#------------------------------------------------------------------------------
#$Date: 2016-02-20 01:53:41 +0100 (Sat 20 de Feb de 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/20/2102029.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2102029
loop_
_publ_author_name
'Steiner, Thomas'
'Mason, Sax A.'
_publ_section_title
;
 Short N⁺---H···Ph hydrogen bonds in ammonium
 tetraphenylborate characterized by neutron diffraction
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              254
_journal_page_last               260
_journal_paper_doi               10.1107/S0108768199012318
_journal_volume                  56
_journal_year                    2000
_chemical_formula_moiety         'N H4 +,C24 H20 B -'
_chemical_formula_sum            'C24 H24 B N'
_chemical_formula_weight         337.27
_chemical_name_common            'ammonium tetraphenylborate'
_chemical_name_systematic
;
 ammonium tetraphenylborate
;
_space_group_IT_number           121
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4 2'
_symmetry_space_group_name_H-M   'I -4 2 m'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.1208(8)
_cell_length_b                   11.1208(8)
_cell_length_c                   8.0033(7)
_cell_measurement_reflns_used    354
_cell_measurement_temperature    20
_cell_measurement_theta_max      44.39
_cell_measurement_theta_min      3.08
_cell_volume                     989.79(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      20
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  D9
_diffrn_measurement_method       'area detector'
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         'ILL high flux neutron reactor'
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     .8469
_diffrn_reflns_av_R_equivalents  .0303
_diffrn_reflns_av_sigmaI/netI    .0599
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1278
_diffrn_reflns_theta_full        45.07
_diffrn_reflns_theta_max         45.07
_diffrn_reflns_theta_min         3.09
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .064
_exptl_absorpt_correction_T_max  .826
_exptl_absorpt_correction_T_min  .761
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            'colorless transparent'
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             360
_exptl_crystal_size_max          1.72
_exptl_crystal_size_mid          1.00
_exptl_crystal_size_min          .83
_refine_diff_density_max         1.376
_refine_diff_density_min         -1.139
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   .0(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     65
_refine_ls_number_reflns         736
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          .0516
_refine_ls_R_factor_gt           .0382
_refine_ls_shift/su_max          .000
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+5.0563P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .0659
_reflns_number_gt                639
_reflns_number_total             736
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ka0046.cif
_cod_data_source_block           lt
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Gaussian' changed to 'gaussian'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic 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               2102029
_cod_database_fobs_code          2102029
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x, y, -z'
'x, -y, -z'
'-y, -x, z'
'y, x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
B .0000 .0000 .0000 .0034(5) Uani d S 1 B
N .0000 .0000 .5000 .0080(3) Uani d S 1 N
C1 .08200(9) .08200(9) .12672(18) .0048(2) Uani d S 1 C
C2 .04000(9) .19147(9) .19306(14) .00640(16) Uani d . 1 C
C3 .10202(9) .25438(9) .31756(14) .00746(17) Uani d . 1 C
C4 .20961(10) .20961(10) .38113(19) .0079(2) Uani d S 1 C
H2 -.0455(2) .2280(2) .1484(3) .0209(5) Uani d . 1 H
H3 .0649(3) .3379(2) .3653(4) .0239(5) Uani d . 1 H
H4 .2569(3) .2569(3) .4807(5) .0228(7) Uani d S 1 H
H5 .0491(5) .0491(5) .4288(12) .092(4) Uani d S 1 H
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
B .0033(7) .0033(7) .0036(12) .000 .000 .000
N .0085(5) .0085(5) .0070(8) .000 .000 .000
C1 .0050(3) .0050(3) .0044(5) .0004(4) -.0008(3) -.0008(3)
C2 .0069(3) .0055(4) .0067(3) .0002(3) -.0007(3) -.0017(4)
C3 .0085(4) .0064(4) .0074(4) .0000(3) -.0003(4) -.0018(3)
C4 .0082(3) .0082(3) .0073(5) -.0010(5) -.0016(4) -.0016(4)
H2 .0149(9) .0235(11) .0243(11) .0074(8) -.0058(9) -.0055(9)
H3 .0270(12) .0175(10) .0274(11) .0062(9) -.0025(11) -.0096(9)
H4 .0233(9) .0233(9) .0217(16) -.0011(13) -.0079(10) -.0079(10)
H5 .104(5) .104(5) .069(5) -.059(6) .029(3) .029(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B .0000 .2130 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
C1 B C1 4 3 103.64(10)
C1 B C1 4 2 112.46(5)
C1 B C1 3 2 112.46(5)
C1 B C1 4 . 112.46(5)
C1 B C1 3 . 112.46(5)
C1 B C1 2 . 103.64(10)
C2 C1 C2 . 8 115.56(13)
C2 C1 B . . 121.96(6)
C2 C1 B 8 . 121.96(6)
C3 C2 C1 . . 122.50(10)
C3 C2 H2 . . 118.37(17)
C1 C2 H2 . . 119.11(17)
C4 C3 C2 . . 120.34(11)
C4 C3 H3 . . 120.28(19)
C2 C3 H3 . . 119.38(18)
C3 C4 C3 . 8 118.76(14)
C3 C4 H4 . . 120.62(7)
C3 C4 H4 8 . 120.62(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
B C1 4 1.6406(14)
B C1 3 1.6406(14)
B C1 2 1.6406(14)
B C1 . 1.6407(14)
N H5 . .960(7)
C1 C2 . 1.4078(13)
C1 C2 8 1.4078(13)
C2 C3 . 1.3993(14)
C2 H2 . 1.095(3)
C3 C4 . 1.3922(13)
C3 H3 . 1.086(3)
C4 C3 8 1.3922(13)
C4 H4 . 1.089(4)
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_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
C1 B C1 C2 4 . 36.02(9)
C1 B C1 C2 3 . 152.58(14)
C1 B C1 C2 2 . -85.70(11)
C1 B C1 C2 4 8 -152.57(14)
C1 B C1 C2 3 8 -36.02(9)
C1 B C1 C2 2 8 85.70(11)
C2 C1 C2 C3 8 . -.4(2)
B C1 C2 C3 . . 171.48(10)
C1 C2 C3 C4 . . -.03(17)
C2 C3 C4 C3 . 8 .5(2)
