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_4111012
_publ_section_title
;
 Osmabenzenes from the Reactions of a Dicationic Osmabenzyne Complex
;
_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         'C55 H53 N2 O Os P2 Si, C F3 S O3, H2 O'
_chemical_formula_sum            'C56 H55 F3 N2 O5 Os P2 S Si'
_chemical_formula_weight         1205.31
_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                 97.087(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.857(3)
_cell_length_b                   19.181(4)
_cell_length_c                   19.294(4)
_cell_measurement_temperature    173(2)
_cell_volume                     5089.0(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1063
_diffrn_reflns_av_sigmaI/netI    0.1253
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30361
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    2.696
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.802551
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Brownish-red
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       Bar
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.469
_refine_diff_density_min         -2.351
_refine_diff_density_rms         0.181
_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     629
_refine_ls_number_reflns         9455
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1082
_refine_ls_R_factor_gt           0.0564
_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^)+(0.0549P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1322
_reflns_number_gt                5971
_reflns_number_total             9455
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja064570wsi20060819_033529.cif
_cod_data_source_block           bin49_Compound3
_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_original_cell_volume        5089.1(17)
_cod_database_code               4111012