Syntheses and crystal structures of three [<i>M</i>(acac)~2~(TMEDA)] complexes (<i>M</i> = Mn, Fe and Zn)
Halz, Jan Henrik; Heiser, Christian; Wagner, Christoph; Merzweiler, Kurt; Acta Crystallographica Section E 76 (2020) 66–71; doi:10.1107/S2056989019016372

data_2243219
_publ_section_title
;
 Syntheses and crystal structures of three [<i>M</i>(acac)~2~(TMEDA)]
 complexes (<i>M</i> = Mn, Fe and Zn)
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              66
_journal_page_last               71
_journal_paper_doi               10.1107/S2056989019016372
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          '[Fe (C5 H7 O2)2 (C6 H16 N2)]'
_chemical_formula_moiety         'C16 H30 Fe N2 O4'
_chemical_formula_sum            'C16 H30 Fe N2 O4'
_chemical_formula_weight         370.27
_chemical_name_systematic
Bis(acetylacetonato-\k^2^<i>O</i>,<i>O</i>')(<i>N</i>,<i>N</i>,<i>N</i>',<i>N</i>'-tetramethylethylenediamine-\k^2^<i>N</i>,<i>N</i>')iron(II)
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.382(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2021(3)
_cell_length_b                   15.4708(4)
_cell_length_c                   12.4881(4)
_cell_measurement_reflns_used    16780
_cell_measurement_temperature    213
_cell_measurement_theta_max      29.56
_cell_measurement_theta_min      1.64
_cell_volume                     1962.37(10)
_computing_cell_refinement
;
X-AREA  (Stoe & Cie, 2016)
;
_computing_data_collection
;
X-AREA  (Stoe & Cie, 2016)
;
_computing_data_reduction
;
X-AREA  (Stoe & Cie, 2016)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2019)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
<i>SHELXL2014/7</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014/7</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      213
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18586
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.268
_diffrn_reflns_theta_min         2.101
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.787
_exptl_absorpt_correction_T_max  0.8942
_exptl_absorpt_correction_T_min  0.8137
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(X-AREA; Stoe & Cie, 2016)
;
_exptl_crystal_colour            'clear reddish brown'
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.263
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.231
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.224
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         5276
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0464P)^2^+0.3681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0862
_reflns_number_gt                4425
_reflns_number_total             5276
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5524sup1.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2243219
_cod_database_fobs_code          2243219
_shelx_estimated_absorpt_t_min   0.820
_shelx_estimated_absorpt_t_max   0.839
_shelx_hkl_checksum              72340
_shelx_res_checksum              61521