#------------------------------------------------------------------------------ #$Date: 2012-02-26 23:34:47 +0200 (Sun, 26 Feb 2012) $ #$Revision: 35909 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/20/11/7201189.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7201189 loop_ _publ_author_name 'Kutasi, Anna M.' 'Turner, David R.' 'Jensen, Paul' 'Moubaraki, Boujemaa' 'Batten, Stuart R.' 'Murray, Keith S.' _publ_section_title ; Coordination polymers of nitrocyanamide, O2NNCN−: synthesis, structure and magnetism ; _journal_issue 10 _journal_name_full CrystEngComm _journal_page_first 2089 _journal_volume 11 _journal_year 2009 _chemical_formula_moiety 'C6 H8 Co N8 O6, 2(H2 O)' _chemical_formula_sum 'C6 H12 Co N8 O8' _chemical_formula_weight 383.17 _chemical_name_common {[Cu(CAN)2(pyz)(H2O)2].2H2O} _chemical_name_systematic ; catena[bis(aqua)bis(nitrocyanamide)(pyrazine)copper(II)] dihydrate ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 109.184(1) _cell_angle_beta 90.647(1) _cell_angle_gamma 107.858(1) _cell_formula_units_Z 1 _cell_length_a 6.7301(1) _cell_length_b 7.0910(1) _cell_length_c 8.6218(2) _cell_measurement_reflns_used 6753 _cell_measurement_temperature 123(1) _cell_measurement_theta_max 27.50 _cell_measurement_theta_min 3.33 _cell_volume 367.002(12) _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_collection 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 123(1) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 6753 _diffrn_reflns_theta_full 27.50 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_min 3.33 _exptl_absorpt_coefficient_mu 1.227 _exptl_absorpt_correction_T_max 0.8568 _exptl_absorpt_correction_T_min 0.6396 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour pink _exptl_crystal_density_diffrn 1.734 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 195 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _refine_diff_density_max 0.280 _refine_diff_density_min -0.459 _refine_diff_density_rms 0.061 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 122 _refine_ls_number_reflns 1680 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.075 _refine_ls_R_factor_all 0.0313 _refine_ls_R_factor_gt 0.0250 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.0565 _reflns_number_gt 1497 _reflns_number_total 1680 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file b905970a.txt _[local]_cod_data_source_block 2Co _[local]_cod_cif_authors_sg_H-M P-1 _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'Multi-scan' changed to 'multi-scan' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_cell_volume 367.001(11) _cod_database_code 7201189 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 0.5000 0.5000 0.5000 0.01063(10) Uani 1 2 d S . . O1 O 0.18205(18) 0.41596(18) 0.51128(17) 0.0155(2) Uani 1 1 d . . . N1 N 0.5038(2) 0.80471(18) 0.50002(16) 0.0116(3) Uani 1 1 d . . . N2 N 0.4320(2) 0.37233(19) 0.23977(16) 0.0147(3) Uani 1 1 d . . . O3 O 0.1924(2) -0.09267(17) -0.03427(15) 0.0251(3) Uani 1 1 d . . . N4 N 0.2032(2) 0.0174(2) -0.12194(16) 0.0181(3) Uani 1 1 d . . . N3 N 0.2971(2) 0.2300(2) -0.05824(16) 0.0183(3) Uani 1 1 d . . . C11 C 0.6329(2) 0.9869(2) 0.60885(19) 0.0134(3) Uani 1 1 d . . . H11 H 0.7296 0.9829 0.6878 0.016 Uiso 1 1 calc R . . O4 O 0.1293(2) -0.05600(19) -0.26952(15) 0.0281(3) Uani 1 1 d . . . C10 C 0.3718(2) 0.8199(2) 0.39145(19) 0.0132(3) Uani 1 1 d . . . H10 H 0.2786 0.6942 0.3121 0.016 Uiso 1 1 calc R . . C12 C 0.3653(2) 0.2940(2) 0.10178(19) 0.0137(3) Uani 1 1 d . . . O2 O 0.07090(19) 0.4553(2) 0.81246(15) 0.0202(3) Uani 1 1 d . . . H3 H 0.140(4) 0.428(4) 0.601(3) 0.041(7) Uiso 1 1 d . . . H4 H 0.097(4) 0.329(4) 0.441(3) 0.041(7) Uiso 1 1 d . . . H5 H 0.143(4) 0.404(4) 0.856(3) 0.047(7) Uiso 1 1 d . . . H6 H 0.107(4) 0.574(4) 0.865(3) 0.055(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01269(17) 0.00774(15) 0.01087(17) 0.00249(11) -0.00135(11) 0.00347(11) O1 0.0132(6) 0.0164(6) 0.0132(7) 0.0020(5) -0.0008(5) 0.0034(5) N1 0.0126(6) 0.0093(6) 0.0129(7) 0.0036(5) 0.0006(5) 0.0040(5) N2 0.0190(7) 0.0112(6) 0.0135(7) 0.0043(5) 0.0005(6) 0.0046(5) O3 0.0359(7) 0.0150(6) 0.0209(7) 0.0047(5) 0.0023(5) 0.0056(5) N4 0.0182(7) 0.0165(7) 0.0138(7) 0.0010(6) 0.0024(6) 0.0021(5) N3 0.0249(8) 0.0137(6) 0.0104(7) 0.0022(5) -0.0024(6) 0.0005(5) C11 0.0134(8) 0.0121(7) 0.0134(8) 0.0031(6) -0.0032(6) 0.0038(6) O4 0.0297(7) 0.0284(7) 0.0114(6) -0.0022(5) -0.0037(5) -0.0008(5) C10 0.0129(8) 0.0117(7) 0.0132(8) 0.0032(6) -0.0019(6) 0.0028(6) C12 0.0152(8) 0.0108(7) 0.0161(9) 0.0063(6) 0.0026(6) 0.0039(6) O2 0.0191(6) 0.0198(6) 0.0175(6) 0.0035(5) -0.0011(5) 0.0040(5) 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O1 Co1 O1 180.00(8) . 2_666 ? O1 Co1 N2 92.11(5) . 2_666 ? O1 Co1 N2 87.89(5) 2_666 2_666 ? O1 Co1 N2 87.89(5) . . ? O1 Co1 N2 92.11(5) 2_666 . ? N2 Co1 N2 180.0 2_666 . ? O1 Co1 N1 89.85(4) . . ? O1 Co1 N1 90.15(4) 2_666 . ? N2 Co1 N1 89.19(5) 2_666 . ? N2 Co1 N1 90.81(5) . . ? O1 Co1 N1 90.15(4) . 2_666 ? O1 Co1 N1 89.85(4) 2_666 2_666 ? N2 Co1 N1 90.81(5) 2_666 2_666 ? N2 Co1 N1 89.19(5) . 2_666 ? N1 Co1 N1 180.0 . 2_666 ? Co1 O1 H3 119.0(16) . . ? Co1 O1 H4 124.6(17) . . ? H3 O1 H4 110(2) . . ? C10 N1 C11 116.69(12) . . ? C10 N1 Co1 120.58(9) . . ? C11 N1 Co1 122.72(10) . . ? C12 N2 Co1 170.20(12) . . ? O4 N4 O3 123.37(13) . . ? O4 N4 N3 115.83(13) . . ? O3 N4 N3 120.80(13) . . ? C12 N3 N4 111.27(13) . . ? N1 C11 C10 121.45(14) . 2_676 ? N1 C11 H11 119.3 . . ? C10 C11 H11 119.3 2_676 . ? N1 C10 C11 121.87(13) . 2_676 ? N1 C10 H10 119.1 . . ? C11 C10 H10 119.1 2_676 . ? N2 C12 N3 172.21(15) . . ? H5 O2 H6 105(2) . . ? 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 O1 2.0504(11) . ? Co1 O1 2.0504(11) 2_666 ? Co1 N2 2.1097(13) 2_666 ? Co1 N2 2.1097(13) . ? Co1 N1 2.1530(12) . ? Co1 N1 2.1530(12) 2_666 ? O1 H3 0.81(3) . ? O1 H4 0.78(2) . ? N1 C10 1.3352(19) . ? N1 C11 1.3420(19) . ? N2 C12 1.1516(19) . ? O3 N4 1.2409(18) . ? N4 O4 1.2364(17) . ? N4 N3 1.3556(18) . ? N3 C12 1.329(2) . ? C11 C10 1.381(2) 2_676 ? C11 H11 0.9500 . ? C10 C11 1.381(2) 2_676 ? C10 H10 0.9500 . ? O2 H5 0.84(3) . ? O2 H6 0.77(3) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H3 O2 0.81(3) 1.85(3) 2.6601(18) 174(2) . O1 H4 O4 0.78(2) 2.12(3) 2.8941(17) 170(2) 2 O2 H5 N3 0.84(3) 2.13(3) 2.9556(19) 172(2) 1_556 O2 H6 O3 0.77(3) 2.11(3) 2.8763(17) 169(3) 1_566