Efficient cascade reactions for luminescent pyrylium biolabels catalysed by light rare-earth elements
Wang, Guangming; Li, Xun; Wang, Xuepu; Zhang, Kaka; New Journal of Chemistry 45 (2021) 12305–12310; doi:10.1039/D1NJ01793D

data_7060779
_publ_section_title
;
 Efficient cascade reactions for luminescent pyrylium biolabels catalysed
 by light rare-earth elements
;
_journal_issue                   27
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              12305
_journal_page_last               12310
_journal_paper_doi               10.1039/D1NJ01793D
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C F3 O3 S, C20 H19 O3'
_chemical_formula_sum            'C21 H19 F3 O6 S'
_chemical_formula_weight         456.443
_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_Int_Tables_number      2
_audit_creation_date             2021-05-11
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2021.04.12 svn.r67f51adf for OlexSys, GUI svn.r6225)
;
_audit_update_record
;
2021-05-20 deposited with the CCDC.	2021-06-07 downloaded from the CCDC.
;
_cell_angle_alpha                100.873(14)
_cell_angle_beta                 105.640(13)
_cell_angle_gamma                95.465(14)
_cell_formula_units_Z            2
_cell_length_a                   8.291(3)
_cell_length_b                   10.898(5)
_cell_length_c                   11.966(5)
_cell_measurement_reflns_used    1041
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      53.155
_cell_measurement_theta_min      4.661
_cell_volume                     1010.2(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      192.99
_diffrn_measured_fraction_theta_full 0.9679
_diffrn_measured_fraction_theta_max 0.9679
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1021
_diffrn_reflns_av_unetI/netI     0.1739
_diffrn_reflns_Laue_measured_fraction_full 0.9679
_diffrn_reflns_Laue_measured_fraction_max 0.9679
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8367
_diffrn_reflns_point_group_measured_fraction_full 0.9679
_diffrn_reflns_point_group_measured_fraction_max 0.9679
_diffrn_reflns_theta_full        24.9997
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    0.225
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             472.594
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.6345
_refine_diff_density_min         -0.6865
_refine_diff_density_rms         0.1572
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             8.7348
_refine_ls_goodness_of_fit_ref   1.1188
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    44
_refine_ls_number_parameters     328
_refine_ls_number_reflns         3432
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.1073
_refine_ls_R_factor_all          0.1823
_refine_ls_R_factor_gt           0.0905
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1025P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2011
_refine_ls_wR_factor_ref         0.2641
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                1679
_reflns_number_total             3432
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1nj01793d2.cif
_cod_data_source_block           mo_d8v20371_0m
_cod_depositor_comments          'Adding full bibliography for 7060779.cif.'
_cod_original_cell_volume        1010.2(8)
_cod_database_code               7060779
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C6, O7}
{O2, C1A}
3. Restrained distances
 C16-O3 \\sim C16-O3A
 with sigma of 0.02
 O3-C19 \\sim O3A-C19A
 with sigma of 0.02
 C16-C19 \\sim C16-C19A
 with sigma of 0.04
 F1-F3 \\sim F1A-F3A
 with sigma of 0.04
 S1-O5 \\sim S1A-O5A
 with sigma of 0.02
 S1-O6 \\sim S1A-O6A
 with sigma of 0.02
 S1-C21 \\sim S1A-C21A
 with sigma of 0.02
 O4-O5 \\sim O4A-O5A
 with sigma of 0.04
 O4-C21 \\sim O4A-C21A
 with sigma of 0.04
 O5-C21 \\sim O5A-C21A
 with sigma of 0.04
 F1-C21 \\sim F1A-C21A
 with sigma of 0.02
 F2-C21 \\sim F2A-C21A
 with sigma of 0.02
 S1-O4 \\sim S1A-O4A
 with sigma of 0.02
 F1-F2 \\sim F1A-F2A
 with sigma of 0.04
 F2-F3 \\sim F2A-F3A
 with sigma of 0.04
 O4-O6 \\sim O4A-O6A
 with sigma of 0.04
 O5-O6 \\sim O5A-O6A
 with sigma of 0.04
 O6-C21 \\sim O6A-C21A
 with sigma of 0.04
 S1-F1 \\sim S1A-F1A
 with sigma of 0.04
 S1-F2 \\sim S1A-F2A
 with sigma of 0.04
 S1-F3 \\sim S1A-F3A
 with sigma of 0.04
 F3-C21 \\sim F3A-C21A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C6) = Uanis(O7)
Uanis(O2) = Uanis(C1A)
5. Rigid body (RIGU) restrains
 C16, O3, C19, O3A, C19A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Others
 Sof(O7)=Sof(C1A)=Sof(H1A)=Sof(O3A)=Sof(C19A)=Sof(H19d)=Sof(H19e)=Sof(H19f)=1-
 FVAR(1)
 Sof(O2)=Sof(C6)=Sof(H6)=Sof(O3)=Sof(C19)=Sof(H19a)=Sof(H19b)=Sof(H19c)=FVAR(1)
 Sof(C21A)=Sof(S1A)=Sof(O4A)=Sof(O5A)=Sof(O6A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=1-
 FVAR(2)
 Sof(S1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(O4)=Sof(O5)=Sof(O6)=Sof(C21)=FVAR(2)
 Fixed Uiso: C21A(0.08) S1A(0.08) O4A(0.08) O5A(0.08) O6A(0.08) F1A(0.08)
 F2A(0.08) F3A(0.08)
7.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14), C15(H15),
 C17(H17), C18(H18), C1A(H1A)
7.b Idealised Me refined as rotating group:
 C2(H2a,H2b,H2c), C20(H20a,H20b,H20c), C19(H19a,H19b,H19c), C19A(H19d,H19e,H19f)
;
_olex2_submission_special_instructions 'No special instructions were received'