data_040819a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H24 Cd Cl2 N12 O12' _chemical_formula_weight 711.73 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 8.404(3) _cell_length_b 8.618(3) _cell_length_c 10.385(3) _cell_angle_alpha 66.379(4) _cell_angle_beta 76.161(5) _cell_angle_gamma 77.081(4) _cell_volume 662.2(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 901 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 24.29 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.785 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 358 _exptl_absorpt_coefficient_mu 1.105 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.684042 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3483 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2332 _reflns_number_gt 2146 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0996P)^2^+0.4408P] 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 2332 _refine_ls_number_parameters 215 _refine_ls_number_restraints 110 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1451 _refine_ls_wR_factor_gt 0.1387 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.178 _refine_ls_shift/su_max 0.005 _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 1.0000 0.0000 0.0284(2) Uani 1 2 d S . . O1 O 1.2144(6) 0.9071(8) 0.1350(6) 0.0622(14) Uani 1 1 d D . . H1A H 1.2266 0.9790 0.1680 0.075 Uiso 1 1 d RD . . H1B H 1.3021 0.8628 0.0937 0.075 Uiso 1 1 d RD . . N1 N 0.8510(6) 0.8036(6) 0.1917(5) 0.0354(11) Uani 1 1 d . . . N2 N 0.6829(8) 0.8222(8) 0.2311(7) 0.0551(15) Uani 1 1 d . . . N3 N 0.7703(6) 0.5728(6) 0.3607(5) 0.0310(10) Uani 1 1 d . . . N4 N 0.7491(6) 0.2913(6) 0.2748(5) 0.0303(10) Uani 1 1 d . . . N5 N 0.8781(6) 0.1940(6) 0.1097(5) 0.0328(10) Uani 1 1 d . . . N6 N 0.8210(9) 0.3626(8) 0.0540(7) 0.0597(17) Uani 1 1 d . . . C1 C 0.8997(7) 0.6466(7) 0.2751(6) 0.0351(13) Uani 1 1 d . . . H1 H 1.0093 0.5944 0.2743 0.042 Uiso 1 1 calc R . . C2 C 0.6299(6) 0.6845(6) 0.3339(6) 0.0270(11) Uani 1 1 d . . . H2 H 0.5215 0.6680 0.3777 0.032 Uiso 1 1 calc R . . C3 C 0.7615(8) 0.3983(7) 0.4597(6) 0.0380(14) Uani 1 1 d . . . H3A H 0.7064 0.3989 0.5530 0.046 Uiso 1 1 calc R . . H3B H 0.8727 0.3372 0.4683 0.046 Uiso 1 1 calc R . . C4 C 0.6682(8) 0.3067(7) 0.4107(6) 0.0377(14) Uani 1 1 d . . . H4A H 0.6583 0.1932 0.4824 0.045 Uiso 1 1 calc R . . H4B H 0.5574 0.3686 0.4018 0.045 Uiso 1 1 calc R . . C5 C 0.8293(7) 0.1539(7) 0.2482(6) 0.0338(12) Uani 1 1 d . . . H5 H 0.8485 0.0452 0.3169 0.041 Uiso 1 1 calc R . . C6 C 0.7416(8) 0.4274(6) 0.1503(5) 0.0329(13) Uani 1 1 d . . . H6 H 0.6921 0.5395 0.1366 0.039 Uiso 1 1 calc R . . Cl1 Cl 0.2590(2) 0.2122(2) 0.32650(19) 0.0552(5) Uani 1 1 d D . . O2 O 0.4291(12) 0.198(3) 0.2658(19) 0.103(6) Uani 0.440(13) 1 d PDU A 1 O3 O 0.217(2) 0.202(2) 0.4688(11) 0.093(6) Uani 0.440(13) 1 d PDU A 1 O4 O 0.225(3) 0.0470(18) 0.332(2) 0.140(9) Uani 0.440(13) 1 d PDU A 1 O5 O 0.1432(18) 0.314(2) 0.2349(16) 0.092(6) Uani 0.440(13) 1 d PDU A 1 O2' O 0.4156(13) 0.1138(19) 0.344(2) 0.116(6) Uani 0.560(13) 1 d PDU A 2 O3' O 0.1379(19) 0.140(2) 0.4451(16) 0.137(7) Uani 0.560(13) 1 d PDU A 2 O4' O 0.204(3) 0.227(3) 0.2022(15) 0.133(7) Uani 0.560(13) 1 d PDU A 2 O5' O 0.2700(17) 0.3906(11) 0.2980(15) 0.095(5) Uani 0.560(13) 1 d PDU A 2 O6 O 0.4926(8) 0.7374(9) 0.0350(8) 0.092(2) Uani 1 1 d DU . . H6A H 0.5267 0.7255 -0.0450 0.110 Uiso 1 1 d RD . . H6B H 0.4993 0.6475 0.1094 0.110 Uiso 1 1 d RD . . 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 0.0306(4) 0.0243(3) 0.0297(4) -0.0140(2) 0.0040(2) -0.0047(2) O1 0.049(3) 0.080(4) 0.071(4) -0.042(3) -0.022(3) 0.005(3) N1 0.033(3) 0.030(2) 0.041(3) -0.015(2) 0.009(2) -0.011(2) N2 0.052(4) 0.051(3) 0.059(4) -0.024(3) 0.002(3) -0.008(3) N3 0.037(3) 0.028(2) 0.027(2) -0.0123(19) 0.005(2) -0.011(2) N4 0.037(3) 0.024(2) 0.028(2) -0.0121(19) 0.0055(19) -0.0073(19) N5 0.044(3) 0.023(2) 0.030(2) -0.0129(19) -0.003(2) 0.000(2) N6 0.084(5) 0.037(3) 0.051(4) -0.014(3) -0.010(3) -0.001(3) C1 0.033(3) 0.033(3) 0.038(3) -0.017(3) -0.002(2) -0.002(2) C2 0.020(3) 0.023(2) 0.034(3) -0.014(2) 0.011(2) -0.005(2) C3 0.050(4) 0.033(3) 0.026(3) -0.012(2) 0.004(3) -0.007(3) C4 0.047(3) 0.028(3) 0.034(3) -0.014(2) 0.011(3) -0.013(3) C5 0.044(3) 0.022(3) 0.033(3) -0.009(2) -0.002(2) -0.006(2) C6 0.059(4) 0.013(2) 0.020(3) -0.009(2) -0.001(2) 0.008(2) Cl1 0.0498(10) 0.0642(11) 0.0469(10) -0.0192(8) -0.0123(8) 0.0032(8) O2 0.084(9) 0.123(11) 0.093(10) -0.035(8) -0.020(7) -0.002(8) O3 0.130(10) 0.105(9) 0.062(8) -0.040(7) -0.013(7) -0.035(8) O4 0.172(13) 0.132(12) 0.146(12) -0.068(9) -0.058(9) -0.014(9) O5 0.084(8) 0.088(9) 0.082(9) -0.016(7) -0.024(7) 0.012(7) O2' 0.085(8) 0.087(8) 0.156(11) -0.033(7) -0.008(7) -0.006(6) O3' 0.116(9) 0.142(10) 0.106(9) -0.017(7) 0.001(7) 0.001(8) O4' 0.164(11) 0.139(10) 0.130(10) -0.059(8) -0.050(8) -0.045(8) O5' 0.103(8) 0.067(6) 0.114(8) -0.026(6) -0.038(6) -0.004(6) O6 0.085(4) 0.096(5) 0.084(4) -0.040(4) -0.033(4) 0.038(4) _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 N5 2.312(4) 2_765 ? Cd1 N5 2.312(4) 1_565 ? Cd1 N1 2.334(4) . ? Cd1 N1 2.334(4) 2_775 ? Cd1 O1 2.349(5) 2_775 ? Cd1 O1 2.349(5) . ? O1 H1A 0.8530 . ? O1 H1B 0.8524 . ? N1 C1 1.316(8) . ? N1 N2 1.366(8) . ? N2 C2 1.319(8) . ? N3 C1 1.330(7) . ? N3 C2 1.353(7) . ? N3 C3 1.449(7) . ? N4 C5 1.322(7) . ? N4 C6 1.357(7) . ? N4 C4 1.457(7) . ? N5 C5 1.319(7) . ? N5 N6 1.350(8) . ? N5 Cd1 2.312(4) 1_545 ? N6 C6 1.311(8) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 C4 1.512(9) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? Cl1 O3 1.404(9) . ? Cl1 O2' 1.405(9) . ? Cl1 O2 1.416(9) . ? Cl1 O3' 1.418(9) . ? Cl1 O5 1.419(9) . ? Cl1 O4' 1.420(9) . ? Cl1 O5' 1.465(8) . ? Cl1 O4 1.490(10) . ? O6 H6A 0.8504 . ? O6 H6B 0.8497 . ? 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 N5 Cd1 N5 179.998(1) 2_765 1_565 ? N5 Cd1 N1 93.96(17) 2_765 . ? N5 Cd1 N1 86.05(17) 1_565 . ? N5 Cd1 N1 86.05(17) 2_765 2_775 ? N5 Cd1 N1 93.95(17) 1_565 2_775 ? N1 Cd1 N1 180.0 . 2_775 ? N5 Cd1 O1 90.11(18) 2_765 2_775 ? N5 Cd1 O1 89.89(18) 1_565 2_775 ? N1 Cd1 O1 92.9(2) . 2_775 ? N1 Cd1 O1 87.06(19) 2_775 2_775 ? N5 Cd1 O1 89.89(18) 2_765 . ? N5 Cd1 O1 90.11(18) 1_565 . ? N1 Cd1 O1 87.06(19) . . ? N1 Cd1 O1 92.93(19) 2_775 . ? O1 Cd1 O1 180.0 2_775 . ? Cd1 O1 H1A 114.2 . . ? Cd1 O1 H1B 111.5 . . ? H1A O1 H1B 116.4 . . ? C1 N1 N2 103.4(5) . . ? C1 N1 Cd1 130.5(4) . . ? N2 N1 Cd1 125.6(4) . . ? C2 N2 N1 113.0(5) . . ? C1 N3 C2 109.2(5) . . ? C1 N3 C3 130.3(5) . . ? C2 N3 C3 120.2(5) . . ? C5 N4 C6 109.6(5) . . ? C5 N4 C4 129.2(5) . . ? C6 N4 C4 121.2(4) . . ? C5 N5 N6 103.8(5) . . ? C5 N5 Cd1 125.0(4) . 1_545 ? N6 N5 Cd1 130.7(4) . 1_545 ? C6 N6 N5 113.5(5) . . ? N1 C1 N3 110.6(5) . . ? N1 C1 H1 124.7 . . ? N3 C1 H1 124.7 . . ? N2 C2 N3 103.8(5) . . ? N2 C2 H2 128.1 . . ? N3 C2 H2 128.1 . . ? N3 C3 C4 111.3(5) . . ? N3 C3 H3A 109.4 . . ? C4 C3 H3A 109.4 . . ? N3 C3 H3B 109.4 . . ? C4 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? N4 C4 C3 112.7(5) . . ? N4 C4 H4A 109.1 . . ? C3 C4 H4A 109.1 . . ? N4 C4 H4B 109.1 . . ? C3 C4 H4B 109.1 . . ? H4A C4 H4B 107.8 . . ? N5 C5 N4 109.9(5) . . ? N5 C5 H5 125.1 . . ? N4 C5 H5 125.1 . . ? N6 C6 N4 103.2(5) . . ? N6 C6 H6 128.4 . . ? N4 C6 H6 128.4 . . ? O3 Cl1 O2' 94.1(11) . . ? O3 Cl1 O2 118.0(10) . . ? O2' Cl1 O2 35.0(8) . . ? O3 Cl1 O3' 44.2(9) . . ? O2' Cl1 O3' 110.5(10) . . ? O2 Cl1 O3' 145.5(11) . . ? O3 Cl1 O5 116.9(10) . . ? O2' Cl1 O5 148.9(11) . . ? O2 Cl1 O5 118.0(10) . . ? O3' Cl1 O5 95.0(10) . . ? O3 Cl1 O4' 147.7(12) . . ? O2' Cl1 O4' 113.7(12) . . ? O2 Cl1 O4' 94.3(12) . . ? O3' Cl1 O4' 107.4(11) . . ? O5 Cl1 O4' 38.6(9) . . ? O3 Cl1 O5' 83.2(9) . . ? O2' Cl1 O5' 109.3(8) . . ? O2 Cl1 O5' 86.3(11) . . ? O3' Cl1 O5' 114.1(10) . . ? O5 Cl1 O5' 73.8(9) . . ? O4' Cl1 O5' 101.7(9) . . ? O3 Cl1 O4 104.2(11) . . ? O2' Cl1 O4 80.2(11) . . ? O2 Cl1 O4 98.4(12) . . ? O3' Cl1 O4 67.6(12) . . ? O5 Cl1 O4 94.1(11) . . ? O4' Cl1 O4 67.0(10) . . ? O5' Cl1 O4 167.9(10) . . ? H6A O6 H6B 117.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Cd1 N1 C1 49.2(5) 2_765 . . . ? N5 Cd1 N1 C1 -130.8(5) 1_565 . . . ? N1 Cd1 N1 C1 -81(11) 2_775 . . . ? O1 Cd1 N1 C1 139.6(5) 2_775 . . . ? O1 Cd1 N1 C1 -40.4(5) . . . . ? N5 Cd1 N1 N2 -121.9(5) 2_765 . . . ? N5 Cd1 N1 N2 58.1(5) 1_565 . . . ? N1 Cd1 N1 N2 107(11) 2_775 . . . ? O1 Cd1 N1 N2 -31.5(5) 2_775 . . . ? O1 Cd1 N1 N2 148.5(5) . . . . ? C1 N1 N2 C2 0.3(7) . . . . ? Cd1 N1 N2 C2 173.4(4) . . . . ? C5 N5 N6 C6 0.5(8) . . . . ? Cd1 N5 N6 C6 172.4(4) 1_545 . . . ? N2 N1 C1 N3 -0.1(7) . . . . ? Cd1 N1 C1 N3 -172.7(4) . . . . ? C2 N3 C1 N1 -0.1(7) . . . . ? C3 N3 C1 N1 173.6(5) . . . . ? N1 N2 C2 N3 -0.4(7) . . . . ? C1 N3 C2 N2 0.3(6) . . . . ? C3 N3 C2 N2 -174.1(5) . . . . ? C1 N3 C3 C4 -112.5(7) . . . . ? C2 N3 C3 C4 60.6(7) . . . . ? C5 N4 C4 C3 108.2(7) . . . . ? C6 N4 C4 C3 -75.6(7) . . . . ? N3 C3 C4 N4 62.5(7) . . . . ? N6 N5 C5 N4 -0.8(7) . . . . ? Cd1 N5 C5 N4 -173.3(4) 1_545 . . . ? C6 N4 C5 N5 0.9(7) . . . . ? C4 N4 C5 N5 177.5(5) . . . . ? N5 N6 C6 N4 0.1(8) . . . . ? C5 N4 C6 N6 -0.6(7) . . . . ? C4 N4 C6 N6 -177.5(6) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.847 _refine_diff_density_min -0.957 _refine_diff_density_rms 0.135