A catenane host system containing integrated triazole C-H hydrogen bond donors for anion recognition
and; Nicholas G. White; Paul D. Beer; Chem.Commun. 48 (2012) 8499–; doi:10.1039/c2cc34210c

data_7108184
_publ_section_title
;
 A catenane host system containing integrated triazole C-H hydrogen bond
 donors for anion recognition
;
_journal_name_full               Chem.Commun.
_journal_page_first              8499
_journal_paper_doi               10.1039/c2cc34210c
_journal_volume                  48
_journal_year                    2012
_chemical_compound_source        synthesized
_chemical_formula_moiety         'C36 H46 N2 O9, C22 H34 N7, Cl'
_chemical_formula_sum            'C58 H80 Cl N9 O9'
_chemical_formula_weight         1082.78
_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                109.827(3)
_cell_angle_beta                 96.627(3)
_cell_angle_gamma                93.298(2)
_cell_formula_units_Z            2
_cell_length_a                   9.3945(5)
_cell_length_b                   17.0675(10)
_cell_length_c                   18.9451(12)
_cell_measurement_reflns_used    8412
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     2823.3(3)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 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 0.957
_diffrn_measured_fraction_theta_max 0.912
_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  0.111
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23720
_diffrn_reflns_theta_full        25.112
_diffrn_reflns_theta_max         27.595
_diffrn_reflns_theta_min         5.104
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.132
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.42
_refine_diff_density_min         -0.56
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9711
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         7022
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0996
_refine_ls_R_factor_gt           0.0694
_refine_ls_shift/su_max          0.0001713
_refine_ls_shift/su_mean         0.0000153
_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:
22.0 31.1 16.8 4.86
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1836
_refine_ls_wR_factor_gt          0.1598
_refine_ls_wR_factor_ref         0.1832
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              20
_reflns_limit_k_min              -22
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                5232
_reflns_number_total             11935
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.15
_oxford_diffrn_Wilson_scale      8.15
_oxford_refine_ls_r_factor_ref   0.0994
_oxford_refine_ls_scale          0.4211(9)
_oxford_reflns_number_all        7027
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c2cc34210c.txt
_cod_data_source_block           1Cl2
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C58 H80 Cl1 N9 O9'
_cod_database_code               7108184