Novel paraben derivatives of tetracyclic spermine cyclotriphosphazenes: synthesis, characterization and biosensor based DNA interaction analysis
Kızılkaya, Perihan; Şenkuytu, Elif; Davarcı, Derya; Pala, Uğur; Ölçer, Zehra; Yenilmez Çiftçi, Gönül; New Journal of Chemistry 44 (2020) 18942–18953; doi:10.1039/D0NJ03908J

data_7060052
_publ_section_title
;
 Novel paraben derivatives of tetracyclic spermine cyclotriphosphazenes:
 synthesis, characterization and biosensor based DNA interaction analysis
;
_journal_issue                   43
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18942
_journal_page_last               18953
_journal_paper_doi               10.1039/D0NJ03908J
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C30 H44 N7 O6 P3'
_chemical_formula_sum            'C30 H44 N7 O6 P3'
_chemical_formula_weight         691.63
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-15 deposited with the CCDC.	2020-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                94.285(11)
_cell_angle_beta                 109.524(11)
_cell_angle_gamma                93.300(13)
_cell_formula_units_Z            2
_cell_length_a                   11.390(2)
_cell_length_b                   11.9524(19)
_cell_length_c                   13.398(2)
_cell_measurement_reflns_used    2492
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.11
_cell_measurement_theta_min      2.45
_cell_volume                     1707.7(5)
_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_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer QUAZAR mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0669
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10774
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         1.621
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.227
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       rod
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.409
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.0010(7)
_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   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         5876
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0558
_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^)+(0.0533P)^2^+1.1231P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1424
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4031
_reflns_number_total             5876
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj03908j2.cif
_cod_data_source_block           19gtu017_es_z_525_8a_0m
_cod_depositor_comments
'Adding full bibliography for 7060050--7060052.cif.'
_cod_database_code               7060052
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.913
_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,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C18-C19
 1.5 with sigma of 0.02
 C9-C10
 1.6 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C20
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C27(H27A,H27B), C25(H25A,H25B), C26(H26A,H26B), C21(H21A,
 H21B), C23(H23A,H23B), C28(H28A,H28B), C30(H30A,H30B), C22(H22A,H22B),
 C29(H29A,H29B), C18(H18A,H18B), C19(H19A,H19B), C8(H8A,H8B), C9(H9A,H9B)
4.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C15(H15), C2(H2), C16(H16), C6(H6), C3(H3), C5(H5)
4.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              52757
_olex2_submission_special_instructions 'No special instructions were received'