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_7017816
_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         'C61 H67 Fe5 N4 O20, C2 H3 N'
_chemical_formula_sum            'C63 H70 Fe5 N5 O20'
_chemical_formula_weight         1496.49
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.4364(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2398(2)
_cell_length_b                   25.8362(4)
_cell_length_c                   21.8856(3)
_cell_measurement_reflns_used    17765
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4999
_cell_measurement_theta_min      3.0162
_cell_volume                     6918.71(18)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0481
_diffrn_reflns_av_sigmaI/netI    0.0783
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            55637
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    1.097
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.874
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Empirical absorption correction (CrysAlis RED, Oxford Diffraction)'
_exptl_crystal_colour            grey-brown
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3092
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;
The crystal structure contains a second acetonitrile
molecule of crystallization which was highly disordered;
attemps to model it with a chemically reasonable geometry
were unsuccessful. 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 this
solvent molecule from the intensity data. The solvent-free model
and intensity data were used for the final results reported here.
;
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.912
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     873
_refine_ls_number_reflns         15800
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      0.914
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0322P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0747
_reflns_number_gt                10049
_reflns_number_total             15800
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c1dt11487e.txt
_cod_data_source_block           ck7-sqz
_cod_database_code               7017816