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_1570895
_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         'C154 H154 Ni11 S22'
_chemical_formula_sum            'C154 H154 Ni11 S22'
_chemical_formula_weight         3355.89
_chemical_name_systematic        Ni11(pMPT)22
_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   geom
_audit_creation_date             2023-11-13
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-11-14 deposited with the CCDC.	2024-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                90.121(7)
_cell_angle_beta                 90.422(7)
_cell_angle_gamma                98.048(7)
_cell_formula_units_Z            4
_cell_length_a                   23.683(3)
_cell_length_b                   27.568(4)
_cell_length_c                   29.823(4)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      47.527
_cell_measurement_theta_min      2.578
_cell_volume                     19279(5)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2019)'
_computing_data_collection       'APEX5 V2023.9-2 (Bruker, 2023)'
_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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193.00
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON II'
_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  0.1862
_diffrn_reflns_av_unetI/netI     0.2219
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            190714
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        51.249
_diffrn_reflns_theta_max         51.249
_diffrn_reflns_theta_min         1.639
_diffrn_source                   MetalJet
_diffrn_source_type              'Liquid Metal source'
_exptl_absorpt_coefficient_mu    7.403
_exptl_absorpt_correction_T_max  0.2972
_exptl_absorpt_correction_T_min  0.1203
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction:
Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48
(2015) 3-10
;
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_description       block
_exptl_crystal_F_000             6952
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.273
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     3391
_refine_ls_number_reflns         62991
_refine_ls_number_restraints     27601
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.3337
_refine_ls_R_factor_gt           0.1480
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3939
_refine_ls_wR_factor_ref         0.4836
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15826
_reflns_number_total             62991
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nr06015b2.cif
_cod_data_source_block           p-1_a_sq_sq
_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.

2025-05-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C308 H308 Ag0 Ni22 S44'
_cod_original_formula_weight         6711.79
_cod_original_formula_moiety         '2(C154 H154 Ni11 S22)'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        19279(4)
_cod_database_code               1570895
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.555
_shelx_estimated_absorpt_t_min   0.446
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.530(2)
 0.470(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 S1_32-S1_33
 2.8 with sigma of 0.01
 S1_41-S1_44
 2.8 with sigma of 0.01
 C7_3-C3_3 \\sim C7_3-C5_3
 C7_4-C3_4 \\sim C7_4-C5_4
 C7_5-C3_5 \\sim C7_5-C5_5
 C7_6-C3_6 \\sim C7_6-C5_6
 C7_7-C3_7 \\sim C7_7-C5_7
 C7_8-C3_8 \\sim C7_8-C5_8
 C7_9-C3_9 \\sim C7_9-C5_9
 C7_10-C3_10 \\sim C7_10-C5_10
 C7_11-C3_11 \\sim C7_11-C5_11
 C7_12-C3_12 \\sim C7_12-C5_12
 C7_13-C3_13 \\sim C7_13-C5_13
 C7_14-C3_14 \\sim C7_14-C5_14
 C7_15-C3_15 \\sim C7_15-C5_15
 C7_16-C3_16 \\sim C7_16-C5_16
 C7_17-C3_17 \\sim C7_17-C5_17
 C7_18-C3_18 \\sim C7_18-C5_18
 C7_19-C3_19 \\sim C7_19-C5_19
 C7_21-C3_21 \\sim C7_21-C5_21
 C7_22-C3_22 \\sim C7_22-C5_22
 C7_23-C3_23 \\sim C7_23-C5_23
 C7_24-C3_24 \\sim C7_24-C5_24
 C7_25-C3_25 \\sim C7_25-C5_25
 C7_26-C3_26 \\sim C7_26-C5_26
 C7_27-C3_27 \\sim C7_27-C5_27
 C7_28-C3_28 \\sim C7_28-C5_28
 C7_29-C3_29 \\sim C7_29-C5_29
 C7_30-C3_30 \\sim C7_30-C5_30
 C7_31-C3_31 \\sim C7_31-C5_31
 C7_32-C3_32 \\sim C7_32-C5_32
 C7_33-C3_33 \\sim C7_33-C5_33
 C7_34-C3_34 \\sim C7_34-C5_34
 C7_35-C3_35 \\sim C7_35-C5_35
 C7_36-C3_36 \\sim C7_36-C5_36
 C7_37-C3_37 \\sim C7_37-C5_37
 C7_38-C3_38 \\sim C7_38-C5_38
 C7_39-C3_39 \\sim C7_39-C5_39
 C7_40-C3_40 \\sim C7_40-C5_40
 C7_41-C3_41 \\sim C7_41-C5_41
 C7_42-C3_42 \\sim C7_42-C5_42
 C7_44-C3_44 \\sim C7_44-C5_44
 C7_45-C3_45 \\sim C7_45-C5_45
 C7_46-C3_46 \\sim C7_46-C5_46
 C7_47-C3_47 \\sim C7_47-C5_47
 C7_43-C3_43 \\sim C7_43-C5_43
 with sigma of 0.01
4. Restrained planarity
 S1_3, C1_3, C2_3, C3_3, C4_3, C5_3, C6_3, C7_3
 S1_4, C1_4, C2_4, C3_4, C4_4, C5_4, C6_4, C7_4
 S1_5, C1_5, C2_5, C3_5, C4_5, C5_5, C6_5, C7_5
 S1_6, C1_6, C2_6, C3_6, C4_6, C5_6, C6_6, C7_6
 S1_7, C1_7, C2_7, C3_7, C4_7, C5_7, C6_7, C7_7
 S1_8, C1_8, C2_8, C3_8, C4_8, C5_8, C6_8, C7_8
 S1_9, C1_9, C2_9, C3_9, C4_9, C5_9, C6_9, C7_9
 S1_10, C1_10, C2_10, C3_10, C4_10, C5_10, C6_10, C7_10
 S1_11, C1_11, C2_11, C3_11, C4_11, C5_11, C6_11, C7_11
 S1_12, C1_12, C2_12, C3_12, C4_12, C5_12, C6_12, C7_12
 S1_13, C1_13, C2_13, C3_13, C4_13, C5_13, C6_13, C7_13
 S1_14, C1_14, C2_14, C3_14, C4_14, C5_14, C6_14, C7_14
 S1_15, C1_15, C2_15, C3_15, C4_15, C5_15, C6_15, C7_15
 S1_16, C1_16, C2_16, C3_16, C4_16, C5_16, C6_16, C7_16
 S1_17, C1_17, C2_17, C3_17, C4_17, C5_17, C6_17, C7_17
 S1_18, C1_18, C2_18, C3_18, C4_18, C5_18, C6_18, C7_18
 S1_19, C1_19, C2_19, C3_19, C4_19, C5_19, C6_19, C7_19
 S1_21, C1_21, C2_21, C3_21, C4_21, C5_21, C6_21, C7_21
 S1_22, C1_22, C2_22, C3_22, C4_22, C5_22, C6_22, C7_22
 S1_23, C1_23, C2_23, C3_23, C4_23, C5_23, C6_23, C7_23
 S1_24, C1_24, C2_24, C3_24, C4_24, C5_24, C6_24, C7_24
 S1_25, C1_25, C2_25, C3_25, C4_25, C5_25, C6_25, C7_25
 S1_26, C1_26, C2_26, C3_26, C4_26, C5_26, C6_26, C7_26
 S1_27, C1_27, C2_27, C3_27, C4_27, C5_27, C6_27, C7_27
 S1_28, C1_28, C2_28, C3_28, C4_28, C5_28, C6_28, C7_28
 S1_29, C1_29, C2_29, C3_29, C4_29, C5_29, C6_29, C7_29
 S1_30, C1_30, C2_30, C3_30, C4_30, C5_30, C6_30, C7_30
 S1_31, C1_31, C2_31, C3_31, C4_31, C5_31, C6_31, C7_31
 S1_32, C1_32, C2_32, C3_32, C4_32, C5_32, C6_32, C7_32
 S1_33, C1_33, C2_33, C3_33, C4_33, C5_33, C6_33, C7_33
 S1_34, C1_34, C2_34, C3_34, C4_34, C5_34, C6_34, C7_34
 S1_35, C1_35, C2_35, C3_35, C4_35, C5_35, C6_35, C7_35
 S1_36, C1_36, C2_36, C3_36, C4_36, C5_36, C6_36, C7_36
 S1_37, C1_37, C2_37, C3_37, C4_37, C5_37, C6_37, C7_37
 S1_38, C1_38, C2_38, C3_38, C4_38, C5_38, C6_38, C7_38
 S1_39, C1_39, C2_39, C3_39, C4_39, C5_39, C6_39, C7_39
 S1_40, C1_40, C2_40, C3_40, C4_40, C5_40, C6_40, C7_40
 S1_41, C1_41, C2_41, C3_41, C4_41, C5_41, C6_41, C7_41
 S1_42, C1_42, C2_42, C3_42, C4_42, C5_42, C6_42, C7_42
 S1_44, C1_44, C2_44, C3_44, C4_44, C5_44, C6_44, C7_44
 S1_45, C1_45, C2_45, C3_45, C4_45, C5_45, C6_45, C7_45
 S1_46, C1_46, C2_46, C3_46, C4_46, C5_46, C6_46, C7_46
 S1_47, C1_47, C2_47, C3_47, C4_47, C5_47, C6_47, C7_47
 S1_43, C1_43, C2_43, C3_43, C4_43, C5_43, C6_43, C7_43
 with sigma of 0.01
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
All non-hydrogen atoms have similar U: within 1A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1A
Uanis(S1_3) \\sim Ueq, Uanis(C1_3) \\sim Ueq, Uanis(C2_3) \\sim Ueq,
Uanis(C3_3) \\sim Ueq, Uanis(C4_3) \\sim Ueq, Uanis(C5_3) \\sim Ueq,
Uanis(C6_3) \\sim Ueq, Uanis(C7_3) \\sim Ueq, Uanis(S1_4) \\sim Ueq,
Uanis(C1_4) \\sim Ueq, Uanis(C2_4) \\sim Ueq, Uanis(C3_4) \\sim Ueq,
Uanis(C4_4) \\sim Ueq, Uanis(C5_4) \\sim Ueq, Uanis(C6_4) \\sim Ueq,
Uanis(C7_4) \\sim Ueq, Uanis(S1_5) \\sim Ueq, Uanis(C1_5) \\sim Ueq,
Uanis(C2_5) \\sim Ueq, Uanis(C3_5) \\sim Ueq, Uanis(C4_5) \\sim Ueq,
Uanis(C5_5) \\sim Ueq, Uanis(C6_5) \\sim Ueq, Uanis(C7_5) \\sim Ueq,
Uanis(S1_6) \\sim Ueq, Uanis(C1_6) \\sim Ueq, Uanis(C2_6) \\sim Ueq,
Uanis(C3_6) \\sim Ueq, Uanis(C4_6) \\sim Ueq, Uanis(C5_6) \\sim Ueq,
Uanis(C6_6) \\sim Ueq, Uanis(C7_6) \\sim Ueq, Uanis(S1_7) \\sim Ueq,
Uanis(C1_7) \\sim Ueq, Uanis(C2_7) \\sim Ueq, Uanis(C3_7) \\sim Ueq,
Uanis(C4_7) \\sim Ueq, Uanis(C5_7) \\sim Ueq, Uanis(C6_7) \\sim Ueq,
Uanis(C7_7) \\sim Ueq, Uanis(S1_8) \\sim Ueq, Uanis(C1_8) \\sim Ueq,
Uanis(C2_8) \\sim Ueq, Uanis(C3_8) \\sim Ueq, Uanis(C4_8) \\sim Ueq,
Uanis(C5_8) \\sim Ueq, Uanis(C6_8) \\sim Ueq, Uanis(C7_8) \\sim Ueq,
Uanis(S1_9) \\sim Ueq, Uanis(C1_9) \\sim Ueq, Uanis(C2_9) \\sim Ueq,
Uanis(C3_9) \\sim Ueq, Uanis(C4_9) \\sim Ueq, Uanis(C5_9) \\sim Ueq,
Uanis(C6_9) \\sim Ueq, Uanis(C7_9) \\sim Ueq, Uanis(S1_10) \\sim Ueq,
Uanis(C1_10) \\sim Ueq, Uanis(C2_10) \\sim Ueq, Uanis(C3_10) \\sim Ueq,
Uanis(C4_10) \\sim Ueq, Uanis(C5_10) \\sim Ueq, Uanis(C6_10) \\sim Ueq,
Uanis(C7_10) \\sim Ueq, Uanis(S1_11) \\sim Ueq, Uanis(C1_11) \\sim Ueq,
Uanis(C2_11) \\sim Ueq, Uanis(C3_11) \\sim Ueq, Uanis(C4_11) \\sim Ueq,
Uanis(C5_11) \\sim Ueq, Uanis(C6_11) \\sim Ueq, Uanis(C7_11) \\sim Ueq,
Uanis(S1_12) \\sim Ueq, Uanis(C1_12) \\sim Ueq, Uanis(C2_12) \\sim Ueq,
Uanis(C3_12) \\sim Ueq, Uanis(C4_12) \\sim Ueq, Uanis(C5_12) \\sim Ueq,
Uanis(C6_12) \\sim Ueq, Uanis(C7_12) \\sim Ueq, Uanis(S1_13) \\sim Ueq,
Uanis(C1_13) \\sim Ueq, Uanis(C2_13) \\sim Ueq, Uanis(C3_13) \\sim Ueq,
Uanis(C4_13) \\sim Ueq, Uanis(C5_13) \\sim Ueq, Uanis(C6_13) \\sim Ueq,
Uanis(C7_13) \\sim Ueq, Uanis(S1_14) \\sim Ueq, Uanis(C1_14) \\sim Ueq,
Uanis(C2_14) \\sim Ueq, Uanis(C3_14) \\sim Ueq, Uanis(C4_14) \\sim Ueq,
Uanis(C5_14) \\sim Ueq, Uanis(C6_14) \\sim Ueq, Uanis(C7_14) \\sim Ueq,
Uanis(S1_15) \\sim Ueq, Uanis(C1_15) \\sim Ueq, Uanis(C2_15) \\sim Ueq,
Uanis(C3_15) \\sim Ueq, Uanis(C4_15) \\sim Ueq, Uanis(C5_15) \\sim Ueq,
Uanis(C6_15) \\sim Ueq, Uanis(C7_15) \\sim Ueq, Uanis(S1_16) \\sim Ueq,
Uanis(C1_16) \\sim Ueq, Uanis(C2_16) \\sim Ueq, Uanis(C3_16) \\sim Ueq,
Uanis(C4_16) \\sim Ueq, Uanis(C5_16) \\sim Ueq, Uanis(C6_16) \\sim Ueq,
Uanis(C7_16) \\sim Ueq, Uanis(S1_17) \\sim Ueq, Uanis(C1_17) \\sim Ueq,
Uanis(C2_17) \\sim Ueq, Uanis(C3_17) \\sim Ueq, Uanis(C4_17) \\sim Ueq,
Uanis(C5_17) \\sim Ueq, Uanis(C6_17) \\sim Ueq, Uanis(C7_17) \\sim Ueq,
Uanis(S1_18) \\sim Ueq, Uanis(C1_18) \\sim Ueq, Uanis(C2_18) \\sim Ueq,
Uanis(C3_18) \\sim Ueq, Uanis(C4_18) \\sim Ueq, Uanis(C5_18) \\sim Ueq,
Uanis(C6_18) \\sim Ueq, Uanis(C7_18) \\sim Ueq, Uanis(S1_19) \\sim Ueq,
Uanis(C1_19) \\sim Ueq, Uanis(C2_19) \\sim Ueq, Uanis(C3_19) \\sim Ueq,
Uanis(C4_19) \\sim Ueq, Uanis(C5_19) \\sim Ueq, Uanis(C6_19) \\sim Ueq,
Uanis(C7_19) \\sim Ueq, Uanis(S1_21) \\sim Ueq, Uanis(C1_21) \\sim Ueq,
Uanis(C2_21) \\sim Ueq, Uanis(C3_21) \\sim Ueq, Uanis(C4_21) \\sim Ueq,
Uanis(C5_21) \\sim Ueq, Uanis(C6_21) \\sim Ueq, Uanis(C7_21) \\sim Ueq,
Uanis(S1_22) \\sim Ueq, Uanis(C1_22) \\sim Ueq, Uanis(C2_22) \\sim Ueq,
Uanis(C3_22) \\sim Ueq, Uanis(C4_22) \\sim Ueq, Uanis(C5_22) \\sim Ueq,
Uanis(C6_22) \\sim Ueq, Uanis(C7_22) \\sim Ueq, Uanis(S1_23) \\sim Ueq,
Uanis(C1_23) \\sim Ueq, Uanis(C2_23) \\sim Ueq, Uanis(C3_23) \\sim Ueq,
Uanis(C4_23) \\sim Ueq, Uanis(C5_23) \\sim Ueq, Uanis(C6_23) \\sim Ueq,
Uanis(C7_23) \\sim Ueq, Uanis(S1_24) \\sim Ueq, Uanis(C1_24) \\sim Ueq,
Uanis(C2_24) \\sim Ueq, Uanis(C3_24) \\sim Ueq, Uanis(C4_24) \\sim Ueq,
Uanis(C5_24) \\sim Ueq, Uanis(C6_24) \\sim Ueq, Uanis(C7_24) \\sim Ueq,
Uanis(S1_25) \\sim Ueq, Uanis(C1_25) \\sim Ueq, Uanis(C2_25) \\sim Ueq,
Uanis(C3_25) \\sim Ueq, Uanis(C4_25) \\sim Ueq, Uanis(C5_25) \\sim Ueq,
Uanis(C6_25) \\sim Ueq, Uanis(C7_25) \\sim Ueq, Uanis(S1_26) \\sim Ueq,
Uanis(C1_26) \\sim Ueq, Uanis(C2_26) \\sim Ueq, Uanis(C3_26) \\sim Ueq,
Uanis(C4_26) \\sim Ueq, Uanis(C5_26) \\sim Ueq, Uanis(C6_26) \\sim Ueq,
Uanis(C7_26) \\sim Ueq, Uanis(S1_27) \\sim Ueq, Uanis(C1_27) \\sim Ueq,
Uanis(C2_27) \\sim Ueq, Uanis(C3_27) \\sim Ueq, Uanis(C4_27) \\sim Ueq,
Uanis(C5_27) \\sim Ueq, Uanis(C6_27) \\sim Ueq, Uanis(C7_27) \\sim Ueq,
Uanis(S1_28) \\sim Ueq, Uanis(C1_28) \\sim Ueq, Uanis(C2_28) \\sim Ueq,
Uanis(C3_28) \\sim Ueq, Uanis(C4_28) \\sim Ueq, Uanis(C5_28) \\sim Ueq,
Uanis(C6_28) \\sim Ueq, Uanis(C7_28) \\sim Ueq, Uanis(S1_29) \\sim Ueq,
Uanis(C1_29) \\sim Ueq, Uanis(C2_29) \\sim Ueq, Uanis(C3_29) \\sim Ueq,
Uanis(C4_29) \\sim Ueq, Uanis(C5_29) \\sim Ueq, Uanis(C6_29) \\sim Ueq,
Uanis(C7_29) \\sim Ueq, Uanis(S1_30) \\sim Ueq, Uanis(C1_30) \\sim Ueq,
Uanis(C2_30) \\sim Ueq, Uanis(C3_30) \\sim Ueq, Uanis(C4_30) \\sim Ueq,
Uanis(C5_30) \\sim Ueq, Uanis(C6_30) \\sim Ueq, Uanis(C7_30) \\sim Ueq,
Uanis(S1_31) \\sim Ueq, Uanis(C1_31) \\sim Ueq, Uanis(C2_31) \\sim Ueq,
Uanis(C3_31) \\sim Ueq, Uanis(C4_31) \\sim Ueq, Uanis(C5_31) \\sim Ueq,
Uanis(C6_31) \\sim Ueq, Uanis(C7_31) \\sim Ueq, Uanis(S1_32) \\sim Ueq,
Uanis(C1_32) \\sim Ueq, Uanis(C2_32) \\sim Ueq, Uanis(C3_32) \\sim Ueq,
Uanis(C4_32) \\sim Ueq, Uanis(C5_32) \\sim Ueq, Uanis(C6_32) \\sim Ueq,
Uanis(C7_32) \\sim Ueq, Uanis(S1_33) \\sim Ueq, Uanis(C1_33) \\sim Ueq,
Uanis(C2_33) \\sim Ueq, Uanis(C3_33) \\sim Ueq, Uanis(C4_33) \\sim Ueq,
Uanis(C5_33) \\sim Ueq, Uanis(C6_33) \\sim Ueq, Uanis(C7_33) \\sim Ueq,
Uanis(S1_34) \\sim Ueq, Uanis(C1_34) \\sim Ueq, Uanis(C2_34) \\sim Ueq,
Uanis(C3_34) \\sim Ueq, Uanis(C4_34) \\sim Ueq, Uanis(C5_34) \\sim Ueq,
Uanis(C6_34) \\sim Ueq, Uanis(C7_34) \\sim Ueq, Uanis(S1_35) \\sim Ueq,
Uanis(C1_35) \\sim Ueq, Uanis(C2_35) \\sim Ueq, Uanis(C3_35) \\sim Ueq,
Uanis(C4_35) \\sim Ueq, Uanis(C5_35) \\sim Ueq, Uanis(C6_35) \\sim Ueq,
Uanis(C7_35) \\sim Ueq, Uanis(S1_36) \\sim Ueq, Uanis(C1_36) \\sim Ueq,
Uanis(C2_36) \\sim Ueq, Uanis(C3_36) \\sim Ueq, Uanis(C4_36) \\sim Ueq,
Uanis(C5_36) \\sim Ueq, Uanis(C6_36) \\sim Ueq, Uanis(C7_36) \\sim Ueq,
Uanis(S1_37) \\sim Ueq, Uanis(C1_37) \\sim Ueq, Uanis(C2_37) \\sim Ueq,
Uanis(C3_37) \\sim Ueq, Uanis(C4_37) \\sim Ueq, Uanis(C5_37) \\sim Ueq,
Uanis(C6_37) \\sim Ueq, Uanis(C7_37) \\sim Ueq, Uanis(S1_38) \\sim Ueq,
Uanis(C1_38) \\sim Ueq, Uanis(C2_38) \\sim Ueq, Uanis(C3_38) \\sim Ueq,
Uanis(C4_38) \\sim Ueq, Uanis(C5_38) \\sim Ueq, Uanis(C6_38) \\sim Ueq,
Uanis(C7_38) \\sim Ueq, Uanis(S1_39) \\sim Ueq, Uanis(C1_39) \\sim Ueq,
Uanis(C2_39) \\sim Ueq, Uanis(C3_39) \\sim Ueq, Uanis(C4_39) \\sim Ueq,
Uanis(C5_39) \\sim Ueq, Uanis(C6_39) \\sim Ueq, Uanis(C7_39) \\sim Ueq,
Uanis(S1_40) \\sim Ueq, Uanis(C1_40) \\sim Ueq, Uanis(C2_40) \\sim Ueq,
Uanis(C3_40) \\sim Ueq, Uanis(C4_40) \\sim Ueq, Uanis(C5_40) \\sim Ueq,
Uanis(C6_40) \\sim Ueq, Uanis(C7_40) \\sim Ueq, Uanis(S1_41) \\sim Ueq,
Uanis(C1_41) \\sim Ueq, Uanis(C2_41) \\sim Ueq, Uanis(C3_41) \\sim Ueq,
Uanis(C4_41) \\sim Ueq, Uanis(C5_41) \\sim Ueq, Uanis(C6_41) \\sim Ueq,
Uanis(C7_41) \\sim Ueq, Uanis(S1_42) \\sim Ueq, Uanis(C1_42) \\sim Ueq,
Uanis(C2_42) \\sim Ueq, Uanis(C3_42) \\sim Ueq, Uanis(C4_42) \\sim Ueq,
Uanis(C5_42) \\sim Ueq, Uanis(C6_42) \\sim Ueq, Uanis(C7_42) \\sim Ueq,
Uanis(S1_44) \\sim Ueq, Uanis(C1_44) \\sim Ueq, Uanis(C2_44) \\sim Ueq,
Uanis(C3_44) \\sim Ueq, Uanis(C4_44) \\sim Ueq, Uanis(C5_44) \\sim Ueq,
Uanis(C6_44) \\sim Ueq, Uanis(C7_44) \\sim Ueq, Uanis(S1_45) \\sim Ueq,
Uanis(C1_45) \\sim Ueq, Uanis(C2_45) \\sim Ueq, Uanis(C3_45) \\sim Ueq,
Uanis(C4_45) \\sim Ueq, Uanis(C5_45) \\sim Ueq, Uanis(C6_45) \\sim Ueq,
Uanis(C7_45) \\sim Ueq, Uanis(S1_46) \\sim Ueq, Uanis(C1_46) \\sim Ueq,
Uanis(C2_46) \\sim Ueq, Uanis(C3_46) \\sim Ueq, Uanis(C4_46) \\sim Ueq,
Uanis(C5_46) \\sim Ueq, Uanis(C6_46) \\sim Ueq, Uanis(C7_46) \\sim Ueq,
Uanis(S1_47) \\sim Ueq, Uanis(C1_47) \\sim Ueq, Uanis(C2_47) \\sim Ueq,
Uanis(C3_47) \\sim Ueq, Uanis(C4_47) \\sim Ueq, Uanis(C5_47) \\sim Ueq,
Uanis(C6_47) \\sim Ueq, Uanis(C7_47) \\sim Ueq, Uanis(S1_43) \\sim Ueq,
Uanis(C1_43) \\sim Ueq, Uanis(C2_43) \\sim Ueq, Uanis(C3_43) \\sim Ueq,
Uanis(C4_43) \\sim Ueq, Uanis(C5_43) \\sim Ueq, Uanis(C6_43) \\sim Ueq,
Uanis(C7_43) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
6. Rigid body (RIGU) restrains
 S1_3, C1_3, C2_3, C3_3, C4_3, C5_3, C6_3, C7_3
 S1_4, C1_4, C2_4, C3_4, C4_4, C5_4, C6_4, C7_4
 S1_5, C1_5, C2_5, C3_5, C4_5, C5_5, C6_5, C7_5
 S1_6, C1_6, C2_6, C3_6, C4_6, C5_6, C6_6, C7_6
 S1_7, C1_7, C2_7, C3_7, C4_7, C5_7, C6_7, C7_7
 S1_8, C1_8, C2_8, C3_8, C4_8, C5_8, C6_8, C7_8
 S1_9, C1_9, C2_9, C3_9, C4_9, C5_9, C6_9, C7_9
 S1_10, C1_10, C2_10, C3_10, C4_10, C5_10, C6_10, C7_10
 S1_11, C1_11, C2_11, C3_11, C4_11, C5_11, C6_11, C7_11
 S1_12, C1_12, C2_12, C3_12, C4_12, C5_12, C6_12, C7_12
 S1_13, C1_13, C2_13, C3_13, C4_13, C5_13, C6_13, C7_13
 S1_14, C1_14, C2_14, C3_14, C4_14, C5_14, C6_14, C7_14
 S1_15, C1_15, C2_15, C3_15, C4_15, C5_15, C6_15, C7_15
 S1_16, C1_16, C2_16, C3_16, C4_16, C5_16, C6_16, C7_16
 S1_17, C1_17, C2_17, C3_17, C4_17, C5_17, C6_17, C7_17
 S1_18, C1_18, C2_18, C3_18, C4_18, C5_18, C6_18, C7_18
 S1_19, C1_19, C2_19, C3_19, C4_19, C5_19, C6_19, C7_19
 S1_21, C1_21, C2_21, C3_21, C4_21, C5_21, C6_21, C7_21
 S1_22, C1_22, C2_22, C3_22, C4_22, C5_22, C6_22, C7_22
 S1_23, C1_23, C2_23, C3_23, C4_23, C5_23, C6_23, C7_23
 S1_24, C1_24, C2_24, C3_24, C4_24, C5_24, C6_24, C7_24
 S1_25, C1_25, C2_25, C3_25, C4_25, C5_25, C6_25, C7_25
 S1_26, C1_26, C2_26, C3_26, C4_26, C5_26, C6_26, C7_26
 S1_27, C1_27, C2_27, C3_27, C4_27, C5_27, C6_27, C7_27
 S1_28, C1_28, C2_28, C3_28, C4_28, C5_28, C6_28, C7_28
 S1_29, C1_29, C2_29, C3_29, C4_29, C5_29, C6_29, C7_29
 S1_30, C1_30, C2_30, C3_30, C4_30, C5_30, C6_30, C7_30
 S1_31, C1_31, C2_31, C3_31, C4_31, C5_31, C6_31, C7_31
 S1_32, C1_32, C2_32, C3_32, C4_32, C5_32, C6_32, C7_32
 S1_33, C1_33, C2_33, C3_33, C4_33, C5_33, C6_33, C7_33
 S1_34, C1_34, C2_34, C3_34, C4_34, C5_34, C6_34, C7_34
 S1_35, C1_35, C2_35, C3_35, C4_35, C5_35, C6_35, C7_35
 S1_36, C1_36, C2_36, C3_36, C4_36, C5_36, C6_36, C7_36
 S1_37, C1_37, C2_37, C3_37, C4_37, C5_37, C6_37, C7_37
 S1_38, C1_38, C2_38, C3_38, C4_38, C5_38, C6_38, C7_38
 S1_39, C1_39, C2_39, C3_39, C4_39, C5_39, C6_39, C7_39
 S1_40, C1_40, C2_40, C3_40, C4_40, C5_40, C6_40, C7_40
 S1_41, C1_41, C2_41, C3_41, C4_41, C5_41, C6_41, C7_41
 S1_42, C1_42, C2_42, C3_42, C4_42, C5_42, C6_42, C7_42
 S1_44, C1_44, C2_44, C3_44, C4_44, C5_44, C6_44, C7_44
 S1_45, C1_45, C2_45, C3_45, C4_45, C5_45, C6_45, C7_45
 S1_46, C1_46, C2_46, C3_46, C4_46, C5_46, C6_46, C7_46
 S1_47, C1_47, C2_47, C3_47, C4_47, C5_47, C6_47, C7_47
 S1_43, C1_43, C2_43, C3_43, C4_43, C5_43, C6_43, C7_43
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Same fragment restrains
{S1_4, C1_4, C2_4, C3_4, C4_4, C5_4, C6_4, C7_4}
{S1_5, C1_5, C2_5, C3_5, C4_5, C5_5, C6_5, C7_5}
{S1_6, C1_6, C2_6, C3_6, C4_6, C5_6, C6_6, C7_6}
{S1_7, C1_7, C2_7, C3_7, C4_7, C5_7, C6_7, C7_7}
{S1_8, C1_8, C2_8, C3_8, C4_8, C5_8, C6_8, C7_8}
{S1_9, C1_9, C2_9, C3_9, C4_9, C5_9, C6_9, C7_9}
{S1_10, C1_10, C2_10, C3_10, C4_10, C5_10, C6_10, C7_10}
{S1_11, C1_11, C2_11, C3_11, C4_11, C5_11, C6_11, C7_11}
{S1_12, C1_12, C2_12, C3_12, C4_12, C5_12, C6_12, C7_12}
{S1_13, C1_13, C2_13, C3_13, C4_13, C5_13, C6_13, C7_13}
{S1_14, C1_14, C2_14, C3_14, C4_14, C5_14, C6_14, C7_14}
{S1_15, C1_15, C2_15, C3_15, C4_15, C5_15, C6_15, C7_15}
{S1_16, C1_16, C2_16, C3_16, C4_16, C5_16, C6_16, C7_16}
{S1_17, C1_17, C2_17, C3_17, C4_17, C5_17, C6_17, C7_17}
{S1_18, C1_18, C2_18, C3_18, C4_18, C5_18, C6_18, C7_18}
{S1_19, C1_19, C2_19, C3_19, C4_19, C5_19, C6_19, C7_19}
{S1_21, C1_21, C2_21, C3_21, C4_21, C5_21, C6_21, C7_21}
{S1_22, C1_22, C2_22, C3_22, C4_22, C5_22, C6_22, C7_22}
{S1_23, C1_23, C2_23, C3_23, C4_23, C5_23, C6_23, C7_23}
{S1_24, C1_24, C2_24, C3_24, C4_24, C5_24, C6_24, C7_24}
{S1_25, C1_25, C2_25, C3_25, C4_25, C5_25, C6_25, C7_25}
{S1_26, C1_26, C2_26, C3_26, C4_26, C5_26, C6_26, C7_26}
{S1_27, C1_27, C2_27, C3_27, C4_27, C5_27, C6_27, C7_27}
{S1_28, C1_28, C2_28, C3_28, C4_28, C5_28, C6_28, C7_28}
{S1_29, C1_29, C2_29, C3_29, C4_29, C5_29, C6_29, C7_29}
{S1_30, C1_30, C2_30, C3_30, C4_30, C5_30, C6_30, C7_30}
{S1_31, C1_31, C2_31, C3_31, C4_31, C5_31, C6_31, C7_31}
{S1_32, C1_32, C2_32, C3_32, C4_32, C5_32, C6_32, C7_32}
{S1_33, C1_33, C2_33, C3_33, C4_33, C5_33, C6_33, C7_33}
{S1_34, C1_34, C2_34, C3_34, C4_34, C5_34, C6_34, C7_34}
{S1_35, C1_35, C2_35, C3_35, C4_35, C5_35, C6_35, C7_35}
{S1_36, C1_36, C2_36, C3_36, C4_36, C5_36, C6_36, C7_36}
{S1_37, C1_37, C2_37, C3_37, C4_37, C5_37, C6_37, C7_37}
{S1_38, C1_38, C2_38, C3_38, C4_38, C5_38, C6_38, C7_38}
{S1_39, C1_39, C2_39, C3_39, C4_39, C5_39, C6_39, C7_39}
{S1_40, C1_40, C2_40, C3_40, C4_40, C5_40, C6_40, C7_40}
{S1_41, C1_41, C2_41, C3_41, C4_41, C5_41, C6_41, C7_41}
{S1_42, C1_42, C2_42, C3_42, C4_42, C5_42, C6_42, C7_42}
{S1_44, C1_44, C2_44, C3_44, C4_44, C5_44, C6_44, C7_44}
{S1_45, C1_45, C2_45, C3_45, C4_45, C5_45, C6_45, C7_45}
{S1_46, C1_46, C2_46, C3_46, C4_46, C5_46, C6_46, C7_46}
{S1_47, C1_47, C2_47, C3_47, C4_47, C5_47, C6_47, C7_47}
{S1_43, C1_43, C2_43, C3_43, C4_43, C5_43, C6_43, C7_43}
as
{S1_3, C1_3, C2_3, C3_3, C4_3, C5_3, C6_3, C7_3} sigma for 1-2: 0.01 1-3: 0.04
8.a Everything fixed:
 S1
8.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C2(H2), C3(H3), C5(H5), C6(H6), C2(H2),
 C3(H3), C5(H5), C6(H6), C2(H2), C3(H3), C5(H5), C6(H6), C2(H2), C3(H3), C5(H5),
  C6(H6), C2(H2), C3(H3), C5(H5), C6(H6), C2(H2), C3(H3), C5(H5), C6(H6),
 C2(H2), C3(H3), C5(H5), C6(H6), C2(H2), C3(H3), C5(H5), C6(H6), C2(H2), C3(H3),
  C5(H5), C6(H6), C2(H2), C3(H3), C5(H5), C6(H6), C2(H2), C3(H3), C5(H5),
 C6(H6), C2(H2), C3(H3), C5(H5), C6(H6), C2(H2), C3(H3), C5(H5), C6(H6), C2(H2),
  C3(H3), C5(H5), C6(H6), C2(H2), C3(H3), C5(H5), C6(H6), C2(H2), C3(H3),
 C5(H5), C6(H6), C2(H2), C3(H3), C5(H5), C6(H6), C2(H2), C3(H3), C5(H5), C6(H6),
  C2(H2), C3(H3), C5(H5), C6(H6), C2(H2), C3(H3), C5(H5), C6(H6), C2(H2),
 C3(H3), C5(H5), C6(H6), C2(H2), C3(H3), C5(H5), C6(H6), C2(H2), C3(H3), C5(H5),
  C6(H6), C2(H2), C3(H3), C5(H5), C6(H6), C2(H2), C3(H3), C5(H5), C6(H6),
 C2(H2), C3(H3), C5(H5), C6(H6), C2(H2), C3(H3), C5(H5), C6(H6), C2(H2), C3(H3),
  C5(H5), C6(H6), C2(H2), C3(H3), C5(H5), C6(H6), C2(H2), C3(H3), C5(H5),
 C6(H6), C2(H2), C3(H3), C5(H5), C6(H6), C2(H2), C3(H3), C5(H5), C6(H6), C2(H2),
  C3(H3), C5(H5), C6(H6), C2(H2), C3(H3), C5(H5), C6(H6), C2(H2), C3(H3),
 C5(H5), C6(H6), C2(H2), C3(H3), C5(H5), C6(H6), C2(H2), C3(H3), C5(H5), C6(H6),
  C2(H2), C3(H3), C5(H5), C6(H6), C2(H2), C3(H3), C5(H5), C6(H6), C2(H2),
 C3(H3), C5(H5), C6(H6), C2(H2), C3(H3), C5(H5), C6(H6), C2(H2), C3(H3), C5(H5),
  C6(H6), C2(H2), C3(H3), C5(H5), C6(H6)
8.c Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6)
8.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C7(H7A,H7B,H7C), C7(H7A,H7B,H7C), C7(H7A,H7B,H7C), C7(H7A,
 H7B,H7C), C7(H7A,H7B,H7C), C7(H7A,H7B,H7C), C7(H7A,H7B,H7C), C7(H7A,H7B,H7C),
 C7(H7A,H7B,H7C), C7(H7A,H7B,H7C), C7(H7A,H7B,H7C), C7(H7A,H7B,H7C), C7(H7A,H7B,
 H7C), C7(H7A,H7B,H7C), C7(H7A,H7B,H7C), C7(H7A,H7B,H7C), C7(H7A,H7B,H7C),
 C7(H7A,H7B,H7C), C7(H7A,H7B,H7C), C7(H7A,H7B,H7C), C7(H7A,H7B,H7C), C7(H7A,H7B,
 H7C), C7(H7A,H7B,H7C), C7(H7A,H7B,H7C), C7(H7A,H7B,H7C), C7(H7A,H7B,H7C),
 C7(H7A,H7B,H7C), C7(H7A,H7B,H7C), C7(H7A,H7B,H7C), C7(H7A,H7B,H7C), C7(H7A,H7B,
 H7C), C7(H7A,H7B,H7C), C7(H7A,H7B,H7C), C7(H7A,H7B,H7C), C7(H7A,H7B,H7C),
 C7(H7A,H7B,H7C), C7(H7A,H7B,H7C), C7(H7A,H7B,H7C), C7(H7A,H7B,H7C), C7(H7A,H7B,
 H7C), C7(H7A,H7B,H7C), C7(H7A,H7B,H7C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              73121
_shelx_hkl_checksum              45837
_shelx_fab_checksum              20756
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU