Reactions of Osmium Hydrido Alkenylcarbyne with Allenoates: Insertion and [3 + 2] Annulation
Zhou, Xiaoxi; He, Xiehua; Lin, Jianfeng; Zhuo, Qingde; Chen, Zhixin; Zhang, Hong; Wang, Jianbo; Xia, Haiping; Organometallics 34 (2015) 1742–; doi:10.1021/acs.organomet.5b00242

data_4087544
_publ_section_title
;
 Reactions of Osmium Hydrido Alkenylcarbyne with Allenoates: Insertion and
 [3 + 2] Annulation
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              1742
_journal_paper_doi               10.1021/acs.organomet.5b00242
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C69 H59 B2 F8 O2 Os P3, C1 Cl3 H1'
_chemical_formula_sum            'C70 H60 B2 Cl3 F8 O2 Os P3'
_chemical_formula_weight         1496.26
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_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                 110.4420(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.7718(8)
_cell_length_b                   23.4779(9)
_cell_length_c                   14.3128(4)
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      55.01
_cell_measurement_theta_min      6.03
_cell_volume                     6225.6(4)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0853
_diffrn_reflns_av_sigmaI/netI    0.0691
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            59993
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    2.326
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4983
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3000
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.051
_refine_diff_density_min         -2.419
_refine_diff_density_rms         0.228
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     779
_refine_ls_number_reflns         14249
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0559
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0824P)^2^+27.0211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1436
_refine_ls_wR_factor_ref         0.1725
_reflns_number_gt                10598
_reflns_number_total             14249
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00242_si_003.cif
_cod_data_source_block           complex_9
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4087544