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_1569238
_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 Se, 2(C4 H10 O)'
_chemical_formula_sum            'C66 H102 Fe2 K2 N6 O2 Se'
_chemical_formula_weight         1280.39
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-02-16 deposited with the CCDC.	2023-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                104.5730(10)
_cell_angle_beta                 102.7920(10)
_cell_angle_gamma                92.5040(10)
_cell_formula_units_Z            2
_cell_length_a                   14.13070(10)
_cell_length_b                   15.18640(10)
_cell_length_c                   16.75930(10)
_cell_measurement_reflns_used    67760
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.08
_cell_volume                     3375.48(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (Rigaku OD, 2019)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'HPC area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HyPix 3000HE'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_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    -41.00  60.00   0.50   15.00    --  -14.00  19.00  60.00  202
  2  \w     -2.00  83.00   0.50   15.00    --   14.70  37.00 150.00  170
  3  \w     -9.00  17.00   0.50   15.00    --   14.70  80.00 102.41   52
  4  \w     -5.00  35.00   0.50   15.00    --   14.70  57.00 150.00   80
  5  \w    -42.00  25.00   0.50   15.00    --  -14.00  77.00 150.00  134
  6  \w    -54.00  -1.00   0.50   15.00    --   14.70 -19.00   0.00  106
  7  \w    -23.00  15.00   0.50   15.00    --  -14.00 -79.00 -13.84   76
  8  \w    -12.00  22.00   0.50   15.00    --   14.70 -78.00 -34.33   68
  9  \w    -22.00  15.00   0.50   15.00    --  -14.00 -80.00 -60.01   74
 10  \w    -22.00  15.00   0.50   15.00    --  -14.00 -80.00-138.99   74
 11  \w      4.00  29.00   0.50   15.00    --   14.70 -78.00-144.56   50
 12  \w    -22.00  15.00   0.50   15.00    --  -14.00 -80.00-157.89   74
 13  \w    -23.00  15.00   0.50   15.00    --  -14.00 -79.00 -93.52   76
 14  \w    -23.00  15.00   0.50   15.00    --  -14.00 -79.00-119.32   76
 15  \w    -23.00  15.00   0.50   15.00    --  -14.00 -79.00 -39.33   76
 16  \w    -22.00  15.00   0.50   15.00    --  -14.00 -80.00  18.21   74
 17  \w    -22.00  15.00   0.50   15.00    --  -14.00 -80.00 100.71   74
 18  \w    -22.00  15.00   0.50   15.00    --  -14.00 -80.00 119.83   74
 19  \w    -23.00  15.00   0.50   15.00    --  -14.00 -79.00  61.33   76
 20  \w    -22.00  15.00   0.50   15.00    --  -14.00 -80.00  74.47   74
 21  \w    -23.00  15.00   0.50   15.00    --  -14.00 -79.00 117.00   76
 22  \w    -23.00  15.00   0.50   15.00    --  -14.00 -79.00 161.85   76
 23  \w    -21.00  24.00   0.50   15.00    --   14.70 -80.00 148.60   90
 24  \w    -22.00  44.00   0.50   15.00    --   14.70 -80.00  50.17  132
 25  \w    -23.00  15.00   0.50   15.00    --  -14.00 -79.00  33.22   76
 26  \w    -22.00  44.00   0.50   15.00    --   14.70 -80.00 -15.77  132
 27  \w     18.00  94.00   0.50   15.00    --   14.70   7.00-143.00  152
 28  \w     -8.00  57.00   0.50   15.00    --   14.70  57.00 -90.00  130
 29  \w    -13.00  25.00   0.50   15.00    --   14.70  77.00 -30.00   76
 30  \w    -14.00  22.00   0.50   15.00    --   14.70  80.00 -97.55   72
 31  \w    -31.00  54.00   0.50   15.00    --  -14.00  37.00-150.00  170
 32  \w    -37.00  54.00   0.50   15.00    --  -14.00  57.00-150.00  182
 33  \w    -34.00  -2.00   0.50   15.00    --   14.70   7.00-143.00   64
 34  \w    -49.00  65.00   0.50   15.00    --  -14.00   7.00-143.00  228
 35  \w    -24.00  10.00   0.50   15.00    --   14.70 -78.00 105.48   68
 36  \w    -51.00 -20.00   0.50   15.00    --   14.70 -19.00  30.00   62
 37  \w    -59.00   9.00   0.50   15.00    --  -14.00 -57.00 -30.00  136
 38  \w    -57.00   5.00   0.50   15.00    --   14.70 -19.00 -90.00  124
 39  \w    -59.00   9.00   0.50   15.00    --  -14.00 -57.00-120.00  136
 40  \w    -59.00   5.00   0.50   15.00    --   14.70 -19.00-150.00  128
 41  \w    -42.00  25.00   0.50   15.00    --  -14.00  77.00 -90.00  134
 42  \w    -64.00   7.00   0.50   15.00    --   14.70  -7.00  41.00  142
 43  \w    -93.00   7.00   0.50   15.00    --  -14.00  -7.00  41.00  200
;
_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      0.0488433000
_diffrn_orient_matrix_UB_12      -0.0034778000
_diffrn_orient_matrix_UB_13      -0.0036434000
_diffrn_orient_matrix_UB_21      -0.0037118000
_diffrn_orient_matrix_UB_22      -0.0457454000
_diffrn_orient_matrix_UB_23      0.0029559000
_diffrn_orient_matrix_UB_31      -0.0167258000
_diffrn_orient_matrix_UB_32      -0.0158213000
_diffrn_orient_matrix_UB_33      -0.0448053000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            128234
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         1.927
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.137
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     764
_refine_ls_number_reflns         15398
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0314
_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^)+(0.0300P)^2^+1.8517P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0743
_reflns_number_gt                13082
_reflns_number_total             15398
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01094e2.cif
_cod_data_source_block           9704_2-Se
_cod_depositor_comments
'Adding full bibliography for 1569232--1569239.cif.'
_cod_original_cell_volume        3375.48(4)
_cod_database_code               1569238
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.895
_shelx_estimated_absorpt_t_min   0.727
_shelx_res_checksum              81908
_shelx_hkl_checksum              14787
_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 1.448
_oxdiff_exptl_absorpt_empirical_full_min 0.575