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_7131499
_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         'C120 H120 N9 O20 Zr6, 2(Cl)'
_chemical_formula_sum            'C120 H120 Cl2 N9 O20 Zr6'
_chemical_formula_weight         2626.46
_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                   17.7435(7)
_cell_length_b                   17.7435(7)
_cell_length_c                   71.981(2)
_cell_measurement_reflns_used    20663
_cell_measurement_temperature    93
_cell_measurement_theta_max      26.8770
_cell_measurement_theta_min      2.5640
_cell_volume                     19625.8(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_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      93
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.888
_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      0.00  31.16   0.38   30.00    --   -3.40 -82.00  60.00   82
  2  \w    -84.00 -51.70   0.38   30.00    --   -3.40 -82.00  60.00   85
  3  \w    -87.00 -51.66   0.38   30.00    --   -3.40 -19.00  30.00   93
  4  \w    -48.00  35.22   0.38   30.00    --   -3.40 -19.00  30.00  219
  5  \w    -92.00 -13.34   0.38   30.00    --   -3.40 -38.00-180.00  207
  6  \w    -25.00   1.22   0.38   30.00    --    3.90  57.00-150.00   69
;
_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      -0.0287252667
_diffrn_orient_matrix_UB_12      -0.0274739333
_diffrn_orient_matrix_UB_13      0.0070034667
_diffrn_orient_matrix_UB_21      -0.0322802333
_diffrn_orient_matrix_UB_22      0.0094568333
_diffrn_orient_matrix_UB_23      -0.0031150667
_diffrn_orient_matrix_UB_31      -0.0163080000
_diffrn_orient_matrix_UB_32      -0.0359044000
_diffrn_orient_matrix_UB_33      -0.0061854000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.888
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       97
_diffrn_reflns_limit_l_min       -89
_diffrn_reflns_number            63539
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.232
_diffrn_reflns_theta_min         2.296
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.564
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       needle
_exptl_crystal_F_000             8022
_exptl_crystal_size_max          1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.810
_refine_diff_density_min         -1.149
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         10565
_refine_ls_number_restraints     569
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1272
_refine_ls_R_factor_gt           0.0758
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1375P)^2^+74.7864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2167
_refine_ls_wR_factor_ref         0.2533
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5981
_reflns_number_total             10565
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00460k3.cif
_cod_data_source_block           20210708
_cod_depositor_comments
'Adding full bibliography for 7131499--7131500.cif.'
_cod_original_cell_volume        19625.8(17)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7131499
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.602
_reflns_odcompleteness_completeness 99.89
_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. Restrained distances
 N1-N2
 1.244 with sigma of 0.02
 N7-N8
 1.244 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N1 \\sim N2 \\sim N0AA: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
N0AA \\sim N7 \\sim N8: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 1*[Sof(N8)+Sof(N7)]+1*[Sof(N1)+Sof(N2)]=1 with esd of 0.0001
 Sof(N8)=Sof(N7)=FVAR(1)
 Sof(N1)=Sof(N2)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C00F(H00F), C00I(H00I), C00J(H00J), C00L(H00L), C00M(H00M), C00P(H00P),
 C00X(H00X), C00Z(H00Z), C010(H010), C012(H012)
6.b Idealised Me refined as rotating group:
 C013(H01A,H01B,H01C), C014(H01D,H01E,H01F), C017(H01G,H01H,H01I), C019(H01J,
 H01K,H01L), C01A(H01M,H01N,H01O), C01C(H01P,H01Q,H01R), C01D(H01S,H01T,H01U),
 C01F(H01V,H01W,H01X), C01G(H01Y,H,HA), C01H(H01Z,HB,HC)
;
_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 1.797
_oxdiff_exptl_absorpt_empirical_full_min 0.612