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_7132542
_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         'C112 H80 N16 Pd2, 2(B F4), 3(C2 H3 N)'
_chemical_formula_sum            'C118 H89 B2 F8 N19 Pd2'
_chemical_formula_weight         2159.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-05
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-09-29 deposited with the CCDC.	2023-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.02(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.567(3)
_cell_length_b                   22.094(4)
_cell_length_c                   18.901(4)
_cell_measurement_temperature    293(2)
_cell_volume                     5875(2)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.930
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.948
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_number            25580
_diffrn_reflns_point_group_measured_fraction_full 0.933
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.921
_diffrn_reflns_theta_min         2.895
_exptl_absorpt_coefficient_mu    0.372
_exptl_crystal_colour            'clear light brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       block
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.427
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details
;
 Flack x determined using 9683 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.52(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1344
_refine_ls_number_reflns         25580
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0931
_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^)+(0.1000P)^2^+20.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2469
_refine_ls_wR_factor_ref         0.2499
_reflns_Friedel_coverage         0.905
_reflns_Friedel_fraction_full    0.918
_reflns_Friedel_fraction_max     0.887
_reflns_number_gt                22854
_reflns_number_total             25580
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04864k2.cif
_cod_data_source_block           work
_cod_depositor_comments
'Adding full bibliography for 7132542--7132545.cif.'
_cod_database_code               7132542
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.923
_shelx_estimated_absorpt_t_min   0.890
_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. Rigid bond restraints
 N200, C201, C202
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N400, C401, C402
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C46, C47, C48, C49, C50, C45
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
N200 \\sim C201 \\sim C202: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
N400 \\sim C401 \\sim C402: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C47 \\sim C46 \\sim C45 \\sim C50 \\sim C49 \\sim C48: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
4.a Riding coordinates:
 C202(H20A,H20B,H20C)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C12(H12),
 C13(H13), C14(H14), C15(H15), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24),
  C25(H25), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C33(H33),
 C34(H34), C36(H36), C37(H37), C38(H38), C40(H40), C41(H41), C43(H43), C44(H44),
  C46(H46), C47(H47), C48(H48), C49(H49), C52(H52), C53(H53), C54(H54),
 C55(H55), C57(H57), C58(H58), C59(H59), C61(H61), C62(H62), C64(H64), C65(H65),
  C66(H66), C68(H68), C69(H69), C70(H70), C71(H71), C74(H74), C75(H75),
 C76(H76), C77(H77), C80(H80), C81(H81), C83(H83), C84(H84), C85(H85), C86(H86),
  C87(H87), C89(H89), C91(H91), C92(H92), C94(H94), C95(H95), C97(H97),
 C98(H98), C99(H99), C100(H100), C103(H103), C104(H104), C105(H105), C106(H106),
  C108(H108), C110(H110), C111(H111), C112(H112)
4.c Idealised Me refined as rotating group:
 C302(H30A,H30B,H30C), C402(H40A,H40B,H40C)
;
_shelx_res_checksum              26715
_shelx_hkl_checksum              29594
_olex2_submission_special_instructions 'No special instructions were received'