Intra- and Intermolecular Second-Sphere Coordination Chemistry: Formation of Capsules, Half-Capsules, and Extended Structures with Hexaaquo- and Hexaamminemetal Ions
Sean A. Dalrymple; Masood Parvez; George K. H. Shimizu; Inorganic Chemistry 41 (2002) 6986–6996; doi:10.1021/ic025627s

data_4319077
_publ_section_title
;
 Intra- and Intermolecular Second-Sphere Coordination Chemistry: Formation
 of Capsules, Half-Capsules, and Extended Structures with Hexaaquo- and
 Hexaamminemetal Ions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6986
_journal_page_last               6996
_journal_paper_doi               10.1021/ic025627s
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C12 H33 Fe O18 S3'
_chemical_formula_weight         617.41
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   13.979(2)
_cell_length_b                   13.979
_cell_length_c                   23.869(3)
_cell_measurement_temperature    173(2)
_cell_volume                     4039.4(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0195
_diffrn_reflns_av_sigmaI/netI    0.0218
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1743
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    0.866
_exptl_absorpt_correction_T_max  0.8323
_exptl_absorpt_correction_T_min  0.6714
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1938
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       0.00074(9)
_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   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         1597
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0275
_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^)+(0.0341P)^2^+11.9597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0722
_refine_ls_wR_factor_ref         0.0788
_reflns_number_gt                1320
_reflns_number_total             1597
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025627s_s1_1.cif
_cod_data_source_block           {Fe(H2O)6}[Fe(H2O)6(L)2].6MeOH(1)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4319077