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_4319080
_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            'C9 H27 O18 S3 Zn1.5'
_chemical_formula_weight         617.54
_space_group_IT_number           173
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_space_group_name_H-M   'P 63'
_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            2
_cell_length_a                   12.0673(6)
_cell_length_b                   12.0673(6)
_cell_length_c                   9.7020(4)
_cell_measurement_temperature    173(2)
_cell_volume                     1223.52(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2615
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         4.43
_exptl_absorpt_coefficient_mu    1.813
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             636
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.53(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         1557
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0601
_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^)+(0.0517P)^2^+4.2300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1487
_refine_ls_wR_factor_ref         0.1503
_reflns_number_gt                1492
_reflns_number_total             1557
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025627s_s1_4.cif
_cod_data_source_block           '[Zn1.5(H2O)9L](4)'
_cod_original_formula_sum        'C9 H27 O18 S3 Zn1.50'
_cod_database_code               4319080