#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/72/2007284.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_2007284
loop_
_publ_author_name
'Aliya K. Nurtaeva'
'Elizabeth M. Holt'
_publ_section_title
;
 (15-Crown-5)caesium Dicopper(I) Triiodide, (15-Crown-5)potassium
 Dicopper(I) Triiodide and (15-Crown-5)rubidium Dicopper(I) Triiodide
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              594
_journal_page_last               597
_journal_paper_doi               10.1107/S0108270197017502
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         '[Cs(C10 H20 O5)][Cu2 I3]'
_chemical_formula_sum            'C10 H20 Cs Cu2 I3 O5'
_chemical_formula_weight         861.0
_chemical_name_systematic        '  Cesium 15-crown-5  Dicopper(I) Triiodide'
_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'
_cell_angle_alpha                90.0
_cell_angle_beta                 120.36(7)
_cell_angle_gamma                90.0
_cell_formula_units_Z            8
_cell_length_a                   25.19(3)
_cell_length_b                   11.177(12)
_cell_length_c                   16.86(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    301
_cell_measurement_theta_max      11.491
_cell_measurement_theta_min      2.855
_cell_volume                     4096(10)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1991)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    'XP (Siemens, 1990)'
_computing_structure_refinement  SHELXS86
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device_type  'Syntex P4 four-circle diffractometer'
_diffrn_measurement_method       θ/2θ
_diffrn_radiation_monochromator  'highly oriented graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            6938
_diffrn_reflns_theta_max         30.0
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0.0001
_diffrn_standards_interval_time  '97 reflections'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.380
_exptl_absorpt_correction_T_max  0.43
_exptl_absorpt_correction_T_min  0.11
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(Sheldrick, 1990)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.798
_exptl_crystal_density_method    none
_exptl_crystal_description       rhombohedron
_exptl_crystal_F_000             3136
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.95
_refine_diff_density_min         -1.19
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.36
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         5956
_refine_ls_R_factor_gt           0.0595
_refine_ls_shift/esd_mean        0.055
_refine_ls_shift/su_max          0.068
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(F)+ 0.0008F²]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_ref         0.0685
_reflns_number_gt                1978
_reflns_number_total             5956
_reflns_threshold_expression     F>6.0σ(F)
_cod_data_source_file            sx1047.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C10 H20 Cs1 Cu2 I3 O5'
_cod_database_code               2007284
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y,1/2-z
x,-y,1/2+z
1/2+x,1/2+y,z
1/2-x,1/2-y,-z
1/2-x,1/2+y,1/2-z
1/2+x,1/2-y,1/2+z
loop_
_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_calc_attached_atom
I(1) .45680(10) -.24000(10) .09800(10) .0470(10) Uani d .
I(2) .59030(10) .02770(10) .25440(10) .0470(10) Uani d .
I(3) .42850(10) .11910(10) .00700(10) .0530(10) Uani d .
Cu(1) .4622(2) -.0231(3) .1583(3) .091(2) Uani d .
Cu(2) .5129(2) -.0641(3) .0711(3) .098(3) Uani d .
Cs(1) .37420(10) -.30820(10) .22590(10) .0600(10) Uani d .
O(1) .2374(8) -.342(2) .0994(14) .089(10) Uani d .
C(2) .2014(12) -.365(4) .144(3) .12(2) Uani d .
H(2A) .1591 -.3441 .1037 .080 Uiso calc R
H(2B) .2035 -.4484 .1592 .080 Uiso calc R
C(3) .226(2) -.300(4) .216(4) .15(3) Uani d .
H(3A) .1976 -.3025 .2388 .080 Uiso calc R
H(3B) .2270 -.2192 .1988 .080 Uiso calc R
O(4) .2804(11) -.327(2) .287(2) .107(13) Uani d .
C(5) .286(2) -.419(4) .343(3) .13(3) Uani d .
H(5A) .2690 -.3948 .3808 .080 Uiso calc R
H(5B) .2619 -.4857 .3066 .080 Uiso calc R
C(6) .344(2) -.454(4) .398(2) .13(3) Uani d .
H(6A) .3458 -.5057 .4458 .080 Uiso calc R
H(6B) .3695 -.3864 .4275 .080 Uiso calc R
O(7) .3654(10) -.518(2) .3473(13) .096(11) Uani d .
C(8) .4271(12) -.542(3) .390(2) .11(2) Uani d .
H(8A) .4500 -.4687 .4006 .080 Uiso calc R
H(8B) .4408 -.5809 .4473 .080 Uiso calc R
C(9) .4359(12) -.624(3) .323(2) .084(15) Uani d .
H(9A) .4062 -.6874 .3012 .080 Uiso calc R
H(9B) .4764 -.6584 .3542 .080 Uiso calc R
O(10) .4280(8) -.552(2) .250(2) .088(11) Uani d .
C(11) .410(2) -.623(3) .171(3) .11(2) Uani d .
H(11A) .4247 -.5869 .1343 .080 Uiso calc R
H(11B) .4281 -.7002 .1898 .080 Uiso calc R
C(12) .3437(15) -.637(2) .116(2) .09(2) Uani d .
H(12A) .3288 -.6782 .1510 .080 Uiso calc R
H(12B) .3344 -.6858 .0636 .080 Uiso calc R
O(13) .3129(9) -.527(2) .0855(12) .078(10) Uani d .
C(14) .2507(12) -.533(3) .045(2) .084(15) Uani d .
H(14A) .2347 -.5802 -.0097 .080 Uiso calc R
H(14B) .2400 -.5720 .0859 .080 Uiso calc R
C(15) .2237(14) -.420(4) .022(2) .11(2) Uani d .
H(15B) .1799 -.4309 -.0131 .080 Uiso calc R
H(15A) .2359 -.3802 -.0166 .080 Uiso calc R
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.002 0.002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H 0.0 0.0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs -0.644 2.119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu 0.263 1.266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I -0.726 1.812 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O 0.008 0.006 '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_3
_geom_angle
_geom_angle_publ_flag
Cu(1) I(1) Cu(2) . 55.8(2) no
Cu(1) I(2) Cu(2) . 50.2(2) no
Cu(1) I(2) Cu(1) 3_655 60.1(2) no
Cu(2) I(2) Cu(1) 3_655 106.2(2) no
Cu(1) I(3) Cu(2) . 52.4(2) no
Cu(1) I(3) Cu(2) 2_655 111.0(2) no
Cu(2) I(3) Cu(2) 2_655 58.6(2) no
I(1) Cu(1) I(2) . 103.1(2) no
I(1) Cu(1) I(3) . 104.2(2) no
I(2) Cu(1) I(3) . 98.2(2) no
I(1) Cu(1) I(2) 3_655 120.3(2) no
I(2) Cu(1) I(2) 3_655 114.0(2) no
I(3) Cu(1) I(2) 3_655 114.2(2) no
I(1) Cu(2) I(2) . 102.5(2) no
I(1) Cu(2) I(3) . 104.6(2) no
I(2) Cu(2) I(3) . 97.2(2) no
I(1) Cu(2) I(3) 2_655 115.1(2) no
I(2) Cu(2) I(3) 2_655 113.1(2) no
I(3) Cu(2) I(3) 2_655 121.4(2) no
C(2) O(1) C(15) . 115(2) no
O(1) C(2) C(3) . 105(4) no
C(2) C(3) O(4) . 121(4) no
C(3) O(4) C(5) . 120(4) no
O(4) C(5) C(6) . 114(4) no
C(5) C(6) O(7) . 110(3) no
C(6) O(7) C(8) . 118(2) no
O(7) C(8) C(9) . 106(2) no
C(8) C(9) O(10) . 106(2) no
C(9) O(10) C(11) . 110(2) no
O(10) C(11) C(12) . 113(4) no
C(11) C(12) O(13) . 112(2) no
C(12) O(13) C(14) . 115(2) no
O(13) C(14) C(15) . 112(3) no
O(1) C(15) C(14) . 116(2) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
I(1) Cu(1) . . 2.607(6) yes
I(1) Cu(2) . . 2.590(6) yes
I(2) Cu(1) . . 2.843(6) yes
I(2) Cu(2) . . 2.882(6) yes
I(2) Cu(1) . 3_655 2.491(7) yes
I(3) Cu(1) . . 2.751(6) yes
I(3) Cu(2) . . 2.750(6) yes
I(3) Cu(2) . 2_655 2.502(7) yes
Cu(1) Cu(2) . . 2.430(9) yes
Cu(1) Cu(1) . 3_655 2.690(8) yes
Cu(2) Cu(2) . 2_655 2.579(10) yes
Cs(1) O(1) . . 3.02(2) no
Cs(1) O(4) . . 3.03(3) no
Cs(1) O(7) . . 3.19(2) no
Cs(1) O(10) . . 2.98(2) no
Cs(1) O(13) . . 3.21(2) no
Cs(1) I(1) . 3_655 3.838(6) yes
Cs(1) I(2) . 3_655 3.834(6) yes
Cs(1) I(1) . . 3.755(6) yes
O(1) C(2) . . 1.46(5) no
O(1) C(15) . . 1.46(4) no
C(2) C(3) . . 1.28(6) no
C(3) O(4) . . 1.32(4) no
O(4) C(5) . . 1.36(6) no
C(5) C(6) . . 1.33(6) no
C(6) O(7) . . 1.42(6) no
O(7) C(8) . . 1.37(4) no
C(8) C(9) . . 1.55(5) no
C(9) O(10) . . 1.40(4) no
O(10) C(11) . . 1.42(5) no
C(11) C(12) . . 1.44(5) no
C(12) O(13) . . 1.40(3) no
O(13) C(14) . . 1.36(4) no
C(14) C(15) . . 1.39(5) no
