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_7126435
_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                74.405(7)
_cell_angle_beta                 86.917(7)
_cell_angle_gamma                66.543(8)
_cell_formula_units_Z            2
_cell_length_a                   8.5049(7)
_cell_length_b                   9.9575(9)
_cell_length_c                   15.6872(12)
_cell_measurement_reflns_used    5391
_cell_measurement_temperature    399.99(11)
_cell_measurement_theta_max      25.7930
_cell_measurement_theta_min      2.6990
_cell_volume                     1171.72(19)
_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      399.99(11)
_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      -0.0508857000
_diffrn_orient_matrix_UB_12      0.0327074000
_diffrn_orient_matrix_UB_13      -0.0404991000
_diffrn_orient_matrix_UB_21      0.0396707000
_diffrn_orient_matrix_UB_22      -0.0698887000
_diffrn_orient_matrix_UB_23      -0.0113533000
_diffrn_orient_matrix_UB_31      -0.0642803000
_diffrn_orient_matrix_UB_32      -0.0234484000
_diffrn_orient_matrix_UB_33      0.0210390000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0175
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.901
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15970
_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         29.446
_diffrn_reflns_theta_min         2.316
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72059
_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    1.174
_exptl_crystal_description       block
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         5853
_refine_ls_number_restraints     210
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0678
_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^)+(0.1335P)^2^+0.0892P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2202
_refine_ls_wR_factor_ref         0.2471
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3484
_reflns_number_total             5853
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc01505a2.cif
_cod_data_source_block           400k
_cod_depositor_comments
'Adding full bibliography for 7126433--7126447.cif.'
_cod_database_code               7126435
_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   0.967
_reflns_odcompleteness_completeness 90.09
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.38
_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
 C19A-C17 = C19-C17 = C20A-C17 = C20-C17 = C18A-C17 = C18-C17 = C24-C21 = C24A-
 C21A = C23-C21 = C22A-C21A = C22-C21 = C23A-C21A
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C19 \\sim C19A \\sim C20A \\sim C20 \\sim C18A \\sim C18: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.01
C23 \\sim C22A \\sim C21 \\sim C21A \\sim C22 \\sim C23A \\sim C24A \\sim C24:
within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20)
\\sim Ueq, Uanis(C18A) \\sim Ueq, Uanis(C20A) \\sim Ueq, Uanis(C19A) \\sim Ueq,
Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C23A)
\\sim Ueq, Uanis(C22A) \\sim Ueq, Uanis(C21A) \\sim Ueq, Uanis(C24) \\sim Ueq,
Uanis(C24A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
4. Others
 Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C20A)=Sof(H20D)=Sof(H20E)=
 Sof(H20F)=Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=1-FVAR(1)
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(1)
 Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C24A)=Sof(H24D)=Sof(H24E)=
 Sof(H24F)=Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=Sof(C21A)=1-FVAR(2)
 Sof(C21)=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(2)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C7(H7), C9(H9), C12(H12), C14(H14), C16(H16)
5.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C),
 C18A(H18D,H18E,H18F), C20A(H20D,H20E,H20F), C19A(H19D,H19E,H19F), C23A(H23D,
 H23E,H23F), C24A(H24D,H24E,H24F), C22A(H22D,H22E,H22F)
;
_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 1.348
_oxdiff_exptl_absorpt_empirical_full_min 0.660