Selective Formation of S4- and T-Symmetric Supramolecular Tetrahedral Cages and Helicates in Polar Media Assembled via Cooperative Action of Coordination and Hydrogen-Bonds.
Shi, Qixun; Zhou, Xiaohong; Yuan, Wei; Su, Xiaoshi; Neniškis, Algirdas; Wei, Xin; Taujenis, Lukas; Snarskis, Gustautas; Ward, Jas S.; Rissanen, Kari; de Mendoza, Javier; Orentas, Edvinas; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c00722

data_4134131
_publ_section_title
;
 Selective Formation of S4- and T-Symmetric Supramolecular Tetrahedral
 Cages and Helicates in Polar Media Assembled via Cooperative Action of
 Coordination and Hydrogen-Bonds.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c00722
_journal_year                    2020
_chemical_formula_moiety         'C51 H48 Hg N18 O6, 0.5(C H Cl3)'
_chemical_formula_sum            'C51.5 H48.5 Cl1.5 Hg N18 O6'
_chemical_formula_weight         1269.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.255(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.9046(8)
_cell_length_b                   27.1387(10)
_cell_length_c                   20.2736(9)
_cell_measurement_reflns_used    9997
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      66.52
_cell_measurement_theta_min      2.722
_cell_volume                     15341.2(10)
_computing_cell_refinement
'SAINT V8.38A (SAINT v8.38a, Bruker AXS Inc.: Madison, WI, USA, 2017.)'
_computing_data_reduction
'SAINT V8.38A (SAINT v8.38a, Bruker AXS Inc.: Madison, WI, USA, 2017.)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.870
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1018
_diffrn_reflns_av_unetI/netI     0.0816
_diffrn_reflns_Laue_measured_fraction_full 0.870
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            79232
_diffrn_reflns_point_group_measured_fraction_full 0.870
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         63.685
_diffrn_reflns_theta_min         2.272
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.472
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.4273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1395 before and 0.0851 after correction. The Ratio of minimum to maximum transmission is 0.5674. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.099
_exptl_crystal_description       block
_exptl_crystal_F_000             5096
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.259
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1339
_refine_ls_number_reflns         24185
_refine_ls_number_restraints     841
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.1959
_refine_ls_R_factor_gt           0.1335
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3611
_refine_ls_wR_factor_ref         0.4101
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10049
_reflns_number_total             24185
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00722_si_002.cif
_cod_data_source_block           Hg2(1b)6
_cod_depositor_comments
;

2020-07-21
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C103 H97 Cl3 Hg2 N36 O12'
_cod_original_formula_weight         2538.69
_cod_original_formula_moiety         '2(C51 H48 Hg N18 O6), C H Cl3'
_cod_original_formula_units_Z            4
_cod_database_code               4134131
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.663
_shelx_estimated_absorpt_t_min   0.573
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O186-C185
 1.25 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C175) \\sim Ueq, Uanis(C174) \\sim Ueq, Uanis(C173) \\sim Ueq, Uanis(C75)
\\sim Ueq, Uanis(C74) \\sim Ueq: with sigma of 0.025 and sigma for terminal
atoms of 0.05
4. Rigid body (RIGU) restrains
5.a Ternary CH refined with riding coordinates:
 C211(H211)
5.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C53(H53A,H53B), C83(H83A,H83B), C123(H12A,H12B), C153(H15A,
 H15B), C183(H18A,H18B)
5.c Aromatic/amide H refined with riding coordinates:
 N24(H24), N27(H27), N33(H33), N54(H54), N57(H57), N63(H63), N84(H84),
 N87(H87), N93(H93), N124(H124), N127(H127), N133(H133), N154(H154), N157(H157),
  N163(H163), N184(H184), N187(H187), N193(H193), C13(H13), C14(H14), C15(H15),
 C12(H12), C19(H19), C21(H21), C22(H22), C31(H31), C44(H44), C43(H43), C42(H42),
  C45(H45), C49(H49), C51(H51), C52(H52), C61(H61), C72(H72), C75(H75),
 C74(H74), C73(H73), C79(H79), C81(H81), C82(H82), C91(H91), C113(H113),
 C112(H112), C115(H115), C114(H114), C119(H119), C121(H121), C122(H122),
 C131(H131), C144(H144), C145(H145), C142(H142), C143(H143), C149(H149),
 C151(H151), C152(H152), C161(H161), C175(H175), C172(H172), C173(H173),
 C174(H174), C179(H179), C181(H181), C182(H182), C191(H191)
5.d Fitted hexagon refined as free rotating group:
 C13(C14,C15,C16,N11,C12), C44(C43,C42,N41,C46,C45), C72(N71,C76,C75,C74,C73),
 C113(C112,N111,C116,C115,C114), C144(C145,C146,N141,C142,C143), C175(C176,N171,
 C172,C173,C174)
5.e Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C65(H65A,H65B,H65C), C95(H95A,H95B,H95C), C135(H13A,H13B,
 H13C), C165(H16A,H16B,H16C), C195(H19A,H19B,H19C)
;
_shelx_res_checksum              78382
_shelx_hkl_checksum              49822
_shelx_fab_checksum              26666
_olex2_submission_special_instructions 'No special instructions were received'