A New Synthetic Route to Chloride Selective [2]Catenanes
L; Laura Hancock; Lydia Gilday; Nathan Kilah; Christopher Serpell; Paul Beer; Chem.Commun. 47 (2011) 1725–; doi:10.1039/c0cc04683c

data_7105949
_publ_section_title
;
 A New Synthetic Route to Chloride Selective [2]Catenanes
;
_journal_name_full               Chem.Commun.
_journal_page_first              1725
_journal_paper_doi               10.1039/c0cc04683c
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety
;
C32 H38 N2 O9, C30 H36 N3 O8, Cl, 0.68(C H Cl3)
;
_chemical_formula_sum            'C62.68 H74.68 Cl3.04 N5 O17'
_chemical_formula_weight         1277.94
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             10-09-28
_audit_creation_method           CRYSTALS_ver_14.07
_audit_update_record
;
2010-10-06 - Report by Nathan L. Kilah
for Paul D. Beer, Lydia C. Gilday
and Laura M. Hancock

2010-10-06 - Passes Checkcif with minor warnings.
;
_cell_angle_alpha                114.1468(4)
_cell_angle_beta                 97.4460(4)
_cell_angle_gamma                102.6071(4)
_cell_formula_units_Z            2
_cell_length_a                   11.8388(1)
_cell_length_b                   17.4493(1)
_cell_length_c                   17.8692(2)
_cell_measurement_reflns_used    14335
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3186.35(5)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       Area
_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  0.025
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26903
_diffrn_reflns_theta_full        26.951
_diffrn_reflns_theta_max         27.501
_diffrn_reflns_theta_min         5.129
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.218
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1346.901
_exptl_crystal_size_max          0.470
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.53
_refine_diff_density_min         -0.70
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9236
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     884
_refine_ls_number_reflns         14470
_refine_ls_number_restraints     297
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.0027246
_refine_ls_shift/su_mean         0.0000496
_refine_ls_structure_factor_coef Fsqd
_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:
73.4 118. 68.2 27.0 5.89
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1345
_refine_ls_wR_factor_gt          0.1217
_refine_ls_wR_factor_ref         0.1342
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              20
_reflns_limit_k_min              -22
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                11819
_reflns_number_total             14487
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.11
_oxford_diffrn_Wilson_scale      1.32
_oxford_refine_ls_r_factor_ref   0.0645
_oxford_refine_ls_scale          0.8194(16)
_oxford_reflns_number_all        14477
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '9251910 072NLK10'
_cod_data_source_file            C0CC04683C.TXT
_cod_data_source_block           4Cl
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7105949