Phosphorus–nitrogen compounds: part 70. Syntheses of tetraaminomono/bis(4-fluorobenzyl)spiro(N/N)cyclotriphosphazenes: structural characterization, Hirshfeld surface analysis and comparative evaluation of esterase activities of hCA I and hCA II isoenzymes
Okumuş, Aytuğ; Elmas, Gamze; Binici, Arzu; Tunca, Ekrem; Hökelek, Tuncer; Kılıç, Zeynel; New Journal of Chemistry 47 (2023) 8578–8588; doi:10.1039/D3NJ00721A

data_7062400
_publ_section_title
;
 Phosphorus--nitrogen compounds: part 70. Syntheses of
 tetraaminomono/bis(4-fluorobenzyl)spiro(N/N)cyclotriphosphazenes:
 structural characterization, Hirshfeld surface analysis and comparative
 evaluation of esterase activities of hCA I and hCA II isoenzymes
;
_journal_issue                   18
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8578
_journal_page_last               8588
_journal_paper_doi               10.1039/D3NJ00721A
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C57 H70 F2 N13 P3'
_chemical_formula_sum            'C57 H70 F2 N13 P3'
_chemical_formula_weight         1068.17
_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   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-03-24 deposited with the CCDC.	2023-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                70.249(2)
_cell_angle_beta                 76.527(3)
_cell_angle_gamma                82.934(4)
_cell_formula_units_Z            2
_cell_length_a                   9.7817(4)
_cell_length_b                   16.5352(5)
_cell_length_c                   18.3684(6)
_cell_measurement_reflns_used    5044
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.39
_cell_measurement_theta_min      2.23
_cell_volume                     2716.03(17)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2012)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2012)'
_computing_data_reduction        <i>SAINT</i>
_computing_molecular_graphics    '<i>ORTEP-3</i> for Windows (Farrugia, 2012)'
_computing_publication_material
'WinGX publication routines (Farrugia, 2012) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Bruker APEX II QUAZAR three-circle diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_unetI/netI     0.0709
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38355
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         1.468
_exptl_absorpt_coefficient_mu    0.168
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       plate
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.216
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.086
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.0018(3)
_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   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         11255
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0482P)^2^+1.1029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1270
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7203
_reflns_number_total             11255
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj00721a2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 7062400.cif.'
_cod_database_code               7062400
_shelx_shelxl_version_number     2018/3
_iucr_geom_hbonds_special_details
;
Cg7, Cg8, Cg10, Cg11 and Cg12 are the centroids, respectively, of the (C1---C6),
(C12---C17), (C32---C37), (C42---C47) and (C52---C57) benzene rings.
;
_shelx_res_checksum              95914