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_7716346
_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 S4'
_chemical_formula_sum            'C13 H12 Fe N6 S4'
_chemical_formula_weight         436.38
_chemical_name_common            '[Fe(II) (L2thiazole) (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 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-30
_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                 93.712(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4981(3)
_cell_length_b                   22.9024(8)
_cell_length_c                   9.2014(3)
_cell_measurement_reflns_used    3914
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.3410
_cell_measurement_theta_min      5.1310
_cell_volume                     1787.08(11)
_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 0.999
_diffrn_measured_fraction_theta_max 0.977
_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    -66.00  33.00   1.00    3.31    --  -41.67  38.00-150.00   99
  2  \w   -114.00 -14.00   1.00    3.31    --  -41.67 -57.00-120.00  100
  3  \w     58.00 129.00   1.00    3.31    --   41.67-178.00 -90.00   71
  4  \w     78.00 177.00   1.00   13.24    --  104.32  45.00 -30.00   99
  5  \w     97.00 178.00   1.00   13.24    --  104.32 125.00  30.00   81
  6  \w     22.00 106.00   1.00   13.24    --  104.32 -95.00  60.00   84
  7  \w     52.00 178.00   1.00   13.24    --  104.32  15.00  90.00  126
  8  \w     97.00 178.00   1.00   13.24    --  104.32 125.00-120.00   81
  9  \w     97.00 178.00   1.00   13.24    --  104.32 125.00 120.00   81
 10  \w   -116.00 -17.00   1.00    3.31    --  -41.67 -38.00 120.00   99
 11  \w   -114.00 -14.00   1.00    3.31    --  -41.67 -57.00  30.00  100
 12  \w     52.00 178.00   1.00   13.24    --  104.32  15.00-120.00  126
 13  \w     32.00 133.00   1.00   13.24    --  104.32 -61.00 120.00  101
;
_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      -0.0781255000
_diffrn_orient_matrix_UB_12      -0.0069153000
_diffrn_orient_matrix_UB_13      -0.1548384000
_diffrn_orient_matrix_UB_21      0.1628639000
_diffrn_orient_matrix_UB_22      -0.0110289000
_diffrn_orient_matrix_UB_23      -0.0591565000
_diffrn_orient_matrix_UB_31      -0.0190856000
_diffrn_orient_matrix_UB_32      -0.0659996000
_diffrn_orient_matrix_UB_33      0.0260491000
_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  0.0480
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13089
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.640
_diffrn_reflns_theta_min         3.860
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.213
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.655
_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 violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_description       plate
_exptl_crystal_F_000             888
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Crystallised from methanol reaction solution on standing'
_exptl_crystal_size_max          0.209
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.069
_refine_diff_density_max         0.842
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3479
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0627P)^2^+4.1704P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1382
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2719
_reflns_number_total             3479
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00884g2.cif
_cod_data_source_block           mgr421
_cod_depositor_comments
'Adding full bibliography for 7716343--7716348.cif.'
_cod_database_code               7716346
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         CHNFeS
_chemical_oxdiff_usercomment     M875
_shelx_estimated_absorpt_t_max   0.512
_shelx_estimated_absorpt_t_min   0.203
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C6(H6A,H6B)
1.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C8(H8), C11(H11), C1(H1), C2(H2), C10(H10)
;
_shelx_res_checksum              47256
_shelx_hkl_checksum              35719
_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 2.278
_oxdiff_exptl_absorpt_empirical_full_min 0.690