Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Hirofumi Yoshikawa' _publ_contact_author_address ; Department of Chemistry, Graduate School of Science, Nagoya University, Furo-cho, Chikusa-ku, Nagoya 464-8602, Japan ; _publ_contact_author_email yoshikawah@mbox.chem.nagoya-u.ac.jp _publ_contact_author_fax '+81 52 789 2484' _publ_contact_author_phone '+81 52 789 2484' _publ_section_title ; Crystal Structures and Spectroscopic Properties of Polycyano-Polycadmate Host Clathrates Including a CT Complex Guest of Methylviologen dication and Aromatic Donor. ; loop_ _publ_author_name 'Hirofumi Yoshikawa' 'Shin-ichi Nishikiori' #------------------------------------------------------------------ data_ocretr21 _database_code_depnum_ccdc_archive 'CCDC 269964' _audit_creation_method SHELXL-97 _chemical_formula_structural '(C12 H14 N2) (Cd3 (C N)8 (H2 O)2) (C7 H8 O)2' _chemical_formula_sum 'C34 H34 Cd3 N10 O4' _chemical_formula_weight 983.94 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 Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 8.9851(2) _cell_length_b 15.7530(2) _cell_length_c 13.7745(3) _cell_angle_alpha 90 _cell_angle_beta 94.4280(6) _cell_angle_gamma 90 _cell_volume 1943.85(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 40626 _cell_measurement_theta_min 1.48 _cell_measurement_theta_max 30.03 _exptl_crystal_description yellow _exptl_crystal_colour block _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.681 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4864 _exptl_absorpt_coefficient_mu 1.667 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8394 _exptl_absorpt_correction_T_max 1.1238 _exptl_absorpt_process_details 'PROCESS-AUTO, RIGAKU Co., Tokyo, Japan(1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_reflns_number 39425 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 30.03 _reflns_number_total 5695 _reflns_number_gt 4669 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0330P)^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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 5695 _refine_ls_number_parameters 234 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0227 _refine_ls_wR_factor_ref 0.0600 _refine_ls_wR_factor_gt 0.0584 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.5000 0.5000 0.0000 0.02836(5) Uani 1 2 d S . . Cd2 Cd 0.029442(16) 0.535467(9) 0.245355(10) 0.03242(5) Uani 1 1 d . . . O1 O 0.48531(19) 0.64827(9) -0.00834(12) 0.0482(4) Uani 1 1 d . . . H1 H 0.3970 0.6766 0.0107 0.072 Uiso 1 1 d . . . H2 H 0.5106 0.6790 -0.0560 0.072 Uiso 1 1 d . . . C1 C 0.2305(2) 0.51396(14) 0.16211(16) 0.0379(4) Uani 1 1 d . . . N1 N 0.3317(2) 0.50399(13) 0.11903(14) 0.0426(4) Uani 1 1 d . . . C2 C 0.8136(2) 0.51448(14) 0.15943(16) 0.0388(4) Uani 1 1 d . . . N2 N 0.7029(2) 0.50748(13) 0.11457(14) 0.0453(4) Uani 1 1 d . . . C3 C 0.0349(2) 0.66674(14) 0.30540(16) 0.0394(4) Uani 1 1 d . . . N3 N 0.0350(2) 0.73244(13) 0.33822(16) 0.0518(5) Uani 1 1 d . . . C4 C 0.0588(3) 0.44318(14) 0.36710(18) 0.0444(5) Uani 1 1 d . . . N4 N 0.0855(3) 0.39429(16) 0.42532(19) 0.0684(7) Uani 1 1 d . . . O201 O 0.2633(2) 0.25934(10) 0.48326(13) 0.0555(4) Uani 1 1 d . . . H201 H 0.2023 0.2981 0.4788 0.083 Uiso 1 1 calc R . . C201 C 0.3639(2) 0.27371(13) 0.56126(16) 0.0395(5) Uani 1 1 d . . . C202 C 0.3493(3) 0.34029(14) 0.62537(19) 0.0464(5) Uani 1 1 d . . . H202 H 0.2692 0.3776 0.6162 0.056 Uiso 1 1 calc . . . C203 C 0.4542(3) 0.35120(16) 0.70302(19) 0.0531(6) Uani 1 1 d . . . H203 H 0.4443 0.3959 0.7462 0.064 Uiso 1 1 calc . . . C204 C 0.5729(3) 0.29652(19) 0.71688(19) 0.0553(6) Uani 1 1 d . . . H204 H 0.6437 0.3041 0.7691 0.066 Uiso 1 1 calc . . . C205 C 0.5864(3) 0.23054(16) 0.65310(19) 0.0502(6) Uani 1 1 d . . . H205 H 0.6665 0.1934 0.6633 0.060 Uiso 1 1 calc . . . C206 C 0.4843(3) 0.21769(13) 0.57415(17) 0.0414(5) Uani 1 1 d . . . C207 C 0.5014(4) 0.14741(17) 0.5024(2) 0.0632(7) Uani 1 1 d . . . H217 H 0.5974 0.1212 0.5151 0.095 Uiso 1 1 calc R . . H227 H 0.4932 0.1702 0.4375 0.095 Uiso 1 1 calc R . . H237 H 0.4245 0.1059 0.5086 0.095 Uiso 1 1 calc R . . N101 N 0.6895(2) 0.34102(11) 0.38252(14) 0.0418(4) Uani 1 1 d . . . C101 C 0.7343(3) 0.36316(15) 0.47314(17) 0.0454(5) Uani 1 1 d . . . H101 H 0.8164 0.3362 0.5049 0.054 Uiso 1 1 calc . . . C102 C 0.6613(2) 0.42497(16) 0.52030(15) 0.0418(5) Uani 1 1 d . . . H102 H 0.6945 0.4396 0.5837 0.050 Uiso 1 1 calc . . . C103 C 0.5396(2) 0.46592(12) 0.47551(14) 0.0326(4) Uani 1 1 d . . . C104 C 0.4949(3) 0.44066(17) 0.38125(18) 0.0578(7) Uani 1 1 d . . . H104 H 0.4126 0.4662 0.3481 0.069 Uiso 1 1 calc . . . C105 C 0.5707(3) 0.37873(17) 0.33716(19) 0.0614(8) Uani 1 1 d . . . H105 H 0.5391 0.3623 0.2741 0.074 Uiso 1 1 calc . . . C111 C 0.7731(3) 0.27573(18) 0.3316(2) 0.0605(7) Uani 1 1 d . . . H111 H 0.7280 0.2212 0.3395 0.091 Uiso 1 1 calc . . . H121 H 0.8748 0.2743 0.3588 0.091 Uiso 1 1 calc . . . H131 H 0.7709 0.2894 0.2636 0.091 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 0.02093(8) 0.03388(9) 0.02994(9) -0.00152(7) -0.00018(7) 0.00015(7) Cd2 0.02331(7) 0.04056(8) 0.03294(8) -0.00025(6) -0.00073(5) 0.00063(5) O1 0.0508(10) 0.0342(7) 0.0607(11) 0.0067(7) 0.0107(8) 0.0056(7) C1 0.0298(10) 0.0466(11) 0.0374(11) -0.0014(8) 0.0025(8) -0.0010(8) N1 0.0310(9) 0.0560(11) 0.0413(10) -0.0040(8) 0.0061(8) -0.0018(8) C2 0.0285(10) 0.0494(11) 0.0382(11) -0.0026(8) -0.0002(8) 0.0011(9) N2 0.0296(9) 0.0633(12) 0.0419(10) -0.0045(9) -0.0051(8) 0.0016(9) C3 0.0315(10) 0.0463(11) 0.0397(11) -0.0001(9) -0.0005(8) 0.0007(9) N3 0.0475(12) 0.0480(10) 0.0591(13) -0.0096(9) -0.0004(10) 0.0028(9) C4 0.0389(12) 0.0468(11) 0.0468(12) 0.0035(9) -0.0013(10) -0.0030(10) N4 0.0689(16) 0.0638(13) 0.0702(16) 0.0255(12) -0.0094(13) -0.0033(13) O201 0.0513(11) 0.0488(9) 0.0637(11) 0.0058(8) -0.0128(9) -0.0060(8) C201 0.0358(11) 0.0362(10) 0.0469(12) 0.0045(8) 0.0054(9) -0.0103(9) C202 0.0403(12) 0.0401(10) 0.0610(15) 0.0007(10) 0.0182(11) -0.0042(9) C203 0.0581(16) 0.0534(13) 0.0503(14) -0.0122(11) 0.0209(12) -0.0178(12) C204 0.0492(14) 0.0695(16) 0.0469(13) -0.0038(12) 0.0013(11) -0.0181(13) C205 0.0393(13) 0.0512(13) 0.0596(15) 0.0023(11) 0.0003(11) -0.0023(10) C206 0.0406(12) 0.0359(10) 0.0481(12) 0.0004(9) 0.0058(10) -0.0039(9) C207 0.076(2) 0.0461(13) 0.0680(19) -0.0104(13) 0.0059(16) 0.0051(14) N101 0.0349(9) 0.0412(9) 0.0494(11) -0.0118(8) 0.0034(8) -0.0030(8) C101 0.0334(11) 0.0575(13) 0.0444(12) -0.0042(10) -0.0023(9) 0.0057(10) C102 0.0341(11) 0.0566(12) 0.0341(10) -0.0055(9) -0.0010(8) -0.0002(10) C103 0.0353(10) 0.0326(9) 0.0295(9) -0.0017(7) 0.0001(8) -0.0065(8) C104 0.0657(17) 0.0591(14) 0.0444(13) -0.0184(11) -0.0217(12) 0.0234(13) C105 0.0710(18) 0.0630(15) 0.0468(14) -0.0228(12) -0.0183(13) 0.0184(14) C111 0.0476(14) 0.0629(15) 0.0711(18) -0.0288(13) 0.0055(13) 0.0066(13) _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cd1 O1 2.3417(14) . . Cd1 N1 2.3155(19) . . Cd1 N2 2.3203(19) . . Cd1 O1 2.3417(14) . 3_665 Cd1 N1 2.3155(19) . 3_665 Cd1 N2 2.3203(19) . 3_665 Cd2 C1 2.2390(19) . . Cd2 C3 2.226(2) . . Cd2 C4 2.220(2) . . Cd2 C2 2.2174(19) . 1_455 O1 H1 0.9642 . . O1 H2 0.8602 . . O201 C201 1.369(3) . . O201 H201 0.8196 . . N1 C1 1.134(3) . . N2 C2 1.135(3) . . N3 C3 1.129(3) . . N4 C4 1.124(3) . . N101 C111 1.482(3) . . N101 C101 1.328(3) . . N101 C105 1.334(3) . . C101 C102 1.366(3) . . C102 C103 1.374(3) . . C103 C104 1.387(3) . . C103 C103 1.479(3) . 3_666 C104 C105 1.360(4) . . C101 H101 0.9306 . . C102 H102 0.9298 . . C104 H104 0.9301 . . C105 H105 0.9295 . . C111 H131 0.9598 . . C111 H111 0.9596 . . C111 H121 0.9607 . . C201 C206 1.397(3) . . C201 C202 1.384(3) . . C202 C203 1.381(4) . . C203 C204 1.373(4) . . C204 C205 1.372(4) . . C205 C206 1.382(4) . . C206 C207 1.500(4) . . C202 H202 0.9302 . . C203 H203 0.9304 . . C204 H204 0.9304 . . C205 H205 0.9297 . . C207 H217 0.9601 . . C207 H227 0.9609 . . C207 H237 0.9599 . . 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_2 _geom_angle_site_symmetry_3 O1 Cd1 N1 88.30(7) . . . O1 Cd1 N2 91.21(7) . . . O1 Cd1 O1 180.00 . . 3_665 O1 Cd1 N1 91.71(7) . . 3_665 O1 Cd1 N2 88.79(7) . . 3_665 N1 Cd1 N2 92.22(7) . . . O1 Cd1 N1 91.71(7) 3_665 . . N1 Cd1 N1 180.00 . . 3_665 N1 Cd1 N2 87.78(7) . . 3_665 O1 Cd1 N2 88.79(7) 3_665 . . N1 Cd1 N2 87.78(7) 3_665 . . N2 Cd1 N2 180.00 . . 3_665 O1 Cd1 N1 88.30(7) 3_665 . 3_665 O1 Cd1 N2 91.21(7) 3_665 . 3_665 N1 Cd1 N2 92.22(7) 3_665 . 3_665 C1 Cd2 C3 109.59(7) . . . C1 Cd2 C4 103.55(9) . . . C1 Cd2 C2 114.27(8) . . 1_455 C3 Cd2 C4 109.25(8) . . . C2 Cd2 C3 109.27(7) 1_455 . . C2 Cd2 C4 110.71(9) 1_455 . . Cd1 O1 H2 125.56 . . . H1 O1 H2 102.62 . . . Cd1 O1 H1 119.52 . . . C201 O201 H201 109.45 . . . Cd1 N1 C1 165.42(18) . . . Cd1 N2 C2 169.95(18) . . . C101 N101 C111 120.0(2) . . . C105 N101 C111 120.3(2) . . . C101 N101 C105 119.8(2) . . . Cd2 C1 N1 179.00(19) . . . Cd2 C2 N2 177.0(2) 1_655 . . Cd2 C3 N3 177.76(19) . . . Cd2 C4 N4 173.7(2) . . . N101 C101 C102 120.8(2) . . . C101 C102 C103 121.1(2) . . . C102 C103 C103 122.01(18) . . 3_666 C103 C103 C104 121.35(19) 3_666 . . C102 C103 C104 116.6(2) . . . C103 C104 C105 120.3(2) . . . N101 C105 C104 121.4(2) . . . N101 C101 H101 119.58 . . . C102 C101 H101 119.60 . . . C103 C102 H102 119.46 . . . C101 C102 H102 119.49 . . . C103 C104 H104 119.81 . . . C105 C104 H104 119.86 . . . C104 C105 H105 119.33 . . . N101 C105 H105 119.30 . . . N101 C111 H111 109.50 . . . N101 C111 H131 109.46 . . . H111 C111 H121 109.39 . . . H111 C111 H131 109.54 . . . H121 C111 H131 109.46 . . . N101 C111 H121 109.47 . . . O201 C201 C206 116.97(19) . . . C202 C201 C206 120.6(2) . . . O201 C201 C202 122.48(19) . . . C201 C202 C203 119.7(2) . . . C202 C203 C204 120.4(2) . . . C203 C204 C205 119.5(2) . . . C204 C205 C206 121.9(2) . . . C201 C206 C207 120.0(2) . . . C205 C206 C207 122.1(2) . . . C201 C206 C205 117.9(2) . . . C201 C202 H202 120.18 . . . C203 C202 H202 120.08 . . . C202 C203 H203 119.75 . . . C204 C203 H203 119.84 . . . C203 C204 H204 120.30 . . . C205 C204 H204 120.21 . . . C204 C205 H205 119.05 . . . C206 C205 H205 119.06 . . . C206 C207 H217 109.49 . . . C206 C207 H227 109.44 . . . C206 C207 H237 109.46 . . . H217 C207 H227 109.48 . . . H217 C207 H237 109.49 . . . H227 C207 H237 109.47 . . . 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 C(102) C(103) C(103) C(102) 180.0(2) . . 3_666 3_666 C(102) C(103) C(103) C(104) -0.5(3) . . 3_666 3_666 loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 O201 O1 2.879(2) . 2_545 O201 N4 2.741(3) . . O1 N3 2.889(3) . 4_564 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.395 _refine_diff_density_min -1.004 _refine_diff_density_rms 0.110 #===END #------------------------------------------------------------------------------ data_mcretr _database_code_depnum_ccdc_archive 'CCDC 269965' _audit_creation_method SHELXL-97 _chemical_formula_structural '(C12 H14 N2) (Cd3 C8 N8) (C7 H8 O)1.5 (H2O)2' _chemical_formula_sum 'C30.5 H30 Cd3 N10 O3.5 ' _chemical_formula_weight 929.872 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 'P n a n' _symmetry_Int_Tables_number 52 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,y,-z x,1/2-y,1/2-z 1/2-x,1/2-y,1/2+z -x,-y,-z 1/2+x,-y,z -x,1/2+y,1/2+z 1/2+x,1/2+y,1/2-z _cell_length_a 15.1715(5) _cell_length_b 16.6564(4) _cell_length_c 29.3251(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7410.5(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 114612 _cell_measurement_theta_min 1.22 _cell_measurement_theta_max 30.03 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_diffrn 1.666 _exptl_crystal_F_000 3640 _exptl_absorpt_coefficient_mu 1.742 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9378 _exptl_absorpt_correction_T_max 0.9606 _exptl_absorpt_process_details 'PROCESS-AUTO, RIGAKU Co., Tokyo, Japan(1998)' _exptl_special_details ; ? ; _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_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_reflns_number 99757 _diffrn_reflns_av_R_equivalents 0.0832 _diffrn_reflns_av_sigmaI/netI 0.1065 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 30.03 _reflns_number_total 10849 _reflns_number_gt 5030 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Space group. For easy comparison with the crystal structure of other related compounds, a non-standard setting space group Pnan was adopted. Structural disorder. One m-cresol molecule(C301, C302, C303, C304, C305, O301) sits on a twofold rotation axis, so that its methyl group(C305) and hydroxy group(O301) occupy the same positions, which are related with the twofold rotation axis, with an occupancy factor of 1/2. ; _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^)+(0.0380P)^2^+0.0P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 10849 _refine_ls_number_parameters 430 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1025 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.1160 _refine_ls_wR_factor_gt 0.0969 _refine_ls_goodness_of_fit_ref 0.786 _refine_ls_restrained_S_all 0.787 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.43528(2) 0.13337(2) 0.400933(12) 0.04271(9) Uani 1 1 d . . . Cd2 Cd 0.2500 0.36992(3) 0.5000 0.03833(11) Uani 1 2 d S . . Cd3 Cd 0.41908(2) 0.62985(2) 0.413964(13) 0.04376(10) Uani 1 1 d . . . Cd4 Cd 0.2500 0.89031(3) 0.5000 0.04400(14) Uani 1 2 d S . . C1 C 0.4266(4) 0.1170(4) 0.3268(2) 0.0630(17) Uani 1 1 d . . . N1 N 0.4218(4) 0.1037(4) 0.28966(18) 0.093(2) Uani 1 1 d . . . C2 C 0.5689(3) 0.1173(3) 0.42985(19) 0.0513(13) Uani 1 1 d . . . N2 N 0.6325(3) 0.1075(3) 0.44865(18) 0.0621(13) Uani 1 1 d . . . C3 C 0.3609(4) 0.2305(3) 0.4337(2) 0.0525(14) Uani 1 1 d . . . N3 N 0.3196(3) 0.2731(3) 0.45464(17) 0.0601(13) Uani 1 1 d . . . C4 C 0.4412(3) 0.3660(3) 0.5653(2) 0.0523(13) Uani 1 1 d . . . N4 N 0.3727(3) 0.3647(3) 0.54982(17) 0.0595(12) Uani 1 1 d . . . C5 C 0.3535(3) 0.5235(3) 0.44325(18) 0.0469(13) Uani 1 1 d . . . N5 N 0.3193(3) 0.4703(3) 0.45846(16) 0.0585(13) Uani 1 1 d . . . C6 C 0.4024(4) 0.6310(4) 0.33669(18) 0.0501(13) Uani 1 1 d . . . N6 N 0.3893(5) 0.6367(5) 0.3027(3) 0.117(3) Uani 1 1 d . . . C7 C 0.3540(4) 0.7390(3) 0.4402(2) 0.0512(14) Uani 1 1 d . . . N7 N 0.3203(3) 0.7926(3) 0.45636(17) 0.0607(13) Uani 1 1 d . . . C8 C 0.3607(3) 1.0290(3) 0.4344(2) 0.0493(14) Uani 1 1 d . . . N8 N 0.3250(3) 0.9872(3) 0.45556(18) 0.0637(14) Uani 1 1 d . . . N101 N 0.5665(3) 0.8918(3) 0.41671(15) 0.0573(12) Uani 1 1 d . . . N102 N 0.6818(3) 0.9832(3) 0.19223(17) 0.0601(13) Uani 1 1 d . . . C101 C 0.6485(4) 0.9108(6) 0.4049(2) 0.100(3) Uani 1 1 d . . . H101 H 0.6929 0.9066 0.4266 0.119 Uiso 1 1 calc D . . C102 C 0.6701(4) 0.9361(5) 0.3620(2) 0.090(3) Uani 1 1 d . . . H102 H 0.7277 0.9519 0.3558 0.108 Uiso 1 1 calc . . . C103 C 0.6090(3) 0.9385(3) 0.32854(18) 0.0492(13) Uani 1 1 d . . . C104 C 0.5239(4) 0.9191(4) 0.3413(2) 0.0670(18) Uani 1 1 d . . . H104 H 0.4791 0.9221 0.3197 0.080 Uiso 1 1 calc . . . C105 C 0.5039(4) 0.8957(4) 0.3849(2) 0.0665(17) Uani 1 1 d . . . H105 H 0.4462 0.8824 0.3923 0.080 Uiso 1 1 calc D . . C106 C 0.7403(5) 0.9916(6) 0.2259(3) 0.104(3) Uani 1 1 d . . . H106 H 0.7979 1.0067 0.2191 0.125 Uiso 1 1 calc . . . C107 C 0.7172(4) 0.9784(6) 0.2701(2) 0.097(3) Uani 1 1 d . . . H107 H 0.7596 0.9831 0.2928 0.116 Uiso 1 1 calc . . . C108 C 0.6324(3) 0.9584(3) 0.28175(19) 0.0479(13) Uani 1 1 d . . . C109 C 0.5727(4) 0.9547(4) 0.2465(2) 0.0684(17) Uani 1 1 d . . . H109 H 0.5138 0.9435 0.2526 0.082 Uiso 1 1 calc . . . C110 C 0.5992(5) 0.9673(4) 0.2029(2) 0.0748(19) Uani 1 1 d . . . H110 H 0.5575 0.9647 0.1796 0.090 Uiso 1 1 calc . . . C111 C 0.5461(5) 0.8647(4) 0.4636(2) 0.085(2) Uani 1 1 d . . . H111 H 0.5529 0.8075 0.4655 0.127 Uiso 1 1 calc RD . . H121 H 0.4865 0.8789 0.4711 0.127 Uiso 1 1 calc R . . H131 H 0.5857 0.8901 0.4847 0.127 Uiso 1 1 calc R . . C112 C 0.7088(5) 0.9929(4) 0.1442(2) 0.088(2) Uani 1 1 d . . . H112 H 0.6667 0.9669 0.1247 0.132 Uiso 1 1 calc R . . H122 H 0.7658 0.9690 0.1398 0.132 Uiso 1 1 calc R . . H132 H 0.7116 1.0490 0.1368 0.132 Uiso 1 1 calc R . . O201 O 0.4180(4) 1.1044(4) 0.19528(17) 0.126(2) Uani 1 1 d . . . H201 H 0.4201 1.1120 0.2223 0.189 Uiso 1 1 d . . . C201 C 0.4908(5) 1.1371(4) 0.1741(2) 0.0755(19) Uani 1 1 d . . . C202 C 0.4969(5) 1.1286(4) 0.1276(2) 0.0769(19) Uani 1 1 d . . . H202 H 0.4520 1.1029 0.1117 0.092 Uiso 1 1 calc D . . C203 C 0.5684(5) 1.1577(5) 0.1045(3) 0.084(2) Uani 1 1 d . . . C204 C 0.6335(6) 1.1972(5) 0.1293(4) 0.107(3) Uani 1 1 d . . . H204 H 0.6821 1.2183 0.1142 0.129 Uiso 1 1 calc D . . C205 C 0.6272(6) 1.2056(6) 0.1753(3) 0.111(3) Uani 1 1 d . . . H205 H 0.6713 1.2323 0.1913 0.134 Uiso 1 1 calc . . . C206 C 0.5569(6) 1.1750(5) 0.1979(3) 0.092(2) Uani 1 1 d . . . H206 H 0.5534 1.1797 0.2295 0.110 Uiso 1 1 calc . . . C207 C 0.5769(5) 1.1455(5) 0.0541(3) 0.120(3) Uani 1 1 d . . . H217 H 0.5522 1.1908 0.0384 0.180 Uiso 1 1 calc RD . . H227 H 0.5458 1.0977 0.0454 0.180 Uiso 1 1 calc R . . H237 H 0.6380 1.1402 0.0462 0.180 Uiso 1 1 calc R . . C301 C 0.7010(7) 0.7377(4) 0.2905(3) 0.096(3) Uani 1 1 d . . . C302 C 0.7451(8) 0.7500 0.2500 0.097(4) Uani 1 2 d S . . H302 H 0.8064 0.7500 0.2500 0.117 Uiso 1.00 2 calc SP . . C303 C 0.6118(7) 0.7374(6) 0.2897(5) 0.124(4) Uani 1 1 d . . . H303 H 0.5792 0.7287 0.3161 0.149 Uiso 1 1 calc . . . C304 C 0.5727(13) 0.7500 0.2500 0.163(10) Uani 1 2 d S . . H304 H 0.5114 0.7500 0.2500 0.195 Uiso 1.00 2 calc SP . . C305 C 0.7507(6) 0.7227(5) 0.3302(3) 0.158(3) Uani 0.50 1 d P . . H315 H 0.8136 0.7234 0.3249 0.236 Uiso 0.50 1 d P . . H325 H 0.7354 0.7564 0.3544 0.236 Uiso 0.50 1 d P . . H335 H 0.7378 0.6656 0.3404 0.236 Uiso 0.50 1 d P . . O301 O 0.7507(6) 0.7227(5) 0.3302(3) 0.158(3) Uani 0.50 1 d P . . H331 H 0.7181 0.7117 0.3523 0.236 Uiso 0.50 1 d P . . O401 O 0.2944(9) 0.8931(8) 0.3518(5) 0.091(5) Uani 0.374(9) 1 d P . . O402 O 0.3388(8) 0.8221(10) 0.2887(4) 0.226(8) Uani 0.626(9) 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03830(17) 0.0525(2) 0.03732(17) -0.00150(18) 0.00036(14) 0.00527(19) Cd2 0.0338(2) 0.0407(2) 0.0405(2) 0.000 0.00041(19) 0.000 Cd3 0.03704(17) 0.04599(19) 0.04826(19) 0.00080(18) -0.00048(15) -0.00243(19) Cd4 0.0317(2) 0.0489(3) 0.0514(3) 0.000 0.0004(2) 0.000 C1 0.058(3) 0.086(5) 0.045(3) 0.001(3) 0.004(3) 0.011(3) N1 0.098(5) 0.141(5) 0.039(3) -0.009(3) 0.000(3) 0.006(4) C2 0.040(3) 0.061(4) 0.053(3) -0.002(3) 0.000(2) -0.004(3) N2 0.042(2) 0.077(3) 0.067(3) 0.002(3) -0.011(2) 0.002(2) C3 0.053(4) 0.049(3) 0.055(4) 0.001(3) 0.000(3) 0.009(3) N3 0.056(3) 0.057(3) 0.067(3) -0.004(3) 0.000(3) 0.010(3) C4 0.041(2) 0.059(3) 0.057(3) -0.001(3) -0.001(2) 0.000(3) N4 0.042(2) 0.074(3) 0.063(3) -0.002(3) -0.008(2) 0.000(3) C5 0.047(3) 0.054(3) 0.040(3) 0.001(2) 0.002(2) -0.006(3) N5 0.060(3) 0.061(3) 0.055(3) 0.006(2) 0.002(3) -0.014(3) C6 0.041(3) 0.072(4) 0.038(3) 0.012(3) 0.001(2) -0.003(3) N6 0.080(5) 0.156(7) 0.116(7) 0.018(6) 0.012(5) -0.012(5) C7 0.042(3) 0.051(3) 0.061(4) -0.006(3) 0.002(3) 0.002(3) N7 0.050(3) 0.059(3) 0.073(4) -0.003(3) 0.000(3) 0.002(2) C8 0.041(3) 0.056(3) 0.051(3) -0.003(3) 0.001(3) -0.001(3) N8 0.054(3) 0.064(4) 0.074(4) -0.001(3) -0.004(3) 0.001(3) N101 0.058(3) 0.072(3) 0.041(2) -0.008(2) 0.005(2) -0.014(2) N102 0.063(3) 0.062(3) 0.056(3) 0.002(3) 0.007(3) -0.009(3) C101 0.054(4) 0.183(8) 0.062(4) 0.015(5) -0.015(3) -0.034(5) C102 0.049(3) 0.169(8) 0.053(4) 0.015(5) -0.005(3) -0.034(5) C103 0.044(3) 0.061(3) 0.043(3) -0.007(3) 0.003(2) -0.002(3) C104 0.041(3) 0.104(5) 0.056(4) 0.016(4) 0.002(3) 0.005(4) C105 0.043(3) 0.095(5) 0.062(4) -0.001(4) 0.007(3) 0.001(3) C106 0.057(4) 0.192(8) 0.063(4) 0.021(6) 0.003(4) -0.029(5) C107 0.057(4) 0.180(8) 0.054(4) 0.022(5) -0.003(3) -0.034(5) C108 0.039(3) 0.053(3) 0.052(3) -0.004(3) 0.002(2) 0.000(3) C109 0.043(3) 0.108(5) 0.054(3) 0.009(3) -0.001(3) -0.014(4) C110 0.069(4) 0.105(5) 0.051(4) 0.006(4) -0.011(3) -0.011(4) C111 0.094(5) 0.111(5) 0.050(4) -0.004(4) 0.007(4) -0.022(5) C112 0.107(6) 0.108(5) 0.049(3) 0.013(4) 0.014(4) -0.019(5) O201 0.103(4) 0.228(7) 0.047(3) 0.002(4) 0.006(3) -0.038(5) C201 0.076(4) 0.100(5) 0.051(3) 0.002(4) -0.001(3) 0.001(5) C202 0.087(5) 0.093(5) 0.051(3) -0.008(4) -0.004(3) -0.005(5) C203 0.094(5) 0.091(5) 0.066(5) 0.012(4) 0.017(4) 0.023(5) C204 0.096(6) 0.111(7) 0.115(8) 0.017(6) 0.008(6) -0.022(6) C205 0.118(7) 0.122(7) 0.094(7) -0.008(6) 0.001(6) -0.034(6) C206 0.115(7) 0.101(6) 0.060(4) -0.016(4) -0.005(5) -0.011(5) C207 0.130(7) 0.159(8) 0.070(5) 0.016(5) 0.020(5) 0.024(7) C301 0.149(9) 0.061(5) 0.079(6) -0.002(4) -0.006(6) -0.012(5) C302 0.104(9) 0.089(7) 0.099(10) 0.007(7) 0.000 0.000 C303 0.099(9) 0.075(6) 0.199(15) -0.005(8) 0.043(9) -0.008(6) C304 0.108(15) 0.100(11) 0.28(3) 0.030(17) 0.000 0.000 C305 0.210(9) 0.159(7) 0.103(6) 0.016(6) -0.017(7) -0.029(8) O301 0.210(9) 0.159(7) 0.103(6) 0.016(6) -0.017(7) -0.029(8) O401 0.084(9) 0.109(11) 0.081(10) 0.028(8) -0.026(8) -0.013(8) O402 0.161(12) 0.337(19) 0.179(14) 0.152(13) 0.041(10) 0.034(12) _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cd1 C1 2.195(6) . . Cd1 C2 2.214(5) . . Cd1 C3 2.194(5) . . Cd1 C8 2.295(5) . 1_545 Cd2 N3 2.342(5) . . Cd2 N4 2.368(5) . . Cd2 N5 2.321(5) . . Cd2 N3 2.342(5) . 2_556 Cd2 N4 2.368(5) . 2_556 Cd2 N5 2.321(5) . 2_556 Cd3 C5 2.206(5) . . Cd3 C6 2.280(5) . . Cd3 C7 2.207(5) . . Cd3 C4 2.206(5) . 5_666 Cd4 N7 2.329(5) . . Cd4 N8 2.366(5) . . Cd4 N7 2.329(5) . 2_556 Cd4 N8 2.366(5) . 2_556 Cd4 N2 2.334(5) . 5_666 Cd4 N2 2.334(5) . 6_465 O301 C301 1.409(13) . . O301 H315 0.9669 . . O301 H325 0.9341 . . O201 C201 1.379(9) . . O301 H335 1.0160 . . O301 H331 0.8356 . . O201 H201 0.8030 . . N1 C1 1.114(8) . . N2 C2 1.123(7) . . N3 C3 1.128(7) . . N4 C4 1.134(7) . . N5 C5 1.120(7) . . N6 C6 1.021(10) . . N7 C7 1.133(7) . . N8 C8 1.079(7) . . N101 C111 1.480(7) . . N101 C105 1.333(7) . . N101 C101 1.330(8) . . N102 C106 1.335(10) . . N102 C110 1.319(9) . . N102 C112 1.476(8) . . C101 C102 1.367(9) . . C102 C103 1.350(8) . . C103 C108 1.456(8) . . C103 C104 1.383(8) . . C104 C105 1.371(8) . . C106 C107 1.361(11) . . C107 C108 1.372(8) . . C108 C109 1.376(8) . . C109 C110 1.357(8) . . C101 H101 0.9293 . . C102 H102 0.9306 . . C104 H104 0.9304 . . C105 H105 0.9287 . . C106 H106 0.9310 . . C107 H107 0.9290 . . C109 H109 0.9302 . . C110 H110 0.9322 . . C111 H131 0.9606 . . C111 H121 0.9602 . . C111 H111 0.9599 . . C112 H112 0.9605 . . C112 H132 0.9602 . . C112 H122 0.9607 . . C301 C305 1.409(13) . . C301 C302 1.379(11) . . C301 C303 1.354(15) . . C303 C304 1.323(16) . . C201 C206 1.375(11) . . C201 C202 1.374(8) . . C202 C203 1.368(11) . . C302 H302 0.9300 . . C303 H303 0.9300 . . C203 C204 1.392(13) . . C203 C207 1.498(12) . . C204 C205 1.360(15) . . C304 H304 0.9300 . . C305 H315 0.9669 . . C305 H325 0.9341 . . C305 H335 1.0160 . . C205 C206 1.355(13) . . C305 H331 0.8356 . . C202 H202 0.9299 . . C204 H204 0.9291 . . C205 H205 0.9304 . . C206 H206 0.9315 . . C207 H217 0.9601 . . C207 H227 0.9600 . . C207 H237 0.9596 . . 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_2 _geom_angle_site_symmetry_3 C1 Cd1 C2 114.8(2) . . . C1 Cd1 C3 119.6(2) . . . C1 Cd1 C8 107.5(2) . . 1_545 C2 Cd1 C3 113.1(2) . . . C2 Cd1 C8 101.31(18) . . 1_545 C3 Cd1 C8 96.76(19) . . 1_545 N3 Cd2 N4 88.32(17) . . . N3 Cd2 N5 89.64(17) . . . N3 Cd2 N3 92.97(17) . . 2_556 N3 Cd2 N4 88.78(17) . . 2_556 N3 Cd2 N5 176.93(17) . . 2_556 N4 Cd2 N5 89.67(16) . . . N3 Cd2 N4 88.78(17) 2_556 . . N4 Cd2 N4 175.79(17) . . 2_556 N4 Cd2 N5 93.37(16) . . 2_556 N3 Cd2 N5 176.93(17) 2_556 . . N4 Cd2 N5 93.37(17) 2_556 . . N5 Cd2 N5 87.81(17) . . 2_556 N3 Cd2 N4 88.32(17) 2_556 . 2_556 N3 Cd2 N5 89.64(17) 2_556 . 2_556 N4 Cd2 N5 89.67(16) 2_556 . 2_556 C5 Cd3 C6 110.1(2) . . . C5 Cd3 C7 108.9(2) . . . C4 Cd3 C5 110.56(18) 5_666 . . C6 Cd3 C7 106.9(2) . . . C4 Cd3 C6 112.4(2) 5_666 . . C4 Cd3 C7 107.9(2) 5_666 . . N7 Cd4 N8 87.35(17) . . . N7 Cd4 N7 91.34(17) . . 2_556 N7 Cd4 N8 178.37(16) . . 2_556 N2 Cd4 N7 90.90(17) 5_666 . . N2 Cd4 N7 90.35(17) 6_465 . . N7 Cd4 N8 178.37(16) 2_556 . . N8 Cd4 N8 93.98(17) . . 2_556 N2 Cd4 N8 88.70(17) 5_666 . . N2 Cd4 N8 90.07(17) 6_465 . . N7 Cd4 N8 87.35(17) 2_556 . 2_556 N2 Cd4 N7 90.35(17) 5_666 . 2_556 N2 Cd4 N7 90.90(17) 6_465 . 2_556 N2 Cd4 N8 90.07(17) 5_666 . 2_556 N2 Cd4 N8 88.70(17) 6_465 . 2_556 N2 Cd4 N2 178.21(18) 5_666 . 6_465 H325 O301 H335 106.92 . . . H331 O301 H335 56.80 . . . C301 O301 H331 111.28 . . . C301 O301 H335 107.82 . . . H315 O301 H325 111.11 . . . H315 O301 H331 135.36 . . . H315 O301 H335 104.40 . . . C301 O301 H315 113.15 . . . C301 O301 H325 112.84 . . . H325 O301 H331 52.80 . . . C201 O201 H201 110.51 . . . Cd4 N2 C2 166.1(5) 5_666 . . Cd2 N3 C3 173.0(5) . . . Cd2 N4 C4 165.1(5) . . . Cd2 N5 C5 171.7(4) . . . Cd4 N7 C7 170.9(5) . . . Cd4 N8 C8 177.2(5) . . . C105 N101 C111 121.1(5) . . . C101 N101 C111 120.7(5) . . . C101 N101 C105 118.2(5) . . . C110 N102 C112 120.8(5) . . . C106 N102 C112 120.7(6) . . . C106 N102 C110 118.5(6) . . . Cd1 C1 N1 175.7(6) . . . Cd1 C2 N2 172.9(5) . . . Cd1 C3 N3 171.0(5) . . . Cd3 C4 N4 172.4(5) 5_666 . . Cd3 C5 N5 178.9(4) . . . Cd3 C6 N6 173.1(7) . . . Cd3 C7 N7 175.5(5) . . . Cd1 C8 N8 169.4(5) 1_565 . . N101 C101 C102 122.5(5) . . . C101 C102 C103 120.9(6) . . . C102 C103 C104 115.9(5) . . . C102 C103 C108 121.6(5) . . . C104 C103 C108 122.4(5) . . . C103 C104 C105 121.7(5) . . . N101 C105 C104 120.6(6) . . . N102 C106 C107 121.1(7) . . . C106 C107 C108 121.2(6) . . . C103 C108 C109 122.5(5) . . . C103 C108 C107 121.2(5) . . . C107 C108 C109 116.2(5) . . . C108 C109 C110 120.4(6) . . . N102 C110 C109 122.4(6) . . . C102 C101 H101 118.67 . . . N101 C101 H101 118.81 . . . C101 C102 H102 119.49 . . . C103 C102 H102 119.62 . . . C103 C104 H104 119.04 . . . C105 C104 H104 119.25 . . . C104 C105 H105 119.63 . . . N101 C105 H105 119.77 . . . N102 C106 H106 119.60 . . . C107 C106 H106 119.31 . . . C108 C107 H107 119.42 . . . C106 C107 H107 119.38 . . . C108 C109 H109 119.80 . . . C110 C109 H109 119.80 . . . N102 C110 H110 118.71 . . . C109 C110 H110 118.85 . . . N101 C111 H121 109.55 . . . H111 C111 H131 109.42 . . . N101 C111 H131 109.47 . . . N101 C111 H111 109.52 . . . H111 C111 H121 109.41 . . . H121 C111 H131 109.45 . . . N102 C112 H122 109.43 . . . H112 C112 H132 109.49 . . . N102 C112 H132 109.54 . . . H112 C112 H122 109.38 . . . N102 C112 H112 109.53 . . . H122 C112 H132 109.45 . . . C302 C301 C305 118.6(9) . . . C303 C301 C305 123.3(10) . . . O301 C301 C303 123.3(10) . . . C302 C301 C303 118.1(10) . . . O301 C301 C302 118.6(9) . . . C301 C302 C301 121.9(11) . . 3_565 C301 C303 C304 117.6(13) . . . C303 C304 C303 126.7(17) . . 3_565 C202 C201 C206 120.1(7) . . . O201 C201 C206 122.5(6) . . . O201 C201 C202 117.4(6) . . . C301 C302 H302 119.04 . . . C201 C202 C203 120.6(7) . . . C301 C302 H302 119.04 3_565 . . C204 C203 C207 121.3(8) . . . C202 C203 C204 118.1(8) . . . C202 C203 C207 120.6(7) . . . C301 C303 H303 121.19 . . . C304 C303 H303 121.24 . . . C203 C204 C205 121.1(9) . . . C303 C304 H304 116.63 3_565 . . C303 C304 H304 116.63 . . . H325 C305 H335 106.92 . . . C301 C305 H335 107.82 . . . H315 C305 H325 111.11 . . . H331 C305 H335 56.80 . . . H315 C305 H335 104.40 . . . H325 C305 H331 52.80 . . . C301 C305 H315 113.15 . . . C301 C305 H325 112.84 . . . C301 C305 H331 111.28 . . . C204 C205 C206 120.1(9) . . . H315 C305 H331 135.36 . . . C201 C206 C205 119.9(8) . . . C201 C202 H202 119.72 . . . C203 C202 H202 119.72 . . . C203 C204 H204 119.53 . . . C205 C204 H204 119.32 . . . C204 C205 H205 119.94 . . . C206 C205 H205 119.94 . . . C201 C206 H206 120.12 . . . C205 C206 H206 119.98 . . . C203 C207 H217 109.45 . . . C203 C207 H227 109.42 . . . C203 C207 H237 109.51 . . . H217 C207 H227 109.42 . . . H217 C207 H237 109.49 . . . H227 C207 H237 109.53 . . . 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 C102 C103 C108 C107 -2.4(9) . . . . C102 C103 C108 C109 174.5(6) . . . . C104 C103 C108 C107 -179.2(7) . . . . C104 C103 C108 C109 -3.9(8) . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 O201 N1 2.768(7) . 1_565 O201 C106 3.261(10) . 6_475 O401 O402 2.18(2) . . O402 N6 2.871(15) . 3_565 O402 N6 3.208(18) . . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.633 _refine_diff_density_min -0.792 _refine_diff_density_rms 0.193 #===END #------------------------------------------------------------------------------ data_pcresol1 _database_code_depnum_ccdc_archive 'CCDC 269966' _audit_creation_method SHELXL-97 _chemical_formula_structural '(C12 H14 N2) (Cd3 (CN)7 Cl) (C7 H8 O)2' _chemical_formula_sum 'C33 H30 Cd3 Cl N9 O2' _chemical_formula_weight 957.346 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' 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 'P c a 21' _symmetry_Int_Tables_number 29 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,1/2+z 1/2-x,y,1/2+z 1/2+x,-y,z _cell_length_a 14.7068(3) _cell_length_b 8.70830(10) _cell_length_c 29.9347(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3833.77(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 63005 _cell_measurement_theta_min 1.38 _cell_measurement_theta_max 30.03 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.230 _exptl_crystal_size_min 0.220 _exptl_crystal_density_diffrn 1.659 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 1.749 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8302 _exptl_absorpt_correction_T_max 1.1334 _exptl_absorpt_process_details 'PROCESS-AUTO, RIGAKU Co., Tokyo, Japan(1998)' _exptl_special_details ; ? ; _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_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_reflns_number 39325 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0494 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 30.03 _reflns_number_total 5710 _reflns_number_gt 4035 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0352P)^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 mixed _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.06(4) _refine_ls_number_reflns 5710 _refine_ls_number_parameters 437 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0755 _refine_ls_wR_factor_gt 0.0715 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.914 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.92085(3) 0.22860(5) 0.088926(13) 0.04018(11) Uani 1 1 d . . . Cd2 Cd 0.75885(3) 0.72882(4) -0.00060(2) 0.03766(9) Uani 1 1 d . . . Cd3 Cd 0.59571(3) 1.23540(5) -0.089961(14) 0.03941(11) Uani 1 1 d . . . Cl Cl 0.58748(18) 1.2496(3) -0.17241(9) 0.0750(7) Uani 1 1 d . . . C1 C 0.9414(6) 0.2354(8) 0.1647(3) 0.0492(18) Uani 1 1 d . . . N1 N 0.9507(9) 0.2373(10) 0.1983(3) 0.120(4) Uani 1 1 d . . . C2 C 0.8490(5) 0.4313(8) 0.0611(3) 0.0471(16) Uani 1 1 d . . . N2 N 0.8179(4) 0.5336(7) 0.0431(2) 0.0533(16) Uani 1 1 d . . . C3 C 1.0560(5) 0.2397(9) 0.0557(3) 0.0540(19) Uani 1 1 d . . . N3 N 1.1222(5) 0.2529(7) 0.0365(3) 0.0595(18) Uani 1 1 d . . . C4 C 0.8554(5) 0.0180(8) 0.0633(3) 0.0465(17) Uani 1 1 d . . . N4 N 0.8226(4) -0.0825(8) 0.0444(2) 0.0542(16) Uani 1 1 d . . . C5 C 0.6623(5) 1.0212(8) -0.0663(3) 0.0451(16) Uani 1 1 d . . . N5 N 0.6967(4) 0.9197(7) -0.0515(2) 0.0530(15) Uani 1 1 d . . . C6 C 0.9568(5) 0.7466(9) -0.0625(3) 0.0487(17) Uani 1 1 d . . . N6 N 0.8881(5) 0.7398(8) -0.0458(2) 0.0566(17) Uani 1 1 d . . . C7 C 0.6734(5) 1.4373(9) -0.0653(3) 0.0524(18) Uani 1 1 d . . . N7 N 0.7045(4) 1.5400(7) -0.0501(2) 0.0591(17) Uani 1 1 d . . . C101 C 0.6102(8) 0.6015(10) -0.2740(3) 0.079(3) Uani 1 1 d . . . H101 H 0.6332 0.5070 -0.2830 0.095 Uiso 1 1 calc D . . C102 C 0.5791(6) 0.6198(9) -0.2316(3) 0.067(2) Uani 1 1 d . . . H102 H 0.5811 0.5380 -0.2116 0.080 Uiso 1 1 calc . . . C103 C 0.5438(5) 0.7623(7) -0.2178(3) 0.0486(15) Uani 1 1 d . . . C104 C 0.5411(5) 0.8776(7) -0.2499(4) 0.0641(17) Uani 1 1 d . . . H104 H 0.5162 0.9726 -0.2427 0.077 Uiso 1 1 calc . . . C105 C 0.5737(6) 0.8541(9) -0.2911(3) 0.070(2) Uani 1 1 d . . . H105 H 0.5725 0.9333 -0.3120 0.084 Uiso 1 1 calc . . . C106 C 0.5089(4) 0.7135(8) -0.0950(3) 0.0562(17) Uani 1 1 d . . . H106 H 0.5311 0.6535 -0.0717 0.067 Uiso 1 1 calc . . . C107 C 0.5426(5) 0.6938(8) -0.1363(2) 0.0522(16) Uani 1 1 d . . . H107 H 0.5876 0.6208 -0.1414 0.063 Uiso 1 1 calc . . . C108 C 0.5101(4) 0.7832(6) -0.1720(2) 0.0429(13) Uani 1 1 d . . . C109 C 0.4459(5) 0.8938(8) -0.1616(2) 0.0583(19) Uani 1 1 d . . . H109 H 0.4247 0.9595 -0.1838 0.070 Uiso 1 1 calc . . . C110 C 0.4130(5) 0.9070(8) -0.1184(3) 0.063(2) Uani 1 1 d . . . H110 H 0.3687 0.9797 -0.1118 0.075 Uiso 1 1 calc D . . C111 C 0.6477(10) 0.6943(13) -0.3475(3) 0.110(4) Uani 1 1 d . . . H111 H 0.6324 0.5937 -0.3582 0.165 Uiso 1 1 calc RD . . H121 H 0.7126 0.7043 -0.3459 0.165 Uiso 1 1 calc R . . H131 H 0.6238 0.7702 -0.3676 0.165 Uiso 1 1 calc R . . C112 C 0.4073(6) 0.8322(11) -0.0398(3) 0.077(3) Uani 1 1 d . . . H112 H 0.3881 0.9362 -0.0349 0.116 Uiso 1 1 calc RD . . H122 H 0.4537 0.8058 -0.0186 0.116 Uiso 1 1 calc R . . H132 H 0.3564 0.7644 -0.0362 0.116 Uiso 1 1 calc R . . N102 N 0.4447(4) 0.8167(7) -0.0866(2) 0.0569(15) Uani 1 1 d . . . N101 N 0.6081(5) 0.7170(8) -0.3025(2) 0.0708(18) Uani 1 1 d . . . C201 C 0.7582(5) 0.9512(8) -0.2192(3) 0.0570(17) Uani 1 1 d . . . C202 C 0.7367(4) 0.9081(7) -0.1761(3) 0.0541(16) Uani 1 1 d . . . H202 H 0.7015 0.9718 -0.1581 0.065 Uiso 1 1 calc . . . C203 C 0.7682(5) 0.7696(9) -0.1599(3) 0.0580(19) Uani 1 1 d . . . H203 H 0.7542 0.7410 -0.1308 0.070 Uiso 1 1 calc D . . C204 C 0.8194(6) 0.6731(9) -0.1859(3) 0.068(2) Uani 1 1 d . . . C205 C 0.8418(7) 0.7189(11) -0.2279(3) 0.079(3) Uani 1 1 d . . . H205 H 0.8776 0.6554 -0.2457 0.094 Uiso 1 1 calc . . . C206 C 0.8121(6) 0.8587(10) -0.2449(3) 0.073(2) Uani 1 1 d . . . H206 H 0.8288 0.8891 -0.2735 0.088 Uiso 1 1 calc . . . C207 C 0.8524(8) 0.5204(12) -0.1676(4) 0.111(4) Uani 1 1 d . . . H207 H 0.8579 0.4479 -0.1916 0.166 Uiso 1 1 calc R . . H217 H 0.8096 0.4827 -0.1460 0.166 Uiso 1 1 calc RD . . H227 H 0.9105 0.5342 -0.1536 0.166 Uiso 1 1 calc R . . O201 O 0.7288(4) 1.0878(6) -0.23757(19) 0.0868(19) Uani 1 1 d . . . H201 H 0.6973 1.1338 -0.2194 0.130 Uiso 1 1 calc . . . C301 C 0.3449(7) 0.6945(10) -0.3186(3) 0.080(3) Uani 1 1 d . . . C302 C 0.3251(7) 0.8269(11) -0.3399(3) 0.085(3) Uani 1 1 d . . . H302 H 0.2941 0.9043 -0.3248 0.102 Uiso 1 1 calc . . . C303 C 0.3505(6) 0.8479(11) -0.3835(3) 0.082(2) Uani 1 1 d . . . H303 H 0.3372 0.9409 -0.3973 0.099 Uiso 1 1 calc D . . C304 C 0.3946(7) 0.7367(11) -0.4073(4) 0.079(3) Uani 1 1 d . . . C305 C 0.4121(8) 0.6021(12) -0.3845(4) 0.114(4) Uani 1 1 d . . . H305 H 0.4424 0.5233 -0.3993 0.137 Uiso 1 1 calc . . . C306 C 0.3866(9) 0.5798(11) -0.3406(4) 0.109(4) Uani 1 1 d . . . H306 H 0.3980 0.4867 -0.3265 0.131 Uiso 1 1 calc . . . C307 C 0.4213(10) 0.7586(14) -0.4549(4) 0.121(6) Uani 1 1 d . . . H307 H 0.3824 0.8338 -0.4684 0.181 Uiso 1 1 calc RD . . H317 H 0.4156 0.6629 -0.4706 0.181 Uiso 1 1 calc R . . H327 H 0.4833 0.7932 -0.4563 0.181 Uiso 1 1 calc R . . O301 O 0.3193(7) 0.6660(9) -0.2761(3) 0.135(3) Uani 1 1 d . . . H301 H 0.2706 0.7084 -0.2711 0.203 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 0.0471(2) 0.0338(2) 0.0396(2) -0.0001(4) -0.0002(2) -0.00236(18) Cd2 0.0374(2) 0.03164(14) 0.04397(18) 0.0003(4) -0.00243(19) -0.00107(18) Cd3 0.0407(2) 0.0313(2) 0.0463(3) 0.0006(3) -0.0001(2) 0.00063(17) Cl 0.1089(17) 0.0600(12) 0.0562(12) 0.0061(11) 0.0021(12) 0.0173(11) C1 0.065(4) 0.033(3) 0.049(4) 0.008(3) -0.011(3) -0.014(3) N1 0.216(12) 0.084(6) 0.061(5) 0.007(4) -0.035(7) -0.027(6) C2 0.053(4) 0.039(4) 0.049(4) 0.001(3) -0.007(3) 0.000(3) N2 0.062(4) 0.043(4) 0.054(4) 0.005(3) -0.005(3) 0.003(3) C3 0.041(3) 0.051(4) 0.069(5) -0.002(4) 0.008(4) -0.007(3) N3 0.054(4) 0.051(4) 0.073(4) -0.012(3) 0.011(3) -0.001(3) C4 0.055(4) 0.039(4) 0.045(4) 0.001(3) 0.003(3) -0.007(3) N4 0.061(4) 0.049(4) 0.053(4) -0.002(3) 0.002(3) -0.007(3) C5 0.050(4) 0.039(4) 0.047(4) -0.001(3) 0.003(3) 0.001(3) N5 0.066(4) 0.040(3) 0.052(4) 0.010(3) 0.000(3) 0.013(3) C6 0.039(3) 0.055(4) 0.053(4) 0.001(3) 0.001(3) -0.005(3) N6 0.052(3) 0.061(4) 0.057(4) -0.004(3) -0.001(3) -0.004(3) C7 0.057(4) 0.037(4) 0.064(5) -0.006(4) -0.009(4) -0.001(3) N7 0.063(4) 0.043(4) 0.072(5) -0.005(3) -0.006(3) -0.007(3) C101 0.139(8) 0.045(4) 0.053(5) -0.003(4) 0.005(5) 0.008(5) C102 0.097(6) 0.042(4) 0.060(5) 0.005(3) -0.007(5) 0.003(4) C103 0.054(4) 0.037(3) 0.055(4) 0.005(3) -0.011(3) 0.000(3) C104 0.088(5) 0.042(3) 0.062(4) 0.013(5) -0.012(5) 0.006(3) C105 0.102(6) 0.059(4) 0.049(4) 0.015(4) -0.007(5) -0.003(4) C106 0.052(3) 0.061(4) 0.055(4) 0.013(4) -0.010(3) 0.011(3) C107 0.054(4) 0.052(4) 0.051(4) 0.008(3) -0.004(3) 0.012(3) C108 0.050(3) 0.036(3) 0.043(3) 0.004(3) -0.009(3) -0.001(3) C109 0.067(5) 0.045(4) 0.063(5) 0.005(3) -0.015(4) 0.011(3) C110 0.071(5) 0.058(4) 0.059(4) -0.002(4) -0.016(4) 0.025(4) C111 0.177(12) 0.108(8) 0.045(5) 0.005(6) 0.016(6) 0.002(9) C112 0.092(7) 0.090(6) 0.049(4) -0.003(5) -0.006(4) 0.028(5) N102 0.057(3) 0.059(3) 0.055(4) -0.001(3) -0.010(3) 0.008(3) N101 0.098(5) 0.067(4) 0.047(3) -0.007(3) -0.002(4) -0.002(4) C201 0.052(4) 0.060(4) 0.059(4) -0.005(4) 0.007(3) -0.001(3) C202 0.048(4) 0.054(4) 0.060(4) -0.010(3) 0.002(3) 0.005(3) C203 0.059(4) 0.064(4) 0.052(4) 0.005(3) -0.001(3) -0.005(4) C204 0.068(5) 0.062(4) 0.073(6) -0.013(4) -0.010(4) 0.019(4) C205 0.087(6) 0.090(6) 0.059(5) -0.019(5) -0.003(5) 0.028(5) C206 0.079(5) 0.097(5) 0.045(5) 0.007(5) 0.010(4) 0.007(4) C207 0.129(9) 0.103(8) 0.100(8) 0.007(7) -0.010(7) 0.053(7) O201 0.109(5) 0.073(3) 0.078(5) 0.022(3) 0.029(3) 0.010(3) C301 0.106(7) 0.072(5) 0.062(5) 0.007(5) 0.023(5) 0.024(5) C302 0.113(8) 0.069(6) 0.074(6) 0.005(5) 0.017(5) 0.038(6) C303 0.097(6) 0.070(6) 0.080(6) 0.006(5) -0.001(6) 0.009(5) C304 0.081(6) 0.093(7) 0.062(5) -0.020(6) -0.002(5) -0.002(5) C305 0.142(10) 0.073(6) 0.127(10) -0.029(7) 0.027(9) 0.028(6) C306 0.142(10) 0.062(6) 0.124(10) 0.008(6) 0.035(8) 0.029(6) C307 0.116(12) 0.155(15) 0.091(10) -0.010(8) 0.011(7) -0.013(8) O301 0.209(9) 0.099(5) 0.097(6) 0.016(5) 0.050(6) 0.056(6) _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cd1 C1 2.289(9) . . Cd1 C2 2.220(7) . . Cd1 C3 2.225(8) . . Cd1 C4 2.209(7) . . Cd2 N2 2.314(6) . . Cd2 N5 2.433(6) . . Cd2 N6 2.335(7) . . Cd2 N7 2.353(6) . 1_545 Cd2 N4 2.322(7) . 1_565 Cd2 N3 2.302(8) . 4_465 Cd3 Cl 2.474(3) . . Cd3 C5 2.223(7) . . Cd3 C7 2.223(8) . . Cd3 C6 2.208(8) . 4_475 O201 C201 1.380(9) . . O201 H201 0.8191 . . O301 C301 1.350(13) . . N1 C1 1.015(13) . . O301 H301 0.8196 . . N2 C2 1.137(10) . . N3 C3 1.136(11) . . N4 C4 1.148(10) . . N5 C5 1.111(10) . . N6 C6 1.129(10) . . N7 C7 1.103(10) . . N101 C111 1.481(12) . . N101 C105 1.341(11) . . N101 C101 1.319(11) . . N102 C106 1.328(9) . . N102 C110 1.320(10) . . N102 C112 1.511(11) . . C101 C102 1.359(13) . . C102 C103 1.407(10) . . C103 C108 1.469(11) . . C103 C104 1.390(12) . . C104 C105 1.339(14) . . C106 C107 1.343(11) . . C107 C108 1.406(9) . . C108 C109 1.384(9) . . C109 C110 1.386(11) . . C101 H101 0.9296 . . C102 H102 0.9310 . . C104 H104 0.9300 . . C105 H105 0.9314 . . C106 H106 0.9306 . . C107 H107 0.9303 . . C109 H109 0.9307 . . C110 H110 0.9297 . . C111 H121 0.9596 . . C111 H131 0.9604 . . C111 H111 0.9595 . . C112 H112 0.9599 . . C112 H122 0.9598 . . C112 H132 0.9595 . . C201 C206 1.367(12) . . C201 C202 1.380(12) . . C202 C203 1.380(10) . . C203 C204 1.371(12) . . C204 C205 1.360(13) . . C204 C207 1.518(14) . . C205 C206 1.390(13) . . C202 H202 0.9306 . . C203 H203 0.9291 . . C205 H205 0.9311 . . C206 H206 0.9292 . . C207 H227 0.9593 . . C207 H207 0.9598 . . C207 H217 0.9602 . . C301 C306 1.344(14) . . C301 C302 1.349(13) . . C302 C303 1.370(13) . . C303 C304 1.366(14) . . C304 C307 1.490(17) . . C304 C305 1.381(15) . . C305 C306 1.380(17) . . C302 H302 0.9308 . . C303 H303 0.9299 . . C305 H305 0.9305 . . C306 H306 0.9293 . . C307 H307 0.9589 . . C307 H317 0.9604 . . C307 H327 0.9612 . . 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_2 _geom_angle_site_symmetry_3 C1 Cd1 C2 114.5(3) . . . C1 Cd1 C3 108.9(3) . . . C1 Cd1 C4 115.0(3) . . . C2 Cd1 C3 102.9(3) . . . C2 Cd1 C4 108.8(3) . . . C3 Cd1 C4 105.7(3) . . . N2 Cd2 N5 175.4(2) . . . N2 Cd2 N6 93.0(2) . . . N2 Cd2 N7 88.3(2) . . 1_545 N2 Cd2 N4 92.3(2) . . 1_565 N2 Cd2 N3 96.1(2) . . 4_465 N5 Cd2 N6 85.1(2) . . . N5 Cd2 N7 87.5(2) . . 1_545 N4 Cd2 N5 91.8(2) 1_565 . . N3 Cd2 N5 85.8(2) 4_465 . . N6 Cd2 N7 86.6(2) . . 1_545 N4 Cd2 N6 88.8(2) 1_565 . . N3 Cd2 N6 170.9(3) 4_465 . . N4 Cd2 N7 175.3(2) 1_565 . 1_545 N3 Cd2 N7 93.2(2) 4_465 . 1_545 N3 Cd2 N4 91.4(2) 4_465 . 1_565 Cl Cd3 C5 112.4(2) . . . Cl Cd3 C7 108.5(2) . . . Cl Cd3 C6 108.8(2) . . 4_475 C5 Cd3 C7 109.4(3) . . . C5 Cd3 C6 110.4(3) . . 4_475 C6 Cd3 C7 107.2(3) 4_475 . . C201 O201 H201 109.52 . . . C301 O301 H301 109.45 . . . Cd2 N2 C2 173.9(6) . . . Cd2 N3 C3 177.6(7) 4_565 . . Cd2 N4 C4 174.0(6) 1_545 . . Cd2 N5 C5 164.7(6) . . . Cd2 N6 C6 170.9(6) . . . Cd2 N7 C7 165.3(6) 1_565 . . C101 N101 C105 121.5(7) . . . C101 N101 C111 118.5(8) . . . C105 N101 C111 119.9(7) . . . C106 N102 C112 119.7(7) . . . C106 N102 C110 121.2(7) . . . C110 N102 C112 119.1(6) . . . Cd1 C1 N1 179.4(9) . . . Cd1 C2 N2 172.9(7) . . . Cd1 C3 N3 174.8(7) . . . Cd1 C4 N4 170.8(7) . . . Cd3 C5 N5 174.7(7) . . . Cd3 C6 N6 175.5(7) 4_575 . . Cd3 C7 N7 172.6(7) . . . N101 C101 C102 120.5(8) . . . C101 C102 C103 120.1(8) . . . C102 C103 C104 116.4(8) . . . C102 C103 C108 120.5(7) . . . C104 C103 C108 123.1(6) . . . C103 C104 C105 121.1(7) . . . N101 C105 C104 120.4(7) . . . N102 C106 C107 121.6(7) . . . C106 C107 C108 120.2(6) . . . C103 C108 C109 121.8(5) . . . C103 C108 C107 121.7(5) . . . C107 C108 C109 116.5(6) . . . C108 C109 C110 120.4(6) . . . N102 C110 C109 120.0(7) . . . N101 C101 H101 119.74 . . . C102 C101 H101 119.81 . . . C103 C102 H102 119.84 . . . C101 C102 H102 120.03 . . . C105 C104 H104 119.37 . . . C103 C104 H104 119.57 . . . N101 C105 H105 119.71 . . . C104 C105 H105 119.92 . . . C107 C106 H106 119.26 . . . N102 C106 H106 119.19 . . . C108 C107 H107 119.70 . . . C106 C107 H107 120.06 . . . C108 C109 H109 119.71 . . . C110 C109 H109 119.90 . . . C109 C110 H110 119.97 . . . N102 C110 H110 120.00 . . . N101 C111 H131 109.52 . . . H111 C111 H121 109.44 . . . H111 C111 H131 109.47 . . . H121 C111 H131 109.44 . . . N101 C111 H121 109.49 . . . N101 C111 H111 109.47 . . . N102 C112 H132 109.46 . . . N102 C112 H112 109.45 . . . H112 C112 H132 109.51 . . . H122 C112 H132 109.45 . . . N102 C112 H122 109.44 . . . H112 C112 H122 109.52 . . . C202 C201 C206 119.9(7) . . . O201 C201 C202 122.4(7) . . . O201 C201 C206 117.7(8) . . . C201 C202 C203 119.3(7) . . . C202 C203 C204 121.4(8) . . . C203 C204 C207 120.5(8) . . . C205 C204 C207 120.9(8) . . . C203 C204 C205 118.6(8) . . . C204 C205 C206 121.3(9) . . . C201 C206 C205 119.5(8) . . . C201 C202 H202 120.43 . . . C203 C202 H202 120.28 . . . C204 C203 H203 119.32 . . . C202 C203 H203 119.30 . . . C204 C205 H205 119.47 . . . C206 C205 H205 119.23 . . . C205 C206 H206 120.25 . . . C201 C206 H206 120.26 . . . C204 C207 H207 109.45 . . . C204 C207 H227 109.43 . . . H207 C207 H217 109.53 . . . H207 C207 H227 109.53 . . . H217 C207 H227 109.42 . . . C204 C207 H217 109.45 . . . O301 C301 C306 116.9(9) . . . C302 C301 C306 120.1(9) . . . O301 C301 C302 122.8(9) . . . C301 C302 C303 120.4(9) . . . C302 C303 C304 122.1(9) . . . C303 C304 C305 115.6(10) . . . C303 C304 C307 122.2(9) . . . C305 C304 C307 122.2(10) . . . C304 C305 C306 122.7(10) . . . C301 C306 C305 119.1(9) . . . C301 C302 H302 119.67 . . . C303 C302 H302 119.97 . . . C302 C303 H303 118.83 . . . C304 C303 H303 119.05 . . . C304 C305 H305 118.69 . . . C306 C305 H305 118.66 . . . C301 C306 H306 120.53 . . . C305 C306 H306 120.41 . . . C304 C307 H307 109.46 . . . C304 C307 H317 109.50 . . . C304 C307 H327 109.37 . . . H307 C307 H317 109.53 . . . H307 C307 H327 109.48 . . . H317 C307 H327 109.48 . . . 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 C102 C103 C108 C107 26.2(10) . . . . C102 C103 C108 C109 -155.0(7) . . . . C104 C103 C108 C107 -155.4(7) . . . . C104 C103 C108 C109 23.4(10) . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Cl O201 3.180(6) . . O201 O301 2.78(1) . 4_575 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.400 _refine_diff_density_min -0.469 _refine_diff_density_rms 0.112 #===END #------------------------------------------------------------------------------ data_meth1 _database_code_depnum_ccdc_archive 'CCDC 269967' _audit_creation_method SHELXL-97 _chemical_formula_structural '(C12 H14 N2) (Cd3 (C N)6.384 Cl1.616) (C11H10)' _chemical_formula_sum 'C29.384 H24 Cd3 Cl1.616 N8.384' _chemical_formula_weight 889.079 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' 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 'P n m a' _symmetry_Int_Tables_number 62 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,-y,1/2+z 1/2+x,1/2-y,1/2-z -x,1/2+y,-z -x,-y,-z 1/2+x,y,1/2-z 1/2-x,1/2+y,1/2+z x,1/2-y,z _cell_length_a 15.5633(2) _cell_length_b 8.77990(10) _cell_length_c 24.8873(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3400.71(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 106415 _cell_measurement_theta_min 0.82 _cell_measurement_theta_max 30.03 _exptl_crystal_description orange _exptl_crystal_colour needle _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.737 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1721.856 _exptl_absorpt_coefficient_mu 2.005 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8835 _exptl_absorpt_correction_T_max 1.0598 _exptl_absorpt_process_details 'PROCESS-AUTO, RIGAKU Co., Tokyo, Japan(1998)' _exptl_special_details ; ? ; _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_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_reflns_number 69656 _diffrn_reflns_av_R_equivalents 0.0760 _diffrn_reflns_av_sigmaI/netI 0.1209 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 30.03 _reflns_number_total 5280 _reflns_number_gt 2284 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Disorder. A structural disorder was found at a coordination site of Cd(3). At the site, 61.6(4)% of a chloride ion Cl(2) and 38.4(4)% of a cyanide ligand C(5) and N(5) are coordinating. Their occupancies were determined by the least square calculation, and they agreed with the results of elementary analysis. The methyl group (C206) of the 1-methylnaphthalene has a structural disorder coming from a mirror plane of the crystal. C206 was found at two positions with occupancy of 1/2, and which are related with the mirror plane. ; _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^)+(0.0595P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5280 _refine_ls_number_parameters 231 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.0907 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.1184 _refine_ls_wR_factor_gt 0.1089 _refine_ls_goodness_of_fit_ref 0.712 _refine_ls_restrained_S_all 0.714 _refine_ls_shift/su_max 0.692 _refine_ls_shift/su_mean 0.039 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.45476(4) 0.7500 0.11410(3) 0.04112(16) Uani 1 2 d S . . Cd2 Cd 0.17552(4) 0.2500 0.40131(3) 0.04178(16) Uani 1 2 d S . . Cd3 Cd 0.26085(5) 0.2500 0.18232(3) 0.0579(2) Uani 1 2 d S . . Cl1 Cl 0.37890(17) 0.7500 0.02419(10) 0.0675(7) Uani 1 2 d S . . Cl2 Cl 0.1408(6) 0.2500 0.1194(3) 0.0712(17) Uani 0.616(4) 2 d SPU . . C5 C 0.145(4) 0.2500 0.1425(15) 0.125(14) Uani 0.384(4) 2 d SPDU . . N5 N 0.108(3) 0.2500 0.1045(13) 0.075(9) Uani 0.384(4) 2 d SPDU . . N1 N 0.5595(3) 0.9311(6) 0.1046(2) 0.0673(16) Uani 1 1 d . . . C1 C 0.6012(4) 1.0356(7) 0.1014(2) 0.0501(14) Uani 1 1 d . . . N2 N 0.2066(6) 0.2500 0.3095(3) 0.064(2) Uani 1 2 d S . . C2 C 0.2219(6) 0.2500 0.2657(4) 0.056(2) Uani 1 2 d S . . C3 C 0.3065(6) 0.2500 0.4337(4) 0.047(2) Uani 1 2 d S . . N3 N 0.3669(6) 0.2500 0.4547(4) 0.078(3) Uani 1 2 d S . . C4 C 0.3362(4) 0.4577(8) 0.1660(3) 0.0620(18) Uani 1 1 d . . . N4 N 0.3741(4) 0.5626(7) 0.1548(2) 0.0698(16) Uani 1 1 d . . . N101 N 0.3243(5) 0.2500 0.0183(3) 0.0513(18) Uani 1 2 d S . . N102 N -0.0888(5) 0.2500 -0.0932(3) 0.062(2) Uani 1 2 d S . . C101 C 0.2842(4) 0.1190(7) 0.0082(3) 0.0644(19) Uani 1 1 d . . . H101 H 0.3113 0.0278 0.0167 0.077 Uiso 1 1 calc R . . C102 C 0.2042(4) 0.1154(7) -0.0145(3) 0.0633(19) Uani 1 1 d . . . H102 H 0.1781 0.0224 -0.0219 0.076 Uiso 1 1 calc R . . C103 C 0.1617(5) 0.2500 -0.0265(3) 0.045(2) Uani 1 2 d S . . C104 C 0.0734(5) 0.2500 -0.0509(4) 0.047(2) Uani 1 2 d S . . C105 C 0.0313(4) 0.1152(7) -0.0624(3) 0.0582(16) Uani 1 1 d . . . H105 H 0.0580 0.0224 -0.0555 0.070 Uiso 1 1 calc R . . C106 C -0.0497(4) 0.1184(8) -0.0837(3) 0.0655(18) Uani 1 1 d . . . H106 H -0.0776 0.0275 -0.0917 0.079 Uiso 1 1 calc R . . C111 C 0.4132(6) 0.2500 0.0429(4) 0.081(4) Uani 1 2 d S . . H111 H 0.4326 0.1469 0.0472 0.121 Uiso 0.50 1 calc PR . . H121 H 0.4113 0.2992 0.0773 0.121 Uiso 0.50 1 calc PR . . H131 H 0.4520 0.3039 0.0197 0.121 Uiso 0.50 1 calc PR . . C112 C -0.1757(6) 0.2500 -0.1190(6) 0.118(5) Uani 1 2 d S . . H112 H -0.2170 0.2074 -0.0946 0.177 Uiso 0.50 1 calc PR . . H122 H -0.1740 0.1900 -0.1512 0.177 Uiso 0.50 1 calc PR . . H132 H -0.1919 0.3526 -0.1277 0.177 Uiso 0.50 1 calc PR . . C201 C 0.1988(6) 0.1625(17) -0.1696(4) 0.167(8) Uani 1 1 d U . . H201 H 0.2451 0.1067 -0.1566 0.200 Uiso 1 1 calc R . . C202 C 0.1271(9) 0.0935(18) -0.1898(4) 0.154(5) Uani 1 1 d U . . H202 H 0.1245 -0.0121 -0.1924 0.185 Uiso 1 1 calc R . . C203 C 0.0616(6) 0.1779(13) -0.2057(4) 0.110(4) Uani 1 1 d U . . C204 C -0.0116(11) 0.087(3) -0.2266(6) 0.194(8) Uani 1 1 d U . . C205 C -0.0747(7) 0.166(2) -0.2430(5) 0.215(12) Uani 1 1 d U . . H205 H -0.1233 0.1161 -0.2556 0.258 Uiso 1 1 calc R . . C206 C 0.005(2) -0.063(4) -0.2265(12) 0.238(19) Uani 0.50 1 d PU . . H216 H 0.0492 -0.0852 -0.2008 0.357 Uiso 0.50 1 calc PR . . H226 H 0.0234 -0.0944 -0.2616 0.357 Uiso 0.50 1 calc PR . . H236 H -0.0464 -0.1181 -0.2170 0.357 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 0.0396(3) 0.0347(3) 0.0490(4) 0.000 0.0012(3) 0.000 Cd2 0.0403(3) 0.0358(3) 0.0493(4) 0.000 0.0033(3) 0.000 Cd3 0.0781(5) 0.0446(3) 0.0510(4) 0.000 0.0238(4) 0.000 Cl1 0.0739(17) 0.0581(13) 0.0705(17) 0.000 -0.0027(14) 0.000 Cl2 0.107(5) 0.057(3) 0.050(5) 0.000 0.000(3) 0.000 C5 0.18(3) 0.09(2) 0.10(3) 0.000 0.02(3) 0.000 N5 0.14(3) 0.043(12) 0.046(19) 0.000 0.018(16) 0.000 N1 0.056(3) 0.048(3) 0.097(5) 0.003(3) -0.004(3) -0.008(3) C1 0.045(3) 0.043(3) 0.063(4) 0.004(3) -0.003(3) -0.005(3) N2 0.080(6) 0.063(5) 0.049(5) 0.000 0.013(4) 0.000 C2 0.077(7) 0.054(5) 0.036(5) 0.000 0.014(5) 0.000 C3 0.043(5) 0.030(4) 0.070(7) 0.000 -0.005(5) 0.000 N3 0.079(6) 0.038(4) 0.117(8) 0.000 0.011(6) 0.000 C4 0.074(5) 0.048(4) 0.063(4) 0.011(3) 0.021(4) -0.003(3) N4 0.078(4) 0.061(4) 0.070(4) 0.015(3) 0.020(3) 0.005(3) N101 0.046(4) 0.063(5) 0.045(4) 0.000 0.008(3) 0.000 N102 0.040(4) 0.080(6) 0.066(5) 0.000 0.005(4) 0.000 C101 0.072(4) 0.048(4) 0.074(5) -0.012(4) -0.006(4) 0.022(3) C102 0.062(4) 0.036(3) 0.092(5) -0.012(3) -0.014(4) 0.008(3) C103 0.047(5) 0.036(4) 0.051(5) 0.000 0.003(4) 0.000 C104 0.046(5) 0.040(4) 0.055(6) 0.000 -0.001(4) 0.000 C105 0.057(4) 0.040(3) 0.077(5) -0.001(3) 0.002(3) -0.001(3) C106 0.052(4) 0.067(4) 0.077(5) -0.010(4) 0.005(3) -0.010(4) C111 0.042(5) 0.119(10) 0.082(8) 0.000 0.000(5) 0.000 C112 0.042(6) 0.149(13) 0.163(14) 0.000 -0.020(8) 0.000 C201 0.125(8) 0.31(2) 0.064(6) 0.049(9) 0.023(5) 0.128(11) C202 0.192(12) 0.177(12) 0.094(9) 0.016(9) 0.052(9) 0.055(13) C203 0.090(6) 0.168(12) 0.072(5) -0.020(6) 0.014(5) -0.023(6) C204 0.158(13) 0.31(2) 0.115(11) -0.053(14) 0.042(10) -0.040(17) C205 0.126(10) 0.42(4) 0.097(8) -0.051(14) 0.012(8) -0.046(16) C206 0.36(4) 0.18(3) 0.18(3) -0.06(3) 0.15(3) -0.09(3) # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cd1 Cl1 2.530(3) . . Cd1 N1 2.289(5) . . Cd1 N4 2.304(6) . . Cd1 N1 2.289(5) . 8_565 Cd1 N4 2.304(6) . 8_565 Cd2 N2 2.336(8) . . Cd2 C3 2.192(9) . . Cd2 C1 2.210(6) . 3_465 Cd2 C1 2.210(6) . 6_445 Cd3 Cl2 2.438(9) . . Cd3 C2 2.162(10) . . Cd3 C4 2.206(7) . . Cd3 C5 2.06(6) . . Cd3 C4 2.206(7) . 8_555 N1 C1 1.127(8) . . N2 C2 1.116(12) . . N3 C3 1.076(13) . . N4 C4 1.129(9) . . N5 C5 1.11(6) . . N101 C101 1.333(7) . . N101 C111 1.513(12) . . N101 C101 1.333(7) . 8_555 N102 C106 1.327(8) . . N102 C112 1.497(13) . . N102 C106 1.327(8) . 8_555 C101 C102 1.368(9) . . C102 C103 1.387(7) . . C103 C104 1.502(11) . . C104 C105 1.383(8) . . C104 C105 1.383(8) . 8_555 C105 C106 1.368(9) . . C201 C202 1.366(18) . . C201 C201 1.54(2) . 8_555 C202 C203 1.321(17) . . C203 C204 1.49(2) . . C203 C203 1.266(16) . 8_555 C204 C205 1.27(2) . . C204 C206 1.34(4) . . C205 C205 1.48(2) . 8_555 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_2 _geom_angle_site_symmetry_3 Cl1 Cd1 N1 103.94(13) . . . Cl1 Cd1 N4 97.73(14) . . . Cl1 Cd1 N1 103.94(13) . . 8_565 Cl1 Cd1 N4 97.73(14) . . 8_565 N1 Cd1 N4 158.32(19) . . . N1 Cd1 N1 87.98(18) . . 8_565 N1 Cd1 N4 86.4(2) . . 8_565 N1 Cd1 N4 86.4(2) 8_565 . . N4 Cd1 N4 91.1(2) . . 8_565 N1 Cd1 N4 158.32(19) 8_565 . 8_565 N2 Cd2 C3 99.6(3) . . . N2 Cd2 C1 94.50(18) . . 3_465 N2 Cd2 C1 94.50(18) . . 6_445 C1 Cd2 C3 119.86(16) 3_465 . . C1 Cd2 C3 119.86(16) 6_445 . . C1 Cd2 C1 116.8(2) 3_465 . 6_445 Cl2 Cd3 C2 113.7(3) . . . Cl2 Cd3 C4 106.8(2) . . . Cl2 Cd3 C4 106.8(2) . . 8_555 C2 Cd3 C4 109.0(2) . . . C2 Cd3 C5 102.5(13) . . . C2 Cd3 C4 109.0(2) . . 8_555 C4 Cd3 C5 112.2(6) . . . C4 Cd3 C4 111.5(2) . . 8_555 C4 Cd3 C5 112.2(6) 8_555 . . Cd1 N1 C1 169.4(5) . . . Cd2 N2 C2 179.6(9) . . . Cd1 N4 C4 167.4(5) . . . C101 N101 C111 120.3(4) 8_555 . . C101 N101 C111 120.3(4) . . . C101 N101 C101 119.4(7) . . 8_555 C106 N102 C112 119.4(4) . . . C106 N102 C106 121.1(7) . . 8_555 C106 N102 C112 119.4(4) 8_555 . . Cd2 C1 N1 175.6(5) 3_565 . . Cd3 C2 N2 176.0(9) . . . Cd2 C3 N3 172.5(9) . . . Cd3 C4 N4 176.3(6) . . . Cd3 C5 N5 150(5) . . . N101 C101 C102 121.6(6) . . . C101 C102 C103 120.2(6) . . . C102 C103 C104 121.6(4) . . . C102 C103 C102 116.9(7) . . 8_555 C102 C103 C104 121.6(4) 8_555 . . C103 C104 C105 121.1(4) . . . C103 C104 C105 121.1(4) . . 8_555 C105 C104 C105 117.7(7) . . 8_555 C104 C105 C106 120.0(6) . . . N102 C106 C105 120.6(6) . . . C201 C201 C202 116.3(11) 8_555 . . C201 C202 C203 119.5(14) . . . C202 C203 C204 113.3(14) . . . C202 C203 C203 124.1(11) . . 8_555 C203 C203 C204 122.5(13) 8_555 . . C203 C204 C205 114(2) . . . C203 C204 C206 112.3(19) . . . C205 C204 C206 133(2) . . . C204 C205 C205 123.1(15) . . 8_555 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 C102 C103 C104 C105 -0.1(13) . . . . C102 C103 C104 C105 179.6(8) . . . 8_555 C201 C201 C202 C203 -2.9(15) 8_555 . . . C202 C201 C201 C202 0.0(14) . . 8_555 8_555 C201 C202 C203 C204 -179.9(11) . . . . C201 C202 C203 C203 3.1(17) . . . 8_555 C202 C203 C204 C205 -178.8(12) . . . . C202 C203 C204 C206 -2(2) . . . . C203 C203 C204 C205 -1.8(19) 8_555 . . . C203 C203 C204 C206 175.2(17) 8_555 . . . C202 C203 C203 C202 0.0(18) . . 8_555 8_555 C202 C203 C203 C204 176.7(11) . . 8_555 8_555 C204 C203 C203 C202 -176.7(11) . . 8_555 8_555 C204 C203 C203 C204 0.0(17) . . 8_555 8_555 C203 C204 C205 C205 2(2) . . . 8_555 C206 C204 C205 C205 -174(2) . . . 8_555 C204 C205 C205 C204 0(2) . . 8_555 8_555 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.770 _refine_diff_density_min -0.611 _refine_diff_density_rms 0.117 #===END #------------------------------------------------------------------------------ data_bl _database_code_depnum_ccdc_archive 'CCDC 269968' _audit_creation_method SHELXL-97 _chemical_formula_structural '(C12 H14 N2)1.5 (Cd5 (C N)11.28 Cl1.72) (C9 H12 O3)' _chemical_formula_sum 'C38.28 H33 Cd5 Cl1.72 N14.28 O3' _chemical_formula_weight 1364.091 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' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 19.1014(6) _cell_length_b 8.8622(2) _cell_length_c 14.8612(5) _cell_angle_alpha 84.8205(11) _cell_angle_beta 86.4434(7) _cell_angle_gamma 84.5316(6) _cell_volume 2490.41(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 65346 _cell_measurement_theta_min 1.07 _cell_measurement_theta_max 30.0 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.819 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1311.76 _exptl_absorpt_coefficient_mu 2.227 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7196 _exptl_absorpt_correction_T_max 1.1450 _exptl_absorpt_process_details 'PROCESS-AUTO, RIGAKU Co., Tokyo, Japan(1998)' _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_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_reflns_number 50917 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0618 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.07 _diffrn_reflns_theta_max 30.01 _reflns_number_total 14279 _reflns_number_gt 8786 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Disorder. A structural disorder was found at a coordination site of Cd(3). At the site, 71.5(14)% of a chloride ion Cl(2) and 28.5(14)% of a cyanide ligand C(12) and N(12) are coordinating. Their occupancies were determined by the least square calculation, and they agreed with the results of elementary analysis. ; _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^)+(0.0682P)^2^+1.2244P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14279 _refine_ls_number_parameters 578 _refine_ls_number_restraints 210 _refine_ls_R_factor_all 0.0940 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1466 _refine_ls_wR_factor_gt 0.1207 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.532 _refine_ls_shift/su_mean 0.015 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.29900(2) 0.29539(4) 0.07850(3) 0.04307(11) Uani 1 1 d . . . Cd2 Cd 0.02130(2) -0.13047(5) 0.29642(3) 0.04733(12) Uani 1 1 d . . . Cd3 Cd 0.47029(2) 0.74653(5) 0.16754(3) 0.04704(12) Uani 1 1 d . . . Cd4 Cd 0.17020(2) 0.30805(5) 0.43206(3) 0.05094(12) Uani 1 1 d . . . Cd5 Cd 0.14815(2) -0.15344(4) -0.04353(3) 0.04628(11) Uani 1 1 d . . . Cl1 Cl 0.22033(15) 0.3061(3) 0.23024(19) 0.0984(7) Uani 1 1 d . . . Cl2 Cl 0.5061(6) 0.7368(14) 0.3252(9) 0.067(2) Uani 0.715(14) 1 d P . . C12 C 0.516(7) 0.722(14) 0.316(9) 0.070(18) Uani 0.285(14) 1 d PU . . N12 N 0.5229(13) 0.725(3) 0.3856(19) 0.069(6) Uani 0.285(14) 1 d PU . . C1 C 0.4079(4) 0.5534(8) 0.1483(5) 0.0567(16) Uani 1 1 d . . . N1 N 0.3737(3) 0.4621(7) 0.1344(4) 0.0659(16) Uani 1 1 d . . . C2 C 0.1989(4) 0.0476(7) -0.0103(5) 0.0589(16) Uani 1 1 d . . . N2 N 0.2241(3) 0.1456(6) 0.0118(5) 0.0705(17) Uani 1 1 d . . . C3 C 0.4314(4) 0.2694(7) -0.0834(5) 0.0543(15) Uani 1 1 d . . . N3 N 0.3802(3) 0.2803(6) -0.0418(4) 0.0649(15) Uani 1 1 d . . . C4 C 0.2094(3) 0.6265(7) -0.0151(4) 0.0508(14) Uani 1 1 d . . . N4 N 0.2372(3) 0.5117(6) 0.0082(4) 0.0566(13) Uani 1 1 d . . . C5 C 0.4013(3) -0.0398(7) 0.1447(5) 0.0536(15) Uani 1 1 d . . . N5 N 0.3651(3) 0.0688(6) 0.1348(4) 0.0613(14) Uani 1 1 d . . . C6 C 0.0516(3) -0.1773(7) 0.1540(5) 0.0516(14) Uani 1 1 d . . . N6 N 0.0709(3) -0.1793(6) 0.0817(4) 0.0628(14) Uani 1 1 d . . . C7 C -0.0886(3) 0.1162(6) 0.1655(4) 0.0489(14) Uani 1 1 d . . . N7 N -0.0562(3) 0.0858(6) 0.2268(4) 0.0577(14) Uani 1 1 d . . . C8 C 0.1152(3) 0.1198(6) 0.3860(4) 0.0463(13) Uani 1 1 d . . . N8 N 0.0843(4) 0.0326(7) 0.3570(4) 0.0689(16) Uani 1 1 d . . . C9 C 0.1207(4) -0.4611(7) 0.3904(4) 0.0539(15) Uani 1 1 d . . . N9 N 0.0969(3) -0.3483(6) 0.3614(4) 0.0646(15) Uani 1 1 d . . . C10 C 0.2828(4) 0.2694(6) 0.4634(5) 0.0535(16) Uani 1 1 d . . . N10 N 0.3392(4) 0.2605(7) 0.4690(6) 0.083(2) Uani 1 1 d . . . C11 C 0.0690(4) 0.2182(7) 0.6224(5) 0.0549(16) Uani 1 1 d . . . N11 N 0.1111(3) 0.2608(6) 0.5728(4) 0.0653(15) Uani 1 1 d . . . N101 N 0.0279(4) 0.5680(7) 0.7626(7) 0.090(2) Uani 1 1 d U . . C101 C 0.0784(5) 0.4967(10) 0.8130(9) 0.100(3) Uani 1 1 d U . . H101 H 0.1216 0.4660 0.7849 0.120 Uiso 1 1 calc . . . C102 C 0.0691(5) 0.4675(10) 0.9033(10) 0.104(4) Uani 1 1 d U . . H102 H 0.1057 0.4155 0.9351 0.124 Uiso 1 1 calc . . . C103 C 0.0056(4) 0.5132(8) 0.9516(7) 0.089(3) Uani 1 1 d U . . C104 C -0.0461(4) 0.5864(10) 0.8932(10) 0.103(4) Uani 1 1 d U . . H104 H -0.0903 0.6179 0.9183 0.124 Uiso 1 1 calc . . . C105 C -0.0337(5) 0.6119(10) 0.8029(9) 0.099(3) Uani 1 1 d U . . H105 H -0.0692 0.6614 0.7681 0.119 Uiso 1 1 calc . . . C111 C 0.0412(6) 0.6032(11) 0.6648(9) 0.107(3) Uani 1 1 d U . . H111 H 0.0163 0.5383 0.6323 0.160 Uiso 1 1 calc . . . H121 H 0.0908 0.5867 0.6496 0.160 Uiso 1 1 calc . . . H131 H 0.0253 0.7076 0.6485 0.160 Uiso 1 1 calc . . . C201 C 0.4639(5) 0.6547(8) 0.6240(5) 0.081(2) Uani 1 1 d U . . H201 H 0.4833 0.5666 0.6554 0.098 Uiso 1 1 calc . . . C202 C 0.4182(5) 0.6425(7) 0.5571(5) 0.070(2) Uani 1 1 d U . . H202 H 0.4070 0.5476 0.5434 0.084 Uiso 1 1 calc . . . C203 C 0.3893(3) 0.7742(6) 0.5105(4) 0.0505(14) Uani 1 1 d U . . C204 C 0.4065(4) 0.9098(7) 0.5372(5) 0.069(2) Uani 1 1 d U . . H204 H 0.3866 1.0006 0.5092 0.083 Uiso 1 1 calc . . . C205 C 0.4518(5) 0.9142(8) 0.6036(6) 0.075(2) Uani 1 1 d U . . H205 H 0.4626 1.0075 0.6204 0.090 Uiso 1 1 calc . . . C206 C 0.2929(4) 0.6315(7) 0.3276(5) 0.0613(17) Uani 1 1 d U . . H206 H 0.2843 0.5388 0.3076 0.074 Uiso 1 1 calc . . . C207 C 0.3305(4) 0.6325(7) 0.4017(5) 0.0609(17) Uani 1 1 d U . . H207 H 0.3478 0.5408 0.4314 0.073 Uiso 1 1 calc . . . C208 C 0.3437(3) 0.7689(6) 0.4342(4) 0.0484(14) Uani 1 1 d U . . C209 C 0.3154(4) 0.9006(7) 0.3875(5) 0.0593(17) Uani 1 1 d U . . H209 H 0.3222 0.9944 0.4074 0.071 Uiso 1 1 calc . . . C210 C 0.2778(4) 0.8954(7) 0.3130(5) 0.0591(16) Uani 1 1 d U . . H210 H 0.2590 0.9856 0.2831 0.071 Uiso 1 1 calc . . . N201 N 0.4806(4) 0.7867(7) 0.6445(4) 0.0672(16) Uani 1 1 d U . . N202 N 0.2675(3) 0.7616(7) 0.2821(4) 0.0562(13) Uani 1 1 d U . . C211 C 0.5321(6) 0.7925(11) 0.7145(6) 0.101(3) Uani 1 1 d U . . H211 H 0.5101 0.7690 0.7733 0.151 Uiso 1 1 calc . . . H221 H 0.5479 0.8927 0.7112 0.151 Uiso 1 1 calc . . . H231 H 0.5717 0.7197 0.7044 0.151 Uiso 1 1 calc . . . C212 C 0.2310(4) 0.7557(10) 0.1977(6) 0.081(2) Uani 1 1 d U . . H212 H 0.2620 0.7825 0.1466 0.121 Uiso 1 1 calc . . . H222 H 0.1896 0.8262 0.1977 0.121 Uiso 1 1 calc . . . H232 H 0.2178 0.6547 0.1941 0.121 Uiso 1 1 calc . . . C301 C 0.2699(5) 0.5890(12) 0.7188(7) 0.090(3) Uani 1 1 d U . . C302 C 0.2421(6) 0.7280(12) 0.6771(8) 0.098(3) Uani 1 1 d U . . C303 C 0.2615(9) 0.8598(17) 0.7001(12) 0.151(5) Uani 1 1 d U . . H303 H 0.2415 0.9517 0.6736 0.181 Uiso 1 1 calc . . . C304 C 0.3079(10) 0.858(3) 0.7590(16) 0.188(8) Uani 1 1 d U . . H304 H 0.3204 0.9516 0.7731 0.226 Uiso 1 1 calc . . . C305 C 0.3394(8) 0.737(3) 0.8011(11) 0.171(7) Uani 1 1 d U . . C306 C 0.3204(6) 0.588(2) 0.7814(8) 0.140(5) Uani 1 1 d U . . H306 H 0.3410 0.4977 0.8093 0.168 Uiso 1 1 calc . . . O301 O 0.2425(4) 0.4663(7) 0.6899(5) 0.111(2) Uani 1 1 d U . . O302 O 0.1959(5) 0.7196(8) 0.6118(5) 0.119(3) Uani 1 1 d U . . O305 O 0.3909(8) 0.750(2) 0.8524(13) 0.272(7) Uani 1 1 d U . . C311 C 0.2722(8) 0.3194(14) 0.7226(11) 0.166(6) Uani 1 1 d U . . H311 H 0.3214 0.3080 0.7044 0.249 Uiso 1 1 calc . . . H321 H 0.2485 0.2429 0.6979 0.249 Uiso 1 1 calc . . . H331 H 0.2666 0.3083 0.7874 0.249 Uiso 1 1 calc . . . C312 C 0.1671(8) 0.8568(13) 0.5658(9) 0.156(6) Uani 1 1 d U . . H312 H 0.1550 0.9315 0.6084 0.235 Uiso 1 1 calc . . . H322 H 0.1257 0.8379 0.5367 0.235 Uiso 1 1 calc . . . H332 H 0.2013 0.8939 0.5211 0.235 Uiso 1 1 calc . . . C315 C 0.3848(12) 0.879(2) 0.888(2) 0.292(15) Uani 1 1 d U . . H315 H 0.4172 0.9447 0.8566 0.438 Uiso 1 1 calc . . . H325 H 0.3952 0.8624 0.9505 0.438 Uiso 1 1 calc . . . H335 H 0.3375 0.9252 0.8827 0.438 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 0.0370(2) 0.03615(19) 0.0556(3) -0.00259(17) -0.00310(18) -0.00188(16) Cd2 0.0516(3) 0.0422(2) 0.0476(2) -0.00072(18) -0.0035(2) -0.00359(18) Cd3 0.0400(2) 0.0413(2) 0.0592(3) -0.00469(18) 0.0001(2) -0.00214(16) Cd4 0.0502(3) 0.0385(2) 0.0628(3) 0.00337(19) -0.0071(2) -0.00146(18) Cd5 0.0522(3) 0.0376(2) 0.0498(2) -0.00105(17) -0.0144(2) -0.00280(17) Cl1 0.0999(18) 0.0802(14) 0.1151(19) -0.0029(13) -0.0085(15) -0.0118(12) Cl2 0.075(3) 0.055(4) 0.070(4) -0.010(2) -0.004(2) -0.002(2) C12 0.08(4) 0.05(2) 0.08(3) -0.01(2) -0.01(3) -0.03(2) N12 0.088(16) 0.074(13) 0.046(14) -0.009(11) -0.036(13) 0.004(11) C1 0.048(4) 0.057(4) 0.065(4) -0.002(3) -0.005(3) -0.006(3) N1 0.052(3) 0.062(3) 0.088(4) -0.007(3) -0.012(3) -0.019(3) C2 0.056(4) 0.051(3) 0.070(4) -0.004(3) -0.009(3) -0.007(3) N2 0.076(4) 0.054(3) 0.087(5) -0.010(3) -0.011(4) -0.024(3) C3 0.053(4) 0.049(3) 0.058(4) 0.000(3) 0.003(3) -0.001(3) N3 0.060(4) 0.063(3) 0.068(4) -0.003(3) 0.015(3) -0.002(3) C4 0.050(3) 0.048(3) 0.055(4) -0.003(3) -0.012(3) 0.000(3) N4 0.054(3) 0.046(3) 0.069(4) -0.002(2) -0.010(3) 0.002(2) C5 0.052(4) 0.051(3) 0.058(4) -0.005(3) -0.003(3) -0.003(3) N5 0.062(4) 0.049(3) 0.070(4) 0.002(3) -0.004(3) 0.005(3) C6 0.047(3) 0.050(3) 0.056(4) -0.004(3) -0.001(3) 0.002(3) N6 0.056(3) 0.062(3) 0.070(4) -0.006(3) -0.003(3) -0.005(3) C7 0.054(4) 0.040(3) 0.052(4) -0.003(3) -0.008(3) 0.000(3) N7 0.069(4) 0.050(3) 0.054(3) 0.000(2) -0.020(3) 0.003(3) C8 0.053(3) 0.042(3) 0.046(3) -0.002(2) -0.009(3) -0.014(3) N8 0.071(4) 0.066(4) 0.065(4) 0.014(3) -0.007(3) 0.005(3) C9 0.056(4) 0.047(3) 0.057(4) 0.004(3) -0.005(3) 0.002(3) N9 0.071(4) 0.040(3) 0.080(4) 0.003(3) -0.014(3) 0.005(3) C10 0.051(4) 0.030(3) 0.078(5) -0.005(3) -0.004(3) 0.003(2) N10 0.075(5) 0.049(3) 0.124(6) 0.004(4) -0.015(4) -0.001(3) C11 0.062(4) 0.042(3) 0.060(4) -0.008(3) 0.003(3) 0.000(3) N11 0.072(4) 0.060(3) 0.063(4) -0.005(3) 0.008(3) -0.010(3) N101 0.067(4) 0.041(3) 0.168(8) -0.018(4) -0.033(5) -0.006(3) C101 0.060(5) 0.057(5) 0.188(11) -0.024(6) -0.042(7) 0.003(4) C102 0.069(6) 0.056(5) 0.191(11) -0.021(6) -0.060(7) 0.008(4) C103 0.049(4) 0.038(3) 0.184(10) -0.002(5) -0.037(6) -0.010(3) C104 0.048(4) 0.063(5) 0.196(11) 0.010(6) -0.026(6) -0.001(4) C105 0.068(6) 0.064(5) 0.165(10) 0.004(6) -0.029(7) -0.005(4) C111 0.101(8) 0.071(6) 0.154(11) -0.024(6) -0.028(8) -0.006(5) C201 0.124(7) 0.055(4) 0.063(5) 0.008(3) -0.029(5) 0.004(4) C202 0.109(6) 0.034(3) 0.067(4) -0.002(3) -0.016(4) 0.003(3) C203 0.057(4) 0.041(3) 0.053(4) -0.002(3) -0.003(3) -0.003(3) C204 0.089(5) 0.037(3) 0.085(5) 0.000(3) -0.035(4) -0.001(3) C205 0.101(6) 0.048(4) 0.078(5) -0.003(3) -0.029(5) -0.009(4) C206 0.055(4) 0.051(3) 0.080(5) -0.006(3) -0.007(4) -0.010(3) C207 0.059(4) 0.044(3) 0.079(5) 0.006(3) -0.009(4) -0.007(3) C208 0.053(3) 0.033(3) 0.058(4) -0.006(2) 0.001(3) -0.001(2) C209 0.075(5) 0.042(3) 0.060(4) -0.007(3) -0.007(4) 0.000(3) C210 0.061(4) 0.053(4) 0.062(4) -0.003(3) -0.007(3) 0.003(3) N201 0.085(4) 0.065(4) 0.053(3) -0.004(3) -0.019(3) -0.001(3) N202 0.043(3) 0.074(4) 0.053(3) -0.011(3) 0.002(2) -0.011(3) C211 0.115(8) 0.109(7) 0.083(6) -0.010(5) -0.048(6) -0.006(6) C212 0.064(5) 0.103(6) 0.078(5) -0.014(5) -0.018(4) -0.007(4) C301 0.077(6) 0.110(7) 0.082(6) 0.007(5) -0.003(5) -0.014(5) C302 0.116(8) 0.085(6) 0.094(7) -0.018(5) 0.036(6) -0.031(6) C303 0.143(12) 0.137(10) 0.179(14) -0.053(10) 0.050(10) -0.045(10) C304 0.106(13) 0.28(2) 0.193(18) -0.077(16) 0.017(12) -0.056(14) C305 0.070(8) 0.35(2) 0.115(10) -0.085(13) -0.009(7) -0.053(12) C306 0.073(7) 0.254(15) 0.093(8) -0.010(9) 0.003(6) -0.020(9) O301 0.101(5) 0.075(4) 0.155(7) 0.017(4) -0.046(5) 0.005(4) O302 0.153(7) 0.083(4) 0.110(6) 0.011(4) -0.009(5) 0.035(4) O305 0.181(13) 0.352(19) 0.305(17) -0.129(15) 0.012(12) -0.061(14) C311 0.142(11) 0.114(9) 0.218(16) 0.061(10) -0.015(11) 0.046(8) C312 0.186(13) 0.112(8) 0.136(10) 0.065(7) 0.049(9) 0.062(9) C315 0.24(2) 0.178(16) 0.48(4) -0.20(2) 0.19(2) -0.109(15) # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cd1 Cl1 2.635(3) . . Cd1 N1 2.383(6) . . Cd1 N2 2.360(6) . . Cd1 N3 2.298(6) . . Cd1 N4 2.350(6) . . Cd1 N5 2.381(6) . . Cd2 N7 2.495(6) . . Cd2 N8 2.247(7) . . Cd2 N9 2.460(6) . . Cd2 C6 2.224(7) . . Cd2 C11 2.205(7) . 2_556 Cd3 Cl2 2.473(13) . . Cd3 C1 2.225(7) . . Cd3 C12 2.41(14) . . Cd3 C5 2.214(6) . 1_565 Cd3 C3 2.191(8) . 2_665 Cd4 N11 2.337(6) . . Cd4 C8 2.233(6) . . Cd4 C10 2.217(8) . . Cd4 C9 2.222(6) . 1_565 Cd5 N6 2.311(6) . . Cd5 C2 2.215(7) . . Cd5 C4 2.197(6) . 1_545 Cd5 C7 2.183(6) . 2_555 O301 C301 1.364(12) . . O301 C311 1.426(15) . . O302 C302 1.363(14) . . O302 C312 1.420(14) . . O305 C305 1.30(2) . . O305 C315 1.30(3) . . N1 C1 1.128(10) . . N2 C2 1.116(9) . . N3 C3 1.125(10) . . N4 C4 1.137(8) . . N5 C5 1.134(8) . . N6 C6 1.115(9) . . N7 C7 1.131(8) . . N8 C8 1.145(9) . . N9 C9 1.119(8) . . N10 C10 1.081(11) . . N11 C11 1.125(9) . . N12 C12 1.05(13) . . N101 C101 1.334(14) . . N101 C111 1.470(17) . . N101 C105 1.327(13) . . N201 C205 1.322(10) . . N201 C211 1.483(12) . . N201 C201 1.308(10) . . N202 C206 1.347(9) . . N202 C212 1.480(10) . . N202 C210 1.345(9) . . C101 C102 1.35(2) . . C102 C103 1.415(14) . . C103 C103 1.442(15) . 2_567 C103 C104 1.425(14) . . C104 C105 1.35(2) . . C201 C202 1.381(12) . . C202 C203 1.388(9) . . C203 C208 1.479(8) . . C203 C204 1.374(8) . . C204 C205 1.358(12) . . C206 C207 1.353(11) . . C207 C208 1.392(8) . . C208 C209 1.384(9) . . C209 C210 1.363(11) . . C301 C302 1.401(15) . . C301 C306 1.380(15) . . C302 C303 1.337(19) . . C303 C304 1.28(3) . . C304 C305 1.31(3) . . C305 C306 1.46(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_2 _geom_angle_site_symmetry_3 Cl1 Cd1 N1 89.08(15) . . . Cl1 Cd1 N2 93.88(18) . . . Cl1 Cd1 N3 172.36(16) . . . Cl1 Cd1 N4 93.44(16) . . . Cl1 Cd1 N5 91.87(15) . . . N1 Cd1 N2 175.0(2) . . . N1 Cd1 N3 85.8(2) . . . N1 Cd1 N4 87.7(2) . . . N1 Cd1 N5 94.7(2) . . . N2 Cd1 N3 91.7(2) . . . N2 Cd1 N4 88.1(2) . . . N2 Cd1 N5 89.3(2) . . . N3 Cd1 N4 92.0(2) . . . N3 Cd1 N5 82.9(2) . . . N4 Cd1 N5 174.2(2) . . . N7 Cd2 N8 90.7(2) . . . N7 Cd2 N9 178.28(18) . . . N7 Cd2 C6 84.5(2) . . . N7 Cd2 C11 91.1(2) . . 2_556 N8 Cd2 N9 90.9(2) . . . N8 Cd2 C6 116.3(2) . . . N8 Cd2 C11 118.3(2) . . 2_556 N9 Cd2 C6 94.1(2) . . . N9 Cd2 C11 88.8(2) . . 2_556 C6 Cd2 C11 125.2(2) . . 2_556 Cl2 Cd3 C1 111.1(3) . . . Cl2 Cd3 C5 106.2(3) . . 1_565 Cl2 Cd3 C3 105.6(3) . . 2_665 C1 Cd3 C12 111(3) . . . C1 Cd3 C5 108.0(2) . . 1_565 C1 Cd3 C3 110.1(3) . . 2_665 C5 Cd3 C12 111(3) 1_565 . . C3 Cd3 C12 100(3) 2_665 . . C3 Cd3 C5 115.8(2) 2_665 . 1_565 N11 Cd4 C8 86.7(2) . . . N11 Cd4 C10 103.3(2) . . . N11 Cd4 C9 100.4(2) . . 1_565 C8 Cd4 C10 120.1(2) . . . C8 Cd4 C9 113.8(2) . . 1_565 C9 Cd4 C10 121.5(2) 1_565 . . N6 Cd5 C2 99.4(2) . . . N6 Cd5 C4 95.5(2) . . 1_545 N6 Cd5 C7 109.3(2) . . 2_555 C2 Cd5 C4 115.2(2) . . 1_545 C2 Cd5 C7 114.4(2) . . 2_555 C4 Cd5 C7 119.0(2) 1_545 . 2_555 C301 O301 C311 117.2(9) . . . C302 O302 C312 118.7(9) . . . C305 O305 C315 112(2) . . . Cd1 N1 C1 169.4(6) . . . Cd1 N2 C2 163.4(6) . . . Cd1 N3 C3 162.4(6) . . . Cd1 N4 C4 170.0(5) . . . Cd1 N5 C5 166.7(6) . . . Cd5 N6 C6 157.7(5) . . . Cd2 N7 C7 140.1(5) . . . Cd2 N8 C8 177.6(6) . . . Cd2 N9 C9 167.3(6) . . . Cd4 N11 C11 157.2(6) . . . C101 N101 C105 118.8(11) . . . C105 N101 C111 120.6(9) . . . C101 N101 C111 120.6(9) . . . C205 N201 C211 120.0(7) . . . C201 N201 C205 120.5(7) . . . C201 N201 C211 119.4(7) . . . C210 N202 C212 121.1(6) . . . C206 N202 C212 119.8(6) . . . C206 N202 C210 119.1(6) . . . Cd3 C1 N1 175.2(7) . . . Cd5 C2 N2 175.8(7) . . . Cd3 C3 N3 178.2(6) 2_665 . . Cd5 C4 N4 172.8(5) 1_565 . . Cd3 C5 N5 178.4(6) 1_545 . . Cd2 C6 N6 169.1(5) . . . Cd5 C7 N7 174.6(5) 2_555 . . Cd4 C8 N8 174.0(5) . . . Cd4 C9 N9 173.6(5) 1_545 . . Cd4 C10 N10 171.3(7) . . . Cd2 C11 N11 172.3(6) 2_556 . . Cd3 C12 N12 165(10) . . . N101 C101 C102 122.4(10) . . . C101 C102 C103 122.4(10) . . . C102 C103 C103 123.8(9) . . 2_567 C103 C103 C104 124.2(8) 2_567 . . C102 C103 C104 112.0(10) . . . C103 C104 C105 122.8(9) . . . N101 C105 C104 121.6(10) . . . N201 C201 C202 121.8(7) . . . C201 C202 C203 118.9(6) . . . C202 C203 C204 116.8(6) . . . C202 C203 C208 121.7(5) . . . C204 C203 C208 121.6(5) . . . C203 C204 C205 121.4(6) . . . N201 C205 C204 120.4(7) . . . N202 C206 C207 121.6(6) . . . C206 C207 C208 120.9(6) . . . C203 C208 C207 122.2(5) . . . C203 C208 C209 121.4(5) . . . C207 C208 C209 116.3(6) . . . C208 C209 C210 121.3(6) . . . N202 C210 C209 120.9(6) . . . O301 C301 C302 113.3(9) . . . O301 C301 C306 127.3(11) . . . C302 C301 C306 119.4(11) . . . O302 C302 C301 116.1(9) . . . O302 C302 C303 123.0(11) . . . C301 C302 C303 120.9(12) . . . C302 C303 C304 119.3(17) . . . C303 C304 C305 126(2) . . . O305 C305 C304 120(2) . . . O305 C305 C306 121.4(19) . . . C304 C305 C306 118.3(16) . . . C301 C306 C305 115.9(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 C102 C103 C103 C104 0.9(12) . . 2_567 2_567 C202 C203 C208 C207 -3.7(10) . . . . C202 C203 C208 C209 -179.5(7) . . . . C204 C203 C208 C207 174.7(7) . . . . C204 C203 C208 C209 -1.2(9) . . . . C302 C301 O301 C311 174.5(10) . . . . C306 C301 O301 C311 -4.7(16) . . . . O301 C301 C302 O302 -3.5(14) . . . . C303 C302 O302 C312 0.2(18) . . . . C301 C302 O302 C312 -178.7(10) . . . . C304 C305 O305 C315 30(3) . . . . C306 C305 O305 C315 -157.1(18) . . . . _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.810 _refine_diff_density_min -0.931 _refine_diff_density_rms 0.130 #===END #------------------------------------------------------------------------------ data_ph4 _database_code_depnum_ccdc_archive 'CCDC 269969' _audit_creation_method SHELXL-97 _chemical_formula_structural '(C12 H14 N2) (Cd3.5 (C N)9 (H2 O)) (C4 H5 N)' _chemical_formula_sum 'C25 H21 Cd3.5 N12 O' _chemical_formula_weight 898.961 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' # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 8.1525(2) _cell_length_b 22.1878(5) _cell_length_c 18.3312(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.9563(11) _cell_angle_gamma 90.00 _cell_volume 3275.43(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 92114 _cell_measurement_theta_min 0.92 _cell_measurement_theta_max 29.99 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.320 _exptl_crystal_size_mid 0.240 _exptl_crystal_size_min 0.210 _exptl_crystal_density_diffrn 1.823 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1724 _exptl_absorpt_coefficient_mu 2.269 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8818 _exptl_absorpt_correction_T_max 1.0985 _exptl_absorpt_process_details 'PROCESS-AUTO, RIGAKU Co., Tokyo, Japan(1998)' _exptl_special_details ; ? ; _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_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_reflns_number 72470 _diffrn_reflns_av_R_equivalents 0.0550 _diffrn_reflns_av_sigmaI/netI 0.0699 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 29.98 _reflns_number_total 9532 _reflns_number_gt 6183 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0285P)^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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 9532 _refine_ls_number_parameters 378 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0574 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0740 _refine_ls_wR_factor_gt 0.0517 _refine_ls_goodness_of_fit_ref 0.874 _refine_ls_restrained_S_all 0.875 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.0000 0.0000 0.0000 0.03465(8) Uani 1 2 d S . . Cd2 Cd 0.55957(3) 0.122642(12) 0.170286(15) 0.03523(6) Uani 1 1 d . . . Cd3 Cd 0.70938(3) -0.044073(12) 0.402436(14) 0.03185(6) Uani 1 1 d . . . Cd4 Cd 0.34836(3) 0.337460(12) 0.258210(15) 0.03365(6) Uani 1 1 d . . . CN1 C 0.9448(4) -0.00905(19) 0.4817(2) 0.0462(9) Uani 0.50 1 d P . . CN'1 N 0.9448(4) -0.00905(19) 0.4817(2) 0.0462(9) Uani 0.50 1 d P . . CN2 C 0.5382(5) -0.00928(19) 0.4789(2) 0.0511(10) Uani 0.50 1 d P . . CN'2 N 0.5382(5) -0.00928(19) 0.4789(2) 0.0511(10) Uani 0.50 1 d P . . C1 C -0.0800(5) 0.1163(2) -0.1336(2) 0.0461(9) Uani 1 1 d . . . N1 N -0.0452(5) 0.0841(2) -0.0873(2) 0.0639(11) Uani 1 1 d . . . C2 C -0.1845(5) 0.0470(2) 0.0680(2) 0.0417(10) Uani 1 1 d . . . N2 N -0.2552(6) 0.06563(19) 0.0935(3) 0.0597(11) Uani 1 1 d . . . C3 C 0.3342(5) 0.08267(19) 0.1045(2) 0.0418(9) Uani 1 1 d . . . N3 N 0.2262(4) 0.05762(17) 0.0721(2) 0.0510(9) Uani 1 1 d . . . C4 C 0.6539(5) 0.06876(18) 0.2700(2) 0.0413(8) Uani 1 1 d . . . N4 N 0.6905(5) 0.03676(17) 0.3185(2) 0.0528(9) Uani 1 1 d . . . C5 C 0.9689(5) -0.12420(19) 0.3078(2) 0.0401(8) Uani 1 1 d . . . N5 N 0.8832(4) -0.09917(17) 0.3387(2) 0.0496(9) Uani 1 1 d . . . C6 C 0.6644(5) 0.20673(18) 0.1312(2) 0.0408(8) Uani 1 1 d . . . N6 N 0.7201(5) 0.24832(18) 0.1105(2) 0.0587(10) Uani 1 1 d . . . C7 C 0.3728(5) 0.23933(18) 0.2552(2) 0.0418(9) Uani 1 1 d . . . N7 N 0.3984(5) 0.19061(17) 0.2465(2) 0.0573(10) Uani 1 1 d . . . C8 C 0.1136(5) 0.3798(2) 0.2079(2) 0.0466(9) Uani 1 1 d . . . N8 N 0.0066(4) 0.40836(18) 0.1801(2) 0.0543(9) Uani 1 1 d . . . O1 O 0.6889(4) -0.14493(14) 0.46266(16) 0.0495(7) Uani 1 1 d . . . H1 H 0.5773 -0.1469 0.4766 0.074 Uiso 1 1 d . . . H2 H 0.6971 -0.1761 0.4345 0.074 Uiso 1 1 d . . . C101 C 0.0456(5) 0.1169(2) 0.2331(2) 0.0474(10) Uani 1 1 d . . . H101 H 0.0339 0.1082 0.1830 0.057 Uiso 1 1 calc D . . C102 C 0.0049(5) 0.17305(19) 0.2554(2) 0.0402(8) Uani 1 1 d . . . H102 H -0.0342 0.2022 0.2206 0.048 Uiso 1 1 calc . . . C103 C 0.0223(5) 0.18630(18) 0.3303(2) 0.0395(8) Uani 1 1 d . . . C104 C 0.0762(7) 0.1418(2) 0.3801(2) 0.0588(12) Uani 1 1 d . . . H104 H 0.0866 0.1493 0.4305 0.071 Uiso 1 1 calc . . . C105 C 0.1149(7) 0.0857(2) 0.3553(3) 0.0661(14) Uani 1 1 d . . . H105 H 0.1503 0.0554 0.3891 0.079 Uiso 1 1 calc D . . C106 C -0.1339(6) 0.3443(2) 0.3336(3) 0.0514(11) Uani 1 1 d . . . H106 H -0.2094 0.3696 0.3052 0.062 Uiso 1 1 calc D . . C107 C -0.1211(5) 0.2853(2) 0.3127(2) 0.0483(10) Uani 1 1 d . . . H107 H -0.1878 0.2705 0.2707 0.058 Uiso 1 1 calc . . . C108 C -0.0075(5) 0.24803(18) 0.3549(2) 0.0383(8) Uani 1 1 d . . . C109 C 0.0833(6) 0.2715(2) 0.4193(2) 0.0508(11) Uani 1 1 d . . . H109 H 0.1559 0.2468 0.4501 0.061 Uiso 1 1 calc . . . C110 C 0.0665(6) 0.3300(2) 0.4372(2) 0.0540(11) Uani 1 1 d . . . H110 H 0.1292 0.3455 0.4799 0.065 Uiso 1 1 calc D . . C111 C 0.1483(9) 0.0135(2) 0.2569(4) 0.089(2) Uani 1 1 d . . . H111 H 0.2638 0.0133 0.2520 0.134 Uiso 1 1 calc RD . . H121 H 0.0826 0.0046 0.2100 0.134 Uiso 1 1 calc R . . H131 H 0.1282 -0.0163 0.2924 0.134 Uiso 1 1 calc R . . C112 C -0.0535(8) 0.4308(2) 0.4127(3) 0.0742(16) Uani 1 1 d . . . H112 H 0.0250 0.4536 0.3900 0.111 Uiso 1 1 calc RD . . H122 H -0.0307 0.4359 0.4653 0.111 Uiso 1 1 calc R . . H132 H -0.1638 0.4446 0.3946 0.111 Uiso 1 1 calc R . . N101 N 0.1019(5) 0.07435(16) 0.2823(2) 0.0529(9) Uani 1 1 d . . . N102 N -0.0393(4) 0.36602(16) 0.3943(2) 0.0459(8) Uani 1 1 d . . . C201 C 0.6062(11) 0.2346(6) 0.4526(7) 0.115(3) Uani 1 1 d . . . H201 H 0.5276 0.2574 0.4222 0.138 Uiso 1 1 calc . . . C202 C 0.699(2) 0.2547(4) 0.5103(9) 0.140(4) Uani 1 1 d . . . H202 H 0.6987 0.2943 0.5268 0.168 Uiso 1 1 calc . . . C203 C 0.7857(17) 0.2158(8) 0.5402(5) 0.150(6) Uani 1 1 d . . . H203 H 0.8602 0.2209 0.5836 0.180 Uiso 1 1 calc . . . N204 N 0.7623(15) 0.1662(5) 0.5042(9) 0.199(6) Uani 1 1 d . . . H204 H 0.8109 0.1321 0.5144 0.239 Uiso 1 1 calc . . . C205 C 0.6355(13) 0.1807(6) 0.4428(5) 0.108(3) Uani 1 1 d . . . H205 H 0.5872 0.1556 0.4049 0.130 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 0.03512(18) 0.03785(19) 0.03095(18) -0.00222(16) 0.00507(14) -0.00288(15) Cd2 0.03611(13) 0.02975(12) 0.03800(14) 0.00164(11) 0.00001(10) -0.00539(10) Cd3 0.03007(12) 0.03672(13) 0.02921(12) -0.00380(11) 0.00605(9) 0.00266(10) Cd4 0.03267(12) 0.03191(13) 0.03716(14) 0.00000(11) 0.00789(10) -0.00026(10) CN1 0.0423(19) 0.059(2) 0.0361(18) -0.0051(18) 0.0028(14) -0.0044(17) CN'1 0.0423(19) 0.059(2) 0.0361(18) -0.0051(18) 0.0028(14) -0.0044(17) CN2 0.051(2) 0.049(2) 0.058(2) -0.008(2) 0.0248(18) 0.0002(18) CN'2 0.051(2) 0.049(2) 0.058(2) -0.008(2) 0.0248(18) 0.0002(18) C1 0.057(2) 0.041(2) 0.041(2) 0.0027(19) 0.0080(18) 0.0011(19) N1 0.082(3) 0.061(3) 0.048(2) 0.008(2) 0.011(2) 0.005(2) C2 0.041(2) 0.049(3) 0.032(2) 0.0069(19) -0.0034(16) -0.0195(19) N2 0.062(3) 0.047(2) 0.067(3) 0.004(2) -0.002(2) -0.015(2) C3 0.0379(19) 0.044(2) 0.044(2) -0.0072(18) 0.0057(16) -0.0031(16) N3 0.0401(17) 0.056(2) 0.055(2) -0.0153(19) 0.0005(16) -0.0109(16) C4 0.0401(19) 0.040(2) 0.044(2) 0.0021(18) 0.0058(16) 0.0022(16) N4 0.062(2) 0.047(2) 0.048(2) 0.0145(18) 0.0029(17) 0.0041(18) C5 0.0357(18) 0.043(2) 0.042(2) -0.0013(18) 0.0063(15) 0.0026(16) N5 0.0453(19) 0.054(2) 0.051(2) -0.0065(18) 0.0123(16) 0.0001(16) C6 0.0424(19) 0.0356(19) 0.042(2) 0.0032(17) 0.0000(16) -0.0056(16) N6 0.068(3) 0.046(2) 0.062(3) 0.0070(19) 0.008(2) -0.0119(19) C7 0.040(2) 0.040(2) 0.047(2) -0.0025(18) 0.0113(17) -0.0017(16) N7 0.059(2) 0.039(2) 0.075(3) -0.0095(19) 0.016(2) 0.0013(17) C8 0.0363(19) 0.049(2) 0.053(2) 0.001(2) 0.0030(17) -0.0024(18) N8 0.0406(18) 0.056(2) 0.062(2) 0.009(2) -0.0048(16) 0.0031(17) O1 0.0617(18) 0.0433(15) 0.0450(16) -0.0025(13) 0.0131(14) 0.0018(14) C101 0.044(2) 0.053(2) 0.046(2) -0.011(2) 0.0102(17) -0.0101(19) C102 0.0377(18) 0.045(2) 0.0364(19) -0.0068(17) 0.0014(15) -0.0033(16) C103 0.0392(19) 0.040(2) 0.0385(19) -0.0021(17) 0.0021(15) -0.0060(16) C104 0.095(4) 0.044(2) 0.037(2) 0.0041(19) 0.011(2) 0.006(2) C105 0.099(4) 0.045(3) 0.057(3) 0.017(2) 0.020(3) 0.007(3) C106 0.049(2) 0.054(3) 0.049(2) -0.003(2) 0.0018(19) 0.014(2) C107 0.048(2) 0.048(2) 0.045(2) -0.009(2) -0.0075(18) 0.0034(19) C108 0.0426(19) 0.0383(19) 0.0336(18) -0.0009(16) 0.0040(15) -0.0008(16) C109 0.066(3) 0.045(2) 0.037(2) -0.0018(18) -0.0075(19) 0.011(2) C110 0.066(3) 0.052(3) 0.039(2) -0.011(2) -0.008(2) 0.004(2) C111 0.140(6) 0.037(3) 0.103(5) -0.008(3) 0.060(5) 0.004(3) C112 0.107(5) 0.044(3) 0.072(3) -0.014(3) 0.014(3) 0.014(3) N101 0.063(2) 0.0361(18) 0.065(2) -0.0041(18) 0.0256(19) -0.0087(17) N102 0.055(2) 0.0396(18) 0.0444(19) -0.0053(16) 0.0122(16) 0.0042(16) C201 0.090(6) 0.133(9) 0.124(8) 0.042(7) 0.024(5) 0.022(6) C202 0.205(13) 0.082(6) 0.151(11) -0.007(7) 0.083(10) -0.023(7) C203 0.182(12) 0.172(12) 0.079(6) 0.039(7) -0.027(6) -0.071(11) N204 0.154(9) 0.165(9) 0.311(16) 0.155(10) 0.135(10) 0.077(7) C205 0.104(6) 0.130(8) 0.095(6) -0.035(6) 0.035(5) -0.044(6) _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles Disorder CN1 and CN'1 are atoms of a bridging cyano group. Because the center of the cyano group sits on an inversion center of the crystal, the cyano group consists of two equivalent atoms, each of which is a hybrid atom of 50% carbon and 50% nitrogen. CN1 and CN'1 are artificial atoms to treat them as a hybrid atom in the calculation. CN2 and CN'2 are atoms of a bridging cyano group. Because the center of the cyano group sits on an inversion center of the crystal, the cyano group consists of two equivalent atoms, each of which is a hybrid atom of 50% carbon and 50% nitrogen. CN2 and CN'2 are artificial atoms to treat them as a hybrid atom in the calculation. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cd1 N1 2.449(4) . . Cd1 N3 2.454(4) . . Cd1 C2 2.343(4) . . Cd1 N1 2.449(4) . 3_555 Cd1 N3 2.454(4) . 3_555 Cd1 C2 2.343(4) . 3_555 Cd2 N7 2.554(4) . . Cd2 C3 2.220(4) . . Cd2 C4 2.219(4) . . Cd2 C6 2.217(4) . . Cd2 N2 2.554(5) . 1_655 Cd3 O1 2.512(3) . . Cd3 N4 2.353(4) . . Cd3 N5 2.320(4) . . Cd3 CN1 2.352(4) . . Cd3 CN2 2.262(4) . . Cd3 N8 2.382(4) . 2_545 Cd4 C7 2.188(4) . . Cd4 C8 2.202(4) . . Cd4 C5 2.229(4) . 2_655 Cd4 C1 2.229(4) . 4_555 O1 H1 0.9835 . . O1 H2 0.8718 . . N1 C1 1.112(6) . . N2 C2 0.898(6) . . N3 C3 1.129(5) . . N4 C4 1.141(5) . . N5 C5 1.114(5) . . N6 C6 1.120(6) . . N7 C7 1.117(6) . . N8 C8 1.133(5) . . N101 C101 1.337(5) . . N101 C105 1.350(7) . . N101 C111 1.496(6) . . N102 C106 1.341(6) . . N102 C110 1.338(6) . . N102 C112 1.485(6) . . N204 C203 1.28(2) . . N204 C205 1.441(18) . . N204 H204 0.8610 . . C101 C102 1.368(6) . . C102 C103 1.390(5) . . C103 C108 1.474(6) . . C103 C104 1.370(6) . . C104 C105 1.379(6) . . C106 C107 1.373(6) . . C107 C108 1.385(6) . . C108 C109 1.393(5) . . C109 C110 1.351(6) . . C101 H101 0.9287 . . C102 H102 0.9293 . . C104 H104 0.9296 . . C105 H105 0.9292 . . C106 H106 0.9302 . . C107 H107 0.9306 . . C109 H109 0.9303 . . C110 H110 0.9315 . . C111 H131 0.9595 . . C111 H121 0.9600 . . C111 H111 0.9597 . . C112 H132 0.9589 . . C112 H112 0.9600 . . C112 H122 0.9598 . . C201 C205 1.238(19) . . C201 C202 1.28(2) . . C202 C203 1.19(2) . . C201 H201 0.9305 . . C202 H202 0.9294 . . C203 H203 0.9296 . . C205 H205 0.9288 . . 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_2 _geom_angle_site_symmetry_3 N1 Cd1 N3 88.80(13) . . . N1 Cd1 C2 87.98(14) . . . N1 Cd1 N1 180.00 . . 3_555 N1 Cd1 N3 91.20(13) . . 3_555 N1 Cd1 C2 92.02(14) . . 3_555 N3 Cd1 C2 88.42(13) . . . N1 Cd1 N3 91.20(13) 3_555 . . N3 Cd1 N3 180.00 . . 3_555 N3 Cd1 C2 91.58(13) . . 3_555 N1 Cd1 C2 92.02(14) 3_555 . . N3 Cd1 C2 91.58(13) 3_555 . . C2 Cd1 C2 180.00 . . 3_555 N1 Cd1 N3 88.80(13) 3_555 . 3_555 N1 Cd1 C2 87.98(14) 3_555 . 3_555 N3 Cd1 C2 88.42(13) 3_555 . 3_555 N7 Cd2 C3 94.61(14) . . . N7 Cd2 C4 90.54(13) . . . N7 Cd2 C6 86.38(13) . . . N2 Cd2 N7 172.96(13) 1_655 . . C3 Cd2 C4 112.56(15) . . . C3 Cd2 C6 119.26(14) . . . N2 Cd2 C3 90.75(15) 1_655 . . C4 Cd2 C6 128.17(14) . . . N2 Cd2 C4 91.62(15) 1_655 . . N2 Cd2 C6 87.02(14) 1_655 . . O1 Cd3 N4 164.68(11) . . . O1 Cd3 N5 80.77(12) . . . O1 Cd3 CN1 97.27(12) . . . O1 Cd3 CN2 86.68(13) . . . O1 Cd3 N8 77.96(12) . . 2_545 N4 Cd3 N5 93.17(13) . . . N4 Cd3 CN1 96.67(14) . . . N4 Cd3 CN2 99.28(14) . . . N4 Cd3 N8 87.46(13) . . 2_545 N5 Cd3 CN1 88.94(12) . . . N5 Cd3 CN2 167.40(14) . . . N5 Cd3 N8 84.02(12) . . 2_545 CN1 Cd3 CN2 91.56(13) . . . N8 Cd3 CN1 172.03(13) 2_545 . . N8 Cd3 CN2 94.50(13) 2_545 . . C7 Cd4 C8 119.39(15) . . . C5 Cd4 C7 107.15(15) 2_655 . . C1 Cd4 C7 117.93(15) 4_555 . . C5 Cd4 C8 102.75(15) 2_655 . . C1 Cd4 C8 105.47(15) 4_555 . . C1 Cd4 C5 101.70(15) 4_555 . 2_655 Cd3 O1 H1 106.33 . . . Cd3 O1 H2 115.47 . . . H1 O1 H2 106.13 . . . Cd1 N1 C1 169.5(4) . . . Cd2 N2 C2 176.3(5) 1_455 . . Cd1 N3 C3 177.5(3) . . . Cd3 N4 C4 165.2(4) . . . Cd3 N5 C5 178.1(4) . . . Cd2 N7 C7 140.6(3) . . . Cd3 N8 C8 167.1(3) 2_555 . . C105 N101 C111 119.5(4) . . . C101 N101 C105 120.2(4) . . . C101 N101 C111 120.3(4) . . . C106 N102 C112 118.8(4) . . . C106 N102 C110 120.5(4) . . . C110 N102 C112 120.7(4) . . . C203 N204 C205 104.0(11) . . . C205 N204 H204 128.00 . . . C203 N204 H204 128.02 . . . Cd4 C1 N1 167.3(4) 4_454 . . Cd1 C2 N2 178.9(5) . . . Cd2 C3 N3 174.0(4) . . . Cd2 C4 N4 173.0(4) . . . Cd4 C5 N5 172.5(4) 2_645 . . Cd2 C6 N6 178.1(4) . . . Cd4 C7 N7 170.5(4) . . . Cd4 C8 N8 170.2(4) . . . N101 C101 C102 121.0(3) . . . C101 C102 C103 119.7(4) . . . C104 C103 C108 121.1(3) . . . C102 C103 C108 120.2(3) . . . C102 C103 C104 118.6(4) . . . C103 C104 C105 119.8(4) . . . N101 C105 C104 120.6(4) . . . N102 C106 C107 121.0(4) . . . C106 C107 C108 119.1(4) . . . C107 C108 C109 118.1(4) . . . C103 C108 C107 120.8(3) . . . C103 C108 C109 121.0(4) . . . C108 C109 C110 120.3(4) . . . N102 C110 C109 120.8(4) . . . C102 C101 H101 119.50 . . . N101 C101 H101 119.48 . . . C103 C102 H102 120.16 . . . C101 C102 H102 120.13 . . . C105 C104 H104 119.95 . . . C103 C104 H104 120.23 . . . C104 C105 H105 119.78 . . . N101 C105 H105 119.63 . . . N102 C106 H106 119.51 . . . C107 C106 H106 119.46 . . . C106 C107 H107 120.50 . . . C108 C107 H107 120.36 . . . C110 C109 H109 119.84 . . . C108 C109 H109 119.87 . . . C109 C110 H110 119.72 . . . N102 C110 H110 119.51 . . . N101 C111 H121 109.36 . . . N101 C111 H111 109.43 . . . H111 C111 H131 109.51 . . . H121 C111 H131 109.59 . . . N101 C111 H131 109.43 . . . H111 C111 H121 109.51 . . . N102 C112 H112 109.32 . . . N102 C112 H122 109.42 . . . N102 C112 H132 109.42 . . . H112 C112 H122 109.60 . . . H112 C112 H132 109.53 . . . H122 C112 H132 109.54 . . . C202 C201 C205 110.7(11) . . . C201 C202 C203 111.0(12) . . . N204 C203 C202 110.8(12) . . . N204 C205 C201 103.5(10) . . . C202 C201 H201 124.64 . . . C205 C201 H201 124.66 . . . C201 C202 H202 124.52 . . . C203 C202 H202 124.45 . . . N204 C203 H203 124.75 . . . C202 C203 H203 124.49 . . . N204 C205 H205 128.27 . . . C201 C205 H205 128.23 . . . 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 C102 C103 C108 C107 30.6(6) . . . . C102 C103 C108 C109 -146.3(4) . . . . C104 C103 C108 C107 -153.1(4) . . . . C104 C103 C108 C109 30.1(6) . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 O1 N6 2.876(5) . 2_645 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 29.98 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.517 _refine_diff_density_min -0.547 _refine_diff_density_rms 0.107 #===END #------------------------------------------------------------------------------ data_antrr _database_code_depnum_ccdc_archive 'CCDC 269970' _audit_creation_method SHELXL-97 _chemical_formula_structural '(C12 H14 N2) (Cd6 (C N)14 (C6 H7 N)) (C6 H7 N)2' _chemical_formula_sum 'C44 H35 Cd6 N19' _chemical_formula_weight 1504.356 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 8.8965(10) _cell_length_b 11.7193(14) _cell_length_c 52.414(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.734(5) _cell_angle_gamma 90.00 _cell_volume 5415.0(11) _cell_formula_units_Z 4 _cell_measurement_temperature 113.15 _cell_measurement_reflns_used 10954 _cell_measurement_theta_min 2.9999 _cell_measurement_theta_max 25.0264 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.845 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2880 _exptl_absorpt_coefficient_mu 2.347 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6461 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 113.15 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector CCD _diffrn_measurement_device 'Mercury CCD (2x2 bin mode)' _diffrn_detector_area_resol_mean 14.6199 _diffrn_measurement_method dtintegrate.ref _diffrn_reflns_number 10031 _diffrn_reflns_av_R_equivalents 0.0880 _diffrn_reflns_av_sigmaI/netI 0.1220 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -60 _diffrn_reflns_limit_l_max 62 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.02 _reflns_number_total 9523 _reflns_number_gt 9344 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+281.0233P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 9523 _refine_ls_number_parameters 602 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0942 _refine_ls_R_factor_gt 0.0918 _refine_ls_wR_factor_ref 0.1939 _refine_ls_wR_factor_gt 0.1927 _refine_ls_goodness_of_fit_ref 1.259 _refine_ls_restrained_S_all 1.259 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.32424(10) 0.11561(8) 0.069171(18) 0.0109(2) Uani 1 1 d . . . Cd2 Cd 0.36123(11) 0.15717(8) 0.179368(18) 0.0118(2) Uani 1 1 d . . . Cd3 Cd 0.88661(11) 0.44135(8) 0.183231(19) 0.0136(2) Uani 1 1 d . . . Cd4 Cd 0.83484(11) 0.41036(8) 0.072676(19) 0.0128(2) Uani 1 1 d . . . Cd5 Cd 0.87510(11) 0.90377(8) 0.210587(19) 0.0143(2) Uani 1 1 d . . . Cd6 Cd 0.78286(11) 0.86560(8) 0.038954(18) 0.0121(2) Uani 1 1 d . . . C1 C 0.3469(14) 0.1238(10) 0.1356(2) 0.010(3) Uani 1 1 d . . . N1 N 0.3402(15) 0.1160(10) 0.1140(3) 0.025(3) Uani 1 1 d . . . C2 C 0.6408(17) 0.2926(12) 0.0686(3) 0.019(3) Uani 1 1 d . . . N2 N 0.5361(12) 0.2323(9) 0.0698(2) 0.012(2) Uiso 1 1 d . . . C3 C -0.0048(16) -0.0477(12) 0.0548(3) 0.017(3) Uani 1 1 d . . . N3 N 0.1044(14) -0.0022(10) 0.0629(2) 0.020(3) Uani 1 1 d . . . C4 C 0.2705(15) 0.1312(12) 0.0031(3) 0.017(3) Uani 1 1 d . . . N4 N 0.2958(14) 0.1265(11) 0.0253(2) 0.022(3) Uani 1 1 d . . . C5 C 0.5904(16) -0.0785(12) 0.0590(3) 0.019(3) Uani 1 1 d . . . N5 N 0.4881(14) -0.0413(10) 0.0675(2) 0.022(3) Uani 1 1 d . . . C6 C 0.0524(19) 0.3277(12) 0.0684(3) 0.022(3) Uani 1 1 d . . . N6 N 0.1599(13) 0.2769(10) 0.0676(2) 0.016(2) Uani 1 1 d . . . C7 C 0.1052(17) 0.3740(12) 0.1746(3) 0.018(3) Uani 1 1 d . . . N7 N 0.2131(14) 0.3245(10) 0.1710(2) 0.021(3) Uani 1 1 d . . . C8 C 0.0436(17) 0.0015(12) 0.1912(3) 0.019(3) Uani 1 1 d . . . N8 N 0.1406(14) 0.0538(10) 0.1844(2) 0.020(3) Uani 1 1 d . . . C9 C 0.6412(18) -0.0286(12) 0.2013(3) 0.018(3) Uani 1 1 d . . . N9 N 0.5283(14) 0.0130(10) 0.1940(2) 0.019(3) Uani 1 1 d . . . C10 C 0.6878(16) 0.3317(12) 0.1803(3) 0.016(3) Uani 1 1 d . . . N10 N 0.5783(14) 0.2716(11) 0.1783(2) 0.023(3) Uani 1 1 d . . . C11 C 0.8358(15) 0.4530(11) 0.1145(3) 0.017(3) Uani 1 1 d . . . N11 N 0.8253(13) 0.4664(10) 0.1361(2) 0.017(3) Uani 1 1 d . . . C12 C 0.8737(17) 0.6267(11) 0.1910(3) 0.017(3) Uani 1 1 d . . . N12 N 0.8723(15) 0.7218(12) 0.1963(2) 0.025(3) Uani 1 1 d . . . C13 C 1.0269(16) 0.3977(13) 0.2489(3) 0.020(3) Uani 1 1 d . . . N13 N 0.9628(16) 0.4036(12) 0.2280(3) 0.031(3) Uani 1 1 d . . . C14 C 0.8144(15) 0.5811(11) 0.0543(3) 0.014(3) Uani 1 1 d . . . N14 N 0.8099(13) 0.6779(10) 0.0488(2) 0.018(3) Uani 1 1 d . . . N101 N 0.4667(14) 0.5210(9) 0.1195(2) 0.017(3) Uani 1 1 d . . . C101 C 0.4955(15) 0.5732(12) 0.1427(3) 0.016(3) Uani 1 1 d . . . H101 H 0.4667 0.5378 0.1572 0.020 Uiso 1 1 calc . . . C102 C 0.5669(16) 0.6781(12) 0.1453(3) 0.017(3) Uani 1 1 d . . . H102 H 0.5795 0.7161 0.1610 0.020 Uiso 1 1 calc . . . C103 C 0.6199(15) 0.7260(11) 0.1238(3) 0.014(3) Uani 1 1 d . . . C104 C 0.5863(15) 0.6707(11) 0.1003(3) 0.015(3) Uani 1 1 d . . . H104 H 0.6144 0.7033 0.0854 0.018 Uiso 1 1 calc . . . C105 C 0.5112(14) 0.5672(11) 0.0989(2) 0.010(3) Uiso 1 1 d . . . H105 H 0.4917 0.5297 0.0832 0.012 Uiso 1 1 calc . . . N102 N 0.8465(12) 1.0456(9) 0.1276(2) 0.013(2) Uani 1 1 d . . . C106 C 0.7216(16) 1.0339(12) 0.1390(3) 0.022(3) Uani 1 1 d . . . H106 H 0.6859 1.0956 0.1476 0.026 Uiso 1 1 calc . . . C107 C 0.6457(15) 0.9314(11) 0.1381(3) 0.015(3) Uani 1 1 d . . . H107 H 0.5575 0.9239 0.1457 0.018 Uiso 1 1 calc . . . C108 C 0.7028(15) 0.8389(12) 0.1257(3) 0.015(3) Uani 1 1 d . . . C109 C 0.8313(16) 0.8508(12) 0.1141(3) 0.016(3) Uiso 1 1 d . . . H109 H 0.8676 0.7900 0.1053 0.019 Uiso 1 1 calc . . . C110 C 0.9083(16) 0.9582(12) 0.1158(3) 0.015(3) Uiso 1 1 d . . . H110 H 0.9985 0.9677 0.1089 0.019 Uiso 1 1 calc . . . C111 C 0.3928(17) 0.4074(12) 0.1183(3) 0.022(3) Uani 1 1 d . . . H111 H 0.3414 0.3945 0.1013 0.033 Uiso 1 1 calc . . . H121 H 0.3209 0.4047 0.1304 0.033 Uiso 1 1 calc . . . H131 H 0.4683 0.3494 0.1225 0.033 Uiso 1 1 calc . . . C112 C 0.9237(18) 1.1601(13) 0.1280(3) 0.025(3) Uani 1 1 d . . . H112 H 0.8555 1.2181 0.1324 0.038 Uiso 1 1 calc . . . H122 H 0.9520 1.1759 0.1114 0.038 Uiso 1 1 calc . . . H132 H 1.0128 1.1592 0.1406 0.038 Uiso 1 1 calc . . . N201 N 0.2341(15) 0.7201(11) 0.0745(2) 0.024(3) Uani 1 1 d . . . H201 H 0.2074 0.6588 0.0660 0.037 Uiso 1 1 calc . . . H211 H 0.2771 0.7746 0.0672 0.037 Uiso 1 1 calc . . . C201 C 0.2076(15) 0.7313(11) 0.1002(3) 0.015(3) Uani 1 1 d . . . C202 C 0.1391(16) 0.6461(12) 0.1126(3) 0.022(3) Uani 1 1 d . . . H202 H 0.1052 0.5807 0.1036 0.027 Uiso 1 1 calc . . . C203 C 0.1197(17) 0.6557(13) 0.1383(3) 0.025(3) Uani 1 1 d . . . H203 H 0.0679 0.5987 0.1458 0.030 Uiso 1 1 calc . . . C204 C 0.1754(17) 0.7480(13) 0.1529(3) 0.022(3) Uani 1 1 d . . . H204 H 0.1672 0.7519 0.1704 0.026 Uiso 1 1 calc . . . C205 C 0.2445(16) 0.8353(12) 0.1406(3) 0.018(3) Uani 1 1 d . . . H205 H 0.2803 0.8995 0.1500 0.021 Uiso 1 1 calc . . . C206 C 0.2609(16) 0.8280(11) 0.1145(3) 0.018(3) Uani 1 1 d . . . H206 H 0.3070 0.8871 0.1065 0.021 Uiso 1 1 calc . . . N301 N 0.3541(15) 0.2295(12) 0.2225(3) 0.028(3) Uani 1 1 d . . . H301 H 0.2642 0.2030 0.2182 0.042 Uiso 1 1 calc . . . H311 H 0.3867 0.2846 0.2139 0.042 Uiso 1 1 calc . . . C301 C 0.4507(17) 0.1814(14) 0.2444(3) 0.025(3) Uani 1 1 d . . . C302 C 0.398(2) 0.0937(15) 0.2580(3) 0.036(4) Uani 1 1 d . . . H302 H 0.2991 0.0673 0.2541 0.043 Uiso 1 1 calc . . . C303 C 0.500(3) 0.0436(17) 0.2786(4) 0.051(6) Uani 1 1 d . . . H303 H 0.4650 -0.0127 0.2888 0.062 Uiso 1 1 calc . . . C304 C 0.651(3) 0.0796(18) 0.2831(4) 0.058(6) Uani 1 1 d . . . H304 H 0.7186 0.0454 0.2958 0.069 Uiso 1 1 calc . . . C305 C 0.695(3) 0.164(2) 0.2686(4) 0.057(6) Uani 1 1 d . . . H305 H 0.7950 0.1902 0.2721 0.069 Uiso 1 1 calc . . . C306 C 0.600(2) 0.2146(16) 0.2491(4) 0.036(4) Uani 1 1 d . . . H306 H 0.6363 0.2709 0.2390 0.043 Uiso 1 1 calc . . . N401 N 0.3863(16) 0.4694(13) 0.0369(3) 0.035(3) Uani 1 1 d . . . H401 H 0.3317 0.4189 0.0432 0.052 Uiso 1 1 calc . . . H411 H 0.4836 0.4636 0.0393 0.052 Uiso 1 1 calc . . . C401 C 0.3179(17) 0.5597(13) 0.0230(3) 0.021(3) Uani 1 1 d . . . C402 C 0.405(2) 0.6431(17) 0.0127(4) 0.038(4) Uani 1 1 d . . . H402 H 0.5104 0.6368 0.0154 0.045 Uiso 1 1 calc . . . C403 C 0.341(2) 0.7346(17) -0.0015(3) 0.039(4) Uani 1 1 d . . . H403 H 0.4007 0.7860 -0.0091 0.046 Uiso 1 1 calc . . . C404 C 0.1832(19) 0.7482(14) -0.0041(3) 0.033(4) Uani 1 1 d . . . H404 H 0.1391 0.8131 -0.0122 0.039 Uiso 1 1 calc . . . C405 C 0.0933(17) 0.6670(15) 0.0050(3) 0.029(4) Uani 1 1 d . . . H405 H -0.0117 0.6741 0.0022 0.035 Uiso 1 1 calc . . . C406 C 0.1618(19) 0.5717(13) 0.0188(3) 0.027(4) Uani 1 1 d . . . H406 H 0.1009 0.5168 0.0251 0.033 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 0.0105(5) 0.0083(4) 0.0139(5) 0.0003(4) 0.0015(4) -0.0007(4) Cd2 0.0102(5) 0.0101(5) 0.0149(5) 0.0001(4) 0.0011(4) 0.0004(4) Cd3 0.0106(5) 0.0119(5) 0.0180(5) -0.0004(4) 0.0013(4) -0.0004(4) Cd4 0.0108(5) 0.0089(5) 0.0189(5) 0.0006(4) 0.0021(4) -0.0001(4) Cd5 0.0146(5) 0.0114(5) 0.0168(5) 0.0010(4) 0.0022(4) 0.0007(4) Cd6 0.0114(5) 0.0101(5) 0.0148(5) 0.0003(4) 0.0014(4) -0.0002(4) C1 0.009(6) 0.005(6) 0.014(7) -0.002(5) 0.000(5) -0.003(5) N1 0.034(8) 0.015(6) 0.025(8) 0.000(5) 0.003(6) 0.004(6) C2 0.027(8) 0.014(7) 0.018(7) 0.001(6) 0.006(6) 0.007(6) C3 0.016(7) 0.012(7) 0.026(8) -0.007(6) 0.010(6) -0.011(6) N3 0.022(7) 0.011(6) 0.027(7) -0.001(5) 0.003(6) 0.003(5) C4 0.009(7) 0.013(7) 0.030(9) 0.002(6) 0.010(6) 0.001(5) N4 0.019(6) 0.023(7) 0.023(7) 0.002(5) 0.005(5) 0.002(5) C5 0.013(7) 0.021(7) 0.024(8) 0.010(6) 0.000(6) 0.003(6) N5 0.024(7) 0.020(6) 0.022(7) -0.010(5) 0.005(5) 0.009(6) C6 0.043(10) 0.009(7) 0.015(7) 0.009(6) 0.005(7) 0.007(7) N6 0.011(6) 0.015(6) 0.020(6) -0.002(5) -0.001(5) 0.001(5) C7 0.022(8) 0.009(6) 0.023(8) 0.002(6) 0.000(6) -0.006(6) N7 0.023(7) 0.017(6) 0.021(7) -0.002(5) -0.001(5) 0.003(5) C8 0.024(8) 0.021(7) 0.014(7) 0.008(6) 0.007(6) 0.011(6) N8 0.026(7) 0.015(6) 0.021(6) 0.013(5) 0.012(5) 0.002(5) C9 0.031(9) 0.014(7) 0.012(7) -0.005(6) 0.010(6) 0.001(6) N9 0.022(7) 0.009(6) 0.026(7) 0.008(5) 0.001(5) 0.009(5) C10 0.018(7) 0.015(7) 0.014(7) -0.005(6) 0.001(6) 0.002(6) N10 0.021(7) 0.022(6) 0.025(7) -0.002(5) 0.002(5) -0.008(6) C11 0.012(7) 0.004(6) 0.040(10) 0.002(6) 0.015(6) -0.001(5) N11 0.010(6) 0.014(6) 0.026(7) 0.001(5) -0.003(5) 0.003(5) C12 0.028(8) 0.003(6) 0.022(7) -0.001(5) 0.016(6) -0.004(6) N12 0.022(7) 0.040(9) 0.016(6) 0.007(6) 0.010(5) 0.000(6) C13 0.020(8) 0.029(8) 0.011(7) -0.002(6) 0.002(6) -0.001(6) N13 0.035(8) 0.025(7) 0.030(8) -0.003(6) -0.008(6) -0.006(6) C14 0.013(7) 0.015(7) 0.013(7) 0.004(5) 0.003(5) 0.011(5) N14 0.014(6) 0.019(7) 0.022(6) 0.000(5) 0.009(5) 0.004(5) N101 0.029(7) 0.003(5) 0.020(6) 0.000(5) 0.005(5) 0.002(5) C101 0.011(7) 0.017(7) 0.023(7) 0.000(6) 0.009(6) 0.002(6) C102 0.017(7) 0.012(7) 0.021(7) -0.001(6) 0.001(6) 0.007(6) C103 0.013(7) 0.007(6) 0.022(7) 0.001(5) 0.000(6) 0.003(5) C104 0.013(7) 0.010(6) 0.024(7) 0.001(6) 0.006(6) 0.008(5) N102 0.013(6) 0.005(5) 0.019(6) 0.004(4) -0.001(5) -0.006(4) C106 0.016(7) 0.013(7) 0.039(9) -0.010(6) 0.009(7) 0.001(6) C107 0.016(7) 0.012(7) 0.020(7) -0.003(6) 0.007(6) -0.006(5) C108 0.016(7) 0.014(7) 0.011(6) 0.003(5) -0.012(5) -0.002(6) C111 0.026(8) 0.013(7) 0.029(8) -0.004(6) 0.013(7) -0.011(6) C112 0.028(8) 0.013(7) 0.033(9) 0.002(6) -0.003(7) -0.008(6) N201 0.023(7) 0.028(7) 0.022(7) -0.001(6) 0.003(5) 0.010(6) C201 0.006(6) 0.013(7) 0.026(8) -0.003(6) -0.002(5) 0.007(5) C202 0.014(7) 0.016(7) 0.035(9) 0.006(6) -0.006(6) 0.009(6) C203 0.023(8) 0.016(7) 0.036(9) 0.000(7) 0.004(7) -0.017(6) C204 0.018(7) 0.030(8) 0.019(7) 0.006(6) 0.008(6) 0.012(6) C205 0.019(7) 0.014(7) 0.019(7) -0.005(6) -0.001(6) -0.003(6) C206 0.014(7) 0.010(6) 0.030(8) -0.002(6) 0.005(6) 0.002(5) N301 0.023(7) 0.034(8) 0.024(7) 0.003(6) -0.008(6) 0.017(6) C301 0.021(8) 0.032(9) 0.025(8) -0.015(7) 0.008(6) -0.002(7) C302 0.055(12) 0.032(9) 0.024(9) 0.006(7) 0.022(8) -0.008(9) C303 0.101(19) 0.030(10) 0.030(10) 0.006(8) 0.033(12) 0.007(11) C304 0.093(19) 0.039(12) 0.040(12) 0.019(10) 0.000(12) 0.022(12) C305 0.058(14) 0.071(15) 0.036(11) 0.013(11) -0.021(10) -0.003(12) C306 0.025(9) 0.038(10) 0.041(10) 0.005(8) -0.007(8) -0.005(8) N401 0.032(8) 0.035(8) 0.037(8) -0.004(7) 0.005(7) 0.002(7) C401 0.020(8) 0.025(8) 0.019(7) 0.001(6) 0.000(6) 0.000(6) C402 0.025(9) 0.053(12) 0.035(10) -0.004(9) 0.004(8) 0.003(8) C403 0.043(11) 0.053(12) 0.023(9) 0.006(8) 0.015(8) -0.012(9) C404 0.026(9) 0.028(9) 0.040(10) 0.017(8) -0.013(8) 0.003(7) C405 0.012(7) 0.037(9) 0.035(9) -0.006(8) -0.009(7) 0.005(7) C406 0.031(9) 0.018(8) 0.034(9) -0.002(7) 0.010(7) 0.003(7) _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cd1 N1 2.335(16) . . Cd1 N2 2.325(11) . . Cd1 N3 2.380(12) . . Cd1 N4 2.283(10) . . Cd1 N5 2.356(12) . . Cd1 N6 2.384(12) . . Cd2 N7 2.370(12) . . Cd2 N8 2.351(12) . . Cd2 N9 2.312(12) . . Cd2 N10 2.358(13) . . Cd2 N301 2.423(15) . . Cd2 C1 2.314(10) . . Cd3 N11 2.475(10) . . Cd3 N13 2.394(16) . . Cd3 C10 2.175(14) . . Cd3 C12 2.216(13) . . Cd3 C7 2.201(15) . 1_655 Cd4 C2 2.198(15) . . Cd4 C11 2.247(15) . . Cd4 C14 2.218(13) . . Cd4 C6 2.203(17) . 1_655 Cd5 N12 2.259(14) . . Cd5 C9 2.219(16) . 1_565 Cd5 C8 2.236(15) . 1_665 Cd5 C13 2.185(16) . 2_755 Cd6 N14 2.265(12) . . Cd6 C5 2.225(15) . 1_565 Cd6 C3 2.207(15) . 1_665 Cd6 C4 2.192(16) . 3_665 N1 C1 1.129(19) . . N2 C2 1.178(18) . . N3 C3 1.139(19) . . N4 C4 1.156(19) . . N5 C5 1.152(19) . . N6 C6 1.13(2) . . N7 C7 1.159(19) . . N8 C8 1.153(19) . . N9 C9 1.14(2) . . N10 C10 1.195(19) . . N11 C11 1.159(19) . . N12 C12 1.149(19) . . N13 C13 1.17(2) . . N14 C14 1.170(18) . . N301 C301 1.45(2) . . N101 C111 1.482(18) . . N101 C105 1.316(16) . . N101 C101 1.355(19) . . N102 C110 1.351(18) . . N102 C106 1.338(18) . . N102 C112 1.506(19) . . N201 C201 1.405(19) . . N401 C401 1.38(2) . . C101 C102 1.38(2) . . C301 C302 1.37(2) . . C301 C306 1.37(2) . . C302 C303 1.44(3) . . C102 C103 1.40(2) . . C103 C108 1.512(19) . . C303 C304 1.40(4) . . C103 C104 1.39(2) . . C104 C105 1.382(18) . . C304 C305 1.34(3) . . C305 C306 1.37(3) . . C106 C107 1.376(19) . . C107 C108 1.39(2) . . C108 C109 1.37(2) . . C109 C110 1.43(2) . . C201 C202 1.38(2) . . C201 C206 1.405(19) . . C202 C203 1.39(2) . . C203 C204 1.38(2) . . C204 C205 1.40(2) . . C205 C206 1.40(2) . . C401 C406 1.38(2) . . C401 C402 1.40(2) . . C402 C403 1.38(3) . . C403 C404 1.40(2) . . C404 C405 1.37(2) . . C405 C406 1.42(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_2 _geom_angle_site_symmetry_3 N1 Cd1 N2 92.6(4) . . . N1 Cd1 N3 94.5(4) . . . N1 Cd1 N4 175.6(4) . . . N1 Cd1 N5 94.9(4) . . . N1 Cd1 N6 89.3(4) . . . N2 Cd1 N3 172.9(4) . . . N2 Cd1 N4 87.8(4) . . . N2 Cd1 N5 87.4(4) . . . N2 Cd1 N6 91.5(4) . . . N3 Cd1 N4 85.2(4) . . . N3 Cd1 N5 92.5(4) . . . N3 Cd1 N6 88.1(4) . . . N4 Cd1 N5 89.5(4) . . . N4 Cd1 N6 86.4(4) . . . N5 Cd1 N6 175.8(4) . . . N7 Cd2 N8 89.7(4) . . . N7 Cd2 N9 169.3(4) . . . N7 Cd2 N10 87.8(4) . . . N7 Cd2 N301 78.4(4) . . . N7 Cd2 C1 90.1(4) . . . N8 Cd2 N9 95.5(4) . . . N8 Cd2 N10 173.9(4) . . . N8 Cd2 N301 87.1(4) . . . N8 Cd2 C1 95.1(4) . . . N9 Cd2 N10 86.1(4) . . . N9 Cd2 N301 92.4(4) . . . N9 Cd2 C1 98.8(4) . . . N10 Cd2 N301 87.0(4) . . . N10 Cd2 C1 90.5(4) . . . N301 Cd2 C1 168.3(4) . . . N11 Cd3 N13 174.6(4) . . . N11 Cd3 C10 86.1(5) . . . N11 Cd3 C12 93.3(5) . . . N11 Cd3 C7 85.4(5) . . 1_655 N13 Cd3 C10 94.6(5) . . . N13 Cd3 C12 90.9(5) . . . N13 Cd3 C7 89.6(5) . . 1_655 C10 Cd3 C12 122.0(5) . . . C7 Cd3 C10 120.4(5) 1_655 . . C7 Cd3 C12 117.3(5) 1_655 . . C2 Cd4 C11 97.7(5) . . . C2 Cd4 C14 120.5(5) . . . C2 Cd4 C6 113.8(5) . . 1_655 C11 Cd4 C14 102.3(5) . . . C6 Cd4 C11 108.0(5) 1_655 . . C6 Cd4 C14 112.0(5) 1_655 . . N12 Cd5 C9 107.2(5) . . 1_565 N12 Cd5 C8 108.1(5) . . 1_665 N12 Cd5 C13 106.1(5) . . 2_755 C8 Cd5 C9 112.6(5) 1_665 . 1_565 C9 Cd5 C13 117.7(6) 1_565 . 2_755 C8 Cd5 C13 104.7(6) 1_665 . 2_755 N14 Cd6 C5 104.1(5) . . 1_565 N14 Cd6 C3 107.6(5) . . 1_665 N14 Cd6 C4 104.4(5) . . 3_665 C3 Cd6 C5 111.2(5) 1_665 . 1_565 C4 Cd6 C5 113.2(5) 3_665 . 1_565 C3 Cd6 C4 115.4(5) 1_665 . 3_665 Cd1 N1 C1 175.5(11) . . . Cd1 N2 C2 176.1(11) . . . Cd1 N3 C3 165.2(11) . . . Cd1 N4 C4 175.2(12) . . . Cd1 N5 C5 146.6(11) . . . Cd1 N6 C6 158.9(11) . . . Cd2 N7 C7 146.8(11) . . . Cd2 N8 C8 168.3(11) . . . Cd2 N9 C9 157.8(12) . . . Cd2 N10 C10 173.5(11) . . . Cd3 N11 C11 157.4(11) . . . Cd5 N12 C12 174.7(11) . . . Cd3 N13 C13 165.7(13) . . . Cd6 N14 C14 175.6(11) . . . Cd2 N301 C301 121.0(10) . . . C101 N101 C111 118.2(11) . . . C105 N101 C111 121.0(11) . . . C101 N101 C105 120.6(11) . . . C106 N102 C110 122.7(12) . . . C110 N102 C112 118.0(11) . . . C106 N102 C112 119.3(11) . . . Cd2 C1 N1 174.9(11) . . . Cd4 C2 N2 171.2(13) . . . Cd6 C3 N3 179.5(15) 1_445 . . Cd6 C4 N4 177.8(13) 3_665 . . Cd6 C5 N5 173.1(13) 1_545 . . Cd4 C6 N6 173.4(13) 1_455 . . Cd3 C7 N7 170.8(12) 1_455 . . Cd5 C8 N8 171.0(13) 1_445 . . Cd5 C9 N9 171.2(13) 1_545 . . Cd3 C10 N10 179.0(13) . . . Cd4 C11 N11 173.1(12) . . . Cd3 C12 N12 176.2(12) . . . Cd5 C13 N13 172.2(13) 2_745 . . Cd4 C14 N14 168.6(12) . . . N301 C301 C302 119.7(14) . . . C302 C301 C306 120.7(16) . . . N101 C101 C102 121.3(13) . . . N301 C301 C306 119.1(15) . . . C301 C302 C303 118.1(17) . . . C101 C102 C103 118.6(14) . . . C104 C103 C108 120.8(13) . . . C102 C103 C108 120.9(13) . . . C102 C103 C104 118.2(12) . . . C302 C303 C304 119.9(19) . . . C103 C104 C105 120.1(13) . . . N101 C105 C104 121.0(11) . . . C301 C306 C305 119.7(19) . . . N102 C106 C107 120.5(13) . . . C106 C107 C108 119.1(13) . . . C103 C108 C109 119.2(13) . . . C103 C108 C107 120.4(12) . . . C107 C108 C109 120.3(13) . . . C108 C109 C110 118.9(13) . . . N102 C110 C109 118.3(13) . . . C202 C201 C206 118.2(14) . . . N201 C201 C202 121.8(13) . . . N201 C201 C206 119.9(13) . . . C201 C202 C203 121.4(14) . . . C202 C203 C204 121.4(14) . . . C203 C204 C205 117.8(14) . . . C204 C205 C206 121.2(13) . . . C201 C206 C205 119.9(13) . . . N401 C401 C402 120.8(15) . . . N401 C401 C406 121.6(14) . . . C402 C401 C406 117.6(15) . . . C401 C402 C403 122.7(16) . . . C402 C403 C404 118.4(16) . . . C403 C404 C405 120.8(16) . . . C404 C405 C406 119.5(15) . . . C401 C406 C405 120.9(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 C102 C103 C108 C107 -47(2) . . . . C102 C103 C108 C109 136.1(15) . . . . C104 C103 C108 C107 129.3(15) . . . . C104 C103 C108 C109 -48(2) . . . . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.698 _refine_diff_density_min -2.108 _refine_diff_density_rms 0.271 #===END