Switching from Separated to Contact Ion-Pair Binding Modes with Diastereomeric Calix[4]pyrrole Bis-phosphonate Receptors
Moira Ciardi; Francesca Tancini; Guzmán Gil-Ramírez; Eduardo C. Escudero Adán; Chiara Massera; Enrico Dalcanale; Pablo Ballester; Journal of the American Chemical Society 134 (2012) 13121–13132; doi:10.1021/ja305684m

data_4118485
_publ_section_title
;
 Switching from Separated to Contact Ion-Pair Binding Modes with
 Diastereomeric Calix[4]pyrrole Bis-phosphonate Receptors
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13121
_journal_page_last               13132
_journal_paper_doi               10.1021/ja305684m
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C73 H67 N9 O7 P2'
_chemical_formula_weight         1244.30
_chemical_name_systematic
;
 ?
;
_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                88.100(3)
_cell_angle_beta                 79.105(3)
_cell_angle_gamma                76.970(3)
_cell_formula_units_Z            2
_cell_length_a                   10.994(2)
_cell_length_b                   13.654(2)
_cell_length_c                   22.642(3)
_cell_measurement_reflns_used    4891
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      27.05
_cell_measurement_theta_min      0.92
_cell_volume                     3251.5(9)
_computing_data_collection       SMART
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_structure_refinement
'SHELXL-97 (G.M. Sheldrick, 2008, Acta Cryst., A64,112-122)'
_computing_structure_solution    'SIR97 (Giacovazzo et al., 1999)'
_diffrn_ambient_temperature      190(2)
_diffrn_detector_area_resol_mean '8.192 pixels/mm'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'BRUKER AXS SMART 1000'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1022
_diffrn_reflns_av_sigmaI/netI    0.2394
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            38993
_diffrn_reflns_theta_full        27.05
_diffrn_reflns_theta_max         27.05
_diffrn_reflns_theta_min         0.92
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.733007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXS SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     764
_refine_ls_number_reflns         14136
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.1889
_refine_ls_R_factor_gt           0.0642
_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^)+(0.0156P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1255
_reflns_number_gt                4340
_reflns_number_total             14136
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja305684m_si_008.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        3251.4(9)
_cod_database_code               4118485