Enhanced stability and reusability of recombinant silicatein upon biomimetic metal-organic framework crystallization.
Zhang, Tongtong; Wang, Xiangyu; Wright, Jack D.; Whitehead, George F. S.; Tidey, Jeremiah P.; Wong, Lu Shin; Riddell, Imogen A.; Chemical science 17 (2026) 3141–3147; doi:10.1039/d5sc05521k

data_1576434
_publ_section_title
;
 Enhanced stability and reusability of recombinant silicatein upon
 biomimetic metal-organic framework crystallization.
;
_journal_issue                   6
_journal_name_full               'Chemical science'
_journal_page_first              3141
_journal_page_last               3147
_journal_paper_doi               10.1039/d5sc05521k
_journal_volume                  17
_journal_year                    2026
_chemical_formula_moiety         'C8 H9 N O6 Zn'
_chemical_formula_sum            'C8 H9 N O6 Zn'
_chemical_formula_weight         280.551
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-01-28
_audit_creation_method
;
Olex2 1.5-ac7-013
(compiled 2025.01.02 svn.rf662f148 for Rigaku Oxford Diffraction, GUI svn.r7109)
;
_audit_update_record
;
2025-01-28 deposited with the CCDC.	2025-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.172(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5078(15)
_cell_length_b                   6.4427(6)
_cell_length_c                   14.9087(12)
_cell_measurement_reflns_used    6102
_cell_measurement_temperature    100(5)
_cell_measurement_theta_max      1.1220
_cell_measurement_theta_min      0.0940
_cell_volume                     909.53(18)
_computing_cell_refinement       'CrysAlisPro 1.171.44.91a (Rigaku OD, 2025)'
_computing_data_collection
'CrysAlisPro system (CCD 44.78a 64-bit (release 25-10-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.44.91a (Rigaku OD, 2025)'
_computing_molecular_graphics    'Olex2 1.5-ac7-013 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac7-013 (Dolomanov et al., 2009)'
_computing_structure_refinement
'olex2.refine 1.5-ac7-013 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      vacuum
_diffrn_ambient_temperature      100(5)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix-ED
_diffrn_measured_fraction_theta_full 0.8965
_diffrn_measured_fraction_theta_max 0.9003
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -70.00  40.00   0.20    0.40    --    0.00   0.00   0.00  550
  2  \w    -62.20  62.00   0.20    0.40    --    0.00   0.00   0.00  621
  3  \w    -65.00  23.00   0.20    0.40    --    0.00   0.00   0.00  440
;
_diffrn_measurement_device       'electron diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy-ED, HyPix-ED, electron source at 200keV'
_diffrn_measurement_method       'continuous rotation electron diffraction'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0026461865
_diffrn_orient_matrix_UB_12      -0.0000042522
_diffrn_orient_matrix_UB_13      0.0001482843
_diffrn_orient_matrix_UB_21      0.0000007881
_diffrn_orient_matrix_UB_22      0.0038991953
_diffrn_orient_matrix_UB_23      0.0000053076
_diffrn_orient_matrix_UB_31      0.0000026063
_diffrn_orient_matrix_UB_32      0.0000004652
_diffrn_orient_matrix_UB_33      0.0016851809
_diffrn_radiation_monochromator  none
_diffrn_radiation_probe          electron
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.02510
_diffrn_reflns_av_R_equivalents  0.2020
_diffrn_reflns_av_unetI/netI     0.1192
_diffrn_reflns_Laue_measured_fraction_full 0.8965
_diffrn_reflns_Laue_measured_fraction_max 0.9003
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12093
_diffrn_reflns_point_group_measured_fraction_full 0.8965
_diffrn_reflns_point_group_measured_fraction_max 0.9003
_diffrn_reflns_theta_full        0.8629
_diffrn_reflns_theta_max         0.90
_diffrn_reflns_theta_min         0.12
_diffrn_source                   'electron diffractometer'
_diffrn_source_type              'JEOL JSM-2300ED, LaB6'
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.91a (Rigaku Oxford Diffraction, 2025)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.049
_exptl_crystal_description       'microcrystalline slab'
_exptl_crystal_F_000             179.960
_refine_diff_density_max         0.8141
_refine_diff_density_min         -0.7746
_refine_diff_density_rms         0.2074
_refine_ls_d_res_high            0.8002
_refine_ls_d_res_low             6.1163
_refine_ls_extinction_coef       21919(1371)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0358
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    12
_refine_ls_number_parameters     167
_refine_ls_number_reflns         1670
_refine_ls_number_restraints     146
_refine_ls_restrained_S_all      0.9889
_refine_ls_R_factor_all          0.1598
_refine_ls_R_factor_gt           0.1437
_refine_ls_shift/su_max          -0.0009
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+1.2132P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2873
_refine_ls_wR_factor_ref         0.2966
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -11
_reflns_limit_k_max              8
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                1490
_reflns_number_total             1670
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5sc05521k2.cif
_cod_data_source_block           m_1383_1384_1385_d08
_cod_database_code               1576434
_chemical_oxdiff_formula         C8H9NO6Zn
_chemical_oxdiff_usercomment
;
 2024NCS0814, S010010, TF-Sila-25 sonicated in Et2O and drop cast (~2x60uL)
 onto holey carbon, flash froze and loaded ~115K, CSD: SIWVEA'
;
_diffrn_oxdiff_scatteringfactors_ed
'UCLA (2022) https://srv.mbi.ucla.edu/faes/data'
_diffrn_oxdiff_digest_creation
;
CAP 1.171.44.91a, AC 1.5-ac7-013
;
_diffrn_oxdiff_digest_hkl
;
43c527a49abfc475b2ae465eb58dde56b9503c
;
_diffrn_oxdiff_digest_hkl_ed
;
53f35de1bf32add995483ce4d3926b4de5957f
;
_diffrn_oxdiff_digest_od_ed
;

;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O15-H15a \\sim O15-H15b \\sim O16-H16b \\sim O16-H16a
 with sigma of 0.02
 H15a-H15b \\sim H16b-H16a
 with sigma of 0.02
 N7-H7b \\sim N7-H7a
 with sigma of 0.02
 C14-H14 \\sim C13-H13 \\sim C8-H8
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O16) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.003
5.a Aromatic/amide H refined with riding coordinates and stretchable bonds:
 C8(H8), C13(H13), C14(H14)
;
_atom_sites_solution_hydrogen    mixed
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   9959
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.786
_oxdiff_exptl_absorpt_empirical_full_min 0.583