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_1570487
_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         'C106 H86 Fe6 In13 O52'
_chemical_formula_sum            'C106 H86 Fe6 In13 O52'
_chemical_formula_weight         4019.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-11
_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                 103.7827(15)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.2041(3)
_cell_length_b                   25.0454(3)
_cell_length_c                   13.8544(2)
_cell_measurement_reflns_used    16011
_cell_measurement_temperature    179.97(10)
_cell_measurement_theta_max      60.3270
_cell_measurement_theta_min      2.8480
_cell_volume                     7145.74(17)
_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      179.97(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.963
_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     60.00 140.00   0.50    0.35    --   72.28  57.00  30.00  160
  2  \w     79.00 136.00   0.50    0.35    --   72.28 125.00 120.00  114
  3  \w     84.00 139.00   0.50    0.35    --   72.28 118.00  35.00  110
  4  \w     68.00 103.00   0.50    0.35    --   72.28 159.00-171.00   70
  5  \w     -7.00  66.00   0.50    0.07    --   -1.25  38.00   0.00  146
  6  \w     54.00  80.00   0.50    0.35    --   72.28-118.00 -50.00   52
  7  \w     33.00  70.00   0.50    0.35    --   72.28 -38.00 -30.00   74
  8  \w     32.00  71.00   0.50    0.07    --   -1.25  57.00 -90.00   78
  9  \w    -84.00 -47.00   0.50    0.35    --  -74.78  57.00  60.00   74
 10  \w   -109.00 -40.00   0.50    0.35    --  -74.78 118.00  35.00  138
 11  \w   -105.00 -23.00   0.50    0.35    --  -74.78 125.00 150.00  164
 12  \w   -113.00 -79.00   0.50    0.35    --  -74.78 159.00-171.00   68
 13  \w   -142.00 -94.00   0.50    0.35    --  -74.78 -99.00  60.00   96
 14  \w   -126.00 -88.00   0.50    0.35    --  -74.78-118.00 -50.00   76
 15  \w   -147.00 -80.00   0.50    0.35    --  -74.78-125.00-180.00  134
;
_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      0.0115058000
_diffrn_orient_matrix_UB_12      -0.0524933000
_diffrn_orient_matrix_UB_13      0.0112711000
_diffrn_orient_matrix_UB_21      0.0585804000
_diffrn_orient_matrix_UB_22      0.0070154000
_diffrn_orient_matrix_UB_23      -0.0186259000
_diffrn_orient_matrix_UB_31      0.0257737000
_diffrn_orient_matrix_UB_32      0.0074345000
_diffrn_orient_matrix_UB_33      0.0971086000
_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  0.0389
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            28167
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.466
_diffrn_reflns_theta_min         2.855
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    14.591
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54003
_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    1.868
_exptl_crystal_description       block
_exptl_crystal_F_000             3862
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         4.371
_refine_diff_density_min         -1.405
_refine_diff_density_rms         0.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         8072
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      2.693
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1161P)^2^+39.7753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1622
_refine_ls_wR_factor_ref         0.1690
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6924
_reflns_number_total             8072
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05824g2.cif
_cod_data_source_block           hy_CCDC1
_cod_depositor_comments
'Adding full bibliography for 1570485--1570493.cif.'
_cod_original_cell_volume        7145.74(18)
_cod_database_code               1570487
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'In Fe C H O P N'
_shelx_estimated_absorpt_t_max   0.323
_shelx_estimated_absorpt_t_min   0.142
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O14-H14B
 0.87 with sigma of 0.002
 H14B-H14A
 1.782 with sigma of 0.002
 H14A-O14
 0.87 with sigma of 0.002
3. Rigid bond restraints
 C25, C26
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C26, O15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C26, O12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C20, C25, C24, C23, C22, C21
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C26 \\sim C25: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
C26 \\sim O15: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
O12 \\sim C26: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
C20 \\sim C24 \\sim C25 \\sim C21 \\sim C22 \\sim C23: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
Uanis(C26) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O15) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
5. Others
 Fixed Sof: H14A(0.5) H14B(0.5) H27A(0.5) H27B(0.5) H27C(0.5)
6.a Rotating group:
 O14(H14A,H14B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C6(H6), C7(H7), C9(H9), C10(H10), C12(H12), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24)
6.c Fitted hexagon refined as free rotating group:
 C20(C21,C22,C23,C24,C25)
6.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C27(H27A,H27B,H27C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              42685
_shelx_fab_checksum              72930
_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 1.840
_oxdiff_exptl_absorpt_empirical_full_min 0.704