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_7126438
_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     dual
_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                70.326(4)
_cell_angle_beta                 79.384(4)
_cell_angle_gamma                77.847(4)
_cell_formula_units_Z            4
_cell_length_a                   10.1293(6)
_cell_length_b                   14.9169(7)
_cell_length_c                   16.0997(7)
_cell_measurement_reflns_used    12950
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      29.1510
_cell_measurement_theta_min      2.3350
_cell_volume                     2222.2(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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.902
_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      0.0167048000
_diffrn_orient_matrix_UB_12      -0.0336277000
_diffrn_orient_matrix_UB_13      0.0412762000
_diffrn_orient_matrix_UB_21      -0.0611885000
_diffrn_orient_matrix_UB_22      -0.0185327000
_diffrn_orient_matrix_UB_23      0.0056974000
_diffrn_orient_matrix_UB_31      0.0344500000
_diffrn_orient_matrix_UB_32      -0.0338105000
_diffrn_orient_matrix_UB_33      -0.0220597000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.902
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30305
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.902
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.479
_diffrn_reflns_theta_min         2.072
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81866
_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    1.238
_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         0.450
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         11160
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0768P)^2^+0.5100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1401
_refine_ls_wR_factor_ref         0.1487
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8874
_reflns_number_total             11160
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc01505a2.cif
_cod_data_source_block           200k
_cod_depositor_comments
'Adding full bibliography for 7126433--7126447.cif.'
_cod_database_code               7126438
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C24 H29 B F2 O3'
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.965
_reflns_odcompleteness_completeness 90.25
_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. Uiso/Uaniso restraints and constraints
O6A \\sim O6 \\sim C25A \\sim C25: 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 0.02
3. 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)
4.a 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)
4.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), 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)
;
_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 1.290
_oxdiff_exptl_absorpt_empirical_full_min 0.680