Unusual Reactivity of Methylphosphaalkyne (P\τbCMe) toward Digermenes and Distannenes: Stepwise Formations of Bridged 2,3,5,6-Tetraphospha-1,4-dimethylidenecyclohexanes
Cameron Jones; Christian Schulten; Andreas Stasch; Inorganic Chemistry 47 (2008) 1273–1278; doi:10.1021/ic700926u

data_4303992
_publ_section_title
;
Unusual Reactivity of Methylphosphaalkyne (P\\tbCMe) toward Digermenes and
Distannenes: Stepwise Formations of Bridged
2,3,5,6-Tetraphospha-1,4-dimethylidenecyclohexanes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1273
_journal_page_last               1278
_journal_paper_doi               10.1021/ic700926u
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C28 H44 Ge O10 P2 Si4 W2'
_chemical_formula_weight         1155.22
_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                   11.323(2)
_cell_length_b                   18.487(4)
_cell_length_c                   20.297(4)
_cell_measurement_temperature    150(2)
_cell_volume                     4248.7(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_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  0.0794
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            34743
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    6.337
_exptl_absorpt_correction_T_max  0.469
_exptl_absorpt_correction_T_min  0.391
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_density_meas      red
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.784
_refine_diff_density_min         -1.406
_refine_diff_density_rms         0.129
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.004(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         9211
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0246
_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^+4.9178P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0533
_refine_ls_wR_factor_ref         0.0538
_reflns_number_gt                8997
_reflns_number_total             9211
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700926u-file001_5.cif
_cod_data_source_block           compound15
_cod_database_code               4303992