#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:25:49 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179327 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/24/4322423.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_4322423
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            'C16 H10 Cu3 N7'
_chemical_formula_weight         490.93
_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                82.468(5)
_cell_angle_beta                 83.126(5)
_cell_angle_gamma                79.832(5)
_cell_formula_units_Z            4
_cell_length_a                   8.542(2)
_cell_length_b                   9.802(2)
_cell_length_c                   20.439(4)
_cell_measurement_temperature    115(2)
_cell_volume                     1661.7(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.911
_diffrn_measured_fraction_theta_max 0.911
_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  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0633
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            11003
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    3.819
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_density_diffrn    1.962
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             968
_refine_diff_density_max         1.156
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.148
_refine_ls_extinction_coef       0.0015(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         7529
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0575P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.1094
_reflns_number_gt                6193
_reflns_number_total             7529
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990385q_4.cif
_cod_data_source_block           '[Cu3(CN)2(trz)(1,10-phen)]'
_cod_database_code               4322423
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 0.88857(5) 0.15004(4) 0.45030(2) 0.01693(11) Uani 1 1 d . . .
Cu2 Cu 0.69491(6) 0.63737(4) 0.37658(2) 0.01764(11) Uani 1 1 d . . .
Cu3 Cu 0.76044(6) 0.97636(4) 0.14020(2) 0.01744(11) Uani 1 1 d . . .
Cu4 Cu 0.60585(6) 1.58710(4) 0.05037(2) 0.01681(11) Uani 1 1 d . . .
Cu5 Cu 0.45539(6) 1.02194(5) 0.22678(2) 0.02106(12) Uani 1 1 d . . .
Cu6 Cu 1.01890(6) 1.19839(5) 0.28790(2) 0.02508(13) Uani 1 1 d . . .
N9 N 0.8090(4) 0.7632(3) 0.41855(15) 0.0166(6) Uani 1 1 d . . .
N10 N 0.9667(4) 0.8446(3) 0.47859(15) 0.0167(6) Uani 1 1 d . . .
N11 N 0.8860(4) 0.9568(3) 0.44051(15) 0.0159(6) Uani 1 1 d . . .
N12 N 0.6937(4) 1.1561(3) 0.08091(15) 0.0161(6) Uani 1 1 d . . .
N13 N 0.5583(4) 1.3192(3) 0.01248(15) 0.0168(6) Uani 1 1 d . . .
N14 N 0.6355(4) 1.3857(3) 0.05154(14) 0.0142(6) Uani 1 1 d . . .
N15 N 0.3122(4) 1.0863(3) 0.15274(15) 0.0196(6) Uani 1 1 d . . .
N16 N 0.4579(4) 1.2326(3) 0.22202(15) 0.0172(6) Uani 1 1 d . . .
N17 N 1.0250(4) 1.4095(3) 0.28218(15) 0.0179(6) Uani 1 1 d . . .
N18 N 1.1833(4) 1.1880(3) 0.35172(15) 0.0165(6) Uani 1 1 d . . .
C1 C 0.7910(4) 0.3298(3) 0.42027(17) 0.0187(7) Uani 0.50 1 d P . .
N1 N 0.7910(4) 0.3298(3) 0.42027(17) 0.0187(7) Uani 0.50 1 d P . .
C2 C 0.7429(4) 0.4459(3) 0.40429(16) 0.0171(7) Uani 0.50 1 d P . .
N2 N 0.7429(4) 0.4459(3) 0.40429(16) 0.0171(7) Uani 0.50 1 d P . .
C3 C 0.5686(4) 0.7651(3) 0.31743(16) 0.0152(6) Uani 0.50 1 d P . .
N3 N 0.5686(4) 0.7651(3) 0.31743(16) 0.0152(6) Uani 0.50 1 d P . .
C4 C 0.5210(5) 0.8613(4) 0.28174(19) 0.0266(8) Uani 0.50 1 d P . .
N4 N 0.5210(5) 0.8613(4) 0.28174(19) 0.0266(8) Uani 0.50 1 d P . .
C5 C 0.6826(4) 0.7194(3) 0.09174(16) 0.0199(7) Uani 0.50 1 d P . .
N5 N 0.6826(4) 0.7194(3) 0.09174(16) 0.0199(7) Uani 0.50 1 d P . .
C6 C 0.7177(4) 0.8117(3) 0.11207(17) 0.0208(7) Uani 0.50 1 d P . .
N6 N 0.7177(4) 0.8117(3) 0.11207(17) 0.0208(7) Uani 0.50 1 d P . .
C7 C 0.8639(4) 1.0354(3) 0.20680(16) 0.0158(6) Uani 0.50 1 d P . .
N7 N 0.8639(4) 1.0354(3) 0.20680(16) 0.0158(6) Uani 0.50 1 d P . .
C8 C 0.9220(5) 1.0934(4) 0.24044(19) 0.0265(8) Uani 0.50 1 d P . .
N8 N 0.9220(5) 1.0934(4) 0.24044(19) 0.0265(8) Uani 0.50 1 d P . .
C9 C 0.9165(4) 0.7339(3) 0.46350(17) 0.0165(7) Uani 1 1 d . . .
H9 H 0.9523 0.6438 0.4822 0.020 Uiso 1 1 calc R . .
C10 C 0.7960(4) 0.9034(3) 0.40544(17) 0.0155(7) Uani 1 1 d . . .
H10 H 0.7307 0.9566 0.3750 0.019 Uiso 1 1 calc R . .
C11 C 0.5966(4) 1.1843(3) 0.03190(18) 0.0169(7) Uani 1 1 d . . .
H11 H 0.5599 1.1156 0.0134 0.020 Uiso 1 1 calc R . .
C12 C 0.7137(4) 1.2852(3) 0.09103(18) 0.0162(7) Uani 1 1 d . . .
H12 H 0.7760 1.3018 0.1225 0.019 Uiso 1 1 calc R . .
C13 C 0.2465(5) 1.0110(5) 0.1168(2) 0.0290(9) Uani 1 1 d . . .
H13 H 0.2689 0.9142 0.1245 0.035 Uiso 1 1 calc R . .
C14 C 0.1459(6) 1.0712(6) 0.0682(2) 0.0366(11) Uani 1 1 d . . .
H14 H 0.1030 1.0157 0.0438 0.044 Uiso 1 1 calc R . .
C15 C 0.1113(5) 1.2144(6) 0.0571(2) 0.0356(11) Uani 1 1 d . . .
H15 H 0.0444 1.2561 0.0248 0.043 Uiso 1 1 calc R . .
C16 C 0.1757(5) 1.2970(5) 0.09371(19) 0.0280(9) Uani 1 1 d . . .
C17 C 0.1498(6) 1.4467(5) 0.0843(2) 0.0364(11) Uani 1 1 d . . .
H17 H 0.0810 1.4938 0.0538 0.044 Uiso 1 1 calc R . .
C18 C 0.2237(6) 1.5203(4) 0.1189(2) 0.0355(12) Uani 1 1 d . . .
H18 H 0.2034 1.6172 0.1120 0.043 Uiso 1 1 calc R . .
C19 C 0.3329(5) 1.4531(4) 0.1663(2) 0.0269(9) Uani 1 1 d . . .
C20 C 0.4177(6) 1.5239(4) 0.2026(2) 0.0323(10) Uani 1 1 d . . .
H20 H 0.4051 1.6207 0.1967 0.039 Uiso 1 1 calc R . .
C21 C 0.5175(5) 1.4496(4) 0.2459(2) 0.0308(10) Uani 1 1 d . . .
H21 H 0.5745 1.4953 0.2696 0.037 Uiso 1 1 calc R . .
C22 C 0.5346(5) 1.3034(4) 0.25496(19) 0.0233(8) Uani 1 1 d . . .
H22 H 0.6026 1.2542 0.2854 0.028 Uiso 1 1 calc R . .
C23 C 0.3572(5) 1.3060(4) 0.17797(18) 0.0191(7) Uani 1 1 d . . .
C24 C 0.2789(5) 1.2273(4) 0.14097(18) 0.0206(8) Uani 1 1 d . . .
C25 C 0.9451(5) 1.5185(4) 0.24675(19) 0.0248(8) Uani 1 1 d . . .
H25 H 0.8770 1.5019 0.2175 0.030 Uiso 1 1 calc R . .
C26 C 0.9596(5) 1.6558(4) 0.2519(2) 0.0304(10) Uani 1 1 d . . .
H26 H 0.9024 1.7288 0.2263 0.036 Uiso 1 1 calc R . .
C27 C 1.0587(5) 1.6826(4) 0.2950(2) 0.0263(9) Uani 1 1 d . . .
H27 H 1.0691 1.7740 0.2989 0.032 Uiso 1 1 calc R . .
C28 C 1.1444(5) 1.5712(4) 0.33321(18) 0.0193(7) Uani 1 1 d . . .
C29 C 1.2526(5) 1.5872(4) 0.37935(19) 0.0227(8) Uani 1 1 d . . .
H29 H 1.2656 1.6763 0.3862 0.027 Uiso 1 1 calc R . .
C30 C 1.3361(5) 1.4750(4) 0.41300(19) 0.0233(8) Uani 1 1 d . . .
H30 H 1.4055 1.4885 0.4424 0.028 Uiso 1 1 calc R . .
C31 C 1.3197(4) 1.3368(4) 0.40426(18) 0.0177(7) Uani 1 1 d . . .
C32 C 1.4082(5) 1.2158(4) 0.43556(18) 0.0226(8) Uani 1 1 d . . .
H32 H 1.4832 1.2234 0.4637 0.027 Uiso 1 1 calc R . .
C33 C 1.3834(5) 1.0868(4) 0.4243(2) 0.0254(8) Uani 1 1 d . . .
H33 H 1.4435 1.0065 0.4438 0.030 Uiso 1 1 calc R . .
C34 C 1.2674(5) 1.0772(4) 0.38350(19) 0.0217(8) Uani 1 1 d . . .
H34 H 1.2479 0.9891 0.3782 0.026 Uiso 1 1 calc R . .
C35 C 1.2106(4) 1.3171(3) 0.36143(17) 0.0141(7) Uani 1 1 d . . .
C36 C 1.1232(4) 1.4356(4) 0.32485(17) 0.0153(7) Uani 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
C1 Cu1 N11 140.62(14) . 1_545 ?
C1 Cu1 N10 110.98(13) . 2_766 ?
N11 Cu1 N10 108.20(12) 1_545 2_766 ?
C2 Cu2 C3 140.85(14) . . ?
C2 Cu2 N9 116.13(13) . . ?
C3 Cu2 N9 103.02(13) . . ?
C6 Cu3 C7 140.43(14) . . ?
C6 Cu3 N12 115.79(13) . . ?
C7 Cu3 N12 103.61(12) . . ?
C6 Cu3 Cu5 93.88(11) . . ?
C7 Cu3 Cu5 88.54(10) . . ?
N12 Cu3 Cu5 91.27(9) . . ?
N5 Cu4 C5 0.00(19) 1_565 1_565 ?
N5 Cu4 N14 138.28(14) 1_565 . ?
C5 Cu4 N14 138.28(14) 1_565 . ?
N5 Cu4 N13 111.27(13) 1_565 2_685 ?
C5 Cu4 N13 111.27(13) 1_565 2_685 ?
N14 Cu4 N13 110.43(12) . 2_685 ?
C4 Cu5 N15 139.12(15) . . ?
C4 Cu5 N16 137.93(14) . . ?
N15 Cu5 N16 82.10(12) . . ?
C4 Cu5 Cu3 90.64(12) . . ?
N15 Cu5 Cu3 96.44(9) . . ?
N16 Cu5 Cu3 92.39(9) . . ?
C8 Cu6 N18 144.08(15) . . ?
C8 Cu6 N17 132.97(15) . . ?
N18 Cu6 N17 82.18(12) . . ?
C9 N9 C10 102.1(3) . . ?
C9 N9 Cu2 131.2(2) . . ?
C10 N9 Cu2 126.7(3) . . ?
C9 N10 N11 105.2(3) . . ?
C9 N10 Cu1 126.8(2) . 2_766 ?
N11 N10 Cu1 127.7(2) . 2_766 ?
C10 N11 N10 106.0(3) . . ?
C10 N11 Cu1 129.4(2) . 1_565 ?
N10 N11 Cu1 124.0(2) . 1_565 ?
C11 N12 C12 101.9(3) . . ?
C11 N12 Cu3 131.1(2) . . ?
C12 N12 Cu3 125.9(2) . . ?
C11 N13 N14 105.4(3) . . ?
C11 N13 Cu4 127.8(2) . 2_685 ?
N14 N13 Cu4 126.1(2) . 2_685 ?
C12 N14 N13 105.7(3) . . ?
C12 N14 Cu4 130.5(2) . . ?
N13 N14 Cu4 123.5(2) . . ?
C13 N15 C24 118.1(4) . . ?
C13 N15 Cu5 129.5(3) . . ?
C24 N15 Cu5 112.4(3) . . ?
C22 N16 C23 118.1(3) . . ?
C22 N16 Cu5 131.1(3) . . ?
C23 N16 Cu5 110.8(2) . . ?
C25 N17 C36 117.9(3) . . ?
C25 N17 Cu6 131.0(3) . . ?
C36 N17 Cu6 111.0(2) . . ?
C34 N18 C35 117.7(3) . . ?
C34 N18 Cu6 129.9(2) . . ?
C35 N18 Cu6 112.4(2) . . ?
C2 C1 Cu1 173.0(3) . . ?
C1 C2 Cu2 172.0(3) . . ?
C4 C3 Cu2 163.4(3) . . ?
C3 C4 Cu5 175.8(3) . . ?
C6 C5 Cu4 171.5(3) . 1_545 ?
C5 C6 Cu3 174.1(3) . . ?
C8 C7 Cu3 168.0(3) . . ?
C7 C8 Cu6 174.7(3) . . ?
N10 C9 N9 113.9(3) . . ?
N11 C10 N9 112.9(3) . . ?
N13 C11 N12 113.7(3) . . ?
N14 C12 N12 113.2(3) . . ?
N15 C13 C14 122.8(4) . . ?
C15 C14 C13 118.8(4) . . ?
C14 C15 C16 120.4(4) . . ?
C15 C16 C24 117.1(4) . . ?
C15 C16 C17 124.3(4) . . ?
C24 C16 C17 118.6(4) . . ?
C18 C17 C16 121.2(4) . . ?
C17 C18 C19 121.9(4) . . ?
C23 C19 C20 117.2(4) . . ?
C23 C19 C18 118.1(4) . . ?
C20 C19 C18 124.7(4) . . ?
C21 C20 C19 119.5(4) . . ?
C20 C21 C22 119.9(4) . . ?
N16 C22 C21 122.7(4) . . ?
N16 C23 C19 122.6(4) . . ?
N16 C23 C24 117.3(3) . . ?
C19 C23 C24 120.0(4) . . ?
N15 C24 C16 122.8(4) . . ?
N15 C24 C23 117.0(3) . . ?
C16 C24 C23 120.1(4) . . ?
N17 C25 C26 122.7(4) . . ?
C27 C26 C25 119.6(4) . . ?
C26 C27 C28 119.5(4) . . ?
C27 C28 C36 117.3(4) . . ?
C27 C28 C29 124.2(3) . . ?
C36 C28 C29 118.5(3) . . ?
C30 C29 C28 121.2(3) . . ?
C29 C30 C31 121.3(4) . . ?
C35 C31 C32 116.9(3) . . ?
C35 C31 C30 119.1(3) . . ?
C32 C31 C30 124.0(4) . . ?
C33 C32 C31 119.8(4) . . ?
C32 C33 C34 119.3(4) . . ?
N18 C34 C33 123.1(3) . . ?
N18 C35 C31 123.0(3) . . ?
N18 C35 C36 117.1(3) . . ?
C31 C35 C36 119.9(3) . . ?
N17 C36 C28 123.0(3) . . ?
N17 C36 C35 117.1(3) . . ?
C28 C36 C35 119.9(3) . . ?
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 1.870(3) . ?
Cu1 N11 1.934(3) 1_545 ?
Cu1 N10 2.029(3) 2_766 ?
Cu2 C2 1.875(3) . ?
Cu2 C3 1.906(3) . ?
Cu2 N9 2.027(3) . ?
Cu3 C6 1.889(3) . ?
Cu3 C7 1.909(3) . ?
Cu3 N12 2.036(3) . ?
Cu3 Cu5 2.9687(9) . ?
Cu4 N5 1.883(3) 1_565 ?
Cu4 C5 1.883(3) 1_565 ?
Cu4 N14 1.943(3) . ?
Cu4 N13 2.032(3) 2_685 ?
Cu5 C4 1.852(4) . ?
Cu5 N15 2.026(3) . ?
Cu5 N16 2.058(3) . ?
Cu6 C8 1.855(4) . ?
Cu6 N18 2.009(3) . ?
Cu6 N17 2.067(3) . ?
N9 C9 1.345(5) . ?
N9 C10 1.353(4) . ?
N10 C9 1.319(4) . ?
N10 N11 1.388(4) . ?
N10 Cu1 2.029(3) 2_766 ?
N11 C10 1.324(5) . ?
N11 Cu1 1.934(3) 1_565 ?
N12 C11 1.347(5) . ?
N12 C12 1.352(4) . ?
N13 C11 1.324(4) . ?
N13 N14 1.383(4) . ?
N13 Cu4 2.032(3) 2_685 ?
N14 C12 1.325(5) . ?
N15 C13 1.336(5) . ?
N15 C24 1.357(5) . ?
N16 C22 1.324(5) . ?
N16 C23 1.366(5) . ?
N17 C25 1.338(5) . ?
N17 C36 1.356(5) . ?
N18 C34 1.330(5) . ?
N18 C35 1.370(4) . ?
C1 C2 1.158(5) . ?
C3 C4 1.158(5) . ?
C5 C6 1.143(5) . ?
C5 Cu4 1.883(3) 1_545 ?
C7 C8 1.151(5) . ?
C13 C14 1.395(6) . ?
C14 C15 1.376(7) . ?
C15 C16 1.391(7) . ?
C16 C24 1.412(5) . ?
C16 C17 1.436(6) . ?
C17 C18 1.349(7) . ?
C18 C19 1.440(7) . ?
C19 C23 1.412(5) . ?
C19 C20 1.412(7) . ?
C20 C21 1.354(7) . ?
C21 C22 1.405(6) . ?
C23 C24 1.439(5) . ?
C25 C26 1.391(6) . ?
C26 C27 1.371(7) . ?
C27 C28 1.403(5) . ?
C28 C36 1.408(5) . ?
C28 C29 1.438(6) . ?
C29 C30 1.354(6) . ?
C30 C31 1.422(5) . ?
C31 C35 1.406(5) . ?
C31 C32 1.411(6) . ?
C32 C33 1.370(6) . ?
C33 C34 1.392(6) . ?
C35 C36 1.437(5) . ?
