Exceptionally high temperature spin crossover in amide-functionalised 2,6-bis(pyrazol-1-yl)pyridine iron(ii) complex revealed by variable temperature Raman spectroscopy and single crystal X-ray diffraction.
Attwood, Max; Akutsu, Hiroki; Martin, Lee; Blundell, Toby J.; Le Maguere, Pierre; Turner, Scott S.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 11843–11851; doi:10.1039/d1dt01743h

data_7707941
_publ_section_title
;
 Exceptionally high temperature spin crossover in amide-functionalised
 2,6-bis(pyrazol-1-yl)pyridine iron(ii) complex revealed by variable
 temperature Raman spectroscopy and single crystal X-ray diffraction.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11843
_journal_page_last               11851
_journal_paper_doi               10.1039/d1dt01743h
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         '2(C12 H10 N6 O) Fe, 2(B F4)'
_chemical_formula_sum            'C24 H20 B2 F8 Fe N12 O2'
_chemical_formula_weight         737.96
_chemical_name_systematic
'bis[2,6-bis(1H-pyrazol-1-yl)pyridine-4-carboxamide]-iron bis[tetrafluoridoborate]'
_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     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2021-07-05 deposited with the CCDC.	2021-07-28 downloaded from the CCDC.
;
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_cell_angle_beta                 109.620(8)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
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_cell_length_b                   32.5863(6)
_cell_length_c                   10.5351(2)
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_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      1.88
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_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
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_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_diffrn_ambient_temperature      290
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_Laue_measured_fraction_full 1.000
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_diffrn_reflns_limit_h_max       11
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_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            29045
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.444
_diffrn_reflns_theta_min         2.145
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.601
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_correction_T_min  0.853
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_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1488.00
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH3NO2 and Et2O'
_exptl_crystal_size_max          0.180
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_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.35
_refine_diff_density_min         -0.30
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     514
_refine_ls_number_reflns         6819
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0440P)^2^+1.8113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0967
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5627
_reflns_number_total             6819
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d1dt01743h2.cif
_cod_data_source_block           M171020A
_cod_depositor_comments
'Adding full bibliography for 7707940--7707943.cif.'
_cod_original_cell_volume        2992.66(17)
_cod_database_code               7707941
_shelx_res_checksum              87319
_shelx_hkl_checksum              9212