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_7027729
_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            'C58 H65 B2 Ba O13'
_chemical_formula_weight         1129.06
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.881(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2348(6)
_cell_length_b                   20.0431(11)
_cell_length_c                   25.0246(13)
_cell_measurement_reflns_used    15851
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.68
_cell_measurement_theta_min      2.08
_cell_volume                     5634.4(5)
_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_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  '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  0.0539
_diffrn_reflns_av_sigmaI/netI    0.0827
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            35072
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.88
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.77
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.602
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2332
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.618
_refine_diff_density_min         -1.175
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       0.00019(6)
_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_ref   0.977
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         13367
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0416P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0985
_reflns_number_gt                8751
_reflns_number_total             13367
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            906089hsup1.cif
_cod_data_source_block           rje215
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7027729