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_1569236
_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         'C47 H56 Fe N3 P S, C7 H8'
_chemical_formula_sum            'C54 H64 Fe N3 P S'
_chemical_formula_weight         873.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-02-16 deposited with the CCDC.	2023-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.2200(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.82150(10)
_cell_length_b                   24.9832(3)
_cell_length_c                   19.1363(3)
_cell_measurement_reflns_used    80807
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      1.95
_cell_volume                     4605.78(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_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    -82.00   3.00   0.50   45.00    --  -14.00 -37.00 -90.00  170
  2  \w    -88.00   5.00   0.50   45.00    --  -14.00 -19.00 150.00  186
  3  \w    -22.00  15.00   0.50   45.00    --  -14.00 -80.00  91.52   74
  4  \w    -22.00  15.00   0.50   45.00    --  -14.00 -80.00-153.67   74
  5  \w    -22.00  15.00   0.50   45.00    --  -14.00 -80.00  64.57   74
  6  \w    -22.00  15.00   0.50   45.00    --  -14.00 -80.00 156.22   74
  7  \w    -82.00   3.00   0.50   45.00    --  -14.00 -37.00-180.00  170
  8  \w    -29.00   8.00   0.50   45.00    --  -14.00 -57.00  60.00   74
  9  \w    -22.00  11.00   0.50   45.00    --  -14.00 -80.00 -59.09   66
 10  \w    -20.00   5.00   0.50   45.00    --  -14.00 -80.00 -98.58   50
 11  \w    -26.00   3.00   0.50   45.00    --  -14.00  37.00  90.00   58
 12  \w      7.00  54.00   0.50   45.00    --  -14.00  37.00  90.00   94
 13  \w    -22.00  14.00   0.50   45.00    --  -14.00 -79.00 -19.17   72
 14  \w    -21.00   5.00   0.50   45.00    --  -14.00 -80.00-126.15   52
 15  \w    -22.00   5.00   0.50   45.00    --  -14.00 -80.00  31.62   54
 16  \w    -22.00   3.00   0.50   45.00    --  -14.00 -80.00 -62.97   50
 17  \w    -58.00   3.00   0.50   45.00    --   14.70 -19.00 -60.00  122
 18  \w      3.00  29.00   0.50   45.00    --   14.70  37.00-120.00   52
 19  \w     -7.00  49.00   0.50   45.00    --   14.70  57.00 -60.00  112
 20  \w    -58.00   3.00   0.50   45.00    --   14.70 -19.00  30.00  122
 21  \w    -27.00  38.00   0.50   45.00    --   14.70 -75.00  62.61  130
 22  \w    -51.00  19.00   0.50   45.00    --   14.70 -37.00 150.00  140
 23  \w     -7.00  57.00   0.50   45.00    --   14.70  57.00-120.00  128
 24  \w     -7.00  19.00   0.50   45.00    --   14.70  79.00 152.53   52
 25  \w    -53.00 -17.00   0.50   45.00    --   14.70 -19.00-180.00   72
 26  \w     -8.00  23.00   0.50   45.00    --   14.70  57.00  60.00   62
 27  \w     33.00  83.00   0.50   45.00    --   14.70  37.00-120.00  100
 28  \w     -7.00  25.00   0.50   45.00    --   14.70  77.00 -30.00   64
 29  \w    -46.00  21.00   0.50   45.00    --   14.70 -37.00 -90.00  134
 30  \w     -4.00  22.00   0.50   45.00    --   14.70 -76.00   6.01   52
 31  \w    -23.00  34.00   0.50   45.00    --   14.70 -76.00  24.41  114
 32  \w    -45.00   3.00   0.50   45.00    --   14.70 -19.00 -90.00   96
 33  \w      5.00  37.00   0.50   45.00    --   14.70 -57.00 -90.00   64
 34  \w    -53.00  -5.00   0.50   45.00    --   14.70 -57.00 -90.00   96
 35  \w    -13.00  25.00   0.50   45.00    --   14.70  77.00 -90.00   76
 36  \w    -59.00 -20.00   0.50   45.00    --   14.70 -19.00 120.00   78
 37  \w    -22.00  25.00   0.50   45.00    --   14.70 -79.00 141.23   94
 38  \w     -9.00  20.00   0.50   45.00    --   14.70  80.00  36.07   58
 39  \w     -6.00  29.00   0.50   45.00    --   14.70  57.00 120.00   70
 40  \w     34.00  59.00   0.50   45.00    --   14.70  57.00 120.00   50
 41  \w    -14.00  21.00   0.50   45.00    --   14.70  80.00-141.12   70
 42  \w    -14.00  14.00   0.50   45.00    --   14.70  80.00 131.65   56
 43  \w     -6.00  20.00   0.50   45.00    --   14.70  77.00-150.00   52
 44  \w    -39.00   3.00   0.50   45.00    --   14.70 -19.00 -30.00   84
 45  \w    -37.00   5.00   0.50   45.00    --   14.70 -19.00  60.00   84
;
_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      0.0171817000
_diffrn_orient_matrix_UB_12      -0.0248876000
_diffrn_orient_matrix_UB_13      -0.0138524000
_diffrn_orient_matrix_UB_21      -0.0712629000
_diffrn_orient_matrix_UB_22      -0.0047888000
_diffrn_orient_matrix_UB_23      -0.0140510000
_diffrn_orient_matrix_UB_31      0.0068815000
_diffrn_orient_matrix_UB_32      0.0127937000
_diffrn_orient_matrix_UB_33      -0.0322284000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            145777
_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         27.484
_diffrn_reflns_theta_min         1.958
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.447
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3360
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       needle
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.638
_refine_diff_density_min         -1.275
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         10564
_refine_ls_number_restraints     204
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0553
_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^)+(0.0790P)^2^+8.4907P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1529
_refine_ls_wR_factor_ref         0.1590
_reflns_number_gt                8949
_reflns_number_total             10564
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01094e2.cif
_cod_data_source_block           9799_1-S-Ph
_cod_depositor_comments
'Adding full bibliography for 1569232--1569239.cif.'
_cod_database_code               1569236
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              3470
_shelx_hkl_checksum              77166
_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 1.875
_oxdiff_exptl_absorpt_empirical_full_min 0.462