#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/28/2102804.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_2102804
loop_
_publ_author_name
'Schwendtner, Karolina'
'Kolitsch, Uwe'
_publ_section_title
;
 Octahedral As in M⁺ arsenates -- architecture and seven new
 members
;
_journal_coeditor_code           SN5044
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              205
_journal_page_last               215
_journal_paper_doi               10.1107/S0108768106054942
_journal_volume                  63
_journal_year                    2007
_chemical_formula_structural     'Rb1 H3 As4 O12'
_chemical_formula_sum            'As4 H3 O12 Rb'
_chemical_formula_weight         580.17
_chemical_name_common            'rubidium hydrogen arsenate'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                63.31(3)
_cell_angle_beta                 79.87(3)
_cell_angle_gamma                84.38(3)
_cell_formula_units_Z            1
_cell_length_a                   5.1690(10)
_cell_length_b                   7.0360(10)
_cell_length_c                   7.766(2)
_cell_measurement_reflns_used    2175
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      34.975
_cell_measurement_theta_min      2.037
_cell_volume                     248.36(11)
_computing_cell_refinement       'HKL SCALEPACK (Otwinowski & Minor 1997)'
_computing_data_collection       'COLLECT (Nonius, 2003)'
_computing_data_reduction
'HKL DENZO, SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2005)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4335
_diffrn_reflns_theta_full        34.98
_diffrn_reflns_theta_max         34.98
_diffrn_reflns_theta_min         2.97
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.269
_exptl_absorpt_correction_T_max  0.4619
_exptl_absorpt_correction_T_min  0.1472
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.879
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tabular
_exptl_crystal_F_000             268
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.374
_refine_diff_density_min         -1.590
_refine_ls_extinction_coef       0.059(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     88
_refine_ls_number_reflns         2190
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0495P)²+0.1743P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0771
_reflns_number_gt                1995
_reflns_number_total             2190
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sn5044.cif
_cod_data_source_block           RbH3As4O12
_cod_original_formula_sum        'H3 As4 O12 Rb'
_cod_database_code               2102804
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_refinement_flags
_atom_site_occupancy
As As1 0.15396(4) 0.32137(3) 0.31490(3) 0.00901(8) Uani d . 1
As As2 0.59768(4) 0.12418(3) 0.56642(3) 0.00815(8) Uani d . 1
Rb Rb1 0.0000 0.0000 0.0000 0.01993(9) Uani d S 1
O O1 0.1052(4) 0.5354(3) 0.1122(3) 0.0209(4) Uani d D 1
O O2 0.2239(3) 0.1092(3) 0.2642(2) 0.0116(3) Uani d . 1
O O3 0.4152(3) 0.3674(2) 0.3963(3) 0.0109(3) Uani d . 1
O O4 0.8874(3) 0.2888(3) 0.4888(3) 0.0129(3) Uani d . 1
O O5 0.4984(4) 0.1927(3) 0.7587(3) 0.0131(3) Uani d D 1
O O6 0.6886(3) 0.0366(3) 0.3769(2) 0.0101(3) Uani d . 1
H H1 0.502(8) 0.328(3) 0.712(6) 0.030(11) Uiso d D 1
H H2 0.053(16) 0.486(13) 0.035(11) 0.022(19) Uiso d PD 0.50
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
As1 0.00904(11) 0.00758(12) 0.01041(12) -0.00053(7) -0.00326(7) -0.00325(8)
As2 0.00761(11) 0.00791(12) 0.01007(12) -0.00086(7) -0.00199(7) -0.00459(8)
Rb1 0.02122(17) 0.02220(18) 0.01891(17) -0.00591(12) -0.00134(12) -0.01081(14)
O1 0.0342(11) 0.0093(7) 0.0167(8) 0.0004(7) -0.0135(8) -0.0002(6)
O2 0.0140(7) 0.0095(7) 0.0126(7) 0.0010(5) -0.0055(5) -0.0050(6)
O3 0.0096(6) 0.0076(6) 0.0153(7) -0.0005(5) -0.0055(5) -0.0036(5)
O4 0.0079(6) 0.0134(7) 0.0206(8) -0.0023(5) -0.0003(5) -0.0107(6)
O5 0.0178(7) 0.0116(7) 0.0128(7) -0.0011(6) -0.0005(6) -0.0083(6)
O6 0.0087(6) 0.0101(7) 0.0128(7) -0.0020(5) -0.0005(5) -0.0061(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 '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'
As As 0.0499 2.0058 '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_1
_geom_angle_site_symmetry_3
_geom_angle
O1 As1 O2 . . 109.12(10)
O1 As1 O3 . . 107.75(10)
O2 As1 O3 . . 109.49(8)
O1 As1 O4 . 1_455 109.11(11)
O2 As1 O4 . 1_455 114.02(8)
O3 As1 O4 . 1_455 107.15(8)
O5 As2 O6 . . 176.13(8)
O5 As2 O6 . 2_656 94.20(8)
O6 As2 O6 . 2_656 82.40(8)
O5 As2 O4 . . 90.07(8)
O6 As2 O4 . . 93.39(8)
O6 As2 O4 2_656 . 175.28(8)
O5 As2 O2 . 2_656 87.66(8)
O6 As2 O2 . 2_656 90.53(8)
O6 As2 O2 2_656 2_656 90.96(8)
O4 As2 O2 . 2_656 91.22(8)
O5 As2 O3 . . 91.04(8)
O6 As2 O3 . . 90.81(8)
O6 As2 O3 2_656 . 89.75(7)
O4 As2 O3 . . 88.18(8)
O2 As2 O3 2_656 . 178.56(7)
As1 O2 As2 . 2_656 118.33(9)
As1 O3 As2 . . 117.10(9)
As1 O4 As2 1_655 . 131.55(10)
As2 O6 As2 . 2_656 97.60(8)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
As1 O1 . 1.657(2)
As1 O2 . 1.6994(17)
As1 O3 . 1.7024(16)
As1 O4 1_455 1.7043(18)
As2 O5 . 1.7474(18)
As2 O6 . 1.8116(17)
As2 O6 2_656 1.8208(17)
As2 O4 . 1.8281(17)
As2 O2 2_656 1.8618(18)
As2 O3 . 1.9119(18)
Rb1 O2 2 2.9264(18)
Rb1 O2 . 2.9264(18)
Rb1 O5 2_556 2.948(2)
Rb1 O5 1_554 2.948(2)
Rb1 O1 1_545 3.000(2)
Rb1 O1 2_565 3.000(2)
Rb1 O6 1_455 3.1878(19)
Rb1 O6 2_655 3.1878(19)
Rb1 O5 2_656 3.288(2)
Rb1 O5 1_454 3.288(2)
O1 Rb1 1_565 3.000(2)
O1 H2 . 0.901(10)
O2 As2 2_656 1.8618(18)
O4 As1 1_655 1.7043(18)
O5 Rb1 1_556 2.948(2)
O5 Rb1 1_656 3.288(2)
O5 H1 . 0.852(19)
O6 As2 2_656 1.8208(17)
O6 Rb1 1_655 3.1878(19)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O5 H1 O3 2_666 0.852(19) 1.98(2) 2.822(3) 169(4)
O1 H2 O1 2_565 0.901(10) 1.58(3) 2.453(4) 161(8)
