#------------------------------------------------------------------------------
#$Date: 2016-02-18 13:25:00 +0100 (jue 18 de feb de 2016) $
#$Revision: 176728 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/29/8102934.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_8102934
loop_
_publ_author_name
'Xu, W.'
'Wang, P.'
'Zheng, Y.-Q.'
_publ_section_title
;
Crystal structure of dipotassium octakis(μ₃-bromo)-hexabromo-
octahedro-hexamolybdenate, K₂[Mo₆Br₁₄]
;
_journal_issue                   2
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              107
_journal_page_last               108
_journal_volume                  221
_journal_year                    2006
_chemical_formula_sum            'Br14 K2 Mo6'
_chemical_formula_weight         1772.58
_chemical_name_systematic
; 
dipotassium octa-μ₃-bromohexabromo-octahedro-hexamolybdenate
;
_space_group_IT_number           201
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 2ab 2bc 3'
_symmetry_space_group_name_H-M   'P n -3 :2'
_atom_sites_solution_hydrogens   geom
_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                   13.8000(16)
_cell_length_b                   13.8000(16)
_cell_length_c                   13.8000(16)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      5
_cell_volume                     2628.1(5)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       theta/2theta
_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  0.3936
_diffrn_reflns_av_sigmaI/netI    0.2571
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3833
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        no
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    24.368
_exptl_absorpt_correction_T_max  0.011
_exptl_absorpt_correction_T_min  0
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    4.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3120
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.495
_refine_diff_density_min         -3.496
_refine_diff_density_rms         0.521
_refine_ls_extinction_coef       0.00012(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.931
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     37
_refine_ls_number_reflns         1016
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.1192
_refine_ls_R_factor_gt           0.0768
_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)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1483
_refine_ls_wR_factor_ref         0.1862
_reflns_number_gt                659
_reflns_number_total             1016
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            409865.cff
_cod_data_source_block           K2[Mo6Br14]
_cod_original_sg_symbol_H-M      Pn-3
_cod_database_code               8102934
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y, -z+1/2'
'x, -y+1/2, -z+1/2'
'z, x, y'
'z, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y'
'-z+1/2, x, -y+1/2'
'y, z, x'
'-y+1/2, z, -x+1/2'
'y, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x-1/2, -y, z-1/2'
'-x, y-1/2, z-1/2'
'-z, -x, -y'
'-z, x-1/2, y-1/2'
'z-1/2, x-1/2, -y'
'z-1/2, -x, y-1/2'
'-y, -z, -x'
'y-1/2, -z, x-1/2'
'-y, z-1/2, x-1/2'
'y-1/2, z-1/2, -x'
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_Wyckoff_symbol
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo Mo 0.12410(9) -0.03159(9) 0.04222(9) 0.0260(4) Uani 1 24 h d . . .
Br1 Br 0.13336(10) 0.13336(10) 0.13336(10) 0.0389(7) Uani 1 8 e d S . .
Br2 Br 0.19522(11) 0.04857(11) -0.11235(12) 0.0339(5) Uani 1 24 h d . . .
Br3 Br 0.29823(12) -0.07770(15) 0.09891(13) 0.0476(6) Uani 1 24 h d . . .
K1 K 0.5000 0.0000 0.0000 0.043(2) Uani 1 4 c d S . .
K2 K 0.2500 0.7500 0.7500 0.042(2) Uani 0.67 6 d d SP . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo 0.0231(6) 0.0286(7) 0.0264(7) -0.0001(4) -0.0014(5) 0.0001(5)
Br1 0.0389(7) 0.0389(7) 0.0389(7) -0.0085(6) -0.0085(6) -0.0085(6)
Br2 0.0289(8) 0.0357(8) 0.0371(8) 0.0035(6) 0.0048(6) -0.0019(6)
Br3 0.0267(8) 0.0679(13) 0.0482(10) 0.0168(9) -0.0048(7) 0.0020(8)
K1 0.043(2) 0.043(2) 0.043(2) 0.008(3) -0.008(3) -0.008(3)
K2 0.033(5) 0.057(7) 0.038(5) 0.000 0.000 0.000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br2 Mo Br2 89.87(5) 17 . ?
Br2 Mo Br1 179.21(7) 17 . ?
Br2 Mo Br1 90.33(5) . . ?
Br2 Mo Br2 89.66(5) 17 9 ?
Br2 Mo Br2 178.58(8) . 9 ?
Br1 Mo Br2 90.12(5) . 9 ?
Br2 Mo Br3 89.43(7) 17 . ?
Br2 Mo Br3 90.12(7) . . ?
Br1 Mo Br3 91.33(7) . . ?
Br2 Mo Br3 91.21(6) 9 . ?
Br2 Mo Mo 59.90(6) 17 21 ?
Br2 Mo Mo 59.35(4) . 21 ?
Br1 Mo Mo 119.61(5) . 21 ?
Br2 Mo Mo 119.29(6) 9 21 ?
Br3 Mo Mo 134.10(7) . 21 ?
Br2 Mo Mo 59.65(6) 17 17 ?
Br2 Mo Mo 119.41(7) . 17 ?
Br1 Mo Mo 119.61(5) . 17 ?
Br2 Mo Mo 59.23(5) 9 17 ?
Br3 Mo Mo 134.65(7) . 17 ?
Mo Mo Mo 60.05(6) 21 17 ?
Br2 Mo Mo 119.63(5) 17 9 ?
Br2 Mo Mo 119.77(6) . 9 ?
Br1 Mo Mo 59.63(3) . 9 ?
Br2 Mo Mo 59.41(6) 9 9 ?
Br3 Mo Mo 135.90(7) . 9 ?
Mo Mo Mo 90.0 21 9 ?
Mo Mo Mo 59.97(3) 17 9 ?
Br2 Mo Mo 119.87(5) 17 5 ?
Br2 Mo Mo 59.77(6) . 5 ?
Br1 Mo Mo 59.63(3) . 5 ?
Br2 Mo Mo 119.41(6) 9 5 ?
Br3 Mo Mo 135.33(7) . 5 ?
Mo Mo Mo 59.97(3) 21 5 ?
Mo Mo Mo 90.0 17 5 ?
Mo Mo Mo 60.0 9 5 ?
Mo Br1 Mo 60.73(6) 9 5 ?
Mo Br1 Mo 60.73(6) 9 . ?
Mo Br1 Mo 60.73(6) 5 . ?
Mo Br2 Mo 60.99(6) 21 . ?
Mo Br2 Mo 60.87(6) 21 5 ?
Mo Br2 Mo 60.82(6) . 5 ?
Mo Br2 K2 123.15(6) 21 21_665 ?
Mo Br2 K2 151.47(6) . 21_665 ?
Mo Br2 K2 95.21(5) 5 21_665 ?
Mo Br3 K2 100.57(6) . 17_656 ?
Mo Br3 K1 125.30(7) . . ?
K2 Br3 K1 133.13(5) 17_656 . ?
Br3 K1 Br3 180.00(3) 22_655 10 ?
Br3 K1 Br3 86.55(5) 22_655 . ?
Br3 K1 Br3 93.45(5) 10 . ?
Br3 K1 Br3 86.55(5) 22_655 7 ?
Br3 K1 Br3 93.45(5) 10 7 ?
Br3 K1 Br3 93.45(5) . 7 ?
Br3 K1 Br3 93.45(5) 22_655 19_655 ?
Br3 K1 Br3 86.55(5) 10 19_655 ?
Br3 K1 Br3 86.55(5) . 19_655 ?
Br3 K1 Br3 180.00(3) 7 19_655 ?
Br3 K1 Br3 93.45(5) 22_655 13_655 ?
Br3 K1 Br3 86.55(5) 10 13_655 ?
Br3 K1 Br3 180.00(7) . 13_655 ?
Br3 K1 Br3 86.55(5) 7 13_655 ?
Br3 K1 Br3 93.45(5) 19_655 13_655 ?
Br3 K2 Br3 156.23(6) 23_566 22_666 ?
Br3 K2 Br3 85.26(8) 23_566 21_566 ?
Br3 K2 Br3 99.64(7) 22_666 21_566 ?
Br3 K2 Br3 99.64(7) 23_566 24_666 ?
Br3 K2 Br3 85.26(8) 22_666 24_666 ?
Br3 K2 Br3 156.23(6) 21_566 24_666 ?
Br3 K2 Br2 67.64(4) 23_566 18_566 ?
Br3 K2 Br2 135.42(4) 22_666 18_566 ?
Br3 K2 Br2 64.56(4) 21_566 18_566 ?
Br3 K2 Br2 95.61(4) 24_666 18_566 ?
Br3 K2 Br2 95.61(4) 23_566 19_666 ?
Br3 K2 Br2 64.56(4) 22_666 19_666 ?
Br3 K2 Br2 135.42(4) 21_566 19_666 ?
Br3 K2 Br2 67.64(4) 24_666 19_666 ?
Br2 K2 Br2 154.69(5) 18_566 19_666 ?
Br3 K2 Br2 64.56(4) 23_566 17_566 ?
Br3 K2 Br2 95.61(4) 22_666 17_566 ?
Br3 K2 Br2 67.64(4) 21_566 17_566 ?
Br3 K2 Br2 135.42(4) 24_666 17_566 ?
Br2 K2 Br2 113.20(5) 18_566 17_566 ?
Br2 K2 Br2 72.67(5) 19_666 17_566 ?
Br3 K2 Br2 135.42(4) 23_566 20_666 ?
Br3 K2 Br2 67.64(4) 22_666 20_666 ?
Br3 K2 Br2 95.61(4) 21_566 20_666 ?
Br3 K2 Br2 64.56(4) 24_666 20_666 ?
Br2 K2 Br2 72.67(5) 18_566 20_666 ?
Br2 K2 Br2 113.20(5) 19_666 20_666 ?
Br2 K2 Br2 154.69(5) 17_566 20_666 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo Br2 2.5875(19) 17 ?
Mo Br2 2.596(2) . ?
Mo Br1 2.604(2) . ?
Mo Br2 2.6051(19) 9 ?
Mo Br3 2.6061(19) . ?
Mo Mo 2.630(2) 21 ?
Mo Mo 2.630(2) 17 ?
Mo Mo 2.632(2) 9 ?
Mo Mo 2.632(2) 5 ?
Br1 Mo 2.604(2) 9 ?
Br1 Mo 2.604(2) 5 ?
Br2 Mo 2.5875(19) 21 ?
Br2 Mo 2.6051(19) 5 ?
Br2 K2 3.4506(15) 21_665 ?
Br3 K2 3.2318(18) 17_656 ?
Br3 K1 3.2811(17) . ?
K1 Br3 3.2811(17) 22_655 ?
K1 Br3 3.2811(17) 10 ?
K1 Br3 3.2811(17) 7 ?
K1 Br3 3.2811(17) 19_655 ?
K1 Br3 3.2811(17) 13_655 ?
K2 Br3 3.2318(18) 23_566 ?
K2 Br3 3.2318(18) 22_666 ?
K2 Br3 3.2318(18) 21_566 ?
K2 Br3 3.2318(18) 24_666 ?
K2 Br2 3.4506(15) 18_566 ?
K2 Br2 3.4506(15) 19_666 ?
K2 Br2 3.4506(15) 17_566 ?
K2 Br2 3.4506(15) 20_666 ?
