#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/46/2004600.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_2004600
loop_
_publ_author_name
'Schödel, H.'
'Vaupel, T.'
'Bock, H.'
_publ_section_title
;
 Lithium Tetraphenylborate.2thf.2H₂O
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              637
_journal_page_last               640
_journal_paper_doi               10.1107/S0108270195012522
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          '[Li (C4 H8 O1)2 (H2 O1)2] (C24 H20 B)'
_chemical_formula_moiety         'C24 H20 B1,Li (C4 H8 O1)2,2H2 O1'
_chemical_formula_sum            'C32 H40 B Li O4'
_chemical_formula_weight         506.39
_chemical_name_systematic
;
Lithiumtetrapenylborate-Dihydrate-Bis(tetrahydrofuran)
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.252(3)
_cell_length_b                   16.565(3)
_cell_length_c                   10.422(2)
_cell_measurement_reflns_used    96
_cell_measurement_temperature    200.0(10)
_cell_measurement_theta_max      16.5
_cell_measurement_theta_min      10
_cell_volume                     2978.4(9)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1988)'
_computing_data_reduction        DIF4
_computing_molecular_graphics    'SHELXTL/PC XP'
_computing_publication_material  'SHELXL93 CIFTAB'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      200.0(10)
_diffrn_measurement_device
'Siemens-Stoe AED2 four-circle diffractometer'
_diffrn_measurement_method       'ω-θ scan'
_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  0.0054
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3648
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         2.28
_diffrn_standards_decay_%        negligible
_diffrn_standards_interval_time  '120 min'
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.306
_refine_ls_extinction_coef       0.0029(10)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.102
_refine_ls_goodness_of_fit_obs   1.202
_refine_ls_hydrogen_treatment    'H atoms: see text'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         3555
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_restrained_S_obs      1.202
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_obs          0.0495
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0705P)²+0.6761P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1607
_refine_ls_wR_factor_obs         0.1392
_reflns_number_observed          2300
_reflns_number_total             3555
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            du1138.cif
_cod_data_source_block           bock83
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0705P)^2^+0.6761P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0705P)^2^+0.6761P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               2004600
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_occupancy
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_type_symbol
Li1 1 .4107(3) .7500 .5996(4) .0526(10) Uani d S Li
O1 1 .30024(13) .7500 .6178(2) .0662(6) Uani d S O
H01A 1 .283(2) .7076(19) .596(3) .142(14) Uiso d . H
O2 1 .4626(2) .7500 .4372(2) .0742(7) Uani d S O
H02A 1 .505(4) .7500 .411(6) .17(3) Uiso d S H
H02B 1 .435(3) .7500 .364(5) .125(17) Uiso d S H
O3 1 .43830(10) .65270(9) .68608(14) .0716(5) Uani d . O
C1 1 .4871(2) .5923(2) .6376(3) .1017(10) Uani d . C
H1A 1 .5419(2) .6088(2) .6474(3) .153 Uiso calc R H
H1B 1 .4766(2) .5840(2) .5451(3) .153 Uiso calc R H
C2 1 .4732(2) .5186(2) .7071(3) .0916(8) Uani d . C
H2A 1 .5226(2) .4903(2) .7248(3) .137 Uiso calc R H
H2B 1 .4390(2) .4822(2) .6574(3) .137 Uiso calc R H
C3 1 .4351(2) .54362(14) .8290(2) .0794(7) Uani d . C
H3A 1 .3929(2) .50576(14) .8521(2) .119 Uiso calc R H
H3B 1 .4730(2) .54550(14) .9002(2) .119 Uiso calc R H
C4 1 .4036(2) .6255(2) .8018(2) .0861(8) Uani d . C
H4A 1 .3465(2) .6232(2) .7922(2) .129 Uiso calc R H
H4B 1 .4161(2) .6628(2) .8730(2) .129 Uiso calc R H
B1 1 .63098(13) .7500 .1490(2) .0327(5) Uani d S B
C11 1 .66935(8) .67098(9) .07685(14) .0352(3) Uani d . C
C12 1 .73717(9) .63262(10) .1201(2) .0454(4) Uani d . C
H12 1 .76057(9) .65090(10) .1973(2) .055 Uiso calc R H
C13 1 .77121(11) .56912(12) .0542(2) .0602(5) Uani d . C
H13 1 .81673(11) .54461(12) .0876(2) .072 Uiso calc R H
C14 1 .73996(12) .54118(12) -.0586(2) .0625(5) Uani d . C
H14 1 .76306(12) .49722(12) -0.1029(2) .075 Uiso calc R H
C15 1 .67453(11) .57816(12) -0.1061(2) .0561(5) Uani d . C
H15 1 .65266(11) .56028(12) -0.1848(2) .067 Uiso calc R H
C16 1 .64015(9) .64175(10) -.0393(2) .0435(4) Uani d . C
H16 1 .59503(9) .66620(10) -.0742(2) .052 Uiso calc R H
C21 1 .53563(12) .7500 .1355(2) .0323(4) Uani d S C
C22 1 .49213(9) .67886(10) .1354(2) .0400(4) Uani d . C
H22 1 .51875(9) .62866(10) .1362(2) .048 Uiso calc R H
C23 1 .41129(9) .67839(11) .1343(2) .0476(4) Uani d . C
H23 1 .38411(9) .62851(11) .1343(2) .057 Uiso calc R H
C24 1 .37077(13) .7500 .1331(2) .0473(6) Uani d S C
H24 1 .31571(13) .7500 .1315(2) .057 Uiso calc SR H
C31 1 .64777(12) .7500 .3047(2) .0351(5) Uani d S C
C32 1 .65351(10) .67900(11) .3764(2) .0447(4) Uani d . C
H32 1 .64778(10) .62876(11) .3335(2) .054 Uiso calc R H
C33 1 .66730(11) .67871(13) .5085(2) .0564(5) Uani d . C
H33 1 .67147(11) .62885(13) .5530(2) .068 Uiso calc R H
C34 1 .6749(2) .7500 .5742(3) .0615(8) Uani d S C
H34 1 .6851(2) .7500 .6637(3) .074 Uiso calc SR H
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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O3 Li1 O3 7_575 . 115.4(2) yes
O3 Li1 O2 7_575 . 107.5(2) yes
O3 Li1 O2 . . 107.5(2) yes
O3 Li1 O1 7_575 . 101.6(2) yes
O3 Li1 O1 . . 101.6(2) yes
O2 Li1 O1 . . 123.6(3) yes
C1 O3 C4 . . 109.5(2) yes
C1 O3 Li1 . . 125.6(2) yes
C4 O3 Li1 . . 124.4(2) yes
O3 C1 C2 . . 108.9(2) yes
C1 C2 C3 . . 105.4(2) yes
C4 C3 C2 . . 104.6(2) yes
O3 C4 C3 . . 107.3(2) yes
C11 B1 C11 . 7_575 105.2(2) no
C11 B1 C31 . . 112.23(11) no
C11 B1 C31 7_575 . 112.23(11) no
C11 B1 C21 . . 111.18(11) no
C11 B1 C21 7_575 . 111.18(11) no
C31 B1 C21 . . 105.0(2) no
C16 C11 C12 . . 114.89(14) no
C16 C11 B1 . . 121.68(14) no
C12 C11 B1 . . 123.18(15) no
C13 C12 C11 . . 122.5(2) no
C14 C13 C12 . . 120.9(2) no
C13 C14 C15 . . 118.7(2) no
C14 C15 C16 . . 120.4(2) no
C15 C16 C11 . . 122.7(2) no
C22 C21 C22 . 7_575 115.0(2) no
C22 C21 B1 . . 122.36(10) no
C22 C21 B1 7_575 . 122.36(10) no
C23 C22 C21 . . 122.8(2) no
C24 C23 C22 . . 120.2(2) no
C23 C24 C23 7_575 . 119.0(2) no
C32 C31 C32 7_575 . 114.7(2) no
C32 C31 B1 7_575 . 122.61(10) no
C32 C31 B1 . . 122.61(10) no
C31 C32 C33 . . 122.8(2) no
C34 C33 C32 . . 120.4(2) no
C33 C34 C33 . 7_575 118.9(2) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Li1 O3 7_575 1.907(3) yes
Li1 O3 . 1.907(3) yes
Li1 O2 . 1.914(5) yes
Li1 O1 . 1.915(5) yes
O3 C1 . 1.401(3) yes
O3 C4 . 1.420(3) yes
C1 C2 . 1.440(4) yes
C2 C3 . 1.490(4) yes
C3 C4 . 1.489(3) yes
B1 C11 . 1.648(2) no
B1 C11 7_575 1.648(2) no
B1 C31 . 1.649(3) no
B1 C21 . 1.651(3) no
C11 C16 . 1.398(2) no
C11 C12 . 1.406(2) no
C12 C13 . 1.386(2) no
C13 C14 . 1.374(3) no
C14 C15 . 1.376(3) no
C15 C16 . 1.395(2) no
C21 C22 . 1.397(2) no
C21 C22 7_575 1.397(2) no
C22 C23 . 1.395(2) no
C23 C24 . 1.377(2) no
C24 C23 7_575 1.377(2) no
C31 C32 7_575 1.397(2) no
C31 C32 . 1.397(2) no
C32 C33 . 1.397(2) no
C33 C34 . 1.372(2) no
C34 C33 7_575 1.372(2) no
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
_geom_torsion_publ_flag
O3 Li1 O3 C1 7_575 . -120.6(3) no
O2 Li1 O3 C1 . . -0.7(4) no
O1 Li1 O3 C1 . . 130.4(3) no
O3 Li1 O3 C4 7_575 . 68.8(4) no
O2 Li1 O3 C4 . . -171.3(2) no
O1 Li1 O3 C4 . . -40.2(3) no
C4 O3 C1 C2 . . 11.4(4) no
Li1 O3 C1 C2 . . -160.4(3) no
O3 C1 C2 C3 . . -19.8(4) no
C1 C2 C3 C4 . . 20.2(3) no
C1 O3 C4 C3 . . 1.9(3) no
Li1 O3 C4 C3 . . 173.8(2) no
C2 C3 C4 O3 . . -13.8(3) no
C11 B1 C11 C16 7_575 . -82.1(2) no
C31 B1 C11 C16 . . 155.58(15) no
C21 B1 C11 C16 . . 38.3(2) no
C11 B1 C11 C12 7_575 . 92.0(2) no
C31 B1 C11 C12 . . -30.3(2) no
C21 B1 C11 C12 . . -147.6(2) no
C16 C11 C12 C13 . . -1.7(2) no
B1 C11 C12 C13 . . -176.2(2) no
C11 C12 C13 C14 . . 0.7(3) no
C12 C13 C14 C15 . . 0.8(3) no
C13 C14 C15 C16 . . -1.1(3) no
C14 C15 C16 C11 . . 0.0(3) no
C12 C11 C16 C15 . . 1.4(2) no
B1 C11 C16 C15 . . 175.9(2) no
C11 B1 C21 C22 . . 34.7(2) no
C11 B1 C21 C22 7_575 . 151.5(2) no
C31 B1 C21 C22 . . -86.9(2) no
C11 B1 C21 C22 . 7_575 -151.5(2) no
C11 B1 C21 C22 7_575 7_575 -34.7(2) no
C31 B1 C21 C22 . 7_575 86.9(2) no
C22 C21 C22 C23 7_575 . 0.5(3) no
B1 C21 C22 C23 . . 174.8(2) no
C21 C22 C23 C24 . . 0.0(3) no
C22 C23 C24 C23 . 7_575 -0.6(3) no
C11 B1 C31 C32 . 7_575 150.7(2) no
C11 B1 C31 C32 7_575 7_575 32.6(2) no
C21 B1 C31 C32 . 7_575 -88.3(2) no
C11 B1 C31 C32 . . -32.6(2) no
C11 B1 C31 C32 7_575 . -150.7(2) no
C21 B1 C31 C32 . . 88.3(2) no
C32 C31 C32 C33 7_575 . -2.7(3) no
B1 C31 C32 C33 . . -179.6(2) no
C31 C32 C33 C34 . . 0.9(3) no
C32 C33 C34 C33 . 7_575 1.1(4) no
