Phosphorus‒nitrogen compounds. Part 42. The comparative syntheses of 2-cis-4-ansa(N/O) and spiro(N/O) cyclotetraphosphazene derivatives: spectroscopic and crystallographic characterization, antituberculosis and cytotoxic activity studies
Binici, Arzu; Okumuş, Aytuğ; Elmas, Gamze; Kılıç, Zeynel; Ramazanoğlu, Nagehan; Açık, Leyla; Şimşek, Hülya; Çağdaş Tunalı, Beste; Türk, Mustafa; Güzel, Remziye; Hökelek, Tuncer; New Journal of Chemistry 43 (2019) 6856–; doi:10.1039/C9NJ00577C

data_7058307
_publ_section_title
;
 Phosphorus--nitrogen compounds. Part 42. The comparative syntheses of
 2-cis-4-ansa(N/O) and spiro(N/O) cyclotetraphosphazene derivatives:
 spectroscopic and crystallographic characterization, antituberculosis and
 cytotoxic activity studies
;
_journal_issue                   18
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              6856
_journal_paper_doi               10.1039/C9NJ00577C
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C14 H17 Cl6 Fe N5 O P4'
_chemical_formula_sum            'C14 H17 Cl6 Fe N5 O P4'
_chemical_formula_weight         663.76
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-08-24 deposited with the CCDC.    2019-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.192(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9606(4)
_cell_length_b                   11.0102(3)
_cell_length_c                   16.3482(5)
_cell_measurement_reflns_used    5483
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.35
_cell_measurement_theta_min      2.24
_cell_volume                     2487.22(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
'WinGX publication routines (Farrugia, 1999) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19186
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    1.528
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6228
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2005'
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.923
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5617
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0641P)^2^+2.9666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1209
_refine_ls_wR_factor_ref         0.1307
_reflns_number_gt                4559
_reflns_number_total             5617
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c9nj00577c2.cif
_cod_data_source_block           17gtu011_ansa3_0m
_cod_depositor_comments          'Adding full bibliography for 7058307.cif.'
_cod_original_cell_volume        2487.22(12)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7058307