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_1566100
_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         'C38 H36 B N7 O4 S Zn'
_chemical_formula_sum            'C38 H36 B N7 O4 S Zn'
_chemical_formula_weight         762.98
_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
_audit_block_doi                 10.5517/ccdc.csd.cc292qbg
_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                87.678(3)
_cell_angle_beta                 87.319(3)
_cell_angle_gamma                84.581(3)
_cell_formula_units_Z            4
_cell_length_a                   9.780(2)
_cell_length_b                   17.966(4)
_cell_length_c                   23.194(5)
_cell_measurement_reflns_used    9924
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      24.905
_cell_measurement_theta_min      2.236
_cell_volume                     4050.0(15)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_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 0.986
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0905
_diffrn_reflns_av_unetI/netI     0.0776
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            82013
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.455
_diffrn_reflns_theta_min         1.414
_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    0.704
_exptl_absorpt_correction_T_max  0.4908
_exptl_absorpt_correction_T_min  0.3967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0794 before and 0.0604 after correction.
The Ratio of minimum to maximum transmission is 0.8083.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_description       block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.285
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     945
_refine_ls_number_reflns         16482
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.1103
_refine_ls_R_factor_gt           0.0760
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+21.4417P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1697
_refine_ls_wR_factor_ref         0.1829
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11908
_reflns_number_total             16482
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc06011b4.cif
_cod_data_source_block           cohen_022421_mkj4_0m_a_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 
;
_cod_original_cell_volume        4050.0(16)
_cod_database_code               1566100
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.933
_shelx_estimated_absorpt_t_min   0.933
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 B02V(H9), B02W(H02W)
2.b Aromatic/amide H refined with riding coordinates:
 N00J(H), N00P(H00P), C00T(HA), C00Y(HB), C00Z(HC), C010(H010), C019(HD),
 C01B(H01B), C01D(H01D), C01E(HE), C01F(HF), C01H(HG), C01I(HH), C01J(H01J),
 C01L(H01L), C01M(H01M), C01N(HI), C01P(H01P), C01Q(HJ), C01S(HK), C01T(H01T),
 C01U(HL), C01V(HM), C01W(HN), C01X(H01X), C01Y(HO), C020(HP), C021(H021),
 C022(HQ), C024(H024), C025(H025), C026(H026), C027(HR), C028(HS), C02C(H02C),
 C02D(H02D), C02E(HW), C02F(H02F), C02G(H02G), C02H(H02H), C02I(HX), C02L(H02L),
  C02M(H2), C02P(H02P), C02S(H02S), C02T(H02T)
2.c Idealised Me refined as rotating group:
 C02A(HT,HU,HV), C02J(HY,HZ,H1), C02K(H02A,H02B,H02E), C02N(H02I,H02J,H02K),
 C02O(H02M,H02N,H02O), C02Q(H3,H4,H5), C02R(H6,H7,H8), C02U(H02Q,H02R,H02U)
;
_shelx_res_checksum              89514
_shelx_hkl_checksum              32858
_shelx_fab_checksum              38697
_olex2_submission_special_instructions 'No special instructions were received'