#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:13:37 +0100 (Wed, 23 Mar 2016) $
#$Revision: 179236 $
#$URL: svn://saulius.grazulis.lt/cod-secondary/cif/4/31/56/4315667.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_4315667
loop_
_publ_author_name
'Michael J. Hughes'
'Michael Gerken'
'H\'el\`ene P. A. Mercier'
'Gary J. Schrobilgen'
_publ_section_title
;
 Syntheses and Multi-NMR Study of fac- and mer-OsO3F2(NCCH3) and the X-ray
 Crystal Structure (n= 2) and Raman Spectrum (n= 0) of
 fac-OsO3F2(NCCH3).nCH3CN
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4768
_journal_page_last               4780
_journal_paper_doi               10.1021/ic100383p
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C6 H9 F2 N3 O3 Os'
_chemical_formula_weight         399.36
_chemical_name_common            'F3 O2 Os N C2 H3 2(C2 H3 N)'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                   7.7995(2)
_cell_length_b                   14.7327(4)
_cell_length_c                   9.5210(2)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      64
_cell_measurement_theta_min      0
_cell_volume                     1094.04(5)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0646
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            27193
_diffrn_reflns_theta_full        32.48
_diffrn_reflns_theta_max         32.48
_diffrn_reflns_theta_min         2.77
_exptl_absorpt_coefficient_mu    11.676
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.522
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 v2.0-2 (Bruker, 2005)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.425
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.029
_refine_diff_density_min         -1.564
_refine_diff_density_rms         0.148
_refine_ls_extinction_coef       0.00352(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         2032
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0215
_refine_ls_R_factor_gt           0.0178
_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/[\s^2^(Fo^2^)+(0.0197P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0403
_refine_ls_wR_factor_ref         0.0413
_reflns_number_gt                1832
_reflns_number_total             2032
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100383p_si_002.cif
_cod_data_source_block           mh16pnma
_cod_database_code               4315667
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.206457(14) 0.2500 0.360716(12) 0.01141(5) Uani 1 2 d S . .
O1 O 0.0700(2) 0.33959(12) 0.37870(17) 0.0188(3) Uani 1 1 d . . .
F1 F 0.39346(18) 0.33312(10) 0.39971(15) 0.0192(3) Uani 1 1 d . . .
O2 O 0.2481(3) 0.2500 0.1859(3) 0.0185(5) Uani 1 2 d S . .
N2 N 0.0541(3) 0.57805(18) 0.2620(2) 0.0305(5) Uani 1 1 d . . .
C4 C 0.1268(3) 0.53404(17) 0.1835(3) 0.0217(5) Uani 1 1 d . . .
C3 C 0.2180(4) 0.4781(2) 0.0821(4) 0.0278(6) Uani 1 1 d . . .
H4A H 0.252(5) 0.509(3) 0.017(4) 0.033 Uiso 1 1 d . . .
H4B H 0.314(5) 0.451(3) 0.127(3) 0.033 Uiso 1 1 d . . .
H4C H 0.149(5) 0.428(2) 0.057(4) 0.033 Uiso 1 1 d . . .
N1 N 0.2052(3) 0.2500 0.5924(3) 0.0168(5) Uani 1 2 d S . .
C1 C 0.2014(4) 0.2500 0.7121(4) 0.0175(6) Uani 1 2 d S . .
C2 C 0.2012(5) 0.2500 0.8631(3) 0.0201(7) Uani 1 2 d S . .
H2C H 0.1210 0.2962 0.8973 0.024 Uiso 0.50 1 calc PR . .
H2A H 0.3168 0.2636 0.8975 0.024 Uiso 0.50 1 calc PR . .
H2B H 0.1656 0.1902 0.8974 0.024 Uiso 0.50 1 calc PR . .
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
Os1 0.01024(7) 0.01397(7) 0.01001(7) 0.000 -0.00060(4) 0.000
O1 0.0189(8) 0.0184(8) 0.0192(8) -0.0001(6) -0.0018(6) 0.0041(7)
F1 0.0166(6) 0.0231(7) 0.0179(6) -0.0006(5) 0.0003(6) -0.0064(6)
O2 0.0195(11) 0.0250(13) 0.0111(10) 0.000 -0.0018(10) 0.000
N2 0.0296(12) 0.0297(13) 0.0322(13) -0.0018(10) 0.0071(11) -0.0035(10)
C4 0.0204(11) 0.0191(11) 0.0256(11) 0.0041(10) -0.0025(11) -0.0044(10)
C3 0.0252(13) 0.0239(13) 0.0342(15) -0.0064(13) -0.0016(12) 0.0033(11)
N1 0.0169(13) 0.0194(14) 0.0141(12) 0.000 0.0006(10) 0.000
C1 0.0162(14) 0.0156(14) 0.0205(16) 0.000 0.0026(12) 0.000
C2 0.030(2) 0.0214(17) 0.0090(13) 0.000 0.0044(13) 0.000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
F F 0.0171 0.0103 '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'
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
O2 Os1 O1 102.60(8) . 7_565 ?
O2 Os1 O1 102.60(8) . . ?
O1 Os1 O1 101.53(13) 7_565 . ?
O2 Os1 F1 92.52(8) . 7_565 ?
O1 Os1 F1 87.79(8) 7_565 7_565 ?
O1 Os1 F1 159.89(8) . 7_565 ?
O2 Os1 F1 92.52(8) . . ?
O1 Os1 F1 159.89(8) 7_565 . ?
O1 Os1 F1 87.79(8) . . ?
F1 Os1 F1 78.27(9) 7_565 . ?
O2 Os1 N1 169.22(11) . . ?
O1 Os1 N1 84.08(7) 7_565 . ?
O1 Os1 N1 84.08(7) . . ?
F1 Os1 N1 79.16(7) 7_565 . ?
F1 Os1 N1 79.16(7) . . ?
N2 C4 C3 179.3(3) . . ?
C1 N1 Os1 178.7(3) . . ?
N1 C1 C2 178.6(3) . . ?
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 O2 1.696(2) . ?
Os1 O1 1.7040(18) 7_565 ?
Os1 O1 1.7040(18) . ?
Os1 F1 1.9402(14) 7_565 ?
Os1 F1 1.9402(14) . ?
Os1 N1 2.206(3) . ?
N2 C4 1.140(3) . ?
C4 C3 1.456(4) . ?
N1 C1 1.140(5) . ?
C1 C2 1.437(5) . ?
