Polyatomic Anion Assistance in the Assembly of [2]Pseudorotaxanes
Virginia Valderrey; Eduardo C. Escudero-Adán; Pablo Ballester; Journal of the American Chemical Society 134 (2012) 10733–10736; doi:10.1021/ja301900s

data_4118171
_publ_section_title
;
 Polyatomic Anion Assistance in the Assembly of [2]Pseudorotaxanes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10733
_journal_page_last               10736
_journal_paper_doi               10.1021/ja301900s
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C202 H200 N28 O6'
_chemical_formula_weight         3115.90
_chemical_name_systematic
; 
 ? 
;
_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                 106.645(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   10.7378(18)
_cell_length_b                   22.469(4)
_cell_length_c                   18.161(3)
_cell_measurement_reflns_used    1150
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      16.01
_cell_measurement_theta_min      2.18
_cell_volume                     4198.1(12)
_computing_cell_refinement       'Bruker APEX2 v2011.4-0'
_computing_data_collection       'Bruker APEX2 v2011.4-0'
_computing_data_reduction        'Bruker SAINT V7.60A'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_solution    Sir2011
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            '4K CCD area detector APEX II'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'APEX DUO Kappa 4-axis goniometer'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
_diffrn_measurement_specimen_support 'magnetic support whith MicroMount'
_diffrn_radiation_monochromator  'Quazar MX Multilayer Optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0550
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5115
_diffrn_reflns_theta_full        21.98
_diffrn_reflns_theta_max         21.98
_diffrn_reflns_theta_min         1.48
_diffrn_source                   'Micorfocus source E025 IuS'
_diffrn_source_current           0.6
_diffrn_source_power             50
_diffrn_source_size              '0.2 mm x 0.2 mm fine focus'
_diffrn_source_type              'Bruker APEX DUO'
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  0.9962
_exptl_absorpt_correction_T_min  0.9924
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 TWINABS Version 2008/0 Bruker-Nonius
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_description       Block
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         5115
_refine_ls_number_restraints     752
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.1649
_refine_ls_R_factor_gt           0.1291
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1467P)^2^+25.1448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3270
_refine_ls_wR_factor_ref         0.3480
_reflns_number_gt                3809
_reflns_number_total             5115
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja301900s_si_003.cif
_cod_data_source_block           mo_vv039_04
_cod_original_cell_volume        4198.0(12)
_cod_database_code               4118171