#------------------------------------------------------------------------------
#$Date: 2017-04-05 12:28:38 +0300 (Wed, 05 Apr 2017) $
#$Revision: 195004 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/49/1544984.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_1544984
loop_
_publ_author_name
'Lee, Hyeong-Hwan'
'Park, In-Hyeok'
'Kim, Seulgi'
'Lee, Eunji'
'Ju, Huiyeong'
'Jung, Jong Hwa'
'Ikeda, Mari'
'Habata, Yoichi'
'Lee, Shim Sung'
_publ_section_title
;
 Anion exchange coupled with the reduction and dimerisation of a
 copper(ii) nitrate complex of tripyridyl dithioether via a
 single-crystal-to-single-crystal transformation
;
_journal_issue                   4
_journal_name_full               'Chem. Sci.'
_journal_page_first              2592
_journal_paper_doi               10.1039/C6SC05341F
_journal_volume                  8
_journal_year                    2017
_chemical_formula_sum            'C34 H30 Cu4 I4 N6 S4'
_chemical_formula_weight         1412.64
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-12-31 deposited with the CCDC.
2017-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                101.5230(10)
_cell_angle_beta                 102.9950(10)
_cell_angle_gamma                104.2830(10)
_cell_formula_units_Z            1
_cell_length_a                   8.81100(10)
_cell_length_b                   10.09970(10)
_cell_length_c                   12.5440(2)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.49
_cell_volume                     1014.82(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16176
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         1.730
_exptl_absorpt_coefficient_mu    5.350
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.311
_exptl_crystal_description       block
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.110
_exptl_transmission_factor_max   0.5910
_exptl_transmission_factor_min   0.2710
_refine_diff_density_max         0.655
_refine_diff_density_min         -1.002
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3994
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0184
_refine_ls_R_factor_gt           0.0171
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0214P)²+0.5021P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0438
_refine_ls_wR_factor_ref         0.0445
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3791
_reflns_number_total             3994
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6sc05341f2.cif
_cod_data_source_block           1b
_cod_depositor_comments
'Adding full bibliography for 1544983--1544989.cif.'
_cod_database_code               1544984
_shelx_shelxl_version_number     2014/7
_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   0.271
_shelx_estimated_absorpt_t_max   0.591
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Cu1 Cu -0.42863(4) 0.65971(3) 0.57566(3) 0.02696(8) Uani 1 1 d . .
Cu2 Cu -0.74022(4) 0.48281(3) 0.31094(3) 0.02692(8) Uani 1 1 d . .
I1 I -0.42583(2) 0.56496(2) 0.36053(2) 0.02036(5) Uani 1 1 d . .
I2 I -0.11337(2) 0.77569(2) 0.69845(2) 0.03091(6) Uani 1 1 d . .
S1 S -0.82146(7) 0.60537(6) 0.46914(5) 0.02272(12) Uani 1 1 d . .
S2 S -0.68327(9) 0.56462(7) -0.05996(5) 0.03318(15) Uani 1 1 d . .
N2 N -0.8519(2) 0.5942(2) 0.21619(17) 0.0232(4) Uani 1 1 d . .
N1 N -0.5482(2) 0.81001(19) 0.58374(16) 0.0210(4) Uani 1 1 d . .
N3 N -0.4674(3) 0.7993(2) 0.09246(18) 0.0344(5) Uani 1 1 d . .
C1 C -0.4575(3) 0.9455(2) 0.63794(19) 0.0245(5) Uani 1 1 d . .
H1A H -0.3458 0.9635 0.6773 0.029 Uiso 1 1 calc R U
C2 C -0.5179(3) 1.0597(2) 0.6394(2) 0.0282(5) Uani 1 1 d . .
H2A H -0.4496 1.1536 0.6786 0.034 Uiso 1 1 calc R U
C3 C -0.6793(3) 1.0336(3) 0.5828(2) 0.0314(6) Uani 1 1 d . .
H3A H -0.7238 1.1100 0.5810 0.038 Uiso 1 1 calc R U
C4 C -0.7764(3) 0.8961(3) 0.5284(2) 0.0286(5) Uani 1 1 d . .
H4A H -0.8888 0.8763 0.4902 0.034 Uiso 1 1 calc R U
C5 C -0.7071(3) 0.7868(2) 0.53058(19) 0.0218(5) Uani 1 1 d . .
C6 C -0.9932(3) 0.6122(3) 0.3614(2) 0.0283(5) Uani 1 1 d . .
H6A H -1.0754 0.5169 0.3323 0.034 Uiso 1 1 calc R U
H6B H -1.0449 0.6786 0.3971 0.034 Uiso 1 1 calc R U
C7 C -0.9485(3) 0.6582(3) 0.2627(2) 0.0265(5) Uani 1 1 d . .
C8 C -1.0103(3) 0.7558(3) 0.2188(3) 0.0353(6) Uani 1 1 d . .
H8A H -1.0760 0.8010 0.2540 0.042 Uiso 1 1 calc R U
C9 C -0.9747(4) 0.7862(3) 0.1234(3) 0.0416(7) Uani 1 1 d . .
H9A H -1.0150 0.8534 0.0922 0.050 Uiso 1 1 calc R U
C10 C -0.8798(3) 0.7180(3) 0.0733(2) 0.0364(6) Uani 1 1 d . .
H10A H -0.8561 0.7366 0.0065 0.044 Uiso 1 1 calc R U
C11 C -0.8195(3) 0.6223(3) 0.1217(2) 0.0267(5) Uani 1 1 d . .
C12 C -0.7118(3) 0.5458(3) 0.0754(2) 0.0296(5) Uani 1 1 d . .
H12A H -0.7581 0.4435 0.0680 0.036 Uiso 1 1 calc R U
H12B H -0.6028 0.5795 0.1322 0.036 Uiso 1 1 calc R U
C13 C -0.5248(3) 0.7284(3) -0.0167(2) 0.0272(5) Uani 1 1 d . .
C14 C -0.4663(4) 0.7759(3) -0.1005(2) 0.0388(7) Uani 1 1 d . .
H14A H -0.5115 0.7226 -0.1779 0.047 Uiso 1 1 calc R U
C15 C -0.3424(4) 0.9005(3) -0.0696(2) 0.0411(7) Uani 1 1 d . .
H15A H -0.2994 0.9350 -0.1253 0.049 Uiso 1 1 calc R U
C16 C -0.2803(3) 0.9758(3) 0.0434(2) 0.0343(6) Uani 1 1 d . .
H16A H -0.1942 1.0630 0.0673 0.041 Uiso 1 1 calc R U
C17 C -0.3462(3) 0.9214(3) 0.1199(2) 0.0367(6) Uani 1 1 d . .
H17A H -0.3033 0.9736 0.1976 0.044 Uiso 1 1 calc R U
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
N1 Cu1 I1 112.48(5) . 2_466
N1 Cu1 I1 109.23(5) . .
I1 Cu1 I1 107.481(11) 2_466 .
N1 Cu1 I2 110.39(6) . .
I1 Cu1 I2 111.229(12) 2_466 .
I1 Cu1 I2 105.756(12) . .
N1 Cu1 Cu2 147.32(5) . 2_466
I1 Cu1 Cu2 57.323(9) 2_466 2_466
I1 Cu1 Cu2 103.403(12) . 2_466
I2 Cu1 Cu2 57.307(10) . 2_466
N2 Cu2 S1 86.22(6) . .
N2 Cu2 I1 114.19(6) . .
S1 Cu2 I1 108.736(18) . .
N2 Cu2 I2 121.61(5) . 2_466
S1 Cu2 I2 98.953(17) . 2_466
I1 Cu2 I2 118.498(12) . 2_466
N2 Cu2 Cu1 174.38(6) . 2_466
S1 Cu2 Cu1 98.224(18) . 2_466
I1 Cu2 Cu1 61.171(10) . 2_466
I2 Cu2 Cu1 61.268(10) 2_466 2_466
Cu2 I1 Cu1 61.507(10) . 2_466
Cu2 I1 Cu1 85.951(10) . .
Cu1 I1 Cu1 72.518(11) 2_466 .
Cu2 I2 Cu1 61.426(10) 2_466 .
C5 S1 C6 102.94(12) . .
C5 S1 Cu2 115.04(7) . .
C6 S1 Cu2 86.48(8) . .
C13 S2 C12 101.12(12) . .
C11 N2 C7 119.0(2) . .
C11 N2 Cu2 125.04(17) . .
C7 N2 Cu2 115.40(16) . .
C5 N1 C1 117.0(2) . .
C5 N1 Cu1 125.32(15) . .
C1 N1 Cu1 117.36(16) . .
C13 N3 C17 116.6(2) . .
N1 C1 C2 123.7(2) . .
C3 C2 C1 118.1(2) . .
C2 C3 C4 119.7(2) . .
C3 C4 C5 118.9(2) . .
N1 C5 C4 122.5(2) . .
N1 C5 S1 114.44(17) . .
C4 C5 S1 122.99(19) . .
C7 C6 S1 114.17(17) . .
N2 C7 C8 122.1(2) . .
N2 C7 C6 116.4(2) . .
C8 C7 C6 121.4(2) . .
C9 C8 C7 118.8(3) . .
C8 C9 C10 119.5(3) . .
C9 C10 C11 119.3(3) . .
N2 C11 C10 121.3(2) . .
N2 C11 C12 115.4(2) . .
C10 C11 C12 123.3(2) . .
C11 C12 S2 117.00(18) . .
N3 C13 C14 123.1(2) . .
N3 C13 S2 119.5(2) . .
C14 C13 S2 117.37(19) . .
C15 C14 C13 118.7(2) . .
C14 C15 C16 119.2(3) . .
C17 C16 C15 118.0(3) . .
N3 C17 C16 124.3(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 2.0493(19) .
Cu1 I1 2.6806(3) 2_466
Cu1 I1 2.6848(3) .
Cu1 I2 2.6851(3) .
Cu1 Cu2 2.6892(4) 2_466
Cu2 N2 2.050(2) .
Cu2 S1 2.4652(6) .
Cu2 I1 2.5755(3) .
Cu2 I2 2.5771(3) 2_466
Cu2 Cu1 2.6892(4) 2_466
I1 Cu1 2.6806(3) 2_466
I2 Cu2 2.5770(3) 2_466
S1 C5 1.773(2) .
S1 C6 1.814(3) .
S2 C13 1.772(3) .
S2 C12 1.811(3) .
N2 C11 1.346(3) .
N2 C7 1.352(3) .
N1 C5 1.348(3) .
N1 C1 1.348(3) .
N3 C13 1.327(3) .
N3 C17 1.340(3) .
C1 C2 1.383(3) .
C2 C3 1.372(4) .
C3 C4 1.378(4) .
C4 C5 1.388(3) .
C6 C7 1.504(4) .
C7 C8 1.385(3) .
C8 C9 1.375(4) .
C9 C10 1.384(4) .
C10 C11 1.389(4) .
C11 C12 1.505(3) .
C13 C14 1.387(4) .
C14 C15 1.365(4) .
C15 C16 1.379(4) .
C16 C17 1.365(4) .
