# 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 _publ_contact_author_name 'Jhy-Der Chen' _publ_contact_author_email JDCHEN@CYCU.EDU.TW _publ_section_title ; Ligand isomerism-controlled structural diversity of cadmium(II) perchlorate coordination polymers containing dipyridyladipoamide ligands ; loop_ _publ_author_name 'Jhy-Der Chen.' 'Yi-Fen Hsu.' 'Hui-Ling Hu.' 'Davide Proserpio' 'Chia-Jun Wu.' ; Chun-Wei Yeh ; # Attachment 'Cd26_36_46-cif.txt' data_L2 _database_code_depnum_ccdc_archive 'CCDC 695629' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H18 N4 O2' _chemical_formula_weight 298.34 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_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' _cell_length_a 9.4559(12) _cell_length_b 7.8465(10) _cell_length_c 10.6879(17) _cell_angle_alpha 90.00 _cell_angle_beta 108.137(11) _cell_angle_gamma 90.00 _cell_volume 753.60(18) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 5.07 _cell_measurement_theta_max 12.47 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 316 _exptl_absorpt_coefficient_mu 0.090 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9200 _exptl_absorpt_correction_T_max 0.9719 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1801 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_sigmaI/netI 0.0488 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1305 _reflns_number_gt 764 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. ; _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^)+(0.0549P)^2^+0.0939P] 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 1305 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1010 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1272 _refine_ls_wR_factor_gt 0.1048 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 O O 0.6307(2) 0.1498(3) -0.16323(17) 0.0834(7) Uani 1 1 d . . . N1 N 0.5891(2) 0.1936(3) 0.0327(2) 0.0563(6) Uani 1 1 d . . . N2 N 0.2233(2) 0.3438(3) -0.17779(19) 0.0689(7) Uani 1 1 d . . . C1 C 0.9236(3) 0.0287(5) -0.0433(3) 0.0650(8) Uani 1 1 d . . . C2 C 0.8285(3) 0.0912(5) 0.0358(3) 0.0668(9) Uani 1 1 d . . . C3 C 0.6737(3) 0.1464(4) -0.0434(2) 0.0577(7) Uani 1 1 d . . . C4 C 0.4466(2) 0.2660(3) -0.0088(2) 0.0505(7) Uani 1 1 d . . . C5 C 0.3885(3) 0.3330(4) 0.0838(3) 0.0667(8) Uani 1 1 d . . . C6 C 0.2492(3) 0.4054(4) 0.0448(3) 0.0738(9) Uani 1 1 d . . . C7 C 0.1709(3) 0.4094(4) -0.0859(3) 0.0668(8) Uani 1 1 d . . . C8 C 0.3590(3) 0.2723(4) -0.1384(2) 0.0652(8) Uani 1 1 d . . . H1N H 0.630(3) 0.189(3) 0.123(3) 0.066(8) Uiso 1 1 d . . . H1A H 0.869(3) -0.066(4) -0.105(3) 0.082(9) Uiso 1 1 d . . . H1B H 0.930(3) 0.133(4) -0.107(3) 0.098(10) Uiso 1 1 d . . . H2A H 0.879(4) 0.188(4) 0.088(3) 0.105(12) Uiso 1 1 d . . . H2B H 0.822(3) 0.011(4) 0.101(3) 0.083(10) Uiso 1 1 d . . . H5 H 0.444(3) 0.327(3) 0.169(3) 0.071(8) Uiso 1 1 d . . . H6 H 0.205(3) 0.451(4) 0.110(3) 0.082(9) Uiso 1 1 d . . . H7 H 0.070(3) 0.460(3) -0.122(2) 0.063(7) Uiso 1 1 d . . . H8 H 0.394(3) 0.226(3) -0.206(3) 0.081(9) Uiso 1 1 d . . . 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 O 0.0653(12) 0.138(2) 0.0462(10) 0.0030(11) 0.0166(9) 0.0235(13) N1 0.0441(11) 0.0844(17) 0.0378(11) 0.0005(11) 0.0092(9) 0.0019(11) N2 0.0552(14) 0.0937(19) 0.0510(12) 0.0039(12) 0.0066(11) 0.0096(13) C1 0.0512(15) 0.089(2) 0.0571(16) 0.0048(17) 0.0197(13) 0.0064(16) C2 0.0518(16) 0.096(3) 0.0529(16) 0.0052(18) 0.0161(14) 0.0047(17) C3 0.0518(14) 0.0743(19) 0.0455(13) 0.0019(13) 0.0129(12) -0.0013(14) C4 0.0433(13) 0.0642(17) 0.0414(13) 0.0020(11) 0.0095(11) -0.0038(13) C5 0.0570(17) 0.096(2) 0.0429(14) -0.0063(15) 0.0094(13) 0.0033(17) C6 0.0598(18) 0.101(2) 0.0613(17) -0.0080(17) 0.0204(15) 0.0117(18) C7 0.0508(16) 0.080(2) 0.0653(17) 0.0058(15) 0.0123(14) 0.0105(15) C8 0.0535(16) 0.096(2) 0.0419(14) 0.0000(14) 0.0089(13) 0.0114(16) _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 O C3 1.217(3) . ? N1 C3 1.358(3) . ? N1 C4 1.401(3) . ? N2 C7 1.333(3) . ? N2 C8 1.343(3) . ? C1 C2 1.496(4) . ? C1 C1 1.522(5) 3_755 ? C2 C3 1.508(4) . ? C4 C8 1.375(3) . ? C4 C5 1.377(4) . ? C5 C6 1.374(4) . ? C6 C7 1.363(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 C3 N1 C4 127.5(2) . . ? C7 N2 C8 117.9(2) . . ? C2 C1 C1 112.2(3) . 3_755 ? C1 C2 C3 115.2(2) . . ? O C3 N1 123.9(2) . . ? O C3 C2 123.0(2) . . ? N1 C3 C2 113.1(2) . . ? C8 C4 C5 117.4(2) . . ? C8 C4 N1 123.5(2) . . ? C5 C4 N1 119.1(2) . . ? C6 C5 C4 119.9(2) . . ? C7 C6 C5 119.0(3) . . ? N2 C7 C6 122.5(3) . . ? N2 C8 C4 123.2(3) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.142 _refine_diff_density_min -0.143 _refine_diff_density_rms 0.037 #===END data_1 _database_code_depnum_ccdc_archive 'CCDC 695630' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H18 Cd Cl2 N4 O10' _chemical_formula_weight 609.64 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(1)/n loop_ _symmetry_equiv_pos_as_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' _cell_length_a 9.1730(11) _cell_length_b 11.3098(13) _cell_length_c 11.0517(10) _cell_angle_alpha 90.00 _cell_angle_beta 107.793(8) _cell_angle_gamma 90.00 _cell_volume 1091.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 4.85 _cell_measurement_theta_max 12.48 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.855 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 1.307 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3425 _exptl_absorpt_correction_T_max 0.3683 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2543 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0392 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1917 _reflns_number_gt 1500 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. ; _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^)+(0.0344P)^2^+1.1440P] 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 1917 _refine_ls_number_parameters 187 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0511 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0793 _refine_ls_wR_factor_gt 0.0713 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Cd Cd 0.0000 0.0000 0.5000 0.03539(15) Uani 1 2 d S . . O1 O 0.0695(3) 0.0653(3) 0.6984(2) 0.0453(7) Uani 1 1 d . . . N1 N 0.2440(4) -0.0684(3) 0.5604(3) 0.0333(7) Uani 1 1 d . . . N2 N 0.2854(4) -0.0454(3) 0.7828(3) 0.0330(8) Uani 1 1 d . . . C1 C 0.3355(4) -0.0788(3) 0.6799(3) 0.0304(8) Uani 1 1 d . . . C2 C 0.4820(5) -0.1260(4) 0.7084(4) 0.0429(10) Uani 1 1 d . . . C3 C 0.5361(5) -0.1594(4) 0.6121(5) 0.0492(12) Uani 1 1 d . . . C4 C 0.4435(5) -0.1481(4) 0.4870(4) 0.0461(11) Uani 1 1 d . . . C5 C 0.3011(5) -0.1030(4) 0.4671(4) 0.0430(11) Uani 1 1 d . . . C6 C 0.1663(4) 0.0215(4) 0.7906(3) 0.0333(9) Uani 1 1 d . . . C7 C 0.1559(5) 0.0409(5) 0.9223(4) 0.0386(10) Uani 1 1 d . . . C8 C 0.0066(5) -0.0086(5) 0.9341(4) 0.0403(9) Uani 1 1 d . . . Cl Cl 0.04009(12) 0.28397(10) 0.37950(9) 0.0408(3) Uani 1 1 d . . . O2 O 0.1017(4) 0.1698(3) 0.4216(5) 0.0858(14) Uani 1 1 d . . . O3 O 0.0054(4) 0.3444(4) 0.4796(3) 0.0759(12) Uani 1 1 d . . . O4 O 0.1511(4) 0.3479(3) 0.3401(3) 0.0649(10) Uani 1 1 d . . . O5 O -0.0965(4) 0.2715(4) 0.2762(3) 0.0707(11) Uani 1 1 d . . . H2N H 0.335(5) -0.066(4) 0.856(4) 0.050(14) Uiso 1 1 d . . . H2 H 0.536(5) -0.137(4) 0.793(4) 0.053(13) Uiso 1 1 d . . . H3 H 0.630(5) -0.196(4) 0.629(4) 0.040(11) Uiso 1 1 d . . . H4 H 0.483(5) -0.177(4) 0.419(4) 0.059(14) Uiso 1 1 d . . . H5 H 0.240(5) -0.100(4) 0.387(4) 0.038(11) Uiso 1 1 d . . . H7A H 0.164(5) 0.123(4) 0.934(4) 0.046(13) Uiso 1 1 d . . . H7B H 0.239(6) 0.001(4) 0.983(5) 0.053(13) Uiso 1 1 d . . . H8A H -0.077(6) 0.021(4) 0.872(5) 0.060(15) Uiso 1 1 d . . . H8B H 0.002(6) -0.091(5) 0.911(4) 0.059(15) Uiso 1 1 d . . . 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 Cd 0.0295(2) 0.0487(3) 0.0260(2) 0.0035(2) 0.00561(14) 0.0073(2) O1 0.0434(17) 0.0599(19) 0.0297(14) -0.0020(14) 0.0067(13) 0.0188(16) N1 0.0310(17) 0.039(2) 0.0305(16) 0.0031(15) 0.0102(13) 0.0070(15) N2 0.0285(17) 0.0440(19) 0.0250(16) -0.0004(14) 0.0059(14) 0.0031(14) C1 0.0268(19) 0.034(2) 0.0326(19) -0.0011(17) 0.0123(16) 0.0001(17) C2 0.031(2) 0.055(3) 0.041(2) 0.002(2) 0.0083(19) 0.008(2) C3 0.035(2) 0.056(3) 0.060(3) 0.001(2) 0.019(2) 0.014(2) C4 0.050(2) 0.051(3) 0.047(3) -0.001(2) 0.029(2) 0.008(2) C5 0.045(3) 0.054(3) 0.032(2) 0.002(2) 0.014(2) 0.005(2) C6 0.0279(19) 0.044(3) 0.0281(18) -0.0040(17) 0.0081(15) -0.0038(18) C7 0.033(2) 0.053(3) 0.029(2) -0.0044(19) 0.0087(17) 0.002(2) C8 0.036(2) 0.056(3) 0.032(2) -0.004(2) 0.0142(17) -0.005(2) Cl 0.0389(5) 0.0417(6) 0.0420(5) 0.0016(5) 0.0126(4) 0.0012(5) O2 0.066(2) 0.060(2) 0.146(4) 0.047(2) 0.054(3) 0.019(2) O3 0.054(2) 0.116(3) 0.058(2) -0.031(2) 0.0173(17) 0.007(2) O4 0.059(2) 0.062(2) 0.077(2) 0.0132(19) 0.0246(18) -0.0143(18) O5 0.057(2) 0.082(3) 0.059(2) -0.0126(19) -0.0045(17) -0.014(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 Cd O1 2.215(3) 3_556 ? Cd O1 2.215(3) . ? Cd N1 2.267(3) . ? Cd N1 2.267(3) 3_556 ? Cd O2 2.409(4) . ? Cd O2 2.409(4) 3_556 ? O1 C6 1.233(4) . ? N1 C1 1.336(5) . ? N1 C5 1.350(5) . ? N2 C6 1.353(5) . ? N2 C1 1.403(5) . ? C1 C2 1.390(5) . ? C2 C3 1.359(6) . ? C3 C4 1.390(6) . ? C4 C5 1.356(6) . ? C6 C7 1.503(5) . ? C7 C8 1.522(6) . ? C8 C8 1.511(8) 3_557 ? Cl O3 1.417(3) . ? Cl O5 1.421(3) . ? Cl O4 1.421(3) . ? Cl O2 1.430(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 O1 Cd O1 180.0 3_556 . ? O1 Cd N1 97.89(10) 3_556 . ? O1 Cd N1 82.11(10) . . ? O1 Cd N1 82.11(10) 3_556 3_556 ? O1 Cd N1 97.89(10) . 3_556 ? N1 Cd N1 180.0 . 3_556 ? O1 Cd O2 86.30(15) 3_556 . ? O1 Cd O2 93.70(15) . . ? N1 Cd O2 85.53(12) . . ? N1 Cd O2 94.47(12) 3_556 . ? O1 Cd O2 93.70(15) 3_556 3_556 ? O1 Cd O2 86.30(15) . 3_556 ? N1 Cd O2 94.47(12) . 3_556 ? N1 Cd O2 85.53(12) 3_556 3_556 ? O2 Cd O2 180.00(11) . 3_556 ? C6 O1 Cd 127.0(3) . . ? C1 N1 C5 117.1(3) . . ? C1 N1 Cd 125.9(2) . . ? C5 N1 Cd 116.9(3) . . ? C6 N2 C1 132.4(3) . . ? N1 C1 C2 122.0(3) . . ? N1 C1 N2 121.0(3) . . ? C2 C1 N2 117.0(3) . . ? C3 C2 C1 119.3(4) . . ? C2 C3 C4 119.7(4) . . ? C5 C4 C3 117.5(4) . . ? N1 C5 C4 124.4(4) . . ? O1 C6 N2 124.3(3) . . ? O1 C6 C7 119.9(4) . . ? N2 C6 C7 115.8(3) . . ? C6 C7 C8 110.7(3) . . ? C8 C8 C7 112.0(5) 3_557 . ? O3 Cl O5 108.8(2) . . ? O3 Cl O4 110.3(2) . . ? O5 Cl O4 110.0(2) . . ? O3 Cl O2 110.0(3) . . ? O5 Cl O2 109.6(3) . . ? O4 Cl O2 108.1(2) . . ? Cl O2 Cd 132.8(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.509 _refine_diff_density_min -0.503 _refine_diff_density_rms 0.080 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 695631' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H52 Cd Cl2 N8 O16' _chemical_formula_weight 1036.16 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6762(11) _cell_length_b 9.9743(11) _cell_length_c 12.4337(14) _cell_angle_alpha 76.553(9) _cell_angle_beta 78.663(9) _cell_angle_gamma 79.367(9) _cell_volume 1132.2(2) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 26 _cell_measurement_theta_min 5.12 _cell_measurement_theta_max 12.47 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 534 _exptl_absorpt_coefficient_mu 0.677 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8203 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4673 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0550 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3919 _reflns_number_gt 3162 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. ; _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^)+(0.0842P)^2^+1.8685P] 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 3919 _refine_ls_number_parameters 305 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0808 _refine_ls_R_factor_gt 0.0617 _refine_ls_wR_factor_ref 0.1605 _refine_ls_wR_factor_gt 0.1467 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Cd Cd -0.5000 0.5000 0.5000 0.0455(2) Uani 1 2 d S . . O1 O -0.7042(5) 0.6278(6) -0.0706(4) 0.0770(14) Uani 1 1 d . . . O2 O -0.9069(5) 1.0818(5) 0.7206(4) 0.0701(12) Uani 1 1 d . . . N1 N -0.5348(5) 0.5847(5) 0.3106(4) 0.0473(11) Uani 1 1 d . . . N2 N -0.6842(5) 0.4883(5) 0.0969(4) 0.0499(11) Uani 1 1 d . . . H2A H -0.6992 0.4078 0.1367 0.060 Uiso 1 1 calc R . . N3 N -0.6967(5) 0.6607(5) 0.5550(4) 0.0484(11) Uani 1 1 d . . . N4 N -0.8159(5) 0.8591(5) 0.7770(4) 0.0552(12) Uani 1 1 d . . . H4A H -0.7865 0.7987 0.8325 0.066 Uiso 1 1 calc R . . C1 C -0.5964(6) 0.5184(6) 0.2561(4) 0.0435(12) Uani 1 1 d . . . H1A H -0.6261 0.4339 0.2937 0.052 Uiso 1 1 calc R . . C2 C -0.6190(5) 0.5684(6) 0.1462(4) 0.0439(12) Uani 1 1 d . . . C3 C -0.5742(6) 0.6947(6) 0.0906(5) 0.0508(14) Uani 1 1 d . . . H3A H -0.5853 0.7315 0.0164 0.061 Uiso 1 1 calc R . . C4 C -0.5132(7) 0.7636(7) 0.1487(5) 0.0590(15) Uani 1 1 d . . . H4B H -0.4842 0.8494 0.1140 0.071 Uiso 1 1 calc R . . C5 C -0.4947(7) 0.7065(6) 0.2577(5) 0.0566(15) Uani 1 1 d . . . H5A H -0.4528 0.7546 0.2954 0.068 Uiso 1 1 calc R . . C6 C -0.7265(6) 0.5204(7) -0.0042(5) 0.0523(14) Uani 1 1 d . . . C7 C -0.8018(7) 0.4160(7) -0.0300(6) 0.0637(17) Uani 1 1 d . . . H7A H -0.7600 0.3230 0.0028 0.076 Uiso 1 1 calc R . . H7B H -0.7872 0.4237 -0.1106 0.076 Uiso 1 1 calc R . . C8 C -0.9590(8) 0.4349(9) 0.0131(11) 0.111(4) Uani 1 1 d . . . H8A H -1.0000 0.3690 -0.0131 0.167 Uiso 1 1 calc R . . H8B H -0.9710 0.4076 0.0942 0.167 Uiso 1 1 calc R . . C9 C -0.7072(6) 0.7122(6) 0.6478(4) 0.0491(13) Uani 1 1 d . . . H9A H -0.6360 0.6811 0.6921 0.059 Uiso 1 1 calc R . . C10 C -0.8207(6) 0.8104(6) 0.6796(4) 0.0453(13) Uani 1 1 d . . . C11 C -0.9275(6) 0.8548(6) 0.6162(5) 0.0545(15) Uani 1 1 d . . . H11A H -1.0058 0.9183 0.6373 0.065 Uiso 1 1 calc R . . C12 C -0.9167(7) 0.8038(7) 0.5207(6) 0.0606(16) Uani 1 1 d . . . H12A H -0.9872 0.8330 0.4757 0.073 Uiso 1 1 calc R . . C13 C -0.7990(7) 0.7079(6) 0.4922(5) 0.0572(15) Uani 1 1 d . . . H13A H -0.7915 0.6755 0.4267 0.069 Uiso 1 1 calc R . . C14 C -0.8534(6) 0.9915(7) 0.7900(5) 0.0550(15) Uani 1 1 d . . . C15 C -0.8204(7) 1.0210(8) 0.8956(5) 0.0678(18) Uani 1 1 d . . . C16 C -0.9260(19) 0.967(3) 1.0049(15) 0.061(4) Uani 0.42 1 d P . . C16' C -0.9583(19) 1.0626(16) 0.9753(10) 0.061(3) Uani 0.58 1 d P . . C17 C -0.6269(9) 0.1936(9) 0.5082(7) 0.087(2) Uani 1 1 d . . . H17A H -0.7157 0.1586 0.5197 0.130 Uiso 1 1 calc R . . H17B H -0.5710 0.1406 0.5638 0.130 Uiso 1 1 calc R . . H17C H -0.5758 0.1857 0.4350 0.130 Uiso 1 1 calc R . . O3 O -0.6541(5) 0.3387(4) 0.5173(4) 0.0617(11) Uani 1 1 d . . . H3C H -0.7502 0.3738 0.5329 0.074 Uiso 1 1 calc R . . Cl Cl 0.3397(2) 0.10517(19) 0.22526(15) 0.0736(5) Uani 1 1 d . . . O4 O 0.2535(7) 0.2310(6) 0.2493(5) 0.1019(19) Uani 1 1 d . . . O5 O 0.2999(11) -0.0024(7) 0.3083(8) 0.175(4) Uani 1 1 d . . . O6 O 0.3333(14) 0.0896(9) 0.1187(7) 0.192(5) Uani 1 1 d . . . O7 O 0.4781(9) 0.1170(15) 0.2232(10) 0.207(5) Uani 1 1 d . . . C18 C 0.0024(9) 0.5547(10) 0.3123(9) 0.101(3) Uani 1 1 d . . . O8 O -0.1271(11) 0.6476(11) 0.3129(9) 0.073(3) Uani 0.60 1 d P . . O8' O -0.0841(18) 0.6488(18) 0.3650(15) 0.078(4) Uani 0.40 1 d P . . 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 Cd 0.0475(4) 0.0528(4) 0.0367(3) -0.0175(3) -0.0070(2) 0.0025(3) O1 0.093(4) 0.080(3) 0.061(3) 0.003(3) -0.040(3) -0.014(3) O2 0.095(3) 0.052(3) 0.060(3) -0.014(2) -0.013(3) 0.002(2) N1 0.053(3) 0.055(3) 0.036(2) -0.016(2) -0.009(2) -0.001(2) N2 0.060(3) 0.052(3) 0.040(3) -0.008(2) -0.016(2) -0.007(2) N3 0.048(3) 0.056(3) 0.038(2) -0.013(2) -0.007(2) 0.006(2) N4 0.070(3) 0.054(3) 0.036(2) -0.014(2) -0.007(2) 0.011(2) C1 0.050(3) 0.044(3) 0.036(3) -0.012(2) -0.007(2) 0.000(2) C2 0.038(3) 0.047(3) 0.045(3) -0.013(2) -0.008(2) 0.006(2) C3 0.055(3) 0.055(3) 0.044(3) -0.007(3) -0.015(3) -0.007(3) C4 0.068(4) 0.050(3) 0.058(4) -0.003(3) -0.013(3) -0.011(3) C5 0.069(4) 0.054(4) 0.054(4) -0.020(3) -0.019(3) -0.006(3) C6 0.047(3) 0.063(4) 0.050(3) -0.017(3) -0.021(3) 0.006(3) C7 0.062(4) 0.076(4) 0.061(4) -0.032(3) -0.024(3) 0.011(3) C8 0.067(5) 0.096(6) 0.205(11) -0.089(7) -0.045(6) -0.001(4) C9 0.051(3) 0.058(3) 0.038(3) -0.016(3) -0.012(2) 0.007(3) C10 0.052(3) 0.046(3) 0.035(3) -0.012(2) 0.000(2) 0.000(2) C11 0.052(3) 0.050(3) 0.057(4) -0.015(3) -0.011(3) 0.010(3) C12 0.058(4) 0.062(4) 0.066(4) -0.021(3) -0.028(3) 0.011(3) C13 0.066(4) 0.061(4) 0.048(3) -0.020(3) -0.020(3) 0.005(3) C14 0.056(3) 0.060(4) 0.047(3) -0.020(3) 0.002(3) -0.002(3) C15 0.069(4) 0.090(5) 0.053(4) -0.039(4) 0.001(3) -0.015(4) C16 0.058(13) 0.090(16) 0.049(9) -0.043(10) -0.002(8) -0.015(12) C16' 0.072(11) 0.056(8) 0.057(7) -0.024(6) 0.001(6) -0.008(8) C17 0.102(6) 0.090(6) 0.073(5) -0.036(4) 0.013(4) -0.030(5) O3 0.060(3) 0.064(3) 0.067(3) -0.023(2) -0.006(2) -0.016(2) Cl 0.0838(12) 0.0656(11) 0.0683(11) -0.0133(9) -0.0092(9) -0.0069(9) O4 0.125(5) 0.066(3) 0.100(4) -0.013(3) 0.010(4) -0.010(3) O5 0.215(9) 0.067(4) 0.172(8) 0.012(5) 0.070(7) 0.005(5) O6 0.353(14) 0.125(6) 0.115(6) -0.054(5) -0.122(8) 0.055(7) O7 0.082(5) 0.334(16) 0.235(12) -0.138(11) 0.002(6) -0.030(7) C18 0.083(6) 0.091(6) 0.127(8) -0.043(6) 0.008(5) -0.001(5) O8 0.065(6) 0.069(6) 0.083(8) -0.024(6) 0.004(5) -0.011(5) O8' 0.074(10) 0.074(9) 0.089(12) -0.033(9) 0.005(8) -0.017(8) _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 Cd O3 2.336(4) 2_466 ? Cd O3 2.336(4) . ? Cd N3 2.352(4) . ? Cd N3 2.352(4) 2_466 ? Cd N1 2.377(4) . ? Cd N1 2.377(4) 2_466 ? O1 C6 1.216(8) . ? O2 C14 1.211(7) . ? N1 C5 1.328(8) . ? N1 C1 1.328(7) . ? N2 C6 1.348(7) . ? N2 C2 1.406(7) . ? N2 H2A 0.8600 . ? N3 C13 1.331(7) . ? N3 C9 1.348(7) . ? N4 C14 1.342(8) . ? N4 C10 1.417(7) . ? N4 H4A 0.8600 . ? C1 C2 1.387(7) . ? C1 H1A 0.9300 . ? C2 C3 1.390(8) . ? C3 C4 1.375(9) . ? C3 H3A 0.9300 . ? C4 C5 1.375(9) . ? C4 H4B 0.9300 . ? C5 H5A 0.9300 . ? C6 C7 1.498(9) . ? C7 C8 1.503(11) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C8 1.396(17) 2_365 ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.391(8) . ? C9 H9A 0.9300 . ? C10 C11 1.369(8) . ? C11 C12 1.376(9) . ? C11 H11A 0.9300 . ? C12 C13 1.390(8) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.514(9) . ? C15 C16' 1.549(16) . ? C15 C16 1.58(2) . ? C16 C16' 0.96(2) . ? C16 C16' 1.175(17) 2_377 ? C16 C16 1.48(4) 2_377 ? C16' C16 1.175(17) 2_377 ? C16' C16' 1.55(3) 2_377 ? C17 O3 1.449(9) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? O3 H3C 0.9300 . ? Cl O5 1.359(7) . ? Cl O7 1.360(8) . ? Cl O6 1.383(7) . ? Cl O4 1.432(6) . ? C18 O8' 1.338(18) . ? C18 O8 1.414(14) . ? O8 O8' 0.839(15) . ? 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 O3 Cd O3 180.0 2_466 . ? O3 Cd N3 90.78(16) 2_466 . ? O3 Cd N3 89.22(16) . . ? O3 Cd N3 89.22(16) 2_466 2_466 ? O3 Cd N3 90.78(16) . 2_466 ? N3 Cd N3 180.000(1) . 2_466 ? O3 Cd N1 91.06(16) 2_466 . ? O3 Cd N1 88.94(16) . . ? N3 Cd N1 89.18(15) . . ? N3 Cd N1 90.82(15) 2_466 . ? O3 Cd N1 88.94(16) 2_466 2_466 ? O3 Cd N1 91.06(16) . 2_466 ? N3 Cd N1 90.82(15) . 2_466 ? N3 Cd N1 89.18(15) 2_466 2_466 ? N1 Cd N1 180.000(1) . 2_466 ? C5 N1 C1 118.2(5) . . ? C5 N1 Cd 118.4(4) . . ? C1 N1 Cd 123.4(4) . . ? C6 N2 C2 128.8(5) . . ? C6 N2 H2A 115.6 . . ? C2 N2 H2A 115.6 . . ? C13 N3 C9 117.8(5) . . ? C13 N3 Cd 120.5(4) . . ? C9 N3 Cd 121.6(4) . . ? C14 N4 C10 125.5(5) . . ? C14 N4 H4A 117.3 . . ? C10 N4 H4A 117.3 . . ? N1 C1 C2 123.6(5) . . ? N1 C1 H1A 118.2 . . ? C2 C1 H1A 118.2 . . ? C1 C2 C3 117.8(5) . . ? C1 C2 N2 118.5(5) . . ? C3 C2 N2 123.7(5) . . ? C4 C3 C2 118.0(5) . . ? C4 C3 H3A 121.0 . . ? C2 C3 H3A 121.0 . . ? C5 C4 C3 120.4(6) . . ? C5 C4 H4B 119.8 . . ? C3 C4 H4B 119.8 . . ? N1 C5 C4 121.9(6) . . ? N1 C5 H5A 119.0 . . ? C4 C5 H5A 119.0 . . ? O1 C6 N2 121.7(6) . . ? O1 C6 C7 122.1(5) . . ? N2 C6 C7 116.1(6) . . ? C6 C7 C8 113.0(5) . . ? C6 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? C6 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C8 C8 C7 119.9(12) 2_365 . ? C8 C8 H8A 107.3 2_365 . ? C7 C8 H8A 107.3 . . ? C8 C8 H8B 107.3 2_365 . ? C7 C8 H8B 107.3 . . ? H8A C8 H8B 106.9 . . ? N3 C9 C10 122.3(5) . . ? N3 C9 H9A 118.8 . . ? C10 C9 H9A 118.8 . . ? C11 C10 C9 119.3(5) . . ? C11 C10 N4 124.3(5) . . ? C9 C10 N4 116.4(5) . . ? C10 C11 C12 118.7(5) . . ? C10 C11 H11A 120.7 . . ? C12 C11 H11A 120.7 . . ? C11 C12 C13 119.2(5) . . ? C11 C12 H12A 120.4 . . ? C13 C12 H12A 120.4 . . ? N3 C13 C12 122.7(5) . . ? N3 C13 H13A 118.7 . . ? C12 C13 H13A 118.7 . . ? O2 C14 N4 122.1(6) . . ? O2 C14 C15 122.3(6) . . ? N4 C14 C15 115.5(6) . . ? C14 C15 C16' 111.5(7) . . ? C14 C15 C16 113.6(8) . . ? C16' C15 C16 35.6(7) . . ? C16' C16 C16' 93(2) . 2_377 ? C16' C16 C16 52.5(17) . 2_377 ? C16' C16 C16 40.3(11) 2_377 2_377 ? C16' C16 C15 70(2) . . ? C16' C16 C15 135.9(15) 2_377 . ? C16 C16 C15 111(2) 2_377 . ? C16 C16' C16 87(2) . 2_377 ? C16 C16' C15 74.0(18) . . ? C16 C16' C15 134.6(13) 2_377 . ? C16 C16' C16' 49.1(14) . 2_377 ? C16 C16' C16' 38.1(13) 2_377 2_377 ? C15 C16' C16' 111.2(14) . 2_377 ? O3 C17 H17A 109.5 . . ? O3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C17 O3 Cd 131.5(4) . . ? C17 O3 H3C 114.2 . . ? Cd O3 H3C 114.2 . . ? O5 Cl O7 110.0(8) . . ? O5 Cl O6 114.3(7) . . ? O7 Cl O6 105.1(7) . . ? O5 Cl O4 108.1(4) . . ? O7 Cl O4 108.0(6) . . ? O6 Cl O4 111.1(4) . . ? O8' C18 O8 35.4(7) . . ? O8' O8 C18 67.4(16) . . ? O8 O8' C18 77.3(16) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.852 _refine_diff_density_min -1.061 _refine_diff_density_rms 0.095 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 695632' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H48 Cd Cl2 N8 O14' _chemical_formula_weight 1000.12 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 Orthorhombic _symmetry_space_group_name_H-M Pcca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x, y, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x, -y, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 16.779(2) _cell_length_b 12.1263(13) _cell_length_c 21.766(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4428.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 5.10 _cell_measurement_theta_max 12.53 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.500 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2056 _exptl_absorpt_coefficient_mu 0.686 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9107 _exptl_absorpt_correction_T_max 0.9836 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4495 _diffrn_reflns_av_R_equivalents 0.0262 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3864 _reflns_number_gt 2735 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. ; _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^)+(0.0826P)^2^+7.9674P] 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 SHELXL _refine_ls_extinction_coef 0.0009(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3864 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0763 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1554 _refine_ls_wR_factor_gt 0.1381 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Cd Cd 0.2500 0.5000 0.34279(2) 0.03853(14) Uani 1 2 d S . . O1 O -0.1566(2) 0.7274(3) 0.3096(2) 0.0855(14) Uani 1 1 d . . . O2 O 0.0211(3) 0.0792(3) 0.16110(17) 0.0729(11) Uani 1 1 d . . . N1 N 0.1428(2) 0.6229(3) 0.34306(18) 0.0445(9) Uani 1 1 d . . . N2 N -0.0496(2) 0.8409(3) 0.3247(2) 0.0553(11) Uani 1 1 d . . . H2A H -0.0367 0.9093 0.3275 0.066 Uiso 1 1 calc R . . N3 N 0.1754(2) 0.4010(3) 0.26900(18) 0.0453(9) Uani 1 1 d . . . N4 N 0.0460(3) 0.2504(3) 0.1265(2) 0.0624(12) Uani 1 1 d . . . H4A H 0.0370 0.2943 0.0963 0.075 Uiso 1 1 calc R . . C1 C 0.1503(3) 0.7325(4) 0.3469(3) 0.0555(13) Uani 1 1 d . . . H1A H 0.2010 0.7611 0.3534 0.067 Uiso 1 1 calc R . . C2 C 0.0887(3) 0.8049(4) 0.3420(2) 0.0530(13) Uani 1 1 d . . . H2B H 0.0979 0.8802 0.3456 0.064 Uiso 1 1 calc R . . C3 C 0.0121(3) 0.7659(3) 0.3316(2) 0.0448(11) Uani 1 1 d . . . C4 C 0.0033(3) 0.6526(3) 0.3279(2) 0.0492(12) Uani 1 1 d . . . H4B H -0.0468 0.6217 0.3216 0.059 Uiso 1 1 calc R . . C5 C 0.0687(3) 0.5865(4) 0.3335(2) 0.0465(11) Uani 1 1 d . . . H5A H 0.0612 0.5107 0.3305 0.056 Uiso 1 1 calc R . . C6 C -0.1292(3) 0.8196(4) 0.3140(3) 0.0699(16) Uani 1 1 d . . . C7 C -0.1790(4) 0.9248(5) 0.3045(4) 0.097(2) Uani 1 1 d . . . H7A H -0.1439 0.9876 0.2991 0.117 Uiso 1 1 calc R . . H7B H -0.2114 0.9174 0.2678 0.117 Uiso 1 1 calc R . . C8 C -0.2293(6) 0.9424(7) 0.3568(5) 0.130(3) Uani 1 1 d . . . H8A H -0.1976 0.9353 0.3939 0.157 Uiso 1 1 calc R . . H8B H -0.2699 0.8855 0.3577 0.196 Uiso 1 1 calc R . . C9 C 0.1473(3) 0.2979(3) 0.2754(2) 0.0478(11) Uani 1 1 d . . . H9A H 0.1584 0.2609 0.3119 0.057 Uiso 1 1 calc R . . C10 C 0.1034(3) 0.2436(4) 0.2318(2) 0.0528(12) Uani 1 1 d . . . H10A H 0.0844 0.1728 0.2392 0.063 Uiso 1 1 calc R . . C11 C 0.0878(3) 0.2958(4) 0.1763(2) 0.0501(12) Uani 1 1 d . . . C12 C 0.1158(3) 0.4035(4) 0.1691(2) 0.0552(13) Uani 1 1 d . . . H12A H 0.1057 0.4423 0.1331 0.066 Uiso 1 1 calc R . . C13 C 0.1580(3) 0.4508(4) 0.2155(2) 0.0524(12) Uani 1 1 d . . . H13A H 0.1760 0.5226 0.2098 0.063 Uiso 1 1 calc R . . C14 C 0.0180(3) 0.1453(4) 0.1200(3) 0.0573(13) Uani 1 1 d . . . C15 C -0.0162(4) 0.1200(5) 0.0573(3) 0.0749(17) Uani 1 1 d . . . H15A H -0.0033 0.1798 0.0294 0.090 Uiso 1 1 calc R . . H15B H -0.0737 0.1151 0.0603 0.090 Uiso 1 1 calc R . . C16 C 0.0164(3) 0.0126(4) 0.0316(2) 0.0602(13) Uani 1 1 d . . . H16A H 0.0740 0.0171 0.0294 0.072 Uiso 1 1 calc R . . H16B H 0.0028 -0.0472 0.0592 0.072 Uiso 1 1 calc R . . O7 O 0.1881(3) 0.3969(3) 0.4221(2) 0.0835(13) Uani 1 1 d . . . C17 C 0.2375(12) 0.326(2) 0.4773(7) 0.264(10) Uani 1 1 d . . . C18 C 0.201(2) 0.292(3) 0.5257(13) 0.203(13) Uani 0.50 1 d P . . C18' C 0.250(2) 0.321(5) 0.5430(18) 0.30(3) Uani 0.50 1 d P . . Cl1 Cl 0.2500 0.0000 0.40928(15) 0.0981(9) Uani 1 2 d S . . O3 O 0.2056(4) 0.0743(5) 0.3723(4) 0.149(3) Uani 1 1 d . . . O4 O 0.1961(3) -0.0613(4) 0.4464(3) 0.129(2) Uani 1 1 d . . . Cl2 Cl 0.0064(4) 0.5164(10) 0.0067(3) 0.103(2) Uani 0.50 1 d P . . O5 O -0.0250(5) 0.4481(9) 0.0484(4) 0.193(4) Uani 1 1 d . . . O6 O 0.0616(10) 0.5723(18) 0.0409(6) 0.196(8) Uani 0.50 1 d P . . O6' O 0.0612(9) 0.4209(16) -0.0074(8) 0.197(7) Uani 0.50 1 d P . . 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 Cd 0.0294(2) 0.0289(2) 0.0574(3) 0.000 0.000 0.00516(17) O1 0.045(2) 0.048(2) 0.163(4) -0.015(2) -0.018(2) 0.0099(17) O2 0.104(3) 0.0399(17) 0.075(2) -0.0026(18) -0.028(2) -0.0119(19) N1 0.0334(18) 0.0313(17) 0.069(2) -0.0013(17) 0.0015(17) 0.0094(15) N2 0.043(2) 0.0316(18) 0.092(3) -0.0088(19) -0.012(2) 0.0140(17) N3 0.0407(19) 0.0298(17) 0.065(2) -0.0010(17) -0.0046(17) 0.0043(15) N4 0.084(3) 0.044(2) 0.060(3) 0.003(2) -0.022(2) -0.005(2) C1 0.038(2) 0.037(2) 0.092(4) -0.008(2) -0.004(2) 0.001(2) C2 0.041(2) 0.030(2) 0.088(4) -0.008(2) -0.003(2) 0.0041(19) C3 0.039(2) 0.035(2) 0.060(3) -0.007(2) -0.002(2) 0.0141(19) C4 0.032(2) 0.036(2) 0.080(3) -0.008(2) -0.004(2) 0.0033(19) C5 0.041(2) 0.028(2) 0.070(3) -0.002(2) 0.000(2) 0.0083(18) C6 0.045(3) 0.052(3) 0.113(5) -0.016(3) -0.015(3) 0.020(2) C7 0.057(3) 0.063(4) 0.171(7) -0.035(4) -0.004(4) 0.019(3) C8 0.139(7) 0.081(6) 0.172(9) 0.013(6) -0.002(7) 0.046(5) C9 0.050(3) 0.038(2) 0.056(3) 0.002(2) -0.006(2) 0.001(2) C10 0.059(3) 0.034(2) 0.065(3) -0.004(2) -0.005(2) -0.004(2) C11 0.047(3) 0.042(2) 0.061(3) -0.003(2) -0.010(2) 0.004(2) C12 0.059(3) 0.040(3) 0.066(3) 0.008(2) -0.012(2) -0.002(2) C13 0.047(3) 0.031(2) 0.080(4) 0.006(2) -0.006(2) -0.002(2) C14 0.064(3) 0.043(3) 0.065(3) -0.010(2) -0.018(3) 0.005(2) C15 0.097(4) 0.061(3) 0.067(3) -0.017(3) -0.026(3) 0.008(3) C16 0.067(3) 0.054(3) 0.060(3) -0.009(3) -0.008(3) -0.006(2) O7 0.089(3) 0.074(3) 0.087(3) 0.022(2) 0.030(2) 0.006(2) C17 0.32(2) 0.35(3) 0.124(10) 0.014(14) 0.076(13) 0.012(18) C18 0.22(3) 0.28(3) 0.116(17) 0.09(2) -0.02(2) -0.03(3) C18' 0.26(4) 0.46(7) 0.18(3) 0.03(4) -0.10(3) -0.17(4) Cl1 0.0714(14) 0.0579(12) 0.165(3) 0.000 0.000 -0.0172(12) O3 0.120(5) 0.092(4) 0.236(7) 0.035(5) -0.045(5) -0.004(4) O4 0.096(4) 0.086(3) 0.204(6) 0.019(4) 0.016(4) -0.018(3) Cl2 0.057(2) 0.197(6) 0.055(3) 0.036(3) 0.008(2) -0.007(3) O5 0.182(8) 0.264(10) 0.134(6) 0.039(7) -0.009(6) -0.008(8) O6 0.171(13) 0.31(2) 0.108(9) 0.024(12) -0.050(9) -0.075(15) O6' 0.143(11) 0.262(18) 0.187(15) 0.035(14) 0.027(10) 0.124(12) _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 Cd N1 2.336(3) 2_565 ? Cd N1 2.336(3) . ? Cd N3 2.364(4) . ? Cd N3 2.364(4) 2_565 ? Cd O7 2.372(4) 2_565 ? Cd O7 2.372(4) . ? O1 C6 1.213(6) . ? O2 C14 1.202(6) . ? N1 C5 1.335(6) . ? N1 C1 1.338(6) . ? N2 C6 1.380(6) . ? N2 C3 1.386(5) . ? N3 C9 1.343(5) . ? N3 C13 1.345(6) . ? N4 C14 1.366(6) . ? N4 C11 1.403(6) . ? C1 C2 1.359(6) . ? C2 C3 1.387(6) . ? C3 C4 1.385(6) . ? C4 C5 1.364(6) . ? C6 C7 1.539(7) . ? C7 C8 1.433(12) . ? C8 C8 1.559(15) 2_475 ? C9 C10 1.370(6) . ? C10 C11 1.388(7) . ? C11 C12 1.397(7) . ? C12 C13 1.359(7) . ? C14 C15 1.511(7) . ? C15 C16 1.519(7) . ? C16 C16 1.512(10) 5 ? O7 C17 1.69(2) . ? C17 C18 1.29(3) . ? C17 C18' 1.45(4) . ? C18 C18' 0.97(4) . ? Cl1 O3 1.420(6) . ? Cl1 O3 1.420(6) 2 ? Cl1 O4 1.422(6) 2 ? Cl1 O4 1.422(6) . ? Cl2 Cl2 0.537(18) 5_565 ? Cl2 O5 1.311(12) 5_565 ? Cl2 O5 1.337(13) . ? Cl2 O6' 1.366(16) 5_565 ? Cl2 O6 1.368(17) . ? Cl2 O6' 1.510(18) . ? Cl2 O6 1.879(17) 5_565 ? O5 Cl2 1.311(12) 5_565 ? O6 Cl2 1.879(17) 5_565 ? O6' Cl2 1.366(16) 5_565 ? 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 N1 Cd N1 179.71(19) 2_565 . ? N1 Cd N3 94.90(12) 2_565 . ? N1 Cd N3 85.29(12) . . ? N1 Cd N3 85.29(12) 2_565 2_565 ? N1 Cd N3 94.90(12) . 2_565 ? N3 Cd N3 94.41(18) . 2_565 ? N1 Cd O7 89.85(14) 2_565 2_565 ? N1 Cd O7 89.94(14) . 2_565 ? N3 Cd O7 173.94(15) . 2_565 ? N3 Cd O7 89.72(15) 2_565 2_565 ? N1 Cd O7 89.94(14) 2_565 . ? N1 Cd O7 89.85(14) . . ? N3 Cd O7 89.72(15) . . ? N3 Cd O7 173.94(15) 2_565 . ? O7 Cd O7 86.5(2) 2_565 . ? C5 N1 C1 115.2(4) . . ? C5 N1 Cd 120.3(3) . . ? C1 N1 Cd 124.2(3) . . ? C6 N2 C3 128.3(4) . . ? C9 N3 C13 115.6(4) . . ? C9 N3 Cd 126.0(3) . . ? C13 N3 Cd 118.4(3) . . ? C14 N4 C11 128.3(4) . . ? N1 C1 C2 124.4(4) . . ? C1 C2 C3 119.8(4) . . ? C4 C3 N2 124.4(4) . . ? C4 C3 C2 116.5(4) . . ? N2 C3 C2 119.1(4) . . ? C5 C4 C3 119.5(4) . . ? N1 C5 C4 124.6(4) . . ? O1 C6 N2 123.5(4) . . ? O1 C6 C7 123.2(5) . . ? N2 C6 C7 113.2(5) . . ? C8 C7 C6 109.7(7) . . ? C7 C8 C8 113.3(6) . 2_475 ? N3 C9 C10 124.3(4) . . ? C9 C10 C11 119.0(4) . . ? C10 C11 C12 117.5(4) . . ? C10 C11 N4 125.9(4) . . ? C12 C11 N4 116.6(4) . . ? C13 C12 C11 119.1(5) . . ? N3 C13 C12 124.5(4) . . ? O2 C14 N4 121.9(5) . . ? O2 C14 C15 123.6(5) . . ? N4 C14 C15 114.5(5) . . ? C14 C15 C16 111.8(5) . . ? C16 C16 C15 112.2(6) 5 . ? C17 O7 Cd 124.7(7) . . ? C18 C17 C18' 41.0(18) . . ? C18 C17 O7 121(2) . . ? C18' C17 O7 143(3) . . ? C18' C18 C17 78(4) . . ? C18 C18' C17 61(3) . . ? O3 Cl1 O3 110.9(7) . 2 ? O3 Cl1 O4 108.9(4) . 2 ? O3 Cl1 O4 108.6(4) 2 2 ? O3 Cl1 O4 108.6(4) . . ? O3 Cl1 O4 108.9(4) 2 . ? O4 Cl1 O4 110.8(6) 2 . ? Cl2 Cl2 O5 80.9(17) 5_565 5_565 ? Cl2 Cl2 O5 76(2) 5_565 . ? O5 Cl2 O5 156.6(8) 5_565 . ? Cl2 Cl2 O6' 95(2) 5_565 5_565 ? O5 Cl2 O6' 91.5(10) 5_565 5_565 ? O5 Cl2 O6' 90.5(9) . 5_565 ? Cl2 Cl2 O6 159(3) 5_565 . ? O5 Cl2 O6 100.0(9) 5_565 . ? O5 Cl2 O6 101.8(9) . . ? O6' Cl2 O6 106.2(14) 5_565 . ? Cl2 Cl2 O6' 64(2) 5_565 . ? O5 Cl2 O6' 85.5(9) 5_565 . ? O5 Cl2 O6' 84.4(10) . . ? O6' Cl2 O6' 159.2(7) 5_565 . ? O6 Cl2 O6' 94.5(12) . . ? Cl2 Cl2 O6 15.3(19) 5_565 5_565 ? O5 Cl2 O6 80.1(7) 5_565 5_565 ? O5 Cl2 O6 77.3(7) . 5_565 ? O6' Cl2 O6 79.7(10) 5_565 5_565 ? O6 Cl2 O6 174.1(8) . 5_565 ? O6' Cl2 O6 79.6(10) . 5_565 ? Cl2 O5 Cl2 23.4(8) 5_565 . ? Cl2 O6 Cl2 5.9(8) . 5_565 ? Cl2 O6' Cl2 20.8(7) 5_565 . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.874 _refine_diff_density_min -0.883 _refine_diff_density_rms 0.092 #===END