# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Myoung Soo Lah' _publ_contact_author_address ; Chemistry and Applied Chemistry Hanyang University 1271 Sa-1-dong Ansan Kyunggi-do 426-791 SOUTH KOREA ; _publ_contact_author_email MSLAH@HANYANG.AC.KR _publ_section_title ; Selective Gas Sorption Property of an Interdigitated 3-D Metal-Organic Framework with 1-D Channels ; loop_ _publ_author_name 'Myoung Soo Lah' 'Hyungphil Chun' 'Seunghee Hong' 'Mira Park' 'Yang Zou' # Attachment 'mslah.cif' data_ligand _database_code_depnum_ccdc_archive 'CCDC 656711' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H7 N5' _chemical_formula_sum 'C7 H7 N5' _chemical_formula_weight 161.18 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' _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 8.214(3) _cell_length_b 5.6315(17) _cell_length_c 15.202(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.539(5) _cell_angle_gamma 90.00 _cell_volume 703.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 2605 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 28.01 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 336 _exptl_absorpt_coefficient_mu 0.104 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9846 _exptl_absorpt_correction_T_max 0.9948 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4149 _diffrn_reflns_av_R_equivalents 0.0842 _diffrn_reflns_av_sigmaI/netI 0.0671 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 28.11 _reflns_number_total 1662 _reflns_number_gt 1449 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics ORTEP3 _computing_publication_material WinGX _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^)+(0.0414P)^2^+1.1404P] 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 1662 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0961 _refine_ls_R_factor_gt 0.0838 _refine_ls_wR_factor_ref 0.1976 _refine_ls_wR_factor_gt 0.1922 _refine_ls_goodness_of_fit_ref 1.295 _refine_ls_restrained_S_all 1.295 _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 N1 N 0.6374(3) 1.1501(5) 0.48722(17) 0.0271(6) Uani 1 1 d . . . H1N H 0.552(8) 1.049(14) 0.500(5) 0.032 Uiso 0.50 1 d P . . N2 N 0.6161(3) 1.3230(5) 0.42651(17) 0.0298(7) Uani 1 1 d . . . N3 N 0.7425(3) 1.4556(5) 0.42636(16) 0.0254(6) Uani 1 1 d . . . N4 N 0.8499(3) 1.3728(5) 0.48735(15) 0.0226(6) Uani 1 1 d . . . H4N H 0.944(7) 1.453(13) 0.499(5) 0.027 Uiso 0.50 1 d P . . N5 N 1.0425(3) 0.6453(6) 0.80321(19) 0.0303(7) Uani 1 1 d . . . H51N H 0.997(5) 0.504(8) 0.816(3) 0.036 Uiso 1 1 d . . . H52N H 1.118(5) 0.716(7) 0.834(3) 0.036 Uiso 1 1 d . . . C1 C 0.7827(3) 1.1844(5) 0.52466(18) 0.0205(6) Uani 1 1 d . . . C2 C 0.8527(3) 1.0409(6) 0.59541(18) 0.0211(6) Uani 1 1 d . . . C3 C 0.7833(3) 0.8249(5) 0.61799(19) 0.0208(6) Uani 1 1 d . . . H3 H 0.689(4) 0.755(6) 0.587(2) 0.025 Uiso 1 1 d . . . C4 C 0.8456(3) 0.6928(6) 0.6865(2) 0.0232(7) Uani 1 1 d . . . H4 H 0.799(4) 0.539(7) 0.701(2) 0.028 Uiso 1 1 d . . . C5 C 0.9796(3) 0.7743(6) 0.73488(18) 0.0215(6) Uani 1 1 d . . . C6 C 1.0498(3) 0.9897(6) 0.71168(19) 0.0240(7) Uani 1 1 d . . . H6 H 1.143(4) 1.051(6) 0.745(2) 0.029 Uiso 1 1 d . . . C7 C 0.9874(3) 1.1217(6) 0.64296(19) 0.0219(6) Uani 1 1 d . . . H7 H 1.031(4) 1.284(7) 0.631(2) 0.026 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 N1 0.0250(13) 0.0353(15) 0.0208(12) 0.0070(12) -0.0046(9) -0.0069(11) N2 0.0287(13) 0.0385(16) 0.0220(13) 0.0076(12) -0.0080(10) -0.0065(12) N3 0.0241(12) 0.0305(15) 0.0214(12) 0.0054(11) -0.0051(9) -0.0043(10) N4 0.0221(12) 0.0288(14) 0.0169(11) 0.0029(11) -0.0035(9) -0.0017(10) N5 0.0301(14) 0.0314(16) 0.0293(14) 0.0117(13) -0.0084(11) -0.0034(12) C1 0.0206(13) 0.0239(15) 0.0169(13) -0.0004(12) 0.0009(10) -0.0003(11) C2 0.0199(13) 0.0294(16) 0.0141(12) -0.0009(12) 0.0008(10) 0.0023(11) C3 0.0197(13) 0.0225(15) 0.0201(13) -0.0012(12) -0.0005(10) -0.0008(11) C4 0.0217(14) 0.0231(16) 0.0249(15) 0.0013(13) 0.0005(11) -0.0002(11) C5 0.0214(13) 0.0239(15) 0.0194(14) 0.0011(12) 0.0001(10) 0.0034(11) C6 0.0214(13) 0.0308(17) 0.0198(14) -0.0016(13) -0.0045(11) -0.0012(12) C7 0.0227(14) 0.0218(15) 0.0212(14) 0.0002(12) -0.0007(11) -0.0032(11) _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 N1 C1 1.332(4) . ? N1 N2 1.352(4) . ? N2 N3 1.279(4) . ? N3 N4 1.356(3) . ? N4 C1 1.326(4) . ? N5 C5 1.365(4) . ? C1 C2 1.459(4) . ? C2 C3 1.388(4) . ? C2 C7 1.393(4) . ? C3 C4 1.375(4) . ? C4 C5 1.395(4) . ? C5 C6 1.390(4) . ? C6 C7 1.377(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 C1 N1 N2 107.3(2) . . ? N3 N2 N1 108.8(2) . . ? N2 N3 N4 108.7(2) . . ? C1 N4 N3 107.3(2) . . ? N4 C1 N1 107.9(3) . . ? N4 C1 C2 126.6(3) . . ? N1 C1 C2 125.5(3) . . ? C3 C2 C7 119.0(3) . . ? C3 C2 C1 120.5(3) . . ? C7 C2 C1 120.5(3) . . ? C4 C3 C2 120.7(3) . . ? C3 C4 C5 120.5(3) . . ? N5 C5 C6 120.2(3) . . ? N5 C5 C4 121.1(3) . . ? C6 C5 C4 118.7(3) . . ? C7 C6 C5 120.8(3) . . ? C6 C7 C2 120.3(3) . . ? 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 N1 H1N N1 0.93(6) 1.93(6) 2.850(5) 173(7) 3_676 N4 H4N N4 0.91(6) 1.97(6) 2.875(5) 175(7) 3_786 N5 H51N N2 0.90(4) 2.67(4) 3.288(4) 126(3) 4_676 N5 H52N N3 0.87(4) 2.53(4) 3.346(4) 156(3) 4_686 _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 28.11 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.321 _refine_diff_density_min -0.283 _refine_diff_density_rms 0.073 #===END data_MOF-1 _database_code_depnum_ccdc_archive 'CCDC 656712' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H39 Cd3 N21 O6' _chemical_formula_sum 'C31 H39 Cd3 N21 O6' _chemical_formula_weight 1139.03 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' Cd Cd -0.8075 1.2024 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.0163(6) _cell_length_b 12.0948(11) _cell_length_c 12.7661(13) _cell_angle_alpha 90.833(2) _cell_angle_beta 105.9450(10) _cell_angle_gamma 97.704(2) _cell_volume 1030.76(17) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5349 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 23.24 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.835 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 564 _exptl_absorpt_coefficient_mu 1.603 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5011 _exptl_absorpt_correction_T_max 0.8309 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5460 _diffrn_reflns_av_R_equivalents 0.0107 _diffrn_reflns_av_sigmaI/netI 0.0182 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3573 _reflns_number_gt 3394 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics ORTEP3 _computing_publication_material WinGX _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^)+(0.0302P)^2^+1.7171P] 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 3573 _refine_ls_number_parameters 291 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0242 _refine_ls_R_factor_gt 0.0231 _refine_ls_wR_factor_ref 0.0599 _refine_ls_wR_factor_gt 0.0592 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.087 _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 Cd1 Cd 0.0000 0.0000 0.0000 0.01334(8) Uani 1 2 d S . . Cd2 Cd 0.50421(3) -0.120118(15) 0.065284(15) 0.01429(8) Uani 1 1 d . . . O1 O 0.3403(3) 0.03055(16) 0.05127(16) 0.0146(4) Uani 1 1 d . . . H1O H 0.382(5) 0.060(3) 0.107(3) 0.022 Uiso 1 1 d . . . O2 O 0.5993(3) -0.29475(18) 0.02567(18) 0.0218(4) Uani 1 1 d . . . H21O H 0.669(6) -0.289(3) -0.017(3) 0.033 Uiso 1 1 d . . . H22O H 0.497(6) -0.327(3) -0.004(3) 0.033 Uiso 1 1 d . . . N1 N -0.1184(3) -0.27341(19) -0.09594(19) 0.0175(5) Uani 1 1 d . . . N2 N 0.0251(3) -0.18636(19) -0.05514(19) 0.0167(5) Uani 1 1 d . . . N3 N 0.2008(3) -0.21586(19) -0.04855(19) 0.0170(5) Uani 1 1 d . . . N4 N 0.1788(3) -0.32350(19) -0.08486(19) 0.0178(5) Uani 1 1 d . . . N5 N -0.4087(4) -0.8028(2) -0.2186(2) 0.0170(5) Uani 1 1 d . . . H51N H -0.522(6) -0.810(3) -0.262(3) 0.025 Uiso 1 1 d . . . H52N H -0.336(5) -0.850(3) -0.234(3) 0.025 Uiso 1 1 d . . . N6 N -0.1309(3) 0.0527(2) -0.26845(19) 0.0190(5) Uani 1 1 d . . . N7 N 0.0181(3) 0.0462(2) -0.17802(19) 0.0175(5) Uani 1 1 d . . . N8 N 0.1908(3) 0.0825(2) -0.19730(19) 0.0200(5) Uani 1 1 d . . . N9 N 0.1597(4) 0.1148(2) -0.29980(19) 0.0218(5) Uani 1 1 d . . . N10 N -0.4613(4) 0.2005(2) -0.7675(2) 0.0247(6) Uani 1 1 d . . . H101 H -0.580(6) 0.224(3) -0.771(3) 0.037 Uiso 1 1 d . . . H102 H -0.389(6) 0.240(3) -0.801(3) 0.037 Uiso 1 1 d . . . C1 C -0.0199(4) -0.3564(2) -0.1129(2) 0.0163(6) Uani 1 1 d . . . C2 C -0.1186(4) -0.4711(2) -0.1503(2) 0.0172(6) Uani 1 1 d . . . C3 C -0.3272(4) -0.4945(2) -0.1869(2) 0.0215(6) Uani 1 1 d . . . H3 H -0.4049 -0.4350 -0.1939 0.026 Uiso 1 1 calc R . . C4 C -0.4217(4) -0.6031(2) -0.2130(2) 0.0209(6) Uani 1 1 d . . . H4 H -0.5637 -0.6178 -0.2379 0.025 Uiso 1 1 calc R . . C5 C -0.3099(4) -0.6910(2) -0.2030(2) 0.0164(5) Uani 1 1 d . . . C6 C -0.1008(4) -0.6681(2) -0.1702(2) 0.0176(6) Uani 1 1 d . . . H6 H -0.0231 -0.7273 -0.1660 0.021 Uiso 1 1 calc R . . C7 C -0.0068(4) -0.5586(2) -0.1438(2) 0.0183(6) Uani 1 1 d . . . H7 H 0.1353 -0.5434 -0.1211 0.022 Uiso 1 1 calc R . . C8 C -0.0395(4) 0.0959(2) -0.3416(2) 0.0187(6) Uani 1 1 d . . . C9 C -0.1470(4) 0.1220(2) -0.4524(2) 0.0213(6) Uani 1 1 d . . . C10 C -0.3541(4) 0.1210(3) -0.4820(2) 0.0268(7) Uani 1 1 d . . . H10 H -0.4260 0.1018 -0.4302 0.032 Uiso 1 1 calc R . . C11 C -0.4558(5) 0.1474(3) -0.5848(3) 0.0284(7) Uani 1 1 d . . . H11 H -0.5969 0.1456 -0.6031 0.034 Uiso 1 1 calc R . . C12 C -0.3550(4) 0.1764(2) -0.6621(2) 0.0220(6) Uani 1 1 d . . . C13 C -0.1482(5) 0.1763(3) -0.6341(3) 0.0290(7) Uani 1 1 d . . . H13 H -0.0770 0.1945 -0.6864 0.035 Uiso 1 1 calc R . . C14 C -0.0460(5) 0.1498(3) -0.5304(3) 0.0286(7) Uani 1 1 d . . . H14 H 0.0949 0.1505 -0.5123 0.034 Uiso 1 1 calc R . . O1D O -0.219(2) -0.5450(12) -0.6770(11) 0.159(5) Uiso 0.50 1 d PD . . N1D N 0.0000 -0.5000 -0.5000 0.203(6) Uiso 1 2 d SD . . C1D C -0.064(3) -0.5072(13) -0.6118(11) 0.123(6) Uiso 0.50 1 d PD . . C2D C -0.180(4) -0.538(3) -0.459(2) 0.233(14) Uiso 0.50 1 d PD . . C3D C 0.217(3) -0.475(5) -0.458(4) 0.400 Uiso 0.50 1 d PD . . O1W O -0.625(8) -0.594(4) -0.550(4) 0.53(3) Uiso 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 Cd1 0.01069(14) 0.01267(14) 0.01632(15) 0.00116(10) 0.00328(10) 0.00146(10) Cd2 0.01094(11) 0.01369(12) 0.01704(12) 0.00186(8) 0.00228(8) 0.00082(7) O1 0.0127(9) 0.0150(9) 0.0146(10) 0.0004(7) 0.0018(8) 0.0006(7) O2 0.0165(10) 0.0216(11) 0.0290(12) 0.0010(9) 0.0087(9) 0.0035(8) N1 0.0143(11) 0.0138(11) 0.0226(13) -0.0006(9) 0.0033(9) -0.0003(9) N2 0.0128(11) 0.0153(12) 0.0206(12) 0.0006(9) 0.0032(9) 0.0002(9) N3 0.0146(11) 0.0139(11) 0.0218(12) -0.0006(9) 0.0042(9) 0.0015(9) N4 0.0156(11) 0.0150(12) 0.0216(12) -0.0016(9) 0.0041(10) 0.0009(9) N5 0.0137(12) 0.0160(12) 0.0192(13) -0.0006(9) 0.0027(10) -0.0006(10) N6 0.0146(11) 0.0222(12) 0.0176(12) -0.0005(10) 0.0006(9) 0.0017(9) N7 0.0143(11) 0.0190(12) 0.0173(12) 0.0003(9) 0.0022(9) 0.0006(9) N8 0.0151(12) 0.0241(13) 0.0188(12) 0.0029(10) 0.0024(10) 0.0001(10) N9 0.0178(12) 0.0286(13) 0.0168(12) 0.0042(10) 0.0026(10) 0.0003(10) N10 0.0223(14) 0.0319(15) 0.0195(13) 0.0046(11) 0.0032(11) 0.0079(11) C1 0.0160(13) 0.0157(14) 0.0172(14) 0.0010(11) 0.0050(11) 0.0011(11) C2 0.0173(13) 0.0158(14) 0.0167(14) -0.0008(11) 0.0033(11) -0.0007(11) C3 0.0181(14) 0.0155(14) 0.0293(16) 0.0008(12) 0.0036(12) 0.0034(11) C4 0.0130(13) 0.0207(15) 0.0258(16) 0.0002(12) 0.0018(11) -0.0014(11) C5 0.0184(13) 0.0161(13) 0.0136(13) -0.0005(10) 0.0040(11) -0.0009(11) C6 0.0167(13) 0.0162(14) 0.0207(14) 0.0013(11) 0.0055(11) 0.0042(11) C7 0.0152(13) 0.0181(14) 0.0210(14) -0.0009(11) 0.0052(11) -0.0001(11) C8 0.0172(14) 0.0194(14) 0.0177(14) -0.0006(11) 0.0025(11) 0.0017(11) C9 0.0181(14) 0.0234(15) 0.0200(15) 0.0003(12) 0.0012(11) 0.0030(11) C10 0.0201(15) 0.0417(19) 0.0183(15) 0.0030(13) 0.0049(12) 0.0040(13) C11 0.0169(14) 0.0430(19) 0.0234(16) -0.0001(14) 0.0022(12) 0.0048(13) C12 0.0237(15) 0.0217(15) 0.0177(14) -0.0017(11) 0.0006(12) 0.0041(12) C13 0.0228(16) 0.044(2) 0.0217(16) 0.0056(14) 0.0074(13) 0.0063(14) C14 0.0175(15) 0.046(2) 0.0224(16) 0.0060(14) 0.0037(12) 0.0065(13) _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 2.2725(18) 2 ? Cd1 O1 2.2725(18) . ? Cd1 N7 2.381(2) . ? Cd1 N7 2.381(2) 2 ? Cd1 N2 2.395(2) 2 ? Cd1 N2 2.395(2) . ? Cd2 O1 2.2657(19) . ? Cd2 O1 2.2802(19) 2_655 ? Cd2 N8 2.315(2) 2_655 ? Cd2 N3 2.361(2) . ? Cd2 O2 2.386(2) . ? Cd2 N5 2.399(2) 2_545 ? Cd2 Cd2 3.3700(4) 2_655 ? O1 Cd2 2.2802(19) 2_655 ? N1 C1 1.339(4) . ? N1 N2 1.343(3) . ? N2 N3 1.310(3) . ? N3 N4 1.350(3) . ? N4 C1 1.343(4) . ? N5 C5 1.420(4) . ? N5 Cd2 2.399(2) 2_545 ? N6 N7 1.339(3) . ? N6 C8 1.345(4) . ? N7 N8 1.321(3) . ? N8 N9 1.339(3) . ? N8 Cd2 2.315(2) 2_655 ? N9 C8 1.338(4) . ? N10 C12 1.404(4) . ? C1 C2 1.475(4) . ? C2 C7 1.389(4) . ? C2 C3 1.396(4) . ? C3 C4 1.382(4) . ? C4 C5 1.391(4) . ? C5 C6 1.398(4) . ? C6 C7 1.391(4) . ? C8 C9 1.470(4) . ? C9 C14 1.393(4) . ? C9 C10 1.395(4) . ? C10 C11 1.376(4) . ? C11 C12 1.387(4) . ? C12 C13 1.396(4) . ? C13 C14 1.386(4) . ? O1D C1D 1.201(14) . ? O1D C3D 1.73(5) 2_544 ? N1D C1D 1.371(13) . ? N1D C1D 1.371(13) 2_544 ? N1D C3D 1.460(18) . ? N1D C3D 1.460(18) 2_544 ? N1D C2D 1.511(17) 2_544 ? N1D C2D 1.511(17) . ? C1D C3D 1.57(4) 2_544 ? C1D C2D 1.71(3) 2_544 ? C2D C3D 1.04(5) 2_544 ? C2D C1D 1.71(3) 2_544 ? C3D C2D 1.04(5) 2_544 ? C3D C1D 1.57(4) 2_544 ? C3D O1D 1.73(5) 2_544 ? 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 180.0 2 . ? O1 Cd1 N7 93.31(7) 2 . ? O1 Cd1 N7 86.69(7) . . ? O1 Cd1 N7 86.69(7) 2 2 ? O1 Cd1 N7 93.31(7) . 2 ? N7 Cd1 N7 180.00(11) . 2 ? O1 Cd1 N2 86.90(7) 2 2 ? O1 Cd1 N2 93.10(7) . 2 ? N7 Cd1 N2 94.57(8) . 2 ? N7 Cd1 N2 85.43(8) 2 2 ? O1 Cd1 N2 93.10(7) 2 . ? O1 Cd1 N2 86.90(7) . . ? N7 Cd1 N2 85.43(8) . . ? N7 Cd1 N2 94.57(8) 2 . ? N2 Cd1 N2 180.00(14) 2 . ? O1 Cd2 O1 84.31(7) . 2_655 ? O1 Cd2 N8 109.97(8) . 2_655 ? O1 Cd2 N8 86.80(8) 2_655 2_655 ? O1 Cd2 N3 85.60(7) . . ? O1 Cd2 N3 104.77(8) 2_655 . ? N8 Cd2 N3 161.72(8) 2_655 . ? O1 Cd2 O2 161.71(8) . . ? O1 Cd2 O2 92.20(7) 2_655 . ? N8 Cd2 O2 87.68(8) 2_655 . ? N3 Cd2 O2 77.92(8) . . ? O1 Cd2 N5 97.68(8) . 2_545 ? O1 Cd2 N5 167.04(8) 2_655 2_545 ? N8 Cd2 N5 80.48(9) 2_655 2_545 ? N3 Cd2 N5 88.16(8) . 2_545 ? O2 Cd2 N5 89.74(8) . 2_545 ? O1 Cd2 Cd2 42.32(5) . 2_655 ? O1 Cd2 Cd2 41.99(5) 2_655 2_655 ? N8 Cd2 Cd2 101.06(6) 2_655 2_655 ? N3 Cd2 Cd2 96.94(6) . 2_655 ? O2 Cd2 Cd2 131.63(6) . 2_655 ? N5 Cd2 Cd2 138.53(6) 2_545 2_655 ? Cd2 O1 Cd1 117.89(8) . . ? Cd2 O1 Cd2 95.69(7) . 2_655 ? Cd1 O1 Cd2 117.69(8) . 2_655 ? C1 N1 N2 105.0(2) . . ? N3 N2 N1 109.4(2) . . ? N3 N2 Cd1 120.16(17) . . ? N1 N2 Cd1 130.42(17) . . ? N2 N3 N4 109.9(2) . . ? N2 N3 Cd2 123.54(17) . . ? N4 N3 Cd2 123.22(17) . . ? C1 N4 N3 104.2(2) . . ? C5 N5 Cd2 116.13(17) . 2_545 ? N7 N6 C8 104.8(2) . . ? N8 N7 N6 109.1(2) . . ? N8 N7 Cd1 121.46(17) . . ? N6 N7 Cd1 129.11(18) . . ? N7 N8 N9 110.1(2) . . ? N7 N8 Cd2 124.95(18) . 2_655 ? N9 N8 Cd2 123.79(17) . 2_655 ? C8 N9 N8 104.4(2) . . ? N1 C1 N4 111.5(2) . . ? N1 C1 C2 123.5(2) . . ? N4 C1 C2 124.8(2) . . ? C7 C2 C3 119.0(3) . . ? C7 C2 C1 120.7(2) . . ? C3 C2 C1 120.3(3) . . ? C4 C3 C2 120.7(3) . . ? C3 C4 C5 120.3(3) . . ? C4 C5 C6 119.4(3) . . ? C4 C5 N5 119.7(3) . . ? C6 C5 N5 120.7(3) . . ? C7 C6 C5 119.9(3) . . ? C2 C7 C6 120.7(3) . . ? N9 C8 N6 111.6(2) . . ? N9 C8 C9 124.6(3) . . ? N6 C8 C9 123.7(2) . . ? C14 C9 C10 118.1(3) . . ? C14 C9 C8 121.3(3) . . ? C10 C9 C8 120.6(3) . . ? C11 C10 C9 121.1(3) . . ? C10 C11 C12 120.8(3) . . ? C11 C12 C13 118.6(3) . . ? C11 C12 N10 120.2(3) . . ? C13 C12 N10 121.1(3) . . ? C14 C13 C12 120.5(3) . . ? C13 C14 C9 120.9(3) . . ? C1D O1D C3D 61.7(12) . 2_544 ? C1D N1D C1D 180.000(5) . 2_544 ? C1D N1D C3D 113(2) . . ? C1D N1D C3D 67(2) 2_544 . ? C1D N1D C3D 67(2) . 2_544 ? C1D N1D C3D 113(2) 2_544 2_544 ? C3D N1D C3D 180.000(5) . 2_544 ? C1D N1D C2D 72.4(12) . 2_544 ? C1D N1D C2D 107.6(12) 2_544 2_544 ? C3D N1D C2D 41(2) . 2_544 ? C3D N1D C2D 139(2) 2_544 2_544 ? C1D N1D C2D 107.6(12) . . ? C1D N1D C2D 72.4(12) 2_544 . ? C3D N1D C2D 139(2) . . ? C3D N1D C2D 41(2) 2_544 . ? C2D N1D C2D 180.000(5) 2_544 . ? O1D C1D N1D 133.6(16) . . ? O1D C1D C3D 75.9(19) . 2_544 ? N1D C1D C3D 59.0(13) . 2_544 ? O1D C1D C2D 167.2(18) . 2_544 ? N1D C1D C2D 57.6(9) . 2_544 ? C3D C1D C2D 116.2(17) 2_544 2_544 ? C3D C2D N1D 66.9(17) 2_544 . ? C3D C2D C1D 116(2) 2_544 2_544 ? N1D C2D C1D 50.0(8) . 2_544 ? C2D C3D N1D 72.2(17) 2_544 . ? C2D C3D C1D 125(2) 2_544 2_544 ? N1D C3D C1D 53.6(11) . 2_544 ? C2D C3D O1D 157(5) 2_544 2_544 ? N1D C3D O1D 95(2) . 2_544 ? C1D C3D O1D 42.3(15) 2_544 2_544 ? 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 N10 H101 N1 0.91(4) 2.47(4) 3.230(3) 141(3) 2_454 N10 H102 N4 0.85(4) 2.48(4) 3.322(4) 170(4) 2_554 N5 H52N N6 0.88(4) 2.10(4) 2.970(4) 173(3) 1_545 N5 H51N N9 0.83(4) 2.21(4) 2.945(3) 148(3) 1_445 O2 H22O N4 0.76(4) 2.20(4) 2.870(3) 148(4) . O2 H21O N1 0.82(4) 2.01(4) 2.822(3) 169(4) 1_655 O1 H1O N10 0.76(4) 2.26(4) 2.973(3) 158(4) 1_656 _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.788 _refine_diff_density_min -0.802 _refine_diff_density_rms 0.083 #===END data_MOF-1a _database_code_depnum_ccdc_archive 'CCDC 656713' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H30 Cd3 N20 O4' _chemical_formula_sum 'C28 H30 Cd3 N20 O4' _chemical_formula_weight 1047.92 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' 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 6.9889(8) _cell_length_b 12.0763(13) _cell_length_c 12.8137(14) _cell_angle_alpha 87.184(2) _cell_angle_beta 105.317(2) _cell_angle_gamma 97.988(2) _cell_volume 1032.9(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4619 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 28.33 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.685 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 514 _exptl_absorpt_coefficient_mu 1.588 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6223 _exptl_absorpt_correction_T_max 0.8323 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5306 _diffrn_reflns_av_R_equivalents 0.0133 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3562 _reflns_number_gt 3220 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics ORTEP3 _computing_publication_material WinGX _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^)+(0.0358P)^2^+0.9698P] 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 3562 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0293 _refine_ls_R_factor_gt 0.0251 _refine_ls_wR_factor_ref 0.0638 _refine_ls_wR_factor_gt 0.0618 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.002 _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 Cd1 Cd 1.0000 0.0000 1.0000 0.01307(9) Uani 1 2 d S . . Cd2 Cd 0.56178(3) 0.121975(17) 1.067268(16) 0.01394(8) Uani 1 1 d . . . O1 O 0.7094(3) -0.02876(17) 1.05050(17) 0.0149(4) Uani 1 1 d . . . H1O H 0.727(6) -0.057(3) 1.106(3) 0.022 Uiso 1 1 d . . . O2 O 0.4271(4) 0.29569(19) 1.02874(19) 0.0215(5) Uani 1 1 d . . . H21O H 0.312(6) 0.287(3) 0.988(3) 0.032 Uiso 1 1 d . . . H22O H 0.499(6) 0.334(3) 0.996(3) 0.032 Uiso 1 1 d . . . N1 N 1.0238(4) 0.2705(2) 0.9060(2) 0.0171(5) Uani 1 1 d . . . N2 N 0.9210(4) 0.1857(2) 0.9476(2) 0.0170(5) Uani 1 1 d . . . N3 N 0.7524(4) 0.2153(2) 0.9545(2) 0.0165(5) Uani 1 1 d . . . N4 N 0.7377(4) 0.3213(2) 0.9176(2) 0.0167(5) Uani 1 1 d . . . N5 N 1.1904(4) 0.7954(2) 0.7798(2) 0.0175(5) Uani 1 1 d . . . H51N H 1.245(6) 0.796(3) 0.729(3) 0.026 Uiso 1 1 d . . . H52N H 1.102(6) 0.842(3) 0.767(3) 0.026 Uiso 1 1 d . . . N6 N 0.8674(4) -0.0570(2) 0.7333(2) 0.0174(5) Uani 1 1 d . . . N7 N 0.8077(4) -0.0509(2) 0.8235(2) 0.0172(5) Uani 1 1 d . . . N8 N 0.6144(4) -0.0862(2) 0.8034(2) 0.0194(6) Uani 1 1 d . . . N9 N 0.5433(4) -0.1172(2) 0.7001(2) 0.0212(6) Uani 1 1 d . . . N10 N 0.6919(5) -0.1926(2) 0.2276(2) 0.0230(6) Uani 1 1 d . . . H101 H 0.791(6) -0.216(3) 0.219(3) 0.034 Uiso 1 1 d . . . H102 H 0.579(6) -0.236(3) 0.190(3) 0.034 Uiso 1 1 d . . . C1 C 0.9080(4) 0.3529(2) 0.8883(2) 0.0155(6) Uani 1 1 d . . . C2 C 0.9683(4) 0.4658(2) 0.8500(2) 0.0164(6) Uani 1 1 d . . . C3 C 1.1418(5) 0.4879(3) 0.8138(3) 0.0202(7) Uani 1 1 d . . . H3 H 1.2135 0.4283 0.8077 0.024 Uiso 1 1 calc R . . C4 C 1.2101(5) 0.5955(3) 0.7868(2) 0.0188(6) Uani 1 1 d . . . H4 H 1.3283 0.6092 0.7623 0.023 Uiso 1 1 calc R . . C5 C 1.1076(4) 0.6836(2) 0.7952(2) 0.0160(6) Uani 1 1 d . . . C6 C 0.9288(5) 0.6616(2) 0.8270(2) 0.0181(6) Uani 1 1 d . . . H6 H 0.8536 0.7207 0.8297 0.022 Uiso 1 1 calc R . . C7 C 0.8619(5) 0.5536(3) 0.8546(2) 0.0185(6) Uani 1 1 d . . . H7 H 0.7414 0.5394 0.8769 0.022 Uiso 1 1 calc R . . C8 C 0.7025(5) -0.0985(2) 0.6586(2) 0.0175(6) Uani 1 1 d . . . C9 C 0.6985(5) -0.1231(3) 0.5470(2) 0.0199(7) Uani 1 1 d . . . C10 C 0.8749(5) -0.1234(3) 0.5165(3) 0.0257(7) Uani 1 1 d . . . H10 H 0.9994 -0.1067 0.5687 0.031 Uiso 1 1 calc R . . C11 C 0.8731(5) -0.1475(3) 0.4122(3) 0.0258(7) Uani 1 1 d . . . H11 H 0.9958 -0.1474 0.3934 0.031 Uiso 1 1 calc R . . C12 C 0.6934(5) -0.1717(3) 0.3345(3) 0.0205(7) Uani 1 1 d . . . C13 C 0.5155(5) -0.1702(3) 0.3634(3) 0.0293(8) Uani 1 1 d . . . H13 H 0.3912 -0.1859 0.3108 0.035 Uiso 1 1 calc R . . C14 C 0.5181(5) -0.1460(3) 0.4684(3) 0.0267(8) Uani 1 1 d . . . H14 H 0.3955 -0.1450 0.4870 0.032 Uiso 1 1 calc R . . 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 0.01092(15) 0.01082(16) 0.01732(16) -0.00021(11) 0.00386(12) 0.00052(11) Cd2 0.01205(12) 0.01155(13) 0.01830(13) -0.00102(8) 0.00515(9) -0.00078(8) O1 0.0127(10) 0.0161(11) 0.0152(11) 0.0020(8) 0.0039(9) 0.0001(8) O2 0.0144(12) 0.0194(12) 0.0301(13) -0.0002(10) 0.0049(10) 0.0014(9) N1 0.0157(13) 0.0118(12) 0.0238(14) 0.0007(10) 0.0063(11) 0.0000(10) N2 0.0147(13) 0.0144(13) 0.0215(14) 0.0019(10) 0.0050(11) 0.0006(10) N3 0.0137(13) 0.0130(13) 0.0220(13) 0.0011(10) 0.0045(10) 0.0001(10) N4 0.0169(13) 0.0104(12) 0.0227(13) 0.0026(10) 0.0057(11) 0.0016(10) N5 0.0155(14) 0.0140(13) 0.0229(14) 0.0007(11) 0.0066(11) -0.0008(11) N6 0.0167(13) 0.0198(13) 0.0165(13) 0.0007(10) 0.0067(11) 0.0009(11) N7 0.0153(13) 0.0168(13) 0.0196(13) -0.0006(10) 0.0059(11) -0.0009(10) N8 0.0150(13) 0.0216(14) 0.0208(14) -0.0037(11) 0.0053(11) -0.0032(11) N9 0.0191(14) 0.0284(15) 0.0159(13) -0.0034(11) 0.0055(11) -0.0007(11) N10 0.0228(15) 0.0295(16) 0.0178(14) -0.0024(12) 0.0064(12) 0.0047(13) C1 0.0144(15) 0.0151(15) 0.0166(15) -0.0012(12) 0.0042(12) 0.0001(12) C2 0.0163(15) 0.0125(15) 0.0188(15) 0.0002(12) 0.0030(12) -0.0004(12) C3 0.0208(16) 0.0136(15) 0.0290(17) -0.0006(13) 0.0113(14) 0.0021(13) C4 0.0152(15) 0.0193(16) 0.0236(16) 0.0006(13) 0.0091(13) -0.0002(12) C5 0.0155(15) 0.0151(15) 0.0146(14) 0.0004(11) 0.0014(12) -0.0028(12) C6 0.0171(15) 0.0125(15) 0.0243(16) -0.0004(12) 0.0048(13) 0.0023(12) C7 0.0140(15) 0.0189(16) 0.0235(16) 0.0015(12) 0.0082(13) -0.0002(12) C8 0.0179(15) 0.0166(15) 0.0186(15) 0.0010(12) 0.0065(13) 0.0011(12) C9 0.0204(16) 0.0212(16) 0.0188(16) 0.0010(13) 0.0080(13) -0.0001(13) C10 0.0183(17) 0.036(2) 0.0203(17) -0.0009(14) 0.0023(13) 0.0003(14) C11 0.0184(17) 0.036(2) 0.0252(17) -0.0005(15) 0.0097(14) 0.0029(15) C12 0.0232(17) 0.0195(16) 0.0198(16) 0.0015(13) 0.0077(13) 0.0030(13) C13 0.0213(18) 0.041(2) 0.0228(17) -0.0047(15) 0.0020(14) 0.0014(16) C14 0.0184(17) 0.040(2) 0.0234(17) -0.0031(15) 0.0075(14) 0.0031(15) _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 2.267(2) 2_757 ? Cd1 O1 2.267(2) . ? Cd1 N7 2.367(3) 2_757 ? Cd1 N7 2.367(3) . ? Cd1 N2 2.405(3) 2_757 ? Cd1 N2 2.405(3) . ? Cd2 O1 2.259(2) . ? Cd2 O1 2.280(2) 2_657 ? Cd2 N8 2.304(3) 2_657 ? Cd2 N3 2.361(2) . ? Cd2 O2 2.394(2) . ? Cd2 N5 2.399(3) 2_767 ? Cd2 Cd2 3.3766(5) 2_657 ? O1 Cd2 2.280(2) 2_657 ? N1 N2 1.340(3) . ? N1 C1 1.342(4) . ? N2 N3 1.304(4) . ? N3 N4 1.351(3) . ? N4 C1 1.341(4) . ? N5 C5 1.419(4) . ? N5 Cd2 2.399(3) 2_767 ? N6 N7 1.337(4) . ? N6 C8 1.341(4) . ? N7 N8 1.319(4) . ? N8 N9 1.338(4) . ? N8 Cd2 2.304(3) 2_657 ? N9 C8 1.343(4) . ? N10 C12 1.402(4) . ? C1 C2 1.469(4) . ? C2 C7 1.389(4) . ? C2 C3 1.397(4) . ? C3 C4 1.381(4) . ? C4 C5 1.386(4) . ? C5 C6 1.401(4) . ? C6 C7 1.385(4) . ? C8 C9 1.468(4) . ? C9 C10 1.388(5) . ? C9 C14 1.393(5) . ? C10 C11 1.379(5) . ? C11 C12 1.385(5) . ? C12 C13 1.391(5) . ? C13 C14 1.385(5) . ? 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 180.0 2_757 . ? O1 Cd1 N7 87.05(8) 2_757 2_757 ? O1 Cd1 N7 92.95(8) . 2_757 ? O1 Cd1 N7 92.95(8) 2_757 . ? O1 Cd1 N7 87.05(8) . . ? N7 Cd1 N7 180.0 2_757 . ? O1 Cd1 N2 86.52(8) 2_757 2_757 ? O1 Cd1 N2 93.48(8) . 2_757 ? N7 Cd1 N2 85.38(9) 2_757 2_757 ? N7 Cd1 N2 94.62(9) . 2_757 ? O1 Cd1 N2 93.48(8) 2_757 . ? O1 Cd1 N2 86.52(8) . . ? N7 Cd1 N2 94.62(9) 2_757 . ? N7 Cd1 N2 85.38(9) . . ? N2 Cd1 N2 180.00(4) 2_757 . ? O1 Cd2 O1 83.86(8) . 2_657 ? O1 Cd2 N8 109.70(9) . 2_657 ? O1 Cd2 N8 86.81(8) 2_657 2_657 ? O1 Cd2 N3 85.76(8) . . ? O1 Cd2 N3 104.02(8) 2_657 . ? N8 Cd2 N3 162.23(9) 2_657 . ? O1 Cd2 O2 161.21(8) . . ? O1 Cd2 O2 91.87(8) 2_657 . ? N8 Cd2 O2 88.25(9) 2_657 . ? N3 Cd2 O2 77.51(9) . . ? O1 Cd2 N5 98.25(9) . 2_767 ? O1 Cd2 N5 167.50(8) 2_657 2_767 ? N8 Cd2 N5 80.87(9) 2_657 2_767 ? N3 Cd2 N5 88.45(9) . 2_767 ? O2 Cd2 N5 89.88(9) . 2_767 ? O1 Cd2 Cd2 42.18(5) . 2_657 ? O1 Cd2 Cd2 41.69(5) 2_657 2_657 ? N8 Cd2 Cd2 100.83(7) 2_657 2_657 ? N3 Cd2 Cd2 96.55(6) . 2_657 ? O2 Cd2 Cd2 130.94(6) . 2_657 ? N5 Cd2 Cd2 139.04(7) 2_767 2_657 ? Cd2 O1 Cd1 118.10(9) . . ? Cd2 O1 Cd2 96.14(8) . 2_657 ? Cd1 O1 Cd2 117.14(9) . 2_657 ? N2 N1 C1 105.0(2) . . ? N3 N2 N1 109.5(2) . . ? N3 N2 Cd1 120.48(18) . . ? N1 N2 Cd1 129.99(19) . . ? N2 N3 N4 110.1(2) . . ? N2 N3 Cd2 123.01(18) . . ? N4 N3 Cd2 123.90(19) . . ? C1 N4 N3 104.2(2) . . ? C5 N5 Cd2 115.55(19) . 2_767 ? N7 N6 C8 105.0(2) . . ? N8 N7 N6 109.3(2) . . ? N8 N7 Cd1 121.26(19) . . ? N6 N7 Cd1 129.28(19) . . ? N7 N8 N9 109.8(2) . . ? N7 N8 Cd2 125.08(19) . 2_657 ? N9 N8 Cd2 124.14(19) . 2_657 ? N8 N9 C8 104.6(2) . . ? N4 C1 N1 111.2(3) . . ? N4 C1 C2 124.6(3) . . ? N1 C1 C2 124.0(3) . . ? C7 C2 C3 118.6(3) . . ? C7 C2 C1 121.2(3) . . ? C3 C2 C1 120.1(3) . . ? C4 C3 C2 120.7(3) . . ? C3 C4 C5 120.5(3) . . ? C4 C5 C6 119.2(3) . . ? C4 C5 N5 120.3(3) . . ? C6 C5 N5 120.3(3) . . ? C7 C6 C5 119.9(3) . . ? C6 C7 C2 121.0(3) . . ? N6 C8 N9 111.2(3) . . ? N6 C8 C9 124.2(3) . . ? N9 C8 C9 124.5(3) . . ? C10 C9 C14 118.1(3) . . ? C10 C9 C8 120.8(3) . . ? C14 C9 C8 121.1(3) . . ? C11 C10 C9 121.4(3) . . ? C10 C11 C12 120.4(3) . . ? C11 C12 C13 118.8(3) . . ? C11 C12 N10 120.3(3) . . ? C13 C12 N10 120.8(3) . . ? C14 C13 C12 120.5(3) . . ? C13 C14 C9 120.8(3) . . ? 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 N10 H102 N3 0.92(4) 2.59(4) 3.341(4) 140(3) 2_656 N10 H102 N4 0.92(4) 2.40(4) 3.306(4) 171(3) 2_656 N10 H101 N1 0.82(4) 2.47(4) 3.200(4) 149(4) 2_756 N5 H52N N6 0.87(4) 2.12(4) 2.988(4) 175(3) 1_565 N5 H51N N9 0.84(4) 2.31(4) 2.957(4) 134(3) 1_665 O2 H22O N4 0.81(4) 2.19(4) 2.870(3) 141(4) . O2 H21O N1 0.83(4) 2.00(4) 2.825(4) 172(4) 1_455 O1 H1O N10 0.77(4) 2.23(4) 2.953(4) 157(4) 1_556 _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.914 _refine_diff_density_min -0.729 _refine_diff_density_rms 0.101