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_7709223
_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
'2(C60 H30 Co F30 N20), 4(B F4), 3.4(C4.3 H3.58 F0.75), C4 H10 O, 2(C1.7 H1.42 F0.25)'
_chemical_formula_sum            'C142 H85 B4 Co2 F79 N40 O'
_chemical_formula_weight         4029.59
_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             2019-09-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-03-12 deposited with the CCDC.	2021-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                68.474(4)
_cell_angle_beta                 80.359(3)
_cell_angle_gamma                86.509(3)
_cell_formula_units_Z            1
_cell_length_a                   11.7351(10)
_cell_length_b                   18.920(2)
_cell_length_c                   19.260(2)
_cell_measurement_reflns_used    10992
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.462
_cell_measurement_theta_min      2.249
_cell_volume                     3921.8(7)
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_collection       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT+ (Bruker, 2009)'
_computing_molecular_graphics    'Diamond 3D, Version 4.0(Brandenburg, 2014)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
'SHELXT 2014/5 (Sheldrick, 2014), intrinsic phasing'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.981
_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  0.0712
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            104728
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.462
_diffrn_reflns_theta_min         2.249
_exptl_absorpt_coefficient_mu    0.373
_exptl_absorpt_correction_T_max  0.7254
_exptl_absorpt_correction_T_min  0.6694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1137 before and 0.0749 after correction. The Ratio of minimum to maximum transmission is 0.9228. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_description       block
_exptl_crystal_F_000             2010
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.971
_refine_diff_density_min         -0.856
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1595
_refine_ls_number_reflns         14271
_refine_ls_number_restraints     720
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.145
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0441P)^2^+7.0560P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1236
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10992
_reflns_number_total             14271
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03535e2.cif
_cod_data_source_block           bip576_2_a
_cod_database_code               7709223
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.964
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C30-C25 \\sim C26-C25 \\sim C27-C26 \\sim C28-C27 \\sim C29-C28 \\sim C30-C29
\\sim C26B-C1A \\sim C30B-
 C1A \\sim C30B-C29B \\sim C29B-C28B \\sim C28B-C27B \\sim C27B-C26B
 with sigma of 0.02
 F15-C30 \\sim F14-C29 \\sim F13-C28 \\sim F12-C27 \\sim F11-C26 \\sim
F15B-C30B \\sim F14B-C29B ~
 F13B-C28B \\sim F12B-C27B \\sim F11B-C26B
 with sigma of 0.02
 C21A-C20A \\sim C21A-C16A \\sim C20A-C19A \\sim C19A-C18A \\sim C18A-C17A
\\sim C17A-C16A \\sim C18-
 C17 \\sim C17-C16 \\sim C21-C16 \\sim C21-C20 \\sim C20-C19 \\sim C19-C18
 with sigma of 0.02
 F5A-C17A \\sim F4A-C18A \\sim F3A-C19A \\sim F2A-C20A \\sim F1A-C21A \\sim
F4-C18 \\sim F3-C19 \\sim F2-
 C20 \\sim F1-C21 \\sim F5-C17
 with sigma of 0.02
 C16-C15 \\sim C16A-C15
 with sigma of 0.2
 C9AA-C7AA \\sim C9AA-C6AA \\sim C6AA-C4AA \\sim C4AA-C3AA \\sim C5AA-C3AA
\\sim C7AA-C5AA
 with sigma of 0.02
 C62-C61 \\sim C66-C61 \\sim C66-C65 \\sim C65-C64 \\sim C64-C63 \\sim C63-C62
 with sigma of 0.02
 C37A-C36 \\sim C37-C36
 with sigma of 0.02
 O1-C71 \\sim O1-C72
 with sigma of 0.02
 O1-C70 \\sim C73-O1
 with sigma of 0.02
 C3AA-C7AA \\sim C4AA-C9AA
 with sigma of 0.02
 C5AA-C6AA \\sim C7AA-C4AA \\sim C3AA-C9AA
 with sigma of 0.02
 C66A-C62A \\sim C63A-C65A
 with sigma of 0.02
 C66A-C61A \\sim C62A-C63A \\sim C64A-C65A \\sim C61-C62 \\sim C63-C64 \\sim
C65-C66
 with sigma of 0.02
 C61A-C62A \\sim C63A-C64A \\sim C65A-C66A
 with sigma of 0.02
 C61A-C64A \\sim C66A-C63A \\sim C62A-C65A
 with sigma of 0.02
 C73-C72 \\sim C71-C70
 with sigma of 0.02
 C73-C71 \\sim C72-C70
 with sigma of 0.02
 C41A-C40A \\sim C42A-C37A \\sim C42A-C41A \\sim C40A-C39A \\sim C39A-C38A
\\sim C38A-C37A \\sim C42-
 C37 \\sim C42-C41 \\sim C41-C40 \\sim C40-C39 \\sim C39-C38 \\sim C38-C37
 with sigma of 0.02
 C42A-C38A \\sim C41A-C39A \\sim C38-C42 \\sim C39-C41
 with sigma of 0.02
 C37-C40 \\sim C37A-C40A \\sim C41A-C38A \\sim C41-C38 \\sim C42A-C39A \\sim
C42-C39
 with sigma of 0.02
 C42A-C37A \\sim C38A-C37A \\sim C42-C37 \\sim C38-C37
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F16 \\sim F17 \\sim F18 \\sim C40 \\sim C41 \\sim C42 \\sim F18A \\sim C40A
\\sim F17A \\sim C41A \\sim F16A \\sim C42A \\sim F19 \\sim F20 \\sim C38 \\sim
C39 \\sim C38A \\sim C39A \\sim F19A \\sim F20A \\sim C37 \\sim C37A: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08
: with sigma of 0.1 and sigma for terminal atoms of 0.2
: with sigma of 0.1 and sigma for terminal atoms of 0.2
: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Others
 Sof(H24C)=Sof(H24D)=Sof(C1A)=Sof(C26B)=Sof(C27B)=Sof(C28B)=Sof(C29B)=
 Sof(C30B)=Sof(F11B)=Sof(F12B)=Sof(F13B)=Sof(F14B)=Sof(F15B)=1-FVAR(1)
 Sof(H24A)=Sof(H24B)=Sof(C25)=Sof(C26)=Sof(C27)=Sof(C28)=Sof(C29)=Sof(C30)=
 Sof(F11)=Sof(F12)=Sof(F13)=Sof(F14)=Sof(F15)=FVAR(1)
 Sof(H15C)=Sof(H15D)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(C16A)=
 Sof(C17A)=Sof(C18A)=Sof(C19A)=Sof(C21A)=Sof(C20A)=1-FVAR(2)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(H15A)=Sof(H15B)=Sof(C16)=Sof(C17)=
 Sof(C18)=Sof(C19)=Sof(C21)=Sof(C20)=FVAR(2)
 Sof(C66A)=Sof(H66A)=Sof(C62A)=Sof(H62A)=Sof(C65A)=Sof(H65A)=Sof(C61A)=
 Sof(C64A)=Sof(H64A)=Sof(C63A)=Sof(H63A)=1-FVAR(3)
 Sof(C61)=Sof(C62)=Sof(H62)=Sof(C63)=Sof(H63)=Sof(C64)=Sof(H64)=Sof(C65)=
 Sof(H65)=Sof(C66)=Sof(H66)=FVAR(3)
 Sof(H36C)=Sof(H36D)=Sof(F18A)=Sof(C40A)=Sof(F17A)=Sof(C41A)=Sof(F16A)=
 Sof(C42A)=Sof(C37A)=Sof(C38A)=Sof(C39A)=Sof(F19A)=Sof(F20A)=1-FVAR(4)
 Sof(F16)=Sof(F17)=Sof(F18)=Sof(F19)=Sof(F20)=Sof(C37)=Sof(H36A)=Sof(H36B)=
 Sof(C38)=Sof(C39)=Sof(C40)=Sof(C41)=Sof(C42)=FVAR(4)
 Fixed Sof: O1(0.5) C6AA(0.5) H6AA(0.5) C72(0.5) H72A(0.5) H72B(0.5) C4AA(0.5)
 H4AA(0.5) C3AA(0.5) H3AA(0.5) C73(0.5) H73A(0.5) H73B(0.5) H73C(0.5) C70(0.5)
 H70A(0.5) H70B(0.5) H70C(0.5) C71(0.5) H71A(0.5) H71B(0.5) C7AA(0.5) H7AA(0.5)
 C5AA(0.5) C9AA(0.5) H9AA(0.5) F0AA(0.5) F31A(0.25) F31(0.75)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C6(H6A,H6B), C15(H15A,H15B), C15(H15C,
 H15D), C24(H24A,H24B), C24(H24C,H24D), C32(H32A,H32B), C31(H31A,H31B),
 C33(H33A,H33B), C36(H36A,H36B), C36(H36C,H36D), C45(H45A,H45B), C54(H54A,H54B),
  C72(H72A,H72B), C71(H71A,H71B)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C14(H14), C23(H23), C35(H35), C44(H44), C53(H53), C62(H62), C63(H63),
 C64(H64), C65(H65), C66(H66), C6AA(H6AA), C4AA(H4AA), C3AA(H3AA), C7AA(H7AA),
 C9AA(H9AA), C66A(H66A), C62A(H62A), C65A(H65A), C64A(H64A), C63A(H63A)
5.c Idealised Me refined as rotating group:
 C73(H73A,H73B,H73C), C70(H70A,H70B,H70C)
;
_shelx_res_checksum              83294
_olex2_submission_special_instructions 'No special instructions were received'