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_7716345
_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         'C17 H14 Br2 Fe N6 S2'
_chemical_formula_sum            'C17 H14 Br2 Fe N6 S2'
_chemical_formula_weight         582.13
_chemical_name_common            '[Fe(II) (LBrpyridine) (NCS)2]'
_chemical_name_systematic
'iron(II) thiocyanate complex of tetradentate Schiff base ligand'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-10
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-03-21 deposited with the CCDC.	2024-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                72.401(4)
_cell_angle_beta                 88.978(4)
_cell_angle_gamma                85.259(4)
_cell_formula_units_Z            2
_cell_length_a                   8.3520(4)
_cell_length_b                   11.5772(5)
_cell_length_c                   11.6323(4)
_cell_measurement_reflns_used    7242
_cell_measurement_temperature    99.9(3)
_cell_measurement_theta_max      74.3560
_cell_measurement_theta_min      3.9060
_cell_volume                     1068.42(8)
_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      99.9(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1725
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.973
_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   -115.00 -14.00   1.00    1.00    --  -41.79 -57.00  30.00  101
  2  \w   -116.00 -17.00   1.00    1.00    --  -41.79 -38.00 120.00   99
  3  \w    -21.00  74.00   1.00    1.00    --   41.79 -77.00-120.00   95
  4  \w      8.00  42.00   1.00    1.00    --   41.79  81.00  14.49   34
  5  \w      8.00  42.00   1.00    1.00    --   41.79  82.00 130.91   34
  6  \w     26.00 107.00   1.00    1.67    --  108.46 -95.00  60.00   81
  7  \w     37.00 112.00   1.00    1.67    --  108.46-125.00 -90.00   75
  8  \w     32.00 141.00   1.00    1.67    --  108.46 -77.00  60.00  109
  9  \w    103.00 178.00   1.00    1.67    --  108.46  77.00-120.00   75
 10  \w    103.00 178.00   1.00    1.67    --  108.46  77.00 -90.00   75
 11  \w     37.00 112.00   1.00    1.67    --  108.46-125.00  60.00   75
 12  \w     32.00 137.00   1.00    1.67    --  108.46 -30.00  90.00  105
 13  \w     35.00 134.00   1.00    1.67    --  108.46 -45.00-150.00   99
 14  \w     26.00 107.00   1.00    1.67    --  108.46 -95.00-120.00   81
 15  \w     26.00 107.00   1.00    1.67    --  108.46 -95.00 -30.00   81
 16  \w     27.00 161.00   1.00    1.67    --  108.46 -15.00 -90.00  134
 17  \w    -83.00  38.00   1.00    1.00    --  -41.79  19.00 150.00  121
 18  \w      8.00  34.00   1.00    1.00    --   41.79  83.00-144.12   26
 19  \w      9.00  42.00   1.00    1.00    --   41.79  79.00 -70.97   33
 20  \w     17.00 116.00   1.00    1.00    --   41.79  38.00   0.00   99
 21  \w     58.00 129.00   1.00    1.00    --   41.79-178.00 120.00   71
 22  \w     80.00 178.00   1.00    1.67    --  108.46  30.00   0.00   98
 23  \w     83.00 178.00   1.00    1.67    --  108.46  45.00 120.00   95
 24  \w     80.00 178.00   1.00    1.67    --  108.46  30.00  90.00   98
 25  \w     79.00 178.00   1.00    1.67    --  108.46  61.00-150.00   99
 26  \w     79.00 178.00   1.00    1.67    --  108.46  61.00  30.00   99
 27  \w     79.00 178.00   1.00    1.67    --  108.46  61.00 -90.00   99
 28  \w     79.00 152.00   1.00    1.67    --  108.46  61.00 -60.00   73
 29  \w     56.00 178.00   1.00    1.67    --  108.46  15.00-150.00  122
;
_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      -0.0385758000
_diffrn_orient_matrix_UB_12      0.1364809000
_diffrn_orient_matrix_UB_13      -0.0162860000
_diffrn_orient_matrix_UB_21      0.1767112000
_diffrn_orient_matrix_UB_22      0.0227408000
_diffrn_orient_matrix_UB_23      -0.0322922000
_diffrn_orient_matrix_UB_31      -0.0392953000
_diffrn_orient_matrix_UB_32      0.0217601000
_diffrn_orient_matrix_UB_33      -0.1341554000
_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  0.0855
_diffrn_reflns_av_unetI/netI     0.0571
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16171
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.079
_diffrn_reflns_theta_min         3.987
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.002
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.370
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_description       plate
_exptl_crystal_F_000             572
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Crystallised from methanol reaction solution on standing'
_exptl_crystal_size_max          0.354
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.069
_refine_diff_density_max         2.588
_refine_diff_density_min         -1.064
_refine_diff_density_rms         0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4300
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0671
_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^)+(0.1343P)^2^+1.6255P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1822
_refine_ls_wR_factor_ref         0.1980
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3572
_reflns_number_total             4300
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00884g2.cif
_cod_data_source_block           mgr464_2_auto
_cod_depositor_comments
'Adding full bibliography for 7716343--7716348.cif.'
_cod_database_code               7716345
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         CHNBrFeS
_chemical_oxdiff_usercomment     M1017
_shelx_estimated_absorpt_t_max   0.491
_shelx_estimated_absorpt_t_min   0.101
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C9(H9A,H9B), C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C1(H1), C6(H6), C3(H3), C10(H10), C4(H4), C13(H13), C12(H12)
;
_shelx_res_checksum              65765
_shelx_hkl_checksum              34120
_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 3.478
_oxdiff_exptl_absorpt_empirical_full_min 0.428