Cubic assembly of a geometrically frustrated {Fe(12)} spin cluster.
Graham, Kristoffer; Douglas, Fraser J.; Mathieson, Jennifer S.; Moggach, Stephen A.; Schnack, Jürgen; Murrie, Mark; Dalton transactions (Cambridge, England : 2003) 40 (2011) 12271–12276; doi:10.1039/c1dt10910c

data_7017275
_publ_section_title
;
 Cubic assembly of a geometrically frustrated {Fe(12)} spin cluster.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12271
_journal_page_last               12276
_journal_paper_doi               10.1039/c1dt10910c
_journal_volume                  40
_journal_year                    2011
_chemical_absolute_configuration unk
_chemical_formula_moiety         '[Fe12O4(OH)2(L)4(OAc)8][Cl]2'
_chemical_formula_sum            'C56 H106 Cl2 Fe12 N8 O38'
_chemical_formula_weight         2240.51
_space_group_IT_number           219
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'F -4a 2 3'
_symmetry_space_group_name_H-M   'F -4 3 c'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             11-05-11
_audit_creation_method           CRYSTALS_ver_14.21
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   39.2647(9)
_cell_length_b                   39.2647(9)
_cell_length_c                   39.2647(9)
_cell_measurement_reflns_used    9860
_cell_measurement_temperature    100
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     60535(2)
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.070
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       2
_diffrn_reflns_number            169895
_diffrn_reflns_theta_full        28.369
_diffrn_reflns_theta_max         28.948
_diffrn_reflns_theta_min         1.467
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.800
_exptl_absorpt_correction_T_max  0.71
_exptl_absorpt_correction_T_min  0.60
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             27936
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_platon_squeeze_details
;
The total electron count in the pores equates to 5689 electrons per unit cell.
A massive amount. Most of this electron density is completely diffuse,
and there is no evidence (at least crystallographically) for the presence of
Cl- ions. Though clearly there could be disordered anions in the pore.
The presence of chloride is confirmed by a positive test using a solution of
silver nitrate.
;
_refine_diff_density_max         0.51
_refine_diff_density_min         -0.62
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8240
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         6568
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0253
_refine_ls_shift/su_max          0.0005169
_refine_ls_shift/su_mean         0.0000358
_refine_ls_structure_factor_coef Fsqd
_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:
1.53 1.92 0.481
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0741
_refine_ls_wR_factor_gt          0.0614
_refine_ls_wR_factor_ref         0.0741
_reflns_limit_h_max              30
_reflns_limit_h_min              -30
_reflns_limit_k_max              36
_reflns_limit_k_min              0
_reflns_limit_l_max              53
_reflns_limit_l_min              2
_reflns_number_gt                5795
_reflns_number_total             6568
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0334
_oxford_refine_ls_scale          0.006(0)
_oxford_reflns_number_all        6568
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'ST1022_0m in F-43c'
_cod_data_source_file            c1dt10910c.txt
_cod_data_source_block           ST1022
_cod_depositor_comments
;
The following automatic conversions were performed:

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

'_atom_sites_solution_primary' value 'Direct' changed to
'direct' 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 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_Hall     'F -4c 2 3'
_cod_original_sg_symbol_H-M      'F -4 3 c '
_cod_original_formula_sum        'C56 H106 Fe12 N8 O38 Cl2'
_cod_database_code               7017275
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
RIDE C ( 2,X'S) H ( 21,X'S) H ( 22,X'S)
RIDE C ( 3,X'S) H ( 31,X'S) H ( 32,X'S)
RIDE C ( 4,X'S) H ( 41,X'S) H ( 42,X'S) H ( 43,X'S)
RIDE C ( 14,X'S) H ( 141,X'S) H ( 142,X'S)
RIDE C ( 15,X'S) H ( 151,X'S) H ( 152,X'S)
RIDE C ( 24,X'S) H ( 241,X'S) H ( 242,X'S)
RIDE C ( 25,X'S) H ( 251,X'S) H ( 252,X'S)
RIDE C ( 27,X'S) H ( 271,X'S) H ( 272,X'S)
RIDE C ( 28,X'S) H ( 281,X'S) H ( 282,X'S)
RIDE C ( 32,X'S) H ( 321,X'S) H ( 322,X'S)
RIDE C ( 33,X'S) H ( 331,X'S) H ( 332,X'S)
RIDE C ( 42,X'S) H ( 421,X'S) H ( 422,X'S) H ( 423,X'S)
RIDE O ( 7,X'S) H ( 71,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;