Facile Transformations of a 1,3,5-Triphosphacyclohexadienyl Anion within the Coordination Sphere of Group 13 and 14 Elements: Synthesis of 1,3-Diphosphacyclopentadienyl Complexes and Phosphaorganometallic Cage Compounds
Brym, Markus; Francis, Matthew D.; Jin, Guoxia; Jones, Cameron; Mills, David P.; Stasch, Andreas; Organometallics 25 (2006) 4799–; doi:10.1021/om0605581

data_4074330
_publ_section_title
;
 Facile Transformations of a 1,3,5-Triphosphacyclohexadienyl Anion within
 the Coordination Sphere of Group 13 and 14 Elements:&#x00A0; Synthesis of
 1,3-Diphosphacyclopentadienyl Complexes and Phosphaorganometallic Cage
 Compounds
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              4799
_journal_paper_doi               10.1021/om0605581
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C47 H75 N3 P2 Sn'
_chemical_formula_weight         862.73
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 117.60(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.036(4)
_cell_length_b                   14.100(3)
_cell_length_c                   19.674(4)
_cell_measurement_temperature    150(2)
_cell_volume                     4680(2)
_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  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0477
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19460
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    0.648
_exptl_absorpt_correction_T_max  0.926
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.420
_refine_diff_density_min         -1.429
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         10167
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0539P)^2^+12.2044P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1283
_refine_ls_wR_factor_ref         0.1368
_reflns_number_gt                8235
_reflns_number_total             10167
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0605581si20060628_061253.cif
_cod_data_source_block           compound8
_cod_original_cell_volume        4679.9(16)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4074330