Programmable synthesis of well-defined, glycosylated iron(ii) supramolecular assemblies with multivalent protein-binding capabilities.
Schwab, Jake H.; Bailey, Jake B.; Gembicky, Milan; Stauber, Julia M.; Chemical science 14 (2023) 1018–1026; doi:10.1039/d2sc05689e

data_1568165
_publ_section_title
;
 Programmable synthesis of well-defined, glycosylated iron(ii)
 supramolecular assemblies with multivalent protein-binding capabilities.
;
_journal_issue                   4
_journal_name_full               'Chemical science'
_journal_page_first              1018
_journal_page_last               1026
_journal_paper_doi               10.1039/d2sc05689e
_journal_volume                  14
_journal_year                    2023
_chemical_absolute_configuration syn
_chemical_formula_moiety
'C120 H132 Fe2 N12 O63 S6, C72 H42 Fe2 N12 O27 S6, 6[C8O6H15], 4[C4H12N1], 60[H2O], 1[]'
_chemical_formula_sum            'C256 H432 Fe4 N28 O186 S12'
_chemical_formula_weight         7486.39
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-13
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-12-14 deposited with the CCDC.	2022-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   22.1273(9)
_cell_length_b                   22.1273(9)
_cell_length_c                   62.674(4)
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      26.31
_cell_measurement_theta_min      2.22
_cell_volume                     26575(2)
_computing_cell_refinement       'SAINT v8.40B (Bruker, 2019)'
_computing_data_collection       'APEX4 v2022.1-1 (Bruker, 2022)'
_computing_data_reduction        'SAINT v8.40B (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II Ultra'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       76
_diffrn_reflns_limit_l_min       -75
_diffrn_reflns_number            70965
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         1.679
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_type              'Bruker TXS'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.340
_exptl_absorpt_correction_T_max  0.4879
_exptl_absorpt_correction_T_min  0.4461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0780 before and 0.0649 after correction.
The Ratio of minimum to maximum transmission is 0.9143.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       block
_exptl_crystal_F_000             11844
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.313
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details
;
 Flack x determined using 5661 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.547(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     913
_refine_ls_number_reflns         22399
_refine_ls_number_restraints     1053
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1235
_refine_ls_R_factor_gt           0.0858
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1710P)^2^+61.4751P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2421
_refine_ls_wR_factor_ref         0.2881
_reflns_Friedel_coverage         0.995
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                14391
_reflns_number_total             22399
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc05689e2.cif
_cod_data_source_block           stauber_for_publication_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 1568165.cif.
;
_cod_original_cell_volume        26575(3)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               1568165
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.935
_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 O(H) groups
2. Restrained distances
 O5-C13
 1.423 with sigma of 0.01
 C13-C14
 1.496 with sigma of 0.01
 O15-C33
 1.423 with sigma of 0.01
 C33-C34
 1.496 with sigma of 0.01
 C34-O16
 1.423 with sigma of 0.01
 C14-O6
 1.423 with sigma of 0.01
 C20-O10
 1.424 with sigma of 0.001
 O20-C40
 1.424 with sigma of 0.001
 O5-C14
 2.389 with sigma of 0.01
 C34-O15
 2.389 with sigma of 0.01
 C13-O6
 2.389 with sigma of 0.01
 C33-O16
 2.389 with sigma of 0.01
 C34-C35
 2.377 with sigma of 0.01
 C14-C15
 2.377 with sigma of 0.01
 C19-O10
 2.426 with sigma of 0.001
 O20-C39
 2.246 with sigma of 0.001
3. Restrained planarity
 C1A, C2A, C3A, C4A, C5A, C6A
 with sigma of 0.02
 C21A, C22A, C23A, C24A, C25A, C26A
 with sigma of 0.02
 C21, C22, C23, C24, C25, C26
 with sigma of 0.02
 C1, C2, C3, C4, C5, C6
 with sigma of 0.02
 O15A, N4A, C28A, C29A, C30A, C31A, C32A
 with sigma of 0.02
 O5A, N2A, C8A, C9A, C10A, C11A, C12A
 with sigma of 0.02
 O15, N4, C28, C29, C30, C31, C32
 with sigma of 0.02
 O5, N2, C8, C9, C10, C11, C12
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O16) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(O17)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq,
Uanis(C40) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(O18)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O10) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(O11)
\\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq,
Uanis(C18) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O7) \\sim
Ueq, Uanis(O6) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of
0.04
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
6.a Free rotating group:
 O6(O7,H7A,O8,H8,O9,H9A,O11,C15,H15,C16,H16,C17,H17,C18,H18,C19,H19,C20,H20A,
 H20B), O16(O17,H17A,O18,H18A,O19,H19A,O21,C35,H35,C36,H36,C37,H37,C38,H38,C39,
 H39,C40,H40A,H40B)
6.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C33(H33A,H33B), C34(H34A,H34B)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C7(H7), C9(H9), C10(H10A), C12(H12), C22(H22),
 C23(H23), C25(H25), C27(H27), C29(H29), C30(H30), C32(H32), C2A(H2A), C3A(H3A),
  C5A(H5A), C7A(H7AA), C9A(H9AA), C10A(H10B), C12A(H12A), C22A(H22A),
 C23A(H23A), C25A(H25A), C27A(H27A), C29A(H29A), C30A(H30A), C32A(H32A)
6.d Tetrahedral OH refined with riding coordinates:
 O10(H10), O20(H20)
;
_shelx_res_checksum              97837
_shelx_fab_checksum              24543
_platon_squeeze_special_details
;
A solvent mask was calculated and 4346 electrons were 
found in a volume of 13497\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
18[C8O6H15], 12[C4H12N1], 180[H2O] per Unit Cell 
which account for 4314 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'