#------------------------------------------------------------------------------ #$Date: 2024-08-05 20:56:12 +0300 (Mon, 05 Aug 2024) $ #$Revision: 293737 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/18/1571800.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_1571800 loop_ _publ_author_name 'Liu, Yang' 'Xu, Ling' 'Jin, Xiaorong' 'Yin, Bangshao' 'Rao, Yutao' 'Zhou, Mingbo' 'Song, Jianxin' 'Osuka, Atsuhiro' _publ_section_title ; The unprecedented strong paratropic ring current of a bis-PdII complex of 5,10,23-trimesityl [28]heptaphyrin(1.1.0.0.1.0.0). ; _journal_issue 29 _journal_name_full 'Chemical science' _journal_page_first 11402 _journal_page_last 11407 _journal_paper_doi 10.1039/d4sc01909a _journal_volume 15 _journal_year 2024 _chemical_formula_moiety 'C58 H48 Cl N7 Pd2' _chemical_formula_sum 'C58 H48 Cl N7 Pd2' _chemical_formula_weight 1091.28 _space_group_crystal_system orthorhombic _space_group_IT_number 62 _space_group_name_Hall '-P 2ac 2n' _space_group_name_H-M_alt 'P n m a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2023-07-07 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2024-02-01 deposited with the CCDC. 2024-06-05 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.5782(3) _cell_length_b 19.0441(4) _cell_length_c 16.8698(5) _cell_measurement_reflns_used 21019 _cell_measurement_temperature 100.01(10) _cell_measurement_theta_max 71.9470 _cell_measurement_theta_min 3.4820 _cell_volume 4683.5(2) _computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _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_environment N~2~ _diffrn_ambient_temperature 100.01(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.0697 _diffrn_detector_type EosS2 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -32.00 42.00 1.00 3.40 -- 34.48 -57.00 30.00 74 2 \w 22.00 73.00 1.00 3.40 -- 34.48 -99.00 120.00 51 3 \w 24.00 87.00 1.00 3.40 -- 34.48-125.00 0.00 63 4 \w 23.00 86.00 1.00 3.40 -- 34.48-125.00 -60.00 63 5 \w 42.00 132.00 1.00 13.70 -- 105.88 -77.00 60.00 90 6 \w 90.00 116.00 1.00 13.70 -- 105.88-111.00 60.00 26 7 \w 45.00 71.00 1.00 13.70 -- 105.88-111.00 60.00 26 8 \w 37.00 102.00 1.00 13.70 -- 105.88 -94.00 0.00 65 9 \w 53.00 116.00 1.00 13.70 -- 105.88-111.00-120.00 63 10 \w 62.00 132.00 1.00 13.70 -- 105.88 -77.00-150.00 70 11 \w 84.00 136.00 1.00 13.70 -- 105.88 30.00 0.00 52 12 \w 121.00 173.00 1.00 13.70 -- 105.88 77.00 30.00 52 13 \w 137.00 167.00 1.00 13.70 -- 105.88 61.00 120.00 30 14 \w 121.00 170.00 1.00 13.70 -- 105.88 77.00 90.00 49 15 \w 125.00 173.00 1.00 13.70 -- 105.88 77.00 60.00 48 16 \w 129.00 172.00 1.00 13.70 -- 105.88 77.00 -30.00 43 17 \w 125.00 171.00 1.00 13.70 -- 105.88 77.00 -60.00 46 18 \w 123.00 172.00 1.00 13.70 -- 105.88 77.00-120.00 49 19 \w 123.00 173.00 1.00 13.70 -- 105.88 77.00-180.00 50 20 \w 123.00 167.00 1.00 13.70 -- 105.88 77.00-150.00 44 21 \w 117.00 173.00 1.00 13.70 -- 105.88 77.00 -90.00 56 22 \w 120.00 171.00 1.00 13.70 -- 105.88 77.00 0.00 51 23 \w 118.00 164.00 1.00 13.70 -- 105.88 77.00 150.00 46 24 \w 88.00 114.00 1.00 13.70 -- 105.88 61.00 90.00 26 25 \w 88.00 114.00 1.00 13.70 -- 105.88 61.00 60.00 26 26 \w 88.00 114.00 1.00 13.70 -- 105.88 61.00 30.00 26 27 \w 88.00 114.00 1.00 13.70 -- 105.88 61.00 0.00 26 28 \w 85.00 130.00 1.00 13.70 -- 105.88 30.00 30.00 45 29 \w 84.00 113.00 1.00 13.70 -- 105.88 30.00 -30.00 29 30 \w 88.00 114.00 1.00 13.70 -- 105.88 61.00 -60.00 26 31 \w 88.00 115.00 1.00 13.70 -- 105.88 61.00 -90.00 27 32 \w 88.00 114.00 1.00 13.70 -- 105.88 61.00-120.00 26 33 \w 88.00 114.00 1.00 13.70 -- 105.88 61.00-150.00 26 34 \w 89.00 114.00 1.00 13.70 -- 105.88 61.00-180.00 25 35 \w 79.00 105.00 1.00 13.70 -- 105.88 77.00-120.00 26 36 \w 79.00 105.00 1.00 13.70 -- 105.88 77.00-150.00 26 37 \w 79.00 104.00 1.00 13.70 -- 105.88 77.00-180.00 25 38 \w 84.00 113.00 1.00 13.70 -- 105.88 30.00-120.00 29 39 \w 85.00 117.00 1.00 13.70 -- 105.88 30.00 -90.00 32 40 \w 84.00 114.00 1.00 13.70 -- 105.88 30.00 -60.00 30 41 \w 79.00 105.00 1.00 13.70 -- 105.88 77.00 0.00 26 42 \w 79.00 105.00 1.00 13.70 -- 105.88 77.00 30.00 26 43 \w 79.00 105.00 1.00 13.70 -- 105.88 77.00 60.00 26 44 \w 79.00 105.00 1.00 13.70 -- 105.88 77.00 90.00 26 45 \w 88.00 114.00 1.00 13.70 -- 105.88 61.00 120.00 26 46 \w 79.00 105.00 1.00 13.70 -- 105.88 77.00 150.00 26 47 \w 79.00 107.00 1.00 13.70 -- 105.88 77.00 120.00 28 48 \w 84.00 112.00 1.00 13.70 -- 105.88 30.00 120.00 28 49 \w 85.00 113.00 1.00 13.70 -- 105.88 30.00 150.00 28 50 \w 84.00 111.00 1.00 13.70 -- 105.88 30.00 90.00 27 51 \w 84.00 110.00 1.00 13.70 -- 105.88 30.00 60.00 26 52 \w 79.00 105.00 1.00 13.70 -- 105.88 77.00 -30.00 26 53 \w 79.00 105.00 1.00 13.70 -- 105.88 77.00 -60.00 26 54 \w 79.00 105.00 1.00 13.70 -- 105.88 77.00 -90.00 26 55 \w 84.00 110.00 1.00 13.70 -- 105.88 30.00-150.00 26 56 \w 84.00 115.00 1.00 13.70 -- 105.88 30.00-180.00 31 57 \w 74.00 101.00 1.00 3.40 -- 34.48 71.00 -27.00 27 58 \w 18.00 93.00 1.00 3.40 -- 34.48 57.00 -30.00 75 59 \w 14.00 61.00 1.00 3.40 -- 34.48 71.00 -27.00 47 60 \w 16.00 103.00 1.00 3.40 -- 34.48 38.00 -90.00 87 61 \w 8.00 82.00 1.00 3.40 -- 34.48 77.00 -90.00 74 62 \w -9.00 47.00 1.00 3.40 -- 34.48 -57.00 -30.00 56 63 \w -32.00 31.00 1.00 3.40 -- 34.48 -57.00-180.00 63 64 \w -15.00 102.00 1.00 3.40 -- 34.48 0.00-180.00 117 65 \w 9.00 50.00 1.00 3.40 -- 34.48 77.00-150.00 41 66 \w -2.00 24.00 1.00 3.40 -- 34.48 96.00 -55.22 26 67 \w 9.00 97.00 1.00 3.40 -- 34.48 77.00 30.00 88 68 \w 9.00 100.00 1.00 3.40 -- 34.48 77.00 150.00 91 69 \w 8.00 68.00 1.00 3.40 -- 34.48 77.00 90.00 60 70 \w -33.00 40.00 1.00 3.40 -- 34.48 -38.00 90.00 73 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, EosS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.1055999000 _diffrn_orient_matrix_UB_12 -0.0025509000 _diffrn_orient_matrix_UB_13 0.0025133000 _diffrn_orient_matrix_UB_21 -0.0045389000 _diffrn_orient_matrix_UB_22 -0.0643061000 _diffrn_orient_matrix_UB_23 0.0554080000 _diffrn_orient_matrix_UB_31 0.0003670000 _diffrn_orient_matrix_UB_32 -0.0490625000 _diffrn_orient_matrix_UB_33 -0.0724734000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0588 _diffrn_reflns_av_unetI/netI 0.0206 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 59585 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 66.597 _diffrn_reflns_theta_max 66.597 _diffrn_reflns_theta_min 3.500 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 7.097 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.07529 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour blue _exptl_crystal_colour_primary blue _exptl_crystal_density_diffrn 1.548 _exptl_crystal_description block _exptl_crystal_F_000 2216 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.512 _refine_diff_density_min -1.080 _refine_diff_density_rms 0.091 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 329 _refine_ls_number_reflns 4276 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.102 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_gt 0.0549 _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^)+(0.0520P)^2^+19.1016P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1348 _refine_ls_wR_factor_ref 0.1376 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3877 _reflns_number_total 4276 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc01909a2.cif _cod_data_source_block exp_3204 _cod_depositor_comments 'Adding full bibliography for 1571798--1571800.cif.' _cod_database_code 1571800 _shelx_shelxl_version_number 2016/6 _chemical_oxdiff_formula 'C100 H100 N6 Pd1 Cl2' _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_max 0.718 _shelx_estimated_absorpt_t_min 0.537 _reflns_odcompleteness_completeness 100.00 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.49 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 2. Others Fixed Sof: H00E(0.5) H00F(0.5) H00H(0.5) H00I(0.5) H00K(0.5) H01E(0.5) H01F(0.5) 3.a Me refined with riding coordinates: C00P(H00D,H00E,H00F), C013(H01D,H01E,H01F) 3.b Aromatic/amide H refined with riding coordinates: N005(H005), N006(H006), C009(H009), C00G(H00G), C00J(H00J), C00L(H00L), C00Q(H00Q), C00T(H00T), C00V(H00V), C00W(H00W), C00Z(H00Z), C011(H011) 3.c Idealised Me refined as rotating group: C00E(H00A,H00B,H00C), C00Y(H00H,H00I,H00K), C012(H01A,H01B,H01C), C014(H01G, H01H,H01I) ; _shelx_res_file ; TITL exp_3204_a.res in Pnma exp_3204.res created by SHELXL-2016/6 at 22:08:33 on 07-Jul-2023 REM Old TITL exp_3204_a.res in Pnma REM SHELXT solution in Pnma REM R1 0.220, Rweak 0.006, Alpha 0.052, Orientation as input REM Formula found by SHELXT: C58 N7 Cl Pd2 CELL 1.54184 14.5782 19.0441 16.8698 90 90 90 ZERR 4 0.0003 0.0004 0.0005 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,-Z SYMM 0.5+X,0.5-Y,0.5-Z SFAC C H Cl N Pd UNIT 232 192 4 28 8 L.S. 8 0 0 PLAN 1 SIZE 0.1 0.1 0.05 TEMP list 4 fmap 2 53 acta SHEL 999 0.84 REM REM REM WGHT 0.052000 19.101604 FVAR 0.17348 PD01 5 0.408043 0.650878 0.569365 11.00000 0.02481 0.03050 = 0.07791 0.00189 -0.01653 -0.00117 CL02 3 0.380194 0.750000 0.492809 10.50000 0.07745 0.02847 = 0.07943 0.00000 -0.03594 0.00000 N003 4 0.377198 0.563883 0.488549 11.00000 0.02491 0.02943 = 0.08525 -0.00463 -0.01574 -0.00029 N004 4 0.430596 0.570688 0.641397 11.00000 0.02499 0.04129 = 0.07939 0.00504 -0.01210 -0.00216 N005 4 0.333833 0.659786 0.342811 11.00000 0.03592 0.03764 = 0.07342 -0.00492 -0.02484 -0.00124 AFIX 43 H005 2 0.348367 0.687380 0.381160 11.00000 -1.20000 AFIX 0 N006 4 0.490860 0.750000 0.776446 10.50000 0.03088 0.05134 = 0.06465 0.00000 -0.00915 0.00000 AFIX 43 H006 2 0.510588 0.749999 0.824489 10.50000 -1.20000 AFIX 0 C007 1 0.472714 0.691211 0.732256 11.00000 0.02289 0.04582 = 0.07563 0.00582 -0.00874 -0.00155 C008 1 0.463017 0.565300 0.717715 11.00000 0.02156 0.04753 = 0.08450 0.00876 -0.00770 -0.00473 C009 1 0.145608 0.750000 0.053071 10.50000 0.05426 0.03300 = 0.09105 0.00000 -0.03746 0.00000 AFIX 43 H009 2 0.083644 0.750000 0.039961 10.50000 -1.20000 AFIX 0 C00A 1 0.355013 0.544369 0.413720 11.00000 0.02524 0.03511 = 0.08301 -0.00231 -0.01364 -0.00040 C00B 1 0.389056 0.502914 0.530080 11.00000 0.02405 0.03513 = 0.09002 0.00574 -0.01031 -0.00264 C00C 1 0.294387 0.750000 0.236806 10.50000 0.03371 0.04977 = 0.07684 0.00000 -0.02442 0.00000 C00D 1 0.306378 0.682144 0.266936 11.00000 0.03604 0.04470 = 0.07701 -0.00334 -0.02478 0.00105 C00E 1 0.682669 0.642077 0.800424 11.00000 0.02655 0.08031 = 0.04596 0.01211 -0.00239 -0.00850 AFIX 137 H00A 2 0.727306 0.605045 0.798764 11.00000 -1.50000 H00B 2 0.712700 0.685755 0.811985 11.00000 -1.50000 H00C 2 0.652405 0.645347 0.750018 11.00000 -1.50000 AFIX 0 C00F 1 0.334193 0.588208 0.347089 11.00000 0.02548 0.03899 = 0.08407 -0.00507 -0.01795 -0.00107 C00G 1 0.354272 0.470176 0.407801 11.00000 0.02753 0.03920 = 0.10392 -0.01161 -0.01152 0.00108 AFIX 43 H00G 2 0.341933 0.443881 0.362587 11.00000 -1.20000 AFIX 0 C00H 1 0.485163 0.622216 0.763009 11.00000 0.02079 0.05517 = 0.07563 0.01374 -0.00629 -0.00362 C00I 1 0.262924 0.750000 0.152523 10.50000 0.04560 0.05217 = 0.06749 0.00000 -0.02331 0.00000 C00J 1 0.468069 0.490897 0.734899 11.00000 0.03168 0.04925 = 0.08497 0.02362 -0.00201 -0.00441 AFIX 43 H00J 2 0.487826 0.470856 0.782183 11.00000 -1.20000 AFIX 0 C00K 1 0.441774 0.713737 0.656426 11.00000 0.02174 0.04792 = 0.07493 0.00420 -0.00990 -0.00064 C00L 1 0.290731 0.619567 0.224298 11.00000 0.04521 0.04539 = 0.09751 -0.00813 -0.03009 0.00791 AFIX 43 H00L 2 0.271820 0.617082 0.171722 11.00000 -1.20000 AFIX 0 C00M 1 0.416866 0.506953 0.610833 11.00000 0.02434 0.03676 = 0.09510 0.00469 -0.00659 -0.00279 C00N 1 0.169852 0.750000 0.132691 10.50000 0.05043 0.02976 = 0.08682 0.00000 -0.02945 0.00000 C00O 1 0.328968 0.750000 0.093037 10.50000 0.05481 0.08189 = 0.07744 0.00000 -0.04167 0.00000 C00P 1 0.098920 0.750000 0.197443 10.50000 0.04603 0.04807 = 0.08967 0.00000 -0.02803 0.00000 PART -1 AFIX 33 H00D 2 0.128917 0.750000 0.248103 10.50000 -1.50000 H00E 2 0.061286 0.791159 0.192777 10.50000 -1.50000 H00F 2 0.061286 0.708841 0.192777 10.50000 -1.50000 AFIX 0 PART 0 C00Q 1 0.307501 0.563671 0.271746 11.00000 0.03830 0.03999 = 0.10547 -0.01351 -0.02372 0.00511 AFIX 43 H00Q 2 0.302260 0.516783 0.257021 11.00000 -1.20000 AFIX 0 C00R 1 0.519605 0.615206 0.845588 11.00000 0.02787 0.05699 = 0.05909 0.01226 -0.00131 -0.00429 C00S 1 0.209044 0.750000 -0.007263 10.50000 0.07278 0.03789 = 0.08054 0.00000 -0.04316 0.00000 C00T 1 0.375306 0.444536 0.481767 11.00000 0.02969 0.03219 = 0.10509 -0.00181 -0.01137 -0.00406 AFIX 43 H00T 2 0.379514 0.397610 0.496589 11.00000 -1.20000 AFIX 0 C00U 1 0.613021 0.626525 0.863957 11.00000 0.02901 0.06723 = 0.06248 0.02128 0.00272 -0.00303 C00V 1 0.439076 0.455904 0.670245 11.00000 0.03307 0.03913 = 0.10306 0.01501 -0.00145 -0.00521 AFIX 43 H00V 2 0.434322 0.407422 0.665069 11.00000 -1.20000 AFIX 0 C00W 1 0.300547 0.750000 0.015259 10.50000 0.06285 0.07384 = 0.09149 0.00000 -0.01652 0.00000 AFIX 43 H00W 2 0.345011 0.750000 -0.024272 10.50000 -1.20000 AFIX 0 C00X 1 0.457167 0.602263 0.907076 11.00000 0.03295 0.07992 = 0.08743 0.00345 0.01187 -0.01244 C00Y 1 0.179509 0.750000 -0.092487 10.50000 0.07554 0.05499 = 0.08648 0.00000 -0.03721 0.00000 PART -1 AFIX 137 H00H 2 0.134709 0.786224 -0.100694 10.50000 -1.50000 H00I 2 0.153204 0.705243 -0.105480 10.50000 -1.50000 H00K 2 0.231721 0.758533 -0.125800 10.50000 -1.50000 AFIX 0 PART 0 C00Z 1 0.640720 0.624147 0.942800 11.00000 0.03199 0.11201 = 0.05595 0.03365 0.00073 -0.00184 AFIX 43 H00Z 2 0.702267 0.630956 0.955095 11.00000 -1.20000 AFIX 0 C010 1 0.579137 0.611953 1.002972 11.00000 0.04801 0.11864 = 0.06227 0.03237 0.01026 -0.00308 C011 1 0.487930 0.601049 0.983843 11.00000 0.05018 0.10851 = 0.07855 0.01061 0.02657 -0.01745 AFIX 43 H011 2 0.446144 0.592623 1.024399 11.00000 -1.20000 AFIX 0 C012 1 0.355491 0.592229 0.888843 11.00000 0.03042 0.11953 = 0.12307 -0.03502 0.02359 -0.02359 AFIX 137 H01A 2 0.333611 0.631387 0.858402 11.00000 -1.50000 H01B 2 0.321695 0.589255 0.937568 11.00000 -1.50000 H01C 2 0.347197 0.549731 0.859088 11.00000 -1.50000 AFIX 0 C013 1 0.431393 0.750000 0.112943 10.50000 0.04401 0.18431 = 0.07558 0.00000 -0.02324 0.00000 PART -1 AFIX 33 H01D 2 0.439187 0.750000 0.169449 10.50000 -1.50000 H01E 2 0.459620 0.708841 0.090932 10.50000 -1.50000 H01F 2 0.459620 0.791159 0.090933 10.50000 -1.50000 AFIX 0 PART 0 C014 1 0.611251 0.613487 1.088098 11.00000 0.06815 0.19812 = 0.06159 0.05172 0.01121 0.01001 AFIX 137 H01G 2 0.647787 0.572613 1.098698 11.00000 -1.50000 H01H 2 0.559024 0.613907 1.122756 11.00000 -1.50000 H01I 2 0.647348 0.654915 1.096933 11.00000 -1.50000 AFIX 0 HKLF 4 REM exp_3204_a.res in Pnma REM R1 = 0.0549 for 3877 Fo > 4sig(Fo) and 0.0592 for all 4276 data REM 329 parameters refined using 0 restraints END WGHT 0.0520 19.1134 REM Highest difference peak 1.512, deepest hole -1.080, 1-sigma level 0.091 Q1 1 0.4081 0.6995 0.5682 11.00000 0.05 1.51 ; _shelx_res_checksum 71061 _shelx_hkl_file ; 0 1 0 0.69 0.36 0 -1 0 0.82 0.66 0 1 0 0.63 0.34 0 2 0 161.17 6.83 0 -2 0 165.92 7.18 0 2 0 163.15 5.73 0 -3 0 -0.12 1.42 0 3 0 0.04 0.82 0 3 0 0.49 1.74 0 -4 0 1719.15 31.73 0 4 0 1689.70 34.36 0 4 0 1632.66 25.35 0 -5 0 0.01 1.90 0 5 0 0.90 1.48 0 5 0 0.33 3.10 0 6 0 211.61 15.31 0 6 0 204.69 13.98 0 6 0 211.08 11.22 0 -6 0 225.71 13.08 0 -7 0 2.48 1.94 0 7 0 0.07 2.19 0 -7 0 2.28 2.01 0 7 0 1.54 1.69 0 7 0 3.67 3.50 0 8 0 1922.35 37.35 0 -8 0 2047.13 45.44 0 8 0 1917.07 48.39 0 -8 0 1921.10 42.01 0 8 0 1797.67 49.39 0 9 0 -0.22 2.47 0 9 0 -4.14 3.50 0 -9 0 1.43 2.45 0 9 0 1.86 1.33 0 -9 0 -0.31 1.93 0 10 0 3280.90 69.41 0 10 0 3118.88 52.15 0 -10 0 3199.29 64.13 0 -10 0 3206.50 59.67 0 10 0 3020.35 66.61 0 11 0 0.88 2.51 0 -11 0 -1.59 2.07 0 -11 0 2.62 3.02 0 11 0 1.91 2.75 0 12 0 681.29 34.57 0 -12 0 680.03 32.22 0 -12 0 667.14 29.79 0 -13 0 1.56 2.76 0 -13 0 -1.86 2.86 0 13 0 1.32 2.40 0 14 0 114.13 16.18 0 -14 0 110.59 12.97 0 14 0 115.98 15.05 0 -15 0 2.24 1.85 0 -15 0 4.31 2.36 0 -15 0 4.49 2.43 0 -16 0 8.82 2.56 0 -16 0 8.55 2.71 0 -16 0 8.44 2.32 0 -17 0 0.71 1.44 0 -17 0 1.61 1.35 0 -17 0 1.45 1.61 0 -18 0 50.19 5.81 0 18 0 40.36 4.27 0 -18 0 47.72 5.96 0 -18 0 55.10 4.94 0 -19 0 0.39 2.14 0 19 0 0.52 1.13 0 -19 0 -0.26 1.43 0 -19 0 0.52 1.27 0 -20 0 700.62 19.48 0 20 0 675.10 14.54 0 -20 0 699.63 20.23 0 20 0 692.71 15.01 0 -20 0 717.08 15.60 0 -21 0 0.27 1.29 0 -21 0 1.49 1.05 0 -22 0 152.17 5.81 0 22 0 176.26 6.60 0 23 0 0.46 0.60 0 23 0 -0.29 0.50 0 -23 0 0.34 0.51 0 0 1 0.93 0.39 0 0 1 0.60 0.29 0 0 -1 0.79 0.39 0 -1 -1 655.02 13.38 0 -1 1 636.92 6.97 0 -1 1 628.79 8.16 0 -1 -1 639.59 8.50 0 -1 -1 628.49 7.73 0 -1 -1 631.90 6.33 0 -2 -1 -0.57 0.81 0 -2 1 -0.72 1.08 0 -2 -1 -1.01 1.45 0 2 -1 -0.06 0.70 0 -2 1 0.13 1.00 0 -2 -1 -0.55 0.90 0 -2 -1 -0.20 0.39 0 2 1 -1.60 1.36 0 2 -1 -0.23 0.73 0 -2 1 -0.50 1.07 0 3 1 768.53 17.81 0 -3 -1 720.40 19.33 0 -3 -1 769.46 19.20 0 -3 1 754.04 17.01 0 -3 1 758.50 16.73 0 3 -1 731.48 18.46 0 -3 -1 755.47 16.40 0 -3 -1 702.80 7.46 0 3 1 754.18 13.09 0 3 -1 704.27 20.68 0 3 -1 728.49 15.74 0 -4 1 -0.41 1.77 0 4 -1 3.62 2.51 0 -4 -1 0.07 1.60 0 4 -1 -0.55 1.40 0 4 1 2.35 2.08 0 4 1 -1.30 2.14 0 -4 -1 3.54 2.82 0 -4 1 -2.04 1.73 0 4 -1 0.00 2.09 0 -4 1 0.54 0.70 0 4 1 0.66 0.81 0 -5 1 1568.10 31.11 0 5 1 1562.43 31.44 0 5 -1 1461.35 38.65 0 -5 -1 1535.81 33.40 0 -5 1 1418.04 30.59 0 5 1 1437.47 33.21 0 5 1 1478.91 25.18 0 5 -1 1419.48 27.18 0 -5 1 1306.13 17.66 0 -6 1 -0.65 2.27 0 -6 1 0.06 0.68 0 -6 -1 -0.32 1.66 0 6 1 -2.33 2.34 0 6 -1 0.13 3.42 0 6 -1 2.56 1.43 0 6 1 -1.12 2.65 0 -6 -1 -1.09 2.64 0 6 -1 -0.61 1.97 0 -6 1 1.07 2.30 0 6 1 0.96 1.54 0 7 1 1.65 2.06 0 -7 -1 1.27 1.82 0 7 1 1.86 2.57 0 -7 1 1.30 0.53 0 7 1 1.82 1.22 0 -7 -1 0.52 1.66 0 7 -1 0.71 1.38 0 7 -1 1.24 1.90 0 7 -1 0.47 3.56 0 -7 1 2.54 2.30 0 -7 1 4.48 3.25 0 8 1 1.56 1.66 0 -8 1 1.38 2.33 0 8 -1 1.32 2.56 0 -8 -1 0.25 1.88 0 -8 -1 1.20 1.63 0 8 1 -1.78 2.76 0 8 -1 -0.79 2.84 0 8 -1 0.50 1.46 0 8 1 -0.30 1.55 0 9 -1 28.87 7.70 0 9 1 39.77 5.75 0 -9 1 38.74 7.02 0 9 -1 43.14 6.27 0 -9 -1 41.79 6.62 0 -9 -1 40.01 7.14 0 9 1 39.54 7.64 0 9 1 39.80 6.80 0 9 -1 43.78 7.84 0 -9 1 44.02 7.15 0 -10 1 -0.64 1.94 0 10 1 2.91 2.91 0 10 -1 1.40 1.78 0 10 -1 0.89 2.60 0 -10 1 5.72 3.66 0 -10 -1 0.75 2.21 0 10 1 0.66 1.79 0 10 1 -0.08 2.18 0 10 -1 -0.09 2.29 0 -10 -1 2.63 2.99 0 11 -1 8.09 3.04 0 11 -1 7.82 4.42 0 -11 -1 6.41 3.74 0 -11 1 5.24 2.72 0 -11 -1 9.77 3.56 0 -11 1 7.51 3.86 0 11 1 6.35 3.63 0 11 -1 9.34 4.49 0 -12 -1 -0.01 1.83 0 -12 -1 1.04 2.24 0 -12 1 0.34 2.72 0 12 -1 -0.70 2.17 0 -12 1 4.14 3.15 0 12 -1 -2.48 2.34 0 12 1 0.50 2.59 0 -13 1 164.31 16.66 0 13 1 167.47 17.88 0 -13 1 170.05 16.53 0 -13 -1 169.88 17.29 0 13 -1 178.44 17.97 0 -13 -1 158.55 14.69 0 14 1 -4.28 3.73 0 -14 1 0.38 1.73 0 14 -1 0.42 2.56 0 14 -1 0.52 3.02 0 -14 -1 -0.53 2.31 0 -15 1 205.72 10.46 0 -15 1 188.56 18.23 0 -15 -1 244.91 12.69 0 -15 1 257.24 12.70 0 15 -1 194.70 20.54 0 -15 -1 245.28 10.07 0 -15 -1 209.76 11.05 0 -15 -1 247.50 12.80 0 -15 1 247.29 12.37 0 -16 -1 1.71 2.14 0 -16 -1 3.10 2.17 0 -16 1 -2.07 2.63 0 -16 1 -0.25 1.57 0 -16 1 0.45 1.48 0 -16 -1 -0.53 1.54 0 -17 -1 2.17 1.52 0 -17 -1 1.91 1.74 0 -17 1 0.51 1.79 0 -17 -1 0.79 1.82 0 17 -1 3.43 1.69 0 -17 1 2.26 2.44 0 -18 -1 -1.91 1.93 0 18 -1 -0.37 1.12 0 -18 1 -1.51 1.69 0 -18 -1 1.06 1.59 0 -18 1 -0.04 1.79 0 -18 -1 1.38 1.92 0 19 -1 13.06 2.33 0 -19 1 10.80 2.44 0 -19 1 10.09 2.74 0 -19 1 12.99 2.95 0 -19 -1 8.01 2.48 0 -19 -1 13.74 2.64 0 19 1 11.63 2.12 0 -19 -1 13.75 2.94 0 -20 1 -0.09 1.21 0 20 -1 2.20 1.40 0 20 -1 1.93 1.65 0 -20 -1 0.13 1.29 0 -20 1 -0.15 1.57 0 -20 1 -0.98 1.84 0 -20 -1 -0.66 1.42 0 -21 1 32.23 4.01 0 21 -1 37.86 3.51 0 -21 -1 31.91 3.04 0 -21 1 29.83 2.83 0 21 -1 32.26 2.98 0 -21 1 30.11 3.84 0 21 -1 34.15 3.08 0 22 -1 -0.25 0.76 0 22 1 -0.57 0.75 0 -22 1 -0.04 0.69 0 22 -1 -1.72 0.93 0 -22 1 1.58 1.20 0 -22 -1 -0.29 0.74 0 23 -1 1.21 0.82 0 -23 -1 0.40 0.56 0 23 -1 0.66 0.63 0 23 1 0.85 0.72 0 0 -2 1339.05 20.01 0 0 2 1319.25 15.24 0 0 2 1320.33 15.63 0 -1 -2 1.12 0.51 0 -1 -2 1.39 0.93 0 -1 -2 3.49 1.04 0 1 2 1.35 0.63 0 -1 -2 2.21 1.10 0 1 -2 3.21 1.89 0 -1 2 2.44 1.20 0 -1 2 1.43 0.46 0 -2 2 7.07 1.59 0 -2 -2 6.92 0.95 0 -2 -2 7.37 1.25 0 -2 -2 6.67 2.16 0 -2 -2 7.64 1.56 0 -2 2 6.46 1.32 0 2 -2 6.95 1.54 0 -2 2 7.65 1.11 0 -2 -2 8.82 1.57 0 2 -2 6.72 3.01 0 -3 2 0.02 1.05 0 -3 -2 1.56 1.07 0 -3 -2 -0.87 2.15 0 -3 -2 0.14 0.55 0 3 -2 -0.41 0.86 0 3 2 0.40 0.61 0 3 -2 -0.05 0.81 0 -3 -2 0.16 0.56 0 -3 -2 -0.04 0.99 0 -3 -2 2.15 1.82 0 -3 2 0.39 1.23 0 -4 -2 166.63 9.53 0 -4 2 163.46 8.97 0 -4 2 169.23 9.62 0 -4 -2 162.42 7.95 0 4 -2 164.34 9.09 0 -4 -2 161.28 9.03 0 -4 -2 151.93 10.67 0 4 2 164.32 8.26 0 4 2 157.79 7.06 0 4 -2 165.30 9.82 0 -4 -2 164.97 9.15 0 5 2 1.01 1.54 0 -5 2 0.58 1.50 0 5 -2 1.11 1.42 0 -5 -2 -1.53 2.34 0 -5 -2 1.69 1.70 0 5 2 -0.04 1.11 0 5 -2 2.32 3.85 0 5 -2 2.14 1.92 0 5 2 1.26 1.45 0 -5 -2 2.35 1.46 0 5 2 1.24 0.62 0 -5 2 0.49 2.08 0 6 -2 7.02 2.11 0 6 -2 6.22 3.11 0 6 2 5.58 2.27 0 6 2 8.97 1.75 0 6 2 8.07 2.27 0 -6 2 6.56 2.68 0 -6 2 5.86 1.23 0 6 2 6.39 2.82 0 -6 -2 8.75 3.43 0 6 -2 7.89 4.91 0 -6 2 4.64 1.48 0 -6 -2 6.88 2.84 0 -6 2 7.23 3.15 0 7 -2 -0.29 2.11 0 -7 2 0.29 1.85 0 7 -2 -1.25 1.77 0 -7 2 -0.50 1.26 0 -7 2 -1.41 2.15 0 7 2 -0.03 1.38 0 -7 -2 0.58 2.50 0 7 -2 -3.39 3.59 0 -7 -2 0.28 1.55 0 7 2 -0.76 2.46 0 7 2 0.15 1.30 0 -8 -2 458.97 21.92 0 -8 -2 466.42 20.61 0 8 2 416.77 18.48 0 -8 2 462.29 21.09 0 8 -2 414.69 26.89 0 8 -2 446.05 19.30 0 8 2 470.47 23.01 0 -8 2 447.45 22.40 0 8 -2 454.37 22.79 0 8 2 453.38 17.82 0 -9 -2 2.44 2.50 0 9 2 2.05 3.14 0 9 -2 0.27 1.38 0 9 -2 1.65 2.71 0 9 2 3.08 1.85 0 -9 2 0.99 2.18 0 9 -2 -1.22 1.89 0 9 2 0.02 1.33 0 -9 2 4.63 3.68 0 -9 -2 0.95 1.44 0 -10 -2 1043.10 36.49 0 -10 2 980.21 35.56 0 10 -2 949.94 42.84 0 -10 2 1055.80 36.12 0 10 2 970.18 38.67 0 10 -2 994.46 31.55 0 -10 -2 996.96 32.39 0 10 2 948.23 29.12 0 10 -2 1046.46 38.02 0 11 -2 0.53 3.56 0 -11 -2 -0.42 1.84 0 11 2 0.42 2.64 0 -11 2 2.59 2.73 0 11 -2 0.75 2.12 0 -11 -2 1.27 2.27 0 -11 2 0.01 2.24 0 11 -2 0.46 1.76 0 -12 -2 205.42 19.27 0 12 -2 204.64 20.39 0 -12 -2 203.90 15.94 0 12 2 217.68 20.34 0 -12 2 207.60 18.21 0 -12 -2 211.06 18.27 0 -12 2 208.27 18.13 0 12 -2 184.18 17.92 0 13 -2 1.54 2.97 0 13 -2 -0.01 2.13 0 13 -2 -0.41 2.74 0 -13 2 1.56 2.92 0 -13 2 2.85 3.57 0 -13 -2 -1.06 2.43 0 13 2 -2.11 2.75 0 14 2 77.91 12.99 0 -14 2 82.76 12.32 0 -14 -2 81.71 13.17 0 14 -2 70.56 12.07 0 -15 2 2.00 2.41 0 15 -2 1.89 1.29 0 -15 2 0.37 1.63 0 -15 -2 -0.20 2.05 0 -15 2 1.38 1.76 0 -15 -2 0.12 1.84 0 -15 -2 1.57 1.74 0 -15 -2 1.66 1.18 0 15 -2 1.67 1.32 0 16 -2 117.09 6.85 0 -16 2 111.60 7.70 0 -16 2 136.88 9.59 0 16 -2 117.48 6.59 0 -16 2 145.33 9.75 0 16 -2 124.51 7.19 0 -16 -2 139.34 8.17 0 -16 -2 115.60 9.29 0 -16 -2 138.32 9.97 0 -16 -2 131.87 7.70 0 -17 -2 0.57 1.86 0 -17 -2 -0.61 1.35 0 -17 2 1.93 2.47 0 17 -2 0.40 1.37 0 -17 -2 2.40 1.96 0 -17 2 -0.07 1.74 0 17 -2 -0.14 1.03 0 18 -2 12.06 2.47 0 18 -2 7.20 2.48 0 -18 -2 17.59 3.75 0 -18 2 17.19 3.77 0 -18 2 16.89 3.58 0 -18 -2 19.73 3.14 0 -18 -2 14.97 3.45 0 -18 2 17.06 2.80 0 -19 -2 -1.10 2.32 0 -19 2 1.73 1.28 0 -19 -2 1.32 1.45 0 19 -2 0.43 1.17 0 -19 2 1.33 1.94 0 -19 2 -2.34 2.10 0 -19 -2 -0.46 1.36 0 -20 2 299.75 9.56 0 -20 2 314.60 13.12 0 20 -2 303.98 10.12 0 -20 -2 329.99 10.87 0 20 -2 330.28 10.95 0 -20 2 330.59 13.48 0 -21 2 0.44 1.31 0 21 -2 2.64 1.44 0 -21 2 1.74 1.74 0 -21 2 -1.08 0.84 0 21 -2 2.32 1.38 0 -21 -2 2.34 1.16 0 21 -2 1.95 1.35 0 21 -2 -1.08 0.97 0 -22 -2 22.85 2.35 0 -22 2 20.32 2.70 0 22 -2 26.05 2.63 0 22 2 24.42 2.35 0 22 -2 22.14 2.49 0 22 -2 25.03 2.45 0 23 -2 0.17 0.59 0 -23 -2 -0.33 0.48 0 23 -2 0.25 0.67 0 23 2 -0.19 0.63 0 0 -3 2.17 1.12 0 0 3 1.92 1.09 0 0 -3 2.28 1.39 0 0 3 1.80 1.05 0 0 3 1.52 1.30 0 -1 -3 1954.25 24.13 0 1 -3 1931.49 35.70 0 -1 -3 1823.79 23.37 0 -1 3 1801.09 13.42 0 -1 3 1878.28 25.25 0 -1 -3 1854.29 17.81 0 1 3 1828.06 20.54 0 -1 -3 1815.19 24.38 0 -2 3 1.93 1.88 0 2 -3 -0.01 2.85 0 -2 -3 0.53 0.71 0 -2 -3 0.11 1.30 0 -2 -3 0.30 1.29 0 -2 3 0.06 0.77 0 -2 3 0.93 1.36 0 -2 3 0.13 0.68 0 -2 -3 0.10 0.83 0 -3 3 1642.05 19.40 0 -3 3 1547.91 24.02 0 -3 -3 1587.99 35.45 0 -3 -3 1601.07 16.80 0 -3 -3 1615.21 25.53 0 -3 3 1621.56 26.40 0 -3 -3 1617.34 24.81 0 -4 -3 2.56 2.49 0 -4 3 4.54 2.70 0 -4 -3 2.25 1.83 0 4 -3 1.01 1.45 0 -4 -3 2.55 1.19 0 -4 -3 2.04 3.33 0 -4 3 1.66 1.53 0 -5 -3 2294.54 40.55 0 -5 -3 2289.63 38.04 0 -5 -3 2113.28 44.62 0 5 -3 2197.33 54.55 0 5 -3 2208.30 39.00 0 5 3 2212.47 30.81 0 5 -3 2152.01 39.01 0 -5 -3 2222.67 38.09 0 -5 -3 2251.14 29.69 0 -5 3 2224.99 36.74 0 -5 3 2259.91 40.22 0 -6 3 0.68 1.03 0 6 -3 -0.18 1.75 0 -6 -3 3.19 2.20 0 6 3 1.97 2.17 0 6 3 1.41 1.50 0 -6 -3 -0.65 1.37 0 6 3 0.93 0.96 0 6 3 1.07 0.90 0 6 -3 2.66 3.67 0 -6 3 2.01 1.99 0 -6 3 0.85 2.16 0 -6 -3 0.98 1.76 0 -6 -3 1.71 2.10 0 6 -3 1.84 1.43 0 -7 -3 347.32 18.90 0 -7 -3 341.00 15.80 0 -7 3 326.55 18.50 0 7 3 325.64 12.59 0 7 -3 319.36 24.01 0 -7 3 317.62 13.13 0 7 3 358.69 14.77 0 7 -3 312.62 17.53 0 -7 3 338.53 17.20 0 7 3 343.20 17.89 0 7 -3 331.29 16.81 0 7 3 328.06 11.25 0 -7 3 306.37 9.90 0 -7 -3 327.66 18.80 0 8 -3 0.69 1.81 0 -8 3 1.43 2.10 0 -8 -3 -0.32 1.90 0 -8 -3 1.00 1.85 0 8 3 -1.46 2.68 0 8 -3 -0.33 2.92 0 -8 3 -2.54 3.14 0 -8 -3 -0.02 1.17 0 8 3 1.04 1.53 0 8 -3 1.23 1.67 0 -8 3 -0.96 1.29 0 9 -3 804.62 28.69 0 -9 -3 786.15 31.39 0 -9 -3 804.11 28.11 0 9 3 771.86 25.30 0 9 3 844.28 33.24 0 -9 3 810.15 33.36 0 -9 3 825.49 30.10 0 9 -3 822.91 32.12 0 9 -3 708.20 38.54 0 -9 -3 774.67 33.92 0 10 3 -0.08 2.65 0 -10 -3 -0.49 2.02 0 -10 3 0.45 2.40 0 -10 -3 2.57 2.14 0 -10 3 0.01 1.81 0 10 -3 1.02 2.98 0 -10 -3 1.83 1.70 0 10 -3 1.57 2.80 0 10 -3 3.27 2.42 0 -11 3 316.11 21.15 0 -11 -3 316.91 21.83 0 11 -3 311.16 22.29 0 -11 3 283.49 21.26 0 11 -3 306.78 26.22 0 -11 -3 326.07 24.38 0 11 3 274.37 22.34 0 12 -3 -3.66 4.50 0 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6.75 0 19 -3 73.91 5.30 0 -19 3 62.27 4.59 0 -20 -3 -0.47 1.50 0 -20 3 1.10 1.83 0 -20 3 0.27 1.51 0 20 -3 -0.09 1.11 0 20 -3 1.25 1.35 0 -20 3 -0.38 1.00 0 20 -3 -0.62 1.22 0 21 -3 218.46 8.08 0 21 -3 212.98 8.04 0 -21 3 180.60 8.83 0 21 -3 200.22 7.42 0 -21 -3 209.00 7.79 0 -21 3 195.85 9.37 0 21 -3 210.16 8.06 0 -22 3 0.04 1.01 0 22 -3 0.82 0.80 0 22 -3 1.34 0.98 0 -22 -3 0.66 0.82 0 22 -3 -0.14 0.86 0 23 3 8.91 1.36 0 23 -3 8.88 1.29 0 23 -3 8.84 1.31 0 -23 -3 9.17 1.31 0 0 4 43.24 4.14 0 0 -4 40.08 4.28 0 0 4 41.60 4.10 0 0 -4 42.67 5.91 0 -1 -4 0.30 1.20 0 -1 4 2.16 1.78 0 1 4 1.53 1.15 0 -1 -4 0.63 0.66 0 -1 -4 0.89 1.26 0 1 -4 0.85 2.56 0 1 4 1.55 1.10 0 -2 4 16.50 2.14 0 -2 4 20.70 3.69 0 2 -4 18.29 6.03 0 -2 -4 16.51 2.85 0 2 4 17.94 2.43 0 -2 -4 15.17 3.06 0 -2 -4 16.61 2.21 0 -3 -4 0.33 0.98 0 3 -4 1.58 4.06 0 -3 4 0.22 0.96 0 3 4 0.28 0.88 0 -3 -4 -0.30 0.87 0 -3 -4 -0.67 1.21 0 -3 4 1.01 1.91 0 -3 4 0.77 1.04 0 -3 4 1.53 2.01 0 -4 -4 305.19 17.44 0 -4 4 305.69 14.59 0 -4 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5.08 -16 4 -6 62.40 7.57 16 4 6 47.42 4.42 -16 -4 -6 34.30 4.53 -16 -4 6 42.67 4.60 -16 4 6 53.33 6.52 -16 -4 -6 55.52 5.15 16 -4 6 46.85 3.80 16 4 6 50.87 4.04 -16 4 -6 50.04 6.79 16 4 6 50.55 4.18 -16 5 6 0.90 1.29 16 5 -6 1.46 1.01 -16 -5 6 0.15 0.84 -16 5 6 -3.25 3.62 16 -5 -6 1.42 1.03 -16 5 6 1.39 1.03 -16 -5 6 0.47 1.03 -16 5 -6 -2.80 5.61 16 5 6 4.98 1.54 -16 -5 -6 0.92 1.48 -16 5 6 -1.04 2.72 -16 -5 6 1.36 1.45 16 -5 6 2.65 1.25 -16 5 -6 0.08 2.05 -16 -5 -6 2.49 1.47 16 5 6 1.67 1.09 16 5 6 3.86 1.39 -16 6 6 60.66 5.24 16 6 -6 62.37 3.85 -16 6 6 89.50 9.49 16 -6 -6 61.26 4.15 -16 -6 6 70.79 4.53 -16 6 -6 126.26 15.69 16 6 6 59.90 4.49 -16 -6 -6 56.67 5.11 -16 -6 6 67.54 4.97 -16 6 6 122.13 12.62 -16 -6 -6 61.32 4.45 16 -6 6 63.15 3.98 16 6 6 66.17 4.19 16 6 6 69.75 4.55 -16 7 6 0.12 0.89 16 7 -6 0.19 0.47 -16 7 6 2.19 1.91 16 -7 -6 -0.19 0.65 -16 -7 6 0.95 0.72 -16 7 -6 5.35 8.95 16 7 6 0.12 0.61 16 -7 6 -1.13 1.12 -16 -7 -6 0.98 1.12 -16 7 6 1.87 3.68 -16 -7 6 0.70 0.79 16 7 6 0.87 0.72 16 7 6 -0.05 0.78 -16 8 -6 4.70 8.35 16 -8 6 4.69 1.39 -16 -8 -6 1.72 1.05 -16 8 6 9.57 3.67 -16 -8 6 5.34 1.34 16 8 6 4.14 1.05 16 0 -7 17.45 2.28 -16 0 7 12.00 3.09 -16 0 7 14.11 2.66 -16 0 7 15.02 3.19 -16 0 -7 19.44 5.16 16 0 7 10.52 1.79 16 -1 -7 7.01 1.71 16 1 -7 6.05 1.48 -16 1 7 0.54 1.84 -16 -1 7 4.84 1.90 -16 -1 7 3.79 1.45 -16 1 7 2.06 1.51 -16 1 7 3.95 2.00 -16 -1 7 3.37 2.07 16 -1 7 3.56 1.42 -16 1 -7 2.85 3.63 -16 -1 -7 8.49 3.69 16 -1 7 2.87 1.07 16 1 7 2.46 1.12 16 2 -7 2.78 1.09 -16 2 7 5.29 2.42 -16 -2 7 4.17 2.11 16 -2 -7 3.31 1.19 -16 -2 7 0.36 0.80 -16 2 7 1.96 1.97 -16 2 7 2.87 1.34 -16 -2 7 6.26 2.39 16 2 7 3.16 1.08 16 -2 7 3.66 1.27 -16 2 -7 2.17 3.51 -16 -2 -7 1.44 1.94 16 2 7 4.02 1.26 16 2 7 4.81 1.53 16 -2 7 4.71 1.33 16 2 7 3.77 1.31 16 3 -7 0.05 0.71 -16 3 7 -1.43 1.57 16 -3 -7 1.46 0.87 -16 3 7 3.81 2.94 16 -3 -7 0.13 0.78 -16 3 7 0.98 1.22 -16 3 -7 4.56 2.91 -16 -3 7 1.29 1.28 16 3 7 0.81 0.99 -16 3 7 0.26 1.28 -16 -3 7 -0.34 1.22 16 -3 7 -0.42 0.92 -16 3 -7 -2.28 3.64 -16 -3 -7 1.11 2.09 16 3 7 2.46 1.16 16 3 7 1.16 0.87 16 -3 7 -0.17 0.73 16 3 7 0.57 0.65 16 -4 -7 4.34 1.10 -16 4 7 8.62 2.43 16 4 -7 4.59 1.12 -16 -4 7 3.73 1.42 -16 4 7 8.12 3.79 16 -4 -7 5.46 1.29 -16 4 7 6.53 1.78 -16 -4 7 4.23 1.48 -16 4 -7 8.66 3.51 16 4 7 5.09 1.50 -16 4 7 8.10 2.79 -16 -4 7 4.10 1.71 16 -4 7 7.50 1.76 -16 4 -7 5.34 3.07 -16 -4 -7 2.03 1.59 16 4 7 4.49 1.41 16 4 7 6.72 1.55 16 -4 7 6.39 1.20 -16 5 7 -0.17 1.13 16 5 -7 0.57 0.66 -16 -5 7 0.70 0.74 -16 5 7 2.32 2.58 -16 -5 7 0.42 0.82 -16 5 -7 5.79 5.23 16 5 7 -0.15 0.73 -16 5 7 -0.73 2.44 -16 -5 7 0.39 0.94 16 -5 7 1.64 1.07 -16 -5 -7 0.35 1.21 16 5 7 -0.33 0.80 16 5 7 1.51 0.95 -16 6 7 -0.72 1.16 16 6 -7 2.20 0.84 -16 6 7 -0.59 2.66 -16 -6 7 3.14 1.03 16 6 7 0.67 0.67 16 -6 7 1.06 0.98 -16 6 7 2.10 2.98 -16 -6 7 0.80 1.03 16 -6 7 0.35 0.71 16 6 7 0.63 0.66 16 6 7 1.41 0.74 16 -7 7 1.11 0.90 16 7 7 2.25 0.85 16 0 -8 174.34 6.63 -16 0 8 181.96 10.72 -16 0 8 162.49 8.24 -16 0 8 167.76 9.55 16 0 8 160.38 7.01 16 0 8 162.35 6.42 16 1 -8 6.49 1.71 -16 1 8 1.30 1.40 -16 -1 8 3.77 1.92 16 -1 -8 3.86 1.16 -16 -1 8 1.25 1.04 -16 1 8 1.02 1.42 -16 1 8 2.89 1.44 -16 -1 8 1.97 1.31 16 -1 8 5.11 1.28 -16 1 -8 -2.09 3.12 -16 -1 -8 1.41 2.52 16 1 8 5.01 1.44 16 -1 8 6.67 1.97 16 1 8 6.44 1.63 16 2 -8 13.51 1.89 -16 2 8 13.06 3.01 -16 -2 8 14.30 2.77 16 -2 -8 12.75 1.83 -16 2 8 11.52 2.99 -16 2 8 7.20 1.92 -16 -2 8 12.60 2.65 16 -2 8 14.36 2.13 -16 2 -8 8.09 3.54 -16 -2 -8 12.84 3.34 16 -2 8 14.34 2.04 16 2 8 11.95 1.81 16 3 -8 1.06 1.04 -16 3 8 1.08 1.14 16 -3 -8 -0.30 0.74 -16 -3 8 0.54 0.93 -16 3 8 -1.31 2.44 -16 -3 8 1.26 1.00 16 -3 8 0.11 0.90 -16 3 -8 -2.28 3.03 -16 -3 -8 -0.94 1.86 16 3 8 2.41 1.20 16 3 8 -0.56 0.76 16 -3 8 0.78 0.76 16 3 8 1.62 1.00 16 4 -8 66.95 3.86 -16 4 8 59.08 5.19 -16 -4 8 61.88 4.34 -16 -4 8 72.17 5.04 -16 -4 -8 59.30 4.75 16 -4 8 64.42 4.09 16 4 8 72.24 4.44 16 4 8 70.69 4.37 16 5 -8 5.86 1.22 -16 5 8 10.64 3.93 -16 -5 8 4.67 1.21 16 -5 8 7.21 1.39 16 5 8 7.01 1.47 16 5 8 7.80 1.53 -16 0 9 22.19 3.51 -16 0 9 17.09 2.70 16 0 9 19.50 2.30 -16 0 -9 17.17 4.06 16 0 -9 21.79 2.28 16 1 -9 41.13 3.02 -16 1 9 34.66 4.11 -16 -1 9 43.21 4.44 -16 1 9 39.28 4.13 -16 -1 9 42.52 4.16 -16 -1 -9 47.16 5.87 16 -1 9 40.75 3.41 16 1 9 36.10 3.11 -16 1 -9 45.96 6.88 16 -1 -9 38.65 2.95 16 2 -9 4.59 1.16 -16 2 9 2.45 1.44 -16 -2 9 2.64 1.17 -16 2 9 5.29 1.99 -16 -2 9 2.02 1.14 -16 -2 -9 3.04 2.02 16 -2 9 5.28 1.34 16 2 9 3.21 1.07 16 3 -9 12.56 1.67 -16 3 9 10.57 2.93 -16 -3 9 10.04 2.01 16 -3 9 13.11 1.88 -17 0 0 0.04 1.56 17 0 0 -0.16 0.77 -17 0 0 1.28 1.82 -17 -1 0 -1.42 1.24 -17 1 0 0.19 1.82 17 -1 0 1.06 1.08 17 1 0 -0.31 0.77 -17 1 0 -0.33 1.67 -17 -1 0 2.05 1.95 17 1 0 0.77 0.75 17 -2 0 0.28 0.80 17 2 0 0.25 0.86 -17 -2 0 -1.40 1.51 17 2 0 1.01 0.82 -17 3 0 -2.82 2.07 17 -3 0 -0.46 0.75 17 3 0 -0.23 0.90 -17 -3 0 -0.51 1.06 17 3 0 0.29 0.73 -17 4 0 -2.23 2.79 17 -4 0 -0.89 0.89 17 4 0 -0.54 0.92 -17 -4 0 -0.90 0.84 17 4 0 1.04 0.78 -17 4 0 1.09 3.20 -17 -4 0 -0.93 1.07 -17 -4 0 -0.18 1.16 -17 4 0 0.80 2.46 -17 5 0 -0.30 1.94 17 -5 0 0.14 0.88 17 5 0 0.63 0.71 -17 5 0 3.23 3.98 -17 -5 0 -1.24 1.37 -17 -5 0 1.16 1.27 -17 5 0 1.50 2.14 -17 6 0 3.56 2.69 17 -6 0 1.70 1.04 17 6 0 0.61 0.79 -17 6 0 -1.86 4.10 -17 -6 0 -0.55 0.94 17 -7 0 0.39 0.74 -17 -7 0 -1.03 0.82 -17 0 -1 109.49 7.62 -17 0 1 114.38 8.37 17 0 -1 113.64 5.99 -17 0 1 119.54 9.35 17 0 1 115.64 6.08 17 0 1 108.32 6.02 -17 1 -1 14.57 3.59 -17 1 1 15.58 3.60 -17 -1 1 14.21 2.72 17 -1 1 15.75 2.37 17 -1 -1 16.35 2.31 17 1 -1 15.29 2.23 17 1 1 13.67 2.16 -17 1 1 13.85 3.32 -17 -1 1 13.98 3.35 17 1 1 15.29 2.40 17 1 -1 13.34 2.01 -17 -1 -1 16.94 3.45 -17 2 -1 20.50 4.63 -17 2 1 20.47 4.41 17 -2 -1 17.80 2.45 17 -2 1 15.52 2.29 17 2 -1 16.26 2.31 17 2 1 17.16 2.30 -17 2 1 13.16 3.29 -17 -2 1 14.56 2.92 17 2 -1 15.04 2.11 17 2 1 15.43 2.33 -17 -2 -1 21.84 3.25 -17 2 -1 17.91 4.35 -17 3 -1 2.44 2.96 -17 3 1 2.72 2.19 17 -3 -1 0.37 0.78 17 -3 1 1.02 0.75 17 3 -1 1.13 0.92 17 3 1 1.01 0.82 -17 -3 1 0.79 1.25 17 3 -1 -0.19 0.85 17 3 1 -0.49 0.77 -17 -3 -1 -0.52 1.42 -17 3 -1 -3.45 3.12 -17 4 -1 102.23 10.49 -17 4 1 74.37 7.87 17 -4 -1 79.49 4.81 17 -4 1 71.33 4.49 -17 -4 1 75.53 4.99 17 4 -1 71.61 4.47 17 4 -1 58.08 4.04 17 4 1 60.80 4.44 -17 4 -1 116.10 12.51 -17 -4 -1 56.30 5.18 -17 -4 1 54.44 5.15 -17 -4 -1 71.33 5.05 -17 4 -1 77.63 8.33 -17 5 -1 31.41 6.14 -17 5 1 21.81 4.06 17 -5 -1 24.30 2.66 17 -5 1 22.50 2.55 -17 -5 1 24.03 2.53 17 5 -1 22.21 2.41 17 5 -1 19.37 2.29 17 5 1 19.39 2.42 -17 5 -1 44.26 9.16 -17 5 1 34.01 6.34 -17 -5 -1 17.47 2.82 -17 -5 1 18.46 2.88 -17 -5 -1 27.65 2.94 -17 -5 1 24.73 2.60 -17 5 -1 28.14 4.43 -17 5 1 27.34 4.44 17 5 1 22.89 2.30 -17 6 -1 206.84 13.79 -17 6 1 171.39 10.73 17 -6 -1 148.18 6.26 17 -6 1 144.47 6.02 17 6 -1 140.80 5.70 17 6 -1 112.98 5.23 17 6 1 127.35 5.95 -17 6 1 196.72 13.51 -17 -6 -1 137.10 7.01 -17 -6 1 141.38 6.93 -17 7 -1 7.36 2.95 -17 7 1 5.93 2.23 17 -7 -1 6.15 1.35 17 7 1 6.14 1.38 -17 7 1 11.40 4.43 -17 0 2 4.50 2.16 17 0 -2 4.86 1.41 17 0 2 4.67 1.36 -17 0 2 4.29 2.19 -17 0 -2 2.03 2.14 -17 1 -2 58.06 6.39 -17 1 2 58.76 6.81 -17 -1 2 52.43 5.13 17 -1 -2 58.22 4.25 17 -1 2 56.64 4.13 17 1 -2 55.74 4.10 -17 1 2 54.95 6.38 17 1 2 56.45 4.15 -17 -1 2 58.76 6.16 17 1 2 53.88 4.37 -17 -1 -2 65.29 6.36 -17 1 -2 61.50 7.48 -17 2 -2 6.49 2.86 -17 2 2 4.47 2.23 -17 -2 2 6.75 1.69 17 -2 -2 6.42 1.59 17 -2 2 8.27 1.77 17 2 -2 5.92 1.38 17 2 2 5.03 1.45 -17 2 2 8.05 2.96 -17 -2 2 8.55 2.29 17 2 2 5.80 1.42 -17 -2 -2 6.46 2.10 -17 2 -2 8.58 3.84 -17 3 -2 16.33 4.57 -17 3 2 13.25 3.50 17 3 -2 13.63 2.08 17 -3 -2 14.28 2.20 17 -3 2 13.21 2.01 17 3 2 13.52 2.07 -17 3 2 16.86 3.45 -17 -3 2 12.86 2.51 17 3 2 13.46 2.20 -17 -3 -2 18.18 2.90 -17 3 -2 22.31 5.27 -17 4 -2 7.39 4.20 -17 4 2 2.01 2.14 17 -4 -2 4.21 1.36 17 -4 2 3.13 1.02 17 4 -2 2.90 0.96 -17 -4 2 2.88 1.15 -17 4 -2 -0.94 2.63 17 4 2 1.49 1.05 17 -4 2 1.46 0.79 -17 -4 -2 -0.31 1.17 -17 -4 2 1.52 1.12 -17 -4 -2 1.48 1.38 -17 4 -2 5.76 3.57 17 4 2 2.34 0.98 -17 5 2 126.67 9.33 17 -5 -2 125.08 5.87 17 -5 2 113.22 5.33 -17 -5 2 129.23 5.78 17 5 -2 120.82 5.39 -17 5 -2 130.85 11.18 17 5 2 105.90 5.79 -17 -5 -2 95.98 6.26 -17 -5 2 98.07 6.15 -17 -5 -2 127.66 6.04 -17 5 -2 127.33 8.54 17 5 2 110.04 5.08 -17 6 -2 35.43 7.23 -17 6 2 24.44 3.98 17 -6 -2 24.18 2.63 17 -6 2 18.33 2.10 17 6 -2 23.23 2.25 -17 6 -2 37.47 9.04 17 6 2 19.87 2.37 -17 6 2 30.48 5.24 -17 -6 -2 23.55 2.98 -17 -6 2 21.49 2.63 -17 7 2 25.71 3.87 17 -7 -2 24.31 2.50 17 7 2 20.00 2.27 -17 0 3 1.18 1.36 17 0 -3 2.90 1.18 17 0 3 2.90 1.01 -17 0 3 2.06 1.53 -17 0 -3 3.13 2.67 -17 1 3 1.07 2.02 -17 -1 3 0.61 1.30 -17 1 3 1.39 1.48 17 -1 -3 -0.06 0.84 17 1 -3 -0.12 0.70 17 -1 3 -0.54 0.73 17 1 3 -0.57 0.82 -17 1 3 -1.07 1.65 -17 -1 3 1.57 1.45 17 1 3 -0.39 1.03 17 -1 3 1.12 0.96 -17 -1 -3 1.86 2.01 -17 2 -3 10.32 3.36 -17 2 3 9.37 3.37 -17 -2 3 3.97 1.42 -17 2 3 9.38 2.76 17 -2 -3 6.88 1.52 17 -2 3 7.02 1.45 17 2 -3 7.44 1.52 17 2 3 7.42 1.53 -17 2 3 9.79 2.81 -17 -2 3 9.12 2.34 17 2 3 7.16 1.75 -17 -2 -3 8.99 2.52 -17 2 -3 12.55 5.05 -17 3 -3 1.46 3.39 -17 3 3 -0.17 2.25 -17 -3 3 -0.24 0.76 -17 3 3 1.40 2.48 17 -3 -3 0.18 0.99 17 -3 3 1.29 0.93 17 3 -3 0.79 0.76 17 3 3 -0.04 0.75 -17 3 3 -2.38 1.62 -17 -3 3 -0.18 1.18 17 3 3 0.76 0.87 -17 -3 -3 3.03 1.56 -17 3 -3 3.42 3.49 17 3 3 -0.57 0.86 -17 4 3 16.82 3.60 17 -4 -3 17.81 2.26 17 4 -3 15.02 1.93 -17 -4 3 18.72 2.58 17 -4 3 12.95 1.82 -17 4 -3 18.59 4.07 17 4 3 13.88 2.26 17 -4 3 16.32 2.04 -17 -4 -3 11.07 2.46 -17 -4 3 16.01 2.72 -17 -4 -3 15.98 2.50 -17 4 -3 22.46 4.26 17 4 3 15.60 2.01 -17 5 -3 3.78 6.62 -17 5 3 1.14 1.93 17 -5 -3 -0.87 0.81 17 -5 3 -1.52 0.89 17 5 -3 -0.13 0.53 -17 -5 3 0.47 0.66 -17 5 -3 1.65 3.35 17 5 3 -0.15 1.03 17 -5 3 -0.90 0.97 -17 -5 -3 0.20 1.13 -17 -5 -3 -1.03 0.97 17 5 3 -0.56 0.57 -17 6 -3 10.18 6.37 -17 6 3 6.28 2.31 17 -6 -3 3.99 1.17 17 6 3 4.69 1.21 -17 0 4 33.29 4.80 -17 0 4 26.69 3.22 17 0 -4 34.44 3.05 17 0 4 32.54 3.01 -17 0 4 38.99 5.12 -17 1 4 90.20 8.01 -17 -1 4 85.54 6.56 -17 1 4 75.38 6.12 17 -1 -4 78.30 4.59 17 1 -4 73.57 4.31 17 -1 4 76.17 4.49 17 1 4 75.45 4.52 -17 1 4 89.18 7.69 -17 -1 4 91.07 7.41 17 1 4 83.97 5.50 -17 -1 -4 98.37 7.56 -17 1 -4 94.26 9.14 17 -1 4 68.50 4.01 17 2 -4 0.59 0.72 -17 2 4 2.76 2.28 -17 -2 4 3.89 1.57 -17 2 4 -0.86 1.56 17 -2 -4 0.91 0.89 17 -2 4 0.26 0.66 17 2 -4 0.89 0.78 17 2 4 1.39 0.64 -17 2 4 1.21 1.43 -17 -2 4 -0.08 1.54 17 2 4 0.45 0.77 17 -2 4 0.61 0.70 -17 -2 -4 -0.53 1.75 -17 2 -4 1.18 3.35 17 3 -4 2.23 0.76 -17 3 4 2.95 1.93 -17 -3 4 -0.57 0.99 -17 3 4 3.08 2.36 17 -3 -4 1.30 0.73 17 -3 4 1.52 0.78 17 3 -4 0.78 0.59 17 3 4 1.18 0.61 -17 3 4 -0.86 1.40 -17 -3 4 0.10 1.03 17 3 4 1.30 1.02 -17 -3 -4 3.31 1.75 -17 3 -4 1.03 3.17 17 3 4 2.02 0.89 -17 4 4 20.85 3.73 17 -4 -4 21.41 2.42 -17 4 4 20.83 3.22 17 4 4 18.10 2.15 -17 -4 4 24.52 2.88 17 4 4 19.56 2.53 -17 -4 -4 22.79 2.75 -17 4 -4 25.23 4.68 17 4 4 20.97 2.43 -17 5 4 147.26 9.27 17 -5 -4 127.71 5.60 -17 -5 4 144.74 6.00 17 5 4 128.09 6.14 17 5 4 137.75 5.65 17 6 4 21.99 2.38 -17 0 5 68.58 6.44 -17 0 5 59.02 4.47 17 0 -5 64.20 3.80 17 0 5 61.40 3.71 -17 0 5 65.95 6.25 17 0 5 52.42 3.59 -17 1 5 23.81 4.26 -17 -1 5 20.37 3.24 -17 1 5 20.54 3.13 17 -1 -5 25.34 2.45 17 1 5 19.78 2.15 -17 1 5 20.14 3.61 -17 -1 5 23.90 3.78 17 -1 5 14.70 1.95 -17 -1 -5 27.35 4.42 -17 1 -5 26.52 5.53 17 2 -5 0.05 0.59 -17 2 5 4.08 2.27 -17 -2 5 0.34 1.11 -17 2 5 0.41 1.57 17 -2 -5 1.61 0.89 17 2 5 0.35 0.52 -17 2 5 1.39 1.32 -17 -2 5 -0.66 1.20 17 -2 5 -0.93 0.77 -17 2 -5 -1.30 3.31 -17 -2 -5 1.32 1.89 17 3 -5 0.40 0.70 -17 3 5 0.73 1.99 -17 3 5 -2.34 2.57 17 -3 -5 -0.86 0.88 17 3 5 -0.07 0.52 -17 3 5 -1.36 1.42 -17 -3 5 0.10 0.86 17 3 5 1.84 1.13 -17 3 -5 3.18 3.19 -17 -3 -5 1.58 1.59 -17 4 5 5.04 2.27 -17 4 5 11.43 3.64 -17 -4 5 7.37 1.54 17 4 5 4.28 1.24 -17 -4 -5 5.71 1.74 17 4 5 7.13 1.40 -17 5 5 45.97 7.05 17 5 5 23.97 2.51 -17 0 6 6.70 2.24 -17 0 6 8.49 2.25 17 0 6 4.61 1.09 -17 0 -6 6.97 2.82 -17 1 6 45.55 5.14 -17 -1 6 46.66 4.58 -17 1 6 42.88 4.64 -17 -1 6 43.51 4.61 -17 -1 -6 52.39 5.54 17 -1 6 36.73 2.92 17 1 6 35.89 2.98 -17 1 -6 47.04 6.39 -17 2 6 5.72 1.97 -17 -2 6 3.35 1.32 -17 -2 -6 2.55 1.45 -17 3 6 2.59 1.33 -17 -3 6 3.98 1.46 0 0 0 0.00 0.00 TITL exp_3204 in Pnma REM Pnma (#62, found as Pnam in a-cb setting) CELL 1.54184 14.578190 19.044118 16.869829 90.0000 90.0000 90.0000 ZERR 2.00 0.000253 0.000422 0.000530 0.0000 0.0000 0.0000 LATT 1 SYMM -x+1/2,-y, z+1/2 SYMM -x, y+1/2,-z SYMM x+1/2,-y+1/2,-z+1/2 SFAC C H N Cl Pd UNIT 200.00 200.00 12.00 4.00 2.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 5450 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 7.628 _oxdiff_exptl_absorpt_empirical_full_min 0.542 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, 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 Pd01 Pd 0.40804(2) 0.65088(2) 0.56936(3) 0.04441(17) Uani 1 1 d . . . . . Cl02 Cl 0.38019(17) 0.750000 0.49281(14) 0.0618(6) Uani 1 2 d S T P . . N003 N 0.3772(3) 0.5639(2) 0.4885(3) 0.0465(11) Uani 1 1 d . . . . . N004 N 0.4306(3) 0.5707(2) 0.6414(3) 0.0486(12) Uani 1 1 d . . . . . N005 N 0.3338(3) 0.6598(2) 0.3428(3) 0.0490(12) Uani 1 1 d . . . . . H005 H 0.348367 0.687380 0.381160 0.059 Uiso 1 1 calc R . . . . N006 N 0.4909(4) 0.750000 0.7764(4) 0.0490(16) Uani 1 2 d S T P . . H006 H 0.510588 0.749999 0.824489 0.059 Uiso 1 2 calc RS T P . . C007 C 0.4727(3) 0.6912(3) 0.7323(4) 0.0481(14) Uani 1 1 d . . . . . C008 C 0.4630(3) 0.5653(3) 0.7177(4) 0.0512(15) Uani 1 1 d . . . . . C009 C 0.1456(6) 0.750000 0.0531(6) 0.059(3) Uani 1 2 d S T P . . H009 H 0.083644 0.750000 0.039961 0.071 Uiso 1 2 calc RS T P . . C00A C 0.3550(3) 0.5444(3) 0.4137(4) 0.0478(14) Uani 1 1 d . . . . . C00B C 0.3891(3) 0.5029(3) 0.5301(4) 0.0497(14) Uani 1 1 d . . . . . C00C C 0.2944(5) 0.750000 0.2368(6) 0.053(2) Uani 1 2 d S T P . . C00D C 0.3064(4) 0.6821(3) 0.2669(4) 0.0526(15) Uani 1 1 d . . . . . C00E C 0.6827(3) 0.6421(3) 0.8004(3) 0.0509(14) Uani 1 1 d . . . . . H00A H 0.727306 0.605045 0.798764 0.076 Uiso 1 1 calc GR . . . . H00B H 0.712700 0.685755 0.811985 0.076 Uiso 1 1 calc GR . . . . H00C H 0.652405 0.645347 0.750018 0.076 Uiso 1 1 calc GR . . . . C00F C 0.3342(3) 0.5882(3) 0.3471(4) 0.0495(14) Uani 1 1 d . . . . . C00G C 0.3543(4) 0.4702(3) 0.4078(4) 0.0569(16) Uani 1 1 d . . . . . H00G H 0.341933 0.443881 0.362587 0.068 Uiso 1 1 calc R . . . . C00H C 0.4852(3) 0.6222(3) 0.7630(4) 0.0505(14) Uani 1 1 d . . . . . C00I C 0.2629(6) 0.750000 0.1525(6) 0.055(2) Uani 1 2 d S T P . . C00J C 0.4681(4) 0.4909(3) 0.7349(4) 0.0553(16) Uani 1 1 d . . . . . H00J H 0.487826 0.470856 0.782183 0.066 Uiso 1 1 calc R . . . . C00K C 0.4418(3) 0.7137(3) 0.6564(4) 0.0482(13) Uani 1 1 d . . . . . C00L C 0.2907(4) 0.6196(3) 0.2243(5) 0.0627(18) Uani 1 1 d . . . . . H00L H 0.271820 0.617082 0.171722 0.075 Uiso 1 1 calc R . . . . C00M C 0.4169(3) 0.5070(3) 0.6108(4) 0.0521(15) Uani 1 1 d . . . . . C00N C 0.1699(6) 0.750000 0.1327(6) 0.056(2) Uani 1 2 d S T P . . C00O C 0.3290(7) 0.750000 0.0930(7) 0.071(3) Uani 1 2 d S T P . . C00P C 0.0989(6) 0.750000 0.1974(6) 0.061(2) Uani 1 2 d S T P . . H00D H 0.128917 0.750000 0.248103 0.092 Uiso 0.5 1 calc RS T P A -1 H00E H 0.061286 0.791159 0.192777 0.092 Uiso 0.5 1 calc R . . A -1 H00F H 0.061286 0.708841 0.192777 0.092 Uiso 0.5 1 calc R . . A -1 C00Q C 0.3075(4) 0.5637(3) 0.2717(4) 0.0613(18) Uani 1 1 d . . . . . H00Q H 0.302260 0.516783 0.257021 0.074 Uiso 1 1 calc R . . . . C00R C 0.5196(3) 0.6152(3) 0.8456(4) 0.0480(13) Uani 1 1 d . . . . . C00S C 0.2090(7) 0.750000 -0.0073(6) 0.064(3) Uani 1 2 d S T P . . C00T C 0.3753(3) 0.4445(3) 0.4818(4) 0.0557(16) Uani 1 1 d . . . . . H00T H 0.379514 0.397610 0.496589 0.067 Uiso 1 1 calc R . . . . C00U C 0.6130(4) 0.6265(3) 0.8640(4) 0.0529(15) Uani 1 1 d . . . . . C00V C 0.4391(4) 0.4559(3) 0.6702(4) 0.0584(17) Uani 1 1 d . . . . . H00V H 0.434322 0.407422 0.665069 0.070 Uiso 1 1 calc R . . . . C00W C 0.3005(7) 0.750000 0.0153(7) 0.076(3) Uani 1 2 d S T P . . H00W H 0.345011 0.750000 -0.024272 0.091 Uiso 1 2 calc RS T P . . C00X C 0.4572(4) 0.6023(4) 0.9071(5) 0.0668(18) Uani 1 1 d . . . . . C00Y C 0.1795(7) 0.750000 -0.0925(6) 0.072(3) Uani 1 2 d S T P . . H00H H 0.134709 0.786224 -0.100694 0.109 Uiso 0.5 1 calc GR . . B -1 H00I H 0.153204 0.705243 -0.105480 0.109 Uiso 0.5 1 calc GR . . B -1 H00K H 0.231721 0.758533 -0.125800 0.109 Uiso 0.5 1 calc GR . . B -1 C00Z C 0.6407(4) 0.6241(4) 0.9428(4) 0.067(2) Uani 1 1 d . . . . . H00Z H 0.702267 0.630956 0.955095 0.080 Uiso 1 1 calc R . . . . C010 C 0.5791(4) 0.6120(5) 1.0030(4) 0.076(2) Uani 1 1 d . . . . . C011 C 0.4879(5) 0.6010(4) 0.9838(5) 0.079(2) Uani 1 1 d . . . . . H011 H 0.446144 0.592623 1.024399 0.095 Uiso 1 1 calc R . . . . C012 C 0.3555(4) 0.5922(5) 0.8888(5) 0.091(3) Uani 1 1 d . . . . . H01A H 0.333611 0.631387 0.858402 0.137 Uiso 1 1 calc GR . . . . H01B H 0.321695 0.589255 0.937568 0.137 Uiso 1 1 calc GR . . . . H01C H 0.347197 0.549731 0.859088 0.137 Uiso 1 1 calc GR . . . . C013 C 0.4314(7) 0.750000 0.1129(7) 0.101(5) Uani 1 2 d S T P . . H01D H 0.439187 0.750000 0.169449 0.152 Uiso 0.5 1 calc RS T P C -1 H01E H 0.459620 0.708841 0.090932 0.152 Uiso 0.5 1 calc R . . C -1 H01F H 0.459620 0.791159 0.090933 0.152 Uiso 0.5 1 calc R . . C -1 C014 C 0.6113(6) 0.6135(7) 1.0881(5) 0.109(4) Uani 1 1 d . . . . . H01G H 0.647787 0.572613 1.098698 0.164 Uiso 1 1 calc GR . . . . H01H H 0.559024 0.613907 1.122756 0.164 Uiso 1 1 calc GR . . . . H01I H 0.647348 0.654915 1.096933 0.164 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 Pd01 0.0248(2) 0.0305(2) 0.0779(3) 0.00189(18) -0.01653(17) -0.00117(13) Cl02 0.0774(14) 0.0285(9) 0.0794(15) 0.000 -0.0359(12) 0.000 N003 0.0249(19) 0.029(2) 0.085(4) -0.005(2) -0.016(2) -0.0003(17) N004 0.025(2) 0.041(2) 0.079(3) 0.005(2) -0.012(2) -0.0022(18) N005 0.036(2) 0.038(2) 0.073(3) -0.005(2) -0.025(2) -0.0012(18) N006 0.031(3) 0.051(4) 0.065(5) 0.000 -0.009(3) 0.000 C007 0.023(2) 0.046(3) 0.076(4) 0.006(3) -0.009(2) -0.002(2) C008 0.022(2) 0.048(3) 0.084(4) 0.009(3) -0.008(3) -0.005(2) C009 0.054(5) 0.033(4) 0.091(7) 0.000 -0.037(5) 0.000 C00A 0.025(2) 0.035(3) 0.083(4) -0.002(3) -0.014(3) 0.000(2) C00B 0.024(2) 0.035(3) 0.090(5) 0.006(3) -0.010(3) -0.003(2) C00C 0.034(4) 0.050(4) 0.077(6) 0.000 -0.024(4) 0.000 C00D 0.036(3) 0.045(3) 0.077(4) -0.003(3) -0.025(3) 0.001(2) C00E 0.027(2) 0.080(4) 0.046(3) 0.012(3) -0.002(2) -0.009(2) C00F 0.025(2) 0.039(3) 0.084(4) -0.005(3) -0.018(3) -0.001(2) C00G 0.028(3) 0.039(3) 0.104(5) -0.012(3) -0.012(3) 0.001(2) C00H 0.021(2) 0.055(3) 0.076(4) 0.014(3) -0.006(2) -0.004(2) C00I 0.046(4) 0.052(5) 0.067(6) 0.000 -0.023(4) 0.000 C00J 0.032(3) 0.049(3) 0.085(5) 0.024(3) -0.002(3) -0.004(2) C00K 0.022(2) 0.048(3) 0.075(4) 0.004(3) -0.010(2) -0.001(2) C00L 0.045(3) 0.045(3) 0.098(5) -0.008(3) -0.030(3) 0.008(3) C00M 0.024(2) 0.037(3) 0.095(5) 0.005(3) -0.007(3) -0.003(2) C00N 0.050(5) 0.030(4) 0.087(7) 0.000 -0.029(5) 0.000 C00O 0.055(6) 0.082(7) 0.077(7) 0.000 -0.042(5) 0.000 C00P 0.046(5) 0.048(5) 0.090(7) 0.000 -0.028(5) 0.000 C00Q 0.038(3) 0.040(3) 0.105(5) -0.014(3) -0.024(3) 0.005(2) C00R 0.028(2) 0.057(3) 0.059(4) 0.012(3) -0.001(2) -0.004(2) C00S 0.073(6) 0.038(4) 0.081(7) 0.000 -0.043(6) 0.000 C00T 0.030(3) 0.032(3) 0.105(5) -0.002(3) -0.011(3) -0.004(2) C00U 0.029(3) 0.067(4) 0.062(4) 0.021(3) 0.003(2) -0.003(3) C00V 0.033(3) 0.039(3) 0.103(5) 0.015(3) -0.001(3) -0.005(2) C00W 0.063(6) 0.074(7) 0.091(8) 0.000 -0.017(6) 0.000 C00X 0.033(3) 0.080(5) 0.087(5) 0.003(4) 0.012(3) -0.012(3) C00Y 0.076(7) 0.055(5) 0.086(7) 0.000 -0.037(6) 0.000 C00Z 0.032(3) 0.112(6) 0.056(4) 0.034(4) 0.001(3) -0.002(3) C010 0.048(4) 0.119(7) 0.062(4) 0.032(4) 0.010(3) -0.003(4) C011 0.050(4) 0.109(6) 0.079(5) 0.011(5) 0.027(4) -0.017(4) C012 0.030(3) 0.120(7) 0.123(7) -0.035(6) 0.024(4) -0.024(4) C013 0.044(5) 0.184(15) 0.076(8) 0.000 -0.023(5) 0.000 C014 0.068(5) 0.198(12) 0.062(5) 0.052(6) 0.011(4) 0.010(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 '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 N003 Pd01 Cl02 103.45(13) . . ? N004 Pd01 Cl02 175.90(16) . . ? N004 Pd01 N003 80.37(19) . . ? C00K Pd01 Cl02 87.94(17) . . ? C00K Pd01 N003 168.6(2) . . ? C00K Pd01 N004 88.3(2) . . ? Pd01 Cl02 Pd01 108.71(9) 7_575 . ? C00A N003 Pd01 146.7(4) . . ? C00A N003 C00B 105.9(5) . . ? C00B N003 Pd01 107.3(4) . . ? C008 N004 Pd01 133.6(4) . . ? C00M N004 Pd01 116.1(4) . . ? C00M N004 C008 110.2(5) . . ? C00F N005 C00D 110.6(5) . . ? C007 N006 C007 109.5(7) . 7_575 ? N006 C007 C00H 122.1(5) . . ? N006 C007 C00K 107.7(5) . . ? C00K C007 C00H 130.2(6) . . ? N004 C008 C00J 106.1(5) . . ? C00H C008 N004 123.1(5) . . ? C00H C008 C00J 130.8(6) . . ? C00S C009 C00N 123.0(8) . . ? N003 C00A C00F 128.4(5) . . ? N003 C00A C00G 109.9(6) . . ? C00G C00A C00F 121.6(6) . . ? N003 C00B C00M 118.7(5) . . ? N003 C00B C00T 111.1(6) . . ? C00T C00B C00M 130.1(5) . . ? C00D C00C C00D 134.8(8) . 7_575 ? C00D C00C C00I 112.6(4) . . ? C00D C00C C00I 112.6(4) 7_575 . ? N005 C00D C00L 104.7(5) . . ? C00C C00D N005 130.2(6) . . ? C00C C00D C00L 125.1(6) . . ? N005 C00F C00A 128.6(5) . . ? N005 C00F C00Q 106.4(5) . . ? C00Q C00F C00A 125.0(5) . . ? C00T C00G C00A 106.8(6) . . ? C007 C00H C00R 117.8(5) . . ? C008 C00H C007 119.9(6) . . ? C008 C00H C00R 122.2(5) . . ? C00N C00I C00C 121.7(9) . . ? C00O C00I C00C 118.3(7) . . ? C00O C00I C00N 120.0(9) . . ? C00V C00J C008 107.8(6) . . ? C007 C00K Pd01 124.7(4) . . ? C00K C00K Pd01 127.70(16) 7_575 . ? C00K C00K C007 107.5(3) 7_575 . ? C00Q C00L C00D 109.5(6) . . ? N004 C00M C00B 117.5(5) . . ? N004 C00M C00V 108.2(6) . . ? C00B C00M C00V 134.2(5) . . ? C009 C00N C00I 118.6(10) . . ? C009 C00N C00P 121.8(8) . . ? C00I C00N C00P 119.6(8) . . ? C00I C00O C013 121.1(9) . . ? C00W C00O C00I 118.7(9) . . ? C00W C00O C013 120.2(11) . . ? C00L C00Q C00F 108.8(5) . . ? C00U C00R C00H 121.1(5) . . ? C00X C00R C00H 119.3(5) . . ? C00X C00R C00U 119.4(6) . . ? C009 C00S C00W 116.4(9) . . ? C009 C00S C00Y 121.1(9) . . ? C00W C00S C00Y 122.6(11) . . ? C00G C00T C00B 106.2(5) . . ? C00R C00U C00E 121.6(5) . . ? C00Z C00U C00E 119.4(5) . . ? C00Z C00U C00R 119.0(5) . . ? C00J C00V C00M 107.6(5) . . ? C00O C00W C00S 123.4(12) . . ? C00R C00X C012 120.2(7) . . ? C011 C00X C00R 119.3(6) . . ? C011 C00X C012 120.4(6) . . ? C010 C00Z C00U 121.5(6) . . ? C00Z C010 C011 118.7(7) . . ? C00Z C010 C014 119.7(6) . . ? C011 C010 C014 121.5(6) . . ? C00X C011 C010 122.1(6) . . ? 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 Pd01 Cl02 2.3229(13) . ? Pd01 N003 2.192(4) . ? Pd01 N004 1.979(5) . ? Pd01 C00K 1.958(6) . ? N003 C00A 1.355(8) . ? N003 C00B 1.367(7) . ? N004 C008 1.375(8) . ? N004 C00M 1.334(7) . ? N005 C00D 1.407(8) . ? N005 C00F 1.365(7) . ? N006 C007 1.371(7) . ? N006 C007 1.371(7) 7_575 ? C007 C00H 1.424(8) . ? C007 C00K 1.423(8) . ? C008 C00H 1.365(9) . ? C008 C00J 1.448(8) . ? C009 C00N 1.389(13) . ? C009 C00S 1.375(14) . ? C00A C00F 1.433(8) . ? C00A C00G 1.417(8) . ? C00B C00M 1.423(9) . ? C00B C00T 1.393(8) . ? C00C C00D 1.400(7) . ? C00C C00D 1.400(7) 7_575 ? C00C C00I 1.494(12) . ? C00D C00L 1.411(8) . ? C00E C00U 1.506(7) . ? C00F C00Q 1.409(9) . ? C00G C00T 1.375(9) . ? C00H C00R 1.487(8) . ? C00I C00N 1.397(11) . ? C00I C00O 1.391(15) . ? C00J C00V 1.346(9) . ? C00K C00K 1.381(11) 7_575 ? C00L C00Q 1.354(9) . ? C00M C00V 1.433(8) . ? C00N C00P 1.504(14) . ? C00O C00W 1.376(15) . ? C00O C013 1.530(12) . ? C00R C00U 1.413(7) . ? C00R C00X 1.402(8) . ? C00S C00W 1.387(13) . ? C00S C00Y 1.501(13) . ? C00U C00Z 1.391(9) . ? C00X C011 1.371(10) . ? C00X C012 1.526(9) . ? C00Z C010 1.375(9) . ? C010 C011 1.384(10) . ? C010 C014 1.511(11) . ?