#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/26/7012619.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_7012619
loop_
_publ_author_name
'Amoore, Jarrod J. M.'
'Hanton, Lyall R.'
'Spicer, Mark D.'
_publ_section_title
;
 Banded ribbons of Cu6I6 hexamers and multimodal thioether pyrazine
 ligands linked by self-complementary N⋯H--C synthons
;
_journal_issue                   6
_journal_name_full               'Dalton Transactions'
_journal_page_first              1056
_journal_paper_doi               10.1039/b212365g
_journal_year                    2003
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C12 H14 Cu3 I3 N4 S1'
_chemical_formula_sum            'C12 H14 Cu3 I3 N4 S'
_chemical_formula_weight         817.66
_chemical_name_common            Cu3LI3
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2002-11-07T09:37:03-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                87.9370(10)
_cell_angle_beta                 86.2090(10)
_cell_angle_gamma                67.2040(10)
_cell_formula_units_Z            2
_cell_length_a                   8.3841(2)
_cell_length_b                   9.2406(2)
_cell_length_c                   13.7990(4)
_cell_measurement_reflns_used    3848
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.91
_cell_measurement_wavelength     0.71073
_cell_volume                     983.34(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD; rotation images; thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.0302574
_diffrn_orient_matrix_UB_12      -0.1042021
_diffrn_orient_matrix_UB_13      0.0335516
_diffrn_orient_matrix_UB_21      -0.0600601
_diffrn_orient_matrix_UB_22      0.0538704
_diffrn_orient_matrix_UB_23      0.0614467
_diffrn_orient_matrix_UB_31      -0.1107708
_diffrn_orient_matrix_UB_32      -0.0046361
_diffrn_orient_matrix_UB_33      -0.019341
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7319
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.95
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    8.031
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.761
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.194
_refine_diff_density_min         -1.274
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         4480
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0190P)²+1.7510P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0589
_refine_ls_wR_factor_ref         0.0628
_reflns_number_gt                3606
_reflns_number_total             4480
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b212365g.txt
_cod_data_source_block           Cu3LI3
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C12 H14 Cu3 I3 N4 S1'
_cod_database_code               7012619
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 1.1441(6) -0.1598(6) 0.0810(4) 0.0314(12) Uani 1 1 d . . .
H1A H 1.2412 -0.2399 0.1128 0.047 Uiso 1 1 calc R . .
H1B H 1.1373 -0.0552 0.0976 0.047 Uiso 1 1 calc R . .
H1C H 1.162 -0.1731 0.0105 0.047 Uiso 1 1 calc R . .
C2 C 0.9789(6) -0.1768(5) 0.1148(3) 0.0233(10) Uani 1 1 d . . .
C3 C 0.8466(7) -0.0610(6) 0.1687(4) 0.0276(11) Uani 1 1 d . . .
C4 C 0.6786(6) -0.2044(5) 0.1689(3) 0.0235(11) Uani 1 1 d . . .
C5 C 0.8105(6) -0.3222(5) 0.1177(3) 0.0195(10) Uani 1 1 d . . .
C6 C -0.2070(6) 0.5300(5) 0.0915(4) 0.0217(10) Uani 1 1 d . . .
C7 C -0.1897(7) 0.4197(6) 0.2834(3) 0.0221(10) Uani 1 1 d . . .
C8 C -0.1293(6) 0.5248(5) 0.3376(3) 0.0184(10) Uani 1 1 d . . .
C9 C 0.2417(7) 0.3667(5) 0.5967(3) 0.0220(10) Uani 1 1 d . . .
C10 C 0.0238(6) 0.2939(5) 0.5577(3) 0.0218(10) Uani 1 1 d . . .
C11 C 0.0918(6) 0.5992(5) 0.3782(3) 0.0212(10) Uani 1 1 d . . .
C12 C 0.2755(6) 0.5820(6) 0.3635(4) 0.0308(12) Uani 1 1 d . . .
H12A H 0.3518 0.4728 0.3763 0.046 Uiso 1 1 calc R . .
H12B H 0.298 0.6511 0.4081 0.046 Uiso 1 1 calc R . .
H12C H 0.2977 0.6106 0.2963 0.046 Uiso 1 1 calc R . .
Cu1 Cu 0.49827(8) 0.11271(7) 0.26196(4) 0.02754(15) Uani 1 1 d . . .
Cu2 Cu 0.35688(7) 0.09561(6) 0.45966(4) 0.02366(14) Uani 1 1 d . . .
Cu3 Cu 0.18285(7) 0.34367(7) 0.22138(4) 0.02708(15) Uani 1 1 d . . .
I1 I 0.64010(4) 0.14716(3) 0.42401(2) 0.02195(8) Uani 1 1 d . . .
I2 I 0.22126(4) 0.04860(3) 0.30582(2) 0.02333(9) Uani 1 1 d . . .
I3 I 0.45453(4) 0.33612(4) 0.13030(2) 0.02618(9) Uani 1 1 d . . .
N1 N 0.6972(5) -0.0741(4) 0.1955(3) 0.0236(9) Uani 1 1 d . . .
N2 N 0.9595(5) -0.3073(4) 0.0903(3) 0.0225(9) Uani 1 1 d . . .
N3 N 0.1896(5) 0.2759(4) 0.5441(3) 0.0204(8) Uani 1 1 d . . .
N4 N 0.0377(5) 0.5058(4) 0.3252(3) 0.0177(8) Uani 1 1 d . . .
S1 S -0.08249(15) 0.36001(13) 0.16421(8) 0.0205(2) Uani 1 1 d . . .
H3 H 0.865(7) 0.043(6) 0.187(4) 0.050(17) Uiso 1 1 d . . .
H4 H 0.570(6) -0.211(5) 0.184(3) 0.024(13) Uiso 1 1 d . . .
H6A H -0.164(8) 0.497(7) 0.024(5) 0.07(2) Uiso 1 1 d . . .
H6B H -0.314(5) 0.538(4) 0.099(3) 0.001(10) Uiso 1 1 d . . .
H7A H -0.173(8) 0.330(7) 0.319(4) 0.057(19) Uiso 1 1 d . . .
H7B H -0.308(6) 0.466(5) 0.273(3) 0.019(12) Uiso 1 1 d . . .
H9 H 0.354(6) 0.354(5) 0.588(3) 0.027(14) Uiso 1 1 d . . .
H10 H -0.026(6) 0.238(6) 0.523(4) 0.028(14) 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 0 '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'
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'
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
N2 C2 C3 120.2(5) . . ?
N2 C2 C1 117.5(4) . . ?
C3 C2 C1 122.3(4) . . ?
N1 C3 C2 122.1(5) . . ?
N1 C4 C5 121.6(5) . . ?
N2 C5 C4 121.0(4) . . ?
N2 C5 C6 117.3(4) . 1_645 ?
C4 C5 C6 121.7(4) . 1_645 ?
C5 C6 S1 114.0(3) 1_465 . ?
C8 C7 S1 115.3(3) . . ?
N4 C8 C9 121.0(4) . 2_566 ?
N4 C8 C7 118.4(4) . . ?
C9 C8 C7 120.5(4) 2_566 . ?
N3 C9 C8 121.9(4) . 2_566 ?
N3 C10 C11 122.9(4) . 2_566 ?
N4 C11 C10 119.9(4) . 2_566 ?
N4 C11 C12 118.0(4) . . ?
C10 C11 C12 122.1(4) 2_566 . ?
N1 Cu1 I3 101.24(11) . . ?
N1 Cu1 I2 112.00(11) . . ?
I3 Cu1 I2 114.64(2) . . ?
N1 Cu1 I1 102.29(11) . . ?
I3 Cu1 I1 115.00(2) . . ?
I2 Cu1 I1 110.59(2) . . ?
N1 Cu1 Cu3 139.99(11) . . ?
I3 Cu1 Cu3 55.356(18) . . ?
I2 Cu1 Cu3 63.34(2) . . ?
I1 Cu1 Cu3 116.73(2) . . ?
N1 Cu1 Cu2 123.12(11) . . ?
I3 Cu1 Cu2 135.41(2) . . ?
I2 Cu1 Cu2 55.403(18) . . ?
I1 Cu1 Cu2 55.243(18) . . ?
Cu3 Cu1 Cu2 88.36(2) . . ?
N3 Cu2 I2 113.60(10) . . ?
N3 Cu2 I1 107.56(11) . . ?
I2 Cu2 I1 114.35(2) . . ?
N3 Cu2 Cu2 116.48(11) . 2_656 ?
I2 Cu2 Cu2 128.05(3) . 2_656 ?
I1 Cu2 Cu2 61.80(2) . 2_656 ?
N3 Cu2 I1 98.42(11) . 2_656 ?
I2 Cu2 I1 101.95(2) . 2_656 ?
I1 Cu2 I1 120.09(2) . 2_656 ?
Cu2 Cu2 I1 58.29(2) 2_656 2_656 ?
N3 Cu2 Cu1 128.16(11) . . ?
I2 Cu2 Cu1 56.701(18) . . ?
I1 Cu2 Cu1 57.703(19) . . ?
Cu2 Cu2 Cu1 99.65(3) 2_656 . ?
I1 Cu2 Cu1 132.87(2) 2_656 . ?
N4 Cu3 S1 86.95(10) . . ?
N4 Cu3 I3 126.37(11) . . ?
S1 Cu3 I3 130.44(4) . . ?
N4 Cu3 Cu1 121.08(10) . . ?
S1 Cu3 Cu1 137.74(4) . . ?
I3 Cu3 Cu1 59.805(19) . . ?
N4 Cu3 I2 104.56(10) . . ?
S1 Cu3 I2 88.14(3) . . ?
I3 Cu3 I2 112.23(2) . . ?
Cu1 Cu3 I2 56.311(19) . . ?
Cu2 I1 Cu1 67.05(2) . . ?
Cu2 I1 Cu2 59.91(2) . 2_656 ?
Cu1 I1 Cu2 104.70(2) . 2_656 ?
Cu2 I2 Cu1 67.90(2) . . ?
Cu2 I2 Cu3 93.51(2) . . ?
Cu1 I2 Cu3 60.345(18) . . ?
Cu3 I3 Cu1 64.84(2) . . ?
C3 N1 C4 117.0(4) . . ?
C3 N1 Cu1 119.6(3) . . ?
C4 N1 Cu1 123.1(3) . . ?
C2 N2 C5 118.1(4) . . ?
C10 N3 C9 116.8(4) . . ?
C10 N3 Cu2 119.5(3) . . ?
C9 N3 Cu2 123.1(3) . . ?
C8 N4 C11 117.4(4) . . ?
C8 N4 Cu3 115.3(3) . . ?
C11 N4 Cu3 127.1(3) . . ?
C7 S1 C6 100.4(2) . . ?
C7 S1 Cu3 90.72(17) . . ?
C6 S1 Cu3 119.09(17) . . ?
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 C2 1.497(7) . ?
C2 N2 1.336(6) . ?
C2 C3 1.399(7) . ?
C3 N1 1.332(6) . ?
C4 N1 1.340(6) . ?
C4 C5 1.387(6) . ?
C5 N2 1.338(6) . ?
C5 C6 1.488(6) 1_645 ?
C6 C5 1.488(6) 1_465 ?
C6 S1 1.821(5) . ?
C7 C8 1.497(6) . ?
C7 S1 1.818(5) . ?
C8 N4 1.342(6) . ?
C8 C9 1.391(6) 2_566 ?
C9 N3 1.339(6) . ?
C9 C8 1.391(6) 2_566 ?
C10 N3 1.336(6) . ?
C10 C11 1.381(6) 2_566 ?
C11 N4 1.371(6) . ?
C11 C10 1.381(6) 2_566 ?
C11 C12 1.486(7) . ?
Cu1 N1 2.069(4) . ?
Cu1 I3 2.6323(7) . ?
Cu1 I2 2.6392(7) . ?
Cu1 I1 2.6855(7) . ?
Cu1 Cu3 2.7565(8) . ?
Cu1 Cu2 2.9256(9) . ?
Cu2 N3 2.052(4) . ?
Cu2 I2 2.5993(6) . ?
Cu2 I1 2.6101(7) . ?
Cu2 Cu2 2.6545(11) 2_656 ?
Cu2 I1 2.7040(7) 2_656 ?
Cu3 N4 2.071(3) . ?
Cu3 S1 2.3574(13) . ?
Cu3 I3 2.5055(7) . ?
Cu3 I2 2.8348(7) . ?
I1 Cu2 2.7040(7) 2_656 ?
