Structural, magnetic and Mössbauer spectroscopic studies of the [Fe(3-bpp)2](CF3COO)2 complex: role of crystal packing leading to an incomplete Fe(ii) high spin ⇋ low spin transition
Sugiyarto, Kristian Handoyo; Onggo, Djulia; Akutsu, Hiroki; Reddy, Varimalla Raghavendra; Sutrisno, Hari; Nakazawa, Yasuhiro; Bhattacharjee, Ashis; CrystEngComm 23 (2021) 2854–2861; doi:10.1039/D0CE01687J

data_7242377
_publ_section_title
;
 Structural, magnetic and M\"ossbauer spectroscopic studies of the
 [Fe(3-bpp)2](CF3COO)2 complex: role of crystal packing leading to an
 incomplete Fe(ii) high spin &#x21CB; low spin transition
;
_journal_issue                   15
_journal_name_full               CrystEngComm
_journal_page_first              2854
_journal_page_last               2861
_journal_paper_doi               10.1039/D0CE01687J
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C22 H18 Fe N10, 2(C2 F3 O2)'
_chemical_formula_sum            'C26 H18 F6 Fe N10 O4'
_chemical_formula_weight         704.33
_chemical_name_common            '[Fe(bpp)2](TFA)2'
_chemical_name_systematic        '[Fe(bpp)2](CF3COO)2'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc27645s
_audit_update_record
;
2021-02-06 deposited with the CCDC.	2021-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 92.151(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   19.2114(7)
_cell_length_b                   21.9406(9)
_cell_length_c                   13.9778(5)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    200
_cell_measurement_theta_max      31.10
_cell_measurement_theta_min      1.99
_cell_volume                     5887.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_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    'SHELXT Version 2018/2 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'XtaLAB Synergy Custom Hipix Micromax-007'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18053
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.056
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.602
_exptl_absorpt_correction_T_max  0.871
_exptl_absorpt_correction_T_min  0.699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.75a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2848.00
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'The aquaous solution was left over few days at RT'
_exptl_crystal_size_max          0.750
_exptl_crystal_size_mid          0.480
_exptl_crystal_size_min          0.230
_refine_diff_density_max         0.81
_refine_diff_density_min         -0.57
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     437
_refine_ls_number_reflns         6668
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0660P)^2^+5.2791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1199
_refine_ls_wR_factor_ref         0.1264
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5492
_reflns_number_total             6668
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d0ce01687j2.cif
_cod_data_source_block           xcalibur
_cod_depositor_comments
'Adding full bibliography for 7242376--7242379.cif.'
_cod_database_code               7242377
_shelx_res_checksum              32708
_shelx_hkl_checksum              71997