Strong magnetic coupling of spins in Fe(ii) dimers with differently charged thioindigo ligands.
Konarev, Dmitri V.; Kuzmin, Alexey V.; Batov, Mikhail S.; Khasanov, Salavat S.; Otsuka, Akihiro; Yamochi, Hideki; Kitagawa, Hiroshi; Lyubovskaya, Rimma N.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 7692–7696; doi:10.1039/d0dt01262a

data_7704438
_publ_section_title
;
 Strong magnetic coupling of spins in Fe(ii) dimers with differently
 charged thioindigo ligands.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7692
_journal_page_last               7696
_journal_paper_doi               10.1039/d0dt01262a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'2(C32 H16 Fe O4 S4), 2(C18 H36 K N2 O6), 2(C6 H4 Cl2)'
_chemical_formula_sum            'C112 H112 Cl4 Fe2 K2 N4 O20 S8'
_chemical_formula_weight         2422.23
_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             2020-04-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-04-24 deposited with the CCDC.	2020-05-19 downloaded from the CCDC.
;
_cell_angle_alpha                68.714(3)
_cell_angle_beta                 78.174(3)
_cell_angle_gamma                73.182(3)
_cell_formula_units_Z            2
_cell_length_a                   14.2994(6)
_cell_length_b                   18.5793(6)
_cell_length_c                   23.5935(7)
_cell_measurement_reflns_used    8276
_cell_measurement_temperature    120.00(14)
_cell_measurement_theta_max      25.7550
_cell_measurement_theta_min      1.7390
_cell_volume                     5555.5(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.00(14)
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -53.00   5.00   1.00   80.00    --  -12.20 -57.00   0.00   58
  2  \w     15.00  45.00   1.00   80.00    --  -12.20  57.00-180.00   30
  3  \w      4.00  32.00   1.00   80.00    --  -12.20  37.00 -60.00   28
  4  \w    -86.00  -3.00   1.00   80.00    --  -12.20 -57.00-150.00   83
  5  \w    -38.00 -11.00   1.00   80.00    --  -12.20 -59.00  19.00   27
  6  \w    -22.00   5.00   1.00   80.00    --  -12.20 -37.00 120.00   27
  7  \w    -85.00  16.00   1.00   80.00    --  -12.20 -57.00 -60.00  101
  8  \w    -76.00   7.00   1.00   80.00    --  -12.20 -57.00  90.00   83
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0766
_diffrn_reflns_av_unetI/netI     0.1405
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            66054
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.500
_diffrn_reflns_theta_min         1.636
_exptl_absorpt_coefficient_mu    0.653
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94309
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       block
_exptl_crystal_F_000             2516
_exptl_crystal_size_max          0.315
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.033
_refine_diff_density_max         0.641
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1499
_refine_ls_number_reflns         25979
_refine_ls_number_restraints     740
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1525
_refine_ls_R_factor_gt           0.0687
_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^)+(0.0418P)^2^+0.5129P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1359
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14229
_reflns_number_total             25979
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01262a2.cif
_cod_data_source_block           cryptkfeti2dimer
_cod_depositor_comments          'Adding full bibliography for 7704438.cif.'
_cod_original_cell_volume        5555.6(4)
_cod_database_code               7704438
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 O402, C405
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Cl61 \\sim Cl62 \\sim Cl51 \\sim Cl52: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1.7A
C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C51 \\sim C52 \\sim
C53 \\sim C54 \\sim C55 \\sim C56: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 1.7A
Cl71 \\sim Cl72 \\sim Cl81 \\sim Cl82 \\sim Cl91 \\sim Cl92: within 1.7A with
sigma of 0.008 and sigma for terminal atoms of 0.016 within 1.7A
C71 \\sim C72 \\sim C73 \\sim C74 \\sim C75 \\sim C76 \\sim C81 \\sim C82 \\sim
C83 \\sim C84 \\sim C85 \\sim C86 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim
C95 \\sim C96: within 1.7A with sigma of 0.008 and sigma for terminal atoms of
0.016 within 1.7A
Uanis(C401) \\sim Ueq, Uanis(C402) \\sim Ueq, Uanis(C403) \\sim Ueq,
Uanis(C404) \\sim Ueq, Uanis(C405) \\sim Ueq, Uanis(C406) \\sim Ueq,
Uanis(C407) \\sim Ueq, Uanis(C408) \\sim Ueq, Uanis(C409) \\sim Ueq,
Uanis(C410) \\sim Ueq, Uanis(C411) \\sim Ueq, Uanis(C412) \\sim Ueq,
Uanis(C413) \\sim Ueq, Uanis(C414) \\sim Ueq, Uanis(C415) \\sim Ueq,
Uanis(C416) \\sim Ueq, Uanis(C417) \\sim Ueq, Uanis(C418) \\sim Ueq: with sigma
of 0.02 and sigma for terminal atoms of 0.04
Uanis(C71) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C74)
\\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C81) \\sim Ueq,
Uanis(C82) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C85)
\\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(C92) \\sim Ueq,
Uanis(C93) \\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(C95) \\sim Ueq, Uanis(C96)
\\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
4. Others
 1*[Sof(Cl71)+Sof(Cl72)+Sof(C71)+Sof(C72)+Sof(C73)+Sof(H73)+Sof(C74)+Sof(H74)+
 Sof(C75)+Sof(H75)+Sof(C76)+Sof(H76)]+1*[Sof(Cl81)+Sof(Cl82)+Sof(C81)+Sof(C82)+
 Sof(C83)+Sof(H83)+Sof(C84)+Sof(H84)+Sof(C85)+Sof(H85)+Sof(C86)+Sof(H86)]+1*
 [Sof(Cl92)+Sof(Cl91)+Sof(C91)+Sof(C92)+Sof(C93)+Sof(H93)+Sof(C94)+Sof(H94)+
 Sof(C95)+Sof(H95)+Sof(C96)+Sof(H96)]=1 with esd of 0.0001
 Sof(Cl71)=Sof(Cl72)=Sof(C71)=Sof(C72)=Sof(C73)=Sof(H73)=Sof(C74)=Sof(H74)=
 Sof(C75)=Sof(H75)=Sof(C76)=Sof(H76)=FVAR(1)
 Sof(Cl81)=Sof(Cl82)=Sof(C81)=Sof(C82)=Sof(C83)=Sof(H83)=Sof(C84)=Sof(H84)=
 Sof(C85)=Sof(H85)=Sof(C86)=Sof(H86)=FVAR(2)
 Sof(Cl92)=Sof(Cl91)=Sof(C91)=Sof(C92)=Sof(C93)=Sof(H93)=Sof(C94)=Sof(H94)=
 Sof(C95)=Sof(H95)=Sof(C96)=Sof(H96)=FVAR(3)
 Sof(Cl52)=Sof(Cl51)=Sof(C51)=Sof(C52)=Sof(C53)=Sof(H53)=Sof(C54)=Sof(H54)=
 Sof(C55)=Sof(H55)=Sof(C56)=Sof(H56)=1-FVAR(4)
 Sof(Cl62)=Sof(Cl61)=Sof(C61)=Sof(C62)=Sof(C63)=Sof(H63)=Sof(C64)=Sof(H64)=
 Sof(C65)=Sof(H65)=Sof(C66)=Sof(H66)=FVAR(4)
5.a Free rotating group:
 Cl62(Cl61,C61,C62,C63,C64,C65,C66), Cl52(Cl51,C51,C52,C53,C54,C55,C56),
 Cl71(Cl72,C71,C72,C73,C74,C75,C76), Cl81(Cl82,C81,C82,C83,C84,C85,C86),
 Cl92(Cl91,C91,C92,C93,C94,C95,C96)
5.b Secondary CH2 refined with riding coordinates:
 C301(H30A,H30B), C302(H30C,H30D), C303(H30E,H30F), C304(H30G,H30H), C305(H30I,
 H30J), C306(H30K,H30L), C307(H30M,H30N), C308(H30O,H30P), C309(H30Q,H30R),
 C310(H31A,H31B), C311(H31C,H31D), C312(H31E,H31F), C313(H31G,H31H), C314(H31I,
 H31J), C315(H31K,H31L), C316(H31M,H31N), C317(H31O,H31P), C318(H31Q,H31R),
 C401(H40A,H40B), C402(H40C,H40D), C403(H40E,H40F), C404(H40G,H40H), C405(H40I,
 H40J), C406(H40K,H40L), C407(H40M,H40N), C408(H40O,H40P), C409(H40Q,H40R),
 C410(H41A,H41B), C411(H41C,H41D), C412(H41E,H41F), C413(H41G,H41H), C414(H41I,
 H41J), C415(H41K,H41L), C416(H41M,H41N), C417(H41O,H41P), C418(H41Q,H41R)
5.c Aromatic/amide H refined with riding coordinates:
 C102(H102), C103(H103), C104(H104), C105(H105), C112(H112), C113(H113),
 C114(H114), C115(H115), C118(H118), C119(H119), C120(H120), C121(H121),
 C128(H128), C129(H129), C130(H130), C131(H131), C202(H202), C203(H203),
 C204(H204), C205(H205), C212(H212), C213(H213), C214(H214), C215(H215),
 C218(H218), C219(H219), C220(H220), C221(H221), C228(H228), C229(H229),
 C230(H230), C231(H231), C63(H63), C64(H64), C65(H65), C66(H66), C53(H53),
 C54(H54), C55(H55), C56(H56), C73(H73), C74(H74), C75(H75), C76(H76), C83(H83),
  C84(H84), C85(H85), C86(H86), C93(H93), C94(H94), C95(H95), C96(H96)
;
_shelx_res_checksum              33297
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;