#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:33:33 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179251 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/71/4317104.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_4317104
loop_
_publ_author_name
'Yongnu Jin'
'Hyun Jee Kim'
'Jai Young Lee'
'So Young Lee'
'Won Joon Shim'
'Sang Hee Hong'
'Shim Sung Lee'
_publ_section_title
;
 Hard/Soft Heterometallic Network Complex of a Macrocycle with
 Endo/Exocyclic Coordination
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10241
_journal_page_last               10243
_journal_paper_doi               10.1021/ic101880r
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C22 H28 Cu2 I2 O4 S2'
_chemical_formula_weight         801.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 104.7520(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.6184(3)
_cell_length_b                   13.4358(2)
_cell_length_c                   16.0851(2)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.62
_cell_volume                     5354.05(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0689
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24131
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    4.077
_exptl_absorpt_correction_T_max  0.6581
_exptl_absorpt_correction_T_min  0.4814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.989
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.779
_refine_diff_density_min         -0.902
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5847
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0244
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0279P)²+2.6129P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0605
_refine_ls_wR_factor_ref         0.0629
_reflns_number_gt                5206
_reflns_number_total             5847
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101880r_si_002_1.cif
_cod_data_source_block           complex1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4317104
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.481223(12) 0.72806(3) 1.16703(2) 0.03167(9) Uani 1 1 d . . .
Cu2 Cu 0.446619(12) 0.57976(2) 1.25338(2) 0.03040(8) Uani 1 1 d . . .
I1 I 0.472584(6) 0.543306(13) 1.105961(10) 0.02936(6) Uani 1 1 d . . .
I2 I 0.413516(6) 0.767492(13) 1.263974(11) 0.02997(6) Uani 1 1 d . . .
S1 S 0.45944(2) 0.84280(5) 1.05754(4) 0.03198(15) Uani 1 1 d . . .
S2 S 0.37639(2) 0.52897(5) 0.75303(4) 0.02821(14) Uani 1 1 d . . .
O1 O 0.27507(7) 0.60443(16) 0.85287(14) 0.0434(5) Uani 1 1 d . . .
O2 O 0.28838(7) 0.79462(16) 0.91199(14) 0.0450(5) Uani 1 1 d . . .
O3 O 0.43501(7) 0.84781(15) 0.84665(12) 0.0386(4) Uani 1 1 d . . .
O4 O 0.37225(9) 0.81190(15) 0.66935(13) 0.0478(5) Uani 1 1 d . . .
C1 C 0.23194(11) 0.6577(2) 0.8743(2) 0.0496(8) Uani 1 1 d . . .
H1A H 0.2334 0.6486 0.9359 0.060 Uiso 1 1 calc R . .
H1B H 0.1967 0.6329 0.8397 0.060 Uiso 1 1 calc R . .
C2 C 0.23864(11) 0.7650(2) 0.8554(2) 0.0507(9) Uani 1 1 d . . .
H2A H 0.2397 0.7740 0.7948 0.061 Uiso 1 1 calc R . .
H2B H 0.2084 0.8048 0.8659 0.061 Uiso 1 1 calc R . .
C3 C 0.30557(10) 0.8908(2) 0.90844(18) 0.0358(6) Uani 1 1 d . . .
C4 C 0.27484(12) 0.9658(3) 0.8594(2) 0.0483(8) Uani 1 1 d . . .
H4A H 0.2399 0.9517 0.8241 0.058 Uiso 1 1 calc R . .
C5 C 0.29564(14) 1.0600(3) 0.8628(2) 0.0521(9) Uani 1 1 d . . .
H5A H 0.2749 1.1113 0.8293 0.062 Uiso 1 1 calc R . .
C6 C 0.34602(14) 1.0814(2) 0.9139(2) 0.0506(8) Uani 1 1 d . . .
H6A H 0.3598 1.1472 0.9161 0.061 Uiso 1 1 calc R . .
C7 C 0.37707(12) 1.0058(2) 0.9629(2) 0.0421(7) Uani 1 1 d . . .
H7A H 0.4119 1.0207 0.9984 0.050 Uiso 1 1 calc R . .
C8 C 0.35732(10) 0.9097(2) 0.95976(17) 0.0310(6) Uani 1 1 d . . .
C9 C 0.38803(9) 0.8234(2) 1.00953(18) 0.0327(6) Uani 1 1 d . . .
H9A H 0.3841 0.7655 0.9704 0.039 Uiso 1 1 calc R . .
H9B H 0.3707 0.8057 1.0559 0.039 Uiso 1 1 calc R . .
C10 C 0.49197(11) 0.7912(2) 0.9789(2) 0.0438(7) Uani 1 1 d . . .
H10A H 0.5306 0.7801 1.0073 0.053 Uiso 1 1 calc R . .
H10B H 0.4757 0.7255 0.9603 0.053 Uiso 1 1 calc R . .
C11 C 0.48805(12) 0.8546(3) 0.9003(2) 0.0511(8) Uani 1 1 d . . .
H11A H 0.4966 0.9247 0.9175 0.061 Uiso 1 1 calc R . .
H11B H 0.5143 0.8312 0.8689 0.061 Uiso 1 1 calc R . .
C12 C 0.42614(13) 0.9198(2) 0.7797(2) 0.0465(7) Uani 1 1 d . . .
H12A H 0.4557 0.9163 0.7503 0.056 Uiso 1 1 calc R . .
H12B H 0.4262 0.9873 0.8044 0.056 Uiso 1 1 calc R . .
C13 C 0.37365(12) 0.9015(2) 0.71654(19) 0.0405(7) Uani 1 1 d . . .
H13A H 0.3448 0.8992 0.7475 0.049 Uiso 1 1 calc R . .
H13B H 0.3658 0.9580 0.6758 0.049 Uiso 1 1 calc R . .
C14 C 0.35498(13) 0.7256(2) 0.7058(2) 0.0412(7) Uani 1 1 d . . .
H14A H 0.3212 0.7000 0.6671 0.049 Uiso 1 1 calc R . .
H14B H 0.3477 0.7424 0.7617 0.049 Uiso 1 1 calc R . .
C15 C 0.39850(11) 0.6469(2) 0.71860(18) 0.0353(6) Uani 1 1 d . . .
H15A H 0.4308 0.6703 0.7623 0.042 Uiso 1 1 calc R . .
H15B H 0.4089 0.6371 0.6640 0.042 Uiso 1 1 calc R . .
C16 C 0.38039(10) 0.5559(2) 0.86593(17) 0.0302(6) Uani 1 1 d . . .
H16A H 0.4181 0.5474 0.9003 0.036 Uiso 1 1 calc R . .
H16B H 0.3698 0.6259 0.8716 0.036 Uiso 1 1 calc R . .
C17 C 0.34423(10) 0.4884(2) 0.90023(17) 0.0300(5) Uani 1 1 d . . .
C18 C 0.36302(13) 0.4001(2) 0.9420(2) 0.0426(7) Uani 1 1 d . . .
H18A H 0.3989 0.3791 0.9454 0.051 Uiso 1 1 calc R . .
C19 C 0.33055(18) 0.3425(3) 0.9786(2) 0.0606(10) Uani 1 1 d . . .
H19A H 0.3439 0.2825 1.0074 0.073 Uiso 1 1 calc R . .
C20 C 0.27832(18) 0.3728(3) 0.9730(3) 0.0669(11) Uani 1 1 d . . .
H20A H 0.2558 0.3328 0.9980 0.080 Uiso 1 1 calc R . .
C21 C 0.25823(13) 0.4593(3) 0.9320(2) 0.0516(9) Uani 1 1 d . . .
H21A H 0.2222 0.4793 0.9288 0.062 Uiso 1 1 calc R . .
C22 C 0.29129(10) 0.5174(2) 0.89521(18) 0.0358(6) 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'
O O 0.0106 0.0060 '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
S1 Cu1 Cu1 137.84(2) . 2_657 ?
S1 Cu1 I1 111.21(2) . . ?
Cu1 Cu1 I1 110.739(8) 2_657 . ?
S1 Cu1 I2 104.34(2) . . ?
Cu1 Cu1 I2 61.602(13) 2_657 . ?
I1 Cu1 I2 113.369(13) . . ?
S1 Cu1 I2 101.877(19) . 2_657 ?
Cu1 Cu1 I2 60.438(12) 2_657 2_657 ?
I1 Cu1 I2 108.436(12) . 2_657 ?
I2 Cu1 I2 116.893(13) . 2_657 ?
S1 Cu1 Cu2 147.13(2) . . ?
Cu1 Cu1 Cu2 63.650(12) 2_657 . ?
I1 Cu1 Cu2 59.625(10) . . ?
I2 Cu1 Cu2 59.898(10) . . ?
I2 Cu1 Cu2 110.975(13) 2_657 . ?
S1 Cu1 Cu2 146.23(2) . 2_657 ?
Cu1 Cu1 Cu2 60.050(11) 2_657 2_657 ?
I1 Cu1 Cu2 59.132(10) . 2_657 ?
I2 Cu1 Cu2 109.071(13) . 2_657 ?
I2 Cu1 Cu2 58.398(10) 2_657 2_657 ?
Cu2 Cu1 Cu2 60.320(14) . 2_657 ?
S2 Cu2 I1 104.57(2) 6_566 . ?
S2 Cu2 I2 109.60(2) 6_566 . ?
I1 Cu2 I2 112.586(13) . . ?
S2 Cu2 I1 108.52(2) 6_566 2_657 ?
I1 Cu2 I1 113.651(12) . 2_657 ?
I2 Cu2 I1 107.793(12) . 2_657 ?
S2 Cu2 Cu1 145.03(2) 6_566 . ?
I1 Cu2 Cu1 59.329(10) . . ?
I2 Cu2 Cu1 59.312(10) . . ?
I1 Cu2 Cu1 106.442(13) 2_657 . ?
S2 Cu2 Cu2 140.846(17) 6_566 2_657 ?
I1 Cu2 Cu2 59.448(11) . 2_657 ?
I2 Cu2 Cu2 109.553(7) . 2_657 ?
I1 Cu2 Cu2 58.455(12) 2_657 2_657 ?
Cu1 Cu2 Cu2 61.497(10) . 2_657 ?
S2 Cu2 Cu1 150.80(2) 6_566 2_657 ?
I1 Cu2 Cu1 104.623(12) . 2_657 ?
I2 Cu2 Cu1 58.893(10) . 2_657 ?
I1 Cu2 Cu1 57.872(10) 2_657 2_657 ?
Cu1 Cu2 Cu1 56.300(15) . 2_657 ?
Cu2 Cu2 Cu1 58.182(11) 2_657 2_657 ?
Cu1 I1 Cu2 61.046(11) . . ?
Cu1 I1 Cu2 62.998(10) . 2_657 ?
Cu2 I1 Cu2 62.098(11) . 2_657 ?
Cu1 I2 Cu2 60.789(10) . . ?
Cu1 I2 Cu1 57.960(12) . 2_657 ?
Cu2 I2 Cu1 62.708(10) . 2_657 ?
C9 S1 C10 103.89(14) . . ?
C9 S1 Cu1 104.57(9) . . ?
C10 S1 Cu1 102.25(10) . . ?
C15 S2 C16 100.79(13) . . ?
C15 S2 Cu2 104.41(9) . 6_565 ?
C16 S2 Cu2 105.97(9) . 6_565 ?
C22 O1 C1 117.7(2) . . ?
C3 O2 C2 118.8(2) . . ?
C11 O3 C12 111.2(2) . . ?
C13 O4 C14 116.1(2) . . ?
O1 C1 C2 107.3(3) . . ?
O2 C2 C1 105.7(3) . . ?
O2 C3 C4 124.3(3) . . ?
O2 C3 C8 114.4(2) . . ?
C4 C3 C8 121.3(3) . . ?
C5 C4 C3 119.2(3) . . ?
C4 C5 C6 121.0(3) . . ?
C5 C6 C7 119.8(3) . . ?
C8 C7 C6 120.4(3) . . ?
C7 C8 C3 118.3(3) . . ?
C7 C8 C9 124.1(2) . . ?
C3 C8 C9 117.6(2) . . ?
C8 C9 S1 116.63(18) . . ?
C11 C10 S1 115.1(2) . . ?
O3 C11 C10 108.9(2) . . ?
O3 C12 C13 110.4(2) . . ?
O4 C13 C12 113.7(2) . . ?
O4 C14 C15 109.3(2) . . ?
C14 C15 S2 112.03(19) . . ?
C17 C16 S2 111.25(18) . . ?
C18 C17 C22 118.6(3) . . ?
C18 C17 C16 121.7(2) . . ?
C22 C17 C16 119.6(2) . . ?
C19 C18 C17 121.0(3) . . ?
C18 C19 C20 119.3(3) . . ?
C21 C20 C19 121.4(3) . . ?
C20 C21 C22 119.1(3) . . ?
O1 C22 C21 123.6(3) . . ?
O1 C22 C17 115.9(2) . . ?
C21 C22 C17 120.5(3) . . ?
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
Cu1 S1 2.2998(7) . ?
Cu1 Cu1 2.5964(6) 2_657 ?
Cu1 I1 2.6581(4) . ?
Cu1 I2 2.6642(4) . ?
Cu1 I2 2.6945(3) 2_657 ?
Cu1 Cu2 2.7041(4) . ?
Cu1 Cu2 2.7966(4) 2_657 ?
Cu2 S2 2.3164(7) 6_566 ?
Cu2 I1 2.6662(4) . ?
Cu2 I2 2.6803(4) . ?
Cu2 I1 2.6942(4) 2_657 ?
Cu2 Cu2 2.7648(6) 2_657 ?
Cu2 Cu1 2.7966(4) 2_657 ?
I1 Cu2 2.6942(4) 2_657 ?
I2 Cu1 2.6944(3) 2_657 ?
S1 C9 1.814(2) . ?
S1 C10 1.820(3) . ?
S2 C15 1.817(3) . ?
S2 C16 1.829(3) . ?
S2 Cu2 2.3164(7) 6_565 ?
O1 C22 1.363(4) . ?
O1 C1 1.430(3) . ?
O2 C3 1.372(4) . ?
O2 C2 1.421(3) . ?
O3 C11 1.415(4) . ?
O3 C12 1.422(3) . ?
O4 C13 1.418(4) . ?
O4 C14 1.420(4) . ?
C1 C2 1.493(5) . ?
C3 C4 1.393(4) . ?
C3 C8 1.395(4) . ?
C4 C5 1.369(5) . ?
C5 C6 1.372(5) . ?
C6 C7 1.402(4) . ?
C7 C8 1.383(4) . ?
C8 C9 1.510(4) . ?
C10 C11 1.506(4) . ?
C12 C13 1.485(4) . ?
C14 C15 1.512(4) . ?
C16 C17 1.498(4) . ?
C17 C18 1.389(4) . ?
C17 C22 1.393(4) . ?
C18 C19 1.373(5) . ?
C19 C20 1.379(6) . ?
C20 C21 1.370(5) . ?
C21 C22 1.390(4) . ?
