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_4106526
_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,C27 H27 N1 O2 P2,2(H2 O)'
_chemical_formula_sum            'C59 H59 N5 O8 P2'
_chemical_formula_weight         1028.05
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.17
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.3677(17)
_cell_length_b                   11.6746(15)
_cell_length_c                   17.642(2)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      12
_cell_volume                     2710.0(6)
_computing_cell_refinement       SMART/SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1921
_diffrn_reflns_av_sigmaI/netI    0.1538
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13440
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.140
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.579408
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       prism
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          .12
_exptl_crystal_size_mid          .08
_exptl_crystal_size_min          .03
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         3898
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.2006
_refine_ls_R_factor_gt           0.0780
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0598P)^2^+2.4612P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1529
_refine_ls_wR_factor_ref         0.2068
_reflns_number_gt                1699
_reflns_number_total             3898
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2049786_si_006.cif
_cod_data_source_block           17
_cod_original_cell_volume        2709.9(6)
_cod_database_code               4106526