Normal and Abnormal NHC Coordination in [Os4(μ-H)4(CO)11(IMes)] and Exhaustive Dehydrogenation of an IMes Methyl Group
Cooke, Craig E.; Jennings, Michael C.; Pomeroy, Roland K.; Clyburne, Jason A. C.; Organometallics 26 (2007) 6059–; doi:10.1021/om7007293

data_4073926
_publ_section_title
;
 Normal and Abnormal NHC Coordination in [Os4(\m-H)4(CO)11(IMes)] and
 Exhaustive Dehydrogenation of an IMes Methyl Group
;
_journal_issue                   25
_journal_name_full               Organometallics
_journal_page_first              6059
_journal_paper_doi               10.1021/om7007293
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C32 H28 N2 O11 Os4'
_chemical_formula_sum            'C32 H28 N2 O11 Os4'
_chemical_formula_weight         1377.36
_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                96.672(2)
_cell_angle_beta                 96.046(2)
_cell_angle_gamma                90.049(2)
_cell_formula_units_Z            4
_cell_length_a                   14.0262(5)
_cell_length_b                   15.9043(6)
_cell_length_c                   16.2287(6)
_cell_measurement_reflns_used    46463
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.04
_cell_volume                     3575.4(2)
_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      150(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_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  0.069
_diffrn_reflns_av_sigmaI/netI    0.0537
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            37795
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.229
_exptl_absorpt_correction_T_max  0.5364
_exptl_absorpt_correction_T_min  0.0825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         7.890
_refine_diff_density_min         -4.527
_refine_diff_density_rms         0.546
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     894
_refine_ls_number_reflns         12034
_refine_ls_number_restraints     782
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0672
_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^)+(0.1544P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1781
_refine_ls_wR_factor_ref         0.1878
_reflns_number_gt                10315
_reflns_number_total             12034
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om7007293-file001.cif
_cod_data_source_block           07113scale
_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_database_code               4073926