Chelate-Free “Turn-ON”-Type Fluorescence Detection of Trivalent Metal Ions
Matsumoto, Shota; Umeno, Tomohiro; Suzuki, Noriko; Usui, Kazuteru; Kawahata, Masatoshi; Karasawa, Satoru; Chemical Communications  (2022) –; doi:10.1039/D2CC04815A

data_7130845
_publ_section_title
;
 Chelate-Free &#x201C;Turn-ON&#x201D;-Type Fluorescence Detection of
 Trivalent Metal Ions
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04815A
_journal_year                    2022
_chemical_formula_moiety         'C22 H18 F6 N4'
_chemical_formula_sum            'C22 H18 F6 N4'
_chemical_formula_weight         452.40
_chemical_name_systematic        5-133_7
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-20
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2022-08-03 deposited with the CCDC.	2022-10-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.4686(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.65252(5)
_cell_length_b                   36.6358(2)
_cell_length_c                   14.87749(10)
_cell_measurement_reflns_used    17077
_cell_measurement_temperature    93
_cell_measurement_theta_max      76.3400
_cell_measurement_theta_min      3.2890
_cell_volume                     4038.71(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.34a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.34a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.34a (Rigaku OD, 2019)'
_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_temperature      93
_diffrn_detector                 'Rigaku HyPix-6000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.888
_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     76.00 121.00   0.50    0.32    --   48.95 125.00-180.00   90
  2  \w     77.00 112.00   0.50    0.32    --   48.95 125.00 -90.00   70
  3  \w     97.00 157.00   0.50    1.28    --  107.74  19.00  90.00  120
  4  \w    -24.00  15.00   0.50    0.32    --   48.95 -19.00 -60.00   78
  5  \w    -20.00  49.00   0.50    0.32    --   48.95 -56.00-148.00  138
  6  \w     39.00  64.00   0.50    1.28    --  107.74 -64.00  42.00   50
  7  \w    -59.00 -33.00   0.50    1.28    --  -97.00  57.00-120.00   52
  8  \w    -58.00 -33.00   0.50    1.28    --  -97.00  57.00 -60.00   50
  9  \w    -69.00 -24.00   0.50    1.28    --  -97.00  56.00  -6.00   90
 10  \w    -65.00 -31.00   0.50    1.28    --  -97.00  57.00  30.00   68
 11  \w   -112.00 -66.00   0.50    1.28    --  -97.00 125.00  90.00   92
 12  \w    -59.00 -25.00   0.50    1.28    --  -97.00 125.00  90.00   68
 13  \w   -158.00 -84.00   0.50    1.28    --  -97.00 -37.00 -90.00  148
 14  \w   -168.00-117.00   0.50    1.28    --  -97.00 -77.00 -90.00  102
 15  \w   -139.00 -84.00   0.50    1.28    --  -97.00-125.00 -22.00  110
 16  \w   -154.00 -87.00   0.50    1.28    --  -97.00 -64.00  42.00  134
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  Rigaku_Synergy-Custom_007
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0236195000
_diffrn_orient_matrix_UB_12      0.0105416000
_diffrn_orient_matrix_UB_13      0.1025878000
_diffrn_orient_matrix_UB_21      0.1475542000
_diffrn_orient_matrix_UB_22      -0.0293377000
_diffrn_orient_matrix_UB_23      0.0291074000
_diffrn_orient_matrix_UB_31      0.1445620000
_diffrn_orient_matrix_UB_32      0.0282177000
_diffrn_orient_matrix_UB_33      -0.0080598000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.888
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22091
_diffrn_reflns_point_group_measured_fraction_full 0.785
_diffrn_reflns_point_group_measured_fraction_max 0.714
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.628
_diffrn_reflns_theta_min         3.068
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              micromax007
_exptl_absorpt_coefficient_mu    1.123
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.34a (Rigaku Oxford Diffraction, 2019)
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    1.488
_exptl_crystal_description       plate
_exptl_crystal_F_000             1856
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.145
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.091
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 4172 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_coef       0.00083(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1162
_refine_ls_number_reflns         12134
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0565P)^2^+0.5243P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0844
_reflns_Friedel_coverage         0.582
_reflns_Friedel_fraction_full    0.603
_reflns_Friedel_fraction_max     0.534
_reflns_number_gt                11781
_reflns_number_total             12134
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04815a2.cif
_cod_data_source_block           7
_cod_database_code               7130845
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N F'
_diffrn_oxdiff_digest_frames
;
01153f68d0025a964b2ebde3d655843456014600627
;
_diffrn_oxdiff_digest_hkl
;
01535df8471eca9a71aca40e2acccd390a4366
;
_reflns_odcompleteness_completeness 96.33
_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.a Secondary CH2 refined with riding coordinates:
 C1K(H1KA,H1KB), C2G(H2GA,H2GB), C2Q(H2QA,H2QB), C2U(H2UA,H2UB), C2Y(H2YA,
 H2YB), C31(H31A,H31B), C32(H32A,H32B), C36(H36A,H36B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C12(H12), C17(H17), C18(H18), C1B(H1B), C1(H1), C1D(H1D),
 C1F(H1F), C1G(H1G), C1M(H1M), C1N(H1N), C1P(H1P), C1S(H1S), C1U(H1U), C1X(H1X),
  C5(H5), C23(H23), C25(H25), C1C(H1C), C29(H29), C2C(H2C), C2E(H2E), C2F(H2F),
 C2I(H2I), C2J(H2J), C20(H20), C2M(H2M), C2P(H2P), C2R(H2R), C2T(H2T), C2V(H2V)
2.c Idealised Me refined as rotating group:
 C2X(H2XA,H2XB,H2XC), C2Z(H2ZA,H2ZB,H2ZC), C30(H30A,H30B,H30C), C33(H33A,H33B,
 H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C)
;
_olex2_submission_original_sample_id 5-133_7
_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 1.415
_oxdiff_exptl_absorpt_empirical_full_min 0.673