Vicinal diphosphoniums: electrostatic repulsion under covalent constraint
Abdalilah, Mohammed; Zurawinski, Remigiuz; Canac, Yves; Laleu, Benoît; Lacour, Jérôme; Lepetit, Christine; Magro, Germinal; Bernardinelli, Gérald; Donnadieu, Bruno; Duhayon, Carine; Mikolajczyk, Marian; Chauvin, Remi; Dalton Transactions  (2009) 8493–8508; doi:10.1039/b903933c

data_7002424
_publ_section_title
;
 Vicinal diphosphoniums: electrostatic repulsion under covalent
 constraint
;
_journal_issue                   40
_journal_name_full               'Dalton Transactions'
_journal_page_first              8493
_journal_page_last               8508
_journal_paper_doi               10.1039/b903933c
_journal_year                    2009
_chemical_formula_moiety
'C32 H30 P2, 2(C F3 O3 S), 2(C0.80 H1.20 O0.40), H2 O'
_chemical_formula_sum            'C35.6 H34.4 F6 O7.8 P2 S2'
_chemical_formula_weight         827.12
_chemical_name_systematic
;
?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 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                 97.25(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.799(2)
_cell_length_b                   12.013(2)
_cell_length_c                   15.743(3)
_cell_measurement_reflns_used    7904
_cell_measurement_temperature    295
_cell_measurement_theta_max      25.95
_cell_measurement_theta_min      2.1
_cell_volume                     2026.0(6)
_computing_cell_refinement       'STOE,s Area Detector Software Version 2003 '
_computing_data_collection       'STOE,s Area Detector Software Version 2003 '
_computing_data_reduction        'STOE,s Area Detector Software Version 2003 '
_computing_molecular_graphics    'Ortep3 for Windows'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'IPDS STOE'
_diffrn_measurement_method       'phi scan'
_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  0.0789
_diffrn_reflns_av_sigmaI/netI    0.0627
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11409
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    0.284
_exptl_absorpt_correction_T_max  0.9722
_exptl_absorpt_correction_T_min  0.8998
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   Difabs
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'prism frag'
_exptl_crystal_F_000             849
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         2869
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      0.925
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0561
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1073P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1394
_refine_ls_wR_factor_ref         0.1652
_reflns_number_gt                1764
_reflns_number_total             2869
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b903933c.txt
_cod_data_source_block           2[OTf]~2~
_cod_original_sg_symbol_Hall     '-P 2yc '
_cod_original_sg_symbol_H-M      P2/c
_cod_database_code               7002424