Mild Dehydrogenation of Ammonia Borane Complexed with Aluminum Borohydride
Dovgaliuk, Iurii; Le Duff, Cécile S.; Robeyns, Koen; Devillers, Michel; Filinchuk, Yaroslav; Chemistry of Materials 27 (2015) 768–; doi:10.1021/cm503601h

data_4002168
_publ_section_title
;
 Mild Dehydrogenation of Ammonia Borane Complexed with Aluminum
 Borohydride
;
_journal_issue                   3
_journal_name_full               'Chemistry of Materials'
_journal_page_first              768
_journal_paper_doi               10.1021/cm503601h
_journal_volume                  27
_journal_year                    2015
_chemical_formula_moiety         'Al B4 H18 N'
_chemical_formula_sum            'Al B4 H18 N'
_chemical_formula_weight         102.37
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 107.695(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8196(8)
_cell_length_b                   7.2809(4)
_cell_length_c                   11.3260(9)
_cell_measurement_reflns_used    1222
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.6219
_cell_measurement_theta_min      3.4189
_cell_volume                     850.01(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection       MAR
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'MERCURY (Macrae et al., 2008)'
_computing_publication_material
;

'MERCURY (Macrae et al., 2008), Platon (Spek, 2009)'

;
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'MAR345 image plate'
_diffrn_measurement_method       '180 images, \D\F 1.0\% '
_diffrn_radiation_monochromator  'Zr filter'
_diffrn_radiation_source         'Rigaku UltraX 18 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_unetI/netI     0.0707
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2629
_diffrn_reflns_point_group_measured_fraction_full 0.921
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.677
_diffrn_reflns_theta_min         3.426
_exptl_absorpt_coefficient_mu    0.135
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'white translucent'
_exptl_crystal_density_diffrn    0.800
_exptl_crystal_description       block
_exptl_crystal_F_000             232
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Flack x determined using 413 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.1(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         1442
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0645
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1043P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1618
_refine_ls_wR_factor_ref         0.1801
_reflns_Friedel_coverage         0.832
_reflns_Friedel_fraction_full    0.849
_reflns_Friedel_fraction_max     0.824
_reflns_number_gt                1095
_reflns_number_total             1442
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm503601h_si_001.cif
_cod_data_source_block           yfnh4bh4_293K
_cod_depositor_comments
'Adding full bibliography for 4002168--4002169.cif.'
_cod_database_code               4002168
_shelx_estimated_absorpt_t_min   0.967
_shelx_estimated_absorpt_t_max   0.974
_shelxl_version_number           2014-3
_shelx_res_checksum              47158
_shelx_hkl_checksum              61561