New examples of –C–F–Ae (Ae = alkaline earth) and –C–F–K bonding
Werner, Daniel; Guo, Zhifang; Blair, Victoria L.; Deacon, Glen B.; Junk, Peter C.; New Journal of Chemistry 49 (2025) 18725–18734; doi:10.1039/D5NJ03383G

data_7064058
_publ_section_title
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 New examples of --C--F--Ae (Ae = alkaline earth) and --C--F--K bonding
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_journal_issue                   43
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18725
_journal_page_last               18734
_journal_paper_doi               10.1039/D5NJ03383G
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'C34 H28 F12 K2 N4 O2'
_chemical_formula_sum            'C34 H28 F12 K2 N4 O2'
_chemical_formula_weight         830.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2025-04-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-07-23 deposited with the CCDC.	2025-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.3940(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5521(7)
_cell_length_b                   14.9796(7)
_cell_length_c                   15.7547(8)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      29.212
_cell_measurement_theta_min      2.212
_cell_volume                     3647.5(3)
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            38045
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.349
_diffrn_reflns_theta_min         1.745
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.359
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0378 before and 0.0326 after correction.
The Ratio of minimum to maximum transmission is 0.9257.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_description       block
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         9958
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0430P)^2^+1.1423P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0903
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7604
_reflns_number_total             9958
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj03383g2.cif
_cod_data_source_block           p21n_3
_cod_depositor_comments
'Adding full bibliography for 7064055--7064062.cif.'
_cod_database_code               7064058
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.900
_olex2_refinement_description
;
1. Others
 Fixed Sof: F12A(0.5) F12B(0.5)
2.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C32(H32A,H32B)
2.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C20(H20), C21(H21), C28(H28), C27(H27), C13(H13), C14(H14),
 C15(H15), C12(H12), C26(H26), C25(H25), C23(H23), C18(H18), C8(H8), C3(H3),
 C4(H4), C5(H5), C6(H6)
2.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C)
;
_shelx_res_checksum              46729
_olex2_submission_special_instructions 'No special instructions were received'