A metal–amide dependent, catalytic C–H functionalisation of triphenylphosphonium methylide
Nako, Adi E.; White, Andrew J. P.; Crimmin, Mark R.; Chemical Science 4 (2013) 691–; doi:10.1039/c2sc21123h

data_1514412
_publ_section_title
;
 A metal--amide dependent, catalytic C--H functionalisation of
 triphenylphosphonium methylide
;
_journal_issue                   2
_journal_name_full               'Chemical Science'
_journal_page_first              691
_journal_paper_doi               10.1039/c2sc21123h
_journal_volume                  4
_journal_year                    2013
_chemical_formula_moiety         'C25 H23 P Si'
_chemical_formula_sum            'C25 H23 P Si'
_chemical_formula_weight         382.49
_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                81.236(2)
_cell_angle_beta                 79.739(2)
_cell_angle_gamma                81.615(2)
_cell_formula_units_Z            8
_cell_length_a                   11.2823(3)
_cell_length_b                   16.8988(4)
_cell_length_c                   22.9869(6)
_cell_measurement_reflns_used    13051
_cell_measurement_temperature    173
_cell_measurement_theta_max      30.7303
_cell_measurement_theta_min      3.0470
_cell_volume                     4230.32(19)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 15.9825
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.842
_diffrn_measurement_device_type  'OD Xcalibur 3'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0516
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            40913
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         30.80
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    0.193
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.943
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
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            'Pale yellow'
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1002
_refine_ls_number_reflns         22303
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0539
_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^)+(0.0565P)^2^+1.5399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1272
_refine_ls_wR_factor_ref         0.1390
_reflns_number_gt                16131
_reflns_number_total             22303
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2sc21123h.txt
_cod_data_source_block           1a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1514412