Fluorescent copolymer aggregate sensor for lithium chloride.
Wang, Hu; Jones, Leighton O.; Zhao, Tian; Hwang, Inhong; Lynch, Vincent M.; Khashab, Niveen M.; Schatz, George C.; Page, Zachariah A.; Sessler, Jonathan L.; Chemical science 14 (2023) 4120–4125; doi:10.1039/d2sc05342j

data_1568686
_publ_section_title
;
 Fluorescent copolymer aggregate sensor for lithium chloride.
;
_journal_issue                   15
_journal_name_full               'Chemical science'
_journal_page_first              4120
_journal_page_last               4125
_journal_paper_doi               10.1039/d2sc05342j
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety
'C58 H68 N4 O10, C14 H16 N, 2.229(C2 H3 N), H2 O, Cl'
_chemical_formula_sum            'C76.46 H92.69 Cl N7.23 O11'
_chemical_formula_weight         1324.45
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-07-01 deposited with the CCDC.	2023-03-22 downloaded from the CCDC.
;
_cell_angle_alpha                104.805(6)
_cell_angle_beta                 97.924(5)
_cell_angle_gamma                96.664(5)
_cell_formula_units_Z            2
_cell_length_a                   12.7225(8)
_cell_length_b                   15.8452(10)
_cell_length_c                   18.7186(13)
_cell_measurement_reflns_used    4089
_cell_measurement_temperature    100.03(16)
_cell_measurement_theta_max      73.1180
_cell_measurement_theta_min      3.5280
_cell_volume                     3568.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.03(16)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2940
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.950
_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   -115.00 -16.00   1.00   13.50    --  -41.59 -57.00  60.00   99
  2  \w    -55.00  33.00   1.00   13.50    --  -41.59  38.00-150.00   88
  3  \w      6.00  76.00   1.00   13.50    --   41.59 -99.00 -90.00   70
  4  \w    -21.00  74.00   1.00   13.50    --   41.59 -77.00 -60.00   95
  5  \w     24.00 107.00   1.00   40.50    --  107.09 -94.00-180.00   83
  6  \w     57.00 133.00   1.00   40.50    --  107.09 -45.00   0.00   76
  7  \w     78.00 175.00   1.00   40.50    --  107.09  59.00 -18.00   97
  8  \w     59.00 130.00   1.00   40.50    --  107.09 -61.00 -90.00   71
  9  \w     36.00 128.00   1.00   40.50    --  107.09 -45.00-180.00   92
 10  \w     27.00 107.00   1.00   40.50    --  107.09 -94.00  60.00   80
 11  \w     64.00 107.00   1.00   40.50    --  107.09 -94.00 -90.00   43
 12  \w     21.00 169.00   1.00   40.50    --  107.09   0.00 150.00  148
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1095505000
_diffrn_orient_matrix_UB_12      -0.0325520000
_diffrn_orient_matrix_UB_13      0.0011470000
_diffrn_orient_matrix_UB_21      -0.0528795000
_diffrn_orient_matrix_UB_22      -0.0861411000
_diffrn_orient_matrix_UB_23      -0.0600471000
_diffrn_orient_matrix_UB_31      0.0230563000
_diffrn_orient_matrix_UB_32      0.0434984000
_diffrn_orient_matrix_UB_33      -0.0621861000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0702
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18197
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.407
_diffrn_reflns_theta_min         2.921
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.996
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_description       prism
_exptl_crystal_F_000             1414
_exptl_crystal_size_max          0.244
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.032
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     950
_refine_ls_number_reflns         18197
_refine_ls_number_restraints     634
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0589
_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^)+(0.1123P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1769
_refine_ls_wR_factor_ref         0.1919
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12649
_reflns_number_total             18197
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9912\% 
around [0.00 0.00 1.00] (reciprocal) or [0.23 0.30 0.93] (direct)
;
_cod_data_source_file            d2sc05342j4.cif
_cod_data_source_block           1-3calix-dibnzylhcl
_cod_depositor_comments          'Adding full bibliography for 1568686.cif.'
_cod_database_code               1568686
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C76H92N7O11Cl
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.4875(11)
 0.5125(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H,H) groups
3. Restrained distances
 C76A-N7
 1.15 with sigma of 0.03
 C80-N78
 2.6 with sigma of 0.02
 N78-C79
 1.15 with sigma of 0.02
 C76-N7
 1.15 with sigma of 0.03
 C76-C75
 1.45 with sigma of 0.03
 C79-C80
 1.45 with sigma of 0.02
 C75A-C76A
 1.45 with sigma of 0.03
 N6-C73 \\sim N6A-C73
 with sigma of 0.04
 N6-C74 \\sim N6A-C74A
 with sigma of 0.02
 C73-C74 \\sim C73-C74A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(N6A) = Uanis(N6)
Uanis(C74A) = Uanis(C74)
5. Others
 Sof(H41)=Sof(O10A)=Sof(O9A)=Sof(C57A)=Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(H77C)=
 Sof(C79)=Sof(C80)=Sof(H80A)=Sof(H80B)=Sof(H80C)=Sof(N78)=1-FVAR(1)
 Sof(O9)=Sof(O10)=Sof(H42)=Sof(C57)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H58C)=
 FVAR(1)
 Sof(C75A)=Sof(H75D)=Sof(H75E)=Sof(H75F)=Sof(C76A)=1-FVAR(2)
 Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(H75C)=Sof(C76)=FVAR(2)
 Sof(H73D)=Sof(H73E)=Sof(H73F)=Sof(C74A)=Sof(N6A)=1-FVAR(3)
 Sof(N6)=Sof(H73A)=Sof(H73B)=Sof(H73C)=Sof(C74)=FVAR(3)
6.a Free rotating group:
 O11(H11A,H11B)
6.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,
 H37B), C38(H38A,H38B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B),
 C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), N5(H5A,H5B), C59(H59A,H59B),
 C66(H66A,H66B)
6.c Me refined with riding coordinates:
 C58(H58A,H58B,H58C), C77(H77A,H77B,H77C)
6.d Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), C2(H2A), C3(H3A), C7(H7), C8(H8), C12(H12),
 C13(H13), C17(H17), C18(H18), C28(H28), C29(H29), C31(H31), C32(H32), C40(H40),
  C41(H41), C42(H42), C43(H43), C52(H52), C53(H53), C55(H55), C56(H56),
 C61(H61), C62(H62), C63(H63), C64(H64), C65(H65), C68(H68), C69(H69), C70(H70),
  C71(H71), C72(H72)
6.e Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C73(H73A,H73B,H73C), C73(H73D,
 H73E,H73F), C75(H75A,H75B,H75C), C80(H80A,H80B,H80C), C75A(H75D,H75E,H75F)
;
_shelx_res_checksum              15867
_shelx_hkl_checksum              59544
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.454
_oxdiff_exptl_absorpt_empirical_full_min 0.850
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2