Binucleating Jäger-type {(N<sub>2</sub>O<sub>2</sub>)<sub>2</sub>}<sup>4-</sup> ligands: magnetic and electronic interactions of Fe(II), Ni(II) and Cu(II) across an in-plane TTF-bridge.
Schreck, Constantin; Schönfeld, Sophie; Liebing, Phil; Hörner, Gerald; Weber, Birgit; Dalton transactions (Cambridge, England : 2003) 53 (2024) 9092–9105; doi:10.1039/d4dt00479e

data_7715943
_publ_section_title
;
 Binucleating J&#xe4;ger-type
 {(N<sub>2</sub>O<sub>2</sub>)<sub>2</sub>}<sup>4-</sup> ligands: magnetic
 and electronic interactions of Fe(II), Ni(II) and Cu(II) across an
 in-plane TTF-bridge.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9092
_journal_page_last               9105
_journal_paper_doi               10.1039/d4dt00479e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C62 H48 F12 N8 Ni2 O12 S4'
_chemical_formula_sum            'C62 H48 F12 N8 Ni2 O12 S4'
_chemical_formula_weight         1570.74
_space_group_crystal_system      tetragonal
_space_group_IT_number           77
_space_group_name_Hall           'P 4c'
_space_group_name_H-M_alt        'P 42'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-09-12
_audit_creation_method
;
'Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)'
;
_audit_update_record
;
2024-02-13 deposited with the CCDC.	2024-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8926(3)
_cell_length_b                   17.8926(3)
_cell_length_c                   24.3239(5)
_cell_measurement_reflns_used    15232
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      29.0
_cell_measurement_theta_min      1.8
_cell_volume                     7787.2(2)
_computing_cell_refinement       X-AREA-STOE
_computing_data_collection       X-AREA-STOE
_computing_data_reduction        X-AREA-STOE
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      180.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Stoe StadiVari diffractometer'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.1060
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            34757
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.094
_diffrn_reflns_theta_min         1.814
_exptl_absorpt_coefficient_mu    0.677
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3200
_exptl_crystal_size_max          0.054
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.041
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.44(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.938
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     953
_refine_ls_number_reflns         16403
_refine_ls_number_restraints     118
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.1274
_refine_ls_R_factor_gt           0.0572
_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^)+(0.0674P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1180
_refine_ls_wR_factor_ref         0.1447
_reflns_Friedel_coverage         0.869
_reflns_Friedel_fraction_full    0.920
_reflns_Friedel_fraction_max     0.910
_reflns_number_gt                8587
_reflns_number_total             16403
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00479e2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 7715943.cif.'
_cod_original_cell_volume        7787.2(3)
_cod_database_code               7715943
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.935
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.56(2)
 0.44(2)
2. 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
3. Uiso/Uaniso restraints and constraints
O12 \\sim C41 \\sim C42: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01 within 2A
Uanis(O5A) \\sim Ueq, Uanis(O5B) \\sim Ueq, Uanis(O6B) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.04
Uanis(O6A) \\sim Ueq, Uanis(C12A) \\sim Ueq, Uanis(C13A) \\sim Ueq, Uanis(C14A)
\\sim Ueq, Uanis(C14B) \\sim Ueq, Uanis(C13B) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C12B) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 O5A, O6A, C12A, C13A, C14A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5B, O6B, C12B, C13B, C14B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C41, C42
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O5B)=Sof(O6B)=Sof(C12B)=Sof(C13B)=Sof(H13C)=Sof(H13D)=Sof(C14B)=Sof(H14D)=
 Sof(H14E)=Sof(H14F)=1-FVAR(1)
 Sof(O5A)=Sof(O6A)=Sof(C12A)=Sof(C13A)=Sof(H13A)=Sof(H13B)=Sof(C14A)=Sof(H14A)=
 Sof(H14B)=Sof(H14C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C34(H34A,H34B), C41(H41A,H41B), C13A(H13A,H13B), C13B(H13C,H13D)
6.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C17(H17), C18(H18), C25(H25), C26(H26), C29(H29), C36(H36),
 C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50),
  C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57),
 C58(H58), C59(H59), C60(H60), C61(H61), C62(H62)
6.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C35(H35A,H35B,H35C), C42(H42A,H42B,H42C), C14A(H14A,H14B,
 H14C), C14B(H14D,H14E,H14F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              2759
_shelx_fab_checksum              51383
_olex2_submission_special_instructions 'No special instructions were received'