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_1570485
_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         'C96 H90 Fe6 In13 N12 O42'
_chemical_formula_sum            'C96 H90 Fe6 In13 N12 O42'
_chemical_formula_weight         3911.55
_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             2023-07-11
_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                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   19.80870(10)
_cell_length_b                   19.80870(10)
_cell_length_c                   28.7268(2)
_cell_measurement_reflns_used    16343
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      60.4050
_cell_measurement_theta_min      2.6030
_cell_volume                     9761.80(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_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      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.981
_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     57.00  84.00   0.50    0.59    --   71.86  38.00 150.00   54
  2  \w     79.00 145.00   0.50    0.59    --   71.86 125.00 150.00  132
  3  \w     82.00 145.00   0.50    0.59    --   71.86 121.00  60.00  126
  4  \w     48.00 145.00   0.50    0.59    --   71.86  77.00 -30.00  194
  5  \w     -2.00  71.00   0.50    0.59    --   71.86 -38.00-150.00  146
  6  \w    -16.00  72.00   0.50    0.15    --   -1.56  38.00-180.00  176
  7  \w    -98.00  -2.00   0.50    0.59    --  -74.99  75.00  50.00  192
  8  \w   -148.00 -84.00   0.50    0.59    --  -74.99 -94.00 -52.00  128
  9  \w   -148.00 -88.00   0.50    0.59    --  -74.99 -99.00 -90.00  120
 10  \w    -74.00  15.00   0.50    0.15    --   -1.56 -57.00-150.00  178
;
_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      -0.0656534000
_diffrn_orient_matrix_UB_12      -0.0029272000
_diffrn_orient_matrix_UB_13      0.0145663000
_diffrn_orient_matrix_UB_21      -0.0409275000
_diffrn_orient_matrix_UB_22      -0.0556374000
_diffrn_orient_matrix_UB_23      -0.0314372000
_diffrn_orient_matrix_UB_31      -0.0106198000
_diffrn_orient_matrix_UB_32      -0.0546569000
_diffrn_orient_matrix_UB_33      0.0312003000
_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  0.0725
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            21620
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.242
_diffrn_reflns_theta_min         2.608
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    16.335
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55070
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.115a (Rigaku Oxford Diffraction, 2021)
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    1.996
_exptl_crystal_description       block
_exptl_crystal_F_000             5637
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         4.376
_refine_diff_density_min         -1.391
_refine_diff_density_rms         0.308
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         4856
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0628
_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^)+(0.1067P)^2^+393.0479P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1894
_refine_ls_wR_factor_ref         0.1921
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4423
_reflns_number_total             4856
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05824g2.cif
_cod_data_source_block           hy
_cod_depositor_comments
'Adding full bibliography for 1570485--1570493.cif.'
_cod_original_cell_volume        9761.79(12)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               1570485
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         InFeCNHO
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained planarity
 N1, C14, C15, N2, C13
 with sigma of 0.01
3. Rigid body (RIGU) restrains
 N1, C14, C15, N2, C13
 with sigma for 1-2 distances of 55 and sigma for 1-3 distances of 55
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C10(H10), N2(H2A), C4(H4), C8(H8), C7(H7), C3(H3), C9(H9), C15(H15),
 C5(H5), C14(H14), C13(H13)
4.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C)
;
_shelx_res_checksum              91605
_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 2.680
_oxdiff_exptl_absorpt_empirical_full_min 0.509
_platon_squeeze_void_probe_radius 1.20