#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2007285.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_2007285
loop_
_publ_author_name
'Nurtaeva, A. K.'
'Holt, E. M.'
_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_volume                  54
_journal_year                    1998
_chemical_formula_moiety         '[K(C10 H20 O5)][Cu2 I3]'
_chemical_formula_sum            'C10 H20 Cu2 I3 K O5'
_chemical_formula_weight         767.1
_chemical_name_systematic
'  Potassium 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                 119.75(2)
_cell_angle_gamma                90.0
_cell_formula_units_Z            8
_cell_length_a                   23.818(14)
_cell_length_b                   10.956(6)
_cell_length_c                   17.071(10)
_cell_measurement_reflns_used    43
_cell_measurement_temperature    298
_cell_measurement_theta_max      12.427
_cell_measurement_theta_min      5.242
_cell_volume                     3868(4)
_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'
_diffrn_measurement_method       \q/2\q
_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  0.081
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            6605
_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    7.206
_exptl_absorpt_correction_T_max  0.49
_exptl_absorpt_correction_T_min  0.24
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(Sheldrick, 1990)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.631
_exptl_crystal_density_method    none
_exptl_crystal_description       polyhedra
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.89
_refine_diff_density_min         -0.87
_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         5650
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(F) + 0.0008F^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_ref         0.0694
_reflns_number_gt                2175
_reflns_number_total             5650
_reflns_threshold_expression     F>5.5\s(F)
_[local]_cod_data_source_file    sx1047.cif
_[local]_cod_data_source_block   II
_[local]_cod_cif_authors_sg_H-M  'C 2/c'
_[local]_cod_chemical_formula_sum_orig 'C10 H20 Cu2 I3 K1 O5'
_cod_database_code               2007285
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) 0.46100(10) -0.26100(10) 0.10090(10) 0.0430(10) Uani d .
I(2) 0.59840(10) -0.00100(10) 0.25700(10) 0.0460(10) Uani d .
I(3) 0.42670(10) 0.10670(10) 0.01540(10) 0.0470(10) Uani d .
Cu(1) 0.46290(10) -0.00395(3) 0.1612(2) 0.077(2) Uani d .
Cu(2) 0.5160(2) -0.0729(3) 0.0715(2) 0.097(2) Uani d .
K(1) 0.3815(2) -0.3435(4) 0.2192(3) 0.051(2) Uani d .
O(1) 0.2519(6) -0.3271(14) 0.1026(9) 0.070(7) Uani d .
C(2) 0.2137(10) -0.313(3) 0.142(2) 0.11(2) Uani d .
H(2A) 0.2062 -0.3919 0.1594 0.080 Uiso calc R
H(2B) 0.1728 -0.2787 0.0988 0.080 Uiso calc R
C(3) 0.2424(12) -0.248(3) 0.221(2) 0.107(15) Uani d .
H(3A) 0.2510 -0.1710 0.2031 0.080 Uiso calc R
H(3B) 0.2143 -0.2347 0.2457 0.080 Uiso calc R
O(4) 0.3030(8) -0.291(2) 0.2880(10) 0.086(9) Uani d .
C(5) 0.3003(13) -0.370(2) 0.349(2) 0.09(2) Uani d .
H(5A) 0.2677 -0.4287 0.3136 0.080 Uiso calc R
H(5B) 0.2875 -0.3279 0.3871 0.080 Uiso calc R
C(6) 0.3611(15) -0.434(2) 0.3985(15) 0.086(15) Uani d .
H(6A) 0.3950 -0.3751 0.4275 0.080 Uiso calc R
H(6B) 0.3604 -0.4852 0.4437 0.080 Uiso calc R
O(7) 0.3697(7) -0.5057(14) 0.3405(9) 0.072(7) Uani d .
C(8) 0.4288(12) -0.567(2) 0.3792(12) 0.091(12) Uani d .
H(8A) 0.4357 -0.6126 0.4312 0.080 Uiso calc R
H(8B) 0.4633 -0.5089 0.3970 0.080 Uiso calc R
C(9) 0.4280(10) -0.649(2) 0.3100(13) 0.066(11) Uani d .
H(9A) 0.4629 -0.7066 0.3340 0.080 Uiso calc R
H(9B) 0.3878 -0.6927 0.2831 0.080 Uiso calc R
O(10) 0.4303(6) -0.5736(12) 0.2477(9) 0.060(7) Uani d .
C(11) 0.4116(10) -0.634(2) 0.1656(14) 0.065(11) Uani d .
H(11A) 0.4308 -0.7132 0.1773 0.080 Uiso calc R
H(11B) 0.4277 -0.5876 0.1331 0.080 Uiso calc R
C(12) 0.3410(12) -0.645(2) 0.1085(15) 0.074(13) Uani d .
H(12A) 0.3291 -0.6923 0.0552 0.080 Uiso calc R
H(12B) 0.3233 -0.6826 0.1422 0.080 Uiso calc R
O(13) 0.3195(7) -0.5238(14) 0.0862(9) 0.071(7) Uani d .
C(14) 0.2514(12) -0.529(2) 0.045(2) 0.096(15) Uani d .
H(14A) 0.2402 -0.5608 0.0881 0.080 Uiso calc R
H(14B) 0.2323 -0.5776 -0.0083 0.080 Uiso calc R
C(15) 0.2295(11) -0.402(2) 0.0277(14) 0.086(12) Uani d .
H(15B) 0.2469 -0.3731 -0.0091 0.080 Uiso calc R
H(15A) 0.1833 -0.3951 -0.0077 0.080 Uiso calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
I(1) 0.0500(10) 0.0360(10) 0.0440(10) -0.0030(10) 0.0240(10) -0.0040(10)
I(2) 0.0450(10) 0.0480(10) 0.0460(10) -0.0070(10) 0.0240(10) -0.0020(10)
I(3) 0.0520(10) 0.0450(10) 0.0500(10) 0.0120(10) 0.0300(10) 0.0100(10)
Cu(1) 0.110(2) 0.063(2) 0.090(2) 0.004(2) 0.075(2) -0.0070(10)
Cu(2) 0.142(3) 0.069(2) 0.149(3) 0.020(2) 0.124(3) 0.023(2)
K(1) 0.045(2) 0.047(2) 0.057(2) -0.001(2) 0.023(2) 0.008(2)
O(1) 0.052(8) 0.076(10) 0.076(9) 0.008(8) 0.027(8) 0.000(8)
C(2) 0.042(13) 0.19(3) 0.09(2) 0.03(2) 0.020(10) 0.02(2)
C(3) 0.08(2) 0.13(3) 0.09(2) 0.06(2) 0.02(15) 0.000(2)
O(4) 0.090(12) 0.102(13) 0.076(10) -0.003(10) 0.049(10) -0.019(9)
C(5) 0.14(2) 0.08(2) 0.12(2) 0.01(2) 0.11(2) 0.00(2)
C(6) 0.16(2) 0.052(14) 0.060(13) -0.02(2) 0.07(2) -0.013(11)
O(7) 0.076(10) 0.078(11) 0.057(8) -0.009(9) 0.030(8) -0.001(8)
C(8) 0.09(2) 0.11(2) 0.033(10) -0.02(2) -0.002(11) 0.032(12)
C(9) 0.071(14) 0.064(14) 0.070(13) -0.012(11) 0.041(11) 0.007(12)
O(10) 0.051(8) 0.048(8) 0.086(9) 0.011(6) 0.038(7) 0.015(7)
C(11) 0.079(15) 0.053(12) 0.083(14) 0.019(11) 0.055(13) -0.006(11)
C(12) 0.11(2) 0.053(14) 0.081(14) -0.024(13) 0.058(14) -0.030(12)
O(13) 0.058(9) 0.072(11) 0.073(9) 0.004(8) 0.025(7) -0.009(8)
C(14) 0.10(2) 0.07(2) 0.10(2) -0.026(15) 0.04(2) -0.035(15)
C(15) 0.067(14) 0.10(2) 0.054(12) -0.001(14) -0.002(11) -0.001(14)
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'
K 0.179 0.250 '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) . 55.60(10) no
Cu(1) I(2) Cu(2) . 50.70(10) no
Cu(1) I(2) Cu(1) 3_655 59.00(10) no
Cu(2) I(2) Cu(1) 3_655 107.30(10) no
Cu(1) I(3) Cu(2) . 53.80(10) no
Cu(1) I(3) Cu(2) 2_655 116.00(10) no
Cu(2) I(3) Cu(2) 2_655 62.3(2) no
I(1) Cu(1) I(2) . 99.00(10) no
I(1) Cu(1) I(3) . 104.50(10) no
I(2) Cu(1) I(3) . 101.20(10) no
I(1) Cu(1) I(2) 3_655 118.20(10) no
I(2) Cu(1) I(2) 3_655 117.70(10) no
I(3) Cu(1) I(2) 3_655 113.80(10) no
I(1) Cu(2) I(2) . 97.90(10) no
I(1) Cu(2) I(3) . 105.1(2) no
I(2) Cu(2) I(3) . 100.20(10) no
I(1) Cu(2) I(3) 2_655 118.10(10) no
I(2) Cu(2) I(3) 2_655 114.70(10) no
I(3) Cu(2) I(3) 2_655 117.7(2) no
C(2) O(1) C(15) . 118(2) no
O(1) C(2) C(3) . 114.20 no
C(2) C(3) O(4) . 116(3) no
C(3) O(4) C(5) . 114(2) no
O(4) C(5) C(6) . 110(3) no
C(5) C(6) O(7) . 109(2) no
C(6) O(7) C(8) . 114(2) no
O(7) C(8) C(9) . 107.6(14) no
C(8) C(9) O(10) . 105(2) no
C(9) O(10) C(11) . 112.3(15) no
O(10) C(11) C(12) . 113(2) no
C(11) C(12) O(13) . 104(2) no
C(12) O(13) C(14) . 106(2) no
O(13) C(14) C(15) . 106(2) 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_2
_geom_bond_distance
_geom_bond_publ_flag
I(1) Cu(1) . 2.628(4) yes
I(1) Cu(2) . 2.620(4) yes
I(1) K(1) . 3.504(6) yes
I(2) Cu(1) . 2.832(4) yes
I(2) Cu(2) . 2.887(4) yes
I(2) Cu(1) 3_655 2.508(5) yes
I(3) Cu(1) . 2.714(4) yes
I(3) Cu(2) . 2.699(4) yes
I(3) Cu(2) 2_655 2.492(5) yes
Cu(1) Cu(2) . 2.448(7) yes
Cu(1) Cu(1) 3_655 2.646(5) yes
Cu(2) Cu(2) 2_655 2.691(8) yes
K(1) O(1) . 2.724(12) no
K(1) O(4) . 2.72(2) no
K(1) O(7) . 2.85(2) no
K(1) O(10) . 2.718(13) no
K(1) O(13) . 2.813(15) no
K(1) I(1) 3_655 3.589(4) yes
K(1) I(2) 3_655 3.779(5) yes
O(1) C(2) . 1.38(4) no
O(1) C(15) . 1.38(3) no
C(2) C(3) . 1.38(4) no
C(3) O(4) . 1.40(3) no
O(4) C(5) . 1.38(4) no
C(5) C(6) . 1.45(4) no
C(6) O(7) . 1.36(4) no
O(7) C(8) . 1.39(3) no
C(8) C(9) . 1.48(4) no
C(9) O(10) . 1.37(3) no
O(10) C(11) . 1.40(3) no
C(11) C(12) . 1.47(3) no
C(12) O(13) . 1.40(3) no
O(13) C(14) . 1.41(3) no
C(14) C(15) . 1.46(4) no