#------------------------------------------------------------------------------ #$Date: 2016-04-02 22:24:05 +0300 (Sat, 02 Apr 2016) $ #$Revision: 180860 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/2/01/91/2019118.hkl $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2019118_Fobs loop_ _publ_author_name 'Sirianni, Eric R.' 'Yap, Glenn P. A.' 'Akturk, Eser S.' 'Theopold, Klaus H.' _publ_section_title ; Improved syntheses, and structural and electronic characterization of carboxamide-substituted Tp^CONHPh,Me^ and Tp^CONHt^-Bu,Me ligands ; _journal_coeditor_code EG3122 _journal_issue 9 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 947 _journal_page_last 953 _journal_volume 69 _journal_year 2013 _space_group_IT_number 88 _symmetry_space_group_name_Hall '-I 4ad' _symmetry_space_group_name_H-M 'I 41/a :2' _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_length_a 30.2283 _cell_length_b 30.2283 _cell_length_c 14.3753 _exptl_crystal_F_000 6432.00 _reflns_d_resolution_high 0.8197 _cod_data_source_file eg3122IIsup2.hkl _cod_data_source_block II #BEGIN Tags that were not found in dictionaries: _shelx_title ' kla0195 in I4(1)/a' _shelx_refln_list_code 4 _shelx_f_calc_maximum 1105.74 _shelx_f_squared_multiplier 1.000 #END Tags that were not found in dictionaries loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_calc _refln_F_squared_meas _refln_F_squared_sigma _refln_observed_status 0 2 0 323355.00 341834.03 3735.03 o 2 2 0 227378.44 249971.03 5046.10 o 0 4 0 4829.39 3427.10 133.78 o 2 4 0 43764.91 50326.11 1254.78 o 4 4 0 687703.12 739996.31 14747.04 o -4 6 0 350088.22 366782.56 16318.89 o -2 6 0 136541.23 137675.41 5862.39 o 0 6 0 648003.75 673210.38 7404.42 o 2 6 0 1222667.00 1318065.12 12368.19 o 4 6 0 8057.65 10294.59 553.18 o 6 6 0 58761.33 52140.37 1416.69 o -6 8 0 69139.00 71549.02 852.38 o -4 8 0 98684.57 92124.82 1736.43 o -2 8 0 177538.42 187263.86 2296.03 o 0 8 0 160379.52 167978.58 1908.49 o 2 8 0 1245.85 1420.10 384.63 o 4 8 0 1026571.38 1077764.88 38210.08 o 6 8 0 729897.56 759221.62 9538.91 o 8 8 0 7.46 -111.36 111.36 o -8 10 0 303249.62 303578.28 2495.18 o -6 10 0 101750.66 102694.10 923.85 o -4 10 0 906.49 1244.22 137.49 o -2 10 0 624130.81 655217.75 10319.56 o 0 10 0 82464.76 84813.33 1707.45 o 2 10 0 18339.36 19190.67 439.84 o 4 10 0 242300.08 238098.03 4213.72 o 6 10 0 8675.59 8438.64 254.54 o 8 10 0 721331.81 773227.06 5900.50 o 10 10 0 96066.59 102541.52 1051.62 o -10 12 0 40811.83 41812.26 568.26 o -8 12 0 69055.46 71016.88 1134.62 o -6 12 0 60231.49 65481.71 882.87 o -4 12 0 547411.25 555925.00 4023.45 o -2 12 0 2882.90 3051.18 152.44 o 0 12 0 40424.66 38977.14 584.54 o 2 12 0 758067.06 780917.25 8351.14 o 4 12 0 9551.89 9708.61 293.96 o 6 12 0 12569.04 12481.90 344.56 o 8 12 0 406271.75 420155.84 3375.39 o 10 12 0 32461.92 37016.84 632.12 o 12 12 0 70829.32 72948.02 1087.21 o -12 14 0 24143.99 24651.90 597.15 o -10 14 0 375403.91 385666.47 3003.42 o -8 14 0 48128.40 50765.33 638.66 o -6 14 0 19838.66 20933.74 390.26 o -4 14 0 239086.30 231084.12 2489.24 o -2 14 0 15667.46 17394.53 374.14 o 0 14 0 98622.44 101597.73 1320.33 o 2 14 0 153969.69 163065.06 3139.02 o 4 14 0 109830.22 113411.38 2088.74 o 6 14 0 786081.81 829210.31 8663.38 o 8 14 0 103654.29 108303.20 1255.14 o 10 14 0 63110.14 65681.67 857.62 o 12 14 0 270793.16 271690.12 2388.12 o 14 14 0 4995.03 5121.34 275.59 o -14 16 0 14713.99 14981.84 651.07 o -12 16 0 21034.03 20646.48 537.25 o -10 16 0 60027.64 57550.38 729.11 o -8 16 0 47950.91 45437.79 730.52 o -6 16 0 628847.19 645173.62 8511.30 o -4 16 0 69811.06 75075.17 901.74 o -2 16 0 32858.26 30757.47 449.21 o 0 16 0 584844.81 592261.31 8776.34 o 2 16 0 1790.97 1905.43 186.40 o 4 16 0 202.64 199.45 155.97 o 6 16 0 52842.48 52232.00 821.34 o 8 16 0 129556.39 137985.38 1378.77 o 10 16 0 188286.64 197288.62 1842.64 o 12 16 0 77.83 20.22 155.82 o 14 16 0 70228.08 65046.75 864.85 o 16 16 0 231367.64 221303.28 4174.31 o -16 18 0 8239.57 8080.15 453.27 o -14 18 0 34969.58 32470.02 769.28 o -12 18 0 339569.16 334156.56 2904.27 o -10 18 0 10771.35 11568.97 361.59 o -8 18 0 3996.64 3829.85 284.51 o -6 18 0 130521.01 130068.59 1775.40 o -4 18 0 10920.36 10982.56 360.99 o -2 18 0 78328.12 77044.38 1245.28 o 0 18 0 15915.07 18134.95 416.00 o 2 18 0 204552.19 208772.44 4455.05 o 4 18 0 283845.75 287602.22 7402.81 o 6 18 0 15885.21 18947.71 462.62 o 8 18 0 7014.48 6839.21 329.17 o 10 18 0 163246.39 159306.58 1989.18 o 12 18 0 31309.02 30142.68 630.18 o 14 18 0 24370.23 24579.60 579.17 o 16 18 0 5497.69 5393.80 391.44 o 18 18 0 141174.75 143176.27 1630.97 o -18 20 0 56355.13 54742.03 885.94 o -16 20 0 185.82 -170.58 215.80 o -14 20 0 57120.39 56548.56 1333.72 o -12 20 0 30043.39 30428.41 1057.46 o -10 20 0 93124.77 87076.67 1435.07 o -8 20 0 226659.50 220376.98 2253.40 o -6 20 0 824.55 821.65 193.49 o -4 20 0 79465.71 80615.88 1443.06 o -2 20 0 228908.70 234167.33 3884.20 o 0 20 0 44361.44 45488.41 872.91 o 2 20 0 51382.63 52630.93 1497.07 o 4 20 0 47424.91 46334.07 1039.09 o 6 20 0 229614.77 223054.88 3408.29 o 8 20 0 127472.94 120219.27 2456.66 o 10 20 0 3639.81 3138.43 344.70 o 12 20 0 111068.06 109449.95 1785.15 o 14 20 0 61731.72 55915.75 1779.57 o 16 20 0 18745.59 19450.98 601.95 o 18 20 0 7945.14 8307.24 396.30 o 20 20 0 63.29 78.33 174.26 o -20 22 0 73783.56 75011.30 953.83 o -18 22 0 5302.99 4722.01 364.34 o -16 22 0 10047.52 9323.08 412.58 o -14 22 0 192035.77 184415.95 1958.55 o -12 22 0 13860.44 12029.70 544.02 o -10 22 0 100.45 529.60 232.50 o -8 22 0 39391.77 35665.20 789.55 o -6 22 0 81534.39 75307.43 1977.18 o -4 22 0 58082.58 57218.66 987.43 o -2 22 0 1474.23 1466.90 349.46 o 0 22 0 168723.38 160778.69 2494.86 o 2 22 0 123261.56 113874.96 1589.42 o 4 22 0 18635.42 18416.65 543.54 o 6 22 0 10129.30 9740.88 449.24 o 8 22 0 2134.93 1425.05 254.82 o 10 22 0 105525.38 100199.91 2342.90 o 12 22 0 57278.95 53983.57 2054.85 o 14 22 0 21447.37 21653.10 1206.78 o 16 22 0 100636.52 100189.39 2487.99 o 18 22 0 19270.91 20876.19 565.10 o 20 22 0 3389.26 3265.64 248.29 o 22 22 0 20657.18 21711.52 453.46 o -22 24 0 1531.85 1279.37 218.18 o -20 24 0 31804.99 33294.04 739.61 o -18 24 0 43046.74 44573.74 742.55 o -16 24 0 34189.73 33242.97 565.83 o -14 24 0 5161.58 4763.33 271.74 o -12 24 0 80594.61 77442.85 1080.78 o -10 24 0 94971.56 90319.37 1246.55 o -8 24 0 77.79 186.07 193.20 o -6 24 0 26695.94 26734.01 777.78 o -4 24 0 16531.86 16064.02 631.77 o -2 24 0 86227.48 79950.16 1489.05 o 0 24 0 7392.85 7017.32 400.22 o 2 24 0 951.85 405.51 210.30 o 4 24 0 173534.11 163552.59 1955.31 o 6 24 0 36323.04 34257.72 770.67 o 8 24 0 32.14 -55.54 255.41 o 10 24 0 51077.85 49681.20 2414.38 o 12 24 0 229.40 469.48 230.44 o 14 24 0 10006.05 10549.42 468.46 o 16 24 0 5665.15 5578.01 267.60 o 18 24 0 342.15 408.09 162.45 o 20 24 0 52808.80 54878.68 810.20 o 22 24 0 7546.62 7496.15 352.98 o 24 24 0 3145.85 3431.48 230.59 o -24 26 0 27687.14 29611.62 1038.90 o -22 26 0 23298.77 26009.80 560.04 o -20 26 0 70.45 189.07 210.16 o -18 26 0 34039.12 33054.98 597.89 o -16 26 0 11421.10 12885.17 346.04 o -14 26 0 20698.46 20132.72 476.77 o -12 26 0 1975.33 2063.60 235.30 o -10 26 0 5926.73 6420.18 304.16 o -8 26 0 105661.13 100904.25 1091.24 o -6 26 0 32983.52 30328.46 603.00 o -4 26 0 7584.22 7485.39 313.32 o -2 26 0 110173.45 105165.57 1569.45 o 0 26 0 9386.68 9637.01 526.63 o 2 26 0 52786.05 47951.89 1320.48 o 4 26 0 875.32 892.76 222.67 o 6 26 0 11792.56 10461.90 390.72 o 8 26 0 115769.58 111542.23 2522.18 o 10 26 0 8876.15 8152.01 399.75 o 12 26 0 6493.52 6395.66 276.63 o 14 26 0 69378.23 65820.87 2471.82 o 16 26 0 2962.59 2884.19 216.06 o 18 26 0 1597.12 1360.00 197.28 o 20 26 0 8960.47 9165.72 351.03 o 22 26 0 2093.30 1826.99 199.95 o 24 26 0 28652.48 31576.10 974.12 o -22 28 0 1531.92 1578.59 458.74 o -20 28 0 35530.77 37340.15 1452.88 o -18 28 0 11644.26 12195.10 351.17 o -16 28 0 861.63 984.22 224.56 o -14 28 0 57192.63 57728.14 785.97 o -12 28 0 15202.54 15471.38 394.82 o -10 28 0 16185.31 14983.37 385.32 o -8 28 0 15994.30 16727.59 433.48 o -6 28 0 9.66 446.35 187.98 o -4 28 0 75503.12 75253.30 768.20 o -2 28 0 231.41 337.20 151.43 o 0 28 0 5211.13 4917.71 244.48 o 2 28 0 108936.96 104503.05 1788.65 o 4 28 0 9213.40 9038.41 380.39 o 6 28 0 6288.82 6821.97 322.57 o 8 28 0 32236.38 29995.42 514.70 o 10 28 0 183.61 -68.21 161.87 o 12 28 0 26867.27 27881.89 953.80 o 14 28 0 6690.69 6445.35 388.21 o 16 28 0 18962.65 19278.35 634.11 o 18 28 0 32451.79 35401.23 1032.44 o 20 28 0 1129.62 1178.71 206.99 o 22 28 0 27.27 -115.85 472.23 o -18 30 0 1247.36 1191.96 220.60 o -16 30 0 21843.86 22546.13 484.07 o -14 30 0 1080.49 980.20 189.45 o -12 30 0 7039.52 7246.58 270.09 o -10 30 0 63252.43 66486.72 772.41 o -8 30 0 5127.64 4205.85 290.68 o -6 30 0 2510.27 3132.11 218.64 o -4 30 0 42785.05 44710.60 977.58 o -2 30 0 10193.60 9447.42 295.25 o 0 30 0 37205.80 37437.02 670.68 o 2 30 0 1328.76 796.08 161.14 o 4 30 0 35728.09 38094.87 710.97 o 6 30 0 69394.23 69255.55 1565.86 o 8 30 0 3090.70 2938.75 222.75 o 10 30 0 1551.52 1699.08 290.31 o 12 30 0 21069.06 22189.18 441.19 o 14 30 0 2209.41 2630.78 234.69 o 16 30 0 3136.33 3364.22 222.57 o 18 30 0 126.74 65.92 169.14 o 20 30 0 5450.58 5676.89 836.52 o -16 32 0 18583.58 22059.84 1106.36 o -14 32 0 3020.12 3555.48 333.01 o -12 32 0 17673.84 18570.42 439.47 o -10 32 0 3566.29 3807.83 323.82 o -8 32 0 5901.27 6394.77 284.50 o -6 32 0 41677.21 44376.36 577.53 o -4 32 0 2182.32 2255.36 197.31 o -2 32 0 14375.98 15422.28 408.10 o 0 32 0 26496.92 27281.98 575.04 o 2 32 0 206.04 100.36 166.81 o 4 32 0 1940.62 1765.09 254.81 o 6 32 0 7831.22 7579.08 274.08 o 8 32 0 9176.18 10947.07 313.17 o 10 32 0 49595.22 51956.05 2659.56 o 12 32 0 1491.12 1490.90 186.67 o 14 32 0 16495.30 19164.34 1168.38 o 16 32 0 27415.72 27713.10 1133.35 o -12 34 0 23174.77 24403.11 777.15 o -10 34 0 185.89 96.09 209.47 o -8 34 0 184.88 -141.07 230.29 o -6 34 0 10527.84 12225.74 382.29 o -4 34 0 6662.90 6447.25 378.37 o -2 34 0 18396.37 18435.35 490.76 o 0 34 0 54.78 227.63 176.73 o 2 34 0 14911.23 17338.26 501.49 o 4 34 0 16468.29 19204.01 832.02 o 6 34 0 193.62 181.94 294.12 o 8 34 0 504.05 1146.84 331.96 o 10 34 0 2925.07 3631.90 299.57 o 12 34 0 15727.21 16547.12 877.00 o -6 36 0 182.24 0.00 364.29 o -4 36 0 3465.00 5100.07 620.64 o -2 36 0 3984.21 3574.39 694.85 o 0 36 0 8167.55 7694.37 522.39 o 2 36 0 1211.95 550.56 318.65 o 4 36 0 586.30 323.81 445.24 o 6 36 0 22473.03 22059.84 1092.87 o 0 1 1 176024.27 194105.17 1895.60 o -1 2 1 1011708.06 1089140.50 9129.28 o 1 2 1 102615.40 113924.43 1910.92 o -2 3 1 87381.76 89196.48 827.85 o 0 3 1 14820.25 16996.03 289.60 o 2 3 1 245749.95 270364.78 2341.01 o -3 4 1 110347.88 117766.75 1239.28 o -1 4 1 1427.00 1331.99 120.04 o 1 4 1 312224.34 335464.91 3203.72 o 3 4 1 155212.78 162969.50 1498.94 o -4 5 1 12852.26 11524.38 305.53 o -2 5 1 83630.01 95087.04 2453.58 o 0 5 1 107306.59 115128.84 5579.05 o 2 5 1 96891.34 100783.48 988.73 o 4 5 1 141218.34 158788.17 1912.07 o -5 6 1 272832.66 286249.69 5089.48 o -3 6 1 9838.87 10020.63 248.88 o -1 6 1 90.03 170.75 89.28 o 1 6 1 111071.28 117747.51 1725.60 o 3 6 1 10670.05 9689.14 223.63 o 5 6 1 3919.24 3842.39 161.33 o -6 7 1 66836.16 74293.29 914.14 o -4 7 1 1142391.75 1264093.50 11345.48 o -2 7 1 271564.84 301957.59 5185.16 o 0 7 1 179561.23 187718.45 2960.27 o 2 7 1 52735.85 48383.43 909.11 o 4 7 1 234244.19 239225.69 4215.51 o 6 7 1 270157.81 296176.88 5437.25 o -7 8 1 115412.92 115465.43 867.41 o -5 8 1 218175.44 222697.77 2637.95 o -3 8 1 53229.09 58547.75 894.05 o -1 8 1 578621.56 609245.88 4926.25 o 1 8 1 360289.09 376777.34 4964.88 o 3 8 1 293.40 718.89 116.66 o 5 8 1 1492.06 1832.20 121.19 o 7 8 1 36618.11 38110.85 372.70 o -8 9 1 113397.10 114698.73 740.80 o -6 9 1 181551.97 187268.33 1162.86 o -4 9 1 62119.00 55727.48 733.34 o -2 9 1 115711.83 129473.05 2981.65 o 0 9 1 354126.25 379456.97 3934.46 o 2 9 1 17700.21 15572.00 468.31 o 4 9 1 64885.94 62049.52 1072.28 o 6 9 1 494472.28 517154.75 3669.40 o 8 9 1 123454.63 132461.95 800.93 o -9 10 1 2416.26 2475.96 121.72 o -7 10 1 126931.96 129777.23 818.21 o -5 10 1 82347.09 92749.80 659.52 o -3 10 1 57467.00 60287.17 492.20 o -1 10 1 65079.15 68646.99 830.21 o 1 10 1 83084.55 80881.29 775.22 o 3 10 1 356034.06 355361.56 3441.33 o 5 10 1 162245.84 162365.23 1037.91 o 7 10 1 28066.66 27386.71 291.40 o 9 10 1 71643.70 70198.76 550.97 o -10 11 1 45489.46 43300.79 587.14 o -8 11 1 100733.06 113920.23 831.21 o -6 11 1 158929.78 160729.11 988.83 o -4 11 1 75.44 245.12 74.73 o -2 11 1 17529.00 17113.99 200.19 o 0 11 1 256908.38 252023.75 2340.08 o 2 11 1 636.43 829.81 79.72 o 4 11 1 23646.31 22753.15 256.27 o 6 11 1 253520.12 264596.50 1495.33 o 8 11 1 2334.28 2391.06 130.03 o 10 11 1 137335.09 138638.89 906.69 o -11 12 1 2780.64 2367.92 157.43 o -9 12 1 214656.94 209367.31 1479.50 o -7 12 1 83015.66 82403.82 604.94 o -5 12 1 8403.11 8400.76 193.85 o -3 12 1 280265.09 289952.66 1807.81 o -1 12 1 52177.02 55557.61 704.90 o 1 12 1 9592.71 10226.85 175.60 o 3 12 1 32696.88 32003.34 344.55 o 5 12 1 36734.40 38194.26 370.02 o 7 12 1 290621.69 301179.03 1763.81 o 9 12 1 149204.62 161002.11 1120.99 o 11 12 1 67440.61 65811.14 569.47 o -12 13 1 135030.47 133276.67 952.75 o -10 13 1 3332.40 3179.97 146.46 o -8 13 1 104537.66 109162.08 981.42 o -6 13 1 145665.70 143635.80 1117.17 o -4 13 1 9194.47 10030.54 200.11 o -2 13 1 175524.86 182288.73 1091.22 o 0 13 1 75216.55 78441.63 851.53 o 2 13 1 1723.79 1936.39 109.32 o 4 13 1 453916.22 473878.59 3096.14 o 6 13 1 9808.66 10728.88 223.17 o 8 13 1 246.53 373.50 96.91 o 10 13 1 186643.59 194593.91 1211.93 o 12 13 1 1191.18 997.96 150.98 o -13 14 1 22411.18 22840.55 378.02 o -11 14 1 5134.27 4636.41 173.58 o -9 14 1 12291.77 12861.95 238.03 o -7 14 1 22426.10 24867.19 293.37 o -5 14 1 142592.98 142222.30 1230.38 o -3 14 1 80711.80 85392.70 671.68 o -1 14 1 40306.54 39840.31 363.26 o 1 14 1 365953.03 376053.28 3165.84 o 3 14 1 121410.09 124144.12 1234.50 o 5 14 1 46902.46 48083.70 465.66 o 7 14 1 19568.08 18833.00 267.62 o 9 14 1 867.28 832.18 112.82 o 11 14 1 30798.96 31230.20 380.22 o 13 14 1 8287.64 8141.15 242.81 o -14 15 1 61557.57 60975.84 656.57 o -12 15 1 13635.95 13532.35 375.64 o -10 15 1 10073.27 11359.47 245.03 o -8 15 1 171258.34 174714.88 1370.49 o -6 15 1 1048.49 973.14 103.97 o -4 15 1 22441.18 24011.22 299.99 o -2 15 1 157815.56 162162.95 1338.90 o 0 15 1 12541.62 13113.87 233.15 o 2 15 1 38026.99 39449.93 431.64 o 4 15 1 71882.26 69828.72 623.94 o 6 15 1 1363.88 1680.13 125.20 o 8 15 1 160171.45 162926.55 1127.75 o 10 15 1 1073.76 1144.81 131.04 o 12 15 1 13195.72 12385.28 288.22 o 14 15 1 96919.43 96185.76 873.09 o -15 16 1 3495.01 3573.84 208.73 o -13 16 1 52676.20 52294.71 601.58 o -11 16 1 124402.09 124669.32 982.86 o -9 16 1 74675.62 79530.09 914.14 o -7 16 1 15374.93 14994.66 252.67 o -5 16 1 27827.12 26747.34 354.22 o -3 16 1 6906.73 7699.88 181.37 o -1 16 1 90626.27 92650.71 1158.36 o 1 16 1 4843.75 5665.95 179.29 o 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