# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Christian Nather' _publ_contact_author_email cnaether@ac.uni-kiel.de loop_ _publ_author_name C.Nather S.Woehlert J.Boeckmann I.Jess data_ta36 _database_code_depnum_ccdc_archive 'CCDC 872124' #TrackingRef '- [Cd(NCS)2(pyridine)2]n_cis_trans.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H10 Cd N4 S2' _chemical_formula_sum 'C12 H10 Cd N4 S2' _chemical_formula_weight 386.76 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_H-M C2/m _symmetry_space_group_name_Hall '-C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 7.9395(7) _cell_length_b 15.2318(8) _cell_length_c 17.7558(13) _cell_angle_alpha 90.00 _cell_angle_beta 93.632(6) _cell_angle_gamma 90.00 _cell_volume 2142.9(3) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7448 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 27.00 _exptl_crystal_description block _exptl_crystal_colour white _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.798 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1140 _exptl_absorpt_coefficient_mu 1.811 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.755 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details 'X-Shape and X-Red32 (Stoe, 2008)' _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 'STOE IPDS-2' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 7448 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0236 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 27.00 _reflns_number_total 2409 _reflns_number_gt 1888 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area (Stoe, 2008)' _computing_cell_refinement 'X-Area (Stoe, 2008)' _computing_data_reduction 'X-Area (Stoe, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; XP in SHELXTL (Sheldrick, 2008) and Diamond (Brandenburg, 2011) ; _computing_publication_material 'XCIF in SHELXTL (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+5.4515P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2409 _refine_ls_number_parameters 147 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0657 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.0959 _refine_ls_wR_factor_gt 0.0892 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.128 _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 0.42334(6) 0.5000 0.83360(3) 0.05450(17) Uani 1 2 d S . . Cd2 Cd 0.5000 0.5000 0.5000 0.0551(2) Uani 1 4 d S . . N1 N 0.6125(7) 0.5000 0.7395(3) 0.0663(16) Uani 1 2 d S . . C1 C 0.6744(8) 0.5000 0.6833(4) 0.0515(15) Uani 1 2 d S . . S1 S 0.7673(2) 0.5000 0.60324(10) 0.0707(6) Uani 1 2 d S . . N2 N 0.3087(7) 0.5000 0.5930(3) 0.0659(17) Uani 1 2 d S . . C2 C 0.2457(8) 0.5000 0.6496(4) 0.0505(15) Uani 1 2 d S . . S2 S 0.1539(2) 0.5000 0.72947(10) 0.0724(6) Uani 1 2 d S . . N3 N 0.6333(7) 0.5000 0.9286(3) 0.0644(16) Uani 1 2 d S . . C3 C 0.7120(8) 0.5000 0.9853(4) 0.0496(14) Uani 1 2 d S . . S3 S 0.8254(2) 0.5000 1.06548(10) 0.0733(6) Uani 1 2 d S . . N10 N 0.4142(5) 0.6549(3) 0.8329(3) 0.0660(11) Uani 1 1 d . . . C10 C 0.4006(8) 0.7004(5) 0.8961(4) 0.0823(17) Uani 1 1 d . . . H10 H 0.4024 0.6700 0.9416 0.099 Uiso 1 1 calc R . . C11 C 0.3839(9) 0.7899(5) 0.8975(5) 0.0920(19) Uani 1 1 d . . . H11 H 0.3743 0.8192 0.9430 0.110 Uiso 1 1 calc R . . C12 C 0.3817(8) 0.8349(5) 0.8322(5) 0.0885(19) Uani 1 1 d . . . H12 H 0.3711 0.8957 0.8320 0.106 Uiso 1 1 calc R . . C13 C 0.3954(8) 0.7900(5) 0.7662(5) 0.092(2) Uani 1 1 d . . . H13 H 0.3938 0.8197 0.7204 0.110 Uiso 1 1 calc R . . C14 C 0.4113(8) 0.7002(5) 0.7686(4) 0.0804(16) Uani 1 1 d . . . H14 H 0.4204 0.6699 0.7236 0.096 Uiso 1 1 calc R . . N20 N 0.5000 0.3432(4) 0.5000 0.0662(16) Uani 1 2 d S . . C20 C 0.4412(8) 0.2975(4) 0.4403(4) 0.0772(16) Uani 1 1 d . . . H20 H 0.3991 0.3279 0.3978 0.093 Uiso 1 1 calc R . . C21 C 0.4396(9) 0.2074(5) 0.4384(5) 0.096(2) Uani 1 1 d . . . H21 H 0.3976 0.1781 0.3952 0.115 Uiso 1 1 calc R . . C22 C 0.5000 0.1613(7) 0.5000 0.096(3) Uani 1 2 d S . . H22 H 0.5000 0.1002 0.5000 0.115 Uiso 1 2 calc SR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0569(3) 0.0645(3) 0.0421(3) 0.000 0.00370(19) 0.000 Cd2 0.0563(4) 0.0667(5) 0.0426(4) 0.000 0.0045(3) 0.000 N1 0.059(3) 0.096(5) 0.045(3) 0.000 0.006(3) 0.000 C1 0.050(3) 0.054(4) 0.049(4) 0.000 -0.004(3) 0.000 S1 0.0506(9) 0.1150(18) 0.0468(9) 0.000 0.0046(7) 0.000 N2 0.057(3) 0.095(5) 0.047(3) 0.000 0.011(3) 0.000 C2 0.047(3) 0.052(4) 0.052(4) 0.000 -0.006(3) 0.000 S2 0.0514(9) 0.1205(18) 0.0455(9) 0.000 0.0049(7) 0.000 N3 0.053(3) 0.092(5) 0.048(3) 0.000 -0.001(3) 0.000 C3 0.050(3) 0.051(4) 0.049(3) 0.000 0.012(3) 0.000 S3 0.0506(9) 0.1229(19) 0.0465(10) 0.000 0.0037(7) 0.000 N10 0.064(2) 0.068(3) 0.066(3) 0.002(2) 0.003(2) 0.000(2) C10 0.100(4) 0.082(4) 0.064(3) -0.010(3) 0.002(3) 0.003(3) C11 0.105(5) 0.078(4) 0.093(5) -0.019(4) 0.006(4) 0.001(4) C12 0.081(4) 0.067(4) 0.117(6) -0.001(4) 0.004(4) 0.003(3) C13 0.099(5) 0.080(5) 0.097(5) 0.024(4) 0.010(4) 0.000(4) C14 0.094(4) 0.078(4) 0.069(4) 0.007(3) 0.008(3) 0.000(3) N20 0.067(4) 0.065(4) 0.067(4) 0.000 0.012(3) 0.000 C20 0.084(4) 0.075(4) 0.073(4) -0.015(3) 0.004(3) -0.003(3) C21 0.103(5) 0.079(5) 0.108(6) -0.026(4) 0.028(4) -0.011(4) C22 0.090(6) 0.065(6) 0.139(10) 0.000 0.056(7) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N3 2.295(6) . ? Cd1 N1 2.316(6) . ? Cd1 N10 2.360(5) 6_565 ? Cd1 N10 2.360(5) . ? Cd1 S2 2.7374(19) . ? Cd1 S3 2.7493(19) 5_667 ? Cd2 N2 2.314(6) . ? Cd2 N2 2.314(6) 5_666 ? Cd2 N20 2.389(7) . ? Cd2 N20 2.389(7) 5_666 ? Cd2 S1 2.7151(18) . ? Cd2 S1 2.7151(18) 5_666 ? N1 C1 1.140(8) . ? C1 S1 1.642(7) . ? N2 C2 1.150(8) . ? C2 S2 1.635(7) . ? N3 C3 1.151(8) . ? C3 S3 1.636(7) . ? S3 Cd1 2.7493(19) 5_667 ? N10 C10 1.330(7) . ? N10 C14 1.333(7) . ? C10 C11 1.370(11) . ? C11 C12 1.346(10) . ? C12 C13 1.368(10) . ? C13 C14 1.373(11) . ? N20 C20 1.328(7) 2_656 ? N20 C20 1.328(7) . ? C20 C21 1.372(10) . ? C21 C22 1.362(9) . ? C22 C21 1.362(9) 2_656 ? 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 N1 93.2(2) . . ? N3 Cd1 N10 91.41(11) . 6_565 ? N1 Cd1 N10 91.00(11) . 6_565 ? N3 Cd1 N10 91.41(11) . . ? N1 Cd1 N10 91.00(12) . . ? N10 Cd1 N10 176.5(2) 6_565 . ? N3 Cd1 S2 175.22(16) . . ? N1 Cd1 S2 91.57(15) . . ? N10 Cd1 S2 88.51(11) 6_565 . ? N10 Cd1 S2 88.51(11) . . ? N3 Cd1 S3 92.26(15) . 5_667 ? N1 Cd1 S3 174.53(15) . 5_667 ? N10 Cd1 S3 88.87(11) 6_565 5_667 ? N10 Cd1 S3 88.87(11) . 5_667 ? S2 Cd1 S3 82.96(5) . 5_667 ? N2 Cd2 N2 180.000(1) . 5_666 ? N2 Cd2 N20 90.000(1) . . ? N2 Cd2 N20 90.000(1) 5_666 . ? N2 Cd2 N20 90.000(1) . 5_666 ? N2 Cd2 N20 90.000(1) 5_666 5_666 ? N20 Cd2 N20 180.000(1) . 5_666 ? N2 Cd2 S1 92.20(15) . . ? N2 Cd2 S1 87.80(15) 5_666 . ? N20 Cd2 S1 90.000(1) . . ? N20 Cd2 S1 90.000(1) 5_666 . ? N2 Cd2 S1 87.80(15) . 5_666 ? N2 Cd2 S1 92.20(15) 5_666 5_666 ? N20 Cd2 S1 90.000(1) . 5_666 ? N20 Cd2 S1 90.0 5_666 5_666 ? S1 Cd2 S1 180.0 . 5_666 ? C1 N1 Cd1 165.2(5) . . ? N1 C1 S1 178.9(6) . . ? C1 S1 Cd2 102.1(2) . . ? C2 N2 Cd2 164.8(5) . . ? N2 C2 S2 179.3(6) . . ? C2 S2 Cd1 102.3(2) . . ? C3 N3 Cd1 166.3(5) . . ? N3 C3 S3 179.5(6) . . ? C3 S3 Cd1 100.9(2) . 5_667 ? C10 N10 C14 117.0(5) . . ? C10 N10 Cd1 121.4(4) . . ? C14 N10 Cd1 121.4(4) . . ? N10 C10 C11 123.2(6) . . ? C12 C11 C10 119.2(7) . . ? C11 C12 C13 119.1(7) . . ? C12 C13 C14 118.9(7) . . ? N10 C14 C13 122.7(6) . . ? C20 N20 C20 116.8(8) 2_656 . ? C20 N20 Cd2 121.6(4) 2_656 . ? C20 N20 Cd2 121.6(4) . . ? N20 C20 C21 123.1(7) . . ? C22 C21 C20 119.6(8) . . ? C21 C22 C21 117.9(10) 2_656 . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.464 _refine_diff_density_min -0.843 _refine_diff_density_rms 0.073 # Attachment '- [Cd(NCS)2(pyridine)2]n_trans.cif' data_TA28a_abbr1 _database_code_depnum_ccdc_archive 'CCDC 872125' #TrackingRef '- [Cd(NCS)2(pyridine)2]n_trans.cif' _chemical_name_systematic ; catena-Poly[bis(thiocyanato-kN)bis(pyridine-kN)cadmium(II)] ; _chemical_name_common catena-Poly(bis(thiocyanato-kN)bis(pyridine-kN)cadmium(ii)) _chemical_formula_moiety 'C12 H10 Cd N4 S2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'C12 H10 Cd N4 S2' _chemical_formula_weight 386.7702 _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products loop_ _atom_type_symbol _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source cd 19.22140 0.59460 17.64440 6.90890 4.46100 24.70080 1.60290 87.48250 5.06940 -0.07900 4.65300 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 s 6.90530 1.46790 5.20340 22.21510 1.43790 0.25360 1.58630 56.17200 0.86690 0.31900 0.55700 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 c 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560 0.01700 0.00900 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 n 12.21260 0.00570 3.13220 9.89330 2.01250 28.99750 1.16630 0.58260 -11.52900 0.02900 0.01800 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 #============================================================================= # 6. POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz #<--must include 'x,y,z' x,y,z -x,-y,-z _cell_length_a 8.7915(9) _cell_length_b 8.7921(7) _cell_length_c 16.1275(18) _cell_angle_alpha 92.773(6) _cell_angle_beta 95.879(6) _cell_angle_gamma 114.341(7) _cell_volume 1124.14(19) _cell_formula_units_Z 3 _cell_measurement_temperature 293 _cell_special_details ; ? ; # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting # This field should be # used to give details of the # container. ; ? ; _pd_spec_mount_mode reflection _pd_spec_shape flat_sheet _pd_char_particle_morphology ? _pd_char_colour white # The following three fields describe the preparation of the specimen. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? # The next four fields are normally only needed for transmission experiments. _exptl_absorpt_coefficient_mu ? _exptl_absorpt_correction_type NONE _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_crystal_density_diffrn 1.669 #============================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; # The following item is used to identify the equipment used to record # the powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; ? ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; ? ; _diffrn_ambient_temperature 293 _diffrn_source ? _diffrn_radiation_type 'Cu K\a' _diffrn_source_target Cu _diffrn_radiation_monochromator ? _diffrn_radiation_wavelength 1.540560 _diffrn_measurement_device_type 'XPert Panalytical' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? # Not in version 2.0.1 _diffrn_detector ? _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method ? # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 3461 _pd_meas_2theta_range_min 5.01000 _pd_meas_2theta_range_max 49.99000 _pd_meas_2theta_range_inc 0.013000 #============================================================================= # 8. REFINEMENT DATA _refine_special_details ; ? ; # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text. _pd_proc_ls_profile_function ? _pd_proc_ls_background_function ? _pd_proc_ls_pref_orient_corr ; ? ; # The following profile R-factors are NOT CORRECTED for background # The sum is extended to all non-excluded points. # These are the current CIF standard _pd_proc_ls_prof_R_factor 5.4172 _pd_proc_ls_prof_wR_factor 7.0397 _pd_proc_ls_prof_wR_expected 3.0657 # The following profile R-factors are CORRECTED for background # The sum is extended to all non-excluded points. # These items are not in the current CIF standard, but are defined above _pd_proc_ls_prof_cR_factor 14.8033 _pd_proc_ls_prof_cwR_factor 14.8857 _pd_proc_ls_prof_cwR_expected 6.4825 # The following items are not in the CIF standard, but are defined above _pd_proc_ls_prof_chi2 5.2730 _pd_proc_ls_prof_echi2 5.2730 # Items related to LS refinement _refine_ls_R_I_factor 2.7794 _refine_ls_number_reflns 661 _refine_ls_number_parameters 41 _refine_ls_number_restraints 9 _refine_ls_hydrogen_treatment undef # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 5.0460 _pd_proc_2theta_range_max 50.0260 _pd_proc_2theta_range_inc 0.013000 _pd_proc_wavelength 1.540560 _pd_block_diffractogram_id ? # The id used for the block containing # the powder pattern profile (section 11) # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? # The following items are used to identify the programs used. _computing_data_collection ? _computing_structure_solution ? _computing_structure_refinement FULLPROF _computing_molecular_graphics ? _computing_publication_material ? #============================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type # Not in version 2.0.1 _atom_site_type_symbol Cd1 0.50000 0.50000 0.50000 0.018(10) 1.00000 Uiso Cd Cd2 0.8261(17) 0.8007(16) 0.8402(11) 0.027(7) 1.00000 Uiso Cd S1 0.565(5) 0.835(4) 0.551(2) 0.027(8) 1.00000 Uiso S C1 0.650(5) 0.851(4) 0.651(2) 0.045(9) 1.00000 Uiso C N1 0.709(5) 0.860(4) 0.721(2) 0.045(9) 1.00000 Uiso N S2 0.781(5) 0.489(3) 0.769(2) 0.027(8) 1.00000 Uiso S C2 0.673(5) 0.466(3) 0.675(2) 0.045(9) 1.00000 Uiso C N2 0.596(5) 0.448(3) 0.608(2) 0.045(9) 1.00000 Uiso N S3 0.884(4) 1.132(3) 0.8405(19) 0.027(8) 1.00000 Uiso S C3 0.981(4) 1.160(3) 0.9383(19) 0.045(9) 1.00000 Uiso C N3 1.048(4) 1.181(3) 1.0081(19) 0.045(9) 1.00000 Uiso N N11 0.563(5) 0.671(6) 0.894(3) 0.045(9) 1.00000 Uiso N C11 0.557(5) 0.730(6) 0.972(3) 0.045(9) 1.00000 Uiso C C12 0.414(5) 0.670(6) 1.011(3) 0.045(9) 1.00000 Uiso C C13 0.270(5) 0.542(6) 0.969(3) 0.045(9) 1.00000 Uiso C C14 0.275(5) 0.478(6) 0.890(3) 0.045(9) 1.00000 Uiso C C15 0.424(5) 0.545(6) 0.855(3) 0.045(9) 1.00000 Uiso C N21 1.106(5) 0.962(5) 0.799(3) 0.045(9) 1.00000 Uiso N C21 1.137(5) 1.072(5) 0.742(3) 0.045(9) 1.00000 Uiso C C22 1.288(5) 1.138(5) 0.709(3) 0.045(9) 1.00000 Uiso C C23 1.412(5) 1.088(5) 0.736(3) 0.045(9) 1.00000 Uiso C C24 1.383(5) 0.976(5) 0.794(3) 0.045(9) 1.00000 Uiso C C25 1.229(5) 0.916(5) 0.824(3) 0.045(9) 1.00000 Uiso C N31 0.786(5) 0.640(6) 0.454(3) 0.045(9) 1.00000 Uiso N C31 0.922(5) 0.754(6) 0.503(3) 0.045(9) 1.00000 Uiso C C32 1.083(5) 0.815(6) 0.482(3) 0.045(9) 1.00000 Uiso C C33 1.107(5) 0.755(6) 0.406(3) 0.045(9) 1.00000 Uiso C C34 0.970(5) 0.635(6) 0.355(3) 0.045(9) 1.00000 Uiso C C35 0.812(5) 0.579(6) 0.381(3) 0.045(9) 1.00000 Uiso C # Note: if the displacement parameters were refined anisotropically # the U matrices should be given as for single-crystal studies. #============================================================================= # 10. DISTANCES AND ANGLES / MOLECULAR GEOMETRY _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N2 2.01(3) . ? Cd1 N2 2.01(3) 2_666 ? Cd1 N31 2.51(5) 2_666 ? Cd1 N31 2.51(5) . ? Cd1 S1 2.82(3) . ? Cd1 S1 2.82(3) 2_666 ? Cd2 N1 2.27(4) . ? Cd2 N11 2.40(5) . ? Cd2 N21 2.46(5) . ? Cd2 N3 2.55(4) 2_777 ? Cd2 S3 2.74(3) . ? Cd2 S2 2.77(3) . ? S1 C1 1.68(5) . ? C1 N1 1.18(5) . ? S2 C2 1.66(5) . ? C2 N2 1.18(5) . ? S3 C3 1.67(4) . ? C3 N3 1.18(4) . ? N3 Cd2 2.55(4) 2_777 ? N11 C15 1.33(7) . ? N11 C11 1.35(7) . ? C11 C12 1.38(7) . ? C12 C13 1.38(7) . ? C13 C14 1.38(7) . ? C14 C15 1.39(7) . ? N21 C21 1.33(6) . ? N21 C25 1.34(7) . ? C21 C22 1.39(7) . ? C22 C23 1.37(7) . ? C23 C24 1.36(6) . ? C24 C25 1.38(7) . ? N31 C35 1.35(7) . ? N31 C31 1.34(7) . ? C31 C32 1.38(7) . ? C32 C33 1.38(7) . ? C33 C34 1.38(7) . ? C34 C35 1.39(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cd1 N2 180.0 . 2_666 ? N2 Cd1 N31 87.82(6) . 2_666 ? N2 Cd1 N31 92.2(16) 2_666 2_666 ? N2 Cd1 N31 92.2(16) . . ? N2 Cd1 N31 87.82(6) 2_666 . ? N31 Cd1 N31 180.0 2_666 . ? N2 Cd1 S1 97.6(10) . . ? N2 Cd1 S1 82.47(5) 2_666 . ? N31 Cd1 S1 98.12(5) 2_666 . ? N31 Cd1 S1 81.9(14) . . ? N2 Cd1 S1 82.47(5) . 2_666 ? N2 Cd1 S1 97.53(5) 2_666 2_666 ? N31 Cd1 S1 81.88(5) 2_666 2_666 ? N31 Cd1 S1 98.12(5) . 2_666 ? S1 Cd1 S1 180.0 . 2_666 ? N1 Cd2 N11 93.8(17) . . ? N1 Cd2 N21 88.8(16) . . ? N11 Cd2 N21 172.9(18) . . ? N1 Cd2 N3 161.73(5) . 2_777 ? N11 Cd2 N3 83.73(6) . 2_777 ? N21 Cd2 N3 91.90(6) . 2_777 ? N1 Cd2 S3 66.5(11) . . ? N11 Cd2 S3 104.5(15) . . ? N21 Cd2 S3 70.5(13) . . ? N3 Cd2 S3 96.52(3) 2_777 . ? N1 Cd2 S2 92.9(12) . . ? N11 Cd2 S2 89.5(15) . . ? N21 Cd2 S2 97.0(14) . . ? N3 Cd2 S2 105.02(3) 2_777 . ? S3 Cd2 S2 155.4(11) . . ? C1 S1 Cd1 100.1(19) . . ? N1 C1 S1 179(5) . . ? C1 N1 Cd2 162(3) . . ? C2 S2 Cd2 104.9(18) . . ? N2 C2 S2 179(5) . . ? C2 N2 Cd1 161(2) . . ? C3 S3 Cd2 87.2(14) . . ? N3 C3 S3 179(4) . . ? C3 N3 Cd2 174.78(13) . 2_777 ? C15 N11 C11 117(5) . . ? C15 N11 Cd2 126(4) . . ? C11 N11 Cd2 117(3) . . ? N11 C11 C12 123(5) . . ? C11 C12 C13 119(4) . . ? C14 C13 C12 119(4) . . ? C13 C14 C15 119(4) . . ? N11 C15 C14 123(5) . . ? C21 N21 C25 117(4) . . ? C21 N21 Cd2 125(4) . . ? C25 N21 Cd2 118(3) . . ? N21 C21 C22 123(4) . . ? C23 C22 C21 119(4) . . ? C24 C23 C22 119(4) . . ? C23 C24 C25 119(4) . . ? N21 C25 C24 124(4) . . ? C35 N31 C31 117(5) . . ? C35 N31 Cd1 118(3) . . ? C31 N31 Cd1 124(5) . . ? N31 C31 C32 124(5) . . ? C31 C32 C33 118(5) . . ? C34 C33 C32 119(5) . . ? C33 C34 C35 119(4) . . ? N31 C35 C34 122(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.011 _refine_diff_density_min -0.013 _refine_diff_density_rms 0.002 # Attachment '- [Cd(NCS)2(pyridine)]n.CIF' data_dap329_1 _database_code_depnum_ccdc_archive 'CCDC 872126' #TrackingRef '- [Cd(NCS)2(pyridine)]n.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H5 Cd N3 S2' _chemical_formula_sum 'C7 H5 Cd N3 S2' _chemical_formula_weight 307.66 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall 'P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 5.9496(3) _cell_length_b 12.2417(8) _cell_length_c 13.8473(7) _cell_angle_alpha 90.00 _cell_angle_beta 102.234(4) _cell_angle_gamma 90.00 _cell_volume 985.64(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15155 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 26.99 _exptl_crystal_description block _exptl_crystal_colour white _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.073 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 2.592 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6105 _exptl_absorpt_correction_T_max 0.8281 _exptl_absorpt_process_details 'X-Shape and X-Red32 (Stoe, 2008)' _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 'STOE IPDS-2' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 15155 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_sigmaI/netI 0.0178 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 26.99 _reflns_number_total 2159 _reflns_number_gt 2026 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area (Stoe, 2008)' _computing_cell_refinement 'X-Area (Stoe, 2008)' _computing_data_reduction 'X-Area (Stoe, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; XP in SHELXTL (Sheldrick, 2008) and Diamond (Brandenburg, 2011) ; _computing_publication_material 'XCIF in SHELXTL (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0191P)^2^+0.4616P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0046(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2159 _refine_ls_number_parameters 119 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0249 _refine_ls_R_factor_gt 0.0218 _refine_ls_wR_factor_ref 0.0465 _refine_ls_wR_factor_gt 0.0454 _refine_ls_goodness_of_fit_ref 1.147 _refine_ls_restrained_S_all 1.147 _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 0.39355(3) 0.841494(13) 0.521245(13) 0.03382(7) Uani 1 1 d . . . N1 N 0.0415(3) 0.89164(17) 0.42664(16) 0.0383(4) Uani 1 1 d . . . C1 C -0.1484(4) 0.91893(17) 0.40917(16) 0.0299(4) Uani 1 1 d . . . S1 S -0.42188(9) 0.95710(4) 0.38080(4) 0.03229(12) Uani 1 1 d . . . N2 N -0.2419(3) 0.80433(19) 0.60476(17) 0.0436(5) Uani 1 1 d . . . C2 C -0.0498(4) 0.78254(18) 0.62879(17) 0.0325(4) Uani 1 1 d . . . S2 S 0.22318(10) 0.74862(5) 0.66495(5) 0.04116(14) Uani 1 1 d . . . N10 N 0.3820(3) 0.67958(15) 0.43231(16) 0.0369(4) Uani 1 1 d . . . C10 C 0.5458(5) 0.6518(2) 0.3847(2) 0.0468(6) Uani 1 1 d . . . H10 H 0.6665 0.7003 0.3851 0.056 Uiso 1 1 calc R . . C11 C 0.5440(5) 0.5542(2) 0.3346(2) 0.0532(7) Uani 1 1 d . . . H11 H 0.6608 0.5379 0.3016 0.064 Uiso 1 1 calc R . . C12 C 0.3691(5) 0.4816(2) 0.3339(2) 0.0514(7) Uani 1 1 d . . . H12 H 0.3661 0.4148 0.3017 0.062 Uiso 1 1 calc R . . C13 C 0.1994(5) 0.5094(2) 0.3816(3) 0.0599(8) Uani 1 1 d . . . H13 H 0.0771 0.4621 0.3817 0.072 Uiso 1 1 calc R . . C14 C 0.2112(5) 0.6086(2) 0.4297(2) 0.0538(7) Uani 1 1 d . . . H14 H 0.0942 0.6268 0.4620 0.065 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.02196(9) 0.03278(10) 0.04685(11) -0.00145(7) 0.00756(7) 0.00157(6) N1 0.0262(9) 0.0415(11) 0.0475(12) -0.0026(9) 0.0083(8) 0.0034(8) C1 0.0293(11) 0.0289(10) 0.0319(11) -0.0026(8) 0.0075(8) -0.0024(8) S1 0.0225(2) 0.0337(3) 0.0396(3) -0.0002(2) 0.0043(2) 0.0024(2) N2 0.0250(9) 0.0533(12) 0.0523(13) 0.0065(10) 0.0079(9) 0.0032(9) C2 0.0314(11) 0.0303(10) 0.0379(12) 0.0014(9) 0.0119(9) -0.0013(9) S2 0.0261(3) 0.0505(3) 0.0479(3) 0.0109(3) 0.0100(2) 0.0081(2) N10 0.0350(10) 0.0319(9) 0.0447(11) -0.0015(8) 0.0104(9) -0.0005(8) C10 0.0459(14) 0.0398(13) 0.0595(17) -0.0014(11) 0.0224(13) -0.0009(11) C11 0.0599(17) 0.0435(14) 0.0613(18) -0.0052(12) 0.0246(14) 0.0093(13) C12 0.0599(17) 0.0363(13) 0.0526(16) -0.0062(12) -0.0004(13) 0.0060(12) C13 0.0535(17) 0.0479(15) 0.078(2) -0.0148(15) 0.0137(16) -0.0178(13) C14 0.0403(14) 0.0541(16) 0.071(2) -0.0172(14) 0.0217(13) -0.0127(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N2 2.277(2) 1_655 ? Cd1 N1 2.306(2) . ? Cd1 N10 2.327(2) . ? Cd1 S2 2.6711(7) . ? Cd1 S1 2.8018(6) 3_576 ? Cd1 S1 2.8100(6) 1_655 ? N1 C1 1.154(3) . ? C1 S1 1.658(2) . ? S1 Cd1 2.8018(6) 3_576 ? S1 Cd1 2.8100(6) 1_455 ? N2 C2 1.152(3) . ? N2 Cd1 2.277(2) 1_455 ? C2 S2 1.648(2) . ? N10 C10 1.331(3) . ? N10 C14 1.332(3) . ? C10 C11 1.381(4) . ? C11 C12 1.367(4) . ? C12 C13 1.361(4) . ? C13 C14 1.380(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cd1 N1 173.95(7) 1_655 . ? N2 Cd1 N10 90.96(8) 1_655 . ? N1 Cd1 N10 90.27(7) . . ? N2 Cd1 S2 90.44(6) 1_655 . ? N1 Cd1 S2 95.40(5) . . ? N10 Cd1 S2 93.35(5) . . ? N2 Cd1 S1 88.67(6) 1_655 3_576 ? N1 Cd1 S1 89.71(5) . 3_576 ? N10 Cd1 S1 176.22(5) . 3_576 ? S2 Cd1 S1 90.42(2) . 3_576 ? N2 Cd1 S1 88.98(6) 1_655 1_655 ? N1 Cd1 S1 85.06(5) . 1_655 ? N10 Cd1 S1 91.99(5) . 1_655 ? S2 Cd1 S1 174.64(2) . 1_655 ? S1 Cd1 S1 84.237(18) 3_576 1_655 ? C1 N1 Cd1 158.06(19) . . ? N1 C1 S1 178.4(2) . . ? C1 S1 Cd1 100.25(8) . 3_576 ? C1 S1 Cd1 101.65(8) . 1_455 ? Cd1 S1 Cd1 95.763(18) 3_576 1_455 ? C2 N2 Cd1 166.6(2) . 1_455 ? N2 C2 S2 178.5(2) . . ? C2 S2 Cd1 99.88(8) . . ? C10 N10 C14 117.1(2) . . ? C10 N10 Cd1 122.46(17) . . ? C14 N10 Cd1 120.45(17) . . ? N10 C10 C11 122.7(3) . . ? C12 C11 C10 119.4(3) . . ? C13 C12 C11 118.4(3) . . ? C12 C13 C14 119.2(3) . . ? N10 C14 C13 123.2(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.324 _refine_diff_density_min -0.336 _refine_diff_density_rms 0.065