Synthesis and Rearrangement of Diphosphorus Analogues of Amidinium Salts
Tsuyoshi Kato; Heinz Gornitzka; Antoine Baceiredo; Wolfgang W. Schoeller; Guy Bertrand; Journal of the American Chemical Society 124 (2002) 2506–2512; doi:10.1021/ja010347h

data_4114668
_publ_section_title
;
 Synthesis and Rearrangement of Diphosphorus Analogues of Amidinium Salts
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2506
_journal_page_last               2512
_journal_paper_doi               10.1021/ja010347h
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C26 H61 Cl4 Ga N4 P2 Si2'
_chemical_formula_weight         759.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 90.2780(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9435(4)
_cell_length_b                   21.9177(8)
_cell_length_c                   18.3228(7)
_cell_measurement_reflns_used    6974
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      33.307
_cell_measurement_theta_min      2.513
_cell_volume                     3993.2(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5716
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    1.119
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorles
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       block
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.8
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         5716
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0672P)^2^+3.4240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1103
_refine_ls_wR_factor_ref         0.1192
_reflns_number_gt                4692
_reflns_number_total             5716
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja010347h_2.cif
_cod_data_source_block           IIIP3
_cod_database_code               4114668