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_7150521
_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            'C30 H12 F18 N2 O4'
_chemical_formula_weight         806.42
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 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                 113.78(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.473(3)
_cell_length_b                   23.261(5)
_cell_length_c                   11.079(2)
_cell_measurement_reflns_used    7295
_cell_measurement_temperature    120.0(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2.2
_cell_volume                     3177.3(14)
_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      120.0(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15431
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.182
_exptl_absorpt_correction_T_max  0.9644
_exptl_absorpt_correction_T_min  0.9208
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.745
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         5778
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.1322
_refine_ls_R_factor_gt           0.1168
_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 
[1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ 
[\s^2^(Fo^2^)+0.0000+24.0000*P+(0.1400P)^2^+0.0000sin\q/\l] 
where P = 1.00000Fo^2^ + 0.00000Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2795
_refine_ls_wR_factor_ref         0.3100
_reflns_number_gt                4792
_reflns_number_total             5778
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303443g.txt
_cod_data_source_block           103s
_cod_original_cell_volume        3177.2(11)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7150521