Synthesis and crystal structure of [IBa(OBut)4{Li(thf)}4(OH)]: a mixed ligand heterometallic cluster with an unusual low coordination number for barium
Fromm, Katharina M.; Gueneau, Estelle D.; Goesmann, H.; Chemical Communications  (2000) 2187–; doi:10.1039/b005638n

data_7115131
_publ_section_title
;
 Synthesis and crystal structure of [IBa(OBut)4{Li(thf)}4(OH)]: a mixed
 ligand heterometallic cluster with an unusual low coordination number for
 barium
;
_journal_issue                   22
_journal_name_full               'Chemical Communications'
_journal_page_first              2187
_journal_paper_doi               10.1039/b005638n
_journal_year                    2000
_chemical_formula_moiety         '[IBa(OtBu)4{Li(thf)}4(OH)]'
_chemical_formula_sum            'C32 H69 Ba I Li4 O9'
_chemical_formula_weight         889.87
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           129
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2a'
_symmetry_space_group_name_H-M   'P 4/n m m :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.574(2)
_cell_length_b                   15.574(2)
_cell_length_c                   10.395(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     2521.3(7)
_computing_cell_refinement       STOE
_computing_data_collection       STOE
_computing_data_reduction        STOE
_computing_molecular_graphics    SCHAKAL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.841
_diffrn_measured_fraction_theta_max 0.841
_diffrn_measurement_device_type  'STOE STADI-4'
_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  0.1139
_diffrn_reflns_av_sigmaI/netI    0.0811
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4721
_diffrn_reflns_theta_full        27.01
_diffrn_reflns_theta_max         27.01
_diffrn_reflns_theta_min         13.71
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.435
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             908
_exptl_crystal_size_max          .65
_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .3
_refine_diff_density_max         1.003
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         1313
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1138
_refine_ls_R_factor_gt           0.0807
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1295P)^2^+1.0636P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2014
_refine_ls_wR_factor_ref         0.2343
_reflns_number_gt                932
_reflns_number_total             1313
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b005638n.txt
_cod_data_source_block           BaLi4-Cluster
_cod_original_cell_volume        2521.5(7)
_cod_original_sg_symbol_H-M      P4/nmm
_cod_original_formula_sum        'C32 H69 Ba1 I1 Li4 O9'
_cod_database_code               7115131