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_1566096
_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 H38 B N7 O4 S Zn'
_chemical_formula_sum            'C39 H38 B N7 O4 S Zn'
_chemical_formula_weight         777.00
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc292q59
_audit_creation_date             2021-08-29
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9864(16)
_cell_length_b                   16.941(2)
_cell_length_c                   18.040(2)
_cell_measurement_reflns_used    3235
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      23.515
_cell_measurement_theta_min      2.368
_cell_volume                     3663.2(8)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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  'XL  (Sheldrick, 2008)'
_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 0.993
_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  0.0703
_diffrn_reflns_av_unetI/netI     0.0973
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20238
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.128
_diffrn_reflns_theta_min         1.649
_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    0.779
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6152
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1296 before and 0.0684 after correction.
The Ratio of minimum to maximum transmission is 0.8254.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       plate
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Flack x determined using 1964 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.000(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.760
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         6978
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.760
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1278
_reflns_Friedel_coverage         0.860
_reflns_Friedel_fraction_full    0.941
_reflns_Friedel_fraction_max     0.913
_reflns_number_gt                5384
_reflns_number_total             6978
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc06011b4.cif
_cod_data_source_block           tpzn2_2
_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        3663.3(8)
_cod_database_code               1566096
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.926
_shelx_estimated_absorpt_t_min   0.860
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H00Q(0.022) H00W(0.026) H015(0.029) H019(0.028) H01L(0.046)
 H01M(0.046) H01N(0.046) H01A(0.036) H01B(0.036) H01C(0.036) H011(0.025)
 H016(0.033) H012(0.033) H00R(0.03) H00T(0.029) H00N(0.024) H01H(0.042)
 H01I(0.042) H01J(0.042) H00X(0.024) H00U(0.027) H00Z(0.03) H01G(0.031)
 H010(0.027) H00L(0.026) H00A(0.035) H00B(0.035) H00C(0.035) H018(0.03)
 H01O(0.039) H01P(0.043) H01K(0.038) H00Y(0.028) H013(0.024) H01D(0.037)
 H01E(0.037) H01F(0.037) H1(0.021)
 Fixed X: H00Q(0.471996) H00W(0.560276) H015(0.59537) H019(0.555694)
 H01L(0.290097) H01M(0.229555) H01N(0.328378) H01A(0.609719) H01B(0.691141)
 H01C(0.722721) H011(0.350567) H016(0.455479) H012(0.583922) H00R(0.608547)
 H00T(0.502927) H00N(0.303052) H01H(0.062773) H01I(0.139801) H01J(0.160988)
 H00X(0.24548) H00U(0.313277) H00Z(0.270976) H01G(0.149069) H010(0.073743)
 H00L(-0.069481) H00A(-0.087381) H00B(-0.169921) H00C(-0.106671) H018(0.53713)
 H01O(0.6787) H01P(0.650589) H01K(0.483529) H00Y(0.342258) H013(0.268446)
 H01D(0.114207) H01E(0.102526) H01F(0.028925) H1(0.087028)
 Fixed Y: H00Q(0.284236) H00W(0.350673) H015(0.486042) H019(0.55005)
 H01L(0.160058) H01M(0.240976) H01N(0.20736) H01A(0.641135) H01B(0.579915)
 H01C(0.613774) H011(0.647329) H016(0.700136) H012(0.801461) H00R(0.846134)
 H00T(0.792876) H00N(0.790336) H01H(0.694738) H01I(0.768695) H01J(0.685051)
 H00X(0.543192) H00U(0.514898) H00Z(0.394276) H01G(0.305894) H010(0.337305)
 H00L(0.449214) H00A(0.490597) H00B(0.494376) H00C(0.572386) H018(0.40948)
 H01O(0.322603) H01P(0.185609) H01K(0.138139) H00Y(0.224351) H013(0.338122)
 H01D(0.517981) H01E(0.428962) H01F(0.458937) H1(0.561568)
 Fixed Z: H00Q(0.305273) H00W(0.209498) H015(0.22208) H019(0.332007)
 H01L(0.43685) H01M(0.458692) H01N(0.509303) H01A(0.450029) H01B(0.409563)
 H01C(0.489677) H011(0.398283) H016(0.302712) H012(0.326611) H00R(0.447296)
 H00T(0.543597) H00N(0.599524) H01H(0.679415) H01I(0.700067) H01J(0.738813)
 H00X(0.35146) H00U(0.233947) H00Z(0.178098) H01G(0.236758) H010(0.351945)
 H00L(0.431554) H00A(0.628434) H00B(0.558798) H00C(0.585939) H018(0.616983)
 H01O(0.581846) H01P(0.590395) H01K(0.638378) H00Y(0.674934) H013(0.767659)
 H01D(0.791004) H01E(0.819654) H01F(0.751202) H1(0.654536)
;
_shelx_res_checksum              31741
_shelx_hkl_checksum              17807
_olex2_submission_special_instructions 'No special instructions were received'