#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:25:48 +0100 (Fri 25 de Mar de 2016) $
#$Revision: 179969 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/63/7026313.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_7026313
loop_
_publ_author_name
'Deng, Zhao-Peng'
'Qi, Hui-Ling'
'Huo, Li-Hua'
'Ng, Seik Weng'
'Zhao, Hui'
'Gao, Shan'
_publ_section_title
;
 Syntheses and structures of copper(I) complexes based on Cu(n)X(n) (X =
 Br and I; n = 1, 2 and 4) units and bis(pyridyl) ligands with longer
 flexible spacer.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10038
_journal_page_last               10050
_journal_paper_doi               10.1039/c0dt00336k
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C18 H18 Cu I N4, C H2 Cl2'
_chemical_formula_sum            'C19 H20 Cl2 Cu I N4'
_chemical_formula_weight         565.73
_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                112.781(3)
_cell_angle_beta                 102.329(2)
_cell_angle_gamma                102.9761(19)
_cell_formula_units_Z            2
_cell_length_a                   8.2067(5)
_cell_length_b                   12.7371(10)
_cell_length_c                   12.8425(11)
_cell_measurement_reflns_used    6872
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      3.14
_cell_volume                     1136.65(15)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       'RAPID-AUTO (Rigaku Corporation, 1998)'
_computing_data_reduction
'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)'
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       ω
_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  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8960
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.13
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.565
_exptl_absorpt_correction_T_max  0.7153
_exptl_absorpt_correction_T_min  0.6023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.195
_refine_diff_density_min         -1.462
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3985
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0337P)²+9.3098P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1460
_reflns_number_gt                2747
_reflns_number_total             3985
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00336k.txt
_cod_data_source_block           complex5
_cod_database_code               7026313
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
I1 I 0.75568(7) 0.34780(6) 0.46398(5) 0.0544(2) Uani 1 1 d . . .
Cu1 Cu 1.09579(14) 0.41874(11) 0.47907(9) 0.0558(3) Uani 1 1 d . . .
N1 N 1.1151(8) 0.3191(6) 0.3153(6) 0.0457(16) Uani 1 1 d . . .
N2 N 1.4502(9) 0.3046(6) 0.1716(6) 0.0521(18) Uani 1 1 d . . .
H2N H 1.5367 0.3634 0.2316 0.063 Uiso 1 1 calc R . .
N3 N 1.2294(8) 0.4034(6) 0.6235(6) 0.0459(16) Uani 1 1 d . . .
N4 N 1.6131(11) 0.3198(9) 0.7068(7) 0.076(3) Uani 1 1 d . . .
H4N H 1.6402 0.3091 0.6433 0.092 Uiso 1 1 calc R . .
C1 C 0.9722(11) 0.2312(8) 0.2254(8) 0.056(2) Uani 1 1 d . . .
H1 H 0.8644 0.2157 0.2389 0.067 Uiso 1 1 calc R . .
C2 C 0.9781(11) 0.1635(8) 0.1146(8) 0.056(2) Uani 1 1 d . . .
H2 H 0.8759 0.1033 0.0543 0.068 Uiso 1 1 calc R . .
C3 C 1.1363(11) 0.1850(7) 0.0930(7) 0.049(2) Uani 1 1 d . . .
H3 H 1.1414 0.1402 0.0176 0.059 Uiso 1 1 calc R . .
C4 C 1.2890(10) 0.2744(7) 0.1847(7) 0.0405(18) Uani 1 1 d . . .
C5 C 1.2683(10) 0.3394(7) 0.2941(7) 0.0433(19) Uani 1 1 d . . .
H5 H 1.3678 0.4008 0.3561 0.052 Uiso 1 1 calc R . .
C6 C 1.4833(13) 0.2428(8) 0.0617(9) 0.059(2) Uani 1 1 d . . .
H6A H 1.5957 0.2922 0.0661 0.071 Uiso 1 1 calc R . .
H6B H 1.3918 0.2376 -0.0038 0.071 Uiso 1 1 calc R . .
C7 C 1.4889(10) 0.1161(7) 0.0310(7) 0.0437(19) Uani 1 1 d . . .
C8 C 1.4801(10) 0.0421(8) -0.0832(7) 0.049(2) Uani 1 1 d . . .
H8 H 1.4653 0.0692 -0.1411 0.059 Uiso 1 1 calc R . .
C9 C 1.4931(10) -0.0719(7) -0.1134(7) 0.047(2) Uani 1 1 d . . .
H9 H 1.4895 -0.1193 -0.1906 0.056 Uiso 1 1 calc R . .
C10 C 1.1827(11) 0.4298(8) 0.7220(8) 0.058(2) Uani 1 1 d . . .
H10 H 1.0840 0.4539 0.7238 0.070 Uiso 1 1 calc R . .
C11 C 1.2743(12) 0.4228(9) 0.8199(8) 0.059(2) Uani 1 1 d . . .
H11 H 1.2378 0.4423 0.8867 0.070 Uiso 1 1 calc R . .
C12 C 1.4212(12) 0.3868(9) 0.8197(8) 0.058(2) Uani 1 1 d . . .
H12 H 1.4842 0.3816 0.8859 0.069 Uiso 1 1 calc R . .
C13 C 1.4732(11) 0.3583(8) 0.7182(7) 0.050(2) Uani 1 1 d . . .
C14 C 1.3715(10) 0.3690(7) 0.6230(7) 0.0451(19) Uani 1 1 d . . .
H14 H 1.4050 0.3511 0.5550 0.054 Uiso 1 1 calc R . .
C15 C 1.7188(14) 0.2959(10) 0.7941(10) 0.075(3) Uani 1 1 d . . .
H15A H 1.7747 0.2405 0.7538 0.090 Uiso 1 1 calc R . .
H15B H 1.6398 0.2547 0.8233 0.090 Uiso 1 1 calc R . .
C16 C 1.8621(12) 0.4046(9) 0.9013(8) 0.055(2) Uani 1 1 d . . .
C17 C 1.9529(13) 0.3874(10) 0.9934(9) 0.062(3) Uani 1 1 d . . .
H17 H 1.9206 0.3111 0.9901 0.075 Uiso 1 1 calc R . .
C18 C 2.0904(13) 0.4812(10) 1.0901(9) 0.063(3) Uani 1 1 d . . .
H18 H 2.1518 0.4671 1.1502 0.075 Uiso 1 1 calc R . .
C19 C 0.071(6) -0.068(5) 0.239(3) 0.28(3) Uani 0.50 1 d PD A 1
H19A H 0.0944 -0.1349 0.1830 0.333 Uiso 0.50 1 calc PR A 1
H19B H 0.0011 -0.0385 0.1937 0.333 Uiso 0.50 1 calc PR A 1
Cl1 Cl 0.262(4) 0.042(3) 0.329(3) 0.400(11) Uiso 0.50 1 d PD A 1
Cl2 Cl -0.046(6) -0.119(4) 0.311(5) 0.62(2) Uiso 0.50 1 d PD A 1
C19' C 0.101(9) 0.030(4) 0.375(4) 0.28(3) Uani 0.50 1 d PD B 2
H19C H 0.1766 0.0932 0.3652 0.333 Uiso 0.50 1 calc PR B 2
H19D H 0.0363 0.0663 0.4253 0.333 Uiso 0.50 1 calc PR B 2
Cl1' Cl 0.228(4) -0.022(3) 0.445(3) 0.400(11) Uiso 0.50 1 d PD B 2
Cl2' Cl -0.044(7) -0.072(6) 0.242(4) 0.62(2) Uiso 0.50 1 d PD B 2
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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
Cu1 I1 Cu1 63.85(4) . 2_766
N3 Cu1 N1 118.0(3) . .
N3 Cu1 I1 104.37(18) . .
N1 Cu1 I1 108.34(18) . .
N3 Cu1 I1 103.73(19) . 2_766
N1 Cu1 I1 106.6(2) . 2_766
I1 Cu1 I1 116.15(4) . 2_766
N3 Cu1 Cu1 117.33(19) . 2_766
N1 Cu1 Cu1 124.61(19) . 2_766
I1 Cu1 Cu1 58.15(4) . 2_766
I1 Cu1 Cu1 57.99(4) 2_766 2_766
C5 N1 C1 117.6(7) . .
C5 N1 Cu1 121.8(5) . .
C1 N1 Cu1 120.6(5) . .
C4 N2 C6 123.2(7) . .
C4 N2 H2N 118.4 . .
C6 N2 H2N 118.4 . .
C14 N3 C10 117.6(7) . .
C14 N3 Cu1 119.9(5) . .
C10 N3 Cu1 122.4(6) . .
C13 N4 C15 124.4(8) . .
C13 N4 H4N 117.8 . .
C15 N4 H4N 117.8 . .
N1 C1 C2 122.8(8) . .
N1 C1 H1 118.6 . .
C2 C1 H1 118.6 . .
C1 C2 C3 119.5(8) . .
C1 C2 H2 120.3 . .
C3 C2 H2 120.3 . .
C2 C3 C4 119.6(8) . .
C2 C3 H3 120.2 . .
C4 C3 H3 120.2 . .
N2 C4 C3 124.1(7) . .
N2 C4 C5 119.4(7) . .
C3 C4 C5 116.4(7) . .
N1 C5 C4 124.2(7) . .
N1 C5 H5 117.9 . .
C4 C5 H5 117.9 . .
N2 C6 C7 116.6(8) . .
N2 C6 H6A 108.2 . .
C7 C6 H6A 108.2 . .
N2 C6 H6B 108.2 . .
C7 C6 H6B 108.2 . .
H6A C6 H6B 107.3 . .
C9 C7 C8 117.7(8) 2_855 .
C9 C7 C6 122.9(7) 2_855 .
C8 C7 C6 119.4(8) . .
C7 C8 C9 121.2(8) . .
C7 C8 H8 119.4 . .
C9 C8 H8 119.4 . .
C7 C9 C8 121.1(8) 2_855 .
C7 C9 H9 119.5 2_855 .
C8 C9 H9 119.5 . .
N3 C10 C11 122.7(8) . .
N3 C10 H10 118.7 . .
C11 C10 H10 118.7 . .
C10 C11 C12 120.0(8) . .
C10 C11 H11 120.0 . .
C12 C11 H11 120.0 . .
C11 C12 C13 118.7(8) . .
C11 C12 H12 120.6 . .
C13 C12 H12 120.6 . .
N4 C13 C12 124.0(8) . .
N4 C13 C14 119.1(8) . .
C12 C13 C14 116.9(8) . .
N3 C14 C13 124.1(7) . .
N3 C14 H14 118.0 . .
C13 C14 H14 118.0 . .
N4 C15 C16 116.6(9) . .
N4 C15 H15A 108.1 . .
C16 C15 H15A 108.1 . .
N4 C15 H15B 108.1 . .
C16 C15 H15B 108.1 . .
H15A C15 H15B 107.3 . .
C18 C16 C17 118.2(9) 2_967 .
C18 C16 C15 123.3(9) 2_967 .
C17 C16 C15 118.4(9) . .
C18 C17 C16 121.1(10) . .
C18 C17 H17 119.4 . .
C16 C17 H17 119.4 . .
C16 C18 C17 120.7(9) 2_967 .
C16 C18 H18 119.7 2_967 .
C17 C18 H18 119.7 . .
Cl1 C19 Cl2 114.0(10) . .
Cl1 C19 H19A 108.8 . .
Cl2 C19 H19A 108.8 . .
Cl1 C19 H19B 108.8 . .
Cl2 C19 H19B 108.8 . .
H19A C19 H19B 107.7 . .
Cl1' C19' Cl2' 115.6(10) . .
Cl1' C19' H19C 108.4 . .
Cl2' C19' H19C 108.4 . .
Cl1' C19' H19D 108.4 . .
Cl2' C19' H19D 108.4 . .
H19C C19' H19D 107.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I1 Cu1 2.6731(12) .
I1 Cu1 2.6778(14) 2_766
Cu1 N3 2.047(7) .
Cu1 N1 2.055(7) .
Cu1 I1 2.6778(14) 2_766
Cu1 Cu1 2.830(2) 2_766
N1 C5 1.333(10) .
N1 C1 1.339(10) .
N2 C4 1.357(10) .
N2 C6 1.444(10) .
N2 H2N 0.8600 .
N3 C14 1.335(10) .
N3 C10 1.339(11) .
N4 C13 1.360(11) .
N4 C15 1.438(12) .
N4 H4N 0.8600 .
C1 C2 1.367(12) .
C1 H1 0.9300 .
C2 C3 1.375(11) .
C2 H2 0.9300 .
C3 C4 1.395(11) .
C3 H3 0.9300 .
C4 C5 1.398(10) .
C5 H5 0.9300 .
C6 C7 1.520(12) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C7 C9 1.375(12) 2_855
C7 C8 1.378(11) .
C8 C9 1.387(11) .
C8 H8 0.9300 .
C9 C7 1.375(12) 2_855
C9 H9 0.9300 .
C10 C11 1.366(12) .
C10 H10 0.9300 .
C11 C12 1.383(12) .
C11 H11 0.9300 .
C12 C13 1.398(12) .
C12 H12 0.9300 .
C13 C14 1.398(11) .
C14 H14 0.9300 .
C15 C16 1.515(14) .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C16 C18 1.371(13) 2_967
C16 C17 1.379(12) .
C17 C18 1.375(14) .
C17 H17 0.9300 .
C18 C16 1.371(13) 2_967
C18 H18 0.9300 .
C19 Cl1 1.653(10) .
C19 Cl2 1.660(10) .
C19 H19A 0.9700 .
C19 H19B 0.9700 .
C19' Cl1' 1.646(10) .
C19' Cl2' 1.653(10) .
C19' H19C 0.9700 .
C19' H19D 0.9700 .
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
_geom_hbond_site_symmetry_A
N2 H2N I1 0.86 3.24 3.802(8) 125.1 1_655
N4 H4N I1 0.86 2.84 3.668(9) 163.3 1_655
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
Cu1 I1 Cu1 N3 113.5(2) 2_766 .
Cu1 I1 Cu1 N1 -119.9(2) 2_766 .
Cu1 I1 Cu1 I1 0.0 2_766 2_766
N3 Cu1 N1 C5 -65.5(7) . .
I1 Cu1 N1 C5 176.3(6) . .
I1 Cu1 N1 C5 50.6(6) 2_766 .
Cu1 Cu1 N1 C5 112.8(6) 2_766 .
N3 Cu1 N1 C1 114.9(7) . .
I1 Cu1 N1 C1 -3.3(7) . .
I1 Cu1 N1 C1 -129.0(6) 2_766 .
Cu1 Cu1 N1 C1 -66.7(7) 2_766 .
N1 Cu1 N3 C14 24.4(7) . .
I1 Cu1 N3 C14 144.7(6) . .
I1 Cu1 N3 C14 -93.2(6) 2_766 .
Cu1 Cu1 N3 C14 -154.0(5) 2_766 .
N1 Cu1 N3 C10 -157.4(6) . .
I1 Cu1 N3 C10 -37.1(7) . .
I1 Cu1 N3 C10 85.0(7) 2_766 .
Cu1 Cu1 N3 C10 24.2(7) 2_766 .
C5 N1 C1 C2 -0.3(14) . .
Cu1 N1 C1 C2 179.3(7) . .
N1 C1 C2 C3 0.1(15) . .
C1 C2 C3 C4 0.9(14) . .
C6 N2 C4 C3 -3.2(13) . .
C6 N2 C4 C5 -179.7(8) . .
C2 C3 C4 N2 -178.2(8) . .
C2 C3 C4 C5 -1.6(12) . .
C1 N1 C5 C4 -0.5(12) . .
Cu1 N1 C5 C4 179.9(6) . .
N2 C4 C5 N1 178.2(8) . .
C3 C4 C5 N1 1.5(12) . .
C4 N2 C6 C7 -72.8(11) . .
N2 C6 C7 C9 -16.0(12) . 2_855
N2 C6 C7 C8 165.6(7) . .
C9 C7 C8 C9 -1.4(13) 2_855 .
C6 C7 C8 C9 177.0(8) . .
C7 C8 C9 C7 1.5(13) . 2_855
C14 N3 C10 C11 0.0(13) . .
Cu1 N3 C10 C11 -178.2(7) . .
N3 C10 C11 C12 -0.3(15) . .
C10 C11 C12 C13 0.1(15) . .
C15 N4 C13 C12 4.2(16) . .
C15 N4 C13 C14 -174.9(9) . .
C11 C12 C13 N4 -178.8(10) . .
C11 C12 C13 C14 0.3(13) . .
C10 N3 C14 C13 0.4(13) . .
Cu1 N3 C14 C13 178.7(6) . .
N4 C13 C14 N3 178.5(9) . .
C12 C13 C14 N3 -0.6(13) . .
C13 N4 C15 C16 -80.9(13) . .
N4 C15 C16 C18 -9.1(14) . 2_967
N4 C15 C16 C17 172.8(9) . .
C18 C16 C17 C18 -1.6(15) 2_967 .
C15 C16 C17 C18 176.6(9) . .
C16 C17 C18 C16 1.6(16) . 2_967
