Anti-Markovnikov 1,3-CH Addition of Allenes to Allenes: A Straightforward Method To Prepare Osmium‒Dienylcarbene Complexes
Castro-Rodrigo, Ruth; Esteruelas, Miguel A.; López, Ana M.; Oñate, Enrique; Organometallics 31 (2012) 1991–; doi:10.1021/om201272q

data_4076505
_publ_section_title
;
 Anti-Markovnikov 1,3-CH Addition of Allenes to Allenes: A Straightforward
 Method To Prepare Osmium--Dienylcarbene Complexes
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1991
_journal_paper_doi               10.1021/om201272q
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C68.35 H71.71 B2 Cl0.71 F24 N6 Os P'
_chemical_formula_weight         1701.16
_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                 91.6720(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2854(13)
_cell_length_b                   20.752(2)
_cell_length_c                   28.060(3)
_cell_measurement_reflns_used    6424
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      2
_cell_volume                     7732.8(13)
_computing_cell_refinement       'SAINT+ v. 6.02 (Bruker AXS, 1999)'
_computing_data_collection       'SMART v. 5.625 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.02 (Bruker AXS, 1999)'
_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      173(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1114
_diffrn_reflns_av_sigmaI/netI    0.1154
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            53818
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.794
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.676
_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            green
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             3411
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.635
_refine_diff_density_min         -1.632
_refine_diff_density_rms         0.143
_refine_ls_extinction_coef       0.00132(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     855
_refine_ls_number_reflns         15173
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1363
_refine_ls_R_factor_gt           0.0861
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0904P)^2^+43.1356P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2063
_refine_ls_wR_factor_ref         0.2311
_reflns_number_gt                9485
_reflns_number_total             15173
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201272q_si_001.cif
_cod_data_source_block           enrique62cs
_cod_original_cell_volume        7733.0(13)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4076505