#------------------------------------------------------------------------------ #$Date: 2013-08-29 16:37:19 +0100 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/23/2012346.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2012346 loop_ _publ_author_name 'Li, Baolong' 'Shen, Xiaoping' 'Zou, Jianzhong' 'Xu, Zheng' 'Yu, Kaibei' _publ_section_title ; A three-dimensional porous framework complex, poly[[bis(ethylenediamine)copper(II)] [potassium hexacyanocobalt(III)]] ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1242 _journal_page_last 1244 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Cu (C2 H8 N2)2] [K Co (CN)6]' _chemical_formula_moiety 'C4 H16 Cu N4 2+ , C6 Co N6 3- , K +' _chemical_formula_sum 'C10 H16 Co Cu K N10' _chemical_formula_weight 437.90 _chemical_name_systematic ; Poly{[bis(ethylenediamine)copper(II)] [potassium hexacyanocobalt(III)]} ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _cell_angle_alpha 90 _cell_angle_beta 98.91(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.391(2) _cell_length_b 16.866(3) _cell_length_c 11.791(2) _cell_measurement_reflns_used 26 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 17.46 _cell_measurement_theta_min 3.03 _cell_volume 1648.6(6) _computing_cell_refinement XSCANS _computing_data_collection 'XSCANS (Siemens, 1996)' _computing_data_reduction 'SHELXTL (Sheldrick, 1995)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 295(2) _diffrn_measured_fraction_theta_full .999 _diffrn_measured_fraction_theta_max .999 _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .013 _diffrn_reflns_av_sigmaI/netI .021 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 2172 _diffrn_reflns_theta_full 27.00 _diffrn_reflns_theta_max 27 _diffrn_reflns_theta_min 2.42 _diffrn_standards_decay_% 3.57 _diffrn_standards_interval_count 97 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 2.562 _exptl_absorpt_correction_T_max .599 _exptl_absorpt_correction_T_min .333 _exptl_absorpt_correction_type \y-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour violet-red _exptl_crystal_density_diffrn 1.764 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 884 _exptl_crystal_size_max .44 _exptl_crystal_size_mid .41 _exptl_crystal_size_min .20 _refine_diff_density_max .43 _refine_diff_density_min -.28 _refine_ls_extinction_coef .0044(3) _refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997)' _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 127 _refine_ls_number_reflns 1797 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.053 _refine_ls_R_factor_all .028 _refine_ls_R_factor_gt .024 _refine_ls_shift/su_max .001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0355P)^2^+0.0854P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .062 _reflns_number_gt 1606 _reflns_number_total 1797 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file sk1474.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'C 2/c' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' 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 The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' 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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2012346 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' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Cu 0 0 0 .03702(13) Uani d S 1 . . Cu Co -0.5 -.11561(2) -0.25 .01809(11) Uani d S 1 . . Co K -0.5 .14220(4) -0.25 .02579(14) Uani d S 1 . . K N1 0.1150(2) .08553(11) -0.07137(15) .0381(5) Uani d P 1 A 1 N H1A 0.2174 .0898 -0.0355 .046 Uiso calc PR .535(4) A 1 H H1B 0.1164 .0748 -0.1460 .046 Uiso calc PR .535(4) A 1 H N2 -0.1205(2) .08848(12) 0.05931(17) .0472(6) Uani d P 1 A 1 N H2A -0.2240 .0876 0.0247 .057 Uiso calc PR .535(4) A 1 H H2B -0.1192 .0824 0.1353 .057 Uiso calc PR .535(4) A 1 H C1 0.0287(10) .1575(5) -0.0597(9) .055(2) Uani d P .535(4) A 1 C H1C 0.1037 .2015 -0.0559 .066 Uiso calc PR .535(4) A 1 H H1D -0.0509 .1647 -0.1279 .066 Uiso calc PR .535(4) A 1 H C2 -0.0510(12) .1605(6) 0.0384(7) .056(2) Uani d P .535(4) A 1 C H2C 0.0261 .1754 0.1050 .068 Uiso calc PR .535(4) A 1 H H2D -0.1341 .2010 0.0268 .068 Uiso calc PR .535(4) A 1 H H1A' 0.2219 .0765 -0.0563 .046 Uiso calc PR .465(4) A 2 H H1B' 0.0853 .0840 -0.1480 .046 Uiso calc PR .465(4) A 2 H H2A' -0.2265 .0769 0.0496 .057 Uiso calc PR .465(4) A 2 H H2B' -0.0861 .0951 0.1349 .057 Uiso calc PR .465(4) A 2 H C1' 0.0804(10) .1669(7) -0.0284(9) .044(2) Uani d P .465(4) A 2 C H1'1 0.0912 .2067 -0.0860 .053 Uiso calc PR .465(4) A 2 H H1'2 0.1542 .1795 0.0409 .053 Uiso calc PR .465(4) A 2 H C2' -0.0944(12) .1636(7) -0.0039(7) .0413(18) Uani d P .465(4) A 2 C H2'1 -0.1154 .2090 0.0420 .050 Uiso calc PR .465(4) A 2 H H2'2 -0.1686 .1655 -0.0756 .050 Uiso calc PR .465(4) A 2 H N3 -0.2401(2) -.24183(11) -0.24466(15) .0451(5) Uani d . 1 . . N N4 -0.49330(19) -.11768(12) 0.00952(13) .0366(4) Uani d . 1 . . N N5 -0.2312(2) .00773(11) -0.20865(17) .0384(4) Uani d . 1 . . N C3 -0.3384(2) -.19515(11) -0.24350(15) .0267(4) Uani d . 1 . . C C4 -0.4945(2) -.11660(11) -0.08784(15) .0241(4) Uani d . 1 . . C C5 -0.3349(2) -.03750(11) -0.22782(14) .0234(4) Uani d . 1 . . C 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 Cu .0317(2) .0334(2) .0518(2) .00252(15) .02479(17) .00547(16) Co .01755(18) .01938(18) .01787(17) 0 .00438(12) 0 K .0281(3) .0260(3) .0241(3) 0 .0067(2) 0 N1 .0324(10) .0466(12) .0372(9) -.0069(8) .0115(7) .0009(8) N2 .0463(12) .0492(13) .0516(12) .0145(10) .0249(9) .0086(10) C1 .053(5) .030(4) .086(6) -.005(3) .023(4) .014(4) C2 .066(6) .044(4) .063(6) -.003(4) .022(4) -.011(5) C1' .035(5) .039(4) .061(5) -.018(3) .012(3) -.007(3) C2' .047(5) .034(3) .043(5) .012(3) .008(3) .011(4) N3 .0456(11) .0461(11) .0437(11) .0194(10) .0077(9) -.0019(10) N4 .0382(10) .0498(12) .0227(9) .0014(8) .0072(7) .0024(7) N5 .0351(10) .0367(10) .0448(11) -.0108(8) .0112(8) -.0062(8) C3 .0270(9) .0283(10) .0248(9) .0028(8) .0042(7) -.0005(8) C4 .0200(8) .0262(9) .0262(10) .0020(7) .0042(7) .0004(7) C5 .0249(9) .0248(9) .0215(8) .0013(8) .0068(7) -.0013(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cu N2 5 1.9895(19) yes Cu N2 . 1.9895(19) yes Cu N1 . 1.9928(18) yes Cu N1 5 1.9928(18) yes Co C5 2_454 1.9001(19) yes Co C5 . 1.9001(19) yes Co C3 . 1.9004(19) yes Co C3 2_454 1.9004(19) yes Co C4 . 1.9056(18) yes Co C4 2_454 1.9056(18) yes K N3 4_454 2.8158(18) yes K N3 3_455 2.8158(18) yes K N4 6 2.8746(16) yes K N4 5_455 2.8746(16) yes K N5 2_454 3.183(2) yes K N5 . 3.183(2) yes K C5 . 3.326(2) yes K C5 2_454 3.326(2) yes N1 C1 . 1.431(10) no N1 H1A . .9000 no N1 H1B . .9000 no N2 C2 . 1.386(11) no N2 H2A . .9000 no N2 H2B . .9000 no C1 C2 . 1.424(15) no C1 H1C . .9700 no C1 H1D . .9700 no C2 H2C . .9700 no C2 H2D . .9700 no C1' C2' . 1.539(15) no C1' H1'1 . .9700 no C1' H1'2 . .9700 no C2' H2'1 . .9700 no C2' H2'2 . .9700 no N3 C3 . 1.142(2) no N3 K 3_545 2.8158(18) no N4 C4 . 1.147(2) no N4 K 5_455 2.8746(16) no N5 C5 . 1.153(2) no loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K .2009 .2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co .3494 .9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu .3201 1.2651 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N2 Cu N2 5 . 180.00(14) no N2 Cu N1 5 . 95.10(9) no N2 Cu N1 . . 84.90(9) no N2 Cu N1 5 5 84.90(9) yes N2 Cu N1 . 5 95.10(9) yes N1 Cu N1 . 5 180.00(12) no C5 Co C5 2_454 . 92.21(11) yes C5 Co C3 2_454 . 174.44(7) yes C5 Co C3 . . 89.05(8) yes C5 Co C3 2_454 2_454 89.05(8) no C5 Co C3 . 2_454 174.44(7) no C3 Co C3 . 2_454 90.20(12) yes C5 Co C4 2_454 . 92.74(7) no C5 Co C4 . . 87.95(7) yes C3 Co C4 . . 92.71(8) yes C3 Co C4 2_454 . 86.58(8) yes C5 Co C4 2_454 2_454 87.95(7) no C5 Co C4 . 2_454 92.74(7) no C3 Co C4 . 2_454 86.58(8) no C3 Co C4 2_454 2_454 92.71(8) no C4 Co C4 . 2_454 179.00(11) yes C1 N1 Cu . . 106.8(4) no C1 N1 H1A . . 110.4 no Cu N1 H1A . . 110.4 no C1 N1 H1B . . 110.4 no Cu N1 H1B . . 110.4 no H1A N1 H1B . . 108.6 no C2 N2 Cu . . 110.1(4) no C2 N2 H2A . . 109.6 no Cu N2 H2A . . 109.6 no C2 N2 H2B . . 109.6 no Cu N2 H2B . . 109.6 no H2A N2 H2B . . 108.1 no C2 C1 N1 . . 114.6(8) no C2 C1 H1C . . 108.6 no N1 C1 H1C . . 108.6 no C2 C1 H1D . . 108.6 no N1 C1 H1D . . 108.6 no H1C C1 H1D . . 107.6 no N2 C2 C1 . . 112.1(7) no N2 C2 H2C . . 109.2 no C1 C2 H2C . . 109.2 no N2 C2 H2D . . 109.2 no C1 C2 H2D . . 109.2 no H2C C2 H2D . . 107.9 no C2' C1' H1'1 . . 110.6 no C2' C1' H1'2 . . 110.6 no H1'1 C1' H1'2 . . 108.7 no C1' C2' H2'1 . . 109.7 no C1' C2' H2'2 . . 109.7 no H2'1 C2' H2'2 . . 108.2 no N3 C3 Co . . 176.75(18) yes N4 C4 Co . . 179.06(18) yes N5 C5 Co . . 176.10(17) yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion _geom_torsion_publ_flag N2 Cu N1 C1 5 169.2(4) no N2 Cu N1 C1 . -10.8(4) no N1 Cu N2 C2 . -9.1(4) no N1 Cu N2 C2 5 170.9(4) no Cu N1 C1 C2 . 29.7(8) no Cu N2 C2 C1 . 27.7(9) no N1 C1 C2 N2 . -39.4(11) no C3 Co C5 K . 174.59(7) no C4 Co C5 K . -92.67(7) no C4 Co C5 K 2_454 88.06(7) no _cod_database_fobs_code 2012346