Ti3C3@C2v(9)-C82: a double-butterfly tri-metal carbide cluster inside a fullerene cage
He, Zhiwen; Cao, Zhengkai; Yao, Yang-Rong; Chen, Ning; Chemical Communications 61 (2025) 9432–9435; doi:10.1039/D5CC02276B

data_7134565
_publ_section_title
;
 Ti3C3@C2v(9)-C82: a double-butterfly tri-metal carbide cluster inside a
 fullerene cage
;
_journal_issue                   52
_journal_name_full               'Chemical Communications'
_journal_page_first              9432
_journal_page_last               9435
_journal_paper_doi               10.1039/D5CC02276B
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C85 Ti3, C36 H44 N4 Ni, 1.5[C6H6], 1[CS2]'
_chemical_formula_sum            'C131 H53 N4 Ni S2 Ti3'
_chemical_formula_weight         1949.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-05-18
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_audit_update_record
;
2025-05-19 deposited with the CCDC.	2025-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.180(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.6365(12)
_cell_length_b                   17.0732(14)
_cell_length_c                   17.8293(9)
_cell_measurement_reflns_used    9484
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      64.6430
_cell_measurement_theta_min      2.5940
_cell_volume                     7703.5(8)
_computing_cell_refinement       'CrysAlisPro 1.171.43.112a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.112a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.112a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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     30.00  79.00   0.50    3.00    --   64.66-125.00 -30.00   98
  2  \w     38.00  79.00   0.50    3.00    --   64.66-125.00-180.00   82
  3  \w     62.00  88.00   0.50    3.00    --   64.66  15.00-180.00   52
  4  \w     60.00  90.00   0.50    3.00    --   64.66  15.00 120.00   60
  5  \w     61.00  98.00   0.50    3.00    --   64.66  15.00  60.00   74
  6  \w     39.00  65.00   0.50    3.00    --   64.66-125.00 -90.00   52
  7  \w     60.00  90.00   0.50    3.00    --   64.66  15.00  30.00   60
  8  \w     78.00 103.00   0.50    3.00    --   64.66  15.00 -30.00   50
  9  \w     67.00  97.00   0.50    3.00    --   69.32  15.00 120.00   60
 10  \w     38.00  86.00   0.50    3.00    --   69.32-125.00-150.00   96
 11  \w   -106.00 -72.00   0.50    8.88    --  -77.20 -15.00  30.00   68
 12  \w   -119.00 -71.00   0.50    8.88    --  -77.20 -15.00 -30.00   96
 13  \w   -108.00 -79.00   0.50    8.88    --  -77.20 -15.00-150.00   58
 14  \w   -102.00 -71.00   0.50    8.88    --  -77.20 -15.00  60.00   62
 15  \w   -112.00 -84.00   0.50    8.88    --  -77.33 -15.00 -90.00   56
 16  \w    -79.00 -54.00   0.50    8.88    --  -77.33 125.00  60.00   50
 17  \w    -96.00 -69.00   0.50    8.88    --  -80.50 137.00-162.23   54
 18  \w   -100.00 -71.00   0.50    8.88    --  -80.50 128.00 135.29   58
 19  \w    -90.00 -41.00   0.50    8.88    --  -80.50 122.00 -36.88   98
 20  \w    -91.00 -46.00   0.50    8.88    --  -80.50 116.00-117.20   90
 21  \w   -104.00 -78.00   0.50    8.88    --  -80.50 136.00 161.69   52
 22  \w    -70.00 -45.00   0.50    8.88    --  -80.50 116.00 -53.39   50
 23  \w    -80.00 -54.00   0.50    8.88    --  -80.50 118.00 -90.69   52
 24  \w   -102.00 -55.00   0.50    8.88    --  -80.50 132.00 142.03   94
 25  \w    -73.00 -48.00   0.50    8.88    --  -80.50 126.00-135.49   50
 26  \w   -103.00 -75.00   0.50    8.88    --  -80.50 134.00  63.69   56
 27  \w    -81.00 -45.00   0.50    8.88    --  -80.50  99.00 145.80   72
 28  \w    -77.00 -52.00   0.50    8.88    --  -80.50 118.00  -9.88   50
 29  \w    -70.00 -45.00   0.50    8.88    --  -80.50  99.00 -67.55   50
 30  \w    -92.00 -42.00   0.50    8.88    --  -80.50 137.00  77.78  100
 31  \w    -79.00 -54.00   0.50    8.88    --  -80.50 101.00 -45.07   50
 32  \w    -93.00 -41.00   0.50    8.88    --  -80.50 124.00  30.07  104
 33  \w    -70.00 -45.00   0.50    8.88    --  -80.50 101.00  24.72   50
 34  \w    -69.00 -42.00   0.50    8.88    --  -80.50 136.00-159.74   54
 35  \w    -99.00 -67.00   0.50    8.88    --  -80.50 126.00 112.86   64
 36  \w    -91.00 -65.00   0.50    8.88    --  -80.50 126.00  39.83   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37397
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.244
_diffrn_reflns_theta_min         2.608
_exptl_absorpt_coefficient_mu    3.889
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.112a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_description       block
_exptl_crystal_F_000             3972
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1186
_refine_ls_number_reflns         7279
_refine_ls_number_restraints     1699
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.2019
_refine_ls_R_factor_gt           0.1394
_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^)+(0.0743P)^2^+74.4310P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2975
_refine_ls_wR_factor_ref         0.3357
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3646
_reflns_number_total             7279
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc02276b2.cif
_cod_data_source_block           ti3c3@c2v(9)-c82
_cod_depositor_comments          'Adding full bibliography for 7134565.cif.'
_cod_database_code               7134565
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.892
_shelx_estimated_absorpt_t_min   0.829
_diffrn_oxdiff_digest_hkl
;
43e709b82004bb08e30c721c8c07839ad3b85e
;
_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
 C24-C45 = C28-C49 = C61-C62 = C64-C65 = C70-C69 = C72-C73
 1.4 with sigma of 0.01
 N1P-C1P \\sim N1P-C18P \\sim N2P-C3P \\sim N2P-C6P \\sim N3P-C8P \\sim
N3P-C11P \\sim N4P-C13P \\sim N4P-
 C16P
 with sigma of 0.02
 N1P-C19P \\sim N1P-C20P \\sim N2P-C4P \\sim N2P-C5P \\sim N3P-C9P \\sim
N3P-C10P \\sim N4P-C14P \\sim N4P-
 C15P
 with sigma of 0.02
 C1P-C2P \\sim C2P-C3P \\sim C6P-C7P \\sim C7P-C8P \\sim C11P-C12P \\sim
C12P-C13P \\sim C16P-C17P ~
 C17P-C18P
 with sigma of 0.02
 C8P-C10P \\sim C9P-C11P \\sim C3P-C5P \\sim C4P-C6P \\sim C1P-C19P \\sim
C18P-C20P \\sim C16P-C14P ~
 C15P-C13P
 with sigma of 0.02
 C21P-C22P \\sim C23P-C24P \\sim C25P-C26P \\sim C27P-C28P \\sim C29P-C30P
\\sim C31P-C32P \\sim C33P-
 C34P \\sim C35P-C36P
 with sigma of 0.02
 C4P-C23P \\sim C5P-C25P \\sim C9P-C27P \\sim C10P-C29P \\sim C14P-C31P \\sim
C15P-C33P \\sim C19P-
 C35P \\sim C20P-C21P
 with sigma of 0.02
 Ni1P-N1P \\sim Ni1P-N2P \\sim Ni1P-N3P \\sim Ni1P-N4P
 with sigma of 0.02
 C1-C2 \\sim C2-C3 \\sim C3-C4 \\sim C4-C5 \\sim C5-C1
 with sigma of 0.02
 C1-C3 \\sim C1-C4 \\sim C2-C4 \\sim C2-C5 \\sim C3-C5
 with sigma of 0.02
 C8-C7 \\sim C7-C23 \\sim C23-C24 \\sim C24-C25 \\sim C25-C8
 with sigma of 0.02
 C8-C23 \\sim C8-C24 \\sim C7-C24 \\sim C7-C25 \\sim C23-C25
 with sigma of 0.02
 C11-C10 \\sim C10-C27 \\sim C27-C28 \\sim C28-C29 \\sim C29-C11
 with sigma of 0.02
 C11-C27 \\sim C11-C28 \\sim C10-C28 \\sim C10-C29 \\sim C27-C29
 with sigma of 0.02
 C49-C48 \\sim C48-C68 \\sim C68-C69 \\sim C69-C50 \\sim C50-C49
 with sigma of 0.02
 C49-C68 \\sim C49-C69 \\sim C48-C69 \\sim C48-C50 \\sim C68-C50
 with sigma of 0.02
 C46-C45 \\sim C45-C44 \\sim C44-C65 \\sim C65-C66 \\sim C66-C46
 with sigma of 0.02
 C46-C44 \\sim C46-C65 \\sim C45-C65 \\sim C45-C66 \\sim C44-C66
 with sigma of 0.02
 C70-C81 \\sim C81-C82 \\sim C82-C72 \\sim C72-C71 \\sim C71-C70
 with sigma of 0.02
 C70-C82 \\sim C70-C72 \\sim C81-C72 \\sim C81-C71 \\sim C82-C71
 with sigma of 0.02
 C79-C64 \\sim C64-C63 \\sim C63-C62 \\sim C62-C78 \\sim C78-C79
 with sigma of 0.02
 C79-C63 \\sim C79-C62 \\sim C64-C62 \\sim C64-C78 \\sim C63-C78
 with sigma of 0.02
 C73-C74 \\sim C74-C56 \\sim C56-C55 \\sim C55-C54 \\sim C54-C73
 with sigma of 0.02
 C73-C56 \\sim C73-C55 \\sim C74-C55 \\sim C74-C54 \\sim C56-C54
 with sigma of 0.02
 C76-C61 \\sim C61-C60 \\sim C60-C59 \\sim C59-C58 \\sim C58-C76
 with sigma of 0.02
 C76-C60 \\sim C76-C59 \\sim C61-C59 \\sim C61-C58 \\sim C60-C58
 with sigma of 0.02
 C36-C37 \\sim C37-C17 \\sim C17-C16 \\sim C16-C35 \\sim C35-C36
 with sigma of 0.02
 C36-C17 \\sim C36-C16 \\sim C37-C16 \\sim C37-C35 \\sim C17-C35
 with sigma of 0.02
 C32-C33 \\sim C33-C14 \\sim C14-C13 \\sim C13-C31 \\sim C31-C32
 with sigma of 0.02
 C32-C14 \\sim C32-C13 \\sim C33-C13 \\sim C33-C31 \\sim C14-C31
 with sigma of 0.02
 C40-C21 \\sim C21-C20 \\sim C20-C19 \\sim C19-C39 \\sim C39-C40
 with sigma of 0.02
 C40-C20 \\sim C40-C19 \\sim C21-C19 \\sim C21-C39 \\sim C20-C39
 with sigma of 0.02
 C24-C44 \\sim C24-C46 \\sim C45-C25 \\sim C45-C23
 with sigma of 0.02
 C28-C48 \\sim C28-C50 \\sim C49-C27 \\sim C49-C29
 with sigma of 0.02
 C62-C60 \\sim C62-C76 \\sim C61-C63 \\sim C61-C78
 with sigma of 0.02
 C64-C66 \\sim C64-C44 \\sim C65-C63 \\sim C65-C79
 with sigma of 0.02
 C69-C71 \\sim C69-C81 \\sim C70-C50 \\sim C70-C68
 with sigma of 0.02
 C72-C74 \\sim C72-C54 \\sim C73-C71 \\sim C73-C82
 with sigma of 0.02
 C6-C5 \\sim C6-C7 \\sim C6-C20
 with sigma of 0.02
 C5-C7 \\sim C7-C20 \\sim C20-C5
 with sigma of 0.02
 C9-C8 \\sim C9-C10 \\sim C9-C1
 with sigma of 0.02
 C8-C10 \\sim C10-C1 \\sim C1-C8
 with sigma of 0.02
 C12-C11 \\sim C12-C13 \\sim C12-C2
 with sigma of 0.02
 C11-C13 \\sim C13-C2 \\sim C2-C11
 with sigma of 0.02
 C15-C14 \\sim C15-C16 \\sim C15-C3
 with sigma of 0.02
 C14-C16 \\sim C16-C3 \\sim C3-C14
 with sigma of 0.02
 C18-C17 \\sim C18-C19 \\sim C18-C4
 with sigma of 0.02
 C17-C19 \\sim C19-C4 \\sim C4-C17
 with sigma of 0.02
 C22-C21 \\sim C22-C23 \\sim C22-C43
 with sigma of 0.02
 C21-C23 \\sim C23-C43 \\sim C43-C21
 with sigma of 0.02
 C26-C25 \\sim C26-C27 \\sim C26-C47
 with sigma of 0.02
 C25-C27 \\sim C27-C47 \\sim C47-C25
 with sigma of 0.02
 C30-C29 \\sim C30-C31 \\sim C30-C51
 with sigma of 0.02
 C29-C31 \\sim C31-C51 \\sim C51-C29
 with sigma of 0.02
 C34-C33 \\sim C34-C35 \\sim C34-C55
 with sigma of 0.02
 C33-C35 \\sim C35-C55 \\sim C55-C33
 with sigma of 0.02
 C38-C37 \\sim C38-C39 \\sim C38-C59
 with sigma of 0.02
 C37-C39 \\sim C39-C59 \\sim C59-C37
 with sigma of 0.02
 C41-C40 \\sim C41-C42 \\sim C41-C60
 with sigma of 0.02
 C40-C42 \\sim C42-C60 \\sim C60-C40
 with sigma of 0.02
 C42-C41 \\sim C42-C43 \\sim C42-C63
 with sigma of 0.02
 C41-C43 \\sim C43-C63 \\sim C63-C41
 with sigma of 0.02
 C47-C46 \\sim C47-C48 \\sim C47-C26
 with sigma of 0.02
 C46-C48 \\sim C48-C26 \\sim C26-C46
 with sigma of 0.02
 C51-C50 \\sim C51-C52 \\sim C51-C30
 with sigma of 0.02
 C50-C52 \\sim C52-C30 \\sim C30-C50
 with sigma of 0.02
 C52-C51 \\sim C52-C53 \\sim C52-C71
 with sigma of 0.02
 C51-C53 \\sim C53-C71 \\sim C71-C51
 with sigma of 0.02
 C53-C52 \\sim C53-C54 \\sim C53-C32
 with sigma of 0.02
 C52-C54 \\sim C54-C32 \\sim C32-C52
 with sigma of 0.02
 C57-C56 \\sim C57-C58 \\sim C57-C36
 with sigma of 0.02
 C56-C58 \\sim C58-C36 \\sim C36-C56
 with sigma of 0.02
 C67-C66 \\sim C67-C68 \\sim C67-C80
 with sigma of 0.02
 C66-C68 \\sim C68-C80 \\sim C80-C66
 with sigma of 0.02
 C75-C74 \\sim C75-C76 \\sim C75-C77
 with sigma of 0.02
 C74-C76 \\sim C76-C77 \\sim C77-C74
 with sigma of 0.02
 C77-C75 \\sim C77-C78 \\sim C77-C82
 with sigma of 0.02
 C75-C78 \\sim C78-C82 \\sim C82-C75
 with sigma of 0.02
 C80-C81 \\sim C80-C79 \\sim C80-C67
 with sigma of 0.02
 C79-C81 \\sim C81-C67 \\sim C67-C79
 with sigma of 0.02
3. Restrained planarity
 C1, C2, C3, C4, C5
 with sigma of 0.1
 C7, C8, C23, C24, C25
 with sigma of 0.1
 C10, C11, C27, C28, C29
 with sigma of 0.1
 C48, C49, C50, C68, C69
 with sigma of 0.1
 C44, C45, C46, C65, C66
 with sigma of 0.1
 C70, C71, C72, C81, C82
 with sigma of 0.1
 C62, C63, C64, C78, C79
 with sigma of 0.1
 C54, C55, C56, C73, C74
 with sigma of 0.1
 C58, C59, C60, C61, C76
 with sigma of 0.1
 C16, C17, C35, C36, C37
 with sigma of 0.1
 C13, C14, C31, C32, C33
 with sigma of 0.1
 C19, C20, C21, C39, C40
 with sigma of 0.1
 C6, C7, C20, C21, C22, C23
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C83 \\sim C84 \\sim C85: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Ni1P \\sim N1P \\sim N2P \\sim N3P \\sim N4P \\sim C1P \\sim C2P \\sim C3P
\\sim C4P \\sim C5P \\sim C6P \\sim C7P \\sim C8P \\sim C9P \\sim C10P \\sim
C11P \\sim C12P \\sim C13P \\sim C14P \\sim C15P \\sim C16P \\sim C17P \\sim
C18P \\sim C19P \\sim C20P \\sim C21P \\sim C22P \\sim C23P \\sim C24P \\sim
C25P \\sim C26P \\sim C27P \\sim C28P \\sim C29P \\sim C30P \\sim C31P \\sim
C32P \\sim C33P \\sim C34P \\sim C35P \\sim C36P: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49
\\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57
\\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65
\\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73
\\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81
\\sim C82: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 2A
Ti1 \\sim Ti2 \\sim Ti3 \\sim Ti4 \\sim Ti5 \\sim Ti6: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
5. Others
 Sof(Ti4)=Sof(Ti5)=Sof(Ti6)=0.5*(1-FVAR(2))
 Sof(Ti1)=Sof(Ti2)=Sof(Ti3)=0.5*FVAR(2)
 Fixed Sof: C1(0.5) C2(0.5) C3(0.5) C4(0.5) C5(0.5) C6(0.5) C7(0.5) C8(0.5)
 C9(0.5) C10(0.5) C11(0.5) C12(0.5) C13(0.5) C14(0.5) C15(0.5) C16(0.5)
 C17(0.5) C18(0.5) C19(0.5) C21(0.5) C22(0.5) C23(0.5) C24(0.5) C25(0.5)
 C26(0.5) C27(0.5) C28(0.5) C29(0.5) C30(0.5) C31(0.5) C32(0.5) C33(0.5)
 C34(0.5) C35(0.5) C36(0.5) C37(0.5) C38(0.5) C39(0.5) C40(0.5) C41(0.5)
 C42(0.5) C43(0.5) C44(0.5) C45(0.5) C46(0.5) C47(0.5) C48(0.5) C49(0.5)
 C50(0.5) C51(0.5) C52(0.5) C53(0.5) C54(0.5) C55(0.5) C56(0.5) C57(0.5)
 C58(0.5) C59(0.5) C60(0.5) C61(0.5) C62(0.5) C64(0.5) C65(0.5) C66(0.5)
 C67(0.5) C68(0.5) C69(0.5) C70(0.5) C71(0.5) C72(0.5) C73(0.5) C74(0.5)
 C75(0.5) C76(0.5) C77(0.5) C78(0.5) C79(0.5) C80(0.5) C81(0.5) C82(0.5)
 C83(0.5) C85(0.5) Ni1P(0.5) N1P(0.5) N2P(0.5) N3P(0.5) N4P(0.5) C1P(0.5)
 C2P(0.5) H2P(0.5) C3P(0.5) C4P(0.5) C5P(0.5) C6P(0.5) C7P(0.5) H7P(0.5)
 C8P(0.5) C9P(0.5) C10P(0.5) C11P(0.5) C12P(0.5) H12P(0.5) C13P(0.5) C14P(0.5)
 C15P(0.5) C16P(0.5) C17P(0.5) H17P(0.5) C18P(0.5) C19P(0.5) C20P(0.5)
 C21P(0.5) H21A(0.5) H21B(0.5) C22P(0.5) H22A(0.5) H22B(0.5) H22C(0.5)
 C23P(0.5) H23A(0.5) H23B(0.5) C24P(0.5) H24A(0.5) H24B(0.5) H24C(0.5)
 C25P(0.5) H25A(0.5) H25B(0.5) C26P(0.5) H26A(0.5) H26B(0.5) H26C(0.5)
 C27P(0.5) H27A(0.5) H27B(0.5) C28P(0.5) H28A(0.5) H28B(0.5) H28C(0.5)
 C29P(0.5) H29A(0.5) H29B(0.5) C30P(0.5) H30A(0.5) H30B(0.5) H30C(0.5)
 C31P(0.5) H31A(0.5) H31B(0.5) C32P(0.5) H32A(0.5) H32B(0.5) H32C(0.5)
 C33P(0.5) H33A(0.5) H33B(0.5) C34P(0.5) H34A(0.5) H34B(0.5) H34C(0.5)
 C35P(0.5) H35A(0.5) H35B(0.5) C36P(0.5) H36A(0.5) H36B(0.5) H36C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C21P(H21A,H21B), C23P(H23A,H23B), C25P(H25A,H25B), C27P(H27A,H27B), C29P(H29A,
 H29B), C31P(H31A,H31B), C33P(H33A,H33B), C35P(H35A,H35B)
6.b Aromatic/amide H refined with riding coordinates:
 C2P(H2P), C7P(H7P), C12P(H12P), C17P(H17P)
6.c Idealised Me refined as rotating group:
 C22P(H22A,H22B,H22C), C24P(H24A,H24B,H24C), C26P(H26A,H26B,H26C), C28P(H28A,
 H28B,H28C), C30P(H30A,H30B,H30C), C32P(H32A,H32B,H32C), C34P(H34A,H34B,H34C),
 C36P(H36A,H36B,H36C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 566 electrons were 
found in a volume of 1380\%A^3^ in 1 void per unit cell. 
The masked solvent molecules are  
1.5[C6H6], 1[CS2] per Asymmetric Unit 
which account for 404 electrons 
per unit cell. The differences of electrons are due to 
the diffuse electron density in the voids.
;
_shelx_res_checksum              29045
_shelx_hkl_checksum              70257
_shelx_fab_checksum              76465
_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 1.704
_oxdiff_exptl_absorpt_empirical_full_min 0.710