#------------------------------------------------------------------------------
#$Date: 2016-02-14 15:26:36 +0100 (dom 14 de feb de 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/01/2200111.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2200111
loop_
_publ_author_name
'Filguieras, Carlos A. L.'
'Horn Jr, Adolfo'
'Skakle, Janet M. S.'
'Wardell, James L.'
_publ_section_title
;
 Tetramethylammonium pentaiodide
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o338
_journal_page_last               o340
_journal_paper_doi               10.1107/S1600536801004536
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          'C4 H12 N 1+, I5 1-'
_chemical_formula_moiety         'C4 H12 N 1+, I5 1-'
_chemical_formula_sum            'C4 H12 I5 N'
_chemical_formula_weight         708.64
_chemical_name_systematic
;
Tetramethylammonium pentaiodide
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.801(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3110(10)
_cell_length_b                   13.5395(11)
_cell_length_c                   8.8727(7)
_cell_measurement_reflns_used    2244
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.421
_cell_measurement_theta_min      2.409
_cell_volume                     1522.5(2)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
;
ATOMS (Dowty, 1999) and ORTEP-3 (Farrugia, 1999)
;
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measurement_device_type  'Bruker SMART 1000 Area CCD'
_diffrn_measurement_method       φ--ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0321
_diffrn_reflns_av_sigmaI/netI    .0303
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4712
_diffrn_reflns_theta_max         30.87
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    10.173
_exptl_absorpt_correction_T_max  .906
_exptl_absorpt_correction_T_min  .742
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1999)'
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    3.092
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          .60
_exptl_crystal_size_mid          .50
_exptl_crystal_size_min          .50
_refine_diff_density_max         1.482
_refine_diff_density_min         -1.473
_refine_ls_extinction_coef       .00143(18)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     48
_refine_ls_number_reflns         2182
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          .0679
_refine_ls_R_factor_gt           .0515
_refine_ls_shift/su_max          .000
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0740P)²+6.1215P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1428
_reflns_number_gt                1622
_reflns_number_total             2182
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bt6024.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C4 H12 N, I5'
_cod_database_code               2200111
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
I1 .0000 .17657(6) .2500 .0682(3) Uani d S 1 . . I
I2 .16060(4) .01915(4) .19877(6) .0605(2) Uani d . 1 . . I
I3 .30588(5) -.12546(5) .18005(8) .0750(3) Uani d . 1 . . I
N1 .0000 .6882(8) .2500 .075(3) Uani d S 1 . . N
C1 .032(2) .6330(18) .135(2) .210(14) Uani d G 1 . . C
H1A -.0277 .5980 .0673 .316 Uiso calc R 1 . . H
H1B .0859 .5868 .1872 .316 Uiso calc R 1 . . H
H1C .0589 .6774 .0718 .316 Uiso calc R 1 . . H
C2 .084(3) .748(3) .333(4) .33(3) Uani d G 1 . . C
H2A .1427 .7387 .2930 .494 Uiso calc R 1 . . H
H2B .1050 .7316 .4436 .494 Uiso calc R 1 . . H
H2C .0626 .8164 .3201 .494 Uiso calc R 1 . . H
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
I1 .0614(5) .0515(4) .1039(7) .000 .0432(4) .000
I2 .0564(3) .0629(4) .0645(4) -.0039(2) .0222(2) -.0007(2)
I3 .0687(4) .0790(5) .0831(5) .0114(3) .0316(3) -.0031(3)
N1 .088(8) .059(6) .091(8) .000 .045(6) .000
C1 .31(3) .20(2) .152(17) .15(2) .12(2) .017(16)
C2 .38(5) .35(5) .33(5) -.26(5) .21(4) -.11(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
I2 I1 I2 . 2 94.79(3)
I3 I2 I1 . . 175.11(2)
C2 N1 C2 2 . 109(3)
C2 N1 C1 2 . 106.9(16)
C2 N1 C1 . . 108.5(16)
C2 N1 C1 2 2 108.5(16)
C2 N1 C1 . 2 106.9(16)
C1 N1 C1 . 2 117(2)
N1 C1 H1A . . 109.5
N1 C1 H1B . . 109.5
H1A C1 H1B . . 109.5
N1 C1 H1C . . 109.5
H1A C1 H1C . . 109.5
H1B C1 H1C . . 109.5
N1 C2 H2A . . 109.5
N1 C2 H2B . . 109.5
H2A C2 H2B . . 109.5
N1 C2 H2C . . 109.5
H2A C2 H2C . . 109.5
H2B C2 H2C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
I1 I2 . 3.1485(8) ?
I1 I2 2 3.1486(8) ?
I2 I3 . 2.7923(8) ?
N1 C2 2 1.40(3) ?
N1 C2 . 1.40(3) ?
N1 C1 . 1.433(17) ?
N1 C1 2 1.433(17) ?
C1 H1A . .9600 ?
C1 H1B . .9600 ?
C1 H1C . .9600 ?
C2 H2A . .9600 ?
C2 H2B . .9600 ?
C2 H2C . .9600 ?
