Selective Construction of Very Large Stacking-Interaction-Induced Molecular 818 Metalla-knots and Borromean Ring Using Curved Dipyridyl Ligands
Zhang, Hai-Ning; Lin, Yue-Jian; Jin, Guo-Xin; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c11925

data_4135465
_publ_section_title
;
 Selective Construction of Very Large Stacking-Interaction-Induced
 Molecular 818 Metalla-knots and Borromean Ring Using Curved Dipyridyl
 Ligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c11925
_journal_year                    2020
_chemical_formula_moiety
'C114 H104 N4 O8 Rh4, 3(C F3 O3 S), 0.67(H2 O)'
_chemical_formula_sum            'C128.67 H160 F12 N4 O37.33 Rh4 S4'
_chemical_formula_weight         3127.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-10-13
_audit_creation_method
; 
Olex2 1.2-beta 
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103) 
;
_cell_angle_alpha                90
_cell_angle_beta                 102.209(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   36.467(4)
_cell_length_b                   29.225(4)
_cell_length_c                   42.676(5)
_cell_measurement_reflns_used    9723
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      69.23
_cell_measurement_theta_min      2.35
_cell_volume                     44453(9)
_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      140.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0934
_diffrn_reflns_av_unetI/netI     0.1136
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            113314
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.500
_diffrn_reflns_theta_min         1.955
_exptl_absorpt_coefficient_mu    4.826
_exptl_absorpt_correction_T_max  0.5857
_exptl_absorpt_correction_T_min  0.4679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1423 before and 0.0919 after correction. 
The Ratio of minimum to maximum transmission is 0.7989. 
The \l/2 correction factor is Not present. 
;
_exptl_crystal_colour            bronze
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       block
_exptl_crystal_F_000             19328
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.519
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2210
_refine_ls_number_reflns         41551
_refine_ls_number_restraints     271
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.1497
_refine_ls_R_factor_gt           0.1015
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2990
_refine_ls_wR_factor_ref         0.3446
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24267
_reflns_number_total             41551
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c11925_si_003.cif
_cod_data_source_block           3
_cod_original_cell_volume        44452(9)
_cod_database_code               4135465
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups, All C(H,H) groups 
 At 1.5 times of: 
  All C(H,H,H) groups, All O(H,H) groups 
2. Restrained distances 
 C38-C39 = C105-C106 = C152-C153 
 1.4 with sigma of 0.02 
 C156-C161 
 1.5 with sigma of 0.02 
 S4-C175 = S5-C176 
 1.8 with sigma of 0.02 
 S4-O24 = S5-O25 = S5-O26 = S5-O27 
 1.43 with sigma of 0.02 
 C175-F12 = C176-F13 = C176-F14 = C176-F15 
 1.32 with sigma of 0.02 
 C174-F7 = C174-F8 = C174-F9 = C175-F10 = C175-F11 
 1.32 with sigma of 0.02 
 F13-F14 = F13-F15 = F14-F15 
 2.1 with sigma of 0.03 
 S5-F15 
 2.6 with sigma of 0.03 
 O11-H31A = O17-H31B 
 2 with sigma of 0.05 
 C152-C153 \\sim C154-C155 \\sim C155-C156 \\sim C156-C152 
 with sigma of 0.02 
3. Uiso/Uaniso restraints and constraints 
Uanis(S4) \\sim Ueq, Uanis(S5) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O25) 
\\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(O27) \\sim Ueq, Uanis(F13) \\sim Ueq, 
Uanis(F14) \\sim Ueq, Uanis(C174) \\sim Ueq, Uanis(C176) \\sim Ueq: with sigma 
of 0.02 and sigma for terminal atoms of 0.04 
Uanis(C252) \\sim Ueq, Uanis(C253) \\sim Ueq, Uanis(C254) \\sim Ueq, 
Uanis(C255) \\sim Ueq, Uanis(C256) \\sim Ueq, Uanis(C257) \\sim Ueq, 
Uanis(C258) \\sim Ueq, Uanis(C259) \\sim Ueq, Uanis(C260) \\sim Ueq, 
Uanis(C261) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04 
Uanis(C152) \\sim Ueq, Uanis(C153) \\sim Ueq, Uanis(C154) \\sim Ueq, 
Uanis(C155) \\sim Ueq, Uanis(C156) \\sim Ueq, Uanis(C157) \\sim Ueq, 
Uanis(C158) \\sim Ueq, Uanis(C159) \\sim Ueq, Uanis(C160) \\sim Ueq, 
Uanis(C161) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04 
Uanis(C53) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C109) \\sim Ueq, Uanis(C110) 
\\sim Ueq, Uanis(C111) \\sim Ueq, Uanis(C112) \\sim Ueq, Uanis(C113) \\sim Ueq, 
Uanis(C114) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04 
Uanis(C54) \\sim Ueq, Uanis(O23) \\sim Ueq: with sigma of 0.01 and sigma for 
terminal atoms of 0.02 
4. Others 
 Sof(C252)=Sof(C253)=Sof(C254)=Sof(C255)=Sof(C256)=Sof(C257)=Sof(H25A)= 
 Sof(H25B)=Sof(H25C)=Sof(C258)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C259)= 
 Sof(H25G)=Sof(H25H)=Sof(H25I)=Sof(C260)=Sof(H26A)=Sof(H26B)=Sof(H26C)= 
 Sof(C261)=Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(1) 
 Sof(C152)=Sof(C153)=Sof(C154)=Sof(C155)=Sof(C156)=Sof(C157)=Sof(H15A)= 
 Sof(H15B)=Sof(H15C)=Sof(C158)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C159)= 
 Sof(H15G)=Sof(H15H)=Sof(H15I)=Sof(C160)=Sof(H16A)=Sof(H16B)=Sof(H16C)= 
 Sof(C161)=Sof(H16D)=Sof(H16E)=Sof(H16F)=FVAR(1) 
 Fixed Sof: S5(0.5) O25(0.5) O26(0.5) O27(0.5) C176(0.5) F13(0.5) F14(0.5) 
5.a Free rotating group: 
 O31(H31A,H31B) 
5.b : 
 C252(C253,C254,C255,C256,C257) 
5.c Secondary CH2 refined with riding coordinates: 
 C23(H23A,H23B), C80(H80A,H80B), C137(H13A,H13B) 
5.d Me refined with riding coordinates: 
 C167(H16G,H16H,H16I) 
5.e Aromatic/amide H refined with riding coordinates: 
 C5(H5), C6(H6), C7(H7), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), 
 C18(H18), C19(H19), C21(H21), C25(H25), C27(H27), C28(H28), C31(H31), C32(H32), 
  C33(H33), C34(H34), C36(H36), C37(H37), C62(H62), C63(H63), C64(H64), 
 C69(H69), C70(H70), C71(H71), C72(H72), C73(H73), C75(H75), C76(H76), C78(H78), 
  C82(H82), C84(H84), C85(H85), C88(H88), C89(H89), C90(H90), C91(H91), 
 C93(H93), C94(H94), C119(H119), C120(H120), C121(H121), C126(H126), C127(H127), 
  C128(H128), C129(H129), C130(H130), C132(H132), C133(H133), C135(H135), 
 C139(H139), C141(H141), C142(H142), C145(H145), C146(H146), C147(H147), 
 C148(H148), C150(H150), C151(H151) 
5.f Idealised Me refined as rotating group: 
 C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B, 
 H46C), C47(H47A,H47B,H47C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C55(H55A, 
 H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C100(H10A,H10B,H10C), 
 C101(H10D,H10E,H10F), C102(H10G,H10H,H10I), C103(H10J,H10K,H10L), C104(H10M, 
 H10N,H10O), C110(H11A,H11B,H11C), C111(H11D,H11E,H11F), C112(H11G,H11H,H11I), 
 C113(H11J,H11K,H11L), C114(H11M,H11N,H11O), C157(H15A,H15B,H15C), C158(H15D, 
 H15E,H15F), C159(H15G,H15H,H15I), C160(H16A,H16B,H16C), C161(H16D,H16E,H16F), 
 C257(H25A,H25B,H25C), C258(H25D,H25E,H25F), C259(H25G,H25H,H25I), C260(H26A, 
 H26B,H26C), C261(H26D,H26E,H26F), C168(H16J,H16K,H16L), C169(H16M,H16N,H16O), 
 C170(H17A,H17B,H17C), C171(H17D,H17E,H17F) 
;
_shelx_res_checksum              57224
_shelx_hkl_checksum              20281
_shelx_fab_checksum              58602
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'