Osmabenzenes from the Reactions of a Dicationic Osmabenzyne Complex
Wai Yiu Hung; Jun Zhu; Ting Bin Wen; Ka Po Yu; Herman H. Y. Sung; Ian D. Williams; Zhenyang Lin; Guochen Jia; Journal of the American Chemical Society 128 (2006) 13742–13752; doi:10.1021/ja064570w

data_4111013
_publ_section_title
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 Osmabenzenes from the Reactions of a Dicationic Osmabenzyne Complex
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13742
_journal_page_last               13752
_journal_paper_doi               10.1021/ja064570w
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C40 H46 N2 Os P Si2, C F3 O3 S, C H2 Cl2'
_chemical_formula_sum            'C42 H48 Cl2 F3 N2 O3 Os P S Si2'
_chemical_formula_weight         1066.13
_chemical_name_systematic
; 
 ? 
;
_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                104.072(2)
_cell_angle_beta                 101.455(2)
_cell_angle_gamma                95.036(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7215(11)
_cell_length_b                   11.4672(11)
_cell_length_c                   20.273(2)
_cell_measurement_reflns_used    3233
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2.36
_cell_volume                     2345.1(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_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  0.0555
_diffrn_reflns_av_sigmaI/netI    0.1150
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15084
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    3.012
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8231
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       Block
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.371
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         8025
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc 
 [0.00000+1.00000exp(1.30(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0150P)^2^+0.0000sin\q/\l] 
 where P = 0.33333Fo^2^ + 0.66667Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0726
_reflns_number_gt                5734
_reflns_number_total             8025
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja064570wsi20060819_033556.cif
_cod_data_source_block           yiu33_Compound6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'Constr' changed to 'constr'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               4111013