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_7127900
_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         'C53 H86.69 Fe N3 O22 Ti5'
_chemical_formula_sum            'C53 H86.68 Fe N3 O22 Ti5'
_chemical_formula_weight         1413.27
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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                78.353(3)
_cell_angle_beta                 76.753(2)
_cell_angle_gamma                63.302(2)
_cell_formula_units_Z            2
_cell_length_a                   13.5246(11)
_cell_length_b                   14.1422(11)
_cell_length_c                   20.7800(15)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    149.98
_cell_measurement_theta_max      25.982
_cell_measurement_theta_min      2.448
_cell_volume                     3433.9(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.26a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.26a (Rigaku OD, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      149.98
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            34690
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.069
_diffrn_reflns_theta_min         2.448
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.829
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.26a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       block
_exptl_crystal_F_000             1475
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     879
_refine_ls_number_reflns         13385
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0587P)^2^+2.2555P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1335
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10410
_reflns_number_total             13385
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc00019e2.cif
_cod_data_source_block           Ti5Fc
_cod_depositor_comments
'Adding full bibliography for 7127900--7127902.cif.'
_cod_database_code               7127900
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.789
_shelx_estimated_absorpt_t_min   0.682
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C44-C45
 1.45 with sigma of 0.01
 C35-C36
 1.45 with sigma of 0.01
 C43-C39 \\sim C43-C41
 with sigma of 0.01
 C43-C40 \\sim C43-C42
 with sigma of 0.01
 C54-C56 \\sim C54-C57 \\sim C54-C55
 with sigma of 0.01
 C35-C36 \\sim C35-C37 \\sim C35-C36A
 with sigma of 0.01
3. Rigid bond restraints
 C23, C22
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 Ti2, O9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
C23 \\sim C22: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Ti2 \\sim O9: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Uanis(C56) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C31)
\\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C46) \\sim Ueq,
Uanis(C32) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(H54a)=Sof(C56)=Sof(H56a)=Sof(H56b)=Sof(H56c)=1-FVAR(1)
 Sof(H54)=Sof(C57)=Sof(H57a)=Sof(H57b)=Sof(H57c)=FVAR(1)
 Sof(C39)=Sof(H39a)=Sof(H39b)=Sof(H39c)=Sof(C41)=Sof(H41a)=Sof(H41b)=Sof(H41c)=
 1-FVAR(2)
 Sof(H43)=Sof(C42)=Sof(H42a)=Sof(H42b)=Sof(H42c)=Sof(C40)=Sof(H40a)=Sof(H40b)=
 Sof(H40c)=FVAR(2)
 Sof(C45)=Sof(H45a)=Sof(H45b)=Sof(H45c)=Sof(C47)=Sof(H47a)=Sof(H47b)=Sof(H47c)=
 1-FVAR(3)
 Sof(C46)=Sof(H46a)=Sof(H46b)=Sof(H46c)=Sof(C48)=Sof(H48a)=Sof(H48b)=Sof(H48c)=
 FVAR(3)
 Sof(H30a)=Sof(C34)=Sof(O1A)=Sof(O2A)=1-FVAR(4)
 Sof(H30)=Sof(C33)=Sof(O1)=Sof(O2)=FVAR(4)
 Sof(H35a)=Sof(C36A)=Sof(H36d)=Sof(H36e)=Sof(H36f)=1-FVAR(5)
 Sof(H35)=Sof(C36)=Sof(H36a)=Sof(H36b)=Sof(H36c)=FVAR(5)
6.a Ternary CH refined with riding coordinates:
 C27(H27), C1(H1), C43(H43), C8(H8), C20(H20), C35(H35), C35(H35a), C5(H5),
 C54(H54), C54(H54a), C30(H30), C30(H30a)
6.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C52(H52), C16(H16), C53(H53), C50(H50), C51(H51), C38(H38),
 C58(H58), C22(H22), C17(H17)
6.c Idealised Me refined as rotating group:
 C12(H12a,H12b,H12c), C13(H13a,H13b,H13c), C29(H29a,H29b,H29c), C9(H9a,H9b,
 H9c), C2(H2a,H2b,H2c), C3(H3a,H3b,H3c), C37(H37a,H37b,H37c), C28(H28a,H28b,
 H28c), C7(H7a,H7b,H7c), C4(H4a,H4b,H4c), C18(H18a,H18b,H18c), C19(H19a,H19b,
 H19c), C36(H36a,H36b,H36c), C55(H55a,H55b,H55c), C57(H57a,H57b,H57c), C56(H56a,
 H56b,H56c), C42(H42a,H42b,H42c), C40(H40a,H40b,H40c), C39(H39a,H39b,H39c),
 C41(H41a,H41b,H41c), C46(H46a,H46b,H46c), C48(H48a,H48b,H48c), C45(H45a,H45b,
 H45c), C47(H47a,H47b,H47c), C6(H6a,H6b,H6c), C32(H32a,H32b,H32c), C31(H31a,
 H31b,H31c), C36A(H36d,H36e,H36f)
;
_shelx_res_checksum              86668
_olex2_submission_special_instructions 'No special instructions were received'