1,3-Bis(trimethylsilyl)-2-phenyl-1-aza-3-phosphapropenide Anions as Bidentate Ligands for the Alkaline Earth Metals Magnesium, Calcium, Strontium, and Barium
Matthias Westerhausen; Matthias H. Digeser; Wolfgang Schwarz; Inorganic Chemistry 36 (1997) 521–527; doi:10.1021/ic960887t

data_4323314
_publ_section_title
;
 1,3-Bis(trimethylsilyl)-2-phenyl-1-aza-3-phosphapropenide Anions as
 Bidentate Ligands for the Alkaline Earth Metals Magnesium, Calcium,
 Strontium, and Barium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              521
_journal_page_last               527
_journal_paper_doi               10.1021/ic960887t
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C38 H70 Ba N2 O3 P2 Si4'
_chemical_formula_weight         914.60
_chemical_name_systematic
;
 Tris(tetrahydrofuran)barium =
bis[1,3-bis(trimethylsilyl)-2-phenyl-1-aza-3-phosphapropenide]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                76.46(2)
_cell_angle_beta                 76.45(2)
_cell_angle_gamma                89.31(2)
_cell_formula_units_Z            4
_cell_length_a                   12.452(4)
_cell_length_b                   19.071(4)
_cell_length_c                   22.123(7)
_cell_measurement_temperature    293(2)
_cell_volume                     4960(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0164
_diffrn_reflns_av_sigmaI/netI    0.0564
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15580
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.994
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_F_000             1912
_refine_diff_density_max         1.467
_refine_diff_density_min         -1.448
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.298
_refine_ls_goodness_of_fit_obs   1.401
_refine_ls_matrix_type           full
_refine_ls_number_parameters     952
_refine_ls_number_reflns         14723
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.341
_refine_ls_restrained_S_obs      1.412
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_obs          0.0590
_refine_ls_shift/esd_max         1.136
_refine_ls_shift/esd_mean        0.052
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0596P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1489
_refine_ls_wR_factor_obs         0.1309
_reflns_number_observed          11109
_reflns_number_total             15558
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960887t_4.cif
_cod_data_source_block           bancp;Compound4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0596P)^2^+0.0000P] 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^)+(0.0596P)^2^+0.0000P] 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        4960.3(25)
_cod_database_code               4323314