Remarkable organophosphorus cage compounds from the reaction of cobaltocene and the triphosphole P3C2But2CH(SiMe3) 2: crystal and molecular structures of [Co(η5-C5H5)(η4-C 4H4CHCHP6C4But 4)] and P6C4But4CH(SiMe3)
Hitchcock, Peter B.; Nixon, John F.; Büyükkidan, Nurgün Sakarya; Chemical Communications  (2001) 2720–; doi:10.1039/b108125j

data_7125524
_publ_section_title
;
 Remarkable organophosphorus cage compounds from the reaction of
 cobaltocene and the triphosphole P3C2But2CH(SiMe3) 2: crystal and
 molecular structures of [Co(\h5-C5H5)(\h4-C 4H4CHCHP6C4But 4)] and
 P6C4But4CH(SiMe3)
;
_journal_issue                   24
_journal_name_full               'Chemical Communications'
_journal_page_first              2720
_journal_paper_doi               10.1039/b108125j
_journal_year                    2001
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C24 H46 P6 Si'
_chemical_formula_structural     'C24 H46 P6 Si'
_chemical_formula_sum            'C24 H46 P6 Si'
_chemical_formula_weight         548.52
_chemical_name_common            '[(CtBu)4P6CHSiMe3]'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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_core_2.1beta5.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta5
_audit_creation_date             1999-09-03T11:46:36-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                100.210(2)
_cell_angle_beta                 97.134(2)
_cell_angle_gamma                102.000(2)
_cell_formula_units_Z            2
_cell_length_a                   10.2274(2)
_cell_length_b                   12.3429(4)
_cell_length_c                   12.7112(4)
_cell_measurement_reflns_used    11528
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      4.076
_cell_measurement_wavelength     0.71073
_cell_volume                     1522.92(8)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXLS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18033
_diffrn_reflns_theta_full        27.89
_diffrn_reflns_theta_max         27.89
_diffrn_reflns_theta_min         4.96
_exptl_absorpt_coefficient_mu    0.404
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         7193
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+0.3963P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0985
_reflns_number_gt                5978
_reflns_number_total             7193
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b108125j.txt
_cod_data_source_block           sep499
_cod_original_cell_volume        1522.92(7)
_cod_original_sg_symbol_Hall     'P -1'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7125524