Proton ionizable 1H-1,2,4-triazole π-electron deficient cyclophanes as hosts and in [2]catenanes
Ramos, Susana; Alcalde, Ermitas; Fraser Stoddart, J.; P. White, Andrew J.; Williams, David J.; Pérez-García, Lluïsa; New Journal of Chemistry 33 (2009) 300–; doi:10.1039/b815355h

data_7051633
_publ_section_title
;
 Proton ionizable 1H-1,2,4-triazole \p-electron deficient cyclophanes
 as hosts and in [2]catenanes
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              300
_journal_paper_doi               10.1039/b815355h
_journal_volume                  33
_journal_year                    2009
_chemical_formula_moiety         'C28 H40 O10, C32 H29 N7, 4(F6 P), 4(C2 H3 N)'
_chemical_formula_sum            'C68 H81 F24 N11 O10 P4'
_chemical_formula_weight         1792.32
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                71.118(5)
_cell_angle_beta                 74.753(5)
_cell_angle_gamma                78.274(5)
_cell_formula_units_Z            2
_cell_length_a                   13.5888(7)
_cell_length_b                   14.7300(10)
_cell_length_c                   22.343(2)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      27.99
_cell_measurement_theta_min      11.03
_cell_volume                     4048.3(5)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12374
_diffrn_reflns_theta_max         60.00
_diffrn_reflns_theta_min         2.14
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.906
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       rhombs
_exptl_crystal_F_000             1844
_exptl_crystal_size_max          0.67
_exptl_crystal_size_mid          0.57
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.940
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.00026(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.049
_refine_ls_goodness_of_fit_obs   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1123
_refine_ls_number_reflns         10953
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.092
_refine_ls_restrained_S_obs      1.129
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_obs          0.0709
_refine_ls_shift/esd_max         0.159
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1090P)^2^+4.0511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2082
_refine_ls_wR_factor_obs         0.1836
_reflns_number_observed          8887
_reflns_number_total             11798
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b815355h.txt
_cod_data_source_block           10_4PF6
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1090P)^2^+4.0511P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1090P)^2^+4.0511P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7051633