#------------------------------------------------------------------------------ #$Date: 2020-08-29 04:40:53 +0300 (Sat, 29 Aug 2020) $ #$Revision: 255724 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705299.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_7705299 loop_ _publ_author_name 'Exp\'osito, J. Emilio' 'Aull\'on, Gabriel' 'Bardaji, Manuel' 'Miguel, Jesus Angel' 'Espinet, Pablo' _publ_section_title ; Fluorescent perylenylpyridine complexes: an experimental and theoretical study ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT02494E _journal_year 2020 _chemical_formula_moiety 'C31 H23 N O2 Pd' _chemical_formula_sum 'C31 H23 N O2 Pd' _chemical_formula_weight 547.90 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2020-07-08 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-07-10 deposited with the CCDC. 2020-08-28 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 100.105(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.9934(3) _cell_length_b 15.8415(8) _cell_length_c 18.4651(7) _cell_measurement_reflns_used 3037 _cell_measurement_temperature 293 _cell_measurement_theta_max 29.4703 _cell_measurement_theta_min 2.2362 _cell_volume 2301.92(17) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 293 _diffrn_detector_area_resol_mean 10.4757 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.854 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -100.00 -56.00 1.0000 22.6900 omega____ theta____ kappa____ phi______ frames - -11.8877 179.0000 -90.0000 44 #__ type_ start__ end____ width___ exp.time_ 2 omega -72.00 0.00 1.0000 22.6900 omega____ theta____ kappa____ phi______ frames - -11.8877 -77.0000 -60.0000 72 #__ type_ start__ end____ width___ exp.time_ 3 omega -19.00 64.00 1.0000 22.6900 omega____ theta____ kappa____ phi______ frames - -11.8877 37.0000 -150.0000 83 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0848006000 _diffrn_orient_matrix_UB_12 -0.0146472000 _diffrn_orient_matrix_UB_13 0.0099489000 _diffrn_orient_matrix_UB_21 -0.0220534000 _diffrn_orient_matrix_UB_22 -0.0207904000 _diffrn_orient_matrix_UB_23 0.0310248000 _diffrn_orient_matrix_UB_31 -0.0213406000 _diffrn_orient_matrix_UB_32 -0.0368217000 _diffrn_orient_matrix_UB_33 -0.0214697000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_unetI/netI 0.0839 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.854 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 11795 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.854 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.536 _diffrn_reflns_theta_min 2.241 _diffrn_source 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.837 _exptl_absorpt_correction_T_max 0.981 _exptl_absorpt_correction_T_min 0.936 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.581 _exptl_crystal_description block _exptl_crystal_F_000 1112 _exptl_crystal_size_max 0.2567 _exptl_crystal_size_mid 0.1406 _exptl_crystal_size_min 0.0509 _refine_diff_density_max 0.539 _refine_diff_density_min -0.554 _refine_diff_density_rms 0.080 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 319 _refine_ls_number_reflns 5480 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.998 _refine_ls_R_factor_all 0.1089 _refine_ls_R_factor_gt 0.0491 _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^)+(0.0246P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0720 _refine_ls_wR_factor_ref 0.0903 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3181 _reflns_number_total 5480 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02494e2.cif _cod_data_source_block 5 _cod_database_code 7705299 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C31 H23 N O2 Pd' _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. ; _reflns_odcompleteness_completeness 99.94 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C8(H8), C9(H9), C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C22(H22), C24(H24), C25(H25), C29(H29) 2.b Idealised Me refined as rotating group: C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C31(H31A,H31B,H31C) ; _shelx_res_file ; TITL je241b_a.res in P2(1)/n je241b.res created by SHELXL-2018/3 at 17:21:45 on 08-Jul-2020 REM Old TITL JE241B in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.138, Rweak 0.024, Alpha 0.031, Orientation as input REM Formula found by SHELXT: C31 N O2 Pd CELL 0.71073 7.9934 15.8415 18.4651 90 100.105 90 ZERR 4 0.0003 0.0008 0.0007 0 0.004 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O Pd UNIT 124 92 4 8 4 L.S. 20 PLAN 10 TEMP 19.85 BOND $H list 4 fmap 2 acta REM REM REM WGHT 0.024600 FVAR 0.31275 PD1 5 0.151849 0.128757 0.449150 11.00000 0.04509 0.04849 = 0.04163 -0.00482 -0.00176 -0.00523 O1 4 0.020100 0.205309 0.370535 11.00000 0.06170 0.05264 = 0.04725 -0.00225 -0.00921 -0.00567 O2 4 0.079795 0.024185 0.381306 11.00000 0.05479 0.05380 = 0.04966 -0.01022 -0.00834 -0.00456 N1 3 0.287102 0.054091 0.525524 11.00000 0.04665 0.04320 = 0.04275 -0.00576 0.00587 -0.00360 C1 1 0.494237 0.164202 0.573580 11.00000 0.04445 0.04369 = 0.04147 -0.00854 0.00370 0.00093 C2 1 0.664273 0.177883 0.602836 11.00000 0.04926 0.04733 = 0.06764 -0.00801 -0.00197 0.00689 AFIX 43 H2 2 0.735471 0.131636 0.614704 11.00000 -1.20000 AFIX 0 C3 1 0.729623 0.256832 0.614622 11.00000 0.04005 0.05909 = 0.06978 -0.01168 -0.00324 -0.00374 AFIX 43 H3 2 0.845964 0.262876 0.630631 11.00000 -1.20000 AFIX 0 C4 1 0.629819 0.328579 0.603733 11.00000 0.04999 0.04708 = 0.03545 -0.00384 0.00353 -0.00035 C5 1 0.452901 0.317541 0.573617 11.00000 0.04545 0.04703 = 0.03439 -0.00267 0.00601 0.00118 C6 1 0.387661 0.235521 0.552756 11.00000 0.03954 0.04792 = 0.03705 -0.00292 0.00568 -0.00307 C7 1 0.220795 0.227623 0.511485 11.00000 0.04435 0.04495 = 0.04229 -0.00444 0.00283 -0.00242 C8 1 0.117526 0.296994 0.505811 11.00000 0.04407 0.05921 = 0.05183 -0.00559 -0.00368 0.00520 AFIX 43 H8 2 0.004655 0.291377 0.483113 11.00000 -1.20000 AFIX 0 C9 1 0.174702 0.374734 0.532479 11.00000 0.04986 0.04894 = 0.05498 -0.00768 0.00109 0.01187 AFIX 43 H9 2 0.097615 0.419081 0.529770 11.00000 -1.20000 AFIX 0 C10 1 0.343053 0.389405 0.563254 11.00000 0.05069 0.04778 = 0.03325 -0.00373 0.00375 0.00287 C11 1 0.410688 0.474267 0.581534 11.00000 0.06041 0.04890 = 0.03194 0.00184 0.00800 -0.00107 C12 1 0.587797 0.484259 0.608823 11.00000 0.06186 0.04852 = 0.03255 -0.00111 0.01010 -0.00899 C13 1 0.697772 0.413594 0.619179 11.00000 0.05763 0.05380 = 0.03388 0.00018 0.00653 -0.00766 C14 1 0.869663 0.428122 0.643193 11.00000 0.05456 0.07043 = 0.05744 0.00185 0.00227 -0.01687 AFIX 43 H14 2 0.944222 0.382575 0.649140 11.00000 -1.20000 AFIX 0 C15 1 0.933428 0.509200 0.658626 11.00000 0.06560 0.07868 = 0.07487 0.00480 -0.00335 -0.02838 AFIX 43 H15 2 1.049057 0.516718 0.675573 11.00000 -1.20000 AFIX 0 C16 1 0.830689 0.576313 0.649408 11.00000 0.08708 0.06003 = 0.07814 0.00278 0.00505 -0.03232 AFIX 43 H16 2 0.875439 0.630044 0.659739 11.00000 -1.20000 AFIX 0 C17 1 0.654618 0.566236 0.624085 11.00000 0.08180 0.05089 = 0.04920 -0.00025 0.01401 -0.01379 C18 1 0.546671 0.635804 0.612486 11.00000 0.10990 0.04160 = 0.07281 -0.00287 0.01865 -0.01317 AFIX 43 H18 2 0.590566 0.689750 0.622512 11.00000 -1.20000 AFIX 0 C19 1 0.378636 0.625755 0.586790 11.00000 0.10445 0.04465 = 0.06674 0.00417 0.01668 0.00770 AFIX 43 H19 2 0.308249 0.672862 0.579567 11.00000 -1.20000 AFIX 0 C20 1 0.310235 0.546103 0.571116 11.00000 0.07360 0.05401 = 0.05125 0.00196 0.00379 0.00503 AFIX 43 H20 2 0.194509 0.540702 0.553231 11.00000 -1.20000 AFIX 0 C21 1 0.429826 0.076936 0.572734 11.00000 0.04692 0.04696 = 0.03780 -0.00798 0.00650 0.00248 C22 1 0.510936 0.016952 0.622079 11.00000 0.05331 0.04834 = 0.04983 -0.00307 0.00158 0.00261 AFIX 43 H22 2 0.605018 0.033624 0.656140 11.00000 -1.20000 AFIX 0 C23 1 0.458958 -0.064745 0.622740 11.00000 0.06297 0.04898 = 0.04518 0.00118 0.01539 0.00675 C24 1 0.314625 -0.085844 0.572910 11.00000 0.07075 0.04550 = 0.05273 -0.00286 0.01581 -0.00433 AFIX 43 H24 2 0.273068 -0.140785 0.570877 11.00000 -1.20000 AFIX 0 C25 1 0.233904 -0.025725 0.526917 11.00000 0.04955 0.05687 = 0.05006 -0.00694 0.00672 -0.01263 AFIX 43 H25 2 0.135978 -0.041118 0.494569 11.00000 -1.20000 AFIX 0 C26 1 0.551190 -0.128923 0.674183 11.00000 0.09628 0.05460 = 0.06450 0.01015 0.01358 0.01534 AFIX 137 H26A 2 0.595537 -0.172174 0.646424 11.00000 -1.50000 H26B 2 0.474212 -0.153642 0.702643 11.00000 -1.50000 H26C 2 0.643062 -0.102175 0.706525 11.00000 -1.50000 AFIX 0 C27 1 -0.137688 0.251560 0.258642 11.00000 0.09127 0.06384 = 0.04985 0.00486 -0.00858 -0.00472 AFIX 137 H27A 2 -0.195393 0.289589 0.286411 11.00000 -1.50000 H27B 2 -0.217523 0.228492 0.218613 11.00000 -1.50000 H27C 2 -0.050474 0.281538 0.239575 11.00000 -1.50000 AFIX 0 C28 1 -0.058909 0.181216 0.307680 11.00000 0.05401 0.05520 = 0.04488 -0.00084 0.00197 -0.00179 C29 1 -0.079683 0.099778 0.282586 11.00000 0.05620 0.05784 = 0.04495 -0.00478 -0.00379 0.00059 AFIX 43 H29 2 -0.141695 0.092912 0.235408 11.00000 -1.20000 AFIX 0 C30 1 -0.019478 0.026528 0.319008 11.00000 0.04417 0.06375 = 0.04641 -0.01540 0.00734 -0.00563 C31 1 -0.070572 -0.058723 0.286540 11.00000 0.08898 0.05843 = 0.06204 -0.02159 -0.00933 -0.00590 AFIX 137 H31A 2 0.028702 -0.088661 0.278165 11.00000 -1.50000 H31B 2 -0.147223 -0.051673 0.240727 11.00000 -1.50000 H31C 2 -0.125792 -0.090224 0.320012 11.00000 -1.50000 AFIX 0 HKLF 4 REM je241b_a.res in P2(1)/n REM wR2 = 0.0903, GooF = S = 0.998, Restrained GooF = 0.998 for all data REM R1 = 0.0491 for 3181 Fo > 4sig(Fo) and 0.1089 for all 5480 data REM 319 parameters refined using 0 restraints END WGHT 0.0246 0.0000 REM Highest difference peak 0.539, deepest hole -0.554, 1-sigma level 0.080 Q1 1 0.8501 0.3934 0.5537 11.00000 0.05 0.54 Q2 1 0.5442 0.1287 0.6544 11.00000 0.05 0.49 Q3 1 0.4931 0.4748 0.6137 11.00000 0.05 0.31 Q4 1 0.0999 0.1222 0.5049 11.00000 0.05 0.31 Q5 1 0.1043 -0.0367 0.3960 11.00000 0.05 0.29 Q6 1 0.1507 0.0774 0.4676 11.00000 0.05 0.29 Q7 1 -0.2969 0.1197 0.1595 11.00000 0.05 0.29 Q8 1 -0.0857 -0.0587 0.2166 11.00000 0.05 0.29 Q9 1 -0.0691 0.1182 0.2490 11.00000 0.05 0.29 Q10 1 0.0741 0.0220 0.3559 11.00000 0.05 0.28 ; _shelx_res_checksum 94714 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -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 Pd1 Pd 0.15185(3) 0.12876(2) 0.44915(2) 0.04620(12) Uani 1 1 d . . . . . O1 O 0.0201(3) 0.20531(18) 0.37053(13) 0.0561(8) Uani 1 1 d . . . . . O2 O 0.0798(3) 0.02419(18) 0.38131(13) 0.0549(8) Uani 1 1 d . . . . . N1 N 0.2871(4) 0.0541(2) 0.52552(15) 0.0444(8) Uani 1 1 d . . . . . C1 C 0.4942(4) 0.1642(3) 0.57358(19) 0.0437(10) Uani 1 1 d . . . . . C2 C 0.6643(5) 0.1779(3) 0.6028(2) 0.0562(11) Uani 1 1 d . . . . . H2 H 0.735471 0.131636 0.614704 0.067 Uiso 1 1 calc R . . . . C3 C 0.7296(5) 0.2568(3) 0.6146(2) 0.0579(12) Uani 1 1 d . . . . . H3 H 0.845964 0.262876 0.630631 0.069 Uiso 1 1 calc R . . . . C4 C 0.6298(5) 0.3286(3) 0.60373(18) 0.0447(10) Uani 1 1 d . . . . . C5 C 0.4529(4) 0.3175(3) 0.57362(18) 0.0424(10) Uani 1 1 d . . . . . C6 C 0.3877(4) 0.2355(3) 0.55276(18) 0.0416(10) Uani 1 1 d . . . . . C7 C 0.2208(4) 0.2276(3) 0.51149(18) 0.0444(10) Uani 1 1 d . . . . . C8 C 0.1175(5) 0.2970(3) 0.5058(2) 0.0532(11) Uani 1 1 d . . . . . H8 H 0.004655 0.291377 0.483113 0.064 Uiso 1 1 calc R . . . . C9 C 0.1747(5) 0.3747(3) 0.5325(2) 0.0522(11) Uani 1 1 d . . . . . H9 H 0.097615 0.419081 0.529770 0.063 Uiso 1 1 calc R . . . . C10 C 0.3431(5) 0.3894(3) 0.56325(17) 0.0443(10) Uani 1 1 d . . . . . C11 C 0.4107(5) 0.4743(3) 0.58153(18) 0.0471(10) Uani 1 1 d . . . . . C12 C 0.5878(5) 0.4843(3) 0.60882(18) 0.0474(10) Uani 1 1 d . . . . . C13 C 0.6978(5) 0.4136(3) 0.61918(19) 0.0486(11) Uani 1 1 d . . . . . C14 C 0.8697(5) 0.4281(3) 0.6432(2) 0.0617(13) Uani 1 1 d . . . . . H14 H 0.944222 0.382575 0.649140 0.074 Uiso 1 1 calc R . . . . C15 C 0.9334(6) 0.5092(4) 0.6586(2) 0.0749(15) Uani 1 1 d . . . . . H15 H 1.049057 0.516718 0.675573 0.090 Uiso 1 1 calc R . . . . C16 C 0.8307(7) 0.5763(4) 0.6494(2) 0.0762(15) Uani 1 1 d . . . . . H16 H 0.875439 0.630044 0.659739 0.091 Uiso 1 1 calc R . . . . C17 C 0.6546(6) 0.5662(3) 0.6241(2) 0.0603(12) Uani 1 1 d . . . . . C18 C 0.5467(7) 0.6358(3) 0.6125(2) 0.0745(14) Uani 1 1 d . . . . . H18 H 0.590566 0.689750 0.622512 0.089 Uiso 1 1 calc R . . . . C19 C 0.3786(7) 0.6258(3) 0.5868(2) 0.0717(13) Uani 1 1 d . . . . . H19 H 0.308249 0.672862 0.579567 0.086 Uiso 1 1 calc R . . . . C20 C 0.3102(6) 0.5461(3) 0.5711(2) 0.0605(12) Uani 1 1 d . . . . . H20 H 0.194509 0.540702 0.553231 0.073 Uiso 1 1 calc R . . . . C21 C 0.4298(5) 0.0769(3) 0.57273(19) 0.0440(10) Uani 1 1 d . . . . . C22 C 0.5109(5) 0.0170(3) 0.6221(2) 0.0514(11) Uani 1 1 d . . . . . H22 H 0.605018 0.033624 0.656140 0.062 Uiso 1 1 calc R . . . . C23 C 0.4590(5) -0.0647(3) 0.6227(2) 0.0517(11) Uani 1 1 d . . . . . C24 C 0.3146(5) -0.0858(3) 0.5729(2) 0.0557(11) Uani 1 1 d . . . . . H24 H 0.273068 -0.140785 0.570877 0.067 Uiso 1 1 calc R . . . . C25 C 0.2339(5) -0.0257(3) 0.5269(2) 0.0524(11) Uani 1 1 d . . . . . H25 H 0.135978 -0.041118 0.494569 0.063 Uiso 1 1 calc R . . . . C26 C 0.5512(6) -0.1289(3) 0.6742(2) 0.0719(13) Uani 1 1 d . . . . . H26A H 0.595537 -0.172174 0.646424 0.108 Uiso 1 1 calc GR . . . . H26B H 0.474212 -0.153642 0.702643 0.108 Uiso 1 1 calc GR . . . . H26C H 0.643062 -0.102175 0.706525 0.108 Uiso 1 1 calc GR . . . . C27 C -0.1377(5) 0.2516(3) 0.2586(2) 0.0709(14) Uani 1 1 d . . . . . H27A H -0.195393 0.289589 0.286411 0.106 Uiso 1 1 calc GR . . . . H27B H -0.217523 0.228492 0.218613 0.106 Uiso 1 1 calc GR . . . . H27C H -0.050474 0.281538 0.239575 0.106 Uiso 1 1 calc GR . . . . C28 C -0.0589(5) 0.1812(3) 0.3077(2) 0.0522(11) Uani 1 1 d . . . . . C29 C -0.0797(5) 0.0998(3) 0.2826(2) 0.0545(12) Uani 1 1 d . . . . . H29 H -0.141695 0.092912 0.235408 0.065 Uiso 1 1 calc R . . . . C30 C -0.0195(5) 0.0265(3) 0.3190(2) 0.0515(11) Uani 1 1 d . . . . . C31 C -0.0706(6) -0.0587(3) 0.2865(2) 0.0725(14) Uani 1 1 d . . . . . H31A H 0.028702 -0.088661 0.278165 0.109 Uiso 1 1 calc GR . . . . H31B H -0.147223 -0.051673 0.240727 0.109 Uiso 1 1 calc GR . . . . H31C H -0.125792 -0.090224 0.320012 0.109 Uiso 1 1 calc GR . . . . 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 Pd1 0.04509(18) 0.0485(2) 0.04163(17) -0.00482(16) -0.00176(12) -0.00523(17) O1 0.0617(17) 0.053(2) 0.0473(16) -0.0022(13) -0.0092(13) -0.0057(15) O2 0.0548(16) 0.054(2) 0.0497(16) -0.0102(14) -0.0083(13) -0.0046(15) N1 0.0467(18) 0.043(2) 0.0428(17) -0.0058(16) 0.0059(15) -0.0036(17) C1 0.044(2) 0.044(3) 0.041(2) -0.0085(19) 0.0037(17) 0.001(2) C2 0.049(2) 0.047(3) 0.068(3) -0.008(2) -0.002(2) 0.007(2) C3 0.040(2) 0.059(4) 0.070(3) -0.012(2) -0.0032(19) -0.004(2) C4 0.050(2) 0.047(3) 0.035(2) -0.0038(19) 0.0035(17) 0.000(2) C5 0.045(2) 0.047(3) 0.0344(19) -0.0027(19) 0.0060(16) 0.001(2) C6 0.040(2) 0.048(3) 0.0371(19) -0.0029(19) 0.0057(17) -0.003(2) C7 0.044(2) 0.045(3) 0.042(2) -0.0044(19) 0.0028(17) -0.002(2) C8 0.044(2) 0.059(4) 0.052(2) -0.006(2) -0.0037(18) 0.005(2) C9 0.050(2) 0.049(3) 0.055(2) -0.008(2) 0.0011(19) 0.012(2) C10 0.051(2) 0.048(3) 0.0332(19) -0.0037(18) 0.0037(17) 0.003(2) C11 0.060(3) 0.049(3) 0.032(2) 0.0018(19) 0.0080(18) -0.001(2) C12 0.062(3) 0.049(3) 0.033(2) -0.0011(19) 0.0101(18) -0.009(2) C13 0.058(3) 0.054(3) 0.034(2) 0.000(2) 0.0065(18) -0.008(2) C14 0.055(3) 0.070(4) 0.057(3) 0.002(2) 0.002(2) -0.017(3) C15 0.066(3) 0.079(5) 0.075(3) 0.005(3) -0.003(2) -0.028(3) C16 0.087(4) 0.060(4) 0.078(3) 0.003(3) 0.005(3) -0.032(3) C17 0.082(3) 0.051(4) 0.049(2) 0.000(2) 0.014(2) -0.014(3) C18 0.110(4) 0.042(4) 0.073(3) -0.003(3) 0.019(3) -0.013(3) C19 0.104(4) 0.045(4) 0.067(3) 0.004(3) 0.017(3) 0.008(3) C20 0.074(3) 0.054(4) 0.051(3) 0.002(2) 0.004(2) 0.005(3) C21 0.047(2) 0.047(3) 0.038(2) -0.008(2) 0.0065(18) 0.002(2) C22 0.053(2) 0.048(3) 0.050(2) -0.003(2) 0.0016(19) 0.003(2) C23 0.063(3) 0.049(3) 0.045(2) 0.001(2) 0.015(2) 0.007(2) C24 0.071(3) 0.046(3) 0.053(2) -0.003(2) 0.016(2) -0.004(2) C25 0.050(2) 0.057(4) 0.050(2) -0.007(2) 0.0067(19) -0.013(2) C26 0.096(3) 0.055(3) 0.065(3) 0.010(3) 0.014(2) 0.015(3) C27 0.091(3) 0.064(4) 0.050(2) 0.005(2) -0.009(2) -0.005(3) C28 0.054(2) 0.055(3) 0.045(2) -0.001(2) 0.0020(19) -0.002(2) C29 0.056(2) 0.058(4) 0.045(2) -0.005(2) -0.0038(19) 0.001(2) C30 0.044(2) 0.064(4) 0.046(2) -0.015(2) 0.0073(19) -0.006(2) C31 0.089(3) 0.058(4) 0.062(3) -0.022(2) -0.009(2) -0.006(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' 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_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -9 -1 -12 0.0817 -9.0000 -1.0000 -12.0000 -0.8679 -0.1526 0.4869 9 0 12 0.0863 9.0000 0.0000 12.0000 0.8825 0.1734 -0.4501 0 -19 -13 0.0519 0.0000 -19.0000 -13.0000 0.1494 -0.0080 0.9783 0 19 13 0.0553 -0.0000 19.0000 13.0000 -0.1494 0.0080 -0.9783 0 1 -25 0.0337 0.0000 1.0000 -25.0000 -0.2635 -0.7961 0.5007 0 -4 25 0.0098 0.0000 -4.0000 25.0000 0.3076 0.8585 -0.3903 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 Pd1 O2 89.49(11) . . ? N1 Pd1 O1 178.50(11) . . ? N1 Pd1 O2 90.68(12) . . ? C7 Pd1 O1 89.98(14) . . ? C7 Pd1 O2 179.11(13) . . ? C7 Pd1 N1 89.83(15) . . ? C28 O1 Pd1 125.5(3) . . ? C30 O2 Pd1 125.2(3) . . ? C21 N1 Pd1 125.7(3) . . ? C25 N1 Pd1 116.0(3) . . ? C25 N1 C21 118.3(3) . . ? C2 C1 C6 118.6(4) . . ? C2 C1 C21 117.8(4) . . ? C6 C1 C21 123.3(3) . . ? C1 C2 H2 119.0 . . ? C3 C2 C1 121.9(4) . . ? C3 C2 H2 119.0 . . ? C2 C3 H3 118.7 . . ? C2 C3 C4 122.5(4) . . ? C4 C3 H3 118.7 . . ? C3 C4 C5 117.4(4) . . ? C3 C4 C13 122.9(4) . . ? C5 C4 C13 119.6(4) . . ? C6 C5 C4 120.2(4) . . ? C6 C5 C10 120.1(3) . . ? C10 C5 C4 119.6(4) . . ? C1 C6 C5 118.4(3) . . ? C7 C6 C1 122.3(4) . . ? C7 C6 C5 119.3(4) . . ? C6 C7 Pd1 121.7(3) . . ? C8 C7 Pd1 119.5(3) . . ? C8 C7 C6 117.9(4) . . ? C7 C8 H8 118.9 . . ? C7 C8 C9 122.3(4) . . ? C9 C8 H8 118.9 . . ? C8 C9 H9 118.8 . . ? C8 C9 C10 122.4(4) . . ? C10 C9 H9 118.8 . . ? C5 C10 C11 120.4(3) . . ? C9 C10 C5 116.8(4) . . ? C9 C10 C11 122.7(4) . . ? C12 C11 C10 119.1(4) . . ? C20 C11 C10 122.6(4) . . ? C20 C11 C12 118.2(4) . . ? C13 C12 C11 121.0(4) . . ? C17 C12 C11 119.3(4) . . ? C17 C12 C13 119.7(4) . . ? C12 C13 C4 120.1(4) . . ? C14 C13 C4 121.9(4) . . ? C14 C13 C12 118.0(4) . . ? C13 C14 H14 119.2 . . ? C13 C14 C15 121.7(5) . . ? C15 C14 H14 119.2 . . ? C14 C15 H15 119.6 . . ? C16 C15 C14 120.9(5) . . ? C16 C15 H15 119.6 . . ? C15 C16 H16 119.8 . . ? C15 C16 C17 120.5(5) . . ? C17 C16 H16 119.8 . . ? C16 C17 C12 119.3(5) . . ? C18 C17 C12 119.6(4) . . ? C18 C17 C16 121.1(5) . . ? C17 C18 H18 119.6 . . ? C19 C18 C17 120.7(5) . . ? C19 C18 H18 119.6 . . ? C18 C19 H19 119.6 . . ? C18 C19 C20 120.8(5) . . ? C20 C19 H19 119.6 . . ? C11 C20 H20 119.3 . . ? C19 C20 C11 121.4(4) . . ? C19 C20 H20 119.3 . . ? N1 C21 C1 120.6(4) . . ? N1 C21 C22 118.7(4) . . ? C22 C21 C1 120.7(3) . . ? C21 C22 H22 118.4 . . ? C23 C22 C21 123.1(4) . . ? C23 C22 H22 118.4 . . ? C22 C23 C24 116.4(4) . . ? C22 C23 C26 122.4(4) . . ? C24 C23 C26 121.3(4) . . ? C23 C24 H24 120.2 . . ? C25 C24 C23 119.6(4) . . ? C25 C24 H24 120.2 . . ? N1 C25 C24 123.8(4) . . ? N1 C25 H25 118.1 . . ? C24 C25 H25 118.1 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C28 C27 H27A 109.5 . . ? C28 C27 H27B 109.5 . . ? C28 C27 H27C 109.5 . . ? O1 C28 C27 114.4(4) . . ? O1 C28 C29 126.8(4) . . ? C29 C28 C27 118.8(4) . . ? C28 C29 H29 116.1 . . ? C28 C29 C30 127.8(4) . . ? C30 C29 H29 116.1 . . ? O2 C30 C29 124.7(4) . . ? O2 C30 C31 114.5(4) . . ? C29 C30 C31 120.8(4) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31B 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? 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 Pd1 O1 2.037(3) . ? Pd1 O2 2.096(3) . ? Pd1 N1 2.005(3) . ? Pd1 C7 1.964(4) . ? O1 C28 1.278(4) . ? O2 C30 1.278(4) . ? N1 C21 1.358(4) . ? N1 C25 1.336(5) . ? C1 C2 1.389(5) . ? C1 C6 1.427(5) . ? C1 C21 1.474(5) . ? C2 H2 0.9300 . ? C2 C3 1.358(6) . ? C3 H3 0.9300 . ? C3 C4 1.383(6) . ? C4 C5 1.437(5) . ? C4 C13 1.461(6) . ? C5 C6 1.428(5) . ? C5 C10 1.430(5) . ? C6 C7 1.421(5) . ? C7 C8 1.367(5) . ? C8 H8 0.9300 . ? C8 C9 1.374(6) . ? C9 H9 0.9300 . ? C9 C10 1.385(5) . ? C10 C11 1.466(6) . ? C11 C12 1.426(5) . ? C11 C20 1.387(6) . ? C12 C13 1.415(6) . ? C12 C17 1.414(6) . ? C13 C14 1.387(5) . ? C14 H14 0.9300 . ? C14 C15 1.393(6) . ? C15 H15 0.9300 . ? C15 C16 1.336(7) . ? C16 H16 0.9300 . ? C16 C17 1.412(6) . ? C17 C18 1.393(6) . ? C18 H18 0.9300 . ? C18 C19 1.353(6) . ? C19 H19 0.9300 . ? C19 C20 1.385(6) . ? C20 H20 0.9300 . ? C21 C22 1.395(5) . ? C22 H22 0.9300 . ? C22 C23 1.360(6) . ? C23 C24 1.385(5) . ? C23 C26 1.495(6) . ? C24 H24 0.9300 . ? C24 C25 1.361(5) . ? C25 H25 0.9300 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C27 C28 1.503(6) . ? C28 C29 1.371(6) . ? C29 H29 0.9300 . ? C29 C30 1.385(6) . ? C30 C31 1.505(6) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ?