Bi-directional geometric constraints in the construction of giant dual-rim nanorings
Zhong, Wanying; Wang, Zhantao; Yu, Wei-Dong; Wang, Ning; Fu, Fan; Wang, Jun; Zhao, He; Liu, Die; Jiang, Zhilong; Wang, Pingshan; Chen, Mingzhao; Dalton Transactions  (2023) –; doi:10.1039/D3DT00897E

data_7712876
_publ_section_title
;
 Bi-directional geometric constraints in the construction of giant
 dual-rim nanorings
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00897E
_journal_year                    2023
_chemical_formula_moiety
'0.5(C109.597 H80.193 N13), 0.25(C222.387 H159.967 N26), 1.298(C3 H7 N O), 0.5(H2 O)'
_chemical_formula_sum            'C114.29 H90.18 N14.3 O1.8'
_chemical_formula_weight         1692.62
_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
_audit_creation_date             2023-04-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2023-04-25 deposited with the CCDC.	2023-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                66.8300(10)
_cell_angle_beta                 87.7140(10)
_cell_angle_gamma                88.7170(10)
_cell_formula_units_Z            4
_cell_length_a                   15.1349(2)
_cell_length_b                   24.4882(3)
_cell_length_c                   26.4272(3)
_cell_measurement_reflns_used    31473
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      73.3140
_cell_measurement_theta_min      2.9080
_cell_volume                     8997.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.969
_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    -78.00  13.00   0.50    3.20    --  -46.85 102.00  43.00  182
  2  \w     -8.00  58.00   0.50    3.20    --   46.85-102.00 -59.00  132
  3  \w   -122.00 -87.00   0.50   26.50    --  -99.00-102.00 -59.00   70
  4  \w   -106.00 -61.00   0.50   26.50    --  -99.00 102.00  43.00   90
  5  \w    101.00 139.00   0.50   26.50    --   99.00 102.00  43.00   76
  6  \w     48.00 104.00   0.50   26.50    --   99.00-102.00 -59.00  112
  7  \w    -85.00 -16.00   0.50    3.20    --  -46.85 125.00  90.00  138
  8  \w    -16.00  10.00   0.50    3.20    --  -46.85  19.00  60.00   52
  9  \w   -118.00 -69.00   0.50    3.20    --  -46.85 -57.00 -90.00   98
 10  \w    -65.00 -40.00   0.50    3.20    --  -46.85 -57.00 -90.00   50
 11  \w   -100.00 -74.00   0.50    3.20    --  -46.85-125.00  60.00   52
 12  \w      0.00  29.00   0.50    3.20    --  -46.85  19.00   0.00   58
 13  \w    -18.00  44.00   0.50    3.20    --   46.85 -37.00 -60.00  124
 14  \w    -26.00  29.00   0.50    3.20    --   46.85 -19.00  30.00  110
 15  \w   -107.00 -82.00   0.50   26.50    --  -99.00 107.00-107.50   50
 16  \w   -167.00 -86.00   0.50   26.50    --  -99.00 -45.00  60.00  162
 17  \w   -109.00 -57.00   0.50   26.50    --  -99.00 115.00 128.40  104
 18  \w    -66.00 -26.00   0.50   26.50    --  -99.00  61.00   0.00   80
 19  \w    -73.00 -33.00   0.50   26.50    --  -99.00 107.00-107.50   80
 20  \w   -112.00 -86.00   0.50   26.50    --  -99.00 125.00  60.00   52
 21  \w    -68.00 -26.00   0.50   26.50    --  -99.00  61.00-180.00   84
 22  \w    -69.00 -44.00   0.50   26.50    --  -99.00  61.00-120.00   50
 23  \w   -108.00 -72.00   0.50   26.50    --  -99.00 113.00 -31.59   72
 24  \w    -71.00 -26.00   0.50   26.50    --  -99.00 125.00  60.00   90
 25  \w   -109.00 -28.00   0.50   26.50    --  -99.00 116.00  77.93  162
 26  \w   -169.00 -89.00   0.50   26.50    --  -99.00 -45.00 150.00  160
 27  \w   -111.00 -26.00   0.50   26.50    --  -99.00 125.00 150.00  170
 28  \w     26.00 105.00   0.50   26.50    --   99.00 -94.00 -60.00  158
 29  \w     27.00 108.00   0.50   26.50    --   99.00-125.00 -90.00  162
 30  \w     27.00  52.00   0.50   26.50    --   99.00 -45.00 -90.00   50
 31  \w     48.00  73.00   0.50   26.50    --   99.00 -61.00  90.00   50
 32  \w     27.00  53.00   0.50   26.50    --   99.00 -45.00  30.00   52
 33  \w     26.00  72.00   0.50   26.50    --   99.00 -61.00   0.00   92
 34  \w     27.00  52.00   0.50   26.50    --   99.00 -45.00   0.00   50
 35  \w     94.00 164.00   0.50   26.50    --   99.00 125.00   0.00  140
 36  \w    121.00 161.00   0.50   26.50    --   99.00  61.00-180.00   80
 37  \w     35.00  60.00   0.50   26.50    --   99.00 -61.00  60.00   50
 38  \w    133.00 159.00   0.50   26.50    --   99.00 125.00  90.00   52
 39  \w     94.00 123.00   0.50   26.50    --   99.00 125.00  90.00   58
 40  \w     49.00  88.00   0.50   26.50    --   99.00 -94.00  30.00   78
 41  \w     28.00  65.00   0.50   26.50    --   99.00 -61.00 -30.00   74
 42  \w     67.00 103.00   0.50   26.50    --   99.00-125.00  90.00   72
 43  \w    147.00 172.00   0.50   26.50    --   99.00 125.00 -60.00   50
 44  \w     82.00 117.00   0.50   26.50    --   99.00 125.00 -60.00   70
 45  \w    101.00 162.00   0.50   26.50    --   99.00  45.00 -30.00  122
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0326790000
_diffrn_orient_matrix_UB_12      -0.0336882000
_diffrn_orient_matrix_UB_13      0.0601147000
_diffrn_orient_matrix_UB_21      -0.0747765000
_diffrn_orient_matrix_UB_22      0.0461308000
_diffrn_orient_matrix_UB_23      -0.0082292000
_diffrn_orient_matrix_UB_31      -0.0609798000
_diffrn_orient_matrix_UB_32      -0.0376815000
_diffrn_orient_matrix_UB_33      -0.0185409000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            130851
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.829
_diffrn_reflns_theta_min         2.922
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96038
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.55a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.250
_exptl_crystal_description       block
_exptl_crystal_F_000             3562
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.247
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.222
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2602
_refine_ls_number_reflns         35268
_refine_ls_number_restraints     215
_refine_ls_restrained_S_all      1.232
_refine_ls_R_factor_all          0.1320
_refine_ls_R_factor_gt           0.0967
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2886
_refine_ls_wR_factor_ref         0.3252
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23229
_reflns_number_total             35268
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00897e2.cif
_cod_data_source_block           cmz-l
_cod_original_formula_sum        'C114.29 H90.18 N14.30 O1.80'
_cod_database_code               7712876
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N'
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.943
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, All O(H,H) groups
2. Restrained distances
 C17-C15 = C66-C06M
 1.54 with sigma of 0.02
 C66-C06M
 1.5 with sigma of 0.05
 C17-C19 \\sim C17-C8
 with sigma of 0.02
 C1B-C03G \\sim C1C-C03G
 with sigma of 0.02
 C1A-C06G \\sim C06G-C0
 with sigma of 0.02
 C063-C03G \\sim C058-C03G
 with sigma of 0.02
 C66-C35 \\sim C66-C20
 with sigma of 0.02
 C06F-C067 \\sim C06F-C05S
 with sigma of 0.02
 C4-C26 \\sim C26-C23
 with sigma of 0.05
 O4-N2 \\sim N1-O3
 with sigma of 0.05
3. Uiso/Uaniso restraints and constraints
C17 \\sim C15 \\sim C8 \\sim C19 \\sim N12 \\sim C18 \\sim C12 \\sim C10 \\sim
N7 \\sim C11: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
C3 \\sim N2 \\sim C6 \\sim C16 \\sim O4: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
O1: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C6 \\sim N2 \\sim C3 \\sim C16 \\sim O4: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
C35 \\sim C06M \\sim C66 \\sim N068 \\sim C06S \\sim C14 \\sim C20: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 N2, C3, C6, C16, O4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C5, C06S, C14, C20, C06M, C35, C66, N068
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Others
 Sof(H05P)=Sof(C067)=Sof(H067)=Sof(C058)=Sof(H058)=Sof(C04H)=Sof(C063)=
 Sof(H063)=Sof(C05S)=Sof(H05S)=Sof(C05J)=Sof(C06F)=Sof(N06G)=Sof(C06P)=
 Sof(H06P)=Sof(C5)=Sof(C1)=Sof(N11)=Sof(C27)=Sof(H27)=Sof(C7)=Sof(H7)=Sof(N10)=
 Sof(C9)=Sof(C2)=Sof(H2A)=Sof(C25)=Sof(H25)=Sof(C32)=Sof(H32)=Sof(N068)=
 Sof(C06S)=Sof(C14)=Sof(H14)=Sof(C20)=Sof(H20)=Sof(C06M)=1-FVAR(1)
 Sof(N051)=Sof(H05W)=Sof(C05Y)=Sof(H3)=Sof(N064)=Sof(C065)=Sof(C06I)=Sof(C06N)=
 Sof(H06Q)=Sof(C06O)=Sof(H06R)=Sof(C06R)=Sof(C06T)=Sof(H06T)=Sof(C21)=Sof(H21A)=
 Sof(H21B)=Sof(H21C)=Sof(C11)=Sof(H11)=Sof(N7)=Sof(C10)=Sof(C17)=Sof(H17A)=
 Sof(H17B)=Sof(H17C)=Sof(C19)=Sof(H19)=Sof(N12)=Sof(C18)=Sof(C12)=Sof(H12)=
 Sof(C8)=Sof(H8)=Sof(C15)=Sof(C06G)=Sof(C0)=Sof(H0)=Sof(C1C)=Sof(H1C)=Sof(C1D)=
 Sof(C1B)=Sof(H1B)=Sof(C1A)=Sof(H1A)=Sof(C24)=Sof(N1)=Sof(C26)=Sof(H26)=Sof(O3)=
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=
 Sof(H66)=FVAR(1)
6.a Riding coordinates:
 C3(H3A,H3B,H3C), C17(H17A,H17B,H17C), O1(H1D,H1E)
6.b Aromatic/amide H refined with riding coordinates:
 C00C(H00C), C00E(H00E), C00K(H00K), C00O(H00O), C00U(H00U), C00V(H00V),
 C00Y(H00Y), C010(H010), C011(H011), C018(H018), C01A(H01A), C01C(H01C),
 C01E(H01E), C01G(H01G), C01H(H01H), C01I(H01I), C01J(H01J), C01N(H01N),
 C01P(H01P), C01Q(H01Q), C01R(H01R), C01S(H01S), C01T(H01T), C01V(H01V),
 C01W(H01W), C01X(H01X), C01Y(H01Y), C020(H020), C022(H022), C023(H023),
 C025(H025), C026(H026), C029(H029), C02A(H02A), C02B(H02B), C02C(H02C),
 C02D(H02D), C02G(H02G), C02H(H02H), C02J(H02J), C02K(H02K), C02M(H02M),
 C02O(H02O), C02P(H02P), C02R(H02R), C02T(H02T), C02Y(H02Y), C02Z(H02Z),
 C031(H031), C032(H032), C033(H033), C037(H037), C03A(H03D), C03E(H03E),
 C03F(H03F), C03I(H03I), C03J(H03J), C03M(H03M), C03P(H03P), C03T(H03T),
 C03V(H03V), C03Z(H03Z), C041(H041), C043(H043), C044(H044), C047(H047),
 C049(H049), C04A(H04A), C04B(H04B), C04E(H04E), C04J(H04J), C04L(H04L),
 C04M(H04M), C04P(H04P), C04Q(H04Q), C04R(H04R), C04S(H04S), C04T(H04T),
 C04U(H04U), C04Y(H04Y), C04Z(H04Z), C050(H050), C052(H052), C056(H056),
 C057(H057), C05A(H05Q), C05B(H05T), C05E(H05Y), C05F(H05G), C05H(H05K),
 C05I(H05L), C05L(H05), C05M(H5), C05R(H05R), C05U(H1), C05V(H2), C05W(H05P),
 C05W(H05W), C05Y(H3), C05Z(H05Z), C062(H062), C067(H067), C058(H058),
 C063(H063), C05S(H05S), C06A(H06D), C06E(H06E), C06H(H06H), C06N(H06Q),
 C06O(H06R), C06P(H06P), C06Q(H06S), C06T(H06T), C16(H16), C11(H11), C19(H19),
 C12(H12), C8(H8), C27(H27), C7(H7), C2(H2A), C25(H25), C32(H32), C0(H0),
 C1C(H1C), C1B(H1B), C1A(H1A), C26(H26), C14(H14), C20(H20)
6.c Fitted hexagon refined as free rotating group:
 C35(N068,C06S,C14,C20,C06M)
6.d Idealised Me refined as rotating group:
 C03N(H03G,H03H,H03K), C03U(H03A,H03B,H03C), C04K(H04C,H04D,H04F), C04W(H04G,
 H04H,H04I), C054(H05A,H05B,H05C), C059(H05D,H05E,H05F), C05C(H05U,H05V,H05X),
 C05G(H05H,H05I,H05J), C05K(H4,H,HA), C05O(H05M,H05N,H05O), C061(H06J,H06K,
 H06L), C069(H06A,H06B,H06C), C06B(H06M,H06N,H06O), C06C(H06U,H06V,H06W),
 C06J(H06F,H06G,H06I), C13(H13A,H13B,H13C), C21(H21A,H21B,H21C), C6(H6A,H6B,
 H6C), C4(H4A,H4B,H4C), C23(H23A,H23B,H23C)
6.e :
 C66(H66)
;
_shelx_res_checksum              16707
_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 1.579
_oxdiff_exptl_absorpt_empirical_full_min 0.672