Linking [M(III)(3)] triangles with "double-headed" phenolic oximes.
Mason, Kevin; Chang, John; Prescimone, Alessandro; Garlatti, Elena; Carretta, Stefano; Tasker, Peter A.; Brechin, Euan K.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 8777–8785; doi:10.1039/c2dt30189j

data_7019332
_publ_section_title
;
 Linking [M(III)(3)] triangles with &quot;double-headed&quot; phenolic
 oximes.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8777
_journal_page_last               8785
_journal_paper_doi               10.1039/c2dt30189j
_journal_volume                  41
_journal_year                    2012
_chemical_compound_source        K.Mason
_chemical_formula_moiety         '[Fe6O(OH)7(oxime)3][BF4]3.4H2O.9MeOH'
_chemical_formula_sum            'C111 H195 B3 F12 Fe6 N12 O33'
_chemical_formula_weight         2821.28
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             11-06-29
_audit_creation_method           CRYSTALS_ver_14.05
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   26.5317(4)
_cell_length_b                   26.5317(4)
_cell_length_c                   101.306(2)
_cell_measurement_reflns_used    29047
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      51.6473
_cell_measurement_theta_min      1.9699
_cell_volume                     61758.4(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_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      100
_diffrn_detector_area_resol_mean 5.1574
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.1257
_diffrn_reflns_av_sigmaI/netI    0.1515
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       100
_diffrn_reflns_limit_l_min       -103
_diffrn_reflns_number            115307
_diffrn_reflns_theta_full        50.671
_diffrn_reflns_theta_max         51.6473
_diffrn_reflns_theta_min         1.9699
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.727
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21018
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.37
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             26783
_exptl_crystal_recrystallization_method
;
Slow evaporation of a MeOH/Pyridine solution
;
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.160
_platon_squeeze_details
;
This equates to 2981 e-/cell thus 165 e-/cluster that can be rationalised as
9MeOH (162 e-).
;
_refine_diff_density_max         1.81
_refine_diff_density_min         -1.43
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0511
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         6609
_refine_ls_number_restraints     585
_refine_ls_R_factor_all          0.1564
_refine_ls_R_factor_gt           0.1468
_refine_ls_shift/su_max          0.0053838
_refine_ls_shift/su_mean         0.6417242
_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:
43.0 48.2 37.9 15.8
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1920
_refine_ls_wR_factor_gt          0.1769
_refine_ls_wR_factor_ref         0.1769
_reflns_limit_h_max              0
_reflns_limit_h_min              -23
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              102
_reflns_limit_l_min              0
_reflns_number_gt                6609
_reflns_number_total             7558
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.31
_oxford_diffrn_Wilson_scale      5.04
_oxford_refine_ls_r_factor_ref   0.1468
_oxford_refine_ls_scale          0.401(2)
_oxford_reflns_number_all        7542
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title 'pt1006 in R-3c'
_cod_data_source_file            c2dt30189j.txt
_cod_data_source_block           pt1006
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        61758.3(19)
_cod_original_sg_symbol_H-M      'R -3 c '
_cod_database_code               7019332
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_theta     50.38