Solid-phase synthesis of titanium-oxo clusters and their unprecedented catalytic performance in oxidative desulfurization of fuel oil
Liu, Xinchun; Yuan, Yanpeng; Fu, Jiawei; Kong, Yuqing; Sun, Yinyong; Li, Xiaolin; Qu, Nan; Green Chemistry 27 (2025) 2995–3003; doi:10.1039/D4GC05728G

data_7249936
_publ_section_title
;
 Solid-phase synthesis of titanium-oxo clusters and their unprecedented
 catalytic performance in oxidative desulfurization of fuel oil
;
_journal_issue                   11
_journal_name_full               'Green Chemistry'
_journal_page_first              2995
_journal_page_last               3003
_journal_paper_doi               10.1039/D4GC05728G
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C76 H190 K O77 Ti29'
_chemical_formula_sum            'C76 H190 K O77 Ti29'
_chemical_formula_weight         3764.47
_chemical_name_systematic        Ti29KO39(OEt)38
_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             2023-08-04
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-08-04 deposited with the CCDC.	2025-02-11 downloaded from the CCDC.
;
_cell_angle_alpha                85.261(3)
_cell_angle_beta                 79.664(3)
_cell_angle_gamma                68.022(2)
_cell_formula_units_Z            2
_cell_length_a                   16.5381(9)
_cell_length_b                   17.0084(9)
_cell_length_c                   28.4386(16)
_cell_measurement_reflns_used    8994
_cell_measurement_temperature    298.30
_cell_measurement_theta_max      56.97
_cell_measurement_theta_min      3.71
_cell_volume                     7296.6(7)
_computing_cell_refinement       ABC
_computing_data_reduction        ABC
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298.30
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0799
_diffrn_reflns_av_unetI/netI     0.0578
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            134312
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.291
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.603
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.4573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1498 before and 0.0771 after correction.
The Ratio of minimum to maximum transmission is 0.6088.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_description       block
_exptl_crystal_F_000             3838
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.071
_refine_diff_density_min         -1.056
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1345
_refine_ls_number_reflns         25683
_refine_ls_number_restraints     148
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0697
_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^)+(0.0988P)^2^+23.7576P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1844
_refine_ls_wR_factor_ref         0.2087
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17623
_reflns_number_total             25683
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4gc05728g4.cif
_cod_data_source_block           20230614_2_0m
_cod_depositor_comments          'Adding full bibliography for 7249936.cif.'
_cod_database_code               7249936
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.831
_shelx_estimated_absorpt_t_min   0.795
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O31-C10 = O2-C12 = O17-C6 = O21-C4 = O41-C58 = O56-C56 = O67-C48 = O27-C50 =
 O29-C44 = O77-C46 = O19-C14 = O33-C42 = O25-C36 = O71-C34 = O5-C38 = O69-C40 =
 O63-C30 = O62-C28 = O65-C26 = O57-C22 = O35-C76 = O47-C74 = O53-C66 = O9-C72 =
 O23-C70 = O15-C18 = O75-C8 = O73-C16 = O39-C68 = O37-C32 = O70-C20 = O59-C24 =
 O55-C2 = O49-C54 = O43-C62 = O61-C60 = O7-C52 = O13-C64
 1.39 with sigma of 0.01
 C69-C70 = C44-C43 = C58-C57 = C14-C13 = C10-C9 = C5-C6 = C40-C39 = C11-C12 =
 C29-C30 = C37-C38 = C32-C31 = C24-C23 = C28-C27 = C26-C25 = C22-C21 = C15-C16 =
  C19-C20 = C74-C73 = C75-C76 = C34-C33 = C35-C36 = C67-C68 = C42-C41 = C45-C46
 = C66-C65 = C64-C63 = C52-C51 = C59-C60 = C62-C61 = C53-C54 = C72-C71 = C17-
 C18 = C55-C56 = C47-C48 = C49-C50 = C1-C2 = C3-C4 = C7-C8
 1.53 with sigma of 0.0001
 C29-C30 \\sim C29A-C30A
 with sigma of 0.02
 O63-C30 \\sim O63-C30A
 with sigma of 0.02
 O63-C29 \\sim O63-C29A
 with sigma of 0.04
 O25-C36 \\sim O25-C36A
 with sigma of 0.02
 C31-C32 \\sim C31A-C32A
 with sigma of 0.02
 C35-C36 \\sim C35A-C36A
 with sigma of 0.02
 C5-C6 \\sim C5A-C6A
 with sigma of 0.02
 O37-C31 \\sim O37-C31A
 with sigma of 0.04
 O17-C6 \\sim O17-C6A
 with sigma of 0.02
 C33-C34 \\sim C33A-C34A
 with sigma of 0.02
 O71-C33 \\sim O71-C33A
 with sigma of 0.04
 C43-C44 \\sim C43A-C44A
 with sigma of 0.02
 O29-C43 \\sim O29-C43A
 with sigma of 0.04
 C13-C14 \\sim C13A-C14A
 with sigma of 0.02
 C9-C10 \\sim C9A-C10A
 with sigma of 0.02
 O19-C14 \\sim O19-C14A
 with sigma of 0.02
 O31-C9 \\sim O31-C9A
 with sigma of 0.04
 O35-C76 \\sim O35-C76A
 with sigma of 0.02
 C75-C76 \\sim C75A-C76A
 with sigma of 0.02
 O17-C5 \\sim O17-C5A
 with sigma of 0.04
 O43-C62 \\sim O43-C62A
 with sigma of 0.02
 C61-C62 \\sim C61A-C62A
 with sigma of 0.02
 O69-C40 \\sim O69-C40A
 with sigma of 0.02
 C65-C66 \\sim C65A-C66A
 with sigma of 0.02
 C39-C40 \\sim C39A-C40A
 with sigma of 0.02
 O53-C65 \\sim O53-C65A
 with sigma of 0.04
 C3-C4 \\sim C3A-C4A
 with sigma of 0.02
 O21-C3 \\sim O21-C3A
 with sigma of 0.04
 C37-C38 \\sim C37A-C38A
 with sigma of 0.02
 O5-C37 \\sim O5-C37A
 with sigma of 0.04
 C55-C56 \\sim C55A-C56A
 with sigma of 0.02
 C17-C18 \\sim C17A-C18A
 with sigma of 0.02
 O56-C56 \\sim O56-C56A
 with sigma of 0.02
 O15-C17 \\sim O15-C17A
 with sigma of 0.04
 O56-C55 \\sim O56-C55A
 with sigma of 0.04
 C53-C54 \\sim C53A-C54A
 with sigma of 0.02
 O49-C53 \\sim O49-C53A
 with sigma of 0.04
 C25-C26 \\sim C25A-C26A
 with sigma of 0.02
 O65-C25 \\sim O65-C25A
 with sigma of 0.04
 O15-C18 \\sim O15-C18A
 with sigma of 0.02
 O53-C66 \\sim O53-C66A
 with sigma of 0.02
 O19-C13 \\sim O19-C13A
 with sigma of 0.04
 O49-C54 \\sim O49-C54A
 with sigma of 0.02
 O33-C42 \\sim O33-C42A
 with sigma of 0.02
 C41-C42 \\sim C41A-C42A
 with sigma of 0.02
 O33-C41 \\sim O33-C41A
 with sigma of 0.04
 O69-C39 \\sim O69-C39A
 with sigma of 0.04
 O65-C26 \\sim O65-C26A
 with sigma of 0.02
 O21-C4 \\sim O21-C4A
 with sigma of 0.02
 O25-C35 \\sim O25-C35A
 with sigma of 0.04
 O75-C8 \\sim O75-C8A
 with sigma of 0.02
 C7-C8 \\sim C7A-C8A
 with sigma of 0.02
 O75-C7 \\sim O75-C7A
 with sigma of 0.04
 O31-C10 \\sim O31-C10A
 with sigma of 0.02
 O5-C38 \\sim O5-C38A
 with sigma of 0.02
 O35-C75 \\sim O35-C75A
 with sigma of 0.04
 O29-C44 \\sim O29-C44A
 with sigma of 0.02
 O23-C70 \\sim O23-C70A
 with sigma of 0.02
 C70-C69 \\sim C70A-C69A
 with sigma of 0.02
 O23-C69 \\sim O23-C69A
 with sigma of 0.04
 O77-C46 \\sim O77-C46A
 with sigma of 0.02
 C45-C46 \\sim C45A-C46A
 with sigma of 0.02
 O77-C45 \\sim O77-C45A
 with sigma of 0.04
 O71-C34 \\sim O71-C34A
 with sigma of 0.02
 O9-C72 \\sim O9-C72A
 with sigma of 0.02
 C71-C72 \\sim C71A-C72A
 with sigma of 0.02
 O9-C71 \\sim O9-C71A
 with sigma of 0.04
 O37-C32 \\sim O37-C32A
 with sigma of 0.02
 O43-C61 \\sim O43-C61A
 with sigma of 0.04
 O55-C2 \\sim O55-C2A
 with sigma of 0.02
 C1-C2 \\sim C1A-C2A
 with sigma of 0.02
 O55-C1 \\sim O55-C1A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C65) = Uanis(C30A) = Uanis(C2) = Uanis(C40A) = Uanis(C3) =
Uanis(C31A) = Uanis(C4) = Uanis(C74) = Uanis(C5) = Uanis(C35A) = Uanis(C6) =
Uanis(C46A) = Uanis(C7) = Uanis(C8) = Uanis(C70) = Uanis(C9) = Uanis(C54A) =
Uanis(C10) = Uanis(C18A) = Uanis(C11) = Uanis(C9A) = Uanis(C12) = Uanis(C43A) =
Uanis(C13) = Uanis(C71A) = Uanis(C14) = Uanis(C65A) = Uanis(C15) = Uanis(C63) =
Uanis(C16) = Uanis(C67) = Uanis(C17) = Uanis(C72) = Uanis(C18) = Uanis(C76) =
Uanis(C19) = Uanis(C42A) = Uanis(C20) = Uanis(C26A) = Uanis(C21) = Uanis(C4A) =
Uanis(C22) = Uanis(C7A) = Uanis(C23) = Uanis(C38A) = Uanis(C24) = Uanis(C76A) =
Uanis(C25) = Uanis(C69A) = Uanis(C26) = Uanis(C33A) = Uanis(C27) = Uanis(C13A)
= Uanis(C28) = Uanis(C55A) = Uanis(C29) = Uanis(C5A) = Uanis(C30) = Uanis(C62A)
= Uanis(C31) = Uanis(C64) = Uanis(C32) = Uanis(C66) = Uanis(C33) = Uanis(C68) =
Uanis(C34) = Uanis(C71) = Uanis(C35) = Uanis(C73) = Uanis(C36) = Uanis(C75) =
Uanis(C37) = Uanis(C53A) = Uanis(C38) = Uanis(C41A) = Uanis(C39) = Uanis(C39A)
= Uanis(C40) = Uanis(C25A) = Uanis(C41) = Uanis(C17A) = Uanis(C42) = Uanis(C3A)
= Uanis(C43) = Uanis(C36A) = Uanis(C44) = Uanis(C8A) = Uanis(C45) = Uanis(C10A)
= Uanis(C46) = Uanis(C37A) = Uanis(C47) = Uanis(C29A) = Uanis(C48) =
Uanis(C75A) = Uanis(C49) = Uanis(C69) = Uanis(C50) = Uanis(C44A) = Uanis(C51) =
Uanis(C70A) = Uanis(C52) = Uanis(C45A) = Uanis(C53) = Uanis(C34A) = Uanis(C54)
= Uanis(C72A) = Uanis(C55) = Uanis(C14A) = Uanis(C56) = Uanis(C32A) =
Uanis(C57) = Uanis(C56A) = Uanis(C58) = Uanis(C66A) = Uanis(C59) = Uanis(C6A) =
Uanis(C60) = Uanis(C61A) = Uanis(C61) = Uanis(C62)
Uanis(C1) = Uanis(C2) = Uanis(C1A) = Uanis(C2A)
4. Others
 Sof(C53A)=Sof(H53D)=Sof(H53E)=Sof(H53F)=Sof(C54A)=Sof(H54C)=Sof(H54D)=1-FVAR(1)
 Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=Sof(C54)=Sof(H54A)=Sof(H54B)=FVAR(1)
 Sof(C41A)=Sof(H41D)=Sof(H41E)=Sof(H41F)=Sof(C42A)=Sof(H42C)=Sof(H42D)=1-FVAR(2)
 Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C42)=Sof(H42A)=Sof(H42B)=FVAR(2)
 Sof(C39A)=Sof(H39D)=Sof(H39E)=Sof(H39F)=Sof(C40A)=Sof(H40C)=Sof(H40D)=1-FVAR(3)
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C40)=Sof(H40A)=Sof(H40B)=FVAR(3)
 Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C26A)=Sof(H26C)=Sof(H26D)=1-FVAR(4)
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C26)=Sof(H26A)=Sof(H26B)=FVAR(4)
 Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C18A)=Sof(H18C)=Sof(H18D)=1-FVAR(5)
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18)=Sof(H18A)=Sof(H18B)=FVAR(5)
 Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=1-FVAR(6)
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(H4A)=Sof(H4B)=FVAR(6)
 Sof(C36A)=Sof(H36C)=Sof(H36D)=Sof(C35A)=Sof(H35D)=Sof(H35E)=Sof(H35F)=1-FVAR(7)
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C36)=Sof(H36A)=Sof(H36B)=FVAR(7)
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=1-FVAR(8)
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=Sof(H8A)=Sof(H8B)=FVAR(8)
 Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=1-FVAR(9)
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C10)=Sof(H10A)=Sof(H10B)=FVAR(9)
 Sof(C37A)=Sof(H37D)=Sof(H37E)=Sof(H37F)=Sof(C38A)=Sof(H38C)=Sof(H38D)=1-
 FVAR(10)
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C38)=Sof(H38A)=Sof(H38B)=FVAR(10)
 Sof(C29A)=Sof(H29D)=Sof(H29E)=Sof(H29F)=Sof(C30A)=Sof(H30C)=Sof(H30D)=1-
 FVAR(11)
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C30)=Sof(H30A)=Sof(H30B)=FVAR(11)
 Sof(C75A)=Sof(H75D)=Sof(H75E)=Sof(H75F)=Sof(C76A)=Sof(H76C)=Sof(H76D)=1-
 FVAR(12)
 Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(H75C)=Sof(C76)=Sof(H76A)=Sof(H76B)=FVAR(12)
 Sof(C43A)=Sof(H43D)=Sof(H43E)=Sof(H43F)=Sof(C44A)=Sof(H44C)=Sof(H44D)=1-
 FVAR(13)
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=Sof(C44)=Sof(H44A)=Sof(H44B)=FVAR(13)
 Sof(C69A)=Sof(H69D)=Sof(H69E)=Sof(H69F)=Sof(C70A)=Sof(H70C)=Sof(H70D)=1-
 FVAR(14)
 Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=FVAR(14)
 Sof(C46A)=Sof(H46C)=Sof(H46D)=Sof(C45A)=Sof(H45D)=Sof(H45E)=Sof(H45F)=1-
 FVAR(15)
 Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=Sof(C46)=Sof(H46A)=Sof(H46B)=FVAR(15)
 Sof(C33A)=Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(C34A)=Sof(H34C)=Sof(H34D)=1-
 FVAR(16)
 Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C34)=Sof(H34A)=Sof(H34B)=FVAR(16)
 Sof(C71A)=Sof(H71D)=Sof(H71E)=Sof(H71F)=Sof(C72A)=Sof(H72C)=Sof(H72D)=1-
 FVAR(17)
 Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=Sof(C72)=Sof(H72A)=Sof(H72B)=FVAR(17)
 Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C14A)=Sof(H14C)=Sof(H14D)=1-
 FVAR(18)
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=Sof(H14A)=Sof(H14B)=FVAR(18)
 Sof(C31A)=Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(C32A)=Sof(H32C)=Sof(H32D)=1-
 FVAR(19)
 Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C32)=Sof(H32A)=Sof(H32B)=FVAR(19)
 Sof(C55A)=Sof(H55D)=Sof(H55E)=Sof(H55F)=Sof(C56A)=Sof(H56C)=Sof(H56D)=1-
 FVAR(20)
 Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=Sof(C56)=Sof(H56A)=Sof(H56B)=FVAR(20)
 Sof(C65A)=Sof(H65D)=Sof(H65E)=Sof(H65F)=Sof(C66A)=Sof(H66C)=Sof(H66D)=1-
 FVAR(21)
 Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(H65C)=Sof(C66)=Sof(H66A)=Sof(H66B)=FVAR(21)
 Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=1-FVAR(22)
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C6)=Sof(H6A)=Sof(H6B)=FVAR(22)
 Sof(C61A)=Sof(H61D)=Sof(H61E)=Sof(H61F)=Sof(C62A)=Sof(H62C)=Sof(H62D)=1-
 FVAR(23)
 Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(H61C)=Sof(C62)=Sof(H62A)=Sof(H62B)=FVAR(23)
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=1-FVAR(24)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=Sof(H2A)=Sof(H2B)=FVAR(24)
 Fixed X: C5(0.81352) C6(0.79531) C9(0.945809) C13(0.87392) C14(0.81577)
 C17(0.641181) C18(0.643721) C23(1.04081) C25(1.032749) C27(1.108941)
 C29(1.14261) C30(1.09696) C33(0.996169) C36(0.84464) C37(1.083409)
 C40(1.08399) C43(0.60055) C53(0.206349) C55(0.37222) C56(0.352469)
 C62(0.263921) C66(0.511061) C67(0.58876) C76(0.71964) C43A(0.47184)
 Fixed Y: C5(-0.18455) C6(-0.15638) C9(-0.23946) C13(-0.28827) C14(-0.23306)
 C17(0.53006) C18(0.54226) C23(0.374269) C25(0.4237) C27(0.19677) C29(-0.04885)
 C30(-0.00784) C33(0.3075) C36(0.12623) C37(0.055409) C40(-0.13443) C43(-
 0.139759) C53(0.434639) C55(0.028241) C56(0.113161) C62(0.66699) C66(0.698981)
 C67(0.35696) C76(0.521291) C43A(-0.049541)
 Fixed Z: C5(0.573999) C6(0.625811) C9(0.744129) C13(0.90596) C14(0.870469)
 C17(0.447189) C18(0.499539) C23(0.57091) C25(0.81579) C27(0.760381)
 C29(0.71783) C30(0.67493) C33(0.970969) C36(0.984269) C37(0.918509)
 C40(0.85103) C43(0.868071) C53(0.644549) C55(0.63809) C56(0.660941)
 C62(0.65565) C66(0.847361) C67(0.986669) C76(0.89978) C43A(0.916049)
5.a Riding coordinates:
 C3(H3A,H3B,H3C), C65(H65A,H65B,H65C), C41A(H41D,H41E,H41F), C3A(H3AA,H3AB,
 H3AC), C33A(H33D,H33E,H33F), C71A(H71D,H71E,H71F), C31A(H31D,H31E,H31F),
 C65A(H65D,H65E,H65F)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C6(H6A,H6B), C8(H8A,H8B), C10(H10A,H10B), C12(H12A,
 H12B), C14(H14A,H14B), C16(H16A,H16B), C18(H18A,H18B), C20(H20A,H20B),
 C22(H22A,H22B), C24(H24A,H24B), C26(H26A,H26B), C28(H28A,H28B), C30(H30A,H30B),
  C32(H32A,H32B), C34(H34A,H34B), C36(H36A,H36B), C38(H38A,H38B), C40(H40A,
 H40B), C42(H42A,H42B), C44(H44A,H44B), C46(H46A,H46B), C48(H48A,H48B),
 C50(H50A,H50B), C52(H52A,H52B), C54(H54A,H54B), C56(H56A,H56B), C58(H58A,H58B),
  C60(H60A,H60B), C62(H62A,H62B), C64(H64A,H64B), C66(H66A,H66B), C68(H68A,
 H68B), C70(H70A,H70B), C72(H72A,H72B), C74(H74A,H74B), C76(H76A,H76B),
 C54A(H54C,H54D), C42A(H42C,H42D), C40A(H40C,H40D), C26A(H26C,H26D), C18A(H18C,
 H18D), C4A(H4AA,H4AB), C36A(H36C,H36D), C8A(H8AA,H8AB), C10A(H10C,H10D),
 C38A(H38C,H38D), C30A(H30C,H30D), C76A(H76C,H76D), C44A(H44C,H44D), C70A(H70C,
 H70D), C46A(H46C,H46D), C34A(H34C,H34D), C72A(H72C,H72D), C14A(H14C,H14D),
 C32A(H32C,H32D), C56A(H56C,H56D), C66A(H66C,H66D), C6A(H6AA,H6AB), C62A(H62C,
 H62D), C2A(H2AA,H2AB)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C11(H11A,
 H11B,H11C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C),
 C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C25(H25A,H25B,
 H25C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C33(H33A,
 H33B,H33C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C),
 C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C47(H47A,H47B,
 H47C), C49(H49A,H49B,H49C), C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C55(H55A,
 H55B,H55C), C57(H57A,H57B,H57C), C59(H59A,H59B,H59C), C61(H61A,H61B,H61C),
 C63(H63A,H63B,H63C), C67(H67A,H67B,H67C), C71(H71A,H71B,H71C), C73(H73A,H73B,
 H73C), C75(H75A,H75B,H75C), C53A(H53D,H53E,H53F), C39A(H39D,H39E,H39F),
 C25A(H25D,H25E,H25F), C17A(H17D,H17E,H17F), C35A(H35D,H35E,H35F), C7A(H7AA,
 H7AB,H7AC), C9A(H9AA,H9AB,H9AC), C37A(H37D,H37E,H37F), C29A(H29D,H29E,H29F),
 C75A(H75D,H75E,H75F), C69(H69A,H69B,H69C), C43A(H43D,H43E,H43F), C69A(H69D,
 H69E,H69F), C45A(H45D,H45E,H45F), C13A(H13D,H13E,H13F), C55A(H55D,H55E,H55F),
 C5A(H5AA,H5AB,H5AC), C61A(H61D,H61E,H61F), C1A(H1AA,H1AB,H1AC)
;
_shelx_res_checksum              2687
_olex2_submission_special_instructions 'No special instructions were received'