data_w3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H36 Cd N8, 2(Cl)' _chemical_formula_sum 'C12 H36 Cd Cl2 N8' _chemical_formula_weight 475.79 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' '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 trigonal _symmetry_space_group_name_H-M 'P 3 1 c' _symmetry_space_group_name_Hall 'P 3 -2c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, z+1/2' '-x, -x+y, z+1/2' 'x-y, -y, z+1/2' _cell_length_a 7.9706(2) _cell_length_b 7.9706(2) _cell_length_c 17.7771(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 978.08(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7679 _cell_measurement_theta_min 2.9510 _cell_measurement_theta_max 27.5579 _exptl_crystal_description rhombohedric _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 492 _exptl_absorpt_coefficient_mu 1.401 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.631 _exptl_absorpt_correction_T_max 0.735 _exptl_absorpt_process_details '(SADABS;Sheldrick,2003)' _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 'Bruker APEX2 CCD area-detector' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 18683 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0085 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 27.56 _reflns_number_total 1524 _reflns_number_gt 1517 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'SMART (Bruker, 2003)' _computing_cell_refinement 'SAINT (Bruker, 2003)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ; Mercury (Macrae et al., 2006) ; _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0394P)^2^+0.6541P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.55(3) _refine_ls_number_reflns 1524 _refine_ls_number_parameters 70 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0235 _refine_ls_R_factor_gt 0.0234 _refine_ls_wR_factor_ref 0.0629 _refine_ls_wR_factor_gt 0.0628 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_restrained_S_all 1.123 _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 0.3333 0.6667 0.100296(13) 0.02455(10) Uani 1 3 d S . . N1 N 0.3333 0.6667 -0.0507(2) 0.0232(8) Uani 1 3 d S . . N2 N 0.0157(4) 0.4376(4) 0.05054(16) 0.0359(5) Uani 1 1 d . . . H2A H 0.1138 0.4226 0.0586 0.043 Uiso 1 1 calc R . . H2B H -0.0634 0.4205 0.0865 0.043 Uiso 1 1 calc R . . N3 N 1.0000 1.0000 0.2733(2) 0.0225(7) Uani 1 3 d S . . N4 N 0.6220(4) 0.8739(4) 0.18003(16) 0.0349(5) Uani 1 1 d . . . H4A H 0.6997 0.9919 0.1670 0.042 Uiso 1 1 calc R . . H4B H 0.5317 0.7969 0.1499 0.042 Uiso 1 1 calc R . . C1 C 0.1424(4) 0.5127(4) -0.07617(17) 0.0300(6) Uani 1 1 d . . . H1A H 0.1419 0.3909 -0.0784 0.036 Uiso 1 1 calc R . . H1B H 0.1176 0.5426 -0.1264 0.036 Uiso 1 1 calc R . . C2 C -0.0162(4) 0.4921(4) -0.02389(18) 0.0349(7) Uani 1 1 d . . . H2C H -0.0160 0.6138 -0.0211 0.042 Uiso 1 1 calc R . . H2D H -0.1413 0.3938 -0.0429 0.042 Uiso 1 1 calc R . . C3 C 0.8086(4) 0.9562(4) 0.30021(16) 0.0271(5) Uani 1 1 d . . . H3A H 0.8016 1.0742 0.2997 0.033 Uiso 1 1 calc R . . H3B H 0.7931 0.9117 0.3519 0.033 Uiso 1 1 calc R . . C4 C 0.6434(4) 0.8040(5) 0.2537(2) 0.0326(6) Uani 1 1 d . . . H4C H 0.6642 0.6951 0.2463 0.039 Uiso 1 1 calc R . . H4D H 0.5237 0.7575 0.2816 0.039 Uiso 1 1 calc R . . Cl1 Cl 0.6667 1.3333 0.19100(9) 0.0362(3) Uani 1 3 d S . . Cl2 Cl 0.0000 1.0000 0.03650(10) 0.0438(3) Uani 1 3 d S . . 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 0.02400(11) 0.02400(11) 0.02566(14) 0.000 0.000 0.01200(5) N1 0.0212(11) 0.0212(11) 0.0272(19) 0.000 0.000 0.0106(6) N2 0.0280(12) 0.0317(13) 0.0433(13) -0.0022(11) 0.0068(10) 0.0113(11) N3 0.0202(10) 0.0202(10) 0.0272(16) 0.000 0.000 0.0101(5) N4 0.0267(11) 0.0318(13) 0.0409(13) -0.0062(11) -0.0116(10) 0.0105(10) C1 0.0274(13) 0.0291(13) 0.0305(12) -0.0065(11) -0.0059(11) 0.0119(11) C2 0.0202(13) 0.0315(14) 0.0512(18) -0.0042(13) -0.0048(12) 0.0115(11) C3 0.0245(13) 0.0259(13) 0.0315(12) -0.0022(10) 0.0021(10) 0.0130(10) C4 0.0201(12) 0.0265(14) 0.0475(17) 0.0006(12) -0.0034(11) 0.0089(11) Cl1 0.0313(4) 0.0313(4) 0.0460(7) 0.000 0.000 0.0156(2) Cl2 0.0370(4) 0.0370(4) 0.0575(8) 0.000 0.000 0.0185(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N2 2.429(3) . ? Cd1 N2 2.429(3) 3_565 ? Cd1 N2 2.429(3) 2_665 ? Cd1 N4 2.496(2) 2_665 ? Cd1 N4 2.496(3) . ? Cd1 N4 2.496(2) 3_565 ? Cd1 N1 2.684(4) . ? N1 C1 1.470(3) 3_565 ? N1 C1 1.470(3) . ? N1 C1 1.470(3) 2_665 ? N2 C2 1.454(4) . ? N2 H2A 0.8600 . ? N2 H2B 0.8600 . ? N3 C3 1.465(3) 3_675 ? N3 C3 1.465(3) . ? N3 C3 1.465(3) 2_765 ? N4 C4 1.466(4) . ? N4 H4A 0.8600 . ? N4 H4B 0.8600 . ? C1 C2 1.510(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2C 0.9700 . ? C2 H2D 0.9700 . ? C3 C4 1.513(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4C 0.9700 . ? C4 H4D 0.9700 . ? 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 N2 Cd1 N2 107.53(7) . 3_565 ? N2 Cd1 N2 107.53(7) . 2_665 ? N2 Cd1 N2 107.53(7) 3_565 2_665 ? N2 Cd1 N4 79.97(9) . 2_665 ? N2 Cd1 N4 79.70(10) 3_565 2_665 ? N2 Cd1 N4 166.75(9) 2_665 2_665 ? N2 Cd1 N4 166.75(9) . . ? N2 Cd1 N4 79.97(9) 3_565 . ? N2 Cd1 N4 79.70(10) 2_665 . ? N4 Cd1 N4 90.93(10) 2_665 . ? N2 Cd1 N4 79.70(10) . 3_565 ? N2 Cd1 N4 166.75(9) 3_565 3_565 ? N2 Cd1 N4 79.97(9) 2_665 3_565 ? N4 Cd1 N4 90.93(10) 2_665 3_565 ? N4 Cd1 N4 90.93(10) . 3_565 ? N2 Cd1 N1 68.65(7) . . ? N2 Cd1 N1 68.65(7) 3_565 . ? N2 Cd1 N1 68.65(7) 2_665 . ? N4 Cd1 N1 124.60(7) 2_665 . ? N4 Cd1 N1 124.60(7) . . ? N4 Cd1 N1 124.60(7) 3_565 . ? C1 N1 C1 110.96(19) 3_565 . ? C1 N1 C1 110.96(19) 3_565 2_665 ? C1 N1 C1 110.96(19) . 2_665 ? C1 N1 Cd1 107.9(2) 3_565 . ? C1 N1 Cd1 107.9(2) . . ? C1 N1 Cd1 107.9(2) 2_665 . ? C2 N2 Cd1 112.29(19) . . ? C2 N2 H2A 120.0 . . ? Cd1 N2 H2A 50.7 . . ? C2 N2 H2B 120.0 . . ? Cd1 N2 H2B 104.7 . . ? H2A N2 H2B 120.0 . . ? C3 N3 C3 109.89(18) 3_675 . ? C3 N3 C3 109.89(18) 3_675 2_765 ? C3 N3 C3 109.89(18) . 2_765 ? C4 N4 Cd1 119.99(19) . . ? C4 N4 H4A 120.0 . . ? Cd1 N4 H4A 119.4 . . ? C4 N4 H4B 120.0 . . ? Cd1 N4 H4B 7.5 . . ? H4A N4 H4B 120.0 . . ? N1 C1 C2 111.3(2) . . ? N1 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? N2 C2 C1 109.3(2) . . ? N2 C2 H2C 109.8 . . ? C1 C2 H2C 109.8 . . ? N2 C2 H2D 109.8 . . ? C1 C2 H2D 109.8 . . ? H2C C2 H2D 108.3 . . ? N3 C3 C4 113.4(2) . . ? N3 C3 H3A 108.9 . . ? C4 C3 H3A 108.9 . . ? N3 C3 H3B 108.9 . . ? C4 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? N4 C4 C3 113.8(2) . . ? N4 C4 H4C 108.8 . . ? C3 C4 H4C 108.8 . . ? N4 C4 H4D 108.8 . . ? C3 C4 H4D 108.8 . . ? H4C C4 H4D 107.7 . . ? 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 N2 Cd1 N1 C1 114.86(15) . . . 3_565 ? N2 Cd1 N1 C1 -5.14(15) 3_565 . . 3_565 ? N2 Cd1 N1 C1 -125.14(15) 2_665 . . 3_565 ? N4 Cd1 N1 C1 54.66(15) 2_665 . . 3_565 ? N4 Cd1 N1 C1 -65.34(15) . . . 3_565 ? N4 Cd1 N1 C1 174.66(15) 3_565 . . 3_565 ? N2 Cd1 N1 C1 -5.14(15) . . . . ? N2 Cd1 N1 C1 -125.14(15) 3_565 . . . ? N2 Cd1 N1 C1 114.86(15) 2_665 . . . ? N4 Cd1 N1 C1 -65.34(15) 2_665 . . . ? N4 Cd1 N1 C1 174.66(15) . . . . ? N4 Cd1 N1 C1 54.66(15) 3_565 . . . ? N2 Cd1 N1 C1 -125.14(15) . . . 2_665 ? N2 Cd1 N1 C1 114.86(15) 3_565 . . 2_665 ? N2 Cd1 N1 C1 -5.14(15) 2_665 . . 2_665 ? N4 Cd1 N1 C1 174.66(15) 2_665 . . 2_665 ? N4 Cd1 N1 C1 54.66(15) . . . 2_665 ? N4 Cd1 N1 C1 -65.34(15) 3_565 . . 2_665 ? N2 Cd1 N2 C2 31.3(2) 3_565 . . . ? N2 Cd1 N2 C2 -84.18(17) 2_665 . . . ? N4 Cd1 N2 C2 107.1(2) 2_665 . . . ? N4 Cd1 N2 C2 154.3(3) . . . . ? N4 Cd1 N2 C2 -160.1(2) 3_565 . . . ? N1 Cd1 N2 C2 -26.42(18) . . . . ? N2 Cd1 N4 C4 30.5(5) . . . . ? N2 Cd1 N4 C4 156.1(2) 3_565 . . . ? N2 Cd1 N4 C4 -93.8(2) 2_665 . . . ? N4 Cd1 N4 C4 76.75(18) 2_665 . . . ? N4 Cd1 N4 C4 -14.2(2) 3_565 . . . ? N1 Cd1 N4 C4 -148.7(2) . . . . ? C1 N1 C1 C2 -83.2(4) 3_565 . . . ? C1 N1 C1 C2 153.0(3) 2_665 . . . ? Cd1 N1 C1 C2 34.9(2) . . . . ? Cd1 N2 C2 C1 56.3(3) . . . . ? N1 C1 C2 N2 -61.9(3) . . . . ? C3 N3 C3 C4 158.3(2) 3_675 . . . ? C3 N3 C3 C4 -80.7(4) 2_765 . . . ? Cd1 N4 C4 C3 -171.30(19) . . . . ? N3 C3 C4 N4 -73.6(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 N2 H2A N4 0.86 2.53 3.157(4) 130.7 3_565 N2 H2B Cl1 0.86 2.66 3.515(3) 174.1 1_445 N4 H4A Cl1 0.86 2.89 3.503(3) 129.3 . N4 H4B N2 0.86 2.58 3.157(4) 125.5 2_665 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.300 _refine_diff_density_min -0.572 _refine_diff_density_rms 0.074