Synthesis and Structure of Solvent-Free Hexameric Magnesium Tri(tert-butyl)silylphosphandiide
Matthias Westerhausen; Mathias Krofta; Arno Pfitzner; Inorganic Chemistry 38 (1999) 598–599; doi:10.1021/ic9810485

data_4321778
_publ_contact_author
;
    Matthias Westerhausen
    Institut fuer Anorganische Chemie
    Ludwig-Maximilians-Universitaet
    Meiserstr. 1
    D-80333 Muenchen
    Germany
;
_publ_contact_author_email       maw@anorg.chemie.uni-muenchen.de
_publ_contact_author_fax         '+49 (89) 5902 578'
_publ_contact_author_phone       '+49 (89) 5902 638'
_publ_section_title
;
 Synthesis and Structure of Solvent-Free Hexameric Magnesium
 Tri(tert-butyl)silylphosphandiide
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              598
_journal_page_last               599
_journal_paper_doi               10.1021/ic9810485
_journal_volume                  38
_journal_year                    1999
_chemical_formula_analytical     MgPSi(t-Bu)3
_chemical_formula_sum            'C13 H28 Mg P Si'
_chemical_formula_weight         3212.69
_chemical_name_systematic
; 
 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
_cell_angle_alpha                90.00
_cell_angle_beta                 104.590(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   13.5940(10)
_cell_length_b                   23.177(2)
_cell_length_c                   16.3510(10)
_cell_measurement_temperature    173(2)
_cell_volume                     4985.6(7)
_computing_cell_refinement       SHELXL-93
_computing_data_collection       SHLELXL-93
_computing_data_reduction        SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       STOE-IPDS
_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  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            41481
_diffrn_reflns_theta_max         25.92
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    0.253
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.070
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             1764
_exptl_crystal_size_max          .3
_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .25
_refine_diff_density_max         1.225
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.062
_refine_ls_goodness_of_fit_obs   1.122
_refine_ls_hydrogen_treatment    'fixed on ideal positions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         9625
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_restrained_S_obs      1.122
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_obs          0.0756
_refine_ls_shift/esd_max         -0.114
_refine_ls_shift/esd_mean        0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1310P)^2^+8.2030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2263
_refine_ls_wR_factor_obs         0.2139
_reflns_number_observed          7755
_reflns_number_total             9625
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9810485.cif
_cod_data_source_block           IC9810485
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1310P)^2^+8.2030P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1310P)^2^+8.2030P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4985.6(6)
_cod_database_code               4321778