Metal-driven folding and assembly of a minimal β-sheet into a 3D-porous honeycomb framework.
Bajpayee, Nikhil; Pophali, Salil; Vijayakanth, Thangavel; Nandi, Shyamapada; Desai, Aamod V.; Kumar, Vinod; Jain, Rahul; Bera, Santu; Shimon, Linda J. W.; Misra, Rajkumar; Chemical communications (Cambridge, England) 60 (2024) 2621–2624; doi:10.1039/d3cc05185d

data_7132786
_publ_section_title
;
 Metal-driven folding and assembly of a minimal &#x3b2;-sheet into a
 3D-porous honeycomb framework.
;
_journal_issue                   19
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2621
_journal_page_last               2624
_journal_paper_doi               10.1039/d3cc05185d
_journal_volume                  60
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C210 H228 Ag3 N36 O24, B F4, 24[C2H6O], 24[H2O]'
_chemical_formula_sum            'C210 H228 Ag3 B F4 N36 O24'
_chemical_formula_weight         4050.69
_space_group_crystal_system      trigonal
_space_group_IT_number           155
_space_group_name_Hall           'R 3 2"'
_space_group_name_H-M_alt        'R 3 2 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-01-05 deposited with the CCDC.	2024-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   38.1751(4)
_cell_length_b                   38.1751(4)
_cell_length_c                   37.5163(6)
_cell_measurement_reflns_used    69011
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      67.2440
_cell_measurement_theta_min      3.4660
_cell_volume                     47349.0(10)
_computing_cell_refinement       'CrysAlisPro 1.171.42.74a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.74a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.74a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01(10)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            142560
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        58.933
_diffrn_reflns_theta_max         58.933
_diffrn_reflns_theta_min         3.534
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    1.890
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.74a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.852
_exptl_crystal_description       'irregular, piece of prism'
_exptl_crystal_F_000             12684
_exptl_crystal_size_max          0.191
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
;
 Flack x determined using 5853 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.079(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     767
_refine_ls_number_reflns         15118
_refine_ls_number_restraints     714
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1196P)^2^+23.6844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1744
_refine_ls_wR_factor_ref         0.1778
_reflns_Friedel_coverage         0.899
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                13757
_reflns_number_total             15118
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05185d2.cif
_cod_data_source_block           raj1b.redo2
_cod_original_cell_volume        47349.0(12)
_cod_original_sg_symbol_H-M      'R 3 2'
_cod_database_code               7132786
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.848
_shelx_estimated_absorpt_t_min   0.714
_oxdiff_exptl_absorpt_empirical_full_min 0.812
_oxdiff_exptl_absorpt_empirical_full_max 1.255
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_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. Uiso/Uaniso restraints and constraints
Uanis(C53) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C54) \\sim Ueq: with sigma of
0.003 and sigma for terminal atoms of 0.006
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Ternary CH refined with riding coordinates:
 C7(H7), C16(H16), C18(H18), C22(H22), C42(H42), C50(H50), C52(H52), C56(H56)
4.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C17(H17A,H17B), C23(H23A,H23B), C43(H43A,H43B), C51(H51A,H51B),
 C57(H57A,H57B)
4.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), N4(H4), N5(H5), N8(H8), N9(H9), N10(H10), N11(H11), C67(H67),
 C66(H66), C69(H69), C68(H68), C5(H5A), C1(H1), C2(H2A), C3(H3A), C14(H14),
 C13(H13), C12(H12), C11(H11A), C10(H10A), C25(H25), C26(H26), C27(H27),
 C28(H28), C29(H29), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38),
  C39(H39), C40(H40), C70(H70), C48(H48), C47(H47), C46(H46), C45(H45),
 C63(H63), C62(H62), C61(H61), C60(H60), C59(H59)
4.d Fitted hexagon refined as free rotating group:
 N12(C67,C66,C65,C69,C68), C4(C5,N1,C1,C2,C3), C9(C14,C13,C12,C11,C10),
 C24(C25,C26,C27,C28,C29), C44(C70,C48,C47,C46,C45), C58(C63,C62,C61,C60,C59)
4.e Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C53(H53A,H53B,H53C), C54(H54A,H54B,
 H54C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated using Olex2 version of Squeeze
and 5460 electrons were 
found in a volume of 22028\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
24[C2H6O], 24[H2O] per Asymmetric Unit 
which account for 5184 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              76776
_shelx_hkl_checksum              68953
_shelx_fab_checksum              74934
_olex2_submission_special_instructions 'No special instructions were received'