Synthesis, crystal and molecular structures of the novel, structurally different, cage compounds P6C4But4SiI2 and P6C4But4GeI2, resulting from intra-molecular coupling of two 1,2,4-triphospholyl rings
Avent, Anthony G.; Cloke, F. Geoffrey N.; Francis, Matthew D.; Hitchcock, Peter B.; Nixon, John F.; Chemical Communications  (2000) 879–; doi:10.1039/b001632m

data_7110909
_publ_section_title
;
 Synthesis, crystal and molecular structures of the novel, structurally
 different, cage compounds P6C4But4SiI2 and P6C4But4GeI2, resulting from
 intra-molecular coupling of two 1,2,4-triphospholyl rings
;
_journal_issue                   10
_journal_name_full               'Chemical Communications'
_journal_page_first              879
_journal_paper_doi               10.1039/b001632m
_journal_year                    2000
_chemical_formula_sum            'C20 H36 I2 P6 Si'
_chemical_formula_weight         744.20
_chemical_name_common            '[P6(CtBu)4SiI2]'
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 94.87(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.827(4)
_cell_length_b                   15.837(9)
_cell_length_c                   15.626(5)
_cell_measurement_temperature    173(2)
_cell_volume                     2916(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0518
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9137
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    2.535
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.174
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.008(13)
_refine_ls_extinction_coef       0.00056(9)
_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   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         8776
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+2.3509P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0696
_reflns_number_gt                7863
_reflns_number_total             8776
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b001632msup1.cif
_cod_data_source_block           apr299
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7110909