#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/41/2234104.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_2234104
loop_
_publ_author_name
'Aydın, Ömür'
'Çaylak Delibaş, Nagihan'
'Necefoğlu, Hacali'
'Hökelek, Tuncer'
_publ_section_title
;
 Tetrakis(μ-2-iodobenzoato-κ²O:O')bis[aquacopper(II)]
;
_journal_coeditor_code           BQ2345
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m409
_journal_page_last               m410
_journal_paper_doi               10.1107/S1600536812010367
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Cu2 (C7 H4 I O2)4 (H2 O)2]'
_chemical_formula_moiety         'C28 H20 Cu2 I4 O10'
_chemical_formula_sum            'C28 H20 Cu2 I4 O10'
_chemical_formula_weight         1151.14
_chemical_name_systematic
;
Tetrakis(μ-2-iodobenzoato-κ²O:O')bis[aquacopper(II)]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                83.167(3)
_cell_angle_beta                 72.779(2)
_cell_angle_gamma                77.227(2)
_cell_formula_units_Z            1
_cell_length_a                   7.3563(2)
_cell_length_b                   10.7448(3)
_cell_length_c                   10.9066(3)
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      2.68
_cell_volume                     801.73(4)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material
'WinGX (Farrugia, 1999) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD area-detector'
_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  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0211
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14335
_diffrn_reflns_theta_full        28.39
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    5.231
_exptl_absorpt_correction_T_max  0.285
_exptl_absorpt_correction_T_min  0.150
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.384
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             538
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.658
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         3987
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0202
_refine_ls_R_factor_gt           0.0186
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0134P)²+0.9745P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0442
_refine_ls_wR_factor_ref         0.0448
_reflns_number_gt                3818
_reflns_number_total             3987
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bq2345.cif
_cod_data_source_block           I
_cod_database_code               2234104
_cod_database_fobs_code          2234104
loop_
_symmetry_equiv_pos_as_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_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
I I1 0.36263(2) 0.882863(16) 0.200310(15) 0.01953(5) Uani d . 1 1
I I2 -0.20180(2) 0.701971(15) 0.777993(14) 0.01579(5) Uani d . 1 1
Cu Cu1 0.65575(4) 0.46820(2) 0.53900(2) 0.00769(6) Uani d . 1 1
O O1 0.6886(2) 0.64727(16) 0.49086(16) 0.0152(3) Uani d . 1 1
O O2 0.4156(2) 0.70018(16) 0.43065(16) 0.0153(3) Uani d . 1 1
O O3 0.4755(2) 0.52102(17) 0.70398(15) 0.0151(3) Uani d . 1 1
O O4 0.7945(2) 0.43067(18) 0.35988(15) 0.0171(4) Uani d . 1 1
O O5 0.9024(2) 0.41164(17) 0.61507(15) 0.0137(3) Uani d D 1 1
H H51 1.010(3) 0.375(3) 0.573(3) 0.031(9) Uiso d D 1 1
H H52 0.920(6) 0.462(3) 0.660(3) 0.050(12) Uiso d D 1 1
C C1 0.5690(3) 0.7241(2) 0.4403(2) 0.0111(4) Uani d . 1 1
C C2 0.6219(3) 0.8508(2) 0.3878(2) 0.0118(4) Uani d . 1 1
C C3 0.5596(3) 0.9249(2) 0.2873(2) 0.0137(4) Uani d . 1 1
C C4 0.6304(4) 1.0353(2) 0.2372(3) 0.0204(5) Uani d . 1 1
H H4 0.5932 1.0828 0.1663 0.024 Uiso calc R 1 1
C C5 0.7553(4) 1.0769(3) 0.2899(3) 0.0247(6) Uani d . 1 1
H H5 0.8022 1.1529 0.2558 0.030 Uiso calc R 1 1
C C6 0.8112(4) 1.0070(2) 0.3925(3) 0.0222(5) Uani d . 1 1
H H6 0.8927 1.0367 0.4310 0.027 Uiso calc R 1 1
C C7 0.7483(3) 0.8947(2) 0.4384(2) 0.0162(5) Uani d . 1 1
H H7 0.7918 0.8456 0.5063 0.019 Uiso calc R 1 1
C C8 0.2958(3) 0.5622(2) 0.7233(2) 0.0102(4) Uani d . 1 1
C C9 0.1865(3) 0.6078(2) 0.8544(2) 0.0095(4) Uani d . 1 1
C C10 -0.0093(3) 0.6684(2) 0.8928(2) 0.0115(4) Uani d . 1 1
C C11 -0.0913(3) 0.7150(2) 1.0144(2) 0.0170(5) Uani d . 1 1
H H11 -0.2233 0.7576 1.0386 0.020 Uiso calc R 1 1
C C12 0.0184(4) 0.6997(3) 1.1009(2) 0.0184(5) Uani d . 1 1
H H12 -0.0385 0.7317 1.1841 0.022 Uiso calc R 1 1
C C13 0.2108(4) 0.6377(2) 1.0661(2) 0.0160(5) Uani d . 1 1
H H13 0.2860 0.6261 1.1255 0.019 Uiso calc R 1 1
C C14 0.2927(3) 0.5930(2) 0.9441(2) 0.0124(4) Uani d . 1 1
H H14 0.4251 0.5510 0.9206 0.015 Uiso calc R 1 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'
O O 0.0106 0.0060 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 Cu1 Cu1 . 2_666 86.36(5)
O1 Cu1 O5 . . 95.68(7)
O2 Cu1 Cu1 2_666 2_666 82.79(5)
O2 Cu1 O1 2_666 . 168.98(7)
O2 Cu1 O4 2_666 . 90.09(8)
O2 Cu1 O5 2_666 . 95.26(7)
O3 Cu1 Cu1 . 2_666 83.11(5)
O3 Cu1 O1 . . 89.93(7)
O3 Cu1 O2 . 2_666 90.68(7)
O3 Cu1 O4 . . 168.90(7)
O3 Cu1 O5 . . 93.88(6)
O4 Cu1 Cu1 . 2_666 86.00(5)
O4 Cu1 O1 . . 87.22(8)
O4 Cu1 O5 . . 97.08(7)
O5 Cu1 Cu1 . 2_666 176.38(5)
C1 O1 Cu1 . . 119.86(14)
C1 O2 Cu1 . 2_666 125.63(15)
C8 O3 Cu1 . . 124.96(14)
C8 O4 Cu1 2_666 . 121.09(15)
Cu1 O5 H51 . . 123(2)
Cu1 O5 H52 . . 117(3)
H51 O5 H52 . . 108(4)
O1 C1 C2 . . 116.23(19)
O2 C1 O1 . . 124.6(2)
O2 C1 C2 . . 119.2(2)
C3 C2 C1 . . 124.2(2)
C7 C2 C1 . . 117.6(2)
C7 C2 C3 . . 118.1(2)
C2 C3 I1 . . 125.24(17)
C4 C3 I1 . . 114.73(17)
C4 C3 C2 . . 120.0(2)
C3 C4 H4 . . 119.8
C5 C4 C3 . . 120.5(2)
C5 C4 H4 . . 119.8
C4 C5 H5 . . 120.1
C6 C5 C4 . . 119.8(2)
C6 C5 H5 . . 120.1
C5 C6 H6 . . 120.1
C7 C6 C5 . . 119.7(2)
C7 C6 H6 . . 120.1
C2 C7 H7 . . 119.1
C6 C7 C2 . . 121.7(2)
C6 C7 H7 . . 119.1
O3 C8 O4 . 2_666 124.6(2)
O3 C8 C9 . . 116.33(18)
O4 C8 C9 2_666 . 119.06(19)
C10 C9 C8 . . 125.79(19)
C14 C9 C8 . . 116.50(19)
C14 C9 C10 . . 117.66(19)
C9 C10 I2 . . 125.52(16)
C11 C10 I2 . . 113.88(16)
C11 C10 C9 . . 120.6(2)
C10 C11 H11 . . 119.8
C12 C11 C10 . . 120.3(2)
C12 C11 H11 . . 119.8
C11 C12 H12 . . 120.0
C13 C12 C11 . . 120.1(2)
C13 C12 H12 . . 120.0
C12 C13 H13 . . 120.3
C14 C13 C12 . . 119.4(2)
C14 C13 H13 . . 120.3
C9 C14 H14 . . 119.0
C13 C14 C9 . . 121.9(2)
C13 C14 H14 . . 119.0
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
I1 C3 . 2.100(2) ?
I2 C10 . 2.102(2) ?
Cu1 Cu1 2_666 2.6009(5) ?
Cu1 O1 . 1.9814(16) yes
Cu1 O2 2_666 1.9577(16) yes
Cu1 O3 . 1.9533(16) yes
Cu1 O4 . 1.9610(16) yes
Cu1 O5 . 2.1525(16) ?
O1 C1 . 1.272(3) ?
O2 Cu1 2_666 1.9577(16) ?
O2 C1 . 1.247(3) ?
O3 C8 . 1.260(3) ?
O4 C8 2_666 1.260(3) ?
O5 H51 . 0.828(18) ?
O5 H52 . 0.828(19) ?
C2 C1 . 1.499(3) ?
C2 C7 . 1.397(3) ?
C3 C2 . 1.404(3) ?
C3 C4 . 1.389(3) ?
C4 H4 . 0.9500 ?
C5 C4 . 1.388(4) ?
C5 H5 . 0.9500 ?
C6 C5 . 1.386(4) ?
C6 H6 . 0.9500 ?
C7 C6 . 1.374(3) ?
C7 H7 . 0.9500 ?
C8 O4 2_666 1.260(3) ?
C8 C9 . 1.498(3) ?
C9 C10 . 1.403(3) ?
C9 C14 . 1.397(3) ?
C10 C11 . 1.388(3) ?
C11 C12 . 1.387(3) ?
C11 H11 . 0.9500 ?
C12 C13 . 1.384(3) ?
C12 H12 . 0.9500 ?
C13 C14 . 1.384(3) ?
C13 H13 . 0.9500 ?
C14 H14 . 0.9500 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O5 H51 O1 2_766 0.83(3) 2.09(3) 2.839(2) 152(3) yes
O5 H52 O4 2_766 0.83(3) 2.56(4) 3.171(2) 132(3) yes
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_4
_geom_torsion
Cu1 Cu1 O1 C1 2_666 . -2.22(16)
O2 Cu1 O1 C1 2_666 . 7.9(5)
O3 Cu1 O1 C1 . . -85.32(17)
O4 Cu1 O1 C1 . . 83.95(17)
O5 Cu1 O1 C1 . . -179.21(16)
Cu1 Cu1 O3 C8 2_666 . 0.27(18)
O1 Cu1 O3 C8 . . 86.62(19)
O2 Cu1 O3 C8 2_666 . -82.38(19)
O4 Cu1 O3 C8 . . 11.6(5)
O5 Cu1 O3 C8 . . -177.70(18)
Cu1 Cu1 O4 C8 2_666 2_666 -4.82(18)
O1 Cu1 O4 C8 . 2_666 -91.37(18)
O2 Cu1 O4 C8 2_666 2_666 77.94(18)
O3 Cu1 O4 C8 . 2_666 -16.0(5)
O5 Cu1 O4 C8 . 2_666 173.25(18)
Cu1 O1 C1 O2 . . 8.5(3)
Cu1 O1 C1 C2 . . -170.57(14)
Cu1 O2 C1 O1 2_666 . -11.8(3)
Cu1 O2 C1 C2 2_666 . 167.28(15)
Cu1 O3 C8 O4 . 2_666 3.5(3)
Cu1 O3 C8 C9 . . -175.06(14)
C3 C2 C1 O1 . . 153.2(2)
C3 C2 C1 O2 . . -25.9(3)
C7 C2 C1 O1 . . -23.8(3)
C7 C2 C1 O2 . . 157.1(2)
C1 C2 C7 C6 . . 177.3(2)
C3 C2 C7 C6 . . 0.1(4)
I1 C3 C2 C1 . . 5.4(3)
I1 C3 C2 C7 . . -177.62(17)
C4 C3 C2 C1 . . -174.1(2)
C4 C3 C2 C7 . . 2.9(3)
I1 C3 C4 C5 . . 177.2(2)
C2 C3 C4 C5 . . -3.3(4)
C6 C5 C4 C3 . . 0.6(4)
C7 C6 C5 C4 . . 2.3(4)
C2 C7 C6 C5 . . -2.7(4)
O3 C8 C9 C10 . . 173.4(2)
O3 C8 C9 C14 . . -3.7(3)
O4 C8 C9 C10 2_666 . -5.2(3)
O4 C8 C9 C14 2_666 . 177.7(2)
C8 C9 C10 C11 . . -175.2(2)
C8 C9 C10 I2 . . 3.2(3)
C14 C9 C10 I2 . . -179.69(16)
C14 C9 C10 C11 . . 1.9(3)
C8 C9 C14 C13 . . 176.4(2)
C10 C9 C14 C13 . . -1.0(3)
I2 C10 C11 C12 . . 179.93(19)
C9 C10 C11 C12 . . -1.5(4)
C10 C11 C12 C13 . . 0.1(4)
C11 C12 C13 C14 . . 0.8(4)
C12 C13 C14 C9 . . -0.4(4)
