Facile Synthesis of Bifunctional Ligands using LiCH2PPh2═NPh Obtained from [PhNH−PPh3+][Br−]
Cao, Thi-Phuong-Anh; Payet, Elina; Auffrant, Audrey; Le Goff, Xavier F.; Le Floch, Pascal; Organometallics 29 (2010) 3991–; doi:10.1021/om100695b

data_4066900
_publ_section_title
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 Facile Synthesis of Bifunctional Ligands using LiCH2PPh2&#x2550;NPh
 Obtained from [PhNH&#x2212;PPh3+][Br&#x2212;]
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_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              3991
_journal_paper_doi               10.1021/om100695b
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C22 H27 N P Si, 0.5Br, 0.5Cl'
_chemical_formula_sum            'C22 H27 Br0.5 Cl0.5 N P Si'
_chemical_formula_weight         422.19
_chemical_name_systematic
; 
 ? 
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_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 108.329(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.378(1)
_cell_length_b                   11.475(1)
_cell_length_c                   22.068(1)
_cell_measurement_reflns_used    4987
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     4417.8(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0458
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15402
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         3.30
_exptl_absorpt_coefficient_mu    1.150
_exptl_absorpt_correction_T_max  0.8744
_exptl_absorpt_correction_T_min  0.7699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo/Scalepack (Otwinowski & Minor, 1996)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         6324
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0385P)^2^+0.3164P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0872
_reflns_number_gt                4621
_reflns_number_total             6324
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100695b_si_002.cif
_cod_data_source_block           ep561
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_original_sg_symbol_H-M      'C2/c     '
_cod_original_formula_sum        'C22 H27 Br0.50 Cl0.50 N P Si'
_cod_database_code               4066900