Clathrate and channel inclusion systems co-exist in the crystal structure of a bis-C-pivot macrocycle (Z′ = 2)
Bilge, Selen; Coles, Simon J.; Davies, David B.; Hursthouse, Michael B.; Kılıç, Zeynel; Rutherford, John S.; Shaw, Robert A.; CrystEngComm 10 (2008) 873–; doi:10.1039/b716882a

data_7201825
_publ_section_title
;
 Clathrate and channel inclusion systems co-exist in the crystal
 structure of a bis-C-pivot macrocycle (Z&#x2032; = 2)
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              873
_journal_paper_doi               10.1039/b716882a
_journal_volume                  10
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C26 H40 N2 O9 P2, C4 H8 O, C H4 O'
_chemical_formula_sum            'C31 H52 N2 O11 P2'
_chemical_formula_weight         690.69
_chemical_name_systematic
;
15,22-bis(dimethoxyphosphoryl)-2,5,8-trioxa-
16,21-diazatricyclo[21.4.0.0^9,14^]heptacosa-
9,11,13,23,25,27(1)-hexaene tetrahydrofuran methanol
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     vecmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2007-07-27 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.6305(4)
_cell_length_b                   16.7308(5)
_cell_length_c                   24.0702(5)
_cell_measurement_temperature    120(2)
_cell_volume                     6697.3(3)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF (Buerskens et al., 1996)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type
'Bruker-Nonius Roper CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2078
_diffrn_reflns_av_sigmaI/netI    0.1746
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            35912
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    0.192
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.143
_refine_ls_abs_structure_details
;
Crystal was refined as an inversion twin. Refined fraction of inverted component
0.38(15)
;
_refine_ls_extinction_coef       0.0198(16)
_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   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     797
_refine_ls_number_reflns         14109
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1371
_refine_ls_R_factor_gt           0.0893
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1408P)^2^+8.9372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2263
_refine_ls_wR_factor_ref         0.2658
_reflns_number_gt                9597
_reflns_number_total             14109
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b716882a.txt
_cod_data_source_block           03src0788
_cod_database_code               7201825