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_4079839
_publ_section_title
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 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
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_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         'C58 H64 B2 Li2 O2 P4 S2'
_chemical_formula_sum            'C58 H64 B2 Li2 O2 P4 S2'
_chemical_formula_weight         1016.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 105.124(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.498(1)
_cell_length_b                   16.165(1)
_cell_length_c                   15.384(1)
_cell_measurement_reflns_used    5396
_cell_measurement_temperature    396(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     2760.3(3)
_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      396(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17716
_diffrn_reflns_theta_full        30.02
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    0.253
_exptl_absorpt_correction_T_max  0.9751
_exptl_absorpt_correction_T_min  0.8839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.895
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     656
_refine_ls_number_reflns         13373
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.088
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0177P)^2^+2.6696P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1024
_reflns_number_gt                12712
_reflns_number_total             13373
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300954a_si_002.cif
_cod_data_source_block           hh831
_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 2.4.2 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      'P21     '
_cod_database_code               4079839