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_1514413
_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         'C50 H70 Li2 N2 P2 Si4'
_chemical_formula_sum            'C50 H70 Li2 N2 P2 Si4'
_chemical_formula_weight         887.26
_chemical_name_systematic
;
?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 100.652(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.8666(4)
_cell_length_b                   22.2888(5)
_cell_length_c                   25.4992(6)
_cell_measurement_reflns_used    13346
_cell_measurement_temperature    173
_cell_measurement_theta_max      28.8484
_cell_measurement_theta_min      2.9590
_cell_volume                     10538.0(4)
_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 0.988
_diffrn_measured_fraction_theta_max 0.863
_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  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            41245
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         28.91
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    0.207
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.941
_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            Colourless
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             3808
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 7777 Friedel pairs'
_refine_ls_abs_structure_Flack   0.44(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1116
_refine_ls_number_reflns         19768
_refine_ls_number_restraints     106
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0596
_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^)+(0.0986P)^2^+3.6605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1549
_refine_ls_wR_factor_ref         0.1685
_reflns_number_gt                16161
_reflns_number_total             19768
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2sc21123h.txt
_cod_data_source_block           2a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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      Cc
_cod_database_code               1514413