Bioinspired Metal-Organic Helicate Drives Electrocatalytic Ethane Production from Carbon Dioxide
Gao, Liu; Wang, Jinfeng; Shen, Keshen; Jing, Xu; Duan, Chunying; Chemical Communications  (2026) –; doi:10.1039/D6CC01440B

data_7135741
_publ_section_title
;
 A bioinspired metal-organic helicate drives electrocatalytic ethane
 production from carbon dioxide.
;
_journal_issue                   37
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9414
_journal_page_last               9418
_journal_paper_doi               10.1039/d6cc01440b
_journal_volume                  62
_journal_year                    2026
_chemical_formula_moiety         'C105 H78 Fe2 N18 O9, 4(C3 H7 N O), 3(B F4)'
_chemical_formula_sum            'C117 H106 B3 F12 Fe2 N22 O13'
_chemical_formula_weight         2400.36
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-06-05
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2026-02-02 deposited with the CCDC.	2026-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                105.195(7)
_cell_angle_beta                 110.112(6)
_cell_angle_gamma                96.793(7)
_cell_formula_units_Z            2
_cell_length_a                   18.370(3)
_cell_length_b                   21.463(3)
_cell_length_c                   24.249(4)
_cell_measurement_reflns_used    9341
_cell_measurement_temperature    185.00
_cell_measurement_theta_max      51.462
_cell_measurement_theta_min      4.822
_cell_volume                     8432(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      185.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.1547
_diffrn_reflns_av_unetI/netI     0.0967
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            319035
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        53.269
_diffrn_reflns_theta_max         53.269
_diffrn_reflns_theta_min         1.785
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    1.309
_exptl_absorpt_correction_T_max  0.7505
_exptl_absorpt_correction_T_min  0.5487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.945
_exptl_crystal_description       block
_exptl_crystal_F_000             2482
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1551
_refine_ls_number_reflns         29321
_refine_ls_number_restraints     1765
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1523
_refine_ls_R_factor_gt           0.1203
_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^)+(0.0300P)^2^+13.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2754
_refine_ls_wR_factor_ref         0.2931
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17985
_reflns_number_total             29321
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6cc01440b2.cif
_cod_data_source_block           12561_0m_a
_cod_depositor_comments          'Adding full bibliography for 7135741.cif.'
_cod_database_code               7135741
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.880
_shelx_estimated_absorpt_t_min   0.848
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O12-C90 = O14-C90 = O9-C83 = O11-C83
 1.4 with sigma of 0.02
 H11-H23
 2.1 with sigma of 0.02
 F5-F6 \\sim F5-F7 \\sim F5-F8 \\sim F6-F7 \\sim F6-F8 \\sim F7-F8
 with sigma of 0.04
 B1-F3 \\sim B1-F4 \\sim B1-F1 \\sim B1-F2
 with sigma of 0.02
 B2-F5 \\sim B2-F6 \\sim B2-F7 \\sim B2-F8
 with sigma of 0.02
 F3-F4 \\sim F3-F1 \\sim F3-F2 \\sim F4-F1 \\sim F4-F2 \\sim F1-F2
 with sigma of 0.04
 F9-F12 \\sim F9-F10 \\sim F9-F11 \\sim F12-F10 \\sim F12-F11 \\sim F10-F11
 with sigma of 0.04
 B14-F9 \\sim B14-F12 \\sim B14-F10 \\sim B14-F11
 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Uanis(F9) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F11)
\\sim Ueq, Uanis(B14) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(B1) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F2) \\sim
Ueq, Uanis(F3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
5. Others
 Sof(H83A)=Sof(H90A)=Sof(O11)=Sof(H11)=Sof(O12)=Sof(H12A)=1-FVAR(1)
 Sof(H83)=Sof(O9)=Sof(H9A)=Sof(H90)=Sof(O14)=Sof(H14A)=FVAR(1)
 Sof(H86A)=Sof(O10)=Sof(H10A)=1-FVAR(2)
 Sof(H86)=Sof(O13)=Sof(H13)=FVAR(2)
6.a Riding coordinates:
 O9(H9A), O14(H14A)
6.b Ternary CH refined with riding coordinates:
 C83(H83), C83(H83A), C86(H86A), C86(H86), C90(H90A), C90(H90)
6.c Aromatic/amide H refined with riding coordinates:
 N3(H3), N6(H6), N8(H8), N12(H12), N15(H15), C1(H1), C2(H2), N17(H17), C4(H4),
 C7(H7), C8(H8A), C9(H9), C10(H10), C14(H14), C15(H15A), C17(H17A), C19(H19),
 C20(H20), C23(H23), C25(H25), C29(H29), C30(H30), C31(H31), C32(H32), C34(H34),
  C38(H38), C40(H40), C47(H47), C49(H49), C50(H50), C51(H51), C52(H52),
 C53(H53), C54(H54), C57(H57), C58(H58), C59(H59), C62(H62), C64(H64), C65(H65),
  C66(H66), C67(H67), C69(H69), C70(H70), C72(H72), C73(H73), C74(H74),
 C75(H75), C76(H76), C78(H78), C79(H79), C81(H81), C82(H82), C85(H85), C87(H87),
  C88(H88), C91(H91), C92(H92), C93(H93), C94(H94), C95(H95), C96(H96),
 C97(H97), C98(H98), C99(H99), C100(H100), C101(H101), C102(H102), C103(H103),
 C106(H106), C107(H107), C108(H108), C109(H109), C110(H110), C113(H113),
 C115(H115)
6.d Fitted hexagon refined as free rotating group:
 C75(C76,C77,C78,C79,C80)
6.e Idealised Me refined as rotating group:
 C89(H89A,H89B,H89C), C104(H10B,H10C,H10D), C105(H10E,H10F,H10G), C111(H11A,
 H11B,H11C), C112(H11D,H11E,H11F), C114(H11G,H11H,H11I), C116(H11J,H11K,H11L),
 C117(H11M,H11N,H11O)
6.f Idealised tetrahedral OH refined as rotating group:
 O10(H10A), O11(H11), O12(H12A), O13(H13)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              19047
_shelx_hkl_checksum              9800
_shelx_fab_checksum              95875
_olex2_submission_special_instructions 'No special instructions were received'