Cyclic phosphazene derivatives combined with two different forms of the phenol-pyrazole group: synthesis, spectroscopic and crystallographic characterization and stereochemical properties
Mutlu Balcı, Ceylan; Palabıyık, Duygu; Beşli, Serap; New Journal of Chemistry 49 (2025) 9583–9599; doi:10.1039/D5NJ01321F

data_7063813
_publ_section_title
;
 Cyclic phosphazene derivatives combined with two different forms of the
 phenol-pyrazole group: synthesis, spectroscopic and crystallographic
 characterization and stereochemical properties
;
_journal_issue                   23
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              9583
_journal_page_last               9599
_journal_paper_doi               10.1039/D5NJ01321F
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'C18 H12 Cl2 N7 O2 P3'
_chemical_formula_sum            'C18 H12 Cl2 N7 O2 P3'
_chemical_formula_weight         522.16
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-02-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2025-03-03 deposited with the CCDC.	2025-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                100.8770(10)
_cell_angle_beta                 95.2510(10)
_cell_angle_gamma                90.9090(10)
_cell_formula_units_Z            4
_cell_length_a                   7.8000(5)
_cell_length_b                   14.4899(9)
_cell_length_c                   19.0386(12)
_cell_measurement_reflns_used    9605
_cell_measurement_temperature    172.16
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      2.38
_cell_volume                     2103.0(2)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      172.16
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0244
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24035
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         1.432
_exptl_absorpt_coefficient_mu    0.571
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6902
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0793 before and 0.0367 after correction.
The Ratio of minimum to maximum transmission is 0.9257.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_description       plate
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.184
_exptl_crystal_size_mid          0.161
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         9622
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0414P)^2^+1.2781P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0889
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8101
_reflns_number_total             9622
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj01321f2.cif
_cod_data_source_block           21gtu29_cpy_01_2_0m
_cod_depositor_comments
'Adding full bibliography for 7063812--7063815.cif.'
_cod_database_code               7063813
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.902
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C20(H20), C5(H5), C2(H2), C8(H8), C7(H7), C35(H35), C17(H17),
 C19(H19), C11(H11), C6(H6), C32(H32), C10(H10), C14(H14), C23(H23), C26(H26),
 C33(H33), C15(H15), C29(H29), C34(H34), C16(H16), C25(H25), C28(H28), C24(H24)
;
_shelx_res_checksum              30315
_shelx_hkl_checksum              62624
_olex2_submission_special_instructions 'No special instructions were received'