Structural chemistry of new lithium bis(oxalato)borate solvates
Zavalij, Peter Y.; Yang, Shoufeng; Whittingham, M. Stanley; Acta Crystallographica Section B 60 (2004) 716–724; doi:10.1107/S0108768104022153

data_2102672
_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       '\w 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/[\s^2^(Fo^2^)+(0.07P)^2^+0.94P], P=(max(Fo^2^,0)+2Fc^2^)/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