Slow epimerization of stereochemically rigid diastereomers of the equatorially substituted cluster [Os3H2(??3-S)(CO)8{(S)-PhCHMeNH2}]
Deeming, Antony J.; Forth, Caroline S.; Hogarth, Graeme; Markham, David; Prince, Jade O.; Steed, Jonathan W.; Chemical Communications  (2002) 2230–; doi:10.1039/b203611h

data_7114458
_publ_section_title
;
 Slow epimerization of stereochemically rigid diastereomers of the
 equatorially substituted cluster [Os3H2(??3-S)(CO)8{(S)-PhCHMeNH2}]
;
_journal_issue                   19
_journal_name_full               'Chemical Communications'
_journal_page_first              2230
_journal_paper_doi               10.1039/b203611h
_journal_year                    2002
_chemical_formula_sum            'C16 H13 N O8 Os3 S'
_chemical_formula_weight         949.93
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.605(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4018(4)
_cell_length_b                   20.5782(11)
_cell_length_c                   11.5621(5)
_cell_measurement_temperature    110(2)
_cell_volume                     2226.25(18)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       Collect
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'XSeed (Barbour, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  KAPPACCD
_diffrn_measurement_method       '1.5o phi & omega frames'
_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  0.1607
_diffrn_reflns_av_sigmaI/netI    0.1769
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11460
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    17.213
_exptl_absorpt_correction_T_max  0.0990
_exptl_absorpt_correction_T_min  0.0788
_exptl_absorpt_correction_type   scaleapck
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.834
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         3.964
_refine_diff_density_min         -3.821
_refine_diff_density_rms         0.563
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_coef       0.00171(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         7126
_refine_ls_number_restraints     457
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0683
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0868P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1731
_refine_ls_wR_factor_ref         0.1781
_reflns_number_gt                6544
_reflns_number_total             7126
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b203611h.txt
_cod_data_source_block           os3chira
_cod_original_sg_symbol_H-M      P21
_cod_database_code               7114458