# Copyright The Royal Society of Chemistry, 1999 # CCDC Number :182/1120 data_alphaCo(dca)2 #----------------------------------------------------------------------- _audit_creation_date 'Tue Oct 13 14:58:16 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #----------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #----------------------------------------------------------------------- _cell_length_a 7.0433(2) _cell_length_b 5.9748(3) _cell_length_c 7.4039(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 311.57(2) _cell_formula_units_Z 2 _cell_measurement_temperature 123.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #----------------------------------------------------------------------- _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n n m ' _symmetry_Int_Tables_number 58 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, +z' '1/2+x,1/2-y,1/2-z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' ' +x, +y, -z' '1/2-x,1/2+y,1/2+z' '1/2+x,1/2-y,1/2+z' #----------------------------------------------------------------------- _exptl_crystal_description 'acicular' _exptl_crystal_colour 'pink' _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.030 _exptl_crystal_size_min 0.030 _exptl_crystal_density_diffrn 2.036 _exptl_crystal_density_meas ? _chemical_formula_weight 191.02 _chemical_formula_analytical ? _chemical_formula_sum 'C4 Co N6 ' _chemical_formula_moiety 'C4 Co N6 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 186.00 _exptl_absorpt_coefficient_mu 2.681 _exptl_absorpt_correction_type none #----------------------------------------------------------------------- _diffrn_special_details none _diffrn_ambient_temperature 123.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD' _diffrn_measurement_device 'Nonius KappaCCD diffractometer' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 4200 _reflns_number_total 473 _reflns_number_observed 336 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 0.047 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 28.26 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #----------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Co 0 2 0.349 0.972 'International Tables' C 0 8 0.003 0.002 'International Tables' N 0 12 0.006 0.003 'International Tables' #----------------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Co(1) 0.0000 0.0000 0.0000 0.0111(2) Uij ? ? N(1) -0.0953(3) 0.2089(3) 0.2079(3) 0.0153(6) Uij ? ? N(2) 0.2725(4) 0.1620(5) 0.0000 0.0146(8) Uij ? ? C(1) -0.1519(3) 0.2644(4) 0.3474(4) 0.0147(6) Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co(1) 0.0101(3) 0.0158(4) 0.0073(3) -0.0003(3) 0.0000 0.0000 N(1) 0.015(1) 0.020(1) 0.010(1) 0.0018(9) -0.0006(8) -0.0015(9) N(2) 0.015(1) 0.024(2) 0.005(1) -0.008(1) 0.0000 0.0000 C(1) 0.011(1) 0.016(1) 0.017(1) -0.0006(9) -0.0061(9) 0.005(1) #----------------------------------------------------------------------- _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 336 _refine_ls_number_parameters 29 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0281 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0285 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.566 _refine_ls_shift/esd_max 0.0000 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.45 _refine_diff_density_max 0.40 #----------------------------------------------------------------------- _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co(1) N(1) 2.092(2) ? ? yes Co(1) N(1) 2.092(2) ? ? yes Co(1) N(1) 2.092(2) ? ? yes Co(1) N(1) 2.092(2) ? ? yes Co(1) N(2) 2.150(3) ? ? yes Co(1) N(2) 2.150(3) ? ? yes N(1) C(1) 1.155(3) ? ? yes N(2) C(1) 1.324(3) ? ? yes N(2) C(1) 1.324(3) ? ? yes #----------------------------------------------------------------------- loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Co(1) N(1) 85.3(1) ? ? ? yes N(1) Co(1) N(1) 180.0 ? ? ? yes N(1) Co(1) N(1) 94.7(1) ? ? ? yes N(1) Co(1) N(2) 91.02(7) ? ? ? yes N(1) Co(1) N(2) 88.98(7) ? ? ? yes N(1) Co(1) N(1) 94.7(1) ? ? ? yes N(1) Co(1) N(1) 180.0 ? ? ? yes N(1) Co(1) N(2) 88.98(7) ? ? ? yes N(1) Co(1) N(2) 91.02(7) ? ? ? yes N(1) Co(1) N(1) 85.3(1) ? ? ? yes N(1) Co(1) N(2) 88.98(7) ? ? ? yes N(1) Co(1) N(2) 91.02(7) ? ? ? yes N(1) Co(1) N(2) 91.02(7) ? ? ? yes N(1) Co(1) N(2) 88.98(7) ? ? ? yes N(2) Co(1) N(2) 180.0 ? ? ? yes Co(1) N(1) C(1) 159.9(2) ? ? ? yes Co(1) N(2) C(1) 120.6(1) ? ? ? yes Co(1) N(2) C(1) 120.6(1) ? ? ? yes C(1) N(2) C(1) 117.1(3) ? ? ? yes N(1) C(1) N(2) 175.2(3) ? ? ? yes #----------------------------------------------------------------------- _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 ; Structural isomers of M(dca)2 molecule-based magnets. Crystal structure of tetrahedrally coordinated sheet-like beta-Zn(dca)2 and beta-Co/Zn(dca)2, and the octahedrally coordinated rutile-like alpha- Co(dca)2, where dca- = dicyanamide, N(CN)2-, and m ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; #=END data_betaZn(dca)2(123K) #----------------------------------------------------------------------- _audit_creation_date 'Tue Oct 13 13:23:36 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #----------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #----------------------------------------------------------------------- _cell_length_a 7.6060(3) _cell_length_b 7.5844(3) _cell_length_c 11.8422(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 683.14(8) _cell_formula_units_Z 4 _cell_measurement_temperature 123.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #----------------------------------------------------------------------- _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a ' _symmetry_Int_Tables_number 62 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x,1/2-y,1/2-z' ' -x,1/2+y, -z' '1/2-x, -y,1/2+z' ' -x, -y, -z' '1/2-x,1/2+y,1/2+z' ' +x,1/2-y, +z' '1/2+x, +y,1/2-z' #----------------------------------------------------------------------- _exptl_crystal_description 'tabular' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.080 _exptl_crystal_density_diffrn 1.920 _exptl_crystal_density_meas ? _chemical_formula_weight 197.46 _chemical_formula_analytical ? _chemical_formula_sum 'C4 N6 Zn ' _chemical_formula_moiety 'C4 N6 Zn ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 384.00 _exptl_absorpt_coefficient_mu 3.528 _exptl_absorpt_correction_type none #----------------------------------------------------------------------- _diffrn_special_details none _diffrn_ambient_temperature 123.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD' _diffrn_measurement_device 'Nonius KappaCCD diffractometer' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 9157 _reflns_number_total 1019 _reflns_number_observed 700 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 0.048 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 28.22 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #----------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Zn 0 4 0.284 1.430 'International Tables' C 0 16 0.003 0.002 'International Tables' N 0 24 0.006 0.003 'International Tables' #----------------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Zn(1) 0.22121(4) 0.2500 0.34730(3) 0.02561(10) Uij ? ? N(1) 0.4296(3) 0.2500 0.4435(2) 0.0376(7) Uij ? ? N(2) 0.7217(3) 0.2500 0.5295(2) 0.0431(8) Uij ? ? N(3) 0.0062(3) 0.2500 0.4348(2) 0.0363(7) Uij ? ? N(4) 0.2311(2) 0.0400(2) 0.2508(1) 0.0334(5) Uij ? ? N(5) 0.3338(4) -0.2500 0.1914(2) 0.0449(8) Uij ? ? C(1) 0.5711(3) 0.2500 0.4785(2) 0.0315(8) Uij ? ? C(2) -0.1319(4) 0.2500 0.4745(2) 0.0296(8) Uij ? ? C(3) 0.2725(2) -0.1005(2) 0.2272(2) 0.0300(5) Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Zn(1) 0.0183(2) 0.0262(2) 0.0323(2) 0.0000 0.0006(1) 0.0000 N(1) 0.019(1) 0.054(1) 0.040(2) 0.0000 0.001(1) 0.0000 N(2) 0.018(1) 0.087(2) 0.025(1) 0.0000 0.000(1) 0.0000 N(3) 0.021(1) 0.056(2) 0.032(2) 0.0000 -0.003(1) 0.0000 N(4) 0.0356(9) 0.0235(8) 0.041(1) -0.0017(7) 0.0023(7) 0.0026(7) N(5) 0.069(2) 0.025(1) 0.041(2) 0.0000 0.023(1) 0.0000 C(1) 0.025(2) 0.044(2) 0.025(2) 0.0000 0.007(1) 0.0000 C(2) 0.025(2) 0.041(1) 0.022(2) 0.0000 -0.007(1) 0.0000 C(3) 0.037(1) 0.025(1) 0.028(1) -0.0051(8) 0.0040(8) 0.0056(8) #----------------------------------------------------------------------- _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 700 _refine_ls_number_parameters 61 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0225 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0226 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.238 _refine_ls_shift/esd_max 0.0001 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.41 _refine_diff_density_max 0.22 #----------------------------------------------------------------------- _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn(1) N(1) 1.952(2) ? ? yes Zn(1) N(3) 1.936(2) ? ? yes Zn(1) N(4) 1.962(2) ? ? yes Zn(1) N(4) 1.962(2) ? ? yes N(1) C(1) 1.153(3) ? ? yes N(2) C(1) 1.295(3) ? ? yes N(2) C(2) 1.291(4) ? ? yes N(3) C(2) 1.151(3) ? ? yes N(4) C(3) 1.146(2) ? ? yes N(5) C(3) 1.297(2) ? ? yes N(5) C(3) 1.297(2) ? ? yes #----------------------------------------------------------------------- loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Zn(1) N(3) 111.93(10) ? ? ? yes N(1) Zn(1) N(4) 107.99(6) ? ? ? yes N(1) Zn(1) N(4) 107.99(6) ? ? ? yes N(3) Zn(1) N(4) 110.13(5) ? ? ? yes N(3) Zn(1) N(4) 110.13(5) ? ? ? yes N(4) Zn(1) N(4) 108.57(10) ? ? ? yes Zn(1) N(1) C(1) 165.4(2) ? ? ? yes C(1) N(2) C(2) 121.8(2) ? ? ? yes Zn(1) N(3) C(2) 171.7(2) ? ? ? yes Zn(1) N(4) C(3) 155.2(2) ? ? ? yes C(3) N(5) C(3) 121.9(2) ? ? ? yes N(1) C(1) N(2) 173.2(3) ? ? ? yes N(2) C(2) N(3) 173.7(3) ? ? ? yes N(4) C(3) N(5) 172.5(2) ? ? ? yes #----------------------------------------------------------------------- _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 ; Structural isomers of M(dca)2 molecule-based magnets. Crystal structure of tetrahedrally coordinated sheet-like beta-Zn(dca)2 and beta-Co/Zn(dca)2, and the octahedrally coordinated rutile-like alpha- Co(dca)2, where dca- = dicyanamide, N(CN)2-, and m ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; #=END data_betaCoZn(dca)2 #----------------------------------------------------------------------- _audit_creation_date 'Tue Oct 13 13:10:50 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #----------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #----------------------------------------------------------------------- _cell_length_a 7.6070(3) _cell_length_b 7.5828(4) _cell_length_c 11.8468(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 683.35(10) _cell_formula_units_Z 4 _cell_measurement_temperature 123.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #----------------------------------------------------------------------- _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a ' _symmetry_Int_Tables_number 62 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x,1/2-y,1/2-z' ' -x,1/2+y, -z' '1/2-x, -y,1/2+z' ' -x, -y, -z' '1/2-x,1/2+y,1/2+z' ' +x,1/2-y, +z' '1/2+x, +y,1/2-z' #----------------------------------------------------------------------- _exptl_crystal_description 'tabular' _exptl_crystal_colour 'blue' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.070 _exptl_crystal_density_diffrn 1.919 _exptl_crystal_density_meas ? _chemical_formula_weight 197.46 _chemical_formula_analytical ? _chemical_formula_sum 'C4 N6 Zn ' _chemical_formula_moiety 'C4 N6 Zn ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 384.00 _exptl_absorpt_coefficient_mu 3.527 _exptl_absorpt_correction_type none #----------------------------------------------------------------------- _diffrn_special_details none _diffrn_ambient_temperature 123.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD' _diffrn_measurement_device 'Nonius KappaCCD diffractometer' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 8876 _reflns_number_total 1020 _reflns_number_observed 667 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 0.059 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 28.26 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #----------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Zn 0 4 0.284 1.430 'International Tables' C 0 16 0.003 0.002 'International Tables' N 0 24 0.006 0.003 'International Tables' #----------------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Zn(1) 0.22120(4) 0.2500 0.34731(3) 0.0285(1) Uij ? ? N(1) 0.4299(4) 0.2500 0.4434(3) 0.0390(9) Uij ? ? N(2) 0.7216(3) 0.2500 0.5302(2) 0.0440(9) Uij ? ? N(3) 0.0067(4) 0.2500 0.4346(2) 0.0380(9) Uij ? ? N(4) 0.2311(2) 0.0405(3) 0.2509(2) 0.0352(6) Uij ? ? N(5) 0.3337(5) -0.2500 0.1914(3) 0.0473(10) Uij ? ? C(1) 0.5707(5) 0.2500 0.4781(3) 0.033(1) Uij ? ? C(2) -0.1309(4) 0.2500 0.4747(3) 0.032(1) Uij ? ? C(3) 0.2727(3) -0.0998(3) 0.2271(2) 0.0328(7) Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Zn(1) 0.0205(2) 0.0305(2) 0.0347(2) 0.0000 0.0006(2) 0.0000 N(1) 0.020(2) 0.058(2) 0.039(2) 0.0000 -0.001(1) 0.0000 N(2) 0.017(2) 0.088(2) 0.027(2) 0.0000 0.002(1) 0.0000 N(3) 0.020(2) 0.061(2) 0.033(2) 0.0000 -0.003(1) 0.0000 N(4) 0.037(1) 0.026(1) 0.042(1) -0.0004(9) 0.0014(9) 0.0019(9) N(5) 0.071(2) 0.028(2) 0.043(2) 0.0000 0.026(2) 0.0000 C(1) 0.027(2) 0.046(2) 0.027(2) 0.0000 0.008(2) 0.0000 C(2) 0.029(2) 0.041(2) 0.025(2) 0.0000 -0.009(2) 0.0000 C(3) 0.038(1) 0.032(1) 0.028(1) -0.006(1) 0.005(1) 0.005(1) #----------------------------------------------------------------------- _refine_special_details ; The structure was refined assuming 100% Zn content, however there was a small amount of Co doping (<1%), as shown by the blue colour of the crystals. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 667 _refine_ls_number_parameters 61 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0273 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0244 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.252 _refine_ls_shift/esd_max 0.0000 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.53 _refine_diff_density_max 0.28 #----------------------------------------------------------------------- _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn(1) N(1) 1.954(3) ? ? yes Zn(1) N(3) 1.932(3) ? ? yes Zn(1) N(4) 1.958(2) ? ? yes Zn(1) N(4) 1.958(2) ? ? yes N(1) C(1) 1.147(4) ? ? yes N(2) C(1) 1.303(4) ? ? yes N(2) C(2) 1.301(4) ? ? yes N(3) C(2) 1.150(4) ? ? yes N(4) C(3) 1.145(3) ? ? yes N(5) C(3) 1.301(3) ? ? yes N(5) C(3) 1.301(3) ? ? yes #----------------------------------------------------------------------- loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Zn(1) N(3) 112.0(1) ? ? ? yes N(1) Zn(1) N(4) 107.98(7) ? ? ? yes N(1) Zn(1) N(4) 107.98(7) ? ? ? yes N(3) Zn(1) N(4) 110.17(7) ? ? ? yes N(3) Zn(1) N(4) 110.17(7) ? ? ? yes N(4) Zn(1) N(4) 108.4(1) ? ? ? yes Zn(1) N(1) C(1) 165.4(3) ? ? ? yes C(1) N(2) C(2) 121.4(3) ? ? ? yes Zn(1) N(3) C(2) 172.0(3) ? ? ? yes Zn(1) N(4) C(3) 155.2(2) ? ? ? yes C(3) N(5) C(3) 122.3(3) ? ? ? yes N(1) C(1) N(2) 172.7(3) ? ? ? yes N(2) C(2) N(3) 174.0(3) ? ? ? yes N(4) C(3) N(5) 172.9(2) ? ? ? yes #----------------------------------------------------------------------- _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 ; Structural isomers of M(dca)2 molecule-based magnets. Crystal structure of tetrahedrally coordinated sheet-like beta-Zn(dca)2 and beta-Co/Zn(dca)2, and the octahedrally coordinated rutile-like alpha- Co(dca)2, where dca- = dicyanamide, N(CN)2-, and m ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; #=END data_betaZn(dca)2(293K) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 N6 Zn' _chemical_formula_weight 197.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Zn' 'Zn' 0.2839 1.4301 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C m c m ' _symmetry_Int_Tables_number 63 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, -z' 'x, y, -z+1/2' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, z' '-x, -y, z-1/2' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, -z-1/2' _cell_length_a 7.5526(3) _cell_length_b 12.2167(8) _cell_length_c 7.5882(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 700.15(7) _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 prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.873 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 384 _exptl_absorpt_coefficient_mu 3.441 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD' _diffrn_measurement_device 'Nonius KappaCCD diffractometer' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2534 _diffrn_reflns_av_R_equivalents 0.036 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 30.00 _reflns_number_total 567 _reflns_number_gt 512 _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. One of the N(CN)2- ligands is disordered over two positions which are related by a mirror plane. The disorder involves only atoms C2 and N4, with the two disordered positions sharing atom N3. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0721P)^2^+0.5258P] 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 567 _refine_ls_number_parameters 39 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.1246 _refine_ls_wR_factor_gt 0.1208 _refine_ls_goodness_of_fit_ref 1.217 _refine_ls_restrained_S_all 1.217 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.0000 0.10053(5) 0.2500 0.0460(3) Uani 1 d S . . N1 N 0.0000 0.1892(3) 0.0362(5) 0.0669(11) Uani 1 d S . . N2 N 0.0000 0.2746(5) -0.2500 0.083(3) Uani 1 d S . . N3 N 0.2104(5) 0.0062(4) 0.2500 0.0635(10) Uani 1 d S . . N4 N 0.5000 -0.0631(9) 0.330(2) 0.100(5) Uani 0.50 d SP . . C1 C 0.0000 0.2236(3) -0.1009(6) 0.0585(11) Uani 1 d S . . C2 C 0.3506(6) -0.0196(4) 0.2858(12) 0.060(2) Uani 0.50 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0479(5) 0.0547(4) 0.0354(4) 0.000 0.000 0.000 N1 0.103(3) 0.063(2) 0.0344(17) 0.0032(15) 0.000 0.000 N2 0.171(8) 0.042(2) 0.036(3) 0.000 0.000 0.000 N3 0.0400(18) 0.072(2) 0.079(3) 0.000 0.000 -0.0030(17) N4 0.042(4) 0.079(5) 0.180(16) 0.000 0.000 0.000 C1 0.094(3) 0.0412(17) 0.0400(19) -0.0060(14) 0.000 0.000 C2 0.042(3) 0.052(2) 0.085(8) 0.015 0.009 -0.0075(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 Zn1 N1 1.951(4) 3 ? Zn1 N1 1.951(4) . ? Zn1 N3 1.963(4) 10 ? Zn1 N3 1.963(4) . ? N1 C1 1.122(6) . ? N2 C1 1.292(5) 3_554 ? N2 C1 1.292(5) . ? N3 C2 1.138(6) . ? N4 C2 1.292(8) . ? N4 C2 1.292(8) 10_655 ? 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 Zn1 N1 112.5(2) 3 . ? N1 Zn1 N3 109.03(8) 3 10 ? N1 Zn1 N3 109.03(9) . 10 ? N1 Zn1 N3 109.03(9) 3 . ? N1 Zn1 N3 109.03(8) . . ? N3 Zn1 N3 108.1(2) 10 . ? C1 N1 Zn1 168.3(4) . . ? C1 N2 C1 122.3(5) 3_554 . ? C2 N3 Zn1 156.3(4) . . ? C2 N4 C2 121.8(11) . 10_655 ? N1 C1 N2 173.2(5) . . ? N3 C2 N4 171.5(7) . . ? _diffrn_measured_fraction_theta_max 0.483 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.483 _refine_diff_density_max 1.072 _refine_diff_density_min -0.778 _refine_diff_density_rms 0.151 _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 ; Structural isomers of M(dca)2 molecule-based magnets. Crystal structure of tetrahedrally coordinated sheet-like beta-Zn(dca)2 and beta-Co/Zn(dca)2, and the octahedrally coordinated rutile-like alpha- Co(dca)2, where dca- = dicyanamide, N(CN)2-, and m ; #=END