Thiazole substituted dispiromonoansa and monospiro cyclotriphosphazenes: Design, synthesis and biological activity
Yenilmez Çiftçi, Gönül; Tanrıverdi Eçik, Esra; Goler, Omer; Yuksel, Fatma; Duygulu, Ercan; Donbaloglu, Fadime; Turhal, Gulseren; Demiroglu-Zergeroglu, Asuman; Inorganica Chimica Acta 498 (2019) 119158–; doi:10.1016/j.ica.2019.119158

data_1565778
_publ_section_title
;
 Thiazole substituted dispiromonoansa and monospiro cyclotriphosphazenes:
 Design, synthesis and biological activity
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119158
_journal_paper_doi               10.1016/j.ica.2019.119158
_journal_volume                  498
_journal_year                    2019
_chemical_formula_moiety         'C26 H34 N9 O2 P3 S2'
_chemical_formula_sum            'C26 H34 N9 O2 P3 S2'
_chemical_formula_weight         661.65
_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
_cell_angle_alpha                79.634(6)
_cell_angle_beta                 85.067(7)
_cell_angle_gamma                71.749(7)
_cell_formula_units_Z            2
_cell_length_a                   10.0646(10)
_cell_length_b                   10.5825(10)
_cell_length_c                   15.2015(13)
_cell_measurement_reflns_used    2545
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      21.96
_cell_measurement_theta_min      2.27
_cell_volume                     1511.8(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      299.47
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0471
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13197
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.362
_exptl_absorpt_coefficient_mu    0.378
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_description       block
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.119
_refine_diff_density_max         0.232
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         5218
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+0.8194P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1010
_refine_ls_wR_factor_ref         0.1147
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3679
_reflns_number_total             5218
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2019-498-119158.cif
_cod_data_source_block           18gtu128_omg_06_0m
_cod_database_code               1565778
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.950
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H4-N4
 0.89 with sigma of 0.02
 H6-N6
 0.89 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B)
3.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C18(H18), C20(H20), C21(H21), C26(H26)
3.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              59350