Phosphorus‒nitrogen compounds. Part 54. syntheses of chiral amino-4-fluorobenzyl-spiro(N/O)cyclotriphosphazenes: structural and stereogenic properties
Mutlu, Ömer Faruk; Binici, Arzu; Okumuş, Aytuğ; Elmas, Gamze; Çoşut, Bünyemin; Kılıç, Zeynel; Hökelek, Tuncer; New Journal of Chemistry 45 (2021) 12178–12192; doi:10.1039/D1NJ00934F

data_7060715
_publ_section_title
;
 Phosphorus--nitrogen compounds. Part 54. syntheses of chiral
 amino-4-fluorobenzyl-spiro(N/O)cyclotriphosphazenes: structural and
 stereogenic properties
;
_journal_issue                   27
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              12178
_journal_page_last               12192
_journal_paper_doi               10.1039/D1NJ00934F
_journal_volume                  45
_journal_year                    2021
_chemical_formula_sum            'C16 H28 Cl2 F N6 O P3'
_chemical_formula_weight         503.25
_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-05-17 deposited with the CCDC.	2021-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                103.929(3)
_cell_angle_beta                 110.726(3)
_cell_angle_gamma                100.441(2)
_cell_formula_units_Z            2
_cell_length_a                   10.1879(3)
_cell_length_b                   10.2669(3)
_cell_length_c                   13.3549(4)
_cell_measurement_temperature    293(2)
_cell_volume                     1212.24(8)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
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_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15025
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         1.728
_exptl_absorpt_coefficient_mu    0.493
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.730
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         4288
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0539
_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^)+(0.0660P)^2^+1.1742P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1412
_refine_ls_wR_factor_ref         0.1508
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3509
_reflns_number_total             4288
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj00934f2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 7060715.cif.'
_cod_original_cell_volume        1212.24(7)
_cod_database_code               7060715
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.862
_shelx_estimated_absorpt_t_max   0.908
_shelx_res_checksum              52688