#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/10/37/7103707.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_7103707
loop_
_publ_author_name
'Ochiai, Masahito'
'Suefuji, Takashi'
'Miyamoto, Kazunori'
'Shiro, Motoo'
_publ_section_title
;
 Solid state structures of pentacoordinated λ3-iodanes with a trigonal
 bipyramidal geometry: synthesis of diphenyl- and alkynyl(phenyl)-λ3-iodane
 complexes with 1,10-phenanthroline
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   12
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              1438
_journal_page_last               1439
_journal_paper_doi               10.1039/b302579a
_journal_year                    2003
_chemical_formula_moiety         'C12 H14 I 1+, B F4 1-, C12 H8 N2'
_chemical_formula_sum            'C24 H22 B F4 I N2'
_chemical_formula_weight         552.16
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             'Tue Sep 17 16:28:59 2002'
_audit_creation_method           'by teXsan'
_cell_angle_alpha                90
_cell_angle_beta                 102.80(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.183(2)
_cell_length_b                   17.257(5)
_cell_length_c                   18.711(5)
_cell_measurement_reflns_used    19352
_cell_measurement_temperature    93.2
_cell_measurement_theta_max      30.1
_cell_measurement_theta_min      3.1
_cell_volume                     2261(1)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'teXsan (MSC & Rigaku, 1999)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'teXsan (MSC & Rigaku, 1999)'
_computing_structure_refinement  'teXsan (MSC & Rigaku, 1999)'
_computing_structure_solution    'PATTY (Beurskens, 1994)'
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9747
_diffrn_measured_fraction_theta_max 0.9747
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       ?w
_diffrn_radiation_type           'Mo K?a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            25941
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_exptl_absorpt_coefficient_mu    1.463
_exptl_absorpt_correction_T_max  0.864
_exptl_absorpt_correction_T_min  0.599
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1096.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.95
_refine_diff_density_min         -1.48
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     289
_refine_ls_number_reflns         6445
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.0009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[?s²(Fo²) + (0.00200(Max(Fo²,0) + 2Fc²)/3)²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0489
_reflns_number_gt                4364
_reflns_number_total             6445
_reflns_threshold_expression     F²>2.0?s(F²)
_cod_data_source_file            b302579a.txt
_cod_data_source_block           General1
_cod_database_code               7103707
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,1/2+y,1/2-z
-x,-y,-z
x,1/2-y,1/2+z
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.56963(2) 0.235942(9) 0.44244(1) 0.01696(3) Uani 1.00 d . . .
F1 F 0.4047(2) 0.20777(9) 0.56707(9) 0.0346(5) Uani 1.00 d . . .
F2 F 0.0841(2) 0.18921(10) 0.54952(9) 0.0399(5) Uani 1.00 d . . .
F3 F 0.2901(3) 0.11477(9) 0.63156(10) 0.0431(5) Uani 1.00 d . . .
F4 F 0.2519(2) 0.2421(1) 0.65568(8) 0.0322(5) Uani 1.00 d . . .
N1 N 0.7456(3) 0.3614(1) 0.5075(1) 0.0172(5) Uani 1.00 d . . .
N2 N 0.5401(3) 0.4094(1) 0.3715(1) 0.0208(6) Uani 1.00 d . . .
C1 C 0.7233(3) 0.2489(1) 0.3591(1) 0.0152(6) Uani 1.00 d . . .
C2 C 0.9191(3) 0.2561(1) 0.3799(1) 0.0214(6) Uani 1.00 d . . .
C3 C 1.0172(3) 0.2694(2) 0.3248(1) 0.0245(7) Uani 1.00 d . . .
C4 C 0.9210(4) 0.2742(2) 0.2523(1) 0.0243(7) Uani 1.00 d . . .
C5 C 0.7251(3) 0.2653(2) 0.2335(1) 0.0233(6) Uani 1.00 d . . .
C6 C 0.6222(3) 0.2524(1) 0.2873(1) 0.0210(7) Uani 1.00 d . . .
C7 C 0.4373(4) 0.1361(1) 0.4018(1) 0.0227(7) Uani 1.00 d . . .
C8 C 0.3281(4) 0.0833(1) 0.3934(1) 0.0191(7) Uani 1.00 d . . .
C9 C 0.1917(4) 0.0183(1) 0.3843(1) 0.0204(7) Uani 1.00 d . . .
C10 C 0.2688(6) -0.0443(2) 0.4394(3) 0.078(1) Uani 1.00 d . . .
C11 C 0.0032(5) 0.0481(2) 0.3979(3) 0.071(1) Uani 1.00 d . . .
C12 C 0.1587(7) -0.0129(2) 0.3077(2) 0.083(2) Uani 1.00 d . . .
C13 C 0.8437(4) 0.3400(1) 0.5734(1) 0.0202(7) Uani 1.00 d . . .
C14 C 0.9317(4) 0.3916(2) 0.6278(1) 0.0242(7) Uani 1.00 d . . .
C15 C 0.9157(4) 0.4694(2) 0.6128(1) 0.0245(7) Uani 1.00 d . . .
C16 C 0.8153(3) 0.4947(1) 0.5441(1) 0.0201(7) Uani 1.00 d . . .
C17 C 0.7994(4) 0.5753(1) 0.5254(2) 0.0238(7) Uani 1.00 d . . .
C18 C 0.7067(4) 0.5991(1) 0.4587(2) 0.0254(8) Uani 1.00 d . . .
C19 C 0.6186(4) 0.5442(1) 0.4037(2) 0.0211(7) Uani 1.00 d . . .
C20 C 0.5235(4) 0.5669(2) 0.3329(2) 0.0283(8) Uani 1.00 d . . .
C21 C 0.4402(4) 0.5118(2) 0.2837(2) 0.0312(8) Uani 1.00 d . . .
C22 C 0.4502(4) 0.4340(2) 0.3059(2) 0.0268(8) Uani 1.00 d . . .
C23 C 0.6260(3) 0.4642(1) 0.4202(1) 0.0188(7) Uani 1.00 d . . .
C24 C 0.7304(3) 0.4387(1) 0.4920(1) 0.0166(6) Uani 1.00 d . . .
B1 B 0.2562(4) 0.1878(2) 0.6013(2) 0.0223(8) Uani 1.00 d . . .
H1 H 0.9850 0.2525 0.4298 0.0272 Uiso 1.00 calc . . .
H2 H 1.1527 0.2749 0.3372 0.0310 Uiso 1.00 calc . . .
H3 H 0.9903 0.2841 0.2153 0.0294 Uiso 1.00 calc . . .
H4 H 0.6596 0.2672 0.1833 0.0299 Uiso 1.00 calc . . .
H5 H 0.4865 0.2462 0.2749 0.0239 Uiso 1.00 calc . . .
H6 H 0.3631 -0.0731 0.4235 0.0881 Uiso 1.00 calc . . .
H7 H 0.1663 -0.0776 0.4446 0.0881 Uiso 1.00 calc . . .
H8 H 0.3213 -0.0209 0.4856 0.0881 Uiso 1.00 calc . . .
H9 H -0.0827 0.0063 0.3977 0.0834 Uiso 1.00 calc . . .
H10 H 0.0233 0.0747 0.4431 0.0834 Uiso 1.00 calc . . .
H11 H -0.0531 0.0835 0.3592 0.0834 Uiso 1.00 calc . . .
H12 H 0.1679 0.0276 0.2745 0.0957 Uiso 1.00 calc . . .
H13 H 0.0369 -0.0364 0.2947 0.0957 Uiso 1.00 calc . . .
H14 H 0.2544 -0.0512 0.3053 0.0957 Uiso 1.00 calc . . .
H15 H 0.8555 0.2859 0.5840 0.0251 Uiso 1.00 calc . . .
H16 H 1.0004 0.3736 0.6743 0.0308 Uiso 1.00 calc . . .
H17 H 0.9726 0.5062 0.6492 0.0296 Uiso 1.00 calc . . .
H18 H 0.8555 0.6126 0.5612 0.0315 Uiso 1.00 calc . . .
H19 H 0.6989 0.6528 0.4476 0.0317 Uiso 1.00 calc . . .
H20 H 0.5163 0.6203 0.3196 0.0363 Uiso 1.00 calc . . .
H21 H 0.3770 0.5259 0.2350 0.0373 Uiso 1.00 calc . . .
H22 H 0.3882 0.3961 0.2714 0.0326 Uiso 1.00 calc . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
B B 0.001 0.001
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
F F 0.017 0.010
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
I I -0.474 1.812
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
N N 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 I1 C7 95.23(9) . . . yes
C13 N1 C24 118.0(2) . . . yes
C22 N2 C23 117.0(2) . . . yes
I1 C1 C2 118.0(2) . . . yes
I1 C1 C6 118.4(2) . . . yes
C2 C1 C6 123.6(2) . . . yes
C1 C2 C3 117.3(2) . . . yes
C1 C2 H1 121.7 . . . no
C3 C2 H1 121.0 . . . no
C2 C3 C4 120.8(2) . . . yes
C2 C3 H2 119.6 . . . no
C4 C3 H2 119.6 . . . no
C3 C4 C5 120.2(2) . . . yes
C3 C4 H3 119.7 . . . no
C5 C4 H3 120.1 . . . no
C4 C5 C6 120.5(2) . . . yes
C4 C5 H4 120.0 . . . no
C6 C5 H4 119.5 . . . no
C1 C6 C5 117.5(2) . . . yes
C1 C6 H5 121.3 . . . no
C5 C6 H5 121.2 . . . no
I1 C7 C8 159.8(2) . . . yes
C7 C8 C9 178.9(3) . . . yes
C8 C9 C10 109.4(2) . . . yes
C8 C9 C11 108.5(2) . . . yes
C8 C9 C12 110.1(2) . . . yes
C10 C9 C11 109.5(3) . . . yes
C10 C9 C12 110.5(3) . . . yes
C11 C9 C12 108.8(3) . . . yes
C9 C10 H6 110.1 . . . no
C9 C10 H7 109.0 . . . no
C9 C10 H8 109.1 . . . no
H6 C10 H7 109.9 . . . no
H6 C10 H8 110.0 . . . no
H7 C10 H8 108.6 . . . no
C9 C11 H9 110.2 . . . no
C9 C11 H10 110.4 . . . no
C9 C11 H11 109.3 . . . no
H9 C11 H10 109.9 . . . no
H9 C11 H11 108.4 . . . no
H10 C11 H11 108.6 . . . no
C9 C12 H12 110.0 . . . no
C9 C12 H13 110.0 . . . no
C9 C12 H14 109.2 . . . no
H12 C12 H13 110.0 . . . no
H12 C12 H14 108.7 . . . no
H13 C12 H14 108.8 . . . no
N1 C13 C14 124.1(2) . . . yes
N1 C13 H15 118.0 . . . no
C14 C13 H15 117.9 . . . no
C13 C14 C15 118.1(2) . . . yes
C13 C14 H16 121.3 . . . no
C15 C14 H16 120.6 . . . no
C14 C15 C16 119.8(2) . . . yes
C14 C15 H17 120.1 . . . no
C16 C15 H17 120.1 . . . no
C15 C16 C17 121.7(2) . . . yes
C15 C16 C24 118.5(2) . . . yes
C17 C16 C24 119.7(2) . . . yes
C16 C17 C18 121.4(2) . . . yes
C16 C17 H18 119.0 . . . no
C18 C17 H18 119.6 . . . no
C17 C18 C19 120.8(2) . . . yes
C17 C18 H19 119.7 . . . no
C19 C18 H19 119.5 . . . no
C18 C19 C20 122.4(2) . . . yes
C18 C19 C23 119.9(2) . . . yes
C20 C19 C23 117.7(2) . . . yes
C19 C20 C21 119.4(2) . . . yes
C19 C20 H20 120.2 . . . no
C21 C20 H20 120.4 . . . no
C20 C21 C22 118.7(3) . . . yes
C20 C21 H21 120.6 . . . no
C22 C21 H21 120.7 . . . no
N2 C22 C21 124.4(3) . . . yes
N2 C22 H22 117.7 . . . no
C21 C22 H22 117.9 . . . no
N2 C23 C19 122.9(2) . . . yes
N2 C23 C24 118.3(2) . . . yes
C19 C23 C24 118.9(2) . . . yes
N1 C24 C16 121.4(2) . . . yes
N1 C24 C23 119.5(2) . . . yes
C16 C24 C23 119.1(2) . . . yes
F1 B1 F2 109.0(2) . . . yes
F1 B1 F3 109.2(2) . . . yes
F1 B1 F4 108.1(2) . . . yes
F2 B1 F3 110.5(2) . . . yes
F2 B1 F4 109.7(2) . . . yes
F3 B1 F4 110.2(2) . . . yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 C1 2.112(2) . . yes
I1 C7 2.032(3) . . yes
F1 B1 1.403(3) . . yes
F2 B1 1.391(3) . . yes
F3 B1 1.381(3) . . yes
F4 B1 1.389(3) . . yes
N1 C13 1.331(3) . . yes
N1 C24 1.365(3) . . yes
N2 C22 1.323(3) . . yes
N2 C23 1.362(3) . . yes
C1 C2 1.379(3) . . yes
C1 C6 1.380(3) . . yes
C2 C3 1.390(3) . . yes
C2 H1 0.951 . . no
C3 C4 1.382(4) . . yes
C3 H2 0.954 . . no
C4 C5 1.381(4) . . yes
C4 H3 0.953 . . no
C5 C6 1.392(3) . . yes
C5 H4 0.954 . . no
C6 H5 0.957 . . no
C7 C8 1.189(3) . . yes
C8 C9 1.475(3) . . yes
C9 C10 1.511(4) . . yes
C9 C11 1.521(4) . . yes
C9 C12 1.500(4) . . yes
C10 H6 0.939 . . no
C10 H7 0.956 . . no
C10 H8 0.954 . . no
C11 H9 0.949 . . no
C11 H10 0.946 . . no
C11 H11 0.964 . . no
C12 H12 0.948 . . no
C12 H13 0.946 . . no
C12 H14 0.961 . . no
C13 C14 1.395(4) . . yes
C13 H15 0.954 . . no
C14 C15 1.372(4) . . yes
C14 H16 0.951 . . no
C15 C16 1.396(4) . . yes
C15 H17 0.955 . . no
C16 C17 1.432(3) . . yes
C16 C24 1.413(3) . . yes
C17 C18 1.342(4) . . yes
C17 H18 0.953 . . no
C18 C19 1.438(4) . . yes
C18 H19 0.949 . . no
C19 C20 1.405(4) . . yes
C19 C23 1.413(3) . . yes
C20 C21 1.367(4) . . yes
C20 H20 0.955 . . no
C21 C22 1.402(4) . . yes
C21 H21 0.956 . . no
C22 H22 0.957 . . no
C23 C24 1.454(4) . . yes
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
I1 N1 2.661(2) . . ?
I1 F1 2.882(1) . . ?
I1 N2 3.263(2) . . ?
I1 C13 3.311(3) . . ?
F1 C7 3.386(3) . . ?
F1 C18 3.437(3) . 3_666 ?
F1 C5 3.470(3) . 4_555 ?
F2 C13 3.208(3) . 1_455 ?
F2 C2 3.339(3) . 1_455 ?
F2 C10 3.599(4) . 3_556 ?
F3 C22 3.318(3) . 4_555 ?
F3 C11 3.482(4) . 3_556 ?
F3 C21 3.560(4) . 4_555 ?
F4 C6 3.201(3) . 4_555 ?
F4 C4 3.302(3) . 4_455 ?
F4 C5 3.391(3) . 4_555 ?
F4 C14 3.418(3) . 1_455 ?
F4 C13 3.438(3) . 1_455 ?
F4 C18 3.530(3) . 3_666 ?
N1 C1 3.362(3) . . ?
N1 C2 3.445(3) . . ?
N1 C18 3.513(3) . 3_666 ?
N2 C1 3.098(3) . . ?
N2 C6 3.253(3) . . ?
N2 C17 3.439(3) . 3_666 ?
C6 C22 3.415(4) . . ?
C13 C18 3.572(4) . 3_766 ?
C14 C18 3.355(4) . 3_766 ?
C14 C20 3.579(4) . 3_666 ?
C14 C19 3.586(4) . 3_766 ?
C15 C19 3.435(4) . 3_766 ?
C15 C18 3.486(4) . 3_766 ?
C15 C21 3.548(4) . 3_666 ?
C15 C20 3.577(4) . 3_666 ?
C16 C16 3.426(5) . 3_766 ?
C16 C23 3.455(3) . 3_666 ?
C16 C17 3.522(3) . 3_766 ?
C16 C19 3.531(3) . 3_666 ?
C17 C24 3.473(4) . 3_766 ?
C17 C23 3.496(3) . 3_666 ?
C18 C24 3.525(3) . 3_666 ?
C19 C24 3.514(3) . 3_666 ?
