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_4113897
_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            'C100 H116 Cl4 N16 Ni2 O10'
_chemical_formula_weight         1961.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_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                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.301(2)
_cell_length_b                   15.301(2)
_cell_length_c                   23.303(5)
_cell_measurement_temperature    293(2)
_cell_volume                     5455.7(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  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  0.0954
_diffrn_reflns_av_sigmaI/netI    0.1779
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            10422
_diffrn_reflns_theta_full        27.60
_diffrn_reflns_theta_max         27.60
_diffrn_reflns_theta_min         5.48
_exptl_absorpt_coefficient_mu    0.503
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_description       Block
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.689
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         3036
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.2125
_refine_ls_R_factor_gt           0.0798
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1981
_refine_ls_wR_factor_ref         0.2398
_reflns_number_gt                1036
_reflns_number_total             3036
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja034267ksi20030121_054932_06.cif
_cod_data_source_block           6
_cod_database_code               4113897