Polyhalogenated heterocyclic compounds. Macrocycles from perfluoro-4-isopropylpyridinePart 50. For part 49 see ref. 1.
Chambers, Richard D.; Hoskin, Philip R.; Kenwright, Alan R.; Khalil, Ali; Richmond, Paul; Sandford, Graham; Yufit, Dmitrii S.; Howard, Judith A. K.; Organic & Biomolecular Chemistry 1 (2003) 2137–; doi:10.1039/b303443g

data_7150520
_publ_section_title
;
 Polyhalogenated heterocyclic compounds. Macrocycles from
 perfluoro-4-isopropylpyridinePart 50. For part 49 see ref. 1.
;
_journal_issue                   12
_journal_name_full               'Organic &amp;  Biomolecular Chemistry'
_journal_page_first              2137
_journal_paper_doi               10.1039/b303443g
_journal_volume                  1
_journal_year                    2003
_chemical_formula_sum            'C24 H16 F18 N2 O6'
_chemical_formula_weight         770.39
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.960(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0542(4)
_cell_length_b                   14.1784(5)
_cell_length_c                   18.7552(6)
_cell_measurement_reflns_used    5732
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.6
_cell_measurement_theta_min      2.4
_cell_volume                     2864.64(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      120(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       \w-scan
_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  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0182
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            33009
_diffrn_reflns_theta_full        30.20
_diffrn_reflns_theta_max         30.20
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.202
_exptl_absorpt_correction_T_max  0.9382
_exptl_absorpt_correction_T_min  0.9308
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         7801
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+2.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1175
_reflns_number_gt                6566
_reflns_number_total             7801
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303443g.txt
_cod_data_source_block           s138
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7150520