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_4076506
_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            'C73 H83 B2 F24 N6 Os P'
_chemical_formula_weight         1743.24
_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                93.825(2)
_cell_angle_beta                 108.678(2)
_cell_angle_gamma                104.976(2)
_cell_formula_units_Z            2
_cell_length_a                   13.397(2)
_cell_length_b                   16.445(3)
_cell_length_c                   18.943(3)
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      2
_cell_volume                     3768.0(11)
_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 8.33
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_device_type  'Bruker APEX II DUO 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  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0516
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            40766
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.55
_diffrn_reflns_theta_min         1.15
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.819
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.699
_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+ v. 7.56a (Bruker AXS, 2008).
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         4.595
_refine_diff_density_min         -1.322
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     958
_refine_ls_number_reflns         18897
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0779P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1251
_reflns_number_gt                15887
_reflns_number_total             18897
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201272q_si_001.cif
_cod_data_source_block           enriquen7b
_cod_original_cell_volume        3768.1(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4076506