Snap-shots of cluster growth: structure and properties of a Zintl ion with an Fe<sub>3</sub> core, [Fe<sub>3</sub>Sn<sub>18</sub>]<sup>4</sup>.
Li, Zi-Sheng; Chen, Wei-Xing; Morgan, Harry W. T.; Shu, Cong-Cong; McGrady, John E.; Sun, Zhong-Ming; Chemical science 15 (2024) 1018–1026; doi:10.1039/d3sc04709a

data_1570480
_publ_section_title
;
 Snap-shots of cluster growth: structure and properties of a Zintl ion
 with an Fe<sub>3</sub> core, [Fe<sub>3</sub>Sn<sub>18</sub>]<sup>4</sup>.
;
_journal_issue                   3
_journal_name_full               'Chemical science'
_journal_page_first              1018
_journal_page_last               1026
_journal_paper_doi               10.1039/d3sc04709a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'Fe3 Sn18, 4(C18 H36 K N2 O6)'
_chemical_formula_sum            'C72 H144 Fe3 K4 N8 O24 Sn18'
_chemical_formula_weight         3966.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-19
_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.	2023-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.689(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.8596(3)
_cell_length_b                   25.1992(4)
_cell_length_c                   18.7930(5)
_cell_measurement_reflns_used    12326
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      72.7450
_cell_measurement_theta_min      3.6220
_cell_volume                     6666.0(3)
_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      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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    -37.00 -10.00   0.50    2.33    --  -35.00 -82.00 -90.00   54
  2  \w   -103.00 -89.00   0.50    2.33    --  -35.00 -77.00   0.00   28
  3  \w    -54.00  29.00   0.50    2.33    --  -35.00  82.00 -60.00  166
  4  \w   -106.00 -76.00   0.50    2.33    --  -35.00 -77.00 -60.00   60
  5  \w   -110.00 -80.00   0.50    2.33    --  -35.00 -77.00-150.00   60
  6  \w   -109.00 -80.00   0.50    2.33    --  -35.00 -77.00 -90.00   58
  7  \w      2.00  32.00   0.50    2.33    --   43.10  77.00-180.00   60
  8  \w      8.00  43.00   0.50    2.33    --   43.10  77.00-150.00   70
  9  \w     76.00 107.00   0.50    2.33    --   43.10  77.00 150.00   62
 10  \w     72.00 184.00   0.50    8.34    --  104.50  45.00-150.00  224
 11  \w     65.00 191.00   0.50    8.34    --  104.50  45.00-180.00  252
 12  \w     55.00 155.00   0.50    8.34    --  104.50 -30.00   0.00  200
 13  \w     16.00  85.00   0.50    8.34    --  104.50 -61.00 -30.00  138
 14  \w     16.00 126.00   0.50    8.34    --  104.50 -61.00   0.00  220
 15  \w    129.00 161.00   0.50    8.34    --  104.50  77.00 120.00   64
 16  \w    102.00 127.00   0.50    8.34    --  104.50 -82.00 -30.00   50
 17  \w     24.00  49.00   0.50    8.34    --  104.50 -82.00 -30.00   50
;
_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      0.0736136000
_diffrn_orient_matrix_UB_12      0.0389454000
_diffrn_orient_matrix_UB_13      -0.0122470000
_diffrn_orient_matrix_UB_21      -0.0326176000
_diffrn_orient_matrix_UB_22      -0.0142476000
_diffrn_orient_matrix_UB_23      -0.0840998000
_diffrn_orient_matrix_UB_31      -0.0741119000
_diffrn_orient_matrix_UB_32      0.0449670000
_diffrn_orient_matrix_UB_33      -0.0159209000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32123
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        65.999
_diffrn_reflns_theta_max         65.999
_diffrn_reflns_theta_min         3.508
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    30.352
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54972
_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 yellowish green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.976
_exptl_crystal_description       block
_exptl_crystal_F_000             3756
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.094
_refine_diff_density_min         -1.028
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         11573
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0544P)^2^+37.0479P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1116
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9781
_reflns_number_total             11573
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc04709a1.cif
_cod_data_source_block           cwx
_cod_depositor_comments          'Adding full bibliography for 1570480.cif.'
_cod_database_code               1570480
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.171
_shelx_estimated_absorpt_t_min   0.073
_reflns_odcompleteness_completeness 99.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.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)
;
_shelx_res_checksum              74020
_shelx_fab_checksum              71504
_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 1.589
_oxdiff_exptl_absorpt_empirical_full_min 0.686