Coordination-induced axial chirality controls the metal-centred configuration in a stereogenic-at-iron catalyst.
Buchberger, Benedikt; Demirel, Nemrud; Xie, Xiulan; Ivlev, Sergei I.; Meggers, Eric; Chemical communications (Cambridge, England) 61 (2025) 1894–1897; doi:10.1039/d4cc06227b

data_7134146
_publ_section_title
;
 Coordination-induced axial chirality controls the metal-centred
 configuration in a stereogenic-at-iron catalyst.
;
_journal_issue                   9
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1894
_journal_page_last               1897
_journal_paper_doi               10.1039/d4cc06227b
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety
'C70 H72 F6 Fe N10, 2(F6 P), C2 H3 N [+ solvent]'
_chemical_formula_sum            'C72 H75 F18 Fe N11 P2'
_chemical_formula_weight         1554.21
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/1
_audit_update_record
;
2024-11-04 deposited with the CCDC.	2025-01-02 downloaded from the CCDC.
;
_cell_angle_alpha                70.3280(10)
_cell_angle_beta                 85.4340(10)
_cell_angle_gamma                76.2540(10)
_cell_formula_units_Z            2
_cell_length_a                   12.86620(10)
_cell_length_b                   15.8429(2)
_cell_length_c                   20.5929(2)
_cell_measurement_reflns_used    171276
_cell_measurement_temperature    100
_cell_measurement_theta_max      77.35
_cell_measurement_theta_min      3.04
_cell_volume                     3839.41(7)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)
;
_computing_data_reduction
;
X-Area Integrate 2.5.3.0 (STOE, 2021)
X-Area LANA 2.7.5.0 (STOE, 2022)
;
_computing_molecular_graphics    'Diamond v4.6.8 (Brandenburg, 2022)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image
processing, for the correction and scaling of reflection intensities and
for outlier rejection, version 2.1, Darmstadt 2022
;
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details      ' 10130 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_collimation    '0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            186465
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         77.316
_diffrn_reflns_theta_min         3.040
_diffrn_source                   'Genix Cu'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.769
_exptl_absorpt_correction_T_max  0.9107
_exptl_absorpt_correction_T_min  0.6370
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published 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.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1604
_exptl_crystal_size_max          0.164
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       0.00031(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1269
_refine_ls_number_reflns         15884
_refine_ls_number_restraints     2272
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.050
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0523P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0906
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11912
_reflns_number_total             15884
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc06227b2.cif
_cod_data_source_block           MBB72C2rac
_cod_depositor_comments
'Adding full bibliography for 7134146--7134147.cif.'
_cod_database_code               7134146
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_min   0.660
_shelx_estimated_absorpt_t_max   0.912
_shelx_res_checksum              55179
_shelx_hkl_checksum              67236
_shelx_fab_checksum              23517