Triplexed Tracking Labile Sulfur-Containing Species on a Single-Molecule "Nezha" Sensor.
Wang, Shuo; Ren, Jia-Shu; Shan, Lian-Yun; Sun, Xiao-Yan; Di, Bin; Gu, Ning; Chen, Jin-Long; Analytical chemistry  (2020) –; doi:10.1021/acs.analchem.9b04688

data_1557149
_publ_section_title
;
 Triplexed Tracking Labile Sulfur-Containing Species on a Single-Molecule
 &quot;Nezha&quot; Sensor.
;
_journal_name_full               'Analytical chemistry'
_journal_paper_doi               10.1021/acs.analchem.9b04688
_journal_year                    2020
_chemical_formula_moiety         'C30 H32 N4 O3'
_chemical_formula_sum            'C30 H32 N4 O3'
_chemical_formula_weight         496.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-06-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.754(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2782(16)
_cell_length_b                   11.9261(15)
_cell_length_c                   18.859(2)
_cell_measurement_reflns_used    8489
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.544
_cell_measurement_theta_min      2.804
_cell_volume                     2682.4(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      149.98
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1047
_diffrn_reflns_av_unetI/netI     0.0756
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            46288
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         2.804
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         4775
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.1814
_refine_ls_R_factor_gt           0.1049
_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^)+(0.0817P)^2^+5.7552P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2285
_refine_ls_wR_factor_ref         0.2638
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2726
_reflns_number_total             4775
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ac9b04688_si_002.cif
_cod_data_source_block           bb_a
_cod_database_code               1557149
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.998
_shelx_estimated_absorpt_t_min   0.996
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N3-C25A = N3-C25 = N3-C23
 1.5 with sigma of 0.005
 C26-C25 = C26A-C25A = C24-C23
 1.54 with sigma of 0.005
 H25D-H24C
 2.1 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C25A) = Uanis(C25)
Uanis(C26) = Uanis(C26A)
4. Others
 Sof(C25A)=Sof(H25C)=Sof(H25D)=Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(1)
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C27(H27A,H27B), C25(H25A,H25B), C23(H23A,H23B), C25A(H25C,H25D)
5.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C20(H20), C18(H18), C12(H12), C3(H3), C9(H9), C15(H15), C4(H4),
 C6(H6), C13(H13), C5(H5), C10(H10)
5.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C28(H28A,H28B,H28C), C24(H24A,H24B,H24C), C26(H26A,H26B,
 H26C), C26A(H26D,H26E,H26F)
;
_shelx_res_checksum              1417
_shelx_hkl_checksum              87176
_olex2_submission_special_instructions 'No special instructions were received'