Magnetic [nxn] (n= 2-5) Grids by Directed Self-Assembly
Louise N. Dawe; Konstantin V. Shuvaev; Laurence K. Thompson; Inorganic Chemistry 48 (2009) 3323–3341; doi:10.1021/ic801078h

data_4301904
_publ_section_title
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Magnetic [nxn] (n= 2-5) Grids by Directed Self-Assembly
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3323
_journal_page_last               3341
_journal_paper_doi               10.1021/ic801078h
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C102 H106 Mn5 N72 O42 Zn4'
_chemical_formula_weight         3548.63
_chemical_name_systematic
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 ? 
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_space_group_IT_number           142
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      142
_symmetry_space_group_name_Hall  '-I 4bd 2c'
_symmetry_space_group_name_H-M   'I 41/a c d :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.958(3)
_cell_length_b                   27.958(3)
_cell_length_c                   39.801(4)
_cell_measurement_reflns_used    39980
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      30.7845
_cell_measurement_theta_min      2.2381
_cell_volume                     31110(6)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics    'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)'
_computing_publication_material  'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0992
_diffrn_reflns_av_sigmaI/netI    0.0397
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            96366
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    1.094
_exptl_absorpt_correction_T_max  0.9111
_exptl_absorpt_correction_T_min  0.8324
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             14424
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
The Platon Squeeze procedure was applied to recover 1523.4 electrons per 
unit cell in one void (total volume 9028.0 ^A^3); that is 190.425 electrons 
per formula unit. A disordered nitrate anion was present in the asymmetric 
unit prior to the application of Squeeze, though a good point atom model 
could not be achieved for this. This accounts for 50 electrons per formula 
unit.  Disordered solvent (14 lattice water molecules) was also present. 
The application of Squeeze gave a good improvement in the data statistics 
and allowed for a full anisotropic refinement of the framework structure.
PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13
;
_refine_diff_density_max         2.184
_refine_diff_density_min         -0.842
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       0.00002(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         7665
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.1292
_refine_ls_R_factor_gt           0.1168
_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^)+(0.1062P)^2^+291.2670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2769
_refine_ls_wR_factor_ref         0.2855
_reflns_number_gt                6977
_reflns_number_total             7665
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801078h_si_001_4.cif
_cod_data_source_block           shelxl_(14)
_cod_depositor_comments
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The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Numerical' changed to 'numerical'
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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        31112(5)
_cod_original_sg_symbol_H-M      'I 41/a c d'
_cod_database_code               4301904