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_7114663
_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         'C36 H84 O2 P4 Si6'
_chemical_formula_sum            'C36 H84 O2 P4 Si6'
_chemical_formula_weight         841.45
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 101.199(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.6209(10)
_cell_length_b                   25.4353(12)
_cell_length_c                   14.4570(10)
_cell_measurement_reflns_used    6799
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.00
_cell_measurement_theta_min      1.60
_cell_volume                     4913.3(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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  0.1344
_diffrn_reflns_av_sigmaI/netI    0.1581
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            57887
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.328
_exptl_absorpt_correction_T_max  0.9842
_exptl_absorpt_correction_T_min  0.9000
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(a) W. R. Busing and H. A. Levy, Acta Crystallogr. 1957, 10, 180-182. 
(b) P. Coppens, L. Leiserowitz and D. Rabinovich, Acta Crystallogr. 1965, 18, 1035-1038. 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.172
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.604
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         10374
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.604
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0242P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0710
_reflns_number_gt                5488
_reflns_number_total             10374
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c4cc02489c2.cif
_cod_data_source_block           kr-17a
_cod_original_cell_volume        4913.3(5)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7114663