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_4106523
_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,C30 H29 N2 O3 P S,2(H2 O),(C H2 Cl2)0.5'
_chemical_formula_sum            'C62.5 H63 Cl N6 O9 P S'
_chemical_formula_weight         1140.67
_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                99.9390(10)
_cell_angle_beta                 99.1520(10)
_cell_angle_gamma                108.4960(10)
_cell_formula_units_Z            2
_cell_length_a                   11.2904(9)
_cell_length_b                   17.0438(14)
_cell_length_c                   19.3603(16)
_cell_measurement_reflns_used    35
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      12
_cell_volume                     3387.7(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0526
_diffrn_reflns_av_sigmaI/netI    0.1254
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17119
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    0.165
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.812376
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_description       prism
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          .18
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .1
_refine_diff_density_max         1.067
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     808
_refine_ls_number_reflns         9666
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.2339
_refine_ls_R_factor_gt           0.1240
_refine_ls_shift/su_max          0.171
_refine_ls_shift/su_mean         0.018
_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          0.3312
_refine_ls_wR_factor_ref         0.3892
_reflns_number_gt                4024
_reflns_number_total             9666
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2049786_si_003.cif
_cod_data_source_block           7
_cod_original_formula_sum        'C62.50 H63 Cl N6 O9 P S'
_cod_database_code               4106523