Heteroleptic iron(ii) complexes of chiral 2,6-bis(oxazolin-2-yl)-pyridine (PyBox) and 2,6-bis(thiazolin-2-yl)pyridine ligands – the interplay of two different ligands on the metal ion spin sate
Shahid, Namrah; Burrows, Kay E.; Pask, Christopher M.; Cespedes, Oscar; Howard, Mark J.; McGowan, Patrick C.; Halcrow, Malcolm A.; Dalton Transactions  (2022) –; doi:10.1039/D2DT00393G

data_7709644
_publ_section_title
;
 Heteroleptic iron(ii) complexes of chiral 2,6-bis(oxazolin-2-yl)-pyridine
 (PyBox) and 2,6-bis(thiazolin-2-yl)pyridine ligands -- the interplay of
 two different ligands on the metal ion spin sate
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00393G
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C42 H32 Fe N8 S2, 2(Cl O4)'
_chemical_formula_sum            'C42 H32 Cl2 Fe N8 O8 S2'
_chemical_formula_weight         967.62
_chemical_name_common
'[2,6-Bis((R)-4-phenyl-4,5-dihydrothiazol-2-yl)pyridine]- [2,6-Bis(benzimidazol-2-yl)pyridine]iron(II) diperchlorate'
_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   geom
_audit_creation_date             2021-03-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-01-10 deposited with the CCDC.	2022-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.601(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.9525(1)
_cell_length_b                   18.2692(1)
_cell_length_c                   11.2555(1)
_cell_measurement_reflns_used    21927
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.48
_cell_measurement_theta_min      1.75
_cell_volume                     2046.41(3)
_computing_cell_refinement       'XIA2 0.4.0.438-g4431aaa (Winter, 2010)'
_computing_data_collection       'GDA - generic data acquisition software'
_computing_data_reduction        'XIA2 0.4.0.438-g4431aaa (Winter, 2010)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            32540
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.817
_diffrn_reflns_theta_full        24.620
_diffrn_reflns_theta_max         35.911
_diffrn_reflns_theta_min         1.754
_diffrn_source                   Synchrotron
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_exptl_absorpt_coefficient_mu    0.617
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.981
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 DIALS 3.3.3-g5efb02d60-release
 Scaling & analysis of unmerged intensities, 
 absorption correction using spherical harmonics
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_description       fragment
_exptl_crystal_F_000             992
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile/diethyl ether'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 6518 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.022(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         17281
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0396P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0726
_refine_ls_wR_factor_ref         0.0735
_reflns_Friedel_coverage         0.754
_reflns_Friedel_fraction_full    0.931
_reflns_Friedel_fraction_max     0.719
_reflns_number_gt                16079
_reflns_number_total             17281
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00393g2.cif
_cod_data_source_block           ns523
_cod_database_code               7709644
_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 N(H) groups
2. Restrained distances
 Cl5B-O55B
 1.42386 with sigma of 0.02
 Cl5B-O56B
 1.42386 with sigma of 0.02
 Cl5B-O57B
 1.42386 with sigma of 0.02
 Cl5B-O58B
 1.42386 with sigma of 0.02
 O55B-O56B
 2.325163 with sigma of 0.02
 O55B-O57B
 2.325163 with sigma of 0.02
 O55B-O58B
 2.325163 with sigma of 0.02
 O56B-O57B
 2.325163 with sigma of 0.02
 O56B-O58B
 2.325163 with sigma of 0.02
 O57B-O58B
 2.325163 with sigma of 0.02
3. Others
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: Cl5A(0.9) O55A(0.9) O56A(0.9) O57A(0.9) O58A(0.9) Cl5B(0.1)
 O56B(0.1) O58B(0.1) O57B(0.1) O55B(0.1)
4.a Ternary CH refined with riding coordinates:
 C10(H10), C21(H21)
4.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C22(H22A,H22B)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18),
 C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C32(H32), C33(H33), C34(H34),
  C39(H39), C40(H40), C41(H41), C42(H42), N44(H44), C48(H48), C49(H49),
 C50(H50), C51(H51), N53(H53)
;
_shelx_res_checksum              70699
_olex2_submission_special_instructions 'No special instructions were received'