A difluoroboron β-diketonate based thermometer with temperature-dependent emission wavelength.
Wang, Jian-Xin; Yu, Yi-Shuai; Niu, Li-Ya; Zou, Bo; Wang, Kai; Yang, Qing-Zheng; Chemical communications (Cambridge, England) 56 (2020) 6269–6272; doi:10.1039/d0cc01505a

data_7126440
_publ_section_title
;
 A difluoroboron \b-diketonate based thermometer with
 temperature-dependent emission wavelength.
;
_journal_issue                   46
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6269
_journal_page_last               6272
_journal_paper_doi               10.1039/d0cc01505a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C24 H29 B F2 O3'
_chemical_formula_sum            'C24 H29 B F2 O3'
_chemical_formula_weight         414.28
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-11-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-25 deposited with the CCDC.	2020-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                70.258(5)
_cell_angle_beta                 78.911(5)
_cell_angle_gamma                79.039(5)
_cell_formula_units_Z            4
_cell_length_a                   10.1611(6)
_cell_length_b                   15.2065(9)
_cell_length_c                   16.1543(9)
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    299.99(10)
_cell_measurement_theta_max      29.1470
_cell_measurement_theta_min      2.3290
_cell_volume                     2284.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.29a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29a (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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      299.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.901
_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     46.00  72.00   0.50    4.00    --  -15.70  57.00 120.00   52
  2  \w    -57.00 -10.00   0.50    4.00    --  -15.70  77.00 -30.00   94
  3  \w    -57.00 -17.00   0.50    4.00    --  -15.70  77.00-120.00   80
  4  \w    -35.00  32.00   0.50    4.00    --  -15.70  57.00 -30.00  134
  5  \w    -56.00 -25.00   0.50    4.00    --  -15.70  77.00  60.00   62
  6  \w    -49.00  30.00   0.50    4.00    --  -15.70  57.00 120.00  158
  7  \w    -14.00  12.00   0.50    4.00    --   15.80  71.00-125.48   52
  8  \w    -18.00 105.00   0.50    4.00    --   15.80  57.00-150.00  246
  9  \w     14.00  81.00   0.50    4.00    --   15.80  57.00  30.00  134
 10  \w     35.00  83.00   0.50    4.00    --   15.80  71.00-125.48   96
 11  \w     35.00 102.00   0.50    4.00    --   15.80  57.00  90.00  134
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0199016000
_diffrn_orient_matrix_UB_12      -0.0307926000
_diffrn_orient_matrix_UB_13      0.0409016000
_diffrn_orient_matrix_UB_21      -0.0613215000
_diffrn_orient_matrix_UB_22      -0.0196601000
_diffrn_orient_matrix_UB_23      0.0100545000
_diffrn_orient_matrix_UB_31      0.0315950000
_diffrn_orient_matrix_UB_32      -0.0341636000
_diffrn_orient_matrix_UB_33      -0.0210902000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0189
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.901
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31152
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.473
_diffrn_reflns_theta_min         2.061
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75934
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         11427
_refine_ls_number_restraints     334
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0622
_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^)+(0.0956P)^2^+0.3469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1754
_refine_ls_wR_factor_ref         0.1933
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7606
_reflns_number_total             11427
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc01505a2.cif
_cod_data_source_block           300k
_cod_depositor_comments
'Adding full bibliography for 7126433--7126447.cif.'
_cod_database_code               7126440
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C24 H29 B F2 O3'
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.966
_reflns_odcompleteness_completeness 90.13
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.41
_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. Restrained distances
 O6-C26 = O6A-C26
 1.36 with sigma of 0.02
 O6-C25 = O6A-C25A
 1.43 with sigma of 0.02
 C43A-C41A = C44-C41 = C44A-C41A = C43-C41 = C42A-C41A = C42-C41
 1.54 with sigma of 0.02
 C22A-C21 = C22-C21 = C23A-C21 = C23-C21 = C24A-C21 = C24-C21
 1.54 with sigma of 0.02
 C46A-C45 = C46-C45 = C47-C45 = C47A-C45 = C48-C45 = C48A-C45
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O6A \\sim C25A \\sim O6 \\sim C25: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.01
C44 \\sim C44A \\sim C43A \\sim C41A \\sim C41 \\sim C43 \\sim C42 \\sim C42A:
within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01
C23 \\sim C23A \\sim C22 \\sim C22A \\sim C24 \\sim C24A: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.01
C47A \\sim C47 \\sim C46A \\sim C46 \\sim C48A \\sim C48: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O6) \\sim Ueq, Uanis(O6A) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C25A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C44A) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C41A) \\sim Ueq, Uanis(C41)
\\sim Ueq, Uanis(C43A) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C42) \\sim Ueq,
Uanis(C42A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C23) \\sim Ueq, Uanis(C23A) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C22A)
\\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C24A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.01
Uanis(C48) \\sim Ueq, Uanis(C48A) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C46A)
\\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C47A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.01
4. Others
 Sof(O6A)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(1)
 Sof(O6)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(1)
 Sof(C43A)=Sof(H43D)=Sof(H43E)=Sof(H43F)=Sof(C42A)=Sof(H42D)=Sof(H42E)=
 Sof(H42F)=Sof(C44A)=Sof(H44D)=Sof(H44E)=Sof(H44F)=Sof(C41A)=1-FVAR(2)
 Sof(C41)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=Sof(C43)=Sof(H43A)=Sof(H43B)=
 Sof(H43C)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=FVAR(2)
 Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C24A)=Sof(H24D)=Sof(H24E)=
 Sof(H24F)=Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(3)
 Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(3)
 Sof(C46A)=Sof(H46D)=Sof(H46E)=Sof(H46F)=Sof(C47A)=Sof(H47D)=Sof(H47E)=
 Sof(H47F)=Sof(C48A)=Sof(H48D)=Sof(H48E)=Sof(H48F)=1-FVAR(4)
 Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=
 Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=FVAR(4)
5.a Me refined with riding coordinates:
 C22(H22A,H22B,H22C)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C7(H7), C9(H9), C12(H12), C14(H14), C16(H16),
 C27(H27), C28(H28), C29(H29), C31(H31), C33(H33), C36(H36), C38(H38), C40(H40)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C42(H42A,
 H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C),
 C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C25A(H25D,H25E,H25F), C43A(H43D,H43E,
 H43F), C42A(H42D,H42E,H42F), C44A(H44D,H44E,H44F), C23A(H23D,H23E,H23F),
 C24A(H24D,H24E,H24F), C22A(H22D,H22E,H22F), C46A(H46D,H46E,H46F), C47A(H47D,
 H47E,H47F), C48A(H48D,H48E,H48F)
;
_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 1.345
_oxdiff_exptl_absorpt_empirical_full_min 0.685