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_7717628
_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, H O0.5'
_chemical_formula_sum            'C13 H11 N2 O2.5'
_chemical_formula_weight         235.24
_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
_atom_sites_solution_primary     iterative
_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                94.416(7)
_cell_angle_beta                 91.100(9)
_cell_angle_gamma                93.667(8)
_cell_formula_units_Z            2
_cell_length_a                   3.8217(9)
_cell_length_b                   5.7898(11)
_cell_length_c                   24.196(5)
_cell_measurement_reflns_used    1178
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      0.980
_cell_measurement_theta_min      0.978
_cell_volume                     532.5(2)
_computing_cell_refinement       'Bruker SHELXL'
_computing_data_collection       'Bruker APEX4'
_computing_data_reduction        'Bruker SAINT'
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 quest photon detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0914
_diffrn_reflns_av_unetI/netI     0.1031
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            8067
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.564
_diffrn_reflns_theta_min         2.534
_diffrn_source                   microfocus
_exptl_absorpt_coefficient_mu    0.104
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       Plate
_exptl_crystal_F_000             246
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.250
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2435
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.1660
_refine_ls_R_factor_gt           0.0695
_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^)+(0.0624P)^2^+0.2484P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1450
_refine_ls_wR_factor_ref         0.2003
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1178
_reflns_number_total             2435
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02857k2.cif
_cod_data_source_block           24diohbicyc
_cod_depositor_comments
'Adding full bibliography for 7717624--7717629.cif.'
_cod_original_formula_sum        'C13 H11 N2 O2.50'
_cod_database_code               7717628
_shelx_shelxl_version_number     2019/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O3-H3
 0.85 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 N2(H2A), C10(H10), C13(H13), C7(H7), C12(H12), C4(H4), C5(H5), C6(H6)
3.b Idealised tetrahedral OH refined as rotating group:
 O2(H2), O1(H1)
;
_shelx_res_checksum              87593
_shelx_hkl_checksum              26364
_olex2_submission_special_instructions 'No special instructions were received'