Structural and optical studies of fluoride ion binding using N-heteroaromatic ligands.
Angarkhe, Priyanka R.; Sahoo, Satyajit; Singhdeo, Simran; Shankar, Sr, Kripa; Upadhyay, Manav; Mahiya, Kuldeep; Tripathy, Jagnyaseni; Behera, Rakesh K.; Mohapatra, Swagat K.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 2069–2077; doi:10.1039/d4dt02857k

data_7717626
_publ_section_title
;
 Structural and optical studies of fluoride ion binding using
 N-heteroaromatic ligands.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2069
_journal_page_last               2077
_journal_paper_doi               10.1039/d4dt02857k
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C13 H10 N2 O2, C16 H36 N, F, 4(H2 O)'
_chemical_formula_sum            'C29 H54 F N3 O6'
_chemical_formula_weight         559.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-10-29
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-10-30 deposited with the CCDC.	2024-12-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.563(12)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.939(7)
_cell_length_b                   16.407(5)
_cell_length_c                   20.147(6)
_cell_measurement_reflns_used    7721
_cell_measurement_temperature    299.00
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.38
_cell_volume                     6591(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      299.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.2001
_diffrn_reflns_av_unetI/netI     0.1413
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            61333
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.256
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5478
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.2040 before and 0.0944 after correction.
The Ratio of minimum to maximum transmission is 0.7349.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.185
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.866
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     732
_refine_ls_number_reflns         11601
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.868
_refine_ls_R_factor_all          0.2421
_refine_ls_R_factor_gt           0.0776
_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^)+(0.0967P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1732
_refine_ls_wR_factor_ref         0.2229
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4095
_reflns_number_total             11601
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02857k2.cif
_cod_data_source_block           24domem_a_a
_cod_depositor_comments
'Adding full bibliography for 7717624--7717629.cif.'
_cod_database_code               7717626
_shelx_shelxl_version_number     2019/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O11-H11B
 0.84 with sigma of 0.02
3.a Riding coordinates:
 O4(H4), O3(H3), N5(H5), O2(H2), O1(H1), N2(H2A), O7(H7A,H7B)
3.b Free rotating group:
 O12(H12A,H12B), O9(H9A,H9B), O10(H10A,H10B), O11(H11A,H11B), O6(H6A,H6B),
 O5(H5B,H5C), O8(H8A,H8B)
3.c Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C14(H14A,H14B), C15(H15A,
 H15B), C16(H16A,H16B), C20(H20A,H20B), C19(H19A,H19B), C18(H18A,H18B),
 C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C59(H59A,H59B), C60(H60A,H60B),
  C61(H61A,H61B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B), C51(H51A,
 H51B), C53(H53A,H53B), C52(H52A,H52B), C47(H47A,H47B), C48(H48A,H48B),
 C49(H49A,H49B)
3.d Aromatic/amide H refined with riding coordinates:
 C33(H33), C34(H34), C35(H35), C36(H36), C42(H42), C41(H41), C39(H39), C7(H7),
 C6(H6), C5(H5A), C4(H4A), C10(H10), C12(H12), C13(H13)
3.e Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C17(H17A,H17B,H17C), C21(H21A,H21B,H21C), C25(H25A,H25B,
 H25C), C62(H62A,H62B,H62C), C58(H58A,H58B,H58C), C54(H54A,H54B,H54C), C50(H50A,
 H50B,H50C)
;
_shelx_res_checksum              71658
_shelx_hkl_checksum              63503
_olex2_submission_special_instructions 'No special instructions were received'