Fluorinated Click-Derived Tripodal Ligands Drive Spin Crossover in both Iron(II) and Cobalt(II) Complexes
Nößler, Maite; Hunger, David; Neuman, Nicolás Ignacio; Reimann, Marc; Reichert, Felix; Winkler, Mario; Klein, Johannes; Bens, Tobias; Suntrup, Lisa; Demeshko, Serhiy; Stubbe, Jessica; Kaupp, Martin; van Slageren, Joris; Sarkar, Biprajit; Dalton Transactions  (2022) –; doi:10.1039/D2DT01005D

data_7710469
_publ_section_title
;
 Fluorinated Click-Derived Tripodal Ligands Drive Spin Crossover in both
 Iron(II) and Cobalt(II) Complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01005D
_journal_year                    2022
_chemical_formula_moiety         'C60 H54 Co F6 N20, 2(B F4)'
_chemical_formula_sum            'C60 H54 B2 Co F14 N20'
_chemical_formula_weight         1401.78
_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
_audit_creation_date             2020-10-08
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2021-03-12 deposited with the CCDC.	2022-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                91.161(12)
_cell_angle_beta                 107.864(13)
_cell_angle_gamma                93.211(13)
_cell_formula_units_Z            2
_cell_length_a                   14.384(6)
_cell_length_b                   14.984(6)
_cell_length_c                   15.384(6)
_cell_measurement_reflns_used    7519
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.391
_cell_measurement_theta_min      1.909
_cell_volume                     3148(2)
_computing_cell_refinement       'APEX 3 (Bruker, 2015)'
_computing_data_collection       'APEX 3 (Bruker, 2015)'
_computing_data_reduction        'SAINT+ (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  'XL n/a (Sheldrick, 2008)'
_computing_structure_solution
'olex2.solve 1.3 (Bourhis et al., 2015), inrinsic phasing'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'Omega + Phi Scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38191
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.391
_diffrn_reflns_theta_min         1.909
_exptl_absorpt_coefficient_mu    0.372
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6363
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0674 before and 0.0566 after correction.
The Ratio of minimum to maximum transmission is 0.8539.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_description       block
_exptl_crystal_F_000             1434
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     896
_refine_ls_number_reflns         11473
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0597
_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^)+(0.0576P)^2^+3.7645P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1362
_refine_ls_wR_factor_ref         0.1607
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7519
_reflns_number_total             11473
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01005d2.cif
_cod_data_source_block           bip594_a
_cod_database_code               7710469
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: C2B(0.5) H2BB(0.5) H2BA(0.5) C3A(0.5) H3AA(0.5) H3AB(0.5) C3B(0.5)
 H3BB(0.5) H3BA(0.5) C2A(0.5) H2AB(0.5) H2AA(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C36(H36A,H36B), C33(H33A,H33B), C3(H3A,H3B),
 C15(H15A,H15B), C24(H24A,H24B), C6(H6A,H6B), C45(H45A,H45B), C44(H44A,H44B),
 C2B(H2BB,H2BA), C3A(H3AA,H3AB), C3B(H3BB,H3BA), C2A(H2AB,H2AA)
3.b Aromatic/amide H refined with riding coordinates:
 C38(H38), C4(H4), C60(H60), C34(H34), C59(H59), C29(H29), C39(H39), C12(H12),
 C9(H9), C27(H27), C8(H8), C52(H52), C1(H1), C51(H51), C11(H11), C17(H17),
 C21(H21), C41(H41), C20(H20), C57(H57), C13(H13), C43(H43), C42(H42), C26(H26),
  C50(H50), C47(H47), C22(H22), C48(H48), C63(H63)
;
_shelx_res_checksum              46839
_shelx_fab_checksum              533
_olex2_submission_special_instructions 'No special instructions were received'