Synergy between the coordination and trace ionization of co-solvents enables reversible magnesium electroplating/stripping behavior
Wang, Min; Sun, Wenhao; Zhang, Kun; Zhang, Zhonghua; Du, Aobing; Dong, Shanmu; Zhang, Jinlei; Liu, Jing; Chen, Xi; Zhou, Zhenfang; Li, Fujun; Li, Zhenjiang; Li, Guicun; Cui, Guanglei; Energy & Environmental Science 17 (2024) 630–641; doi:10.1039/D3EE02450D

data_1570432
_publ_section_title
;
 Synergy between the coordination and trace ionization of co-solvents
 enables reversible magnesium electroplating/stripping behavior
;
_journal_issue                   2
_journal_name_full               'Energy &amp; Environmental Science'
_journal_page_first              630
_journal_page_last               641
_journal_paper_doi               10.1039/D3EE02450D
_journal_volume                  17
_journal_year                    2024
_chemical_formula_moiety
'C2 H F6 N O4 S2, C2 H0.6 F6 N O4 S2, 2(C15 H42 Mg0.5 N6)'
_chemical_formula_sum            'C34 H85.6 F12 Mg N14 O8 S4'
_chemical_formula_weight         1199.31
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-04-11
_audit_creation_method
;
Olex2 1.3-beta
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-07-26 deposited with the CCDC.	2023-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                91.969(8)
_cell_angle_beta                 96.720(9)
_cell_angle_gamma                101.570(9)
_cell_formula_units_Z            2
_cell_length_a                   9.611(2)
_cell_length_b                   15.130(3)
_cell_length_c                   21.533(5)
_cell_measurement_reflns_used    7475
_cell_measurement_temperature    170
_cell_measurement_theta_max      27.312
_cell_measurement_theta_min      2.282
_cell_volume                     3041.1(11)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker D8'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_unetI/netI     0.0694
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            37340
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.560
_diffrn_reflns_theta_min         1.908
_exptl_absorpt_coefficient_mu    0.256
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0919 before and 0.0493 after correction.
The Ratio of minimum to maximum transmission is 0.9189.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       block
_exptl_crystal_F_000             1271
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     766
_refine_ls_number_reflns         13901
_refine_ls_number_restraints     210
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_gt           0.0640
_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^)+(0.0659P)^2^+2.2461P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1746
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8832
_reflns_number_total             13901
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ee02450d2.cif
_cod_data_source_block           pdag14_0m
_cod_depositor_comments          'Adding full bibliography for 1570432.cif.'
_cod_original_cell_volume        3041.0(12)
_cod_original_formula_sum        'C34 H85.60 F12 Mg N14 O8 S4'
_cod_database_code               1570432
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.951
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S06-C2
 1.8 with sigma of 0.01
 C2-F5
 1.27 with sigma of 0.02
 C2-F3
 1.29 with sigma of 0.02
 C2-F4
 1.36 with sigma of 0.02
 C1-F1
 1.29 with sigma of 0.02
 C1-F2
 1.36 with sigma of 0.02
 C1-F6
 1.27 with sigma of 0.02
 N01I-C01V = N4-C86
 1.45 with sigma of 0.001
 C01F-C012
 1.45 with sigma of 0.01
 N01I-C01F
 1.45 with sigma of 0.1
 F3-F4 \\sim F4-F5 \\sim F5-F3
 with sigma of 0.03
 C2-F3 \\sim C2-F4 \\sim C2-F5
 with sigma of 0.02
 F1-F2 \\sim F2-F6 \\sim F6-F1
 with sigma of 0.03
 C1-F1 \\sim C1-F2 \\sim C1-F6
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C012 \\sim C01F \\sim N4 \\sim N01I \\sim C5: within 3.8A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 3.8A
S06 \\sim C2 \\sim F3 \\sim F5 \\sim F4 \\sim O01U: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
H01C \\sim C86 \\sim C3 \\sim H01D \\sim F6 \\sim C01F \\sim H3D \\sim H01R
\\sim H86B \\sim H01S \\sim N4 \\sim S1 \\sim H3C \\sim O2 \\sim H3E \\sim C1
\\sim H86A \\sim F1 \\sim H86C \\sim F2: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
4. Others
 Sof(H01C)=Sof(H01D)=1-FVAR(1)
 Sof(H01A)=Sof(H01B)=FVAR(1)
 Fixed Sof: S06(0.6) C01F(0.33333) H01R(0.33333) H01S(0.33333) N01I(0.66667)
 O01U(0.6) C01V(0.66667) H01Z(0.66667) HP(0.66667) HQ(0.66667) C01Z(0.66667)
 H1(0.66667) HV(0.66667) HW(0.66667) H2A(0.6) S1(0.4) O2(0.4) C2(0.6) F3(0.6)
 F4(0.6) F5(0.6) C1(0.4) F1(0.4) F2(0.4) F6(0.4) N4(0.33333) C3(0.33333)
 H3C(0.33333) H3D(0.33333) H3E(0.33333) C5(0.66667) H5C(0.66667) H5D(0.66667)
 C86(0.33333) H86A(0.33333) H86B(0.33333) H86C(0.33333)
5.a Secondary CH2 refined with riding coordinates:
 N008(H00C,H00D), N5(H5A,H5B), N3(H3A,H3B), N1(H1A,H1B), N00I(H00E,H00F),
 N00J(H00G,H00H), C00X(H00A,H00B), C011(H2,H), C012(H01A,H01B), C012(H01C,H01D),
  C013(H01E,H01F), C014(H01G,H01H), C015(H01I,H01J), C016(H3,HA), C017(H01K,
 H01L), C019(H4,HB), C01A(H5,HC), C01B(H01M,H01N), C01E(H6,HD), C01F(H01R,H01S),
  C01G(H01T,H01U), C01L(H7,HE), C01M(H8,HF), C01P(H10,HI), C020(H02A,H02B),
 C5(H5C,H5D)
5.b Aromatic/amide H refined with riding coordinates:
 N00N(H00N), N2(H2A)
5.c Idealised Me refined as rotating group:
 C01C(H01O,H01P,H01Q), C01J(H01V,H01W,H01X), C01N(H9,HG,HH), C01R(H01Y,HJ,HK),
 C01S(H11,HL,HM), C01T(H12,HN,HO), C01V(H01Z,HP,HQ), C01W(H01,HR,HS), C01Y(H13,
 HT,HU), C01Z(H1,HV,HW), C022(H02C,H02D,H02E), C023(H02F,H02G,H02H), C3(H3C,H3D,
 H3E), C86(H86A,H86B,H86C)
;
_shelx_res_checksum              53228
_olex2_submission_special_instructions 'No special instructions were received'