16) 0.0083(18) N4 0.045(2) 0.041(3) 0.034(2) 0.006(2) 0.0105(17) 0.005(2) O1 0.0358(15) 0.046(2) 0.0284(16) -0.0006(13) 0.0089(12) 0.0048(14) O2 0.0515(19) 0.083(3) 0.0396(19) -0.0132(18) 0.0143(15) -0.0238(18) O3 0.0400(17) 0.070(2) 0.0345(18) -0.0100(17) 0.0072(14) -0.0100(16) O4 0.062(2) 0.034(2) 0.053(2) -0.0033(16) 0.0083(16) -0.0080(16) O5 0.0473(17) 0.049(2) 0.056(2) -0.0042(17) 0.0201(15) -0.0049(17) O6 0.069(2) 0.038(2) 0.0349(19) 0.0010(15) 0.0114(15) 0.0122(16) O7 0.0640(19) 0.035(2) 0.0366(18) -0.0016(16) 0.0147(15) 0.0019(16) P1 0.0815(11) 0.0575(11) 0.0545(10) 0.0018(9) -0.0058(8) -0.0031(9) F1 0.125(5) 0.371(11) 0.117(5) -0.100(6) 0.048(4) -0.131(6) F2 0.260(7) 0.099(4) 0.116(5) 0.044(3) 0.033(5) 0.070(4) F3 0.098(5) 0.238(11) 0.202(8) -0.082(6) 0.067(4) -0.055(4) F4 0.229(8) 0.123(6) 0.155(6) -0.001(4) -0.056(5) 0.096(5) F5 0.174(5) 0.179(6) 0.045(3) -0.046(3) -0.018(3) 0.072(4) F6 0.135(4) 0.117(4) 0.051(3) -0.019(3) 0.004(2) -0.035(3) Zn1 0.0411(3) 0.0352(3) 0.0275(3) -0.0025(3) 0.0087(2) 0.0012(3) Zn2 0.0362(3) 0.0398(3) 0.0272(3) -0.0037(3) 0.0069(2) -0.0006(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.374(6) . ? C1 C6 1.388(5) . ? C1 C7 1.520(5) . ? C2 C3 1.394(5) . ? C2 H2 0.93 . ? C3 C4 1.401(5) . ? C3 C8 1.495(5) . ? C4 O1 1.343(4) . ? C4 C5 1.390(5) . ? C5 C6 1.392(5) . ? C5 C25 1.507(5) . ? C6 H6 0.93 . ? C7 H7A 0.96 . ? C7 H7B 0.96 . ? C7 H7C 0.96 . ? C8 N1 1.482(5) . ? C8 H8A 0.97 . ? C8 H8B 0.97 . ? C9 N2 1.354(4) . ? C9 C10 1.370(5) . ? C9 C14 1.498(5) . ? C10 C11 1.373(5) . ? C10 H10 0.93 . ? C11 C12 1.367(5) . ? C11 H11 0.93 . ? C12 C13 1.372(6) . ? C12 H12 0.93 . ? C13 N2 1.338(5) . ? C13 H13 0.93 . ? C14 N1 1.473(5) . ? C14 H14A 0.97 . ? C14 H14B 0.97 . ? C15 N1 1.491(5) . ? C15 C16 1.516(6) . ? C15 H15A 0.97 . ? C15 H15B 0.97 . ? C16 O4 1.419(4) . ? C16 H16A 0.97 . ? C16 H16B 0.97 . ? C17 N4 1.335(5) . ? C17 C18 1.380(5) . ? C17 H17 0.93 . ? C18 C19 1.377(6) . ? C18 H18 0.93 . ? C19 C20 1.386(6) . ? C19 H19 0.93 . ? C20 C21 1.365(5) . ? C20 H20 0.93 . ? C21 N4 1.345(5) . ? C21 C22 1.502(5) . ? C22 N3 1.471(4) . ? C22 H22A 0.97 . ? C22 H22B 0.97 . ? C23 N3 1.491(5) . ? C23 C24 1.506(5) . ? C23 H23A 0.97 . ? C23 H23B 0.97 . ? C24 O5 1.424(5) . ? C24 H24A 0.97 . ? C24 H24B 0.97 . ? C25 N3 1.488(5) . ? C25 H25A 0.97 . ? C25 H25B 0.97 . ? C26 C27 1.493(5) . ? C26 H26A 0.96 . ? C26 H26B 0.96 . ? C26 H26C 0.96 . ? C27 O2 1.236(5) . ? C27 O3 1.263(5) . ? C28 O7 1.238(5) . ? C28 O6 1.267(5) . ? C28 C29 1.499(6) . ? C29 H29A 0.96 . ? C29 H29B 0.96 . ? C29 H29C 0.96 . ? C30 O5 1.427(5) . ? C30 H30A 0.96 . ? C30 H30B 0.96 . ? C30 H30C 0.96 . ? C31 O4 1.425(5) . ? C31 H31A 0.96 . ? C31 H31B 0.96 . ? C31 H31C 0.96 . ? N1 Zn2 2.188(3) . ? N2 Zn2 2.148(3) . ? N3 Zn1 2.184(3) . ? N4 Zn1 2.123(3) . ? O1 Zn1 2.006(2) . ? O1 Zn2 2.024(3) . ? O2 Zn1 2.049(3) . ? O3 Zn2 1.992(2) . ? O4 Zn2 2.467(3) . ? O5 Zn1 2.397(3) . ? O6 Zn1 1.997(3) . ? O7 Zn2 2.076(3) . ? P1 F6' 1.361(11) . ? P1 F4' 1.462(10) . ? P1 F3' 1.497(11) . ? P1 F3 1.506(5) . ? P1 F5 1.520(4) . ? P1 F4 1.533(5) . ? P1 F2 1.535(4) . ? P1 F1 1.562(5) . ? P1 F1' 1.584(12) . ? P1 F6 1.609(4) . ? P1 F2' 1.653(10) . ? P1 F5' 1.768(10) . ? 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 C2 C1 C6 117.3(4) . . ? C2 C1 C7 121.8(4) . . ? C6 C1 C7 120.9(4) . . ? C1 C2 C3 122.7(4) . . ? C1 C2 H2 118.7 . . ? C3 C2 H2 118.7 . . ? C2 C3 C4 118.7(4) . . ? C2 C3 C8 120.9(3) . . ? C4 C3 C8 120.3(3) . . ? O1 C4 C5 120.9(3) . . ? O1 C4 C3 119.3(4) . . ? C5 C4 C3 119.9(4) . . ? C4 C5 C6 119.1(4) . . ? C4 C5 C25 119.9(3) . . ? C6 C5 C25 121.0(4) . . ? C1 C6 C5 122.4(4) . . ? C1 C6 H6 118.8 . . ? C5 C6 H6 118.8 . . ? C1 C7 H7A 109.3 . . ? C1 C7 H7B 109.9 . . ? H7A C7 H7B 109.5 . . ? C1 C7 H7C 109.2 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C3 113.5(3) . . ? N1 C8 H8A 108.9 . . ? C3 C8 H8A 108.9 . . ? N1 C8 H8B 108.9 . . ? C3 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? N2 C9 C10 121.4(4) . . ? N2 C9 C14 114.6(4) . . ? C10 C9 C14 124.0(4) . . ? C9 C10 C11 120.2(4) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C12 C11 C10 118.5(4) . . ? C12 C11 H11 120.7 . . ? C10 C11 H11 120.7 . . ? C11 C12 C13 119.2(4) . . ? C11 C12 H12 120.4 . . ? C13 C12 H12 120.4 . . ? N2 C13 C12 122.9(4) . . ? N2 C13 H13 118.6 . . ? C12 C13 H13 118.6 . . ? N1 C14 C9 110.7(3) . . ? N1 C14 H14A 109.5 . . ? C9 C14 H14A 109.5 . . ? N1 C14 H14B 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? N1 C15 C16 114.6(3) . . ? N1 C15 H15A 108.6 . . ? C16 C15 H15A 108.6 . . ? N1 C15 H15B 108.6 . . ? C16 C15 H15B 108.6 . . ? H15A C15 H15B 107.6 . . ? O4 C16 C15 107.9(4) . . ? O4 C16 H16A 110.1 . . ? C15 C16 H16A 110.1 . . ? O4 C16 H16B 110.1 . . ? C15 C16 H16B 110.1 . . ? H16A C16 H16B 108.4 . . ? N4 C17 C18 122.3(5) . . ? N4 C17 H17 118.9 . . ? C18 C17 H17 118.9 . . ? C19 C18 C17 117.8(5) . . ? C19 C18 H18 121.1 . . ? C17 C18 H18 121.1 . . ? C18 C19 C20 120.0(4) . . ? C18 C19 H19 120 . . ? C20 C19 H19 120 . . ? C21 C20 C19 119.0(4) . . ? C21 C20 H20 120.5 . . ? C19 C20 H20 120.5 . . ? N4 C21 C20 121.3(4) . . ? N4 C21 C22 115.2(4) . . ? C20 C21 C22 123.5(4) . . ? N3 C22 C21 110.7(3) . . ? N3 C22 H22A 109.5 . . ? C21 C22 H22A 109.5 . . ? N3 C22 H22B 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? N3 C23 C24 113.8(3) . . ? N3 C23 H23A 108.8 . . ? C24 C23 H23A 108.8 . . ? N3 C23 H23B 108.8 . . ? C24 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? O5 C24 C23 108.5(3) . . ? O5 C24 H24A 110 . . ? C23 C24 H24A 110 . . ? O5 C24 H24B 110 . . ? C23 C24 H24B 110 . . ? H24A C24 H24B 108.4 . . ? N3 C25 C5 113.8(3) . . ? N3 C25 H25A 108.8 . . ? C5 C25 H25A 108.8 . . ? N3 C25 H25B 108.8 . . ? C5 C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? C27 C26 H26A 109.5 . . ? C27 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C27 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O2 C27 O3 125.7(4) . . ? O2 C27 C26 117.3(4) . . ? O3 C27 C26 117.0(4) . . ? O7 C28 O6 125.8(4) . . ? O7 C28 C29 118.8(4) . . ? O6 C28 C29 115.4(4) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O5 C30 H30A 109.5 . . ? O5 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O5 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O4 C31 H31A 109.5 . . ? O4 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O4 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C14 N1 C8 110.1(3) . . ? C14 N1 C15 109.1(3) . . ? C8 N1 C15 112.4(3) . . ? C14 N1 Zn2 102.3(2) . . ? C8 N1 Zn2 108.3(2) . . ? C15 N1 Zn2 114.2(2) . . ? C13 N2 C9 117.8(4) . . ? C13 N2 Zn2 129.1(3) . . ? C9 N2 Zn2 112.9(3) . . ? C22 N3 C25 110.9(3) . . ? C22 N3 C23 108.7(3) . . ? C25 N3 C23 112.3(3) . . ? C22 N3 Zn1 102.3(2) . . ? C25 N3 Zn1 109.0(2) . . ? C23 N3 Zn1 113.3(2) . . ? C17 N4 C21 119.6(4) . . ? C17 N4 Zn1 127.1(3) . . ? C21 N4 Zn1 113.2(3) . . ? C4 O1 Zn1 122.6(2) . . ? C4 O1 Zn2 127.5(2) . . ? Zn1 O1 Zn2 109.70(11) . . ? C27 O2 Zn1 134.0(3) . . ? C27 O3 Zn2 129.1(3) . . ? C16 O4 C31 111.3(3) . . ? C16 O4 Zn2 109.8(2) . . ? C31 O4 Zn2 121.2(3) . . ? C24 O5 C30 112.4(3) . . ? C24 O5 Zn1 113.4(3) . . ? C30 O5 Zn1 121.8(3) . . ? C28 O6 Zn1 131.0(3) . . ? C28 O7 Zn2 131.9(3) . . ? F6' P1 F4' 106.2(8) . . ? F6' P1 F3' 101.5(8) . . ? F4' P1 F3' 83.1(6) . . ? F3 P1 F5 99.4(4) . . ? F3 P1 F4 84.9(4) . . ? F5 P1 F4 90.2(3) . . ? F3 P1 F2 91.9(5) . . ? F5 P1 F2 92.7(3) . . ? F4 P1 F2 176.0(4) . . ? F3 P1 F1 172.6(4) . . ? F5 P1 F1 86.8(3) . . ? F4 P1 F1 99.2(5) . . ? F2 P1 F1 83.8(4) . . ? F6' P1 F1' 90.3(7) . . ? F4' P1 F1' 104.3(7) . . ? F3' P1 F1' 163.9(9) . . ? F3 P1 F6 89.2(3) . . ? F5 P1 F6 171.4(3) . . ? F4 P1 F6 90.3(3) . . ? F2 P1 F6 87.3(3) . . ? F1 P1 F6 84.7(3) . . ? F6' P1 F2' 91.8(7) . . ? F4' P1 F2' 161.2(7) . . ? F3' P1 F2' 88.0(6) . . ? F1' P1 F2' 80.6(6) . . ? F6' P1 F5' 165.3(8) . . ? F4' P1 F5' 84.5(5) . . ? F3' P1 F5' 89.7(6) . . ? F1' P1 F5' 77.1(6) . . ? F2' P1 F5' 78.9(5) . . ? O6 Zn1 O1 99.21(11) . . ? O6 Zn1 O2 102.15(12) . . ? O1 Zn1 O2 91.69(11) . . ? O6 Zn1 N4 93.23(13) . . ? O1 Zn1 N4 167.50(13) . . ? O2 Zn1 N4 84.39(12) . . ? O6 Zn1 N3 155.99(13) . . ? O1 Zn1 N3 91.24(11) . . ? O2 Zn1 N3 99.06(13) . . ? N4 Zn1 N3 77.71(13) . . ? O6 Zn1 O5 84.22(11) . . ? O1 Zn1 O5 89.46(10) . . ? O2 Zn1 O5 173.24(12) . . ? N4 Zn1 O5 93.09(11) . . ? N3 Zn1 O5 74.25(12) . . ? O3 Zn2 O1 100.72(11) . . ? O3 Zn2 O7 102.16(11) . . ? O1 Zn2 O7 92.69(11) . . ? O3 Zn2 N2 91.48(12) . . ? O1 Zn2 N2 167.01(11) . . ? O7 Zn2 N2 89.03(12) . . ? O3 Zn2 N1 157.91(13) . . ? O1 Zn2 N1 88.93(10) . . ? O7 Zn2 N1 97.13(12) . . ? N2 Zn2 N1 78.08(12) . . ? O3 Zn2 O4 86.12(11) . . ? O1 Zn2 O4 88.43(10) . . ? O7 Zn2 O4 171.27(10) . . ? N2 Zn2 O4 87.96(11) . . ? N1 Zn2 O4 74.23(11) . . ? #===END #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2011-06-15 at 18:09:27 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : 433ld5 433 struct data_433ld5 _database_code_depnum_ccdc_archive 'CCDC 830842' #TrackingRef 'supdata.cif' _audit_creation_date 2011-06-15T18:09:27-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C41 H45 F6 N4 O7 P1 Zn2' _chemical_formula_sum 'C41 H45 F6 N4 O7 P Zn2' _chemical_formula_weight 981.52 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4535(7) _cell_length_b 13.1726(8) _cell_length_c 16.4175(8) _cell_angle_alpha 83.319(5) _cell_angle_beta 85.597(5) _cell_angle_gamma 84.177(5) _cell_volume 2228.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2787 _cell_measurement_theta_min 2.8304 _cell_measurement_theta_max 29.015 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.188 _exptl_absorpt_correction_type multi-scan _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_absorpt_correction_T_min 0.98303 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 16.0696 _diffrn_orient_matrix_ub_11 -0.0213579 _diffrn_orient_matrix_ub_12 -0.0486668 _diffrn_orient_matrix_ub_13 -0.0033782 _diffrn_orient_matrix_ub_21 0.0640651 _diffrn_orient_matrix_ub_22 -0.0191526 _diffrn_orient_matrix_ub_23 -0.0111132 _diffrn_orient_matrix_ub_31 0.0105641 _diffrn_orient_matrix_ub_32 -0.0151612 _diffrn_orient_matrix_ub_33 0.0420178 _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_unetI/netI 0.2183 _diffrn_reflns_number 15104 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 7839 _reflns_number_gt 2750 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0280P)^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_number_reflns 7839 _refine_ls_number_parameters 576 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1673 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.0855 _refine_ls_wR_factor_gt 0.0713 _refine_ls_goodness_of_fit_ref 0.704 _refine_ls_restrained_S_all 0.703 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.398 _refine_diff_density_min -0.258 _refine_diff_density_rms 0.047 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8244(9) 0.0712(6) 0.9066(4) 0.102(3) Uani 1 1 d . . . C2 C 0.7562(7) 0.1640(6) 0.8824(4) 0.097(2) Uani 1 1 d . . . H3 H 0.6733 0.1781 0.9058 0.117 Uiso 1 1 calc R . . C3 C 0.8076(7) 0.2370(5) 0.8241(4) 0.0742(18) Uani 1 1 d . . . C4 C 0.9300(7) 0.2178(5) 0.7876(4) 0.0649(16) Uani 1 1 d . . . C5 C 0.9998(7) 0.1235(5) 0.8101(4) 0.0763(18) Uani 1 1 d . . . C6 C 0.9463(8) 0.0521(5) 0.8690(4) 0.100(2) Uani 1 1 d . . . H7 H 0.9938 -0.0102 0.8834 0.121 Uiso 1 1 calc R . . C7 C 0.7709(7) -0.0076(4) 0.9716(3) 0.164(3) Uani 1 1 d . . . H1A H 0.8335 -0.0657 0.9799 0.246 Uiso 1 1 calc R . . H1B H 0.6937 -0.0293 0.9538 0.246 Uiso 1 1 calc R . . H1C H 0.7515 0.0224 1.0222 0.246 Uiso 1 1 calc R . . C8 C 0.7314(5) 0.3389(4) 0.8026(3) 0.0786(17) Uani 1 1 d . . . H8A H 0.72 0.3486 0.7441 0.094 Uiso 1 1 calc R . . H8B H 0.6467 0.3388 0.8313 0.094 Uiso 1 1 calc R . . C9 C 0.8041(7) 0.6105(5) 0.8030(3) 0.0707(17) Uani 1 1 d . . . C10 C 0.7611(7) 0.7036(6) 0.8303(4) 0.102(2) Uani 1 1 d . . . H19 H 0.6762 0.7163 0.8507 0.122 Uiso 1 1 calc R . . C11 C 0.8463(9) 0.7780(6) 0.8270(4) 0.114(3) Uani 1 1 d . . . H20 H 0.8189 0.8415 0.845 0.137 Uiso 1 1 calc R . . C12 C 0.9690(8) 0.7581(5) 0.7975(4) 0.102(2) Uani 1 1 d . . . H21 H 1.0271 0.8074 0.7961 0.123 Uiso 1 1 calc R . . C13 C 1.0079(6) 0.6652(5) 0.7698(3) 0.0799(18) Uani 1 1 d . . . H22 H 1.0925 0.6517 0.7491 0.096 Uiso 1 1 calc R . . C14 C 0.7194(5) 0.5239(4) 0.8031(3) 0.0764(16) Uani 1 1 d . . . H17A H 0.6462 0.5322 0.8426 0.092 Uiso 1 1 calc R . . H17B H 0.6874 0.5244 0.7492 0.092 Uiso 1 1 calc R . . C15 C 0.8176(6) 0.4152(4) 0.9156(3) 0.0770(18) Uani 1 1 d . . . H9A H 0.7505 0.3769 0.9448 0.092 Uiso 1 1 calc R . . H9B H 0.8079 0.4832 0.9338 0.092 Uiso 1 1 calc R . . C16 C 0.9468(6) 0.3629(4) 0.9390(3) 0.0840(19) Uani 1 1 d . . . H10A H 0.958 0.3678 0.9964 0.101 Uiso 1 1 calc R . . H10B H 0.9527 0.2909 0.9304 0.101 Uiso 1 1 calc R . . C17 C 1.1947(5) 0.2417(4) 0.4484(4) 0.0726(17) Uani 1 1 d . . . H37 H 1.1437 0.3021 0.4337 0.087 Uiso 1 1 calc R . . C18 C 1.2701(7) 0.1964(6) 0.3887(4) 0.094(2) Uani 1 1 d . . . H36 H 1.2739 0.2268 0.3347 0.112 Uiso 1 1 calc R . . C19 C 1.3413(6) 0.1033(6) 0.4110(5) 0.095(2) Uani 1 1 d . . . H35 H 1.3915 0.0689 0.3717 0.114 Uiso 1 1 calc R . . C20 C 1.3361(6) 0.0632(5) 0.4918(5) 0.0842(19) Uani 1 1 d . . . H34 H 1.3828 0.0011 0.5078 0.101 Uiso 1 1 calc R . . C21 C 1.2624(6) 0.1145(5) 0.5488(4) 0.0692(17) Uani 1 1 d . . . C22 C 1.2584(6) 0.0813(4) 0.6388(4) 0.0837(18) Uani 1 1 d . . . H32A H 1.2856 0.0085 0.648 0.1 Uiso 1 1 calc R . . H32B H 1.3179 0.118 0.6642 0.1 Uiso 1 1 calc R . . C23 C 1.0481(7) 0.0238(4) 0.6558(4) 0.096(2) Uani 1 1 d . . . H24A H 1.0885 -0.0048 0.6073 0.115 Uiso 1 1 calc R . . H24B H 1.0477 -0.0315 0.7003 0.115 Uiso 1 1 calc R . . C24 C 0.9157(8) 0.0600(5) 0.6402(5) 0.134(3) Uani 1 1 d . . . H25A H 0.8725 0.0038 0.6251 0.161 Uiso 1 1 calc R . . H25B H 0.8717 0.0821 0.6902 0.161 Uiso 1 1 calc R . . C25 C 1.1287(6) 0.1008(4) 0.7689(4) 0.0810(18) Uani 1 1 d . . . H23A H 1.165 0.0338 0.7919 0.097 Uiso 1 1 calc R . . H23B H 1.1846 0.1511 0.7804 0.097 Uiso 1 1 calc R . . C26 C 0.7955(5) 0.4705(3) 0.5085(3) 0.0788(18) Uani 1 1 d . . . H39A H 0.8157 0.4317 0.4624 0.118 Uiso 1 1 calc R . . H39B H 0.8019 0.542 0.491 0.118 Uiso 1 1 calc R . . H39C H 0.7093 0.4607 0.5306 0.118 Uiso 1 1 calc R . . C27 C 0.8882(5) 0.4347(4) 0.5732(4) 0.0565(15) Uani 1 1 d . . . C28 C 1.2472(6) 0.4054(5) 0.6876(3) 0.0611(16) Uani 1 1 d . . . C29 C 1.3801(5) 0.4426(4) 0.6906(3) 0.103(2) Uani 1 1 d . . . H41A H 1.3716 0.5056 0.7155 0.155 Uiso 1 1 calc R . . H41B H 1.4188 0.454 0.6358 0.155 Uiso 1 1 calc R . . H41C H 1.4334 0.3917 0.7224 0.155 Uiso 1 1 calc R . . C30 C 0.7867(9) 0.1778(5) 0.5505(7) 0.089(2) Uani 1 1 d . . . C31 C 1.1660(7) 0.3889(6) 0.9104(3) 0.0726(17) Uani 1 1 d . . . C32 C 0.7845(9) 0.2049(5) 0.4676(6) 0.108(2) Uani 1 1 d . . . H27 H 0.8589 0.1956 0.4334 0.13 Uiso 1 1 calc R . . C33 C 0.6717(13) 0.2456(8) 0.4365(7) 0.148(4) Uani 1 1 d . . . H28 H 0.6698 0.2643 0.3801 0.178 Uiso 1 1 calc R . . C34 C 0.5586(19) 0.2604(13) 0.4860(11) 0.217(10) Uani 1 1 d . . . H29 H 0.4813 0.2872 0.4641 0.261 Uiso 1 1 calc R . . C35 C 0.5662(13) 0.2353(10) 0.5632(10) 0.181(7) Uani 1 1 d . . . H30 H 0.4914 0.2467 0.5967 0.217 Uiso 1 1 calc R . . C36 C 0.6766(11) 0.1923(6) 0.6018(5) 0.124(3) Uani 1 1 d . . . H31 H 0.6761 0.1745 0.6583 0.148 Uiso 1 1 calc R . . C37 C 1.2434(7) 0.4672(5) 0.9029(3) 0.0810(18) Uani 1 1 d . . . H16 H 1.2107 0.533 0.8832 0.097 Uiso 1 1 calc R . . C38 C 1.3708(7) 0.4498(6) 0.9241(4) 0.093(2) Uani 1 1 d . . . H15 H 1.4233 0.5034 0.9184 0.111 Uiso 1 1 calc R . . C39 C 1.4177(7) 0.3528(7) 0.9535(3) 0.104(2) Uani 1 1 d . . . H14 H 1.5017 0.3405 0.9696 0.125 Uiso 1 1 calc R . . C40 C 1.3409(9) 0.2739(6) 0.9590(4) 0.127(3) Uani 1 1 d . . . H13 H 1.3738 0.2073 0.9765 0.152 Uiso 1 1 calc R . . C41 C 1.2148(8) 0.2934(6) 0.9388(4) 0.114(2) Uani 1 1 d . . . H12 H 1.1621 0.2399 0.9447 0.137 Uiso 1 1 calc R . . N1 N 0.7977(4) 0.4254(3) 0.8255(2) 0.0617(12) Uani 1 1 d . . . N2 N 0.9243(5) 0.5930(3) 0.7722(2) 0.0665(12) Uani 1 1 d . . . N3 N 1.1276(5) 0.1014(3) 0.6772(3) 0.0711(13) Uani 1 1 d . . . N4 N 1.1912(4) 0.2026(4) 0.5274(3) 0.0655(13) Uani 1 1 d . . . O1 O 0.9814(3) 0.2879(2) 0.73298(19) 0.0651(10) Uani 1 1 d . . . O2 O 0.9752(4) 0.3631(3) 0.55671(18) 0.0674(10) Uani 1 1 d . . . O3 O 0.8756(3) 0.4762(2) 0.6378(2) 0.0687(11) Uani 1 1 d . . . O4 O 1.0419(4) 0.4125(3) 0.8890(2) 0.0898(12) Uani 1 1 d . . . O5 O 0.9068(5) 0.1385(4) 0.5798(3) 0.1160(16) Uani 1 1 d . . . O6 O 1.2439(3) 0.3230(3) 0.65667(19) 0.0657(10) Uani 1 1 d . . . O7 O 1.1537(4) 0.4610(3) 0.71374(19) 0.0648(10) Uani 1 1 d . . . P1 P 0.6369(3) 0.2099(2) 0.17474(15) 0.1249(8) Uani 1 1 d . . . F1 F 0.7231(10) 0.1521(7) 0.2403(5) 0.230(5) Uani 0.719(11) 1 d PD A 1 F2 F 0.7548(10) 0.1837(16) 0.1156(7) 0.294(7) Uani 0.719(11) 1 d PD A 1 F3 F 0.5634(9) 0.2713(10) 0.1115(5) 0.278(6) Uani 0.719(11) 1 d PD A 1 F4 F 0.5234(7) 0.2101(13) 0.2402(5) 0.264(6) Uani 0.719(11) 1 d PD A 1 F5 F 0.6933(11) 0.3054(6) 0.2006(7) 0.269(6) Uani 0.719(11) 1 d PD A 1 F6 F 0.5843(17) 0.1117(11) 0.1543(9) 0.364(8) Uani 0.719(11) 1 d PD A 1 F1' F 0.7153(18) 0.1166(11) 0.1466(9) 0.141(9) Uiso 0.281(11) 1 d PD A 2 F2' F 0.5799(19) 0.1309(10) 0.2423(9) 0.139(8) Uiso 0.281(11) 1 d PD A 2 F3' F 0.5444(14) 0.2965(10) 0.1987(9) 0.104(7) Uiso 0.281(11) 1 d PD A 2 F4' F 0.7129(15) 0.2790(10) 0.1120(8) 0.113(7) Uiso 0.281(11) 1 d PD A 2 F5' F 0.5417(15) 0.1833(13) 0.1102(9) 0.125(8) Uiso 0.281(11) 1 d PD A 2 F6' F 0.7275(16) 0.2311(17) 0.2356(10) 0.138(8) Uiso 0.281(11) 1 d PD A 2 Zn1 Zn 1.08291(6) 0.26255(4) 0.62756(3) 0.0635(2) Uani 1 1 d . . . Zn2 Zn 0.96956(6) 0.44059(4) 0.74190(3) 0.0611(2) 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 C1 0.141(8) 0.076(5) 0.087(5) -0.001(5) 0.031(5) -0.039(6) C2 0.105(7) 0.097(5) 0.094(5) -0.020(5) 0.026(4) -0.046(5) C3 0.079(6) 0.069(5) 0.076(4) -0.001(4) 0.000(4) -0.031(5) C4 0.052(5) 0.069(5) 0.073(4) -0.002(4) -0.002(4) -0.010(4) C5 0.082(6) 0.071(5) 0.072(4) -0.001(4) 0.009(4) -0.002(5) C6 0.150(8) 0.069(5) 0.077(5) 0.013(4) 0.007(5) -0.018(5) C7 0.278(10) 0.104(5) 0.108(5) -0.005(4) 0.069(6) -0.083(6) C8 0.055(5) 0.102(5) 0.081(4) -0.009(4) 0.004(3) -0.027(4) C9 0.057(5) 0.080(5) 0.076(4) -0.027(4) -0.011(4) 0.013(4) C10 0.074(6) 0.109(6) 0.122(5) -0.045(5) 0.006(4) 0.020(5) C11 0.108(8) 0.095(6) 0.145(6) -0.053(5) 0.000(6) 0.007(6) C12 0.099(7) 0.069(5) 0.139(6) -0.018(4) -0.016(5) 0.002(5) C13 0.069(5) 0.064(4) 0.104(5) -0.004(4) -0.004(4) 0.004(4) C14 0.046(4) 0.103(5) 0.080(4) -0.022(4) 0.006(3) 0.004(4) C15 0.078(5) 0.097(5) 0.061(4) -0.023(3) 0.011(3) -0.028(4) C16 0.064(5) 0.119(5) 0.070(4) -0.010(4) 0.001(4) -0.020(5) C17 0.073(5) 0.079(4) 0.069(4) -0.016(4) -0.009(4) -0.012(4) C18 0.111(7) 0.101(6) 0.075(5) -0.029(5) 0.005(4) -0.031(5) C19 0.077(6) 0.089(6) 0.126(7) -0.055(5) 0.008(5) -0.003(5) C20 0.072(5) 0.073(5) 0.111(5) -0.030(5) -0.002(5) -0.004(4) C21 0.060(5) 0.070(5) 0.082(5) -0.025(4) 0.007(4) -0.012(4) C22 0.078(6) 0.059(4) 0.109(5) -0.005(4) -0.006(4) 0.015(4) C23 0.100(6) 0.057(4) 0.130(5) 0.002(4) -0.005(5) -0.023(5) C24 0.128(9) 0.088(6) 0.196(8) -0.012(6) -0.023(7) -0.048(6) C25 0.103(6) 0.050(4) 0.088(5) 0.009(3) -0.036(4) 0.005(4) C26 0.083(5) 0.070(4) 0.090(4) -0.010(3) -0.032(4) -0.011(3) C27 0.042(4) 0.053(4) 0.072(4) 0.012(3) -0.009(4) -0.011(3) C28 0.057(5) 0.074(5) 0.049(4) 0.005(3) -0.003(3) 0.001(4) C29 0.052(5) 0.139(5) 0.129(5) -0.053(4) 0.001(4) -0.019(4) C30 0.086(8) 0.067(4) 0.121(7) -0.018(5) -0.023(7) -0.016(5) C31 0.060(5) 0.089(5) 0.065(4) 0.012(4) 0.001(4) -0.018(5) C32 0.125(9) 0.080(5) 0.125(8) -0.028(5) -0.027(6) -0.006(5) C33 0.173(13) 0.106(7) 0.184(10) -0.017(7) -0.099(11) -0.032(9) C34 0.150(14) 0.115(9) 0.42(3) -0.071(15) -0.146(19) -0.016(10) C35 0.046(7) 0.131(10) 0.39(2) -0.112(14) -0.035(12) -0.007(7) C36 0.108(8) 0.114(6) 0.163(7) -0.070(6) 0.039(8) -0.050(6) C37 0.075(6) 0.098(5) 0.071(4) -0.013(4) -0.002(4) -0.008(5) C38 0.070(6) 0.127(7) 0.080(5) -0.005(5) -0.001(4) -0.014(5) C39 0.062(6) 0.160(7) 0.079(5) 0.020(5) -0.013(4) 0.011(6) C40 0.100(8) 0.117(6) 0.149(6) 0.055(5) -0.015(6) -0.014(6) C41 0.072(6) 0.118(6) 0.143(6) 0.052(5) -0.029(5) -0.018(5) N1 0.053(3) 0.069(3) 0.064(3) -0.020(3) 0.000(2) -0.002(3) N2 0.054(4) 0.066(3) 0.078(3) -0.012(3) 0.004(3) -0.001(3) N3 0.065(4) 0.054(3) 0.090(4) 0.000(3) 0.000(3) -0.002(3) N4 0.070(4) 0.053(3) 0.072(4) -0.004(3) 0.001(3) -0.005(3) O1 0.059(3) 0.059(2) 0.073(2) 0.0056(19) 0.010(2) -0.010(2) O2 0.064(3) 0.071(3) 0.066(2) -0.003(2) -0.008(2) 0.000(2) O3 0.076(3) 0.067(2) 0.064(2) -0.020(2) -0.008(2) 0.004(2) O4 0.055(3) 0.122(3) 0.087(3) 0.020(2) -0.003(3) -0.022(3) O5 0.103(5) 0.090(3) 0.148(4) 0.034(3) -0.017(4) -0.022(3) O6 0.053(3) 0.067(2) 0.076(2) -0.013(2) 0.0027(19) 0.002(2) O7 0.056(3) 0.065(3) 0.072(2) -0.0111(19) 0.002(2) 0.001(2) P1 0.109(2) 0.132(2) 0.1272(19) 0.0017(17) -0.022(2) 0.0137(19) F1 0.236(11) 0.137(7) 0.293(10) 0.063(6) -0.101(8) 0.055(7) F2 0.202(12) 0.44(2) 0.243(10) -0.136(13) 0.065(9) 0.018(12) F3 0.172(10) 0.408(15) 0.225(9) 0.154(10) -0.114(7) -0.022(10) F4 0.112(7) 0.47(2) 0.167(7) 0.081(10) 0.055(5) 0.000(9) F5 0.359(15) 0.106(6) 0.364(14) 0.002(6) -0.130(10) -0.085(7) F6 0.40(2) 0.361(16) 0.40(2) -0.168(15) -0.011(14) -0.226(14) Zn1 0.0628(6) 0.0528(4) 0.0724(4) -0.0041(3) -0.0013(4) 0.0012(4) Zn2 0.0553(5) 0.0598(4) 0.0663(4) -0.0070(3) 0.0020(3) -0.0011(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.383(8) . ? C1 C6 1.386(8) . ? C1 C7 1.515(7) . ? C2 C3 1.394(7) . ? C2 H3 0.93 . ? C3 C4 1.383(7) . ? C3 C8 1.509(7) . ? C4 O1 1.334(6) . ? C4 C5 1.401(7) . ? C5 C6 1.394(7) . ? C5 C25 1.480(7) . ? C6 H7 0.93 . ? C7 H1A 0.96 . ? C7 H1B 0.96 . ? C7 H1C 0.96 . ? C8 N1 1.489(5) . ? C8 H8A 0.97 . ? C8 H8B 0.97 . ? C9 N2 1.326(6) . ? C9 C10 1.376(7) . ? C9 C14 1.513(7) . ? C10 C11 1.383(8) . ? C10 H19 0.93 . ? C11 C12 1.347(8) . ? C11 H20 0.93 . ? C12 C13 1.367(7) . ? C12 H21 0.93 . ? C13 N2 1.351(6) . ? C13 H22 0.93 . ? C14 N1 1.486(6) . ? C14 H17A 0.97 . ? C14 H17B 0.97 . ? C15 N1 1.498(5) . ? C15 C16 1.508(6) . ? C15 H9A 0.97 . ? C15 H9B 0.97 . ? C16 O4 1.404(5) . ? C16 H10A 0.97 . ? C16 H10B 0.97 . ? C17 N4 1.337(6) . ? C17 C18 1.364(7) . ? C17 H37 0.93 . ? C18 C19 1.395(7) . ? C18 H36 0.93 . ? C19 C20 1.368(7) . ? C19 H35 0.93 . ? C20 C21 1.363(7) . ? C20 H34 0.93 . ? C21 N4 1.340(6) . ? C21 C22 1.490(6) . ? C22 N3 1.473(6) . ? C22 H32A 0.97 . ? C22 H32B 0.97 . ? C23 C24 1.449(7) . ? C23 N3 1.470(6) . ? C23 H24A 0.97 . ? C23 H24B 0.97 . ? C24 O5 1.347(7) . ? C24 H25A 0.97 . ? C24 H25B 0.97 . ? C25 N3 1.505(6) . ? C25 H23A 0.97 . ? C25 H23B 0.97 . ? C26 C27 1.497(6) . ? C26 H39A 0.96 . ? C26 H39B 0.96 . ? C26 H39C 0.96 . ? C27 O3 1.241(5) . ? C27 O2 1.279(6) . ? C28 O7 1.241(6) . ? C28 O6 1.256(5) . ? C28 C29 1.525(6) . ? C29 H41A 0.96 . ? C29 H41B 0.96 . ? C29 H41C 0.96 . ? C30 C32 1.367(8) . ? C30 C36 1.383(8) . ? C30 O5 1.407(7) . ? C31 C41 1.352(7) . ? C31 C37 1.363(6) . ? C31 O4 1.366(6) . ? C32 C33 1.357(10) . ? C32 H27 0.93 . ? C33 C34 1.393(17) . ? C33 H28 0.93 . ? C34 C35 1.278(18) . ? C34 H29 0.93 . ? C35 C36 1.397(12) . ? C35 H30 0.93 . ? C36 H31 0.93 . ? C37 C38 1.392(7) . ? C37 H16 0.93 . ? C38 C39 1.368(7) . ? C38 H15 0.93 . ? C39 C40 1.366(8) . ? C39 H14 0.93 . ? C40 C41 1.376(8) . ? C40 H13 0.93 . ? C41 H12 0.93 . ? N1 Zn2 2.187(4) . ? N2 Zn2 2.123(4) . ? N3 Zn1 2.200(4) . ? N4 Zn1 2.108(4) . ? O1 Zn1 2.003(3) . ? O1 Zn2 2.024(3) . ? O2 Zn1 1.979(3) . ? O3 Zn2 2.021(3) . ? O4 Zn2 2.561(3) . ? O5 Zn1 2.793(4) . ? O6 Zn1 2.044(3) . ? O7 Zn2 1.982(4) . ? P1 F3 1.457(7) . ? P1 F3' 1.487(10) . ? P1 F6' 1.496(13) . ? P1 F1' 1.505(12) . ? P1 F4' 1.525(11) . ? P1 F6 1.537(8) . ? P1 F4 1.539(7) . ? P1 F1 1.539(7) . ? P1 F2 1.545(8) . ? P1 F5 1.557(7) . ? P1 F2' 1.557(12) . ? P1 F5' 1.599(11) . ? 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 C2 C1 C6 117.2(7) . . ? C2 C1 C7 122.6(8) . . ? C6 C1 C7 120.2(7) . . ? C1 C2 C3 122.1(7) . . ? C1 C2 H3 118.9 . . ? C3 C2 H3 118.9 . . ? C4 C3 C2 120.2(7) . . ? C4 C3 C8 119.7(6) . . ? C2 C3 C8 120.0(7) . . ? O1 C4 C3 120.9(6) . . ? O1 C4 C5 120.6(6) . . ? C3 C4 C5 118.5(6) . . ? C6 C5 C4 120.0(6) . . ? C6 C5 C25 121.2(6) . . ? C4 C5 C25 118.8(6) . . ? C1 C6 C5 121.9(7) . . ? C1 C6 H7 119.1 . . ? C5 C6 H7 119.1 . . ? C1 C7 H1A 109.5 . . ? C1 C7 H1B 109.5 . . ? H1A C7 H1B 109.5 . . ? C1 C7 H1C 109.5 . . ? H1A C7 H1C 109.5 . . ? H1B C7 H1C 109.5 . . ? N1 C8 C3 111.3(4) . . ? N1 C8 H8A 109.4 . . ? C3 C8 H8A 109.4 . . ? N1 C8 H8B 109.4 . . ? C3 C8 H8B 109.4 . . ? H8A C8 H8B 108 . . ? N2 C9 C10 120.7(6) . . ? N2 C9 C14 115.8(6) . . ? C10 C9 C14 123.5(7) . . ? C9 C10 C11 118.9(7) . . ? C9 C10 H19 120.6 . . ? C11 C10 H19 120.6 . . ? C12 C11 C10 119.8(7) . . ? C12 C11 H20 120.1 . . ? C10 C11 H20 120.1 . . ? C11 C12 C13 119.8(7) . . ? C11 C12 H21 120.1 . . ? C13 C12 H21 120.1 . . ? N2 C13 C12 120.5(6) . . ? N2 C13 H22 119.8 . . ? C12 C13 H22 119.8 . . ? N1 C14 C9 108.3(5) . . ? N1 C14 H17A 110 . . ? C9 C14 H17A 110 . . ? N1 C14 H17B 110 . . ? C9 C14 H17B 110 . . ? H17A C14 H17B 108.4 . . ? N1 C15 C16 114.7(4) . . ? N1 C15 H9A 108.6 . . ? C16 C15 H9A 108.6 . . ? N1 C15 H9B 108.6 . . ? C16 C15 H9B 108.6 . . ? H9A C15 H9B 107.6 . . ? O4 C16 C15 107.5(5) . . ? O4 C16 H10A 110.2 . . ? C15 C16 H10A 110.2 . . ? O4 C16 H10B 110.2 . . ? C15 C16 H10B 110.2 . . ? H10A C16 H10B 108.5 . . ? N4 C17 C18 122.6(6) . . ? N4 C17 H37 118.7 . . ? C18 C17 H37 118.7 . . ? C17 C18 C19 118.1(6) . . ? C17 C18 H36 120.9 . . ? C19 C18 H36 120.9 . . ? C20 C19 C18 118.9(6) . . ? C20 C19 H35 120.6 . . ? C18 C19 H35 120.6 . . ? C21 C20 C19 119.9(6) . . ? C21 C20 H34 120.1 . . ? C19 C20 H34 120.1 . . ? N4 C21 C20 121.5(6) . . ? N4 C21 C22 114.7(6) . . ? C20 C21 C22 123.8(7) . . ? N3 C22 C21 111.1(5) . . ? N3 C22 H32A 109.4 . . ? C21 C22 H32A 109.4 . . ? N3 C22 H32B 109.4 . . ? C21 C22 H32B 109.4 . . ? H32A C22 H32B 108 . . ? C24 C23 N3 115.6(5) . . ? C24 C23 H24A 108.4 . . ? N3 C23 H24A 108.4 . . ? C24 C23 H24B 108.4 . . ? N3 C23 H24B 108.4 . . ? H24A C23 H24B 107.4 . . ? O5 C24 C23 112.5(7) . . ? O5 C24 H25A 109.1 . . ? C23 C24 H25A 109.1 . . ? O5 C24 H25B 109.1 . . ? C23 C24 H25B 109.1 . . ? H25A C24 H25B 107.8 . . ? C5 C25 N3 113.8(5) . . ? C5 C25 H23A 108.8 . . ? N3 C25 H23A 108.8 . . ? C5 C25 H23B 108.8 . . ? N3 C25 H23B 108.8 . . ? H23A C25 H23B 107.7 . . ? C27 C26 H39A 109.5 . . ? C27 C26 H39B 109.5 . . ? H39A C26 H39B 109.5 . . ? C27 C26 H39C 109.5 . . ? H39A C26 H39C 109.5 . . ? H39B C26 H39C 109.5 . . ? O3 C27 O2 125.3(5) . . ? O3 C27 C26 118.2(5) . . ? O2 C27 C26 116.5(5) . . ? O7 C28 O6 126.8(6) . . ? O7 C28 C29 116.8(5) . . ? O6 C28 C29 116.3(5) . . ? C28 C29 H41A 109.5 . . ? C28 C29 H41B 109.5 . . ? H41A C29 H41B 109.5 . . ? C28 C29 H41C 109.5 . . ? H41A C29 H41C 109.5 . . ? H41B C29 H41C 109.5 . . ? C32 C30 C36 120.9(8) . . ? C32 C30 O5 116.2(9) . . ? C36 C30 O5 122.8(10) . . ? C41 C31 C37 119.0(7) . . ? C41 C31 O4 123.8(6) . . ? C37 C31 O4 117.2(7) . . ? C33 C32 C30 118.6(9) . . ? C33 C32 H27 120.7 . . ? C30 C32 H27 120.7 . . ? C32 C33 C34 122.2(15) . . ? C32 C33 H28 118.9 . . ? C34 C33 H28 118.9 . . ? C35 C34 C33 117(2) . . ? C35 C34 H29 121.6 . . ? C33 C34 H29 121.6 . . ? C34 C35 C36 126(2) . . ? C34 C35 H30 117 . . ? C36 C35 H30 117 . . ? C30 C36 C35 115.7(10) . . ? C30 C36 H31 122.2 . . ? C35 C36 H31 122.2 . . ? C31 C37 C38 120.9(6) . . ? C31 C37 H16 119.6 . . ? C38 C37 H16 119.6 . . ? C39 C38 C37 119.1(7) . . ? C39 C38 H15 120.5 . . ? C37 C38 H15 120.5 . . ? C40 C39 C38 119.9(7) . . ? C40 C39 H14 120 . . ? C38 C39 H14 120 . . ? C39 C40 C41 119.7(7) . . ? C39 C40 H13 120.1 . . ? C41 C40 H13 120.1 . . ? C31 C41 C40 121.3(7) . . ? C31 C41 H12 119.3 . . ? C40 C41 H12 119.3 . . ? C14 N1 C8 109.4(4) . . ? C14 N1 C15 108.8(4) . . ? C8 N1 C15 112.0(4) . . ? C14 N1 Zn2 101.8(3) . . ? C8 N1 Zn2 107.6(3) . . ? C15 N1 Zn2 116.5(3) . . ? C9 N2 C13 120.4(5) . . ? C9 N2 Zn2 113.1(4) . . ? C13 N2 Zn2 126.1(5) . . ? C23 N3 C22 108.2(5) . . ? C23 N3 C25 111.3(4) . . ? C22 N3 C25 111.7(5) . . ? C23 N3 Zn1 118.7(3) . . ? C22 N3 Zn1 100.2(3) . . ? C25 N3 Zn1 106.3(3) . . ? C17 N4 C21 119.0(5) . . ? C17 N4 Zn1 127.8(4) . . ? C21 N4 Zn1 113.3(4) . . ? C4 O1 Zn1 126.8(3) . . ? C4 O1 Zn2 125.7(3) . . ? Zn1 O1 Zn2 107.49(16) . . ? C27 O2 Zn1 132.2(3) . . ? C27 O3 Zn2 129.7(3) . . ? C31 O4 C16 116.5(5) . . ? C31 O4 Zn2 125.5(3) . . ? C16 O4 Zn2 107.8(3) . . ? C24 O5 C30 120.9(6) . . ? C24 O5 Zn1 100.4(4) . . ? C30 O5 Zn1 123.0(3) . . ? C28 O6 Zn1 126.5(4) . . ? C28 O7 Zn2 133.6(4) . . ? F3 P1 F3' 61.2(6) . . ? F3 P1 F6' 135.6(9) . . ? F3' P1 F6' 90.6(7) . . ? F3 P1 F1' 114.6(7) . . ? F3' P1 F1' 172.4(9) . . ? F6' P1 F1' 96.4(11) . . ? F3 P1 F4' 63.8(6) . . ? F3' P1 F4' 93.2(7) . . ? F6' P1 F4' 86.3(8) . . ? F1' P1 F4' 90.2(7) . . ? F3 P1 F6 90.8(6) . . ? F3' P1 F6 119.0(9) . . ? F6' P1 F6 133.6(12) . . ? F1' P1 F6 53.7(7) . . ? F4' P1 F6 123.2(7) . . ? F3 P1 F4 94.3(6) . . ? F3' P1 F4 50.3(5) . . ? F6' P1 F4 91.5(8) . . ? F1' P1 F4 126.3(8) . . ? F4' P1 F4 143.4(8) . . ? F6 P1 F4 83.5(6) . . ? F3 P1 F1 175.0(7) . . ? F3' P1 F1 118.2(5) . . ? F6' P1 F1 40.0(6) . . ? F1' P1 F1 66.5(7) . . ? F4' P1 F1 111.6(8) . . ? F6 P1 F1 93.6(9) . . ? F4 P1 F1 88.6(5) . . ? F3 P1 F2 94.6(6) . . ? F3' P1 F2 142.6(8) . . ? F6' P1 F2 88.6(8) . . ? F1' P1 F2 41.1(6) . . ? F4' P1 F2 49.4(7) . . ? F6 P1 F2 87.1(6) . . ? F4 P1 F2 167.2(9) . . ? F1 P1 F2 83.3(7) . . ? F3 P1 F5 92.8(6) . . ? F3' P1 F5 62.3(5) . . ? F6' P1 F5 42.8(7) . . ? F1' P1 F5 125.2(8) . . ? F4' P1 F5 59.5(5) . . ? F6 P1 F5 176.3(8) . . ? F4 P1 F5 95.3(6) . . ? F1 P1 F5 82.8(4) . . ? F2 P1 F5 93.5(7) . . ? F3 P1 F2' 124.7(9) . . ? F3' P1 F2' 93.5(7) . . ? F6' P1 F2' 87.9(7) . . ? F1' P1 F2' 83.8(8) . . ? F4' P1 F2' 171.2(11) . . ? F6 P1 F2' 57.7(7) . . ? F4 P1 F2' 43.4(6) . . ? F1 P1 F2' 60.0(6) . . ? F2 P1 F2' 123.8(11) . . ? F5 P1 F2' 119.2(7) . . ? F3 P1 F5' 46.2(5) . . ? F3' P1 F5' 91.0(7) . . ? F6' P1 F5' 178.1(11) . . ? F1' P1 F5' 81.9(6) . . ? F4' P1 F5' 94.6(6) . . ? F6 P1 F5' 44.6(6) . . ? F4 P1 F5' 88.8(8) . . ? F1 P1 F5' 138.2(7) . . ? F2 P1 F5' 90.7(8) . . ? F5 P1 F5' 139.0(7) . . ? F2' P1 F5' 91.1(8) . . ? O2 Zn1 O1 95.65(14) . . ? O2 Zn1 O6 111.58(13) . . ? O1 Zn1 O6 95.01(13) . . ? O2 Zn1 N4 93.73(18) . . ? O1 Zn1 N4 167.69(17) . . ? O6 Zn1 N4 88.92(15) . . ? O2 Zn1 N3 147.67(16) . . ? O1 Zn1 N3 89.34(16) . . ? O6 Zn1 N3 99.71(16) . . ? N4 Zn1 N3 78.48(19) . . ? O2 Zn1 O5 78.60(15) . . ? O1 Zn1 O5 93.86(13) . . ? O6 Zn1 O5 165.70(16) . . ? N4 Zn1 O5 80.19(15) . . ? N3 Zn1 O5 69.19(17) . . ? O7 Zn2 O3 107.51(13) . . ? O7 Zn2 O1 97.80(14) . . ? O3 Zn2 O1 93.12(12) . . ? O7 Zn2 N2 93.07(18) . . ? O3 Zn2 N2 90.17(15) . . ? O1 Zn2 N2 167.12(17) . . ? O7 Zn2 N1 154.54(14) . . ? O3 Zn2 N1 96.43(15) . . ? O1 Zn2 N1 89.24(15) . . ? N2 Zn2 N1 78.02(18) . . ? O7 Zn2 O4 83.05(14) . . ? O3 Zn2 O4 167.27(15) . . ? O1 Zn2 O4 92.43(12) . . ? N2 Zn2 O4 82.01(14) . . ? N1 Zn2 O4 72.19(15) . . ? #===END #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2011-06-15 at 17:54:18 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : 457ld9 457 struct data_457ld9 _database_code_depnum_ccdc_archive 'CCDC 830843' #TrackingRef 'supdata.cif' _audit_creation_date 2011-06-15T17:54:18-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C30 H38 F6 N5 O9 P1 Zn2' _chemical_formula_sum 'C30 H38 F6 N5 O9 P Zn2' _chemical_formula_weight 888.36 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.9260(10) _cell_length_b 31.571(2) _cell_length_c 13.3124(9) _cell_angle_alpha 90 _cell_angle_beta 103.264(9) _cell_angle_gamma 90 _cell_volume 3651.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3346 _cell_measurement_theta_min 3.4081 _cell_measurement_theta_max 64.2039 _cell_measurement_wavelength 1.5418 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.823 _exptl_absorpt_correction_type multi-scan _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_absorpt_correction_T_min 0.62244 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 16.0696 _diffrn_orient_matrix_ub_11 -0.0260358 _diffrn_orient_matrix_ub_12 -0.0463009 _diffrn_orient_matrix_ub_13 0.0281762 _diffrn_orient_matrix_ub_21 -0.1147669 _diffrn_orient_matrix_ub_22 -0.0059292 _diffrn_orient_matrix_ub_23 -0.1047842 _diffrn_orient_matrix_ub_31 0.1326516 _diffrn_orient_matrix_ub_32 -0.0142244 _diffrn_orient_matrix_ub_33 -0.0486106 _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0621 _diffrn_reflns_av_unetI/netI 0.0506 _diffrn_reflns_number 20343 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.69 _diffrn_reflns_theta_max 62.49 _diffrn_reflns_theta_full 62.49 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 5800 _reflns_number_gt 3675 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0736P)^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_number_reflns 5800 _refine_ls_number_parameters 503 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0787 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1257 _refine_ls_wR_factor_gt 0.1149 _refine_ls_goodness_of_fit_ref 0.93 _refine_ls_restrained_S_all 0.929 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.407 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.056 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8034(5) 0.46140(13) 0.4766(3) 0.0582(11) Uani 1 1 d . . . C2 C 0.9432(5) 0.44083(13) 0.4953(3) 0.0573(11) Uani 1 1 d . . . H2 H 1.0118 0.446 0.4536 0.069 Uiso 1 1 calc R . . C3 C 0.9808(4) 0.41256(12) 0.5761(3) 0.0532(10) Uani 1 1 d . . . C4 C 0.8737(4) 0.40530(13) 0.6382(3) 0.0537(10) Uani 1 1 d . . . C5 C 0.7320(5) 0.42648(14) 0.6177(3) 0.0585(11) Uani 1 1 d . . . C6 C 0.6972(5) 0.45466(14) 0.5356(4) 0.0626(11) Uani 1 1 d . . . H6 H 0.6033 0.4688 0.5206 0.075 Uiso 1 1 calc R . . C7 C 1.1311(5) 0.38950(12) 0.5999(4) 0.0590(11) Uani 1 1 d . . . H7A H 1.194 0.3993 0.5541 0.071 Uiso 1 1 calc R . . H7B H 1.1854 0.3957 0.6702 0.071 Uiso 1 1 calc R . . C8 C 1.0293(5) 0.33095(15) 0.4813(4) 0.0689(12) Uani 1 1 d . . . H8A H 1.0681 0.3036 0.4659 0.083 Uiso 1 1 calc R . . H8B H 1.0558 0.3513 0.4337 0.083 Uiso 1 1 calc R . . C9 C 0.8591(6) 0.32847(18) 0.4626(4) 0.0867(15) Uani 1 1 d . . . H9A H 0.8156 0.3568 0.4566 0.104 Uiso 1 1 calc R . . H9B H 0.8179 0.3135 0.3986 0.104 Uiso 1 1 calc R . . C10 C 1.2589(5) 0.32132(14) 0.6158(4) 0.0672(12) Uani 1 1 d . . . H10A H 1.3206 0.3336 0.6786 0.081 Uiso 1 1 calc R . . H10B H 1.3136 0.3252 0.5613 0.081 Uiso 1 1 calc R . . C11 C 1.2357(5) 0.27447(14) 0.6319(4) 0.0700(13) Uani 1 1 d . . . C12 C 1.3261(6) 0.24377(18) 0.6050(5) 0.0939(17) Uani 1 1 d . . . H12 H 1.4048 0.251 0.5729 0.113 Uiso 1 1 calc R . . C13 C 1.3002(7) 0.20155(19) 0.6258(6) 0.110(2) Uani 1 1 d . . . H13 H 1.3617 0.1801 0.6093 0.132 Uiso 1 1 calc R . . C14 C 1.1799(7) 0.19254(18) 0.6719(5) 0.1003(19) Uani 1 1 d . . . H14 H 1.1589 0.1647 0.6865 0.12 Uiso 1 1 calc R . . C15 C 1.0930(6) 0.22437(15) 0.6956(4) 0.0798(14) Uani 1 1 d . . . H15 H 1.0125 0.2179 0.7267 0.096 Uiso 1 1 calc R . . C16 C 0.6184(5) 0.41750(15) 0.6830(4) 0.0645(12) Uani 1 1 d . . . H16A H 0.5238 0.4328 0.6549 0.077 Uiso 1 1 calc R . . H16B H 0.5947 0.3875 0.6797 0.077 Uiso 1 1 calc R . . C17 C 0.7210(5) 0.47538(14) 0.8052(4) 0.0663(12) Uani 1 1 d . . . H17A H 0.6969 0.4857 0.8683 0.08 Uiso 1 1 calc R . . H17B H 0.6596 0.4914 0.7483 0.08 Uiso 1 1 calc R . . C18 C 0.8885(5) 0.48347(15) 0.8100(4) 0.0709(13) Uani 1 1 d . . . H18A H 0.9095 0.4799 0.7422 0.085 Uiso 1 1 calc R . . H18B H 0.9154 0.5122 0.8331 0.085 Uiso 1 1 calc R . . C19 C 1.1353(5) 0.46150(19) 0.9052(5) 0.0995(19) Uani 1 1 d . . . H19A H 1.1853 0.4404 0.9532 0.149 Uiso 1 1 calc R . . H19B H 1.1557 0.4891 0.9357 0.149 Uiso 1 1 calc R . . H19C H 1.1738 0.4601 0.8436 0.149 Uiso 1 1 calc R . . C20 C 0.5618(5) 0.41996(17) 0.8532(4) 0.0710(13) Uani 1 1 d . . . H20A H 0.5172 0.3923 0.834 0.085 Uiso 1 1 calc R . . H20B H 0.4796 0.4408 0.839 0.085 Uiso 1 1 calc R . . C21 C 0.6383(5) 0.42043(15) 0.9669(4) 0.0684(13) Uani 1 1 d . . . C22 C 0.5676(6) 0.43502(18) 1.0420(4) 0.0820(15) Uani 1 1 d . . . H22 H 0.468 0.4458 1.0241 0.098 Uiso 1 1 calc R . . C23 C 0.6465(7) 0.43346(18) 1.1442(5) 0.0887(17) Uani 1 1 d . . . H23 H 0.5986 0.4419 1.1961 0.106 Uiso 1 1 calc R . . C24 C 0.7958(7) 0.41943(16) 1.1685(4) 0.0791(14) Uani 1 1 d . . . H24 H 0.8525 0.4192 1.2365 0.095 Uiso 1 1 calc R . . C25 C 0.8592(6) 0.40568(14) 1.0894(4) 0.0656(12) Uani 1 1 d . . . H25 H 0.9602 0.396 1.1054 0.079 Uiso 1 1 calc R . . C26 C 0.7469(6) 0.29774(18) 0.8152(4) 0.0709(13) Uani 1 1 d . . . C27 C 0.6420(7) 0.26306(19) 0.8353(5) 0.107(2) Uani 1 1 d . . . H27A H 0.6703 0.2368 0.8083 0.16 Uiso 1 1 calc R . . H27B H 0.5375 0.2699 0.8021 0.16 Uiso 1 1 calc R . . H27C H 0.6511 0.2604 0.9083 0.16 Uiso 1 1 calc R . . C28 C 1.1695(6) 0.34257(15) 0.9196(4) 0.0700(12) Uani 1 1 d . . . C29 C 1.3050(7) 0.3319(2) 1.0052(5) 0.117(2) Uani 1 1 d . . . H29A H 1.2884 0.3427 1.0692 0.176 Uiso 1 1 calc R . . H29B H 1.3962 0.3444 0.9914 0.176 Uiso 1 1 calc R . . H29C H 1.3171 0.3017 1.01 0.176 Uiso 1 1 calc R . . C30 C 0.6583(7) 0.3019(3) 0.5286(6) 0.145(3) Uani 1 1 d . . . H30A H 0.6334 0.2872 0.5858 0.218 Uiso 1 1 calc R . . H30B H 0.6218 0.2858 0.4666 0.218 Uiso 1 1 calc R . . H30C H 0.6101 0.3292 0.5215 0.218 Uiso 1 1 calc R . . N3 N 1.1085(4) 0.34315(10) 0.5877(3) 0.0575(9) Uani 1 1 d . . . N4 N 1.1189(4) 0.26481(11) 0.6760(3) 0.0669(10) Uani 1 1 d . . . N1 N 0.6767(4) 0.42984(11) 0.7917(3) 0.0574(9) Uani 1 1 d . . . N2 N 0.7830(4) 0.40559(11) 0.9914(3) 0.0619(9) Uani 1 1 d . . . N5 N 0.7660(5) 0.49080(12) 0.3903(3) 0.0708(10) Uani 1 1 d . . . O1 O 0.9082(3) 0.37864(9) 0.7173(2) 0.0566(7) Uani 1 1 d . . . O5 O 0.8190(4) 0.30680(12) 0.5463(3) 0.0879(10) Uani 1 1 d . . . O4 O 0.9756(3) 0.45415(9) 0.8803(3) 0.0721(9) Uani 1 1 d . . . O2 O 0.8505(4) 0.28658(10) 0.7698(3) 0.0829(10) Uani 1 1 d . . . O3 O 0.7270(4) 0.33362(11) 0.8449(3) 0.0807(10) Uani 1 1 d . . . O6 O 1.1742(4) 0.33076(11) 0.8318(3) 0.0795(9) Uani 1 1 d . . . O7 O 1.0616(4) 0.36239(11) 0.9443(2) 0.0780(9) Uani 1 1 d . . . O8 O 0.8546(4) 0.49467(11) 0.3340(3) 0.0858(10) Uani 1 1 d . . . O9 O 0.6491(5) 0.51157(14) 0.3785(3) 0.1100(14) Uani 1 1 d . . . P1 P 0.67693(18) 0.60683(5) 0.69079(12) 0.0880(4) Uani 1 1 d . . . F1 F 0.5508(10) 0.6329(3) 0.7233(7) 0.181(5) Uani 0.758(12) 1 d PD A 1 F2 F 0.5671(10) 0.5687(3) 0.6625(5) 0.164(4) Uani 0.758(12) 1 d PD A 1 F3 F 0.8131(9) 0.5806(4) 0.6670(5) 0.170(4) Uani 0.758(12) 1 d PD A 1 F4 F 0.8003(13) 0.6426(3) 0.7342(6) 0.209(5) Uani 0.758(12) 1 d PD A 1 F5 F 0.6417(9) 0.6251(3) 0.5834(5) 0.204(6) Uani 0.758(12) 1 d PD A 1 F6 F 0.7174(8) 0.58672(17) 0.8051(4) 0.117(3) Uani 0.758(12) 1 d PD A 1 F1' F 0.4927(12) 0.6029(6) 0.6640(13) 0.098(6) Uiso 0.242(12) 1 d PD A 2 F2' F 0.677(2) 0.5606(4) 0.6364(12) 0.121(7) Uiso 0.242(12) 1 d PD A 2 F3' F 0.8454(12) 0.6110(6) 0.6943(13) 0.098(6) Uiso 0.242(12) 1 d PD A 2 F4' F 0.666(2) 0.6516(4) 0.7260(13) 0.121(7) Uiso 0.242(12) 1 d PD A 2 F5' F 0.6475(16) 0.6251(4) 0.5673(9) 0.099(7) Uiso 0.242(12) 1 d PD A 2 F6' F 0.691(2) 0.5862(6) 0.7873(11) 0.20(2) Uiso 0.242(12) 1 d PD A 2 Zn1 Zn 0.99581(7) 0.319447(17) 0.70665(5) 0.06125(19) Uani 1 1 d . . . Zn2 Zn 0.86647(6) 0.386978(18) 0.86052(4) 0.05964(19) 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 C1 0.073(3) 0.050(2) 0.048(3) 0.003(2) 0.005(2) 0.004(2) C2 0.067(3) 0.053(2) 0.054(3) -0.006(2) 0.021(2) -0.003(2) C3 0.057(2) 0.049(2) 0.053(3) -0.006(2) 0.011(2) 0.0002(19) C4 0.057(2) 0.051(2) 0.052(3) -0.003(2) 0.011(2) 0.0009(19) C5 0.057(2) 0.063(3) 0.055(3) -0.001(2) 0.011(2) 0.004(2) C6 0.057(2) 0.066(3) 0.060(3) 0.000(2) 0.005(2) 0.010(2) C7 0.059(2) 0.052(2) 0.070(3) 0.001(2) 0.023(2) 0.005(2) C8 0.082(3) 0.065(3) 0.061(3) -0.006(2) 0.021(3) 0.004(2) C9 0.097(4) 0.088(4) 0.074(4) -0.011(3) 0.018(3) -0.006(3) C10 0.058(2) 0.065(3) 0.082(3) 0.000(3) 0.022(2) 0.007(2) C11 0.062(3) 0.059(3) 0.081(4) -0.010(3) 0.002(3) 0.010(2) C12 0.080(3) 0.078(4) 0.123(5) -0.009(4) 0.023(3) 0.010(3) C13 0.104(4) 0.063(4) 0.160(7) -0.023(4) 0.022(4) 0.018(3) C14 0.112(4) 0.059(3) 0.118(5) -0.012(3) 0.001(4) 0.003(3) C15 0.091(3) 0.054(3) 0.085(4) -0.002(3) 0.001(3) 0.004(3) C16 0.055(2) 0.072(3) 0.066(3) -0.003(3) 0.014(2) 0.004(2) C17 0.068(3) 0.062(3) 0.072(3) 0.004(2) 0.022(2) 0.013(2) C18 0.081(3) 0.057(3) 0.078(3) 0.005(3) 0.026(3) 0.002(2) C19 0.061(3) 0.112(4) 0.118(5) 0.025(4) 0.004(3) -0.018(3) C20 0.057(2) 0.088(3) 0.073(3) -0.005(3) 0.023(2) 0.000(2) C21 0.063(3) 0.074(3) 0.075(3) -0.004(3) 0.029(3) -0.012(2) C22 0.070(3) 0.102(4) 0.083(4) -0.018(3) 0.037(3) -0.011(3) C23 0.101(4) 0.093(4) 0.086(4) -0.016(3) 0.053(4) -0.021(3) C24 0.105(4) 0.074(3) 0.063(3) -0.007(3) 0.028(3) -0.012(3) C25 0.075(3) 0.059(3) 0.063(3) 0.002(2) 0.016(3) -0.010(2) C26 0.079(3) 0.077(4) 0.051(3) 0.008(3) 0.004(3) -0.017(3) C27 0.137(5) 0.100(4) 0.088(4) 0.002(4) 0.036(4) -0.052(4) C28 0.073(3) 0.060(3) 0.066(3) 0.002(3) -0.005(3) 0.010(2) C29 0.110(4) 0.142(6) 0.079(4) -0.024(4) -0.022(4) 0.049(4) C30 0.083(4) 0.232(9) 0.119(6) 0.000(6) 0.021(4) -0.050(5) N3 0.062(2) 0.051(2) 0.061(2) -0.0028(18) 0.0164(18) 0.0065(16) N4 0.078(2) 0.048(2) 0.070(3) -0.0031(19) 0.008(2) 0.0032(18) N1 0.0541(18) 0.064(2) 0.056(2) 0.0031(19) 0.0163(17) 0.0043(17) N2 0.069(2) 0.062(2) 0.058(3) 0.0004(19) 0.019(2) -0.0075(18) N5 0.084(3) 0.062(2) 0.064(3) 0.003(2) 0.011(2) 0.004(2) O1 0.0609(16) 0.0578(16) 0.0511(17) 0.0045(14) 0.0132(14) 0.0117(13) O5 0.074(2) 0.112(3) 0.074(2) 0.002(2) 0.0103(18) -0.014(2) O4 0.0619(18) 0.0628(18) 0.090(2) 0.0140(18) 0.0153(17) -0.0021(15) O2 0.111(3) 0.0612(19) 0.083(2) 0.0037(18) 0.037(2) -0.0100(18) O3 0.093(2) 0.063(2) 0.095(3) -0.004(2) 0.042(2) -0.0176(18) O6 0.079(2) 0.090(2) 0.062(2) -0.0137(19) 0.0020(18) 0.0179(18) O7 0.085(2) 0.082(2) 0.063(2) 0.0031(18) 0.0080(18) 0.0249(19) O8 0.111(3) 0.084(2) 0.065(2) 0.0143(19) 0.026(2) 0.000(2) O9 0.112(3) 0.115(3) 0.105(3) 0.046(3) 0.028(3) 0.043(3) P1 0.0991(10) 0.0934(10) 0.0816(10) 0.0069(9) 0.0416(8) 0.0049(9) F1 0.220(8) 0.170(7) 0.202(7) 0.053(6) 0.146(7) 0.095(7) F2 0.188(8) 0.178(7) 0.114(5) -0.007(4) 0.011(5) -0.070(6) F3 0.160(6) 0.232(10) 0.144(5) 0.020(6) 0.085(5) 0.085(7) F4 0.250(11) 0.172(8) 0.214(8) -0.011(6) 0.076(8) -0.096(7) F5 0.174(7) 0.341(13) 0.122(5) 0.145(7) 0.089(5) 0.107(7) F6 0.145(5) 0.144(6) 0.067(3) 0.022(3) 0.032(3) 0.000(3) Zn1 0.0702(4) 0.0530(3) 0.0612(4) 0.0001(3) 0.0165(3) 0.0037(3) Zn2 0.0639(3) 0.0609(4) 0.0564(4) 0.0032(3) 0.0185(3) 0.0038(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.378(6) . ? C1 C6 1.380(6) . ? C1 N5 1.455(6) . ? C2 C3 1.378(6) . ? C2 H2 0.93 . ? C3 C4 1.419(5) . ? C3 C7 1.495(6) . ? C4 O1 1.328(5) . ? C4 C5 1.401(6) . ? C5 C6 1.389(6) . ? C5 C16 1.505(6) . ? C6 H6 0.93 . ? C7 N3 1.481(5) . ? C7 H7A 0.97 . ? C7 H7B 0.97 . ? C8 N3 1.481(6) . ? C8 C9 1.484(7) . ? C8 H8A 0.97 . ? C8 H8B 0.97 . ? C9 O5 1.422(6) . ? C9 H9A 0.97 . ? C9 H9B 0.97 . ? C10 N3 1.479(5) . ? C10 C11 1.516(6) . ? C10 H10A 0.97 . ? C10 H10B 0.97 . ? C11 N4 1.343(6) . ? C11 C12 1.361(7) . ? C12 C13 1.392(8) . ? C12 H12 0.93 . ? C13 C14 1.383(8) . ? C13 H13 0.93 . ? C14 C15 1.350(7) . ? C14 H14 0.93 . ? C15 N4 1.334(6) . ? C15 H15 0.93 . ? C16 N1 1.474(6) . ? C16 H16A 0.97 . ? C16 H16B 0.97 . ? C17 N1 1.491(6) . ? C17 C18 1.503(6) . ? C17 H17A 0.97 . ? C17 H17B 0.97 . ? C18 O4 1.415(5) . ? C18 H18A 0.97 . ? C18 H18B 0.97 . ? C19 O4 1.407(5) . ? C19 H19A 0.96 . ? C19 H19B 0.96 . ? C19 H19C 0.96 . ? C20 N1 1.485(5) . ? C20 C21 1.510(7) . ? C20 H20A 0.97 . ? C20 H20B 0.97 . ? C21 N2 1.342(6) . ? C21 C22 1.378(6) . ? C22 C23 1.383(8) . ? C22 H22 0.93 . ? C23 C24 1.371(7) . ? C23 H23 0.93 . ? C24 C25 1.376(6) . ? C24 H24 0.93 . ? C25 N2 1.326(6) . ? C25 H25 0.93 . ? C26 O3 1.226(6) . ? C26 O2 1.264(6) . ? C26 C27 1.504(7) . ? C27 H27A 0.96 . ? C27 H27B 0.96 . ? C27 H27C 0.96 . ? C28 O6 1.237(6) . ? C28 O7 1.254(5) . ? C28 C29 1.498(7) . ? C29 H29A 0.96 . ? C29 H29B 0.96 . ? C29 H29C 0.96 . ? C30 O5 1.408(6) . ? C30 H30A 0.96 . ? C30 H30B 0.96 . ? C30 H30C 0.96 . ? N3 Zn1 2.193(3) . ? N4 Zn1 2.134(4) . ? N1 Zn2 2.197(3) . ? N2 Zn2 2.129(4) . ? N5 O9 1.212(5) . ? N5 O8 1.214(5) . ? O1 Zn2 2.041(3) . ? O1 Zn1 2.043(3) . ? O5 Zn1 2.380(4) . ? O4 Zn2 2.323(3) . ? O2 Zn1 1.992(3) . ? O3 Zn2 2.076(3) . ? O6 Zn1 2.055(3) . ? O7 Zn2 1.997(3) . ? P1 F6' 1.420(12) . ? P1 F4' 1.499(12) . ? P1 F3' 1.499(11) . ? P1 F5 1.506(5) . ? P1 F1 1.534(5) . ? P1 F2 1.543(6) . ? P1 F3 1.562(5) . ? P1 F4 1.590(7) . ? P1 F1' 1.605(10) . ? P1 F6 1.611(6) . ? P1 F2' 1.628(11) . ? P1 F5' 1.704(11) . ? 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 C2 C1 C6 122.5(4) . . ? C2 C1 N5 118.5(4) . . ? C6 C1 N5 119.0(4) . . ? C1 C2 C3 119.7(4) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C2 C3 C4 118.9(4) . . ? C2 C3 C7 121.8(4) . . ? C4 C3 C7 119.3(4) . . ? O1 C4 C5 119.4(4) . . ? O1 C4 C3 120.0(3) . . ? C5 C4 C3 120.6(4) . . ? C6 C5 C4 119.2(4) . . ? C6 C5 C16 121.1(4) . . ? C4 C5 C16 119.7(4) . . ? C1 C6 C5 119.2(4) . . ? C1 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? N3 C7 C3 111.4(3) . . ? N3 C7 H7A 109.3 . . ? C3 C7 H7A 109.3 . . ? N3 C7 H7B 109.3 . . ? C3 C7 H7B 109.3 . . ? H7A C7 H7B 108 . . ? N3 C8 C9 114.8(4) . . ? N3 C8 H8A 108.6 . . ? C9 C8 H8A 108.6 . . ? N3 C8 H8B 108.6 . . ? C9 C8 H8B 108.6 . . ? H8A C8 H8B 107.5 . . ? O5 C9 C8 109.0(4) . . ? O5 C9 H9A 109.9 . . ? C8 C9 H9A 109.9 . . ? O5 C9 H9B 109.9 . . ? C8 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? N3 C10 C11 110.2(4) . . ? N3 C10 H10A 109.6 . . ? C11 C10 H10A 109.6 . . ? N3 C10 H10B 109.6 . . ? C11 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? N4 C11 C12 121.3(5) . . ? N4 C11 C10 115.3(4) . . ? C12 C11 C10 123.3(5) . . ? C11 C12 C13 119.6(6) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C14 C13 C12 117.8(5) . . ? C14 C13 H13 121.1 . . ? C12 C13 H13 121.1 . . ? C15 C14 C13 119.8(6) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? N4 C15 C14 122.1(5) . . ? N4 C15 H15 118.9 . . ? C14 C15 H15 118.9 . . ? N1 C16 C5 112.6(3) . . ? N1 C16 H16A 109.1 . . ? C5 C16 H16A 109.1 . . ? N1 C16 H16B 109.1 . . ? C5 C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? N1 C17 C18 113.7(3) . . ? N1 C17 H17A 108.8 . . ? C18 C17 H17A 108.8 . . ? N1 C17 H17B 108.8 . . ? C18 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? O4 C18 C17 107.9(4) . . ? O4 C18 H18A 110.1 . . ? C17 C18 H18A 110.1 . . ? O4 C18 H18B 110.1 . . ? C17 C18 H18B 110.1 . . ? H18A C18 H18B 108.4 . . ? O4 C19 H19A 109.5 . . ? O4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N1 C20 C21 109.8(3) . . ? N1 C20 H20A 109.7 . . ? C21 C20 H20A 109.7 . . ? N1 C20 H20B 109.7 . . ? C21 C20 H20B 109.7 . . ? H20A C20 H20B 108.2 . . ? N2 C21 C22 121.0(5) . . ? N2 C21 C20 115.4(4) . . ? C22 C21 C20 123.5(5) . . ? C21 C22 C23 119.2(5) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C24 C23 C22 119.5(5) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C23 C24 C25 118.0(5) . . ? C23 C24 H24 121 . . ? C25 C24 H24 121 . . ? N2 C25 C24 123.1(5) . . ? N2 C25 H25 118.4 . . ? C24 C25 H25 118.4 . . ? O3 C26 O2 126.0(4) . . ? O3 C26 C27 118.2(5) . . ? O2 C26 C27 115.8(5) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O6 C28 O7 126.4(4) . . ? O6 C28 C29 117.1(5) . . ? O7 C28 C29 116.6(5) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O5 C30 H30A 109.5 . . ? O5 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O5 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C10 N3 C7 109.9(3) . . ? C10 N3 C8 109.1(3) . . ? C7 N3 C8 112.6(4) . . ? C10 N3 Zn1 101.4(3) . . ? C7 N3 Zn1 109.4(2) . . ? C8 N3 Zn1 113.9(3) . . ? C15 N4 C11 119.3(4) . . ? C15 N4 Zn1 128.0(3) . . ? C11 N4 Zn1 112.7(3) . . ? C16 N1 C20 110.7(3) . . ? C16 N1 C17 113.4(4) . . ? C20 N1 C17 109.5(3) . . ? C16 N1 Zn2 108.1(2) . . ? C20 N1 Zn2 101.8(3) . . ? C17 N1 Zn2 112.7(3) . . ? C25 N2 C21 119.1(4) . . ? C25 N2 Zn2 127.5(3) . . ? C21 N2 Zn2 113.3(3) . . ? O9 N5 O8 121.9(4) . . ? O9 N5 C1 118.8(4) . . ? O8 N5 C1 119.2(4) . . ? C4 O1 Zn2 126.9(2) . . ? C4 O1 Zn1 123.2(2) . . ? Zn2 O1 Zn1 109.73(13) . . ? C30 O5 C9 110.6(5) . . ? C30 O5 Zn1 127.5(4) . . ? C9 O5 Zn1 112.8(3) . . ? C19 O4 C18 114.9(4) . . ? C19 O4 Zn2 123.6(3) . . ? C18 O4 Zn2 111.7(3) . . ? C26 O2 Zn1 132.4(3) . . ? C26 O3 Zn2 130.8(3) . . ? C28 O6 Zn1 129.1(3) . . ? C28 O7 Zn2 132.2(3) . . ? F6' P1 F4' 98.5(8) . . ? F6' P1 F3' 97.7(7) . . ? F4' P1 F3' 92.6(8) . . ? F6' P1 F5 171.9(9) . . ? F4' P1 F5 85.5(8) . . ? F3' P1 F5 89.1(7) . . ? F6' P1 F1 84.7(8) . . ? F4' P1 F1 45.6(7) . . ? F3' P1 F1 137.6(8) . . ? F5 P1 F1 93.2(4) . . ? F6' P1 F2 77.4(8) . . ? F4' P1 F2 136.6(8) . . ? F3' P1 F2 130.8(8) . . ? F5 P1 F2 94.9(4) . . ? F1 P1 F2 91.2(5) . . ? F6' P1 F3 91.7(8) . . ? F4' P1 F3 132.4(8) . . ? F3' P1 F3 39.9(5) . . ? F5 P1 F3 90.8(3) . . ? F1 P1 F3 175.3(5) . . ? F2 P1 F3 91.0(5) . . ? F6' P1 F4 95.0(9) . . ? F4' P1 F4 46.2(5) . . ? F3' P1 F4 47.1(7) . . ? F5 P1 F4 92.8(4) . . ? F1 P1 F4 90.5(5) . . ? F2 P1 F4 172.0(4) . . ? F3 P1 F4 86.8(5) . . ? F6' P1 F1' 92.1(7) . . ? F4' P1 F1' 90.2(8) . . ? F3' P1 F1' 169.3(8) . . ? F5 P1 F1' 80.8(7) . . ? F1 P1 F1' 47.5(5) . . ? F2 P1 F1' 47.5(6) . . ? F3 P1 F1' 135.9(7) . . ? F4 P1 F1' 136.4(7) . . ? F6' P1 F6 8.5(8) . . ? F4' P1 F6 95.3(7) . . ? F3' P1 F6 90.0(7) . . ? F5 P1 F6 178.8(4) . . ? F1 P1 F6 88.0(3) . . ? F2 P1 F6 85.2(3) . . ? F3 P1 F6 88.0(3) . . ? F4 P1 F6 87.1(4) . . ? F1' P1 F6 100.1(6) . . ? F6' P1 F2' 89.0(7) . . ? F4' P1 F2' 171.9(8) . . ? F3' P1 F2' 89.6(8) . . ? F5 P1 F2' 86.7(8) . . ? F1 P1 F2' 132.8(7) . . ? F2 P1 F2' 42.0(5) . . ? F3 P1 F2' 49.9(6) . . ? F4 P1 F2' 136.7(7) . . ? F1' P1 F2' 86.3(7) . . ? F6 P1 F2' 92.5(7) . . ? F6' P1 F5' 171.7(8) . . ? F4' P1 F5' 88.6(6) . . ? F3' P1 F5' 86.1(6) . . ? F5 P1 F5' 4.3(7) . . ? F1 P1 F5' 97.5(6) . . ? F2 P1 F5' 94.6(5) . . ? F3 P1 F5' 86.5(6) . . ? F4 P1 F5' 92.9(6) . . ? F1' P1 F5' 83.6(6) . . ? F6 P1 F5' 174.5(6) . . ? F2' P1 F5' 83.7(6) . . ? O2 Zn1 O1 98.64(13) . . ? O2 Zn1 O6 101.96(15) . . ? O1 Zn1 O6 91.30(13) . . ? O2 Zn1 N4 94.21(15) . . ? O1 Zn1 N4 167.04(13) . . ? O6 Zn1 N4 87.59(14) . . ? O2 Zn1 N3 158.99(15) . . ? O1 Zn1 N3 89.11(11) . . ? O6 Zn1 N3 97.32(14) . . ? N4 Zn1 N3 78.24(13) . . ? O2 Zn1 O5 85.93(14) . . ? O1 Zn1 O5 91.72(13) . . ? O6 Zn1 O5 171.03(13) . . ? N4 Zn1 O5 87.57(14) . . ? N3 Zn1 O5 74.28(13) . . ? O7 Zn2 O1 98.56(12) . . ? O7 Zn2 O3 99.58(15) . . ? O1 Zn2 O3 92.03(13) . . ? O7 Zn2 N2 94.27(15) . . ? O1 Zn2 N2 166.63(13) . . ? O3 Zn2 N2 89.51(13) . . ? O7 Zn2 N1 164.23(14) . . ? O1 Zn2 N1 88.77(11) . . ? O3 Zn2 N1 94.07(14) . . ? N2 Zn2 N1 77.88(14) . . ? O7 Zn2 O4 90.13(13) . . ? O1 Zn2 O4 93.56(12) . . ? O3 Zn2 O4 167.95(12) . . ? N2 Zn2 O4 82.63(12) . . ? N1 Zn2 O4 75.41(12) . . ? #===END #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2011-06-15 at 18:02:06 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : 478ld10 478 struct data_478ld10 _database_code_depnum_ccdc_archive 'CCDC 830844' #TrackingRef 'supdata.cif' _audit_creation_date 2011-06-15T18:02:06-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C66 H80 N10 O20 P2 Zn4, 2(F6 P)' _chemical_formula_sum 'C66 H80 F12 N10 O20 P4 Zn4' _chemical_formula_weight 1946.76 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 26.602(2) _cell_length_b 14.3664(7) _cell_length_c 23.0070(10) _cell_angle_alpha 90 _cell_angle_beta 107.464(6) _cell_angle_gamma 90 _cell_volume 8387.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5896 _cell_measurement_theta_min 3.0293 _cell_measurement_theta_max 62.6444 _cell_measurement_wavelength 1.5418 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3976 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.883 _exptl_absorpt_correction_type multi-scan _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_absorpt_correction_T_min 0.92513 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 16.0696 _diffrn_orient_matrix_ub_11 0.0606512 _diffrn_orient_matrix_ub_12 0.0026321 _diffrn_orient_matrix_ub_13 0.0226722 _diffrn_orient_matrix_ub_21 0.0020706 _diffrn_orient_matrix_ub_22 -0.0778594 _diffrn_orient_matrix_ub_23 -0.0452743 _diffrn_orient_matrix_ub_31 0.0001147 _diffrn_orient_matrix_ub_32 0.0736749 _diffrn_orient_matrix_ub_33 -0.0486545 _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0592 _diffrn_reflns_av_unetI/netI 0.0723 _diffrn_reflns_number 42499 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.48 _diffrn_reflns_theta_max 62.5 _diffrn_reflns_theta_full 62.5 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _reflns_number_total 13255 _reflns_number_gt 5930 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0791P)^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_number_reflns 13255 _refine_ls_number_parameters 1095 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1089 _refine_ls_R_factor_gt 0.05 _refine_ls_wR_factor_ref 0.1415 _refine_ls_wR_factor_gt 0.1248 _refine_ls_goodness_of_fit_ref 0.816 _refine_ls_restrained_S_all 0.816 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.684 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.054 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.0157(3) 0.6557(6) 0.3160(4) 0.174(4) Uani 1 1 d . . . H1A H -0.0034 0.593 0.3161 0.261 Uiso 1 1 calc R . . H1B H -0.0421 0.6683 0.278 0.261 Uiso 1 1 calc R . . H1C H -0.0307 0.6636 0.3488 0.261 Uiso 1 1 calc R . . C2 C 0.0302(4) 0.7229(6) 0.3243(3) 0.118(2) Uani 1 1 d . . . C3 C 0.0805(4) 0.6873(5) 0.3315(3) 0.116(2) Uani 1 1 d . . . H3 H 0.0853 0.6233 0.3305 0.139 Uiso 1 1 calc R . . C4 C 0.1242(3) 0.7473(5) 0.3401(3) 0.0935(18) Uani 1 1 d . . . C5 C 0.1174(3) 0.8447(4) 0.3408(2) 0.0822(16) Uani 1 1 d . . . C6 C 0.0666(3) 0.8783(4) 0.3346(3) 0.0867(17) Uani 1 1 d . . . C7 C 0.0237(3) 0.8187(6) 0.3257(3) 0.113(2) Uani 1 1 d . . . H7 H -0.0097 0.8433 0.3205 0.135 Uiso 1 1 calc R . . C8 C 0.1784(3) 0.7104(4) 0.3474(3) 0.104(2) Uani 1 1 d . . . H8A H 0.1786 0.6436 0.354 0.125 Uiso 1 1 calc R . . H8B H 0.2029 0.7383 0.3832 0.125 Uiso 1 1 calc R . . C9 C 0.2493(3) 0.6861(4) 0.3011(3) 0.116(2) Uani 1 1 d . . . H9A H 0.2452 0.619 0.301 0.139 Uiso 1 1 calc R . . H9B H 0.2725 0.7038 0.3408 0.139 Uiso 1 1 calc R . . C10 C 0.2756(3) 0.7125(5) 0.2525(3) 0.126(3) Uani 1 1 d . . . C11 C 0.2939(3) 0.8424(5) 0.2019(3) 0.142(3) Uani 1 1 d . . . H11A H 0.2893 0.9085 0.197 0.212 Uiso 1 1 calc R . . H11B H 0.2777 0.8122 0.1637 0.212 Uiso 1 1 calc R . . H11C H 0.3309 0.8281 0.2153 0.212 Uiso 1 1 calc R . . C12 C 0.1579(3) 0.6967(4) 0.2362(3) 0.102(2) Uani 1 1 d . . . H12A H 0.1384 0.645 0.246 0.123 Uiso 1 1 calc R . . H12B H 0.1766 0.6738 0.2088 0.123 Uiso 1 1 calc R . . C13 C 0.1199(3) 0.7703(5) 0.2043(2) 0.0887(17) Uani 1 1 d . . . C14 C 0.0715(3) 0.7485(5) 0.1657(3) 0.116(2) Uani 1 1 d . . . H14 H 0.0606 0.6868 0.1603 0.139 Uiso 1 1 calc R . . C15 C 0.0395(3) 0.8168(6) 0.1355(3) 0.131(3) Uani 1 1 d . . . H15 H 0.0064 0.8027 0.1091 0.157 Uiso 1 1 calc R . . C16 C 0.0566(3) 0.9085(5) 0.1442(3) 0.110(2) Uani 1 1 d . . . H16 H 0.0355 0.957 0.1236 0.133 Uiso 1 1 calc R . . C17 C 0.1046(3) 0.9249(4) 0.1835(3) 0.0932(18) Uani 1 1 d . . . H17 H 0.1162 0.9861 0.1901 0.112 Uiso 1 1 calc R . . C18 C 0.0567(2) 0.9810(4) 0.3353(3) 0.0938(18) Uani 1 1 d . . . H18A H 0.0695 1.011 0.3047 0.113 Uiso 1 1 calc R . . H18B H 0.0191 0.9921 0.3249 0.113 Uiso 1 1 calc R . . C19 C 0.0711(3) 1.1252(4) 0.3958(3) 0.1016(19) Uani 1 1 d . . . H19B H 0.0765 1.1534 0.3598 0.122 Uiso 1 1 calc R . . H19D H 0.0343 1.1329 0.3933 0.122 Uiso 1 1 calc R . . C20 C 0.1045(3) 1.1749(4) 0.4512(3) 0.104(2) Uani 1 1 d . . . H20B H 0.1013 1.2416 0.4448 0.125 Uiso 1 1 calc R . . H20D H 0.0927 1.1596 0.4861 0.125 Uiso 1 1 calc R . . C21 C 0.1916(3) 1.1919(5) 0.5149(3) 0.117(2) Uani 1 1 d . . . H21A H 0.2271 1.1711 0.521 0.175 Uiso 1 1 calc R . . H21B H 0.1809 1.1762 0.55 0.175 Uiso 1 1 calc R . . H21C H 0.1898 1.2582 0.5093 0.175 Uiso 1 1 calc R . . C22 C 0.0664(3) 0.9734(4) 0.4444(3) 0.1021(19) Uani 1 1 d . . . H22A H 0.0312 0.9486 0.4264 0.123 Uiso 1 1 calc R . . H22B H 0.0649 1.0174 0.4758 0.123 Uiso 1 1 calc R . . C23 C 0.1032(3) 0.8953(5) 0.4727(3) 0.0892(17) Uani 1 1 d . . . C24 C 0.0853(3) 0.8189(6) 0.4970(4) 0.122(2) Uani 1 1 d . . . H24 H 0.0497 0.8129 0.4937 0.147 Uiso 1 1 calc R . . C25 C 0.1205(4) 0.7524(6) 0.5258(4) 0.142(3) Uani 1 1 d . . . H25 H 0.1097 0.6999 0.5425 0.17 Uiso 1 1 calc R . . C26 C 0.1732(4) 0.7656(5) 0.5296(3) 0.130(3) Uani 1 1 d . . . H26 H 0.1983 0.7221 0.5495 0.156 Uiso 1 1 calc R . . C27 C 0.1877(3) 0.8422(5) 0.5039(3) 0.0978(19) Uani 1 1 d . . . H27 H 0.2229 0.8493 0.5056 0.117 Uiso 1 1 calc R . . C28 C 0.5250(3) 1.4688(7) 0.3896(5) 0.229(6) Uani 1 1 d . . . H28A H 0.5438 1.4504 0.3619 0.343 Uiso 1 1 calc R . . H28B H 0.5485 1.469 0.4305 0.343 Uiso 1 1 calc R . . H28C H 0.5107 1.5301 0.3793 0.343 Uiso 1 1 calc R . . C29 C 0.4795(4) 1.3992(8) 0.3853(6) 0.159(4) Uani 1 1 d . . . C30 C 0.4458(4) 1.4072(6) 0.4184(5) 0.138(3) Uani 1 1 d . . . H30 H 0.4498 1.4559 0.4461 0.166 Uiso 1 1 calc R . . C31 C 0.4041(3) 1.3426(6) 0.4119(4) 0.115(2) Uani 1 1 d . . . C32 C 0.3971(3) 1.2698(5) 0.3723(3) 0.0954(19) Uani 1 1 d . . . C33 C 0.4321(3) 1.2607(6) 0.3390(4) 0.118(2) Uani 1 1 d . . . C34 C 0.4739(3) 1.3269(7) 0.3445(4) 0.134(3) Uani 1 1 d . . . H34 H 0.4966 1.321 0.3208 0.161 Uiso 1 1 calc R . . C35 C 0.3652(3) 1.3549(5) 0.4469(3) 0.123(3) Uani 1 1 d . . . H35A H 0.364 1.2986 0.4698 0.148 Uiso 1 1 calc R . . H35B H 0.3765 1.4056 0.4757 0.148 Uiso 1 1 calc R . . C36 C 0.3103(3) 1.4600(4) 0.3663(4) 0.122(3) Uani 1 1 d . . . H36A H 0.2767 1.4908 0.3608 0.147 Uiso 1 1 calc R . . H36B H 0.3376 1.5025 0.3886 0.147 Uiso 1 1 calc R . . C37 C 0.3168(4) 1.4457(6) 0.3064(4) 0.142(3) Uani 1 1 d . . . H37A H 0.3029 1.4987 0.2804 0.171 Uiso 1 1 calc R . . H37B H 0.3538 1.4392 0.3099 0.171 Uiso 1 1 calc R . . C38 C 0.2840(3) 1.3474(7) 0.2203(4) 0.166(4) Uani 1 1 d . . . H38A H 0.2649 1.2906 0.2073 0.248 Uiso 1 1 calc R . . H38B H 0.3184 1.3424 0.2151 0.248 Uiso 1 1 calc R . . H38C H 0.2653 1.3983 0.1962 0.248 Uiso 1 1 calc R . . C39 C 0.2746(4) 1.3838(5) 0.4417(3) 0.121(2) Uani 1 1 d . . . H39A H 0.28 1.333 0.4707 0.145 Uiso 1 1 calc R . . H39B H 0.2809 1.4418 0.4644 0.145 Uiso 1 1 calc R . . C40 C 0.2199(4) 1.3819(6) 0.4012(4) 0.112(2) Uani 1 1 d . . . C41 C 0.1800(6) 1.4319(6) 0.4103(5) 0.157(3) Uani 1 1 d . . . H41 H 0.1858 1.4742 0.4422 0.188 Uiso 1 1 calc R . . C42 C 0.1279(5) 1.4173(9) 0.3686(7) 0.180(5) Uani 1 1 d . . . H42 H 0.0989 1.4472 0.3746 0.216 Uiso 1 1 calc R . . C43 C 0.1220(5) 1.3590(8) 0.3204(5) 0.160(4) Uani 1 1 d . . . H43 H 0.0887 1.3484 0.2933 0.192 Uiso 1 1 calc R . . C44 C 0.1630(4) 1.3181(5) 0.3123(4) 0.114(3) Uani 1 1 d . . . H44 H 0.1591 1.284 0.2769 0.137 Uiso 1 1 calc R . . C45 C 0.4268(3) 1.1803(6) 0.2961(3) 0.114(2) Uani 1 1 d . . . H45A H 0.4521 1.1869 0.2736 0.137 Uiso 1 1 calc R . . H45B H 0.3918 1.1803 0.2671 0.137 Uiso 1 1 calc R . . C46 C 0.4895(2) 1.0847(5) 0.3755(3) 0.114(2) Uani 1 1 d . . . H46A H 0.514 1.1152 0.3578 0.137 Uiso 1 1 calc R . . H46B H 0.4999 1.0199 0.3817 0.137 Uiso 1 1 calc R . . C47 C 0.4954(3) 1.1287(5) 0.4379(4) 0.130(3) Uani 1 1 d . . . H47A H 0.5287 1.1111 0.4671 0.156 Uiso 1 1 calc R . . H47B H 0.4935 1.196 0.435 0.156 Uiso 1 1 calc R . . C48 C 0.4521(3) 1.1248(6) 0.5135(3) 0.159(3) Uani 1 1 d . . . H48A H 0.4231 1.0994 0.5251 0.238 Uiso 1 1 calc R . . H48B H 0.4494 1.1915 0.512 0.238 Uiso 1 1 calc R . . H48C H 0.4847 1.107 0.5427 0.238 Uiso 1 1 calc R . . C49 C 0.4278(3) 1.0102(7) 0.2890(4) 0.132(3) Uani 1 1 d . . . H49A H 0.4565 1.0054 0.2714 0.158 Uiso 1 1 calc R . . H49B H 0.3952 1.018 0.2562 0.158 Uiso 1 1 calc R . . C50 C 0.4251(3) 0.9234(7) 0.3256(4) 0.135(3) Uani 1 1 d . . . C51 C 0.4477(6) 0.8455(9) 0.3112(5) 0.196(6) Uani 1 1 d . . . H51 H 0.4654 0.8445 0.2819 0.235 Uiso 1 1 calc R . . C52 C 0.4421(4) 0.7675(10) 0.3443(6) 0.197(6) Uani 1 1 d . . . H52 H 0.4556 0.7111 0.3358 0.236 Uiso 1 1 calc R . . C53 C 0.4158(3) 0.7698(6) 0.3925(5) 0.146(3) Uani 1 1 d . . . H53 H 0.4123 0.7169 0.4143 0.175 Uiso 1 1 calc R . . C54 C 0.3963(3) 0.8568(6) 0.4032(4) 0.122(2) Uani 1 1 d . . . H54 H 0.3802 0.8631 0.4337 0.147 Uiso 1 1 calc R . . C55 C 0.2080(3) 1.0803(5) 0.1462(2) 0.0838(16) Uani 1 1 d . . . C56 C 0.1998(3) 1.0176(5) 0.0989(3) 0.113(2) Uani 1 1 d . . . H56 H 0.2257 0.9748 0.0976 0.136 Uiso 1 1 calc R . . C57 C 0.1517(4) 1.0202(6) 0.0529(3) 0.125(3) Uani 1 1 d . . . H57 H 0.1447 0.9774 0.0212 0.15 Uiso 1 1 calc R . . C58 C 0.1159(3) 1.0835(7) 0.0544(3) 0.116(3) Uani 1 1 d . . . C59 C 0.1238(3) 1.1475(5) 0.0994(3) 0.108(2) Uani 1 1 d . . . H59 H 0.0981 1.1917 0.0991 0.129 Uiso 1 1 calc R . . C60 C 0.1713(3) 1.1456(5) 0.1462(3) 0.0919(18) Uani 1 1 d . . . H60 H 0.1778 1.1892 0.1774 0.11 Uiso 1 1 calc R . . C61 C 0.3392(2) 1.0630(5) 0.5671(2) 0.0857(17) Uani 1 1 d . . . C62 C 0.3388(3) 0.9675(5) 0.5654(3) 0.104(2) Uani 1 1 d . . . H62 H 0.3205 0.9362 0.53 0.125 Uiso 1 1 calc R . . C63 C 0.3663(3) 0.9176(5) 0.6174(3) 0.112(2) Uani 1 1 d . . . H63 H 0.3673 0.8529 0.6167 0.134 Uiso 1 1 calc R . . C64 C 0.3913(3) 0.9646(6) 0.6686(3) 0.110(2) Uani 1 1 d . . . C65 C 0.3938(3) 1.0588(6) 0.6702(3) 0.118(2) Uani 1 1 d . . . H65 H 0.4134 1.0891 0.7055 0.142 Uiso 1 1 calc R . . C66 C 0.3668(3) 1.1100(5) 0.6189(3) 0.104(2) Uani 1 1 d . . . H66 H 0.3674 1.1747 0.6197 0.124 Uiso 1 1 calc R . . N1A N 0.08350(19) 1.0230(3) 0.3963(2) 0.0924(14) Uani 1 1 d . . . N1B N 0.4362(2) 1.0890(4) 0.3307(2) 0.1050(16) Uani 1 1 d . . . N2A N 0.1538(2) 0.9064(3) 0.4768(2) 0.0838(13) Uani 1 1 d . . . N2B N 0.4009(2) 0.9309(4) 0.3698(3) 0.1128(18) Uani 1 1 d . . . N3A N 0.1966(2) 0.7302(3) 0.2926(2) 0.0931(14) Uani 1 1 d . . . N3B N 0.3120(2) 1.3752(3) 0.4055(2) 0.1029(16) Uani 1 1 d . . . N4A N 0.13623(18) 0.8576(3) 0.21309(19) 0.0811(13) Uani 1 1 d . . . N4B N 0.2101(2) 1.3236(4) 0.3529(3) 0.0979(16) Uani 1 1 d . . . N9 N 0.4201(3) 0.9120(7) 0.7237(3) 0.148(3) Uani 1 1 d . . . N10 N 0.0647(4) 1.0804(7) 0.0032(5) 0.159(4) Uani 1 1 d . . . O1A O 0.15843(15) 0.9017(2) 0.34790(15) 0.0768(10) Uani 1 1 d . . . O1B O 0.35774(16) 1.2064(3) 0.36598(17) 0.0903(11) Uani 1 1 d . . . O2A O 0.24661(14) 1.0096(2) 0.44791(14) 0.0782(10) Uani 1 1 d . . . O2B O 0.33435(14) 1.0363(2) 0.43199(15) 0.0809(10) Uani 1 1 d . . . O3A O 0.27120(14) 0.8811(2) 0.36306(15) 0.0867(11) Uani 1 1 d . . . H19A H 0.2962 0.9228 0.3543 0.13 Uiso 1 1 d R . . H19C H 0.2628 0.9024 0.3986 0.13 Uiso 1 1 d R . . O3B O 0.26779(14) 1.1691(2) 0.41549(14) 0.0790(10) Uani 1 1 d . . . O4A O 0.15718(18) 1.1475(3) 0.46209(18) 0.0969(12) Uani 1 1 d . . . O4B O 0.45054(18) 1.0905(3) 0.4553(2) 0.1165(14) Uani 1 1 d . . . O5A O 0.27038(19) 0.8108(3) 0.24561(19) 0.1192(15) Uani 1 1 d . . . O5B O 0.28885(18) 1.3629(3) 0.2804(2) 0.1138(14) Uani 1 1 d . . . O6A O 0.21311(15) 1.0111(2) 0.26697(14) 0.0820(10) Uani 1 1 d . . . O6B O 0.24737(14) 1.1729(2) 0.27904(15) 0.0842(10) Uani 1 1 d . . . O7A O 0.16647(14) 1.1037(2) 0.34488(15) 0.0831(10) Uani 1 1 d . . . H20A H 0.1911 1.1526 0.3616 0.125 Uiso 1 1 d R . . H20C H 0.1761 1.0735 0.3125 0.125 Uiso 1 1 d R . . O7B O 0.31154(14) 1.0371(3) 0.29462(15) 0.0891(11) Uani 1 1 d . . . O8 O 0.25562(15) 1.0741(3) 0.19155(15) 0.0897(11) Uani 1 1 d . . . O9 O 0.31363(15) 1.1174(2) 0.51855(15) 0.0862(11) Uani 1 1 d . . . O10 O 0.0328(3) 1.1391(6) 0.0085(3) 0.190(3) Uani 1 1 d . . . O11 O 0.0572(4) 1.0274(7) -0.0366(3) 0.236(5) Uani 1 1 d . . . O12 O 0.4414(4) 0.9511(6) 0.7673(3) 0.258(5) Uani 1 1 d . . . O13 O 0.4256(3) 0.8293(6) 0.7185(3) 0.197(3) Uani 1 1 d . . . P3 P 0.11619(9) 0.45204(14) 0.14396(9) 0.1115(6) Uani 1 1 d . . . F1 F 0.0636(4) 0.4113(9) 0.0949(4) 0.223(6) Uani 0.637(14) 1 d PD A 1 F2 F 0.1286(6) 0.3544(5) 0.1660(4) 0.205(7) Uani 0.637(14) 1 d PD A 1 F3 F 0.0834(4) 0.4747(9) 0.1892(5) 0.190(5) Uani 0.637(14) 1 d PD A 1 F4 F 0.0986(8) 0.5511(7) 0.1178(5) 0.284(8) Uani 0.637(14) 1 d PD A 1 F5 F 0.1441(5) 0.4418(9) 0.0928(5) 0.214(6) Uani 0.637(14) 1 d PD A 1 F6 F 0.1614(5) 0.4836(10) 0.1978(7) 0.283(11) Uani 0.637(14) 1 d PD A 1 F1' F 0.0795(6) 0.4228(9) 0.0843(6) 0.134(7) Uiso 0.363(14) 1 d PD A 2 F2' F 0.1599(4) 0.3921(9) 0.1316(7) 0.135(6) Uiso 0.363(14) 1 d PD A 2 F3' F 0.1345(5) 0.5427(8) 0.1246(6) 0.115(6) Uiso 0.363(14) 1 d PD A 2 F4' F 0.0746(5) 0.5055(9) 0.1634(7) 0.120(6) Uiso 0.363(14) 1 d PD A 2 F5' F 0.0978(5) 0.3611(10) 0.1761(7) 0.130(6) Uiso 0.363(14) 1 d PD A 2 F6' F 0.1640(5) 0.4791(8) 0.2059(5) 0.121(6) Uiso 0.363(14) 1 d PD A 2 P4 P 0.32585(10) 0.66345(16) 0.51971(11) 0.1304(7) Uani 1 1 d . . . F7 F 0.2708(3) 0.6256(5) 0.4770(5) 0.205(4) Uani 0.777(11) 1 d PD B 1 F8 F 0.3520(5) 0.6284(8) 0.4729(6) 0.285(7) Uani 0.777(11) 1 d PD B 1 F9 F 0.3329(5) 0.5724(6) 0.5519(6) 0.278(6) Uani 0.777(11) 1 d PD B 1 F10 F 0.3018(3) 0.7108(7) 0.5660(3) 0.221(5) Uani 0.777(11) 1 d PD B 1 F11 F 0.3131(4) 0.7568(5) 0.4834(4) 0.230(5) Uani 0.777(11) 1 d PD B 1 F12 F 0.3782(3) 0.7091(7) 0.5551(6) 0.232(5) Uani 0.777(11) 1 d PD B 1 F7' F 0.2768(6) 0.6086(12) 0.5258(11) 0.134(9) Uiso 0.223(11) 1 d PD B 2 F8' F 0.3078(8) 0.6621(15) 0.4531(6) 0.153(11) Uiso 0.223(11) 1 d PD B 2 F9' F 0.3003(6) 0.7508(10) 0.5269(11) 0.136(9) Uiso 0.223(11) 1 d PD B 2 F10' F 0.3559(7) 0.6574(13) 0.5927(5) 0.120(8) Uiso 0.223(11) 1 d PD B 2 F11' F 0.3534(6) 0.5663(10) 0.5191(8) 0.101(7) Uiso 0.223(11) 1 d PD B 2 F12' F 0.3804(6) 0.7043(16) 0.5189(10) 0.136(10) Uiso 0.223(11) 1 d PD B 2 P1 P 0.25768(6) 1.07472(11) 0.26357(6) 0.0799(4) Uani 1 1 d . . . P2 P 0.28903(6) 1.08067(10) 0.44816(6) 0.0741(4) Uani 1 1 d . . . Zn1 Zn 0.20286(3) 0.87940(5) 0.28942(3) 0.0807(2) Uani 1 1 d . . . Zn2 Zn 0.16758(3) 1.00530(5) 0.41439(3) 0.0771(2) Uani 1 1 d . . . Zn3 Zn 0.28212(3) 1.25447(5) 0.34905(3) 0.0821(2) Uani 1 1 d . . . Zn4 Zn 0.37229(3) 1.06870(5) 0.37205(3) 0.0843(2) 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 C1 0.167(8) 0.144(7) 0.219(10) -0.021(7) 0.071(7) -0.062(7) C2 0.120(7) 0.122(7) 0.111(5) -0.008(5) 0.033(5) -0.040(6) C3 0.137(7) 0.094(5) 0.111(5) 0.005(4) 0.029(5) -0.030(6) C4 0.100(5) 0.092(5) 0.079(4) 0.013(3) 0.012(3) 0.003(5) C5 0.098(5) 0.076(5) 0.064(4) -0.002(3) 0.011(3) 0.003(4) C6 0.089(5) 0.081(4) 0.079(4) -0.006(3) 0.009(3) -0.007(4) C7 0.117(6) 0.103(6) 0.108(5) -0.012(4) 0.017(4) -0.016(5) C8 0.137(6) 0.080(4) 0.084(5) 0.017(3) 0.017(4) 0.016(4) C9 0.120(6) 0.077(4) 0.128(6) 0.000(4) 0.004(5) 0.038(4) C10 0.178(8) 0.097(6) 0.118(6) 0.016(5) 0.066(6) 0.025(5) C11 0.195(8) 0.149(7) 0.091(5) 0.024(5) 0.059(6) 0.043(6) C12 0.118(5) 0.077(4) 0.098(5) -0.011(4) 0.011(4) 0.010(4) C13 0.105(5) 0.082(5) 0.064(4) -0.004(3) 0.002(3) 0.005(4) C14 0.104(5) 0.088(5) 0.127(6) 0.006(4) -0.006(5) -0.009(4) C15 0.108(6) 0.110(6) 0.130(6) 0.005(5) -0.030(4) -0.006(5) C16 0.095(5) 0.097(5) 0.116(6) 0.018(4) -0.003(4) 0.006(4) C17 0.102(5) 0.088(5) 0.076(4) 0.002(3) 0.006(4) 0.001(4) C18 0.093(4) 0.096(5) 0.085(4) -0.002(4) 0.015(3) 0.004(4) C19 0.099(5) 0.083(5) 0.120(5) 0.012(4) 0.030(4) 0.026(4) C20 0.115(6) 0.081(4) 0.120(6) -0.005(4) 0.040(4) 0.015(4) C21 0.128(6) 0.116(6) 0.110(5) -0.025(5) 0.041(5) 0.005(5) C22 0.105(5) 0.097(5) 0.105(5) -0.001(4) 0.032(4) 0.008(4) C23 0.110(6) 0.084(5) 0.077(4) -0.001(3) 0.033(4) 0.002(4) C24 0.148(7) 0.095(6) 0.145(7) 0.002(5) 0.075(6) 0.000(5) C25 0.184(9) 0.097(6) 0.160(8) 0.025(5) 0.076(7) 0.008(7) C26 0.158(8) 0.104(6) 0.131(6) 0.045(5) 0.047(6) 0.028(6) C27 0.114(5) 0.086(5) 0.088(4) 0.024(4) 0.021(4) 0.014(4) C28 0.122(7) 0.195(10) 0.311(14) 0.090(10) -0.026(8) -0.071(7) C29 0.117(8) 0.128(9) 0.190(12) 0.038(8) -0.017(7) -0.003(8) C30 0.110(7) 0.104(6) 0.166(9) 0.008(6) -0.013(6) -0.009(6) C31 0.106(6) 0.087(5) 0.125(6) 0.003(5) -0.005(5) 0.008(5) C32 0.090(5) 0.099(6) 0.090(5) 0.016(4) 0.015(4) 0.023(5) C33 0.108(6) 0.101(6) 0.119(6) 0.030(5) -0.004(5) 0.017(5) C34 0.098(6) 0.123(7) 0.160(8) 0.055(6) 0.007(5) -0.001(6) C35 0.136(7) 0.087(5) 0.111(6) -0.017(4) -0.017(5) 0.010(5) C36 0.126(6) 0.059(4) 0.164(7) 0.029(5) 0.016(5) 0.013(4) C37 0.176(8) 0.135(8) 0.119(7) 0.003(6) 0.050(6) 0.012(7) C38 0.157(8) 0.225(11) 0.108(7) -0.007(7) 0.031(6) -0.013(7) C39 0.159(8) 0.077(5) 0.111(6) -0.007(4) 0.017(6) 0.005(5) C40 0.132(7) 0.084(5) 0.125(7) 0.029(5) 0.047(6) 0.039(5) C41 0.204(11) 0.122(7) 0.157(9) 0.005(6) 0.074(9) 0.030(8) C42 0.161(11) 0.166(11) 0.238(14) 0.106(10) 0.100(11) 0.077(9) C43 0.198(13) 0.150(9) 0.123(8) 0.011(6) 0.035(8) 0.008(8) C44 0.116(6) 0.113(6) 0.121(6) 0.045(5) 0.045(6) 0.044(5) C45 0.103(5) 0.143(7) 0.094(5) 0.050(5) 0.028(4) 0.014(5) C46 0.075(4) 0.147(6) 0.112(6) 0.036(5) 0.015(4) 0.025(4) C47 0.110(6) 0.150(7) 0.124(7) 0.026(5) 0.026(5) 0.028(5) C48 0.194(9) 0.202(9) 0.072(5) -0.024(5) 0.028(5) 0.015(7) C49 0.136(7) 0.163(8) 0.105(6) 0.024(6) 0.051(5) 0.026(6) C50 0.137(7) 0.129(8) 0.126(7) -0.020(6) 0.018(6) 0.037(6) C51 0.292(16) 0.159(11) 0.135(9) -0.015(8) 0.060(9) 0.005(11) C52 0.166(9) 0.248(16) 0.169(10) -0.099(10) 0.039(8) 0.065(10) C53 0.148(7) 0.090(6) 0.175(9) 0.003(6) 0.013(6) 0.013(5) C54 0.117(6) 0.104(6) 0.139(7) 0.026(5) 0.027(5) 0.020(5) C55 0.096(5) 0.094(4) 0.055(4) 0.013(3) 0.013(3) 0.004(4) C56 0.151(7) 0.110(5) 0.065(4) 0.000(4) 0.011(4) 0.011(5) C57 0.174(9) 0.112(6) 0.073(5) -0.006(4) 0.013(5) -0.017(6) C58 0.129(7) 0.117(7) 0.074(5) 0.020(5) -0.010(5) -0.031(5) C59 0.099(5) 0.122(6) 0.092(5) 0.030(5) 0.012(4) -0.009(4) C60 0.085(4) 0.112(5) 0.066(4) 0.016(3) 0.005(3) -0.001(4) C61 0.099(4) 0.094(5) 0.057(4) 0.000(3) 0.013(3) 0.011(4) C62 0.124(5) 0.096(5) 0.069(4) 0.007(4) -0.006(4) 0.005(4) C63 0.128(6) 0.109(5) 0.084(5) 0.025(4) 0.009(4) 0.005(4) C64 0.114(5) 0.138(7) 0.066(5) 0.008(5) 0.009(4) 0.020(5) C65 0.127(6) 0.147(7) 0.063(4) -0.020(5) 0.001(4) 0.011(5) C66 0.123(5) 0.108(5) 0.069(4) -0.011(4) 0.012(4) 0.010(4) N1A 0.101(4) 0.084(4) 0.092(4) 0.007(3) 0.031(3) 0.018(3) N1B 0.107(4) 0.121(5) 0.088(4) 0.010(4) 0.030(3) 0.018(3) N2A 0.099(4) 0.080(3) 0.071(3) 0.011(2) 0.023(3) 0.007(3) N2B 0.114(4) 0.118(5) 0.113(4) 0.025(4) 0.044(4) 0.039(4) N3A 0.117(4) 0.071(3) 0.074(3) 0.002(3) 0.001(3) 0.019(3) N3B 0.109(4) 0.083(4) 0.101(4) 0.002(3) 0.009(4) 0.012(3) N4A 0.097(3) 0.074(3) 0.060(3) 0.000(2) 0.006(2) 0.007(3) N4B 0.110(5) 0.074(3) 0.094(4) 0.012(3) 0.007(4) 0.025(3) N9 0.190(7) 0.159(7) 0.071(5) 0.023(5) 0.004(4) 0.036(6) N10 0.125(7) 0.185(10) 0.142(8) 0.057(7) 0.001(7) 0.005(6) O1A 0.087(3) 0.068(2) 0.068(2) 0.0001(18) 0.0130(19) 0.003(2) O1B 0.087(3) 0.075(3) 0.098(3) 0.010(2) 0.012(2) 0.004(2) O2A 0.087(2) 0.075(2) 0.061(2) 0.0035(18) 0.0051(17) 0.008(2) O2B 0.087(3) 0.079(2) 0.074(2) 0.0137(19) 0.0214(19) 0.024(2) O3A 0.090(3) 0.090(3) 0.069(2) -0.0006(19) 0.0058(19) 0.015(2) O3B 0.092(3) 0.068(2) 0.069(2) 0.0101(18) 0.0113(19) 0.0126(19) O4A 0.100(3) 0.094(3) 0.096(3) -0.014(2) 0.026(2) 0.014(3) O4B 0.101(3) 0.131(4) 0.107(4) 0.008(3) 0.015(3) -0.002(3) O5A 0.163(4) 0.108(4) 0.088(3) 0.006(3) 0.039(3) 0.027(3) O5B 0.116(4) 0.111(4) 0.106(4) 0.018(3) 0.019(3) 0.003(3) O6A 0.101(3) 0.075(2) 0.060(2) 0.0052(18) 0.0096(19) 0.004(2) O6B 0.098(3) 0.075(2) 0.069(2) 0.0077(19) 0.010(2) 0.013(2) O7A 0.100(3) 0.074(2) 0.070(2) 0.0112(18) 0.018(2) 0.011(2) O7B 0.088(3) 0.096(3) 0.071(2) 0.001(2) 0.005(2) 0.019(2) O8 0.091(3) 0.114(3) 0.059(2) 0.011(2) 0.013(2) 0.013(2) O9 0.108(3) 0.077(2) 0.060(2) 0.0012(19) 0.004(2) 0.008(2) O10 0.145(6) 0.250(9) 0.127(5) 0.021(5) -0.032(5) -0.043(6) O11 0.245(9) 0.289(11) 0.112(5) -0.027(6) -0.043(5) -0.067(8) O12 0.355(11) 0.241(8) 0.086(4) -0.006(5) -0.072(6) 0.071(7) O13 0.248(8) 0.200(7) 0.113(5) 0.057(5) 0.006(4) 0.054(7) P3 0.1296(16) 0.1014(15) 0.1025(14) -0.0051(11) 0.0333(13) 0.0140(13) F1 0.125(7) 0.378(17) 0.148(8) -0.057(9) 0.017(6) -0.051(9) F2 0.329(17) 0.078(5) 0.178(9) 0.014(5) 0.029(11) 0.041(7) F3 0.218(10) 0.266(14) 0.119(7) -0.001(7) 0.099(7) 0.015(8) F4 0.47(2) 0.176(10) 0.203(10) 0.085(8) 0.094(14) 0.150(12) F5 0.280(12) 0.250(12) 0.165(9) -0.024(9) 0.145(9) 0.013(9) F6 0.197(11) 0.247(14) 0.314(18) -0.152(13) -0.063(11) -0.004(8) P4 0.154(2) 0.1039(16) 0.1233(18) 0.0037(14) 0.0259(17) 0.0196(16) F7 0.173(7) 0.169(6) 0.206(9) -0.006(6) -0.046(6) -0.003(5) F8 0.309(13) 0.263(12) 0.369(14) -0.170(12) 0.232(12) -0.049(9) F9 0.289(13) 0.186(9) 0.295(13) 0.130(9) -0.010(10) -0.008(8) F10 0.255(10) 0.308(11) 0.121(6) -0.026(7) 0.087(6) 0.025(8) F11 0.377(13) 0.149(7) 0.168(7) 0.059(5) 0.089(8) 0.038(7) F12 0.156(7) 0.215(9) 0.305(13) -0.123(9) 0.040(8) -0.029(6) P1 0.0904(11) 0.0863(11) 0.0530(8) 0.0084(8) 0.0063(7) 0.0102(10) P2 0.0862(11) 0.0703(9) 0.0570(8) 0.0049(7) 0.0081(7) 0.0099(9) Zn1 0.0960(5) 0.0733(5) 0.0602(4) 0.0007(4) 0.0044(4) 0.0103(4) Zn2 0.0863(5) 0.0722(5) 0.0676(4) 0.0059(4) 0.0149(4) 0.0099(4) Zn3 0.0922(5) 0.0699(5) 0.0744(5) 0.0088(4) 0.0098(4) 0.0100(4) Zn4 0.0860(5) 0.0855(5) 0.0757(5) 0.0122(4) 0.0156(4) 0.0166(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.524(10) . ? C1 H1A 0.96 . ? C1 H1B 0.96 . ? C1 H1C 0.96 . ? C2 C7 1.388(9) . ? C2 C3 1.395(10) . ? C3 C4 1.413(9) . ? C3 H3 0.93 . ? C4 C5 1.412(8) . ? C4 C8 1.496(8) . ? C5 O1A 1.334(7) . ? C5 C6 1.402(8) . ? C6 C7 1.390(8) . ? C6 C18 1.500(8) . ? C7 H7 0.93 . ? C8 N3A 1.508(7) . ? C8 H8A 0.97 . ? C8 H8B 0.97 . ? C9 N3A 1.497(7) . ? C9 C10 1.533(9) . ? C9 H9A 0.97 . ? C9 H9B 0.97 . ? C10 O5A 1.423(8) . ? C11 O5A 1.410(7) . ? C11 H11A 0.96 . ? C11 H11B 0.96 . ? C11 H11C 0.96 . ? C12 N3A 1.474(7) . ? C12 C13 1.494(8) . ? C12 H12A 0.97 . ? C12 H12B 0.97 . ? C13 N4A 1.324(7) . ? C13 C14 1.363(8) . ? C14 C15 1.348(8) . ? C14 H14 0.93 . ? C15 C16 1.387(9) . ? C15 H15 0.93 . ? C16 C17 1.347(8) . ? C16 H16 0.93 . ? C17 N4A 1.327(7) . ? C17 H17 0.93 . ? C18 N1A 1.498(7) . ? C18 H18A 0.97 . ? C18 H18B 0.97 . ? C19 C20 1.496(8) . ? C19 N1A 1.504(7) . ? C19 H19B 0.97 . ? C19 H19D 0.97 . ? C20 O4A 1.405(7) . ? C20 H20B 0.97 . ? C20 H20D 0.97 . ? C21 O4A 1.434(7) . ? C21 H21A 0.96 . ? C21 H21B 0.96 . ? C21 H21C 0.96 . ? C22 N1A 1.496(7) . ? C22 C23 1.505(8) . ? C22 H22A 0.97 . ? C22 H22B 0.97 . ? C23 N2A 1.330(7) . ? C23 C24 1.381(9) . ? C24 C25 1.363(10) . ? C24 H24 0.93 . ? C25 C26 1.391(10) . ? C25 H25 0.93 . ? C26 C27 1.360(9) . ? C26 H26 0.93 . ? C27 N2A 1.309(7) . ? C27 H27 0.93 . ? C28 C29 1.548(13) . ? C28 H28A 0.96 . ? C28 H28B 0.96 . ? C28 H28C 0.96 . ? C29 C30 1.345(13) . ? C29 C34 1.379(13) . ? C30 C31 1.418(11) . ? C30 H30 0.93 . ? C31 C32 1.364(9) . ? C31 C35 1.501(10) . ? C32 O1B 1.362(8) . ? C32 C33 1.377(10) . ? C33 C34 1.440(10) . ? C33 C45 1.499(10) . ? C34 H34 0.93 . ? C35 N3B 1.479(8) . ? C35 H35A 0.97 . ? C35 H35B 0.97 . ? C36 C37 1.453(9) . ? C36 N3B 1.509(7) . ? C36 H36A 0.97 . ? C36 H36B 0.97 . ? C37 O5B 1.434(9) . ? C37 H37A 0.97 . ? C37 H37B 0.97 . ? C38 O5B 1.370(8) . ? C38 H38A 0.96 . ? C38 H38B 0.96 . ? C38 H38C 0.96 . ? C39 C40 1.474(10) . ? C39 N3B 1.481(9) . ? C39 H39A 0.97 . ? C39 H39B 0.97 . ? C40 C41 1.348(11) . ? C40 N4B 1.352(9) . ? C41 C42 1.444(13) . ? C41 H41 0.93 . ? C42 C43 1.361(14) . ? C42 H42 0.93 . ? C43 C44 1.300(12) . ? C43 H43 0.93 . ? C44 N4B 1.320(8) . ? C44 H44 0.93 . ? C45 N1B 1.515(8) . ? C45 H45A 0.97 . ? C45 H45B 0.97 . ? C46 N1B 1.483(7) . ? C46 C47 1.533(9) . ? C46 H46A 0.97 . ? C46 H46B 0.97 . ? C47 O4B 1.475(8) . ? C47 H47A 0.97 . ? C47 H47B 0.97 . ? C48 O4B 1.415(7) . ? C48 H48A 0.96 . ? C48 H48B 0.96 . ? C48 H48C 0.96 . ? C49 N1B 1.456(9) . ? C49 C50 1.518(11) . ? C49 H49A 0.97 . ? C49 H49B 0.97 . ? C50 C51 1.357(13) . ? C50 N2B 1.363(10) . ? C51 C52 1.388(15) . ? C51 H51 0.93 . ? C52 C53 1.479(12) . ? C52 H52 0.93 . ? C53 C54 1.403(10) . ? C53 H53 0.93 . ? C54 N2B 1.339(8) . ? C54 H54 0.93 . ? C55 C60 1.354(8) . ? C55 C56 1.379(8) . ? C55 O8 1.381(6) . ? C56 C57 1.395(10) . ? C56 H56 0.93 . ? C57 C58 1.324(10) . ? C57 H57 0.93 . ? C58 C59 1.354(9) . ? C58 N10 1.510(11) . ? C59 C60 1.392(8) . ? C59 H59 0.93 . ? C60 H60 0.93 . ? C61 O9 1.365(6) . ? C61 C62 1.373(8) . ? C61 C66 1.376(8) . ? C62 C63 1.399(8) . ? C62 H62 0.93 . ? C63 C64 1.346(9) . ? C63 H63 0.93 . ? C64 C65 1.355(9) . ? C64 N9 1.477(9) . ? C65 C66 1.393(9) . ? C65 H65 0.93 . ? C66 H66 0.93 . ? N1A Zn2 2.164(5) . ? N1B Zn4 2.202(5) . ? N2A Zn2 2.129(5) . ? N2B Zn4 2.126(6) . ? N3A Zn1 2.154(4) . ? N3B Zn3 2.170(5) . ? N4A Zn1 2.111(4) . ? N4B Zn3 2.184(6) . ? N9 O12 1.143(9) . ? N9 O13 1.207(9) . ? N10 O11 1.161(12) . ? N10 O10 1.228(10) . ? O1A Zn1 2.065(4) . ? O1A Zn2 2.096(3) . ? O1B Zn4 2.013(4) . ? O1B Zn3 2.050(4) . ? O2A P2 1.521(4) . ? O2A Zn2 2.011(4) . ? O2B P2 1.506(4) . ? O2B Zn4 1.993(3) . ? O3A Zn1 2.080(3) . ? O3A H19A 0.96 . ? O3A H19C 0.96 . ? O3B P2 1.498(3) . ? O3B Zn3 2.082(3) . ? O4A Zn2 2.374(4) . ? O4B Zn4 2.389(4) . ? O5B Zn3 2.262(4) . ? O6A P1 1.518(4) . ? O6A Zn1 2.001(4) . ? O6B P1 1.499(4) . ? O6B Zn3 1.982(4) . ? O7A Zn2 2.128(3) . ? O7A H20A 0.96 . ? O7A H20C 0.96 . ? O7B P1 1.497(4) . ? O7B Zn4 2.065(4) . ? O8 P1 1.641(4) . ? O9 P2 1.641(4) . ? P3 F1' 1.487(10) . ? P3 F2 1.494(7) . ? P3 F3' 1.503(10) . ? P3 F6 1.514(8) . ? P3 F4' 1.521(11) . ? P3 F2' 1.541(9) . ? P3 F4 1.561(8) . ? P3 F5 1.577(7) . ? P3 F3 1.578(7) . ? P3 F1 1.621(8) . ? P3 F5' 1.646(11) . ? P3 F6' 1.646(9) . ? P4 F9' 1.461(14) . ? P4 F8' 1.462(13) . ? P4 F9 1.487(7) . ? P4 F8 1.533(7) . ? P4 F12 1.534(7) . ? P4 F10 1.554(7) . ? P4 F11 1.562(7) . ? P4 F7' 1.566(13) . ? P4 F12' 1.571(12) . ? P4 F11' 1.578(12) . ? P4 F7 1.594(6) . ? P4 F10' 1.631(12) . ? 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C7 C2 C3 118.8(7) . . ? C7 C2 C1 122.0(9) . . ? C3 C2 C1 119.2(8) . . ? C2 C3 C4 120.9(7) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 120.2(7) . . ? C5 C4 C8 118.2(6) . . ? C3 C4 C8 121.6(7) . . ? O1A C5 C6 122.0(6) . . ? O1A C5 C4 120.4(6) . . ? C6 C5 C4 117.6(6) . . ? C7 C6 C5 121.8(6) . . ? C7 C6 C18 118.0(6) . . ? C5 C6 C18 120.2(6) . . ? C2 C7 C6 120.8(7) . . ? C2 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C4 C8 N3A 112.3(5) . . ? C4 C8 H8A 109.1 . . ? N3A C8 H8A 109.1 . . ? C4 C8 H8B 109.1 . . ? N3A C8 H8B 109.1 . . ? H8A C8 H8B 107.9 . . ? N3A C9 C10 114.5(5) . . ? N3A C9 H9A 108.6 . . ? C10 C9 H9A 108.6 . . ? N3A C9 H9B 108.6 . . ? C10 C9 H9B 108.6 . . ? H9A C9 H9B 107.6 . . ? O5A C10 C9 106.1(6) . . ? O5A C11 H11A 109.5 . . ? O5A C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O5A C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N3A C12 C13 113.1(5) . . ? N3A C12 H12A 109 . . ? C13 C12 H12A 109 . . ? N3A C12 H12B 109 . . ? C13 C12 H12B 109 . . ? H12A C12 H12B 107.8 . . ? N4A C13 C14 121.3(6) . . ? N4A C13 C12 117.0(6) . . ? C14 C13 C12 121.7(6) . . ? C15 C14 C13 119.7(7) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 119.3(6) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C17 C16 C15 117.8(6) . . ? C17 C16 H16 121.1 . . ? C15 C16 H16 121.1 . . ? N4A C17 C16 123.0(6) . . ? N4A C17 H17 118.5 . . ? C16 C17 H17 118.5 . . ? N1A C18 C6 111.8(5) . . ? N1A C18 H18A 109.3 . . ? C6 C18 H18A 109.3 . . ? N1A C18 H18B 109.3 . . ? C6 C18 H18B 109.3 . . ? H18A C18 H18B 107.9 . . ? C20 C19 N1A 112.7(5) . . ? C20 C19 H19B 109 . . ? N1A C19 H19B 109 . . ? C20 C19 H19D 109 . . ? N1A C19 H19D 109 . . ? H19B C19 H19D 107.8 . . ? O4A C20 C19 108.9(5) . . ? O4A C20 H20B 109.9 . . ? C19 C20 H20B 109.9 . . ? O4A C20 H20D 109.9 . . ? C19 C20 H20D 109.9 . . ? H20B C20 H20D 108.3 . . ? O4A C21 H21A 109.5 . . ? O4A C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O4A C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N1A C22 C23 111.8(5) . . ? N1A C22 H22A 109.3 . . ? C23 C22 H22A 109.3 . . ? N1A C22 H22B 109.3 . . ? C23 C22 H22B 109.3 . . ? H22A C22 H22B 107.9 . . ? N2A C23 C24 122.2(6) . . ? N2A C23 C22 117.1(6) . . ? C24 C23 C22 120.6(7) . . ? C25 C24 C23 118.9(8) . . ? C25 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? C24 C25 C26 117.9(8) . . ? C24 C25 H25 121.1 . . ? C26 C25 H25 121.1 . . ? C27 C26 C25 119.8(8) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? N2A C27 C26 122.1(7) . . ? N2A C27 H27 119 . . ? C26 C27 H27 119 . . ? C29 C28 H28A 109.5 . . ? C29 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C29 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C34 119.7(11) . . ? C30 C29 C28 123.4(13) . . ? C34 C29 C28 117.0(13) . . ? C29 C30 C31 121.2(11) . . ? C29 C30 H30 119.4 . . ? C31 C30 H30 119.4 . . ? C32 C31 C30 121.2(9) . . ? C32 C31 C35 118.0(8) . . ? C30 C31 C35 120.7(9) . . ? O1B C32 C31 122.1(8) . . ? O1B C32 C33 120.2(8) . . ? C31 C32 C33 117.6(9) . . ? C32 C33 C34 121.5(9) . . ? C32 C33 C45 119.6(8) . . ? C34 C33 C45 118.9(10) . . ? C29 C34 C33 118.7(10) . . ? C29 C34 H34 120.6 . . ? C33 C34 H34 120.6 . . ? N3B C35 C31 111.1(6) . . ? N3B C35 H35A 109.4 . . ? C31 C35 H35A 109.4 . . ? N3B C35 H35B 109.4 . . ? C31 C35 H35B 109.4 . . ? H35A C35 H35B 108 . . ? C37 C36 N3B 117.5(6) . . ? C37 C36 H36A 107.9 . . ? N3B C36 H36A 107.9 . . ? C37 C36 H36B 107.9 . . ? N3B C36 H36B 107.9 . . ? H36A C36 H36B 107.2 . . ? O5B C37 C36 108.5(7) . . ? O5B C37 H37A 110 . . ? C36 C37 H37A 110 . . ? O5B C37 H37B 110 . . ? C36 C37 H37B 110 . . ? H37A C37 H37B 108.4 . . ? O5B C38 H38A 109.5 . . ? O5B C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? O5B C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 N3B 110.2(6) . . ? C40 C39 H39A 109.6 . . ? N3B C39 H39A 109.6 . . ? C40 C39 H39B 109.6 . . ? N3B C39 H39B 109.6 . . ? H39A C39 H39B 108.1 . . ? C41 C40 N4B 119.4(9) . . ? C41 C40 C39 124.4(10) . . ? N4B C40 C39 116.2(7) . . ? C40 C41 C42 117.5(10) . . ? C40 C41 H41 121.2 . . ? C42 C41 H41 121.2 . . ? C43 C42 C41 118.9(11) . . ? C43 C42 H42 120.5 . . ? C41 C42 H42 120.5 . . ? C44 C43 C42 119.9(12) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C43 C44 N4B 122.0(9) . . ? C43 C44 H44 119 . . ? N4B C44 H44 119 . . ? C33 C45 N1B 110.7(5) . . ? C33 C45 H45A 109.5 . . ? N1B C45 H45A 109.5 . . ? C33 C45 H45B 109.5 . . ? N1B C45 H45B 109.5 . . ? H45A C45 H45B 108.1 . . ? N1B C46 C47 116.2(6) . . ? N1B C46 H46A 108.2 . . ? C47 C46 H46A 108.2 . . ? N1B C46 H46B 108.2 . . ? C47 C46 H46B 108.2 . . ? H46A C46 H46B 107.4 . . ? O4B C47 C46 103.7(6) . . ? O4B C47 H47A 111 . . ? C46 C47 H47A 111 . . ? O4B C47 H47B 111 . . ? C46 C47 H47B 111 . . ? H47A C47 H47B 109 . . ? O4B C48 H48A 109.5 . . ? O4B C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? O4B C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N1B C49 C50 107.3(6) . . ? N1B C49 H49A 110.3 . . ? C50 C49 H49A 110.3 . . ? N1B C49 H49B 110.3 . . ? C50 C49 H49B 110.3 . . ? H49A C49 H49B 108.5 . . ? C51 C50 N2B 126.2(10) . . ? C51 C50 C49 116.4(10) . . ? N2B C50 C49 117.4(8) . . ? C50 C51 C52 113.8(12) . . ? C50 C51 H51 123.1 . . ? C52 C51 H51 123.1 . . ? C51 C52 C53 123.1(11) . . ? C51 C52 H52 118.5 . . ? C53 C52 H52 118.5 . . ? C54 C53 C52 115.7(9) . . ? C54 C53 H53 122.1 . . ? C52 C53 H53 122.1 . . ? N2B C54 C53 120.5(8) . . ? N2B C54 H54 119.8 . . ? C53 C54 H54 119.8 . . ? C60 C55 C56 120.6(6) . . ? C60 C55 O8 122.9(6) . . ? C56 C55 O8 116.5(6) . . ? C55 C56 C57 118.2(7) . . ? C55 C56 H56 120.9 . . ? C57 C56 H56 120.9 . . ? C58 C57 C56 120.2(7) . . ? C58 C57 H57 119.9 . . ? C56 C57 H57 119.9 . . ? C57 C58 C59 122.6(7) . . ? C57 C58 N10 116.5(9) . . ? C59 C58 N10 120.9(10) . . ? C58 C59 C60 118.3(7) . . ? C58 C59 H59 120.9 . . ? C60 C59 H59 120.9 . . ? C55 C60 C59 120.1(6) . . ? C55 C60 H60 119.9 . . ? C59 C60 H60 119.9 . . ? O9 C61 C62 123.5(5) . . ? O9 C61 C66 115.7(6) . . ? C62 C61 C66 120.8(6) . . ? C61 C62 C63 119.4(6) . . ? C61 C62 H62 120.3 . . ? C63 C62 H62 120.3 . . ? C64 C63 C62 119.1(7) . . ? C64 C63 H63 120.5 . . ? C62 C63 H63 120.5 . . ? C63 C64 C65 122.2(7) . . ? C63 C64 N9 119.1(8) . . ? C65 C64 N9 118.6(8) . . ? C64 C65 C66 119.7(6) . . ? C64 C65 H65 120.2 . . ? C66 C65 H65 120.2 . . ? C61 C66 C65 118.8(6) . . ? C61 C66 H66 120.6 . . ? C65 C66 H66 120.6 . . ? C22 N1A C18 109.7(5) . . ? C22 N1A C19 110.9(5) . . ? C18 N1A C19 110.2(5) . . ? C22 N1A Zn2 109.2(4) . . ? C18 N1A Zn2 107.8(3) . . ? C19 N1A Zn2 109.1(4) . . ? C49 N1B C46 110.5(6) . . ? C49 N1B C45 111.0(6) . . ? C46 N1B C45 111.9(5) . . ? C49 N1B Zn4 101.3(4) . . ? C46 N1B Zn4 113.3(4) . . ? C45 N1B Zn4 108.4(4) . . ? C27 N2A C23 119.2(6) . . ? C27 N2A Zn2 123.8(5) . . ? C23 N2A Zn2 114.0(4) . . ? C54 N2B C50 120.6(7) . . ? C54 N2B Zn4 129.2(6) . . ? C50 N2B Zn4 110.2(6) . . ? C12 N3A C9 110.9(5) . . ? C12 N3A C8 111.2(5) . . ? C9 N3A C8 109.5(5) . . ? C12 N3A Zn1 109.6(3) . . ? C9 N3A Zn1 110.2(4) . . ? C8 N3A Zn1 105.3(3) . . ? C35 N3B C39 109.2(6) . . ? C35 N3B C36 113.3(6) . . ? C39 N3B C36 111.4(5) . . ? C35 N3B Zn3 109.6(4) . . ? C39 N3B Zn3 102.5(4) . . ? C36 N3B Zn3 110.3(4) . . ? C13 N4A C17 119.0(5) . . ? C13 N4A Zn1 115.0(4) . . ? C17 N4A Zn1 124.3(4) . . ? C44 N4B C40 121.7(7) . . ? C44 N4B Zn3 127.0(6) . . ? C40 N4B Zn3 111.0(5) . . ? O12 N9 O13 121.9(9) . . ? O12 N9 C64 119.7(9) . . ? O13 N9 C64 117.8(8) . . ? O11 N10 O10 124.6(11) . . ? O11 N10 C58 122.4(11) . . ? O10 N10 C58 113.0(11) . . ? C5 O1A Zn1 115.6(3) . . ? C5 O1A Zn2 115.9(3) . . ? Zn1 O1A Zn2 128.4(2) . . ? C32 O1B Zn4 121.6(4) . . ? C32 O1B Zn3 118.3(4) . . ? Zn4 O1B Zn3 120.1(2) . . ? P2 O2A Zn2 135.3(2) . . ? P2 O2B Zn4 133.0(2) . . ? Zn1 O3A H19A 109.1 . . ? Zn1 O3A H19C 109.1 . . ? H19A O3A H19C 109.5 . . ? P2 O3B Zn3 138.0(2) . . ? C20 O4A C21 112.1(5) . . ? C20 O4A Zn2 114.0(4) . . ? C21 O4A Zn2 129.9(4) . . ? C48 O4B C47 109.4(6) . . ? C48 O4B Zn4 125.1(5) . . ? C47 O4B Zn4 114.4(4) . . ? C11 O5A C10 110.5(5) . . ? C38 O5B C37 115.8(6) . . ? C38 O5B Zn3 126.2(5) . . ? C37 O5B Zn3 114.8(4) . . ? P1 O6A Zn1 138.8(2) . . ? P1 O6B Zn3 132.5(2) . . ? Zn2 O7A H20A 109.4 . . ? Zn2 O7A H20C 109.7 . . ? H20A O7A H20C 109.5 . . ? P1 O7B Zn4 136.2(2) . . ? C55 O8 P1 120.5(3) . . ? C61 O9 P2 125.2(4) . . ? F1' P3 F2 93.8(7) . . ? F1' P3 F3' 98.8(7) . . ? F2 P3 F3' 148.8(6) . . ? F1' P3 F6 168.6(10) . . ? F2 P3 F6 87.9(6) . . ? F3' P3 F6 74.6(8) . . ? F1' P3 F4' 94.6(7) . . ? F2 P3 F4' 118.7(7) . . ? F3' P3 F4' 88.8(6) . . ? F6 P3 F4' 94.5(8) . . ? F1' P3 F2' 89.7(6) . . ? F2 P3 F2' 55.7(7) . . ? F3' P3 F2' 95.7(6) . . ? F6 P3 F2' 81.9(7) . . ? F4' P3 F2' 173.3(7) . . ? F1' P3 F4 82.2(9) . . ? F2 P3 F4 175.3(8) . . ? F3' P3 F4 35.1(7) . . ? F6 P3 F4 96.6(7) . . ? F4' P3 F4 59.5(7) . . ? F2' P3 F4 126.4(6) . . ? F1' P3 F5 67.0(7) . . ? F2 P3 F5 93.5(6) . . ? F3' P3 F5 66.0(6) . . ? F6 P3 F5 101.6(8) . . ? F4' P3 F5 144.6(6) . . ? F2' P3 F5 42.2(5) . . ? F4 P3 F5 87.2(5) . . ? F1' P3 F3 109.1(7) . . ? F2 P3 F3 94.6(5) . . ? F3' P3 F3 107.9(7) . . ? F6 P3 F3 81.9(8) . . ? F4' P3 F3 26.8(5) . . ? F2' P3 F3 146.5(6) . . ? F4 P3 F3 84.5(5) . . ? F5 P3 F3 171.3(6) . . ? F1' P3 F1 20.7(9) . . ? F2 P3 F1 87.4(6) . . ? F3' P3 F1 113.3(7) . . ? F6 P3 F1 170.4(9) . . ? F4' P3 F1 80.5(7) . . ? F2' P3 F1 102.2(6) . . ? F4 P3 F1 88.0(6) . . ? F5 P3 F1 87.0(6) . . ? F3 P3 F1 90.1(5) . . ? F1' P3 F5' 89.4(7) . . ? F2 P3 F5' 33.6(6) . . ? F3' P3 F5' 170.6(8) . . ? F6 P3 F5' 98.1(9) . . ? F4' P3 F5' 85.9(6) . . ? F2' P3 F5' 89.0(6) . . ? F4 P3 F5' 143.3(7) . . ? F5 P3 F5' 122.1(7) . . ? F3 P3 F5' 64.6(6) . . ? F1 P3 F5' 73.5(7) . . ? F1' P3 F6' 171.3(8) . . ? F2 P3 F6' 83.8(7) . . ? F3' P3 F6' 79.5(7) . . ? F6 P3 F6' 5.0(13) . . ? F4' P3 F6' 93.8(6) . . ? F2' P3 F6' 82.1(6) . . ? F4 P3 F6' 100.5(8) . . ? F5 P3 F6' 104.7(7) . . ? F3 P3 F6' 79.4(7) . . ? F1 P3 F6' 165.7(8) . . ? F5' P3 F6' 93.1(7) . . ? F9' P4 F8' 96.5(8) . . ? F9' P4 F9 133.8(11) . . ? F8' P4 F9 117.6(9) . . ? F9' P4 F8 133.4(9) . . ? F8' P4 F8 48.2(8) . . ? F9 P4 F8 92.6(6) . . ? F9' P4 F12 87.2(8) . . ? F8' P4 F12 121.4(10) . . ? F9 P4 F12 98.9(6) . . ? F8 P4 F12 89.0(6) . . ? F9' P4 F10 40.9(8) . . ? F8' P4 F10 130.6(8) . . ? F9 P4 F10 93.4(7) . . ? F8 P4 F10 173.1(5) . . ? F12 P4 F10 86.9(5) . . ? F9' P4 F11 44.7(8) . . ? F8' P4 F11 60.0(8) . . ? F9 P4 F11 174.8(6) . . ? F8 P4 F11 88.7(6) . . ? F12 P4 F11 86.2(6) . . ? F10 P4 F11 85.6(4) . . ? F9' P4 F7' 89.7(8) . . ? F8' P4 F7' 93.9(9) . . ? F9 P4 F7' 59.7(7) . . ? F8 P4 F7' 117.6(8) . . ? F12 P4 F7' 144.7(10) . . ? F10 P4 F7' 68.5(8) . . ? F11 P4 F7' 115.2(8) . . ? F9' P4 F12' 98.2(10) . . ? F8' P4 F12' 90.4(9) . . ? F9 P4 F12' 110.9(8) . . ? F8 P4 F12' 60.0(9) . . ? F12 P4 F12' 31.9(6) . . ? F10 P4 F12' 114.6(10) . . ? F11 P4 F12' 74.2(9) . . ? F7' P4 F12' 170.6(10) . . ? F9' P4 F11' 173.8(11) . . ? F8' P4 F11' 89.2(8) . . ? F9 P4 F11' 40.3(6) . . ? F8 P4 F11' 52.6(6) . . ? F12 P4 F11' 91.8(7) . . ? F10 P4 F11' 132.9(7) . . ? F11 P4 F11' 141.4(8) . . ? F7' P4 F11' 87.6(7) . . ? F12' P4 F11' 84.1(8) . . ? F9' P4 F7 89.5(8) . . ? F8' P4 F7 53.0(8) . . ? F9 P4 F7 87.8(5) . . ? F8 P4 F7 88.9(5) . . ? F12 P4 F7 173.1(7) . . ? F10 P4 F7 94.6(5) . . ? F11 P4 F7 87.2(5) . . ? F7' P4 F7 41.2(7) . . ? F12' P4 F7 143.3(8) . . ? F11' P4 F7 92.1(7) . . ? F9' P4 F10' 91.7(9) . . ? F8' P4 F10' 169.6(9) . . ? F9 P4 F10' 59.4(7) . . ? F8 P4 F10' 121.4(7) . . ? F12 P4 F10' 52.5(7) . . ? F10 P4 F10' 59.5(6) . . ? F11 P4 F10' 123.8(7) . . ? F7' P4 F10' 92.6(8) . . ? F12' P4 F10' 82.1(7) . . ? F11' P4 F10' 82.9(7) . . ? F7 P4 F10' 133.8(7) . . ? O7B P1 O6B 116.3(2) . . ? O7B P1 O6A 114.1(2) . . ? O6B P1 O6A 110.7(2) . . ? O7B P1 O8 102.5(2) . . ? O6B P1 O8 107.0(2) . . ? O6A P1 O8 105.0(2) . . ? O3B P2 O2B 116.4(2) . . ? O3B P2 O2A 113.6(2) . . ? O2B P2 O2A 111.3(2) . . ? O3B P2 O9 101.59(19) . . ? O2B P2 O9 105.6(2) . . ? O2A P2 O9 107.2(2) . . ? O6A Zn1 O1A 99.84(15) . . ? O6A Zn1 O3A 92.61(14) . . ? O1A Zn1 O3A 89.92(14) . . ? O6A Zn1 N4A 94.05(17) . . ? O1A Zn1 N4A 93.61(16) . . ? O3A Zn1 N4A 171.81(17) . . ? O6A Zn1 N3A 165.46(17) . . ? O1A Zn1 N3A 93.81(18) . . ? O3A Zn1 N3A 92.40(16) . . ? N4A Zn1 N3A 80.01(18) . . ? O2A Zn2 O1A 100.42(14) . . ? O2A Zn2 O7A 92.58(14) . . ? O1A Zn2 O7A 87.19(13) . . ? O2A Zn2 N2A 97.68(18) . . ? O1A Zn2 N2A 90.71(16) . . ? O7A Zn2 N2A 169.74(18) . . ? O2A Zn2 N1A 166.23(17) . . ? O1A Zn2 N1A 93.23(17) . . ? O7A Zn2 N1A 89.85(16) . . ? N2A Zn2 N1A 80.2(2) . . ? O2A Zn2 O4A 92.85(15) . . ? O1A Zn2 O4A 160.83(14) . . ? O7A Zn2 O4A 78.39(14) . . ? N2A Zn2 O4A 101.24(16) . . ? N1A Zn2 O4A 74.37(17) . . ? O6B Zn3 O1B 98.45(16) . . ? O6B Zn3 O3B 96.00(14) . . ? O1B Zn3 O3B 92.72(15) . . ? O6B Zn3 N3B 163.13(17) . . ? O1B Zn3 N3B 89.64(19) . . ? O3B Zn3 N3B 98.39(18) . . ? O6B Zn3 N4B 95.8(2) . . ? O1B Zn3 N4B 165.5(2) . . ? O3B Zn3 N4B 83.22(16) . . ? N3B Zn3 N4B 77.3(2) . . ? O6B Zn3 O5B 87.45(18) . . ? O1B Zn3 O5B 94.93(16) . . ? O3B Zn3 O5B 171.06(16) . . ? N3B Zn3 O5B 77.1(2) . . ? N4B Zn3 O5B 88.24(18) . . ? O2B Zn4 O1B 98.67(16) . . ? O2B Zn4 O7B 96.78(15) . . ? O1B Zn4 O7B 94.10(15) . . ? O2B Zn4 N2B 93.3(2) . . ? O1B Zn4 N2B 167.4(2) . . ? O7B Zn4 N2B 88.15(19) . . ? O2B Zn4 N1B 161.20(17) . . ? O1B Zn4 N1B 89.8(2) . . ? O7B Zn4 N1B 99.31(19) . . ? N2B Zn4 N1B 77.6(2) . . ? O2B Zn4 O4B 88.63(16) . . ? O1B Zn4 O4B 91.72(16) . . ? O7B Zn4 O4B 171.37(16) . . ? N2B Zn4 O4B 84.8(2) . . ? N1B Zn4 O4B 74.31(19) . . ? #===END #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2011-06-15 at 16:51:30 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : 551ld13 551abs struct data_551ld13 _database_code_depnum_ccdc_archive 'CCDC 830845' #TrackingRef 'supdata.cif' _audit_creation_date 2011-06-15T16:51:30-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C52 H68 Br2 F2 N8 O14 P2 Zn4, 2 (F6 P)' _chemical_formula_sum 'C52 H68 Br2 F14 N8 O14 P4 Zn4' _chemical_formula_weight 1840.32 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.3002(6) _cell_length_b 15.8922(6) _cell_length_c 19.6397(7) _cell_angle_alpha 94.791(3) _cell_angle_beta 109.511(4) _cell_angle_gamma 112.586(4) _cell_volume 3504.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11972 _cell_measurement_theta_min 3.1025 _cell_measurement_theta_max 62.3232 _cell_measurement_wavelength 1.5418 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2692 _exptl_crystal_size_mid 0.1191 _exptl_crystal_size_min 0.0824 _exptl_crystal_density_diffrn 1.744 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 -1 0.0386 -1 0 1 0.0438 0 -1 -1 0.0404 0 0 1 0.0517 0 0 -1 0.0438 0 -1 1 0.0923 0 1 -1 0.0862 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.658 _exptl_absorpt_correction_type analytical _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) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.58 _exptl_absorpt_correction_T_max 0.759 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 16.0696 _diffrn_orient_matrix_ub_11 -0.1063059 _diffrn_orient_matrix_ub_12 0.0005593 _diffrn_orient_matrix_ub_13 0.0149982 _diffrn_orient_matrix_ub_21 -0.0859345 _diffrn_orient_matrix_ub_22 -0.0729452 _diffrn_orient_matrix_ub_23 -0.0745124 _diffrn_orient_matrix_ub_31 -0.003538 _diffrn_orient_matrix_ub_32 -0.0799734 _diffrn_orient_matrix_ub_33 0.0398066 _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_unetI/netI 0.0368 _diffrn_reflns_number 36029 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 62.41 _diffrn_reflns_theta_full 62.41 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 11083 _reflns_number_gt 7837 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.1061P)^2^+2.4267P] 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_number_reflns 11083 _refine_ls_number_parameters 900 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0778 _refine_ls_R_factor_gt 0.053 _refine_ls_wR_factor_ref 0.1675 _refine_ls_wR_factor_gt 0.1522 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.886 _refine_diff_density_min -0.972 _refine_diff_density_rms 0.102 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8996(6) 0.0105(4) 1.1041(3) 0.0452(14) Uani 1 1 d . . . C2 C 0.9887(5) 0.0605(4) 1.0829(3) 0.0433(13) Uani 1 1 d . . . H2 H 1.0655 0.0683 1.1092 0.052 Uiso 1 1 calc R . . C3 C 0.9645(5) 0.1001(4) 1.0212(3) 0.0422(13) Uani 1 1 d . . . C4 C 0.8475(5) 0.0873(4) 0.9814(3) 0.0393(13) Uani 1 1 d . . . C5 C 0.7583(5) 0.0371(4) 1.0048(3) 0.0420(13) Uani 1 1 d . . . C6 C 0.7855(6) -0.0011(4) 1.0659(3) 0.0447(14) Uani 1 1 d . . . H6 H 0.7259 -0.0349 1.0812 0.054 Uiso 1 1 calc R . . C7 C 1.0639(5) 0.1585(4) 1.0001(3) 0.0442(14) Uani 1 1 d . . . H7A H 1.135 0.1523 1.0283 0.053 Uiso 1 1 calc R . . H7B H 1.0428 0.1351 0.9476 0.053 Uiso 1 1 calc R . . C8 C 0.9975(5) 0.2849(4) 1.1011(3) 0.0408(13) Uani 1 1 d . . . C9 C 0.9798(6) 0.2688(4) 1.1655(3) 0.0480(14) Uani 1 1 d . . . H9 H 1.0378 0.2637 1.2052 0.058 Uiso 1 1 calc R . . C10 C 0.8757(6) 0.2606(5) 1.1700(4) 0.0536(16) Uani 1 1 d . . . H10 H 0.8629 0.2506 1.213 0.064 Uiso 1 1 calc R . . C11 C 0.7901(6) 0.2672(4) 1.1101(3) 0.0479(14) Uani 1 1 d . . . H11 H 0.7191 0.2622 1.1119 0.058 Uiso 1 1 calc R . . C12 C 0.8131(5) 0.2815(4) 1.0474(3) 0.0417(13) Uani 1 1 d . . . H12 H 0.7551 0.2846 1.0064 0.05 Uiso 1 1 calc R . . C13 C 1.1110(5) 0.2979(4) 1.0929(3) 0.0441(13) Uani 1 1 d . . . H13A H 1.1651 0.3644 1.1082 0.053 Uiso 1 1 calc R . . H13B H 1.1485 0.2664 1.1255 0.053 Uiso 1 1 calc R . . C14 C 1.1918(5) 0.3125(4) 0.9970(3) 0.0463(14) Uani 1 1 d . . . H14A H 1.1794 0.2813 0.9483 0.056 Uiso 1 1 calc R . . H14B H 1.2627 0.3131 1.0333 0.056 Uiso 1 1 calc R . . C15 C 1.2093(5) 0.4116(4) 0.9975(4) 0.0480(14) Uani 1 1 d . . . H15A H 1.2461 0.449 1.0483 0.058 Uiso 1 1 calc R . . H15B H 1.2608 0.4393 0.9722 0.058 Uiso 1 1 calc R . . C16 C 0.6181(6) -0.1558(4) 0.8295(3) 0.0506(15) Uani 1 1 d . . . C17 C 0.6004(6) -0.2479(5) 0.8115(4) 0.0611(18) Uani 1 1 d . . . H17 H 0.5563 -0.2937 0.8301 0.073 Uiso 1 1 calc R . . C18 C 0.6504(7) -0.2700(6) 0.7649(4) 0.074(2) Uani 1 1 d . . . H18 H 0.6409 -0.3311 0.7522 0.089 Uiso 1 1 calc R . . C19 C 0.7141(6) -0.2009(6) 0.7377(4) 0.067(2) Uani 1 1 d . . . H19 H 0.7486 -0.2143 0.7068 0.08 Uiso 1 1 calc R . . C20 C 0.7256(6) -0.1120(5) 0.7571(4) 0.0583(17) Uani 1 1 d . . . H20 H 0.7663 -0.0655 0.7376 0.07 Uiso 1 1 calc R . . C21 C 0.5735(7) -0.1265(4) 0.8843(4) 0.0579(17) Uani 1 1 d . . . H21A H 0.4924 -0.1722 0.8715 0.069 Uiso 1 1 calc R . . H21B H 0.6211 -0.1275 0.9337 0.069 Uiso 1 1 calc R . . C22 C 0.4534(6) -0.0394(5) 0.8526(4) 0.0555(16) Uani 1 1 d . . . H22A H 0.4068 -0.0742 0.8785 0.067 Uiso 1 1 calc R . . H22B H 0.4573 0.0231 0.859 0.067 Uiso 1 1 calc R . . C23 C 0.3932(7) -0.0875(5) 0.7714(4) 0.0677(19) Uani 1 1 d . . . H23A H 0.3799 -0.1526 0.7647 0.081 Uiso 1 1 calc R . . H23B H 0.3169 -0.086 0.75 0.081 Uiso 1 1 calc R . . C24 C 0.6341(5) 0.0254(4) 0.9653(3) 0.0440(13) Uani 1 1 d . . . H24A H 0.5868 -0.0048 0.9923 0.053 Uiso 1 1 calc R . . H24B H 0.6355 0.0868 0.9652 0.053 Uiso 1 1 calc R . . C25 C 0.4184(8) -0.0848(7) 0.6576(4) 0.091(3) Uani 1 1 d . . . H25A H 0.4703 -0.0511 0.635 0.136 Uiso 1 1 calc R . . H25B H 0.3422 -0.0854 0.6337 0.136 Uiso 1 1 calc R . . H25C H 0.4096 -0.1481 0.6522 0.136 Uiso 1 1 calc R . . C26 C 1.1078(6) 0.5025(4) 0.9560(3) 0.0476(14) Uani 1 1 d . . . H26A H 1.0304 0.4993 0.9307 0.071 Uiso 1 1 calc R . . H26B H 1.1561 0.528 0.9291 0.071 Uiso 1 1 calc R . . H26C H 1.1439 0.5423 1.0054 0.071 Uiso 1 1 calc R . . C27 C 0.6708(6) 0.4217(6) 0.4360(4) 0.068(2) Uani 1 1 d . . . C28 C 0.5915(6) 0.3315(6) 0.4312(4) 0.0620(18) Uani 1 1 d . . . H28 H 0.5291 0.2951 0.3861 0.074 Uiso 1 1 calc R . . C29 C 0.6055(5) 0.2959(5) 0.4936(3) 0.0518(15) Uani 1 1 d . . . C30 C 0.7037(5) 0.3496(5) 0.5607(3) 0.0487(15) Uani 1 1 d . . . C31 C 0.7815(6) 0.4402(5) 0.5644(4) 0.0562(17) Uani 1 1 d . . . C32 C 0.7650(6) 0.4771(6) 0.5023(4) 0.0657(19) Uani 1 1 d . . . H32 H 0.8164 0.538 0.5051 0.079 Uiso 1 1 calc R . . C33 C 0.5155(6) 0.2012(5) 0.4906(3) 0.0567(17) Uani 1 1 d . . . H33A H 0.4561 0.1728 0.4401 0.068 Uiso 1 1 calc R . . H33B H 0.5546 0.1609 0.504 0.068 Uiso 1 1 calc R . . C34 C 0.3356(7) 0.1165(6) 0.6034(4) 0.074(2) Uani 1 1 d . . . C35 C 0.2327(10) 0.0577(8) 0.6014(6) 0.123(4) Uani 1 1 d . . . H35 H 0.1764 0.013 0.5575 0.148 Uiso 1 1 calc R . . C36 C 0.2068(11) 0.0620(9) 0.6661(7) 0.136(5) Uani 1 1 d . . . H36 H 0.1344 0.0211 0.6658 0.163 Uiso 1 1 calc R . . C37 C 0.2952(10) 0.1306(8) 0.7298(6) 0.111(4) Uani 1 1 d . . . H37 H 0.2838 0.1348 0.774 0.134 Uiso 1 1 calc R . . C38 C 0.3951(7) 0.1895(6) 0.7275(4) 0.074(2) Uani 1 1 d . . . H38 H 0.4493 0.2399 0.7683 0.088 Uiso 1 1 calc R . . C39 C 0.3724(6) 0.1127(5) 0.5389(4) 0.067(2) Uani 1 1 d . . . H39A H 0.4095 0.0705 0.5412 0.081 Uiso 1 1 calc R . . H39B H 0.3029 0.0889 0.4923 0.081 Uiso 1 1 calc R . . C40 C 0.3947(6) 0.2689(5) 0.5242(4) 0.0607(18) Uani 1 1 d . . . H40A H 0.3293 0.2485 0.54 0.073 Uiso 1 1 calc R . . H40B H 0.3612 0.2601 0.4706 0.073 Uiso 1 1 calc R . . C41 C 0.4719(7) 0.3729(6) 0.5595(5) 0.080(2) Uani 1 1 d . . . H41A H 0.5228 0.3997 0.5337 0.097 Uiso 1 1 calc R . . H41B H 0.423 0.4057 0.5572 0.097 Uiso 1 1 calc R . . C42 C 0.8872(6) 0.4974(5) 0.6372(4) 0.0607(17) Uani 1 1 d . . . H42A H 0.9286 0.5604 0.6325 0.073 Uiso 1 1 calc R . . H42B H 0.8595 0.502 0.6765 0.073 Uiso 1 1 calc R . . C43 C 1.1374(6) 0.4550(5) 0.7600(3) 0.0511(15) Uani 1 1 d . . . C44 C 1.2532(6) 0.4979(6) 0.8079(4) 0.0672(19) Uani 1 1 d . . . H44 H 1.2943 0.5631 0.8224 0.081 Uiso 1 1 calc R . . C45 C 1.3085(7) 0.4426(7) 0.8346(4) 0.077(2) Uani 1 1 d . . . H45 H 1.3876 0.4697 0.868 0.092 Uiso 1 1 calc R . . C46 C 1.2426(7) 0.3440(7) 0.8102(4) 0.073(2) Uani 1 1 d . . . H46 H 1.2779 0.3049 0.8263 0.087 Uiso 1 1 calc R . . C47 C 1.1282(7) 0.3076(6) 0.7633(4) 0.0624(18) Uani 1 1 d . . . H47 H 1.0855 0.2426 0.7468 0.075 Uiso 1 1 calc R . . C48 C 1.0693(5) 0.5089(5) 0.7305(3) 0.0520(15) Uani 1 1 d . . . H48A H 1.0376 0.5232 0.7655 0.062 Uiso 1 1 calc R . . H48B H 1.1218 0.5678 0.725 0.062 Uiso 1 1 calc R . . C49 C 1.0193(6) 0.4481(5) 0.6005(4) 0.0615(18) Uani 1 1 d . . . H49A H 1.0972 0.4502 0.6247 0.074 Uiso 1 1 calc R . . H49B H 1.0295 0.5027 0.5799 0.074 Uiso 1 1 calc R . . C50 C 0.9442(6) 0.3617(5) 0.5382(4) 0.0628(18) Uani 1 1 d . . . H50A H 0.8747 0.3662 0.5048 0.075 Uiso 1 1 calc R . . H50B H 0.9888 0.3537 0.51 0.075 Uiso 1 1 calc R . . C51 C 0.8329(8) 0.1971(6) 0.5156(5) 0.090(3) Uani 1 1 d . . . H51A H 0.8112 0.1468 0.5397 0.134 Uiso 1 1 calc R . . H51B H 0.8737 0.1856 0.4865 0.134 Uiso 1 1 calc R . . H51C H 0.7627 0.2005 0.4838 0.134 Uiso 1 1 calc R . . C52 C 0.6253(8) 0.4821(8) 0.6715(6) 0.134(5) Uani 1 1 d . . . H52A H 0.673 0.4886 0.7225 0.201 Uiso 1 1 calc R . . H52B H 0.5808 0.5178 0.6698 0.201 Uiso 1 1 calc R . . H52C H 0.6758 0.505 0.6454 0.201 Uiso 1 1 calc R . . N1A N 1.0892(4) 0.2598(3) 1.0147(2) 0.0390(10) Uani 1 1 d . . . N1B N 0.4559(4) 0.2070(4) 0.5417(3) 0.0524(13) Uani 1 1 d . . . N2A N 0.9153(4) 0.2911(3) 1.0428(2) 0.0371(10) Uani 1 1 d . . . N2B N 0.4209(5) 0.1786(4) 0.6671(3) 0.0615(15) Uani 1 1 d . . . N3A N 0.5769(4) -0.0321(3) 0.8866(3) 0.0442(11) Uani 1 1 d . . . N3B N 0.9703(4) 0.4540(4) 0.6572(3) 0.0515(13) Uani 1 1 d . . . N4A N 0.6800(4) -0.0893(4) 0.8035(3) 0.0498(12) Uani 1 1 d . . . N4B N 1.0722(5) 0.3610(4) 0.7389(3) 0.0539(13) Uani 1 1 d . . . O1A O 0.8236(3) 0.1242(3) 0.9222(2) 0.0414(9) Uani 1 1 d . . . O1B O 0.7209(3) 0.3148(3) 0.6214(2) 0.0466(10) Uani 1 1 d . . . O2A O 0.9662(3) 0.2361(3) 0.8480(2) 0.0419(9) Uani 1 1 d . . . H2A H 0.892 0.2056 0.8054 0.05 Uiso 1 1 d R . . H2B H 1.0029 0.1943 0.8564 0.05 Uiso 1 1 d R . . O2B O 0.6735(4) 0.3222(3) 0.7651(2) 0.0550(11) Uani 1 1 d . . . O3A O 0.7533(4) 0.0874(3) 0.7548(2) 0.0603(12) Uani 1 1 d . . . O3B O 0.8855(3) 0.3629(3) 0.7811(2) 0.0426(9) Uani 1 1 d . . . O4A O 1.0970(3) 0.4102(3) 0.9605(2) 0.0454(9) Uani 1 1 d . . . O4B O 0.5423(5) 0.3814(4) 0.6359(3) 0.0777(15) Uani 1 1 d . . . O5A O 0.4678(4) -0.0395(3) 0.7351(2) 0.0658(13) Uani 1 1 d . . . O5B O 0.9098(4) 0.2847(3) 0.5713(2) 0.0624(12) Uani 1 1 d . . . O6A O 0.6144(4) 0.1434(3) 0.8250(2) 0.0540(11) Uani 1 1 d . . . H6A H 0.679 0.205 0.8398 0.065 Uiso 1 1 d R . . H6B H 0.5591 0.1333 0.7754 0.065 Uiso 1 1 d R . . O6B O 0.8273(4) 0.1832(3) 0.6737(2) 0.0549(11) Uani 1 1 d . . . O7A O 0.8163(3) 0.3156(3) 0.8832(2) 0.0396(8) Uani 1 1 d . . . O7B O 0.6154(4) 0.1391(3) 0.6662(3) 0.0609(12) Uani 1 1 d . . . P3 P 0.94765(19) -0.21616(15) 0.61901(10) 0.0657(5) Uani 1 1 d . . . F1 F 1.0256(5) -0.2714(4) 0.6244(3) 0.1010(16) Uani 1 1 d . . . F2 F 0.8627(6) -0.2784(5) 0.5374(3) 0.128(2) Uani 1 1 d . . . F3 F 0.8681(6) -0.2904(4) 0.6508(3) 0.1146(19) Uani 1 1 d . . . F4 F 1.0317(5) -0.1560(3) 0.7016(2) 0.0918(15) Uani 1 1 d . . . F5 F 1.0273(6) -0.1433(4) 0.5885(4) 0.121(2) Uani 1 1 d . . . F6 F 0.8728(5) -0.1576(4) 0.6133(3) 0.1095(18) Uani 1 1 d . . . P4 P 0.48913(15) 0.29125(13) 0.97796(10) 0.0560(4) Uani 1 1 d . . . F7 F 0.5177(3) 0.2023(3) 0.9845(2) 0.0691(11) Uani 1 1 d . A . F8 F 0.4371(10) 0.2624(8) 0.8914(3) 0.125(4) Uani 0.785(11) 1 d P A 1 F9 F 0.3616(5) 0.2270(4) 0.9765(4) 0.084(2) Uani 0.785(11) 1 d P A 1 F10 F 0.5322(9) 0.3150(4) 1.0680(3) 0.118(4) Uani 0.785(11) 1 d P A 1 F11 F 0.6172(6) 0.3588(6) 0.9917(8) 0.145(6) Uani 0.785(11) 1 d P A 1 F8' F 0.384(3) 0.233(2) 0.9087(18) 0.096(9) Uiso 0.215(11) 1 d P A 2 F9' F 0.437(2) 0.2874(18) 1.0292(15) 0.079(7) Uiso 0.215(11) 1 d P A 2 F10' F 0.6087(19) 0.3460(16) 1.0416(11) 0.061(6) Uiso 0.215(11) 1 d P A 2 F11' F 0.5781(19) 0.3016(16) 0.9269(12) 0.070(7) Uiso 0.215(11) 1 d P A 2 F12 F 0.4597(4) 0.3788(3) 0.9739(3) 0.0957(16) Uani 1 1 d . A . F13 F 0.6708(4) 0.0244(3) 0.6202(2) 0.0731(12) Uani 1 1 d . . . F14 F 0.8368(3) 0.4649(2) 0.85081(19) 0.0557(9) Uani 1 1 d . . . P1 P 0.71817(16) 0.11543(12) 0.68221(9) 0.0514(4) Uani 1 1 d . . . P2 P 0.80100(13) 0.35911(11) 0.81662(8) 0.0406(3) Uani 1 1 d . . . Zn1 Zn 0.67974(7) 0.04301(6) 0.82745(4) 0.0472(2) Uani 1 1 d . . . Zn2 Zn 0.93599(6) 0.27174(5) 0.94137(4) 0.03868(19) Uani 1 1 d . . . Zn3 Zn 0.88398(7) 0.31778(6) 0.67710(4) 0.0451(2) Uani 1 1 d . . . Zn4 Zn 0.58593(7) 0.25771(6) 0.65678(4) 0.0467(2) Uani 1 1 d . . . Br1 Br 0.93500(7) -0.04453(5) 1.18593(4) 0.0561(2) Uani 1 1 d . . . Br2 Br 0.65140(7) 0.47054(8) 0.34892(5) 0.0874(3) 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 C1 0.052(4) 0.043(3) 0.047(3) 0.007(3) 0.023(3) 0.025(3) C2 0.050(3) 0.041(3) 0.050(3) 0.009(3) 0.026(3) 0.026(3) C3 0.050(3) 0.042(3) 0.046(3) 0.005(3) 0.026(3) 0.026(3) C4 0.049(3) 0.034(3) 0.036(3) 0.001(2) 0.019(3) 0.019(3) C5 0.043(3) 0.043(3) 0.039(3) -0.003(3) 0.019(3) 0.017(3) C6 0.054(4) 0.039(3) 0.047(3) 0.003(3) 0.028(3) 0.021(3) C7 0.045(3) 0.051(3) 0.050(3) 0.011(3) 0.022(3) 0.032(3) C8 0.040(3) 0.043(3) 0.038(3) -0.001(2) 0.013(3) 0.020(3) C9 0.049(3) 0.061(4) 0.038(3) 0.010(3) 0.016(3) 0.030(3) C10 0.063(4) 0.066(4) 0.047(4) 0.014(3) 0.032(3) 0.034(4) C11 0.054(4) 0.055(4) 0.048(3) 0.011(3) 0.030(3) 0.029(3) C12 0.043(3) 0.042(3) 0.043(3) 0.003(3) 0.017(3) 0.023(3) C13 0.042(3) 0.052(3) 0.036(3) 0.000(3) 0.011(3) 0.023(3) C14 0.038(3) 0.056(4) 0.048(3) 0.010(3) 0.017(3) 0.024(3) C15 0.039(3) 0.052(4) 0.051(3) 0.009(3) 0.019(3) 0.019(3) C16 0.047(3) 0.046(4) 0.046(3) -0.003(3) 0.005(3) 0.021(3) C17 0.063(4) 0.052(4) 0.050(4) -0.006(3) 0.006(3) 0.026(3) C18 0.074(5) 0.066(5) 0.066(5) -0.015(4) 0.000(4) 0.045(4) C19 0.058(4) 0.082(5) 0.050(4) -0.014(4) 0.003(3) 0.042(4) C20 0.053(4) 0.072(5) 0.046(4) -0.007(3) 0.012(3) 0.034(4) C21 0.068(4) 0.046(4) 0.050(4) 0.002(3) 0.021(3) 0.019(3) C22 0.045(4) 0.058(4) 0.053(4) 0.003(3) 0.014(3) 0.019(3) C23 0.060(4) 0.066(5) 0.056(4) 0.000(4) 0.017(4) 0.014(4) C24 0.042(3) 0.044(3) 0.046(3) 0.002(3) 0.023(3) 0.016(3) C25 0.086(6) 0.095(6) 0.056(5) -0.013(4) 0.015(4) 0.023(5) C26 0.053(4) 0.042(3) 0.041(3) 0.003(3) 0.016(3) 0.018(3) C27 0.055(4) 0.096(6) 0.054(4) 0.028(4) 0.019(3) 0.036(4) C28 0.044(4) 0.091(5) 0.045(4) 0.008(4) 0.013(3) 0.029(4) C29 0.039(3) 0.074(4) 0.041(3) 0.007(3) 0.015(3) 0.025(3) C30 0.042(3) 0.067(4) 0.037(3) 0.010(3) 0.015(3) 0.024(3) C31 0.040(3) 0.075(5) 0.048(4) 0.018(3) 0.011(3) 0.025(3) C32 0.043(4) 0.088(5) 0.059(4) 0.021(4) 0.016(3) 0.024(4) C33 0.049(4) 0.071(4) 0.036(3) -0.009(3) 0.012(3) 0.021(3) C34 0.063(5) 0.079(5) 0.060(5) -0.004(4) 0.029(4) 0.013(4) C35 0.110(8) 0.109(8) 0.102(8) -0.022(6) 0.057(7) -0.001(7) C36 0.119(9) 0.119(9) 0.129(10) -0.021(8) 0.074(8) 0.000(7) C37 0.103(8) 0.113(8) 0.093(7) -0.004(6) 0.055(6) 0.016(7) C38 0.063(5) 0.094(6) 0.059(4) 0.001(4) 0.030(4) 0.028(4) C39 0.051(4) 0.073(5) 0.050(4) -0.012(3) 0.015(3) 0.010(4) C40 0.041(3) 0.083(5) 0.050(4) 0.005(3) 0.011(3) 0.028(4) C41 0.054(4) 0.102(6) 0.074(5) -0.003(5) 0.015(4) 0.036(4) C42 0.051(4) 0.065(4) 0.052(4) 0.011(3) 0.012(3) 0.020(3) C43 0.051(4) 0.055(4) 0.039(3) 0.003(3) 0.018(3) 0.017(3) C44 0.051(4) 0.082(5) 0.058(4) 0.010(4) 0.018(4) 0.023(4) C45 0.049(4) 0.118(7) 0.055(4) 0.016(5) 0.008(3) 0.038(5) C46 0.073(5) 0.105(7) 0.057(4) 0.027(4) 0.023(4) 0.059(5) C47 0.066(5) 0.077(5) 0.059(4) 0.018(4) 0.034(4) 0.038(4) C48 0.041(3) 0.054(4) 0.041(3) -0.001(3) 0.009(3) 0.011(3) C49 0.046(4) 0.083(5) 0.050(4) 0.015(4) 0.023(3) 0.020(4) C50 0.058(4) 0.077(5) 0.054(4) 0.013(4) 0.030(3) 0.024(4) C51 0.099(7) 0.082(6) 0.066(5) -0.015(4) 0.043(5) 0.015(5) C52 0.072(6) 0.147(10) 0.124(9) -0.078(8) -0.003(6) 0.047(6) N1A 0.032(2) 0.049(3) 0.040(2) 0.005(2) 0.016(2) 0.022(2) N1B 0.039(3) 0.065(3) 0.041(3) -0.002(2) 0.013(2) 0.016(3) N2A 0.036(2) 0.039(2) 0.040(2) 0.004(2) 0.016(2) 0.019(2) N2B 0.047(3) 0.082(4) 0.044(3) -0.005(3) 0.020(3) 0.020(3) N3A 0.043(3) 0.042(3) 0.042(3) -0.001(2) 0.018(2) 0.014(2) N3B 0.038(3) 0.069(3) 0.038(3) 0.003(2) 0.012(2) 0.020(3) N4A 0.046(3) 0.048(3) 0.046(3) -0.005(2) 0.014(2) 0.019(2) N4B 0.048(3) 0.068(4) 0.051(3) 0.006(3) 0.024(3) 0.028(3) O1A 0.046(2) 0.039(2) 0.042(2) 0.0043(17) 0.0197(18) 0.0205(18) O1B 0.039(2) 0.063(3) 0.035(2) 0.0054(19) 0.0111(17) 0.024(2) O2A 0.043(2) 0.047(2) 0.042(2) 0.0063(18) 0.0210(18) 0.0238(18) O2B 0.046(2) 0.080(3) 0.039(2) -0.001(2) 0.0160(19) 0.030(2) O3A 0.069(3) 0.061(3) 0.052(3) 0.012(2) 0.029(2) 0.026(2) O3B 0.041(2) 0.052(2) 0.0338(19) 0.0035(17) 0.0134(17) 0.0213(19) O4A 0.040(2) 0.041(2) 0.051(2) 0.0063(18) 0.0127(18) 0.0181(18) O4B 0.063(3) 0.078(3) 0.077(4) -0.007(3) 0.012(3) 0.035(3) O5A 0.066(3) 0.068(3) 0.045(2) -0.001(2) 0.015(2) 0.020(3) O5B 0.065(3) 0.065(3) 0.048(3) 0.000(2) 0.027(2) 0.018(2) O6A 0.045(2) 0.050(2) 0.059(3) 0.007(2) 0.012(2) 0.022(2) O6B 0.055(3) 0.052(3) 0.057(3) 0.007(2) 0.026(2) 0.021(2) O7A 0.039(2) 0.044(2) 0.039(2) 0.0034(17) 0.0167(17) 0.0224(18) O7B 0.062(3) 0.058(3) 0.058(3) 0.005(2) 0.027(2) 0.021(2) P3 0.0774(13) 0.0741(12) 0.0509(10) 0.0083(9) 0.0297(9) 0.0361(11) F1 0.120(4) 0.099(4) 0.117(4) 0.025(3) 0.060(4) 0.070(3) F2 0.158(6) 0.133(5) 0.065(3) -0.014(3) 0.015(3) 0.069(4) F3 0.131(5) 0.090(4) 0.128(5) 0.019(3) 0.087(4) 0.025(3) F4 0.113(4) 0.085(3) 0.059(3) 0.003(2) 0.016(3) 0.043(3) F5 0.174(6) 0.107(4) 0.126(5) 0.051(4) 0.105(5) 0.063(4) F6 0.108(4) 0.125(4) 0.102(4) 0.006(3) 0.025(3) 0.077(4) P4 0.0440(9) 0.0606(10) 0.0576(10) 0.0119(8) 0.0107(8) 0.0256(8) F7 0.058(2) 0.071(3) 0.091(3) 0.019(2) 0.032(2) 0.039(2) F8 0.198(10) 0.202(9) 0.049(4) 0.040(5) 0.058(5) 0.151(9) F9 0.055(3) 0.069(4) 0.147(6) 0.020(4) 0.053(4) 0.036(3) F10 0.182(9) 0.064(4) 0.053(4) 0.001(3) 0.006(5) 0.037(5) F11 0.052(4) 0.096(6) 0.313(17) 0.116(8) 0.082(6) 0.039(4) F12 0.085(3) 0.066(3) 0.117(4) 0.024(3) 0.009(3) 0.042(3) F13 0.075(3) 0.064(2) 0.058(2) -0.0239(19) 0.031(2) 0.014(2) F14 0.070(2) 0.053(2) 0.0457(19) 0.0014(16) 0.0155(17) 0.0361(19) P1 0.0641(10) 0.0494(9) 0.0383(8) -0.0020(7) 0.0204(8) 0.0250(8) P2 0.0408(8) 0.0475(8) 0.0311(7) -0.0023(6) 0.0116(6) 0.0218(7) Zn1 0.0536(5) 0.0459(4) 0.0416(4) 0.0013(3) 0.0211(4) 0.0212(4) Zn2 0.0399(4) 0.0442(4) 0.0357(4) 0.0041(3) 0.0174(3) 0.0214(3) Zn3 0.0413(4) 0.0533(5) 0.0356(4) -0.0011(3) 0.0095(3) 0.0230(4) Zn4 0.0391(4) 0.0588(5) 0.0357(4) -0.0012(4) 0.0132(3) 0.0189(4) Br1 0.0657(4) 0.0615(4) 0.0516(4) 0.0185(3) 0.0286(3) 0.0328(4) Br2 0.0558(5) 0.1398(9) 0.0667(5) 0.0496(5) 0.0204(4) 0.0412(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.367(8) . ? C1 C6 1.379(9) . ? C1 Br1 1.902(6) . ? C2 C3 1.411(8) . ? C2 H2 0.93 . ? C3 C4 1.411(8) . ? C3 C7 1.507(8) . ? C4 O1A 1.343(7) . ? C4 C5 1.398(8) . ? C5 C6 1.394(8) . ? C5 C24 1.500(8) . ? C6 H6 0.93 . ? C7 N1A 1.493(7) . ? C7 H7A 0.97 . ? C7 H7B 0.97 . ? C8 N2A 1.334(7) . ? C8 C9 1.388(8) . ? C8 C13 1.509(8) . ? C9 C10 1.374(9) . ? C9 H9 0.93 . ? C10 C11 1.382(9) . ? C10 H10 0.93 . ? C11 C12 1.382(8) . ? C11 H11 0.93 . ? C12 N2A 1.344(7) . ? C12 H12 0.93 . ? C13 N1A 1.491(7) . ? C13 H13A 0.97 . ? C13 H13B 0.97 . ? C14 N1A 1.473(7) . ? C14 C15 1.500(9) . ? C14 H14A 0.97 . ? C14 H14B 0.97 . ? C15 O4A 1.415(7) . ? C15 H15A 0.97 . ? C15 H15B 0.97 . ? C16 N4A 1.325(8) . ? C16 C17 1.384(9) . ? C16 C21 1.512(9) . ? C17 C18 1.392(11) . ? C17 H17 0.93 . ? C18 C19 1.377(11) . ? C18 H18 0.93 . ? C19 C20 1.368(10) . ? C19 H19 0.93 . ? C20 N4A 1.346(8) . ? C20 H20 0.93 . ? C21 N3A 1.479(8) . ? C21 H21A 0.97 . ? C21 H21B 0.97 . ? C22 C23 1.497(9) . ? C22 N3A 1.506(8) . ? C22 H22A 0.97 . ? C22 H22B 0.97 . ? C23 O5A 1.434(8) . ? C23 H23A 0.97 . ? C23 H23B 0.97 . ? C24 N3A 1.499(7) . ? C24 H24A 0.97 . ? C24 H24B 0.97 . ? C25 O5A 1.433(9) . ? C25 H25A 0.96 . ? C25 H25B 0.96 . ? C25 H25C 0.96 . ? C26 O4A 1.432(7) . ? C26 H26A 0.96 . ? C26 H26B 0.96 . ? C26 H26C 0.96 . ? C27 C32 1.383(10) . ? C27 C28 1.388(11) . ? C27 Br2 1.917(7) . ? C28 C29 1.378(9) . ? C28 H28 0.93 . ? C29 C30 1.405(9) . ? C29 C33 1.502(10) . ? C30 O1B 1.344(7) . ? C30 C31 1.391(9) . ? C31 C32 1.386(9) . ? C31 C42 1.518(9) . ? C32 H32 0.93 . ? C33 N1B 1.489(8) . ? C33 H33A 0.97 . ? C33 H33B 0.97 . ? C34 C35 1.312(12) . ? C34 N2B 1.346(9) . ? C34 C39 1.508(10) . ? C35 C36 1.427(15) . ? C35 H35 0.93 . ? C36 C37 1.393(14) . ? C36 H36 0.93 . ? C37 C38 1.318(12) . ? C37 H37 0.93 . ? C38 N2B 1.355(9) . ? C38 H38 0.93 . ? C39 N1B 1.466(9) . ? C39 H39A 0.97 . ? C39 H39B 0.97 . ? C40 N1B 1.495(9) . ? C40 C41 1.515(11) . ? C40 H40A 0.97 . ? C40 H40B 0.97 . ? C41 O4B 1.440(9) . ? C41 H41A 0.97 . ? C41 H41B 0.97 . ? C42 N3B 1.480(9) . ? C42 H42A 0.97 . ? C42 H42B 0.97 . ? C43 N4B 1.348(8) . ? C43 C44 1.357(9) . ? C43 C48 1.489(9) . ? C44 C45 1.381(11) . ? C44 H44 0.93 . ? C45 C46 1.412(12) . ? C45 H45 0.93 . ? C46 C47 1.341(10) . ? C46 H46 0.93 . ? C47 N4B 1.349(9) . ? C47 H47 0.93 . ? C48 N3B 1.486(7) . ? C48 H48A 0.97 . ? C48 H48B 0.97 . ? C49 N3B 1.480(8) . ? C49 C50 1.493(10) . ? C49 H49A 0.97 . ? C49 H49B 0.97 . ? C50 O5B 1.426(8) . ? C50 H50A 0.97 . ? C50 H50B 0.97 . ? C51 O5B 1.444(9) . ? C51 H51A 0.96 . ? C51 H51B 0.96 . ? C51 H51C 0.96 . ? C52 O4B 1.487(11) . ? C52 H52A 0.96 . ? C52 H52B 0.96 . ? C52 H52C 0.96 . ? N1A Zn2 2.156(4) . ? N1B Zn4 2.182(5) . ? N2A Zn2 2.114(4) . ? N2B Zn4 2.159(6) . ? N3A Zn1 2.164(5) . ? N3B Zn3 2.165(6) . ? N4A Zn1 2.118(5) . ? N4B Zn3 2.173(5) . ? O1A Zn1 2.028(4) . ? O1A Zn2 2.159(4) . ? O1B Zn4 2.054(4) . ? O1B Zn3 2.057(4) . ? O2A Zn2 2.083(4) . ? O2A H2A 0.96 . ? O2A H2B 0.96 . ? O2B P2 1.495(4) . ? O2B Zn4 1.999(4) . ? O3A P1 1.508(5) . ? O3A Zn1 2.015(4) . ? O3B P2 1.493(4) . ? O3B Zn3 2.099(4) . ? O4A Zn2 2.296(4) . ? O4B Zn4 2.285(5) . ? O5B Zn3 2.269(4) . ? O6A Zn1 2.086(4) . ? O6A H6A 0.96 . ? O6A H6B 0.96 . ? O6B P1 1.512(5) . ? O6B Zn3 1.962(4) . ? O7A P2 1.520(4) . ? O7A Zn2 2.024(4) . ? O7B P1 1.495(5) . ? O7B Zn4 2.078(5) . ? P3 F5 1.555(6) . ? P3 F2 1.579(6) . ? P3 F1 1.581(5) . ? P3 F4 1.583(5) . ? P3 F3 1.583(6) . ? P3 F6 1.589(5) . ? P4 F9' 1.39(2) . ? P4 F8' 1.48(3) . ? P4 F10' 1.51(2) . ? P4 F11 1.539(6) . ? P4 F8 1.555(6) . ? P4 F12 1.585(5) . ? P4 F9 1.598(6) . ? P4 F7 1.603(4) . ? P4 F10 1.627(7) . ? P4 F11' 1.76(2) . ? F13 P1 1.570(4) . ? F14 P2 1.577(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 120.6(6) . . ? C2 C1 Br1 119.0(5) . . ? C6 C1 Br1 120.4(5) . . ? C1 C2 C3 120.3(6) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? C2 C3 C4 119.4(5) . . ? C2 C3 C7 119.9(5) . . ? C4 C3 C7 120.6(5) . . ? O1A C4 C5 121.0(5) . . ? O1A C4 C3 119.7(5) . . ? C5 C4 C3 119.2(5) . . ? C6 C5 C4 119.8(5) . . ? C6 C5 C24 119.8(5) . . ? C4 C5 C24 120.4(5) . . ? C1 C6 C5 120.8(6) . . ? C1 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? N1A C7 C3 111.7(4) . . ? N1A C7 H7A 109.3 . . ? C3 C7 H7A 109.3 . . ? N1A C7 H7B 109.3 . . ? C3 C7 H7B 109.3 . . ? H7A C7 H7B 107.9 . . ? N2A C8 C9 121.9(5) . . ? N2A C8 C13 115.8(5) . . ? C9 C8 C13 122.3(5) . . ? C10 C9 C8 119.2(6) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C9 C10 C11 119.5(6) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C12 C11 C10 118.0(6) . . ? C12 C11 H11 121 . . ? C10 C11 H11 121 . . ? N2A C12 C11 123.0(6) . . ? N2A C12 H12 118.5 . . ? C11 C12 H12 118.5 . . ? N1A C13 C8 111.8(4) . . ? N1A C13 H13A 109.3 . . ? C8 C13 H13A 109.3 . . ? N1A C13 H13B 109.3 . . ? C8 C13 H13B 109.3 . . ? H13A C13 H13B 107.9 . . ? N1A C14 C15 111.3(5) . . ? N1A C14 H14A 109.4 . . ? C15 C14 H14A 109.4 . . ? N1A C14 H14B 109.4 . . ? C15 C14 H14B 109.4 . . ? H14A C14 H14B 108 . . ? O4A C15 C14 108.5(5) . . ? O4A C15 H15A 110 . . ? C14 C15 H15A 110 . . ? O4A C15 H15B 110 . . ? C14 C15 H15B 110 . . ? H15A C15 H15B 108.4 . . ? N4A C16 C17 122.2(6) . . ? N4A C16 C21 117.5(5) . . ? C17 C16 C21 120.2(7) . . ? C16 C17 C18 118.1(8) . . ? C16 C17 H17 121 . . ? C18 C17 H17 121 . . ? C19 C18 C17 119.6(7) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C20 C19 C18 118.6(7) . . ? C20 C19 H19 120.7 . . ? C18 C19 H19 120.7 . . ? N4A C20 C19 122.3(8) . . ? N4A C20 H20 118.9 . . ? C19 C20 H20 118.9 . . ? N3A C21 C16 114.0(5) . . ? N3A C21 H21A 108.8 . . ? C16 C21 H21A 108.8 . . ? N3A C21 H21B 108.8 . . ? C16 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? C23 C22 N3A 111.9(6) . . ? C23 C22 H22A 109.2 . . ? N3A C22 H22A 109.2 . . ? C23 C22 H22B 109.2 . . ? N3A C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? O5A C23 C22 108.4(6) . . ? O5A C23 H23A 110 . . ? C22 C23 H23A 110 . . ? O5A C23 H23B 110 . . ? C22 C23 H23B 110 . . ? H23A C23 H23B 108.4 . . ? N3A C24 C5 112.4(4) . . ? N3A C24 H24A 109.1 . . ? C5 C24 H24A 109.1 . . ? N3A C24 H24B 109.1 . . ? C5 C24 H24B 109.1 . . ? H24A C24 H24B 107.8 . . ? O5A C25 H25A 109.5 . . ? O5A C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O5A C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O4A C26 H26A 109.5 . . ? O4A C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O4A C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C32 C27 C28 121.3(7) . . ? C32 C27 Br2 119.0(6) . . ? C28 C27 Br2 119.7(5) . . ? C29 C28 C27 119.9(6) . . ? C29 C28 H28 120 . . ? C27 C28 H28 120 . . ? C28 C29 C30 119.5(6) . . ? C28 C29 C33 120.4(6) . . ? C30 C29 C33 120.0(6) . . ? O1B C30 C31 120.1(5) . . ? O1B C30 C29 120.4(6) . . ? C31 C30 C29 119.5(6) . . ? C32 C31 C30 120.8(6) . . ? C32 C31 C42 120.2(6) . . ? C30 C31 C42 119.0(6) . . ? C27 C32 C31 118.8(7) . . ? C27 C32 H32 120.6 . . ? C31 C32 H32 120.6 . . ? N1B C33 C29 112.2(5) . . ? N1B C33 H33A 109.2 . . ? C29 C33 H33A 109.2 . . ? N1B C33 H33B 109.2 . . ? C29 C33 H33B 109.2 . . ? H33A C33 H33B 107.9 . . ? C35 C34 N2B 121.1(8) . . ? C35 C34 C39 123.4(8) . . ? N2B C34 C39 115.1(6) . . ? C34 C35 C36 120.3(10) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C37 C36 C35 116.8(10) . . ? C37 C36 H36 121.6 . . ? C35 C36 H36 121.6 . . ? C38 C37 C36 119.9(10) . . ? C38 C37 H37 120 . . ? C36 C37 H37 120 . . ? C37 C38 N2B 121.6(8) . . ? C37 C38 H38 119.2 . . ? N2B C38 H38 119.2 . . ? N1B C39 C34 109.8(6) . . ? N1B C39 H39A 109.7 . . ? C34 C39 H39A 109.7 . . ? N1B C39 H39B 109.7 . . ? C34 C39 H39B 109.7 . . ? H39A C39 H39B 108.2 . . ? N1B C40 C41 115.5(6) . . ? N1B C40 H40A 108.4 . . ? C41 C40 H40A 108.4 . . ? N1B C40 H40B 108.4 . . ? C41 C40 H40B 108.4 . . ? H40A C40 H40B 107.5 . . ? O4B C41 C40 106.8(7) . . ? O4B C41 H41A 110.4 . . ? C40 C41 H41A 110.4 . . ? O4B C41 H41B 110.4 . . ? C40 C41 H41B 110.4 . . ? H41A C41 H41B 108.6 . . ? N3B C42 C31 111.3(6) . . ? N3B C42 H42A 109.4 . . ? C31 C42 H42A 109.4 . . ? N3B C42 H42B 109.4 . . ? C31 C42 H42B 109.4 . . ? H42A C42 H42B 108 . . ? N4B C43 C44 123.4(7) . . ? N4B C43 C48 114.2(5) . . ? C44 C43 C48 122.2(6) . . ? C43 C44 C45 118.5(8) . . ? C43 C44 H44 120.8 . . ? C45 C44 H44 120.8 . . ? C44 C45 C46 118.6(7) . . ? C44 C45 H45 120.7 . . ? C46 C45 H45 120.7 . . ? C47 C46 C45 118.9(7) . . ? C47 C46 H46 120.6 . . ? C45 C46 H46 120.6 . . ? C46 C47 N4B 123.0(8) . . ? C46 C47 H47 118.5 . . ? N4B C47 H47 118.5 . . ? N3B C48 C43 110.6(5) . . ? N3B C48 H48A 109.5 . . ? C43 C48 H48A 109.5 . . ? N3B C48 H48B 109.5 . . ? C43 C48 H48B 109.5 . . ? H48A C48 H48B 108.1 . . ? N3B C49 C50 114.2(6) . . ? N3B C49 H49A 108.7 . . ? C50 C49 H49A 108.7 . . ? N3B C49 H49B 108.7 . . ? C50 C49 H49B 108.7 . . ? H49A C49 H49B 107.6 . . ? O5B C50 C49 106.6(6) . . ? O5B C50 H50A 110.4 . . ? C49 C50 H50A 110.4 . . ? O5B C50 H50B 110.4 . . ? C49 C50 H50B 110.4 . . ? H50A C50 H50B 108.6 . . ? O5B C51 H51A 109.5 . . ? O5B C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? O5B C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O4B C52 H52A 109.5 . . ? O4B C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? O4B C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C14 N1A C13 111.3(4) . . ? C14 N1A C7 108.3(4) . . ? C13 N1A C7 112.1(5) . . ? C14 N1A Zn2 109.1(3) . . ? C13 N1A Zn2 108.2(3) . . ? C7 N1A Zn2 107.9(3) . . ? C39 N1B C33 110.2(5) . . ? C39 N1B C40 110.9(5) . . ? C33 N1B C40 111.7(5) . . ? C39 N1B Zn4 103.7(4) . . ? C33 N1B Zn4 109.6(4) . . ? C40 N1B Zn4 110.5(4) . . ? C8 N2A C12 118.4(5) . . ? C8 N2A Zn2 114.6(3) . . ? C12 N2A Zn2 123.9(4) . . ? C34 N2B C38 119.5(6) . . ? C34 N2B Zn4 113.2(5) . . ? C38 N2B Zn4 127.2(5) . . ? C21 N3A C24 110.8(5) . . ? C21 N3A C22 110.7(5) . . ? C24 N3A C22 107.9(4) . . ? C21 N3A Zn1 110.7(4) . . ? C24 N3A Zn1 107.4(3) . . ? C22 N3A Zn1 109.2(4) . . ? C49 N3B C42 112.1(5) . . ? C49 N3B C48 109.4(5) . . ? C42 N3B C48 109.9(5) . . ? C49 N3B Zn3 111.8(4) . . ? C42 N3B Zn3 109.9(4) . . ? C48 N3B Zn3 103.4(4) . . ? C16 N4A C20 119.2(6) . . ? C16 N4A Zn1 116.1(4) . . ? C20 N4A Zn1 124.1(5) . . ? C43 N4B C47 117.5(6) . . ? C43 N4B Zn3 113.4(4) . . ? C47 N4B Zn3 128.8(5) . . ? C4 O1A Zn1 118.8(3) . . ? C4 O1A Zn2 115.4(3) . . ? Zn1 O1A Zn2 125.56(19) . . ? C30 O1B Zn4 120.6(3) . . ? C30 O1B Zn3 118.7(4) . . ? Zn4 O1B Zn3 120.67(19) . . ? Zn2 O2A H2A 109.5 . . ? Zn2 O2A H2B 109.3 . . ? H2A O2A H2B 109.5 . . ? P2 O2B Zn4 132.3(2) . . ? P1 O3A Zn1 137.2(3) . . ? P2 O3B Zn3 139.9(2) . . ? C15 O4A C26 111.4(5) . . ? C15 O4A Zn2 115.5(3) . . ? C26 O4A Zn2 131.7(3) . . ? C41 O4B C52 108.7(8) . . ? C41 O4B Zn4 115.0(5) . . ? C52 O4B Zn4 125.4(5) . . ? C25 O5A C23 111.5(6) . . ? C50 O5B C51 111.5(6) . . ? C50 O5B Zn3 115.1(4) . . ? C51 O5B Zn3 122.4(4) . . ? Zn1 O6A H6A 109.5 . . ? Zn1 O6A H6B 109.4 . . ? H6A O6A H6B 109.5 . . ? P1 O6B Zn3 130.2(3) . . ? P2 O7A Zn2 134.3(2) . . ? P1 O7B Zn4 137.2(3) . . ? F5 P3 F2 90.7(4) . . ? F5 P3 F1 89.2(3) . . ? F2 P3 F1 89.4(3) . . ? F5 P3 F4 90.6(3) . . ? F2 P3 F4 178.5(4) . . ? F1 P3 F4 90.1(3) . . ? F5 P3 F3 179.2(4) . . ? F2 P3 F3 89.8(4) . . ? F1 P3 F3 90.1(3) . . ? F4 P3 F3 88.9(3) . . ? F5 P3 F6 88.8(4) . . ? F2 P3 F6 91.2(3) . . ? F1 P3 F6 178.0(4) . . ? F4 P3 F6 89.4(3) . . ? F3 P3 F6 91.8(4) . . ? F9' P4 F8' 101.1(17) . . ? F9' P4 F10' 88.3(14) . . ? F8' P4 F10' 169.6(15) . . ? F9' P4 F11 125.6(13) . . ? F8' P4 F11 131.9(14) . . ? F10' P4 F11 40.3(8) . . ? F9' P4 F8 132.9(12) . . ? F8' P4 F8 33.4(11) . . ? F10' P4 F8 138.2(10) . . ? F11 P4 F8 98.4(7) . . ? F9' P4 F12 78.0(10) . . ? F8' P4 F12 92.3(12) . . ? F10' P4 F12 93.9(8) . . ? F11 P4 F12 87.3(3) . . ? F8 P4 F12 89.5(4) . . ? F9' P4 F9 46.0(12) . . ? F8' P4 F9 56.5(12) . . ? F10' P4 F9 131.6(10) . . ? F11 P4 F9 171.5(6) . . ? F8 P4 F9 89.9(5) . . ? F12 P4 F9 91.2(3) . . ? F9' P4 F7 100.1(10) . . ? F8' P4 F7 88.4(12) . . ? F10' P4 F7 85.7(8) . . ? F11 P4 F7 93.6(3) . . ? F8 P4 F7 92.1(3) . . ? F12 P4 F7 178.1(3) . . ? F9 P4 F7 87.6(3) . . ? F9' P4 F10 42.5(11) . . ? F8' P4 F10 141.5(13) . . ? F10' P4 F10 46.8(8) . . ? F11 P4 F10 86.6(6) . . ? F8 P4 F10 175.0(6) . . ? F12 P4 F10 91.0(3) . . ? F9 P4 F10 85.1(4) . . ? F7 P4 F10 87.3(3) . . ? F9' P4 F11' 169.9(13) . . ? F8' P4 F11' 88.3(14) . . ? F10' P4 F11' 82.0(11) . . ? F11 P4 F11' 46.2(7) . . ? F8 P4 F11' 57.1(8) . . ? F12 P4 F11' 105.4(8) . . ? F9 P4 F11' 142.0(8) . . ? F7 P4 F11' 76.4(7) . . ? F10 P4 F11' 127.4(8) . . ? O7B P1 O3A 113.9(3) . . ? O7B P1 O6B 118.0(3) . . ? O3A P1 O6B 110.1(3) . . ? O7B P1 F13 104.6(3) . . ? O3A P1 F13 105.1(3) . . ? O6B P1 F13 103.6(2) . . ? O3B P2 O2B 116.2(2) . . ? O3B P2 O7A 113.9(2) . . ? O2B P2 O7A 112.0(2) . . ? O3B P2 F14 105.1(2) . . ? O2B P2 F14 103.6(2) . . ? O7A P2 F14 104.3(2) . . ? O3A Zn1 O1A 97.42(18) . . ? O3A Zn1 O6A 93.12(19) . . ? O1A Zn1 O6A 91.46(16) . . ? O3A Zn1 N4A 91.2(2) . . ? O1A Zn1 N4A 108.47(17) . . ? O6A Zn1 N4A 158.89(19) . . ? O3A Zn1 N3A 167.66(18) . . ? O1A Zn1 N3A 93.55(17) . . ? O6A Zn1 N3A 92.24(18) . . ? N4A Zn1 N3A 79.95(19) . . ? O7A Zn2 O2A 92.17(15) . . ? O7A Zn2 N2A 96.66(16) . . ? O2A Zn2 N2A 170.32(16) . . ? O7A Zn2 N1A 166.52(17) . . ? O2A Zn2 N1A 91.92(16) . . ? N2A Zn2 N1A 80.38(17) . . ? O7A Zn2 O1A 100.99(15) . . ? O2A Zn2 O1A 87.30(15) . . ? N2A Zn2 O1A 87.13(16) . . ? N1A Zn2 O1A 92.02(17) . . ? O7A Zn2 O4A 94.05(15) . . ? O2A Zn2 O4A 81.96(15) . . ? N2A Zn2 O4A 101.30(16) . . ? N1A Zn2 O4A 73.83(16) . . ? O1A Zn2 O4A 161.83(14) . . ? O6B Zn3 O1B 97.20(18) . . ? O6B Zn3 O3B 98.07(17) . . ? O1B Zn3 O3B 92.05(15) . . ? O6B Zn3 N3B 161.52(19) . . ? O1B Zn3 N3B 90.11(18) . . ? O3B Zn3 N3B 98.61(17) . . ? O6B Zn3 N4B 98.1(2) . . ? O1B Zn3 N4B 164.7(2) . . ? O3B Zn3 N4B 84.72(17) . . ? N3B Zn3 N4B 75.6(2) . . ? O6B Zn3 O5B 86.84(18) . . ? O1B Zn3 O5B 93.85(16) . . ? O3B Zn3 O5B 171.80(17) . . ? N3B Zn3 O5B 75.71(18) . . ? N4B Zn3 O5B 88.10(18) . . ? O2B Zn4 O1B 99.51(17) . . ? O2B Zn4 O7B 95.88(19) . . ? O1B Zn4 O7B 91.53(17) . . ? O2B Zn4 N2B 93.98(19) . . ? O1B Zn4 N2B 166.47(18) . . ? O7B Zn4 N2B 86.1(2) . . ? O2B Zn4 N1B 162.55(19) . . ? O1B Zn4 N1B 90.36(17) . . ? O7B Zn4 N1B 98.2(2) . . ? N2B Zn4 N1B 76.8(2) . . ? O2B Zn4 O4B 89.09(19) . . ? O1B Zn4 O4B 88.42(19) . . ? O7B Zn4 O4B 174.97(18) . . ? N2B Zn4 O4B 92.8(2) . . ? N1B Zn4 O4B 76.8(2) . . ? #===END #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2011-06-15 at 18:15:19 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : 593_twin1_hklf4 593 struct data_593_twin1_hklf4 _database_code_depnum_ccdc_archive 'CCDC 830846' #TrackingRef 'supdata.cif' _audit_creation_date 2011-06-15T18:15:19-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C30 H38 Br1 F6 N4 O7 P1 Zn2' _chemical_formula_sum 'C30 H38 Br F6 N4 O7 P Zn2' _chemical_formula_weight 922.26 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9022(5) _cell_length_b 13.1115(7) _cell_length_c 16.6071(9) _cell_angle_alpha 99.071(5) _cell_angle_beta 91.761(4) _cell_angle_gamma 102.970(5) _cell_volume 1860.92(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7385 _cell_measurement_theta_min 3.5044 _cell_measurement_theta_max 60.2702 _cell_measurement_wavelength 1.54184 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.646 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 932 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.954 _exptl_absorpt_correction_type multi-scan _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_absorpt_correction_T_min 0.8732 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 16.0696 _diffrn_orient_matrix_ub_11 -0.0318582 _diffrn_orient_matrix_ub_12 -0.0966754 _diffrn_orient_matrix_ub_13 0.0442823 _diffrn_orient_matrix_ub_21 -0.0282703 _diffrn_orient_matrix_ub_22 -0.0749543 _diffrn_orient_matrix_ub_23 -0.0830912 _diffrn_orient_matrix_ub_31 0.1728335 _diffrn_orient_matrix_ub_32 -0.0008134 _diffrn_orient_matrix_ub_33 0.001235 _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_unetI/netI 0.0357 _diffrn_reflns_number 19461 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 60.57 _diffrn_reflns_theta_full 60.57 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 19461 _reflns_number_gt 14871 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.1181P)^2^+2.6022P] 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_number_reflns 19461 _refine_ls_number_parameters 478 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0924 _refine_ls_R_factor_gt 0.07 _refine_ls_wR_factor_ref 0.2067 _refine_ls_wR_factor_gt 0.1872 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.629 _refine_diff_density_min -0.613 _refine_diff_density_rms 0.092 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8030(6) -0.0162(4) 0.5736(3) 0.0671(13) Uani 1 1 d . . . C2 C 0.9426(6) 0.0104(4) 0.6194(3) 0.0641(12) Uani 1 1 d . . . H2 H 1.0125 -0.0327 0.6117 0.077 Uiso 1 1 calc R . . C3 C 0.9770(5) 0.1029(4) 0.6775(3) 0.0584(11) Uani 1 1 d . . . C4 C 0.8753(5) 0.1693(4) 0.6867(3) 0.0566(11) Uani 1 1 d . . . C5 C 0.7317(5) 0.1390(4) 0.6404(3) 0.0652(12) Uani 1 1 d . . . C6 C 0.6991(6) 0.0460(4) 0.5840(3) 0.0683(13) Uani 1 1 d . . . H6 H 0.6053 0.0258 0.5529 0.082 Uiso 1 1 calc R . . C7 C 1.1294(5) 0.1359(4) 0.7286(3) 0.0637(12) Uani 1 1 d . . . H7A H 1.1913 0.0848 0.7127 0.076 Uiso 1 1 calc R . . H7B H 1.1858 0.2046 0.7184 0.076 Uiso 1 1 calc R . . C8 C 1.0186(6) 0.0390(4) 0.8378(4) 0.0762(14) Uani 1 1 d . . . H8A H 1.0439 -0.0182 0.8001 0.091 Uiso 1 1 calc R . . H8B H 1.0546 0.0335 0.8923 0.091 Uiso 1 1 calc R . . C9 C 0.8498(7) 0.0234(5) 0.8348(4) 0.0937(18) Uani 1 1 d . . . H9A H 0.8081 0.0109 0.7785 0.112 Uiso 1 1 calc R . . H9B H 0.8041 -0.0376 0.8595 0.112 Uiso 1 1 calc R . . C10 C 0.6555(11) 0.1089(9) 0.8745(8) 0.174(5) Uani 1 1 d . . . H10A H 0.6329 0.1717 0.9048 0.261 Uiso 1 1 calc R . . H10B H 0.6055 0.0481 0.8972 0.261 Uiso 1 1 calc R . . H10C H 0.6185 0.1006 0.8184 0.261 Uiso 1 1 calc R . . C11 C 1.2579(5) 0.1774(5) 0.8652(3) 0.0735(14) Uani 1 1 d . . . H11A H 1.3246 0.233 0.8421 0.088 Uiso 1 1 calc R . . H11B H 1.3071 0.1181 0.8626 0.088 Uiso 1 1 calc R . . C12 C 1.2343(6) 0.2178(4) 0.9524(3) 0.0757(15) Uani 1 1 d . . . C13 C 1.3251(7) 0.2056(5) 1.0179(4) 0.0906(18) Uani 1 1 d . . . H13 H 1.4012 0.1675 1.009 0.109 Uiso 1 1 calc R . . C14 C 1.3029(10) 0.2493(6) 1.0951(4) 0.107(2) Uani 1 1 d . . . H14 H 1.3649 0.2423 1.1391 0.128 Uiso 1 1 calc R . . C15 C 1.1902(12) 0.3031(7) 1.1078(4) 0.121(3) Uani 1 1 d . . . H15 H 1.1749 0.334 1.1604 0.145 Uiso 1 1 calc R . . C16 C 1.0962(9) 0.3117(5) 1.0406(4) 0.0982(19) Uani 1 1 d . . . H16 H 1.0167 0.3469 1.0489 0.118 Uiso 1 1 calc R . . C17 C 0.6200(5) 0.2088(4) 0.6526(4) 0.0722(14) Uani 1 1 d . . . H17A H 0.5246 0.1741 0.6201 0.087 Uiso 1 1 calc R . . H17B H 0.5966 0.2183 0.7096 0.087 Uiso 1 1 calc R . . C18 C 0.7223(6) 0.3096(5) 0.5436(3) 0.0730(14) Uani 1 1 d . . . H18A H 0.7011 0.3708 0.5234 0.088 Uiso 1 1 calc R . . H18B H 0.6565 0.2466 0.5109 0.088 Uiso 1 1 calc R . . C19 C 0.8879(6) 0.3071(5) 0.5313(3) 0.0804(15) Uani 1 1 d . . . H19A H 0.9055 0.2387 0.5387 0.097 Uiso 1 1 calc R . . H19B H 0.9126 0.3183 0.4765 0.097 Uiso 1 1 calc R . . C20 C 1.1354(8) 0.4114(8) 0.5786(5) 0.136(3) Uani 1 1 d . . . H20A H 1.1876 0.4675 0.6213 0.204 Uiso 1 1 calc R . . H20B H 1.1524 0.4335 0.5265 0.204 Uiso 1 1 calc R . . H20C H 1.175 0.3494 0.5805 0.204 Uiso 1 1 calc R . . C21 C 0.5698(6) 0.3808(5) 0.6443(4) 0.0807(15) Uani 1 1 d . . . H21A H 0.5242 0.371 0.6957 0.097 Uiso 1 1 calc R . . H21B H 0.4875 0.3588 0.6012 0.097 Uiso 1 1 calc R . . C22 C 0.6445(6) 0.4972(5) 0.6476(3) 0.0737(14) Uani 1 1 d . . . C23 C 0.5712(7) 0.5708(5) 0.6260(4) 0.0866(17) Uani 1 1 d . . . H23 H 0.4682 0.55 0.6062 0.104 Uiso 1 1 calc R . . C24 C 0.6479(8) 0.6742(6) 0.6334(4) 0.0973(19) Uani 1 1 d . . . H24 H 0.5975 0.7244 0.6192 0.117 Uiso 1 1 calc R . . C25 C 0.8031(8) 0.7043(5) 0.6625(4) 0.0905(17) Uani 1 1 d . . . H25 H 0.8583 0.7745 0.6677 0.109 Uiso 1 1 calc R . . C26 C 0.8710(6) 0.6281(5) 0.6829(3) 0.0723(13) Uani 1 1 d . . . H26 H 0.9747 0.6472 0.7013 0.087 Uiso 1 1 calc R . . C27 C 0.7535(6) 0.3988(4) 0.8870(4) 0.0739(14) Uani 1 1 d . . . C28 C 0.6470(9) 0.4320(6) 0.9472(4) 0.105(2) Uani 1 1 d . . . H28A H 0.6723 0.4146 0.9992 0.158 Uiso 1 1 calc R . . H28B H 0.5426 0.3958 0.9288 0.158 Uiso 1 1 calc R . . H28C H 0.6571 0.5073 0.9526 0.158 Uiso 1 1 calc R . . C29 C 1.1872(6) 0.4752(5) 0.8041(3) 0.0730(14) Uani 1 1 d . . . C30 C 1.3345(7) 0.5596(6) 0.8138(4) 0.103(2) Uani 1 1 d . . . H30D H 1.4094 0.5405 0.8479 0.155 Uiso 1 1 calc R . . H30E H 1.315 0.6261 0.8387 0.155 Uiso 1 1 calc R . . H30F H 1.3735 0.566 0.7612 0.155 Uiso 1 1 calc R . . N1 N 0.6800(4) 0.3145(3) 0.6295(2) 0.0631(10) Uani 1 1 d . . . N2 N 0.7946(5) 0.5265(4) 0.6775(2) 0.0682(10) Uani 1 1 d . . . N3 N 1.1048(4) 0.1425(3) 0.8174(2) 0.0597(9) Uani 1 1 d . . . N4 N 1.1210(5) 0.2697(3) 0.9651(2) 0.0729(11) Uani 1 1 d . . . O1 O 0.9063(3) 0.2600(3) 0.74120(18) 0.0635(8) Uani 1 1 d . . . O2 O 0.8550(5) 0.3567(3) 0.9127(2) 0.0854(11) Uani 1 1 d . . . O3 O 0.7369(4) 0.4147(3) 0.8158(2) 0.0810(10) Uani 1 1 d . . . O4 O 0.9814(4) 0.3883(3) 0.5893(2) 0.0836(11) Uani 1 1 d . . . O5 O 0.8150(4) 0.1180(3) 0.8790(3) 0.0941(12) Uani 1 1 d . . . O6 O 1.1837(4) 0.3952(3) 0.8362(2) 0.0794(10) Uani 1 1 d . . . O7 O 1.0767(4) 0.4933(3) 0.7644(2) 0.0813(10) Uani 1 1 d . . . Zn1 Zn 0.99876(7) 0.27665(5) 0.85565(4) 0.0642(2) Uani 1 1 d . . . Zn2 Zn 0.87386(7) 0.40057(5) 0.71818(4) 0.06270(19) Uani 1 1 d . . . Br1 Br 0.75801(7) -0.14213(5) 0.49330(4) 0.0868(2) Uani 1 1 d . . . P1 P 0.67195(19) 0.15294(14) 0.28986(11) 0.0894(5) Uani 1 1 d . . . F1 F 0.6398(7) 0.0338(4) 0.2503(4) 0.181(3) Uani 1 1 d . . . F6 F 0.7066(5) 0.2740(3) 0.3318(3) 0.1187(12) Uani 1 1 d . . . F2 F 0.7883(12) 0.1883(8) 0.2218(6) 0.183(4) Uani 0.763(12) 1 d PD . . F3 F 0.8184(8) 0.1442(5) 0.3414(7) 0.147(4) Uani 0.763(12) 1 d PD . . F4 F 0.5719(10) 0.1343(6) 0.3640(4) 0.143(3) Uani 0.763(12) 1 d PD . . F5 F 0.5314(8) 0.1701(6) 0.2406(5) 0.141(4) Uani 0.763(12) 1 d PD . . F2' F 0.652(3) 0.176(2) 0.2026(11) 0.152(10) Uiso 0.237(12) 1 d PD . . F3' F 0.8387(18) 0.1533(19) 0.2805(17) 0.125(8) Uiso 0.237(12) 1 d PD . . F4' F 0.678(3) 0.101(2) 0.3725(10) 0.138(9) Uiso 0.237(12) 1 d PD . . F5' F 0.4843(17) 0.1237(18) 0.2970(15) 0.127(8) Uiso 0.237(12) 1 d PD . . 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 C1 0.073(3) 0.055(3) 0.062(3) 0.004(2) -0.008(2) -0.004(2) C2 0.071(3) 0.062(3) 0.057(3) 0.011(2) 0.000(2) 0.011(2) C3 0.057(3) 0.061(3) 0.057(3) 0.012(2) -0.0055(19) 0.013(2) C4 0.057(3) 0.058(3) 0.051(3) 0.013(2) -0.0058(18) 0.005(2) C5 0.057(3) 0.065(3) 0.070(3) 0.018(2) -0.009(2) 0.003(2) C6 0.064(3) 0.064(3) 0.069(3) 0.013(2) -0.019(2) 0.000(2) C7 0.058(3) 0.062(3) 0.072(3) 0.016(2) -0.006(2) 0.015(2) C8 0.090(4) 0.059(3) 0.080(4) 0.022(3) -0.006(3) 0.011(3) C9 0.091(4) 0.076(4) 0.108(5) 0.026(3) -0.003(3) 0.000(3) C10 0.119(7) 0.137(9) 0.242(13) 0.008(8) 0.056(7) -0.011(6) C11 0.055(3) 0.085(4) 0.077(3) 0.017(3) -0.016(2) 0.011(2) C12 0.084(4) 0.065(3) 0.063(3) 0.018(2) -0.024(2) -0.015(3) C13 0.094(4) 0.093(4) 0.078(4) 0.027(3) -0.029(3) 0.002(3) C14 0.134(6) 0.095(5) 0.073(5) 0.028(4) -0.038(4) -0.015(4) C15 0.182(8) 0.107(6) 0.051(4) 0.008(3) -0.020(4) -0.006(6) C16 0.144(6) 0.085(4) 0.058(4) 0.010(3) -0.006(3) 0.014(4) C17 0.054(3) 0.071(3) 0.088(4) 0.020(3) -0.010(2) 0.005(2) C18 0.068(3) 0.081(4) 0.063(3) 0.007(2) -0.016(2) 0.010(2) C19 0.085(4) 0.084(4) 0.068(3) 0.005(3) -0.003(3) 0.018(3) C20 0.074(5) 0.166(8) 0.135(7) -0.026(6) 0.022(4) -0.004(4) C21 0.062(3) 0.087(4) 0.098(4) 0.029(3) -0.002(3) 0.020(3) C22 0.070(3) 0.084(4) 0.077(3) 0.030(3) 0.011(2) 0.026(3) C23 0.071(3) 0.097(5) 0.110(5) 0.044(4) 0.017(3) 0.037(3) C24 0.100(5) 0.099(5) 0.119(5) 0.055(4) 0.026(4) 0.050(4) C25 0.109(5) 0.074(4) 0.100(4) 0.029(3) 0.015(3) 0.035(3) C26 0.072(3) 0.073(4) 0.072(3) 0.011(3) 0.010(2) 0.018(3) C27 0.077(3) 0.066(3) 0.082(4) 0.012(3) 0.013(3) 0.022(3) C28 0.123(5) 0.103(5) 0.101(5) 0.025(4) 0.029(4) 0.044(4) C29 0.076(3) 0.069(3) 0.063(3) 0.016(3) -0.016(2) -0.007(3) C30 0.090(4) 0.101(5) 0.105(5) 0.043(4) -0.031(3) -0.018(3) N1 0.055(2) 0.062(2) 0.072(3) 0.0163(19) -0.0065(17) 0.0115(18) N2 0.071(3) 0.070(3) 0.069(3) 0.0161(19) 0.0035(19) 0.023(2) N3 0.059(2) 0.062(2) 0.057(2) 0.0117(17) -0.0121(16) 0.0120(17) N4 0.092(3) 0.064(3) 0.057(3) 0.0097(19) -0.012(2) 0.009(2) O1 0.0637(18) 0.064(2) 0.0606(19) 0.0061(15) -0.0136(14) 0.0149(14) O2 0.110(3) 0.083(3) 0.064(2) 0.0066(18) 0.0022(19) 0.029(2) O3 0.093(3) 0.088(3) 0.075(3) 0.0217(19) 0.0203(18) 0.041(2) O4 0.062(2) 0.106(3) 0.073(2) 0.004(2) -0.0016(16) 0.0081(19) O5 0.070(3) 0.078(3) 0.128(3) 0.014(2) 0.017(2) 0.0044(19) O6 0.072(2) 0.073(2) 0.085(2) 0.0267(19) -0.0183(17) -0.0046(17) O7 0.076(2) 0.067(2) 0.096(3) 0.0249(19) -0.0242(19) 0.0020(17) Zn1 0.0714(4) 0.0605(4) 0.0575(4) 0.0093(3) -0.0092(3) 0.0108(3) Zn2 0.0609(4) 0.0610(4) 0.0651(4) 0.0124(3) -0.0082(3) 0.0125(3) Br1 0.1035(4) 0.0704(4) 0.0709(4) -0.0021(3) -0.0123(3) 0.0000(3) P1 0.0854(10) 0.0844(11) 0.1025(12) 0.0109(9) -0.0044(9) 0.0332(8) F1 0.163(4) 0.100(3) 0.260(7) -0.050(4) -0.073(4) 0.060(3) F6 0.129(3) 0.092(3) 0.134(3) 0.003(2) -0.009(2) 0.036(2) F2 0.182(9) 0.213(9) 0.147(7) 0.004(6) 0.069(6) 0.043(6) F3 0.111(5) 0.120(5) 0.206(9) 0.008(5) -0.064(5) 0.041(4) F4 0.163(7) 0.128(5) 0.147(6) 0.046(4) 0.039(5) 0.032(4) F5 0.146(6) 0.139(5) 0.144(6) -0.018(4) -0.066(5) 0.083(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.362(7) . ? C1 C2 1.382(7) . ? C1 Br1 1.907(5) . ? C2 C3 1.393(7) . ? C2 H2 0.93 . ? C3 C4 1.385(7) . ? C3 C7 1.517(6) . ? C4 O1 1.345(6) . ? C4 C5 1.414(6) . ? C5 C6 1.382(7) . ? C5 C17 1.494(8) . ? C6 H6 0.93 . ? C7 N3 1.489(6) . ? C7 H7A 0.97 . ? C7 H7B 0.97 . ? C8 C9 1.469(8) . ? C8 N3 1.496(7) . ? C8 H8A 0.97 . ? C8 H8B 0.97 . ? C9 O5 1.441(8) . ? C9 H9A 0.97 . ? C9 H9B 0.97 . ? C10 O5 1.396(10) . ? C10 H10A 0.96 . ? C10 H10B 0.96 . ? C10 H10C 0.96 . ? C11 N3 1.495(6) . ? C11 C12 1.500(8) . ? C11 H11A 0.97 . ? C11 H11B 0.97 . ? C12 N4 1.343(8) . ? C12 C13 1.386(8) . ? C13 C14 1.359(10) . ? C13 H13 0.93 . ? C14 C15 1.354(12) . ? C14 H14 0.93 . ? C15 C16 1.409(11) . ? C15 H15 0.93 . ? C16 N4 1.334(8) . ? C16 H16 0.93 . ? C17 N1 1.483(7) . ? C17 H17A 0.97 . ? C17 H17B 0.97 . ? C18 N1 1.483(7) . ? C18 C19 1.501(7) . ? C18 H18A 0.97 . ? C18 H18B 0.97 . ? C19 O4 1.408(7) . ? C19 H19A 0.97 . ? C19 H19B 0.97 . ? C20 O4 1.360(7) . ? C20 H20A 0.96 . ? C20 H20B 0.96 . ? C20 H20C 0.96 . ? C21 N1 1.453(7) . ? C21 C22 1.514(8) . ? C21 H21A 0.97 . ? C21 H21B 0.97 . ? C22 N2 1.360(7) . ? C22 C23 1.365(8) . ? C23 C24 1.358(9) . ? C23 H23 0.93 . ? C24 C25 1.398(9) . ? C24 H24 0.93 . ? C25 C26 1.358(8) . ? C25 H25 0.93 . ? C26 N2 1.341(7) . ? C26 H26 0.93 . ? C27 O3 1.242(7) . ? C27 O2 1.256(7) . ? C27 C28 1.482(9) . ? C28 H28A 0.96 . ? C28 H28B 0.96 . ? C28 H28C 0.96 . ? C29 O6 1.245(6) . ? C29 O7 1.254(6) . ? C29 C30 1.499(8) . ? C30 H30D 0.96 . ? C30 H30E 0.96 . ? C30 H30F 0.96 . ? N1 Zn2 2.206(4) . ? N2 Zn2 2.127(4) . ? N3 Zn1 2.196(4) . ? N4 Zn1 2.114(4) . ? O1 Zn1 2.007(3) . ? O1 Zn2 2.020(3) . ? O2 Zn1 2.000(4) . ? O3 Zn2 2.068(4) . ? O4 Zn2 2.368(4) . ? O5 Zn1 2.433(4) . ? O6 Zn1 2.067(3) . ? O7 Zn2 1.991(3) . ? P1 F3' 1.496(15) . ? P1 F2' 1.539(17) . ? P1 F5 1.551(5) . ? P1 F1 1.556(5) . ? P1 F4 1.559(7) . ? P1 F3 1.573(5) . ? P1 F6 1.587(4) . ? P1 F2 1.609(8) . ? P1 F4' 1.631(16) . ? P1 F5' 1.641(14) . ? F2 F2' 1.22(2) . ? F2 F3' 1.25(2) . ? F3 F3' 1.05(2) . ? F3 F4' 1.40(2) . ? F4 F4' 1.14(2) . ? F4 F5' 1.31(2) . ? F5 F5' 1.23(2) . ? F5 F2' 1.25(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 121.3(4) . . ? C6 C1 Br1 119.9(3) . . ? C2 C1 Br1 118.7(4) . . ? C1 C2 C3 119.0(5) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C4 C3 C2 120.4(4) . . ? C4 C3 C7 118.7(4) . . ? C2 C3 C7 120.9(4) . . ? O1 C4 C3 121.8(4) . . ? O1 C4 C5 118.7(4) . . ? C3 C4 C5 119.4(4) . . ? C6 C5 C4 119.1(5) . . ? C6 C5 C17 121.6(4) . . ? C4 C5 C17 119.3(4) . . ? C1 C6 C5 120.6(4) . . ? C1 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? N3 C7 C3 111.2(4) . . ? N3 C7 H7A 109.4 . . ? C3 C7 H7A 109.4 . . ? N3 C7 H7B 109.4 . . ? C3 C7 H7B 109.4 . . ? H7A C7 H7B 108 . . ? C9 C8 N3 115.2(4) . . ? C9 C8 H8A 108.5 . . ? N3 C8 H8A 108.5 . . ? C9 C8 H8B 108.5 . . ? N3 C8 H8B 108.5 . . ? H8A C8 H8B 107.5 . . ? O5 C9 C8 107.8(5) . . ? O5 C9 H9A 110.2 . . ? C8 C9 H9A 110.2 . . ? O5 C9 H9B 110.2 . . ? C8 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? O5 C10 H10A 109.5 . . ? O5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N3 C11 C12 109.3(4) . . ? N3 C11 H11A 109.8 . . ? C12 C11 H11A 109.8 . . ? N3 C11 H11B 109.8 . . ? C12 C11 H11B 109.8 . . ? H11A C11 H11B 108.3 . . ? N4 C12 C13 120.3(6) . . ? N4 C12 C11 116.6(4) . . ? C13 C12 C11 123.1(6) . . ? C14 C13 C12 120.0(7) . . ? C14 C13 H13 120 . . ? C12 C13 H13 120 . . ? C15 C14 C13 119.8(6) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 119.3(7) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? N4 C16 C15 120.2(7) . . ? N4 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? N1 C17 C5 112.7(4) . . ? N1 C17 H17A 109 . . ? C5 C17 H17A 109 . . ? N1 C17 H17B 109 . . ? C5 C17 H17B 109 . . ? H17A C17 H17B 107.8 . . ? N1 C18 C19 114.6(4) . . ? N1 C18 H18A 108.6 . . ? C19 C18 H18A 108.6 . . ? N1 C18 H18B 108.6 . . ? C19 C18 H18B 108.6 . . ? H18A C18 H18B 107.6 . . ? O4 C19 C18 107.9(4) . . ? O4 C19 H19A 110.1 . . ? C18 C19 H19A 110.1 . . ? O4 C19 H19B 110.1 . . ? C18 C19 H19B 110.1 . . ? H19A C19 H19B 108.4 . . ? O4 C20 H20A 109.5 . . ? O4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N1 C21 C22 112.0(4) . . ? N1 C21 H21A 109.2 . . ? C22 C21 H21A 109.2 . . ? N1 C21 H21B 109.2 . . ? C22 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? N2 C22 C23 120.5(6) . . ? N2 C22 C21 114.4(4) . . ? C23 C22 C21 125.0(5) . . ? C24 C23 C22 120.4(6) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 119.4(5) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? C26 C25 C24 118.0(6) . . ? C26 C25 H25 121 . . ? C24 C25 H25 121 . . ? N2 C26 C25 122.8(5) . . ? N2 C26 H26 118.6 . . ? C25 C26 H26 118.6 . . ? O3 C27 O2 125.1(5) . . ? O3 C27 C28 118.3(5) . . ? O2 C27 C28 116.6(6) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O6 C29 O7 125.8(5) . . ? O6 C29 C30 118.3(5) . . ? O7 C29 C30 115.9(5) . . ? C29 C30 H30D 109.5 . . ? C29 C30 H30E 109.5 . . ? H30D C30 H30E 109.5 . . ? C29 C30 H30F 109.5 . . ? H30D C30 H30F 109.5 . . ? H30E C30 H30F 109.5 . . ? C21 N1 C17 111.0(4) . . ? C21 N1 C18 109.3(4) . . ? C17 N1 C18 113.8(4) . . ? C21 N1 Zn2 101.7(3) . . ? C17 N1 Zn2 107.7(3) . . ? C18 N1 Zn2 112.8(3) . . ? C26 N2 C22 118.9(4) . . ? C26 N2 Zn2 128.0(3) . . ? C22 N2 Zn2 113.0(4) . . ? C7 N3 C11 109.3(4) . . ? C7 N3 C8 112.4(4) . . ? C11 N3 C8 109.7(4) . . ? C7 N3 Zn1 108.3(3) . . ? C11 N3 Zn1 102.1(3) . . ? C8 N3 Zn1 114.5(3) . . ? C16 N4 C12 120.4(5) . . ? C16 N4 Zn1 126.6(4) . . ? C12 N4 Zn1 113.0(3) . . ? C4 O1 Zn1 125.0(3) . . ? C4 O1 Zn2 124.8(3) . . ? Zn1 O1 Zn2 110.21(14) . . ? C27 O2 Zn1 132.6(4) . . ? C27 O3 Zn2 131.1(3) . . ? C20 O4 C19 116.5(5) . . ? C20 O4 Zn2 124.4(4) . . ? C19 O4 Zn2 111.5(3) . . ? C10 O5 C9 109.8(6) . . ? C10 O5 Zn1 122.7(6) . . ? C9 O5 Zn1 111.3(3) . . ? C29 O6 Zn1 130.4(3) . . ? C29 O7 Zn2 131.8(3) . . ? O2 Zn1 O1 97.86(14) . . ? O2 Zn1 O6 103.46(17) . . ? O1 Zn1 O6 92.35(14) . . ? O2 Zn1 N4 94.02(17) . . ? O1 Zn1 N4 167.80(16) . . ? O6 Zn1 N4 87.56(15) . . ? O2 Zn1 N3 157.93(17) . . ? O1 Zn1 N3 89.66(13) . . ? O6 Zn1 N3 96.89(16) . . ? N4 Zn1 N3 78.25(15) . . ? O2 Zn1 O5 85.58(16) . . ? O1 Zn1 O5 91.14(15) . . ? O6 Zn1 O5 169.75(15) . . ? N4 Zn1 O5 87.00(17) . . ? N3 Zn1 O5 73.49(14) . . ? O7 Zn2 O1 99.09(13) . . ? O7 Zn2 O3 102.17(17) . . ? O1 Zn2 O3 91.79(14) . . ? O7 Zn2 N2 93.76(16) . . ? O1 Zn2 N2 166.91(15) . . ? O3 Zn2 N2 87.91(15) . . ? O7 Zn2 N1 160.90(16) . . ? O1 Zn2 N1 89.33(13) . . ? O3 Zn2 N1 94.61(16) . . ? N2 Zn2 N1 77.66(16) . . ? O7 Zn2 O4 87.34(15) . . ? O1 Zn2 O4 95.33(14) . . ? O3 Zn2 O4 167.09(14) . . ? N2 Zn2 O4 82.72(15) . . ? N1 Zn2 O4 74.76(14) . . ? F3' P1 F2' 91.7(10) . . ? F3' P1 F5 139.5(11) . . ? F2' P1 F5 47.9(10) . . ? F3' P1 F1 85.5(10) . . ? F2' P1 F1 86.4(11) . . ? F5 P1 F1 92.2(3) . . ? F3' P1 F4 130.0(11) . . ? F2' P1 F4 138.3(11) . . ? F5 P1 F4 90.5(5) . . ? F1 P1 F4 95.4(4) . . ? F3' P1 F3 40.0(8) . . ? F2' P1 F3 131.5(10) . . ? F5 P1 F3 176.0(4) . . ? F1 P1 F3 91.7(3) . . ? F4 P1 F3 90.1(5) . . ? F3' P1 F6 94.0(9) . . ? F2' P1 F6 94.7(10) . . ? F5 P1 F6 88.9(3) . . ? F1 P1 F6 178.8(3) . . ? F4 P1 F6 84.1(3) . . ? F3 P1 F6 87.2(3) . . ? F3' P1 F2 47.4(9) . . ? F2' P1 F2 45.4(8) . . ? F5 P1 F2 92.5(5) . . ? F1 P1 F2 92.4(5) . . ? F4 P1 F2 171.5(5) . . ? F3 P1 F2 86.4(5) . . ? F6 P1 F2 88.0(4) . . ? F3' P1 F4' 89.7(10) . . ? F2' P1 F4' 167.0(14) . . ? F5 P1 F4' 129.8(8) . . ? F1 P1 F4' 80.8(9) . . ? F4 P1 F4' 41.8(7) . . ? F3 P1 F4' 51.9(8) . . ? F6 P1 F4' 98.1(9) . . ? F2 P1 F4' 137.1(9) . . ? F3' P1 F5' 167.2(12) . . ? F2' P1 F5' 91.3(10) . . ? F5 P1 F5' 45.2(7) . . ? F1 P1 F5' 82.2(8) . . ? F4 P1 F5' 48.2(8) . . ? F3 P1 F5' 136.5(9) . . ? F6 P1 F5' 98.2(8) . . ? F2 P1 F5' 136.6(9) . . ? F4' P1 F5' 84.6(8) . . ? F2' F2 F3' 123.8(12) . . ? F2' F2 P1 64.3(7) . . ? F3' F2 P1 61.6(7) . . ? F3' F3 F4' 127.7(14) . . ? F3' F3 P1 66.1(9) . . ? F4' F3 P1 66.2(8) . . ? F4' F4 F5' 128.0(13) . . ? F4' F4 P1 72.4(8) . . ? F5' F4 P1 69.2(8) . . ? F5' F5 F2' 132.6(14) . . ? F5' F5 P1 71.2(7) . . ? F2' F5 P1 65.6(9) . . ? F2 F2' F5 135.0(15) . . ? F2 F2' P1 70.3(9) . . ? F5 F2' P1 66.5(8) . . ? F3 F3' F2 141.7(17) . . ? F3 F3' P1 73.9(9) . . ? F2 F3' P1 71.0(10) . . ? F4 F4' F3 120.9(16) . . ? F4 F4' P1 65.7(8) . . ? F3 F4' P1 61.9(7) . . ? F5 F5' F4 120.9(13) . . ? F5 F5' P1 63.5(7) . . ? F4 F5' P1 62.7(7) . . ? #===END