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_4068779
_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         'C59 H51 Cl2 O2 Os P3,2CH2CL2'
_chemical_formula_sum            'C61 H55 Cl6 O2 Os P3'
_chemical_formula_weight         1315.86
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 104.597(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6801(3)
_cell_length_b                   21.1499(4)
_cell_length_c                   21.4017(4)
_cell_measurement_reflns_used    6925
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.2010
_cell_measurement_theta_min      2.1545
_cell_volume                     5554.3(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0440
_diffrn_reflns_av_sigmaI/netI    0.0838
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            16374
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    2.715
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86842
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brownish
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.581
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.006(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.876
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     656
_refine_ls_number_reflns         7315
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      0.876
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0278
_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^)+(0.0002P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0372
_refine_ls_wR_factor_ref         0.0385
_reflns_number_gt                5881
_reflns_number_total             7315
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8010867_si_001.cif
_cod_data_source_block           complex1
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               4068779