Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _journal_name_full 'Dalton Transaction' loop_ _publ_author_name 'Hirofumi Yoshikawa' 'Shin-ichi Nishikiori' 'Tokuko Watanabe' 'Toshimasa Ishida' 'Go Watanabe' 'Makoto Murakami' 'Roman Luboradzki' 'Kinga Suwinska' 'Janusz Lipkowski' _publ_contact_author_name 'Shin-ichi Nishikiori' _publ_contact_author_address ; Department of Basic Science, Graduate School of Arts and Sciences, The University of Tokyo, Komaba3-8-1, Meguro-ku, Tokyo 153-8902, Japan Tel +81-5454-6569 ; _publ_contact_author_email 'cnskor@mail.ecc.u-tokyo.ac.jp' _publ_section_title ; Polycyano-polycadmate host clathrates including a methylviologen dication. Syntheses, crystal structures and photo-induced reduction of methylviologen dication. ; data_Ia-1 _database_code_CSD 175538 _audit_creation_method SHELXL-97 _chemical_formula_structural 'Cd5 (C12 N12)(C12 N2 H14)(C4 O1 H10)' _chemical_formula_sum 'C28 H24 Cd5 N14 O1' _chemical_formula_weight 1134.65 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' 'Cd' 'Cd' -0.8075 1.2024 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Cccm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z+1/2' 'x, -y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x, -y, z-1/2' '-x, y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, z-1/2' _cell_length_a 10.970(6) _cell_length_b 23.744(8) _cell_length_c 15.906(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4143.1(30) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _exptl_crystal_description column _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 1.84 _exptl_crystal_density_diffrn 1.82 _exptl_crystal_density_method 'floating method' _exptl_crystal_F_000 2152 _exptl_absorpt_coefficient_mu 2.545 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC5S' _diffrn_measurement_method 'profile data from theta/2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 1% _diffrn_reflns_number 3351 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 29.99 _reflns_number_total 3138 _reflns_number_observed 1897 _reflns_observed_criterion >3sigma(F) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for windows' _refine_special_details ; Weighted R-factors wR and all goodnesses 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 observed criterion of F > 3sigma(F) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. CN1 is an atom of a bridging cyano group whose center is positioned at an inversion center of the crystal. CN1 was treated as a hybrid atom of 50% carbon and 50% nitrogen. CN2 is an atom of a bridging cyano group whose center is positioned at an inversion center of the crystal. CN2 was treated as a hybrid atom of 50% carbon and 50% nitrogen. Only part of the atoms of the guest molecule 1-butanol could be found clearly because of a static and/or dynamic disorder of the guest molecule. ; _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^)+(0.0741P)^2^+30.5538P] 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 noref _refine_ls_extinction_method none _refine_ls_number_reflns 1897 _refine_ls_number_parameters 120 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs 0.0586 _refine_ls_wR_factor_obs 0.1466 _refine_ls_goodness_of_fit_obs 1.167 _refine_ls_restrained_S_obs 1.167 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.2500 0.2500 0.5000 0.0306(3) Uani 1 4 d S . . Cd2 Cd 0.0000 0.38180(4) 0.2500 0.0340(2) Uani 1 2 d S . . Cd3 Cd -0.13980(10) 0.09851(6) 0.5000 0.0532(3) Uani 1 2 d S . . C1 C 0.1017(9) 0.3331(4) 0.3481(6) 0.042(2) Uani 1 1 d . . . N1 N 0.1559(7) 0.3070(3) 0.3939(5) 0.0451(19) Uani 1 1 d . . . C2 C 0.0114(15) 0.1615(7) 0.5000 0.053(4) Uani 1 2 d S . . N2 N 0.0871(13) 0.1929(6) 0.5000 0.058(3) Uani 1 2 d S . . C3 C 0.2491(10) 0.3936(6) 0.1148(7) 0.061(3) Uani 1 1 d . . . N3 N 0.1844(9) 0.3872(5) 0.1673(6) 0.075(3) Uani 1 1 d . . . CN1 C 0.0000 0.4766(5) 0.2500 0.053(3) Uani 1 2 d S . . CN2 C -0.0305(13) 0.0204(7) 0.5000 0.067(5) Uani 1 2 d S . . N101 N 0.5000 0.3535(5) 0.2500 0.068(4) Uani 1 2 d S . . C101 C 0.4168(11) 0.3804(5) 0.2947(7) 0.061(3) Uani 1 1 d . . . H101 H 0.3589 0.3603 0.3251 0.073 Uiso 1 1 calc R . . C102 C 0.4164(10) 0.4391(5) 0.2960(7) 0.053(3) Uani 1 1 d . . . H102 H 0.3590 0.4582 0.3283 0.064 Uiso 1 1 calc R . . C103 C 0.5000 0.4687(6) 0.2500 0.043(3) Uani 1 2 d S . . C111 C 0.5000 0.2911(8) 0.2500 0.142(13) Uani 1 2 d S . . H111 H 0.4197 0.2776 0.2630 0.213 Uiso 0.50 1 calc PR . . H121 H 0.5564 0.2776 0.2915 0.213 Uiso 0.50 1 calc PR . . H131 H 0.5239 0.2776 0.1955 0.213 Uiso 0.50 1 calc PR . . C201 C -0.0241(16) 0.4704(9) 0.0000 0.079(6) Uani 1 2 d S . . C202 C -0.154(3) 0.4624(13) 0.0000 0.140(12) Uani 1 2 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 0.0337(6) 0.0299(6) 0.0283(5) 0.000 0.000 0.0006(5) Cd2 0.0448(5) 0.0270(4) 0.0302(4) 0.000 -0.0062(4) 0.000 Cd3 0.0452(6) 0.0780(8) 0.0365(5) 0.000 0.000 -0.0230(6) C1 0.055(5) 0.034(4) 0.037(4) -0.001(4) -0.005(4) 0.003(4) N1 0.050(5) 0.044(4) 0.041(4) 0.007(4) -0.008(4) 0.009(4) C2 0.050(8) 0.061(9) 0.047(7) 0.000 0.000 -0.007(8) N2 0.070(9) 0.042(7) 0.063(8) 0.000 0.000 -0.014(7) C3 0.048(6) 0.090(9) 0.044(5) 0.000(6) 0.003(5) 0.009(6) N3 0.060(6) 0.119(10) 0.045(5) 0.012(6) 0.005(5) 0.000(6) CN1 0.075(9) 0.030(5) 0.053(7) 0.000 0.001(7) 0.000 CN2 0.051(10) 0.085(13) 0.065(9) 0.000 0.000 -0.026(8) N101 0.114(12) 0.030(6) 0.059(8) 0.000 -0.014(8) 0.000 C101 0.073(8) 0.054(6) 0.056(6) 0.003(6) 0.008(6) -0.019(6) C102 0.055(6) 0.053(6) 0.051(6) -0.004(5) 0.011(5) -0.013(5) C103 0.046(7) 0.044(7) 0.040(6) 0.000 -0.002(6) 0.000 C111 0.29(4) 0.026(8) 0.107(18) 0.000 -0.01(2) 0.000 C201 0.049(11) 0.098(16) 0.089(13) 0.000 0.000 0.012(10) C202 0.091(19) 0.10(2) 0.22(4) 0.000 0.000 0.006(17) _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 2.243(14) 13_556 ? Cd1 N2 2.243(14) . ? Cd1 N1 2.397(8) 10_556 ? Cd1 N1 2.397(8) 13_556 ? Cd1 N1 2.397(8) 6 ? Cd1 N1 2.397(8) . ? Cd2 C1 2.239(9) 3 ? Cd2 C1 2.239(9) . ? Cd2 CN1 2.252(12) . ? Cd2 N3 2.417(10) . ? Cd2 N3 2.417(10) 3 ? Cd3 C3 2.203(11) 8_455 ? Cd3 C3 2.203(11) 15_456 ? Cd3 CN2 2.208(17) . ? Cd3 C2 2.234(17) . ? C1 N1 1.127(11) . ? C2 N2 1.116(19) . ? C3 N3 1.106(14) . ? C3 Cd3 2.203(11) 15 ? CN1 CN1 1.11(2) 2_565 ? CN2 CN2 1.18(3) 9_556 ? N101 C101 1.322(14) 3_655 ? N101 C101 1.322(13) . ? N101 C111 1.48(2) . ? C101 C102 1.392(15) . ? C102 C103 1.369(12) . ? C103 C102 1.369(12) 3_655 ? C103 C103 1.49(3) 2_665 ? C201 C202 1.44(3) . ? C201 C201 1.50(4) 9_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 N2 Cd1 N2 180.0 13_556 . ? N2 Cd1 N1 90.1(3) 13_556 10_556 ? N2 Cd1 N1 89.9(3) . 10_556 ? N2 Cd1 N1 89.9(3) 13_556 13_556 ? N2 Cd1 N1 90.1(3) . 13_556 ? N1 Cd1 N1 90.5(4) 10_556 13_556 ? N2 Cd1 N1 89.9(3) 13_556 6 ? N2 Cd1 N1 90.1(3) . 6 ? N1 Cd1 N1 180.0 10_556 6 ? N1 Cd1 N1 89.5(4) 13_556 6 ? N2 Cd1 N1 90.1(3) 13_556 . ? N2 Cd1 N1 89.9(3) . . ? N1 Cd1 N1 89.5(4) 10_556 . ? N1 Cd1 N1 180.0 13_556 . ? N1 Cd1 N1 90.5(4) 6 . ? C1 Cd2 C1 117.8(5) 3 . ? C1 Cd2 CN1 121.1(2) 3 . ? C1 Cd2 CN1 121.1(2) . . ? C1 Cd2 N3 93.8(4) 3 . ? C1 Cd2 N3 89.4(4) . . ? CN1 Cd2 N3 86.9(3) . . ? C1 Cd2 N3 89.4(4) 3 3 ? C1 Cd2 N3 93.8(4) . 3 ? CN1 Cd2 N3 86.9(3) . 3 ? N3 Cd2 N3 173.9(6) . 3 ? C3 Cd3 C3 111.9(6) 8_455 15_456 ? C3 Cd3 CN2 111.8(4) 8_455 . ? C3 Cd3 CN2 111.8(4) 15_456 . ? C3 Cd3 C2 110.7(4) 8_455 . ? C3 Cd3 C2 110.7(4) 15_456 . ? CN2 Cd3 C2 99.1(6) . . ? N1 C1 Cd2 176.2(8) . . ? C1 N1 Cd1 173.5(8) . . ? N2 C2 Cd3 179.9(15) . . ? C2 N2 Cd1 175.3(14) . . ? N3 C3 Cd3 172.8(11) . 15 ? C3 N3 Cd2 162.8(10) . . ? CN1 CN1 Cd2 180.0 2_565 . ? CN2 CN2 Cd3 178.3(19) 9_556 . ? C101 N101 C101 122.1(13) 3_655 . ? C101 N101 C111 118.9(7) 3_655 . ? C101 N101 C111 118.9(7) . . ? N101 C101 C102 119.6(10) . . ? C103 C102 C101 120.3(10) . . ? C102 C103 C102 118.1(13) . 3_655 ? C102 C103 C103 121.0(7) . 2_665 ? C102 C103 C103 121.0(7) 3_655 2_665 ? C202 C201 C201 118(2) . 9_565 ? 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 C102 C103 C103 C102 102.8(11) . . 2_665 2_665 ? _refine_diff_density_max 1.024 _refine_diff_density_min -1.615 _refine_diff_density_rms 0.212 #===END data_Ia-2 _database_code_CSD 175539 _audit_creation_method SHELXL-97 _chemical_formula_structural 'Cd5(C12N12)(C12N2H14)(C1N1O2H3)2(O1H2)' _chemical_formula_sum 'C26 H22 Cd5 N16 O5' _chemical_formula_weight 1200.62 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' 'Cd' 'Cd' -0.8075 1.2024 '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 orthorhombic _symmetry_space_group_name_H-M Cccm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y, -z+1/2' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' '-x, y, z-1/2' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z' '-x+1/2, y+1/2, z-1/2' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.0655(2) _cell_length_b 23.9517(7) _cell_length_c 15.7838(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4183.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2558 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.91 _exptl_crystal_F_000 2280 _exptl_absorpt_coefficient_mu 2.536 _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 'Nonius-CCD' _diffrn_measurement_method \w _diffrn_reflns_number 13600 _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 27.46 _reflns_number_total 2480 _reflns_number_gt 2161 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Denzo/Scalepack' _computing_cell_refinement 'Denzo/Scalepack' _computing_data_reduction 'Denzo/Scalepack' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows' _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. CN1 is an atom of a bridging cyano group whose center is positioned at an inversion center of the crystal. CN1 was treated as a hybrid atom of 50% carbon and 50% nitrogen. CN2 is an atom of a bridging cyano group whose center is positioned at an inversion center of the crystal. CN2 was treated as a hybrid atom of 50% carbon and 50% nitrogen. ; _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^)+(0.0528P)^2^+6.0677P] 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 noref _refine_ls_extinction_method none _refine_ls_number_reflns 2480 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0995 _refine_ls_wR_factor_gt 0.0917 _refine_ls_goodness_of_fit_ref 1.177 _refine_ls_restrained_S_all 1.177 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.2500 0.2500 0.5000 0.03647(15) Uani 1 4 d S . . Cd2 Cd 0.0000 0.382420(15) 0.2500 0.03857(13) Uani 1 2 d S . . Cd3 Cd -0.13473(4) 0.09721(2) 0.5000 0.05245(16) Uani 1 2 d S . . C1 C 0.1027(4) 0.33191(17) 0.3461(2) 0.0455(8) Uani 1 1 d . . . N1 N 0.1551(3) 0.30538(15) 0.3929(2) 0.0535(8) Uani 1 1 d . . . C2 C 0.0118(6) 0.1599(3) 0.5000 0.0565(15) Uani 1 2 d S . . N2 N 0.0891(5) 0.1908(2) 0.5000 0.0579(13) Uani 1 2 d S . . C3 C 0.2493(4) 0.3951(2) 0.1123(3) 0.0582(11) Uani 1 1 d . . . N3 N 0.1792(4) 0.3890(2) 0.1620(2) 0.0703(11) Uani 1 1 d . . . CN1 C 0.0000 0.4760(2) 0.2500 0.0550(13) Uani 1 2 d S . . CN2 C -0.0310(6) 0.0199(3) 0.5000 0.0722(18) Uani 1 2 d S . . N101 N 0.5000 0.3550(3) 0.2500 0.0706(17) Uani 1 2 d S . . C101 C 0.4163(5) 0.3827(2) 0.2929(3) 0.0713(14) Uani 1 1 d . . . H101 H 0.3583 0.3629 0.3230 0.086 Uiso 1 1 calc R . . C102 C 0.4130(4) 0.4394(2) 0.2940(3) 0.0567(10) Uani 1 1 d . . . H102 H 0.3529 0.4581 0.3239 0.068 Uiso 1 1 calc R . . C103 C 0.5000 0.4690(2) 0.2500 0.0403(11) Uani 1 2 d S . . C111 C 0.5000 0.2938(5) 0.2500 0.159(7) Uani 1 2 d S . . H111 H 0.4751 0.2804 0.3046 0.238 Uiso 0.50 1 calc PR . . H121 H 0.5799 0.2804 0.2378 0.238 Uiso 0.50 1 calc PR . . H131 H 0.4450 0.2804 0.2076 0.238 Uiso 0.50 1 calc PR . . N201 N 0.1561(7) 0.4482(4) 0.5000 0.091(2) Uani 1 2 d S . . C201 C 0.0306(8) 0.4286(5) 0.5000 0.089(3) Uani 1 2 d S . . H211 H 0.0294 0.3886 0.5029 0.134 Uiso 0.50 1 calc PR . . H221 H -0.0087 0.4407 0.4490 0.134 Uiso 0.50 1 calc PR . . H231 H -0.0110 0.4438 0.5481 0.134 Uiso 0.50 1 calc PR . . O201 O 0.2009(8) 0.4573(5) 0.4331(6) 0.221(5) Uani 1 1 d . . . O1 O -0.2500 0.2500 0.5000 0.70(5) Uani 1 4 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 0.0386(3) 0.0346(3) 0.0363(3) 0.000 0.000 0.00038(19) Cd2 0.0451(2) 0.0354(2) 0.0353(2) 0.000 -0.00428(13) 0.000 Cd3 0.0414(2) 0.0754(3) 0.0406(2) 0.000 0.000 -0.0141(2) C1 0.0470(19) 0.047(2) 0.0428(19) 0.0062(15) -0.0014(15) 0.0029(16) N1 0.0595(19) 0.053(2) 0.0480(18) 0.0089(15) -0.0048(15) 0.0085(16) C2 0.051(3) 0.063(4) 0.055(3) 0.000 0.000 -0.011(3) N2 0.055(3) 0.053(3) 0.066(3) 0.000 0.000 -0.015(2) C3 0.048(2) 0.082(3) 0.045(2) 0.000(2) -0.0016(17) 0.007(2) N3 0.062(2) 0.100(4) 0.048(2) 0.002(2) 0.0073(19) -0.001(2) CN1 0.066(3) 0.042(3) 0.057(3) 0.000 0.002(2) 0.000 CN2 0.064(4) 0.078(5) 0.075(4) 0.000 0.000 -0.012(3) N101 0.116(5) 0.044(3) 0.052(3) 0.000 -0.014(3) 0.000 C101 0.089(4) 0.065(3) 0.059(3) 0.008(2) -0.003(3) -0.026(3) C102 0.057(2) 0.063(3) 0.050(2) -0.0011(19) 0.0089(18) -0.009(2) C103 0.042(3) 0.047(3) 0.033(2) 0.000 -0.0034(17) 0.000 C111 0.31(2) 0.042(5) 0.125(10) 0.000 -0.015(11) 0.000 N201 0.062(4) 0.112(6) 0.099(6) 0.000 0.000 -0.015(4) C201 0.070(5) 0.102(7) 0.095(6) 0.000 0.000 -0.015(5) O201 0.161(7) 0.331(13) 0.172(7) 0.002(8) 0.095(6) -0.061(7) O1 0.49(6) 0.28(4) 1.32(15) 0.000 0.000 0.30(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 N2 2.276(5) 13_556 ? Cd1 N2 2.276(5) . ? Cd1 N1 2.392(3) 6 ? Cd1 N1 2.392(3) . ? Cd1 N1 2.392(3) 10_556 ? Cd1 N1 2.392(3) 13_556 ? Cd2 CN1 2.241(6) . ? Cd2 C1 2.249(4) 4 ? Cd2 C1 2.249(4) . ? Cd2 N3 2.426(4) . ? Cd2 N3 2.426(4) 4 ? Cd3 CN2 2.179(8) . ? Cd3 C3 2.196(5) 7_455 ? Cd3 C3 2.196(5) 16_456 ? Cd3 C2 2.210(6) . ? C1 N1 1.134(5) . ? C2 N2 1.130(8) . ? C3 N3 1.113(6) . ? C3 Cd3 2.196(5) 7 ? CN1 CN1 1.151(12) 2_565 ? CN2 CN2 1.174(15) 9_556 ? N101 C101 1.326(7) 4_655 ? N101 C101 1.326(7) . ? N101 C111 1.465(12) . ? C101 C102 1.358(7) . ? C102 C103 1.382(5) . ? C103 C102 1.382(5) 4_655 ? C103 C103 1.487(12) 2_665 ? N201 O201 1.186(7) . ? N201 O201 1.186(7) 10_556 ? N201 C201 1.466(11) . ? 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 180.0 13_556 . ? N2 Cd1 N1 90.14(14) 13_556 6 ? N2 Cd1 N1 89.86(14) . 6 ? N2 Cd1 N1 89.86(14) 13_556 . ? N2 Cd1 N1 90.14(14) . . ? N1 Cd1 N1 90.03(18) 6 . ? N2 Cd1 N1 89.86(14) 13_556 10_556 ? N2 Cd1 N1 90.14(14) . 10_556 ? N1 Cd1 N1 180.0 6 10_556 ? N1 Cd1 N1 89.97(18) . 10_556 ? N2 Cd1 N1 90.14(14) 13_556 13_556 ? N2 Cd1 N1 89.86(14) . 13_556 ? N1 Cd1 N1 89.97(18) 6 13_556 ? N1 Cd1 N1 180.0 . 13_556 ? N1 Cd1 N1 90.03(18) 10_556 13_556 ? CN1 Cd2 C1 122.55(11) . 4 ? CN1 Cd2 C1 122.55(11) . . ? C1 Cd2 C1 114.9(2) 4 . ? CN1 Cd2 N3 86.28(12) . . ? C1 Cd2 N3 93.56(14) 4 . ? C1 Cd2 N3 90.44(15) . . ? CN1 Cd2 N3 86.28(12) . 4 ? C1 Cd2 N3 90.44(15) 4 4 ? C1 Cd2 N3 93.56(14) . 4 ? N3 Cd2 N3 172.6(2) . 4 ? CN2 Cd3 C3 112.30(17) . 7_455 ? CN2 Cd3 C3 112.30(17) . 16_456 ? C3 Cd3 C3 107.6(2) 7_455 16_456 ? CN2 Cd3 C2 101.0(3) . . ? C3 Cd3 C2 111.80(16) 7_455 . ? C3 Cd3 C2 111.80(16) 16_456 . ? N1 C1 Cd2 178.1(4) . . ? C1 N1 Cd1 174.8(3) . . ? N2 C2 Cd3 178.0(6) . . ? C2 N2 Cd1 177.7(6) . . ? N3 C3 Cd3 170.9(4) . 7 ? C3 N3 Cd2 169.0(4) . . ? CN1 CN1 Cd2 180.0 2_565 . ? CN2 CN2 Cd3 176.1(9) 9_556 . ? C101 N101 C101 119.8(6) 4_655 . ? C101 N101 C111 120.1(3) 4_655 . ? C101 N101 C111 120.1(3) . . ? N101 C101 C102 121.8(5) . . ? C101 C102 C103 119.1(5) . . ? C102 C103 C102 118.4(6) . 4_655 ? C102 C103 C103 120.8(3) . 2_665 ? C102 C103 C103 120.8(3) 4_655 2_665 ? O201 N201 O201 125.7(12) . 10_556 ? O201 N201 C201 117.1(6) . . ? O201 N201 C201 117.1(6) 10_556 . ? 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 C102 C103 C103 C102 108.4(4) . . 2_665 2_665 ? _refine_diff_density_max 1.198 _refine_diff_density_min -1.016 _refine_diff_density_rms 0.131 #===END data_Ib-1 _database_code_CSD 175540 _audit_creation_method SHELXL-97 _chemical_formula_structural 'Cd5 (C12 N12)(C12 N2 H14)(C2 Cl2 H4)1.5' _chemical_formula_sum 'C27 H20 Cd5 Cl3 N14 ' _chemical_formula_weight 1208.96 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' 'Cd' 'Cd' -0.8075 1.2024 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pncm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y+1/2, z+1/2' '-x, y+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' '-x, y-1/2, -z-1/2' 'x, -y-1/2, -z-1/2' _cell_length_a 10.946(3) _cell_length_b 23.705(3) _cell_length_c 15.847(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4111.9(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _exptl_crystal_description column _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 1.94 _exptl_crystal_density_diffrn 1.95 _exptl_crystal_density_method 'floating method' _exptl_crystal_F_000 2284 _exptl_absorpt_coefficient_mu 2.756 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC5S' _diffrn_measurement_method 'profile data from theta/2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 2% _diffrn_reflns_number 5269 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4900 _reflns_number_observed 1885 _reflns_observed_criterion >3sigma(F) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for windows' _refine_special_details ; Weighted R-factors wR and all goodnesses 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 observed criterion of F > 3sigma(F) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. A non-standard crystal axes setting is applied for easy comparison of the crystal structure with the other crystal structures. CN1 is an atom of a bridging cyano group whose center is positioned at an inversion center of the crystal. CN1 was treated as a hybrid atom of 50% carbon and 50% nitrogen. One of two 1,2-dichloroethane molecules(Cl3, C301) lies on a site with 2/m symmetry. Its conformation is trans, and its molecular plane is perpendicular to the mirror plane. This structural situation gives a disordered structure in which two trans form molecules overlap each other. ; _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^)+(0.0605P)^2^+0.0000P] 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 noref _refine_ls_extinction_method none _refine_ls_number_reflns 1885 _refine_ls_number_parameters 237 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs 0.0716 _refine_ls_wR_factor_obs 0.1356 _refine_ls_goodness_of_fit_obs 1.098 _refine_ls_restrained_S_obs 1.098 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.5000 0.5000 0.5000 0.0283(7) Uani 1 4 d S . . Cd2 Cd 1.0000 0.5000 1.0000 0.0315(7) Uani 1 4 d S . . Cd3 Cd 0.76920(12) 0.36831(6) 0.74078(8) 0.0326(4) Uani 1 1 d . . . Cd4 Cd 1.41770(18) 0.36459(10) 1.0000 0.0387(5) Uani 1 2 d S . . Cd5 Cd 0.13864(19) 0.33205(10) 0.5000 0.0388(6) Uani 1 2 d S . . CN1 C 0.7491(19) 0.2731(7) 0.7486(13) 0.052(5) Uani 1 1 d . . . C1 C 0.6662(16) 0.4170(8) 0.6435(10) 0.029(4) Uani 1 1 d . . . N1 N 0.6061(14) 0.4449(7) 0.6015(10) 0.044(4) Uani 1 1 d . . . C2 C 0.277(3) 0.3986(12) 0.5000 0.040(7) Uani 1 2 d S . . N2 N 0.347(2) 0.4348(11) 0.5000 0.045(6) Uani 1 2 d S . . C3 C 1.261(2) 0.4230(13) 1.0000 0.040(8) Uani 1 2 d S . . N3 N 1.178(3) 0.4500(10) 1.0000 0.058(8) Uani 1 2 d S . . C4 C 0.5237(17) 0.3712(10) 0.8872(13) 0.053(6) Uani 1 1 d . . . N4 N 0.5852(17) 0.3734(9) 0.8295(11) 0.068(6) Uani 1 1 d . . . C5 C 0.247(3) 0.2587(11) 0.5000 0.045(9) Uani 1 2 d S . . N5 N 0.309(3) 0.2184(14) 0.5000 0.080(10) Uani 1 2 d S . . C6 C 0.0209(15) 0.3405(9) 0.6126(14) 0.050(6) Uani 1 1 d . . . N6 N -0.0506(14) 0.3473(7) 0.6606(12) 0.054(5) Uani 1 1 d . . . C7 C 0.8723(18) 0.4146(9) 0.8389(13) 0.045(5) Uani 1 1 d . . . N7 N 0.9189(15) 0.4410(7) 0.8914(10) 0.045(5) Uani 1 1 d . . . N101 N 0.2723(19) 0.3963(8) 0.7563(10) 0.051(5) Uani 1 1 d . . . C101 C 0.186(2) 0.3688(10) 0.7973(15) 0.056(6) Uani 1 1 d . . . H101 H 0.1264 0.3884 0.8267 0.067 Uiso 1 1 calc R . . C102 C 0.1818(19) 0.3109(10) 0.7961(13) 0.056(6) Uani 1 1 d . . . H102 H 0.1206 0.2911 0.8246 0.067 Uiso 1 1 calc R . . C103 C 0.2706(18) 0.2817(7) 0.7506(13) 0.040(5) Uani 1 1 d . . . C104 C 0.359(2) 0.3104(9) 0.7072(13) 0.052(6) Uani 1 1 d . . . H104 H 0.4217 0.2913 0.6788 0.062 Uiso 1 1 calc R . . C105 C 0.349(2) 0.3679(11) 0.7091(13) 0.058(6) Uani 1 1 d . . . H105 H 0.4028 0.3877 0.6744 0.070 Uiso 1 1 calc R . . C111 C 0.279(3) 0.4590(10) 0.7597(18) 0.109(12) Uani 1 1 d . . . H111 H 0.2894 0.4737 0.7037 0.166 Uiso 1 1 calc R . . H121 H 0.3468 0.4701 0.7942 0.166 Uiso 1 1 calc R . . H131 H 0.2046 0.4734 0.7835 0.166 Uiso 1 1 calc R . . Cl1 Cl -0.0412(10) 0.2022(5) 0.5000 0.092(4) Uani 1 2 d S . . Cl2 Cl -0.4054(10) 0.2722(6) 0.5000 0.111(4) Uani 1 2 d S . . Cl3 Cl 1.0000 0.5000 0.6332(10) 0.151(6) Uani 1 2 d S . . C201 C -0.210(5) 0.214(2) 0.5000 0.123(19) Uiso 1 2 d S . . H211 H -0.2357 0.1960 0.4512 0.175 Uiso 0.50 1 calc PR . . H221 H -0.2357 0.1960 0.5488 0.175 Uiso 0.50 1 calc PR . . C202 C -0.249(6) 0.262(3) 0.5000 0.16(2) Uiso 1 2 d S . . H212 H -0.2278 0.2809 0.4511 0.243 Uiso 0.50 1 calc PR . . H222 H -0.2278 0.2809 0.5489 0.243 Uiso 0.50 1 calc PR . . C301 C 0.953(4) 0.485(2) 0.531(3) 0.080(18) Uiso 0.50 1 d P . . H312 H 0.9652 0.4479 0.5545 0.097 Uiso 0.50 1 calc PR . . H322 H 0.8822 0.5034 0.5545 0.097 Uiso 0.50 1 calc PR . . 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 0.0284(15) 0.0272(17) 0.0292(14) 0.000 0.000 -0.0002(13) Cd2 0.0313(15) 0.0348(19) 0.0284(14) 0.000 0.000 0.0036(15) Cd3 0.0403(8) 0.0287(7) 0.0289(7) 0.0003(7) -0.0038(6) 0.0036(7) Cd4 0.0300(11) 0.0512(14) 0.0349(11) 0.000 0.000 0.0057(12) Cd5 0.0332(12) 0.0464(14) 0.0367(11) 0.000 0.000 -0.0063(11) CN1 0.073(14) 0.041(10) 0.042(10) -0.005(13) 0.015(11) 0.014(9) C1 0.038(11) 0.023(10) 0.027(9) 0.003(8) 0.011(8) 0.008(8) N1 0.047(11) 0.043(11) 0.043(10) 0.012(9) 0.004(8) 0.010(9) C2 0.047(18) 0.023(17) 0.049(17) 0.000 0.000 -0.001(16) N2 0.047(16) 0.048(17) 0.040(14) 0.000 0.000 0.002(14) C3 0.020(15) 0.05(2) 0.053(17) 0.000 0.000 0.017(15) N3 0.07(2) 0.024(16) 0.08(2) 0.000 0.000 0.012(14) C4 0.038(14) 0.072(17) 0.049(12) 0.000(13) -0.007(10) 0.003(13) N4 0.063(13) 0.079(15) 0.061(12) 0.016(12) 0.023(11) 0.010(12) C5 0.06(2) 0.02(2) 0.054(18) 0.000 0.000 0.015(16) N5 0.08(3) 0.09(3) 0.07(2) 0.000 0.000 -0.03(2) C6 0.007(12) 0.067(16) 0.075(15) 0.006(13) -0.003(10) 0.010(9) N6 0.026(10) 0.064(14) 0.073(13) 0.005(10) 0.016(9) -0.007(8) C7 0.033(11) 0.050(14) 0.053(13) -0.003(12) 0.015(11) 0.005(10) N7 0.045(11) 0.058(13) 0.032(9) 0.000(9) -0.002(9) -0.002(9) N101 0.071(13) 0.050(11) 0.034(9) 0.006(10) -0.028(10) 0.005(11) C101 0.069(16) 0.028(13) 0.072(15) -0.026(14) 0.004(13) 0.000(13) C102 0.055(14) 0.068(18) 0.045(13) -0.007(13) -0.012(11) 0.014(12) C103 0.024(10) 0.046(12) 0.050(12) -0.012(12) 0.010(11) -0.013(9) C104 0.055(14) 0.049(15) 0.052(13) -0.017(12) -0.001(12) -0.010(12) C105 0.079(17) 0.054(16) 0.043(12) 0.008(13) -0.005(12) 0.002(16) C111 0.20(4) 0.023(13) 0.10(2) 0.002(15) -0.03(2) 0.010(18) Cl1 0.085(8) 0.087(8) 0.105(9) 0.000 0.000 -0.028(6) Cl2 0.060(7) 0.145(12) 0.128(11) 0.000 0.000 -0.026(7) Cl3 0.167(13) 0.112(11) 0.175(14) 0.000 0.000 -0.023(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 Cd1 N2 2.28(3) . ? Cd1 N2 2.28(3) 5_666 ? Cd1 N1 2.375(16) 6_556 ? Cd1 N1 2.375(16) 2_665 ? Cd1 N1 2.375(16) . ? Cd1 N1 2.375(16) 5_666 ? Cd2 N3 2.28(3) . ? Cd2 N3 2.28(3) 5_767 ? Cd2 N7 2.390(17) . ? Cd2 N7 2.390(17) 6_557 ? Cd2 N7 2.390(17) 5_767 ? Cd2 N7 2.390(17) 2_765 ? Cd3 C7 2.21(2) . ? Cd3 C1 2.230(18) . ? Cd3 CN1 2.271(17) . ? Cd3 N6 2.398(16) 1_655 ? Cd3 N4 2.459(18) . ? Cd4 C4 2.14(2) 6_657 ? Cd4 C4 2.14(2) 1_655 ? Cd4 C3 2.20(3) . ? Cd4 N5 2.30(4) 3_655 ? Cd5 C5 2.10(3) . ? Cd5 C2 2.19(3) . ? Cd5 C6 2.21(2) 6_556 ? Cd5 C6 2.21(2) . ? CN1 CN1 1.10(3) 8_567 ? C1 N1 1.15(2) . ? C2 N2 1.15(3) . ? C3 N3 1.11(3) . ? C4 N4 1.14(2) . ? C4 Cd4 2.14(2) 1_455 ? C5 N5 1.17(4) . ? N5 Cd4 2.30(4) 3_454 ? C6 N6 1.10(2) . ? N6 Cd3 2.398(16) 1_455 ? C7 N7 1.16(2) . ? N101 C105 1.31(3) . ? N101 C101 1.32(3) . ? N101 C111 1.49(3) . ? C101 C102 1.37(3) . ? C102 C103 1.39(3) . ? C103 C104 1.37(3) . ? C103 C103 1.50(4) 8_567 ? C104 C105 1.37(3) . ? Cl1 C201 1.87(5) . ? Cl2 C202 1.73(6) . ? Cl3 C301 1.74(5) . ? C201 C202 1.23(7) . ? C301 C301 1.58(8) 5_766 ? 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 180.0(10) . 5_666 ? N2 Cd1 N1 89.2(6) . 6_556 ? N2 Cd1 N1 90.8(6) 5_666 6_556 ? N2 Cd1 N1 90.8(6) . 2_665 ? N2 Cd1 N1 89.2(6) 5_666 2_665 ? N1 Cd1 N1 180.000(3) 6_556 2_665 ? N2 Cd1 N1 89.2(6) . . ? N2 Cd1 N1 90.8(6) 5_666 . ? N1 Cd1 N1 85.2(7) 6_556 . ? N1 Cd1 N1 94.8(7) 2_665 . ? N2 Cd1 N1 90.8(6) . 5_666 ? N2 Cd1 N1 89.2(6) 5_666 5_666 ? N1 Cd1 N1 94.8(7) 6_556 5_666 ? N1 Cd1 N1 85.2(7) 2_665 5_666 ? N1 Cd1 N1 180.000(3) . 5_666 ? N3 Cd2 N3 180.000(7) . 5_767 ? N3 Cd2 N7 90.8(6) . . ? N3 Cd2 N7 89.2(6) 5_767 . ? N3 Cd2 N7 90.8(6) . 6_557 ? N3 Cd2 N7 89.2(6) 5_767 6_557 ? N7 Cd2 N7 92.2(8) . 6_557 ? N3 Cd2 N7 89.2(6) . 5_767 ? N3 Cd2 N7 90.8(6) 5_767 5_767 ? N7 Cd2 N7 180.000(4) . 5_767 ? N7 Cd2 N7 87.8(8) 6_557 5_767 ? N3 Cd2 N7 89.2(6) . 2_765 ? N3 Cd2 N7 90.8(6) 5_767 2_765 ? N7 Cd2 N7 87.8(8) . 2_765 ? N7 Cd2 N7 180.000(3) 6_557 2_765 ? N7 Cd2 N7 92.2(8) 5_767 2_765 ? C7 Cd3 C1 119.1(7) . . ? C7 Cd3 CN1 120.3(8) . . ? C1 Cd3 CN1 120.2(7) . . ? C7 Cd3 N6 93.2(6) . 1_655 ? C1 Cd3 N6 99.0(6) . 1_655 ? CN1 Cd3 N6 84.4(6) . 1_655 ? C7 Cd3 N4 89.5(7) . . ? C1 Cd3 N4 87.5(6) . . ? CN1 Cd3 N4 86.5(7) . . ? N6 Cd3 N4 170.6(6) 1_655 . ? C4 Cd4 C4 113.6(10) 6_657 1_655 ? C4 Cd4 C3 112.1(7) 6_657 . ? C4 Cd4 C3 112.1(7) 1_655 . ? C4 Cd4 N5 110.0(7) 6_657 3_655 ? C4 Cd4 N5 110.0(7) 1_655 3_655 ? C3 Cd4 N5 97.8(11) . 3_655 ? C5 Cd5 C2 101.8(12) . . ? C5 Cd5 C6 113.8(7) . 6_556 ? C2 Cd5 C6 109.8(7) . 6_556 ? C5 Cd5 C6 113.8(7) . . ? C2 Cd5 C6 109.8(7) . . ? C6 Cd5 C6 107.7(10) 6_556 . ? CN1 CN1 Cd3 174.4(6) 8_567 . ? N1 C1 Cd3 171.8(14) . . ? C1 N1 Cd1 172.5(14) . . ? N2 C2 Cd5 178(3) . . ? C2 N2 Cd1 175(2) . . ? N3 C3 Cd4 176(3) . . ? C3 N3 Cd2 176(3) . . ? N4 C4 Cd4 176.2(19) . 1_455 ? C4 N4 Cd3 160.6(17) . . ? N5 C5 Cd5 179(3) . . ? C5 N5 Cd4 176(3) . 3_454 ? N6 C6 Cd5 169.6(18) . . ? C6 N6 Cd3 168.2(18) . 1_455 ? N7 C7 Cd3 175.2(18) . . ? C7 N7 Cd2 175.3(17) . . ? C105 N101 C101 119(2) . . ? C105 N101 C111 120(2) . . ? C101 N101 C111 121(2) . . ? N101 C101 C102 121(2) . . ? C101 C102 C103 119(2) . . ? C104 C103 C102 120.5(19) . . ? C104 C103 C103 119.4(17) . 8_567 ? C102 C103 C103 120.2(18) . 8_567 ? C105 C104 C103 115(2) . . ? N101 C105 C104 125(2) . . ? C301 Cl3 C301 42(3) . 2_765 ? C202 C201 Cl1 119(5) . . ? C201 C202 Cl2 118(6) . . ? C301 C301 Cl3 107(4) 5_766 . ? _refine_diff_density_max 0.760 _refine_diff_density_min -0.824 _refine_diff_density_rms 0.180 #===END data_IIa-1 _database_code_CSD 175541 _audit_creation_method SHELXL-97 _chemical_formula_structural 'Cd6 (C14 N14)(C12 N2 H14)(C1 Cl3 H1)2' _chemical_formula_sum 'C28 H16 Cd6 Cl6 N16 ' _chemical_formula_weight 1463.73 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' 'Cd' 'Cd' -0.8075 1.2024 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.6454(2) _cell_length_b 27.2037(4) _cell_length_c 13.5497(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5029.72(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6005 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description platlet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.93 _exptl_crystal_F_000 2744 _exptl_absorpt_coefficient_mu 2.825 _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 'Nonius-CCD' _diffrn_measurement_method \w _diffrn_reflns_number 32532 _diffrn_reflns_av_R_equivalents 0.046 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5660 _reflns_number_gt 4342 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Denzo/Scalepack' _computing_cell_refinement 'Denzo/Scalepack' _computing_data_reduction 'Denzo/Scalepack' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows' _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. ; _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^)+(0.0526P)^2^+8.5848P] 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 noref _refine_ls_extinction_method none _refine_ls_number_reflns 5660 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0602 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.1121 _refine_ls_wR_factor_gt 0.0948 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.82567(3) 0.875723(13) 0.01342(3) 0.03488(12) Uani 1 1 d . . . Cd2 Cd 0.44769(3) 0.808074(14) 0.11674(3) 0.04080(12) Uani 1 1 d . . . Cd3 Cd 0.70555(3) 0.923127(14) -0.37520(3) 0.04001(12) Uani 1 1 d . . . N1 N 0.6714(4) 0.84676(18) 0.0561(4) 0.0510(12) Uani 1 1 d . . . C1 C 0.5980(4) 0.8308(2) 0.0762(4) 0.0455(13) Uani 1 1 d . . . N2 N 0.8894(4) 0.8573(2) 0.1665(4) 0.0617(14) Uani 1 1 d . . . C2 C 0.9103(5) 0.8403(2) 0.2394(4) 0.0531(14) Uani 1 1 d . . . N3 N 0.9789(4) 0.90191(19) -0.0464(4) 0.0556(12) Uani 1 1 d . . . C3 C 1.0557(4) 0.9060(2) -0.0757(4) 0.0463(13) Uani 1 1 d . . . N4 N 0.7575(4) 0.9031(2) -0.1383(4) 0.0586(13) Uani 1 1 d . . . C4 C 0.7363(5) 0.9111(2) -0.2180(4) 0.0500(14) Uani 1 1 d . . . N5 N 0.3632(4) 0.8618(2) 0.0187(4) 0.0627(14) Uani 1 1 d . . . C5 C 0.3113(5) 0.8838(2) -0.0308(5) 0.0520(15) Uani 1 1 d . . . N6 N 0.7944(4) 0.95599(18) 0.0734(4) 0.0583(13) Uani 1 1 d . . . C6 C 0.7882(4) 0.9960(2) 0.0935(4) 0.0479(14) Uani 1 1 d . . . N7 N 0.8618(4) 0.80020(18) -0.0515(4) 0.0577(13) Uani 1 1 d . . . C7 C 0.8926(4) 0.7633(2) -0.0747(4) 0.0495(14) Uani 1 1 d . . . N101 N 0.5594(4) 0.9825(2) 0.2482(4) 0.0646(14) Uani 1 1 d . . . C101 C 0.5653(6) 0.9458(2) 0.1845(6) 0.075(2) Uani 1 1 d . . . H101 H 0.5860 0.9151 0.2064 0.090 Uiso 1 1 calc R . . C102 C 0.5417(6) 0.9519(2) 0.0880(6) 0.073(2) Uani 1 1 d . . . H102 H 0.5455 0.9252 0.0452 0.088 Uiso 1 1 calc R . . C103 C 0.5126(4) 0.9963(2) 0.0527(4) 0.0466(13) Uani 1 1 d . . . C104 C 0.5093(7) 1.0343(3) 0.1202(5) 0.077(2) Uani 1 1 d . . . H104 H 0.4903 1.0655 0.0996 0.093 Uiso 1 1 calc R . . C105 C 0.5333(7) 1.0269(3) 0.2155(6) 0.089(3) Uani 1 1 d . . . H105 H 0.5316 1.0532 0.2594 0.106 Uiso 1 1 calc R . . C111 C 0.5864(9) 0.9743(4) 0.3532(6) 0.108(3) Uani 1 1 d . . . H111 H 0.5309 0.9614 0.3882 0.161 Uiso 1 1 calc R . . H121 H 0.6060 1.0049 0.3824 0.161 Uiso 1 1 calc R . . H131 H 0.6396 0.9513 0.3567 0.161 Uiso 1 1 calc R . . Cl1 Cl 0.6958(4) 0.72281(19) 0.2070(3) 0.215(2) Uani 1 1 d . . . Cl2 Cl 0.6309(4) 0.77560(17) 0.3714(4) 0.229(3) Uani 1 1 d . . . Cl3 Cl 0.5265(3) 0.6915(2) 0.3089(4) 0.221(2) Uani 1 1 d . . . C201 C 0.6406(8) 0.7188(5) 0.3197(8) 0.124(4) Uani 1 1 d . . . H201 H 0.6814 0.6983 0.3626 0.149 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 0.0366(2) 0.03465(19) 0.0334(2) 0.00094(14) -0.00080(15) -0.00132(15) Cd2 0.0420(2) 0.0390(2) 0.0414(2) -0.00583(16) 0.00587(16) -0.00514(16) Cd3 0.0414(2) 0.0407(2) 0.0380(2) 0.00400(16) -0.00718(16) 0.00046(16) N1 0.046(3) 0.049(3) 0.058(3) 0.002(2) 0.008(2) -0.003(2) C1 0.047(3) 0.041(3) 0.050(3) -0.001(2) 0.006(3) -0.001(3) N2 0.065(3) 0.075(4) 0.045(3) 0.010(3) -0.008(3) 0.000(3) C2 0.056(4) 0.059(4) 0.044(3) 0.007(3) -0.006(3) -0.003(3) N3 0.047(3) 0.064(3) 0.055(3) 0.001(3) 0.004(2) -0.010(3) C3 0.043(3) 0.051(3) 0.045(3) 0.001(3) 0.006(3) -0.008(3) N4 0.071(4) 0.064(3) 0.041(3) 0.008(2) -0.014(3) 0.002(3) C4 0.057(4) 0.051(3) 0.042(3) 0.010(3) -0.008(3) -0.004(3) N5 0.064(3) 0.063(3) 0.061(3) 0.010(3) -0.006(3) 0.006(3) C5 0.051(4) 0.054(4) 0.051(4) 0.005(3) 0.002(3) 0.005(3) N6 0.071(4) 0.043(3) 0.061(3) -0.010(2) 0.004(3) 0.000(2) C6 0.053(4) 0.042(3) 0.048(3) -0.002(3) 0.007(3) -0.008(3) N7 0.058(3) 0.045(3) 0.070(4) -0.010(2) 0.003(3) 0.008(2) C7 0.045(3) 0.046(3) 0.058(4) -0.004(3) 0.000(3) 0.002(3) N101 0.076(4) 0.065(4) 0.052(3) 0.010(3) 0.007(3) -0.001(3) C101 0.105(6) 0.044(4) 0.076(5) 0.000(3) -0.030(4) 0.002(4) C102 0.100(6) 0.045(4) 0.074(5) -0.009(3) -0.036(4) 0.011(4) C103 0.039(3) 0.045(3) 0.056(3) -0.002(3) 0.005(3) 0.000(2) C104 0.117(7) 0.057(4) 0.057(5) 0.000(3) 0.020(4) 0.023(4) C105 0.137(8) 0.073(5) 0.056(5) -0.011(4) 0.025(5) 0.018(5) C111 0.154(9) 0.116(7) 0.053(5) 0.014(5) -0.002(5) 0.002(7) Cl1 0.283(6) 0.211(5) 0.150(3) 0.094(3) 0.034(3) 0.054(4) Cl2 0.250(5) 0.159(4) 0.280(6) -0.033(4) -0.076(4) 0.103(4) Cl3 0.129(3) 0.326(7) 0.209(5) 0.039(4) -0.074(3) 0.001(3) C201 0.117(8) 0.150(10) 0.106(8) 0.043(7) -0.014(6) 0.042(7) _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 N7 2.289(5) . ? Cd1 N2 2.305(5) . ? Cd1 N1 2.321(5) . ? Cd1 N3 2.353(5) . ? Cd1 N6 2.369(5) . ? Cd1 N4 2.376(5) . ? Cd2 C7 2.159(6) 4_465 ? Cd2 C2 2.198(6) 6_556 ? Cd2 C1 2.212(6) . ? Cd2 N5 2.288(6) . ? Cd3 C4 2.196(6) . ? Cd3 C3 2.201(6) 6 ? Cd3 C5 2.202(6) 6_655 ? Cd3 C6 2.241(6) 2_674 ? N1 C1 1.125(7) . ? N2 C2 1.126(7) . ? C2 Cd2 2.198(6) 6_656 ? N3 C3 1.126(7) . ? C3 Cd3 2.201(6) 6_655 ? N4 C4 1.139(7) . ? N5 C5 1.143(8) . ? C5 Cd3 2.202(6) 6 ? N6 C6 1.127(7) . ? C6 Cd3 2.241(6) 2_675 ? N7 C7 1.133(7) . ? C7 Cd2 2.159(6) 4_565 ? N101 C101 1.324(9) . ? N101 C105 1.333(9) . ? N101 C111 1.486(10) . ? C101 C102 1.357(10) . ? C102 C103 1.359(8) . ? C103 C104 1.382(9) . ? C103 C103 1.482(12) 5_675 ? C104 C105 1.347(10) . ? Cl1 C201 1.705(12) . ? Cl2 C201 1.702(13) . ? Cl3 C201 1.731(13) . ? 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 N7 Cd1 N2 94.0(2) . . ? N7 Cd1 N1 89.22(18) . . ? N2 Cd1 N1 92.52(19) . . ? N7 Cd1 N3 87.03(19) . . ? N2 Cd1 N3 92.34(19) . . ? N1 Cd1 N3 174.06(18) . . ? N7 Cd1 N6 176.60(19) . . ? N2 Cd1 N6 87.7(2) . . ? N1 Cd1 N6 93.66(18) . . ? N3 Cd1 N6 89.95(18) . . ? N7 Cd1 N4 91.9(2) . . ? N2 Cd1 N4 174.09(19) . . ? N1 Cd1 N4 88.11(19) . . ? N3 Cd1 N4 87.41(19) . . ? N6 Cd1 N4 86.38(19) . . ? C7 Cd2 C2 120.8(2) 4_465 6_556 ? C7 Cd2 C1 120.6(2) 4_465 . ? C2 Cd2 C1 108.9(2) 6_556 . ? C7 Cd2 N5 104.2(2) 4_465 . ? C2 Cd2 N5 98.2(2) 6_556 . ? C1 Cd2 N5 98.3(2) . . ? C4 Cd3 C3 116.1(2) . 6 ? C4 Cd3 C5 111.3(2) . 6_655 ? C3 Cd3 C5 109.3(2) 6 6_655 ? C4 Cd3 C6 108.8(2) . 2_674 ? C3 Cd3 C6 100.7(2) 6 2_674 ? C5 Cd3 C6 110.0(2) 6_655 2_674 ? C1 N1 Cd1 177.2(5) . . ? N1 C1 Cd2 173.6(5) . . ? C2 N2 Cd1 166.8(5) . . ? N2 C2 Cd2 178.5(6) . 6_656 ? C3 N3 Cd1 168.0(5) . . ? N3 C3 Cd3 172.9(5) . 6_655 ? C4 N4 Cd1 168.4(5) . . ? N4 C4 Cd3 175.5(6) . . ? C5 N5 Cd2 170.6(6) . . ? N5 C5 Cd3 177.1(6) . 6 ? C6 N6 Cd1 171.3(5) . . ? N6 C6 Cd3 172.8(5) . 2_675 ? C7 N7 Cd1 169.1(5) . . ? N7 C7 Cd2 178.3(6) . 4_565 ? C101 N101 C105 118.9(6) . . ? C101 N101 C111 119.7(7) . . ? C105 N101 C111 121.3(7) . . ? N101 C101 C102 121.4(6) . . ? C101 C102 C103 121.1(6) . . ? C102 C103 C104 116.2(6) . . ? C102 C103 C103 121.9(7) . 5_675 ? C104 C103 C103 121.9(7) . 5_675 ? C105 C104 C103 121.0(7) . . ? N101 C105 C104 121.3(7) . . ? Cl2 C201 Cl1 110.2(7) . . ? Cl2 C201 Cl3 110.7(7) . . ? Cl1 C201 Cl3 110.4(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 C102 C103 C103 C102 180.0 . . 5_675 5_675 ? _refine_diff_density_max 0.850 _refine_diff_density_min -0.806 _refine_diff_density_rms 0.141 #===END data_IIa-2 _database_code_CSD 175542 _audit_creation_method SHELXL-97 _chemical_formula_structural 'Cd6 (C14 N14)(C12 N2 H14)(C2 N1 H3)2' _chemical_formula_sum 'C30 H20 Cd6 N18' _chemical_formula_weight 1307.08 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' 'Cd' 'Cd' -0.8075 1.2024 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.794(8) _cell_length_b 26.990(6) _cell_length_c 13.665(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5087.5(37) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _exptl_crystal_description platlet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 1.75 _exptl_crystal_density_diffrn 1.71 _exptl_crystal_density_method 'floating method' _exptl_crystal_F_000 2456 _exptl_absorpt_coefficient_mu 2.482 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC5S' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 2% _diffrn_reflns_number 8172 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 30.01 _reflns_number_total 7429 _reflns_number_observed 2658 _reflns_observed_criterion >3sigma(F) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for windows' _refine_special_details ; Weighted R-factors wR and all goodnesses 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 observed criterion of F > 3sigma(F) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. ; _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^)+(0.0896P)^2^+30.7340P] 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 noref _refine_ls_extinction_method none _refine_ls_number_reflns 2658 _refine_ls_number_parameters 229 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs 0.0776 _refine_ls_wR_factor_obs 0.1807 _refine_ls_goodness_of_fit_obs 1.146 _refine_ls_restrained_S_obs 1.146 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.83317(9) 0.87191(5) 0.00156(11) 0.0326(3) Uani 1 1 d . . . Cd2 Cd 0.45748(11) 0.81575(6) 0.12199(11) 0.0451(4) Uani 1 1 d . . . Cd3 Cd 0.71253(11) 0.92696(5) -0.38067(11) 0.0405(4) Uani 1 1 d . . . N1 N 0.6803(11) 0.8458(7) 0.0443(13) 0.050(5) Uani 1 1 d . . . C1 C 0.6090(16) 0.8335(7) 0.0727(14) 0.042(5) Uani 1 1 d . . . N2 N 0.8970(13) 0.8535(7) 0.1564(12) 0.052(5) Uani 1 1 d . . . C2 C 0.9189(14) 0.8411(7) 0.2296(13) 0.041(5) Uani 1 1 d . . . N3 N 0.9875(12) 0.8976(7) -0.0536(12) 0.047(4) Uani 1 1 d . . . C3 C 1.0642(15) 0.9037(8) -0.0757(15) 0.043(5) Uani 1 1 d . . . N4 N 0.7723(13) 0.9005(7) -0.1494(12) 0.057(5) Uani 1 1 d . . . C4 C 0.7493(15) 0.9106(7) -0.2244(15) 0.042(5) Uani 1 1 d . . . N5 N 0.3722(16) 0.8705(7) 0.0224(14) 0.065(6) Uani 1 1 d . . . C5 C 0.3208(15) 0.8920(8) -0.0226(16) 0.048(6) Uani 1 1 d . . . N6 N 0.8054(14) 0.9536(8) 0.0592(14) 0.063(5) Uani 1 1 d . . . C6 C 0.7946(15) 0.9929(8) 0.0837(14) 0.042(5) Uani 1 1 d . . . N7 N 0.8679(13) 0.7936(7) -0.0545(13) 0.051(5) Uani 1 1 d . . . C7 C 0.8981(15) 0.7570(7) -0.0792(17) 0.046(5) Uani 1 1 d . . . N101 N 0.5566(13) 0.9841(7) 0.2454(13) 0.059(5) Uani 1 1 d . . . C101 C 0.5776(18) 0.9489(9) 0.178(2) 0.066(7) Uani 1 1 d . . . H101 H 0.6082 0.9200 0.1983 0.080 Uiso 1 1 calc R . . C102 C 0.5548(19) 0.9551(7) 0.0822(17) 0.059(6) Uani 1 1 d . . . H102 H 0.5687 0.9301 0.0375 0.070 Uiso 1 1 calc R . . C103 C 0.5128(15) 0.9966(8) 0.0519(14) 0.044(5) Uani 1 1 d . . . C104 C 0.493(2) 1.0322(10) 0.1200(17) 0.095(11) Uani 1 1 d . . . H104 H 0.4582 1.0600 0.1001 0.114 Uiso 1 1 calc R . . C105 C 0.521(2) 1.0291(11) 0.2179(17) 0.085(9) Uani 1 1 d . . . H105 H 0.5166 1.0557 0.2609 0.102 Uiso 1 1 calc R . . C111 C 0.576(3) 0.9778(12) 0.3567(19) 0.106(12) Uani 1 1 d . . . H111 H 0.5895 0.9436 0.3707 0.159 Uiso 1 1 calc R . . H121 H 0.5200 0.9882 0.3929 0.159 Uiso 1 1 calc R . . H131 H 0.6307 0.9977 0.3753 0.159 Uiso 1 1 calc R . . N201 N 0.672(2) 0.8589(12) 0.321(2) 0.131(11) Uiso 1 1 d . . . C201 C 0.657(3) 0.8266(14) 0.371(3) 0.112(11) Uiso 1 1 d . . . C202 C 0.623(4) 0.779(2) 0.424(4) 0.21(2) Uiso 1 1 d . . . H212 H 0.6313 0.7832 0.4935 0.309 Uiso 1 1 calc R . . H222 H 0.6614 0.7516 0.4023 0.309 Uiso 1 1 calc R . . H232 H 0.5561 0.7731 0.4099 0.309 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 0.0299(6) 0.0371(6) 0.0309(6) 0.0022(6) -0.0004(6) 0.0007(6) Cd2 0.0411(8) 0.0546(9) 0.0397(8) -0.0130(7) 0.0089(8) -0.0135(7) Cd3 0.0379(8) 0.0439(8) 0.0397(7) 0.0066(7) -0.0102(7) -0.0016(7) N1 0.018(9) 0.073(13) 0.059(11) 0.004(10) 0.015(8) -0.006(8) C1 0.051(13) 0.044(11) 0.031(10) -0.021(9) 0.007(10) 0.006(10) N2 0.058(12) 0.062(11) 0.035(9) -0.001(9) -0.006(9) 0.005(10) C2 0.037(11) 0.059(13) 0.026(11) 0.012(9) 0.003(9) -0.004(10) N3 0.030(10) 0.070(12) 0.042(10) 0.009(9) 0.002(8) -0.001(9) C3 0.036(12) 0.052(13) 0.041(11) 0.001(10) -0.009(10) 0.009(10) N4 0.052(12) 0.079(13) 0.038(10) 0.016(10) -0.016(9) 0.007(11) C4 0.045(12) 0.035(10) 0.047(13) 0.004(9) -0.008(10) -0.001(9) N5 0.068(14) 0.063(13) 0.065(14) 0.009(11) -0.001(11) -0.011(11) C5 0.035(12) 0.056(13) 0.054(14) 0.015(10) -0.004(10) 0.010(10) N6 0.058(13) 0.062(13) 0.070(13) -0.009(11) 0.021(10) -0.003(10) C6 0.040(11) 0.051(13) 0.036(10) -0.001(10) 0.008(9) 0.009(11) N7 0.048(11) 0.046(10) 0.058(11) -0.013(9) -0.012(9) 0.005(9) C7 0.044(13) 0.032(11) 0.064(14) -0.003(10) -0.015(11) 0.003(10) N101 0.051(12) 0.080(13) 0.045(10) 0.031(11) 0.010(10) 0.008(10) C101 0.055(15) 0.052(14) 0.09(2) -0.012(14) -0.018(14) 0.014(13) C102 0.082(18) 0.022(10) 0.071(15) -0.009(10) -0.022(14) 0.011(11) C103 0.046(13) 0.036(10) 0.051(11) -0.005(11) 0.009(10) 0.002(10) C104 0.15(3) 0.096(19) 0.040(13) -0.004(15) -0.008(16) 0.08(2) C105 0.11(2) 0.10(2) 0.051(15) -0.026(15) 0.001(15) 0.052(19) C111 0.14(3) 0.13(3) 0.046(16) -0.002(16) 0.009(17) 0.02(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 N7 2.299(17) . ? Cd1 N1 2.299(16) . ? Cd1 N2 2.345(17) . ? Cd1 N4 2.358(16) . ? Cd1 N3 2.362(17) . ? Cd1 N6 2.37(2) . ? Cd2 C7 2.21(2) 4_465 ? Cd2 C2 2.206(18) 6_556 ? Cd2 C1 2.25(2) . ? Cd2 N5 2.33(2) . ? Cd3 C5 2.21(2) 6_655 ? Cd3 C6 2.22(2) 2_674 ? Cd3 C3 2.22(2) 6 ? Cd3 C4 2.24(2) . ? N1 C1 1.11(2) . ? N2 C2 1.10(2) . ? C2 Cd2 2.206(18) 6_656 ? N3 C3 1.11(2) . ? C3 Cd3 2.22(2) 6_655 ? N4 C4 1.11(2) . ? N5 C5 1.10(3) . ? C5 Cd3 2.21(2) 6 ? N6 C6 1.12(3) . ? C6 Cd3 2.22(2) 2_675 ? N7 C7 1.12(2) . ? C7 Cd2 2.21(2) 4_565 ? N101 C101 1.35(3) . ? N101 C105 1.36(3) . ? N101 C111 1.55(3) . ? C101 C102 1.36(3) . ? C102 C103 1.33(3) . ? C103 C104 1.37(3) . ? C103 C103 1.47(4) 5_675 ? C104 C105 1.40(3) . ? N201 C201 1.13(4) . ? C201 C202 1.54(6) . ? 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 N7 Cd1 N1 89.6(7) . . ? N7 Cd1 N2 91.6(6) . . ? N1 Cd1 N2 92.9(6) . . ? N7 Cd1 N4 94.8(7) . . ? N1 Cd1 N4 89.8(6) . . ? N2 Cd1 N4 173.1(6) . . ? N7 Cd1 N3 88.6(6) . . ? N1 Cd1 N3 176.1(6) . . ? N2 Cd1 N3 90.7(6) . . ? N4 Cd1 N3 86.9(6) . . ? N7 Cd1 N6 177.3(7) . . ? N1 Cd1 N6 93.0(6) . . ? N2 Cd1 N6 87.6(7) . . ? N4 Cd1 N6 85.9(7) . . ? N3 Cd1 N6 88.8(6) . . ? C7 Cd2 C2 115.5(8) 4_465 6_556 ? C7 Cd2 C1 117.1(7) 4_465 . ? C2 Cd2 C1 115.7(7) 6_556 . ? C7 Cd2 N5 102.8(8) 4_465 . ? C2 Cd2 N5 102.6(7) 6_556 . ? C1 Cd2 N5 99.1(7) . . ? C5 Cd3 C6 108.4(8) 6_655 2_674 ? C5 Cd3 C3 110.0(7) 6_655 6 ? C6 Cd3 C3 100.1(8) 2_674 6 ? C5 Cd3 C4 109.5(8) 6_655 . ? C6 Cd3 C4 114.3(7) 2_674 . ? C3 Cd3 C4 114.2(7) 6 . ? C1 N1 Cd1 174.2(18) . . ? N1 C1 Cd2 174(2) . . ? C2 N2 Cd1 172.2(18) . . ? N2 C2 Cd2 177.9(19) . 6_656 ? C3 N3 Cd1 170.8(18) . . ? N3 C3 Cd3 172(2) . 6_655 ? C4 N4 Cd1 173.2(19) . . ? N4 C4 Cd3 175(2) . . ? C5 N5 Cd2 170(2) . . ? N5 C5 Cd3 173(2) . 6 ? C6 N6 Cd1 177.2(19) . . ? N6 C6 Cd3 173.1(19) . 2_675 ? C7 N7 Cd1 170.2(18) . . ? N7 C7 Cd2 178(2) . 4_565 ? C101 N101 C105 121(2) . . ? C101 N101 C111 123(2) . . ? C105 N101 C111 115(2) . . ? N101 C101 C102 121(2) . . ? C103 C102 C101 120(2) . . ? C102 C103 C104 118(2) . . ? C102 C103 C103 121(2) . 5_675 ? C104 C103 C103 121(2) . 5_675 ? C103 C104 C105 124(2) . . ? N101 C105 C104 115(2) . . ? N201 C201 C202 170(5) . . ? 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 C102 C103 C103 C102 180.0 . . 5_675 5_675 ? _refine_diff_density_max 1.565 _refine_diff_density_min -1.083 _refine_diff_density_rms 0.202 #===END data_IIa-3 _database_code_CSD 175543 _audit_creation_method SHELXL-97 _chemical_formula_structural 'Cd6 (C14 N14)(C12 N2 H14)(C3 O1 H8)2(O1 H2)3' _chemical_formula_sum 'C32 H36 Cd6 N16 O5' _chemical_formula_weight 1399.21 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' 'Cd' 'Cd' -0.8075 1.2024 '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 orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.724(4) _cell_length_b 27.269(6) _cell_length_c 13.569(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5078.2(27) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _exptl_crystal_description platlet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 1.81 _exptl_crystal_density_diffrn 1.83 _exptl_crystal_density_method 'floating method' _exptl_crystal_F_000 2672 _exptl_absorpt_coefficient_mu 2.500 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC5S' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 3% _diffrn_reflns_number 8150 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 30.06 _reflns_number_total 7409 _reflns_number_observed 3516 _reflns_observed_criterion >3sigma(F) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for windows' _refine_special_details ; Weighted R-factors wR and all goodnesses 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 observed criterion of F > 3sigma(F) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. The atomic positions of the guest molecule 2-propanol could not be determined because of a static and/or dynamic disorder of the guest molecule. The atoms of the 2-propanol molecule were not included in the calculation. ; _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^)+(0.1036P)^2^+36.7402P] 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 noref _refine_ls_extinction_method none _refine_ls_number_reflns 3516 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs 0.0745 _refine_ls_wR_factor_obs 0.1956 _refine_ls_goodness_of_fit_obs 1.158 _refine_ls_restrained_S_obs 1.158 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.83199(7) 0.87444(4) 0.00371(7) 0.0393(3) Uani 1 1 d . . . Cd2 Cd 0.46256(9) 0.80856(4) 0.12792(8) 0.0515(3) Uani 1 1 d . . . Cd3 Cd 0.71595(8) 0.92447(4) -0.38434(7) 0.0439(3) Uani 1 1 d . . . N1 N 0.6790(9) 0.8509(5) 0.0490(11) 0.060(4) Uani 1 1 d . . . C1 C 0.6064(11) 0.8344(6) 0.0739(11) 0.050(4) Uani 1 1 d . . . N2 N 0.8920(11) 0.8588(6) 0.1619(10) 0.066(4) Uani 1 1 d . . . C2 C 0.9154(13) 0.8434(6) 0.2340(12) 0.060(4) Uani 1 1 d . . . N3 N 0.9886(9) 0.8978(5) -0.0500(9) 0.052(3) Uani 1 1 d . . . C3 C 1.0654(11) 0.9038(5) -0.0752(11) 0.047(4) Uani 1 1 d . . . N4 N 0.7738(11) 0.9020(6) -0.1517(10) 0.066(4) Uani 1 1 d . . . C4 C 0.7514(12) 0.9121(6) -0.2275(11) 0.053(4) Uani 1 1 d . . . N5 N 0.3740(12) 0.8648(6) 0.0273(12) 0.077(5) Uani 1 1 d . . . C5 C 0.3224(12) 0.8861(6) -0.0205(11) 0.055(4) Uani 1 1 d . . . N6 N 0.8021(11) 0.9557(5) 0.0616(10) 0.060(4) Uani 1 1 d . . . C6 C 0.7899(12) 0.9949(6) 0.0839(12) 0.054(4) Uani 1 1 d . . . N7 N 0.8694(10) 0.7962(5) -0.0486(12) 0.063(4) Uani 1 1 d . . . C7 C 0.8995(11) 0.7605(6) -0.0738(12) 0.052(4) Uani 1 1 d . . . N101 N 0.5497(11) 0.9848(6) 0.2491(10) 0.062(4) Uani 1 1 d . . . C101 C 0.5676(16) 0.9484(7) 0.1871(13) 0.073(5) Uani 1 1 d . . . H101 H 0.5934 0.9189 0.2095 0.087 Uiso 1 1 calc R . . C102 C 0.5475(16) 0.9551(7) 0.0900(14) 0.078(6) Uani 1 1 d . . . H102 H 0.5597 0.9294 0.0467 0.093 Uiso 1 1 calc R . . C103 C 0.5116(10) 0.9961(5) 0.0539(11) 0.043(3) Uani 1 1 d . . . C104 C 0.494(2) 1.0328(8) 0.1208(15) 0.099(8) Uani 1 1 d . . . H104 H 0.4675 1.0622 0.0989 0.118 Uiso 1 1 calc R . . C105 C 0.515(2) 1.0276(8) 0.2183(13) 0.112(10) Uani 1 1 d . . . H105 H 0.5059 1.0534 0.2621 0.134 Uiso 1 1 calc R . . C111 C 0.5756(19) 0.9780(9) 0.3550(14) 0.092(7) Uani 1 1 d . . . H111 H 0.5603 0.9451 0.3748 0.138 Uiso 1 1 calc R . . H121 H 0.5391 1.0008 0.3944 0.138 Uiso 1 1 calc R . . H131 H 0.6440 0.9839 0.3639 0.138 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 0.0435(5) 0.0393(5) 0.0351(5) 0.0012(4) -0.0004(4) -0.0004(4) Cd2 0.0562(7) 0.0500(6) 0.0482(6) -0.0107(5) 0.0119(5) -0.0109(5) Cd3 0.0481(6) 0.0452(5) 0.0383(5) 0.0037(5) -0.0088(5) 0.0008(5) N1 0.040(7) 0.063(9) 0.075(9) 0.008(7) 0.023(7) -0.006(6) C1 0.051(9) 0.050(9) 0.048(8) -0.003(7) -0.001(7) 0.017(7) N2 0.073(9) 0.082(11) 0.043(7) 0.012(7) -0.008(7) -0.010(8) C2 0.066(11) 0.060(10) 0.055(10) 0.009(8) -0.012(8) -0.004(9) N3 0.048(7) 0.062(8) 0.046(7) 0.000(6) 0.005(6) -0.004(6) C3 0.041(8) 0.048(9) 0.053(9) 0.003(7) 0.014(7) -0.006(6) N4 0.075(10) 0.074(10) 0.049(7) -0.010(7) -0.016(7) 0.012(8) C4 0.064(10) 0.057(10) 0.040(8) 0.008(7) -0.010(7) 0.011(8) N5 0.075(10) 0.077(11) 0.078(10) 0.019(9) -0.014(9) 0.007(9) C5 0.059(10) 0.061(10) 0.046(9) 0.000(7) 0.005(7) -0.005(8) N6 0.081(10) 0.040(7) 0.060(8) 0.000(6) 0.015(8) -0.007(7) C6 0.052(9) 0.050(9) 0.059(9) -0.011(8) 0.008(8) -0.007(8) N7 0.064(9) 0.048(8) 0.078(10) -0.009(7) 0.001(8) 0.018(7) C7 0.048(8) 0.051(10) 0.057(9) 0.002(8) 0.001(7) 0.004(7) N101 0.070(9) 0.075(9) 0.040(7) 0.010(7) 0.005(7) -0.005(8) C101 0.103(15) 0.065(11) 0.050(10) -0.004(9) -0.028(10) 0.012(11) C102 0.100(15) 0.059(11) 0.074(12) -0.011(9) -0.037(11) 0.026(11) C103 0.042(8) 0.040(8) 0.048(8) -0.003(6) 0.007(6) 0.002(6) C104 0.16(2) 0.074(13) 0.064(12) 0.007(11) 0.017(14) 0.057(14) C105 0.23(3) 0.073(14) 0.037(9) 0.014(9) 0.017(14) 0.048(17) C111 0.122(19) 0.105(18) 0.050(10) 0.001(11) 0.005(11) 0.008(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 N1 2.280(12) . ? Cd1 N7 2.306(13) . ? Cd1 N2 2.338(14) . ? Cd1 N3 2.357(13) . ? Cd1 N4 2.377(14) . ? Cd1 N6 2.387(14) . ? Cd2 C7 2.199(16) 4_465 ? Cd2 C2 2.199(16) 6_556 ? Cd2 C1 2.220(17) . ? Cd2 N5 2.386(16) . ? Cd3 C4 2.209(14) . ? Cd3 C3 2.211(14) 6 ? Cd3 C5 2.212(18) 6_655 ? Cd3 C6 2.241(16) 2_674 ? N1 C1 1.144(19) . ? N2 C2 1.111(19) . ? C2 Cd2 2.199(16) 6_656 ? N3 C3 1.120(18) . ? C3 Cd3 2.211(14) 6_655 ? N4 C4 1.109(18) . ? N5 C5 1.12(2) . ? C5 Cd3 2.212(18) 6 ? N6 C6 1.124(19) . ? C6 Cd3 2.241(16) 2_675 ? N7 C7 1.112(19) . ? C7 Cd2 2.199(16) 4_565 ? N101 C101 1.33(2) . ? N101 C105 1.33(2) . ? N101 C111 1.49(2) . ? C101 C102 1.36(2) . ? C102 C103 1.32(2) . ? C103 C104 1.37(2) . ? C103 C103 1.51(3) 5_675 ? C104 C105 1.36(3) . ? 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 Cd1 N7 91.5(5) . . ? N1 Cd1 N2 91.5(5) . . ? N7 Cd1 N2 92.0(6) . . ? N1 Cd1 N3 177.6(5) . . ? N7 Cd1 N3 87.2(5) . . ? N2 Cd1 N3 90.7(5) . . ? N1 Cd1 N4 91.1(5) . . ? N7 Cd1 N4 95.4(5) . . ? N2 Cd1 N4 172.1(5) . . ? N3 Cd1 N4 86.9(5) . . ? N1 Cd1 N6 90.9(5) . . ? N7 Cd1 N6 176.8(5) . . ? N2 Cd1 N6 85.9(5) . . ? N3 Cd1 N6 90.4(5) . . ? N4 Cd1 N6 86.6(5) . . ? C7 Cd2 C2 122.6(6) 4_465 6_556 ? C7 Cd2 C1 120.7(6) 4_465 . ? C2 Cd2 C1 113.9(6) 6_556 . ? C7 Cd2 N5 99.1(6) 4_465 . ? C2 Cd2 N5 93.5(6) 6_556 . ? C1 Cd2 N5 93.4(6) . . ? C4 Cd3 C3 113.9(6) . 6 ? C4 Cd3 C5 110.1(6) . 6_655 ? C3 Cd3 C5 110.6(6) 6 6_655 ? C4 Cd3 C6 110.1(6) . 2_674 ? C3 Cd3 C6 99.7(6) 6 2_674 ? C5 Cd3 C6 112.0(6) 6_655 2_674 ? C1 N1 Cd1 172.9(13) . . ? N1 C1 Cd2 175.1(14) . . ? C2 N2 Cd1 168.1(16) . . ? N2 C2 Cd2 176.4(17) . 6_656 ? C3 N3 Cd1 172.7(13) . . ? N3 C3 Cd3 173.0(14) . 6_655 ? C4 N4 Cd1 174.4(15) . . ? N4 C4 Cd3 173.3(15) . . ? C5 N5 Cd2 170.0(16) . . ? N5 C5 Cd3 176.9(16) . 6 ? C6 N6 Cd1 176.1(14) . . ? N6 C6 Cd3 172.0(14) . 2_675 ? C7 N7 Cd1 171.0(15) . . ? N7 C7 Cd2 177.7(16) . 4_565 ? C101 N101 C105 121.7(15) . . ? C101 N101 C111 118.4(16) . . ? C105 N101 C111 119.8(17) . . ? N101 C101 C102 118.5(17) . . ? C103 C102 C101 123.4(18) . . ? C102 C103 C104 116.0(16) . . ? C102 C103 C103 123.8(17) . 5_675 ? C104 C103 C103 120.1(17) . 5_675 ? C105 C104 C103 122.0(18) . . ? N101 C105 C104 118.3(19) . . ? 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 C102 C103 C103 C102 180.0 . . 5_665 5_665 ? _refine_diff_density_max 1.754 _refine_diff_density_min -1.684 _refine_diff_density_rms 0.230 #===END data_IIb-1 _database_code_CSD 175544 _audit_creation_method SHELXL-97 _chemical_formula_structural 'Cd6 (C14 N14)(O1 H2)2(C12 N2 H14)(C4 O1 H10)2' _chemical_formula_sum 'C34 H38 Cd6 N16 O4' _chemical_formula_weight 1409.25 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' 'Cd' 'Cd' -0.8075 1.2024 '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 orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.718(7) _cell_length_b 27.232(5) _cell_length_c 13.639(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5095.2(32) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _exptl_crystal_description platlet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 1.83 _exptl_crystal_density_diffrn 1.84 _exptl_crystal_density_method 'floating method' _exptl_crystal_F_000 2696 _exptl_absorpt_coefficient_mu 2.491 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC5S' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 3% _diffrn_reflns_number 8164 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 29.98 _reflns_number_total 7422 _reflns_number_observed 3443 _reflns_observed_criterion >3sigma(F) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for windows' _refine_special_details ; Weighted R-factors wR and all goodnesses 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 observed criterion of F > 3sigma(F) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. The atomic positions of the guest molecule diethyl ether could not be determined because of a static and/or dynamic disorder of the guest molecule. The atoms of the diethyl ether molecule were not included in the calculation. ; _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^)+(0.0873P)^2^+20.6225P] 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 noref _refine_ls_extinction_method none _refine_ls_number_reflns 3443 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs 0.0702 _refine_ls_wR_factor_obs 0.1770 _refine_ls_goodness_of_fit_obs 1.170 _refine_ls_restrained_S_obs 1.170 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.83374(7) 0.87367(4) -0.00401(7) 0.0291(2) Uani 1 1 d . . . Cd2 Cd 0.47048(8) 0.80752(4) 0.13743(8) 0.0367(3) Uani 1 1 d . . . Cd3 Cd 0.72245(8) 0.92530(4) -0.39199(7) 0.0330(3) Uani 1 1 d . . . N1 N 0.6803(9) 0.8498(5) 0.0429(10) 0.044(3) Uani 1 1 d . . . C1 C 0.6103(11) 0.8349(6) 0.0751(11) 0.039(4) Uani 1 1 d . . . N2 N 0.8942(10) 0.8581(5) 0.1538(9) 0.047(3) Uani 1 1 d . . . C2 C 0.9201(11) 0.8417(7) 0.2245(11) 0.045(4) Uani 1 1 d . . . N3 N 0.9908(10) 0.8982(5) -0.0518(10) 0.044(3) Uani 1 1 d . . . C3 C 1.0698(12) 0.9045(5) -0.0725(10) 0.035(3) Uani 1 1 d . . . N4 N 0.7792(12) 0.9014(5) -0.1590(10) 0.055(4) Uani 1 1 d . . . C4 C 0.7571(12) 0.9107(6) -0.2346(11) 0.040(4) Uani 1 1 d . . . N5 N 0.3771(10) 0.8669(5) 0.0374(10) 0.049(3) Uani 1 1 d . . . C5 C 0.3277(12) 0.8876(6) -0.0100(11) 0.041(4) Uani 1 1 d . . . N6 N 0.8001(10) 0.9553(5) 0.0500(10) 0.047(3) Uani 1 1 d . . . C6 C 0.7881(12) 0.9940(6) 0.0736(11) 0.042(4) Uani 1 1 d . . . N7 N 0.8711(10) 0.7949(5) -0.0553(10) 0.049(4) Uani 1 1 d . . . C7 C 0.9024(11) 0.7607(6) -0.0829(10) 0.035(3) Uani 1 1 d . . . O1 O 0.5854(15) 0.7516(6) 0.2528(13) 0.108(6) Uani 1 1 d . . . N101 N 0.5457(12) 0.9841(6) 0.2489(11) 0.059(4) Uani 1 1 d . . . C101 C 0.5664(16) 0.9487(7) 0.1856(13) 0.061(5) Uani 1 1 d . . . H101 H 0.5925 0.9194 0.2087 0.073 Uiso 1 1 calc R . . C102 C 0.5503(14) 0.9541(6) 0.0864(12) 0.053(5) Uani 1 1 d . . . H102 H 0.5682 0.9294 0.0430 0.064 Uiso 1 1 calc R . . C103 C 0.5082(12) 0.9959(5) 0.0529(10) 0.037(3) Uani 1 1 d . . . C104 C 0.488(2) 1.0334(8) 0.1196(15) 0.098(9) Uani 1 1 d . . . H104 H 0.4599 1.0625 0.0977 0.117 Uiso 1 1 calc R . . C105 C 0.508(2) 1.0276(9) 0.2160(16) 0.108(11) Uani 1 1 d . . . H105 H 0.4966 1.0531 0.2598 0.130 Uiso 1 1 calc R . . C111 C 0.5646(17) 0.9770(8) 0.3572(14) 0.076(6) Uani 1 1 d . . . H111 H 0.5179 0.9543 0.3836 0.114 Uiso 1 1 calc R . . H121 H 0.5588 1.0080 0.3903 0.114 Uiso 1 1 calc R . . H131 H 0.6292 0.9642 0.3665 0.114 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 0.0297(5) 0.0304(5) 0.0273(4) 0.0006(4) 0.0005(4) 0.0007(5) Cd2 0.0374(6) 0.0364(6) 0.0361(5) -0.0083(5) 0.0083(5) -0.0074(5) Cd3 0.0334(5) 0.0338(5) 0.0319(5) 0.0036(5) -0.0045(4) 0.0013(5) N1 0.032(7) 0.039(8) 0.061(9) -0.002(7) 0.014(6) -0.002(6) C1 0.038(8) 0.037(9) 0.042(8) 0.003(7) 0.001(7) 0.007(7) N2 0.058(9) 0.054(9) 0.031(7) 0.005(6) -0.004(6) 0.009(7) C2 0.038(9) 0.062(11) 0.034(8) 0.000(7) -0.006(7) 0.001(9) N3 0.035(8) 0.045(8) 0.052(8) 0.004(6) 0.011(6) -0.003(6) C3 0.041(9) 0.032(8) 0.033(7) 0.002(6) -0.006(7) 0.005(7) N4 0.078(11) 0.048(9) 0.039(8) 0.008(6) -0.017(8) 0.004(8) C4 0.048(9) 0.041(9) 0.030(8) 0.005(6) -0.002(7) 0.009(7) N5 0.052(9) 0.048(9) 0.045(7) 0.006(7) -0.006(7) 0.001(7) C5 0.048(9) 0.037(8) 0.038(8) -0.001(7) 0.001(8) -0.001(7) N6 0.049(8) 0.034(8) 0.057(9) 0.000(7) 0.008(7) -0.006(6) C6 0.052(10) 0.041(9) 0.034(8) 0.006(7) 0.006(7) -0.002(8) N7 0.047(8) 0.048(9) 0.052(8) -0.011(7) 0.000(7) 0.002(7) C7 0.033(8) 0.034(9) 0.038(8) -0.005(6) 0.004(6) 0.005(6) O1 0.155(18) 0.068(10) 0.100(12) -0.002(10) -0.041(12) -0.009(12) N101 0.066(11) 0.061(10) 0.048(8) 0.005(8) 0.008(8) -0.007(9) C101 0.088(14) 0.046(11) 0.049(10) -0.008(9) -0.027(10) 0.023(10) C102 0.067(12) 0.042(10) 0.051(10) -0.008(8) -0.004(9) 0.014(9) C103 0.046(9) 0.028(8) 0.039(8) -0.001(6) 0.006(7) 0.007(7) C104 0.17(3) 0.068(15) 0.053(12) -0.004(10) 0.010(15) 0.062(17) C105 0.20(3) 0.077(17) 0.052(12) 0.010(11) 0.033(16) 0.053(18) C111 0.085(16) 0.094(17) 0.050(11) 0.010(11) -0.010(11) -0.005(14) _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 N1 2.294(12) . ? Cd1 N7 2.313(14) . ? Cd1 N2 2.346(13) . ? Cd1 N3 2.348(13) . ? Cd1 N4 2.366(13) . ? Cd1 N6 2.387(14) . ? Cd2 C7 2.209(15) 4_465 ? Cd2 C2 2.210(16) 6_556 ? Cd2 C1 2.226(16) . ? Cd2 N5 2.474(14) . ? Cd2 O1 2.699(17) . ? Cd3 C5 2.219(17) 6_655 ? Cd3 C3 2.223(17) 6 ? Cd3 C4 2.234(14) . ? Cd3 C6 2.253(17) 2_674 ? N1 C1 1.131(18) . ? N2 C2 1.121(18) . ? C2 Cd2 2.210(16) 6_656 ? N3 C3 1.133(18) . ? C3 Cd3 2.223(17) 6_655 ? N4 C4 1.104(18) . ? N5 C5 1.09(2) . ? C5 Cd3 2.219(17) 6 ? N6 C6 1.11(2) . ? C6 Cd3 2.253(17) 2_675 ? N7 C7 1.093(18) . ? C7 Cd2 2.209(15) 4_565 ? N101 C101 1.32(2) . ? N101 C105 1.37(3) . ? N101 C111 1.51(2) . ? C101 C102 1.38(2) . ? C102 C103 1.35(2) . ? C103 C104 1.40(2) . ? C103 C103 1.48(3) 5_675 ? C104 C105 1.35(3) . ? 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 Cd1 N7 91.4(5) . . ? N1 Cd1 N2 91.0(5) . . ? N7 Cd1 N2 91.8(5) . . ? N1 Cd1 N3 179.9(6) . . ? N7 Cd1 N3 88.7(5) . . ? N2 Cd1 N3 88.9(5) . . ? N1 Cd1 N4 92.8(5) . . ? N7 Cd1 N4 95.5(5) . . ? N2 Cd1 N4 171.7(5) . . ? N3 Cd1 N4 87.2(5) . . ? N1 Cd1 N6 90.0(5) . . ? N7 Cd1 N6 178.3(5) . . ? N2 Cd1 N6 87.3(5) . . ? N3 Cd1 N6 89.9(5) . . ? N4 Cd1 N6 85.3(5) . . ? C7 Cd2 C2 120.5(6) 4_465 6_556 ? C7 Cd2 C1 121.2(6) 4_465 . ? C2 Cd2 C1 117.0(6) 6_556 . ? C7 Cd2 N5 98.4(5) 4_465 . ? C2 Cd2 N5 91.9(5) 6_556 . ? C1 Cd2 N5 91.0(5) . . ? C7 Cd2 O1 88.2(5) 4_465 . ? C2 Cd2 O1 85.6(6) 6_556 . ? C1 Cd2 O1 84.7(6) . . ? N5 Cd2 O1 173.4(5) . . ? C5 Cd3 C3 111.4(5) 6_655 6 ? C5 Cd3 C4 111.0(6) 6_655 . ? C3 Cd3 C4 111.4(6) 6 . ? C5 Cd3 C6 111.5(6) 6_655 2_674 ? C3 Cd3 C6 98.2(6) 6 2_674 ? C4 Cd3 C6 112.8(5) . 2_674 ? C1 N1 Cd1 171.4(14) . . ? N1 C1 Cd2 178.4(14) . . ? C2 N2 Cd1 166.8(15) . . ? N2 C2 Cd2 178.7(16) . 6_656 ? C3 N3 Cd1 171.9(13) . . ? N3 C3 Cd3 173.8(14) . 6_655 ? C4 N4 Cd1 173.9(15) . . ? N4 C4 Cd3 175.1(15) . . ? C5 N5 Cd2 169.9(14) . . ? N5 C5 Cd3 176.4(15) . 6 ? C6 N6 Cd1 177.0(14) . . ? N6 C6 Cd3 173.1(14) . 2_675 ? C7 N7 Cd1 169.0(14) . . ? N7 C7 Cd2 178.1(14) . 4_565 ? C101 N101 C105 119.8(16) . . ? C101 N101 C111 120.5(17) . . ? C105 N101 C111 119.7(17) . . ? N101 C101 C102 121.9(17) . . ? C103 C102 C101 119.3(16) . . ? C102 C103 C104 118.6(15) . . ? C102 C103 C103 121.4(17) . 5_675 ? C104 C103 C103 119.7(18) . 5_675 ? C105 C104 C103 120.5(19) . . ? C104 C105 N101 120(2) . . ? 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 C102 C103 C103 C102 180.0 . . 5_665 5_665 ? _refine_diff_density_max 2.059 _refine_diff_density_min -0.944 _refine_diff_density_rms 0.234 #===END data_IIb-2 _database_code_CSD 175545 _audit_creation_method SHELXL-97 _chemical_formula_structural 'Cd6 (C14 N14)(O1 H2)2(C12 N2 H14)(C2 O1 H6)2(O1 H2)3' _chemical_formula_sum 'C30 H36 Cd6 N16 O7' _chemical_formula_weight 1407.19 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' 'Cd' 'Cd' -0.8075 1.2024 '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 orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.740(6) _cell_length_b 27.030(10) _cell_length_c 13.647(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5068.4(37) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _exptl_crystal_description platlet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 1.79 _exptl_crystal_density_diffrn 1.84 _exptl_crystal_density_method 'floating method' _exptl_crystal_F_000 2688 _exptl_absorpt_coefficient_mu 2.508 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC5S' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 2% _diffrn_reflns_number 8121 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 29.99 _reflns_number_total 7380 _reflns_number_observed 4117 _reflns_observed_criterion >3sigma(F) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for windows' _refine_special_details ; Weighted R-factors wR and all goodnesses 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 observed criterion of F > 3sigma(F) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. The atomic positions of the guest molecule ethanol could not be determined because of a static and/or dynamic disorder of the guest molecule. The atoms of the ethanol molecule were not included in the calculation. ; _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^)+(0.0955P)^2^+19.1330P] 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 noref _refine_ls_extinction_method none _refine_ls_number_reflns 4117 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs 0.0623 _refine_ls_wR_factor_obs 0.1706 _refine_ls_goodness_of_fit_obs 1.130 _refine_ls_restrained_S_obs 1.130 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.83208(5) 0.87481(3) -0.00233(5) 0.03297(18) Uani 1 1 d . . . Cd2 Cd 0.46977(6) 0.80749(3) 0.13680(6) 0.0449(2) Uani 1 1 d . . . Cd3 Cd 0.72078(6) 0.92325(3) -0.39089(5) 0.0383(2) Uani 1 1 d . . . N1 N 0.6807(7) 0.8490(4) 0.0433(8) 0.050(2) Uani 1 1 d . . . C1 C 0.6098(8) 0.8329(5) 0.0746(8) 0.044(3) Uani 1 1 d . . . N2 N 0.8944(8) 0.8566(5) 0.1540(8) 0.059(3) Uani 1 1 d . . . C2 C 0.9215(9) 0.8413(5) 0.2237(9) 0.049(3) Uani 1 1 d . . . N3 N 0.9886(7) 0.8973(4) -0.0520(7) 0.051(3) Uani 1 1 d . . . C3 C 1.0680(8) 0.9031(4) -0.0732(8) 0.043(3) Uani 1 1 d . . . N4 N 0.7759(8) 0.9020(5) -0.1573(7) 0.057(3) Uani 1 1 d . . . C4 C 0.7561(9) 0.9108(5) -0.2342(8) 0.045(3) Uani 1 1 d . . . N5 N 0.3770(8) 0.8667(5) 0.0375(9) 0.064(3) Uani 1 1 d . . . C5 C 0.3262(9) 0.8864(5) -0.0111(9) 0.049(3) Uani 1 1 d . . . N6 N 0.7997(8) 0.9552(4) 0.0546(8) 0.051(3) Uani 1 1 d . . . C6 C 0.7876(9) 0.9955(5) 0.0762(9) 0.047(3) Uani 1 1 d . . . N7 N 0.8688(8) 0.7962(4) -0.0570(8) 0.056(3) Uani 1 1 d . . . C7 C 0.9010(9) 0.7614(5) -0.0830(9) 0.052(3) Uani 1 1 d . . . O1 O 0.5866(12) 0.7509(7) 0.2493(11) 0.139(6) Uani 1 1 d . . . N101 N 0.5464(9) 0.9840(5) 0.2488(8) 0.060(3) Uani 1 1 d . . . C101 C 0.5678(11) 0.9489(6) 0.1882(11) 0.066(4) Uani 1 1 d . . . H101 H 0.5953 0.9198 0.2115 0.080 Uiso 1 1 calc R . . C102 C 0.5500(11) 0.9545(5) 0.0881(9) 0.056(3) Uani 1 1 d . . . H102 H 0.5663 0.9289 0.0458 0.067 Uiso 1 1 calc R . . C103 C 0.5091(9) 0.9968(4) 0.0503(8) 0.044(3) Uani 1 1 d . . . C104 C 0.4892(18) 1.0342(7) 0.1200(11) 0.105(8) Uani 1 1 d . . . H104 H 0.4634 1.0643 0.0996 0.126 Uiso 1 1 calc R . . C105 C 0.508(2) 1.0262(7) 0.2173(11) 0.132(11) Uani 1 1 d . . . H105 H 0.4929 1.0508 0.2624 0.159 Uiso 1 1 calc R . . C111 C 0.5686(14) 0.9778(7) 0.3574(10) 0.081(5) Uani 1 1 d . . . H111 H 0.5872 0.9441 0.3700 0.121 Uiso 1 1 calc R . . H121 H 0.5117 0.9858 0.3950 0.121 Uiso 1 1 calc R . . H131 H 0.6208 0.9995 0.3755 0.121 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 0.0325(3) 0.0345(4) 0.0320(3) 0.0015(3) 0.0000(3) 0.0006(3) Cd2 0.0457(4) 0.0444(5) 0.0446(4) -0.0126(4) 0.0125(4) -0.0120(4) Cd3 0.0371(4) 0.0412(4) 0.0365(4) 0.0047(3) -0.0073(3) 0.0010(3) N1 0.038(5) 0.044(6) 0.067(7) 0.003(5) 0.010(5) -0.002(4) C1 0.044(6) 0.043(7) 0.046(6) -0.003(5) 0.001(5) 0.008(5) N2 0.059(6) 0.072(8) 0.046(6) 0.011(6) -0.007(5) 0.002(6) C2 0.045(6) 0.062(8) 0.041(6) 0.003(6) -0.004(5) 0.005(6) N3 0.038(5) 0.065(7) 0.051(6) 0.006(5) 0.005(4) -0.002(5) C3 0.043(6) 0.045(7) 0.041(5) 0.003(5) -0.003(5) -0.004(5) N4 0.058(6) 0.070(8) 0.043(5) 0.004(5) -0.013(5) 0.007(6) C4 0.048(6) 0.051(7) 0.034(6) 0.002(5) -0.003(5) 0.001(5) N5 0.055(7) 0.070(8) 0.066(7) 0.004(6) -0.009(6) 0.001(6) C5 0.043(6) 0.050(7) 0.055(7) 0.008(6) -0.002(5) -0.001(5) N6 0.062(6) 0.035(6) 0.056(6) -0.010(5) 0.003(5) -0.003(5) C6 0.049(7) 0.047(7) 0.045(6) -0.006(5) 0.011(5) -0.005(6) N7 0.061(6) 0.043(6) 0.063(7) -0.011(5) 0.002(5) 0.021(5) C7 0.047(6) 0.062(9) 0.049(7) -0.012(6) -0.003(5) 0.006(6) O1 0.129(14) 0.167(16) 0.122(12) -0.014(12) -0.024(10) 0.029(12) N101 0.065(7) 0.070(8) 0.043(5) 0.006(6) 0.008(5) 0.008(6) C101 0.071(9) 0.057(9) 0.071(9) 0.001(8) -0.022(7) 0.015(7) C102 0.077(9) 0.040(7) 0.051(7) -0.013(6) -0.011(6) 0.008(6) C103 0.049(6) 0.035(6) 0.048(6) 0.003(5) 0.007(5) 0.010(5) C104 0.18(2) 0.081(12) 0.056(9) -0.005(8) 0.026(11) 0.076(14) C105 0.27(3) 0.090(14) 0.040(7) 0.005(8) 0.034(13) 0.099(17) C111 0.104(13) 0.101(14) 0.037(7) -0.003(8) -0.004(8) 0.010(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 Cd1 N1 2.281(9) . ? Cd1 N7 2.307(10) . ? Cd1 N3 2.335(10) . ? Cd1 N6 2.351(10) . ? Cd1 N2 2.351(11) . ? Cd1 N4 2.368(10) . ? Cd2 C1 2.212(12) . ? Cd2 C2 2.213(12) 6_556 ? Cd2 C7 2.214(14) 4_465 ? Cd2 N5 2.454(12) . ? Cd2 O1 2.697(16) . ? Cd3 C5 2.209(13) 6_655 ? Cd3 C4 2.218(11) . ? Cd3 C3 2.224(12) 6 ? Cd3 C6 2.245(13) 2_674 ? N1 C1 1.149(14) . ? N2 C2 1.102(15) . ? C2 Cd2 2.213(12) 6_656 ? N3 C3 1.140(14) . ? C3 Cd3 2.224(12) 6_655 ? N4 C4 1.110(14) . ? N5 C5 1.100(16) . ? C5 Cd3 2.209(12) 6 ? N6 C6 1.139(15) . ? C6 Cd3 2.245(13) 2_675 ? N7 C7 1.099(15) . ? C7 Cd2 2.214(14) 4_565 ? N101 C101 1.291(18) . ? N101 C105 1.329(19) . ? N101 C111 1.522(17) . ? C101 C102 1.396(19) . ? C102 C103 1.374(17) . ? C103 C103 1.41(2) 5_675 ? C103 C104 1.413(18) . ? C104 C105 1.37(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 N7 90.4(4) . . ? N1 Cd1 N3 177.2(4) . . ? N7 Cd1 N3 86.8(4) . . ? N1 Cd1 N6 91.1(4) . . ? N7 Cd1 N6 178.2(4) . . ? N3 Cd1 N6 91.7(4) . . ? N1 Cd1 N2 91.2(4) . . ? N7 Cd1 N2 91.2(4) . . ? N3 Cd1 N2 89.0(4) . . ? N6 Cd1 N2 87.9(4) . . ? N1 Cd1 N4 92.3(4) . . ? N7 Cd1 N4 93.9(4) . . ? N3 Cd1 N4 87.7(4) . . ? N6 Cd1 N4 87.0(4) . . ? N2 Cd1 N4 173.8(4) . . ? C1 Cd2 C2 117.5(5) . 6_556 ? C1 Cd2 C7 120.4(4) . 4_465 ? C2 Cd2 C7 120.3(5) 6_556 4_465 ? C1 Cd2 N5 92.1(4) . . ? C2 Cd2 N5 92.9(4) 6_556 . ? C7 Cd2 N5 98.3(5) 4_465 . ? C1 Cd2 O1 83.0(5) . . ? C2 Cd2 O1 85.6(5) 6_556 . ? C7 Cd2 O1 88.0(5) 4_465 . ? N5 Cd2 O1 173.4(5) . . ? C5 Cd3 C4 111.8(5) 6_655 . ? C5 Cd3 C3 112.0(4) 6_655 6 ? C4 Cd3 C3 112.4(4) . 6 ? C5 Cd3 C6 110.7(5) 6_655 2_674 ? C4 Cd3 C6 110.6(4) . 2_674 ? C3 Cd3 C6 98.5(4) 6 2_674 ? C1 N1 Cd1 172.0(10) . . ? N1 C1 Cd2 175.9(10) . . ? C2 N2 Cd1 170.0(13) . . ? N2 C2 Cd2 176.9(13) . 6_656 ? C3 N3 Cd1 172.4(11) . . ? N3 C3 Cd3 173.5(11) . 6_655 ? C4 N4 Cd1 172.3(11) . . ? N4 C4 Cd3 175.9(12) . . ? C5 N5 Cd2 167.9(12) . . ? N5 C5 Cd3 177.8(12) . 6 ? C6 N6 Cd1 174.8(10) . . ? N6 C6 Cd3 173.5(11) . 2_675 ? C7 N7 Cd1 168.9(12) . . ? N7 C7 Cd2 178.2(13) . 4_565 ? C101 N101 C105 120.9(12) . . ? C101 N101 C111 119.7(13) . . ? C105 N101 C111 119.3(13) . . ? N101 C101 C102 120.4(13) . . ? C103 C102 C101 121.9(12) . . ? C102 C103 C103 122.7(14) . 5_675 ? C102 C103 C104 114.9(12) . . ? C103 C103 C104 122.4(14) 5_675 . ? C105 C104 C103 120.2(15) . . ? N101 C105 C104 121.5(14) . . ? 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 C102 C103 C103 C102 180.0 . . 5_665 5_665 ? _refine_diff_density_max 2.465 _refine_diff_density_min -0.994 _refine_diff_density_rms 0.216 #===END data_III-1 _database_code_CSD 175546 _audit_creation_method SHELXL-97 _chemical_formula_structural 'Cd5 (C12 N12)(C12 N2 H14)(C6 H6)' _chemical_formula_sum 'C30 H20 Cd5 N14' _chemical_formula_weight 1138.64 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' '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 Icmm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y+1/2, -z' '-x, -y, z' '-x, y+1/2, -z' 'x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1, -z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1, -z+1/2' '-x, -y, -z' '-x, y-1/2, z' 'x, y, -z' 'x, -y-1/2, z' '-x+1/2, -y+1/2, -z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, y+1/2, -z+1/2' 'x+1/2, -y, z+1/2' _cell_length_a 11.1290(5) _cell_length_b 23.6971(11) _cell_length_c 15.7539(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4154.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2480 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 27.48 _exptl_crystal_description platlet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.82 _exptl_crystal_F_000 2152 _exptl_absorpt_coefficient_mu 2.537 _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 'Nonius-CCD' _diffrn_measurement_method \w _diffrn_reflns_number 13340 _diffrn_reflns_av_R_equivalents 0.071 _diffrn_reflns_av_sigmaI/netI 0.0300 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 27.42 _reflns_number_total 2484 _reflns_number_gt 2039 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Denzo/Scalepack' _computing_cell_refinement 'Denzo/Scalepack' _computing_data_reduction 'Denzo/Scalepack' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows' _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. A non-standard crystal axes setting is applied for easy comparison of the crystal structure with the other crystal structures. CN1 is an atom of a bridging cyano group whose center is positioned at an inversion center of the crystal. CN1 was treated as a hybrid atom of 50% carbon and 50% nitrogen. CN2 is an atom of a bridging cyano group whose center is positioned at an inversion center of the crystal. CN2 was treated as a hybrid atom of 50% carbon and 50% nitrogen. ; _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^)+(0.0729P)^2^+58.0052P] 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 noref _refine_ls_extinction_method none _refine_ls_number_reflns 2484 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0761 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1741 _refine_ls_wR_factor_gt 0.1532 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.131 _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_symetry_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 0.0417(3) Uani 1 4 d S . . Cd2 Cd 0.2500 0.13272(3) 0.2500 0.0421(2) Uani 1 2 d S . . Cd3 Cd 0.40165(9) -0.14124(6) 0.0000 0.0743(4) Uani 1 2 d S . . C1 C 0.1483(7) 0.0824(3) 0.1523(5) 0.0472(16) Uani 1 1 d . . . N1 N 0.0957(7) 0.0557(3) 0.1062(4) 0.0559(16) Uani 1 1 d . . . C2 C 0.2413(12) -0.0876(6) 0.0000 0.065(3) Uani 1 2 d S . . N2 N 0.1575(10) -0.0608(5) 0.0000 0.065(3) Uani 1 2 d S . . C3 C 0.4909(11) 0.1347(8) 0.1129(8) 0.112(5) Uani 1 1 d . . . N3 N 0.4317(11) 0.1327(7) 0.1671(8) 0.139(6) Uani 1 1 d . . . CN1 C 0.2500 0.2257(5) 0.2500 0.086(5) Uani 1 2 d S . . CN2 C 0.324(2) -0.2325(8) 0.0000 0.144(10) Uani 1 2 d S . . N101 N 0.7500 0.1017(4) 0.2500 0.067(3) Uani 1 2 d S . . C101 C 0.6684(12) 0.1306(4) 0.2936(7) 0.079(3) Uani 1 1 d . . . H101 H 0.6109 0.1108 0.3244 0.095 Uiso 1 1 calc R . . C102 C 0.6656(10) 0.1883(4) 0.2951(6) 0.069(3) Uani 1 1 d . . . H102 H 0.6072 0.2072 0.3263 0.082 Uiso 1 1 calc R . . C103 C 0.7500 0.2179(4) 0.2500 0.044(2) Uani 1 2 d S . . C111 C 0.7500 0.0409(6) 0.2500 0.174(15) Uani 1 2 d S . . H111 H 0.6730 0.0274 0.2315 0.262 Uiso 0.50 1 calc PR . . H121 H 0.7658 0.0274 0.3064 0.262 Uiso 0.50 1 calc PR . . H131 H 0.8112 0.0274 0.2121 0.262 Uiso 0.50 1 calc PR . . C201 C 0.255(3) 0.2500 0.5000 0.102(8) Uani 1 4 d S . . H201 H 0.1718 0.2500 0.5000 0.122 Uiso 1 4 calc SR . . C202 C 0.315(2) 0.2009(7) 0.5000 0.099(6) Uani 1 2 d S . . H202 H 0.2713 0.1674 0.5000 0.119 Uiso 1 2 calc SR . . C203 C 0.434(2) 0.1988(8) 0.5000 0.103(6) Uani 1 2 d S . . H203 H 0.4731 0.1641 0.5000 0.123 Uiso 1 2 calc SR . . C204 C 0.503(3) 0.2500 0.5000 0.102(9) Uani 1 4 d S . . H204 H 0.5867 0.2500 0.5000 0.123 Uiso 1 4 calc SR . . 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 0.0477(6) 0.0378(5) 0.0395(5) 0.000 0.000 -0.0023(4) Cd2 0.0519(4) 0.0368(4) 0.0376(4) 0.000 -0.0016(3) 0.000 Cd3 0.0471(5) 0.1237(10) 0.0523(6) 0.000 0.000 0.0201(5) C1 0.052(4) 0.043(3) 0.046(4) 0.003(3) -0.005(3) -0.003(3) N1 0.067(4) 0.051(4) 0.049(4) -0.004(3) -0.008(3) -0.008(3) C2 0.051(7) 0.078(9) 0.066(8) 0.000 0.000 -0.006(6) N2 0.058(6) 0.057(6) 0.079(7) 0.000 0.000 0.000(5) C3 0.058(6) 0.217(17) 0.061(7) -0.013(8) -0.001(5) 0.014(8) N3 0.088(7) 0.269(19) 0.061(6) 0.033(8) 0.023(6) -0.008(9) CN1 0.155(15) 0.049(6) 0.055(7) 0.000 -0.025(8) 0.000 CN2 0.20(2) 0.13(2) 0.109(13) 0.000 0.000 0.085(17) N101 0.114(10) 0.037(5) 0.051(6) 0.000 -0.008(6) 0.000 C101 0.112(9) 0.058(6) 0.067(6) 0.002(4) 0.007(6) -0.019(5) C102 0.082(7) 0.055(5) 0.068(6) -0.008(4) 0.022(5) -0.017(4) C103 0.049(5) 0.049(6) 0.033(5) 0.000 -0.001(4) 0.000 C111 0.38(5) 0.024(6) 0.120(17) 0.000 -0.04(2) 0.000 C201 0.12(2) 0.10(2) 0.083(17) 0.000 0.000 0.000 C202 0.127(17) 0.064(10) 0.105(14) 0.000 0.000 -0.009(10) C203 0.132(18) 0.086(12) 0.090(13) 0.000 0.000 0.033(12) C204 0.096(18) 0.17(3) 0.044(11) 0.000 0.000 0.000 _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 2.269(11) . ? Cd1 N2 2.269(11) 9 ? Cd1 N1 2.382(7) 9 ? Cd1 N1 2.382(7) . ? Cd1 N1 2.382(7) 3 ? Cd1 N1 2.382(7) 11 ? Cd2 CN1 2.205(12) . ? Cd2 C1 2.252(7) . ? Cd2 C1 2.252(7) 8_545 ? Cd2 N3 2.407(11) 8_545 ? Cd2 N3 2.407(11) . ? Cd3 C3 2.149(13) 3_655 ? Cd3 C3 2.149(13) 9_655 ? Cd3 C2 2.191(14) . ? Cd3 CN2 2.33(2) . ? C1 N1 1.128(10) . ? C2 N2 1.128(17) . ? C3 N3 1.079(16) . ? C3 Cd3 2.149(13) 9_655 ? CN1 CN1 1.15(2) 13 ? CN2 CN2 0.83(4) 2_545 ? N101 C101 1.328(13) 8_645 ? N101 C101 1.328(13) . ? N101 C111 1.442(16) . ? C101 C102 1.368(13) . ? C102 C103 1.371(10) . ? C103 C102 1.371(10) 8_645 ? C103 C103 1.52(2) 12_565 ? C201 C202 1.34(2) 12_565 ? C201 C202 1.34(2) . ? C202 C203 1.33(3) . ? C203 C204 1.44(3) . ? C204 C203 1.44(3) 12_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 N2 Cd1 N2 180.0 . 9 ? N2 Cd1 N1 89.6(3) . 9 ? N2 Cd1 N1 90.4(3) 9 9 ? N2 Cd1 N1 90.4(3) . . ? N2 Cd1 N1 89.6(3) 9 . ? N1 Cd1 N1 180.0 9 . ? N2 Cd1 N1 89.6(3) . 3 ? N2 Cd1 N1 90.4(3) 9 3 ? N1 Cd1 N1 89.2(3) 9 3 ? N1 Cd1 N1 90.8(3) . 3 ? N2 Cd1 N1 90.4(3) . 11 ? N2 Cd1 N1 89.6(3) 9 11 ? N1 Cd1 N1 90.8(3) 9 11 ? N1 Cd1 N1 89.2(3) . 11 ? N1 Cd1 N1 180.0 3 11 ? CN1 Cd2 C1 121.97(18) . . ? CN1 Cd2 C1 121.97(18) . 8_545 ? C1 Cd2 C1 116.1(4) . 8_545 ? CN1 Cd2 N3 90.0(4) . 8_545 ? C1 Cd2 N3 87.1(4) . 8_545 ? C1 Cd2 N3 92.9(4) 8_545 8_545 ? CN1 Cd2 N3 90.0(4) . . ? C1 Cd2 N3 92.9(4) . . ? C1 Cd2 N3 87.1(4) 8_545 . ? N3 Cd2 N3 180.0 8_545 . ? C3 Cd3 C3 111.7(7) 3_655 9_655 ? C3 Cd3 C2 114.3(4) 3_655 . ? C3 Cd3 C2 114.3(4) 9_655 . ? C3 Cd3 CN2 105.9(6) 3_655 . ? C3 Cd3 CN2 105.9(6) 9_655 . ? C2 Cd3 CN2 103.6(6) . . ? N1 C1 Cd2 176.9(7) . . ? C1 N1 Cd1 174.7(7) . . ? N2 C2 Cd3 178.8(12) . . ? C2 N2 Cd1 174.8(11) . . ? N3 C3 Cd3 176.0(13) . 9_655 ? C3 N3 Cd2 160.3(12) . . ? CN1 CN1 Cd2 180.0 13 . ? CN2 CN2 Cd3 158.2(5) 2_545 . ? C101 N101 C101 118.1(11) 8_645 . ? C101 N101 C111 121.0(5) 8_645 . ? C101 N101 C111 121.0(5) . . ? N101 C101 C102 122.6(10) . . ? C101 C102 C103 119.2(10) . . ? C102 C103 C102 118.4(11) . 8_645 ? C102 C103 C103 120.8(6) . 12_565 ? C102 C103 C103 120.8(6) 8_645 12_565 ? C202 C201 C202 121(3) 12_565 . ? C202 C201 H201 119.6 12_565 . ? C203 C202 C201 122(2) . . ? C202 C203 C204 120.2(19) . . ? C203 C204 C203 115(3) . 12_565 ? _refine_diff_density_max 1.847 _refine_diff_density_min -1.340 _refine_diff_density_rms 0.171 #===END data_III-2 _database_code_CSD 175547 _audit_creation_method SHELXL-97 _chemical_formula_structural 'Cd5 (C12 N12)(C12 N2 H14)(C7 H8)' _chemical_formula_sum 'C31 H22 Cd5 N14' _chemical_formula_weight 1152.67 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 orthorhombic _symmetry_space_group_name_H-M Icmm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y+1/2, -z' '-x, -y, z' '-x, y+1/2, -z' 'x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1, -z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1, -z+1/2' '-x, -y, -z' '-x, y-1/2, z' 'x, y, -z' 'x, -y-1/2, z' '-x+1/2, -y+1/2, -z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, y+1/2, -z+1/2' 'x+1/2, -y, z+1/2' _cell_length_a 11.4002(4) _cell_length_b 23.4038(11) _cell_length_c 15.6457(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4174.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.840 _exptl_crystal_F_000 2184 _exptl_absorpt_coefficient_mu 2.526 _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_reflns_number 34097 _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_av_sigmaI/netI 0.0338 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 30.03 _reflns_number_total 3229 _reflns_number_gt 2559 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP 3 for windows' _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. A non-standard crystal axes setting is applied for easy comparison of the crystal structure with the other crystal structures. CN1 is an atom of a bridging cyano group whose center is positioned at an inversion center of the crystal. CN1 was treated as a hybrid atom of 50% carbon and 50% nitrogen. CN2 is an atom of a bridging cyano group whose center is positioned at an inversion center of the crystal. CN2 was treated as a hybrid atom of 50% carbon and 50% nitrogen. ; _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^)+(0.0453P)^2^+0.0000P] 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 noref _refine_ls_extinction_method none _refine_ls_number_reflns 3229 _refine_ls_number_parameters 132 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0360 _refine_ls_R_factor_gt 0.0276 _refine_ls_wR_factor_ref 0.0741 _refine_ls_wR_factor_gt 0.0697 _refine_ls_goodness_of_fit_ref 0.896 _refine_ls_restrained_S_all 0.896 _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_symetry_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 0.03618(8) Uani 1 4 d S . . Cd2 Cd 0.2500 0.130897(10) 0.2500 0.03824(7) Uani 1 2 d S . . Cd3 Cd 0.40354(2) -0.134988(15) 0.0000 0.05712(10) Uani 1 2 d S . . C1 C 0.1477(2) 0.08241(11) 0.15107(15) 0.0463(5) Uani 1 1 d . . . N1 N 0.0925(2) 0.05613(10) 0.10555(14) 0.0532(5) Uani 1 1 d . . . C2 C 0.2412(3) -0.08602(19) 0.0000 0.0543(9) Uani 1 2 d S . . N2 N 0.1586(3) -0.06008(16) 0.0000 0.0586(8) Uani 1 2 d S . . C3 C 0.4904(3) 0.12616(18) 0.1147(2) 0.0753(10) Uani 1 1 d . . . N3 N 0.4263(3) 0.12695(18) 0.1659(2) 0.0949(12) Uani 1 1 d . . . CN1 C 0.2500 0.22587(15) 0.2500 0.0553(9) Uani 1 2 d S . . CN2 C 0.3513(4) -0.2259(2) 0.0000 0.0975(18) Uani 1 2 d S . . N101 N 0.7500 0.10166(16) 0.2500 0.0755(13) Uani 1 2 d S . . C101 C 0.6683(4) 0.12915(15) 0.2903(3) 0.0844(12) Uani 1 1 d . . . H101 H 0.6109 0.1086 0.3192 0.101 Uiso 1 1 calc R . . C102 C 0.6638(3) 0.18796(13) 0.2916(2) 0.0669(8) Uani 1 1 d . . . H102 H 0.6035 0.2067 0.3201 0.080 Uiso 1 1 calc R . . C103 C 0.7500 0.21882(16) 0.2500 0.0438(7) Uani 1 2 d S . . C111 C 0.7500 0.0384(3) 0.2500 0.171(6) Uani 1 2 d S . . H111 H 0.7269 0.0247 0.1947 0.257 Uiso 0.50 1 calc PR . . H121 H 0.6958 0.0247 0.2923 0.257 Uiso 0.50 1 calc PR . . H131 H 0.8273 0.0247 0.2631 0.257 Uiso 0.50 1 calc PR . . C201 C 0.3056(7) 0.2500 0.5000 0.0640(15) Uani 1 4 d S . . C202 C 0.3617(7) 0.2015(2) 0.5000 0.0825(16) Uani 1 2 d S . . H202 H 0.3188 0.1676 0.5000 0.099 Uiso 1 2 calc SR . . C203 C 0.4784(7) 0.1987(4) 0.5000 0.114(3) Uani 1 2 d S . . H203 H 0.5158 0.1634 0.5000 0.136 Uiso 1 2 calc SR . . C204 C 0.5458(7) 0.2500 0.5000 0.166(8) Uani 1 4 d S . . H204 H 0.6274 0.2500 0.5000 0.199 Uiso 1 4 calc SR . . C205 C 0.1683(9) 0.2500 0.5000 0.144(6) Uani 1 4 d S . . H215 H 0.1403 0.2478 0.4422 0.217 Uiso 0.25 1 calc PR . . H225 H 0.1403 0.2845 0.5260 0.217 Uiso 0.25 1 calc PR . . H235 H 0.1403 0.2177 0.5318 0.217 Uiso 0.25 1 calc PR . . 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 0.03622(15) 0.03404(16) 0.03828(15) 0.000 0.000 0.00011(13) Cd2 0.04665(13) 0.03040(12) 0.03767(12) 0.000 -0.00183(9) 0.000 Cd3 0.03713(13) 0.0841(3) 0.05011(16) 0.000 0.000 0.01320(13) C1 0.0552(12) 0.0394(12) 0.0444(11) -0.0020(10) -0.0026(11) -0.0014(11) N1 0.0631(13) 0.0468(12) 0.0497(11) -0.0065(10) -0.0068(10) -0.0060(10) C2 0.0421(17) 0.058(2) 0.063(2) 0.000 0.000 0.0035(18) N2 0.0447(16) 0.0540(19) 0.077(2) 0.000 0.000 0.0092(15) C3 0.0545(15) 0.108(3) 0.0634(18) -0.0041(18) 0.0034(15) 0.0156(18) N3 0.079(2) 0.143(4) 0.0631(18) 0.0129(18) 0.0213(16) 0.007(2) CN1 0.078(2) 0.0365(16) 0.0514(18) 0.000 -0.0046(16) 0.000 CN2 0.053(2) 0.093(4) 0.147(5) 0.000 0.000 -0.002(2) N101 0.132(4) 0.0370(19) 0.058(2) 0.000 -0.006(2) 0.000 C101 0.114(3) 0.060(2) 0.079(2) 0.0094(18) 0.006(2) -0.033(2) C102 0.0723(18) 0.0533(16) 0.0751(19) -0.0008(15) 0.0200(17) -0.0103(15) C103 0.0511(18) 0.0410(18) 0.0392(15) 0.000 -0.0044(13) 0.000 C111 0.359(18) 0.036(3) 0.118(6) 0.000 -0.008(8) 0.000 C201 0.077(4) 0.062(4) 0.053(3) 0.000 0.000 0.000 C202 0.122(5) 0.046(2) 0.080(3) 0.000 0.000 0.006(3) C203 0.118(6) 0.133(7) 0.090(4) 0.000 0.000 0.086(5) C204 0.035(3) 0.40(3) 0.063(5) 0.000 0.000 0.000 C205 0.063(5) 0.257(18) 0.113(8) 0.000 0.000 0.000 _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 2.290(3) 9 ? Cd1 N2 2.290(3) . ? Cd1 N1 2.359(2) . ? Cd1 N1 2.359(2) 11 ? Cd1 N1 2.359(2) 9 ? Cd1 N1 2.359(2) 3 ? Cd2 CN1 2.223(4) . ? Cd2 C1 2.245(2) . ? Cd2 C1 2.245(2) 8_545 ? Cd2 N3 2.404(3) . ? Cd2 N3 2.404(3) 8_545 ? Cd3 C3 2.174(4) 3_655 ? Cd3 C3 2.174(4) 9_655 ? Cd3 C2 2.177(4) . ? Cd3 CN2 2.208(6) . ? C1 N1 1.132(3) . ? C2 N2 1.121(5) . ? C3 N3 1.084(4) . ? C3 Cd3 2.174(4) 9_655 ? CN1 CN1 1.129(7) 13 ? CN2 CN2 1.130(11) 2_545 ? N101 C101 1.296(5) 8_645 ? N101 C101 1.296(5) . ? N101 C111 1.481(7) . ? C101 C102 1.377(5) . ? C102 C103 1.382(4) . ? C103 C102 1.382(4) 8_645 ? C103 C103 1.459(7) 12_565 ? C201 C202 1.304(7) 12_565 ? C201 C202 1.304(7) . ? C201 C205 1.564(12) . ? C202 C203 1.332(11) . ? C203 C204 1.426(11) . ? C204 C203 1.426(11) 12_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 N2 Cd1 N2 180.0 9 . ? N2 Cd1 N1 90.64(9) 9 . ? N2 Cd1 N1 89.36(9) . . ? N2 Cd1 N1 90.64(9) 9 11 ? N2 Cd1 N1 89.36(9) . 11 ? N1 Cd1 N1 88.85(12) . 11 ? N2 Cd1 N1 89.36(9) 9 9 ? N2 Cd1 N1 90.64(9) . 9 ? N1 Cd1 N1 180.0 . 9 ? N1 Cd1 N1 91.15(12) 11 9 ? N2 Cd1 N1 89.36(9) 9 3 ? N2 Cd1 N1 90.64(9) . 3 ? N1 Cd1 N1 91.15(12) . 3 ? N1 Cd1 N1 180.0 11 3 ? N1 Cd1 N1 88.85(12) 9 3 ? CN1 Cd2 C1 120.35(6) . . ? CN1 Cd2 C1 120.35(6) . 8_545 ? C1 Cd2 C1 119.29(13) . 8_545 ? CN1 Cd2 N3 92.20(10) . . ? C1 Cd2 N3 92.12(12) . . ? C1 Cd2 N3 85.65(11) 8_545 . ? CN1 Cd2 N3 92.20(10) . 8_545 ? C1 Cd2 N3 85.65(11) . 8_545 ? C1 Cd2 N3 92.12(12) 8_545 8_545 ? N3 Cd2 N3 175.6(2) . 8_545 ? C3 Cd3 C3 111.30(19) 3_655 9_655 ? C3 Cd3 C2 115.02(11) 3_655 . ? C3 Cd3 C2 115.02(11) 9_655 . ? C3 Cd3 CN2 103.97(13) 3_655 . ? C3 Cd3 CN2 103.97(13) 9_655 . ? C2 Cd3 CN2 106.14(17) . . ? N1 C1 Cd2 175.4(2) . . ? C1 N1 Cd1 172.5(2) . . ? N2 C2 Cd3 179.0(4) . . ? C2 N2 Cd1 174.9(4) . . ? N3 C3 Cd3 169.4(4) . 9_655 ? C3 N3 Cd2 165.6(3) . . ? CN1 CN1 Cd2 180.0 13 . ? CN2 CN2 Cd3 164.37(12) 2_545 . ? C101 N101 C101 120.5(4) 8_645 . ? C101 N101 C111 119.8(2) 8_645 . ? C101 N101 C111 119.8(2) . . ? N101 C101 C102 122.0(4) . . ? C101 C102 C103 119.3(3) . . ? C102 C103 C102 117.0(4) . 8_645 ? C102 C103 C103 121.51(19) . 12_565 ? C102 C103 C103 121.51(19) 8_645 12_565 ? C202 C201 C202 121.2(9) 12_565 . ? C202 C201 C205 119.4(4) 12_565 . ? C202 C201 C205 119.4(4) . . ? C201 C202 C203 122.2(7) . . ? C202 C203 C204 119.8(6) . . ? C203 C204 C203 114.7(7) . 12_565 ? _refine_diff_density_max 0.605 _refine_diff_density_min -1.036 _refine_diff_density_rms 0.117 #===END data_IV-1 _database_code_CSD 175548 _audit_creation_method SHELXL-97 _chemical_formula_structural 'Cd3 (C7 N7 Cl1)(C12 N2 H14)(O1 H2)2' _chemical_formula_sum 'C19 H18 Cd3 Cl1 N9 O2 ' _chemical_formula_weight 777.10 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' 'Cd' 'Cd' -0.8075 1.2024 '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' _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 8.668(2) _cell_length_b 24.152(13) _cell_length_c 8.438(2) _cell_angle_alpha 96.96(4) _cell_angle_beta 116.23(2) _cell_angle_gamma 115.54(3) _cell_volume 1319.4(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 1.93 _exptl_crystal_density_diffrn 1.96 _exptl_crystal_density_method 'floating method' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 2.513 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC5S' _diffrn_measurement_method 'profile data from theta/2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 2% _diffrn_reflns_number 8168 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 30.02 _reflns_number_total 7697 _reflns_number_observed 4691 _reflns_observed_criterion >3sigma(F) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for windows' _refine_special_details ; Weighted R-factors wR and all goodnesses 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 observed criterion of F > 3sigma(F) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. ; _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^)+(0.0788P)^2^+1.7991P] 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 noref _refine_ls_extinction_method none _refine_ls_number_reflns 4691 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs 0.0553 _refine_ls_wR_factor_obs 0.1358 _refine_ls_goodness_of_fit_obs 1.090 _refine_ls_restrained_S_obs 1.090 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.0000 0.5000 0.0000 0.02967(19) Uani 1 2 d S . . Cd2 Cd 0.0000 0.0000 0.5000 0.0321(2) Uani 1 2 d S . . Cd3 Cd -0.11759(9) 0.13513(3) 0.00141(9) 0.03273(16) Uani 1 1 d . . . Cd4 Cd 0.15062(9) 0.32047(3) -0.29617(8) 0.03065(15) Uani 1 1 d . . . Cl1 Cl 0.0843(4) 0.44652(13) 0.2477(3) 0.0454(5) Uani 1 1 d . . . N1 N 0.0216(13) 0.4258(4) -0.1920(12) 0.0449(19) Uani 1 1 d . . . C1 C 0.0551(13) 0.3895(4) -0.2400(12) 0.0359(18) Uani 1 1 d . . . N2 N 0.6442(11) 0.4211(4) -0.1399(12) 0.0445(19) Uani 1 1 d . . . C2 C 0.4808(12) 0.3854(4) -0.1897(12) 0.0360(18) Uani 1 1 d . . . N3 N 0.0831(14) 0.2569(5) -0.1319(13) 0.055(2) Uani 1 1 d . . . C3 C 0.0295(13) 0.2219(4) -0.0648(12) 0.0322(17) Uani 1 1 d . . . N4 N -0.0885(14) 0.2227(5) 0.2488(13) 0.054(2) Uani 1 1 d . . . C4 C -0.0208(13) 0.2558(4) 0.3969(13) 0.0350(18) Uani 1 1 d . . . N5 N 0.0390(18) 0.0798(6) 0.3413(15) 0.066(3) Uani 1 1 d . . . C5 C -0.0019(16) 0.1012(5) 0.2302(15) 0.046(2) Uani 1 1 d . . . N6 N -0.0738(14) 0.0778(5) 0.7900(13) 0.052(2) Uani 1 1 d . . . C6 C -0.0395(13) 0.0557(5) 0.6967(13) 0.040(2) Uani 1 1 d . . . N7 N 0.3735(14) 0.0624(5) 0.7283(13) 0.054(2) Uani 1 1 d . . . C7 C 0.5418(13) 0.0866(5) 0.8199(12) 0.0365(19) Uani 1 1 d . . . C101 C 0.5692(16) 0.6116(5) 0.6507(16) 0.048(2) Uani 1 1 d . . . H101 H 0.6507 0.6004 0.6298 0.072 Uiso 1 1 calc R . . C102 C 0.5723(15) 0.6677(5) 0.6276(14) 0.046(2) Uani 1 1 d . . . H102 H 0.6499 0.6926 0.5847 0.070 Uiso 1 1 calc R . . C103 C 0.4601(13) 0.6869(5) 0.6683(12) 0.0370(19) Uani 1 1 d . . . C104 C 0.3340(15) 0.6441(5) 0.7144(15) 0.047(2) Uani 1 1 d . . . H104 H 0.2515 0.6540 0.7373 0.070 Uiso 1 1 calc R . . C105 C 0.3287(14) 0.5864(5) 0.7270(14) 0.044(2) Uani 1 1 d . . . H105 H 0.2390 0.5571 0.7528 0.066 Uiso 1 1 calc R . . C106 C 0.5505(16) 0.8550(5) 0.8351(15) 0.049(2) Uani 1 1 d . . . H106 H 0.5921 0.8859 0.9463 0.073 Uiso 1 1 calc R . . C107 C 0.5416(15) 0.7961(6) 0.8341(14) 0.048(2) Uani 1 1 d . . . H107 H 0.5788 0.7878 0.9458 0.072 Uiso 1 1 calc R . . C108 C 0.4784(12) 0.7498(5) 0.6695(12) 0.0350(18) Uani 1 1 d . . . C109 C 0.4306(15) 0.7647(5) 0.5078(14) 0.049(2) Uani 1 1 d . . . H109 H 0.3904 0.7350 0.3953 0.074 Uiso 1 1 calc R . . C110 C 0.4430(18) 0.8236(6) 0.5147(15) 0.063(3) Uani 1 1 d . . . H110 H 0.4123 0.8338 0.4062 0.094 Uiso 1 1 calc R . . C111 C 0.4525(16) 0.5144(6) 0.7315(15) 0.051(2) Uani 1 1 d . . . H111 H 0.5611 0.5142 0.7270 0.061 Uiso 1 1 calc R . . H121 H 0.3235 0.4747 0.6325 0.061 Uiso 1 1 calc R . . H131 H 0.4737 0.5158 0.8540 0.061 Uiso 1 1 calc R . . C112 C 0.499(3) 0.9279(8) 0.670(3) 0.099(5) Uani 1 1 d . . . H112 H 0.3782 0.9227 0.6605 0.119 Uiso 1 1 calc R . . H122 H 0.4992 0.9356 0.5613 0.119 Uiso 1 1 calc R . . H132 H 0.6185 0.9651 0.7851 0.119 Uiso 1 1 calc R . . N101 N 0.4514(11) 0.5736(4) 0.7021(10) 0.0360(16) Uani 1 1 d . . . N102 N 0.4986(13) 0.8668(5) 0.6752(14) 0.053(2) Uani 1 1 d . . . O1 O -0.2580(14) 0.2868(5) -0.0482(12) 0.075(3) Uani 1 1 d . . . H11 H -0.1590 0.3328 0.0360 0.112 Uiso 1 1 calc . . . H12 H -0.2087 0.2784 -0.1262 0.112 Uiso 1 1 calc . . . O2 O -0.680(3) 0.2292(9) -0.284(3) 0.210(9) Uani 1 1 calc . . . H21 H -0.5341 0.2492 -0.2055 0.314 Uiso 1 1 calc . . . H22 H -0.7355 0.2033 -0.4136 0.314 Uiso 1 1 calc . . . 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 0.0218(4) 0.0294(4) 0.0352(4) 0.0107(3) 0.0154(3) 0.0127(3) Cd2 0.0310(4) 0.0399(5) 0.0287(4) 0.0130(4) 0.0159(3) 0.0225(4) Cd3 0.0278(3) 0.0354(3) 0.0326(3) 0.0162(3) 0.0148(2) 0.0166(3) Cd4 0.0249(3) 0.0279(3) 0.0307(3) 0.0075(2) 0.0158(2) 0.0088(2) Cl1 0.0378(11) 0.0608(15) 0.0499(13) 0.0307(12) 0.0260(10) 0.0315(11) N1 0.049(5) 0.046(5) 0.048(5) 0.011(4) 0.029(4) 0.030(4) C1 0.033(4) 0.032(4) 0.034(4) 0.008(3) 0.016(4) 0.015(4) N2 0.023(3) 0.044(5) 0.048(5) 0.019(4) 0.015(3) 0.010(3) C2 0.025(4) 0.037(5) 0.038(4) 0.017(4) 0.014(4) 0.014(4) N3 0.046(5) 0.054(5) 0.056(5) 0.016(4) 0.025(4) 0.026(5) C3 0.039(4) 0.029(4) 0.033(4) 0.018(3) 0.023(4) 0.016(4) N4 0.054(5) 0.061(6) 0.047(5) 0.016(4) 0.031(4) 0.028(5) C4 0.028(4) 0.030(4) 0.038(4) 0.007(4) 0.019(4) 0.011(3) N5 0.087(8) 0.084(8) 0.065(6) 0.051(6) 0.053(6) 0.058(7) C5 0.052(6) 0.055(6) 0.049(6) 0.037(5) 0.033(5) 0.032(5) N6 0.051(5) 0.057(5) 0.053(5) 0.015(4) 0.033(4) 0.030(5) C6 0.033(4) 0.040(5) 0.040(5) 0.009(4) 0.020(4) 0.016(4) N7 0.043(5) 0.064(6) 0.048(5) 0.016(4) 0.024(4) 0.028(4) C7 0.030(4) 0.043(5) 0.031(4) 0.008(4) 0.016(4) 0.018(4) C101 0.048(6) 0.044(6) 0.061(6) 0.016(5) 0.040(5) 0.022(5) C102 0.043(5) 0.042(5) 0.054(6) 0.012(5) 0.037(5) 0.012(4) C103 0.028(4) 0.048(5) 0.029(4) 0.015(4) 0.015(3) 0.016(4) C104 0.038(5) 0.065(7) 0.061(6) 0.032(5) 0.036(5) 0.033(5) C105 0.038(5) 0.059(6) 0.049(5) 0.029(5) 0.029(4) 0.028(5) C106 0.045(5) 0.055(6) 0.052(6) 0.021(5) 0.030(5) 0.027(5) C107 0.043(5) 0.063(7) 0.039(5) 0.019(5) 0.021(4) 0.032(5) C108 0.023(4) 0.045(5) 0.031(4) 0.016(4) 0.014(3) 0.015(4) C109 0.041(5) 0.047(6) 0.035(5) 0.014(4) 0.019(4) 0.008(4) C110 0.055(7) 0.069(8) 0.040(6) 0.034(6) 0.021(5) 0.019(6) C111 0.049(6) 0.061(7) 0.049(6) 0.027(5) 0.025(5) 0.036(5) C112 0.134(15) 0.069(10) 0.126(14) 0.059(10) 0.079(13) 0.065(11) N101 0.035(4) 0.039(4) 0.035(4) 0.015(3) 0.021(3) 0.020(3) N102 0.039(4) 0.050(5) 0.063(6) 0.027(5) 0.027(4) 0.018(4) O1 0.079(6) 0.078(6) 0.052(5) 0.014(4) 0.029(5) 0.043(5) O2 0.19(2) 0.160(17) 0.25(2) 0.034(16) 0.118(18) 0.094(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 Cd1 N2 2.388(7) 2_665 ? Cd1 N2 2.388(7) 1_455 ? Cd1 N1 2.392(7) . ? Cd1 N1 2.392(7) 2_565 ? Cd1 Cl1 2.586(2) 2_565 ? Cd1 Cl1 2.586(2) . ? Cd2 C6 2.244(9) 2_556 ? Cd2 C6 2.244(9) . ? Cd2 N7 2.457(9) . ? Cd2 N7 2.457(9) 2_556 ? Cd2 N5 2.467(9) . ? Cd2 N5 2.467(9) 2_556 ? Cd3 C5 2.187(9) . ? Cd3 C3 2.223(8) . ? Cd3 C7 2.240(9) 1_454 ? Cd3 N6 2.387(9) 1_554 ? Cd3 N4 2.627(9) . ? Cd4 C2 2.230(8) . ? Cd4 C4 2.230(9) 1_554 ? Cd4 C1 2.244(9) . ? Cd4 N3 2.254(10) . ? N1 C1 1.121(11) . ? N2 C2 1.122(11) . ? N2 Cd1 2.388(7) 1_655 ? N3 C3 1.122(12) . ? N4 C4 1.118(12) . ? C4 Cd4 2.230(9) 1_556 ? N5 C5 1.121(12) . ? N6 C6 1.112(12) . ? N6 Cd3 2.387(9) 1_556 ? N7 C7 1.107(12) . ? C7 Cd3 2.240(9) 1_656 ? C101 N101 1.324(12) . ? C101 C102 1.383(14) . ? C102 C103 1.387(13) . ? C103 C104 1.384(12) . ? C103 C108 1.456(13) . ? C104 C105 1.392(14) . ? C105 N101 1.319(11) . ? C106 N102 1.330(13) . ? C106 C107 1.391(15) . ? C107 C108 1.379(13) . ? C108 C109 1.381(12) . ? C109 C110 1.372(16) . ? C110 N102 1.342(15) . ? C111 N101 1.484(13) . ? C112 N102 1.483(16) . ? 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 180.0 2_665 1_455 ? N2 Cd1 N1 87.8(3) 2_665 . ? N2 Cd1 N1 92.2(3) 1_455 . ? N2 Cd1 N1 92.2(3) 2_665 2_565 ? N2 Cd1 N1 87.8(3) 1_455 2_565 ? N1 Cd1 N1 180.0 . 2_565 ? N2 Cd1 Cl1 88.6(2) 2_665 2_565 ? N2 Cd1 Cl1 91.4(2) 1_455 2_565 ? N1 Cd1 Cl1 92.6(2) . 2_565 ? N1 Cd1 Cl1 87.4(2) 2_565 2_565 ? N2 Cd1 Cl1 91.4(2) 2_665 . ? N2 Cd1 Cl1 88.6(2) 1_455 . ? N1 Cd1 Cl1 87.4(2) . . ? N1 Cd1 Cl1 92.6(2) 2_565 . ? Cl1 Cd1 Cl1 180.0 2_565 . ? C6 Cd2 C6 180.0 2_556 . ? C6 Cd2 N7 87.5(3) 2_556 . ? C6 Cd2 N7 92.5(3) . . ? C6 Cd2 N7 92.5(3) 2_556 2_556 ? C6 Cd2 N7 87.5(3) . 2_556 ? N7 Cd2 N7 180.0 . 2_556 ? C6 Cd2 N5 87.1(3) 2_556 . ? C6 Cd2 N5 92.9(3) . . ? N7 Cd2 N5 90.6(4) . . ? N7 Cd2 N5 89.4(4) 2_556 . ? C6 Cd2 N5 92.9(3) 2_556 2_556 ? C6 Cd2 N5 87.1(3) . 2_556 ? N7 Cd2 N5 89.4(4) . 2_556 ? N7 Cd2 N5 90.6(4) 2_556 2_556 ? N5 Cd2 N5 180.0 . 2_556 ? C5 Cd3 C3 133.7(4) . . ? C5 Cd3 C7 116.3(4) . 1_454 ? C3 Cd3 C7 108.9(3) . 1_454 ? C5 Cd3 N6 96.4(4) . 1_554 ? C3 Cd3 N6 85.1(3) . 1_554 ? C7 Cd3 N6 99.9(3) 1_454 1_554 ? C5 Cd3 N4 87.0(4) . . ? C3 Cd3 N4 83.1(3) . . ? C7 Cd3 N4 90.2(3) 1_454 . ? N6 Cd3 N4 166.5(3) 1_554 . ? C2 Cd4 C4 108.4(3) . 1_554 ? C2 Cd4 C1 105.9(3) . . ? C4 Cd4 C1 115.0(3) 1_554 . ? C2 Cd4 N3 115.5(3) . . ? C4 Cd4 N3 109.5(3) 1_554 . ? C1 Cd4 N3 102.6(3) . . ? C1 N1 Cd1 162.6(8) . . ? N1 C1 Cd4 172.7(8) . . ? C2 N2 Cd1 173.9(8) . 1_655 ? N2 C2 Cd4 175.3(8) . . ? C3 N3 Cd4 173.1(8) . . ? N3 C3 Cd3 166.9(8) . . ? C4 N4 Cd3 153.2(8) . . ? N4 C4 Cd4 172.3(8) . 1_556 ? C5 N5 Cd2 159.3(10) . . ? N5 C5 Cd3 173.6(10) . . ? C6 N6 Cd3 174.5(9) . 1_556 ? N6 C6 Cd2 173.6(9) . . ? C7 N7 Cd2 173.5(9) . . ? N7 C7 Cd3 179.1(9) . 1_656 ? N101 C101 C102 120.7(8) . . ? C101 C102 C103 120.2(8) . . ? C104 C103 C102 116.5(9) . . ? C104 C103 C108 121.3(8) . . ? C102 C103 C108 122.2(8) . . ? C103 C104 C105 121.1(8) . . ? N101 C105 C104 119.7(8) . . ? N102 C106 C107 119.3(10) . . ? C108 C107 C106 120.8(9) . . ? C107 C108 C109 118.1(9) . . ? C107 C108 C103 120.1(8) . . ? C109 C108 C103 121.8(9) . . ? C110 C109 C108 119.5(10) . . ? N102 C110 C109 121.2(9) . . ? C105 N101 C101 121.5(8) . . ? C105 N101 C111 118.0(8) . . ? C101 N101 C111 120.5(8) . . ? C106 N102 C110 121.2(10) . . ? C106 N102 C112 120.4(11) . . ? C110 N102 C112 118.4(11) . . ? 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 C104 C103 C108 C107 57.8(12) . . . . ? C102 C103 C108 C107 -119.9(10) . . . . ? C104 C103 C108 C109 -121.1(10) . . . . ? C102 C103 C108 C109 61.1(13) . . . . ? _refine_diff_density_max 1.763 _refine_diff_density_min -1.848 _refine_diff_density_rms 0.198 #===END data_V-1 _database_code_CSD 175549 _audit_creation_method SHELXL-97 _chemical_formula_structural 'Cd2 (C6 N6)(C12 N2 H14)' _chemical_formula_sum 'C18 H14 Cd2 N8' _chemical_formula_weight 567.19 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' 'Cd' 'Cd' -0.8075 1.2024 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 10.015(4) _cell_length_b 14.675(3) _cell_length_c 15.0340(14) _cell_angle_alpha 90.00 _cell_angle_beta 93.169(15) _cell_angle_gamma 90.00 _cell_volume 2206.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.71 _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 1.933 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC5S' _diffrn_measurement_method 'profile data from theta/2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 2% _diffrn_reflns_number 3527 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 30.00 _reflns_number_total 3233 _reflns_number_observed 2265 _reflns_observed_criterion >3sigma(F) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for windows' _refine_special_details ; Weighted R-factors wR and all goodnesses 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 observed criterion of F > 3sigma(F) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. ; _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^)+(0.0387P)^2^+1.2097P] 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 noref _refine_ls_extinction_method none _refine_ls_number_reflns 2265 _refine_ls_number_parameters 129 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs 0.0388 _refine_ls_wR_factor_obs 0.0871 _refine_ls_goodness_of_fit_obs 1.090 _refine_ls_restrained_S_obs 1.090 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.0000 0.49447(3) 0.2500 0.03080(12) Uani 1 2 d S . . Cd2 Cd 0.2500 0.2500 0.0000 0.03618(13) Uani 1 2 d S . . C1 C 0.1035(5) 0.3995(3) 0.1609(3) 0.0355(9) Uani 1 1 d . . . N1 N 0.1472(5) 0.3476(3) 0.1145(3) 0.0490(11) Uani 1 1 d . . . C2 C 0.1338(6) 0.5799(3) 0.3382(3) 0.0431(11) Uani 1 1 d . . . N2 N 0.1938(5) 0.6228(3) 0.3889(3) 0.0558(12) Uani 1 1 d . . . C3 C 0.4466(5) 0.3100(3) 0.0385(3) 0.0386(10) Uani 1 1 d . . . N3 N 0.5482(5) 0.3389(3) 0.0622(4) 0.0563(12) Uani 1 1 d . . . N101 N 0.2448(4) 0.1037(3) 0.4231(3) 0.0341(8) Uani 1 1 d . . . C101 C 0.2358(5) 0.1765(3) 0.3681(3) 0.0410(11) Uani 1 1 d . . . H101 H 0.2962 0.2244 0.3759 0.049 Uiso 1 1 calc R . . C102 C 0.1385(5) 0.1799(3) 0.3012(3) 0.0409(11) Uani 1 1 d . . . H102 H 0.1303 0.2310 0.2647 0.049 Uiso 1 1 calc R . . C103 C 0.0517(5) 0.1069(3) 0.2877(3) 0.0337(9) Uani 1 1 d . . . C104 C 0.0633(5) 0.0338(3) 0.3454(3) 0.0381(10) Uani 1 1 d . . . H104 H 0.0055 -0.0155 0.3382 0.046 Uiso 1 1 calc R . . C105 C 0.1593(5) 0.0345(3) 0.4126(3) 0.0398(11) Uani 1 1 d . . . H105 H 0.1656 -0.0143 0.4521 0.048 Uiso 1 1 calc R . . C111 C 0.3495(5) 0.1025(4) 0.4970(4) 0.0490(13) Uani 1 1 d . . . H111 H 0.4145 0.1490 0.4871 0.073 Uiso 1 1 calc R . . H121 H 0.3926 0.0441 0.4992 0.073 Uiso 1 1 calc R . . H131 H 0.3092 0.1138 0.5524 0.073 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 0.0397(3) 0.0282(2) 0.0249(2) 0.000 0.00491(17) 0.000 Cd2 0.0321(2) 0.0342(3) 0.0424(3) -0.00370(19) 0.00305(19) 0.00368(18) C1 0.039(2) 0.037(2) 0.031(2) 0.0006(18) 0.0060(18) 0.0012(19) N1 0.048(3) 0.055(3) 0.045(2) -0.009(2) 0.010(2) 0.006(2) C2 0.053(3) 0.038(2) 0.039(3) -0.006(2) 0.009(2) -0.009(2) N2 0.058(3) 0.056(3) 0.054(3) -0.013(2) 0.006(2) -0.014(2) C3 0.035(2) 0.033(2) 0.048(3) 0.003(2) 0.004(2) 0.0081(19) N3 0.044(3) 0.048(3) 0.077(4) -0.001(2) 0.003(2) 0.001(2) N101 0.035(2) 0.0345(19) 0.0333(19) -0.0011(15) 0.0018(15) 0.0013(16) C101 0.045(3) 0.032(2) 0.046(3) 0.006(2) -0.001(2) -0.004(2) C102 0.049(3) 0.034(2) 0.039(2) 0.0065(19) -0.003(2) -0.005(2) C103 0.039(2) 0.028(2) 0.033(2) -0.0014(17) 0.0000(18) 0.0014(18) C104 0.042(3) 0.032(2) 0.040(2) 0.0026(19) -0.003(2) -0.007(2) C105 0.043(3) 0.032(2) 0.043(3) 0.010(2) -0.001(2) -0.002(2) C111 0.041(3) 0.053(3) 0.051(3) 0.008(3) -0.012(2) 0.003(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 C2 2.220(5) . ? Cd1 C2 2.220(5) 2 ? Cd1 C1 2.228(5) . ? Cd1 C1 2.228(5) 2 ? Cd2 C3 2.205(5) . ? Cd2 C3 2.205(5) 7 ? Cd2 N1 2.504(4) . ? Cd2 N1 2.504(4) 7 ? Cd2 N2 2.548(5) 6_565 ? Cd2 N2 2.548(5) 4_545 ? C1 N1 1.137(6) . ? C2 N2 1.134(7) . ? N2 Cd2 2.548(5) 4 ? C3 N3 1.141(7) . ? N101 C105 1.332(6) . ? N101 C101 1.352(6) . ? N101 C111 1.485(6) . ? C101 C102 1.361(7) . ? C102 C103 1.387(6) . ? C103 C104 1.380(6) . ? C103 C103 1.493(9) 2 ? C104 C105 1.356(7) . ? 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 C2 Cd1 C2 111.3(3) . 2 ? C2 Cd1 C1 115.27(18) . . ? C2 Cd1 C1 106.23(17) 2 . ? C2 Cd1 C1 106.23(17) . 2 ? C2 Cd1 C1 115.27(18) 2 2 ? C1 Cd1 C1 102.6(2) . 2 ? C3 Cd2 C3 180.0 . 7 ? C3 Cd2 N1 89.20(17) . . ? C3 Cd2 N1 90.80(17) 7 . ? C3 Cd2 N1 90.80(17) . 7 ? C3 Cd2 N1 89.20(17) 7 7 ? N1 Cd2 N1 180.00(14) . 7 ? C3 Cd2 N2 92.34(17) . 6_565 ? C3 Cd2 N2 87.66(17) 7 6_565 ? N1 Cd2 N2 86.99(15) . 6_565 ? N1 Cd2 N2 93.01(15) 7 6_565 ? C3 Cd2 N2 87.66(17) . 4_545 ? C3 Cd2 N2 92.34(17) 7 4_545 ? N1 Cd2 N2 93.01(15) . 4_545 ? N1 Cd2 N2 86.99(15) 7 4_545 ? N2 Cd2 N2 180.0(2) 6_565 4_545 ? N1 C1 Cd1 174.7(5) . . ? C1 N1 Cd2 172.7(4) . . ? N2 C2 Cd1 173.8(5) . . ? C2 N2 Cd2 159.5(5) . 4 ? N3 C3 Cd2 176.7(5) . . ? C105 N101 C101 120.6(4) . . ? C105 N101 C111 120.2(4) . . ? C101 N101 C111 119.1(4) . . ? N101 C101 C102 120.1(4) . . ? C101 C102 C103 119.8(4) . . ? C104 C103 C102 118.5(4) . . ? C104 C103 C103 120.5(3) . 2 ? C102 C103 C103 120.9(3) . 2 ? C105 C104 C103 119.6(4) . . ? N101 C105 C104 121.2(4) . . ? _refine_diff_density_max 0.521 _refine_diff_density_min -0.963 _refine_diff_density_rms 0.111 #===END