#------------------------------------------------------------------------------ #$Date: 2023-05-06 11:46:54 +0100 (Sat, 06 May 2023) $ #$Revision: 283587 $ #$URL: svn://www.crystallography.net/cod/cif/2/24/42/2244228.cif $ #------------------------------------------------------------------------------ # # 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_2244228 loop_ _publ_author_name 'Wark, Stephen' 'Lyons, Megan J.' 'Slawin, Alexandra M. Z.' 'Harrison, William T. A.' _publ_section_title ; Consistent zincophosphite 4-ring 'ladder' chain structural motif with isomeric ligands. ; _journal_coeditor_code PK2681 _journal_issue 'Pt 4' _journal_name_full 'Acta crystallographica. Section E, Crystallographic communications' _journal_page_first 272 _journal_page_last 279 _journal_paper_doi 10.1107/S2056989023002062 _journal_volume 79 _journal_year 2023 _chemical_formula_iupac '(C6 H9 N2)2 [Zn3 (H P O3)4], H2 O' _chemical_formula_moiety '2(C6 H9 N2 +), H4 O12 P4 Zn3 2-, H2 O' _chemical_formula_sum 'C12 H24 N4 O13 P4 Zn3' _chemical_formula_weight 752.34 _chemical_name_systematic ; Poly[bis(2-amino-4-methylpyridinium) [tetra-\m~3~-phosphonato-trizinc] monohydrate] ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 81.03130(10) _cell_angle_beta 88.06460(10) _cell_angle_gamma 80.07820(10) _cell_formula_units_Z 2 _cell_length_a 9.03805(13) _cell_length_b 9.36837(13) _cell_length_c 15.0207(2) _cell_measurement_reflns_used 10623 _cell_measurement_temperature 93(2) _cell_measurement_theta_max 75.2490 _cell_measurement_theta_min 5.7000 _cell_volume 1237.46(3) _computing_cell_refinement ; CrystalClear (Rigaku, 2015) ; _computing_data_collection ; CrystalClear (Rigaku, 2015) ; _computing_data_reduction ; CrystalClear (Rigaku, 2015) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 2012) ; _computing_publication_material ; publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL-2018/3 (Sheldrick, 2015) ; _computing_structure_solution ; SHELXS-97 (Sheldrick, 2008) ; _diffrn_ambient_temperature 93(2) _diffrn_measured_fraction_theta_full 0.969 _diffrn_measured_fraction_theta_max 0.942 _diffrn_measurement_device_type 'Rigaku Pilatus 200K CCD' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0121 _diffrn_reflns_av_unetI/netI 0.0083 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 11869 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 75.378 _diffrn_reflns_theta_min 2.978 _diffrn_source 'fine-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 6.486 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.74368 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrystalClear (Rigaku, 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.019 _exptl_crystal_description prism _exptl_crystal_F_000 756 _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _refine_diff_density_max 1.247 _refine_diff_density_min -0.668 _refine_ls_extinction_coef 0.0053(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL-2018/3 (Sheldrick 2015) ; _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 343 _refine_ls_number_reflns 4842 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.104 _refine_ls_R_factor_all 0.0311 _refine_ls_R_factor_gt 0.0308 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0455P)^2^+2.3807P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0846 _refine_ls_wR_factor_ref 0.0847 _reflns_number_gt 4831 _reflns_number_total 4842 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file pk2681sup1.cif _cod_data_source_block IV _cod_depositor_comments 'Adding full bibliography for 2244225--2244229.cif.' _cod_database_code 2244228 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.563 _shelx_estimated_absorpt_t_max 0.563 _shelx_hkl_file ; 0 0 1 9916.63 26.4490 1 0 0 1 10080.9 29.9140 2 0 0 2 31596.0 67.0514 1 0 0 -2 34052.6 74.3863 2 0 0 -3 12983.4 60.6467 2 0 0 -3 13002.7 46.3993 1 0 0 4 186791. 246.764 1 0 0 -5 20051.8 74.8151 1 0 0 -5 20490.8 97.8842 2 0 0 -6 469851. 518.380 2 0 0 -7 98680.0 195.385 1 0 0 -7 93914.1 253.887 2 0 0 -8 101798. 325.713 4 0 0 -8 113007. 214.125 1 0 0 -8 105806. 312.892 10 0 0 -8 109426. 297.762 2 0 0 -9 17538.4 138.660 10 0 0 -9 19430.6 159.444 4 0 0 -9 17562.4 144.884 12 0 0 -9 18898.4 133.183 2 0 0 -9 18086.4 133.489 8 0 0 -9 16863.7 139.337 7 0 0 -10 1355.38 45.2004 12 0 0 -10 1372.14 44.7446 10 0 0 -11 185627. 528.607 12 0 0 -11 184349. 509.598 10 0 0 -12 45632.8 275.202 7 0 0 -12 47945.6 270.973 10 0 0 -12 45801.7 292.717 4 0 0 -12 48052.3 279.945 12 0 0 -13 24232.4 198.610 7 0 0 -13 24025.5 198.831 10 0 0 -13 24531.5 219.713 4 0 0 -14 22328.0 188.779 10 0 0 -14 23060.3 217.090 4 0 0 -14 22712.2 194.683 12 0 0 -15 2296.34 61.9602 12 0 0 -15 2138.81 57.9179 7 0 0 -15 2186.20 68.7324 4 0 0 -15 2149.92 60.2070 10 0 0 -16 358.201 27.8906 12 0 0 -16 644.423 38.8513 4 0 0 -16 246.993 26.4070 10 0 0 -16 764.516 36.3301 7 0 0 16 328.232 24.4477 5 0 0 -17 91805.5 298.496 10 0 0 -17 88849.9 293.153 7 0 0 17 97898.4 300.931 5 0 0 -17 95805.6 347.433 4 0 0 18 25716.2 125.200 5 0 0 -18 25549.6 146.059 4 0 1 -18 19328.0 121.348 4 0 1 -17 17646.5 116.283 10 0 1 -17 16215.2 114.518 7 0 1 -16 4026.67 69.9718 10 0 -1 16 3887.97 66.0326 5 0 1 -16 3768.34 70.3735 12 0 1 -16 3943.55 69.0958 7 0 1 -15 1959.69 55.5791 7 0 -1 15 2001.42 54.4113 5 0 1 -15 2169.04 67.6731 4 0 1 -15 2176.37 60.1767 12 0 1 -15 1957.91 56.2632 10 0 1 -14 253.475 35.1860 4 0 1 -14 234.185 27.9975 7 0 1 -14 181.493 29.5676 12 0 1 -13 6688.82 104.243 10 0 1 -13 6659.32 105.668 7 0 -1 13 6034.04 95.8956 5 0 1 -13 6179.81 105.486 12 0 1 -13 6756.07 124.020 4 0 1 -12 47399.6 269.488 10 0 -1 12 47927.7 260.320 5 0 1 -12 48099.4 287.534 12 0 1 -12 47702.2 310.458 4 0 1 -11 190998. 552.448 12 0 1 -11 191208. 536.685 7 0 1 -11 192382. 533.252 10 0 1 -11 191539. 592.185 4 0 1 -10 1401.66 49.9652 12 0 1 -10 1493.60 47.2724 10 0 1 -9 140083. 426.127 12 0 1 -9 140235. 400.099 10 0 1 -9 135600. 356.427 6 0 1 -9 142941. 391.756 8 0 1 -9 138213. 444.156 4 0 1 -9 138319. 415.165 7 0 1 -8 60707.5 259.246 12 0 1 -8 60723.4 239.795 8 0 1 -8 60431.4 250.567 7 0 1 -8 60103.7 239.036 10 0 1 -7 37497.5 110.883 1 0 1 -7 37866.4 169.279 2 0 1 -5 168605. 210.936 1 0 1 -5 169746. 300.830 2 0 -1 4 2503.00 24.9967 1 0 1 -4 2583.86 34.9941 2 0 1 -3 12012.3 47.2301 1 0 1 -3 11763.1 62.7392 2 0 1 -2 81386.5 110.038 1 0 -1 2 82296.2 145.164 2 0 -1 1 7494.43 34.7575 2 0 -1 1 7337.53 31.4169 1 0 -1 -1 127372. 145.573 1 0 1 2 90893.8 132.452 1 0 -1 -3 183.100 8.20164 2 0 -1 -3 160.137 13.1549 1 0 -1 -5 2582.16 33.6825 1 0 -1 -5 2539.46 32.9999 2 0 -1 -7 117850. 239.152 1 0 -1 -7 117823. 265.857 2 0 -1 -8 96125.6 217.346 1 0 -1 -8 100730. 276.416 2 0 -1 -9 40926.6 213.659 12 0 -1 -9 42584.2 147.793 1 0 -1 -9 41108.5 214.345 4 0 1 9 41716.8 196.618 5 0 1 9 42406.9 243.123 11 0 -1 -10 38861.6 224.584 7 0 1 10 40147.0 244.600 11 0 -1 -10 39163.4 223.591 12 0 -1 -10 39394.0 221.822 10 0 -1 -10 40561.9 234.971 4 0 1 10 38072.5 199.544 5 0 1 11 114844. 373.263 5 0 -1 -11 115080. 407.508 7 0 -1 -11 113907. 427.918 4 0 -1 -11 120703. 420.715 12 0 1 11 119421. 435.145 11 0 -1 -11 117921. 408.128 10 0 -1 -12 34576.7 249.474 4 0 1 12 32876.9 231.575 11 0 -1 -12 33214.1 226.212 10 0 1 12 34845.5 215.515 5 0 -1 -12 31681.2 231.034 7 0 -1 -12 33674.0 228.106 12 0 -1 -13 222825. 590.782 12 0 -1 -13 222214. 595.628 10 0 -1 -13 223022. 606.328 7 0 1 14 9379.45 116.300 5 0 -1 -14 9578.55 126.980 7 0 -1 -14 9343.65 134.916 4 0 -1 -14 9721.68 126.706 12 0 -1 -14 9845.63 127.277 10 0 -1 -15 62412.9 301.623 7 0 -1 -15 62608.1 298.078 12 0 1 15 62885.8 282.017 5 0 -1 -16 9276.05 110.136 7 0 -1 -16 9345.10 122.578 4 0 -1 -16 8973.82 111.538 10 0 1 16 9149.24 103.138 5 0 -1 -16 8876.61 107.151 12 0 -1 -17 77250.4 279.831 7 0 -1 -17 79042.4 291.038 10 0 -1 -18 23361.8 131.754 10 0 -1 -18 23156.4 143.357 4 0 -2 17 3239.54 49.2860 5 0 2 -17 3371.74 59.1107 4 0 -2 16 21021.4 142.771 5 0 2 -16 19594.9 136.672 7 0 2 -16 19048.4 143.718 12 0 2 -16 21742.7 175.147 4 0 2 -15 1148.12 41.2671 7 0 -2 15 933.126 37.1276 5 0 2 -15 1034.21 42.9388 12 0 2 -15 844.605 44.9188 4 0 2 -15 783.916 34.9078 10 0 2 -14 65508.2 303.491 10 0 2 -14 65540.5 320.212 7 0 2 -13 1969.08 68.8126 4 0 2 -13 1977.17 59.2558 10 0 2 -13 2055.00 61.5709 7 0 2 -13 1949.47 63.7936 12 0 2 -12 12185.9 137.594 10 0 2 -12 14073.4 162.395 12 0 2 -12 12441.4 129.052 6 0 2 -12 13486.2 152.830 7 0 -2 12 12669.7 137.182 5 0 2 -11 48001.3 291.159 12 0 -2 11 47482.1 255.346 5 0 2 -11 48193.3 267.631 10 0 2 -10 39644.5 241.225 7 0 2 -10 39119.0 234.699 10 0 2 -9 156097. 413.179 6 0 2 -9 155664. 443.051 10 0 2 -9 156007. 477.242 12 0 2 -8 4402.98 69.1043 10 0 2 -8 4770.66 69.8266 6 0 2 -8 4750.32 79.7108 12 0 2 -8 4207.16 68.4493 9 0 2 -8 4883.54 76.8201 7 0 2 -7 10226.7 95.8993 6 0 2 -7 10298.8 109.757 4 0 2 -7 12343.1 70.5543 1 0 2 -7 12325.5 117.440 12 0 2 -7 12437.0 112.191 7 0 2 -6 40318.3 120.298 1 0 2 -5 303298. 327.043 1 0 2 -4 80958.8 158.517 1 0 2 -2 64569.2 138.459 1 0 -2 1 9832.78 49.6065 2 0 2 -1 10092.0 53.3065 1 0 2 1 7237.78 46.2080 1 0 2 3 2089.30 28.5378 1 0 -2 -3 1401.27 16.0096 2 0 -2 -5 116637. 267.796 1 0 -2 -5 115248. 198.169 2 0 -2 -6 331133. 403.250 2 0 -2 -6 340934. 469.534 1 0 -2 -7 310277. 465.095 1 0 -2 -7 318531. 425.131 2 0 2 8 718326. 982.621 11 0 -2 -9 25741.7 169.146 12 0 -2 -9 25266.5 143.978 2 0 2 9 25184.2 195.835 11 0 -2 -9 24796.3 164.220 4 0 -2 -9 25414.2 136.373 1 0 -2 -10 17391.8 150.467 4 0 -2 -10 18030.3 153.044 12 0 2 10 18103.1 139.028 5 0 -2 -10 17642.1 129.007 2 0 2 11 189.128 25.6632 11 0 -2 -11 261.039 26.0246 4 0 -2 -11 205.725 24.2214 12 0 2 12 137599. 508.046 11 0 -2 -12 137259. 454.618 12 0 -2 -12 137017. 481.349 4 0 -2 -13 331250. 714.045 12 0 -2 -13 333884. 732.486 7 0 2 13 328515. 777.867 11 0 -2 -13 329184. 776.465 4 0 2 13 331973. 669.543 5 0 2 14 26299.5 213.572 11 0 -2 -14 25539.1 197.225 12 0 -2 -14 26132.7 204.501 7 0 2 14 24924.8 184.106 5 0 -2 -14 24356.2 215.726 4 0 -2 -15 166627. 524.980 4 0 2 15 165113. 457.414 5 0 2 16 19865.2 148.310 5 0 -2 -16 20144.3 166.088 10 0 -2 -16 19827.3 160.674 7 0 -2 -17 40147.7 210.452 10 0 -2 -17 40196.0 220.569 4 0 -2 -18 24487.5 139.920 10 0 2 18 24032.4 119.470 5 0 3 -17 443.179 19.5657 4 0 -3 17 468.220 17.6027 5 0 -3 16 15613.2 112.048 5 0 3 -16 14907.8 114.004 12 0 3 -15 14116.5 136.073 12 0 -3 15 13924.0 123.157 5 0 3 -14 200689. 557.586 12 0 3 -14 201346. 518.393 7 0 -3 14 202344. 505.680 5 0 3 -14 202658. 469.938 6 0 3 -13 33360.0 228.016 7 0 3 -13 33612.3 210.617 10 0 -3 12 31897.3 219.852 5 0 3 -12 32575.5 218.166 6 0 3 -12 32055.9 217.459 10 0 3 -12 32466.9 236.007 7 0 3 -11 29474.0 230.844 7 0 3 -11 28613.6 210.614 9 0 3 -11 29224.9 236.628 12 0 3 -11 28657.3 204.045 6 0 -3 11 29019.0 206.954 5 0 3 -10 33379.9 237.413 7 0 3 -10 33380.5 259.114 4 0 3 -10 33449.1 217.815 6 0 3 -10 33751.0 221.743 10 0 3 -9 216908. 568.409 9 0 3 -9 216840. 538.006 10 0 3 -9 212240. 522.403 6 0 3 -9 218440. 635.702 4 0 3 -9 222510. 609.580 12 0 3 -9 218982. 575.203 7 0 3 -8 30138.0 190.837 10 0 3 -8 30513.6 201.655 9 0 3 -8 29175.9 186.394 6 0 3 -8 29016.4 216.717 4 0 3 -8 29987.4 215.407 12 0 3 -8 31315.5 207.411 7 0 3 -7 64298.7 276.178 7 0 3 -7 62508.8 288.220 12 0 3 -7 64008.2 178.702 1 0 3 -7 61794.5 254.733 10 0 3 -7 62277.0 261.059 6 0 3 -7 64275.4 277.073 9 0 3 -6 36474.7 195.265 7 0 3 -6 36202.8 189.801 6 0 3 -6 35737.8 174.998 8 0 3 -6 35731.0 202.493 12 0 3 -6 36823.3 198.842 9 0 3 -5 1391.20 27.1400 1 0 3 -4 131047. 248.672 1 0 3 -2 59754.6 161.469 1 0 3 -1 2937.74 37.2292 1 0 3 1 38073.3 129.638 1 0 3 2 122498. 240.037 1 0 3 4 42742.8 150.693 1 0 -3 -4 47918.8 106.441 2 0 3 5 98710.8 242.532 1 0 -3 -5 101457. 175.402 2 0 -3 -6 45895.9 202.116 1 0 -3 -6 51646.6 146.556 2 0 -3 -7 126833. 345.341 1 0 -3 -7 125131. 251.097 2 0 -3 -8 427519. 630.155 1 0 -3 -8 427653. 513.075 2 0 -3 -9 7951.65 96.4182 12 0 3 9 8569.54 120.153 11 0 -3 -9 9642.74 103.487 4 0 3 9 9089.55 93.3832 5 0 3 10 18534.8 141.817 5 0 -3 -10 17739.3 149.715 12 0 -3 -10 18859.6 153.321 4 0 3 10 17491.2 183.764 11 0 -3 -11 61758.3 296.084 12 0 -3 -11 61053.1 292.111 4 0 3 11 60888.0 272.147 5 0 3 12 88528.1 425.745 11 0 -3 -12 89004.2 361.838 12 0 3 12 89847.2 343.610 5 0 -3 -12 89843.8 372.047 10 0 -3 -13 38762.0 243.723 12 0 3 13 39547.0 229.779 5 0 -3 -13 38263.7 251.816 4 0 -3 -13 40007.4 255.064 10 0 -3 -13 40261.0 255.338 7 0 3 13 40148.6 283.618 11 0 -3 -14 13294.2 147.662 10 0 -3 -14 13683.1 149.512 7 0 3 14 13117.7 131.556 5 0 -3 -14 12921.6 147.459 4 0 -3 -14 13305.8 139.198 12 0 3 14 13618.0 157.523 11 0 3 15 57783.3 299.783 11 0 -3 -15 60122.3 294.706 7 0 -3 -15 58306.9 301.373 4 0 3 15 57657.0 262.763 5 0 -3 -15 56007.6 289.297 10 0 -3 -15 59443.0 278.365 12 0 3 16 14549.4 123.051 5 0 -3 -16 14290.4 135.858 7 0 -3 -16 14317.1 141.972 4 0 3 17 3259.21 50.2023 5 0 -3 -17 3252.94 59.9969 4 0 -3 -17 3084.10 56.9213 7 0 -3 -18 35139.6 149.363 7 0 -4 16 161.842 12.0601 5 0 4 -16 149.339 13.5916 12 0 -4 15 15571.1 115.678 5 0 4 -15 15382.8 124.737 12 0 4 -14 128909. 379.014 7 0 4 -14 135332. 453.241 4 0 4 -14 129982. 427.155 12 0 4 -14 138434. 370.986 6 0 -4 14 137281. 382.222 5 0 4 -13 127999. 463.997 12 0 4 -13 128389. 421.000 7 0 4 -12 248.085 33.4625 12 0 4 -12 332.643 30.1893 7 0 -4 12 323.301 27.2074 5 0 4 -12 339.142 36.6268 4 0 4 -12 268.495 26.2676 9 0 4 -11 11688.5 131.715 6 0 -4 11 11160.8 127.476 5 0 4 -11 11538.8 160.465 4 0 4 -11 11232.5 137.667 9 0 4 -10 7224.38 112.819 9 0 4 -10 7422.67 122.681 12 0 4 -10 7622.10 128.825 4 0 4 -10 7591.39 108.364 6 0 4 -10 7318.53 115.796 7 0 4 -9 17377.3 187.884 4 0 4 -9 17344.0 159.251 6 0 4 -9 17486.5 175.445 7 0 4 -9 18433.9 177.102 9 0 4 -9 18435.9 186.717 12 0 4 -8 74821.0 325.112 6 0 4 -8 75613.0 359.249 9 0 4 -8 75174.8 371.873 4 0 4 -8 76650.5 366.959 12 0 4 -8 76881.8 305.285 10 0 4 -8 77761.4 350.404 7 0 4 -7 283845. 612.897 6 0 4 -7 285277. 676.449 4 0 4 -7 289964. 647.115 7 0 4 -7 289943. 661.288 9 0 4 -7 280088. 669.092 12 0 4 -6 105346. 373.943 9 0 4 -6 105508. 353.099 6 0 4 -6 105307. 386.885 12 0 4 -6 104001. 379.818 4 0 4 -6 107584. 261.854 1 0 4 -6 107765. 369.889 7 0 4 -5 66657.0 208.017 1 0 4 -5 67913.0 291.817 12 0 4 -5 66091.1 271.380 7 0 4 -5 67522.0 285.629 9 0 4 -4 121412. 358.462 9 0 4 -4 120837. 278.195 1 0 4 -4 120387. 335.562 6 0 4 -2 9069.55 75.0678 1 0 4 -1 61955.9 195.599 1 0 4 0 18011.5 103.730 1 0 4 2 2438.29 41.1841 1 0 4 4 115639. 290.997 1 0 4 5 74477.9 238.463 1 0 4 6 330.932 25.1895 11 0 4 6 372.037 20.7642 7 0 4 7 1614.99 40.2448 3 0 -4 -7 1456.67 45.5331 1 0 4 8 174919. 550.693 11 0 -4 -8 182853. 470.030 1 0 4 8 180729. 426.878 3 0 -4 -8 188636. 445.297 12 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197.672 9 2 7 2 26603.9 180.631 3 2 7 2 27884.7 196.230 7 2 7 3 89344.7 348.600 7 2 7 3 89914.2 307.583 4 2 7 3 89368.0 337.105 3 2 7 3 88587.9 350.862 1 2 7 4 393498. 642.468 4 2 7 4 397858. 811.432 11 2 7 4 382677. 716.888 3 2 7 4 380498. 720.372 1 2 7 4 402096. 746.295 7 2 7 5 102595. 334.350 4 2 7 5 102265. 377.761 1 2 7 6 5860.09 90.9186 7 2 7 6 5608.06 94.0624 3 2 7 6 5704.30 106.580 11 2 7 7 3043.43 82.3400 11 2 7 7 3230.01 72.4304 3 2 7 7 3000.15 67.3803 7 2 7 8 9653.93 119.692 7 2 7 8 9976.39 123.376 3 2 7 9 9431.62 147.711 11 -2 -7 -9 9142.84 124.173 12 2 7 10 19222.6 206.469 11 -2 -7 -10 19838.6 185.071 12 2 7 10 19286.5 168.988 3 2 7 11 319007. 826.989 11 -2 -7 -11 319682. 716.248 12 2 7 12 14977.0 136.381 3 -2 -7 -12 15262.8 136.713 4 -2 -7 -13 509.831 32.3668 12 2 7 13 356.796 23.0026 3 -2 -7 -14 12991.0 120.114 12 2 7 14 12910.8 138.159 11 -2 -7 -14 13215.6 114.251 7 2 7 15 42509.6 217.013 11 -2 -7 -15 42258.8 185.525 12 2 7 16 4905.76 61.1098 11 -2 -7 -16 5219.10 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75028.3 344.476 9 2 8 1 75260.1 345.905 7 2 8 2 32233.1 188.702 4 2 8 2 31607.3 205.195 3 2 8 3 41665.5 214.095 4 2 8 3 41205.3 239.961 3 2 8 3 41951.8 254.915 7 2 8 4 38262.8 239.707 7 2 8 4 38013.9 201.001 4 2 8 4 37921.2 236.719 3 2 8 5 1456.63 52.3900 11 2 8 5 1123.63 45.2229 7 2 8 5 1900.47 46.5654 4 2 8 5 1297.03 48.4605 3 2 8 5 1767.64 53.6703 1 2 8 6 6535.33 99.1664 7 2 8 6 7508.89 118.169 11 2 8 7 2579.76 72.9279 11 2 8 7 2647.11 67.1639 3 2 8 8 2859.79 66.0084 7 2 8 8 2883.52 69.7368 3 -2 -8 -9 28439.8 212.056 12 2 8 9 28989.0 240.995 11 -2 -8 -10 2747.27 68.3322 12 2 8 10 2894.97 65.3047 3 -2 -8 -11 145456. 452.245 12 2 8 11 143164. 424.665 3 -2 -8 -12 31493.7 196.772 12 2 8 12 31729.0 182.919 3 2 8 13 14386.7 139.533 11 -2 -8 -13 14524.0 123.169 12 -2 -8 -14 3631.61 51.9587 7 -2 -8 -14 3790.27 55.0740 12 -2 -8 -14 3769.02 58.3251 10 -2 -8 -15 5670.82 58.9908 10 2 9 -9 26162.6 133.631 12 2 9 -9 25907.8 129.259 7 2 9 -8 2070.07 45.4876 7 2 9 -8 2221.14 48.7243 12 2 9 -7 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223.369 13 -4 9 3 73179.3 230.869 3 -4 9 2 13927.3 97.0488 3 -4 8 12 925.235 24.3501 13 -4 8 11 79983.6 212.655 3 -4 8 10 43375.0 185.957 3 -4 8 9 9474.06 101.196 13 -4 8 9 12360.7 107.861 3 -4 8 8 29144.6 183.732 13 -4 8 8 30725.5 181.488 3 -4 8 7 7549.11 96.3003 3 -4 8 7 7869.42 99.8161 13 -4 8 6 23552.2 170.713 13 -4 8 5 1265.64 44.0540 3 -4 8 5 711.629 36.1515 13 -4 8 4 5176.59 83.3311 13 -4 8 4 4307.15 65.7803 5 -4 8 3 208658. 488.838 3 -4 8 3 213239. 459.344 5 -4 8 2 133.422 19.3953 3 -4 8 2 186.717 23.1655 13 -4 8 1 2513.62 55.1432 13 -4 8 1 2470.20 50.3697 3 -4 8 0 7232.90 79.7503 3 -4 8 0 7124.11 83.9121 5 -4 8 -1 19683.5 142.694 6 -4 8 -1 19451.1 133.427 13 -4 8 -2 239.103 20.3563 9 -4 8 -2 258.359 20.2745 5 -4 8 -3 106718. 335.271 6 -4 8 -3 108094. 333.717 9 -4 8 -4 3266.83 58.6296 6 -4 8 -4 3120.85 59.1058 9 -4 8 -5 30351.7 167.407 6 -4 8 -5 31177.2 176.808 9 -4 8 -6 2012.17 41.9992 6 -4 8 -6 1342.00 36.8441 9 -4 8 -7 24487.9 127.889 6 -4 8 -7 23994.3 134.120 9 -4 8 -8 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8104.41 118.500 8 8 5 5 39805.3 287.342 11 -8 -5 -5 40545.1 259.635 8 8 5 6 47344.9 309.582 11 -8 -5 -6 46813.6 265.827 8 8 5 7 18849.4 193.579 11 8 5 7 18258.7 159.156 3 8 5 8 80256.4 379.887 11 8 5 8 83548.8 317.643 3 8 5 9 6717.21 108.576 11 8 5 9 5834.11 84.3596 3 8 5 10 1265.42 47.3349 11 8 5 10 1369.67 38.5489 3 8 5 11 6617.35 91.9697 11 8 5 11 6609.06 69.0477 3 -8 -5 -11 6694.67 74.2190 4 8 5 12 99520.7 300.269 11 -8 -5 -12 103952. 261.031 4 -8 -6 8 498.267 23.1632 8 8 6 -7 69338.6 225.179 4 -8 -6 7 68604.5 265.894 8 8 6 -6 41837.2 192.038 4 -8 -6 6 38710.3 216.864 8 8 6 -5 36611.8 190.973 4 -8 -6 5 34309.5 213.967 8 8 6 -4 25875.1 167.526 4 -8 -6 4 23666.2 185.797 8 8 6 -3 1623.04 45.6597 4 8 6 -3 1485.43 50.5194 11 8 6 -2 6051.86 101.048 11 -8 -6 2 5854.19 98.0641 8 8 6 -1 387.961 32.9736 11 -8 -6 1 309.731 28.9106 8 8 6 0 504.478 38.1155 11 8 6 0 417.572 29.0735 3 8 6 1 165374. 459.714 4 8 6 1 164761. 481.218 3 8 6 2 6706.38 93.4790 4 8 6 2 6050.75 112.608 11 8 6 2 7291.33 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147.037 11 8 7 9 18718.2 127.541 3 8 7 10 5146.04 75.5580 11 8 7 10 5696.96 61.4558 3 8 7 11 663.754 26.3959 11 -8 -7 -11 866.172 23.4920 4 8 8 -5 27744.5 122.612 4 8 8 -4 9924.16 82.1512 4 8 8 -3 598.578 24.8050 4 8 8 -2 162737. 369.985 4 8 8 -1 295.150 21.0010 4 8 8 0 91.7502 16.0377 4 8 8 1 33788.7 182.715 4 8 8 1 34079.4 161.734 3 8 8 2 8322.46 101.274 11 8 8 2 8737.48 89.3732 3 8 8 3 62069.3 282.979 11 8 8 3 63407.4 246.543 3 8 8 4 5980.60 90.5771 11 8 8 4 5819.23 77.5514 3 8 8 5 12879.1 132.218 11 8 8 5 13053.5 114.225 3 8 8 6 243.300 24.5163 11 8 8 6 239.607 20.5844 3 8 8 7 24578.4 171.247 11 8 8 8 261.638 22.3418 11 8 8 8 318.052 19.1058 3 8 8 9 62685.9 235.255 11 8 8 9 70048.6 202.876 3 8 9 -2 134394. 262.583 4 8 9 -1 11956.8 84.5013 4 8 9 0 10816.3 84.6293 4 8 9 1 25028.7 130.594 4 8 9 4 32205.9 137.373 3 8 9 5 45361.6 162.902 3 8 9 6 4196.91 49.1022 3 8 9 7 528.340 18.2587 3 9 -5 -5 29138.3 116.353 3 -9 5 5 27171.5 111.261 5 9 -5 -4 210.494 15.5875 3 -9 5 4 193.340 14.0541 5 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335.206 8 9 1 -5 8974.46 129.394 11 9 1 -5 9093.94 103.462 3 -9 -1 5 9117.56 118.489 8 9 1 -4 53909.2 314.059 11 9 1 -4 53270.9 259.136 3 9 1 -3 44645.5 293.998 11 -9 -1 3 44281.2 270.641 8 9 1 -2 117643. 470.757 11 -9 -1 2 115176. 455.115 8 9 1 -1 22257.1 205.027 11 -9 -1 1 22130.5 201.394 8 9 1 0 3333.87 81.3903 11 -9 -1 0 3297.08 79.1172 8 9 1 1 28240.8 226.839 11 9 1 1 29848.6 215.173 3 9 1 2 9636.05 136.257 11 9 1 2 9695.37 121.536 3 -9 -1 -3 57066.1 277.241 13 9 1 3 56447.5 283.440 3 -9 -1 -4 142839. 431.054 13 9 1 4 147309. 446.012 3 9 1 5 57251.5 306.054 11 -9 -1 -5 56371.0 303.263 8 9 1 6 19774.8 155.052 3 -9 -1 -6 19182.0 167.758 8 9 1 7 404.561 25.1574 3 -9 -1 -7 222.525 25.0061 8 -9 -1 -8 37934.6 216.009 8 -9 -1 -9 68642.6 265.428 8 -9 -1 -10 7103.66 76.8110 8 -9 -1 -11 634.818 21.1479 8 -9 -2 10 27629.4 131.754 8 9 2 -9 29315.7 164.868 11 -9 -2 9 32993.3 168.664 8 9 2 -8 3736.24 68.0979 11 -9 -2 8 3939.62 66.3619 8 9 2 -7 3091.79 69.0165 11 9 2 -6 73894.4 346.468 11 -9 -2 6 75618.6 324.993 8 9 2 -5 4713.38 71.0846 3 -9 -2 5 4692.64 86.6448 8 9 2 -4 70605.9 290.351 3 9 2 -3 30775.9 239.982 11 9 2 -3 31067.1 203.978 3 9 2 -2 237958. 671.798 11 9 2 -2 244488. 585.195 3 9 2 -1 698.512 46.4139 11 9 2 -1 963.079 43.8327 3 9 2 0 60960.2 301.653 3 -9 -2 0 60289.2 333.258 8 9 2 1 79663.3 393.309 11 -9 -2 -1 72988.6 376.478 8 9 2 2 20663.6 198.967 11 -9 -2 -2 20699.7 201.606 8 9 2 3 2051.63 66.9914 11 -9 -2 -3 2195.42 67.3542 8 9 2 4 250460. 602.738 3 -9 -2 -4 244275. 665.985 8 9 2 5 5465.84 100.775 11 9 2 5 5652.68 89.2736 3 -9 -2 -5 5627.67 99.0257 8 9 2 6 39510.1 224.293 3 -9 -2 -6 38859.4 250.066 8 9 2 7 3237.61 72.2047 11 9 2 7 3463.67 66.1593 3 -9 -2 -7 3417.83 72.6035 8 9 2 8 17541.7 132.799 3 -9 -2 -8 18984.8 157.349 8 -9 -2 -9 38197.4 201.210 8 -9 -2 -10 4543.56 62.7680 8 -9 -2 -11 12605.1 88.2160 8 -9 -3 10 6702.61 61.8134 8 -9 -3 9 4258.19 60.2317 8 9 3 -8 1922.48 45.3013 11 9 3 -7 1454.97 46.5657 11 9 3 -6 63211.0 302.859 11 -9 -3 6 52656.2 274.238 8 9 3 -5 50796.2 287.995 11 -9 -3 5 51078.0 281.800 8 9 3 -4 54820.0 309.844 11 -9 -3 4 55507.6 301.278 8 9 3 -3 8253.26 103.217 3 -9 -3 3 8403.55 120.456 8 9 3 -2 24116.6 183.554 3 -9 -3 2 22955.7 204.955 8 9 3 -1 14415.3 167.068 11 9 3 -1 14996.3 149.073 3 9 3 0 60171.5 348.344 11 -9 -3 0 60562.5 338.233 8 9 3 1 73974.6 389.303 11 -9 -3 -1 73747.4 375.341 8 9 3 2 75232.5 373.029 11 -9 -3 -2 78470.9 382.345 8 9 3 3 21907.1 201.973 11 -9 -3 -3 22406.6 205.191 8 9 3 4 157306. 545.195 11 -9 -3 -4 157522. 527.746 8 9 3 5 17933.5 180.942 11 9 3 5 18702.8 160.963 3 9 3 6 93140.8 406.223 11 -9 -3 -6 96238.4 383.925 8 9 3 7 9575.58 125.760 11 9 3 7 9387.18 107.019 3 -9 -3 -7 9667.12 116.735 8 9 3 8 1195.45 38.3171 3 -9 -3 -8 1057.04 38.9262 8 9 3 9 14407.4 130.861 11 -9 -3 -9 14104.1 121.288 8 -9 -3 -10 31414.2 158.090 8 -9 -3 -11 197.905 12.8393 8 -9 -4 9 1189.83 30.3020 8 -9 -4 8 309.375 21.1176 8 9 4 -7 18845.6 136.245 11 -9 -4 7 21533.5 156.517 8 9 4 -6 19310.9 156.558 11 -9 -4 6 19546.3 160.522 8 9 4 -5 106480. 391.853 11 -9 -4 5 108226. 397.976 8 9 4 -4 22764.6 192.383 11 -9 -4 4 22342.4 185.144 8 9 4 -3 9530.35 102.702 3 -9 -4 3 9287.47 124.323 8 9 4 -2 9621.44 136.711 11 -9 -4 2 9721.30 130.371 8 9 4 -1 6336.82 113.441 11 -9 -4 1 6354.15 107.514 8 9 4 0 19078.0 165.141 3 -9 -4 0 17631.2 180.692 8 9 4 1 154695. 548.401 11 -9 -4 -1 163078. 542.483 8 9 4 2 82913.3 394.673 11 -9 -4 -2 82795.3 384.424 8 9 4 3 36134.7 261.844 11 -9 -4 -3 36001.1 250.238 8 9 4 4 36534.5 261.127 11 9 4 4 37334.8 231.902 3 9 4 5 10793.6 141.211 11 -9 -4 -5 11104.9 133.903 8 9 4 6 225974. 541.400 3 -9 -4 -6 217241. 557.009 8 9 4 7 21611.3 187.974 11 -9 -4 -7 22269.3 168.691 8 9 4 8 192.396 24.6846 11 -9 -4 -8 237.766 21.5304 8 9 4 9 53230.4 207.256 3 -9 -4 -9 52293.0 216.421 8 9 4 10 47186.0 213.981 11 -9 -4 -10 43128.5 170.664 8 -9 -5 8 5079.60 59.5486 8 -9 -5 7 19422.8 132.341 8 -9 -5 6 10498.8 107.867 8 9 5 -5 33151.3 186.543 11 -9 -5 5 34741.2 206.372 8 9 5 -4 1682.80 50.8640 11 -9 -5 4 1541.26 48.8092 8 9 5 -3 9175.53 118.901 11 -9 -5 3 9102.57 115.816 8 9 5 -2 7192.69 85.9722 3 -9 -5 2 7466.59 106.903 8 9 5 -1 1433.14 53.4725 11 9 5 -1 1161.17 40.2009 3 9 5 0 4489.35 90.9517 11 9 5 0 4553.45 78.7860 3 -9 -5 0 4538.01 87.5338 8 9 5 1 212673. 623.105 11 -9 -5 -1 208747. 571.412 8 9 5 2 5682.99 90.4699 3 -9 -5 -2 5289.23 93.7123 8 -9 -5 -3 2353.50 61.7772 8 9 5 4 2019.17 63.7190 11 -9 -5 -4 1875.76 52.4321 8 9 5 5 16494.6 169.818 11 -9 -5 -5 16667.8 148.033 8 9 5 6 69522.0 340.459 11 -9 -5 -6 67810.0 281.280 8 9 5 7 67177.5 318.389 11 -9 -5 -7 66409.7 258.804 8 9 5 8 1446.11 48.1257 11 9 5 8 1783.34 42.3126 3 9 5 9 112409. 293.300 3 -9 -5 -9 116251. 264.174 4 9 5 10 1502.52 39.3234 11 9 5 10 829.821 23.5523 3 -9 -6 6 42437.3 179.262 8 -9 -6 5 709.159 27.9461 8 -9 -6 4 1492.26 41.5882 8 9 6 -3 557.213 27.7864 11 -9 -6 3 727.740 32.2904 8 9 6 -2 14680.8 138.056 11 -9 -6 2 14678.3 137.483 8 9 6 -1 6973.13 101.316 11 9 6 -1 6749.80 77.5676 3 -9 -6 1 6717.76 94.6237 8 9 6 0 15304.1 152.850 11 9 6 0 15101.4 123.383 3 9 6 1 223878. 458.501 4 9 6 1 213498. 577.114 11 9 6 1 221081. 495.104 3 -9 -6 -1 212552. 527.325 8 9 6 2 6253.93 103.058 11 -9 -6 -2 6444.76 91.0390 8 9 6 3 38405.1 253.678 11 -9 -6 -3 36104.8 200.216 8 9 6 4 3749.73 66.9243 3 9 6 6 4831.54 85.9736 11 9 6 6 6124.94 81.1351 3 9 6 7 77773.2 325.731 11 9 6 7 81134.3 280.164 3 9 6 8 18194.3 148.605 11 9 6 8 19833.5 128.252 3 9 6 9 40825.9 203.591 11 9 6 9 40487.4 161.684 3 9 6 10 149.955 16.4904 11 9 7 -3 221.271 14.4112 4 9 7 -2 37845.6 159.680 4 9 7 -1 7710.77 75.5815 4 9 7 0 587.865 24.1017 4 9 7 0 294.529 23.8415 11 9 7 1 17882.8 149.313 11 9 7 1 18536.8 120.232 3 9 7 2 2132.63 55.3710 11 9 7 2 2932.70 52.5502 3 9 7 3 48179.0 251.544 11 9 7 3 51223.1 220.173 3 9 7 4 644.438 32.6564 11 9 7 4 931.092 32.9889 3 9 7 5 222.278 23.8756 11 9 7 5 222.052 19.9700 3 9 7 6 46757.3 235.961 11 9 7 7 32599.0 156.048 3 9 7 8 1028.36 26.6540 3 9 7 9 73439.1 229.116 11 9 8 3 28956.9 128.142 3 9 8 4 28694.7 155.681 11 9 8 4 31421.4 135.818 3 9 8 5 13383.8 104.346 11 9 8 5 14593.3 91.5547 3 9 8 6 1980.70 33.2396 3 10 -3 -3 79935.3 216.513 3 -10 3 3 70128.5 187.374 5 10 -3 -2 18860.5 109.006 3 -10 3 2 17587.9 96.6176 5 -10 3 1 102.487 11.5875 13 10 -3 -1 105.117 13.3031 3 10 -3 0 7980.51 69.6550 3 -10 3 0 8080.44 64.0452 5 -10 3 -1 913.907 24.7252 13 10 -3 1 1016.68 25.7244 3 -10 3 -2 98061.2 229.258 13 -10 3 -3 16448.1 93.8709 6 10 -2 -5 6024.25 67.3267 11 10 -2 -5 6988.58 65.4556 3 10 -2 -4 27057.2 137.674 3 -10 2 4 25539.2 122.884 5 -10 2 3 86239.3 234.473 5 10 -2 -2 9179.68 90.9627 3 -10 2 2 8751.48 76.9183 5 10 -2 -1 29585.0 160.201 3 -10 2 1 28721.6 140.305 5 -10 2 0 255.782 17.8490 13 10 -2 0 220.534 19.6525 3 -10 2 -1 658.919 25.5085 13 10 -2 1 693.974 27.0752 3 -10 2 -2 736.665 26.2571 13 10 -2 2 1124.71 31.1033 3 -10 2 -3 1040.96 29.5138 13 10 -2 3 729.969 25.0675 3 -10 2 -5 1902.34 33.4306 6 10 -1 -7 4490.38 57.7997 11 10 -1 -6 440.910 23.7867 11 10 -1 -6 431.270 17.9855 3 10 -1 -5 9638.18 99.1365 11 10 -1 -5 10346.4 86.5760 3 10 -1 -4 9811.63 103.713 11 10 -1 -4 10445.8 96.5580 3 10 -1 -3 62463.2 261.931 11 10 -1 -3 66884.8 252.193 3 10 -1 -2 9507.89 103.126 11 -10 1 2 10364.1 90.9941 8 10 -1 -1 83640.6 306.326 11 -10 1 1 85697.2 271.373 8 10 -1 0 17082.3 132.362 3 -10 1 0 15565.5 119.217 8 10 -1 1 2663.27 53.2410 3 -10 1 -1 2848.55 51.1363 8 10 -1 2 5669.81 74.1244 3 -10 1 -2 5699.62 72.5068 8 -10 1 -3 20974.6 130.297 13 10 -1 3 20998.9 132.753 3 -10 1 -3 21040.8 132.698 8 10 -1 4 18970.4 119.328 3 -10 1 -4 19308.9 122.496 8 -10 1 -5 38219.3 159.724 8 -10 1 -6 33603.6 139.899 6 -10 1 -6 38912.5 146.952 8 10 0 -8 10042.8 82.2572 11 10 0 -7 49510.0 205.697 11 10 0 -6 32315.0 183.128 11 -10 0 6 29572.1 134.795 8 10 0 -5 46986.9 237.866 11 10 0 -5 46637.0 181.455 3 10 0 -4 7474.35 97.7909 11 -10 0 4 7352.01 82.4144 8 10 0 -3 16095.2 146.767 11 -10 0 3 15975.8 127.040 8 10 0 -2 1915.25 53.9839 11 -10 0 2 1826.15 47.1798 8 10 0 -1 92126.2 357.901 11 -10 0 1 96548.7 333.705 8 10 0 0 6516.56 94.3871 11 -10 0 0 6994.19 89.3720 8 10 0 1 18883.2 154.819 11 10 0 1 19011.9 145.631 3 10 0 2 886.899 34.8077 11 -10 0 -2 903.346 35.1212 8 10 0 3 14473.0 121.940 3 -10 0 -3 15320.0 128.518 8 10 0 4 50497.3 213.896 3 -10 0 -4 50501.4 229.094 8 -10 0 -5 96627.4 303.820 8 -10 0 -6 68803.2 233.864 8 -10 0 -7 788.804 25.3424 8 -10 0 -8 572.100 18.5601 8 10 1 -8 12019.0 90.0293 11 -10 -1 7 74140.2 217.464 8 10 1 -6 10985.8 110.596 11 -10 -1 6 11476.5 97.0950 8 10 1 -5 35583.7 211.018 11 10 1 -5 36034.7 157.892 3 10 1 -4 15560.5 143.602 11 10 1 -4 15584.1 115.051 3 10 1 -3 7976.25 107.887 11 10 1 -3 7945.27 90.0324 3 -10 -1 3 8224.67 100.508 8 10 1 -2 13054.8 137.511 11 -10 -1 2 13329.4 131.816 8 10 1 -1 3943.31 68.5056 3 -10 -1 1 3886.92 72.8598 8 10 1 0 2146.23 60.4547 11 -10 -1 0 2008.47 53.8176 8 10 1 1 45598.1 250.854 11 -10 -1 -1 46723.1 251.054 8 10 1 2 6215.00 92.9683 11 10 1 2 6359.82 86.8485 3 -10 -1 -2 6172.26 92.0525 8 10 1 3 295.180 25.0635 11 10 1 3 404.487 26.7525 3 10 1 4 17272.4 141.128 11 10 1 4 17940.0 137.337 3 10 1 5 94900.0 295.417 3 10 1 6 4563.12 61.9244 3 -10 -1 -7 14291.7 108.418 8 -10 -1 -8 1422.02 32.4650 8 -10 -1 -9 6214.90 54.1148 8 10 2 -7 20807.4 130.646 11 -10 -2 7 22537.6 127.301 8 10 2 -6 5576.74 76.5815 11 -10 -2 6 5207.46 69.1450 8 -10 -2 5 33198.6 187.704 8 10 2 -4 3566.83 53.9838 3 -10 -2 4 3537.25 66.5189 8 10 2 -3 781.146 38.6809 11 10 2 -3 663.622 28.6995 3 10 2 -2 23887.3 191.493 11 10 2 -2 25285.9 163.970 3 10 2 -1 21850.9 187.000 11 10 2 -1 22100.7 158.703 3 10 2 0 10623.3 129.645 11 10 2 0 12175.6 121.426 3 10 2 1 79065.2 351.532 11 -10 -2 -1 75612.5 323.724 8 10 2 2 5407.62 90.4751 11 -10 -2 -2 5242.57 88.1670 8 10 2 3 26360.0 193.974 11 -10 -2 -3 26704.1 192.617 8 10 2 4 1642.37 49.8687 11 10 2 4 1757.99 46.6826 3 10 2 5 30933.0 193.135 11 -10 -2 -5 31248.6 190.492 8 10 2 6 712.110 30.2722 11 -10 -2 -6 824.505 31.8579 8 10 2 7 9648.22 82.6386 3 -10 -2 -7 10338.1 97.4896 8 -10 -2 -8 4854.49 59.7217 8 -10 -2 -9 1405.22 28.5416 8 -10 -3 7 1028.44 28.0556 8 10 3 -6 2271.47 46.9815 11 10 3 -5 44936.7 225.069 11 10 3 -4 507.344 30.7426 11 -10 -3 4 335.610 24.4240 8 10 3 -3 3072.43 51.1109 3 -10 -3 3 3643.42 70.4863 8 10 3 -2 151184. 381.459 3 -10 -3 2 145670. 443.786 8 10 3 -1 3852.87 66.2977 3 -10 -3 1 4431.30 81.3084 8 10 3 0 958.215 44.1619 11 -10 -3 0 841.074 39.6277 8 10 3 1 105542. 402.201 11 -10 -3 -1 108017. 395.942 8 10 3 2 14948.4 151.079 11 -10 -3 -2 15105.8 146.902 8 10 3 3 11965.5 132.695 11 -10 -3 -3 12204.7 124.325 8 10 3 4 28985.6 200.660 11 -10 -3 -4 29328.4 190.864 8 10 3 5 15526.6 141.779 11 -10 -3 -5 15378.2 132.108 8 10 3 6 8108.28 85.8481 3 -10 -3 -6 8094.99 92.3987 8 10 3 7 154.419 16.7378 11 10 3 7 183.670 15.9298 3 -10 -3 -7 206.104 18.2525 8 10 3 8 8195.05 68.2430 3 -10 -3 -8 9287.46 80.2782 8 -10 -4 6 2286.51 42.6551 8 10 4 -5 2551.96 47.7519 11 -10 -4 5 2906.71 53.8204 8 10 4 -4 43047.5 215.032 11 -10 -4 4 43458.9 214.523 8 10 4 -3 16588.8 142.776 11 -10 -4 3 16144.3 137.489 8 10 4 -2 164603. 468.247 11 -10 -4 2 165101. 458.608 8 10 4 -1 65229.3 244.117 3 -10 -4 1 60842.8 281.021 8 10 4 0 315.512 24.0450 3 -10 -4 0 120.788 21.0364 8 10 4 1 68281.0 321.489 11 -10 -4 -1 70072.2 304.739 8 10 4 2 775.060 39.3723 11 -10 -4 -2 821.324 36.4377 8 10 4 3 437.649 30.7265 11 -10 -4 -3 380.049 25.4667 8 10 4 4 35483.7 222.550 11 10 4 4 35948.6 193.989 3 10 4 5 43043.6 234.549 11 -10 -4 -5 42518.4 210.077 8 10 4 6 7265.59 93.3014 11 -10 -4 -6 7633.92 83.1413 8 10 4 7 892.949 32.4207 11 -10 -4 -7 898.290 27.9402 8 10 4 8 6415.73 71.7631 11 10 4 8 6421.92 60.8350 3 -10 -4 -8 6604.14 62.9914 8 -10 -5 5 7803.86 74.0569 8 -10 -5 4 50312.2 205.345 8 10 5 -3 10857.5 102.212 11 -10 -5 3 11091.7 103.513 8 10 5 -2 70027.8 276.020 11 -10 -5 2 72063.5 269.727 8 10 5 -1 46275.0 233.852 11 -10 -5 1 46375.0 225.636 8 10 5 0 8918.93 107.740 11 -10 -5 0 8862.01 100.213 8 10 5 1 8391.93 106.194 11 -10 -5 -1 8711.73 98.5315 8 10 5 2 3148.90 55.6916 3 -10 -5 -2 3302.12 61.5343 8 10 5 3 25569.8 184.456 11 10 5 3 26160.7 156.001 3 10 5 4 15487.0 139.909 11 -10 -5 -4 15160.2 119.734 8 10 5 5 93596.0 332.998 11 -10 -5 -5 94297.4 278.997 8 10 5 6 26434.0 167.071 11 10 5 6 30776.8 150.540 3 10 5 7 706.412 28.0270 11 10 5 7 1038.42 27.5658 3 10 5 8 15398.8 106.011 11 10 5 8 14213.9 82.7365 3 -10 -6 2 67657.2 217.184 8 10 6 -1 114.082 15.6473 11 -10 -6 1 292.509 17.2564 8 10 6 0 25854.2 158.431 11 -10 -6 0 25199.6 141.390 8 10 6 1 29662.7 174.748 11 10 6 1 31473.9 143.689 3 10 6 2 3726.61 65.0048 11 10 6 2 3347.89 50.4170 3 10 6 3 2879.74 57.7105 11 10 6 3 2659.14 45.2589 3 10 6 4 19190.7 117.859 3 10 6 6 80626.3 264.781 11 10 6 6 86277.4 222.356 3 10 6 7 11062.7 91.0054 11 10 6 7 12368.8 76.8056 3 11 0 -2 10444.0 73.0308 3 11 0 0 444.312 18.8842 3 11 0 1 56235.7 181.378 3 11 0 2 8032.62 65.6996 3 11 1 -3 1906.09 38.7665 11 11 1 -2 65105.3 221.065 11 -11 -1 2 71183.8 202.564 8 11 1 -1 4779.92 61.4780 11 -11 -1 1 5084.42 57.4690 8 11 1 0 3359.55 52.0415 11 -11 -1 0 3769.56 51.1827 8 11 1 1 24482.8 126.372 3 -11 -1 -1 23935.5 125.162 8 11 1 2 4913.81 56.0371 3 -11 -1 -2 4943.15 57.5368 8 11 1 3 2626.26 39.9588 3 -11 -1 -3 3080.59 43.3039 8 11 1 4 894.404 22.2929 3 -11 -1 -4 1253.14 26.7924 8 11 2 -3 91.7997 15.1848 11 -11 -2 3 134.887 12.4533 8 11 2 -2 196197. 396.055 11 -11 -2 2 195530. 352.529 8 11 2 -1 2285.87 45.6324 11 -11 -2 1 2506.09 44.2629 8 11 2 0 9452.38 92.6041 11 11 2 0 9779.47 82.5942 3 11 2 1 23120.1 142.080 11 11 2 2 2694.41 48.0942 11 11 2 2 3125.25 47.9854 3 11 2 3 23476.6 120.460 3 -11 -2 -3 24021.1 130.797 8 11 2 4 55812.9 174.279 3 -11 -2 -4 59892.1 190.990 8 -11 -2 -5 2693.41 39.0641 8 11 3 -2 68274.1 233.645 11 -11 -3 2 70224.5 219.405 8 11 3 -1 10925.5 96.8883 11 -11 -3 1 10916.9 87.1695 8 11 3 0 1064.96 33.2234 11 -11 -3 0 1017.30 30.0713 8 11 3 1 9933.42 93.7821 11 11 3 1 9566.15 82.4085 3 11 3 2 5805.74 71.7411 11 -11 -3 -2 6613.64 70.6889 8 11 3 3 11778.1 85.5600 3 -11 -3 -3 11975.7 90.1064 8 11 3 4 68378.3 192.575 3 -11 -3 -4 71783.0 205.288 8 -11 -4 1 12841.3 87.3696 8 11 4 0 698.569 27.0665 11 -11 -4 0 720.922 23.7983 8 11 4 1 5755.58 70.2566 11 11 4 1 5669.57 55.0791 3 11 4 2 47026.0 191.664 11 -11 -4 -2 48251.2 174.452 8 11 4 3 284.816 19.5678 11 -11 -4 -3 35.3957 10.6935 8 11 4 4 10343.5 69.8384 3 0 0 0 0.00 0.00 0 TITL ABER105 in P-1 REM P-1 (#2 in standard setting) CELL 1.54184 9.038047 9.368370 15.020718 81.0313 88.0646 80.0782 ZERR 3.00 0.000132 0.000127 0.000217 0.0012 0.0012 0.0012 LATT 1 SFAC C H N O P Zn UNIT 36.00 30.00 6.00 18.00 3.00 3.00 TREF HKLF 4 END ; _shelx_hkl_checksum 82602 _shelx_res_file ; TITL 105 105.res created by SHELXL-2018/3 at 16:12:12 on 31-Dec-2021 CELL 1.54184 9.03805 9.36837 15.0207 81.0313 88.0646 80.0782 ZERR 2 0.00013 0.00013 0.0002 0.00012 0.00012 0.00012 LATT 1 SFAC C H N O P ZN UNIT 24 48 8 26 8 6 L.S. 6 BOND $H CONF temp -180 size 0.10 0.10 0.10 rem colourless prism mpla 3 o1 o2 o3 p1 mpla 3 o4 o5 o6 p2 mpla 3 o7 o8 o9 p3 mpla 3 o10 o11 o12 p4 acta FMAP 2 htab mpla c1 c2 c3 c4 c5 n1 mpla c7 c8 c9 c10 c11 n3 omit 1 -2 1 PLAN 20 REM Instructions for potential hydrogen bonds EQIV $1 -x, -y+1, -z HTAB N1 O5_$1 HTAB N2 O3 HTAB N2 O10 EQIV $2 -x, -y, -z+1 HTAB N3 O1 EQIV $4 -x, -y, -z HTAB N4 O13_$4 HTAB N4 O2 EQIV $5 -x+1, -y+1, -z HTAB O13 O12_$5 HTAB O13 O4_$3 HTAB C5 O4_$1 HTAB C8 O8_$2 HTAB C11 O7 EQIV $3 -x+1, -y, -z HTAB C11 O13_$3 WGHT 0.045500 2.380700 EXTI 0.005295 FVAR 6.79866 mole 1 ZN1 6 0.247430 0.401031 0.262831 11.00000 0.01172 0.01579 = 0.01205 0.00056 -0.00061 -0.00462 ZN2 6 -0.396861 0.536503 0.373170 11.00000 0.01256 0.01957 = 0.01204 -0.00209 0.00048 -0.00494 ZN3 6 0.360573 0.449622 -0.086061 11.00000 0.01393 0.01878 = 0.01254 0.00086 -0.00082 -0.00717 P1 5 -0.111797 0.494213 0.238146 11.00000 0.01166 0.01349 = 0.01137 0.00082 -0.00039 -0.00409 AFIX 13 1.3200 H1 2 -0.085208 0.618572 0.259906 11.00000 -1.20000 AFIX 0 O1 4 0.034914 0.385762 0.248861 11.00000 0.01117 0.01847 = 0.02464 -0.00095 -0.00137 -0.00460 O2 4 -0.230535 0.442516 0.302858 11.00000 0.01936 0.01903 = 0.01888 -0.00030 0.00756 -0.00468 O3 4 -0.163401 0.525839 0.140742 11.00000 0.01693 0.02859 = 0.01397 0.00385 -0.00331 -0.01006 P2 5 0.438401 0.286499 0.104504 11.00000 0.01170 0.01347 = 0.01282 -0.00031 0.00079 -0.00306 AFIX 13 1.3200 H2 2 0.489858 0.157007 0.080888 11.00000 -1.20000 AFIX 0 O4 4 0.371092 0.255084 0.198751 11.00000 0.01909 0.01863 = 0.01299 0.00160 0.00183 -0.00210 O5 4 0.314233 0.359281 0.036968 11.00000 0.01393 0.02303 = 0.01371 0.00181 -0.00063 -0.00484 O6 4 0.570866 0.365280 0.098600 11.00000 0.01405 0.01885 = 0.02644 -0.00124 -0.00043 -0.00622 P3 5 0.391820 0.303957 0.460608 11.00000 0.01570 0.01474 = 0.01208 0.00017 0.00055 -0.00527 AFIX 13 1.3200 H3 2 0.431225 0.160024 0.476842 11.00000 -1.20000 AFIX 0 O7 4 0.272115 0.334057 0.388557 11.00000 0.02500 0.02902 = 0.01321 0.00048 -0.00284 -0.00812 O8 4 0.324699 0.348793 0.548100 11.00000 0.02226 0.03296 = 0.01442 -0.00647 0.00259 -0.01368 O9 4 0.534367 0.363236 0.431664 11.00000 0.01956 0.02368 = 0.03142 -0.00055 0.00765 -0.00894 P4 5 0.384372 0.699377 0.208562 11.00000 0.01270 0.01290 = 0.01490 -0.00019 -0.00150 -0.00273 AFIX 13 1.3200 H4 2 0.303842 0.832430 0.198557 11.00000 -1.20000 AFIX 0 O10 4 0.270152 0.596948 0.209143 11.00000 0.01795 0.01971 = 0.02849 0.00313 -0.00423 -0.00889 O11 4 0.487218 0.698545 0.127051 11.00000 0.02806 0.02056 = 0.02195 -0.00127 0.00823 -0.00600 O12 4 0.464945 0.683633 0.296929 11.00000 0.02586 0.02573 = 0.02021 -0.00616 -0.00837 0.00034 mole 2 C1 1 0.058908 0.763520 -0.017042 11.00000 0.01400 0.01545 = 0.01479 -0.00263 0.00190 -0.00062 C2 1 0.163515 0.861153 -0.035009 11.00000 0.01302 0.01803 = 0.01769 -0.00307 0.00065 -0.00247 AFIX 43 H2A 2 0.251603 0.845508 0.000413 11.00000 -1.20000 AFIX 0 C3 1 0.138466 0.978123 -0.103209 11.00000 0.01588 0.01541 = 0.02003 -0.00342 0.00491 -0.00320 C4 1 0.005864 0.999824 -0.154697 11.00000 0.02336 0.01732 = 0.01895 0.00210 -0.00042 -0.00237 AFIX 43 H4A 2 -0.014596 1.081128 -0.201535 11.00000 -1.20000 AFIX 0 C5 1 -0.091632 0.904104 -0.136836 11.00000 0.01862 0.01999 = 0.02006 0.00025 -0.00525 -0.00267 AFIX 43 H5 2 -0.179518 0.917499 -0.172217 11.00000 -1.20000 AFIX 0 C6 1 0.247827 1.083387 -0.123011 11.00000 0.01842 0.01762 = 0.03200 0.00016 0.00488 -0.00649 AFIX 137 H6A 2 0.193054 1.184235 -0.129661 11.00000 -1.50000 H6B 2 0.302513 1.067140 -0.178991 11.00000 -1.50000 H6C 2 0.319166 1.067367 -0.073283 11.00000 -1.50000 AFIX 0 N1 3 -0.064961 0.788753 -0.068622 11.00000 0.01525 0.01653 = 0.01956 -0.00069 -0.00068 -0.00533 AFIX 43 H1A 2 -0.130665 0.728796 -0.057878 11.00000 -1.20000 AFIX 0 N2 3 0.077030 0.648452 0.048028 11.00000 0.01738 0.02225 = 0.01897 0.00379 -0.00106 -0.00685 H2N 2 0.007520 0.598042 0.063205 11.00000 -1.20000 H3N 2 0.152446 0.636806 0.082518 11.00000 -1.20000 mole3 C7 1 -0.112559 0.049908 0.363824 11.00000 0.02387 0.02571 = 0.03617 0.00078 0.00437 -0.00435 C8 1 -0.095061 -0.104551 0.392051 11.00000 0.03146 0.02638 = 0.03191 -0.00208 0.00694 -0.00933 AFIX 43 H8 2 -0.178225 -0.153971 0.391019 11.00000 -1.20000 AFIX 0 C9 1 0.042156 -0.181124 0.420618 11.00000 0.02740 0.02137 = 0.03108 -0.00051 0.00416 -0.00606 C10 1 0.168171 -0.109820 0.415830 11.00000 0.02446 0.02750 = 0.04159 -0.00457 -0.00269 -0.00473 AFIX 43 H10 2 0.264069 -0.162712 0.434784 11.00000 -1.20000 AFIX 0 C11 1 0.150071 0.034472 0.383928 11.00000 0.03460 0.03728 = 0.03851 -0.00742 0.00146 -0.01442 AFIX 43 H11 2 0.235379 0.082043 0.376766 11.00000 -1.20000 AFIX 0 C12 1 0.059199 -0.341558 0.452048 11.00000 0.03595 0.01989 = 0.03847 -0.00079 -0.00116 -0.00292 AFIX 137 H12A 2 0.094069 -0.363281 0.514548 11.00000 -1.50000 H12B 2 0.132633 -0.393645 0.413711 11.00000 -1.50000 H12C 2 -0.037868 -0.373520 0.448605 11.00000 -1.50000 AFIX 0 N3 3 0.012963 0.112932 0.361902 11.00000 0.02736 0.01619 = 0.04211 0.00310 0.00272 -0.00985 H4N 2 0.010971 0.199267 0.338377 11.00000 -1.20000 N4 3 -0.240934 0.129151 0.337185 11.00000 0.02468 0.01915 = 0.04147 0.00097 0.00225 -0.00421 H5N 2 -0.321016 0.080824 0.333381 11.00000 -1.20000 H6N 2 -0.249201 0.224842 0.320876 11.00000 -1.20000 mole 4 O13 4 0.495748 0.010344 -0.321319 11.00000 0.03424 0.02811 = 0.03549 0.00158 -0.00847 -0.00884 AFIX 3 H1O 2 0.511797 0.109711 -0.317211 11.00000 -1.20000 H2O 2 0.552497 -0.056389 -0.275011 11.00000 -1.20000 AFIX 0 HKLF 4 REM 105 REM wR2 = 0.0847, GooF = S = 1.104, Restrained GooF = 1.104 for all data REM R1 = 0.0308 for 4831 Fo > 4sig(Fo) and 0.0311 for all 4842 data REM 343 parameters refined using 0 restraints END WGHT 0.0438 2.4271 REM Instructions for potential hydrogen bonds HTAB C5 O4_$1 HTAB N1 O5_$1 HTAB N2 O3 HTAB N2 O10 HTAB C8 O8_$2 HTAB C11 O7 HTAB C11 O13_$3 HTAB N3 O1 HTAB N4 O13_$4 HTAB N4 O2 HTAB O13 O12_$5 HTAB O13 O4_$3 REM Highest difference peak 1.247, deepest hole -0.668, 1-sigma level 0.104 Q1 1 -0.1057 -0.0809 0.4543 11.00000 0.05 1.25 Q2 1 0.1366 0.0561 0.4486 11.00000 0.05 1.11 Q3 1 0.1569 0.9013 -0.0738 11.00000 0.05 0.46 Q4 1 0.1272 0.8099 -0.0393 11.00000 0.05 0.37 Q5 1 0.1851 1.0223 -0.0998 11.00000 0.05 0.36 Q6 1 0.4726 0.6694 0.2619 11.00000 0.05 0.36 Q7 1 0.1024 -0.0434 0.4024 11.00000 0.05 0.35 Q8 1 0.5038 0.3816 0.4072 11.00000 0.05 0.34 Q9 1 0.2670 0.2036 0.4631 11.00000 0.05 0.33 Q10 1 0.4432 0.3227 -0.0324 11.00000 0.05 0.33 Q11 1 0.5116 0.1771 0.1862 11.00000 0.05 0.33 Q12 1 0.3125 0.3515 -0.0041 11.00000 0.05 0.33 Q13 1 0.3576 0.4143 0.5247 11.00000 0.05 0.32 Q14 1 -0.0745 0.8546 -0.0972 11.00000 0.05 0.31 Q15 1 0.3216 0.2722 0.1592 11.00000 0.05 0.31 Q16 1 0.2766 0.5775 -0.1349 11.00000 0.05 0.31 Q17 1 0.0428 -0.2253 0.4218 11.00000 0.05 0.31 Q18 1 -0.1875 0.3811 0.1833 11.00000 0.05 0.31 Q19 1 0.2913 0.8038 0.1617 11.00000 0.05 0.30 Q20 1 -0.1310 0.1572 0.3503 11.00000 0.05 0.30 ; _shelx_res_checksum 349 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Zn Zn1 0.24743(4) 0.40103(4) 0.26283(2) 0.01319(11) Uani d 1 . . Zn Zn2 -0.39686(4) 0.53650(4) 0.37317(2) 0.01450(11) Uani d 1 . . Zn Zn3 0.36057(4) 0.44962(4) -0.08606(2) 0.01489(11) Uani d 1 . . P P1 -0.11180(7) 0.49421(7) 0.23815(4) 0.01223(14) Uani d 1 . . H H1 -0.085208 0.618572 0.259906 0.015 Uiso calc 1 . . O O1 0.0349(2) 0.3858(2) 0.24886(13) 0.0181(4) Uani d 1 . . O O2 -0.2305(2) 0.4425(2) 0.30286(13) 0.0194(4) Uani d 1 . . O O3 -0.1634(2) 0.5258(2) 0.14074(12) 0.0198(4) Uani d 1 . . P P2 0.43840(7) 0.28650(7) 0.10450(4) 0.01276(14) Uani d 1 . . H H2 0.489858 0.157007 0.080888 0.015 Uiso calc 1 . . O O4 0.3711(2) 0.2551(2) 0.19875(12) 0.0175(4) Uani d 1 . . O O5 0.3142(2) 0.3593(2) 0.03697(12) 0.0172(4) Uani d 1 . . O O6 0.5709(2) 0.3653(2) 0.09860(13) 0.0196(4) Uani d 1 . . P P3 0.39182(7) 0.30396(7) 0.46061(4) 0.01410(15) Uani d 1 . . H H3 0.431225 0.160024 0.476842 0.017 Uiso calc 1 . . O O7 0.2721(2) 0.3341(2) 0.38856(12) 0.0223(4) Uani d 1 . . O O8 0.3247(2) 0.3488(2) 0.54810(12) 0.0219(4) Uani d 1 . . O O9 0.5344(2) 0.3632(2) 0.43166(14) 0.0248(4) Uani d 1 . . P P4 0.38437(7) 0.69938(7) 0.20856(4) 0.01361(15) Uani d 1 . . H H4 0.303842 0.832430 0.198557 0.016 Uiso calc 1 . . O O10 0.2702(2) 0.5969(2) 0.20914(14) 0.0220(4) Uani d 1 . . O O11 0.4872(2) 0.6985(2) 0.12705(13) 0.0237(4) Uani d 1 . . O O12 0.4649(2) 0.6836(2) 0.29693(13) 0.0240(4) Uani d 1 . . C C1 0.0589(3) 0.7635(3) -0.01704(17) 0.0150(5) Uani d 1 . . C C2 0.1635(3) 0.8612(3) -0.03501(17) 0.0162(5) Uani d 1 . . H H2A 0.251603 0.845508 0.000413 0.019 Uiso calc 1 . . C C3 0.1385(3) 0.9781(3) -0.10321(18) 0.0171(5) Uani d 1 . . C C4 0.0059(3) 0.9998(3) -0.15470(18) 0.0205(5) Uani d 1 . . H H4A -0.014596 1.081128 -0.201535 0.025 Uiso calc 1 . . C C5 -0.0916(3) 0.9041(3) -0.13684(18) 0.0199(5) Uani d 1 . . H H5 -0.179518 0.917499 -0.172217 0.024 Uiso calc 1 . . C C6 0.2478(3) 1.0834(3) -0.1230(2) 0.0228(6) Uani d 1 . . H H6A 0.193054 1.184235 -0.129661 0.034 Uiso calc 1 . . H H6B 0.302513 1.067140 -0.178991 0.034 Uiso calc 1 . . H H6C 0.319166 1.067367 -0.073283 0.034 Uiso calc 1 . . N N1 -0.0650(2) 0.7888(2) -0.06862(15) 0.0170(4) Uani d 1 . . H H1A -0.130665 0.728796 -0.057878 0.020 Uiso calc 1 . . N N2 0.0770(3) 0.6485(3) 0.04803(16) 0.0198(5) Uani d 1 . . H H2N 0.008(4) 0.598(4) 0.063(2) 0.024 Uiso d 1 . . H H3N 0.152(4) 0.637(4) 0.083(3) 0.024 Uiso d 1 . . C C7 -0.1126(4) 0.0499(3) 0.3638(2) 0.0293(6) Uani d 1 . . C C8 -0.0951(4) -0.1046(3) 0.3921(2) 0.0298(7) Uani d 1 . . H H8 -0.178225 -0.153971 0.391019 0.036 Uiso calc 1 . . C C9 0.0422(4) -0.1811(3) 0.4206(2) 0.0269(6) Uani d 1 . . C C10 0.1682(4) -0.1098(4) 0.4158(2) 0.0312(7) Uani d 1 . . H H10 0.264069 -0.162712 0.434784 0.037 Uiso calc 1 . . C C11 0.1501(4) 0.0345(4) 0.3839(2) 0.0357(7) Uani d 1 . . H H11 0.235379 0.082043 0.376766 0.043 Uiso calc 1 . . C C12 0.0592(4) -0.3416(3) 0.4520(2) 0.0320(7) Uani d 1 . . H H12A 0.094069 -0.363281 0.514548 0.048 Uiso calc 1 . . H H12B 0.132633 -0.393645 0.413711 0.048 Uiso calc 1 . . H H12C -0.037868 -0.373520 0.448605 0.048 Uiso calc 1 . . N N3 0.0130(3) 0.1129(3) 0.3619(2) 0.0287(6) Uani d 1 . . H H4N 0.011(5) 0.199(5) 0.338(3) 0.034 Uiso d 1 . . N N4 -0.2409(3) 0.1292(3) 0.3372(2) 0.0290(6) Uani d 1 . . H H5N -0.321(5) 0.081(5) 0.333(3) 0.035 Uiso d 1 . . H H6N -0.249(5) 0.225(5) 0.321(3) 0.035 Uiso d 1 . . O O13 0.4957(3) 0.0103(2) -0.32132(16) 0.0327(5) Uani d 1 . . H H1O 0.511797 0.109711 -0.317211 0.039 Uiso d 1 . . H H2O 0.552497 -0.056389 -0.275011 0.039 Uiso d 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Zn1 0.01172(17) 0.01579(18) 0.01205(17) -0.00462(13) -0.00061(12) 0.00056(12) Zn2 0.01256(18) 0.01957(19) 0.01204(17) -0.00494(13) 0.00048(12) -0.00209(13) Zn3 0.01393(18) 0.01878(19) 0.01254(17) -0.00717(13) -0.00082(12) 0.00086(13) P1 0.0117(3) 0.0135(3) 0.0114(3) -0.0041(2) -0.0004(2) 0.0008(2) O1 0.0112(8) 0.0185(9) 0.0246(9) -0.0046(7) -0.0014(7) -0.0009(7) O2 0.0194(9) 0.0190(9) 0.0189(9) -0.0047(7) 0.0076(7) -0.0003(7) O3 0.0169(9) 0.0286(10) 0.0140(9) -0.0101(8) -0.0033(7) 0.0039(7) P2 0.0117(3) 0.0135(3) 0.0128(3) -0.0031(2) 0.0008(2) -0.0003(2) O4 0.0191(9) 0.0186(9) 0.0130(8) -0.0021(7) 0.0018(7) 0.0016(7) O5 0.0139(8) 0.0230(9) 0.0137(8) -0.0048(7) -0.0006(7) 0.0018(7) O6 0.0141(9) 0.0189(9) 0.0264(10) -0.0062(7) -0.0004(7) -0.0012(7) P3 0.0157(3) 0.0147(3) 0.0121(3) -0.0053(2) 0.0006(2) 0.0002(2) O7 0.0250(10) 0.0290(10) 0.0132(9) -0.0081(8) -0.0028(7) 0.0005(7) O8 0.0223(10) 0.0330(11) 0.0144(9) -0.0137(8) 0.0026(7) -0.0065(8) O9 0.0196(10) 0.0237(10) 0.0314(11) -0.0089(8) 0.0077(8) -0.0005(8) P4 0.0127(3) 0.0129(3) 0.0149(3) -0.0027(2) -0.0015(2) -0.0002(2) O10 0.0180(9) 0.0197(10) 0.0285(10) -0.0089(8) -0.0042(8) 0.0031(8) O11 0.0281(10) 0.0206(10) 0.0220(10) -0.0060(8) 0.0082(8) -0.0013(8) O12 0.0259(10) 0.0257(10) 0.0202(10) 0.0003(8) -0.0084(8) -0.0062(8) C1 0.0140(11) 0.0154(12) 0.0148(11) -0.0006(9) 0.0019(9) -0.0026(9) C2 0.0130(11) 0.0180(12) 0.0177(12) -0.0025(10) 0.0006(9) -0.0031(10) C3 0.0159(12) 0.0154(12) 0.0200(12) -0.0032(10) 0.0049(10) -0.0034(10) C4 0.0234(14) 0.0173(13) 0.0189(12) -0.0024(11) -0.0004(10) 0.0021(10) C5 0.0186(13) 0.0200(13) 0.0201(13) -0.0027(10) -0.0053(10) 0.0002(10) C6 0.0184(13) 0.0176(13) 0.0320(15) -0.0065(11) 0.0049(11) 0.0002(11) N1 0.0153(10) 0.0165(11) 0.0196(11) -0.0053(8) -0.0007(8) -0.0007(8) N2 0.0174(11) 0.0223(12) 0.0190(11) -0.0069(9) -0.0011(9) 0.0038(9) C7 0.0239(15) 0.0257(15) 0.0362(17) -0.0043(12) 0.0044(12) 0.0008(12) C8 0.0315(16) 0.0264(15) 0.0319(16) -0.0093(13) 0.0069(13) -0.0021(12) C9 0.0274(15) 0.0214(14) 0.0311(15) -0.0061(12) 0.0042(12) -0.0005(11) C10 0.0245(15) 0.0275(16) 0.0416(18) -0.0047(12) -0.0027(13) -0.0046(13) C11 0.0346(18) 0.0373(18) 0.0385(18) -0.0144(15) 0.0015(14) -0.0074(14) C12 0.0360(17) 0.0199(15) 0.0385(17) -0.0029(13) -0.0012(14) -0.0008(12) N3 0.0274(13) 0.0162(12) 0.0421(15) -0.0099(10) 0.0027(11) 0.0031(11) N4 0.0247(13) 0.0191(13) 0.0415(15) -0.0042(10) 0.0023(11) 0.0010(11) O13 0.0342(12) 0.0281(11) 0.0355(12) -0.0088(10) -0.0085(10) 0.0016(9) 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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O7 Zn1 O10 . . 122.18(9) ? O7 Zn1 O4 . . 107.57(8) ? O10 Zn1 O4 . . 110.71(8) ? O7 Zn1 O1 . . 100.42(8) ? O10 Zn1 O1 . . 106.69(8) ? O4 Zn1 O1 . . 108.12(8) ? O9 Zn2 O8 1_455 2_566 115.30(9) ? O9 Zn2 O12 1_455 1_455 118.93(9) ? O8 Zn2 O12 2_566 1_455 102.04(9) ? O9 Zn2 O2 1_455 . 98.33(8) ? O8 Zn2 O2 2_566 . 110.78(8) ? O12 Zn2 O2 1_455 . 111.74(8) ? O6 Zn3 O11 2_665 2_665 110.85(8) ? O6 Zn3 O3 2_665 2_565 110.21(8) ? O11 Zn3 O3 2_665 2_565 115.57(9) ? O6 Zn3 O5 2_665 . 117.10(8) ? O11 Zn3 O5 2_665 . 103.07(8) ? O3 Zn3 O5 2_565 . 99.70(8) ? O2 P1 O3 . . 112.70(11) ? O2 P1 O1 . . 111.00(11) ? O3 P1 O1 . . 111.15(11) ? O2 P1 H1 . . 107.2 ? O3 P1 H1 . . 107.2 ? O1 P1 H1 . . 107.2 ? P1 O1 Zn1 . . 135.03(12) ? P1 O2 Zn2 . . 135.93(12) ? P1 O3 Zn3 . 2_565 132.51(12) ? O6 P2 O4 . . 115.33(11) ? O6 P2 O5 . . 113.41(11) ? O4 P2 O5 . . 110.08(10) ? O6 P2 H2 . . 105.7 ? O4 P2 H2 . . 105.7 ? O5 P2 H2 . . 105.7 ? P2 O4 Zn1 . . 125.40(11) ? P2 O5 Zn3 . . 121.78(11) ? P2 O6 Zn3 . 2_665 146.90(13) ? O9 P3 O7 . . 114.49(12) ? O9 P3 O8 . . 113.97(12) ? O7 P3 O8 . . 110.19(11) ? O9 P3 H3 . . 105.8 ? O7 P3 H3 . . 105.8 ? O8 P3 H3 . . 105.8 ? P3 O7 Zn1 . . 140.37(13) ? P3 O8 Zn2 . 2_566 129.47(12) ? P3 O9 Zn2 . 1_655 141.65(14) ? O12 P4 O11 . . 114.13(12) ? O12 P4 O10 . . 114.03(12) ? O11 P4 O10 . . 112.68(12) ? O12 P4 H4 . . 104.9 ? O11 P4 H4 . . 104.9 ? O10 P4 H4 . . 104.9 ? P4 O10 Zn1 . . 138.13(12) ? P4 O11 Zn3 . 2_665 133.31(12) ? P4 O12 Zn2 . 1_655 138.52(13) ? N2 C1 N1 . . 118.5(2) ? N2 C1 C2 . . 123.2(2) ? N1 C1 C2 . . 118.3(2) ? C3 C2 C1 . . 120.4(2) ? C3 C2 H2A . . 119.8 ? C1 C2 H2A . . 119.8 ? C2 C3 C4 . . 118.8(2) ? C2 C3 C6 . . 121.2(2) ? C4 C3 C6 . . 120.0(2) ? C5 C4 C3 . . 119.7(2) ? C5 C4 H4A . . 120.2 ? C3 C4 H4A . . 120.2 ? C4 C5 N1 . . 120.7(2) ? C4 C5 H5 . . 119.7 ? N1 C5 H5 . . 119.7 ? C3 C6 H6A . . 109.5 ? C3 C6 H6B . . 109.5 ? H6A C6 H6B . . 109.5 ? C3 C6 H6C . . 109.5 ? H6A C6 H6C . . 109.5 ? H6B C6 H6C . . 109.5 ? C1 N1 C5 . . 122.1(2) ? C1 N1 H1A . . 118.9 ? C5 N1 H1A . . 118.9 ? C1 N2 H2N . . 122(2) ? C1 N2 H3N . . 118(2) ? H2N N2 H3N . . 119(3) ? N4 C7 N3 . . 120.2(3) ? N4 C7 C8 . . 122.4(3) ? N3 C7 C8 . . 117.3(3) ? C9 C8 C7 . . 119.6(3) ? C9 C8 H8 . . 120.2 ? C7 C8 H8 . . 120.2 ? C8 C9 C10 . . 120.2(3) ? C8 C9 C12 . . 119.5(3) ? C10 C9 C12 . . 120.2(3) ? C11 C10 C9 . . 118.8(3) ? C11 C10 H10 . . 120.6 ? C9 C10 H10 . . 120.6 ? C10 C11 N3 . . 121.3(3) ? C10 C11 H11 . . 119.4 ? N3 C11 H11 . . 119.4 ? C9 C12 H12A . . 109.5 ? C9 C12 H12B . . 109.5 ? H12A C12 H12B . . 109.5 ? C9 C12 H12C . . 109.5 ? H12A C12 H12C . . 109.5 ? H12B C12 H12C . . 109.5 ? C11 N3 C7 . . 122.5(3) ? C11 N3 H4N . . 116(3) ? C7 N3 H4N . . 121(3) ? C7 N4 H5N . . 118(3) ? C7 N4 H6N . . 121(3) ? H5N N4 H6N . . 122(4) ? H1O O13 H2O . . 108.6 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zn1 O7 . 1.9028(19) ? Zn1 O10 . 1.9283(19) ? Zn1 O4 . 1.9637(19) ? Zn1 O1 . 1.9710(18) ? Zn2 O9 1_455 1.913(2) ? Zn2 O8 2_566 1.9154(19) ? Zn2 O12 1_455 1.945(2) ? Zn2 O2 . 1.9690(19) ? Zn3 O6 2_665 1.9202(19) ? Zn3 O11 2_665 1.936(2) ? Zn3 O3 2_565 1.9499(18) ? Zn3 O5 . 1.9720(18) ? P1 O2 . 1.5142(18) ? P1 O3 . 1.5196(18) ? P1 O1 . 1.5217(19) ? P1 H1 . 1.3200 ? P2 O6 . 1.5043(19) ? P2 O4 . 1.5279(18) ? P2 O5 . 1.5333(18) ? P2 H2 . 1.3200 ? P3 O9 . 1.514(2) ? P3 O7 . 1.517(2) ? P3 O8 . 1.5172(19) ? P3 H3 . 1.3200 ? P4 O12 . 1.5103(19) ? P4 O11 . 1.512(2) ? P4 O10 . 1.5247(19) ? P4 H4 . 1.3200 ? C1 N2 . 1.329(3) ? C1 N1 . 1.349(3) ? C1 C2 . 1.417(4) ? C2 C3 . 1.372(4) ? C2 H2A . 0.9500 ? C3 C4 . 1.416(4) ? C3 C6 . 1.504(4) ? C4 C5 . 1.354(4) ? C4 H4A . 0.9500 ? C5 N1 . 1.363(3) ? C5 H5 . 0.9500 ? C6 H6A . 0.9800 ? C6 H6B . 0.9800 ? C6 H6C . 0.9800 ? N1 H1A . 0.8800 ? N2 H2N . 0.85(4) ? N2 H3N . 0.85(4) ? C7 N4 . 1.304(4) ? C7 N3 . 1.364(4) ? C7 C8 . 1.426(4) ? C8 C9 . 1.368(5) ? C8 H8 . 0.9500 ? C9 C10 . 1.411(4) ? C9 C12 . 1.486(4) ? C10 C11 . 1.346(5) ? C10 H10 . 0.9500 ? C11 N3 . 1.350(4) ? C11 H11 . 0.9500 ? C12 H12A . 0.9800 ? C12 H12B . 0.9800 ? C12 H12C . 0.9800 ? N3 H4N . 0.83(4) ? N4 H5N . 0.93(4) ? N4 H6N . 0.88(4) ? O13 H1O . 0.9780 ? O13 H2O . 0.9570 ? 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_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1A O5 2_565 0.88 1.97 2.833(3) 166 yes N2 H2N O3 . 0.85(4) 2.05(4) 2.853(3) 157(3) yes N2 H3N O10 . 0.85(4) 2.16(4) 2.961(3) 156(3) yes N3 H4N O1 . 0.83(4) 2.07(4) 2.873(3) 163(4) yes N4 H5N O13 2 0.93(4) 1.95(4) 2.871(4) 177(4) yes N4 H6N O2 . 0.88(4) 2.05(4) 2.918(3) 167(4) yes O13 H1O O12 2_665 0.98 2.05 3.028(3) 175 yes O13 H2O O4 2_655 0.96 2.05 2.952(3) 157 yes C5 H5 O4 2_565 0.95 2.64 3.370(3) 134 yes C8 H8 O8 2_556 0.95 2.48 3.350(4) 152 yes C11 H11 O7 . 0.95 2.47 3.199(4) 133 yes C11 H11 O13 2_655 0.95 2.59 3.281(4) 130 yes 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag O2 P1 O1 Zn1 . . . . -131.13(16) ? O3 P1 O1 Zn1 . . . . 102.59(17) ? O3 P1 O2 Zn2 . . . . -89.87(19) ? O1 P1 O2 Zn2 . . . . 144.71(16) ? O2 P1 O3 Zn3 . . . 2_565 14.2(2) ? O1 P1 O3 Zn3 . . . 2_565 139.51(15) ? O6 P2 O4 Zn1 . . . . 74.23(16) ? O5 P2 O4 Zn1 . . . . -55.63(16) ? O6 P2 O5 Zn3 . . . . 37.41(16) ? O4 P2 O5 Zn3 . . . . 168.29(11) ? O4 P2 O6 Zn3 . . . 2_665 -85.7(2) ? O5 P2 O6 Zn3 . . . 2_665 42.5(3) ? O9 P3 O7 Zn1 . . . . 12.1(3) ? O8 P3 O7 Zn1 . . . . 142.09(19) ? O9 P3 O8 Zn2 . . . 2_566 -1.7(2) ? O7 P3 O8 Zn2 . . . 2_566 -132.07(16) ? O7 P3 O9 Zn2 . . . 1_655 47.6(3) ? O8 P3 O9 Zn2 . . . 1_655 -80.5(2) ? O12 P4 O10 Zn1 . . . . -34.6(2) ? O11 P4 O10 Zn1 . . . . 97.6(2) ? O12 P4 O11 Zn3 . . . 2_665 66.5(2) ? O10 P4 O11 Zn3 . . . 2_665 -65.6(2) ? O11 P4 O12 Zn2 . . . 1_655 -67.0(2) ? O10 P4 O12 Zn2 . . . 1_655 64.4(2) ? N2 C1 C2 C3 . . . . 180.0(2) ? N1 C1 C2 C3 . . . . 0.1(4) ? C1 C2 C3 C4 . . . . 0.4(4) ? C1 C2 C3 C6 . . . . 179.7(2) ? C2 C3 C4 C5 . . . . -1.1(4) ? C6 C3 C4 C5 . . . . 179.6(3) ? C3 C4 C5 N1 . . . . 1.3(4) ? N2 C1 N1 C5 . . . . -179.8(2) ? C2 C1 N1 C5 . . . . 0.1(4) ? C4 C5 N1 C1 . . . . -0.8(4) ? N4 C7 C8 C9 . . . . -179.0(3) ? N3 C7 C8 C9 . . . . 3.7(5) ? C7 C8 C9 C10 . . . . -4.7(5) ? C7 C8 C9 C12 . . . . 178.6(3) ? C8 C9 C10 C11 . . . . 0.9(5) ? C12 C9 C10 C11 . . . . 177.5(3) ? C9 C10 C11 N3 . . . . 4.1(5) ? C10 C11 N3 C7 . . . . -5.2(5) ? N4 C7 N3 C11 . . . . -176.2(3) ? C8 C7 N3 C11 . . . . 1.2(5) ?