Synthesis of Tris(1,2-dimethoxyethane-O,O')barium Bis(2,2,5,5-tetramethyl-2,5-disilaphospholanide) and the Monomer-Dimer Equilibrium in Toluene Solution
M. Westerhausen; M. Hartmann; W. Schwarz; Inorganic Chemistry 35 (1996) 2421–2426; doi:10.1021/ic950854y

data_4323804
_publ_section_title
;
 Synthesis of Tris(1,2-dimethoxyethane-O,O')barium
 Bis(2,2,5,5-tetramethyl-2,5-disilaphospholanide) and the Monomer-Dimer
 Equilibrium in Toluene Solution
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2421
_journal_page_last               2426
_journal_paper_doi               10.1021/ic950854y
_journal_volume                  35
_journal_year                    1996
_chemical_formula_sum            'C18 H48 P2 Si6'
_chemical_formula_weight         495.04
_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                72.45(1)
_cell_angle_beta                 78.13(1)
_cell_angle_gamma                70.83(1)
_cell_formula_units_Z            2
_cell_length_a                   9.433(2)
_cell_length_b                   12.783(3)
_cell_length_c                   14.135(3)
_cell_measurement_temperature    193(2)
_cell_volume                     1524.2(6)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(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  0.0993
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6972
_diffrn_reflns_theta_max         27.08
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    0.384
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_F_000             540
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.605
_refine_ls_goodness_of_fit_obs   1.670
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         6548
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.791
_refine_ls_restrained_S_obs      1.670
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_obs          0.0495
_refine_ls_shift/esd_max         -0.048
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0622P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1553
_refine_ls_wR_factor_obs         0.1474
_reflns_number_observed          5510
_reflns_number_total             6568
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic950854y_1.cif
_cod_data_source_block           phosphane2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0622P)^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^)+(0.0622P)^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        1520.8(6)
_cod_database_code               4323804