##############################################################################
#                                                                            #
# This CIF contains the data in a paper accepted for publication in          #
# Acta Crystallographica Section E. It conforms to the requirements of       #
# Notes for Authors for Acta Crystallographica Section E, and has been       #
# peer reviewed under the auspices of the IUCr Commission on Journals.       #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic.                                       #
#                                                                            #
# Software is freely available for graphical display of the structure(s)     #
# in this CIF. For information consult the CIF software page                 #
# http://www.iucr.org/resources/cif/software.                                #
#                                                                            #
# This file may be used for bona fide research purposes within the           #
# scientific community so long as proper attribution is given to the journal # 
# article from which it was obtained.                                        #
#                                                                            #
##############################################################################
data_I
_audit_creation_method     SHELXL-97
_chemical_name_systematic
;
Magnesium hydroxide hydrogenarsenate (6.75/3/4)
;
_chemical_name_common     ?
_chemical_formula_moiety     ?
_chemical_formula_sum     'As4 H4.50 Mg6.75 O19'
_chemical_formula_structural     'Mg6.75 (O H)3 (H0.166 As O4)3 (H As O4)'
_chemical_formula_iupac     'Mg6.75 (O H)3 (H0.166 As O4)3 (H As O4)'
_chemical_formula_weight     772.31
_chemical_melting_point     ?
_symmetry_cell_setting     hexagonal
_symmetry_space_group_name_H-M     'P 63 m c'
_symmetry_space_group_name_Hall     'P 6c -2c'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-y, x-y, z'
    '-x+y, -x, z'
    '-x, -y, z+1/2'
    'y, -x+y, z+1/2'
    'x-y, x, z+1/2'
    '-y, -x, z'
    '-x+y, y, z'
    'x, x-y, z'
    'y, x, z+1/2'
    'x-y, -y, z+1/2'
    '-x, -x+y, z+1/2'
_cell_length_a     12.7651(3)
_cell_length_b     12.7651(3)
_cell_length_c     5.08440(10)
_cell_angle_alpha     90.00
_cell_angle_beta     90.00
_cell_angle_gamma     120.00
_cell_volume     717.49(3)
_cell_formula_units_Z     2
_cell_measurement_reflns_used     5443
_cell_measurement_theta_min     6.192
_cell_measurement_theta_max     34.407
_cell_measurement_temperature     296(2)
_exptl_crystal_description     'needle'
_exptl_crystal_colour     'colourless'
_exptl_crystal_size_max     0.30
_exptl_crystal_size_mid     0.02
_exptl_crystal_size_min     0.02
_exptl_crystal_density_diffrn     3.575
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     739
_exptl_absorpt_coefficient_mu     9.649
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details     '(SADABS; Bruker, 2008)'
_exptl_absorpt_correction_T_min     0.1599
_exptl_absorpt_correction_T_max     0.8304
_exptl_special_details     ?
_diffrn_ambient_temperature     296(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Bruker APEXII CCD'
_diffrn_measurement_method     'ω and φ scans'
_diffrn_detector_area_resol_mean     ?
_diffrn_reflns_number     21473
_diffrn_reflns_av_R_equivalents     0.0511
_diffrn_reflns_av_sigmaI/netI     0.0269
_diffrn_reflns_theta_min     1.84
_diffrn_reflns_theta_max     36.21
_diffrn_reflns_theta_full     36.21
_diffrn_measured_fraction_theta_max     1.000
_diffrn_measured_fraction_theta_full     1.000
_diffrn_reflns_limit_h_min     -21
_diffrn_reflns_limit_h_max     21
_diffrn_reflns_limit_k_min     -21
_diffrn_reflns_limit_k_max     21
_diffrn_reflns_limit_l_min     -5
_diffrn_reflns_limit_l_max     8
_diffrn_standards_number     0
_diffrn_standards_interval_count     .
_diffrn_standards_interval_time     .
_diffrn_standards_decay_%     ?
_refine_special_details
;
Refinement of F² against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F², conventional
R-factors R are based on F, with F set to zero for
negative F². The threshold expression of F² >
σ(F²) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F² are statistically about twice as large
as those based on F, and R- factors based on ALL data will be
even larger.
;
_reflns_number_total     1144
_reflns_number_gt     1066
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0329
_refine_ls_R_factor_gt     0.0291
_refine_ls_wR_factor_gt     0.0568
_refine_ls_wR_factor_ref     0.0575
_refine_ls_goodness_of_fit_ref     1.205
_refine_ls_restrained_S_all     1.205
_refine_ls_number_reflns     1144
_refine_ls_number_parameters     60
_refine_ls_number_restraints     1
_refine_ls_hydrogen_treatment     noref
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
              'w=1/[σ²(Fo²)+(0.0061P)²+2.8884P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     .
_atom_sites_solution_primary     isomor
_atom_sites_solution_secondary     .
_refine_ls_shift/su_max     0.000
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     1.308
_refine_diff_density_min     -2.164
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_extinction_coef     0.0015(4)
_refine_ls_extinction_expression
                                  'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_abs_structure_details     'Flack (1983), 446 Friedel pairs'
_refine_ls_abs_structure_Flack     0.022(16)
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'
    'Mg' 'Mg' 0.0486 0.0363
                         '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'
    'H' 'H' 0.0000 0.0000
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'APEX2 (Bruker, 2008)'
_computing_cell_refinement     'SAINT (Bruker, 2008)'
_computing_data_reduction     'SAINT (Bruker, 2008)'
_computing_structure_solution     'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement     'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics     'ATOMS for Windows (Dowty, 2006)'
_computing_publication_material     'publCIF (Westrip, 2010)'
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_symmetry_multiplicity
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    Mg Mg1 0.0000 0.0000 0.8698(12) 0.0227(15) Uani d SP 0.750(14) 6 . .
    Mg Mg2 0.65062(9) 0.57400(10) 0.5491(3) 0.0085(2) Uani d . 1 1 . .
    As As1 0.69764(4) 0.848821(19) 0.57265(9) 0.00778(9) Uani d S 1 2 . .
    As As2 0.6667 0.3333 0.78398(17) 0.00550(14) Uani d S 1 6 . .
    O O1 0.8487(3) 0.92434(17) 0.6201(9) 0.0257(10) Uani d S 1 2 . .
    O O2 0.6564(2) 0.7229(2) 0.3969(5) 0.0100(4) Uani d . 1 1 . .
    O O3 0.6168(3) 0.80839(17) 0.8561(7) 0.0115(6) Uani d S 1 2 . .
    O O4 0.52447(15) 0.47553(15) 0.2427(7) 0.0091(6) Uani d S 1 2 . .
    O O5 0.59609(16) 0.40391(16) 0.6823(8) 0.0173(8) Uani d S 1 2 . .
    O O6 0.3333 0.6667 0.6202(15) 0.0319(19) Uani d S 1 6 . .
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
    Mg1 0.0120(13) 0.0120(13) 0.044(4) 0.0060(6) 0.000 0.000
    Mg2 0.0103(4) 0.0092(4) 0.0073(5) 0.0059(3) -0.0005(4) 0.0001(4)
    As1 0.01061(18) 0.00811(12) 0.00544(16) 0.00530(9) -0.0004(2) -0.00021(10)
    As2 0.00468(17) 0.00468(17) 0.0071(3) 0.00234(9) 0.000 0.000
    O1 0.0089(14) 0.0320(17) 0.029(3) 0.0044(7) -0.0038(16) -0.0019(8)
    O2 0.0141(10) 0.0099(9) 0.0072(10) 0.0070(8) -0.0016(8) -0.0015(8)
    O3 0.0188(16) 0.0110(10) 0.0074(14) 0.0094(8) 0.0073(12) 0.0036(6)
    O4 0.0099(10) 0.0099(10) 0.0082(14) 0.0053(11) 0.0009(5) -0.0009(5)
    O5 0.0099(10) 0.0099(10) 0.034(2) 0.0065(12) -0.0037(7) 0.0037(7)
    O6 0.042(3) 0.042(3) 0.011(4) 0.0212(15) 0.000 0.000
_geom_special_details
;
All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes.
;
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
    Mg1 O1 1_445 2.100(5) y
    Mg1 O1 2_655 2.100(5) ?
    Mg1 O1 3_565 2.100(5) ?
    Mg1 O1 4_665 2.102(5) y
    Mg1 O1 5_455 2.102(5) ?
    Mg1 O1 6_545 2.102(5) ?
    Mg1 Mg1 4 2.54220(10)
                        y
    Mg1 Mg1 4_554 2.54220(10)
                            ?
    Mg2 O2 . 2.018(3) y
    Mg2 O2 10 2.029(3) y
    Mg2 O5 . 2.036(3) y
    Mg2 O3 6_654 2.053(2) y
    Mg2 O4 . 2.139(3) y
    Mg2 O4 4_665 2.225(3) y
    As1 O2 . 1.678(2) y
    As1 O2 9_565 1.678(2) ?
    As1 O1 . 1.687(4) y
    As1 O3 . 1.696(3) y
    As2 O5 2_655 1.644(3) ?
    As2 O5 3_665 1.644(3) ?
    As2 O5 . 1.644(3) y
    As2 O6 4_665 1.710(8) y
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 Mg1 O1 1_445 2_655 87.2(2) ?
    O1 Mg1 O1 1_445 3_565 87.2(2) ?
    O1 Mg1 O1 2_655 3_565 87.2(2) ?
    O1 Mg1 O1 1_445 4_665 179.9(3) ?
    O1 Mg1 O1 2_655 4_665 92.81(9) ?
    O1 Mg1 O1 3_565 4_665 92.81(9) ?
    O1 Mg1 O1 1_445 5_455 92.81(9) ?
    O1 Mg1 O1 2_655 5_455 179.9(3) ?
    O1 Mg1 O1 3_565 5_455 92.81(9) ?
    O1 Mg1 O1 4_665 5_455 87.1(2) ?
    O1 Mg1 O1 1_445 6_545 92.81(9) ?
    O1 Mg1 O1 2_655 6_545 92.81(9) ?
    O1 Mg1 O1 3_565 6_545 179.9(3) ?
    O1 Mg1 O1 4_665 6_545 87.1(2) ?
    O1 Mg1 O1 5_455 6_545 87.1(2) ?
    O2 Mg2 O2 . 10 93.03(10) ?
    O2 Mg2 O5 . . 164.45(12) ?
    O2 Mg2 O5 10 . 95.00(14) ?
    O2 Mg2 O3 . 6_654 89.84(12) ?
    O2 Mg2 O3 10 6_654 98.49(13) ?
    O5 Mg2 O3 . 6_654 102.09(14) ?
    O2 Mg2 O4 . . 86.36(11) ?
    O2 Mg2 O4 10 . 162.38(12) ?
    O5 Mg2 O4 . . 81.96(12) ?
    O3 Mg2 O4 6_654 . 99.12(14) ?
    O2 Mg2 O4 . 4_665 89.76(11) ?
    O2 Mg2 O4 10 4_665 83.86(11) ?
    O5 Mg2 O4 . 4_665 77.91(13) ?
    O3 Mg2 O4 6_654 4_665 177.63(15) ?
    O4 Mg2 O4 . 4_665 78.53(7) ?
    O2 As1 O2 . 9_565 106.56(16) ?
    O2 As1 O1 . . 110.19(12) ?
    O2 As1 O1 9_565 . 110.19(12) ?
    O2 As1 O3 . . 108.02(11) ?
    O2 As1 O3 9_565 . 108.02(11) ?
    O1 As1 O3 . . 113.6(2) ?
    O5 As2 O5 2_655 3_665 110.58(15) ?
    O5 As2 O5 2_655 . 110.58(15) ?
    O5 As2 O5 3_665 . 110.58(15) ?
    O5 As2 O6 2_655 4_665 108.33(15) ?
    O5 As2 O6 3_665 4_665 108.33(15) ?
    O5 As2 O6 . 4_665 108.33(15) ?
    As1 O1 Mg1 . 1_665 151.0(3) ?
    As1 O1 Mg1 . 4_664 134.5(3) ?
    Mg1 O1 Mg1 1_665 4_664 74.46(12) ?
    As1 O2 Mg2 . . 122.99(14) ?
    As1 O2 Mg2 . 10_554 137.98(14) ?
    Mg2 O2 Mg2 . 10_554 98.03(11) ?
    As1 O3 Mg2 . 10 121.83(9) ?
    As1 O3 Mg2 . 5_565 121.83(9) ?
    Mg2 O3 Mg2 10 5_565 115.94(18) ?
    Mg2 O4 Mg2 . 7_665 84.17(14) ?
    Mg2 O4 Mg2 . 4_664 147.49(17) ?
    Mg2 O4 Mg2 7_665 4_664 88.83(7) ?
    Mg2 O4 Mg2 . 10_554 88.83(7) ?
    Mg2 O4 Mg2 7_665 10_554 147.49(17) ?
    Mg2 O4 Mg2 4_664 10_554 80.23(13) ?
    As2 O5 Mg2 . 7_665 134.44(9) ?
    As2 O5 Mg2 . . 134.44(9) ?
    Mg2 O5 Mg2 7_665 . 89.51(15) ?
_iucr_refine_instructions_details
;
TITL MgAsOH
CELL 0.71073  12.7651  12.7651   5.0844  90.000  90.000 120.000
ZERR    2.00   0.0003   0.0003   0.0001   0.000   0.000   0.000
LATT -1
SYMM -Y, X-Y, Z
SYMM -X+Y, -X, Z
SYMM -X, -Y, 0.5+Z
SYMM Y, -X+Y, 0.5+Z
SYMM X-Y, X, 0.5+Z
SYMM -Y, -X, Z
SYMM -X+Y, Y, Z
SYMM X, X-Y, Z
SYMM Y, X, 0.5+Z
SYMM X-Y, -Y, 0.5+Z
SYMM -X, -X+Y, 0.5+Z
SFAC O MG AS H
UNIT 38 13.5 8 9
TEMP 23.000
L.S. 4
BOND
FMAP 2
PLAN 20
acta
size 0.3 0.02 0.02
WGHT    0.006100    2.888400
EXTI    0.001188
FVAR       0.13665
AS1   3    0.697644    0.848822    0.572278    10.50000    0.01049    0.00794 =
         0.00530   -0.00019   -0.00037    0.00524
AS2   3    0.666667    0.333333    0.783596    10.16667    0.00463    0.00463 =
         0.00706    0.00000    0.00000    0.00231
MG1   2    0.000000    0.000000    0.871908     0.12318    0.01180    0.01180 =
         0.04487    0.00000    0.00000    0.00590
MG2   2    0.650557    0.574021    0.550725    11.00000    0.00992    0.00875 =
         0.00830   -0.00015   -0.00027    0.00570
O1    1    0.849020    0.924510    0.622726    10.50000    0.01087    0.03226 =
         0.02734   -0.00141   -0.00282    0.00543
O2    1    0.656126    0.722681    0.399257    11.00000    0.01458    0.00994 =
         0.00638   -0.00132   -0.00127    0.00698
O3    1    0.616560    0.808280    0.858345    10.50000    0.01762    0.01147 =
         0.00820    0.00400    0.00799    0.00881
O4    1    0.524340    0.475660    0.244762    10.50000    0.01010    0.01010 =
         0.00883   -0.00129    0.00129    0.00533
O5    1    0.596145    0.403855    0.685383    10.50000    0.00980    0.00980 =
         0.03212    0.00340   -0.00340    0.00628
O6    1    0.333333    0.666667    0.620361    10.16667    0.04602    0.04602 =
         0.01067    0.00000    0.00000    0.02301
HKLF 4
REM  mw_mghgdesclo2_0m in P6(3)mc
REM R1 =  0.0310 for    656 Fo > 4sig(Fo)  and  0.0340 for all    698 data
REM     60 parameters refined using      0 restraints
END
WGHT      0.0000      4.9215
REM Highest difference peak  1.662,  deepest hole -2.376,  1-sigma level  0.221
Q1    1   0.6667  0.3333  0.5607  10.16667  0.05    1.66
Q2    1   0.6414  0.3586  0.5794  10.50000  0.05    1.18
Q3    1   0.5184  0.4816  0.3760  10.50000  0.05    0.99
Q4    1   0.8852  0.9426  0.7225  10.50000  0.05    0.98
Q5    1   0.6304  0.2607  0.7620  10.50000  0.05    0.92
Q6    1   0.8348  0.8775  0.5706  11.00000  0.05    0.90
Q7    1   0.5997  0.4003  0.8177  10.50000  0.05    0.84
Q8    1   0.6230  0.7645  0.7672  11.00000  0.05    0.82
Q9    1   0.0250  0.0499  1.0811  10.50000  0.05    0.79
Q10   1   0.7761  0.8881  0.5475  10.50000  0.05    0.77
Q11   1   0.6153  0.3076  0.9377  10.50000  0.05    0.74
Q12   1   0.4908  0.5092  0.2759  10.50000  0.05    0.72
Q13   1   0.5850  0.3288  0.5863  11.00000  0.05    0.71
Q14   1   0.5549  0.4451  0.1551  10.50000  0.05    0.70
Q15   1   0.7177  0.8131  0.7734  11.00000  0.05    0.70
Q16   1   0.5650  0.4350  0.2795  10.50000  0.05    0.70
Q17   1   0.5562  0.4438  0.9273  10.50000  0.05    0.69
Q18   1   0.8761  0.9380  0.4056  10.50000  0.05    0.68
Q19   1  -0.0667 -0.0588  0.9402  11.00000  0.05    0.68
Q20   1   0.7675  0.7799  0.5716  11.00000  0.05    0.67
;
data_global
_journal_date_recd_electronic     2013-04-18
_journal_date_accepted     2013-04-19
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2013
_journal_volume     69
_journal_issue      5
_journal_page_first     i29
_journal_page_last     i29
_journal_paper_category     QI
_journal_paper_doi     10.1107/S1600536813010714
_journal_coeditor_code     VN2069
_publ_contact_author_name
;
Matthias Weil
;
_publ_contact_author_address
;
Institute for Chemical Technologies and Analytics
Division of Structural Chemistry
Vienna University of Technology
Getreidemarkt 9/164-SC
A-1060 Vienna
Austria
;
_publ_contact_author_email     'mweil@mail.zserv.tuwien.ac.at'
_publ_contact_author_fax     '+43 1 58801 17199'
_publ_contact_author_phone     '+43 1 58801 17122'
_publ_section_title
;
Mg~6.75~(OH)₃(H~0.166~AsO₄)₃(HAsO₄), a member of the
M₁₋ₓM'₆(OH)₃(H₂ₓ~/3~AsO₄)₃(HAsO₄)
family (M,M' = Co; Ni)
;
loop_
    _publ_author_name
    _publ_author_address
    'Weil, Matthias'
;
Institute for Chemical Technologies and Analytics
Division of Structural Chemistry
Vienna University of Technology
Getreidemarkt 9/164-SC
A-1060 Vienna
Austria
;
