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_7712154
_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            'C31.8 H33.7 Cl6 Fe4 N4.7 O6.4'
_chemical_formula_weight         1020.23
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   34.0344(2)
_cell_length_b                   34.0344(2)
_cell_length_c                   21.8653(3)
_cell_measurement_reflns_used    23647
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      71.87
_cell_measurement_theta_min      6.61
_cell_volume                     21934.2(4)
_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      170(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.991
_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  0.1231
_diffrn_reflns_av_unetI/netI     0.0852
_diffrn_reflns_Laue_measured_fraction_full 0.932
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            32103
_diffrn_reflns_point_group_measured_fraction_full 0.932
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         64.994
_diffrn_reflns_theta_min         6.607
_exptl_absorpt_coefficient_mu    12.726
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.088
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             9263
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.679
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         4124
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0553
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0751P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1583
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3032
_reflns_number_total             4124
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03944c2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 7712154--7712155.cif.'
_cod_original_formula_sum        'C31.80 H33.70 Cl6 Fe4 N4.70 O6.40'
_cod_database_code               7712154
_shelxl_version_number           2014/6
_shelx_res_checksum              45592