Strategy for Preparing Molecular Cylinders with Synthetically Programmable Structural Parameters
Joshua R. Farrell; Chad A. Mirkin; Louise M. Liable-Sands; Arnold L. Rheingold; Journal of the American Chemical Society 120 (1998) 11834–11835; doi:10.1021/ja982688+

data_4116890
_publ_contact_author
; 
     Dr. C. A. Mirkin 
     Department of Chemistry
     Northwestern University
     2145 Sheridan Road
     Evanston, IL  60208
     USA 
;
_publ_contact_author_email       camirkin@chem.nwu.edu
_publ_contact_author_fax         '+847 467 5123'
_publ_contact_author_phone       '+847 491 2907'
_publ_section_title
;
 Strategy for Preparing Molecular Cylinders with Synthetically
 Programmable Structural Parameters
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11834
_journal_page_last               11835
_journal_paper_doi               10.1021/ja982688+
_journal_volume                  120
_journal_year                    1998
_chemical_formula_sum            'C294 H208 B4 Cl20 F80 N8 O8 P8 Rh4'
_chemical_formula_weight         6912.32
_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                82.6712(4)
_cell_angle_beta                 86.6043(12)
_cell_angle_gamma                81.0029(9)
_cell_formula_units_Z            1
_cell_length_a                   17.1270(2)
_cell_length_b                   20.3437(4)
_cell_length_c                   24.4755(4)
_cell_measurement_reflns_used    6185
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     8347.5(2)
_computing_cell_refinement       SAINT
_computing_data_collection       'Siemens P4/CCD'
_computing_data_reduction        SAINT
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      198(2)
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'Siemens P4/CCD'
_diffrn_measurement_method       'phi, omega'
_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  0.1168
_diffrn_reflns_av_sigmaI/netI    0.3027
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            30616
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.490
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.577
_exptl_absorpt_correction_type   DIFABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             3472
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.361
_refine_diff_density_min         -1.088
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    'idealized contributions'
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1612
_refine_ls_number_reflns         30616
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.2309
_refine_ls_R_factor_gt           0.0900
_refine_ls_shift/su_max          0.557
_refine_ls_shift/su_mean         0.039
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2185
_refine_ls_wR_factor_ref         0.2706
_reflns_number_gt                10230
_reflns_number_total             30616
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9826882B.cif
_cod_data_source_block           mir22
_cod_original_cell_volume        8347.4(3)
_cod_database_code               4116890