Synthesis and structural, magnetic and spectroscopic characterization of iron(III) complexes with <i>in situ</i> formed ligands from methyl-2-pyridyl ketone transformations.
Tzani, Sofia; Pissas, Michael; Psycharis, Vassilis; Pantazis, Dimitrios A.; Sanakis, Yiannis; Raptopoulou, Catherine P.; Dalton transactions (Cambridge, England : 2003) 52 (2023) 1582–1594; doi:10.1039/d2dt03944c

data_7712155
_publ_section_title
;
 Synthesis and structural, magnetic and spectroscopic characterization of
 iron(III) complexes with <i>in situ</i> formed ligands from
 methyl-2-pyridyl ketone transformations.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1582
_journal_page_last               1594
_journal_paper_doi               10.1039/d2dt03944c
_journal_volume                  52
_journal_year                    2023
_chemical_formula_sum            'C24 H32.4 Cl4 Fe3 N3 O8.2'
_chemical_formula_weight         803.48
_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
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2022-12-07 deposited with the CCDC.	2023-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                112.9060(10)
_cell_angle_beta                 101.9300(10)
_cell_angle_gamma                105.5150(10)
_cell_formula_units_Z            2
_cell_length_a                   11.0768(2)
_cell_length_b                   12.9640(2)
_cell_length_c                   13.9148(3)
_cell_measurement_reflns_used    17569
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      71.88
_cell_measurement_theta_min      6.52
_cell_volume                     1661.22(6)
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_molecular_graphics    'Diamond ver.3.1'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.834
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       '\q scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0830
_diffrn_reflns_av_unetI/netI     0.0870
_diffrn_reflns_Laue_measured_fraction_full 0.834
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21930
_diffrn_reflns_point_group_measured_fraction_full 0.834
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         62.491
_diffrn_reflns_theta_min         6.525
_exptl_absorpt_coefficient_mu    13.743
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.334
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            orange-brown
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             818
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.836
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         5011
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0329P)^2^+10.0246P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1591
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3356
_reflns_number_total             5011
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03944c2.cif
_cod_data_source_block           shelxl_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7712154--7712155.cif.'
_cod_original_cell_volume        1661.21(6)
_cod_original_formula_sum        'C24 H32.40 Cl4 Fe3 N3 O8.20'
_cod_database_code               7712155
_shelxl_version_number           2014/6
_shelx_res_checksum              95677