Tetraphenoxoborate complexes of barium: crystal structures of the metalloborates [Ba(thf )4{B(OPh)4}2] and [Ba(dme)2{B(OPh)4}2] †
Errington, R. John; Tombul, Mustafa; Walker, Gary L. P.; Clegg, William; Heath, Sarah L.; Horsburgh, Lynne; Journal of the Chemical Society, Dalton Transactions  (1999) 3533–; doi:10.1039/a906089h

data_7027728
_publ_section_title
;
 Tetraphenoxoborate complexes of barium: crystal structures of the
 metalloborates [Ba(thf&#x200A;)4{B(OPh)4}2] and
 [Ba(dme)2{B(OPh)4}2]&#x200A;&#x2020;
;
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3533
_journal_paper_doi               10.1039/a906089h
_journal_year                    1999
_chemical_formula_sum            'C72 H88 B2 Ba O14'
_chemical_formula_weight         1336.38
_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                104.461(2)
_cell_angle_beta                 104.083(2)
_cell_angle_gamma                93.135(2)
_cell_formula_units_Z            1
_cell_length_a                   11.0751(9)
_cell_length_b                   11.7693(10)
_cell_length_c                   13.5004(11)
_cell_measurement_reflns_used    10079
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.41
_cell_measurement_theta_min      2.07
_cell_volume                     1640.2(2)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measurement_device       'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0227
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10382
_diffrn_reflns_theta_max         28.42
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    0.671
_exptl_absorpt_correction_T_max  0.5979
_exptl_absorpt_correction_T_min  0.4948
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       Block
_exptl_crystal_F_000             698
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.0032(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.076
_refine_ls_goodness_of_fit_obs   1.076
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         7185
_refine_ls_number_restraints     308
_refine_ls_restrained_S_all      1.108
_refine_ls_restrained_S_obs      1.108
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_obs          0.0289
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+1.1879P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0785
_refine_ls_wR_factor_obs         0.0783
_reflns_number_observed          7163
_reflns_number_total             7185
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            906089hsup1.cif
_cod_data_source_block           rje99
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+1.1879P] 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^)+(0.0436P)^2^+1.1879P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7027728