Synthesis and crystal structure of hydrated μ-oxalato-bis{bis[3-methyl-5-(pyridin-2-yl)-1<i>H</i>-1,2,4-triazole]iron(II)} bis(toluenesulfonate) 2.75-hydrate
Petrenko, Yuliia P.; Bibik, Yurii S.; Khomenko, Dmytro M.; Doroshchuk, Roman O.; Gural'skiy, Il`ya A.; Shova, Sergiu; Lampeka, Rostyslav D.; Raspertova, Ilona V.; Acta Crystallographica Section E 78 (2022) –; doi:10.1107/S2056989022007460

data_2244135
_publ_section_title
;
 Synthesis and crystal structure of hydrated
 \m-oxalato-bis{bis[3-methyl-5-(pyridin-2-yl)-1<i>H</i>-1,2,4-triazole]iron(II)}
 bis(toluenesulfonate) 2.75-hydrate
;
_journal_coeditor_code           VM2269
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989022007460
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac
'[Fe2 (C2 O4) (C8 H8 N4)4] (C7 H7 O3 S1)2, 2.75H2 O'
_chemical_formula_moiety
'C34 H32 Fe2 N16 O4 2+, 2(C7 H7 O3 S -), 2.75(H2 O)'
_chemical_formula_sum            'C48 H51.5 Fe2 N16 O12.75 S2'
_chemical_formula_weight         1232.37
_chemical_name_systematic
'\m-Oxalato-\k^4^<i>O</i>^1^,<i>O</i>^2^:<i>O</i>^1'^,<i>O</i>^2'^-bis{bis[3-methyl-5-(pyridin-2-yl)-1<i>H</i>-1,2,4-triazole-\k^2^<i>N</i>^4^,<i>N</i>^5^]iron(II)} bis(toluenesulfonate) 2.75-hydrate'
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_cell_angle_alpha                96.736(4)
_cell_angle_beta                 101.490(4)
_cell_angle_gamma                95.216(4)
_cell_formula_units_Z            2
_cell_length_a                   9.9635(4)
_cell_length_b                   14.4905(6)
_cell_length_c                   20.1131(8)
_cell_measurement_reflns_used    5996
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.2330
_cell_measurement_theta_min      1.9810
_cell_volume                     2806.5(2)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT  (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0797
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0578
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20140
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.645
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.667
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92320
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2021)
;
_exptl_crystal_colour            'clear light brown'
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_description       block
_exptl_crystal_F_000             1275
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.523
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         9886
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0582
_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^)+(0.0447P)^2^+1.2466P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1318
_reflns_number_gt                7117
_reflns_number_total             9886
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vm2269sup1.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C48 H51.50 Fe2 N16 O12.75 S2'
_cod_database_code               2244135
_shelx_estimated_absorpt_t_min   0.800
_shelx_estimated_absorpt_t_max   0.907
_shelx_hkl_checksum              52248
_shelx_res_checksum              21218
_cod_database_fobs_code 2244135