Molecular Recognition of Pyridine N-Oxides in Water Using Calix[4]pyrrole Receptors
Begoña Verdejo; Guzmán Gil-Ramírez; Pablo Ballester; Journal of the American Chemical Society 131 (2009) 3178–3179; doi:10.1021/ja900151u

data_4104308
_publ_section_title
;
 Molecular Recognition of Pyridine N-Oxides in Water Using Calix[4]pyrrole
 Receptors
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3178
_journal_page_last               3179
_journal_paper_doi               10.1021/ja900151u
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C69 H74 N7 O14.5'
_chemical_formula_weight         1233.35
_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-97
_cell_angle_alpha                87.207(2)
_cell_angle_beta                 85.586(2)
_cell_angle_gamma                73.617(2)
_cell_formula_units_Z            2
_cell_length_a                   11.0003(5)
_cell_length_b                   13.8639(6)
_cell_length_c                   21.2479(9)
_cell_measurement_reflns_used    7305
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.63
_cell_measurement_theta_min      3.59
_cell_volume                     3098.4(2)
_computing_cell_refinement       'Bruker-Nonius Apex v1.0-22 2002'
_computing_data_collection       'Bruker-Nonius Apex v1.0-22 2002'
_computing_data_reduction        'SAINT+ Version 7.06A Bruker-Nonius, 2004'
_computing_molecular_graphics    'Shelxtl Version 6.12 (Sheldrick, 2001)'
_computing_publication_material  'Shelxtl Version 6.12 (Sheldrick, 2001)'
_computing_structure_refinement  'Shelxtl Version 6.12 (Sheldrick, 2001)'
_computing_structure_solution    'Shelxtl Version 6.12 (Sheldrick, 2001)'
_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 0.897
_diffrn_measured_fraction_theta_max 0.897
_diffrn_measurement_device_type  'Kappa 4-axis goniometer bruker-nonius'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
_diffrn_measurement_specimen_support
'magnetic support whith 10 micron nylon fiber cryoloop'
_diffrn_radiation_monochromator  'Multilayer Montel 200 mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_sigmaI/netI    0.0555
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            73849
_diffrn_reflns_theta_full        38.31
_diffrn_reflns_theta_max         38.31
_diffrn_reflns_theta_min         2.64
_diffrn_source                   'rotating anode X-ray tube'
_diffrn_source_current           70
_diffrn_source_power             50
_diffrn_source_size              '3 mm x 0.3 mm fine focus'
_diffrn_source_type              'Bruker-Nonius FR 591'
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9671
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 SADABS Version 2.1 2003 Bruker-Nonius
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1306
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     911
_refine_ls_number_reflns         30911
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0635
_refine_ls_shift/su_max          0.137
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0964P)^2^+1.0385P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1721
_refine_ls_wR_factor_ref         0.1897
_reflns_number_gt                23068
_reflns_number_total             30911
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja900151u_si_004.cif
_cod_data_source_block           bv103meno_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_diffrn_measurement_specimen_suppport' was replaced with
'_diffrn_measurement_specimen_support' as specified in the
replacement file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C69 H74 N7 O14.50'
_cod_database_code               4104308