#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/32/24/4322455.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_4322455
loop_
_publ_author_name
'Hans-Hermann Giese'
'Tassilo Habereder'
'Heinrich Nöth'
'Werner Ponikwar'
'Steffen Thomas'
'Marcus Warchhold'
_publ_contact_author
;
      Heinrich Nöth
      Institut für anorganische Chemie
      Universität München
      Meiserstr. 1
      80333 München
      Bundesrepublik Deutschland
;
_publ_contact_author_email       H.Noeth@lrz.uni-muenchen.de
_publ_contact_author_fax         '089 5902 451'
_publ_contact_author_phone       '089 5902 396'
_publ_section_title
;
 Metal Tetrahydridoborates and Tetrahydridoborato Metalates. 23.1 Amine
 Solvates of Lithium and Sodium Tetrahydridoborate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4188
_journal_page_last               4196
_journal_paper_doi               10.1021/ic990205c
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C15 H19 B Li N3'
_chemical_formula_weight         259.08
_chemical_name_systematic
; 

Lithium Tetrahydridoborate 3 Pyridine

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-CIF-file updated by CIFRTF'
_cell_angle_alpha                90.00
_cell_angle_beta                 94.721(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9939(5)
_cell_length_b                   9.9171(4)
_cell_length_c                   14.8260(8)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    193
_cell_measurement_theta_max      11.74
_cell_measurement_theta_min      4.02
_cell_volume                     1610.96(13)
_computing_cell_refinement       'SMART (V4.C50)'
_computing_data_collection       'SMART (V4.C50)'
_computing_data_reduction        'SAINT (V4.D50)'
_computing_molecular_graphics    'XP (SHELXTL-Ver.5)'
_computing_publication_material  'SHELXL (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193
_diffrn_measured_fraction_theta_full 0.747
_diffrn_measured_fraction_theta_max 0.747
_diffrn_measurement_device_type  'Siemens SMART Area-detector'
_diffrn_measurement_method       Hemisphere
_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  0.0586
_diffrn_reflns_av_sigmaI/netI    0.0515
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7296
_diffrn_reflns_theta_full        24.70
_diffrn_reflns_theta_max         24.70
_diffrn_reflns_theta_min         2.22
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    0.063
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.068
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.170
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         2050
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0538P)²+0.1860P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1266
_reflns_number_gt                1314
_reflns_number_total             2050
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990205c_1.cif
_cod_data_source_block           noeth50
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'mixed ' changed to 'mixed'
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 1673 2011-04-08 12:14:43Z adriana 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

'_atom_sites_solution_hydrogens' value 'geometrically' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_database_code               4322455
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
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Li Li 0.4041(4) 0.1979(5) 0.2815(3) 0.0532(13) Uani 1 1 d . . .
B B 0.5312(4) 0.0041(6) 0.3136(3) 0.0639(12) Uani 1 1 d . . .
N1 N 0.48438(19) 0.3871(2) 0.29676(14) 0.0498(7) Uani 1 1 d . . .
N11 N 0.34233(19) 0.1946(3) 0.14559(14) 0.0478(7) Uani 1 1 d . . .
N21 N 0.26323(19) 0.1994(2) 0.36548(14) 0.0486(7) Uani 1 1 d . . .
C2 C 0.5802(3) 0.4118(4) 0.24897(19) 0.0539(9) Uani 1 1 d . . .
H2 H 0.596(2) 0.340(3) 0.206(2) 0.066(9) Uiso 1 1 d . . .
C3 C 0.6499(3) 0.5251(4) 0.2580(2) 0.0634(11) Uani 1 1 d . . .
H3 H 0.715(3) 0.534(3) 0.2245(18) 0.065(9) Uiso 1 1 d . . .
C4 C 0.6207(3) 0.6204(5) 0.3189(3) 0.0730(11) Uani 1 1 d . . .
H4 H 0.661(3) 0.704(4) 0.325(2) 0.076(12) Uiso 1 1 d . . .
C5 C 0.5244(3) 0.5997(5) 0.3687(3) 0.0738(11) Uani 1 1 d . . .
H5 H 0.499(3) 0.660(4) 0.412(2) 0.090(11) Uiso 1 1 d . . .
C6 C 0.4586(3) 0.4826(4) 0.3563(2) 0.0606(10) Uani 1 1 d . . .
H6 H 0.390(3) 0.459(3) 0.389(2) 0.085(11) Uiso 1 1 d . . .
C12 C 0.3671(3) 0.0905(4) 0.0937(2) 0.0532(9) Uani 1 1 d . . .
H12 H 0.420(2) 0.022(3) 0.1185(16) 0.048(8) Uiso 1 1 d . . .
C13 C 0.3235(3) 0.0765(4) 0.0047(2) 0.0642(10) Uani 1 1 d . . .
H13 H 0.348(2) -0.003(3) -0.0295(19) 0.064(9) Uiso 1 1 d . . .
C14 C 0.2494(3) 0.1760(5) -0.0335(2) 0.0691(11) Uani 1 1 d . . .
H14 H 0.217(3) 0.169(3) -0.097(2) 0.094(11) Uiso 1 1 d . . .
C15 C 0.2222(3) 0.2850(5) 0.0178(2) 0.0630(10) Uani 1 1 d . . .
H15 H 0.171(3) 0.355(3) -0.005(2) 0.074(11) Uiso 1 1 d . . .
C16 C 0.2703(3) 0.2901(4) 0.1071(2) 0.0520(9) Uani 1 1 d . . .
H16 H 0.253(2) 0.371(3) 0.1444(19) 0.070(10) Uiso 1 1 d . . .
C22 C 0.2858(3) 0.1526(3) 0.45029(18) 0.0551(9) Uani 1 1 d . . .
H22 H 0.369(2) 0.129(2) 0.4681(16) 0.052(8) Uiso 1 1 d . . .
C23 C 0.1972(3) 0.1375(3) 0.5099(2) 0.0604(9) Uani 1 1 d . . .
H23 H 0.223(2) 0.096(3) 0.572(2) 0.073(9) Uiso 1 1 d . . .
C24 C 0.0792(3) 0.1699(3) 0.4818(2) 0.0606(9) Uani 1 1 d . . .
H24 H 0.016(3) 0.160(3) 0.521(2) 0.076(9) Uiso 1 1 d . . .
C25 C 0.0546(3) 0.2195(3) 0.3956(2) 0.0602(9) Uani 1 1 d . . .
H25 H -0.028(3) 0.243(3) 0.3712(17) 0.061(8) Uiso 1 1 d . . .
C26 C 0.1476(3) 0.2328(3) 0.3404(2) 0.0545(9) Uani 1 1 d . . .
H26 H 0.134(2) 0.273(3) 0.2822(19) 0.058(8) Uiso 1 1 d . . .
HA H 0.427(3) -0.006(3) 0.2999(18) 0.074(8) Uiso 1 1 d . . .
HB H 0.574(4) -0.070(4) 0.274(3) 0.138(15) Uiso 1 1 d . . .
HC H 0.564(3) 0.111(4) 0.306(2) 0.123(15) Uiso 1 1 d . . .
HD H 0.565(4) -0.032(5) 0.381(3) 0.177(19) Uiso 1 1 d . . .
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'
Li Li -0.0003 0.0001 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N21 Li N11 112.6(2) . . ?
N21 Li N1 105.1(2) . . ?
N11 Li N1 102.8(2) . . ?
N21 Li B 109.8(2) . . ?
N11 Li B 108.6(2) . . ?
N1 Li B 117.8(2) . . ?
C2 N1 C6 115.9(3) . . ?
C2 N1 Li 116.9(2) . . ?
C6 N1 Li 126.8(2) . . ?
C12 N11 C16 116.6(3) . . ?
C12 N11 Li 120.6(3) . . ?
C16 N11 Li 122.7(2) . . ?
C26 N21 C22 116.3(2) . . ?
C26 N21 Li 125.3(2) . . ?
C22 N21 Li 118.1(2) . . ?
N1 C2 C3 124.0(3) . . ?
C2 C3 C4 118.5(4) . . ?
C5 C4 C3 119.5(4) . . ?
C4 C5 C6 118.8(4) . . ?
N1 C6 C5 123.2(3) . . ?
N11 C12 C13 124.2(4) . . ?
C14 C13 C12 118.2(4) . . ?
C15 C14 C13 119.2(3) . . ?
C14 C15 C16 118.5(4) . . ?
N11 C16 C15 123.4(4) . . ?
N21 C22 C23 123.5(3) . . ?
C24 C23 C22 118.8(3) . . ?
C23 C24 C25 118.4(3) . . ?
C26 C25 C24 119.4(3) . . ?
N21 C26 C25 123.4(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Li N21 2.065(5) . ?
Li N11 2.074(5) . ?
Li N1 2.078(6) . ?
Li B 2.401(7) . ?
N1 C2 1.340(3) . ?
N1 C6 1.341(4) . ?
N11 C12 1.329(4) . ?
N11 C16 1.332(4) . ?
N21 C26 1.337(3) . ?
N21 C22 1.344(3) . ?
C2 C3 1.361(4) . ?
C3 C4 1.363(5) . ?
C4 C5 1.355(5) . ?
C5 C6 1.372(5) . ?
C12 C13 1.374(4) . ?
C13 C14 1.372(5) . ?
C14 C15 1.369(5) . ?
C15 C16 1.386(4) . ?
C22 C23 1.376(4) . ?
C23 C24 1.368(4) . ?
C24 C25 1.375(4) . ?
C25 C26 1.367(4) . ?
