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#$Date: 2020-06-06 08:28:45 +0300 (Sat, 06 Jun 2020) $
#$Revision: 252979 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/34/2243422.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2243422
loop_
_publ_author_name
'Assoumatine, Tokouré'
'Stoeckli-Evans, Helen'
_publ_section_title
;
 Crystal structures of [(μ₂-L1)dibromidodicopper(II)] dibromide and
 poly[[(μ₂-L1)diiodidodicopper(I)]-di-μ-iodido-dicopper(I)], where L1
 is 2,5,8,11,14,17-hexathia-[9.9](2,6,3,5)-pyrazinophane
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              984
_journal_page_last               989
_journal_paper_doi               10.1107/S2056989020007161
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          '[Cu4 I4 (C16 H24 N2 S6)]'
_chemical_formula_moiety         'C16 H24 Cu4 I4 N2 S6'
_chemical_formula_sum            'C16 H24 Cu4 I4 N2 S6'
_chemical_formula_weight         1198.49
_chemical_name_systematic
Poly[[μ₂-2,5,8,11,14,17-hexathia-[9.9](2,6,3,5)-pyrazinophane]tetra-μ-iodido-tetracopper(I)]
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                106.839(13)
_cell_angle_beta                 104.644(13)
_cell_angle_gamma                93.412(12)
_cell_formula_units_Z            1
_cell_length_a                   7.7713(8)
_cell_length_b                   8.9456(9)
_cell_length_c                   11.2464(14)
_cell_measurement_reflns_used    4652
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.79
_cell_measurement_theta_min      1.97
_cell_volume                     716.53(16)
_computing_cell_refinement
;
CELL in IPDS-I (Stoe & Cie, 1997)
;
_computing_data_collection
;
EXPOSE in IPDS-I (Stoe & Cie, 1997)
;
_computing_data_reduction
;
INTEGRATE in IPDS-I (Stoe & Cie, 1997)
;
_computing_molecular_graphics
;
Mercury (Macrae et al.,  2020)
;
_computing_publication_material
;
SHELXL2018/3 (Sheldrick, 2015), PLATON (Spek, 2020) and
publcif (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS-97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'image plate'
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device       '1 circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 1'
_diffrn_measurement_method       'φ rotation'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0996
_diffrn_reflns_av_unetI/netI     0.1159
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5260
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.490
_diffrn_reflns_theta_min         2.404
_exptl_absorpt_coefficient_mu    7.686
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4346
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(MULABS; Spek, 2020)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.777
_exptl_crystal_description       plate
_exptl_crystal_F_000             558
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.251
_refine_diff_density_min         -2.577
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         2505
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.0923
_refine_ls_R_factor_gt           0.0699
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1100P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1760
_refine_ls_wR_factor_ref         0.1834
_reflns_number_gt                1698
_reflns_number_total             2505
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            pk2634sup1.cif
_cod_data_source_block           II
_cod_original_cell_volume        716.53(15)
_cod_database_code               2243422
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.206
_shelx_estimated_absorpt_t_max   0.700
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I I1 0.73534(12) 0.70224(11) 0.11663(9) 0.0396(3) Uani d 1 . .
I I2 0.34990(12) 0.56223(11) 0.29340(9) 0.0370(3) Uani d 1 . .
Cu Cu1 1.2404(2) 0.2890(2) 0.28830(16) 0.0332(4) Uani d 1 . .
Cu Cu2 0.5027(2) 0.4653(2) 0.10778(18) 0.0415(5) Uani d 1 . .
S S1 1.3999(4) 0.0851(4) 0.3255(3) 0.0326(8) Uani d 1 . .
S S2 1.1079(5) 0.2923(4) 0.4531(3) 0.0349(8) Uani d 1 . .
S S3 0.6749(4) 0.2663(4) 0.1450(3) 0.0296(7) Uani d 1 . .
N N1 1.0914(12) 0.1189(12) 0.1149(10) 0.025(2) Uani d 1 . .
C C1 0.9371(16) 0.1373(15) 0.0368(12) 0.0238(18) Uani d 1 . .
C C2 1.1538(15) -0.0213(15) 0.0762(11) 0.0238(18) Uani d 1 . .
C C3 1.3271(19) -0.0448(18) 0.1606(13) 0.038(3) Uani d 1 . .
H H3A 1.421167 -0.033142 0.120089 0.046 Uiso calc 1 . .
H H3B 1.314897 -0.152610 0.162526 0.046 Uiso calc 1 . .
C C4 1.2385(17) 0.0077(18) 0.3947(13) 0.035(3) Uani d 1 . .
H H4A 1.126049 -0.037376 0.327911 0.042 Uiso calc 1 . .
H H4B 1.284935 -0.075140 0.427765 0.042 Uiso calc 1 . .
C C5 1.206(2) 0.1374(18) 0.5023(14) 0.039(2) Uani d 1 . .
H H5A 1.319763 0.181893 0.567821 0.047 Uiso calc 1 . .
H H5B 1.127970 0.092387 0.541897 0.047 Uiso calc 1 . .
C C6 0.8751(19) 0.2106(18) 0.3709(14) 0.039(2) Uani d 1 . .
H H6A 0.868179 0.113955 0.301594 0.047 Uiso calc 1 . .
H H6B 0.817806 0.185297 0.431304 0.047 Uiso calc 1 . .
C C7 0.7789(16) 0.3263(16) 0.3162(12) 0.030(2) Uani d 1 . .
H H7A 0.864140 0.420800 0.338968 0.036 Uiso calc 1 . .
H H7B 0.686666 0.355435 0.359299 0.036 Uiso calc 1 . .
C C8 0.8623(16) 0.2892(16) 0.0814(13) 0.030(2) Uani d 1 . .
H H8A 0.824277 0.329504 0.008985 0.036 Uiso calc 1 . .
H H8B 0.956964 0.366690 0.147795 0.036 Uiso calc 1 . .
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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Cu1 S2 . . 110.2(3) y
N1 Cu1 S1 . . 85.3(3) y
S2 Cu1 S1 . . 91.74(14) y
N1 Cu1 I2 . 1_655 121.1(3) y
S2 Cu1 I2 . 1_655 112.48(12) y
S1 Cu1 I2 . 1_655 130.61(10) y
S3 Cu2 I2 . . 109.54(11) y
S3 Cu2 I1 . . 105.86(10) y
I2 Cu2 I1 . . 109.04(8) y
S3 Cu2 I1 . 2_665 99.22(11) y
I2 Cu2 I1 . 2_665 112.01(7) y
I1 Cu2 I1 . 2_665 120.18(7) y
Cu2 I1 Cu2 . 2_665 59.82(7) y
Cu1 I2 Cu2 1_455 . 94.93(7) y
Cu2 Cu2 I1 2_665 . 60.27(7) y
Cu2 Cu2 I1 2_665 2_665 59.91(7) y
S3 Cu2 Cu2 . 2_665 115.75(13) y
I2 Cu2 Cu2 . 2_665 134.68(11) y
C3 S1 C4 . . 100.9(7) ?
C3 S1 Cu1 . . 96.4(5) ?
C4 S1 Cu1 . . 94.5(5) ?
C5 S2 C6 . . 104.7(7) ?
C5 S2 Cu1 . . 98.8(5) ?
C6 S2 Cu1 . . 105.0(5) ?
C7 S3 C8 . . 102.8(6) ?
C7 S3 Cu2 . . 106.0(4) ?
C8 S3 Cu2 . . 105.2(5) ?
C1 N1 C2 . . 116.6(10) ?
C1 N1 Cu1 . . 124.9(9) ?
C2 N1 Cu1 . . 118.5(8) ?
N1 C1 C2 . 2_755 122.1(12) ?
N1 C1 C8 . . 117.1(11) ?
C2 C1 C8 2_755 . 120.8(11) ?
N1 C2 C1 . 2_755 121.3(11) ?
N1 C2 C3 . . 117.9(11) ?
C1 C2 C3 2_755 . 120.7(12) ?
C2 C3 S1 . . 116.7(10) ?
C2 C3 H3A . . 108.1 ?
S1 C3 H3A . . 108.1 ?
C2 C3 H3B . . 108.1 ?
S1 C3 H3B . . 108.1 ?
H3A C3 H3B . . 107.3 ?
C5 C4 S1 . . 110.1(10) ?
C5 C4 H4A . . 109.6 ?
S1 C4 H4A . . 109.6 ?
C5 C4 H4B . . 109.6 ?
S1 C4 H4B . . 109.6 ?
H4A C4 H4B . . 108.2 ?
C4 C5 S2 . . 114.4(10) ?
C4 C5 H5A . . 108.7 ?
S2 C5 H5A . . 108.7 ?
C4 C5 H5B . . 108.7 ?
S2 C5 H5B . . 108.7 ?
H5A C5 H5B . . 107.6 ?
C7 C6 S2 . . 110.2(10) ?
C7 C6 H6A . . 109.6 ?
S2 C6 H6A . . 109.6 ?
C7 C6 H6B . . 109.6 ?
S2 C6 H6B . . 109.6 ?
H6A C6 H6B . . 108.1 ?
C6 C7 S3 . . 117.8(10) ?
C6 C7 H7A . . 107.9 ?
S3 C7 H7A . . 107.9 ?
C6 C7 H7B . . 107.9 ?
S3 C7 H7B . . 107.9 ?
H7A C7 H7B . . 107.2 ?
C1 C8 S3 . . 113.2(9) ?
C1 C8 H8A . . 108.9 ?
S3 C8 H8A . . 108.9 ?
C1 C8 H8B . . 108.9 ?
S3 C8 H8B . . 108.9 ?
H8A C8 H8B . . 107.7 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 N1 . 2.095(10) y
Cu1 S1 . 2.342(4) y
Cu1 S2 . 2.331(4) y
Cu1 I2 1_655 2.5193(18) y
Cu2 S3 . 2.359(4) y
Cu2 I1 . 2.665(2) y
Cu2 I2 . 2.6166(19) y
I1 Cu2 2_665 2.675(2) y
Cu2 Cu2 2_665 2.663(4) y
S1 C3 . 1.803(13) ?
S1 C4 . 1.834(13) ?
S2 C5 . 1.779(16) ?
S2 C6 . 1.808(14) ?
S3 C7 . 1.793(13) ?
S3 C8 . 1.803(12) ?
N1 C1 . 1.346(16) ?
N1 C2 . 1.364(16) ?
C1 C2 2_755 1.373(17) ?
C1 C8 . 1.511(18) ?
C2 C3 . 1.504(19) ?
C3 H3A . 0.9700 ?
C3 H3B . 0.9700 ?
C4 C5 . 1.50(2) ?
C4 H4A . 0.9700 ?
C4 H4B . 0.9700 ?
C5 H5A . 0.9700 ?
C5 H5B . 0.9700 ?
C6 C7 . 1.50(2) ?
C6 H6A . 0.9700 ?
C6 H6B . 0.9700 ?
C7 H7A . 0.9700 ?
C7 H7B . 0.9700 ?
C8 H8A . 0.9700 ?
C8 H8B . 0.9700 ?
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C2 N1 C1 C2 . . . 2_755 0.0(19) ?
Cu1 N1 C1 C2 . . . 2_755 179.6(9) ?
C2 N1 C1 C8 . . . . 177.4(10) ?
Cu1 N1 C1 C8 . . . . -3.0(15) ?
C1 N1 C2 C1 . . . 2_755 0.0(19) ?
Cu1 N1 C2 C1 . . . 2_755 -179.6(9) ?
C1 N1 C2 C3 . . . . 179.3(11) ?
Cu1 N1 C2 C3 . . . . -0.3(15) ?
N1 C2 C3 S1 . . . . 18.3(17) ?
C1 C2 C3 S1 2_755 . . . -162.3(10) ?
C4 S1 C3 C2 . . . . 72.6(13) ?
Cu1 S1 C3 C2 . . . . -23.2(12) ?
C3 S1 C4 C5 . . . . -150.3(10) ?
Cu1 S1 C4 C5 . . . . -52.9(10) ?
S1 C4 C5 S2 . . . . 62.8(12) ?
C6 S2 C5 C4 . . . . 74.9(11) ?
Cu1 S2 C5 C4 . . . . -33.3(10) ?
C5 S2 C6 C7 . . . . -176.2(10) ?
Cu1 S2 C6 C7 . . . . -72.6(10) ?
S2 C6 C7 S3 . . . . 121.3(9) ?
C8 S3 C7 C6 . . . . -78.8(11) ?
Cu2 S3 C7 C6 . . . . 171.0(9) ?
N1 C1 C8 S3 . . . . -103.2(11) ?
C2 C1 C8 S3 2_755 . . . 74.2(14) ?
C7 S3 C8 C1 . . . . 96.8(10) ?
Cu2 S3 C8 C1 . . . . -152.4(8) ?

_cod_database_fobs_code 2243422
