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_1570488
_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         'C78 H78 Fe6 In13 O48'
_chemical_formula_sum            'C78 H78 Fe6 In13 O48'
_chemical_formula_weight         3611.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-04-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-07-14 deposited with the CCDC.	2023-11-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.153(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.0443(7)
_cell_length_b                   14.9493(3)
_cell_length_c                   28.0793(7)
_cell_measurement_reflns_used    18983
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      50.3340
_cell_measurement_theta_min      3.1130
_cell_volume                     13415.8(5)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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    -20.00  70.00   0.50    0.05    --   53.03 -63.00  38.00  180
  2  \w     56.00 119.00   0.50    0.05    --   53.03  63.00 175.00  126
  3  \w     79.00 125.00   0.50    0.05    --   53.03 125.00  90.00   92
  4  \w     79.00 125.00   0.50    0.05    --   53.03 125.00  30.00   92
  5  \w     80.00 121.00   0.50    0.05    --   53.03 125.00-120.00   82
  6  \w     26.00  51.00   0.50    0.05    --   -0.94  63.00 175.00   50
  7  \w    -73.00  18.00   0.50    0.05    --  -54.91  63.00 175.00  182
  8  \w    -28.00  -3.00   0.50    0.05    --   -0.94 -63.00  38.00   50
  9  \w   -106.00 -81.00   0.50    0.05    --  -54.91 -63.00  38.00   50
 10  \w    -87.00 -45.00   0.50    0.05    --  -54.91 -38.00-120.00   84
 11  \w   -128.00-102.00   0.50    0.05    --  -54.91 -38.00-120.00   52
 12  \w   -116.00 -79.00   0.50    0.05    --  -54.91-125.00-150.00   74
 13  \w   -127.00-102.00   0.50    0.05    --  -54.91-125.00-180.00   50
 14  \w   -113.00 -88.00   0.50    0.05    --  -54.91-125.00 -30.00   50
 15  \w   -112.00 -85.00   0.50    0.05    --  -54.91-125.00 150.00   54
;
_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      -0.0370409000
_diffrn_orient_matrix_UB_12      0.0210283000
_diffrn_orient_matrix_UB_13      -0.0222136000
_diffrn_orient_matrix_UB_21      -0.0185415000
_diffrn_orient_matrix_UB_22      -0.0625760000
_diffrn_orient_matrix_UB_23      0.0252871000
_diffrn_orient_matrix_UB_31      -0.0062733000
_diffrn_orient_matrix_UB_32      0.0604872000
_diffrn_orient_matrix_UB_33      0.0339548000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            39412
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        50.637
_diffrn_reflns_theta_max         50.637
_diffrn_reflns_theta_min         3.114
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    15.472
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37868
_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 yellowish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_description       block
_exptl_crystal_F_000             6892
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.496
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     661
_refine_ls_number_reflns         10636
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0770P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1321
_refine_ls_wR_factor_ref         0.1396
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7991
_reflns_number_total             10636
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05824g2.cif
_cod_data_source_block           5-12-18_auto
_cod_depositor_comments
'Adding full bibliography for 1570485--1570493.cif.'
_cod_database_code               1570488
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'In Fe C N O'
_shelx_estimated_absorpt_t_max   0.281
_shelx_estimated_absorpt_t_min   0.258
_diffrn_oxdiff_digest_frames
;
016d9334ba46876be9dc8b807dd9096bd9012680a00
;
_diffrn_oxdiff_digest_hkl
;
01403414fd31ec804ccd65845cc3bcb364865a
;
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     49.54
_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
 H20B-O20
 1 with sigma of 0.02
 O20-H20A
 1 with sigma of 0.02
3.a Rotating group:
 O20(H20A,H20B), O23(H23A,H23B), O24(H24A,H24B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C6(H6), C11(H11), C14(H14), C15(H15), C16(H16), C18(H18), C20(H20),
 C21(H21), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29),
  C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C39(H39)
3.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C31(H31A,H31B,H31C), C38(H38A,H38B,H38C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              38016
_shelx_fab_checksum              19767
_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 1.962
_oxdiff_exptl_absorpt_empirical_full_min 0.501