#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/14/7011406.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_7011406
loop_
_publ_author_name
'Paula L. Caradoc-Davies'
'Lyall R. Hanton'
'Justin M. Hodgkiss'
'Mark D. Spicer'
_publ_section_title
;
 Methyl group influence on the formation of CuI complexes with
 thio-pyridine ligands
;
_journal_issue                   8
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              1581
_journal_page_last               1585
_journal_paper_doi               10.1039/b111400j
_journal_year                    2002
_chemical_formula_sum            'C28 H32 Cu4 I4 N4 S2'
_chemical_formula_weight         1250.46
_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                105.338(5)
_cell_angle_beta                 102.112(5)
_cell_angle_gamma                102.073(5)
_cell_formula_units_Z            1
_cell_length_a                   9.351(5)
_cell_length_b                   10.314(5)
_cell_length_c                   10.441(5)
_cell_measurement_reflns_used    3680
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.11
_cell_volume                     911.3(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      163(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0203
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11726
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    5.829
_exptl_absorpt_correction_T_max  0.592
_exptl_absorpt_correction_T_min  0.514
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (sheldrick 1996)'
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    2.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.313
_refine_diff_density_min         -0.935
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         3680
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0273
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0469P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0708
_reflns_number_gt                3187
_reflns_number_total             3680
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b111400j.txt
_cod_data_source_block           '[Cu4(L1)2I4]'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7011406
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
C1 C 1.0088(5) 0.3863(4) 1.2715(4) 0.0344(9) Uani 1 1 d . . .
C2 C 1.0728(5) 0.2749(5) 1.2629(5) 0.0476(11) Uani 1 1 d . . .
H2 H 1.1756 0.2909 1.3056 0.057 Uiso 1 1 calc R . .
C3 C 0.9833(6) 0.1433(5) 1.1917(5) 0.0522(12) Uani 1 1 d . . .
H3 H 1.0247 0.0680 1.1841 0.063 Uiso 1 1 calc R . .
C4 C 0.8283(5) 0.1203(4) 1.1294(5) 0.0433(10) Uani 1 1 d . . .
H4 H 0.7651 0.0299 1.0822 0.052 Uiso 1 1 calc R . .
C5 C 0.7710(4) 0.2345(4) 1.1393(4) 0.0282(8) Uani 1 1 d . . .
C6 C 0.6059(4) 0.2190(4) 1.0767(4) 0.0298(8) Uani 1 1 d . . .
H6A H 0.5562 0.2360 1.1498 0.036 Uiso 1 1 calc R . .
H6B H 0.5572 0.1237 1.0155 0.036 Uiso 1 1 calc R . .
C7 C 0.6677(4) 0.2712(4) 0.8469(4) 0.0282(8) Uani 1 1 d . . .
H7A H 0.6751 0.3320 0.7904 0.034 Uiso 1 1 calc R . .
H7B H 0.7700 0.2708 0.8900 0.034 Uiso 1 1 calc R . .
C8 C 0.5769(4) 0.1255(4) 0.7568(4) 0.0272(8) Uani 1 1 d . . .
C9 C 0.6460(5) 0.0208(4) 0.7267(4) 0.0375(9) Uani 1 1 d . . .
H9 H 0.7502 0.0384 0.7644 0.045 Uiso 1 1 calc R . .
C10 C 0.5584(5) -0.1121(4) 0.6391(4) 0.0443(11) Uani 1 1 d . . .
H10 H 0.6025 -0.1852 0.6187 0.053 Uiso 1 1 calc R . .
C11 C 0.4043(5) -0.1330(4) 0.5832(4) 0.0418(10) Uani 1 1 d . . .
H11 H 0.3440 -0.2204 0.5231 0.050 Uiso 1 1 calc R . .
C12 C 0.3399(5) -0.0242(4) 0.6166(4) 0.0343(9) Uani 1 1 d . . .
C13 C 0.1763(5) -0.0395(5) 0.5525(5) 0.0555(13) Uani 1 1 d . . .
H13A H 0.1296 -0.0070 0.6237 0.083 Uiso 1 1 calc R . .
H13B H 0.1249 -0.1362 0.5015 0.083 Uiso 1 1 calc R . .
H13C H 0.1694 0.0151 0.4910 0.083 Uiso 1 1 calc R . .
C14 C 1.1017(5) 0.5321(5) 1.3537(5) 0.0560(13) Uani 1 1 d . . .
H14A H 1.0939 0.5913 1.2969 0.084 Uiso 1 1 calc R . .
H14B H 1.2063 0.5337 1.3855 0.084 Uiso 1 1 calc R . .
H14C H 1.0648 0.5655 1.4318 0.084 Uiso 1 1 calc R . .
N1 N 0.8613(3) 0.3667(3) 1.2079(3) 0.0271(7) Uani 1 1 d . . .
N2 N 0.4241(3) 0.1033(3) 0.7047(3) 0.0262(6) Uani 1 1 d . . .
S1 S 0.58042(10) 0.33909(9) 0.98004(9) 0.02490(19) Uani 1 1 d . . .
Cu1 Cu 0.33751(5) 0.26379(5) 0.77776(5) 0.03207(13) Uani 1 1 d . . .
Cu2 Cu 0.76565(5) 0.52310(4) 1.18387(5) 0.02905(12) Uani 1 1 d . . .
I1 I 0.10799(3) 0.26305(3) 0.87876(3) 0.03471(9) Uani 1 1 d . . .
I2 I 0.40978(3) 0.44687(3) 0.64871(3) 0.03398(9) 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'
S S 0.1246 0.1234 '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'
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
N1 C1 C2 121.8(4) . . ?
N1 C1 C14 117.4(3) . . ?
C2 C1 C14 120.7(4) . . ?
C3 C2 C1 119.0(4) . . ?
C2 C3 C4 120.0(4) . . ?
C5 C4 C3 118.7(4) . . ?
N1 C5 C4 121.4(4) . . ?
N1 C5 C6 116.5(3) . . ?
C4 C5 C6 122.1(3) . . ?
C5 C6 S1 112.3(2) . . ?
C8 C7 S1 111.3(2) . . ?
N2 C8 C9 122.0(3) . . ?
N2 C8 C7 116.9(3) . . ?
C9 C8 C7 121.0(4) . . ?
C8 C9 C10 119.3(4) . . ?
C11 C10 C9 118.5(4) . . ?
C12 C11 C10 120.1(4) . . ?
N2 C12 C11 121.3(4) . . ?
N2 C12 C13 116.7(4) . . ?
C11 C12 C13 122.0(4) . . ?
C1 N1 C5 119.0(3) . . ?
C1 N1 Cu2 124.8(2) . . ?
C5 N1 Cu2 115.7(2) . . ?
C12 N2 C8 118.7(3) . . ?
C12 N2 Cu1 124.5(3) . . ?
C8 N2 Cu1 116.6(2) . . ?
C7 S1 C6 98.17(17) . . ?
C7 S1 Cu2 112.51(13) . . ?
C6 S1 Cu2 86.39(13) . . ?
C7 S1 Cu1 84.48(13) . . ?
C6 S1 Cu1 117.56(12) . . ?
Cu2 S1 Cu1 149.22(4) . . ?
N2 Cu1 Cu2 166.27(9) . 2_667 ?
N2 Cu1 S1 82.47(9) . . ?
Cu2 Cu1 S1 104.12(3) 2_667 . ?
N2 Cu1 I1 129.45(9) . . ?
Cu2 Cu1 I1 60.50(2) 2_667 . ?
S1 Cu1 I1 108.14(5) . . ?
N2 Cu1 I2 106.26(9) . . ?
Cu2 Cu1 I2 60.96(3) 2_667 . ?
S1 Cu1 I2 100.88(4) . . ?
I1 Cu1 I2 119.03(2) . . ?
N1 Cu2 S1 84.79(9) . . ?
N1 Cu2 Cu1 165.08(9) . 2_667 ?
S1 Cu2 Cu1 106.51(4) . 2_667 ?
N1 Cu2 I1 125.11(9) . 2_667 ?
S1 Cu2 I1 111.83(4) . 2_667 ?
Cu1 Cu2 I1 60.35(4) 2_667 2_667 ?
N1 Cu2 I2 107.85(9) . 2_667 ?
S1 Cu2 I2 99.29(4) . 2_667 ?
Cu1 Cu2 I2 61.41(2) 2_667 2_667 ?
I1 Cu2 I2 119.32(3) 2_667 2_667 ?
Cu1 I1 Cu2 59.15(2) . 2_667 ?
Cu2 I2 Cu1 57.62(2) 2_667 . ?
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
C1 N1 1.346(5) . ?
C1 C2 1.394(5) . ?
C1 C14 1.487(6) . ?
C2 C3 1.351(6) . ?
C3 C4 1.400(6) . ?
C4 C5 1.381(5) . ?
C5 N1 1.354(4) . ?
C5 C6 1.502(5) . ?
C6 S1 1.814(4) . ?
C7 C8 1.499(5) . ?
C7 S1 1.813(4) . ?
C8 N2 1.364(5) . ?
C8 C9 1.371(5) . ?
C9 C10 1.393(6) . ?
C10 C11 1.384(6) . ?
C11 C12 1.381(6) . ?
C12 N2 1.349(5) . ?
C12 C13 1.492(6) . ?
N1 Cu2 2.047(3) . ?
N2 Cu1 2.031(3) . ?
S1 Cu2 2.4642(12) . ?
S1 Cu1 2.5699(14) . ?
Cu1 Cu2 2.5506(12) 2_667 ?
Cu1 I1 2.5818(12) . ?
Cu1 I2 2.6519(10) . ?
Cu2 Cu1 2.5506(12) 2_667 ?
Cu2 I1 2.5857(11) 2_667 ?
Cu2 I2 2.6405(11) 2_667 ?
I1 Cu2 2.5857(10) 2_667 ?
I2 Cu2 2.6405(11) 2_667 ?
