#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:35:38 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178817 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/71/4107183.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_4107183
loop_
_publ_author_name
'Wei Luo'
'Patrick G. Campbell'
'Lev N. Zakharov'
'Shih-Yuan Liu'
_publ_section_title
;
 A Single-Component Liquid-Phase Hydrogen Storage Material
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              19326
_journal_page_last               19329
_journal_paper_doi               10.1021/ja208834v
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C4 H12 B N'
_chemical_formula_weight         84.96
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXLTL
_cell_angle_alpha                90.00
_cell_angle_beta                 117.149(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.919(3)
_cell_length_b                   7.278(2)
_cell_length_c                   9.294(3)
_cell_measurement_reflns_used    1128
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.45
_cell_measurement_theta_min      2.31
_cell_volume                     597.0(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Apex CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0222
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4558
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    0.053
_exptl_absorpt_correction_T_max  0.9963
_exptl_absorpt_correction_T_min  0.9651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.945
_exptl_crystal_description       needle
_exptl_crystal_F_000             192
_exptl_crystal_size_max          0.67
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.231
_refine_diff_density_min         -0.148
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         1053
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0710
_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)+(0.1001P)²+0.2805P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1978
_refine_ls_wR_factor_ref         0.2147
_reflns_number_gt                816
_reflns_number_total             1053
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja208834v_si_002.cif
_cod_data_source_block           liu113n
_cod_original_cell_volume        597.1(3)
_cod_database_code               4107183
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.1079(3) 1.2248(3) 0.6635(3) 0.0452(7) Uani 1 1 d . . .
C1 C 0.2706(3) 1.2591(4) 0.7138(4) 0.0610(9) Uani 1 1 d . A .
B1 B 0.0996(3) 1.0336(4) 0.7453(4) 0.0513(9) Uani 0.50 1 d PD A 1
H1BA H 0.0312 0.9450 0.6638 0.062 Uiso 0.50 1 calc PRD A 1
H1BB H 0.0661 1.0517 0.8296 0.062 Uiso 0.50 1 calc PRD A 1
C2 C 0.3391(3) 1.0758(5) 0.7282(5) 0.0778(11) Uani 0.50 1 d PD A 1
H2A H 0.4511 1.0831 0.7855 0.093 Uiso 0.50 1 calc PR A 1
H2B H 0.3077 1.0204 0.6203 0.093 Uiso 0.50 1 calc PR A 1
C3 C 0.2793(4) 0.9659(6) 0.8246(5) 0.0500(10) Uani 0.673(5) 1 d PD A 1
H3A H 0.3325 1.0061 0.9401 0.060 Uiso 0.673(5) 1 calc PR A 1
C4 C 0.3026(15) 0.7616(15) 0.8164(13) 0.081(2) Uani 0.673(5) 1 d PD A 1
H4A H 0.4113 0.7349 0.8647 0.121 Uiso 0.673(5) 1 calc PR A 1
H4B H 0.2540 0.7217 0.7032 0.121 Uiso 0.673(5) 1 calc PR A 1
H4C H 0.2577 0.6957 0.8759 0.121 Uiso 0.673(5) 1 calc PR A 1
B1A B 0.0996(3) 1.0336(4) 0.7453(4) 0.0513(9) Uani 0.50 1 d PD A 2
H1BC H -0.0017 0.9762 0.6871 0.062 Uiso 0.50 1 calc PRD A 2
H1BD H 0.1243 1.0500 0.8604 0.062 Uiso 0.50 1 calc PRD A 2
C2A C 0.3391(3) 1.0758(5) 0.7282(5) 0.0778(11) Uani 0.50 1 d PD A 2
H2AA H 0.4346 1.0694 0.8304 0.093 Uiso 0.50 1 calc PR A 2
H2AB H 0.3644 1.0576 0.6377 0.093 Uiso 0.50 1 calc PR A 2
C3A C 0.2277(8) 0.9142(11) 0.7258(10) 0.0500(10) Uani 0.327(5) 1 d PD A 2
H3AA H 0.1841 0.8463 0.6207 0.060 Uiso 0.327(5) 1 calc PR A 2
C4A C 0.302(4) 0.786(4) 0.866(3) 0.081(2) Uani 0.327(5) 1 d PD A 2
H4AA H 0.3809 0.7159 0.8549 0.121 Uiso 0.327(5) 1 calc PR A 2
H4AB H 0.2257 0.7010 0.8675 0.121 Uiso 0.327(5) 1 calc PR A 2
H4AC H 0.3467 0.8564 0.9666 0.121 Uiso 0.327(5) 1 calc PR A 2
H1N H 0.064(3) 1.215(3) 0.566(3) 0.044(8) Uiso 1 1 d . . .
H2N H 0.057(3) 1.318(4) 0.684(3) 0.064(8) Uiso 1 1 d . . .
H1C H 0.280(3) 1.341(5) 0.647(4) 0.069(9) Uiso 1 1 d . . .
H1D H 0.305(4) 1.322(5) 0.813(4) 0.093(12) 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
N1 0.0552(14) 0.0434(13) 0.0429(14) 0.0019(10) 0.0275(11) 0.0048(10)
C1 0.0624(19) 0.0618(19) 0.0613(19) 0.0041(15) 0.0302(15) -0.0116(14)
B1 0.0607(19) 0.0445(17) 0.0636(19) 0.0075(14) 0.0414(16) 0.0028(13)
C2 0.0551(18) 0.081(2) 0.106(3) 0.026(2) 0.0437(18) 0.0094(16)
C3 0.051(2) 0.054(2) 0.049(2) 0.0039(18) 0.027(2) 0.0043(17)
C4 0.083(3) 0.067(4) 0.118(7) 0.023(5) 0.067(5) 0.030(3)
B1A 0.0607(19) 0.0445(17) 0.0636(19) 0.0075(14) 0.0414(16) 0.0028(13)
C2A 0.0551(18) 0.081(2) 0.106(3) 0.026(2) 0.0437(18) 0.0094(16)
C3A 0.051(2) 0.054(2) 0.049(2) 0.0039(18) 0.027(2) 0.0043(17)
C4A 0.083(3) 0.067(4) 0.118(7) 0.023(5) 0.067(5) 0.030(3)
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C1 N1 B1 106.3(2)
C1 N1 H1N 109.0(18)
B1 N1 H1N 109.5(19)
C1 N1 H2N 115.7(18)
B1 N1 H2N 113.0(18)
H1N N1 H2N 103(2)
C2 C1 N1 105.5(2)
C2 C1 H1C 118(2)
N1 C1 H1C 109.8(19)
C2 C1 H1D 114(2)
N1 C1 H1D 104(2)
H1C C1 H1D 105(3)
N1 B1 C3 101.0(2)
N1 B1 H1BA 111.6
C3 B1 H1BA 111.6
N1 B1 H1BB 111.6
C3 B1 H1BB 111.6
H1BA B1 H1BB 109.4
C1 C2 C3 104.0(3)
C1 C2 H2A 110.9
C3 C2 H2A 110.9
C1 C2 H2B 110.9
C3 C2 H2B 110.9
H2A C2 H2B 109.0
C2 C3 C4 112.3(5)
C2 C3 B1 102.3(3)
C4 C3 B1 115.3(6)
C2 C3 H3A 108.9
C4 C3 H3A 108.9
B1 C3 H3A 108.9
C3 C4 H4A 109.5
C3 C4 H4B 109.5
H4A C4 H4B 109.5
C3 C4 H4C 109.5
H4A C4 H4C 109.5
H4B C4 H4C 109.5
C4A C3A H3AA 111.3
C3A C4A H4AA 109.5
C3A C4A H4AB 109.5
H4AA C4A H4AB 109.5
C3A C4A H4AC 109.5
H4AA C4A H4AC 109.5
H4AB C4A H4AC 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
N1 C1 1.482(4)
N1 B1 1.606(3)
N1 H1N 0.81(3)
N1 H2N 0.92(3)
C1 C2 1.475(5)
C1 H1C 0.90(3)
C1 H1D 0.95(4)
B1 C3 1.662(5)
B1 H1BA 0.9900
B1 H1BB 0.9900
C2 C3 1.510(5)
C2 H2A 0.9900
C2 H2B 0.9900
C3 C4 1.512(10)
C3 H3A 1.0000
C4 H4A 0.9800
C4 H4B 0.9800
C4 H4C 0.9800
C3A C4A 1.494(18)
C3A H3AA 1.0000
C4A H4AA 0.9800
C4A H4AB 0.9800
C4A H4AC 0.9800
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
B1 N1 C1 C2 32.5(3)
C1 N1 B1 C3 -6.6(3)
N1 C1 C2 C3 -47.4(4)
C1 C2 C3 C4 165.1(6)
C1 C2 C3 B1 40.9(4)
N1 B1 C3 C2 -20.4(3)
N1 B1 C3 C4 -142.6(5)
