Ditopic N-Crowned 4-(p-Aminophenyl)-2,6-diphenylpyridines: Implications of Macrocycle Topology on the Spectroscopic Properties, Cation Complexation, and Differential Anion Responses
Beatriz García-Acosta; Ramón Martínez-Máñez; Félix Sancenón; Juan Soto; Knut Rurack; Monika Spieles; Eduardo García-Breijo; Luis Gil; Inorganic Chemistry 46 (2007) 3123–3135; doi:10.1021/ic062069z

data_4307591
_publ_section_title
;
Ditopic N-Crowned 4-(p-Aminophenyl)-2,6-diphenylpyridines: Implications
of Macrocycle Topology on the Spectroscopic Properties, Cation
Complexation, and Differential Anion Responses
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3123
_journal_page_last               3135
_journal_paper_doi               10.1021/ic062069z
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C33 H36 N2 O2 S2'
_chemical_formula_weight         556.76
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.10(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.548(2)
_cell_length_b                   10.067(2)
_cell_length_c                   33.777(8)
_cell_measurement_reflns_used    70
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.56
_cell_measurement_theta_min      4.78
_cell_volume                     2906.6(11)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            6864
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        4.56
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.216
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.838
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_description       Monoclinic_crystals
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.037
_refine_ls_extinction_coef       0.0073(6)
_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   0.954
_refine_ls_goodness_of_fit_obs   0.907
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5014
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.749
_refine_ls_restrained_S_obs      0.907
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_obs          0.0429
_refine_ls_shift/esd_max         -0.031
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+1.9614P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2270
_refine_ls_wR_factor_obs         0.1026
_reflns_number_observed          3845
_reflns_number_total             5069
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic062069zsi20061030_050137.cif
_cod_data_source_block           feincs
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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^)+(0.0503P)^2^+1.9614P] 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^)+(0.0503P)^2^+1.9614P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2906.7(10)
_cod_database_code               4307591