Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Cheng-Yong Su' _publ_contact_author_email CESSCY@MAIL.SYSU.EDU.CN _publ_section_title ; The interplay of coordinative and hydrogen-bonding in directing the [M(4,4'-bpy)2(H2O)2] square-grid networks: Formation of 3D porous framework [Cd(4,4'-bpy)2(H2O)2](ClO4)2(4,4'-bpy)(CH3OH)2 ; loop_ _publ_author_name 'Cheng-Yong Su.' 'Rong Cao.' 'Ji-Jun Jiang.' 'Yong-Ru Liu.' 'Mei Pan.' ; Rui Yang ; # Attachment 'struture.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 671878' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H36 Cd Cl2 N6 O12' _chemical_formula_weight 879.97 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 16.5140(4) _cell_length_b 11.7929(2) _cell_length_c 20.8057(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.894(2) _cell_angle_gamma 90.00 _cell_volume 3949.70(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 0.753 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7947 _exptl_absorpt_correction_T_max 0.8640 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Germini S Ultra' _diffrn_measurement_method '\w and \p scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21245 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.00 _reflns_number_total 8387 _reflns_number_gt 6020 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One of perchlorate anion is disordered along Cl-O bond with three O atoms located at two set of positions. Another perchlorate anion occupies two different sites with all five atoms fractionally distributed. SADI was applied to make all Cl-O bonds and O...O seperations appraximate to model a tetrahedral geometry. The H atoms of the water molecules were fixed with the distances around 0.83 A\% by DFIX. The C-O bonds of the disordered metanol molecules were also fixed around 1.45 A\% by DIFX. The total restraints are 80. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0840P)^2^+12.5000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8387 _refine_ls_number_parameters 495 _refine_ls_number_restraints 80 _refine_ls_R_factor_all 0.0805 _refine_ls_R_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.1726 _refine_ls_wR_factor_gt 0.1620 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.001 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.2500 0.47541(4) 0.2500 0.03207(16) Uani 1 2 d S . . Cd2 Cd -0.2500 -0.50123(4) 0.2500 0.02941(16) Uani 1 2 d S . . N1 N 0.2500 0.2753(4) 0.2500 0.0318(12) Uani 1 2 d S . . N2 N 0.2500 -0.3243(5) 0.2500 0.0377(14) Uani 1 2 d S . . N3 N 0.3458(3) 0.4831(3) 0.35101(19) 0.0311(9) Uani 1 1 d . . . N4 N -0.2500 -0.3003(4) 0.2500 0.0286(12) Uani 1 2 d S . . N5 N -0.2500 0.2990(4) 0.2500 0.0302(12) Uani 1 2 d S . . N6 N -0.3468(3) -0.5064(3) 0.1497(2) 0.0328(9) Uani 1 1 d . . . N7 N 0.0491(3) 0.2802(4) 0.2811(2) 0.0481(12) Uani 1 1 d . . . N8 N -0.0598(3) -0.2948(4) 0.2038(2) 0.0447(11) Uani 1 1 d . . . C1 C 0.2989(4) 0.2157(4) 0.2984(3) 0.0453(14) Uani 1 1 d . . . H1A H 0.3346 0.2561 0.3330 0.054 Uiso 1 1 calc R . . C2 C 0.3000(4) 0.0991(4) 0.3005(3) 0.0428(13) Uani 1 1 d . . . H2A H 0.3350 0.0609 0.3364 0.051 Uiso 1 1 calc R . . C3 C 0.2500 0.0373(5) 0.2500 0.0312(14) Uani 1 2 d S . . C4 C 0.2627(4) -0.2651(4) 0.3065(3) 0.0406(13) Uani 1 1 d . . . H4A H 0.2711 -0.3055 0.3469 0.049 Uiso 1 1 calc R . . C5 C 0.2640(4) -0.1491(4) 0.3084(3) 0.0396(12) Uani 1 1 d D . . H5A H 0.2745 -0.1107 0.3496 0.048 Uiso 1 1 calc R . . C6 C 0.2500 -0.0876(5) 0.2500 0.0299(14) Uani 1 2 d S . . C7 C 0.4179(4) 0.5359(5) 0.3545(3) 0.0441(14) Uani 1 1 d . . . H7B H 0.4277 0.5692 0.3153 0.053 Uiso 1 1 calc R . . C8 C 0.4791(4) 0.5451(5) 0.4111(2) 0.0426(13) Uani 1 1 d . . . H8B H 0.5291 0.5846 0.4104 0.051 Uiso 1 1 calc R . . C9 C 0.4676(3) 0.4965(4) 0.4691(2) 0.0317(10) Uani 1 1 d . . . C10 C 0.3923(3) 0.4423(4) 0.4663(2) 0.0375(11) Uani 1 1 d . . . H10A H 0.3811 0.4082 0.5047 0.045 Uiso 1 1 calc R . . C11 C 0.3336(3) 0.4378(4) 0.4074(2) 0.0359(11) Uani 1 1 d . . . H11A H 0.2823 0.4009 0.4068 0.043 Uiso 1 1 calc R . . C12 C -0.3005(3) -0.2408(4) 0.2027(2) 0.0344(11) Uani 1 1 d . . . H12A H -0.3369 -0.2813 0.1686 0.041 Uiso 1 1 calc R . . C13 C -0.3027(3) -0.1236(4) 0.2008(2) 0.0322(10) Uani 1 1 d . . . H13A H -0.3398 -0.0852 0.1661 0.039 Uiso 1 1 calc R . . C14 C -0.2500 -0.0626(5) 0.2500 0.0250(13) Uani 1 2 d S . . C15 C -0.2500 0.0629(5) 0.2500 0.0259(13) Uani 1 2 d S . . C16 C -0.2566(3) 0.2410(4) 0.1943(2) 0.0354(11) Uani 1 1 d . . . H16A H -0.2614 0.2821 0.1543 0.042 Uiso 1 1 calc R . . C17 C -0.2569(3) 0.1235(4) 0.1917(2) 0.0332(11) Uani 1 1 d . . . H17A H -0.2616 0.0851 0.1508 0.040 Uiso 1 1 calc R . . C18 C -0.4216(4) -0.5497(5) 0.1454(3) 0.0476(14) Uani 1 1 d . . . H18A H -0.4339 -0.5825 0.1838 0.057 Uiso 1 1 calc R . . C19 C -0.4831(4) -0.5500(5) 0.0880(3) 0.0490(14) Uani 1 1 d . . . H19A H -0.5358 -0.5828 0.0877 0.059 Uiso 1 1 calc R . . C20 C -0.4678(3) -0.5026(4) 0.0312(2) 0.0327(11) Uani 1 1 d . . . C21 C -0.3884(3) -0.4587(5) 0.0355(3) 0.0414(12) Uani 1 1 d . . . H21A H -0.3742 -0.4263 -0.0024 0.050 Uiso 1 1 calc R . . C22 C -0.3304(3) -0.4623(5) 0.0944(3) 0.0393(12) Uani 1 1 d . . . H22A H -0.2766 -0.4323 0.0961 0.047 Uiso 1 1 calc R . . C23 C 0.0032(4) 0.2504(5) 0.2228(3) 0.0497(14) Uani 1 1 d . . . H23A H -0.0147 0.3084 0.1911 0.060 Uiso 1 1 calc R . . C24 C -0.0199(4) 0.1414(5) 0.2055(3) 0.0425(13) Uani 1 1 d . . . H24A H -0.0537 0.1258 0.1631 0.051 Uiso 1 1 calc R . . C25 C 0.0060(3) 0.0531(5) 0.2499(2) 0.0340(10) Uani 1 1 d . . . C26 C 0.0547(5) 0.0836(5) 0.3104(3) 0.0579(18) Uani 1 1 d . . . H26A H 0.0741 0.0277 0.3430 0.069 Uiso 1 1 calc R . . C27 C 0.0747(5) 0.1959(5) 0.3227(3) 0.0606(18) Uani 1 1 d . . . H27A H 0.1096 0.2143 0.3641 0.073 Uiso 1 1 calc R . . C28 C -0.0158(3) -0.0670(4) 0.2325(3) 0.0354(11) Uani 1 1 d . . . C29 C -0.0783(4) -0.0973(4) 0.1781(3) 0.0413(12) Uani 1 1 d . . . H29A H -0.1070 -0.0405 0.1495 0.050 Uiso 1 1 calc R . . C30 C -0.0978(4) -0.2099(5) 0.1661(3) 0.0456(13) Uani 1 1 d . . . H30A H -0.1407 -0.2284 0.1290 0.055 Uiso 1 1 calc R . . C31 C 0.0002(4) -0.2666(5) 0.2554(3) 0.0492(14) Uani 1 1 d . . . H31A H 0.0279 -0.3253 0.2831 0.059 Uiso 1 1 calc R . . C32 C 0.0241(4) -0.1547(5) 0.2708(3) 0.0464(13) Uani 1 1 d . . . H32A H 0.0680 -0.1389 0.3077 0.056 Uiso 1 1 calc R . . O2 O -0.1405(2) -0.5006(3) 0.1950(2) 0.0386(8) Uani 1 1 d D . . O1 O 0.1388(3) 0.4798(3) 0.30104(19) 0.0411(9) Uani 1 1 d D . . H12 H 0.109(3) 0.422(3) 0.299(3) 0.051(18) Uiso 1 1 d D . . H22 H -0.112(4) -0.441(3) 0.195(3) 0.055(19) Uiso 1 1 d D . . H11 H 0.138(4) 0.513(5) 0.336(2) 0.06(2) Uiso 1 1 d D . . H21 H -0.151(5) -0.525(5) 0.1563(16) 0.07(2) Uiso 1 1 d D . . Cl1 Cl -0.16373(15) 0.29088(13) 0.04105(8) 0.0708(6) Uani 1 1 d DU A 1 O6 O -0.1782(3) 0.1844(4) 0.0664(2) 0.0705(13) Uani 1 1 d DU A 1 O5 O -0.1798(4) 0.2976(5) -0.0265(3) 0.0612(17) Uiso 0.80 1 d PD A 1 O4 O -0.1747(5) 0.3849(6) 0.0761(4) 0.067(2) Uiso 0.60 1 d PD A 1 O3 O -0.0642(5) 0.2895(8) 0.0573(5) 0.095(3) Uiso 0.60 1 d PD A 1 O5' O -0.1445(12) 0.2905(14) -0.0231(7) 0.029(4) Uiso 0.20 1 d PD B 2 O4' O -0.2513(8) 0.3404(13) 0.0360(7) 0.086(4) Uiso 0.40 1 d PD C 2 O3' O -0.1173(7) 0.3620(10) 0.0859(5) 0.060(3) Uiso 0.40 1 d PD D 2 Cl2 Cl -0.2792(3) -0.1850(3) 0.0064(2) 0.0779(10) Uiso 0.60 1 d PD E 1 O10 O -0.2329(6) -0.2880(7) 0.0300(4) 0.079(2) Uiso 0.60 1 d PD E 1 O9 O -0.2498(6) -0.0986(7) 0.0547(4) 0.070(2) Uiso 0.60 1 d PD E 1 O8 O -0.2541(8) -0.1577(12) -0.0551(6) 0.134(5) Uiso 0.60 1 d PD E 1 O7 O -0.3651(6) -0.2019(10) -0.0042(6) 0.122(4) Uiso 0.60 1 d PD E 1 Cl2' Cl -0.2508(4) -0.1693(6) -0.0073(3) 0.0849(17) Uiso 0.40 1 d P F 2 O10' O -0.1686(19) -0.184(2) -0.0075(13) 0.168(9) Uiso 0.40 1 d P F 2 O9' O -0.2884(15) -0.142(2) 0.0532(11) 0.133(7) Uiso 0.40 1 d P F 2 O8' O -0.2757(9) -0.0833(13) -0.0561(7) 0.077(4) Uiso 0.40 1 d P F 2 O7' O -0.2924(13) -0.2710(19) -0.0391(10) 0.126(6) Uiso 0.40 1 d P F 2 O1W O -0.3481(4) 0.3939(6) -0.0899(3) 0.0613(17) Uiso 0.70 1 d PD G -1 C1W C -0.399(7) 0.305(13) -0.071(5) 0.21(8) Uiso 0.10 1 d PD G -1 O5W O -0.367(2) 0.112(3) -0.0274(17) 0.149(12) Uiso 0.25 1 d PD H -1 C5W C -0.304(3) 0.0824(18) -0.0630(16) 0.121(15) Uiso 0.25 1 d PD H -1 O2W O -0.4129(10) 0.1984(15) -0.0718(8) 0.070(4) Uiso 0.30 1 d PD I 2 C2W C -0.4982(8) 0.2112(13) -0.0709(7) 0.110(4) Uiso 0.80 1 d PD I 2 O3W O 0.4574(8) 0.0330(11) 0.4210(6) 0.091(4) Uiso 0.50 1 d PD J 1 C3W C 0.4687(11) -0.0647(14) 0.4639(8) 0.098(5) Uiso 0.60 1 d PD J 1 O4W O 0.4637(18) 0.133(2) 0.4617(13) 0.106(8) Uiso 0.25 1 d PD K -2 C4W C 0.500(3) 0.022(3) 0.477(2) 0.099(12) Uiso 0.25 1 d PD K -2 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 0.0398(3) 0.0167(2) 0.0289(3) 0.000 -0.0153(2) 0.000 Cd2 0.0324(3) 0.0148(2) 0.0334(3) 0.000 -0.0091(2) 0.000 N1 0.031(3) 0.018(3) 0.041(3) 0.000 -0.004(2) 0.000 N2 0.050(4) 0.018(3) 0.036(3) 0.000 -0.009(3) 0.000 N3 0.035(2) 0.0239(19) 0.026(2) -0.0007(14) -0.0111(17) -0.0035(16) N4 0.037(3) 0.017(3) 0.029(3) 0.000 0.002(2) 0.000 N5 0.041(3) 0.013(2) 0.034(3) 0.000 0.004(3) 0.000 N6 0.033(2) 0.0197(19) 0.036(2) -0.0044(15) -0.0115(18) 0.0008(15) N7 0.054(3) 0.031(2) 0.054(3) -0.012(2) 0.001(2) -0.005(2) N8 0.047(3) 0.031(2) 0.057(3) -0.008(2) 0.012(2) -0.0050(19) C1 0.056(4) 0.021(2) 0.049(3) -0.003(2) -0.009(3) -0.001(2) C2 0.049(3) 0.024(2) 0.050(3) 0.004(2) -0.002(3) 0.003(2) C3 0.032(4) 0.016(3) 0.045(4) 0.000 0.007(3) 0.000 C4 0.060(4) 0.021(2) 0.033(3) 0.0024(19) -0.006(2) -0.002(2) C5 0.056(3) 0.019(2) 0.036(3) -0.0034(19) -0.004(2) -0.003(2) C6 0.031(3) 0.017(3) 0.039(4) 0.000 0.000(3) 0.000 C7 0.051(3) 0.043(3) 0.029(3) 0.011(2) -0.013(2) -0.014(2) C8 0.041(3) 0.046(3) 0.031(3) 0.010(2) -0.013(2) -0.014(2) C9 0.036(3) 0.027(2) 0.025(2) -0.0024(17) -0.009(2) 0.0015(19) C10 0.041(3) 0.039(3) 0.026(2) 0.003(2) -0.006(2) -0.004(2) C11 0.034(3) 0.034(3) 0.032(3) 0.001(2) -0.009(2) -0.006(2) C12 0.045(3) 0.018(2) 0.034(3) -0.0035(18) -0.004(2) 0.0006(19) C13 0.045(3) 0.017(2) 0.031(2) 0.0024(17) 0.000(2) 0.0046(19) C14 0.036(4) 0.014(3) 0.025(3) 0.000 0.010(3) 0.000 C15 0.032(3) 0.016(3) 0.030(3) 0.000 0.006(3) 0.000 C16 0.056(3) 0.016(2) 0.033(3) 0.0044(18) 0.007(2) -0.001(2) C17 0.050(3) 0.020(2) 0.029(2) -0.0008(17) 0.008(2) -0.001(2) C18 0.041(3) 0.045(3) 0.046(3) 0.016(2) -0.014(2) -0.012(2) C19 0.039(3) 0.046(3) 0.051(3) 0.013(3) -0.013(3) -0.012(3) C20 0.029(3) 0.025(2) 0.037(3) -0.0062(18) -0.005(2) 0.0014(18) C21 0.032(3) 0.055(3) 0.033(3) -0.011(2) -0.001(2) -0.004(2) C22 0.031(3) 0.046(3) 0.037(3) -0.009(2) -0.003(2) -0.002(2) C23 0.051(4) 0.031(3) 0.058(4) -0.001(3) -0.007(3) 0.004(2) C24 0.042(3) 0.034(3) 0.042(3) -0.005(2) -0.012(2) 0.000(2) C25 0.035(3) 0.029(3) 0.037(3) -0.0022(19) 0.006(2) 0.000(2) C26 0.094(5) 0.035(3) 0.036(3) 0.001(2) -0.003(3) -0.007(3) C27 0.091(5) 0.038(3) 0.043(3) -0.008(3) -0.007(3) -0.006(3) C28 0.034(3) 0.030(3) 0.043(3) -0.004(2) 0.012(2) -0.002(2) C29 0.048(3) 0.030(3) 0.043(3) 0.000(2) 0.004(2) -0.004(2) C30 0.050(3) 0.037(3) 0.045(3) -0.009(2) 0.002(3) -0.009(2) C31 0.051(3) 0.031(3) 0.060(4) 0.000(2) -0.001(3) 0.000(2) C32 0.046(3) 0.030(3) 0.056(3) -0.005(2) -0.003(3) 0.001(2) O2 0.038(2) 0.0263(19) 0.048(2) -0.0060(15) 0.0020(18) -0.0041(15) O1 0.046(2) 0.0293(19) 0.042(2) -0.0098(16) -0.0035(18) -0.0033(16) Cl1 0.1335(18) 0.0392(8) 0.0389(8) 0.0016(6) 0.0177(9) -0.0002(9) O6 0.091(4) 0.048(3) 0.070(3) 0.011(2) 0.013(3) -0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Cd1 O1 2.318(4) 2 ? Cd1 O1 2.318(4) . ? Cd1 N3 2.333(4) 2 ? Cd1 N3 2.333(4) . ? Cd1 N1 2.360(5) . ? Cd1 N2 2.362(5) 1_565 ? Cd2 N6 2.329(4) . ? Cd2 N6 2.329(4) 2_455 ? Cd2 O2 2.345(4) . ? Cd2 O2 2.345(4) 2_455 ? Cd2 N5 2.356(5) 1_545 ? Cd2 N4 2.369(5) . ? N1 C1 1.340(6) 2 ? N1 C1 1.340(6) . ? N2 C4 1.342(6) 2 ? N2 C4 1.342(6) . ? N2 Cd1 2.362(5) 1_545 ? N3 C7 1.332(7) . ? N3 C11 1.345(6) . ? N4 C12 1.338(5) . ? N4 C12 1.338(5) 2_455 ? N5 C16 1.329(5) . ? N5 C16 1.329(5) 2_455 ? N5 Cd2 2.356(5) 1_565 ? N6 C18 1.322(7) . ? N6 C22 1.344(7) . ? N7 C27 1.324(8) . ? N7 C23 1.326(7) . ? N8 C31 1.331(7) . ? N8 C30 1.338(8) . ? C1 C2 1.376(7) . ? C1 H1A 0.9500 . ? C2 C3 1.390(6) . ? C2 H2A 0.9500 . ? C3 C2 1.390(6) 2 ? C3 C6 1.472(8) . ? C4 C5 1.368(7) . ? C4 H4A 0.9500 . ? C5 C6 1.390(6) . ? C5 H5A 0.9500 . ? C6 C5 1.390(6) 2 ? C7 C8 1.374(7) . ? C7 H7B 0.9500 . ? C8 C9 1.389(7) . ? C8 H8B 0.9500 . ? C9 C10 1.387(7) . ? C9 C9 1.480(9) 3_666 ? C10 C11 1.383(6) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 C13 1.384(6) . ? C12 H12A 0.9500 . ? C13 C14 1.387(6) . ? C13 H13A 0.9500 . ? C14 C13 1.387(6) 2_455 ? C14 C15 1.480(8) . ? C15 C17 1.391(6) . ? C15 C17 1.391(6) 2_455 ? C16 C17 1.387(6) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C19 1.384(7) . ? C18 H18A 0.9500 . ? C19 C20 1.381(8) . ? C19 H19A 0.9500 . ? C20 C21 1.394(7) . ? C20 C20 1.485(10) 3_445 ? C21 C22 1.378(7) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C24 1.366(8) . ? C23 H23A 0.9500 . ? C24 C25 1.394(7) . ? C24 H24A 0.9500 . ? C25 C26 1.382(7) . ? C25 C28 1.486(7) . ? C26 C27 1.374(8) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C28 C32 1.379(8) . ? C28 C29 1.398(8) . ? C29 C30 1.375(8) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C32 1.393(8) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? O2 H22 0.85(2) . ? O2 H21 0.84(2) . ? O1 H12 0.83(2) . ? O1 H11 0.83(2) . ? Cl1 O4 1.361(7) . ? Cl1 O5 1.373(5) . ? Cl1 O6 1.403(5) . ? Cl1 O3 1.603(8) . ? Cl2 O7 1.400(10) . ? Cl2 O9 1.438(9) . ? Cl2 O10 1.461(9) . ? Cl2 O8 1.466(11) . ? Cl2' O10' 1.37(3) . ? Cl2' O8' 1.430(16) . ? Cl2' O7' 1.46(2) . ? Cl2' O9' 1.56(2) . ? O1W C1W 1.45(2) . ? O5W C5W 1.450(19) . ? O2W C2W 1.420(15) . ? O3W C3W 1.444(15) . ? O4W C4W 1.45(2) . ? 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 Cd1 O1 177.41(19) 2 . ? O1 Cd1 N3 91.92(15) 2 2 ? O1 Cd1 N3 87.98(15) . 2 ? O1 Cd1 N3 87.98(15) 2 . ? O1 Cd1 N3 91.92(15) . . ? N3 Cd1 N3 175.54(19) 2 . ? O1 Cd1 N1 91.29(9) 2 . ? O1 Cd1 N1 91.29(9) . . ? N3 Cd1 N1 92.23(9) 2 . ? N3 Cd1 N1 92.23(9) . . ? O1 Cd1 N2 88.71(9) 2 1_565 ? O1 Cd1 N2 88.71(9) . 1_565 ? N3 Cd1 N2 87.77(9) 2 1_565 ? N3 Cd1 N2 87.77(9) . 1_565 ? N1 Cd1 N2 180.000(1) . 1_565 ? N6 Cd2 N6 177.00(18) . 2_455 ? N6 Cd2 O2 90.71(15) . . ? N6 Cd2 O2 89.30(15) 2_455 . ? N6 Cd2 O2 89.30(15) . 2_455 ? N6 Cd2 O2 90.71(15) 2_455 2_455 ? O2 Cd2 O2 179.66(17) . 2_455 ? N6 Cd2 N5 88.50(9) . 1_545 ? N6 Cd2 N5 88.50(9) 2_455 1_545 ? O2 Cd2 N5 90.17(9) . 1_545 ? O2 Cd2 N5 90.17(9) 2_455 1_545 ? N6 Cd2 N4 91.50(9) . . ? N6 Cd2 N4 91.50(9) 2_455 . ? O2 Cd2 N4 89.83(9) . . ? O2 Cd2 N4 89.83(9) 2_455 . ? N5 Cd2 N4 180.0 1_545 . ? C1 N1 C1 116.8(6) 2 . ? C1 N1 Cd1 121.6(3) 2 . ? C1 N1 Cd1 121.6(3) . . ? C4 N2 C4 117.3(6) 2 . ? C4 N2 Cd1 121.3(3) 2 1_545 ? C4 N2 Cd1 121.3(3) . 1_545 ? C7 N3 C11 116.4(4) . . ? C7 N3 Cd1 119.0(3) . . ? C11 N3 Cd1 124.6(3) . . ? C12 N4 C12 116.7(5) . 2_455 ? C12 N4 Cd2 121.6(3) . . ? C12 N4 Cd2 121.6(3) 2_455 . ? C16 N5 C16 118.1(5) . 2_455 ? C16 N5 Cd2 121.0(3) . 1_565 ? C16 N5 Cd2 121.0(3) 2_455 1_565 ? C18 N6 C22 117.1(4) . . ? C18 N6 Cd2 121.0(4) . . ? C22 N6 Cd2 121.9(3) . . ? C27 N7 C23 115.6(5) . . ? C31 N8 C30 116.9(5) . . ? N1 C1 C2 123.3(5) . . ? N1 C1 H1A 118.3 . . ? C2 C1 H1A 118.3 . . ? C1 C2 C3 119.9(5) . . ? C1 C2 H2A 120.0 . . ? C3 C2 H2A 120.0 . . ? C2 C3 C2 116.7(6) . 2 ? C2 C3 C6 121.7(3) . . ? C2 C3 C6 121.7(3) 2 . ? N2 C4 C5 123.0(5) . . ? N2 C4 H4A 118.5 . . ? C5 C4 H4A 118.5 . . ? C4 C5 C6 119.8(5) . . ? C4 C5 H5A 120.1 . . ? C6 C5 H5A 120.1 . . ? C5 C6 C5 117.1(6) 2 . ? C5 C6 C3 121.5(3) 2 . ? C5 C6 C3 121.5(3) . . ? N3 C7 C8 124.1(5) . . ? N3 C7 H7B 117.9 . . ? C8 C7 H7B 117.9 . . ? C7 C8 C9 119.7(5) . . ? C7 C8 H8B 120.2 . . ? C9 C8 H8B 120.2 . . ? C10 C9 C8 116.6(4) . . ? C10 C9 C9 122.1(6) . 3_666 ? C8 C9 C9 121.2(6) . 3_666 ? C11 C10 C9 120.0(5) . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? N3 C11 C10 123.1(5) . . ? N3 C11 H11A 118.5 . . ? C10 C11 H11A 118.5 . . ? N4 C12 C13 123.6(5) . . ? N4 C12 H12A 118.2 . . ? C13 C12 H12A 118.2 . . ? C12 C13 C14 119.2(4) . . ? C12 C13 H13A 120.4 . . ? C14 C13 H13A 120.4 . . ? C13 C14 C13 117.6(5) . 2_455 ? C13 C14 C15 121.2(3) . . ? C13 C14 C15 121.2(3) 2_455 . ? C17 C15 C17 118.2(6) . 2_455 ? C17 C15 C14 120.9(3) . . ? C17 C15 C14 120.9(3) 2_455 . ? N5 C16 C17 123.2(4) . . ? N5 C16 H16A 118.4 . . ? C17 C16 H16A 118.4 . . ? C16 C17 C15 118.7(4) . . ? C16 C17 H17A 120.7 . . ? C15 C17 H17A 120.7 . . ? N6 C18 C19 123.7(5) . . ? N6 C18 H18A 118.1 . . ? C19 C18 H18A 118.1 . . ? C20 C19 C18 119.8(5) . . ? C20 C19 H19A 120.1 . . ? C18 C19 H19A 120.1 . . ? C19 C20 C21 116.5(5) . . ? C19 C20 C20 122.1(6) . 3_445 ? C21 C20 C20 121.4(6) . 3_445 ? C22 C21 C20 120.2(5) . . ? C22 C21 H21A 119.9 . . ? C20 C21 H21A 119.9 . . ? N6 C22 C21 122.7(5) . . ? N6 C22 H22A 118.6 . . ? C21 C22 H22A 118.6 . . ? N7 C23 C24 124.0(6) . . ? N7 C23 H23A 118.0 . . ? C24 C23 H23A 118.0 . . ? C23 C24 C25 120.1(5) . . ? C23 C24 H24A 119.9 . . ? C25 C24 H24A 119.9 . . ? C26 C25 C24 116.0(5) . . ? C26 C25 C28 122.0(5) . . ? C24 C25 C28 122.0(5) . . ? C27 C26 C25 119.2(6) . . ? C27 C26 H26A 120.4 . . ? C25 C26 H26A 120.4 . . ? N7 C27 C26 125.0(6) . . ? N7 C27 H27A 117.5 . . ? C26 C27 H27A 117.5 . . ? C32 C28 C29 116.5(5) . . ? C32 C28 C25 121.1(5) . . ? C29 C28 C25 122.3(5) . . ? C30 C29 C28 119.6(5) . . ? C30 C29 H29A 120.2 . . ? C28 C29 H29A 120.2 . . ? N8 C30 C29 123.8(5) . . ? N8 C30 H30A 118.1 . . ? C29 C30 H30A 118.1 . . ? N8 C31 C32 122.9(6) . . ? N8 C31 H31A 118.5 . . ? C32 C31 H31A 118.5 . . ? C28 C32 C31 120.2(5) . . ? C28 C32 H32A 119.9 . . ? C31 C32 H32A 119.9 . . ? Cd2 O2 H22 120(4) . . ? Cd2 O2 H21 117(5) . . ? H22 O2 H21 106(3) . . ? Cd1 O1 H12 119(4) . . ? Cd1 O1 H11 125(4) . . ? H12 O1 H11 108(3) . . ? O4 Cl1 O5 118.9(4) . . ? O4 Cl1 O6 118.2(4) . . ? O5 Cl1 O6 115.2(3) . . ? O4 Cl1 O3 98.5(5) . . ? O5 Cl1 O3 99.9(4) . . ? O6 Cl1 O3 99.4(4) . . ? O7 Cl2 O9 112.5(6) . . ? O7 Cl2 O10 111.8(6) . . ? O9 Cl2 O10 106.5(5) . . ? O7 Cl2 O8 111.6(7) . . ? O9 Cl2 O8 109.7(7) . . ? O10 Cl2 O8 104.3(6) . . ? O10' Cl2' O8' 102.3(14) . . ? O10' Cl2' O7' 105.3(16) . . ? O8' Cl2' O7' 103.2(11) . . ? O10' Cl2' O9' 127.1(16) . . ? O8' Cl2' O9' 108.9(11) . . ? O7' Cl2' O9' 107.6(14) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H12 N7 0.83(2) 1.94(2) 2.763(6) 169(5) . O2 H22 N8 0.85(2) 1.92(2) 2.756(6) 170(6) . _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 2.060 _refine_diff_density_min -1.123 _refine_diff_density_rms 0.129