#------------------------------------------------------------------------------
#$Date: 2019-12-26 22:11:56 +0200 (Thu, 26 Dec 2019) $
#$Revision: 246154 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/18/2311888.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_2311888
loop_
_publ_author_name
'Schwendtner, Karolina'
'Kolitsch, Uwe'
_publ_section_title
;
 M³⁺(H₂AsO₄)(H₂As₂O₇)
 (M³⁺ = Al, Ga) and
 In₂(H₂AsO₄)₂(H₂As₂O₇)₂:
 a new layer structure type and a new framework structure type containing
 the rare H₂As₂O₇²⁻ group.
;
_journal_coeditor_code           LY3048
_journal_issue                   'Pt 8'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first              600
_journal_page_last               608
_journal_paper_doi               10.1107/S2053229617009676
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'In2 (H2 As1 O4)2 (H2 As2 O7)2'
_chemical_formula_structural     'In2 (H2 As1 O4)2 (H2 As2 O7)2'
_chemical_formula_sum            'As6 H8 In2 O22'
_chemical_formula_weight         1039.22
_chemical_name_common
'indum dihydrogen arsenate dihydrogen diarsenate'
_chemical_name_systematic
'Diindium bis[dihydrogen arsenate(V)] bis[dihydrogen diarsenate(V)]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 101.40(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.487(2)
_cell_length_b                   11.529(2)
_cell_length_c                   12.553(3)
_cell_measurement_reflns_used    6682
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.577
_cell_measurement_theta_min      2.037
_cell_volume                     1771.5(6)
_computing_cell_refinement
;
SCALEPACK (Otwinowski et al., 2003)
;
_computing_data_collection
;
COLLECT (Nonius, 2003)
;
_computing_data_reduction
;
DENZO and SCALEPACK (Otwinowski et al., 2003)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2005)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD single-crystal four-circle'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12567
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.581
_diffrn_reflns_theta_min         2.102
_exptl_absorpt_coefficient_mu    13.841
_exptl_absorpt_correction_T_max  0.6815
_exptl_absorpt_correction_T_min  0.4034
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SCALEPACK; Otwinowski et al., 2003)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.897
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocky
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.030
_refine_diff_density_max         2.135
_refine_diff_density_min         -1.678
_refine_ls_extinction_coef       0.00083(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2016 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.222
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         6428
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.222
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+19.0117P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0718
_reflns_number_gt                5562
_reflns_number_total             6428
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ly3048sup1.cif
_cod_data_source_block           In2H2AsO42H2As2O72
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2311888
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.404
_shelx_estimated_absorpt_t_max   0.682
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
In In1 0.74844(3) 1.00138(3) 0.73467(3) 0.00950(7) Uani d 1
In In2 0.73920(3) 0.98874(3) 0.23819(3) 0.00933(7) Uani d 1
As As1 0.77893(4) 0.60833(4) 0.51413(4) 0.01103(9) Uani d 1
As As2 0.77259(4) 0.88225(4) 0.49339(4) 0.01012(9) Uani d 1
As As3 0.99559(4) 0.60869(4) 0.21703(4) 0.01123(9) Uani d 1
As As4 0.99662(4) 0.88304(4) 0.22744(4) 0.00994(9) Uani d 1
As As5 0.89658(4) 0.75944(4) 0.83829(4) 0.01077(9) Uani d 1
As As6 0.66222(4) 0.72935(4) 0.10470(4) 0.01034(9) Uani d 1
O O1 0.7315(3) 0.6058(3) 0.3820(3) 0.0155(7) Uani d 1
O O2 0.7086(3) 0.5319(3) 0.5889(3) 0.0165(7) Uani d 1
O O3 0.9141(3) 0.5786(4) 0.5351(3) 0.0240(9) Uani d 1
O O4 0.7653(4) 0.7507(3) 0.5572(3) 0.0211(8) Uani d 1
O O5 0.7187(3) 0.8680(3) 0.3629(3) 0.0141(7) Uani d 1
O O6 0.7124(3) 0.9760(3) 0.5620(3) 0.0150(7) Uani d 1
O O7 0.9101(3) 0.9130(4) 0.5153(3) 0.0235(8) Uani d 1
O O8 1.1287(3) 0.6170(3) 0.2610(3) 0.0170(7) Uani d 1
O O9 0.9331(3) 0.5205(3) 0.2893(3) 0.0166(7) Uani d 1
O O10 0.9713(3) 0.5814(4) 0.0812(3) 0.0223(8) Uani d 1
O O11 0.9421(3) 0.7458(3) 0.2327(4) 0.0205(8) Uani d 1
O O12 0.9160(3) 0.9635(3) 0.2866(3) 0.0168(7) Uani d 1
O O13 1.1270(3) 0.8780(3) 0.2866(3) 0.0136(6) Uani d 1
O O14 0.9824(3) 0.9163(4) 0.0927(3) 0.0232(8) Uani d 1
O O15 0.8697(3) 0.6343(3) 0.7753(3) 0.0160(7) Uani d 1
O O16 0.8751(3) 0.8757(3) 0.7583(3) 0.0154(7) Uani d 1
O O17 1.0297(3) 0.7632(4) 0.9070(3) 0.0205(8) Uani d 1
O O18 0.8227(3) 0.7661(4) 0.9400(3) 0.0197(8) Uani d 1
O O19 0.7244(3) 0.8566(3) 0.1211(3) 0.0156(7) Uani d 1
O O20 0.7432(3) 0.6155(3) 0.1360(3) 0.0159(7) Uani d 1
O O21 0.5922(3) 0.7177(4) -0.0267(3) 0.0212(8) Uani d 1
O O22 0.5595(3) 0.7290(3) 0.1772(3) 0.0192(7) Uani d 1
H H3A 0.936(11) 0.560(12) 0.604(4) 0.02(4) Uiso d 0.5
H H3B 0.943(10) 0.512(6) 0.520(11) 0.02(3) Uiso d 0.5
H H7 0.941(6) 0.936(7) 0.464(6) 0.03(2) Uiso d 1
H H10A 1.000(11) 0.522(9) 0.051(10) 0.025 Uiso d 0.5
H H10B 0.906(6) 0.612(12) 0.083(12) 0.03(4) Uiso d 0.5
H H21 0.628(6) 0.702(7) -0.077(5) 0.03(2) Uiso d 1
H H22 0.529(5) 0.661(4) 0.172(6) 0.024(18) Uiso d 1
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'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In -0.7276 1.3100 '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'
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
O8 In1 O15 4_576 2_656 88.30(14)
O8 In1 O16 4_576 . 93.93(14)
O15 In1 O16 2_656 . 174.56(15)
O8 In1 O13 4_576 3_776 178.09(14)
O15 In1 O13 2_656 3_776 92.16(14)
O16 In1 O13 . 3_776 85.46(14)
O8 In1 O6 4_576 . 93.25(15)
O15 In1 O6 2_656 . 91.97(14)
O16 In1 O6 . . 92.87(14)
O13 In1 O6 3_776 . 88.58(14)
O8 In1 O2 4_576 2_656 89.12(15)
O15 In1 O2 2_656 2_656 88.41(14)
O16 In1 O2 . 2_656 86.66(14)
O13 In1 O2 3_776 2_656 89.04(14)
O6 In1 O2 . 2_656 177.61(15)
O19 In2 O1 . 2_655 88.12(14)
O19 In2 O20 . 2_655 176.74(15)
O1 In2 O20 2_655 2_655 94.84(14)
O19 In2 O9 . 2_655 93.69(14)
O1 In2 O9 2_655 2_655 94.94(15)
O20 In2 O9 2_655 2_655 87.44(14)
O19 In2 O5 . . 91.91(14)
O1 In2 O5 2_655 . 176.90(15)
O20 In2 O5 2_655 . 85.07(14)
O9 In2 O5 2_655 . 88.15(15)
O19 In2 O12 . . 92.45(14)
O1 In2 O12 2_655 . 88.59(15)
O20 In2 O12 2_655 . 86.25(14)
O9 In2 O12 2_655 . 173.01(14)
O5 In2 O12 . . 88.31(15)
O1 As1 O2 . . 115.77(19)
O1 As1 O3 . . 107.6(2)
O2 As1 O3 . . 115.3(2)
O1 As1 O4 . . 106.90(18)
O2 As1 O4 . . 103.23(19)
O3 As1 O4 . . 107.3(2)
O5 As2 O6 . . 116.35(18)
O5 As2 O7 . . 112.1(2)
O6 As2 O7 . . 108.9(2)
O5 As2 O4 . . 108.92(17)
O6 As2 O4 . . 105.14(19)
O7 As2 O4 . . 104.4(2)
O8 As3 O9 . . 113.89(19)
O8 As3 O10 . . 108.4(2)
O9 As3 O10 . . 115.2(2)
O8 As3 O11 . . 107.04(18)
O9 As3 O11 . . 105.20(19)
O10 As3 O11 . . 106.6(2)
O8 As3 H10B . . 134(3)
O9 As3 H10B . . 104(4)
O10 As3 H10B . . 29(2)
O11 As3 H10B . . 85(3)
O12 As4 O13 . . 116.89(18)
O12 As4 O14 . . 111.5(2)
O13 As4 O14 . . 110.69(19)
O12 As4 O11 . . 102.54(19)
O13 As4 O11 . . 108.15(18)
O14 As4 O11 . . 106.2(2)
O15 As5 O16 . . 115.00(19)
O15 As5 O17 . . 110.4(2)
O16 As5 O17 . . 107.88(19)
O15 As5 O18 . . 107.91(19)
O16 As5 O18 . . 111.48(19)
O17 As5 O18 . . 103.57(19)
O19 As6 O20 . . 115.11(19)
O19 As6 O21 . . 109.1(2)
O20 As6 O21 . . 109.8(2)
O19 As6 O22 . . 108.55(18)
O20 As6 O22 . . 110.97(19)
O21 As6 O22 . . 102.6(2)
As1 O1 In2 . 2_645 130.7(2)
As1 O2 In1 . 2_646 127.1(2)
As1 O3 H3A . . 108(9)
As1 O3 H3B . . 125(9)
H3A O3 H3B . . 86(10)
As2 O4 As1 . . 131.6(2)
As2 O5 In2 . . 125.06(19)
As2 O6 In1 . . 126.13(19)
As2 O7 H7 . . 122(5)
As3 O8 In1 . 4_675 127.7(2)
As3 O9 In2 . 2_645 125.7(2)
As3 O10 H10A . . 124(9)
As3 O10 H10B . . 83(9)
H10A O10 H10B . . 140(10)
As4 O11 As3 . . 131.6(2)
As4 O12 In2 . . 128.4(2)
As4 O13 In1 . 3_776 126.65(19)
As5 O15 In1 . 2_646 137.5(2)
As5 O16 In1 . . 131.3(2)
As6 O19 In2 . . 134.9(2)
As6 O20 In2 . 2_645 133.5(2)
As6 O21 H21 . . 119(5)
As6 O22 H22 . . 109(5)
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
In1 O8 4_576 2.098(4) y
In1 O15 2_656 2.114(4) y
In1 O16 . 2.122(4) y
In1 O13 3_776 2.142(3) y
In1 O6 . 2.145(4) y
In1 O2 2_656 2.201(4) y
In2 O19 . 2.099(4) y
In2 O1 2_655 2.110(3) y
In2 O20 2_655 2.130(4) y
In2 O9 2_655 2.143(4) y
In2 O5 . 2.148(3) y
In2 O12 . 2.190(4) y
As1 O1 . 1.648(3) y
As1 O2 . 1.660(4) y
As1 O3 . 1.691(4) y
As1 O4 . 1.747(4) y
As2 O5 . 1.651(3) y
As2 O6 . 1.653(3) y
As2 O7 . 1.721(4) y
As2 O4 . 1.726(4) y
As3 O8 . 1.648(4) y
As3 O9 . 1.657(4) y
As3 O10 . 1.701(4) y
As3 O11 . 1.743(4) y
As4 O12 . 1.650(4) y
As4 O13 . 1.651(3) y
As4 O14 . 1.709(4) y
As4 O11 . 1.728(4) y
As5 O15 . 1.647(4) y
As5 O16 . 1.664(4) y
As5 O17 . 1.715(4) y
As5 O18 . 1.718(4) y
As6 O19 . 1.654(4) y
As6 O20 . 1.657(4) y
As6 O21 . 1.712(4) y
As6 O22 . 1.714(4) y
O3 H3A . 0.88(4) ?
O3 H3B . 0.88(4) ?
O7 H7 . 0.86(8) ?
O10 H10A . 0.89(4) ?
O10 H10B . 0.89(4) ?
O21 H21 . 0.86(4) ?
O22 H22 . 0.87(4) ?
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
O3 H3A O9 3_766 0.88(4) 2.11(9) 2.853(6) 142(12)
O3 H3A O15 . 0.88(4) 2.60(11) 3.235(6) 130(11)
O3 H3B O3 3_766 0.88(4) 2.29(8) 3.069(9) 146(11)
O7 H7 O7 3_776 0.86(8) 2.52(8) 3.091(9) 125(6)
O7 H7 O12 . 0.86(8) 2.21(8) 2.944(6) 143(7)
O10 H10A O6 4_675 0.89(4) 2.62(13) 3.137(6) 118(11)
O10 H10A O10 3_765 0.89(4) 2.13(7) 2.961(8) 155(12)
O10 H10B O18 1_554 0.89(4) 2.59(13) 3.134(6) 120(11)
O10 H10B O20 . 0.89(4) 2.26(8) 3.085(6) 153(13)
O21 H21 O13 4_575 0.86(4) 1.95(5) 2.702(5) 147(7)
O21 H21 O18 1_554 0.86(4) 2.52(7) 3.041(6) 120(6)
O22 H22 O7 4_575 0.87(4) 2.38(6) 2.965(6) 125(6)
O22 H22 O12 2_645 0.87(4) 2.41(6) 3.100(6) 137(6)
O22 H22 O16 4_575 0.87(4) 2.42(6) 2.952(5) 120(6)
