Crystal structure of tetrakis(acetylacetonato)dichloridodi-μ~3~-methanolato-tetra-μ~2~-methanolato-tetrairon(III)
Richers, Casseday P.; Bertke, Jeffery A.; Gray, Danielle L.; Rauchfuss, Thomas B.; Acta Crystallographica Section E 71 (2015) 976–979; doi:10.1107/S2056989015013535

data_2240965
_publ_contact_author
;
Danielle L. Gray
University of Illinois
School of Chemical Sciences, Box 59-1
505 South Mathews Avenue
Urbana, Illinois  61801
USA
;
_publ_section_title
;
 Crystal structure of
 tetrakis(acetylacetonato)dichloridodi-\m~3~-methanolato-tetra-\m~2~-methanolato-tetrairon(III)
;
_journal_coeditor_code           CV5491
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              976
_journal_page_last               979
_journal_paper_doi               10.1107/S2056989015013535
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Fe4 (C5 H7 O2)4 (C H3 O)6 Cl2]'
_chemical_formula_moiety         'C26 H46 Cl2 Fe4 O14'
_chemical_formula_sum            'C26 H46 Cl2 Fe4 O14'
_chemical_formula_weight         876.93
_chemical_name_systematic
Tetrakis(acetylacetonato)dichloridodi-\m~3~-methanolato-tetra-\m~2~-methanolato-tetrairon(III)
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0714(6)
_cell_length_b                   12.1888(4)
_cell_length_c                   21.3543(7)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.39
_cell_volume                     3662.6(2)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013),
XPREP (Bruker, 2013),
SADABS (Bruker, 2012) and
TWINABS (Bruker, 2012)
;
_computing_molecular_graphics
;
SHELXTL (Bruker, 2013) and CrystalMaker (CrystalMaker, 2014)
;
_computing_publication_material
;
XCIF (Bruker, 2013) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXTL (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      102(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker D8 Venture/Photon 100'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            46682
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.331
_diffrn_reflns_theta_min         2.920
_exptl_absorpt_coefficient_mu    1.758
_exptl_absorpt_correction_T_max  0.7177
_exptl_absorpt_correction_T_min  0.5683
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2012)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.379
_exptl_crystal_size_mid          0.373
_exptl_crystal_size_min          0.232
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.336
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         4559
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0282
_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^)+(0.0352P)^2^+1.8648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0699
_reflns_number_gt                3837
_reflns_number_total             4559
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cv5491sup1.cf
_cod_data_source_block           I
_cod_database_code               2240965
_shelx_estimated_absorpt_t_min   0.555
_shelx_estimated_absorpt_t_max   0.686
_shelx_hkl_checksum              4311
_shelx_res_checksum              21524
_shelxl_version_number           2014/6
_cod_database_fobs_code 2240965