#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/37/4103784.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_4103784
loop_
_publ_author_name
'Chang Won Yoon'
'Patrick J. Carroll'
'Larry G. Sneddon'
_publ_section_title
;
 Ammonia Triborane: A New Synthesis, Structural Determinations, and
 Hydrolytic Hydrogen-Release Properties
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              855
_journal_page_last               864
_journal_paper_doi               10.1021/ja808045p
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'B3 H10 N'
_chemical_formula_weight         56.52
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.141(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.358(3)
_cell_length_b                   4.8041(12)
_cell_length_c                   9.967(3)
_cell_measurement_temperature    143(1)
_cell_volume                     449.0(2)
_computing_data_collection       'CrystalClear (Rigaku, 1999)'
_computing_data_reduction        'CrystalClear (Rigaku, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      143(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       'phi and omega rotations'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3496
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.74
_exptl_absorpt_coefficient_mu    0.041
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    0.836
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             128
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.159
_refine_diff_density_min         -0.173
_refine_diff_density_rms         0.030
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         791
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0411
_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)+(0.0513P)²+0.1018P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1098
_reflns_number_gt                722
_reflns_number_total             791
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja808045p_si_002_2.cif
_cod_data_source_block           Penn3323
_cod_original_cell_volume        448.9(2)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'H10 B3 N'
_cod_database_code               4103784
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x+1/2, -y+1/2, z+1/2'
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
B1 B 0.59812(13) 0.6803(3) 0.38641(13) 0.0241(4) Uani 1 1 d
B2 B 0.43554(14) 0.5386(3) 0.24217(14) 0.0309(4) Uani 1 1 d
B3 B 0.56389(14) 0.6849(3) 0.19384(14) 0.0315(4) Uani 1 1 d
N4 N 0.70030(11) 0.4390(2) 0.48165(11) 0.0283(4) Uani 1 1 d
H1A H 0.5515(14) 0.792(3) 0.4511(14) 0.041(4) Uiso 1 1 d
H1B H 0.6642(14) 0.831(3) 0.3593(14) 0.043(4) Uiso 1 1 d
H2A H 0.4360(13) 0.321(3) 0.2718(14) 0.037(3) Uiso 1 1 d
H2B H 0.3411(15) 0.666(3) 0.2258(14) 0.041(4) Uiso 1 1 d
H3A H 0.6433(14) 0.557(3) 0.1801(15) 0.038(3) Uiso 1 1 d
H3B H 0.5381(15) 0.883(3) 0.1365(15) 0.044(4) Uiso 1 1 d
H23 H 0.4458(15) 0.527(3) 0.1289(15) 0.047(4) Uiso 1 1 d
H4A H 0.655(2) 0.308(4) 0.505(2) 0.067(5) Uiso 1 1 d
H4B H 0.767(2) 0.499(4) 0.571(2) 0.071(5) Uiso 1 1 d
H4C H 0.7423(18) 0.356(4) 0.4341(19) 0.058(5) 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
B1 0.0254(7) 0.0227(7) 0.0241(7) 0.0004(5) 0.0105(5) 0.0010(5)
B2 0.0233(7) 0.0414(9) 0.0239(7) 0.0038(5) 0.0062(5) -0.0004(6)
B3 0.0305(7) 0.0398(9) 0.0271(7) 0.0051(5) 0.0148(5) 0.0036(6)
N4 0.0247(6) 0.0310(7) 0.0245(6) 0.0003(4) 0.0058(5) 0.0019(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
N4 B1 B3 115.28(9)
N4 B1 B2 110.98(9)
B3 B1 B2 57.61(7)
N4 B1 H1A 110.9(7)
B3 B1 H1A 133.2(7)
B2 B1 H1A 99.1(7)
N4 B1 H1B 107.5(7)
B3 B1 H1B 66.0(7)
B2 B1 H1B 120.9(7)
H1A B1 H1B 107.0(10)
B3 B2 B1 60.58(7)
B3 B2 H2A 123.2(7)
B1 B2 H2A 104.5(7)
B3 B2 H2B 117.9(7)
B1 B2 H2B 112.0(7)
H2A B2 H2B 118.2(10)
B3 B2 H23 50.5(7)
B1 B2 H23 110.1(7)
H2A B2 H23 103.0(10)
H2B B2 H23 108.6(10)
B2 B3 B1 61.81(7)
B2 B3 H3A 121.2(7)
B1 B3 H3A 108.3(7)
B2 B3 H3B 117.0(7)
B1 B3 H3B 117.8(7)
H3A B3 H3B 117.5(10)
B2 B3 H23 42.5(6)
B1 B3 H23 103.5(6)
H3A B3 H23 101.9(9)
H3B B3 H23 105.7(9)
B1 N4 H4A 112.9(12)
B1 N4 H4B 113.0(12)
H4A N4 H4B 104.1(16)
B1 N4 H4C 112.0(11)
H4A N4 H4C 105.1(16)
H4B N4 H4C 109.3(17)
B2 H23 B3 87.0(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
B1 N4 1.5849(15)
B1 B3 1.7976(17)
B1 B2 1.8190(18)
B1 H1A 1.097(13)
B1 H1B 1.106(14)
B2 B3 1.7427(19)
B2 H2A 1.087(14)
B2 H2B 1.105(14)
B2 H23 1.179(14)
B3 H3A 1.080(14)
B3 H3B 1.085(14)
B3 H23 1.347(14)
B3 H1B 1.685(13)
N4 H4A 0.87(2)
N4 H4B 0.91(2)
N4 H4C 0.866(19)
