#------------------------------------------------------------------------------ #$Date: 2019-05-17 13:01:13 +0100 (Fri, 17 May 2019) $ #$Revision: 215255 $ #$URL: svn://www.crystallography.net/cod/cif/3/00/02/3000217.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_3000217 loop_ _publ_author_name 'Br\'azda, Petr' 'Palatinus, Luk\'a\et al. 2015). ; _computing_structure_solution ; SIR2011 (Brla M.C. et al.). ; _diffrn_ambient_temperature 100 _diffrn_detector 'CCD camera Olympus SIS Veleta' _diffrn_detector_area_resol_mean 2048.2048 _diffrn_measurement_device 'Transmission electron microscope' _diffrn_measurement_device_type 'Philips CM120' _diffrn_measurement_method PEDT _diffrn_measurement_specimen_support 'Cu grid with carbon foil' _diffrn_radiation_probe electron _diffrn_radiation_source 'Lanthanum hexaboride cathode' _diffrn_radiation_type electron _diffrn_radiation_wavelength 0.0335 _diffrn_reflns_number 48871 _diffrn_reflns_reduction_process 'data integration using rocking curve profile with PETS' _diffrn_source electron _diffrn_source_voltage 120 _exptl_crystal_colour none _exptl_crystal_density_diffrn 1.290 _exptl_crystal_density_method 'not measured' _exptl_crystal_description ; ribbon-shaped crystal on carbon film of Cu TEM grid ; _exptl_crystal_F_000 1340 _exptl_crystal_size_max 0.001 _exptl_crystal_size_mid 0.0005 _exptl_crystal_size_min 0.00007 _refine_ls_abs_structure_details ' 1132 of Friedel pairs used in the refinement' _refine_ls_extinction_method none _refine_ls_goodness_of_fit_gt 3.01 _refine_ls_goodness_of_fit_ref 2.40 _refine_ls_hydrogen_treatment constr _refine_ls_number_constraints 132 _refine_ls_number_parameters 266 _refine_ls_number_reflns 5071 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1623 _refine_ls_R_factor_gt 0.0986 _refine_ls_structure_factor_coef F _refine_ls_weighting_details w=1/(\s^2^(F)+0.0001F^2^) _refine_ls_weighting_scheme sigma _refine_ls_wR_factor_gt 0.0912 _refine_ls_wR_factor_ref 0.0962 _reflns_number_gt 2985 _reflns_number_total 5071 _reflns_threshold_expression I>3\s(I) _cod_data_source_file SF_L-proline_normal_final_check.cif _cod_data_source_block I _cod_depositor_comments ;By accicent the originally deposited structure had wrong absolute structure. The updated cif corrects this error. Releasing structure 3000217 into public domain as published material. ; _cod_original_cell_volume 3127 _cod_original_formula_sum 'C27 H38 F1 N4 O11 P1' _cod_database_code 3000217 _publcif_info_exptl_table_max_cols 4 _publcif_info_exptl_table_use_headnotes n loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x+1/2,-y,z+1/2 3 -x,y+1/2,-z+1/2 4 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_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.1166(8) 0.6363(2) 0.4136(2) Uiso -0.0031(14) 4 1 d . . . F1 F -0.2480(17) 0.3682(5) 0.5240(5) Uiso 0.018(2) 4 1 d . . . N1 N 0.2355(16) 0.3524(5) 0.6497(5) Uiso 0.020(3) 4 1 d . . . N2 N 0.0104(16) 0.3695(5) 0.4111(5) Uiso 0.014(3) 4 1 d . . . N3 N 0.1952(16) 0.2816(5) 0.3613(5) Uiso 0.012(3) 4 1 d . . . N4 N -0.1053(15) 0.6463(5) 0.3763(5) Uiso 0.011(3) 4 1 d . . . O1 O 0.7649(17) 0.4582(5) 0.6160(4) Uiso 0.020(3) 4 1 d . . . O2 O 0.7219(17) 0.3523(5) 0.6424(5) Uiso 0.031(3) 4 1 d . . . O3 O 0.5360(17) 0.3103(5) 0.3270(5) Uiso 0.027(3) 4 1 d . . . O4 O -0.1485(18) 0.2588(5) 0.4082(5) Uiso 0.027(3) 4 1 d . . . O5 O -0.2472(16) 0.4536(4) 0.4439(4) Uiso 0.009(2) 4 1 d . . . O6 O 0.0571(18) 0.4735(5) 0.5496(6) Uiso 0.029(3) 4 1 d . . . O7 O 0.0620(15) 0.5719(4) 0.4437(5) Uiso 0.010(3) 4 1 d . . . O8 O 0.0619(16) 0.6922(5) 0.4448(5) Uiso 0.018(3) 4 1 d . . . O9 O 0.3651(14) 0.6297(4) 0.3958(4) Uiso 0.010(2) 4 1 d . . . O10 O -0.391(2) 0.6665(6) 0.2844(6) Uiso 0.050(4) 4 1 d . . . O11 O -0.0827(16) 0.7311(5) 0.2953(5) Uiso 0.011(3) 4 1 d . . . C1 C 0.6436(16) 0.4077(5) 0.6318(5) Uiso 0.006(3) 4 1 d . . . C2 C 0.3608(17) 0.4175(5) 0.6359(5) Uiso 0.026(3) 4 1 d . . . C3 C 0.2999(19) 0.4659(6) 0.6736(5) Uiso 0.031(4) 4 1 d . . . C4 C 0.242(3) 0.4233(7) 0.7152(8) Uiso 0.103(6) 4 1 d . . . C5 C 0.268(2) 0.3507(7) 0.6981(6) Uiso 0.054(5) 4 1 d . . . C6 C 0.018(2) 0.3024(5) 0.3950(5) Uiso 0.024(3) 4 1 d . . . C7 C 0.1753(16) 0.4156(5) 0.3977(5) Uiso 0.018(3) 4 1 d . . . C8 C 0.3537(19) 0.3985(5) 0.3666(5) Uiso 0.020(3) 4 1 d . . . C9 C 0.3733(17) 0.3296(5) 0.3500(5) Uiso 0.004(3) 4 1 d . . . C10 C -0.1608(16) 0.3857(5) 0.4491(5) Uiso 0.005(3) 4 1 d . . . C11 C -0.0536(16) 0.3823(5) 0.4966(5) Uiso 0.002(3) 4 1 d . . . C12 C 0.1512(17) 0.3319(5) 0.5030(5) Uiso 0.033(3) 4 1 d . . . C13 C 0.0200(18) 0.4544(5) 0.5039(5) Uiso 0.007(3) 4 1 d . . . C14 C -0.2027(18) 0.4917(4) 0.4787(5) Uiso 0.007(3) 4 1 d . . . C15 C -0.1611(15) 0.5710(4) 0.4665(4) Uiso 0.011(3) 4 1 d . . . C16 C -0.058(2) 0.6234(6) 0.3291(6) Uiso 0.034(4) 4 1 d . . . C17 C -0.167(2) 0.5522(5) 0.3205(5) Uiso 0.032(3) 4 1 d . . . C18 C -0.192(2) 0.6788(6) 0.2973(5) Uiso 0.023(4) 4 1 d . . . C19 C -0.201(2) 0.7898(5) 0.2787(5) Uiso 0.028(4) 4 1 d . . . C20 C -0.001(2) 0.8378(6) 0.2562(6) Uiso 0.057(5) 4 1 d . . . C21 C -0.369(2) 0.8239(7) 0.3093(6) Uiso 0.059(5) 4 1 d . . . C22 C 0.0364(18) 0.7656(5) 0.4356(5) Uiso 0.012(3) 4 1 d . . . C23 C 0.225(2) 0.7966(6) 0.4095(5) Uiso 0.032(4) 4 1 d . . . C24 C 0.211(2) 0.8682(6) 0.4096(5) Uiso 0.038(4) 4 1 d . . . C25 C 0.0088(17) 0.8993(6) 0.4264(5) Uiso 0.018(3) 4 1 d . . . C26 C -0.1637(19) 0.8676(5) 0.4486(5) Uiso 0.022(3) 4 1 d . . . C27 C -0.1370(18) 0.8023(5) 0.4569(5) Uiso 0.019(3) 4 1 d . . . H1c2 H 0.30(10) 0.44(10) 0.60(10) Uiso 0.051 4 1 d . . . H1c3 H 0.46(10) 0.50(10) 0.68(10) Uiso 0.0624 4 1 d . . . H2c3 H 0.14(10) 0.50(10) 0.66(10) Uiso 0.0624 4 1 d . . . H1c4 H 0.05(10) 0.43(10) 0.73(10) Uiso 0.2052 4 1 d . . . H2c4 H 0.38(10) 0.43(10) 0.74(10) Uiso 0.2052 4 1 d . . . H1c5 H 0.45(10) 0.33(10) 0.71(10) Uiso 0.1082 4 1 d . . . H2c5 H 0.12(10) 0.32(10) 0.71(10) Uiso 0.1082 4 1 d . . . H1c7 H 0.17(10) 0.47(10) 0.41(10) Uiso 0.0368 4 1 d . . . H1c8 H 0.48(10) 0.44(10) 0.35(10) Uiso 0.0399 4 1 d . . . H1c10 H -0.30(10) 0.35(10) 0.45(10) Uiso 0.0108 4 1 d . . . H1c12 H 0.33(10) 0.36(10) 0.49(10) Uiso 0.0661 4 1 d . . . H2c12 H 0.15(10) 0.32(10) 0.54(10) Uiso 0.0661 4 1 d . . . H3c12 H 0.12(10) 0.29(10) 0.48(10) Uiso 0.0661 4 1 d . . . H1c13 H 0.20(10) 0.47(10) 0.49(10) Uiso 0.0149 4 1 d . . . H1c14 H -0.36(10) 0.50(10) 0.50(10) Uiso 0.0139 4 1 d . . . H1c15 H -0.31(10) 0.59(10) 0.44(10) Uiso 0.0213 4 1 d . . . H2c15 H -0.14(10) 0.60(10) 0.50(10) Uiso 0.0213 4 1 d . . . H1c23 H 0.37(10) 0.77(10) 0.39(10) Uiso 0.0641 4 1 d . . . H1c24 H 0.36(10) 0.90(10) 0.40(10) Uiso 0.0767 4 1 d . . . H1c25 H -0.01(10) 0.95(10) 0.42(10) Uiso 0.0357 4 1 d . . . H1c26 H -0.33(10) 0.89(10) 0.46(10) Uiso 0.0442 4 1 d . . . H1c27 H -0.26(10) 0.78(10) 0.48(10) Uiso 0.0372 4 1 d . . . H1c16 H 0.14(10) 0.62(10) 0.32(10) Uiso 0.0672 4 1 d . . . H1c17 H -0.12(10) 0.54(10) 0.29(10) Uiso 0.0638 4 1 d . . . H2c17 H -0.09(10) 0.52(10) 0.34(10) Uiso 0.0638 4 1 d . . . H3c17 H -0.37(10) 0.55(10) 0.32(10) Uiso 0.0638 4 1 d . . . H1c19 H -0.33(10) 0.77(10) 0.25(10) Uiso 0.0568 4 1 d . . . H1c20 H 0.12(10) 0.81(10) 0.24(10) Uiso 0.1135 4 1 d . . . H2c20 H -0.10(10) 0.88(10) 0.24(10) Uiso 0.1135 4 1 d . . . H3c20 H 0.11(10) 0.86(10) 0.28(10) Uiso 0.1135 4 1 d . . . H1c21 H -0.26(10) 0.86(10) 0.33(10) Uiso 0.1189 4 1 d . . . H2c21 H -0.51(10) 0.85(10) 0.29(10) Uiso 0.1189 4 1 d . . . H3c21 H -0.47(10) 0.79(10) 0.33(10) Uiso 0.1189 4 1 d . . . loop_ _atom_type_symbol _atom_type_scat_source C International_Tables_Vol_C H International_Tables_Vol_C F International_Tables_Vol_C N International_Tables_Vol_C O International_Tables_Vol_C P International_Tables_Vol_C loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance P1 N4 . . 1.639(13) P1 O7 . . 1.575(12) P1 O8 . . 1.467(13) P1 O9 . . 1.433(10) F1 C11 . . 1.351(15) N1 C2 . . 1.494(14) N1 C5 . . 1.46(2) N2 C6 . . 1.397(15) N2 C7 . . 1.321(14) N2 C10 . . 1.492(17) N3 C6 . . 1.441(18) N3 C9 . . 1.377(13) N4 C16 . . 1.51(2) O1 C1 . . 1.269(14) O2 C1 . . 1.204(15) O3 C9 . . 1.170(16) O4 C6 . . 1.293(15) O5 C10 . . 1.413(13) O5 C14 . . 1.304(17) O6 C13 . . 1.43(2) O7 C15 . . 1.372(13) O8 C22 . . 1.467(14) O10 C18 . . 1.152(17) O11 C18 . . 1.178(14) O11 C19 . . 1.400(15) C1 C2 . . 1.524(13) C2 C3 . . 1.51(2) C3 C4 . . 1.53(3) C4 C5 . . 1.51(2) C7 C8 . . 1.373(17) C8 C9 . . 1.439(15) C10 C11 . . 1.538(19) C11 C12 . . 1.482(13) C11 C13 . . 1.479(13) C13 C14 . . 1.585(15) C14 C15 . . 1.607(13) C16 C17 . . 1.529(15) C16 C18 . . 1.609(19) C19 C20 . . 1.573(18) C19 C21 . . 1.446(19) C22 C23 . . 1.410(17) C22 C27 . . 1.333(16) C23 C24 . . 1.401(16) C24 C25 . . 1.335(16) C25 C26 . . 1.294(16) C26 C27 . . 1.308(15) loop_ _refln_index_h _refln_index_k _refln_index_l _refln_intensity_calc _refln_intensity_meas _refln_intensity_sigma _refln_scale_group_code _refln_observed_status -1 -14 -20 208.15 44.50 44.30 1%1 < 0 -13 -18 59.89 2.20 43.70 1%1 < -2 -12 -18 31.13 -7.80 43.50 1%1 < -3 -11 -17 40.04 87.70 43.40 1%1 < 1 -12 -16 756.78 683.20 51.50 1%1 o -1 -11 -16 237.56 209.90 45.80 1%1 o 2 -11 -14 529.52 452.00 51.10 1%1 o 0 -10 -14 148.23 137.10 45.30 1%1 o -3 -8 -13 117.39 31.70 44.30 1%1 < 3 -10 -12 870.53 737.70 51.80 1%1 o 1 -9 -12 1340.00 1462.50 59.70 1%1 o -4 -7 -12 242.14 195.40 46.50 1%1 o 4 -10 -11 181.32 49.80 45.10 1%1 < -2 -7 -11 229.48 499.70 50.10 1%1 o 3 -8 -9 51.32 26.10 45.30 1%1 < -4 -4 -8 120.55 172.10 45.80 1%1 o 4 -7 -7 228.82 139.60 46.30 1%1 o 2 -6 -7 759.86 721.10 54.20 1%1 o -5 -3 -7 7.57 25.10 43.50 1%1 < -3 -3 -6 603.38 652.30 51.70 1%1 o 3 -5 -5 722.96 692.40 52.20 1%1 o 1 -4 -5 4600.00 4448.40 86.90 1%1 o -4 -2 -5 444.87 578.30 49.70 1%1 o 4 -5 -4 304.04 199.20 48.10 1%1 o -2 -2 -4 8078.30 8106.30 105.60 1%1 o -5 -1 -4 140.51 122.70 44.40 1%1 < 5 -4 -2 153.33 99.40 47.00 1%1 < 4 -2 0 248.44 14.60 45.40 1%1 < 2 -1 0 114.28 85.20 52.20 1%1 < 5 -2 1 63.12 111.60 45.70 1%1 < -4 3 2 978.32 1074.70 56.30 1%1 o 4 0 3 288.59 333.10 47.30 1%1 o -5 4 3 234.96 281.60 46.30 1%1 o 5 0 4 603.03 517.70 49.70 1%1 o -3 4 4 322.00 299.90 47.80 1%1 o 3 2 5 455.15 412.50 49.80 1%1 o 1 3 5 6035.60 6362.60 101.60 1%1 o -4 5 5 679.50 544.70 49.50 1%1 o 4 2 6 115.25 5.20 44.60 1%1 < -2 5 6 279.94 224.70 49.90 1%1 o -3 6 7 734.17 703.30 51.10 1%1 o 3 4 8 928.10 1051.80 56.20 1%1 o 1 5 8 412.50 236.30 51.90 1%1 o -1 6 8 3399.30 3606.20 79.00 1%1 o -4 7 8 114.89 164.70 44.90 1%1 o -2 7 9 2045.30 2096.70 64.20 1%1 o -3 8 10 95.72 183.30 44.60 1%1 o 3 6 11 137.81 124.90 46.50 1%1 < -1 8 11 576.76 444.00 50.10 1%1 o -4 9 11 25.91 146.60 43.80 1%1 o -2 9 12 999.85 1127.60 56.90 1%1 o 2 8 13 471.76 191.10 45.90 1%1 o -3 10 13 426.39 473.50 49.40 1%1 o 3 8 14 454.72 268.90 47.50 1%1 o -1 10 14 544.09 554.20 49.50 1%1 o -2 11 15 376.66 320.10 48.60 1%1 o 2 10 16 55.21 -3.00 44.20 1%1 < -3 12 16 63.52 -13.70 44.30 1%1 < 3 10 17 213.86 163.90 45.30 1%1 o 1 11 17 266.08 233.20 46.60 1%1 o -1 12 17 159.12 149.60 45.60 1%1 o -2 13 18 95.03 -28.10 44.50 1%1 < 2 12 19 553.61 140.90 47.30 1%1 < 1 13 20 170.72 77.90 45.10 1%1 < -1 14 20 182.20 151.30 45.40 1%1 o 0 -14 -20 75.81 44.70 43.90 2%1 < 1 -13 -18 123.52 5.70 44.60 2%1 < -2 -11 -17 302.45 240.50 47.00 2%1 o 2 -12 -16 56.25 -52.60 44.50 2%1 < 0 -11 -16 268.52 328.40 47.70 2%1 o -3 -10 -16 152.02 148.50 44.60 2%1 o -1 -10 -15 296.12 92.20 45.10 2%1 < 3 -11 -14 213.63 233.50 47.00 2%1 o -2 -9 -14 236.55 231.10 45.70 2%1 o 0 -9 -13 78.55 124.60 46.10 2%1 < -4 -7 -12 349.05 311.30 45.50 2%1 o 3 -9 -11 403.34 257.20 46.70 2%1 o 1 -8 -11 902.09 658.10 52.30 2%1 o 4 -8 -9 120.57 99.10 45.20 2%1 < 2 -7 -9 2499.90 2549.50 69.00 2%1 o -2 -4 -7 5518.10 5845.00 92.80 2%1 o 4 -6 -6 79.00 7.50 45.10 2%1 < 2 -5 -6 192.53 487.20 51.40 2%1 o -3 -3 -6 935.07 857.10 55.20 2%1 o -1 -3 -5 5682.80 6182.10 101.10 2%1 o -4 -2 -5 421.76 429.40 48.40 2%1 o -2 -2 -4 9475.50 9274.00 113.30 2%1 o -5 -1 -4 78.87 125.50 44.10 2%1 < 4 -4 -3 48.24 -0.60 46.10 2%1 < -3 -1 -3 1265.40 1507.50 60.90 2%1 o -4 0 -2 82.93 265.70 47.80 2%1 o 3 -2 -1 426.46 346.80 49.10 2%1 o -5 1 -1 150.26 -6.20 44.50 2%1 < -3 1 0 2674.80 3228.80 74.80 2%1 o -4 2 1 495.58 339.40 48.10 2%1 o 5 -1 2 183.85 66.90 45.70 2%1 < 3 0 2 66.82 85.40 47.20 2%1 < -5 3 2 37.79 125.60 44.50 2%1 < 0 2 3 16070.00 17702.00 162.40 2%1 o -4 4 4 522.33 272.40 48.30 2%1 o 5 1 5 64.47 31.60 44.60 2%1 < 3 2 5 419.56 372.10 51.20 2%1 o -5 5 5 241.29 168.00 44.80 2%1 o 0 4 6 4337.70 3879.50 87.10 2%1 o -3 5 6 293.96 362.10 50.80 2%1 o -4 6 7 1500.40 1162.80 56.80 2%1 o 5 3 8 31.34 27.80 44.30 2%1 < 3 4 8 1477.40 1588.20 60.80 2%1 o 0 6 9 601.73 429.80 56.60 2%1 o -3 7 9 120.12 193.80 46.00 2%1 o -1 7 10 1761.70 1547.90 61.20 2%1 o -4 8 10 240.25 160.80 45.70 2%1 o 3 6 11 173.38 204.10 46.30 2%1 o -2 8 11 425.71 406.50 49.30 2%1 o 4 6 12 190.94 347.30 47.10 2%1 o 0 8 12 2742.20 2416.90 68.50 2%1 o -3 9 12 205.60 136.80 45.90 2%1 < -1 9 13 712.07 690.00 52.20 2%1 o 3 8 14 559.02 371.30 47.80 2%1 o -2 10 14 256.31 539.70 50.00 2%1 o 4 8 15 106.39 43.10 44.90 2%1 < 2 9 15 309.40 242.50 46.30 2%1 o -3 11 15 165.81 167.50 44.50 2%1 o -1 11 16 129.36 46.00 47.00 2%1 < -2 12 17 1456.80 1193.90 55.80 2%1 o 2 11 18 144.57 127.20 45.40 2%1 < 1 12 19 103.11 -3.30 45.10 2%1 < 0 13 20 34.44 42.20 44.80 2%1 < -1 -12 -18 50.39 82.20 45.00 3%1 < 1 -12 -17 184.08 123.70 46.20 3%1 < -2 -11 -17 365.41 374.60 47.90 3%1 o 0 -11 -16 317.92 233.80 46.10 3%1 o -3 -10 -16 131.62 182.10 44.60 3%1 o -1 -10 -15 400.62 100.30 45.10 3%1 < 1 -10 -14 741.53 678.30 51.10 3%1 o -3 -8 -13 145.34 -93.20 45.40 3%1 < 4 -10 -12 258.59 142.50 47.20 3%1 o 2 -9 -12 1184.70 1286.70 57.80 3%1 o -4 -7 -12 312.62 188.50 45.20 3%1 o 3 -8 -10 157.71 125.20 47.70 3%1 < 4 -8 -9 147.06 23.10 45.50 3%1 < 2 -7 -9 2736.60 2777.70 69.10 3%1 o -5 -4 -8 225.71 108.20 45.20 3%1 < 3 -6 -7 611.73 711.30 52.30 3%1 o -2 -4 -7 6719.50 6438.60 96.30 3%1 o -1 -3 -5 5535.10 6201.40 100.80 3%1 o -5 -2 -5 374.64 132.90 46.80 3%1 < 5 -5 -4 102.29 -12.10 45.00 3%1 < 3 -4 -4 467.41 248.20 48.30 3%1 o -2 -2 -4 10321.00 9939.30 114.60 3%1 o 0 -2 -3 17779.00 17153.00 160.60 3%1 o -3 -1 -3 2370.40 3458.90 75.00 3%1 o 4 -3 -2 826.43 902.00 54.30 3%1 o -1 -1 -2 22954.00 20888.20 165.70 3%1 o -5 0 -2 38.93 41.10 44.00 3%1 < 5 -3 -1 229.36 185.70 44.80 3%1 o 3 -2 -1 365.29 361.70 48.70 3%1 o -2 0 -1 552.28 1656.70 65.70 3%1 o -3 1 0 3536.90 3696.40 78.40 3%1 o 4 -1 1 712.87 639.00 51.70 3%1 o -1 1 1 40839.00 39293.30 219.00 3%1 o -5 2 1 27.75 63.90 44.70 3%1 < 5 -1 2 145.53 197.50 45.70 3%1 o -2 2 2 1296.70 1516.10 64.40 3%1 o 0 2 3 16829.00 15711.40 156.20 3%1 o -3 3 3 215.27 108.70 47.20 3%1 < 4 1 4 159.67 201.40 47.40 3%1 o -1 3 4 1582.50 1326.20 72.70 3%1 o -5 4 4 144.63 137.70 44.80 3%1 o 5 1 5 95.92 41.70 45.00 3%1 < 3 2 5 503.50 665.70 52.90 3%1 o -2 4 5 254.19 460.80 53.20 3%1 o 0 4 6 3212.40 3201.90 82.20 3%1 o -3 5 6 331.71 314.80 50.80 3%1 o 4 3 7 109.69 121.70 46.10 3%1 < -1 5 7 3282.70 3413.30 79.00 3%1 o 5 3 8 20.48 14.90 44.00 3%1 < 3 4 8 1686.10 1795.10 62.50 3%1 o -2 6 8 317.67 429.30 50.80 3%1 o -1 7 10 1988.10 1903.70 63.80 3%1 o 3 6 11 279.04 288.10 47.20 3%1 o -4 9 12 218.30 147.80 45.10 3%1 o 3 8 14 441.42 232.00 47.50 3%1 o -3 10 14 175.21 -20.20 45.30 3%1 < 4 8 15 93.08 38.90 44.30 3%1 < 2 9 15 155.27 234.70 46.50 3%1 o 1 10 16 258.49 231.60 47.20 3%1 o -2 11 16 647.94 465.70 50.00 3%1 o 0 11 17 940.68 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182.13 305.80 49.20 3%2 o 5 -6 3 184.27 159.90 46.50 3%2 o -3 -10 4 127.18 106.00 47.30 3%2 < -2 -10 4 1257.60 1459.00 61.30 3%2 o -1 -10 4 408.72 348.60 53.60 3%2 o 0 -10 4 120.44 93.10 51.00 3%2 < 1 -10 4 283.61 289.10 52.30 3%2 o 4 -9 4 289.75 116.30 45.00 3%2 < -4 -12 5 39.46 -64.80 44.70 3%2 < -3 -12 5 532.14 273.20 48.30 3%2 o 2 -12 5 315.20 313.50 49.80 3%2 o 3 -12 5 270.42 168.90 48.20 3%2 o -1 -15 6 976.54 1045.70 57.70 3%2 o 0 -15 6 49.36 -54.70 46.70 3%2 < 3 -14 6 118.19 123.40 46.30 3%2 < -2 -17 7 145.06 118.50 45.70 3%2 < -1 -17 7 582.42 467.50 50.70 3%2 o 0 -17 7 39.33 51.50 46.20 3%2 < 1 -17 7 519.67 386.30 49.80 3%2 o 2 -17 7 222.68 265.80 47.50 3%2 o 0 16 -6 128.92 150.60 45.90 4%2 o 1 16 -6 136.14 125.80 47.90 4%2 < 2 16 -6 639.33 740.30 53.50 4%2 o -2 17 -6 35.58 69.00 46.50 4%2 < -1 17 -6 356.65 454.20 50.60 4%2 o 1 13 -5 230.20 174.80 48.80 4%2 o 2 13 -5 177.45 257.30 47.80 4%2 o 3 13 -5 79.83 76.00 46.20 4%2 < -2 14 -5 325.10 396.60 49.50 4%2 o -1 14 -5 24.84 51.50 47.10 4%2 < -3 15 -5 61.33 83.00 46.40 4%2 < 2 10 -4 1675.20 1409.00 61.90 4%2 o 3 10 -4 93.30 64.10 46.80 4%2 < 4 10 -4 100.02 -12.70 46.80 4%2 < -1 11 -4 189.23 162.00 49.90 4%2 o -3 12 -4 248.53 238.10 48.20 4%2 o 0 8 -3 8749.40 8388.20 113.10 4%2 o -3 9 -3 554.03 664.10 53.80 4%2 o -4 10 -3 90.67 72.60 46.70 4%2 < 1 5 -2 2527.40 2715.40 80.40 4%2 o 4 5 -2 120.69 163.30 46.90 4%2 o 5 5 -2 108.98 122.80 45.70 4%2 < -2 6 -2 1932.70 2050.80 69.40 4%2 o -4 7 -2 676.56 974.60 56.80 4%2 o 3 2 -1 96.45 9.10 49.10 4%2 < 4 2 -1 491.98 374.80 50.30 4%2 o 5 2 -1 69.01 84.70 46.70 4%2 < -1 3 -1 4053.30 4208.00 96.60 4%2 o -3 4 -1 953.71 1242.60 58.90 4%2 o -5 5 -1 35.48 15.10 46.40 4%2 < -4 2 0 169.13 40.20 46.40 4%2 < 2 -3 1 2086.80 2037.80 71.00 4%2 o 3 -3 1 260.56 429.40 53.30 4%2 o 4 -3 1 807.63 604.90 53.10 4%2 o 5 -3 1 128.90 53.70 45.20 4%2 < -5 0 1 129.01 223.30 47.10 4%2 o 0 -5 2 330.79 385.10 67.00 4%2 o 5 -5 2 114.01 99.90 45.50 4%2 < -3 -4 2 1500.30 962.10 60.30 4%2 o -4 -3 2 635.92 848.10 56.00 4%2 o 2 -8 3 719.27 375.90 52.40 4%2 o 3 -8 3 348.55 461.20 49.70 4%2 o 4 -8 3 175.03 304.50 47.30 4%2 o -5 -5 3 162.09 293.60 47.00 4%2 o 0 -10 4 140.17 213.50 51.20 4%2 o 1 -10 4 417.10 464.90 53.20 4%2 o 2 -10 4 1438.00 1269.80 60.40 4%2 o 3 -10 4 107.85 121.10 47.70 4%2 < 4 -10 4 30.93 13.90 44.60 4%2 < -2 -9 4 140.80 84.80 47.20 4%2 < -4 -8 4 326.01 351.90 49.80 4%2 o -1 -12 5 709.08 610.30 54.90 4%2 o -3 -11 5 530.63 471.00 48.80 4%2 o 1 -15 6 1009.20 1113.20 58.40 4%2 o 2 -15 6 201.77 219.90 48.10 4%2 o 3 -15 6 415.70 412.30 48.70 4%2 o -2 -14 6 342.25 303.20 49.90 4%2 o -1 -14 6 229.34 158.80 47.60 4%2 o 0 -17 7 35.26 21.70 46.00 4%2 < 1 -17 7 497.01 384.80 50.30 4%2 o 2 -17 7 178.47 203.60 47.90 4%2 o -2 -16 7 95.40 73.40 45.40 4%2 < 1 18 -7 173.75 95.80 47.10 5%2 < 2 15 -6 149.01 158.10 48.60 5%2 o 0 16 -6 70.79 35.80 46.20 5%2 < -1 17 -6 408.16 534.50 50.20 5%2 o 2 12 -5 434.81 325.90 50.50 5%2 o 3 12 -5 393.27 271.20 49.90 5%2 o 0 13 -5 1064.80 771.00 53.70 5%2 o -1 14 -5 80.19 130.00 46.50 5%2 < 3 9 -4 40.46 -4.90 47.60 5%2 < 4 9 -4 433.35 168.50 46.00 5%2 o 1 10 -4 579.79 723.60 55.20 5%2 o -1 11 -4 298.03 304.50 51.10 5%2 o -2 12 -4 59.10 140.20 47.80 5%2 < -3 13 -4 583.81 354.00 50.60 5%2 o 4 6 -3 288.10 113.20 47.50 5%2 < 5 6 -3 230.39 249.30 47.30 5%2 o -2 9 -3 2006.10 1911.90 68.40 5%2 o -3 10 -3 120.17 112.30 46.40 5%2 < -4 11 -3 53.66 20.70 45.10 5%2 < 2 4 -2 393.65 434.70 56.80 5%2 o -4 8 -2 112.47 61.30 46.30 5%2 < 4 1 -1 467.51 481.60 51.30 5%2 o 5 1 -1 65.95 -42.00 45.10 5%2 < 1 2 -1 603.98 1187.50 79.70 5%2 o -2 4 -1 272.11 375.70 54.60 5%2 o 5 -2 0 785.32 788.00 53.90 5%2 o 2 -1 0 218.29 239.90 55.00 5%2 o -3 2 0 1533.70 1536.70 63.70 5%2 o -4 3 0 19.09 9.40 46.40 5%2 < -5 4 0 22.02 124.70 46.70 5%2 < 4 -4 1 314.76 377.20 50.50 5%2 o 5 -4 1 113.42 82.00 45.80 5%2 < 1 -3 1 3668.70 3923.80 95.80 5%2 o 2 -6 2 1919.50 1864.40 69.10 5%2 o 3 -6 2 30.79 105.20 46.50 5%2 < 0 -5 2 276.50 256.70 66.60 5%2 o -3 -3 2 433.46 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3 165.92 39.40 54.40 6%2 < 0 -7 3 1075.80 934.30 66.80 6%2 o -4 -3 3 220.11 185.20 48.20 6%2 o -5 -2 3 40.22 12.80 45.60 6%2 < 4 -12 4 25.95 79.10 44.00 6%2 < 2 -11 4 123.69 123.70 48.20 6%2 < 1 -10 4 390.34 401.30 54.70 6%2 o -5 -4 4 146.54 150.90 45.30 6%2 o 2 -13 5 100.60 169.20 47.60 6%2 o -2 -10 5 378.20 315.60 51.40 6%2 o -3 -9 5 139.41 378.80 49.20 6%2 o -4 -8 5 639.54 636.20 53.10 6%2 o 2 -15 6 97.19 152.20 48.00 6%2 o 0 -14 6 200.36 265.90 49.40 6%2 o -1 -13 6 73.47 129.80 49.20 6%2 < -2 -12 6 272.88 556.40 53.80 6%2 o -3 -11 6 306.03 306.10 48.60 6%2 o -4 -10 6 312.36 260.60 48.40 6%2 o 1 -17 7 424.58 359.20 51.00 6%2 o 0 -16 7 22.30 78.90 47.70 6%2 < -1 -15 7 157.34 344.50 49.60 6%2 o -4 -12 7 61.33 1.70 44.70 6%2 < 0 -18 8 70.64 21.50 46.20 6%2 < 3 14 -7 137.58 99.70 46.40 7%2 < 2 15 -7 609.81 447.10 51.30 7%2 o 4 11 -6 38.47 85.40 45.10 7%2 < 1 14 -6 190.32 111.30 47.00 7%2 < 0 15 -6 118.79 171.20 46.60 7%2 o -1 16 -6 178.86 145.10 47.40 7%2 o 4 8 -5 571.82 628.10 52.20 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18%4 < -3 -10 10 659.21 852.60 61.00 18%4 o -3 -9 10 137.39 -64.40 53.90 18%4 < -3 9 10 181.87 113.20 53.60 18%4 < -3 10 10 576.54 680.50 61.20 18%4 o -3 11 10 43.14 152.90 52.00 18%4 < -3 12 10 83.02 181.70 50.20 18%4 o -3 13 10 75.75 -12.70 50.70 18%4 < -3 14 10 412.23 376.90 53.40 18%4 o 3 -14 -11 11.39 57.90 51.50 19%4 < 3 -13 -11 64.05 52.90 52.20 19%4 < 3 -12 -11 150.86 220.70 53.50 19%4 o 3 -11 -11 366.07 441.30 55.10 19%4 o 3 -10 -11 157.39 183.40 53.40 19%4 o 3 10 -11 193.28 98.30 53.80 19%4 < 3 11 -11 443.27 455.60 54.20 19%4 o 3 12 -11 274.64 193.80 54.80 19%4 o 3 13 -11 58.10 185.10 50.50 19%4 o 3 14 -11 21.50 64.10 49.30 19%4 < 1 -19 -4 134.53 91.20 48.30 19%4 < 1 -18 -4 159.91 84.70 51.10 19%4 < 1 -17 -4 37.87 37.90 50.80 19%4 < 1 -16 -4 35.40 117.70 53.60 19%4 < 1 16 -4 51.94 103.30 54.50 19%4 < 1 17 -4 49.12 -16.10 51.00 19%4 < 1 18 -4 97.25 122.30 50.80 19%4 < 1 19 -4 59.25 72.40 48.60 19%4 < 0 -4 0 45521.00 44568.50 263.70 19%4 o 0 -2 0 4758.50 3180.90 156.10 19%4 o 0 2 0 6181.30 5072.80 166.20 19%4 o 0 4 0 49437.00 56244.50 280.80 19%4 o -1 -19 3 60.41 -66.70 48.50 19%4 < -1 -18 3 152.96 262.20 50.50 19%4 o -1 -17 3 93.78 60.80 51.70 19%4 < -1 -16 3 188.58 300.10 54.40 19%4 o -1 -15 3 137.76 172.40 55.50 19%4 o -1 15 3 119.02 179.60 55.70 19%4 o -1 16 3 121.98 100.80 53.10 19%4 < -1 17 3 107.17 95.70 51.20 19%4 < -1 18 3 183.70 182.20 51.20 19%4 o -1 19 3 78.16 26.50 47.80 19%4 < -3 -14 10 494.11 408.50 53.80 19%4 o -3 -13 10 14.53 149.80 50.60 19%4 < -3 -12 10 79.57 -85.10 52.40 19%4 < -3 -11 10 29.68 25.90 53.60 19%4 < -3 -10 10 642.79 893.40 61.80 19%4 o -3 -9 10 125.12 113.00 54.90 19%4 < -3 -8 10 30.00 -5.70 52.90 19%4 < -3 8 10 94.91 106.90 54.60 19%4 < -3 9 10 147.40 229.30 54.30 19%4 o -3 10 10 559.66 817.60 60.70 19%4 o -3 11 10 37.47 113.30 52.60 19%4 < -3 12 10 73.31 109.50 51.00 19%4 < -3 13 10 40.18 0.40 50.50 19%4 < -3 14 10 351.73 273.50 53.10 19%4 o loop_ _reflns_scale_group_code _reflns_scale_meas_intensity 1%1 1180.485 2%1 1237.885 3%1 1296.117 4%1 1219.695 5%1 1210.973 6%1 1199.827 7%1 1120.227 8%1 1190.823 9%1 1216.276 10%1 1189.842 11%1 1098.187 12%1 1037.626 13%1 1037.045 32%1 756.489 33%1 817.775 34%1 798.031 35%1 847.094 36%1 784.625 37%1 834.999 38%1 784.705 39%1 799.823 40%1 755.169 41%1 745.867 42%1 761.476 43%1 675.366 44%1 521.987 1%2 807.377 2%2 1001.826 3%2 970.186 4%2 998.260 5%2 1006.077 6%2 905.807 7%2 934.551 8%2 942.463 9%2 890.781 10%2 901.799 11%2 826.716 12%2 868.765 13%2 833.572 14%2 798.759 15%2 806.949 16%2 722.439 17%2 793.613 18%2 841.917 19%2 825.829 20%2 803.611 21%2 794.943 22%2 755.539 23%2 815.646 24%2 741.026 25%2 823.759 26%2 843.182 27%2 792.645 1%3 1202.232 2%3 1425.929 3%3 1299.661 4%3 1336.262 5%3 1255.834 6%3 1223.100 7%3 1062.617 8%3 1049.401 9%3 911.222 10%3 902.622 11%3 995.617 12%3 905.787 13%3 942.826 14%3 950.501 1%4 1139.569 2%4 1154.458 3%4 1204.934 4%4 1162.252 5%4 1095.408 6%4 1238.863 7%4 1123.220 8%4 944.948 9%4 903.649 10%4 1032.365 11%4 900.043 12%4 765.274 13%4 856.422 14%4 919.834 15%4 963.184 16%4 811.336 17%4 772.306 18%4 774.568 19%4 753.410