Organic Nanoparticles-Assisted Low-Power STED Nanoscopy.
Man, Zhongwei; Cui, Hongtu; Lv, Zheng; Xu, Zhenzhen; Wu, Zhaoyang; Wu, Yishi; Liao, Qing; Liu, Meihui; Xi, Peng; Zheng, Lemin; Fu, Hongbing; Nano letters 21 (2021) 3487–3494; doi:10.1021/acs.nanolett.1c00161

data_1562353
_publ_section_title
;
 Organic Nanoparticles-Assisted Low-Power STED Nanoscopy.
;
_journal_issue                   8
_journal_name_full               'Nano letters'
_journal_page_first              3487
_journal_page_last               3494
_journal_paper_doi               10.1021/acs.nanolett.1c00161
_journal_volume                  21
_journal_year                    2021
_chemical_formula_moiety         '0.5(C H2 Cl2), C56 H60 N4, C6 H14'
_chemical_formula_sum            'C62.5 H75 Cl N4'
_chemical_formula_weight         917.71
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.290(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.5082(4)
_cell_length_b                   20.3290(6)
_cell_length_c                   37.5089(12)
_cell_measurement_reflns_used    10429
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.3190
_cell_measurement_theta_min      2.3420
_cell_volume                     10973.3(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.970
_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    -69.00   5.00   1.00    5.00    --  -40.98  57.00 150.00   74
  2  \w    -32.00  -3.00   1.00    5.00    --  -40.98 125.00  90.00   29
  3  \w    -74.00  32.00   1.00    5.00    --  -40.98  77.00-120.00  106
  4  \w     56.00  97.00   1.00    5.00    --   40.98-125.00 -30.00   41
  5  \w     62.00 105.00   1.00   10.00    --  106.95 -95.00 -60.00   43
  6  \w     26.00  96.00   1.00   10.00    --  106.95 -95.00-180.00   70
  7  \w     79.00 177.00   1.00   10.00    --  106.95  30.00 -60.00   98
  8  \w    150.00 178.00   1.00   10.00    --  106.95  45.00-150.00   28
  9  \w    101.00 177.00   1.00   10.00    --  106.95 125.00-120.00   76
 10  \w     85.00 137.00   1.00   10.00    --  106.95 -77.00 150.00   52
 11  \w     46.00 121.00   1.00   10.00    --  106.95-125.00 120.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0201354000
_diffrn_orient_matrix_UB_12      -0.0723882000
_diffrn_orient_matrix_UB_13      0.0101971000
_diffrn_orient_matrix_UB_21      0.1047851000
_diffrn_orient_matrix_UB_22      0.0124808000
_diffrn_orient_matrix_UB_23      -0.0000671000
_diffrn_orient_matrix_UB_31      0.0090838000
_diffrn_orient_matrix_UB_32      0.0184437000
_diffrn_orient_matrix_UB_33      0.0401422000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            44555
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.522
_diffrn_reflns_theta_min         2.375
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.919
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84452
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
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    1.111
_exptl_crystal_description       block
_exptl_crystal_F_000             3960
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.697
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1232
_refine_ls_number_reflns         21435
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1158
_refine_ls_R_factor_gt           0.0932
_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^)+(0.1672P)^2^+10.8076P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2633
_refine_ls_wR_factor_ref         0.2919
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16062
_reflns_number_total             21435
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nl1c00161_si_002.cif
_cod_data_source_block           mzw
_cod_original_formula_sum        'C62.50 H75 Cl N4'
_cod_database_code               1562353
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Rigid bond restraints
 C032, C03E
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C49, C50
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C49, C52
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1S, C2S
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C032, C03D
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C030, C03N
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C032 \\sim C03E: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
C49 \\sim C50: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
C49 \\sim C52: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
C1S \\sim C2S: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
C032 \\sim C03D: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
C030 \\sim C03N: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
Uanis(C032) = Uanis(C03E)
Uanis(C030) = Uanis(C03L)
4.a Secondary CH2 refined with riding coordinates:
 C13S(H13A,H13B), C8S(H8SA,H8SB), C9S(H9SA,H9SB), C4S(H4SA,H4SB), C2S(H2SA,
 H2SB), C10S(H10A,H10B), C11S(H11A,H11B), C5S(H5SA,H5SB), C3S(H3SA,H3SB)
4.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C22(H22), C00B(H00B), C32(H32), C21(H21), C00G(H00G), C00J(H00J),
 C00K(H00K), C00L(H00L), C00O(H00O), C00Q(H00Q), C00R(H00R), C19(H19), C18(H18),
  C28(H28), C29(H29), C015(H015), C016(H016), C019(H019), C5(H5), C48(H48),
 C01I(H01I), C11(H11), C12(H12), C44(H44), C8(H8), C47(H47), C01S(H01S),
 C45(H45), C01U(H01U), C4(H4), C9(H9), C01Z(H01Z), C020(H020), C021(H021),
 C34(H34), C025(H025), C026(H026), C02B(H02D), C38(H38), C02E(H02E), C36(H36),
 C35(H35), C1(H1), C02R(H02U), C02S(H02V), C2(H2), C02U(H02W)
4.c Idealised Me refined as rotating group:
 C029(H02A,H02B,H02C), C02F(H02F,H02G,H02H), C02K(H02I,H02J,H02K), C02L(H02L,
 H02M,H02N), C02M(H02O,H02P,H02Q), C15(H15A,H15B,H15C), C02O(H02R,H02S,H02T),
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C02Z(H02X,H02Y,H), C031(H03A,H03B,
 H03C), C51(H51A,H51B,H51C), C42(H42A,H42B,H42C), C41(H41A,H41B,H41C), C50(H50A,
 H50B,H50C), C037(H03P,H03Q,H03R), C40(H40A,H40B,H40C), C52(H52A,H52B,H52C),
 C03C(H03S,H03T,H03U), C03D(H03D,H03E,H03F), C03E(H03G,H03H,H03I), C03F(H03V,
 H03W,H03X), C12S(H12A,H12B,H12C), C03L(H03J,H03K,H03L), C7S(H7SA,H7SB,H7SC),
 C03N(H03M,H03N,H03O), C1S(H1SA,H1SB,H1SC), C6S(H6SA,H6SB,H6SC)
;
_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 1.329
_oxdiff_exptl_absorpt_empirical_full_min 0.771