#------------------------------------------------------------------------------
#$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/26/2102673.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_2102673
loop_
_publ_author_name
'Zavalij, Peter Y.'
'Yang, Shoufeng'
'Whittingham, M. Stanley'
_publ_section_title
;
 Structural chemistry of new lithium bis(oxalato)borate solvates
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              716
_journal_page_last               724
_journal_paper_doi               10.1107/S0108768104022153
_journal_volume                  60
_journal_year                    2004
_chemical_formula_moiety         'C8 H10 B Li O10'
_chemical_formula_structural     Li[B(C2O4)2].(C4H10O2)
_chemical_formula_sum            'C8 H10 B Li O10'
_chemical_formula_weight         283.91
_chemical_name_common
'Lithium bis(oxalato)borate dimethoxyethylene'
_chemical_name_systematic
;
Lithium bis(oxalato)borate dimethoxyethylene
;
_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 & ZCIF'
_cell_angle_alpha                114.159(2)
_cell_angle_beta                 94.764(2)
_cell_angle_gamma                106.412(2)
_cell_formula_units_Z            2
_cell_length_a                   8.6690(7)
_cell_length_b                   8.8519(7)
_cell_length_c                   9.3328(8)
_cell_measurement_reflns_used    2770
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      31.1
_cell_measurement_theta_min      2.7
_cell_volume                     610.46(9)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Materials Studio (2001)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       'ω 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  0.0213
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7526
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.46
_diffrn_standards_decay_%        -0.54
_exptl_absorpt_coefficient_mu    0.142
_exptl_absorpt_correction_T_max  0.964
_exptl_absorpt_correction_T_min  0.841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XPREP (Sheldrick, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             292
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3509
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0661P)²], P=(max(Fo²,0)+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.0959
_reflns_number_gt                3051
_reflns_number_total             3509
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ta5011.cif
_cod_data_source_block           IV
_cod_original_cell_volume        610.45(9)
_cod_database_code               2102673
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_occupancy
_atom_site_type_symbol
Li1 0.9908(2) 0.4673(2) 0.66495(19) 0.0229(3) Uani d 1 Li
B1 0.40189(12) 0.22735(12) 0.35914(12) 0.01674(19) Uani d 1 B
C1 0.64402(10) 0.21424(11) 0.46098(10) 0.01740(17) Uani d 1 C
C2 0.52292(10) 0.02575(11) 0.34779(10) 0.01819(17) Uani d 1 C
O1 0.57021(7) 0.32714(8) 0.46203(8) 0.01825(14) Uani d 1 O
O2 0.78055(8) 0.25042(9) 0.53412(8) 0.02201(15) Uani d 1 O
O3 0.38654(7) 0.04142(8) 0.28830(8) 0.01931(14) Uani d 1 O
O4 0.54796(9) -0.10880(9) 0.31981(9) 0.02514(16) Uani d 1 O
C3 0.24817(10) 0.34638(12) 0.25628(10) 0.01801(17) Uani d 1 C
C4 0.19216(10) 0.33526(11) 0.40392(10) 0.01550(16) Uani d 1 C
O5 0.37064(8) 0.28348(9) 0.23412(8) 0.01965(14) Uani d 1 O
O6 0.18617(8) 0.40082(10) 0.17704(8) 0.02549(16) Uani d 1 O
O7 0.27791(7) 0.26145(8) 0.45761(7) 0.01679(14) Uani d 1 O
O8 0.08443(7) 0.38691(8) 0.45699(8) 0.01888(14) Uani d 1 O
C5 1.20340(14) 0.86761(13) 0.88249(13) 0.0280(2) Uani d 1 C
H51 1.1326(16) 0.8849(17) 0.9588(16) 0.032(3) Uiso d 1 H
H52 1.1604(16) 0.8882(17) 0.7965(16) 0.030(3) Uiso d 1 H
H53 1.3164(17) 0.9499(18) 0.9335(16) 0.031(3) Uiso d 1 H
O9 1.20013(8) 0.69028(8) 0.81689(7) 0.02184(15) Uani d 1 O
C6 1.26904(12) 0.65323(13) 0.93876(11) 0.0250(2) Uani d 1 C
H61 1.2022(15) 0.6723(16) 1.0206(15) 0.029(3) Uiso d 1 H
H62 1.3850(17) 0.7268(18) 0.9867(16) 0.035(3) Uiso d 1 H
C7 1.25813(11) 0.46405(13) 0.85966(11) 0.02255(19) Uani d 1 C
H71 1.3247(14) 0.4436(15) 0.7803(14) 0.019(3) Uiso d 1 H
H72 1.2981(15) 0.4322(16) 0.9414(15) 0.024(3) Uiso d 1 H
O10 1.08761(8) 0.35962(9) 0.78452(8) 0.02237(15) Uani d 1 O
C8 1.05617(14) 0.17565(13) 0.73139(14) 0.0273(2) Uani d 1 C
H81 1.0806(17) 0.1551(18) 0.8241(17) 0.037(3) Uiso d 1 H
H82 1.1243(16) 0.1343(18) 0.6584(17) 0.034(3) Uiso d 1 H
H83 0.9404(18) 0.1152(19) 0.6741(17) 0.038(3) Uiso d 1 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
O10 Li1 O2 . . 96.17(7)
O10 Li1 O8 . 1_655 100.87(7)
O2 Li1 O8 . 1_655 86.83(7)
O10 Li1 O9 . . 81.46(6)
O2 Li1 O9 . . 175.18(9)
O8 Li1 O9 1_655 . 97.73(7)
O10 Li1 O8 . 2_666 172.64(9)
O2 Li1 O8 . 2_666 90.94(6)
O8 Li1 O8 1_655 2_666 77.61(6)
O9 Li1 O8 . 2_666 91.57(7)
O10 Li1 O6 . 2_666 106.28(7)
O2 Li1 O6 . 2_666 86.16(6)
O8 Li1 O6 1_655 2_666 152.52(8)
O9 Li1 O6 . 2_666 90.46(6)
O8 Li1 O6 2_666 2_666 75.98(5)
O10 Li1 Li1 . 2_766 140.56(10)
O2 Li1 Li1 . 2_766 88.65(7)
O8 Li1 Li1 1_655 2_766 40.17(4)
O9 Li1 Li1 . 2_766 95.84(8)
O8 Li1 Li1 2_666 2_766 37.44(4)
O6 Li1 Li1 2_666 2_766 113.09(8)
O3 B1 O1 . . 106.01(6)
O3 B1 O5 . . 111.68(7)
O1 B1 O5 . . 112.24(7)
O3 B1 O7 . . 111.55(7)
O1 B1 O7 . . 110.05(7)
O5 B1 O7 . . 105.41(7)
O2 C1 O1 . . 126.66(8)
O2 C1 C2 . . 125.50(8)
O1 C1 C2 . . 107.83(7)
O4 C2 O3 . . 126.78(8)
O4 C2 C1 . . 126.00(8)
O3 C2 C1 . . 107.22(7)
C1 O1 B1 . . 109.08(7)
C1 O2 Li1 . . 139.52(8)
C2 O3 B1 . . 109.71(7)
O6 C3 O5 . . 128.35(8)
O6 C3 C4 . . 123.92(8)
O5 C3 C4 . . 107.72(7)
O8 C4 O7 . . 127.70(8)
O8 C4 C3 . . 123.38(8)
O7 C4 C3 . . 108.92(7)
C3 O5 B1 . . 109.10(7)
C3 O6 Li1 . 2_666 104.28(7)
C4 O7 B1 . . 108.76(6)
C4 O8 Li1 . 1_455 142.70(7)
C4 O8 Li1 . 2_666 110.73(7)
Li1 O8 Li1 1_455 2_666 102.39(6)
O9 C5 H51 . . 109.6(7)
O9 C5 H52 . . 108.7(8)
H51 C5 H52 . . 108.1(10)
O9 C5 H53 . . 110.4(8)
H51 C5 H53 . . 111.2(11)
H52 C5 H53 . . 108.9(11)
C5 O9 C6 . . 111.40(7)
C5 O9 Li1 . . 124.38(7)
C6 O9 Li1 . . 107.55(7)
O9 C6 C7 . . 107.67(7)
O9 C6 H61 . . 107.5(7)
C7 C6 H61 . . 110.4(7)
O9 C6 H62 . . 111.8(8)
C7 C6 H62 . . 108.1(8)
H61 C6 H62 . . 111.3(11)
O10 C7 C6 . . 106.92(7)
O10 C7 H71 . . 110.3(7)
C6 C7 H71 . . 111.5(7)
O10 C7 H72 . . 110.4(7)
C6 C7 H72 . . 109.7(7)
H71 C7 H72 . . 108.0(9)
C8 O10 C7 . . 112.18(7)
C8 O10 Li1 . . 126.24(8)
C7 O10 Li1 . . 110.05(7)
O10 C8 H81 . . 109.4(8)
O10 C8 H82 . . 111.2(8)
H81 C8 H82 . . 108.4(11)
O10 C8 H83 . . 106.2(8)
H81 C8 H83 . . 112.7(12)
H82 C8 H83 . . 109.0(12)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Li1 O10 . 2.0059(17)
Li1 O2 . 2.0574(17)
Li1 O8 1_655 2.0949(17)
Li1 O9 . 2.1112(17)
Li1 O8 2_666 2.2229(17)
Li1 O6 2_666 2.4232(18)
Li1 Li1 2_766 3.366(3)
B1 O3 . 1.4611(11)
B1 O1 . 1.4751(11)
B1 O5 . 1.4765(11)
B1 O7 . 1.4870(11)
C1 O2 . 1.2009(10)
C1 O1 . 1.3277(10)
C1 C2 . 1.5444(12)
C2 O4 . 1.1978(10)
C2 O3 . 1.3311(10)
C3 O6 . 1.2001(11)
C3 O5 . 1.3252(10)
C3 C4 . 1.5294(12)
C4 O8 . 1.2081(10)
C4 O7 . 1.3081(10)
C5 O9 . 1.4231(11)
C5 H51 . 0.972(13)
C5 H52 . 0.962(13)
C5 H53 . 0.976(14)
O9 C6 . 1.4356(11)
C6 C7 . 1.4984(14)
C6 H61 . 0.986(13)
C6 H62 . 0.976(14)
C7 O10 . 1.4340(11)
C7 H71 . 0.967(12)
C7 H72 . 0.984(12)
O10 C8 . 1.4276(12)
C8 H81 . 0.973(14)
C8 H82 . 0.965(14)
C8 H83 . 0.976(15)
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
O2 C1 C2 O4 . . 1.14(14)
O1 C1 C2 O4 . . -178.99(8)
O2 C1 C2 O3 . . -179.05(8)
O1 C1 C2 O3 . . 0.82(9)
O2 C1 O1 B1 . . -178.51(8)
C2 C1 O1 B1 . . 1.62(9)
O3 B1 O1 C1 . . -3.32(9)
O5 B1 O1 C1 . . -125.50(7)
O7 B1 O1 C1 . . 117.44(7)
O1 C1 O2 Li1 . . -11.63(17)
C2 C1 O2 Li1 . . 168.21(9)
O10 Li1 O2 C1 . . 159.67(10)
O8 Li1 O2 C1 1_655 . -99.73(11)
O8 Li1 O2 C1 2_666 . -22.20(13)
O6 Li1 O2 C1 2_666 . 53.68(12)
O4 C2 O3 B1 . . 176.89(9)
C1 C2 O3 B1 . . -2.92(9)
O1 B1 O3 C2 . . 3.89(9)
O5 B1 O3 C2 . . 126.43(7)
O7 B1 O3 C2 . . -115.90(8)
O6 C3 C4 O8 . . -2.95(14)
O5 C3 C4 O8 . . 178.17(8)
O6 C3 C4 O7 . . 176.49(8)
O5 C3 C4 O7 . . -2.39(9)
O6 C3 O5 B1 . . -178.34(9)
C4 C3 O5 B1 . . 0.48(9)
O3 B1 O5 C3 . . 122.62(7)
O1 B1 O5 C3 . . -118.47(8)
O7 B1 O5 C3 . . 1.32(9)
O5 C3 O6 Li1 . 2_666 -170.36(9)
C4 C3 O6 Li1 . 2_666 10.99(11)
O8 C4 O7 B1 . . -177.41(9)
C3 C4 O7 B1 . . 3.18(9)
O3 B1 O7 C4 . . -124.26(7)
O1 B1 O7 C4 . . 118.36(7)
O5 B1 O7 C4 . . -2.88(9)
O7 C4 O8 Li1 . 1_455 21.13(17)
C3 C4 O8 Li1 . 1_455 -159.55(10)
O7 C4 O8 Li1 . 2_666 172.26(8)
C3 C4 O8 Li1 . 2_666 -8.41(11)
O10 Li1 O9 C5 . . -145.33(8)
O8 Li1 O9 C5 1_655 . 114.76(8)
O8 Li1 O9 C5 2_666 . 37.06(10)
O6 Li1 O9 C5 2_666 . -38.94(10)
O10 Li1 O9 C6 . . -12.48(8)
O8 Li1 O9 C6 1_655 . -112.38(7)
O8 Li1 O9 C6 2_666 . 169.91(6)
O6 Li1 O9 C6 2_666 . 93.92(7)
C5 O9 C6 C7 . . 179.15(8)
Li1 O9 C6 C7 . . 39.68(9)
O9 C6 C7 O10 . . -56.72(10)
C6 C7 O10 C8 . . -168.80(8)
C6 C7 O10 Li1 . . 45.27(9)
O2 Li1 O10 C8 . . 25.70(11)
O8 Li1 O10 C8 1_655 . -62.25(11)
O9 Li1 O10 C8 . . -158.54(8)
O6 Li1 O10 C8 2_666 . 113.48(9)
O2 Li1 O10 C7 . . 165.67(7)
O8 Li1 O10 C7 1_655 . 77.72(8)
O9 Li1 O10 C7 . . -18.57(8)
O6 Li1 O10 C7 2_666 . -106.55(8)
