Spin-state control of cobalt(II) and iron(II) complexes with click-derived tripodal ligands through non-covalent and fluorine-specific interactions.
Nößler, Maite; Hunger, David; Reichert, Felix; Winkler, Mario; Reimann, Marc; Klein, Johannes; Suhr, Simon; Suntrup, Lisa; Beerhues, Julia; Kaupp, Martin; van Slageren, Joris; Sarkar, Biprajit; Dalton transactions (Cambridge, England : 2003) 50 (2021) 18097–18106; doi:10.1039/d1dt03535e

data_7709218
_publ_section_title
;
 Spin-state control of cobalt(II) and iron(II) complexes with
 click-derived tripodal ligands through non-covalent and fluorine-specific
 interactions.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18097
_journal_page_last               18106
_journal_paper_doi               10.1039/d1dt03535e
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'C60 H41.597 Co F20 N20, 1.5(B F4), 2(B0.229 F0.972)'
_chemical_formula_sum            'C60 H41.62 B1.96 Co F27.95 N20'
_chemical_formula_weight         1653.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-11-09
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_audit_update_record
;
2021-11-09 deposited with the CCDC.	2021-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.6950(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.6532(5)
_cell_length_b                   24.4358(5)
_cell_length_c                   11.6193(2)
_cell_measurement_reflns_used    5707
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.370
_cell_measurement_theta_min      2.365
_cell_volume                     6738.7(2)
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_collection       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT+ (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_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  0.0269
_diffrn_reflns_av_unetI/netI     0.0136
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            50937
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.370
_diffrn_reflns_theta_min         2.365
_exptl_absorpt_coefficient_mu    0.390
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1430 before and 0.0431 after correction.
The Ratio of minimum to maximum transmission is 0.9514.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_description       block
_exptl_crystal_F_000             3320
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.057
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     766
_refine_ls_number_reflns         6157
_refine_ls_number_restraints     571
_refine_ls_restrained_S_all      1.213
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0719P)^2^+21.7355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1615
_refine_ls_wR_factor_ref         0.1647
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5704
_reflns_number_total             6157
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03535e2.cif
_cod_data_source_block           bip587_a
_cod_database_code               7709218
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 B1-F14 = B1-F15 = B1-F16 = B1-F17
 1.42 with sigma of 0.02
 C1C-C1B = C1B-C1A = C1A-C32 = C32-C31 = C31-C23 = C23-C1C
 1.39 with sigma of 0.01
 C25-C30 = C30-C29 = C29-C28 = C28-C27 = C27-C26 = C26-C25
 1.39 with sigma of 0.01
 C7-CXF = CXF-CXE = CXE-CXD = CXD-C22 = C22-C37 = C37-C7
 1.39 with sigma of 0.01
 B2-F11 \\sim B2-F12 \\sim B2-F13 \\sim B2-F18
 with sigma of 0.02
 C7-F21 \\sim F21-C22
 with sigma of 0.01
 C1B-C14 \\sim C14-C23
 with sigma of 0.001
 CXF-C4 \\sim C4-C37
 with sigma of 0.001
 C7-F19 \\sim F19-CXE
 with sigma of 0.001
 CXF-F20 \\sim F20-CXD
 with sigma of 0.001
 CXE-F22 \\sim F22-C22
 with sigma of 0.001
 F11-F12 \\sim F12-F13 \\sim F13-F18 \\sim F18-F11 \\sim F12-F18 \\sim F11-F13
 with sigma of 0.04
 B2-F11 \\sim B2A-F11A
 with sigma of 0.02
 B2-F13 \\sim B2A-F13A
 with sigma of 0.02
 B2-F18 \\sim B2A-F18A
 with sigma of 0.02
 F12-F18 \\sim F12A-F18A
 with sigma of 0.04
 B2-F12 \\sim B2A-F12A
 with sigma of 0.02
 F12-F13 \\sim F12A-F13A
 with sigma of 0.04
 F13-F18 \\sim F13A-F18A
 with sigma of 0.04
 F11-F12 \\sim F11A-F12A
 with sigma of 0.04
 F11-F13 \\sim F11A-F13A
 with sigma of 0.04
 F11-F18 \\sim F11A-F18A
 with sigma of 0.04
 F14-F15 \\sim F15-F16 \\sim F16-F17 \\sim F17-F14 \\sim F15-F17 \\sim F14-F16
 with sigma of 0.04
 B1-F14 \\sim B1-F15 \\sim B1-F16 \\sim B1-F17
 with sigma of 0.02
 B1-F16 \\sim B1A-F16A
 with sigma of 0.02
 F15-F17 \\sim F15A-F17A
 with sigma of 0.04
 B1-F14 \\sim B1A-F14A
 with sigma of 0.02
 B1-F15 \\sim B1A-F15A
 with sigma of 0.02
 F16-F17 \\sim F16A-F17A
 with sigma of 0.04
 F14-F15 \\sim F14A-F15A
 with sigma of 0.04
 F14-F16 \\sim F14A-F16A
 with sigma of 0.04
 F14-F17 \\sim F14A-F17A
 with sigma of 0.04
 B1-F17 \\sim B1A-F17A
 with sigma of 0.02
 F15-F16 \\sim F15A-F16A
 with sigma of 0.04
 C7-CXE \\sim CXF-CXD \\sim CXE-C22 \\sim CXD-C37 \\sim C22-C7 \\sim C37-CXF
 with sigma of 0.02
 C25-C29 \\sim C30-C28 \\sim C29-C27 \\sim C28-C26 \\sim C27-C25 \\sim C26-C30
 with sigma of 0.02
 C1C-C1A \\sim C1B-C32 \\sim C1A-C31 \\sim C32-C23 \\sim C31-C1C \\sim C23-C1B
 with sigma of 0.02
3. Restrained planarity
 C14, C23, C31, C32, C1A, C1B, C1C
 with sigma of 0.001
 C4, F20, F21, F22, C7, C37, C22, CXD, CXE, F23, CXF, F19
 with sigma of 0.01
 C25, C30, C29, C28, C27, C26
 with sigma of 0.1
 C1C, C1B, C1A, C32, C31, C23
 with sigma of 0.1
 C7, CXF, CXE, CXD, C22, C37
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
F19 \\sim CXF \\sim C7 \\sim C37 \\sim C22 \\sim F21 \\sim F23 \\sim F22 \\sim
CXD \\sim CXE \\sim F20: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
B2 \\sim F11 \\sim F12 \\sim F13 \\sim F18: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
B1 \\sim F14 \\sim F15 \\sim F16 \\sim F17: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C1C \\sim C23 \\sim C31 \\sim C32 \\sim C1A \\sim C1B: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(B2A) \\sim Ueq, Uanis(B2) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(F18A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C23) = Uanis(C31) = Uanis(C32) = Uanis(C1A) = Uanis(C1B) = Uanis(C1C)
5. Rigid body (RIGU) restrains
 B2, F11, F12, F13, F18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F13, B2, F11, F12, F18
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 B2A, F11A, F12A, F13A, F18A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 B1, F14, F15, F16, F17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B1A, F14A, F15A, F16A, F17A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(H14C)=Sof(H14D)=Sof(H4A)=Sof(H4B)=Sof(F19)=Sof(F20)=Sof(F21)=Sof(F22)=
 Sof(C7)=Sof(C37)=Sof(C22)=Sof(CXD)=Sof(CXE)=Sof(CXF)=Sof(F23)=1-FVAR(1)
 Sof(F5)=Sof(F4)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(H14A)=Sof(H14B)=Sof(C5)=Sof(C10)=
 Sof(H10)=Sof(H4AA)=Sof(H4AB)=Sof(C2AA)=Sof(H2AA)=Sof(C3AA)=Sof(H3AA)=Sof(C6)=
 Sof(H6)=Sof(C1AA)=Sof(H1AA)=FVAR(1)
 Fixed Sof: C19(0.7) C20(0.7) C15(0.7) C17(0.7) C18(0.7) C16(0.7) B2(0.25)
 F11(0.25) F12(0.25) F13(0.25) F18(0.25) B2A(0.25) F11A(0.25) F12A(0.25)
 F13A(0.25) F18A(0.25) B1(0.25) F14(0.25) F15(0.25) F16(0.25) F17(0.25)
 C23(0.3) H23(0.3) C31(0.3) H31(0.3) C32(0.3) H32(0.3) C1A(0.3) H1AB(0.3)
 C1B(0.3) H1BA(0.3) C1C(0.3)
7.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C14(H14C,H14D), C14(H14A,H14B), C21(H21A,H21B), C1(H1A,H1B),
 C24(H24A,H24B), C4(H4A,H4B), C4(H4AA,H4AB)
7.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C9(H9), C3(H3), C10(H10), C2AA(H2AA), C3AA(H3AA), C6(H6),
 C1AA(H1AA), C23(H23), C31(H31), C32(H32), C1A(H1AB), C1B(H1BA)
;
_shelx_res_checksum              66822
_olex2_submission_special_instructions 'No special instructions were received'