#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:14:19 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178774 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/28/4102815.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_4102815
loop_
_publ_author_name
'Xuenian Chen'
'Ji-Cheng Zhao'
'Sheldon G. Shore'
_publ_section_title
;
 Facile Synthesis of Aminodiborane and Inorganic Butane Analogue
 NH3BH2NH2BH3
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10658
_journal_page_last               10659
_journal_paper_doi               10.1021/ja104938v
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C12 H24 O6, 2(B2 H7 N)'
_chemical_formula_sum            'C12 H38 B4 N2 O6'
_chemical_formula_weight         349.68
_chemical_name_common            ZHAO1770
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                117.05(3)
_cell_angle_beta                 97.77(3)
_cell_angle_gamma                107.32(3)
_cell_formula_units_Z            1
_cell_length_a                   8.4990(17)
_cell_length_b                   8.5720(17)
_cell_length_c                   8.8830(18)
_cell_measurement_reflns_used    1815
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.26
_cell_volume                     521.6(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0190
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            13189
_diffrn_reflns_theta_full        24.94
_diffrn_reflns_theta_max         24.94
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.9880
_exptl_absorpt_correction_T_min  0.9848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL SCALEPACK (OTWINOWSKI & MINOR, 1997)'
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             192
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         1821
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0460
_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)+(0.0877P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1293
_reflns_number_gt                1392
_reflns_number_total             1821
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja104938v_si_002.cif
_cod_data_source_block           p
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'TRICLINIC' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'MULTI-SCAN'
changed to 'multi-scan' 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 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               4102815
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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 0.68835(19) 0.2370(2) 0.10567(17) 0.0309(4) Uani 1 1 d .
H2 H 0.715(2) 0.139(3) 0.086(2) 0.043(5) Uiso 1 1 d .
H1 H 0.591(2) 0.224(2) 0.129(2) 0.038(5) Uiso 1 1 d .
B1 B 0.7267(3) 0.3124(3) -0.0174(3) 0.0387(5) Uani 1 1 d .
H4 H 0.631(2) 0.359(2) -0.057(2) 0.050(5) Uiso 1 1 d .
H3 H 0.797(2) 0.243(2) -0.112(2) 0.040(4) Uiso 1 1 d .
B2 B 0.8394(3) 0.4346(3) 0.2320(2) 0.0352(5) Uani 1 1 d .
H6 H 0.961(2) 0.433(2) 0.276(2) 0.040(4) Uiso 1 1 d .
H7 H 0.857(2) 0.476(2) 0.108(2) 0.038(4) Uiso 1 1 d .
H5 H 0.800(2) 0.545(2) 0.326(2) 0.048(5) Uiso 1 1 d .
O1 O 0.78371(13) -0.08753(14) 0.07127(13) 0.0320(3) Uani 1 1 d .
O2 O 0.63891(13) 0.06348(14) 0.35060(12) 0.0320(3) Uani 1 1 d .
O3 O 0.41610(13) 0.23888(14) 0.29116(12) 0.0318(3) Uani 1 1 d .
C1 C 0.7848(2) -0.2456(2) -0.0825(2) 0.0358(4) Uani 1 1 d .
H1A H 0.6908 -0.3660 -0.1119 0.043 Uiso 1 1 calc R
H1B H 0.8972 -0.2562 -0.0587 0.043 Uiso 1 1 calc R
C2 C 0.8049(2) -0.1084(2) 0.2226(2) 0.0347(4) Uani 1 1 d .
H2A H 0.9148 -0.1232 0.2491 0.042 Uiso 1 1 calc R
H2B H 0.7074 -0.2240 0.1978 0.042 Uiso 1 1 calc R
C3 C 0.8086(2) 0.0661(2) 0.3785(2) 0.0343(4) Uani 1 1 d .
H3A H 0.8457 0.0669 0.4895 0.041 Uiso 1 1 calc R
H3B H 0.8923 0.1831 0.3905 0.041 Uiso 1 1 calc R
C4 C 0.6324(2) 0.2318(2) 0.48642(19) 0.0354(4) Uani 1 1 d .
H4A H 0.7149 0.3467 0.4941 0.042 Uiso 1 1 calc R
H4B H 0.6657 0.2428 0.6032 0.042 Uiso 1 1 calc R
C5 C 0.4515(2) 0.2195(2) 0.44204(19) 0.0343(4) Uani 1 1 d .
H5A H 0.3676 0.0945 0.4152 0.041 Uiso 1 1 calc R
H5B H 0.4387 0.3225 0.5453 0.041 Uiso 1 1 calc R
C6 C 0.2413(2) 0.2156(2) 0.2353(2) 0.0337(4) Uani 1 1 d .
H6A H 0.2169 0.3095 0.3352 0.040 Uiso 1 1 calc R
H6B H 0.1604 0.0851 0.1985 0.040 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
B B 0.0013 0.0007 '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'
O O 0.0106 0.0060 '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
B1 N1 B2 77.00(12) . .
B1 N1 H2 114.8(11) . .
B2 N1 H2 114.3(11) . .
B1 N1 H1 119.0(11) . .
B2 N1 H1 115.3(11) . .
H2 N1 H1 112.2(16) . .
N1 B1 B2 51.75(10) . .
N1 B1 H4 114.6(9) . .
B2 B1 H4 117.0(9) . .
N1 B1 H3 115.1(8) . .
B2 B1 H3 117.2(8) . .
H4 B1 H3 121.5(12) . .
N1 B1 H7 95.3(7) . .
B2 B1 H7 43.5(7) . .
H4 B1 H7 103.1(11) . .
H3 B1 H7 101.1(10) . .
N1 B2 B1 51.25(10) . .
N1 B2 H6 115.8(9) . .
B1 B2 H6 119.4(8) . .
N1 B2 H7 95.1(7) . .
B1 B2 H7 43.9(7) . .
H6 B2 H7 103.0(11) . .
N1 B2 H5 114.0(9) . .
B1 B2 H5 118.0(8) . .
H6 B2 H5 119.5(12) . .
H7 B2 H5 104.7(10) . .
C1 O1 C2 112.23(11) . .
C3 O2 C4 112.56(12) . .
C6 O3 C5 112.02(11) . .
O1 C1 C6 109.15(12) . 2_655
O1 C1 H1A 109.9 . .
C6 C1 H1A 109.8 2_655 .
O1 C1 H1B 109.8 . .
C6 C1 H1B 109.9 2_655 .
H1A C1 H1B 108.3 . .
O1 C2 C3 108.52(12) . .
O1 C2 H2A 110.0 . .
C3 C2 H2A 110.0 . .
O1 C2 H2B 110.0 . .
C3 C2 H2B 110.0 . .
H2A C2 H2B 108.4 . .
O2 C3 C2 108.52(13) . .
O2 C3 H3A 110.0 . .
C2 C3 H3A 110.0 . .
O2 C3 H3B 110.0 . .
C2 C3 H3B 110.0 . .
H3A C3 H3B 108.4 . .
O2 C4 C5 108.66(13) . .
O2 C4 H4A 110.0 . .
C5 C4 H4A 110.0 . .
O2 C4 H4B 110.0 . .
C5 C4 H4B 110.0 . .
H4A C4 H4B 108.3 . .
O3 C5 C4 109.48(12) . .
O3 C5 H5A 109.8 . .
C4 C5 H5A 109.8 . .
O3 C5 H5B 109.8 . .
C4 C5 H5B 109.8 . .
H5A C5 H5B 108.2 . .
O3 C6 C1 109.27(13) . 2_655
O3 C6 H6A 109.8 . .
C1 C6 H6A 109.8 2_655 .
O3 C6 H6B 109.8 . .
C1 C6 H6B 109.8 2_655 .
H6A C6 H6B 108.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 B1 1.527(2) .
N1 B2 1.538(3) .
N1 H2 0.882(19) .
N1 H1 0.869(18) .
B1 B2 1.908(3) .
B1 H4 1.092(17) .
B1 H3 1.140(16) .
B1 H7 1.324(16) .
B2 H6 1.064(17) .
B2 H7 1.316(15) .
B2 H5 1.116(16) .
O1 C1 1.4247(18) .
O1 C2 1.4302(18) .
O2 C3 1.4212(18) .
O2 C4 1.4224(18) .
O3 C6 1.4234(19) .
O3 C5 1.4277(17) .
C1 C6 1.492(2) 2_655
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 C3 1.495(2) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 C5 1.493(2) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 C1 1.492(2) 2_655
C6 H6A 0.9900 .
C6 H6B 0.9900 .
