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_1570492
_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         'C92 H96 Fe6 In13 N6 O46'
_chemical_formula_sum            'C92 H96 Fe6 In13 N6 O46'
_chemical_formula_weight         3849.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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                 94.0511(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.37206(19)
_cell_length_b                   15.00755(12)
_cell_length_c                   31.8968(3)
_cell_measurement_reflns_used    33620
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      60.9610
_cell_measurement_theta_min      2.4020
_cell_volume                     13070.07(19)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.969
_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     51.00 141.00   0.50    0.27    --   74.47  77.00 150.00  180
  2  \w    108.00 146.00   0.50    0.27    --   74.47  77.00  90.00   76
  3  \w     52.00  90.00   0.50    0.27    --   74.47  77.00  90.00   76
  4  \w     65.00 146.00   0.50    0.27    --   74.47  45.00  55.00  162
  5  \w     80.00 132.00   0.50    0.27    --   74.47 125.00 -60.00  104
  6  \w     19.00  75.00   0.50    0.27    --   74.47 -45.00 -94.00  112
  7  \w     14.00  67.00   0.50    0.27    --   74.47 -38.00  60.00  106
  8  \w     44.00  69.00   0.50    0.06    --   -0.31  45.00  55.00   50
  9  \w    -51.00 -25.00   0.50    0.27    --  -75.09  45.00  55.00   52
 10  \w    -12.00  38.00   0.50    0.06    --   -0.31  45.00  55.00  100
 11  \w    -61.00  -1.00   0.50    0.27    --  -75.09  38.00-120.00  120
 12  \w    -10.00  16.00   0.50    0.06    --   -0.31  38.00-180.00   52
 13  \w    -70.00  -3.00   0.50    0.06    --   -0.31 -45.00 -94.00  134
 14  \w   -144.00 -91.00   0.50    0.27    --  -75.09-125.00   0.00  106
 15  \w   -114.00 -83.00   0.50    0.27    --  -75.09 -45.00 -94.00   62
 16  \w   -146.00 -98.00   0.50    0.27    --  -75.09 -99.00-150.00   96
;
_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      0.0415007000
_diffrn_orient_matrix_UB_12      -0.0469861000
_diffrn_orient_matrix_UB_13      -0.0008771000
_diffrn_orient_matrix_UB_21      0.0013732000
_diffrn_orient_matrix_UB_22      0.0174299000
_diffrn_orient_matrix_UB_23      -0.0410699000
_diffrn_orient_matrix_UB_31      0.0260945000
_diffrn_orient_matrix_UB_32      0.0738576000
_diffrn_orient_matrix_UB_33      0.0091571000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            49091
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         61.176
_diffrn_reflns_theta_min         2.415
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    15.915
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18204
_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    1.956
_exptl_crystal_description       block
_exptl_crystal_F_000             7404
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.063
_refine_diff_density_min         -3.605
_refine_diff_density_rms         0.321
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     743
_refine_ls_number_reflns         14802
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      3.577
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0641
_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^)+(0.1435P)^2^+20.7721P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1829
_refine_ls_wR_factor_ref         0.1872
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13203
_reflns_number_total             14802
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05824g2.cif
_cod_data_source_block           hy_CCDC3
_cod_depositor_comments
'Adding full bibliography for 1570485--1570493.cif.'
_cod_original_cell_volume        13070.05(17)
_cod_database_code               1570492
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'In Fe C N O H'
_shelx_estimated_absorpt_t_max   0.299
_shelx_estimated_absorpt_t_min   0.143
_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, All O(H,H) groups
2. Restrained distances
 H2B-O2
 0.87 with sigma of 0.002
 H2A-H2B
 1.87 with sigma of 0.002
 O2-H2B
 0.87 with sigma of 0.002
 H2A-O2
 0.87 with sigma of 0.002
3.a Rotating group:
 O2(H2A,H2B)
3.b Aromatic/amide H refined with riding coordinates:
 N4(H4), C3(H3), C5(H5), C8(H8), C10(H10), C12(H12), C14(H14), C16(H16),
 C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26),
  C28(H28), C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38),
 C39(H39), C40(H40), C41(H41), C42(H42), C46(H46)
3.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C43(H43A,H43B,
 H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              50893
_shelx_fab_checksum              69119
_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 3.043
_oxdiff_exptl_absorpt_empirical_full_min 0.319