[H(EtOH)2][{OsCl(η4-COD)}2(μ-H)(μ-Cl)2] as an Intermediate for the Preparation of [OsCl2(COD)]xand Its Activity as an Ionic Hydrogenation and Etherification Catalyst
Esteruelas, Miguel A.; García-Yebra, Cristina; Oñate, Enrique; Organometallics 27 (2008) 3029–; doi:10.1021/om800150z

data_4071404
_publ_section_title
;
 [H(EtOH)2][{OsCl(\h4-COD)}2(\m-H)(\m-Cl)2] as an Intermediate for the
 Preparation of [OsCl2(COD)]xand Its Activity as an Ionic Hydrogenation
 and Etherification Catalyst
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3029
_journal_paper_doi               10.1021/om800150z
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C18 H28 Cl3 N Os2'
_chemical_formula_weight         745.16
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 100.5180(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.4555(11)
_cell_length_b                   9.2944(7)
_cell_length_c                   13.9390(10)
_cell_measurement_reflns_used    4065
_cell_measurement_temperature    105.0(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2.5
_cell_volume                     1968.7(2)
_computing_cell_refinement       'SAINT+ v. 6.02 (Bruker AXS, 1999)'
_computing_data_collection       'SMART v. 5.625 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.02 (Bruker AXS, 1999)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      105.0(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_sigmaI/netI    0.0450
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23817
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.78
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    13.304
_exptl_absorpt_correction_T_max  0.35
_exptl_absorpt_correction_T_min  0.242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Absorption correction performed with SADABS program. This is based on the
method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.514
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.552
_refine_diff_density_min         -1.366
_refine_diff_density_rms         0.245
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         4810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+0.9261P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0796
_reflns_number_gt                4153
_reflns_number_total             4810
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800150z-file001.cif
_cod_data_source_block           mae272bs
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4071404