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_4113901
_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            'C138 H138 Cu10 I10 N24 O6'
_chemical_formula_weight         4133.12
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 108.19(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.893(6)
_cell_length_b                   40.398(13)
_cell_length_c                   23.814(9)
_cell_measurement_reflns_used    38
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.03
_cell_measurement_theta_min      9.5
_cell_volume                     18181(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Siemens P4'
_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  0.1351
_diffrn_reflns_av_sigmaI/netI    0.3255
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17245
_diffrn_reflns_theta_full        20.00
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         1.87
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.892
_exptl_absorpt_correction_T_max  0.35
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Yellowish
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       Block
_exptl_crystal_F_000             8008
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.082
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.183
_refine_ls_extinction_coef       0.000079(8)
_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   0.929
_refine_ls_hydrogen_treatment    geom
_refine_ls_matrix_type           full
_refine_ls_number_parameters     922
_refine_ls_number_reflns         16630
_refine_ls_number_restraints     237
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.2241
_refine_ls_R_factor_gt           0.0817
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1726
_refine_ls_wR_factor_ref         0.2110
_reflns_number_gt                5856
_reflns_number_total             16630
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja034267ksi20030121_054932_10.cif
_cod_data_source_block           9.ben
_cod_original_cell_volume        18182(11)
_cod_database_code               4113901