#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/32/4343260.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4343260
loop_
_publ_author_name
'Gong, Pifu'
'Luo, Siyang'
'Kang, Lei'
'Jiang, Xingxing'
'Xu, Jing'
'Zhang, Guochun'
'Lin, Zheshuai'
'Wu, Yicheng'
'Chen, Chuangtian'
_publ_section_title
;
 K5Mo4O14F: A Novel Fluorinated Polyoxomolybdate and Its Structural
 Stability.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6066
_journal_page_last               6068
_journal_paper_doi               10.1021/acs.inorgchem.5b00643
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'K5 Mo4 O14 F'
_chemical_formula_sum            'F K5 Mo4 O14'
_chemical_formula_weight         822.26
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.128(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.8632(6)
_cell_length_b                   10.6729(3)
_cell_length_c                   8.4569(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1596.13(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0211
_diffrn_reflns_av_sigmaI/netI    0.0321
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2783
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    4.450
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bulk
_exptl_crystal_F_000             1535
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.650
_refine_diff_density_min         -1.909
_refine_diff_density_rms         0.170
_refine_ls_extinction_coef       0.0253(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         1407
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0323P)²+18.9097P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0742
_reflns_number_gt                1305
_reflns_number_total             1407
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic5b00643_si_002.cif
_cod_data_source_block           20150112
_cod_depositor_comments          'Adding full bibliography for 4343260.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4343260
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Mo1 Mo -0.15122(3) 0.21775(5) -0.10365(6) 0.0117(2) Uani 1 1 d .
Mo2 Mo 0.04748(3) 0.25492(5) -0.07124(5) 0.0135(2) Uani 1 1 d .
F1 F 0.0000 0.3925(4) -0.2500 0.0193(11) Uani 1 2 d S
O1 O -0.0615(2) 0.1870(4) -0.1911(4) 0.0116(8) Uani 1 1 d .
O2 O -0.0013(2) 0.3218(4) 0.0712(5) 0.0229(10) Uani 1 1 d .
O3 O 0.0715(2) 0.1061(4) 0.0051(5) 0.0163(9) Uani 1 1 d .
O4 O 0.1352(2) 0.3320(4) -0.0498(5) 0.0189(9) Uani 1 1 d .
O5 O -0.2242(2) 0.1394(4) -0.2223(5) 0.0239(10) Uani 1 1 d .
O6 O -0.1728(2) 0.3760(4) -0.0995(5) 0.0206(9) Uani 1 1 d .
O7 O -0.1437(2) 0.1596(5) 0.0891(5) 0.0241(10) Uani 1 1 d .
K1 K -0.22024(10) 0.1028(2) -0.5907(3) 0.0738(9) Uani 1 1 d .
K2 K 0.0000 0.05893(18) -0.7500 0.0199(4) Uani 1 2 d S
K3 K -0.11399(8) 0.56793(12) -0.27212(15) 0.0189(3) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
F F 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2010 0.2490 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6830 0.6860 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O7 Mo1 O6 108.5(2) . .
O7 Mo1 O5 108.8(2) . .
O6 Mo1 O5 109.2(2) . .
O7 Mo1 O1 110.48(18) . .
O6 Mo1 O1 112.37(18) . .
O5 Mo1 O1 107.39(19) . .
O2 Mo2 O3 103.8(2) . .
O2 Mo2 O4 105.3(2) . .
O3 Mo2 O4 102.65(19) . .
O2 Mo2 O1 155.33(17) . 2_554
O3 Mo2 O1 89.09(17) . 2_554
O4 Mo2 O1 91.92(17) . 2_554
O2 Mo2 O1 87.51(17) . .
O3 Mo2 O1 91.49(17) . .
O4 Mo2 O1 157.76(17) . .
O1 Mo2 O1 70.97(16) 2_554 .
O2 Mo2 F1 91.15(16) . .
O3 Mo2 F1 156.39(16) . .
O4 Mo2 F1 90.58(15) . .
O1 Mo2 F1 70.78(13) 2_554 .
O1 Mo2 F1 70.72(12) . .
O2 Mo2 Mo2 113.46(14) . 2_554
O3 Mo2 Mo2 114.37(13) . 2_554
O4 Mo2 Mo2 115.89(14) . 2_554
O1 Mo2 Mo2 41.99(10) 2_554 2_554
O1 Mo2 Mo2 41.91(10) . 2_554
F1 Mo2 Mo2 42.09(9) . 2_554
Mo2 F1 Mo2 95.81(18) 2_554 .
Mo1 O1 Mo2 121.16(19) . 2_554
Mo1 O1 Mo2 120.70(18) . .
Mo2 O1 Mo2 96.10(15) 2_554 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O7 1.732(4) .
Mo1 O6 1.734(4) .
Mo1 O5 1.743(4) .
Mo1 O1 1.886(4) .
Mo2 O2 1.737(4) .
Mo2 O3 1.745(4) .
Mo2 O4 1.756(4) .
Mo2 O1 2.184(4) 2_554
Mo2 O1 2.187(4) .
Mo2 F1 2.191(3) .
Mo2 Mo2 3.2510(9) 2_554
F1 Mo2 2.191(3) 2_554
O1 Mo2 2.184(4) 2_554
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O2 Mo2 F1 Mo2 -124.87(15) . 2_554
O3 Mo2 F1 Mo2 5.0(3) . 2_554
O4 Mo2 F1 Mo2 129.80(14) . 2_554
O1 Mo2 F1 Mo2 37.97(11) 2_554 2_554
O1 Mo2 F1 Mo2 -37.91(10) . 2_554
O7 Mo1 O1 Mo2 -177.0(2) . 2_554
O6 Mo1 O1 Mo2 -55.6(3) . 2_554
O5 Mo1 O1 Mo2 64.5(3) . 2_554
O7 Mo1 O1 Mo2 -56.7(3) . .
O6 Mo1 O1 Mo2 64.6(3) . .
O5 Mo1 O1 Mo2 -175.3(2) . .
O2 Mo2 O1 Mo1 -1.8(2) . .
O3 Mo2 O1 Mo1 101.9(2) . .
O4 Mo2 O1 Mo1 -128.1(4) . .
O1 Mo2 O1 Mo1 -169.53(18) 2_554 .
F1 Mo2 O1 Mo1 -93.9(2) . .
Mo2 Mo2 O1 Mo1 -132.0(3) 2_554 .
O2 Mo2 O1 Mo2 130.17(19) . 2_554
O3 Mo2 O1 Mo2 -126.08(17) . 2_554
O4 Mo2 O1 Mo2 3.9(5) . 2_554
O1 Mo2 O1 Mo2 -37.55(18) 2_554 2_554
F1 Mo2 O1 Mo2 38.08(11) . 2_554
