Fine-Tuning the Ring-Size of Metallacyclophanes: A Rational Approach to Molecular Pentagons
Cristian Saul Campos-Fernández; Rodolphe Clérac; John M. Koomen; David H. Russell; Kim R. Dunbar; Journal of the American Chemical Society 123 (2001) 773–774; doi:10.1021/ja002960r

data_4115429
_publ_section_title
;
 Fine-Tuning the Ring-Size of Metallacyclophanes: A Rational Approach to
 Molecular Pentagons
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              773
_journal_page_last               774
_journal_paper_doi               10.1021/ja002960r
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C70 H65 Cl8 N35 O32 Zn4'
_chemical_formula_weight         2453.7
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 102.30(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            10
_cell_length_a                   20.377(4)
_cell_length_b                   16.634(3)
_cell_length_c                   28.283(6)
_cell_measurement_temperature    110(2)
_cell_volume                     9366(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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0654
_diffrn_reflns_av_sigmaI/netI    0.0670
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            44125
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    1.348
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_F_000             5094
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.401
_refine_diff_density_min         -1.232
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     727
_refine_ls_number_reflns         7997
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1284
_refine_ls_R_factor_gt           0.0764
_refine_ls_shift/su_max          3.266
_refine_ls_shift/su_mean         0.052
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1669P)^2^+17.7577P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2218
_refine_ls_wR_factor_ref         0.2610
_reflns_number_gt                4776
_reflns_number_total             7997
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja002960r_3.cif
_cod_data_source_block           c2c
_cod_database_code               4115429