μ-Oxo-bis[(diethyl 6,17-dimethyldibenzo[<i>a</i>,<i>h</i>]-5,9,14,18-tetraaza[14]annulene-7,16-dicarboxylato)iron(III)] sesquihydrate
Jäger, Ernst-Gottfried; Knaudt, Jutta; Imhof, Wolfgang; Acta Crystallographica Section E 62 (2006) m492–m495; doi:10.1107/S1600536806004636

data_2208337
_publ_section_title
;\m-Oxo-bis[(diethyl
 6,17-dimethyldibenzo[<i>a</i>,<i>h</i>]-5,9,14,18-tetraaza[14]annulene-7,16-dicarboxylato)iron(III)]
 sesquihydrate
;
_journal_coeditor_code           HG2003
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m492
_journal_page_last               m495
_journal_paper_doi               10.1107/S1600536806004636
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Fe2 (C26 H26 N4 O4) O], 1.5H2 O1'
_chemical_formula_moiety         'C52 H52 Fe2 N8 O9, 1.5H2 O1'
_chemical_formula_sum            'C52 H55 Fe2 N8 O10.5'
_chemical_formula_weight         1071.72
_chemical_name_systematic
;
\m-oxo-bis{[4,15-bis(ethoxycarbonyl)-5,14-dimethyl-2,7,13,17-
tetraazatricyclo[16.4.0.0^7,12^]docosa-3,5,7,9,11,13,15,18(1),19,21-decaene-
2,17-diido]iron(III)} sesquihydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 111.26(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.322(6)
_cell_length_b                   13.494(4)
_cell_length_c                   29.838(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      20.1
_cell_volume                     10252(4)
_computing_cell_refinement       'SET4 (Boer et al., 1984)'
_computing_data_collection       'CAD-4 EXPRESS (Enraf--Nonius, 1994)'
_computing_data_reduction        'MolEN (Nonius, 1990)'
_computing_molecular_graphics    'XP (Siemens, 1990)'
_computing_publication_material  XP
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            9161
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        3.64
_diffrn_standards_interval_time  600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.634
_exptl_absorpt_correction_T_max  0.8299
_exptl_absorpt_correction_T_min  0.7760
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North <i>et al.</i>,  1968)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             4448
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.738
_refine_diff_density_min         -0.515
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     681
_refine_ls_number_reflns         8963
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0507P)^2^+35.0302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1314
_reflns_number_gt                6718
_reflns_number_total             8963
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg2003.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2208337
_cod_database_fobs_code          2208337