#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:25:49 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179327 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/24/4322421.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4322421
loop_
_publ_author_name
'Douglas J. Chesnut'
'Anakarin Kusnetzow'
'Robert Birge'
'Jon Zubieta'
_publ_section_title
;
 Ligand Influences on Copper Cyanide Solid-State Architecture: Flattened
 and Fused "Slinky", Corrugated Sheet, and Ribbon Motifs in the
 Copper-Cyanide-Triazolate-Organoamine Family
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5484
_journal_page_last               5494
_journal_paper_doi               10.1021/ic990385q
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C34 H24 Cu10 N22'
_chemical_formula_weight         1376.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.2060(10)
_cell_angle_beta                 90.4920(10)
_cell_angle_gamma                112.5340(10)
_cell_formula_units_Z            1
_cell_length_a                   9.1183(5)
_cell_length_b                   9.9838(6)
_cell_length_c                   12.7545(8)
_cell_measurement_temperature    115(2)
_cell_volume                     1068.72(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.902
_diffrn_measured_fraction_theta_max 0.902
_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  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6913
_diffrn_reflns_theta_full        28.22
_diffrn_reflns_theta_max         28.22
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    4.925
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_density_diffrn    2.138
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             672
_refine_diff_density_max         0.817
_refine_diff_density_min         -0.938
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       0.0033(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         4751
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0615P)²+1.5764P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1113
_reflns_number_gt                3921
_reflns_number_total             4751
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990385q_2.cif
_cod_data_source_block           '[Cu5(CN)3(trz)2(2,2'-bpy)]'
_cod_database_code               4322421
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu -0.5000 0.0000 -0.5000 0.01910(18) Uani 1 2 d S . .
Cu2 Cu -0.43673(6) 0.24993(6) -0.15198(4) 0.01938(14) Uani 1 1 d . . .
Cu3 Cu 0.18575(6) 0.36698(6) 0.07679(4) 0.01740(14) Uani 1 1 d . . .
Cu4 Cu -0.09322(6) 0.39354(6) 0.27217(4) 0.01572(14) Uani 1 1 d . . .
Cu5 Cu 0.5000 0.5000 0.5000 0.01627(16) Uani 1 2 d S . .
Cu6 Cu -0.61346(6) 0.20377(6) 0.42598(4) 0.01896(14) Uani 1 1 d . . .
N7 N -0.2648(4) 0.3020(4) -0.0411(3) 0.0189(7) Uani 1 1 d . . .
N8 N -0.0387(4) 0.3388(4) 0.0452(3) 0.0191(7) Uani 1 1 d . . .
N9 N -0.1418(4) 0.3595(4) 0.1174(3) 0.0179(7) Uani 1 1 d . . .
N10 N 0.2385(4) 0.4389(4) 0.2281(3) 0.0158(7) Uani 1 1 d . . .
N11 N 0.1364(4) 0.4603(4) 0.3007(3) 0.0161(7) Uani 1 1 d . . .
N12 N 0.3633(4) 0.4950(4) 0.3855(3) 0.0165(7) Uani 1 1 d . . .
C1 C -0.4600(5) 0.0982(4) -0.3685(3) 0.0173(8) Uani 0.50 1 d P . .
N1 N -0.4600(5) 0.0982(4) -0.3685(3) 0.0173(8) Uani 0.50 1 d P . .
C2 C -0.4456(5) 0.1578(5) -0.2864(3) 0.0243(9) Uani 0.50 1 d P . .
N2 N -0.4456(5) 0.1578(5) -0.2864(3) 0.0243(9) Uani 0.50 1 d P . .
C3 C -0.6017(5) 0.2920(5) -0.0789(3) 0.0189(8) Uani 0.50 1 d P . .
N3 N -0.6017(5) 0.2920(5) -0.0789(3) 0.0189(8) Uani 0.50 1 d P . .
C4 C 0.3164(5) 0.3201(5) -0.0200(3) 0.0278(9) Uani 0.50 1 d P . .
N4 N 0.3164(5) 0.3201(5) -0.0200(3) 0.0278(9) Uani 0.50 1 d P . .
C5 C -0.2782(4) 0.3318(4) 0.3518(3) 0.0157(7) Uani 0.50 1 d P . .
N5 N -0.2782(4) 0.3318(4) 0.3518(3) 0.0157(7) Uani 0.50 1 d P . .
C6 C -0.4030(5) 0.2793(4) 0.3859(3) 0.0217(8) Uani 0.50 1 d P . .
N6 N -0.4030(5) 0.2793(4) 0.3859(3) 0.0217(8) Uani 0.50 1 d P . .
C7 C -0.1153(5) 0.3053(5) -0.0464(3) 0.0198(9) Uani 1 1 d . . .
H7 H -0.0716 0.2858 -0.1085 0.024 Uiso 1 1 calc R . .
C8 C -0.2731(5) 0.3368(5) 0.0618(3) 0.0203(9) Uani 1 1 d . . .
H8 H -0.3630 0.3443 0.0911 0.024 Uiso 1 1 calc R . .
C9 C 0.3719(5) 0.4613(5) 0.2819(3) 0.0172(8) Uani 1 1 d . . .
H9 H 0.4615 0.4545 0.2516 0.021 Uiso 1 1 calc R . .
C10 C 0.2159(5) 0.4947(4) 0.3928(3) 0.0150(8) Uani 1 1 d . . .
H10 H 0.1745 0.5161 0.4553 0.018 Uiso 1 1 calc R . .
N13 N -0.8101(4) 0.1135(4) 0.3226(3) 0.0201(7) Uani 1 1 d . . .
N14 N -0.7843(4) 0.2032(4) 0.5249(3) 0.0176(7) Uani 1 1 d . . .
C11 C -0.8129(6) 0.0666(5) 0.2217(4) 0.0258(10) Uani 1 1 d . . .
H11 H -0.7212 0.0603 0.1945 0.031 Uiso 1 1 calc R . .
C12 C -0.9471(6) 0.0269(5) 0.1557(4) 0.0285(10) Uani 1 1 d . . .
H12 H -0.9445 -0.0039 0.0854 0.034 Uiso 1 1 calc R . .
C13 C -1.0840(6) 0.0336(5) 0.1954(4) 0.0287(10) Uani 1 1 d . . .
H13 H -1.1755 0.0065 0.1526 0.034 Uiso 1 1 calc R . .
C14 C -1.0834(6) 0.0823(5) 0.3019(4) 0.0239(9) Uani 1 1 d . . .
H14 H -1.1741 0.0885 0.3308 0.029 Uiso 1 1 calc R . .
C15 C -0.9433(5) 0.1211(4) 0.3631(3) 0.0176(8) Uani 1 1 d . . .
C16 C -0.9279(5) 0.1740(4) 0.4768(3) 0.0169(8) Uani 1 1 d . . .
C17 C -1.0519(5) 0.1936(5) 0.5306(4) 0.0200(9) Uani 1 1 d . . .
H17 H -1.1498 0.1723 0.4966 0.024 Uiso 1 1 calc R . .
C18 C -1.0260(5) 0.2457(5) 0.6363(4) 0.0216(9) Uani 1 1 d . . .
H18 H -1.1066 0.2602 0.6737 0.026 Uiso 1 1 calc R . .
C19 C -0.8790(6) 0.2759(5) 0.6853(4) 0.0219(9) Uani 1 1 d . . .
H19 H -0.8593 0.3109 0.7557 0.026 Uiso 1 1 calc R . .
C20 C -0.7618(5) 0.2527(5) 0.6267(3) 0.0188(8) Uani 1 1 d . . .
H20 H -0.6635 0.2724 0.6596 0.023 Uiso 1 1 calc R . .
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Cu1 N1 180.000(1) . 2_454 ?
C1 Cu1 C1 180.000(1) . 2_454 ?
N1 Cu1 C1 0.00(12) 2_454 2_454 ?
C1 Cu1 Cu6 90.30(12) . 1_554 ?
N1 Cu1 Cu6 89.70(12) 2_454 1_554 ?
C1 Cu1 Cu6 89.70(12) 2_454 1_554 ?
C1 Cu1 Cu6 89.70(12) . 2_455 ?
N1 Cu1 Cu6 90.30(12) 2_454 2_455 ?
C1 Cu1 Cu6 90.30(12) 2_454 2_455 ?
Cu6 Cu1 Cu6 180.0 1_554 2_455 ?
C2 Cu2 C3 129.07(17) . . ?
C2 Cu2 N7 127.68(16) . . ?
C3 Cu2 N7 102.69(15) . . ?
C4 Cu3 N8 124.28(17) . . ?
C4 Cu3 N10 127.24(17) . . ?
N8 Cu3 N10 108.36(14) . . ?
C5 Cu4 N11 136.58(15) . . ?
C5 Cu4 N9 112.76(16) . . ?
N11 Cu4 N9 110.10(14) . . ?
N12 Cu5 N12 180.000(1) 2_666 . ?
N12 Cu5 Cu6 78.76(11) 2_666 2_566 ?
N12 Cu5 Cu6 101.24(11) . 2_566 ?
N12 Cu5 Cu6 101.24(11) 2_666 1_655 ?
N12 Cu5 Cu6 78.76(11) . 1_655 ?
Cu6 Cu5 Cu6 180.0 2_566 1_655 ?
C6 Cu6 N14 151.03(16) . . ?
C6 Cu6 N13 124.85(16) . . ?
N14 Cu6 N13 80.67(15) . . ?
C6 Cu6 Cu5 75.59(12) . 1_455 ?
N14 Cu6 Cu5 79.22(10) . 1_455 ?
N13 Cu6 Cu5 120.86(10) . 1_455 ?
C6 Cu6 Cu1 78.77(12) . 1_556 ?
N14 Cu6 Cu1 104.60(10) . 1_556 ?
N13 Cu6 Cu1 114.31(10) . 1_556 ?
Cu5 Cu6 Cu1 124.45(2) 1_455 1_556 ?
C8 N7 C7 102.0(3) . . ?
C8 N7 Cu2 127.4(3) . . ?
C7 N7 Cu2 130.6(3) . . ?
C7 N8 N9 106.6(3) . . ?
C7 N8 Cu3 127.9(3) . . ?
N9 N8 Cu3 125.4(3) . . ?
C8 N9 N8 104.9(3) . . ?
C8 N9 Cu4 131.4(3) . . ?
N8 N9 Cu4 123.4(3) . . ?
C9 N10 N11 105.8(3) . . ?
C9 N10 Cu3 127.3(3) . . ?
N11 N10 Cu3 126.6(3) . . ?
C10 N11 N10 106.3(3) . . ?
C10 N11 Cu4 128.6(3) . . ?
N10 N11 Cu4 122.8(3) . . ?
C10 N12 C9 103.1(3) . . ?
C10 N12 Cu5 125.9(3) . . ?
C9 N12 Cu5 129.7(3) . . ?
C2 C1 Cu1 175.5(4) . . ?
C1 C2 Cu2 176.2(4) . . ?
N4 C3 C4 0.0(6) 1_455 1_455 ?
N4 C3 Cu2 168.2(4) 1_455 . ?
C4 C3 Cu2 168.2(4) 1_455 . ?
N3 C4 C3 0.0(5) 1_655 1_655 ?
N3 C4 Cu3 179.3(4) 1_655 . ?
C3 C4 Cu3 179.3(4) 1_655 . ?
C6 C5 Cu4 168.8(4) . . ?
C5 C6 Cu6 172.5(4) . . ?
N8 C7 N7 112.7(4) . . ?
N9 C8 N7 113.7(4) . . ?
N10 C9 N12 112.5(4) . . ?
N11 C10 N12 112.3(4) . . ?
C11 N13 C15 119.1(4) . . ?
C11 N13 Cu6 127.4(3) . . ?
C15 N13 Cu6 113.0(3) . . ?
C20 N14 C16 118.7(4) . . ?
C20 N14 Cu6 125.9(3) . . ?
C16 N14 Cu6 114.2(3) . . ?
N13 C11 C12 122.6(5) . . ?
C13 C12 C11 119.3(5) . . ?
C12 C13 C14 118.9(4) . . ?
C15 C14 C13 118.4(4) . . ?
N13 C15 C14 121.7(4) . . ?
N13 C15 C16 114.9(4) . . ?
C14 C15 C16 123.4(4) . . ?
N14 C16 C17 121.7(4) . . ?
N14 C16 C15 115.6(4) . . ?
C17 C16 C15 122.7(4) . . ?
C18 C17 C16 118.7(4) . . ?
C19 C18 C17 119.4(4) . . ?
C18 C19 C20 118.5(4) . . ?
N14 C20 C19 122.9(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 C1 1.839(4) . ?
Cu1 N1 1.839(4) 2_454 ?
Cu1 C1 1.839(4) 2_454 ?
Cu1 Cu6 2.8247(5) 1_554 ?
Cu1 Cu6 2.8247(5) 2_455 ?
Cu2 C2 1.871(4) . ?
Cu2 C3 1.939(4) . ?
Cu2 N7 1.989(3) . ?
Cu3 C4 1.879(5) . ?
Cu3 N8 1.990(4) . ?
Cu3 N10 1.997(3) . ?
Cu4 C5 1.893(4) . ?
Cu4 N11 1.960(3) . ?
Cu4 N9 1.995(3) . ?
Cu5 N12 1.897(3) 2_666 ?
Cu5 N12 1.897(3) . ?
Cu5 Cu6 2.8173(6) 2_566 ?
Cu5 Cu6 2.8173(6) 1_655 ?
Cu6 C6 1.865(4) . ?
Cu6 N14 2.012(4) . ?
Cu6 N13 2.077(4) . ?
Cu6 Cu5 2.8173(6) 1_455 ?
Cu6 Cu1 2.8247(5) 1_556 ?
N7 C8 1.343(5) . ?
N7 C7 1.354(5) . ?
N8 C7 1.310(5) . ?
N8 N9 1.382(5) . ?
N9 C8 1.320(5) . ?
N10 C9 1.325(5) . ?
N10 N11 1.381(5) . ?
N11 C10 1.326(5) . ?
N12 C10 1.348(5) . ?
N12 C9 1.350(5) . ?
C1 C2 1.147(6) . ?
C3 N4 1.157(6) 1_455 ?
C3 C4 1.157(6) 1_455 ?
C4 N3 1.157(6) 1_655 ?
C4 C3 1.157(6) 1_655 ?
C5 C6 1.159(6) . ?
N13 C11 1.333(6) . ?
N13 C15 1.350(6) . ?
N14 C20 1.340(6) . ?
N14 C16 1.358(5) . ?
C11 C12 1.387(7) . ?
C12 C13 1.374(7) . ?
C13 C14 1.408(7) . ?
C14 C15 1.397(6) . ?
C15 C16 1.492(6) . ?
C16 C17 1.397(6) . ?
C17 C18 1.393(6) . ?
C18 C19 1.389(6) . ?
C19 C20 1.389(6) . ?
