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_4301907
_publ_section_title
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Magnetic [nxn] (n= 2-5) Grids by Directed Self-Assembly
;
_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            'C140 H101.6 Cu16 F36 N96 O54.8 S12'
_chemical_formula_weight         6090.75
_chemical_name_systematic
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 ? 
;
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      86
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :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            2
_cell_length_a                   23.579(3)
_cell_length_b                   23.579(3)
_cell_length_c                   22.196(2)
_cell_measurement_reflns_used    22268
_cell_measurement_temperature    138(2)
_cell_measurement_theta_max      30.8486
_cell_measurement_theta_min      1.7272
_cell_volume                     12340(2)
_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      138(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            26597
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    1.563
_exptl_absorpt_correction_T_max  0.7983
_exptl_absorpt_correction_T_min  0.6241
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            Red-Brown
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             6064
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.25
_platon_squeeze_details
;
The Platon Squeeze procedure was applied to recover 640.9 electrons per 
unit cell in one void (total volume 3601.4 ^A^3) that is 320.45 electrons 
per formula unit. An area of disperse electron density was present in the 
asymmetric unit prior to the application of Squeeze, which is a full occupancy 
triflate anion, though a good point atom model could not be achieved for this. 
The remaining electron density are solvent water molecules.  The application 
of Squeeze gave a good improvement in the data statistics and allowed for a 
full anisotropic refinement of the framework cationic structure.
PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13
;
_refine_diff_density_max         3.469
_refine_diff_density_min         -0.892
_refine_diff_density_rms         0.172
_refine_ls_extinction_coef       0.0033(6)
_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   1.245
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     663
_refine_ls_number_reflns         11965
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.245
_refine_ls_R_factor_all          0.1334
_refine_ls_R_factor_gt           0.1133
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3190
_refine_ls_wR_factor_ref         0.3400
_reflns_number_gt                8267
_reflns_number_total             11965
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801078h_si_001_7.cif
_cod_data_source_block           shelxl_(21)
_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        12341(2)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_original_formula_sum        'C140 H101.60 Cu16 F36 N96 O54.80 S12'
_cod_database_code               4301907