Monomeric and Dimeric Tetrahydrofuran Complexes of Barium Bis[bis(dimethyl-tert-butylsilyl)arsanide]
Matthias Westerhausen; Matthias H. Digeser; Jörg Knizek; Wolfgang Schwarz; Inorganic Chemistry 37 (1998) 619–623; doi:10.1021/ic9710770

data_4322657
_publ_section_title
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 Monomeric and Dimeric Tetrahydrofuran Complexes of Barium
 Bis[bis(dimethyl-tert-butylsilyl)arsanide]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              619
_journal_page_last               623
_journal_paper_doi               10.1021/ic9710770
_journal_volume                  37
_journal_year                    1998
_chemical_formula_moiety         {(thf)Ba[As(SiMe2t-Bu)2]2}2
_chemical_formula_sum            'C65 H145 As4 Ba2 O2 Si8'
_chemical_formula_weight         1757.89
_chemical_melting_point          362(3)
_chemical_name_systematic
; 
 Dimeric (Tetrahydrofuran)barium bis[bis(dimethyl-tert.-butylsilyl)arsanide] 
;
_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                 93.58
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.77910(10)
_cell_length_b                   11.65530(10)
_cell_length_c                   26.11670(10)
_cell_measurement_temperature    293(2)
_cell_volume                     9350.81(9)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measurement_device       P4
_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  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            53360
_diffrn_reflns_theta_max         29.61
_diffrn_reflns_theta_min         0.66
_exptl_absorpt_coefficient_mu    2.377
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             3628
_exptl_crystal_size_max          .2
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .2
_refine_diff_density_max         2.339
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.184
_refine_ls_goodness_of_fit_obs   1.224
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     728
_refine_ls_number_reflns         18676
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.277
_refine_ls_restrained_S_obs      1.224
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_obs          0.0587
_refine_ls_shift/esd_max         -2.522
_refine_ls_shift/esd_mean        0.053
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0329P)^2^+51.1470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1488
_refine_ls_wR_factor_obs         0.1295
_reflns_number_observed          15971
_reflns_number_total             19305
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9710770_2.cif
_cod_data_source_block           dimeric_barium_bisarsanide
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0329P)^2^+51.1470P] 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^)+(0.0329P)^2^+51.1470P] 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        9350.76(9)
_cod_database_code               4322657