Selective construction and stability studies of molecular trefoil knot and Solomon link
Dang, Li-Long; Li, Ting-Ting; Cui, Zheng; Dong, Sui; Ma, Lufang; Jin, Guo-Xin; Dalton Transactions  (2021) –; doi:10.1039/D1DT02755G

data_7708299
_publ_section_title
;
 Selective construction and stability studies of molecular trefoil knot
 and Solomon link
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02755G
_journal_year                    2021
_chemical_formula_moiety
'3(C F3 O3 S), C198 H168 N12 O24 Rh6, 9[C6H14O], 1[CH3OH]'
_chemical_formula_sum            'C256 H298 F9 N12 O43 Rh6 S3'
_chemical_formula_weight         5115.69
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-04-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-05-08 deposited with the CCDC.	2021-09-15 downloaded from the CCDC.
;
_cell_angle_alpha                86.260(7)
_cell_angle_beta                 85.845(7)
_cell_angle_gamma                82.804(7)
_cell_formula_units_Z            2
_cell_length_a                   16.554(3)
_cell_length_b                   21.628(3)
_cell_length_c                   31.264(5)
_cell_measurement_reflns_used    9371
_cell_measurement_temperature    172.99
_cell_measurement_theta_max      54.89
_cell_measurement_theta_min      3.29
_cell_volume                     11058(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      172.99
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            145476
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.063
_diffrn_reflns_theta_min         2.933
_diffrn_source_current           2.86
_diffrn_source_power             0.1999426
_diffrn_source_voltage           69.91
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.054
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.4212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_description       block
_exptl_crystal_F_000             5322
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.13
_refine_diff_density_max         3.912
_refine_diff_density_min         -3.582
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2406
_refine_ls_number_reflns         42016
_refine_ls_number_restraints     7320
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.1024
_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^)+(0.1548P)^2^+41.1009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2846
_refine_ls_wR_factor_ref         0.2980
_reflns_Friedel_coverage         0.000
_reflns_number_gt                33857
_reflns_number_total             42016
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02755g2.cif
_cod_data_source_block           ga_210303d_a
_cod_original_cell_volume        11059(3)
_cod_database_code               7708299
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.692
_shelx_estimated_absorpt_t_min   0.360
_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
 C06J-C07N = C07N-C06D = C06D-C06N = C06N-C076 = C076-C06J
 1.41 with sigma of 0.01
 C06Y-C06B = C06B-C06S = C06S-C06C = C06C-C06I = C06I-C06Y
 1.41 with sigma of 0.01
 C05A-C05U = C05U-C06L = C06L-C04V = C04V-C05F = C05F-C05A
 1.41 with sigma of 0.01
 O1-O2 = O2-O3 = O1-O3
 2.39 with sigma of 0.01
 S008-C38
 1.78 with sigma of 0.01
 F06O-F07G = F07G-F06R = F06R-F06O = F1-F2 = F2-F3 = F1-F3
 2.1 with sigma of 0.01
 C1-F1 = C1-F2 = C1-F3
 1.31 with sigma of 0.01
 S1-O1 = S1-O2 = S1-O3
 1.41 with sigma of 0.01
 C06B-C37 = C06D-C078 = C44-C06S = C06F-C07O = C07E-C06N = C06Q-C07N
 1.54 with sigma of 0.02
3. Restrained planarity
 C06J, C07N, C06D, C076, C06N
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C011 \\sim C015 \\sim C016 \\sim C017 \\sim C019 \\sim C01A \\sim C01B \\sim
C01C \\sim C01D \\sim C01E \\sim C1 \\sim C01G \\sim C01H \\sim C01J \\sim C01L
\\sim C01M \\sim C01N \\sim C01O \\sim C01P \\sim C01Q \\sim C01T \\sim C01U
\\sim C01V \\sim C01W \\sim C01X \\sim C01Y \\sim C020 \\sim C022 \\sim C023
\\sim C024 \\sim C025 \\sim C026 \\sim C027 \\sim C028 \\sim C029 \\sim C02A
\\sim C02B \\sim C02C \\sim C02D \\sim C02E \\sim C02F \\sim C02G \\sim C02H
\\sim C02I \\sim C02J \\sim C02K \\sim C02L \\sim C02M \\sim C02N \\sim C02O
\\sim C02P \\sim C02Q \\sim C02R \\sim C02S \\sim C02T \\sim C02U \\sim C02V
\\sim C02W \\sim C02X \\sim C02Y \\sim C02Z \\sim C031 \\sim C033 \\sim C034
\\sim C035 \\sim C036 \\sim C037 \\sim C038 \\sim C03A \\sim C03B \\sim C03C
\\sim C03D \\sim C03E \\sim C03F \\sim C03G \\sim C03H \\sim C03I \\sim C03J
\\sim C03K \\sim C03L \\sim C03M \\sim C03N \\sim C03O \\sim C03P \\sim C03R
\\sim C03S \\sim C03T \\sim C03U \\sim C03V \\sim C03W \\sim C03X \\sim C03Y
\\sim C03Z \\sim C040 \\sim C041 \\sim C042 \\sim C043 \\sim C044 \\sim C045
\\sim C046 \\sim C047 \\sim C048 \\sim C049 \\sim C04A \\sim C04B \\sim C04C
\\sim C04D \\sim C04E \\sim C04F \\sim C04G \\sim C04H \\sim C04I \\sim C04J
\\sim C04L \\sim C04M \\sim C04N \\sim C04O \\sim C04P \\sim C04Q \\sim C04R
\\sim C04S \\sim C04T \\sim C04U \\sim C04V \\sim C04W \\sim C04X \\sim C04Z
\\sim C050 \\sim C051 \\sim C052 \\sim C053 \\sim C054 \\sim C055 \\sim C056
\\sim C057 \\sim C058 \\sim C059 \\sim C05A \\sim C05B \\sim C05C \\sim C05D
\\sim C05F \\sim C05G \\sim C05H \\sim C05I \\sim C05K \\sim C05M \\sim C05O
\\sim C05P \\sim C05Q \\sim C05R \\sim C05T \\sim C05U \\sim C05W \\sim C05X
\\sim C05Z \\sim C060 \\sim C061 \\sim C062 \\sim C065 \\sim C066 \\sim C067
\\sim C068 \\sim C069 \\sim C06A \\sim C06B \\sim C06C \\sim C06D \\sim C06E
\\sim C06F \\sim C06G \\sim C06I \\sim C06J \\sim C06L \\sim C06M \\sim C06N
\\sim C06Q \\sim C06S \\sim C06V \\sim C06Y \\sim C06Z \\sim C071 \\sim C072
\\sim C074 \\sim C076 \\sim C078 \\sim C07B \\sim C07E \\sim C07K \\sim C07N
\\sim C07O \\sim C17 \\sim C18 \\sim C37 \\sim C38 \\sim C39 \\sim C44 \\sim
C57 \\sim C58 \\sim C92 \\sim C166: within 3.8A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 3.8A
6.a Secondary CH2 refined with riding coordinates:
 C02F(H02A,H02D), C02I(H02E,H02F), C042(H04A,H04B), C04L(H04H,H04I), C04N(H04J,
 H04K), C052(H05A,H05B)
6.b Me refined with riding coordinates:
 C18(H18A,H18B,H18C)
6.c Aromatic/amide H refined with riding coordinates:
 C01B(H01B), C01D(H01D), C01L(H01L), C01M(H01M), C01O(H01O), C01P(H01P),
 C01T(H01T), C01U(H01U), C01X(H01X), C01Y(H01Y), C024(H024), C029(H029),
 C02B(H02B), C02C(H02C), C02G(H02G), C02K(H02K), C02L(H02L), C02M(H02M),
 C02N(H02N), C02P(H02P), C02Q(H02Q), C02W(H02W), C02Y(H02Y), C02Z(H02Z),
 C033(H033), C036(H036), C037(H037), C03A(H03A), C03B(H03B), C03F(H03F),
 C03J(H03J), C03K(H03K), C03L(H03L), C03V(H03V), C03Z(H03Z), C040(H040),
 C045(H045), C046(H046), C04D(H04F), C04G(H04G), C04O(H04O), C04Q(H04Q),
 C04R(H04R), C04S(H04S), C04U(H04U), C04W(H04W), C04X(H04X), C04Z(H04Z),
 C050(H050), C051(H051), C053(H053), C057(H057), C058(H058), C05C(H05F),
 C05D(H05G), C05G(H05H), C05H(H05I), C05I(H05J), C05K(H05K), C05T(H05T),
 C05W(H05W), C05X(H05X), C060(H060), C061(H061), C062(H062), C066(H066)
6.d Idealised Me refined as rotating group:
 C049(H04C,H04D,H04E), C059(H05C,H05D,H05E), C05O(H05L,H05M,H05N), C05Z(H05O,
 H05P,H05Q), C065(H06A,H06B,H06C), C067(H06D,H06E,H06F), C069(H06G,H06H,H06I),
 C06E(H06J,H06K,H06L), C06G(H06M,H06N,H06O), C06M(H06P,H06Q,H06R), C06Q(H06S,
 H06T,H06U), C06V(H06V,H06W,H06X), C06Z(H06Y,H,HA), C071(H07A,H07B,H07C),
 C072(H07D,H07E,H07F), C074(H07G,H07H,H07I), C078(H07J,H07K,H07L), C07B(H07M,
 H07N,H07O), C07E(H07P,H07Q,H07R), C07K(H07S,H07T,H07U), C07O(H07V,H07W,H07X),
 C17(H17A,H17B,H17C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C44(H44A,H44B,
 H44C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C92(H92A,H92B,H92C),
 C166(H16A,H16B,H16C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 1115 electrons were 
found in a volume of 3056\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
9[C6H14O], 1[CH3OH] per Asymmetric Unit 
which account for 1080 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              93760
_shelx_hkl_checksum              87301
_shelx_fab_checksum              17001
_olex2_submission_special_instructions 'No special instructions were received'