#------------------------------------------------------------------------------ #$Date: 2019-08-20 07:06:37 +0300 (Tue, 20 Aug 2019) $ #$Revision: 217608 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/17/2021747.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_2021747 loop_ _publ_author_name 'Zhou, Lian' 'Shi, Pei-Dong' 'Guo, Xiao-Kun' 'Feng, Xiu-Cun' 'Wang, Lin-Lin' 'Zhang, Jun' _publ_section_title ; A new lanthanum coordination polymer built from a semi-rigid tripodal carboxylic acid ligand: synthesis, crystal structure and properties ; _journal_coeditor_code YP3192 _journal_issue 9 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first ; ; _journal_paper_doi 10.1107/S2053229619011240 _journal_volume 75 _journal_year 2019 _chemical_formula_iupac '[La (C33 H27 O9) (C3 H7 N O)2], 4C3 H7 N O, 0.25H2 O' _chemical_formula_moiety 'C39 H41 La N2 O11, 4(C3 H7 N O), 0.25(H2 O)' _chemical_formula_sum 'C51 H69.5 La N6 O15.25' _chemical_formula_weight 1149.53 _chemical_name_systematic ;Poly[[bis(dimethylformamide)(\m~6~-4,4',4''-{[(2,4,6-trimethylbenzene-1,3,5-triyl)tris(methylene)]tris(oxy)}tribenzoato)lanthanum(III)] dimethylformamide tetrasolvate 0.25-hydrate] ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_method ; Olex2 1.2-beta (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 77.482(3) _cell_angle_beta 73.859(3) _cell_angle_gamma 85.101(2) _cell_formula_units_Z 2 _cell_length_a 12.947(3) _cell_length_b 13.889(3) _cell_length_c 16.2890(11) _cell_measurement_reflns_used 1570 _cell_measurement_temperature 291(2) _cell_measurement_theta_max 20.458 _cell_measurement_theta_min 2.197 _cell_volume 2745.8(9) _computing_cell_refinement ; SAINT (Bruker, 2009) ; _computing_data_collection ; APEX2 (Bruker, 2009) ; _computing_data_reduction ; SAINT (Bruker, 2009) ; _computing_molecular_graphics ; OLEX2 (Dolomanov et al., 2009) ; _computing_publication_material ; OLEX2 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015) ; _computing_structure_solution ; SHELXS97 (Sheldrick, 2008) ; _diffrn_ambient_temperature 291.15 _diffrn_detector 'Bruker APEXII area detector' _diffrn_detector_area_resol_mean 7.9 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART APEXII area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_unetI/netI 0.0954 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 23526 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.999 _diffrn_reflns_theta_min 1.502 _diffrn_source 'microfocus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.848 _exptl_absorpt_correction_T_max 0.8354 _exptl_absorpt_correction_T_min 0.7972 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2008) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1193 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _refine_diff_density_max 0.847 _refine_diff_density_min -0.685 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 680 _refine_ls_number_reflns 11881 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.014 _refine_ls_R_factor_all 0.0698 _refine_ls_R_factor_gt 0.0599 _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^)+(0.0890P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1450 _refine_ls_wR_factor_ref 0.1470 _reflns_number_gt 8526 _reflns_number_total 11881 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file yp3192sup1.cif _cod_data_source_block I _cod_original_formula_sum 'C51 H69.50 La N6 O15.25' _cod_database_code 2021747 _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 0.797 _shelx_estimated_absorpt_t_max 0.835 _shelx_hkl_file ; -2 0 0 587.05 86.46 -3 0 0 3317.56 279.72 -4 0 0 2262.48 74.62 -5 0 0 1011.52 25.73 -6 0 0 148.05 18.00 -7 0 0 15.26 23.35 -8 0 0 406.69 33.56 -8 0 0 406.87 42.94 -9 0 0 475.30 42.09 -9 0 0 475.43 49.13 -10 0 0 24.52 30.14 -10 0 0 15.88 8.92 -10 0 0 24.52 23.25 -11 0 0 10.52 9.92 -11 0 0 13.03 26.97 -11 0 0 13.11 35.20 -12 0 0 239.22 23.00 -12 0 0 239.13 39.86 -12 0 0 239.27 49.93 -13 0 0 109.29 29.65 -13 0 0 109.41 40.60 -14 0 0 6.47 30.79 -14 0 0 0.32 40.51 -15 0 0 43.98 37.43 -16 0 0 106.27 14.03 -16 0 0 106.20 38.03 -15 1 0 60.58 37.78 -14 1 0 0.66 43.13 -14 1 0 0.66 28.56 -13 1 0 26.02 41.50 -13 1 0 13.92 27.27 -12 1 0 41.97 29.45 -12 1 0 51.75 38.77 -11 1 0 320.02 19.34 -11 1 0 320.13 36.94 -11 1 0 320.00 43.23 -10 1 0 255.46 12.10 -10 1 0 255.40 35.55 -9 1 0 48.48 28.85 -9 1 0 43.55 7.64 -8 1 0 779.53 58.16 -8 1 0 779.18 30.29 -7 1 0 2213.33 79.03 -7 1 0 2213.32 50.87 -6 1 0 1285.69 37.28 -6 1 0 1285.66 59.74 -5 1 0 1907.66 81.75 -5 1 0 1907.73 55.03 -4 1 0 4448.21 180.22 -4 1 0 4447.57 126.92 -3 1 0 222.98 45.36 -3 1 0 223.13 28.85 -2 1 0 18.34 8.68 1 -1 0 2845.95 85.92 -1 1 0 2846.20 115.62 0 -1 0 1229.12 33.07 0 1 0 1229.06 62.32 -2 -1 0 184.25 16.41 -3 -1 0 154.24 31.83 -4 -1 0 1097.40 47.30 -5 -1 0 2024.41 76.30 -5 -1 0 2024.56 64.01 -6 -1 0 263.87 23.25 -6 -1 0 263.98 24.44 -7 -1 0 281.39 21.02 -7 -1 0 281.40 18.94 -8 -1 0 398.98 28.66 -9 -1 0 913.47 43.63 -9 -1 0 913.52 47.40 -10 -1 0 689.81 43.73 -10 -1 0 689.87 50.67 -11 -1 0 43.18 31.63 -11 -1 0 43.16 26.77 -12 -1 0 531.58 52.90 -12 -1 0 531.55 25.83 -12 -1 0 531.31 37.38 -13 -1 0 181.56 29.90 -13 -1 0 252.99 40.26 -14 -1 0 27.69 28.01 -15 -1 0 76.26 11.35 -15 -1 0 69.34 31.93 -16 -1 0 49.85 12.20 -16 -1 0 49.90 37.04 -15 2 0 113.30 57.56 -15 2 0 81.59 37.93 -14 2 0 0.49 33.61 -14 2 0 0.58 46.46 -13 2 0 5.43 41.05 -13 2 0 5.42 25.09 -12 2 0 87.86 30.39 -12 2 0 193.28 41.84 -11 2 0 219.20 63.71 -10 2 0 218.35 13.19 -10 2 0 319.01 38.42 -9 2 0 43.67 8.58 -9 2 0 43.68 30.99 -8 2 0 130.81 15.52 -8 2 0 130.81 37.23 -7 2 0 293.14 27.76 -7 2 0 293.15 53.89 -6 2 0 950.18 39.91 -6 2 0 950.10 66.24 -5 2 0 555.51 32.37 -5 2 0 555.48 15.62 -4 2 0 3425.14 104.91 -4 2 0 3425.76 151.21 3 -2 0 688.44 33.81 -3 2 0 688.40 45.31 2 -2 0 34.36 14.38 -2 2 0 34.37 20.97 1 -2 0 26.54 1.98 1 -2 0 26.56 4.61 -1 2 0 26.55 6.05 -1 2 0 26.62 13.83 0 2 0 1529.00 143.53 0 2 0 1529.15 103.12 -1 -2 0 73.58 2.28 -1 -2 0 73.58 5.01 1 2 0 67.30 8.13 1 2 0 73.58 4.31 -3 -2 0 1147.46 90.73 -4 -2 0 2117.64 69.26 -5 -2 0 3426.39 141.50 -6 -2 0 3250.11 105.11 -6 -2 0 3250.27 86.76 -7 -2 0 135.72 22.66 -7 -2 0 93.52 20.87 -8 -2 0 324.64 32.18 -8 -2 0 324.76 35.85 -9 -2 0 1111.31 72.24 -9 -2 0 1111.16 64.50 -10 -2 0 34.42 26.57 -10 -2 0 82.48 25.93 -11 -2 0 47.09 30.09 -11 -2 0 34.15 22.46 -12 -2 0 364.39 42.04 -12 -2 0 364.21 43.83 -13 -2 0 357.35 34.66 -14 -2 0 18.49 32.33 -14 -2 0 7.80 9.67 -15 -2 0 5.25 30.44 -15 -2 0 5.33 10.16 -16 -2 0 22.98 13.39 -15 3 0 54.89 36.19 -15 3 0 54.89 51.66 -14 3 0 17.85 48.04 -14 3 0 17.83 34.46 -13 3 0 14.09 42.64 -12 3 0 211.90 44.92 -11 3 0 150.27 56.17 -10 3 0 238.57 49.73 -10 3 0 238.41 17.06 -9 3 0 39.79 9.47 -9 3 0 39.86 35.50 -8 3 0 91.63 8.68 -8 3 0 91.64 31.58 -7 3 0 444.52 19.29 -7 3 0 444.48 43.93 -6 3 0 960.71 53.15 -6 3 0 960.74 25.83 -5 3 0 358.45 20.28 -5 3 0 358.54 43.08 4 -3 0 468.16 16.66 -4 3 0 468.33 44.92 -4 3 0 468.06 23.90 3 -3 0 1861.38 50.97 -3 3 0 1861.30 70.25 2 -3 0 1172.44 34.41 -2 3 0 1511.97 49.78 1 -3 0 596.64 21.22 1 -3 0 596.60 13.73 -1 3 0 596.64 38.62 -1 3 0 596.52 22.11 0 -3 0 2386.96 66.73 0 -3 0 2386.91 47.00 0 3 0 2386.41 91.77 0 3 0 2386.50 64.60 -1 -3 0 4.57 4.16 -1 -3 0 4.58 1.74 1 3 0 3.72 12.44 1 3 0 3.72 6.00 -2 -3 0 446.50 8.28 -2 -3 0 446.51 15.96 2 3 0 446.43 18.34 -3 -3 0 10.67 13.68 -4 -3 0 382.83 22.61 -5 -3 0 3269.77 79.57 -6 -3 0 131.22 25.88 -7 -3 0 103.69 14.68 -7 -3 0 102.61 15.22 -8 -3 0 555.41 39.86 -8 -3 0 555.41 38.32 -9 -3 0 853.76 56.22 -9 -3 0 853.73 53.79 -10 -3 0 18.13 26.33 -10 -3 0 7.63 20.67 -11 -3 0 9.21 23.10 -11 -3 0 11.09 28.06 -12 -3 0 49.08 10.31 -12 -3 0 49.11 28.26 -13 -3 0 137.60 32.72 -13 -3 0 137.61 12.74 -14 -3 0 140.12 13.83 -14 -3 0 140.09 35.20 -15 -3 0 1.68 9.02 -15 -3 0 1.68 33.07 -15 4 0 68.30 40.60 -15 4 0 61.35 53.59 -14 4 0 50.30 45.17 -13 4 0 8.35 46.31 -12 4 0 29.99 43.98 -11 4 0 716.28 70.45 -10 4 0 314.59 52.45 -9 4 0 7.80 35.35 -9 4 0 8.67 10.61 -8 4 0 17.90 11.85 -8 4 0 17.95 35.45 -7 4 0 457.50 17.45 -7 4 0 457.57 43.28 -6 4 0 842.67 58.45 -6 4 0 842.61 29.40 5 -4 0 143.90 6.05 -5 4 0 143.83 25.24 -5 4 0 143.86 12.69 4 -4 0 337.54 16.21 -4 4 0 337.42 26.08 3 -4 0 882.13 19.98 -3 4 0 882.14 33.52 2 -4 0 605.67 24.74 2 -4 0 605.67 15.77 -2 4 0 605.67 27.27 1 -4 0 24.35 3.82 1 -4 0 24.37 7.98 -1 4 0 94.63 28.41 -1 4 0 24.38 12.89 0 -4 0 56.06 2.58 0 -4 0 56.06 6.10 0 4 0 56.04 9.87 0 4 0 48.09 18.84 -1 -4 0 2042.29 26.67 -1 -4 0 2042.30 38.82 1 4 0 2042.00 56.72 1 4 0 2042.22 38.42 -2 -4 0 136.16 11.25 -2 -4 0 136.16 6.10 2 4 0 136.17 11.65 2 4 0 136.11 19.48 -3 -4 0 289.99 28.71 -4 -4 0 437.13 34.61 -5 -4 0 882.30 16.96 -5 -4 0 882.39 32.28 -6 -4 0 279.30 31.53 -6 -4 0 279.27 15.37 -7 -4 0 35.02 18.39 -7 -4 0 23.95 4.61 -8 -4 0 57.91 19.04 -8 -4 0 57.85 8.28 -8 -4 0 57.85 23.70 -9 -4 0 1055.34 43.63 -9 -4 0 1055.44 23.30 -9 -4 0 1055.38 45.36 -10 -4 0 357.31 15.27 -10 -4 0 357.21 33.12 -11 -4 0 48.94 7.68 -11 -4 0 48.94 24.05 -12 -4 0 129.56 31.04 -12 -4 0 34.69 10.56 -13 -4 0 121.28 12.99 -13 -4 0 121.25 34.56 -14 -4 0 118.47 32.77 -14 -4 0 118.53 12.44 -15 -4 0 29.39 9.72 -15 -4 0 29.39 31.09 -15 5 0 109.84 65.00 -14 5 0 74.03 53.54 -13 5 0 16.98 48.59 -12 5 0 72.57 46.21 -11 5 0 193.20 57.81 -10 5 0 507.49 60.93 -9 5 0 30.01 15.77 -9 5 0 22.42 40.36 -8 5 0 50.34 15.27 -8 5 0 50.38 38.47 -7 5 0 362.59 52.55 -7 5 0 362.51 24.84 -6 5 0 485.54 30.54 -6 5 0 485.60 56.82 5 -5 0 216.07 5.85 -5 5 0 216.02 14.77 -5 5 0 216.07 17.20 4 -5 0 56.17 3.97 -4 5 0 56.24 28.81 -4 5 0 56.20 14.77 3 -5 0 638.77 12.35 -3 5 0 638.93 45.17 -3 5 0 638.77 23.60 2 -5 0 536.98 24.19 2 -5 0 537.03 15.32 -2 5 0 537.05 27.42 1 -5 0 1173.57 25.73 1 -5 0 1173.61 38.23 -1 5 0 1173.48 39.22 -1 5 0 1173.46 65.00 0 -5 0 87.97 7.73 0 -5 0 87.99 3.72 0 5 0 87.95 11.50 0 5 0 88.02 24.44 -1 -5 0 1164.88 15.27 -1 -5 0 1164.98 24.14 1 5 0 1164.89 25.93 1 5 0 1164.72 40.11 2 5 0 246.78 23.20 2 5 0 246.55 35.85 -3 -5 0 693.67 16.26 -3 -5 0 693.64 26.03 3 5 0 693.58 32.92 -4 -5 0 160.51 5.11 -4 -5 0 160.50 14.28 -5 -5 0 809.77 42.24 -6 -5 0 594.85 18.54 -6 -5 0 594.84 36.04 -7 -5 0 26.67 18.74 -7 -5 0 38.29 6.94 -8 -5 0 26.41 7.54 -8 -5 0 26.38 16.31 -8 -5 0 15.96 19.93 -9 -5 0 325.98 17.15 -9 -5 0 325.94 33.91 -10 -5 0 245.25 13.73 -10 -5 0 245.26 33.56 -11 -5 0 168.79 11.45 -11 -5 0 166.75 25.78 -12 -5 0 15.28 7.49 -12 -5 0 21.41 29.75 -13 -5 0 119.18 11.70 -13 -5 0 145.04 35.25 -14 -5 0 236.70 13.98 -14 -5 0 236.65 36.59 -15 -5 0 10.18 32.52 -15 -5 0 10.35 9.77 -14 6 0 19.70 56.57 -13 6 0 24.55 56.87 -12 6 0 16.00 50.22 -11 6 0 307.18 55.03 -10 6 0 167.12 52.85 -9 6 0 66.96 44.72 -8 6 0 2.36 20.28 -8 6 0 6.56 39.12 -7 6 0 226.09 25.19 -7 6 0 267.13 22.01 6 -6 0 42.91 6.15 -6 6 0 42.87 15.72 -6 6 0 127.34 23.00 5 -6 0 890.61 17.35 -5 6 0 890.71 33.22 -4 6 0 106.89 17.75 -4 6 0 106.87 37.48 3 -6 0 834.91 19.58 -3 6 0 834.77 59.89 -3 6 0 834.80 33.27 2 -6 0 1795.60 69.61 2 -6 0 1795.75 48.24 -2 6 0 1795.63 108.13 -2 6 0 1795.82 69.76 1 -6 0 893.93 24.79 1 -6 0 893.99 16.21 -1 6 0 894.04 29.80 0 -6 0 328.02 3.97 0 -6 0 328.00 8.58 0 6 0 327.99 11.55 0 6 0 327.99 24.99 -1 -6 0 2515.46 52.80 1 6 0 1988.67 77.99 1 6 0 2515.59 53.05 -2 -6 0 2285.15 40.60 -2 -6 0 2285.11 58.95 2 6 0 2285.07 57.91 -3 -6 0 193.25 7.78 -3 -6 0 193.29 16.51 3 6 0 193.26 17.10 3 6 0 193.12 21.47 -4 -6 0 59.97 11.35 -4 -6 0 59.95 4.26 4 6 0 60.02 14.33 -5 -6 0 568.73 17.85 -5 -6 0 568.80 34.41 -6 -6 0 131.73 20.33 -6 -6 0 75.48 6.64 -7 -6 0 48.78 2.33 -7 -6 0 48.77 16.41 -8 -6 0 14.60 21.86 -8 -6 0 14.60 6.05 -9 -6 0 648.93 40.01 -9 -6 0 648.91 19.48 -10 -6 0 415.39 40.31 -10 -6 0 415.39 19.24 -11 -6 0 264.77 29.60 -11 -6 0 291.96 13.04 -12 -6 0 20.89 28.51 -12 -6 0 20.89 7.78 -13 -6 0 26.15 31.53 -13 -6 0 32.15 10.51 -14 -6 0 91.84 33.52 -14 -6 0 91.83 11.70 -15 -6 0 43.01 10.51 -14 7 0 40.61 61.87 -13 7 0 55.06 61.53 -12 7 0 2.19 53.20 -11 7 0 6.78 47.84 -10 7 0 169.31 51.91 -9 7 0 67.98 48.74 -8 7 0 68.15 42.89 7 -7 0 103.62 7.14 -7 7 0 113.75 21.47 -7 7 0 102.49 14.13 6 -7 0 414.76 19.78 -6 7 0 414.74 35.15 5 -7 0 76.48 1.88 -5 7 0 76.48 39.02 -5 7 0 81.36 18.54 -4 7 0 32.58 16.01 -4 7 0 32.59 38.08 3 -7 0 477.56 12.79 -3 7 0 477.51 54.29 -3 7 0 477.58 26.57 2 -7 0 858.02 40.31 -2 7 0 858.02 77.14 -2 7 0 858.12 43.18 -1 7 0 52.65 37.63 -1 7 0 116.03 21.02 0 -7 0 135.06 2.73 0 -7 0 130.88 6.54 0 7 0 130.88 9.82 0 7 0 131.30 12.35 -1 -7 0 693.73 11.11 -1 -7 0 693.77 20.87 1 7 0 606.92 34.21 1 7 0 693.72 23.05 -2 -7 0 775.46 12.89 -2 -7 0 775.51 23.45 2 7 0 775.24 35.94 2 7 0 775.47 25.14 -3 -7 0 787.56 16.61 -3 -7 0 787.48 27.22 3 7 0 787.62 30.19 -4 -7 0 7.39 10.16 -4 -7 0 17.58 4.51 4 7 0 7.29 14.92 -5 -7 0 9.36 15.47 -5 -7 0 9.35 6.59 -6 -7 0 486.50 16.41 -6 -7 0 486.60 32.42 -7 -7 0 248.36 27.02 -8 -7 0 14.39 21.02 -8 -7 0 9.67 5.90 -9 -7 0 15.11 24.19 -9 -7 0 23.22 8.63 -10 -7 0 425.15 41.75 -10 -7 0 425.20 20.72 -11 -7 0 127.12 11.60 -11 -7 0 127.08 30.84 -12 -7 0 11.20 8.28 -12 -7 0 11.20 28.31 -13 -7 0 28.88 28.90 -13 -7 0 29.82 10.26 -14 -7 0 210.52 14.18 -13 8 0 42.65 63.61 -12 8 0 2.36 58.80 -11 8 0 37.89 57.31 -10 8 0 191.72 60.09 -9 8 0 91.95 51.07 -8 8 0 64.75 49.18 7 -8 0 42.40 6.99 -7 8 0 42.41 19.73 -7 8 0 37.04 46.46 6 -8 0 334.71 11.90 -6 8 0 334.64 24.44 -6 8 0 334.55 57.51 5 -8 0 622.63 17.45 -5 8 0 622.50 68.17 -5 8 0 622.37 30.19 4 -8 0 21.94 4.02 -4 8 0 21.95 16.56 -4 8 0 22.05 48.98 3 -8 0 68.52 13.78 3 -8 0 68.52 6.79 -3 8 0 61.86 43.08 -3 8 0 68.50 18.94 2 -8 0 974.39 33.12 2 -8 0 974.46 21.22 -2 8 0 974.43 37.33 -2 8 0 974.21 68.02 1 -8 0 1249.61 31.28 1 -8 0 1249.61 46.85 -1 8 0 1249.62 49.48 -1 8 0 1249.26 80.22 0 -8 0 57.56 5.01 0 -8 0 57.59 10.81 0 8 0 57.10 32.23 0 8 0 57.61 16.81 -1 -8 0 189.68 6.54 -1 -8 0 189.71 13.78 1 8 0 133.42 14.28 1 8 0 133.46 17.30 -2 -8 0 941.76 28.76 -2 -8 0 941.72 17.60 2 8 0 941.91 34.56 -3 -8 0 63.51 13.14 -3 -8 0 63.46 5.65 3 8 0 54.64 21.02 3 8 0 63.45 14.72 -4 -8 0 13.48 10.76 -4 -8 0 10.66 4.16 4 8 0 13.55 19.63 4 8 0 13.52 14.48 -5 -8 0 91.11 8.87 -5 -8 0 81.69 16.66 -6 -8 0 215.46 8.87 -6 -8 0 215.40 16.51 -7 -8 0 328.33 16.06 -7 -8 0 328.34 32.62 -8 -8 0 442.84 30.24 -8 -8 0 442.92 14.72 -9 -8 0 61.64 28.01 -9 -8 0 57.71 7.54 -10 -8 0 450.80 35.89 -10 -8 0 450.68 14.38 -11 -8 0 267.53 30.34 -11 -8 0 326.16 15.27 -12 -8 0 28.20 26.82 -12 -8 0 35.95 11.16 -13 -8 0 27.80 10.56 -14 -8 0 89.19 11.90 -13 9 0 48.54 70.40 -12 9 0 61.38 68.07 -11 9 0 1.00 53.25 -10 9 0 64.42 55.08 -9 9 0 131.99 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68.63 23.75 -7 -7 -20 68.60 10.86 -8 -7 -20 124.94 26.08 -2 -8 -20 95.42 14.43 2 8 20 95.37 73.43 -3 -8 -20 0.49 11.30 3 8 20 13.30 74.52 -4 -8 -20 91.48 12.99 4 8 20 91.48 75.76 -5 -8 -20 143.23 12.25 5 8 20 136.66 71.34 -6 -8 -20 26.50 10.02 6 8 20 26.50 75.11 -7 -8 -20 0.49 20.08 -7 -8 -20 0.49 10.02 -3 -9 -20 3.21 11.55 -4 -9 -20 28.71 11.16 4 9 20 28.71 67.92 -5 -9 -20 97.15 12.59 5 9 20 151.13 83.24 -6 -9 -20 46.04 11.25 -5 -3 -21 1.68 35.20 -6 -3 -21 57.61 34.95 -6 -4 -21 5.59 29.20 -4 -5 -21 70.88 12.10 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 55551 _shelx_res_file ; TITL P-1 20150626d.res created by SHELXL-2018/3 at 12:59:54 on 23-Jun-2019 CELL 0.71073 12.947 13.889 16.289 77.482 73.859 85.101 ZERR 2 0.003 0.003 0.0011 0.003 0.003 0.002 LATT 1 SFAC C H La N O UNIT 102 139 2 12 30.5 EQIV $1 1-X,-Y,1-Z EQIV $2 2-X,-Y,-Z EQIV $3 -X,1-Y,1-Z L.S. 15 PLAN 2 SIZE 0.28 0.24 0.22 TEMP 18 HTAB C23 O14_$1 HTAB C41 O12_$2 HTAB C47 O14_$3 BOND $H htab conf fmap 2 acta OMIT -1 54 OMIT -1 0 3 REM REM REM WGHT 0.089000 FVAR 0.44685 C1 1 1.071490 0.475189 0.086643 11.00000 0.03546 0.03343 = 0.04332 0.00520 -0.01137 -0.00322 C2 1 1.134901 0.409642 0.035889 11.00000 0.04269 0.04203 = 0.04629 -0.01019 -0.01530 -0.01215 C3 1 1.236662 0.433070 -0.011730 11.00000 0.03325 0.04541 = 0.04045 -0.00654 0.00291 -0.00088 C4 1 1.283298 0.521887 -0.012074 11.00000 0.03721 0.04093 = 0.03596 0.00841 -0.00896 -0.00881 C5 1 1.219913 0.584057 0.041405 11.00000 0.04880 0.04325 = 0.02979 -0.00888 -0.00852 -0.01292 C6 1 1.118562 0.560919 0.092981 11.00000 0.03751 0.04061 = 0.03980 -0.00601 -0.00622 -0.01118 C7 1 1.083518 0.314327 0.036216 11.00000 0.04689 0.03686 = 0.04870 -0.00994 -0.01570 -0.00640 AFIX 137 H7A 2 1.033377 0.328992 0.001182 11.00000 -1.50000 H7B 2 1.046444 0.284933 0.094966 11.00000 -1.50000 H7C 2 1.138492 0.269244 0.012704 11.00000 -1.50000 AFIX 0 C8 1 1.394956 0.546127 -0.066764 11.00000 0.04015 0.04948 = 0.03904 -0.01135 -0.00903 -0.00817 AFIX 3 H8A 2 1.397916 0.557328 -0.127924 11.00000 -1.50000 H8B 2 1.416396 0.604538 -0.054204 11.00000 -1.50000 H8C 2 1.442336 0.492008 -0.053184 11.00000 -1.50000 AFIX 0 C9 1 1.058241 0.628457 0.155916 11.00000 0.05048 0.03884 = 0.04043 -0.00604 -0.00700 0.00351 AFIX 33 H9A 2 0.988732 0.602390 0.187244 11.00000 -1.50000 H9B 2 1.098764 0.631373 0.196485 11.00000 -1.50000 H9C 2 1.049749 0.693572 0.123121 11.00000 -1.50000 AFIX 0 C10 1 0.953845 0.456174 0.135163 11.00000 0.04294 0.04319 = 0.04308 0.00633 -0.01385 -0.00953 AFIX 23 H10A 2 0.917753 0.516415 0.150618 11.00000 -1.20000 H10B 2 0.917486 0.433202 0.098643 11.00000 -1.20000 AFIX 0 C11 1 0.859320 0.331113 0.250054 11.00000 0.04279 0.03662 = 0.04048 0.01011 -0.01126 -0.01240 C12 1 0.862349 0.253544 0.320080 11.00000 0.03880 0.04139 = 0.04249 -0.00591 -0.00943 -0.00086 AFIX 43 H12 2 0.924563 0.240106 0.338930 11.00000 -1.20000 AFIX 0 C13 1 0.772480 0.196450 0.361589 11.00000 0.05373 0.03454 = 0.04240 0.01410 -0.01366 0.00308 AFIX 43 H13 2 0.774761 0.144618 0.408071 11.00000 -1.20000 AFIX 0 C14 1 0.679661 0.216326 0.334120 11.00000 0.03723 0.04013 = 0.04283 0.00197 -0.00895 -0.00612 C15 1 0.677357 0.295561 0.264045 11.00000 0.04459 0.03841 = 0.03925 -0.00565 -0.01025 -0.01579 AFIX 43 H15 2 0.614918 0.310336 0.245662 11.00000 -1.20000 AFIX 0 C16 1 0.767460 0.351437 0.222491 11.00000 0.04246 0.04816 = 0.04449 0.01277 -0.01361 -0.00269 AFIX 43 H16 2 0.765800 0.403007 0.175667 11.00000 -1.20000 AFIX 0 C17 1 0.584232 0.154056 0.375903 11.00000 0.02869 0.03913 = 0.03472 -0.00673 0.00470 -0.00375 C18 1 0.698161 -0.362130 0.067256 11.00000 0.04802 0.04533 = 0.03776 -0.01435 -0.01470 0.00730 AFIX 23 H18A 2 0.706952 -0.294479 0.035211 11.00000 -1.20000 H18B 2 0.622351 -0.377038 0.084915 11.00000 -1.20000 AFIX 0 C19 1 0.702853 -0.309249 0.197858 11.00000 0.04400 0.04298 = 0.03698 -0.00980 -0.00315 0.00495 C20 1 0.625469 -0.240800 0.184925 11.00000 0.04195 0.03837 = 0.04460 -0.01253 -0.01371 0.01439 AFIX 43 H20 2 0.594043 -0.237494 0.139490 11.00000 -1.20000 AFIX 0 C21 1 0.593125 -0.173372 0.243205 11.00000 0.04039 0.04622 = 0.03467 -0.01511 -0.00648 -0.00522 AFIX 43 H21 2 0.541965 -0.123621 0.235035 11.00000 -1.20000 AFIX 0 C22 1 0.639343 -0.183437 0.312104 11.00000 0.03283 0.04030 = 0.03331 -0.00134 -0.00564 -0.01034 C23 1 0.718170 -0.257053 0.322389 11.00000 0.04096 0.03475 = 0.03508 0.00198 -0.00865 -0.00646 AFIX 43 H23 2 0.748673 -0.263156 0.368717 11.00000 -1.20000 AFIX 0 C24 1 0.752751 -0.322921 0.263387 11.00000 0.03560 0.04432 = 0.03558 -0.00365 0.00220 -0.00494 AFIX 43 H24 2 0.805556 -0.371755 0.269098 11.00000 -1.20000 AFIX 0 C25 1 0.600914 -0.118800 0.377029 11.00000 0.03758 0.02700 = 0.03966 -0.00819 -0.00712 -0.00611 C26 1 0.267095 -0.321684 0.050675 11.00000 0.04735 0.04466 = 0.04461 -0.01412 -0.01111 -0.01422 AFIX 23 H26A 2 0.321265 -0.295242 -0.002269 11.00000 -1.20000 H26B 2 0.210957 -0.271659 0.062253 11.00000 -1.20000 AFIX 0 C27 1 0.318157 -0.282919 0.170061 11.00000 0.04283 0.04383 = 0.04681 -0.01738 -0.01088 -0.01376 C28 1 0.332211 -0.318528 0.251485 11.00000 0.05361 0.04556 = 0.05208 -0.01687 -0.02076 -0.00984 AFIX 43 H28 2 0.342725 -0.385866 0.270417 11.00000 -1.20000 AFIX 0 C29 1 0.330649 -0.251967 0.307001 11.00000 0.04287 0.04582 = 0.04705 -0.01283 -0.01350 -0.01375 AFIX 43 H29 2 0.341147 -0.275873 0.362090 11.00000 -1.20000 AFIX 0 C30 1 0.313623 -0.151945 0.279614 11.00000 0.04086 0.04696 = 0.04786 -0.01179 -0.01272 -0.01570 C31 1 0.301965 -0.117902 0.198623 11.00000 0.05023 0.04133 = 0.04494 -0.00955 -0.01255 -0.01214 AFIX 43 H31 2 0.294210 -0.050238 0.179449 11.00000 -1.20000 AFIX 0 C32 1 0.301112 -0.180992 0.142166 11.00000 0.04247 0.04232 = 0.03561 -0.00755 -0.00849 -0.01255 AFIX 43 H32 2 0.289552 -0.156038 0.087572 11.00000 -1.20000 AFIX 0 C33 1 0.314048 -0.084757 0.337150 11.00000 0.03485 0.04986 = 0.04519 -0.01572 -0.01067 -0.01548 C34 1 0.301595 0.269162 0.335589 11.00000 0.04538 0.04287 = 0.03758 -0.00573 0.00451 -0.00958 AFIX 43 H34 2 0.349794 0.307305 0.346782 11.00000 -1.20000 AFIX 0 C35 1 0.308857 0.396083 0.200495 11.00000 0.04730 0.05164 = 0.05048 0.00740 -0.01463 -0.01307 AFIX 137 H35A 2 0.355134 0.426569 0.223790 11.00000 -1.50000 H35B 2 0.249000 0.439880 0.193582 11.00000 -1.50000 H35C 2 0.348311 0.382206 0.144832 11.00000 -1.50000 AFIX 0 C36 1 0.192240 0.247951 0.235982 11.00000 0.04980 0.05006 = 0.05283 0.01952 -0.01214 -0.01287 AFIX 137 H36A 2 0.229746 0.194063 0.211005 11.00000 -1.50000 H36B 2 0.161815 0.291673 0.193948 11.00000 -1.50000 H36C 2 0.135817 0.222856 0.286748 11.00000 -1.50000 AFIX 0 C37 1 0.125862 0.093610 0.564658 11.00000 0.03978 0.04131 = 0.04972 -0.00982 -0.01571 -0.00869 AFIX 43 H37 2 0.157946 0.153881 0.555189 11.00000 -1.20000 AFIX 0 C38 1 -0.034446 0.161925 0.663840 11.00000 0.04457 0.04623 = 0.06464 -0.01121 0.00537 -0.00852 AFIX 137 H38A 2 0.017366 0.195912 0.678486 11.00000 -1.50000 H38B 2 -0.085966 0.132299 0.716280 11.00000 -1.50000 H38C 2 -0.070726 0.207944 0.627357 11.00000 -1.50000 AFIX 0 C39 1 -0.038101 -0.008721 0.626174 11.00000 0.04485 0.04824 = 0.04473 0.01479 0.01362 -0.01253 AFIX 137 H39A 2 -0.090058 0.005751 0.592787 11.00000 -1.50000 H39B 2 -0.074274 -0.030976 0.686653 11.00000 -1.50000 H39C 2 0.011386 -0.059391 0.605831 11.00000 -1.50000 AFIX 0 C40 1 0.862551 0.124039 0.078202 11.00000 0.06381 0.06017 = 0.05144 -0.01404 -0.01285 -0.02039 AFIX 43 H40 2 0.840441 0.178366 0.104204 11.00000 -1.20000 AFIX 0 C41 1 0.858656 -0.063266 0.098954 11.00000 0.05818 0.05380 = 0.04602 -0.01558 0.00067 -0.01614 AFIX 137 H41A 2 0.928190 -0.094759 0.095917 11.00000 -1.50000 H41B 2 0.845981 -0.049727 0.042169 11.00000 -1.50000 H41C 2 0.804359 -0.106022 0.139080 11.00000 -1.50000 AFIX 0 C42 1 0.830476 0.026920 0.224413 11.00000 0.05602 0.05932 = 0.06311 -0.02013 -0.01348 -0.01580 AFIX 137 H42A 2 0.754608 0.019431 0.250299 11.00000 -1.50000 H42B 2 0.852263 0.086973 0.234061 11.00000 -1.50000 H42C 2 0.868861 -0.028040 0.250450 11.00000 -1.50000 AFIX 0 C43 1 0.471760 0.185982 0.025148 11.00000 0.05569 0.05013 = 0.06168 -0.00885 -0.01652 -0.00028 AFIX 43 H43 2 0.423260 0.168739 -0.001618 11.00000 -1.20000 AFIX 0 C44 1 0.573399 0.013732 0.074082 11.00000 0.05899 0.05868 = 0.06447 -0.01216 -0.00847 0.01301 AFIX 137 H44A 2 0.609622 -0.004536 0.119453 11.00000 -1.50000 H44B 2 0.624080 0.012819 0.018587 11.00000 -1.50000 H44C 2 0.517832 -0.032223 0.083752 11.00000 -1.50000 AFIX 0 C45 1 0.531510 0.160102 0.149562 11.00000 0.04916 0.06282 = 0.04821 -0.01448 0.00776 -0.01804 AFIX 137 H45A 2 0.493808 0.222819 0.146471 11.00000 -1.50000 H45B 2 0.605532 0.169154 0.145665 11.00000 -1.50000 H45C 2 0.499384 0.117213 0.203961 11.00000 -1.50000 AFIX 0 C46 1 0.136740 0.405138 0.504415 11.00000 0.05487 0.05254 = 0.05543 -0.00875 -0.02698 0.01394 AFIX 43 H46 2 0.201151 0.438383 0.485630 11.00000 -1.20000 AFIX 0 C47 1 0.080835 0.486777 0.361241 11.00000 0.06199 0.06992 = 0.04230 -0.01108 -0.01476 0.00800 AFIX 137 H47A 2 0.136321 0.533666 0.348479 11.00000 -1.50000 H47B 2 0.012407 0.520933 0.366149 11.00000 -1.50000 H47C 2 0.094570 0.450687 0.315098 11.00000 -1.50000 AFIX 0 C48 1 -0.008134 0.343374 0.466754 11.00000 0.05994 0.06286 = 0.06784 -0.02480 -0.02068 -0.01088 AFIX 137 H48A 2 -0.044132 0.355106 0.421188 11.00000 -1.50000 H48B 2 -0.058968 0.350202 0.520845 11.00000 -1.50000 H48C 2 0.023022 0.277825 0.472327 11.00000 -1.50000 AFIX 0 C49 1 0.518277 0.473660 0.361096 11.00000 0.05841 0.04185 = 0.04986 -0.00971 -0.01499 -0.01379 AFIX 43 H49 2 0.561414 0.522246 0.320952 11.00000 -1.20000 AFIX 0 C50 1 0.495312 0.337556 0.492766 11.00000 0.05097 0.04145 = 0.03768 -0.00794 -0.01148 -0.01272 AFIX 137 H50A 2 0.446913 0.363231 0.539867 11.00000 -1.50000 H50B 2 0.544376 0.290259 0.515145 11.00000 -1.50000 H50C 2 0.454977 0.306182 0.465051 11.00000 -1.50000 AFIX 0 C51 1 0.662899 0.440446 0.433376 11.00000 0.05805 0.04497 = 0.04208 -0.00876 -0.00612 -0.01351 AFIX 137 H51A 2 0.692281 0.493431 0.385917 11.00000 -1.50000 H51B 2 0.709287 0.382976 0.429115 11.00000 -1.50000 H51C 2 0.657144 0.459549 0.487730 11.00000 -1.50000 AFIX 0 LA1 3 0.375778 0.038713 0.440135 11.00000 0.02964 0.03034 = 0.02944 -0.00858 -0.00916 -0.00946 N1 4 0.268866 0.302714 0.261214 11.00000 0.04348 0.04273 = 0.05594 0.01051 -0.01088 -0.01037 N2 4 0.022248 0.082560 0.615633 11.00000 0.04131 0.04735 = 0.04615 -0.01277 0.01412 -0.00992 N3 4 0.854693 0.030616 0.129414 11.00000 0.07124 0.05587 = 0.05422 0.01025 -0.01923 -0.01940 N4 4 0.524892 0.114553 0.074784 11.00000 0.05914 0.04895 = 0.06144 -0.00825 -0.01594 -0.02009 N5 4 0.079610 0.417428 0.444537 11.00000 0.06472 0.05082 = 0.06347 -0.01518 -0.02085 0.00802 N6 4 0.555554 0.418033 0.429340 11.00000 0.05376 0.04683 = 0.04285 -0.01389 0.00647 -0.00877 O1 5 0.951632 0.382089 0.212764 11.00000 0.03724 0.04369 = 0.03822 0.01036 -0.00442 -0.01309 O2 5 0.504729 0.169225 0.344003 11.00000 0.04388 0.03831 = 0.03806 0.01035 -0.01221 -0.01030 O3 5 0.579846 0.090717 0.445595 11.00000 0.03216 0.03149 = 0.03096 -0.00820 -0.01011 -0.01149 O4 5 0.740494 -0.376917 0.141894 11.00000 0.04732 0.04191 = 0.04235 -0.01177 -0.00996 0.00550 O5 5 0.528885 -0.053869 0.363755 11.00000 0.03689 0.04812 = 0.03635 -0.01438 -0.00578 -0.00671 O6 5 0.642331 -0.126179 0.440317 11.00000 0.02799 0.03119 = 0.02906 -0.00958 -0.00833 -0.00827 O7 5 0.313797 -0.351222 0.122465 11.00000 0.05423 0.03968 = 0.04971 -0.01370 -0.01964 -0.01090 O8 5 0.303619 -0.117906 0.416743 11.00000 0.04189 0.03879 = 0.04453 -0.01082 -0.00652 -0.01566 O9 5 0.323680 0.006997 0.307711 11.00000 0.04666 0.04314 = 0.03979 -0.01126 -0.01563 -0.01219 O10 5 0.272233 0.192194 0.389121 11.00000 0.03883 0.03750 = 0.04137 -0.00823 -0.00881 -0.00845 O11 5 0.179041 0.027064 0.530474 11.00000 0.03235 0.04105 = 0.03929 -0.00429 -0.00750 -0.00976 O12 5 0.899280 0.136800 -0.003348 11.00000 0.06469 0.06695 = 0.06928 -0.02067 -0.01871 -0.01932 O13 5 0.492629 0.274706 0.018380 11.00000 0.07571 0.05357 = 0.06849 -0.01758 -0.02251 0.00713 O14 5 0.116827 0.356377 0.580729 11.00000 0.06080 0.05647 = 0.06512 0.00989 -0.01614 -0.01385 O15 5 0.426408 0.459683 0.352217 11.00000 0.05963 0.04703 = 0.05801 -0.00832 -0.01992 0.00995 O1W 5 0.147076 0.075868 0.122107 10.25000 0.06176 0.04712 = 0.11356 -0.04366 -0.01368 0.00642 AFIX 3 H1WA 2 0.128456 0.032768 0.168917 10.25000 -1.50000 H1WB 2 0.098136 0.120638 0.121067 10.25000 -1.50000 AFIX 0 HKLF 4 REM P-1 REM wR2 = 0.1470, GooF = S = 1.014, Restrained GooF = 1.014 for all data REM R1 = 0.0599 for 8526 Fo > 4sig(Fo) and 0.0698 for all 11881 data REM 680 parameters refined using 0 restraints END WGHT 0.0890 0.0000 REM Instructions for potential hydrogen bonds EQIV $6 x, y+1, z HTAB C10 O4_$6 EQIV $7 -x+1, -y, -z HTAB C18 O13_$7 HTAB C26 O13_$7 HTAB C26 O12_$7 EQIV $8 x, y-1, z HTAB C28 O15_$8 HTAB C34 O15 HTAB C35 O15 HTAB C37 O6_$1 HTAB C38 O14 HTAB C41 O12_$2 HTAB C45 O2 HTAB C47 O14_$3 REM Highest difference peak 0.847, deepest hole -0.685, 1-sigma level 0.137 Q1 1 0.3661 0.3663 0.4582 11.00000 0.05 0.60 Q2 1 0.2345 -0.0253 0.4150 11.00000 0.05 0.57 ; _shelx_res_checksum 59311 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 C C1 1.0715(4) 0.4752(3) 0.0866(3) 0.0391(11) Uani d 1 C C2 1.1349(4) 0.4096(3) 0.0359(3) 0.0421(12) Uani d 1 C C3 1.2367(4) 0.4331(4) -0.0117(3) 0.0427(12) Uani d 1 C C4 1.2833(4) 0.5219(3) -0.0121(3) 0.0403(12) Uani d 1 C C5 1.2199(4) 0.5841(3) 0.0414(3) 0.0401(12) Uani d 1 C C6 1.1186(4) 0.5609(3) 0.0930(3) 0.0399(11) Uani d 1 C C7 1.0835(4) 0.3143(3) 0.0362(3) 0.0430(12) Uani d 1 H H7A 1.033377 0.328992 0.001182 0.065 Uiso calc 1 H H7B 1.046444 0.284933 0.094966 0.065 Uiso calc 1 H H7C 1.138492 0.269244 0.012704 0.065 Uiso calc 1 C C8 1.3950(4) 0.5461(4) -0.0668(3) 0.0424(12) Uani d 1 H H8A 1.397916 0.557328 -0.127924 0.064 Uiso d 1 H H8B 1.416396 0.604538 -0.054204 0.064 Uiso d 1 H H8C 1.442336 0.492008 -0.053184 0.064 Uiso d 1 C C9 1.0582(5) 0.6285(3) 0.1559(3) 0.0449(12) Uani d 1 H H9A 0.988732 0.602390 0.187244 0.067 Uiso calc 1 H H9B 1.098764 0.631373 0.196485 0.067 Uiso calc 1 H H9C 1.049749 0.693572 0.123121 0.067 Uiso calc 1 C C10 0.9538(4) 0.4562(4) 0.1352(3) 0.0444(12) Uani d 1 H H10A 0.917753 0.516415 0.150618 0.053 Uiso calc 1 H H10B 0.917486 0.433202 0.098643 0.053 Uiso calc 1 C C11 0.8593(4) 0.3311(3) 0.2501(3) 0.0421(12) Uani d 1 C C12 0.8623(4) 0.2535(3) 0.3201(3) 0.0416(12) Uani d 1 H H12 0.924563 0.240106 0.338930 0.050 Uiso calc 1 C C13 0.7725(5) 0.1965(3) 0.3616(4) 0.0471(13) Uani d 1 H H13 0.774761 0.144618 0.408071 0.057 Uiso calc 1 C C14 0.6797(4) 0.2163(3) 0.3341(3) 0.0417(12) Uani d 1 C C15 0.6774(4) 0.2956(3) 0.2640(3) 0.0404(12) Uani d 1 H H15 0.614918 0.310336 0.245662 0.048 Uiso calc 1 C C16 0.7675(5) 0.3514(4) 0.2225(4) 0.0480(13) Uani d 1 H H16 0.765800 0.403007 0.175667 0.058 Uiso calc 1 C C17 0.5842(4) 0.1541(3) 0.3759(3) 0.0368(11) Uani d 1 C C18 0.6982(5) -0.3621(4) 0.0673(3) 0.0426(12) Uani d 1 H H18A 0.706952 -0.294479 0.035211 0.051 Uiso calc 1 H H18B 0.622351 -0.377038 0.084915 0.051 Uiso calc 1 C C19 0.7029(4) -0.3092(4) 0.1979(3) 0.0430(12) Uani d 1 C C20 0.6255(4) -0.2408(3) 0.1849(3) 0.0415(12) Uani d 1 H H20 0.594043 -0.237494 0.139490 0.050 Uiso calc 1 C C21 0.5931(4) -0.1734(3) 0.2432(3) 0.0398(11) Uani d 1 H H21 0.541965 -0.123621 0.235035 0.048 Uiso calc 1 C C22 0.6393(4) -0.1834(3) 0.3121(3) 0.0365(11) Uani d 1 C C23 0.7182(4) -0.2571(3) 0.3224(3) 0.0383(11) Uani d 1 H H23 0.748673 -0.263156 0.368717 0.046 Uiso calc 1 C C24 0.7528(4) -0.3229(4) 0.2634(3) 0.0414(11) Uani d 1 H H24 0.805556 -0.371755 0.269098 0.050 Uiso calc 1 C C25 0.6009(4) -0.1188(3) 0.3770(3) 0.0348(11) Uani d 1 C C26 0.2671(4) -0.3217(3) 0.0507(3) 0.0442(12) Uani d 1 H H26A 0.321265 -0.295242 -0.002269 0.053 Uiso calc 1 H H26B 0.210957 -0.271659 0.062253 0.053 Uiso calc 1 C C27 0.3182(4) -0.2829(3) 0.1701(3) 0.0426(12) Uani d 1 C C28 0.3322(4) -0.3185(4) 0.2515(3) 0.0474(13) Uani d 1 H H28 0.342725 -0.385866 0.270417 0.057 Uiso calc 1 C C29 0.3306(4) -0.2520(3) 0.3070(3) 0.0436(12) Uani d 1 H H29 0.341147 -0.275873 0.362090 0.052 Uiso calc 1 C C30 0.3136(4) -0.1519(3) 0.2796(3) 0.0438(12) Uani d 1 C C31 0.3020(4) -0.1179(4) 0.1986(3) 0.0447(13) Uani d 1 H H31 0.294210 -0.050238 0.179449 0.054 Uiso calc 1 C C32 0.3011(4) -0.1810(3) 0.1422(3) 0.0399(12) Uani d 1 H H32 0.289552 -0.156038 0.087572 0.048 Uiso calc 1 C C33 0.3140(4) -0.0848(4) 0.3371(3) 0.0415(12) Uani d 1 C C34 0.3016(5) 0.2692(3) 0.3356(3) 0.0450(12) Uani d 1 H H34 0.349794 0.307305 0.346782 0.054 Uiso calc 1 C C35 0.3089(5) 0.3961(4) 0.2005(4) 0.0516(14) Uani d 1 H H35A 0.355134 0.426569 0.223790 0.077 Uiso calc 1 H H35B 0.249000 0.439880 0.193582 0.077 Uiso calc 1 H H35C 0.348311 0.382206 0.144832 0.077 Uiso calc 1 C C36 0.1922(5) 0.2480(4) 0.2360(4) 0.0552(15) Uani d 1 H H36A 0.229746 0.194063 0.211005 0.083 Uiso calc 1 H H36B 0.161815 0.291673 0.193948 0.083 Uiso calc 1 H H36C 0.135817 0.222856 0.286748 0.083 Uiso calc 1 C C37 0.1259(4) 0.0936(3) 0.5647(3) 0.0423(12) Uani d 1 H H37 0.157946 0.153881 0.555189 0.051 Uiso calc 1 C C38 -0.0344(5) 0.1619(4) 0.6638(4) 0.0555(15) Uani d 1 H H38A 0.017366 0.195912 0.678486 0.083 Uiso calc 1 H H38B -0.085966 0.132299 0.716280 0.083 Uiso calc 1 H H38C -0.070726 0.207944 0.627357 0.083 Uiso calc 1 C C39 -0.0381(5) -0.0087(4) 0.6262(4) 0.0543(15) Uani d 1 H H39A -0.090058 0.005751 0.592787 0.081 Uiso calc 1 H H39B -0.074274 -0.030976 0.686653 0.081 Uiso calc 1 H H39C 0.011386 -0.059391 0.605831 0.081 Uiso calc 1 C C40 0.8626(5) 0.1240(4) 0.0782(4) 0.0574(16) Uani d 1 H H40 0.840441 0.178366 0.104204 0.069 Uiso calc 1 C C41 0.8587(5) -0.0633(4) 0.0990(4) 0.0539(15) Uani d 1 H H41A 0.928190 -0.094759 0.095917 0.081 Uiso calc 1 H H41B 0.845981 -0.049727 0.042169 0.081 Uiso calc 1 H H41C 0.804359 -0.106022 0.139080 0.081 Uiso calc 1 C C42 0.8305(5) 0.0269(4) 0.2244(4) 0.0579(16) Uani d 1 H H42A 0.754608 0.019431 0.250299 0.087 Uiso calc 1 H H42B 0.852263 0.086973 0.234061 0.087 Uiso calc 1 H H42C 0.868861 -0.028040 0.250450 0.087 Uiso calc 1 C C43 0.4718(5) 0.1860(4) 0.0251(4) 0.0561(15) Uani d 1 H H43 0.423260 0.168739 -0.001618 0.067 Uiso calc 1 C C44 0.5734(6) 0.0137(4) 0.0741(4) 0.0633(16) Uani d 1 H H44A 0.609622 -0.004536 0.119453 0.095 Uiso calc 1 H H44B 0.624080 0.012819 0.018587 0.095 Uiso calc 1 H H44C 0.517832 -0.032223 0.083752 0.095 Uiso calc 1 C C45 0.5315(5) 0.1601(4) 0.1496(4) 0.0561(15) Uani d 1 H H45A 0.493808 0.222819 0.146471 0.084 Uiso calc 1 H H45B 0.605532 0.169154 0.145665 0.084 Uiso calc 1 H H45C 0.499384 0.117213 0.203961 0.084 Uiso calc 1 C C46 0.1367(5) 0.4051(4) 0.5044(4) 0.0530(14) Uani d 1 H H46 0.201151 0.438383 0.485630 0.064 Uiso calc 1 C C47 0.0808(6) 0.4868(4) 0.3612(4) 0.0585(15) Uani d 1 H H47A 0.136321 0.533666 0.348479 0.088 Uiso calc 1 H H47B 0.012407 0.520933 0.366149 0.088 Uiso calc 1 H H47C 0.094570 0.450687 0.315098 0.088 Uiso calc 1 C C48 -0.0081(5) 0.3434(4) 0.4668(4) 0.0604(16) Uani d 1 H H48A -0.044132 0.355106 0.421188 0.091 Uiso calc 1 H H48B -0.058968 0.350202 0.520845 0.091 Uiso calc 1 H H48C 0.023022 0.277825 0.472327 0.091 Uiso calc 1 C C49 0.5183(5) 0.4737(4) 0.3611(4) 0.0491(14) Uani d 1 H H49 0.561414 0.522246 0.320952 0.059 Uiso calc 1 C C50 0.4953(4) 0.3376(3) 0.4928(3) 0.0427(12) Uani d 1 H H50A 0.446913 0.363231 0.539867 0.064 Uiso calc 1 H H50B 0.544376 0.290259 0.515145 0.064 Uiso calc 1 H H50C 0.454977 0.306182 0.465051 0.064 Uiso calc 1 C C51 0.6629(5) 0.4404(4) 0.4334(3) 0.0491(13) Uani d 1 H H51A 0.692281 0.493431 0.385917 0.074 Uiso calc 1 H H51B 0.709287 0.382976 0.429115 0.074 Uiso calc 1 H H51C 0.657144 0.459549 0.487730 0.074 Uiso calc 1 La La1 0.37578(2) 0.03871(2) 0.44013(2) 0.02861(10) Uani d 1 N N1 0.2689(4) 0.3027(3) 0.2612(3) 0.0505(12) Uani d 1 N N2 0.0222(4) 0.0826(3) 0.6156(3) 0.0492(11) Uani d 1 N N3 0.8547(5) 0.0306(3) 0.1294(3) 0.0622(14) Uani d 1 N N4 0.5249(4) 0.1146(3) 0.0748(3) 0.0559(13) Uani d 1 N N5 0.0796(4) 0.4174(3) 0.4445(3) 0.0589(13) Uani d 1 N N6 0.5556(4) 0.4180(3) 0.4293(3) 0.0506(12) Uani d 1 O O1 0.9516(3) 0.3821(2) 0.2128(2) 0.0431(8) Uani d 1 O O2 0.5047(3) 0.1692(2) 0.3440(2) 0.0421(8) Uani d 1 O O3 0.5798(2) 0.0907(2) 0.44560(19) 0.0302(7) Uani d 1 O O4 0.7405(3) -0.3769(2) 0.1419(2) 0.0442(8) Uani d 1 O O5 0.5289(3) -0.0539(2) 0.3638(2) 0.0400(8) Uani d 1 O O6 0.6423(2) -0.12618(19) 0.44032(18) 0.0283(7) Uani d 1 O O7 0.3138(3) -0.3512(2) 0.1225(2) 0.0454(9) Uani d 1 O O8 0.3036(3) -0.1179(2) 0.4167(2) 0.0415(8) Uani d 1 O O9 0.3237(3) 0.0070(2) 0.3077(2) 0.0412(8) Uani d 1 O O10 0.2722(3) 0.1922(2) 0.3891(2) 0.0391(8) Uani d 1 O O11 0.1790(3) 0.0271(2) 0.5305(2) 0.0381(8) Uani d 1 O O12 0.8993(4) 0.1368(3) -0.0033(3) 0.0646(12) Uani d 1 O O13 0.4926(4) 0.2747(3) 0.0184(3) 0.0650(12) Uani d 1 O O14 0.1168(4) 0.3564(3) 0.5807(3) 0.0637(11) Uani d 1 O O15 0.4264(3) 0.4597(3) 0.3522(3) 0.0551(10) Uani d 1 O O1W 0.1471(15) 0.0759(11) 0.1221(13) 0.072(5) Uani d 0.25 H H1WA 0.128456 0.032768 0.168917 0.108 Uiso d 0.25 H H1WB 0.098136 0.120638 0.121067 0.108 Uiso d 0.25 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 C1 0.035(3) 0.033(2) 0.043(3) -0.003(2) -0.011(2) 0.005(2) C2 0.043(3) 0.042(2) 0.046(3) -0.012(2) -0.015(3) -0.010(2) C3 0.033(3) 0.045(3) 0.040(3) -0.001(2) 0.003(2) -0.007(2) C4 0.037(3) 0.041(2) 0.036(3) -0.009(2) -0.009(2) 0.008(2) C5 0.049(3) 0.043(2) 0.030(3) -0.013(2) -0.009(2) -0.009(2) C6 0.038(3) 0.041(2) 0.040(3) -0.011(2) -0.006(2) -0.006(2) C7 0.047(3) 0.037(2) 0.049(3) -0.006(2) -0.016(3) -0.010(2) C8 0.040(3) 0.049(3) 0.039(3) -0.008(2) -0.009(3) -0.011(2) C9 0.050(3) 0.039(2) 0.040(3) 0.004(2) -0.007(3) -0.006(2) C10 0.043(3) 0.043(2) 0.043(3) -0.010(2) -0.014(3) 0.006(2) C11 0.043(3) 0.037(2) 0.040(3) -0.012(2) -0.011(3) 0.010(2) C12 0.039(3) 0.041(2) 0.042(3) -0.001(2) -0.009(2) -0.006(2) C13 0.054(4) 0.035(2) 0.042(3) 0.003(2) -0.014(3) 0.014(2) C14 0.037(3) 0.040(2) 0.043(3) -0.006(2) -0.009(3) 0.002(2) C15 0.045(3) 0.038(2) 0.039(3) -0.016(2) -0.010(2) -0.006(2) C16 0.042(3) 0.048(3) 0.044(3) -0.003(2) -0.014(3) 0.013(2) C17 0.029(3) 0.039(2) 0.035(3) -0.004(2) 0.005(2) -0.007(2) C18 0.048(3) 0.045(2) 0.038(3) 0.007(2) -0.015(3) -0.014(2) C19 0.044(3) 0.043(2) 0.037(3) 0.005(2) -0.003(3) -0.010(2) C20 0.042(3) 0.038(2) 0.045(3) 0.014(2) -0.014(3) -0.013(2) C21 0.040(3) 0.046(2) 0.035(3) -0.005(2) -0.006(2) -0.015(2) C22 0.033(3) 0.040(2) 0.033(3) -0.010(2) -0.006(2) -0.0013(19) C23 0.041(3) 0.035(2) 0.035(3) -0.006(2) -0.009(2) 0.0020(19) C24 0.036(3) 0.044(2) 0.036(3) -0.005(2) 0.002(2) -0.004(2) C25 0.038(3) 0.027(2) 0.040(3) -0.006(2) -0.007(2) -0.0082(18) C26 0.047(3) 0.045(2) 0.045(3) -0.014(2) -0.011(3) -0.014(2) C27 0.043(3) 0.044(2) 0.047(3) -0.014(2) -0.011(3) -0.017(2) C28 0.054(3) 0.046(3) 0.052(3) -0.010(2) -0.021(3) -0.017(2) C29 0.043(3) 0.046(2) 0.047(3) -0.014(2) -0.013(3) -0.013(2) C30 0.041(3) 0.047(3) 0.048(3) -0.016(2) -0.013(3) -0.012(2) C31 0.050(3) 0.041(2) 0.045(3) -0.012(2) -0.013(3) -0.010(2) C32 0.042(3) 0.042(2) 0.036(3) -0.013(2) -0.008(2) -0.008(2) C33 0.035(3) 0.050(3) 0.045(3) -0.015(2) -0.011(2) -0.016(2) C34 0.045(3) 0.043(2) 0.038(3) -0.010(2) 0.005(3) -0.006(2) C35 0.047(3) 0.052(3) 0.050(3) -0.013(3) -0.015(3) 0.007(2) C36 0.050(4) 0.050(3) 0.053(4) -0.013(3) -0.012(3) 0.020(3) C37 0.040(3) 0.041(2) 0.050(3) -0.009(2) -0.016(3) -0.010(2) C38 0.045(3) 0.046(3) 0.065(4) -0.009(3) 0.005(3) -0.011(3) C39 0.045(3) 0.048(3) 0.045(3) -0.013(3) 0.014(3) 0.015(2) C40 0.064(4) 0.060(3) 0.051(4) -0.020(3) -0.013(3) -0.014(3) C41 0.058(4) 0.054(3) 0.046(3) -0.016(3) 0.001(3) -0.016(2) C42 0.056(4) 0.059(3) 0.063(4) -0.016(3) -0.013(3) -0.020(3) C43 0.056(4) 0.050(3) 0.062(4) 0.000(3) -0.017(3) -0.009(3) C44 0.059(4) 0.059(3) 0.064(4) 0.013(3) -0.008(3) -0.012(3) C45 0.049(4) 0.063(3) 0.048(3) -0.018(3) 0.008(3) -0.014(3) C46 0.055(4) 0.053(3) 0.055(4) 0.014(3) -0.027(3) -0.009(3) C47 0.062(4) 0.070(4) 0.042(3) 0.008(3) -0.015(3) -0.011(3) C48 0.060(4) 0.063(3) 0.068(4) -0.011(3) -0.021(3) -0.025(3) C49 0.058(4) 0.042(2) 0.050(3) -0.014(3) -0.015(3) -0.010(2) C50 0.051(3) 0.041(2) 0.038(3) -0.013(2) -0.011(3) -0.008(2) C51 0.058(4) 0.045(3) 0.042(3) -0.014(3) -0.006(3) -0.009(2) La1 0.02964(16) 0.03034(14) 0.02944(15) -0.00946(10) -0.00916(11) -0.00858(10) N1 0.043(3) 0.043(2) 0.056(3) -0.010(2) -0.011(2) 0.011(2) N2 0.041(3) 0.047(2) 0.046(3) -0.010(2) 0.014(2) -0.013(2) N3 0.071(4) 0.056(3) 0.054(3) -0.019(3) -0.019(3) 0.010(2) N4 0.059(3) 0.049(2) 0.061(3) -0.020(2) -0.016(3) -0.008(2) N5 0.065(4) 0.051(2) 0.063(3) 0.008(2) -0.021(3) -0.015(2) N6 0.054(3) 0.047(2) 0.043(3) -0.009(2) 0.006(2) -0.014(2) O1 0.037(2) 0.0437(17) 0.038(2) -0.0131(16) -0.0044(17) 0.0104(15) O2 0.044(2) 0.0383(16) 0.0381(19) -0.0103(15) -0.0122(18) 0.0103(14) O3 0.0322(17) 0.0315(13) 0.0310(17) -0.0115(13) -0.0101(14) -0.0082(13) O4 0.047(2) 0.0419(17) 0.042(2) 0.0055(16) -0.0100(18) -0.0118(15) O5 0.037(2) 0.0481(18) 0.0363(19) -0.0067(17) -0.0058(16) -0.0144(15) O6 0.0280(17) 0.0312(13) 0.0291(16) -0.0083(13) -0.0083(14) -0.0096(12) O7 0.054(2) 0.0397(16) 0.050(2) -0.0109(16) -0.0196(19) -0.0137(15) O8 0.042(2) 0.0388(16) 0.045(2) -0.0157(15) -0.0065(17) -0.0108(15) O9 0.047(2) 0.0431(17) 0.0398(19) -0.0122(16) -0.0156(17) -0.0113(15) O10 0.039(2) 0.0375(15) 0.041(2) -0.0084(15) -0.0088(16) -0.0082(14) O11 0.0324(19) 0.0410(16) 0.0393(19) -0.0098(15) -0.0075(16) -0.0043(14) O12 0.065(3) 0.067(2) 0.069(3) -0.019(2) -0.019(2) -0.021(2) O13 0.076(3) 0.054(2) 0.068(3) 0.007(2) -0.023(3) -0.018(2) O14 0.061(3) 0.056(2) 0.065(3) -0.014(2) -0.016(2) 0.010(2) O15 0.060(3) 0.0470(19) 0.058(3) 0.0099(19) -0.020(2) -0.0083(18) O1W 0.062(12) 0.047(8) 0.114(15) 0.006(8) -0.014(11) -0.044(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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 C2 C1 C6 . . 119.3(5) ? C2 C1 C10 . . 121.9(4) ? C6 C1 C10 . . 118.8(5) ? C1 C2 C7 . . 117.6(4) ? C3 C2 C1 . . 120.0(4) ? C3 C2 C7 . . 122.4(5) ? C2 C3 C4 . . 121.9(5) ? C2 C3 C18 . 2_755 118.8(4) ? C4 C3 C18 . 2_755 119.3(5) ? C3 C4 C8 . . 120.4(5) ? C5 C4 C3 . . 116.9(5) ? C5 C4 C8 . . 122.7(4) ? C4 C5 C26 . 1_665 120.5(4) ? C6 C5 C4 . . 122.8(4) ? C6 C5 C26 . 1_665 116.5(4) ? C1 C6 C9 . . 121.7(5) ? C5 C6 C1 . . 118.7(5) ? C5 C6 C9 . . 119.6(4) ? C2 C7 H7A . . 109.5 ? C2 C7 H7B . . 109.5 ? C2 C7 H7C . . 109.5 ? H7A C7 H7B . . 109.5 ? H7A C7 H7C . . 109.5 ? H7B C7 H7C . . 109.5 ? C4 C8 H8A . . 110.4 ? C4 C8 H8B . . 109.2 ? C4 C8 H8C . . 108.8 ? H8A C8 H8B . . 109.2 ? H8A C8 H8C . . 109.4 ? H8B C8 H8C . . 109.9 ? C6 C9 H9A . . 109.5 ? C6 C9 H9B . . 109.5 ? C6 C9 H9C . . 109.5 ? H9A C9 H9B . . 109.5 ? H9A C9 H9C . . 109.5 ? H9B C9 H9C . . 109.5 ? C1 C10 H10A . . 110.2 ? C1 C10 H10B . . 110.2 ? H10A C10 H10B . . 108.5 ? O1 C10 C1 . . 107.4(4) ? O1 C10 H10A . . 110.2 ? O1 C10 H10B . . 110.2 ? C16 C11 C12 . . 120.1(5) ? O1 C11 C12 . . 115.8(4) ? O1 C11 C16 . . 124.1(4) ? C11 C12 H12 . . 120.0 ? C13 C12 C11 . . 120.0(5) ? C13 C12 H12 . . 120.0 ? C12 C13 H13 . . 119.9 ? C14 C13 C12 . . 120.3(4) ? C14 C13 H13 . . 119.9 ? C13 C14 C15 . . 119.1(4) ? C13 C14 C17 . . 120.9(4) ? C15 C14 C17 . . 120.0(4) ? C14 C15 H15 . . 119.9 ? C16 C15 C14 . . 120.3(5) ? C16 C15 H15 . . 119.9 ? C11 C16 C15 . . 120.2(5) ? C11 C16 H16 . . 119.9 ? C15 C16 H16 . . 119.9 ? C14 C17 La1 . . 172.0(4) ? O2 C17 C14 . . 118.9(4) ? O2 C17 La1 . . 53.3(2) ? O2 C17 O3 . . 120.3(4) ? O3 C17 C14 . . 120.6(4) ? O3 C17 La1 . . 67.3(2) ? C3 C18 H18A 2_755 . 110.7 ? C3 C18 H18B 2_755 . 110.7 ? H18A C18 H18B . . 108.8 ? O4 C18 C3 . 2_755 105.0(4) ? O4 C18 H18A . . 110.7 ? O4 C18 H18B . . 110.7 ? C20 C19 C24 . . 126.3(5) ? C20 C19 O4 . . 121.3(4) ? C24 C19 O4 . . 112.5(5) ? C19 C20 H20 . . 121.0 ? C19 C20 C21 . . 118.1(5) ? C21 C20 H20 . . 121.0 ? C20 C21 H21 . . 120.5 ? C22 C21 C20 . . 119.0(5) ? C22 C21 H21 . . 120.5 ? C21 C22 C23 . . 119.9(4) ? C21 C22 C25 . . 119.7(5) ? C23 C22 C25 . . 120.3(4) ? C22 C23 H23 . . 119.3 ? C22 C23 C24 . . 121.4(4) ? C24 C23 H23 . . 119.3 ? C19 C24 C23 . . 115.3(5) ? C19 C24 H24 . . 122.4 ? C23 C24 H24 . . 122.4 ? O5 C25 C22 . . 116.9(4) ? O6 C25 C22 . . 120.8(4) ? O6 C25 O5 . . 122.2(4) ? C5 C26 H26A 1_445 . 110.6 ? C5 C26 H26B 1_445 . 110.6 ? H26A C26 H26B . . 108.7 ? O7 C26 C5 . 1_445 105.7(4) ? O7 C26 H26A . . 110.6 ? O7 C26 H26B . . 110.6 ? C28 C27 C32 . . 119.9(4) ? O7 C27 C28 . . 116.5(4) ? O7 C27 C32 . . 123.4(4) ? C27 C28 H28 . . 120.2 ? C27 C28 C29 . . 119.6(5) ? C29 C28 H28 . . 120.2 ? C28 C29 H29 . . 119.8 ? C30 C29 C28 . . 120.4(5) ? C30 C29 H29 . . 119.8 ? C29 C30 C33 . . 119.5(5) ? C31 C30 C29 . . 119.2(4) ? C31 C30 C33 . . 121.2(4) ? C30 C31 H31 . . 118.9 ? C30 C31 C32 . . 122.3(5) ? C32 C31 H31 . . 118.9 ? C27 C32 H32 . . 120.8 ? C31 C32 C27 . . 118.5(5) ? C31 C32 H32 . . 120.8 ? C30 C33 La1 . . 164.9(4) ? O8 C33 C30 . . 119.8(4) ? O8 C33 La1 . . 61.3(2) ? O8 C33 O9 . . 119.4(4) ? O9 C33 C30 . . 120.8(5) ? O9 C33 La1 . . 60.6(2) ? N1 C34 H34 . . 117.4 ? O10 C34 H34 . . 117.4 ? O10 C34 N1 . . 125.2(4) ? H35A C35 H35B . . 109.5 ? H35A C35 H35C . . 109.5 ? H35B C35 H35C . . 109.5 ? N1 C35 H35A . . 109.5 ? N1 C35 H35B . . 109.5 ? N1 C35 H35C . . 109.5 ? H36A C36 H36B . . 109.5 ? H36A C36 H36C . . 109.5 ? H36B C36 H36C . . 109.5 ? N1 C36 H36A . . 109.5 ? N1 C36 H36B . . 109.5 ? N1 C36 H36C . . 109.5 ? N2 C37 H37 . . 118.4 ? O11 C37 H37 . . 118.4 ? O11 C37 N2 . . 123.1(4) ? H38A C38 H38B . . 109.5 ? H38A C38 H38C . . 109.5 ? H38B C38 H38C . . 109.5 ? N2 C38 H38A . . 109.5 ? N2 C38 H38B . . 109.5 ? N2 C38 H38C . . 109.5 ? H39A C39 H39B . . 109.5 ? H39A C39 H39C . . 109.5 ? H39B C39 H39C . . 109.5 ? N2 C39 H39A . . 109.5 ? N2 C39 H39B . . 109.5 ? N2 C39 H39C . . 109.5 ? N3 C40 H40 . . 119.6 ? O12 C40 H40 . . 119.6 ? O12 C40 N3 . . 120.8(6) ? H41A C41 H41B . . 109.5 ? H41A C41 H41C . . 109.5 ? H41B C41 H41C . . 109.5 ? N3 C41 H41A . . 109.5 ? N3 C41 H41B . . 109.5 ? N3 C41 H41C . . 109.5 ? H42A C42 H42B . . 109.5 ? H42A C42 H42C . . 109.5 ? H42B C42 H42C . . 109.5 ? N3 C42 H42A . . 109.5 ? N3 C42 H42B . . 109.5 ? N3 C42 H42C . . 109.5 ? N4 C43 H43 . . 121.5 ? O13 C43 H43 . . 121.5 ? O13 C43 N4 . . 116.9(5) ? H44A C44 H44B . . 109.5 ? H44A C44 H44C . . 109.5 ? H44B C44 H44C . . 109.5 ? N4 C44 H44A . . 109.5 ? N4 C44 H44B . . 109.5 ? N4 C44 H44C . . 109.5 ? H45A C45 H45B . . 109.5 ? H45A C45 H45C . . 109.5 ? H45B C45 H45C . . 109.5 ? N4 C45 H45A . . 109.5 ? N4 C45 H45B . . 109.5 ? N4 C45 H45C . . 109.5 ? N5 C46 H46 . . 114.8 ? O14 C46 H46 . . 114.8 ? O14 C46 N5 . . 130.4(6) ? H47A C47 H47B . . 109.5 ? H47A C47 H47C . . 109.5 ? H47B C47 H47C . . 109.5 ? N5 C47 H47A . . 109.5 ? N5 C47 H47B . . 109.5 ? N5 C47 H47C . . 109.5 ? H48A C48 H48B . . 109.5 ? H48A C48 H48C . . 109.5 ? H48B C48 H48C . . 109.5 ? N5 C48 H48A . . 109.5 ? N5 C48 H48B . . 109.5 ? N5 C48 H48C . . 109.5 ? N6 C49 H49 . . 119.2 ? O15 C49 H49 . . 119.2 ? O15 C49 N6 . . 121.5(5) ? H50A C50 H50B . . 109.5 ? H50A C50 H50C . . 109.5 ? H50B C50 H50C . . 109.5 ? N6 C50 H50A . . 109.5 ? N6 C50 H50B . . 109.5 ? N6 C50 H50C . . 109.5 ? H51A C51 H51B . . 109.5 ? H51A C51 H51C . . 109.5 ? H51B C51 H51C . . 109.5 ? N6 C51 H51A . . 109.5 ? N6 C51 H51B . . 109.5 ? N6 C51 H51C . . 109.5 ? C17 La1 La1 . 2_656 59.02(10) ? C33 La1 C17 . . 122.80(13) ? C33 La1 La1 . 2_656 123.07(11) ? O2 La1 C17 . . 23.60(12) ? O2 La1 C33 . . 111.32(13) ? O2 La1 La1 . 2_656 82.62(8) ? O2 La1 O3 . . 47.96(9) y O2 La1 O8 . . 134.30(11) y O2 La1 O9 . . 91.06(10) y O2 La1 O10 . . 70.09(11) y O2 La1 O11 . . 138.56(11) y O3 La1 C17 2_656 . 100.21(12) ? O3 La1 C17 . . 24.42(11) ? O3 La1 C33 2_656 . 99.45(12) ? O3 La1 C33 . . 131.34(12) ? O3 La1 La1 2_656 2_656 41.32(6) ? O3 La1 La1 . 2_656 34.87(6) ? O3 La1 O2 2_656 . 123.71(10) y O3 La1 O3 2_656 . 76.18(9) y O3 La1 O5 2_656 . 74.94(11) y O3 La1 O6 2_656 2_656 77.31(9) y O3 La1 O8 2_656 . 76.93(9) y O3 La1 O9 2_656 . 124.55(9) y O3 La1 O10 2_656 . 152.29(11) y O3 La1 O11 2_656 . 87.92(10) y O5 La1 C17 . . 67.17(11) ? O5 La1 C33 . . 67.23(12) ? O5 La1 La1 . 2_656 63.79(7) ? O5 La1 O2 . . 75.42(11) y O5 La1 O3 . . 64.87(9) y O5 La1 O6 . 2_656 130.71(10) y O5 La1 O8 . . 71.96(10) y O5 La1 O9 . . 74.53(11) y O5 La1 O10 . . 132.54(11) y O5 La1 O11 . . 144.16(10) y O6 La1 C17 2_656 . 78.87(11) ? O6 La1 C33 2_656 . 158.14(12) ? O6 La1 La1 2_656 2_656 68.39(7) ? O6 La1 O2 2_656 . 87.62(10) ? O6 La1 O3 2_656 . 69.42(9) ? O6 La1 O8 2_656 . 138.06(10) ? O6 La1 O9 2_656 . 153.00(11) ? O6 La1 O10 2_656 . 79.68(10) ? O6 La1 O11 2_656 . 72.92(9) ? O8 La1 C17 . . 138.18(12) ? O8 La1 C33 . . 25.17(12) ? O8 La1 La1 . 2_656 109.60(8) ? O8 La1 O3 . . 133.56(10) y O9 La1 C17 . . 108.82(12) ? O9 La1 C33 . . 25.44(13) ? O9 La1 La1 . 2_656 138.13(8) ? O9 La1 O3 . . 127.17(10) y O9 La1 O8 . . 49.95(10) y O10 La1 C17 . . 90.23(12) ? O10 La1 C33 . . 96.15(12) ? O10 La1 La1 . 2_656 138.62(6) ? O10 La1 O3 . . 109.70(9) y O10 La1 O8 . . 111.73(10) y O10 La1 O9 . . 74.55(10) y O10 La1 O11 . . 70.61(10) y O11 La1 C17 . . 148.14(11) ? O11 La1 C33 . . 85.41(12) ? O11 La1 La1 . 2_656 120.68(7) ? O11 La1 O3 . . 141.44(9) y O11 La1 O8 . . 73.61(10) y O11 La1 O9 . . 90.81(11) y C34 N1 C35 . . 121.4(4) ? C34 N1 C36 . . 122.4(4) ? C35 N1 C36 . . 116.2(4) ? C37 N2 C38 . . 120.8(4) ? C37 N2 C39 . . 121.2(4) ? C39 N2 C38 . . 118.0(4) ? C40 N3 C41 . . 126.2(5) ? C40 N3 C42 . . 115.1(5) ? C42 N3 C41 . . 118.5(4) ? C43 N4 C44 . . 139.2(5) ? C43 N4 C45 . . 105.0(4) ? C44 N4 C45 . . 115.9(5) ? C46 N5 C47 . . 135.7(5) ? C46 N5 C48 . . 113.7(5) ? C47 N5 C48 . . 110.5(5) ? C49 N6 C50 . . 122.8(5) ? C49 N6 C51 . . 117.0(4) ? C50 N6 C51 . . 120.2(4) ? C11 O1 C10 . . 116.7(4) ? C17 O2 La1 . . 103.1(3) ? C17 O3 La1 . 2_656 164.0(3) ? C17 O3 La1 . . 88.3(3) ? La1 O3 La1 2_656 . 103.82(9) ? C19 O4 C18 . . 115.7(4) ? C25 O5 La1 . . 142.2(3) ? C25 O6 La1 . 2_656 136.5(3) ? C27 O7 C26 . . 118.1(4) ? C33 O8 La1 . . 93.6(2) ? C33 O9 La1 . . 94.0(3) ? C34 O10 La1 . . 131.8(4) ? C37 O11 La1 . . 125.2(3) ? H1WA O1W H1WB . . 109.5 ? 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 C1 C2 . 1.417(7) ? C1 C6 . 1.418(6) ? C1 C10 . 1.524(7) ? C2 C3 . 1.356(7) ? C2 C7 . 1.530(5) ? C3 C4 . 1.417(6) ? C3 C18 2_755 1.523(7) ? C4 C5 . 1.409(7) ? C4 C8 . 1.495(7) ? C5 C6 . 1.369(7) ? C5 C26 1_665 1.544(5) ? C6 C9 . 1.545(7) ? C7 H7A . 0.9600 ? C7 H7B . 0.9600 ? C7 H7C . 0.9600 ? C8 H8A . 0.9648 ? C8 H8B . 0.9587 ? C8 H8C . 0.9565 ? C9 H9A . 0.9600 ? C9 H9B . 0.9600 ? C9 H9C . 0.9600 ? C10 H10A . 0.9700 ? C10 H10B . 0.9700 ? C10 O1 . 1.442(6) ? C11 C12 . 1.396(7) ? C11 C16 . 1.371(7) ? C11 O1 . 1.361(5) ? C12 H12 . 0.9300 ? C12 C13 . 1.388(7) ? C13 H13 . 0.9300 ? C13 C14 . 1.382(7) ? C14 C15 . 1.408(7) ? C14 C17 . 1.482(6) ? C15 H15 . 0.9300 ? C15 C16 . 1.382(7) ? C16 H16 . 0.9300 ? C17 La1 . 3.064(5) ? C17 O2 . 1.260(6) ? C17 O3 . 1.267(5) ? C18 H18A . 0.9700 ? C18 H18B . 0.9700 ? C18 O4 . 1.437(6) ? C19 C20 . 1.349(7) ? C19 C24 . 1.367(7) ? C19 O4 . 1.414(6) ? C20 H20 . 0.9300 ? C20 C21 . 1.432(6) ? C21 H21 . 0.9300 ? C21 C22 . 1.389(6) ? C22 C23 . 1.399(7) ? C22 C25 . 1.488(6) ? C23 H23 . 0.9300 ? C23 C24 . 1.426(7) ? C24 H24 . 0.9300 ? C25 O5 . 1.270(6) ? C25 O6 . 1.270(5) ? C26 H26A . 0.9700 ? C26 H26B . 0.9700 ? C26 O7 . 1.430(6) ? C27 C28 . 1.368(7) ? C27 C32 . 1.408(7) ? C27 O7 . 1.363(5) ? C28 H28 . 0.9300 ? C28 C29 . 1.422(6) ? C29 H29 . 0.9300 ? C29 C30 . 1.382(7) ? C30 C31 . 1.347(7) ? C30 C33 . 1.460(6) ? C31 H31 . 0.9300 ? C31 C32 . 1.404(6) ? C32 H32 . 0.9300 ? C33 La1 . 2.936(4) ? C33 O8 . 1.251(6) ? C33 O9 . 1.264(6) ? C34 H34 . 0.9300 ? C34 N1 . 1.368(7) ? C34 O10 . 1.236(6) ? C35 H35A . 0.9600 ? C35 H35B . 0.9600 ? C35 H35C . 0.9600 ? C35 N1 . 1.484(6) ? C36 H36A . 0.9600 ? C36 H36B . 0.9600 ? C36 H36C . 0.9600 ? C36 N1 . 1.491(6) ? C37 H37 . 0.9300 ? C37 N2 . 1.369(7) ? C37 O11 . 1.241(6) ? C38 H38A . 0.9600 ? C38 H38B . 0.9600 ? C38 H38C . 0.9600 ? C38 N2 . 1.512(7) ? C39 H39A . 0.9600 ? C39 H39B . 0.9600 ? C39 H39C . 0.9600 ? C39 N2 . 1.499(6) ? C40 H40 . 0.9300 ? C40 N3 . 1.377(7) ? C40 O12 . 1.258(7) ? C41 H41A . 0.9600 ? C41 H41B . 0.9600 ? C41 H41C . 0.9600 ? C41 N3 . 1.485(7) ? C42 H42A . 0.9600 ? C42 H42B . 0.9600 ? C42 H42C . 0.9600 ? C42 N3 . 1.481(8) ? C43 H43 . 0.9300 ? C43 N4 . 1.399(7) ? C43 O13 . 1.259(6) ? C44 H44A . 0.9600 ? C44 H44B . 0.9600 ? C44 H44C . 0.9600 ? C44 N4 . 1.486(7) ? C45 H45A . 0.9600 ? C45 H45B . 0.9600 ? C45 H45C . 0.9600 ? C45 N4 . 1.514(7) ? C46 H46 . 0.9300 ? C46 N5 . 1.355(7) ? C46 O14 . 1.248(7) ? C47 H47A . 0.9600 ? C47 H47B . 0.9600 ? C47 H47C . 0.9600 ? C47 N5 . 1.481(7) ? C48 H48A . 0.9600 ? C48 H48B . 0.9600 ? C48 H48C . 0.9600 ? C48 N5 . 1.513(7) ? C49 H49 . 0.9300 ? C49 N6 . 1.388(7) ? C49 O15 . 1.273(6) ? C50 H50A . 0.9600 ? C50 H50B . 0.9600 ? C50 H50C . 0.9600 ? C50 N6 . 1.458(6) ? C51 H51A . 0.9600 ? C51 H51B . 0.9600 ? C51 H51C . 0.9600 ? C51 N6 . 1.472(7) ? La1 La1 2_656 4.1587(8) y La1 O2 . 2.522(3) y La1 O3 2_656 2.448(3) y La1 O3 . 2.827(3) y La1 O5 . 2.453(4) y La1 O6 2_656 2.459(2) y La1 O8 . 2.580(3) y La1 O9 . 2.564(3) y La1 O10 . 2.529(3) y La1 O11 . 2.562(3) y O1W H1WA . 0.8500 ? O1W H1WB . 0.8500 ? 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 C23 H23 O14 2_656 0.93 2.31 3.063(7) 137.8 yes C41 H41A O12 2_755 0.96 2.43 3.274(8) 147.0 yes C47 H47B O14 2_566 0.96 2.41 3.284(8) 151.5 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_4 _geom_torsion C1 C2 C3 C4 . . 0.6(8) C1 C2 C3 C18 . 2_755 -178.6(4) C1 C10 O1 C11 . . -159.0(4) C2 C1 C6 C5 . . 7.9(7) C2 C1 C6 C9 . . -172.4(5) C2 C1 C10 O1 . . 77.7(6) C2 C3 C4 C5 . . 1.6(8) C2 C3 C4 C8 . . -178.8(5) C3 C4 C5 C6 . . 1.0(7) C3 C4 C5 C26 . 1_665 175.3(4) C3 C18 O4 C19 2_755 . 171.6(4) C4 C5 C6 C1 . . -5.8(8) C4 C5 C6 C9 . . 174.5(4) C5 C26 O7 C27 1_445 . -151.3(4) C6 C1 C2 C3 . . -5.4(7) C6 C1 C2 C7 . . 175.6(4) C6 C1 C10 O1 . . -102.0(5) C7 C2 C3 C4 . . 179.6(5) C7 C2 C3 C18 . 2_755 0.3(8) C8 C4 C5 C6 . . -178.5(5) C8 C4 C5 C26 . 1_665 -4.3(7) C10 C1 C2 C3 . . 174.8(5) C10 C1 C2 C7 . . -4.2(7) C10 C1 C6 C5 . . -172.3(5) C10 C1 C6 C9 . . 7.3(7) C11 C12 C13 C14 . . -0.3(8) C12 C11 C16 C15 . . 0.3(8) C12 C11 O1 C10 . . 174.1(4) C12 C13 C14 C15 . . -0.5(8) C12 C13 C14 C17 . . 178.0(5) C13 C14 C15 C16 . . 1.1(8) C13 C14 C17 O2 . . -173.8(5) C13 C14 C17 O3 . . 10.5(7) C14 C15 C16 C11 . . -1.0(8) C14 C17 O2 La1 . . 178.4(4) C14 C17 O3 La1 . . -179.2(4) C14 C17 O3 La1 . 2_656 -39.5(11) C15 C14 C17 O2 . . 4.7(7) C15 C14 C17 O3 . . -171.0(4) C16 C11 C12 C13 . . 0.4(8) C16 C11 O1 C10 . . -5.4(8) C17 C14 C15 C16 . . -177.4(5) C18 C3 C4 C5 2_755 . -179.2(4) C18 C3 C4 C8 2_755 . 0.4(7) C19 C20 C21 C22 . . -2.4(7) C20 C19 C24 C23 . . -0.3(8) C20 C19 O4 C18 . . 5.3(7) C20 C21 C22 C23 . . 1.6(7) C20 C21 C22 C25 . . -175.5(4) C21 C22 C23 C24 . . -0.1(7) C21 C22 C25 O5 . . -2.6(6) C21 C22 C25 O6 . . -179.6(4) C22 C23 C24 C19 . . -0.6(7) C22 C25 O5 La1 . . 150.0(3) C22 C25 O6 La1 . 2_656 175.5(3) C23 C22 C25 O5 . . -179.7(4) C23 C22 C25 O6 . . 3.3(6) C24 C19 C20 C21 . . 1.8(8) C24 C19 O4 C18 . . -175.1(4) C25 C22 C23 C24 . . 177.0(4) C26 C5 C6 C1 1_665 . 179.8(4) C26 C5 C6 C9 1_665 . 0.1(7) C27 C28 C29 C30 . . 0.9(8) C28 C27 C32 C31 . . 1.7(8) C28 C27 O7 C26 . . 161.0(5) C28 C29 C30 C31 . . -2.1(8) C28 C29 C30 C33 . . -179.0(5) C29 C30 C31 C32 . . 3.3(8) C29 C30 C33 La1 . . 72.7(15) C29 C30 C33 O8 . . -17.2(7) C29 C30 C33 O9 . . 163.5(5) C30 C31 C32 C27 . . -3.1(8) C30 C33 O8 La1 . . 162.8(4) C30 C33 O9 La1 . . -162.6(4) C31 C30 C33 La1 . . -104.1(14) C31 C30 C33 O8 . . 165.9(5) C31 C30 C33 O9 . . -13.3(8) C32 C27 C28 C29 . . -0.7(8) C32 C27 O7 C26 . . -14.1(7) C33 C30 C31 C32 . . -179.9(5) La1 C17 O3 La1 . 2_656 139.7(9) N1 C34 O10 La1 . . 118.8(5) N2 C37 O11 La1 . . -177.0(4) O1 C11 C12 C13 . . -179.2(5) O1 C11 C16 C15 . . 179.8(5) O2 C17 O3 La1 . . 5.1(4) O2 C17 O3 La1 . 2_656 144.8(7) O3 C17 O2 La1 . . -5.9(5) O4 C19 C20 C21 . . -178.7(4) O4 C19 C24 C23 . . -179.8(4) O5 C25 O6 La1 . 2_656 -1.4(7) O6 C25 O5 La1 . . -33.1(7) O7 C27 C28 C29 . . -176.0(5) O7 C27 C32 C31 . . 176.7(5) O8 C33 O9 La1 . . 18.1(5) O9 C33 O8 La1 . . -18.0(5) O10 C34 N1 C35 . . -179.8(5) O10 C34 N1 C36 . . -0.3(9) O11 C37 N2 C38 . . 173.1(5) O11 C37 N2 C39 . . -6.3(8) O12 C40 N3 C41 . . -17.0(10) O12 C40 N3 C42 . . 168.6(6) O13 C43 N4 C44 . . -142.9(7) O13 C43 N4 C45 . . 36.8(7) O14 C46 N5 C47 . . 164.4(6) O14 C46 N5 C48 . . -15.2(9) O15 C49 N6 C50 . . 2.9(8) O15 C49 N6 C51 . . -180.0(5) _cod_database_fobs_code 2021747