#------------------------------------------------------------------------------ #$Date: 2019-11-07 22:39:14 +0200 (Thu, 07 Nov 2019) $ #$Revision: 223831 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/97/7049718.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_7049718 loop_ _publ_author_name 'Zhu, Li-Na' 'Deng, Zhao-Peng' 'Ng, Seik Weng' 'Huo, Li-Hua' 'Gao, Shan' _publ_section_title ; Cd(ii) coordination polymers constructed from bis(pyridyl) ligands with an asymmetric spacer in chelating mode and diverse organic dicarboxylates: syntheses, structural evolutions and properties. ; _journal_issue 22 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 7589 _journal_page_last 7601 _journal_paper_doi 10.1039/c9dt00840c _journal_volume 48 _journal_year 2019 _chemical_formula_moiety '[Cd2 (H2 O)2 (C15 H20 N4)2 (C8 H4 O4)], 2(Cl O4), 2(H2 O)' _chemical_formula_sum 'C38 H52 Cd2 Cl2 N8 O16' _chemical_formula_weight 1172.57 _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' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2019-04-01 deposited with the CCDC. 2019-04-14 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 94.159(4) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 11.5239(6) _cell_length_b 10.9162(4) _cell_length_c 18.5387(6) _cell_measurement_reflns_used 2922 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 28.4980 _cell_measurement_theta_min 3.7780 _cell_volume 2325.98(17) _computing_cell_refinement ; CrysAlis Pro (Agilent, 2013) ; _computing_data_collection ; CrysAlis Pro (Agilent, 2013) ; _computing_data_reduction ; CrysAlis Pro (Agilent, 2013) ; _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _diffrn_ambient_temperature 295(2) _diffrn_detector_area_resol_mean 16.1954 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.858 _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_unetI/netI 0.0612 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.858 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 10829 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.858 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.214 _diffrn_reflns_theta_min 3.304 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 1.106 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.86988 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis Pro (Agilent, 2013) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.674 _exptl_crystal_description prism _exptl_crystal_F_000 1188 _exptl_crystal_size_max 0.210 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.120 _refine_diff_density_max 0.970 _refine_diff_density_min -0.821 _refine_diff_density_rms 0.099 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 337 _refine_ls_number_reflns 5929 _refine_ls_number_restraints 212 _refine_ls_restrained_S_all 1.006 _refine_ls_R_factor_all 0.0891 _refine_ls_R_factor_gt 0.0510 _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^)+(0.0666P)^2^+0.8424P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1208 _refine_ls_wR_factor_ref 0.1422 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3899 _reflns_number_total 5929 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9dt00840c2.cif _cod_data_source_block d9070 _cod_depositor_comments 'Adding full bibliography for 7049708--7049720.cif.' _cod_database_code 7049718 _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 0.801 _shelx_estimated_absorpt_t_max 0.879 _shelx_res_file ; TITL P21/n d9070.res created by SHELXL-2018/3 at 19:21:14 on 27-Mar-2019 CELL 0.71073 11.5239 10.9162 18.5387 90 94.1587 90 ZERR 2y 0.0006 0.0004 0.0006 0 0.0038 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O Cl Cd UNIT 76 104 16 32 4 4 ACTA SADI 0.01 Cl1 O3 Cl1 O4 Cl1 O5 Cl1 O6 = CL1' O3' CL1' O4' CL1' O5' CL1' O6'= SADI 0.01 O3 O4 O3 O5 O3 O6 O4 O5 O4 O6 O5 O6 = O3' O4' O3' O5' O3' O6' O4' O5' O4' O6' O5' O6' = O3" O4" O3" O5" O3" O6" O4" O5" O4" O6" O5" O6" PLAN -1 L.S. 10 SIZE 0.21 0.16 0.12 EADP Cl1 Cl1' Cl1" EADP O3 O3' O3" EADP O4 O4' O4" EADP O5 O5' O5" EADP O6 O6' O6" ISOR Cl1 O3 O4 O5 O6 DFIX 1.54 0.01 C7 C8 TEMP 22 WGHT 0.066600 0.842400 FVAR 3.85135 CD1 6 0.383323 0.297117 0.745326 11.00000 0.04327 0.04612 = 0.03231 0.00671 -0.00143 0.00489 O1 4 0.504778 0.204341 0.844314 11.00000 0.07934 0.08200 = 0.04929 0.03423 -0.00116 -0.00014 O2 4 0.336528 0.111937 0.836071 11.00000 0.07452 0.06025 = 0.04489 0.00413 -0.02816 0.01027 O1W 4 0.337061 0.445825 0.648192 11.00000 0.06314 0.05284 = 0.05270 0.00893 -0.00799 -0.00513 AFIX 3 H11 2 0.391641 0.494375 0.638823 11.00000 -1.50000 H12 2 0.277061 0.478555 0.662751 11.00000 -1.50000 AFIX 0 O2W 4 0.675796 0.363039 0.903478 11.00000 0.13934 0.09747 = 0.09960 -0.00911 -0.04437 0.01313 AFIX 3 H21 2 0.747985 0.351359 0.905148 11.00000 -1.50000 H22 2 0.641866 0.300769 0.918268 11.00000 -1.50000 AFIX 0 PART 1 CL1 5 0.552850 0.693392 0.546178 10.50000 0.10661 0.08927 = 0.07020 0.01377 0.02078 0.00121 O3 4 0.436499 0.657833 0.564238 10.50000 0.10250 0.14444 = 0.11616 0.02578 0.02953 -0.01209 O4 4 0.579024 0.817246 0.571741 10.50000 0.10452 0.06253 = 0.15765 -0.02409 -0.01497 0.01894 O5 4 0.638142 0.608181 0.579688 10.50000 0.16228 0.15935 = 0.12959 0.08660 0.06745 0.09344 O6 4 0.558935 0.689616 0.467901 10.50000 0.26782 0.15106 = 0.08900 0.06981 0.07756 0.09952 PART 2 CL1' 5 0.531886 0.696481 0.535598 10.25000 0.10661 0.08927 = 0.07020 0.01377 0.02078 0.00121 O3' 4 0.465888 0.590691 0.557952 10.25000 0.10250 0.14444 = 0.11616 0.02578 0.02953 -0.01209 O4' 4 0.575178 0.765090 0.599287 10.25000 0.10452 0.06253 = 0.15765 -0.02409 -0.01497 0.01894 O5' 4 0.456324 0.773937 0.488537 10.25000 0.16228 0.15935 = 0.12959 0.08660 0.06745 0.09344 O6' 4 0.629251 0.654266 0.495965 10.25000 0.26782 0.15106 = 0.08900 0.06981 0.07756 0.09952 PART 3 CL1" 5 0.550711 0.687162 0.543289 10.25000 0.10661 0.08927 = 0.07020 0.01377 0.02078 0.00121 O3" 4 0.463485 0.675193 0.590811 10.25000 0.10250 0.14444 = 0.11616 0.02578 0.02953 -0.01209 O4" 4 0.642621 0.783972 0.587081 10.25000 0.10452 0.06253 = 0.15765 -0.02409 -0.01497 0.01894 O5" 4 0.518669 0.757272 0.479644 10.25000 0.16228 0.15935 = 0.12959 0.08660 0.06745 0.09344 O6" 4 0.621438 0.587257 0.532802 10.25000 0.26782 0.15106 = 0.08900 0.06981 0.07756 0.09952 PART 0 N1 3 0.224108 -0.104837 0.670579 11.00000 0.05795 0.04231 = 0.03598 -0.00012 0.00079 0.00125 N2 3 0.506762 0.193566 0.671452 11.00000 0.05402 0.05202 = 0.05448 0.00093 0.01540 -0.00161 AFIX 13 0.8800 H2 2 0.487368 0.214660 0.626369 11.00000 -1.20000 AFIX 0 N3 3 0.558266 0.422819 0.750997 11.00000 0.04466 0.05283 = 0.04664 0.00347 -0.00424 0.00103 AFIX 13 0.8800 H3 2 0.595854 0.406180 0.792869 11.00000 -1.20000 AFIX 0 N4 3 0.300608 0.724575 0.809485 11.00000 0.05612 0.04036 = 0.03557 -0.00412 -0.00622 -0.00540 C1 1 0.324091 -0.051699 0.691946 11.00000 0.05908 0.04158 = 0.03745 -0.00031 -0.00142 0.00268 AFIX 43 H1 2 0.345742 -0.050241 0.741251 11.00000 -1.20000 AFIX 0 C2 1 0.397644 0.001202 0.646259 11.00000 0.06086 0.03388 = 0.05528 -0.00052 0.01364 0.00853 C3 1 0.364554 -0.004107 0.572373 11.00000 0.09322 0.06765 = 0.04997 0.01043 0.02666 0.00938 AFIX 43 H3A 2 0.411765 0.029559 0.538908 11.00000 -1.20000 AFIX 0 C4 1 0.262536 -0.059070 0.550034 11.00000 0.10554 0.08840 = 0.03851 0.00599 -0.00205 -0.02006 AFIX 43 H4 2 0.239204 -0.063752 0.501027 11.00000 -1.20000 AFIX 0 C5 1 0.195533 -0.106693 0.599480 11.00000 0.07703 0.06782 = 0.04301 0.00359 -0.00736 -0.00792 AFIX 43 H5 2 0.125402 -0.142929 0.583246 11.00000 -1.20000 AFIX 0 C6 1 0.508875 0.059102 0.675040 11.00000 0.05308 0.04971 = 0.08420 0.00224 0.01238 0.00535 AFIX 23 H6A 2 0.525125 0.034243 0.724986 11.00000 -1.20000 H6B 2 0.571666 0.029106 0.647701 11.00000 -1.20000 AFIX 0 C7 1 0.627936 0.239777 0.690829 11.00000 0.04981 0.08439 = 0.07633 -0.00030 0.01577 0.00257 AFIX 23 PART 1 H7A 2 0.656102 0.205908 0.737210 10.50000 -1.20000 H7B 2 0.679010 0.211691 0.654901 10.50000 -1.20000 AFIX 13 PART 2 H7' 2 0.660818 0.202746 0.735939 10.50000 -1.20000 AFIX 0 PART 0 C8 1 0.632261 0.374764 0.694728 11.00000 0.05364 0.07394 = 0.07561 -0.00198 0.01240 -0.00751 AFIX 13 PART 1 H8' 2 0.603587 0.408104 0.647686 10.50000 -1.20000 AFIX 23 PART 2 H8A 2 0.605788 0.408751 0.648062 10.50000 -1.20000 H8B 2 0.712053 0.400787 0.705786 10.50000 -1.20000 AFIX 0 PART 1 C9 1 0.764111 0.398726 0.705610 10.50000 0.04643 0.06702 = 0.09556 -0.00886 0.01135 -0.00431 AFIX 33 H9A 2 0.777950 0.485329 0.708972 10.50000 -1.50000 H9B 2 0.794690 0.359680 0.749338 10.50000 -1.50000 H9C 2 0.801856 0.366103 0.665300 10.50000 -1.50000 AFIX 0 PART 2 C9' 1 0.707473 0.216903 0.628064 10.50000 0.07948 0.10010 = 0.16100 -0.02362 0.05691 0.00499 AFIX 33 H9'1 2 0.712804 0.130482 0.619301 10.50000 -1.50000 H9'2 2 0.675106 0.256988 0.585111 10.50000 -1.50000 H9'3 2 0.783682 0.249098 0.640975 10.50000 -1.50000 AFIX 0 PART 0 C10 1 0.556394 0.556632 0.745143 11.00000 0.05083 0.05594 = 0.05341 0.00491 0.00123 -0.00757 AFIX 23 H10A 2 0.531044 0.578927 0.695851 11.00000 -1.20000 H10B 2 0.634951 0.587307 0.754961 11.00000 -1.20000 AFIX 0 C11 1 0.376604 0.670181 0.768812 11.00000 0.04758 0.04333 = 0.03547 -0.00266 -0.00668 -0.00784 AFIX 43 H11A 2 0.358905 0.667775 0.719084 11.00000 -1.20000 AFIX 0 C12 1 0.478694 0.617790 0.795393 11.00000 0.04971 0.04548 = 0.04482 0.00577 -0.00485 -0.00581 C13 1 0.503066 0.622892 0.868971 11.00000 0.07041 0.08377 = 0.05203 0.00193 -0.01653 0.01418 AFIX 43 H13 2 0.571198 0.587948 0.889620 11.00000 -1.20000 AFIX 0 C14 1 0.427454 0.679225 0.912064 11.00000 0.08871 0.09718 = 0.03647 -0.00082 -0.01523 0.02279 AFIX 43 H14 2 0.444118 0.683648 0.961836 11.00000 -1.20000 AFIX 0 C15 1 0.327847 0.728487 0.881018 11.00000 0.07332 0.05391 = 0.03631 -0.00276 -0.00436 0.00273 AFIX 43 H15 2 0.276563 0.766374 0.910454 11.00000 -1.20000 AFIX 0 C16 1 0.434250 0.129816 0.867480 11.00000 0.06714 0.04768 = 0.03574 0.00993 -0.00723 0.00962 C17 1 0.384616 0.026517 0.981960 11.00000 0.04791 0.05777 = 0.04025 0.00827 -0.01713 0.00111 AFIX 43 H17 2 0.306648 0.044357 0.970099 11.00000 -1.20000 AFIX 0 C18 1 0.468195 0.062327 0.936479 11.00000 0.05418 0.04075 = 0.03151 0.00528 -0.00801 -0.00006 C19 1 0.582856 0.036037 0.954715 11.00000 0.05103 0.05744 = 0.03333 0.01125 -0.00245 -0.00376 AFIX 43 H19 2 0.639349 0.060383 0.924332 11.00000 -1.20000 AFIX 0 HKLF 4 REM P21/n REM wR2 = 0.1422, GooF = S = 1.016, Restrained GooF = 1.006 for all data REM R1 = 0.0510 for 3899 Fo > 4sig(Fo) and 0.0891 for all 5929 data REM 337 parameters refined using 212 restraints END WGHT 0.0655 0.9654 REM Highest difference peak 0.970, deepest hole -0.821, 1-sigma level 0.099 Q1 1 0.5859 0.2911 0.6465 11.00000 0.05 0.97 ; _shelx_res_checksum 14519 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 Cd1 Cd 0.38332(3) 0.29712(3) 0.74533(2) 0.04077(13) Uani 1 1 d . . . . . O1 O 0.5048(4) 0.2043(3) 0.8443(2) 0.0705(11) Uani 1 1 d . . . . . O2 O 0.3365(3) 0.1119(3) 0.83607(18) 0.0615(10) Uani 1 1 d . . . . . O1W O 0.3371(3) 0.4458(3) 0.64819(18) 0.0568(9) Uani 1 1 d . . . . . H11 H 0.391641 0.494375 0.638823 0.085 Uiso 1 1 d R U . . . H12 H 0.277061 0.478555 0.662751 0.085 Uiso 1 1 d R U . . . O2W O 0.6758(5) 0.3630(4) 0.9035(3) 0.1147(19) Uani 1 1 d . . . . . H21 H 0.747985 0.351359 0.905148 0.172 Uiso 1 1 d R U . . . H22 H 0.641866 0.300769 0.918268 0.172 Uiso 1 1 d R U . . . Cl1 Cl 0.5528(10) 0.6934(9) 0.5462(6) 0.0880(10) Uani 0.5 1 d D U P A 1 O3 O 0.4365(10) 0.6578(13) 0.5642(7) 0.120(4) Uani 0.5 1 d D U P A 1 O4 O 0.5790(10) 0.8172(7) 0.5717(7) 0.109(4) Uani 0.5 1 d D U P A 1 O5 O 0.6381(11) 0.6082(9) 0.5797(6) 0.148(5) Uani 0.5 1 d D U P A 1 O6 O 0.5589(13) 0.6896(11) 0.4679(5) 0.166(6) Uani 0.5 1 d D U P A 1 Cl1' Cl 0.5319(15) 0.6965(15) 0.5356(8) 0.0880(10) Uani 0.25 1 d D . P B 2 O3' O 0.466(2) 0.5907(18) 0.5580(13) 0.120(4) Uani 0.25 1 d D . P B 2 O4' O 0.575(2) 0.7651(19) 0.5993(11) 0.109(4) Uani 0.25 1 d D . P B 2 O5' O 0.4563(18) 0.774(2) 0.4885(11) 0.148(5) Uani 0.25 1 d D . P B 2 O6' O 0.6293(19) 0.654(2) 0.4960(12) 0.166(6) Uani 0.25 1 d D . P B 2 Cl1" Cl 0.551(2) 0.687(2) 0.5433(12) 0.0880(10) Uani 0.25 1 d . . P C 3 O3" O 0.463(2) 0.675(3) 0.5908(13) 0.120(4) Uani 0.25 1 d D . P C 3 O4" O 0.6426(19) 0.7840(17) 0.5871(14) 0.109(4) Uani 0.25 1 d D . P C 3 O5" O 0.519(2) 0.757(2) 0.4796(11) 0.148(5) Uani 0.25 1 d D . P C 3 O6" O 0.621(2) 0.5873(16) 0.5328(11) 0.166(6) Uani 0.25 1 d D . P C 3 N1 N 0.2241(4) -0.1048(3) 0.6706(2) 0.0455(9) Uani 1 1 d . . . . . N2 N 0.5068(4) 0.1936(3) 0.6715(2) 0.0529(10) Uani 1 1 d . . . . . H2 H 0.487368 0.214660 0.626369 0.064 Uiso 1 1 calc R U . . . N3 N 0.5583(4) 0.4228(3) 0.7510(2) 0.0484(10) Uani 1 1 d . . . . . H3 H 0.595854 0.406180 0.792869 0.058 Uiso 1 1 calc R U . . . N4 N 0.3006(4) 0.7246(3) 0.8095(2) 0.0445(9) Uani 1 1 d . . . . . C1 C 0.3241(4) -0.0517(4) 0.6919(3) 0.0463(11) Uani 1 1 d . . . . . H1 H 0.345742 -0.050241 0.741251 0.056 Uiso 1 1 calc R U . . . C2 C 0.3976(5) 0.0012(4) 0.6463(3) 0.0495(12) Uani 1 1 d . . . . . C3 C 0.3646(6) -0.0041(5) 0.5724(3) 0.0692(17) Uani 1 1 d . . . . . H3A H 0.411765 0.029559 0.538908 0.083 Uiso 1 1 calc R U . . . C4 C 0.2625(7) -0.0591(6) 0.5500(3) 0.0778(19) Uani 1 1 d . . . . . H4 H 0.239204 -0.063752 0.501027 0.093 Uiso 1 1 calc R U . . . C5 C 0.1955(5) -0.1067(5) 0.5995(3) 0.0632(14) Uani 1 1 d . . . . . H5 H 0.125402 -0.142929 0.583246 0.076 Uiso 1 1 calc R U . . . C6 C 0.5089(5) 0.0591(4) 0.6750(3) 0.0620(14) Uani 1 1 d . . . . . H6A H 0.525125 0.034243 0.724986 0.074 Uiso 1 1 calc R U . . . H6B H 0.571666 0.029106 0.647701 0.074 Uiso 1 1 calc R U . . . C7 C 0.6279(5) 0.2398(5) 0.6908(4) 0.0696(16) Uani 1 1 d D . . . . H7A H 0.656102 0.205908 0.737210 0.084 Uiso 0.5 1 calc R U P D 1 H7B H 0.679010 0.211691 0.654901 0.084 Uiso 0.5 1 calc R U P D 1 H7' H 0.660818 0.202746 0.735939 0.084 Uiso 0.5 1 calc R U P E 2 C8 C 0.6323(5) 0.3748(5) 0.6947(3) 0.0674(15) Uani 1 1 d D . . . . H8' H 0.603587 0.408104 0.647686 0.081 Uiso 0.5 1 calc R U P F 1 H8A H 0.605788 0.408751 0.648062 0.081 Uiso 0.5 1 calc R U P G 2 H8B H 0.712053 0.400787 0.705786 0.081 Uiso 0.5 1 calc R U P G 2 C9 C 0.7641(9) 0.3987(10) 0.7056(7) 0.069(3) Uani 0.5 1 d . . P H 1 H9A H 0.777950 0.485329 0.708972 0.104 Uiso 0.5 1 calc R U P H 1 H9B H 0.794690 0.359680 0.749338 0.104 Uiso 0.5 1 calc R U P H 1 H9C H 0.801856 0.366103 0.665300 0.104 Uiso 0.5 1 calc R U P H 1 C9' C 0.7075(14) 0.2169(13) 0.6281(10) 0.111(6) Uani 0.5 1 d . . P I 2 H9'1 H 0.712804 0.130482 0.619301 0.167 Uiso 0.5 1 calc R U P I 2 H9'2 H 0.675106 0.256988 0.585111 0.167 Uiso 0.5 1 calc R U P I 2 H9'3 H 0.783682 0.249098 0.640975 0.167 Uiso 0.5 1 calc R U P I 2 C10 C 0.5564(5) 0.5566(4) 0.7451(3) 0.0535(12) Uani 1 1 d . . . . . H10A H 0.531044 0.578927 0.695851 0.064 Uiso 1 1 calc R U . . . H10B H 0.634951 0.587307 0.754961 0.064 Uiso 1 1 calc R U . . . C11 C 0.3766(4) 0.6702(4) 0.7688(2) 0.0426(11) Uani 1 1 d . . . . . H11A H 0.358905 0.667775 0.719084 0.051 Uiso 1 1 calc R U . . . C12 C 0.4787(4) 0.6178(4) 0.7954(3) 0.0471(11) Uani 1 1 d . . . . . C13 C 0.5031(5) 0.6229(6) 0.8690(3) 0.0698(16) Uani 1 1 d . . . . . H13 H 0.571198 0.587948 0.889620 0.084 Uiso 1 1 calc R U . . . C14 C 0.4275(6) 0.6792(6) 0.9121(3) 0.0751(18) Uani 1 1 d . . . . . H14 H 0.444118 0.683648 0.961836 0.090 Uiso 1 1 calc R U . . . C15 C 0.3278(5) 0.7285(4) 0.8810(3) 0.0549(13) Uani 1 1 d . . . . . H15 H 0.276563 0.766374 0.910454 0.066 Uiso 1 1 calc R U . . . C16 C 0.4343(5) 0.1298(4) 0.8675(2) 0.0507(12) Uani 1 1 d . . . . . C17 C 0.3846(4) 0.0265(4) 0.9820(2) 0.0496(12) Uani 1 1 d . . . . . H17 H 0.306648 0.044357 0.970099 0.060 Uiso 1 1 calc R U . . . C18 C 0.4682(4) 0.0623(4) 0.9365(2) 0.0427(10) Uani 1 1 d . . . . . C19 C 0.5829(4) 0.0360(4) 0.9547(2) 0.0475(11) Uani 1 1 d . . . . . H19 H 0.639349 0.060383 0.924332 0.057 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 Cd1 0.0433(2) 0.0461(2) 0.03231(18) 0.00671(14) -0.00143(13) 0.00489(16) O1 0.079(3) 0.082(3) 0.049(2) 0.0342(19) -0.001(2) 0.000(2) O2 0.075(3) 0.060(2) 0.0449(19) 0.0041(16) -0.0282(18) 0.010(2) O1W 0.063(2) 0.0528(18) 0.053(2) 0.0089(16) -0.0080(17) -0.0051(18) O2W 0.139(5) 0.097(3) 0.100(4) -0.009(3) -0.044(3) 0.013(3) Cl1 0.107(2) 0.0893(15) 0.0702(18) 0.0138(12) 0.0208(16) 0.0012(16) O3 0.103(8) 0.144(9) 0.116(9) 0.026(9) 0.030(7) -0.012(8) O4 0.105(8) 0.063(6) 0.158(10) -0.024(6) -0.015(8) 0.019(6) O5 0.162(11) 0.159(8) 0.130(8) 0.087(7) 0.067(8) 0.093(8) O6 0.268(17) 0.151(9) 0.089(8) 0.070(6) 0.078(10) 0.100(9) Cl1' 0.107(2) 0.0893(15) 0.0702(18) 0.0138(12) 0.0208(16) 0.0012(16) O3' 0.103(8) 0.144(9) 0.116(9) 0.026(9) 0.030(7) -0.012(8) O4' 0.105(8) 0.063(6) 0.158(10) -0.024(6) -0.015(8) 0.019(6) O5' 0.162(11) 0.159(8) 0.130(8) 0.087(7) 0.067(8) 0.093(8) O6' 0.268(17) 0.151(9) 0.089(8) 0.070(6) 0.078(10) 0.100(9) Cl1" 0.107(2) 0.0893(15) 0.0702(18) 0.0138(12) 0.0208(16) 0.0012(16) O3" 0.103(8) 0.144(9) 0.116(9) 0.026(9) 0.030(7) -0.012(8) O4" 0.105(8) 0.063(6) 0.158(10) -0.024(6) -0.015(8) 0.019(6) O5" 0.162(11) 0.159(8) 0.130(8) 0.087(7) 0.067(8) 0.093(8) O6" 0.268(17) 0.151(9) 0.089(8) 0.070(6) 0.078(10) 0.100(9) N1 0.058(3) 0.0423(19) 0.036(2) -0.0001(16) 0.0008(18) 0.001(2) N2 0.054(3) 0.052(2) 0.054(3) 0.0009(18) 0.015(2) -0.002(2) N3 0.045(2) 0.053(2) 0.047(2) 0.0035(17) -0.0042(18) 0.0010(19) N4 0.056(2) 0.040(2) 0.036(2) -0.0041(15) -0.0062(18) -0.0054(18) C1 0.059(3) 0.042(2) 0.037(2) -0.0003(19) -0.001(2) 0.003(2) C2 0.061(3) 0.034(2) 0.055(3) -0.001(2) 0.014(2) 0.009(2) C3 0.093(5) 0.068(3) 0.050(3) 0.010(3) 0.027(3) 0.009(3) C4 0.106(5) 0.088(4) 0.039(3) 0.006(3) -0.002(3) -0.020(4) C5 0.077(4) 0.068(3) 0.043(3) 0.004(3) -0.007(3) -0.008(3) C6 0.053(3) 0.050(3) 0.084(4) 0.002(3) 0.012(3) 0.005(3) C7 0.050(3) 0.084(4) 0.076(4) 0.000(3) 0.016(3) 0.003(3) C8 0.054(3) 0.074(4) 0.076(4) -0.002(3) 0.012(3) -0.008(3) C9 0.046(6) 0.067(7) 0.096(9) -0.009(6) 0.011(6) -0.004(6) C9' 0.079(11) 0.100(11) 0.161(17) -0.024(10) 0.057(11) 0.005(9) C10 0.051(3) 0.056(3) 0.053(3) 0.005(2) 0.001(2) -0.008(3) C11 0.048(3) 0.043(2) 0.035(2) -0.0027(19) -0.007(2) -0.008(2) C12 0.050(3) 0.045(2) 0.045(3) 0.006(2) -0.005(2) -0.006(2) C13 0.070(4) 0.084(4) 0.052(3) 0.002(3) -0.017(3) 0.014(3) C14 0.089(5) 0.097(4) 0.036(3) -0.001(3) -0.015(3) 0.023(4) C15 0.073(4) 0.054(3) 0.036(2) -0.003(2) -0.004(2) 0.003(3) C16 0.067(3) 0.048(3) 0.036(2) 0.010(2) -0.007(2) 0.010(3) C17 0.048(3) 0.058(3) 0.040(2) 0.008(2) -0.017(2) 0.001(2) C18 0.054(3) 0.041(2) 0.032(2) 0.0053(18) -0.008(2) 0.000(2) C19 0.051(3) 0.057(3) 0.033(2) 0.011(2) -0.002(2) -0.004(2) 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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 N1 Cd1 N2 173.57(15) 2_556 . N1 Cd1 N4 86.52(14) 2_556 2_546 N2 Cd1 N4 98.49(14) . 2_546 N1 Cd1 N3 101.03(13) 2_556 . N2 Cd1 N3 76.15(14) . . N4 Cd1 N3 154.31(13) 2_546 . N1 Cd1 O1 89.49(14) 2_556 . N2 Cd1 O1 84.25(15) . . N4 Cd1 O1 128.07(13) 2_546 . N3 Cd1 O1 76.93(13) . . N1 Cd1 O1W 95.15(13) 2_556 . N2 Cd1 O1W 89.94(13) . . N4 Cd1 O1W 76.76(12) 2_546 . N3 Cd1 O1W 78.11(12) . . O1 Cd1 O1W 155.05(13) . . C16 O1 Cd1 100.2(3) . . O4 Cl1 O3 110.2(6) . . O4 Cl1 O6 109.0(6) . . O3 Cl1 O6 109.4(6) . . O4 Cl1 O5 109.6(6) . . O3 Cl1 O5 109.6(6) . . O6 Cl1 O5 109.0(6) . . O4' Cl1' O5' 110.0(6) . . O4' Cl1' O3' 109.4(6) . . O5' Cl1' O3' 109.1(6) . . O4' Cl1' O6' 109.9(6) . . O5' Cl1' O6' 109.2(6) . . O3' Cl1' O6' 109.2(6) . . O6" Cl1" O3" 118.4(17) . . O6" Cl1" O5" 115.1(18) . . O3" Cl1" O5" 114.7(19) . . O6" Cl1" O4" 102.0(17) . . O3" Cl1" O4" 102.4(16) . . O5" Cl1" O4" 100.3(14) . . C1 N1 C5 116.7(4) . . C1 N1 Cd1 119.7(3) . 2_546 C5 N1 Cd1 123.4(4) . 2_546 C6 N2 C7 108.2(4) . . C6 N2 Cd1 117.7(3) . . C7 N2 Cd1 107.0(3) . . C10 N3 C8 107.8(4) . . C10 N3 Cd1 123.4(3) . . C8 N3 Cd1 106.6(3) . . C11 N4 C15 117.2(4) . . C11 N4 Cd1 120.0(3) . 2_556 C15 N4 Cd1 122.7(4) . 2_556 N1 C1 C2 124.3(5) . . C1 C2 C3 116.9(5) . . C1 C2 C6 120.8(5) . . C3 C2 C6 122.3(5) . . C4 C3 C2 119.1(5) . . C5 C4 C3 119.3(6) . . N1 C5 C4 123.7(6) . . N2 C6 C2 113.3(4) . . C8 C7 N2 112.0(5) . . C8 C7 C9' 100.2(7) . . N2 C7 C9' 110.8(8) . . C7 C8 N3 111.5(4) . . C7 C8 C9 101.9(6) . . N3 C8 C9 117.2(6) . . N3 C10 C12 113.9(4) . . N4 C11 C12 124.4(4) . . C11 C12 C13 116.7(5) . . C11 C12 C10 120.0(4) . . C13 C12 C10 123.2(5) . . C14 C13 C12 120.3(5) . . C15 C14 C13 119.0(5) . . N4 C15 C14 122.5(5) . . O2 C16 O1 122.1(4) . . O2 C16 C18 119.5(5) . . O1 C16 C18 118.5(5) . . C18 C17 C19 119.9(4) . 3_657 C19 C18 C17 119.5(4) . . C19 C18 C16 120.0(4) . . C17 C18 C16 120.5(4) . . C18 C19 C17 120.6(5) . 3_657 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Cd1 N1 2.321(4) 2_556 Cd1 N2 2.337(4) . Cd1 N4 2.417(4) 2_546 Cd1 N3 2.435(4) . Cd1 O1 2.445(4) . Cd1 O1W 2.454(3) . O1 C16 1.248(6) . O2 C16 1.245(6) . Cl1 O4 1.457(7) . Cl1 O3 1.458(7) . Cl1 O6 1.458(7) . Cl1 O5 1.459(7) . Cl1' O4' 1.455(7) . Cl1' O5' 1.457(7) . Cl1' O3' 1.459(7) . Cl1' O6' 1.460(7) . Cl1" O6" 1.38(3) . Cl1" O3" 1.39(3) . Cl1" O5" 1.43(3) . Cl1" O4" 1.67(3) . N1 C1 1.325(6) . N1 C5 1.335(6) . N2 C6 1.469(6) . N2 C7 1.504(7) . N3 C10 1.465(6) . N3 C8 1.490(7) . N4 C11 1.336(6) . N4 C15 1.341(6) . C1 C2 1.369(7) . C2 C3 1.396(7) . C2 C6 1.493(7) . C3 C4 1.358(9) . C4 C5 1.345(8) . C7 C8 1.476(6) . C7 C9' 1.553(15) . C8 C9 1.541(12) . C10 C12 1.495(7) . C11 C12 1.367(6) . C12 C13 1.374(7) . C13 C14 1.370(8) . C14 C15 1.357(8) . C16 C18 1.503(6) . C17 C18 1.382(7) . C17 C19 1.386(6) 3_657 C18 C19 1.370(7) .