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_7717293
_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         'C84 H96 Co2 F4 N4, 3(C3 H7)'
_chemical_formula_sum            'C93 H117 Co2 F4 N4'
_chemical_formula_weight         1484.76
_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
_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                92.130(4)
_cell_angle_beta                 99.925(3)
_cell_angle_gamma                107.864(3)
_cell_formula_units_Z            2
_cell_length_a                   14.0847(15)
_cell_length_b                   14.5294(16)
_cell_length_c                   21.074(2)
_cell_measurement_reflns_used    9083
_cell_measurement_temperature    100
_cell_measurement_theta_max      36.25
_cell_measurement_theta_min      2.46
_cell_volume                     4024.6(7)
_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)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.928
_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  0.0520
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            252002
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         37.323
_diffrn_reflns_theta_min         1.947
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.469
_exptl_absorpt_correction_T_max  0.7472
_exptl_absorpt_correction_T_min  0.6849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1040 before and 0.0631 after correction. The Ratio of minimum to maximum transmission is 0.9166. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_description       block
_exptl_crystal_F_000             1586
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.205
_refine_diff_density_min         -2.218
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     958
_refine_ls_number_reflns         38853
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0509
_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^)+(0.0915P)^2^+2.2618P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1530
_refine_ls_wR_factor_ref         0.1714
_reflns_Friedel_coverage         0.000
_reflns_number_gt                31558
_reflns_number_total             38853
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02791d2.cif
_cod_data_source_block           mo_gk_octacobaltrepeat_0m
_cod_depositor_comments
'Adding full bibliography for 7717291--7717293.cif.'
_cod_original_cell_volume        4024.6(8)
_cod_database_code               7717293
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.884
_olex2_refinement_description
;
1. Others
 Sof(C92)=Sof(H92A)=Sof(H92B)=Sof(H92C)=1-FVAR(1)
 Sof(C93)=Sof(H93A)=Sof(H93B)=Sof(H93C)=FVAR(1)
2.a Ternary CH refined with riding coordinates:
 C69(H69), C70(H70), C71(H71), C78(H78), C73(H73), C72(H72), C45(H45),
 C60(H60), C22(H22), C56(H56), C53(H53), C75(H75), C74(H74), C31(H31), C76(H76),
  C34(H34), C77(H77), C18(H18)
2.b Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B), C95(H95A,H95B), C38(H38A,H38B), C21(H21A,H21B), C86(H86A,
 H86B), C89(H89A,H89B), C85(H85A,H85B), C88(H88A,H88B), C90(H90A,H90B),
 C91(H91A,H91B)
2.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C64(H64), C16(H16), C66(H66), C51(H51), C14(H14), C67(H67),
 C63(H63), C65(H65), C27(H27), C81(H81), C50(H50), C59(H59), C80(H80), C29(H29),
  C28(H28), C44(H44), C42(H42), C79(H79), C43(H43), C82(H82), C83(H83)
2.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C55(H55A,H55B,H55C), C32(H32A,H32B,
 H32C), C58(H58A,H58B,H58C), C57(H57A,H57B,H57C), C54(H54A,H54B,H54C), C36(H36A,
 H36B,H36C), C61(H61A,H61B,H61C), C35(H35A,H35B,H35C), C33(H33A,H33B,H33C),
 C62(H62A,H62B,H62C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C20(H20A,H20B,
 H20C), C19(H19A,H19B,H19C), C84(H84A,H84B,H84C), C87(H87A,H87B,H87C), C93(H93A,
 H93B,H93C), C92(H92A,H92B,H92C)
;
_shelx_res_checksum              4362
_shelx_hkl_checksum              7281
_olex2_submission_special_instructions 'No special instructions were received'