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
Michael J. Hughes; Michael Gerken; Hélène P. A. Mercier; Gary J. Schrobilgen; Inorganic Chemistry 49 (2010) 4768–4780; doi:10.1021/ic100383p

data_4315667
_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