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_7709646
_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         'C42 H32 Fe N8 O2, 2(Cl O4), C2 H3 N'
_chemical_formula_sum            'C44 H35 Cl2 Fe N9 O10'
_chemical_formula_weight         976.56
_chemical_name_systematic
'[2,6-Bis((R)-4-phenyl-4,5-dihydrooxazol-2-yl)pyridine]- [2,6-Bis(benzimidazol-2-yl)pyridine]iron(II) diperchlorate  acetonitrile solvate'
_space_group_crystal_system      tetragonal
_space_group_IT_number           76
_space_group_name_Hall           'P 4w'
_space_group_name_H-M_alt        'P 41'
_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            8
_cell_length_a                   10.6379(1)
_cell_length_b                   10.6379(1)
_cell_length_c                   73.8154(8)
_cell_measurement_reflns_used    13278
_cell_measurement_temperature    130.00(10)
_cell_measurement_theta_max      72.0270
_cell_measurement_theta_min      4.1710
_cell_volume                     8353.31(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_molecular_graphics    'X-Seed (Barbour, 2001)'
_computing_publication_material  'Olex2 1.3 (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      130.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.982
_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    -63.00  28.50   0.75    5.17    --  -41.04  37.00 -30.00  122
  2  \w    -26.00   9.25   0.75    5.17    --  -41.04  37.00  60.00   47
  3  \w   -103.00 -16.00   0.75    5.17    --  -41.04 -57.00  30.00  116
  4  \w     39.00 132.00   0.75   20.70    --  103.83 -61.00  60.00  124
  5  \w     96.00 141.00   0.75   20.70    --  103.83  15.00  30.00   60
  6  \w    134.00 174.50   0.75   20.70    --  103.83  45.00 150.00   54
  7  \w    101.00 127.25   0.75   20.70    --  103.83 -45.00-150.00   35
  8  \w     62.00  88.25   0.75   20.70    --  103.83  15.00  30.00   35
  9  \w     76.00 175.00   0.75   20.70    --  103.83  30.00-120.00  132
 10  \w     22.00 102.25   0.75   20.70    --  103.83 -15.00  60.00  107
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0440479000
_diffrn_orient_matrix_UB_12      -0.0408032000
_diffrn_orient_matrix_UB_13      -0.0189960000
_diffrn_orient_matrix_UB_21      -0.0722844000
_diffrn_orient_matrix_UB_22      0.1245835000
_diffrn_orient_matrix_UB_23      -0.0020899000
_diffrn_orient_matrix_UB_31      0.1176839000
_diffrn_orient_matrix_UB_32      0.0611386000
_diffrn_orient_matrix_UB_33      -0.0083951000
_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  0.0532
_diffrn_reflns_av_unetI/netI     0.0797
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       89
_diffrn_reflns_limit_l_min       -90
_diffrn_reflns_number            32362
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         72.472
_diffrn_reflns_theta_min         3.593
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.698
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.834
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_description       needle
_exptl_crystal_F_000             4016
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile/diethyl ether'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.977
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Flack x determined using 5770 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1192
_refine_ls_number_reflns         16045
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0706
_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^)+42.6672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1558
_refine_ls_wR_factor_ref         0.1585
_reflns_Friedel_coverage         0.955
_reflns_Friedel_fraction_full    0.962
_reflns_Friedel_fraction_max     0.954
_reflns_number_gt                14875
_reflns_number_total             16045
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00393g2.cif
_cod_data_source_block           ns520
_cod_original_cell_volume        8353.31(18)
_cod_database_code               7709646
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9773(14)
 0.0227(14)
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. Uiso/Uaniso restraints and constraints
Uanis(C3A) \\sim Ueq, Uanis(C33A) \\sim Ueq, Uanis(C16B) \\sim Ueq, Uanis(O67)
\\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
4.a Ternary CH refined with riding coordinates:
 C10A(H10A), C21A(H21A), C10B(H10B), C21B(H21B)
4.b Secondary CH2 refined with riding coordinates:
 C11A(H11A,H11B), C22A(H22A,H22B), C11B(H11C,H11D), C22B(H22C,H22D)
4.c Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C5A(H5A), C6A(H6A), C14A(H14A), C15A(H15A), C16A(H16A), C17A(H17A),
 C18A(H18A), C25A(H25A), C26A(H26A), C27A(H27A), C28A(H28A), C29A(H29A),
 C32A(H32A), C33A(H33A), C34A(H34A), C39A(H39A), C40A(H40A), C41A(H41A),
 C42A(H42A), N44A(H44A), C48A(H48A), C49A(H49A), C50A(H50A), C51A(H51A),
 N53A(H53A), C4B(H4B), C5B(H5B), C6B(H6B), C14B(H14B), C15B(H15B), C16B(H16B),
 C17B(H17B), C18B(H18B), C25B(H25B), C26B(H26B), C27B(H27B), C28B(H28B),
 C29B(H29B), C32B(H32B), C33B(H33B), C34B(H34B), C39B(H39B), C40B(H40B),
 C41B(H41B), C42B(H42B), N44B(H44B), C48B(H48B), C49B(H49B), C50B(H50B),
 C51B(H51B), N53B(H53B)
4.d Idealised Me refined as rotating group:
 C74(H74A,H74B,H74C), C77(H77A,H77B,H77C)
;
_shelx_res_checksum              82852
_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 1.416
_oxdiff_exptl_absorpt_empirical_full_min 0.770