Aggregate assembly of ferrocene functionalized indium-oxo clusters.
Zhang, Rong; Lan, Jiajing; Wang, Fei; Chen, Shumei; Zhang, Jian; Chemical science 15 (2024) 726–735; doi:10.1039/d3sc05824g

data_1570491
_publ_section_title
;
 Aggregate assembly of ferrocene functionalized indium-oxo clusters.
;
_journal_issue                   2
_journal_name_full               'Chemical science'
_journal_page_first              726
_journal_page_last               735
_journal_paper_doi               10.1039/d3sc05824g
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C88 H83.369 Fe6 In7 N6 O28'
_chemical_formula_sum            'C88 H84 Fe6 In7 N6 O28'
_chemical_formula_weight         2812.45
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-09
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-07-14 deposited with the CCDC.	2023-11-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   25.3175(3)
_cell_length_b                   25.3175(3)
_cell_length_c                   29.8382(4)
_cell_measurement_reflns_used    41789
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      60.4960
_cell_measurement_theta_min      2.1650
_cell_volume                     16563.2(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (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 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.979
_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     64.00 147.00   0.50    0.25    --   72.85  36.00 171.00  166
  2  \w    118.00 147.00   0.50    0.25    --   72.85  38.00  90.00   58
  3  \w     74.00  99.00   0.50    0.25    --   72.85  38.00  90.00   50
  4  \w      1.00  28.00   0.50    0.25    --   72.85 -99.00   0.00   54
  5  \w     27.00  98.00   0.50    0.25    --   72.85-125.00   0.00  142
  6  \w     78.00 105.00   0.50    0.25    --   72.85 -99.00   0.00   54
  7  \w      8.00  66.00   0.50    0.25    --   72.85 -77.00   0.00  116
  8  \w     25.00  70.00   0.50    0.25    --   72.85 -36.00  14.00   90
  9  \w     71.00  97.00   0.50    0.25    --   72.85 -77.00   0.00   52
 10  \w     92.00 117.00   0.50    0.25    --   72.85 109.00-103.00   50
 11  \w     97.00 146.00   0.50    0.25    --   72.85 125.00   0.00   98
 12  \w     85.00 128.00   0.50    0.25    --   72.85 125.00  30.00   86
 13  \w     82.00 118.00   0.50    0.25    --   72.85  91.00   1.00   72
 14  \w    -30.00  -4.00   0.50    0.06    --   -1.09  91.00   1.00   52
 15  \w    -12.00  13.00   0.50    0.06    --   -1.09 -77.00-180.00   50
 16  \w    -67.00 -21.00   0.50    0.06    --   -1.09 -77.00-180.00   92
 17  \w    -73.00   7.00   0.50    0.06    --   -1.09 -57.00 -90.00  160
 18  \w   -106.00 -29.00   0.50    0.25    --  -75.04 109.00-103.00  154
 19  \w    -99.00 -21.00   0.50    0.25    --  -75.04  77.00-150.00  156
 20  \w    -88.00 -41.00   0.50    0.25    --  -75.04  57.00-180.00   94
 21  \w    -36.00 -10.00   0.50    0.25    --  -75.04  57.00-180.00   52
 22  \w    -36.00  -2.00   0.50    0.25    --  -75.04  38.00  60.00   68
 23  \w    -65.00 -39.00   0.50    0.25    --  -75.04  38.00  60.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0248689000
_diffrn_orient_matrix_UB_12      -0.0274658000
_diffrn_orient_matrix_UB_13      -0.0231478000
_diffrn_orient_matrix_UB_21      0.0386820000
_diffrn_orient_matrix_UB_22      0.0101289000
_diffrn_orient_matrix_UB_23      0.0338567000
_diffrn_orient_matrix_UB_31      -0.0402049000
_diffrn_orient_matrix_UB_32      -0.0535982000
_diffrn_orient_matrix_UB_33      0.0182177000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Ga K\a'
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            55496
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.509
_diffrn_reflns_theta_min         3.735
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    12.430
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45287
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_description       block
_exptl_crystal_F_000             8262
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         3.786
_refine_diff_density_min         -2.722
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         8256
_refine_ls_number_restraints     306
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0759P)^2^+315.7832P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1297
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7721
_reflns_number_total             8256
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05824g2.cif
_cod_data_source_block           zr_auto
_cod_depositor_comments
'Adding full bibliography for 1570485--1570493.cif.'
_cod_original_cell_volume        16563.2(5)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               1570491
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         FeInCHON
_shelx_estimated_absorpt_t_max   0.342
_shelx_estimated_absorpt_t_min   0.342
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N2-C28
 1.45 with sigma of 0.02
 C26-N1
 1.45 with sigma of 0.02
 C29-N1 \\sim C29A-N1
 with sigma of 0.02
 N1-C26A \\sim N1A-C26A
 with sigma of 0.02
 N2-C28 \\sim N2-C28A
 with sigma of 0.02
 C27-C28 \\sim C27-C28A
 with sigma of 0.02
 N2-C25 \\sim N2A-C25
 with sigma of 0.02
 C25-C26 \\sim C25-C26A
 with sigma of 0.02
 N1-C26 \\sim N1-C26A
 with sigma of 0.02
 In3-N2 \\sim In3-N2A
 with sigma of 0.02
 N2-C28 \\sim N2A-C28
 with sigma of 0.02
 C27-N1 \\sim C27-N1A
 with sigma of 0.02
 N2-C28A \\sim N2A-C28A
 with sigma of 0.02
 C29-N1 \\sim C29-N1A
 with sigma of 0.02
 N1-C26 \\sim N1A-C26
 with sigma of 0.02
 C29-N1A \\sim C29A-N1A
 with sigma of 0.02
 C25-C26 \\sim C25A-C26
 with sigma of 0.02
 N2-C25 \\sim N2-C25A
 with sigma of 0.02
 C25-C26A \\sim C25A-C26A
 with sigma of 0.02
 C25-N2A \\sim C25A-N2A
 with sigma of 0.02
3. Rigid bond restraints
 N2, C27, C25, C29, N1, C28, C26, C28A, C26A, N1A, N2A, C29A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N2, C27, C25, C29, N1, C28, C26, C28A, C26A, N1A, N2A, C29A, C25A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C21, C20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N2 \\sim C27 \\sim C25 \\sim C29 \\sim N1 \\sim C28 \\sim C26 \\sim C28A \\sim
C26A \\sim N1A \\sim N2A \\sim C29A: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1.7A
N2 \\sim C27 \\sim C25 \\sim C29 \\sim N1 \\sim C28 \\sim C26 \\sim C28A \\sim
C26A \\sim N1A \\sim N2A \\sim C29A \\sim C25A: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 1.7A
C21 \\sim C20: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
Uanis(N2) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C26) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N2) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C26) \\sim Ueq,
Uanis(C28A) \\sim Ueq, Uanis(C26A) \\sim Ueq, Uanis(N1A) \\sim Ueq, Uanis(N2A)
\\sim Ueq, Uanis(C29A) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(N2) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C26) \\sim Ueq,
Uanis(C28A) \\sim Ueq, Uanis(C26A) \\sim Ueq, Uanis(N1A) \\sim Ueq, Uanis(N2A)
\\sim Ueq, Uanis(C29A) \\sim Ueq, Uanis(C25A) \\sim Ueq: with sigma of 0.001
and sigma for terminal atoms of 0.002
Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(H27C)=Sof(H27D)=Sof(C28A)=Sof(H28C)=Sof(H28D)=1-FVAR(1)
 Sof(C28)=Sof(H28A)=Sof(H28B)=FVAR(1)
 Sof(C26A)=Sof(H26C)=Sof(H26D)=1-FVAR(2)
 Sof(C26)=Sof(H26A)=Sof(H26B)=FVAR(2)
 Sof(N1A)=1-FVAR(3)
 Sof(H27A)=Sof(H27B)=Sof(N1)=FVAR(3)
 Sof(N2A)=1-FVAR(4)
 Sof(N2)=FVAR(4)
 Sof(C29A)=Sof(H29D)=Sof(H29E)=Sof(H29F)=1-FVAR(5)
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=FVAR(5)
 Sof(C25A)=Sof(H25C)=Sof(H25D)=1-FVAR(6)
 Sof(C25)=Sof(H25A)=Sof(H25B)=FVAR(6)
 Fixed Sof: H30A(0.33333) H30B(0.33333) H30C(0.33333)
6.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C27(H27C,H27D), C25(H25A,H25B), C28(H28A,H28B), C26(H26A,
 H26B), C28A(H28C,H28D), C26A(H26C,H26D), C25A(H25C,H25D)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C3(H3), C7(H7), C10(H10), C8(H8), C14(H14), C19(H19),
 C9(H9), C22(H22), C17(H17), C15(H15), C21(H21), C20(H20), C16(H16)
6.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C29(H29A,H29B,H29C), C29A(H29D,H29E,H29F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              69602
_shelx_fab_checksum              5992
_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 2.589
_oxdiff_exptl_absorpt_empirical_full_min 0.565