#------------------------------------------------------------------------------
#$Date: 2020-07-22 08:31:12 +0300 (Wed, 22 Jul 2020) $
#$Revision: 254476 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/86/1558656.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_1558656
loop_
_publ_author_name
'Corfield, Peter W. R.'
'Stavola, Thomas James'
_publ_section_title
;
 Poly[diethylammonium
 [tetra-μ₂-cyanido-κ⁸C:N-tricuprate(I)]], a
 two-dimensional network solid
;
_journal_coeditor_code           PK4028
_journal_issue                   7
_journal_name_full               IUCrData
_journal_page_first              x200968
_journal_paper_doi               10.1107/S2414314620009682
_journal_volume                  5
_journal_year                    2020
_chemical_formula_iupac          '(C4 H12 N1) [Cu3 (C N)4]'
_chemical_formula_moiety         'C4 H12 N1 +, Cu3 C4 N4  -'
_chemical_formula_sum            'C8 H12 Cu3 N5'
_chemical_formula_weight         368.85
_chemical_name_systematic
;
Poly[diethylammonium
[tetra-μ₂-cyanido-κ⁸C:N-tricuprate(I)]]
;
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 120.444(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.6825(8)
_cell_length_b                   8.3355(5)
_cell_length_c                   7.2205(5)
_cell_measurement_reflns_used    791
_cell_measurement_temperature    302(2)
_cell_measurement_theta_max      27.41
_cell_measurement_theta_min      3.28
_cell_volume                     658.07(8)
_computing_cell_refinement
;
SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
KappaCCD Server Software (Nonius, 1997)
;
_computing_data_reduction
;
DENZO and SCALEPACK (Otwinowski & Minor,1997)
;
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 for Windows  (Farrugia,
2012)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2017/1 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      302(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Enraf--Nonius KappaCCD'
_diffrn_measurement_method       'combination of ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2500
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         27.412
_diffrn_reflns_theta_min         3.272
_exptl_absorpt_coefficient_mu    4.783
_exptl_absorpt_correction_T_max  0.68
_exptl_absorpt_correction_T_min  0.51
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(Otwinowski & Minor,1997)
;
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.861
_exptl_crystal_density_meas      1.840(10)
_exptl_crystal_density_method    'flotation in CCl4/dibromoethane mixtures'
_exptl_crystal_description       ' irregular block'
_exptl_crystal_F_000             364
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.216
_refine_diff_density_min         -0.290
_refine_ls_abs_structure_details
;
 Twinning involves reflection, so the Flack parameter of 0.13 (5)
 implies the presence of a small amount of the inverted form
;
_refine_ls_abs_structure_Flack   0.13(5)
_refine_ls_extinction_coef       0.015(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2017/1 (Sheldrick 2015)
;
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         1487
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0210P)²+0.7300P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0623
_refine_ls_wR_factor_ref         0.0692
_reflns_number_gt                1191
_reflns_number_total             1487
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            pk4028sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               1558656
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.534
_shelx_estimated_absorpt_t_max   0.701
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
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_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu Cu1 0.000000 0.0002(2) 0.000000 0.0860(6) Uani d 1 . .
Cu Cu2 0.18717(6) -0.02348(14) 0.78258(9) 0.0636(3) Uani d 1 . .
C C1 0.1211(4) -0.0060(10) 0.4775(7) 0.0605(12) Uani d 0.5 . .
N N1A 0.1211(4) -0.0060(10) 0.4775(7) 0.0605(12) Uani d 0.5 . .
N N1 0.0777(4) -0.0015(11) 0.2956(8) 0.0683(16) Uani d 0.5 . .
C C1A 0.0777(4) -0.0015(11) 0.2956(8) 0.0683(16) Uani d 0.5 . .
C C2A 0.2142(6) 0.1819(7) 0.9323(10) 0.066(2) Uani d 0.22(8) . .
N N2 0.2142(6) 0.1819(7) 0.9323(10) 0.066(2) Uani d 0.78(8) . .
N N2A 0.2525(7) 0.2919(8) 1.0428(11) 0.064(2) Uani d 0.22(8) . .
C C2 0.2525(7) 0.2919(8) 1.0428(11) 0.064(2) Uani d 0.78(8) . .
N N3 0.000000 0.3473(8) 0.500000 0.0606(17) Uani d 1 . .
H H3 0.033(6) 0.277(6) 0.606(8) 0.09(2) Uiso d 1 . .
C C31 0.0968(5) 0.4390(8) 0.4846(11) 0.071(2) Uani d 1 . .
H H31A 0.140222 0.506523 0.610650 0.106 Uiso calc 1 . .
H H31B 0.155145 0.363683 0.484731 0.106 Uiso calc 1 . .
C C32 0.0488(8) 0.5391(14) 0.2931(14) 0.118(4) Uani d 1 . .
H H32A 0.115278 0.590203 0.288774 0.177 Uiso calc 1 . .
H H32B -0.004388 0.619311 0.297044 0.177 Uiso calc 1 . .
H H32C 0.003720 0.473602 0.167536 0.177 Uiso calc 1 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
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'
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
N1 Cu1 N1 2 . 179.1(6) ?
N2A Cu2 C1 4_547 . 128.3(3) ?
N2A Cu2 N2 4_547 . 116.4(2) ?
C1 Cu2 N2 . . 114.7(3) ?
N1 C1 Cu2 . . 176.5(6) ?
C1 N1 Cu1 . . 176.8(6) ?
C2 N2 Cu2 . . 167.0(6) ?
N2 C2 Cu2 . 4_557 178.3(5) ?
C31 N3 C31 . 2_556 118.6(7) ?
C31 N3 H3 . . 111(5) ?
C31 N3 H3 2_556 . 109(5) ?
C32 C31 N3 . . 113.5(5) ?
C32 C31 H31A . . 108.9 ?
N3 C31 H31A . . 108.9 ?
C32 C31 H31B . . 108.9 ?
N3 C31 H31B . . 108.9 ?
H31A C31 H31B . . 107.7 ?
C31 C32 H32A . . 109.5 ?
C31 C32 H32B . . 109.5 ?
H32A C32 H32B . . 109.5 ?
C31 C32 H32C . . 109.5 ?
H32A C32 H32C . . 109.5 ?
H32B C32 H32C . . 109.5 ?
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
Cu1 N1 2 1.842(5) ?
Cu1 N1 . 1.842(5) ?
Cu2 N2A 4_547 1.889(7) ?
Cu2 C1 . 1.925(4) ?
Cu2 N2 . 1.960(7) ?
C1 N1 . 1.139(6) ?
N2 C2 . 1.149(7) ?
N3 C31 . 1.497(7) ?
N3 C31 2_556 1.497(7) ?
N3 H3 . 0.885(14) ?
C31 C32 . 1.457(10) ?
C31 H31A . 0.9700 ?
C31 H31B . 0.9700 ?
C32 H32A . 0.9600 ?
C32 H32B . 0.9600 ?
C32 H32C . 0.9600 ?
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
N3 H3 N2 . 0.885(14) 2.44(4) 3.230(6) 149(6) yes

_cod_database_fobs_code 1558656
