Designing Potassium Battery Salts through a Solvent-in-Anion Concept for Concentrated Electrolytes and Mimicking Solvation Structures
Schkeryantz, Luke A.; Zheng, Jingfeng; McCulloch, William D.; Qin, Lei; Zhang, Songwei; Moore, Curtis E.; Wu, Yiying; Chemistry of Materials 32 (2020) 10423–10434; doi:10.1021/acs.chemmater.0c02983

data_4003835
_publ_section_title
;
 Designing Potassium Battery Salts through a Solvent-in-Anion Concept for
 Concentrated Electrolytes and Mimicking Solvation Structures
;
_journal_issue                   24
_journal_name_full               'Chemistry of Materials'
_journal_page_first              10423
_journal_page_last               10434
_journal_paper_doi               10.1021/acs.chemmater.0c02983
_journal_volume                  32
_journal_year                    2020
_chemical_formula_moiety
'0.02(C448 H704 F192 K64 N64 O192 S64), 0.25(C H2 Cl2)'
_chemical_formula_sum            'C7.25 H11.5 Cl0.5 F3 K N O3 S'
_chemical_formula_weight         306.56
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            64
_cell_length_a                   18.2533(14)
_cell_length_b                   32.815(3)
_cell_length_c                   32.965(3)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.262
_cell_measurement_theta_min      3.344
_cell_volume                     19745(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0810
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            61277
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.378
_diffrn_reflns_theta_min         2.837
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.740
_exptl_absorpt_correction_T_max  0.2590
_exptl_absorpt_correction_T_min  0.2157
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0660 before and 0.0590 after correction. The Ratio of minimum to maximum transmission is 0.8328. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_description       needle
_exptl_crystal_F_000             10016
_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.940
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4542
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0454P)^2^+131.6360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.1061
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3417
_reflns_number_total             4542
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm0c02983_si_004.cif
_cod_data_source_block           fddd
_cod_depositor_comments
'Adding full bibliography for 4003834--4003838.cif.'
_cod_original_sg_symbol_H-M      'F d d d'
_cod_original_formula_sum        'C7.25 H11.50 Cl0.50 F3 K N O3 S'
_cod_database_code               4003835
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.848
_olex2_refinement_description
;
1. Others
 Fixed Sof: Cl1(0.5) Cl2(0.5) C8(0.5) H8A(0.5) H8B(0.5)
 Fixed U12: K1'(0)
 Fixed U13: K1"(0)
 Fixed U23: K1"(0) K1'(0)
 Fixed Uiso: H1A(0.023) H1B(0.023) H1'A(0.042) H1'B(0.042) H2(0.023) H2'(0.03)
 H3A(0.028) H3B(0.028) H3'A(0.041) H3'B(0.041) H4A(0.037) H4B(0.037) H4'A(0.06)
 H4'B(0.06) H5A(0.032) H5B(0.032) H5'A(0.046) H5'B(0.046) H6A(0.025) H6B(0.025)
 H6'A(0.051) H6'B(0.051) H8A(0.089) H8B(0.089)
 Fixed X: K1"(0.125) K1'(0.375) H1A(0.314045) H1B(0.282273) H1'A(0.292222)
 H1'B(0.26555) H2(0.414484) H2'(0.372878) H3A(0.408836) H3B(0.330171)
 H3'A(0.44889) H3'B(0.391665) H4A(0.463772) H4B(0.420864) H4'A(0.486284)
 H4'B(0.470387) H5A(0.333071) H5B(0.410347) H5'A(0.362442) H5'B(0.304713)
 H6A(0.273082) H6B(0.318679) H6'A(0.262705) H6'B(0.271638) H8A(0.385365)
 H8B(0.389052)
 Fixed Y: K1"(0.625) H1A(0.853336) H1B(0.808619) H1'A(0.542195) H1'B(0.539345)
 H2(0.822205) H2'(0.499627) H3A(0.7555) H3B(0.748616) H3'A(0.516822)
 H3'B(0.498614) H4A(0.761707) H4B(0.719199) H4'A(0.450873) H4'B(0.451169)
 H5A(0.809958) H5B(0.816893) H5'A(0.420906) H5'B(0.401334) H6A(0.80821)
 H6B(0.849814) H6'A(0.465065) H6'B(0.465869) H8A(0.589162) H8B(0.587135)
 Fixed Z: K1'(0.375) H1A(0.540382) H1B(0.548934) H1'A(0.27896) H1'B(0.325163)
 H2(0.504591) H2'(0.340022) H3A(0.53055) H3B(0.510023) H3'A(0.286021)
 H3'B(0.253905) H4A(0.466531) H4B(0.468839) H4'A(0.264791) H4'B(0.312595)
 H5A(0.406412) H5B(0.428326) H5'A(0.337491) H5'B(0.30653) H6A(0.469395)
 H6B(0.465825) H6'A(0.331146) H6'B(0.282816) H8A(0.098002) H8B(0.146163)
;
_shelx_res_checksum              51208
_shelx_hkl_checksum              77583
_olex2_submission_special_instructions 'No special instructions were received'