Synthesis, characterization and photophysical properties of cyclotriphosphazenes including heterocyclic rings
İbişoğlu, Hanife; Erdemir, Eda; Atilla, Devrim; Zorlu, Yunus; Şenkuytu, Elif; Inorganica Chimica Acta 498 (2019) 119120–; doi:10.1016/j.ica.2019.119120

data_1565738
_publ_section_title
;
 Synthesis, characterization and photophysical properties of
 cyclotriphosphazenes including heterocyclic rings
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119120
_journal_paper_doi               10.1016/j.ica.2019.119120
_journal_volume                  498
_journal_year                    2019
_chemical_formula_moiety         'C24 H20 N11 O2 P3, C4 H8 O'
_chemical_formula_sum            'C28 H28 N11 O3 P3'
_chemical_formula_weight         659.52
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.5764(6)
_cell_length_b                   18.2189(12)
_cell_length_c                   35.880(2)
_cell_measurement_reflns_used    4035
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.14
_cell_measurement_theta_min      2.41
_cell_volume                     6260.0(7)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.1542
_diffrn_reflns_av_unetI/netI     0.1302
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            35950
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.135
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.241
_exptl_absorpt_correction_T_max  0.7075
_exptl_absorpt_correction_T_min  0.6065
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0943 before and 0.0732 after correction.
The Ratio of minimum to maximum transmission is 0.8572.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       plate
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.164
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         5467
_refine_ls_number_restraints     611
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1647
_refine_ls_R_factor_gt           0.0726
_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^)+(0.0810P)^2^+2.9717P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1633
_refine_ls_wR_factor_ref         0.2026
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2663
_reflns_number_total             5467
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            2.cif
_cod_data_source_block           19gtu095_1187646_a1_eda_0ma_a_pl
_cod_database_code               1565738
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O3-C25 \\sim O3A-C25A
 with sigma of 0.02
 O3-C28 \\sim O3A-C28A
 with sigma of 0.02
 C25-C26 \\sim C25A-C26A
 with sigma of 0.02
 C26-C27 \\sim C26A-C27A
 with sigma of 0.02
 C27-C28 \\sim C27A-C28A
 with sigma of 0.02
 O3-C26 \\sim O3A-C26A
 with sigma of 0.04
 O3-C27 \\sim O3A-C27A
 with sigma of 0.04
 C25-C27 \\sim C25A-C27A
 with sigma of 0.04
 C25-C28 \\sim C25A-C28A
 with sigma of 0.04
 C26-C28 \\sim C26A-C28A
 with sigma of 0.04
 P2-N6 \\sim P2-N6A
 with sigma of 0.02
 N6-C24 \\sim N6A-C24A
 with sigma of 0.02
 N6-C22 \\sim N6A-C22A
 with sigma of 0.02
 N7-C24 \\sim N7A-C24A
 with sigma of 0.02
 N7-C23 \\sim N7A-C23A
 with sigma of 0.02
 C22-C23 \\sim C22A-C23A
 with sigma of 0.02
 P2-C24 \\sim P2-C24A
 with sigma of 0.04
 P2-C22 \\sim P2-C22A
 with sigma of 0.04
 N6-N7 \\sim N6A-N7A
 with sigma of 0.04
 N6-C23 \\sim N6A-C23A
 with sigma of 0.04
 N7-C22 \\sim N7A-C22A
 with sigma of 0.04
 C24-C22 \\sim C24A-C22A
 with sigma of 0.04
 C24-C23 \\sim C24A-C23A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.005 and
sigma for terminal atoms of 0.08
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.005 and
sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 N6, N7, C22, C23, C24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N6A, N7A, C22A, C23A, C24A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O3A)=Sof(C25A)=Sof(H25C)=Sof(H25D)=Sof(C26A)=Sof(H26C)=Sof(H26D)=
 Sof(C27A)=Sof(H27C)=Sof(H27D)=Sof(C28A)=Sof(H28C)=Sof(H28D)=1-FVAR(1)
 Sof(O3)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C27)=
 Sof(H27A)=Sof(H27B)=Sof(C28)=Sof(H28A)=Sof(H28B)=FVAR(1)
 Sof(N6A)=Sof(N7A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=
 1-FVAR(2)
 Sof(N6)=Sof(N7)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C25A(H25C,
 H25D), C26A(H26C,H26D), C27A(H27C,H27D), C28A(H28C,H28D)
6.b Aromatic/amide H refined with riding coordinates:
 C0AA(H0AA), C2(H2), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11),
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20),
  C21(H21), C22(H22), C23(H23), C24(H24), C22A(H22A), C23A(H23A), C24A(H24A)
;