Fe-Fe bonding in the rhombic Fe<sub>4</sub> cores of the Zintl clusters [Fe<sub>4</sub>E<sub>18</sub>]<sup>4-</sup> (E = Sn and Pb).
Chen, Wei-Xing; Li, Zi-Sheng; Morgan, Harry W. T.; Shu, Cong-Cong; Sun, Zhong-Ming; McGrady, John E.; Chemical science 15 (2024) 4981–4988; doi:10.1039/d4sc00165f

data_1571069
_publ_section_title
;
 Fe-Fe bonding in the rhombic Fe<sub>4</sub> cores of the Zintl clusters
 [Fe<sub>4</sub>E<sub>18</sub>]<sup>4-</sup> (E = Sn and Pb).
;
_journal_issue                   13
_journal_name_full               'Chemical science'
_journal_page_first              4981
_journal_page_last               4988
_journal_paper_doi               10.1039/d4sc00165f
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'Fe2 Pb9, 2(C18 H36 K N2 O6), 2(C5 H5 N)'
_chemical_formula_sum            'C46 H82 Fe2 K2 N6 O12 Pb9'
_chemical_formula_weight         2965.78
_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             2021-04-25
_audit_creation_method
;
Olex2 1.3-beta
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-05 deposited with the CCDC.	2024-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.7180(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.32980(10)
_cell_length_b                   27.6726(2)
_cell_length_c                   18.9178(2)
_cell_measurement_reflns_used    23217
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.9690
_cell_measurement_theta_min      4.0280
_cell_volume                     7016.60(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.999
_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    -31.00  -6.00   0.50    1.95    --    0.00  82.00-150.00   50
  2  \w    -28.00  34.00   0.50    1.95    --    0.00 -82.00-180.00  124
  3  \w    -15.00  38.00   0.50    1.95    --    0.00  82.00 150.00  106
  4  \w    -12.00  13.00   0.50    1.95    --    0.00  38.00-150.00   50
  5  \w    -33.00  33.00   0.50    1.95    --    0.00  82.00  90.00  132
  6  \w     80.00 186.00   0.50    7.81    --  101.30  19.00-150.00  212
  7  \w     13.00  92.00   0.50    7.81    --  101.30 -77.00 -90.00  158
  8  \w     22.00  74.00   0.50    7.81    --  101.30 -82.00-150.00  104
  9  \w     14.00 125.00   0.50    7.81    --  101.30 -38.00  30.00  222
 10  \w    103.00 129.00   0.50    7.81    --  101.30 -82.00-150.00   52
 11  \w     26.00 127.00   0.50    7.81    --  101.30 -82.00 -60.00  202
 12  \w     34.00 122.00   0.50    7.81    --  101.30 -57.00 -60.00  176
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0149611000
_diffrn_orient_matrix_UB_12      0.0498958000
_diffrn_orient_matrix_UB_13      -0.0386680000
_diffrn_orient_matrix_UB_21      0.0154688000
_diffrn_orient_matrix_UB_22      -0.0227391000
_diffrn_orient_matrix_UB_23      -0.0694151000
_diffrn_orient_matrix_UB_31      -0.1128019000
_diffrn_orient_matrix_UB_32      -0.0096795000
_diffrn_orient_matrix_UB_33      -0.0356090000
_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  0.0768
_diffrn_reflns_av_unetI/netI     0.0608
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35931
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.998
_diffrn_reflns_theta_min         3.664
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    45.713
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.02822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dull black'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.808
_exptl_crystal_description       plate
_exptl_crystal_F_000             5296
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.432
_refine_diff_density_min         -2.765
_refine_diff_density_rms         0.431
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         12483
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0597
_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^)+(0.1215P)^2^+22.1855P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1603
_refine_ls_wR_factor_ref         0.1658
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10758
_reflns_number_total             12483
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc00165f2.cif
_cod_data_source_block           scc2
_cod_depositor_comments
'Adding full bibliography for 1571069--1571071.cif.'
_cod_database_code               1571069
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.462
_shelx_estimated_absorpt_t_min   0.462
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00U(H00A,H00B), C00V(H00G,H00H), C00W(H00I,H00J), C00X(H00C,H00D), C00Z(H00E,
 H00F), C010(H01A,H01B), C011(H1,H), C013(H2,HA), C015(H3,HB), C017(H4,HC),
 C018(H5,HD), C019(H6,HE), C01A(H01C,H01D), C01B(H01E,H01F), C01C(H01G,H01H),
 C01D(H7,HF), C01E(H01I,H01J), C01F(H01K,H01L), C01G(H8,HG), C01J(H01M,H01N),
 C01K(H9,HH), C01L(H10,HI), C01M(H01O,H01P), C01N(H11,HJ), C01O(H12,HK),
 C01P(H01Q,H01R), C01Q(H01S,H01T), C01R(H01U,H01V), C01S(H01W,H01X), C01T(H13,
 HL), C01U(H01Y,HM), C01V(H01Z,HN), C01X(H14,HO), C01Y(H01,HP), C8(H8A,H8B),
 C12(H12A,H12B)
2.b Aromatic/amide H refined with riding coordinates:
 C00Y(H00Y), C016(H016), C01H(H15), C01I(H16), C01W(H17), C11(H11A), C1(H1A),
 C2(H2A), C4(H4A), C5(H5A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              54813
_shelx_fab_checksum              26983
_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 11.697
_oxdiff_exptl_absorpt_empirical_full_min 0.300