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_7134893
_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_formula_moiety         'C28 H28 B2 Fe N7 O, 0.5(C2 H3 N)'
_chemical_formula_sum            'C29 H29.5 B2 Fe N7.5 O'
_chemical_formula_weight         576.57
_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             2024-11-21
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-06-26 deposited with the CCDC.	2025-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.690(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5019(5)
_cell_length_b                   17.6496(5)
_cell_length_c                   13.4172(5)
_cell_measurement_reflns_used    22201
_cell_measurement_temperature    220.0
_cell_measurement_theta_max      31.37
_cell_measurement_theta_min      2.14
_cell_volume                     2950.64(18)
_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      220.0
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.844
_diffrn_measurement_details
;
 1330 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  0.0304
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.844
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27570
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.844
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.702
_diffrn_reflns_theta_min         2.141
_exptl_absorpt_coefficient_mu    0.547
_exptl_absorpt_correction_T_max  0.9518
_exptl_absorpt_correction_T_min  0.5935
_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    1.298
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.243
_exptl_crystal_size_min          0.16
_exptl_crystal_size_rad          0.140
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         9156
_refine_ls_number_restraints     246
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_gt           0.0777
_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^)+(0.0697P)^2^+2.7006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2016
_refine_ls_wR_factor_ref         0.2156
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6471
_reflns_number_total             9156
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03779d2.cif
_cod_data_source_block           jgb-mh-010-002_220k_3d
_cod_depositor_comments
'Adding full bibliography for 7134889--7134894.cif.'
_cod_original_formula_sum        'C29 H29.50 B2 Fe N7.50 O'
_cod_database_code               7134893
_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
 At 1.5 times of:
  All B(H,H,H) groups, All C(H,H,H) groups
2. Restrained distances
 C29-C30 = C29A-C30A
 1.48 with sigma of 0.01
 N8-C30 = N8A-C30A
 2.62 with sigma of 0.01
 N8-C29 = N8A-C29A
 1.14 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
N8 \\sim C29 \\sim C30A \\sim C30 \\sim C29A \\sim N8A: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04 within 1.7A
Uanis(C5A) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C7A)
\\sim Ueq, Uanis(C2A) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C4A) \\sim Ueq,
Uanis(C10A) \\sim Ueq, Uanis(C9A) \\sim Ueq, Uanis(C8A) \\sim Ueq, Uanis(C3)
\\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq,
Uanis(C10) \\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C11) \\sim Ueq: with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N4A) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C17A) \\sim Ueq, Uanis(C16A)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18A) \\sim Ueq,
Uanis(C18) \\sim Ueq, Uanis(C19A) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20)
\\sim Ueq, Uanis(C20A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C30) = Uanis(C30A)
Uanis(N8) = Uanis(N8A)
Uanis(C29) = Uanis(C29A)
4. 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(C13A)=Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(2)
 Sof(C13)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(2)
 Sof(H15C)=Sof(H15D)=Sof(C16A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(H18A)=
 Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=Sof(N4A)=1-FVAR(3)
 Sof(H15A)=Sof(H15B)=Sof(C16)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18)=Sof(C19)=
 Sof(H19)=Sof(C20)=Sof(H20)=Sof(N4)=FVAR(3)
 Fixed Sof: N8(0.25) C29(0.25) C30(0.25) H30A(0.25) H30B(0.25) H30C(0.25)
 N8A(0.25) C29A(0.25) C30A(0.25) H30D(0.25) H30E(0.25) H30F(0.25)
5.a Riding coordinates:
 C30(H30A,H30B,H30C)
5.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C15(H15C,H15D), C21(H21A,H21B)
5.c 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), C17A(H17A), C18A(H18A), C19A(H19A), C20A(H20A), C23(H23), C24(H24),
 C25(H25), C26(H26)
5.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C14A(H14D,H14E,H14F), B1(H1B,H1C,H1D), B2(H2A,H2B,H2C),
 C30A(H30D,H30E,H30F)
;
_shelx_res_checksum              14769
_shelx_hkl_checksum              13542
_olex2_submission_special_instructions 'No special instructions were received'