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_7114662
_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         'C34 H82 Ba O9 P2 Si3'
_chemical_formula_sum            'C34 H82 Ba O9 P2 Si3'
_chemical_formula_weight         918.55
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   12.266(3)
_cell_length_b                   16.570(3)
_cell_length_c                   23.821(5)
_cell_measurement_reflns_used    17755
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.18
_cell_measurement_theta_min      1.87
_cell_volume                     4841.6(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0652
_diffrn_reflns_av_sigmaI/netI    0.0844
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            24870
_diffrn_reflns_theta_full        26.72
_diffrn_reflns_theta_max         26.72
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    1.003
_exptl_absorpt_correction_T_max  0.9029
_exptl_absorpt_correction_T_min  0.8216
_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    1.260
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.905
_refine_diff_density_min         -1.648
_refine_diff_density_rms         0.330
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.026(16)
_refine_ls_extinction_coef       0.0058(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         10184
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0621P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.1143
_reflns_number_gt                8337
_reflns_number_total             10184
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc02489c2.cif
_cod_data_source_block           c:\xray\kr-ba\p2si3oba
_cod_original_cell_volume        4841.6(17)
_cod_database_code               7114662
_exptl_special_detail
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