# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1654 data_FK9907L _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C62 H92 N7 Cl8 Br' _chemical_formula_weight 1298.94 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Pn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 17.4715(15) _cell_length_b 9.8009(11) _cell_length_c 20.0372(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.004(6) _cell_angle_gamma 90.00 _cell_volume 3431.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 11.12 _cell_measurement_theta_max 27.49 _exptl_crystal_description 'platy needles' _exptl_crystal_colour Clear _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.53 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.257 _exptl_crystal_density_method ? _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 3.997 _exptl_absorpt_correction_type 'Lamina [1 0 -1]' _exptl_absorpt_correction_T_min 0.4257 _exptl_absorpt_correction_T_max 0.7189 _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5380 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0218 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.36 _diffrn_reflns_theta_max 63.81 _reflns_number_total 5380 _reflns_number_observed 5253 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 20 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0974P)^2^+3.5517P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0021(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(2) _refine_ls_number_reflns 5360 _refine_ls_number_parameters 704 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_obs 0.0540 _refine_ls_wR_factor_all 0.1447 _refine_ls_wR_factor_obs 0.1417 _refine_ls_goodness_of_fit_all 1.051 _refine_ls_goodness_of_fit_obs 1.058 _refine_ls_restrained_S_all 1.066 _refine_ls_restrained_S_obs 1.058 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Br Br 0.00913(3) 0.19721(8) 0.40483(3) 0.0399(2) Uani 1 d . . N1 N -0.0640(3) 0.3816(5) 0.2768(2) 0.0259(10) Uani 1 d . . H1 H -0.0432(3) 0.3341(5) 0.3107(2) 0.031 Uiso 1 calc R . N2 N 0.1208(3) 0.2603(5) 0.2729(2) 0.0269(10) Uani 1 d . . H2 H 0.0994(3) 0.2567(5) 0.3137(2) 0.032 Uiso 1 calc R . N3 N 0.1992(3) 0.1443(5) 0.4045(3) 0.0298(10) Uani 1 d . . H3 H 0.1482(3) 0.1558(5) 0.4073(3) 0.036 Uiso 1 calc R . N4 N 0.1047(3) 0.1431(5) 0.5505(2) 0.0302(11) Uani 1 d . . H4 H 0.0797(3) 0.1620(5) 0.5124(2) 0.036 Uiso 1 calc R . N5 N -0.0664(3) 0.2529(6) 0.5575(2) 0.0312(11) Uani 1 d . . H5 H -0.0424(3) 0.2449(6) 0.5179(2) 0.037 Uiso 1 calc R . N6 N -0.1550(3) 0.3799(5) 0.4177(2) 0.0297(10) Uani 1 d . . H6 H -0.1096(3) 0.3372(5) 0.4140(2) 0.036 Uiso 1 calc R . C1 C -0.1409(3) 0.3814(6) 0.2612(3) 0.0249(11) Uani 1 d . . C2 C -0.1494(4) 0.4659(7) 0.2071(3) 0.0347(14) Uani 1 d . . H2A H -0.1961(4) 0.4863(7) 0.1849(3) 0.042 Uiso 1 calc R . C3 C -0.0756(4) 0.5176(7) 0.1902(3) 0.0324(13) Uani 1 d . . H3A H -0.0646(4) 0.5787(7) 0.1547(3) 0.039 Uiso 1 calc R . C4 C -0.0230(3) 0.4637(6) 0.2340(3) 0.0274(11) Uani 1 d . . C5 C 0.0617(3) 0.4875(6) 0.2424(3) 0.0288(12) Uani 1 d . . C5A C 0.0781(4) 0.5384(7) 0.3144(4) 0.0379(15) Uani 1 d . . H5AA H 0.0468(4) 0.6191(7) 0.3238(4) 0.057 Uiso 1 calc R . H5AB H 0.1324(4) 0.5620(7) 0.3186(4) 0.057 Uiso 1 calc R . H5AC H 0.0654(4) 0.4661(7) 0.3464(4) 0.057 Uiso 1 calc R . C5B C 0.0858(4) 0.6016(7) 0.1938(4) 0.043(2) Uani 1 d . . H5BA H 0.0556(4) 0.6838(7) 0.2028(4) 0.065 Uiso 1 calc R . H5BB H 0.0769(4) 0.5716(7) 0.1478(4) 0.065 Uiso 1 calc R . H5BC H 0.1403(4) 0.6218(7) 0.1999(4) 0.065 Uiso 1 calc R . C6 C 0.1089(3) 0.3643(6) 0.2271(3) 0.0278(12) Uani 1 d . . C7 C 0.1517(4) 0.3287(8) 0.1712(3) 0.0359(15) Uani 1 d . . H7A H 0.1553(4) 0.3794(8) 0.1309(3) 0.043 Uiso 1 calc R . C8 C 0.1890(4) 0.2036(7) 0.1848(3) 0.0389(15) Uani 1 d . . H8A H 0.2218(4) 0.1559(7) 0.1551(3) 0.047 Uiso 1 calc R . C9 C 0.1700(3) 0.1629(6) 0.2474(3) 0.0289(12) Uani 1 d . . C10 C 0.1943(3) 0.0398(6) 0.2884(3) 0.0312(13) Uani 1 d . . C10A C 0.1261(4) -0.0526(7) 0.3066(4) 0.0404(15) Uani 1 d . . H10A H 0.0994(4) -0.0802(7) 0.2657(4) 0.061 Uiso 1 calc R . H10B H 0.0908(4) -0.0025(7) 0.3356(4) 0.061 Uiso 1 calc R . H10C H 0.1448(4) -0.1338(7) 0.3300(4) 0.061 Uiso 1 calc R . C10B C 0.2505(5) -0.0450(8) 0.2451(4) 0.049(2) Uani 1 d . . H10D H 0.2245(5) -0.0749(8) 0.2043(4) 0.074 Uiso 1 calc R . H10E H 0.2677(5) -0.1249(8) 0.2704(4) 0.074 Uiso 1 calc R . H10F H 0.2948(5) 0.0114(8) 0.2333(4) 0.074 Uiso 1 calc R . C11 C 0.2365(3) 0.0838(6) 0.3506(3) 0.0300(12) Uani 1 d . . C12 C 0.3122(4) 0.0854(8) 0.3663(3) 0.0394(15) Uani 1 d . . H12A H 0.3523(4) 0.0507(8) 0.3391(3) 0.047 Uiso 1 calc R . C13 C 0.3218(3) 0.1471(7) 0.4296(3) 0.0361(14) Uani 1 d . . H13A H 0.3690(3) 0.1607(7) 0.4522(3) 0.043 Uiso 1 calc R . C14 C 0.2503(4) 0.1840(6) 0.4526(3) 0.0327(13) Uani 1 d . . C15 C 0.2269(4) 0.2608(7) 0.5149(4) 0.0357(14) Uani 1 d . . C15A C 0.1823(5) 0.3878(7) 0.4933(4) 0.048(2) Uani 1 d . . H15A H 0.2134(5) 0.4415(7) 0.4622(4) 0.072 Uiso 1 calc R . H15B H 0.1702(5) 0.4432(7) 0.5326(4) 0.072 Uiso 1 calc R . H15C H 0.1347(5) 0.3601(7) 0.4712(4) 0.072 Uiso 1 calc R . C15B C 0.2989(5) 0.3092(10) 0.5506(5) 0.058(2) Uani 1 d . . H15D H 0.3301(5) 0.3635(10) 0.5198(5) 0.087 Uiso 1 calc R . H15E H 0.3284(5) 0.2300(10) 0.5658(5) 0.087 Uiso 1 calc R . H15F H 0.2846(5) 0.3653(10) 0.5891(5) 0.087 Uiso 1 calc R . C16 C 0.1797(4) 0.1778(7) 0.5624(3) 0.0337(13) Uani 1 d . . C17 C 0.1959(4) 0.1296(10) 0.6246(3) 0.048(2) Uani 1 d . . H17A H 0.2436(4) 0.1378(10) 0.6470(3) 0.057 Uiso 1 calc R . C18 C 0.1294(4) 0.0650(10) 0.6501(3) 0.049(2) Uani 1 d . . H18A H 0.1251(4) 0.0214(10) 0.6922(3) 0.058 Uiso 1 calc R . C19 C 0.0728(4) 0.0761(6) 0.6036(3) 0.0318(13) Uani 1 d . . C20 C -0.0109(4) 0.0335(6) 0.6045(3) 0.0338(13) Uani 1 d . . C20A C -0.0301(4) -0.0531(8) 0.5426(4) 0.044(2) Uani 1 d . . H20A H 0.0032(4) -0.1336(8) 0.5414(4) 0.066 Uiso 1 calc R . H20B H -0.0220(4) 0.0015(8) 0.5022(4) 0.066 Uiso 1 calc R . H20C H -0.0837(4) -0.0822(8) 0.5447(4) 0.066 Uiso 1 calc R . C20B C -0.0247(5) -0.0549(8) 0.6669(4) 0.051(2) Uani 1 d . . H20D H 0.0079(5) -0.1362(8) 0.6649(4) 0.077 Uiso 1 calc R . H20E H -0.0786(5) -0.0826(8) 0.6685(4) 0.077 Uiso 1 calc R . H20F H -0.0122(5) -0.0020(8) 0.7069(4) 0.077 Uiso 1 calc R . C21 C -0.0612(4) 0.1584(7) 0.6078(3) 0.0311(13) Uani 1 d . . C22 C -0.1069(4) 0.2075(7) 0.6593(3) 0.039(2) Uani 1 d . . H22A H -0.1152(4) 0.1644(7) 0.7012(3) 0.046 Uiso 1 calc R . C23 C -0.1391(4) 0.3333(8) 0.6382(4) 0.039(2) Uani 1 d . . H23A H -0.1731(4) 0.3888(8) 0.6634(4) 0.047 Uiso 1 calc R . C24 C -0.1125(3) 0.3613(7) 0.5745(3) 0.0296(13) Uani 1 d . . C25 C -0.1239(3) 0.4834(6) 0.5304(3) 0.0312(13) Uani 1 d . . C25A C -0.0467(4) 0.5353(7) 0.5037(3) 0.0360(14) Uani 1 d . . H25A H -0.0553(4) 0.6149(7) 0.4751(3) 0.054 Uiso 1 calc R . H25B H -0.0219(4) 0.4629(7) 0.4778(3) 0.054 Uiso 1 calc R . H25C H -0.0138(4) 0.5610(7) 0.5413(3) 0.054 Uiso 1 calc R . C25B C -0.1584(5) 0.5982(7) 0.5723(4) 0.046(2) Uani 1 d . . H25D H -0.1662(5) 0.6789(7) 0.5442(4) 0.069 Uiso 1 calc R . H25E H -0.1235(5) 0.6210(7) 0.6089(4) 0.069 Uiso 1 calc R . H25F H -0.2077(5) 0.5685(7) 0.5907(4) 0.069 Uiso 1 calc R . C26 C -0.1772(3) 0.4563(7) 0.4723(3) 0.0330(13) Uani 1 d . . C27 C -0.2501(4) 0.5007(8) 0.4584(4) 0.043(2) Uani 1 d . . H27A H -0.2811(4) 0.5549(8) 0.4869(4) 0.051 Uiso 1 calc R . C28 C -0.2710(4) 0.4520(8) 0.3945(4) 0.043(2) Uani 1 d . . H28A H -0.3184(4) 0.4683(8) 0.3725(4) 0.051 Uiso 1 calc R . C29 C -0.2111(3) 0.3775(6) 0.3699(3) 0.0284(12) Uani 1 d . . C30 C -0.2006(4) 0.3083(6) 0.3023(3) 0.0279(13) Uani 1 d . . C30A C -0.1790(4) 0.1582(7) 0.3128(4) 0.0385(14) Uani 1 d . . H30A H -0.2186(4) 0.1131(7) 0.3396(4) 0.058 Uiso 1 calc R . H30B H -0.1298(4) 0.1529(7) 0.3363(4) 0.058 Uiso 1 calc R . H30C H -0.1747(4) 0.1126(7) 0.2695(4) 0.058 Uiso 1 calc R . C30B C -0.2769(5) 0.3141(9) 0.2643(4) 0.046(2) Uani 1 d . . H30D H -0.3165(5) 0.2671(9) 0.2901(4) 0.069 Uiso 1 calc R . H30E H -0.2710(5) 0.2694(9) 0.2208(4) 0.069 Uiso 1 calc R . H30F H -0.2918(5) 0.4095(9) 0.2576(4) 0.069 Uiso 1 calc R . N40 N 0.4374(3) 0.7729(6) 0.5169(3) 0.0356(12) Uani 1 d . . C41 C 0.4438(4) 0.8357(7) 0.4479(3) 0.0395(15) Uani 1 d . . H41A H 0.4096(4) 0.9161(7) 0.4458(3) 0.047 Uiso 1 calc R . H41B H 0.4249(4) 0.7685(7) 0.4148(3) 0.047 Uiso 1 calc R . C42 C 0.5238(4) 0.8801(8) 0.4275(4) 0.043(2) Uani 1 d . . H42A H 0.5573(4) 0.7991(8) 0.4235(4) 0.052 Uiso 1 calc R . H42B H 0.5455(4) 0.9408(8) 0.4621(4) 0.052 Uiso 1 calc R . C43 C 0.5206(4) 0.9550(8) 0.3611(3) 0.041(2) Uani 1 d . . H43A H 0.4990(4) 0.8938(8) 0.3266(3) 0.049 Uiso 1 calc R . H43B H 0.4864(4) 1.0351(8) 0.3652(3) 0.049 Uiso 1 calc R . C44 C 0.5993(5) 1.0020(10) 0.3396(4) 0.055(2) Uani 1 d . . H44A H 0.5955(5) 1.0498(10) 0.2967(4) 0.083 Uiso 1 calc R . H44B H 0.6330(5) 0.9227(10) 0.3347(4) 0.083 Uiso 1 calc R . H44C H 0.6204(5) 1.0639(10) 0.3733(4) 0.083 Uiso 1 calc R . C45 C 0.4887(5) 0.6501(7) 0.5238(4) 0.043(2) Uani 1 d . . H45A H 0.4778(5) 0.6059(7) 0.5672(4) 0.052 Uiso 1 calc R . H45B H 0.5425(5) 0.6820(7) 0.5251(4) 0.052 Uiso 1 calc R . C46 C 0.4815(5) 0.5433(8) 0.4692(4) 0.049(2) Uani 1 d . . H46A H 0.4272(5) 0.5162(8) 0.4644(4) 0.059 Uiso 1 calc R . H46B H 0.4987(5) 0.5824(8) 0.4262(4) 0.059 Uiso 1 calc R . C47 C 0.5294(6) 0.4190(9) 0.4859(5) 0.059(2) Uani 1 d . . H47A H 0.5827(6) 0.4481(9) 0.4944(5) 0.070 Uiso 1 calc R . H47B H 0.5095(6) 0.3769(9) 0.5273(5) 0.070 Uiso 1 calc R . C48 C 0.5290(6) 0.3143(10) 0.4311(6) 0.067(3) Uani 1 d . . H48A H 0.5607(6) 0.2363(10) 0.4443(6) 0.101 Uiso 1 calc R . H48B H 0.5497(6) 0.3548(10) 0.3902(6) 0.101 Uiso 1 calc R . H48C H 0.4765(6) 0.2835(10) 0.4231(6) 0.101 Uiso 1 calc R . C49 C 0.4610(4) 0.8806(7) 0.5684(3) 0.0400(15) Uani 1 d . . H49A H 0.5158(4) 0.9022(7) 0.5618(3) 0.048 Uiso 1 calc R . H49B H 0.4315(4) 0.9650(7) 0.5598(3) 0.048 Uiso 1 calc R . C50 C 0.4490(6) 0.8390(8) 0.6409(4) 0.050(2) Uani 1 d . . H50A H 0.3938(6) 0.8241(8) 0.6493(4) 0.059 Uiso 1 calc R . H50B H 0.4764(6) 0.7525(8) 0.6499(4) 0.059 Uiso 1 calc R . C51 C 0.4788(4) 0.9495(8) 0.6867(4) 0.044(2) Uani 1 d . . H51A H 0.4736(4) 0.9181(8) 0.7334(4) 0.053 Uiso 1 calc R . H51B H 0.5340(4) 0.9630(8) 0.6777(4) 0.053 Uiso 1 calc R . C52 C 0.4389(6) 1.0839(8) 0.6797(4) 0.057(2) Uani 1 d . . H52A H 0.4613(6) 1.1497(8) 0.7109(4) 0.085 Uiso 1 calc R . H52B H 0.3844(6) 1.0725(8) 0.6897(4) 0.085 Uiso 1 calc R . H52C H 0.4449(6) 1.1174(8) 0.6339(4) 0.085 Uiso 1 calc R . C53 C 0.3541(4) 0.7277(8) 0.5279(4) 0.045(2) Uani 1 d . . H53A H 0.3387(4) 0.6693(8) 0.4899(4) 0.054 Uiso 1 calc R . H53B H 0.3522(4) 0.6706(8) 0.5687(4) 0.054 Uiso 1 calc R . C54 C 0.2956(5) 0.8404(10) 0.5351(6) 0.070(3) Uani 1 d . . H54A H 0.2992(5) 0.9024(10) 0.4962(6) 0.084 Uiso 1 calc R . H54B H 0.3070(5) 0.8942(10) 0.5757(6) 0.084 Uiso 1 calc R . C55 C 0.2142(5) 0.7837(11) 0.5398(5) 0.061(2) Uani 1 d . . H55A H 0.2155(5) 0.6939(11) 0.5624(5) 0.074 Uiso 1 calc R . H55B H 0.1825(5) 0.8459(11) 0.5672(5) 0.074 Uiso 1 calc R . C56 C 0.1787(8) 0.7680(14) 0.4735(7) 0.085(3) Uani 1 d . . H56A H 0.1268(8) 0.7315(14) 0.4786(7) 0.128 Uiso 1 calc R . H56B H 0.2094(8) 0.7049(14) 0.4466(7) 0.128 Uiso 1 calc R . H56C H 0.1764(8) 0.8570(14) 0.4513(7) 0.128 Uiso 1 calc R . C60 C 0.3070(5) 0.4129(9) 0.3007(5) 0.056(2) Uani 1 d . . H60A H 0.2668(5) 0.4059(9) 0.2661(5) 0.067 Uiso 1 calc R . H60B H 0.2933(5) 0.3500(9) 0.3375(5) 0.067 Uiso 1 calc R . Cl1 Cl 0.39483(15) 0.3623(3) 0.26653(13) 0.0752(7) Uani 1 d . . Cl2 Cl 0.3092(2) 0.5791(3) 0.33121(14) 0.0731(6) Uani 1 d . . C65 C -0.2614(6) 0.1329(13) 0.5261(6) 0.074(3) Uani 1 d . . H65A H -0.2581(6) 0.2028(13) 0.4906(6) 0.089 Uiso 1 calc R . H65B H -0.2189(6) 0.1484(13) 0.5579(6) 0.089 Uiso 1 calc R . Cl3 Cl -0.3495(2) 0.1485(4) 0.5681(2) 0.0923(9) Uani 1 d . . Cl4 Cl -0.2530(2) -0.0286(4) 0.4911(2) 0.1027(11) Uani 1 d . . C70 C 0.5576(6) 0.5956(11) 0.1851(5) 0.070(3) Uani 1 d . . H70A H 0.5041(6) 0.6169(11) 0.1725(5) 0.084 Uiso 1 calc R . H70B H 0.5914(6) 0.6590(11) 0.1605(5) 0.084 Uiso 1 calc R . Cl5 Cl 0.5781(2) 0.4314(3) 0.16126(14) 0.0789(8) Uani 1 d . . Cl6 Cl 0.5689(2) 0.6235(3) 0.27059(15) 0.0848(8) Uani 1 d . . C75 C -0.1430(4) -0.2934(7) 0.3383(4) 0.043(2) Uani 1 d . . H75A H -0.1602(4) -0.3497(7) 0.3765(4) 0.052 Uiso 1 calc R . H75B H -0.1148(4) -0.3535(7) 0.3071(4) 0.052 Uiso 1 calc R . Cl7 Cl -0.08112(14) -0.1654(2) 0.36746(11) 0.0600(5) Uani 1 d . . Cl8 Cl -0.22371(14) -0.2259(3) 0.29736(15) 0.0697(6) Uani 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 Br 0.0257(3) 0.0688(5) 0.0253(3) 0.0079(3) 0.0062(2) 0.0127(3) N1 0.024(2) 0.033(2) 0.021(2) 0.006(2) 0.002(2) 0.000(2) N2 0.027(2) 0.036(3) 0.018(2) 0.001(2) 0.012(2) 0.005(2) N3 0.016(2) 0.039(3) 0.034(3) 0.000(2) 0.005(2) 0.001(2) N4 0.033(3) 0.037(3) 0.021(2) 0.004(2) -0.003(2) -0.003(2) N5 0.033(3) 0.043(3) 0.017(2) 0.000(2) 0.011(2) 0.006(2) N6 0.016(2) 0.041(3) 0.032(3) -0.006(2) 0.004(2) 0.006(2) C1 0.022(3) 0.030(3) 0.022(3) -0.001(2) -0.001(2) 0.002(2) C2 0.027(3) 0.048(4) 0.029(3) 0.001(3) -0.007(2) 0.002(3) C3 0.031(3) 0.035(3) 0.031(3) 0.002(3) 0.003(2) 0.003(3) C4 0.031(3) 0.029(3) 0.022(3) 0.002(2) 0.001(2) -0.001(2) C5 0.029(3) 0.029(3) 0.029(3) 0.000(2) 0.004(2) 0.000(2) C5A 0.034(3) 0.038(3) 0.042(4) -0.013(3) -0.003(3) 0.003(3) C5B 0.041(4) 0.035(3) 0.054(4) 0.011(3) 0.005(3) -0.004(3) C6 0.026(3) 0.034(3) 0.024(3) -0.002(2) 0.007(2) 0.001(2) C7 0.034(4) 0.048(4) 0.025(3) 0.003(3) 0.011(3) 0.004(3) C8 0.035(3) 0.047(4) 0.035(3) -0.006(3) 0.011(3) 0.013(3) C9 0.024(3) 0.031(3) 0.032(3) -0.001(2) 0.012(2) 0.002(2) C10 0.030(3) 0.032(3) 0.032(3) -0.005(2) 0.014(2) 0.010(3) C10A 0.042(4) 0.039(3) 0.039(4) 0.003(3) -0.004(3) -0.005(3) C10B 0.048(4) 0.054(4) 0.045(4) -0.013(3) 0.016(3) 0.025(4) C11 0.027(3) 0.033(3) 0.029(3) 0.003(2) 0.006(2) 0.008(2) C12 0.027(3) 0.050(4) 0.041(4) 0.010(3) 0.012(3) 0.008(3) C13 0.016(3) 0.049(4) 0.044(4) 0.012(3) 0.001(2) 0.003(3) C14 0.020(3) 0.035(3) 0.043(4) 0.003(3) 0.001(2) -0.002(2) C15 0.030(3) 0.037(3) 0.039(4) -0.005(3) -0.001(3) -0.002(3) C15A 0.063(5) 0.033(3) 0.049(4) -0.001(3) 0.010(3) 0.000(3) C15B 0.040(5) 0.077(6) 0.058(5) -0.014(4) -0.006(4) -0.022(4) C16 0.029(3) 0.045(3) 0.027(3) -0.005(3) -0.004(2) 0.002(3) C17 0.030(3) 0.087(6) 0.026(3) 0.005(3) -0.006(3) 0.005(4) C18 0.037(4) 0.080(6) 0.028(3) 0.008(3) 0.001(3) 0.005(4) C19 0.032(3) 0.035(3) 0.028(3) 0.002(3) 0.004(2) 0.000(3) C20 0.043(4) 0.031(3) 0.028(3) 0.003(2) 0.007(2) -0.001(3) C20A 0.045(4) 0.041(4) 0.047(4) -0.007(3) 0.004(3) -0.008(3) C20B 0.061(5) 0.049(4) 0.043(4) 0.022(3) 0.018(3) 0.002(4) C21 0.031(3) 0.037(3) 0.026(3) -0.003(2) 0.010(2) -0.005(3) C22 0.040(4) 0.051(4) 0.025(3) 0.005(3) 0.017(3) -0.005(3) C23 0.036(4) 0.053(4) 0.029(4) -0.002(3) 0.019(3) -0.002(3) C24 0.024(3) 0.037(3) 0.029(3) -0.003(3) 0.011(2) -0.001(2) C25 0.029(3) 0.030(3) 0.034(3) -0.002(3) 0.004(2) 0.001(2) C25A 0.028(3) 0.045(4) 0.035(3) 0.007(3) 0.000(2) -0.004(3) C25B 0.055(4) 0.040(4) 0.042(4) -0.011(3) 0.007(3) 0.014(3) C26 0.022(3) 0.047(4) 0.030(3) 0.001(3) 0.006(2) 0.003(2) C27 0.030(3) 0.059(4) 0.039(4) 0.000(3) 0.006(3) 0.012(3) C28 0.016(3) 0.061(4) 0.052(4) 0.002(3) -0.002(3) 0.006(3) C29 0.016(3) 0.035(3) 0.034(3) -0.002(2) 0.003(2) 0.000(2) C30 0.022(3) 0.034(3) 0.028(3) 0.001(2) 0.001(2) -0.004(2) C30A 0.042(4) 0.030(3) 0.044(4) 0.002(3) 0.003(3) -0.009(3) C30B 0.033(4) 0.061(5) 0.045(4) 0.000(3) -0.005(3) -0.012(3) N40 0.038(3) 0.033(3) 0.036(3) -0.001(2) -0.002(2) 0.001(2) C41 0.041(4) 0.044(4) 0.034(3) 0.006(3) 0.001(3) -0.005(3) C42 0.041(4) 0.052(4) 0.036(4) 0.007(3) 0.002(3) 0.002(3) C43 0.035(3) 0.060(4) 0.027(3) 0.002(3) 0.002(2) -0.007(3) C44 0.044(4) 0.081(6) 0.041(4) -0.008(4) 0.017(3) -0.012(4) C45 0.049(4) 0.036(3) 0.044(4) 0.001(3) 0.000(3) 0.013(3) C46 0.061(5) 0.042(4) 0.043(4) -0.003(3) 0.005(3) 0.000(3) C47 0.059(5) 0.047(4) 0.070(6) -0.015(4) 0.004(4) 0.015(4) C48 0.052(5) 0.061(5) 0.089(7) -0.024(5) 0.006(4) 0.000(4) C49 0.047(4) 0.039(3) 0.034(3) 0.000(3) 0.003(3) -0.004(3) C50 0.072(5) 0.043(4) 0.034(4) 0.004(3) 0.005(3) 0.003(4) C51 0.043(4) 0.052(4) 0.037(4) -0.003(3) 0.000(3) 0.001(3) C52 0.071(6) 0.044(4) 0.055(5) -0.006(4) 0.000(4) -0.001(4) C53 0.045(4) 0.045(4) 0.045(4) 0.000(3) 0.010(3) -0.012(3) C54 0.039(4) 0.058(5) 0.113(8) 0.028(5) 0.018(5) -0.007(4) C55 0.036(4) 0.074(6) 0.074(6) 0.008(5) 0.010(4) -0.009(4) C56 0.083(8) 0.081(7) 0.092(8) 0.008(6) -0.009(6) 0.008(6) C60 0.046(4) 0.059(5) 0.064(5) -0.001(4) 0.001(4) -0.007(4) Cl1 0.0596(13) 0.095(2) 0.0707(14) 0.0156(13) 0.0186(10) 0.0064(12) Cl2 0.073(2) 0.0667(13) 0.080(2) -0.0092(11) -0.0015(12) -0.0103(12) C65 0.056(5) 0.092(7) 0.076(6) -0.004(6) -0.003(5) -0.012(5) Cl3 0.088(2) 0.117(2) 0.072(2) 0.002(2) 0.0112(14) 0.034(2) Cl4 0.087(2) 0.121(3) 0.100(2) -0.032(2) -0.012(2) 0.025(2) C70 0.065(6) 0.072(6) 0.072(6) 0.011(5) -0.002(5) 0.015(5) Cl5 0.083(2) 0.078(2) 0.076(2) -0.0070(13) -0.0347(13) 0.0227(13) Cl6 0.096(2) 0.085(2) 0.073(2) -0.0153(14) -0.0127(14) 0.013(2) C75 0.045(4) 0.033(3) 0.052(4) -0.001(3) 0.001(3) 0.003(3) Cl7 0.0682(13) 0.0501(10) 0.0617(12) -0.0052(9) -0.0100(10) -0.0057(9) Cl8 0.0472(11) 0.0651(12) 0.097(2) 0.0116(12) -0.0090(11) 0.0096(10) _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 Br N2 3.344(5) . ? Br N3 3.361(5) . ? Br N5 3.376(5) . ? Br N1 3.389(5) . ? Br N6 3.391(5) . ? Br N4 3.404(5) . ? N1 C4 1.376(7) . ? N1 C1 1.379(7) . ? N2 C9 1.383(7) . ? N2 C6 1.388(8) . ? N3 C14 1.371(8) . ? N3 C11 1.393(8) . ? N4 C19 1.368(8) . ? N4 C16 1.375(8) . ? N5 C21 1.372(8) . ? N5 C24 1.376(8) . ? N6 C29 1.370(8) . ? N6 C26 1.381(8) . ? C1 C2 1.372(9) . ? C1 C30 1.509(8) . ? C2 C3 1.427(9) . ? C3 C4 1.376(9) . ? C4 C5 1.508(8) . ? C5 C6 1.494(8) . ? C5 C5B 1.541(9) . ? C5 C5A 1.555(9) . ? C6 C7 1.391(9) . ? C7 C8 1.415(10) . ? C8 C9 1.357(9) . ? C9 C10 1.519(9) . ? C10 C11 1.513(9) . ? C10 C10A 1.540(9) . ? C10 C10B 1.551(7) . ? C11 C12 1.360(9) . ? C12 C13 1.415(10) . ? C13 C14 1.380(9) . ? C14 C15 1.513(10) . ? C15 C16 1.500(10) . ? C15 C15B 1.523(10) . ? C15 C15A 1.531(10) . ? C16 C17 1.361(10) . ? C17 C18 1.419(11) . ? C18 C19 1.364(10) . ? C19 C20 1.520(9) . ? C20 C21 1.508(9) . ? C20 C20B 1.539(9) . ? C20 C20A 1.540(9) . ? C21 C22 1.391(9) . ? C22 C23 1.420(11) . ? C23 C24 1.386(9) . ? C24 C25 1.500(9) . ? C25 C26 1.516(9) . ? C25 C25B 1.528(9) . ? C25 C25A 1.536(8) . ? C26 C27 1.374(9) . ? C27 C28 1.414(11) . ? C28 C29 1.369(9) . ? C29 C30 1.527(9) . ? C30 C30A 1.534(9) . ? C30 C30B 1.536(10) . ? N40 C45 1.508(9) . ? N40 C41 1.518(9) . ? N40 C49 1.533(9) . ? N40 C53 1.537(9) . ? C41 C42 1.520(10) . ? C42 C43 1.520(10) . ? C43 C44 1.513(10) . ? C45 C46 1.519(10) . ? C46 C47 1.516(11) . ? C47 C48 1.503(12) . ? C49 C50 1.523(10) . ? C50 C51 1.512(11) . ? C51 C52 1.496(11) . ? C53 C54 1.512(12) . ? C54 C55 1.530(11) . ? C55 C56 1.47(2) . ? C60 Cl2 1.740(9) . ? C60 Cl1 1.752(9) . ? C65 Cl4 1.737(12) . ? C65 Cl3 1.759(11) . ? C70 Cl5 1.717(11) . ? C70 Cl6 1.745(11) . ? C75 Cl7 1.756(8) . ? C75 Cl8 1.760(8) . ? 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 N2 Br N3 56.65(12) . . ? N2 Br N5 156.16(13) . . ? N3 Br N5 114.39(13) . . ? N2 Br N1 61.49(12) . . ? N3 Br N1 116.95(12) . . ? N5 Br N1 116.91(12) . . ? N2 Br N6 117.15(12) . . ? N3 Br N6 156.54(13) . . ? N5 Br N6 60.99(12) . . ? N1 Br N6 57.13(12) . . ? N2 Br N4 114.87(13) . . ? N3 Br N4 59.54(13) . . ? N5 Br N4 55.94(13) . . ? N1 Br N4 156.53(13) . . ? N6 Br N4 115.59(13) . . ? C4 N1 C1 111.5(5) . . ? C4 N1 Br 126.0(4) . . ? C1 N1 Br 122.5(3) . . ? C9 N2 C6 110.9(5) . . ? C9 N2 Br 121.8(4) . . ? C6 N2 Br 124.9(3) . . ? C14 N3 C11 111.1(5) . . ? C14 N3 Br 126.7(4) . . ? C11 N3 Br 122.0(4) . . ? C19 N4 C16 111.9(5) . . ? C19 N4 Br 122.7(4) . . ? C16 N4 Br 125.3(4) . . ? C21 N5 C24 112.2(5) . . ? C21 N5 Br 122.1(4) . . ? C24 N5 Br 125.3(4) . . ? C29 N6 C26 111.2(5) . . ? C29 N6 Br 122.9(4) . . ? C26 N6 Br 125.8(4) . . ? C2 C1 N1 106.4(5) . . ? C2 C1 C30 130.0(5) . . ? N1 C1 C30 123.4(5) . . ? C1 C2 C3 107.7(5) . . ? C4 C3 C2 108.4(6) . . ? C3 C4 N1 106.0(5) . . ? C3 C4 C5 131.8(6) . . ? N1 C4 C5 122.1(5) . . ? C6 C5 C4 113.2(5) . . ? C6 C5 C5B 107.8(5) . . ? C4 C5 C5B 108.1(5) . . ? C6 C5 C5A 110.4(5) . . ? C4 C5 C5A 109.5(5) . . ? C5B C5 C5A 107.7(5) . . ? N2 C6 C7 105.5(5) . . ? N2 C6 C5 122.7(5) . . ? C7 C6 C5 131.7(6) . . ? C6 C7 C8 108.1(6) . . ? C9 C8 C7 108.7(6) . . ? C8 C9 N2 106.9(5) . . ? C8 C9 C10 131.6(5) . . ? N2 C9 C10 121.5(5) . . ? C11 C10 C9 110.8(5) . . ? C11 C10 C10A 110.5(5) . . ? C9 C10 C10A 112.3(5) . . ? C11 C10 C10B 107.8(5) . . ? C9 C10 C10B 107.5(5) . . ? C10A C10 C10B 107.9(6) . . ? C12 C11 N3 105.8(6) . . ? C12 C11 C10 131.9(6) . . ? N3 C11 C10 122.1(5) . . ? C11 C12 C13 109.0(5) . . ? C14 C13 C12 107.8(6) . . ? N3 C14 C13 106.2(6) . . ? N3 C14 C15 123.0(6) . . ? C13 C14 C15 130.6(6) . . ? C16 C15 C14 113.8(6) . . ? C16 C15 C15B 108.9(6) . . ? C14 C15 C15B 108.6(6) . . ? C16 C15 C15A 109.9(6) . . ? C14 C15 C15A 108.0(6) . . ? C15B C15 C15A 107.4(7) . . ? C17 C16 N4 105.8(6) . . ? C17 C16 C15 130.9(6) . . ? N4 C16 C15 123.2(6) . . ? C16 C17 C18 108.3(6) . . ? C19 C18 C17 108.2(6) . . ? C18 C19 N4 105.8(6) . . ? C18 C19 C20 131.9(6) . . ? N4 C19 C20 122.3(5) . . ? C21 C20 C19 109.7(5) . . ? C21 C20 C20B 109.2(5) . . ? C19 C20 C20B 108.4(6) . . ? C21 C20 C20A 110.8(6) . . ? C19 C20 C20A 110.6(5) . . ? C20B C20 C20A 108.1(6) . . ? N5 C21 C22 105.8(6) . . ? N5 C21 C20 123.7(5) . . ? C22 C21 C20 130.4(6) . . ? C21 C22 C23 107.9(6) . . ? C24 C23 C22 108.2(6) . . ? N5 C24 C23 105.8(6) . . ? N5 C24 C25 123.2(5) . . ? C23 C24 C25 130.9(6) . . ? C24 C25 C26 113.2(5) . . ? C24 C25 C25B 108.5(5) . . ? C26 C25 C25B 108.0(5) . . ? C24 C25 C25A 110.6(5) . . ? C26 C25 C25A 109.3(5) . . ? C25B C25 C25A 107.1(6) . . ? C27 C26 N6 105.8(6) . . ? C27 C26 C25 132.1(6) . . ? N6 C26 C25 122.1(5) . . ? C26 C27 C28 108.4(6) . . ? C29 C28 C27 107.9(6) . . ? C28 C29 N6 106.7(5) . . ? C28 C29 C30 130.4(6) . . ? N6 C29 C30 122.8(5) . . ? C1 C30 C29 110.9(5) . . ? C1 C30 C30A 111.1(5) . . ? C29 C30 C30A 109.4(5) . . ? C1 C30 C30B 108.2(5) . . ? C29 C30 C30B 108.6(6) . . ? C30A C30 C30B 108.5(6) . . ? C45 N40 C41 111.3(6) . . ? C45 N40 C49 109.1(5) . . ? C41 N40 C49 108.3(5) . . ? C45 N40 C53 108.7(5) . . ? C41 N40 C53 108.5(5) . . ? C49 N40 C53 110.9(5) . . ? N40 C41 C42 115.4(6) . . ? C41 C42 C43 109.9(6) . . ? C44 C43 C42 111.4(6) . . ? N40 C45 C46 115.7(6) . . ? C47 C46 C45 110.4(7) . . ? C48 C47 C46 112.7(8) . . ? C50 C49 N40 114.9(6) . . ? C51 C50 C49 109.9(6) . . ? C52 C51 C50 114.4(7) . . ? C54 C53 N40 116.3(6) . . ? C53 C54 C55 111.6(8) . . ? C56 C55 C54 111.9(10) . . ? Cl2 C60 Cl1 112.5(5) . . ? Cl4 C65 Cl3 110.3(6) . . ? Cl5 C70 Cl6 113.4(6) . . ? Cl7 C75 Cl8 112.3(4) . . ? _refine_diff_density_max 0.780 _refine_diff_density_min -1.125 _refine_diff_density_rms 0.077 data_FK9905 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C62 H98 N7 Cl9' _chemical_formula_weight 1260.52 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Pn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 17.5921(9) _cell_length_b 9.9697(7) _cell_length_c 20.0503(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.550(4) _cell_angle_gamma 90.00 _cell_volume 3516.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 10.99 _cell_measurement_theta_max 24.99 _exptl_crystal_description blocks _exptl_crystal_colour Clear _exptl_crystal_size_max 0.73 _exptl_crystal_size_mid 0.47 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.191 _exptl_crystal_density_method ? _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 3.584 _exptl_absorpt_correction_type Ellipsoidal _exptl_absorpt_correction_T_min 0.1099 _exptl_absorpt_correction_T_max 0.2342 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4370 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0260 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.33 _diffrn_reflns_theta_max 61.96 _reflns_number_total 4370 _reflns_number_observed 3700 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 147 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1089P)^2^+0.4727P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0011(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 4223 _refine_ls_number_parameters 704 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_obs 0.0534 _refine_ls_wR_factor_all 0.1635 _refine_ls_wR_factor_obs 0.1474 _refine_ls_goodness_of_fit_all 1.050 _refine_ls_goodness_of_fit_obs 1.077 _refine_ls_restrained_S_all 1.083 _refine_ls_restrained_S_obs 1.077 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cl Cl 0.01296(8) 0.2220(2) 0.40738(7) 0.0730(6) Uani 1 d . . N1 N -0.0603(3) 0.3698(6) 0.2751(2) 0.0558(15) Uani 1 d . . H1 H -0.0386(3) 0.3235(6) 0.3088(2) 0.067 Uiso 1 calc R . N2 N 0.1182(3) 0.2542(7) 0.2751(2) 0.058(2) Uani 1 d . . H2 H 0.0960(3) 0.2537(7) 0.3153(2) 0.070 Uiso 1 calc R . N3 N 0.1948(3) 0.1388(7) 0.4092(3) 0.062(2) Uani 1 d . . H3 H 0.1442(3) 0.1488(7) 0.4128(3) 0.075 Uiso 1 calc R . N4 N 0.0985(3) 0.1420(7) 0.5488(2) 0.062(2) Uani 1 d . . H4 H 0.0748(3) 0.1686(7) 0.5111(2) 0.074 Uiso 1 calc R . N5 N -0.0714(3) 0.2505(7) 0.5526(2) 0.063(2) Uani 1 d . . H5 H -0.0476(3) 0.2455(7) 0.5132(2) 0.076 Uiso 1 calc R . N6 N -0.1530(3) 0.3724(7) 0.4146(2) 0.059(2) Uani 1 d . . H6 H -0.1063(3) 0.3359(7) 0.4122(2) 0.071 Uiso 1 calc R . C1 C -0.1371(3) 0.3663(8) 0.2585(3) 0.062(2) Uani 1 d . . C2 C -0.1461(4) 0.4478(9) 0.2052(3) 0.066(2) Uani 1 d . . H2A H -0.1915(4) 0.4651(9) 0.1828(3) 0.079 Uiso 1 calc R . C3 C -0.0751(4) 0.5015(9) 0.1895(3) 0.067(2) Uani 1 d . . H3A H -0.0654(4) 0.5608(9) 0.1548(3) 0.081 Uiso 1 calc R . C4 C -0.0229(4) 0.4528(8) 0.2332(3) 0.058(2) Uani 1 d . . C5 C 0.0624(4) 0.4784(8) 0.2408(3) 0.060(2) Uani 1 d . . C5A C 0.0779(4) 0.5315(10) 0.3124(4) 0.075(2) Uani 1 d . . H5AA H 0.0482(4) 0.6108(10) 0.3198(4) 0.113 Uiso 1 calc R . H5AB H 0.1309(4) 0.5525(10) 0.3174(4) 0.113 Uiso 1 calc R . H5AC H 0.0641(4) 0.4640(10) 0.3442(4) 0.113 Uiso 1 calc R . C5B C 0.0859(5) 0.5870(11) 0.1915(5) 0.095(3) Uani 1 d . . H5BA H 0.0563(5) 0.6664(11) 0.1990(5) 0.142 Uiso 1 calc R . H5BB H 0.0773(5) 0.5557(11) 0.1468(5) 0.142 Uiso 1 calc R . H5BC H 0.1388(5) 0.6072(11) 0.1978(5) 0.142 Uiso 1 calc R . C6 C 0.1090(3) 0.3536(8) 0.2289(3) 0.058(2) Uani 1 d . . C7 C 0.1524(4) 0.3185(10) 0.1750(3) 0.071(2) Uani 1 d . . H7A H 0.1583(4) 0.3682(10) 0.1362(3) 0.085 Uiso 1 calc R . C8 C 0.1861(4) 0.1934(11) 0.1891(3) 0.076(3) Uani 1 d . . H8A H 0.2171(4) 0.1451(11) 0.1605(3) 0.092 Uiso 1 calc R . C9 C 0.1656(4) 0.1547(9) 0.2523(3) 0.064(2) Uani 1 d . . C10 C 0.1869(4) 0.0345(9) 0.2948(3) 0.069(2) Uani 1 d . . C10A C 0.1164(5) -0.0461(9) 0.3138(4) 0.078(2) Uani 1 d . . H10A H 0.0901(5) -0.0745(9) 0.2741(4) 0.116 Uiso 1 calc R . H10B H 0.0834(5) 0.0089(9) 0.3400(4) 0.116 Uiso 1 calc R . H10C H 0.1316(5) -0.1234(9) 0.3392(4) 0.116 Uiso 1 calc R . C10B C 0.2397(6) -0.0582(12) 0.2538(5) 0.103(3) Uani 1 d . . H10D H 0.2133(6) -0.0882(12) 0.2144(5) 0.154 Uiso 1 calc R . H10E H 0.2541(6) -0.1344(12) 0.2804(5) 0.154 Uiso 1 calc R . H10F H 0.2844(6) -0.0095(12) 0.2413(5) 0.154 Uiso 1 calc R . C11 C 0.2291(3) 0.0801(9) 0.3560(3) 0.066(2) Uani 1 d . . C12 C 0.3059(4) 0.0846(11) 0.3709(4) 0.083(3) Uani 1 d . . H12A H 0.3447(4) 0.0531(11) 0.3438(4) 0.099 Uiso 1 calc R . C13 C 0.3156(4) 0.1444(9) 0.4331(4) 0.073(2) Uani 1 d . . H13A H 0.3618(4) 0.1575(9) 0.4551(4) 0.087 Uiso 1 calc R . C14 C 0.2461(3) 0.1805(8) 0.4563(3) 0.061(2) Uani 1 d . . C15 C 0.2224(4) 0.2520(9) 0.5195(4) 0.069(2) Uani 1 d . . C15A C 0.1799(6) 0.3829(10) 0.4982(5) 0.090(3) Uani 1 d . . H15A H 0.2117(6) 0.4347(10) 0.4693(5) 0.135 Uiso 1 calc R . H15B H 0.1680(6) 0.4347(10) 0.5371(5) 0.135 Uiso 1 calc R . H15C H 0.1337(6) 0.3599(10) 0.4750(5) 0.135 Uiso 1 calc R . C15B C 0.2955(5) 0.2940(13) 0.5582(6) 0.114(4) Uani 1 d . . H15D H 0.3272(5) 0.3466(13) 0.5297(6) 0.170 Uiso 1 calc R . H15E H 0.3226(5) 0.2152(13) 0.5724(6) 0.170 Uiso 1 calc R . H15F H 0.2818(5) 0.3460(13) 0.5966(6) 0.170 Uiso 1 calc R . C16 C 0.1736(4) 0.1703(9) 0.5644(3) 0.067(2) Uani 1 d . . C17 C 0.1870(5) 0.1086(12) 0.6237(3) 0.091(3) Uani 1 d . . H17A H 0.2333(5) 0.1079(12) 0.6464(3) 0.110 Uiso 1 calc R . C18 C 0.1203(5) 0.0463(11) 0.6454(3) 0.093(3) Uani 1 d . . H18A H 0.1148(5) -0.0016(11) 0.6849(3) 0.111 Uiso 1 calc R . C19 C 0.0646(4) 0.0679(9) 0.5984(3) 0.064(2) Uani 1 d . . C20 C -0.0184(4) 0.0297(9) 0.5956(3) 0.067(2) Uani 1 d . . C20A C -0.0352(5) -0.0447(10) 0.5300(4) 0.083(3) Uani 1 d . . H20A H -0.0035(5) -0.1228(10) 0.5273(4) 0.124 Uiso 1 calc R . H20B H -0.0249(5) 0.0135(10) 0.4930(4) 0.124 Uiso 1 calc R . H20C H -0.0876(5) -0.0713(10) 0.5287(4) 0.124 Uiso 1 calc R . C20B C -0.0367(6) -0.0646(12) 0.6552(5) 0.099(3) Uani 1 d . . H20D H -0.0062(6) -0.1442(12) 0.6523(5) 0.148 Uiso 1 calc R . H20E H -0.0895(6) -0.0886(12) 0.6536(5) 0.148 Uiso 1 calc R . H20F H -0.0257(6) -0.0191(12) 0.6964(5) 0.148 Uiso 1 calc R . C21 C -0.0670(4) 0.1528(9) 0.6017(3) 0.063(2) Uani 1 d . . C22 C -0.1100(4) 0.1998(11) 0.6528(3) 0.077(3) Uani 1 d . . H22A H -0.1178(4) 0.1567(11) 0.6933(3) 0.092 Uiso 1 calc R . C23 C -0.1407(4) 0.3245(12) 0.6337(4) 0.082(3) Uani 1 d . . H23A H -0.1725(4) 0.3770(12) 0.6596(4) 0.098 Uiso 1 calc R . C24 C -0.1165(4) 0.3561(9) 0.5716(3) 0.063(2) Uani 1 d . . C25 C -0.1292(4) 0.4779(9) 0.5283(3) 0.064(2) Uani 1 d . . C25A C -0.0514(4) 0.5335(10) 0.5039(4) 0.079(3) Uani 1 d . . H25A H -0.0599(4) 0.6110(10) 0.4764(4) 0.119 Uiso 1 calc R . H25B H -0.0258(4) 0.4658(10) 0.4786(4) 0.119 Uiso 1 calc R . H25C H -0.0206(4) 0.5581(10) 0.5418(4) 0.119 Uiso 1 calc R . C25B C -0.1671(6) 0.5875(13) 0.5687(5) 0.105(4) Uani 1 d . . H25D H -0.1751(6) 0.6649(13) 0.5411(5) 0.158 Uiso 1 calc R . H25E H -0.1349(6) 0.6112(13) 0.6059(5) 0.158 Uiso 1 calc R . H25F H -0.2150(6) 0.5557(13) 0.5848(5) 0.158 Uiso 1 calc R . C26 C -0.1789(4) 0.4451(9) 0.4679(3) 0.067(2) Uani 1 d . . C27 C -0.2514(4) 0.4836(11) 0.4518(4) 0.089(3) Uani 1 d . . H27A H -0.2831(4) 0.5356(11) 0.4782(4) 0.106 Uiso 1 calc R . C28 C -0.2698(4) 0.4310(11) 0.3884(4) 0.084(3) Uani 1 d . . H28A H -0.3162(4) 0.4411(11) 0.3663(4) 0.101 Uiso 1 calc R . C29 C -0.2082(3) 0.3624(8) 0.3648(3) 0.061(2) Uani 1 d . . C30 C -0.1945(4) 0.2919(10) 0.3003(3) 0.065(2) Uani 1 d . . C30A C -0.1685(5) 0.1471(10) 0.3133(4) 0.077(3) Uani 1 d . . H30A H -0.1598(5) 0.1028(10) 0.2715(4) 0.116 Uiso 1 calc R . H30B H -0.2071(5) 0.1000(10) 0.3374(4) 0.116 Uiso 1 calc R . H30C H -0.1222(5) 0.1478(10) 0.3391(4) 0.116 Uiso 1 calc R . C30B C -0.2708(5) 0.2854(12) 0.2613(4) 0.098(3) Uani 1 d . . H30D H -0.2633(5) 0.2403(12) 0.2196(4) 0.148 Uiso 1 calc R . H30E H -0.2890(5) 0.3747(12) 0.2531(4) 0.148 Uiso 1 calc R . H30F H -0.3075(5) 0.2370(12) 0.2871(4) 0.148 Uiso 1 calc R . N40 N 0.4388(4) 0.7714(8) 0.5104(3) 0.084(2) Uani 1 d . . C41 C 0.4448(6) 0.8345(13) 0.4433(4) 0.103(3) Uani 1 d . . H41A H 0.4261(6) 0.7707(13) 0.4105(4) 0.124 Uiso 1 calc R . H41B H 0.4109(6) 0.9113(13) 0.4421(4) 0.124 Uiso 1 calc R . C42 C 0.5188(6) 0.8787(14) 0.4229(5) 0.110(4) Uani 1 d . . H42A H 0.5517(6) 0.8014(14) 0.4178(5) 0.132 Uiso 1 calc R . H42B H 0.5406(6) 0.9357(14) 0.4573(5) 0.132 Uiso 1 calc R . C43 C 0.5153(6) 0.9573(15) 0.3562(5) 0.118(4) Uani 1 d . . H43A H 0.4960(6) 0.8987(15) 0.3214(5) 0.142 Uiso 1 calc R . H43B H 0.4802(6) 1.0317(15) 0.3606(5) 0.142 Uiso 1 calc R . C44 C 0.5899(8) 1.0093(21) 0.3364(6) 0.162(7) Uani 1 d . . H44A H 0.5849(8) 1.0570(21) 0.2950(6) 0.243 Uiso 1 calc R . H44B H 0.6247(8) 0.9360(21) 0.3310(6) 0.243 Uiso 1 calc R . H44C H 0.6089(8) 1.0689(21) 0.3703(6) 0.243 Uiso 1 calc R . C45 C 0.4919(8) 0.6563(15) 0.5211(5) 0.127(4) Uani 1 d . . H45A H 0.5440(8) 0.6875(15) 0.5182(5) 0.152 Uiso 1 calc R . H45B H 0.4846(8) 0.6192(15) 0.5653(5) 0.152 Uiso 1 calc R . C46 C 0.4781(8) 0.5501(16) 0.4700(7) 0.135(5) Uani 1 d . . H46A H 0.4882(8) 0.5858(16) 0.4260(7) 0.162 Uiso 1 calc R . H46B H 0.4253(8) 0.5224(16) 0.4712(7) 0.162 Uiso 1 calc R . C47 C 0.5303(8) 0.4273(16) 0.4835(7) 0.139(5) Uani 1 d . . H47A H 0.5825(8) 0.4574(16) 0.4874(7) 0.167 Uiso 1 calc R . H47B H 0.5163(8) 0.3864(16) 0.5255(7) 0.167 Uiso 1 calc R . C48 C 0.5247(8) 0.3291(19) 0.4316(8) 0.160(6) Uani 1 d . . H48A H 0.5577(8) 0.2551(19) 0.4418(8) 0.239 Uiso 1 calc R . H48B H 0.5394(8) 0.3687(19) 0.3900(8) 0.239 Uiso 1 calc R . H48C H 0.4732(8) 0.2978(19) 0.4281(8) 0.239 Uiso 1 calc R . C49 C 0.4606(7) 0.8803(16) 0.5652(5) 0.129(5) Uani 1 d . . H49A H 0.5138(7) 0.9025(16) 0.5593(5) 0.154 Uiso 1 calc R . H49B H 0.4317(7) 0.9608(16) 0.5552(5) 0.154 Uiso 1 calc R . C50 C 0.4500(9) 0.8504(15) 0.6345(5) 0.129(5) Uani 1 d . . H50A H 0.4769(9) 0.7685(15) 0.6458(5) 0.155 Uiso 1 calc R . H50B H 0.3964(9) 0.8363(15) 0.6429(5) 0.155 Uiso 1 calc R . C51 C 0.4781(7) 0.9598(15) 0.6760(5) 0.110(4) Uani 1 d . . H51A H 0.4766(7) 0.9285(15) 0.7217(5) 0.132 Uiso 1 calc R . H51B H 0.5313(7) 0.9717(15) 0.6652(5) 0.132 Uiso 1 calc R . C52 C 0.4445(8) 1.0901(17) 0.6753(6) 0.126(5) Uani 1 d . . H52A H 0.4713(8) 1.1473(17) 0.7060(6) 0.189 Uiso 1 calc R . H52B H 0.3922(8) 1.0836(17) 0.6882(6) 0.189 Uiso 1 calc R . H52C H 0.4474(8) 1.1271(17) 0.6312(6) 0.189 Uiso 1 calc R . C53 C 0.3563(7) 0.7284(14) 0.5239(6) 0.121(4) Uani 1 d . . H53A H 0.3434(7) 0.6610(14) 0.4908(6) 0.145 Uiso 1 calc R . H53B H 0.3566(7) 0.6835(14) 0.5668(6) 0.145 Uiso 1 calc R . C54 C 0.2961(7) 0.8194(21) 0.5248(9) 0.171(7) Uani 1 d . . H54A H 0.2973(7) 0.8697(21) 0.4834(9) 0.205 Uiso 1 calc R . H54B H 0.3059(7) 0.8826(21) 0.5606(9) 0.205 Uiso 1 calc R . C55 C 0.2175(8) 0.7678(19) 0.5329(10) 0.155(6) Uani 1 d . . H55A H 0.2214(8) 0.6762(19) 0.5490(10) 0.186 Uiso 1 calc R . H55B H 0.1939(8) 0.8198(19) 0.5680(10) 0.186 Uiso 1 calc R . C56 C 0.1731(14) 0.7675(24) 0.4841(15) 0.243(13) Uani 1 d . . H56A H 0.1249(14) 0.7314(24) 0.4972(15) 0.364 Uiso 1 calc R . H56B H 0.1940(14) 0.7133(24) 0.4492(15) 0.364 Uiso 1 calc R . H56C H 0.1663(14) 0.8576(24) 0.4682(15) 0.364 Uiso 1 calc R . C60 C 0.3045(5) 0.3996(14) 0.2994(6) 0.108(4) Uani 1 d . . H60A H 0.2926(5) 0.3400(14) 0.3361(6) 0.129 Uiso 1 calc R . H60B H 0.2642(5) 0.3917(14) 0.2662(6) 0.129 Uiso 1 calc R . Cl1 Cl 0.3892(2) 0.3516(5) 0.2646(2) 0.1467(14) Uani 1 d . . Cl2 Cl 0.3082(2) 0.5656(5) 0.3288(2) 0.1489(14) Uani 1 d . . C65 C -0.2640(7) 0.1267(15) 0.5231(7) 0.129(5) Uani 1 d . . H65A H -0.2604(7) 0.1902(15) 0.4866(7) 0.155 Uiso 1 calc R . H65B H -0.2206(7) 0.1402(15) 0.5525(7) 0.155 Uiso 1 calc R . Cl3 Cl -0.3477(2) 0.1546(6) 0.5667(2) 0.172(2) Uani 1 d . . Cl4 Cl -0.2629(3) -0.0350(6) 0.4921(3) 0.191(2) Uani 1 d . . C70 C -0.4452(9) -0.3994(17) 0.1858(7) 0.144(5) Uani 1 d . . H70A H -0.4972(9) -0.3817(17) 0.1722(7) 0.173 Uiso 1 calc R . H70B H -0.4128(9) -0.3351(17) 0.1634(7) 0.173 Uiso 1 calc R . Cl5 Cl -0.4208(3) -0.5569(6) 0.1615(2) 0.173(2) Uani 1 d . . Cl6 Cl -0.4366(4) -0.3769(7) 0.2721(2) 0.202(2) Uani 1 d . . C75 C -0.1486(7) -0.3019(12) 0.3328(5) 0.104(3) Uani 1 d . . H75A H -0.1675(7) -0.3543(12) 0.3699(5) 0.124 Uiso 1 calc R . H75B H -0.1216(7) -0.3623(12) 0.3034(5) 0.124 Uiso 1 calc R . Cl7 Cl -0.0861(2) -0.1836(4) 0.3629(2) 0.1291(11) Uani 1 d . . Cl8 Cl -0.2260(2) -0.2333(4) 0.2892(2) 0.1493(14) Uani 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 Cl 0.0599(7) 0.109(2) 0.0507(6) 0.0156(9) 0.0041(5) 0.0275(9) N1 0.056(3) 0.050(5) 0.061(3) 0.010(3) -0.013(2) 0.003(2) N2 0.061(3) 0.059(5) 0.054(2) -0.001(3) 0.009(2) 0.010(3) N3 0.050(2) 0.063(5) 0.073(3) -0.001(3) -0.004(2) -0.005(3) N4 0.069(3) 0.065(6) 0.052(2) 0.009(2) -0.017(2) -0.004(3) N5 0.067(3) 0.068(6) 0.054(3) 0.004(3) 0.011(2) -0.004(3) N6 0.047(2) 0.069(5) 0.061(3) 0.004(3) -0.001(2) 0.013(2) C1 0.054(3) 0.073(7) 0.059(3) -0.001(3) -0.013(2) 0.006(3) C2 0.072(4) 0.067(7) 0.058(3) 0.005(3) -0.016(3) 0.010(4) C3 0.089(4) 0.054(7) 0.058(3) 0.009(3) -0.011(3) 0.009(4) C4 0.069(3) 0.045(6) 0.060(3) -0.001(3) -0.008(3) 0.002(3) C5 0.065(3) 0.047(6) 0.066(3) 0.008(3) -0.002(3) 0.000(3) C5A 0.077(4) 0.061(8) 0.088(5) -0.012(4) -0.019(3) 0.000(4) C5B 0.098(6) 0.068(9) 0.119(7) 0.033(6) -0.001(5) -0.007(5) C6 0.058(3) 0.059(7) 0.056(3) 0.007(3) 0.000(2) -0.001(3) C7 0.066(4) 0.085(8) 0.061(3) 0.015(4) 0.013(3) 0.007(4) C8 0.065(4) 0.105(9) 0.060(3) -0.007(4) 0.015(3) 0.003(4) C9 0.058(3) 0.076(7) 0.058(3) -0.005(3) 0.005(2) 0.005(3) C10 0.071(4) 0.064(7) 0.074(4) -0.010(4) 0.002(3) 0.015(4) C10A 0.098(5) 0.050(7) 0.085(4) 0.002(4) -0.017(4) -0.003(4) C10B 0.110(6) 0.101(10) 0.097(5) -0.027(5) 0.010(5) 0.042(6) C11 0.054(3) 0.067(7) 0.076(4) 0.007(3) 0.007(3) 0.020(3) C12 0.052(3) 0.098(9) 0.098(5) 0.020(5) 0.013(3) 0.015(4) C13 0.058(3) 0.070(8) 0.090(4) 0.017(4) -0.006(3) 0.001(3) C14 0.053(3) 0.057(7) 0.071(3) 0.009(3) -0.010(3) -0.009(3) C15 0.066(3) 0.060(7) 0.081(4) -0.008(4) -0.011(3) -0.016(4) C15A 0.116(6) 0.055(8) 0.099(5) -0.002(5) 0.010(5) -0.008(5) C15B 0.086(5) 0.127(11) 0.127(7) -0.031(7) -0.021(5) -0.040(6) C16 0.069(4) 0.061(7) 0.070(4) -0.004(3) -0.021(3) -0.001(3) C17 0.083(5) 0.132(10) 0.059(4) 0.001(4) -0.025(3) 0.006(5) C18 0.096(5) 0.134(10) 0.047(3) 0.019(4) -0.011(3) 0.009(5) C19 0.077(4) 0.065(7) 0.049(3) 0.006(3) -0.007(3) 0.000(4) C20 0.084(4) 0.053(7) 0.063(3) 0.021(3) -0.003(3) -0.009(4) C20A 0.079(4) 0.074(8) 0.096(5) -0.008(5) -0.010(4) -0.007(4) C20B 0.115(7) 0.072(9) 0.109(6) 0.030(5) 0.015(5) -0.004(5) C21 0.069(4) 0.068(7) 0.051(3) 0.006(3) 0.004(3) -0.013(4) C22 0.080(4) 0.091(9) 0.058(3) 0.006(4) 0.014(3) -0.016(5) C23 0.075(4) 0.108(10) 0.062(4) -0.011(5) 0.017(3) 0.001(5) C24 0.061(3) 0.065(7) 0.064(3) -0.012(4) 0.014(3) 0.004(3) C25 0.075(4) 0.053(6) 0.064(3) -0.008(3) 0.005(3) 0.014(4) C25A 0.078(4) 0.073(8) 0.087(5) 0.003(4) -0.015(3) -0.014(4) C25B 0.117(7) 0.101(11) 0.097(6) -0.029(6) 0.000(5) 0.042(6) C26 0.059(3) 0.068(7) 0.075(4) 0.002(4) 0.009(3) 0.011(3) C27 0.065(4) 0.109(9) 0.093(5) -0.001(5) 0.018(3) 0.022(4) C28 0.052(3) 0.112(9) 0.089(5) 0.017(5) 0.003(3) 0.011(4) C29 0.048(3) 0.066(7) 0.069(3) 0.014(3) -0.004(2) 0.002(3) C30 0.060(3) 0.061(8) 0.073(4) 0.007(4) -0.015(3) -0.002(3) C30A 0.095(5) 0.056(9) 0.081(4) 0.006(4) -0.002(4) -0.019(5) C30B 0.073(4) 0.130(10) 0.092(5) 0.003(5) -0.027(4) -0.026(5) N40 0.097(4) 0.073(7) 0.082(4) 0.006(3) -0.016(3) -0.004(4) C41 0.114(7) 0.117(11) 0.079(5) 0.009(5) -0.002(4) 0.001(6) C42 0.099(6) 0.141(12) 0.091(6) -0.003(6) -0.006(5) 0.000(6) C43 0.100(6) 0.175(14) 0.081(5) 0.012(6) 0.000(4) -0.016(7) C44 0.127(9) 0.257(21) 0.101(7) 0.002(9) 0.017(6) -0.034(11) C45 0.137(9) 0.142(14) 0.101(6) 0.023(7) -0.011(6) 0.012(8) C46 0.140(10) 0.139(15) 0.126(8) 0.028(9) -0.034(7) -0.020(9) C47 0.128(9) 0.135(15) 0.153(10) -0.016(10) -0.020(8) 0.038(9) C48 0.119(9) 0.180(19) 0.180(13) -0.050(12) 0.005(9) 0.000(9) C49 0.112(7) 0.191(15) 0.082(5) 0.006(7) -0.025(5) -0.009(8) C50 0.169(12) 0.125(13) 0.092(6) 0.007(7) -0.015(7) 0.000(9) C51 0.135(8) 0.107(13) 0.087(5) -0.009(6) -0.003(5) 0.006(8) C52 0.144(10) 0.127(15) 0.107(7) -0.012(7) -0.012(7) 0.008(9) C53 0.126(8) 0.112(12) 0.125(8) -0.009(7) 0.008(6) -0.032(8) C54 0.094(7) 0.224(21) 0.194(14) 0.061(13) -0.015(8) -0.030(10) C55 0.119(9) 0.140(17) 0.207(16) 0.006(12) -0.001(10) -0.026(9) C56 0.217(21) 0.168(22) 0.340(32) 0.061(21) -0.136(23) -0.010(17) C60 0.087(6) 0.117(12) 0.119(7) -0.006(7) -0.007(5) -0.009(6) Cl1 0.125(2) 0.178(4) 0.137(2) 0.018(2) 0.023(2) 0.007(2) Cl2 0.146(3) 0.121(4) 0.178(3) -0.016(2) -0.029(2) -0.017(2) C65 0.118(8) 0.119(14) 0.149(10) 0.006(9) -0.007(7) -0.039(8) Cl3 0.153(3) 0.218(6) 0.146(3) 0.021(3) 0.018(2) 0.054(3) Cl4 0.152(3) 0.195(6) 0.224(5) -0.050(4) -0.022(3) 0.016(3) C70 0.140(10) 0.133(15) 0.160(11) 0.040(10) -0.038(8) 0.031(9) Cl5 0.188(4) 0.177(5) 0.154(3) -0.001(3) -0.058(3) 0.056(3) Cl6 0.249(6) 0.203(6) 0.153(3) -0.021(3) -0.040(4) -0.003(4) C75 0.134(8) 0.075(9) 0.101(6) 0.011(5) -0.012(5) 0.027(6) Cl7 0.165(3) 0.089(3) 0.132(2) -0.002(2) -0.045(2) -0.005(2) Cl8 0.123(2) 0.121(3) 0.202(3) 0.023(3) -0.043(2) 0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl N2 3.265(5) . ? Cl N6 3.286(5) . ? Cl N1 3.287(5) . ? Cl N5 3.294(5) . ? Cl N4 3.295(5) . ? Cl N3 3.305(5) . ? N1 C4 1.355(9) . ? N1 C1 1.388(8) . ? N2 C6 1.365(9) . ? N2 C9 1.376(9) . ? N3 C11 1.361(9) . ? N3 C14 1.364(8) . ? N4 C19 1.380(9) . ? N4 C16 1.385(9) . ? N5 C24 1.374(10) . ? N5 C21 1.386(10) . ? N6 C26 1.374(9) . ? N6 C29 1.390(8) . ? C1 C2 1.350(10) . ? C1 C30 1.513(11) . ? C2 C3 1.396(11) . ? C3 C4 1.353(9) . ? C4 C5 1.528(9) . ? C5 C6 1.510(11) . ? C5 C5B 1.524(12) . ? C5 C5A 1.552(10) . ? C6 C7 1.375(10) . ? C7 C8 1.408(13) . ? C8 C9 1.376(10) . ? C9 C10 1.515(12) . ? C10 C11 1.499(10) . ? C10 C10A 1.529(12) . ? C10 C10B 1.551(11) . ? C11 C12 1.383(10) . ? C12 C13 1.391(13) . ? C13 C14 1.361(10) . ? C14 C15 1.517(11) . ? C15 C16 1.491(11) . ? C15 C15B 1.553(10) . ? C15 C15A 1.563(13) . ? C16 C17 1.356(11) . ? C17 C18 1.400(13) . ? C18 C19 1.370(10) . ? C19 C20 1.508(10) . ? C20 C21 1.502(12) . ? C20 C20A 1.536(11) . ? C20 C20B 1.556(11) . ? C21 C22 1.362(11) . ? C22 C23 1.406(14) . ? C23 C24 1.357(10) . ? C24 C25 1.508(12) . ? C25 C25B 1.519(12) . ? C25 C26 1.520(10) . ? C25 C25A 1.561(11) . ? C26 C27 1.368(10) . ? C27 C28 1.411(13) . ? C28 C29 1.369(10) . ? C29 C30 1.493(11) . ? C30 C30A 1.536(13) . ? C30 C30B 1.549(8) . ? N40 C41 1.489(11) . ? N40 C45 1.494(15) . ? N40 C53 1.540(13) . ? N40 C49 1.590(15) . ? C41 C42 1.439(14) . ? C42 C43 1.550(15) . ? C43 C44 1.47(2) . ? C45 C46 1.49(2) . ? C46 C47 1.55(2) . ? C47 C48 1.43(2) . ? C49 C50 1.434(15) . ? C50 C51 1.46(2) . ? C51 C52 1.43(2) . ? C53 C54 1.39(2) . ? C54 C55 1.49(2) . ? C55 C56 1.25(2) . ? C60 Cl1 1.720(11) . ? C60 Cl2 1.758(14) . ? C65 Cl4 1.73(2) . ? C65 Cl3 1.742(14) . ? C70 Cl5 1.70(2) . ? C70 Cl6 1.75(2) . ? C75 Cl7 1.719(13) . ? C75 Cl8 1.749(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 N2 Cl N6 120.11(14) . . ? N2 Cl N1 61.41(13) . . ? N6 Cl N1 59.28(13) . . ? N2 Cl N5 166.8(2) . . ? N6 Cl N5 60.91(13) . . ? N1 Cl N5 119.89(15) . . ? N2 Cl N4 117.72(14) . . ? N6 Cl N4 118.10(14) . . ? N1 Cl N4 167.2(2) . . ? N5 Cl N4 57.71(14) . . ? N2 Cl N3 58.48(13) . . ? N6 Cl N3 167.0(2) . . ? N1 Cl N3 119.57(14) . . ? N5 Cl N3 117.15(14) . . ? N4 Cl N3 59.73(14) . . ? C4 N1 C1 110.1(5) . . ? C4 N1 Cl 125.8(4) . . ? C1 N1 Cl 123.8(4) . . ? C6 N2 C9 111.5(5) . . ? C6 N2 Cl 123.9(4) . . ? C9 N2 Cl 123.3(4) . . ? C11 N3 C14 112.3(5) . . ? C11 N3 Cl 122.3(4) . . ? C14 N3 Cl 124.3(5) . . ? C19 N4 C16 111.4(5) . . ? C19 N4 Cl 123.6(4) . . ? C16 N4 Cl 124.9(4) . . ? C24 N5 C21 111.7(6) . . ? C24 N5 Cl 125.2(4) . . ? C21 N5 Cl 123.0(5) . . ? C26 N6 C29 111.2(5) . . ? C26 N6 Cl 125.2(4) . . ? C29 N6 Cl 123.5(4) . . ? C2 C1 N1 106.3(6) . . ? C2 C1 C30 131.3(5) . . ? N1 C1 C30 122.1(5) . . ? C1 C2 C3 108.1(6) . . ? C4 C3 C2 108.6(7) . . ? C3 C4 N1 106.8(6) . . ? C3 C4 C5 131.6(7) . . ? N1 C4 C5 121.5(6) . . ? C6 C5 C5B 109.4(6) . . ? C6 C5 C4 112.4(6) . . ? C5B C5 C4 109.0(6) . . ? C6 C5 C5A 109.6(6) . . ? C5B C5 C5A 108.1(7) . . ? C4 C5 C5A 108.2(6) . . ? N2 C6 C7 106.6(7) . . ? N2 C6 C5 123.6(5) . . ? C7 C6 C5 129.8(7) . . ? C6 C7 C8 107.7(6) . . ? C9 C8 C7 108.6(7) . . ? C8 C9 N2 105.6(7) . . ? C8 C9 C10 132.3(7) . . ? N2 C9 C10 122.1(5) . . ? C11 C10 C9 109.8(7) . . ? C11 C10 C10A 110.6(6) . . ? C9 C10 C10A 111.0(6) . . ? C11 C10 C10B 108.6(6) . . ? C9 C10 C10B 108.7(6) . . ? C10A C10 C10B 108.1(8) . . ? N3 C11 C12 104.8(7) . . ? N3 C11 C10 123.5(5) . . ? C12 C11 C10 131.5(7) . . ? C11 C12 C13 108.5(7) . . ? C14 C13 C12 108.5(6) . . ? C13 C14 N3 105.8(7) . . ? C13 C14 C15 131.7(6) . . ? N3 C14 C15 122.5(6) . . ? C16 C15 C14 114.3(7) . . ? C16 C15 C15B 108.9(7) . . ? C14 C15 C15B 108.2(7) . . ? C16 C15 C15A 110.2(7) . . ? C14 C15 C15A 107.3(7) . . ? C15B C15 C15A 107.7(8) . . ? C17 C16 N4 105.3(7) . . ? C17 C16 C15 132.8(7) . . ? N4 C16 C15 121.9(6) . . ? C16 C17 C18 109.6(6) . . ? C19 C18 C17 108.2(7) . . ? C18 C19 N4 105.6(7) . . ? C18 C19 C20 132.2(7) . . ? N4 C19 C20 122.2(5) . . ? C21 C20 C19 110.0(7) . . ? C21 C20 C20A 111.0(6) . . ? C19 C20 C20A 109.4(6) . . ? C21 C20 C20B 108.0(7) . . ? C19 C20 C20B 109.4(6) . . ? C20A C20 C20B 109.0(8) . . ? C22 C21 N5 105.3(8) . . ? C22 C21 C20 131.5(7) . . ? N5 C21 C20 123.0(6) . . ? C21 C22 C23 108.3(7) . . ? C24 C23 C22 109.4(7) . . ? C23 C24 N5 105.2(8) . . ? C23 C24 C25 132.0(7) . . ? N5 C24 C25 122.7(5) . . ? C24 C25 C25B 109.6(6) . . ? C24 C25 C26 111.5(7) . . ? C25B C25 C26 109.2(7) . . ? C24 C25 C25A 109.9(6) . . ? C25B C25 C25A 107.6(8) . . ? C26 C25 C25A 109.0(6) . . ? C27 C26 N6 106.3(6) . . ? C27 C26 C25 130.9(7) . . ? N6 C26 C25 122.7(6) . . ? C26 C27 C28 108.3(7) . . ? C29 C28 C27 108.8(6) . . ? C28 C29 N6 105.4(6) . . ? C28 C29 C30 132.0(6) . . ? N6 C29 C30 122.5(5) . . ? C29 C30 C1 111.3(7) . . ? C29 C30 C30A 110.3(6) . . ? C1 C30 C30A 110.8(6) . . ? C29 C30 C30B 108.1(6) . . ? C1 C30 C30B 108.7(6) . . ? C30A C30 C30B 107.5(7) . . ? C41 N40 C45 113.9(8) . . ? C41 N40 C53 110.6(8) . . ? C45 N40 C53 110.5(9) . . ? C41 N40 C49 108.5(8) . . ? C45 N40 C49 106.2(8) . . ? C53 N40 C49 106.9(8) . . ? C42 C41 N40 117.3(8) . . ? C41 C42 C43 111.9(8) . . ? C44 C43 C42 112.6(10) . . ? C46 C45 N40 110.4(9) . . ? C45 C46 C47 110.4(10) . . ? C48 C47 C46 112.1(12) . . ? C50 C49 N40 119.7(12) . . ? C49 C50 C51 110.6(13) . . ? C52 C51 C50 122.6(11) . . ? C54 C53 N40 122.6(12) . . ? C53 C54 C55 118.9(17) . . ? C56 C55 C54 119.4(21) . . ? Cl1 C60 Cl2 111.6(7) . . ? Cl4 C65 Cl3 110.0(7) . . ? Cl5 C70 Cl6 112.4(8) . . ? Cl7 C75 Cl8 113.6(7) . . ? _refine_diff_density_max 0.252 _refine_diff_density_min -0.227 _refine_diff_density_rms 0.042