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_1570489
_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         'C73 H51 Cl3 Fe6 In7 O28, C22 H15 P'
_chemical_formula_sum            'C95 H66 Cl3 Fe6 In7 O28 P'
_chemical_formula_weight         2931.63
_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             2023-07-07
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_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            6
_cell_length_a                   16.15060(10)
_cell_length_b                   16.15060(10)
_cell_length_c                   65.6859(3)
_cell_measurement_reflns_used    28412
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      60.5200
_cell_measurement_theta_min      2.7960
_cell_volume                     14838.16(15)
_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_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 0.996
_diffrn_measured_fraction_theta_max 0.986
_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      1.00  85.36   0.38    0.70    --   73.53 -52.00 -88.00  222
  2  \w     69.00 104.34   0.38    0.70    --   73.53  52.00  56.00   93
  3  \w    115.00 145.78   0.38    0.70    --   73.53  52.00  56.00   81
  4  \w     99.00 139.28   0.38    0.70    --   73.53 125.00 -90.00  106
  5  \w      3.00  28.08   0.38    0.14    --   -0.62  52.00  56.00   66
  6  \w    -66.00 -30.66   0.38    0.70    --  -74.78  52.00  56.00   93
  7  \w    -12.00  72.36   0.38    0.14    --   -0.62  38.00-120.00  222
  8  \w    -70.00 -17.94   0.38    0.70    --  -74.78  38.00-120.00  137
  9  \w    -46.00   0.36   0.38    0.70    --  -74.78  19.00-120.00  122
 10  \w   -127.00 -60.12   0.38    0.70    --  -74.78 -52.00 -88.00  176
 11  \w   -138.00-112.92   0.38    0.70    --  -74.78 -99.00-150.00   66
 12  \w   -147.00 -81.26   0.38    0.70    --  -74.78-125.00   0.00  173
 13  \w   -143.00 -88.28   0.38    0.70    --  -74.78 -99.00  30.00  144
 14  \w   -148.00 -88.34   0.38    0.70    --  -74.78 -99.00 -30.00  157
 15  \w   -144.00 -93.84   0.38    0.70    --  -74.78 -99.00 -90.00  132
 16  \w    -72.00 -39.70   0.38    0.14    --   -0.62 -52.00 -88.00   85
 17  \w    -24.00  13.24   0.38    0.14    --   -0.62 -52.00 -88.00   98
;
_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      -0.0470974000
_diffrn_orient_matrix_UB_12      0.0058873000
_diffrn_orient_matrix_UB_13      0.0161951000
_diffrn_orient_matrix_UB_21      -0.0318160000
_diffrn_orient_matrix_UB_22      -0.0922521000
_diffrn_orient_matrix_UB_23      0.0042015000
_diffrn_orient_matrix_UB_31      0.0770859000
_diffrn_orient_matrix_UB_32      0.0251191000
_diffrn_orient_matrix_UB_33      0.0116415000
_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  0.0339
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       85
_diffrn_reflns_limit_l_min       -85
_diffrn_reflns_number            41444
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.670
_diffrn_reflns_theta_min         2.808
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    14.146
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67513
_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 black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.968
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             8550
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         3.452
_refine_diff_density_min         -1.891
_refine_diff_density_rms         0.097
_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     409
_refine_ls_number_reflns         7492
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0241
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+67.1517P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0701
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7040
_reflns_number_total             7492
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05824g2.cif
_cod_data_source_block           hy_CCDC2
_cod_depositor_comments
'Adding full bibliography for 1570485--1570493.cif.'
_cod_original_cell_volume        14838.2(2)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               1570489
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'In Fe C O H N'
_shelx_estimated_absorpt_t_max   0.305
_shelx_estimated_absorpt_t_min   0.305
_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. Others
 Fixed Sof: H2A(0.333333) H2B(0.333333) H2C(0.333333)
3.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25),
  C26(H26), C31(H31), C30(H30), C28(H28), C29(H29), C27(H27)
3.b Fitted hexagon refined as free rotating group:
 C31(C30,C1,C28,C29,C27)
3.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              13913
_shelx_fab_checksum              33919
_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 1.758
_oxdiff_exptl_absorpt_empirical_full_min 0.526