#------------------------------------------------------------------------------ #$Date: 2023-11-30 04:23:03 +0200 (Thu, 30 Nov 2023) $ #$Revision: 287874 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/78/7247801.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_7247801 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 '0.5(Cl), 0.5(C31 H25 Cl N5 O2 Pd)' _chemical_formula_sum 'C15.5 H12.5 Cl N2.5 O Pd0.5' _chemical_formula_weight 338.43 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _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 86.5890(10) _cell_angle_beta 73.2160(10) _cell_angle_gamma 76.0760(10) _cell_formula_units_Z 4 _cell_length_a 9.5070(4) _cell_length_b 11.2651(5) _cell_length_c 13.3444(5) _cell_measurement_reflns_used 1750 _cell_measurement_temperature 100.0 _cell_measurement_theta_max 29.60 _cell_measurement_theta_min 2.30 _cell_volume 1327.99(10) _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 100.0 _diffrn_detector CPAD _diffrn_detector_area_resol_mean 7.41 _diffrn_detector_type 'Bruker PHOTON II' _diffrn_measured_fraction_theta_full 0.855 _diffrn_measured_fraction_theta_max 0.661 _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_R_equivalents 0.0437 _diffrn_reflns_av_unetI/netI 0.0788 _diffrn_reflns_Laue_measured_fraction_full 0.855 _diffrn_reflns_Laue_measured_fraction_max 0.661 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 8475 _diffrn_reflns_point_group_measured_fraction_full 0.855 _diffrn_reflns_point_group_measured_fraction_max 0.661 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 29.653 _diffrn_reflns_theta_min 2.301 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type 'Incoatec I\ms' _exptl_absorpt_coefficient_mu 0.941 _exptl_absorpt_correction_T_max 0.6690 _exptl_absorpt_correction_T_min 0.5845 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1036 before and 0.0528 after correction. The Ratio of minimum to maximum transmission is 0.8737. The \l/2 correction factor is Not present. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.693 _exptl_crystal_description block _exptl_crystal_F_000 684 _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _refine_diff_density_max 1.072 _refine_diff_density_min -1.162 _refine_diff_density_rms 0.146 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 370 _refine_ls_number_reflns 4965 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.086 _refine_ls_R_factor_all 0.0783 _refine_ls_R_factor_gt 0.0461 _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^)+4.7677P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0855 _refine_ls_wR_factor_ref 0.1073 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3744 _reflns_number_total 4965 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ra06477h2.cif _cod_data_source_block 4a_komal_navedzafar_qau_0ma_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_original_formula_sum 'C15.50 H12.50 Cl N2.50 O Pd0.50' _cod_database_code 7247801 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2.a Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C25(H25A,H25B) 2.b Aromatic/amide H refined with riding coordinates: C21(H21), C22(H22), C9(H9), C11(H11), C8(H8), C16(H16), C29(H29), C15(H15), C2(H2), C31(H31), C24(H24), C17(H17), C30(H30), C23(H23), C6(H6), C12(H12), C27(H27), C3(H3), C5(H5), C28(H28), C4(H4) ; _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 0.785 _shelx_estimated_absorpt_t_max 0.864 _diffrn_measurement_ambient_temperature_device_make 'Oxford Cobra Cryo device' _shelx_res_file ; TITL 4A_Komal_Navedzafar_QAU_0ma_a.res in P-1 4a_komal_navedzafar_qau_0ma_a.res created by SHELXL-2018/3 at 16:25:56 on 15-Jul-2023 REM Old TITL 4A_Komal_Navedzafar_QAU_0ma in P-1 REM SHELXT solution in P-1 REM R1 0.173, Rweak 0.006, Alpha 0.037, Orientation as input REM Formula found by SHELXT: C34 Ni O6 CELL 0.71073 9.507 11.2651 13.3444 86.589 73.216 76.076 ZERR 4 0.0004 0.0005 0.0005 0.001 0.001 0.001 LATT 1 SFAC C H Cl N O Pd UNIT 62 50 4 10 4 2 L.S. 20 PLAN 5 SIZE 0.16 0.22 0.27 TEMP -173.15 CONF LIST 6 MORE -1 BOND $H fmap 2 acta 50 OMIT 11 0 6 OMIT 1 0 4 OMIT 11 1 3 OMIT 10 0 1 OMIT 11 3 11 OMIT 10 1 1 OMIT 11 6 4 OMIT -1 3 5 OMIT 11 5 2 OMIT 11 4 6 OMIT -4 9 8 OMIT -7 3 10 OMIT 11 3 8 OMIT 12 8 2 OMIT 11 2 3 OMIT 11 5 7 OMIT 4 2 16 OMIT 12 7 4 OMIT 11 4 3 OMIT 11 2 0 OMIT 12 4 7 OMIT 11 9 2 OMIT 11 -1 6 OMIT 11 1 0 OMIT -8 4 7 OMIT 9 -3 2 OMIT -9 3 0 OMIT 11 1 6 OMIT 11 -1 5 OMIT 12 6 4 OMIT 11 0 3 OMIT 12 4 1 OMIT 11 3 1 OMIT 11 3 6 OMIT 11 6 3 OMIT 11 -1 8 OMIT 11 4 8 OMIT 11 1 10 OMIT 11 4 9 OMIT 11 2 11 OMIT -10 -3 3 OMIT 8 -6 5 OMIT 11 5 6 OMIT 10 -1 2 OMIT 11 -1 9 OMIT 11 0 2 OMIT -11 -3 2 OMIT 9 -5 3 OMIT -10 3 1 OMIT 11 7 4 OMIT -2 2 1 OMIT -10 2 4 OMIT 8 -2 2 OMIT -10 1 4 OMIT 11 -1 1 OMIT 12 2 4 OMIT 11 0 8 OMIT 11 1 2 OMIT 12 9 2 OMIT 11 2 10 OMIT 12 4 3 OMIT 11 5 5 OMIT 11 1 7 OMIT 7 7 16 OMIT 10 -1 1 OMIT 11 5 8 OMIT -3 2 14 OMIT 11 5 3 OMIT -9 2 1 OMIT 11 2 1 OMIT 11 1 5 OMIT -9 1 4 OMIT 12 3 1 OMIT 12 5 4 OMIT 9 -4 2 OMIT 10 0 15 OMIT 12 4 6 OMIT 9 -7 5 OMIT 11 3 7 OMIT 11 -2 5 OMIT 11 -1 4 OMIT 2 10 4 OMIT 12 2 1 OMIT 2 10 1 OMIT 11 -2 3 OMIT -1 0 16 OMIT 11 4 5 OMIT 10 7 3 OMIT 10 -4 5 OMIT 11 -1 7 OMIT -11 0 2 OMIT -6 5 7 OMIT 10 -3 3 OMIT 11 2 7 OMIT 10 -5 3 OMIT 11 3 9 OMIT 10 -4 6 OMIT -10 0 2 OMIT 2 10 13 OMIT -9 2 5 OMIT 9 -5 4 OMIT -10 0 3 OMIT 10 6 3 OMIT -10 2 0 OMIT -10 0 1 OMIT 11 8 2 OMIT -10 1 3 OMIT 11 3 4 OMIT 11 0 10 OMIT 11 0 9 OMIT -10 3 2 OMIT 11 1 11 OMIT -3 8 8 OMIT 11 5 10 OMIT 12 7 2 OMIT 8 -4 4 OMIT 10 -5 4 OMIT 12 3 6 OMIT -11 0 3 OMIT -10 2 1 OMIT 11 4 12 OMIT -9 1 5 OMIT 12 2 0 OMIT 11 -2 7 OMIT 1 11 10 OMIT 7 10 14 OMIT 9 2 7 OMIT 10 -3 1 OMIT -1 6 14 OMIT 11 5 9 OMIT -12 -2 1 OMIT 5 -12 2 OMIT 10 -2 2 OMIT -11 -1 1 OMIT 11 3 12 OMIT 11 0 1 OMIT -5 -1 4 OMIT -10 1 0 OMIT 2 2 13 OMIT 11 7 3 OMIT 5 3 17 OMIT 8 7 16 OMIT 2 4 15 OMIT 12 6 2 OMIT 10 -4 4 OMIT 7 -4 9 OMIT 8 -9 8 OMIT 10 -3 12 OMIT 9 -6 11 OMIT 6 -1 2 REM REM REM WGHT 0.000000 4.767700 FVAR 0.63300 CL2 3 0.382309 0.333990 0.451069 11.00000 0.02985 0.02735 = 0.02860 0.00042 -0.01462 -0.00684 O4 5 0.164186 0.693617 1.010726 11.00000 0.01162 0.02326 = 0.02198 -0.00776 0.00049 -0.00521 CL1 3 0.740480 0.429810 0.770932 11.00000 0.01794 0.01617 = 0.02319 -0.00376 -0.00431 -0.00363 N4 4 0.399332 0.589354 0.906458 11.00000 0.01021 0.01510 = 0.01668 0.00032 -0.00279 -0.00604 PD1 6 0.617741 0.611439 0.860230 11.00000 0.01296 0.01480 = 0.01585 -0.00101 -0.00303 -0.00610 O2 5 0.861657 0.839623 0.919450 11.00000 0.01828 0.03192 = 0.02802 -0.00771 -0.00148 -0.01501 N2 4 0.800755 0.686127 0.841012 11.00000 0.01214 0.01818 = 0.01841 0.00070 -0.00382 -0.00993 N3 4 0.526559 0.743364 0.962479 11.00000 0.02123 0.01880 = 0.01273 0.00181 -0.00505 -0.01352 N1 4 1.165956 0.657530 0.573263 11.00000 0.01737 0.01844 = 0.01714 0.00257 -0.00415 -0.00709 N5 4 0.214632 0.360989 0.773764 11.00000 0.00759 0.01420 = 0.02285 -0.00357 -0.00735 0.00139 C21 1 0.215569 0.463825 0.922982 11.00000 0.01496 0.01186 = 0.01769 -0.00109 -0.00478 -0.00237 AFIX 43 H21 2 0.173288 0.482921 0.995486 11.00000 -1.20000 AFIX 0 C14 1 0.618320 0.803518 0.985074 11.00000 0.02048 0.01108 = 0.01873 0.00070 -0.00898 -0.00424 C20 1 0.337383 0.511343 0.864841 11.00000 0.01642 0.01399 = 0.01837 0.00355 -0.01242 -0.00237 C22 1 0.156831 0.390188 0.876444 11.00000 0.01305 0.01655 = 0.02195 0.00210 -0.00514 -0.00593 AFIX 43 H22 2 0.073897 0.359065 0.917129 11.00000 -1.20000 AFIX 0 C19 1 0.301798 0.674369 0.980656 11.00000 0.01802 0.01202 = 0.02323 0.00154 -0.00550 -0.00586 C1 1 1.239986 0.804223 0.437765 11.00000 0.01644 0.01909 = 0.01570 -0.00313 0.00290 -0.00516 C18 1 0.383694 0.753413 1.017953 11.00000 0.01056 0.01447 = 0.01461 0.00151 -0.00280 -0.00468 C13 1 0.775619 0.778244 0.912769 11.00000 0.01388 0.01266 = 0.02170 0.00002 -0.00714 -0.00507 C9 1 1.065495 0.695544 0.755515 11.00000 0.01517 0.01656 = 0.01873 -0.00050 -0.00475 -0.00409 AFIX 43 H9 2 1.079235 0.716744 0.819320 11.00000 -1.20000 AFIX 0 C11 1 0.921039 0.628980 0.659051 11.00000 0.01184 0.01804 = 0.02038 -0.00130 -0.00406 -0.00624 AFIX 43 H11 2 0.833442 0.604757 0.655678 11.00000 -1.20000 AFIX 0 C8 1 1.178805 0.690689 0.664701 11.00000 0.01328 0.02047 = 0.01839 0.00211 -0.00747 -0.00531 AFIX 43 H8 2 1.269412 0.711328 0.666087 11.00000 -1.20000 AFIX 0 C10 1 0.929027 0.669432 0.755141 11.00000 0.01716 0.01230 = 0.02040 0.00232 -0.00575 -0.00511 C16 1 0.416642 0.897045 1.129662 11.00000 0.02468 0.01808 = 0.01947 -0.00866 -0.00637 -0.00487 AFIX 43 H16 2 0.378329 0.950268 1.188924 11.00000 -1.20000 AFIX 0 C29 1 0.298249 -0.098020 0.792824 11.00000 0.03201 0.01765 = 0.02867 -0.00158 -0.01444 -0.00719 AFIX 43 H29 2 0.331142 -0.182221 0.806859 11.00000 -1.20000 AFIX 0 C7 1 1.280033 0.674034 0.473528 11.00000 0.01664 0.02375 = 0.01713 -0.00004 0.00045 -0.00548 AFIX 23 H7A 2 1.281484 0.616949 0.419430 11.00000 -1.20000 H7B 2 1.381786 0.655898 0.484320 11.00000 -1.20000 AFIX 0 C15 1 0.564558 0.882710 1.070338 11.00000 0.01681 0.01812 = 0.02093 -0.00454 -0.00543 -0.00731 AFIX 43 H15 2 0.628574 0.926315 1.087552 11.00000 -1.20000 AFIX 0 C25 1 0.147321 0.280650 0.725356 11.00000 0.01986 0.01957 = 0.03203 -0.00442 -0.01360 -0.01093 AFIX 23 H25A 2 0.176035 0.291213 0.648494 11.00000 -1.20000 H25B 2 0.035767 0.305209 0.751801 11.00000 -1.20000 AFIX 0 C2 1 1.296623 0.892456 0.470538 11.00000 0.01899 0.02703 = 0.01880 0.00279 -0.00526 -0.00825 AFIX 43 H2 2 1.365905 0.869887 0.511211 11.00000 -1.20000 AFIX 0 C26 1 0.200862 0.148032 0.750427 11.00000 0.02011 0.01586 = 0.02289 -0.00308 -0.00771 -0.00829 C31 1 0.335312 0.078213 0.687363 11.00000 0.01799 0.02298 = 0.01655 -0.00333 -0.00091 -0.00934 AFIX 43 H31 2 0.393565 0.114739 0.629158 11.00000 -1.20000 AFIX 0 C24 1 0.397721 0.475711 0.759148 11.00000 0.01348 0.01557 = 0.01854 0.00302 -0.00412 -0.00359 AFIX 43 H24 2 0.483414 0.502680 0.717490 11.00000 -1.20000 AFIX 0 C17 1 0.322431 0.833811 1.103287 11.00000 0.01893 0.01964 = 0.02049 -0.00046 -0.00429 -0.00630 AFIX 43 H17 2 0.219304 0.845326 1.142506 11.00000 -1.20000 AFIX 0 C30 1 0.385309 -0.044527 0.708665 11.00000 0.02475 0.02528 = 0.02628 -0.01159 -0.00302 -0.00522 AFIX 43 H30 2 0.478142 -0.091407 0.666080 11.00000 -1.20000 AFIX 0 C23 1 0.334732 0.402420 0.715018 11.00000 0.01332 0.01745 = 0.02020 -0.00417 -0.00517 -0.00429 AFIX 43 H23 2 0.375646 0.380707 0.642935 11.00000 -1.20000 AFIX 0 C6 1 1.136758 0.838551 0.379909 11.00000 0.02163 0.02347 = 0.01674 -0.00461 -0.00403 -0.00087 AFIX 43 H6 2 1.096949 0.778406 0.357676 11.00000 -1.20000 AFIX 0 C12 1 1.038445 0.624838 0.571891 11.00000 0.02338 0.02029 = 0.02162 -0.00269 -0.00649 -0.01075 AFIX 43 H12 2 1.031162 0.598163 0.507751 11.00000 -1.20000 AFIX 0 C27 1 0.116999 0.093221 0.835749 11.00000 0.01431 0.02413 = 0.02373 -0.00723 -0.00442 -0.00951 AFIX 43 H27 2 0.026404 0.140713 0.880365 11.00000 -1.20000 AFIX 0 C3 1 1.252317 1.013756 0.444051 11.00000 0.02880 0.02113 = 0.02931 -0.00606 0.00111 -0.00898 AFIX 43 H3 2 1.292675 1.074116 0.465403 11.00000 -1.20000 AFIX 0 C5 1 1.091540 0.959946 0.354452 11.00000 0.03067 0.03592 = 0.01495 0.00040 -0.00501 0.00087 AFIX 43 H5 2 1.020781 0.982965 0.314934 11.00000 -1.20000 AFIX 0 C28 1 0.164203 -0.029946 0.856367 11.00000 0.02245 0.02166 = 0.02547 -0.00130 -0.00526 -0.01356 AFIX 43 H28 2 0.104989 -0.067123 0.913586 11.00000 -1.20000 AFIX 0 C4 1 1.148950 1.046929 0.386313 11.00000 0.03505 0.02433 = 0.02132 0.00128 0.00101 -0.00217 AFIX 43 H4 2 1.117847 1.130208 0.368796 11.00000 -1.20000 AFIX 0 HKLF 4 REM 4A_Komal_Navedzafar_QAU_0ma_a.res in P-1 REM wR2 = 0.1073, GooF = S = 1.086, Restrained GooF = 1.086 for all data REM R1 = 0.0461 for 3744 Fo > 4sig(Fo) and 0.0783 for all 4965 data REM 370 parameters refined using 0 restraints END WGHT 0.0000 4.7677 REM Highest difference peak 1.072, deepest hole -1.162, 1-sigma level 0.146 Q1 1 1.1459 1.1661 0.4224 11.00000 0.05 1.07 Q2 1 0.5234 0.7129 0.9035 11.00000 0.05 1.05 Q3 1 0.9723 0.6562 0.4940 11.00000 0.05 0.91 Q4 1 0.3808 0.4482 0.8364 11.00000 0.05 0.90 Q5 1 0.7387 0.5186 0.8142 11.00000 0.05 0.75 ; _shelx_res_checksum 87611 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 Cl2 Cl 0.38231(16) 0.33399(13) 0.45107(11) 0.0272(3) Uani 1 1 d . . . . . O4 O 0.1642(4) 0.6936(3) 1.0107(3) 0.0195(8) Uani 1 1 d . . . . . Cl1 Cl 0.74048(14) 0.42981(11) 0.77093(10) 0.0193(3) Uani 1 1 d . . . . . N4 N 0.3993(4) 0.5894(4) 0.9065(3) 0.0137(8) Uani 1 1 d . . . . . Pd1 Pd 0.61774(4) 0.61144(3) 0.86023(3) 0.01420(12) Uani 1 1 d . . . . . O2 O 0.8617(4) 0.8396(3) 0.9194(3) 0.0252(9) Uani 1 1 d . . . . . N2 N 0.8008(4) 0.6861(4) 0.8410(3) 0.0152(9) Uani 1 1 d . . . . . N3 N 0.5266(5) 0.7434(4) 0.9625(3) 0.0160(9) Uani 1 1 d . . . . . N1 N 1.1660(5) 0.6575(4) 0.5733(3) 0.0174(9) Uani 1 1 d . . . . . N5 N 0.2146(4) 0.3610(4) 0.7738(3) 0.0148(9) Uani 1 1 d . . . . . C21 C 0.2156(5) 0.4638(4) 0.9230(4) 0.0149(10) Uani 1 1 d . . . . . H21 H 0.173288 0.482921 0.995486 0.018 Uiso 1 1 calc R U . . . C14 C 0.6183(6) 0.8035(4) 0.9851(4) 0.0159(10) Uani 1 1 d . . . . . C20 C 0.3374(6) 0.5113(4) 0.8648(4) 0.0150(10) Uani 1 1 d . . . . . C22 C 0.1568(6) 0.3902(4) 0.8764(4) 0.0168(11) Uani 1 1 d . . . . . H22 H 0.073897 0.359065 0.917129 0.020 Uiso 1 1 calc R U . . . C19 C 0.3018(6) 0.6744(4) 0.9807(4) 0.0175(11) Uani 1 1 d . . . . . C1 C 1.2400(6) 0.8042(5) 0.4378(4) 0.0184(11) Uani 1 1 d . . . . . C18 C 0.3837(5) 0.7534(4) 1.0180(4) 0.0131(10) Uani 1 1 d . . . . . C13 C 0.7756(5) 0.7782(4) 0.9128(4) 0.0153(10) Uani 1 1 d . . . . . C9 C 1.0655(5) 0.6955(4) 0.7555(4) 0.0167(11) Uani 1 1 d . . . . . H9 H 1.079235 0.716744 0.819320 0.020 Uiso 1 1 calc R U . . . C11 C 0.9210(5) 0.6290(4) 0.6591(4) 0.0163(10) Uani 1 1 d . . . . . H11 H 0.833442 0.604757 0.655678 0.020 Uiso 1 1 calc R U . . . C8 C 1.1788(6) 0.6907(4) 0.6647(4) 0.0166(11) Uani 1 1 d . . . . . H8 H 1.269412 0.711328 0.666087 0.020 Uiso 1 1 calc R U . . . C10 C 0.9290(6) 0.6694(4) 0.7551(4) 0.0163(10) Uani 1 1 d . . . . . C16 C 0.4166(6) 0.8970(5) 1.1297(4) 0.0204(11) Uani 1 1 d . . . . . H16 H 0.378329 0.950268 1.188924 0.024 Uiso 1 1 calc R U . . . C29 C 0.2982(6) -0.0980(5) 0.7928(4) 0.0245(12) Uani 1 1 d . . . . . H29 H 0.331142 -0.182221 0.806859 0.029 Uiso 1 1 calc R U . . . C7 C 1.2800(6) 0.6740(5) 0.4735(4) 0.0202(11) Uani 1 1 d . . . . . H7A H 1.281484 0.616949 0.419430 0.024 Uiso 1 1 calc R U . . . H7B H 1.381786 0.655898 0.484320 0.024 Uiso 1 1 calc R U . . . C15 C 0.5646(6) 0.8827(5) 1.0703(4) 0.0178(11) Uani 1 1 d . . . . . H15 H 0.628574 0.926315 1.087552 0.021 Uiso 1 1 calc R U . . . C25 C 0.1473(6) 0.2807(5) 0.7254(4) 0.0211(12) Uani 1 1 d . . . . . H25A H 0.176035 0.291213 0.648494 0.025 Uiso 1 1 calc R U . . . H25B H 0.035767 0.305209 0.751801 0.025 Uiso 1 1 calc R U . . . C2 C 1.2966(6) 0.8925(5) 0.4705(4) 0.0212(12) Uani 1 1 d . . . . . H2 H 1.365905 0.869887 0.511211 0.025 Uiso 1 1 calc R U . . . C26 C 0.2009(6) 0.1480(5) 0.7504(4) 0.0184(11) Uani 1 1 d . . . . . C31 C 0.3353(6) 0.0782(5) 0.6874(4) 0.0191(11) Uani 1 1 d . . . . . H31 H 0.393565 0.114739 0.629158 0.023 Uiso 1 1 calc R U . . . C24 C 0.3977(5) 0.4757(4) 0.7591(4) 0.0160(10) Uani 1 1 d . . . . . H24 H 0.483414 0.502680 0.717490 0.019 Uiso 1 1 calc R U . . . C17 C 0.3224(6) 0.8338(5) 1.1033(4) 0.0196(11) Uani 1 1 d . . . . . H17 H 0.219304 0.845326 1.142506 0.024 Uiso 1 1 calc R U . . . C30 C 0.3853(6) -0.0445(5) 0.7087(4) 0.0259(13) Uani 1 1 d . . . . . H30 H 0.478142 -0.091407 0.666080 0.031 Uiso 1 1 calc R U . . . C23 C 0.3347(5) 0.4024(4) 0.7150(4) 0.0166(11) Uani 1 1 d . . . . . H23 H 0.375646 0.380707 0.642935 0.020 Uiso 1 1 calc R U . . . C6 C 1.1368(6) 0.8386(5) 0.3799(4) 0.0215(11) Uani 1 1 d . . . . . H6 H 1.096949 0.778406 0.357676 0.026 Uiso 1 1 calc R U . . . C12 C 1.0384(6) 0.6248(5) 0.5719(4) 0.0206(11) Uani 1 1 d . . . . . H12 H 1.031162 0.598163 0.507751 0.025 Uiso 1 1 calc R U . . . C27 C 0.1170(6) 0.0932(5) 0.8357(4) 0.0197(11) Uani 1 1 d . . . . . H27 H 0.026404 0.140713 0.880365 0.024 Uiso 1 1 calc R U . . . C3 C 1.2523(6) 1.0138(5) 0.4441(4) 0.0276(13) Uani 1 1 d . . . . . H3 H 1.292675 1.074116 0.465403 0.033 Uiso 1 1 calc R U . . . C5 C 1.0915(7) 0.9599(5) 0.3545(4) 0.0290(13) Uani 1 1 d . . . . . H5 H 1.020781 0.982965 0.314934 0.035 Uiso 1 1 calc R U . . . C28 C 0.1642(6) -0.0299(5) 0.8564(4) 0.0220(12) Uani 1 1 d . . . . . H28 H 0.104989 -0.067123 0.913586 0.026 Uiso 1 1 calc R U . . . C4 C 1.1489(7) 1.0469(5) 0.3863(4) 0.0297(14) Uani 1 1 d . . . . . H4 H 1.117847 1.130208 0.368796 0.036 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 Cl2 0.0299(7) 0.0273(7) 0.0286(7) 0.0004(6) -0.0146(6) -0.0068(6) O4 0.0116(18) 0.023(2) 0.0220(19) -0.0078(15) 0.0005(15) -0.0052(15) Cl1 0.0179(6) 0.0162(6) 0.0232(6) -0.0038(5) -0.0043(5) -0.0036(5) N4 0.010(2) 0.015(2) 0.017(2) 0.0003(16) -0.0028(17) -0.0060(17) Pd1 0.0130(2) 0.0148(2) 0.0158(2) -0.00101(14) -0.00303(15) -0.00610(15) O2 0.0183(19) 0.032(2) 0.028(2) -0.0077(17) -0.0015(17) -0.0150(18) N2 0.012(2) 0.018(2) 0.018(2) 0.0007(17) -0.0038(17) -0.0099(18) N3 0.021(2) 0.019(2) 0.013(2) 0.0018(17) -0.0050(18) -0.0135(19) N1 0.017(2) 0.018(2) 0.017(2) 0.0026(17) -0.0041(18) -0.0071(19) N5 0.008(2) 0.014(2) 0.023(2) -0.0036(17) -0.0074(17) 0.0014(17) C21 0.015(2) 0.012(2) 0.018(2) -0.0011(19) -0.005(2) -0.002(2) C14 0.020(3) 0.011(2) 0.019(3) 0.001(2) -0.009(2) -0.004(2) C20 0.016(3) 0.014(3) 0.018(2) 0.0036(19) -0.012(2) -0.002(2) C22 0.013(2) 0.017(3) 0.022(3) 0.002(2) -0.005(2) -0.006(2) C19 0.018(3) 0.012(3) 0.023(3) 0.002(2) -0.006(2) -0.006(2) C1 0.016(3) 0.019(3) 0.016(2) -0.003(2) 0.003(2) -0.005(2) C18 0.011(2) 0.014(2) 0.015(2) 0.0015(19) -0.0028(19) -0.005(2) C13 0.014(2) 0.013(2) 0.022(3) 0.000(2) -0.007(2) -0.005(2) C9 0.015(3) 0.017(3) 0.019(3) -0.001(2) -0.005(2) -0.004(2) C11 0.012(2) 0.018(3) 0.020(3) -0.001(2) -0.004(2) -0.006(2) C8 0.013(2) 0.020(3) 0.018(3) 0.002(2) -0.007(2) -0.005(2) C10 0.017(3) 0.012(2) 0.020(3) 0.002(2) -0.006(2) -0.005(2) C16 0.025(3) 0.018(3) 0.019(3) -0.009(2) -0.006(2) -0.005(2) C29 0.032(3) 0.018(3) 0.029(3) -0.002(2) -0.014(3) -0.007(2) C7 0.017(3) 0.024(3) 0.017(3) 0.000(2) 0.000(2) -0.005(2) C15 0.017(3) 0.018(3) 0.021(3) -0.005(2) -0.005(2) -0.007(2) C25 0.020(3) 0.020(3) 0.032(3) -0.004(2) -0.014(2) -0.011(2) C2 0.019(3) 0.027(3) 0.019(3) 0.003(2) -0.005(2) -0.008(2) C26 0.020(3) 0.016(3) 0.023(3) -0.003(2) -0.008(2) -0.008(2) C31 0.018(3) 0.023(3) 0.017(2) -0.003(2) -0.001(2) -0.009(2) C24 0.013(2) 0.016(3) 0.019(2) 0.003(2) -0.004(2) -0.004(2) C17 0.019(3) 0.020(3) 0.020(3) 0.000(2) -0.004(2) -0.006(2) C30 0.025(3) 0.025(3) 0.026(3) -0.012(2) -0.003(2) -0.005(3) C23 0.013(2) 0.017(3) 0.020(3) -0.004(2) -0.005(2) -0.004(2) C6 0.022(3) 0.023(3) 0.017(3) -0.005(2) -0.004(2) -0.001(2) C12 0.023(3) 0.020(3) 0.022(3) -0.003(2) -0.006(2) -0.011(2) C27 0.014(3) 0.024(3) 0.024(3) -0.007(2) -0.004(2) -0.010(2) C3 0.029(3) 0.021(3) 0.029(3) -0.006(2) 0.001(3) -0.009(3) C5 0.031(3) 0.036(3) 0.015(3) 0.000(2) -0.005(2) 0.001(3) C28 0.022(3) 0.022(3) 0.025(3) -0.001(2) -0.005(2) -0.014(2) C4 0.035(3) 0.024(3) 0.021(3) 0.001(2) 0.001(3) -0.002(3) 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' Cl Cl 0.1484 0.1585 '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' Pd Pd -0.9988 1.0072 '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 C20 N4 Pd1 128.5(3) . . ? C19 N4 Pd1 113.5(3) . . ? C19 N4 C20 117.6(4) . . ? N4 Pd1 Cl1 100.09(11) . . ? N2 Pd1 Cl1 98.74(12) . . ? N2 Pd1 N4 161.16(16) . . ? N3 Pd1 Cl1 166.74(12) . . ? N3 Pd1 N4 80.74(16) . . ? N3 Pd1 N2 80.84(16) . . ? C13 N2 Pd1 113.4(3) . . ? C13 N2 C10 118.9(4) . . ? C10 N2 Pd1 126.5(3) . . ? C14 N3 Pd1 117.3(3) . . ? C18 N3 Pd1 117.8(3) . . ? C18 N3 C14 123.8(4) . . ? C8 N1 C7 120.0(4) . . ? C8 N1 C12 119.0(4) . . ? C12 N1 C7 120.4(4) . . ? C22 N5 C25 119.7(4) . . ? C22 N5 C23 120.3(4) . . ? C23 N5 C25 120.0(4) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C22 C21 C20 120.7(5) . . ? N3 C14 C13 115.2(4) . . ? N3 C14 C15 119.6(5) . . ? C15 C14 C13 125.3(4) . . ? N4 C20 C21 123.6(4) . . ? N4 C20 C24 119.9(4) . . ? C21 C20 C24 116.6(4) . . ? N5 C22 C21 121.1(5) . . ? N5 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? O4 C19 N4 127.3(5) . . ? O4 C19 C18 120.7(4) . . ? N4 C19 C18 111.9(4) . . ? C2 C1 C7 119.6(5) . . ? C2 C1 C6 119.5(5) . . ? C6 C1 C7 120.7(5) . . ? N3 C18 C19 115.1(4) . . ? N3 C18 C17 119.2(4) . . ? C17 C18 C19 125.8(5) . . ? O2 C13 N2 128.0(5) . . ? O2 C13 C14 119.7(4) . . ? N2 C13 C14 112.2(4) . . ? C8 C9 H9 119.9 . . ? C8 C9 C10 120.3(5) . . ? C10 C9 H9 119.9 . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C12 C11 C10 119.9(5) . . ? N1 C8 C9 121.8(5) . . ? N1 C8 H8 119.1 . . ? C9 C8 H8 119.1 . . ? N2 C10 C9 124.4(4) . . ? N2 C10 C11 118.8(4) . . ? C9 C10 C11 116.7(4) . . ? C15 C16 H16 119.8 . . ? C15 C16 C17 120.4(5) . . ? C17 C16 H16 119.8 . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C28 C29 C30 120.7(5) . . ? N1 C7 C1 109.1(4) . . ? N1 C7 H7A 109.9 . . ? N1 C7 H7B 109.9 . . ? C1 C7 H7A 109.9 . . ? C1 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? C14 C15 H15 120.6 . . ? C16 C15 C14 118.7(5) . . ? C16 C15 H15 120.6 . . ? N5 C25 H25A 109.4 . . ? N5 C25 H25B 109.4 . . ? N5 C25 C26 111.1(4) . . ? H25A C25 H25B 108.0 . . ? C26 C25 H25A 109.4 . . ? C26 C25 H25B 109.4 . . ? C1 C2 H2 120.0 . . ? C1 C2 C3 120.0(5) . . ? C3 C2 H2 120.0 . . ? C31 C26 C25 119.9(5) . . ? C31 C26 C27 119.0(5) . . ? C27 C26 C25 121.1(5) . . ? C26 C31 H31 119.7 . . ? C30 C31 C26 120.7(5) . . ? C30 C31 H31 119.7 . . ? C20 C24 H24 119.5 . . ? C23 C24 C20 121.0(5) . . ? C23 C24 H24 119.5 . . ? C18 C17 C16 118.3(5) . . ? C18 C17 H17 120.9 . . ? C16 C17 H17 120.9 . . ? C29 C30 C31 119.4(5) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? N5 C23 C24 120.3(5) . . ? N5 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C1 C6 H6 119.8 . . ? C5 C6 C1 120.4(5) . . ? C5 C6 H6 119.8 . . ? N1 C12 H12 119.0 . . ? C11 C12 N1 122.1(5) . . ? C11 C12 H12 119.0 . . ? C26 C27 H27 119.6 . . ? C28 C27 C26 120.8(5) . . ? C28 C27 H27 119.6 . . ? C2 C3 H3 120.0 . . ? C2 C3 C4 119.9(5) . . ? C4 C3 H3 120.0 . . ? C6 C5 H5 120.0 . . ? C4 C5 C6 120.0(5) . . ? C4 C5 H5 120.0 . . ? C29 C28 C27 119.4(5) . . ? C29 C28 H28 120.3 . . ? C27 C28 H28 120.3 . . ? C3 C4 H4 119.9 . . ? C5 C4 C3 120.2(5) . . ? C5 C4 H4 119.9 . . ? 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 O4 C19 1.221(6) . ? Cl1 Pd1 2.3035(12) . ? N4 Pd1 2.060(4) . ? N4 C20 1.387(6) . ? N4 C19 1.383(6) . ? Pd1 N2 2.055(4) . ? Pd1 N3 1.939(4) . ? O2 C13 1.215(6) . ? N2 C13 1.385(6) . ? N2 C10 1.394(6) . ? N3 C14 1.331(6) . ? N3 C18 1.327(6) . ? N1 C8 1.344(6) . ? N1 C7 1.489(6) . ? N1 C12 1.354(6) . ? N5 C22 1.349(6) . ? N5 C25 1.494(6) . ? N5 C23 1.354(6) . ? C21 H21 0.9500 . ? C21 C20 1.400(7) . ? C21 C22 1.368(7) . ? C14 C13 1.498(7) . ? C14 C15 1.385(7) . ? C20 C24 1.403(7) . ? C22 H22 0.9500 . ? C19 C18 1.502(7) . ? C1 C7 1.509(7) . ? C1 C2 1.384(7) . ? C1 C6 1.389(7) . ? C18 C17 1.394(7) . ? C9 H9 0.9500 . ? C9 C8 1.363(7) . ? C9 C10 1.399(7) . ? C11 H11 0.9500 . ? C11 C10 1.414(7) . ? C11 C12 1.354(7) . ? C8 H8 0.9500 . ? C16 H16 0.9500 . ? C16 C15 1.376(7) . ? C16 C17 1.397(7) . ? C29 H29 0.9500 . ? C29 C30 1.390(8) . ? C29 C28 1.384(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C15 H15 0.9500 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C25 C26 1.509(7) . ? C2 H2 0.9500 . ? C2 C3 1.386(7) . ? C26 C31 1.391(7) . ? C26 C27 1.394(7) . ? C31 H31 0.9500 . ? C31 C30 1.391(7) . ? C24 H24 0.9500 . ? C24 C23 1.374(7) . ? C17 H17 0.9500 . ? C30 H30 0.9500 . ? C23 H23 0.9500 . ? C6 H6 0.9500 . ? C6 C5 1.384(8) . ? C12 H12 0.9500 . ? C27 H27 0.9500 . ? C27 C28 1.389(7) . ? C3 H3 0.9500 . ? C3 C4 1.388(8) . ? C5 H5 0.9500 . ? C5 C4 1.371(8) . ? C28 H28 0.9500 . ? C4 H4 0.9500 . ? 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 O4 C19 C18 N3 -164.7(4) . . . . ? O4 C19 C18 C17 15.1(8) . . . . ? N4 C20 C24 C23 -177.4(4) . . . . ? N4 C19 C18 N3 10.9(6) . . . . ? N4 C19 C18 C17 -169.3(5) . . . . ? Pd1 N4 C20 C21 151.8(4) . . . . ? Pd1 N4 C20 C24 -27.8(6) . . . . ? Pd1 N4 C19 O4 168.9(4) . . . . ? Pd1 N4 C19 C18 -6.4(5) . . . . ? Pd1 N2 C13 O2 -178.8(4) . . . . ? Pd1 N2 C13 C14 -1.8(5) . . . . ? Pd1 N2 C10 C9 -163.2(4) . . . . ? Pd1 N2 C10 C11 19.9(6) . . . . ? Pd1 N3 C14 C13 11.9(5) . . . . ? Pd1 N3 C14 C15 -168.3(4) . . . . ? Pd1 N3 C18 C19 -10.6(5) . . . . ? Pd1 N3 C18 C17 169.6(4) . . . . ? N3 C14 C13 O2 171.1(5) . . . . ? N3 C14 C13 N2 -6.2(6) . . . . ? N3 C14 C15 C16 0.0(7) . . . . ? N3 C18 C17 C16 -2.7(7) . . . . ? N5 C25 C26 C31 -86.6(6) . . . . ? N5 C25 C26 C27 94.0(6) . . . . ? C21 C20 C24 C23 2.9(7) . . . . ? C14 N3 C18 C19 -178.2(4) . . . . ? C14 N3 C18 C17 2.0(7) . . . . ? C20 N4 C19 O4 -4.1(8) . . . . ? C20 N4 C19 C18 -179.4(4) . . . . ? C20 C21 C22 N5 0.2(7) . . . . ? C20 C24 C23 N5 -1.4(7) . . . . ? C22 N5 C25 C26 -78.8(6) . . . . ? C22 N5 C23 C24 -0.8(7) . . . . ? C22 C21 C20 N4 178.0(4) . . . . ? C22 C21 C20 C24 -2.3(7) . . . . ? C19 N4 C20 C21 -36.4(7) . . . . ? C19 N4 C20 C24 144.0(5) . . . . ? C19 C18 C17 C16 177.5(5) . . . . ? C1 C2 C3 C4 1.2(8) . . . . ? C1 C6 C5 C4 0.1(8) . . . . ? C18 N3 C14 C13 179.6(4) . . . . ? C18 N3 C14 C15 -0.6(7) . . . . ? C13 N2 C10 C9 30.1(7) . . . . ? C13 N2 C10 C11 -146.8(5) . . . . ? C13 C14 C15 C16 179.8(5) . . . . ? C8 N1 C7 C1 -82.9(6) . . . . ? C8 N1 C12 C11 2.6(8) . . . . ? C8 C9 C10 N2 -171.9(5) . . . . ? C8 C9 C10 C11 5.0(7) . . . . ? C10 N2 C13 O2 -10.5(8) . . . . ? C10 N2 C13 C14 166.6(4) . . . . ? C10 C9 C8 N1 -2.1(8) . . . . ? C10 C11 C12 N1 0.6(8) . . . . ? C7 N1 C8 C9 169.4(5) . . . . ? C7 N1 C12 C11 -168.6(5) . . . . ? C7 C1 C2 C3 -175.6(5) . . . . ? C7 C1 C6 C5 174.9(5) . . . . ? C15 C14 C13 O2 -8.7(8) . . . . ? C15 C14 C13 N2 174.0(5) . . . . ? C15 C16 C17 C18 2.1(8) . . . . ? C25 N5 C22 C21 -179.8(4) . . . . ? C25 N5 C23 C24 -179.6(4) . . . . ? C25 C26 C31 C30 -179.2(5) . . . . ? C25 C26 C27 C28 177.8(5) . . . . ? C2 C1 C7 N1 89.8(6) . . . . ? C2 C1 C6 C5 0.5(8) . . . . ? C2 C3 C4 C5 -0.6(8) . . . . ? C26 C31 C30 C29 1.1(8) . . . . ? C26 C27 C28 C29 1.7(8) . . . . ? C31 C26 C27 C28 -1.7(7) . . . . ? C17 C16 C15 C14 -0.8(8) . . . . ? C30 C29 C28 C27 -0.3(8) . . . . ? C23 N5 C22 C21 1.4(7) . . . . ? C23 N5 C25 C26 100.1(5) . . . . ? C6 C1 C7 N1 -84.6(6) . . . . ? C6 C1 C2 C3 -1.1(8) . . . . ? C6 C5 C4 C3 0.0(8) . . . . ? C12 N1 C8 C9 -1.8(7) . . . . ? C12 N1 C7 C1 88.2(6) . . . . ? C12 C11 C10 N2 172.8(5) . . . . ? C12 C11 C10 C9 -4.3(7) . . . . ? C27 C26 C31 C30 0.2(8) . . . . ? C28 C29 C30 C31 -1.1(8) . . . . ?