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_7710468
_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, B2 F8, C2 H8 O2'
_chemical_formula_sum            'C62 H62 B2 Co F14 N20 O2'
_chemical_formula_weight         1465.86
_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
_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                90
_cell_angle_beta                 98.408(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.7391(3)
_cell_length_b                   20.7813(8)
_cell_length_c                   20.1509(9)
_cell_measurement_reflns_used    4420
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.490
_cell_measurement_theta_min      4.255
_cell_volume                     3206.0(2)
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_collection       'APEX3 (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    'intrinsic phasing'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'omega + phi scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0634
_diffrn_reflns_av_unetI/netI     0.0677
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21514
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.490
_diffrn_reflns_theta_min         4.255
_exptl_absorpt_coefficient_mu    3.003
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6002
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0966 before and 0.0685 after correction.
The Ratio of minimum to maximum transmission is 0.7970.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       block
_exptl_crystal_F_000             1506
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.882
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         5786
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1219
_refine_ls_R_factor_gt           0.0928
_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^)+(0.0726P)^2^+15.4198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2113
_refine_ls_wR_factor_ref         0.2274
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4420
_reflns_number_total             5786
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01005d2.cif
_cod_data_source_block           bip422_a
_cod_database_code               7710468
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H30A-H20D
 1.9 with sigma of 0.02
 H30B-H10A
 1.9 with sigma of 0.02
 H100-O100
 1 with sigma of 0.02
3. Rigid body (RIGU) restrains
 H100, O100
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C10B)=Sof(H10C)=Sof(H10D)=Sof(C20B)=Sof(H20C)=Sof(H20D)=1-FVAR(1)
 Sof(C10A)=Sof(H10A)=Sof(H10B)=Sof(C20A)=Sof(H20A)=Sof(H20B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C23(H23A,H23B), C30(H30A,H30B), C33(H33A,H33B), C10A(H10A,
 H10B), C20A(H20A,H20B), C10B(H10C,H10D), C20B(H20C,H20D)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C15(H15), C16(H16), C18(H18), C19(H19), C25(H25), C26(H26),
 C28(H28), C29(H29), C35(H35), C36(H36), C38(H38), C39(H39), C32(H32), C22(H22)
5.c Idealised Me refined as rotating group:
 C100(H10E,H10F,H10G)
;
_shelx_res_checksum              37177
_olex2_submission_special_instructions 'No special instructions were received'