#------------------------------------------------------------------------------ #$Date: 2014-07-30 07:23:07 +0300 (Wed, 30 Jul 2014) $ #$Revision: 120907 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/51/72/1517241.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1517241 loop_ _publ_author_name 'Pawle, R. H.' 'Haas, T. E.' 'M\"uller, P.' 'Thomas III, S. W.' _publ_section_title ; Twisting and piezochromism of phenylene-ethynylenes with aromatic interactions between side chains and main chains ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/C4SC01466A _journal_year 2014 _chemical_formula_sum 'C40 H20 F10 O6' _chemical_formula_weight 786.56 _chemical_name_systematic ; ? ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2013 _cell_angle_alpha 79.881(7) _cell_angle_beta 81.961(7) _cell_angle_gamma 75.475(7) _cell_formula_units_Z 1 _cell_length_a 6.816(2) _cell_length_b 7.448(3) _cell_length_c 16.417(6) _cell_measurement_temperature 100(2) _cell_volume 790.2(5) _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.996 _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0706 _diffrn_reflns_av_unetI/netI 0.0581 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 11514 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.369 _diffrn_reflns_theta_min 2.856 _exptl_absorpt_coefficient_mu 0.150 _exptl_crystal_density_diffrn 1.653 _exptl_crystal_F_000 398 _exptl_crystal_size_max 0.480 _exptl_crystal_size_mid 0.117 _exptl_crystal_size_min 0.101 _refine_diff_density_max 0.555 _refine_diff_density_min -0.423 _refine_diff_density_rms 0.128 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 254 _refine_ls_number_reflns 3224 _refine_ls_number_restraints 68 _refine_ls_restrained_S_all 1.054 _refine_ls_R_factor_all 0.0908 _refine_ls_R_factor_gt 0.0751 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1469P)^2^+0.3675P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2009 _refine_ls_wR_factor_ref 0.2180 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2558 _reflns_number_total 3224 _reflns_threshold_expression 'I > 2\s(I)' _[local]_cod_data_source_file c4sc01466a1.cif _[local]_cod_data_source_block RP100913_0m_a_a _cod_database_code 1517241 _diffrn_reflns_laue_measured_fraction_full 0.995 _diffrn_reflns_laue_measured_fraction_max 0.996 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.996 _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. ; _shelx_estimated_absorpt_t_min 0.932 _shelx_estimated_absorpt_t_max 0.985 _shelxl_version_number 2013-3 _shelx_res_file ; TITL RP100913_0m in P-1 CELL 0.71073 6.8160 7.4483 16.4170 79.881 81.961 75.475 ZERR 1.00 0.00230 0.00260 0.00580 0.0065 0.0066 0.0065 LATT 1 SFAC C H O F UNIT 40 20 6 10 REM Solution 1 R1 0.142 Rweak 0.006, Alpha= 0.0601 in P-1 REM Formula: C20 O3 F5 L.S. 10 SHEL 999 0.8 ACTA BOND FMAP 2 PLAN 20 SIZE 0.101 0.117 0.480 DELU TEMP -173.150 WGHT 0.146900 0.367500 FVAR 0.60131 F001 4 0.357190 0.124233 1.197028 11.00000 0.03451 0.01242 = 0.02562 -0.00301 -0.00165 -0.00558 F002 4 0.184140 0.781196 1.185936 11.00000 0.04452 0.01118 = 0.03593 0.00152 -0.01146 -0.00573 F003 4 0.291157 0.084341 1.365641 11.00000 0.04358 0.02437 = 0.02440 0.01010 -0.00544 -0.00928 F004 4 0.126580 0.739545 1.353896 11.00000 0.03748 0.02928 = 0.03826 -0.01876 -0.00375 -0.00327 F005 4 0.177945 0.391276 1.443451 11.00000 0.04189 0.04923 = 0.01721 -0.00660 -0.00216 -0.01173 O006 3 0.169387 0.376274 1.067572 11.00000 0.02447 0.01987 = 0.01896 -0.00275 -0.00200 -0.00864 O007 3 0.230583 -0.153867 0.646022 11.00000 0.04089 0.01500 = 0.01897 0.00255 -0.00018 -0.00702 O008 3 0.415671 0.240673 0.976431 11.00000 0.03046 0.02800 = 0.03077 -0.00916 0.00613 -0.01525 C009 1 0.250101 0.253135 1.014968 11.00000 0.02603 0.01383 = 0.01501 0.00318 -0.00287 -0.00609 C00A 1 0.064867 -0.113321 0.935403 11.00000 0.02298 0.01270 = 0.01519 0.00327 -0.00294 -0.00494 C00B 1 0.138453 -0.217966 0.867286 11.00000 0.02174 0.01655 = 0.01788 0.00164 -0.00177 -0.00596 C00C 1 0.173594 0.014863 0.947518 11.00000 0.02040 0.01353 = 0.01559 0.00372 -0.00178 -0.00506 AFIX 43 H00C 2 0.294161 0.024656 0.911950 11.00000 -1.20000 AFIX 0 C00D 1 0.112040 0.127954 1.009400 11.00000 0.02103 0.01168 = 0.01592 0.00514 -0.00368 -0.00545 C00E 1 0.270683 0.453488 1.186766 11.00000 0.01731 0.01403 = 0.02068 0.00009 -0.00382 -0.00443 C00F 1 0.293194 -0.616243 0.767005 11.00000 0.02532 0.02011 = 0.02046 -0.00090 -0.00230 -0.00471 AFIX 43 H00F 2 0.282529 -0.669025 0.824039 11.00000 -1.20000 AFIX 0 C00G 1 0.198899 -0.303815 0.809956 11.00000 0.02120 0.02256 = 0.02097 -0.00094 -0.00189 -0.00746 C00H 1 0.297067 0.278429 1.234948 11.00000 0.02044 0.01646 = 0.02194 -0.00297 -0.00163 -0.00621 C00I 1 0.257178 -0.422377 0.746650 11.00000 0.02078 0.02001 = 0.02305 -0.00316 -0.00198 -0.00480 C00J 1 0.211879 0.607878 1.228744 11.00000 0.02359 0.01465 = 0.02726 -0.00075 -0.00614 -0.00536 C00K 1 0.207479 0.412416 1.360140 11.00000 0.02332 0.02921 = 0.01729 -0.00200 -0.00230 -0.00660 C00L 1 0.265233 0.255579 1.320118 11.00000 0.02532 0.01996 = 0.02202 0.00330 -0.00395 -0.00803 C00M 1 0.306481 0.472286 1.093456 11.00000 0.02728 0.01987 = 0.01996 0.00061 -0.00285 -0.01325 AFIX 23 H00A 2 0.276660 0.606099 1.068572 11.00000 -1.20000 H00B 2 0.449863 0.413992 1.075759 11.00000 -1.20000 AFIX 0 C00N 1 0.322618 -0.463433 0.601683 11.00000 0.02456 0.02327 = 0.01829 -0.00249 -0.00127 -0.00553 AFIX 43 H00N 2 0.332024 -0.411390 0.544533 11.00000 -1.20000 AFIX 0 C00O 1 0.181116 0.588634 1.314539 11.00000 0.02050 0.02461 = 0.02830 -0.01117 -0.00398 -0.00254 C00P 1 0.272109 -0.346131 0.661891 11.00000 0.02292 0.01798 = 0.02388 -0.00128 -0.00225 -0.00511 C00Q 1 0.343651 -0.734858 0.707964 11.00000 0.02934 0.01802 = 0.03633 -0.00397 -0.00637 -0.00248 AFIX 43 H00Q 2 0.367059 -0.866838 0.723796 11.00000 -1.20000 AFIX 0 C00R 1 0.359626 -0.656599 0.624226 11.00000 0.03310 0.02172 = 0.02687 -0.00956 -0.00230 -0.00512 AFIX 43 H00R 2 0.396015 -0.735961 0.582456 11.00000 -1.20000 AFIX 0 C00S 1 0.231363 -0.073592 0.561146 11.00000 0.04057 0.02580 = 0.02264 0.00352 -0.00275 -0.00743 AFIX 137 H00D 2 0.369347 -0.107991 0.533202 11.00000 -1.50000 H00E 2 0.187421 0.063195 0.556903 11.00000 -1.50000 H00G 2 0.137860 -0.120433 0.534603 11.00000 -1.50000 AFIX 0 HKLF 4 REM RP100913_0m in P-1 REM R1 = 0.0751 for 2558 Fo > 4sig(Fo) and 0.0908 for all 3224 data REM 254 parameters refined using 68 restraints END WGHT 0.1473 0.3563 REM Highest difference peak 0.555, deepest hole -0.423, 1-sigma level 0.128 Q1 1 0.1611 0.1018 1.3547 11.00000 0.05 0.56 Q2 1 0.2738 -0.4625 0.6917 11.00000 0.05 0.54 Q3 1 0.2218 -0.4050 0.6296 11.00000 0.05 0.53 Q4 1 0.2094 0.1509 1.1915 11.00000 0.05 0.53 Q5 1 0.2752 -0.2788 0.8410 11.00000 0.05 0.53 Q6 1 0.0260 0.4148 1.4431 11.00000 0.05 0.51 Q7 1 0.4072 0.2447 1.0236 11.00000 0.05 0.51 Q8 1 0.5543 0.2205 0.9854 11.00000 0.05 0.51 Q9 1 0.2812 0.2529 0.9653 11.00000 0.05 0.50 Q10 1 0.0686 -0.2468 0.8289 11.00000 0.05 0.50 Q11 1 -0.0201 0.7575 1.3534 11.00000 0.05 0.50 Q12 1 0.3149 0.3641 1.0727 11.00000 0.05 0.50 Q13 1 0.3391 0.7451 1.1860 11.00000 0.05 0.48 Q14 1 0.0919 -0.1366 0.6283 11.00000 0.05 0.48 Q15 1 0.1614 -0.1066 0.6812 11.00000 0.05 0.45 Q16 1 0.3602 -0.1533 0.6691 11.00000 0.05 0.45 Q17 1 0.0383 0.4061 1.0672 11.00000 0.05 0.44 Q18 1 0.3278 -0.6589 0.7369 11.00000 0.05 0.44 Q19 1 0.1469 0.2409 0.9929 11.00000 0.05 0.44 Q20 1 0.1183 -0.1728 0.8982 11.00000 0.05 0.44 ; _shelx_res_checksum 86715 _shelx_hkl_file ; 1 0 0 52.39 5.20 1 0 0 47.40 5.60 -2 0 0 9999.00 742.33 -2 0 0 8262.87 736.13 -2 0 0 8007.80 690.93 -3 0 0 92.89 8.20 -3 0 0 109.89 8.80 -3 0 0 91.59 8.80 -4 0 0 0.20 1.80 -4 0 0 -1.00 1.30 -4 0 0 -1.10 1.30 -5 0 0 4.10 2.50 -5 0 0 2.20 1.80 -5 0 0 0.60 1.60 -6 0 0 10.10 2.80 -6 0 0 6.60 2.60 -7 0 0 5.00 1.80 -7 0 0 4.60 3.20 7 0 0 7.40 4.20 -8 0 0 5.20 1.80 -8 0 0 6.00 2.40 8 0 0 4.30 2.50 -8 1 0 17.00 2.50 -8 1 0 16.60 3.20 -7 1 0 3.80 3.70 -7 1 0 4.50 1.80 6 -1 0 35.10 5.00 -6 1 0 30.50 5.40 5 -1 0 9.30 2.80 -5 1 0 8.00 2.00 -5 1 0 7.60 2.20 4 -1 0 13.00 2.20 -4 1 0 10.10 1.80 -4 1 0 11.00 2.00 -4 1 0 7.70 1.00 -4 1 0 10.50 1.20 3 -1 0 25.00 3.40 -3 1 0 29.30 2.50 -3 1 0 35.60 3.90 -3 1 0 30.50 3.20 -3 1 0 32.00 2.60 2 -1 0 261.17 25.10 -2 1 0 301.57 23.50 -2 1 0 319.37 21.00 -2 1 0 298.17 21.00 1 -1 0 264.67 18.70 -1 1 0 258.37 18.70 0 -1 0 886.11 74.09 0 -1 0 990.30 66.49 -1 -1 0 52.29 4.40 -1 -1 0 46.60 3.70 -1 -1 0 50.09 4.30 1 1 0 50.99 4.50 1 1 0 49.40 3.80 -2 -1 0 4889.11 300.37 -2 -1 0 3909.81 300.37 -2 -1 0 3939.01 334.97 -3 -1 0 -1.10 1.50 -3 -1 0 -0.20 1.10 -3 -1 0 0.40 1.20 -4 -1 0 267.97 24.60 -4 -1 0 259.67 23.00 -4 -1 0 330.07 24.60 -5 -1 0 3.00 2.30 -5 -1 0 0.00 1.90 -5 -1 0 1.90 1.50 -6 -1 0 4.70 2.30 -7 -1 0 10.20 4.40 -8 -1 0 -0.10 1.70 7 -2 0 17.90 2.90 -7 2 0 14.10 4.40 -7 2 0 10.50 2.40 6 -2 0 0.30 3.80 -6 2 0 -0.40 1.40 -6 2 0 1.00 2.90 5 -2 0 6.40 2.90 -5 2 0 6.80 1.60 -5 2 0 9.40 1.50 -5 2 0 5.40 2.30 -5 2 0 6.50 2.30 4 -2 0 141.19 13.40 -4 2 0 143.49 13.60 -4 2 0 169.88 11.20 -4 2 0 147.49 11.00 -4 2 0 150.08 12.50 3 -2 0 62.09 6.60 -3 2 0 67.29 5.30 -3 2 0 73.09 6.90 -3 2 0 75.99 5.50 2 -2 0 171.38 16.90 2 -2 0 209.58 14.30 -2 2 0 197.88 14.10 -2 2 0 205.58 14.20 1 -2 0 94.29 7.50 1 -2 0 71.59 6.30 -1 2 0 89.59 7.40 -1 2 0 72.99 6.20 0 -2 0 748.43 50.09 0 -2 0 626.24 59.49 0 2 0 736.23 50.09 0 2 0 662.63 55.69 0 2 0 752.52 50.09 -1 -2 0 78.99 6.80 -1 -2 0 88.09 7.50 1 2 0 71.39 6.20 1 2 0 86.89 7.30 -2 -2 0 176.48 14.80 -2 -2 0 197.78 15.70 -2 -2 0 188.68 13.30 -2 -2 0 169.98 13.20 2 2 0 184.48 13.30 -3 -2 0 35.10 3.50 -3 -2 0 28.10 3.50 -3 -2 0 25.90 2.50 -3 -2 0 30.20 2.80 3 2 0 34.40 3.40 -4 -2 0 -1.20 1.90 -4 -2 0 0.90 0.80 -4 -2 0 -0.30 1.10 -4 -2 0 0.30 0.50 4 2 0 -0.10 1.50 -5 -2 0 8.70 1.80 -5 -2 0 11.60 3.10 5 2 0 7.40 2.40 -6 -2 0 42.30 5.00 6 2 0 37.80 6.20 -7 -2 0 4.90 1.40 7 2 0 2.30 4.00 -8 -2 0 3.80 1.70 8 2 0 7.50 2.30 7 -3 0 3.90 3.00 -6 3 0 -0.60 1.60 -6 3 0 2.60 2.10 -6 3 0 0.70 0.60 5 -3 0 58.19 7.90 -5 3 0 54.79 6.20 -5 3 0 58.69 4.70 -5 3 0 73.59 5.90 4 -3 0 5.10 2.70 -4 3 0 6.70 2.20 -4 3 0 5.20 2.00 -4 3 0 4.90 1.20 3 -3 0 3.10 1.70 -3 3 0 3.50 1.70 -3 3 0 1.70 0.80 -3 3 0 -0.10 1.40 2 -3 0 121.69 11.40 2 -3 0 127.79 9.80 -2 3 0 147.79 11.50 -2 3 0 117.89 9.50 1 -3 0 143.09 11.30 -1 3 0 148.59 11.10 -1 3 0 178.48 13.30 -1 3 0 132.49 11.30 0 -3 0 0.90 1.70 0 -3 0 0.20 1.70 0 3 0 -1.60 1.10 0 3 0 0.30 1.10 0 3 0 -0.50 1.40 -1 -3 0 162.48 10.90 -1 -3 0 150.18 13.20 1 3 0 133.59 12.90 -2 -3 0 725.23 55.09 -2 -3 0 832.72 61.49 2 3 0 768.22 55.19 -3 -3 0 126.19 10.20 -3 -3 0 130.69 11.50 -3 -3 0 146.19 10.40 -3 -3 0 157.78 12.30 -4 -3 0 42.10 3.60 -4 -3 0 42.80 4.50 -4 -3 0 44.90 5.00 -4 -3 0 44.80 4.00 4 3 0 46.50 5.00 -5 -3 0 407.26 33.60 -5 -3 0 437.66 35.90 -5 -3 0 457.05 29.90 -5 -3 0 423.06 29.80 5 3 0 365.76 35.90 -6 -3 0 65.99 6.20 -6 -3 0 75.09 8.50 6 3 0 49.90 7.50 -7 -3 0 15.40 2.70 -7 -3 0 19.30 4.90 7 3 0 16.40 4.30 -8 -3 0 11.60 2.10 8 3 0 16.50 2.70 6 -4 0 3.70 2.40 -6 4 0 -0.90 0.90 -6 4 0 1.00 3.00 -6 4 0 3.10 1.80 5 -4 0 38.40 5.00 -5 4 0 38.50 4.70 -5 4 0 39.50 3.40 -5 4 0 45.80 6.10 4 -4 0 -1.30 2.70 -4 4 0 0.10 2.60 3 -4 0 7.40 2.10 3 -4 0 4.10 3.30 -3 4 0 4.60 1.10 -3 4 0 5.90 1.90 -3 4 0 4.70 2.40 2 -4 0 4.90 2.70 2 -4 0 5.80 1.70 -2 4 0 2.10 1.00 -2 4 0 2.90 2.20 -2 4 0 2.00 1.70 1 -4 0 29.40 4.10 -1 4 0 32.00 3.40 -1 4 0 34.00 3.80 0 -4 0 97.59 9.40 0 -4 0 119.69 8.50 0 4 0 108.19 8.10 0 4 0 86.79 9.20 0 4 0 101.09 8.60 -1 -4 0 345.97 24.10 -1 -4 0 304.37 28.60 1 4 0 357.06 24.20 1 4 0 330.57 26.80 -2 -4 0 96.49 8.20 -2 -4 0 88.19 6.70 -2 -4 0 83.09 7.40 2 4 0 77.69 7.20 -3 -4 0 16.90 3.00 -3 -4 0 12.60 1.80 -3 -4 0 16.50 2.40 3 4 0 14.00 2.80 -4 -4 0 10.90 2.00 -4 -4 0 12.20 2.50 -4 -4 0 9.10 1.60 -4 -4 0 11.80 2.20 -5 -4 0 3.00 2.80 -5 -4 0 0.40 1.00 -5 -4 0 -2.10 1.80 -5 -4 0 1.10 1.50 -6 -4 0 -0.40 1.10 -6 -4 0 2.00 3.80 -6 -4 0 0.30 1.70 -6 -4 0 0.70 0.70 6 4 0 0.10 3.50 -7 -4 0 27.00 3.50 7 4 0 41.00 8.00 -8 -4 0 2.90 2.50 -8 -4 0 -1.80 1.60 5 -5 0 302.17 25.50 -5 5 0 269.57 25.50 -5 5 0 297.47 21.10 -4 5 0 21.00 2.70 3 -5 0 514.35 44.70 -3 5 0 529.25 37.50 2 -5 0 140.49 11.70 2 -5 0 149.19 12.80 -2 5 0 121.29 11.90 -2 5 0 144.59 10.90 -2 5 0 143.29 12.90 1 -5 0 101.29 8.90 -1 5 0 91.89 7.90 -1 5 0 90.19 9.10 0 -5 0 7.80 2.20 0 -5 0 6.90 2.20 0 5 0 9.60 3.00 0 5 0 7.60 2.40 0 5 0 6.70 2.10 -1 -5 0 25.00 3.60 -1 -5 0 19.60 3.90 1 5 0 21.10 3.90 1 5 0 25.10 3.70 1 5 0 20.80 2.90 -2 -5 0 34.80 4.30 -2 -5 0 32.40 3.70 2 5 0 27.10 4.50 2 5 0 35.30 5.10 2 5 0 35.50 4.10 -3 -5 0 104.79 9.00 -3 -5 0 82.09 8.20 -3 -5 0 102.49 8.40 -3 -5 0 97.69 7.40 3 5 0 86.99 8.60 -4 -5 0 5.20 1.70 -4 -5 0 6.70 1.20 -4 -5 0 8.30 2.60 -4 -5 0 7.50 2.40 4 5 0 3.60 3.60 -5 -5 0 4.60 2.50 -5 -5 0 6.60 3.30 -6 -5 0 37.00 3.00 -6 -5 0 45.90 7.50 -6 -5 0 38.50 5.30 -6 -5 0 26.10 3.80 -7 -5 0 15.30 2.60 -7 -5 0 17.40 2.00 -7 -5 0 15.90 2.50 7 5 0 26.90 5.90 -8 -5 0 28.40 4.00 -8 -5 0 23.60 5.00 8 5 0 36.00 7.40 -5 6 0 7.00 1.40 -5 6 0 1.20 2.10 4 -6 0 18.10 3.20 -4 6 0 9.60 1.80 -4 6 0 11.60 2.40 3 -6 0 8.30 2.30 -3 6 0 11.40 1.80 2 -6 0 105.69 9.70 2 -6 0 96.19 10.80 -2 6 0 101.19 8.90 1 -6 0 24.80 4.30 1 -6 0 30.80 4.10 -1 6 0 24.70 3.70 -1 6 0 29.70 5.50 0 -6 0 364.86 32.20 0 -6 0 390.46 27.50 0 6 0 362.06 30.10 0 6 0 375.56 32.50 -1 -6 0 9.30 2.70 -1 -6 0 8.40 2.70 1 6 0 10.10 3.10 1 6 0 10.90 3.30 1 6 0 7.10 2.50 -2 -6 0 10.80 2.20 -2 -6 0 10.40 2.40 2 6 0 10.10 3.30 2 6 0 9.20 2.70 2 6 0 8.40 2.80 -3 -6 0 -0.70 1.40 -3 -6 0 0.70 2.00 3 6 0 1.60 3.60 3 6 0 0.00 2.10 -4 -6 0 7.80 3.00 -4 -6 0 6.50 1.40 -5 -6 0 -0.60 0.90 -5 -6 0 -1.60 3.30 -6 -6 0 2.00 0.90 -6 -6 0 3.40 1.50 -7 -6 0 45.30 5.60 -7 -6 0 38.00 3.40 -7 -6 0 41.80 4.60 -7 -6 0 30.30 5.00 3 -7 0 12.40 2.90 -3 7 0 8.70 2.40 -3 7 0 10.70 2.00 2 -7 0 23.10 4.00 -2 7 0 17.30 2.40 -2 7 0 20.20 3.70 1 -7 0 34.00 5.20 1 -7 0 30.60 4.50 -1 7 0 35.00 4.70 0 -7 0 6.80 2.10 0 -7 0 6.90 4.00 0 7 0 5.50 3.90 0 7 0 5.70 3.00 0 7 0 5.10 3.60 -1 -7 0 86.29 8.30 -1 -7 0 71.89 7.70 1 7 0 80.79 8.20 1 7 0 80.69 9.10 1 7 0 85.19 8.90 -2 -7 0 63.09 6.40 -2 -7 0 71.59 7.10 2 7 0 69.49 9.00 2 7 0 66.29 7.40 2 7 0 58.19 7.90 -3 -7 0 2.90 1.70 -3 -7 0 3.60 2.50 3 7 0 3.00 3.00 3 7 0 0.90 4.70 -4 -7 0 1.40 1.10 -4 -7 0 0.30 1.50 4 7 0 -0.90 1.60 -5 -7 0 -1.50 1.10 5 7 0 -3.10 1.60 -6 -7 0 4.70 2.40 -6 -7 0 6.10 1.20 6 7 0 4.60 2.10 2 -8 0 3.00 2.70 -2 8 0 8.00 2.60 -2 8 0 0.40 2.10 1 -8 0 5.30 2.40 -1 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-19 11.50 3.50 -1 0 19 1.00 2.20 -1 0 19 6.20 1.50 0 0 -19 45.60 6.00 0 0 -19 59.39 7.40 0 0 19 44.30 5.90 0 0 19 51.29 5.60 -1 0 -19 3.10 3.00 1 0 19 -1.30 3.50 1 0 19 -1.40 5.50 1 0 19 -2.30 1.90 -2 0 -19 5.80 2.80 -2 0 -19 -0.90 1.50 2 0 19 -1.90 2.40 2 0 19 -2.70 1.80 -3 0 -19 18.90 3.20 -3 0 -19 17.80 3.40 3 0 19 22.70 3.70 2 -1 -19 10.10 3.40 -2 1 19 6.70 1.80 -1 1 19 14.70 2.20 -1 1 19 12.90 2.50 0 -1 -19 22.50 3.90 0 -1 -19 18.70 4.80 0 1 19 17.10 4.10 -1 -1 -19 14.30 3.40 1 1 19 13.00 4.00 1 1 19 13.50 2.30 -2 -1 -19 38.10 4.10 -2 -1 -19 30.80 5.20 2 1 19 31.00 4.60 -3 -1 -19 30.50 5.00 -3 -1 -19 25.80 3.50 -3 -1 -19 30.30 4.30 3 1 19 22.70 3.10 -4 -1 -19 7.80 2.60 -4 -1 -19 1.80 1.40 -4 -1 -19 4.50 2.20 4 1 19 1.60 1.70 2 -2 -19 6.90 3.40 -2 2 19 2.80 2.30 -2 2 19 4.60 1.70 1 -2 -19 5.10 3.20 0 -2 -19 13.10 4.30 0 2 19 13.60 4.00 0 2 19 14.20 2.50 -1 -2 -19 4.90 3.90 -1 -2 -19 1.40 2.50 -1 -2 -19 2.80 4.00 1 2 19 3.60 4.20 1 2 19 -2.40 1.90 -2 -2 -19 29.90 4.80 2 2 19 25.20 3.40 -3 -2 -19 50.19 5.70 -3 -2 -19 53.39 4.70 3 2 19 45.60 5.30 -4 -2 -19 1.20 1.40 -4 -2 -19 3.90 2.00 4 2 19 2.40 1.80 1 -3 -19 16.20 3.50 -1 3 19 9.90 2.40 -1 3 19 11.30 2.00 0 -3 -19 26.50 5.20 0 3 19 22.00 4.30 0 3 19 33.20 5.80 -1 -3 -19 8.90 2.50 -1 -3 -19 7.00 4.60 1 3 19 4.40 4.40 -2 -3 -19 -1.40 5.10 -2 -3 -19 0.30 2.00 -2 -3 -19 -2.60 1.50 2 3 19 -0.60 1.80 -3 -3 -19 1.60 1.50 -3 -3 -19 5.70 2.00 -3 -3 -19 3.70 4.70 3 3 19 1.80 1.70 -4 -3 -19 2.60 2.20 -4 -3 -19 4.10 1.50 4 3 19 2.30 1.80 0 -4 -19 52.19 6.40 0 4 19 35.30 5.20 1 4 19 3.60 4.30 -2 -4 -19 82.29 6.40 -2 -4 -19 66.49 7.50 2 4 19 73.79 7.10 -3 -4 -19 -1.40 1.40 -3 -4 -19 -2.50 2.20 3 4 19 -3.60 1.70 -4 -4 -19 14.30 2.30 -4 -4 -19 20.00 3.30 4 4 19 16.00 2.70 -1 -5 -19 3.10 1.60 -1 -5 -19 2.20 2.10 1 5 19 5.70 1.90 1 5 19 3.40 4.70 -2 -5 -19 9.00 1.80 -2 -5 -19 9.70 2.40 2 5 19 7.40 2.00 -3 -5 -19 -1.10 1.80 3 5 19 -2.80 1.70 0 0 -20 7.50 3.80 0 0 -20 4.80 5.10 0 0 20 2.00 4.40 0 0 20 5.60 2.20 -1 0 -20 12.00 2.10 -1 0 -20 18.40 3.70 1 0 20 10.20 2.50 -2 0 -20 11.50 1.90 -2 0 -20 15.10 3.50 2 0 20 7.60 2.70 2 0 20 4.20 2.30 1 -1 -20 12.40 3.90 -1 1 20 12.10 2.60 -1 1 20 10.90 2.00 0 -1 -20 -1.20 3.50 0 -1 -20 -0.50 4.80 0 1 20 0.70 4.10 0 1 20 -3.90 2.00 -1 -1 -20 -1.10 1.90 -1 -1 -20 -1.80 3.10 1 1 20 6.10 2.10 -2 -1 -20 -2.90 2.10 -2 -1 -20 -1.10 1.70 -2 -1 -20 -0.30 2.70 2 1 20 3.30 2.00 -3 -1 -20 12.80 3.00 -3 -1 -20 11.50 2.50 -3 -1 -20 9.40 1.90 0 -2 -20 8.50 3.20 0 -2 -20 2.70 4.60 0 2 20 -0.30 2.00 -1 -2 -20 10.30 2.00 -1 -2 -20 4.90 3.10 -1 -2 -20 6.90 4.80 1 2 20 2.80 2.10 1 2 20 6.70 5.00 -2 -2 -20 0.90 1.60 -2 -2 -20 0.20 2.50 2 2 20 -2.70 1.90 -3 -2 -20 1.30 2.50 3 2 20 -0.30 1.90 0 -3 -20 37.30 5.70 0 -3 -20 22.80 6.10 0 3 20 24.60 4.50 -1 -3 -20 35.60 4.50 -1 -3 -20 38.20 6.40 -1 -3 -20 49.60 5.80 1 3 20 32.50 5.00 1 3 20 34.70 5.80 -2 -3 -20 0.40 1.80 -2 -3 -20 -1.80 2.10 -2 -3 -20 3.40 2.30 2 3 20 -1.00 1.90 -3 -3 -20 6.10 2.30 -3 -3 -20 3.00 1.50 3 3 20 3.70 1.90 -2 -4 -20 0.60 1.50 -2 -4 -20 2.10 2.20 2 4 20 1.10 2.00 ; _shelx_hkl_checksum 37437 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 F001 F 0.3572(2) 0.1242(2) 1.19703(10) 0.0243(4) Uani 1 1 d . U F002 F 0.1841(3) 0.7812(2) 1.18594(11) 0.0306(5) Uani 1 1 d . U F003 F 0.2912(3) 0.0843(3) 1.36564(11) 0.0320(5) Uani 1 1 d . U F004 F 0.1266(3) 0.7395(3) 1.35390(12) 0.0341(5) Uani 1 1 d . U F005 F 0.1779(3) 0.3913(3) 1.44345(11) 0.0358(5) Uani 1 1 d . U O006 O 0.1694(3) 0.3763(3) 1.06757(12) 0.0205(5) Uani 1 1 d . U O007 O 0.2306(3) -0.1539(3) 0.64602(12) 0.0258(5) Uani 1 1 d . U O008 O 0.4157(3) 0.2407(3) 0.97643(13) 0.0285(5) Uani 1 1 d . U C009 C 0.2501(4) 0.2531(4) 1.01497(16) 0.0186(6) Uani 1 1 d . U C00A C 0.0649(4) -0.1133(4) 0.93540(16) 0.0174(5) Uani 1 1 d . U C00B C 0.1385(4) -0.2180(4) 0.86729(16) 0.0190(6) Uani 1 1 d . U C00C C 0.1736(4) 0.0149(4) 0.94752(16) 0.0170(5) Uani 1 1 d . U H00C H 0.2942 0.0247 0.9119 0.020 Uiso 1 1 calc R U C00D C 0.1120(4) 0.1280(4) 1.00940(16) 0.0166(5) Uani 1 1 d . U C00E C 0.2707(4) 0.4535(4) 1.18677(16) 0.0173(6) Uani 1 1 d . U C00F C 0.2932(4) -0.6162(4) 0.76701(18) 0.0223(6) Uani 1 1 d . U H00F H 0.2825 -0.6690 0.8240 0.027 Uiso 1 1 calc R U C00G C 0.1989(4) -0.3038(4) 0.80996(17) 0.0214(6) Uani 1 1 d . U C00H C 0.2971(4) 0.2784(4) 1.23495(17) 0.0193(6) Uani 1 1 d . U C00I C 0.2572(4) -0.4224(4) 0.74665(18) 0.0213(6) Uani 1 1 d . U C00J C 0.2119(4) 0.6079(4) 1.22874(18) 0.0216(6) Uani 1 1 d . U C00K C 0.2075(4) 0.4124(4) 1.36014(17) 0.0233(6) Uani 1 1 d . U C00L C 0.2652(4) 0.2556(4) 1.32012(18) 0.0226(6) Uani 1 1 d . U C00M C 0.3065(4) 0.4723(4) 1.09346(17) 0.0214(6) Uani 1 1 d . U H00A H 0.2767 0.6061 1.0686 0.026 Uiso 1 1 calc R U H00B H 0.4499 0.4140 1.0758 0.026 Uiso 1 1 calc R U C00N C 0.3226(4) -0.4634(4) 0.60168(17) 0.0222(6) Uani 1 1 d . U H00N H 0.3320 -0.4114 0.5445 0.027 Uiso 1 1 calc R U C00O C 0.1811(4) 0.5886(4) 1.31454(18) 0.0239(6) Uani 1 1 d . U C00P C 0.2721(4) -0.3461(4) 0.66189(18) 0.0218(6) Uani 1 1 d . U C00Q C 0.3437(4) -0.7349(4) 0.7080(2) 0.0281(7) Uani 1 1 d . U H00Q H 0.3671 -0.8668 0.7238 0.034 Uiso 1 1 calc R U C00R C 0.3596(5) -0.6566(4) 0.62423(19) 0.0268(6) Uani 1 1 d . U H00R H 0.3960 -0.7360 0.5825 0.032 Uiso 1 1 calc R U C00S C 0.2314(5) -0.0736(5) 0.56115(19) 0.0306(7) Uani 1 1 d . U H00D H 0.3693 -0.1080 0.5332 0.046 Uiso 1 1 calc R U H00E H 0.1874 0.0632 0.5569 0.046 Uiso 1 1 calc R U H00G H 0.1379 -0.1204 0.5346 0.046 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 F001 0.0345(10) 0.0124(8) 0.0256(9) -0.0030(7) -0.0017(7) -0.0056(6) F002 0.0445(11) 0.0112(8) 0.0359(10) 0.0015(7) -0.0115(8) -0.0057(7) F003 0.0436(11) 0.0244(10) 0.0244(9) 0.0101(7) -0.0054(7) -0.0093(8) F004 0.0375(10) 0.0293(10) 0.0383(11) -0.0188(9) -0.0037(8) -0.0033(8) F005 0.0419(11) 0.0492(13) 0.0172(9) -0.0066(8) -0.0022(7) -0.0117(9) O006 0.0245(10) 0.0199(10) 0.0190(10) -0.0028(8) -0.0020(7) -0.0086(8) O007 0.0409(12) 0.0150(10) 0.0190(10) 0.0026(8) -0.0002(8) -0.0070(8) O008 0.0305(11) 0.0280(12) 0.0308(12) -0.0092(9) 0.0061(9) -0.0152(9) C009 0.0260(14) 0.0138(12) 0.0150(12) 0.0032(10) -0.0029(10) -0.0061(10) C00A 0.0230(13) 0.0127(12) 0.0152(12) 0.0033(9) -0.0029(10) -0.0049(10) C00B 0.0217(13) 0.0166(13) 0.0179(13) 0.0016(10) -0.0018(10) -0.0060(10) C00C 0.0204(13) 0.0135(12) 0.0156(12) 0.0037(10) -0.0018(9) -0.0051(10) C00D 0.0210(13) 0.0117(12) 0.0159(12) 0.0051(10) -0.0037(9) -0.0054(9) C00E 0.0173(12) 0.0140(13) 0.0207(13) 0.0001(10) -0.0038(9) -0.0044(10) C00F 0.0253(14) 0.0201(14) 0.0205(14) -0.0009(11) -0.0023(10) -0.0047(11) C00G 0.0212(13) 0.0226(14) 0.0210(13) -0.0009(11) -0.0019(10) -0.0075(11) C00H 0.0204(13) 0.0165(13) 0.0219(14) -0.0030(11) -0.0016(10) -0.0062(10) C00I 0.0208(13) 0.0200(14) 0.0231(14) -0.0032(11) -0.0020(10) -0.0048(11) C00J 0.0236(14) 0.0147(13) 0.0273(15) -0.0008(11) -0.0061(11) -0.0054(10) C00K 0.0233(14) 0.0292(16) 0.0173(13) -0.0020(12) -0.0023(10) -0.0066(11) C00L 0.0253(14) 0.0200(14) 0.0220(14) 0.0033(11) -0.0040(11) -0.0080(11) C00M 0.0273(14) 0.0199(13) 0.0200(14) 0.0006(11) -0.0029(10) -0.0132(11) C00N 0.0246(14) 0.0233(15) 0.0183(13) -0.0025(11) -0.0013(10) -0.0055(11) C00O 0.0205(14) 0.0246(15) 0.0283(15) -0.0112(12) -0.0040(11) -0.0025(11) C00P 0.0229(14) 0.0180(14) 0.0239(14) -0.0013(11) -0.0022(10) -0.0051(10) C00Q 0.0293(15) 0.0180(14) 0.0363(17) -0.0040(12) -0.0064(12) -0.0025(11) C00R 0.0331(16) 0.0217(15) 0.0269(15) -0.0096(12) -0.0023(12) -0.0051(12) C00S 0.0406(18) 0.0258(16) 0.0226(15) 0.0035(12) -0.0027(12) -0.0074(13) 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C009 O006 C00M 117.0(2) . . C00P O007 C00S 116.1(2) . . O008 C009 O006 124.5(2) . . O008 C009 C00D 123.0(2) . . O006 C009 C00D 112.5(2) . . C00C C00A C00D 117.5(2) . 2_557 C00C C00A C00B 117.7(2) . . C00D C00A C00B 124.8(2) 2_557 . C00G C00B C00A 179.4(3) . . C00D C00C C00A 122.5(2) . . C00C C00D C00A 119.9(2) . 2_557 C00C C00D C009 115.4(2) . . C00A C00D C009 124.6(2) 2_557 . C00H C00E C00J 116.8(3) . . C00H C00E C00M 120.7(2) . . C00J C00E C00M 122.4(2) . . C00Q C00F C00I 122.7(3) . . C00B C00G C00I 173.0(3) . . F001 C00H C00L 118.5(2) . . F001 C00H C00E 119.0(2) . . C00L C00H C00E 122.5(3) . . C00F C00I C00P 118.0(3) . . C00F C00I C00G 120.9(3) . . C00P C00I C00G 121.1(3) . . F002 C00J C00O 118.3(3) . . F002 C00J C00E 119.9(3) . . C00O C00J C00E 121.8(3) . . F005 C00K C00O 120.3(3) . . F005 C00K C00L 119.7(3) . . C00O C00K C00L 120.0(3) . . F003 C00L C00H 121.5(3) . . F003 C00L C00K 119.3(3) . . C00H C00L C00K 119.3(3) . . O006 C00M C00E 106.3(2) . . C00P C00N C00R 120.5(3) . . F004 C00O C00K 119.6(3) . . F004 C00O C00J 120.9(3) . . C00K C00O C00J 119.6(3) . . O007 C00P C00N 124.9(3) . . O007 C00P C00I 115.1(2) . . C00N C00P C00I 120.0(3) . . C00F C00Q C00R 118.4(3) . . C00N C00R C00Q 120.4(3) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 F001 C00H 1.348(3) . F002 C00J 1.339(3) . F003 C00L 1.344(3) . F004 C00O 1.341(3) . F005 C00K 1.341(3) . O006 C009 1.335(3) . O006 C00M 1.455(3) . O007 C00P 1.373(3) . O007 C00S 1.416(4) . O008 C009 1.205(3) . C009 C00D 1.502(4) . C00A C00C 1.401(4) . C00A C00D 1.419(4) 2_557 C00A C00B 1.436(4) . C00B C00G 1.198(4) . C00C C00D 1.386(4) . C00D C00A 1.419(4) 2_557 C00E C00H 1.385(4) . C00E C00J 1.389(4) . C00E C00M 1.504(4) . C00F C00Q 1.376(4) . C00F C00I 1.390(4) . C00G C00I 1.431(4) . C00H C00L 1.372(4) . C00I C00P 1.407(4) . C00J C00O 1.382(4) . C00K C00O 1.375(4) . C00K C00L 1.385(4) . C00N C00P 1.384(4) . C00N C00R 1.388(4) . C00Q C00R 1.396(4) .