Molecular Cursor Caliper: A Fluorescent Sensor for Dicarboxylate Dianions.
Chen, Wei; Guo, Chenxing; He, Qing; Chi, Xiaodong; Lynch, Vincent M.; Zhang, Zhiyun; Su, Jianhua; Tian, He; Sessler, Jonathan L.; Journal of the American Chemical Society 141 (2019) 14798–14806; doi:10.1021/jacs.9b07170

data_4127631
_publ_section_title
;
 Molecular Cursor Caliper: A Fluorescent Sensor for Dicarboxylate
 Dianions.
;
_journal_issue                   37
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14798
_journal_page_last               14806
_journal_paper_doi               10.1021/jacs.9b07170
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C90 H90 N10 O4, H2 O, 3(C2 H6 O)'
_chemical_formula_sum            'C96 H110 N10 O8'
_chemical_formula_weight         1531.93
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-07-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                107.827(5)
_cell_angle_beta                 90.675(5)
_cell_angle_gamma                97.043(5)
_cell_formula_units_Z            2
_cell_length_a                   10.2435(6)
_cell_length_b                   20.2635(12)
_cell_length_c                   21.1965(11)
_cell_measurement_reflns_used    3928
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.6510
_cell_measurement_theta_min      3.6410
_cell_volume                     4151.2(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Agilent SuperNova with Atlas S2 CCD'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1039
_diffrn_reflns_av_unetI/netI     0.1878
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30115
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.853
_diffrn_reflns_theta_min         2.192
_exptl_absorpt_coefficient_mu    0.620
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_description       needle
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.111
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.039
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1177
_refine_ls_number_reflns         16734
_refine_ls_number_restraints     1060
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1822
_refine_ls_R_factor_gt           0.0980
_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^)+(0.1178P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2445
_refine_ls_wR_factor_ref         0.3215
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7691
_reflns_number_total             16734
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b07170_si_004.cif
_cod_data_source_block           cwhost
_cod_database_code               4127631
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained planarity
 N3, C11, C12, C13, C14
 with sigma of 0.01
 N3A, C11A, C12A, C13A, C14A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
N3 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C10 \\sim C88 \\sim C89 \\sim
N3A \\sim C11A \\sim C12A \\sim C13A \\sim C14A \\sim C10A \\sim C88A \\sim
C89A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
O1D \\sim C1D \\sim C2D \\sim O1E \\sim C1E \\sim C2E: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
4. Others
 Fixed Sof: N3(0.6) H3A(0.6) C11(0.6) C12(0.6) H12(0.6) C13(0.6) H13(0.6)
 C14(0.6) C10(0.6) C88(0.6) H88A(0.6) H88B(0.6) H88C(0.6) C89(0.6) H89A(0.6)
 H89B(0.6) H89C(0.6) N3A(0.4) H3AA(0.4) C11A(0.4) C12A(0.4) H12A(0.4) C13A(0.4)
 H13A(0.4) C14A(0.4) C10A(0.4) C88A(0.4) H88D(0.4) H88E(0.4) H88F(0.4)
 C89A(0.4) H89D(0.4) H89E(0.4) H89F(0.4) O1C(0.6) H1C(0.6) C1C(0.6) H1CA(0.6)
 H1CB(0.6) C2C(0.6) H2CA(0.6) H2CB(0.6) H2CC(0.6) O1B(0.4) H1B(0.4) C1B(0.4)
 H1BA(0.4) H1BB(0.4) C2B(0.4) H2BA(0.4) H2BB(0.4) H2BC(0.4) O1D(0.5) H1D(0.5)
 C1D(0.5) H1DA(0.5) H1DB(0.5) C2D(0.5) H2DA(0.5) H2DB(0.5) H2DC(0.5) O1E(0.5)
 H1E(0.5) C1E(0.5) H1EA(0.5) H1EB(0.5) C2E(0.5) H2EA(0.5) H2EB(0.5) H2EC(0.5)
5.a Free rotating group:
 O5(H5A,H5B)
5.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C55(H55A,H55B), C1A(H1AA,H1AB), C1C(H1CA,H1CB), C1B(H1BA,
 H1BB), C1D(H1DA,H1DB), C1E(H1EA,H1EB)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C8(H8), N3(H3A), C12(H12), C13(H13), N3A(H3AA),
 C12A(H12A), C13A(H13A), C17(H17), C18(H18), C24(H24), C25(H25), C27(H27),
 C28(H28), C30(H30), C31(H31), C32(H32), C33(H33), C37(H37), C38(H38), C39(H39),
  C40(H40), C43(H43), C44(H44), C45(H45), C46(H46), C50(H50), C51(H51),
 C53(H53), C54(H54), C59(H59), C60(H60), C64(H64), C65(H65), C69(H69), C70(H70),
  C74(H74), C75(H75), N1(H1), N2(H2A), N4(H4), N7(H7A), N8(H8A), N9(H9),
 N10(H10)
5.d Tetrahedral OH refined with riding coordinates:
 O1A(H1A), O1C(H1C), O1B(H1B), O1D(H1D), O1E(H1E)
5.e Idealised Me refined as rotating group:
 C02L(H02A,H02B,H02C), C88(H88A,H88B,H88C), C89(H89A,H89B,H89C), C88A(H88D,
 H88E,H88F), C89A(H89D,H89E,H89F), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C),
 C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C81(H81A,H81B,H81C), C82(H82A,H82B,
 H82C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C85(H85A,H85B,H85C), C86(H86A,
 H86B,H86C), C87(H87A,H87B,H87C), C2A(H2AA,H2AB,H2AC), C2C(H2CA,H2CB,H2CC),
 C2B(H2BA,H2BB,H2BC), C2D(H2DA,H2DB,H2DC), C2E(H2EA,H2EB,H2EC)
;
_shelx_res_checksum              88353
_shelx_hkl_checksum              19623
_olex2_submission_special_instructions 'No special instructions were received'