Unprecedented C-F bond cleavage in perfluoronaphthalene during cobaltocene reduction.
Kundu, Gargi; Pramanik, Debjit; Dash, Soumya Ranjan; Kumar, Ravi; Sangole, Mayur; Tothadi, Srinu; Ghosh, Aryya; Vanka, Kumar; Singh, Kirandeep; Sen, Sakya S.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 17789–17793; doi:10.1039/d4dt02791d

data_7717291
_publ_section_title
;
 Unprecedented C-F bond cleavage in perfluoronaphthalene during
 cobaltocene reduction.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17789
_journal_page_last               17793
_journal_paper_doi               10.1039/d4dt02791d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C64 H76 F6 N4, 4(C H2 Cl2), 2(F3 H2)'
_chemical_formula_sum            'C68 H88 Cl8 F12 N4'
_chemical_formula_weight         1473.02
_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             2023-06-14
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_audit_update_record
;
2023-06-15 deposited with the CCDC.	2024-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.463(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.6927(8)
_cell_length_b                   18.5978(11)
_cell_length_c                   14.5593(8)
_cell_measurement_reflns_used    9832
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.65
_cell_volume                     3676.5(4)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON II CPAD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            61641
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.340
_diffrn_reflns_theta_min         2.001
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.378
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1020 before and 0.0576 after correction. The Ratio of minimum to maximum transmission is 0.9118. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.491
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         9146
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0652
_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^)+(0.0799P)^2^+5.4908P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1714
_refine_ls_wR_factor_ref         0.1818
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7884
_reflns_number_total             9146
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02791d2.cif
_cod_data_source_block           platon_pl
_cod_depositor_comments
'Adding full bibliography for 7717291--7717293.cif.'
_cod_database_code               7717291
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.942
_olex2_refinement_description
;
1. Others
 Sof(H32C)=Sof(H32D)=Sof(Cl1A)=1-FVAR(1)
 Sof(Cl1B)=Sof(H32A)=Sof(H32B)=FVAR(1)
2.a Ternary CH refined with riding coordinates:
 C26(H26), C29(H29), C7(H7), C10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C13(H13A,H13B), C33(H33A,H33B), C32(H32A,H32B), C32(H32C,H32D)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C22(H22), C24(H24), C23(H23), C5(H5), C8(H8)
2.d Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C11(H11A,H11B,H11C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C37(H37A,
 H37B,H37C)
;
_shelx_res_checksum              67961
_shelx_hkl_checksum              20382
_olex2_submission_special_instructions 'No special instructions were received'