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_4323806
_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
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_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            'C48 H106 Ba2 O6 P4 Si8'
_chemical_formula_weight         1402.61
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 98.929(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.563(2)
_cell_length_b                   20.000(3)
_cell_length_c                   29.869(2)
_cell_measurement_temperature    193(2)
_cell_volume                     7413.9(17)
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0625
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            12184
_diffrn_reflns_theta_max         24.01
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    1.307
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_F_000             2904
_refine_diff_density_max         0.754
_refine_diff_density_min         -0.910
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.214
_refine_ls_goodness_of_fit_obs   1.286
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         11580
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.260
_refine_ls_restrained_S_obs      1.286
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_obs          0.0517
_refine_ls_shift/esd_max         2.151
_refine_ls_shift/esd_mean        0.053
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0548P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1334
_refine_ls_wR_factor_obs         0.1195
_reflns_number_observed          8431
_reflns_number_total             11597
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic950854y_3.cif
_cod_data_source_block           dimbap3b
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0548P)^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^)+(0.0548P)^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 
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_cod_database_code               4323806