#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/22/4312256.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_4312256
loop_
_publ_author_name
'Guanghua Li'
'Zhan Shi'
'Xiaomin Liu'
'Zhimin Dai'
'Lu Gao'
'Shouhua Feng'
_publ_contact_author
;
      Feng,Shouhua
      College of Chemistry
      Jilin University
      Changchun, 130012
      P. R. China
;
_publ_section_title
;
 A New Inorganic-Organic Hybrid Copper Iodate with Potentially Large Void
 Volume
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8224
_journal_page_last               8226
_journal_paper_doi               10.1021/ic049098z
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C20 H25.50 Cl1.50 Cu2 I3.38 N4 O13.50'
_chemical_formula_sum            'C20 H25.5 Cl1.5 Cu2 I3.38 N4 O13.5'
_chemical_formula_weight         1146.49
_chemical_melting_point          ?
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           108
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4 -2c'
_symmetry_space_group_name_H-M   'I 4 c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.6755(4)
_cell_length_b                   29.6755(4)
_cell_length_c                   6.98570(10)
_cell_measurement_temperature    293(2)
_cell_volume                     6151.85(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0208
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            13353
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.75
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.971
_exptl_absorpt_correction_T_max  0.2983
_exptl_absorpt_correction_T_min  0.1918
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'brown green'
_exptl_crystal_density_diffrn    2.476
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       pillar
_exptl_crystal_F_000             4351
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.123
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.08(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         2239
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0272
_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)+(0.0555P)²+15.0190P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0786
_reflns_number_gt                2151
_reflns_number_total             2239
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049098zsi20041026_104242.cif
_cod_data_source_block           sad
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to '/home/adriana/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_formula_sum        'C20 H25.50 Cl1.50 Cu2 I3.38 N4 O13.50'
_cod_database_code               4312256
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x, -y, z+1/2'
'-x, y, z+1/2'
'-y, -x, z+1/2'
'y, x, z+1/2'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -y+1/2, z+1'
'-x+1/2, y+1/2, z+1'
'-y+1/2, -x+1/2, z+1'
'y+1/2, x+1/2, z+1'
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 0.61885(3) 0.27198(3) 1.05794(16) 0.0313(3) Uani 1 1 d . . .
I1 I 0.719464(15) 0.335656(14) 1.02885(9) 0.02752(17) Uani 1 1 d . . .
I2 I 0.700073(16) 0.200073(16) 0.97249(12) 0.0284(2) Uani 1 2 d S . .
I3 I 0.5000 0.5000 1.028(2) 0.089(2) Uani 0.30 4 d SP . .
I3' I 0.5000 0.5000 0.6870(18) 0.079(2) Uani 0.30 4 d SP . .
I3" I 0.5000 0.5000 0.861(4) 0.133(7) Uani 0.15 4 d SPU . .
Cl1 Cl 0.5849(3) 0.0849(3) 1.4908(12) 0.0447(18) Uani 1 2 d S . .
Cl1' Cl 0.5817(5) 0.0817(5) 1.5583(16) 0.032(3) Uani 0.50 2 d SP . .
O1 O 0.66477(19) 0.3186(2) 1.1182(10) 0.0394(14) Uani 1 1 d . . .
O2 O 0.65710(18) 0.22064(19) 1.1380(8) 0.0326(13) Uani 1 1 d . . .
O3 O 0.7434(2) 0.3473(2) 1.2618(9) 0.0460(17) Uani 1 1 d . . .
O4 O 0.7082(2) 0.39109(19) 0.9444(11) 0.0473(17) Uani 1 1 d . . .
O5 O 0.74220(18) 0.24220(18) 1.0113(17) 0.048(2) Uani 1 2 d S . .
O1W O 0.5449(3) 0.0449(3) 1.199(2) 0.072(3) Uani 1 2 d SU . .
O2W O 0.6790(3) 0.1790(3) 1.508(2) 0.099(4) Uani 1 2 d S . .
O3W O 0.6426(5) 0.1426(5) 1.493(3) 0.055(5) Uani 0.50 2 d SP . .
O4W O 0.62717(19) 0.12717(19) 1.8218(12) 0.0269(19) Uani 1 2 d S . .
O5W O 0.6085(5) 0.1085(5) 1.807(2) 0.086(4) Uani 1 2 d SU . .
N1 N 0.5619(2) 0.2357(2) 1.0803(9) 0.0308(16) Uani 1 1 d . . .
N2 N 0.5752(2) 0.3189(2) 0.9748(11) 0.0361(17) Uani 1 1 d . . .
C1 C 0.5593(3) 0.1928(3) 1.1360(15) 0.040(2) Uani 1 1 d . . .
H1 H 0.5857 0.1768 1.1584 0.080 Uiso 1 1 calc . . .
C2 C 0.5173(3) 0.1711(3) 1.1617(16) 0.049(3) Uani 1 1 d . . .
H2 H 0.5153 0.1409 1.1966 0.080 Uiso 1 1 calc . . .
C3 C 0.4798(3) 0.1967(4) 1.1328(17) 0.055(3) Uani 1 1 d . . .
H3 H 0.4516 0.1837 1.1521 0.080 Uiso 1 1 calc . . .
C4 C 0.4818(3) 0.2399(3) 1.0777(13) 0.039(2) Uani 1 1 d . . .
H4 H 0.4556 0.2567 1.0599 0.080 Uiso 1 1 calc . . .
C5 C 0.5240(2) 0.2588(3) 1.0480(13) 0.0340(18) Uani 1 1 d . . .
C6 C 0.5308(2) 0.3061(3) 0.9836(13) 0.0317(19) Uani 1 1 d . . .
C7 C 0.4969(3) 0.3360(3) 0.9324(15) 0.044(2) Uani 1 1 d . . .
H7 H 0.4668 0.3274 0.9410 0.080 Uiso 1 1 calc . . .
C8 C 0.5077(4) 0.3770(4) 0.8712(19) 0.064(3) Uani 1 1 d . . .
H8 H 0.4849 0.3971 0.8391 0.080 Uiso 1 1 calc . . .
C9 C 0.5530(4) 0.3904(3) 0.854(2) 0.062(3) Uani 1 1 d . . .
H9 H 0.5607 0.4187 0.8064 0.080 Uiso 1 1 calc . . .
C10 C 0.5859(3) 0.3598(3) 0.9109(16) 0.048(3) Uani 1 1 d . . .
H10 H 0.6161 0.3681 0.9041 0.080 Uiso 1 1 calc . . .
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'
O O 0.0106 0.0060 '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'
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
O2 Cu1 O1 94.7(2) . . ?
O2 Cu1 N2 174.0(3) . . ?
O1 Cu1 N2 91.2(3) . . ?
O2 Cu1 N1 92.8(2) . . ?
O1 Cu1 N1 158.9(3) . . ?
N2 Cu1 N1 81.3(3) . . ?
O2 Cu1 O3 81.6(2) . 7_664 ?
O1 Cu1 O3 91.7(3) . 7_664 ?
N2 Cu1 O3 99.1(3) . 7_664 ?
N1 Cu1 O3 108.9(3) . 7_664 ?
O4 I1 O3 101.3(3) . . ?
O4 I1 O1 101.8(3) . . ?
O3 I1 O1 95.5(3) . . ?
O5 I2 O2 99.1(3) . . ?
O5 I2 O2 99.1(3) . 16_544 ?
O2 I2 O2 93.8(4) . 16_544 ?
I3' I3 I3" 180.00(3) 5_565 . ?
I3' I3 I3" 0.000(8) 5_565 5_565 ?
I3" I3 I3" 180.00(4) . 5_565 ?
I3' I3 I3' 180.000(18) 5_565 . ?
I3" I3 I3' 0.000(14) . . ?
I3" I3 I3' 180.000(14) 5_565 . ?
I3 I3' I3" 180.00(4) 5_564 . ?
I3 I3' I3" 0.000(9) 5_564 5_564 ?
I3" I3' I3" 180.00(4) . 5_564 ?
I3 I3' I3 180.00(2) 5_564 . ?
I3" I3' I3 0.000(14) . . ?
I3" I3' I3 180.000(13) 5_564 . ?
I3 I3" I3' 180.000(19) . . ?
I3 I3" I3' 0.000(6) . 5_565 ?
I3' I3" I3' 180.000(15) . 5_565 ?
I3 I3" I3 180.00(2) . 5_564 ?
I3' I3" I3 0.000(4) . 5_564 ?
I3' I3" I3 180.000(11) 5_565 5_564 ?
I1 O1 Cu1 137.4(3) . . ?
I2 O2 Cu1 118.6(3) . . ?
I1 O3 Cu1 143.1(3) . 7_665 ?
O4W O5W Cl1' 130(2) . . ?
C1 N1 C5 119.3(7) . . ?
C1 N1 Cu1 125.6(6) . . ?
C5 N1 Cu1 114.9(5) . . ?
C10 N2 C6 119.7(7) . . ?
C10 N2 Cu1 125.5(6) . . ?
C6 N2 Cu1 114.7(6) . . ?
N1 C1 C2 121.5(9) . . ?
N1 C1 H1 119.2 . . ?
C2 C1 H1 119.2 . . ?
C3 C2 C1 116.5(9) . . ?
C3 C2 H2 121.8 . . ?
C1 C2 H2 121.8 . . ?
C4 C3 C2 122.8(9) . . ?
C4 C3 H3 118.6 . . ?
C2 C3 H3 118.6 . . ?
C3 C4 C5 118.0(8) . . ?
C3 C4 H4 121.0 . . ?
C5 C4 H4 121.0 . . ?
N1 C5 C4 121.9(8) . . ?
N1 C5 C6 114.8(7) . . ?
C4 C5 C6 123.3(7) . . ?
N2 C6 C7 120.4(8) . . ?
N2 C6 C5 113.9(7) . . ?
C7 C6 C5 125.6(7) . . ?
C8 C7 C6 119.6(9) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
C7 C8 C9 121.1(9) . . ?
C7 C8 H8 119.4 . . ?
C9 C8 H8 119.4 . . ?
C10 C9 C8 117.4(9) . . ?
C10 C9 H9 121.3 . . ?
C8 C9 H9 121.3 . . ?
N2 C10 C9 121.6(9) . . ?
N2 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
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 O2 1.980(5) . ?
Cu1 O1 1.986(6) . ?
Cu1 N2 1.988(7) . ?
Cu1 N1 2.010(6) . ?
Cu1 O3 2.344(6) 7_664 ?
I1 O4 1.780(6) . ?
I1 O3 1.809(6) . ?
I1 O1 1.811(6) . ?
I2 O5 1.789(8) . ?
I2 O2 1.826(6) . ?
I2 O2 1.826(6) 16_544 ?
I3 I3' 1.108(12) 5_565 ?
I3 I3" 1.17(3) . ?
I3 I3" 2.32(3) 5_565 ?
I3 I3' 2.385(12) . ?
I3' I3 1.108(12) 5_564 ?
I3' I3" 1.22(3) . ?
I3' I3" 2.28(3) 5_564 ?
I3" I3' 2.28(3) 5_565 ?
I3" I3 2.32(3) 5_564 ?
Cl1' O5W 2.07(2) . ?
O3 Cu1 2.344(6) 7_665 ?
O2W O3W 1.53(3) . ?
O4W O5W 0.788(17) . ?
N1 C1 1.335(11) . ?
N1 C5 1.335(10) . ?
N2 C10 1.332(12) . ?
N2 C6 1.373(10) . ?
C1 C2 1.414(14) . ?
C1 H1 0.9300 . ?
C2 C3 1.363(16) . ?
C2 H2 0.9300 . ?
C3 C4 1.338(15) . ?
C3 H3 0.9300 . ?
C4 C5 1.388(11) . ?
C4 H4 0.9300 . ?
C5 C6 1.488(11) . ?
C6 C7 1.389(12) . ?
C7 C8 1.328(16) . ?
C7 H7 0.9300 . ?
C8 C9 1.409(17) . ?
C8 H8 0.9300 . ?
C9 C10 1.392(15) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
