Isostructural bridging diferrous chalcogenide cores [Fe<sup>II</sup>(μ-E)Fe<sup>II</sup>] (E = O, S, Se, Te) with decreasing antiferromagnetic coupling down the chalcogenide series.
Zars, Ethan; Gravogl, Lisa; Gau, Michael R.; Carroll, Patrick J.; Meyer, Karsten; Mindiola, Daniel J.; Chemical science 14 (2023) 6770–6779; doi:10.1039/d3sc01094e

data_1569237
_publ_section_title
;
 Isostructural bridging diferrous chalcogenide cores
 [Fe<sup>II</sup>(&#x3bc;-E)Fe<sup>II</sup>] (E = O, S, Se, Te) with
 decreasing antiferromagnetic coupling down the chalcogenide series.
;
_journal_issue                   24
_journal_name_full               'Chemical science'
_journal_page_first              6770
_journal_page_last               6779
_journal_paper_doi               10.1039/d3sc01094e
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C58 H82 Fe2 K2 N6 O, 2.5(C7 H8), 0.5(C5 H12)'
_chemical_formula_sum            'C78 H108 Fe2 K2 N6 O'
_chemical_formula_weight         1335.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-15
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2023-02-16 deposited with the CCDC.	2023-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.8250(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.3804(2)
_cell_length_b                   13.85310(10)
_cell_length_c                   23.00070(10)
_cell_measurement_reflns_used    80457
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.8260
_cell_measurement_theta_min      1.9370
_cell_volume                     7361.53(9)
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_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
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_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100
_diffrn_detector                 'HPC area detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix 3000HE'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -10.00  91.00   0.50   15.00    --   20.19  33.00  17.00  202
  2  \w     -8.00  95.00   0.50   15.00    --   20.19  45.00-120.00  206
  3  \w     -3.00  54.00   0.50   15.00    --   20.19 -80.00 -67.61  114
  4  \w    -17.00  55.00   0.50   15.00    --   20.19 -80.00 -35.94  144
  5  \w    -22.00  16.00   0.50   15.00    --  -19.56 -80.00 -43.30   76
  6  \w    -22.00  16.00   0.50   15.00    --  -19.56 -80.00 -97.47   76
  7  \w    -24.00  15.00   0.50   15.00    --  -19.56 -78.00-144.02   78
  8  \w    -23.00  15.00   0.50   15.00    --  -19.56 -79.00-157.83   76
  9  \w    -22.00  55.00   0.50   15.00    --   20.19 -80.00 -84.65  154
 10  \w    -23.00  15.00   0.50   15.00    --  -19.56 -79.00   7.54   76
 11  \w    -22.00  16.00   0.50   15.00    --  -19.56 -80.00  73.99   76
 12  \w    -22.00  16.00   0.50   15.00    --  -19.56 -80.00 100.07   76
 13  \w    -25.00  15.00   0.50   15.00    --  -19.56 -77.00 150.00   80
 14  \w    -22.00  16.00   0.50   15.00    --  -19.56 -80.00 137.60   76
 15  \w    -25.00  15.00   0.50   15.00    --  -19.56 -77.00  90.00   80
 16  \w    -22.00  16.00   0.50   15.00    --  -19.56 -80.00  46.81   76
 17  \w    -22.00  16.00   0.50   15.00    --  -19.56 -80.00  -9.87   76
 18  \w    -22.00  55.00   0.50   15.00    --   20.19 -80.00 -60.27  154
 19  \w    -23.00  55.00   0.50   15.00    --   20.19 -79.00  87.92  156
 20  \w    -22.00  55.00   0.50   15.00    --   20.19 -80.00 148.17  154
 21  \w    -22.00  55.00   0.50   15.00    --   20.19 -80.00  65.10  154
 22  \w     -8.00  95.00   0.50   15.00    --   20.19  45.00  60.00  206
 23  \w     -8.00  95.00   0.50   15.00    --   20.19  45.00 150.00  206
 24  \w    -15.00  22.00   0.50   15.00    --   20.19  80.00  71.43   74
 25  \w    -11.00  48.00   0.50   15.00    --   20.19  61.00  60.00  118
 26  \w    -11.00  48.00   0.50   15.00    --   20.19  61.00 -60.00  118
 27  \w    -11.00  48.00   0.50   15.00    --   20.19  61.00-180.00  118
 28  \w    -14.00  25.00   0.50   15.00    --   20.19  77.00 -60.00   78
 29  \w    -49.00  57.00   0.50   15.00    --  -19.56  33.00  17.00  212
 30  \w    -48.00  12.00   0.50   15.00    --  -19.56 -61.00 -90.00  120
 31  \w    -57.00  17.00   0.50   15.00    --   20.19 -33.00-140.00  148
 32  \w    -51.00  48.00   0.50   15.00    --  -19.56  61.00-150.00  198
 33  \w    -55.00  22.00   0.50   15.00    --  -19.56  80.00 -81.80  154
 34  \w    -57.00  14.00   0.50   15.00    --   20.19 -30.00   0.00  142
 35  \w    -57.00  14.00   0.50   15.00    --   20.19 -30.00  30.00  142
 36  \w    -53.00  58.00   0.50   15.00    --  -19.56  30.00 150.00  222
 37  \w    -55.00  22.00   0.50   15.00    --  -19.56  80.00 148.74  154
 38  \w    -57.00  14.00   0.50   15.00    --   20.19 -30.00  60.00  142
 39  \w    -57.00  14.00   0.50   15.00    --   20.19 -30.00 150.00  142
 40  \w    -63.00   3.00   0.50   15.00    --   20.19 -15.00  60.00  132
 41  \w    -63.00   3.00   0.50   15.00    --   20.19 -15.00  90.00  132
 42  \w    -63.00   3.00   0.50   15.00    --   20.19 -15.00 -60.00  132
 43  \w    -57.00  14.00   0.50   15.00    --   20.19 -30.00-180.00  142
 44  \w    -96.00   9.00   0.50   15.00    --  -19.56 -33.00-140.00  210
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-i'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0194981000
_diffrn_orient_matrix_UB_12      -0.0363170000
_diffrn_orient_matrix_UB_13      -0.0063332000
_diffrn_orient_matrix_UB_21      0.0237097500
_diffrn_orient_matrix_UB_22      0.0296959500
_diffrn_orient_matrix_UB_23      0.0116875000
_diffrn_orient_matrix_UB_31      -0.0002196500
_diffrn_orient_matrix_UB_32      -0.0204337500
_diffrn_orient_matrix_UB_33      0.0282518000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            131883
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         1.870
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.554
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74167
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            'light red'
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_description       block
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         8435
_refine_ls_number_restraints     174
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0559P)^2^+11.6443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1044
_refine_ls_wR_factor_ref         0.1067
_reflns_number_gt                7691
_reflns_number_total             8435
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01094e2.cif
_cod_data_source_block           9707i_2-O
_cod_depositor_comments
'Adding full bibliography for 1569232--1569239.cif.'
_cod_database_code               1569237
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              7568
_shelx_hkl_checksum              15383
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.268
_oxdiff_exptl_absorpt_empirical_full_min 0.827