Solid-state NMR spectroscopic study of coordination compounds of XeF(2) with metal cations and the crystal structure of [Ba(XeF(2))(5)][AsF(6)](2).
Gerken, Michael; Hazendonk, Paul; Iuga, Adriana; Nieboer, Jared; Tramsek, Melita; Goreshnik, Evgeny; Zemva, Boris; Zheng, Shaohui; Autschbach, Jochen; Inorganic chemistry 46 (2007) 6069–6077; doi:10.1021/ic700557m

data_4339053
_publ_section_title
;
 Solid-state NMR spectroscopic study of coordination compounds of XeF(2)
 with metal cations and the crystal structure of
 [Ba(XeF(2))(5)][AsF(6)](2).
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6069
_journal_page_last               6077
_journal_paper_doi               10.1021/ic700557m
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         '2(F6 Sb), 5(F2 Xe), Ba'
_chemical_formula_sum            'Ba F22 Sb2 Xe5'
_chemical_formula_weight         1955.30
_space_group_IT_number           69
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2 2'
_symmetry_space_group_name_H-M   'F m m m'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2005-12-01T21:15:39-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0985(9)
_cell_length_b                   13.9437(10)
_cell_length_c                   13.6072(11)
_cell_measurement_reflns_used    148
_cell_measurement_temperature    200
_cell_measurement_theta_max      30.0326
_cell_measurement_theta_min      2.6835
_cell_volume                     2295.5(3)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_publication_material  'enCIFer 1.1 (CCDC, 2004)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
SIR92 (Altomare, et. al. 1994)
;
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.808
_diffrn_measurement_device
;
        Mercury CCD (2x2 bin mode)
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            3837
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.05
_diffrn_reflns_theta_min         3.37
_exptl_absorpt_coefficient_mu    11.452
_exptl_absorpt_correction_T_max  0.3621
_exptl_absorpt_correction_T_min  0.2058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing R.H., 1995'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    4.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Chunk
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         3.007
_refine_diff_density_min         -3.569
_refine_diff_density_rms         0.529
_refine_ls_extinction_coef       0.00071(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_matrix_type           full
_refine_ls_number_parameters     51
_refine_ls_number_reflns         765
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0534P)^2^+105.1887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1391
_refine_ls_wR_factor_ref         0.1531
_reflns_number_gt                575
_reflns_number_total             765
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic700557m-file010.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

2022-02-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'Ba2 F44 Sb4 Xe10'
_cod_original_formula_weight         2910.60
_cod_original_formula_moiety
'4(F6 Sb), F4 Xe2, F8 Xe4, F8 Xe4, 16(Ba0.12) '
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      Fmmm
_cod_database_code               4339053