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_1570937
_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_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           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-09-28 deposited with the CCDC.	2024-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.286(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.5191(14)
_cell_length_b                   6.0356(3)
_cell_length_c                   17.3921(9)
_cell_measurement_reflns_used    5756
_cell_measurement_temperature    113.15
_cell_measurement_theta_max      29.7200
_cell_measurement_theta_min      2.3630
_cell_volume                     2566.6(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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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 0.998
_diffrn_measured_fraction_theta_max 0.958
_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    -11.00  84.00   0.50    7.33    --   20.00  54.00  90.00  190
  2  \w    -73.00  40.00   0.50    7.33    --   20.00  54.00 -60.00  226
  3  \w     79.00 106.00   0.50    7.33    --   20.00  54.00 -60.00   54
  4  \w    -64.00 -39.00   0.50    7.33    --   20.00  54.00  30.00   50
  5  \w    -33.00  67.00   0.50    7.33    --   20.00  54.00  30.00  200
  6  \w     74.00  99.00   0.50    7.33    --   20.00  54.00  30.00   50
  7  \w    -49.00 104.00   0.50    7.33    --   20.00  54.00 -30.00  306
  8  \w     16.00  43.00   0.50    7.33    --   20.00  54.00  60.00   54
  9  \w    -61.00 -34.00   0.50    7.33    --   20.00  54.00-150.00   54
 10  \w      8.00  33.00   0.50    7.33    --   20.00  54.00-150.00   50
 11  \w    -57.00 -32.00   0.50    7.33    --   20.00  54.00  90.00   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      0.0285163000
_diffrn_orient_matrix_UB_12      0.0170750000
_diffrn_orient_matrix_UB_13      0.0075805000
_diffrn_orient_matrix_UB_21      -0.0034090000
_diffrn_orient_matrix_UB_22      0.0036448000
_diffrn_orient_matrix_UB_23      0.0401158000
_diffrn_orient_matrix_UB_31      0.0041241000
_diffrn_orient_matrix_UB_32      -0.1162074000
_diffrn_orient_matrix_UB_33      0.0023832000
_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  0.0373
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26908
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.394
_diffrn_reflns_theta_min         2.349
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82703
_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    1.434
_exptl_crystal_description       plate
_exptl_crystal_F_000             1152
_exptl_crystal_preparation       CH2Cl2/EtOH
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.275
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         7434
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0514
_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^)+(0.0554P)^2^+0.7761P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1197
_refine_ls_wR_factor_ref         0.1324
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5201
_reflns_number_total             7434
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sm01590d2.cif
_cod_data_source_block           exp_1050_autored
_cod_depositor_comments
'Adding full bibliography for 1570934--1570937.cif.'
_cod_database_code               1570937
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C14H14NO2BF2
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00T(H00A,H00B), C00V(H00C,H00D), C00Y(H00E,H00H), C010(H01A,H01B)
2.b Aromatic/amide H refined with riding coordinates:
 C00F(H00F), C00G(H00G), C00I(H00I), C00M(H00M), C00N(H00N), C00O(H00O),
 C00P(H00P), C00Q(H00Q), C00R(H00R), C00S(H00S), C00U(H00U), C00W(H00W),
 C00X(H00X), C00Z(H00Z)
2.c Idealised Me refined as rotating group:
 C013(H01C,H01D,H01E), C014(H01F,H01G,H01H)
;
_shelx_res_checksum              40229
_shelx_hkl_checksum              74699
_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 1.273
_oxdiff_exptl_absorpt_empirical_full_min 0.761