Polymorphism of Alkali Bis(fluorosulfonyl)amides (M[N(SO2F)2], M = Na, K, and Cs)
Kazuhiko Matsumoto; Takaaki Oka; Toshiyuki Nohira; Rika Hagiwara; Inorganic Chemistry 52 (2013) 568–576; doi:10.1021/ic3010486

data_4333519
_publ_contact_author_address
;
Graduate School of Energy Science, Kyoto University
Yoshida, Sakyo-ku, Kyoto 606-8501, Japan
;
_publ_contact_author_email       k-matsumoto@energy.kyoto-u.ac.jp
_publ_contact_author_fax         81-75-753-4817
_publ_contact_author_name        'Kazuhiko Matsumoto'
_publ_contact_author_phone       81-75-753-4817
_publ_section_title
;
 Polymorphism of Alkali Bis(fluorosulfonyl)amides (M[N(SO2F)2], M = Na, K,
 and Cs)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              568
_journal_page_last               576
_journal_paper_doi               10.1021/ic3010486
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety
;
(K +), (N(SO2F)2 -)
;
_chemical_formula_sum            'F2 K N O4 S2'
_chemical_formula_weight         219.23
_chemical_name_common            K[N(SO2F)2]
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2bc 2ac'
_symmetry_space_group_name_H-M   'P c a b'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   12.0147(2)
_cell_length_b                   14.3150(3)
_cell_length_c                   14.3560(3)
_cell_measurement_reflns_used    18117
_cell_measurement_temperature    298
_cell_measurement_theta_max      54.96
_cell_measurement_theta_min      6.35
_cell_volume                     2469.09(8)
_computing_cell_refinement       'RAPID AUTO 2.40 (Rigaku 2006)'
_computing_data_collection       'Rigaku R-AXIS Rapid-II'
_computing_data_reduction        'RAPID AUTO 2.40 (Rigaku 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altmare et al., 1994)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku R-AXIS RapidII'
_diffrn_measurement_method       'imaging plate'
_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  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0181
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22532
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.17
_exptl_absorpt_coefficient_mu    1.534
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.500
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'RAPID AUTO 2.40 (Rigaku 2006)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.359
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2818
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+2.0576P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0799
_reflns_number_gt                2452
_reflns_number_total             2818
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3010486_si_001_03.cif
_cod_data_source_block           K[N(SO2F)2]_I-298K
_cod_database_code               4333519