P,N-Containing cyclophanes with large helical hydrophobic cavities: prospective precursors for the design of a molecular reactor
Karasik, A. A.; Kulikov, D. V.; Balueva, A. S.; Ignat'eva, S. N.; Kataeva, O. N.; Lönnecke, P.; Kozlov, A. V.; Latypov, S. K.; Hey-Hawkins, E.; Sinyashin, O. G.; Dalton Transactions  (2009) 490–494; doi:10.1039/b812508b

data_7000317
_publ_section_title
;
 P,N-Containing cyclophanes with large helical hydrophobic cavities:
 prospective precursors for the design of a molecular reactor
;
_journal_issue                   3
_journal_name_full               'Dalton Transactions'
_journal_page_first              490
_journal_page_last               494
_journal_paper_doi               10.1039/b812508b
_journal_year                    2009
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C116 H156 N4 P4, C6 H6'
_chemical_formula_sum            'C164 H204 N4 P4'
_chemical_formula_weight         2355.19
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                80.860(10)
_cell_angle_beta                 73.850(10)
_cell_angle_gamma                76.480(10)
_cell_formula_units_Z            2
_cell_length_a                   15.3460(10)
_cell_length_b                   19.3170(10)
_cell_length_c                   26.2610(10)
_cell_measurement_reflns_used    628
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      19.46
_cell_measurement_theta_min      4.61
_cell_volume                     7233.6(8)
_computing_cell_refinement       'Dirax/lsq (Duisenberg, 1992)'
_computing_data_collection       'Collect (Nonius BV, 1999)'
_computing_data_reduction        'EvalCCD (Duisenberg et al., 2003)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material
'WinGX (Farrugia 1999), enCIFer (Allen et al. 2004)'
_computing_structure_refinement
'SHELXL-97 (Sheldrick, 1997), WinGX (Farrugia 1999), PLATON (Spek 2005)'
_computing_structure_solution    'SIR2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      198(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       \f
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            151059
_diffrn_reflns_theta_full        25.40
_diffrn_reflns_theta_max         25.40
_diffrn_reflns_theta_min         3.07
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_T_max  0.9847
_exptl_absorpt_correction_T_min  0.8141
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS version 2.10 (Sheldrick,Bruker AXS Inc.,2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2552
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1573
_refine_ls_number_reflns         26405
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0566
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+5.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1188
_refine_ls_wR_factor_ref         0.1376
_reflns_number_gt                18022
_reflns_number_total             26405
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b812508b.txt
_cod_data_source_block           balu1
_cod_original_cell_volume        7233.6(7)
_cod_database_code               7000317