Stepwise synthesis of a stable diphosphasilirane and its unexpected dimerization
Kirsten Reuter; Carsten von Hanisch; Chem.Commun. 50 (2014) 7709–; doi:10.1039/C4CC02489C

data_7114661
_publ_section_title
;
 Stepwise synthesis of a stable diphosphasilirane and its unexpected
 dimerization
;
_journal_name_full               Chem.Commun.
_journal_page_first              7709
_journal_paper_doi               10.1039/C4CC02489C
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C26 H62 O5 P2 Si3 Sr'
_chemical_formula_sum            'C26 H62 O5 P2 Si3 Sr'
_chemical_formula_weight         688.59
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.051(3)
_cell_length_b                   16.095(3)
_cell_length_c                   33.152(7)
_cell_measurement_reflns_used    3007
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.50
_cell_measurement_theta_min      1.23
_cell_volume                     7497(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  IPDS
_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  0.1286
_diffrn_reflns_av_sigmaI/netI    0.0940
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            47121
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    1.649
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.792
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         4900
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.792
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0705
_refine_ls_wR_factor_ref         0.0763
_reflns_number_gt                3007
_reflns_number_total             4900
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc02489c2.cif
_cod_data_source_block           h:\carsten\todo\kirsten\kr24a\pbca
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7114661