#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/92/2229259.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_2229259
loop_
_publ_author_name
'Li, Bao'
'Ye, Ling'
'Wu, Li-Xin'
_publ_section_title
;
 [Al(H₂O)₆][Cr(OH)₆Mo₆O₁₈]·10H₂O
;
_journal_coeditor_code           WM2434
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i8
_journal_paper_doi               10.1107/S1600536810053936
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Al(H2 O)6] [Cr (O H)6 Mo6 O18], 10H2 O'
_chemical_formula_moiety         'Al H12 O6 3+, Cr H6 Mo6 O24 3-, 10(H2 O) '
_chemical_formula_structural     '[Al(H2 O)6] [Cr (O H)6 Mo6 O18] 10(H2 O)'
_chemical_formula_sum            'Al Cr H38 Mo6 O40'
_chemical_formula_weight         1332.92
_chemical_name_systematic
;
hexaaquaaluminium hexahydroxidooctadecaoxidomolybdochromate(III) decahydrate,
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                101.26(3)
_cell_angle_beta                 97.02(3)
_cell_angle_gamma                101.81(3)
_cell_formula_units_Z            1
_cell_length_a                   6.809(5)
_cell_length_b                   11.267(7)
_cell_length_c                   11.596(9)
_cell_measurement_reflns_used    7543
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      27.06
_cell_measurement_theta_min      3.24
_cell_volume                     841.7(11)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2002)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      290(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_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  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0510
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8257
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.23
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.629
_exptl_absorpt_correction_T_max  0.7698
_exptl_absorpt_correction_T_min  0.7449
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.630
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             647
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.887
_refine_diff_density_min         -0.856
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3801
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0331P)²+2.7190P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0929
_reflns_number_gt                3346
_reflns_number_total             3801
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            wm2434.cif
_cod_data_source_block           I
_cod_original_cell_volume        841.7(10)
_cod_database_code               2229259
_cod_database_fobs_code          2229259
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Al Al1 0.0000 0.5000 0.5000 0.0162(4) Uani d S 1 . .
Cr Cr1 0.0000 0.0000 0.0000 0.01424(19) Uani d S 1 . .
Mo Mo1 0.37029(5) 0.16663(3) -0.10502(3) 0.01629(11) Uani d . 1 . .
Mo Mo2 0.33617(6) 0.24360(3) 0.17992(3) 0.01870(11) Uani d . 1 . .
Mo Mo3 -0.02648(6) 0.07285(3) 0.29050(3) 0.01802(11) Uani d . 1 . .
O OH1 0.2099(4) -0.0332(3) -0.0983(3) 0.0156(6) Uani d D 1 . .
H H1 0.2955 -0.0782 -0.0941 0.023 Uiso d RD 1 . .
O OB1 0.1450(5) 0.1055(3) -0.2357(3) 0.0203(6) Uani d . 1 . .
O OT1 0.5602(5) 0.1125(3) -0.1683(3) 0.0251(7) Uani d . 1 . .
O OT2 0.4158(5) 0.3199(3) -0.1095(3) 0.0287(8) Uani d . 1 . .
O OH2 0.1174(4) 0.1756(3) 0.0024(3) 0.0159(6) Uani d D 1 . .
H H2 0.0530 0.2258 -0.0217 0.024 Uiso d RD 1 . .
O OB2 0.4843(5) 0.1784(3) 0.0594(3) 0.0209(6) Uani d . 1 . .
O OT3 0.3656(6) 0.3945(3) 0.1671(3) 0.0321(8) Uani d . 1 . .
O OT4 0.5053(6) 0.2483(4) 0.3027(3) 0.0365(9) Uani d . 1 . .
O OB3 0.0878(5) 0.2295(3) 0.2494(3) 0.0202(6) Uani d . 1 . .
O OH3 0.1830(5) 0.0372(3) 0.1527(3) 0.0166(6) Uani d D 1 . .
H H3 0.2705 -0.0068 0.1480 0.025 Uiso d RD 1 . .
O OT5 0.1586(6) 0.0662(3) 0.3999(3) 0.0315(8) Uani d . 1 . .
O OT6 -0.2117(6) 0.1163(4) 0.3617(3) 0.0334(8) Uani d . 1 . .
O OW1 0.1050(5) 0.3690(3) 0.5388(3) 0.0242(7) Uani d . 1 . .
H H4 0.2073 0.3992 0.5942 0.036 Uiso d R 1 . .
H H5 0.0411 0.3152 0.5715 0.036 Uiso d R 1 . .
O OW2 0.0105(5) 0.5686(3) 0.6627(3) 0.0234(7) Uani d D 1 . .
H H6 -0.0143 0.6394 0.6869 0.035 Uiso d RD 1 . .
H H7 0.0689 0.5534 0.7255 0.035 Uiso d RD 1 . .
O OW3 0.2655(5) 0.5935(3) 0.5085(3) 0.0254(7) Uani d D 1 . .
H H8 0.3070 0.6445 0.5758 0.038 Uiso d RD 1 . .
H H9 0.3240 0.6029 0.4491 0.038 Uiso d RD 1 . .
O OW4 0.9017(6) 0.2342(3) 0.6599(4) 0.0379(9) Uani d D 1 . .
H H10 0.9862 0.2141 0.7084 0.057 Uiso d RD 1 . .
H H11 0.8043 0.2487 0.6955 0.057 Uiso d RD 1 . .
O OW5 0.0885(6) 0.6667(3) 0.0685(4) 0.0361(9) Uani d D 1 . .
H H12 0.1879 0.7302 0.0967 0.054 Uiso d RD 1 . .
H H13 0.1180 0.6225 0.0079 0.054 Uiso d RD 1 . .
O OW6 0.1882(6) 0.5186(4) 0.8662(4) 0.0378(9) Uani d D 1 . .
H H14 0.1337 0.4753 0.9112 0.057 Uiso d RD 1 . .
H H15 0.3078 0.5567 0.9018 0.057 Uiso d RD 1 . .
O OW7 0.4894(4) 0.3814(3) 0.6484(3) 0.0359(9) Uani d D 1 . .
H H16 0.5251 0.4239 0.7199 0.054 Uiso d RD 1 . .
H H17 0.4701 0.3052 0.6506 0.054 Uiso d RD 1 . .
O OW8 0.4860(4) 0.1318(3) 0.5850(3) 0.0407(9) Uani d D 1 . .
H H18 0.4573 0.0970 0.6416 0.061 Uiso d RD 1 . .
H H19 0.5475 0.0869 0.5416 0.061 Uiso d RD 1 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 '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'
Mo Mo -1.6832 0.6857 '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'
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
OW1 Al1 OW1 2_566 . 180.0000(10) ?
OW1 Al1 OW3 2_566 2_566 89.98(16) ?
OW1 Al1 OW3 . 2_566 90.02(16) ?
OW1 Al1 OW3 2_566 . 90.02(16) ?
OW1 Al1 OW3 . . 89.98(16) ?
OW3 Al1 OW3 2_566 . 180.0(2) ?
OW1 Al1 OW2 2_566 . 89.59(15) ?
OW1 Al1 OW2 . . 90.41(15) ?
OW3 Al1 OW2 2_566 . 90.13(15) ?
OW3 Al1 OW2 . . 89.87(15) ?
OW1 Al1 OW2 2_566 2_566 90.41(15) ?
OW1 Al1 OW2 . 2_566 89.59(15) ?
OW3 Al1 OW2 2_566 2_566 89.87(15) ?
OW3 Al1 OW2 . 2_566 90.13(15) ?
OW2 Al1 OW2 . 2_566 180.0000(10) ?
OH3 Cr1 OH3 2 . 180.00(18) ?
OH3 Cr1 OH2 2 . 96.53(13) ?
OH3 Cr1 OH2 . . 83.47(13) ?
OH3 Cr1 OH2 2 2 83.47(13) ?
OH3 Cr1 OH2 . 2 96.53(13) ?
OH2 Cr1 OH2 . 2 180.00(18) ?
OH3 Cr1 OH1 2 2 94.97(14) ?
OH3 Cr1 OH1 . 2 85.03(14) ?
OH2 Cr1 OH1 . 2 95.90(12) ?
OH2 Cr1 OH1 2 2 84.10(12) ?
OH3 Cr1 OH1 2 . 85.03(14) ?
OH3 Cr1 OH1 . . 94.97(14) ?
OH2 Cr1 OH1 . . 84.10(12) ?
OH2 Cr1 OH1 2 . 95.90(12) ?
OH1 Cr1 OH1 2 . 180.00(15) ?
OT2 Mo1 OT1 . . 104.94(17) ?
OT2 Mo1 OB1 . . 97.87(16) ?
OT1 Mo1 OB1 . . 101.08(16) ?
OT2 Mo1 OB2 . . 100.85(16) ?
OT1 Mo1 OB2 . . 96.87(16) ?
OB1 Mo1 OB2 . . 149.69(14) ?
OT2 Mo1 OH2 . . 94.45(14) ?
OT1 Mo1 OH2 . . 159.55(14) ?
OB1 Mo1 OH2 . . 82.26(14) ?
OB2 Mo1 OH2 . . 72.74(13) ?
OT2 Mo1 OH1 . . 162.67(14) ?
OT1 Mo1 OH1 . . 90.85(14) ?
OB1 Mo1 OH1 . . 71.64(12) ?
OB2 Mo1 OH1 . . 83.95(13) ?
OH2 Mo1 OH1 . . 70.89(11) ?
OT4 Mo2 OT3 . . 105.5(2) ?
OT4 Mo2 OB2 . . 98.10(17) ?
OT3 Mo2 OB2 . . 101.59(16) ?
OT4 Mo2 OB3 . . 99.29(18) ?
OT3 Mo2 OB3 . . 97.85(16) ?
OB2 Mo2 OB3 . . 149.30(13) ?
OT4 Mo2 OH2 . . 162.45(15) ?
OT3 Mo2 OH2 . . 90.88(16) ?
OB2 Mo2 OH2 . . 72.01(13) ?
OB3 Mo2 OH2 . . 84.24(13) ?
OT4 Mo2 OH3 . . 94.98(16) ?
OT3 Mo2 OH3 . . 158.26(16) ?
OB2 Mo2 OH3 . . 82.20(13) ?
OB3 Mo2 OH3 . . 71.27(12) ?
OH2 Mo2 OH3 . . 69.73(11) ?
OT6 Mo3 OT5 . . 105.4(2) ?
OT6 Mo3 OB1 . 2 99.75(17) ?
OT5 Mo3 OB1 . 2 97.91(16) ?
OT6 Mo3 OB3 . . 99.14(17) ?
OT5 Mo3 OB3 . . 102.04(17) ?
OB1 Mo3 OB3 2 . 147.66(13) ?
OT6 Mo3 OH3 . . 163.68(15) ?
OT5 Mo3 OH3 . . 89.62(16) ?
OB1 Mo3 OH3 2 . 84.03(12) ?
OB3 Mo3 OH3 . . 71.00(12) ?
OT6 Mo3 OH1 . 2 95.90(16) ?
OT5 Mo3 OH1 . 2 157.46(14) ?
OB1 Mo3 OH1 2 2 70.90(12) ?
OB3 Mo3 OH1 . 2 81.26(13) ?
OH3 Mo3 OH1 . 2 70.18(12) ?
Cr1 OH1 Mo1 . . 101.22(12) ?
Cr1 OH1 Mo3 . 2 101.37(13) ?
Mo1 OH1 Mo3 . 2 92.79(11) ?
Cr1 OH1 H1 . . 131.8 ?
Mo1 OH1 H1 . . 110.7 ?
Mo3 OH1 H1 2 . 111.9 ?
Mo1 OB1 Mo3 . 2 120.22(16) ?
Cr1 OH2 Mo1 . . 103.79(12) ?
Cr1 OH2 Mo2 . . 103.22(13) ?
Mo1 OH2 Mo2 . . 93.30(12) ?
Cr1 OH2 H2 . . 125.8 ?
Mo1 OH2 H2 . . 106.7 ?
Mo2 OH2 H2 . . 118.4 ?
Mo1 OB2 Mo2 . . 116.61(16) ?
Mo2 OB3 Mo3 . . 118.42(15) ?
Cr1 OH3 Mo2 . . 103.55(13) ?
Cr1 OH3 Mo3 . . 103.34(14) ?
Mo2 OH3 Mo3 . . 93.88(11) ?
Cr1 OH3 H3 . . 110.0 ?
Mo2 OH3 H3 . . 110.7 ?
Mo3 OH3 H3 . . 131.6 ?
Al1 OW1 H4 . . 108.5 ?
Al1 OW1 H5 . . 122.9 ?
H4 OW1 H5 . . 97.7 ?
Al1 OW2 H6 . . 122.0 ?
Al1 OW2 H7 . . 131.7 ?
H6 OW2 H7 . . 103.9 ?
Al1 OW3 H8 . . 111.0 ?
Al1 OW3 H9 . . 125.4 ?
H8 OW3 H9 . . 120.8 ?
H10 OW4 H11 . . 107.7 ?
H12 OW5 H13 . . 108.5 ?
H14 OW6 H15 . . 107.7 ?
H16 OW7 H17 . . 107.5 ?
H18 OW8 H19 . . 107.7 ?
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
Al1 OW1 2_566 1.872(3) ?
Al1 OW1 . 1.872(3) ?
Al1 OW3 2_566 1.877(3) ?
Al1 OW3 . 1.877(3) ?
Al1 OW2 . 1.881(3) ?
Al1 OW2 2_566 1.881(3) ?
Cr1 OH3 2 1.954(3) ?
Cr1 OH3 . 1.954(3) ?
Cr1 OH2 . 1.970(3) ?
Cr1 OH2 2 1.970(3) ?
Cr1 OH1 2 1.983(3) ?
Cr1 OH1 . 1.983(3) ?
Mo1 OT2 . 1.703(3) ?
Mo1 OT1 . 1.721(3) ?
Mo1 OB1 . 1.927(3) ?
Mo1 OB2 . 1.937(4) ?
Mo1 OH2 . 2.252(3) ?
Mo1 OH1 . 2.314(3) ?
Mo2 OT4 . 1.703(4) ?
Mo2 OT3 . 1.709(4) ?
Mo2 OB2 . 1.939(3) ?
Mo2 OB3 . 1.951(3) ?
Mo2 OH2 . 2.283(3) ?
Mo2 OH3 . 2.288(3) ?
Mo3 OT6 . 1.691(4) ?
Mo3 OT5 . 1.699(4) ?
Mo3 OB1 2 1.951(3) ?
Mo3 OB3 . 1.951(3) ?
Mo3 OH3 . 2.300(3) ?
Mo3 OH1 2 2.330(3) ?
OH1 Mo3 2 2.330(3) ?
OH1 H1 . 0.8500 ?
OB1 Mo3 2 1.951(3) ?
OH2 H2 . 0.8499 ?
OH3 H3 . 0.8501 ?
OW1 H4 . 0.8500 ?
OW1 H5 . 0.8500 ?
OW2 H6 . 0.8501 ?
OW2 H7 . 0.8499 ?
OW3 H8 . 0.8500 ?
OW3 H9 . 0.8500 ?
OW4 H10 . 0.8500 ?
OW4 H11 . 0.8500 ?
OW5 H12 . 0.8559 ?
OW5 H13 . 0.8496 ?
OW6 H14 . 0.8500 ?
OW6 H15 . 0.8500 ?
OW7 H16 . 0.8509 ?
OW7 H17 . 0.8480 ?
OW8 H18 . 0.8499 ?
OW8 H19 . 0.8500 ?
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
OH3 H3 OT1 2_655 0.85 1.85 2.681(4) 166.8
OH1 H1 OB2 2_655 0.85 2.10 2.944(4) 172.4
OH2 H2 OW5 2_565 0.85 1.82 2.665(5) 178.1
OW3 H8 OT4 2_666 0.85 1.83 2.628(5) 156.2
OW3 H9 OW7 2_666 0.85 1.81 2.632(5) 163.4
OW1 H4 OW7 . 0.85 2.01 2.730(5) 142.1
OW1 H5 OW4 1_455 0.85 1.74 2.577(5) 167.2
OW2 H6 OB3 2_566 0.85 1.72 2.559(4) 170.5
OW2 H7 OW6 . 0.85 1.88 2.728(5) 177.8
OW4 H10 OB1 1_656 0.85 1.94 2.737(5) 155.5
OW5 H12 OT1 2_665 0.86 2.15 3.002(6) 179.1
OW5 H13 OW6 1_554 0.85 1.99 2.842(6) 179.8
OW6 H14 OW5 2_566 0.85 2.04 2.800(6) 149.2
OW6 H15 OT3 2_666 0.85 2.45 3.091(6) 133.0
OW7 H16 OT3 2_666 0.85 2.13 2.878(5) 146.0
OW7 H17 OW8 . 0.85 1.98 2.759(5) 151.6
OW8 H18 OT1 1_556 0.85 2.19 2.902(5) 140.9
OW8 H18 OT6 2_556 0.85 2.62 3.241(5) 130.7
OW8 H19 OW8 2_656 0.85 2.56 3.283(6) 143.5
