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_7129345
_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         'C79 H64 Fe2 N23 O6, O, 4(B F4)'
_chemical_formula_sum            'C79 H64 B4 F16 Fe2 N23 O7'
_chemical_formula_weight         1906.44
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_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                104.066(5)
_cell_angle_beta                 100.757(4)
_cell_angle_gamma                94.934(4)
_cell_formula_units_Z            2
_cell_length_a                   12.7733(13)
_cell_length_b                   19.091(2)
_cell_length_c                   22.774(3)
_cell_measurement_reflns_used    8492
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      23.26
_cell_measurement_theta_min      2.22
_cell_volume                     5241.8(10)
_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      120.0
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.1043
_diffrn_reflns_av_unetI/netI     0.0828
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            106089
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.144
_diffrn_reflns_theta_max         25.144
_diffrn_reflns_theta_min         2.218
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.476
_exptl_absorpt_correction_T_max  0.0096
_exptl_absorpt_correction_T_min  0.0014
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1006 before and 0.0741 after correction.
The Ratio of minimum to maximum transmission is 0.1458.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.077
_exptl_crystal_description       block
_exptl_crystal_F_000             3182
_refine_diff_density_max         0.914
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1180
_refine_ls_number_reflns         18645
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1705
_refine_ls_R_factor_gt           0.1133
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3021
_refine_ls_wR_factor_ref         0.3456
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9679
_reflns_number_total             18645
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06166f2.cif
_cod_data_source_block           1021d
_cod_depositor_comments
;

2024-09-02
Formula changed to actual composition, that in the orginal file makes no sense
                 miguel
;
_cod_original_formula_weight         3277.88
_cod_original_cell_volume        5241.7(10)
_cod_original_formula_sum        'C33 H33 B0.50 F0.50 Fe33 N33 O33'
_cod_database_code               7129345
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Uiso/Uaniso restraints and constraints
F27 \\sim F24 \\sim B7 \\sim F25 \\sim F26: within 2.8A with sigma of 0.04 and
sigma for terminal atoms of 0.08
3.a Secondary CH2 refined with riding coordinates:
 C028(H02A,H02B), C02F(H02D,H02F), C02P(H02L,H02O), C037(H03A,H03B), C03G(H03G,
 H03H), C03H(H03I,H03J)
3.b Aromatic/amide H refined with riding coordinates:
 N19(H19), N00G(H00G), C42(H42), C41(H41), C43(H43), C019(H019), C01C(H01C),
 N20(H20), C01J(H01J), N21(H21), C01P(H01P), C01S(H01S), C01U(H01U), C01W(H01W),
  C01X(H01X), C01Y(H01Y), C01Z(H01Z), C020(H020), C021(H021), C022(H022),
 C023(H023), C024(H024), C02A(H02C), C02E(H02E), C02G(H02G), C02H(H02H),
 C02I(H02I), C02J(H02J), C02K(H02K), C02M(H02M), C02N(H02N), C02Q(H02Q),
 C02R(H02R), C02T(H02T), C02U(H02U), C02V(H02V), C02W(H02W), C02X(H02X),
 C02Y(H02Y), C030(H030), C031(H031), C034(H034), C036(H036), C038(H038),
 C03A(H03C), C03B(H03D), C03C(H03E), C03F(H03F), C03I(H03K), C03J(H03L),
 C03M(H03M), C03Q(H03Q)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              64802
_shelx_fab_checksum              91341
_olex2_submission_special_instructions 'No special instructions were received'