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_4078233
_publ_section_title
;
 SET Oxidation of Li/X Phosphinidenoid Complexes by TEMPO
;
_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         'C17 H28 Li O11 P Si W, C4 H10 O'
_chemical_formula_sum            'C21 H38 Li O12 P Si W'
_chemical_formula_weight         732.36
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 119.045(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7563(6)
_cell_length_b                   20.7282(7)
_cell_length_c                   12.9136(6)
_cell_measurement_reflns_used    8547
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.90
_cell_measurement_theta_min      2.95
_cell_volume                     2985.1(2)
_computing_cell_refinement       'STOE X-AREA (STOE&CIE, 2008)'
_computing_data_collection       'STOE X-AREA (STOE&CIE, 2008)'
_computing_data_reduction        'STOE X-RED (STOE&CIE, 2008)'
_computing_molecular_graphics    'DIAMOND2.1c (Brandenburg, 1999)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details      ' 139 frames, detector distance = 105 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18560
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         3.28
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    4.017
_exptl_absorpt_correction_T_max  0.3905
_exptl_absorpt_correction_T_min  0.2190
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'XShape, STOE&CIE, 2008'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.51
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.138
_refine_diff_density_min         -1.530
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         7080
_refine_ls_number_restraints     159
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0752
_reflns_number_gt                5746
_reflns_number_total             7080
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300099g_si_001.cif
_cod_data_source_block           Seb126
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4078233