Dehydrogenative Addition of Aldehydes to a Mixed NHC-Osmium-Phosphine Hydroxide Complex: Formation of Carboxylate Derivatives
Buil, María L.; Cardo, Juan J. F.; Esteruelas, Miguel A.; Oñate, Enrique; Organometallics 35 (2016) 2171–; doi:10.1021/acs.organomet.6b00396

data_4088765
_publ_section_title
;
 Dehydrogenative Addition of Aldehydes to a Mixed NHC-Osmium-Phosphine
 Hydroxide Complex: Formation of Carboxylate Derivatives
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              2171
_journal_paper_doi               10.1021/acs.organomet.6b00396
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C52 H70 N2 O2 Os P, C F3 O3 S'
_chemical_formula_sum            'C53 H70 F3 N2 O5 Os P S'
_chemical_formula_weight         1125.34
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.561(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0512(14)
_cell_length_b                   23.076(3)
_cell_length_c                   20.426(3)
_cell_measurement_reflns_used    9878
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2
_cell_volume                     5208.7(12)
_computing_cell_refinement       'SAINT+ v. 7.56a (Bruker AXS, 2008)'
_computing_data_collection       'apex2 v. 7.0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+ v. 7.56a (Bruker AXS, 2008)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.14 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.14 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'Bruker APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_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  0.0501
_diffrn_reflns_av_sigmaI/netI    0.0369
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            82817
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.52
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    2.577
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.748
_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.

SADABS: Area-Detector Absorption Correction. Bruker-AXS 
within SAINT+ package, v. 7.56a (2008).
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.256
_refine_diff_density_min         -0.774
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.204
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         13742
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.220
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0311
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0341P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0753
_reflns_number_gt                11078
_reflns_number_total             13742
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00396_si_001.cif
_cod_data_source_block           enriquen115
_cod_original_cell_volume        5208.6(11)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4088765