Highly efficient H2S scavengers via thiolysis of positively-charged NBD amines
Ismail, Ismail; Chen, Zhuoyue; Sun, Lu; Ji, Xiuru; Ye, Haishun; Kang, Xueying; Huang, Haojie; Song, Haibin; Bolton, Sarah G.; Xi, Zhen; Pluth, Michael D.; Yi, Long; Chemical Science 11 (2020) 7823–7828; doi:10.1039/D0SC01518K

data_1558556
_publ_section_title
;
 Highly efficient H2S scavengers via thiolysis of positively-charged NBD
 amines
;
_journal_issue                   30
_journal_name_full               'Chemical Science'
_journal_page_first              7823
_journal_page_last               7828
_journal_paper_doi               10.1039/D0SC01518K
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C15 H14 N6 O3'
_chemical_formula_sum            'C15 H14 N6 O3'
_chemical_formula_weight         326.32
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc242dxk
_audit_creation_date             2019-11-27
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2019-11-29 deposited with the CCDC.	2020-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.450(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.3096(6)
_cell_length_b                   29.084(2)
_cell_length_c                   7.5539(8)
_cell_measurement_reflns_used    3907
_cell_measurement_temperature    133.15
_cell_measurement_theta_max      32.9400
_cell_measurement_theta_min      2.7720
_cell_volume                     1385.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrystalClear (Rigaku, 2008)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      133.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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   -115.00  65.00   1.00    1.00    --  -25.00  45.00   0.00  180
  2  \w   -115.00  35.00   1.00    1.00    --  -25.00  45.00  90.00  150
  3  \w   -115.00   5.00   1.00    1.00    --  -25.00  45.00 180.00  120
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0453820000
_diffrn_orient_matrix_UB_12      -0.0221941000
_diffrn_orient_matrix_UB_13      -0.0101425000
_diffrn_orient_matrix_UB_21      -0.1022811000
_diffrn_orient_matrix_UB_22      0.0099801000
_diffrn_orient_matrix_UB_23      -0.0081381000
_diffrn_orient_matrix_UB_31      0.0108910000
_diffrn_orient_matrix_UB_32      0.0015120000
_diffrn_orient_matrix_UB_33      -0.0930743000
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            12221
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.364
_diffrn_reflns_theta_min         2.787
_diffrn_source                   'rotating anode'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_description       needle
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       0.016(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2826
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0615
_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^)+(0.0637P)^2^+1.2721P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1544
_refine_ls_wR_factor_ref         0.1686
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2159
_reflns_number_total             2826
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc01518k2.cif
_cod_data_source_block           r20191127a
_cod_depositor_comments
;Adding full bibliography for 1558556--1558557.cif.

 Adding full bibliography for 1558556--1558557.cif.
;
_cod_original_cell_volume        1385.7(2)
_cod_database_code               1558556
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C15H16N6O3
_reflns_odcompleteness_completeness 92.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.80
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C6(H6A,H6B), C8(H8A,H8B), C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C4(H4), C2(H2), C1(H1), C3(H3)
;
_shelx_res_checksum              21803
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.261
_oxdiff_exptl_absorpt_empirical_full_min 0.646