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_4082112
_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 H31 N2 Os, C F3 O3 S, C H Cl3'
_chemical_formula_sum            'C29 H32 Cl3 F3 N2 O3 Os S'
_chemical_formula_weight         842.18
_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                111.661(8)
_cell_angle_beta                 96.007(7)
_cell_angle_gamma                105.374(9)
_cell_formula_units_Z            2
_cell_length_a                   11.6662(11)
_cell_length_b                   12.3634(16)
_cell_length_c                   12.7660(11)
_cell_measurement_reflns_used    123
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      18.454
_cell_measurement_theta_min      3.532
_cell_volume                     1607.3(3)
_computing_cell_refinement
'Dirax/lsq (Duisenberg A.J.M., Nonius B.V., 1989-2000)'
_computing_data_collection
'Collect (Hooft, R.W.W., 1998. Nonius B.V., 1997-2000)'
_computing_data_reduction        'EvalCCD (Hooft R.W.W., Nonius B.V., 1998)'
_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 G.M., Bruker AXS, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick G.M., Bruker AXS, 1990)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector                 'Apex II 95mm CCD camera'
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker-Nonus KappaCCD with \k-goniostat'
_diffrn_measurement_method       'sequential \f and \w 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  0.0938
_diffrn_reflns_av_sigmaI/netI    0.0611
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23721
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.42
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    4.331
_exptl_absorpt_correction_T_max  0.0545740
_exptl_absorpt_correction_T_min  0
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Bruker Nonius Area Dector Scaling and Absorption Correction
 SADABS 2.10 (Bruker, 2003)
 based on an algorithm described by
 R.H. Blessing, Acta Cryst. (1995), a51, 33-38
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.208
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.095
_refine_diff_density_max         2.982
_refine_diff_density_min         -1.777
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         5594
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0542
_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^)+(0.0325P)^2^+25.2522P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1328
_reflns_number_gt                4873
_reflns_number_total             5594
_reflns_threshold_expression     I>2/s(I)
_cod_data_source_file            om400875r_si_001.cif
_cod_data_source_block           adp165
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4082112