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_4115428
_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            'C72 H68 B8 F32 N36 Zn4'
_chemical_formula_weight         2393.6
_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                94.458(5)
_cell_angle_beta                 92.510(5)
_cell_angle_gamma                97.790(5)
_cell_formula_units_Z            2
_cell_length_a                   13.924(5)
_cell_length_b                   17.071(5)
_cell_length_c                   21.940(5)
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      1.21
_cell_volume                     5144(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 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_av_sigmaI/netI    0.0886
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            63108
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         1.21
_exptl_absorpt_coefficient_mu    1.039
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_F_000             2398
_exptl_crystal_size_max          0.117
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.024
_refine_diff_density_max         1.681
_refine_diff_density_min         -1.191
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1394
_refine_ls_number_reflns         24635
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1335
_refine_ls_R_factor_gt           0.0695
_refine_ls_shift/su_max          5.026
_refine_ls_shift/su_mean         0.109
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1525P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2017
_refine_ls_wR_factor_ref         0.2614
_reflns_number_gt                13131
_reflns_number_total             24635
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja002960r_2.cif
_cod_data_source_block           p-1
_cod_database_code               4115428