SET Oxidation of Li/X Phosphinidenoid Complexes by TEMPO
Nesterov, Vitaly; Schwieger, Sebastian; Schnakenburg, Gregor; Grimme, Stefan; Streubel, Rainer; Organometallics 31 (2012) 3457–; doi:10.1021/om300099g

data_4078232
_publ_section_title
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 SET Oxidation of Li/X Phosphinidenoid Complexes by TEMPO
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_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              3457
_journal_paper_doi               10.1021/om300099g
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C20 H35 F Li O10 P Si2 W'
_chemical_formula_sum            'C20 H35 F Li O10 P Si2 W'
_chemical_formula_weight         732.42
_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                91.249(2)
_cell_angle_beta                 93.490(2)
_cell_angle_gamma                92.907(2)
_cell_formula_units_Z            4
_cell_length_a                   10.1458(9)
_cell_length_b                   16.7946(15)
_cell_length_c                   17.6451(15)
_cell_measurement_reflns_used    4896
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.93
_cell_measurement_theta_min      2.38
_cell_volume                     2996.3(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'Bruker X8-KappaApexII'
_diffrn_measurement_method       '\f and \w CCD rotation images, thin slices'
_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  0.1141
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            33689
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.16
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.040
_exptl_absorpt_correction_T_max  0.6626
_exptl_absorpt_correction_T_min  0.3046
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Twinabs 2009/2, Bruker AXS 2009'
_exptl_crystal_colour            'light yellowish'
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.11
_refine_diff_density_max         4.048
_refine_diff_density_min         -2.690
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     691
_refine_ls_number_reflns         10252
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0721P)^2^+27.1405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1329
_refine_ls_wR_factor_ref         0.1363
_reflns_number_gt                9807
_reflns_number_total             10252
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300099g_si_001.cif
_cod_data_source_block           Greg1605_0t2
_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.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' 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 
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_cod_database_code               4078232