Trinuclear clusters of osmium containing monodentate, chelating and orthometallated forms of 2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (BINAP)
Deeming, Antony J.; Stchedroff, Marc; Journal of the Chemical Society, Dalton Transactions  (1998) 3819–; doi:10.1039/a806430j

data_7027056
_publ_section_title
;
 Trinuclear clusters of osmium containing monodentate, chelating and
 orthometallated forms of
 2,2&#x2032;-bis(diphenylphosphino)-1,1&#x2032;-binaphthyl (BINAP)
;
_journal_issue                   22
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3819
_journal_paper_doi               10.1039/a806430j
_journal_year                    1998
_chemical_formula_structural     Os3H(BINAP-H)(CO)8
_chemical_formula_sum            'C52 H32 O8 Os3 P2'
_chemical_formula_weight         1417.32
_chemical_name_systematic
; 
 (orthometallated BINAP)hydridooctacarbonyltriosmium
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.661(4)
_cell_length_b                   21.265(16)
_cell_length_c                   24.214(16)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      16
_cell_volume                     5489(6)
_computing_cell_refinement       SHELXTL-PLUS
_computing_data_collection       SHELXTL-PLUS
_computing_data_reduction        SHELXTL-PLUS
_computing_molecular_graphics    SHELXTL-PLUS
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Nicolet 3v/m'
_diffrn_measurement_method       'omega scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0571
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5266
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.55
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.032
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.728
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_description       block
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.27
_refine_diff_density_max         3.929
_refine_diff_density_min         -2.096
_refine_diff_density_rms         0.389
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.075
_refine_ls_goodness_of_fit_obs   1.115
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         5259
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_restrained_S_obs      1.115
_refine_ls_R_factor_all          0.1131
_refine_ls_R_factor_obs          0.0891
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0866P)^2^+478.4703P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2727
_refine_ls_wR_factor_obs         0.2411
_reflns_number_observed          4231
_reflns_number_total             5266
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            806430jsup1.cif
_cod_data_source_block           str599
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0866P)^2^+478.4703P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0866P)^2^+478.4703P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               7027056