Cleavage of Both C(sp3)-C(sp2) Bonds of Alkylidenecyclopropanes: Formation of Ethylene-Osmium-Vinylidene Complexes
Ruth Castro-Rodrigo; Miguel A. Esteruelas; Ana M. López; Fernando López; José L. Mascareñas; Montserrat Oliván; Enrique Oñate; Lucía Saya; Lara Villarino; Journal of the American Chemical Society 132 (2010) 454–455; doi:10.1021/ja909240q

data_4101792
_publ_contact_author
;
  Dr. Enrique O\~nate Rodr\'iguez
  Departamento de Qu\'imica Inorg\'anica - I.C.M.A.
  Facultad de Ciencias
  Universidad de Zaragoza - C.S.I.C.
  50009 Zaragoza, Spain
;
_publ_contact_author_email       enriqueo@posta.unizar.es
_publ_section_title
;
 Cleavage of Both C(sp3)-C(sp2) Bonds of Alkylidenecyclopropanes:
 Formation of Ethylene-Osmium-Vinylidene Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              454
_journal_page_last               455
_journal_paper_doi               10.1021/ja909240q
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C56 H71 B2 N6 O Os P'
_chemical_formula_weight         1086.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.519(2)
_cell_angle_beta                 96.857(2)
_cell_angle_gamma                118.8300(10)
_cell_formula_units_Z            2
_cell_length_a                   13.1940(12)
_cell_length_b                   13.2046(12)
_cell_length_c                   17.0692(15)
_cell_measurement_reflns_used    7345
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     2568.9(4)
_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 0.981
_diffrn_measured_fraction_theta_max 0.907
_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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24537
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.74
_diffrn_reflns_theta_min         1.21
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    2.558
_exptl_absorpt_correction_T_max  0.822
_exptl_absorpt_correction_T_min  0.697
_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            violet
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.554
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         12077
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+0.9614P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0770
_reflns_number_gt                10826
_reflns_number_total             12077
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja909240q_si_001_2.cif
_cod_data_source_block           mae363as
_cod_database_code               4101792