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_4106524
_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 Se,H2 O,(C H2 Cl2)0.5'
_chemical_formula_sum            'C62.5 H60 Cl N6 O8 P Se'
_chemical_formula_weight         1168.54
_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                100.417(2)
_cell_angle_beta                 99.293(2)
_cell_angle_gamma                108.483(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2835(11)
_cell_length_b                   17.0534(16)
_cell_length_c                   19.5006(19)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      12
_cell_volume                     3402.5(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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0967
_diffrn_reflns_av_sigmaI/netI    0.2489
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18542
_diffrn_reflns_theta_full        23.37
_diffrn_reflns_theta_max         23.37
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.813929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_description       prism
_exptl_crystal_F_000             1214
_exptl_crystal_size_max          .1
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .05
_refine_diff_density_max         1.647
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.183
_refine_ls_extinction_coef       0.0255(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     723
_refine_ls_number_reflns         9761
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.3005
_refine_ls_R_factor_gt           0.1456
_refine_ls_shift/su_max          0.100
_refine_ls_shift/su_mean         0.010
_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          0.3702
_refine_ls_wR_factor_ref         0.4299
_reflns_number_gt                3025
_reflns_number_total             9761
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2049786_si_004.cif
_cod_data_source_block           8
_cod_original_formula_sum        'C62.50 H60 Cl N6 O8 P Se'
_cod_database_code               4106524