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_7712875
_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         'C64 H45 Br2 N7'
_chemical_formula_sum            'C64 H42 Br2 N7'
_chemical_formula_weight         1068.86
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-25
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-04-25 deposited with the CCDC.	2023-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                101.4560(16)
_cell_angle_beta                 98.3563(16)
_cell_angle_gamma                107.5337(16)
_cell_formula_units_Z            2
_cell_length_a                   11.3268(2)
_cell_length_b                   15.5229(3)
_cell_length_c                   17.3816(3)
_cell_measurement_reflns_used    26413
_cell_measurement_temperature    99.93(18)
_cell_measurement_theta_max      30.8080
_cell_measurement_theta_min      2.2970
_cell_volume                     2786.40(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.93(18)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.846
_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      2.00  27.00   0.50    9.05    --    4.36 -76.00  -9.00   50
  2  \w    -46.00 -12.00   0.50    9.05    --    4.36 -76.00  -9.00   68
  3  \w     17.00  52.00   0.50    9.05    --    4.36  76.00 117.00   70
  4  \w    -28.00  39.00   0.50    9.05    --   -6.08  76.00 117.00  134
  5  \w    -11.00  27.00   0.50    9.05    --   -6.08 -99.00 150.00   76
  6  \w    -15.00  26.00   0.50    9.05    --   -6.08 -99.00-150.00   82
  7  \w    -19.00  68.00   0.50    9.05    --   -6.08  32.00 -22.11  174
  8  \w    -17.00  27.00   0.50    9.05    --   -6.08 -99.00   0.00   88
  9  \w    -19.00   7.00   0.50    9.05    --   -6.08  34.00 124.50   52
 10  \w     19.00  67.00   0.50    9.05    --   -6.08  34.00 124.50   96
 11  \w    -50.00  -8.00   0.50    9.05    --   -6.08 117.00 -44.68   84
 12  \w    -19.00  65.00   0.50    9.05    --   -6.08  33.00  57.79  168
 13  \w    -19.00  68.00   0.50    9.05    --   -6.08  34.00-157.97  174
 14  \w    -19.00  50.00   0.50    9.05    --   -6.08  19.00 -60.00  138
 15  \w    -79.00 -24.00   0.50    9.05    --   -6.08 -76.00  -9.00  110
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0451830000
_diffrn_orient_matrix_UB_12      -0.0103889000
_diffrn_orient_matrix_UB_13      -0.0210920000
_diffrn_orient_matrix_UB_21      -0.0165058000
_diffrn_orient_matrix_UB_22      0.0235772000
_diffrn_orient_matrix_UB_23      -0.0286319000
_diffrn_orient_matrix_UB_31      0.0470885000
_diffrn_orient_matrix_UB_32      0.0423656000
_diffrn_orient_matrix_UB_33      0.0235961000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0710
_diffrn_reflns_av_unetI/netI     0.0596
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.846
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            75324
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.846
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.896
_diffrn_reflns_theta_min         2.291
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.500
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
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    1.274
_exptl_crystal_description       block
_exptl_crystal_F_000             1090
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.092
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     674
_refine_ls_number_reflns         14885
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0648P)^2^+0.4612P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1208
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10873
_reflns_number_total             14885
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00897e2.cif
_cod_data_source_block           exp_1899_zwy_197_auto
_cod_original_cell_volume        2786.38(9)
_cod_database_code               7712875
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H Br Cl N Ru'
_chemical_oxdiff_usercomment     zwy_197
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.841
_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.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C9(H9), C10(H10), C13(H13), C19(H19), C23(H23), C25(H25), C26(H26),
 C29(H29), C33(H33), C34(H34), C37(H37), C38(H38), C39(H39), C41(H41), C42(H42),
  C43(H43), C45(H45), C46(H46), C47(H47), C49(H49), C50(H50), C51(H51),
 C52(H52), C53(H53), C55(H55), C56(H56), C58(H58), C59(H59), C60(H60)
2.b Idealised Me refined as rotating group:
 C57(H57A,H57B,H57C), C61(H61A,H61B,H61C), C63(H63A,H63B,H63C), C64(H64A,H64B,
 H64C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 147 electrons were 
found in a volume of 520\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
4[CH3OH] per Asymmetric Unit 
which account for 144 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              57844
_shelx_fab_checksum              69522
_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 3.418
_oxdiff_exptl_absorpt_empirical_full_min 0.295