#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/82/2018253.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_2018253
loop_
_publ_author_name
'Friese, K.'
'Halasyamani, P. S.'
'Tolkiehn, M.'
'Grzechnik, A.'
_publ_section_title
;
 A high-pressure single-crystal synchrotron diffraction study of
 NH₄RbTe₄O₉·2H₂O: stability of three different
 TeOₓ coordination polyhedra
;
_journal_coeditor_code           LG3063
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              i45
_journal_page_last               i49
_journal_paper_doi               10.1107/S0108270111025728
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'N H4 Rb Te4 O9 , 2H2 O'
_chemical_formula_moiety         'O9 Te4 (NH4) 2(H2O) Rb'
_chemical_formula_sum            'H8 N O11 Rb Te4'
_chemical_formula_weight         793.9
_chemical_name_systematic
;
ammonium rubidium nonaoxotetratellurate(IV) dihydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_cell_angle_alpha                90
_cell_angle_beta                 101.61(18)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.770(4)
_cell_length_b                   6.645(4)
_cell_length_c                   20.800(7)
_cell_measurement_reflns_used    2941
_cell_measurement_temperature    293
_cell_measurement_theta_max      20.898
_cell_measurement_theta_min      1.24
_cell_volume                     2541(2)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'Automar (Marresearch, 2009)'
_computing_data_reduction
;
XDS (Kabsch, 2010) and JANA2006 (Petříček et al.,
2006)
;
_computing_molecular_graphics    'ATOMS (Dowty, 1999)'
_computing_publication_material
;
JANA2006 (Petříček et al., 2006)
;
_computing_structure_refinement
;
JANA2006 (Petříček et al., 2006)
;
_computing_structure_solution    'coordinates from Kim & Halasyamani (2008)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.41
_diffrn_measured_fraction_theta_max 0.12
_diffrn_measurement_device       'Huber four-circle'
_diffrn_measurement_device_type
'Huber four-circle diffractometer with Marresearch MarCCD165 area detector'
_diffrn_measurement_method       φ
_diffrn_radiation_source         HASYLAB
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.3978
_diffrn_reflns_av_R_equivalents  0.1888
_diffrn_reflns_av_sigmaI/netI    0.0836
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            2941
_diffrn_reflns_reduction_process
;
XDS (Kabsch, 2010) and JANA2006 (Pet\<r\'i\<cek et al., 2006)
;
_diffrn_reflns_theta_full        8.73
_diffrn_reflns_theta_max         20.898
_diffrn_reflns_theta_min         1.24
_exptl_absorpt_coefficient_mu    2.223
_exptl_absorpt_correction_T_max  0.7863
_exptl_absorpt_correction_T_min  0.5315
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'(JANA2006; Petříček et al., 2006)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    4.112
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         4.36
_refine_diff_density_min         -3.28
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   3.38
_refine_ls_hydrogen_treatment    undef
_refine_ls_number_constraints    0
_refine_ls_number_parameters     85
_refine_ls_number_reflns         987
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1251
_refine_ls_R_factor_gt           0.1251
_refine_ls_shift/su_max          0.0042
_refine_ls_shift/su_mean         0.0005
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/(σ²(F)+0.0001F²)'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1149
_reflns_number_gt                987
_reflns_number_total             987
_reflns_threshold_expression     I>3σ(I)
_cod_data_source_file            lg3063.cif
_cod_data_source_block           I_1.13GPa
_cod_original_cell_volume        2541(3)
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_original_formula_sum        'H8 N1 O11 Rb1 Te4'
_cod_database_code               2018253
_cod_database_fobs_code          2018253
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x+1/2,y,-z
3 -x,-y,-z
4 x+1/2,-y,z
5 x+1/2,y+1/2,z+1/2
6 -x,y+1/2,-z+1/2
7 -x+1/2,-y+1/2,-z+1/2
8 x,-y+1/2,z+1/2
loop_
_atom_site_type_symbol
_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_occupancy
_atom_site_symmetry_multiplicity
Te Te1 0.1211(2) 0.6159(6) 0.3071(5) 0.020(5) Uani d 1 8
Te Te2 0.0556(2) 0.1224(5) 0.1987(5) 0.030(5) Uani d 1 8
Te Te3 0.2200(2) 0.1902(5) 0.3163(5) 0.015(4) Uani d 1 8
Te Te4 0.3146(2) 0.6700(6) 0.3544(5) 0.029(5) Uani d 1 8
Rb Rb1 0.25 0.4185(13) 0.5 0.026(2) Uiso d 0.78 4
Rb Rb2 0.0345(4) 0.1016(11) 0.3951(10) 0.0154(16) Uiso d 0.61 8
O O1 0.0529(19) 0.672(5) 0.359(4) 0.019(3) Uiso d 1 8
O O2 0.205(2) 0.718(5) 0.358(4) 0.019(3) Uiso d 1 8
O O3 0.1397(19) 0.359(4) 0.343(4) 0.019(3) Uiso d 1 8
O O4 -0.007(2) -0.016(5) 0.246(5) 0.019(3) Uiso d 1 8
O O5 0.429(2) 0.581(5) 0.358(4) 0.019(3) Uiso d 1 8
O O6 0.1492(19) 0.024(5) 0.263(4) 0.019(3) Uiso d 1 8
O O7 0.2115(19) 0.405(5) 0.249(4) 0.019(3) Uiso d 1 8
O O8 0.3003(19) 0.400(5) 0.374(4) 0.019(3) Uiso d 1 8
O O9 0.3445(19) 0.789(5) 0.428(4) 0.019(3) Uiso d 1 8
O O10 0.077(2) 0.368(5) 0.057(5) 0.025(7) Uiso d 1 8
O O11 0.313(2) 0.496(5) 0.040(5) 0.025(7) Uiso d 1 8
N N1 0.098(4) 0.487(11) 0.507(10) 0.009(13) Uiso d 0.5 8
N N1A 0.052(4) 0.535(11) 0.487(9) 0.009(13) Uiso d 0.5 8
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N 0.0004 0.0009 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Rb 0.2686 1.1082 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Te -3.2035 0.5975 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
O 0.0015 0.0017 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Te1 O2 . . 102(3) no
O1 Te1 O3 . . 92(3) no
O1 Te1 O4 . 6_555 72(3) no
O2 Te1 O3 . . 92(2) no
O2 Te1 O4 . 6_555 173(4) no
O3 Te1 O4 . 6_555 85.8(17) no
O1 Te2 O4 6_545 . 76(3) no
O1 Te2 O5 6_545 7_555 90(2) no
O1 Te2 O6 6_545 . 168(2) no
O4 Te2 O5 . 7_555 99(3) no
O4 Te2 O6 . . 93(2) no
O5 Te2 O6 7_555 . 88(2) no
O3 Te3 O6 . . 90(2) no
O3 Te3 O7 . . 81(3) no
O3 Te3 O7 . 7_555 155(3) no
O3 Te3 O8 . . 88.1(18) no
O6 Te3 O7 . . 93(3) no
O6 Te3 O7 . 7_555 84(2) no
O6 Te3 O8 . . 176(2) no
O7 Te3 O7 . 7_555 75(2) no
O7 Te3 O8 . . 83(2) no
O7 Te3 O8 7_555 . 96(2) no
O2 Te4 O5 . . 172(2) no
O2 Te4 O8 . . 87.4(16) no
O2 Te4 O9 . . 93(3) no
O5 Te4 O8 . . 85.3(16) no
O5 Te4 O9 . . 87(2) no
O8 Te4 O9 . . 107(3) no
O8 Rb1 O8 . 2_556 175.2(9) no
O8 Rb1 O11 . 7_555 84.1(19) no
O8 Rb1 O11 . 8_555 91.5(19) no
O8 Rb1 N1 . . 123(4) no
O8 Rb1 N1 . 2_556 58(4) no
O8 Rb1 O11 2_556 7_555 91.5(19) no
O8 Rb1 O11 2_556 8_555 84.1(19) no
O8 Rb1 N1 2_556 . 58(4) no
O8 Rb1 N1 2_556 2_556 123(4) no
O11 Rb1 O11 7_555 8_555 50.3(13) no
O11 Rb1 N1 7_555 . 80.0(19) no
O11 Rb1 N1 7_555 2_556 117(2) no
O11 Rb1 N1 8_555 . 117(2) no
O11 Rb1 N1 8_555 2_556 80.0(19) no
N1 Rb1 N1 . 2_556 162(2) no
O1 Rb2 O3 1_545 . 109.9(17) no
O1 Rb2 O4 1_545 . 62.2(17) no
O1 Rb2 O5 1_545 4_465 137.6(15) no
O1 Rb2 O10 1_545 6_545 72.8(16) no
O1 Rb2 O10 1_545 8_555 107.3(18) no
O1 Rb2 O11 1_545 7_555 76.0(12) no
O1 Rb2 N1A 1_545 . 160(3) no
O3 Rb2 O4 . . 80.6(18) no
O3 Rb2 O5 . 4_465 87.2(13) no
O3 Rb2 O10 . 6_545 176.2(11) no
O3 Rb2 O10 . 8_555 107.1(17) no
O3 Rb2 O11 . 7_555 69.1(16) no
O3 Rb2 N1A . . 74(3) no
O4 Rb2 O5 . 4_465 84.0(18) no
O4 Rb2 O10 . 6_545 98.6(19) no
O4 Rb2 O10 . 8_555 169.0(10) no
O4 Rb2 O11 . 7_555 114.9(19) no
O4 Rb2 N1A . . 137(3) no
O5 Rb2 O10 4_465 6_545 89.0(13) no
O5 Rb2 O10 4_465 8_555 103.9(19) no
O5 Rb2 O11 4_465 7_555 145.4(11) no
O5 Rb2 N1A 4_465 . 61(2) no
O10 Rb2 O10 6_545 8_555 74.2(19) no
O10 Rb2 O11 6_545 7_555 114.5(18) no
O10 Rb2 N1A 6_545 . 104(3) no
O10 Rb2 O11 8_555 7_555 63(2) no
O10 Rb2 N1A 8_555 . 53(3) no
O11 Rb2 N1A 7_555 . 87.4(18) 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
Te1 O1 . 1.87(7) no
Te1 O2 . 1.84(5) no
Te1 O3 . 1.87(4) no
Te2 O1 6_545 2.17(5) no
Te2 O4 . 1.92(7) no
Te2 O5 7_555 1.85(6) no
Te2 O6 . 2.09(5) no
Te3 O3 . 2.05(5) no
Te3 O6 . 1.90(5) no
Te3 O7 . 1.99(7) no
Te3 O7 7_555 2.14(7) no
Te3 O8 . 2.21(5) no
Te4 O2 . 2.09(4) no
Te4 O5 . 2.22(4) no
Te4 O8 . 1.87(4) no
Te4 O9 . 1.71(8) no
Rb1 O8 . 2.97(8) no
Rb1 O8 2_556 2.97(8) no
Rb1 O11 7_555 3.04(4) no
Rb1 O11 8_555 3.04(4) no
Rb1 N1 . 2.93(9) no
Rb1 N1 2_556 2.93(9) no
Rb2 O1 1_545 2.99(4) no
Rb2 O3 . 2.97(6) no
Rb2 O4 . 3.14(9) no
Rb2 O5 4_465 2.88(4) no
Rb2 O10 6_545 2.93(6) no
Rb2 O10 8_555 3.31(9) no
Rb2 O11 7_555 2.99(4) no
Rb2 N1A . 3.44(12) no
N1 N1A . 0.94(12) no
N1A N1A 3_566 2.16(16) no
