Reactions of an Osmium Bis(dihydrogen) Complex under Ethylene: Phosphine Addition to a C‒C Double Bond and C‒H Bond Activation of Fluoroarenes
Bajo, Sonia; Esteruelas, Miguel A.; López, Ana M.; Oñate, Enrique; Organometallics 30 (2011) 5710–; doi:10.1021/om2005854

data_4065145
_publ_section_title
;
 Reactions of an Osmium Bis(dihydrogen) Complex under Ethylene: Phosphine
 Addition to a C--C Double Bond and C--H Bond Activation of Fluoroarenes
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5710
_journal_paper_doi               10.1021/om2005854
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C22H39B2F4N6OsP x 0.85 CH2Cl2 x 0.15 H2O'
_chemical_formula_sum            'C22.85 H41 B2 Cl1.7 F4 N6 O0.15 Os P'
_chemical_formula_weight         781.27
_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                 101.6800(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7811(4)
_cell_length_b                   18.3167(8)
_cell_length_c                   18.7410(9)
_cell_measurement_reflns_used    9947
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     2951.9(2)
_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_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36308
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.84
_diffrn_reflns_theta_min         1.57
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.579
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.578
_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.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1549
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.601
_refine_diff_density_min         -2.226
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         7256
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0442P)^2^+6.3450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0855
_reflns_number_gt                6231
_reflns_number_total             7256
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2005854_si_001.cif
_cod_data_source_block           enrique18as
_cod_original_sg_symbol_H-M      P21/n
_cod_original_formula_sum        'C22.85 H41 B2 Cl1.70 F4 N6 O0.15 Os P'
_cod_database_code               4065145