Nine-Membered Osmacycles Derived from Metathesis Reactions between Alkynes and an Osmafuran
Lin, Yumei; Gong, Lei; Xu, Hui; He, Xumin; Wen, Ting Bin; Xia, Haiping; Organometallics 28 (2009) 1524–; doi:10.1021/om8010867

data_4068781
_publ_section_title
;
 Nine-Membered Osmacycles Derived from Metathesis Reactions between
 Alkynes and an Osmafuran
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1524
_journal_paper_doi               10.1021/om8010867
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety
'C57 H48 Cl2 O2 Os P2&#x00A3;&#x00AC;H2O,0.5CH2Cl2'
_chemical_formula_sum            'C57.5 H51 Cl3 O3 Os P2'
_chemical_formula_weight         1148.47
_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                104.013(3)
_cell_angle_beta                 105.535(3)
_cell_angle_gamma                102.005(3)
_cell_formula_units_Z            2
_cell_length_a                   13.3346(5)
_cell_length_b                   13.6669(4)
_cell_length_c                   16.7686(5)
_cell_measurement_reflns_used    10516
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.1306
_cell_measurement_theta_min      2.3160
_cell_volume                     2732.29(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0732
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21566
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    2.580
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94134
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1154
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         3.828
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         9496
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1081P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1634
_refine_ls_wR_factor_ref         0.1695
_reflns_number_gt                7587
_reflns_number_total             9496
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8010867_si_003.cif
_cod_data_source_block           complex4
_cod_original_cell_volume        2732.29(15)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C57.50 H51 Cl3 O3 Os P2'
_cod_database_code               4068781