data_publication_text _ccdc_journal_manuscript_code 'Cryst. growth & Des.' _publ_contact_author_name 'J N Moorthy' _publ_contact_author_address ;Department of Chemistry IIT Kanpur Kanpur INDIA ; _publ_contact_author_email moorthy@iitk.ac.in loop_ _publ_author_name _publ_author_address 'J N Moorthy' ;Department of Chemistry IIT Kanpur Kanpur INDIA ; 'Govardhan, Savitha' ;Department of Chemistry IIT Kanpur Kanpur INDIA ; 'Bajpai, Alankriti' ;Department of Chemistry IIT Kanpur Kanpur INDIA ; 'Ishita, Neogi' ;Department of Chemistry IIT Kanpur Kanpur INDIA ; data_TB-G7 _publ_section_title '' _publ_section_abstract '' _publ_section_references '' _publ_requested_journal 'Cryst.Growth Des.' _publ_contact_author_name 'J N Moorthy' _publ_contact_author_address ;Department of Chemistry IIT Kanur Kanpur 208016 INDIA ; _publ_contact_author_email moorthy@iitk.ac.in loop_ _publ_author_name _publ_author_address 'J N Moorthy' ;Department of Chemistry IIT Kanpur Kanpur 208016 INDIA ; _audit_creation_method SHELXL-2014 _chemical_name_systematic 3,3,5,5-Tetrakis(2,6-dimethyl-4-methoxyphenyl)biphenyl-cyclododecene _chemical_name_common TB _chemical_melting_point ? _chemical_formula_moiety 'C48 H50 O4, C12 H24' _chemical_formula_sum 'C60 H74 O4' _chemical_formula_weight 859.19 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 2/c' _space_group_name_Hall '-C 2yc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.348(6) _cell_length_b 11.778(2) _cell_length_c 30.986(5) _cell_angle_alpha 90 _cell_angle_beta 101.909(6) _cell_angle_gamma 90 _cell_volume 10123(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description square _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.128 _exptl_crystal_F_000 3728 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_absorpt_coefficient_mu 0.068 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 31351 _diffrn_reflns_av_unetI/netI 0.0963 _diffrn_reflns_av_R_equivalents 0.0743 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.774 _diffrn_reflns_theta_max 28.361 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.923 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.923 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.923 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 11700 _reflns_number_gt 5974 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SHELX-97 _computing_structure_refinement 'SHELXL-2014/5 (Sheldrick, 2014)' _computing_molecular_graphics 'Ortep for Windows (Farrugia, 2012)' _computing_publication_material 'WinGX publication routines (Farrugia, 2012)' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 11700 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1959 _refine_ls_R_factor_gt 0.1189 _refine_ls_wR_factor_ref 0.3945 _refine_ls_wR_factor_gt 0.3251 _refine_ls_goodness_of_fit_ref 1.201 _refine_ls_restrained_S_all 1.201 _refine_ls_shift/su_max 0.000 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.48724(11) 0.1900(3) 0.10706(10) 0.0457(8) Uani 1 1 d . . . . . O2 O 0.50221(11) 0.7608(3) 0.45554(9) 0.0444(8) Uani 1 1 d . . . . . O3 O 0.11466(12) 0.3989(3) 0.42628(10) 0.0506(8) Uani 1 1 d . . . . . O4 O 0.08350(11) 0.5626(3) 0.03301(9) 0.0439(8) Uani 1 1 d . . . . . C1 C 0.50055(16) 0.0731(4) 0.11227(15) 0.0444(11) Uani 1 1 d . . . . . H1A H 0.5161 0.0505 0.0889 0.067 Uiso 1 1 calc R U . . . H1B H 0.4722 0.0277 0.1112 0.067 Uiso 1 1 calc R U . . . H1C H 0.5222 0.0624 0.1402 0.067 Uiso 1 1 calc R U . . . C2 C 0.46817(14) 0.2392(3) 0.14047(13) 0.0348(9) Uani 1 1 d . . . . . C3 C 0.45999(15) 0.3553(4) 0.13617(14) 0.0423(10) Uani 1 1 d . . . . . H3 H 0.4680 0.3943 0.1126 0.051 Uiso 1 1 calc R U . . . C4 C 0.43994(15) 0.4132(4) 0.16694(14) 0.0384(10) Uani 1 1 d . . . . . C5 C 0.42832(13) 0.3543(3) 0.20285(13) 0.0321(9) Uani 1 1 d . . . . . C6 C 0.43722(14) 0.2380(3) 0.20738(13) 0.0336(9) Uani 1 1 d . . . . . C7 C 0.45672(14) 0.1810(3) 0.17565(13) 0.0365(9) Uani 1 1 d . . . . . H7 H 0.4621 0.1031 0.1782 0.044 Uiso 1 1 calc R U . . . C8 C 0.42671(16) 0.1727(4) 0.24580(15) 0.0449(11) Uani 1 1 d . . . . . H8A H 0.4351 0.0944 0.2432 0.067 Uiso 1 1 calc R U . . . H8B H 0.3930 0.1785 0.2461 0.067 Uiso 1 1 calc R U . . . H8C H 0.4453 0.2034 0.2727 0.067 Uiso 1 1 calc R U . . . C9 C 0.43088(18) 0.5395(4) 0.16179(18) 0.0553(13) Uani 1 1 d . . . . . H9A H 0.3971 0.5544 0.1593 0.083 Uiso 1 1 calc R U . . . H9B H 0.4408 0.5658 0.1357 0.083 Uiso 1 1 calc R U . . . H9C H 0.4490 0.5785 0.1871 0.083 Uiso 1 1 calc R U . . . C10 C 0.40438(14) 0.4155(3) 0.23497(13) 0.0331(9) Uani 1 1 d . . . . . C11 C 0.43157(14) 0.4691(3) 0.27229(13) 0.0348(9) Uani 1 1 d . . . . . H11 H 0.4650 0.4691 0.2768 0.042 Uiso 1 1 calc R U . . . C12 C 0.40877(13) 0.5232(3) 0.30322(13) 0.0308(9) Uani 1 1 d . . . . . C13 C 0.35839(13) 0.5211(3) 0.29540(12) 0.0308(9) Uani 1 1 d . . . . . H13 H 0.3430 0.5559 0.3156 0.037 Uiso 1 1 calc R U . . . C14 C 0.33045(13) 0.4688(3) 0.25847(12) 0.0281(8) Uani 1 1 d . . . . . C15 C 0.35438(14) 0.4165(3) 0.22863(13) 0.0301(8) Uani 1 1 d . . . . . H15 H 0.3363 0.3812 0.2038 0.036 Uiso 1 1 calc R U . . . C16 C 0.43658(13) 0.5816(3) 0.34325(13) 0.0329(9) Uani 1 1 d . . . . . C17 C 0.45383(14) 0.6942(3) 0.34066(13) 0.0351(9) Uani 1 1 d . . . . . C18 C 0.47572(14) 0.7472(3) 0.37901(13) 0.0376(10) Uani 1 1 d . . . . . H18 H 0.4873 0.8206 0.3775 0.045 Uiso 1 1 calc R U . . . C19 C 0.48123(14) 0.6959(3) 0.41980(14) 0.0373(10) Uani 1 1 d . . . . . C20 C 0.46550(15) 0.5854(3) 0.42180(14) 0.0378(10) Uani 1 1 d . . . . . H20 H 0.4699 0.5488 0.4489 0.045 Uiso 1 1 calc R U . . . C21 C 0.44309(14) 0.5281(3) 0.38374(14) 0.0354(9) Uani 1 1 d . . . . . C22 C 0.42550(16) 0.4072(4) 0.38753(15) 0.0466(11) Uani 1 1 d . . . . . H22A H 0.4430 0.3736 0.4143 0.070 Uiso 1 1 calc R U . . . H22B H 0.4307 0.3635 0.3628 0.070 Uiso 1 1 calc R U . . . H22C H 0.3917 0.4082 0.3879 0.070 Uiso 1 1 calc R U . . . C23 C 0.44842(17) 0.7542(4) 0.29731(15) 0.0498(12) Uani 1 1 d . . . . . H23A H 0.4591 0.8313 0.3022 0.075 Uiso 1 1 calc R U . . . H23B H 0.4152 0.7532 0.2825 0.075 Uiso 1 1 calc R U . . . H23C H 0.4675 0.7164 0.2795 0.075 Uiso 1 1 calc R U . . . C24 C 0.5124(2) 0.7064(4) 0.49736(15) 0.0586(14) Uani 1 1 d . . . . . H24A H 0.5270 0.7598 0.5195 0.088 Uiso 1 1 calc R U . . . H24B H 0.5342 0.6443 0.4966 0.088 Uiso 1 1 calc R U . . . H24C H 0.4830 0.6782 0.5042 0.088 Uiso 1 1 calc R U . . . C25 C 0.27728(13) 0.4672(3) 0.25155(12) 0.0269(8) Uani 1 1 d . . . . . C26 C 0.25443(13) 0.4554(3) 0.28694(12) 0.0277(8) Uani 1 1 d . . . . . H26 H 0.2730 0.4499 0.3153 0.033 Uiso 1 1 calc R U . . . C27 C 0.20413(13) 0.4515(3) 0.28078(12) 0.0292(8) Uani 1 1 d . . . . . C28 C 0.17689(14) 0.4635(3) 0.23785(12) 0.0304(9) Uani 1 1 d . . . . . H28 H 0.1434 0.4618 0.2334 0.036 Uiso 1 1 calc R U . . . C29 C 0.19815(13) 0.4777(3) 0.20186(13) 0.0292(8) Uani 1 1 d . . . . . C30 C 0.24858(13) 0.4773(3) 0.20899(12) 0.0282(8) Uani 1 1 d . . . . . H30 H 0.2634 0.4838 0.1850 0.034 Uiso 1 1 calc R U . . . C31 C 0.18011(13) 0.4356(3) 0.31884(12) 0.0318(9) Uani 1 1 d . . . . . C32 C 0.17094(14) 0.5303(3) 0.34383(13) 0.0351(9) Uani 1 1 d . . . . . C33 C 0.14737(15) 0.5140(4) 0.37817(13) 0.0383(10) Uani 1 1 d . . . . . H33 H 0.1394 0.5762 0.3937 0.046 Uiso 1 1 calc R U . . . C34 C 0.13540(14) 0.4041(4) 0.38983(13) 0.0362(9) Uani 1 1 d . . . . . C35 C 0.14490(14) 0.3125(3) 0.36560(13) 0.0348(9) Uani 1 1 d . . . . . H35 H 0.1368 0.2399 0.3733 0.042 Uiso 1 1 calc R U . . . C36 C 0.16658(14) 0.3272(3) 0.32965(13) 0.0336(9) Uani 1 1 d . . . . . C37 C 0.17537(18) 0.2244(4) 0.30370(15) 0.0467(11) Uani 1 1 d . . . . . H37A H 0.1975 0.1745 0.3223 0.070 Uiso 1 1 calc R U . . . H37B H 0.1888 0.2476 0.2791 0.070 Uiso 1 1 calc R U . . . H37C H 0.1454 0.1856 0.2932 0.070 Uiso 1 1 calc R U . . . C38 C 0.18623(17) 0.6483(3) 0.33435(15) 0.0449(11) Uani 1 1 d . . . . . H38A H 0.1639 0.7022 0.3419 0.067 Uiso 1 1 calc R U . . . H38B H 0.1867 0.6549 0.3036 0.067 Uiso 1 1 calc R U . . . H38C H 0.2179 0.6630 0.3515 0.067 Uiso 1 1 calc R U . . . C39 C 0.11248(18) 0.2872(4) 0.44509(16) 0.0513(12) Uani 1 1 d . . . . . H39A H 0.1015 0.2934 0.4723 0.077 Uiso 1 1 calc R U . . . H39B H 0.1440 0.2535 0.4506 0.077 Uiso 1 1 calc R U . . . H39C H 0.0905 0.2406 0.4248 0.077 Uiso 1 1 calc R U . . . C40 C 0.16860(13) 0.4974(3) 0.15691(12) 0.0287(8) Uani 1 1 d . . . . . C41 C 0.15008(14) 0.4039(3) 0.12949(13) 0.0338(9) Uani 1 1 d . . . . . C42 C 0.12167(14) 0.4252(3) 0.08789(13) 0.0353(9) Uani 1 1 d . . . . . H42 H 0.1096 0.3646 0.0697 0.042 Uiso 1 1 calc R U . . . C43 C 0.11116(14) 0.5349(3) 0.07335(12) 0.0329(9) Uani 1 1 d . . . . . C44 C 0.12951(14) 0.6251(3) 0.10019(13) 0.0357(9) Uani 1 1 d . . . . . H44 H 0.1228 0.6988 0.0901 0.043 Uiso 1 1 calc R U . . . C45 C 0.15743(14) 0.6082(3) 0.14140(13) 0.0322(9) Uani 1 1 d . . . . . C46 C 0.17638(18) 0.7092(4) 0.16997(15) 0.0500(12) Uani 1 1 d . . . . . H46A H 0.1703 0.7775 0.1528 0.075 Uiso 1 1 calc R U . . . H46B H 0.2104 0.7007 0.1808 0.075 Uiso 1 1 calc R U . . . H46C H 0.1604 0.7134 0.1944 0.075 Uiso 1 1 calc R U . . . C47 C 0.16215(17) 0.2843(3) 0.14509(14) 0.0456(11) Uani 1 1 d . . . . . H47A H 0.1430 0.2319 0.1251 0.068 Uiso 1 1 calc R U . . . H47B H 0.1554 0.2748 0.1740 0.068 Uiso 1 1 calc R U . . . H47C H 0.1957 0.2700 0.1462 0.068 Uiso 1 1 calc R U . . . C48 C 0.06719(19) 0.4726(4) 0.00247(14) 0.0531(13) Uani 1 1 d . . . . . H48A H 0.0488 0.5038 -0.0244 0.080 Uiso 1 1 calc R U . . . H48B H 0.0473 0.4214 0.0150 0.080 Uiso 1 1 calc R U . . . H48C H 0.0945 0.4323 -0.0037 0.080 Uiso 1 1 calc R U . . . C50 C 0.2408(7) 0.5658(18) -0.0115(5) 0.299(3) Uani 1 1 d . . . . . H50A H 0.2536 0.4901 -0.0137 0.359 Uiso 1 1 calc R U . . . H50B H 0.2093 0.5621 -0.0310 0.359 Uiso 1 1 calc R U . . . C51 C 0.2220(7) 0.5360(17) 0.0252(5) 0.299(3) Uani 1 1 d . . . . . H51A H 0.2004 0.4725 0.0162 0.359 Uiso 1 1 calc R U . . . H51B H 0.2019 0.5991 0.0306 0.359 Uiso 1 1 calc R U . . . C52 C 0.2512(7) 0.5060(18) 0.0673(5) 0.299(3) Uani 1 1 d . . . . . H52A H 0.2727 0.5708 0.0730 0.359 Uiso 1 1 calc R U . . . H52B H 0.2286 0.5172 0.0866 0.359 Uiso 1 1 calc R U . . . C53 C 0.2791(7) 0.4238(19) 0.0885(5) 0.299(3) Uani 1 1 d . . . . . H53A H 0.3032 0.4608 0.1107 0.359 Uiso 1 1 calc R U . . . H53B H 0.2590 0.3800 0.1042 0.359 Uiso 1 1 calc R U . . . C54 C 0.3022(6) 0.3497(18) 0.0686(5) 0.299(3) Uani 1 1 d . . . . . H54A H 0.2980 0.2795 0.0838 0.359 Uiso 1 1 calc R U . . . H54B H 0.2811 0.3424 0.0398 0.359 Uiso 1 1 calc R U . . . C55 C 0.3347(7) 0.340(2) 0.0617(5) 0.299(3) Uani 1 1 d . . . . . H55A H 0.3474 0.2795 0.0822 0.359 Uiso 1 1 calc R U . . . H55B H 0.3506 0.4079 0.0752 0.359 Uiso 1 1 calc R U . . . C56 C 0.3608(6) 0.3206(18) 0.0283(5) 0.299(3) Uani 1 1 d . . . . . H56A H 0.3928 0.3514 0.0395 0.359 Uiso 1 1 calc R U . . . H56B H 0.3647 0.2390 0.0270 0.359 Uiso 1 1 calc R U . . . C57 C 0.3479(6) 0.357(2) -0.0156(5) 0.299(3) Uani 1 1 d . . . . . H57A H 0.3160 0.3247 -0.0254 0.359 Uiso 1 1 calc R U . . . H57B H 0.3687 0.3119 -0.0302 0.359 Uiso 1 1 calc R U . . . C58 C 0.3448(7) 0.4640(19) -0.0386(5) 0.299(3) Uani 1 1 d . . . . . H58A H 0.3480 0.5227 -0.0163 0.359 Uiso 1 1 calc R U . . . H58B H 0.3733 0.4691 -0.0513 0.359 Uiso 1 1 calc R U . . . C59 C 0.3064(7) 0.4944(19) -0.0712(5) 0.299(3) Uani 1 1 d . . . . . H59A H 0.3184 0.4974 -0.0984 0.359 Uiso 1 1 calc R U . . . H59B H 0.2838 0.4317 -0.0744 0.359 Uiso 1 1 calc R U . . . C60 C 0.2806(7) 0.589(2) -0.0701(5) 0.299(3) Uani 1 1 d . . . . . H60A H 0.2573 0.5949 -0.0977 0.359 Uiso 1 1 calc R U . . . H60B H 0.3021 0.6536 -0.0683 0.359 Uiso 1 1 calc R U . . . C61 C 0.2567(7) 0.5959(17) -0.0363(5) 0.299(3) Uani 1 1 d . . . . . H61A H 0.2773 0.6520 -0.0190 0.359 Uiso 1 1 calc R U . . . H61B H 0.2295 0.6401 -0.0517 0.359 Uiso 1 1 calc R U . . . 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 0.0491(18) 0.0480(18) 0.0436(18) -0.0007(14) 0.0182(15) 0.0087(14) O2 0.0500(18) 0.0448(17) 0.0338(17) -0.0072(13) -0.0022(13) -0.0084(14) O3 0.061(2) 0.056(2) 0.0437(19) -0.0035(15) 0.0295(16) -0.0029(16) O4 0.0448(17) 0.0538(18) 0.0277(16) 0.0042(13) -0.0049(13) -0.0008(14) C1 0.039(2) 0.045(2) 0.050(3) -0.013(2) 0.013(2) 0.009(2) C2 0.029(2) 0.038(2) 0.038(2) -0.0046(18) 0.0082(18) 0.0041(17) C3 0.040(2) 0.049(3) 0.043(3) 0.005(2) 0.021(2) 0.002(2) C4 0.032(2) 0.041(2) 0.044(3) -0.0003(19) 0.0125(19) 0.0032(18) C5 0.0257(19) 0.037(2) 0.034(2) -0.0015(17) 0.0051(16) -0.0015(16) C6 0.031(2) 0.034(2) 0.037(2) -0.0004(17) 0.0090(17) 0.0006(17) C7 0.029(2) 0.035(2) 0.044(3) -0.0046(18) 0.0049(18) 0.0011(17) C8 0.048(3) 0.040(2) 0.048(3) 0.003(2) 0.014(2) 0.007(2) C9 0.051(3) 0.041(3) 0.082(4) 0.012(2) 0.035(3) 0.008(2) C10 0.029(2) 0.034(2) 0.037(2) -0.0034(17) 0.0061(17) 0.0009(16) C11 0.0239(19) 0.037(2) 0.041(2) -0.0033(18) 0.0029(17) -0.0033(16) C12 0.028(2) 0.0288(19) 0.034(2) -0.0032(16) 0.0040(16) -0.0017(15) C13 0.0285(19) 0.034(2) 0.030(2) -0.0030(16) 0.0053(16) -0.0013(16) C14 0.0254(19) 0.0305(19) 0.028(2) 0.0029(15) 0.0038(16) -0.0015(15) C15 0.033(2) 0.0280(19) 0.029(2) -0.0018(15) 0.0055(17) -0.0015(16) C16 0.0258(19) 0.034(2) 0.039(2) -0.0028(17) 0.0051(17) 0.0017(16) C17 0.031(2) 0.035(2) 0.037(2) -0.0031(17) 0.0010(17) -0.0029(17) C18 0.040(2) 0.031(2) 0.039(2) -0.0015(18) 0.0014(19) -0.0023(17) C19 0.034(2) 0.038(2) 0.038(2) -0.0071(18) 0.0036(18) -0.0055(18) C20 0.036(2) 0.041(2) 0.033(2) -0.0021(18) -0.0002(18) -0.0078(18) C21 0.030(2) 0.032(2) 0.042(2) -0.0033(18) 0.0014(18) -0.0037(16) C22 0.048(3) 0.038(2) 0.049(3) 0.002(2) -0.001(2) -0.012(2) C23 0.053(3) 0.046(3) 0.045(3) 0.000(2) -0.001(2) -0.015(2) C24 0.070(3) 0.060(3) 0.038(3) -0.005(2) -0.007(2) -0.017(3) C25 0.0249(18) 0.0262(18) 0.028(2) -0.0014(15) 0.0011(15) 0.0012(15) C26 0.0292(19) 0.0293(19) 0.0239(19) -0.0008(15) 0.0040(16) 0.0037(15) C27 0.0287(19) 0.0303(19) 0.028(2) -0.0008(15) 0.0054(16) 0.0007(15) C28 0.0228(18) 0.034(2) 0.034(2) -0.0018(17) 0.0039(16) 0.0029(15) C29 0.0267(19) 0.0289(18) 0.031(2) -0.0023(16) 0.0043(16) -0.0009(15) C30 0.0232(18) 0.0293(19) 0.032(2) -0.0015(16) 0.0046(16) -0.0009(15) C31 0.0268(19) 0.040(2) 0.026(2) -0.0001(17) 0.0003(16) 0.0031(17) C32 0.032(2) 0.036(2) 0.035(2) -0.0020(17) 0.0035(18) 0.0083(17) C33 0.044(2) 0.041(2) 0.031(2) -0.0044(18) 0.0113(19) 0.0062(19) C34 0.034(2) 0.045(2) 0.032(2) -0.0050(18) 0.0116(18) 0.0001(18) C35 0.036(2) 0.035(2) 0.035(2) -0.0002(17) 0.0103(18) -0.0036(17) C36 0.029(2) 0.039(2) 0.035(2) -0.0042(17) 0.0101(17) -0.0034(17) C37 0.055(3) 0.042(2) 0.048(3) -0.008(2) 0.023(2) -0.006(2) C38 0.054(3) 0.037(2) 0.047(3) -0.0024(19) 0.019(2) 0.003(2) C39 0.058(3) 0.060(3) 0.044(3) 0.002(2) 0.029(2) -0.005(2) C40 0.0255(19) 0.036(2) 0.025(2) -0.0029(16) 0.0044(15) 0.0013(16) C41 0.031(2) 0.037(2) 0.032(2) -0.0006(17) 0.0036(17) -0.0044(17) C42 0.034(2) 0.038(2) 0.031(2) -0.0037(17) 0.0011(17) -0.0056(17) C43 0.030(2) 0.043(2) 0.025(2) 0.0030(17) 0.0033(16) -0.0002(17) C44 0.033(2) 0.035(2) 0.036(2) 0.0053(18) 0.0008(17) 0.0085(17) C45 0.034(2) 0.0295(19) 0.032(2) -0.0028(16) 0.0020(17) -0.0001(16) C46 0.057(3) 0.036(2) 0.045(3) -0.003(2) -0.016(2) 0.004(2) C47 0.058(3) 0.034(2) 0.039(3) 0.0046(19) -0.001(2) -0.008(2) C48 0.062(3) 0.063(3) 0.028(2) 0.000(2) -0.004(2) -0.013(2) C50 0.286(7) 0.467(9) 0.183(5) 0.141(5) 0.140(5) 0.166(6) C51 0.286(7) 0.467(9) 0.183(5) 0.141(5) 0.140(5) 0.166(6) C52 0.286(7) 0.467(9) 0.183(5) 0.141(5) 0.140(5) 0.166(6) C53 0.286(7) 0.467(9) 0.183(5) 0.141(5) 0.140(5) 0.166(6) C54 0.286(7) 0.467(9) 0.183(5) 0.141(5) 0.140(5) 0.166(6) C55 0.286(7) 0.467(9) 0.183(5) 0.141(5) 0.140(5) 0.166(6) C56 0.286(7) 0.467(9) 0.183(5) 0.141(5) 0.140(5) 0.166(6) C57 0.286(7) 0.467(9) 0.183(5) 0.141(5) 0.140(5) 0.166(6) C58 0.286(7) 0.467(9) 0.183(5) 0.141(5) 0.140(5) 0.166(6) C59 0.286(7) 0.467(9) 0.183(5) 0.141(5) 0.140(5) 0.166(6) C60 0.286(7) 0.467(9) 0.183(5) 0.141(5) 0.140(5) 0.166(6) C61 0.286(7) 0.467(9) 0.183(5) 0.141(5) 0.140(5) 0.166(6) _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 1.390(5) . ? O1 C1 1.428(5) . ? O2 C19 1.376(5) . ? O2 C24 1.421(6) . ? O3 C34 1.378(5) . ? O3 C39 1.445(5) . ? O4 C43 1.371(5) . ? O4 C48 1.433(5) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C7 1.382(6) . ? C2 C3 1.388(6) . ? C3 C4 1.386(6) . ? C3 H3 0.9300 . ? C4 C5 1.407(6) . ? C4 C9 1.513(6) . ? C5 C6 1.395(5) . ? C5 C10 1.500(5) . ? C6 C7 1.396(5) . ? C6 C8 1.498(6) . ? C7 H7 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C15 1.390(5) . ? C10 C11 1.401(5) . ? C11 C12 1.413(5) . ? C11 H11 0.9300 . ? C12 C13 1.399(5) . ? C12 C16 1.493(5) . ? C13 C14 1.393(5) . ? C13 H13 0.9300 . ? C14 C15 1.398(5) . ? C14 C25 1.478(5) . ? C15 H15 0.9300 . ? C16 C21 1.382(6) . ? C16 C17 1.422(5) . ? C17 C18 1.372(5) . ? C17 C23 1.497(6) . ? C18 C19 1.380(6) . ? C18 H18 0.9300 . ? C19 C20 1.381(5) . ? C20 C21 1.393(6) . ? C20 H20 0.9300 . ? C21 C22 1.521(6) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.391(5) . ? C25 C30 1.404(5) . ? C26 C27 1.400(5) . ? C26 H26 0.9300 . ? C27 C28 1.401(5) . ? C27 C31 1.490(5) . ? C28 C29 1.383(5) . ? C28 H28 0.9300 . ? C29 C30 1.401(5) . ? C29 C40 1.488(5) . ? C30 H30 0.9300 . ? C31 C36 1.393(5) . ? C31 C32 1.413(5) . ? C32 C33 1.382(6) . ? C32 C38 1.502(6) . ? C33 C34 1.404(6) . ? C33 H33 0.9300 . ? C34 C35 1.372(5) . ? C35 C36 1.390(5) . ? C35 H35 0.9300 . ? C36 C37 1.502(5) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C45 1.404(5) . ? C40 C41 1.423(5) . ? C41 C42 1.394(5) . ? C41 C47 1.505(6) . ? C42 C43 1.381(6) . ? C42 H42 0.9300 . ? C43 C44 1.382(6) . ? C44 C45 1.371(5) . ? C44 H44 0.9300 . ? C45 C46 1.513(5) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C50 C61 1.029(16) . ? C50 C51 1.400(15) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.438(19) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C53 1.333(19) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C54 1.32(2) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 C55 0.994(18) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 C56 1.411(16) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 C57 1.399(16) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 C58 1.44(2) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 C59 1.37(2) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 C60 1.34(2) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 C61 1.364(15) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? 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 C1 116.9(3) . . ? C19 O2 C24 117.2(3) . . ? C34 O3 C39 115.6(3) . . ? C43 O4 C48 118.2(3) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C7 C2 C3 120.2(4) . . ? C7 C2 O1 124.8(4) . . ? C3 C2 O1 115.0(4) . . ? C4 C3 C2 120.2(4) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 119.9(4) . . ? C3 C4 C9 119.7(4) . . ? C5 C4 C9 120.4(4) . . ? C6 C5 C4 119.8(4) . . ? C6 C5 C10 120.2(3) . . ? C4 C5 C10 120.0(4) . . ? C5 C6 C7 119.4(4) . . ? C5 C6 C8 121.5(3) . . ? C7 C6 C8 119.1(4) . . ? C2 C7 C6 120.6(4) . . ? C2 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C15 C10 C11 119.0(3) . . ? C15 C10 C5 119.9(3) . . ? C11 C10 C5 121.1(3) . . ? C10 C11 C12 120.8(3) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C13 C12 C11 117.9(3) . . ? C13 C12 C16 119.8(3) . . ? C11 C12 C16 122.3(3) . . ? C14 C13 C12 122.5(4) . . ? C14 C13 H13 118.7 . . ? C12 C13 H13 118.7 . . ? C13 C14 C15 117.8(3) . . ? C13 C14 C25 121.0(3) . . ? C15 C14 C25 121.2(3) . . ? C10 C15 C14 122.0(4) . . ? C10 C15 H15 119.0 . . ? C14 C15 H15 119.0 . . ? C21 C16 C17 119.6(4) . . ? C21 C16 C12 119.5(3) . . ? C17 C16 C12 120.8(4) . . ? C18 C17 C16 118.3(4) . . ? C18 C17 C23 120.5(4) . . ? C16 C17 C23 121.2(4) . . ? C17 C18 C19 122.7(4) . . ? C17 C18 H18 118.7 . . ? C19 C18 H18 118.7 . . ? O2 C19 C18 116.3(4) . . ? O2 C19 C20 125.2(4) . . ? C18 C19 C20 118.5(4) . . ? C19 C20 C21 120.9(4) . . ? C19 C20 H20 119.5 . . ? C21 C20 H20 119.5 . . ? C16 C21 C20 120.0(4) . . ? C16 C21 C22 120.8(4) . . ? C20 C21 C22 119.2(4) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C17 C23 H23A 109.5 . . ? C17 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C17 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O2 C24 H24A 109.5 . . ? O2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C30 118.3(3) . . ? C26 C25 C14 120.9(3) . . ? C30 C25 C14 120.7(3) . . ? C25 C26 C27 121.5(3) . . ? C25 C26 H26 119.2 . . ? C27 C26 H26 119.2 . . ? C26 C27 C28 118.2(3) . . ? C26 C27 C31 121.0(3) . . ? C28 C27 C31 120.8(3) . . ? C29 C28 C27 122.1(3) . . ? C29 C28 H28 118.9 . . ? C27 C28 H28 118.9 . . ? C28 C29 C30 118.2(3) . . ? C28 C29 C40 121.3(3) . . ? C30 C29 C40 120.5(3) . . ? C29 C30 C25 121.5(3) . . ? C29 C30 H30 119.2 . . ? C25 C30 H30 119.2 . . ? C36 C31 C32 120.1(4) . . ? C36 C31 C27 119.9(3) . . ? C32 C31 C27 120.0(4) . . ? C33 C32 C31 119.0(4) . . ? C33 C32 C38 119.0(4) . . ? C31 C32 C38 122.0(4) . . ? C32 C33 C34 120.5(4) . . ? C32 C33 H33 119.7 . . ? C34 C33 H33 119.7 . . ? C35 C34 O3 125.4(4) . . ? C35 C34 C33 119.9(4) . . ? O3 C34 C33 114.7(4) . . ? C34 C35 C36 120.7(4) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? C35 C36 C31 119.7(4) . . ? C35 C36 C37 118.6(4) . . ? C31 C36 C37 121.7(4) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C32 C38 H38A 109.5 . . ? C32 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C32 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O3 C39 H39A 109.5 . . ? O3 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? O3 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C45 C40 C41 119.0(3) . . ? C45 C40 C29 120.6(3) . . ? C41 C40 C29 120.3(3) . . ? C42 C41 C40 119.0(4) . . ? C42 C41 C47 121.0(4) . . ? C40 C41 C47 120.0(4) . . ? C43 C42 C41 121.0(4) . . ? C43 C42 H42 119.5 . . ? C41 C42 H42 119.5 . . ? O4 C43 C42 124.3(4) . . ? O4 C43 C44 116.1(4) . . ? C42 C43 C44 119.6(4) . . ? C45 C44 C43 121.5(4) . . ? C45 C44 H44 119.2 . . ? C43 C44 H44 119.2 . . ? C44 C45 C40 120.0(4) . . ? C44 C45 C46 119.9(4) . . ? C40 C45 C46 120.2(3) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C41 C47 H47A 109.5 . . ? C41 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C41 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? O4 C48 H48A 109.5 . . ? O4 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? O4 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C61 C50 C51 173(3) . . ? C61 C50 H50A 92.2 . . ? C51 C50 H50A 92.2 . . ? C61 C50 H50B 92.2 . . ? C51 C50 H50B 92.2 . . ? H50A C50 H50B 103.0 . . ? C50 C51 C52 123.7(16) . . ? C50 C51 H51A 106.4 . . ? C52 C51 H51A 106.4 . . ? C50 C51 H51B 106.4 . . ? C52 C51 H51B 106.4 . . ? H51A C51 H51B 106.5 . . ? C53 C52 C51 143(2) . . ? C53 C52 H52A 101.3 . . ? C51 C52 H52A 101.3 . . ? C53 C52 H52B 101.3 . . ? C51 C52 H52B 101.3 . . ? H52A C52 H52B 104.5 . . ? C54 C53 C52 123.6(15) . . ? C54 C53 H53A 106.4 . . ? C52 C53 H53A 106.4 . . ? C54 C53 H53B 106.4 . . ? C52 C53 H53B 106.4 . . ? H53A C53 H53B 106.5 . . ? C55 C54 C53 139(3) . . ? C55 C54 H54A 102.5 . . ? C53 C54 H54A 102.5 . . ? C55 C54 H54B 102.5 . . ? C53 C54 H54B 102.5 . . ? H54A C54 H54B 104.9 . . ? C54 C55 C56 146(3) . . ? C54 C55 H55A 100.4 . . ? C56 C55 H55A 100.4 . . ? C54 C55 H55B 100.4 . . ? C56 C55 H55B 100.4 . . ? H55A C55 H55B 104.3 . . ? C57 C56 C55 126.4(15) . . ? C57 C56 H56A 105.7 . . ? C55 C56 H56A 105.7 . . ? C57 C56 H56B 105.7 . . ? C55 C56 H56B 105.7 . . ? H56A C56 H56B 106.2 . . ? C56 C57 C58 136(2) . . ? C56 C57 H57A 103.1 . . ? C58 C57 H57A 103.1 . . ? C56 C57 H57B 103.1 . . ? C58 C57 H57B 103.1 . . ? H57A C57 H57B 105.1 . . ? C59 C58 C57 123(2) . . ? C59 C58 H58A 106.5 . . ? C57 C58 H58A 106.5 . . ? C59 C58 H58B 106.5 . . ? C57 C58 H58B 106.5 . . ? H58A C58 H58B 106.5 . . ? C60 C59 C58 124(2) . . ? C60 C59 H59A 106.4 . . ? C58 C59 H59A 106.4 . . ? C60 C59 H59B 106.4 . . ? C58 C59 H59B 106.4 . . ? H59A C59 H59B 106.5 . . ? C59 C60 C61 115.6(16) . . ? C59 C60 H60A 108.4 . . ? C61 C60 H60A 108.4 . . ? C59 C60 H60B 108.4 . . ? C61 C60 H60B 108.4 . . ? H60A C60 H60B 107.4 . . ? C50 C61 C60 156(2) . . ? C50 C61 H61A 97.3 . . ? C60 C61 H61A 97.3 . . ? C50 C61 H61B 97.3 . . ? C60 C61 H61B 97.3 . . ? H61A C61 H61B 103.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 O1 C2 C7 -6.9(6) . . . . ? C1 O1 C2 C3 174.2(4) . . . . ? C7 C2 C3 C4 -0.5(6) . . . . ? O1 C2 C3 C4 178.4(4) . . . . ? C2 C3 C4 C5 0.7(6) . . . . ? C2 C3 C4 C9 -179.6(4) . . . . ? C3 C4 C5 C6 0.2(6) . . . . ? C9 C4 C5 C6 -179.5(4) . . . . ? C3 C4 C5 C10 -177.0(4) . . . . ? C9 C4 C5 C10 3.3(6) . . . . ? C4 C5 C6 C7 -1.3(6) . . . . ? C10 C5 C6 C7 176.0(3) . . . . ? C4 C5 C6 C8 178.2(4) . . . . ? C10 C5 C6 C8 -4.6(6) . . . . ? C3 C2 C7 C6 -0.5(6) . . . . ? O1 C2 C7 C6 -179.3(4) . . . . ? C5 C6 C7 C2 1.4(6) . . . . ? C8 C6 C7 C2 -178.1(4) . . . . ? C6 C5 C10 C15 -84.6(5) . . . . ? C4 C5 C10 C15 92.6(5) . . . . ? C6 C5 C10 C11 93.3(5) . . . . ? C4 C5 C10 C11 -89.5(5) . . . . ? C15 C10 C11 C12 0.2(6) . . . . ? C5 C10 C11 C12 -177.7(4) . . . . ? C10 C11 C12 C13 0.2(6) . . . . ? C10 C11 C12 C16 -179.7(4) . . . . ? C11 C12 C13 C14 -0.5(6) . . . . ? C16 C12 C13 C14 179.4(4) . . . . ? C12 C13 C14 C15 0.4(6) . . . . ? C12 C13 C14 C25 179.3(3) . . . . ? C11 C10 C15 C14 -0.3(6) . . . . ? C5 C10 C15 C14 177.7(3) . . . . ? C13 C14 C15 C10 0.0(5) . . . . ? C25 C14 C15 C10 -179.0(4) . . . . ? C13 C12 C16 C21 78.1(5) . . . . ? C11 C12 C16 C21 -102.0(5) . . . . ? C13 C12 C16 C17 -98.0(5) . . . . ? C11 C12 C16 C17 81.9(5) . . . . ? C21 C16 C17 C18 -1.3(6) . . . . ? C12 C16 C17 C18 174.8(4) . . . . ? C21 C16 C17 C23 178.7(4) . . . . ? C12 C16 C17 C23 -5.2(6) . . . . ? C16 C17 C18 C19 -0.6(6) . . . . ? C23 C17 C18 C19 179.5(4) . . . . ? C24 O2 C19 C18 -174.1(4) . . . . ? C24 O2 C19 C20 6.0(6) . . . . ? C17 C18 C19 O2 -177.6(4) . . . . ? C17 C18 C19 C20 2.3(6) . . . . ? O2 C19 C20 C21 177.7(4) . . . . ? C18 C19 C20 C21 -2.1(6) . . . . ? C17 C16 C21 C20 1.4(6) . . . . ? C12 C16 C21 C20 -174.7(3) . . . . ? C17 C16 C21 C22 -179.4(4) . . . . ? C12 C16 C21 C22 4.5(6) . . . . ? C19 C20 C21 C16 0.3(6) . . . . ? C19 C20 C21 C22 -178.9(4) . . . . ? C13 C14 C25 C26 -36.8(5) . . . . ? C15 C14 C25 C26 142.2(4) . . . . ? C13 C14 C25 C30 143.4(4) . . . . ? C15 C14 C25 C30 -37.6(5) . . . . ? C30 C25 C26 C27 1.1(5) . . . . ? C14 C25 C26 C27 -178.7(3) . . . . ? C25 C26 C27 C28 -2.0(5) . . . . ? C25 C26 C27 C31 178.3(3) . . . . ? C26 C27 C28 C29 0.6(6) . . . . ? C31 C27 C28 C29 -179.6(3) . . . . ? C27 C28 C29 C30 1.5(5) . . . . ? C27 C28 C29 C40 -176.2(3) . . . . ? C28 C29 C30 C25 -2.5(5) . . . . ? C40 C29 C30 C25 175.2(3) . . . . ? C26 C25 C30 C29 1.2(5) . . . . ? C14 C25 C30 C29 -179.0(3) . . . . ? C26 C27 C31 C36 -94.9(5) . . . . ? C28 C27 C31 C36 85.4(5) . . . . ? C26 C27 C31 C32 85.3(5) . . . . ? C28 C27 C31 C32 -94.4(4) . . . . ? C36 C31 C32 C33 -1.7(6) . . . . ? C27 C31 C32 C33 178.1(4) . . . . ? C36 C31 C32 C38 178.0(4) . . . . ? C27 C31 C32 C38 -2.2(6) . . . . ? C31 C32 C33 C34 3.9(6) . . . . ? C38 C32 C33 C34 -175.8(4) . . . . ? C39 O3 C34 C35 13.6(6) . . . . ? C39 O3 C34 C33 -166.0(4) . . . . ? C32 C33 C34 C35 -3.3(6) . . . . ? C32 C33 C34 O3 176.2(4) . . . . ? O3 C34 C35 C36 -179.1(4) . . . . ? C33 C34 C35 C36 0.4(6) . . . . ? C34 C35 C36 C31 1.9(6) . . . . ? C34 C35 C36 C37 -178.9(4) . . . . ? C32 C31 C36 C35 -1.3(6) . . . . ? C27 C31 C36 C35 178.9(4) . . . . ? C32 C31 C36 C37 179.5(4) . . . . ? C27 C31 C36 C37 -0.2(6) . . . . ? C28 C29 C40 C45 91.5(5) . . . . ? C30 C29 C40 C45 -86.1(5) . . . . ? C28 C29 C40 C41 -86.7(5) . . . . ? C30 C29 C40 C41 95.7(4) . . . . ? C45 C40 C41 C42 0.5(6) . . . . ? C29 C40 C41 C42 178.7(3) . . . . ? C45 C40 C41 C47 179.1(4) . . . . ? C29 C40 C41 C47 -2.7(6) . . . . ? C40 C41 C42 C43 -0.5(6) . . . . ? C47 C41 C42 C43 -179.1(4) . . . . ? C48 O4 C43 C42 -4.8(6) . . . . ? C48 O4 C43 C44 174.6(4) . . . . ? C41 C42 C43 O4 -179.9(4) . . . . ? C41 C42 C43 C44 0.8(6) . . . . ? O4 C43 C44 C45 179.6(3) . . . . ? C42 C43 C44 C45 -1.0(6) . . . . ? C43 C44 C45 C40 1.0(6) . . . . ? C43 C44 C45 C46 -179.3(4) . . . . ? C41 C40 C45 C44 -0.7(6) . . . . ? C29 C40 C45 C44 -178.9(4) . . . . ? C41 C40 C45 C46 179.6(4) . . . . ? C29 C40 C45 C46 1.4(6) . . . . ? C50 C51 C52 C53 -73(4) . . . . ? C51 C52 C53 C54 26(5) . . . . ? C52 C53 C54 C55 95(4) . . . . ? C53 C54 C55 C56 -126(5) . . . . ? C54 C55 C56 C57 32(7) . . . . ? C55 C56 C57 C58 70(4) . . . . ? C56 C57 C58 C59 -135(2) . . . . ? C57 C58 C59 C60 124(2) . . . . ? C58 C59 C60 C61 -63(3) . . . . ? C59 C60 C61 C50 -21(7) . . . . ? _refine_diff_density_max 1.164 _refine_diff_density_min -0.642 _refine_diff_density_rms 0.098 _shelxl_version_number 2014/5 _shelx_res_file ; TITL shelx New: C2/c New: C2/c CELL 0.71073 28.3480 11.7780 30.9860 90.000 101.909 90.000 ZERR 8.00 0.0060 0.0020 0.0050 0.000 0.006 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H O UNIT 480 592 32 MERG 2 EADP C50 C51 C52 C53 C54 C55 C56 C57 C58 C59 C60 C61 FREE C53 C55 FMAP 2 PLAN 20 ACTA BOND $H CONF L.S. 50 WGHT 0.200000 FVAR 0.15338 O1 3 0.487242 0.189957 0.107061 11.00000 0.04912 0.04802 = 0.04358 -0.00073 0.01819 0.00866 O2 3 0.502209 0.760783 0.455544 11.00000 0.05000 0.04483 = 0.03376 -0.00717 -0.00220 -0.00836 O3 3 0.114655 0.398916 0.426281 11.00000 0.06077 0.05551 = 0.04366 -0.00353 0.02953 -0.00288 O4 3 0.083504 0.562555 0.033010 11.00000 0.04485 0.05378 = 0.02765 0.00422 -0.00486 -0.00075 C1 1 0.500547 0.073078 0.112266 11.00000 0.03943 0.04484 = 0.05039 -0.01319 0.01260 0.00883 AFIX 137 H1A 2 0.516137 0.050549 0.088908 11.00000 -1.50000 H1B 2 0.472206 0.027696 0.111235 11.00000 -1.50000 H1C 2 0.522245 0.062394 0.140155 11.00000 -1.50000 AFIX 0 C2 1 0.468173 0.239243 0.140467 11.00000 0.02912 0.03791 = 0.03786 -0.00459 0.00819 0.00415 C3 1 0.459991 0.355302 0.136174 11.00000 0.04025 0.04919 = 0.04294 0.00514 0.02148 0.00168 AFIX 43 H3 2 0.467989 0.394309 0.112590 11.00000 -1.20000 AFIX 0 C4 1 0.439936 0.413179 0.166942 11.00000 0.03226 0.04087 = 0.04417 -0.00034 0.01252 0.00325 C5 1 0.428320 0.354293 0.202846 11.00000 0.02570 0.03660 = 0.03369 -0.00147 0.00510 -0.00153 C6 1 0.437219 0.237991 0.207382 11.00000 0.03060 0.03389 = 0.03723 -0.00038 0.00900 0.00064 C7 1 0.456723 0.180994 0.175649 11.00000 0.02890 0.03496 = 0.04442 -0.00458 0.00488 0.00105 AFIX 43 H7 2 0.462063 0.103146 0.178196 11.00000 -1.20000 AFIX 0 C8 1 0.426707 0.172742 0.245799 11.00000 0.04845 0.03977 = 0.04832 0.00264 0.01448 0.00711 AFIX 137 H8A 2 0.435095 0.094428 0.243212 11.00000 -1.50000 H8B 2 0.393001 0.178535 0.246114 11.00000 -1.50000 H8C 2 0.445288 0.203434 0.272697 11.00000 -1.50000 AFIX 0 C9 1 0.430879 0.539512 0.161787 11.00000 0.05148 0.04145 = 0.08216 0.01248 0.03543 0.00765 AFIX 137 H9A 2 0.397133 0.554450 0.159298 11.00000 -1.50000 H9B 2 0.440797 0.565803 0.135710 11.00000 -1.50000 H9C 2 0.448960 0.578453 0.187082 11.00000 -1.50000 AFIX 0 C10 1 0.404379 0.415531 0.234966 11.00000 0.02865 0.03359 = 0.03671 -0.00336 0.00605 0.00093 C11 1 0.431570 0.469115 0.272292 11.00000 0.02394 0.03747 = 0.04140 -0.00331 0.00288 -0.00329 AFIX 43 H11 2 0.465036 0.469122 0.276775 11.00000 -1.20000 AFIX 0 C12 1 0.408772 0.523159 0.303219 11.00000 0.02808 0.02884 = 0.03429 -0.00316 0.00398 -0.00166 C13 1 0.358392 0.521061 0.295397 11.00000 0.02852 0.03353 = 0.03010 -0.00300 0.00530 -0.00130 AFIX 43 H13 2 0.342959 0.555856 0.315614 11.00000 -1.20000 AFIX 0 C14 1 0.330448 0.468834 0.258474 11.00000 0.02543 0.03048 = 0.02771 0.00285 0.00384 -0.00151 C15 1 0.354379 0.416450 0.228633 11.00000 0.03261 0.02803 = 0.02941 -0.00183 0.00550 -0.00154 AFIX 43 H15 2 0.336304 0.381153 0.203796 11.00000 -1.20000 AFIX 0 C16 1 0.436579 0.581592 0.343255 11.00000 0.02582 0.03357 = 0.03858 -0.00284 0.00515 0.00174 C17 1 0.453834 0.694237 0.340655 11.00000 0.03110 0.03460 = 0.03704 -0.00311 0.00103 -0.00294 C18 1 0.475722 0.747182 0.379005 11.00000 0.03964 0.03135 = 0.03877 -0.00146 0.00137 -0.00230 AFIX 43 H18 2 0.487323 0.820609 0.377455 11.00000 -1.20000 AFIX 0 C19 1 0.481231 0.695936 0.419796 11.00000 0.03397 0.03837 = 0.03795 -0.00709 0.00358 -0.00547 C20 1 0.465497 0.585438 0.421797 11.00000 0.03642 0.04075 = 0.03310 -0.00205 -0.00017 -0.00780 AFIX 43 H20 2 0.469918 0.548815 0.448926 11.00000 -1.20000 AFIX 0 C21 1 0.443094 0.528081 0.383736 11.00000 0.02983 0.03179 = 0.04187 -0.00326 0.00145 -0.00371 C22 1 0.425498 0.407175 0.387533 11.00000 0.04837 0.03781 = 0.04878 0.00202 -0.00139 -0.01151 AFIX 137 H22A 2 0.443004 0.373586 0.414317 11.00000 -1.50000 H22B 2 0.430664 0.363486 0.362765 11.00000 -1.50000 H22C 2 0.391724 0.408161 0.387912 11.00000 -1.50000 AFIX 0 C23 1 0.448420 0.754175 0.297313 11.00000 0.05347 0.04636 = 0.04505 -0.00044 -0.00062 -0.01543 AFIX 137 H23A 2 0.459071 0.831349 0.302235 11.00000 -1.50000 H23B 2 0.415168 0.753174 0.282451 11.00000 -1.50000 H23C 2 0.467549 0.716445 0.279454 11.00000 -1.50000 AFIX 0 C24 1 0.512427 0.706365 0.497357 11.00000 0.06970 0.05993 = 0.03830 -0.00547 -0.00736 -0.01719 AFIX 137 H24A 2 0.526965 0.759833 0.519530 11.00000 -1.50000 H24B 2 0.534192 0.644281 0.496632 11.00000 -1.50000 H24C 2 0.483027 0.678209 0.504164 11.00000 -1.50000 AFIX 0 C25 1 0.277284 0.467229 0.251549 11.00000 0.02492 0.02624 = 0.02780 -0.00139 0.00112 0.00120 C26 1 0.254430 0.455396 0.286939 11.00000 0.02918 0.02928 = 0.02386 -0.00085 0.00395 0.00369 AFIX 43 H26 2 0.272998 0.449935 0.315349 11.00000 -1.20000 AFIX 0 C27 1 0.204135 0.451518 0.280781 11.00000 0.02873 0.03029 = 0.02835 -0.00084 0.00541 0.00071 C28 1 0.176891 0.463484 0.237846 11.00000 0.02278 0.03401 = 0.03361 -0.00177 0.00386 0.00287 AFIX 43 H28 2 0.143436 0.461817 0.233402 11.00000 -1.20000 AFIX 0 C29 1 0.198151 0.477693 0.201864 11.00000 0.02667 0.02889 = 0.03139 -0.00235 0.00434 -0.00087 C30 1 0.248579 0.477276 0.208991 11.00000 0.02318 0.02926 = 0.03170 -0.00149 0.00457 -0.00092 AFIX 43 H30 2 0.263397 0.483805 0.184979 11.00000 -1.20000 AFIX 0 C31 1 0.180112 0.435566 0.318837 11.00000 0.02684 0.04040 = 0.02593 -0.00005 0.00026 0.00314 C32 1 0.170936 0.530322 0.343829 11.00000 0.03219 0.03635 = 0.03515 -0.00202 0.00348 0.00828 C33 1 0.147371 0.513958 0.378170 11.00000 0.04436 0.04146 = 0.03064 -0.00437 0.01127 0.00618 AFIX 43 H33 2 0.139379 0.576209 0.393682 11.00000 -1.20000 AFIX 0 C34 1 0.135397 0.404070 0.389827 11.00000 0.03383 0.04512 = 0.03170 -0.00501 0.01162 0.00010 C35 1 0.144902 0.312528 0.365604 11.00000 0.03572 0.03463 = 0.03541 -0.00021 0.01034 -0.00356 AFIX 43 H35 2 0.136757 0.239907 0.373324 11.00000 -1.20000 AFIX 0 C36 1 0.166576 0.327199 0.329648 11.00000 0.02876 0.03912 = 0.03454 -0.00422 0.01012 -0.00344 C37 1 0.175370 0.224449 0.303697 11.00000 0.05513 0.04214 = 0.04823 -0.00775 0.02318 -0.00592 AFIX 137 H37A 2 0.197503 0.174493 0.322254 11.00000 -1.50000 H37B 2 0.188785 0.247624 0.279063 11.00000 -1.50000 H37C 2 0.145442 0.185559 0.293189 11.00000 -1.50000 AFIX 0 C38 1 0.186229 0.648251 0.334351 11.00000 0.05445 0.03679 = 0.04703 -0.00243 0.01851 0.00297 AFIX 137 H38A 2 0.163892 0.702247 0.341916 11.00000 -1.50000 H38B 2 0.186677 0.654900 0.303559 11.00000 -1.50000 H38C 2 0.217891 0.662980 0.351518 11.00000 -1.50000 AFIX 0 C39 1 0.112482 0.287211 0.445091 11.00000 0.05759 0.06017 = 0.04423 0.00245 0.02940 -0.00550 AFIX 137 H39A 2 0.101497 0.293422 0.472301 11.00000 -1.50000 H39B 2 0.143982 0.253460 0.450614 11.00000 -1.50000 H39C 2 0.090525 0.240562 0.424849 11.00000 -1.50000 AFIX 0 C40 1 0.168596 0.497394 0.156911 11.00000 0.02546 0.03581 = 0.02457 -0.00292 0.00435 0.00127 C41 1 0.150076 0.403897 0.129487 11.00000 0.03066 0.03705 = 0.03246 -0.00062 0.00356 -0.00442 C42 1 0.121672 0.425173 0.087889 11.00000 0.03385 0.03813 = 0.03138 -0.00373 0.00111 -0.00561 AFIX 43 H42 2 0.109633 0.364581 0.069672 11.00000 -1.20000 AFIX 0 C43 1 0.111159 0.534923 0.073349 11.00000 0.02957 0.04294 = 0.02520 0.00295 0.00333 -0.00023 C44 1 0.129512 0.625070 0.100190 11.00000 0.03346 0.03536 = 0.03553 0.00528 0.00078 0.00846 AFIX 43 H44 2 0.122764 0.698821 0.090058 11.00000 -1.20000 AFIX 0 C45 1 0.157431 0.608232 0.141400 11.00000 0.03359 0.02946 = 0.03163 -0.00279 0.00200 -0.00012 C46 1 0.176379 0.709198 0.169973 11.00000 0.05737 0.03576 = 0.04543 -0.00258 -0.01559 0.00382 AFIX 137 H46A 2 0.170309 0.777512 0.152824 11.00000 -1.50000 H46B 2 0.210446 0.700740 0.180825 11.00000 -1.50000 H46C 2 0.160403 0.713391 0.194394 11.00000 -1.50000 AFIX 0 C47 1 0.162147 0.284341 0.145090 11.00000 0.05813 0.03440 = 0.03932 0.00461 -0.00139 -0.00849 AFIX 137 H47A 2 0.143020 0.231922 0.125056 11.00000 -1.50000 H47B 2 0.155410 0.274799 0.173989 11.00000 -1.50000 H47C 2 0.195712 0.270047 0.146175 11.00000 -1.50000 AFIX 0 C48 1 0.067190 0.472575 0.002466 11.00000 0.06212 0.06350 = 0.02768 -0.00033 -0.00439 -0.01334 AFIX 137 H48A 2 0.048796 0.503796 -0.024414 11.00000 -1.50000 H48B 2 0.047347 0.421375 0.015017 11.00000 -1.50000 H48C 2 0.094494 0.432255 -0.003674 11.00000 -1.50000 AFIX 0 C50 1 0.240839 0.565780 -0.011529 11.00000 0.28571 0.46673 = 0.18330 0.14066 0.13974 0.16565 AFIX 23 H50A 2 0.253624 0.490085 -0.013713 11.00000 -1.20000 H50B 2 0.209342 0.562061 -0.031004 11.00000 -1.20000 AFIX 0 C51 1 0.221967 0.536024 0.025244 11.00000 0.28571 0.46673 = 0.18330 0.14066 0.13974 0.16565 AFIX 23 H51A 2 0.200414 0.472489 0.016226 11.00000 -1.20000 H51B 2 0.201915 0.599100 0.030566 11.00000 -1.20000 AFIX 0 C52 1 0.251200 0.505999 0.067334 11.00000 0.28571 0.46673 = 0.18330 0.14066 0.13974 0.16565 AFIX 23 H52A 2 0.272724 0.570763 0.073042 11.00000 -1.20000 H52B 2 0.228633 0.517188 0.086606 11.00000 -1.20000 AFIX 0 C53 1 0.279059 0.423762 0.088482 11.00000 0.28571 0.46673 = 0.18330 0.14066 0.13974 0.16565 AFIX 23 H53A 2 0.303246 0.460787 0.110744 11.00000 -1.20000 H53B 2 0.258977 0.380031 0.104197 11.00000 -1.20000 AFIX 0 C54 1 0.302196 0.349657 0.068613 11.00000 0.28571 0.46673 = 0.18330 0.14066 0.13974 0.16565 AFIX 23 H54A 2 0.298027 0.279479 0.083779 11.00000 -1.20000 H54B 2 0.281095 0.342438 0.039817 11.00000 -1.20000 AFIX 0 C55 1 0.334704 0.339872 0.061747 11.00000 0.28571 0.46673 = 0.18330 0.14066 0.13974 0.16565 AFIX 23 H55A 2 0.347407 0.279549 0.082171 11.00000 -1.20000 H55B 2 0.350600 0.407858 0.075221 11.00000 -1.20000 AFIX 0 C56 1 0.360831 0.320636 0.028318 11.00000 0.28571 0.46673 = 0.18330 0.14066 0.13974 0.16565 AFIX 23 H56A 2 0.392765 0.351359 0.039489 11.00000 -1.20000 H56B 2 0.364746 0.238967 0.027050 11.00000 -1.20000 AFIX 0 C57 1 0.347942 0.356709 -0.015572 11.00000 0.28571 0.46673 = 0.18330 0.14066 0.13974 0.16565 AFIX 23 H57A 2 0.315994 0.324730 -0.025383 11.00000 -1.20000 H57B 2 0.368745 0.311927 -0.030176 11.00000 -1.20000 AFIX 0 C58 1 0.344802 0.463984 -0.038613 11.00000 0.28571 0.46673 = 0.18330 0.14066 0.13974 0.16565 AFIX 23 H58A 2 0.347984 0.522712 -0.016252 11.00000 -1.20000 H58B 2 0.373250 0.469076 -0.051345 11.00000 -1.20000 AFIX 0 C59 1 0.306436 0.494371 -0.071250 11.00000 0.28571 0.46673 = 0.18330 0.14066 0.13974 0.16565 AFIX 23 H59A 2 0.318407 0.497418 -0.098381 11.00000 -1.20000 H59B 2 0.283806 0.431653 -0.074392 11.00000 -1.20000 AFIX 0 C60 1 0.280637 0.588874 -0.070136 11.00000 0.28571 0.46673 = 0.18330 0.14066 0.13974 0.16565 AFIX 23 H60A 2 0.257292 0.594857 -0.097740 11.00000 -1.20000 H60B 2 0.302130 0.653569 -0.068337 11.00000 -1.20000 AFIX 0 C61 1 0.256653 0.595870 -0.036340 11.00000 0.28571 0.46673 = 0.18330 0.14066 0.13974 0.16565 AFIX 23 H61A 2 0.277343 0.652029 -0.018971 11.00000 -1.20000 H61B 2 0.229455 0.640078 -0.051713 11.00000 -1.20000 AFIX 0 HKLF 4 REM shelx New: C2/c New: C2/c REM R1 = 0.1189 for 5974 Fo > 4sig(Fo) and 0.1959 for all 11700 data REM 523 parameters refined using 0 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 1.164, deepest hole -0.642, 1-sigma level 0.098 Q1 1 0.3606 0.4598 0.0564 11.00000 0.05 1.16 Q2 1 0.3959 0.4051 0.0245 11.00000 0.05 1.09 Q3 1 0.3398 0.4459 -0.0512 11.00000 0.05 0.95 Q4 1 0.2519 0.5921 0.0798 11.00000 0.05 0.82 Q5 1 0.3334 0.3781 0.0820 11.00000 0.05 0.78 Q6 1 0.2982 0.4371 0.1014 11.00000 0.05 0.71 Q7 1 0.2600 0.4268 -0.0477 11.00000 0.05 0.68 Q8 1 0.2977 0.5119 0.0799 11.00000 0.05 0.67 Q9 1 0.3709 0.3576 -0.0132 11.00000 0.05 0.59 Q10 1 0.3126 0.3602 -0.0283 11.00000 0.05 0.55 Q11 1 0.2458 0.5601 -0.0349 11.00000 0.05 0.53 Q12 1 0.2416 0.6292 0.0029 11.00000 0.05 0.53 Q13 1 0.2267 0.4139 0.0383 11.00000 0.05 0.51 Q14 1 0.2681 0.5813 0.0316 11.00000 0.05 0.48 Q15 1 0.2033 0.4739 -0.0013 11.00000 0.05 0.47 Q16 1 0.2222 0.6222 0.0334 11.00000 0.05 0.45 Q17 1 0.3811 0.4387 -0.0143 11.00000 0.05 0.42 Q18 1 0.1611 0.4539 0.1456 11.00000 0.05 0.39 Q19 1 0.1969 0.6833 0.1980 11.00000 0.05 0.38 Q20 1 0.3467 0.2460 0.0300 11.00000 0.05 0.37 ; _shelx_res_checksum 96380 _shelx_hkl_file ; 1 1 0 106.24 5.06 2 2 0 6647.07 214.39 -2 -2 0 6251.10 176.33 -3 -3 0 58.24 3.85 3 3 0 78.69 5.14 4 4 0 488.96 20.18 -4 -4 0 461.00 16.76 -5 -5 0 44.51 4.59 5 5 0 40.78 5.15 6 6 0 20.62 4.26 -6 -6 0 28.52 4.21 7 7 0 10.93 3.52 -7 -7 0 8.73 2.65 -7 -7 0 1.87 1.52 -8 -8 0 0.08 1.23 -8 -8 0 3.98 2.41 -9 -9 0 0.45 1.90 -9 -9 0 -0.41 1.83 -10 -10 0 20.79 4.93 -11 -11 0 13.50 4.49 -12 -12 0 6.80 3.37 -13 -13 0 3.46 3.36 -15 -13 0 -1.47 2.84 -14 -12 0 14.39 4.72 -13 -11 0 23.32 5.89 -12 -10 0 2.73 2.65 -11 -9 0 87.19 9.21 -10 -8 0 22.33 4.50 -10 -8 0 25.05 4.20 -9 -7 0 36.81 5.30 9 7 0 42.86 7.13 -9 -7 0 27.60 3.91 -8 -6 0 115.06 6.83 8 6 0 119.70 9.66 -8 -6 0 111.97 7.50 -7 -5 0 178.55 9.28 -7 -5 0 179.56 8.60 7 5 0 192.91 11.99 -6 -4 0 376.29 13.40 6 4 0 338.47 17.24 -6 -4 0 350.82 13.78 -5 -3 0 251.70 9.93 -5 -3 0 255.33 9.48 5 3 0 248.34 12.92 -4 -2 0 668.74 21.11 4 2 0 698.46 26.90 -4 -2 0 707.86 21.44 3 1 0 1519.30 53.73 -3 -1 0 1537.70 43.40 -3 -1 0 1568.34 45.65 0 -2 0 5410.21 144.19 0 -2 0 5077.46 151.48 -1 -3 0 163.48 7.38 -1 -3 0 176.19 7.44 1 3 0 178.32 7.92 -2 -4 0 1.74 1.04 2 4 0 4.22 1.47 -2 -4 0 4.30 1.45 -3 -5 0 -0.12 0.99 -3 -5 0 0.66 0.92 3 5 0 -0.25 1.42 4 6 0 11.28 2.96 -4 -6 0 10.33 2.51 -4 -6 0 9.14 2.39 5 7 0 9.64 3.06 -5 -7 0 7.93 2.54 -5 -7 0 10.06 2.62 -6 -8 0 7.35 2.47 -6 -8 0 1.31 1.71 -7 -9 0 38.44 5.65 -7 -9 0 28.74 5.22 -8 -10 0 45.41 6.30 -8 -10 0 62.95 7.90 -9 -11 0 1.94 2.77 -10 -12 0 8.44 4.01 -11 -13 0 4.63 3.44 -12 -14 0 2.48 3.17 -17 -13 0 12.50 4.75 -16 -12 0 6.85 4.01 -15 -11 0 6.37 3.43 -14 -10 0 5.38 3.09 -13 -9 0 9.59 3.52 -12 -8 0 9.61 3.48 11 7 0 12.73 4.74 -11 -7 0 10.98 3.11 -11 -7 0 8.61 2.39 -10 -6 0 8.73 2.72 -10 -6 0 13.60 2.61 10 6 0 17.12 4.95 -9 -5 0 251.37 10.78 -9 -5 0 272.12 12.39 9 5 0 272.01 16.45 8 4 0 99.73 8.76 -8 -4 0 105.37 5.37 -8 -4 0 95.63 6.08 -7 -3 0 37.65 2.70 7 3 0 36.13 5.41 -7 -3 0 33.11 3.40 6 2 0 2859.41 100.60 -6 -2 0 2962.37 84.07 -6 -2 0 2829.21 80.97 -5 -1 0 179.82 6.27 -5 -1 0 188.06 7.02 5 1 0 179.55 10.15 4 0 0 320.18 14.02 -4 0 0 297.22 10.11 -3 1 0 1480.47 42.53 -2 2 0 6039.97 166.77 -2 2 0 6103.93 176.06 2 -2 0 5954.44 174.25 1 -3 0 163.83 7.22 1 -3 0 140.39 6.54 0 -4 0 1835.88 57.45 0 -4 0 1901.15 54.87 1 5 0 174.74 8.78 -1 -5 0 173.33 8.82 -1 -5 0 171.60 8.96 -2 -6 0 350.88 15.23 -2 -6 0 356.46 15.49 2 6 0 371.94 16.00 -3 -7 0 -1.08 1.08 3 7 0 -0.42 1.68 -3 -7 0 0.46 1.63 -4 -8 0 3.22 2.35 -4 -8 0 12.13 3.26 -5 -9 0 6.80 2.80 -5 -9 0 8.04 3.11 -6 -10 0 26.78 5.39 -6 -10 0 38.45 6.11 -7 -11 0 25.64 5.63 -8 -12 0 -0.74 2.59 -9 -13 0 0.80 2.80 -10 -14 0 14.02 5.43 -18 -12 0 7.81 4.18 -17 -11 0 3.89 3.17 -16 -10 0 13.59 4.44 -15 -9 0 -1.23 2.38 -14 -8 0 0.97 1.82 13 7 0 6.62 3.61 -13 -7 0 0.13 1.79 -12 -6 0 3.17 1.88 12 6 0 10.15 4.55 -12 -6 0 5.04 1.87 -11 -5 0 26.59 2.99 11 5 0 36.03 7.06 -11 -5 0 25.22 4.03 10 4 0 5.23 3.08 -10 -4 0 2.78 1.29 -10 -4 0 5.66 1.91 -9 -3 0 5.21 1.30 -9 -3 0 2.56 1.24 9 3 0 -0.08 1.66 8 2 0 82.98 7.76 -8 -2 0 96.91 4.15 -8 -2 0 86.71 5.08 -7 -1 0 2443.90 68.51 -7 -1 0 2468.43 70.91 7 1 0 2341.92 86.36 -6 0 0 1291.54 37.75 6 0 0 1286.45 48.35 -5 1 0 166.13 7.01 -4 2 0 642.33 21.25 -3 3 0 59.14 4.75 -3 3 0 67.71 5.19 3 -3 0 57.78 4.06 2 -4 0 1.93 1.15 2 -4 0 1.54 1.09 1 -5 0 198.24 9.23 1 -5 0 159.02 8.95 0 -6 0 302.16 13.97 0 -6 0 300.57 13.54 -1 -7 0 37.45 5.09 -1 -7 0 43.93 5.50 1 7 0 42.02 4.50 -2 -8 0 6.75 2.69 -2 -8 0 7.04 2.65 -3 -9 0 18.89 4.22 -3 -9 0 11.69 3.48 -4 -10 0 72.58 8.61 -4 -10 0 85.99 8.71 -5 -11 0 -2.19 1.78 -6 -12 0 3.23 3.16 -7 -13 0 1.58 2.72 -8 -14 0 -1.15 2.99 -20 -12 0 -0.52 3.31 -19 -11 0 2.97 3.27 -18 -10 0 2.08 2.75 -17 -9 0 0.39 2.43 -16 -8 0 4.46 2.81 -15 -7 0 14.08 3.99 15 7 0 8.94 5.05 -14 -6 0 23.62 4.55 14 6 0 23.94 6.74 -13 -5 0 13.22 3.25 13 5 0 14.02 5.21 -13 -5 0 12.57 2.14 -12 -4 0 220.75 8.92 12 4 0 220.74 16.45 -12 -4 0 224.45 11.07 -11 -3 0 35.54 4.08 11 3 0 29.38 6.44 -11 -3 0 40.70 2.81 -10 -2 0 112.40 4.92 -10 -2 0 101.72 6.02 10 2 0 129.09 10.89 -9 -1 0 238.40 8.66 9 1 0 222.39 14.80 -9 -1 0 239.98 9.66 -8 0 0 540.82 18.15 -7 1 0 2310.55 66.25 -6 2 0 2809.95 80.48 -5 3 0 230.96 11.00 -4 4 0 440.46 18.80 -4 4 0 424.73 17.56 4 -4 0 434.38 16.77 3 -5 0 -0.48 0.97 3 -5 0 -0.13 0.97 2 -6 0 328.21 15.13 2 -6 0 346.32 14.68 1 -7 0 38.38 5.30 1 -7 0 33.14 4.91 0 -8 0 69.36 7.37 0 -8 0 68.55 7.18 -1 -9 0 1.19 1.90 -1 -9 0 -0.69 1.84 -2 -10 0 -0.97 1.85 -3 -11 0 10.15 3.76 -4 -12 0 -2.52 2.56 -5 -13 0 5.30 3.69 -6 -14 0 -1.81 2.97 -21 -11 0 4.42 3.70 -20 -10 0 7.30 4.07 -19 -9 0 9.40 3.70 -18 -8 0 1.25 2.29 -17 -7 0 5.20 2.83 16 6 0 2.46 4.10 -16 -6 0 1.83 2.12 15 5 0 29.13 7.49 -15 -5 0 29.38 4.83 14 4 0 10.92 4.95 -14 -4 0 12.94 2.05 -14 -4 0 19.32 3.71 -13 -3 0 106.69 5.08 -13 -3 0 94.87 6.58 13 3 0 115.14 12.92 12 2 0 123.71 11.87 -12 -2 0 143.26 6.12 -12 -2 0 134.32 7.55 -11 -1 0 600.80 20.76 -11 -1 0 624.15 19.92 11 1 0 593.05 29.97 -10 0 0 2073.29 60.67 -9 1 0 251.85 10.93 -8 2 0 82.36 5.54 -7 3 0 34.67 4.39 -6 4 0 344.91 15.65 -5 5 0 35.50 5.50 -5 5 0 41.34 6.10 4 -6 0 10.13 2.85 -4 6 0 5.49 2.85 -4 6 0 7.19 2.88 3 -7 0 1.38 1.59 3 -7 0 1.89 1.69 2 -8 0 10.38 3.19 2 -8 0 10.74 3.36 1 -9 0 0.59 1.82 0 -10 0 2.73 2.81 -1 -11 0 -1.92 2.42 -2 -12 0 80.96 10.42 -3 -13 0 10.51 4.26 -4 -14 0 5.24 3.48 -23 -11 0 2.75 3.49 -22 -10 0 1.88 2.68 -21 -9 0 2.34 3.14 -20 -8 0 1.32 2.85 -19 -7 0 -0.38 1.98 -18 -6 0 4.20 2.86 -17 -5 0 3.97 2.66 -16 -4 0 10.11 2.96 16 4 0 10.46 5.37 15 3 0 8.30 4.46 -15 -3 0 5.60 2.07 -15 -3 0 8.48 1.61 -14 -2 0 31.35 4.23 14 2 0 33.13 7.79 -14 -2 0 34.79 2.89 -13 -1 0 264.70 10.47 -13 -1 0 279.58 11.98 -12 0 0 856.90 28.37 -11 1 0 606.12 21.78 -10 2 0 98.96 6.53 -9 3 0 2.54 1.66 -8 4 0 98.95 7.46 -7 5 0 162.01 10.72 -6 6 0 28.74 5.41 -6 6 0 23.69 4.88 -5 7 0 3.57 2.44 -5 7 0 5.05 2.93 -4 8 0 4.93 3.16 -4 8 0 7.81 2.90 3 -9 0 15.51 4.28 2 -10 0 3.72 2.94 1 -11 0 1.21 2.75 0 -12 0 1.65 2.93 -1 -13 0 3.46 3.26 -2 -14 0 2.02 3.42 -3 -15 0 5.16 4.03 -24 -10 0 10.13 4.69 -23 -9 0 14.72 5.14 -22 -8 0 0.62 2.83 -21 -7 0 1.08 2.24 -20 -6 0 -1.52 1.77 -19 -5 0 21.41 4.59 -18 -4 0 9.16 3.02 -17 -3 0 4.30 2.25 -16 -2 0 34.22 3.06 -16 -2 0 31.28 4.57 -15 -1 0 2.34 1.18 -15 -1 0 0.98 1.53 -14 0 0 12.55 2.93 -13 1 0 270.14 12.65 -12 2 0 105.32 7.24 -11 3 0 32.65 4.79 -10 4 0 3.50 2.01 -9 5 0 288.81 15.26 -8 6 0 116.30 9.78 -7 7 0 15.25 4.17 -7 7 0 9.57 3.76 -6 8 0 3.50 2.63 -6 8 0 5.16 2.51 -5 9 0 1.66 2.82 -5 9 0 15.62 4.44 -4 10 0 73.31 10.29 -4 10 0 67.55 9.52 -3 11 0 12.09 4.75 -3 11 0 10.13 4.35 -26 -10 0 3.17 3.21 -25 -9 0 3.40 3.16 -24 -8 0 -3.35 2.48 -23 -7 0 13.84 4.81 -22 -6 0 1.09 2.32 -21 -5 0 13.28 3.80 -20 -4 0 7.20 3.05 -19 -3 0 1.46 2.00 -18 -2 0 34.29 5.12 -17 -1 0 29.06 4.56 -17 -1 0 36.90 3.58 -16 0 0 166.54 9.56 -15 1 0 0.85 1.58 -14 2 0 36.82 5.48 -13 3 0 103.41 7.77 -12 4 0 195.49 11.45 -11 5 0 28.10 5.42 -10 6 0 10.72 3.66 -9 7 0 17.26 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