"Squaring the Circle": Molecular Squares and Rectangles from Chelate-Induced Structural Transformations of Known Fe10 and New Fe12 Ferric Wheels
Theocharis C. Stamatatos; Alexander G. Christou; Candace M. Jones; Brian J. O'Callaghan; Khalil A. Abboud; Ted A. O'Brien; George Christou; Journal of the American Chemical Society 129 (2007) 9840–9841; doi:10.1021/ja073236c

data_4109773
_publ_section_title
;
 "Squaring the Circle": Molecular Squares and Rectangles from
 Chelate-Induced Structural Transformations of Known Fe10 and New Fe12
 Ferric Wheels
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9840
_journal_page_last               9841
_journal_paper_doi               10.1021/ja073236c
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C176 H186 Cl8 Fe12 N34 O60'
_chemical_formula_weight         4691.39
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                85.786(9)
_cell_angle_beta                 81.646(8)
_cell_angle_gamma                89.639(7)
_cell_formula_units_Z            2
_cell_length_a                   19.293(7)
_cell_length_b                   19.914(8)
_cell_length_c                   26.176(10)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     9923(7)
_computing_cell_refinement
'Bruker SMART v5.624 & SAINT 6.36a (Bruker 1998)'
_computing_data_collection       'Bruker SMART v5.624 (Bruker 1998)'
_computing_data_reduction        'Bruker SHELXTL v6.14 (Bruker 2000)'
_computing_molecular_graphics    'Bruker SHELXTL v6.14'
_computing_publication_material  'Bruker SHELXTL v6.14'
_computing_structure_refinement  'Bruker SHELXTL v6.14'
_computing_structure_solution    'Bruker SHELXTL v6.14'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'SMART CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1750
_diffrn_reflns_av_sigmaI/netI    0.6741
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            56215
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.79
_diffrn_standards_decay_%        1
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.049
_exptl_absorpt_correction_T_max  0.9793
_exptl_absorpt_correction_T_min  0.8261
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'based on measured indexed crystal faces, Bruker SHELXTL  v6.12 (Bruker 1998)'
_exptl_crystal_colour            needles
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_description       yellow
_exptl_crystal_F_000             4816
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.954
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.680
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1502
_refine_ls_number_reflns         34738
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      0.682
_refine_ls_R_factor_all          0.2621
_refine_ls_R_factor_gt           0.0867
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0617P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1866
_refine_ls_wR_factor_ref         0.2172
_reflns_number_gt                7265
_reflns_number_total             34738
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja073236csi20070507_053436.cif
_cod_data_source_block           st89
_cod_original_cell_volume        9923(6)
_cod_database_code               4109773