Phosphorus-Nitrogen Compounds. Part 24. Syntheses, Crystal Structures, Spectroscopic and Stereogenic Properties, Biological Activities, and DNA Interactions of Novel Spiro-ansa-spiro- and Ansa-spiro-ansa-cyclotetraphosphazenes
Gamze Elmas; Aytuğ Okumuş; Zeynel Kiliç; Tuncer Hökelek; Leyla Açik; Hakan Dal; Nagehan Ramazanoğlu; L.Yasemin Koç; Inorganic Chemistry 51 (2012) 12841–12856; doi:10.1021/ic3017134

data_4331159
_publ_section_title
;
 Phosphorus-Nitrogen Compounds. Part 24. Syntheses, Crystal Structures,
 Spectroscopic and Stereogenic Properties, Biological Activities, and DNA
 Interactions of Novel Spiro-ansa-spiro- and
 Ansa-spiro-ansa-cyclotetraphosphazenes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12841
_journal_page_last               12856
_journal_paper_doi               10.1021/ic3017134
_journal_volume                  51
_journal_year                    2012
_chemical_absolute_configuration 'determined reliably'
_chemical_formula_moiety         'C17 H18 Cl4 N6 O2 P4'
_chemical_formula_sum            'C17 H18 Cl4 N6 O2 P4'
_chemical_formula_weight         604.05
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9387(3)
_cell_length_b                   11.7933(3)
_cell_length_c                   20.7778(6)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.68
_cell_volume                     2435.37(12)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Bruker Kappa APEXII CCD area-detector diffractometer'
_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  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            12665
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    0.779
_exptl_absorpt_correction_T_max  0.8000
_exptl_absorpt_correction_T_min  0.7407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_description       prism
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
'Flack H D (1983) with 2563 Friedel pairs measured'
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5984
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0217
_refine_ls_R_factor_gt           0.0210
_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^)+(0.0282P)^2^+0.5884P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0558
_reflns_number_gt                5850
_reflns_number_total             5984
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic3017134_si_005.cif
_cod_data_source_block           ag23_0m
_cod_database_code               4331159