#------------------------------------------------------------------------------ #$Date: 2013-08-29 16:37:19 +0100 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/29/2012978.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_2012978 loop_ _publ_author_name '\n~^n^+ and the unusual [Ag~2~(CN)~3~]^{-^} anion (dien is diethylenetriamine) ; _journal_issue 10 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m490 _journal_page_last m493 _journal_volume 58 _journal_year 2002 _chemical_formula_iupac '[Cu (C4 H13 N3) Ag (C N)2]2 [Ag (C N)2] [Ag2 (C N)3]' _chemical_formula_moiety '2C6 H13 Ag Cu N5 + , C2 Ag N2 - , C3 Ag2 N3 -' _chemical_formula_sum 'C17 H26 Ag5 Cu2 N15' _chemical_formula_weight 1106.96 _chemical_name_systematic ; catena-poly[bis[[\m-cyano-1:2\k^2^C:N-diethylenetriamine- 2\k^3^N-copper(II)silver(I)]-\m-cyano-1:2'\k^2^C:N] dicyanosilver(I) tricyanodisilver(I)] ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL97 _cell_angle_alpha 90 _cell_angle_beta 90.794(11) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 12.5588(12) _cell_length_b 17.8070(12) _cell_length_c 6.9608(6) _cell_measurement_reflns_used 8000 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 30.25 _cell_measurement_theta_min 2.80 _cell_volume 1556.5(2) _computing_cell_refinement 'CELL in IPDS' _computing_data_collection 'EXPOSE in IPDS (Stoe & Cie, 1999)' _computing_data_reduction 'INTEGRATE in IPDS' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1985)' _diffrn_ambient_temperature 193(2) _diffrn_measured_fraction_theta_full 0.96 _diffrn_measured_fraction_theta_max 0.96 _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method \f _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 0.056 _diffrn_reflns_av_sigmaI/netI 0.051 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 18169 _diffrn_reflns_theta_full 30.25 _diffrn_reflns_theta_max 30.25 _diffrn_reflns_theta_min 2.80 _diffrn_standards_decay_% negligible _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 4.454 _exptl_absorpt_correction_T_max 0.809 _exptl_absorpt_correction_T_min 0.414 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details '(SHELXTL; Sheldrick, 1995)' _exptl_crystal_colour blue _exptl_crystal_density_diffrn 2.362 _exptl_crystal_density_meas 2.360(10) _exptl_crystal_density_method flotation _exptl_crystal_description parallelepiped _exptl_crystal_F_000 1052 _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.83 _refine_diff_density_min -0.65 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.876 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 219 _refine_ls_number_reflns 4462 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.876 _refine_ls_R_factor_all 0.058 _refine_ls_R_factor_gt 0.031 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0352P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.061 _refine_ls_wR_factor_ref 0.067 _reflns_number_gt 2988 _reflns_number_total 4462 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file gg1124.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_database_code 2012978 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -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 Ag1 0.21171(3) 0.419404(15) 0.19494(5) 0.03281(8) Uani d . 1 . . Ag Ag2 0.0000 0.5000 0.0000 0.03470(11) Uani d S 1 . . Ag Ag3 0.17822(2) 0.440834(16) 0.64119(5) 0.03363(8) Uani d . 1 . . Ag Cu 0.19075(3) 0.18433(2) 0.61891(6) 0.02184(10) Uani d . 1 . . Cu N1 0.0331(3) 0.17241(19) 0.6590(5) 0.0296(7) Uani d . 1 . . N H1A 0.012(4) 0.218(3) 0.690(7) 0.034(5) Uiso d . 1 . . H H1B -0.003(4) 0.160(2) 0.559(7) 0.034(5) Uiso d . 1 . . H N2 0.2048(3) 0.12959(19) 0.8741(5) 0.0321(7) Uani d . 1 . . N H2 0.232(4) 0.080(2) 0.839(6) 0.034(5) Uiso d . 1 . . H N3 0.3431(3) 0.21506(18) 0.6773(5) 0.0285(7) Uani d . 1 . . N H3A 0.379(4) 0.208(2) 0.572(7) 0.034(5) Uiso d . 1 . . H H3B 0.341(4) 0.261(3) 0.704(7) 0.034(5) Uiso d . 1 . . H N11 0.1780(3) 0.26263(16) 0.4163(5) 0.0282(7) Uani d . 1 . . N N12 0.2231(3) 0.08427(17) 0.4517(5) 0.0303(7) Uani d . 1 . . N N21 -0.0163(3) 0.6725(2) 0.1352(6) 0.0439(9) Uani d . 1 . . N N31 0.4001(3) 0.3815(2) 0.8151(6) 0.0444(9) Uani d . 1 . . N C32 0.0398(3) 0.48861(19) 0.5275(5) 0.0329(8) Uani d P 0.50 . . C N32 0.0398(3) 0.48861(19) 0.5275(5) 0.0329(8) Uani d P 0.50 . . N C11 0.1877(3) 0.31622(19) 0.3255(6) 0.0287(8) Uani d . 1 . . C C12 0.2544(3) 0.52626(19) 0.1053(6) 0.0271(8) Uani d . 1 . . C C21 -0.0148(3) 0.6121(2) 0.0803(6) 0.0338(9) Uani d . 1 . . C C31 0.3236(3) 0.4062(2) 0.7514(6) 0.0315(9) Uani d . 1 . . C C1 0.0155(4) 0.1164(3) 0.8136(7) 0.0400(10) Uani d . 1 . . C H1C 0.019(4) 0.068(3) 0.754(7) 0.049(5) Uiso d . 1 . . H H1D -0.041(4) 0.123(3) 0.870(8) 0.049(5) Uiso d . 1 . . H C2 0.0994(4) 0.1303(3) 0.9690(7) 0.0453(12) Uani d . 1 . . C H2A 0.093(4) 0.186(3) 1.022(7) 0.049(5) Uiso d . 1 . . H H2B 0.100(4) 0.098(3) 1.043(8) 0.049(5) Uiso d . 1 . . H C3 0.2951(4) 0.1616(3) 0.9827(7) 0.0418(10) Uani d . 1 . . C H3C 0.309(4) 0.127(3) 1.081(8) 0.049(5) Uiso d . 1 . . H H3D 0.268(4) 0.208(3) 1.019(7) 0.049(5) Uiso d . 1 . . H C4 0.3840(3) 0.1728(3) 0.8441(7) 0.0387(10) Uani d . 1 . . C H4A 0.432(4) 0.204(3) 0.912(8) 0.049(5) Uiso d . 1 . . H H4B 0.410(4) 0.121(3) 0.795(7) 0.049(5) Uiso d . 1 . . H 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 Ag1 0.04474(18) 0.02123(12) 0.03246(19) -0.00092(11) 0.00121(12) 0.00723(11) Ag2 0.0415(2) 0.0328(2) 0.0298(3) -0.00204(17) 0.00086(18) 0.00180(16) Ag3 0.03189(16) 0.03372(14) 0.0351(2) 0.00696(11) -0.00694(12) -0.00175(12) Cu 0.0265(2) 0.02080(18) 0.0182(2) 0.00041(15) -0.00066(16) 0.00275(15) N1 0.0297(17) 0.0350(17) 0.024(2) 0.0026(13) -0.0061(13) -0.0005(13) N2 0.0332(18) 0.0361(17) 0.027(2) 0.0042(13) -0.0004(14) 0.0079(14) N3 0.0281(17) 0.0259(15) 0.032(2) -0.0018(12) 0.0005(14) 0.0012(13) N11 0.0357(18) 0.0218(14) 0.0272(19) 0.0028(12) -0.0019(14) 0.0021(12) N12 0.0402(18) 0.0241(14) 0.027(2) 0.0018(13) 0.0033(14) 0.0005(12) N21 0.046(2) 0.043(2) 0.043(3) 0.0013(16) 0.0066(17) -0.0014(16) N31 0.040(2) 0.050(2) 0.042(3) 0.0078(16) -0.0081(17) -0.0064(17) CN32 0.0368(19) 0.0371(18) 0.025(2) 0.0106(15) -0.0008(15) 0.0013(14) C11 0.035(2) 0.0258(16) 0.025(2) 0.0011(14) -0.0008(15) 0.0008(14) C12 0.036(2) 0.0248(16) 0.021(2) -0.0018(14) -0.0006(15) 0.0001(14) C21 0.037(2) 0.038(2) 0.027(2) -0.0025(16) 0.0026(17) 0.0025(16) C31 0.036(2) 0.0295(18) 0.029(2) 0.0061(15) -0.0073(16) -0.0076(15) C1 0.031(2) 0.055(3) 0.034(3) -0.0067(19) 0.0025(18) 0.010(2) C2 0.035(2) 0.074(3) 0.027(3) -0.003(2) 0.0037(18) 0.021(2) C3 0.037(2) 0.063(3) 0.026(3) 0.007(2) -0.0044(18) 0.001(2) C4 0.031(2) 0.052(3) 0.034(3) -0.0059(18) -0.0073(17) 0.0041(19) 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 Ag1 Ag2 . 3.2970(4) y Ag1 Ag3 . 3.1635(6) y Ag1 C11 . 2.074(4) y Ag1 C12 . 2.075(3) y Ag2 C21 . 2.082(4) y Ag3 C31 . 2.065(4) y Cu N1 . 2.014(3) y Cu N2 . 2.032(3) y Cu N3 . 2.026(3) y Cu N11 . 1.988(3) y Cu N12 . 2.170(3) y N1 C1 . 1.486(5) ? N2 C2 . 1.487(5) ? N2 C3 . 1.469(6) ? N3 C4 . 1.470(5) ? N11 C11 . 1.152(5) y N21 C21 . 1.142(5) y N31 C31 . 1.141(5) y C12 N12 2 1.143(4) ? C1 C2 . 1.520(7) ? C3 C4 . 1.499(7) ? N1 H1B . 0.86(5) ? N1 H1A . 0.89(4) ? N2 H2 . 0.97(4) ? N3 H3A . 0.88(5) ? N3 H3B . 0.85(5) ? C1 H1C . 0.96(5) ? C1 H1D . 0.83(5) ? C2 H2A . 1.07(5) ? C2 H2B . 0.77(5) ? C3 H3C . 0.94(5) ? C3 H3D . 0.92(5) ? C4 H4A . 0.94(5) ? C4 H4B . 1.04(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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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 C11 Ag1 C12 . . 169.69(15) y C11 Ag1 Ag3 . . 69.78(11) ? C12 Ag1 Ag3 . . 102.90(11) ? C11 Ag1 Ag2 . . 116.42(11) ? C12 Ag1 Ag2 . . 71.78(11) ? Ag3 Ag1 Ag2 . . 103.543(14) ? C21 Ag2 C21 . 3_565 180.0 ? C21 Ag2 Ag1 . 3_565 67.58(12) ? C21 Ag2 Ag1 . . 112.42(12) ? C31 Ag3 Ag1 . . 101.54(12) ? N11 Cu N1 . . 95.89(13) y N11 Cu N3 . . 91.11(13) y N1 Cu N3 . . 158.13(15) y N11 Cu N2 . . 164.12(14) y N1 Cu N2 . . 84.36(13) y N3 Cu N2 . . 83.34(14) y N11 Cu N12 . . 102.07(13) y N1 Cu N12 . . 100.33(14) y N3 Cu N12 . . 98.41(14) y N2 Cu N12 . . 93.47(13) y C1 N1 Cu . . 109.1(3) ? C1 N1 H1A . . 113(3) ? Cu N1 H1A . . 104(3) ? C1 N1 H1B . . 109(3) ? Cu N1 H1B . . 115(3) ? H1A N1 H1B . . 106(4) ? C3 N2 C2 . . 116.9(4) ? C3 N2 Cu . . 108.7(3) ? C2 N2 Cu . . 108.5(3) ? C3 N2 H2 . . 102(3) ? C2 N2 H2 . . 116(3) ? Cu N2 H2 . . 104(3) ? C4 N3 Cu . . 109.8(2) ? C4 N3 H3A . . 114(3) ? Cu N3 H3A . . 107(3) ? C4 N3 H3B . . 110(3) ? Cu N3 H3B . . 106(3) ? H3A N3 H3B . . 110(4) ? C11 N11 Cu . . 164.2(3) y C12 N12 Cu 2_545 . 167.7(3) y N11 C11 Ag1 . . 172.6(3) ? N12 C12 Ag1 2 . 177.2(3) ? N21 C21 Ag2 . . 174.3(4) ? N31 C31 Ag3 . . 174.5(4) ? N1 C1 C2 . . 107.3(4) ? N1 C1 H1C . . 107(3) ? C2 C1 H1C . . 115(3) ? N1 C1 H1D . . 112(4) ? C2 C1 H1D . . 103(4) ? H1C C1 H1D . . 113(5) ? N2 C2 C1 . . 107.1(4) ? N2 C2 H2A . . 104(3) ? C1 C2 H2A . . 110(3) ? N2 C2 H2B . . 107(4) ? C1 C2 H2B . . 110(4) ? H2A C2 H2B . . 118(5) ? N2 C3 C4 . . 107.3(4) ? N2 C3 H3C . . 104(3) ? C4 C3 H3C . . 115(3) ? N2 C3 H3D . . 102(3) ? C4 C3 H3D . . 109(3) ? H3C C3 H3D . . 117(4) ? N3 C4 C3 . . 108.7(4) ? N3 C4 H4A . . 108(3) ? C3 C4 H4A . . 104(3) ? N3 C4 H4B . . 108(3) ? C3 C4 H4B . . 110(3) ? H4A C4 H4B . . 119(4) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1A N21 3_566 0.89(5) 2.29(5) 3.119(5) 154(4) yes N1 H1B N31 4_565 0.86(5) 2.20(5) 3.055(5) 175(4) yes N2 H2 N12 . 0.97(4) 2.70(5) 3.061(5) 103(3) yes N3 H3B N31 . 0.85(5) 2.39(5) 3.194(5) 159(4) yes N3 H3A N21 2_545 0.88(5) 2.35(5) 3.189(5) 161(4) yes _cod_database_fobs_code 2012978