data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44.40 H34.40 Cl7.20 N4 O8 S2' _chemical_formula_weight 1071.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M 'P 21 21 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' '-x, -y, z' _cell_length_a 15.769(12) _cell_length_b 27.12(2) _cell_length_c 11.319(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4841(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2189 _exptl_absorpt_coefficient_mu 0.563 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8814 _exptl_absorpt_correction_T_max 0.9153 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 64709 _diffrn_reflns_av_R_equivalents 0.0674 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.44 _reflns_number_total 10986 _reflns_number_gt 10548 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0962P)^2^+2.4643P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.07(6) _refine_ls_number_reflns 10986 _refine_ls_number_parameters 651 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0626 _refine_ls_R_factor_gt 0.0601 _refine_ls_wR_factor_ref 0.1665 _refine_ls_wR_factor_gt 0.1639 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C101 C 0.5295(3) 0.67378(17) 0.1948(4) 0.0423(9) Uani 1 1 d D A 1 H101 H 0.530(3) 0.6947(18) 0.124(5) 0.051 Uiso 1 1 d . B 1 Cl11 Cl 0.43432(8) 0.66282(6) 0.27208(11) 0.0602(3) Uani 1 1 d D A 1 Cl12 Cl 0.55988(7) 0.62084(5) 0.11629(11) 0.0573(3) Uani 1 1 d D A 1 Cl13 Cl 0.61144(8) 0.69334(4) 0.28920(11) 0.0539(3) Uani 1 1 d D A 1 C201 C 0.4765(7) 1.0131(4) 0.4101(9) 0.049(3) Uiso 0.40 1 d PD . 2 Cl21 Cl 0.4908(4) 1.06167(16) 0.4891(3) 0.0989(18) Uani 0.40 1 d PD . 2 Cl22 Cl 0.42235(18) 0.97016(12) 0.4827(3) 0.0558(7) Uani 0.40 1 d PD . 2 Cl23 Cl 0.4653(3) 1.00158(16) 0.2849(4) 0.0917(15) Uani 0.40 1 d PD . 2 C301 C 0.5362(4) 0.9192(2) 0.7887(5) 0.0482(14) Uani 0.70 1 d PD C 3 H301 H 0.4779 0.9238 0.7558 0.058 Uiso 0.70 1 calc PR C 3 Cl31 Cl 0.60183(13) 0.97121(7) 0.74808(17) 0.0604(4) Uani 0.70 1 d PD C 3 Cl32 Cl 0.53098(12) 0.91394(8) 0.94362(16) 0.0478(4) Uani 0.70 1 d PD C 3 Cl33 Cl 0.58246(13) 0.86477(10) 0.7288(2) 0.0628(6) Uani 0.70 1 d PD C 3 C401 C 0.5840(11) 0.8688(9) 0.7758(11) 0.134(19) Uani 0.30 1 d PD D 4 H401 H 0.5507 0.8381 0.7606 0.160 Uiso 0.30 1 calc PR D 4 Cl41 Cl 0.6873(3) 0.84721(17) 0.7794(4) 0.0611(10) Uani 0.30 1 d PD D 4 Cl42 Cl 0.5407(3) 0.8900(2) 0.9056(5) 0.0632(12) Uani 0.30 1 d PD D 4 Cl43 Cl 0.5627(4) 0.9036(2) 0.6534(5) 0.0771(13) Uani 0.30 1 d PD D 4 S1 S 0.86787(5) 0.74700(3) 0.02400(7) 0.02948(19) Uani 1 1 d . . . S2 S 0.63757(5) 0.86378(3) 0.25213(8) 0.03061(19) Uani 1 1 d . . . O7 O 0.59103(16) 0.61719(9) 0.7647(2) 0.0328(5) Uani 1 1 d . . . O8 O 0.92118(15) 0.78975(10) 0.0196(2) 0.0323(5) Uani 1 1 d . . . O9 O 0.50064(19) 0.73459(11) 0.6870(3) 0.0431(7) Uani 1 1 d . . . O10 O 0.56073(17) 0.88786(10) 0.2157(2) 0.0383(6) Uani 1 1 d . . . O56 O 0.71415(18) 0.89162(10) 0.2705(3) 0.0383(6) Uani 1 1 d . . . O57 O 0.86794(16) 0.71329(11) -0.0734(2) 0.0377(6) Uani 1 1 d . . . O58 O 0.78442(15) 0.61050(9) 0.7178(2) 0.0319(5) Uani 1 1 d . . . O59 O 0.94054(15) 0.67325(10) 0.5498(2) 0.0322(5) Uani 1 1 d . . . N5 N 0.82073(18) 0.62925(11) 0.4995(3) 0.0315(6) Uani 1 1 d . . . H5 H 0.7776 0.6133 0.5306 0.038 Uiso 1 1 calc R . . N53 N 0.89615(17) 0.71848(11) 0.1439(3) 0.0288(6) Uani 1 1 d . . . H53 H 0.9414 0.7297 0.1807 0.035 Uiso 1 1 calc R . . N54 N 0.63697(19) 0.70462(11) 0.6662(3) 0.0303(6) Uani 1 1 d . . . H54 H 0.6706 0.6804 0.6882 0.036 Uiso 1 1 calc R . . N55 N 0.61255(18) 0.83492(12) 0.3726(3) 0.0318(6) Uani 1 1 d . . . H55 H 0.5594 0.8375 0.3953 0.059(15) Uiso 1 1 calc R . . C4 C 0.7739(2) 0.56919(12) 0.7898(3) 0.0279(7) Uani 1 1 d . . . C6 C 0.6875(2) 0.49958(13) 0.8470(3) 0.0277(6) Uani 1 1 d . . . C7 C 0.7041(2) 0.53990(12) 0.7688(3) 0.0265(6) Uani 1 1 d . . . C8 C 0.8576(2) 0.67460(13) 0.3182(3) 0.0272(7) Uani 1 1 d . . . H8 H 0.8838 0.7000 0.3628 0.033 Uiso 1 1 calc R . . C9 C 0.8796(2) 0.64673(12) 0.5767(3) 0.0290(7) Uani 1 1 d . . . C10 C 0.6490(2) 0.54972(12) 0.6632(3) 0.0260(6) Uani 1 1 d . . . C11 C 0.6563(2) 0.51923(13) 0.5597(3) 0.0304(7) Uani 1 1 d . . . C12 C 0.6614(2) 0.81760(13) 0.1459(3) 0.0289(7) Uani 1 1 d . . . C13 C 0.6663(2) 0.80588(13) 0.4461(3) 0.0276(7) Uani 1 1 d . . . C14 C 0.6253(2) 0.77158(12) 0.5186(3) 0.0272(6) Uani 1 1 d . . . H14 H 0.5654 0.7682 0.5162 0.033 Uiso 1 1 calc R . . C15 C 0.8209(2) 0.63380(14) 0.3746(3) 0.0292(7) Uani 1 1 d . . . C16 C 0.8315(2) 0.55902(14) 0.8820(3) 0.0343(8) Uani 1 1 d . . . H16 H 0.8786 0.5801 0.8953 0.041 Uiso 1 1 calc R . . C17 C 0.8546(2) 0.67701(13) 0.1950(3) 0.0281(7) Uani 1 1 d . . . C18 C 0.7458(2) 0.48828(13) 0.9390(3) 0.0307(7) Uani 1 1 d . . . C19 C 0.6740(2) 0.74237(12) 0.5946(3) 0.0280(7) Uani 1 1 d . . . C20 C 0.6068(2) 0.53043(14) 0.4586(3) 0.0346(8) Uani 1 1 d . . . C21 C 0.8017(2) 0.78083(15) 0.5223(4) 0.0372(8) Uani 1 1 d . . . H21 H 0.8618 0.7833 0.5224 0.045 Uiso 1 1 calc R . . C22 C 0.7611(2) 0.76681(14) 0.0449(3) 0.0299(7) Uani 1 1 d . . . C23 C 0.7555(2) 0.81033(14) 0.4468(3) 0.0327(8) Uani 1 1 d . . . H23 H 0.7832 0.8332 0.3962 0.039 Uiso 1 1 calc R . . C24 C 0.7450(2) 0.80294(14) 0.1287(3) 0.0290(7) Uani 1 1 d . . . H24 H 0.7898 0.8173 0.1731 0.035 Uiso 1 1 calc R . . C25 C 0.6164(3) 0.50141(16) 0.3539(3) 0.0408(9) Uani 1 1 d . . . H25 H 0.5843 0.5091 0.2854 0.049 Uiso 1 1 calc R . . C26 C 0.5504(3) 0.57087(15) 0.4631(4) 0.0395(9) Uani 1 1 d . . . H26 H 0.5171 0.5784 0.3955 0.047 Uiso 1 1 calc R . . C27 C 0.5925(2) 0.58879(12) 0.6624(3) 0.0283(7) Uani 1 1 d . . . C28 C 0.8678(2) 0.63031(13) 0.7030(3) 0.0298(7) Uani 1 1 d . . . H28A H 0.9105 0.6049 0.7230 0.036 Uiso 1 1 calc R . . H28B H 0.8758 0.6587 0.7568 0.036 Uiso 1 1 calc R . . C29 C 0.5305(3) 0.65637(14) 0.7716(4) 0.0378(8) Uani 1 1 d . . . H29A H 0.5223 0.6653 0.8557 0.045 Uiso 1 1 calc R . . H29B H 0.4754 0.6443 0.7410 0.045 Uiso 1 1 calc R . . C30 C 0.7293(3) 0.44765(14) 1.0144(3) 0.0376(8) Uani 1 1 d . . . H30 H 0.7695 0.4391 1.0735 0.045 Uiso 1 1 calc R . . C31 C 0.5551(2) 0.70219(14) 0.7040(3) 0.0328(7) Uani 1 1 d . . . C32 C 0.6567(3) 0.42050(14) 1.0037(3) 0.0401(9) Uani 1 1 d . . . H32 H 0.6462 0.3938 1.0561 0.048 Uiso 1 1 calc R . . C33 C 0.6971(2) 0.74643(16) -0.0233(4) 0.0387(9) Uani 1 1 d . . . H33 H 0.7096 0.7217 -0.0801 0.046 Uiso 1 1 calc R . . C34 C 0.7816(2) 0.59636(15) 0.3085(3) 0.0353(8) Uani 1 1 d . . . H34 H 0.7570 0.5688 0.3476 0.042 Uiso 1 1 calc R . . C35 C 0.7204(3) 0.45090(16) 0.4539(4) 0.0429(9) Uani 1 1 d . . . H35 H 0.7586 0.4238 0.4520 0.052 Uiso 1 1 calc R . . C36 C 0.6720(3) 0.46228(16) 0.3522(4) 0.0458(10) Uani 1 1 d . . . H36 H 0.6780 0.4429 0.2827 0.055 Uiso 1 1 calc R . . C37 C 0.6127(2) 0.47008(13) 0.8358(3) 0.0321(7) Uani 1 1 d . . . H37 H 0.5734 0.4766 0.7742 0.039 Uiso 1 1 calc R . . C38 C 0.8191(2) 0.51847(14) 0.9526(3) 0.0345(8) Uani 1 1 d . . . H38 H 0.8599 0.5105 1.0113 0.041 Uiso 1 1 calc R . . C40 C 0.5422(2) 0.59954(14) 0.5620(3) 0.0354(8) Uani 1 1 d . . . H40 H 0.5033 0.6263 0.5632 0.043 Uiso 1 1 calc R . . C41 C 0.7627(2) 0.74759(14) 0.5985(3) 0.0350(8) Uani 1 1 d . . . H41 H 0.7955 0.7287 0.6524 0.042 Uiso 1 1 calc R . . C42 C 0.8151(2) 0.64027(15) 0.1288(4) 0.0371(8) Uani 1 1 d . . . H42 H 0.8127 0.6426 0.0452 0.045 Uiso 1 1 calc R . . C44 C 0.5976(3) 0.43214(15) 0.9146(3) 0.0403(9) Uani 1 1 d . . . H44 H 0.5466 0.4136 0.9086 0.048 Uiso 1 1 calc R . . C45 C 0.7130(3) 0.47847(14) 0.5557(3) 0.0348(8) Uani 1 1 d . . . H45 H 0.7458 0.4702 0.6232 0.042 Uiso 1 1 calc R . . C47 C 0.5950(2) 0.79840(15) 0.0780(4) 0.0364(8) Uani 1 1 d . . . H47 H 0.5384 0.8093 0.0894 0.044 Uiso 1 1 calc R . . C48 C 0.7786(3) 0.59949(16) 0.1873(4) 0.0409(9) Uani 1 1 d . . . H48 H 0.7518 0.5742 0.1429 0.049 Uiso 1 1 calc R . . C49 C 0.6143(2) 0.76271(18) -0.0072(4) 0.0452(10) Uani 1 1 d . . . H49 H 0.5702 0.7494 -0.0547 0.054 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C101 0.041(2) 0.053(2) 0.0330(19) -0.0066(18) -0.0094(16) -0.0003(19) Cl11 0.0473(6) 0.0900(9) 0.0434(6) 0.0052(6) 0.0052(5) 0.0057(6) Cl12 0.0457(6) 0.0699(8) 0.0563(6) -0.0272(6) -0.0157(5) 0.0088(5) Cl13 0.0612(7) 0.0510(6) 0.0495(6) -0.0062(5) -0.0255(5) -0.0063(5) Cl21 0.171(5) 0.086(3) 0.0400(16) 0.0043(16) 0.010(2) -0.078(3) Cl22 0.0445(14) 0.0654(17) 0.0574(15) -0.0036(14) 0.0093(12) -0.0365(14) Cl23 0.125(4) 0.0530(17) 0.097(3) 0.002(2) -0.062(3) 0.009(3) C301 0.054(4) 0.050(3) 0.041(3) -0.012(3) 0.002(3) -0.004(3) Cl31 0.0693(11) 0.0557(9) 0.0562(10) 0.0006(8) 0.0106(9) -0.0096(8) Cl32 0.0410(8) 0.0601(11) 0.0424(8) -0.0036(8) 0.0081(6) -0.0058(8) Cl33 0.0575(10) 0.0583(12) 0.0725(14) -0.0257(11) 0.0112(10) 0.0018(9) C401 0.25(4) 0.036(11) 0.11(2) 0.007(14) -0.14(3) 0.011(16) Cl41 0.048(2) 0.066(2) 0.070(3) -0.017(2) -0.0021(19) 0.0037(18) Cl42 0.049(2) 0.072(3) 0.069(3) 0.016(3) 0.007(2) -0.005(2) Cl43 0.074(3) 0.088(4) 0.069(3) 0.007(3) 0.011(3) -0.001(3) S1 0.0186(3) 0.0462(5) 0.0237(3) -0.0033(3) 0.0022(3) -0.0012(3) S2 0.0267(4) 0.0313(4) 0.0338(4) 0.0035(4) 0.0072(3) 0.0006(3) O7 0.0339(13) 0.0291(12) 0.0355(13) -0.0028(10) -0.0006(11) 0.0078(10) O8 0.0217(10) 0.0462(14) 0.0290(11) 0.0051(11) 0.0022(9) -0.0043(10) O9 0.0443(15) 0.0422(15) 0.0427(15) 0.0120(12) 0.0181(13) 0.0222(13) O10 0.0338(13) 0.0400(14) 0.0410(14) 0.0138(12) 0.0084(11) 0.0111(11) O56 0.0394(14) 0.0340(13) 0.0415(14) 0.0007(12) 0.0091(12) -0.0093(11) O57 0.0282(12) 0.0563(16) 0.0288(12) -0.0118(12) 0.0020(10) -0.0008(12) O58 0.0208(10) 0.0326(12) 0.0423(14) 0.0142(11) -0.0028(10) -0.0039(10) O59 0.0237(11) 0.0381(13) 0.0347(13) 0.0076(11) -0.0067(10) -0.0076(10) N5 0.0264(13) 0.0347(15) 0.0333(15) 0.0025(12) -0.0020(11) -0.0105(12) N53 0.0191(12) 0.0388(16) 0.0287(14) -0.0026(12) -0.0020(11) -0.0038(11) N54 0.0307(14) 0.0262(14) 0.0339(14) -0.0015(12) -0.0026(12) 0.0037(12) N55 0.0233(13) 0.0395(16) 0.0326(15) 0.0078(13) 0.0082(11) 0.0049(12) C4 0.0271(15) 0.0267(16) 0.0300(16) 0.0039(13) 0.0035(13) 0.0023(13) C6 0.0285(16) 0.0267(15) 0.0278(15) -0.0019(13) 0.0054(13) 0.0018(13) C7 0.0271(15) 0.0231(15) 0.0294(15) -0.0014(13) 0.0012(13) 0.0016(12) C8 0.0209(14) 0.0306(16) 0.0300(16) -0.0016(13) -0.0034(12) -0.0013(13) C9 0.0266(16) 0.0269(16) 0.0335(17) 0.0071(13) -0.0025(13) -0.0001(13) C10 0.0245(15) 0.0239(15) 0.0295(15) 0.0034(13) 0.0021(12) -0.0025(12) C11 0.0291(16) 0.0333(17) 0.0289(16) -0.0038(14) 0.0065(13) -0.0067(14) C12 0.0219(15) 0.0332(18) 0.0315(16) 0.0048(14) 0.0006(13) -0.0018(13) C13 0.0245(15) 0.0298(16) 0.0285(15) -0.0051(13) 0.0007(12) 0.0030(13) C14 0.0252(15) 0.0304(16) 0.0261(14) -0.0027(13) 0.0002(13) 0.0021(13) C15 0.0206(14) 0.0344(18) 0.0327(16) -0.0034(14) -0.0020(13) -0.0031(13) C16 0.0318(17) 0.0341(19) 0.0369(19) 0.0057(15) -0.0034(15) -0.0041(15) C17 0.0196(14) 0.0361(18) 0.0284(16) -0.0026(13) 0.0013(12) -0.0047(13) C18 0.0352(18) 0.0289(17) 0.0280(15) 0.0003(13) 0.0029(14) 0.0002(14) C19 0.0322(16) 0.0215(15) 0.0303(16) -0.0069(13) 0.0001(13) 0.0021(13) C20 0.0300(17) 0.0363(18) 0.0376(19) 0.0021(15) 0.0004(14) -0.0131(15) C21 0.0245(15) 0.043(2) 0.044(2) -0.0052(17) -0.0034(15) -0.0010(15) C22 0.0218(14) 0.0410(19) 0.0268(16) -0.0004(14) -0.0013(12) -0.0054(14) C23 0.0234(15) 0.0352(18) 0.0395(19) -0.0073(15) 0.0047(14) -0.0067(14) C24 0.0203(14) 0.0386(18) 0.0281(15) 0.0029(14) 0.0027(12) -0.0046(13) C25 0.040(2) 0.048(2) 0.0344(18) -0.0024(17) -0.0025(16) -0.0216(18) C26 0.039(2) 0.044(2) 0.0360(19) 0.0043(17) -0.0099(16) -0.0090(17) C27 0.0268(16) 0.0265(16) 0.0316(16) 0.0018(13) 0.0026(13) -0.0030(13) C28 0.0241(15) 0.0299(16) 0.0353(17) 0.0035(14) -0.0022(13) -0.0053(13) C29 0.0363(18) 0.0350(19) 0.042(2) 0.0021(16) 0.0045(16) 0.0112(16) C30 0.048(2) 0.0353(19) 0.0290(17) 0.0036(15) -0.0020(16) -0.0018(17) C31 0.0347(18) 0.0325(18) 0.0312(16) 0.0000(14) 0.0046(14) 0.0130(14) C32 0.053(2) 0.0346(19) 0.0327(18) 0.0078(15) 0.0074(17) -0.0106(17) C33 0.0247(16) 0.053(2) 0.0381(19) -0.0177(18) -0.0031(14) -0.0015(16) C34 0.0306(17) 0.0350(19) 0.0402(19) -0.0058(16) -0.0006(15) -0.0094(15) C35 0.051(2) 0.039(2) 0.039(2) -0.0089(17) 0.0144(18) -0.0016(18) C36 0.051(2) 0.045(2) 0.042(2) -0.0132(19) 0.0104(19) -0.016(2) C37 0.0352(18) 0.0329(17) 0.0283(16) -0.0028(14) 0.0040(14) -0.0073(15) C38 0.0346(18) 0.0367(18) 0.0323(17) 0.0060(15) -0.0046(14) -0.0022(15) C40 0.0343(18) 0.0317(18) 0.0403(19) 0.0041(15) -0.0110(15) 0.0017(15) C41 0.0280(16) 0.038(2) 0.0394(18) -0.0025(16) -0.0043(14) 0.0050(15) C42 0.0288(17) 0.048(2) 0.0347(18) -0.0117(17) 0.0032(14) -0.0103(16) C44 0.053(2) 0.036(2) 0.0321(18) -0.0021(15) 0.0075(17) -0.0146(18) C45 0.0408(19) 0.0317(18) 0.0319(17) 0.0019(15) 0.0076(15) 0.0001(15) C47 0.0187(15) 0.047(2) 0.043(2) -0.0022(17) 0.0011(14) -0.0008(15) C48 0.0328(19) 0.045(2) 0.045(2) -0.0086(18) 0.0006(16) -0.0101(17) C49 0.0204(16) 0.064(3) 0.051(2) -0.017(2) -0.0081(15) -0.0019(17) _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 C101 Cl12 1.755(5) . ? C101 Cl13 1.758(4) . ? C101 Cl11 1.763(5) . ? C201 C201 1.03(2) 4_675 ? C201 Cl23 1.462(10) . ? C201 Cl21 1.609(10) . ? C201 Cl22 1.662(11) . ? C201 Cl23 1.735(11) 4_675 ? C201 Cl22 1.851(11) 4_675 ? Cl21 Cl22 1.620(7) 4_675 ? Cl22 Cl21 1.620(7) 4_675 ? Cl22 C201 1.851(12) 4_675 ? Cl23 Cl23 1.099(10) 4_675 ? Cl23 C201 1.735(11) 4_675 ? C301 Cl32 1.762(6) . ? C301 Cl33 1.781(6) . ? C301 Cl31 1.808(6) . ? C401 Cl43 1.711(13) . ? C401 Cl42 1.719(13) . ? C401 Cl41 1.730(12) . ? S1 O57 1.432(3) . ? S1 O8 1.433(3) . ? S1 N53 1.624(3) . ? S1 C22 1.783(4) . ? S2 O10 1.437(3) . ? S2 O56 1.439(3) . ? S2 N55 1.621(3) . ? S2 C12 1.777(4) . ? O7 C27 1.390(4) . ? O7 C29 1.431(4) . ? O9 C31 1.244(4) . ? O58 C4 1.396(4) . ? O58 C28 1.430(4) . ? O59 C9 1.238(4) . ? N5 C9 1.360(4) . ? N5 C15 1.420(5) . ? N53 C17 1.424(5) . ? N54 C31 1.361(5) . ? N54 C19 1.431(5) . ? N55 C13 1.425(5) . ? C4 C7 1.378(5) . ? C4 C16 1.410(5) . ? C6 C18 1.423(5) . ? C6 C7 1.431(5) . ? C6 C37 1.431(5) . ? C7 C10 1.502(5) . ? C8 C17 1.397(5) . ? C8 C15 1.402(5) . ? C9 C28 1.509(5) . ? C10 C27 1.384(5) . ? C10 C11 1.438(5) . ? C11 C20 1.419(5) . ? C11 C45 1.423(5) . ? C12 C24 1.390(5) . ? C12 C47 1.399(5) . ? C13 C14 1.399(5) . ? C13 C23 1.412(5) . ? C14 C19 1.400(5) . ? C15 C34 1.406(5) . ? C16 C38 1.373(5) . ? C17 C42 1.394(5) . ? C18 C30 1.418(5) . ? C18 C38 1.424(5) . ? C19 C41 1.406(5) . ? C20 C26 1.413(6) . ? C20 C25 1.430(6) . ? C21 C23 1.380(6) . ? C21 C41 1.391(6) . ? C22 C33 1.386(5) . ? C22 C24 1.387(5) . ? C25 C36 1.377(7) . ? C26 C40 1.369(6) . ? C27 C40 1.417(5) . ? C29 C31 1.510(5) . ? C30 C32 1.366(6) . ? C32 C44 1.409(6) . ? C33 C49 1.390(5) . ? C34 C48 1.374(6) . ? C35 C45 1.378(5) . ? C35 C36 1.415(7) . ? C37 C44 1.382(5) . ? C42 C48 1.412(6) . ? C47 C49 1.400(6) . ? 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 Cl12 C101 Cl13 110.8(2) . . ? Cl12 C101 Cl11 110.2(3) . . ? Cl13 C101 Cl11 112.0(2) . . ? C201 C201 Cl23 86.5(5) 4_675 . ? C201 C201 Cl21 117.8(12) 4_675 . ? Cl23 C201 Cl21 137.0(8) . . ? C201 C201 Cl22 83.4(10) 4_675 . ? Cl23 C201 Cl22 105.5(6) . . ? Cl21 C201 Cl22 111.8(6) . . ? C201 C201 Cl23 57.3(5) 4_675 4_675 ? Cl23 C201 Cl23 39.0(4) . 4_675 ? Cl21 C201 Cl23 124.6(7) . 4_675 ? Cl22 C201 Cl23 121.0(6) . 4_675 ? C201 C201 Cl22 63.1(10) 4_675 4_675 ? Cl23 C201 Cl22 126.0(7) . 4_675 ? Cl21 C201 Cl22 55.3(4) . 4_675 ? Cl22 C201 Cl22 113.3(6) . 4_675 ? Cl23 C201 Cl22 87.9(5) 4_675 4_675 ? C201 Cl21 Cl22 69.9(5) . 4_675 ? Cl21 Cl22 C201 87.8(4) 4_675 . ? Cl21 Cl22 C201 54.7(4) 4_675 4_675 ? C201 Cl22 C201 33.4(7) . 4_675 ? Cl23 Cl23 C201 84.0(5) 4_675 . ? Cl23 Cl23 C201 56.9(4) 4_675 4_675 ? C201 Cl23 C201 36.2(8) . 4_675 ? Cl32 C301 Cl33 109.3(4) . . ? Cl32 C301 Cl31 110.1(3) . . ? Cl33 C301 Cl31 108.4(3) . . ? Cl43 C401 Cl42 115.4(9) . . ? Cl43 C401 Cl41 113.0(9) . . ? Cl42 C401 Cl41 117.9(9) . . ? O57 S1 O8 119.33(16) . . ? O57 S1 N53 109.79(17) . . ? O8 S1 N53 104.65(15) . . ? O57 S1 C22 107.18(16) . . ? O8 S1 C22 108.33(17) . . ? N53 S1 C22 106.96(16) . . ? O10 S2 O56 120.69(18) . . ? O10 S2 N55 104.82(16) . . ? O56 S2 N55 109.64(17) . . ? O10 S2 C12 107.74(17) . . ? O56 S2 C12 106.86(16) . . ? N55 S2 C12 106.28(17) . . ? C27 O7 C29 117.9(3) . . ? C4 O58 C28 118.6(3) . . ? C9 N5 C15 127.4(3) . . ? C17 N53 S1 126.1(2) . . ? C31 N54 C19 126.9(3) . . ? C13 N55 S2 127.8(2) . . ? C7 C4 O58 117.2(3) . . ? C7 C4 C16 121.9(3) . . ? O58 C4 C16 120.9(3) . . ? C18 C6 C7 119.9(3) . . ? C18 C6 C37 118.5(3) . . ? C7 C6 C37 121.6(3) . . ? C4 C7 C6 118.7(3) . . ? C4 C7 C10 119.9(3) . . ? C6 C7 C10 121.4(3) . . ? C17 C8 C15 118.5(3) . . ? O59 C9 N5 125.1(3) . . ? O59 C9 C28 120.0(3) . . ? N5 C9 C28 114.9(3) . . ? C27 C10 C11 119.1(3) . . ? C27 C10 C7 120.9(3) . . ? C11 C10 C7 120.0(3) . . ? C20 C11 C45 119.1(3) . . ? C20 C11 C10 119.4(3) . . ? C45 C11 C10 121.5(3) . . ? C24 C12 C47 121.7(3) . . ? C24 C12 S2 119.8(3) . . ? C47 C12 S2 118.4(3) . . ? C14 C13 C23 120.9(3) . . ? C14 C13 N55 115.8(3) . . ? C23 C13 N55 123.3(3) . . ? C13 C14 C19 118.9(3) . . ? C8 C15 C34 120.7(3) . . ? C8 C15 N5 121.5(3) . . ? C34 C15 N5 117.8(3) . . ? C38 C16 C4 119.7(3) . . ? C42 C17 C8 121.2(3) . . ? C42 C17 N53 123.5(3) . . ? C8 C17 N53 115.3(3) . . ? C30 C18 C6 119.3(3) . . ? C30 C18 C38 122.1(3) . . ? C6 C18 C38 118.7(3) . . ? C14 C19 C41 120.5(3) . . ? C14 C19 N54 122.0(3) . . ? C41 C19 N54 117.4(3) . . ? C26 C20 C11 118.9(4) . . ? C26 C20 C25 121.6(4) . . ? C11 C20 C25 119.5(4) . . ? C23 C21 C41 121.8(3) . . ? C33 C22 C24 121.9(3) . . ? C33 C22 S1 119.6(3) . . ? C24 C22 S1 118.5(3) . . ? C21 C23 C13 118.7(4) . . ? C22 C24 C12 118.2(3) . . ? C36 C25 C20 120.2(4) . . ? C40 C26 C20 122.0(4) . . ? C10 C27 O7 115.5(3) . . ? C10 C27 C40 121.5(3) . . ? O7 C27 C40 123.0(3) . . ? O58 C28 C9 109.6(3) . . ? O7 C29 C31 114.3(3) . . ? C32 C30 C18 121.3(4) . . ? O9 C31 N54 124.9(4) . . ? O9 C31 C29 118.8(3) . . ? N54 C31 C29 116.3(3) . . ? C30 C32 C44 119.8(4) . . ? C22 C33 C49 119.0(4) . . ? C48 C34 C15 120.1(4) . . ? C45 C35 C36 121.1(4) . . ? C25 C36 C35 120.0(4) . . ? C44 C37 C6 120.1(4) . . ? C16 C38 C18 120.8(3) . . ? C26 C40 C27 119.1(3) . . ? C21 C41 C19 119.1(3) . . ? C17 C42 C48 119.4(4) . . ? C37 C44 C32 121.0(4) . . ? C35 C45 C11 120.1(4) . . ? C12 C47 C49 118.2(3) . . ? C34 C48 C42 120.1(4) . . ? C33 C49 C47 120.9(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.134 _refine_diff_density_min -0.577 _refine_diff_density_rms 0.076