Stepwise activation of 'non-innocent' Cp* substituents ‒ a Cp* based cascade reaction
Markus Stubenhofer; Giuliano Lassandro; Gabor Balazs; Alexey Y. Timoshkin; Manfred Scheer; Chem.Commun. 48 (2012) 7262–7264; doi:10.1039/c2cc32690f

data_7107991
_publ_section_title
;
 Stepwise activation of 'non-innocent' Cp* substituents -- a Cp* based
 cascade reaction
;
_journal_coden_Cambridge         0182
_journal_issue                   58
_journal_name_full               Chem.Commun.
_journal_page_first              7262
_journal_page_last               7264
_journal_paper_doi               10.1039/c2cc32690f
_journal_volume                  48
_journal_year                    2012
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C20 H17 O10 P3 W2'
_chemical_formula_sum            'C20 H17 O10 P3 W2'
_chemical_formula_weight         877.93
_chemical_name_systematic        ?
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                71.461(5)
_cell_angle_beta                 89.764(4)
_cell_angle_gamma                64.716(5)
_cell_formula_units_Z            2
_cell_length_a                   9.4184(5)
_cell_length_b                   10.4395(5)
_cell_length_c                   15.6135(8)
_cell_measurement_reflns_used    3446
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      70.5998
_cell_measurement_theta_min      4.8496
_cell_volume                     1300.46(14)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug 2 2010,13:00:58)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug 2 2010,13:00:58)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug 2 2010,13:00:58)
;
_computing_molecular_graphics    'SXGRAPH (Farrugia, 1999)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SUPERFLIP (Palatinus, Chapuis, 2007)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.3546
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'SuperNova,Single source at offset,Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_sigmaI/netI    0.0610
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8886
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        70.78
_diffrn_reflns_theta_max         70.78
_diffrn_reflns_theta_min         4.86
_exptl_absorpt_coefficient_mu    18.315
_exptl_absorpt_correction_T_max  0.638
_exptl_absorpt_correction_T_min  0.362
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug 2 2010,13:00:58)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.242
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.0804
_exptl_crystal_size_mid          0.0645
_exptl_crystal_size_min          0.0268
_refine_diff_density_max         1.178
_refine_diff_density_min         -2.646
_refine_diff_density_rms         0.208
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         4805
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0664P)^2^+1.4103P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1179
_refine_ls_wR_factor_ref         0.1263
_reflns_number_gt                3975
_reflns_number_total             4805
_reflns_threshold_expression     >2\s(i)
_cod_data_source_file            c2cc32690f.txt
_cod_data_source_block           MS340
_cod_database_code               7107991