#------------------------------------------------------------------------------ #$Date: 2022-04-20 01:23:03 +0300 (Wed, 20 Apr 2022) $ #$Revision: 274584 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/68/1566825.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_1566825 loop_ _publ_author_name 'Zhou, Jun' 'Mao, Lijun' 'Wu, Meng-Xiang' 'Peng, Zhiyong' 'Yang, Yiming' 'Zhou, Manfei' 'Zhao, Xiao-Li' 'Shi, Xueliang' 'Yang, Hai-Bo' _publ_section_title ; Extended phenothiazines: synthesis, photophysical and redox properties, and efficient photocatalytic oxidative coupling of amines ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D2SC01086K _journal_year 2022 _chemical_formula_moiety 'C26 H23 N S' _chemical_formula_sum 'C26 H23 N S' _chemical_formula_weight 381.51 _space_group_crystal_system orthorhombic _space_group_IT_number 56 _space_group_name_Hall '-P 2ab 2ac' _space_group_name_H-M_alt 'P c c n' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2022-01-24 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408) ; _audit_update_record ; 2022-01-28 deposited with the CCDC. 2022-04-08 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 23.8497(9) _cell_length_b 21.8615(7) _cell_length_c 7.9142(3) _cell_measurement_reflns_used 4242 _cell_measurement_temperature 201(40) _cell_measurement_theta_max 72.7470 _cell_measurement_theta_min 3.6830 _cell_volume 4126.4(3) _computing_cell_refinement 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/1 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 201(40) _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w 23.00 49.00 0.50 2.00 -- 0.00 16.00 -29.00 52 2 \w -32.00 -7.00 0.50 2.00 -- 0.00 -16.00 160.00 50 3 \w 127.00 152.00 0.50 10.00 -- 95.80 16.00 -29.00 50 4 \w 92.00 119.00 0.50 10.00 -- 95.80 -16.00 160.00 54 5 \w -66.00 21.00 0.50 2.00 -- 0.00 -57.00 60.00 174 6 \w -60.00 -30.00 0.50 2.00 -- 0.00 -37.00 0.00 60 7 \w 84.00 182.00 0.50 10.00 -- 95.80 30.00 60.00 196 8 \w 56.00 107.00 0.50 10.00 -- 95.80 -82.00 -30.00 102 9 \w 8.00 34.00 0.50 10.00 -- 95.80 -82.00 -30.00 52 10 \w 7.00 90.00 0.50 10.00 -- 95.80 -30.00 90.00 166 11 \w 79.00 104.00 0.50 10.00 -- 95.80 30.00-150.00 50 12 \w 121.00 147.00 0.50 10.00 -- 95.80 30.00-150.00 52 13 \w 14.00 114.00 0.50 10.00 -- 95.80 -61.00 30.00 200 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB AFC12 (RINC): Kappa dual home/near' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0445297000 _diffrn_orient_matrix_UB_12 -0.0505982000 _diffrn_orient_matrix_UB_13 -0.0180589000 _diffrn_orient_matrix_UB_21 -0.0448418000 _diffrn_orient_matrix_UB_22 0.0487576000 _diffrn_orient_matrix_UB_23 -0.0386521000 _diffrn_orient_matrix_UB_31 0.0133256000 _diffrn_orient_matrix_UB_32 -0.0051118000 _diffrn_orient_matrix_UB_33 -0.1900000000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0673 _diffrn_reflns_av_unetI/netI 0.0620 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 16520 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 67.080 _diffrn_reflns_theta_max 67.080 _diffrn_reflns_theta_min 3.707 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 1.453 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.64509 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.228 _exptl_crystal_description block _exptl_crystal_F_000 1616 _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.766 _refine_diff_density_min -0.465 _refine_diff_density_rms 0.069 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 256 _refine_ls_number_reflns 3670 _refine_ls_number_restraints 14 _refine_ls_restrained_S_all 1.069 _refine_ls_R_factor_all 0.0987 _refine_ls_R_factor_gt 0.0834 _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^)+(0.0806P)^2^+9.4770P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2097 _refine_ls_wR_factor_ref 0.2207 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2974 _reflns_number_total 3670 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d2sc01086k2.cif _cod_data_source_block exp_2556 _cod_database_code 1566825 _shelx_shelxl_version_number 2018/1 _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_max 0.845 _shelx_estimated_absorpt_t_min 0.623 _reflns_odcompleteness_completeness 99.71 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Rigid bond restraints C15, C14 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 C15, C16 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 3. Uiso/Uaniso restraints and constraints C14 \\sim C15: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A C16 \\sim C15: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A 4.a Aromatic/amide H refined with riding coordinates: C15(H15), C13(H13), C10(H10), C2(H2), C8(H8), C21(H21), C22(H22), C18(H18), C19(H19), C12(H12), C5(H5), C11(H11), C3(H3), C4(H4) 4.b Idealised Me refined as rotating group: C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C24(H24A,H24B,H24C) ; _shelx_res_file ; TITL exp_2556_a.res in Pccn exp_2556.res created by SHELXL-2018/1 at 11:26:08 on 24-Jan-2022 REM Old TITL exp_2556 in Pccn REM SHELXT solution in Pccn REM R1 0.171, Rweak 0.021, Alpha 0.039, Orientation as input REM Formula found by SHELXT: C26 N S CELL 1.54184 23.8497 21.8615 7.9142 90 90 90 ZERR 8 0.0009 0.0007 0.0003 0 0 0 LATT 1 SYMM 0.5-X,0.5-Y,+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,-Y,0.5-Z SFAC C H N S UNIT 208 184 8 8 DELU 0.001 0.001 C15 C14 SIMU 0.01 0.02 2 C14 C15 SIMU 0.01 0.02 2 C16 C15 DELU 0.001 0.001 C15 C16 L.S. 99 PLAN 2 SIZE 0.36 0.14 0.12 CONF list 4 fmap 2 53 MORE -1 BOND $H ACTA SHEL 999 0.837 OMIT 1 3 1 OMIT 1 2 1 OMIT 1 4 1 OMIT 2 2 2 OMIT 3 5 0 OMIT 2 2 1 REM REM REM WGHT 0.080600 9.476999 FVAR 0.21710 S1 4 0.308740 0.503040 0.027437 11.00000 0.07336 0.04475 = 0.03567 0.00109 -0.01285 0.00788 N1 3 0.368328 0.437087 0.318582 11.00000 0.04284 0.03994 = 0.03308 -0.00008 -0.00866 0.00567 C6 1 0.341969 0.398993 0.198825 11.00000 0.03696 0.03950 = 0.03728 0.00290 0.00649 0.00537 C14 1 0.312256 0.617982 0.421473 11.00000 0.03673 0.03495 = 0.03802 0.00844 0.00060 -0.00296 C9 1 0.344899 0.585272 0.540688 11.00000 0.04053 0.03787 = 0.03972 0.00713 -0.00431 -0.00858 C16 1 0.317562 0.530486 0.231830 11.00000 0.03841 0.03366 = 0.03749 0.00517 -0.00352 0.00264 C15 1 0.298888 0.588675 0.260088 11.00000 0.03336 0.02861 = 0.05417 0.00392 -0.01583 0.00039 AFIX 43 H15 2 0.278111 0.609246 0.178482 11.00000 -1.20000 AFIX 0 C17 1 0.403475 0.409867 0.446390 11.00000 0.04043 0.03411 = 0.03894 -0.00016 -0.00384 0.00236 C13 1 0.297486 0.678890 0.455369 11.00000 0.04599 0.03685 = 0.03931 0.00661 0.00469 0.00079 AFIX 43 H13 2 0.275523 0.700254 0.378261 11.00000 -1.20000 AFIX 0 C7 1 0.349427 0.496711 0.355021 11.00000 0.03115 0.03894 = 0.03862 0.00990 0.00078 0.00475 C20 1 0.471627 0.362273 0.704075 11.00000 0.03906 0.04523 = 0.03785 0.00356 -0.00106 0.00500 C1 1 0.310417 0.423471 0.064216 11.00000 0.04089 0.04505 = 0.03144 0.00146 -0.00031 0.00345 C10 1 0.360660 0.616149 0.692904 11.00000 0.04657 0.04980 = 0.03636 0.00699 -0.00792 -0.00266 AFIX 43 H10 2 0.380816 0.595282 0.775344 11.00000 -1.20000 AFIX 0 C2 1 0.283568 0.385630 -0.050180 11.00000 0.04053 0.05073 = 0.03935 0.00425 0.00041 -0.00047 AFIX 43 H2 2 0.261467 0.402709 -0.134723 11.00000 -1.20000 AFIX 0 C8 1 0.361753 0.525098 0.504782 11.00000 0.03904 0.04066 = 0.04051 0.00792 -0.01127 -0.00347 AFIX 43 H8 2 0.382066 0.503700 0.585823 11.00000 -1.20000 AFIX 0 C21 1 0.413460 0.358249 0.712111 11.00000 0.04444 0.04475 = 0.04053 0.00854 -0.00062 0.00095 AFIX 43 H21 2 0.396943 0.339557 0.805198 11.00000 -1.20000 AFIX 0 C22 1 0.379466 0.381330 0.585211 11.00000 0.03957 0.04385 = 0.04730 0.00257 -0.00475 0.00147 AFIX 43 H22 2 0.340702 0.377700 0.593093 11.00000 -1.20000 AFIX 0 C18 1 0.461105 0.414679 0.435203 11.00000 0.04502 0.04576 = 0.03943 0.00317 0.00323 0.00052 AFIX 43 H18 2 0.477409 0.433699 0.342282 11.00000 -1.20000 AFIX 0 C19 1 0.494695 0.391047 0.563048 11.00000 0.03756 0.06173 = 0.03971 0.00673 -0.00121 0.00609 AFIX 43 H19 2 0.533451 0.394509 0.554311 11.00000 -1.20000 AFIX 0 C12 1 0.314911 0.707323 0.600166 11.00000 0.05201 0.03885 = 0.04601 0.00117 0.00675 -0.00122 AFIX 43 H12 2 0.305523 0.748027 0.619302 11.00000 -1.20000 AFIX 0 C5 1 0.347553 0.335302 0.205433 11.00000 0.04888 0.04315 = 0.04125 0.00253 0.00104 0.00106 AFIX 43 H5 2 0.369141 0.317722 0.290394 11.00000 -1.20000 AFIX 0 C11 1 0.346442 0.675763 0.718241 11.00000 0.05706 0.04561 = 0.04463 -0.00694 -0.00184 -0.00650 AFIX 43 H11 2 0.358076 0.695535 0.816203 11.00000 -1.20000 AFIX 0 C23 1 0.507476 0.337166 0.848783 11.00000 0.04466 0.06502 = 0.02912 0.00631 -0.00587 0.01084 C3 1 0.289154 0.322574 -0.040526 11.00000 0.05329 0.04516 = 0.04880 -0.00623 0.00179 -0.01086 AFIX 43 H3 2 0.271590 0.297125 -0.118407 11.00000 -1.20000 AFIX 0 C4 1 0.321870 0.298476 0.089347 11.00000 0.05460 0.03874 = 0.05860 0.00075 0.01060 -0.00316 AFIX 43 H4 2 0.326328 0.256310 0.097189 11.00000 -1.20000 AFIX 0 C25 1 0.568685 0.334611 0.802008 11.00000 0.05195 0.12128 = 0.05217 0.02555 -0.00112 0.02715 AFIX 137 H25A 2 0.572995 0.312649 0.697773 11.00000 -1.50000 H25B 2 0.589197 0.314123 0.889701 11.00000 -1.50000 H25C 2 0.582854 0.375432 0.788754 11.00000 -1.50000 AFIX 0 C26 1 0.499169 0.374272 1.007122 11.00000 0.07230 0.07768 = 0.05389 -0.00608 -0.00987 0.00771 AFIX 137 H26A 2 0.509263 0.416073 0.985773 11.00000 -1.50000 H26B 2 0.522394 0.358143 1.095613 11.00000 -1.50000 H26C 2 0.460556 0.372254 1.040922 11.00000 -1.50000 AFIX 0 C24 1 0.488331 0.270697 0.885823 11.00000 0.10358 0.06330 = 0.05292 0.00949 -0.01446 0.00488 AFIX 137 H24A 2 0.450578 0.271086 0.927883 11.00000 -1.50000 H24B 2 0.512665 0.252793 0.968832 11.00000 -1.50000 H24C 2 0.489901 0.247074 0.783678 11.00000 -1.50000 AFIX 0 HKLF 4 REM exp_2556_a.res in Pccn REM R1 = 0.0834 for 2974 Fo > 4sig(Fo) and 0.0987 for all 3670 data REM 256 parameters refined using 14 restraints END WGHT 0.0806 9.4771 REM Highest difference peak 0.766, deepest hole -0.465, 1-sigma level 0.069 Q1 1 0.3099 0.5849 0.1663 11.00000 0.05 0.77 Q2 1 0.2776 0.4787 0.0863 11.00000 0.05 0.53 ; _shelx_res_checksum 8653 _shelx_hkl_file ; 2 0 0 1151.13 99.24 3 0 0 0.59 0.67 4 0 0 306.03 26.62 5 0 0 -0.52 1.23 -6 0 0 9417.71 836.20 6 0 0 9999.00 836.21 7 0 0 1.43 1.24 -7 0 0 2.34 1.27 8 0 0 270.58 23.88 9 0 0 -0.13 1.20 -9 0 0 0.27 1.21 -10 0 0 904.53 78.52 10 0 0 901.47 78.46 -11 0 0 1.60 1.34 11 0 0 1.31 1.48 12 0 0 2.99 0.78 -12 0 0 2.44 1.56 12 0 0 1.83 1.36 -13 0 0 0.23 1.39 13 0 0 0.20 1.20 13 0 0 0.76 0.74 -14 0 0 119.27 13.86 14 0 0 158.33 13.16 15 0 0 0.47 0.84 16 0 0 57.87 5.39 17 0 0 0.21 1.04 18 0 0 211.18 18.59 19 0 0 0.08 1.18 20 0 0 112.52 9.81 -20 0 0 102.91 9.79 21 0 0 -0.75 1.38 -21 0 0 -0.45 1.36 22 0 0 23.17 2.82 -22 0 0 22.91 2.79 23 0 0 -0.28 1.36 -23 0 0 1.35 1.44 24 0 0 10.67 1.84 -24 0 0 9.63 1.87 25 0 0 1.28 1.29 -25 0 0 1.21 1.36 -26 0 0 59.21 5.13 26 0 0 49.20 5.03 -27 0 0 1.24 1.02 27 0 0 1.96 0.91 2 -1 0 0.27 0.41 3 1 0 194.65 16.35 -3 -1 0 179.24 16.33 -3 1 0 188.04 16.32 -4 -1 0 0.58 1.03 4 1 0 -0.17 0.97 -4 1 0 -0.22 0.93 5 1 0 119.27 10.44 -5 1 0 113.42 10.41 6 1 0 2.12 1.77 -6 1 0 26.56 2.16 7 -1 0 59.72 5.94 -7 1 0 63.27 5.98 7 1 0 64.15 5.99 8 1 0 0.69 1.24 -8 1 0 2.57 1.20 8 -1 0 1.20 1.45 9 -1 0 214.54 19.98 9 1 0 226.04 20.03 -9 1 0 233.96 20.04 -10 -1 0 3.53 1.55 10 -1 0 4.57 1.58 -10 1 0 8.67 1.98 10 1 0 -0.45 1.32 11 -1 0 81.87 8.24 -11 -1 0 80.21 8.32 -11 1 0 86.21 8.32 11 1 0 96.64 8.38 -12 -1 0 0.21 1.40 -12 1 0 0.21 1.30 12 -1 0 -1.26 1.32 12 -1 0 0.38 0.69 -13 -1 0 78.55 6.70 -13 1 0 67.72 7.50 13 -1 0 75.03 6.69 13 -1 0 77.67 7.44 -13 -1 0 61.78 7.40 14 1 0 0.54 0.82 -14 1 0 -0.52 1.25 14 -1 0 2.43 0.87 -14 -1 0 1.31 1.36 14 -1 0 0.44 1.13 15 -1 0 19.96 2.18 15 1 0 19.97 2.18 16 -1 0 -1.04 0.97 16 1 0 -0.39 0.95 17 1 0 98.04 8.47 17 -1 0 89.44 8.44 18 -1 0 -0.39 1.15 18 1 0 0.78 1.19 -19 1 0 10.52 1.92 19 1 0 13.35 1.89 19 -1 0 14.30 1.94 20 -1 0 3.33 1.46 -20 1 0 -0.34 1.40 20 1 0 1.25 1.36 21 -1 0 16.98 2.24 21 1 0 17.23 2.25 -21 1 0 12.62 2.11 -21 -1 0 12.95 2.17 22 1 0 0.19 1.33 -22 -1 0 0.64 1.55 -22 1 0 -0.18 1.47 22 -1 0 0.19 1.39 23 1 0 6.05 1.64 -23 -1 0 5.45 1.68 23 -1 0 5.38 1.60 -23 1 0 6.04 1.62 24 -1 0 1.62 1.40 -24 1 0 1.36 1.34 -24 -1 0 1.31 1.41 24 1 0 0.95 1.31 -25 -1 0 15.21 1.99 -25 1 0 10.29 1.83 25 -1 0 13.97 1.93 25 1 0 11.39 1.81 26 -1 0 1.56 1.12 26 1 0 1.25 1.07 -26 1 0 -0.21 1.17 -26 -1 0 0.73 1.19 27 -1 0 0.28 0.90 -27 -1 0 0.44 1.01 27 1 0 -0.15 0.79 1 -2 0 0.53 0.44 -1 2 0 0.57 0.44 2 -2 0 796.69 69.38 -2 2 0 811.59 69.39 3 -2 0 1.64 0.73 -3 2 0 0.89 0.81 -4 -2 0 1039.17 92.47 -4 2 0 1071.71 92.44 4 -2 0 1095.46 92.43 -5 2 0 2.48 1.43 -5 -2 0 0.63 1.36 -6 -2 0 176.08 15.46 -6 2 0 170.68 15.38 -7 2 0 1.77 1.21 -8 2 0 18.49 2.40 -9 2 0 0.56 1.21 9 -2 0 1.80 1.25 -10 2 0 3.71 1.55 10 -2 0 4.88 1.48 11 2 0 1.37 0.83 -11 2 0 0.92 1.40 -11 -2 0 1.60 0.68 11 -2 0 -0.64 1.32 12 -2 0 162.82 13.72 -12 -2 0 148.81 12.97 -12 2 0 155.16 13.83 12 -2 0 147.26 12.98 12 2 0 142.11 13.03 13 2 0 0.84 1.01 13 -2 0 0.92 0.80 -13 2 0 0.47 1.34 13 -2 0 -0.59 1.30 -13 -2 0 0.23 0.81 -13 -2 0 1.19 1.34 -14 -2 0 26.81 2.63 14 -2 0 22.62 3.18 -14 2 0 22.48 3.38 14 -2 0 26.17 2.60 14 2 0 26.10 2.75 15 2 0 0.12 0.87 15 2 0 0.52 1.09 15 -2 0 0.96 0.88 -15 -2 0 -0.34 0.93 16 2 0 35.28 3.55 16 2 0 32.77 3.38 16 -2 0 34.29 3.38 17 -2 0 0.44 1.03 17 2 0 -0.15 1.04 -17 2 0 -0.84 1.05 18 2 0 120.71 11.31 18 -2 0 129.26 11.31 -18 2 0 128.93 11.31 -19 2 0 -0.48 1.27 19 -2 0 0.34 1.27 19 2 0 1.34 1.28 -20 2 0 18.29 2.36 20 -2 0 18.33 2.38 20 2 0 15.67 2.28 21 2 0 0.09 1.27 -21 2 0 0.35 1.38 21 -2 0 1.80 1.47 22 -2 0 22.07 2.67 -22 2 0 20.58 2.60 -22 -2 0 20.26 2.71 22 2 0 20.91 2.59 23 -2 0 0.10 1.41 -23 -2 0 0.55 1.55 23 2 0 0.99 1.38 -23 2 0 0.35 1.33 -24 -2 0 14.74 2.22 -24 2 0 15.69 2.14 24 2 0 14.64 2.08 24 -2 0 16.87 2.23 -25 -2 0 2.47 1.41 25 2 0 -0.22 1.10 -25 2 0 2.86 1.31 25 -2 0 1.75 1.30 26 -2 0 9.82 1.54 26 2 0 6.81 1.35 -26 -2 0 10.35 1.67 -26 2 0 9.07 1.55 -27 -2 0 -0.32 1.10 27 -2 0 1.80 0.95 27 2 0 1.48 0.83 -28 -2 0 1.23 0.86 0 -3 0 0.69 0.65 1 -3 0 101.82 8.76 -1 3 0 96.79 8.75 2 -3 0 1.49 0.81 -2 3 0 1.33 0.81 -3 3 0 525.85 44.96 3 -3 0 512.65 44.93 4 -3 0 0.06 1.10 -4 -3 0 2.32 1.38 -4 3 0 1.07 1.29 -5 3 0 203.79 19.12 -5 -3 0 219.06 19.20 5 -3 0 229.39 19.13 -6 -3 0 2.81 1.32 -6 3 0 1.98 1.29 -7 3 0 159.14 14.11 -7 -3 0 155.08 14.17 -8 3 0 1.02 1.23 -8 -3 0 0.56 1.26 -9 3 0 29.47 3.40 10 -3 0 0.60 1.33 -10 3 0 0.33 1.35 11 -3 0 66.76 6.15 11 -3 0 58.99 5.38 -11 -3 0 58.87 5.39 -11 3 0 58.42 6.13 11 3 0 60.70 5.45 12 -3 0 0.27 0.73 -12 3 0 2.98 1.50 12 -3 0 0.18 1.18 12 3 0 1.66 0.90 -12 -3 0 0.96 0.75 13 -3 0 5.82 1.68 13 3 0 9.26 1.39 -13 -3 0 9.37 1.26 -13 3 0 5.54 1.83 13 -3 0 8.03 1.21 14 3 0 1.49 1.11 -14 3 0 1.03 0.86 14 -3 0 0.88 1.15 -14 3 0 -1.89 1.56 -14 -3 0 1.51 0.93 14 -3 0 0.56 0.82 -15 3 0 2.67 0.94 -15 -3 0 1.90 1.03 15 -3 0 2.15 0.95 15 3 0 1.58 1.25 16 3 0 0.50 1.25 16 3 0 1.17 1.05 16 -3 0 0.14 0.92 -16 3 0 0.71 0.96 -16 -3 0 0.89 1.08 17 3 0 33.60 3.48 17 -3 0 34.81 3.47 -17 3 0 36.36 3.49 17 3 0 32.19 3.67 18 -3 0 1.86 1.29 18 3 0 0.08 1.12 -18 3 0 0.83 1.14 19 -3 0 3.39 1.58 19 3 0 2.28 1.33 -19 3 0 6.12 1.54 -20 3 0 -0.17 1.32 20 3 0 0.70 1.28 20 -3 0 -0.55 1.44 -21 3 0 9.39 1.69 21 3 0 4.61 1.53 21 -3 0 6.50 1.71 22 3 0 1.71 1.34 22 -3 0 1.84 1.48 -22 3 0 2.18 1.44 -23 3 0 5.22 1.48 23 3 0 5.38 1.46 23 -3 0 4.79 1.60 -23 -3 0 2.50 1.60 -24 -3 0 1.24 1.50 24 3 0 0.56 1.17 24 -3 0 2.47 1.52 -24 3 0 0.65 1.29 -25 -3 0 0.58 1.43 25 3 0 3.48 1.20 -25 3 0 2.99 1.26 25 -3 0 3.85 1.43 26 -3 0 0.22 1.15 -26 -3 0 0.89 1.30 26 3 0 2.10 0.95 27 -3 0 1.64 1.00 -27 -3 0 1.90 1.11 -28 -3 0 -0.56 0.88 28 -3 0 0.20 0.71 0 -4 0 4077.60 351.32 1 -4 0 -0.05 0.95 -2 4 0 1071.78 94.30 2 -4 0 1113.71 94.31 -3 4 0 2.93 1.29 3 -4 0 5.80 1.39 -4 4 0 33.12 3.68 4 -4 0 39.78 3.67 -5 -4 0 1.28 1.63 5 -4 0 2.96 1.35 -5 4 0 3.13 1.30 -6 4 0 40.53 4.28 -6 -4 0 43.37 4.46 6 -4 0 44.85 4.27 -7 -4 0 2.38 1.42 -7 4 0 1.89 1.30 -8 4 0 499.60 44.22 -8 -4 0 513.23 44.33 -9 4 0 1.85 1.27 -9 -4 0 1.19 1.51 -10 4 0 5.95 1.84 11 -4 0 -0.17 0.71 -11 4 0 0.20 1.32 11 4 0 0.24 0.84 -11 4 0 0.61 0.70 11 -4 0 0.69 1.24 -12 -4 0 8.24 2.08 -12 4 0 14.94 1.49 12 -4 0 12.77 2.15 12 -4 0 12.18 1.50 -12 4 0 14.91 2.38 12 4 0 10.98 1.59 -13 -4 0 2.31 1.53 13 -4 0 0.26 0.74 13 -4 0 1.22 1.20 -13 4 0 0.15 0.76 -13 4 0 -0.25 1.40 13 4 0 1.29 0.97 14 4 0 144.69 12.59 14 -4 0 143.58 13.27 -14 4 0 126.17 13.36 14 -4 0 136.92 12.50 -14 4 0 150.14 12.50 -14 -4 0 139.07 12.49 15 -4 0 0.19 0.90 -15 -4 0 0.53 1.04 -15 4 0 1.21 0.91 15 4 0 1.07 1.24 -16 4 0 156.88 13.79 16 4 0 154.48 13.91 -16 -4 0 155.52 13.80 16 -4 0 156.80 13.81 -17 -4 0 -0.07 1.24 -17 4 0 1.28 1.06 17 4 0 2.21 1.45 17 4 0 0.38 1.09 17 -4 0 0.15 1.08 18 4 0 37.54 3.97 -18 4 0 41.53 3.96 18 -4 0 40.53 4.00 18 4 0 39.27 4.20 -19 4 0 0.08 1.26 19 4 0 0.93 1.25 19 -4 0 -0.44 1.31 -20 4 0 1.85 1.36 20 -4 0 2.04 1.46 20 4 0 2.28 1.34 21 4 0 2.58 1.34 21 -4 0 0.58 1.50 -21 4 0 0.60 1.29 22 -4 0 9.16 1.90 -22 4 0 8.76 1.74 22 4 0 9.03 1.67 23 -4 0 -0.67 1.45 -23 4 0 0.67 1.34 23 4 0 0.17 1.19 -24 -4 0 49.54 4.72 24 -4 0 52.07 4.69 -24 4 0 48.34 4.56 24 4 0 40.12 4.44 25 -4 0 2.26 1.37 25 4 0 -0.07 0.98 -25 -4 0 0.90 1.39 -26 -4 0 0.95 1.26 26 4 0 0.59 0.83 26 -4 0 0.15 1.14 -27 -4 0 -0.56 1.08 27 -4 0 -0.35 0.92 -28 -4 0 0.20 0.82 28 -4 0 0.04 0.67 0 -5 0 6.25 1.64 1 -5 0 54.01 5.14 2 -5 0 4.35 1.39 -2 5 0 4.36 1.30 -3 5 0 76.50 7.33 3 -5 0 83.88 7.37 4 -5 0 1.56 1.18 -4 5 0 0.72 1.18 -5 5 0 28.39 3.04 5 -5 0 28.45 3.00 -6 5 0 0.87 1.11 -6 -5 0 0.54 1.33 6 -5 0 1.07 1.08 -7 -5 0 3.00 1.66 -7 5 0 4.34 1.31 -8 5 0 0.42 1.26 -8 -5 0 1.31 1.52 -9 5 0 9.69 1.86 -9 -5 0 5.89 1.92 10 5 0 0.80 0.78 10 -5 0 0.39 0.68 -10 -5 0 -1.45 1.44 -10 5 0 1.64 1.36 11 5 0 1.96 0.90 -11 5 0 1.19 0.75 11 -5 0 2.46 0.81 -11 5 0 3.68 1.56 12 -5 0 0.59 1.13 -12 5 0 -0.91 1.37 12 -5 0 0.15 0.77 -12 5 0 0.14 0.76 12 5 0 -0.39 0.91 13 -5 0 7.63 1.59 -13 5 0 3.42 0.93 -13 5 0 3.83 1.60 13 5 0 4.54 1.12 13 -5 0 3.83 1.00 -14 5 0 1.70 1.47 14 5 0 0.42 1.11 14 -5 0 1.72 0.98 -14 5 0 1.02 0.85 -15 5 0 9.01 1.34 15 5 0 7.22 1.55 15 -5 0 7.43 1.38 16 5 0 2.06 1.36 16 -5 0 2.84 1.22 -16 5 0 0.67 1.02 -17 5 0 35.35 3.66 17 -5 0 38.87 3.78 17 5 0 39.05 3.95 -17 -5 0 36.10 3.76 -18 5 0 2.23 1.24 -18 -5 0 0.94 1.46 18 5 0 1.56 1.20 18 5 0 2.71 1.70 18 -5 0 1.61 1.36 -19 5 0 2.51 1.29 19 5 0 3.58 1.33 19 5 0 -0.64 1.69 19 -5 0 2.61 1.45 20 5 0 -1.13 1.26 -20 5 0 -2.01 1.26 20 -5 0 2.17 1.51 21 -5 0 4.38 1.65 21 5 0 4.35 1.33 -21 5 0 2.04 1.34 22 -5 0 1.47 1.56 22 5 0 0.09 1.23 -22 5 0 1.26 1.32 23 5 0 3.36 1.27 23 -5 0 5.96 1.72 24 -5 0 3.83 1.50 24 5 0 -0.58 1.02 -24 -5 0 0.89 1.50 25 -5 0 0.66 1.34 -25 -5 0 0.08 1.39 25 5 0 0.87 0.93 -26 -5 0 0.87 1.21 26 -5 0 1.94 1.20 27 -5 0 -0.06 0.92 -27 -5 0 -1.23 1.12 28 -5 0 0.86 0.68 -28 -5 0 -1.02 0.87 -29 -5 0 0.07 0.58 0 -6 0 238.30 20.97 1 -6 0 4.67 1.48 2 -6 0 356.41 31.09 -3 6 0 1.78 1.05 3 -6 0 1.01 1.05 -4 6 0 43.44 4.21 4 -6 0 42.06 4.21 -5 6 0 0.50 1.08 5 -6 0 2.80 1.11 -6 6 0 21.62 2.60 -6 -6 0 22.50 2.95 6 -6 0 22.27 2.56 -7 6 0 1.05 1.18 7 -6 0 4.24 1.35 -7 -6 0 3.04 1.63 -8 -6 0 250.01 22.68 -8 6 0 254.58 22.49 -9 -6 0 1.41 1.63 -9 6 0 -1.51 1.34 10 6 0 8.70 1.26 10 -6 0 9.37 1.24 -10 6 0 8.82 1.99 -10 -6 0 9.19 2.14 -11 -6 0 -0.75 1.48 11 6 0 1.05 0.91 11 -6 0 1.33 0.79 -11 6 0 0.22 0.71 -12 6 0 11.92 2.31 12 -6 0 12.99 1.65 -12 6 0 14.19 1.59 12 6 0 14.40 1.73 -13 6 0 2.08 1.34 13 -6 0 -0.22 1.21 13 -6 0 0.54 0.87 13 6 0 -0.39 1.01 -13 6 0 0.70 0.81 14 -6 0 56.73 5.39 -14 6 0 61.01 5.38 14 6 0 56.51 5.49 -15 6 0 0.45 0.94 15 -6 0 1.90 1.16 15 6 0 -0.24 1.23 16 -6 0 9.27 1.59 16 6 0 11.24 1.82 -17 6 0 0.51 1.07 17 -6 0 1.71 1.26 17 6 0 1.90 1.53 18 6 0 29.45 3.44 -18 6 0 29.62 3.10 18 -6 0 28.44 3.22 19 6 0 1.29 1.68 -19 6 0 1.30 1.32 19 -6 0 1.75 1.54 19 6 0 2.05 1.25 20 -6 0 2.40 1.52 20 6 0 2.50 1.31 -20 6 0 2.41 1.31 21 -6 0 0.79 1.48 21 6 0 0.09 1.17 -21 6 0 1.00 1.27 22 6 0 2.20 1.27 22 -6 0 3.94 1.64 23 -6 0 0.48 1.52 23 6 0 -0.30 1.03 24 -6 0 21.65 2.44 24 6 0 16.38 2.07 -25 -6 0 2.00 1.43 25 -6 0 -0.65 1.28 25 6 0 0.23 0.83 -26 -6 0 3.80 1.30 26 -6 0 3.35 1.24 -27 -6 0 1.48 1.07 27 -6 0 0.77 0.92 28 -6 0 0.66 0.63 -28 -6 0 1.11 0.84 0 -7 0 5.51 1.46 -1 -7 0 195.35 17.35 1 -7 0 195.67 17.31 2 -7 0 1.49 1.13 3 -7 0 185.35 15.92 -3 7 0 173.32 15.85 4 -7 0 1.72 1.12 -4 7 0 0.90 1.04 5 -7 0 58.05 5.30 -5 7 0 50.82 5.24 6 -7 0 0.58 1.14 -6 7 0 0.85 1.17 -7 -7 0 35.11 3.88 7 -7 0 30.78 3.40 -7 7 0 27.04 3.33 -8 7 0 1.08 1.23 -8 -7 0 1.67 1.66 -9 7 0 1.56 1.41 -9 -7 0 1.57 1.72 9 7 0 0.31 0.77 9 -7 0 1.12 0.79 -10 7 0 0.97 1.31 -10 -7 0 1.48 1.58 10 7 0 -0.74 0.82 10 -7 0 -0.21 0.81 -10 7 0 -0.22 0.69 -11 -7 0 1.63 1.54 -11 7 0 2.46 0.83 11 -7 0 2.74 0.93 -11 7 0 1.30 1.30 11 7 0 3.07 0.98 12 -7 0 0.24 0.86 -12 -7 0 -0.21 0.88 -12 7 0 1.24 0.78 -12 7 0 0.24 1.30 12 7 0 0.24 0.93 13 7 0 43.94 3.94 -13 7 0 31.97 4.55 13 -7 0 38.57 3.89 -13 7 0 41.39 3.82 14 7 0 2.39 1.17 -14 7 0 0.24 0.84 14 -7 0 1.67 1.06 -15 7 0 2.70 1.03 15 -7 0 3.51 1.24 15 7 0 3.01 1.35 16 7 0 0.53 1.35 16 -7 0 0.56 1.16 -16 7 0 -0.56 1.04 17 7 0 0.39 1.57 17 -7 0 1.36 1.36 -17 7 0 0.90 1.13 18 7 0 0.21 1.61 -18 7 0 0.71 1.20 18 -7 0 0.72 1.47 19 7 0 14.98 2.14 19 7 0 13.14 2.37 19 -7 0 20.64 2.38 20 7 0 -1.33 1.79 20 7 0 0.93 1.19 20 -7 0 0.59 1.60 21 -7 0 4.26 1.68 21 7 0 1.81 1.19 22 -7 0 -0.59 1.54 22 7 0 0.23 1.13 23 7 0 -0.14 0.99 23 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2.21 18 8 0 11.83 2.25 19 8 0 0.32 1.67 19 8 0 0.76 1.17 19 -8 0 1.07 1.56 20 8 0 1.32 1.18 20 8 0 0.11 1.77 20 -8 0 2.28 1.62 21 -8 0 0.50 1.54 21 8 0 0.87 1.11 22 -8 0 11.73 1.91 22 8 0 5.35 1.32 23 8 0 1.05 0.94 23 -8 0 1.31 1.47 24 -8 0 8.87 1.67 24 8 0 5.56 1.11 -25 -8 0 -1.21 1.32 25 -8 0 -0.15 1.21 26 -8 0 12.23 1.58 -26 -8 0 8.38 1.60 -27 -8 0 -0.48 0.91 27 -8 0 -0.53 0.80 -28 -8 0 -0.87 0.72 0 -9 0 0.52 1.22 -1 -9 0 56.98 5.65 1 -9 0 56.51 5.59 -2 -9 0 1.28 1.29 2 -9 0 -0.63 1.17 3 -9 0 1.65 1.27 4 -9 0 2.33 1.26 -5 9 0 63.36 6.40 5 -9 0 70.17 6.48 -6 9 0 3.53 1.27 6 -9 0 1.55 1.17 -7 9 0 7.23 1.64 7 9 0 9.84 1.22 7 -9 0 8.65 1.61 8 9 0 1.89 0.85 8 -9 0 1.37 1.09 -8 -9 0 0.79 1.63 -8 9 0 0.86 1.19 9 9 0 4.71 0.98 -9 -9 0 5.08 2.00 -9 9 0 1.71 1.31 -10 9 0 -0.42 1.13 10 -9 0 1.40 0.96 -10 -9 0 0.90 1.50 10 9 0 0.78 0.87 11 9 0 -0.12 0.97 11 -9 0 0.68 0.98 -11 9 0 0.23 1.11 12 -9 0 1.00 1.02 12 9 0 0.54 1.05 -13 -9 0 2.58 1.17 13 9 0 3.39 1.21 13 -9 0 5.31 1.31 14 -9 0 0.56 1.19 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1.51 23 -11 0 48.11 4.71 24 -11 0 0.95 1.17 25 -11 0 6.07 1.34 26 -11 0 0.38 0.81 0 -12 0 650.06 55.57 0 -12 0 619.69 56.09 1 12 0 9.39 1.08 -1 -12 0 8.59 1.84 1 -12 0 9.04 1.81 -1 -12 0 10.17 1.50 1 -12 0 9.49 1.50 2 12 0 85.13 7.60 2 -12 0 85.17 8.25 -2 -12 0 85.70 8.36 2 12 0 87.40 7.68 2 -12 0 82.32 7.79 -2 -12 0 90.67 7.81 3 -12 0 -0.18 1.05 -3 -12 0 -0.64 1.21 3 -12 0 0.86 1.05 3 12 0 1.47 0.57 3 12 0 0.10 0.78 4 12 0 11.38 1.25 -4 -12 0 9.45 2.04 4 12 0 10.87 1.37 4 -12 0 12.29 1.91 4 -12 0 8.76 1.58 -5 -12 0 2.30 1.28 5 -12 0 0.07 1.08 5 12 0 1.30 0.85 6 12 0 58.10 5.41 6 -12 0 60.62 5.55 7 12 0 4.15 1.04 7 -12 0 2.38 1.18 8 12 0 141.17 12.48 9 12 0 -0.13 0.95 10 12 0 4.42 1.22 11 12 0 0.44 1.13 12 12 0 2.35 1.26 13 -12 0 -0.57 1.45 13 12 0 0.84 1.30 14 -12 0 28.15 3.20 -14 -12 0 26.65 3.12 14 12 0 27.52 3.12 15 -12 0 3.11 1.74 -15 -12 0 3.09 1.69 15 12 0 5.43 1.64 -16 -12 0 46.72 4.44 16 12 0 38.45 4.37 16 -12 0 43.38 4.43 -17 -12 0 0.73 1.59 17 12 0 2.42 1.69 17 -12 0 -0.10 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-2 1 -9 7.18 0.92 -2 -1 -9 5.62 0.93 -3 1 -9 2.65 0.73 -3 -1 -9 2.22 0.72 -4 1 -9 8.25 1.09 -4 -1 -9 8.52 1.13 -5 1 -9 3.01 0.76 -5 -1 -9 0.88 0.74 -6 1 -9 10.99 1.19 -6 -1 -9 8.09 1.17 -7 -1 -9 10.68 1.26 -8 -1 -9 3.97 0.80 0 -2 -9 -0.07 0.55 1 -2 -9 0.99 0.50 -1 -2 -9 0.11 0.59 -2 -2 -9 2.37 0.73 -3 -2 -9 12.06 1.37 -4 -2 -9 2.87 0.78 -5 -2 -9 7.64 1.07 -6 -2 -9 3.64 0.81 -7 -2 -9 3.04 0.76 -8 -2 -9 8.08 1.05 0 -3 -9 1.34 0.60 1 -3 -9 1.19 0.55 -1 -3 -9 1.51 0.64 -2 -3 -9 12.05 1.36 -3 -3 -9 4.22 0.85 -4 -3 -9 46.28 4.23 -5 -3 -9 1.57 0.75 -6 -3 -9 17.69 1.82 -7 -3 -9 0.40 0.67 -7 3 -9 1.52 0.53 -8 -3 -9 1.47 0.66 -8 3 -9 0.20 0.47 -9 3 -9 2.46 0.55 -10 -3 -9 24.01 2.26 0 -4 -9 0.10 0.57 1 -4 -9 0.55 0.53 -1 -4 -9 0.84 0.63 -2 -4 -9 -0.11 0.66 -3 -4 -9 1.72 0.72 -4 -4 -9 9.88 1.24 -5 -4 -9 1.99 0.74 -6 -4 -9 0.38 0.68 -6 4 -9 0.58 0.51 -7 -4 -9 2.55 0.75 -7 4 -9 3.07 0.61 -8 -4 -9 5.90 0.97 -8 4 -9 7.40 0.86 -9 4 -9 1.00 0.49 -10 -4 -9 5.46 0.74 -11 -4 -9 1.57 0.42 0 -5 -9 -0.17 0.56 1 -5 -9 4.23 0.75 -1 -5 -9 6.50 0.89 -2 -5 -9 18.79 1.91 -3 -5 -9 5.42 0.94 -4 -5 -9 48.37 4.40 -5 -5 -9 2.98 0.81 -5 5 -9 2.90 0.65 -6 -5 -9 18.04 1.96 -6 5 -9 20.67 1.90 -7 -5 -9 12.42 1.33 -7 5 -9 11.31 1.24 -8 5 -9 1.80 0.53 -9 5 -9 1.26 0.48 -10 -5 -9 10.99 1.15 0 -6 -9 0.60 0.60 1 -6 -9 4.75 0.76 -1 -6 -9 5.70 0.87 -2 -6 -9 5.42 0.89 -3 -6 -9 2.81 0.74 -4 -6 -9 0.73 0.71 -4 6 -9 0.21 0.49 -5 -6 -9 8.76 1.10 -5 6 -9 8.14 0.99 -6 -6 -9 1.15 0.66 -6 6 -9 0.29 0.50 -7 -6 -9 3.29 0.67 -7 6 -9 1.86 0.54 -8 6 -9 0.61 0.47 -10 -6 -9 2.31 0.47 0 -7 -9 -0.10 0.55 1 -7 -9 4.37 0.75 -1 -7 -9 5.80 0.84 -2 -7 -9 31.13 2.91 -3 7 -9 3.35 0.63 -3 -7 -9 4.63 0.78 -4 -7 -9 11.65 1.37 -4 7 -9 12.98 1.30 -5 -7 -9 6.30 0.96 -5 7 -9 6.70 0.83 -6 -7 -9 3.40 0.76 -6 7 -9 3.70 0.63 -7 -7 -9 0.63 0.61 -7 7 -9 0.24 0.45 -8 7 -9 6.00 0.75 -9 -7 -9 1.51 0.45 0 -8 -9 -0.60 0.52 1 -8 -9 1.76 0.49 -1 -8 -9 0.52 0.56 -2 8 -9 0.66 0.42 -2 -8 -9 0.71 0.60 -3 8 -9 1.02 0.48 -3 -8 -9 1.34 0.64 -4 8 -9 1.69 0.49 -4 -8 -9 1.83 0.66 -5 8 -9 1.38 0.49 -5 -8 -9 0.89 0.62 -6 8 -9 8.95 0.96 -6 -8 -9 8.17 1.03 -7 -8 -9 -0.32 0.48 0 -9 -9 0.86 0.47 -1 -9 -9 5.85 0.81 -2 -9 -9 15.57 1.58 -3 -9 -9 6.26 0.85 -4 -9 -9 6.85 0.89 -5 -9 -9 0.76 0.48 -6 -9 -9 0.71 0.50 -7 -9 -9 5.23 0.70 -1 -10 -9 1.99 0.49 -2 -10 -9 0.85 0.46 -3 -10 -9 0.16 0.47 -4 -10 -9 1.62 0.49 -5 -10 -9 0.72 0.43 0 0 0 0.00 0.00 TITL exp_2556 in Pccn REM Pccn (#56, found as Pnaa in -cba setting) CELL 1.54184 23.849659 21.861500 7.914242 90.0000 90.0000 90.0000 ZERR 18.00 0.000883 0.000747 0.000263 0.0000 0.0000 0.0000 LATT 1 SYMM -x+1/2,-y+1/2, z SYMM -x, y+1/2,-z+1/2 SYMM x+1/2,-y,-z+1/2 SFAC C H N O UNIT 198.00 180.00 18.00 18.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 30093 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.301 _oxdiff_exptl_absorpt_empirical_full_min 0.655 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' 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 S1 S 0.30874(5) 0.50304(5) 0.02744(13) 0.0513(4) Uani 1 1 d . . . . . N1 N 0.36833(14) 0.43709(15) 0.3186(4) 0.0386(8) Uani 1 1 d . . . . . C6 C 0.34197(16) 0.39899(18) 0.1988(5) 0.0379(9) Uani 1 1 d . . . . . C14 C 0.31226(16) 0.61798(17) 0.4215(5) 0.0366(8) Uani 1 1 d . U . . . C9 C 0.34490(17) 0.58527(18) 0.5407(5) 0.0394(9) Uani 1 1 d . . . . . C16 C 0.31756(16) 0.53049(17) 0.2318(5) 0.0365(8) Uani 1 1 d . U . . . C15 C 0.29889(16) 0.58867(16) 0.2601(5) 0.0387(8) Uani 1 1 d . U . . . H15 H 0.278111 0.609246 0.178482 0.046 Uiso 1 1 calc R U . . . C17 C 0.40348(16) 0.40987(17) 0.4464(5) 0.0378(9) Uani 1 1 d . . . . . C13 C 0.29749(17) 0.67889(18) 0.4554(5) 0.0407(9) Uani 1 1 d . . . . . H13 H 0.275523 0.700254 0.378261 0.049 Uiso 1 1 calc R U . . . C7 C 0.34943(15) 0.49671(17) 0.3550(5) 0.0362(8) Uani 1 1 d . . . . . C20 C 0.47163(17) 0.36227(19) 0.7041(5) 0.0407(9) Uani 1 1 d . . . . . C1 C 0.31042(16) 0.42347(19) 0.0642(5) 0.0391(9) Uani 1 1 d . . . . . C10 C 0.36066(18) 0.6161(2) 0.6929(5) 0.0442(10) Uani 1 1 d . . . . . H10 H 0.380816 0.595282 0.775344 0.053 Uiso 1 1 calc R U . . . C2 C 0.28357(17) 0.38563(19) -0.0502(5) 0.0435(10) Uani 1 1 d . . . . . H2 H 0.261467 0.402709 -0.134723 0.052 Uiso 1 1 calc R U . . . C8 C 0.36175(16) 0.52510(18) 0.5048(5) 0.0401(9) Uani 1 1 d . . . . . H8 H 0.382066 0.503700 0.585823 0.048 Uiso 1 1 calc R U . . . C21 C 0.41346(17) 0.35825(19) 0.7121(5) 0.0432(10) Uani 1 1 d . . . . . H21 H 0.396943 0.339557 0.805198 0.052 Uiso 1 1 calc R U . . . C22 C 0.37947(18) 0.38133(19) 0.5852(5) 0.0436(10) Uani 1 1 d . . . . . H22 H 0.340702 0.377700 0.593093 0.052 Uiso 1 1 calc R U . . . C18 C 0.46110(17) 0.41468(19) 0.4352(5) 0.0434(10) Uani 1 1 d . . . . . H18 H 0.477409 0.433699 0.342282 0.052 Uiso 1 1 calc R U . . . C19 C 0.49469(18) 0.3910(2) 0.5630(5) 0.0463(10) Uani 1 1 d . . . . . H19 H 0.533451 0.394509 0.554311 0.056 Uiso 1 1 calc R U . . . C12 C 0.31491(18) 0.70732(19) 0.6002(6) 0.0456(10) Uani 1 1 d . . . . . H12 H 0.305523 0.748027 0.619302 0.055 Uiso 1 1 calc R U . . . C5 C 0.34755(18) 0.33530(19) 0.2054(5) 0.0444(10) Uani 1 1 d . . . . . H5 H 0.369141 0.317722 0.290394 0.053 Uiso 1 1 calc R U . . . C11 C 0.34644(19) 0.6758(2) 0.7182(6) 0.0491(11) Uani 1 1 d . . . . . H11 H 0.358076 0.695535 0.816203 0.059 Uiso 1 1 calc R U . . . C23 C 0.50748(17) 0.3372(2) 0.8488(5) 0.0463(10) Uani 1 1 d . . . . . C3 C 0.28915(19) 0.3226(2) -0.0405(6) 0.0491(11) Uani 1 1 d . . . . . H3 H 0.271590 0.297125 -0.118407 0.059 Uiso 1 1 calc R U . . . C4 C 0.32187(19) 0.2985(2) 0.0893(6) 0.0506(11) Uani 1 1 d . . . . . H4 H 0.326328 0.256310 0.097189 0.061 Uiso 1 1 calc R U . . . C25 C 0.5687(2) 0.3346(3) 0.8020(7) 0.0751(17) Uani 1 1 d . . . . . H25A H 0.572995 0.312649 0.697773 0.113 Uiso 1 1 calc R U . . . H25B H 0.589197 0.314123 0.889701 0.113 Uiso 1 1 calc R U . . . H25C H 0.582854 0.375432 0.788754 0.113 Uiso 1 1 calc R U . . . C26 C 0.4992(2) 0.3743(3) 1.0071(7) 0.0680(14) Uani 1 1 d . . . . . H26A H 0.509263 0.416073 0.985773 0.102 Uiso 1 1 calc R U . . . H26B H 0.522394 0.358143 1.095613 0.102 Uiso 1 1 calc R U . . . H26C H 0.460556 0.372254 1.040922 0.102 Uiso 1 1 calc R U . . . C24 C 0.4883(3) 0.2707(2) 0.8858(7) 0.0733(16) Uani 1 1 d . . . . . H24A H 0.450578 0.271086 0.927883 0.110 Uiso 1 1 calc R U . . . H24B H 0.512665 0.252793 0.968832 0.110 Uiso 1 1 calc R U . . . H24C H 0.489901 0.247074 0.783678 0.110 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 S1 0.0734(8) 0.0448(6) 0.0357(6) 0.0011(4) -0.0129(5) 0.0079(5) N1 0.0428(18) 0.0399(18) 0.0331(17) -0.0001(14) -0.0087(14) 0.0057(14) C6 0.037(2) 0.040(2) 0.037(2) 0.0029(17) 0.0065(17) 0.0054(16) C14 0.037(2) 0.0349(19) 0.0380(18) 0.0084(14) 0.0006(15) -0.0030(16) C9 0.041(2) 0.038(2) 0.040(2) 0.0071(17) -0.0043(17) -0.0086(17) C16 0.038(2) 0.0337(16) 0.037(2) 0.0052(16) -0.0035(16) 0.0026(15) C15 0.0334(18) 0.0286(15) 0.054(2) 0.0039(15) -0.0158(17) 0.0004(14) C17 0.040(2) 0.0341(19) 0.039(2) -0.0002(16) -0.0038(17) 0.0024(16) C13 0.046(2) 0.037(2) 0.039(2) 0.0066(17) 0.0047(18) 0.0008(17) C7 0.0312(18) 0.039(2) 0.039(2) 0.0099(17) 0.0008(16) 0.0048(16) C20 0.039(2) 0.045(2) 0.038(2) 0.0036(18) -0.0011(17) 0.0050(17) C1 0.041(2) 0.045(2) 0.031(2) 0.0015(17) -0.0003(16) 0.0034(17) C10 0.047(2) 0.050(2) 0.036(2) 0.0070(19) -0.0079(18) -0.0027(19) C2 0.041(2) 0.051(2) 0.039(2) 0.0043(19) 0.0004(18) -0.0005(19) C8 0.039(2) 0.041(2) 0.041(2) 0.0079(17) -0.0113(17) -0.0035(17) C21 0.044(2) 0.045(2) 0.041(2) 0.0085(18) -0.0006(18) 0.0010(18) C22 0.040(2) 0.044(2) 0.047(2) 0.0026(19) -0.0047(18) 0.0015(18) C18 0.045(2) 0.046(2) 0.039(2) 0.0032(18) 0.0032(18) 0.0005(19) C19 0.038(2) 0.062(3) 0.040(2) 0.007(2) -0.0012(18) 0.0061(19) C12 0.052(2) 0.039(2) 0.046(2) 0.0012(18) 0.007(2) -0.0012(19) C5 0.049(2) 0.043(2) 0.041(2) 0.0025(19) 0.0010(19) 0.0011(19) C11 0.057(3) 0.046(2) 0.045(2) -0.0069(19) -0.002(2) -0.007(2) C23 0.045(2) 0.065(3) 0.029(2) 0.0063(19) -0.0059(17) 0.011(2) C3 0.053(3) 0.045(2) 0.049(2) -0.006(2) 0.002(2) -0.011(2) C4 0.055(3) 0.039(2) 0.059(3) 0.001(2) 0.011(2) -0.003(2) C25 0.052(3) 0.121(5) 0.052(3) 0.026(3) -0.001(2) 0.027(3) C26 0.072(3) 0.078(4) 0.054(3) -0.006(3) -0.010(3) 0.008(3) C24 0.104(4) 0.063(3) 0.053(3) 0.009(3) -0.014(3) 0.005(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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 _geom_angle_publ_flag C16 S1 C1 100.61(18) . . ? C6 N1 C17 119.1(3) . . ? C7 N1 C6 122.8(3) . . ? C7 N1 C17 115.1(3) . . ? N1 C6 C1 121.5(3) . . ? C5 C6 N1 121.3(4) . . ? C5 C6 C1 117.2(4) . . ? C9 C14 C15 118.7(3) . . ? C13 C14 C9 119.3(4) . . ? C13 C14 C15 121.8(3) . . ? C14 C9 C10 117.8(4) . . ? C8 C9 C14 119.7(4) . . ? C8 C9 C10 122.5(4) . . ? C15 C16 S1 115.7(3) . . ? C15 C16 C7 122.6(4) . . ? C7 C16 S1 121.1(3) . . ? C14 C15 H15 120.7 . . ? C16 C15 C14 118.6(3) . . ? C16 C15 H15 120.7 . . ? C22 C17 N1 120.1(4) . . ? C18 C17 N1 120.1(4) . . ? C18 C17 C22 119.7(4) . . ? C14 C13 H13 119.5 . . ? C12 C13 C14 121.0(4) . . ? C12 C13 H13 119.5 . . ? N1 C7 C16 120.3(3) . . ? C8 C7 N1 121.8(3) . . ? C8 C7 C16 117.8(4) . . ? C21 C20 C19 117.3(4) . . ? C21 C20 C23 120.0(4) . . ? C19 C20 C23 122.7(4) . . ? C6 C1 S1 120.7(3) . . ? C2 C1 S1 118.1(3) . . ? C2 C1 C6 121.0(4) . . ? C9 C10 H10 119.7 . . ? C11 C10 C9 120.7(4) . . ? C11 C10 H10 119.7 . . ? C1 C2 H2 119.5 . . ? C1 C2 C3 120.9(4) . . ? C3 C2 H2 119.5 . . ? C9 C8 H8 118.7 . . ? C7 C8 C9 122.5(4) . . ? C7 C8 H8 118.7 . . ? C20 C21 H21 119.1 . . ? C22 C21 C20 121.8(4) . . ? C22 C21 H21 119.1 . . ? C17 C22 H22 120.1 . . ? C21 C22 C17 119.8(4) . . ? C21 C22 H22 120.1 . . ? C17 C18 H18 120.1 . . ? C17 C18 C19 119.9(4) . . ? C19 C18 H18 120.1 . . ? C20 C19 H19 119.2 . . ? C18 C19 C20 121.5(4) . . ? C18 C19 H19 119.2 . . ? C13 C12 H12 119.9 . . ? C13 C12 C11 120.3(4) . . ? C11 C12 H12 119.9 . . ? C6 C5 H5 119.4 . . ? C4 C5 C6 121.2(4) . . ? C4 C5 H5 119.4 . . ? C10 C11 C12 120.9(4) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C20 C23 C24 108.2(4) . . ? C25 C23 C20 111.7(4) . . ? C25 C23 C24 107.3(4) . . ? C26 C23 C20 110.8(4) . . ? C26 C23 C25 110.6(4) . . ? C26 C23 C24 108.0(4) . . ? C2 C3 H3 121.0 . . ? C2 C3 C4 118.0(4) . . ? C4 C3 H3 121.0 . . ? C5 C4 C3 121.6(4) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? 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 S1 C16 1.738(4) . ? S1 C1 1.764(4) . ? N1 C6 1.410(5) . ? N1 C17 1.442(5) . ? N1 C7 1.409(5) . ? C6 C1 1.410(5) . ? C6 C5 1.400(6) . ? C14 C9 1.417(5) . ? C14 C15 1.464(6) . ? C14 C13 1.403(5) . ? C9 C10 1.431(6) . ? C9 C8 1.405(6) . ? C16 C15 1.366(5) . ? C16 C7 1.440(5) . ? C15 H15 0.9300 . ? C17 C22 1.387(6) . ? C17 C18 1.381(6) . ? C13 H13 0.9300 . ? C13 C12 1.368(6) . ? C7 C8 1.370(6) . ? C20 C21 1.392(6) . ? C20 C19 1.394(6) . ? C20 C23 1.531(5) . ? C1 C2 1.384(6) . ? C10 H10 0.9300 . ? C10 C11 1.361(6) . ? C2 H2 0.9300 . ? C2 C3 1.387(6) . ? C8 H8 0.9300 . ? C21 H21 0.9300 . ? C21 C22 1.386(6) . ? C22 H22 0.9300 . ? C18 H18 0.9300 . ? C18 C19 1.390(6) . ? C19 H19 0.9300 . ? C12 H12 0.9300 . ? C12 C11 1.384(6) . ? C5 H5 0.9300 . ? C5 C4 1.367(6) . ? C11 H11 0.9300 . ? C23 C25 1.507(6) . ? C23 C26 1.506(7) . ? C23 C24 1.551(7) . ? C3 H3 0.9300 . ? C3 C4 1.394(7) . ? C4 H4 0.9300 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? 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 S1 C16 C15 C14 -171.2(3) . . . . ? S1 C16 C7 N1 -7.9(5) . . . . ? S1 C16 C7 C8 170.4(3) . . . . ? S1 C1 C2 C3 171.9(3) . . . . ? N1 C6 C1 S1 6.7(5) . . . . ? N1 C6 C1 C2 -178.4(4) . . . . ? N1 C6 C5 C4 179.9(4) . . . . ? N1 C17 C22 C21 -176.5(4) . . . . ? N1 C17 C18 C19 176.8(4) . . . . ? N1 C7 C8 C9 177.7(4) . . . . ? C6 N1 C17 C22 -77.7(5) . . . . ? C6 N1 C17 C18 105.4(4) . . . . ? C6 N1 C7 C16 -24.4(5) . . . . ? C6 N1 C7 C8 157.4(4) . . . . ? C6 C1 C2 C3 -3.2(6) . . . . ? C6 C5 C4 C3 0.1(7) . . . . ? C14 C9 C10 C11 -2.5(6) . . . . ? C14 C9 C8 C7 2.2(6) . . . . ? C14 C13 C12 C11 -1.6(6) . . . . ? C9 C14 C15 C16 1.1(5) . . . . ? C9 C14 C13 C12 1.1(6) . . . . ? C9 C10 C11 C12 2.1(7) . . . . ? C16 S1 C1 C6 -30.1(4) . . . . ? C16 S1 C1 C2 154.8(3) . . . . ? C16 C7 C8 C9 -0.5(6) . . . . ? C15 C14 C9 C10 175.9(4) . . . . ? C15 C14 C9 C8 -2.5(5) . . . . ? C15 C14 C13 C12 -173.7(4) . . . . ? C15 C16 C7 N1 -179.1(4) . . . . ? C15 C16 C7 C8 -0.9(6) . . . . ? C17 N1 C6 C1 -175.5(3) . . . . ? C17 N1 C6 C5 2.4(6) . . . . ? C17 N1 C7 C16 175.3(3) . . . . ? C17 N1 C7 C8 -2.8(5) . . . . ? C17 C18 C19 C20 0.0(7) . . . . ? C13 C14 C9 C10 0.9(6) . . . . ? C13 C14 C9 C8 -177.5(4) . . . . ? C13 C14 C15 C16 176.0(4) . . . . ? C13 C12 C11 C10 0.0(7) . . . . ? C7 N1 C6 C1 25.0(6) . . . . ? C7 N1 C6 C5 -157.1(4) . . . . ? C7 N1 C17 C22 83.4(4) . . . . ? C7 N1 C17 C18 -93.5(4) . . . . ? C7 C16 C15 C14 0.5(6) . . . . ? C20 C21 C22 C17 -0.6(6) . . . . ? C1 S1 C16 C15 -157.6(3) . . . . ? C1 S1 C16 C7 30.6(4) . . . . ? C1 C6 C5 C4 -2.1(6) . . . . ? C1 C2 C3 C4 1.0(6) . . . . ? C10 C9 C8 C7 -176.2(4) . . . . ? C2 C3 C4 C5 0.5(7) . . . . ? C8 C9 C10 C11 175.8(4) . . . . ? C21 C20 C19 C18 -0.2(7) . . . . ? C21 C20 C23 C25 168.9(5) . . . . ? C21 C20 C23 C26 -67.2(6) . . . . ? C21 C20 C23 C24 51.0(5) . . . . ? C22 C17 C18 C19 -0.1(6) . . . . ? C18 C17 C22 C21 0.4(6) . . . . ? C19 C20 C21 C22 0.5(6) . . . . ? C19 C20 C23 C25 -12.8(6) . . . . ? C19 C20 C23 C26 111.1(5) . . . . ? C19 C20 C23 C24 -130.7(5) . . . . ? C5 C6 C1 S1 -171.3(3) . . . . ? C5 C6 C1 C2 3.7(6) . . . . ? C23 C20 C21 C22 178.9(4) . . . . ? C23 C20 C19 C18 -178.5(4) . . . . ?