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_1570486
_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         'C68 H56 Cl2 Fe4 In13 N8 O38'
_chemical_formula_sum            'C68 H56 Cl2 Fe4 In13 N8 O38'
_chemical_formula_weight         3380.16
_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   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                 95.854(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.6313(8)
_cell_length_b                   22.9290(6)
_cell_length_c                   13.3713(4)
_cell_measurement_reflns_used    12901
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      60.2820
_cell_measurement_theta_min      2.5870
_cell_volume                     5987.4(3)
_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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.975
_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    -14.00  67.00   0.50    0.12    --   -1.25  57.00 -60.00  162
  2  \w     23.00  48.00   0.50    0.12    --   -1.25  72.00 -28.00   50
  3  \w     94.00 130.00   0.50    0.50    --   72.28  72.00 -28.00   72
  4  \w     -1.00  93.00   0.50    0.50    --   72.28 -72.00-158.00  188
  5  \w    -71.00 -28.00   0.50    0.50    --  -74.78  72.00 -28.00   86
  6  \w    -90.00  -2.00   0.50    0.50    --  -74.78  57.00  60.00  176
  7  \w    -76.00 -50.00   0.50    0.50    --  -74.78  57.00 150.00   52
  8  \w    -34.00  -5.00   0.50    0.50    --  -74.78  57.00 150.00   58
  9  \w   -102.00 -77.00   0.50    0.50    --  -74.78 -38.00  30.00   50
 10  \w   -125.00-100.00   0.50    0.50    --  -74.78 -72.00-158.00   50
 11  \w    -73.00  -9.00   0.50    0.12    --   -1.25 -72.00-158.00  128
 12  \w   -147.00-107.00   0.50    0.50    --  -74.78 -38.00  30.00   80
 13  \w   -137.00 -88.00   0.50    0.50    --  -74.78 -99.00 -30.00   98
 14  \w   -147.00 -88.00   0.50    0.50    --  -74.78 -99.00 -90.00  118
 15  \w   -128.00 -79.00   0.50    0.50    --  -74.78-125.00 150.00   98
 16  \w   -147.00 -90.00   0.50    0.50    --  -74.78 -99.00 120.00  114
 17  \w   -147.00-118.00   0.50    0.50    --  -74.78 -99.00 150.00   58
;
_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      0.0627717000
_diffrn_orient_matrix_UB_12      -0.0028357000
_diffrn_orient_matrix_UB_13      -0.0308284000
_diffrn_orient_matrix_UB_21      0.0142163000
_diffrn_orient_matrix_UB_22      -0.0466946000
_diffrn_orient_matrix_UB_23      0.0587087000
_diffrn_orient_matrix_UB_31      -0.0237236000
_diffrn_orient_matrix_UB_32      -0.0350037000
_diffrn_orient_matrix_UB_33      -0.0756513000
_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  0.0307
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24481
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.476
_diffrn_reflns_theta_min         2.584
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    16.298
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68377
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.875
_exptl_crystal_description       prism
_exptl_crystal_F_000             3198
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         5.581
_refine_diff_density_min         -2.941
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         6860
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0770P)^2^+52.6835P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1318
_refine_ls_wR_factor_ref         0.1356
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5921
_reflns_number_total             6860
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05824g2.cif
_cod_data_source_block           4-9-26_auto
_cod_depositor_comments
'Adding full bibliography for 1570485--1570493.cif.'
_cod_database_code               1570486
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'In Fe C N H O'
_shelx_estimated_absorpt_t_max   0.293
_shelx_estimated_absorpt_t_min   0.139
_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
2. Restrained distances
 O9-C17
 1.45 with sigma of 0.02
 C17-O9
 1.45 with sigma of 0.002
3. Restrained planarity
 C17, O9, In5, O8
 with sigma of 0.1
4. Rigid bond restraints
 O9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C17
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O9, C17
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
O9: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
1.7A
O9 \\sim C17: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
Uanis(O9) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C17) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O9) \\sim Ueq, Uanis(C17) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
6. Rigid body (RIGU) restrains
 O9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Fixed Sof: C17(0.5)
8.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C15(H15), C13(H13), C11(H11), C10(H10), C5(H5), C9(H9), C14(H14),
 C2(H2), C3(H3), C4(H4)
8.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C)
;
_shelx_res_checksum              7204
_shelx_fab_checksum              38726
_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 2.586
_oxdiff_exptl_absorpt_empirical_full_min 0.489