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_1571070
_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         'Fe4 Sn18, 4(C18 H36 K N2 O6), 4(C5 H5 N)'
_chemical_formula_sum            'C92 H164 Fe4 K4 N12 O24 Sn18'
_chemical_formula_weight         4338.56
_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
_audit_creation_date             2022-09-10
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2022-09-10 deposited with the CCDC.	2024-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.6780(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.30740(10)
_cell_length_b                   27.4645(2)
_cell_length_c                   18.80560(10)
_cell_measurement_reflns_used    17015
_cell_measurement_temperature    100.01(11)
_cell_measurement_theta_max      75.5710
_cell_measurement_theta_min      4.0440
_cell_volume                     6913.54(9)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(11)
_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      8.00  39.00   0.50    1.00    --    0.00  82.00  90.00   62
  2  \w    -35.00   3.00   0.50    1.00    --    0.00  82.00  90.00   76
  3  \w    -36.00  39.00   0.50    1.00    --    0.00  82.00-120.00  150
  4  \w    -12.00  14.00   0.50    1.00    --    0.00  82.00 -60.00   52
  5  \w    -34.00  33.00   0.50    1.00    --    0.00  82.00   0.00  134
  6  \w     21.00 131.00   0.50    2.50    --  101.30 -77.00  60.00  220
  7  \w     13.00 129.00   0.50    2.50    --  101.30 -57.00  60.00  232
  8  \w     99.00 129.00   0.50    2.50    --  101.30  57.00-180.00   60
  9  \w     78.00 175.00   0.50    2.50    --  101.30  57.00 -60.00  194
 10  \w     83.00 156.00   0.50    2.50    --  101.30  82.00-180.00  146
 11  \w     83.00 172.00   0.50    2.50    --  101.30  38.00 -90.00  178
;
_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      -0.0982903000
_diffrn_orient_matrix_UB_12      0.0211951000
_diffrn_orient_matrix_UB_13      -0.0557192000
_diffrn_orient_matrix_UB_21      -0.0525897000
_diffrn_orient_matrix_UB_22      -0.0490222000
_diffrn_orient_matrix_UB_23      -0.0005118000
_diffrn_orient_matrix_UB_31      -0.0288732000
_diffrn_orient_matrix_UB_32      0.0170957000
_diffrn_orient_matrix_UB_33      0.0674933000
_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  0.0450
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34230
_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         3.673
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    30.148
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64471
_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    2.084
_exptl_crystal_description       block
_exptl_crystal_F_000             4144
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.954
_refine_diff_density_min         -1.287
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     749
_refine_ls_number_reflns         12283
_refine_ls_number_restraints     2094
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0506P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0921
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10383
_reflns_number_total             12283
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc00165f2.cif
_cod_data_source_block           fe4sn18
_cod_depositor_comments
'Adding full bibliography for 1571069--1571071.cif.'
_cod_database_code               1571070
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.172
_shelx_estimated_absorpt_t_min   0.111
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Sn1A \\sim Sn5A \\sim Sn6A: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 3.8A
All non-hydrogen atoms have similar U: within 3.8A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 3.8A
Uanis(Sn1A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Sn1A) \\sim Ueq, Uanis(Sn2A) \\sim Ueq, Uanis(Sn6A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(Sn2A)=Sof(Sn1A)=Sof(Sn6A)=Sof(Sn7A)=Sof(Sn9A)=Sof(Sn5A)=1-FVAR(1)
 Sof(Sn1)=Sof(Sn2)=Sof(Sn5)=Sof(Sn6)=Sof(Sn7)=Sof(Sn9)=FVAR(1)
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:
 C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43),
 C44(H44), C45(H45), C46(H46)
;
_shelx_res_checksum              77905
_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 1.434
_oxdiff_exptl_absorpt_empirical_full_min 0.566