#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:55:43 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179218 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/44/4314475.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_4314475
loop_
_publ_author_name
'Michael J. Hughes'
'Hélène P. A. Mercier'
'Gary J. Schrobilgen'
_publ_section_title
;
 Fluoride Ion Donor Properties of cis-OsO2F4: Synthesis, Raman
 Spectroscopic Study, and X-ray Crystal Structure of [OsO2F3][Sb2F11]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              271
_journal_page_last               284
_journal_paper_doi               10.1021/ic901999e
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'F14 O2 Os Sb2'
_chemical_formula_weight         731.70
_chemical_name_common            'F3 O2 Os, Sb2 F11'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.597(2)
_cell_angle_beta                 111.263(2)
_cell_angle_gamma                110.697(2)
_cell_formula_units_Z            2
_cell_length_a                   7.4284(3)
_cell_length_b                   8.6649(4)
_cell_length_c                   10.0349(4)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69
_cell_measurement_theta_min      0
_cell_volume                     537.39(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker Saint'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_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  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0586
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12832
_diffrn_reflns_theta_full        34.50
_diffrn_reflns_theta_max         34.50
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    16.981
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    4.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.690
_refine_diff_density_min         -2.471
_refine_diff_density_rms         0.397
_refine_ls_extinction_coef       0.0135(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   1.242
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         4355
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.242
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0157P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0672
_refine_ls_wR_factor_ref         0.0694
_reflns_number_gt                3724
_reflns_number_total             4355
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901999e_si_002.cif
_cod_data_source_block           mh08check
_cod_database_code               4314475
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.18568(3) 0.77030(3) 0.75412(2) 0.00874(7) Uani 1 1 d . . .
Sb1 Sb 0.08890(5) 0.80192(5) 1.13604(4) 0.00628(8) Uani 1 1 d . . .
Sb2 Sb 0.55673(5) 0.65245(5) 1.31972(4) 0.00720(8) Uani 1 1 d . . .
F7 F -0.1019(5) 0.5712(4) 1.0626(4) 0.0112(7) Uani 1 1 d . . .
F11 F 0.3462(5) 0.4272(5) 1.2375(4) 0.0167(7) Uani 1 1 d . . .
F8 F -0.1154(5) 0.8781(4) 1.0525(4) 0.0125(7) Uani 1 1 d . . .
F6 F 0.0877(5) 0.8225(5) 1.3201(4) 0.0146(7) Uani 1 1 d . . .
F3 F -0.0290(5) 0.8363(5) 0.7016(4) 0.0164(7) Uani 1 1 d . . .
F4 F 0.1255(5) 0.7707(4) 0.9522(3) 0.0115(7) Uani 1 1 d . . .
F12 F 0.4830(5) 0.6773(5) 1.4766(4) 0.0177(8) Uani 1 1 d . . .
O2 O -0.0086(5) 0.5544(5) 0.6954(4) 0.0071(7) Uani 1 1 d . . .
F13 F 0.5932(5) 0.6410(5) 1.1470(4) 0.0134(7) Uani 1 1 d . . .
F9 F 0.3148(5) 0.7183(5) 1.2083(4) 0.0139(7) Uani 1 1 d . . .
F14 F 0.7316(5) 0.8884(5) 1.3898(4) 0.0166(7) Uani 1 1 d . . .
F5 F 0.3182(5) 1.0177(5) 1.2050(4) 0.0140(7) Uani 1 1 d . . .
F2 F 0.3879(5) 0.7135(5) 0.8664(4) 0.0162(7) Uani 1 1 d . . .
F1 F 0.3601(5) 0.9929(5) 0.8683(4) 0.0154(7) Uani 1 1 d . . .
O1 O 0.2345(6) 0.7727(6) 0.6060(4) 0.0134(8) Uani 1 1 d . . .
F10 F 0.7756(5) 0.5909(5) 1.4156(4) 0.0130(7) 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 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 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
_geom_angle_publ_flag
O1 Os1 O2 99.9(2) . . ?
O1 Os1 F2 100.23(17) . . ?
O2 Os1 F2 90.32(16) . . ?
O1 Os1 F3 100.07(17) . . ?
O2 Os1 F3 88.61(16) . . ?
F2 Os1 F3 159.55(16) . . ?
O1 Os1 F1 100.12(19) . . ?
O2 Os1 F1 159.89(17) . . ?
F2 Os1 F1 87.83(16) . . ?
F3 Os1 F1 86.21(16) . . ?
O1 Os1 F4 179.15(18) . . ?
O2 Os1 F4 80.89(15) . . ?
F2 Os1 F4 79.49(13) . . ?
F3 Os1 F4 80.18(14) . . ?
F1 Os1 F4 79.08(14) . . ?
F6 Sb1 F8 97.63(15) . . ?
F6 Sb1 F7 92.86(16) . . ?
F8 Sb1 F7 94.86(14) . . ?
F6 Sb1 F5 91.98(16) . . ?
F8 Sb1 F5 94.74(15) . . ?
F7 Sb1 F5 168.58(15) . . ?
F6 Sb1 F4 171.46(14) . . ?
F8 Sb1 F4 90.87(14) . . ?
F7 Sb1 F4 87.11(15) . . ?
F5 Sb1 F4 86.58(15) . . ?
F6 Sb1 F9 88.04(14) . . ?
F8 Sb1 F9 174.31(15) . . ?
F7 Sb1 F9 85.30(14) . . ?
F5 Sb1 F9 84.54(14) . . ?
F4 Sb1 F9 83.45(13) . . ?
F13 Sb2 F11 90.47(17) . . ?
F13 Sb2 F14 89.89(16) . . ?
F11 Sb2 F14 170.68(15) . . ?
F13 Sb2 F12 169.68(15) . . ?
F11 Sb2 F12 89.38(17) . . ?
F14 Sb2 F12 88.60(17) . . ?
F13 Sb2 F10 94.16(15) . . ?
F11 Sb2 F10 94.11(15) . . ?
F14 Sb2 F10 95.14(15) . . ?
F12 Sb2 F10 96.15(15) . . ?
F13 Sb2 F9 84.36(14) . . ?
F11 Sb2 F9 85.52(14) . . ?
F14 Sb2 F9 85.25(14) . . ?
F12 Sb2 F9 85.34(14) . . ?
F10 Sb2 F9 178.46(15) . . ?
Sb1 F4 Os1 172.99(18) . . ?
Sb1 F9 Sb2 170.0(2) . . ?
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
Os1 O1 1.654(4) . ?
Os1 O2 1.764(4) . ?
Os1 F2 1.791(3) . ?
Os1 F3 1.807(3) . ?
Os1 F1 1.812(4) . ?
Os1 F4 2.190(3) . ?
Sb1 F6 1.835(3) . ?
Sb1 F8 1.837(3) . ?
Sb1 F7 1.844(3) . ?
Sb1 F5 1.851(3) . ?
Sb1 F4 1.958(3) . ?
Sb1 F9 1.995(3) . ?
Sb2 F13 1.844(3) . ?
Sb2 F11 1.848(4) . ?
Sb2 F14 1.855(4) . ?
Sb2 F12 1.856(4) . ?
Sb2 F10 1.862(3) . ?
Sb2 F9 2.060(3) . ?
