Fluoride ion chelation <i>via</i> pnictogen bonding using a distibora[1.1]ferrocenophane.
Thakur, Arunabha; Murphy, Brendan L.; Jiang, You; Bhuvanesh, Nattamai; Gabbaï, François P; Chemical communications (Cambridge, England) 62 (2026) 5293–5296; doi:10.1039/d5cc06492a

data_7135439
_publ_section_title
;
 Fluoride ion chelation <i>via</i> pnictogen bonding using a
 distibora[1.1]ferrocenophane.
;
_journal_issue                   18
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5293
_journal_page_last               5296
_journal_paper_doi               10.1039/d5cc06492a
_journal_volume                  62
_journal_year                    2026
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C44 H26 Cl8 F Fe2 O4 Sb2, 1.67(C2 H6 O S), C16 H36 N'
_chemical_formula_sum            'C63.34 H72.02 Cl8 F Fe2 N O5.67 S1.67 Sb2'
_chemical_formula_weight         1649.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-12-13
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2026-01-12 deposited with the CCDC.	2026-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.355(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3688(9)
_cell_length_b                   36.463(3)
_cell_length_c                   14.5282(10)
_cell_measurement_reflns_used    4295
_cell_measurement_temperature    110
_cell_measurement_theta_max      20.61
_cell_measurement_theta_min      2.23
_cell_volume                     6759.6(9)
_computing_cell_refinement       'SAINT V8.41 (Bruker, 2016)'
_computing_data_collection       'APEX 4 (Bruker, 2022)'
_computing_data_reduction        'SAINT V8.41 (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Quest (PHOTON III)'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1042
_diffrn_reflns_av_unetI/netI     0.0849
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            44397
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        22.507
_diffrn_reflns_theta_max         22.507
_diffrn_reflns_theta_min         1.845
_diffrn_source                   'Bruker QUEST MoIuS'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.631
_exptl_absorpt_correction_T_max  0.7060
_exptl_absorpt_correction_T_min  0.6346
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1102 before and 0.0797 after correction. 
The Ratio of minimum to maximum transmission is 0.8989. 
The \l/2 correction factor is Not present. 
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_description       block
_exptl_crystal_F_000             3321
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.397
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details
;
 Flack x determined using 3062 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     791
_refine_ls_number_reflns         8817
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0477
_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^)+(0.0526P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1106
_reflns_Friedel_coverage         0.995
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                7317
_reflns_number_total             8817
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06492a2.cif
_cod_data_source_block           fg_at_sb_3
_cod_depositor_comments
'Adding full bibliography for 7135436--7135439.cif.'
_cod_original_cell_volume        6759.5(8)
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               7135439
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.564
_shelx_estimated_absorpt_t_min   0.451
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S5S-C7S \\sim S5S-C8S
 with sigma of 0.02
 C7S-O6S \\sim C8S-O6S
 with sigma of 0.04
 S5T-C8T \\sim S5T-C7T
 with sigma of 0.02
 C8T-O6T \\sim C7T-O6T
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O6S \\sim S5S \\sim C7S \\sim C8S: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
O6T \\sim S5T \\sim C7T \\sim C8T: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C17 \\sim C18 \\sim C19: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Uanis(C7S) = Uanis(C7T)
Uanis(C8S) = Uanis(C8T)
Uanis(O6T) = Uanis(O6S)
4. Rigid body (RIGU) restrains
 O6S, S5S, C7S, C8S
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O6T, S5T, C7T, C8T
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C17, C18, C19
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Fixed Sof: S1S(0.83) O2S(0.83) C3S(0.83) H3SA(0.83) H3SB(0.83) H3SC(0.83)
 C4S(0.83) H4SA(0.83) H4SB(0.83) H4SC(0.83) O6S(0.44) S5S(0.44) C7S(0.44)
 H7SA(0.44) H7SB(0.44) H7SC(0.44) C8S(0.44) H8SA(0.44) H8SB(0.44) H8SC(0.44)
 O6T(0.4) S5T(0.4) C7T(0.4) H7TA(0.4) H7TB(0.4) H7TC(0.4) C8T(0.4) H8TA(0.4)
 H8TB(0.4) H8TC(0.4)
6.a Free rotating group:
 O6S(S5S,C7S,C8S), O6T(S5T,C7T,C8T)
6.b Ternary CH refined with riding coordinates:
 C8(H8)
6.c Secondary CH2 refined with riding coordinates:
 C1C(H1CA,H1CB), C2C(H2CA,H2CB), C3C(H3CA,H3CB), C5C(H5CA,H5CB), C6C(H6CA,
 H6CB), C7C(H7CA,H7CB), C9C(H9CA,H9CB), C10C(H10A,H10B), C11C(H11A,H11B),
 C13C(H13A,H13B), C14C(H14A,H14B), C15C(H15A,H15B)
6.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C9(H9), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23),
  C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32)
6.e Idealised Me refined as rotating group:
 C3S(H3SA,H3SB,H3SC), C4S(H4SA,H4SB,H4SC), C4C(H4CA,H4CB,H4CC), C8C(H8CA,H8CB,
 H8CC), C12C(H12A,H12B,H12C), C16C(H16A,H16B,H16C), C7S(H7SA,H7SB,H7SC),
 C8S(H8SA,H8SB,H8SC), C7T(H7TA,H7TB,H7TC), C8T(H8TA,H8TB,H8TC)
;
_shelx_res_checksum              9773
_shelx_hkl_checksum              15785
_olex2_submission_original_sample_id FGB_AT_251212_dQ_17R_at_sb_3
_olex2_submission_special_instructions 'No special instructions were received'