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_1570490
_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         'C304 H224 Fe24 In28 N8 O116'
_chemical_formula_sum            'C304 H216 Fe24 In28 N8 O116'
_chemical_formula_weight         10392.20
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-07-08
_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                90
_cell_formula_units_Z            2
_cell_length_a                   35.1846(4)
_cell_length_b                   35.1846(4)
_cell_length_c                   15.8530(4)
_cell_measurement_reflns_used    17039
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      60.1420
_cell_measurement_theta_min      3.0950
_cell_volume                     19625.3(6)
_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 (Sheldrick, 2015)'
_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 0.998
_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     12.00  51.00   0.50    6.50    --   73.53 -62.00  37.00   78
  2  \w    -94.00  -3.00   0.50    6.50    --  -74.78  69.00 -49.00  182
  3  \w    -29.00  12.00   0.50    1.44    --   -0.62  93.00  49.00   82
  4  \w    -28.00   7.00   0.50    1.44    --   -0.62 -93.00 -62.00   70
  5  \w    104.00 147.00   0.50    6.50    --   73.53 125.00 120.00   86
  6  \w   -141.00 -81.00   0.50    6.50    --  -74.78-125.00-120.00  120
  7  \w   -134.00 -91.00   0.50    6.50    --  -74.78 -99.00-120.00   86
;
_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      0.0350771000
_diffrn_orient_matrix_UB_12      -0.0078561000
_diffrn_orient_matrix_UB_13      0.0281021000
_diffrn_orient_matrix_UB_21      -0.0037689000
_diffrn_orient_matrix_UB_22      0.0265804000
_diffrn_orient_matrix_UB_23      0.0598119000
_diffrn_orient_matrix_UB_31      -0.0144235000
_diffrn_orient_matrix_UB_32      -0.0260354000
_diffrn_orient_matrix_UB_33      0.0525505000
_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  0.0504
_diffrn_reflns_av_unetI/netI     0.0633
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            69336
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.691
_diffrn_reflns_theta_min         2.183
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    13.631
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79154
_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    1.759
_exptl_crystal_description       block
_exptl_crystal_F_000             10040
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.932
_refine_diff_density_min         -1.536
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1083
_refine_ls_number_reflns         22086
_refine_ls_number_restraints     240
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1105
_refine_ls_R_factor_gt           0.0644
_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^)+(0.1148P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1758
_refine_ls_wR_factor_ref         0.2001
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12306
_reflns_number_total             22086
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05824g2.cif
_cod_data_source_block           5-3-4_auto
_cod_depositor_comments
'Adding full bibliography for 1570485--1570493.cif.'
_cod_original_cell_volume        19625.3(7)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               1570490
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'In Fe C N H O'
_shelx_estimated_absorpt_t_max   0.772
_shelx_estimated_absorpt_t_min   0.549
_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 planarity
 C21, C02L, C036, C035, C02W
 with sigma of 0.1
 C037, C039, C034, C22, C24
 with sigma of 0.1
3. Rigid bond restraints
 C21, C02L, C02W, C036, C035
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C24, C037, C039, C034, C22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C21 \\sim C02L \\sim C02W \\sim C036 \\sim C035: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 1.7A
C22 \\sim C24 \\sim C037 \\sim C039 \\sim C034: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 1.7A
Uanis(C21) \\sim Ueq, Uanis(C035) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C24)
\\sim Ueq, Uanis(C039) \\sim Ueq, Uanis(C034) \\sim Ueq, Uanis(C0AA) \\sim Ueq,
Uanis(C032) \\sim Ueq, Uanis(C02M) \\sim Ueq, Uanis(C02Y) \\sim Ueq,
Uanis(C02U) \\sim Ueq, Uanis(C028) \\sim Ueq, Uanis(C02V) \\sim Ueq,
Uanis(C038) \\sim Ueq, Uanis(C02Z) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C037) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C039) \\sim Ueq, Uanis(C034)
\\sim Ueq, Uanis(C22) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
5. Rigid body (RIGU) restrains
 C21, C035, C036, C02W, C02L
 with sigma for 1-2 distances of 55 and sigma for 1-3 distances of 55
 C039, C037, C24, C22, C034
 with sigma for 1-2 distances of 55 and sigma for 1-3 distances of 55
6.a Rotating group:
 O014(H01A,H01B)
6.b Ternary CH refined with riding coordinates:
 C031(H031), C034(H034), C035(H035), C036(H036)
6.c Aromatic/amide H refined with riding coordinates:
 C01E(H01E), C01O(H01O), C01P(H01P), C01R(H01R), C01S(H01S), C01U(H01U),
 C01V(H01V), C01W(H01W), C01X(H01X), C01Z(H01Z), C020(H020), C021(H021),
 C024(H024), C025(H025), C027(H027), C029(H029), C02A(H02A), C02B(H02B),
 C02C(H02C), C02D(H02D), C02E(H02E), C02F(H02F), C02G(H02G), C02H(H02H),
 C02I(H02I), C02J(H02J), C02K(H02K), C02M(H02M), C02N(H02N), C02O(H02O),
 C02P(H02P), C02Q(H02Q), C02S(H02T), C02T(H02U), C02U(H02V), C02W(H02W),
 C02X(H02X), C02Y(H02Y), C02Z(H02Z), C030(H030), C032(H032), C038(H038),
 C039(H039), C21(H21), C22(H22), C24(H24), C0AA(H0AA)
6.d Idealised Me refined as rotating group:
 C02R(H02L,H02R,H02S)
;
_shelx_res_checksum              79803
_shelx_fab_checksum              18549
_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 2.046
_oxdiff_exptl_absorpt_empirical_full_min 0.590