Dye-loaded metal-organic helical capsules applied to the combination of photocatalytic H2S splitting and nitroaromatic hydrogenation
Yang, Yang; Li, Hanning; Jing, Xu; Wu, Yuchen; Shi, Youpeng; Duan, Chunying; Chemical Communications  (2021) –; doi:10.1039/D1CC06166F

data_7129346
_publ_section_title
;
 Dye-loaded metal-organic helical capsules applied to the combination of
 photocatalytic H2S splitting and nitroaromatic hydrogenation
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06166F
_journal_year                    2021
_chemical_formula_moiety
'C15 H11 Fe0.33 N2, 2(C0.33 F O S0.33), 0.17(C2 N)'
_chemical_formula_sum            'C16 H11 F2 Fe0.33 N2.17 O2 S0.67'
_chemical_formula_weight         343.59
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-10-24 deposited with the CCDC.	2021-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   10.407(3)
_cell_length_b                   10.407(3)
_cell_length_c                   48.843(12)
_cell_measurement_reflns_used    875
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      17.79
_cell_measurement_theta_min      2.26
_cell_volume                     4581(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      223.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.1381
_diffrn_reflns_av_unetI/netI     0.0930
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            16050
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.092
_diffrn_reflns_theta_max         25.092
_diffrn_reflns_theta_min         2.085
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.503
_exptl_absorpt_correction_T_max  0.0140
_exptl_absorpt_correction_T_min  0.0032
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0740 before and 0.0588 after correction.
The Ratio of minimum to maximum transmission is 0.2286.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_description       block
_exptl_crystal_F_000             2106
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         2738
_refine_ls_number_restraints     125
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.2597
_refine_ls_R_factor_gt           0.1199
_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^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2810
_refine_ls_wR_factor_ref         0.3444
_reflns_Friedel_coverage         0.000
_reflns_number_gt                993
_reflns_number_total             2738
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06166f2.cif
_cod_data_source_block           1023b
_cod_original_cell_volume        4581(3)
_cod_database_code               7129346
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.940(3)
 0.060(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 C101-C102
 1.47 with sigma of 0.02
 C102-N101
 1.1 with sigma of 0.02
 C101-N101
 2.57 with sigma of 0.02
 S2-C21
 1.75 with sigma of 0.02
 S2-O21 = S2-O22 = S2-O23
 1.4 with sigma of 0.02
 C21-F21 = C21-F22 = C21-F23
 1.47 with sigma of 0.02
 C12-C13
 1.5 with sigma of 0.02
 F21-F22 \\sim F21-F23 \\sim F22-F23
 with sigma of 0.02
 O21-O22 \\sim O21-O23 \\sim O22-O23
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
S2 \\sim O21 \\sim F21 \\sim F22 \\sim C21 \\sim O22 \\sim F23 \\sim O23:
within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(S2) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(F21) \\sim Ueq, Uanis(F22)
\\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(F23) \\sim Ueq,
Uanis(O23) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C13) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
5. Others
 Fixed Sof: C101(0.16667) N101(0.16667) C102(0.16667) S2(0.33333) O21(0.33333)
 F21(0.33333) F22(0.33333) C21(0.33333) O22(0.33333) F23(0.33333) O23(0.33333)
6.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C1(H1), C4(H4), C3(H3), C2(H2), C8(H8), C12(H12), C7(H7),
 C15(H15), C14(H14)
;
_shelx_res_checksum              98400
_olex2_submission_special_instructions 'No special instructions were received'