Accurate assembly of ferrocene-functionalized {Ti22Fc4} clusters with photocatalytic amine oxidation activity.
Han, Er-Meng; Yu, Wei-Dong; Li, Lei-Jiao; Yi, Xiao-Yi; Yan, Jun; Liu, Chao; Chemical communications (Cambridge, England) 57 (2021) 2792–2795; doi:10.1039/d1cc00019e

data_7127901
_publ_section_title
;
 Accurate assembly of ferrocene-functionalized {Ti22Fc4} clusters with
 photocatalytic amine oxidation activity.
;
_journal_issue                   22
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2792
_journal_page_last               2795
_journal_paper_doi               10.1039/d1cc00019e
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C80 H130 Fe2 N10 O39 Ti11, C3 H7 O'
_chemical_formula_sum            'C83 H137 Fe2 N10 O39 Ti11'
_chemical_formula_weight         2537.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-11-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2021-01-03 deposited with the CCDC.	2021-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.058(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.8611(6)
_cell_length_b                   21.3692(5)
_cell_length_c                   25.6759(9)
_cell_measurement_reflns_used    13349
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      69.9870
_cell_measurement_theta_min      4.1090
_cell_volume                     11267.1(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.981
_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     39.00  66.00   1.00    5.00    --  108.00 -50.00   0.00   27
  2  \w     39.00 109.00   1.00    5.00    --  108.00-111.00-120.00   70
  3  \w     52.00 135.00   1.00    5.00    --  108.00 -77.00-120.00   83
  4  \w     39.00  87.00   1.00    3.00    --   54.00  57.00-120.00   48
  5  \w    101.00 178.00   1.00    5.00    --  108.00 111.00 -90.00   77
  6  \w    134.00 163.00   1.00    5.00    --  108.00 111.00-120.00   29
  7  \w    100.00 174.00   1.00    5.00    --  108.00 111.00 -60.00   74
  8  \w     88.00 176.00   1.00    5.00    --  108.00  63.00   0.00   88
  9  \w     38.00 127.00   1.00    5.00    --  108.00 -50.00-150.00   89
 10  \w     24.00 108.00   1.00    3.00    --   54.00-125.00-150.00   84
 11  \w     -1.00  25.00   1.00    1.00    --    0.00 -38.00 -90.00   26
 12  \w      2.00  68.00   1.00    3.00    --   54.00   0.00 -90.00   66
 13  \w    -15.00  72.00   1.00    3.00    --   54.00 -57.00 -90.00   87
 14  \w    -31.00  14.00   1.00    1.00    --    0.00 -57.00  30.00   45
 15  \w    -67.00 -36.00   1.00    1.00    --    0.00 -57.00  30.00   31
 16  \w    -69.00 -29.00   1.00    1.00    --    0.00 -38.00 -90.00   40
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0682194000
_diffrn_orient_matrix_UB_12      0.0238647000
_diffrn_orient_matrix_UB_13      0.0348430000
_diffrn_orient_matrix_UB_21      -0.0038781000
_diffrn_orient_matrix_UB_22      -0.0363395000
_diffrn_orient_matrix_UB_23      0.0505627000
_diffrn_orient_matrix_UB_31      0.0309307000
_diffrn_orient_matrix_UB_32      -0.0575453000
_diffrn_orient_matrix_UB_33      -0.0174942000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_unetI/netI     0.0794
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            44929
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.926
_diffrn_reflns_theta_min         3.665
_exptl_absorpt_coefficient_mu    8.948
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26248
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       block
_exptl_crystal_F_000             5244
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.663
_refine_diff_density_min         -0.980
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1351
_refine_ls_number_reflns         20948
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1018
_refine_ls_R_factor_gt           0.0675
_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^)+(0.0903P)^2^+36.6653P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1689
_refine_ls_wR_factor_ref         0.1951
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14678
_reflns_number_total             20948
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc00019e2.cif
_cod_data_source_block           Ti11Fc2
_cod_depositor_comments
'Adding full bibliography for 7127900--7127902.cif.'
_cod_database_code               7127901
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.174
_shelx_estimated_absorpt_t_min   0.094
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
 C2-C3
 1.45 with sigma of 0.01
 C2-C1
 1.45 with sigma of 0.01
3. Rigid bond restraints
 C7, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C7, O33
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C7 \\sim C8: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
C7 \\sim O33: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
Uanis(C46) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1)
\\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C4) \\sim Ueq,
Uanis(C5) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C75) \\sim
Ueq, Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
5.a Ternary CH refined with riding coordinates:
 C13(H13), C37(H37), C69(H69), C72(H72), C50(H50), C5(H5), C15(H15), C40(H40),
 C47(H47), C76(H76), C2(H2), C65(H65), C7(H7)
5.b Aromatic/amide H refined with riding coordinates:
 C58(H58), C68(H68), C66(H66), C67(H67), C61(H61), C59(H59), C60(H60),
 C64(H64), C26(H26), C23(H23), C31(H31), C29(H29), C24(H24), C27(H27), C25(H25),
  C28(H28)
5.c Idealised Me refined as rotating group:
 C53(H53a,H53b,H53c), C45(H45a,H45b,H45c), C44(H44a,H44b,H44c), C55(H55a,H55b,
 H55c), C17(H17a,H17b,H17c), C38(H38a,H38b,H38c), C85(H85a,H85b,H85c), C12(H12a,
 H12b,H12c), C71(H71a,H71b,H71c), C20(H20a,H20b,H20c), C84(H84a,H84b,H84c),
 C49(H49a,H49b,H49c), C36(H36a,H36b,H36c), C41(H41a,H41b,H41c), C73(H73a,H73b,
 H73c), C14(H14a,H14b,H14c), C35(H35a,H35b,H35c), C74(H74a,H74b,H74c), C11(H11a,
 H11b,H11c), C51(H51a,H51b,H51c), C70(H70a,H70b,H70c), C6(H6a,H6b,H6c),
 C33(H33a,H33b,H33c), C3(H3a,H3b,H3c), C16(H16a,H16b,H16c), C4(H4a,H4b,H4c),
 C48(H48a,H48b,H48c), C39(H39a,H39b,H39c), C46(H46a,H46b,H46c), C1(H1a,H1b,H1c),
  C86(H86a,H86b,H86c), C83(H83a,H83b,H83c), C75(H75a,H75b,H75c), C77(H77a,H77b,
 H77c), C9(H9a,H9b,H9c), C8(H8a,H8b,H8c)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              12611
_shelx_fab_checksum              50044
_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 2.885
_oxdiff_exptl_absorpt_empirical_full_min 0.600