Water-tunable solvatochromic and nanoaggregate fluorescence: dual colour visualisation and quantification of trace water in tetrahydrofuran.
Tanioka, Masaru; Kamino, Shinichiro; Muranaka, Atsuya; Shirasaki, Yoshinao; Ooyama, Yousuke; Ueda, Masashi; Uchiyama, Masanobu; Enomoto, Shuichi; Sawada, Daisuke; Physical chemistry chemical physics : PCCP 19 (2017) 1209–1216; doi:10.1039/c6cp06808a

data_7227091
_publ_section_title
;
 Water-tunable solvatochromic and nanoaggregate fluorescence: dual colour
 visualisation and quantification of trace water in tetrahydrofuran.
;
_journal_issue                   2
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              1209
_journal_page_last               1216
_journal_paper_doi               10.1039/c6cp06808a
_journal_volume                  19
_journal_year                    2017
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C46 H36 N2 O6, 1.5(C H Cl3)'
_chemical_formula_sum            'C47.5 H37.5 Cl4.5 N2 O6'
_chemical_formula_weight         891.86
_chemical_name_systematic        trans-ABPX103
_chemical_properties_physical    ', Light-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2016-06-28 deposited with the CCDC.
2016-11-11 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 93.387(6)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   9.374(7)
_cell_length_b                   35.90(3)
_cell_length_c                   12.405(9)
_cell_measurement_reflns_used    8300
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.00
_cell_volume                     4167(6)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r16'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r16'
_computing_molecular_graphics    'CrystalStructure 4.2'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_structure_refinement  'SHELXL Version 2013/4 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            37634
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.417
_diffrn_reflns_theta_min         3.026
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.369
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1844.00
_exptl_crystal_preparation       ', Luminescent'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.39
_refine_diff_density_min         -0.41
_refine_ls_abs_structure_details
;
 Flack x determined using 4298 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.47(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1081
_refine_ls_number_reflns         18238
_refine_ls_number_restraints     1929
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0761
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0303P)^2^+3.3833P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1363
_reflns_Friedel_coverage         0.904
_reflns_Friedel_fraction_full    0.948
_reflns_Friedel_fraction_max     0.928
_reflns_number_gt                13826
_reflns_number_total             18238
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c6cp06808a3.cif
_cod_data_source_block           279_0419a
_cod_depositor_comments
;
         Adding full bibliography for 7227091.cif.

2017-11-19
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     'C95 H75 Cl9 N4 O12'
_cod_original_formula_sum        'C95 H75 Cl9 N4 O12'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1783.73
_cod_database_code               7227091
_shelxl_version_number           2013-4
_shelx_res_checksum              97003
_shelx_hkl_checksum              89087
_solvent_exptl_crystal_recrystallization_method chloroform