Preparation of Half-Sandwich Osmium Complexes by Deprotonation of Aromatic and Pro-aromatic Acids with a Hexahydride Brønsted Base
Esteruelas, Miguel A.; García-Raboso, Jorge; Oliván, Montserrat; Organometallics 30 (2011) 3844–; doi:10.1021/om200371r

data_4064861
_publ_section_title
;
 Preparation of Half-Sandwich Osmium Complexes by Deprotonation of
 Aromatic and Pro-aromatic Acids with a Hexahydride Br\/onsted Base
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3844
_journal_paper_doi               10.1021/om200371r
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C22 H47 N Os P2'
_chemical_formula_weight         577.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 96.380(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.589(4)
_cell_length_b                   11.559(4)
_cell_length_c                   16.492(6)
_cell_measurement_reflns_used    7276
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      3
_cell_volume                     2385.0(14)
_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      120(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.941
_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  0.0679
_diffrn_reflns_av_sigmaI/netI    0.0564
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28346
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.01
_diffrn_reflns_theta_min         1.63
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    5.488
_exptl_absorpt_correction_T_max  0.688
_exptl_absorpt_correction_T_min  0.565
_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    1.609
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         7.519
_refine_diff_density_min         -2.453
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         5974
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0500
_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^)+(0.0364P)^2^+11.3050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1067
_reflns_number_gt                5094
_reflns_number_total             5974
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200371r_si_001.cif
_cod_data_source_block           mae364as
_cod_original_cell_volume        2385.1(14)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4064861