# Electronic Supplementary Material (ESI) for Dalton Transactions. # This journal is © The Royal Society of Chemistry 2024 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_mo_mja_nk_11052021_2_0m _database_code_depnum_ccdc_archive 'CCDC 2248985' loop_ _audit_author_name _audit_author_address 'Cassandra Ward' ;Wayne State University United States of America ; _audit_update_record ; 2023-03-15 deposited with the CCDC. 2024-04-29 downloaded from the CCDC. ; _audit_creation_date 2021-11-10 _audit_creation_method ; Olex2 1.5 (compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410) ; _shelx_SHELXL_version_number 2019/1 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C20 H38 N4 O5 U, 3(I)' _chemical_formula_sum 'C20 H38 I3 N4 O5 U' _chemical_formula_weight 1033.27 _chemical_melting_point ? 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' I I -0.4742 1.8119 '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' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system orthorhombic _space_group_IT_number 73 _space_group_name_H-M_alt 'I b c a' _space_group_name_Hall '-I 2b 2c' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-x+1/2, y+1, -z+1' 'x+1, -y+1, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'x+1/2, -y, z' '-x, y, z+1/2' _cell_length_a 13.9235(4) _cell_length_b 14.4448(3) _cell_length_c 30.0718(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6048.1(3) _cell_formula_units_Z 8 _cell_measurement_reflns_used 9950 _cell_measurement_temperature 100 _cell_measurement_theta_max 34.309 _cell_measurement_theta_min 2.442 _shelx_estimated_absorpt_T_max 0.728 _shelx_estimated_absorpt_T_min 0.485 _exptl_absorpt_coefficient_mu 8.463 _exptl_absorpt_correction_T_max 0.4972 _exptl_absorpt_correction_T_min 0.3892 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1114 before and 0.0678 after correction. The Ratio of minimum to maximum transmission is 0.7828. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 2.270 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 3816 _exptl_crystal_recrystallization_method 'Vapour diffusion with acetonitrile, hexane, and ether.' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_unetI/netI 0.0258 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_number 37598 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.725 _diffrn_reflns_theta_min 2.442 _diffrn_ambient_temperature 100 _diffrn_detector 'Photon III' _diffrn_detector_area_resol_mean ? _diffrn_detector_type 'CPAD area detector' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device '\k--geometry diffractometer' _diffrn_measurement_device_type 'Bruker D8 VENTURE' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_collimation '0.8 mm pinhole collimator' _diffrn_radiation_monochromator 'multilayer mirror' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'microfocus sealed tube' _diffrn_source_current 1.4 _diffrn_source_power 0.07 _diffrn_source_target Mo _diffrn_source_type 'Incoatec I\mS' _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2747 _reflns_number_total 3215 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_collection ? _computing_data_reduction 'SAINT V8.40B (?, 2016)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _refine_diff_density_max 1.926 _refine_diff_density_min -1.133 _refine_diff_density_rms 0.154 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 168 _refine_ls_number_reflns 3215 _refine_ls_number_restraints 90 _refine_ls_R_factor_all 0.0321 _refine_ls_R_factor_gt 0.0254 _refine_ls_restrained_S_all 1.030 _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^)+(0.0293P)^2^+28.8178P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.0635 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Uiso/Uaniso restraints and constraints All non-hydrogen atoms have similar U: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A 3. Others Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=1-FVAR(1) Sof(C2S)=Sof(H2SA)=Sof(H2SB)=Sof(H2SC)=FVAR(1) Fixed Sof: I3(0.5) 4.a Secondary CH2 refined with riding coordinates: C3(H3A,H3B), C7(H7A,H7B), C8(H8A,H8B), C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B) 4.b Idealised Me refined as rotating group: C2S(H2SA,H2SB,H2SC), C9(H9A,H9B,H9C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.500000 0.250000 0.38367(2) 0.01293(7) Uani 1 2 d S T P . . O3 O 0.500000 0.250000 0.46644(14) 0.0194(6) Uani 1 2 d S TU P . . N1S N 0.4328(3) 0.1731(3) 0.31022(13) 0.0339(7) Uani 1 1 d . U . . . C3 C 0.3156(3) 0.4129(3) 0.37024(14) 0.0200(5) Uani 1 1 d . U . . . H3A H 0.297754 0.461881 0.348750 0.024 Uiso 1 1 calc R U . . . H3B H 0.288868 0.429481 0.399694 0.024 Uiso 1 1 calc R U . . . C7 C 0.5384(3) 0.4109(3) 0.46529(14) 0.0197(5) Uani 1 1 d . U . . . H7A H 0.471855 0.432919 0.460586 0.024 Uiso 1 1 calc R U . . . H7B H 0.573885 0.460113 0.481272 0.024 Uiso 1 1 calc R U . . . C8 C 0.5361(3) 0.3250(3) 0.49374(13) 0.0202(5) Uani 1 1 d . U . . . H8A H 0.601485 0.310269 0.504627 0.024 Uiso 1 1 calc R U . . . H8B H 0.493728 0.334639 0.519758 0.024 Uiso 1 1 calc R U . . . O1 O 0.4187(2) 0.4045(2) 0.37287(9) 0.0195(4) Uani 1 1 d . U . . . O2 O 0.3205(2) 0.25350(19) 0.38374(10) 0.0206(5) Uani 1 1 d . U . . . N1 N 0.5842(2) 0.3953(2) 0.42164(12) 0.0190(4) Uani 1 1 d . U . . . C1 C 0.2675(3) 0.1687(3) 0.38821(15) 0.0215(6) Uani 1 1 d . U . . . H1A H 0.273941 0.130298 0.361103 0.026 Uiso 1 1 calc R U . . . H1B H 0.198566 0.181486 0.393422 0.026 Uiso 1 1 calc R U . . . C1S C 0.4244(4) 0.1501(4) 0.27479(17) 0.0356(7) Uani 1 1 d . U . . . C2 C 0.2766(3) 0.3217(3) 0.35540(15) 0.0207(5) Uani 1 1 d . U . . . H2A H 0.205863 0.320188 0.358567 0.025 Uiso 1 1 calc R U . . . H2B H 0.293229 0.309998 0.323881 0.025 Uiso 1 1 calc R U . . . C4 C 0.4624(3) 0.4922(3) 0.38238(15) 0.0205(5) Uani 1 1 d . U . . . H4A H 0.430369 0.521258 0.408245 0.025 Uiso 1 1 calc R U . . . H4B H 0.455316 0.534025 0.356508 0.025 Uiso 1 1 calc R U . . . C5 C 0.5685(3) 0.4773(3) 0.39250(15) 0.0202(5) Uani 1 1 d . U . . . H5A H 0.603924 0.468567 0.364268 0.024 Uiso 1 1 calc R U . . . H5B H 0.594516 0.533160 0.407317 0.024 Uiso 1 1 calc R U . . . C2S C 0.4261(7) 0.0997(9) 0.2299(3) 0.0369(11) Uani 0.567(12) 1 d . U P A 1 H2SA H 0.479028 0.054955 0.229542 0.055 Uiso 0.567(12) 1 calc R U P A 1 H2SB H 0.435210 0.144777 0.205901 0.055 Uiso 0.567(12) 1 calc R U P A 1 H2SC H 0.365110 0.067038 0.225504 0.055 Uiso 0.567(12) 1 calc R U P A 1 I1 I 0.500000 0.250000 0.62046(2) 0.02075(10) Uani 1 2 d S T P . . I2 I 0.250000 0.38189(3) 0.500000 0.02050(10) Uani 1 2 d S T P . . I3 I 0.16855(5) 0.03766(6) 0.25659(3) 0.0533(3) Uani 0.5 1 d . . P B -1 C9 C 0.4048(9) 0.1518(11) 0.2271(4) 0.0366(11) Uani 0.433(12) 1 d . U P A 2 H9A H 0.384583 0.214155 0.218340 0.055 Uiso 0.433(12) 1 calc R U P A 2 H9B H 0.353475 0.107574 0.220250 0.055 Uiso 0.433(12) 1 calc R U P A 2 H9C H 0.463015 0.134715 0.210774 0.055 Uiso 0.433(12) 1 calc R U P A 2 C6 C 0.6889(3) 0.3793(3) 0.42757(14) 0.0193(6) Uani 1 1 d . U . . . H6A H 0.699351 0.341231 0.454511 0.023 Uiso 1 1 calc R U . . . H6B H 0.721411 0.439496 0.432108 0.023 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.01059(11) 0.01107(11) 0.01714(12) 0.000 0.000 0.00042(8) O3 0.0182(12) 0.0193(13) 0.0207(13) 0.000 0.000 -0.0030(11) N1S 0.0312(16) 0.0453(19) 0.0253(15) 0.0014(14) -0.0052(14) -0.0068(14) C3 0.0151(10) 0.0177(10) 0.0274(10) 0.0047(9) -0.0008(9) 0.0021(9) C7 0.0172(10) 0.0188(10) 0.0231(10) -0.0030(8) 0.0014(8) -0.0024(9) C8 0.0185(11) 0.0199(11) 0.0220(11) -0.0023(8) 0.0005(8) -0.0030(9) O1 0.0158(9) 0.0159(9) 0.0269(10) 0.0024(8) 0.0001(8) 0.0016(8) O2 0.0138(9) 0.0194(10) 0.0287(11) 0.0078(9) -0.0029(8) -0.0003(8) N1 0.0157(9) 0.0168(9) 0.0245(9) -0.0024(8) 0.0011(8) -0.0017(8) C1 0.0140(12) 0.0203(13) 0.0301(13) 0.0076(11) -0.0032(11) -0.0008(10) C1S 0.0327(16) 0.048(2) 0.0261(15) 0.0015(15) -0.0049(14) -0.0086(14) C2 0.0148(10) 0.0190(10) 0.0281(11) 0.0068(9) -0.0018(9) 0.0010(9) C4 0.0175(10) 0.0163(10) 0.0276(10) 0.0008(8) 0.0007(9) 0.0002(9) C5 0.0174(10) 0.0166(10) 0.0266(10) -0.0005(9) 0.0009(9) -0.0011(9) C2S 0.035(2) 0.049(2) 0.026(2) 0.000(2) -0.0043(19) -0.009(2) I1 0.01405(19) 0.0169(2) 0.0313(2) 0.000 0.000 -0.00145(14) I2 0.02018(18) 0.02075(19) 0.02056(19) 0.000 0.00178(15) 0.000 I3 0.0285(3) 0.0976(8) 0.0339(4) 0.0289(5) -0.0010(3) -0.0083(4) C9 0.035(2) 0.049(2) 0.026(2) 0.001(2) -0.0051(19) -0.008(2) C6 0.0150(11) 0.0176(11) 0.0254(12) -0.0033(10) 0.0008(10) -0.0017(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O3 2.489(4) . ? U1 N1S 2.644(4) 6_554 ? U1 N1S 2.644(4) . ? U1 O1 2.524(3) . ? U1 O1 2.524(3) 6_554 ? U1 O2 2.499(3) . ? U1 O2 2.499(3) 6_554 ? U1 N1 2.661(3) 6_554 ? U1 N1 2.661(3) . ? O3 C8 1.450(5) . ? O3 C8 1.450(5) 6_554 ? N1S C1S 1.122(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 O1 1.443(5) . ? C3 C2 1.493(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.507(6) . ? C7 N1 1.477(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? O1 C4 1.434(5) . ? O2 C1 1.437(5) . ? O2 C2 1.439(5) . ? N1 C5 1.490(5) . ? N1 C6 1.486(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C1 C6 1.500(6) 6_554 ? C1S C2S 1.535(11) . ? C1S C9 1.460(13) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C4 C5 1.523(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 U1 N1S 146.66(9) . . ? O3 U1 N1S 146.66(9) . 6_554 ? O3 U1 O1 97.40(6) . . ? O3 U1 O1 97.40(6) . 6_554 ? O3 U1 O2 89.95(7) . 6_554 ? O3 U1 O2 89.95(7) . . ? O3 U1 N1 64.59(7) . 6_554 ? O3 U1 N1 64.59(7) . . ? N1S U1 N1S 66.68(18) . 6_554 ? N1S U1 N1 82.59(12) . 6_554 ? N1S U1 N1 147.77(12) 6_554 6_554 ? N1S U1 N1 82.59(12) 6_554 . ? N1S U1 N1 147.77(12) . . ? O1 U1 N1S 96.04(12) . . ? O1 U1 N1S 96.04(12) 6_554 6_554 ? O1 U1 N1S 71.31(12) 6_554 . ? O1 U1 N1S 71.31(12) . 6_554 ? O1 U1 O1 165.21(13) . 6_554 ? O1 U1 N1 123.71(10) . 6_554 ? O1 U1 N1 63.61(10) 6_554 6_554 ? O1 U1 N1 123.71(10) 6_554 . ? O1 U1 N1 63.61(10) . . ? O2 U1 N1S 110.26(11) 6_554 . ? O2 U1 N1S 69.83(11) . . ? O2 U1 N1S 69.83(11) 6_554 6_554 ? O2 U1 N1S 110.25(11) . 6_554 ? O2 U1 O1 62.20(9) 6_554 6_554 ? O2 U1 O1 62.20(9) . . ? O2 U1 O1 117.81(9) . 6_554 ? O2 U1 O1 117.81(9) 6_554 . ? O2 U1 O2 179.91(14) . 6_554 ? O2 U1 N1 64.86(9) . 6_554 ? O2 U1 N1 64.86(9) 6_554 . ? O2 U1 N1 115.09(10) 6_554 6_554 ? O2 U1 N1 115.09(10) . . ? N1 U1 N1 129.18(15) 6_554 . ? C8 O3 U1 124.5(2) . . ? C8 O3 U1 124.5(2) 6_554 . ? C8 O3 C8 111.0(4) . 6_554 ? C1S N1S U1 162.6(4) . . ? H3A C3 H3B 108.5 . . ? O1 C3 H3A 110.2 . . ? O1 C3 H3B 110.2 . . ? O1 C3 C2 107.7(3) . . ? C2 C3 H3A 110.2 . . ? C2 C3 H3B 110.2 . . ? H7A C7 H7B 107.8 . . ? C8 C7 H7A 109.0 . . ? C8 C7 H7B 109.0 . . ? N1 C7 H7A 109.0 . . ? N1 C7 H7B 109.0 . . ? N1 C7 C8 112.8(3) . . ? O3 C8 C7 107.5(3) . . ? O3 C8 H8A 110.2 . . ? O3 C8 H8B 110.2 . . ? C7 C8 H8A 110.2 . . ? C7 C8 H8B 110.2 . . ? H8A C8 H8B 108.5 . . ? C3 O1 U1 121.8(2) . . ? C4 O1 U1 124.4(2) . . ? C4 O1 C3 111.1(3) . . ? C1 O2 U1 119.8(2) . . ? C1 O2 C2 114.9(3) . . ? C2 O2 U1 116.0(2) . . ? C7 N1 U1 108.2(2) . . ? C7 N1 C5 109.8(3) . . ? C7 N1 C6 109.9(3) . . ? C5 N1 U1 108.1(2) . . ? C6 N1 U1 111.2(2) . . ? C6 N1 C5 109.7(3) . . ? O2 C1 H1A 110.7 . . ? O2 C1 H1B 110.7 . . ? O2 C1 C6 105.1(3) . 6_554 ? H1A C1 H1B 108.8 . . ? C6 C1 H1A 110.7 6_554 . ? C6 C1 H1B 110.7 6_554 . ? N1S C1S C2S 167.0(7) . . ? N1S C1S C9 161.3(8) . . ? C3 C2 H2A 110.6 . . ? C3 C2 H2B 110.6 . . ? O2 C2 C3 105.8(3) . . ? O2 C2 H2A 110.6 . . ? O2 C2 H2B 110.6 . . ? H2A C2 H2B 108.7 . . ? O1 C4 H4A 109.9 . . ? O1 C4 H4B 109.9 . . ? O1 C4 C5 109.1(3) . . ? H4A C4 H4B 108.3 . . ? C5 C4 H4A 109.9 . . ? C5 C4 H4B 109.9 . . ? N1 C5 C4 111.8(3) . . ? N1 C5 H5A 109.3 . . ? N1 C5 H5B 109.3 . . ? C4 C5 H5A 109.3 . . ? C4 C5 H5B 109.3 . . ? H5A C5 H5B 107.9 . . ? C1S C2S H2SA 109.5 . . ? C1S C2S H2SB 109.5 . . ? C1S C2S H2SC 109.5 . . ? H2SA C2S H2SB 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? C1S C9 H9A 109.5 . . ? C1S C9 H9B 109.5 . . ? C1S C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C6 C1 112.0(3) . 6_554 ? N1 C6 H6A 109.2 . . ? N1 C6 H6B 109.2 . . ? C1 C6 H6A 109.2 6_554 . ? C1 C6 H6B 109.2 6_554 . ? H6A C6 H6B 107.9 . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag U1 O3 C8 C7 20.1(4) . . . . ? U1 N1S C1S C2S 90(3) . . . . ? U1 N1S C1S C9 -75(3) . . . . ? U1 O1 C4 C5 9.0(5) . . . . ? U1 O2 C1 C6 49.6(4) . . . 6_554 ? U1 O2 C2 C3 -57.5(4) . . . . ? U1 N1 C5 C4 54.1(4) . . . . ? U1 N1 C6 C1 40.3(4) . . . 6_554 ? C3 O1 C4 C5 170.6(3) . . . . ? C7 N1 C5 C4 -63.6(4) . . . . ? C7 N1 C6 C1 160.0(3) . . . 6_554 ? C8 O3 C8 C7 -159.9(4) 6_554 . . . ? C8 C7 N1 U1 52.3(4) . . . . ? C8 C7 N1 C5 170.0(3) . . . . ? C8 C7 N1 C6 -69.2(4) . . . . ? O1 C3 C2 O2 49.5(4) . . . . ? O1 C4 C5 N1 -42.7(5) . . . . ? N1 C7 C8 O3 -48.3(4) . . . . ? C1 O2 C2 C3 155.8(3) . . . . ? C2 C3 O1 U1 -24.0(4) . . . . ? C2 C3 O1 C4 173.9(3) . . . . ? C2 O2 C1 C6 -165.1(3) . . . 6_554 ? C5 N1 C6 C1 -79.2(4) . . . 6_554 ? C6 N1 C5 C4 175.5(3) . . . . ? _shelx_res_file ; TITL mo_mja_nk_11052021_2_0m_a.res in Ibca mo_mja_nk_11052021_2_0m.res created by SHELXL-2019/1 at 08:51:34 on 10-Nov-2021 REM Old TITL mo_MJA_NK_11052021_2_0m in Ibca REM SHELXT solution in Ibca: R1 0.303, Rweak 0.003, Alpha 0.029 REM 0.250 for 324 systematic absences, Orientation as input REM Formula found by SHELXT: C22 N4 O5 I2 U CELL 0.71073 13.9235 14.4448 30.0718 90 90 90 ZERR 8 0.0004 0.0003 0.0009 0 0 0 LATT 2 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H I N O U UNIT 160 304 24 32 40 8 SIMU 0.001 0.002 2 L.S. 10 PLAN 20 SIZE 0.04 0.04 0.1 TEMP -173.15 CONF BOND list 4 MORE -1 BOND $H fmap 2 acta SHEL 999 0.79 REM REM REM WGHT 0.029300 28.817799 FVAR 0.06793 0.56721 U1 6 0.500000 0.250000 0.383673 10.50000 0.01059 0.01107 = 0.01714 0.00000 0.00000 0.00042 O3 5 0.500000 0.250000 0.466436 10.50000 0.01816 0.01930 = 0.02066 0.00000 0.00000 -0.00302 N1S 4 0.432766 0.173068 0.310223 11.00000 0.03120 0.04528 = 0.02527 0.00141 -0.00520 -0.00680 C3 1 0.315561 0.412881 0.370241 11.00000 0.01509 0.01767 = 0.02737 0.00473 -0.00084 0.00211 AFIX 23 H3A 2 0.297754 0.461881 0.348750 11.00000 -1.20000 H3B 2 0.288868 0.429481 0.399694 11.00000 -1.20000 AFIX 0 C7 1 0.538416 0.410900 0.465294 11.00000 0.01718 0.01880 = 0.02311 -0.00296 0.00144 -0.00242 AFIX 23 H7A 2 0.471855 0.432919 0.460586 11.00000 -1.20000 H7B 2 0.573885 0.460113 0.481272 11.00000 -1.20000 AFIX 0 C8 1 0.536147 0.325015 0.493745 11.00000 0.01854 0.01989 = 0.02202 -0.00231 0.00055 -0.00295 AFIX 23 H8A 2 0.601485 0.310269 0.504627 11.00000 -1.20000 H8B 2 0.493728 0.334639 0.519758 11.00000 -1.20000 AFIX 0 O1 5 0.418680 0.404508 0.372868 11.00000 0.01577 0.01591 = 0.02691 0.00242 0.00008 0.00164 O2 5 0.320549 0.253498 0.383739 11.00000 0.01375 0.01939 = 0.02867 0.00776 -0.00294 -0.00032 N1 4 0.584182 0.395277 0.421641 11.00000 0.01575 0.01677 = 0.02454 -0.00243 0.00106 -0.00167 C1 1 0.267506 0.168692 0.388210 11.00000 0.01401 0.02029 = 0.03014 0.00762 -0.00322 -0.00084 AFIX 23 H1A 2 0.273941 0.130298 0.361103 11.00000 -1.20000 H1B 2 0.198566 0.181486 0.393422 11.00000 -1.20000 AFIX 0 C1S 1 0.424430 0.150150 0.274792 11.00000 0.03271 0.04795 = 0.02607 0.00151 -0.00488 -0.00864 C2 1 0.276620 0.321654 0.355398 11.00000 0.01482 0.01901 = 0.02812 0.00681 -0.00184 0.00096 AFIX 23 H2A 2 0.205863 0.320188 0.358567 11.00000 -1.20000 H2B 2 0.293229 0.309998 0.323881 11.00000 -1.20000 AFIX 0 C4 1 0.462410 0.492202 0.382382 11.00000 0.01748 0.01626 = 0.02761 0.00083 0.00065 0.00025 AFIX 23 H4A 2 0.430369 0.521258 0.408245 11.00000 -1.20000 H4B 2 0.455316 0.534025 0.356508 11.00000 -1.20000 AFIX 0 C5 1 0.568504 0.477327 0.392502 11.00000 0.01742 0.01661 = 0.02659 -0.00054 0.00090 -0.00110 AFIX 23 H5A 2 0.603924 0.468567 0.364268 11.00000 -1.20000 H5B 2 0.594516 0.533160 0.407317 11.00000 -1.20000 AFIX 0 PART 1 C2S 1 0.426095 0.099665 0.229874 21.00000 0.03544 0.04908 = 0.02613 0.00025 -0.00428 -0.00863 AFIX 137 H2SA 2 0.479028 0.054955 0.229542 21.00000 -1.50000 H2SB 2 0.435210 0.144777 0.205901 21.00000 -1.50000 H2SC 2 0.365110 0.067038 0.225504 21.00000 -1.50000 AFIX 0 PART 0 I1 3 0.500000 0.250000 0.620458 10.50000 0.01405 0.01687 = 0.03134 0.00000 0.00000 -0.00145 I2 3 0.250000 0.381885 0.500000 10.50000 0.02018 0.02075 = 0.02056 0.00000 0.00178 0.00000 PART -1 I3 3 0.168552 0.037656 0.256594 10.50000 0.02852 0.09764 = 0.03388 0.02890 -0.00098 -0.00832 PART 2 C9 1 0.404760 0.151783 0.227123 -21.00000 0.03456 0.04916 = 0.02610 0.00121 -0.00508 -0.00796 AFIX 137 H9A 2 0.384583 0.214155 0.218340 -21.00000 -1.50000 H9B 2 0.353475 0.107574 0.220250 -21.00000 -1.50000 H9C 2 0.463015 0.134715 0.210774 -21.00000 -1.50000 AFIX 0 PART 0 C6 1 0.688856 0.379303 0.427571 11.00000 0.01501 0.01761 = 0.02538 -0.00330 0.00081 -0.00167 AFIX 23 H6A 2 0.699351 0.341231 0.454511 11.00000 -1.20000 H6B 2 0.721411 0.439496 0.432108 11.00000 -1.20000 AFIX 0 HKLF 4 REM mo_mja_nk_11052021_2_0m_a.res in Ibca REM wR2 = 0.0635, GooF = S = 1.030, Restrained GooF = 1.030 for all data REM R1 = 0.0254 for 2747 Fo > 4sig(Fo) and 0.0321 for all 3215 data REM 168 parameters refined using 90 restraints END WGHT 0.0293 28.8380 REM Highest difference peak 1.926, deepest hole -1.133, 1-sigma level 0.154 Q1 1 0.5000 0.2500 0.6448 10.50000 0.05 1.93 Q2 1 0.5000 0.2500 0.3541 10.50000 0.05 1.62 Q3 1 0.1983 0.0000 0.2500 10.50000 0.05 1.10 Q4 1 0.5080 0.4968 0.3872 11.00000 0.05 0.91 Q5 1 0.5000 0.2500 0.4201 10.50000 0.05 0.90 Q6 1 0.3262 0.0000 0.2500 10.50000 0.05 0.86 Q7 1 0.2518 0.1155 0.2612 11.00000 0.05 0.80 Q8 1 0.7500 0.3677 0.5000 10.50000 0.05 0.70 Q9 1 0.5000 0.2500 0.5814 10.50000 0.05 0.65 Q10 1 0.2456 0.1178 0.2407 11.00000 0.05 0.65 Q11 1 0.4024 0.1861 0.2760 11.00000 0.05 0.58 Q12 1 0.5335 0.3713 0.4797 11.00000 0.05 0.51 Q13 1 0.4416 0.1175 0.2763 11.00000 0.05 0.48 Q14 1 0.4549 0.1941 0.3274 11.00000 0.05 0.46 Q15 1 0.7000 0.3702 0.4037 11.00000 0.05 0.46 Q16 1 0.2877 0.3732 0.3640 11.00000 0.05 0.45 Q17 1 0.5749 0.1781 0.1853 11.00000 0.05 0.43 Q18 1 0.5000 0.2500 0.5336 10.50000 0.05 0.43 Q19 1 0.4848 0.1992 0.4068 11.00000 0.05 0.42 Q20 1 0.3277 0.0659 0.2501 11.00000 0.05 0.41 ; _shelx_res_checksum 5360 _olex2_exptl_crystal_mounting_method 'The crystal was mounted on a MicroMount (MiTeGen) with paratone oil (Parabar 10312, Hampton Research).' _olex2_submission_special_instructions 'No special instructions were received' ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_mo_mja_nk_11052021_0m _database_code_depnum_ccdc_archive 'CCDC 2248986' loop_ _audit_author_name _audit_author_address 'Cassandra Ward' ;Wayne State University United States of America ; _audit_update_record ; 2023-03-15 deposited with the CCDC. 2024-04-29 downloaded from the CCDC. ; # start Validation Reply Form _vrf_PLAT973_mo_mja_nk_11052021_0m ; PROBLEM: Check Calcd Positive Resid. Density on U1 1.61 eA-3 RESPONSE: This is due to absorption despite using a small crystal and adjusting the mu*r value. ; # end Validation Reply Form _audit_creation_date 2021-11-10 _audit_creation_method ; Olex2 1.5 (compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410) ; _shelx_SHELXL_version_number 2019/1 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C22 H46 N4 O7 U, 3(I)' _chemical_formula_sum 'C22 H46 I3 N4 O7 U' _chemical_formula_weight 1097.36 _chemical_melting_point ? 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' I I -0.4742 1.8119 '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' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system orthorhombic _space_group_IT_number 73 _space_group_name_H-M_alt 'I b c a' _space_group_name_Hall '-I 2b 2c' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-x+1/2, y+1, -z+1' 'x+1, -y+1, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'x+1/2, -y, z' '-x, y, z+1/2' _cell_length_a 14.2159(5) _cell_length_b 14.8269(5) _cell_length_c 31.2033(11) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6577.0(4) _cell_formula_units_Z 8 _cell_measurement_reflns_used 9997 _cell_measurement_temperature 100.00 _cell_measurement_theta_max 30.477 _cell_measurement_theta_min 2.376 _shelx_estimated_absorpt_T_max 0.652 _shelx_estimated_absorpt_T_min 0.652 _exptl_absorpt_coefficient_mu 7.794 _exptl_absorpt_correction_T_max 0.4935 _exptl_absorpt_correction_T_min 0.4108 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1285 before and 0.0693 after correction. The Ratio of minimum to maximum transmission is 0.8324. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 2.216 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 4104 _exptl_crystal_recrystallization_method 'Vapour diffusion in dimethylformamide and ether' _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_unetI/netI 0.0233 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_number 38026 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.020 _diffrn_reflns_theta_min 2.376 _diffrn_ambient_temperature 100.00 _diffrn_detector 'Photon III' _diffrn_detector_area_resol_mean ? _diffrn_detector_type 'CPAD area detector' _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device '\k--geometry diffractometer' _diffrn_measurement_device_type 'Bruker D8 VENTURE' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_collimation '0.8 mm pinhole collimator' _diffrn_radiation_monochromator 'multilayer mirror' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'microfocus sealed tube' _diffrn_source_current 1.4 _diffrn_source_power 0.07 _diffrn_source_target Mo _diffrn_source_type 'Incoatec I\mS' _diffrn_source_voltage 50.0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 3040 _reflns_number_total 3240 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_collection ? _computing_data_reduction 'SAINT V8.40B (?, 2016)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _refine_diff_density_max 1.831 _refine_diff_density_min -1.318 _refine_diff_density_rms 0.142 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 172 _refine_ls_number_reflns 3240 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0273 _refine_ls_R_factor_gt 0.0252 _refine_ls_restrained_S_all 1.031 _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^)+(0.0356P)^2^+37.2613P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.0668 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C8(H8A,H8B), C2(H2A,H2B), C4(H4A,H4B), C7(H7A,H7B), C6(H6A,H6B), C3(H3A,H3B), C1(H1A,H1B), C5(H5A,H5B) 2.b Aromatic/amide H refined with riding coordinates: C1S(H1S) 2.c Idealised Me refined as rotating group: C3S(H3SA,H3SB,H3SC), C2S(H2SA,H2SB,H2SC) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.500000 0.250000 0.61257(2) 0.01274(8) Uani 1 2 d S T P . . I1 I 0.500000 -0.250000 0.61324(2) 0.01851(10) Uani 1 2 d S T P . . I2 I 0.750000 0.10922(3) 0.500000 0.02773(11) Uani 1 2 d S T P . . O2 O 0.57841(19) 0.09543(17) 0.62401(9) 0.0197(6) Uani 1 1 d . . . . . O3 O 0.500000 0.250000 0.53221(12) 0.0194(8) Uani 1 2 d S T P . . O1S O 0.5710(2) 0.31557(19) 0.67780(8) 0.0227(6) Uani 1 1 d . . . . . O1 O 0.3217(2) 0.25854(17) 0.60931(9) 0.0199(6) Uani 1 1 d . . . . . N1 N 0.4157(2) 0.1083(2) 0.57535(10) 0.0186(7) Uani 1 1 d . . . . . N1S N 0.5643(3) 0.3439(2) 0.74917(10) 0.0202(7) Uani 1 1 d . . . . . C1S C 0.5380(3) 0.3564(3) 0.70959(12) 0.0203(8) Uani 1 1 d . . . . . H1S H 0.490112 0.399726 0.704452 0.024 Uiso 1 1 calc R U . . . C8 C 0.4626(3) 0.1781(3) 0.50597(12) 0.0247(9) Uani 1 1 d . . . . . H8A H 0.502926 0.168774 0.480493 0.030 Uiso 1 1 calc R U . . . H8B H 0.398387 0.193588 0.496092 0.030 Uiso 1 1 calc R U . . . C2 C 0.3122(3) 0.1241(3) 0.56990(14) 0.0248(9) Uani 1 1 d . . . . . H2A H 0.279773 0.065368 0.566874 0.030 Uiso 1 1 calc R U . . . H2B H 0.301318 0.159102 0.543341 0.030 Uiso 1 1 calc R U . . . C4 C 0.5339(4) 0.0111(3) 0.61225(14) 0.0249(9) Uani 1 1 d . . . . . H4A H 0.540272 -0.032881 0.635923 0.030 Uiso 1 1 calc R U . . . H4B H 0.564817 -0.014264 0.586512 0.030 Uiso 1 1 calc R U . . . C7 C 0.4601(3) 0.0940(3) 0.53277(12) 0.0221(8) Uani 1 1 d . . . . . H7A H 0.424839 0.046683 0.517161 0.027 Uiso 1 1 calc R U . . . H7B H 0.525212 0.071964 0.536987 0.027 Uiso 1 1 calc R U . . . C6 C 0.7203(3) 0.1756(3) 0.63704(12) 0.0234(9) Uani 1 1 d . . . . . H6A H 0.705530 0.189322 0.667357 0.028 Uiso 1 1 calc R U . . . H6B H 0.789508 0.175370 0.633474 0.028 Uiso 1 1 calc R U . . . C3 C 0.4311(3) 0.0281(3) 0.60309(14) 0.0236(9) Uani 1 1 d . . . . . H3A H 0.404085 -0.025731 0.588874 0.028 Uiso 1 1 calc R U . . . H3B H 0.397401 0.036849 0.630536 0.028 Uiso 1 1 calc R U . . . C1 C 0.2714(3) 0.1744(3) 0.60735(14) 0.0250(9) Uani 1 1 d . . . . . H1A H 0.203292 0.185152 0.603032 0.030 Uiso 1 1 calc R U . . . H1B H 0.280077 0.139734 0.634183 0.030 Uiso 1 1 calc R U . . . C5 C 0.6799(3) 0.0862(3) 0.62457(14) 0.0239(9) Uani 1 1 d . . . . . H5A H 0.703038 0.068232 0.595883 0.029 Uiso 1 1 calc R U . . . H5B H 0.698850 0.039350 0.645480 0.029 Uiso 1 1 calc R U . . . C3S C 0.5315(3) 0.4012(3) 0.78391(13) 0.0267(9) Uani 1 1 d . . . . . H3SA H 0.475325 0.434201 0.774670 0.040 Uiso 1 1 calc R U . . . H3SB H 0.581051 0.444219 0.791628 0.040 Uiso 1 1 calc R U . . . H3SC H 0.516091 0.363866 0.808853 0.040 Uiso 1 1 calc R U . . . C2S C 0.6374(3) 0.2790(3) 0.76007(14) 0.0272(9) Uani 1 1 d . . . . . H2SA H 0.641947 0.233534 0.737383 0.041 Uiso 1 1 calc R U . . . H2SB H 0.621597 0.249563 0.787247 0.041 Uiso 1 1 calc R U . . . H2SC H 0.697751 0.310353 0.762910 0.041 Uiso 1 1 calc R U . . . I3 I 0.71714(4) 0.000000 0.750000 0.03956(13) Uani 1 2 d S T P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.01529(13) 0.01098(12) 0.01196(11) 0.000 0.000 0.00065(6) I1 0.0199(2) 0.0200(2) 0.01565(19) 0.000 0.000 -0.00198(12) I2 0.0339(2) 0.0271(2) 0.0222(2) 0.000 0.00181(15) 0.000 O2 0.0226(15) 0.0137(13) 0.0228(13) 0.0007(11) 0.0029(11) 0.0027(11) O3 0.026(2) 0.0162(19) 0.0158(19) 0.000 0.000 -0.0022(14) O1S 0.0256(16) 0.0242(14) 0.0184(13) -0.0066(11) -0.0028(11) -0.0003(12) O1 0.0168(15) 0.0204(14) 0.0224(15) -0.0021(10) -0.0006(11) 0.0006(11) N1 0.0201(17) 0.0158(15) 0.0200(16) -0.0013(13) 0.0009(13) -0.0004(13) N1S 0.0241(19) 0.0174(16) 0.0190(17) -0.0026(12) -0.0009(13) 0.0008(14) C1S 0.023(2) 0.0156(18) 0.022(2) -0.0035(15) 0.0000(16) -0.0012(15) C8 0.032(2) 0.027(2) 0.0156(19) -0.0063(16) -0.0006(17) -0.0054(19) C2 0.020(2) 0.024(2) 0.031(2) -0.0016(17) -0.0008(17) -0.0053(16) C4 0.033(3) 0.0129(19) 0.028(2) 0.0003(15) 0.0065(19) 0.0021(17) C7 0.027(2) 0.020(2) 0.0186(19) -0.0071(15) 0.0016(16) -0.0019(16) C6 0.023(2) 0.026(2) 0.021(2) 0.0039(16) 0.0000(16) 0.0058(18) C3 0.030(2) 0.0134(18) 0.027(2) -0.0014(16) 0.0027(18) -0.0040(17) C1 0.018(2) 0.022(2) 0.034(2) -0.0022(18) 0.0014(17) -0.0057(17) C5 0.022(2) 0.023(2) 0.027(2) 0.0038(17) 0.0037(17) 0.0088(17) C3S 0.032(2) 0.028(2) 0.020(2) -0.0007(17) 0.0015(18) 0.0031(19) C2S 0.030(2) 0.024(2) 0.028(2) -0.0019(18) -0.0073(18) 0.0048(19) I3 0.0261(3) 0.0284(2) 0.0642(3) 0.0132(2) 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O2 2.573(3) . ? U1 O2 2.573(3) 6_554 ? U1 O3 2.507(4) . ? U1 O1S 2.471(3) 6_554 ? U1 O1S 2.471(3) . ? U1 O1 2.540(3) . ? U1 O1 2.540(3) 6_554 ? U1 N1 2.683(3) . ? U1 N1 2.683(3) 6_554 ? O2 C4 1.448(5) . ? O2 C5 1.449(5) . ? O3 C8 1.446(5) . ? O3 C8 1.446(5) 6_554 ? O1S C1S 1.253(5) . ? O1 C6 1.434(5) 6_554 ? O1 C1 1.440(5) . ? N1 C2 1.499(5) . ? N1 C7 1.487(5) . ? N1 C3 1.488(5) . ? N1S C1S 1.303(5) . ? N1S C3S 1.454(5) . ? N1S C2S 1.456(5) . ? C1S H1S 0.9500 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 C7 1.502(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2 C1 1.503(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C4 C3 1.510(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C6 C5 1.497(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C3S H3SA 0.9800 . ? C3S H3SB 0.9800 . ? C3S H3SC 0.9800 . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 U1 O2 164.05(12) 6_554 . ? O2 U1 N1 124.32(9) 6_554 . ? O2 U1 N1 124.32(9) . 6_554 ? O2 U1 N1 63.66(9) 6_554 6_554 ? O2 U1 N1 63.66(9) . . ? O3 U1 O2 97.98(6) . . ? O3 U1 O2 97.97(6) . 6_554 ? O3 U1 O1 87.71(6) . . ? O3 U1 O1 87.71(6) . 6_554 ? O3 U1 N1 64.36(7) . . ? O3 U1 N1 64.36(7) . 6_554 ? O1S U1 O2 73.28(9) . 6_554 ? O1S U1 O2 73.28(9) 6_554 . ? O1S U1 O2 93.39(9) 6_554 6_554 ? O1S U1 O2 93.39(9) . . ? O1S U1 O3 145.46(7) . . ? O1S U1 O3 145.46(7) 6_554 . ? O1S U1 O1S 69.08(13) . 6_554 ? O1S U1 O1 114.89(9) 6_554 6_554 ? O1S U1 O1 69.21(9) 6_554 . ? O1S U1 O1 114.89(9) . . ? O1S U1 O1 69.21(9) . 6_554 ? O1S U1 N1 82.30(10) 6_554 . ? O1S U1 N1 147.88(9) . . ? O1S U1 N1 82.30(10) . 6_554 ? O1S U1 N1 147.88(9) 6_554 6_554 ? O1 U1 O2 118.83(9) . . ? O1 U1 O2 61.89(8) . 6_554 ? O1 U1 O2 61.89(8) 6_554 . ? O1 U1 O2 118.83(9) 6_554 6_554 ? O1 U1 O1 175.42(12) 6_554 . ? O1 U1 N1 112.93(9) . 6_554 ? O1 U1 N1 112.93(9) 6_554 . ? O1 U1 N1 64.90(9) 6_554 6_554 ? O1 U1 N1 64.90(9) . . ? N1 U1 N1 128.72(14) . 6_554 ? C4 O2 U1 123.0(3) . . ? C4 O2 C5 110.9(3) . . ? C5 O2 U1 121.2(2) . . ? C8 O3 U1 124.5(2) 6_554 . ? C8 O3 U1 124.5(2) . . ? C8 O3 C8 111.0(4) . 6_554 ? C1S O1S U1 133.6(3) . . ? C6 O1 U1 115.2(2) 6_554 . ? C6 O1 C1 114.1(3) 6_554 . ? C1 O1 U1 117.0(2) . . ? C2 N1 U1 111.4(2) . . ? C7 N1 U1 108.0(2) . . ? C7 N1 C2 109.8(3) . . ? C7 N1 C3 110.0(3) . . ? C3 N1 U1 108.0(2) . . ? C3 N1 C2 109.6(3) . . ? C1S N1S C3S 122.1(4) . . ? C1S N1S C2S 121.3(3) . . ? C3S N1S C2S 116.1(3) . . ? O1S C1S N1S 125.1(4) . . ? O1S C1S H1S 117.5 . . ? N1S C1S H1S 117.5 . . ? O3 C8 H8A 110.1 . . ? O3 C8 H8B 110.1 . . ? O3 C8 C7 107.8(3) . . ? H8A C8 H8B 108.5 . . ? C7 C8 H8A 110.1 . . ? C7 C8 H8B 110.1 . . ? N1 C2 H2A 109.3 . . ? N1 C2 H2B 109.3 . . ? N1 C2 C1 111.6(3) . . ? H2A C2 H2B 108.0 . . ? C1 C2 H2A 109.3 . . ? C1 C2 H2B 109.3 . . ? O2 C4 H4A 109.9 . . ? O2 C4 H4B 109.9 . . ? O2 C4 C3 109.1(3) . . ? H4A C4 H4B 108.3 . . ? C3 C4 H4A 109.9 . . ? C3 C4 H4B 109.9 . . ? N1 C7 C8 112.9(3) . . ? N1 C7 H7A 109.0 . . ? N1 C7 H7B 109.0 . . ? C8 C7 H7A 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? O1 C6 H6A 110.4 6_554 . ? O1 C6 H6B 110.4 6_554 . ? O1 C6 C5 106.6(3) 6_554 . ? H6A C6 H6B 108.6 . . ? C5 C6 H6A 110.4 . . ? C5 C6 H6B 110.4 . . ? N1 C3 C4 112.7(3) . . ? N1 C3 H3A 109.1 . . ? N1 C3 H3B 109.1 . . ? C4 C3 H3A 109.1 . . ? C4 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? O1 C1 C2 105.7(3) . . ? O1 C1 H1A 110.6 . . ? O1 C1 H1B 110.6 . . ? C2 C1 H1A 110.6 . . ? C2 C1 H1B 110.6 . . ? H1A C1 H1B 108.7 . . ? O2 C5 C6 107.5(3) . . ? O2 C5 H5A 110.2 . . ? O2 C5 H5B 110.2 . . ? C6 C5 H5A 110.2 . . ? C6 C5 H5B 110.2 . . ? H5A C5 H5B 108.5 . . ? N1S C3S H3SA 109.5 . . ? N1S C3S H3SB 109.5 . . ? N1S C3S H3SC 109.5 . . ? H3SA C3S H3SB 109.5 . . ? H3SA C3S H3SC 109.5 . . ? H3SB C3S H3SC 109.5 . . ? N1S C2S H2SA 109.5 . . ? N1S C2S H2SB 109.5 . . ? N1S C2S H2SC 109.5 . . ? H2SA C2S H2SB 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag U1 O2 C4 C3 -13.3(4) . . . . ? U1 O2 C5 C6 24.5(4) . . . . ? U1 O3 C8 C7 -21.6(4) . . . . ? U1 O1S C1S N1S 138.7(3) . . . . ? U1 O1 C1 C2 -54.1(4) . . . . ? U1 N1 C2 C1 -37.5(4) . . . . ? U1 N1 C7 C8 -52.0(4) . . . . ? U1 N1 C3 C4 -55.0(4) . . . . ? O2 C4 C3 N1 46.1(4) . . . . ? O3 C8 C7 N1 49.1(4) . . . . ? O1 C6 C5 O2 -51.2(4) 6_554 . . . ? N1 C2 C1 O1 59.3(4) . . . . ? C8 O3 C8 C7 158.4(4) 6_554 . . . ? C2 N1 C7 C8 69.7(4) . . . . ? C2 N1 C3 C4 -176.6(3) . . . . ? C4 O2 C5 C6 -179.9(3) . . . . ? C7 N1 C2 C1 -157.1(3) . . . . ? C7 N1 C3 C4 62.7(4) . . . . ? C6 O1 C1 C2 167.2(3) 6_554 . . . ? C3 N1 C2 C1 82.0(4) . . . . ? C3 N1 C7 C8 -169.6(3) . . . . ? C5 O2 C4 C3 -168.4(3) . . . . ? C3S N1S C1S O1S 172.2(4) . . . . ? C2S N1S C1S O1S 0.2(6) . . . . ? _shelx_res_file ; TITL mo_mja_nk_11052021_0m_a.res in Ibca mo_mja_nk_11052021_0m.res created by SHELXL-2019/1 at 11:57:03 on 10-Nov-2021 REM Old TITL mo_mja_nk_11052021_0m_a.res in Ibca REM SHELXT solution in Ibca: R1 0.082, Rweak 0.003, Alpha 0.058 REM 0.275 for 340 systematic absences, Orientation as input REM Formula found by SHELXT: C22 I3 N4 O7 U CELL 0.71073 14.2159 14.8269 31.2033 90 90 90 ZERR 8 0.0005 0.0005 0.0011 0 0 0 LATT 2 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H I N O U UNIT 176 368 24 32 56 8 L.S. 10 PLAN 7 SIZE 0.06 0.06 0.06 TEMP -173.15 CONF BOND list 4 MORE -1 BOND $H fmap 2 acta SHEL 999 0.81 REM REM REM WGHT 0.035600 37.261303 FVAR 0.07005 U1 6 0.500000 0.250000 0.612565 10.50000 0.01529 0.01098 = 0.01196 0.00000 0.00000 0.00065 I1 3 0.500000 -0.250000 0.613240 10.50000 0.01992 0.01997 = 0.01565 0.00000 0.00000 -0.00198 I2 3 0.750000 0.109223 0.500000 10.50000 0.03391 0.02711 = 0.02218 0.00000 0.00181 0.00000 O2 5 0.578411 0.095429 0.624009 11.00000 0.02256 0.01368 = 0.02283 0.00069 0.00289 0.00273 O3 5 0.500000 0.250000 0.532211 10.50000 0.02613 0.01616 = 0.01585 0.00000 0.00000 -0.00220 O1S 5 0.570989 0.315569 0.677803 11.00000 0.02557 0.02423 = 0.01840 -0.00655 -0.00281 -0.00029 O1 5 0.321689 0.258540 0.609311 11.00000 0.01683 0.02038 = 0.02241 -0.00214 -0.00057 0.00057 N1 4 0.415661 0.108311 0.575354 11.00000 0.02013 0.01576 = 0.02001 -0.00132 0.00091 -0.00037 N1S 4 0.564272 0.343886 0.749169 11.00000 0.02413 0.01738 = 0.01902 -0.00265 -0.00086 0.00075 C1S 1 0.537991 0.356356 0.709591 11.00000 0.02325 0.01560 = 0.02220 -0.00351 0.00005 -0.00124 AFIX 43 H1S 2 0.490112 0.399726 0.704452 11.00000 -1.20000 AFIX 0 C8 1 0.462568 0.178101 0.505967 11.00000 0.03178 0.02668 = 0.01562 -0.00635 -0.00055 -0.00536 AFIX 23 H8A 2 0.502926 0.168774 0.480493 11.00000 -1.20000 H8B 2 0.398387 0.193588 0.496092 11.00000 -1.20000 AFIX 0 C2 1 0.312217 0.124106 0.569901 11.00000 0.02022 0.02352 = 0.03072 -0.00159 -0.00084 -0.00533 AFIX 23 H2A 2 0.279773 0.065368 0.566874 11.00000 -1.20000 H2B 2 0.301318 0.159102 0.543341 11.00000 -1.20000 AFIX 0 C4 1 0.533877 0.011139 0.612246 11.00000 0.03336 0.01294 = 0.02847 0.00027 0.00652 0.00209 AFIX 23 H4A 2 0.540272 -0.032881 0.635923 11.00000 -1.20000 H4B 2 0.564817 -0.014264 0.586512 11.00000 -1.20000 AFIX 0 C7 1 0.460113 0.093961 0.532772 11.00000 0.02718 0.02050 = 0.01858 -0.00712 0.00158 -0.00186 AFIX 23 H7A 2 0.424839 0.046683 0.517161 11.00000 -1.20000 H7B 2 0.525212 0.071964 0.536987 11.00000 -1.20000 AFIX 0 C6 1 0.720310 0.175638 0.637042 11.00000 0.02307 0.02645 = 0.02055 0.00393 -0.00001 0.00578 AFIX 23 H6A 2 0.705530 0.189322 0.667357 11.00000 -1.20000 H6B 2 0.789508 0.175370 0.633474 11.00000 -1.20000 AFIX 0 C3 1 0.431102 0.028051 0.603088 11.00000 0.03036 0.01337 = 0.02718 -0.00140 0.00272 -0.00402 AFIX 23 H3A 2 0.404085 -0.025731 0.588874 11.00000 -1.20000 H3B 2 0.397401 0.036849 0.630536 11.00000 -1.20000 AFIX 0 C1 1 0.271363 0.174385 0.607355 11.00000 0.01826 0.02236 = 0.03426 -0.00216 0.00140 -0.00568 AFIX 23 H1A 2 0.203292 0.185152 0.603032 11.00000 -1.20000 H1B 2 0.280077 0.139734 0.634183 11.00000 -1.20000 AFIX 0 C5 1 0.679892 0.086160 0.624569 11.00000 0.02201 0.02286 = 0.02680 0.00380 0.00372 0.00885 AFIX 23 H5A 2 0.703038 0.068232 0.595883 11.00000 -1.20000 H5B 2 0.698850 0.039350 0.645480 11.00000 -1.20000 AFIX 0 C3S 1 0.531514 0.401217 0.783912 11.00000 0.03231 0.02805 = 0.01984 -0.00065 0.00147 0.00306 AFIX 137 H3SA 2 0.475325 0.434201 0.774670 11.00000 -1.50000 H3SB 2 0.581051 0.444219 0.791628 11.00000 -1.50000 H3SC 2 0.516091 0.363866 0.808853 11.00000 -1.50000 AFIX 0 C2S 1 0.637366 0.279033 0.760068 11.00000 0.03036 0.02360 = 0.02778 -0.00195 -0.00731 0.00480 AFIX 137 H2SA 2 0.641947 0.233534 0.737383 11.00000 -1.50000 H2SB 2 0.621597 0.249563 0.787247 11.00000 -1.50000 H2SC 2 0.697751 0.310353 0.762910 11.00000 -1.50000 AFIX 0 I3 3 0.717140 0.000000 0.750000 10.50000 0.02608 0.02838 = 0.06422 0.01318 0.00000 0.00000 HKLF 4 REM mo_mja_nk_11052021_0m_a.res in Ibca REM wR2 = 0.0668, GooF = S = 1.031, Restrained GooF = 1.031 for all data REM R1 = 0.0252 for 3040 Fo > 4sig(Fo) and 0.0273 for all 3240 data REM 172 parameters refined using 0 restraints END WGHT 0.0356 37.2909 REM Highest difference peak 1.831, deepest hole -1.318, 1-sigma level 0.142 Q1 1 0.6979 -0.0310 0.7190 11.00000 0.05 1.83 Q2 1 0.7889 0.0000 0.7500 10.50000 0.05 1.25 Q3 1 0.2500 0.1107 0.5000 10.50000 0.05 1.22 Q4 1 0.8022 0.0791 0.4883 11.00000 0.05 1.03 Q5 1 0.5000 0.2500 0.6546 10.50000 0.05 0.90 Q6 1 0.5000 0.2500 0.5842 10.50000 0.05 0.80 Q7 1 0.5000 -0.2500 0.6584 10.50000 0.05 0.66 ; _shelx_res_checksum 38407 _olex2_exptl_crystal_mounting_method 'The crystal was mounted on a MicroMount (MiTeGen) with paratone oil (Parabar 10312, Hampton Research).' _olex2_submission_special_instructions 'No special instructions were received' ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_mb_nk_aza222_ui3_3 _database_code_depnum_ccdc_archive 'CCDC 2248987' loop_ _audit_author_name _audit_author_address 'Cassandra Ward' ;Wayne State University United States of America ; _audit_update_record ; 2023-03-15 deposited with the CCDC. 2024-04-29 downloaded from the CCDC. ; _audit_creation_date 2021-12-09 _audit_creation_method ; Olex2 1.5 (compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C20.174 H41.762 N3.013 O6.555 U0.885, 3(I), 0.115(C24 H50 N4 O8 U1), C1.073 H2.503 N0.528 O0.528' _chemical_formula_sum 'C24 H50.01 I3 N4 O8 U' _chemical_formula_weight 1141.44 _chemical_melting_point ? 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' I I -0.4742 1.8119 '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' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.8644(12) _cell_length_b 10.3453(6) _cell_length_c 18.2109(10) _cell_angle_alpha 90 _cell_angle_beta 104.769(2) _cell_angle_gamma 90 _cell_volume 3436.6(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9870 _cell_measurement_temperature 100 _cell_measurement_theta_max 28.024 _cell_measurement_theta_min 2.233 _shelx_estimated_absorpt_T_max 0.273 _shelx_estimated_absorpt_T_min 0.089 _exptl_absorpt_coefficient_mu 7.465 _exptl_absorpt_correction_T_max 0.7458 _exptl_absorpt_correction_T_min 0.4980 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1320 before and 0.0937 after correction. The Ratio of minimum to maximum transmission is 0.6677. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour green _exptl_crystal_colour_primary green _exptl_crystal_density_diffrn 2.206 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 2148 _exptl_crystal_size_max 0.626 _exptl_crystal_size_mid 0.385 _exptl_crystal_size_min 0.235 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0938 _diffrn_reflns_av_unetI/netI 0.0415 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 134878 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.730 _diffrn_reflns_theta_min 2.233 _diffrn_ambient_temperature 100 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _diffrn_source_current 30.0 _diffrn_source_power 1.5 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 6465 _reflns_number_total 7296 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_collection ? _computing_data_reduction 'SAINT V8.40B (?, 2016)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _refine_diff_density_max 0.959 _refine_diff_density_min -1.776 _refine_diff_density_rms 0.153 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.202 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 764 _refine_ls_number_reflns 7296 _refine_ls_number_restraints 1818 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0367 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+29.3223P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0872 _refine_ls_wR_factor_ref 0.0900 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Shared sites {N3, N3C} {O7, O7C} 3. Restrained distances O7-C19C \\sim O7-C19 \\sim O8-C22 \\sim O7B-C19B with sigma of 0.02 C19C-C21C \\sim C19-C21 \\sim C22-C23 \\sim C21B-C20B with sigma of 0.02 N3-C19C \\sim N3-C19 \\sim N4-C22 \\sim N3B-C19B with sigma of 0.02 C19C-C20C \\sim C19-C20 \\sim C22-C24 \\sim C19B-C20B with sigma of 0.02 N3-C21C \\sim N3-C20 \\sim N3-C20C \\sim N3-C21 \\sim N4-C24 \\sim N4-C23 \\sim N3B-C20B \\sim N3B-C21B with sigma of 0.02 C21-C20 \\sim C23-C24 \\sim C20C-C21C with sigma of 0.02 O2B-C4B \\sim O2B-C5B \\sim O1-C2 \\sim O1-C3 \\sim O3B-C8B \\sim O3B-C9B \\sim O2-C4 \\sim O2-C5 \\sim O4B- C10B \\sim O4B-C11B \\sim O3-C8 \\sim O3-C9 \\sim O1B-C2B \\sim O1B-C3B \\sim O4-C10 \\sim O4-C11 \\sim O5-C14 \\sim O5-C15 \\sim O6-C16 \\sim O6-C17 \\sim O5B-C15B \\sim O5B-C14B \\sim O6B-C16B \\sim O6B-C17B with sigma of 0.02 N1-C12 \\sim N1-C13 \\sim N1-C1 \\sim N2B-C6B \\sim N2B-C7B \\sim N2B-C18B \\sim N2-C7 \\sim N2-C18 \\sim N2- C6 \\sim N1B-C1B \\sim N1B-C13B \\sim N1B-C12B with sigma of 0.02 C12-C11 \\sim C9-C10 \\sim C2B-C1B \\sim C14B-C13B \\sim C16B-C15B \\sim C18B-C17B \\sim C14-C13 ~ C16-C15 \\sim C8B-C7B \\sim C4-C3 \\sim C10B-C9B \\sim C6-C5 \\sim C3B-C4B \\sim C6B-C5B \\sim C2-C1 \\sim C18- C17 \\sim C8-C7 \\sim C12B-C11B with sigma of 0.02 U1-N2 \\sim U1B-N1B \\sim U1-N1 \\sim U1B-N2B with sigma of 0.02 U1-O3 \\sim U1B-O4B \\sim U1-O2 \\sim U1B-O3B \\sim U1-O1 \\sim U1B-O2B \\sim U1-O4 \\sim U1B-O1B \\sim U1-O5 \\sim U1B-O6B \\sim U1B-O5B \\sim U1-O6 with sigma of 0.02 C4-C5 \\sim C2-C3 \\sim C10-C11 \\sim C8-C9 \\sim C17B-C16B \\sim C15B-C14B \\sim C14-C15 \\sim C16-C17 ~ C5B-C4B \\sim C3B-C2B \\sim C11B-C10B \\sim C9B-C8B with sigma of 0.02 C1-C12 \\sim C6B-C7B \\sim C12B-C1B \\sim C7-C6 with sigma of 0.02 C23B-C25 \\sim C23-C24 \\sim C21-C20 \\sim C20C-C21C with sigma of 0.02 N4B-C25 \\sim N4B-C23B \\sim N4-C23 \\sim N4-C24 \\sim N3-C21 \\sim N3-C20C \\sim N3-C20 \\sim N3-C21C with sigma of 0.02 C22B-C25 \\sim C22-C24 \\sim C19C-C20C \\sim C19-C20 with sigma of 0.02 4. Uiso/Uaniso restraints and constraints U1 \\sim O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim O8 \\sim N1 \\sim N2 \\sim N3 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim U1B \\sim O1B \\sim O2B \\sim O3B \\sim O4B \\sim O5B \\sim O6B \\sim O7B \\sim O8B \\sim N1B \\sim N2B \\sim N3B \\sim C1B \\sim C2B \\sim C3B \\sim C4B \\sim C5B \\sim C6B \\sim C7B \\sim C8B \\sim C9B \\sim C10B \\sim C11B \\sim C12B \\sim C13B \\sim C14B \\sim C15B \\sim C16B \\sim C17B \\sim C18B \\sim C19B \\sim C20B \\sim C21B \\sim C22B \\sim C19C \\sim H19C \\sim C20C \\sim C21C: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A N4B \\sim C22B \\sim C23B \\sim C25: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A Uanis(N3) = Uanis(N3C) Uanis(O7) = Uanis(O7C) 5. Others 1*[Sof(O7)+Sof(N3)+Sof(C19C)+Sof(H19C)+Sof(C20C)+Sof(H20G)+Sof(H20H)+ Sof(H20I)+Sof(C21C)+Sof(H21G)+Sof(H21H)+Sof(H21I)]+1*[Sof(C19)+Sof(H19)+ Sof(C20)+Sof(H20A)+Sof(H20B)+Sof(H20C)+Sof(C21)+Sof(H21A)+Sof(H21B)+Sof(H21C)+ Sof(O7C)+Sof(N3C)]=0.885 with esd of 0.001 Sof(U1B)=Sof(O1B)=Sof(O2B)=Sof(O3B)=Sof(O4B)=Sof(O5B)=Sof(O6B)=Sof(O7B)= Sof(O8B)=Sof(N1B)=Sof(N2B)=Sof(N3B)=Sof(N4B)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)= Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=Sof(C4B)=Sof(H4BA)= Sof(H4BB)=Sof(C5B)=Sof(H5BA)=Sof(H5BB)=Sof(C6B)=Sof(H6BA)=Sof(H6BB)=Sof(C7B)= Sof(H7BB)=Sof(H7BA)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)= Sof(C10B)=Sof(H10C)=Sof(H10D)=Sof(C11B)=Sof(H11C)=Sof(H11D)=Sof(C12B)= Sof(H12D)=Sof(H12C)=Sof(C13B)=Sof(H13C)=Sof(H13D)=Sof(C14B)=Sof(H14C)= Sof(H14D)=Sof(C15B)=Sof(H15C)=Sof(H15D)=Sof(C16B)=Sof(H16C)=Sof(H16D)= Sof(C17B)=Sof(H17C)=Sof(H17D)=Sof(C18B)=Sof(H18D)=Sof(H18C)=Sof(C19B)= Sof(H19B)=Sof(C20B)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C21B)=Sof(H21D)= Sof(H21E)=Sof(H21F)=Sof(C22B)=Sof(H22B)=Sof(C23B)=Sof(H23D)=Sof(H23E)= Sof(H23F)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=1-FVAR(1) Sof(U1)=Sof(O1)=Sof(O2)=Sof(O3)=Sof(O4)=Sof(O5)=Sof(O6)=Sof(O8)=Sof(N1)= Sof(N2)=Sof(N4)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C3)= Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)= Sof(H6B)=Sof(H6A)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C9)= Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(C11)=Sof(H11A)=Sof(H11B)= Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14B)= Sof(H14A)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(C17)= Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(H18B)=Sof(H18A)=Sof(C22)=Sof(H22)=Sof(C23)= Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(1) Sof(O7)=Sof(N3)=Sof(C19C)=Sof(H19C)=Sof(C20C)=Sof(H20G)=Sof(H20H)=Sof(H20I)= Sof(C21C)=Sof(H21G)=Sof(H21H)=Sof(H21I)=FVAR(2) Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C21)=Sof(H21A)= Sof(H21B)=Sof(H21C)=Sof(O7C)=Sof(N3C)=FVAR(3) Sof(I1B)=1-FVAR(4) Sof(I1)=FVAR(4) Sof(I2B)=1-FVAR(5) Sof(I2)=FVAR(5) Sof(I3B)=1-FVAR(6) Sof(I3)=FVAR(6) 6.a Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6B,H6A), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14B,H14A), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18B,H18A), C1B(H1BA,H1BB), C2B(H2BA,H2BB), C3B(H3BA, H3BB), C4B(H4BA,H4BB), C5B(H5BA,H5BB), C6B(H6BA,H6BB), C7B(H7BB,H7BA), C8B(H8BA,H8BB), C9B(H9BA,H9BB), C10B(H10C,H10D), C11B(H11C,H11D), C12B(H12D, H12C), C13B(H13C,H13D), C14B(H14C,H14D), C15B(H15C,H15D), C16B(H16C,H16D), C17B(H17C,H17D), C18B(H18D,H18C) 6.b Aromatic/amide H refined with riding coordinates: C19(H19), C22(H22), C19B(H19B), C22B(H22B), C19C(H19C) 6.c Idealised Me refined as rotating group: C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B, H24C), C20B(H20D,H20E,H20F), C21B(H21D,H21E,H21F), C23B(H23D,H23E,H23F), C25(H25A,H25B,H25C), C20C(H20G,H20H,H20I), C21C(H21G,H21H,H21I) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.76377(7) 0.47717(10) 0.42062(7) 0.01336(19) Uani 0.885(2) 1 d D U P A 1 O1 O 0.8189(3) 0.6047(5) 0.3214(3) 0.0173(10) Uani 0.885(2) 1 d D U P A 1 O2 O 0.7195(3) 0.7197(5) 0.3755(3) 0.0206(11) Uani 0.885(2) 1 d D U P A 1 O3 O 0.6723(3) 0.3211(5) 0.4598(3) 0.0195(10) Uani 0.885(2) 1 d D U P A 1 O4 O 0.7400(3) 0.2472(5) 0.3567(3) 0.0178(11) Uani 0.885(2) 1 d D U P A 1 O5 O 0.8670(3) 0.3321(5) 0.5156(3) 0.0185(10) Uani 0.885(2) 1 d D U P A 1 O6 O 0.7758(5) 0.4826(6) 0.5685(3) 0.0184(12) Uani 0.885(2) 1 d D U P A 1 O7 O 0.6628(5) 0.4871(6) 0.3097(5) 0.0228(16) Uani 0.357(9) 1 d D U P A 1 O8 O 0.8693(3) 0.6106(5) 0.4869(3) 0.0190(11) Uani 0.885(2) 1 d D U P A 1 N1 N 0.8689(3) 0.3589(6) 0.3607(3) 0.0175(12) Uani 0.885(2) 1 d D U P A 1 N2 N 0.6546(3) 0.5941(6) 0.4765(3) 0.0176(11) Uani 0.885(2) 1 d D U P A 1 N3 N 0.5767(4) 0.4864(6) 0.1976(4) 0.0158(13) Uani 0.357(9) 1 d D U P A 1 N4 N 0.8938(3) 0.8153(6) 0.5319(3) 0.0161(12) Uani 0.885(2) 1 d D . P A 1 C1 C 0.9192(4) 0.4571(7) 0.3444(4) 0.0184(14) Uani 0.885(2) 1 d D U P A 1 H1A H 0.954943 0.414871 0.320660 0.022 Uiso 0.885(2) 1 calc R U P A 1 H1B H 0.946936 0.496744 0.392701 0.022 Uiso 0.885(2) 1 calc R U P A 1 C2 C 0.8793(4) 0.5615(7) 0.2924(4) 0.0187(13) Uani 0.885(2) 1 d D U P A 1 H2A H 0.912814 0.634421 0.290722 0.022 Uiso 0.885(2) 1 calc R U P A 1 H2B H 0.860774 0.527154 0.240224 0.022 Uiso 0.885(2) 1 calc R U P A 1 C3 C 0.7768(4) 0.7036(7) 0.2738(4) 0.0178(13) Uani 0.885(2) 1 d D U P A 1 H3A H 0.735089 0.664400 0.236074 0.021 Uiso 0.885(2) 1 calc R U P A 1 H3B H 0.807872 0.750421 0.246219 0.021 Uiso 0.885(2) 1 calc R U P A 1 C4 C 0.7495(4) 0.7943(7) 0.3240(4) 0.0193(14) Uani 0.885(2) 1 d D U P A 1 H4A H 0.790204 0.848921 0.352843 0.023 Uiso 0.885(2) 1 calc R U P A 1 H4B H 0.711265 0.851425 0.293027 0.023 Uiso 0.885(2) 1 calc R U P A 1 C5 C 0.6664(4) 0.7924(8) 0.4031(5) 0.0226(15) Uani 0.885(2) 1 d D U P A 1 H5A H 0.638721 0.851306 0.363144 0.027 Uiso 0.885(2) 1 calc R U P A 1 H5B H 0.691209 0.844661 0.447835 0.027 Uiso 0.885(2) 1 calc R U P A 1 C6 C 0.6158(4) 0.6960(7) 0.4245(4) 0.0225(14) Uani 0.885(2) 1 d D U P A 1 H6B H 0.581943 0.742034 0.449051 0.027 Uiso 0.885(2) 1 calc R U P A 1 H6A H 0.585881 0.654778 0.377710 0.027 Uiso 0.885(2) 1 calc R U P A 1 C7 C 0.5986(5) 0.4976(7) 0.4861(5) 0.0178(19) Uani 0.885(2) 1 d D U P A 1 H7A H 0.560082 0.491788 0.437731 0.021 Uiso 0.885(2) 1 calc R U P A 1 H7B H 0.575150 0.530009 0.525318 0.021 Uiso 0.885(2) 1 calc R U P A 1 C8 C 0.6276(4) 0.3647(7) 0.5081(4) 0.0195(13) Uani 0.885(2) 1 d D U P A 1 H8A H 0.657057 0.365244 0.561533 0.023 Uiso 0.885(2) 1 calc R U P A 1 H8B H 0.586151 0.304182 0.504147 0.023 Uiso 0.885(2) 1 calc R U P A 1 C9 C 0.6404(4) 0.2165(7) 0.4107(4) 0.0195(14) Uani 0.885(2) 1 d D U P A 1 H9A H 0.603070 0.249898 0.366296 0.023 Uiso 0.885(2) 1 calc R U P A 1 H9B H 0.616441 0.154724 0.438235 0.023 Uiso 0.885(2) 1 calc R U P A 1 C10 C 0.7001(4) 0.1513(7) 0.3855(4) 0.0215(14) Uani 0.885(2) 1 d D U P A 1 H10A H 0.733001 0.105583 0.428752 0.026 Uiso 0.885(2) 1 calc R U P A 1 H10B H 0.679272 0.087188 0.345490 0.026 Uiso 0.885(2) 1 calc R U P A 1 C11 C 0.7767(4) 0.1956(7) 0.3032(4) 0.0185(14) Uani 0.885(2) 1 d D U P A 1 H11A H 0.740532 0.173002 0.255228 0.022 Uiso 0.885(2) 1 calc R U P A 1 H11B H 0.804058 0.116442 0.323957 0.022 Uiso 0.885(2) 1 calc R U P A 1 C12 C 0.8285(4) 0.2967(7) 0.2889(4) 0.0185(13) Uani 0.885(2) 1 d D U P A 1 H12A H 0.863848 0.256432 0.263934 0.022 Uiso 0.885(2) 1 calc R U P A 1 H12B H 0.800578 0.363131 0.254157 0.022 Uiso 0.885(2) 1 calc R U P A 1 C13 C 0.9124(4) 0.2610(7) 0.4127(4) 0.0201(14) Uani 0.885(2) 1 d D U P A 1 H13A H 0.957310 0.240573 0.396247 0.024 Uiso 0.885(2) 1 calc R U P A 1 H13B H 0.883389 0.180582 0.409678 0.024 Uiso 0.885(2) 1 calc R U P A 1 C14 C 0.9336(4) 0.3076(8) 0.4934(4) 0.0194(14) Uani 0.885(2) 1 d D U P A 1 H14B H 0.963204 0.241097 0.526735 0.023 Uiso 0.885(2) 1 calc R U P A 1 H14A H 0.963123 0.387630 0.497416 0.023 Uiso 0.885(2) 1 calc R U P A 1 C15 C 0.8839(4) 0.3572(8) 0.5962(3) 0.0209(15) Uani 0.885(2) 1 d D U P A 1 H15A H 0.916301 0.433611 0.608848 0.025 Uiso 0.885(2) 1 calc R U P A 1 H15B H 0.909432 0.281954 0.624691 0.025 Uiso 0.885(2) 1 calc R U P A 1 C16 C 0.8139(4) 0.3811(7) 0.6167(4) 0.0213(14) Uani 0.885(2) 1 d D U P A 1 H16A H 0.783752 0.301535 0.609356 0.026 Uiso 0.885(2) 1 calc R U P A 1 H16B H 0.823619 0.407243 0.670680 0.026 Uiso 0.885(2) 1 calc R U P A 1 C17 C 0.7343(4) 0.5621(7) 0.6064(4) 0.0208(14) Uani 0.885(2) 1 d D U P A 1 H17A H 0.767498 0.608598 0.649157 0.025 Uiso 0.885(2) 1 calc R U P A 1 H17B H 0.700314 0.508443 0.626855 0.025 Uiso 0.885(2) 1 calc R U P A 1 C18 C 0.6923(4) 0.6563(7) 0.5495(4) 0.0225(14) Uani 0.885(2) 1 d D U P A 1 H18B H 0.655330 0.699888 0.570936 0.027 Uiso 0.885(2) 1 calc R U P A 1 H18A H 0.726286 0.723167 0.539755 0.027 Uiso 0.885(2) 1 calc R U P A 1 C19 C 0.6239(6) 0.4306(11) 0.2521(6) 0.0174(19) Uani 0.528(9) 1 d D U P A 1 H19 H 0.629790 0.339835 0.248617 0.021 Uiso 0.528(9) 1 calc R U P A 1 C20 C 0.5313(7) 0.4157(11) 0.1334(6) 0.022(3) Uani 0.528(9) 1 d D U P A 1 H20A H 0.548430 0.433126 0.087911 0.033 Uiso 0.528(9) 1 calc R U P A 1 H20B H 0.480211 0.443512 0.124837 0.033 Uiso 0.528(9) 1 calc R U P A 1 H20C H 0.534858 0.322836 0.144428 0.033 Uiso 0.528(9) 1 calc R U P A 1 C21 C 0.5674(7) 0.6284(9) 0.1950(7) 0.024(3) Uani 0.528(9) 1 d D U P A 1 H21A H 0.520443 0.650814 0.205348 0.036 Uiso 0.528(9) 1 calc R U P A 1 H21B H 0.568259 0.660212 0.144490 0.036 Uiso 0.528(9) 1 calc R U P A 1 H21C H 0.607463 0.668421 0.233320 0.036 Uiso 0.528(9) 1 calc R U P A 1 C22 C 0.8840(4) 0.7278(7) 0.4785(4) 0.0177(14) Uani 0.885(2) 1 d D U P A 1 H22 H 0.888377 0.754225 0.429841 0.021 Uiso 0.885(2) 1 calc R U P A 1 C23 C 0.8893(4) 0.7852(7) 0.6091(3) 0.0196(15) Uani 0.885(2) 1 d D U P A 1 H23A H 0.928314 0.831061 0.645735 0.029 Uiso 0.885(2) 1 calc R U P A 1 H23B H 0.895081 0.691907 0.617842 0.029 Uiso 0.885(2) 1 calc R U P A 1 H23C H 0.841511 0.812631 0.615522 0.029 Uiso 0.885(2) 1 calc R U P A 1 C24 C 0.9055(4) 0.9504(7) 0.5161(4) 0.0229(16) Uani 0.885(2) 1 d D . P A 1 H24A H 0.911206 0.958741 0.464314 0.034 Uiso 0.885(2) 1 calc R U P A 1 H24B H 0.949850 0.981984 0.552299 0.034 Uiso 0.885(2) 1 calc R U P A 1 H24C H 0.863227 1.001595 0.521071 0.034 Uiso 0.885(2) 1 calc R U P A 1 I1 I 1.05691(3) 1.06349(5) 0.70066(3) 0.02036(14) Uani 0.8937(15) 1 d . . P B 1 I2 I 0.43069(6) 0.4502(5) 0.30028(5) 0.0342(8) Uani 0.552(6) 1 d . . P C 1 I3 I 0.71976(16) 0.4727(3) 0.09330(16) 0.0187(7) Uani 0.77(4) 1 d . . P D 1 U1B U 0.7643(5) 0.5134(7) 0.4192(6) 0.0086(11) Uani 0.115(2) 1 d D U P A 2 O1B O 0.720(2) 0.274(2) 0.373(2) 0.018(3) Uani 0.115(2) 1 d D U P A 2 O2B O 0.8194(17) 0.381(3) 0.3219(16) 0.018(3) Uani 0.115(2) 1 d D U P A 2 O3B O 0.740(2) 0.745(2) 0.356(2) 0.019(3) Uani 0.115(2) 1 d D U P A 2 O4B O 0.6742(17) 0.676(3) 0.462(2) 0.022(3) Uani 0.115(2) 1 d D U P A 2 O5B O 0.778(4) 0.506(6) 0.5681(13) 0.020(3) Uani 0.115(2) 1 d D U P A 2 O6B O 0.8667(15) 0.655(4) 0.5116(16) 0.018(3) Uani 0.115(2) 1 d D U P A 2 O7B O 0.660(4) 0.452(6) 0.313(4) 0.019(3) Uani 0.115(2) 1 d D U P A 2 O8B O 0.871(2) 0.379(4) 0.484(2) 0.018(3) Uani 0.115(2) 1 d . U P A 2 N1B N 0.6537(15) 0.401(4) 0.4744(18) 0.019(3) Uani 0.115(2) 1 d D U P A 2 N2B N 0.8694(15) 0.633(3) 0.3584(17) 0.017(3) Uani 0.115(2) 1 d D U P A 2 N3B N 0.578(4) 0.447(5) 0.197(3) 0.018(3) Uani 0.115(2) 1 d D U P A 2 N4B N 0.894(2) 0.178(3) 0.5297(19) 0.018(3) Uani 0.115(2) 1 d D U P A 2 C1B C 0.616(2) 0.301(4) 0.420(3) 0.019(3) Uani 0.115(2) 1 d D U P A 2 H1BA H 0.589344 0.343822 0.372126 0.022 Uiso 0.115(2) 1 calc R U P A 2 H1BB H 0.579326 0.256622 0.441300 0.022 Uiso 0.115(2) 1 calc R U P A 2 C2B C 0.667(3) 0.203(4) 0.402(3) 0.017(3) Uani 0.115(2) 1 d D U P A 2 H2BA H 0.691809 0.154085 0.448319 0.021 Uiso 0.115(2) 1 calc R U P A 2 H2BB H 0.640324 0.141078 0.363374 0.021 Uiso 0.115(2) 1 calc R U P A 2 C3B C 0.749(3) 0.194(4) 0.323(3) 0.020(3) Uani 0.115(2) 1 d D U P A 2 H3BA H 0.709990 0.138372 0.292072 0.024 Uiso 0.115(2) 1 calc R U P A 2 H3BB H 0.788756 0.137449 0.352554 0.024 Uiso 0.115(2) 1 calc R U P A 2 C4B C 0.778(3) 0.283(4) 0.274(2) 0.018(3) Uani 0.115(2) 1 d D U P A 2 H4BA H 0.810149 0.234897 0.247448 0.022 Uiso 0.115(2) 1 calc R U P A 2 H4BB H 0.737380 0.321783 0.234768 0.022 Uiso 0.115(2) 1 calc R U P A 2 C5B C 0.877(2) 0.431(4) 0.291(2) 0.017(3) Uani 0.115(2) 1 d D U P A 2 H5BA H 0.855698 0.466634 0.239980 0.021 Uiso 0.115(2) 1 calc R U P A 2 H5BB H 0.910487 0.359197 0.286150 0.021 Uiso 0.115(2) 1 calc R U P A 2 C6B C 0.919(2) 0.533(3) 0.341(2) 0.018(3) Uani 0.115(2) 1 d D U P A 2 H6BA H 0.948103 0.493622 0.389002 0.022 Uiso 0.115(2) 1 calc R U P A 2 H6BB H 0.954060 0.573912 0.315561 0.022 Uiso 0.115(2) 1 calc R U P A 2 C7B C 0.830(3) 0.695(4) 0.286(2) 0.018(3) Uani 0.115(2) 1 d D U P A 2 H7BB H 0.804391 0.628595 0.249868 0.021 Uiso 0.115(2) 1 calc R U P A 2 H7BA H 0.865965 0.739226 0.262991 0.021 Uiso 0.115(2) 1 calc R U P A 2 C8B C 0.776(3) 0.791(4) 0.301(3) 0.019(3) Uani 0.115(2) 1 d D U P A 2 H8BA H 0.802418 0.872235 0.319922 0.023 Uiso 0.115(2) 1 calc R U P A 2 H8BB H 0.739575 0.810199 0.253142 0.023 Uiso 0.115(2) 1 calc R U P A 2 C9B C 0.705(3) 0.846(4) 0.388(3) 0.020(3) Uani 0.115(2) 1 d D U P A 2 H9BA H 0.685348 0.912894 0.348954 0.024 Uiso 0.115(2) 1 calc R U P A 2 H9BB H 0.741209 0.888052 0.430621 0.024 Uiso 0.115(2) 1 calc R U P A 2 C10B C 0.645(2) 0.783(5) 0.415(3) 0.021(3) Uani 0.115(2) 1 d D U P A 2 H10C H 0.623539 0.846486 0.443744 0.025 Uiso 0.115(2) 1 calc R U P A 2 H10D H 0.606143 0.753719 0.370728 0.025 Uiso 0.115(2) 1 calc R U P A 2 C11B C 0.628(2) 0.635(4) 0.509(2) 0.020(3) Uani 0.115(2) 1 d D U P A 2 H11C H 0.586867 0.696263 0.505821 0.024 Uiso 0.115(2) 1 calc R U P A 2 H11D H 0.655555 0.624828 0.562358 0.024 Uiso 0.115(2) 1 calc R U P A 2 C12B C 0.600(3) 0.507(5) 0.474(5) 0.019(3) Uani 0.115(2) 1 d D U P A 2 H12D H 0.564020 0.475038 0.500703 0.023 Uiso 0.115(2) 1 calc R U P A 2 H12C H 0.573435 0.523384 0.420749 0.023 Uiso 0.115(2) 1 calc R U P A 2 C13B C 0.692(3) 0.337(4) 0.546(2) 0.021(3) Uani 0.115(2) 1 d D U P A 2 H13C H 0.727342 0.273412 0.536091 0.025 Uiso 0.115(2) 1 calc R U P A 2 H13D H 0.655694 0.289813 0.567092 0.025 Uiso 0.115(2) 1 calc R U P A 2 C14B C 0.732(3) 0.432(4) 0.604(3) 0.020(3) Uani 0.115(2) 1 d D U P A 2 H14C H 0.696592 0.489107 0.620615 0.024 Uiso 0.115(2) 1 calc R U P A 2 H14D H 0.761737 0.386297 0.649318 0.024 Uiso 0.115(2) 1 calc R U P A 2 C15B C 0.811(2) 0.613(5) 0.614(3) 0.020(3) Uani 0.115(2) 1 d D U P A 2 H15C H 0.821622 0.590321 0.668955 0.024 Uiso 0.115(2) 1 calc R U P A 2 H15D H 0.778128 0.689199 0.605055 0.024 Uiso 0.115(2) 1 calc R U P A 2 C16B C 0.881(2) 0.642(6) 0.5928(18) 0.019(4) Uani 0.115(2) 1 d D U P A 2 H16C H 0.901967 0.723699 0.617499 0.022 Uiso 0.115(2) 1 calc R U P A 2 H16D H 0.916331 0.571993 0.610595 0.022 Uiso 0.115(2) 1 calc R U P A 2 C17B C 0.933(2) 0.677(5) 0.4888(19) 0.018(3) Uani 0.115(2) 1 d D U P A 2 H17C H 0.959898 0.595068 0.489308 0.021 Uiso 0.115(2) 1 calc R U P A 2 H17D H 0.964824 0.738612 0.523968 0.021 Uiso 0.115(2) 1 calc R U P A 2 C18B C 0.912(3) 0.732(4) 0.4103(18) 0.017(4) Uani 0.115(2) 1 d D U P A 2 H18D H 0.881770 0.810755 0.409179 0.020 Uiso 0.115(2) 1 calc R U P A 2 H18C H 0.956343 0.755752 0.393965 0.020 Uiso 0.115(2) 1 calc R U P A 2 C19B C 0.616(4) 0.505(6) 0.257(3) 0.019(3) Uani 0.115(2) 1 d D U P A 2 H19B H 0.610656 0.596583 0.258890 0.023 Uiso 0.115(2) 1 calc R U P A 2 C20B C 0.525(4) 0.516(6) 0.136(4) 0.019(6) Uani 0.115(2) 1 d D U P A 2 H20D H 0.530526 0.485676 0.087035 0.028 Uiso 0.115(2) 1 calc R U P A 2 H20E H 0.535170 0.608691 0.141339 0.028 Uiso 0.115(2) 1 calc R U P A 2 H20F H 0.475418 0.498506 0.140471 0.028 Uiso 0.115(2) 1 calc R U P A 2 C21B C 0.577(5) 0.308(5) 0.185(4) 0.018(6) Uani 0.115(2) 1 d D U P A 2 H21D H 0.535406 0.269694 0.200882 0.027 Uiso 0.115(2) 1 calc R U P A 2 H21E H 0.622675 0.270216 0.214916 0.027 Uiso 0.115(2) 1 calc R U P A 2 H21F H 0.571296 0.289605 0.130974 0.027 Uiso 0.115(2) 1 calc R U P A 2 C22B C 0.883(3) 0.264(4) 0.480(3) 0.018(3) Uani 0.115(2) 1 d D U P A 2 H22B H 0.885066 0.234906 0.430986 0.021 Uiso 0.115(2) 1 calc R U P A 2 C23B C 0.892(3) 0.214(5) 0.607(2) 0.018(3) Uani 0.115(2) 1 d D U P A 2 H23D H 0.907398 0.140017 0.640813 0.027 Uiso 0.115(2) 1 calc R U P A 2 H23E H 0.841370 0.237536 0.606666 0.027 Uiso 0.115(2) 1 calc R U P A 2 H23F H 0.924356 0.287049 0.623904 0.027 Uiso 0.115(2) 1 calc R U P A 2 C25 C 0.907(3) 0.041(3) 0.517(2) 0.018(3) Uani 0.115(2) 1 d D U P A 2 H25A H 0.947931 0.008934 0.557361 0.027 Uiso 0.115(2) 1 calc R U P A 2 H25B H 0.918216 0.030188 0.467717 0.027 Uiso 0.115(2) 1 calc R U P A 2 H25C H 0.862589 -0.009102 0.517213 0.027 Uiso 0.115(2) 1 calc R U P A 2 I1B I 1.0582(2) 0.9417(4) 0.7014(2) 0.0175(11) Uani 0.1063(15) 1 d . . P B 2 I2B I 0.42744(6) 0.5236(3) 0.29959(6) 0.0145(5) Uani 0.448(6) 1 d . . P C 2 I3B I 0.7193(6) 0.505(5) 0.0921(6) 0.046(3) Uani 0.23(4) 1 d . . P D 2 O7C O 0.6628(5) 0.4871(6) 0.3097(5) 0.0228(16) Uani 0.528(9) 1 d . . P A 3 N3C N 0.5767(4) 0.4864(6) 0.1976(4) 0.0158(13) Uani 0.528(9) 1 d . . P A 3 C19C C 0.6197(12) 0.5408(17) 0.2575(11) 0.020(2) Uani 0.357(9) 1 d D U P A 3 H19C H 0.617066 0.632287 0.260440 0.024 Uiso 0.357(9) 1 calc R U P A 3 C20C C 0.5308(13) 0.5535(17) 0.1365(12) 0.018(4) Uani 0.357(9) 1 d D U P A 3 H20G H 0.549504 0.543793 0.091292 0.027 Uiso 0.357(9) 1 calc R U P A 3 H20H H 0.529946 0.645366 0.149446 0.027 Uiso 0.357(9) 1 calc R U P A 3 H20I H 0.481048 0.518219 0.126221 0.027 Uiso 0.357(9) 1 calc R U P A 3 C21C C 0.5731(15) 0.3394(15) 0.1956(12) 0.024(4) Uani 0.357(9) 1 d D U P A 3 H21G H 0.610776 0.304265 0.238293 0.035 Uiso 0.357(9) 1 calc R U P A 3 H21H H 0.581702 0.308302 0.147735 0.035 Uiso 0.357(9) 1 calc R U P A 3 H21I H 0.524627 0.311069 0.199384 0.035 Uiso 0.357(9) 1 calc R U P A 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.01031(17) 0.0226(5) 0.00759(17) -0.0014(3) 0.00296(12) -0.0017(3) O1 0.015(2) 0.026(2) 0.012(2) 0.0003(19) 0.0057(18) 0.0017(19) O2 0.019(3) 0.032(3) 0.013(2) -0.001(2) 0.0075(19) 0.003(2) O3 0.017(2) 0.029(3) 0.015(2) -0.0037(19) 0.0085(18) -0.005(2) O4 0.017(2) 0.024(2) 0.015(2) -0.0026(19) 0.0075(19) -0.003(2) O5 0.015(2) 0.032(3) 0.009(2) 0.003(2) 0.0032(19) -0.003(2) O6 0.014(2) 0.031(3) 0.011(2) -0.0012(19) 0.0053(18) -0.002(2) O7 0.016(2) 0.029(4) 0.019(2) 0.001(3) -0.003(2) 0.003(3) O8 0.016(2) 0.027(3) 0.014(2) -0.001(2) 0.0037(19) -0.002(2) N1 0.015(3) 0.026(3) 0.012(2) 0.001(2) 0.005(2) 0.002(2) N2 0.015(2) 0.026(3) 0.012(2) -0.003(2) 0.005(2) -0.003(2) N3 0.013(2) 0.018(3) 0.015(2) -0.003(3) 0.001(2) 0.000(3) N4 0.013(3) 0.024(3) 0.011(3) 0.001(2) 0.003(2) -0.002(2) C1 0.017(3) 0.024(3) 0.015(3) 0.002(3) 0.005(2) -0.002(3) C2 0.019(3) 0.027(3) 0.013(3) 0.002(2) 0.009(2) 0.000(3) C3 0.017(3) 0.024(3) 0.012(3) 0.001(2) 0.004(2) -0.002(3) C4 0.017(3) 0.028(3) 0.014(3) 0.003(3) 0.005(2) -0.004(3) C5 0.023(3) 0.029(3) 0.019(3) -0.002(3) 0.009(3) 0.003(3) C6 0.021(3) 0.028(3) 0.019(3) -0.004(3) 0.008(3) 0.001(3) C7 0.012(3) 0.030(3) 0.014(4) -0.002(3) 0.008(3) -0.006(3) C8 0.016(3) 0.031(3) 0.014(3) -0.001(3) 0.008(2) -0.005(3) C9 0.020(3) 0.023(3) 0.017(3) 0.000(3) 0.006(3) -0.004(3) C10 0.024(3) 0.021(3) 0.021(3) 0.002(3) 0.009(3) 0.000(3) C11 0.019(3) 0.025(3) 0.012(3) -0.005(3) 0.007(3) -0.002(3) C12 0.019(3) 0.025(3) 0.012(3) -0.002(2) 0.005(2) 0.001(3) C13 0.016(3) 0.029(3) 0.015(3) 0.003(3) 0.004(3) 0.004(3) C14 0.013(3) 0.034(3) 0.012(3) 0.004(3) 0.004(2) 0.000(3) C15 0.018(3) 0.034(4) 0.008(3) 0.003(3) -0.001(3) 0.001(3) C16 0.018(3) 0.033(4) 0.012(3) 0.002(3) 0.001(2) -0.003(3) C17 0.016(3) 0.037(3) 0.012(3) -0.006(3) 0.007(2) -0.006(3) C18 0.017(3) 0.034(3) 0.018(3) -0.008(3) 0.007(3) -0.002(3) C19 0.016(4) 0.020(4) 0.016(4) -0.004(3) 0.003(3) 0.002(3) C20 0.022(5) 0.022(6) 0.018(5) -0.002(4) -0.003(4) -0.002(5) C21 0.020(5) 0.027(5) 0.022(5) -0.003(4) 0.001(4) 0.003(4) C22 0.010(3) 0.033(4) 0.012(3) 0.004(3) 0.006(2) -0.003(3) C23 0.019(4) 0.034(4) 0.007(3) -0.004(3) 0.005(3) -0.001(3) C24 0.023(4) 0.025(4) 0.021(4) 0.002(3) 0.007(3) -0.006(3) I1 0.0182(2) 0.0296(3) 0.0143(2) -0.00222(18) 0.00594(18) -0.00430(19) I2 0.0169(5) 0.073(2) 0.0136(4) -0.0056(6) 0.0052(3) -0.0150(6) I3 0.0201(6) 0.0244(14) 0.0119(7) -0.0023(6) 0.0046(5) -0.0015(5) U1B 0.0051(12) 0.013(3) 0.0091(13) -0.001(2) 0.0039(9) 0.001(2) O1B 0.019(5) 0.021(5) 0.015(5) -0.002(5) 0.008(5) -0.002(5) O2B 0.018(5) 0.024(5) 0.013(5) -0.001(5) 0.005(5) -0.002(5) O3B 0.018(5) 0.026(5) 0.014(5) 0.000(5) 0.006(5) 0.001(5) O4B 0.019(5) 0.031(5) 0.017(5) -0.004(4) 0.008(4) 0.001(4) O5B 0.016(5) 0.032(5) 0.012(5) -0.001(5) 0.004(5) -0.004(5) O6B 0.012(6) 0.029(6) 0.012(6) -0.001(6) 0.005(6) -0.001(6) O7B 0.016(5) 0.022(6) 0.016(5) -0.004(6) 0.000(5) 0.001(6) O8B 0.013(5) 0.032(6) 0.010(5) 0.004(5) 0.002(5) -0.001(5) N1B 0.015(4) 0.030(4) 0.013(4) -0.002(4) 0.006(4) -0.004(4) N2B 0.014(5) 0.025(5) 0.013(5) 0.002(5) 0.008(5) -0.001(5) N3B 0.015(5) 0.021(5) 0.015(5) -0.003(5) 0.003(5) 0.002(5) N4B 0.012(5) 0.031(5) 0.011(5) 0.003(5) 0.005(5) 0.001(5) C1B 0.016(5) 0.028(5) 0.015(5) -0.001(5) 0.009(5) -0.005(5) C2B 0.017(5) 0.022(5) 0.015(5) -0.001(5) 0.009(5) -0.004(5) C3B 0.020(5) 0.024(5) 0.016(5) -0.001(5) 0.006(5) -0.001(5) C4B 0.019(5) 0.024(5) 0.013(5) -0.002(5) 0.006(5) -0.001(5) C5B 0.016(5) 0.024(5) 0.013(5) 0.000(5) 0.007(4) 0.000(5) C6B 0.016(5) 0.025(5) 0.014(5) 0.001(5) 0.006(5) 0.000(5) C7B 0.017(5) 0.025(5) 0.013(5) 0.002(5) 0.006(5) 0.000(5) C8B 0.018(6) 0.026(6) 0.014(6) 0.002(6) 0.004(6) 0.000(6) C9B 0.018(5) 0.028(5) 0.016(5) -0.001(5) 0.006(5) 0.002(5) C10B 0.019(5) 0.029(5) 0.016(5) -0.003(5) 0.008(5) 0.003(5) C11B 0.017(5) 0.029(5) 0.016(5) -0.003(5) 0.007(4) -0.002(5) C12B 0.015(5) 0.029(5) 0.014(5) -0.002(5) 0.007(5) -0.003(5) C13B 0.017(6) 0.032(6) 0.014(6) -0.002(5) 0.006(5) -0.005(5) C14B 0.016(5) 0.032(5) 0.012(5) -0.001(5) 0.004(5) -0.005(5) C15B 0.016(6) 0.032(6) 0.012(6) -0.004(6) 0.003(5) -0.004(6) C16B 0.015(6) 0.028(6) 0.012(6) -0.002(6) 0.003(6) -0.003(6) C17B 0.013(6) 0.028(6) 0.013(6) -0.001(6) 0.005(6) 0.000(6) C18B 0.013(7) 0.028(7) 0.011(7) 0.002(6) 0.005(6) -0.001(6) C19B 0.017(4) 0.023(5) 0.018(4) -0.002(4) 0.003(4) 0.001(4) C20B 0.016(9) 0.023(10) 0.016(9) -0.002(10) 0.002(9) 0.002(10) C21B 0.019(9) 0.018(10) 0.016(9) -0.003(9) 0.002(9) 0.001(9) C22B 0.012(5) 0.031(5) 0.011(5) 0.003(5) 0.005(5) 0.001(5) C23B 0.012(5) 0.031(6) 0.011(5) 0.003(5) 0.005(5) 0.001(5) C25 0.012(5) 0.031(6) 0.011(5) 0.003(5) 0.005(5) 0.002(5) I1B 0.021(2) 0.017(2) 0.017(2) 0.0000(14) 0.0092(15) 0.0032(14) I2B 0.0148(5) 0.0145(13) 0.0148(5) -0.0005(4) 0.0051(3) -0.0029(4) I3B 0.031(2) 0.086(11) 0.026(2) 0.016(4) 0.0154(18) 0.011(4) O7C 0.016(2) 0.029(4) 0.019(2) 0.001(3) -0.003(2) 0.003(3) N3C 0.013(2) 0.018(3) 0.015(2) -0.003(3) 0.001(2) 0.000(3) C19C 0.017(4) 0.024(4) 0.018(4) -0.006(4) 0.002(4) 0.003(4) C20C 0.014(7) 0.024(8) 0.013(6) 0.000(7) -0.003(5) 0.005(7) C21C 0.024(7) 0.021(8) 0.020(7) -0.001(7) -0.004(7) 0.001(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O1 2.655(5) . ? U1 O2 2.705(5) . ? U1 O3 2.593(5) . ? U1 O4 2.637(5) . ? U1 O5 2.705(5) . ? U1 O6 2.646(5) . ? U1 O7 2.399(7) . ? U1 O8 2.469(5) . ? U1 N1 2.779(6) . ? U1 N2 2.794(6) . ? O1 C2 1.443(7) . ? O1 C3 1.442(7) . ? O2 C4 1.437(7) . ? O2 C5 1.442(7) . ? O3 C8 1.437(7) . ? O3 C9 1.435(7) . ? O4 C10 1.424(7) . ? O4 C11 1.433(7) . ? O5 C14 1.439(7) . ? O5 C15 1.443(7) . ? O6 C16 1.438(9) . ? O6 C17 1.428(9) . ? O7 C19 1.260(11) . ? O8 C22 1.262(8) . ? N1 C1 1.472(8) . ? N1 C12 1.482(8) . ? N1 C13 1.484(8) . ? N2 C6 1.480(8) . ? N2 C7 1.495(9) . ? N2 C18 1.485(8) . ? N3 C19 1.289(10) . ? N3 C20 1.456(10) . ? N3 C21 1.479(10) . ? N4 C22 1.307(8) . ? N4 C23 1.465(7) . ? N4 C24 1.455(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C1 C2 1.506(8) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.490(8) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C5 C6 1.500(9) . ? C6 H6B 0.9900 . ? C6 H6A 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.497(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C9 C10 1.482(8) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C11 C12 1.498(8) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 C14 1.500(8) . ? C14 H14B 0.9900 . ? C14 H14A 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 C16 1.483(8) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C17 C18 1.495(9) . ? C18 H18B 0.9900 . ? C18 H18A 0.9900 . ? C19 H19 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22 0.9500 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? U1B O1B 2.672(15) . ? U1B O2B 2.651(14) . ? U1B O3B 2.647(15) . ? U1B O4B 2.646(15) . ? U1B O5B 2.658(15) . ? U1B O6B 2.656(15) . ? U1B O7B 2.47(6) . ? U1B O8B 2.48(4) . ? U1B N1B 2.789(17) . ? U1B N2B 2.793(17) . ? O1B C2B 1.447(15) . ? O1B C3B 1.444(15) . ? O2B C4B 1.437(15) . ? O2B C5B 1.439(15) . ? O3B C8B 1.432(15) . ? O3B C9B 1.431(15) . ? O4B C10B 1.428(15) . ? O4B C11B 1.432(15) . ? O5B C14B 1.438(15) . ? O5B C15B 1.439(15) . ? O6B C16B 1.440(15) . ? O6B C17B 1.432(15) . ? O7B C19B 1.262(19) . ? O8B C22B 1.22(6) . ? N1B C1B 1.486(16) . ? N1B C12B 1.488(16) . ? N1B C13B 1.485(16) . ? N2B C6B 1.486(15) . ? N2B C7B 1.484(16) . ? N2B C18B 1.483(16) . ? N3B C19B 1.295(19) . ? N3B C20B 1.460(16) . ? N3B C21B 1.458(16) . ? N4B C22B 1.25(4) . ? N4B C23B 1.461(16) . ? N4B C25 1.467(16) . ? C1B H1BA 0.9900 . ? C1B H1BB 0.9900 . ? C1B C2B 1.495(16) . ? C2B H2BA 0.9900 . ? C2B H2BB 0.9900 . ? C3B H3BA 0.9900 . ? C3B H3BB 0.9900 . ? C3B C4B 1.486(16) . ? C4B H4BA 0.9900 . ? C4B H4BB 0.9900 . ? C5B H5BA 0.9900 . ? C5B H5BB 0.9900 . ? C5B C6B 1.488(16) . ? C6B H6BA 0.9900 . ? C6B H6BB 0.9900 . ? C7B H7BB 0.9900 . ? C7B H7BA 0.9900 . ? C7B C8B 1.495(16) . ? C8B H8BA 0.9900 . ? C8B H8BB 0.9900 . ? C9B H9BA 0.9900 . ? C9B H9BB 0.9900 . ? C9B C10B 1.499(16) . ? C10B H10C 0.9900 . ? C10B H10D 0.9900 . ? C11B H11C 0.9900 . ? C11B H11D 0.9900 . ? C11B C12B 1.494(16) . ? C12B H12D 0.9900 . ? C12B H12C 0.9900 . ? C13B H13C 0.9900 . ? C13B H13D 0.9900 . ? C13B C14B 1.493(16) . ? C14B H14C 0.9900 . ? C14B H14D 0.9900 . ? C15B H15C 0.9900 . ? C15B H15D 0.9900 . ? C15B C16B 1.492(16) . ? C16B H16C 0.9900 . ? C16B H16D 0.9900 . ? C17B H17C 0.9900 . ? C17B H17D 0.9900 . ? C17B C18B 1.494(16) . ? C18B H18D 0.9900 . ? C18B H18C 0.9900 . ? C19B H19B 0.9500 . ? C20B H20D 0.9800 . ? C20B H20E 0.9800 . ? C20B H20F 0.9800 . ? C21B H21D 0.9800 . ? C21B H21E 0.9800 . ? C21B H21F 0.9800 . ? C22B H22B 0.9500 . ? C23B H23D 0.9800 . ? C23B H23E 0.9800 . ? C23B H23F 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? O7C C19C 1.217(18) . ? N3C C19C 1.310(16) . ? N3C C20C 1.406(15) . ? N3C C21C 1.522(16) . ? C19C H19C 0.9500 . ? C20C H20G 0.9800 . ? C20C H20H 0.9800 . ? C20C H20I 0.9800 . ? C21C H21G 0.9800 . ? C21C H21H 0.9800 . ? C21C H21I 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 U1 O2 58.42(15) . . ? O1 U1 O5 111.58(15) . . ? O1 U1 N1 60.58(16) . . ? O1 U1 N2 119.07(16) . . ? O2 U1 N1 119.00(16) . . ? O2 U1 N2 60.67(16) . . ? O3 U1 O1 154.28(16) . . ? O3 U1 O2 119.08(17) . . ? O3 U1 O4 60.62(15) . . ? O3 U1 O5 84.21(16) . . ? O3 U1 O6 67.85(18) . . ? O3 U1 N1 115.17(17) . . ? O3 U1 N2 64.25(17) . . ? O4 U1 O1 101.54(16) . . ? O4 U1 O2 134.27(17) . . ? O4 U1 O5 78.20(16) . . ? O4 U1 O6 115.44(18) . . ? O4 U1 N1 59.15(16) . . ? O4 U1 N2 119.56(16) . . ? O5 U1 O2 145.59(17) . . ? O5 U1 N1 62.47(15) . . ? O5 U1 N2 118.97(16) . . ? O6 U1 O1 137.37(18) . . ? O6 U1 O2 103.3(2) . . ? O6 U1 O5 60.0(2) . . ? O6 U1 N1 121.7(2) . . ? O6 U1 N2 60.0(2) . . ? O7 U1 O1 76.7(2) . . ? O7 U1 O2 65.61(19) . . ? O7 U1 O3 79.5(2) . . ? O7 U1 O4 70.0(2) . . ? O7 U1 O5 148.2(2) . . ? O7 U1 O6 134.4(3) . . ? O7 U1 O8 139.1(2) . . ? O7 U1 N1 100.4(3) . . ? O7 U1 N2 77.7(3) . . ? O8 U1 O1 69.39(16) . . ? O8 U1 O2 77.18(17) . . ? O8 U1 O3 136.33(17) . . ? O8 U1 O4 138.19(17) . . ? O8 U1 O5 68.81(17) . . ? O8 U1 O6 69.0(2) . . ? O8 U1 N1 82.61(17) . . ? O8 U1 N2 99.03(17) . . ? N1 U1 N2 178.11(17) . . ? C2 O1 U1 125.3(4) . . ? C3 O1 U1 120.7(4) . . ? C3 O1 C2 111.4(5) . . ? C4 O2 U1 123.7(4) . . ? C4 O2 C5 111.8(5) . . ? C5 O2 U1 124.5(4) . . ? C8 O3 U1 120.6(4) . . ? C9 O3 U1 120.1(4) . . ? C9 O3 C8 113.6(5) . . ? C10 O4 U1 120.8(4) . . ? C10 O4 C11 112.6(5) . . ? C11 O4 U1 125.4(4) . . ? C14 O5 U1 117.2(4) . . ? C14 O5 C15 109.6(5) . . ? C15 O5 U1 119.2(4) . . ? C16 O6 U1 120.4(5) . . ? C17 O6 U1 126.1(5) . . ? C17 O6 C16 112.1(5) . . ? C19 O7 U1 148.2(7) . . ? C22 O8 U1 130.8(5) . . ? C1 N1 U1 109.7(4) . . ? C1 N1 C12 109.6(5) . . ? C1 N1 C13 108.6(5) . . ? C12 N1 U1 106.2(4) . . ? C12 N1 C13 110.1(5) . . ? C13 N1 U1 112.6(4) . . ? C6 N2 U1 111.5(4) . . ? C6 N2 C7 107.5(5) . . ? C6 N2 C18 108.1(6) . . ? C7 N2 U1 111.2(4) . . ? C18 N2 U1 106.6(4) . . ? C18 N2 C7 112.1(6) . . ? C19 N3 C20 122.8(8) . . ? C19 N3 C21 121.5(8) . . ? C20 N3 C21 115.7(7) . . ? C22 N4 C23 122.4(6) . . ? C22 N4 C24 121.2(6) . . ? C24 N4 C23 116.2(6) . . ? N1 C1 H1A 109.2 . . ? N1 C1 H1B 109.2 . . ? N1 C1 C2 112.1(6) . . ? H1A C1 H1B 107.9 . . ? C2 C1 H1A 109.2 . . ? C2 C1 H1B 109.2 . . ? O1 C2 C1 107.8(5) . . ? O1 C2 H2A 110.1 . . ? O1 C2 H2B 110.1 . . ? C1 C2 H2A 110.1 . . ? C1 C2 H2B 110.1 . . ? H2A C2 H2B 108.5 . . ? O1 C3 H3A 110.2 . . ? O1 C3 H3B 110.2 . . ? O1 C3 C4 107.5(5) . . ? H3A C3 H3B 108.5 . . ? C4 C3 H3A 110.2 . . ? C4 C3 H3B 110.2 . . ? O2 C4 C3 108.5(6) . . ? O2 C4 H4A 110.0 . . ? O2 C4 H4B 110.0 . . ? C3 C4 H4A 110.0 . . ? C3 C4 H4B 110.0 . . ? H4A C4 H4B 108.4 . . ? O2 C5 H5A 110.4 . . ? O2 C5 H5B 110.4 . . ? O2 C5 C6 106.8(6) . . ? H5A C5 H5B 108.6 . . ? C6 C5 H5A 110.4 . . ? C6 C5 H5B 110.4 . . ? N2 C6 C5 113.3(6) . . ? N2 C6 H6B 108.9 . . ? N2 C6 H6A 108.9 . . ? C5 C6 H6B 108.9 . . ? C5 C6 H6A 108.9 . . ? H6B C6 H6A 107.7 . . ? N2 C7 H7A 108.5 . . ? N2 C7 H7B 108.5 . . ? N2 C7 C8 115.0(7) . . ? H7A C7 H7B 107.5 . . ? C8 C7 H7A 108.5 . . ? C8 C7 H7B 108.5 . . ? O3 C8 C7 110.9(6) . . ? O3 C8 H8A 109.5 . . ? O3 C8 H8B 109.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? O3 C9 H9A 110.2 . . ? O3 C9 H9B 110.2 . . ? O3 C9 C10 107.8(6) . . ? H9A C9 H9B 108.5 . . ? C10 C9 H9A 110.2 . . ? C10 C9 H9B 110.2 . . ? O4 C10 C9 108.2(6) . . ? O4 C10 H10A 110.1 . . ? O4 C10 H10B 110.1 . . ? C9 C10 H10A 110.1 . . ? C9 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? O4 C11 H11A 110.1 . . ? O4 C11 H11B 110.1 . . ? O4 C11 C12 107.9(5) . . ? H11A C11 H11B 108.4 . . ? C12 C11 H11A 110.1 . . ? C12 C11 H11B 110.1 . . ? N1 C12 C11 111.2(5) . . ? N1 C12 H12A 109.4 . . ? N1 C12 H12B 109.4 . . ? C11 C12 H12A 109.4 . . ? C11 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? N1 C13 H13A 109.2 . . ? N1 C13 H13B 109.2 . . ? N1 C13 C14 111.9(6) . . ? H13A C13 H13B 107.9 . . ? C14 C13 H13A 109.2 . . ? C14 C13 H13B 109.2 . . ? O5 C14 C13 107.4(5) . . ? O5 C14 H14B 110.2 . . ? O5 C14 H14A 110.2 . . ? C13 C14 H14B 110.2 . . ? C13 C14 H14A 110.2 . . ? H14B C14 H14A 108.5 . . ? O5 C15 H15A 110.1 . . ? O5 C15 H15B 110.1 . . ? O5 C15 C16 107.8(5) . . ? H15A C15 H15B 108.5 . . ? C16 C15 H15A 110.1 . . ? C16 C15 H15B 110.1 . . ? O6 C16 C15 107.9(6) . . ? O6 C16 H16A 110.1 . . ? O6 C16 H16B 110.1 . . ? C15 C16 H16A 110.1 . . ? C15 C16 H16B 110.1 . . ? H16A C16 H16B 108.4 . . ? O6 C17 H17A 110.2 . . ? O6 C17 H17B 110.2 . . ? O6 C17 C18 107.4(6) . . ? H17A C17 H17B 108.5 . . ? C18 C17 H17A 110.2 . . ? C18 C17 H17B 110.2 . . ? N2 C18 C17 112.8(6) . . ? N2 C18 H18B 109.0 . . ? N2 C18 H18A 109.0 . . ? C17 C18 H18B 109.0 . . ? C17 C18 H18A 109.0 . . ? H18B C18 H18A 107.8 . . ? O7 C19 N3 125.2(10) . . ? O7 C19 H19 117.4 . . ? N3 C19 H19 117.4 . . ? N3 C20 H20A 109.5 . . ? N3 C20 H20B 109.5 . . ? N3 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 H21A 109.5 . . ? N3 C21 H21B 109.5 . . ? N3 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O8 C22 N4 124.6(6) . . ? O8 C22 H22 117.7 . . ? N4 C22 H22 117.7 . . ? N4 C23 H23A 109.5 . . ? N4 C23 H23B 109.5 . . ? N4 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N4 C24 H24A 109.5 . . ? N4 C24 H24B 109.5 . . ? N4 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O1B U1B N1B 61.8(12) . . ? O1B U1B N2B 118.7(11) . . ? O2B U1B O1B 57.1(11) . . ? O2B U1B O5B 135.6(19) . . ? O2B U1B O6B 111.3(11) . . ? O2B U1B N1B 118.9(11) . . ? O2B U1B N2B 61.7(10) . . ? O3B U1B O1B 134.0(14) . . ? O3B U1B O2B 103.4(12) . . ? O3B U1B O5B 115.5(17) . . ? O3B U1B O6B 78.1(13) . . ? O3B U1B N1B 117.9(13) . . ? O3B U1B N2B 59.3(11) . . ? O4B U1B O1B 120.5(13) . . ? O4B U1B O2B 156.3(12) . . ? O4B U1B O3B 60.0(11) . . ? O4B U1B O5B 67.6(19) . . ? O4B U1B O6B 83.1(12) . . ? O4B U1B N1B 64.0(12) . . ? O4B U1B N2B 114.2(11) . . ? O5B U1B O1B 103.5(14) . . ? O5B U1B N1B 60.4(14) . . ? O5B U1B N2B 121.6(13) . . ? O6B U1B O1B 145.7(14) . . ? O6B U1B O5B 60.3(13) . . ? O6B U1B N1B 119.4(10) . . ? O6B U1B N2B 62.1(10) . . ? O7B U1B O1B 52.9(17) . . ? O7B U1B O2B 73(2) . . ? O7B U1B O3B 82.7(17) . . ? O7B U1B O4B 87(2) . . ? O7B U1B O5B 130(2) . . ? O7B U1B O6B 160.8(16) . . ? O7B U1B O8B 128.2(19) . . ? O7B U1B N1B 70(2) . . ? O7B U1B N2B 108(2) . . ? O8B U1B O1B 77.2(14) . . ? O8B U1B O2B 67.8(13) . . ? O8B U1B O3B 138.3(14) . . ? O8B U1B O4B 135.8(13) . . ? O8B U1B O5B 69(2) . . ? O8B U1B O6B 68.9(14) . . ? O8B U1B N1B 100.6(13) . . ? O8B U1B N2B 82.5(13) . . ? N1B U1B N2B 176.9(11) . . ? C2B O1B U1B 123(2) . . ? C3B O1B U1B 127(2) . . ? C3B O1B C2B 109.9(15) . . ? C4B O2B U1B 122(2) . . ? C4B O2B C5B 111.0(15) . . ? C5B O2B U1B 123(2) . . ? C8B O3B U1B 123(2) . . ? C9B O3B U1B 122(2) . . ? C9B O3B C8B 112.7(15) . . ? C10B O4B U1B 120(3) . . ? C10B O4B C11B 113.0(16) . . ? C11B O4B U1B 122(2) . . ? C14B O5B U1B 125(3) . . ? C14B O5B C15B 111.5(16) . . ? C15B O5B U1B 119(3) . . ? C16B O6B U1B 121(2) . . ? C17B O6B U1B 117(3) . . ? C17B O6B C16B 111.7(15) . . ? C19B O7B U1B 139(5) . . ? C22B O8B U1B 132(4) . . ? C1B N1B U1B 109(2) . . ? C1B N1B C12B 107.7(16) . . ? C12B N1B U1B 105(4) . . ? C13B N1B U1B 105(2) . . ? C13B N1B C1B 109(3) . . ? C13B N1B C12B 121(5) . . ? C6B N2B U1B 109(2) . . ? C7B N2B U1B 108(2) . . ? C7B N2B C6B 108.1(16) . . ? C18B N2B U1B 112(2) . . ? C18B N2B C6B 110(3) . . ? C18B N2B C7B 109(3) . . ? C19B N3B C20B 122(2) . . ? C19B N3B C21B 125(3) . . ? C21B N3B C20B 112.8(19) . . ? C22B N4B C23B 118(3) . . ? C22B N4B C25 125(3) . . ? C23B N4B C25 116.3(19) . . ? N1B C1B H1BA 108.9 . . ? N1B C1B H1BB 108.9 . . ? N1B C1B C2B 113(4) . . ? H1BA C1B H1BB 107.8 . . ? C2B C1B H1BA 108.9 . . ? C2B C1B H1BB 108.9 . . ? O1B C2B C1B 106(4) . . ? O1B C2B H2BA 110.5 . . ? O1B C2B H2BB 110.5 . . ? C1B C2B H2BA 110.5 . . ? C1B C2B H2BB 110.5 . . ? H2BA C2B H2BB 108.7 . . ? O1B C3B H3BA 110.4 . . ? O1B C3B H3BB 110.4 . . ? O1B C3B C4B 106(3) . . ? H3BA C3B H3BB 108.6 . . ? C4B C3B H3BA 110.4 . . ? C4B C3B H3BB 110.4 . . ? O2B C4B C3B 107(3) . . ? O2B C4B H4BA 110.3 . . ? O2B C4B H4BB 110.3 . . ? C3B C4B H4BA 110.3 . . ? C3B C4B H4BB 110.3 . . ? H4BA C4B H4BB 108.6 . . ? O2B C5B H5BA 109.5 . . ? O2B C5B H5BB 109.5 . . ? O2B C5B C6B 111(3) . . ? H5BA C5B H5BB 108.0 . . ? C6B C5B H5BA 109.5 . . ? C6B C5B H5BB 109.5 . . ? N2B C6B C5B 111(3) . . ? N2B C6B H6BA 109.5 . . ? N2B C6B H6BB 109.5 . . ? C5B C6B H6BA 109.5 . . ? C5B C6B H6BB 109.5 . . ? H6BA C6B H6BB 108.1 . . ? N2B C7B H7BB 109.8 . . ? N2B C7B H7BA 109.8 . . ? N2B C7B C8B 109(3) . . ? H7BB C7B H7BA 108.3 . . ? C8B C7B H7BB 109.8 . . ? C8B C7B H7BA 109.8 . . ? O3B C8B C7B 112(4) . . ? O3B C8B H8BA 109.1 . . ? O3B C8B H8BB 109.1 . . ? C7B C8B H8BA 109.1 . . ? C7B C8B H8BB 109.1 . . ? H8BA C8B H8BB 107.9 . . ? O3B C9B H9BA 110.6 . . ? O3B C9B H9BB 110.6 . . ? O3B C9B C10B 106(4) . . ? H9BA C9B H9BB 108.7 . . ? C10B C9B H9BA 110.6 . . ? C10B C9B H9BB 110.6 . . ? O4B C10B C9B 109(3) . . ? O4B C10B H10C 109.8 . . ? O4B C10B H10D 109.8 . . ? C9B C10B H10C 109.8 . . ? C9B C10B H10D 109.8 . . ? H10C C10B H10D 108.3 . . ? O4B C11B H11C 111.3 . . ? O4B C11B H11D 111.3 . . ? O4B C11B C12B 102(5) . . ? H11C C11B H11D 109.2 . . ? C12B C11B H11C 111.3 . . ? C12B C11B H11D 111.3 . . ? N1B C12B C11B 119(5) . . ? N1B C12B H12D 107.5 . . ? N1B C12B H12C 107.5 . . ? C11B C12B H12D 107.5 . . ? C11B C12B H12C 107.5 . . ? H12D C12B H12C 107.0 . . ? N1B C13B H13C 109.2 . . ? N1B C13B H13D 109.2 . . ? N1B C13B C14B 112(4) . . ? H13C C13B H13D 107.9 . . ? C14B C13B H13C 109.2 . . ? C14B C13B H13D 109.2 . . ? O5B C14B C13B 106(4) . . ? O5B C14B H14C 110.5 . . ? O5B C14B H14D 110.5 . . ? C13B C14B H14C 110.5 . . ? C13B C14B H14D 110.5 . . ? H14C C14B H14D 108.7 . . ? O5B C15B H15C 110.5 . . ? O5B C15B H15D 110.5 . . ? O5B C15B C16B 106(4) . . ? H15C C15B H15D 108.6 . . ? C16B C15B H15C 110.5 . . ? C16B C15B H15D 110.5 . . ? O6B C16B C15B 110(3) . . ? O6B C16B H16C 109.6 . . ? O6B C16B H16D 109.6 . . ? C15B C16B H16C 109.6 . . ? C15B C16B H16D 109.6 . . ? H16C C16B H16D 108.1 . . ? O6B C17B H17C 110.2 . . ? O6B C17B H17D 110.2 . . ? O6B C17B C18B 107(3) . . ? H17C C17B H17D 108.5 . . ? C18B C17B H17C 110.2 . . ? C18B C17B H17D 110.2 . . ? N2B C18B C17B 108(3) . . ? N2B C18B H18D 110.0 . . ? N2B C18B H18C 110.0 . . ? C17B C18B H18D 110.0 . . ? C17B C18B H18C 110.0 . . ? H18D C18B H18C 108.4 . . ? O7B C19B N3B 126(5) . . ? O7B C19B H19B 117.0 . . ? N3B C19B H19B 117.0 . . ? N3B C20B H20D 109.5 . . ? N3B C20B H20E 109.5 . . ? N3B C20B H20F 109.5 . . ? H20D C20B H20E 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? N3B C21B H21D 109.5 . . ? N3B C21B H21E 109.5 . . ? N3B C21B H21F 109.5 . . ? H21D C21B H21E 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? O8B C22B N4B 130(5) . . ? O8B C22B H22B 114.8 . . ? N4B C22B H22B 114.8 . . ? N4B C23B H23D 109.5 . . ? N4B C23B H23E 109.5 . . ? N4B C23B H23F 109.5 . . ? H23D C23B H23E 109.5 . . ? H23D C23B H23F 109.5 . . ? H23E C23B H23F 109.5 . . ? N4B C25 H25A 109.5 . . ? N4B C25 H25B 109.5 . . ? N4B C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C19C N3C C20C 124.9(11) . . ? C19C N3C C21C 117.6(11) . . ? C20C N3C C21C 117.4(10) . . ? O7C C19C N3C 127.2(14) . . ? O7C C19C H19C 116.4 . . ? N3C C19C H19C 116.4 . . ? N3C C20C H20G 109.5 . . ? N3C C20C H20H 109.5 . . ? N3C C20C H20I 109.5 . . ? H20G C20C H20H 109.5 . . ? H20G C20C H20I 109.5 . . ? H20H C20C H20I 109.5 . . ? N3C C21C H21G 109.5 . . ? N3C C21C H21H 109.5 . . ? N3C C21C H21I 109.5 . . ? H21G C21C H21H 109.5 . . ? H21G C21C H21I 109.5 . . ? H21H C21C H21I 109.5 . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag U1 O1 C2 C1 -17.3(8) . . . . ? U1 O1 C3 C4 51.1(7) . . . . ? U1 O2 C4 C3 27.3(7) . . . . ? U1 O2 C5 C6 -28.9(8) . . . . ? U1 O3 C8 C7 41.4(7) . . . . ? U1 O3 C9 C10 46.6(7) . . . . ? U1 O4 C10 C9 37.2(7) . . . . ? U1 O4 C11 C12 -1.7(8) . . . . ? U1 O5 C14 C13 -49.4(7) . . . . ? U1 O5 C15 C16 41.5(7) . . . . ? U1 O6 C16 C15 46.5(8) . . . . ? U1 O6 C17 C18 -9.1(8) . . . . ? U1 O7 C19 N3 -169.0(10) . . . . ? U1 O8 C22 N4 121.2(7) . . . . ? U1 N1 C1 C2 -56.0(6) . . . . ? U1 N1 C12 C11 -61.7(6) . . . . ? U1 N1 C13 C14 -42.7(7) . . . . ? U1 N2 C6 C5 -51.8(7) . . . . ? U1 N2 C7 C8 33.2(8) . . . . ? U1 N2 C18 C17 -59.4(6) . . . . ? O1 C3 C4 O2 -46.6(7) . . . . ? O2 C5 C6 N2 52.4(8) . . . . ? O3 C9 C10 O4 -51.1(8) . . . . ? O4 C11 C12 N1 43.6(8) . . . . ? O5 C15 C16 O6 -54.2(8) . . . . ? O6 C17 C18 N2 46.8(8) . . . . ? N1 C1 C2 O1 48.5(8) . . . . ? N1 C13 C14 O5 60.7(8) . . . . ? N2 C7 C8 O3 -49.0(9) . . . . ? C1 N1 C12 C11 179.8(6) . . . . ? C1 N1 C13 C14 79.0(7) . . . . ? C2 O1 C3 C4 -146.3(6) . . . . ? C3 O1 C2 C1 -179.0(6) . . . . ? C4 O2 C5 C6 154.5(6) . . . . ? C5 O2 C4 C3 -156.0(6) . . . . ? C6 N2 C7 C8 155.5(6) . . . . ? C6 N2 C18 C17 -179.3(6) . . . . ? C7 N2 C6 C5 -173.9(6) . . . . ? C7 N2 C18 C17 62.5(8) . . . . ? C8 O3 C9 C10 -160.1(6) . . . . ? C9 O3 C8 C7 -111.7(7) . . . . ? C10 O4 C11 C12 -168.7(6) . . . . ? C11 O4 C10 C9 -155.2(6) . . . . ? C12 N1 C1 C2 60.3(7) . . . . ? C12 N1 C13 C14 -161.0(6) . . . . ? C13 N1 C1 C2 -179.4(6) . . . . ? C13 N1 C12 C11 60.4(7) . . . . ? C14 O5 C15 C16 -179.7(6) . . . . ? C15 O5 C14 C13 170.9(6) . . . . ? C16 O6 C17 C18 -175.2(6) . . . . ? C17 O6 C16 C15 -146.5(7) . . . . ? C18 N2 C6 C5 65.0(7) . . . . ? C18 N2 C7 C8 -85.9(8) . . . . ? C20 N3 C19 O7 -177.9(12) . . . . ? C21 N3 C19 O7 4.6(19) . . . . ? C23 N4 C22 O8 0.7(11) . . . . ? C24 N4 C22 O8 -175.5(7) . . . . ? U1B O1B C2B C1B 32(6) . . . . ? U1B O1B C3B C4B -27(6) . . . . ? U1B O2B C4B C3B -51(5) . . . . ? U1B O2B C5B C6B 22(5) . . . . ? U1B O3B C8B C7B -1(6) . . . . ? U1B O3B C9B C10B -40(5) . . . . ? U1B O4B C10B C9B -45(6) . . . . ? U1B O4B C11B C12B -42(4) . . . . ? U1B O5B C14B C13B 15(7) . . . . ? U1B O5B C15B C16B -49(7) . . . . ? U1B O6B C16B C15B -34(6) . . . . ? U1B O6B C17B C18B 54(5) . . . . ? U1B O7B C19B N3B 160(8) . . . . ? U1B O8B C22B N4B -119(6) . . . . ? U1B N1B C1B C2B 54(4) . . . . ? U1B N1B C12B C11B -49(8) . . . . ? U1B N1B C13B C14B 63(4) . . . . ? U1B N2B C6B C5B 54(3) . . . . ? U1B N2B C7B C8B 59(4) . . . . ? U1B N2B C18B C17B 45(4) . . . . ? O1B C3B C4B O2B 45(5) . . . . ? O2B C5B C6B N2B -51(5) . . . . ? O3B C9B C10B O4B 52(6) . . . . ? O4B C11B C12B N1B 62(8) . . . . ? O5B C15B C16B O6B 51(6) . . . . ? O6B C17B C18B N2B -65(5) . . . . ? N1B C1B C2B O1B -57(6) . . . . ? N1B C13B C14B O5B -53(6) . . . . ? N2B C7B C8B O3B -40(6) . . . . ? C1B N1B C12B C11B -165(6) . . . . ? C1B N1B C13B C14B 180(4) . . . . ? C2B O1B C3B C4B 158(5) . . . . ? C3B O1B C2B C1B -153(4) . . . . ? C4B O2B C5B C6B 180(4) . . . . ? C5B O2B C4B C3B 151(4) . . . . ? C6B N2B C7B C8B 177(4) . . . . ? C6B N2B C18B C17B -77(4) . . . . ? C7B N2B C6B C5B -62(5) . . . . ? C7B N2B C18B C17B 164(3) . . . . ? C8B O3B C9B C10B 156(4) . . . . ? C9B O3B C8B C7B 162(4) . . . . ? C10B O4B C11B C12B 110(5) . . . . ? C11B O4B C10B C9B 162(4) . . . . ? C12B N1B C1B C2B 168(5) . . . . ? C12B N1B C13B C14B -55(6) . . . . ? C13B N1B C1B C2B -60(5) . . . . ? C13B N1B C12B C11B 70(9) . . . . ? C14B O5B C15B C16B 154(5) . . . . ? C15B O5B C14B C13B 172(5) . . . . ? C16B O6B C17B C18B -161(4) . . . . ? C17B O6B C16B C15B -177(4) . . . . ? C18B N2B C6B C5B 178(3) . . . . ? C18B N2B C7B C8B -63(5) . . . . ? C20B N3B C19B O7B 177(9) . . . . ? C21B N3B C19B O7B 2(15) . . . . ? C23B N4B C22B O8B 1(9) . . . . ? C25 N4B C22B O8B 178(5) . . . . ? C20C N3C C19C O7C -176(2) . . . . ? C21C N3C C19C O7C 7(3) . . . . ? _shelx_res_file ; TITL mb_nk_aza222_ui3_b.res in P2(1)/c mb_nk_aza222_ui3_3.res created by SHELXL-2018/3 at 15:27:59 on 09-Dec-2021 REM Old TITL MB_NK_aza222_UI3 in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.274, Rweak 0.008, Alpha 0.055 REM 1.073 for 412 systematic absences, Orientation as input REM Formula found by SHELXT: C21C N4B O8 I3B U CELL 0.71073 18.8644 10.3453 18.2109 90 104.769 90 ZERR 4 0.0012 0.0006 0.001 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H I N O U UNIT 96.01 200.02 12 16 32 4 SADI O7 C19C O7 C19 O8 C22 O7B C19B SADI C19C C21C C19 C21 C22 C23 C21B C20B SADI N3 C19C N3 C19 N4 C22 N3B C19B SADI C19C C20C C19 C20 C22 C24 C19B C20B SADI N3 C21C N3 C20 N3 C20C N3 C21 N4 C24 N4 C23 N3B C20B N3B C21B SADI C21 C20 C23 C24 C20C C21C SADI O2B C4B O2B C5B O1 C2 O1 C3 O3B C8B O3B C9B O2 C4 O2 C5 O4B C10B O4B = C11B O3 C8 O3 C9 O1B C2B O1B C3B O4 C10 O4 C11 O5 C14 O5 C15 O6 C16 O6 C17 = O5B C15B O5B C14B O6B C16B O6B C17B SADI N1 C12 N1 C13 N1 C1 N2B C6B N2B C7B N2B C18B N2 C7 N2 C18 N2 C6 N1B = C1B N1B C13B N1B C12B SADI C12 C11 C9 C10 C2B C1B C14B C13B C16B C15B C18B C17B C14 C13 C16 C15 = C8B C7B C4 C3 C10B C9B C6 C5 C3B C4B C6B C5B C2 C1 C18 C17 C8 C7 C12B C11B SADI U1 N2 U1B N1B U1 N1 U1B N2B SADI U1 O3 U1B O4B U1 O2 U1B O3B U1 O1 U1B O2B U1 O4 U1B O1B U1 O5 U1B O6B = U1B O5B U1 O6 SADI C4 C5 C2 C3 C10 C11 C8 C9 C17B C16B C15B C14B C14 C15 C16 C17 C5B C4B = C3B C2B C11B C10B C9B C8B SADI C1 C12 C6B C7B C12B C1B C7 C6 SADI C23B C25 C23 C24 C21 C20 C20C C21C SADI N4B C25 N4B C23B N4 C23 N4 C24 N3 C21 N3 C20C N3 C20 N3 C21C SADI C22B C25 C22 C24 C19C C20C C19 C20 SIMU 0.01 0.02 2 U1 > N3 C1 > C24 U1B > N3B C1B > C22B C19C H19C C20C C21C EADP N3 N3C EADP O7 O7C SIMU 0.001 0.002 2 N4B C22B > C25 EXYZ N3 N3C EXYZ O7 O7C SUMP 0.885 0.001 1 3 1 4 L.S. 10 PLAN 40 SIZE 0.235 0.385 0.626 TEMP -173.15 CONF BOND LIST 6 MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.000000 29.322300 FVAR 0.11277 0.88529 0.35750 0.52777 0.89365 0.55221 0.77066 PART 1 U1 6 0.763770 0.477168 0.420619 21.00000 0.01031 0.02255 = 0.00759 -0.00142 0.00296 -0.00172 O1 5 0.818940 0.604710 0.321411 21.00000 0.01544 0.02626 = 0.01156 0.00035 0.00571 0.00165 O2 5 0.719500 0.719667 0.375459 21.00000 0.01881 0.03152 = 0.01322 -0.00061 0.00746 0.00323 O3 5 0.672339 0.321063 0.459837 21.00000 0.01693 0.02938 = 0.01452 -0.00368 0.00847 -0.00451 O4 5 0.740005 0.247175 0.356673 21.00000 0.01660 0.02391 = 0.01484 -0.00256 0.00752 -0.00286 O5 5 0.866964 0.332120 0.515600 21.00000 0.01510 0.03190 = 0.00852 0.00253 0.00316 -0.00250 O6 5 0.775763 0.482590 0.568534 21.00000 0.01412 0.03142 = 0.01078 -0.00120 0.00530 -0.00221 O7 5 0.662824 0.487076 0.309743 31.00000 0.01620 0.02938 = 0.01894 0.00068 -0.00270 0.00336 O8 5 0.869252 0.610557 0.486898 21.00000 0.01595 0.02706 = 0.01379 -0.00107 0.00370 -0.00210 N1 4 0.868881 0.358877 0.360658 21.00000 0.01525 0.02633 = 0.01191 0.00098 0.00532 0.00216 N2 4 0.654612 0.594092 0.476493 21.00000 0.01521 0.02628 = 0.01242 -0.00349 0.00538 -0.00291 N3 4 0.576662 0.486415 0.197566 31.00000 0.01312 0.01804 = 0.01453 -0.00265 0.00060 -0.00048 N4 4 0.893826 0.815281 0.531866 21.00000 0.01331 0.02440 = 0.01070 0.00107 0.00317 -0.00175 C1 1 0.919245 0.457132 0.344405 21.00000 0.01749 0.02388 = 0.01457 0.00158 0.00534 -0.00186 AFIX 23 H1A 2 0.954943 0.414871 0.320660 21.00000 -1.20000 H1B 2 0.946936 0.496744 0.392701 21.00000 -1.20000 AFIX 0 C2 1 0.879288 0.561464 0.292352 21.00000 0.01852 0.02711 = 0.01296 0.00172 0.00865 0.00008 AFIX 23 H2A 2 0.912814 0.634421 0.290722 21.00000 -1.20000 H2B 2 0.860774 0.527154 0.240224 21.00000 -1.20000 AFIX 0 C3 1 0.776807 0.703610 0.273792 21.00000 0.01669 0.02446 = 0.01241 0.00125 0.00424 -0.00153 AFIX 23 H3A 2 0.735089 0.664400 0.236074 21.00000 -1.20000 H3B 2 0.807872 0.750421 0.246219 21.00000 -1.20000 AFIX 0 C4 1 0.749479 0.794268 0.323996 21.00000 0.01666 0.02810 = 0.01378 0.00332 0.00486 -0.00444 AFIX 23 H4A 2 0.790204 0.848921 0.352843 21.00000 -1.20000 H4B 2 0.711265 0.851425 0.293027 21.00000 -1.20000 AFIX 0 C5 1 0.666431 0.792411 0.403104 21.00000 0.02274 0.02851 = 0.01861 -0.00184 0.00920 0.00336 AFIX 23 H5A 2 0.638721 0.851306 0.363144 21.00000 -1.20000 H5B 2 0.691209 0.844661 0.447835 21.00000 -1.20000 AFIX 0 C6 1 0.615772 0.695995 0.424471 21.00000 0.02149 0.02815 = 0.01927 -0.00410 0.00761 0.00082 AFIX 23 H6B 2 0.581943 0.742034 0.449051 21.00000 -1.20000 H6A 2 0.585881 0.654778 0.377710 21.00000 -1.20000 AFIX 0 C7 1 0.598595 0.497640 0.486059 21.00000 0.01198 0.02976 = 0.01393 -0.00210 0.00761 -0.00585 AFIX 23 H7A 2 0.560082 0.491788 0.437731 21.00000 -1.20000 H7B 2 0.575150 0.530009 0.525318 21.00000 -1.20000 AFIX 0 C8 1 0.627616 0.364681 0.508090 21.00000 0.01587 0.03131 = 0.01350 -0.00081 0.00779 -0.00500 AFIX 23 H8A 2 0.657057 0.365244 0.561533 21.00000 -1.20000 H8B 2 0.586151 0.304182 0.504147 21.00000 -1.20000 AFIX 0 C9 1 0.640440 0.216501 0.410722 21.00000 0.01996 0.02263 = 0.01680 0.00022 0.00642 -0.00380 AFIX 23 H9A 2 0.603070 0.249898 0.366296 21.00000 -1.20000 H9B 2 0.616441 0.154724 0.438235 21.00000 -1.20000 AFIX 0 C10 1 0.700094 0.151338 0.385518 21.00000 0.02427 0.02086 = 0.02112 0.00185 0.00893 0.00002 AFIX 23 H10A 2 0.733001 0.105583 0.428752 21.00000 -1.20000 H10B 2 0.679272 0.087188 0.345490 21.00000 -1.20000 AFIX 0 C11 1 0.776698 0.195595 0.303227 21.00000 0.01943 0.02480 = 0.01250 -0.00503 0.00656 -0.00250 AFIX 23 H11A 2 0.740532 0.173002 0.255228 21.00000 -1.20000 H11B 2 0.804058 0.116442 0.323957 21.00000 -1.20000 AFIX 0 C12 1 0.828469 0.296671 0.288898 21.00000 0.01861 0.02537 = 0.01213 -0.00184 0.00488 0.00124 AFIX 23 H12A 2 0.863848 0.256432 0.263934 21.00000 -1.20000 H12B 2 0.800578 0.363131 0.254157 21.00000 -1.20000 AFIX 0 C13 1 0.912436 0.261001 0.412687 21.00000 0.01617 0.02918 = 0.01475 0.00279 0.00362 0.00432 AFIX 23 H13A 2 0.957310 0.240573 0.396247 21.00000 -1.20000 H13B 2 0.883389 0.180582 0.409678 21.00000 -1.20000 AFIX 0 C14 1 0.933643 0.307552 0.493368 21.00000 0.01278 0.03382 = 0.01213 0.00413 0.00423 -0.00026 AFIX 23 H14B 2 0.963204 0.241097 0.526735 21.00000 -1.20000 H14A 2 0.963123 0.387630 0.497416 21.00000 -1.20000 AFIX 0 C15 1 0.883901 0.357185 0.596158 21.00000 0.01809 0.03430 = 0.00779 0.00270 -0.00131 0.00058 AFIX 23 H15A 2 0.916301 0.433611 0.608848 21.00000 -1.20000 H15B 2 0.909432 0.281954 0.624691 21.00000 -1.20000 AFIX 0 C16 1 0.813869 0.381138 0.616724 21.00000 0.01803 0.03311 = 0.01150 0.00209 0.00142 -0.00306 AFIX 23 H16A 2 0.783752 0.301535 0.609356 21.00000 -1.20000 H16B 2 0.823619 0.407243 0.670680 21.00000 -1.20000 AFIX 0 C17 1 0.734334 0.562100 0.606427 21.00000 0.01563 0.03671 = 0.01201 -0.00554 0.00738 -0.00595 AFIX 23 H17A 2 0.767498 0.608598 0.649157 21.00000 -1.20000 H17B 2 0.700314 0.508443 0.626855 21.00000 -1.20000 AFIX 0 C18 1 0.692272 0.656285 0.549506 21.00000 0.01736 0.03356 = 0.01796 -0.00826 0.00679 -0.00225 AFIX 23 H18B 2 0.655330 0.699888 0.570936 21.00000 -1.20000 H18A 2 0.726286 0.723167 0.539755 21.00000 -1.20000 AFIX 0 C19 1 0.623883 0.430635 0.252124 41.00000 0.01566 0.01981 = 0.01595 -0.00388 0.00250 0.00156 AFIX 43 H19 2 0.629790 0.339835 0.248617 41.00000 -1.20000 AFIX 0 C20 1 0.531333 0.415688 0.133441 41.00000 0.02165 0.02201 = 0.01820 -0.00155 -0.00285 -0.00183 AFIX 137 H20A 2 0.548430 0.433126 0.087911 41.00000 -1.50000 H20B 2 0.480211 0.443512 0.124837 41.00000 -1.50000 H20C 2 0.534858 0.322836 0.144428 41.00000 -1.50000 AFIX 0 C21 1 0.567428 0.628445 0.194961 41.00000 0.02022 0.02658 = 0.02227 -0.00330 0.00124 0.00317 AFIX 137 H21A 2 0.520443 0.650814 0.205348 41.00000 -1.50000 H21B 2 0.568259 0.660212 0.144490 41.00000 -1.50000 H21C 2 0.607463 0.668421 0.233320 41.00000 -1.50000 AFIX 0 C22 1 0.884045 0.727758 0.478461 21.00000 0.00993 0.03294 = 0.01194 0.00399 0.00574 -0.00279 AFIX 43 H22 2 0.888377 0.754225 0.429841 21.00000 -1.20000 AFIX 0 C23 1 0.889310 0.785235 0.609132 21.00000 0.01903 0.03406 = 0.00690 -0.00427 0.00548 -0.00133 AFIX 137 H23A 2 0.928314 0.831061 0.645735 21.00000 -1.50000 H23B 2 0.895081 0.691907 0.617842 21.00000 -1.50000 H23C 2 0.841511 0.812631 0.615522 21.00000 -1.50000 AFIX 0 C24 1 0.905479 0.950436 0.516100 21.00000 0.02340 0.02521 = 0.02079 0.00222 0.00683 -0.00566 AFIX 137 H24A 2 0.911206 0.958741 0.464314 21.00000 -1.50000 H24B 2 0.949850 0.981984 0.552299 21.00000 -1.50000 H24C 2 0.863227 1.001595 0.521071 21.00000 -1.50000 AFIX 0 I1 3 1.056912 1.063493 0.700659 51.00000 0.01815 0.02962 = 0.01431 -0.00222 0.00594 -0.00430 I2 3 0.430685 0.450188 0.300282 61.00000 0.01691 0.07266 = 0.01364 -0.00562 0.00522 -0.01496 I3 3 0.719756 0.472718 0.093304 71.00000 0.02012 0.02437 = 0.01193 -0.00225 0.00461 -0.00145 PART 2 U1B 6 0.764343 0.513377 0.419212 -21.00000 0.00513 0.01264 = 0.00907 -0.00095 0.00389 0.00106 O1B 5 0.720393 0.274430 0.373398 -21.00000 0.01936 0.02124 = 0.01528 -0.00225 0.00786 -0.00218 O2B 5 0.819362 0.381046 0.321891 -21.00000 0.01785 0.02400 = 0.01308 -0.00131 0.00450 -0.00154 O3B 5 0.739762 0.744875 0.355958 -21.00000 0.01816 0.02587 = 0.01369 -0.00001 0.00591 0.00085 O4B 5 0.674229 0.675863 0.462130 -21.00000 0.01945 0.03056 = 0.01653 -0.00420 0.00795 0.00122 O5B 5 0.777825 0.505917 0.568058 -21.00000 0.01560 0.03226 = 0.01179 -0.00107 0.00430 -0.00403 O6B 5 0.866669 0.655272 0.511610 -21.00000 0.01245 0.02918 = 0.01242 -0.00089 0.00494 -0.00107 O7B 5 0.659734 0.452480 0.312837 -21.00000 0.01616 0.02181 = 0.01593 -0.00444 -0.00025 0.00119 O8B 5 0.870835 0.378524 0.484385 -21.00000 0.01291 0.03174 = 0.00963 0.00375 0.00156 -0.00088 N1B 4 0.653666 0.401440 0.474384 -21.00000 0.01541 0.03008 = 0.01309 -0.00205 0.00590 -0.00365 N2B 4 0.869381 0.632895 0.358438 -21.00000 0.01439 0.02514 = 0.01259 0.00222 0.00765 -0.00056 N3B 4 0.577606 0.447154 0.196893 -21.00000 0.01528 0.02128 = 0.01539 -0.00308 0.00261 0.00203 N4B 4 0.894134 0.177649 0.529706 -21.00000 0.01247 0.03124 = 0.01109 0.00287 0.00532 0.00136 C1B 1 0.615968 0.301142 0.419854 -21.00000 0.01608 0.02790 = 0.01461 -0.00093 0.00936 -0.00466 AFIX 23 H1BA 2 0.589344 0.343822 0.372126 -21.00000 -1.20000 H1BB 2 0.579326 0.256622 0.441300 -21.00000 -1.20000 AFIX 0 C2B 1 0.667238 0.202854 0.402056 -21.00000 0.01721 0.02247 = 0.01500 -0.00125 0.00911 -0.00426 AFIX 23 H2BA 2 0.691809 0.154085 0.448319 -21.00000 -1.20000 H2BB 2 0.640324 0.141078 0.363374 -21.00000 -1.20000 AFIX 0 C3B 1 0.749180 0.193709 0.323065 -21.00000 0.02023 0.02387 = 0.01577 -0.00111 0.00567 -0.00066 AFIX 23 H3BA 2 0.709990 0.138372 0.292072 -21.00000 -1.20000 H3BB 2 0.788756 0.137449 0.352554 -21.00000 -1.20000 AFIX 0 C4B 1 0.778193 0.282569 0.273613 -21.00000 0.01877 0.02414 = 0.01303 -0.00223 0.00603 -0.00145 AFIX 23 H4BA 2 0.810149 0.234897 0.247448 -21.00000 -1.20000 H4BB 2 0.737380 0.321783 0.234768 -21.00000 -1.20000 AFIX 0 C5B 1 0.877084 0.430562 0.291197 -21.00000 0.01598 0.02435 = 0.01289 0.00029 0.00711 -0.00003 AFIX 23 H5BA 2 0.855698 0.466634 0.239980 -21.00000 -1.20000 H5BB 2 0.910487 0.359197 0.286150 -21.00000 -1.20000 AFIX 0 C6B 1 0.919331 0.532960 0.341089 -21.00000 0.01602 0.02530 = 0.01410 0.00127 0.00612 -0.00009 AFIX 23 H6BA 2 0.948103 0.493622 0.389002 -21.00000 -1.20000 H6BB 2 0.954060 0.573912 0.315561 -21.00000 -1.20000 AFIX 0 C7B 1 0.830320 0.695025 0.285984 -21.00000 0.01660 0.02528 = 0.01296 0.00194 0.00644 0.00032 AFIX 23 H7BB 2 0.804391 0.628595 0.249868 -21.00000 -1.20000 H7BA 2 0.865965 0.739226 0.262991 -21.00000 -1.20000 AFIX 0 C8B 1 0.776449 0.790832 0.301221 -21.00000 0.01750 0.02600 = 0.01377 0.00178 0.00431 0.00042 AFIX 23 H8BA 2 0.802418 0.872235 0.319922 -21.00000 -1.20000 H8BB 2 0.739575 0.810199 0.253142 -21.00000 -1.20000 AFIX 0 C9B 1 0.705490 0.846430 0.387779 -21.00000 0.01793 0.02842 = 0.01570 -0.00078 0.00648 0.00222 AFIX 23 H9BA 2 0.685348 0.912894 0.348954 -21.00000 -1.20000 H9BB 2 0.741209 0.888052 0.430621 -21.00000 -1.20000 AFIX 0 C10B 1 0.645201 0.783425 0.414806 -21.00000 0.01905 0.02879 = 0.01586 -0.00311 0.00816 0.00339 AFIX 23 H10C 2 0.623539 0.846486 0.443744 -21.00000 -1.20000 H10D 2 0.606143 0.753719 0.370728 -21.00000 -1.20000 AFIX 0 C11B 1 0.627676 0.634728 0.508694 -21.00000 0.01666 0.02904 = 0.01574 -0.00257 0.00742 -0.00194 AFIX 23 H11C 2 0.586867 0.696263 0.505821 -21.00000 -1.20000 H11D 2 0.655555 0.624828 0.562358 -21.00000 -1.20000 AFIX 0 C12B 1 0.600255 0.507379 0.474210 -21.00000 0.01498 0.02946 = 0.01403 -0.00188 0.00737 -0.00315 AFIX 23 H12D 2 0.564020 0.475038 0.500703 -21.00000 -1.20000 H12C 2 0.573435 0.523384 0.420749 -21.00000 -1.20000 AFIX 0 C13B 1 0.691964 0.337147 0.546464 -21.00000 0.01719 0.03174 = 0.01379 -0.00207 0.00553 -0.00503 AFIX 23 H13C 2 0.727342 0.273412 0.536091 -21.00000 -1.20000 H13D 2 0.655694 0.289813 0.567092 -21.00000 -1.20000 AFIX 0 C14B 1 0.731758 0.431919 0.604227 -21.00000 0.01580 0.03203 = 0.01224 -0.00097 0.00439 -0.00457 AFIX 23 H14C 2 0.696592 0.489107 0.620615 -21.00000 -1.20000 H14D 2 0.761737 0.386297 0.649318 -21.00000 -1.20000 AFIX 0 C15B 1 0.811139 0.613251 0.614463 -21.00000 0.01592 0.03214 = 0.01173 -0.00397 0.00333 -0.00360 AFIX 23 H15C 2 0.821622 0.590321 0.668955 -21.00000 -1.20000 H15D 2 0.778128 0.689199 0.605055 -21.00000 -1.20000 AFIX 0 C16B 1 0.880559 0.642431 0.592763 -21.00000 0.01542 0.02782 = 0.01209 -0.00188 0.00266 -0.00267 AFIX 23 H16C 2 0.901967 0.723699 0.617499 -21.00000 -1.20000 H16D 2 0.916331 0.571993 0.610595 -21.00000 -1.20000 AFIX 0 C17B 1 0.932882 0.677251 0.488764 -21.00000 0.01293 0.02826 = 0.01264 -0.00074 0.00493 -0.00018 AFIX 23 H17C 2 0.959898 0.595068 0.489308 -21.00000 -1.20000 H17D 2 0.964824 0.738612 0.523968 -21.00000 -1.20000 AFIX 0 C18B 1 0.911848 0.732017 0.410273 -21.00000 0.01253 0.02761 = 0.01108 0.00162 0.00545 -0.00134 AFIX 23 H18D 2 0.881770 0.810755 0.409179 -21.00000 -1.20000 H18C 2 0.956343 0.755752 0.393965 -21.00000 -1.20000 AFIX 0 C19B 1 0.615965 0.505432 0.256857 -21.00000 0.01688 0.02277 = 0.01771 -0.00217 0.00285 0.00081 AFIX 43 H19B 2 0.610656 0.596583 0.258890 -21.00000 -1.20000 AFIX 0 C20B 1 0.525391 0.515631 0.136472 -21.00000 0.01554 0.02306 = 0.01593 -0.00173 0.00179 0.00237 AFIX 137 H20D 2 0.530526 0.485676 0.087035 -21.00000 -1.50000 H20E 2 0.535170 0.608691 0.141339 -21.00000 -1.50000 H20F 2 0.475418 0.498506 0.140471 -21.00000 -1.50000 AFIX 0 C21B 1 0.576669 0.307740 0.184936 -21.00000 0.01929 0.01788 = 0.01647 -0.00285 0.00213 0.00090 AFIX 137 H21D 2 0.535406 0.269694 0.200882 -21.00000 -1.50000 H21E 2 0.622675 0.270216 0.214916 -21.00000 -1.50000 H21F 2 0.571296 0.289605 0.130974 -21.00000 -1.50000 AFIX 0 C22B 1 0.883304 0.263637 0.480036 -21.00000 0.01248 0.03123 = 0.01106 0.00292 0.00525 0.00134 AFIX 43 H22B 2 0.885066 0.234906 0.430986 -21.00000 -1.20000 AFIX 0 C23B 1 0.891606 0.213515 0.606603 -21.00000 0.01244 0.03127 = 0.01101 0.00285 0.00548 0.00134 AFIX 137 H23D 2 0.907398 0.140017 0.640813 -21.00000 -1.50000 H23E 2 0.841370 0.237536 0.606666 -21.00000 -1.50000 H23F 2 0.924356 0.287049 0.623904 -21.00000 -1.50000 AFIX 0 C25 1 0.906765 0.040545 0.516940 -21.00000 0.01239 0.03130 = 0.01117 0.00257 0.00549 0.00153 AFIX 137 H25A 2 0.947931 0.008934 0.557361 -21.00000 -1.50000 H25B 2 0.918216 0.030188 0.467717 -21.00000 -1.50000 H25C 2 0.862589 -0.009102 0.517213 -21.00000 -1.50000 AFIX 0 I1B 3 1.058175 0.941705 0.701422 -51.00000 0.02136 0.01690 = 0.01673 -0.00004 0.00923 0.00321 I2B 3 0.427435 0.523626 0.299590 -61.00000 0.01481 0.01454 = 0.01485 -0.00048 0.00507 -0.00293 I3B 3 0.719340 0.505176 0.092086 -71.00000 0.03056 0.08575 = 0.02585 0.01559 0.01540 0.01087 PART 3 O7C 5 0.662824 0.487076 0.309743 41.00000 0.01620 0.02938 = 0.01894 0.00068 -0.00270 0.00336 N3C 4 0.576662 0.486415 0.197566 41.00000 0.01312 0.01804 = 0.01453 -0.00265 0.00060 -0.00048 C19C 1 0.619739 0.540808 0.257464 31.00000 0.01730 0.02379 = 0.01838 -0.00610 0.00237 0.00259 AFIX 43 H19C 2 0.617066 0.632287 0.260440 31.00000 -1.20000 AFIX 0 C20C 1 0.530819 0.553530 0.136509 31.00000 0.01392 0.02427 = 0.01282 0.00017 -0.00320 0.00533 AFIX 137 H20G 2 0.549504 0.543793 0.091292 31.00000 -1.50000 H20H 2 0.529946 0.645366 0.149446 31.00000 -1.50000 H20I 2 0.481048 0.518219 0.126221 31.00000 -1.50000 AFIX 0 C21C 1 0.573127 0.339424 0.195567 31.00000 0.02420 0.02120 = 0.02042 -0.00113 -0.00370 0.00084 AFIX 137 H21G 2 0.610776 0.304265 0.238293 31.00000 -1.50000 H21H 2 0.581702 0.308302 0.147735 31.00000 -1.50000 H21I 2 0.524627 0.311069 0.199384 31.00000 -1.50000 AFIX 0 HKLF 4 REM mb_nk_aza222_ui3_b.res in P2(1)/c REM wR2 = 0.0900, GooF = S = 1.202, Restrained GooF = 1.099 for all data REM R1 = 0.0367 for 6465 Fo > 4sig(Fo) and 0.0436 for all 7296 data REM 764 parameters refined using 1818 restraints END WGHT 0.0000 29.3370 REM Highest difference peak 0.959, deepest hole -1.776, 1-sigma level 0.153 Q1 1 0.9543 0.9559 0.6507 11.00000 0.05 0.96 Q2 1 0.7408 0.5987 0.4376 11.00000 0.05 0.80 Q3 1 0.6701 0.5350 0.3472 11.00000 0.05 0.79 Q4 1 0.3810 0.4832 0.3340 11.00000 0.05 0.79 Q5 1 0.6783 0.0799 0.2532 11.00000 0.05 0.79 Q6 1 0.5648 0.4766 0.3476 11.00000 0.05 0.78 Q7 1 0.7554 0.4003 0.0605 11.00000 0.05 0.77 Q8 1 0.6271 0.8907 0.5260 11.00000 0.05 0.74 Q9 1 1.0931 0.9228 0.6721 11.00000 0.05 0.73 Q10 1 0.8113 0.5406 0.3932 11.00000 0.05 0.73 Q11 1 0.6703 0.4647 0.0950 11.00000 0.05 0.67 Q12 1 1.0157 0.9509 0.7147 11.00000 0.05 0.65 Q13 1 0.8068 0.1125 0.2534 11.00000 0.05 0.64 Q14 1 0.8505 0.9654 0.6367 11.00000 0.05 0.63 Q15 1 0.5818 0.4830 0.0227 11.00000 0.05 0.62 Q16 1 1.0595 0.8684 0.6981 11.00000 0.05 0.61 Q17 1 0.5598 0.5760 0.3421 11.00000 0.05 0.61 Q18 1 0.6399 0.4749 0.3873 11.00000 0.05 0.60 Q19 1 0.4182 0.3857 0.3123 11.00000 0.05 0.59 Q20 1 0.7157 0.1192 0.2546 11.00000 0.05 0.59 Q21 1 0.4209 0.6410 0.2817 11.00000 0.05 0.58 Q22 1 0.9201 0.6024 0.4473 11.00000 0.05 0.58 Q23 1 0.7273 0.3751 0.4400 11.00000 0.05 0.55 Q24 1 0.8665 0.5072 0.4618 11.00000 0.05 0.55 Q25 1 0.9978 0.5330 0.5210 11.00000 0.05 0.55 Q26 1 0.4922 0.4887 0.3595 11.00000 0.05 0.54 Q27 1 0.6264 0.0451 0.5119 11.00000 0.05 0.54 Q28 1 1.0790 1.1741 0.6802 11.00000 0.05 0.54 Q29 1 0.6866 0.5774 0.1171 11.00000 0.05 0.53 Q30 1 0.7785 0.5391 0.0610 11.00000 0.05 0.53 Q31 1 1.1103 1.1044 0.6641 11.00000 0.05 0.52 Q32 1 0.7909 0.3644 0.3992 11.00000 0.05 0.52 Q33 1 0.5804 0.5125 0.0738 11.00000 0.05 0.51 Q34 1 0.9523 0.1251 0.6359 11.00000 0.05 0.51 Q35 1 0.7422 0.8419 0.5665 11.00000 0.05 0.51 Q36 1 0.4624 0.3341 0.2838 11.00000 0.05 0.51 Q37 1 1.0210 0.8571 0.7257 11.00000 0.05 0.50 Q38 1 0.4855 0.5585 0.2987 11.00000 0.05 0.50 Q39 1 0.8983 0.6559 0.4607 11.00000 0.05 0.50 Q40 1 0.7103 0.4528 0.4603 11.00000 0.05 0.49 ; _shelx_res_checksum 8777 _olex2_exptl_crystal_mounting_method 'MicroMount (MiTeGen) with paratone oil (Parabar 10312, Hampton Research)' _olex2_submission_special_instructions 'No special instructions were received'