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_7132543
_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_formula_moiety         '2(C H2 Cl2), C34 H24 N4'
_chemical_formula_sum            'C36 H28 Cl4 N4'
_chemical_formula_weight         658.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 98.834(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.1218(6)
_cell_length_b                   7.9693(4)
_cell_length_c                   15.0239(9)
_cell_measurement_reflns_used    2903
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      71.3110
_cell_measurement_theta_min      4.0880
_cell_volume                     1552.44(14)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     27.00  88.00   1.00    2.00    --    0.00  37.00-180.00   61
  2  \w     -6.00  20.00   1.00    2.00    --    0.00  37.00-180.00   26
  3  \w    -87.00 -44.00   1.00    2.00    --    0.00 -37.00  60.00   43
  4  \w     36.00  88.00   1.00    2.00    --    0.00  37.00 -60.00   52
  5  \w      5.00  54.00   1.00    2.00    --    0.00  57.00-150.00   49
  6  \w    -37.00   4.00   1.00    2.00    --    0.00 -37.00  60.00   41
  7  \w    -13.00  30.00   1.00    2.00    --    0.00  37.00 -60.00   43
  8  \w     13.00  52.00   1.00    2.00    --   95.80 -77.00 150.00   39
  9  \w     42.00  68.00   1.00    2.00    --   95.80 -82.00-180.00   26
 10  \w      6.00  71.00   1.00    2.00    --   95.80 -77.00 -90.00   65
 11  \w     11.00 120.00   1.00    2.00    --   95.80 -61.00 -30.00  109
 12  \w     89.00 128.00   1.00    2.00    --   95.80 -82.00-180.00   39
 13  \w     92.00 132.00   1.00    2.00    --   95.80  15.00-150.00   40
 14  \w    148.00 185.00   1.00    2.00    --   95.80  15.00-150.00   37
 15  \w     27.00  64.00   1.00    2.00    --   95.80 -82.00 -90.00   37
 16  \w     80.00 158.00   1.00    2.00    --   95.80  61.00  90.00   78
 17  \w     56.00 122.00   1.00    2.00    --   95.80 -82.00 120.00   66
 18  \w     14.00  40.00   1.00    2.00    --   95.80 -82.00 120.00   26
 19  \w     94.00 124.00   1.00    2.00    --   95.80 -77.00 150.00   30
 20  \w     87.00 113.00   1.00    2.00    --   95.80 -82.00 -90.00   26
 21  \w     10.00  46.00   1.00    2.00    --   95.80 -82.00  30.00   36
 22  \w     92.00 127.00   1.00    2.00    --   95.80 -82.00  30.00   35
 23  \w      8.00 124.00   1.00    2.00    --   95.80 -82.00 -30.00  116
 24  \w     59.00  85.00   1.00    2.00    --   95.80 -77.00 150.00   26
 25  \w     76.00 164.00   1.00    2.00    --   95.80  30.00-120.00   88
 26  \w      7.00  76.00   1.00    2.00    --   95.80 -45.00 150.00   69
 27  \w     81.00 146.00   1.00    2.00    --   95.80  61.00 120.00   65
;
_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      0.0471762000
_diffrn_orient_matrix_UB_12      0.1581582000
_diffrn_orient_matrix_UB_13      -0.0360900000
_diffrn_orient_matrix_UB_21      -0.0326352000
_diffrn_orient_matrix_UB_22      0.1036204000
_diffrn_orient_matrix_UB_23      0.0774845000
_diffrn_orient_matrix_UB_31      0.1040963000
_diffrn_orient_matrix_UB_32      -0.0395771000
_diffrn_orient_matrix_UB_33      0.0589221000
_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  0.1086
_diffrn_reflns_av_unetI/netI     0.0811
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14584
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.049
_diffrn_reflns_theta_max         67.049
_diffrn_reflns_theta_min         4.168
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.724
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64273
_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    1.409
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.863
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0763
_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^)+(0.0762P)^2^+2.3584P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1969
_refine_ls_wR_factor_ref         0.2107
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2125
_reflns_number_total             2768
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04864k2.cif
_cod_data_source_block           exp_3502
_cod_depositor_comments
'Adding full bibliography for 7132542--7132545.cif.'
_cod_database_code               7132543
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.554
_shelx_estimated_absorpt_t_min   0.382
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), C17(H17)
;
_shelx_res_checksum              48058
_shelx_hkl_checksum              27237
_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 3.677
_oxdiff_exptl_absorpt_empirical_full_min 0.360