#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/80/2238070.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_2238070
loop_
_publ_author_name
'Jouini, Raja'
'Zid, Mohamed Faouzi'
'Driss, Ahmed'
_publ_section_title
;
 K(MoO₂)₄O₃(AsO₄)
;
_journal_coeditor_code           VN2070
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i37
_journal_paper_doi               10.1107/S1600536813013664
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'K (Mo O2)4 O3 (As O4)'
_chemical_formula_moiety         'As Mo4 O15, K'
_chemical_formula_sum            'As K Mo4 O15'
_chemical_formula_weight         737.78
_chemical_name_systematic
;
Potassium tetrakis(dioxomolybdenum) arsenate trioxide
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.0442(8)
_cell_length_b                   11.9167(9)
_cell_length_c                   12.6799(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     1215.50(18)
_computing_cell_refinement
'CAD-4 EXPRESS (Duisenberg, 1992; Macíček & Yordanov, 1992)'
_computing_data_collection
'CAD-4 EXPRESS (Duisenberg, 1992; Macíček & Yordanov, 1992)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1998)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       ω/2θ
_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  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8046
_diffrn_reflns_theta_full        26.97
_diffrn_reflns_theta_max         26.97
_diffrn_reflns_theta_min         2.35
_diffrn_standards_decay_%        1.2
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    7.160
_exptl_absorpt_correction_T_max  0.212
_exptl_absorpt_correction_T_min  0.077
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.032
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.685
_refine_ls_abs_structure_details 'Flack (1983), 2399 Friedel pairs'
_refine_ls_abs_structure_Flack   0.089(10)
_refine_ls_extinction_coef       0.00488(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2647
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0181
_refine_ls_R_factor_gt           0.0177
_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)+(0.0195P)²+2.5252P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0450
_refine_ls_wR_factor_ref         0.0452
_reflns_number_gt                2611
_reflns_number_total             2647
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            vn2070.cif
_cod_data_source_block           I
_cod_database_code               2238070
_cod_database_fobs_code          2238070
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-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
Mo Mo1 0.99047(5) 0.41688(3) 0.61974(3) 0.01100(9) Uani d 1 1
Mo Mo2 0.78403(5) 0.64073(3) 0.90494(3) 0.00936(9) Uani d 1 1
Mo Mo3 0.19469(5) 0.63578(3) 0.92886(3) 0.00829(9) Uani d 1 1
Mo Mo4 0.46142(5) 0.71544(3) 0.68083(3) 0.01289(10) Uani d 1 1
As As1 0.56223(6) 0.43948(3) 0.65276(3) 0.00879(10) Uani d 1 1
K K1 0.9351(2) 0.75546(14) 0.60338(12) 0.0474(4) Uani d 1 1
O O1 0.7659(5) 0.5009(3) 0.9106(3) 0.0236(8) Uani d 1 1
O O2 0.4420(4) 0.5521(2) 0.6643(3) 0.0155(7) Uani d 1 1
O O3 0.3320(4) 0.6807(3) 0.8313(2) 0.0146(7) Uani d 1 1
O O4 0.6627(4) 0.6759(3) 0.7968(3) 0.0187(8) Uani d 1 1
O O5 0.4982(6) 0.8616(3) 0.7455(3) 0.0273(9) Uani d 1 1
O O6 0.7604(5) 0.4761(3) 0.6609(3) 0.0313(10) Uani d 1 1
O O7 0.2779(6) 0.7443(3) 0.6214(3) 0.0305(10) Uani d 1 1
O O8 0.6055(6) 0.7332(3) 0.5839(3) 0.0330(10) Uani d 1 1
O O9 0.2086(5) 0.4954(3) 0.9257(3) 0.0200(8) Uani d 1 1
O O10 0.9963(4) 0.6679(2) 0.8464(2) 0.0136(6) Uani d 1 1
O O11 0.8536(4) 0.3194(2) 0.5245(2) 0.0099(6) Uani d 1 1
O O12 0.1790(4) 0.3351(2) 0.5557(2) 0.0100(6) Uani d 1 1
O O13 0.5239(4) 0.3741(2) 0.5374(2) 0.0103(6) Uani d 1 1
O O14 0.0441(5) 0.3976(4) 0.7460(3) 0.0309(10) Uani d 1 1
O O15 0.0494(5) 0.5469(3) 0.5840(4) 0.0347(10) Uani d 1 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'
K K 0.2009 0.2494 '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'
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
O14 Mo1 O15 1_655 1_655 108.2(2)
O14 Mo1 O12 1_655 1_655 97.31(16)
O15 Mo1 O12 1_655 1_655 97.29(16)
O14 Mo1 O11 1_655 . 129.64(18)
O15 Mo1 O11 1_655 . 121.71(18)
O12 Mo1 O11 1_655 . 83.60(13)
O14 Mo1 O6 1_655 . 92.10(18)
O15 Mo1 O6 1_655 . 90.35(19)
O12 Mo1 O6 1_655 . 165.36(13)
O11 Mo1 O6 . . 81.76(14)
O1 Mo2 O4 . . 103.02(19)
O1 Mo2 O10 . . 105.44(17)
O4 Mo2 O10 . . 99.00(15)
O1 Mo2 O11 . 2_665 99.25(16)
O4 Mo2 O11 . 2_665 103.76(14)
O10 Mo2 O11 . 2_665 141.44(13)
O1 Mo2 O13 . 2_665 87.18(16)
O4 Mo2 O13 . 2_665 168.11(14)
O10 Mo2 O13 . 2_665 72.05(12)
O11 Mo2 O13 2_665 2_665 80.21(12)
O1 Mo2 O12 . 4_656 165.31(15)
O4 Mo2 O12 . 4_656 90.04(14)
O10 Mo2 O12 . 4_656 78.65(12)
O11 Mo2 O12 2_665 4_656 70.72(12)
O13 Mo2 O12 2_665 4_656 80.64(10)
O9 Mo3 O3 . . 104.30(17)
O9 Mo3 O12 . 2_565 99.44(15)
O3 Mo3 O12 . 2_565 101.66(14)
O9 Mo3 O10 . 1_455 103.77(16)
O3 Mo3 O10 . 1_455 94.47(15)
O12 Mo3 O10 2_565 1_455 147.40(12)
O9 Mo3 O13 . 2_565 90.84(15)
O3 Mo3 O13 . 2_565 162.09(13)
O12 Mo3 O13 2_565 2_565 84.88(12)
O10 Mo3 O13 1_455 2_565 72.32(12)
O9 Mo3 O11 . 4_656 165.14(15)
O3 Mo3 O11 . 4_656 89.84(13)
O12 Mo3 O11 2_565 4_656 72.79(11)
O10 Mo3 O11 1_455 4_656 79.19(12)
O13 Mo3 O11 2_565 4_656 76.06(11)
O7 Mo4 O8 . . 104.3(2)
O7 Mo4 O5 . . 97.95(19)
O8 Mo4 O5 . . 95.13(18)
O7 Mo4 O2 . . 94.84(16)
O8 Mo4 O2 . . 95.74(17)
O5 Mo4 O2 . . 160.62(14)
O7 Mo4 O3 . . 90.67(18)
O8 Mo4 O3 . . 165.03(19)
O5 Mo4 O3 . . 82.88(13)
O2 Mo4 O3 . . 82.47(13)
O7 Mo4 O4 . . 165.11(18)
O8 Mo4 O4 . . 90.47(19)
O5 Mo4 O4 . . 78.55(16)
O2 Mo4 O4 . . 85.37(14)
O3 Mo4 O4 . . 74.58(12)
O6 As1 O2 . . 110.01(18)
O6 As1 O5 . 4_646 112.4(2)
O2 As1 O5 . 4_646 102.26(18)
O6 As1 O13 . . 110.60(17)
O2 As1 O13 . . 110.10(15)
O5 As1 O13 4_646 . 111.22(16)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Mo1 O14 1_655 1.674(4)
Mo1 O15 1_655 1.682(4)
Mo1 O12 1_655 1.977(3)
Mo1 O11 . 2.005(3)
Mo1 O6 . 2.048(4)
Mo2 O1 . 1.675(4)
Mo2 O4 . 1.735(3)
Mo2 O10 . 1.890(4)
Mo2 O11 2_665 1.936(3)
Mo2 O13 2_665 2.289(3)
Mo2 O12 4_656 2.388(3)
Mo3 O9 . 1.677(3)
Mo3 O3 . 1.742(3)
Mo3 O12 2_565 1.934(3)
Mo3 O10 1_455 1.946(3)
Mo3 O13 2_565 2.237(3)
Mo3 O11 4_656 2.300(3)
Mo4 O7 . 1.693(4)
Mo4 O8 . 1.703(4)
Mo4 O5 . 1.947(3)
Mo4 O2 . 1.964(3)
Mo4 O3 . 2.213(3)
Mo4 O4 . 2.237(3)
As1 O6 . 1.656(4)
As1 O2 . 1.661(3)
As1 O5 4_646 1.662(3)
As1 O13 . 1.685(3)
K1 O14 4_656 2.558(4)
K1 O15 1_655 2.662(4)
K1 O8 . 2.676(5)
K1 O8 3_566 2.745(5)
K1 O7 1_655 2.771(5)
K1 O9 4_656 3.106(4)
K1 O7 3_566 3.118(5)
K1 O10 . 3.290(3)
K1 O4 . 3.423(4)
