A homologous series of macrocyclic Ni clusters: synthesis, structures, and catalytic properties.
Xiang, Huixin; Cheng, Ranran; Ruan, Chenhao; Meng, Changqing; Gan, Yuzheng; Cheng, Wanyu; Zhao, Yue; Xu, Cong-Qiao; Li, Jun; Yao, Chuanhao; Nanoscale 16 (2024) 4563–4570; doi:10.1039/d3nr06015b

data_1570893
_publ_section_title
;
 A homologous series of macrocyclic Ni clusters: synthesis, structures,
 and catalytic properties.
;
_journal_issue                   9
_journal_name_full               Nanoscale
_journal_page_first              4563
_journal_page_last               4570
_journal_paper_doi               10.1039/d3nr06015b
_journal_volume                  16
_journal_year                    2024
_chemical_formula_moiety         'C126 H126 Ni9 S18'
_chemical_formula_sum            'C126 H126 Ni9 S18'
_chemical_formula_weight         2745.73
_chemical_name_systematic        Ni9(pMPT)18
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-22
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2023-11-14 deposited with the CCDC.	2024-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   28.916(7)
_cell_length_b                   28.916(7)
_cell_length_c                   69.42(3)
_cell_measurement_reflns_used    9243
_cell_measurement_temperature    173.00
_cell_measurement_theta_max      47.41
_cell_measurement_theta_min      2.66
_cell_volume                     50268(3)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2019)'
_computing_data_collection       'Bruker BIS V6.2.14'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2019)'
_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      173.00
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Metaljet PHOTON III'
_diffrn_measurement_method       '\w and \f shutterless scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_monochromator  'Helios Multi-layer Optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.1127
_diffrn_reflns_av_unetI/netI     0.0612
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       87
_diffrn_reflns_limit_l_min       -87
_diffrn_reflns_number            163359
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         57.450
_diffrn_reflns_theta_min         1.893
_diffrn_source                   MetalJet
_diffrn_source_current           2.86
_diffrn_source_power             0.19931339999999997
_diffrn_source_type              'Liquid Metal source'
_diffrn_source_voltage           69.69
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.969
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.5098
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1633 before and 0.1004 after correction.
The Ratio of minimum to maximum transmission is 0.6786.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.088
_exptl_crystal_description       block
_exptl_crystal_F_000             17064
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.789
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         11546
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1175P)^2^+67.3417P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1969
_refine_ls_wR_factor_ref         0.2151
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7529
_reflns_number_total             11546
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nr06015b2.cif
_cod_data_source_block           a_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 1570892--1570895.cif.
;
_cod_original_cell_volume        50265(30)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               1570893
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.542
_shelx_estimated_absorpt_t_min   0.464
_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. Uiso/Uaniso restraints and constraints
C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C29: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01 within 2A
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01 within 2A
3.a Aromatic/amide H refined with riding coordinates:
 C30(H30), C31(H31), C33(H33), C34(H34), C13(H13), C9(H9), C41(H41), C12(H12),
 C37(H37), C20(H20), C10(H10), C40(H40), C6(H6), C16(H16), C17(H17), C23(H23),
 C27(H27), C5(H5), C19(H19), C2(H2), C38(H38), C24(H24), C26(H26), C3(H3)
3.b Fitted hexagon refined as free rotating group:
 C29(C30,C31,C32,C33,C34)
3.c Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C14(H14A,H14B,H14C), C7(H7A,H7B,H7C), C42(H42A,H42B,
 H42C), C21(H21A,H21B,H21C), C28(H28A,H28B,H28C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              18008
_shelx_hkl_checksum              58382
_shelx_fab_checksum              88962
_olex2_submission_special_instructions 'No special instructions were received'