#------------------------------------------------------------------------------
#$Date: 2016-02-16 21:30:59 +0100 (mar 16 de feb de 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/59/4335978.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_4335978
loop_
_publ_author_name
'Charles J. Simmons'
'Horst Stratemeier'
'Michael A. Hitchman'
'Mark J. Riley'
_publ_section_title
;
 Influence of Lattice Interactions on the Jahn-Teller Distortion of the
 [Cu(H2O)6]2+ Ion: Dependence of the Crystal Structure of
 K2xRb2-2x[Cu(H2O)6](SeO4)2 upon the K/Rb Ratio
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10481
_journal_page_last               10499
_journal_paper_doi               10.1021/ic401385f
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'Cu H12 K0.52 O14 Rb1.48 Se2 '
_chemical_formula_sum            'Cu H12 K0.52 O14 Rb1.48 Se2'
_chemical_formula_weight         604.32
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_cell_angle_alpha                90
_cell_angle_beta                 104.495(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.3369(3)
_cell_length_b                   12.4707(3)
_cell_length_c                   6.3437(2)
_cell_measurement_reflns_used    7225
_cell_measurement_temperature    270
_cell_measurement_theta_max      37.1
_cell_measurement_theta_min      1.6
_cell_volume                     715.13(4)
_computing_cell_refinement       'HKL Scalepack'
_computing_data_collection       'KappaCCD Server Control'
_computing_data_reduction        'HKL Denzo and Scalepack'
_computing_publication_material  'teXsan for Windows v. 1.06 MSC'
_computing_structure_refinement  'teXsan for Windows v. 1.06 MSC'
_computing_structure_solution
;
SIR92 (Altomare, et. al. 1994)
;
_diffrn_ambient_temperature      270
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Nonius CCD camera'
_diffrn_measurement_method       'φ scans ω scans κ offsets'
_diffrn_radiation_detector       'Nonius Kappa CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed x-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.02471
_diffrn_reflns_av_sigmaI/netI    0.062
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7225
_diffrn_reflns_theta_full        37.09
_diffrn_reflns_theta_max         37.09
_diffrn_reflns_theta_min         1.63
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.83
_exptl_absorpt_correction_T_max  0.899
_exptl_absorpt_correction_T_min  0.715
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Denzo-SMN; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.807
_exptl_crystal_description       sphere
_exptl_crystal_F_000             571.3
_exptl_crystal_size_rad          0.30
_refine_diff_density_max         0.40
_refine_diff_density_min         -0.48
_refine_ls_extinction_coef       0.00000059(3)
_refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.'
_refine_ls_extinction_method     'Zachariasen (1967)'
_refine_ls_goodness_of_fit_all   1.326
_refine_ls_goodness_of_fit_ref   1.330
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    1
_refine_ls_number_parameters     123
_refine_ls_number_reflns         2069
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0184
_refine_ls_R_factor_gt           0.0180
_refine_ls_shift/su_max          0.0800
_refine_ls_shift/su_mean         0.0042
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(Fo)]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0190
_refine_ls_wR_factor_ref         0.0190
_reflns_number_gt                2069
_reflns_number_total             3625
_reflns_threshold_expression     I>5.00σ(I)
_cod_data_source_file            ic401385f_si_003_20.cif
_cod_data_source_block           '_Template_texray.inf19'
_cod_original_cell_volume        715.13(3)
_cod_original_sg_symbol_H-M      'P 21/a '
_cod_original_formula_sum        'Cu H12 K0.52 O14 Rb1.48 Se2 '
_cod_database_code               4335978
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'1/2-x,1/2+y,   -z'
'   -x,   -y,   -z'
'1/2+x,1/2-y,   +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_occupancy
_atom_site_refinement_flags
_atom_site_adp_type
_atom_site_calc_flag
Rb(10) 0.12631(4) 0.34333(3) 0.34408(6) 0.02641(7) 0.7402(10) S Uani d
Se(2) 0.40101(2) 0.138205(12) 0.73013(3) 0.01913(4) 1.000 . Uani d
Cu(1) 0.0000 0.0000 0.0000 0.01620(6) 1.000 S Uani d
K(10) 0.1404(3) 0.3548(2) 0.3495(4) 0.0285(5) 0.260 SP Uani d
O(3) 0.40676(13) 0.24368(9) 0.5794(2) 0.0301(3) 1.000 . Uani d
O(4) 0.55221(12) 0.06883(10) 0.7593(2) 0.0375(4) 1.000 . Uani d
O(5) 0.26163(11) 0.06313(9) 0.6029(2) 0.0240(3) 1.000 . Uani d
O(6) 0.37763(12) 0.17569(9) 0.9667(2) 0.0288(3) 1.000 . Uani d
O(7) 0.1569(1) 0.11173(10) 0.1630(2) 0.0289(3) 1.000 . Uani d
O(8) -0.1790(1) 0.11146(10) 0.0319(2) 0.0297(3) 1.000 . Uani d
O(9) -0.00441(12) -0.06167(9) 0.2797(2) 0.0210(3) 1.000 . Uani d
H(15) 0.189(2) 0.101(1) 0.262(3) 0.026(5) 1.000 . Uiso d
H(16) 0.221(2) 0.126(1) 0.105(3) 0.041(6) 1.000 . Uiso d
H(17) -0.248(2) 0.107(2) -0.049(3) 0.044(6) 1.000 . Uiso d
H(18) -0.155(2) 0.165(2) 0.006(3) 0.033(6) 1.000 . Uiso d
H(19) -0.075(2) -0.053(2) 0.310(3) 0.051(6) 1.000 . Uiso d
H(20) 0.029(2) -0.123(1) 0.315(3) 0.032(5) 1.000 . Uiso d
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
Rb(10) 0.0267(1) 0.0276(2) 0.0262(2) -0.00161(12) 0.00908(11) -0.00046(12)
Se(2) 0.01862(7) 0.02033(7) 0.01854(8) -0.00259(6) 0.00484(6) -0.00125(6)
Cu(1) 0.01625(12) 0.01795(13) 0.01462(12) -0.00210(10) 0.00429(10) 0.00101(10)
K(10) 0.0303(9) 0.0235(9) 0.0359(11) -0.0097(8) 0.0164(7) -0.0037(8)
O(3) 0.0430(7) 0.0250(6) 0.0230(6) -0.0095(5) 0.0097(5) 0.0023(5)
O(4) 0.0203(6) 0.0423(8) 0.0473(8) 0.0069(6) 0.0039(5) -0.0054(6)
O(5) 0.0197(5) 0.0293(6) 0.0234(6) -0.0090(5) 0.0062(4) -0.0063(5)
O(6) 0.0412(7) 0.0293(6) 0.0169(6) -0.0026(6) 0.0092(5) -0.0024(5)
O(7) 0.0281(6) 0.0396(7) 0.0191(6) -0.0038(6) 0.0062(5) 0.0028(6)
O(8) 0.0273(7) 0.0283(7) 0.0309(7) -0.0047(6) 0.0026(5) 0.0040(6)
O(9) 0.0220(6) 0.0227(6) 0.0200(5) 0.0019(5) 0.0083(4) 0.0034(5)
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H 0 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
O 0 0.008 0.006
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
K 0 0.179 0.250
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
Cu 0 0.263 1.266
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Se 0 -0.178 2.223
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Rb 0 -1.044 2.973
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
0 0 0
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
O3 SE2 O4 109.88(7) ?
O3 SE2 O5 108.01(6) ?
O3 SE2 O6 109.73(6) ?
O4 SE2 O5 108.14(7) ?
O4 SE2 O6 111.01(7) ?
O5 SE2 O6 110.01(6) ?
O7 CU1 O7 180.00 ?
O7 CU1 O8 89.30(6) ?
O7 CU1 O9 89.12(6) ?
O8 CU1 O8 180.00 ?
O8 CU1 O9 88.63(5) ?
O9 CU1 O9 180.00 ?
CU1 O7 H15 116.4(19) no
CU1 O7 H16 115.7(15) no
H15 O7 H16 106.4(23) no
CU1 O8 H17 116.7(18) no
CU1 O8 H18 105.7(16) no
H17 O8 H18 100.1(22) no
CU1 O9 H19 113.9(18) no
CU1 O9 H20 120.8(13) no
H19 O9 H20 111.2(22) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
RB10 K10 0.191(3) ?
SE2 O3 1.6348(12) ?
SE2 O4 1.6263(13) ?
SE2 O5 1.6420(12) ?
SE2 O6 1.6379(12) ?
CU1 O7 2.097(1) ?
CU1 O7 2.097(1) ?
CU1 O8 2.222(2) ?
CU1 O8 2.222(2) ?
CU1 O9 1.9439(12) ?
CU1 O9 1.9439(12) ?
O7 H15 0.64(2) no
O7 H16 0.80(2) no
O8 H17 0.72(2) no
O8 H18 0.74(2) no
O9 H19 0.74(2) no
O9 H20 0.84(2) no
