Synthesis and X-ray Crystal Structure of (OsO3F2)2.2XeOF4 and the Raman Spectra of (OsO3F2)\ιnfty, (OsO3F2)2, and (OsO3F2)2.2XeOF4
Michael J. Hughes; Hélène P. A. Mercier; Gary J. Schrobilgen; Inorganic Chemistry 48 (2009) 4478–4490; doi:10.1021/ic900242m

data_4302135
_publ_section_title
;
Synthesis and X-ray Crystal Structure of (OsO3F2)2.2XeOF4 and the Raman
Spectra of (OsO3F2)\\infty, (OsO3F2)2, and (OsO3F2)2.2XeOF4
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4478
_journal_page_last               4490
_journal_paper_doi               10.1021/ic900242m
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'F12 O8 Os2 Xe2'
_chemical_formula_weight         999.00
_chemical_name_common            'F4 O6 Os2, 2(Xe O F4)'
_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                80.012(4)
_cell_angle_beta                 83.659(4)
_cell_angle_gamma                89.217(4)
_cell_formula_units_Z            1
_cell_length_a                   5.0808(6)
_cell_length_b                   7.7446(9)
_cell_length_c                   9.2133(11)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65
_cell_measurement_theta_min      0
_cell_volume                     354.85(7)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0510
_diffrn_reflns_av_sigmaI/netI    0.0517
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8774
_diffrn_reflns_theta_full        32.49
_diffrn_reflns_theta_max         32.49
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    22.759
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    4.675
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.736
_refine_diff_density_min         -4.602
_refine_diff_density_rms         0.482
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         2534
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0623P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.0988
_reflns_number_gt                2134
_reflns_number_total             2534
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900242m_si_002.cif
_cod_data_source_block           mh13
_cod_database_code               4302135