Crystal structure of bis(bis{μ~3~-3-methyl-3-[(4-nitro-2-oxidobenzylidene)amino]propane-1,3-diolato}tris[chlorido(dimethyl sulfoxide)iron(III)]) dimethyl sulfoxide heptasolvate dihydrate
Chygorin, Eduard; Smal, Yuri; Omelchenko, Irina V.; Acta Crystallographica Section E 72 (2016) 1848–1851; doi:10.1107/S2056989016018508

data_2241964
_publ_section_title
;
 Crystal structure of
 bis(bis{\m~3~-3-methyl-3-[(4-nitro-2-oxidobenzylidene)amino]propane-1,3-diolato}tris[chlorido(dimethyl
 sulfoxide)iron(III)]) dimethyl sulfoxide heptasolvate dihydrate
;
_journal_coeditor_code           BG2596
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1848
_journal_page_last               1851
_journal_paper_doi               10.1107/S2056989016018508
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac
'[Fe3 (C11 H11 N2 O5)2 Cl3 (C2 H6 O S)3]2, 7C2 H6 O S, 2H2 O'
_chemical_formula_moiety
'2(C28 H40 Cl3 Fe3 N4 O13 S3), 7(C2 H6 O S), 2(H2 O)'
_chemical_formula_sum            'C70 H126 Cl6 Fe6 N8 O35 S13'
_chemical_formula_weight         2604.36
_chemical_name_systematic
;Bis(bis{\m~3~-3-methyl-3-[(4-nitro-2-oxidobenzylidene)amino]propane-1,3-diolato}tris[chlorido(dimethyl sulfoxide)iron(III)]) dimethyl sulfoxide
heptasolvate dihydrate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                94.005(5)
_cell_angle_beta                 105.839(6)
_cell_angle_gamma                103.952(6)
_cell_formula_units_Z            1
_cell_length_a                   11.4286(7)
_cell_length_b                   12.7227(8)
_cell_length_c                   20.1915(12)
_cell_measurement_reflns_used    2112
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.9198
_cell_measurement_theta_min      2.7912
_cell_volume                     2712.0(3)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2012)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2012)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2012)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 16.1827
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.847
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0847
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            21211
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.984
_diffrn_reflns_theta_min         2.797
_exptl_absorpt_coefficient_mu    1.257
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98472
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2012)
;
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_description       block
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.960
_refine_diff_density_min         -0.786
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         12221
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.1824
_refine_ls_R_factor_gt           0.0811
_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^)+(0.0472P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1273
_refine_ls_wR_factor_ref         0.1634
_reflns_number_gt                6081
_reflns_number_total             12221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bg2596sup1.cif
_cod_data_source_block           I
_cod_database_code               2241964
_cod_database_fobs_code          2241964
_shelx_estimated_absorpt_t_min   0.633
_shelx_estimated_absorpt_t_max   0.633