Chirality without compromise: identical spin crossover behavior between the racemate and the enantiopure Fe(II) complexes.
Becker, Jens-Georg; Sundaresan, Sriram; Carrella, Luca M.; Rentschler, Eva; Chemical communications (Cambridge, England) 61 (2025) 13389–13392; doi:10.1039/d5cc03779d

data_7134894
_publ_section_title
;
 Chirality without compromise: identical spin crossover behavior between
 the racemate and the enantiopure Fe(II) complexes.
;
_journal_issue                   71
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              13389
_journal_page_last               13392
_journal_paper_doi               10.1039/d5cc03779d
_journal_volume                  61
_journal_year                    2025
_chemical_absolute_configuration syn
_chemical_formula_moiety         '2(C28 H29 B2 Fe N7 O), C2 H3 N'
_chemical_formula_sum            'C58 H61 B4 Fe2 N15 O2'
_chemical_formula_weight         1155.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2025-04-16
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7205)
;
_audit_update_record
;
2025-06-26 deposited with the CCDC.	2025-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.564(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.5324(2)
_cell_length_b                   17.6041(3)
_cell_length_c                   13.3803(3)
_cell_measurement_reflns_used    45962
_cell_measurement_temperature    220
_cell_measurement_theta_max      32.42
_cell_measurement_theta_min      2.14
_cell_volume                     2942.62(10)
_computing_cell_refinement
;
X-Area Recipe 2.0.2 (STOE, 2024)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.194.0 (STOE, 2023)
;
_computing_data_reduction
;
X-Area Integrate 2.5.18.0 (STOE, 2024)
X-Area LANA 2.8.4 (STOE, 2024)
;
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      223.00
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.897
_diffrn_measurement_details
;
 2500 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0203
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.897
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            57456
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.624
_diffrn_reflns_theta_min         2.143
_exptl_absorpt_coefficient_mu    0.549
_exptl_absorpt_correction_T_max  0.7751
_exptl_absorpt_correction_T_min  0.5413
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens in: F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard,
Copenhagen (1970), 255 - 270. Afterwards scaling of reflection intensities was
performed within STOE LANA. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta
Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1204
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.257
_exptl_crystal_size_min          0.13
_exptl_crystal_size_rad          0.170
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.020(18)
_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     946
_refine_ls_number_reflns         18295
_refine_ls_number_restraints     1086
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0810P)^2^+0.8574P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1397
_refine_ls_wR_factor_ref         0.1502
_reflns_Friedel_coverage         0.842
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.799
_reflns_number_gt                15064
_reflns_number_total             18295
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03779d2.cif
_cod_data_source_block           jgb-mh-026_220k_3d
_cod_depositor_comments
'Adding full bibliography for 7134889--7134894.cif.'
_cod_database_code               7134894
_shelx_shelxl_version_number     2018/3
_diffrn_oxdiff_ac3_digest_hkl    413df083928fb769665369861fff3aefb8ca33
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.980(18)
 0.020(18)
2. 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 B(H,H,H) groups, All C(H,H,H) groups
3. Restrained distances
 C57-C58 = C57A-C58A
 1.48 with sigma of 0.01
 N15-C57 = N15A-C57A
 1.14 with sigma of 0.01
 C21-C22 \\sim C21-C22A
 with sigma of 0.02
4. Rigid bond restraints
 C22, C22A, C23A, C23, C24, C24A, C25, C25A, C26, C26A, N5, N5A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C38 \\sim C38A \\sim C29 \\sim C29A \\sim C37 \\sim C37A \\sim C36A \\sim C30
\\sim C30A \\sim C31A \\sim C36 \\sim C35 \\sim C35A \\sim C31 \\sim C34A \\sim
C32 \\sim C33 \\sim C33A \\sim C34 \\sim C32A: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 1.7A
C10 \\sim C10A \\sim C9A \\sim C1 \\sim C1A \\sim C9 \\sim C8 \\sim C2A \\sim
C2 \\sim C8A \\sim C7A \\sim C7 \\sim C3A \\sim C6 \\sim C4A \\sim C5A \\sim C5
\\sim C6A \\sim C4 \\sim C3: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 1.7A
C22A \\sim C22 \\sim N5 \\sim N5A \\sim C26A \\sim C26 \\sim C25A \\sim C25
\\sim C24A \\sim C24 \\sim C23A \\sim C23: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 1.7A
Uanis(C38) \\sim Ueq, Uanis(C38A) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C29A)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C37A) \\sim Ueq, Uanis(C36A) \\sim Ueq,
Uanis(C30) \\sim Ueq, Uanis(C30A) \\sim Ueq, Uanis(C31A) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C35A) \\sim Ueq, Uanis(C31) \\sim Ueq,
Uanis(C34A) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C33A)
\\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C32A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C10) \\sim Ueq, Uanis(C10A) \\sim Ueq, Uanis(C9A) \\sim Ueq, Uanis(C1)
\\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C8) \\sim Ueq,
Uanis(C2A) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C8A) \\sim Ueq, Uanis(C7A)
\\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C6) \\sim Ueq,
Uanis(C4A) \\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6A)
\\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C22) \\sim Ueq, Uanis(C22A) \\sim Ueq, Uanis(C23A) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C24A) \\sim Ueq, Uanis(C25) \\sim Ueq,
Uanis(C25A) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C26A) \\sim Ueq, Uanis(N5A)
\\sim Ueq, Uanis(N5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uiso(C58) = Uiso(C58A)
Uiso(N15) = Uiso(N15A)
Uiso(C57) = Uiso(C57A)
6. Others
 Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=
 Sof(H5A)=Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9A)=
 Sof(C10A)=1-FVAR(1)
 Sof(C1)=Sof(H1)=Sof(C2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=
 Sof(C6)=Sof(H6)=Sof(C7)=Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9)=Sof(C10)=FVAR(1)
 Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32A)=
 Sof(C33A)=Sof(H33A)=Sof(C34A)=Sof(H34A)=Sof(C35A)=Sof(C36A)=Sof(H36A)=
 Sof(C37A)=Sof(H37A)=Sof(C38A)=1-FVAR(2)
 Sof(C29)=Sof(H29)=Sof(C30)=Sof(C31)=Sof(H31)=Sof(C32)=Sof(H32)=Sof(C33)=
 Sof(H33)=Sof(C34)=Sof(H34)=Sof(C35)=Sof(C36)=Sof(H36)=Sof(C37)=Sof(H37)=
 Sof(C38)=FVAR(2)
 Sof(H21C)=Sof(H21D)=Sof(C22A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=
 Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=Sof(N5)=1-FVAR(3)
 Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)=
 Sof(H25)=Sof(C26)=Sof(H26)=Sof(N5A)=FVAR(3)
 Sof(N15A)=Sof(C57A)=Sof(C58A)=Sof(H58D)=Sof(H58E)=Sof(H58F)=1-FVAR(4)
 Sof(N15)=Sof(C57)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H58C)=FVAR(4)
7.a Riding coordinates:
 C58A(H58D,H58E,H58F)
7.b Ternary CH refined with riding coordinates:
 C13(H13), C41(H41)
7.c Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C21(H21A,H21B), C21(H21C,H21D), C43(H43A,H43B), C49(H49A,H49B)
7.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C1A(H1A), C3A(H3A),
 C4A(H4A), C5A(H5A), C6A(H6A), C8A(H8A), C9A(H9A), C17(H17), C18(H18), C19(H19),
  C20(H20), C23(H23), C24(H24), C25(H25), C26(H26), C23A(H23A), C24A(H24A),
 C25A(H25A), C26A(H26A), C29(H29), C31(H31), C32(H32), C33(H33), C34(H34),
 C36(H36), C37(H37), C29A(H29A), C31A(H31A), C32A(H32A), C33A(H33A), C34A(H34A),
  C36A(H36A), C37A(H37A), C45(H45), C46(H46), C47(H47), C48(H48), C51(H51),
 C52(H52), C53(H53), C54(H54)
7.e Fitted hexagon refined as free rotating group:
 C22(C23,C24,C25,C26,N5A), C22A(C23A,C24A,C25A,C26A,N5)
7.f Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), B1(H1B,H1C,H1D), B2(H2A,H2B,H2C), C42(H42A,H42B,H42C),
 B3(H3B,H3C,H3D), B4(H4B,H4C,H4D), C58(H58A,H58B,H58C)
;
_shelx_res_checksum              86430
_shelx_hkl_checksum              18810
_olex2_submission_special_instructions 'No special instructions were received'