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_7709224
_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(C30 H15 Co0.5 F15 N10), 2(B F4), 1.35(C7 H8), 0.65(C4 H8 O)'
_chemical_formula_sum            'C72.05 H46 B2 Co F38 N20 O0.65'
_chemical_formula_weight         2004.823
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2021-11-05
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2021-11-09 deposited with the CCDC.	2021-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                68.616(2)
_cell_angle_beta                 80.878(3)
_cell_angle_gamma                86.182(3)
_cell_formula_units_Z            2
_cell_length_a                   11.6982(10)
_cell_length_b                   18.9258(13)
_cell_length_c                   19.4058(16)
_cell_measurement_reflns_used    11515
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.437
_cell_measurement_theta_min      2.233
_cell_volume                     3949.9(5)
_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  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution
'olex2.solve (Bourhis et al., 2015), intrinsic phasing'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.9987
_diffrn_measured_fraction_theta_max 0.9971
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'Omega + Phi Scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0737
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_Laue_measured_fraction_full 0.9987
_diffrn_reflns_Laue_measured_fraction_max 0.9971
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            72484
_diffrn_reflns_point_group_measured_fraction_full 0.9987
_diffrn_reflns_point_group_measured_fraction_max 0.9971
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         26.44
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    0.367
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6823
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1127 before and 0.0582 after correction.
The Ratio of minimum to maximum transmission is 0.9153.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            clear
_exptl_crystal_colour_lustre     clear
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_description       block
_exptl_crystal_F_000             2007.473
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.5601
_refine_diff_density_min         -0.9186
_refine_diff_density_rms         0.1419
_refine_ls_d_res_high            0.7982
_refine_ls_d_res_low             9.1196
_refine_ls_goodness_of_fit_ref   1.0882
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    94
_refine_ls_number_parameters     1350
_refine_ls_number_reflns         16211
_refine_ls_number_restraints     414
_refine_ls_restrained_S_all      1.0734
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0650
_refine_ls_shift/su_max          -0.0500
_refine_ls_shift/su_mean         0.0011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+11.3117P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1389
_refine_ls_wR_factor_ref         0.1598
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              23
_reflns_limit_k_min              -21
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                11515
_reflns_number_total             16211
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1dt03535e2.cif
_cod_data_source_block           bip226_a
_cod_original_cell_volume        3949.9(6)
_cod_database_code               7709224
_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
 C9-C14 = C9-C19 = C15-C16
 1.39 with sigma of 0.02
 C8-C9
 1.51 with sigma of 0.02
 C14-C15 = C16-C18 = C18-C19
 1.38 with sigma of 0.02
 C14-C16
 2.39 with sigma of 0.04
 C9-C18
 2.41 with sigma of 0.04
 C15-C18 = C16-C19
 2.4 with sigma of 0.04
 C8-C14 = C8-C19
 2.52 with sigma of 0.04
 C9-C15
 2.42 with sigma of 0.04
 C27A-F28B \\sim C4-F28C
 with sigma of 0.04
 F29A-C29A \\sim F29B-C2
 with sigma of 0.02
 C29A-F28B \\sim C2-F28C
 with sigma of 0.04
 F25A-C25A \\sim F25B-C6
 with sigma of 0.02
 C9-C18 \\sim C9-C15 \\sim C19-C16 \\sim C14-C19 \\sim C15-C18 \\sim C14-C16
 with sigma of 0.04
 C24A-C29A \\sim C1-C2
 with sigma of 0.02
 C24A-C25A \\sim C1-C6
 with sigma of 0.02
 C29A-C28A \\sim C2-C3
 with sigma of 0.02
 C8-C19 \\sim C8-C14
 with sigma of 0.04
 C28A-C27A \\sim C3-C4
 with sigma of 0.02
 C24A-C26A \\sim C1-C5
 with sigma of 0.04
 C28A-F28B \\sim C3-F28C
 with sigma of 0.02
 C29A-C25A \\sim C2-C6
 with sigma of 0.04
 C28A-C26A \\sim C3-C5
 with sigma of 0.04
 C27A-C26A \\sim C4-C5
 with sigma of 0.02
 C9-C14 \\sim C14-C15 \\sim C15-C16 \\sim C16-C18 \\sim C18-C19 \\sim C19-C9
 with sigma of 0.02
 C27A-F27B \\sim C4-F27C
 with sigma of 0.02
 C26A-C25A \\sim C5-C6
 with sigma of 0.02
 C26A-F26B \\sim C5-F26C
 with sigma of 0.02
 C29A-C27A \\sim C2-C4
 with sigma of 0.04
 C28A-F27B \\sim C3-F27C
 with sigma of 0.04
 C27A-C25A \\sim C4-C6
 with sigma of 0.04
 C27A-F26B \\sim C4-F26C
 with sigma of 0.04
 C26A-F27B \\sim C5-F27C
 with sigma of 0.04
 N22A-C24A \\sim N22A-C1
 with sigma of 0.04
 C25A-F26B \\sim C6-F26C
 with sigma of 0.04
 F29A-C24A \\sim F29B-C1
 with sigma of 0.04
 F29A-C28A \\sim F29B-C3
 with sigma of 0.04
 F25A-C24A \\sim F25B-C1
 with sigma of 0.04
 F25A-C26A \\sim F25B-C5
 with sigma of 0.04
 C24A-C28A \\sim C1-C3
 with sigma of 0.04
 C7-C1 \\sim C7-C24A
 with sigma of 0.001
3. Restrained planarity
 C8, C9, C14, C15, C16, C18, C19
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C8 \\sim C9 \\sim C14 \\sim C15 \\sim C16 \\sim C18 \\sim C19: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C8 \\sim C9 \\sim C14 \\sim C19 \\sim C15 \\sim C18 \\sim C16: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C11 \\sim O1 \\sim C12 \\sim C10 \\sim C13: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
5. Rigid body (RIGU) restrains
 F29A, F26B, F25A, F28B, C24A, C25A, C29A, F31A, C28A, F27B, C27A, C26A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F29B, C7, C5, F25B, F27C, C1, C6, C2, F28C, C3, F26C, C4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C203, C206, C205, C201, C204, C202, C200
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(F29B)=Sof(F25B)=Sof(C1)=Sof(C2)=Sof(C3)=Sof(C4)=Sof(C5)=Sof(C6)=Sof(H7bc)=
 Sof(H7bd)=Sof(F28C)=Sof(F27C)=Sof(F26C)=1-FVAR(1)
 Sof(F29A)=Sof(F25A)=Sof(C24A)=Sof(C29A)=Sof(C28A)=Sof(C27A)=Sof(C26A)=
 Sof(C25A)=Sof(F28B)=Sof(F27B)=Sof(F26B)=Sof(H7aa)=Sof(H7ab)=FVAR(1)
 Fixed Sof: F31A(0.75) F20(0.25) O1(0.65) C10(0.65) H10e(0.65) H10f(0.65)
 H10g(0.65) C11(0.65) H11(0.65) C12(0.65) H12(0.65) C13(0.65) H13e(0.65)
 H13f(0.65) H13g(0.65) C8(0.35) H8a(0.35) H8b(0.35) H8c(0.35) C9(0.35)
 C14(0.35) H14(0.35) C15(0.35) H15(0.35) C16(0.35) H16(0.35) C18(0.35)
 H18(0.35) C19(0.35) H19(0.35)
7.a Riding coordinates:
 C10(H10e,H10f,H10g), C13(H13e,H13f,H13g), C8(H8a,H8b,H8c)
7.b Secondary CH2 refined with riding coordinates:
 C10A(H10a,H10b), C10B(H10c,H10d), C20A(H20a,H20b), C13B(H13c,H13d), C13A(H13a,
 H13b), C20B(H20c,H20d), C30A(H30a,H30b), C23B(H23a,H23b), C30B(H30c,H30d),
 C33A(H33a,H33b), C33B(H33c,H33d), C7(H7aa,H7ab), C7(H7bc,H7bd)
7.c Aromatic/amide H refined with riding coordinates:
 C12A(H12A), C206(H206), C205(H205), C204(H204), C203(H203), C202(H202),
 C12B(H12B), C22A(H22A), C22B(H22B), C32B(H32B), C32A(H32A), C11(H11), C12(H12),
  C14(H14), C15(H15), C16(H16), C18(H18), C19(H19)
7.d Fitted hexagon refined as free rotating group:
 C24A(C29A,C28A,C27A,C26A,C25A), C1(C2,C3,C4,C5,C6)
7.e Idealised Me refined as rotating group:
 C200(H20e,H20f,H20g)
;
_olex2_submission_special_instructions 'No special instructions were received'