Pentameric Circular Iron(II) Double Helicates and a Molecular Pentafoil Knot
Jean-François Ayme; Jonathon E. Beves; David A. Leigh; Roy T. McBurney; Kari Rissanen; David Schultz; Journal of the American Chemical Society 134 (2012) 9488–9497; doi:10.1021/ja303355v

data_4118021
_publ_contact_author_address
;School of Chemistry
University of Edinburgh
The King?s Buildings
West Mains Road
Edinburgh EH9 3JJ
United King-dom
;
_publ_contact_author_email       David.Leigh@ed.ac.uk
_publ_contact_author_name        'David A. Leigh'
_publ_section_title
;
 Pentameric Circular Iron(II) Double Helicates and a Molecular Pentafoil
 Knot
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9488
_journal_page_last               9497
_journal_paper_doi               10.1021/ja303355v
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C240 H234 Cl F45 Fe5 N37 O20 P7.50'
_chemical_formula_sum            'C240 H234 Cl F45 Fe5 N37 O20 P7.5'
_chemical_formula_weight         5358.62
_chemical_name_common
'2,4-dimethoxybenzylamine-derived pentameric iron(II) helicate'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-12-01T08:01:09-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 94.386(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   34.023(2)
_cell_length_b                   23.7143(18)
_cell_length_c                   36.537(2)
_cell_measurement_reflns_used    25684
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      21.2
_cell_volume                     29393(3)
_computing_cell_refinement
;
        CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_collection
;
        CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_reduction
;
        CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 22.2222
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device
;
        AFC11 (Right): Eulerian 3 circle
;
_diffrn_measurement_device_type
;
        Rigaku Saturn944+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.020501
_diffrn_orient_matrix_UB_12      -0.002733
_diffrn_orient_matrix_UB_13      0.021005
_diffrn_orient_matrix_UB_21      -0.021286
_diffrn_orient_matrix_UB_22      0.027102
_diffrn_orient_matrix_UB_23      0.024302
_diffrn_orient_matrix_UB_31      -0.012536
_diffrn_orient_matrix_UB_32      -0.021008
_diffrn_orient_matrix_UB_33      0.012449
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0875
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            256369
_diffrn_reflns_theta_full        60
_diffrn_reflns_theta_max         60
_diffrn_reflns_theta_min         2.22
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    3.157
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.5
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_description       Block
_exptl_crystal_F_000             11030
_exptl_crystal_recrystallization_method Nitromethane-acetonitrile-diethylether
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.27
_refine_diff_density_min         -0.836
_refine_diff_density_rms         0.157
_refine_ls_extinction_coef       0.00050(4)
_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   1.411
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3206
_refine_ls_number_reflns         43584
_refine_ls_number_restraints     151
_refine_ls_restrained_S_all      1.411
_refine_ls_R_factor_all          0.1561
_refine_ls_R_factor_gt           0.1392
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0
_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          0.3627
_refine_ls_wR_factor_ref         0.3835
_reflns_number_gt                30867
_reflns_number_total             43584
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja303355v_si_002.cif
_cod_data_source_block           OMe2_helicate
_cod_original_cell_volume        29393(4)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C240 H234 Cl F45 Fe5 N37 O20 P7.50'
_cod_database_code               4118021