Pentanuclear complexes with unusual structural topologies from the initial use of two aliphatic amino-alcohol ligands in Fe chemistry.
Kizas, Christos M.; Manos, Manolis J.; Nastopoulos, Vassilios; Boudalis, Athanassios K.; Sanakis, Yiannis; Tasiopoulos, Anastasios J.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 1544–1552; doi:10.1039/c1dt11487e

data_7017815
_publ_section_title
;
 Pentanuclear complexes with unusual structural topologies from the
 initial use of two aliphatic amino-alcohol ligands in Fe chemistry.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1544
_journal_page_last               1552
_journal_paper_doi               10.1039/c1dt11487e
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C47 H95 Fe5 N4 O20'
_chemical_formula_sum            'C47 H95 Fe5 N4 O20'
_chemical_formula_weight         1315.52
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.0880(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.3966(2)
_cell_length_b                   19.0674(3)
_cell_length_c                   19.9009(3)
_cell_measurement_reflns_used    13541
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.4088
_cell_measurement_theta_min      3.1041
_cell_volume                     6564.06(16)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2008)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2008)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2008)'
_computing_molecular_graphics
;
PLATON (Spek, 2008), ORTEP-3 (Farrugia, 1997)
;
_computing_publication_material  'WINGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0288
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Oxford Diffraction Xcalibur-3 with Sapphire CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_sigmaI/netI    0.0988
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            53073
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    1.144
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Empirical absorption correction (CrysAlis RED, Oxford Diffraction)'
_exptl_crystal_colour            'translucent brown-purple'
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2780
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;
The crystal structure contains lattice water molecules which
appear to be highly disordered and it was not possible to model
their position and distribution reliably. Therefore, the SQUEEZE
procedure of PLATON (van der Sluis & Spek, 1990; Spek, 2001)
was employed to remove the contribution of the electron density
associated with the disordered solvent from the intensity data.
The solvent-free model and intensity data were used for the final
results reported here.
;
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.882
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     730
_refine_ls_number_reflns         15054
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      0.886
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0334P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0822
_reflns_number_gt                8602
_reflns_number_total             15054
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c1dt11487e.txt
_cod_data_source_block           ck3-sqz
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geom & difmap' was changed to
'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
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_cod_database_code               7017815