Phosphorus-Based Functional Groups as Hydrogen Bonding Templates for Rotaxane Formation
Rehan Ahmed; Andrea Altieri; Daniel M. D'Souza; David A. Leigh; Kathleen M. Mullen; Marcus Papmeyer; Alexandra M. Z. Slawin; Jenny K. Y. Wong; J. Derek Woollins; Journal of the American Chemical Society 133 (2011) 12304–12310; doi:10.1021/ja2049786

data_4106525
_publ_section_title
;
 Phosphorus-Based Functional Groups as Hydrogen Bonding Templates for
 Rotaxane Formation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12304
_journal_page_last               12310
_journal_paper_doi               10.1021/ja2049786
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C32 H28 N4 O4,C26 H26 N2 O2 P2,2(C H Cl3)'
_chemical_formula_sum            'C60 H56 Cl6 N6 O6 P2'
_chemical_formula_weight         1231.75
_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                75.17(4)
_cell_angle_beta                 65.18(5)
_cell_angle_gamma                79.37(5)
_cell_formula_units_Z            1
_cell_length_a                   10.159(2)
_cell_length_b                   12.609(5)
_cell_length_c                   13.2847(17)
_cell_measurement_reflns_used    1124
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.1987
_cell_measurement_theta_min      3.5898
_cell_volume                     1487.3(9)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.742
_diffrn_measured_fraction_theta_max 0.720
_diffrn_measurement_device_type  ccd
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1946
_diffrn_reflns_av_sigmaI/netI    0.1232
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10872
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         70.08
_diffrn_reflns_theta_min         3.64
_exptl_absorpt_coefficient_mu    3.596
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.6148
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Corp., 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       prism
_exptl_crystal_F_000             638
_exptl_crystal_size_max          .1
_exptl_crystal_size_mid          .05
_exptl_crystal_size_min          .05
_refine_diff_density_max         1.189
_refine_diff_density_min         -1.044
_refine_diff_density_rms         0.263
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.464
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         4074
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      2.447
_refine_ls_R_factor_all          0.2632
_refine_ls_R_factor_gt           0.2367
_refine_ls_shift/su_max          0.071
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5928
_refine_ls_wR_factor_ref         0.6115
_reflns_number_gt                3350
_reflns_number_total             4074
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2049786_si_005.cif
_cod_data_source_block           12
_cod_original_cell_volume        1487.4(7)
_cod_database_code               4106525