#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/84/2018404.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_2018404
loop_
_publ_author_name
'Jia, Li-Na'
'Hou, Lei'
_publ_section_title
;
 Poly[tetraamminecopper(II)
 bis[tris(μ₂-cyanido-κ²C,N)dicuprate(I)]]: a unique
 CuI--CuII mixed-valence complex containing anionic cuprous cyanide
 layers and [Cu(NH₃)₄]²⁺ cations
;
_journal_coeditor_code           WQ3010
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m45
_journal_page_last               m47
_journal_paper_doi               10.1107/S0108270112002429
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Cu (N H3)4] [Cu (C N)3]'
_chemical_formula_moiety         'Cu H12 N4 2+, 2(C3 Cu2 N3 -)'
_chemical_formula_sum            'C6 H12 Cu5 N10'
_chemical_formula_weight         541.96
_chemical_name_systematic
;
Poly[tetraamminecopper(II) bis[tris(μ₂-cyanido-
κ²C,N)dicuprate(I)]]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 123.086(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.6501(9)
_cell_length_b                   8.9083(10)
_cell_length_c                   13.2509(12)
_cell_measurement_reflns_used    1643
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.32
_cell_measurement_theta_min      2.93
_cell_volume                     756.61(15)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2005)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
;
Bruker SMART APEX area-detector
;
_diffrn_measurement_method       'φ and ω 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  0.0197
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3397
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    6.918
_exptl_absorpt_correction_T_max  0.5166
_exptl_absorpt_correction_T_min  0.3532
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    2.379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             526
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.751
_refine_diff_density_min         -0.442
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         1479
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0493P)²+0.5775P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0943
_reflns_number_gt                1261
_reflns_number_total             1479
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            wq3010.cif
_cod_data_source_block           I
_cod_original_cell_volume        756.61(14)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2018404
_cod_database_fobs_code          2018404
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_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_symmetry_multiplicity
Cu Cu1 0.86771(7) 0.59343(5) 0.31346(4) 0.04692(19) Uani d . 1 1
Cu Cu2 0.17894(8) 0.40406(5) -0.02790(5) 0.0523(2) Uani d . 1 1
N N1 0.4450(5) 0.4664(4) 0.1178(3) 0.0550(9) Uani d . 1 1
N N2 1.0584(5) 0.4212(3) 0.3998(3) 0.0463(8) Uani d . 1 1
N N3 1.0300(5) 0.9123(4) 0.3907(3) 0.0488(8) Uani d . 1 1
C C1 0.6004(5) 0.5134(4) 0.1958(3) 0.0424(8) Uani d . 1 1
C C2 1.1100(5) 0.3001(4) 0.4260(3) 0.0403(8) Uani d . 1 1
C C3 0.9665(5) 0.7933(4) 0.3571(3) 0.0363(7) Uani d . 1 1
Cu Cu3 0.5000 1.0000 0.0000 0.0386(2) Uani d S 1 2
N N4 0.6351(5) 1.1244(4) 0.1529(3) 0.0471(7) Uani d . 1 1
H H4C 0.6854 1.2088 0.1423 0.071 Uiso calc R 1 1
H H4A 0.7387 1.0723 0.2134 0.071 Uiso calc R 1 1
H H4B 0.5405 1.1465 0.1700 0.071 Uiso calc R 1 1
N N5 0.4292(6) 0.8440(4) 0.0816(3) 0.0523(8) Uani d . 1 1
H H5A 0.3624 0.7682 0.0311 0.078 Uiso calc R 1 1
H H5B 0.3478 0.8845 0.1031 0.078 Uiso calc R 1 1
H H5C 0.5460 0.8103 0.1468 0.078 Uiso calc R 1 1
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'
Cu Cu 0.3201 1.2651 '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'
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
C3 Cu1 C1 . . 132.12(14)
C3 Cu1 N2 . . 120.18(13)
C1 Cu1 N2 . . 107.69(14)
C2 Cu2 N3 4_465 4_475 130.57(13)
C2 Cu2 N1 4_465 . 122.80(14)
N3 Cu2 N1 4_475 . 106.52(13)
C1 N1 Cu2 . . 173.4(4)
C2 N2 Cu1 . . 158.4(3)
C3 N3 Cu2 . 4_676 169.9(3)
N1 C1 Cu1 . . 173.8(4)
N2 C2 Cu2 . 4_666 175.5(4)
N3 C3 Cu1 . . 175.7(3)
N5 Cu3 N5 . 3_675 180.0000(10)
N5 Cu3 N4 . . 88.87(14)
N5 Cu3 N4 3_675 . 91.13(14)
N5 Cu3 N4 . 3_675 91.13(14)
N5 Cu3 N4 3_675 3_675 88.87(14)
N4 Cu3 N4 . 3_675 180.0
Cu3 N4 H4C . . 109.5
Cu3 N4 H4A . . 109.5
H4C N4 H4A . . 109.5
Cu3 N4 H4B . . 109.5
H4C N4 H4B . . 109.5
H4A N4 H4B . . 109.5
Cu3 N5 H5A . . 109.5
Cu3 N5 H5B . . 109.5
H5A N5 H5B . . 109.5
Cu3 N5 H5C . . 109.5
H5A N5 H5C . . 109.5
H5B N5 H5C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Cu1 C3 . 1.897(3)
Cu1 C1 . 1.907(3)
Cu1 N2 . 1.992(3)
Cu2 C2 4_465 1.899(4)
Cu2 N3 4_475 1.949(3)
Cu2 N1 . 1.972(4)
N1 C1 . 1.147(5)
N2 C2 . 1.136(4)
N3 C3 . 1.149(4)
N3 Cu2 4_676 1.949(3)
C2 Cu2 4_666 1.899(4)
Cu3 N5 . 2.008(3)
Cu3 N5 3_675 2.008(3)
Cu3 N4 . 2.028(3)
Cu3 N4 3_675 2.028(3)
N4 H4C . 0.8900
N4 H4A . 0.8900
N4 H4B . 0.8900
N5 H5A . 0.8900
N5 H5B . 0.8900
N5 H5C . 0.8900
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
N4 H4A N3 0.89 2.61 3.498(5) 177.5
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
C2 Cu2 N1 C1 4_465 . 136(3)
N3 Cu2 N1 C1 4_475 . -40(3)
C3 Cu1 N2 C2 . . 175.4(9)
C1 Cu1 N2 C2 . . -3.7(10)
Cu2 N1 C1 Cu1 . . -42(6)
C3 Cu1 C1 N1 . . 86(3)
N2 Cu1 C1 N1 . . -95(3)
Cu1 N2 C2 Cu2 . 4_666 -54(5)
Cu2 N3 C3 Cu1 4_676 . 43(6)
C1 Cu1 C3 N3 . . 123(4)
N2 Cu1 C3 N3 . . -56(5)
