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_7132545
_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         'C204 H144 N24 Pd3, 6(B F4)'
_chemical_formula_sum            'C204 H144 B6 F24 N24 Pd3'
_chemical_formula_weight         3771.48
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-09-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-09-29 deposited with the CCDC.	2023-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                110.4510(10)
_cell_angle_beta                 94.9270(10)
_cell_angle_gamma                100.3290(10)
_cell_formula_units_Z            2
_cell_length_a                   16.7748(3)
_cell_length_b                   28.6322(5)
_cell_length_c                   29.6738(5)
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    307(2)
_cell_measurement_theta_max      51.066
_cell_measurement_theta_min      2.361
_cell_volume                     12965.9(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      307.0
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.1111
_diffrn_reflns_av_unetI/netI     0.1444
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            157808
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.015
_diffrn_reflns_theta_min         2.360
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.451
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.4524
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1333 before and 0.0529 after correction. The Ratio of minimum to maximum transmission is 0.6026. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    0.966
_exptl_crystal_description       block
_exptl_crystal_F_000             3840
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.892
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2433
_refine_ls_number_reflns         48916
_refine_ls_number_restraints     2107
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.2494
_refine_ls_R_factor_gt           0.1022
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+45.2688P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2379
_refine_ls_wR_factor_ref         0.3090
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17351
_reflns_number_total             48916
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04864k2.cif
_cod_data_source_block           mj22352_0m
_cod_depositor_comments
'Adding full bibliography for 7132542--7132545.cif.'
_cod_database_code               7132545
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.905
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 B4-F15
 1.4 with sigma of 0.01
 F13-B4
 1.4 with sigma of 0.01
 B4-F16
 1.4 with sigma of 0.01
 F8-B2
 1.4 with sigma of 0.01
 B2-F6
 1.4 with sigma of 0.01
 B2-F5
 1.4 with sigma of 0.01
 B6-F18
 1.4 with sigma of 0.01
 B6-F20
 1.4 with sigma of 0.01
 B6-F19
 1.4 with sigma of 0.01
 B6-F17
 1.4 with sigma of 0.01
 B1-F3
 1.4 with sigma of 0.01
 B1-F4
 1.4 with sigma of 0.01
 F2-B1
 1.4 with sigma of 0.01
 B1-F1
 1.4 with sigma of 0.01
 B2-F7
 1.4 with sigma of 0.01
 B4-F14
 1.4 with sigma of 0.01
 F21-F22
 2.2 with sigma of 0.01
 F21-F24
 2.2 with sigma of 0.01
 F24-F23
 2.2 with sigma of 0.01
 F22-F23
 2.2 with sigma of 0.01
 F22-F24
 2.2 with sigma of 0.01
 F21-F23
 2.2 with sigma of 0.01
 F6-F5
 2.2 with sigma of 0.01
 F6-F8
 2.2 with sigma of 0.01
 F7-F6
 2.2 with sigma of 0.01
 F5-F8
 2.2 with sigma of 0.01
 F8-F7
 2.2 with sigma of 0.01
 F3-F1
 2.2 with sigma of 0.01
 F4-F2
 2.2 with sigma of 0.01
 F4-F3
 2.2 with sigma of 0.01
 F4-F1
 2.2 with sigma of 0.01
 F2-F1
 2.2 with sigma of 0.01
 F2-F3
 2.2 with sigma of 0.01
 F10-B0AA
 1.4 with sigma of 0.01
 F10-F1AA
 2.2 with sigma of 0.01
 F9-F1AA
 2.2 with sigma of 0.01
 F10-F9
 2.2 with sigma of 0.01
 F10-F0AA
 2.2 with sigma of 0.01
 F0AA-F1AA
 2.2 with sigma of 0.01
 B0AB-F0AB
 1.4 with sigma of 0.01
 B0AB-F1AB
 1.4 with sigma of 0.01
 B0AB-F9A
 1.4 with sigma of 0.01
 B0AB-F10A
 1.4 with sigma of 0.01
 F0AB-F9A
 2.2 with sigma of 0.01
 F1AB-F9A
 2.2 with sigma of 0.01
 F1AB-F10A
 2.2 with sigma of 0.01
 F9A-F10A
 2.2 with sigma of 0.01
 F0AB-F1AB
 2.2 with sigma of 0.01
 F10A-F0AB
 2.2 with sigma of 0.01
 B0AA-F0AA
 1.4 with sigma of 0.01
 F1AA-B0AA
 1.4 with sigma of 0.01
 B0AA-F9
 1.4 with sigma of 0.01
 B0AA-F10
 1.4 with sigma of 0.01
 B5-F22
 1.4 with sigma of 0.01
 B5-F24
 1.4 with sigma of 0.01
 B5-F23
 1.4 with sigma of 0.01
 B5-F21
 1.4 with sigma of 0.01
 B5-F24A
 1.4 with sigma of 0.01
 B5-F22A
 1.4 with sigma of 0.01
 B5-F21A
 1.4 with sigma of 0.01
 B5-F23A
 1.4 with sigma of 0.01
 F24A-F22A
 2.2 with sigma of 0.01
 F24A-F23A
 2.2 with sigma of 0.01
 F21A-F22A
 2.2 with sigma of 0.01
 F23A-F21A
 2.2 with sigma of 0.01
 F24-B5 \\sim F23-B5 \\sim F22-B5 \\sim F21-B5
 with sigma of 0.02
 F23-F22 \\sim F21-F24
 with sigma of 0.02
 F10-B0AA \\sim F9-B0AA \\sim F0AA-B0AA \\sim F1AA-B0AA
 with sigma of 0.02
 F1AB-B0AB \\sim F9A-B0AB \\sim F10A-B0AB \\sim F0AB-B0AB
 with sigma of 0.02
3. Rigid bond restraints
 B2, F7, F8, F5, F6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 B1, F3, F2, F1, F4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 B6, F18, F19, F17, F20
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 B5, F24
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F10, F9, B0AA, F1AA, F0AA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F9A, B0AB, F10A, F0AB, F1AB
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 B0AB, F9A, F10A, F1AB, F0AB, F24A, F23A, F21A, F22A, B5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
B2 \\sim F7 \\sim F8 \\sim F6 \\sim F5: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
B1 \\sim F3 \\sim F1 \\sim F4 \\sim F2: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
B6 \\sim F18 \\sim F19 \\sim F17 \\sim F20: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
B5 \\sim F21 \\sim F24 \\sim F23 \\sim F22: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
F9 \\sim F10 \\sim B0AA \\sim F1AA \\sim F0AA: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
B0AB \\sim F10A \\sim F9A \\sim F0AB \\sim F1AB: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
B5 \\sim F23A \\sim F24A \\sim F21A \\sim F22A: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
Uanis(F9) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
5. Others
 Sof(B0AB)=Sof(F9A)=Sof(F10A)=Sof(F1AB)=Sof(F0AB)=1-FVAR(1)
 Sof(B0AA)=Sof(F1AA)=Sof(F9)=Sof(F10)=Sof(F0AA)=FVAR(1)
 Sof(F24A)=Sof(F23A)=Sof(F21A)=Sof(F22A)=1-FVAR(2)
 Sof(F24)=Sof(F23)=Sof(F22)=Sof(F21)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C103(H103), C171(H171), C98(H98), C170(H170), C28(H28), C78(H78), C113(H113),
 C30(H30), C175(H175), C64(H64), C79(H79), C94(H94), C200(H200), C147(H147),
 C137(H137), C132(H132), C39(H39), C136(H136), C73(H73), C5(H5), C75(H75),
 C35(H35), C141(H141), C130(H130), C107(H107), C112(H112), C93(H93), C76(H76),
 C29(H29), C199(H199), C82(H82), C96(H96), C139(H139), C146(H146), C180(H180),
 C84(H84), C26(H26), C1(H1), C128(H128), C105(H105), C8(H8), C34(H34), C69(H69),
  C134(H134), C181(H181), C71(H71), C72(H72), C37(H37), C42(H42), C173(H173),
 C81(H81), C140(H140), C19(H19), C41(H41), C22(H22), C165(H165), C106(H106),
 C122(H122), C164(H164), C109(H109), C123(H123), C97(H97), C174(H174), C25(H25),
  C153(H153), C125(H125), C159(H159), C14(H14), C166(H166), C115(H115),
 C162(H162), C91(H91), C7(H7), C133(H133), C186(H186), C131(H131), C83(H83),
 C143(H143), C198(H198), C68(H68), C63(H63), C192(H192), C116(H116), C127(H127),
  C60(H60), C110(H110), C118(H118), C17(H17), C204(H204), C150(H150),
 C100(H100), C102(H102), C189(H189), C62(H62), C36(H36), C32(H32), C54(H54),
 C59(H59), C57(H57), C195(H195), C44(H44), C168(H168), C124(H124), C152(H152),
 C161(H161), C167(H167), C144(H144), C196(H196), C10(H10), C202(H202), C15(H15),
  C90(H90), C158(H158), C2(H2), C55(H55), C185(H185), C33(H33), C45(H45),
 C20(H20), C88(H88), C21(H21), C117(H117), C156(H156), C16(H16), C89(H89),
 C3(H3), C151(H151), C183(H183), C49(H49), C101(H101), C66(H66), C184(H184),
 C177(H177), C56(H56), C203(H203), C46(H46), C178(H178), C191(H191), C47(H47),
 C190(H190), C11(H11), C67(H67), C48(H48), C157(H157)
;
_shelx_res_checksum              50786
_shelx_hkl_checksum              5349
_olex2_submission_special_instructions 'No special instructions were received'