#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:20:38 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179477 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/74/4337411.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_4337411
loop_
_publ_author_name
'Xu, Xiang'
'Yang, Bing-Ping'
'Huang, Chao'
'Mao, Jiang-Gao'
_publ_section_title
;
 Explorations of New Second-Order Nonlinear Optical Materials in the
 Ternary Rubidium Iodate System: Noncentrosymmetric β-RbIO3(HIO3)2 and
 Centrosymmetric Rb3(IO3)3(I2O5)(HIO3)4(H2O).
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1756
_journal_page_last               1763
_journal_paper_doi               10.1021/ic4028942
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'H6 I9 O27 Rb3'
_chemical_formula_weight         1836.56
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 111.053(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5195(3)
_cell_length_b                   25.5012(7)
_cell_length_c                   13.3874(7)
_cell_measurement_reflns_used    8146
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.3124
_cell_measurement_theta_min      2.2776
_cell_volume                     2714.4(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3503
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0538
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13217
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    15.731
_exptl_absorpt_correction_T_max  0.755
_exptl_absorpt_correction_T_min  0.126
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3240
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.470
_refine_diff_density_min         -1.743
_refine_diff_density_rms         0.311
_refine_ls_extinction_coef       0.00199(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         5542
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0324
_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)+(0.0233P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0706
_reflns_number_gt                4898
_reflns_number_total             5542
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4028942_si_002.cif
_cod_data_source_block           Rb3H6I9O27
_cod_original_cell_volume        2714.36(19)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4337411
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Rb1 Rb 0.66897(8) 0.42631(3) 0.74475(5) 0.02473(16) Uani 1 1 d .
Rb2 Rb 0.25358(8) 0.42523(3) 0.06395(5) 0.02640(16) Uani 1 1 d .
Rb3 Rb 0.96974(8) 0.42887(3) 0.39829(5) 0.02327(15) Uani 1 1 d .
I1 I 0.17822(4) 0.305708(15) 0.26837(3) 0.01325(10) Uani 1 1 d .
I2 I 0.96136(5) 0.201858(15) 0.44428(3) 0.01417(10) Uani 1 1 d .
I3 I 0.44825(4) 0.316789(16) -0.08091(3) 0.01498(10) Uani 1 1 d .
I4 I 0.85914(4) 0.304467(15) 0.59344(3) 0.01383(10) Uani 1 1 d .
I5 I 1.11320(5) 0.412554(16) 0.72810(3) 0.01571(11) Uani 1 1 d .
I6 I 0.78318(5) 0.415594(16) 0.07784(3) 0.01711(11) Uani 1 1 d .
I7 I 0.66911(4) 0.302090(15) 0.26403(3) 0.01364(10) Uani 1 1 d .
I8 I 0.46883(5) 0.418728(16) 0.40644(3) 0.01633(10) Uani 1 1 d .
I9 I 0.36493(4) 0.305125(15) 0.59943(3) 0.01370(10) Uani 1 1 d .
O1 O 0.1315(5) 0.33119(18) 0.1358(3) 0.0250(10) Uani 1 1 d .
O2 O 0.3840(5) 0.27705(17) 0.2950(3) 0.0206(10) Uani 1 1 d .
O3 O 0.2262(5) 0.36849(17) 0.3385(3) 0.0211(10) Uani 1 1 d .
O4 O 0.8946(5) 0.13550(17) 0.4303(3) 0.0224(10) Uani 1 1 d .
O5 O 0.8601(5) 0.22519(18) 0.3077(3) 0.0236(10) Uani 1 1 d .
O6 O 0.8023(5) 0.22897(17) 0.4972(3) 0.0201(10) Uani 1 1 d .
O7 O 0.4844(5) 0.33998(18) -0.1973(3) 0.0236(10) Uani 1 1 d .
O8 O 0.2285(5) 0.33292(18) -0.1154(3) 0.0245(10) Uani 1 1 d .
O9 O 0.5278(5) 0.37454(18) 0.0033(3) 0.0250(10) Uani 1 1 d .
O10 O 0.8253(5) 0.33735(18) 0.4695(3) 0.0247(10) Uani 1 1 d .
O11 O 1.0761(5) 0.28534(17) 0.6390(3) 0.0199(10) Uani 1 1 d .
O12 O 0.9065(5) 0.37189(16) 0.6736(3) 0.0207(10) Uani 1 1 d .
O13 O 1.0634(5) 0.45999(18) 0.6244(3) 0.0266(11) Uani 1 1 d .
O14 O 1.0463(5) 0.44560(17) 0.8230(3) 0.0225(10) Uani 1 1 d .
O15 O 0.7046(5) 0.46170(19) -0.0281(3) 0.0267(11) Uani 1 1 d .
O16 O 0.6859(5) 0.43888(17) 0.1697(3) 0.0208(10) Uani 1 1 d .
O17 O 0.9897(5) 0.45180(18) 0.1501(4) 0.0294(11) Uani 1 1 d .
H17A H 0.9703 0.4829 0.1558 0.035 Uiso 1 1 d R
O18 O 0.8415(5) 0.33321(18) 0.2403(3) 0.0215(10) Uani 1 1 d .
O19 O 0.5637(5) 0.27260(17) 0.1351(3) 0.0203(10) Uani 1 1 d .
O20 O 0.5436(5) 0.36635(17) 0.2421(3) 0.0202(10) Uani 1 1 d .
H20A H 0.6220 0.3890 0.2588 0.024 Uiso 1 1 d R
O21 O 0.3865(5) 0.46248(18) 0.2977(3) 0.0271(11) Uani 1 1 d .
O22 O 0.3689(5) 0.44255(18) 0.4961(3) 0.0238(10) Uani 1 1 d .
O23 O 0.6771(5) 0.45455(19) 0.4756(4) 0.0338(12) Uani 1 1 d .
H23A H 0.6584 0.4856 0.4829 0.041 Uiso 1 1 d R
O24 O 0.2551(5) 0.27401(18) 0.4738(3) 0.0220(10) Uani 1 1 d .
O25 O 0.5360(5) 0.33690(16) 0.5756(3) 0.0182(9) Uani 1 1 d .
O26 O 0.2384(5) 0.36888(16) 0.5782(3) 0.0178(9) Uani 1 1 d .
H26A H 0.3152 0.3918 0.6026 0.021 Uiso 1 1 d R
O1W O 0.3866(5) 0.45932(19) 0.8133(4) 0.0306(11) Uani 1 1 d .
H1WA H 0.4216 0.4613 0.8811 0.046 Uiso 1 1 d R
H1WB H 0.3503 0.4891 0.7863 0.046 Uiso 1 1 d R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.9393 2.9676 '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
O1 I1 O2 101.28(19) . .
O1 I1 O3 96.9(2) . .
O2 I1 O3 103.31(18) . .
O4 I2 O5 100.8(2) . .
O4 I2 O6 98.28(18) . .
O5 I2 O6 96.51(18) . .
O7 I3 O8 100.87(19) . .
O7 I3 O9 97.4(2) . .
O8 I3 O9 95.42(19) . .
O10 I4 O11 104.25(19) . .
O10 I4 O12 91.68(19) . .
O11 I4 O12 93.85(18) . .
O10 I4 O6 86.61(17) . .
O11 I4 O6 86.92(16) . .
O12 I4 O6 178.26(16) . .
O13 I5 O14 100.8(2) . .
O13 I5 O12 98.07(19) . .
O14 I5 O12 92.36(18) . .
O13 I5 O1W 87.32(18) . 1_655
O14 I5 O1W 86.18(17) . 1_655
O12 I5 O1W 174.59(17) . 1_655
O15 I6 O16 101.0(2) . .
O15 I6 O17 95.7(2) . .
O16 I6 O17 93.47(18) . .
O15 I6 O9 85.88(18) . .
O16 I6 O9 81.45(16) . .
O17 I6 O9 174.90(16) . .
O18 I7 O19 100.00(18) . .
O18 I7 O20 92.39(19) . .
O19 I7 O20 98.70(18) . .
O18 I7 O5 83.23(17) . .
O19 I7 O5 87.40(16) . .
O20 I7 O5 173.05(16) . .
O21 I8 O22 101.1(2) . .
O21 I8 O23 97.0(2) . .
O22 I8 O23 95.40(19) . .
O21 I8 O3 89.51(18) . .
O22 I8 O3 83.13(17) . .
O23 I8 O3 173.48(18) . .
O24 I9 O25 102.53(18) . .
O24 I9 O26 99.25(18) . .
O25 I9 O26 92.31(18) . .
O24 I9 O19 85.35(16) . 4_566
O25 I9 O19 81.75(16) . 4_566
O26 I9 O19 173.20(16) . 4_566
I1 O3 I8 133.5(2) . .
I2 O5 I7 121.97(19) . .
I2 O6 I4 119.47(19) . .
I3 O9 I6 135.9(2) . .
I5 O12 I4 130.0(2) . .
I6 O17 H17A 109.5 . .
I7 O19 I9 125.21(19) . 4_565
I7 O20 H20A 101.4 . .
I8 O23 H23A 109.4 . .
I9 O26 H26A 102.2 . .
I5 O1W H1WA 115.4 1_455 .
I5 O1W H1WB 95.5 1_455 .
H1WA O1W H1WB 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I1 O1 1.795(4) .
I1 O2 1.812(4) .
I1 O3 1.826(4) .
I2 O4 1.774(4) .
I2 O5 1.819(4) .
I2 O6 1.873(4) .
I3 O7 1.794(4) .
I3 O8 1.807(4) .
I3 O9 1.830(4) .
I4 O10 1.788(4) .
I4 O11 1.793(4) .
I4 O12 1.990(4) .
I4 O6 2.270(4) .
I5 O13 1.774(4) .
I5 O14 1.780(4) .
I5 O12 1.946(4) .
I5 O1W 2.498(4) 1_655
I6 O15 1.777(4) .
I6 O16 1.813(4) .
I6 O17 1.914(4) .
I6 O9 2.295(4) .
I7 O18 1.795(4) .
I7 O19 1.799(4) .
I7 O20 1.921(4) .
I7 O5 2.480(4) .
I8 O21 1.767(4) .
I8 O22 1.807(4) .
I8 O23 1.913(4) .
I8 O3 2.322(4) .
I9 O24 1.790(4) .
I9 O25 1.794(4) .
I9 O26 1.915(4) .
I9 O19 2.538(4) 4_566
O17 H17A 0.8202 .
O19 I9 2.538(4) 4_565
O20 H20A 0.8501 .
O23 H23A 0.8198 .
O26 H26A 0.8501 .
O1W I5 2.498(4) 1_455
O1W H1WA 0.8500 .
O1W H1WB 0.8500 .
