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_7150522
_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            'C20 H8 F18 N2 O4'
_chemical_formula_weight         682.28
_chemical_melting_point          192.5(15)
_chemical_name_systematic
;\
19,20-diaza-8,17-bis[1,2,2,2-tetrafluoromethyl)ethyl]\
-7,9,16,18-tetrafluoro-2,5,11,14-\
tetraoxatricyclo[13.3.1.1^6,10^]icosa-\
1(19),6,8,10(20),15,17-hexaene
;
_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                 102.114(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.2011(5)
_cell_length_b                   8.4725(3)
_cell_length_c                   9.4479(3)
_cell_measurement_reflns_used    4496
_cell_measurement_temperature    120.0(2)
_cell_measurement_theta_max      29.8
_cell_measurement_theta_min      2.8
_cell_volume                     1111.45(7)
_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  'SHELX-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS (Sheldrick, 1990)'
_diffrn_ambient_temperature      120.0(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'Bruker SMART CCD 1K'
_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  0.0516
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12347
_diffrn_reflns_theta_full        30.31
_diffrn_reflns_theta_max         30.31
_diffrn_reflns_theta_min         1.47
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.240
_exptl_absorpt_correction_T_max  0.9858
_exptl_absorpt_correction_T_min  0.9273
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.039
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         3089
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0500P)^2^+0.6000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.1101
_reflns_number_gt                2323
_reflns_number_total             3089
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303443g.txt
_cod_data_source_block           s139
_cod_depositor_comments
;
 Correcting the _chemical_name_systematic data item value by replacing
 the '<', '>' symbols with the '^' symbol. This is the preferred way of
 denoting superscript symbols in CIF files.

 Antanas Vaitkus,
 2018-10-12

The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/adriana/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value '191-194' was changed to '192.5(15)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7150522