Anion Templated Double Cyclization Assembly of a Chloride Selective [2]Catenane
P. D. Beer; Andrew R. Cowley; Ka-Yuen Ng.; Chemical Communications  (2006) –; doi:10.1039/b606503a

data_7101365
_publ_section_title
;
Anion Templated Double Cyclization Assembly of a
Chloride Selective [2]Catenane
;
_journal_issue                   35
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/b606503a
_journal_year                    2006
_chemical_absolute_configuration ad
_chemical_compound_source
;
synthesis as described
;
_chemical_formula_moiety
'2( C36 H46 N3 O10 ), F6 O ,2( C H2 Cl2 ), Cl'
_chemical_formula_sum            'C74 H96 Cl5 F6 N6 O20 P'
_chemical_formula_weight         1711.83
_chemical_name_systematic
;
?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 92.313(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.5488(19)
_cell_length_b                   13.3481(9)
_cell_length_c                   27.620(3)
_cell_measurement_reflns_used    26601
_cell_measurement_temperature    150
_cell_measurement_theta_max      74
_cell_measurement_theta_min      5
_cell_volume                     7938.0(11)
_computing_cell_refinement
;
Gemini software 'Crysalis' (Oxford Diffraction, 2005)
;
_computing_data_collection
;
Gemini software 'Crysalis' (Oxford Diffraction, 2005)
;
_computing_data_reduction
;
Gemini software 'Crysalis' (Oxford Diffraction, 2005)
;
_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 0.994
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type
;
Oxford Diffraction Gemini
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54248
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            26601
_diffrn_reflns_theta_full        68.
_diffrn_reflns_theta_max         74.182
_diffrn_reflns_theta_min         3.898
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.615
_exptl_absorpt_correction_T_max  0.59
_exptl_absorpt_correction_T_min  0.34
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Gemini software 'Crysalis' (Oxford Diffraction, 2005)
;
_exptl_crystal_colour            ' pale yellow '
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       ' fragment '
_exptl_crystal_F_000             3584
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_exptl_crystal_thermal_history
;
The material was crystallised at ambient temperature. A suitable crystal
was cooled rapidly to 150K for single-crystal X-ray diffraction analysis.
;
_refine_diff_density_max         0.97
_refine_diff_density_min         -0.54
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0090
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1010
_refine_ls_number_reflns         10548
_refine_ls_number_restraints     298
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0770
_refine_ls_shift/su_max          0.023255
_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:
23.4 -1.59 19.7
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0988
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.0914
_reflns_limit_h_max              26
_reflns_limit_h_min              -22
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              34
_reflns_limit_l_min              -33
_reflns_number_gt                10548
_reflns_number_total             13870
_reflns_threshold_expression     I>2.00u(I)
_cod_data_source_file            b606503a.txt
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'C 1 c 1 '
_cod_original_formula_sum        ' C74 H96 Cl5 F6 N6 O20 P '
_cod_database_code               7101365