Polyhedral Members of the Mg2nP2m Family Derived from Dimeric Magnesium Trialkylsilylphosphandiide
Matthias Westerhausen; Mathias Krofta; Peter Mayer; Marcus Warchhold; Heinrich Nöth; Inorganic Chemistry 39 (2000) 4721–4724; doi:10.1021/ic000038c

data_4321427
_publ_contact_author
;
    Matthias Westerhausen
    Department Chemie
    Ludwig-Maximilians-Universitaet Muenchen
    Butenandtstr. 9 (Haus D)
    D-81377 Muenchen
    Germany
;
_publ_contact_author_email       maw@cup.uni-muenchen.de
_publ_contact_author_fax         '+49 (89) 2180 7867'
_publ_contact_author_phone       '+49 (89) 2180 7481'
_publ_section_title
;
 Polyhedral Members of the Mg2nP2m Family Derived from Dimeric Magnesium
 Trialkylsilylphosphandiide
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4721
_journal_page_last               4724
_journal_paper_doi               10.1021/ic000038c
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety         Mg2[PHSiBu3][PSiBu3]
_chemical_formula_sum            'C36 H83 Mg2 P3 Si3'
_chemical_formula_weight         741.82
_chemical_name_systematic
; 
 tetramagnesium bis[tri(tert-butylsilyl)phosphanide] 
bis[tri(tert-butyl)silylphosphandiide] 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.4150(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9513(10)
_cell_length_b                   14.2692(10)
_cell_length_c                   24.2088(17)
_cell_measurement_temperature    183(2)
_cell_volume                     4706.6(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.718
_diffrn_measured_fraction_theta_max 0.718
_diffrn_measurement_device_type  Siemens-P4/SMART-CCD
_diffrn_measurement_method       area-detector
_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  0.0808
_diffrn_reflns_av_sigmaI/netI    0.0533
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            26700
_diffrn_reflns_theta_full        29.04
_diffrn_reflns_theta_max         29.04
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.251
_exptl_absorpt_correction_T_max  0.9284
_exptl_absorpt_correction_T_min  0.9062
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.047
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         9013
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1065P)^2^+3.4329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1569
_refine_ls_wR_factor_ref         0.1750
_reflns_number_gt                7189
_reflns_number_total             9013
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000038c_2.cif
_cod_data_source_block           Mg4P6
_cod_database_code               4321427