Efficient Synthesis of the Os−Os Dimers [Cp(CO)2Os]2, [Cp*(CO)2Os]2, and [(iPr4C5H)(CO)2Os]2and Computational Studies on the Relative Stabilities of Their Geometrical Isomers
Zhang, Jie; Huang, Kuo-Wei; Szalda, David J.; Bullock, R. Morris; Organometallics 25 (2006) 2209–; doi:10.1021/om060075x

data_4075160
_publ_section_title
;
 Efficient Synthesis of the Os&#x2212;Os Dimers [Cp(CO)2Os]2,
 [Cp*(CO)2Os]2, and [(iPr4C5H)(CO)2Os]2and Computational Studies on the
 Relative Stabilities of Their Geometrical Isomers
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2209
_journal_paper_doi               10.1021/om060075x
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C24 H30 O4 Os2'
_chemical_formula_sum            'C24 H30 O4 Os2'
_chemical_formula_weight         762.88
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.83(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.792(2)
_cell_length_b                   8.3580(17)
_cell_length_c                   14.374(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32
_cell_measurement_theta_min      15
_cell_volume                     1159.1(4)
_computing_cell_refinement       'CAD-4 (Enraf-Nonius, 1977)'
_computing_data_collection       'CAD-4 (Enraf-Nonius, 1977)'
_computing_data_reduction        'XCAD4VAX (Sheldrick, 1993)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Enraf Nonius CAD-4'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0711
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2382
_diffrn_reflns_theta_full        75.16
_diffrn_reflns_theta_max         75.16
_diffrn_reflns_theta_min         6.15
_diffrn_standards_decay_%        <2%
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    20.601
_exptl_absorpt_correction_T_max  1.834
_exptl_absorpt_correction_T_min  .548
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
Parkin, S., Moezzi, B., and Hope, H.,  J. Appl. Cryst., 1995, 28, 53-56. 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.186
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.184
_refine_diff_density_min         -5.115
_refine_diff_density_rms         0.263
_refine_ls_extinction_coef       0.00130(14)
_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   1.063
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         2382
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.077
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0552P)^2^+6.3428P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1067
_reflns_number_gt                1975
_reflns_number_total             2382
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060075xsi20060124_111107.cif
_cod_data_source_block           osco719
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'refu' changed to 'refU'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
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_sg_symbol_H-M      P21/n
_cod_database_code               4075160