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_4321426
_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         '[(THF)MgPSiBu3]4'
_chemical_formula_sum            'C68 H148 Mg4 O5 P4 Si4'
_chemical_formula_weight         1379.34
_chemical_name_systematic
; 
 tetrakis[(THF)magnesium tri(tert-butyl)silylphosphandiide] 
;
_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                 96.528(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4542(14)
_cell_length_b                   26.1232(14)
_cell_length_c                   24.5392(15)
_cell_measurement_temperature    200(2)
_cell_volume                     8568.8(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean area-detector
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  STOE-IPDS
_diffrn_measurement_method       IPDS
_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  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            45003
_diffrn_reflns_theta_full        22.35
_diffrn_reflns_theta_max         22.35
_diffrn_reflns_theta_min         1.52
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.214
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.069
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          .30
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .25
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     766
_refine_ls_number_reflns         10756
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0542
_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^)+(0.0910P)^2^+4.1155P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1516
_reflns_number_gt                8132
_reflns_number_total             10756
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000038c_1.cif
_cod_data_source_block           mg4p4
_cod_database_code               4321426