Redetermination of the crystal structure of tetralithium octafluoridozirconate(IV), Li~4~ZrF~8~, from single-crystal X-ray data
Chemey, Alexander T.; Albrecht-Schmitt, Thomas E.; Acta Crystallographica Section E 75 (2019) 139–141; doi:10.1107/S2056989018018194

data_2242811
_publ_section_title
;
 Redetermination of the crystal structure of tetralithium
 octafluoridozirconate(IV), Li~4~ZrF~8~, from single-crystal X-ray data
;
_journal_coeditor_code           WM5477
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              139
_journal_page_last               141
_journal_paper_doi               10.1107/S2056989018018194
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          'Li4 Zr F8'
_chemical_formula_moiety         'Zr F8, 4Li'
_chemical_formula_sum            'F8 Li4 Zr'
_chemical_formula_weight         270.98
_chemical_name_common            'Lithium zirconium octafluoride'
_chemical_name_systematic        'Tetralithium octafluoridozirconate(IV)'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5959(3)
_cell_length_b                   9.6218(3)
_cell_length_c                   5.6735(2)
_cell_measurement_reflns_used    2777
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      49.525
_cell_measurement_theta_min      4.170
_cell_volume                     523.83(3)
_computing_cell_refinement
;
SAINT (Bruker, 2015)
;
_computing_data_collection
;
APEX3 (Bruker, 2015)
;
_computing_data_reduction
;
SAINT (Bruker, 2015)
;
_computing_molecular_graphics
;
<i>SHELXP2014</i> (Sheldrick, 2008) and
<i>VESTA</i> (Momma & Izumi, 2011)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL-2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXS-2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '0.5\% wide /w exposures'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            60244
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         49.525
_diffrn_reflns_theta_min         4.170
_diffrn_source                   'I\ms microfocused'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.208
_exptl_absorpt_correction_T_max  0.1353
_exptl_absorpt_correction_T_min  0.0671
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2015)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.436
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.672
_refine_diff_density_min         -0.759
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     71
_refine_ls_number_reflns         2776
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0289
_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^)+(0.0375P)^2^+0.2784P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0688
_refine_ls_wR_factor_ref         0.0733
_reflns_number_gt                2299
_reflns_number_total             2776
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5477sup1.cif
_cod_data_source_block           I
_cod_database_code               2242811
_shelx_estimated_absorpt_t_min   0.843
_shelx_estimated_absorpt_t_max   0.843
_shelx_hkl_checksum              30977
_shelx_res_checksum              63829
_shelxl_version_number           2.014
_cod_database_fobs_code 2242811