#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/33/2013381.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_2013381
loop_
_publ_author_name
'Potočňák, Ivan'
'Triščíková, Ľubica'
'Wagner, Christoph'
_publ_section_title
;
 Low-dimensional compounds containing cyano groups. VI. A unique two-
 and one-dimensional structure in
 amminebis(1,4-diaminobutane)tetrakis[dicyanoargentato(I)]dicopper(II)
 dihydrate
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m249
_journal_page_last               m251
_journal_paper_doi               10.1107/S0108270103010151
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Cu2 Ag4 (CN)8 (C4 H12 N2)2 (N H3)], 2H2 O'
_chemical_formula_moiety         'C16 H27 Ag4 Cu2 N13, 2H2 O'
_chemical_formula_sum            'C16 H31 Ag4 Cu2 N13 O2'
_chemical_formula_weight         996.10
_chemical_name_systematic
;amminebis(1,4-diaminobutane)tetrakis[dicyanoargentato(I)]dicopper(II)
 dihydrate
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.84(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.862(6)
_cell_length_b                   16.541(5)
_cell_length_c                   10.210(12)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.64
_cell_measurement_theta_min      8.05
_cell_volume                     1523(2)
_computing_cell_refinement
;
STADI4 Diffractometer Control and Data Collection Software 1.06
;
_computing_data_collection
;
STADI4 Diffractometer Control and Data Collection Software 1.06 (Stoe & Cie,
1996)
;
_computing_data_reduction
;
X-RED 1.07 STOE Data Reduction Program (Stoe & Cie, 1996)
;
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2000)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  STOE-STADI-IV
_diffrn_measurement_method       θ/2θ
_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  0.0615
_diffrn_reflns_av_sigmaI/netI    0.0565
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5248
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         2.26
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  '60 min'
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.928
_exptl_absorpt_correction_T_max  0.619
_exptl_absorpt_correction_T_min  0.422
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   'North et al., 1968'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.172
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.099
_refine_diff_density_min         -1.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         2694
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0422
_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/[σ²(Fo²)+(0.0564P)²+0.251P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1133
_reflns_number_gt                2160
_reflns_number_total             2694
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            tr1059.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               2013381
_cod_database_fobs_code          2013381
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, 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
Ag3 0.5000 0.64008(4) 0.2500 0.05118(19) Uani d S 1 . . Ag
C5 0.7169(6) 0.6243(4) 0.3987(6) 0.0442(14) Uani d . 1 . . C
N5 0.8258(6) 0.6069(4) 0.4806(6) 0.0604(16) Uani d . 1 . . N
Cu2 1.0000 0.58158(5) 0.7500 0.0434(3) Uani d S 1 . . Cu
N7 1.0000 0.7032(4) 0.7500 0.0422(16) Uani d S 1 . . N
H7A 0.9968 0.7211 0.6666 0.063 Uiso calc PR 0.50 . . H
H7B 1.0821 0.7211 0.8207 0.063 Uiso calc PR 0.50 . . H
H7C 0.9211 0.7211 0.7627 0.063 Uiso calc PR 0.50 . . H
N8 1.1556(4) 0.5788(3) 0.6668(5) 0.0383(11) Uani d . 1 . . N
H8A 1.1358 0.5361 0.6072 0.046 Uiso calc R 1 . . H
H8B 1.1443 0.6235 0.6132 0.046 Uiso calc R 1 . . H
C8 1.3128(5) 0.5738(3) 0.7673(6) 0.0345(12) Uani d . 1 . . C
H8C 1.3284 0.5236 0.8206 0.041 Uiso calc R 1 . . H
H8D 1.3347 0.6180 0.8352 0.041 Uiso calc R 1 . . H
C9 1.4190(5) 0.5772(3) 0.6954(6) 0.0369(13) Uani d . 1 . . C
H9A 1.4001 0.6257 0.6374 0.044 Uiso calc R 1 . . H
H9B 1.4023 0.5310 0.6323 0.044 Uiso calc R 1 . . H
N2 1.0000 0.4609(5) 0.7500 0.060(2) Uani d S 1 . . N
C2 1.0000 0.3927(5) 0.7500 0.059(2) Uani d S 1 . . C
Ag1 1.0000 0.26818(4) 0.7500 0.0665(2) Uani d S 1 . . Ag
C1 1.0000 0.1437(5) 0.7500 0.054(2) Uani d S 1 . . C
N1 1.0000 0.0748(4) 0.7500 0.0524(19) Uani d S 1 . . N
Cu1 1.0000 -0.04769(5) 0.7500 0.0270(2) Uani d S 1 . . Cu
N6 1.1606(4) -0.0491(3) 0.6761(5) 0.0309(9) Uani d . 1 . . N
H6A 1.1620 -0.0989 0.6412 0.037 Uiso calc R 1 . . H
H6B 1.1334 -0.0147 0.6016 0.037 Uiso calc R 1 . . H
C6 1.3148(5) -0.0287(3) 0.7738(6) 0.0331(12) Uani d . 1 . . C
H6C 1.3498 -0.0678 0.8512 0.040 Uiso calc R 1 . . H
H6D 1.3160 0.0241 0.8153 0.040 Uiso calc R 1 . . H
C7 1.4194(5) -0.0282(3) 0.6982(6) 0.0362(12) Uani d . 1 . . C
H7D 1.4002 -0.0755 0.6370 0.043 Uiso calc R 1 . . H
H7E 1.3999 0.0193 0.6378 0.043 Uiso calc R 1 . . H
N3 0.8740(4) -0.1142(3) 0.5746(5) 0.0393(11) Uani d . 1 . . N
C3 0.8083(6) -0.1494(4) 0.4724(6) 0.0399(13) Uani d . 1 . . C
Ag2 0.68400(5) -0.20290(3) 0.27767(5) 0.05431(15) Uani d . 1 . . Ag
C4 0.5614(7) -0.2239(4) 0.0646(7) 0.0477(15) Uani d . 1 . . C
N4 0.4936(7) -0.2296(4) -0.0562(6) 0.0607(15) Uani d . 1 . . N
O1 0.2491(5) 0.7724(3) 0.6635(5) 0.0539(11) Uani d D 1 . . O
H1W 0.306(4) 0.782(3) 0.743(2) 0.023(14) Uiso d D 1 . . H
H2W 0.299(3) 0.776(6) 0.619(3) 0.10(3) Uiso d 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'
O O 0.0106 0.0060 '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
C5 Ag3 C5 2_655 . 165.6(3) yes
C5 Ag3 Ag2 2_655 1_565 124.10(17) ?
C5 Ag3 Ag2 . 1_565 69.45(18) ?
C5 Ag3 Ag2 2_655 2_665 69.45(18) ?
C5 Ag3 Ag2 . 2_665 124.10(17) ?
Ag2 Ag3 Ag2 1_565 2_665 67.02(4) ?
N5 C5 Ag3 . . 171.3(6) yes
N2 Cu2 N7 . . 180 yes
N2 Cu2 N8 . 2_756 88.69(13) ?
N7 Cu2 N8 . 2_756 91.31(13) ?
N2 Cu2 N8 . . 88.69(13) yes
N7 Cu2 N8 . . 91.31(13) yes
N8 Cu2 N8 2_756 . 177.4(3) yes
Cu2 N7 H7A . . 109.5 ?
Cu2 N7 H7B . . 109.5 ?
H7A N7 H7B . . 109.5 ?
Cu2 N7 H7C . . 109.5 ?
H7A N7 H7C . . 109.5 ?
H7B N7 H7C . . 109.5 ?
C8 N8 Cu2 . . 118.0(4) ?
C8 N8 H8A . . 107.8 ?
Cu2 N8 H8A . . 107.8 ?
C8 N8 H8B . . 107.8 ?
Cu2 N8 H8B . . 107.8 ?
H8A N8 H8B . . 107.2 ?
N8 C8 C9 . . 113.7(5) ?
N8 C8 H8C . . 108.8 ?
C9 C8 H8C . . 108.8 ?
N8 C8 H8D . . 108.8 ?
C9 C8 H8D . . 108.8 ?
H8C C8 H8D . . 107.7 ?
C8 C9 C9 . 2_856 111.8(6) ?
C8 C9 H9A . . 109.3 ?
C9 C9 H9A 2_856 . 109.3 ?
C8 C9 H9B . . 109.3 ?
C9 C9 H9B 2_856 . 109.3 ?
H9A C9 H9B . . 107.9 ?
C2 N2 Cu2 . . 180.0000(10) ?
N2 C2 Ag1 . . 180.0000(10) ?
C2 Ag1 C1 . . 180.000(2) ?
N1 C1 Ag1 . . 180.0000(10) ?
C1 N1 Cu1 . . 180.0000(10) ?
N6 Cu1 N6 2_756 . 178.7(3) yes
N6 Cu1 N1 2_756 . 90.66(13) ?
N6 Cu1 N1 . . 90.66(13) yes
N6 Cu1 N3 2_756 . 91.73(18) yes
N6 Cu1 N3 . . 87.55(18) yes
N1 Cu1 N3 . . 122.65(14) yes
N6 Cu1 N3 2_756 2_756 87.55(18) ?
N6 Cu1 N3 . 2_756 91.73(18) ?
N1 Cu1 N3 . 2_756 122.65(14) ?
N3 Cu1 N3 . 2_756 114.7(3) yes
C6 N6 Cu1 . . 119.7(3) ?
C6 N6 H6A . . 107.4 ?
Cu1 N6 H6A . . 107.4 ?
C6 N6 H6B . . 107.4 ?
Cu1 N6 H6B . . 107.4 ?
H6A N6 H6B . . 106.9 ?
N6 C6 C7 . . 112.5(4) ?
N6 C6 H6C . . 109.1 ?
C7 C6 H6C . . 109.1 ?
N6 C6 H6D . . 109.1 ?
C7 C6 H6D . . 109.1 ?
H6C C6 H6D . . 107.8 ?
C7 C7 C6 2_856 . 112.5(6) ?
C7 C7 H7D 2_856 . 109.1 ?
C6 C7 H7D . . 109.1 ?
C7 C7 H7E 2_856 . 109.1 ?
C6 C7 H7E . . 109.1 ?
H7D C7 H7E . . 107.8 ?
C3 N3 Cu1 . . 175.8(5) ?
N3 C3 Ag2 . . 174.7(5) ?
C4 Ag2 C3 . . 164.0(2) ?
C4 Ag2 Ag3 . 1_545 71.96(17) ?
C3 Ag2 Ag3 . 1_545 122.80(16) ?
N4 C4 Ag2 . . 174.9(6) ?
H1W O1 H2W . . 103(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
Ag3 C5 2_655 2.080(6) ?
Ag3 C5 . 2.080(6) yes
Ag3 Ag2 1_565 3.1152(12) yes
Ag3 Ag2 2_665 3.1152(12) ?
C5 N5 . 1.099(7) yes
Cu2 N2 . 1.997(8) yes
Cu2 N7 . 2.011(6) yes
Cu2 N8 2_756 2.033(4) ?
Cu2 N8 . 2.033(4) yes
N7 H7A . 0.8900 ?
N7 H7B . 0.8900 ?
N7 H7C . 0.8900 ?
N8 C8 . 1.475(6) ?
N8 H8A . 0.9000 ?
N8 H8B . 0.9000 ?
C8 C9 . 1.503(7) ?
C8 H8C . 0.9700 ?
C8 H8D . 0.9700 ?
C9 C9 2_856 1.535(10) ?
C9 H9A . 0.9700 ?
C9 H9B . 0.9700 ?
N2 C2 . 1.128(11) yes
C2 Ag1 . 2.059(8) yes
Ag1 C1 . 2.059(8) yes
C1 N1 . 1.140(11) yes
N1 Cu1 . 2.026(7) yes
Cu1 N6 2_756 2.011(4) ?
Cu1 N6 . 2.011(4) yes
Cu1 N3 . 2.040(5) yes
Cu1 N3 2_756 2.040(5) ?
N6 C6 . 1.482(6) ?
N6 H6A . 0.9000 ?
N6 H6B . 0.9000 ?
C6 C7 . 1.517(7) ?
C6 H6C . 0.9700 ?
C6 H6D . 0.9700 ?
C7 C7 2_856 1.511(9) ?
C7 H7D . 0.9700 ?
C7 H7E . 0.9700 ?
N3 C3 . 1.141(7) yes
C3 Ag2 . 2.066(6) yes
Ag2 C4 . 2.047(7) yes
Ag2 Ag3 1_545 3.1152(12) ?
C4 N4 . 1.144(8) yes
O1 H1W . 0.795(10) ?
O1 H2W . 0.799(10) ?
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_site_symmetry_4
_geom_torsion
N2 Cu2 N8 C8 . . -87.1(4)
N7 Cu2 N8 C8 . . 92.9(4)
Cu2 N8 C8 C9 . . -176.4(3)
N8 C8 C9 C9 . 2_856 176.4(3)
N1 Cu1 N6 C6 . . 74.4(4)
N3 Cu1 N6 C6 . . -162.9(4)
N3 Cu1 N6 C6 2_756 . -48.3(4)
Cu1 N6 C6 C7 . . -176.8(4)
N6 C6 C7 C7 . 2_856 -165.7(3)
