#------------------------------------------------------------------------------ #$Date: 2023-11-30 04:23:03 +0200 (Thu, 30 Nov 2023) $ #$Revision: 287874 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/78/7247800.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7247800 loop_ _publ_author_name 'Khurshid, Afshan' 'Tanveer, Tania' 'Hafeez, Komal' 'Ahmed, Maqsood' 'Akhtar, Zareen' 'Zafar, M. Naveed' _publ_section_title ; Palladium-anchored donor-flexible pyridylidene amide (PYA) electrocatalysts for CO2 reduction ; _journal_issue 49 _journal_name_full 'RSC Advances' _journal_page_first 34817 _journal_page_last 34825 _journal_paper_doi 10.1039/D3RA06477H _journal_volume 13 _journal_year 2023 _chemical_formula_moiety '2(I), C21 H23 N5 O2, H2 O' _chemical_formula_sum 'C21 H25 I2 N5 O3' _chemical_formula_weight 649.26 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _audit_creation_date 2023-07-15 _audit_creation_method ;FinalCif V118 by Daniel Kratzert, Freiburg 2023, https://dkratzert.de/finalcif.html ; _audit_update_record ; 2023-07-15 deposited with the CCDC. 2023-11-15 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 110.401(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.8789(13) _cell_length_b 10.7830(9) _cell_length_c 15.3311(11) _cell_measurement_reflns_used 9960 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25.45 _cell_measurement_theta_min 2.33 _cell_volume 2460.4(3) _computing_cell_refinement 'SAINT V8.38A (Bruker, 2018)' _computing_data_reduction 'SAINT V8.38A (Bruker, 2018)' _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 2014/5 (Sheldrick, 2014)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 293(2) _diffrn_detector CPAD _diffrn_detector_area_resol_mean 7.41 _diffrn_detector_type 'Bruker PHOTON II' _diffrn_measured_fraction_theta_full 0.977 _diffrn_measured_fraction_theta_max 0.977 _diffrn_measurement_device 'Four-circle diffractometer' _diffrn_measurement_device_type 'Bruker D8 VENTURE dual wavelength Mo/Cu' _diffrn_measurement_method '\w and \f scans' _diffrn_measurement_specimen_support 'MiTeGen micromount' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_unetI/netI 0.0323 _diffrn_reflns_Laue_measured_fraction_full 0.977 _diffrn_reflns_Laue_measured_fraction_max 0.977 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 4582 _diffrn_reflns_point_group_measured_fraction_full 0.977 _diffrn_reflns_point_group_measured_fraction_max 0.977 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.707 _diffrn_reflns_theta_min 2.332 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type 'Incoatec I\ms' _exptl_absorpt_coefficient_mu 2.587 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_correction_T_min 0.6050 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1173 before and 0.0725 after correction. The Ratio of minimum to maximum transmission is 0.8118. The \l/2 correction factor is Not present. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.753 _exptl_crystal_description block _exptl_crystal_F_000 1264 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _refine_diff_density_max 3.480 _refine_diff_density_min -1.080 _refine_diff_density_rms 0.219 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 286 _refine_ls_number_reflns 4582 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.071 _refine_ls_R_factor_all 0.1066 _refine_ls_R_factor_gt 0.0880 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1577P)^2^+34.7324P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2703 _refine_ls_wR_factor_ref 0.2946 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3651 _reflns_number_total 4582 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ra06477h2.cif _cod_data_source_block 2d_komal_naveedzafar_qau_0ma_a_a _cod_depositor_comments ; The following automatic conversions were performed: data item '_diffrn_radiation_probe' value 'X-ray' was changed to 'x-ray' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas ; _cod_database_code 7247800 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.893(3) 0.107(3) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H,H) groups 3.a Free rotating group: O3(H3A,H3B) 3.b Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C20(H20A,H20B) 3.c Aromatic/amide H refined with riding coordinates: N2(H2), N4(H4), C6(H6), C12(H12), C18(H18), C7(H7), C3(H3), C10(H10), C4(H4A), C19(H19), C11(H11), C16(H16), C17(H17) 3.d Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C21(H21A,H21B,H21C) ; _olex2_submission_special_instructions 'No special instructions were received' _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.492 _shelx_estimated_absorpt_t_max 0.600 _diffrn_measurement_ambient_temperature_device_make 'Oxford Cobra Cryo device' _shelx_res_file ; TITL 2D_Komal_Naveedzafar_QAU_0ma_a_a.res in P2(1)/c 2d_komal_naveedzafar_qau_0ma_a_a.res created by SHELXL-2018/3 at 15:35:05 on 15-Jul-2023 REM Old TITL 2D_Komal_Naveedzafar_QAU_0ma_a.hkl REM SHELXT solution in P2(1)/c REM R1 0.208, Rweak 0.054, Alpha 0.088, Orientation as input REM Formula found by SHELXT: C40 Mo2 CELL 0.71073 15.8789 10.783 15.3311 90 110.401 90 ZERR 4 0.0013 0.0009 0.0011 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H I N O UNIT 84 100 8 20 12 L.S. 20 PLAN 6 SIZE 0.22 0.24 0.32 CONF BOND $H LIST 6 MORE -1 fmap 2 acta OMIT 2 0 4 OMIT -3 1 7 OMIT -1 1 7 OMIT -6 4 7 OMIT -8 4 7 OMIT -11 1 7 OMIT -8 2 4 OMIT -1 2 7 OMIT -11 5 4 OMIT -11 1 11 OMIT 2 4 7 OMIT -1 1 11 OMIT -3 1 11 OMIT 0 2 7 OMIT 0 4 7 OMIT -9 3 4 OMIT -11 3 4 OMIT 2 2 7 OMIT -1 5 4 OMIT -6 6 11 OMIT -13 3 7 OMIT -10 2 7 OMIT 4 2 4 OMIT 7 5 4 OMIT -8 2 7 OMIT -6 4 11 OMIT -2 5 7 OMIT 2 4 11 OMIT -14 2 4 OMIT -7 4 4 OMIT 5 1 7 OMIT -6 6 7 OMIT -8 0 14 OMIT 7 1 7 OMIT -9 1 7 OMIT -7 5 7 OMIT -10 3 11 OMIT 5 7 4 OMIT -4 7 4 OMIT -9 5 4 OMIT -11 3 11 OMIT 12 0 4 OMIT -2 3 11 OMIT 2 6 11 OMIT 1 4 4 OMIT 7 2 7 OMIT 7 1 11 OMIT -2 5 11 OMIT -6 1 7 OMIT 10 2 4 OMIT 7 3 4 OMIT -3 3 11 OMIT -9 1 4 OMIT 6 5 7 OMIT -14 6 7 OMIT -9 1 11 OMIT 7 4 7 OMIT -8 4 4 OMIT -16 4 7 OMIT -5 3 7 OMIT -7 6 4 OMIT 2 6 7 OMIT 10 2 7 OMIT -6 2 11 OMIT -3 7 4 OMIT 10 4 7 OMIT -9 2 4 OMIT 2 8 3 OMIT -8 4 11 OMIT -4 9 4 OMIT -14 6 11 OMIT 9 3 4 OMIT 6 9 4 OMIT 5 6 4 OMIT 4 5 4 OMIT -2 9 4 OMIT -3 3 7 OMIT 3 1 7 OMIT -11 3 7 OMIT -5 7 7 OMIT -6 2 4 OMIT -10 4 7 OMIT -5 9 7 OMIT -4 2 4 REM REM REM WGHT 0.157700 34.732399 BASF 0.10661 FVAR 0.91616 I1 3 0.556881 0.467282 0.806036 11.00000 0.04547 0.06758 = 0.04809 0.00991 0.01184 0.00354 I2 3 -0.057383 0.434439 0.784284 11.00000 0.06422 0.07983 = 0.09077 -0.01231 0.02183 -0.00734 N2 4 0.595565 0.714831 0.658408 11.00000 0.03260 0.05667 = 0.04692 -0.00344 0.00908 -0.00559 AFIX 43 H2 2 0.555854 0.700066 0.683475 11.00000 -1.20000 AFIX 0 N3 4 0.425285 0.647469 0.578634 11.00000 0.03691 0.04002 = 0.03956 -0.00117 0.00294 -0.00043 N1 4 0.839823 0.834806 0.841846 11.00000 0.03489 0.04271 = 0.06571 -0.00003 0.00834 0.00046 O2 5 0.203444 0.605209 0.572080 11.00000 0.03116 0.09358 = 0.05458 0.01407 0.00358 -0.00325 N4 4 0.332581 0.610210 0.697758 11.00000 0.03338 0.04632 = 0.05327 -0.00312 0.00523 -0.00096 AFIX 43 H4 2 0.390150 0.612249 0.713921 11.00000 -1.20000 AFIX 0 O1 5 0.615931 0.709651 0.516363 11.00000 0.05531 0.10421 = 0.05586 0.00573 0.02116 -0.00871 N5 4 0.235404 0.595308 0.914606 11.00000 0.04993 0.05804 = 0.06295 0.00103 0.02119 0.00970 C14 1 0.283915 0.613093 0.603494 11.00000 0.04830 0.04168 = 0.04361 0.00766 0.00728 0.00488 C9 1 0.471194 0.656468 0.521573 11.00000 0.04323 0.03308 = 0.05269 0.00059 0.00435 0.00323 C6 1 0.688065 0.779038 0.810262 11.00000 0.03670 0.05750 = 0.05718 0.00914 0.01533 -0.00045 AFIX 43 H6 2 0.639660 0.769631 0.830574 11.00000 -1.20000 AFIX 0 C15 1 0.297602 0.604348 0.768805 11.00000 0.03071 0.04949 = 0.04486 0.00006 0.00413 -0.00455 C12 1 0.298114 0.592720 0.448266 11.00000 0.04188 0.04839 = 0.05819 -0.00430 0.00041 -0.00546 AFIX 43 H12 2 0.238239 0.568171 0.424864 11.00000 -1.20000 AFIX 0 C5 1 0.678706 0.752768 0.717704 11.00000 0.03146 0.04338 = 0.04917 0.00968 0.00870 -0.00262 C18 1 0.323620 0.567146 0.927325 11.00000 0.04155 0.07700 = 0.04741 0.00385 -0.00068 0.01011 AFIX 43 H18 2 0.362383 0.545072 0.986295 11.00000 -1.20000 AFIX 0 C7 1 0.769143 0.818516 0.869850 11.00000 0.03806 0.05639 = 0.04924 0.00308 0.00764 -0.00614 AFIX 43 H7 2 0.775856 0.834645 0.931507 11.00000 -1.20000 AFIX 0 C2 1 0.929736 0.879687 0.906139 11.00000 0.04277 0.05434 = 0.08267 -0.01301 0.00671 -0.01359 AFIX 23 H2A 2 0.954075 0.938615 0.873368 11.00000 -1.20000 H2B 2 0.922006 0.922234 0.958586 11.00000 -1.20000 AFIX 0 C13 1 0.338873 0.617072 0.541173 11.00000 0.04023 0.03545 = 0.05744 0.00967 0.00351 0.00107 C8 1 0.569240 0.698128 0.564959 11.00000 0.03876 0.04956 = 0.04918 0.00613 0.00872 -0.00102 C3 1 0.832701 0.807770 0.755616 11.00000 0.04213 0.07479 = 0.07209 -0.00925 0.02556 -0.00743 AFIX 43 H3 2 0.882861 0.816802 0.738112 11.00000 -1.20000 AFIX 0 C10 1 0.435416 0.633700 0.426798 11.00000 0.05375 0.05793 = 0.04206 0.01844 0.00901 0.00559 AFIX 43 H10 2 0.470666 0.637904 0.389525 11.00000 -1.20000 AFIX 0 C4 1 0.753756 0.766759 0.690862 11.00000 0.03896 0.06538 = 0.06066 -0.00820 0.02120 -0.00399 AFIX 43 H4A 2 0.750280 0.748661 0.630393 11.00000 -1.20000 AFIX 0 C19 1 0.354163 0.570840 0.857744 11.00000 0.03630 0.06920 = 0.04580 0.00011 -0.00010 0.00977 AFIX 43 H19 2 0.413852 0.550960 0.868034 11.00000 -1.20000 AFIX 0 C11 1 0.346148 0.604807 0.390411 11.00000 0.05783 0.06395 = 0.04083 -0.00669 -0.00145 -0.00128 AFIX 43 H11 2 0.318364 0.593472 0.326633 11.00000 -1.20000 AFIX 0 C16 1 0.209320 0.635699 0.755545 11.00000 0.03807 0.06103 = 0.06018 0.01037 0.00713 0.00429 AFIX 43 H16 2 0.170552 0.661642 0.697611 11.00000 -1.20000 AFIX 0 C17 1 0.180598 0.627531 0.829842 11.00000 0.04960 0.07207 = 0.06001 -0.00509 0.02248 0.00428 AFIX 43 H17 2 0.120811 0.645061 0.820876 11.00000 -1.20000 AFIX 0 C1 1 0.992845 0.778179 0.940129 11.00000 0.04292 0.09133 = 0.10041 -0.01238 -0.00445 0.00565 AFIX 137 H1A 2 1.003613 0.739207 0.888697 11.00000 -1.50000 H1B 2 0.968234 0.718552 0.971135 11.00000 -1.50000 H1C 2 1.048399 0.809690 0.983022 11.00000 -1.50000 AFIX 0 C20 1 0.206114 0.588387 0.995395 11.00000 0.06318 0.07427 = 0.06879 0.00316 0.02490 0.01493 AFIX 23 H20A 2 0.153232 0.639758 0.984192 11.00000 -1.20000 H20B 2 0.253231 0.620602 1.049791 11.00000 -1.20000 AFIX 0 C21 1 0.184862 0.458533 1.013904 11.00000 0.11453 0.09201 = 0.08210 -0.00620 0.04909 -0.02781 AFIX 137 H21A 2 0.222667 0.402229 0.995838 11.00000 -1.50000 H21B 2 0.123023 0.440986 0.978732 11.00000 -1.50000 H21C 2 0.195208 0.448750 1.079062 11.00000 -1.50000 AFIX 6 O3 5 0.086809 0.337688 0.388889 11.00000 0.19190 0.12127 = 0.11601 0.00032 0.08248 0.02096 H3A 2 0.106357 0.399846 0.424251 11.00000 -1.50000 H3B 2 0.036299 0.361217 0.350758 11.00000 -1.50000 AFIX 0 HKLF 5 REM 2D_Komal_Naveedzafar_QAU_0ma_a_a.res in P2(1)/c REM wR2 = 0.2946, GooF = S = 1.071, Restrained GooF = 1.071 for all data REM R1 = 0.0880 for 3651 Fo > 4sig(Fo) and 0.1066 for all 4582 data REM 286 parameters refined using 0 restraints END WGHT 0.1577 34.7329 REM Highest difference peak 3.480, deepest hole -1.080, 1-sigma level 0.219 Q1 1 0.4418 0.5344 0.4718 11.00000 0.05 3.48 Q2 1 0.4412 0.5283 0.9112 11.00000 0.05 2.92 Q3 1 1.0587 0.9356 0.9934 11.00000 0.05 2.36 Q4 1 0.4428 0.5310 0.7519 11.00000 0.05 2.15 Q5 1 0.0589 0.5643 0.9256 11.00000 0.05 2.13 Q6 1 0.0569 0.5650 0.7674 11.00000 0.05 1.80 ; _shelx_res_checksum 82439 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' 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 I1 I 0.55688(6) 0.46728(9) 0.80604(6) 0.0549(3) Uani 1 1 d . . . . . I2 I -0.05738(8) 0.43444(13) 0.78428(10) 0.0796(4) Uani 1 1 d . . . . . N2 N 0.5956(6) 0.7148(10) 0.6584(7) 0.047(2) Uani 1 1 d . . . . . H2 H 0.555854 0.700066 0.683475 0.056 Uiso 1 1 calc R U . . . N3 N 0.4253(6) 0.6475(9) 0.5786(7) 0.042(2) Uani 1 1 d . . . . . N1 N 0.8398(7) 0.8348(10) 0.8418(8) 0.050(3) Uani 1 1 d . . . . . O2 O 0.2034(6) 0.6052(12) 0.5721(7) 0.063(3) Uani 1 1 d . . . . . N4 N 0.3326(7) 0.6102(10) 0.6978(8) 0.047(2) Uani 1 1 d . . . . . H4 H 0.390150 0.612249 0.713921 0.056 Uiso 1 1 calc R U . . . O1 O 0.6159(7) 0.7097(13) 0.5164(7) 0.071(3) Uani 1 1 d . . . . . N5 N 0.2354(8) 0.5953(11) 0.9146(9) 0.057(3) Uani 1 1 d . . . . . C14 C 0.2839(9) 0.6131(12) 0.6035(9) 0.047(3) Uani 1 1 d . . . . . C9 C 0.4712(8) 0.6565(11) 0.5216(9) 0.046(3) Uani 1 1 d . . . . . C6 C 0.6881(8) 0.7790(13) 0.8103(10) 0.051(3) Uani 1 1 d . . . . . H6 H 0.639660 0.769631 0.830574 0.061 Uiso 1 1 calc R U . . . C15 C 0.2976(8) 0.6043(12) 0.7688(9) 0.044(3) Uani 1 1 d . . . . . C12 C 0.2981(9) 0.5927(13) 0.4483(10) 0.054(3) Uani 1 1 d . . . . . H12 H 0.238239 0.568171 0.424864 0.065 Uiso 1 1 calc R U . . . C5 C 0.6787(7) 0.7528(11) 0.7177(9) 0.043(3) Uani 1 1 d . . . . . C18 C 0.3236(9) 0.5671(15) 0.9273(10) 0.060(4) Uani 1 1 d . . . . . H18 H 0.362383 0.545072 0.986295 0.072 Uiso 1 1 calc R U . . . C7 C 0.7691(8) 0.8185(13) 0.8699(9) 0.050(3) Uani 1 1 d . . . . . H7 H 0.775856 0.834645 0.931507 0.060 Uiso 1 1 calc R U . . . C2 C 0.9297(9) 0.8797(14) 0.9061(12) 0.064(4) Uani 1 1 d . . . . . H2A H 0.954075 0.938615 0.873368 0.077 Uiso 1 1 calc R U . . . H2B H 0.922006 0.922234 0.958586 0.077 Uiso 1 1 calc R U . . . C13 C 0.3389(8) 0.6171(11) 0.5412(10) 0.048(3) Uani 1 1 d . . . . . C8 C 0.5692(8) 0.6981(12) 0.5650(9) 0.048(3) Uani 1 1 d . . . . . C3 C 0.8327(9) 0.8078(15) 0.7556(11) 0.062(4) Uani 1 1 d . . . . . H3 H 0.882861 0.816802 0.738112 0.074 Uiso 1 1 calc R U . . . C10 C 0.4354(9) 0.6337(13) 0.4268(9) 0.053(3) Uani 1 1 d . . . . . H10 H 0.470666 0.637904 0.389525 0.064 Uiso 1 1 calc R U . . . C4 C 0.7538(8) 0.7668(14) 0.6909(10) 0.054(3) Uani 1 1 d . . . . . H4A H 0.750280 0.748661 0.630393 0.065 Uiso 1 1 calc R U . . . C19 C 0.3542(9) 0.5708(14) 0.8577(9) 0.054(3) Uani 1 1 d . . . . . H19 H 0.413852 0.550960 0.868034 0.065 Uiso 1 1 calc R U . . . C11 C 0.3461(10) 0.6048(14) 0.3904(10) 0.059(4) Uani 1 1 d . . . . . H11 H 0.318364 0.593472 0.326633 0.071 Uiso 1 1 calc R U . . . C16 C 0.2093(9) 0.6357(14) 0.7555(10) 0.056(3) Uani 1 1 d . . . . . H16 H 0.170552 0.661642 0.697611 0.067 Uiso 1 1 calc R U . . . C17 C 0.1806(10) 0.6275(15) 0.8298(11) 0.060(3) Uani 1 1 d . . . . . H17 H 0.120811 0.645061 0.820876 0.072 Uiso 1 1 calc R U . . . C1 C 0.9928(10) 0.7782(19) 0.9401(15) 0.086(6) Uani 1 1 d . . . . . H1A H 1.003613 0.739207 0.888697 0.129 Uiso 1 1 calc R U . . . H1B H 0.968234 0.718552 0.971135 0.129 Uiso 1 1 calc R U . . . H1C H 1.048399 0.809690 0.983022 0.129 Uiso 1 1 calc R U . . . C20 C 0.2061(12) 0.5884(16) 0.9954(12) 0.068(4) Uani 1 1 d . . . . . H20A H 0.153232 0.639758 0.984192 0.082 Uiso 1 1 calc R U . . . H20B H 0.253231 0.620602 1.049791 0.082 Uiso 1 1 calc R U . . . C21 C 0.1849(16) 0.4585(19) 1.0139(15) 0.092(6) Uani 1 1 d . . . . . H21A H 0.222667 0.402229 0.995838 0.138 Uiso 1 1 calc R U . . . H21B H 0.123023 0.440986 0.978732 0.138 Uiso 1 1 calc R U . . . H21C H 0.195208 0.448750 1.079062 0.138 Uiso 1 1 calc R U . . . O3 O 0.0868(19) 0.338(2) 0.3889(16) 0.135(7) Uani 1 1 d G . . . . H3A H 0.106357 0.399846 0.424251 0.203 Uiso 1 1 d G U . . . H3B H 0.036299 0.361217 0.350758 0.203 Uiso 1 1 d G 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 I1 0.0455(5) 0.0676(6) 0.0481(5) 0.0099(4) 0.0118(4) 0.0035(4) I2 0.0642(7) 0.0798(8) 0.0908(9) -0.0123(6) 0.0218(6) -0.0073(5) N2 0.033(5) 0.057(6) 0.047(6) -0.003(5) 0.009(4) -0.006(4) N3 0.037(5) 0.040(5) 0.040(5) -0.001(4) 0.003(4) 0.000(4) N1 0.035(5) 0.043(5) 0.066(7) 0.000(5) 0.008(5) 0.000(4) O2 0.031(4) 0.094(8) 0.055(5) 0.014(5) 0.004(4) -0.003(5) N4 0.033(5) 0.046(6) 0.053(6) -0.003(5) 0.005(4) -0.001(4) O1 0.055(6) 0.104(9) 0.056(6) 0.006(6) 0.021(5) -0.009(6) N5 0.050(6) 0.058(7) 0.063(7) 0.001(6) 0.021(6) 0.010(5) C14 0.048(7) 0.042(6) 0.044(6) 0.008(5) 0.007(5) 0.005(5) C9 0.043(6) 0.033(6) 0.053(7) 0.001(5) 0.004(5) 0.003(5) C6 0.037(6) 0.058(8) 0.057(7) 0.009(6) 0.015(6) 0.000(5) C15 0.031(5) 0.049(7) 0.045(6) 0.000(5) 0.004(5) -0.005(5) C12 0.042(7) 0.048(7) 0.058(8) -0.004(6) 0.000(6) -0.005(5) C5 0.031(5) 0.043(6) 0.049(6) 0.010(5) 0.009(5) -0.003(5) C18 0.042(7) 0.077(10) 0.047(7) 0.004(7) -0.001(6) 0.010(6) C7 0.038(6) 0.056(7) 0.049(7) 0.003(6) 0.008(5) -0.006(5) C2 0.043(7) 0.054(8) 0.083(10) -0.013(7) 0.007(7) -0.014(6) C13 0.040(6) 0.035(6) 0.057(7) 0.010(5) 0.004(5) 0.001(5) C8 0.039(6) 0.050(7) 0.049(7) 0.006(5) 0.009(5) -0.001(5) C3 0.042(7) 0.075(10) 0.072(10) -0.009(8) 0.026(7) -0.007(7) C10 0.054(7) 0.058(8) 0.042(6) 0.018(6) 0.009(6) 0.006(6) C4 0.039(6) 0.065(8) 0.061(8) -0.008(7) 0.021(6) -0.004(6) C19 0.036(6) 0.069(9) 0.046(7) 0.000(6) 0.000(5) 0.010(6) C11 0.058(8) 0.064(9) 0.041(7) -0.007(6) -0.001(6) -0.001(7) C16 0.038(6) 0.061(8) 0.060(8) 0.010(7) 0.007(6) 0.004(6) C17 0.050(7) 0.072(9) 0.060(8) -0.005(7) 0.022(7) 0.004(7) C1 0.043(8) 0.091(13) 0.100(14) -0.012(11) -0.004(8) 0.006(8) C20 0.063(9) 0.074(10) 0.069(10) 0.003(8) 0.025(8) 0.015(8) C21 0.115(17) 0.092(14) 0.082(13) -0.006(10) 0.049(13) -0.028(12) O3 0.19(2) 0.121(15) 0.116(15) 0.000(11) 0.082(14) 0.021(14) 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' 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 C5 N2 H2 116.3 . . ? C8 N2 H2 116.3 . . ? C8 N2 C5 127.4(11) . . ? C9 N3 C13 117.1(11) . . ? C7 N1 C2 122.7(13) . . ? C3 N1 C7 120.1(11) . . ? C3 N1 C2 117.2(12) . . ? C14 N4 H4 116.9 . . ? C14 N4 C15 126.3(10) . . ? C15 N4 H4 116.9 . . ? C18 N5 C20 118.3(13) . . ? C17 N5 C18 118.7(13) . . ? C17 N5 C20 123.0(12) . . ? O2 C14 N4 123.2(13) . . ? O2 C14 C13 121.3(12) . . ? N4 C14 C13 115.4(11) . . ? N3 C9 C8 116.4(11) . . ? N3 C9 C10 124.2(12) . . ? C10 C9 C8 119.4(12) . . ? C5 C6 H6 120.5 . . ? C7 C6 H6 120.5 . . ? C7 C6 C5 118.9(12) . . ? N4 C15 C19 118.9(11) . . ? N4 C15 C16 122.4(12) . . ? C16 C15 C19 118.7(13) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C11 C12 C13 119.3(12) . . ? N2 C5 C6 117.8(11) . . ? N2 C5 C4 123.8(12) . . ? C4 C5 C6 118.4(11) . . ? N5 C18 H18 119.3 . . ? C19 C18 N5 121.4(13) . . ? C19 C18 H18 119.3 . . ? N1 C7 C6 121.7(13) . . ? N1 C7 H7 119.1 . . ? C6 C7 H7 119.1 . . ? N1 C2 H2A 109.3 . . ? N1 C2 H2B 109.3 . . ? H2A C2 H2B 107.9 . . ? C1 C2 N1 111.8(13) . . ? C1 C2 H2A 109.3 . . ? C1 C2 H2B 109.3 . . ? N3 C13 C14 118.2(12) . . ? N3 C13 C12 122.6(13) . . ? C12 C13 C14 119.2(11) . . ? N2 C8 C9 112.9(11) . . ? O1 C8 N2 126.8(12) . . ? O1 C8 C9 120.3(12) . . ? N1 C3 H3 118.9 . . ? N1 C3 C4 122.2(13) . . ? C4 C3 H3 118.9 . . ? C9 C10 H10 121.4 . . ? C11 C10 C9 117.2(13) . . ? C11 C10 H10 121.4 . . ? C5 C4 H4A 120.7 . . ? C3 C4 C5 118.6(13) . . ? C3 C4 H4A 120.7 . . ? C15 C19 H19 119.8 . . ? C18 C19 C15 120.4(13) . . ? C18 C19 H19 119.8 . . ? C12 C11 C10 119.5(13) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C15 C16 H16 120.8 . . ? C17 C16 C15 118.4(13) . . ? C17 C16 H16 120.8 . . ? N5 C17 C16 122.3(13) . . ? N5 C17 H17 118.9 . . ? C16 C17 H17 118.9 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N5 C20 H20A 109.3 . . ? N5 C20 H20B 109.3 . . ? N5 C20 C21 111.6(15) . . ? H20A C20 H20B 108.0 . . ? C21 C20 H20A 109.3 . . ? C21 C20 H20B 109.3 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? H3A O3 H3B 104.5 . . ? 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 N2 H2 0.8600 . ? N2 C5 1.378(15) . ? N2 C8 1.357(16) . ? N3 C9 1.323(17) . ? N3 C13 1.331(15) . ? N1 C7 1.346(17) . ? N1 C2 1.504(16) . ? N1 C3 1.320(19) . ? O2 C14 1.201(16) . ? N4 H4 0.8600 . ? N4 C14 1.381(16) . ? N4 C15 1.386(17) . ? O1 C8 1.227(16) . ? N5 C18 1.379(18) . ? N5 C17 1.33(2) . ? N5 C20 1.47(2) . ? C14 C13 1.50(2) . ? C9 C8 1.532(17) . ? C9 C10 1.385(19) . ? C6 H6 0.9300 . ? C6 C5 1.403(19) . ? C6 C7 1.361(18) . ? C15 C19 1.394(17) . ? C15 C16 1.386(18) . ? C12 H12 0.9300 . ? C12 C13 1.37(2) . ? C12 C11 1.36(2) . ? C5 C4 1.398(17) . ? C18 H18 0.9300 . ? C18 C19 1.32(2) . ? C7 H7 0.9300 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 C1 1.45(2) . ? C3 H3 0.9300 . ? C3 C4 1.37(2) . ? C10 H10 0.9300 . ? C10 C11 1.37(2) . ? C4 H4A 0.9300 . ? C19 H19 0.9300 . ? C11 H11 0.9300 . ? C16 H16 0.9300 . ? C16 C17 1.37(2) . ? C17 H17 0.9300 . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 C21 1.49(3) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? O3 H3A 0.8498 . ? O3 H3B 0.8500 . ? 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 N2 C5 C4 C3 178.6(14) . . . . ? N3 C9 C8 N2 2.6(16) . . . . ? N3 C9 C8 O1 -179.4(13) . . . . ? N3 C9 C10 C11 3(2) . . . . ? N1 C3 C4 C5 0(2) . . . . ? O2 C14 C13 N3 168.4(13) . . . . ? O2 C14 C13 C12 -9.9(19) . . . . ? N4 C14 C13 N3 -16.0(16) . . . . ? N4 C14 C13 C12 165.7(12) . . . . ? N4 C15 C19 C18 178.4(14) . . . . ? N4 C15 C16 C17 -179.8(13) . . . . ? N5 C18 C19 C15 0(2) . . . . ? C14 N4 C15 C19 163.9(13) . . . . ? C14 N4 C15 C16 -19(2) . . . . ? C9 N3 C13 C14 -176.7(10) . . . . ? C9 N3 C13 C12 1.6(18) . . . . ? C9 C10 C11 C12 -4(2) . . . . ? C6 C5 C4 C3 -1(2) . . . . ? C15 N4 C14 O2 -3(2) . . . . ? C15 N4 C14 C13 -178.9(12) . . . . ? C15 C16 C17 N5 3(2) . . . . ? C5 N2 C8 O1 3(2) . . . . ? C5 N2 C8 C9 -179.4(11) . . . . ? C5 C6 C7 N1 1(2) . . . . ? C18 N5 C17 C16 -1(2) . . . . ? C18 N5 C20 C21 -81(2) . . . . ? C7 N1 C2 C1 99.9(18) . . . . ? C7 N1 C3 C4 2(2) . . . . ? C7 C6 C5 N2 -179.0(12) . . . . ? C7 C6 C5 C4 1(2) . . . . ? C2 N1 C7 C6 179.3(13) . . . . ? C2 N1 C3 C4 -179.6(14) . . . . ? C13 N3 C9 C8 176.9(10) . . . . ? C13 N3 C9 C10 -1.5(18) . . . . ? C13 C12 C11 C10 4(2) . . . . ? C8 N2 C5 C6 172.1(13) . . . . ? C8 N2 C5 C4 -8(2) . . . . ? C8 C9 C10 C11 -175.8(12) . . . . ? C3 N1 C7 C6 -3(2) . . . . ? C3 N1 C2 C1 -78(2) . . . . ? C10 C9 C8 N2 -178.9(11) . . . . ? C10 C9 C8 O1 -1(2) . . . . ? C19 C15 C16 C17 -3(2) . . . . ? C11 C12 C13 N3 -3(2) . . . . ? C11 C12 C13 C14 175.4(13) . . . . ? C16 C15 C19 C18 1(2) . . . . ? C17 N5 C18 C19 0(2) . . . . ? C17 N5 C20 C21 99(2) . . . . ? C20 N5 C18 C19 179.6(15) . . . . ? C20 N5 C17 C16 178.8(15) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.893(3) 2 0.107(3)