#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/96/2239658.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_2239658
loop_
_publ_author_name
'Souilem, Amira'
'Zid, Mohamed Faouzi'
'Driss, Ahmed'
_publ_section_title
;
 β-K₃Fe(MoO₄)₂Mo₂O₇
;
_journal_coeditor_code           WM5025
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i38
_journal_paper_doi               10.1107/S1600536814013087
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'K3 Fe (Mo O4)2 Mo2 O7'
_chemical_formula_moiety         'Fe K3 Mo4 O15'
_chemical_formula_sum            'Fe K3 Mo4 O15'
_chemical_formula_weight         796.91
_chemical_name_systematic
;
Tripotassium iron(III) bis(orthomolybdate) dimolybdate
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.143(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   32.873(2)
_cell_length_b                   5.7137(7)
_cell_length_c                   7.9177(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      11
_cell_volume                     1486.9(3)
_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 & Putz, 1999)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3443
_diffrn_reflns_theta_full        26.97
_diffrn_reflns_theta_max         26.97
_diffrn_reflns_theta_min         2.48
_diffrn_standards_decay_%        1.3
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    5.146
_exptl_absorpt_correction_T_max  0.4884
_exptl_absorpt_correction_T_min  0.2855
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.560
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1484
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.216
_refine_diff_density_min         -1.573
_refine_ls_extinction_coef       0.00379(16)
_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   1.063
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         1789
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0291
_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)+(0.0306P)²+20.6944P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0764
_reflns_number_gt                1636
_reflns_number_total             1789
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            wm5025sup1.cf
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               2239658
_cod_database_fobs_code          2239658
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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_symmetry_multiplicity
Mo Mo1 0.568576(15) 0.5000 -0.03610(7) 0.01354(16) Uani d S 1 2
Mo Mo2 0.649834(16) 0.0000 0.73776(7) 0.01577(16) Uani d S 1 2
Mo Mo3 0.718491(15) 0.0000 0.18432(7) 0.01355(16) Uani d S 1 2
Mo Mo4 0.55700(2) 0.5000 0.49609(8) 0.0375(2) Uani d S 1 2
Fe Fe1 0.68040(3) 0.5000 -0.01846(11) 0.0118(2) Uani d S 1 2
K K1 0.51309(5) 0.0000 0.7616(2) 0.0253(3) Uani d S 1 2
K K2 0.60638(5) 0.0000 0.2307(2) 0.0340(4) Uani d S 1 2
K K3 0.68689(5) 0.5000 0.4756(2) 0.0361(5) Uani d S 1 2
O O1 0.62085(14) 0.5000 0.0211(7) 0.0257(11) Uani d S 1 2
O O2 0.73729(17) 0.0000 0.3855(7) 0.0373(15) Uani d S 1 2
O O3 0.54601(11) 0.7403(7) 0.0504(5) 0.0277(8) Uani d . 1 1
O O4 0.68711(12) 0.7469(9) 0.1610(6) 0.0459(13) Uani d . 1 1
O O5 0.60430(19) 0.5000 0.4216(9) 0.053(2) Uani d S 1 2
O O6 0.75919(14) 0.0000 0.0434(6) 0.0223(11) Uani d S 1 2
O O7 0.67523(14) 0.2575(11) 0.8080(7) 0.0669(19) Uani d . 1 1
O O8 0.55792(18) 0.5000 0.7337(6) 0.0329(13) Uani d S 1 2
O O9 0.64948(18) 0.0000 0.5221(7) 0.0346(14) Uani d S 1 2
O O10 0.60110(17) 0.0000 0.8120(8) 0.0396(15) Uani d S 1 2
O O11 0.5491(2) 0.1696(14) 0.4498(9) 0.031(2) Uani d P 0.524(11) 1
O O12 0.5224(3) 0.3608(15) 0.3916(10) 0.034(3) Uani d P 0.476(11) 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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
0 4 0
0 2 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
O3 Mo1 O3 . 6_565 106.8(3)
O3 Mo1 O1 . . 108.94(15)
O3 Mo1 O1 6_565 . 108.94(15)
O3 Mo1 O8 . 1_554 108.63(16)
O3 Mo1 O8 6_565 1_554 108.63(16)
O1 Mo1 O8 . 1_554 114.6(2)
O9 Mo2 O10 . . 110.8(3)
O9 Mo2 O7 . . 107.9(2)
O10 Mo2 O7 . . 109.20(18)
O9 Mo2 O7 . 6 107.9(2)
O10 Mo2 O7 . 6 109.20(18)
O7 Mo2 O7 . 6 111.9(4)
O2 Mo3 O6 . . 109.2(3)
O2 Mo3 O4 . 1_545 107.2(2)
O6 Mo3 O4 . 1_545 112.33(14)
O2 Mo3 O4 . 6_565 107.2(2)
O6 Mo3 O4 . 6_565 112.33(14)
O4 Mo3 O4 1_545 6_565 108.3(3)
O12 Mo4 O12 . 6_565 59.4(7)
O12 Mo4 O5 . . 118.2(4)
O12 Mo4 O5 6_565 . 118.2(4)
O12 Mo4 O8 . . 120.8(3)
O12 Mo4 O8 6_565 . 120.8(3)
O5 Mo4 O8 . . 110.9(3)
O12 Mo4 O11 . . 47.9(4)
O12 Mo4 O11 6_565 . 107.1(4)
O5 Mo4 O11 . . 93.2(2)
O8 Mo4 O11 . . 100.9(2)
O12 Mo4 O11 . 6_565 107.1(4)
O12 Mo4 O11 6_565 6_565 47.9(4)
O5 Mo4 O11 . 6_565 93.2(2)
O8 Mo4 O11 . 6_565 100.9(2)
O11 Mo4 O11 . 6_565 153.4(4)
O7 Fe1 O7 1_554 6_564 90.2(4)
O7 Fe1 O1 1_554 . 92.22(17)
O7 Fe1 O1 6_564 . 92.22(17)
O7 Fe1 O6 1_554 7_655 90.18(17)
O7 Fe1 O6 6_564 7_655 90.18(17)
O1 Fe1 O6 . 7_655 176.6(2)
O7 Fe1 O4 1_554 . 178.6(2)
O7 Fe1 O4 6_564 . 90.4(3)
O1 Fe1 O4 . . 89.03(15)
O6 Fe1 O4 7_655 . 88.54(16)
O7 Fe1 O4 1_554 6_565 90.4(3)
O7 Fe1 O4 6_564 6_565 178.6(2)
O1 Fe1 O4 . 6_565 89.03(15)
O6 Fe1 O4 7_655 6_565 88.54(16)
O4 Fe1 O4 . 6_565 89.1(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Mo1 O3 . 1.710(4)
Mo1 O3 6_565 1.710(4)
Mo1 O1 . 1.768(5)
Mo1 O8 1_554 1.849(5)
Mo2 O9 . 1.708(5)
Mo2 O10 . 1.717(6)
Mo2 O7 . 1.776(5)
Mo2 O7 6 1.776(5)
Mo3 O2 . 1.697(5)
Mo3 O6 . 1.759(5)
Mo3 O4 1_545 1.784(4)
Mo3 O4 6_565 1.784(4)
Mo4 O12 . 1.605(7)
Mo4 O12 6_565 1.605(7)
Mo4 O5 . 1.674(6)
Mo4 O8 . 1.881(5)
Mo4 O11 . 1.940(8)
Mo4 O11 6_565 1.940(8)
Fe1 O7 1_554 1.956(4)
Fe1 O7 6_564 1.956(4)
Fe1 O1 . 1.989(5)
Fe1 O6 7_655 2.000(5)
Fe1 O4 . 2.011(4)
Fe1 O4 6_565 2.011(4)
K1 O12 5_656 2.650(8)
K1 O12 2_656 2.650(8)
K1 O11 5_656 2.789(8)
K1 O11 2_656 2.789(8)
K1 O3 2_646 2.882(4)
K1 O3 5_666 2.882(4)
K1 O10 . 2.913(6)
K1 O3 6_566 2.916(4)
K1 O3 1_546 2.916(4)
K1 O11 6 2.924(7)
K1 O11 . 2.924(7)
K1 O8 1_545 3.224(3)
K2 O9 . 2.683(6)
K2 O11 . 2.762(7)
K2 O11 6 2.762(7)
K2 O3 1_545 2.841(4)
K2 O3 6_565 2.841(4)
K2 O4 6_565 3.082(5)
K2 O4 1_545 3.082(5)
K2 O5 . 3.233(3)
K2 O5 1_545 3.233(3)
K2 O10 1_554 3.317(7)
K2 O1 1_545 3.343(3)
K2 O1 . 3.343(3)
K3 O2 7_656 2.704(6)
K3 O5 . 2.740(7)
K3 O4 6_565 2.863(5)
K3 O4 . 2.863(5)
K3 O7 6_565 3.005(7)
K3 O7 . 3.005(7)
K3 O9 . 3.135(3)
K3 O9 1_565 3.135(3)
K3 O2 1_565 3.386(3)
K3 O2 . 3.386(3)
