Unusual C‒H bond activation—aldol condensation of aromatic aldehydes with the methyl group of a carbene-like triosmium cluster
Sergey P. Tunik; Irina A. Balova; Maxim E. Borovitov; Ebbe Nordlander; Matti Haukka; Tapani A. Pakkanen; J. Chem. Soc., Dalton Trans.  (2002) 827–828; doi:10.1039/b200707j

data_7011513
_publ_section_title
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 Unusual C--H bond activation---aldol condensation of aromatic
 aldehydes with the methyl group of a carbene-like triosmium cluster
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_journal_issue                   6
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              827
_journal_page_last               828
_journal_paper_doi               10.1039/b200707j
_journal_year                    2002
_chemical_formula_moiety         HOs3(CO)10(C13H9O)
_chemical_formula_sum            'C23 H10 O11 Os3'
_chemical_formula_weight         1032.91
_chemical_name_common            HOs3(CO)10(C13H9O)
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.8138(6)
_cell_angle_beta                 91.0860(7)
_cell_angle_gamma                96.8966(8)
_cell_formula_units_Z            2
_cell_length_a                   9.52160(10)
_cell_length_b                   9.66420(10)
_cell_length_c                   13.9842(2)
_cell_measurement_reflns_used    22008
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      0.998
_cell_volume                     1264.82(3)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP in SHELXTL v.5.1 (Bruker Axs, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF99 (Beurskens et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19096
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         3.71
_exptl_absorpt_coefficient_mu    15.090
_exptl_absorpt_correction_T_max  0.13092
_exptl_absorpt_correction_T_min  0.08487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Xprep in Shelxtl v. 5.1 (Bruker AXS, 1998)'
_exptl_crystal_colour            'greenish yellow'
_exptl_crystal_density_diffrn    2.712
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.400
_refine_diff_density_min         -1.509
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4929
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0225
_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^)+(0.0169P)^2^+3.7584P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0556
_reflns_number_gt                4735
_reflns_number_total             4929
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b200707j.txt
_cod_data_source_block           HOs3(CO)10(C13H9O)
_cod_depositor_comments
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The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
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_cod_database_code               7011513