#------------------------------------------------------------------------------
#$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/26/2102672.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_2102672
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         'C7 H6 B Li O9, 0.33(C3 H6 O)'
_chemical_formula_structural     Li[B(C2O4)2].4/3CH3COCH3
_chemical_formula_sum            'C8 H8 B Li O9.33'
_chemical_formula_weight         271.21
_chemical_name_common            'Lithium bis(oxalato)borate acetone'
_chemical_name_systematic
;
Lithium bis(oxalato)borate acetone
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                90.00
_cell_angle_beta                 121.201(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.3987(16)
_cell_length_b                   7.6308(7)
_cell_length_c                   10.9904(11)
_cell_measurement_reflns_used    2604
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      31.1
_cell_measurement_theta_min      2.6
_cell_volume                     1176.4(2)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0408
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4923
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        -0.30
_exptl_absorpt_coefficient_mu    0.139
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XPREP (Sheldrick, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             555
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.320
_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     134
_refine_ls_number_reflns         1437
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0466
_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)+(0.07P)²+0.94P], P=(max(Fo²,0)+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1293
_reflns_number_gt                1116
_reflns_number_total             1437
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ta5011.cif
_cod_data_source_block           III
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               2102672
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Li1 0.4553(3) 0.5000 0.3184(5) 0.0353(12) Uani d S 1 Li
B1 0.1970(2) 0.5000 0.4670(3) 0.0199(6) Uani d S 1 B
C1 0.04544(12) 0.3988(3) 0.38430(18) 0.0213(4) Uani d . 1 C
O1 0.13486(8) 0.34723(16) 0.43429(13) 0.0229(3) Uani d . 1 O
O2 -0.02221(9) 0.30551(19) 0.34642(14) 0.0284(4) Uani d . 1 O
C2 0.33668(17) 0.5000 0.4698(3) 0.0175(5) Uani d S 1 C
O3 0.24415(12) 0.5000 0.38254(17) 0.0184(4) Uani d S 1 O
O4 0.39806(12) 0.5000 0.44008(19) 0.0211(4) Uani d S 1 O
C3 0.35768(18) 0.5000 0.6224(3) 0.0205(6) Uani d S 1 C
O5 0.27568(12) 0.5000 0.61686(18) 0.0236(5) Uani d S 1 O
O6 0.43586(13) 0.5000 0.72712(19) 0.0255(5) Uani d S 1 O
O7 0.34606(14) 0.5000 0.1240(2) 0.0383(6) Uani d SD 1 O
C4 0.3209(3) 0.4491(5) 0.0033(4) 0.0378(12) Uani d PDU 0.50 C
C5 0.2275(3) 0.5302(12) -0.1198(5) 0.059(2) Uani d PDU 0.50 C
H5A 0.1813 0.5442 -0.0893 0.088 Uiso calc PR 0.50 H
H5B 0.2008 0.4527 -0.2028 0.088 Uiso calc PR 0.50 H
H5C 0.2414 0.6450 -0.1449 0.088 Uiso calc PR 0.50 H
C6 0.3752(4) 0.3209(7) -0.0274(5) 0.0482(13) Uani d PDU 0.50 C
H6A 0.4065 0.3811 -0.0710 0.072 Uiso calc PR 0.50 H
H6B 0.3317 0.2315 -0.0929 0.072 Uiso calc PR 0.50 H
H6C 0.4235 0.2650 0.0614 0.072 Uiso calc PR 0.50 H
O8 0.4733(4) 0.0000 -0.1384(6) 0.0348(18) Uani d SPDU 0.334(4) O
C7 0.4232(6) 0.0000 -0.0894(7) 0.053(3) Uani d SPDU 0.334(4) C
C8 0.3905(7) 0.1639(13) -0.0577(9) 0.069(3) Uani d PDU 0.334(4) C
H8A 0.3921 0.2587 -0.1166 0.104 Uiso calc PR 0.334(4) H
H8B 0.4325 0.1934 0.0431 0.104 Uiso calc PR 0.334(4) H
H8C 0.3252 0.1488 -0.0783 0.104 Uiso calc PR 0.334(4) 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
O7 Li1 O4 . . 104.5(2)
O7 Li1 O6 . 5_666 98.8(2)
O4 Li1 O6 . 5_666 156.8(3)
O7 Li1 O2 . 3 97.81(12)
O4 Li1 O2 . 3 90.47(12)
O6 Li1 O2 5_666 3 86.35(12)
O7 Li1 O2 . 8 97.81(12)
O4 Li1 O2 . 8 90.47(12)
O6 Li1 O2 5_666 8 86.35(12)
O2 Li1 O2 3 8 163.6(2)
O7 Li1 O4 . 5_666 176.2(3)
O4 Li1 O4 . 5_666 79.34(17)
O6 Li1 O4 5_666 5_666 77.45(16)
O2 Li1 O4 3 5_666 82.04(12)
O2 Li1 O4 8 5_666 82.04(12)
O1 B1 O1 . 6_565 105.5(2)
O1 B1 O5 . . 111.68(14)
O1 B1 O5 6_565 . 111.68(14)
O1 B1 O3 . . 111.55(14)
O1 B1 O3 6_565 . 111.55(14)
O5 B1 O3 . . 105.1(2)
O2 C1 O1 . . 126.29(18)
O2 C1 C1 . 6_565 126.51(11)
O1 C1 C1 . 6_565 107.20(10)
C1 O1 B1 . . 110.06(15)
C1 O2 Li1 . 3_445 133.49(17)
O4 C2 O3 . . 127.8(2)
O4 C2 C3 . . 123.5(2)
O3 C2 C3 . . 108.7(2)
C2 O3 B1 . . 108.87(19)
C2 O4 Li1 . . 158.3(2)
C2 O4 Li1 . 5_666 101.00(19)
Li1 O4 Li1 . 5_666 100.66(17)
O6 C3 O5 . . 127.1(2)
O6 C3 C2 . . 125.1(2)
O5 C3 C2 . . 107.8(2)
C3 O5 B1 . . 109.54(19)
C3 O6 Li1 . 5_666 113.0(2)
C4 O7 Li1 . . 141.7(3)
O7 C4 C6 . . 123.4(4)
O7 C4 C5 . . 116.2(4)
C6 C4 C5 . . 120.3(4)
C4 C5 H5A . . 109.5
C4 C5 H5B . . 109.5
H5A C5 H5B . . 109.5
C4 C5 H5C . . 109.5
H5A C5 H5C . . 109.5
H5B C5 H5C . . 109.5
C4 C6 H6A . . 109.5
C4 C6 H6B . . 109.5
H6A C6 H6B . . 109.5
C4 C6 H6C . . 109.5
H6A C6 H6C . . 109.5
H6B C6 H6C . . 109.5
O8 C7 C8 . . 121.8(6)
O8 C7 C8 . 6 121.8(6)
C8 C7 C8 . 6 116.4(11)
C7 C8 H8A . . 109.5
C7 C8 H8B . . 109.5
H8A C8 H8B . . 109.5
C7 C8 H8C . . 109.5
H8A C8 H8C . . 109.5
H8B C8 H8C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Li1 O7 . 1.951(5)
Li1 O4 . 1.993(5)
Li1 O6 5_666 2.087(5)
Li1 O2 3 2.3554(17)
Li1 O2 8 2.3554(17)
Li1 O4 5_666 2.493(5)
Li1 Li1 5_666 3.468(9)
B1 O1 . 1.465(2)
B1 O1 6_565 1.465(2)
B1 O5 . 1.475(3)
B1 O3 . 1.485(3)
C1 O2 . 1.197(2)
C1 O1 . 1.331(2)
C1 C1 6_565 1.544(4)
C2 O4 . 1.208(3)
C2 O3 . 1.309(3)
C2 C3 . 1.527(4)
C3 O6 . 1.200(3)
C3 O5 . 1.314(3)
O7 C4 . 1.230(4)
C4 C6 . 1.475(7)
C4 C5 . 1.553(7)
C5 H5A . 0.9800
C5 H5B . 0.9800
C5 H5C . 0.9800
C6 H6A . 0.9800
C6 H6B . 0.9800
C6 H6C . 0.9800
O8 C7 . 1.193(13)
C7 C8 . 1.472(11)
C7 C8 6 1.472(11)
C8 H8A . 0.9800
C8 H8B . 0.9800
C8 H8C . 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_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
O2 C1 O1 B1 . . 179.07(19)
C1 C1 O1 B1 6_565 . -0.88(16)
O1 B1 O1 C1 6_565 . 1.4(3)
O5 B1 O1 C1 . . 122.88(17)
O3 B1 O1 C1 . . -119.87(17)
O1 C1 O2 Li1 . 3_445 -5.6(3)
C1 C1 O2 Li1 6_565 3_445 174.36(17)
O4 C2 O3 B1 . . 180.0
C3 C2 O3 B1 . . 0.0
O1 B1 O3 C2 . . -121.17(15)
O1 B1 O3 C2 6_565 . 121.17(15)
O5 B1 O3 C2 . . 0.0
O3 C2 O4 Li1 . . 0.000(2)
C3 C2 O4 Li1 . . 180.0000(10)
O3 C2 O4 Li1 . 5_666 180.0
C3 C2 O4 Li1 . 5_666 0.0
O7 Li1 O4 C2 . . 0.0000(10)
O6 Li1 O4 C2 5_666 . 180.000(2)
O2 Li1 O4 C2 3 . 98.19(12)
O2 Li1 O4 C2 8 . -98.19(12)
O4 Li1 O4 C2 5_666 . 180.0000(10)
C3 Li1 O4 C2 5_666 . 180.0000(10)
O7 Li1 O4 Li1 . 5_666 180.0
O6 Li1 O4 Li1 5_666 5_666 0.000(2)
O2 Li1 O4 Li1 3 5_666 -81.81(12)
O2 Li1 O4 Li1 8 5_666 81.81(12)
O4 Li1 O4 Li1 5_666 5_666 0.0000(10)
C3 Li1 O4 Li1 5_666 5_666 0.0000(10)
O4 C2 C3 O6 . . 0.0
O3 C2 C3 O6 . . 180.0
O4 C2 C3 O5 . . 180.0
O3 C2 C3 O5 . . 0.0
O4 C2 C3 Li1 . 5_666 0.0
O3 C2 C3 Li1 . 5_666 180.0
O6 C3 O5 B1 . . 180.0000(10)
C2 C3 O5 B1 . . 0.0
O1 B1 O5 C3 . . 121.09(15)
O1 B1 O5 C3 6_565 . -121.09(15)
O3 B1 O5 C3 . . 0.0
O5 C3 O6 Li1 . 5_666 180.0
C2 C3 O6 Li1 . 5_666 0.0
O4 Li1 O7 C4 . . -149.3(3)
O6 Li1 O7 C4 5_666 . 30.7(3)
O2 Li1 O7 C4 3 . 118.1(2)
O2 Li1 O7 C4 8 . -56.8(3)
Li1 O7 C4 C6 . . 13.2(4)
Li1 O7 C4 C5 . . -165.7(4)
