#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:31:43 +0100 (lun 21 de mar de 2016) $
#$Revision: 178815 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/69/4106960.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4106960
loop_
_publ_author_name
'David J. Wolstenholme'
'James T. Titah'
'Franklin N. Che'
'Kyle T. Traboulsee'
'Jenna Flogeras'
'G. Sean McGrady'
_publ_contact_author_address
;Department of Chemistry
University of New Brunswick
Fredericton, NB
E3B 5A3
Canada
;
_publ_contact_author_email       adecken@unb.ca
_publ_contact_author_fax         '(506) 453-4981'
_publ_contact_author_name        'Andreas Decken'
_publ_contact_author_phone       '(506) 453-4875'
_publ_section_title
;
 Homopolar Dihydrogen Bonding in Alkali-Metal Amidoboranes and Its
 Implications for Hydrogen Storage
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16598
_journal_page_last               16604
_journal_paper_doi               10.1021/ja206357a
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'B H5 N, Na'
_chemical_formula_sum            'B H5 N Na'
_chemical_formula_weight         52.85
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   difmap
_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            8
_cell_length_a                   5.6446(16)
_cell_length_b                   7.425(2)
_cell_length_c                   14.514(4)
_cell_measurement_reflns_used    2229
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.994
_cell_measurement_theta_min      2.7435
_cell_volume                     608.3(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker AXS SMART1000/P4'
_diffrn_measurement_method       'φ and ω 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  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0167
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3539
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.81
_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    0.191
_exptl_absorpt_correction_T_max  0.9628
_exptl_absorpt_correction_T_min  0.8699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_description       Rod
_exptl_crystal_F_000             224
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.154
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.249
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     48
_refine_ls_number_reflns         690
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.249
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0318
_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/[σ²(Fo²)+(0.0463P)²+0.1301P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.0946
_reflns_number_gt                618
_reflns_number_total             690
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja206357a_si_002.cif
_cod_data_source_block           sg110148
_cod_database_code               4106960
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
Na1 Na 1.07100(9) 1.03022(8) 0.16610(3) 0.0298(2) Uani 1 1 d
B1 B 0.5474(2) 0.9012(2) 0.14382(9) 0.0239(3) Uani 1 1 d
N1 N 0.7552(2) 0.92001(17) 0.07603(8) 0.0298(3) Uani 1 1 d
H1 H 0.790(3) 0.821(2) 0.0579(11) 0.030(4) Uiso 1 1 d
H2 H 0.721(3) 0.984(3) 0.0298(16) 0.049(5) Uiso 1 1 d
H3 H 0.605(3) 0.817(2) 0.2088(11) 0.034(4) Uiso 1 1 d
H4 H 0.486(4) 1.041(2) 0.1697(12) 0.032(4) Uiso 1 1 d
H5 H 0.377(3) 0.829(2) 0.1131(11) 0.031(4) Uiso 1 1 d
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Na1 0.0261(3) 0.0349(4) 0.0283(3) 0.0043(2) 0.00192(18) 0.0044(2)
B1 0.0239(7) 0.0260(7) 0.0217(6) -0.0014(5) 0.0003(5) -0.0003(5)
N1 0.0306(6) 0.0301(6) 0.0287(6) -0.0015(5) 0.0064(5) 0.0005(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Na1 B1 95.46(5) . 8_765
N1 Na1 B1 121.99(5) . 1_655
B1 Na1 B1 121.90(4) 8_765 1_655
N1 Na1 B1 112.03(5) . 6_656
B1 Na1 B1 114.37(4) 8_765 6_656
B1 Na1 B1 92.27(5) 1_655 6_656
N1 Na1 B1 28.43(4) . .
B1 Na1 B1 93.60(3) 8_765 .
B1 Na1 B1 140.51(6) 1_655 .
B1 Na1 B1 87.37(4) 6_656 .
N1 Na1 Na1 159.21(4) . 6_656
B1 Na1 Na1 104.56(3) 8_765 6_656
B1 Na1 Na1 50.57(3) 1_655 6_656
B1 Na1 Na1 54.41(3) 6_656 6_656
B1 Na1 Na1 141.63(3) . 6_656
N1 Na1 Na1 77.86(4) . 6_556
B1 Na1 Na1 84.07(3) 8_765 6_556
B1 Na1 Na1 141.46(4) 1_655 6_556
B1 Na1 Na1 49.38(3) 6_656 6_556
B1 Na1 Na1 49.56(3) . 6_556
Na1 Na1 Na1 98.42(3) 6_656 6_556
N1 B1 Na1 109.81(8) . 8_755
N1 B1 Na1 139.11(9) . 1_455
Na1 B1 Na1 95.16(4) 8_755 1_455
N1 B1 Na1 122.65(9) . 6_556
Na1 B1 Na1 102.71(5) 8_755 6_556
Na1 B1 Na1 80.05(4) 1_455 6_556
N1 B1 Na1 46.88(6) . .
Na1 B1 Na1 120.40(5) 8_755 .
Na1 B1 Na1 140.51(6) 1_455 .
Na1 B1 Na1 76.04(4) 6_556 .
N1 B1 H3 110.4(8) . .
Na1 B1 H3 57.4(8) 8_755 .
Na1 B1 H3 110.3(8) 1_455 .
Na1 B1 H3 53.5(8) 6_556 .
Na1 B1 H3 79.5(8) . .
N1 B1 H4 110.9(10) . .
Na1 B1 H4 139.3(10) 8_755 .
Na1 B1 H4 51.9(10) 1_455 .
Na1 B1 H4 54.1(8) 6_556 .
Na1 B1 H4 88.6(10) . .
H3 B1 H4 107.4(12) . .
N1 B1 H5 114.7(7) . .
Na1 B1 H5 54.2(7) 8_755 .
Na1 B1 H5 55.7(7) 1_455 .
Na1 B1 H5 122.7(7) 6_556 .
Na1 B1 H5 160.5(7) . .
H3 B1 H5 106.5(11) . .
H4 B1 H5 106.6(12) . .
B1 N1 Na1 104.69(8) . .
B1 N1 H1 108.3(11) . .
Na1 N1 H1 108.2(11) . .
B1 N1 H2 112.8(14) . .
Na1 N1 H2 114.7(14) . .
H1 N1 H2 107.9(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Na1 N1 2.3573(14) .
Na1 B1 2.8527(17) 8_765
Na1 B1 2.8728(16) 1_655
Na1 B1 2.9234(16) 6_656
Na1 B1 3.1237(17) .
Na1 Na1 3.7278(10) 6_656
Na1 Na1 3.7278(10) 6_556
B1 N1 1.5372(17) .
B1 Na1 2.8527(17) 8_755
B1 Na1 2.8728(16) 1_455
B1 Na1 2.9234(16) 6_556
B1 H3 1.179(16) .
B1 H4 1.156(18) .
B1 H5 1.187(15) .
N1 H1 0.805(17) .
N1 H2 0.84(2) .
