Reactions of a Dihydride−Osmium(IV) Complex with Aldehydes: Influence of the Substituent at the Carbonyl Group
Esteruelas, Miguel A.; Hernández, Yohar A.; López, Ana M.; Oliván, Montserrat; Rubio, Lucía; Organometallics 27 (2008) 799–; doi:10.1021/om701075d

data_4070846
_publ_section_title
;
 Reactions of a Dihydride&#x2212;Osmium(IV) Complex with Aldehydes:
 Influence of the Substituent at the Carbonyl Group
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              799
_journal_paper_doi               10.1021/om701075d
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C47 H54 B O Os P'
_chemical_formula_weight         866.88
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.482(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.8600(17)
_cell_length_b                   10.1387(10)
_cell_length_c                   23.855(2)
_cell_measurement_reflns_used    1764
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      17
_cell_measurement_theta_min      2
_cell_volume                     3981.4(7)
_computing_cell_refinement       'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_computing_data_collection       'SMART v. 5.625 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_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(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Bruker SMART 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  0.1208
_diffrn_reflns_av_sigmaI/netI    0.1981
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            40894
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.93
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    3.278
_exptl_absorpt_correction_T_max  0.864
_exptl_absorpt_correction_T_min  0.770
_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. 6.1 (2000).
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.271
_refine_diff_density_min         -1.459
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.801
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         9794
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.801
_refine_ls_R_factor_all          0.1293
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0199P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0994
_reflns_number_gt                5185
_reflns_number_total             9794
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om701075d-file002.cif
_cod_data_source_block           mae257as
_cod_original_cell_volume        3981.3(7)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4070846