#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/99/2219947.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_2219947
loop_
_publ_author_name
'Zhang, Shi-Shen'
_publ_section_title
Poly[[μ₃-N,N'-bis(3-pyridylmethyl)thiourea-κ³N:N':S]iodidocopper(I)]
_journal_coeditor_code           NG2496
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1395
_journal_paper_doi               10.1107/S1600536808031188
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Cu I (C13 H14 N4 S)]'
_chemical_formula_moiety         'C13 H14 Cu I N4 S'
_chemical_formula_sum            'C13 H14 Cu I N4 S'
_chemical_formula_weight         448.78
_chemical_name_systematic
;
Poly[[μ₃-N,N'-bis(3-pyridylmethyl)thiourea-
κ³N:N':S]iodidocopper(I)]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 102.001(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3610(10)
_cell_length_b                   8.3673(7)
_cell_length_c                   14.2686(11)
_cell_measurement_reflns_used    3234
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      27.74
_cell_measurement_theta_min      2.84
_cell_volume                     1560.3(2)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 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  0.0200
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8191
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.84
_exptl_absorpt_coefficient_mu    3.507
_exptl_absorpt_correction_T_max  0.6783
_exptl_absorpt_correction_T_min  0.5406
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.910
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.281
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2750
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0263
_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)+(0.0275P)²+0.8144P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0592
_refine_ls_wR_factor_ref         0.0615
_reflns_number_gt                2418
_reflns_number_total             2750
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ng2496.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               2219947
_cod_database_fobs_code          2219947
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
C C1 0.4137(2) 0.8305(4) 0.3317(2) 0.0340(7) Uani d . 1
H H1A 0.4469 0.7269 0.3368 0.041 Uiso calc R 1
H H1B 0.4581 0.9036 0.3739 0.041 Uiso calc R 1
C C2 0.4006(2) 0.8893(3) 0.2301(2) 0.0290(6) Uani d . 1
C C3 0.3491(2) 1.0308(3) 0.2012(2) 0.0315(7) Uani d . 1
H H3 0.3220 1.0879 0.2460 0.038 Uiso calc R 1
C C4 0.3768(2) 1.0054(4) 0.0489(2) 0.0361(7) Uani d . 1
H H4 0.3685 1.0441 -0.0134 0.043 Uiso calc R 1
C C5 0.4292(2) 0.8663(4) 0.0718(2) 0.0402(7) Uani d . 1
H H5 0.4565 0.8122 0.0260 0.048 Uiso calc R 1
C C6 0.4415(2) 0.8065(4) 0.1630(2) 0.0376(7) Uani d . 1
H H6 0.4770 0.7115 0.1795 0.045 Uiso calc R 1
C C7 -0.0360(2) 0.7596(4) 0.4500(2) 0.0379(7) Uani d . 1
H H7 -0.0490 0.7921 0.3863 0.045 Uiso calc R 1
C C8 0.0621(2) 0.7151(4) 0.4916(2) 0.0372(7) Uani d . 1
C C9 0.0813(3) 0.6670(5) 0.5858(3) 0.0521(9) Uani d . 1
H H9 0.1469 0.6365 0.6166 0.063 Uiso calc R 1
C C10 0.0020(3) 0.6648(5) 0.6337(3) 0.0571(10) Uani d . 1
H H10 0.0130 0.6307 0.6970 0.068 Uiso calc R 1
C C11 -0.0934(3) 0.7134(4) 0.5874(2) 0.0445(8) Uani d . 1
H H11 -0.1460 0.7147 0.6210 0.053 Uiso calc R 1
C C12 0.1456(2) 0.7225(4) 0.4347(3) 0.0413(8) Uani d . 1
H H12A 0.1909 0.6314 0.4502 0.050 Uiso calc R 1
H H12B 0.1157 0.7194 0.3667 0.050 Uiso calc R 1
C C13 0.2875(2) 0.9112(3) 0.4274(2) 0.0309(6) Uani d . 1
Cu Cu1 0.26574(3) 1.19634(5) 0.57370(3) 0.04022(12) Uani d . 1
N N1 0.20322(18) 0.8710(3) 0.45837(19) 0.0397(6) Uani d . 1
H H1 0.1810 0.9377 0.4952 0.048 Uiso calc R 1
N N2 0.31731(18) 0.8164(3) 0.36364(17) 0.0317(6) Uani d . 1
H H2 0.2765 0.7407 0.3393 0.038 Uiso calc R 1
N N3 0.33636(18) 1.0893(3) 0.11266(18) 0.0328(6) Uani d . 1
N N4 -0.11373(19) 0.7591(3) 0.4956(2) 0.0396(6) Uani d . 1
S S3 0.35264(6) 1.07993(10) 0.46956(6) 0.0397(2) Uani d . 1
I I1 0.24731(2) 1.03780(3) 0.728706(18) 0.05208(10) Uani d . 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'
O O 0.0106 0.0060 '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
N2 C1 C2 . . 113.3(2)
N2 C1 H1A . . 108.9
C2 C1 H1A . . 108.9
N2 C1 H1B . . 108.9
C2 C1 H1B . . 108.9
H1A C1 H1B . . 107.7
C6 C2 C3 . . 117.6(3)
C6 C2 C1 . . 121.3(3)
C3 C2 C1 . . 121.1(2)
N3 C3 C2 . . 123.6(3)
N3 C3 H3 . . 118.2
C2 C3 H3 . . 118.2
N3 C4 C5 . . 122.7(3)
N3 C4 H4 . . 118.6
C5 C4 H4 . . 118.6
C4 C5 C6 . . 119.6(3)
C4 C5 H5 . . 120.2
C6 C5 H5 . . 120.2
C5 C6 C2 . . 119.1(3)
C5 C6 H6 . . 120.4
C2 C6 H6 . . 120.4
N4 C7 C8 . . 123.9(3)
N4 C7 H7 . . 118.0
C8 C7 H7 . . 118.0
C7 C8 C9 . . 118.0(3)
C7 C8 C12 . . 120.1(3)
C9 C8 C12 . . 121.9(3)
C8 C9 C10 . . 118.8(3)
C8 C9 H9 . . 120.6
C10 C9 H9 . . 120.6
C11 C10 C9 . . 119.5(3)
C11 C10 H10 . . 120.3
C9 C10 H10 . . 120.3
N4 C11 C10 . . 122.4(3)
N4 C11 H11 . . 118.8
C10 C11 H11 . . 118.8
N1 C12 C8 . . 108.8(2)
N1 C12 H12A . . 109.9
C8 C12 H12A . . 109.9
N1 C12 H12B . . 109.9
C8 C12 H12B . . 109.9
H12A C12 H12B . . 108.3
N2 C13 N1 . . 118.0(3)
N2 C13 S3 . . 122.2(2)
N1 C13 S3 . . 119.8(2)
N3 Cu1 N4 4_586 3_576 108.54(10)
N3 Cu1 S3 4_586 . 106.38(7)
N4 Cu1 S3 3_576 . 110.01(8)
N3 Cu1 I1 4_586 . 109.34(7)
N4 Cu1 I1 3_576 . 103.57(7)
S3 Cu1 I1 . . 118.69(3)
C13 N1 C12 . . 125.3(2)
C13 N1 H1 . . 117.4
C12 N1 H1 . . 117.4
C13 N2 C1 . . 125.2(3)
C13 N2 H2 . . 117.4
C1 N2 H2 . . 117.4
C3 N3 C4 . . 117.3(3)
C3 N3 Cu1 . 4_585 122.7(2)
C4 N3 Cu1 . 4_585 119.9(2)
C7 N4 C11 . . 117.2(3)
C7 N4 Cu1 . 3_576 123.0(2)
C11 N4 Cu1 . 3_576 119.4(2)
C13 S3 Cu1 . . 106.95(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C1 N2 . 1.457(4)
C1 C2 . 1.506(4)
C1 H1A . 0.9700
C1 H1B . 0.9700
C2 C6 . 1.384(4)
C2 C3 . 1.388(4)
C3 N3 . 1.332(4)
C3 H3 . 0.9300
C4 N3 . 1.348(4)
C4 C5 . 1.363(4)
C4 H4 . 0.9300
C5 C6 . 1.371(5)
C5 H5 . 0.9300
C6 H6 . 0.9300
C7 N4 . 1.335(4)
C7 C8 . 1.372(4)
C7 H7 . 0.9300
C8 C9 . 1.374(5)
C8 C12 . 1.512(4)
C9 C10 . 1.376(5)
C9 H9 . 0.9300
C10 C11 . 1.370(5)
C10 H10 . 0.9300
C11 N4 . 1.337(4)
C11 H11 . 0.9300
C12 N1 . 1.464(4)
C12 H12A . 0.9700
C12 H12B . 0.9700
C13 N2 . 1.330(4)
C13 N1 . 1.335(4)
C13 S3 . 1.701(3)
Cu1 N3 4_586 2.049(2)
Cu1 N4 3_576 2.099(3)
Cu1 S3 . 2.2852(8)
Cu1 I1 . 2.6341(5)
N1 H1 . 0.8600
N2 H2 . 0.8600
N3 Cu1 4_585 2.049(2)
N4 Cu1 3_576 2.099(3)
