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_4115430
_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            'C74 H73 Cl8 N36 Ni4 O33'
_chemical_formula_weight         2499.005
_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                 104.11(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.082(3)
_cell_length_b                   31.922(6)
_cell_length_c                   22.305(5)
_cell_measurement_temperature    110(2)
_cell_volume                     10415(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.1143
_diffrn_reflns_av_sigmaI/netI    0.2323
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            79465
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.14
_exptl_absorpt_coefficient_mu    1.014
_exptl_crystal_colour            dark_green
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_F_000             5180
_exptl_crystal_size_max          0.111
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.084
_refine_diff_density_max         1.474
_refine_diff_density_min         -1.008
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.874
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1414
_refine_ls_number_reflns         25404
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.878
_refine_ls_R_factor_all          0.1970
_refine_ls_R_factor_gt           0.0605
_refine_ls_shift/su_max          0.257
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0846P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1477
_refine_ls_wR_factor_ref         0.2047
_reflns_number_gt                9335
_reflns_number_total             25404
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja002960r_4.cif
_cod_data_source_block           sad1
_cod_database_code               4115430