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#$Date: 2016-03-23 15:53:43 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179352 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/49/4324907.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_4324907
loop_
_publ_author_name
'Zhenguo Huang'
'Xuenian Chen'
'Teshome Yisgedu'
'Edward A. Meyers'
'Sheldon G. Shore'
'Ji-Cheng Zhao'
_publ_section_title
;
 Ammonium Octahydrotriborate (NH4B3H8): New Synthesis, Structure, and
 Hydrolytic Hydrogen Release
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3738
_journal_page_last               3742
_journal_paper_doi               10.1021/ic2000987
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'B3 H8, H4 N'
_chemical_formula_sum            'B3 H12 N'
_chemical_formula_weight         58.54
_chemical_name_common            ZHAO1800
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   geom
_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            4
_cell_length_a                   7.1530(14)
_cell_length_b                   8.2648(17)
_cell_length_c                   8.3895(17)
_cell_measurement_reflns_used    861
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.72
_cell_measurement_theta_min      3.77
_cell_volume                     495.97(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'NONIUS KAPPA CCD'
_diffrn_measurement_method       'PHI SCANS & OMEGA SCANS'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_sigmaI/netI    0.0174
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            1617
_diffrn_reflns_theta_full        24.72
_diffrn_reflns_theta_max         24.72
_diffrn_reflns_theta_min         3.77
_exptl_absorpt_coefficient_mu    0.038
_exptl_absorpt_correction_T_max  0.9985
_exptl_absorpt_correction_T_min  0.9913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL SCALEPACK (OTWINOWSKI & MINOR, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.784
_exptl_crystal_description       needle
_exptl_crystal_F_000             136
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.197
_refine_diff_density_min         -0.147
_refine_diff_density_rms         0.030
_refine_ls_extinction_coef       0.019(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     32
_refine_ls_number_reflns         251
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0370
_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)+(0.0764P)²+0.0771P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1153
_reflns_number_gt                220
_reflns_number_total             251
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2000987_si_002.cif
_cod_data_source_block           c
_cod_database_code               4324907
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -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
_atom_site_refinement_flags
N1 N 0.0000 0.3221(2) 0.7500 0.0286(7) Uani 1 4 d S
B1 B 0.0000 0.9037(3) 0.7500 0.0316(8) Uani 1 4 d S
B2 B 0.0000 0.71840(17) 0.64193(16) 0.0263(6) Uani 1 2 d S
H3 H -0.1303(18) 0.6627(13) 0.6004(15) 0.040(3) Uiso 1 1 d .
H4 H 0.0000 0.843(2) 0.585(2) 0.048(5) Uiso 1 2 d S
H1 H -0.128(2) 0.973(2) 0.7500 0.044(4) Uiso 1 2 d S
H5 H 0.094(4) 0.259(4) 0.7500 0.122(11) Uiso 1 2 d S
H6 H 0.0000 0.383(5) 0.678(5) 0.19(2) Uiso 1 2 d S
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
N1 0.0344(11) 0.0236(10) 0.0279(11) 0.000 0.000 0.000
B1 0.0254(13) 0.0204(12) 0.0491(15) 0.000 0.000 0.000
B2 0.0312(10) 0.0250(9) 0.0227(9) 0.0031(6) 0.000 0.000
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'
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
H5 N1 H6 113(2) . .
B2 B1 B2 61.27(11) . 10_557
B2 B1 H4 100.8(7) 10_557 .
B2 B1 H1 117.3(7) . .
B2 B1 H1 117.3(7) 10_557 .
H4 B1 H1 100.4(4) . .
B1 B2 B2 59.37(5) . 10_557
B1 B2 H3 121.5(6) . .
B2 B2 H3 108.5(7) 10_557 .
B1 B2 H4 55.7(9) . .
B2 B2 H4 115.0(9) 10_557 .
H3 B2 H4 104.2(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 H5 0.85(3) .
N1 H6 0.79(4) .
B1 B2 1.779(2) .
B1 B2 1.779(2) 10_557
B1 H4 1.475(18) .
B1 H1 1.079(17) .
B2 B2 1.813(3) 10_557
B2 H3 1.096(13) .
B2 H4 1.137(17) .
