#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/87/2238742.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_2238742
loop_
_publ_author_name
'Basu Baul, Tushar S.'
'Kundu, Sajal'
'Ng, Seik Weng'
'Tiekink, Edward R. T.'
_publ_section_title
;
 Di-μ-iodido-bis(iodido{methyl
 4-[(pyridin-2-ylmethylidene)amino]benzoate-κ²N,N'}cadmium)
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m623
_journal_page_last               m624
_journal_paper_doi               10.1107/S160053681302905X
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Cd2 I4 (C14 H12 N2 O2)2]'
_chemical_formula_moiety         'C28 H24 Cd2 I4 N4 O4'
_chemical_formula_sum            'C28 H24 Cd2 I4 N4 O4'
_chemical_formula_weight         1212.91
_chemical_name_systematic
;
Di-μ-iodido-bis(iodido{methyl
4-[(pyridin-2-ylmethylidene)amino]benzoate-κ²N,N'}cadmium)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.516(5)
_cell_angle_beta                 95.868(3)
_cell_angle_gamma                90.242(4)
_cell_formula_units_Z            1
_cell_length_a                   8.4883(3)
_cell_length_b                   9.3677(5)
_cell_length_c                   10.9029(5)
_cell_measurement_reflns_used    5933
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4920
_cell_measurement_theta_min      2.3039
_cell_volume                     812.18(7)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2013)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2013)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2013)'
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and
DIAMOND (Brandenburg, 2006)
;
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4041
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Agilent SuperNova Dual diffractometer with an Atlas detector'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_monochromator  Mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11886
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         2.31
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.150
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Agilent, 2013)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.578
_refine_diff_density_min         -1.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         3738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0217
_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)+(0.0210P)²+0.5485P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0470
_refine_ls_wR_factor_ref         0.0495
_reflns_number_gt                3374
_reflns_number_total             3738
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hg5357.cif
_cod_data_source_block           I
_cod_original_cell_volume        812.18(6)
_cod_database_code               2238742
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.36407(2) 0.52109(2) 0.344025(19) 0.01447(6) Uani d . 1 1
I I2 0.54922(2) 0.97175(3) 0.69338(2) 0.01683(6) Uani d . 1 1
Cd Cd 0.39702(2) 0.69721(3) 0.61836(2) 0.01149(6) Uani d . 1 1
N N1 0.2891(3) 0.6752(3) 0.8000(2) 0.0118(5) Uani d . 1 1
N N2 0.1161(3) 0.7293(3) 0.5962(2) 0.0110(5) Uani d . 1 1
O O1 -0.1491(3) 0.9351(3) 0.1141(2) 0.0162(5) Uani d . 1 1
O O2 -0.3079(3) 0.7290(3) 0.0766(2) 0.0206(5) Uani d . 1 1
C C1 0.3737(4) 0.6588(4) 0.9039(3) 0.0153(7) Uani d . 1 1
H H1 0.4858 0.6579 0.9063 0.018 Uiso calc R 1 1
C C2 0.3043(4) 0.6428(4) 1.0096(3) 0.0150(7) Uani d . 1 1
H H2 0.3682 0.6340 1.0833 0.018 Uiso calc R 1 1
C C3 0.1418(4) 0.6401(4) 1.0051(3) 0.0157(7) Uani d . 1 1
H H3 0.0915 0.6254 1.0741 0.019 Uiso calc R 1 1
C C4 0.0520(4) 0.6593(4) 0.8977(3) 0.0139(7) Uani d . 1 1
H H4 -0.0604 0.6582 0.8924 0.017 Uiso calc R 1 1
C C5 0.1304(4) 0.6800(4) 0.7980(3) 0.0123(6) Uani d . 1 1
C C6 0.0422(4) 0.7113(4) 0.6870(3) 0.0119(6) Uani d . 1 1
H H6 -0.0697 0.7181 0.6826 0.014 Uiso calc R 1 1
C C7 0.0294(3) 0.7576(4) 0.4877(3) 0.0107(6) Uani d . 1 1
C C8 -0.1235(4) 0.6954(4) 0.4383(3) 0.0130(6) Uani d . 1 1
H H8 -0.1757 0.6374 0.4800 0.016 Uiso calc R 1 1
C C9 -0.1987(4) 0.7191(4) 0.3279(3) 0.0153(7) Uani d . 1 1
H H9 -0.3021 0.6761 0.2933 0.018 Uiso calc R 1 1
C C10 -0.1227(3) 0.8059(4) 0.2677(3) 0.0103(6) Uani d . 1 1
C C11 0.0284(3) 0.8706(4) 0.3191(3) 0.0115(6) Uani d . 1 1
H H11 0.0785 0.9326 0.2798 0.014 Uiso calc R 1 1
C C12 0.1058(3) 0.8445(4) 0.4279(3) 0.0114(6) Uani d . 1 1
H H12 0.2101 0.8857 0.4613 0.014 Uiso calc R 1 1
C C13 -0.2045(4) 0.8179(4) 0.1441(3) 0.0135(7) Uani d . 1 1
C C14 -0.2324(4) 0.9537(4) -0.0024(3) 0.0175(7) Uani d . 1 1
H H14A -0.2363 0.8575 -0.0752 0.026 Uiso calc R 1 1
H H14B -0.1767 1.0318 -0.0248 0.026 Uiso calc R 1 1
H H14C -0.3406 0.9843 0.0144 0.026 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'
O O 0.0106 0.0060 '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_3
_geom_angle
Cd I1 Cd 2_666 92.716(9)
N1 Cd N2 . 70.33(8)
N1 Cd I2 . 107.66(7)
N2 Cd I2 . 109.09(6)
N1 Cd I1 . 134.10(7)
N2 Cd I1 . 87.44(6)
I2 Cd I1 . 117.588(10)
N1 Cd I1 2_666 86.88(6)
N2 Cd I1 2_666 141.81(6)
I2 Cd I1 2_666 106.827(10)
I1 Cd I1 2_666 87.284(9)
C1 N1 C5 . 118.7(3)
C1 N1 Cd . 124.5(2)
C5 N1 Cd . 116.87(19)
C6 N2 C7 . 119.8(3)
C6 N2 Cd . 115.35(19)
C7 N2 Cd . 124.74(18)
C13 O1 C14 . 114.2(2)
N1 C1 C2 . 122.7(3)
N1 C1 H1 . 118.6
C2 C1 H1 . 118.6
C3 C2 C1 . 118.8(3)
C3 C2 H2 . 120.6
C1 C2 H2 . 120.6
C2 C3 C4 . 119.0(3)
C2 C3 H3 . 120.5
C4 C3 H3 . 120.5
C3 C4 C5 . 118.8(3)
C3 C4 H4 . 120.6
C5 C4 H4 . 120.6
N1 C5 C4 . 121.9(3)
N1 C5 C6 . 117.1(3)
C4 C5 C6 . 121.0(3)
N2 C6 C5 . 120.1(3)
N2 C6 H6 . 119.9
C5 C6 H6 . 119.9
C12 C7 C8 . 120.5(3)
C12 C7 N2 . 117.5(3)
C8 C7 N2 . 122.0(3)
C9 C8 C7 . 119.6(3)
C9 C8 H8 . 120.2
C7 C8 H8 . 120.2
C8 C9 C10 . 120.1(3)
C8 C9 H9 . 119.9
C10 C9 H9 . 119.9
C11 C10 C9 . 120.1(3)
C11 C10 C13 . 122.2(3)
C9 C10 C13 . 117.6(3)
C12 C11 C10 . 120.1(3)
C12 C11 H11 . 120.0
C10 C11 H11 . 120.0
C11 C12 C7 . 119.6(3)
C11 C12 H12 . 120.2
C7 C12 H12 . 120.2
O2 C13 O1 . 123.6(3)
O2 C13 C10 . 123.2(3)
O1 C13 C10 . 113.2(3)
O1 C14 H14A . 109.5
O1 C14 H14B . 109.5
H14A C14 H14B . 109.5
O1 C14 H14C . 109.5
H14A C14 H14C . 109.5
H14B C14 H14C . 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 Cd . 2.8765(4) y
I1 Cd 2_666 2.9813(3) y
I2 Cd . 2.7023(4) y
Cd N1 . 2.333(2) y
Cd N2 . 2.402(2) y
Cd I1 2_666 2.9813(3) ?
N1 C1 . 1.332(4) ?
N1 C5 . 1.346(4) ?
N2 C6 . 1.280(4) ?
N2 C7 . 1.430(4) ?
O1 C13 . 1.342(4) ?
O1 C14 . 1.452(4) ?
O2 C13 . 1.207(4) ?
C1 C2 . 1.396(4) ?
C1 H1 . 0.9500 ?
C2 C3 . 1.375(5) ?
C2 H2 . 0.9500 ?
C3 C4 . 1.394(4) ?
C3 H3 . 0.9500 ?
C4 C5 . 1.397(4) ?
C4 H4 . 0.9500 ?
C5 C6 . 1.471(4) ?
C6 H6 . 0.9500 ?
C7 C12 . 1.394(4) ?
C7 C8 . 1.399(4) ?
C8 C9 . 1.388(4) ?
C8 H8 . 0.9500 ?
C9 C10 . 1.396(4) ?
C9 H9 . 0.9500 ?
C10 C11 . 1.395(4) ?
C10 C13 . 1.491(4) ?
C11 C12 . 1.390(4) ?
C11 H11 . 0.9500 ?
C12 H12 . 0.9500 ?
C14 H14A . 0.9800 ?
C14 H14B . 0.9800 ?
C14 H14C . 0.9800 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C1 H1 O2 1_656 0.95 2.34 3.066(4) 133
C14 H14B Cg1 2_576 0.98 2.79 3.416(4) 123
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
Cd I1 Cd N1 2_666 . -83.00(8)
Cd I1 Cd N2 2_666 . -142.16(6)
Cd I1 Cd I2 2_666 . 107.590(12)
Cd I1 Cd I1 2_666 2_666 0.0
N2 Cd N1 C1 . . -175.4(3)
I2 Cd N1 C1 . . -70.8(3)
I1 Cd N1 C1 . . 119.0(2)
I1 Cd N1 C1 2_666 . 35.8(3)
N2 Cd N1 C5 . . 4.5(2)
I2 Cd N1 C5 . . 109.0(2)
I1 Cd N1 C5 . . -61.1(2)
I1 Cd N1 C5 2_666 . -144.3(2)
N1 Cd N2 C6 . . -3.7(2)
I2 Cd N2 C6 . . -106.2(2)
I1 Cd N2 C6 . . 135.4(2)
I1 Cd N2 C6 2_666 . 53.1(3)
N1 Cd N2 C7 . . -180.0(3)
I2 Cd N2 C7 . . 77.5(2)
I1 Cd N2 C7 . . -40.9(2)
I1 Cd N2 C7 2_666 . -123.2(2)
C5 N1 C1 C2 . . 1.5(5)
Cd N1 C1 C2 . . -178.6(2)
N1 C1 C2 C3 . . 1.7(5)
C1 C2 C3 C4 . . -2.5(5)
C2 C3 C4 C5 . . 0.2(5)
C1 N1 C5 C4 . . -3.9(5)
Cd N1 C5 C4 . . 176.3(3)
C1 N1 C5 C6 . . 174.9(3)
Cd N1 C5 C6 . . -5.0(4)
C3 C4 C5 N1 . . 3.0(5)
C3 C4 C5 C6 . . -175.7(3)
C7 N2 C6 C5 . . 179.1(3)
Cd N2 C6 C5 . . 2.6(4)
N1 C5 C6 N2 . . 1.5(5)
C4 C5 C6 N2 . . -179.7(3)
C6 N2 C7 C12 . . 150.0(3)
Cd N2 C7 C12 . . -33.8(4)
C6 N2 C7 C8 . . -32.9(5)
Cd N2 C7 C8 . . 143.3(2)
C12 C7 C8 C9 . . 0.8(5)
N2 C7 C8 C9 . . -176.2(3)
C7 C8 C9 C10 . . -0.7(5)
C8 C9 C10 C11 . . -0.8(5)
C8 C9 C10 C13 . . 175.7(3)
C9 C10 C11 C12 . . 2.2(5)
C13 C10 C11 C12 . . -174.0(3)
C10 C11 C12 C7 . . -2.1(5)
C8 C7 C12 C11 . . 0.6(5)
N2 C7 C12 C11 . . 177.7(3)
C14 O1 C13 O2 . . 4.4(4)
C14 O1 C13 C10 . . -177.0(2)
C11 C10 C13 O2 . . 156.5(3)
C9 C10 C13 O2 . . -19.9(5)
C11 C10 C13 O1 . . -22.1(4)
C9 C10 C13 O1 . . 161.5(3)
