Reaction of tris[(diphenylphosphino)dimethylsilyl]methane with molybdenum hexacarbonyl and deprotonation to give a salt with a planar carbanion. Crystal structures of (Ph2PMe2Si)3CH and [Li(tmen)2][C(SiMe2PPh2)3], tmen = N,N,N ′,N ′-tetramethylethane-1,2-diamine
Avent, Anthony G.; Bonafoux, Dominique; Eaborn, Colin; Gupta, Sushil K.; Hitchcock, Peter B.; Smith, J. David; Journal of the Chemical Society, Dalton Transactions  (1999) 831–; doi:10.1039/a808971j

data_7027185
_publ_section_title
;
 Reaction of tris[(diphenylphosphino)dimethylsilyl]methane with molybdenum
 hexacarbonyl and deprotonation to give a salt with a planar carbanion.
 Crystal structures of (Ph2PMe2Si)3CH and [Li(tmen)2][C(SiMe2PPh2)3],
 tmen&#x2005;=&#x2005;N,N,N&#x200A;&#x2032;,N&#x200A;&#x2032;-tetramethylethane-1,2-diamine
;
_journal_issue                   6
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              831
_journal_paper_doi               10.1039/a808971j
_journal_year                    1999
_chemical_formula_structural     '[Li(tmeda)2][C(SiMe2PPh2)3]'
_chemical_formula_sum            'C55 H80 Li N4 P3 Si3'
_chemical_formula_weight         981.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.78(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.023(4)
_cell_length_b                   16.592(4)
_cell_length_c                   23.174(11)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7
_cell_volume                     5776(3)
_computing_cell_refinement       'Enraf-Nonius CAD4'
_computing_data_collection       'Enraf-Nonius CAD4'
_computing_molecular_graphics    'CAMERON (Watkin and Pearce,1993)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       ' Enraf-Nonius CAD4'
_diffrn_measurement_method       \w--2\q
_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  0.0698
_diffrn_reflns_av_sigmaI/netI    0.1873
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            8371
_diffrn_reflns_theta_max         22.99
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.202
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.088
_refine_ls_goodness_of_fit_obs   1.269
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         8026
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_restrained_S_obs      1.269
_refine_ls_R_factor_all          0.1887
_refine_ls_R_factor_obs          0.0897
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+13.9776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1789
_refine_ls_wR_factor_obs         0.1445
_reflns_number_observed          4106
_reflns_number_total             8027
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            808971jsup1.cif
_cod_data_source_block           jds-a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+13.9776P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+13.9776P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5775.9(34)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7027185