#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$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
'Černák, Juraj'
'Chomič, Jozef'
'Massa, Werner'
_publ_section_title
;
 Cu₂(dien)₂Ag₅(CN)₉ containing the one-dimensional polymeric
 cation [Cu(dien)Ag(CN)₂]ₙⁿ+ and the unusual
 [Ag₂(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_paper_doi               10.1107/S0108270102013240
_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[[μ-cyano-1:2κ²C:N-diethylenetriamine-
2κ³N-copper(II)silver(I)]-μ-cyano-1:2'κ²C: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       φ
_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/[σ²(Fo²)+(0.0352P)²] where P=(Fo²+2Fc²)/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>2σ(I)
_cod_data_source_file            gg1124.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2012978
_cod_database_fobs_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_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_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_
_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
