#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:34:46 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179336 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/33/4323300.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_4323300
loop_
_publ_author_name
'Volkmar Stenzel'
'Jörg Jeske'
'Wolf-Walther du Mont'
'Peter G. Jones'
_publ_contact_author
;
      Jones, Peter G.
      Institut für Analytische und Anorganische Chemie
      Technische Universität Braunschweig
      Postfach 3329
      38023 Braunschweig
      Germany
;
_publ_contact_author_email       P.Jones@tu-bs.de
_publ_contact_author_fax         '049 531 391-5387'
_publ_contact_author_phone       '049 531 391-5382'
_publ_section_title
;
 Supramolecular Soft-Soft Interactions of
 Diiodo(tert-butyl)(isopropyl)phosphonium Cations with μ₂- to
 μ₅-Bridging Iodide Anions. Formation of Chains, Helices, and Columnar
 Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              443
_journal_page_last               448
_journal_paper_doi               10.1021/ic9603058
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C7 H16 I3.25 P'
_chemical_formula_weight         543.59
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           130
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2ac'
_symmetry_space_group_name_H-M   'P 4/n c c :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   19.730(3)
_cell_length_b                   19.730(3)
_cell_length_c                   14.485(4)
_cell_measurement_reflns_used    52
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      11.5
_cell_measurement_theta_min      10
_cell_volume                     5639(2)
_computing_cell_refinement       DIF4
_computing_data_collection       DIF4
_computing_data_reduction        REDU4
_computing_molecular_graphics    'SIEMENS XP'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_measurement_device       'STOE STADI-4'
_diffrn_measurement_method       Omega-Scans
_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  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0352
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4788
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         3.17
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.271
_exptl_absorpt_correction_T_max  0.547
_exptl_absorpt_correction_T_min  0.447
_exptl_absorpt_correction_type   Psi-Scans
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    2.561
_exptl_crystal_description       prism
_exptl_crystal_F_000             3924
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.35
_refine_diff_density_max         3.012
_refine_diff_density_min         -2.283
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.095
_refine_ls_goodness_of_fit_obs   1.130
_refine_ls_hydrogen_treatment    'rigid methyls, other riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         2493
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_restrained_S_obs      1.130
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_obs          0.0356
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0242P)²+41.9659P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0800
_refine_ls_wR_factor_obs         0.0747
_reflns_number_observed          2068
_reflns_number_total             2494
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9603058_3.cif
_cod_data_source_block           oioioi
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to the
built-in table from CIF Core dictionary named 'cif_core.dic' version
2.4.1 from 2010-06-29 (11 times).

'_geom_angle_publ_flag' value 'Y'
changed to 'y' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (21
time).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0242P)^2^+41.9659P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0242P)^2^+41.9659P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5638.6(20)
_cod_original_sg_symbol_H-M      P4/ncc
_cod_database_code               4323300
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y, -x, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'
'-y-1/2, -x-1/2, z-1/2'
'y, x, z-1/2'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
I1 0.0249(3) 0.0240(3) 0.0297(3) 0.0004(2) -0.0084(2) 0.0013(2)
I2 0.0293(3) 0.0222(3) 0.0245(3) 0.0036(2) -0.0051(2) -0.0030(2)
I3 0.0274(3) 0.0274(3) 0.0252(4) 0.0071(2) 0.0071(2) 0.0023(3)
I4 0.0277(3) 0.0277(3) 0.0302(6) 0.000 0.000 0.0026(5)
I5 0.0344(9) 0.0344(9) 0.093(3) 0.000 0.000 0.000
I6 0.0451(12) 0.0451(12) 0.097(3) 0.000 0.000 0.000
I7 0.025(3) 0.025(3) 0.245(8) 0.000 0.000 0.000
I8 0.018(3) 0.018(3) 0.723(33) 0.000 0.000 0.000
P 0.0220(10) 0.0195(10) 0.0201(10) 0.0013(8) -0.0042(8) 0.0000(8)
C1 0.027(4) 0.017(4) 0.020(4) 0.000(3) -0.007(3) -0.002(3)
C2 0.030(5) 0.040(5) 0.036(5) -0.002(4) -0.008(4) -0.006(4)
C3 0.042(6) 0.033(5) 0.046(6) -0.011(5) 0.011(5) 0.002(4)
C4 0.055(6) 0.022(5) 0.033(5) 0.002(4) -0.008(5) -0.001(4)
C5 0.029(5) 0.043(5) 0.013(4) 0.003(4) -0.006(3) 0.004(4)
C6 0.056(6) 0.040(6) 0.028(5) -0.007(4) -0.001(5) 0.019(5)
C7 0.065(8) 0.060(7) 0.041(6) 0.010(5) 0.021(6) -0.008(6)
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
I1 I 0.61690(3) 0.23508(3) 0.58376(4) 0.02619(15) Uani 1 d . .
I2 I 0.52541(3) 0.33560(3) 0.38085(4) 0.02534(15) Uani 1 d . .
I3 I 0.52656(3) 0.47344(3) 0.2500 0.0267(2) Uani 1 d S .
I4 I 0.7500 0.2500 0.7500 0.0285(3) Uani 1 d S .
I5 I 0.2500 0.2500 0.7467(3) 0.0541(8) Uani 0.50 d SP .
I6 I 0.2500 0.2500 0.3323(3) 0.0623(9) Uani 0.50 d SP .
I7 I 0.2500 0.2500 0.5141(9) 0.098(3) Uani 0.50 d SP .
I8 I 0.2500 0.2500 1.0322(17) 0.253(11) Uani 0.50 d SP .
P P 0.51673(10) 0.24126(10) 0.48835(14) 0.0205(4) Uani 1 d . .
C1 C 0.5044(4) 0.1619(4) 0.4210(5) 0.021(2) Uani 1 d . .
C2 C 0.4339(4) 0.1664(5) 0.3755(6) 0.035(2) Uani 1 d . .
H2A H 0.4309(11) 0.2080(15) 0.3389(31) 0.042 Uiso 1 calc R .
H2B H 0.3989(5) 0.1668(29) 0.4235(7) 0.042 Uiso 1 calc R .
H2C H 0.4271(12) 0.1271(15) 0.3352(30) 0.042 Uiso 1 calc R .
C3 C 0.5601(5) 0.1581(5) 0.3458(7) 0.040(2) Uani 1 d . .
H3A H 0.5572(19) 0.1981(15) 0.3059(25) 0.048 Uiso 1 calc R .
H3B H 0.5536(18) 0.1171(16) 0.3086(26) 0.048 Uiso 1 calc R .
H3C H 0.6048(5) 0.1566(30) 0.3753(7) 0.048 Uiso 1 calc R .
C4 C 0.5088(5) 0.0998(4) 0.4823(6) 0.037(2) Uani 1 d . .
H4A H 0.5529(12) 0.0990(16) 0.5134(30) 0.044 Uiso 1 calc R .
H4B H 0.5038(29) 0.0589(4) 0.4446(8) 0.044 Uiso 1 calc R .
H4C H 0.4726(18) 0.1013(15) 0.5286(25) 0.044 Uiso 1 calc R .
C5 C 0.4452(4) 0.2617(4) 0.5649(5) 0.028(2) Uani 1 d . .
H5 H 0.4037(4) 0.2660(4) 0.5257(5) 0.034 Uiso 1 calc R .
C6 C 0.4581(5) 0.3308(5) 0.6107(6) 0.041(2) Uani 1 d . .
H6A H 0.4650(30) 0.3653(7) 0.5629(6) 0.049 Uiso 1 calc R .
H6B H 0.4986(18) 0.3280(9) 0.6498(32) 0.049 Uiso 1 calc R .
H6C H 0.4189(13) 0.3432(14) 0.6487(32) 0.049 Uiso 1 calc R .
C7 C 0.4317(6) 0.2079(6) 0.6366(7) 0.055(3) Uani 1 d . .
H7A H 0.4735(10) 0.1982(25) 0.6706(32) 0.066 Uiso 1 calc R .
H7B H 0.4158(33) 0.1665(12) 0.6061(8) 0.066 Uiso 1 calc R .
H7C H 0.3969(25) 0.2240(15) 0.6796(28) 0.066 Uiso 1 calc R .
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'
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
P I1 I4 169.28(5) . . y
P I2 I3 173.79(5) . . y
I2 I3 I2 109.77(3) 8_665 . y
I1 I4 I1 125.07(2) 8_666 . y
I1 I4 I1 95.32(3) . 2_655 y
I1 I4 I1 109.43(2) . 7_546 y
C5 P C1 113.6(4) . . y
C5 P I1 107.1(3) . . y
C1 P I1 111.4(3) . . y
C5 P I2 105.8(3) . . y
C1 P I2 108.5(3) . . y
I1 P I2 110.33(8) . . y
C4 C1 C2 110.4(7) . . y
C4 C1 C3 109.3(7) . . y
C2 C1 C3 110.0(7) . . y
C4 C1 P 111.4(6) . . y
C2 C1 P 107.1(6) . . y
C3 C1 P 108.5(6) . . y
C7 C5 C6 110.8(7) . . y
C7 C5 P 113.4(7) . . y
C6 C5 P 109.1(6) . . y
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
I1 P 2.415(2) . y
I1 I4 3.5751(7) . y
I2 P 2.433(2) . y
I2 I3 3.3149(8) . y
P C5 1.839(8) . y
P C1 1.861(8) . y
C1 C4 1.516(11) . y
C1 C2 1.541(11) . y
C1 C3 1.550(12) . y
C5 C7 1.509(12) . y
C5 C6 1.538(12) . y
