Specific insertion reactions of a germylene, stannylene and plumbylene into the unique P‒P bond of the hexaphospha-pentaprismane cage, P6C4tBu4: Crystal and molecular structures of P6C4tBu4ER2 (E = Ge, Sn, R = N(SiMe3)2; E = Pb, R = (C6H3(NMe2)2 -2,6)
Al-Ktaifani, Mahmoud M.; Hitchcock, Peter B.; Lappert, Michael F.; Nixon, John F.; Uiterweerd, Philip; Dalton Transactions  (2008) 2825–2831; doi:10.1039/b800458g

data_7003835
_publ_section_title
;
 Specific insertion reactions of a germylene, stannylene and plumbylene
 into the unique P--P bond of the hexaphospha-pentaprismane cage,
 P6C4tBu4: Crystal and molecular structures of P6C4tBu4ER2 (E = Ge, Sn,
 R = N(SiMe3)2; E = Pb, R = (C6H3(NMe2)2 -2,6)
;
_journal_issue                   21
_journal_name_full               'Dalton Transactions'
_journal_page_first              2825
_journal_page_last               2831
_journal_paper_doi               10.1039/b800458g
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C40 H66 N4 P6 Pb1'
_chemical_formula_structural     'C40 H66 N4 P6 PB'
_chemical_formula_sum            'C40 H66 N4 P6 Pb'
_chemical_formula_weight         995.98
_chemical_name_common            '[Pb{P6(CtBu)4}{C6H3(NMe2)2}2]'
_chemical_name_systematic
;
?
;
_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_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1
_audit_creation_date             2001-03-05T10:44:55-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 112.074(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2177(3)
_cell_length_b                   33.3392(11)
_cell_length_c                   13.1175(4)
_cell_measurement_reflns_used    33423
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     4546.2(2)
_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    'SHELXS-97 (Sheldri8ck, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_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  0.0697
_diffrn_reflns_av_unetI/netI     0.0844
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23962
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         3.82
_exptl_absorpt_coefficient_mu    3.954
_exptl_absorpt_correction_T_max  0.558
_exptl_absorpt_correction_T_min  0.455
_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    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.344
_refine_diff_density_min         -1.844
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         10524
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.075
_refine_ls_R_factor_gt           0.0461
_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^)+(0.0419P)^2^+0.6017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.093
_refine_ls_wR_factor_ref         0.1034
_reflns_number_gt                7750
_reflns_number_total             10524
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b800458g.txt
_cod_data_source_block           mar401
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7003835