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_4317298
_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 H24 B Na O5'
_chemical_formula_sum            'C10 H24 B Na O5'
_chemical_formula_weight         258.09
_chemical_name_systematic
;
1,4,7,10,13-Pentaoxacyclopentadecanesodium tetrahydroborate 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     'using coords of known structure'
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7751(17)
_cell_length_b                   11.519(2)
_cell_length_c                   16.058(4)
_cell_measurement_reflns_used    4620
_cell_measurement_temperature    100(2)
_cell_volume                     1438.2(5)
_computing_cell_refinement
;
'Gutmann, M. J., Wilson, C. C. (2001). SXD-2001. ISIS, Rutherford Appleton
Laboratories, Oxfordshire, England.
;
_computing_data_collection
;
'Gutmann, M. J., Wilson, C. C. (2001). SXD-2001. ISIS, Rutherford Appleton
Laboratories, Oxfordshire, England.
;
_computing_data_reduction
;
'Gutmann, M. J., Wilson, C. C. (2001). SXD-2001. ISIS, Rutherford Appleton
Laboratories, Oxfordshire, England.
;
_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
;
Spek, A.L. (2003). J. Appl. Cryst. 36, 7-13.
;
_computing_structure_refinement
;
Sheldrick, G. M. (1997). SHELXL-97. University of Go\"ttingen, Germany.
;
_computing_structure_solution    'using coords of known structure'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.100
_diffrn_measured_fraction_theta_max 0.101
_diffrn_measurement_device_type  'SXD at ISIS neutron source'
_diffrn_measurement_method       'time-of-flight Laue diffraction'
_diffrn_radiation_monochromator  none
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         'ISIS spallation neutron source'
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     0.35-10.0
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0663
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            6329
_diffrn_reflns_reduction_process
;
The variable wavelength nature of the data collection
procedure means that sensible values of
_diffrn_reflns_theta_min & _diffrn_reflns_theta_max
cannot be given instead the following limits are given
_diffrn_reflns_sin(theta)/lambda_min      0.05
_diffrn_reflns_sin(theta)/lambda_max      2.05
;
_diffrn_reflns_theta_full        84.71
_diffrn_reflns_theta_max         84.71
_diffrn_reflns_theta_min         8.14
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    '0.57102 + 0.1198 * lambda'
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SXD-2001 (Gutmann, Wilson, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             560
_exptl_crystal_size_max          5.00
_exptl_crystal_size_mid          1.00
_exptl_crystal_size_min          1.00
_refine_diff_density_max         1.232
_refine_diff_density_min         -1.137
_refine_diff_density_rms         0.259
_refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(14)
_refine_ls_extinction_coef       0.00081(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_ref   1.039
_refine_ls_hydrogen_treatment    anisotropic
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         6329
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0758
_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^)+(0.1337P)^2^+20.5817P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1895
_refine_ls_wR_factor_ref         0.1895
_reflns_number_gt                1787
_reflns_number_total             1787
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic1014187_si_002_2.cif
_cod_data_source_block           na_15c5_bh4_Compound1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 
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_cod_database_code               4317298