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_4106522
_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         'C62 H57 N6 O8 P,C H2 Cl2,H2 O'
_chemical_formula_sum            'C63 H61 Cl2 N6 O9 P'
_chemical_formula_weight         1148.05
_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                66.344(14)
_cell_angle_beta                 83.747(19)
_cell_angle_gamma                84.97(2)
_cell_formula_units_Z            2
_cell_length_a                   11.195(3)
_cell_length_b                   16.747(4)
_cell_length_c                   16.954(3)
_cell_measurement_reflns_used    5944
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      28.6
_cell_measurement_theta_min      2.2
_cell_volume                     2890.8(12)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2004)'
_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      93(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1008
_diffrn_reflns_av_sigmaI/netI    0.2022
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18443
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.33
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    0.203
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.8357
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1204
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.779
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.231
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         10218
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.223
_refine_ls_R_factor_all          0.2643
_refine_ls_R_factor_gt           0.1684
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4024
_refine_ls_wR_factor_ref         0.4691
_reflns_number_gt                4636
_reflns_number_total             10218
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2049786_si_002.cif
_cod_data_source_block           6
_cod_database_code               4106522