Tetrakis(2,3,5,6-tetrafluoro-4-iodophenyloxymethyl)methane bis(pyridine <i>N</i>-oxide) monohydrate
Emanuela Guido; Pierangelo Metrangolo; Tullio Pilati; Giuseppe Resnati; Acta Crystallographica Section E 60 (2004) o788–o790; doi:10.1107/S1600536804008438

data_2203637
_publ_section_title
;
 Tetrakis(2,3,5,6-tetrafluoro-4-iodophenyloxymethyl)methane
 bis(pyridine <i>N</i>-oxide) monohydrate
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o788
_journal_page_last               o790
_journal_paper_doi               10.1107/S1600536804008438
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C29 H8 F16 I4 O4, 2C5 H5 N O, H2 O'
_chemical_formula_moiety         'C29 H8 F16 I4 O4, 2C5 H5 N O, H2 O'
_chemical_formula_sum            'C39 H20 F16 I4 N2 O7'
_chemical_formula_weight         1440.17
_chemical_name_systematic
;
Tetrakis(2,3,5,6-tetrafluoro-4-iodophenyoxymethyl)methane
bis(pyridine N-oxide) monohydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                76.25(5)
_cell_angle_beta                 82.28(5)
_cell_angle_gamma                89.73(5)
_cell_formula_units_Z            2
_cell_length_a                   8.034(2)
_cell_length_b                   13.412(3)
_cell_length_c                   21.624(5)
_cell_measurement_reflns_used    2447
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.570
_cell_measurement_theta_min      2.783
_cell_volume                     2241.8(11)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material
;
SHELXL97, PARST (Nardelli, 1983) and GEO (Pilati, 2004)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       '\w and \f'
_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  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18906
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        23.
_exptl_absorpt_coefficient_mu    2.897
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_correction_T_min  0.744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.133
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.634
_refine_diff_density_min         -0.398
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.913
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         7905
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.913
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0638P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.0993
_reflns_number_gt                5029
_reflns_number_total             7905
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            na6314.cif
_cod_data_source_block           I
_cod_original_cell_volume        2241.9(9)
_cod_database_code               2203637
_cod_database_fobs_code          2203637