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_4068784
_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         'C68 H58 Cl1  O3 Os P3,CH2CL2'
_chemical_formula_sum            'C69 H60 Cl3 N0 O3 Os P3'
_chemical_formula_weight         1326.63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 95.6750(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9807(2)
_cell_length_b                   25.0138(4)
_cell_length_c                   16.0283(2)
_cell_measurement_temperature    173(2)
_cell_volume                     5976.75(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31031
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    2.395
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83695
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2680
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.959
_refine_diff_density_min         -0.796
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         10489
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0285
_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^)+(0.0113P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0433
_refine_ls_wR_factor_ref         0.0448
_reflns_number_gt                7940
_reflns_number_total             10489
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8010867_si_006.cif
_cod_data_source_block           complex7
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4068784