ESIPT on/off switching and crystallization-enhanced emission properties of new design phenol-pyrazole modified cyclotriphosphazenes
Mutlu Balcı, Ceylan; Tümay, Süreyya Oğuz; Beşli, Serap; New Journal of Chemistry 45 (2021) 8492–8505; doi:10.1039/D1NJ00894C

data_7060538
_publ_section_title
;
 ESIPT on/off switching and crystallization-enhanced emission properties
 of new design phenol-pyrazole modified cyclotriphosphazenes
;
_journal_issue                   19
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8492
_journal_page_last               8505
_journal_paper_doi               10.1039/D1NJ00894C
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C33 H22 N5 O5 P3, [+ solvents]'
_chemical_formula_sum            'C33 H22 N5 O5 P3'
_chemical_formula_weight         661.46
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-02-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-02-13 deposited with the CCDC.	2021-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 121.915(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.254(3)
_cell_length_b                   42.772(13)
_cell_length_c                   7.7060(19)
_cell_measurement_reflns_used    462
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      18.30
_cell_measurement_theta_min      2.42
_cell_volume                     3428.4(17)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1632
_diffrn_reflns_av_unetI/netI     0.2394
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7888
_diffrn_reflns_point_group_measured_fraction_full 0.687
_diffrn_reflns_point_group_measured_fraction_max 0.687
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         1.904
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.220
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4503
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1428 before and 0.0655 after correction.
The Ratio of minimum to maximum transmission is 0.6043.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_description       plate
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.213
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.203
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.3(2)
_refine_ls_extinction_coef       0.0036(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.886
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         4170
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      0.883
_refine_ls_R_factor_all          0.1953
_refine_ls_R_factor_gt           0.0647
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0253P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1539
_reflns_Friedel_coverage         0.399
_reflns_Friedel_fraction_full    0.394
_reflns_Friedel_fraction_max     0.394
_reflns_number_gt                1616
_reflns_number_total             4170
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj00894c2.cif
_cod_data_source_block           19gtu109_319_cd_02_2_zn_0m_a
_cod_depositor_comments
'Adding full bibliography for 7060537--7060538.cif.'
_cod_original_cell_volume        3428.3(17)
_cod_database_code               7060538
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.955
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C31 \\sim C32: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C25 \\sim C24: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C18 \\sim C17: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C12 \\sim C11: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C20 \\sim C21: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C5 \\sim C4: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
C25 \\sim C26: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C13 \\sim C12: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C30 \\sim C31: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
3.a Aromatic/amide H refined with riding coordinates:
 C29(H29), C32(H32), C14(H14), C17(H17), C30(H30), C31(H31), C8(H8), C12(H12),
 C23(H23), C24(H24), C2(H2), C25(H25), C20(H20), C18(H18), C11(H11), C26(H26),
 C19(H19), C1(H1), C13(H13), C5(H5), C7(H7), C6(H6)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 96 electrons were 
found in a volume of 614\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 
[+ solvents] per Formula Unit 
which account for 104 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              79697
_shelx_fab_checksum              86447
_olex2_submission_special_instructions 'No special instructions were received'