Synthesis, Characterization, and Reactivity of the First Osmium β-Diketiminato Complexes and Application in Catalysis
Schreiber, Dominique F.; O’Connor, Crystal; Grave, Christian; Müller-Bunz, Helge; Scopelliti, Rosario; Dyson, Paul J.; Phillips, Andrew D.; Organometallics 32 (2013) 7345–; doi:10.1021/om400875r

data_4082116
_publ_section_title
;
 Synthesis, Characterization, and Reactivity of the First Osmium
 \b-Diketiminato Complexes and Application in Catalysis
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              7345
_journal_paper_doi               10.1021/om400875r
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C36 H40 N3 Os, C F3 O3 S'
_chemical_formula_sum            'C37 H40 F3 N3 O3 Os S'
_chemical_formula_weight         853.98
_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_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                84.903(5)
_cell_angle_beta                 88.577(5)
_cell_angle_gamma                68.497(5)
_cell_formula_units_Z            2
_cell_length_a                   10.9959(6)
_cell_length_b                   12.4489(7)
_cell_length_c                   13.0820(8)
_cell_measurement_reflns_used    11972
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      28.6159
_cell_measurement_theta_min      3.1008
_cell_volume                     1659.47(18)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_molecular_graphics
'Diamond 3.2 (Brandenburg, K., Crystal Impact GbR, 2009)'
_computing_publication_material  'WinGX 1.80.05'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(2)
_diffrn_detector_area_resol_mean 8.2812
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0203
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14274
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.68
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    3.964
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48316
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.111
_refine_diff_density_max         2.064
_refine_diff_density_min         -1.345
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         7843
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0268
_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^)+(0.0511P)^2^+0.0471P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0699
_reflns_number_gt                7110
_reflns_number_total             7843
_reflns_threshold_expression     I>2/s(I)
_cod_data_source_file            om400875r_si_001.cif
_cod_data_source_block           adp547
_cod_original_cell_volume        1659.47(16)
_cod_database_code               4082116