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_4082114
_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         'C27 H33 N2 Os, C4 H8 O, C F3 O3 S'
_chemical_formula_sum            'C32 H41 F3 N2 O4 Os S'
_chemical_formula_weight         796.93
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.022(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9956(1)
_cell_length_b                   11.8815(1)
_cell_length_c                   21.8518(2)
_cell_measurement_reflns_used    65417
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      45.4951
_cell_measurement_theta_min      3.2799
_cell_volume                     3106.77(5)
_computing_cell_refinement
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) 
(compiled Jan  5 2010,16:28:46) 
;
_computing_data_collection
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) 
(compiled Jan  5 2010,16:28:46) 
;
_computing_data_reduction
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) 
(compiled Jan  5 2010,16:28:46) 
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3196
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            128074
_diffrn_reflns_theta_full        45.00
_diffrn_reflns_theta_max         45.61
_diffrn_reflns_theta_min         3.29
_exptl_absorpt_coefficient_mu    4.229
_exptl_absorpt_correction_T_max  0.584
_exptl_absorpt_correction_T_min  0.465
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) 
(compiled Jan  5 2010,16:28:46) 
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.2622
_exptl_crystal_size_mid          0.1917
_exptl_crystal_size_min          0.1859
_refine_diff_density_max         3.817
_refine_diff_density_min         -1.800
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         26159
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0233
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0535
_refine_ls_wR_factor_ref         0.0543
_reflns_number_gt                20348
_reflns_number_total             26159
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om400875r_si_001.cif
_cod_data_source_block           adp620
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4082114