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_7110910
_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_compound_source        'synthesis as described'
_chemical_formula_moiety         'C20 H36 Ge1 I2 P6'
_chemical_formula_structural     'C20 H36 P6 GE I2'
_chemical_formula_sum            'C20 H36 Ge I2 P6'
_chemical_formula_weight         788.7
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_conform_dict_location     ftp://ftp.iucr.org/cifdics/cif_core2.1beta.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta3
_audit_creation_date             1999-08-16T14:46:56-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.000(14)
_cell_angle_beta                 95.009(14)
_cell_angle_gamma                90.000(11)
_cell_formula_units_Z            4
_cell_length_a                   11.8196(12)
_cell_length_b                   17.491(3)
_cell_length_c                   13.850(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      9.34
_cell_measurement_theta_min      7.3
_cell_measurement_wavelength     0.71073
_cell_volume                     2852.4(8)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      0.9725E-2
_diffrn_orient_matrix_UB_12      0.56522E-1
_diffrn_orient_matrix_UB_13      -0.6296E-2
_diffrn_orient_matrix_UB_21      -0.76357E-1
_diffrn_orient_matrix_UB_22      0.3505E-2
_diffrn_orient_matrix_UB_23      -0.36989E-1
_diffrn_orient_matrix_UB_31      -0.03589
_diffrn_orient_matrix_UB_32      0.00784
_diffrn_orient_matrix_UB_33      0.62013E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_sigmaI/netI    0.085
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5261
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.08
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.583
_exptl_absorpt_correction_T_max  0.702
_exptl_absorpt_correction_T_min  0.5925
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
        Number of psi-scan sets used was   1
        Theta correction was applied.
        Averaged transmission function was used.
        No Fourier smoothing was applied.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.837
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.888
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         5012
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.888
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.1076
_reflns_number_gt                3416
_reflns_number_total             5012
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b001632msup1.cif
_cod_data_source_block           aug1299
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7110910
_exptl_absorpt_factor_mur        0.348
_exptl_absorpt_correction_t_ave  0.6499
_diffrn_standards_decay_corr_max 1.025
_diffrn_standards_decay_corr_min 0.97