Iron(II) spin crossover complexes of tetradentate Schiff-bases: tuning <i>T</i><sub>1/2</sub> by choice of formyl-heterocycle component.
Robb, Matthew G.; Chong, Shen V.; Brooker, Sally; Dalton transactions (Cambridge, England : 2003) 53 (2024) 10974–10981; doi:10.1039/d4dt00884g

data_7716348
_publ_section_title
;
 Iron(II) spin crossover complexes of tetradentate Schiff-bases: tuning
 <i>T</i><sub>1/2</sub> by choice of formyl-heterocycle component.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10974
_journal_page_last               10981
_journal_paper_doi               10.1039/d4dt00884g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C13 H12 Fe N6 O2 S2'
_chemical_formula_sum            'C13 H12 Fe N6 O2 S2'
_chemical_formula_weight         404.26
_chemical_name_common            '[Fe(II) (L4oxazole) (NCS)2]'
_chemical_name_systematic
'iron(II) thiocyanate complex of tetradentate Schiff base ligand'
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-09
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-03-21 deposited with the CCDC.	2024-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.860(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.07340(10)
_cell_length_b                   8.1467(2)
_cell_length_c                   25.2676(5)
_cell_measurement_reflns_used    5725
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.2370
_cell_measurement_theta_min      5.5940
_cell_volume                     1655.91(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3449
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_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   -126.00 -37.00   1.00    1.00    --  -42.04 178.00 -90.00   89
  2  \w   -130.00 -39.00   1.00    1.00    --  -42.04-178.00 -30.00   91
  3  \w   -114.00 -14.00   1.00    1.00    --  -42.04 -57.00-120.00  100
  4  \w     32.00 133.00   1.00    3.05    --  104.32 -61.00-120.00  101
  5  \w    103.00 178.00   1.00    3.05    --  104.32  77.00 120.00   75
  6  \w    103.00 178.00   1.00    3.05    --  104.32  77.00-120.00   75
  7  \w     78.00 177.00   1.00    3.05    --  104.32  45.00  30.00   99
  8  \w     97.00 178.00   1.00    3.05    --  104.32 125.00 -60.00   81
  9  \w     97.00 178.00   1.00    3.05    --  104.32 125.00   0.00   81
 10  \w    103.00 178.00   1.00    3.05    --  104.32  77.00  90.00   75
 11  \w   -114.00 -14.00   1.00    1.00    --  -42.04 -57.00   0.00  100
 12  \w   -126.00 -37.00   1.00    1.00    --  -42.04 178.00  90.00   89
 13  \w   -114.00 -14.00   1.00    1.00    --  -42.04 -57.00 120.00  100
 14  \w     75.00 141.00   1.00    3.05    --  104.32  61.00 -60.00   66
 15  \w    103.00 178.00   1.00    3.05    --  104.32  77.00-180.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_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      0.1680361000
_diffrn_orient_matrix_UB_12      -0.0900839000
_diffrn_orient_matrix_UB_13      0.0005975000
_diffrn_orient_matrix_UB_21      0.0716711000
_diffrn_orient_matrix_UB_22      0.1440337000
_diffrn_orient_matrix_UB_23      -0.0303526000
_diffrn_orient_matrix_UB_31      0.0575665000
_diffrn_orient_matrix_UB_32      0.0830861000
_diffrn_orient_matrix_UB_33      0.0531077000
_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  0.0534
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            12392
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.682
_diffrn_reflns_theta_min         3.511
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.847
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.210
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_description       plate
_exptl_crystal_F_000             824
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Crystallised from methanol reaction solution on standing'
_exptl_crystal_size_max          0.586
_exptl_crystal_size_mid          0.247
_exptl_crystal_size_min          0.117
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3235
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0564P)^2^+0.3520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1005
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2809
_reflns_number_total             3235
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00884g2.cif
_cod_data_source_block           mgr412
_cod_depositor_comments
'Adding full bibliography for 7716343--7716348.cif.'
_cod_database_code               7716348
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         CHNOSFe
_chemical_oxdiff_usercomment     M852
_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
2. Restrained distances
 C5-C14 \\sim C7-C14 \\sim C6-C5 \\sim C7-C6
 with sigma of 0.02
3. Others
 Fixed Sof: H7AA(0.85) H7AB(0.85) H7BC(0.15) H7BD(0.15) H5AA(0.85) H5AB(0.85)
 H5BC(0.15) H5BD(0.15) C6(0.85) H6A(0.85) H6B(0.85) C14(0.15) H14A(0.15)
 H14B(0.15)
4.a Secondary CH2 refined with riding coordinates:
 C7(H7AA,H7AB), C7(H7BC,H7BD), C5(H5AA,H5AB), C5(H5BC,H5BD), C6(H6A,H6B),
 C14(H14A,H14B)
4.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C10(H10), C4(H4), C11(H11), C2(H2), C1(H1)
;
_shelx_res_checksum              80113
_shelx_hkl_checksum              31613
_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 2.870
_oxdiff_exptl_absorpt_empirical_full_min 0.464