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#$Date: 2017-04-05 12:28:38 +0300 (Wed, 05 Apr 2017) $
#$Revision: 195004 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/49/1544985.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_1544985
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            'C35 H32 Cl2 Cu4 I4 N6 S4'
_chemical_formula_weight         1497.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                90
_cell_angle_beta                 109.4630(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.2650(8)
_cell_length_b                   16.1159(5)
_cell_length_c                   10.1658(3)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.37
_cell_measurement_theta_min      2.37
_cell_volume                     4366.1(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 0.999
_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  0.0449
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            18913
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.369
_exptl_absorpt_coefficient_mu    5.100
_exptl_absorpt_correction_T_max  0.6858
_exptl_absorpt_correction_T_min  0.2178
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.278
_exptl_crystal_description       needle
_exptl_crystal_F_000             2840
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.352
_refine_diff_density_min         -1.413
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         4306
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0441P)²+12.2274P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0801
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3968
_reflns_number_total             4306
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6sc05341f2.cif
_cod_data_source_block           1c
_cod_depositor_comments
'Adding full bibliography for 1544983--1544989.cif.'
_cod_database_code               1544985
_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   0.218
_shelx_estimated_absorpt_t_max   0.686
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
_atom_site_refinement_flags_occupancy
Cu1 Cu 0.21792(2) 0.24622(3) 0.35186(5) 0.02363(13) Uani 1 1 d . . .
Cu2 Cu 0.15648(2) 0.28076(3) 0.51500(5) 0.02337(13) Uani 1 1 d . . .
I1 I 0.20759(2) 0.14433(2) 0.55015(2) 0.02014(9) Uani 1 1 d . . .
I2 I 0.13292(2) 0.33355(2) 0.26083(3) 0.02370(9) Uani 1 1 d . . .
S1 S 0.20377(4) 0.40222(6) 0.62942(9) 0.0212(2) Uani 1 1 d . . .
S2 S 0.02239(5) 0.17704(8) 0.43351(12) 0.0406(3) Uani 1 1 d . . .
N1 N 0.27385(12) 0.3163(2) 0.8156(3) 0.0211(7) Uani 1 1 d . . .
N2 N 0.11185(12) 0.3022(2) 0.6363(3) 0.0225(7) Uani 1 1 d . . .
N3 N -0.01715(14) 0.0801(2) 0.5819(4) 0.0318(8) Uani 1 1 d . . .
C1 C 0.30270(16) 0.2944(3) 0.9452(4) 0.0254(9) Uani 1 1 d . . .
H1A H 0.3270 0.2520 0.9554 0.031 Uiso 1 1 calc R U .
C2 C 0.29862(16) 0.3305(3) 1.0642(4) 0.0283(9) Uani 1 1 d . . .
H2A H 0.3193 0.3126 1.1539 0.034 Uiso 1 1 calc R U .
C3 C 0.26382(17) 0.3933(3) 1.0504(4) 0.0317(10) Uani 1 1 d . . .
H3A H 0.2603 0.4193 1.1305 0.038 Uiso 1 1 calc R U .
C4 C 0.23440(16) 0.4171(3) 0.9187(4) 0.0251(9) Uani 1 1 d . . .
H4A H 0.2107 0.4607 0.9065 0.030 Uiso 1 1 calc R U .
C5 C 0.23961(14) 0.3768(2) 0.8043(4) 0.0196(8) Uani 1 1 d . . .
C6 C 0.14587(15) 0.4418(3) 0.6459(4) 0.0259(9) Uani 1 1 d . . .
H6A H 0.1538 0.4893 0.7113 0.031 Uiso 1 1 calc R U .
H6B H 0.1242 0.4625 0.5538 0.031 Uiso 1 1 calc R U .
C7 C 0.11737(15) 0.3780(3) 0.6972(4) 0.0252(9) Uani 1 1 d . . .
C8 C 0.09622(16) 0.3974(3) 0.7979(4) 0.0354(11) Uani 1 1 d . . .
H8A H 0.0999 0.4515 0.8369 0.043 Uiso 1 1 calc R U .
C9 C 0.06975(18) 0.3377(3) 0.8415(5) 0.0401(12) Uani 1 1 d . . .
H9A H 0.0561 0.3493 0.9132 0.048 Uiso 1 1 calc R U .
C10 C 0.06355(16) 0.2607(3) 0.7783(5) 0.0356(11) Uani 1 1 d . . .
H10A H 0.0455 0.2185 0.8064 0.043 Uiso 1 1 calc R U .
C11 C 0.08385(15) 0.2452(3) 0.6731(4) 0.0277(9) Uani 1 1 d . . .
C12 C 0.07456(17) 0.1649(3) 0.5959(5) 0.0329(10) Uani 1 1 d . . .
H12A H 0.0666 0.1213 0.6538 0.039 Uiso 1 1 calc R U .
H12B H 0.1051 0.1478 0.5756 0.039 Uiso 1 1 calc R U .
C13 C -0.02639(16) 0.1201(3) 0.4617(4) 0.0264(9) Uani 1 1 d . . .
C14 C -0.0563(2) 0.0381(3) 0.5978(6) 0.0470(14) Uani 1 1 d . . .
H14A H -0.0509 0.0095 0.6832 0.056 Uiso 1 1 calc R U .
C15 C -0.1022(2) 0.0340(4) 0.5014(7) 0.0553(16) Uani 1 1 d . . .
H15A H -0.1283 0.0039 0.5194 0.066 Uiso 1 1 calc R U .
C16 C -0.11080(19) 0.0739(4) 0.3770(7) 0.0521(15) Uani 1 1 d . . .
H16A H -0.1427 0.0705 0.3062 0.063 Uiso 1 1 calc R U .
C17 C -0.07288(18) 0.1188(3) 0.3555(5) 0.0391(11) Uani 1 1 d . . .
H17A H -0.0781 0.1481 0.2708 0.047 Uiso 1 1 calc R U .
C18 C 0.0000 0.3702(4) 0.2500 0.0336(14) Uani 1 2 d S T P
H18A H -0.0293 0.3341 0.2404 0.040 Uiso 0.5 1 calc R U P
H18B H 0.0293 0.3341 0.2596 0.040 Uiso 0.5 1 calc R U P
Cl1 Cl 0.01217(5) 0.43207(9) 0.40058(13) 0.0482(3) 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'
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
N1 Cu1 I2 107.96(9) 7_556 .
N1 Cu1 I1 109.86(9) 7_556 7_556
I2 Cu1 I1 106.712(19) . 7_556
N1 Cu1 I1 113.04(9) 7_556 .
I2 Cu1 I1 105.756(18) . .
I1 Cu1 I1 113.102(17) 7_556 .
N1 Cu1 Cu2 147.42(9) 7_556 .
I2 Cu1 Cu2 56.071(15) . .
I1 Cu1 Cu2 102.299(19) 7_556 .
I1 Cu1 Cu2 55.904(14) . .
N1 Cu1 Cu1 131.56(10) 7_556 7_556
I2 Cu1 Cu1 120.47(3) . 7_556
I1 Cu1 Cu1 56.850(17) 7_556 7_556
I1 Cu1 Cu1 56.252(16) . 7_556
Cu2 Cu1 Cu1 71.47(2) . 7_556
N2 Cu2 S1 85.84(10) . .
N2 Cu2 I2 122.39(9) . .
S1 Cu2 I2 97.49(3) . .
N2 Cu2 I1 118.90(9) . .
S1 Cu2 I1 115.11(3) . .
I2 Cu2 I1 111.294(18) . .
N2 Cu2 Cu1 178.22(10) . .
S1 Cu2 Cu1 95.27(3) . .
I2 Cu2 Cu1 58.882(15) . .
I1 Cu2 Cu1 59.361(15) . .
Cu2 I1 Cu1 79.917(17) . 7_556
Cu2 I1 Cu1 64.734(16) . .
Cu1 I1 Cu1 66.899(17) 7_556 .
Cu2 I2 Cu1 65.047(15) . .
C5 S1 C6 102.71(18) . .
C5 S1 Cu2 109.37(13) . .
C6 S1 Cu2 87.61(14) . .
C13 S2 C12 103.8(2) . .
C1 N1 C5 117.1(3) . .
C1 N1 Cu1 118.9(3) . 7_556
C5 N1 Cu1 123.9(3) . 7_556
C11 N2 C7 118.6(3) . .
C11 N2 Cu2 125.8(3) . .
C7 N2 Cu2 115.1(3) . .
C13 N3 C14 115.8(4) . .
N1 C1 C2 123.1(4) . .
C1 C2 C3 118.9(4) . .
C4 C3 C2 118.7(4) . .
C3 C4 C5 119.3(4) . .
N1 C5 C4 122.8(4) . .
N1 C5 S1 113.9(3) . .
C4 C5 S1 123.3(3) . .
C7 C6 S1 113.3(3) . .
N2 C7 C8 122.0(4) . .
N2 C7 C6 116.9(3) . .
C8 C7 C6 121.1(4) . .
C9 C8 C7 119.7(5) . .
C8 C9 C10 118.3(4) . .
C9 C10 C11 119.8(4) . .
N2 C11 C10 121.4(4) . .
N2 C11 C12 117.6(4) . .
C10 C11 C12 121.0(4) . .
C11 C12 S2 109.4(3) . .
N3 C13 C17 123.4(4) . .
N3 C13 S2 118.6(3) . .
C17 C13 S2 118.0(4) . .
C15 C14 N3 124.6(5) . .
C14 C15 C16 118.9(5) . .
C15 C16 C17 119.3(5) . .
C16 C17 C13 118.0(5) . .
Cl1 C18 Cl1 111.1(4) . 2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 2.057(3) 7_556
Cu1 I2 2.6700(6) .
Cu1 I1 2.6718(5) 7_556
Cu1 I1 2.6902(5) .
Cu1 Cu2 2.8276(7) .
Cu1 Cu1 2.9556(9) 7_556
Cu2 N2 2.066(3) .
Cu2 S1 2.4362(11) .
Cu2 I2 2.5877(5) .
Cu2 I1 2.5893(6) .
I1 Cu1 2.6718(5) 7_556
S1 C5 1.776(4) .
S1 C6 1.815(4) .
S2 C13 1.757(4) .
S2 C12 1.821(5) .
N1 C1 1.346(5) .
N1 C5 1.351(5) .
N1 Cu1 2.057(3) 7_556
N2 C11 1.345(5) .
N2 C7 1.354(5) .
N3 C13 1.328(6) .
N3 C14 1.352(6) .
C1 C2 1.381(6) .
C2 C3 1.385(6) .
C3 C4 1.375(6) .
C4 C5 1.382(5) .
C6 C7 1.503(6) .
C7 C8 1.382(6) .
C8 C9 1.378(7) .
C9 C10 1.382(7) .
C10 C11 1.395(6) .
C11 C12 1.490(6) .
C13 C17 1.396(6) .
C14 C15 1.341(8) .
C15 C16 1.366(9) .
C16 C17 1.370(8) .
C18 Cl1 1.762(4) .
C18 Cl1 1.762(4) 2
