Differences in solubilities, crystal structures, NMR spectra and fluorescence emissions induced by potassium cation/benzo-21-crown-7 molecular recognition
Ouyang, Yunyun; Zhang, Yi; Luo, Zheng; Li, Xing; Duan, Abing; Dong, Shengyi; New Journal of Chemistry 43 (2019) 14299–; doi:10.1039/C9NJ03208H

data_7058750
_publ_section_title
;
 Differences in solubilities, crystal structures, NMR spectra and
 fluorescence emissions induced by potassium cation/benzo-21-crown-7
 molecular recognition
;
_journal_issue                   36
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14299
_journal_paper_doi               10.1039/C9NJ03208H
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C23 H24.5 K N O9, F6 P'
_chemical_formula_sum            'C23 H24.5 F6 K N O9 P'
_chemical_formula_weight         643.00
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-04-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-14 deposited with the CCDC.    2019-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.509(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5206(11)
_cell_length_b                   14.1906(12)
_cell_length_c                   15.6156(16)
_cell_measurement_reflns_used    9168
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.57
_cell_volume                     2747.4(4)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23869
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.669
_diffrn_reflns_theta_min         2.181
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.344
_exptl_absorpt_correction_T_max  0.842
_exptl_absorpt_correction_T_min  0.759
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       cube
_exptl_crystal_F_000             1318
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.993
_refine_diff_density_min         -1.005
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         6368
_refine_ls_number_restraints     379
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1373
_refine_ls_R_factor_gt           0.1110
_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^)+(0.1555P)^2^+9.4321P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2996
_refine_ls_wR_factor_ref         0.3214
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4700
_reflns_number_total             6368
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj03208h2.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 7058749--7058750.cif.'
_cod_original_formula_sum        'C23 H24.50 F6 K N O9 P'
_cod_database_code               7058750
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.847
_shelx_estimated_absorpt_t_min   0.771
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H) groups
2. Rigid bond restraints
 C1, C0AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
C00B \\sim C00C \\sim C00D \\sim C00E \\sim C00F \\sim C00G \\sim C00H \\sim
C00I \\sim C00K \\sim C00M \\sim C00P \\sim C00R \\sim C00S \\sim C00T \\sim
C00V \\sim C00W \\sim C00X \\sim C00Z \\sim C011 \\sim C014 \\sim C0 \\sim C1
\\sim C0AA \\sim C15: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Others
 Sof(H00V)=Sof(O0)=1-FVAR(1)
 Sof(O010)=FVAR(1)
 Sof(C0)=Sof(H0)=Sof(H15)=1-FVAR(2)
 Sof(C014)=Sof(H01C)=Sof(H01D)=Sof(H15A)=Sof(H15B)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C00M(H00A,H00B), C00P(H00D,H00E), C00R(H00G,H00J), C00T(H00K,H00L), C00X(H00M,
 H00N), C00Z(H00O,H00P), C011(H01A,H01B), C014(H01C,H01D), C15(H15A,H15B)
5.b Aromatic/amide H refined with riding coordinates:
 C00C(H00C), C00F(H00F), C00H(H00H), C00I(H00I), C00S(H00S), C00V(H00V),
 C00W(H00W), C0(H0), C0AA(H0AA), C15(H15)
;
_shelx_res_checksum              18950
_olex2_submission_special_instructions 'No special instructions were received'