Structural Study of Triazole and Amide Containing Anion-Templated Pseudorotaxanes
White, Nicholas G.; Serpell, Christopher J.; Beer, Paul D.; Crystal Growth & Design 14 (2014) 3472–; doi:10.1021/cg500420u

data_4511017
_publ_section_title
;
 Structural Study of Triazole and Amide Containing Anion-Templated
 Pseudorotaxanes
;
_journal_issue                   7
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              3472
_journal_paper_doi               10.1021/cg500420u
_journal_volume                  14
_journal_year                    2014
_chemical_absolute_configuration unk
_chemical_compound_source        synthesized
_chemical_formula_moiety         'C36 H46 N2 O9, C10 H8 N7, C7 H5 O2'
_chemical_formula_sum            'C53 H59 N9 O11'
_chemical_formula_weight         998.10
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8836(7)
_cell_length_b                   16.6797(16)
_cell_length_c                   36.187(3)
_cell_measurement_reflns_used    2879
_cell_measurement_temperature    150
_cell_measurement_theta_max      51.81
_cell_measurement_theta_min      2.91
_cell_volume                     6569.2(9)
_computing_cell_refinement       'CrysAlis Pro (Oxford Diffraction, 2010)'
_computing_data_collection       'CrysAlis Pro (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis Pro(Oxford Diffraction, 2010)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution
'isomorphic substitution from structure of 1.BzO.3'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.109
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            16049
_diffrn_reflns_theta_full        50.315
_diffrn_reflns_theta_max         51.872
_diffrn_reflns_theta_min         2.917
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.591
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.599
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis Pro (Oxford Diffraction, 2010)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.009
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_platon_squeeze_details
;
;
_refine_diff_density_max         0.73
_refine_diff_density_min         -0.46
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1233
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         5230
_refine_ls_number_restraints     699
_refine_ls_R_factor_all          0.1582
_refine_ls_R_factor_gt           0.1245
_refine_ls_shift/su_max          0.0003781
_refine_ls_shift/su_mean         0.0000393
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.20P)^2^ + 0.00P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3545
_refine_ls_wR_factor_gt          0.3145
_refine_ls_wR_factor_ref         0.3545
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              36
_reflns_limit_l_min              0
_reflns_number_gt                3318
_reflns_number_total             6913
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.53
_oxford_diffrn_Wilson_scale      1.15
_oxford_refine_ls_r_factor_ref   0.1582
_oxford_refine_ls_scale          1.187(15)
_oxford_reflns_number_all        5230
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            cg500420u_si_001.cif
_cod_data_source_block           1.BzO.2
_cod_depositor_comments
'Adding full bibliography for 4511009--4511017.cif.'
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_database_code               4511017