# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1585 data_Codca2apymLT _audit_creation_method SHELXL-97 _chemical_name_systematic ; cobalt bis(dicyanamide) 2-amino-pyrimidine ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Co(dca)2(apym) _chemical_formula_sum 'C8 H5 Co N9' _chemical_formula_weight 286.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Co' 'Co' 0.3494 0.9721 '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' '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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(2)/mbc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z+1/2' 'y, -x, z+1/2' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z-1/2' '-y, x, -z-1/2' 'x-1/2, -y-1/2, z' '-x-1/2, y-1/2, z' '-y-1/2, -x-1/2, z-1/2' 'y-1/2, x-1/2, z-1/2' _cell_length_a 17.1243(2) _cell_length_b 17.1243(2) _cell_length_c 7.38160(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2164.59(5) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description acicular _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.756 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 1.582 _exptl_absorpt_correction_type Face-indexed _exptl_absorpt_correction_T_min 0.791 _exptl_absorpt_correction_T_max 0.880 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius KappaCCD' _diffrn_measurement_method Phi-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31921 _diffrn_reflns_av_R_equivalents 0.050 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 30.03 _reflns_number_total 1695 _reflns_number_gt 1471 _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^)+(0.0245P)^2^+1.7960P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1695 _refine_ls_number_parameters 102 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0279 _refine_ls_wR_factor_ref 0.0626 _refine_ls_wR_factor_gt 0.0579 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _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 Co1 Co 0.481548(16) 0.299981(15) 0.0000 0.00810(8) Uani 1 2 d S . . N1 N 0.54639(7) 0.35468(7) -0.20733(17) 0.0138(3) Uani 1 1 d . . . N2 N 0.59496(11) 0.40523(11) -0.5000 0.0126(4) Uani 1 2 d S . . N3 N 0.41114(7) 0.25500(7) -0.20628(17) 0.0138(3) Uani 1 1 d . . . N4 N 0.35394(11) 0.21923(12) -0.5000 0.0168(4) Uani 1 2 d S . . N5 N 0.55845(10) 0.20081(10) 0.0000 0.0121(3) Uani 1 2 d S . . N6 N 0.59111(12) 0.06464(11) 0.0000 0.0222(4) Uani 1 2 d S . . N7 N 0.46327(12) 0.10421(12) 0.0000 0.0198(4) Uani 1 2 d S . . H1 H 0.4491(17) 0.0574(18) 0.0000 0.024 Uiso 1 2 d S . . H2 H 0.4287(18) 0.1389(18) -0.019(9) 0.024 Uiso 0.50 1 d P . . C1 C 0.56684(8) 0.37695(8) -0.34689(19) 0.0110(3) Uani 1 1 d . . . C2 C 0.38666(8) 0.23989(8) -0.34758(19) 0.0107(3) Uani 1 1 d . . . C3 C 0.63512(13) 0.21714(13) 0.0000 0.0156(4) Uani 1 2 d S . . H3 H 0.6507 0.2704 0.0000 0.019 Uiso 1 2 calc SR . . C4 C 0.69215(13) 0.16069(14) 0.0000 0.0217(5) Uani 1 2 d S . . H4 H 0.7462 0.1733 0.0000 0.026 Uiso 1 2 calc SR . . C5 C 0.66594(15) 0.08424(14) 0.0000 0.0262(5) Uani 1 2 d S . . H5 H 0.7037 0.0436 0.0000 0.031 Uiso 1 2 calc SR . . C6 C 0.53848(13) 0.12393(12) 0.0000 0.0145(4) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.00995(14) 0.00874(14) 0.00561(13) 0.000 0.000 -0.00006(10) N1 0.0146(6) 0.0153(6) 0.0114(6) 0.0007(5) 0.0017(5) -0.0024(5) N2 0.0149(8) 0.0165(9) 0.0065(8) 0.000 0.000 -0.0064(7) N3 0.0158(6) 0.0154(6) 0.0104(6) 0.0002(5) 0.0001(5) -0.0021(5) N4 0.0186(9) 0.0234(10) 0.0084(8) 0.000 0.000 -0.0091(8) N5 0.0123(8) 0.0107(8) 0.0134(8) 0.000 0.000 -0.0001(7) N6 0.0183(9) 0.0111(9) 0.0371(12) 0.000 0.000 0.0027(7) N7 0.0154(9) 0.0084(8) 0.0356(12) 0.000 0.000 -0.0006(7) C1 0.0103(6) 0.0103(6) 0.0122(7) -0.0022(5) -0.0010(5) -0.0009(5) C2 0.0116(6) 0.0099(6) 0.0105(7) 0.0016(5) 0.0027(5) -0.0018(5) C3 0.0137(10) 0.0150(10) 0.0182(11) 0.000 0.000 -0.0001(8) C4 0.0128(10) 0.0199(11) 0.0325(13) 0.000 0.000 0.0028(8) C5 0.0175(11) 0.0178(11) 0.0433(15) 0.000 0.000 0.0078(9) C6 0.0161(10) 0.0118(10) 0.0155(10) 0.000 0.000 0.0009(8) _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 Co1 N3 2.0893(13) 10 ? Co1 N3 2.0893(13) . ? Co1 N1 2.1101(12) . ? Co1 N1 2.1102(12) 10 ? Co1 N5 2.1490(18) . ? Co1 N2 2.2237(18) 11_565 ? N1 C1 1.1529(19) . ? N2 C1 1.3205(17) 10_554 ? N2 C1 1.3205(17) . ? N2 Co1 2.2236(18) 3_654 ? N3 C2 1.1535(19) . ? N4 C2 1.3058(17) 10_554 ? N4 C2 1.3058(17) . ? N5 C3 1.342(3) . ? N5 C6 1.360(3) . ? N6 C5 1.325(3) . ? N6 C6 1.358(3) . ? N7 C6 1.332(3) . ? C3 C4 1.374(3) . ? C4 C5 1.384(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 N3 Co1 N3 93.57(7) 10 . ? N3 Co1 N1 174.79(5) 10 . ? N3 Co1 N1 86.49(5) . . ? N3 Co1 N1 86.49(5) 10 10 ? N3 Co1 N1 174.79(5) . 10 ? N1 Co1 N1 92.98(7) . 10 ? N3 Co1 N5 93.57(5) 10 . ? N3 Co1 N5 93.57(5) . . ? N1 Co1 N5 91.62(5) . . ? N1 Co1 N5 91.62(5) 10 . ? N3 Co1 N2 87.66(5) 10 11_565 ? N3 Co1 N2 87.66(5) . 11_565 ? N1 Co1 N2 87.14(5) . 11_565 ? N1 Co1 N2 87.14(5) 10 11_565 ? N5 Co1 N2 178.21(7) . 11_565 ? C1 N1 Co1 162.69(12) . . ? C1 N2 C1 117.71(17) 10_554 . ? C1 N2 Co1 120.70(9) 10_554 3_654 ? C1 N2 Co1 120.70(9) . 3_654 ? C2 N3 Co1 162.06(12) . . ? C2 N4 C2 119.01(18) 10_554 . ? C3 N5 C6 116.58(19) . . ? C3 N5 Co1 115.77(14) . . ? C6 N5 Co1 127.65(14) . . ? C5 N6 C6 116.9(2) . . ? N1 C1 N2 175.40(16) . . ? N3 C2 N4 174.78(16) . . ? N5 C3 C4 123.3(2) . . ? C3 C4 C5 115.8(2) . . ? N6 C5 C4 123.6(2) . . ? N7 C6 N6 116.9(2) . . ? N7 C6 N5 119.2(2) . . ? N6 C6 N5 123.8(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.305 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.090 _publ_contact_author ; Prof. K.S. Murray Department of Chemistry Monash University Clayton, Vic. 3168 AUSTRALIA ; _publ_contact_author_phone ' +61 3 9905 4512 ' _publ_contact_author_fax ' +61 3 9905 4597 ' _publ_contact_author_email ' Keith.S.Murray@sci.monash.edu.au ' loop_ _publ_author_name _publ_author_address ' Murray, Keith S. ' ; Department of Chemistry Monash University Clayton, Vic. 3168 AUSTRALIA ; _publ_section_title ; Infinite molecular tubes: structure and magnetism of M(dca)2(apym), M = Co, Ni, apym = 2-aminopyrimidine, dca = dicyanamide, N(CN)2- ; #=END data_Codca2apymRT _audit_creation_method SHELXL-97 _chemical_name_systematic ; cobalt bis(dicyanamide) 2-amino-pyrimidine ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Co(dca)2(apym) _chemical_formula_sum 'C8 H5 Co N9' _chemical_formula_weight 286.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Co' 'Co' 0.3494 0.9721 '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' '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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(2)/mbc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z+1/2' 'y, -x, z+1/2' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z-1/2' '-y, x, -z-1/2' 'x-1/2, -y-1/2, z' '-x-1/2, y-1/2, z' '-y-1/2, -x-1/2, z-1/2' 'y-1/2, x-1/2, z-1/2' _cell_length_a 17.2018(4) _cell_length_b 17.2018(4) _cell_length_c 7.3742(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2182.04(9) _cell_formula_units_Z 8 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description acicular _exptl_crystal_colour red _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.742 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 1.570 _exptl_absorpt_correction_type Face-indexed _exptl_absorpt_correction_T_min 0.846 _exptl_absorpt_correction_T_max 0.939 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Nonius KappaCCD' _diffrn_measurement_method Phi-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20522 _diffrn_reflns_av_R_equivalents 0.125 _diffrn_reflns_av_sigmaI/netI 0.0748 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 30.03 _reflns_number_total 1718 _reflns_number_gt 1297 _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^)+(0.0112P)^2^+3.1942P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1718 _refine_ls_number_parameters 97 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1142 _refine_ls_R_factor_gt 0.0706 _refine_ls_wR_factor_ref 0.0847 _refine_ls_wR_factor_gt 0.0781 _refine_ls_goodness_of_fit_ref 1.198 _refine_ls_restrained_S_all 1.198 _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 Co1 Co 0.48106(3) 0.30020(3) 0.0000 0.01466(15) Uani 1 2 d S . . N1 N 0.54572(14) 0.35486(13) -0.2074(3) 0.0251(5) Uani 1 1 d . . . N2 N 0.59410(19) 0.40453(19) -0.5000 0.0222(7) Uani 1 2 d S . . N3 N 0.41068(14) 0.25576(14) -0.2056(3) 0.0253(6) Uani 1 1 d . . . N4 N 0.3549(2) 0.2208(2) -0.5000 0.0330(9) Uani 1 2 d S . . N5 N 0.55732(18) 0.20048(18) 0.0000 0.0212(7) Uani 1 2 d S . . N6 N 0.5902(2) 0.0657(2) 0.0000 0.0407(10) Uani 1 2 d S . . N7 N 0.4632(2) 0.1050(2) 0.0000 0.0412(11) Uani 1 2 d S . . H1 H 0.4498 0.0568 0.0000 0.049 Uiso 1 2 calc SR . . H2 H 0.4283 0.1407 0.0000 0.049 Uiso 1 2 calc SR . . C1 C 0.56588(15) 0.37670(15) -0.3467(4) 0.0188(6) Uani 1 1 d . . . C2 C 0.38704(15) 0.24127(15) -0.3470(4) 0.0190(6) Uani 1 1 d . . . C3 C 0.6341(2) 0.2171(2) 0.0000 0.0308(10) Uani 1 2 d S . . H3 H 0.6495 0.2689 0.0000 0.037 Uiso 1 2 calc SR . . C4 C 0.6897(3) 0.1608(3) 0.0000 0.0422(13) Uani 1 2 d S . . H4 H 0.7424 0.1730 0.0000 0.051 Uiso 1 2 calc SR . . C5 C 0.6642(3) 0.0855(3) 0.0000 0.0499(14) Uani 1 2 d S . . H5 H 0.7012 0.0461 0.0000 0.060 Uiso 1 2 calc SR . . C6 C 0.5382(2) 0.1242(2) 0.0000 0.0270(10) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0191(3) 0.0163(3) 0.0086(2) 0.000 0.000 0.0001(2) N1 0.0287(13) 0.0279(13) 0.0188(12) 0.0034(11) 0.0051(11) -0.0029(11) N2 0.0269(19) 0.0301(19) 0.0097(15) 0.000 0.000 -0.0127(15) N3 0.0303(13) 0.0298(13) 0.0158(12) -0.0002(11) -0.0009(11) -0.0052(11) N4 0.038(2) 0.050(2) 0.0114(17) 0.000 0.000 -0.0237(19) N5 0.0208(17) 0.0169(16) 0.0258(19) 0.000 0.000 -0.0014(14) N6 0.040(2) 0.022(2) 0.060(3) 0.000 0.000 0.0078(18) N7 0.029(2) 0.0166(18) 0.078(3) 0.000 0.000 0.0001(16) C1 0.0174(13) 0.0194(14) 0.0196(15) -0.0022(12) -0.0016(12) -0.0042(11) C2 0.0209(13) 0.0177(13) 0.0183(15) 0.0022(12) 0.0055(12) -0.0030(11) C3 0.025(2) 0.024(2) 0.043(3) 0.000 0.000 -0.0008(19) C4 0.023(2) 0.040(3) 0.064(4) 0.000 0.000 0.005(2) C5 0.033(3) 0.039(3) 0.078(4) 0.000 0.000 0.017(2) C6 0.029(2) 0.021(2) 0.030(2) 0.000 0.000 0.0030(18) _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 Co1 N3 2.085(2) . ? Co1 N3 2.085(2) 10 ? Co1 N1 2.112(2) . ? Co1 N1 2.112(2) 10 ? Co1 N5 2.160(3) . ? Co1 N2 2.245(3) 11_565 ? N1 C1 1.147(3) . ? N2 C1 1.320(3) . ? N2 C1 1.320(3) 10_554 ? N2 Co1 2.245(3) 3_654 ? N3 C2 1.146(3) . ? N4 C2 1.305(3) . ? N4 C2 1.305(3) 10_554 ? N5 C3 1.351(5) . ? N5 C6 1.353(5) . ? N6 C5 1.318(6) . ? N6 C6 1.347(5) . ? N7 C6 1.331(5) . ? C3 C4 1.361(6) . ? C4 C5 1.368(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 N3 Co1 N3 93.27(13) . 10 ? N3 Co1 N1 86.70(9) . . ? N3 Co1 N1 174.54(10) 10 . ? N3 Co1 N1 174.54(10) . 10 ? N3 Co1 N1 86.70(9) 10 10 ? N1 Co1 N1 92.81(13) . 10 ? N3 Co1 N5 93.52(9) . . ? N3 Co1 N5 93.52(9) 10 . ? N1 Co1 N5 91.93(9) . . ? N1 Co1 N5 91.93(9) 10 . ? N3 Co1 N2 87.51(9) . 11_565 ? N3 Co1 N2 87.50(9) 10 11_565 ? N1 Co1 N2 87.04(9) . 11_565 ? N1 Co1 N2 87.04(9) 10 11_565 ? N5 Co1 N2 178.50(13) . 11_565 ? C1 N1 Co1 162.4(2) . . ? C1 N2 C1 117.8(3) . 10_554 ? C1 N2 Co1 120.69(16) . 3_654 ? C1 N2 Co1 120.69(16) 10_554 3_654 ? C2 N3 Co1 161.2(2) . . ? C2 N4 C2 119.7(3) . 10_554 ? C3 N5 C6 116.3(3) . . ? C3 N5 Co1 115.2(3) . . ? C6 N5 Co1 128.5(3) . . ? C5 N6 C6 116.7(4) . . ? N1 C1 N2 175.2(3) . . ? N3 C2 N4 174.4(3) . . ? N5 C3 C4 122.5(4) . . ? C3 C4 C5 116.6(4) . . ? N6 C5 C4 123.7(4) . . ? N7 C6 N6 117.3(4) . . ? N7 C6 N5 118.5(4) . . ? N6 C6 N5 124.2(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.726 _refine_diff_density_min -0.708 _refine_diff_density_rms 0.100 _publ_contact_author ; Prof. K.S. Murray Department of Chemistry Monash University Clayton, Vic. 3168 AUSTRALIA ; _publ_contact_author_phone ' +61 3 9905 4512 ' _publ_contact_author_fax ' +61 3 9905 4597 ' _publ_contact_author_email ' Keith.S.Murray@sci.monash.edu.au ' loop_ _publ_author_name _publ_author_address ' Murray, Keith S. ' ; Department of Chemistry Monash University Clayton, Vic. 3168 AUSTRALIA ; _publ_section_title ; Infinite molecular tubes: structure and magnetism of M(dca)2(apym), M = Co, Ni, apym = 2-aminopyrimidine, dca = dicyanamide, N(CN)2- ; #=END data_Nidca2apym _audit_creation_method SHELXL-97 _chemical_name_systematic ; nickel bis(dicyanamide) 2-amino-pyrimidine ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Ni(dca)2(apym) _chemical_formula_sum 'C8 H5 N9 Ni' _chemical_formula_weight 285.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ni' 'Ni' 0.3393 1.1124 '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' '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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(2)/mbc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z+1/2' 'y, -x, z+1/2' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z-1/2' '-y, x, -z-1/2' 'x-1/2, -y-1/2, z' '-x-1/2, y-1/2, z' '-y-1/2, -x-1/2, z-1/2' 'y-1/2, x-1/2, z-1/2' _cell_length_a 17.0863(6) _cell_length_b 17.0863(6) _cell_length_c 7.3099(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2134.06(12) _cell_formula_units_Z 8 _cell_measurement_temperature 297(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description acicular _exptl_crystal_colour blue _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.780 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 1.815 _exptl_absorpt_correction_type Face-indexed _exptl_absorpt_correction_T_min 0.863 _exptl_absorpt_correction_T_max 0.918 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 297(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 'Nonius KappaCCD' _diffrn_measurement_method Phi-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15738 _diffrn_reflns_av_R_equivalents 0.113 _diffrn_reflns_av_sigmaI/netI 0.0719 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 30.03 _reflns_number_total 1653 _reflns_number_gt 1127 _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^)+(0.0335P)^2^+2.6803P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1653 _refine_ls_number_parameters 97 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1013 _refine_ls_R_factor_gt 0.0530 _refine_ls_wR_factor_ref 0.1010 _refine_ls_wR_factor_gt 0.0867 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _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 Ni1 Ni 0.48123(3) 0.30138(3) 0.0000 0.01773(17) Uani 1 2 d S . . N1 N 0.54569(16) 0.35482(15) -0.2054(3) 0.0268(6) Uani 1 1 d . . . N2 N 0.5942(2) 0.4059(2) -0.5000 0.0248(8) Uani 1 2 d S . . N3 N 0.41195(16) 0.25686(15) -0.2037(3) 0.0271(6) Uani 1 1 d . . . N4 N 0.3559(2) 0.2202(3) -0.5000 0.0346(10) Uani 1 2 d S . . N5 N 0.5572(2) 0.2028(2) 0.0000 0.0217(8) Uani 1 2 d S . . N6 N 0.5904(2) 0.0668(2) 0.0000 0.0387(11) Uani 1 2 d S . . N7 N 0.4626(2) 0.1059(2) 0.0000 0.0404(11) Uani 1 2 d S . . H1 H 0.4494 0.0573 0.0000 0.048 Uiso 1 2 calc SR . . H2 H 0.4271 0.1416 0.0000 0.048 Uiso 1 2 calc SR . . C1 C 0.56624(17) 0.37754(18) -0.3457(4) 0.0218(7) Uani 1 1 d . . . C2 C 0.38838(17) 0.24151(17) -0.3460(4) 0.0211(7) Uani 1 1 d . . . C3 C 0.6339(3) 0.2191(3) 0.0000 0.0301(11) Uani 1 2 d S . . H3 H 0.6494 0.2713 0.0000 0.036 Uiso 1 2 calc SR . . C4 C 0.6905(3) 0.1627(3) 0.0000 0.0409(13) Uani 1 2 d S . . H4 H 0.7435 0.1750 0.0000 0.049 Uiso 1 2 calc SR . . C5 C 0.6645(4) 0.0870(3) 0.0000 0.0498(15) Uani 1 2 d S . . H5 H 0.7017 0.0472 0.0000 0.060 Uiso 1 2 calc SR . . C6 C 0.5378(3) 0.1258(3) 0.0000 0.0285(10) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0217(3) 0.0204(3) 0.0111(3) 0.000 0.000 -0.0005(2) N1 0.0301(15) 0.0296(15) 0.0209(13) 0.0034(11) 0.0053(11) -0.0044(12) N2 0.029(2) 0.034(2) 0.0118(16) 0.000 0.000 -0.0123(17) N3 0.0332(16) 0.0325(16) 0.0155(13) -0.0013(11) -0.0029(12) -0.0052(12) N4 0.038(2) 0.050(3) 0.0159(19) 0.000 0.000 -0.020(2) N5 0.023(2) 0.0194(19) 0.0231(19) 0.000 0.000 0.0010(16) N6 0.034(3) 0.022(2) 0.060(3) 0.000 0.000 0.0059(19) N7 0.030(2) 0.018(2) 0.073(3) 0.000 0.000 -0.0022(18) C1 0.0224(16) 0.0233(16) 0.0198(16) -0.0027(12) 0.0001(12) -0.0006(13) C2 0.0232(16) 0.0197(15) 0.0203(16) 0.0032(12) 0.0048(12) -0.0013(13) C3 0.025(3) 0.026(3) 0.039(3) 0.000 0.000 0.000(2) C4 0.022(3) 0.038(3) 0.062(4) 0.000 0.000 0.005(2) C5 0.037(3) 0.040(3) 0.072(4) 0.000 0.000 0.018(3) C6 0.029(3) 0.026(3) 0.030(2) 0.000 0.000 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N3 2.048(3) . ? Ni1 N3 2.048(3) 10 ? Ni1 N1 2.074(3) 10 ? Ni1 N1 2.074(3) . ? Ni1 N5 2.126(4) . ? Ni1 N2 2.201(4) 11_565 ? N1 C1 1.151(4) . ? N2 C1 1.317(3) 10_554 ? N2 C1 1.317(3) . ? N2 Ni1 2.201(4) 3_654 ? N3 C2 1.146(4) . ? N4 C2 1.306(4) 10_554 ? N4 C2 1.306(4) . ? N5 C3 1.341(6) . ? N5 C6 1.358(6) . ? N6 C5 1.312(7) . ? N6 C6 1.350(6) . ? N7 C6 1.329(6) . ? C3 C4 1.365(7) . ? C4 C5 1.368(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 Ni1 N3 93.23(15) . 10 ? N3 Ni1 N1 175.21(11) . 10 ? N3 Ni1 N1 86.81(10) 10 10 ? N3 Ni1 N1 86.81(10) . . ? N3 Ni1 N1 175.21(11) 10 . ? N1 Ni1 N1 92.76(15) 10 . ? N3 Ni1 N5 93.36(10) . . ? N3 Ni1 N5 93.36(10) 10 . ? N1 Ni1 N5 91.42(10) 10 . ? N1 Ni1 N5 91.42(10) . . ? N3 Ni1 N2 87.88(10) . 11_565 ? N3 Ni1 N2 87.88(10) 10 11_565 ? N1 Ni1 N2 87.33(10) 10 11_565 ? N1 Ni1 N2 87.34(10) . 11_565 ? N5 Ni1 N2 178.19(14) . 11_565 ? C1 N1 Ni1 162.8(3) . . ? C1 N2 C1 117.9(4) 10_554 . ? C1 N2 Ni1 120.59(18) 10_554 3_654 ? C1 N2 Ni1 120.59(18) . 3_654 ? C2 N3 Ni1 161.4(3) . . ? C2 N4 C2 119.0(4) 10_554 . ? C3 N5 C6 116.1(4) . . ? C3 N5 Ni1 115.6(3) . . ? C6 N5 Ni1 128.3(3) . . ? C5 N6 C6 116.5(4) . . ? N1 C1 N2 175.8(3) . . ? N3 C2 N4 174.3(3) . . ? N5 C3 C4 123.1(5) . . ? C3 C4 C5 115.9(5) . . ? N6 C5 C4 124.2(5) . . ? N7 C6 N6 116.9(4) . . ? N7 C6 N5 118.9(4) . . ? N6 C6 N5 124.2(4) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.500 _refine_diff_density_min -0.933 _refine_diff_density_rms 0.127 _publ_contact_author ; Prof. K.S. Murray Department of Chemistry Monash University Clayton, Vic. 3168 AUSTRALIA ; _publ_contact_author_phone ' +61 3 9905 4512 ' _publ_contact_author_fax ' +61 3 9905 4597 ' _publ_contact_author_email ' Keith.S.Murray@sci.monash.edu.au ' loop_ _publ_author_name _publ_author_address ' Murray, Keith S. ' ; Department of Chemistry Monash University Clayton, Vic. 3168 AUSTRALIA ; _publ_section_title ; Infinite molecular tubes: structure and magnetism of M(dca)2(apym), M = Co, Ni, apym = 2-aminopyrimidine, dca = dicyanamide, N(CN)2- ; #=END