Direct Access to POP-Type Osmium(II) and Osmium(IV) Complexes: Osmium a Promising Alternative to Ruthenium for the Synthesis of Imines from Alcohols and Amines
Esteruelas, Miguel A.; Honczek, Nicole; Oliván, Montserrat; Oñate, Enrique; Valencia, Marta; Organometallics 30 (2011) 2468–; doi:10.1021/om200290u

data_4064711
_publ_section_title
;
 Direct Access to POP-Type Osmium(II) and Osmium(IV) Complexes: Osmium a
 Promising Alternative to Ruthenium for the Synthesis of Imines from
 Alcohols and Amines
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2468
_journal_paper_doi               10.1021/om200290u
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C24 H37 Cl O Os P2, C4 H8 O'
_chemical_formula_sum            'C28 H45 Cl O2 Os P2'
_chemical_formula_weight         701.23
_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                 97.962(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.249(3)
_cell_length_b                   12.810(3)
_cell_length_c                   19.873(5)
_cell_measurement_reflns_used    3559
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     2836.1(12)
_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      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.938
_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  0.1110
_diffrn_reflns_av_sigmaI/netI    0.1246
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            34777
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.92
_diffrn_reflns_theta_min         1.90
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    4.726
_exptl_absorpt_correction_T_max  0.784
_exptl_absorpt_correction_T_min  0.598
_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            'pale yellow'
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.181
_refine_diff_density_min         -1.284
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.809
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         7019
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      0.819
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0101P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0525
_refine_ls_wR_factor_ref         0.0588
_reflns_number_gt                4324
_reflns_number_total             7019
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200290u_si_002.cif
_cod_data_source_block           mae446as
_cod_original_cell_volume        2836.3(12)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4064711