About the polymorphism of [Li(C~4~H~8~O)~3~]I: crystal structures of trigonal and tetragonal polymorphs
Gärtner, Stefanie; Gärtner, Tobias; Gschwind, Ruth-Maria; Korber, Nikolaus; Acta Crystallographica Section E 70 (2014) 555–558; doi:10.1107/S160053681402529X

data_2240232
_publ_section_title
;
 About the polymorphism of [Li(C~4~H~8~O)~3~]I: crystal structures of
 trigonal and tetragonal polymorphs
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              555
_journal_page_last               558
_journal_paper_doi               10.1107/S160053681402529X
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Li (C4 H8 O)3] I'
_chemical_formula_moiety         'C12 H24 Li1 O3 +, I -'
_chemical_formula_sum            'C12 H24 I Li O3'
_chemical_formula_weight         350.15
_chemical_name_systematic
;
Iodidotris(tetrahydrofuran-\k<i>O</i>)lithium
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           110
_space_group_name_Hall           'I 4bw -2c'
_space_group_name_H-M_alt        'I 41 c d'
_symmetry_space_group_name_Hall  'I 4bw -2c'
_symmetry_space_group_name_H-M   'I 41 c d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   18.288(3)
_cell_length_b                   18.288(3)
_cell_length_c                   18.511(4)
_cell_measurement_temperature    123.0(10)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      2.2
_cell_volume                     6191(2)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2002)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2002)
;
_computing_data_reduction
;
X-AREA (Stoe & Cie, 2002)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2012)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      123.0(10)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14474
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.470
_diffrn_reflns_theta_min         2.227
_exptl_absorpt_coefficient_mu    2.063
_exptl_absorpt_correction_T_max  0.744
_exptl_absorpt_correction_T_min  0.629
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(<i>X-RED</i> and <i>X-SHAPE</i>; Stoe & Cie, 2002)
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_description       needle
_exptl_crystal_F_000             2816
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.209
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 922 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2802
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0296P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0559
_refine_ls_wR_factor_ref         0.0580
_reflns_number_gt                2130
_reflns_number_total             2802
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm5091sup1.cif
_cod_data_source_block           LiI_3THF_tetragonal
_cod_database_code               2240232
_cod_database_fobs_code          2240232
_shelx_estimated_absorpt_t_min   0.629
_shelx_estimated_absorpt_t_max   0.744
_shelxl_version_number           2.014