Salicylate Metal-Binding Isosteres as Fragments for Metalloenzyme Inhibition
Jackl, Moritz K.; Seo, Hyeonglim; Karges, Johannes; Kalaj, Mark; Cohen, Seth M.; Chemical Science  (2022) –; doi:10.1039/D1SC06011B

data_1566091
_publ_section_title
;
 Salicylate Metal-Binding Isosteres as Fragments for Metalloenzyme
 Inhibition
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC06011B
_journal_year                    2022
_chemical_formula_moiety         'C39 H34 B N7 O4 Zn'
_chemical_formula_sum            'C39 H34 B N7 O4 Zn'
_chemical_formula_weight         740.91
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc292q26
_audit_creation_date             2021-08-27
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-10-22 deposited with the CCDC.	2022-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                115.6050(10)
_cell_angle_beta                 90.7810(10)
_cell_angle_gamma                98.5870(10)
_cell_formula_units_Z            2
_cell_length_a                   11.8862(8)
_cell_length_b                   12.1596(8)
_cell_length_c                   13.5975(9)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.43
_cell_measurement_theta_min      2.34
_cell_volume                     1745.7(2)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution
'olex2.solve 1.3-alpha (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22366
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         26.438
_diffrn_reflns_theta_min         1.667
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5802
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1070 before and 0.0507 after correction.
The Ratio of minimum to maximum transmission is 0.7784.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       block
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         7180
_refine_ls_number_restraints     491
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0265P)^2^+0.9458P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0735
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6820
_reflns_number_total             7180
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc06011b4.cif
_cod_data_source_block           mkj1_a
_cod_database_code               1566091
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C00O, O00B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C00O \\sim O00B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
Uanis(C00O) \\sim Ueq, Uanis(O00B) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Ternary CH refined with riding coordinates:
 B019(H019)
5.b Aromatic/amide H refined with riding coordinates:
 C00D(H00D), C00I(H00I), C00L(H00L), C00M(H00M), C00P(H00P), C00Q(H00Q),
 C00S(H00S), C00T(H00T), C00U(H00U), C00W(H00W), C00X(H00X), C00Z(H00Z),
 C011(H011), C012(H012), C015(H015), C016(H016), C017(H017), C018(H018),
 C01D(H01J), C01F(H01N), C01G(H01O)
5.c Idealised Me refined as rotating group:
 C010(H01A,H01B,H01C), C013(H01D,H01E,H01F), C01B(H01G,H01H,H01I), C01E(H01K,
 H01L,H01M)
;
_shelx_res_checksum              94086
_shelx_hkl_checksum              49241
_olex2_submission_special_instructions 'No special instructions were received'