#------------------------------------------------------------------------------ #$Date: 2019-11-24 08:06:04 +0200 (Sun, 24 Nov 2019) $ #$Revision: 237235 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/08/80/4088056.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_4088056 loop_ _publ_author_name '\'Alvarez-Rodr\'iguez, Luc\'ia' 'Cabeza, Javier A.' 'Garc\'ia-\'Alvarez, Pablo' 'Polo, Diego' _publ_section_title ; Amidinatogermylene Complexes of Copper, Silver, and Gold ; _journal_issue 22 _journal_name_full Organometallics _journal_page_first 5479 _journal_paper_doi 10.1021/acs.organomet.5b00828 _journal_volume 34 _journal_year 2015 _chemical_formula_moiety 'C15 H25 Cl N2' _chemical_formula_sum 'C15 H25 Cl N2' _chemical_formula_weight 268.82 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2014 _cell_angle_alpha 90 _cell_angle_beta 111.803(4) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 8.5679(3) _cell_length_b 10.9211(2) _cell_length_c 9.1349(3) _cell_measurement_reflns_used 2213 _cell_measurement_temperature 153(2) _cell_measurement_theta_max 69.2000 _cell_measurement_theta_min 5.2050 _cell_volume 793.62(5) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_molecular_graphics 'X-SEED (Barbour, 1999)' _computing_publication_material 'SHELXL-2014 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_structure_solution 'SIR-97 (Giacovazzo, 1999)' _diffrn_ambient_temperature 153(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.980 _diffrn_measurement_device_type 'Xcalibur, Onyx, Nova' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.5418 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_unetI/netI 0.0344 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.980 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 3766 _diffrn_reflns_point_group_measured_fraction_full 0.739 _diffrn_reflns_point_group_measured_fraction_max 0.724 _diffrn_reflns_theta_full 67.680 _diffrn_reflns_theta_max 69.492 _diffrn_reflns_theta_min 5.215 _diffrn_source 'sealed X-ray tube' _exptl_absorpt_coefficient_mu 2.004 _exptl_absorpt_correction_T_max 0.952 _exptl_absorpt_correction_T_min 0.831 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.125 _exptl_crystal_description fragment _exptl_crystal_F_000 292 _exptl_crystal_size_max 0.1396 _exptl_crystal_size_mid 0.1160 _exptl_crystal_size_min 0.0232 _refine_diff_density_max 0.150 _refine_diff_density_min -0.190 _refine_diff_density_rms 0.037 _refine_ls_abs_structure_details ; Flack x determined using 558 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.04(2) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 177 _refine_ls_number_reflns 2158 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.041 _refine_ls_R_factor_all 0.0368 _refine_ls_R_factor_gt 0.0323 _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^)+(0.0449P)^2^+0.1087P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0815 _refine_ls_wR_factor_ref 0.0864 _reflns_Friedel_coverage 0.399 _reflns_Friedel_fraction_full 0.453 _reflns_Friedel_fraction_max 0.438 _reflns_number_gt 1979 _reflns_number_total 2158 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file om5b00828_si_002.cif _cod_data_source_block 15069_lu301 _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 4088056 _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. ; _shelxl_version_number 2014-3 _shelx_res_file ; TITL 15069_lu301 in P21 CELL 1.54180 8.5679 10.9211 9.1349 90.000 111.803 90.000 ZERR 2.00 0.0003 0.0002 0.0003 0.000 0.004 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H CL N UNIT 30 50 2 4 MERG 2 OMIT -3.00 180.00 FMAP 2 PLAN 20 ACTA BOND BOND $H L.S. 32 TEMP -120.00 WGHT 0.044900 0.108700 FVAR 9.00524 C1 1 0.911000 -0.240903 0.014690 11.00000 0.09418 0.03854 = 0.06138 0.00348 0.05577 0.00986 AFIX 137 H1A 2 0.800920 -0.277752 -0.043123 11.00000 -1.50000 H1B 2 0.974663 -0.293648 0.103645 11.00000 -1.50000 H1C 2 0.972858 -0.232043 -0.055931 11.00000 -1.50000 AFIX 0 C2 1 0.802346 -0.030306 -0.062502 11.00000 0.06173 0.05261 = 0.04830 0.01691 0.02977 0.01374 AFIX 137 H2A 2 0.784536 0.049814 -0.022948 11.00000 -1.50000 H2B 2 0.693786 -0.064853 -0.129746 11.00000 -1.50000 H2C 2 0.874139 -0.020801 -0.123928 11.00000 -1.50000 AFIX 0 C3 1 1.051695 -0.061576 0.182474 11.00000 0.04563 0.07538 = 0.05939 -0.00408 0.02145 0.00125 AFIX 137 H3A 2 1.103737 -0.115555 0.273340 11.00000 -1.50000 H3B 2 1.031603 0.019062 0.219166 11.00000 -1.50000 H3C 2 1.126859 -0.052942 0.124289 11.00000 -1.50000 AFIX 0 C10 1 0.721198 -0.534447 0.170670 11.00000 0.05319 0.03074 = 0.06373 -0.00930 0.02894 -0.00372 AFIX 43 H10 2 0.648282 -0.592591 0.101095 11.00000 -1.20000 AFIX 0 C15 1 0.688412 -0.293287 0.564188 11.00000 0.04580 0.04553 = 0.04351 0.01002 0.02049 0.00071 AFIX 137 H15A 2 0.789000 -0.244027 0.618408 11.00000 -1.50000 H15B 2 0.719743 -0.366593 0.519569 11.00000 -1.50000 H15C 2 0.637188 -0.317644 0.639464 11.00000 -1.50000 AFIX 0 H100 2 0.742614 -0.043371 0.173916 11.00000 0.02852 H200 2 0.627408 -0.075443 0.326858 11.00000 0.03348 MOLE 1 C4 1 0.887079 -0.115815 0.075858 11.00000 0.04525 0.03392 = 0.03597 0.00544 0.02137 0.00626 C5 1 0.733323 -0.196199 0.252598 11.00000 0.02999 0.02840 = 0.02687 0.00008 0.00728 -0.00252 C6 1 0.783178 -0.327597 0.260245 11.00000 0.03553 0.02825 = 0.03018 0.00199 0.01501 0.00230 C7 1 0.935112 -0.365665 0.374614 11.00000 0.03968 0.04047 = 0.03322 0.00337 0.01417 0.00487 AFIX 43 H7 2 1.008948 -0.307689 0.443657 11.00000 -1.20000 AFIX 0 C8 1 0.977278 -0.488678 0.386561 11.00000 0.05091 0.04327 = 0.04491 0.01522 0.02482 0.01711 AFIX 43 H8 2 1.080291 -0.515403 0.464244 11.00000 -1.20000 AFIX 0 C9 1 0.869892 -0.572345 0.285824 11.00000 0.06591 0.02866 = 0.06879 0.00972 0.04210 0.01295 AFIX 43 H9 2 0.898441 -0.656811 0.295719 11.00000 -1.20000 AFIX 0 C11 1 0.678404 -0.411242 0.156711 11.00000 0.03945 0.03299 = 0.04074 -0.00591 0.01548 0.00018 AFIX 43 H11 2 0.577346 -0.384595 0.076169 11.00000 -1.20000 AFIX 0 C12 1 0.563265 -0.218223 0.432557 11.00000 0.03943 0.02535 = 0.03649 -0.00183 0.01885 -0.00304 C13 1 0.418634 -0.297582 0.330677 11.00000 0.04384 0.03194 = 0.04917 -0.00552 0.01889 -0.00628 AFIX 137 H13A 2 0.463006 -0.369908 0.295744 11.00000 -1.50000 H13B 2 0.347712 -0.250676 0.238517 11.00000 -1.50000 H13C 2 0.351647 -0.323485 0.391883 11.00000 -1.50000 AFIX 0 C14 1 0.497395 -0.114249 0.504348 11.00000 0.05704 0.03211 = 0.05161 -0.00470 0.03285 -0.00395 AFIX 137 H14A 2 0.416619 -0.065488 0.419970 11.00000 -1.50000 H14B 2 0.591307 -0.062098 0.567617 11.00000 -1.50000 H14C 2 0.441812 -0.148162 0.571717 11.00000 -1.50000 AFIX 0 CL1 3 0.643584 0.131371 0.252252 11.00000 0.06237 0.02621 = 0.05315 0.00030 0.02736 0.00392 N1 4 0.772482 -0.115436 0.164581 11.00000 0.05651 0.02554 = 0.04590 0.00539 0.03067 0.00713 N2 4 0.644467 -0.155024 0.333734 11.00000 0.04583 0.02228 = 0.03927 -0.00019 0.02331 -0.00070 HKLF 4 REM 15069_lu301 in P21 REM R1 = 0.0323 for 1979 Fo > 4sig(Fo) and 0.0368 for all 2158 data REM 177 parameters refined using 1 restraints END WGHT 0.0445 0.1119 REM Highest difference peak 0.150, deepest hole -0.190, 1-sigma level 0.037 Q1 1 0.7292 0.1269 0.1964 11.00000 0.05 0.15 Q2 1 0.8472 -0.7203 0.3176 11.00000 0.05 0.13 Q3 1 0.5033 0.0507 0.1613 11.00000 0.05 0.13 Q4 1 0.4957 0.0784 0.2369 11.00000 0.05 0.13 Q5 1 0.3847 -0.3793 -0.0231 11.00000 0.05 0.13 Q6 1 0.5266 0.2175 0.1487 11.00000 0.05 0.12 Q7 1 0.7709 0.0412 0.3435 11.00000 0.05 0.12 Q8 1 0.2054 -0.3174 0.4175 11.00000 0.05 0.12 Q9 1 0.4889 0.1789 0.2489 11.00000 0.05 0.12 Q10 1 0.4262 -0.0460 0.7147 11.00000 0.05 0.11 Q11 1 0.2804 -0.3683 0.4973 11.00000 0.05 0.11 Q12 1 0.4740 -0.4922 0.2831 11.00000 0.05 0.11 Q13 1 0.7254 -0.0513 0.4210 11.00000 0.05 0.11 Q14 1 0.8291 -0.7637 0.1772 11.00000 0.05 0.11 Q15 1 0.3224 -0.1857 0.6345 11.00000 0.05 0.11 Q16 1 0.3535 -0.1159 0.6429 11.00000 0.05 0.11 Q17 1 0.5051 -0.0515 -0.2204 11.00000 0.05 0.11 Q18 1 0.5203 -0.3567 0.5900 11.00000 0.05 0.11 Q19 1 0.8989 -0.0920 -0.2357 11.00000 0.05 0.11 Q20 1 0.9257 0.0759 0.3061 11.00000 0.05 0.11 ; _shelx_res_checksum 94207 _shelx_hkl_file ; 0 -13 0-7.87441 102.880 15 0 -13 1 5380.06 266.588 15 0 -12 0 11702.8 476.636 15 0 -12 -1 926.902 188.755 15 0 -12 1 1017.10 146.776 10 0 -12 1 974.143 182.312 15 0 -12 -2 1409.14 189.797 15 0 -12 2 1097.64 162.188 15 0 -12 -3 2624.95 237.863 11 0 -12 3 2146.85 183.907 15 0 -12 -4 1771.01 177.653 11 0 -11 0 7.75553 145.641 15 0 -11 1 10111.8 500.076 15 0 -11 -1 10293.3 518.853 11 0 -11 -1 10754.2 514.549 15 0 -11 -2 234.401 176.213 11 0 -11 -2 147.510 154.505 15 0 -11 2 132.660 134.809 15 0 -11 3 3509.34 287.620 15 0 -11 -3 3740.38 323.759 11 0 -11 -3 4018.80 293.041 15 0 -11 -4-1.55394 110.182 11 0 -11 4 112.984 42.0048 15 0 -11 -5 3159.61 249.567 11 0 -10 0 680.354 192.856 15 0 -10 0 611.678 190.689 11 0 -10 -1 4088.60 366.768 11 0 -10 -1 4051.73 349.364 15 0 -10 -2 17089.9 709.311 11 0 -10 -2 16741.3 703.887 13 0 -10 -2 16493.2 632.270 15 0 -10 -3 7445.59 477.580 11 0 -10 -3 7199.15 457.552 13 0 -10 -3 7621.29 423.956 15 0 -10 -4 3208.30 306.930 13 0 -10 -4 3021.59 325.749 11 0 -10 -5 24.8762 133.284 11 0 -10 -5-180.699 126.080 13 0 -10 -6 2621.94 232.497 11 0 -9 0-54.9667 125.567 11 0 -9 1 22565.0 732.374 14 0 -9 1 22231.9 701.509 11 0 -9 -1 21851.2 721.576 15 0 -9 -1 21241.3 788.255 13 0 -9 -1 21937.4 758.031 11 0 -9 2 5792.91 394.575 14 0 -9 -2 6311.53 448.360 11 0 -9 -2 6232.49 450.871 13 0 -9 -2 6702.92 418.350 15 0 -9 -3 13935.4 660.799 11 0 -9 -3 13945.5 557.853 15 0 -9 3 14686.6 578.069 14 0 -9 -3 14515.3 664.878 13 0 -9 -4 762.230 209.167 11 0 -9 4 970.362 161.657 14 0 -9 -4 752.910 176.367 13 0 -9 -5 13730.0 600.405 13 0 -9 -5 15124.8 639.628 11 0 -9 -6 710.902 159.226 11 0 -9 -6 586.648 152.864 13 0 -9 -7 1022.48 148.779 11 0 -8 0 16888.3 610.078 11 0 -8 0 17446.3 667.115 13 0 -8 0 17901.4 617.942 14 0 -8 -1 2010.60 205.187 8 0 -8 1 2040.16 251.303 14 0 -8 -1 1709.71 246.051 13 0 -8 -1 1958.86 252.674 11 0 -8 1 2073.27 228.904 11 0 -8 2 75.4049 126.889 14 0 -8 -2-0.70584 108.705 8 0 -8 -2 48.7827 125.517 15 0 -8 -2 199.731 158.764 11 0 -8 -2 40.1489 136.875 13 0 -8 -3 63.3269 112.515 13 0 -8 3 24.9379 127.114 14 0 -8 -3 5.14445 143.791 15 0 -8 -3 44.7414 162.913 11 0 -8 -4 8493.14 517.399 11 0 -8 4 8960.36 438.767 14 0 -8 -4 8962.71 439.035 15 0 -8 -5 622.578 202.819 11 0 -8 -6 7103.24 446.579 11 0 -8 -7 879.128 158.014 11 0 -7 0-38.8171 109.577 11 0 -7 0-82.1175 128.019 13 0 -7 0 15.6544 105.763 14 0 -7 -1 16542.2 576.075 11 0 -7 -1 16604.8 601.924 13 0 -7 1 16747.5 556.835 14 0 -7 -1 16717.6 546.024 14 0 -7 -1 15141.4 479.567 8 0 -7 1 16899.3 878.552 2 0 -7 1 15352.9 517.137 11 0 -7 -2 22694.8 618.012 8 0 -7 2 24614.2 682.182 14 0 -7 -2 23471.6 644.205 15 0 -7 -2 23950.4 729.489 11 0 -7 -3 52432.7 1130.72 11 0 -7 3 49703.7 983.173 14 0 -7 -3 51640.7 978.327 8 0 -7 -3 51202.1 936.593 15 0 -7 -4 11170.8 457.205 15 0 -7 -4 11482.7 570.077 11 0 -7 4 11760.3 486.703 14 0 -7 -5 5138.30 416.161 11 0 -7 -6 1694.24 261.801 11 0 -7 -7 5518.14 378.200 11 0 -6 1 18264.5 820.013 2 0 -6 -1 18777.5 554.284 11 0 -6 -1 18758.2 529.122 14 0 -6 -2 46196.2 805.327 8 0 -6 -2 46541.8 916.875 11 0 -6 2 45973.0 1357.85 2 0 -6 -3 10843.1 486.212 11 0 -6 3 10461.0 730.255 2 0 -6 -3 10216.5 393.876 15 0 -6 -3 10497.6 424.353 8 0 -6 -4 14643.0 610.459 11 0 -6 -4 14455.1 475.644 15 0 -6 4 15675.6 938.346 2 0 -6 -5 2567.67 298.808 11 0 -6 -6 14524.9 637.515 11 0 -6 -7 1498.24 241.645 11 0 -5 0-123.871 150.002 2 0 -5 1 23103.4 830.378 2 0 -5 2 6576.17 488.803 2 0 -5 -3 15710.5 479.297 8 0 -5 3 15772.4 812.877 2 0 -5 -4 14637.5 501.185 8 0 -5 4 12818.9 466.668 16 0 -5 4 15375.3 896.407 2 0 -5 -4 13137.7 415.792 15 0 -5 5 10593.4 878.939 2 0 -5 5 9521.08 439.374 16 0 -5 -6 1750.72 259.585 11 0 -4 0 174993. 1918.39 2 0 -4 1 2197.32 252.963 2 0 -4 2 89997.2 1557.18 2 0 -4 3 6632.75 512.585 2 0 -4 -4 8833.48 362.431 8 0 -4 4 7896.23 641.163 2 0 -4 4 7836.61 353.427 16 0 -4 5 11203.9 467.457 16 0 -4 5 11311.9 905.251 2 0 -4 -5 11292.7 403.040 7 0 -4 6 939.943 183.521 16 0 -4 6 1351.37 495.954 2 0 -4 -6 1074.22 173.651 7 0 -4 -7 1793.18 224.077 7 0 -4 -8 5820.92 331.245 7 0 -3 0 9.54398 108.311 2 0 -3 1 111596. 1360.70 2 0 -3 2 18565.8 652.788 2 0 -3 3 46880.5 1202.26 2 0 -3 4 8107.38 620.174 2 0 -3 5 48502.1 1694.71 2 0 -3 5 50827.2 944.001 16 0 -3 -5 48417.8 799.459 7 0 -3 -6 2063.06 207.792 7 0 -3 6 1859.22 239.646 16 0 -3 -7 4221.36 318.020 7 0 -3 7 4421.49 802.183 2 0 -3 -8 179.145 118.726 7 0 -3 -9 1694.05 177.514 7 0 -2 0 8677.22 308.347 2 0 -2 1 61717.8 867.651 2 0 -2 2 45229.3 908.568 2 0 -2 3 55055.2 1208.91 2 0 -2 4 25480.9 993.694 2 0 -2 5 4233.94 553.329 2 0 -2 5 4022.54 278.514 16 0 -2 6 19703.6 649.587 16 0 -2 -6 19605.5 585.942 7 0 -2 6 19485.8 1262.89 2 0 -2 7 2802.41 303.336 16 0 -2 -7 3111.48 271.534 7 0 -2 -8 10786.3 485.609 7 0 -2 -9 4252.09 288.993 7 0 -1 0 21.3731 39.7995 2 0 -1 1 93582.2 875.046 2 0 -1 2 8047.09 350.058 3 0 -1 3 60700.9 1165.36 3 0 -1 4 5152.82 456.182 3 0 -1 5 23965.8 1127.00 2 0 -1 5 21852.7 597.398 16 0 -1 6 1331.59 197.129 16 0 -1 6 1155.35 419.312 2 0 -1 -7 3077.01 280.308 7 0 -1 7 2338.11 279.839 16 0 -1 7 2336.04 595.086 2 0 -1 -8 999.006 196.747 7 0 -1 -9 93.3794 123.524 7 0 -1 -10 494.401 103.685 7 0 0 1 9012.26 235.966 3 0 0 2 107391. 503.989 1 0 0 2 111767. 1186.23 3 0 0 3 60.1859 139.697 3 0 0 4 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4084.15 519.535 1 5 2 1 3908.93 286.872 6 5 2 1 4118.43 553.985 1 5 2 2 8139.35 419.616 6 5 2 2 6712.72 688.533 1 5 2 3 9595.55 496.422 16 5 2 3 9511.65 465.602 6 5 2 4 8658.40 475.672 16 5 2 5 6050.21 366.789 16 -5 3 10 500.618 147.440 5 -5 3 9-48.6111 158.361 5 -5 3 8 9131.61 505.571 5 -5 3 7 1276.52 225.570 5 -5 3 6 14045.0 561.541 5 -5 3 5 4764.85 324.835 5 5 3 -4 8186.62 645.026 1 -5 3 4 7203.13 363.009 5 -5 3 3 1464.94 186.268 5 5 3 0 1883.58 334.222 4 5 3 1 1194.09 280.018 4 5 3 2 5339.71 362.476 16 5 3 2 5097.74 600.903 1 5 3 3 8938.68 459.220 16 -5 4 10 602.461 128.197 5 -5 4 9 5500.20 358.607 5 -5 4 8 940.671 203.471 5 -5 4 7 2207.55 275.818 5 -5 4 6 205.760 144.662 5 -5 4 5 33664.0 818.581 5 -5 4 4 5737.82 336.261 5 5 4 0 1330.95 287.667 4 5 4 1 6332.52 628.597 4 5 4 2 2372.96 514.325 1 -5 5 10 1380.60 165.294 5 -5 5 9 914.059 178.913 5 -5 5 8 5118.08 365.051 5 -5 5 7 1222.52 214.207 5 -5 5 6 6617.53 398.342 5 -5 5 5 2655.44 256.353 5 5 5 0 8518.17 731.551 4 5 5 1 3294.97 501.147 4 5 5 2 11672.7 970.456 4 -5 6 9 1365.06 177.674 5 -5 6 8 135.492 117.203 5 -5 6 7 6868.65 390.901 5 -5 6 6 9543.96 460.036 5 5 6 -1 1361.93 356.025 4 5 6 0 4426.03 603.438 4 5 6 1 2135.81 519.221 4 -5 7 8 4692.29 264.015 5 -5 7 7 505.509 135.546 5 5 7 -1 6568.46 727.533 4 5 7 0 34482.3 1614.37 4 -6 -10 5 971.799 142.251 14 -6 -10 4 659.546 129.951 14 6 -10 -4 859.370 143.879 10 -6 -10 3 500.376 111.255 8 -6 -10 3 1006.30 152.572 14 6 -10 -2 1636.96 193.920 10 -6 -10 2 1466.54 162.169 8 -6 -10 1 819.405 137.267 8 -6 -10 0 1250.10 145.217 8 -6 -9 7-135.419 77.7645 14 -6 -9 6 628.109 150.637 14 -6 -9 5 623.159 150.194 14 -6 -9 4 4684.61 312.340 14 -6 -9 4 3847.64 290.815 8 -6 -9 3 2590.67 243.132 14 6 -9 -3 3353.47 264.180 10 -6 -9 3 3013.29 273.801 8 6 -9 -2 2501.76 256.950 10 -6 -9 2 1878.90 248.395 8 -6 -9 1 48.4591 128.380 8 6 -9 -1 109.071 182.853 10 -6 -9 0 98.2691 104.330 8 -6 -9 -1 455.707 99.4520 8 -6 -9 -2 2510.37 181.577 8 -6 -8 8 11.6024 67.5137 14 6 -8 -7 215.948 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3 2496.94 263.633 5 7 3 -3 2255.23 483.130 1 7 3 -2 6.39961 130.273 12 7 3 -2 127.391 295.406 1 7 3 -1 1828.95 510.165 1 7 3 1 702.715 178.245 16 -7 4 9-174.899 116.390 5 -7 4 8 4637.97 331.573 5 -7 4 7 1516.32 231.182 5 -7 4 6 4169.96 330.520 5 -7 4 5 991.248 191.571 5 -7 4 4 6776.27 397.969 5 -7 5 9 1720.23 182.608 5 -7 5 8 1634.28 201.470 5 -7 5 7 2894.06 260.991 5 -7 5 6 165.039 136.615 5 -8 -8 4 48.3369 88.6417 8 -8 -8 3 2754.64 202.615 8 -8 -8 2 728.713 133.033 8 -8 -8 1 484.998 101.458 8 -8 -7 6 236.858 73.6447 14 8 -7 -5 2684.18 201.772 12 8 -7 -4 667.397 128.253 12 8 -7 -3 161.676 111.863 6 -8 -7 2 207.502 123.279 8 8 -7 -2 284.530 109.085 6 8 -7 -1 2682.05 210.233 6 -8 -7 1 3207.50 230.209 8 -8 -7 0 1346.94 158.437 8 8 -6 -7 242.270 101.977 12 8 -6 -6 1188.40 164.949 12 8 -6 -5 3174.54 260.593 12 8 -6 -4 2190.28 226.956 12 8 -6 -3 2199.67 227.239 12 8 -6 -2 4964.59 335.495 6 -8 -6 1 170.424 114.814 8 8 -6 -1 195.551 118.673 6 -8 -6 0 64.2934 93.3201 8 8 -6 0-38.9826 24.2025 16 8 -6 1 70.6095 72.2566 6 -8 -5 7 3394.81 233.723 5 -8 -5 6 1768.14 213.390 5 8 -5 -6 2117.29 225.169 12 -8 -5 5 1585.26 218.003 5 8 -5 -5 1715.76 221.436 12 8 -5 -4 9672.39 469.537 12 8 -5 -3 855.625 189.564 12 8 -5 -2 2619.48 261.018 12 8 -5 -1 396.387 146.929 16 8 -5 -1 456.133 152.689 6 8 -5 0 1497.03 206.696 16 8 -5 0 1737.93 219.586 6 -8 -5 0 1369.05 194.784 8 8 -5 1 457.719 137.189 16 8 -5 1 678.771 135.568 6 8 -4 -8 27.0969 101.974 9 -8 -4 8-272.148 98.4252 5 8 -4 -7 1374.27 203.598 9 -8 -4 7 1386.90 200.076 5 8 -4 -6 740.678 195.076 9 -8 -4 6 576.928 178.435 5 8 -4 -5 539.804 185.078 12 -8 -4 5 469.937 185.083 5 -8 -4 4 1947.24 253.578 5 8 -4 -4 1945.87 256.940 12 8 -4 -3 3402.44 324.880 12 8 -4 -2 181.468 146.111 12 8 -4 -1 6691.27 426.955 6 -8 -4 0 2292.99 232.166 8 8 -4 0 2418.94 266.715 16 8 -4 1 2779.73 257.187 16 8 -4 1 3834.87 288.494 6 8 -4 2 95.3329 106.839 16 8 -4 2 285.177 122.101 6 8 -3 -9-20.0188 106.791 9 8 -3 -8 584.149 162.445 9 -8 -3 8 544.114 155.620 5 -8 -3 7 2041.94 243.241 5 8 -3 -7 2030.46 249.047 9 8 -3 -6 767.185 203.123 9 -8 -3 6 419.309 187.859 5 8 -3 -5 560.542 169.318 12 8 -3 -5 350.611 178.384 9 -8 -3 5 140.605 181.208 5 -8 -3 4 5267.04 391.560 5 8 -3 -4 5471.97 396.062 12 -8 -3 3 10772.3 530.624 5 8 -3 -3 10773.2 540.744 12 8 -3 -2-19.6420 142.149 12 8 -3 -1 6133.85 426.004 6 8 -3 0 422.500 174.763 6 8 -3 1 2162.04 264.461 16 8 -3 1 2520.53 256.316 6 8 -3 2 1.89215 96.5026 16 8 -3 2 64.5992 95.5935 6 8 -3 3 262.993 86.5077 16 -8 -2 9 5221.02 281.841 5 8 -2 -9 5244.50 299.375 9 8 -2 -8 987.815 183.379 9 -8 -2 8 1139.14 197.916 5 -8 -2 7 3080.62 310.877 5 8 -2 -7 3139.22 297.647 9 -8 -2 6 6503.22 435.118 5 8 -2 -6 6061.73 411.692 9 -8 -2 5 12875.3 603.973 5 8 -2 -5 12339.7 557.578 12 8 -2 -5 12180.9 578.084 9 -8 -2 4 2843.72 321.530 5 8 -2 -4 2671.61 299.956 12 -8 -2 3 6535.67 419.434 5 8 -2 -3 6784.11 445.448 12 8 -2 -2 2325.19 291.047 12 8 -2 -1 7849.91 480.589 6 8 -2 -1 7946.29 469.791 12 8 -2 0 1809.04 251.158 6 8 -2 1 1083.06 212.921 16 8 -2 1 1251.45 214.055 6 8 -2 2 79.0421 104.934 16 8 -2 2 114.046 107.282 6 8 -2 3 868.444 135.792 16 -8 -1 9 3243.20 258.447 5 8 -1 -9 3481.22 250.586 9 8 -1 -8 436.382 154.946 9 -8 -1 8 366.479 181.444 5 8 -1 -7 156.937 153.596 9 -8 -1 7 125.321 165.902 5 -8 -1 6 5984.55 429.037 5 8 -1 -6 5780.61 396.852 9 8 -1 -5 46.5572 146.546 12 8 -1 -5-22.1370 157.732 9 -8 -1 5-20.6511 189.042 5 -8 -1 4 4157.64 376.048 5 8 -1 -4 4356.35 359.600 12 8 -1 -3 9.32084 152.494 12 -8 -1 3 26.5822 155.060 5 -8 -1 2 1866.63 268.398 5 8 -1 -2 2110.23 281.723 12 8 -1 -1 1578.42 249.031 6 8 -1 0 3197.78 316.563 6 8 -1 1 1339.03 233.348 16 8 -1 1 1476.55 216.004 6 8 -1 2 173.513 130.543 16 8 -1 2 215.929 106.736 6 8 -1 3 166.438 96.2363 16 8 0 -9-0.53541 97.3599 9 -8 0 9 79.3976 108.736 5 -8 0 8 3705.54 329.171 5 8 0 -8 4171.40 299.206 9 8 0 -7 619.267 184.543 9 -8 0 7 727.878 220.740 5 8 0 -6 1427.59 225.148 9 -8 0 6 1517.48 254.191 5 8 0 -5 2430.87 273.690 12 -8 0 5 2647.63 306.817 5 8 0 -5 2227.25 274.245 9 -8 0 4 9687.71 521.376 5 8 0 -4 10195.7 504.998 12 8 0 -3 1497.86 242.863 12 -8 0 3 1390.42 252.468 5 -8 0 2 2636.12 282.851 5 8 0 -2 2717.90 290.274 12 8 0 -1 5626.20 395.214 6 8 0 0-17.8503 127.150 6 8 0 1 1659.88 248.418 16 8 0 1 1677.65 212.915 6 8 0 2 800.928 170.406 16 8 0 3 683.230 132.793 16 -8 1 9 3652.32 257.470 5 8 1 -9 2689.09 229.961 9 8 1 -8 220.484 80.4896 12 8 1 -8 567.396 157.781 9 -8 1 8 554.634 180.949 5 8 1 -7 230.430 130.267 12 8 1 -7 174.374 133.631 9 -8 1 7 108.727 158.455 5 8 1 -6 6852.71 385.020 12 -8 1 6 6373.96 427.630 5 8 1 -6 6711.77 405.260 9 8 1 -5 64.5522 131.295 12 8 1 -5 154.073 142.406 9 -8 1 5 251.858 183.981 5 8 1 -4 5117.55 365.963 12 -8 1 4 5595.61 392.118 5 8 1 -3 12.5362 147.015 12 -8 1 3 114.760 157.319 5 -8 1 2 1673.18 223.086 5 8 1 -2 1472.79 228.096 12 8 1 -1 1811.33 223.722 6 8 1 0 2750.78 261.263 6 8 1 1 1246.57 206.363 16 8 1 1 1417.47 188.919 6 8 1 2 243.647 110.685 16 -8 2 9 5322.76 300.906 5 -8 2 8 1445.54 208.079 5 8 2 -8 1310.89 181.983 9 -8 2 7 3230.79 310.340 5 8 2 -7 3215.77 257.538 9 -8 2 6 5307.72 392.621 5 8 2 -6 5283.21 348.138 9 8 2 -5 12308.7 507.216 12 -8 2 5 11673.4 541.810 5 8 2 -4 2884.45 265.006 12 -8 2 4 2854.41 292.425 5 -8 2 3 6653.52 406.864 5 8 2 -3 6567.83 388.858 12 -8 2 2 2975.10 255.778 5 8 2 1 729.398 167.560 16 8 2 2-26.8172 88.3609 16 -8 3 9 66.1514 90.1910 5 -8 3 8 436.100 150.260 5 -8 3 7 1979.38 237.286 5 -8 3 6 838.303 191.023 5 -8 3 5 338.391 156.939 5 -8 3 4 4535.22 329.671 5 -8 4 8 381.696 104.120 5 -8 4 7 1328.81 197.768 5 -8 4 6 572.110 158.451 5 -8 4 5 1177.79 149.803 5 9 -6 -4 457.831 105.389 6 9 -6 -3 2512.61 196.622 6 -9 -6 2 106.635 59.4027 8 9 -6 -2 8.64168 81.1489 6 9 -5 -6 772.996 135.895 12 9 -5 -5 770.183 130.966 12 9 -5 -4 142.412 89.4495 12 9 -5 -3 142.792 98.4617 6 9 -5 -2 601.236 134.552 16 9 -5 -2 1124.44 163.249 6 -9 -5 1 185.923 93.2686 8 9 -5 -1 27.0469 58.3733 16 9 -5 -1 244.069 96.8840 6 -9 -4 7 490.893 114.795 5 9 -4 -7 725.449 127.155 12 9 -4 -6 795.018 152.817 12 9 -4 -5 3301.00 267.130 12 9 -4 -4 1587.35 203.968 12 9 -4 -3 1233.99 177.615 12 9 -4 -2 1956.95 222.036 6 -9 -4 1 75.9341 68.0446 8 9 -4 -1 219.460 106.908 16 9 -4 -1 227.331 123.037 6 9 -4 0 170.422 89.0686 16 9 -4 0 244.660 101.062 6 9 -3 -8 749.810 122.651 12 9 -3 -7 564.475 127.040 12 -9 -3 7 357.625 114.772 5 -9 -3 6 1538.96 215.672 5 9 -3 -6 1591.56 202.246 12 9 -3 -5 101.975 124.840 12 -9 -3 5 27.5938 132.831 5 9 -3 -4 845.971 166.372 12 9 -3 -3 2341.67 249.905 12 9 -3 -2 7213.71 399.007 6 -9 -3 1 4.29374 77.6076 8 9 -3 -1 120.704 86.6687 16 9 -3 -1 24.5082 124.200 6 9 -3 0 2977.02 236.481 16 9 -3 0 3290.83 244.642 6 9 -3 1 135.465 77.8070 16 9 -3 1 129.517 80.0361 6 -9 -2 8 1182.32 174.105 5 9 -2 -8 1526.86 154.501 12 -9 -2 7 2105.84 227.943 5 9 -2 -7 1747.10 199.064 12 9 -2 -6 608.061 164.049 12 -9 -2 6 807.564 184.710 5 -9 -2 5 3964.98 326.541 5 9 -2 -5 4434.53 326.163 12 -9 -2 4 4018.45 320.373 5 9 -2 -4 4605.75 333.528 12 9 -2 -3-13.1372 132.441 12 9 -2 -2 641.432 183.194 6 9 -2 -1 444.441 143.786 6 9 -2 0 471.579 146.549 16 9 -2 0 170.512 128.677 6 9 -2 1-171.406 86.3146 16 9 -2 1 33.9453 71.7627 6 9 -1 -8 649.504 119.526 12 -9 -1 8 542.875 133.383 5 9 -1 -7 327.847 123.887 12 -9 -1 7 199.565 144.145 5 9 -1 -6 1401.19 194.036 12 -9 -1 6 1070.34 219.358 5 9 -1 -5 837.819 169.743 12 -9 -1 5 559.691 172.914 5 -9 -1 4 2264.64 259.530 5 9 -1 -4 2681.29 266.910 12 9 -1 -3 1627.69 231.544 12 9 -1 -2 1727.94 223.074 6 9 -1 -1 28.8845 99.0233 6 9 -1 0 819.672 170.508 16 9 -1 0 666.861 146.889 6 9 -1 1 87.2858 86.2165 16 9 -1 1 53.2824 66.8140 6 -9 0 8 260.141 120.752 5 -9 0 7 4962.07 330.388 5 9 0 -7 4440.18 281.610 12 9 0 -6 1091.52 181.628 12 -9 0 6 1149.84 194.996 5 -9 0 5 2618.35 296.612 5 9 0 -5 2849.61 267.917 12 -9 0 4 1439.35 217.611 5 9 0 -4 1724.99 231.170 12 9 0 -3 2057.18 244.686 12 9 0 -2 478.768 159.922 6 9 0 -1 2882.08 248.714 6 9 0 0 838.435 162.638 16 9 0 0 327.734 122.206 6 9 0 1 1975.04 186.472 16 -9 1 8 424.469 128.239 5 -9 1 7 222.451 139.026 5 9 1 -6 1928.26 204.432 12 -9 1 6 1486.75 213.022 5 9 1 -5 544.310 156.873 12 -9 1 5 680.843 181.090 5 -9 1 4 2476.05 253.738 5 9 1 -4 2411.79 239.548 12 9 1 -3 1921.63 213.299 6 9 1 -2 1150.88 171.056 6 9 1 0 644.069 154.430 16 9 1 1 58.7954 62.1958 16 -9 2 8 1171.15 155.724 5 -9 2 7 1960.60 220.840 5 -9 2 6 535.655 153.424 5 -9 2 5 3691.78 293.035 5 -9 2 4 4249.37 297.768 5 9 2 0 85.0639 103.484 16 -9 3 7 467.707 114.103 5 -9 3 6 1589.94 196.888 5 -9 3 5 46.2185 90.2135 5 9 3 -1 41.4437 65.7237 16 10 -3 -5 1417.05 148.067 12 10 -3 -4 1504.13 174.666 6 10 -3 -3 2232.10 194.192 6 10 -2 -6 1303.19 133.760 12 10 -2 -5 309.511 95.3214 12 10 -2 -4 662.964 125.147 6 10 -2 -3 292.228 83.8266 6 10 -2 -2 220.559 91.3522 16 -10 -1 6 671.001 136.489 5 10 -1 -6 808.535 122.349 12 10 -1 -5 545.131 116.438 12 10 -1 -4 675.959 128.832 6 10 -1 -3 2615.07 207.906 6 -10 0 6 530.577 120.556 5 10 0 -4-294.585 102.590 6 0 0 0 0.00 0.00 0 TITL 15069_lu301 in P2(1) REM P2(1) (#4 in standard setting) CELL 1.54184 8.567876 10.921117 9.134913 90.0000 111.8029 90.0000 ZERR 2.00 0.000280 0.000194 0.000273 0.0000 0.0036 0.0000 LATT -1 SYMM -x, y+1/2,-z SFAC C H N Cl UNIT 30.00 50.00 4.00 2.00 TREF HKLF 4 END ; _shelx_hkl_checksum 56989 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -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 C1 C 0.9110(6) -0.2409(4) 0.0147(5) 0.0570(11) Uani 1 1 d . . H1A H 0.8009 -0.2778 -0.0431 0.085 Uiso 1 1 calc R U H1B H 0.9747 -0.2936 0.1036 0.085 Uiso 1 1 calc R U H1C H 0.9729 -0.2320 -0.0559 0.085 Uiso 1 1 calc R U C2 C 0.8023(5) -0.0303(4) -0.0625(4) 0.0515(9) Uani 1 1 d . . H2A H 0.7845 0.0498 -0.0229 0.077 Uiso 1 1 calc R U H2B H 0.6938 -0.0649 -0.1297 0.077 Uiso 1 1 calc R U H2C H 0.8741 -0.0208 -0.1239 0.077 Uiso 1 1 calc R U C3 C 1.0517(5) -0.0616(4) 0.1825(5) 0.0596(11) Uani 1 1 d . . H3A H 1.1037 -0.1156 0.2733 0.089 Uiso 1 1 calc R U H3B H 1.0316 0.0191 0.2192 0.089 Uiso 1 1 calc R U H3C H 1.1269 -0.0529 0.1243 0.089 Uiso 1 1 calc R U C10 C 0.7212(5) -0.5344(3) 0.1707(5) 0.0471(9) Uani 1 1 d . . H10 H 0.6483 -0.5926 0.1011 0.057 Uiso 1 1 calc R U C15 C 0.6884(4) -0.2933(3) 0.5642(4) 0.0438(8) Uani 1 1 d . . H15A H 0.7890 -0.2440 0.6184 0.066 Uiso 1 1 calc R U H15B H 0.7197 -0.3666 0.5196 0.066 Uiso 1 1 calc R U H15C H 0.6372 -0.3176 0.6395 0.066 Uiso 1 1 calc R U H100 H 0.743(4) -0.043(3) 0.174(4) 0.029(8) Uiso 1 1 d . . H200 H 0.627(4) -0.075(4) 0.327(4) 0.033(9) Uiso 1 1 d . . C4 C 0.8871(4) -0.1158(3) 0.0759(4) 0.0366(7) Uani 1 1 d . . C5 C 0.7333(4) -0.1962(3) 0.2526(3) 0.0294(6) Uani 1 1 d . . C6 C 0.7832(4) -0.3276(3) 0.2602(3) 0.0305(6) Uani 1 1 d . . C7 C 0.9351(3) -0.3657(4) 0.3746(3) 0.0376(6) Uani 1 1 d . . H7 H 1.0089 -0.3077 0.4437 0.045 Uiso 1 1 calc R U C8 C 0.9773(5) -0.4887(3) 0.3866(4) 0.0443(8) Uani 1 1 d . . H8 H 1.0803 -0.5154 0.4642 0.053 Uiso 1 1 calc R U C9 C 0.8699(5) -0.5723(3) 0.2858(5) 0.0495(9) Uani 1 1 d . . H9 H 0.8984 -0.6568 0.2957 0.059 Uiso 1 1 calc R U C11 C 0.6784(4) -0.4112(3) 0.1567(4) 0.0376(7) Uani 1 1 d . . H11 H 0.5773 -0.3846 0.0762 0.045 Uiso 1 1 calc R U C12 C 0.5633(4) -0.2182(3) 0.4326(4) 0.0324(6) Uani 1 1 d . . C13 C 0.4186(4) -0.2976(3) 0.3307(4) 0.0412(8) Uani 1 1 d . . H13A H 0.4630 -0.3699 0.2957 0.062 Uiso 1 1 calc R U H13B H 0.3477 -0.2507 0.2385 0.062 Uiso 1 1 calc R U H13C H 0.3516 -0.3235 0.3919 0.062 Uiso 1 1 calc R U C14 C 0.4974(5) -0.1142(4) 0.5043(5) 0.0433(7) Uani 1 1 d . . H14A H 0.4166 -0.0655 0.4200 0.065 Uiso 1 1 calc R U H14B H 0.5913 -0.0621 0.5676 0.065 Uiso 1 1 calc R U H14C H 0.4418 -0.1482 0.5717 0.065 Uiso 1 1 calc R U Cl1 Cl 0.64358(10) 0.13137(7) 0.25225(9) 0.0455(2) Uani 1 1 d . . N1 N 0.7725(4) -0.1154(3) 0.1646(3) 0.0393(6) Uani 1 1 d . . N2 N 0.6445(3) -0.1550(2) 0.3337(3) 0.0336(6) Uani 1 1 d . . 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 C1 0.094(3) 0.0385(19) 0.061(2) 0.0035(18) 0.056(2) 0.0099(19) C2 0.062(2) 0.053(2) 0.048(2) 0.0169(18) 0.0298(18) 0.0137(19) C3 0.046(2) 0.075(3) 0.059(2) -0.004(2) 0.0214(18) 0.001(2) C10 0.053(2) 0.0307(17) 0.064(2) -0.0093(18) 0.0289(19) -0.0037(15) C15 0.0458(18) 0.046(2) 0.0435(17) 0.0100(15) 0.0205(15) 0.0007(16) C4 0.0453(17) 0.0339(17) 0.0360(15) 0.0054(14) 0.0214(14) 0.0063(14) C5 0.0300(14) 0.0284(15) 0.0269(14) 0.0001(12) 0.0073(11) -0.0025(12) C6 0.0355(15) 0.0282(14) 0.0302(14) 0.0020(12) 0.0150(12) 0.0023(12) C7 0.0397(14) 0.0405(16) 0.0332(13) 0.0034(16) 0.0142(12) 0.0049(17) C8 0.0509(18) 0.043(2) 0.0449(18) 0.0152(17) 0.0248(16) 0.0171(16) C9 0.066(2) 0.0287(18) 0.069(2) 0.0097(17) 0.042(2) 0.0130(17) C11 0.0395(16) 0.0330(16) 0.0407(17) -0.0059(13) 0.0155(14) 0.0002(13) C12 0.0394(16) 0.0254(15) 0.0365(15) -0.0018(13) 0.0188(13) -0.0030(13) C13 0.0438(17) 0.0319(18) 0.0492(18) -0.0055(14) 0.0189(15) -0.0063(14) C14 0.0570(17) 0.0321(15) 0.0516(17) -0.0047(14) 0.0328(14) -0.0039(14) Cl1 0.0624(5) 0.0262(3) 0.0531(4) 0.0003(4) 0.0274(4) 0.0039(4) N1 0.0565(17) 0.0255(14) 0.0459(15) 0.0054(12) 0.0307(14) 0.0071(13) N2 0.0458(14) 0.0223(13) 0.0393(14) -0.0002(11) 0.0233(12) -0.0007(11) 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' Cl Cl 0.3639 0.7018 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C4 C1 H1A 109.5 C4 C1 H1B 109.5 H1A C1 H1B 109.5 C4 C1 H1C 109.5 H1A C1 H1C 109.5 H1B C1 H1C 109.5 C4 C2 H2A 109.5 C4 C2 H2B 109.5 H2A C2 H2B 109.5 C4 C2 H2C 109.5 H2A C2 H2C 109.5 H2B C2 H2C 109.5 C4 C3 H3A 109.5 C4 C3 H3B 109.5 H3A C3 H3B 109.5 C4 C3 H3C 109.5 H3A C3 H3C 109.5 H3B C3 H3C 109.5 C9 C10 C11 119.9(4) C9 C10 H10 120.1 C11 C10 H10 120.1 C12 C15 H15A 109.5 C12 C15 H15B 109.5 H15A C15 H15B 109.5 C12 C15 H15C 109.5 H15A C15 H15C 109.5 H15B C15 H15C 109.5 N1 C4 C3 107.2(3) N1 C4 C1 114.2(3) C3 C4 C1 111.7(3) N1 C4 C2 104.1(3) C3 C4 C2 109.8(3) C1 C4 C2 109.5(3) N1 C5 N2 116.4(3) N1 C5 C6 122.6(3) N2 C5 C6 121.0(3) C11 C6 C7 120.3(3) C11 C6 C5 120.2(3) C7 C6 C5 119.5(3) C8 C7 C6 119.4(3) C8 C7 H7 120.3 C6 C7 H7 120.3 C9 C8 C7 120.0(3) C9 C8 H8 120.0 C7 C8 H8 120.0 C8 C9 C10 120.6(3) C8 C9 H9 119.7 C10 C9 H9 119.7 C6 C11 C10 119.8(3) C6 C11 H11 120.1 C10 C11 H11 120.1 N2 C12 C13 110.5(2) N2 C12 C15 112.1(2) C13 C12 C15 110.7(3) N2 C12 C14 104.2(3) C13 C12 C14 110.0(3) C15 C12 C14 109.1(3) C12 C13 H13A 109.5 C12 C13 H13B 109.5 H13A C13 H13B 109.5 C12 C13 H13C 109.5 H13A C13 H13C 109.5 H13B C13 H13C 109.5 C12 C14 H14A 109.5 C12 C14 H14B 109.5 H14A C14 H14B 109.5 C12 C14 H14C 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 C5 N1 C4 134.4(3) C5 N1 H100 114(2) C4 N1 H100 110(2) C5 N2 C12 132.4(3) C5 N2 H200 114(2) C12 N2 H200 113(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 C4 1.518(5) C1 H1A 0.9800 C1 H1B 0.9800 C1 H1C 0.9800 C2 C4 1.522(5) C2 H2A 0.9800 C2 H2B 0.9800 C2 H2C 0.9800 C3 C4 1.506(5) C3 H3A 0.9800 C3 H3B 0.9800 C3 H3C 0.9800 C10 C9 1.380(5) C10 C11 1.388(5) C10 H10 0.9500 C15 C12 1.520(5) C15 H15A 0.9800 C15 H15B 0.9800 C15 H15C 0.9800 C4 N1 1.487(4) C5 N1 1.318(4) C5 N2 1.323(4) C5 C6 1.491(4) C6 C11 1.380(4) C6 C7 1.396(4) C7 C8 1.385(5) C7 H7 0.9500 C8 C9 1.378(5) C8 H8 0.9500 C9 H9 0.9500 C11 H11 0.9500 C12 N2 1.497(4) C12 C13 1.515(4) C12 C14 1.521(5) C13 H13A 0.9800 C13 H13B 0.9800 C13 H13C 0.9800 C14 H14A 0.9800 C14 H14B 0.9800 C14 H14C 0.9800 N1 H100 0.84(4) N2 H200 0.88(4)