Two pseudopolymorphs of LiCl trimers with semicubane structures
Wioleta Domanska-Babul; Katarzyna Baranowska; Jerzy Pikies; Acta Crystallographica Section C 64 (2008) m20–m22; doi:10.1107/S0108270107058763

data_2016385
_publ_section_title
;
 Two pseudopolymorphs of LiCl trimers with semicubane structures
;
_journal_coeditor_code           GZ3103
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m20
_journal_page_last               m22
_journal_paper_doi               10.1107/S0108270107058763
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Li3 Cl3 (C6 H15 O P)4] , C7 H8'
_chemical_formula_moiety         'C24 H60 Cl3 Li3 O4 P4, C7 H8'
_chemical_formula_sum            'C31 H68 Cl3 Li3 O4 P4'
_chemical_formula_weight         755.9
_chemical_name_systematic
;
trichlorido(\m~3~-triethylphosphine
oxide-\k^3^O:O:O)tris(\m~2~-triethylphosphine oxide-\k^2^O:O)trilithium(I)
toluene solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 134.162(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3414(7)
_cell_length_b                   32.9899(19)
_cell_length_c                   16.1000(10)
_cell_measurement_reflns_used    14410
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      32.4826
_cell_measurement_theta_min      2.1475
_cell_volume                     4321.3(5)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '4-axis \k geometry diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction KM4 CCD'
_diffrn_measurement_method       '\w scans, 0.75 deg width'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.06
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29430
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    0.39
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.928
_refine_diff_density_min         -0.49
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         7657
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.06
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0438P)^2^+6.5385P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1272
_reflns_number_gt                5468
_reflns_number_total             7657
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gz3103.cif
_cod_data_source_block           I
_cod_database_code               2016385
_cod_database_fobs_code          2016385