Stacking-interaction-induced host-guest chemistry and Borromean rings based on a polypyridyl ligand.
Zhang, Hai-Ning; Gao, Wen-Xi; Deng, Yu-Xin; Lin, Yue-Jian; Jin, Guo-Xin; Chemical communications (Cambridge, England) 54 (2018) 1559–1562; doi:10.1039/c7cc09448e

data_7121014
_publ_section_title
;
 Stacking-interaction-induced host-guest chemistry and Borromean rings
 based on a polypyridyl ligand.
;
_journal_issue                   13
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1559
_journal_page_last               1562
_journal_paper_doi               10.1039/c7cc09448e
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety
'C128 H108 N16 Rh4, 7.33(C F3 O3 S), 3.33(C2 H3 N), 2.67(C O)'
_chemical_formula_sum            'C168 H192 F24 N28 O40 Rh4 S8'
_chemical_formula_weight         4367.60
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-07-14
_audit_creation_method
; 
Olex2 1.2-beta 
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) 
;
_audit_update_record
;
2017-11-21 deposited with the CCDC.
2017-12-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.492(3)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   26.607(4)
_cell_length_b                   31.867(5)
_cell_length_c                   33.813(5)
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.49
_cell_measurement_theta_min      2.36
_cell_volume                     28581(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1345
_diffrn_reflns_av_unetI/netI     0.1478
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            165754
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.150
_diffrn_reflns_theta_max         25.150
_diffrn_reflns_theta_min         0.879
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.532
_exptl_absorpt_correction_T_max  0.6466
_exptl_absorpt_correction_T_min  0.5246
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2008/1 (Bruker,2008) was used for absorption correction. 
wR2(int) was 0.1054 before and 0.0824 after correction. 
The Ratio of minimum to maximum transmission is 0.8113. 
The \l/2 correction factor is 0.0015. 
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       block
_exptl_crystal_F_000             13440
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.33
_refine_diff_density_max         2.119
_refine_diff_density_min         -1.475
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2586
_refine_ls_number_reflns         51040
_refine_ls_number_restraints     760
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.2228
_refine_ls_R_factor_gt           0.1563
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1356P)^2^+801.4222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3705
_refine_ls_wR_factor_ref         0.4106
_reflns_Friedel_coverage         0.000
_reflns_number_gt                29460
_reflns_number_total             51040
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc09448e2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7121010--7121014.cif.'
_cod_database_code               7121014
_shelx_estimated_absorpt_t_max   0.844
_shelx_estimated_absorpt_t_min   0.807
_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 
 C217-O39 
 1.42 with sigma of 0.03 
 F31-F32 = F31-F33 = F32-F33 
 2.1 with sigma of 0.03 
 C203-F31 = C203-F32 = C203-F33 
 1.35 with sigma of 0.02 
 C202-F28 = C202-F29 = C202-F30 
 1.35 with sigma of 0.02 
 C201-F25 = C201-F26 = C201-F27 
 1.35 with sigma of 0.02 
 C200-F22 = C200-F23 = C200-F24 
 1.35 with sigma of 0.02 
 C199-F19 = C199-F20 = C199-F21 
 1.35 with sigma of 0.02 
 C298-F16' = C298-F17' = C298-F18' 
 1.35 with sigma of 0.02 
 C198-F16 = C198-F17 = C198-F18 
 1.35 with sigma of 0.02 
 S6'-O16' = S6'-O17' = S6'-O18' = S8-O22 = S10-O29 
 1.42 with sigma of 0.02 
 S11-O31 = S11-O32 = S11-O33 
 1.42 with sigma of 0.02 
 S6'-C298 
 1.8 with sigma of 0.02 
 C195-F7 = C195-F8 = C195-F9 
 1.35 with sigma of 0.02 
 C194-F4 = C194-F5 = C194-F6 
 1.35 with sigma of 0.02 
3. Uiso/Uaniso restraints and constraints 
F16 \\sim F16': within 2A with sigma of 0.02 and sigma for terminal atoms of 
0.05 
O17 \\sim O18 \\sim O17' \\sim O18': within 2A with sigma of 0.02 and sigma for 
terminal atoms of 0.05 
C45 \\sim C46 \\sim C50 \\sim C51 \\sim C45' \\sim C46' \\sim C50' \\sim C51': 
within 2A with sigma of 0.02 and sigma for terminal atoms of 0.05 
Uanis(O17') \\sim Ueq, Uanis(O18') \\sim Ueq, Uanis(C298) \\sim Ueq, 
Uanis(F16') \\sim Ueq, Uanis(F18') \\sim Ueq: with sigma of 0.02 and sigma for 
terminal atoms of 0.04 
Uanis(O16) \\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(C198) \\sim Ueq, Uanis(F16) 
\\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F18) \\sim Ueq, Uanis(O16') \\sim Ueq: 
with sigma of 0.02 and sigma for terminal atoms of 0.04 
Uanis(C45') \\sim Ueq, Uanis(C46') \\sim Ueq, Uanis(C48') \\sim Ueq, 
Uanis(C49') \\sim Ueq, Uanis(C50') \\sim Ueq, Uanis(C51') \\sim Ueq, 
Uanis(C52') \\sim Ueq, Uanis(C53') \\sim Ueq, Uanis(C54') \\sim Ueq: with sigma 
of 0.02 and sigma for terminal atoms of 0.04 
Uanis(S6) \\sim Ueq, Uanis(S6') \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46) 
\\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq, 
Uanis(C50) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C54) 
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04 
Uanis(O7) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O13) \\sim 
Ueq, Uanis(O14) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(O22) \\sim Ueq, 
Uanis(O23) \\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(O26) 
\\sim Ueq, Uanis(O27) \\sim Ueq: with sigma of 0.02 and sigma for terminal 
atoms of 0.04 
Uanis(O28) \\sim Ueq, Uanis(O29) \\sim Ueq, Uanis(O30) \\sim Ueq, Uanis(O31) 
\\sim Ueq, Uanis(O32) \\sim Ueq, Uanis(O33) \\sim Ueq, Uanis(S7) \\sim Ueq, 
Uanis(S11) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04 
Uanis(F4) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F7) \\sim 
Ueq, Uanis(F8) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F23) 
\\sim Ueq, Uanis(F31) \\sim Ueq, Uanis(F32) \\sim Ueq, Uanis(F33) \\sim Ueq: 
with sigma of 0.02 and sigma for terminal atoms of 0.04 
Uanis(C4) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C71) 
\\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C73) \\sim Ueq: with sigma of 0.02 and 
sigma for terminal atoms of 0.04 
Uanis(C117) \\sim Ueq, Uanis(C118) \\sim Ueq, Uanis(C119) \\sim Ueq, 
Uanis(C120) \\sim Ueq, Uanis(C121) \\sim Ueq, Uanis(C125) \\sim Ueq, 
Uanis(C126) \\sim Ueq, Uanis(C127) \\sim Ueq, Uanis(C128) \\sim Ueq: with sigma 
of 0.02 and sigma for terminal atoms of 0.04 
Uanis(C179) \\sim Ueq, Uanis(C199) \\sim Ueq, Uanis(C200) \\sim Ueq, 
Uanis(C201) \\sim Ueq, Uanis(C202) \\sim Ueq, Uanis(C203) \\sim Ueq: with sigma 
of 0.02 and sigma for terminal atoms of 0.04 
Uanis(C207) \\sim Ueq, Uanis(C208) \\sim Ueq, Uanis(N26) \\sim Ueq, Uanis(C211) 
\\sim Ueq, Uanis(C213) \\sim Ueq, Uanis(C214) \\sim Ueq, Uanis(N29) \\sim Ueq: 
with sigma of 0.02 and sigma for terminal atoms of 0.04 
Uanis(C216) \\sim Ueq, Uanis(C217) \\sim Ueq, Uanis(C218) \\sim Ueq, Uanis(O38) 
\\sim Ueq, Uanis(O39) \\sim Ueq, Uanis(O40) \\sim Ueq: with sigma of 0.02 and 
sigma for terminal atoms of 0.04 
Uanis(C53) \\sim Ueq, Uanis(C47') \\sim Ueq, Uanis(C122) \\sim Ueq, Uanis(O17) 
\\sim Ueq, Uanis(F17') \\sim Ueq: with sigma of 0.01 and sigma for terminal 
atoms of 0.02 
4. Others 
 Sof(S6')=Sof(O16')=Sof(O17')=Sof(O18')=Sof(C298)=Sof(F16')=Sof(F17')= 
 Sof(F18')=1-FVAR(1) 
 Sof(S6)=Sof(O16)=Sof(O17)=Sof(O18)=Sof(C198)=Sof(F16)=Sof(F17)=Sof(F18)=FVAR(1) 
 Sof(C45')=Sof(C46')=Sof(C47')=Sof(C48')=Sof(C49')=Sof(C50')=Sof(H50D)= 
 Sof(H50E)=Sof(H50F)=Sof(C51')=Sof(H51D)=Sof(H51E)=Sof(H51F)=Sof(C52')= 
 Sof(H52D)=Sof(H52E)=Sof(H52F)=Sof(C53')=Sof(H53D)=Sof(H53E)=Sof(H53F)= 
 Sof(C54')=Sof(H54D)=Sof(H54E)=Sof(H54F)=1-FVAR(2) 
 Sof(C45)=Sof(C46)=Sof(C47)=Sof(C48)=Sof(C49)=Sof(C50)=Sof(H50A)=Sof(H50B)= 
 Sof(H50C)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(H51C)=Sof(C52)=Sof(H52A)=Sof(H52B)= 
 Sof(H52C)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=Sof(C54)=Sof(H54A)=Sof(H54B)= 
 Sof(H54C)=FVAR(2) 
5.a : 
 C45(C46,C47,C48,C49,C50,C51,C52,C53,C54,C45',C46',C47',C48',C49',C50',C51', 
 C52',C53',C54',C55,C56,C57,C58,C59,C60,C61,C62,C63,C64,C65,C66,C67,C68,C69,C70, 
 C71,C72,C73,C74,C75,C76,C77,C78,C79,C80,C81,C82,C83,C84,C85,C86,C87,C88,C89, 
 C90,C91,C92,C93,C94,C95,C96,C97,C98,C99,C100,C101,C102,C103,C104,C105,C106, 
 C107,C108,C109,C110,C111,C112,C113,C114,C115,C116,C117,C118,C119,C120,C121, 
 C122,C123,C124,C125,C126,C127,C128,C129,C130,C131,C132,C133,C134,C135,C136, 
 C137,C138,C139,C140,C141,C142,C143,C144,C145,C146,C147,C148,C149,C150,C151, 
 C152,C153,C154,C155,C156,C157,C158,C159,C160,C161,C162,C163,C164,C165,C166, 
 C167,C168,C169,C170,C171,C172,C173,C174,C175,C176,C177,C178,C179,C180,C181, 
 C182,C183,C184,C185,C186,C187,C188,C189,C190,C191,C192,C193,C194,C195,C196, 
 C197,S6,O16,O17,O18,C198,F16,F17,F18,S6',O16',O17',O18',C298,F16',F17',F18', 
 C199,C200,C201,C202,C203,C205,C206,N25,C207,C208,N26,C209,C210,N27,C211,C212, 
 N28,C213,C214,N29,C215,C216,C217,C218,O37,O38,O39,O40) 
5.b Me refined with riding coordinates: 
 C51(H51A,H51B,H51C), C50'(H50D,H50E,H50F) 
5.c Aromatic/amide H refined with riding coordinates: 
 C1(H1), C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C15(H15), C16(H16), 
 C17(H17), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), 
  C33(H33), C34(H34), C36(H36), C37(H37), C40(H40), C41(H41), C43(H43), 
 C44(H44), C65(H65), C66(H66), C67(H67), C72(H72), C73(H73), C74(H74), C79(H79), 
  C80(H80), C81(H81), C86(H86), C87(H87), C88(H88), C89(H89), C90(H90), 
 C92(H92), C93(H93), C97(H97), C98(H98), C100(H100), C101(H101), C104(H104), 
 C105(H105), C107(H107), C108(H108), C129(H129), C130(H130), C131(H131), 
 C136(H136), C137(H137), C138(H138), C143(H143), C144(H144), C145(H145), 
 C150(H150), C151(H151), C152(H152), C153(H153), C154(H154), C156(H156), 
 C157(H157), C161(H161), C162(H162), C164(H164), C165(H165), C168(H168), 
 C169(H169), C171(H171), C172(H172) 
5.d Idealised Me refined as rotating group: 
 C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,H54B, 
 H54C), C51'(H51D,H51E,H51F), C52'(H52D,H52E,H52F), C53'(H53D,H53E,H53F), 
 C54'(H54D,H54E,H54F), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,H62B, 
 H62C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C114(H11A,H11B,H11C), 
 C115(H11D,H11E,H11F), C116(H11G,H11H,H11I), C117(H11J,H11K,H11L), C118(H11M, 
 H11N,H11O), C124(H12A,H12B,H12C), C125(H12D,H12E,H12F), C126(H12G,H12H,H12I), 
 C127(H12J,H12K,H12L), C128(H12M,H12N,H12O), C178(H17A,H17B,H17C), C179(H17D, 
 H17E,H17F), C180(H18A,H18B,H18C), C181(H18D,H18E,H18F), C182(H18G,H18H,H18I), 
 C188(H18J,H18K,H18L), C189(H18M,H18N,H18O), C190(H19A,H19B,H19C), C191(H19D, 
 H19E,H19F), C192(H19G,H19H,H19I), C206(H20A,H20B,H20C), C208(H20D,H20E,H20F), 
 C210(H21A,H21B,H21C), C212(H21D,H21E,H21F), C214(H21G,H21H,H21I) 
;
_shelx_res_checksum              433
_shelx_fab_checksum              18522
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'