#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/13/2231345.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_2231345
loop_
_publ_author_name
'Zhou, Yuanyuan'
'Wang, Zhaoyang'
'Yang, Guang'
'Ng, Seik Weng'
_publ_section_title
;
 catena-Poly[[diiodidocadmium]-μ-[4,4'-(2,3,5,6-tetramethyl-1,4-phenylene)bis(methylene)]bis(3,5-dimethyl-1H-pyrazole)-κ²N²:N^2'^]
;
_journal_coeditor_code           WM2507
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1037
_journal_paper_doi               10.1107/S1600536811025797
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Cd I2 (C22 H30 N4)]'
_chemical_formula_moiety         'C22 H30 Cd I2 N4'
_chemical_formula_sum            'C22 H30 Cd I2 N4'
_chemical_formula_weight         716.70
_chemical_name_systematic
;
catena-Poly[[diiodidocadmium]-μ-[4,4'-(2,3,5,6-tetramethyl-
1,4-phenylene)bis(methylene)]bis(3,5-dimethyl-1H-pyrazole)-
κ²N²:N^2'^]
;
_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'
_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                 93.407(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.118(8)
_cell_length_b                   6.840(2)
_cell_length_c                   17.057(6)
_cell_measurement_reflns_used    3092
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.5746
_cell_measurement_theta_min      2.1381
_cell_volume                     2575.9(15)
_computing_cell_refinement       'CrystalClear (Rigaku, 2006)'
_computing_data_collection       'CrystalClear (Rigaku, 2006)'
_computing_data_reduction        'CrystalClear (Rigaku, 2006)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku Saturn 724 CCD'
_diffrn_measurement_method       'φ and ω'
_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  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14901
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.39
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.260
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2006)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.848
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.119
_refine_diff_density_min         -0.742
_refine_ls_extinction_coef       0.00092(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         2951
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0555P)²+7.4182P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1273
_refine_ls_wR_factor_ref         0.1344
_reflns_number_gt                2589
_reflns_number_total             2951
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            wm2507.cif
_cod_data_source_block           I
_cod_original_cell_volume        2575.8(16)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2231345
_cod_database_fobs_code          2231345
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_type_symbol
_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_symmetry_multiplicity
I I1 0.53637(2) 0.41499(7) 0.12116(3) 0.0692(2) Uani d . 1 1
Cd Cd1 0.5000 0.60117(8) 0.2500 0.0424(2) Uani d S 1 2
N N1 0.43399(19) 0.8146(7) 0.1908(2) 0.0438(10) Uani d . 1 1
N N2 0.44190(19) 0.8589(6) 0.1144(2) 0.0421(10) Uani d . 1 1
H H2 0.4695 0.8045 0.0863 0.051 Uiso calc R 1 1
C C1 0.3667(4) 0.9231(11) 0.2924(4) 0.071(2) Uani d . 1 1
H H1A 0.3239 0.8970 0.2889 0.106 Uiso calc R 1 1
H H1B 0.3741 1.0464 0.3181 0.106 Uiso calc R 1 1
H H1C 0.3873 0.8213 0.3220 0.106 Uiso calc R 1 1
C C2 0.3894(2) 0.9304(8) 0.2115(3) 0.0433(12) Uani d . 1 1
C C3 0.3678(2) 1.0496(8) 0.1477(3) 0.0409(11) Uani d . 1 1
C C4 0.4023(2) 0.9968(8) 0.0868(3) 0.0421(11) Uani d . 1 1
C C5 0.4040(3) 1.0599(9) 0.0030(3) 0.0554(15) Uani d . 1 1
H H5A 0.3636 1.0599 -0.0210 0.083 Uiso calc R 1 1
H H5B 0.4287 0.9710 -0.0246 0.083 Uiso calc R 1 1
H H5C 0.4206 1.1892 0.0009 0.083 Uiso calc R 1 1
C C6 0.3180(3) 1.1960(10) 0.1503(3) 0.0590(16) Uani d . 1 1
H H6A 0.3353 1.3203 0.1674 0.071 Uiso calc R 1 1
H H6B 0.2905 1.1547 0.1893 0.071 Uiso calc R 1 1
C C7 0.2817(2) 1.2271(8) 0.0728(3) 0.0438(12) Uani d . 1 1
C C8 0.2379(2) 1.0890(7) 0.0473(4) 0.0469(13) Uani d . 1 1
C C9 0.2061(2) 1.1132(8) -0.0256(3) 0.0460(12) Uani d . 1 1
C C10 0.1571(3) 0.9684(10) -0.0503(5) 0.0701(19) Uani d . 1 1
H H10A 0.1639 0.9195 -0.1018 0.105 Uiso calc R 1 1
H H10B 0.1183 1.0318 -0.0512 0.105 Uiso calc R 1 1
H H10C 0.1578 0.8617 -0.0137 0.105 Uiso calc R 1 1
C C11 0.2249(3) 0.9125(9) 0.0990(5) 0.0687(19) Uani d . 1 1
H H11A 0.2565 0.8998 0.1397 0.103 Uiso calc R 1 1
H H11B 0.2232 0.7962 0.0675 0.103 Uiso calc R 1 1
H H11C 0.1868 0.9310 0.1223 0.103 Uiso calc R 1 1
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'
Cd Cd -0.8075 1.2024 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N1 Cd1 N1 6_656 . 99.6(2)
N1 Cd1 I1 6_656 . 116.88(12)
N1 Cd1 I1 . . 98.99(11)
N1 Cd1 I1 6_656 6_656 98.99(11)
N1 Cd1 I1 . 6_656 116.88(12)
I1 Cd1 I1 . 6_656 123.80(4)
C2 N1 N2 . . 105.2(4)
C2 N1 Cd1 . . 137.3(4)
N2 N1 Cd1 . . 117.2(3)
C4 N2 N1 . . 111.9(4)
C4 N2 H2 . . 124.1
N1 N2 H2 . . 124.1
C2 C1 H1A . . 109.5
C2 C1 H1B . . 109.5
H1A C1 H1B . . 109.5
C2 C1 H1C . . 109.5
H1A C1 H1C . . 109.5
H1B C1 H1C . . 109.5
N1 C2 C3 . . 111.1(5)
N1 C2 C1 . . 121.4(5)
C3 C2 C1 . . 127.5(5)
C4 C3 C2 . . 104.6(4)
C4 C3 C6 . . 130.0(5)
C2 C3 C6 . . 125.4(5)
N2 C4 C3 . . 107.2(4)
N2 C4 C5 . . 118.8(5)
C3 C4 C5 . . 133.9(5)
C4 C5 H5A . . 109.5
C4 C5 H5B . . 109.5
H5A C5 H5B . . 109.5
C4 C5 H5C . . 109.5
H5A C5 H5C . . 109.5
H5B C5 H5C . . 109.5
C3 C6 C7 . . 114.9(4)
C3 C6 H6A . . 108.5
C7 C6 H6A . . 108.5
C3 C6 H6B . . 108.5
C7 C6 H6B . . 108.5
H6A C6 H6B . . 107.5
C9 C7 C8 7_575 . 120.3(5)
C9 C7 C6 7_575 . 120.1(5)
C8 C7 C6 . . 119.6(5)
C7 C8 C9 . . 119.7(5)
C7 C8 C11 . . 120.2(5)
C9 C8 C11 . . 120.1(5)
C7 C9 C8 7_575 . 120.0(5)
C7 C9 C10 7_575 . 121.0(5)
C8 C9 C10 . . 119.0(5)
C9 C10 H10A . . 109.5
C9 C10 H10B . . 109.5
H10A C10 H10B . . 109.5
C9 C10 H10C . . 109.5
H10A C10 H10C . . 109.5
H10B C10 H10C . . 109.5
C8 C11 H11A . . 109.5
C8 C11 H11B . . 109.5
H11A C11 H11B . . 109.5
C8 C11 H11C . . 109.5
H11A C11 H11C . . 109.5
H11B C11 H11C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
I1 Cd1 . 2.7034(8)
Cd1 N1 6_656 2.260(4)
Cd1 N1 . 2.260(4)
Cd1 I1 6_656 2.7034(8)
N1 C2 . 1.329(7)
N1 N2 . 1.358(6)
N2 C4 . 1.353(6)
N2 H2 . 0.8800
C1 C2 . 1.497(8)
C1 H1A . 0.9600
C1 H1B . 0.9600
C1 H1C . 0.9600
C2 C3 . 1.420(7)
C3 C4 . 1.375(7)
C3 C6 . 1.491(7)
C4 C5 . 1.494(7)
C5 H5A . 0.9600
C5 H5B . 0.9600
C5 H5C . 0.9600
C6 C7 . 1.520(7)
C6 H6A . 0.9700
C6 H6B . 0.9700
C7 C9 7_575 1.392(8)
C7 C8 . 1.403(8)
C8 C9 . 1.403(8)
C8 C11 . 1.532(8)
C9 C7 7_575 1.392(8)
C9 C10 . 1.509(8)
C10 H10A . 0.9600
C10 H10B . 0.9600
C10 H10C . 0.9600
C11 H11A . 0.9600
C11 H11B . 0.9600
C11 H11C . 0.9600
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
N1 Cd1 N1 C2 6_656 . -76.4(5)
I1 Cd1 N1 C2 . . 164.2(5)
I1 Cd1 N1 C2 6_656 . 28.8(6)
N1 Cd1 N1 N2 6_656 . 96.0(4)
I1 Cd1 N1 N2 . . -23.4(4)
I1 Cd1 N1 N2 6_656 . -158.7(3)
C2 N1 N2 C4 . . -1.4(6)
Cd1 N1 N2 C4 . . -176.1(3)
N2 N1 C2 C3 . . 0.7(6)
Cd1 N1 C2 C3 . . 173.7(4)
N2 N1 C2 C1 . . 179.2(5)
Cd1 N1 C2 C1 . . -7.7(9)
N1 C2 C3 C4 . . 0.3(6)
C1 C2 C3 C4 . . -178.2(6)
N1 C2 C3 C6 . . 179.9(5)
C1 C2 C3 C6 . . 1.4(9)
N1 N2 C4 C3 . . 1.6(6)
N1 N2 C4 C5 . . -178.8(5)
C2 C3 C4 N2 . . -1.1(6)
C6 C3 C4 N2 . . 179.4(6)
C2 C3 C4 C5 . . 179.3(6)
C6 C3 C4 C5 . . -0.2(11)
C4 C3 C6 C7 . . 29.6(9)
C2 C3 C6 C7 . . -149.9(5)
C3 C6 C7 C9 . 7_575 -99.5(7)
C3 C6 C7 C8 . . 77.4(7)
C9 C7 C8 C9 7_575 . -0.5(9)
C6 C7 C8 C9 . . -177.5(5)
C9 C7 C8 C11 7_575 . 179.5(5)
C6 C7 C8 C11 . . 2.6(8)
C7 C8 C9 C7 . 7_575 0.5(9)
C11 C8 C9 C7 . 7_575 -179.5(5)
C7 C8 C9 C10 . . -177.1(5)
C11 C8 C9 C10 . . 2.9(8)
