En Route to a Molecular Sheaf: Active Metal Template Synthesis of a [3]Rotaxane with Two Axles Threaded through One Ring
Hei Man Cheng; David A. Leigh; Francesca Maffei; Paul R. McGonigal; Alexandra M. Z. Slawin; Jhenyi Wu; Journal of the American Chemical Society 133 (2011) 12298–12303; doi:10.1021/ja205167e

data_4106533
_publ_section_title
;
 En Route to a Molecular Sheaf: Active Metal Template Synthesis of a
 [3]Rotaxane with Two Axles Threaded through One Ring
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12298
_journal_page_last               12303
_journal_paper_doi               10.1021/ja205167e
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C47 H49 Cl2 N3 Ni O2,C4 H10 O,C3 H7 N O'
_chemical_formula_sum            'C54 H66 Cl2 N4 Ni O4'
_chemical_formula_weight         964.72
_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                 92.939(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   48.61(2)
_cell_length_b                   13.472(6)
_cell_length_c                   15.627(7)
_cell_measurement_reflns_used    9527
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      28.1
_cell_measurement_theta_min      2.3
_cell_volume                     10220(8)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3344
_diffrn_reflns_av_sigmaI/netI    0.2156
_diffrn_reflns_limit_h_max       58
_diffrn_reflns_limit_h_min       -58
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            51374
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    0.532
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             4096
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.507
_refine_diff_density_min         -1.029
_refine_diff_density_rms         0.231
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.889
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         9350
_refine_ls_number_restraints     286
_refine_ls_restrained_S_all      1.859
_refine_ls_R_factor_all          0.3606
_refine_ls_R_factor_gt           0.3104
_refine_ls_shift/su_max          0.088
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.6109
_refine_ls_wR_factor_ref         0.6280
_reflns_number_gt                5948
_reflns_number_total             9350
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja205167e_si_003.cif
_cod_data_source_block           1.NiCl2
_cod_database_code               4106533