Creation of single molecular conjugates of metal-organic cages and DNA.
Nakajo, Toshinobu; Kusaka, Shinpei; Hiraoka, Haruka; Nomura, Kohei; Matsubara, Noriaki; Baba, Rintaro; Yoshida, Yuki; Nakamoto, Kosuke; Honma, Masakazu; Iguchi, Hiroaki; Uchihashi, Takayuki; Abe, Hiroshi; Matsuda, Ryotaro; Chemical communications (Cambridge, England) 59 (2023) 4974–4977; doi:10.1039/d3cc00460k

data_7131500
_publ_section_title
;
 Creation of single molecular conjugates of metal-organic cages and DNA.
;
_journal_issue                   33
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4974
_journal_page_last               4977
_journal_paper_doi               10.1039/d3cc00460k
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C84 H96 N9 O20 Zr6, 1(Cl2)'
_chemical_formula_sum            'C84 H96 Cl2 N9 O20 Zr6'
_chemical_formula_weight         2169.91
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-10-31 deposited with the CCDC.	2023-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   18.9840(10)
_cell_length_b                   18.9840(10)
_cell_length_c                   51.415(2)
_cell_measurement_reflns_used    11592
_cell_measurement_temperature    297
_cell_measurement_theta_max      22.3860
_cell_measurement_theta_min      2.1910
_cell_volume                     16047.1(13)
_computing_cell_refinement       'CrysAlisPro 1.171.41.91a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.91a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.91a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      297
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.884
_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    -75.00  -8.00   0.50   90.00    --   -3.50 -38.00 -90.00  134
  2  \w    -30.00  34.00   0.50   90.00    --   -3.50 -82.00  90.00  128
  3  \w    -91.00 -45.00   0.50   90.00    --   -3.50 -57.00  30.00   92
  4  \w    -40.00  -1.00   0.50   90.00    --   -3.50 -57.00  30.00   78
  5  \w    -30.00  41.00   0.50   90.00    --    3.80 -82.00-120.00  142
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0312122000
_diffrn_orient_matrix_UB_12      -0.0092472000
_diffrn_orient_matrix_UB_13      0.0024618000
_diffrn_orient_matrix_UB_21      -0.0094687333
_diffrn_orient_matrix_UB_22      -0.0039558667
_diffrn_orient_matrix_UB_23      0.0134637333
_diffrn_orient_matrix_UB_31      -0.0281874000
_diffrn_orient_matrix_UB_32      -0.0419720000
_diffrn_orient_matrix_UB_33      -0.0018282000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1905
_diffrn_reflns_av_unetI/netI     0.1713
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_limit_l_min       -70
_diffrn_reflns_number            51674
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.521
_diffrn_reflns_theta_min         2.011
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.674
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.91a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_description       plate
_exptl_crystal_F_000             6582
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.809
_refine_diff_density_min         -0.983
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         8823
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.1963
_refine_ls_R_factor_gt           0.0772
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1231P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1825
_refine_ls_wR_factor_ref         0.2389
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3508
_reflns_number_total             8823
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00460k3.cif
_cod_data_source_block           20220803_cps-mop-tere-n3_auto
_cod_depositor_comments
'Adding full bibliography for 7131499--7131500.cif.'
_cod_original_cell_volume        16047.2(18)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7131500
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.987
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
Zr01 \\sim Zr01 \\sim Zr01 \\sim Cl1: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(Cl1) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
3. Rigid body (RIGU) restrains
 Zr01, Zr01, Cl1, Zr01
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: N16(0.5) N12(0.5) N5(0.5) N10(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C00I(H00I), C00K(H00K)
5.b Idealised Me refined as rotating group:
 C00T(H00A,H00B,H00C), C00V(H00D,H00E,H00F), C00W(H00G,H00H,H00J), C00X(H00L,
 H00M,H00N), C010(H01A,H01B,H01C), C012(H01D,H01E,H01F), C013(H01G,H01H,H01I),
 C015(H01J,H01K,H01L), C017(H01M,H01N,H01O), C019(H01P,H01Q,H01R)
;
_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 2.164
_oxdiff_exptl_absorpt_empirical_full_min 0.580