#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:27:35 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180430 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/99/7209977.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_7209977
loop_
_publ_author_name
'Węcławik, Magdalena'
'Gągor, Anna'
'Piecha, Anna'
'Jakubas, Ryszard'
'Medycki, Wojciech'
_publ_section_title
;
 Synthesis, crystal structure and phase transitions of a series of
 imidazolium iodides
;
_journal_issue                   28
_journal_name_full               CrystEngComm
_journal_page_first              5633
_journal_paper_doi               10.1039/c3ce40559a
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C3 H3 I3 N2'
_chemical_formula_weight         447.77
_chemical_name_systematic
;
?
;
_space_group_IT_number           59
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2a'
_symmetry_space_group_name_H-M   'P m m n :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.2366(3)
_cell_length_b                   8.4314(3)
_cell_length_c                   7.2292(3)
_cell_measurement_reflns_used    1414
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.65
_cell_measurement_theta_min      3.73
_cell_volume                     441.09(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            1414
_diffrn_reflns_theta_full        25.65
_diffrn_reflns_theta_max         25.65
_diffrn_reflns_theta_min         3.71
_exptl_absorpt_coefficient_mu    10.549
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55165
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    3.371
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     29
_refine_ls_number_reflns         489
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0230
_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)+(0.0250P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0492
_refine_ls_wR_factor_ref         0.0514
_reflns_number_gt                432
_reflns_number_total             489
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce40559a.txt
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      Pmmn
_cod_database_code               7209977
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z'
'x+1/2, -y, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z'
'-x-1/2, y, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
I1 I 0.2500 0.7500 0.96500(9) 0.0448(2) Uani 1 4 d S
I2 I 0.2500 0.48988(5) 0.34955(6) 0.03800(18) Uani 1 2 d S
N1 N 0.2500 0.3776(6) 0.7494(7) 0.0364(13) Uani 1 2 d SD
H1 H 0.2500 0.477(3) 0.789(11) 0.044 Uiso 1 2 d SD
C2 C 0.2500 0.2500 0.8553(13) 0.040(2) Uani 1 4 d S
H2 H 0.2500 0.2500 0.9840 0.047 Uiso 1 4 calc SR
C3 C 0.2500 0.3295(7) 0.5672(8) 0.0304(13) Uani 1 2 d S
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 0.0743(4) 0.0252(3) 0.0350(4) 0.000 0.000 0.000
I2 0.0474(3) 0.0313(3) 0.0354(3) 0.00629(18) 0.000 0.000
N1 0.049(3) 0.028(3) 0.032(3) -0.003(3) 0.000 0.000
C2 0.052(5) 0.038(6) 0.028(5) 0.000 0.000 0.000
C3 0.035(3) 0.029(3) 0.027(3) 0.000(3) 0.000 0.000
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'
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
C2 N1 C3 108.3(6) .
C2 N1 H1 126(5) .
C3 N1 H1 126(5) .
N1 C2 N1 109.1(8) 2
N1 C2 H2 125.5 2
N1 C2 H2 125.5 .
C3 C3 N1 107.1(3) 2
C3 C3 I2 130.66(16) 2
N1 C3 I2 122.2(4) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I2 C3 2.075(6) .
N1 C2 1.321(7) .
N1 C3 1.378(8) .
N1 H1 0.889(10) .
C2 N1 1.321(7) 2
C2 H2 0.9300 .
C3 C3 1.341(12) 2
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1 I1 0.889(10) 2.627(19) 3.505(5) 170(7)
