Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 1145 loop_ _publ_author_name 'Howard Colquhoun' 'Fabio Arico' 'Abderrazak Ben-Haida' 'P. Hodge' 'Lionel G. Sestiaa' 'D. Williams' 'Zhixue Zhu' 'Mikhail G. Zolotukhin' _publ_contact_author_name 'Prof Howard Colquhoun' _publ_contact_author_address ; School of Chemistry The University of Reading Whiteknights Reading RG6 6AD U.K. ; _publ_contact_author_email H.M.COLQUHOUN@RDG.AC.UK _publ_requested_journal 'Journal of Materials Chemistry' _publ_section_title ; Microfabrication of high-performance aromatic polymers as nanotubes or fibrils by in situ ring-opening polymerisation of macrocyclic precursors ; data_macrocycle_3 _database_code_CSD 208055 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C80 H48 O12 . 2(CH2Cl2)' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C82 H52 Cl4 O12' _chemical_formula_weight 1371.04 _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' O O 0.0492 0.0322 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6992(9) _cell_length_b 12.5318(14) _cell_length_c 14.6417(15) _cell_angle_alpha 77.935(7) _cell_angle_beta 88.098(9) _cell_angle_gamma 71.147(8) _cell_volume 1645.9(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 10.80 _cell_measurement_theta_max 24.96 _exptl_crystal_description plates _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.63 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.383 _exptl_crystal_density_method ? _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 2.188 _exptl_absorpt_correction_type 'empirical (lamina 0 0 1)' _exptl_absorpt_correction_T_min 0.4378 _exptl_absorpt_correction_T_max 0.9114 _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 5058 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 61.98 _reflns_number_total 4731 _reflns_number_observed 3852 _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 254 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^)+(0.0823P)^2^+0.6570P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0013(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4477 _refine_ls_number_parameters 447 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0644 _refine_ls_R_factor_obs 0.0509 _refine_ls_wR_factor_all 0.1492 _refine_ls_wR_factor_obs 0.1347 _refine_ls_goodness_of_fit_all 1.037 _refine_ls_goodness_of_fit_obs 1.063 _refine_ls_restrained_S_all 1.056 _refine_ls_restrained_S_obs 1.067 _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 O1 O -0.3946(2) 1.2456(2) 0.7188(2) 0.0540(6) Uani 1 d . . C2 C -0.3749(3) 1.1820(2) 0.8093(2) 0.0401(6) Uani 1 d . . C3 C -0.4407(3) 1.2279(3) 0.8836(2) 0.0476(7) Uani 1 d . . H3A H -0.5076 1.3020 0.8733 0.057 Uiso 1 calc R . C4 C -0.4066(3) 1.1632(2) 0.9734(2) 0.0465(7) Uani 1 d . . H4A H -0.4517 1.1938 1.0236 0.056 Uiso 1 calc R . C5 C -0.3059(3) 1.0531(2) 0.9897(2) 0.0394(6) Uani 1 d . . C6 C -0.2411(3) 1.0088(2) 0.9136(2) 0.0449(7) Uani 1 d . . H6A H -0.1735 0.9350 0.9237 0.054 Uiso 1 calc R . C7 C -0.2749(3) 1.0721(2) 0.8236(2) 0.0468(7) Uani 1 d . . H7A H -0.2313 1.0413 0.7732 0.056 Uiso 1 calc R . C8 C -0.2633(3) 0.9899(2) 1.0878(2) 0.0445(6) Uani 1 d . . O8 O -0.3015(3) 1.0382(2) 1.1529(2) 0.0691(7) Uani 1 d . . C9 C -0.1704(3) 0.8663(2) 1.1079(2) 0.0405(6) Uani 1 d . . C10 C -0.0494(4) 0.8296(3) 1.1686(2) 0.0522(7) Uani 1 d . . H10A H -0.0236 0.8829 1.1940 0.063 Uiso 1 calc R . C11 C 0.0326(4) 0.7143(3) 1.1914(2) 0.0589(8) Uani 1 d . . H11A H 0.1165 0.6908 1.2295 0.071 Uiso 1 calc R . C12 C -0.0088(4) 0.6342(3) 1.1583(2) 0.0505(7) Uani 1 d . . H12A H 0.0441 0.5562 1.1766 0.061 Uiso 1 calc R . C13 C -0.1296(3) 0.6690(2) 1.0976(2) 0.0414(6) Uani 1 d . . C14 C -0.2082(3) 0.7859(2) 1.0708(2) 0.0382(6) Uani 1 d . . H14A H -0.2863 0.8102 1.0279 0.046 Uiso 1 calc R . C15 C -0.1805(4) 0.5815(2) 1.0678(2) 0.0512(7) Uani 1 d . . O15 O -0.1742(5) 0.4932(2) 1.1239(2) 0.1004(13) Uani 1 d . . C16 C -0.2418(3) 0.6030(2) 0.9710(2) 0.0409(6) Uani 1 d . . C17 C -0.3309(4) 0.5411(3) 0.9536(2) 0.0494(7) Uani 1 d . . H17A H -0.3525 0.4887 1.0023 0.059 Uiso 1 calc R . C18 C -0.3871(4) 0.5571(3) 0.8646(2) 0.0520(7) Uani 1 d . . H18A H -0.4476 0.5166 0.8532 0.062 Uiso 1 calc R . C19 C -0.3530(3) 0.6336(2) 0.7926(2) 0.0407(6) Uani 1 d . . C20 C -0.2645(3) 0.6952(2) 0.8079(2) 0.0444(6) Uani 1 d . . H20A H -0.2423 0.7467 0.7588 0.053 Uiso 1 calc R . C21 C -0.2092(3) 0.6792(2) 0.8973(2) 0.0411(6) Uani 1 d . . H21A H -0.1490 0.7202 0.9081 0.049 Uiso 1 calc R . O22 O -0.4023(3) 0.6389(2) 0.70339(15) 0.0526(6) Uani 1 d . . C23 C -0.4802(3) 0.7427(2) 0.6481(2) 0.0384(6) Uani 1 d . . C24 C -0.4934(3) 0.7424(2) 0.5538(2) 0.0468(7) Uani 1 d . . H24A H -0.4448 0.6765 0.5313 0.056 Uiso 1 calc R . C25 C -0.5780(3) 0.8395(3) 0.4946(2) 0.0460(7) Uani 1 d . . H25A H -0.5852 0.8398 0.4314 0.055 Uiso 1 calc R . C26 C -0.6540(3) 0.9385(2) 0.5279(2) 0.0395(6) Uani 1 d . . C27 C -0.6376(3) 0.9375(2) 0.6218(2) 0.0414(6) Uani 1 d . . H27A H -0.6859 1.0034 0.6444 0.050 Uiso 1 calc R . C28 C -0.5506(3) 0.8404(2) 0.6824(2) 0.0407(6) Uani 1 d . . H28A H -0.5397 0.8409 0.7451 0.049 Uiso 1 calc R . C29 C -0.7451(3) 1.0406(3) 0.4601(2) 0.0451(7) Uani 1 d . . O29 O -0.7226(3) 1.0517(2) 0.37649(15) 0.0626(6) Uani 1 d . . C30 C -0.8683(3) 1.1309(2) 0.4930(2) 0.0403(6) Uani 1 d . . C31 C -0.9587(3) 1.1029(3) 0.5626(2) 0.0464(7) Uani 1 d . . H31A H -0.9382 1.0270 0.5952 0.056 Uiso 1 calc R . C32 C -1.0802(3) 1.1888(3) 0.5835(2) 0.0491(7) Uani 1 d . . H32A H -1.1407 1.1703 0.6304 0.059 Uiso 1 calc R . C33 C -1.1117(3) 1.3014(3) 0.5350(2) 0.0477(7) Uani 1 d . . H33A H -1.1934 1.3583 0.5492 0.057 Uiso 1 calc R . C34 C -1.0221(3) 1.3302(2) 0.4651(2) 0.0409(6) Uani 1 d . . C35 C -0.8999(3) 1.2443(2) 0.4452(2) 0.0422(6) Uani 1 d . . H35A H -0.8384 1.2632 0.3991 0.051 Uiso 1 calc R . C36 C -1.0457(3) 1.4503(2) 0.4102(2) 0.0452(7) Uani 1 d . . O36 O -0.9415(3) 1.4832(2) 0.3889(2) 0.0624(6) Uani 1 d . . C37 C -1.1966(3) 1.5280(2) 0.3792(2) 0.0425(6) Uani 1 d . . C38 C -1.3124(3) 1.4877(2) 0.3721(2) 0.0494(7) Uani 1 d . . H38A H -1.2987 1.4091 0.3903 0.059 Uiso 1 calc R . C39 C -1.4486(4) 1.5632(3) 0.3382(2) 0.0506(7) Uani 1 d . . H39A H -1.5268 1.5364 0.3346 0.061 Uiso 1 calc R . C40 C -1.4653(3) 1.6788(2) 0.3099(2) 0.0436(6) Uani 1 d . . C41 C -1.3527(3) 1.7206(2) 0.3154(2) 0.0485(7) Uani 1 d . . H41A H -1.3666 1.7990 0.2954 0.058 Uiso 1 calc R . C42 C -1.2181(3) 1.6457(2) 0.3508(2) 0.0455(6) Uani 1 d . . H42A H -1.1415 1.6738 0.3557 0.055 Uiso 1 calc R . C44 C 0.1788(4) 0.7595(3) 0.8269(3) 0.0646(9) Uani 1 d D . H44A H 0.2186 0.6795 0.8214 0.077 Uiso 1 d R . H44B H 0.2551 0.7942 0.8127 0.077 Uiso 1 d R . Cl1 Cl 0.12523(11) 0.76442(10) 0.94089(7) 0.0761(3) Uani 1 d D . Cl2 Cl 0.0271(2) 0.83419(15) 0.74709(10) 0.0798(4) Uani 0.83 d PD . Cl2' Cl 0.0775(10) 0.7914(8) 0.7308(7) 0.090(3) Uiso 0.17 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 O1 0.0453(11) 0.0504(12) 0.0468(11) 0.0035(9) 0.0019(9) 0.0024(9) C2 0.0352(14) 0.0370(14) 0.0423(14) -0.0034(11) -0.0014(11) -0.0065(11) C3 0.042(2) 0.0389(14) 0.055(2) -0.0123(13) -0.0031(13) -0.0022(12) C4 0.047(2) 0.044(2) 0.0463(15) -0.0176(13) 0.0005(13) -0.0061(12) C5 0.0434(15) 0.0366(14) 0.0398(14) -0.0113(11) 0.0002(11) -0.0131(11) C6 0.050(2) 0.0326(13) 0.0445(15) -0.0062(12) 0.0033(12) -0.0038(12) C7 0.055(2) 0.0377(14) 0.0404(14) -0.0066(12) 0.0049(13) -0.0070(13) C8 0.055(2) 0.0409(15) 0.0412(14) -0.0131(12) 0.0012(13) -0.0179(13) O8 0.108(2) 0.0541(13) 0.0432(12) -0.0204(11) 0.0068(12) -0.0171(13) C9 0.050(2) 0.0420(14) 0.0324(12) -0.0071(11) 0.0007(11) -0.0195(12) C10 0.058(2) 0.061(2) 0.0429(15) -0.0110(14) -0.0093(14) -0.024(2) C11 0.051(2) 0.068(2) 0.052(2) -0.007(2) -0.0185(15) -0.013(2) C12 0.055(2) 0.047(2) 0.0380(14) -0.0011(13) -0.0068(13) -0.0044(13) C13 0.050(2) 0.0399(14) 0.0299(12) -0.0036(11) -0.0033(11) -0.0109(12) C14 0.0443(15) 0.0393(14) 0.0303(12) -0.0038(11) -0.0039(11) -0.0141(11) C15 0.074(2) 0.0350(15) 0.0396(15) -0.0016(12) -0.0084(14) -0.0135(14) O15 0.198(4) 0.056(2) 0.0553(15) 0.0152(13) -0.040(2) -0.064(2) C16 0.048(2) 0.0333(13) 0.0380(14) -0.0045(11) -0.0049(12) -0.0098(11) C17 0.065(2) 0.0425(15) 0.0439(15) -0.0029(12) -0.0009(14) -0.0259(14) C18 0.057(2) 0.042(2) 0.060(2) -0.0052(14) -0.0107(15) -0.0222(14) C19 0.0441(15) 0.0328(13) 0.0398(14) -0.0076(11) -0.0114(12) -0.0038(11) C20 0.055(2) 0.0440(15) 0.0359(13) -0.0051(12) 0.0012(12) -0.0208(13) C21 0.0438(15) 0.0422(14) 0.0413(14) -0.0109(12) -0.0013(12) -0.0175(12) O22 0.0710(14) 0.0359(10) 0.0460(11) -0.0096(9) -0.0195(10) -0.0077(9) C23 0.0392(14) 0.0362(13) 0.0395(14) -0.0094(11) -0.0071(11) -0.0099(11) C24 0.055(2) 0.0409(15) 0.0419(15) -0.0186(12) -0.0053(13) -0.0045(13) C25 0.049(2) 0.050(2) 0.0352(13) -0.0144(12) -0.0033(12) -0.0066(13) C26 0.0393(14) 0.0388(14) 0.0364(13) -0.0086(11) -0.0001(11) -0.0066(11) C27 0.0428(15) 0.0394(14) 0.0397(14) -0.0148(12) -0.0013(11) -0.0057(11) C28 0.0441(15) 0.0446(15) 0.0328(12) -0.0126(11) 0.0010(11) -0.0106(12) C29 0.046(2) 0.046(2) 0.0387(15) -0.0087(12) 0.0020(12) -0.0081(13) O29 0.072(2) 0.0587(13) 0.0367(11) -0.0069(10) 0.0029(10) 0.0038(11) C30 0.0391(14) 0.0404(14) 0.0361(13) -0.0064(11) -0.0039(11) -0.0060(11) C31 0.046(2) 0.0429(15) 0.0431(14) 0.0000(12) -0.0034(12) -0.0104(12) C32 0.041(2) 0.055(2) 0.0434(15) -0.0008(13) 0.0050(12) -0.0123(13) C33 0.0385(14) 0.052(2) 0.0451(15) -0.0082(13) -0.0024(12) -0.0047(12) C34 0.0409(14) 0.0396(14) 0.0361(13) -0.0041(11) -0.0056(11) -0.0066(11) C35 0.0412(15) 0.046(2) 0.0346(13) -0.0045(11) -0.0011(11) -0.0091(12) C36 0.045(2) 0.0423(15) 0.0446(15) -0.0073(13) -0.0052(12) -0.0100(13) O36 0.0495(13) 0.0536(13) 0.075(2) 0.0037(11) -0.0019(11) -0.0153(10) C37 0.046(2) 0.0375(14) 0.0388(13) -0.0054(11) -0.0060(12) -0.0075(12) C38 0.054(2) 0.0322(13) 0.058(2) -0.0051(13) -0.0134(14) -0.0099(12) C39 0.049(2) 0.043(2) 0.058(2) -0.0068(13) -0.0121(14) -0.0133(13) C40 0.044(2) 0.0391(14) 0.0384(13) -0.0042(11) -0.0025(12) -0.0028(12) C41 0.056(2) 0.0313(13) 0.051(2) -0.0034(12) 0.0005(14) -0.0077(12) C42 0.049(2) 0.0412(15) 0.0442(15) -0.0082(12) 0.0007(13) -0.0125(12) C44 0.067(2) 0.056(2) 0.070(2) -0.007(2) 0.009(2) -0.025(2) Cl1 0.0704(6) 0.0946(7) 0.0693(6) -0.0148(5) 0.0000(4) -0.0363(5) Cl2 0.0854(9) 0.0829(9) 0.0626(7) 0.0041(7) -0.0095(7) -0.0265(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C2 1.381(3) . ? O1 C40 1.400(3) 2_386 ? C2 C3 1.378(4) . ? C2 C7 1.383(4) . ? C3 C4 1.381(4) . ? C4 C5 1.387(4) . ? C5 C6 1.389(4) . ? C5 C8 1.488(4) . ? C6 C7 1.378(4) . ? C8 O8 1.218(4) . ? C8 C9 1.491(4) . ? C9 C14 1.387(4) . ? C9 C10 1.388(4) . ? C10 C11 1.381(5) . ? C11 C12 1.372(5) . ? C12 C13 1.388(4) . ? C13 C14 1.393(4) . ? C13 C15 1.484(4) . ? C15 O15 1.218(4) . ? C15 C16 1.492(4) . ? C16 C21 1.385(4) . ? C16 C17 1.394(4) . ? C17 C18 1.380(4) . ? C18 C19 1.378(4) . ? C19 C20 1.376(4) . ? C19 O22 1.388(3) . ? C20 C21 1.381(4) . ? O22 C23 1.373(3) . ? C23 C28 1.382(4) . ? C23 C24 1.391(4) . ? C24 C25 1.366(4) . ? C25 C26 1.399(4) . ? C26 C27 1.387(4) . ? C26 C29 1.483(4) . ? C27 C28 1.384(4) . ? C29 O29 1.224(4) . ? C29 C30 1.501(4) . ? C30 C35 1.386(4) . ? C30 C31 1.386(4) . ? C31 C32 1.392(4) . ? C32 C33 1.381(4) . ? C33 C34 1.386(4) . ? C34 C35 1.390(4) . ? C34 C36 1.500(4) . ? C36 O36 1.218(4) . ? C36 C37 1.494(4) . ? C37 C38 1.388(4) . ? C37 C42 1.394(4) . ? C38 C39 1.388(4) . ? C39 C40 1.378(4) . ? C40 C41 1.367(5) . ? C40 O1 1.400(3) 2_386 ? C41 C42 1.380(4) . ? C44 Cl2' 1.645(10) . ? C44 Cl1 1.740(4) . ? C44 Cl2 1.781(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 O1 C40 117.5(2) . 2_386 ? C3 C2 O1 122.4(2) . . ? C3 C2 C7 120.8(3) . . ? O1 C2 C7 116.5(3) . . ? C2 C3 C4 119.6(3) . . ? C3 C4 C5 120.7(3) . . ? C4 C5 C6 118.5(3) . . ? C4 C5 C8 119.0(3) . . ? C6 C5 C8 122.3(3) . . ? C7 C6 C5 121.4(3) . . ? C6 C7 C2 118.9(3) . . ? O8 C8 C5 120.9(3) . . ? O8 C8 C9 118.8(3) . . ? C5 C8 C9 120.2(2) . . ? C14 C9 C10 119.4(3) . . ? C14 C9 C8 120.6(3) . . ? C10 C9 C8 119.9(3) . . ? C11 C10 C9 120.2(3) . . ? C12 C11 C10 120.4(3) . . ? C11 C12 C13 120.3(3) . . ? C12 C13 C14 119.4(3) . . ? C12 C13 C15 119.9(3) . . ? C14 C13 C15 120.5(3) . . ? C9 C14 C13 120.2(3) . . ? O15 C15 C13 119.1(3) . . ? O15 C15 C16 120.6(3) . . ? C13 C15 C16 120.3(2) . . ? C21 C16 C17 118.9(3) . . ? C21 C16 C15 122.4(3) . . ? C17 C16 C15 118.7(3) . . ? C18 C17 C16 120.3(3) . . ? C19 C18 C17 119.5(3) . . ? C20 C19 C18 121.3(3) . . ? C20 C19 O22 121.6(3) . . ? C18 C19 O22 116.9(3) . . ? C19 C20 C21 118.9(3) . . ? C20 C21 C16 121.1(3) . . ? C23 O22 C19 120.5(2) . . ? O22 C23 C28 123.6(2) . . ? O22 C23 C24 115.4(2) . . ? C28 C23 C24 120.8(3) . . ? C25 C24 C23 119.6(3) . . ? C24 C25 C26 120.9(3) . . ? C27 C26 C25 118.6(3) . . ? C27 C26 C29 123.2(2) . . ? C25 C26 C29 118.2(2) . . ? C28 C27 C26 121.2(2) . . ? C23 C28 C27 118.9(2) . . ? O29 C29 C26 120.5(3) . . ? O29 C29 C30 119.0(3) . . ? C26 C29 C30 120.5(2) . . ? C35 C30 C31 119.6(3) . . ? C35 C30 C29 118.0(3) . . ? C31 C30 C29 122.1(3) . . ? C30 C31 C32 119.6(3) . . ? C33 C32 C31 120.5(3) . . ? C32 C33 C34 120.3(3) . . ? C33 C34 C35 119.1(3) . . ? C33 C34 C36 124.0(3) . . ? C35 C34 C36 116.9(3) . . ? C30 C35 C34 121.0(3) . . ? O36 C36 C37 120.2(3) . . ? O36 C36 C34 119.8(3) . . ? C37 C36 C34 119.9(3) . . ? C38 C37 C42 119.1(3) . . ? C38 C37 C36 123.1(3) . . ? C42 C37 C36 117.6(3) . . ? C37 C38 C39 120.7(3) . . ? C40 C39 C38 118.4(3) . . ? C41 C40 C39 122.0(3) . . ? C41 C40 O1 120.3(3) . 2_386 ? C39 C40 O1 117.6(3) . 2_386 ? C40 C41 C42 119.5(3) . . ? C41 C42 C37 120.2(3) . . ? Cl2' C44 Cl1 129.2(4) . . ? Cl1 C44 Cl2 110.1(2) . . ? _refine_diff_density_max 0.232 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.046