Insights into Metal Borohydride and Aluminohydride Bonding: X-Ray and Neutron Diffraction Structures and a DFT and Charge Density Study of [Na(15-crown-5)][EH4] (E = B, Al)
Peter Sirsch; Natascha L. N. Clark; Lenuţa Onuţ; Richard P. L. Burchell; Andreas Decken; G. Sean McGrady; Aziz Daoud-Aladine; Matthias J. Gutmann; Inorganic Chemistry 49 (2010) 11395–11402; doi:10.1021/ic1014187

data_4317297
_publ_contact_author_address
;
Department of Chemistry
University of New Brunswick
Fredericton, NB
E3B 5A3 (Canada)
;
_publ_contact_author_email       psirsch@unb.ca
_publ_contact_author_fax         1(506)4534981
_publ_contact_author_name
;
 P. Sirsch
;
_publ_contact_author_phone       1(506)4558929
_publ_section_title
;
 Insights into Metal Borohydride and Aluminohydride Bonding: X-Ray and
 Neutron Diffraction Structures and a DFT and Charge Density Study of
 [Na(15-crown-5)][EH4] (E = B, Al)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11395
_journal_page_last               11402
_journal_paper_doi               10.1021/ic1014187
_journal_volume                  49
_journal_year                    2010
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C10 H20 Na O5, Al H4'
_chemical_formula_sum            'C10 H24 Al Na O5'
_chemical_formula_weight         274.26
_chemical_name_systematic
;
1,4,7,10,13-Pentaoxacyclopentadecanesodium tetrahydroaluminate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 97.395(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7904(18)
_cell_length_b                   10.2580(18)
_cell_length_c                   15.926(3)
_cell_measurement_reflns_used    4690
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.18
_cell_measurement_theta_min      2.37
_cell_volume                     1586.1(5)
_computing_cell_refinement
;
Bruker (1999). SMART, version 5.054, Bruker AXS Inc., Madison,
Wisconsin, USA.
;
_computing_data_collection
;
Bruker (1999). SMART, version 5.054, Bruker AXS Inc., Madison,
Wisconsin, USA.
;
_computing_data_reduction
;
Bruker (2001). SAINT, version 7.23a, Bruker AXS Inc., Madison,
Wisconsin, USA.
;
_computing_molecular_graphics
;
Farrugia, L. J. (1997) ORTEP-3. J Appl. Crystallogr. 30, 565.
Spek, A.L. (2003). J. Appl. Cryst. 36, 7-13.
;
_computing_publication_material
;
Bruker AXS (2003). SHELXTL. Version 6.14. Bruker AXS Inc., Madison,
Wisconsin, USA.
Spek, A.L. (2003). J. Appl. Cryst. 36, 7-13.
;
_computing_structure_refinement
;
Sheldrick, G. M. (1997). SHELXL97. University of
Gottingen, Germany.
;
_computing_structure_solution
;
Sheldrick, G. M. (1997). SHELXS97. University of
Gottingen, Germany.
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker AXS SMART1000/P4'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10418
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.10
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              K760
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.161
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.953
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         3527
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0615
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0679P)^2^+2.8867P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1825
_refine_ls_wR_factor_ref         0.1876
_reflns_number_gt                2791
_reflns_number_total             3527
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic1014187_si_002_1.cif
_cod_data_source_block           sg050259_Compound2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4317297