Ferrocene-Functionalized Polyoxo-Titanium Cluster for CO2 Photoreduction
Liu, Jing-Jing; Li, Ning; Sun, Jia-Wei; Liu, Jiang; Dong, Long-Zhang; Yao, Su-Juan; Zhang, Lei; Xin, Zhi-Feng; Shi, Jing-Wen; Wang, Jing-Xuan; Li, Shun-Li; Lan, Ya-Qian; ACS Catalysis  (2021) 4510–4519; doi:10.1021/acscatal.0c04495

data_4518588
_publ_section_title
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 Ferrocene-Functionalized Polyoxo-Titanium Cluster for CO2 Photoreduction
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_journal_name_full               'ACS Catalysis'
_journal_page_first              4510
_journal_page_last               4519
_journal_paper_doi               10.1021/acscatal.0c04495
_journal_year                    2021
_chemical_formula_moiety         'C60 H100 Fe2 O30 S2 Ti6, 2(C3 H8 O)'
_chemical_formula_sum            'C66 H116 Fe2 O32 S2 Ti6'
_chemical_formula_weight         1884.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-08-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
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_cell_angle_alpha                90
_cell_angle_beta                 94.632(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.653(6)
_cell_length_b                   14.083(3)
_cell_length_c                   20.207(4)
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.520
_cell_measurement_theta_min      2.31
_cell_volume                     8978(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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      296.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36561
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.600
_diffrn_reflns_theta_min         1.584
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.939
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0625 before and 0.0457 after correction.
The Ratio of minimum to maximum transmission is 0.9248.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             3936
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         10259
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0817P)^2^+14.4644P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1331
_refine_ls_wR_factor_ref         0.1525
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7834
_reflns_number_total             10259
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c04495_si_001.cif
_cod_data_source_block           Ti6-Fcdc
_cod_database_code               4518588
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.981
_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) groups
2. Restrained distances
 C31-H31
 0.82 with sigma of 0.02
 C28-H28
 0.82 with sigma of 0.02
 C33-H31
 2.1 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C22(H22), C16(H16), C19(H19), C13(H13), C25(H25), C31(H31)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C12(H12), C6(H6), C9(H9), C4(H4), C10(H10), C5(H5), C11(H11)
3.c Idealised Me refined as rotating group:
 C23(H23a,H23b,H23c), C24(H24a,H24b,H24c), C14(H14a,H14b,H14c), C15(H15a,H15b,
 H15c), C26(H26a,H26b,H26c), C17(H17a,H17b,H17c), C20(H20a,H20b,H20c), C27(H27a,
 H27b,H27c), C18(H18a,H18b,H18c), C21(H21a,H21b,H21c), C30(H30a,H30b,H30c),
 C29(H29a,H29b,H29c), C32(H32a,H32b,H32c), C33(H33a,H33b,H33c)
3.d Idealised tetrahedral OH refined as rotating group:
 O16(H16a)
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_shelx_res_checksum              78584
_shelx_hkl_checksum              9107
_olex2_submission_special_instructions 'No special instructions were received'