Luminescent solvent-free liquids based on Schiff-base boron difluoride complexes with polyethylene glycol chains.
Ikeshita, Masahiro; Ichinose, Miku; Tsuno, Takashi; Soft matter 20 (2024) 2178–2184; doi:10.1039/d3sm01590d

data_1570936
_publ_section_title
;
 Luminescent solvent-free liquids based on Schiff-base boron difluoride
 complexes with polyethylene glycol chains.
;
_journal_issue                   9
_journal_name_full               'Soft matter'
_journal_page_first              2178
_journal_page_last               2184
_journal_paper_doi               10.1039/d3sm01590d
_journal_volume                  20
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C14 H14 B F2 N O2'
_chemical_formula_sum            'C14 H14 B F2 N O2'
_chemical_formula_weight         277.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-05
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-09-28 deposited with the CCDC.	2024-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.467(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7885(11)
_cell_length_b                   12.1016(11)
_cell_length_c                   8.5117(9)
_cell_measurement_reflns_used    2642
_cell_measurement_temperature    113.15
_cell_measurement_theta_max      30.1900
_cell_measurement_theta_min      2.3840
_cell_volume                     1269.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      113.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.953
_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    -14.00  91.00   0.50    0.50    --   20.00  54.00 150.00  210
  2  \w    -74.00 -42.00   0.50    0.50    --   20.00  54.00-120.00   64
  3  \w    -26.00  63.00   0.50    0.50    --   20.00  54.00-120.00  178
  4  \w    -65.00  98.00   0.50    0.50    --   20.00  54.00 -90.00  326
  5  \w    -58.00 -33.00   0.50    0.50    --   20.00  54.00  30.00   50
  6  \w      1.00  26.00   0.50    0.50    --   20.00  54.00  30.00   50
  7  \w     58.00  83.00   0.50    0.50    --   20.00  54.00  30.00   50
  8  \w    -67.00 -42.00   0.50    0.50    --   20.00  54.00 150.00   50
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II (JP)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0077565000
_diffrn_orient_matrix_UB_12      -0.0572897000
_diffrn_orient_matrix_UB_13      0.0104023000
_diffrn_orient_matrix_UB_21      -0.0555427000
_diffrn_orient_matrix_UB_22      0.0054012000
_diffrn_orient_matrix_UB_23      -0.0427125000
_diffrn_orient_matrix_UB_31      0.0128780000
_diffrn_orient_matrix_UB_32      -0.0110686000
_diffrn_orient_matrix_UB_33      -0.0745148000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5208
_diffrn_reflns_point_group_measured_fraction_full 0.845
_diffrn_reflns_point_group_measured_fraction_max 0.737
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.409
_diffrn_reflns_theta_min         2.359
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.115
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63317
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.81a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_preparation       CH2Cl2/EtOH
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.171
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details
;
 Flack x determined using 824 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.2(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2822
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0651P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1013
_reflns_Friedel_coverage         0.543
_reflns_Friedel_fraction_full    0.689
_reflns_Friedel_fraction_max     0.520
_reflns_number_gt                2513
_reflns_number_total             2822
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sm01590d2.cif
_cod_data_source_block           exp_1045_auto
_cod_depositor_comments
'Adding full bibliography for 1570934--1570937.cif.'
_cod_database_code               1570936
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C14H14BF2NO2
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C00H(H00I,H00J)
1.b Aromatic/amide H refined with riding coordinates:
 C00A(H00A), C00B(H00B), C00C(H00C), C00E(H00F), C00F(H00G), C00G(H00H),
 C00I(H00K)
1.c Idealised Me refined as rotating group:
 C00J(H00L,H00M,H00N)
;
_shelx_res_checksum              54422
_shelx_hkl_checksum              57106
_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 1.647
_oxdiff_exptl_absorpt_empirical_full_min 0.708