Barium tetraalkylaluminate complexes supported by the super-bulky hydrotris(pyrazolyl)borate ligand
Shi, Xianghui; Liu, Zhizhou; Cheng, Jianhua; Dalton Transactions  (2019) –; doi:10.1039/C9DT04182F

data_7702928
_publ_section_title
;
 Barium tetraalkylaluminate complexes supported by the super-bulky
 hydrotris(pyrazolyl)borate ligand
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT04182F
_journal_year                    2019
_chemical_formula_moiety         'C56  H90  B1  N6  Al1  Ba1'
_chemical_formula_sum            'C56 H90 Al B Ba N6'
_chemical_formula_weight         1022.46
_chemical_name_common            '[(TpAd,iPr)Ba(AlEt4)]'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   iterative
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-09-30 deposited with the CCDC.	2019-11-21 downloaded from the CCDC.
;
_cell_angle_alpha                80.1520(10)
_cell_angle_beta                 80.8310(10)
_cell_angle_gamma                75.5280(10)
_cell_formula_units_Z            2
_cell_length_a                   11.6917(6)
_cell_length_b                   13.0673(6)
_cell_length_c                   19.1695(9)
_cell_measurement_reflns_used    9708
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.14
_cell_volume                     2773.0(2)
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis,2007)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0166
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14145
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.625
_exptl_absorpt_coefficient_mu    0.772
_exptl_absorpt_correction_T_max  0.870
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'Sheldrick, G. M. SADABS, Version 2.10; Bruker AXS, Inc.: Madison, WI 2003.'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1084
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Hexane'
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.841
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         9497
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+2.2118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0821
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8766
_reflns_number_total             9497
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04182f2.cif
_cod_data_source_block           G081
_cod_database_code               7702928
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.830
_shelx_estimated_absorpt_t_max   0.874
_shelx_res_checksum              77338