Self-assembly of conformation-adaptive dihydrophenazine-based coordination cages.
Wu, Meng-Xiang; Hong, Qiong-Yan; Li, Minghui; Jiang, Wei-Ling; Huang, Bin; Lu, Shuai; Wang, Heng; Yang, Hai-Bo; Zhao, Xiao-Li; Shi, Xueliang; Chemical communications (Cambridge, England) 60 (2024) 1184–1187; doi:10.1039/d3cc04864k

data_7132544
_publ_section_title
;
 Self-assembly of conformation-adaptive dihydrophenazine-based
 coordination cages.
;
_journal_issue                   9
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1184
_journal_page_last               1187
_journal_paper_doi               10.1039/d3cc04864k
_journal_volume                  60
_journal_year                    2024
_chemical_absolute_configuration unk
_chemical_formula_moiety         '1.5(C H2 Cl2), C28 H21 N4'
_chemical_formula_sum            'C29.5 H24 Cl3 N4'
_chemical_formula_weight         540.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-31
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-09-29 deposited with the CCDC.	2023-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.307(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.380(4)
_cell_length_b                   7.7267(9)
_cell_length_c                   12.8140(17)
_cell_measurement_reflns_used    1786
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      52.9530
_cell_measurement_theta_min      4.4920
_cell_volume                     2584.5(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (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      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -18.00  89.00   1.00    3.00    --    0.00  37.00-150.00  107
  2  \w    -89.00  16.00   1.00    3.00    --    0.00 -37.00-120.00  105
  3  \w    -23.00   2.00   1.00    3.00    --    0.00 -37.00 150.00   25
  4  \w    -88.00 -32.00   1.00    3.00    --    0.00 -57.00 -30.00   56
  5  \w    -10.00  23.00   1.00    3.00    --    0.00 -57.00  90.00   33
  6  \w      7.00  32.00   1.00    3.00    --   95.80 -82.00  30.00   25
  7  \w      7.00 113.00   1.00    3.00    --   95.80 -82.00 -30.00  106
  8  \w     51.00  88.00   1.00    3.00    --   95.80 -77.00 -90.00   37
  9  \w     64.00 127.00   1.00    3.00    --   95.80 -82.00 120.00   63
 10  \w     14.00 122.00   1.00    3.00    --   95.80 -15.00 120.00  108
 11  \w     76.00 159.00   1.00    3.00    --   95.80  30.00 -60.00   83
 12  \w     45.00 120.00   1.00    3.00    --   95.80 -61.00  90.00   75
 13  \w     75.00 128.00   1.00    3.00    --   95.80 -82.00-180.00   53
 14  \w     70.00 125.00   1.00    3.00    --   95.80 -82.00  30.00   55
 15  \w     73.00 115.00   1.00    3.00    --   95.80 -30.00   0.00   42
 16  \w     42.00  67.00   1.00    3.00    --   95.80 -45.00-180.00   25
 17  \w      7.00 120.00   1.00    3.00    --   95.80 -61.00 -30.00  113
 18  \w     21.00 123.00   1.00    3.00    --   95.80 -15.00 -30.00  102
 19  \w     13.00  38.00   1.00    3.00    --   95.80 -77.00 -90.00   25
 20  \w     60.00 101.00   1.00    3.00    --   95.80 -82.00-120.00   41
 21  \w     74.00  99.00   1.00    3.00    --   95.80 -82.00   0.00   25
 22  \w     16.00  79.00   1.00    3.00    --   95.80 -30.00  90.00   63
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0490364000
_diffrn_orient_matrix_UB_12      -0.0268618000
_diffrn_orient_matrix_UB_13      0.0794323000
_diffrn_orient_matrix_UB_21      0.0300808000
_diffrn_orient_matrix_UB_22      -0.0408850000
_diffrn_orient_matrix_UB_23      -0.0914841000
_diffrn_orient_matrix_UB_31      0.0131416000
_diffrn_orient_matrix_UB_32      0.1933698000
_diffrn_orient_matrix_UB_33      -0.0085890000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1695
_diffrn_reflns_av_unetI/netI     0.1938
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12548
_diffrn_reflns_point_group_measured_fraction_full 0.797
_diffrn_reflns_point_group_measured_fraction_max 0.797
_diffrn_reflns_theta_full        67.066
_diffrn_reflns_theta_max         67.066
_diffrn_reflns_theta_min         4.497
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.417
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68323
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (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    1.390
_exptl_crystal_description       plate
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Flack x determined using 319 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         3675
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.1625
_refine_ls_R_factor_gt           0.0958
_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^)+(0.1601P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2678
_refine_ls_wR_factor_ref         0.3543
_reflns_Friedel_coverage         0.476
_reflns_Friedel_fraction_full    0.559
_reflns_Friedel_fraction_max     0.559
_reflns_number_gt                2112
_reflns_number_total             3675
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04864k2.cif
_cod_data_source_block           exp_3500
_cod_depositor_comments
'Adding full bibliography for 7132542--7132545.cif.'
_cod_original_formula_sum        'C29.50 H24 Cl3 N4'
_cod_database_code               7132544
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.408
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 Cl4-C30
 1.7 with sigma of 0.01
 Cl3-C30
 1.7 with sigma of 0.01
3. Rigid bond restraints
 Cl3, Cl4, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Cl3 \\sim Cl4 \\sim C30: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
5. Others
 Fixed Sof: Cl3(0.5) Cl4(0.5) C30(0.5) H30A(0.5) H30B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C30(H30A,H30B)
6.b Aromatic/amide H refined with riding coordinates:
 N4(H4), C1(H1), C3(H3), C4(H4A), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10),
 C13(H13), C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21),
  C24(H24), C25(H25), C27(H27), C28(H28)
;
_shelx_res_checksum              26864
_shelx_hkl_checksum              60984
_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 3.201
_oxdiff_exptl_absorpt_empirical_full_min 0.269