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_4077326
_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           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 111.96(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.661(6)
_cell_length_b                   16.427(9)
_cell_length_c                   11.028(8)
_cell_measurement_temperature    293(2)
_cell_volume                     1455.2(17)
_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  0.0508
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7317
_diffrn_reflns_theta_max         27.96
_diffrn_reflns_theta_min         2.35
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    13.245
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    2.536
_exptl_crystal_description       prism
_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         1.849
_refine_diff_density_min         -1.949
_refine_diff_density_rms         0.170
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.093(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.055
_refine_ls_goodness_of_fit_obs   1.080
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         6971
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.055
_refine_ls_restrained_S_obs      1.081
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_obs          0.0335
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+9.2526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0938
_refine_ls_wR_factor_obs         0.0904
_reflns_number_observed          6207
_reflns_number_total             6976
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om010223d.cif
_cod_data_source_block           os3pschelating
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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^)+(0.0533P)^2^+9.2526P] 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^)+(0.0533P)^2^+9.2526P] 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)
_cod_database_code               4077326