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_1569232
_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 O P, C5 H12'
_chemical_formula_sum            'C52 H68 Fe N3 O P'
_chemical_formula_weight         837.91
_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             2021-06-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2023-02-16 deposited with the CCDC.	2023-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.3550(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9812(2)
_cell_length_b                   16.29860(10)
_cell_length_c                   18.9525(2)
_cell_measurement_reflns_used    36061
_cell_measurement_temperature    100
_cell_measurement_theta_max      74.2130
_cell_measurement_theta_min      3.0820
_cell_volume                     4597.64(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2012)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (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-6000HE
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_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    -11.00  21.00   0.50    1.50    --  -46.92  40.00  68.00   64
  2  \w   -119.00 -68.00   0.50    1.50    --  -46.92 -40.00 -85.00  102
  3  \w     -8.00  20.00   0.50    1.50    --   46.92 -40.00 -85.00   56
  4  \w     36.00 118.00   0.50    1.50    --   46.92  40.00  68.00  164
  5  \w    -40.00 -14.00   0.50    5.50    --  -86.25  40.00  68.00   52
  6  \w   -140.00-115.00   0.50    5.50    --  -86.25 -40.00 -85.00   50
  7  \w     95.00 176.00   0.50    5.50    --  107.75  40.00  68.00  162
  8  \w    -61.00 -35.00   0.50    1.50    --  -46.92  57.00 -90.00   52
  9  \w    -30.00  14.00   0.50    1.50    --  -46.92  19.00  60.00   88
 10  \w    -27.00   0.00   0.50    1.50    --  -46.92  57.00 -90.00   54
 11  \w    -68.00  26.00   0.50    1.50    --  -46.92  77.00 -30.00  188
 12  \w    -15.00  23.00   0.50    1.50    --   46.92 -19.00-120.00   76
 13  \w    -26.00  21.00   0.50    1.50    --   46.92 -19.00 -60.00   94
 14  \w    -26.00  23.00   0.50    1.50    --   46.92 -19.00-180.00   98
 15  \w    -25.00  22.00   0.50    1.50    --   46.92 -19.00 120.00   94
 16  \w    -37.00 -12.00   0.50    5.50    --  -86.25  30.00-180.00   50
 17  \w    -38.00 -12.00   0.50    5.50    --  -86.25  30.00-150.00   52
 18  \w   -108.00 -24.00   0.50    5.50    --  -86.25  77.00-120.00  168
 19  \w    -53.00 -15.00   0.50    5.50    --  -86.25  45.00-120.00   76
 20  \w    138.00 168.00   0.50    5.50    --  107.75  30.00 -60.00   60
 21  \w     95.00 134.00   0.50    5.50    --  107.75  30.00 -60.00   78
 22  \w     35.00  67.00   0.50    5.50    --  107.75 -61.00 150.00   64
 23  \w     35.00  91.00   0.50    5.50    --  107.75 -77.00 150.00  112
 24  \w     36.00  68.00   0.50    5.50    --  107.75 -61.00  90.00   64
 25  \w    114.00 159.00   0.50    5.50    --  107.75  30.00 150.00   90
 26  \w     37.00  68.00   0.50    5.50    --  107.75 -61.00 -60.00   62
 27  \w     48.00  78.00   0.50    5.50    --  107.75 -80.00  54.04   60
 28  \w     97.00 177.00   0.50    5.50    --  107.75  15.00-120.00  160
 29  \w     42.00  67.00   0.50    5.50    --  107.75 -61.00  60.00   50
 30  \w     81.00 108.00   0.50    5.50    --  107.75 -80.00  54.04   54
 31  \w     35.00  69.00   0.50    5.50    --  107.75 -79.00-158.38   68
 32  \w    110.00 175.00   0.50    5.50    --  107.75  45.00 120.00  130
 33  \w    101.00 149.00   0.50    5.50    --  107.75  15.00  30.00   96
 34  \w     99.00 124.00   0.50    5.50    --  107.75 -80.00 -98.40   50
 35  \w     72.00 129.00   0.50    5.50    --  107.75 -80.00 114.31  114
 36  \w     86.00 129.00   0.50    5.50    --  107.75 -79.00 -23.13   86
 37  \w     44.00  81.00   0.50    5.50    --  107.75 -80.00 -76.40   74
 38  \w     40.00  75.00   0.50    5.50    --  107.75 -79.00 -23.13   70
 39  \w    106.00 169.00   0.50    5.50    --  107.75  15.00-150.00  126
 40  \w     35.00  68.00   0.50    5.50    --  107.75 -61.00 -90.00   66
 41  \w    110.00 171.00   0.50    5.50    --  107.75  59.00  86.65  122
 42  \w     88.00 113.00   0.50    5.50    --  107.75 -80.00  12.64   50
 43  \w     37.00  72.00   0.50    5.50    --  107.75 -64.00-123.43   70
 44  \w     40.00  68.00   0.50    5.50    --  107.75 -61.00-150.00   56
 45  \w     61.00 131.00   0.50    5.50    --  107.75 -80.00-120.76  140
 46  \w     35.00  85.00   0.50    5.50    --  107.75 -80.00  12.64  100
 47  \w     92.00 122.00   0.50    5.50    --  107.75 -80.00 -76.40   60
 48  \w    146.00 171.00   0.50    5.50    --  107.75  61.00  30.00   50
 49  \w    101.00 132.00   0.50    5.50    --  107.75 -80.00 162.99   62
 50  \w    102.00 147.00   0.50    5.50    --  107.75  61.00 -19.60   90
 51  \w    101.00 144.00   0.50    5.50    --  107.75  61.00  30.00   86
 52  \w     47.00  88.00   0.50    5.50    --  107.75 -77.00  60.00   82
 53  \w     38.00  64.00   0.50    5.50    --  107.75 -61.00   0.00   52
 54  \w     68.00 105.00   0.50    5.50    --  107.75 -78.00 -71.06   74
 55  \w    108.00 134.00   0.50    5.50    --  107.75  45.00 -90.00   52
 56  \w     36.00  82.00   0.50    5.50    --  107.75 -77.00-150.00   92
 57  \w     74.00 129.00   0.50    5.50    --  107.75 -79.00-158.38  110
 58  \w     37.00  71.00   0.50    5.50    --  107.75 -79.00 142.95   68
 59  \w     79.00 108.00   0.50    5.50    --  107.75 -79.00 142.95   58
 60  \w     36.00  92.00   0.50    5.50    --  107.75 -77.00  90.00  112
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-S'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0638595000
_diffrn_orient_matrix_UB_12      0.0006341000
_diffrn_orient_matrix_UB_13      0.0443819000
_diffrn_orient_matrix_UB_21      -0.0062273000
_diffrn_orient_matrix_UB_22      0.0941751000
_diffrn_orient_matrix_UB_23      -0.0064521000
_diffrn_orient_matrix_UB_31      -0.0812363000
_diffrn_orient_matrix_UB_32      -0.0077379000
_diffrn_orient_matrix_UB_33      -0.0748827000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            73300
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.491
_diffrn_reflns_theta_min         3.110
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.256
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66320
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_description       plate
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         9320
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0491P)^2^+2.0217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.0953
_reflns_number_gt                8527
_reflns_number_total             9320
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01094e2.cif
_cod_data_source_block           9758_1-OPh
_cod_depositor_comments
'Adding full bibliography for 1569232--1569239.cif.'
_cod_database_code               1569232
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.03
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_shelx_res_checksum              47103
_shelx_hkl_checksum              47227
_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 1.732
_oxdiff_exptl_absorpt_empirical_full_min 0.594