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_7709642
_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 ab
_chemical_formula_moiety         'C36 H36 Fe N8 O2, 2(Cl O4)'
_chemical_formula_sum            'C36 H36 Cl2 Fe N8 O10'
_chemical_formula_weight         867.48
_chemical_name_systematic
'[2,6-Bis((S)-4-isopropyl-4,5-dihydrooxazol-2-yl)pyridine]-[2,6-bis(1H-benzimidazol-2-yl)pyridine]iron(II) diperchlorate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-09-08
_audit_creation_method
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_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
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1310(5)
_cell_length_b                   19.1776(10)
_cell_length_c                   19.2647(10)
_cell_measurement_reflns_used    6457
_cell_measurement_temperature    120.02(16)
_cell_measurement_theta_max      72.87
_cell_measurement_theta_min      4.58
_cell_volume                     3742.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.02(16)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -53.00  24.00   1.00    1.00    --  -38.50  37.00 -30.00   77
  2  \w   -107.00 -18.00   1.00    1.00    --  -38.50 -57.00 -30.00   89
  3  \w     82.00 115.00   1.00    4.00    --  104.98 -61.00 -30.00   33
  4  \w     56.00 117.00   1.00    4.00    --  104.98 -65.00 -66.57   61
  5  \w     45.00 128.00   1.00    4.00    --  104.98 -15.00 -60.00   83
  6  \w     98.00 171.00   1.00    4.00    --  104.98  30.00 150.00   73
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0122214000
_diffrn_orient_matrix_UB_12      -0.0765764000
_diffrn_orient_matrix_UB_13      0.0374918000
_diffrn_orient_matrix_UB_21      0.0793887000
_diffrn_orient_matrix_UB_22      0.0125203000
_diffrn_orient_matrix_UB_23      -0.0003516000
_diffrn_orient_matrix_UB_31      -0.0030393000
_diffrn_orient_matrix_UB_32      0.0194848000
_diffrn_orient_matrix_UB_33      0.1472406000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9691
_diffrn_reflns_point_group_measured_fraction_full 0.870
_diffrn_reflns_point_group_measured_fraction_max 0.854
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.718
_diffrn_reflns_theta_min         3.252
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.147
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             1792
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetone/diethyl ether'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.950
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details
;
 Flack x determined using 2240 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         6463
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0533
_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^)+(0.0763P)^2^+4.5119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1396
_refine_ls_wR_factor_ref         0.1426
_reflns_Friedel_coverage         0.591
_reflns_Friedel_fraction_full    0.738
_reflns_Friedel_fraction_max     0.719
_reflns_number_gt                6287
_reflns_number_total             6463
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00393g2.cif
_cod_data_source_block           kb-054
_cod_database_code               7709642
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.644(2)
 0.356(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C18-C21A = C21A-C22A = C21A-C23A = C18-C21B = C21B-C22B = C21B-C23B
 1.53415 with sigma of 0.02
 C18-C22A = C18-C23A = C22A-C23A = C18-C22B = C18-C23B = C22B-C23B
 2.505267 with sigma of 0.02
4. Others
 1(DFIX)=FVAR(1)
 1(DFIX)=1.633*FVAR(2)
 Fixed Sof: H18(0.5) H18A(0.5) C21A(0.5) H21A(0.5) C22A(0.5) H22A(0.5)
 H22B(0.5) H22C(0.5) C23A(0.5) H23A(0.5) H23B(0.5) H23C(0.5) C21B(0.5)
 H21B(0.5) C22B(0.5) H22D(0.5) H22E(0.5) H22F(0.5) C23B(0.5) H23D(0.5)
 H23E(0.5) H23F(0.5)
5.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C18(H18), C18(H18A), C21A(H21A), C21B(H21B)
5.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C19(H19A,H19B)
5.c Me refined with riding coordinates:
 C22A(H22A,H22B,H22C), C23A(H23A,H23B,H23C), C22B(H22D,H22E,H22F), C23B(H23D,
 H23E,H23F)
5.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C26(H26), C27(H27), C28(H28), C33(H33), C34(H34),
 C35(H35), C36(H36), N38(H38), C42(H42), C43(H43), C44(H44), C45(H45), N47(H47)
5.e Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              33573
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.348
_oxdiff_exptl_absorpt_empirical_full_min 0.837