Design, Formation and Properties of Tetrahedral M4L4 and M4L6 Supramolecular Clusters1
Dana L. Caulder; Christian Brückner; Ryan E. Powers; Stefan König; Tatjana N. Parac; Julie A. Leary; Kenneth N. Raymond; Journal of the American Chemical Society 123 (2001) 8923–8938; doi:10.1021/ja0104507

data_4115686
_publ_contact_author
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Kenneth N. Raymond
Department of Chemistry
University of California
Berkeley, CA  94720-1460
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_publ_contact_author_email       raymond@socrates.berkeley.edu
_publ_contact_author_fax         510-486-5283
_publ_contact_author_phone       510-642-7219
_publ_section_title
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 Design, Formation and Properties of Tetrahedral M4L4 and M4L6
 Supramolecular Clusters1
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8923
_journal_page_last               8938
_journal_paper_doi               10.1021/ja0104507
_journal_volume                  123
_journal_year                    2001
_chemical_compound_source        synthetic
_chemical_formula_structural
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Fe4 (C24 H14 N2 O6)6, K5 (N(C2 H5)4)7 (H2 O)8 (C H4 O)3
;
_chemical_formula_sum            'C203 H312 Fe4 K5 N19 O47'
_chemical_formula_weight         4189.62
_space_group_IT_number           220
_symmetry_cell_setting           cubic
_symmetry_Int_Tables_number      220
_symmetry_space_group_name_Hall  'I -4bd 2c 3'
_symmetry_space_group_name_H-M   'I -4 3 d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   43.707(8)
_cell_length_b                   43.707(8)
_cell_length_c                   43.707(8)
_cell_measurement_reflns_used    87
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      23.21
_cell_measurement_theta_min      1.5
_cell_volume                     83494(3)
_computing_cell_refinement
;
SMART (Siemens, 1995), SAINT (Siemens, 1995)
;
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction
;
SAINT (Siemens, 1995), XPREP (Siemens, 1995),
;
_computing_structure_refinement
;
SHELXL-93 (Siemens, 1993)
;
_computing_structure_solution    'SHELXS-86 (Siemens, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_measurement_device       '3 circle diffractometer'
_diffrn_measurement_method
;
omega scans with profile analysis
;
_diffrn_radiation_detector       'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.2138
_diffrn_reflns_av_sigmaI/netI    0.0651
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            131662
_diffrn_reflns_theta_max         20.84
_diffrn_reflns_theta_min         1.14
_exptl_absorpt_coefficient_mu    0.453
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.834
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       block
_exptl_crystal_F_000             35808
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.104
_refine_ls_goodness_of_fit_obs   1.115
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         5482
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.207
_refine_ls_restrained_S_obs      1.119
_refine_ls_R_factor_all          0.1504
_refine_ls_R_factor_obs          0.0978
_refine_ls_shift/esd_max         -0.089
_refine_ls_shift/esd_mean        0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1660P)^2^+779.9778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3288
_refine_ls_wR_factor_obs         0.2552
_reflns_number_observed          4672
_reflns_number_total             7336
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja0104507_3.cif
_cod_data_source_block           borg2m
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '
calc w=1/[\s^2^(Fo^2^)+(0.1660P)^2^+779.9778P] where
P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w=1/[\s^2^(Fo^2^)+(0.1660P)^2^+779.9778P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        83491.3(258)
_cod_database_code               4115686