Ligand-Directed Molecular Architectures: Self-Assembly of Two-Dimensional Rectangular Metallacycles and Three-Dimensional Trigonal or Tetragonal Prisms
Cheng-Yong Su; Yue-Peng Cai; Chun-Long Chen; Mark D. Smith; Wolfgang Kaim; Hans-Conrad zur Loye; Journal of the American Chemical Society 125 (2003) 8595–8613; doi:10.1021/ja034267k

data_4113900
_publ_section_title
;
 Ligand-Directed Molecular Architectures: Self-Assembly of Two-Dimensional
 Rectangular Metallacycles and Three-Dimensional Trigonal or Tetragonal
 Prisms
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8595
_journal_page_last               8613
_journal_paper_doi               10.1021/ja034267k
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C132 H144 Cu10 I10 N24 O7'
_chemical_formula_weight         4083.11
_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                101.72(3)
_cell_angle_beta                 102.94(3)
_cell_angle_gamma                91.36(3)
_cell_formula_units_Z            2
_cell_length_a                   16.935(3)
_cell_length_b                   17.165(3)
_cell_length_c                   30.625(6)
_cell_measurement_temperature    293(2)
_cell_volume                     8473(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.556
_diffrn_measured_fraction_theta_max 0.556
_diffrn_measurement_device_type  'Kappa CCD'
_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  0.0529
_diffrn_reflns_av_sigmaI/netI    0.0769
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            15214
_diffrn_reflns_theta_full        21.49
_diffrn_reflns_theta_max         21.49
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    3.102
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'HABITUS, W. Herrendorf and H. B\"arnighausen, Karlsruhe 1993, Gie\&sen, 1996'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_description       rod
_exptl_crystal_F_000             3960
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.134
_refine_diff_density_min         -1.168
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1616
_refine_ls_number_reflns         10822
_refine_ls_number_restraints     320
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1108
_refine_ls_R_factor_gt           0.0847
_refine_ls_shift/su_max          0.065
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1393P)^2^+87.2354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2301
_refine_ls_wR_factor_ref         0.2471
_reflns_number_gt                8007
_reflns_number_total             10822
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja034267ksi20030121_054932_09.cif
_cod_data_source_block           9
_cod_database_code               4113900