#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:25:49 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179327 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/24/4322422.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_4322422
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            'C28 H20 Cu6 N14'
_chemical_formula_weight         933.82
_chemical_name_systematic
; 
 ? 
;
_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                 106.8690(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.75820(10)
_cell_length_b                   17.1622(2)
_cell_length_c                   9.901
_cell_measurement_temperature    115(2)
_cell_volume                     1586.79(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_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  0.0217
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9873
_diffrn_reflns_theta_full        28.20
_diffrn_reflns_theta_max         28.20
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    3.994
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             920
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         3731
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0214P)²+1.6887P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0574
_refine_ls_wR_factor_ref         0.0594
_reflns_number_gt                3284
_reflns_number_total             3731
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990385q_3.cif
_cod_data_source_block           '[Cu3(CN)2(trz)(2,2'-bpy)]'
_cod_original_cell_volume        1586.86(2)
_cod_database_code               4322422
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_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 0.37686(3) 0.082146(16) 0.98399(3) 0.01497(7) Uani 1 1 d . . .
Cu2 Cu -0.07569(3) 0.217760(17) 0.93701(3) 0.01679(7) Uani 1 1 d . . .
Cu3 Cu -0.44290(3) 0.421481(16) 0.81701(3) 0.01731(7) Uani 1 1 d . . .
N5 N 0.5804(2) 0.09442(11) 1.0067(2) 0.0145(4) Uani 1 1 d . . .
N6 N 0.32432(19) -0.03226(11) 0.97747(19) 0.0145(4) Uani 1 1 d . . .
N7 N -0.2089(2) 0.14181(11) 0.9970(2) 0.0158(4) Uani 1 1 d . . .
N8 N -0.6489(2) 0.43949(11) 0.81335(19) 0.0164(4) Uani 1 1 d . . .
N9 N -0.4410(2) 0.54057(11) 0.82878(19) 0.0155(4) Uani 1 1 d . . .
C1 C -0.1988(2) 0.30620(12) 0.8802(2) 0.0149(4) Uani 0.50 1 d P . .
N1 N -0.1988(2) 0.30620(12) 0.8802(2) 0.0149(4) Uani 0.50 1 d P . .
C2 C -0.2925(2) 0.35004(13) 0.8510(2) 0.0216(5) Uani 0.50 1 d P . .
N2 N -0.2925(2) 0.35004(13) 0.8510(2) 0.0216(5) Uani 0.50 1 d P . .
C3 C 0.1067(2) 0.17838(13) 0.9467(2) 0.0195(4) Uani 0.50 1 d P . .
N3 N 0.1067(2) 0.17838(13) 0.9467(2) 0.0195(4) Uani 0.50 1 d P . .
C4 C 0.2140(2) 0.14637(12) 0.9593(2) 0.0179(4) Uani 0.50 1 d P . .
N4 N 0.2140(2) 0.14637(12) 0.9593(2) 0.0179(4) Uani 0.50 1 d P . .
C5 C 0.6540(2) 0.15729(14) 0.9920(2) 0.0154(4) Uani 1 1 d . . .
C6 C 0.2024(2) -0.06365(14) 0.9839(2) 0.0162(4) Uani 1 1 d . . .
C11 C -0.7495(3) 0.38476(15) 0.8064(3) 0.0208(5) Uani 1 1 d . . .
C12 C -0.8869(3) 0.40155(16) 0.8103(3) 0.0241(5) Uani 1 1 d . . .
C13 C -0.9223(3) 0.47891(17) 0.8228(3) 0.0248(5) Uani 1 1 d . . .
C14 C -0.8197(3) 0.53658(15) 0.8322(2) 0.0205(5) Uani 1 1 d . . .
C15 C -0.6837(2) 0.51530(13) 0.8265(2) 0.0151(4) Uani 1 1 d . . .
C16 C -0.5663(2) 0.57264(13) 0.8344(2) 0.0142(4) Uani 1 1 d . . .
C17 C -0.5814(3) 0.65305(14) 0.8461(2) 0.0181(5) Uani 1 1 d . . .
C18 C -0.4651(3) 0.70126(14) 0.8530(2) 0.0203(5) Uani 1 1 d . . .
C19 C -0.3367(3) 0.66838(15) 0.8474(3) 0.0206(5) Uani 1 1 d . . .
C20 C -0.3293(3) 0.58812(14) 0.8348(2) 0.0189(5) Uani 1 1 d . . .
H5 H 0.611(3) 0.2075(15) 0.973(3) 0.008(6) Uiso 1 1 d . . .
H19 H -0.252(3) 0.6984(16) 0.860(3) 0.019(7) Uiso 1 1 d . . .
H17 H -0.673(3) 0.6767(16) 0.850(3) 0.018(7) Uiso 1 1 d . . .
H20 H -0.243(3) 0.5627(15) 0.825(3) 0.017(7) Uiso 1 1 d . . .
H14 H -0.841(3) 0.5905(17) 0.842(3) 0.021(7) Uiso 1 1 d . . .
H18 H -0.471(3) 0.7570(19) 0.864(3) 0.029(8) Uiso 1 1 d . . .
H12 H -0.957(3) 0.362(2) 0.797(3) 0.036(9) Uiso 1 1 d . . .
H6 H 0.120(3) -0.0344(18) 0.978(3) 0.028(8) Uiso 1 1 d . . .
H13 H -1.010(4) 0.4942(19) 0.826(3) 0.038(9) Uiso 1 1 d . . .
H11 H -0.723(4) 0.337(2) 0.799(4) 0.041(9) Uiso 1 1 d . . .
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
C4 Cu1 N5 138.07(9) . . ?
C4 Cu1 N6 111.43(8) . . ?
N5 Cu1 N6 110.45(7) . . ?
C3 Cu2 C1 143.45(9) . . ?
C3 Cu2 N7 115.34(8) . . ?
C1 Cu2 N7 101.11(8) . . ?
C2 Cu3 N8 145.95(9) . . ?
C2 Cu3 N9 130.68(9) . . ?
N8 Cu3 N9 80.87(8) . . ?
C5 N5 N6 105.71(18) . 3_657 ?
C5 N5 Cu1 129.95(16) . . ?
N6 N5 Cu1 123.75(15) 3_657 . ?
C6 N6 N5 105.21(18) . 3_657 ?
C6 N6 Cu1 127.98(15) . . ?
N5 N6 Cu1 125.74(14) 3_657 . ?
C5 N7 C6 101.91(19) 1_455 3_557 ?
C5 N7 Cu2 124.75(16) 1_455 . ?
C6 N7 Cu2 131.53(16) 3_557 . ?
C11 N8 C15 118.3(2) . . ?
C11 N8 Cu3 126.88(17) . . ?
C15 N8 Cu3 114.75(15) . . ?
C20 N9 C16 118.6(2) . . ?
C20 N9 Cu3 126.93(16) . . ?
C16 N9 Cu3 114.44(15) . . ?
C2 C1 Cu2 166.8(2) . . ?
C1 C2 Cu3 176.0(2) . . ?
C4 C3 Cu2 171.9(2) . . ?
C3 C4 Cu1 172.5(2) . . ?
N5 C5 N7 113.4(2) . 1_655 ?
N6 C6 N7 113.8(2) . 3_557 ?
N8 C11 C12 123.5(2) . . ?
C11 C12 C13 118.1(2) . . ?
C12 C13 C14 119.6(2) . . ?
C13 C14 C15 119.1(2) . . ?
N8 C15 C14 121.5(2) . . ?
N8 C15 C16 115.18(19) . . ?
C14 C15 C16 123.4(2) . . ?
N9 C16 C17 121.5(2) . . ?
N9 C16 C15 114.65(19) . . ?
C17 C16 C15 123.9(2) . . ?
C18 C17 C16 119.2(2) . . ?
C17 C18 C19 119.3(2) . . ?
C20 C19 C18 118.5(2) . . ?
N9 C20 C19 122.9(2) . . ?
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 C4 1.891(2) . ?
Cu1 N5 1.9447(19) . ?
Cu1 N6 2.0256(19) . ?
Cu2 C3 1.880(2) . ?
Cu2 C1 1.916(2) . ?
Cu2 N7 2.047(2) . ?
Cu3 C2 1.867(2) . ?
Cu3 N8 2.024(2) . ?
Cu3 N9 2.047(2) . ?
N5 C5 1.327(3) . ?
N5 N6 1.394(3) 3_657 ?
N6 C6 1.325(3) . ?
N6 N5 1.394(3) 3_657 ?
N7 C5 1.351(3) 1_455 ?
N7 C6 1.354(3) 3_557 ?
N8 C11 1.346(3) . ?
N8 C15 1.361(3) . ?
N9 C20 1.348(3) . ?
N9 C16 1.357(3) . ?
C1 C2 1.154(3) . ?
C3 C4 1.157(3) . ?
C5 N7 1.351(3) 1_655 ?
C6 N7 1.354(3) 3_557 ?
C11 C12 1.383(4) . ?
C12 C13 1.386(4) . ?
C13 C14 1.391(4) . ?
C14 C15 1.393(3) . ?
C15 C16 1.495(3) . ?
C16 C17 1.396(3) . ?
C17 C18 1.390(4) . ?
C18 C19 1.390(3) . ?
C19 C20 1.387(3) . ?
