#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2007286.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_2007286
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         '[Rb(C10 H20 O5)][Cu2 I3]'
_chemical_formula_sum            'C10 H20 Cu2 I3 O5 Rb'
_chemical_formula_weight         813.5
_chemical_name_systematic
;
Rubidium 15-Crown-5  Dicopper 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                 119.900(10)
_cell_angle_gamma                90.0
_cell_formula_units_Z            8
_cell_length_a                   24.613(3)
_cell_length_b                   11.1700(10)
_cell_length_c                   17.211(3)
_cell_measurement_reflns_used    46
_cell_measurement_temperature    301
_cell_measurement_theta_max      12.481
_cell_measurement_theta_min      5.018
_cell_volume                     4102.0(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'
_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  0.0347
_diffrn_reflns_limit_h_max       34
_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            6963
_diffrn_reflns_theta_max         30
_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    8.960
_exptl_absorpt_correction_T_max  0.41
_exptl_absorpt_correction_T_min  0.17
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(Sheldrick, 1990)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.635
_exptl_crystal_density_method    none
_exptl_crystal_description       rods
_exptl_crystal_F_000             2992
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.0
_refine_diff_density_min         -0.99
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.93
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         5968
_refine_ls_R_factor_gt           0.0584
_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         0.0575
_reflns_number_gt                1929
_reflns_number_total             5968
_reflns_threshold_expression     F>3.5\s(F)
_[local]_cod_data_source_file    sx1047.cif
_[local]_cod_data_source_block   III
_[local]_cod_cif_authors_sg_H-M  'C 2/c'
_[local]_cod_chemical_formula_sum_orig 'C10 H20 Cu2 I3 O5 Rb1'
_cod_original_cell_volume        4101.9(9)
_cod_database_code               2007286
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) 0.45950(10) -0.25250(10) 0.09840(10) 0.0430(10) Uani d .
I(2) 0.59550(10) 0.00820(10) 0.25560(10) 0.0440(10) Uani d .
I(3) 0.42740(10) 0.11100(10) 0.01360(10) 0.0470(10) Uani d .
Cu(1) 0.4627(2) -0.0337(3) 0.1602(2) 0.076(2) Uani d .
Cu(2) 0.5149(2) -0.0690(3) 0.0707(3) 0.094(2) Uani d .
Rb(1) 0.37890(10) -0.3294(2) 0.22000(10) 0.0510(10) Uani d .
O(1) 0.2467(6) -0.330(2) 0.0991(11) 0.070(9) Uani d .
C(2) 0.2095(12) -0.341(3) 0.138(2) 0.12(2) Uani d .
H(2A) 0.2054 -0.4234 0.1491 0.080 Uiso calc R
H(2B) 0.1685 -0.3098 0.0976 0.080 Uiso calc R
C(3) 0.236(2) -0.273(3) 0.219(2) 0.12(2) Uani d .
H(3A) 0.2380 -0.1908 0.2057 0.080 Uiso calc R
H(3B) 0.2077 -0.2786 0.2424 0.080 Uiso calc R
O(4) 0.2921(11) -0.307(2) 0.2849(15) 0.097(13) Uani d .
C(5) 0.294(2) -0.383(3) 0.343(2) 0.10(2) Uani d .
H(5A) 0.2628 -0.4433 0.3118 0.080 Uiso calc R
H(5B) 0.2829 -0.3419 0.3822 0.080 Uiso calc R
C(6) 0.354(2) -0.440(3) 0.397(2) 0.10(2) Uani d .
H(6A) 0.3861 -0.3814 0.4281 0.080 Uiso calc R
H(6B) 0.3526 -0.4910 0.4414 0.080 Uiso calc R
O(7) 0.3678(8) -0.510(2) 0.3411(10) 0.075(9) Uani d .
C(8) 0.4286(11) -0.554(3) 0.3832(15) 0.076(14) Uani d .
H(8A) 0.4371 -0.5990 0.4355 0.080 Uiso calc R
H(8B) 0.4583 -0.4893 0.4010 0.080 Uiso calc R
C(9) 0.4322(9) -0.630(3) 0.317(2) 0.073(13) Uani d .
H(9A) 0.4706 -0.6748 0.3464 0.080 Uiso calc R
H(9B) 0.3981 -0.6861 0.2943 0.080 Uiso calc R
O(10) 0.4298(6) -0.5650(15) 0.2468(12) 0.069(9) Uani d .
C(11) 0.4095(13) -0.629(2) 0.164(2) 0.08(2) Uani d .
H(11A) 0.4271 -0.7076 0.1773 0.080 Uiso calc R
H(11B) 0.4246 -0.5881 0.1296 0.080 Uiso calc R
C(12) 0.3437(13) -0.637(2) 0.113(2) 0.09(2) Uani d .
H(12A) 0.3322 -0.6864 0.0616 0.080 Uiso calc R
H(12B) 0.3285 -0.6754 0.1488 0.080 Uiso calc R
O(13) 0.3154(7) -0.527(2) 0.0859(11) 0.068(9) Uani d .
C(14) 0.2483(11) -0.530(3) 0.042(2) 0.078(15) Uani d .
H(14A) 0.2347 -0.5671 0.0797 0.080 Uiso calc R
H(14B) 0.2315 -0.5736 -0.0130 0.080 Uiso calc R
C(15) 0.2269(14) -0.402(3) 0.024(2) 0.10(2) Uani d .
H(15A) 0.2411 -0.3673 -0.0140 0.080 Uiso calc R
H(15B) 0.1819 -0.4019 -0.0094 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) 0.0520(10) 0.0350(10) 0.0450(10) -0.0040(10) 0.0270(10) -0.0040(10)
I(2) 0.0500(10) 0.0420(10) 0.0470(10) -0.0090(10) 0.0290(10) -0.0040(10)
I(3) 0.0560(10) 0.0440(10) 0.0500(10) 0.0140(10) 0.0350(10) 0.0110(10)
Cu(1) 0.115(2) 0.064(2) 0.085(2) 0.001(2) 0.077(2) -0.009(2)
Cu(2) 0.139(3) 0.064(2) 0.147(3) 0.025(2) 0.123(3) 0.028(2)
Rb(1) 0.0490(10) 0.0410(10) 0.0610(10) -0.0070(10) 0.0260(10) 0.0070(10)
O(1) 0.039(9) 0.088(14) 0.068(11) 0.016(9) 0.014(9) -0.002(10)
C(2) 0.05(2) 0.18(4) 0.09(2) 0.01(2) 0.01(2) 0.01(3)
C(3) 0.11(3) 0.13(3) 0.13(3) 0.05(3) 0.08(3) 0.03(3)
O(4) 0.13(2) 0.09(2) 0.091(15) 0.030(14) 0.068(14) 0.020(13)
C(5) 0.15(3) 0.11(3) 0.08(2) 0.00(2) 0.07(2) 0.01(2)
C(6) 0.18(3) 0.09(2) 0.05(2) -0.03(2) 0.06(2) 0.00(2)
O(7) 0.088(12) 0.076(13) 0.062(11) -0.011(11) 0.039(10) -0.005(11)
C(8) 0.07(2) 0.10(2) 0.043(14) -0.02(2) 0.012(14) 0.01(2)
C(9) 0.029(12) 0.10(2) 0.07(2) 0.012(14) 0.011(12) 0.03(2)
O(10) 0.057(10) 0.067(12) 0.091(12) 0.009(9) 0.043(10) 0.022(11)
C(11) 0.11(2) 0.07(2) 0.10(2) 0.04(2) 0.08(2) 0.03(2)
C(12) 0.09(2) 0.07(2) 0.14(3) -0.04(2) 0.09(2) -0.04(2)
O(13) 0.069(11) 0.057(12) 0.078(11) -0.008(10) 0.037(10) -0.014(10)
C(14) 0.07(2) 0.08(2) 0.06(2) -0.03(2) 0.017(14) -0.01(2)
C(15) 0.12(2) 0.09(3) 0.08(2) -0.01(2) 0.05(2) 0.00(2)
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'
Rb -1.044 2.973 '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) . 56.00(10) no
Cu(1) I(2) Cu(2) . 50.70(10) no
Cu(1) I(2) Cu(1) 3_655 59.40(10) no
Cu(2) I(2) Cu(1) 3_655 107.30(10) no
Cu(1) I(3) Cu(2) . 53.70(10) no
Cu(1) I(3) Cu(2) 2_655 114.00(10) no
Cu(2) I(3) Cu(2) 2_655 60.3(2) no
I(1) Cu(1) I(2) . 100.20(10) no
I(1) Cu(1) I(3) . 104.00(10) no
I(2) Cu(1) I(3) . 100.20(10) no
I(1) Cu(1) I(2) 3_655 119.2(2) no
I(2) Cu(1) I(2) 3_655 116.70(10) no
I(3) Cu(1) I(2) 3_655 114.00(10) no
I(1) Cu(2) I(2) . 99.5(2) no
I(1) Cu(2) I(3) . 104.5(2) no
I(2) Cu(2) I(3) . 99.20(10) no
I(1) Cu(2) I(3) 2_655 116.70(10) no
I(2) Cu(2) I(3) 2_655 114.20(10) no
I(3) Cu(2) I(3) 2_655 119.7(2) no
C(2) O(1) C(15) . 113(2) no
O(1) C(2) C(3) . 110(3) no
C(2) C(3) O(4) . 117(3) no
C(3) O(4) C(5) . 118(3) no
O(4) C(5) C(6) . 115(4) 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) . 106(2) no
C(8) C(9) O(10) . 112(2) no
C(9) O(10) C(11) . 117(2) no
O(10) C(11) C(12) . 112(3) 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) . 107(2) no
O(1) C(15) C(14) . 115(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) . 2.650(4) yes
I(1) Cu(2) . 2.633(5) yes
I(1) Rb(1) . 3.632(3) yes
I(2) Cu(1) . 2.872(4) yes
I(2) Cu(2) . 2.917(4) yes
I(2) Cu(1) 3_655 2.538(5) yes
I(3) Cu(1) . 2.747(4) yes
I(3) Cu(2) . 2.745(4) yes
I(3) Cu(2) 2_655 2.529(6) yes
Cu(1) Cu(2) . 2.480(7) yes
Cu(1) I(2) 3_655 2.538(5) yes
Cu(1) Cu(1) 3_655 2.697(6) yes
Cu(2) I(3) 2_655 2.529(6) yes
Cu(2) Cu(2) 2_655 2.657(8) yes
Rb(1) O(1) . 2.858(13) no
Rb(1) O(4) . 2.87(3) no
Rb(1) O(7) . 3.01(2) no
Rb(1) O(10) . 2.85(2) no
Rb(1) O(13) . 3.01(2) no
O(1) C(2) . 1.38(4) no
O(1) C(15) . 1.39(4) no
C(2) C(3) . 1.43(5) no
C(3) O(4) . 1.33(3) no
O(4) C(5) . 1.29(5) no
C(5) C(6) . 1.45(4) no
C(6) O(7) . 1.40(4) no
O(7) C(8) . 1.39(3) no
C(8) C(9) . 1.46(4) no
C(9) O(10) . 1.39(4) no
O(10) C(11) . 1.44(4) no
C(11) C(12) . 1.41(4) no
C(12) O(13) . 1.37(3) no
O(13) C(14) . 1.43(3) no
C(14) C(15) . 1.49(4) no