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_7105950
_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         'C30 H36 N3 O8, C30 H34 N2 O8, F6 P, H2 O'
_chemical_formula_sum            'C60 H72 F6 N5 O17 P'
_chemical_formula_weight         1280.22
_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
_audit_creation_date             10-11-23
_audit_creation_method           CRYSTALS_ver_14.07
_cell_angle_alpha                74.5452(5)
_cell_angle_beta                 78.3493(5)
_cell_angle_gamma                85.1917(5)
_cell_formula_units_Z            2
_cell_length_a                   9.74820(10)
_cell_length_b                   14.2731(2)
_cell_length_c                   23.7801(3)
_cell_measurement_reflns_used    13080
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3121.77(7)
_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    'CAMERON (Watkin et al., 1996)'
_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 0.988
_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  0.030
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            52283
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         27.551
_diffrn_reflns_theta_min         5.112
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.135
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.51
_refine_diff_density_min         -0.42
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9462
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     802
_refine_ls_number_reflns         14263
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0501
_refine_ls_shift/su_max          0.0003573
_refine_ls_shift/su_mean         0.0000269
_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:
17.5 25.6 12.4 3.11
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1321
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1321
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              18
_reflns_limit_k_min              -17
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                10210
_reflns_number_total             14264
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.74
_oxford_diffrn_Wilson_scale      6.92
_oxford_refine_ls_r_factor_ref   0.0785
_oxford_refine_ls_scale          0.3919(3)
_oxford_reflns_number_all        14263
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 048CJS10
_cod_data_source_file            C0CC04683C.TXT
_cod_data_source_block           5PF6
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C60 H72 F6 N5 O17 P1'
_cod_database_code               7105950