Disulphide bond exchange inhibited by air - kinetic and thermodynamic products in a library of macrocyclic cysteine derivatives.
Cholewiak, Agnieszka; Dobrzycki, Łukasz; Jurczak, Janusz; Ulatowski, Filip; Organic & biomolecular chemistry 16 (2018) 2411–2420; doi:10.1039/c7ob03123h

data_7156095
_publ_section_title
;
 Disulphide bond exchange inhibited by air - kinetic and thermodynamic
 products in a library of macrocyclic cysteine derivatives.
;
_journal_issue                   14
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2411
_journal_page_last               2420
_journal_paper_doi               10.1039/c7ob03123h
_journal_volume                  16
_journal_year                    2018
_chemical_absolute_configuration rmad
_chemical_formula_sum            'C124.4 H156.62 N20 O25.4 S16.2'
_chemical_formula_weight         2857.88
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2017-05-23 deposited with the CCDC.
2018-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.763(2)
_cell_length_b                   21.594(2)
_cell_length_c                   33.712(4)
_cell_measurement_reflns_used    9331
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      20.0328
_cell_measurement_theta_min      2.2328
_cell_volume                     14387(3)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX2 V2014 (Bruker AXS Inc., 2014)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_publication_material  'APEX2 V2014 (Bruker AXS Inc., 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  TRIUMPH
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1044
_diffrn_reflns_av_unetI/netI     0.1159
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            210438
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.15
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.316
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6022
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DMSO; water'
_exptl_crystal_size_max          0.366
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.427
_refine_ls_abs_structure_details
;
Flack x determined using 5391 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2035
_refine_ls_number_reflns         30740
_refine_ls_number_restraints     508
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.1545
_refine_ls_R_factor_gt           0.0964
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1039P)^2^+21.4939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2197
_refine_ls_wR_factor_ref         0.2599
_reflns_number_gt                20093
_reflns_number_total             30740
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ob03123h2.cif
_cod_data_source_block           FU_805_A2_twin
_cod_depositor_comments
'Adding full bibliography for 7156094--7156095.cif.'
_cod_original_cell_volume        14387.(3)
_cod_original_formula_sum        'C124.40 H156.62 N20 O25.40 S16.20'
_cod_database_code               7156095
_shelx_res_checksum              40788