Synthesis of Five-Membered Osmacycles with Osmium–Vinyl Bonds from Hydrido Alkenylcarbyne Complexes
Chen, Jinxiang; Huang, Zi-Ao; Hua, Yuhui; Zhang, Hong; Xia, Haiping; Organometallics 34 (2015) 340–; doi:10.1021/om501076z

data_4085098
_publ_section_title
;
 Synthesis of Five-Membered Osmacycles with Osmium--Vinyl Bonds from
 Hydrido Alkenylcarbyne Complexes
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              340
_journal_paper_doi               10.1021/om501076z
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C65 H50 B Cl2 F4 N2 O2 Os P3,CH9Cl2O3.5'
_chemical_formula_sum            'C66 H59 B Cl4 F4 N2 O5.5 Os P3'
_chemical_formula_weight         1479.87
_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                 109.74(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.201(3)
_cell_length_b                   22.916(5)
_cell_length_c                   17.849(4)
_cell_measurement_reflns_used    52608
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      55.02
_cell_measurement_theta_min      6.01
_cell_volume                     6622(3)
_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_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  0.0795
_diffrn_reflns_av_sigmaI/netI    0.0496
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            79589
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    2.221
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6019
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2972
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.483
_refine_diff_density_min         -1.956
_refine_diff_density_rms         0.190
_refine_ls_extinction_coef       0.0044(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    conster
_refine_ls_matrix_type           full
_refine_ls_number_parameters     785
_refine_ls_number_reflns         11641
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0646
_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^)+(0.1331P)^2^+10.2314P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1827
_refine_ls_wR_factor_ref         0.2127
_reflns_number_gt                9233
_reflns_number_total             11641
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501076z_si_002.cif
_cod_data_source_block           Coumpound_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2935 2014-11-11 08:27:57Z andrius 

 Adding full bibliography for 4085098--4085105.cif.
;
_cod_original_cell_volume        6622(2)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C66 H59 B Cl4 F4 N2 O5.50 Os P3'
_cod_database_code               4085098