Anion-Templated Assembly of a [2]Catenane
Mark R. Sambrook; Paul D. Beer; James A. Wisner; Rowena L. Paul; Andrew R. Cowley; Journal of the American Chemical Society 126 (2004) 15364–15365; doi:10.1021/ja045080b

data_4113217
_publ_section_title
;
 Anion-Templated Assembly of a [2]Catenane
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15364
_journal_page_last               15365
_journal_paper_doi               10.1021/ja045080b
_journal_volume                  126
_journal_year                    2004
_chemical_compound_source
;
synthesis as described
;
_chemical_formula_moiety         ' C32 H38 N2 O9, C32 H38 N3 O8, Cl '
_chemical_formula_sum            'C64 H76 Cl N5 O17'
_chemical_formula_weight         1222.78
_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
_cell_angle_alpha                64.4415(5)
_cell_angle_beta                 90.0332(6)
_cell_angle_gamma                78.4160(11)
_cell_formula_units_Z            2
_cell_length_a                   10.9113(2)
_cell_length_b                   17.3319(2)
_cell_length_c                   19.6884(4)
_cell_measurement_reflns_used    12793
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3274.52(10)
_computing_cell_refinement
; 
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) 
;
_computing_data_collection
; 
KappaCCD software 'Collect' (Nonius, 2000) 
;
_computing_data_reduction
; 
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) 
;
_computing_publication_material
; 
CRYSTALS (Watkin et al, 2001) 
;
_computing_structure_refinement
; 
CRYSTALS (Watkin et al, 2001) 
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type
; 
Nonius KappaCCD 
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.062
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            45029
_diffrn_reflns_theta_full        27.544
_diffrn_reflns_theta_max         27.544
_diffrn_reflns_theta_min         5.128
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_exptl_crystal_colour            ' yellow '
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_description       ' plate '
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.48
_refine_diff_density_min         -0.63
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0644
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     790
_refine_ls_number_reflns         6697
_refine_ls_number_restraints     72
_refine_ls_R_factor_all          0.1821
_refine_ls_R_factor_gt           0.1082
_refine_ls_shift/su_max          0.010897
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 2.61 2.36 1.71 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1448
_refine_ls_wR_factor_gt          0.1181
_refine_ls_wR_factor_ref         0.1181
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              22
_reflns_limit_k_min              -19
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                6697
_reflns_number_total             14745
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            ja045080bsi20040816_092003.cif
_cod_data_source_block           Compound_1
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C64 H76 Cl1 N5 O17 '
_cod_database_code               4113217