Synthesis of Open and Closed Metallacages Using Novel Tripodal Ligands: Unusually Stable Silver(I) Inclusion Compound
Daniel L. Reger; Radu F. Semeniuc; Mark D. Smith; Inorganic Chemistry 42 (2003) 8137–8139; doi:10.1021/ic035192o

data_4312742
_publ_contact_author_address
;
Department of Chemistry and Biochemistry
University of South Carolina
Columbia, South Carolina 29208
USA
;
_publ_contact_author_email       reger@mail.chem.sc.edu
_publ_contact_author_fax         '1 803 777 9521'
_publ_contact_author_name        'Professor Daniel L. Reger'
_publ_contact_author_phone       '1 803 777 2587'
_publ_section_title
;
 Synthesis of Open and Closed Metallacages Using Novel Tripodal Ligands:
 Unusually Stable Silver(I) Inclusion Compound
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8137
_journal_page_last               8139
_journal_paper_doi               10.1021/ic035192o
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C120 H161 B8 Cd4 F32 N45 O13'
_chemical_formula_weight         3586.02
_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                72.7100(10)
_cell_angle_beta                 70.8220(10)
_cell_angle_gamma                74.5800(10)
_cell_formula_units_Z            1
_cell_length_a                   15.3996(10)
_cell_length_b                   17.0481(11)
_cell_length_c                   17.2755(11)
_cell_measurement_reflns_used    7048
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      25.024
_cell_measurement_theta_min      2.464
_cell_volume                     4018.3(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0529
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33081
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         1.43
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_T_max  0.8309
_exptl_absorpt_correction_T_min  0.5888
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             1820
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.367
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1105
_refine_ls_number_reflns         14172
_refine_ls_number_restraints     190
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0651P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1197
_refine_ls_wR_factor_ref         0.1238
_reflns_number_gt                10406
_reflns_number_total             14172
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035192osi20031015_014726_1.cif
_cod_data_source_block           1
_cod_database_code               4312742