Linking [FeIII3] triangles with "double-headed" phenolic oximes
Brechin, Euan; Chem.Commun. 47 (2011) 6018–; doi:10.1039/c1cc11146a

data_7106443
_publ_section_title
;
 Linking [FeIII3] triangles with "double-headed" phenolic oximes
;
_journal_coden_Cambridge         0182
_journal_name_full               Chem.Commun.
_journal_page_first              6018
_journal_paper_doi               10.1039/c1cc11146a
_journal_volume                  47
_journal_year                    2011
_chemical_compound_source        'Kevin Mason'
_chemical_formula_moiety
'[Fe7O2(OH)6(oxyme)3(Py)6][BF4]5.14(MeOH).6(H2O)'
_chemical_formula_sum            'C140 H242 B5 F20 Fe7 N18 O40'
_chemical_formula_weight         3642.50
_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
_audit_creation_date             11-01-14
_audit_creation_method           CRYSTALS_ver_14.05
_cell_angle_alpha                90
_cell_angle_beta                 94.336(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9480(11)
_cell_length_b                   32.864(2)
_cell_length_c                   31.135(2)
_cell_measurement_reflns_used    8055
_cell_measurement_temperature    150
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     17291.9(19)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.106
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            110344
_diffrn_reflns_theta_full        25.973
_diffrn_reflns_theta_max         26.503
_diffrn_reflns_theta_min         1.805
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.40
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             7650
_exptl_crystal_recrystallization_method
;
Slow evaporation of a MeOH/Pyridine solution
;
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_platon_squeeze_details
;
This equates to 1142 e-/cell thus 285 e-/cluster.
It could be interpreted as 13 MeOH + 1 water (244 e-) plus 1 BF4 (41 e-)
The presence of the extra BF4 anion is needed for charge balancing and it has
been proved by ion exchange chromatographic measurements.
;
_refine_diff_density_max         1.82
_refine_diff_density_min         -1.07
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0984
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1657
_refine_ls_number_reflns         17942
_refine_ls_number_restraints     1380
_refine_ls_R_factor_all          0.1772
_refine_ls_R_factor_gt           0.1166
_refine_ls_shift/su_max          0.0023410
_refine_ls_shift/su_mean         0.0669959
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
1.39 1.78 1.31 0.529 0.281
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1532
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1115
_reflns_limit_h_max              21
_reflns_limit_h_min              -21
_reflns_limit_k_max              41
_reflns_limit_k_min              0
_reflns_limit_l_max              39
_reflns_limit_l_min              0
_reflns_number_gt                17942
_reflns_number_total             36222
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.10
_oxford_diffrn_Wilson_scale      212.01
_oxford_refine_ls_r_factor_ref   0.1166
_oxford_refine_ls_scale          0.04668(8)
_oxford_reflns_number_all        35431
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title 'pt9047 in P2(1)/n'
_cod_data_source_file            c1cc11146a.txt
_cod_data_source_block           pt9047
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z adriana 
;
_cod_original_cell_volume        17291.7(20)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               7106443