Quantification of Nitrate-π Interactions and Selective Transport of Nitrate Using Calix[4]pyrroles with Two Aromatic Walls
Louis Adriaenssens; Carolina Estarellas; Andreas Vargas Jentzsch; Marta Martinez Belmonte; Stefan Matile; Pablo Ballester; Journal of the American Chemical Society 135 (2013) 8324–8330; doi:10.1021/ja4021793

data_4119835
_publ_section_title
;
 Quantification of Nitrate-\p Interactions and Selective Transport of
 Nitrate Using Calix[4]pyrroles with Two Aromatic Walls
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8324
_journal_page_last               8330
_journal_paper_doi               10.1021/ja4021793
_journal_volume                  135
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_sum            'C44 H51 Cl0.12 N10.88 O10.9'
_chemical_formula_weight         910.93
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_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-97
_cell_angle_alpha                109.280(3)
_cell_angle_beta                 102.198(3)
_cell_angle_gamma                91.952(3)
_cell_formula_units_Z            1
_cell_length_a                   10.0402(8)
_cell_length_b                   10.6867(8)
_cell_length_c                   11.3007(9)
_cell_measurement_reflns_used    9843
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.44
_cell_measurement_theta_min      2.29
_cell_volume                     1111.58(15)
_computing_cell_refinement       'Bruker APEX2 v2011.4-0'
_computing_data_collection       'Bruker APEX2 v2011.4-0'
_computing_data_reduction        'Bruker SAINT V7.60A'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_solution    Sir2011
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            '4K CCD area detector APEX II'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'APEX DUO Kappa 4-axis goniometer'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
_diffrn_measurement_specimen_support 'magnetic support with MicroMount'
_diffrn_radiation_monochromator  'Quazar MX Multilayer Optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            34694
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.08
_diffrn_reflns_theta_min         1.96
_diffrn_source                   'Microfocus source E025 IuS'
_diffrn_source_current           0.6
_diffrn_source_power             50
_diffrn_source_size              '0.2 mm x 0.2 mm fine focus'
_diffrn_source_type              'Bruker APEX DUO'
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_T_max  0.9947
_exptl_absorpt_correction_T_min  0.9790
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 SADABS Version 2008/1 Bruker-Nonius
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       plate
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     755
_refine_ls_number_reflns         13492
_refine_ls_number_restraints     228
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0797P)^2^+0.1791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1207
_reflns_number_gt                12866
_reflns_number_total             13492
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4021793_si_003.cif
_cod_data_source_block           mo_lab64ii_ns_0m
_cod_original_formula_sum        'C44 H51 Cl0.12 N10.88 O10.90'
_cod_database_code               4119835