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_4068783
_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         'C50.00 H44.00 Cl2 O3 Os P2,1.25CH2CL2'
_chemical_formula_sum            'C51.25 H46.5 Cl4.5 O3 Os P2'
_chemical_formula_weight         1122.05
_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                102.2530(10)
_cell_angle_beta                 100.8660(10)
_cell_angle_gamma                111.483(3)
_cell_formula_units_Z            2
_cell_length_a                   12.0519(7)
_cell_length_b                   13.0418(7)
_cell_length_c                   18.7115(8)
_cell_measurement_reflns_used    8790
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.1136
_cell_measurement_theta_min      2.2746
_cell_volume                     2557.2(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0723
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17660
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    2.830
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91443
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1121
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.719
_refine_diff_density_min         -1.100
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         8798
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0685P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1198
_refine_ls_wR_factor_ref         0.1227
_reflns_number_gt                7040
_reflns_number_total             8798
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8010867_si_005.cif
_cod_data_source_block           complex6
_cod_original_formula_sum        'C51.25 H46.50 Cl4.50 O3 Os P2'
_cod_database_code               4068783