#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:33:56 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179335 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/32/4323298.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_4323298
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 P'
_chemical_formula_weight         511.87
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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            8
_cell_length_a                   13.413(3)
_cell_length_b                   14.693(3)
_cell_length_c                   14.240(3)
_cell_measurement_reflns_used    70
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      11.5
_cell_measurement_theta_min      10
_cell_volume                     2806.4(10)
_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  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            2807
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         3.04
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.753
_exptl_absorpt_correction_T_max  0.630
_exptl_absorpt_correction_T_min  0.142
_exptl_absorpt_correction_type   Psi-Scans
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.423
_exptl_crystal_description       'cut tablet'
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.608
_refine_diff_density_min         -1.909
_refine_diff_density_rms         0.266
_refine_ls_extinction_coef       0.00056(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.072
_refine_ls_goodness_of_fit_obs   1.112
_refine_ls_hydrogen_treatment    'rigid methyls, other riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         2339
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.127
_refine_ls_restrained_S_obs      1.102
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_obs          0.0646
_refine_ls_shift/esd_max         -0.034
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0886P)²+78.6520P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2005
_refine_ls_wR_factor_obs         0.1798
_reflns_number_observed          1969
_reflns_number_total             2349
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9603058_1.cif
_cod_data_source_block           blast
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0886P)^2^+78.6520P] 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^)+(0.0886P)^2^+78.6520P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      Pbcn
_cod_database_code               4323298
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'
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 0.0376(6) 0.0350(6) 0.0313(5) -0.0009(4) 0.0094(3) -0.0007(4)
I2 0.0371(6) 0.0441(7) 0.0412(6) 0.0067(4) -0.0013(4) 0.0055(4)
I3 0.0540(9) 0.0605(10) 0.0410(8) 0.000 -0.0246(6) 0.000
I4 0.0456(8) 0.0412(8) 0.0400(7) 0.000 0.0195(6) 0.000
P 0.029(2) 0.032(2) 0.0282(15) 0.0021(14) 0.0017(13) -0.0022(15)
C1 0.089(13) 0.050(11) 0.066(11) -0.009(8) -0.032(9) -0.044(9)
C2 0.209(29) 0.143(23) 0.113(19) -0.092(19) 0.108(20) -0.126(20)
C3 0.084(15) 0.149(23) 0.062(12) -0.025(13) 0.023(10) -0.059(16)
C4 0.028(7) 0.054(9) 0.035(7) 0.007(6) 0.009(5) 0.000(6)
C5 0.052(8) 0.028(7) 0.036(7) 0.001(6) 0.004(6) -0.001(6)
C6 0.056(9) 0.044(9) 0.047(8) 0.004(6) 0.013(7) -0.013(7)
C7 0.048(9) 0.067(11) 0.042(8) 0.000(7) 0.003(6) 0.024(8)
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 0.16041(7) 0.14449(7) 0.10859(6) 0.0346(3) Uani 1 d . .
I2 I 0.15685(7) 0.31270(7) -0.10780(7) 0.0408(4) Uani 1 d . .
I3 I 0.0000 0.42924(12) -0.2500 0.0519(5) Uani 1 d S .
I4 I 0.0000 0.03570(10) 0.2500 0.0423(4) Uani 1 d S .
P P 0.2641(3) 0.2267(2) -0.0036(2) 0.0297(7) Uani 1 d . .
C1 C 0.3415(15) 0.3065(13) 0.0678(14) 0.068(5) Uani 1 d U .
H1 H 0.3863(15) 0.2717(13) 0.1109(14) 0.082 Uiso 1 calc R .
C2 C 0.2711(26) 0.3679(21) 0.1246(19) 0.155(15) Uani 1 d U .
H2A H 0.2184(117) 0.3308(33) 0.1529(152) 0.186 Uiso 1 calc R .
H2B H 0.2412(147) 0.4134(115) 0.0829(38) 0.186 Uiso 1 calc R .
H2C H 0.3088(48) 0.3987(136) 0.1742(115) 0.186 Uiso 1 calc R .
C3 C 0.4013(17) 0.3702(20) 0.0080(15) 0.098(9) Uani 1 d U .
H3A H 0.3658(58) 0.3816(88) -0.0510(51) 0.118 Uiso 1 calc R .
H3B H 0.4664(48) 0.3429(50) -0.0055(93) 0.118 Uiso 1 calc R .
H3C H 0.4109(103) 0.4278(43) 0.0415(50) 0.118 Uiso 1 calc R .
C4 C 0.3321(10) 0.1385(11) -0.0781(10) 0.039(3) Uani 1 d U .
C5 C 0.2550(11) 0.0793(10) -0.1244(10) 0.038(3) Uani 1 d U .
H5A H 0.2087(42) 0.1175(11) -0.1603(54) 0.046 Uiso 1 calc R .
H5B H 0.2180(48) 0.0456(49) -0.0763(10) 0.046 Uiso 1 calc R .
H5C H 0.2879(12) 0.0363(43) -0.1669(50) 0.046 Uiso 1 calc R .
C6 C 0.3950(13) 0.1932(11) -0.1525(11) 0.049(4) Uani 1 d U .
H6A H 0.4515(48) 0.2227(61) -0.1212(17) 0.059 Uiso 1 calc R .
H6B H 0.3528(26) 0.2397(48) -0.1818(55) 0.059 Uiso 1 calc R .
H6C H 0.4197(66) 0.1514(16) -0.2008(42) 0.059 Uiso 1 calc R .
C7 C 0.3980(12) 0.0847(13) -0.0146(10) 0.052(4) Uani 1 d U .
H7A H 0.3594(22) 0.0631(63) 0.0394(40) 0.063 Uiso 1 calc R .
H7B H 0.4529(46) 0.1232(24) 0.0074(60) 0.063 Uiso 1 calc R .
H7C H 0.4251(65) 0.0324(42) -0.0488(25) 0.063 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 174.74(9) . . ?
P I2 I3 177.98(9) . . ?
I2 I3 I2 119.23(6) 3_554 . ?
I1 I4 I1 123.05(5) . 3 ?
C1 P C4 117.6(9) . . ?
C1 P I2 109.6(7) . . ?
C4 P I2 107.3(5) . . ?
C1 P I1 105.8(7) . . ?
C4 P I1 107.5(5) . . ?
I2 P I1 108.74(13) . . ?
C3 C1 C2 105.2(19) . . ?
C3 C1 P 112.4(14) . . ?
C2 C1 P 108.3(16) . . ?
C7 C4 C5 111.6(14) . . ?
C7 C4 C6 111.2(12) . . ?
C5 C4 C6 111.6(12) . . ?
C7 C4 P 107.9(10) . . ?
C5 C4 P 107.9(9) . . ?
C6 C4 P 106.5(11) . . ?
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 2.438(3) . ?
I1 I4 3.3525(12) . ?
I2 P 2.423(3) . ?
I2 I3 3.3850(13) . ?
I3 I2 3.3850(13) 3_554 ?
I4 I1 3.3525(11) 3 ?
P C1 1.868(15) . ?
P C4 1.91(2) . ?
C1 C3 1.50(3) . ?
C1 C2 1.54(4) . ?
C4 C7 1.49(2) . ?
C4 C5 1.50(2) . ?
C4 C6 1.58(2) . ?
