# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Nather, Christian' 'Boeckmann, Jan' 'Jess, Inke' _publ_contact_author_name 'Nather, Christian' _publ_contact_author_email cnaether@ac.uni-kiel.de _publ_section_title ; New Cadmium Thio- and Selenocyanato Coordination Compounds: Structural Snapshots on the Reaction Pathway to more Condensed Anionic Networks ; # Attachment 'Compound_1D_[Cd(NCS)2]3(pyrimidine)2_CD62.CIF' data_cd62 _database_code_depnum_ccdc_archive 'CCDC 836232' #TrackingRef 'Compound_1D_[Cd(NCS)2]3(pyrimidine)2_CD62.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H8 Cd3 N10 S6' _chemical_formula_sum 'C14 H8 Cd3 N10 S6' _chemical_formula_weight 845.86 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.9128(4) _cell_length_b 9.2461(6) _cell_length_c 10.6609(7) _cell_angle_alpha 108.162(5) _cell_angle_beta 91.352(5) _cell_angle_gamma 103.857(5) _cell_volume 625.04(7) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.247 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 402 _exptl_absorpt_coefficient_mu 3.055 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.694 _exptl_absorpt_correction_T_max 0.774 _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 ? _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 7240 _diffrn_reflns_av_R_equivalents 0.0171 _diffrn_reflns_av_sigmaI/netI 0.0165 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.99 _reflns_number_total 2980 _reflns_number_gt 2761 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0207P)^2^+0.2013P] 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 0.0023(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2980 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0228 _refine_ls_R_factor_gt 0.0190 _refine_ls_wR_factor_ref 0.0426 _refine_ls_wR_factor_gt 0.0416 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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 0.0000 0.5000 0.5000 0.03323(7) Uani 1 2 d S . . Cd2 Cd 0.0000 0.0000 0.0000 0.03510(7) Uani 1 2 d S . . Cd3 Cd 0.5000 0.5000 0.0000 0.03064(7) Uani 1 2 d S . . S1 S 0.32033(9) 0.74957(7) 0.60476(5) 0.04093(13) Uani 1 1 d . . . C1 C 0.2437(3) 0.8345(2) 0.7474(2) 0.0333(4) Uani 1 1 d . . . N1 N 0.1910(3) 0.8957(2) 0.8471(2) 0.0452(5) Uani 1 1 d . . . S2 S 0.32706(8) 0.26203(6) 0.09725(5) 0.03633(12) Uani 1 1 d . . . C2 C 0.2339(3) 0.3642(2) 0.2264(2) 0.0345(4) Uani 1 1 d . . . N2 N 0.1706(4) 0.4338(3) 0.3179(2) 0.0500(5) Uani 1 1 d . . . S3 S 0.12315(11) -0.11156(7) 0.18645(6) 0.04653(14) Uani 1 1 d . . . C3 C 0.1975(3) -0.2650(3) 0.0994(2) 0.0351(4) Uani 1 1 d . . . N3 N 0.2529(3) -0.3733(3) 0.0421(2) 0.0460(5) Uani 1 1 d . . . N11 N 0.1553(3) 0.3540(2) 0.59651(17) 0.0366(4) Uani 1 1 d . . . C11 C 0.2389(3) 0.4161(2) 0.72145(19) 0.0351(4) Uani 1 1 d . . . H11 H 0.2188 0.5128 0.7710 0.042 Uiso 1 1 calc R . . N12 N 0.3484(3) 0.3523(2) 0.78156(16) 0.0323(4) Uani 1 1 d . . . C12 C 0.3719(3) 0.2115(3) 0.7106(2) 0.0378(5) Uani 1 1 d . . . H12 H 0.4467 0.1626 0.7497 0.045 Uiso 1 1 calc R . . C13 C 0.2883(4) 0.1372(3) 0.5814(2) 0.0405(5) Uani 1 1 d . . . H13 H 0.3033 0.0385 0.5328 0.049 Uiso 1 1 calc R . . C14 C 0.1819(4) 0.2144(3) 0.5268(2) 0.0395(5) Uani 1 1 d . . . H14 H 0.1267 0.1680 0.4387 0.047 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 0.04590(13) 0.03556(12) 0.02157(9) 0.00781(8) 0.00237(8) 0.01893(9) Cd2 0.04112(12) 0.03176(11) 0.03168(11) 0.00508(8) 0.00885(8) 0.01466(9) Cd3 0.03400(11) 0.03444(12) 0.02521(10) 0.00842(8) 0.00095(7) 0.01405(8) S1 0.0455(3) 0.0411(3) 0.0325(3) 0.0070(2) 0.0117(2) 0.0104(2) C1 0.0330(10) 0.0290(10) 0.0373(10) 0.0090(8) 0.0047(8) 0.0095(8) N1 0.0466(11) 0.0403(11) 0.0426(10) 0.0021(8) 0.0121(8) 0.0145(9) S2 0.0422(3) 0.0292(2) 0.0335(2) 0.00635(19) 0.0113(2) 0.0061(2) C2 0.0394(11) 0.0312(10) 0.0290(9) 0.0091(8) 0.0040(8) 0.0031(8) N2 0.0591(13) 0.0467(11) 0.0347(10) 0.0030(8) 0.0148(9) 0.0088(10) S3 0.0619(4) 0.0454(3) 0.0367(3) 0.0106(2) 0.0069(3) 0.0258(3) C3 0.0304(10) 0.0417(11) 0.0367(10) 0.0174(9) 0.0025(8) 0.0098(8) N3 0.0438(11) 0.0508(12) 0.0510(11) 0.0176(9) 0.0083(9) 0.0247(9) N11 0.0472(10) 0.0333(9) 0.0301(8) 0.0089(7) -0.0042(7) 0.0145(8) C11 0.0462(12) 0.0301(10) 0.0291(9) 0.0074(8) 0.0003(8) 0.0135(9) N12 0.0370(9) 0.0301(8) 0.0303(8) 0.0119(6) -0.0019(7) 0.0075(7) C12 0.0409(11) 0.0324(11) 0.0427(11) 0.0136(9) -0.0018(9) 0.0131(9) C13 0.0470(12) 0.0313(10) 0.0418(11) 0.0065(9) 0.0035(9) 0.0149(9) C14 0.0491(12) 0.0358(11) 0.0293(9) 0.0053(8) -0.0015(9) 0.0110(9) _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 2.291(2) . ? Cd1 N2 2.291(2) 2_566 ? Cd1 N11 2.3542(17) . ? Cd1 N11 2.3542(17) 2_566 ? Cd1 S1 2.7027(6) 2_566 ? Cd1 S1 2.7027(6) . ? Cd2 N1 2.2499(19) 2_566 ? Cd2 N1 2.2499(19) 1_544 ? Cd2 S3 2.7127(6) . ? Cd2 S3 2.7127(6) 2 ? Cd2 S2 2.7849(6) 2 ? Cd2 S2 2.7849(6) . ? Cd3 N3 2.271(2) 2_655 ? Cd3 N3 2.271(2) 1_565 ? Cd3 N12 2.3671(16) 1_554 ? Cd3 N12 2.3671(16) 2_666 ? Cd3 S2 2.7507(6) . ? Cd3 S2 2.7507(6) 2_665 ? S1 C1 1.644(2) . ? C1 N1 1.151(3) . ? N1 Cd2 2.2499(19) 1_566 ? S2 C2 1.651(2) . ? C2 N2 1.149(3) . ? S3 C3 1.640(2) . ? C3 N3 1.155(3) . ? N3 Cd3 2.271(2) 1_545 ? N11 C11 1.329(3) . ? N11 C14 1.332(3) . ? C11 N12 1.326(3) . ? N12 C12 1.337(3) . ? N12 Cd3 2.3671(16) 1_556 ? C12 C13 1.373(3) . ? C13 C14 1.371(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cd1 N2 180.000(1) . 2_566 ? N2 Cd1 N11 89.63(8) . . ? N2 Cd1 N11 90.37(8) 2_566 . ? N2 Cd1 N11 90.37(8) . 2_566 ? N2 Cd1 N11 89.63(8) 2_566 2_566 ? N11 Cd1 N11 180.00(7) . 2_566 ? N2 Cd1 S1 93.56(6) . 2_566 ? N2 Cd1 S1 86.44(6) 2_566 2_566 ? N11 Cd1 S1 91.64(5) . 2_566 ? N11 Cd1 S1 88.36(5) 2_566 2_566 ? N2 Cd1 S1 86.44(6) . . ? N2 Cd1 S1 93.56(6) 2_566 . ? N11 Cd1 S1 88.36(5) . . ? N11 Cd1 S1 91.64(5) 2_566 . ? S1 Cd1 S1 180.00(2) 2_566 . ? N1 Cd2 N1 180.00(9) 2_566 1_544 ? N1 Cd2 S3 84.78(6) 2_566 . ? N1 Cd2 S3 95.22(6) 1_544 . ? N1 Cd2 S3 95.22(6) 2_566 2 ? N1 Cd2 S3 84.78(6) 1_544 2 ? S3 Cd2 S3 180.00(2) . 2 ? N1 Cd2 S2 87.15(5) 2_566 2 ? N1 Cd2 S2 92.85(5) 1_544 2 ? S3 Cd2 S2 91.95(2) . 2 ? S3 Cd2 S2 88.05(2) 2 2 ? N1 Cd2 S2 92.85(5) 2_566 . ? N1 Cd2 S2 87.15(5) 1_544 . ? S3 Cd2 S2 88.05(2) . . ? S3 Cd2 S2 91.95(2) 2 . ? S2 Cd2 S2 180.00(3) 2 . ? N3 Cd3 N3 180.0 2_655 1_565 ? N3 Cd3 N12 88.29(7) 2_655 1_554 ? N3 Cd3 N12 91.71(7) 1_565 1_554 ? N3 Cd3 N12 91.71(7) 2_655 2_666 ? N3 Cd3 N12 88.29(7) 1_565 2_666 ? N12 Cd3 N12 180.00(5) 1_554 2_666 ? N3 Cd3 S2 84.01(6) 2_655 . ? N3 Cd3 S2 95.99(6) 1_565 . ? N12 Cd3 S2 92.61(4) 1_554 . ? N12 Cd3 S2 87.39(4) 2_666 . ? N3 Cd3 S2 95.99(6) 2_655 2_665 ? N3 Cd3 S2 84.01(6) 1_565 2_665 ? N12 Cd3 S2 87.39(4) 1_554 2_665 ? N12 Cd3 S2 92.61(4) 2_666 2_665 ? S2 Cd3 S2 180.0 . 2_665 ? C1 S1 Cd1 100.13(8) . . ? N1 C1 S1 179.2(2) . . ? C1 N1 Cd2 162.0(2) . 1_566 ? C2 S2 Cd3 99.40(8) . . ? C2 S2 Cd2 99.01(8) . . ? Cd3 S2 Cd2 132.46(2) . . ? N2 C2 S2 178.5(2) . . ? C2 N2 Cd1 163.3(2) . . ? C3 S3 Cd2 103.61(8) . . ? N3 C3 S3 177.6(2) . . ? C3 N3 Cd3 150.51(18) . 1_545 ? C11 N11 C14 116.84(18) . . ? C11 N11 Cd1 120.39(14) . . ? C14 N11 Cd1 122.43(13) . . ? N12 C11 N11 125.64(19) . . ? C11 N12 C12 116.73(17) . . ? C11 N12 Cd3 118.11(13) . 1_556 ? C12 N12 Cd3 125.09(13) . 1_556 ? N12 C12 C13 121.67(19) . . ? C14 C13 C12 117.3(2) . . ? N11 C14 C13 121.79(19) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.411 _refine_diff_density_min -0.963 _refine_diff_density_rms 0.061 # Attachment 'Compound_1C_Cd(NCS)2(pyrimidine)_CD77A.CIF' data_cd77a _database_code_depnum_ccdc_archive 'CCDC 836233' #TrackingRef 'Compound_1C_Cd(NCS)2(pyrimidine)_CD77A.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H4 Cd N4 S2' _chemical_formula_sum 'C6 H4 Cd N4 S2' _chemical_formula_weight 308.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'P 21/m' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 5.6358(9) _cell_length_b 12.4946(15) _cell_length_c 7.1516(13) _cell_angle_alpha 90.00 _cell_angle_beta 105.634(14) _cell_angle_gamma 90.00 _cell_volume 484.96(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.114 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 296 _exptl_absorpt_coefficient_mu 2.637 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.658 _exptl_absorpt_correction_T_max 0.803 _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 ? _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 6520 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0281 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 25.89 _reflns_number_total 6520 _reflns_number_gt 5132 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0230P)^2^+0.3927P] 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 6520 _refine_ls_number_parameters 65 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0526 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0636 _refine_ls_wR_factor_gt 0.0595 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 0.5000 0.5000 0.04022(6) Uani 1 2 d S . . S1 S 0.36039(10) 0.58526(5) 0.80117(8) 0.05313(14) Uani 1 1 d . . . C1 C 0.0665(3) 0.59259(14) 0.6874(3) 0.0385(4) Uani 1 1 d . . . N1 N -0.1418(3) 0.59545(14) 0.6098(3) 0.0508(4) Uani 1 1 d . . . N11 N 0.3074(3) 0.65539(12) 0.3211(2) 0.0385(4) Uani 1 1 d . . . C13 C 0.4022(5) 0.7500 0.3830(4) 0.0394(6) Uani 1 2 d S . . H13 H 0.5503 0.7500 0.4798 0.047 Uiso 1 2 calc SR . . C11 C 0.0937(4) 0.65654(15) 0.1812(3) 0.0447(5) Uani 1 1 d . . . H11 H 0.0205 0.5919 0.1330 0.054 Uiso 1 1 calc R . . C12 C -0.0192(5) 0.7500 0.1078(4) 0.0493(7) Uani 1 2 d S . . H12 H -0.1676 0.7500 0.0113 0.059 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 0.02975(8) 0.03083(8) 0.05718(11) -0.00093(12) 0.00673(7) 0.00277(12) S1 0.0371(2) 0.0698(4) 0.0467(3) -0.0075(3) 0.0014(2) 0.0067(3) C1 0.0394(11) 0.0306(9) 0.0469(10) -0.0030(7) 0.0140(9) 0.0007(9) N1 0.0322(9) 0.0432(10) 0.0756(11) -0.0107(8) 0.0122(8) -0.0026(8) N11 0.0401(9) 0.0295(8) 0.0446(8) -0.0011(6) 0.0091(7) 0.0019(7) C13 0.0360(14) 0.0294(13) 0.0503(14) 0.000 0.0073(11) 0.000 C11 0.0513(12) 0.0367(10) 0.0421(10) -0.0054(8) 0.0058(9) -0.0040(9) C12 0.0478(16) 0.0445(16) 0.0457(15) 0.000 -0.0042(12) 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 N1 2.2935(17) 3_566 ? Cd1 N1 2.2935(17) 1_655 ? Cd1 N11 2.4160(15) . ? Cd1 N11 2.4160(15) 3_666 ? Cd1 S1 2.7030(7) . ? Cd1 S1 2.7030(7) 3_666 ? S1 C1 1.639(2) . ? C1 N1 1.156(2) . ? N1 Cd1 2.2935(17) 1_455 ? N11 C13 1.3234(19) . ? N11 C11 1.342(2) . ? C13 N11 1.3234(18) 4_575 ? C11 C12 1.365(2) . ? C12 C11 1.365(2) 4_575 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 N1 180.00(8) 3_566 1_655 ? N1 Cd1 N11 90.47(6) 3_566 . ? N1 Cd1 N11 89.53(6) 1_655 . ? N1 Cd1 N11 89.53(6) 3_566 3_666 ? N1 Cd1 N11 90.47(6) 1_655 3_666 ? N11 Cd1 N11 180.000(1) . 3_666 ? N1 Cd1 S1 93.40(5) 3_566 . ? N1 Cd1 S1 86.60(5) 1_655 . ? N11 Cd1 S1 85.39(4) . . ? N11 Cd1 S1 94.61(4) 3_666 . ? N1 Cd1 S1 86.60(5) 3_566 3_666 ? N1 Cd1 S1 93.40(5) 1_655 3_666 ? N11 Cd1 S1 94.61(4) . 3_666 ? N11 Cd1 S1 85.39(4) 3_666 3_666 ? S1 Cd1 S1 180.000(11) . 3_666 ? C1 S1 Cd1 95.66(7) . . ? N1 C1 S1 178.23(19) . . ? C1 N1 Cd1 146.57(16) . 1_455 ? C13 N11 C11 116.11(17) . . ? C13 N11 Cd1 117.21(13) . . ? C11 N11 Cd1 126.02(12) . . ? N11 C13 N11 126.5(2) . 4_575 ? N11 C11 C12 121.82(19) . . ? C11 C12 C11 117.6(3) 4_575 . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.89 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.397 _refine_diff_density_min -0.770 _refine_diff_density_rms 0.078 # Attachment 'Compound_1B_[Cd(NCS)2]2(pyrimidine)3_CD77.CIF' data_cd77 _database_code_depnum_ccdc_archive 'CCDC 836234' #TrackingRef 'Compound_1B_[Cd(NCS)2]2(pyrimidine)3_CD77.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H12 Cd2 N10 S4' _chemical_formula_sum 'C16 H12 Cd2 N10 S4' _chemical_formula_weight 697.40 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 orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2' _symmetry_space_group_name_Hall 'P 2 2ab' 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' _cell_length_a 11.2398(6) _cell_length_b 14.8326(7) _cell_length_c 7.3449(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1224.51(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.891 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 676 _exptl_absorpt_coefficient_mu 2.103 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.361 _exptl_absorpt_correction_T_max 0.524 _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 ? _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 6607 _diffrn_reflns_av_R_equivalents 0.0456 _diffrn_reflns_av_sigmaI/netI 0.0453 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.10 _reflns_number_total 2180 _reflns_number_gt 1896 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0237P)^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 constr _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 0.01(5) _refine_ls_number_reflns 2180 _refine_ls_number_parameters 146 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.0647 _refine_ls_wR_factor_gt 0.0625 _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_restrained_S_all 1.148 _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 0.54982(4) 0.28012(3) 0.45093(7) 0.04685(13) Uani 1 1 d . . . S1 S 0.70539(17) 0.36597(15) 0.2262(3) 0.0645(6) Uani 1 1 d . . . N1 N 0.9110(4) 0.2845(5) 0.3631(8) 0.0606(15) Uani 1 1 d . . . C1 C 0.8268(6) 0.3186(4) 0.3075(9) 0.0454(15) Uani 1 1 d . . . S2 S 0.89756(17) 0.18410(17) 0.8194(3) 0.0721(6) Uani 1 1 d . . . N2 N 0.6895(5) 0.2558(4) 0.6780(9) 0.0624(18) Uani 1 1 d . . . C2 C 0.7759(6) 0.2264(6) 0.7345(8) 0.0504(15) Uani 1 1 d . . . N11 N 0.5118(5) 0.4207(4) 0.6035(7) 0.0497(14) Uani 1 1 d . . . C11 C 0.5000 0.5000 0.5205(13) 0.052(2) Uani 1 2 d S . . H11 H 0.5000 0.5000 0.3939 0.063 Uiso 1 2 calc SR . . C12 C 0.5097(7) 0.4218(5) 0.7828(10) 0.066(2) Uani 1 1 d . . . H12 H 0.5149 0.3678 0.8464 0.079 Uiso 1 1 calc R . . C13 C 0.5000 0.5000 0.8759(16) 0.084(4) Uani 1 2 d S . . H13 H 0.5000 0.5000 1.0026 0.101 Uiso 1 2 calc SR . . N21 N 0.6093(5) 0.1415(4) 0.3227(10) 0.0650(17) Uani 1 1 d . . . N22 N 0.6469(11) 0.0519(7) 0.0589(18) 0.146(4) Uani 1 1 d . . . C21 C 0.6170(9) 0.1299(7) 0.1436(15) 0.100(3) Uani 1 1 d . . . H21 H 0.6004 0.1794 0.0702 0.120 Uiso 1 1 calc R . . C22 C 0.6685(12) -0.0173(8) 0.178(3) 0.124(5) Uani 1 1 d . . . H22 H 0.6867 -0.0736 0.1301 0.148 Uiso 1 1 calc R . . C23 C 0.6654(11) -0.0096(6) 0.3555(19) 0.097(3) Uani 1 1 d . . . H23 H 0.6844 -0.0576 0.4317 0.116 Uiso 1 1 calc R . . C24 C 0.6337(8) 0.0699(6) 0.4211(15) 0.087(3) Uani 1 1 d . . . H24 H 0.6284 0.0756 0.5469 0.104 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 0.0447(2) 0.0455(2) 0.0504(2) 0.0015(3) 0.0039(3) 0.0036(3) S1 0.0497(10) 0.0757(14) 0.0682(14) 0.0302(11) 0.0044(9) 0.0073(9) N1 0.048(3) 0.071(4) 0.063(3) 0.016(4) -0.002(2) 0.011(3) C1 0.046(4) 0.046(4) 0.044(4) 0.006(3) 0.006(3) -0.003(3) S2 0.0543(10) 0.1060(18) 0.0561(12) 0.0273(11) -0.0002(9) 0.0144(10) N2 0.054(3) 0.075(5) 0.057(4) 0.011(3) 0.000(3) 0.005(3) C2 0.053(4) 0.057(4) 0.042(4) 0.003(4) 0.004(3) -0.005(4) N11 0.060(3) 0.051(3) 0.039(3) 0.001(2) 0.005(2) 0.000(2) C11 0.078(6) 0.044(5) 0.035(5) 0.000 0.000 0.009(4) C12 0.096(6) 0.046(4) 0.057(5) 0.008(4) 0.014(4) 0.014(4) C13 0.137(12) 0.067(8) 0.048(6) 0.000 0.000 0.017(7) N21 0.074(4) 0.047(4) 0.074(5) 0.007(3) 0.019(4) 0.000(3) N22 0.196(10) 0.096(7) 0.145(9) -0.039(8) 0.085(9) -0.014(7) C21 0.137(9) 0.071(6) 0.093(7) -0.004(6) 0.043(6) -0.003(6) C22 0.120(9) 0.067(8) 0.183(15) -0.028(9) 0.048(11) 0.005(7) C23 0.115(8) 0.041(5) 0.135(9) 0.001(6) 0.002(8) 0.027(5) C24 0.100(6) 0.067(6) 0.093(7) 0.001(6) 0.007(6) 0.009(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N1 2.284(6) 4_456 ? Cd1 N2 2.319(6) . ? Cd1 N21 2.358(6) . ? Cd1 N11 2.406(5) . ? Cd1 S2 2.674(2) 4_456 ? Cd1 S1 2.7210(19) . ? S1 C1 1.647(7) . ? N1 C1 1.149(8) . ? N1 Cd1 2.284(6) 4_556 ? S2 C2 1.628(7) . ? S2 Cd1 2.674(2) 4_556 ? N2 C2 1.142(8) . ? N11 C12 1.317(9) . ? N11 C11 1.331(7) . ? C11 N11 1.331(7) 2_665 ? C12 C13 1.351(9) . ? C13 C12 1.351(9) 2_665 ? N21 C24 1.313(10) . ? N21 C21 1.329(11) . ? N22 C21 1.356(13) . ? N22 C22 1.372(17) . ? C22 C23 1.306(16) . ? C23 C24 1.323(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 N2 88.11(18) 4_456 . ? N1 Cd1 N21 93.8(2) 4_456 . ? N2 Cd1 N21 87.7(2) . . ? N1 Cd1 N11 87.9(2) 4_456 . ? N2 Cd1 N11 85.4(2) . . ? N21 Cd1 N11 172.8(2) . . ? N1 Cd1 S2 95.18(14) 4_456 4_456 ? N2 Cd1 S2 176.49(15) . 4_456 ? N21 Cd1 S2 93.32(18) . 4_456 ? N11 Cd1 S2 93.45(13) . 4_456 ? N1 Cd1 S1 176.36(18) 4_456 . ? N2 Cd1 S1 94.24(15) . . ? N21 Cd1 S1 89.07(16) . . ? N11 Cd1 S1 89.48(13) . . ? S2 Cd1 S1 82.41(6) 4_456 . ? C1 S1 Cd1 96.5(2) . . ? C1 N1 Cd1 163.8(5) . 4_556 ? N1 C1 S1 179.1(7) . . ? C2 S2 Cd1 100.2(2) . 4_556 ? C2 N2 Cd1 153.7(6) . . ? N2 C2 S2 178.8(6) . . ? C12 N11 C11 116.4(7) . . ? C12 N11 Cd1 118.7(5) . . ? C11 N11 Cd1 124.7(5) . . ? N11 C11 N11 125.5(9) . 2_665 ? N11 C12 C13 121.2(8) . . ? C12 C13 C12 119.1(11) . 2_665 ? C24 N21 C21 115.2(8) . . ? C24 N21 Cd1 123.0(6) . . ? C21 N21 Cd1 121.8(6) . . ? C21 N22 C22 112.8(11) . . ? N21 C21 N22 125.5(11) . . ? C23 C22 N22 124.5(11) . . ? C22 C23 C24 116.6(11) . . ? N21 C24 C23 125.2(10) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.627 _refine_diff_density_min -0.629 _refine_diff_density_rms 0.080 # Attachment 'Compound_1A_Cd(NCS)2(pyrimidine)2_CD11.CIF' data_cd11 _database_code_depnum_ccdc_archive 'CCDC 836235' #TrackingRef 'Compound_1A_Cd(NCS)2(pyrimidine)2_CD11.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H8 Cd N6 S2' _chemical_formula_sum 'C10 H8 Cd N6 S2' _chemical_formula_weight 388.74 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 orthorhombic _symmetry_space_group_name_H-M 'C m c a' _symmetry_space_group_name_Hall '-C 2bc 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' 'x, -y, -z' '-x, y+1/2, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1, -z+1/2' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x, y, z' 'x, -y-1/2, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' '-x+1/2, y+1/2, z' 'x+1/2, -y, z-1/2' _cell_length_a 10.0015(6) _cell_length_b 15.6680(7) _cell_length_c 8.6696(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1358.56(13) _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 ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.901 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 1.908 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.753 _exptl_absorpt_correction_T_max 0.937 _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 ? _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 7848 _diffrn_reflns_av_R_equivalents 0.0816 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 29.21 _reflns_number_total 967 _reflns_number_gt 795 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0382P)^2^+0.8555P] 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 967 _refine_ls_number_parameters 51 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0670 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.0895 _refine_ls_wR_factor_gt 0.0843 _refine_ls_goodness_of_fit_ref 1.213 _refine_ls_restrained_S_all 1.213 _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 0.0000 0.5000 0.0000 0.03335(17) Uani 1 4 d S . . N1 N 0.0000 0.3912(4) 0.1647(6) 0.0496(13) Uani 1 2 d S . . C1 C 0.0000 0.3785(4) 0.2958(7) 0.0383(12) Uani 1 2 d S . . S1 S 0.0000 0.35891(15) 0.47668(18) 0.0636(5) Uani 1 2 d S . . N11 N 0.1684(3) 0.5736(2) 0.1506(4) 0.0405(7) Uani 1 1 d . . . C11 C 0.1729(4) 0.6591(3) 0.1481(5) 0.0418(9) Uani 1 1 d . . . H11 H 0.1224 0.6885 0.0753 0.050 Uiso 1 1 calc R . . C12 C 0.2500 0.7044(4) 0.2500 0.0451(13) Uani 1 2 d S . . H12 H 0.2500 0.7637 0.2500 0.054 Uiso 1 2 calc SR . . C13 C 0.2500 0.5352(4) 0.2500 0.0424(12) Uani 1 2 d S . . H13 H 0.2500 0.4758 0.2500 0.051 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 0.0322(2) 0.0393(3) 0.0285(2) 0.0020(3) 0.000 0.000 N1 0.055(3) 0.049(3) 0.045(3) 0.011(2) 0.000 0.000 C1 0.038(3) 0.030(3) 0.047(3) 0.004(2) 0.000 0.000 S1 0.0891(13) 0.0705(11) 0.0310(8) 0.0043(7) 0.000 0.000 N11 0.0334(16) 0.0442(18) 0.0438(18) 0.0016(15) -0.0057(14) -0.0003(14) C11 0.038(2) 0.043(2) 0.045(2) 0.0057(17) -0.0059(17) 0.0008(17) C12 0.042(3) 0.034(3) 0.059(4) 0.000 0.000(3) 0.000 C13 0.037(3) 0.041(3) 0.049(3) 0.000 -0.008(3) 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 N1 2.224(5) 9_565 ? Cd1 N1 2.224(5) . ? Cd1 N11 2.423(3) 9_565 ? Cd1 N11 2.423(3) . ? Cd1 N11 2.423(3) 3_565 ? Cd1 N11 2.423(3) 11 ? N1 C1 1.154(8) . ? C1 S1 1.598(6) . ? N11 C13 1.331(5) . ? N11 C11 1.341(6) . ? C11 C12 1.370(5) . ? C12 C11 1.370(5) 8_545 ? C13 N11 1.331(5) 8_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 N1 180.0(3) 9_565 . ? N1 Cd1 N11 91.08(14) 9_565 9_565 ? N1 Cd1 N11 88.92(14) . 9_565 ? N1 Cd1 N11 88.92(14) 9_565 . ? N1 Cd1 N11 91.08(14) . . ? N11 Cd1 N11 180.0(2) 9_565 . ? N1 Cd1 N11 91.08(14) 9_565 3_565 ? N1 Cd1 N11 88.92(14) . 3_565 ? N11 Cd1 N11 88.07(17) 9_565 3_565 ? N11 Cd1 N11 91.93(17) . 3_565 ? N1 Cd1 N11 88.92(14) 9_565 11 ? N1 Cd1 N11 91.08(14) . 11 ? N11 Cd1 N11 91.93(17) 9_565 11 ? N11 Cd1 N11 88.07(17) . 11 ? N11 Cd1 N11 180.0 3_565 11 ? C1 N1 Cd1 139.9(5) . . ? N1 C1 S1 178.9(6) . . ? C13 N11 C11 116.2(4) . . ? C13 N11 Cd1 124.0(3) . . ? C11 N11 Cd1 119.3(3) . . ? N11 C11 C12 121.7(4) . . ? C11 C12 C11 117.7(6) . 8_545 ? N11 C13 N11 126.2(6) 8_545 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.21 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.653 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.096 # Attachment 'Compound_2B_Cd(NCSe)2(pyrimidine)_TR108.CIF' data_tr108 _database_code_depnum_ccdc_archive 'CCDC 836236' #TrackingRef 'Compound_2B_Cd(NCSe)2(pyrimidine)_TR108.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'poly[bis(selenocyanato-N)-bis(selenocyanato-Se)-(\m2-pyrimidine-N,N')cadmium(II)]' ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H8 Cd2 N8 Se4' _chemical_formula_sum 'C12 H8 Cd2 N8 Se4' _chemical_formula_weight 804.90 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' Se Se -0.0929 2.2259 '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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 8.6778(3) _cell_length_b 16.7503(5) _cell_length_c 29.2877(8) _cell_angle_alpha 90.00 _cell_angle_beta 92.158(2) _cell_angle_gamma 90.00 _cell_volume 4254.1(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 23689 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 26.8 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1010 _exptl_crystal_size_mid 0.0885 _exptl_crystal_size_min 0.0700 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2944 _exptl_absorpt_coefficient_mu 8.857 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.398 _exptl_absorpt_correction_T_max 0.521 _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 Scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% NONE _diffrn_reflns_number 23168 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0162 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 26.81 _reflns_number_total 4500 _reflns_number_gt 4092 _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)' _computing_publication_material ? _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^)+(0.0231P)^2^+19.9873P] 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 4500 _refine_ls_number_parameters 237 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0371 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0663 _refine_ls_wR_factor_gt 0.0644 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _refine_ls_shift/su_max 0.003 _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 0.51027(3) 0.329453(19) 0.628603(11) 0.03873(8) Uani 1 1 d . . . Cd2 Cd 0.5000 0.0000 0.5000 0.03900(11) Uani 1 2 d S . . Cd3 Cd 0.0000 0.51680(3) 0.7500 0.03938(11) Uani 1 2 d S . . Se1 Se 0.25271(5) 0.23768(3) 0.642174(18) 0.05032(13) Uani 1 1 d . . . C1 C 0.3461(5) 0.1633(3) 0.67851(17) 0.0464(10) Uani 1 1 d . . . N1 N 0.4016(5) 0.1157(3) 0.70178(17) 0.0616(12) Uani 1 1 d . . . Se2 Se 0.66390(7) 0.28824(3) 0.708181(19) 0.05993(15) Uani 1 1 d . . . C2 C 0.8078(6) 0.3646(3) 0.70647(15) 0.0479(11) Uani 1 1 d . . . N2 N 0.8988(6) 0.4143(3) 0.70673(16) 0.0672(13) Uani 1 1 d . . . N3 N 0.3946(5) 0.3660(3) 0.55931(15) 0.0625(12) Uani 1 1 d . . . C3 C 0.3469(5) 0.3927(3) 0.52577(17) 0.0452(10) Uani 1 1 d . . . Se3 Se 0.27901(5) 0.43648(3) 0.472419(16) 0.04826(12) Uani 1 1 d . . . N4 N 0.7142(4) 0.4103(3) 0.60538(14) 0.0504(10) Uani 1 1 d . . . C4 C 0.8411(5) 0.4228(3) 0.59811(16) 0.0475(11) Uani 1 1 d . . . Se4 Se 1.04152(6) 0.43468(5) 0.58657(2) 0.0764(2) Uani 1 1 d . . . N11 N 0.6456(4) 0.2272(2) 0.58619(14) 0.0497(9) Uani 1 1 d . . . N12 N 0.6427(4) 0.1207(3) 0.53266(15) 0.0533(10) Uani 1 1 d . . . C11 C 0.5764(5) 0.1728(3) 0.55977(17) 0.0504(11) Uani 1 1 d . . . H11 H 0.4694 0.1709 0.5603 0.060 Uiso 1 1 calc R . . C12 C 0.7944(6) 0.1259(4) 0.5314(3) 0.081(2) Uani 1 1 d . . . H12 H 0.8462 0.0922 0.5120 0.097 Uiso 1 1 calc R . . C13 C 0.8781(6) 0.1793(4) 0.5577(3) 0.099(3) Uani 1 1 d . . . H13 H 0.9849 0.1821 0.5564 0.119 Uiso 1 1 calc R . . C14 C 0.7989(6) 0.2286(4) 0.5862(2) 0.0709(17) Uani 1 1 d . . . H14 H 0.8532 0.2633 0.6056 0.085 Uiso 1 1 calc R . . N21 N 0.4104(4) 0.4507(2) 0.66282(14) 0.0460(9) Uani 1 1 d . . . N22 N 0.2319(4) 0.5156(2) 0.70922(14) 0.0463(9) Uani 1 1 d . . . C21 C 0.2859(5) 0.4525(3) 0.68791(16) 0.0423(10) Uani 1 1 d . . . H21 H 0.2317 0.4050 0.6907 0.051 Uiso 1 1 calc R . . C22 C 0.3096(7) 0.5825(3) 0.7054(3) 0.0746(19) Uani 1 1 d . . . H22 H 0.2753 0.6281 0.7201 0.090 Uiso 1 1 calc R . . C23 C 0.4397(8) 0.5870(4) 0.6803(3) 0.104(3) Uani 1 1 d . . . H23 H 0.4942 0.6345 0.6779 0.125 Uiso 1 1 calc R . . C24 C 0.4854(7) 0.5196(4) 0.6593(3) 0.083(2) Uani 1 1 d . . . H24 H 0.5725 0.5215 0.6418 0.100 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 0.03354(15) 0.04240(17) 0.04066(17) 0.00096(13) 0.00677(12) 0.00164(12) Cd2 0.0316(2) 0.0504(3) 0.0353(2) -0.00252(19) 0.00535(16) 0.00376(17) Cd3 0.0343(2) 0.0377(2) 0.0466(2) 0.000 0.00744(17) 0.000 Se1 0.0388(2) 0.0528(3) 0.0590(3) 0.0132(2) -0.0026(2) -0.0084(2) C1 0.042(2) 0.046(3) 0.052(3) 0.001(2) 0.011(2) -0.006(2) N1 0.059(3) 0.053(3) 0.072(3) 0.021(2) 0.006(2) 0.006(2) Se2 0.0629(3) 0.0606(3) 0.0553(3) 0.0153(3) -0.0109(2) -0.0187(3) C2 0.057(3) 0.052(3) 0.035(2) -0.002(2) -0.001(2) 0.001(2) N2 0.079(3) 0.068(3) 0.054(3) -0.004(2) -0.006(2) -0.029(3) N3 0.047(2) 0.089(3) 0.051(3) 0.020(2) 0.0017(19) 0.012(2) C3 0.032(2) 0.051(3) 0.053(3) -0.001(2) 0.0070(19) 0.0040(18) Se3 0.0379(2) 0.0687(3) 0.0385(2) 0.0003(2) 0.00515(17) 0.0155(2) N4 0.037(2) 0.064(3) 0.051(2) 0.013(2) 0.0120(17) -0.0008(18) C4 0.044(2) 0.059(3) 0.039(2) 0.011(2) 0.0065(19) 0.004(2) Se4 0.0325(2) 0.1448(6) 0.0523(3) 0.0375(4) 0.0047(2) -0.0029(3) N11 0.0370(19) 0.054(2) 0.058(2) -0.013(2) 0.0038(17) 0.0064(17) N12 0.041(2) 0.059(3) 0.060(3) -0.017(2) 0.0083(18) 0.0005(18) C11 0.038(2) 0.059(3) 0.055(3) -0.012(2) 0.005(2) 0.000(2) C12 0.043(3) 0.079(4) 0.121(6) -0.043(4) 0.025(3) 0.000(3) C13 0.031(3) 0.094(5) 0.173(8) -0.073(5) 0.016(3) 0.000(3) C14 0.039(3) 0.067(4) 0.107(5) -0.036(3) -0.004(3) 0.006(2) N21 0.0392(19) 0.044(2) 0.056(2) 0.0013(18) 0.0166(17) 0.0024(16) N22 0.0395(19) 0.040(2) 0.061(2) -0.0034(18) 0.0163(17) -0.0023(15) C21 0.038(2) 0.040(2) 0.050(3) -0.0001(19) 0.0096(18) -0.0043(17) C22 0.068(3) 0.041(3) 0.118(6) -0.014(3) 0.044(4) -0.005(2) C23 0.088(5) 0.048(3) 0.183(9) -0.017(4) 0.083(5) -0.020(3) C24 0.066(4) 0.053(3) 0.136(6) -0.001(4) 0.061(4) -0.005(3) _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 2.312(4) . ? Cd1 N4 2.349(4) . ? Cd1 N21 2.438(4) . ? Cd1 N11 2.442(4) . ? Cd1 Se2 2.7298(6) . ? Cd1 Se1 2.7538(5) . ? Cd2 N12 2.539(4) 5_656 ? Cd2 N12 2.539(4) . ? Cd2 Se4 2.7723(5) 3_445 ? Cd2 Se4 2.7723(5) 7_656 ? Cd2 Se3 2.7918(4) 3_545 ? Cd2 Se3 2.7918(4) 7_556 ? Cd3 N2 2.289(4) 1_455 ? Cd3 N2 2.289(4) 2_656 ? Cd3 N1 2.319(4) 4_556 ? Cd3 N1 2.319(4) 3_455 ? Cd3 N22 2.379(4) 2_556 ? Cd3 N22 2.379(4) . ? Se1 C1 1.810(5) . ? C1 N1 1.143(6) . ? N1 Cd3 2.319(4) 3_545 ? Se2 C2 1.789(5) . ? C2 N2 1.148(6) . ? N2 Cd3 2.289(4) 1_655 ? N3 C3 1.143(6) . ? C3 Se3 1.805(5) . ? Se3 Cd2 2.7918(4) 3_455 ? N4 C4 1.149(6) . ? C4 Se4 1.795(5) . ? Se4 Cd2 2.7723(5) 3 ? N11 C11 1.325(6) . ? N11 C14 1.331(6) . ? N12 C12 1.321(6) . ? N12 C11 1.325(6) . ? C12 C13 1.371(9) . ? C13 C14 1.374(8) . ? N21 C21 1.330(5) . ? N21 C24 1.331(7) . ? N22 C22 1.315(6) . ? N22 C21 1.322(6) . ? C22 C23 1.371(8) . ? C23 C24 1.353(8) . ? 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 N4 84.28(15) . . ? N3 Cd1 N21 89.48(16) . . ? N4 Cd1 N21 85.53(13) . . ? N3 Cd1 N11 86.58(16) . . ? N4 Cd1 N11 82.83(14) . . ? N21 Cd1 N11 168.03(13) . . ? N3 Cd1 Se2 176.50(11) . . ? N4 Cd1 Se2 92.52(10) . . ? N21 Cd1 Se2 91.68(10) . . ? N11 Cd1 Se2 91.62(10) . . ? N3 Cd1 Se1 86.93(12) . . ? N4 Cd1 Se1 171.08(10) . . ? N21 Cd1 Se1 95.90(9) . . ? N11 Cd1 Se1 95.18(10) . . ? Se2 Cd1 Se1 96.231(18) . . ? N12 Cd2 N12 180.00(12) 5_656 . ? N12 Cd2 Se4 94.30(11) 5_656 3_445 ? N12 Cd2 Se4 85.70(11) . 3_445 ? N12 Cd2 Se4 85.70(11) 5_656 7_656 ? N12 Cd2 Se4 94.30(11) . 7_656 ? Se4 Cd2 Se4 180.0 3_445 7_656 ? N12 Cd2 Se3 90.19(9) 5_656 3_545 ? N12 Cd2 Se3 89.81(9) . 3_545 ? Se4 Cd2 Se3 91.714(16) 3_445 3_545 ? Se4 Cd2 Se3 88.285(16) 7_656 3_545 ? N12 Cd2 Se3 89.81(9) 5_656 7_556 ? N12 Cd2 Se3 90.19(9) . 7_556 ? Se4 Cd2 Se3 88.286(16) 3_445 7_556 ? Se4 Cd2 Se3 91.715(16) 7_656 7_556 ? Se3 Cd2 Se3 180.000(18) 3_545 7_556 ? N2 Cd3 N2 82.8(3) 1_455 2_656 ? N2 Cd3 N1 176.11(18) 1_455 4_556 ? N2 Cd3 N1 94.23(18) 2_656 4_556 ? N2 Cd3 N1 94.23(18) 1_455 3_455 ? N2 Cd3 N1 176.11(17) 2_656 3_455 ? N1 Cd3 N1 88.8(3) 4_556 3_455 ? N2 Cd3 N22 87.57(16) 1_455 2_556 ? N2 Cd3 N22 91.71(16) 2_656 2_556 ? N1 Cd3 N22 89.96(15) 4_556 2_556 ? N1 Cd3 N22 90.72(15) 3_455 2_556 ? N2 Cd3 N22 91.71(16) 1_455 . ? N2 Cd3 N22 87.57(16) 2_656 . ? N1 Cd3 N22 90.72(15) 4_556 . ? N1 Cd3 N22 89.96(15) 3_455 . ? N22 Cd3 N22 179.05(19) 2_556 . ? C1 Se1 Cd1 96.96(14) . . ? N1 C1 Se1 178.3(4) . . ? C1 N1 Cd3 176.7(4) . 3_545 ? C2 Se2 Cd1 96.56(15) . . ? N2 C2 Se2 177.8(5) . . ? C2 N2 Cd3 142.9(4) . 1_655 ? C3 N3 Cd1 171.6(5) . . ? N3 C3 Se3 177.8(4) . . ? C3 Se3 Cd2 99.37(13) . 3_455 ? C4 N4 Cd1 153.7(4) . . ? N4 C4 Se4 175.9(5) . . ? C4 Se4 Cd2 97.04(15) . 3 ? C11 N11 C14 116.3(4) . . ? C11 N11 Cd1 124.3(3) . . ? C14 N11 Cd1 119.2(3) . . ? C12 N12 C11 115.4(5) . . ? C12 N12 Cd2 121.0(4) . . ? C11 N12 Cd2 122.2(3) . . ? N11 C11 N12 127.3(4) . . ? N12 C12 C13 122.4(5) . . ? C12 C13 C14 117.8(5) . . ? N11 C14 C13 120.8(5) . . ? C21 N21 C24 115.6(4) . . ? C21 N21 Cd1 123.7(3) . . ? C24 N21 Cd1 120.6(3) . . ? C22 N22 C21 116.7(4) . . ? C22 N22 Cd3 118.8(3) . . ? C21 N22 Cd3 124.4(3) . . ? N22 C21 N21 126.1(4) . . ? N22 C22 C23 121.8(5) . . ? C24 C23 C22 117.3(5) . . ? N21 C24 C23 122.4(5) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.81 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.332 _refine_diff_density_min -1.074 _refine_diff_density_rms 0.088 # Attachment 'Compound_2A_Cd(NCSe)2(pyrimidine)2_TR185.CIF' data_tr185 _database_code_depnum_ccdc_archive 'CCDC 836237' #TrackingRef 'Compound_2A_Cd(NCSe)2(pyrimidine)2_TR185.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'poly[bis(\m2-selenocyanato-N)-bis(\m2-selenocyanato-Se)-bis(pyridine-N)cadmium(II)]' ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H8 Cd N6 Se2' _chemical_formula_sum 'C10 H8 Cd N6 Se2' _chemical_formula_weight 482.54 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' Se Se -0.0929 2.2259 '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_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.566(2) _cell_length_b 6.0220(10) _cell_length_c 13.829(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.07(3) _cell_angle_gamma 90.00 _cell_volume 712.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5549 _cell_measurement_theta_min 6.15 _cell_measurement_theta_max 28.05 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4644 _exptl_crystal_size_mid 0.3558 _exptl_crystal_size_min 0.2537 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.248 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 452 _exptl_absorpt_coefficient_mu 6.632 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.0441 _exptl_absorpt_correction_T_max 0.1144 _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-1' _diffrn_measurement_method 'Phi Scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% NONE _diffrn_reflns_number 5395 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 27.98 _reflns_number_total 1667 _reflns_number_gt 1347 _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)' _computing_publication_material ? _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^)+(0.0377P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1667 _refine_ls_number_parameters 88 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0374 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0666 _refine_ls_wR_factor_gt 0.0635 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 0.0000 -0.5000 -0.5000 0.03594(11) Uani 1 2 d S . . N1 N -0.1016(4) -0.8168(5) -0.5749(2) 0.0406(6) Uani 1 1 d . . . C1 C -0.0943(4) -0.9863(5) -0.6117(2) 0.0338(6) Uani 1 1 d . . . Se1 Se -0.08010(4) -1.25311(6) -0.67067(2) 0.04306(12) Uani 1 1 d . . . N11 N -0.2449(3) -0.4307(5) -0.43171(18) 0.0369(6) Uani 1 1 d . . . N12 N -0.4345(4) -0.1749(6) -0.3794(3) 0.0586(9) Uani 1 1 d . . . C11 C -0.2985(5) -0.2286(6) -0.4167(3) 0.0479(8) Uani 1 1 d . . . H11 H -0.2345 -0.1114 -0.4340 0.057 Uiso 1 1 calc R . . C12 C -0.5238(5) -0.3445(8) -0.3551(3) 0.0544(10) Uani 1 1 d . . . H12 H -0.6200 -0.3149 -0.3287 0.065 Uiso 1 1 calc R . . C13 C -0.4804(5) -0.5610(8) -0.3672(3) 0.0522(10) Uani 1 1 d . . . H13 H -0.5447 -0.6778 -0.3498 0.063 Uiso 1 1 calc R . . C14 C -0.3381(5) -0.5977(6) -0.4061(3) 0.0464(8) Uani 1 1 d . . . H14 H -0.3050 -0.7431 -0.4151 0.056 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 0.03859(18) 0.02658(15) 0.04335(17) -0.00418(13) 0.01108(13) 0.00129(14) N1 0.0499(17) 0.0298(13) 0.0420(14) -0.0037(11) 0.0001(12) 0.0017(12) C1 0.0342(15) 0.0358(15) 0.0317(12) 0.0052(12) 0.0040(11) -0.0011(13) Se1 0.0616(3) 0.03308(18) 0.03445(17) -0.00573(12) 0.00110(15) 0.00246(15) N11 0.0394(15) 0.0332(13) 0.0388(13) -0.0007(10) 0.0098(12) 0.0029(11) N12 0.052(2) 0.056(2) 0.069(2) -0.0091(17) 0.0155(17) 0.0160(17) C11 0.050(2) 0.0382(18) 0.057(2) -0.0021(15) 0.0156(17) 0.0045(16) C12 0.038(2) 0.079(3) 0.0459(19) -0.0003(18) 0.0087(16) 0.007(2) C13 0.045(2) 0.065(3) 0.0464(18) 0.0101(17) 0.0072(16) -0.0092(18) C14 0.050(2) 0.0377(17) 0.0516(18) 0.0060(15) 0.0090(16) -0.0019(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N1 2.325(3) . ? Cd1 N1 2.325(3) 3_544 ? Cd1 N11 2.368(3) . ? Cd1 N11 2.368(3) 3_544 ? Cd1 Se1 2.8521(7) 3_534 ? Cd1 Se1 2.8521(7) 1_565 ? N1 C1 1.143(4) . ? C1 Se1 1.808(3) . ? Se1 Cd1 2.8521(7) 1_545 ? N11 C11 1.320(4) . ? N11 C14 1.339(5) . ? N12 C12 1.326(6) . ? N12 C11 1.331(5) . ? C12 C13 1.368(6) . ? C13 C14 1.369(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 N1 180.0 . 3_544 ? N1 Cd1 N11 89.98(11) . . ? N1 Cd1 N11 90.02(11) 3_544 . ? N1 Cd1 N11 90.02(11) . 3_544 ? N1 Cd1 N11 89.98(11) 3_544 3_544 ? N11 Cd1 N11 180.0 . 3_544 ? N1 Cd1 Se1 90.92(7) . 3_534 ? N1 Cd1 Se1 89.08(7) 3_544 3_534 ? N11 Cd1 Se1 87.24(7) . 3_534 ? N11 Cd1 Se1 92.76(7) 3_544 3_534 ? N1 Cd1 Se1 89.08(7) . 1_565 ? N1 Cd1 Se1 90.92(7) 3_544 1_565 ? N11 Cd1 Se1 92.76(7) . 1_565 ? N11 Cd1 Se1 87.24(7) 3_544 1_565 ? Se1 Cd1 Se1 180.0 3_534 1_565 ? C1 N1 Cd1 154.8(3) . . ? N1 C1 Se1 179.2(3) . . ? C1 Se1 Cd1 96.21(9) . 1_545 ? C11 N11 C14 115.9(3) . . ? C11 N11 Cd1 122.9(2) . . ? C14 N11 Cd1 121.2(2) . . ? C12 N12 C11 115.6(4) . . ? N11 C11 N12 126.8(4) . . ? N12 C12 C13 122.8(4) . . ? C12 C13 C14 116.9(4) . . ? N11 C14 C13 122.0(4) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.98 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.441 _refine_diff_density_min -0.719 _refine_diff_density_rms 0.103