#------------------------------------------------------------------------------ #$Date: 2017-09-12 05:11:09 +0300 (Tue, 12 Sep 2017) $ #$Revision: 200505 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/69/1546995.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_1546995 loop_ _publ_author_name 'Dixon, Darren' 'Xie, Lan-Gui' _publ_section_title ; Tertiary Amine Synthesis via Reductive Coupling of Amides with Grignard Reagents ; _journal_name_full 'Chem. Sci.' _journal_paper_doi 10.1039/C7SC03613B _journal_year 2017 _chemical_absolute_configuration ad _chemical_formula_moiety 'C17.67 H21.28 Cl1.30 N0.89 O1.78' _chemical_formula_sum 'C17.67 H21.28 Cl1.3 N0.89 O1.78' _chemical_formula_weight 320.75 _chemical_melting_point ? _chemical_name_systematic 'Compound 24' _space_group_IT_number 5 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'C 2y' _symmetry_space_group_name_H-M 'C 1 2 1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary other _audit_creation_date 2017-05-26 _audit_creation_method CRYSTALS_ver_14.61_build_6156 _audit_update_record ; 2017-06-30 deposited with the CCDC. 2017-09-11 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 96.376(14) _cell_angle_gamma 90 _cell_formula_units_Z 9 _cell_length_a 18.548(4) _cell_length_b 11.9461(13) _cell_length_c 18.0773(18) _cell_measurement_reflns_used 2350 _cell_measurement_temperature 150 _cell_measurement_theta_max 73 _cell_measurement_theta_min 4 _cell_volume 3980.7(10) _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _diffrn_ambient_temperature 150 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.968 _diffrn_measurement_device Serial _diffrn_measurement_device_type Unknown _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.088 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 20977 _diffrn_reflns_theta_full 74.871 _diffrn_reflns_theta_max 78.811 _diffrn_reflns_theta_min 4.410 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.356 _exptl_absorpt_correction_T_max 0.89 _exptl_absorpt_correction_T_min 0.29 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_crystal_colour clear_pale_colourless _exptl_crystal_density_diffrn 1.204 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1528.965 _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.050 _refine_diff_density_max 1.64 _refine_diff_density_min -0.68 _refine_ls_abs_structure_details 'Flack (1983), 3811 Friedel-pairs' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_extinction_method None _refine_ls_goodness_of_fit_ref 1.0347 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 577 _refine_ls_number_reflns 8132 _refine_ls_number_restraints 558 _refine_ls_R_factor_all 0.1184 _refine_ls_R_factor_gt 0.0893 _refine_ls_shift/su_max 0.0111264 _refine_ls_shift/su_mean 0.0007827 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.402E+04 0.659E+04 0.404E+04 0.167E+04 314. ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.2966 _refine_ls_wR_factor_gt 0.2241 _refine_ls_wR_factor_ref 0.2959 _reflns_limit_h_max 22 _reflns_limit_h_min -22 _reflns_limit_k_max 14 _reflns_limit_k_min -14 _reflns_limit_l_max 22 _reflns_limit_l_min 0 _reflns_number_gt 5403 _reflns_number_total 8167 _reflns_threshold_expression I>2.0\s(I) _oxford_diffrn_Wilson_B_factor 4.37 _oxford_diffrn_Wilson_scale 0.13 _oxford_refine_ls_r_factor_ref 0.1184 _oxford_refine_ls_scale 3.01(6) _oxford_reflns_number_all 8133 _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _oxford_structure_analysis_title 016djd17 _iucr_refine_instructions_details ; # # Punched on 26/05/17 at 17:41:28 # #LIST 12 BLOCK CONT SCALE CONT CL ( 1 ,X'S,U'S) UNTIL C ( 181 ) CONT H ( 111 ,X'S) UNTIL H ( 341 ) CONT CL ( 2 ,X'S,U'S) CONT ENANTIO EQUIVALENCE PART(-1, OCC) EQUIVALENCE PART(1001, OCC) CONTINUE PART(1002, OCC) CONTINUE PART(1003, OCC) CONTINUE PART(1004, OCC) WEIGHT -1 PART(1004, OCC) RIDE C ( 4,X'S) H ( 41,X'S) H ( 42,X'S) RIDE C ( 7,X'S) H ( 72,X'S) H ( 73,X'S) H ( 71,X'S) RIDE C ( 10,X'S) H ( 101,X'S) RIDE C ( 12,X'S) H ( 121,X'S) CONT H ( 122,X'S) RIDE C ( 19,X'S) H ( 191,X'S) H ( 192,X'S) RIDE C ( 21,X'S) H ( 211,X'S) RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 24,X'S) H ( 241,X'S) RIDE C ( 25,X'S) H ( 251,X'S) RIDE C ( 26,X'S) H ( 261,X'S) H ( 262,X'S) RIDE C ( 27,X'S) H ( 271,X'S) H ( 272,X'S) RIDE C ( 28,X'S) H ( 281,X'S) H ( 282,X'S) RIDE C ( 30,X'S) H ( 301,X'S) H ( 302,X'S) H ( 303,X'S) RIDE C ( 33,X'S) H ( 331,X'S) RIDE C ( 35,X'S) H ( 351,X'S) RIDE C ( 37,X'S) H ( 371,X'S) RIDE C ( 38,X'S) H ( 381,X'S) RIDE C ( 39,X'S) H ( 391,X'S) RIDE C ( 40,X'S) H ( 401,X'S) RIDE C ( 41,X'S) H ( 411,X'S) RIDE C ( 42,X'S) H ( 422,X'S) CONT H ( 421,X'S) H ( 423,X'S) RIDE C ( 45,X'S) H ( 451,X'S) RIDE C ( 46,X'S) H ( 461,X'S) RIDE C ( 47,X'S) H ( 471,X'S) RIDE C ( 48,X'S) H ( 483,X'S) RIDE C ( 49,X'S) H ( 491,X'S) RIDE C ( 50,X'S) H ( 501,X'S) RIDE C ( 51,X'S) H ( 511,X'S) RIDE C ( 52,X'S) H ( 521,X'S) RIDE C ( 53,X'S) H ( 531,X'S) RIDE C ( 54,X'S) H ( 541,X'S) RIDE C ( 55,X'S) H ( 551,X'S) H ( 552,X'S) RIDE C ( 56,X'S) H ( 562,X'S) H ( 561,X'S) RIDE C ( 57,X'S) H ( 572,X'S) H ( 571,X'S) RIDE C ( 140,X'S) H (1401,X'S) RIDE C ( 141,X'S) H (1411,X'S) RIDE C ( 150,X'S) H (1501,X'S) RIDE C ( 151,X'S) H (1511,X'S) RIDE C ( 160,X'S) H (1601,X'S) RIDE C ( 161,X'S) H (1611,X'S) RIDE C ( 170,X'S) H (1701,X'S) RIDE C ( 171,X'S) H (1711,X'S) RIDE C ( 180,X'S) H (1801,X'S) RIDE C ( 181,X'S) H (1811,X'S) END # # Punched on 26/05/17 at 17:41:28 # #LIST 16 SAME CL(5) C(4) CL(3) AND CONT CL(3) C(4) CL(5) SIMU 0.01 CL(5) C(4) CL(3) AND CONT CL(3) C(4) CL(5) DELU 0.01 CL(5) C(4) CL(3) AND CONT CL(3) C(4) CL(5) SAME C(42) C(44) C(53) C(52) C(50) C(48) C(46) AND CONT C(42) C(44) C(46) C(48) C(50) C(52) C(53) SIMU 0.01 C(42) C(44) C(53) C(52) C(50) C(48) C(46) AND CONT C(42) C(44) C(46) C(48) C(50) C(52) C(53) DELU 0.01 C(42) C(44) C(53) C(52) C(50) C(48) C(46) AND CONT C(42) C(44) C(46) C(48) C(50) C(52) C(53) SAME C(42) C(43) C(45) C(47) C(49) C(51) C(54) AND CONT C(42) C(43) C(54) C(51) C(49) C(47) C(45) SIMU 0.01 C(42) C(43) C(45) C(47) C(49) C(51) C(54) AND CONT C(42) C(43) C(54) C(51) C(49) C(47) C(45) DELU 0.01 C(42) C(43) C(45) C(47) C(49) C(51) C(54) AND CONT C(42) C(43) C(54) C(51) C(49) C(47) C(45) SAME C(12) C(130) C(141) C(151) C(160) C(170) C(180) AND CONT C(12) C(130) C(180) C(170) C(160) C(151) C(141) SIMU 0.01 C(12) C(130) C(141) C(151) C(160) C(170) C(180) AND CONT C(12) C(130) C(180) C(170) C(160) C(151) C(141) DELU 0.01 C(12) C(130) C(141) C(151) C(160) C(170) C(180) AND CONT C(12) C(130) C(180) C(170) C(160) C(151) C(141) SAME C(12) C(131) C(140) C(150) C(161) C(171) C(181) AND CONT C(12) C(131) C(181) C(171) C(161) C(150) C(140) SIMU C(12) C(131) C(140) C(150) C(161) C(171) C(181) AND CONT C(12) C(131) C(181) C(171) C(161) C(150) C(140) DELU C(12) C(131) C(140) C(150) C(161) C(171) C(181) AND CONT C(12) C(131) C(181) C(171) C(161) C(150) C(140) NO REM HREST START (DO NOT REMOVE THIS LINE) REM NO H NO #H U MULT DIST REM C-H REM >4 1.5 .96 DISORDER REM 1 1 1.2 .93 C C-H (ACETYLENE) REM 1 2 1.2 .93 C-C(H)-C REM 1 3 1.2 .98 (C)3-C-H REM 2 1 1.2 .93 C=C-H(2) REM 2 2 1.2 .97 (C)2-C-(H)2 REM 3 1 1.5 .96 C-C-(H)3 REM N-H REM >4 1.5 .89 DISORDER REM 1 1 1.2 .86 N-N/H REM 1 2 1.2 .86 (C)2-N-H REM 1 3 1.2 .89 (C)3-N-H REM 2 1 1.2 .86 C-N-(H)2 REM 2 2 1.2 .89 (C)2-N-(H)2 REM 3 1 1.2 .89 C-H-(H)3 REM O-H REM 1 1 1.5 .82 O-H REM REM DIST ESD = 0.02 REM VIB ESD = 0.002 REM ANGLE ESD = 2.0 REM REM TO ACTIVATE THE VIB RESTRAINTS, REMOVE LEADING REM REM POSSIBLY DISORDERED, NO OF H ATOMS= 1 DIST 0.89, 0.02 = CONT N ( 11) TO H(111) REST 0.075, 0.002 = H(111,U[ISO]) ANGLE 109.54, 2.0 = CONT C(10) TO N ( 11) TO H(111) CONT C(12) TO N ( 11) TO H(111) CONT C(26) TO N ( 11) TO H(111) REM POSSIBLY DISORDERED, NO OF H ATOMS= 1 DIST 0.89, 0.02 = CONT N ( 34) TO H(341) REST 0.066, 0.002 = H(341,U[ISO]) ANGLE 109.54, 2.0 = CONT C(33) TO N ( 34) TO H(341) CONT C(35) TO N ( 34) TO H(341) CONT C(55) TO N ( 34) TO H(341) REM HREST END (DO NOT REMOVE THIS LINE) DISTANCE 1.770000 , 0.050000 = C(4) TO CL(5) DISTANCE 1.770000 , 0.010000 = CL(3) TO C(4) DISTANCE 1.700000 , 0.010000 = C(4) TO CL(5) END ; _cod_data_source_file c7sc03613b2.cif _cod_data_source_block 24 _cod_depositor_comments ; The following automatic conversions were performed: '_chemical_melting_point' value 'not measured' was changed to '?' - the value is undefined or not given. '_atom_sites_solution_primary' value 'Other' changed to 'other' according to /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas ; _cod_original_sg_symbol_H-M 'C 2 ' _cod_original_formula_sum 'C17.67 H21.28 Cl1.30 N0.89 O1.78' _cod_database_code 1546995 _iucr_refine_reflections_details ; # An asterisk in column 34 indicates a format overflow # Data was input as F-squared 0 -14 0 2575.72 487.50 0 -14 -1 1549.25 360.05 0 -14 -2 4641.95 559.45 0 -14 -3 534.04 344.82 0 -14 4 2654.27 446.47 0 -14 5 403.97 344.05 0 -14 6 2091.84 362.26 0 -14 7 3066.98 367.65 0 -12 0 18539.1 1598.0 0 -12 -1 -417.31 503.67 0 -12 1 303.27 468.86 0 -12 2 11402.5 1255.1 0 -12 -2 12166.4 1247.0 0 -12 -3 272.79 463.54 0 -12 3 323.17 412.01 0 -12 4 746.77 453.99 0 -12 5 -235.54 420.01 0 -12 -5 -270.02 442.10 0 -12 6 2015.66 583.97 0 -12 -6 867.77 410.98 0 -12 7 2839.82 820.57 0 -12 -7 1344.33 459.18 0 -12 8 6821.95 1018.10 0 -12 -8 4740.43 879.86 0 -12 9 1405.19 616.28 0 -12 -9 415.46 364.64 0 -12 10 1238.30 598.53 0 -12 -10 1047.50 500.19 0 -12 -11 2159.91 617.45 0 -12 11 2738.69 600.72 0 -12 12 1488.70 489.01 0 -10 0 35503.7 2302.4 0 -10 1 9568.76 1229.31 0 -10 -1 9110.83 1175.32 0 -10 -2 10174.1 1233.9 0 -10 2 10682.7 1309.3 0 -10 3 11076.3 1311.0 0 -10 -3 10069.0 1198.7 0 -10 -4 4473.20 651.11 0 -10 4 4638.73 891.82 0 -10 5 17234.8 1950.9 0 -10 5 12502.0 1391.9 0 -10 5 15242.4 1402.6 0 -10 6 13514.4 1400.7 0 -10 6 16326.8 1461.2 0 -10 6 19084.5 2064.6 0 -10 7 9544.34 1140.03 0 -10 7 13197.3 1821.4 0 -10 7 10707.9 1221.4 0 -10 8 8403.95 1106.22 0 -10 8 8980.55 1089.50 0 -10 -8 6785.28 1185.75 0 -10 -9 1230.02 548.40 0 -10 9 2783.96 692.95 0 -10 9 2850.41 878.62 0 -10 9 2232.51 618.76 0 -10 10 1926.79 531.91 0 -10 -10 1771.57 657.42 0 -10 10 2223.85 822.78 0 -10 11 2623.72 590.18 0 -10 11 3611.56 938.77 0 -10 -11 2361.67 790.19 0 -10 12 1219.66 574.02 0 -10 -12 1800.49 637.59 0 -10 12 1349.99 470.30 0 -10 13 984.68 392.32 0 -10 -13 973.64 505.96 0 -10 13 245.16 413.53 0 -10 -14 1748.62 618.71 0 -10 14 405.73 326.52 0 -10 14 1323.64 429.54 0 -10 15 427.61 338.13 0 -10 15 -310.61 386.24 0 -10 16 75.93 281.50 0 -10 16 459.86 343.87 0 -8 0 47431.7 3611.4 0 -8 0 45263.2 3934.0 0 -8 -1 28004.4 2923.2 0 -8 -1 27198.5 2972.7 0 -8 -2 27798.3 3064.4 0 -8 -2 29599.6 3160.6 0 -8 -3 14639.6 2370.9 0 -8 -3 13913.4 2223.4 0 -8 -4 12491.9 2233.8 0 -8 -4 11312.0 2122.8 0 -8 -5 5428.12 1558.75 0 -8 -5 5000.15 1467.93 0 -8 -6 2808.43 783.08 0 -8 6 3977.49 892.86 0 -8 -6 4171.73 868.34 0 -8 -6 3245.33 1204.54 0 -8 6 3925.69 881.00 0 -8 -7 3946.87 1538.86 0 -8 7 5044.45 1280.55 0 -8 7 2859.20 745.76 0 -8 7 3436.16 938.86 0 -8 -7 3276.53 863.92 0 -8 -7 3386.16 718.08 0 -8 8 19297.5 2099.2 0 -8 -8 14224.8 1566.5 0 -8 8 16920.2 1724.8 0 -8 -8 14445.0 2606.2 0 -8 -8 14842.5 1713.5 0 -8 8 15192.4 1412.4 0 -8 -9 28278.3 2341.2 0 -8 9 31918.4 2622.4 0 -8 9 28253.1 1828.0 0 -8 -9 31633.5 2369.6 0 -8 -9 30824.2 3736.1 0 -8 9 30796.2 2319.4 0 -8 -10 2429.45 890.49 0 -8 -10 2603.67 715.45 0 -8 10 2200.36 811.46 0 -8 -10 1674.03 614.71 0 -8 10 2319.44 997.50 0 -8 -11 325.34 365.79 0 -8 11 1561.41 846.20 0 -8 -11 660.62 661.31 0 -8 -11 566.79 416.29 0 -8 -12 5768.15 1213.52 0 -8 -12 7505.49 1273.98 0 -8 12 5720.07 1285.61 0 -8 -12 6734.22 1164.88 0 -8 13 215.57 537.36 0 -8 -13 -44.17 459.39 0 -8 -13 524.89 573.89 0 -8 -13 562.79 433.30 0 -8 -14 3414.99 812.19 0 -8 -14 3810.20 929.97 0 -8 14 3138.39 871.96 0 -8 15 -114.93 412.62 0 -8 15 361.66 395.12 0 -8 -15 203.35 396.60 0 -8 -15 279.34 464.47 0 -8 -16 738.26 429.01 0 -8 16 569.22 434.13 0 -8 16 397.98 323.34 0 -8 17 1166.93 438.86 0 -8 17 459.93 401.78 0 -8 -17 1197.53 438.70 0 -8 18 1360.76 430.19 0 -8 18 337.85 298.88 0 -8 19 796.70 285.03 0 -6 0 40876.5 2938.4 0 -6 -1 10365.3 1562.0 0 -6 1 9138.90 1343.87 0 -6 2 138977. 4801. 0 -6 -2 136146. 5693. 0 -6 -2 133550. 5832. 0 -6 -3 4890.10 1069.83 0 -6 -3 4412.09 1080.12 0 -6 3 4958.23 780.16 0 -6 -4 6988.54 1406.28 0 -6 -4 6062.28 1322.70 0 -6 -5 37391.2 3433.6 0 -6 -5 38109.7 3317.7 0 -6 -6 7379.99 1588.18 0 -6 -6 7364.48 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296.76 -21 -5 4 1289.97 448.63 -21 -5 3 504.78 337.14 -21 -5 3 1025.71 374.17 -21 -5 2 -87.20 268.64 -21 -5 2 508.39 346.31 -21 -5 1 333.40 285.96 -21 -5 1 699.52 305.36 -21 -5 0 246.32 294.11 -21 -5 0 573.40 311.22 -21 -5 -1 567.04 332.05 -21 -5 -1 1003.38 318.63 -21 -5 -2 888.97 350.27 -21 -5 -2 925.95 317.55 -21 -5 -3 -134.59 195.25 -21 -3 10 411.95 250.36 -21 -3 9 -165.02 217.26 -21 -3 9 44.27 271.11 -21 -3 8 198.31 276.67 -21 -3 8 -171.22 270.71 -21 -3 7 86.51 265.58 -21 -3 7 413.10 339.98 -21 -3 6 -222.85 258.41 -21 -3 6 545.40 362.60 -21 -3 5 239.94 254.90 -21 -3 5 204.95 339.08 -21 -3 4 643.53 362.88 -21 -3 4 495.65 412.40 -21 -3 3 406.64 380.16 -21 -3 3 5.83 286.40 -21 -3 3 714.40 409.10 -21 -3 2 669.10 407.89 -21 -3 2 637.39 416.56 -21 -3 2 1149.00 477.16 -21 -3 1 253.52 328.35 -21 -3 1 919.07 436.52 -21 -3 0 35.51 255.87 -21 -3 0 519.67 387.15 -21 -3 -1 184.44 297.93 -21 -3 -1 294.79 350.13 -21 -3 -2 341.32 311.96 -21 -3 -2 205.86 288.47 -21 -3 -3 378.95 264.11 -21 -3 -3 1486.78 438.26 -21 -3 -3 1550.39 422.74 -21 -3 -4 1943.95 438.04 -21 -3 -4 1277.85 357.73 -21 -3 -5 813.09 310.62 -21 -3 -6 270.80 245.91 -21 -1 11 279.73 259.45 -21 -1 10 -78.81 229.74 -21 -1 10 -7.56 228.77 -21 -1 9 -30.35 254.56 -21 -1 9 12.72 253.26 -21 -1 8 357.17 373.83 -21 -1 8 -211.35 285.98 -21 -1 7 338.25 362.08 -21 -1 7 730.55 364.56 -21 -1 6 527.02 409.66 -21 -1 6 717.25 404.45 -21 -1 5 606.73 409.67 -21 -1 5 13.40 366.32 -21 -1 4 101.75 336.43 -21 -1 4 -157.12 331.15 -21 -1 3 634.19 362.29 -21 -1 3 684.55 397.02 -21 -1 3 1205.94 459.17 -21 -1 2 242.00 376.18 -21 -1 2 592.49 401.53 -21 -1 2 694.64 482.10 -21 -1 1 228.22 341.74 -21 -1 1 -39.92 250.08 -21 -1 1 79.06 348.44 -21 -1 0 -21.23 354.62 -21 -1 -1 253.62 329.71 -21 -1 -2 134.61 321.20 -21 -1 -3 2624.48 567.84 -21 -1 -4 267.43 308.58 -21 -1 -5 78.62 307.89 -21 -1 -5 283.45 357.55 -21 -1 -6 395.92 304.35 -21 -1 -6 679.00 323.46 -21 -1 -7 -214.47 229.82 -21 1 11 434.53 275.76 -21 1 10 138.61 261.98 -21 1 9 168.59 286.64 -21 1 8 951.49 461.43 -21 1 7 1383.06 469.75 -21 1 7 594.74 323.96 -21 1 6 493.94 383.06 -21 1 6 405.28 358.64 -21 1 5 541.74 410.38 -21 1 5 975.70 428.91 -21 1 4 -116.63 368.16 -21 1 4 239.47 355.46 -21 1 3 458.56 356.07 -21 1 3 644.19 357.40 -21 1 2 17.84 339.27 -21 1 2 371.01 359.45 -21 1 1 144.89 299.30 -21 1 1 -112.04 378.33 -21 1 1 90.72 323.56 -21 1 0 -216.00 350.21 -21 1 0 521.78 404.19 -21 1 0 -549.06 365.63 -21 1 -1 326.99 392.38 -21 1 -1 -57.26 326.58 -21 1 -2 135.12 395.04 -21 1 -2 305.32 321.24 -21 1 -3 2381.48 673.33 -21 1 -3 2050.83 490.43 -21 1 -4 552.34 418.34 -21 1 -4 482.97 303.02 -21 1 -5 48.96 263.92 -21 1 -5 108.50 318.10 -21 1 -6 662.66 341.76 -21 1 -7 54.79 215.72 -21 3 9 -6.21 252.65 -21 3 8 111.07 259.79 21 3 -8 50.37 221.98 -21 3 7 351.18 316.02 21 3 -7 492.09 251.12 -21 3 6 238.36 273.53 21 3 -6 -77.88 261.85 -21 3 5 28.38 277.89 21 3 -5 265.42 264.88 -21 3 4 276.66 365.52 21 3 -4 425.00 246.71 -21 3 3 721.55 447.09 21 3 -3 310.98 258.37 -21 3 2 781.33 437.38 21 3 -2 48.89 246.35 -21 3 1 290.60 456.47 -21 3 0 320.65 426.99 -21 3 -1 -84.89 377.34 -21 3 -2 620.11 399.43 -21 3 -3 1519.85 549.81 -21 3 -4 1798.30 562.48 -21 3 -4 1216.42 396.27 -21 3 -5 533.84 308.60 21 5 -8 0.89 164.49 21 5 -7 293.44 203.14 21 5 -6 79.17 206.03 21 5 -5 1219.91 255.55 21 5 -4 217.82 210.94 -21 5 3 1117.42 476.98 21 5 -3 459.53 204.34 -21 5 2 -753.34 341.69 -21 5 2 11.41 388.24 21 5 -2 -24.26 198.90 -21 5 1 470.81 318.72 -21 5 1 1436.08 478.72 -21 5 0 -10.28 254.36 -21 5 0 97.94 301.02 -21 5 -1 757.42 350.86 -21 5 -1 1483.24 460.47 -21 5 -2 1217.49 426.49 -21 5 -3 220.96 269.77 -22 -4 6 43.78 202.22 -22 -4 6 281.09 228.54 -22 -4 5 -115.95 194.51 -22 -4 5 230.70 263.15 -22 -4 4 115.85 220.18 -22 -4 4 258.09 238.55 -22 -4 3 36.30 211.03 -22 -4 3 358.59 265.90 -22 -4 2 91.11 214.58 -22 -4 2 4.04 245.53 -22 -4 1 319.12 247.49 -22 -4 1 410.12 255.69 -22 -4 0 -333.73 246.16 -22 -4 -1 91.43 206.77 -22 -2 8 363.74 205.16 -22 -2 8 -2.72 201.96 -22 -2 7 245.97 240.77 -22 -2 7 174.33 259.86 -22 -2 6 757.04 328.55 -22 -2 6 533.79 319.14 -22 -2 6 359.37 313.03 -22 -2 5 367.05 337.38 -22 -2 5 498.75 299.44 -22 -2 5 1094.79 419.22 -22 -2 4 114.96 261.11 -22 -2 4 370.71 315.93 -22 -2 4 -89.46 269.67 -22 -2 3 337.58 293.87 -22 -2 3 764.79 319.61 -22 -2 3 828.69 392.27 -22 -2 2 461.06 249.46 -22 -2 2 617.61 378.06 -22 -2 1 47.01 267.25 -22 -2 0 -52.33 262.90 -22 -2 -1 1095.66 382.30 -22 -2 -2 543.38 315.53 -22 -2 -3 246.27 251.16 -22 -2 -3 -215.69 204.89 -22 -2 -4 -251.04 222.86 -22 0 9 57.25 220.42 -22 0 8 672.10 347.34 -22 0 7 -189.31 250.85 -22 0 7 156.23 265.96 -22 0 6 -84.42 251.05 -22 0 6 -201.96 223.38 -22 0 5 307.40 317.73 -22 0 5 25.59 271.53 -22 0 4 166.98 312.04 -22 0 4 254.59 322.58 -22 0 4 694.05 362.35 -22 0 3 -82.02 287.03 -22 0 3 149.38 314.19 -22 0 3 298.37 333.12 -22 0 2 120.53 292.00 -22 0 2 186.46 323.84 -22 0 2 436.47 321.27 -22 0 1 80.12 407.01 -22 0 1 362.42 334.82 -22 0 0 818.86 448.40 -22 0 0 558.83 315.42 -22 0 -1 296.04 311.41 -22 0 -1 -13.45 260.68 -22 0 -2 96.59 245.80 -22 0 -3 394.10 279.42 -22 0 -4 956.38 301.84 -22 0 -4 876.84 354.99 -22 0 -5 -247.10 211.20 -22 2 8 -59.71 227.10 -22 2 7 131.53 246.08 -22 2 6 363.32 323.62 -22 2 5 552.33 337.44 -22 2 4 178.21 306.73 -22 2 3 216.34 325.99 -22 2 3 -13.95 361.72 -22 2 2 579.37 409.64 -22 2 1 337.48 345.74 -22 2 0 -55.97 320.48 -22 2 -1 1535.78 519.18 -22 2 -2 861.30 400.42 -22 2 -3 332.81 308.23 -22 2 -3 -233.21 255.95 -22 2 -4 -28.21 216.20 -22 4 5 247.08 309.72 -22 4 4 121.59 273.22 -22 4 3 267.81 341.30 -22 4 2 -59.32 290.30 -22 4 1 475.08 352.50 -22 4 0 634.00 345.48 -22 4 -1 401.23 294.66 -22 4 -2 -170.35 236.96 ; loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,y+1/2,z -x,y,-z -x+1/2,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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.67358(13) 0.4532(2) 0.02746(13) 0.0800 1.0000 Uani . . . . Cl3 Cl 0.5062(4) 0.4377(5) 0.1184(5) 0.1211 0.465(9) Uani D P . -1 C4 C 0.5065(15) 0.5203(8) 0.0381(4) 0.1097 0.465(9) Uani D P . -1 Cl5 Cl 0.5306(3) 0.6567(5) 0.0628(4) 0.0961 0.465(9) Uani D P . -1 O6 O 0.5715(3) 0.0607(5) 0.0718(3) 0.0704 1.0000 Uani . . . . C7 C 0.5430(5) -0.0407(10) 0.1023(6) 0.0841 1.0000 Uani . . . . C8 C 0.6234(4) 0.0448(7) 0.0293(4) 0.0581 1.0000 Uani . . . . O9 O 0.6466(3) -0.0444(5) 0.0113(3) 0.0722 1.0000 Uani . . . . C10 C 0.6532(4) 0.1571(6) 0.0029(4) 0.0530 1.0000 Uani D . . . N11 N 0.7344(3) 0.1552(5) 0.0089(3) 0.0496 1.0000 Uani D . . . C12 C 0.7688(3) 0.2047(4) 0.0816(3) 0.0453 1.0000 Uani D . . . C19 C 0.8510(4) 0.2007(6) 0.0880(4) 0.0581 1.0000 Uani . . . . C20 C 0.8843(4) 0.2588(6) 0.1581(4) 0.0514 1.0000 Uani . . . . C21 C 0.8713(4) 0.3708(7) 0.1703(4) 0.0599 1.0000 Uani . . . . C22 C 0.9018(5) 0.4276(8) 0.2339(5) 0.0696 1.0000 Uani . . . . C23 C 0.9492(5) 0.3679(8) 0.2858(4) 0.0698 1.0000 Uani . . . . C24 C 0.9635(5) 0.2559(9) 0.2751(5) 0.0748 1.0000 Uani . . . . C25 C 0.9299(5) 0.2021(8) 0.2116(5) 0.0678 1.0000 Uani . . . . C26 C 0.7558(5) 0.2134(7) -0.0585(4) 0.0643 1.0000 Uani D . . . C27 C 0.6970(5) 0.1787(8) -0.1183(5) 0.0754 1.0000 Uani . . . . C28 C 0.6279(5) 0.1792(7) -0.0803(4) 0.0670 1.0000 Uani . . . . O29 O 0.6018(3) 0.4970(4) 0.4439(3) 0.0590 1.0000 Uani . . . . C30 C 0.5355(5) 0.4697(7) 0.3959(6) 0.0830 1.0000 Uani . . . . C31 C 0.6122(4) 0.6062(6) 0.4580(3) 0.0464 1.0000 Uani . . . . O32 O 0.5712(3) 0.6787(4) 0.4354(3) 0.0606 1.0000 Uani . . . . C33 C 0.6794(4) 0.6215(5) 0.5113(3) 0.0499 1.0000 Uani D . . . N34 N 0.7211(3) 0.7251(4) 0.4932(3) 0.0444 1.0000 Uani D . . . C35 C 0.7770(4) 0.6989(5) 0.4388(3) 0.0472 1.0000 Uani D . . . C36 C 0.7381(3) 0.6550(5) 0.3661(3) 0.0424 1.0000 Uani . . . . C37 C 0.6865(4) 0.7181(6) 0.3224(4) 0.0517 1.0000 Uani . . . . C38 C 0.6531(4) 0.6749(7) 0.2555(4) 0.0574 1.0000 Uani . . . . C39 C 0.6747(5) 0.5686(7) 0.2327(4) 0.0633 1.0000 Uani . . . . C40 C 0.7250(5) 0.5098(7) 0.2738(4) 0.0657 1.0000 Uani . . . . C41 C 0.7577(4) 0.5511(6) 0.3419(4) 0.0510 1.0000 Uani . . . . C42 C 0.8239(3) 0.8010(5) 0.4290(4) 0.0547 1.0000 Uani D . . . C43 C 0.8826(5) 0.7695(10) 0.3905(5) 0.0517 0.228(7) Uani D P 1 1 C44 C 0.8783(4) 0.7807(6) 0.3716(4) 0.0575 0.655(7) Uani D P 1 2 C45 C 0.9353(8) 0.6940(16) 0.4234(9) 0.0513 0.228(7) Uani D P 1 1 C46 C 0.9308(5) 0.6962(8) 0.3831(5) 0.0674 0.655(7) Uani D P 1 2 C47 C 0.9911(8) 0.6543(18) 0.3798(12) 0.0559 0.228(7) Uani D P 1 1 C48 C 0.9814(6) 0.6771(10) 0.3310(6) 0.0743 0.655(7) Uani D P 1 2 C49 C 0.9818(10) 0.6842(18) 0.3100(11) 0.0559 0.228(7) Uani D P 1 1 C50 C 0.9775(5) 0.7434(9) 0.2667(5) 0.0720 0.655(7) Uani D P 1 2 C51 C 0.9424(10) 0.762(2) 0.2755(9) 0.0562 0.228(7) Uani D P 1 1 C52 C 0.9274(6) 0.8312(8) 0.2552(4) 0.0676 0.655(7) Uani D P 1 2 C53 C 0.8780(5) 0.8495(7) 0.3086(4) 0.0614 0.655(7) Uani D P 1 2 C54 C 0.8853(10) 0.8049(18) 0.3163(7) 0.0522 0.228(7) Uani D P 1 1 C55 C 0.7534(4) 0.7680(6) 0.5671(4) 0.0546 1.0000 Uani D . . . C56 C 0.6916(5) 0.7533(6) 0.6140(4) 0.0593 1.0000 Uani . . . . C57 C 0.6589(6) 0.6392(7) 0.5920(4) 0.0707 1.0000 Uani . . . . C130 C 0.7399(9) 0.1423(5) 0.1461(7) 0.0469 0.559(7) Uani D P 1 4 C131 C 0.7350(11) 0.1583(8) 0.1463(9) 0.0451 0.441(7) Uani D P 1 3 C140 C 0.6894(8) 0.2257(9) 0.1815(7) 0.0467 0.441(7) Uani D P 1 3 C141 C 0.6968(8) 0.1960(6) 0.1959(6) 0.0482 0.559(7) Uani D P 1 4 C150 C 0.6614(9) 0.1874(12) 0.2451(7) 0.0624 0.441(7) Uani D P 1 3 C151 C 0.6679(7) 0.1407(8) 0.2527(6) 0.0510 0.559(7) Uani D P 1 4 C160 C 0.6817(8) 0.0246(8) 0.2619(6) 0.0527 0.559(7) Uani D P 1 4 C161 C 0.6722(8) 0.0730(12) 0.2645(6) 0.0452 0.441(7) Uani D P 1 3 C170 C 0.7253(9) -0.0328(7) 0.2151(7) 0.0529 0.559(7) Uani D P 1 4 C171 C 0.7162(11) 0.0021(10) 0.2250(10) 0.0565 0.441(7) Uani D P 1 3 C180 C 0.7512(11) 0.0254(7) 0.1577(8) 0.0490 0.559(7) Uani D P 1 4 C181 C 0.7502(12) 0.0492(10) 0.1676(11) 0.0550 0.441(7) Uani D P 1 3 H72 H 0.5336 -0.0268 0.1527 0.1260 1.0000 Uiso R . . . H73 H 0.4990 -0.0609 0.0726 0.1261 1.0000 Uiso R . . . H71 H 0.5777 -0.0998 0.1009 0.1259 1.0000 Uiso R . . . H101 H 0.6369 0.2176 0.0338 0.0635 1.0000 Uiso R . . . H121 H 0.7557 0.2841 0.0801 0.0551 0.441(7) Uiso R P 1 3 H122 H 0.7535 0.2829 0.0844 0.0551 0.559(7) Uiso R P 1 4 H191 H 0.8672 0.2365 0.0447 0.0690 1.0000 Uiso R . . . H192 H 0.8657 0.1229 0.0895 0.0686 1.0000 Uiso R . . . H211 H 0.8408 0.4102 0.1349 0.0711 1.0000 Uiso R . . . H221 H 0.8915 0.5040 0.2420 0.0831 1.0000 Uiso R . . . H231 H 0.9722 0.4054 0.3275 0.0840 1.0000 Uiso R . . . H241 H 0.9954 0.2160 0.3093 0.0898 1.0000 Uiso R . . . H251 H 0.9388 0.1262 0.2045 0.0810 1.0000 Uiso R . . . H261 H 0.7567 0.2938 -0.0514 0.0769 1.0000 Uiso R . . . H262 H 0.8037 0.1867 -0.0694 0.0767 1.0000 Uiso R . . . H271 H 0.6938 0.2304 -0.1605 0.0908 1.0000 Uiso R . . . H272 H 0.7068 0.1038 -0.1356 0.0910 1.0000 Uiso R . . . H281 H 0.6041 0.2519 -0.0853 0.0799 1.0000 Uiso R . . . H282 H 0.5950 0.1216 -0.1006 0.0800 1.0000 Uiso R . . . H301 H 0.5314 0.3893 0.3916 0.1241 1.0000 Uiso R . . . H302 H 0.4944 0.4992 0.4175 0.1240 1.0000 Uiso R . . . H303 H 0.5384 0.5022 0.3473 0.1240 1.0000 Uiso R . . . H331 H 0.7094 0.5554 0.5100 0.0602 1.0000 Uiso R . . . H351 H 0.8097 0.6397 0.4598 0.0553 1.0000 Uiso R . . . H371 H 0.6737 0.7883 0.3380 0.0610 1.0000 Uiso R . . . H381 H 0.6169 0.7156 0.2269 0.0689 1.0000 Uiso R . . . H391 H 0.6537 0.5394 0.1883 0.0762 1.0000 Uiso R . . . H401 H 0.7387 0.4396 0.2574 0.0779 1.0000 Uiso R . . . H411 H 0.7931 0.5081 0.3704 0.0611 1.0000 Uiso R . . . H422 H 0.8151 0.8728 0.4458 0.0650 0.228(7) Uiso R P 1 1 H421 H 0.8509 0.8194 0.4765 0.0649 0.655(7) Uiso R P 1 2 H423 H 0.7927 0.8637 0.4121 0.0646 0.655(7) Uiso R P 1 2 H461 H 0.9326 0.6528 0.4258 0.0809 0.655(7) Uiso R P 1 2 H471 H 1.0305 0.6120 0.4001 0.0671 0.228(7) Uiso R P 1 1 H491 H 1.0077 0.6411 0.2793 0.0671 0.228(7) Uiso R P 1 1 H511 H 0.9510 0.7894 0.2291 0.0670 0.228(7) Uiso R P 1 1 H531 H 0.8450 0.9080 0.3014 0.0731 0.655(7) Uiso R P 1 2 H551 H 0.7953 0.7232 0.5852 0.0649 1.0000 Uiso R . . . H552 H 0.7670 0.8460 0.5637 0.0648 1.0000 Uiso R . . . H562 H 0.7092 0.7547 0.6667 0.0708 1.0000 Uiso R . . . H561 H 0.6560 0.8123 0.6035 0.0710 1.0000 Uiso R . . . H572 H 0.6790 0.5805 0.6252 0.0839 1.0000 Uiso R . . . H571 H 0.6063 0.6402 0.5920 0.0839 1.0000 Uiso R . . . H1401 H 0.6777 0.2972 0.1628 0.0560 0.441(7) Uiso R P 1 3 H1411 H 0.6881 0.2722 0.1897 0.0581 0.559(7) Uiso R P 1 4 H1501 H 0.6358 0.2353 0.2735 0.0741 0.441(7) Uiso R P 1 3 H1511 H 0.6396 0.1785 0.2842 0.0622 0.559(7) Uiso R P 1 4 H1701 H 0.7360 -0.1088 0.2222 0.0641 0.559(7) Uiso R P 1 4 H1711 H 0.7221 -0.0733 0.2372 0.0662 0.441(7) Uiso R P 1 3 H1801 H 0.7777 -0.0133 0.1253 0.0589 0.559(7) Uiso R P 1 4 H1811 H 0.7821 0.0066 0.1430 0.0640 0.441(7) Uiso R P 1 3 H111 H 0.7488(13) 0.0840(17) 0.0064(13) 0.0749 1.0000 Uiso D . . . H341 H 0.6901(12) 0.7754(19) 0.4719(13) 0.0661 1.0000 Uiso D . . . H483 H 1.0169 0.6225 0.3397 0.0898 0.655(7) Uiso R P 1 2 H451 H 0.9341 0.6704 0.4721 0.0611 0.228(7) Uiso R P 1 1 H521 H 0.9265 0.8775 0.2136 0.0821 0.655(7) Uiso R P 1 2 H541 H 0.8502 0.8531 0.2937 0.0620 0.228(7) Uiso R P 1 1 H501 H 1.0085 0.7281 0.2303 0.0869 0.655(7) Uiso R P 1 2 H1611 H 0.6501 0.0431 0.3043 0.0541 0.441(7) Uiso R P 1 3 H1601 H 0.6620 -0.0145 0.2997 0.0637 0.559(7) Uiso R P 1 4 H41 H 0.5410 0.4893 0.0068 0.1320 0.465(9) Uiso R P . -1 H42 H 0.4582 0.5195 0.0110 0.1321 0.465(9) Uiso R P . -1 Cl2 Cl 0.15704(9) 0.4569(2) 0.45252(8) 0.0531 1.0000 Uani . . . . 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 Cl1 0.1011(14) 0.0459(9) 0.0895(14) 0.0162(10) -0.0047(11) -0.0016(11) Cl3 0.098(4) 0.097(4) 0.167(6) 0.024(4) 0.007(4) -0.022(3) C4 0.086(5) 0.094(5) 0.149(6) 0.009(5) 0.017(5) -0.014(5) Cl5 0.073(3) 0.090(4) 0.130(5) -0.002(3) 0.030(3) -0.003(3) O6 0.062(3) 0.070(4) 0.079(4) 0.022(3) 0.004(3) -0.003(3) C7 0.077(5) 0.086(6) 0.089(6) 0.030(6) 0.006(4) -0.011(5) C8 0.073(5) 0.053(4) 0.043(3) 0.008(3) -0.015(3) -0.005(3) O9 0.110(4) 0.036(2) 0.070(3) 0.002(3) 0.005(3) -0.006(3) C10 0.075(4) 0.037(3) 0.045(3) 0.004(3) -0.007(3) -0.003(3) N11 0.073(3) 0.035(2) 0.039(3) 0.002(2) -0.002(2) -0.006(2) C12 0.069(3) 0.029(2) 0.036(3) -0.001(2) -0.002(2) -0.001(2) C19 0.078(5) 0.038(3) 0.056(4) -0.005(3) 0.001(3) -0.003(3) C20 0.054(3) 0.047(3) 0.052(4) 0.001(3) 0.001(3) -0.006(3) C21 0.066(4) 0.057(4) 0.054(4) -0.010(3) -0.005(3) -0.011(3) C22 0.076(5) 0.070(6) 0.060(4) -0.003(4) -0.005(4) -0.015(4) C23 0.080(5) 0.082(6) 0.045(4) 0.010(4) -0.004(3) -0.009(4) C24 0.073(5) 0.084(6) 0.062(4) 0.009(4) -0.013(4) 0.001(4) C25 0.074(5) 0.060(4) 0.068(5) 0.006(4) -0.004(4) 0.002(4) C26 0.091(5) 0.059(4) 0.043(3) 0.011(3) 0.003(3) -0.012(4) C27 0.097(6) 0.074(6) 0.054(4) 0.006(4) 0.002(4) -0.013(5) C28 0.086(5) 0.065(5) 0.045(3) 0.016(3) -0.016(3) -0.004(4) O29 0.070(3) 0.036(2) 0.066(3) -0.005(2) -0.016(2) -0.004(2) C30 0.083(5) 0.051(5) 0.104(7) -0.007(4) -0.040(5) -0.015(4) C31 0.064(4) 0.038(3) 0.036(3) 0.002(2) -0.001(2) -0.004(3) O32 0.068(3) 0.042(3) 0.069(3) 0.006(2) -0.007(2) 0.007(2) C33 0.068(4) 0.035(3) 0.044(3) 0.000(2) -0.004(3) -0.008(3) N34 0.056(3) 0.037(3) 0.038(2) -0.0036(19) -0.006(2) -0.006(2) C35 0.065(4) 0.031(3) 0.043(3) -0.006(2) -0.004(3) -0.005(3) C36 0.052(3) 0.034(3) 0.039(3) -0.001(2) -0.004(2) -0.005(2) C37 0.063(4) 0.045(3) 0.044(3) -0.006(3) -0.003(3) -0.005(3) C38 0.064(4) 0.062(4) 0.043(3) 0.002(3) -0.007(3) -0.013(3) C39 0.076(5) 0.072(5) 0.040(3) -0.015(3) -0.004(3) -0.012(4) C40 0.102(6) 0.046(4) 0.048(4) -0.015(3) 0.005(4) -0.007(4) C41 0.067(4) 0.039(3) 0.045(3) -0.002(3) -0.001(3) -0.004(3) C42 0.055(3) 0.040(3) 0.068(4) -0.018(3) 0.003(3) -0.005(2) C43 0.048(5) 0.039(5) 0.067(6) -0.026(5) 0.003(5) -0.011(5) C44 0.054(4) 0.045(4) 0.073(4) -0.025(3) 0.007(3) -0.007(3) C45 0.044(6) 0.039(6) 0.070(7) -0.025(6) 0.003(6) -0.014(5) C46 0.062(4) 0.054(4) 0.086(5) -0.024(4) 0.007(4) -0.006(4) C47 0.047(7) 0.047(7) 0.074(8) -0.025(7) 0.006(6) -0.014(6) C48 0.065(5) 0.065(5) 0.093(5) -0.026(4) 0.011(4) -0.008(4) C49 0.053(7) 0.046(7) 0.068(8) -0.032(7) 0.004(7) -0.012(6) C50 0.061(4) 0.071(5) 0.085(5) -0.030(4) 0.012(4) -0.006(4) C51 0.053(7) 0.047(7) 0.068(8) -0.035(7) 0.005(7) -0.010(6) C52 0.066(4) 0.069(5) 0.068(5) -0.025(4) 0.011(4) -0.006(4) C53 0.061(4) 0.059(5) 0.064(4) -0.026(4) 0.005(4) -0.004(4) C54 0.049(7) 0.042(7) 0.064(7) -0.033(6) 0.003(6) -0.013(6) C55 0.073(4) 0.040(3) 0.047(3) -0.007(3) -0.012(3) -0.010(3) C56 0.087(5) 0.050(4) 0.039(3) -0.003(3) -0.003(3) -0.007(4) C57 0.121(7) 0.054(4) 0.035(3) -0.002(3) 0.000(3) -0.030(4) C130 0.067(5) 0.032(4) 0.040(4) -0.002(3) -0.001(4) 0.002(4) C131 0.053(8) 0.045(7) 0.036(6) -0.001(6) -0.003(5) 0.002(6) C140 0.051(8) 0.046(8) 0.041(7) 0.012(6) -0.002(6) 0.013(6) C141 0.066(5) 0.036(5) 0.040(4) 0.002(4) -0.005(4) 0.009(4) C150 0.067(9) 0.062(10) 0.059(8) 0.018(8) 0.011(7) 0.009(9) C151 0.066(5) 0.042(6) 0.043(4) 0.003(4) -0.002(4) 0.009(5) C160 0.070(6) 0.042(6) 0.043(4) 0.005(4) -0.006(4) 0.014(5) C161 0.045(7) 0.054(10) 0.035(6) 0.003(7) -0.003(5) 0.004(8) C170 0.072(6) 0.039(5) 0.046(4) 0.003(4) -0.002(4) 0.011(5) C171 0.062(9) 0.043(9) 0.065(10) 0.020(8) 0.008(7) 0.021(8) C180 0.071(6) 0.031(4) 0.043(5) -0.001(4) -0.001(4) 0.008(4) C181 0.072(10) 0.048(8) 0.045(9) 0.007(8) 0.004(7) 0.004(9) Cl2 0.0683(9) 0.0385(7) 0.0521(7) -0.0014(6) 0.0041(6) 0.0009(7) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.3639 0.7018 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 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_publ_flag Cl3 C4 Cl5 109.88(7) yes Cl3 C4 H41 109.2 no Cl5 C4 H41 109.8 no Cl3 C4 H42 108.9 no Cl5 C4 H42 109.7 no H41 C4 H42 109.3 no C7 O6 C8 115.0(7) yes O6 C7 H72 109.1 no O6 C7 H73 108.7 no H72 C7 H73 109.9 no O6 C7 H71 109.4 no H72 C7 H71 110.2 no H73 C7 H71 109.5 no O6 C8 O9 126.4(7) yes O6 C8 C10 111.5(7) yes O9 C8 C10 122.1(7) yes C8 C10 N11 110.8(6) yes C8 C10 C28 111.6(6) yes N11 C10 C28 105.4(6) yes C8 C10 H101 108.7 no N11 C10 H101 109.9 no C28 C10 H101 110.4 no C10 N11 C12 112.3(5) yes C10 N11 C26 106.8(5) yes C12 N11 C26 113.7(5) yes C10 N11 H111 108.3(16) no C12 N11 H111 108.3(15) no C26 N11 H111 107.2(16) no N11 C12 C19 112.1(5) yes N11 C12 C131 111.2(10) yes C19 C12 C131 115.8(9) yes N11 C12 H121 105.9 no C19 C12 H121 106.0 no C131 C12 H121 104.9 no N11 C12 C19 112.1(5) yes N11 C12 C130 108.7(7) yes C19 C12 C130 111.2(8) yes N11 C12 H122 108.6 no C19 C12 H122 108.7 no C130 C12 H122 107.3 no C12 C19 C20 111.3(6) yes C12 C19 H191 108.9 no C20 C19 H191 109.9 no C12 C19 H192 108.0 no C20 C19 H192 109.2 no H191 C19 H192 109.5 no C19 C20 C21 121.0(6) yes C19 C20 C25 121.3(7) yes C21 C20 C25 117.7(7) yes C20 C21 C22 122.6(8) yes C20 C21 H211 118.9 no C22 C21 H211 118.5 no C21 C22 C23 117.9(8) yes C21 C22 H221 121.6 no C23 C22 H221 120.5 no C22 C23 C24 120.9(8) yes C22 C23 H231 119.3 no C24 C23 H231 119.8 no C23 C24 C25 119.0(8) yes C23 C24 H241 121.1 no C25 C24 H241 119.9 no C24 C25 C20 121.9(8) yes C24 C25 H251 119.3 no C20 C25 H251 118.8 no N11 C26 C27 102.7(6) yes N11 C26 H261 110.8 no C27 C26 H261 111.7 no N11 C26 H262 109.7 no C27 C26 H262 111.5 no H261 C26 H262 110.2 no C26 C27 C28 104.7(7) yes C26 C27 H271 111.2 no C28 C27 H271 111.6 no C26 C27 H272 109.7 no C28 C27 H272 110.3 no H271 C27 H272 109.2 no C10 C28 C27 105.0(7) yes C10 C28 H281 109.3 no C27 C28 H281 111.0 no C10 C28 H282 111.0 no C27 C28 H282 110.7 no H281 C28 H282 109.8 no C30 O29 C31 115.1(6) yes O29 C30 H301 108.9 no O29 C30 H302 109.2 no H301 C30 H302 109.8 no O29 C30 H303 108.8 no H301 C30 H303 109.8 no H302 C30 H303 110.4 no O29 C31 O32 124.6(6) yes O29 C31 C33 109.4(5) yes O32 C31 C33 125.8(6) yes C31 C33 N34 111.6(5) yes C31 C33 C57 110.2(7) yes N34 C33 C57 106.0(5) yes C31 C33 H331 108.9 no N34 C33 H331 110.7 no C57 C33 H331 109.5 no C33 N34 C35 111.7(5) yes C33 N34 C55 104.5(5) yes C35 N34 C55 114.2(5) yes C33 N34 H341 109.0(16) no C35 N34 H341 108.0(15) no C55 N34 H341 109.3(16) no N34 C35 C36 109.5(5) yes N34 C35 C42 110.3(5) yes C36 C35 C42 113.5(5) yes N34 C35 H351 109.3 no C36 C35 H351 107.5 no C42 C35 H351 106.6 no C35 C36 C37 122.2(6) yes C35 C36 C41 117.9(6) yes C37 C36 C41 119.8(6) yes C36 C37 C38 120.2(6) yes C36 C37 H371 120.1 no C38 C37 H371 119.7 no C37 C38 C39 118.2(7) yes C37 C38 H381 120.5 no C39 C38 H381 121.2 no C38 C39 C40 121.3(6) yes C38 C39 H391 119.3 no C40 C39 H391 119.3 no C39 C40 C41 120.9(7) yes C39 C40 H401 119.8 no C41 C40 H401 119.3 no C40 C41 C36 119.5(7) yes C40 C41 H411 119.8 no C36 C41 H411 120.7 no C35 C42 C43 109.1(7) yes C35 C42 H422 125.3 no C43 C42 H422 125.6 no C35 C42 C44 112.1(5) yes C35 C42 H421 109.0 no C44 C42 H421 108.6 no C35 C42 H423 109.0 no C44 C42 H423 108.7 no H421 C42 H423 109.5 no C42 C43 C45 120.08(7) yes C42 C43 C54 120.07(7) yes C45 C43 C54 119.58(7) yes C42 C44 C46 120.56(6) yes C42 C44 C53 120.55(6) yes C46 C44 C53 118.84(6) yes C43 C45 C47 118.98(7) yes C43 C45 H451 120.4 no C47 C45 H451 120.7 no C44 C46 C48 121.08(6) yes C44 C46 H461 119.1 no C48 C46 H461 119.8 no C45 C47 C49 114.23(7) yes C45 C47 H471 122.8 no C49 C47 H471 123.0 no C46 C48 C50 118.82(6) yes C46 C48 H483 120.6 no C50 C48 H483 120.6 no C47 C49 C51 131.86(7) yes C47 C49 H491 113.9 no C51 C49 H491 114.2 no C48 C50 C52 121.24(6) yes C48 C50 H501 119.4 no C52 C50 H501 119.3 no C49 C51 C54 114.24(7) yes C49 C51 H511 122.7 no C54 C51 H511 123.1 no C50 C52 C53 118.81(6) yes C50 C52 H521 121.1 no C53 C52 H521 120.1 no C52 C53 C44 121.09(6) yes C52 C53 H531 119.1 no C44 C53 H531 119.8 no C51 C54 C43 118.99(7) yes C51 C54 H541 120.5 no C43 C54 H541 120.5 no N34 C55 C56 102.0(5) yes N34 C55 H551 109.8 no C56 C55 H551 112.1 no N34 C55 H552 110.8 no C56 C55 H552 111.5 no H551 C55 H552 110.3 no C55 C56 C57 105.2(6) yes C55 C56 H562 110.9 no C57 C56 H562 110.6 no C55 C56 H561 110.4 no C57 C56 H561 110.8 no H562 C56 H561 109.0 no C56 C57 C33 103.5(6) yes C56 C57 H572 111.7 no C33 C57 H572 111.3 no C56 C57 H571 110.9 no C33 C57 H571 110.4 no H572 C57 H571 108.9 no C12 C130 C141 122.11(7) yes C12 C130 C180 122.12(7) yes C141 C130 C180 115.70(6) yes C12 C131 C140 118.61(6) yes C12 C131 C181 118.62(6) yes C140 C131 C181 122.77(6) yes C131 C140 C150 119.71(7) yes C131 C140 H1401 119.9 no C150 C140 H1401 120.4 no C130 C141 C151 123.21(6) yes C130 C141 H1411 118.0 no C151 C141 H1411 118.8 no C140 C150 C161 117.76(7) yes C140 C150 H1501 120.9 no C161 C150 H1501 121.3 no C141 C151 C160 118.45(6) yes C141 C151 H1511 121.0 no C160 C151 H1511 120.5 no C151 C160 C170 120.88(6) yes C151 C160 H1601 119.7 no C170 C160 H1601 119.4 no C150 C161 C171 121.51(7) yes C150 C161 H1611 119.6 no C171 C161 H1611 118.9 no C160 C170 C180 118.45(6) yes C160 C170 H1701 121.1 no C180 C170 H1701 120.5 no C161 C171 C181 117.76(7) yes C161 C171 H1711 121.1 no C181 C171 H1711 121.1 no C130 C180 C170 123.21(6) yes C130 C180 H1801 118.3 no C170 C180 H1801 118.5 no C171 C181 C131 119.71(7) yes C171 C181 H1811 120.0 no C131 C181 H1811 120.2 no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Cl3 C4 1.755(5) yes C4 Cl5 1.735(5) yes C4 H41 0.974 no C4 H42 0.972 no O6 C7 1.454(11) yes O6 C8 1.311(10) yes C7 H72 0.961 no C7 H73 0.957 no C7 H71 0.956 no C8 O9 1.207(10) yes C8 C10 1.545(9) yes C10 N11 1.499(9) yes C10 C28 1.547(9) yes C10 H101 0.982 no N11 C12 1.517(7) yes N11 C26 1.494(9) yes N11 H111 0.894(19) no C12 C19 1.516(10) yes C12 C131 1.493(6) yes C12 H121 0.979 no C12 C19 1.516(10) yes C12 C130 1.530(6) yes C12 H122 0.980 no C19 C20 1.514(9) yes C19 H191 0.969 no C19 H192 0.969 no C20 C21 1.382(10) yes C20 C25 1.388(10) yes C21 C22 1.400(10) yes C21 H211 0.933 no C22 C23 1.407(12) yes C22 H221 0.947 no C23 C24 1.381(14) yes C23 H231 0.938 no C24 C25 1.400(12) yes C24 H241 0.938 no C25 H251 0.933 no C26 C27 1.506(12) yes C26 H261 0.968 no C26 H262 0.985 no C27 C28 1.520(13) yes C27 H271 0.978 no C27 H272 0.972 no C28 H281 0.975 no C28 H282 0.966 no O29 C30 1.462(8) yes O29 C31 1.339(8) yes C30 H301 0.966 no C30 H302 0.961 no C30 H303 0.967 no C31 O32 1.195(8) yes C31 C33 1.499(9) yes C33 N34 1.513(8) yes C33 C57 1.561(10) yes C33 H331 0.968 no N34 C35 1.538(8) yes N34 C55 1.494(7) yes N34 H341 0.889(19) no C35 C36 1.520(8) yes C35 C42 1.521(9) yes C35 H351 0.981 no C36 C37 1.393(9) yes C36 C41 1.378(9) yes C37 C38 1.396(9) yes C37 H371 0.924 no C38 C39 1.407(12) yes C38 H381 0.936 no C39 C40 1.327(12) yes C39 H391 0.920 no C40 C41 1.402(9) yes C40 H401 0.934 no C41 H411 0.941 no C42 C43 1.406(6) yes C42 H422 0.930 no C42 C44 1.545(6) yes C42 H421 0.970 no C42 H423 0.974 no C43 C45 1.412(6) yes C43 C54 1.412(6) yes C44 C46 1.401(5) yes C44 C53 1.405(5) yes C45 C47 1.448(6) yes C45 H451 0.928 no C46 C48 1.421(5) yes C46 H461 0.927 no C47 C49 1.305(6) yes C47 H471 0.930 no C48 C50 1.402(5) yes C48 H483 0.928 no C49 C51 1.301(6) yes C49 H491 0.929 no C50 C52 1.401(5) yes C50 H501 0.938 no C51 C54 1.449(6) yes C51 H511 0.928 no C52 C53 1.419(5) yes C52 H521 0.933 no C53 H531 0.928 no C54 H541 0.929 no C55 C56 1.510(11) yes C55 H551 0.970 no C55 H552 0.969 no C56 C57 1.527(10) yes C56 H562 0.971 no C56 H561 0.970 no C57 H572 0.970 no C57 H571 0.976 no C130 C141 1.421(5) yes C130 C180 1.424(5) yes C131 C140 1.374(5) yes C131 C181 1.379(5) yes C140 C150 1.390(6) yes C140 H1401 0.935 no C141 C151 1.380(5) yes C141 H1411 0.929 no C150 C161 1.420(6) yes C150 H1501 0.934 no C151 C160 1.416(5) yes C151 H1511 0.933 no C160 C170 1.413(5) yes C160 H1601 0.935 no C161 C171 1.422(5) yes C161 H1611 0.938 no C170 C180 1.378(5) yes C170 H1701 0.935 no C171 C181 1.391(6) yes C171 H1711 0.930 no C180 H1801 0.930 no C181 H1811 0.931 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C24 H241 O32 2_545 156 0.94 2.58 3.457(15) yes