Synthesis and Characterization of Triosmium Clusters Containing the Bidentate Ligand Ph2PCH2CH2SMe: Detection of an Isomerization Reaction Involving Bridging and Chelating Ligand Coordination Modes
Persson, Roger; Monari, Magda; Gobetto, Roberto; Russo, Andrea; Aime, Silvio; Calhorda, Maria José; Nordlander, Ebbe; Organometallics 20 (2001) 4150–; doi:10.1021/om010223d

data_4077325
_publ_section_title
;
 Synthesis and Characterization of Triosmium Clusters Containing the
 Bidentate Ligand Ph2PCH2CH2SMe:&#x00A0; Detection of an Isomerization
 Reaction Involving Bridging and Chelating Ligand Coordination Modes
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              4150
_journal_paper_doi               10.1021/om010223d
_journal_volume                  20
_journal_year                    2001
_chemical_formula_sum            'C25 H17 O10 Os3 P S'
_chemical_formula_weight         1111.02
_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
_cell_angle_alpha                93.02(3)
_cell_angle_beta                 95.65(4)
_cell_angle_gamma                111.47(4)
_cell_formula_units_Z            2
_cell_length_a                   11.415(7)
_cell_length_b                   11.413(3)
_cell_length_c                   11.940(5)
_cell_measurement_temperature    293(2)
_cell_volume                     1433.9(12)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf Nonius CAD4'
_diffrn_measurement_method       /w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0587
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8296
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    13.441
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.573
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.080
_refine_diff_density_min         -2.374
_refine_diff_density_rms         0.351
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.027
_refine_ls_goodness_of_fit_obs   1.147
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         8276
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_restrained_S_obs      1.147
_refine_ls_R_factor_all          0.1016
_refine_ls_R_factor_obs          0.0526
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0889P)^2^+9.9923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1606
_refine_ls_wR_factor_obs         0.1378
_reflns_number_observed          5328
_reflns_number_total             8296
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om010223d.cif
_cod_data_source_block           os3psbridg
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

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

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0889P)^2^+9.9923P] 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^)+(0.0889P)^2^+9.9923P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1433.9(11)
_cod_original_sg_symbol_H-M      'P 1 bar'
_cod_database_code               4077325