Guest Inclusion Modulates Concentration and Persistence of Photogenerated Radicals in Assembled Triphenylamine Macrocycles.
Sindt, Ammon J.; DeHaven, Baillie A.; Goodlett, Dustin W.; Hartel, Johannes O.; Ayare, Pooja J.; Du, Yong; Smith, Mark D.; Mehta, Anil K.; Brugh, Alexander M.; Forbes, Malcolm D. E.; Bowers, Clifford R.; Vannucci, Aaron K.; Shimizu, Linda S.; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b11518

data_4133817
_publ_section_title
;
 Guest Inclusion Modulates Concentration and Persistence of Photogenerated
 Radicals in Assembled Triphenylamine Macrocycles.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b11518
_journal_year                    2019
_chemical_formula_moiety         'C42 H36 Br2 N6 O2, 0.58(C4 H8 O2)'
_chemical_formula_sum            'C44.33 H40.67 Br2 N6 O3.17'
_chemical_formula_weight         867.97
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.746(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.838(2)
_cell_length_b                   4.6056(6)
_cell_length_c                   26.637(3)
_cell_measurement_reflns_used    6655
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.029
_cell_measurement_theta_min      2.610
_cell_volume                     1915.0(4)
_computing_cell_refinement       'SAINT+ Ver. 8.38A (Bruker-AXS, 2016)'
_computing_data_collection       'Bruker APEX3 v2016.5-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT+ Ver. 8.38A (Bruker-AXS, 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      100(2)
_diffrn_detector                 'Bruker PHOTON-100 area detector'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            19443
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.180
_diffrn_reflns_theta_max         25.182
_diffrn_reflns_theta_min         2.190
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.168
_exptl_absorpt_correction_T_max  0.8620
_exptl_absorpt_correction_T_min  0.8002
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0579 before and 0.0455 after correction.
The Ratio of minimum to maximum transmission is 0.9283.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       needle
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         3429
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0467
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+5.8823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1079
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2817
_reflns_number_total             3429
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11518_si_003.cif
_cod_data_source_block           brnph3dmc_diox
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               4133817
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.781
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 N1-H1 = N2-H2
 0.85 with sigma of 0.02
 O2S-C4S_$1 = O2S-C3S = O2S_$1-C3S_$1 = O2S_$1-C4S = O1S_$2-C1S_$2 = O1S_$2-
 C2S = O1S-C2S_$2 = O1S-C1S = O3S_$2-C5S_$2 = O3S_$2-C6S = O3S-C6S_$2 = O3S-C5S
 1.42 with sigma of 0.01
 C4S_$1-C3S_$1 = C4S-C3S = C2S_$2-C1S_$2 = C2S-C1S = C6S_$2-C5S_$2 = C6S-C5S
 1.48 with sigma of 0.01
 O2S-O2S_$1 = O3S-O3S_$2 = O1S-O1S_$2
 2.81 with sigma of 0.015
 C1S_$2-C1S = C2S-C2S_$2 = C3S-C3S_$1 = C4S_$1-C4S = C6S_$2-C6S = C5S-C5S_$2
 2.76 with sigma of 0.015
 C3S-C4S_$1 = C4S-C3S_$1 = C1S_$2-C2S = C2S_$2-C1S = C5S_$2-C6S = C6S_$2-C5S
 2.33 with sigma of 0.015
3. Uiso/Uaniso restraints and constraints
Uiso(H2) = Uiso(H1)
Uiso(O2S) = Uiso(C3S) = Uiso(C4S)
Uiso(O3S) = Uiso(C5S) = Uiso(C6S)
4. Others
 Sof(O1S)=Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(C2S)=Sof(H2SA)=Sof(H2SB)=FVAR(1)
 Sof(O2S)=Sof(C3S)=Sof(H3SA)=Sof(H3SB)=Sof(C4S)=Sof(H4SA)=Sof(H4SB)=FVAR(2)
 Sof(O3S)=Sof(C5S)=Sof(H5SA)=Sof(H5SB)=Sof(C6S)=Sof(H6SA)=Sof(H6SB)=FVAR(3)
5.a Riding coordinates:
 C3S(H3SA,H3SB)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C21(H21A,H21B), C1S(H1SA,H1SB), C2S(H2SA,H2SB), C4S(H4SA,H4SB),
 C5S(H5SA,H5SB), C6S(H6SA,H6SB)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13), C14(H14),
 C16(H16), C17(H17), C19(H19), C20(H20)
;
_shelx_res_checksum              63914
_shelx_hkl_checksum              47856
_olex2_submission_special_instructions 'No special instructions were received'