Synthesis of Phosphorus(V)-Stabilized Geminal Dianions. The Cases of Mixed P═X/P→BH3(X = S, O) and P═S/SiMe3Derivatives
Heuclin, Hadrien; Fustier-Boutignon, Marie; Ho, Samuel Ying-Fu; Goff, Xavier-Frédéric Le; Carenco, Sophie; So, Cheuk-Wai; Mézailles, Nicolas; Organometallics 32 (2013) 498–; doi:10.1021/om300954a

data_4079844
_publ_section_title
;
 Synthesis of Phosphorus(V)-Stabilized Geminal Dianions. The Cases of
 Mixed P&#x2550;X/P\\rightarrow BH3(X = S, O) and
 P&#x2550;S/SiMe3Derivatives
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              498
_journal_paper_doi               10.1021/om300954a
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C78 H81 B3 Li4 O4 P6 Si, 1/2(C7H8)'
_chemical_formula_sum            'C81.5 H85 B3 Li4 O4 P6 Si'
_chemical_formula_weight         1402.59
_chemical_name_systematic
; 
 ? 
;
_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                105.110(1)
_cell_angle_beta                 99.058(1)
_cell_angle_gamma                92.240(1)
_cell_formula_units_Z            4
_cell_length_a                   12.909(1)
_cell_length_b                   23.904(1)
_cell_length_c                   26.912(1)
_cell_measurement_reflns_used    900
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     7889.3(8)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997) & COLLECT'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        'DENZO & COLLECT'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.0393
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            106400
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    0.199
_exptl_absorpt_correction_T_max  0.9804
_exptl_absorpt_correction_T_min  0.9428
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2948
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
 Two one and half ighly disordered C7H8 molecule were accounted for using the
 Platon SQUEEZE function.
;
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1789
_refine_ls_number_reflns         44974
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0629
_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^)+(0.0634P)^2^+7.7712P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1568
_refine_ls_wR_factor_ref         0.1701
_reflns_number_gt                34578
_reflns_number_total             44974
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300954a_si_002.cif
_cod_data_source_block           mf173
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P-1     '
_cod_original_formula_sum        'C81.50 H85 B3 Li4 O4 P6 Si'
_cod_database_code               4079844