NHC Complexes of Osmium Clusters: A Structural and Reactivity Study
Cooke, Craig E.; Jennings, Michael C.; Katz, Michael J.; Pomeroy, R. K.; Clyburne, Jason A. C.; Organometallics 27 (2008) 5777–; doi:10.1021/om800577x

data_4072091
_publ_section_title
;
 NHC Complexes of Osmium Clusters: A Structural and Reactivity Study
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5777
_journal_paper_doi               10.1021/om800577x
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         '2(C30 H25 Cl N2 O9 Os3), C7 H8'
_chemical_formula_sum            'C33.5 H29 Cl N2 O9 Os3'
_chemical_formula_weight         1209.64
_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-97
_cell_angle_alpha                80.968(2)
_cell_angle_beta                 81.369(2)
_cell_angle_gamma                71.935(2)
_cell_formula_units_Z            2
_cell_length_a                   8.3651(2)
_cell_length_b                   10.8743(3)
_cell_length_c                   20.4975(7)
_cell_measurement_reflns_used    6205
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      1.70
_cell_volume                     1740.42(9)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 2001)'
_computing_publication_material  SHELXTL/PC
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_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  0.054
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21096
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.58
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.056
_exptl_absorpt_correction_T_max  0.3275
_exptl_absorpt_correction_T_min  0.1899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1122
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.942
_refine_diff_density_min         -2.338
_refine_diff_density_rms         0.242
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         7106
_refine_ls_number_restraints     405
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0442P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0836
_reflns_number_gt                6040
_reflns_number_total             7106
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om800577x_si_011.cif
_cod_data_source_block           05119
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_formula_sum        'C33.50 H29 Cl N2 O9 Os3'
_cod_database_code               4072091