#------------------------------------------------------------------------------
#$Date: 2019-03-05 09:52:05 +0100 (Tue 05 de Mar de 2019) $
#$Revision: 213973 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/06/7050632.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7050632
loop_
_publ_author_name
'Chu, Qianli'
'Wang, Zheming'
'Huang, Qichen'
'Yan, Chunhua'
'Zhu, Shizheng'
_publ_section_title
;
 Fluorine-containing donor-acceptor complexes: crystallographic study
 of the interactions between electronegative atoms (N, O, S) and
 halogen atoms (I, Br)
;
_journal_issue                   10
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1522
_journal_paper_doi               10.1039/b305312c
_journal_volume                  27
_journal_year                    2003
_chemical_formula_sum            'C8 H18 F4 I2 N3 O P'
_chemical_formula_weight         533.02
_chemical_melting_point          363
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 101.89(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.0280(14)
_cell_length_b                   16.461(3)
_cell_length_c                   14.947(3)
_cell_measurement_temperature    180(2)
_cell_volume                     1692.1(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_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  0.0541
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26197
_diffrn_reflns_theta_full        30.02
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         3.73
_exptl_absorpt_coefficient_mu    3.846
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.092
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.42
_refine_diff_density_max         7.122
_refine_diff_density_min         -1.754
_refine_diff_density_rms         0.360
_refine_ls_extinction_coef       0.0011(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         4806
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0584
_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/[σ²(Fo²)+(0.1111P)²+20.6789P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1818
_refine_ls_wR_factor_ref         0.1886
_reflns_number_gt                4095
_reflns_number_total             4806
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b305312c.txt
_cod_data_source_block           Comp10
_cod_database_code               7050632
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.26639(7) 0.61557(3) 0.94292(3) 0.02304(18) Uani 1 1 d . . .
I2 I 0.64548(7) 0.36488(3) 0.56299(3) 0.02551(18) Uani 1 1 d . . .
P3 P 0.0438(2) 0.27607(11) 0.74432(13) 0.0185(3) Uani 1 1 d . . .
O1 O -0.0989(7) 0.2488(3) 0.6619(4) 0.0231(10) Uani 1 1 d . . .
F1 F 0.4523(9) 0.5286(4) 1.1056(3) 0.0435(14) Uani 1 1 d . . .
F2 F 0.2851(8) 0.4486(3) 1.0049(5) 0.0435(14) Uani 1 1 d . . .
F3 F 0.4525(12) 0.4463(4) 0.3979(4) 0.0548(19) Uani 1 1 d . . .
N2 N 0.0619(11) 0.3735(4) 0.7667(5) 0.0299(15) Uani 1 1 d . . .
F4 F 0.2812(8) 0.4511(4) 0.5020(5) 0.0534(17) Uani 1 1 d . . .
N3 N 0.2651(9) 0.2509(4) 0.7330(5) 0.0282(14) Uani 1 1 d . . .
N1 N -0.0184(10) 0.2381(4) 0.8372(5) 0.0253(13) Uani 1 1 d . . .
C8 C 0.4072(11) 0.5124(4) 1.0154(5) 0.0222(13) Uani 1 1 d . . .
C2 C -0.0978(14) 0.1543(6) 0.8283(6) 0.0341(18) Uani 1 1 d . . .
C7 C 0.4643(12) 0.4573(5) 0.4873(6) 0.0288(16) Uani 1 1 d . . .
C6 C 0.2946(14) 0.1844(6) 0.6728(7) 0.039(2) Uani 1 1 d . . .
C3 C -0.0836(13) 0.4165(5) 0.8082(6) 0.0328(18) Uani 1 1 d . . .
C5 C 0.4398(13) 0.2733(7) 0.8002(7) 0.040(2) Uani 1 1 d . . .
C4 C 0.1603(14) 0.4279(5) 0.7118(7) 0.0362(19) Uani 1 1 d . . .
C1 C 0.1008(14) 0.2540(6) 0.9286(6) 0.0351(18) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O P N1 118.4(3) . . ?
O P N3 109.1(3) . . ?
N1 P N3 103.5(4) . . ?
O P N2 109.1(3) . . ?
N1 P N2 102.6(4) . . ?
N3 P N2 114.1(4) . . ?
C1 N1 C2 112.9(7) . . ?
C1 N1 P 121.6(6) . . ?
C2 N1 P 120.0(6) . . ?
C4 N2 C3 112.4(7) . . ?
C4 N2 P 120.9(6) . . ?
C3 N2 P 115.6(5) . . ?
C5 N3 C6 113.5(7) . . ?
C5 N3 P 120.6(6) . . ?
C6 N3 P 123.0(6) . . ?
F2 C7 F1 106.6(6) . . ?
F2 C7 C7 108.8(8) . 3_456 ?
F1 C7 C7 108.1(8) . 3_456 ?
F2 C7 I1 110.1(5) . . ?
F1 C7 I1 109.7(5) . . ?
C7 C7 I1 113.2(6) 3_456 . ?
F3 C8 F4 106.6(7) . . ?
F3 C8 C8 108.9(9) . 3_466 ?
F4 C8 C8 108.1(8) . 3_466 ?
F3 C8 I2 109.8(5) . . ?
F4 C8 I2 110.0(5) . . ?
C8 C8 I2 113.2(7) 3_466 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O P 1.489(5) . ?
P N1 1.639(6) . ?
P N3 1.650(6) . ?
P N2 1.664(7) . ?
N1 C1 1.469(11) . ?
N1 C2 1.473(11) . ?
N2 C4 1.466(11) . ?
N2 C3 1.481(11) . ?
N3 C5 1.453(11) . ?
N3 C6 1.458(11) . ?
I1 C7 2.143(7) . ?
C7 F2 1.344(8) . ?
C7 F1 1.349(9) . ?
C7 C7 1.526(14) 3_456 ?
I2 C8 2.150(7) . ?
C8 F3 1.336(10) . ?
C8 F4 1.350(10) . ?
C8 C8 1.519(15) 3_466 ?
