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_1571071
_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 Sn9, 2(C18 H36 K N2 O6), 2(C3 H7 N O)'
_chemical_formula_sum            'C42 H86 Fe2 K2 N6 O14 Sn9'
_chemical_formula_weight         2157.27
_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             2021-12-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-05-03 deposited with the CCDC.	2024-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                107.7610(14)
_cell_angle_beta                 97.0389(12)
_cell_angle_gamma                112.8799(15)
_cell_formula_units_Z            2
_cell_length_a                   15.7369(2)
_cell_length_b                   15.9735(3)
_cell_length_c                   16.6129(2)
_cell_measurement_reflns_used    18896
_cell_measurement_temperature    129.99(10)
_cell_measurement_theta_max      75.7730
_cell_measurement_theta_min      4.1590
_cell_volume                     3522.99(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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      129.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -19.00  30.00   0.50    0.50    --    0.00  82.00  90.00   98
  2  \w    -21.00  31.00   0.50    0.50    --    0.00  77.00 -60.00  104
  3  \w    -38.00  -8.00   0.50    0.50    --    0.00 -82.00   0.00   60
  4  \w    -32.00  40.00   0.50    0.50    --    0.00  77.00 150.00  144
  5  \w    -28.00  44.00   0.50    0.50    --    0.00  77.00   0.00  144
  6  \w    -24.00  32.00   0.50    0.50    --    0.00  82.00-150.00  112
  7  \w     65.00 185.00   0.50    0.88    --  101.30  19.00 -90.00  240
  8  \w     13.00 129.00   0.50    0.88    --  101.30 -57.00 -90.00  232
  9  \w     40.00 138.00   0.50    0.88    --  101.30 -82.00 -90.00  196
 10  \w     13.00 138.00   0.50    0.88    --  101.30 -82.00 120.00  250
 11  \w    109.00 188.00   0.50    0.88    --  101.30  19.00 150.00  158
 12  \w     75.00 133.00   0.50    0.88    --  101.30 -82.00-150.00  116
 13  \w     99.00 138.00   0.50    0.88    --  101.30 -82.00 -60.00   78
 14  \w     48.00  74.00   0.50    0.88    --  101.30 -77.00  90.00   52
 15  \w     83.00 109.00   0.50    0.88    --  101.30 -82.00  60.00   52
 16  \w     37.00 103.00   0.50    0.88    --  101.30 -82.00  30.00  132
 17  \w     50.00  75.00   0.50    0.88    --  101.30 -82.00  60.00   50
 18  \w     13.00 121.00   0.50    0.88    --  101.30 -57.00 120.00  216
 19  \w     66.00 191.00   0.50    0.88    --  101.30  19.00-150.00  250
 20  \w     15.00  66.00   0.50    0.88    --  101.30 -38.00  60.00  102
;
_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      0.0681708000
_diffrn_orient_matrix_UB_12      0.0563974000
_diffrn_orient_matrix_UB_13      0.0938076000
_diffrn_orient_matrix_UB_21      0.0324657000
_diffrn_orient_matrix_UB_22      0.0970384000
_diffrn_orient_matrix_UB_23      -0.0148666000
_diffrn_orient_matrix_UB_31      -0.0806927000
_diffrn_orient_matrix_UB_32      0.0166221000
_diffrn_orient_matrix_UB_33      0.0351500000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            34014
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        66.999
_diffrn_reflns_theta_max         66.999
_diffrn_reflns_theta_min         4.190
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    29.596
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.08031
_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            'metallic dark brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.034
_exptl_crystal_description       needle
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         3.488
_refine_diff_density_min         -1.568
_refine_diff_density_rms         0.234
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     680
_refine_ls_number_reflns         12507
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0518
_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^)+(0.0816P)^2^+22.6837P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1385
_refine_ls_wR_factor_ref         0.1423
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11070
_reflns_number_total             12507
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc00165f2.cif
_cod_data_source_block           exp_1690
_cod_depositor_comments
'Adding full bibliography for 1571069--1571071.cif.'
_cod_original_cell_volume        3522.99(10)
_cod_database_code               1571071
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.231
_shelx_estimated_absorpt_t_min   0.095
_reflns_odcompleteness_completeness 99.72
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C27-C28
 1.53 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O13 \\sim C40 \\sim C41: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(O10) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B),
  C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,
 H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
 C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
  C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,
 H35B), C36(H36A,H36B)
4.b Aromatic/amide H refined with riding coordinates:
 C39(H39), C42(H42)
4.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C41(H41A,H41B,
 H41C)
;
_shelx_res_checksum              24286
_shelx_fab_checksum              54652
_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 6.122
_oxdiff_exptl_absorpt_empirical_full_min 0.627