Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Nirmalendu Chaudhuri' _publ_contact_author_address ; Department of Inorganic Chemistry Indian Association for the Cultivation of Science Kolkata 700 032 INDIA ; _publ_contact_author_email ICNRC@IACS.RES.IN _publ_section_title ; Towards rational design of supramolecular helices using linear pseudohalides in Cd(II) 2,2'-biimidazole system ; loop_ _publ_author_name 'Nirmalendu Chaudhuri' 'Ananta Kumar Ghosh' 'Debajyoti Ghoshal' 'Atish Dipankar Jana' 'Golam Mostafa' data_Complex1 _database_code_depnum_ccdc_archive 'CCDC 623785' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H12 Cd N10 S2' _chemical_formula_sum 'C14 H12 Cd N10 S2' _chemical_formula_weight 496.89 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' S S 0.1246 0.1234 '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_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,y,1/2-z 3 -x,-y,-z 4 x,-y,1/2+z 5 1/2+x,1/2+y,z 6 1/2-x,1/2+y,1/2-z 7 1/2-x,1/2-y,-z 8 1/2+x,1/2-y,1/2+z _cell_length_a 15.214(2) _cell_length_b 25.819(2) _cell_length_c 19.042(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.003(2) _cell_angle_gamma 90.00 _cell_volume 7451.2(14) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.772 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3936 _exptl_absorpt_coefficient_mu 1.419 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30345 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8546 _reflns_number_gt 5612 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for windows (Farugia 1997)' _computing_publication_material 'PLATON-2003 (Spek 2003)' _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^)+(0.0224P)^2^+14.4051P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8546 _refine_ls_number_parameters 488 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0944 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.1124 _refine_ls_wR_factor_gt 0.1002 _refine_ls_goodness_of_fit_ref 1.215 _refine_ls_restrained_S_all 1.215 _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 C1 C 0.5721(3) 0.7172(2) 0.8499(3) 0.0525(13) Uani 1 1 d . . . H1 H 0.5330 0.6950 0.8246 0.063 Uiso 1 1 calc R . . C2 C 0.5563(4) 0.7420(2) 0.9099(3) 0.0643(16) Uani 1 1 d . . . H2 H 0.5050 0.7402 0.9330 0.077 Uiso 1 1 calc R . . C3 C 0.6867(3) 0.76170(16) 0.8815(2) 0.0363(10) Uani 1 1 d . . . C4 C 0.7735(3) 0.78395(17) 0.8798(2) 0.0380(10) Uani 1 1 d . . . C5 C 0.8966(4) 0.8259(2) 0.9044(3) 0.0604(14) Uani 1 1 d . . . H5 H 0.9401 0.8472 0.9263 0.072 Uiso 1 1 calc R . . C6 C 0.9013(3) 0.7990(2) 0.8443(3) 0.0526(13) Uani 1 1 d . . . H6 H 0.9493 0.7987 0.8173 0.063 Uiso 1 1 calc R . . C7 C 0.9355(3) 0.6889(2) 0.6504(3) 0.0529(13) Uani 1 1 d . . . H7 H 0.9659 0.6632 0.6767 0.064 Uiso 1 1 calc R . . C8 C 0.9583(3) 0.7076(2) 0.5894(3) 0.0587(14) Uani 1 1 d . . . H8 H 1.0062 0.6973 0.5656 0.070 Uiso 1 1 calc R . . C9 C 0.8396(3) 0.74730(17) 0.6180(2) 0.0356(10) Uani 1 1 d . . . C10 C 0.7622(3) 0.77976(17) 0.6185(2) 0.0373(10) Uani 1 1 d . . . C11 C 0.6573(4) 0.8355(2) 0.5924(3) 0.0614(15) Uani 1 1 d . . . H11 H 0.6225 0.8613 0.5701 0.074 Uiso 1 1 calc R . . C12 C 0.6427(4) 0.8107(2) 0.6525(3) 0.0560(13) Uani 1 1 d . . . H12 H 0.5949 0.8167 0.6787 0.067 Uiso 1 1 calc R . . C13 C 0.6489(3) 0.66330(19) 0.6011(2) 0.0487(12) Uani 1 1 d . . . C14 C 0.8118(3) 0.64823(17) 0.9011(2) 0.0424(11) Uani 1 1 d . . . C15 C 0.1114(4) 0.0606(2) 0.8480(3) 0.0567(14) Uani 1 1 d . . . H15 H 0.1598 0.0662 0.8224 0.068 Uiso 1 1 calc R . . C16 C 0.0943(4) 0.0861(2) 0.9072(3) 0.0616(15) Uani 1 1 d . . . H16 H 0.1282 0.1124 0.9294 0.074 Uiso 1 1 calc R . . C17 C -0.0095(3) 0.02924(17) 0.8812(2) 0.0394(11) Uani 1 1 d . . . C18 C -0.0867(3) -0.00206(18) 0.8811(2) 0.0381(10) Uani 1 1 d . . . C19 C -0.2069(4) -0.0404(2) 0.9090(3) 0.0631(15) Uani 1 1 d . . . H19 H -0.2556 -0.0504 0.9321 0.076 Uiso 1 1 calc R . . C20 C -0.1820(3) -0.05907(19) 0.8464(3) 0.0507(12) Uani 1 1 d . . . H20 H -0.2118 -0.0844 0.8190 0.061 Uiso 1 1 calc R . . C21 C -0.0992(3) -0.08821(19) 0.6002(2) 0.0484(12) Uani 1 1 d . . . C22 C 0.1475(3) 0.54932(19) 0.8426(3) 0.0520(13) Uani 1 1 d . . . H22 H 0.1945 0.5495 0.8145 0.062 Uiso 1 1 calc R . . C23 C 0.1453(4) 0.5752(2) 0.9034(3) 0.0638(15) Uani 1 1 d . . . H23 H 0.1896 0.5960 0.9251 0.077 Uiso 1 1 calc R . . C24 C 0.0217(3) 0.53253(17) 0.8801(2) 0.0398(10) Uani 1 1 d . . . C25 C -0.0644(3) 0.51102(17) 0.8828(2) 0.0372(10) Uani 1 1 d . . . C26 C -0.1955(4) 0.4909(2) 0.9123(3) 0.0608(15) Uani 1 1 d . . . H26 H -0.2464 0.4891 0.9360 0.073 Uiso 1 1 calc R . . C27 C -0.1801(3) 0.4653(2) 0.8520(2) 0.0542(13) Uani 1 1 d . . . H27 H -0.2188 0.4426 0.8272 0.065 Uiso 1 1 calc R . . C28 C -0.0627(3) 0.39992(19) 0.5988(2) 0.0482(12) Uani 1 1 d . . . N1 N 0.6540(3) 0.72972(15) 0.83219(18) 0.0421(9) Uani 1 1 d . . . N2 N 0.8246(2) 0.77228(14) 0.82918(18) 0.0399(9) Uani 1 1 d . . . N3 N 0.8607(2) 0.71319(15) 0.66852(17) 0.0395(8) Uani 1 1 d . . . N4 N 0.7080(3) 0.77556(14) 0.66936(18) 0.0409(9) Uani 1 1 d . . . N5 N 0.6292(3) 0.76988(15) 0.92980(18) 0.0462(10) Uani 1 1 d . . . H5N H 0.6372 0.7892 0.9665 0.055 Uiso 1 1 calc R . . N6 N 0.8152(3) 0.81558(15) 0.9273(2) 0.0514(11) Uani 1 1 d . . . H6N H 0.7949 0.8273 0.9650 0.062 Uiso 1 1 calc R . . N7 N 0.8973(3) 0.74527(16) 0.56835(19) 0.0500(10) Uani 1 1 d . . . H7N H 0.8964 0.7638 0.5308 0.060 Uiso 1 1 calc R . . N8 N 0.7336(3) 0.81522(15) 0.57087(19) 0.0500(10) Uani 1 1 d . . . H8N H 0.7585 0.8237 0.5337 0.060 Uiso 1 1 calc R . . N9 N 0.7943(3) 0.66048(19) 0.9567(2) 0.0711(14) Uani 1 1 d . . . N10 N 0.6471(4) 0.68145(18) 0.5456(2) 0.0713(14) Uani 1 1 d . . . N11 N 0.0455(3) 0.02490(14) 0.83155(19) 0.0431(9) Uani 1 1 d . . . N12 N -0.1076(2) -0.03508(15) 0.83040(17) 0.0413(9) Uani 1 1 d . . . N13 N 0.0182(3) 0.06616(16) 0.9281(2) 0.0539(11) Uani 1 1 d . . . H13N H -0.0076 0.0754 0.9645 0.065 Uiso 1 1 calc R . . N14 N -0.1449(3) -0.00388(16) 0.93038(19) 0.0506(10) Uani 1 1 d . . . H14N H -0.1435 0.0144 0.9682 0.061 Uiso 1 1 calc R . . N15 N -0.1000(4) -0.07060(19) 0.5445(2) 0.0739(15) Uani 1 1 d . . . N16 N 0.0705(3) 0.52261(14) 0.82803(19) 0.0436(9) Uani 1 1 d . . . N17 N -0.0983(3) 0.47861(15) 0.83397(18) 0.0426(9) Uani 1 1 d . . . N18 N 0.0647(3) 0.56487(15) 0.92744(19) 0.0503(10) Uani 1 1 d . . . H18N H 0.0452 0.5767 0.9653 0.060 Uiso 1 1 calc R . . N19 N -0.1220(3) 0.51938(16) 0.93112(19) 0.0516(11) Uani 1 1 d . . . H19N H -0.1140 0.5392 0.9674 0.062 Uiso 1 1 calc R . . N20 N -0.0450(4) 0.41146(19) 0.5435(2) 0.0735(15) Uani 1 1 d . . . S1 S 0.64827(9) 0.63817(5) 0.67991(6) 0.0458(3) Uani 1 1 d . . . S2 S 0.83497(9) 0.62992(5) 0.82238(6) 0.0443(3) Uani 1 1 d . . . S3 S -0.09830(9) -0.11471(5) 0.67892(6) 0.0449(3) Uani 1 1 d . . . S5 S -0.08711(9) 0.38234(5) 0.67787(6) 0.0482(3) Uani 1 1 d . . . Cd1 Cd 0.75455(2) 0.709492(17) 0.750414(15) 0.04241(11) Uani 1 1 d . . . Cd2 Cd 0.0000 -0.040862(19) 0.7500 0.03471(12) Uani 1 2 d S . . Cd3 Cd 0.0000 0.459968(19) 0.7500 0.03600(12) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.040(3) 0.057(3) 0.062(3) -0.005(3) 0.011(2) -0.009(2) C2 0.047(3) 0.089(5) 0.061(3) 0.001(3) 0.025(3) -0.003(3) C3 0.043(3) 0.033(2) 0.033(2) 0.0030(18) 0.0074(18) 0.004(2) C4 0.045(3) 0.040(3) 0.029(2) 0.0049(19) 0.0024(17) 0.000(2) C5 0.059(4) 0.057(3) 0.064(3) -0.004(3) 0.000(3) -0.019(3) C6 0.042(3) 0.060(3) 0.056(3) 0.005(3) 0.005(2) -0.009(3) C7 0.044(3) 0.059(3) 0.056(3) -0.004(2) 0.009(2) 0.007(2) C8 0.050(3) 0.073(4) 0.056(3) -0.002(3) 0.022(2) 0.008(3) C9 0.036(3) 0.043(3) 0.028(2) -0.0019(18) 0.0045(17) -0.007(2) C10 0.041(3) 0.039(3) 0.031(2) -0.0045(18) -0.0004(17) -0.010(2) C11 0.072(4) 0.047(3) 0.063(3) 0.006(3) -0.009(3) 0.016(3) C12 0.052(3) 0.053(3) 0.062(3) -0.010(3) 0.003(2) 0.013(3) C13 0.058(3) 0.051(3) 0.037(2) -0.005(2) 0.005(2) -0.011(2) C14 0.052(3) 0.038(3) 0.036(2) 0.0023(19) -0.002(2) 0.007(2) C15 0.055(4) 0.056(3) 0.059(3) 0.007(3) 0.001(2) -0.011(3) C16 0.066(4) 0.055(4) 0.061(3) -0.003(3) -0.012(3) -0.016(3) C17 0.055(3) 0.033(2) 0.029(2) -0.0017(18) 0.0006(19) 0.007(2) C18 0.042(3) 0.046(3) 0.026(2) 0.0009(19) 0.0020(17) 0.008(2) C19 0.045(3) 0.086(4) 0.061(3) -0.008(3) 0.024(2) -0.010(3) C20 0.043(3) 0.049(3) 0.060(3) -0.013(2) 0.000(2) -0.001(2) C21 0.055(3) 0.048(3) 0.042(3) -0.011(2) 0.004(2) -0.007(2) C22 0.048(3) 0.048(3) 0.061(3) 0.000(2) 0.010(2) -0.008(2) C23 0.050(4) 0.061(4) 0.080(4) -0.007(3) 0.000(3) -0.009(3) C24 0.057(3) 0.029(2) 0.034(2) -0.0003(18) 0.0076(19) 0.005(2) C25 0.040(3) 0.039(3) 0.033(2) 0.0022(18) 0.0066(18) 0.009(2) C26 0.051(4) 0.083(4) 0.052(3) 0.001(3) 0.023(2) -0.001(3) C27 0.041(3) 0.072(4) 0.050(3) 0.011(3) 0.006(2) -0.009(3) C28 0.055(3) 0.047(3) 0.040(3) 0.001(2) -0.006(2) -0.011(2) N1 0.037(2) 0.050(2) 0.040(2) 0.0046(17) 0.0054(16) 0.0003(18) N2 0.040(2) 0.044(2) 0.0353(19) 0.0008(16) 0.0022(15) -0.0005(17) N3 0.039(2) 0.048(2) 0.0318(18) 0.0014(17) 0.0077(14) 0.0004(18) N4 0.045(2) 0.043(2) 0.0348(19) -0.0028(16) 0.0039(16) -0.0005(18) N5 0.050(3) 0.053(3) 0.037(2) -0.0031(17) 0.0116(17) 0.003(2) N6 0.067(3) 0.047(3) 0.041(2) -0.0085(18) 0.0053(19) -0.007(2) N7 0.052(3) 0.062(3) 0.038(2) 0.0041(19) 0.0157(18) -0.005(2) N8 0.061(3) 0.048(2) 0.040(2) 0.0083(18) -0.0017(19) -0.003(2) N9 0.102(4) 0.075(3) 0.036(2) -0.006(2) 0.002(2) 0.019(3) N10 0.110(4) 0.066(3) 0.038(2) 0.001(2) 0.005(2) -0.022(3) N11 0.048(3) 0.037(2) 0.044(2) 0.0020(17) 0.0039(17) -0.0093(18) N12 0.040(2) 0.051(2) 0.0337(19) -0.0024(17) 0.0069(15) 0.0070(19) N13 0.067(3) 0.049(3) 0.045(2) -0.0106(19) -0.001(2) -0.002(2) N14 0.054(3) 0.060(3) 0.040(2) -0.0099(19) 0.0163(18) 0.001(2) N15 0.115(5) 0.069(3) 0.039(2) -0.001(2) 0.010(2) -0.025(3) N16 0.054(3) 0.037(2) 0.041(2) -0.0005(16) 0.0101(17) -0.0040(19) N17 0.039(2) 0.048(2) 0.043(2) 0.0004(17) 0.0083(16) 0.0048(18) N18 0.065(3) 0.044(2) 0.041(2) -0.0115(18) 0.0008(19) 0.002(2) N19 0.059(3) 0.057(3) 0.041(2) -0.0029(19) 0.0175(19) 0.012(2) N20 0.102(4) 0.077(3) 0.041(2) 0.006(2) -0.002(2) -0.029(3) S1 0.0560(8) 0.0435(7) 0.0370(6) 0.0036(5) -0.0013(5) -0.0059(6) S2 0.0544(8) 0.0426(7) 0.0364(6) 0.0030(5) 0.0076(5) 0.0042(6) S3 0.0516(8) 0.0469(7) 0.0351(6) 0.0028(5) -0.0019(5) -0.0117(6) S5 0.0572(8) 0.0504(8) 0.0367(6) 0.0017(5) 0.0029(5) -0.0144(6) Cd1 0.0462(2) 0.0478(2) 0.03418(17) 0.00019(14) 0.00836(14) 0.00008(15) Cd2 0.0392(3) 0.0403(3) 0.0255(2) 0.000 0.00765(17) 0.000 Cd3 0.0437(3) 0.0388(3) 0.0264(2) 0.000 0.00816(17) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.349(7) . ? C1 N1 1.359(6) . ? C1 H1 0.9300 . ? C2 N5 1.349(6) . ? C2 H2 0.9300 . ? C3 N1 1.315(5) . ? C3 N5 1.341(5) . ? C3 C4 1.444(6) . ? C4 N2 1.324(5) . ? C4 N6 1.336(5) . ? C5 C6 1.345(7) . ? C5 N6 1.375(6) . ? C5 H5 0.9300 . ? C6 N2 1.365(6) . ? C6 H6 0.9300 . ? C7 C8 1.330(7) . ? C7 N3 1.370(6) . ? C7 H7 0.9300 . ? C8 N7 1.379(6) . ? C8 H8 0.9300 . ? C9 N3 1.323(5) . ? C9 N7 1.346(5) . ? C9 C10 1.446(6) . ? C10 N4 1.331(5) . ? C10 N8 1.334(5) . ? C11 C12 1.345(7) . ? C11 N8 1.369(7) . ? C11 H11 0.9300 . ? C12 N4 1.363(6) . ? C12 H12 0.9300 . ? C13 N10 1.155(5) . ? C13 S1 1.636(5) . ? C14 N9 1.158(5) . ? C14 S2 1.640(5) . ? C15 C16 1.350(7) . ? C15 N11 1.377(6) . ? C15 H15 0.9300 . ? C16 N13 1.358(7) . ? C16 H16 0.9300 . ? C17 N11 1.321(5) . ? C17 N13 1.348(5) . ? C17 C18 1.426(6) . ? C18 N12 1.307(5) . ? C18 N14 1.346(5) . ? C19 C20 1.370(6) . ? C19 N14 1.371(6) . ? C19 H19 0.9300 . ? C20 N12 1.348(6) . ? C20 H20 0.9300 . ? C21 N15 1.153(6) . ? C21 S3 1.647(5) . ? C22 C23 1.339(7) . ? C22 N16 1.367(6) . ? C22 H22 0.9300 . ? C23 N18 1.371(6) . ? C23 H23 0.9300 . ? C24 N16 1.314(5) . ? C24 N18 1.354(5) . ? C24 C25 1.428(6) . ? C25 N17 1.322(5) . ? C25 N19 1.342(5) . ? C26 N19 1.360(7) . ? C26 C27 1.363(7) . ? C26 H26 0.9300 . ? C27 N17 1.363(6) . ? C27 H27 0.9300 . ? C28 N20 1.149(6) . ? C28 S5 1.646(5) . ? N1 Cd1 2.335(4) . ? N2 Cd1 2.394(4) . ? N3 Cd1 2.343(3) . ? N4 Cd1 2.367(4) . ? N5 H5N 0.8600 . ? N6 H6N 0.8600 . ? N7 H7N 0.8600 . ? N8 H8N 0.8600 . ? N11 Cd2 2.364(4) . ? N12 Cd2 2.342(3) . ? N13 H13N 0.8600 . ? N14 H14N 0.8600 . ? N16 Cd3 2.386(4) . ? N17 Cd3 2.333(4) . ? N18 H18N 0.8600 . ? N19 H19N 0.8600 . ? S1 Cd1 2.7257(13) . ? S2 Cd1 2.7024(13) . ? S3 Cd2 2.7114(12) . ? S5 Cd3 2.7097(13) . ? Cd2 N12 2.342(3) 2_556 ? Cd2 N11 2.364(4) 2_556 ? Cd2 S3 2.7114(12) 2_556 ? Cd3 N17 2.333(4) 2_556 ? Cd3 N16 2.386(4) 2_556 ? Cd3 S5 2.7097(13) 2_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 N1 109.4(5) . . ? C2 C1 H1 125.3 . . ? N1 C1 H1 125.3 . . ? N5 C2 C1 106.8(4) . . ? N5 C2 H2 126.6 . . ? C1 C2 H2 126.6 . . ? N1 C3 N5 111.1(4) . . ? N1 C3 C4 121.6(4) . . ? N5 C3 C4 127.3(4) . . ? N2 C4 N6 111.0(4) . . ? N2 C4 C3 121.4(4) . . ? N6 C4 C3 127.5(4) . . ? C6 C5 N6 106.6(4) . . ? C6 C5 H5 126.7 . . ? N6 C5 H5 126.7 . . ? C5 C6 N2 109.5(5) . . ? C5 C6 H6 125.3 . . ? N2 C6 H6 125.3 . . ? C8 C7 N3 109.9(5) . . ? C8 C7 H7 125.1 . . ? N3 C7 H7 125.1 . . ? C7 C8 N7 106.8(4) . . ? C7 C8 H8 126.6 . . ? N7 C8 H8 126.6 . . ? N3 C9 N7 110.7(4) . . ? N3 C9 C10 121.8(4) . . ? N7 C9 C10 127.5(4) . . ? N4 C10 N8 111.4(4) . . ? N4 C10 C9 120.9(4) . . ? N8 C10 C9 127.6(4) . . ? C12 C11 N8 106.2(5) . . ? C12 C11 H11 126.9 . . ? N8 C11 H11 126.9 . . ? C11 C12 N4 110.3(5) . . ? C11 C12 H12 124.9 . . ? N4 C12 H12 124.9 . . ? N10 C13 S1 178.3(5) . . ? N9 C14 S2 178.8(5) . . ? C16 C15 N11 109.1(5) . . ? C16 C15 H15 125.4 . . ? N11 C15 H15 125.4 . . ? C15 C16 N13 106.8(5) . . ? C15 C16 H16 126.6 . . ? N13 C16 H16 126.6 . . ? N11 C17 N13 110.7(4) . . ? N11 C17 C18 121.6(4) . . ? N13 C17 C18 127.7(4) . . ? N12 C18 N14 111.0(4) . . ? N12 C18 C17 121.2(4) . . ? N14 C18 C17 127.7(4) . . ? C20 C19 N14 105.4(4) . . ? C20 C19 H19 127.3 . . ? N14 C19 H19 127.3 . . ? N12 C20 C19 109.7(4) . . ? N12 C20 H20 125.2 . . ? C19 C20 H20 125.2 . . ? N15 C21 S3 178.7(5) . . ? C23 C22 N16 110.0(5) . . ? C23 C22 H22 125.0 . . ? N16 C22 H22 125.0 . . ? C22 C23 N18 106.4(5) . . ? C22 C23 H23 126.8 . . ? N18 C23 H23 126.8 . . ? N16 C24 N18 110.5(4) . . ? N16 C24 C25 122.1(4) . . ? N18 C24 C25 127.4(4) . . ? N17 C25 N19 110.2(4) . . ? N17 C25 C24 121.6(4) . . ? N19 C25 C24 128.2(4) . . ? N19 C26 C27 106.6(4) . . ? N19 C26 H26 126.7 . . ? C27 C26 H26 126.7 . . ? N17 C27 C26 108.6(5) . . ? N17 C27 H27 125.7 . . ? C26 C27 H27 125.7 . . ? N20 C28 S5 178.9(6) . . ? C3 N1 C1 105.7(4) . . ? C3 N1 Cd1 112.8(3) . . ? C1 N1 Cd1 141.3(3) . . ? C4 N2 C6 106.0(4) . . ? C4 N2 Cd1 110.7(3) . . ? C6 N2 Cd1 143.2(3) . . ? C9 N3 C7 105.9(4) . . ? C9 N3 Cd1 112.0(3) . . ? C7 N3 Cd1 141.8(3) . . ? C10 N4 C12 105.0(4) . . ? C10 N4 Cd1 111.4(3) . . ? C12 N4 Cd1 143.5(3) . . ? C3 N5 C2 107.0(4) . . ? C3 N5 H5N 126.5 . . ? C2 N5 H5N 126.5 . . ? C4 N6 C5 106.9(4) . . ? C4 N6 H6N 126.5 . . ? C5 N6 H6N 126.5 . . ? C9 N7 C8 106.7(4) . . ? C9 N7 H7N 126.7 . . ? C8 N7 H7N 126.7 . . ? C10 N8 C11 107.1(4) . . ? C10 N8 H8N 126.5 . . ? C11 N8 H8N 126.5 . . ? C17 N11 C15 105.9(4) . . ? C17 N11 Cd2 111.3(3) . . ? C15 N11 Cd2 142.8(3) . . ? C18 N12 C20 106.8(4) . . ? C18 N12 Cd2 112.7(3) . . ? C20 N12 Cd2 140.1(3) . . ? C17 N13 C16 107.4(4) . . ? C17 N13 H13N 126.3 . . ? C16 N13 H13N 126.3 . . ? C18 N14 C19 107.1(4) . . ? C18 N14 H14N 126.4 . . ? C19 N14 H14N 126.4 . . ? C24 N16 C22 106.2(4) . . ? C24 N16 Cd3 110.5(3) . . ? C22 N16 Cd3 143.0(3) . . ? C25 N17 C27 106.9(4) . . ? C25 N17 Cd3 112.3(3) . . ? C27 N17 Cd3 140.7(3) . . ? C24 N18 C23 107.0(4) . . ? C24 N18 H18N 126.5 . . ? C23 N18 H18N 126.5 . . ? C25 N19 C26 107.7(4) . . ? C25 N19 H19N 126.2 . . ? C26 N19 H19N 126.2 . . ? C13 S1 Cd1 97.67(17) . . ? C14 S2 Cd1 96.92(16) . . ? C21 S3 Cd2 97.04(17) . . ? C28 S5 Cd3 96.91(17) . . ? N1 Cd1 N3 164.67(14) . . ? N1 Cd1 N4 95.60(13) . . ? N3 Cd1 N4 73.80(13) . . ? N1 Cd1 N2 73.28(13) . . ? N3 Cd1 N2 95.42(13) . . ? N4 Cd1 N2 90.69(13) . . ? N1 Cd1 S2 97.23(9) . . ? N3 Cd1 S2 93.48(10) . . ? N4 Cd1 S2 167.15(9) . . ? N2 Cd1 S2 92.30(9) . . ? N1 Cd1 S1 94.86(10) . . ? N3 Cd1 S1 96.51(10) . . ? N4 Cd1 S1 91.99(9) . . ? N2 Cd1 S1 168.05(9) . . ? S2 Cd1 S1 87.65(4) . . ? N12 Cd2 N12 172.7(2) 2_556 . ? N12 Cd2 N11 72.92(13) 2_556 2_556 ? N12 Cd2 N11 101.66(13) . 2_556 ? N12 Cd2 N11 101.66(13) 2_556 . ? N12 Cd2 N11 72.92(13) . . ? N11 Cd2 N11 88.16(18) 2_556 . ? N12 Cd2 S3 96.03(9) 2_556 . ? N12 Cd2 S3 89.12(10) . . ? N11 Cd2 S3 93.44(10) 2_556 . ? N11 Cd2 S3 161.89(10) . . ? N12 Cd2 S3 89.12(10) 2_556 2_556 ? N12 Cd2 S3 96.03(9) . 2_556 ? N11 Cd2 S3 161.89(10) 2_556 2_556 ? N11 Cd2 S3 93.44(10) . 2_556 ? S3 Cd2 S3 90.62(6) . 2_556 ? N17 Cd3 N17 156.19(19) 2_556 . ? N17 Cd3 N16 73.35(13) 2_556 2_556 ? N17 Cd3 N16 90.40(13) . 2_556 ? N17 Cd3 N16 90.40(13) 2_556 . ? N17 Cd3 N16 73.35(13) . . ? N16 Cd3 N16 94.66(18) 2_556 . ? N17 Cd3 S5 96.87(9) 2_556 . ? N17 Cd3 S5 100.70(10) . . ? N16 Cd3 S5 90.71(10) 2_556 . ? N16 Cd3 S5 171.97(9) . . ? N17 Cd3 S5 100.70(10) 2_556 2_556 ? N17 Cd3 S5 96.87(9) . 2_556 ? N16 Cd3 S5 171.97(9) 2_556 2_556 ? N16 Cd3 S5 90.71(10) . 2_556 ? S5 Cd3 S5 84.60(6) . 2_556 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.939 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.069 #END data_Complex2 _database_code_depnum_ccdc_archive 'CCDC 623786' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H12 Cd N10 Se2' _chemical_formula_sum 'C14 H12 Cd N10 Se2' _chemical_formula_weight 590.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8080 1.2020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0930 2.2260 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_Hall 'P 32 2c (0 0 -1)' _symmetry_space_group_name_H-M 'P 32 1 2' _symmetry_Int_Tables_number 153 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' '-y, -x, -z+1/3' 'x, x-y, -z' '-x+y, y, -z+2/3' _cell_length_a 7.6958(2) _cell_length_b 7.6958(2) _cell_length_c 28.592(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1466.50(12) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Brown _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.006 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 846 _exptl_absorpt_coefficient_mu 4.861 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11350 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.1173 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2232 _reflns_number_gt 2183 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for windows (Farugia 1997)' _computing_publication_material 'PLATON-2003 (Spek 2003)' _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^)+(0.1029P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(3) _refine_ls_number_reflns 2232 _refine_ls_number_parameters 123 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0657 _refine_ls_R_factor_gt 0.0648 _refine_ls_wR_factor_ref 0.1734 _refine_ls_wR_factor_gt 0.1719 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.21191(13) 0.10595(6) 1.0000 0.0433(2) Uani 1 2 d S . . Se1 Se 0.51252(14) 0.07253(16) 0.95256(3) 0.0510(3) Uani 1 1 d . . . N1 N -0.0436(11) -0.1300(12) 0.9487(2) 0.0491(14) Uani 1 1 d . . . N4 N 0.1576(13) 0.2960(12) 0.9436(2) 0.0515(17) Uani 1 1 d . . . C1 C -0.1717(16) -0.3288(17) 0.9404(5) 0.069(3) Uani 1 1 d . . . H1 H -0.1842 -0.4312 0.9599 0.082 Uiso 1 1 calc R . . C2 C -0.2751(19) -0.359(2) 0.9019(4) 0.081(3) Uani 1 1 d . . . H2 H -0.3646 -0.4816 0.8884 0.097 Uiso 1 1 calc R . . C5 C 0.132(3) 0.487(2) 0.8907(5) 0.085(4) Uani 1 1 d . . . H5 H 0.1578 0.5987 0.8732 0.102 Uiso 1 1 calc R . . C6 C 0.220(3) 0.489(2) 0.9314(5) 0.086(4) Uani 1 1 d . . . H6 H 0.3086 0.6030 0.9482 0.103 Uiso 1 1 calc R . . C7 C 0.3987(19) 0.050(2) 0.8960(3) 0.071(3) Uani 1 1 d . . . N2 N -0.2236(14) -0.1715(18) 0.8857(3) 0.068(2) Uani 1 1 d . . . H2N H -0.2716 -0.1451 0.8613 0.082 Uiso 1 1 calc R . . N3 N 0.0019(16) 0.2955(17) 0.8793(3) 0.068(2) Uani 1 1 d . . . H3N H -0.0772 0.2552 0.8556 0.081 Uiso 1 1 calc R . . N5 N 0.327(2) 0.040(3) 0.8606(3) 0.114(6) Uani 1 1 d . . . C3 C -0.0839(13) -0.0357(15) 0.9150(2) 0.0504(18) Uani 1 1 d . . . C4 C 0.0179(13) 0.1764(15) 0.9127(3) 0.0493(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0452(4) 0.0441(4) 0.0409(4) 0.0011(2) 0.000 0.0226(2) Se1 0.0467(5) 0.0611(6) 0.0508(4) -0.0043(4) 0.0004(3) 0.0312(4) N1 0.042(3) 0.049(4) 0.051(3) -0.001(3) 0.004(2) 0.018(3) N4 0.067(5) 0.051(4) 0.052(3) 0.004(3) 0.000(3) 0.041(4) C1 0.043(4) 0.047(5) 0.097(7) -0.009(5) 0.013(5) 0.008(4) C2 0.055(6) 0.064(7) 0.092(7) -0.029(6) -0.003(5) 0.006(5) C5 0.103(10) 0.085(9) 0.091(7) 0.038(7) 0.019(7) 0.064(9) C6 0.119(12) 0.082(9) 0.094(8) 0.017(6) 0.022(7) 0.079(9) C7 0.065(6) 0.108(10) 0.055(5) -0.002(5) 0.008(4) 0.055(7) N2 0.055(5) 0.088(7) 0.055(4) -0.014(4) -0.012(3) 0.031(5) N3 0.080(6) 0.083(7) 0.056(4) 0.018(4) 0.000(4) 0.053(5) N5 0.118(11) 0.232(19) 0.041(4) 0.007(6) -0.001(4) 0.124(13) C3 0.038(4) 0.077(6) 0.036(3) -0.004(3) 0.001(3) 0.029(4) C4 0.051(4) 0.066(5) 0.047(3) 0.006(3) 0.006(3) 0.042(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N4 2.351(7) 5_557 ? Cd1 N4 2.351(7) . ? Cd1 N1 2.397(7) . ? Cd1 N1 2.397(7) 5_557 ? Cd1 Se1 2.8024(11) 5_557 ? Cd1 Se1 2.8024(10) . ? Se1 C7 1.805(10) . ? N1 C3 1.333(11) . ? N1 C1 1.364(13) . ? N4 C4 1.339(12) . ? N4 C6 1.359(15) . ? C1 C2 1.309(19) . ? C1 H1 0.9300 . ? C2 N2 1.37(2) . ? C2 H2 0.9300 . ? C5 N3 1.34(2) . ? C5 C6 1.34(2) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 N5 1.137(13) . ? N2 C3 1.350(12) . ? N2 H2N 0.8600 . ? N3 C4 1.372(11) . ? N3 H3N 0.8600 . ? C3 C4 1.415(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Cd1 N4 162.3(4) 5_557 . ? N4 Cd1 N1 93.6(3) 5_557 . ? N4 Cd1 N1 73.6(3) . . ? N4 Cd1 N1 73.6(3) 5_557 5_557 ? N4 Cd1 N1 93.6(3) . 5_557 ? N1 Cd1 N1 89.5(4) . 5_557 ? N4 Cd1 Se1 97.87(19) 5_557 5_557 ? N4 Cd1 Se1 94.8(2) . 5_557 ? N1 Cd1 Se1 168.4(2) . 5_557 ? N1 Cd1 Se1 92.1(2) 5_557 5_557 ? N4 Cd1 Se1 94.8(2) 5_557 . ? N4 Cd1 Se1 97.87(19) . . ? N1 Cd1 Se1 92.08(19) . . ? N1 Cd1 Se1 168.4(2) 5_557 . ? Se1 Cd1 Se1 88.73(5) 5_557 . ? C7 Se1 Cd1 93.3(3) . . ? C3 N1 C1 104.5(9) . . ? C3 N1 Cd1 110.9(6) . . ? C1 N1 Cd1 144.6(8) . . ? C4 N4 C6 107.9(9) . . ? C4 N4 Cd1 110.8(5) . . ? C6 N4 Cd1 141.3(9) . . ? C2 C1 N1 112.3(12) . . ? C2 C1 H1 123.9 . . ? N1 C1 H1 123.9 . . ? C1 C2 N2 105.5(9) . . ? C1 C2 H2 127.3 . . ? N2 C2 H2 127.3 . . ? N3 C5 C6 108.8(11) . . ? N3 C5 H5 125.6 . . ? C6 C5 H5 125.6 . . ? C5 C6 N4 107.8(14) . . ? C5 C6 H6 126.1 . . ? N4 C6 H6 126.1 . . ? N5 C7 Se1 178.6(15) . . ? C3 N2 C2 107.8(9) . . ? C3 N2 H2N 126.1 . . ? C2 N2 H2N 126.1 . . ? C5 N3 C4 107.2(9) . . ? C5 N3 H3N 126.4 . . ? C4 N3 H3N 126.4 . . ? N1 C3 N2 109.8(9) . . ? N1 C3 C4 121.0(8) . . ? N2 C3 C4 129.2(9) . . ? N4 C4 N3 108.0(8) . . ? N4 C4 C3 123.7(7) . . ? N3 C4 C3 128.3(9) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.227 _refine_diff_density_min -1.472 _refine_diff_density_rms 0.245 #END data_Complex3 _database_code_depnum_ccdc_archive 'CCDC 623787' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H12 Cd N14' _chemical_formula_sum 'C16 H12 Cd N14' _chemical_formula_weight 512.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_Hall '-P 2n 2ab' _symmetry_space_group_name_H-M 'P b c n' _symmetry_Int_Tables_number 60 loop_ _symmetry_equiv_pos_as_xyz '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' 'x, -y, z-1/2' _cell_length_a 13.3982(4) _cell_length_b 7.7207(2) _cell_length_c 19.1997(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1986.08(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Brown _exptl_crystal_size_max .19 _exptl_crystal_size_mid .16 _exptl_crystal_size_min .11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.715 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 1.137 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min .7613 _exptl_absorpt_correction_T_max .8863 _exptl_absorpt_process_details empirical _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14615 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0182 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2263 _reflns_number_gt 2195 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for windows (Farugia 1997)' _computing_publication_material 'PLATON-2003 (Spek 2003)' _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^)+(0.0703P)^2^+4.1044P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2263 _refine_ls_number_parameters 141 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1470 _refine_ls_wR_factor_gt 0.1460 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.148 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.5000 0.67126(5) 0.2500 0.04184(19) Uani 1 2 d S . . N1 N 0.4890(2) 0.4799(5) 0.1524(2) 0.0478(8) Uani 1 1 d . . . N2 N 0.3899(3) 0.3782(5) 0.0710(2) 0.0555(9) Uani 1 1 d . . . H2N H 0.3363 0.3538 0.0484 0.067 Uiso 1 1 d R . . N3 N 0.3324(3) 0.6303(5) 0.2280(2) 0.0451(7) Uani 1 1 d . . . N4 N 0.2158(3) 0.5290(5) 0.1598(2) 0.0512(9) Uani 1 1 d . . . H4N H 0.1875 0.4770 0.1254 0.061 Uiso 1 1 d R . . N5 N 0.4672(4) 0.8845(6) 0.3341(2) 0.0618(10) Uani 1 1 d . . . N6 N 0.3310(4) 0.9358(9) 0.4144(3) 0.0906(11) Uani 1 1 d U . . N7 N 0.3160(4) 1.1069(8) 0.5178(3) 0.0860(16) Uani 1 1 d . . . C1 C 0.5449(4) 0.3946(7) 0.1041(3) 0.0579(11) Uani 1 1 d . . . H1 H 0.6138 0.3818 0.1059 0.070 Uiso 1 1 calc R . . C2 C 0.4857(4) 0.3314(7) 0.0531(3) 0.0622(14) Uani 1 1 d . . . H2 H 0.5055 0.2693 0.0139 0.075 Uiso 1 1 calc R . . C3 C 0.3957(3) 0.4694(5) 0.1307(2) 0.0447(9) Uani 1 1 d . . . C4 C 0.3148(3) 0.5431(5) 0.1706(2) 0.0439(9) Uani 1 1 d . . . C5 C 0.1690(3) 0.6111(7) 0.2126(3) 0.0566(11) Uani 1 1 d . . . H5 H 0.1005 0.6223 0.2187 0.068 Uiso 1 1 calc R . . C6 C 0.2417(4) 0.6740(6) 0.2550(2) 0.0509(11) Uani 1 1 d . . . H6 H 0.2313 0.7367 0.2957 0.061 Uiso 1 1 calc R . . C7 C 0.4086(5) 0.9118(11) 0.3746(3) 0.0887(12) Uani 1 1 d U . . C8 C 0.3299(5) 1.0285(11) 0.4700(4) 0.0881(12) Uani 1 1 d U . . 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 0.0305(3) 0.0484(3) 0.0466(3) 0.000 -0.00393(14) 0.000 N1 0.0405(18) 0.052(2) 0.051(2) -0.0032(17) -0.0067(14) 0.0030(14) N2 0.058(2) 0.057(2) 0.052(2) -0.0014(18) -0.0150(17) -0.0004(18) N3 0.0344(17) 0.0492(18) 0.0516(18) 0.0031(16) -0.0019(15) -0.0029(15) N4 0.0392(17) 0.054(2) 0.061(2) 0.0116(17) -0.0139(16) -0.0072(15) N5 0.064(2) 0.064(2) 0.057(2) -0.010(2) 0.008(2) 0.002(2) N6 0.0683(19) 0.127(3) 0.077(2) -0.025(2) 0.0244(17) -0.023(2) N7 0.078(3) 0.105(4) 0.075(3) -0.004(3) 0.033(3) -0.009(3) C1 0.049(3) 0.062(3) 0.063(3) 0.000(2) 0.000(2) 0.010(2) C2 0.071(3) 0.063(3) 0.053(3) -0.006(2) -0.001(2) 0.013(2) C3 0.045(2) 0.045(2) 0.045(2) 0.0025(16) -0.0081(16) 0.0006(16) C4 0.0367(18) 0.046(2) 0.049(2) 0.0113(17) -0.0089(16) -0.0039(16) C5 0.033(2) 0.062(3) 0.075(3) 0.017(2) 0.001(2) -0.0016(19) C6 0.035(2) 0.054(3) 0.064(3) 0.0042(19) 0.0072(18) -0.0007(17) C7 0.067(2) 0.125(3) 0.075(2) -0.025(2) 0.0235(18) -0.023(2) C8 0.066(2) 0.125(3) 0.073(2) -0.024(2) 0.0260(18) -0.022(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N3 2.306(3) . ? Cd1 N3 2.306(3) 4_655 ? Cd1 N5 2.348(4) . ? Cd1 N5 2.348(4) 4_655 ? Cd1 N1 2.390(4) . ? Cd1 N1 2.390(4) 4_655 ? N1 C3 1.320(5) . ? N1 C1 1.363(6) . ? N2 C3 1.346(6) . ? N2 C2 1.377(7) . ? N2 H2N 0.8600 . ? N3 C4 1.312(6) . ? N3 C6 1.364(6) . ? N4 C4 1.347(5) . ? N4 C5 1.350(7) . ? N4 H4N 0.8609 . ? N5 C7 1.124(7) . ? N6 C8 1.284(8) . ? N6 C7 1.305(7) . ? N7 C8 1.116(8) . ? C1 C2 1.351(8) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 C4 1.444(6) . ? C5 C6 1.359(7) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cd1 N3 164.22(19) . 4_655 ? N3 Cd1 N5 92.32(16) . . ? N3 Cd1 N5 98.75(15) 4_655 . ? N3 Cd1 N5 98.75(15) . 4_655 ? N3 Cd1 N5 92.32(16) 4_655 4_655 ? N5 Cd1 N5 90.9(2) . 4_655 ? N3 Cd1 N1 73.22(13) . . ? N3 Cd1 N1 96.84(12) 4_655 . ? N5 Cd1 N1 163.95(15) . . ? N5 Cd1 N1 84.60(16) 4_655 . ? N3 Cd1 N1 96.84(12) . 4_655 ? N3 Cd1 N1 73.22(13) 4_655 4_655 ? N5 Cd1 N1 84.60(16) . 4_655 ? N5 Cd1 N1 163.95(15) 4_655 4_655 ? N1 Cd1 N1 103.6(2) . 4_655 ? C3 N1 C1 105.9(4) . . ? C3 N1 Cd1 110.2(3) . . ? C1 N1 Cd1 143.0(3) . . ? C3 N2 C2 107.2(4) . . ? C3 N2 H2N 126.3 . . ? C2 N2 H2N 126.5 . . ? C4 N3 C6 106.6(4) . . ? C4 N3 Cd1 113.5(3) . . ? C6 N3 Cd1 139.8(3) . . ? C4 N4 C5 107.7(4) . . ? C4 N4 H4N 126.1 . . ? C5 N4 H4N 126.2 . . ? C7 N5 Cd1 137.5(5) . . ? C8 N6 C7 125.1(6) . . ? C2 C1 N1 110.2(4) . . ? C2 C1 H1 124.9 . . ? N1 C1 H1 124.9 . . ? C1 C2 N2 105.7(5) . . ? C1 C2 H2 127.2 . . ? N2 C2 H2 127.2 . . ? N1 C3 N2 110.9(4) . . ? N1 C3 C4 121.2(4) . . ? N2 C3 C4 127.9(4) . . ? N3 C4 N4 110.3(4) . . ? N3 C4 C3 120.9(3) . . ? N4 C4 C3 128.7(4) . . ? N4 C5 C6 106.6(4) . . ? N4 C5 H5 126.7 . . ? C6 C5 H5 126.7 . . ? C5 C6 N3 108.8(4) . . ? C5 C6 H6 125.6 . . ? N3 C6 H6 125.6 . . ? N5 C7 N6 171.4(7) . . ? N7 C8 N6 171.0(7) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.139 _refine_diff_density_min -1.614 _refine_diff_density_rms 0.099 #END