#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:19:47 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179917 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/12/7021221.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_7021221
loop_
_publ_author_name
'Barszcz, Barbara'
'Masternak, Joanna'
'Sawka-Dobrowolska, Wanda'
_publ_section_title
;
 Assembling novel Cd(ii) complexes with multidentate nitrogen donor
 ligands obtained in situ from the system: zerovalent copper, cadmium
 oxide, 1-hydroxymethyl-3,5-dimethylpyrazole and ammonium thiocyanate.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5960
_journal_page_last               5963
_journal_paper_doi               10.1039/c3dt32987a
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C6 H10 Cd N4 O S2'
_chemical_formula_weight         330.73
_chemical_name_common
;
catena-Poly-(bis(mu2-hexamathylenetetraamine)-tetra(mu2-
thicyanato)-di(methanol)dicadium(ii))
;
_chemical_name_systematic
;
catena-Poly-(bis(μ2-hexamathylenetetraamine)-
tetra(μ2-thicyanato)-di(methanol)dicadium(II))
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 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                 107.309(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8702(2)
_cell_length_b                   9.2216(3)
_cell_length_c                   13.7007(3)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      0.989
_cell_volume                     1069.93(5)
_computing_cell_refinement
;
CrysAlis RED Oxford Diffraction Ltd., version 1.171.13
;
_computing_data_collection
;
CrysAlis CCD Oxford Diffraction Ltd., version 1.171.13
;
_computing_data_reduction
;
CrysAlis RED Oxford Diffraction Ltd., version 1.171.13
;
_computing_molecular_graphics    'SHELXTL-NT V5.1, Bruker AXS,1999'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'KM4 CCD kappa-geometry diffractometer'
_diffrn_measurement_method       /w
_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  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0183
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13274
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         4.69
_exptl_absorpt_coefficient_mu    2.403
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.665
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   CrysAlis
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.053
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         3021
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.0192
_refine_ls_R_factor_gt           0.0160
_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)+(0.0376P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0437
_refine_ls_wR_factor_ref         0.0446
_reflns_number_gt                2746
_reflns_number_total             3021
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt32987a.txt
_cod_data_source_block           (4)
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               7021221
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
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
Cd2 Cd 0.0000 0.661776(15) 0.2500 0.01219(5) Uani 1 2 d S
Cd1 Cd -0.5000 1.0000 0.0000 0.01053(5) Uani 1 2 d S
S1 S -0.56394(4) 0.74789(4) 0.08055(3) 0.01355(7) Uani 1 1 d .
S2 S 0.07373(4) 0.86953(4) 0.13398(3) 0.01569(8) Uani 1 1 d .
N2 N -0.35565(14) 1.31805(13) 0.27827(8) 0.0120(2) Uani 1 1 d .
N1 N -0.49968(13) 1.13105(13) 0.16046(8) 0.0109(2) Uani 1 1 d .
C1 C -0.35721(16) 1.22507(16) 0.19074(10) 0.0122(3) Uani 1 1 d .
H11 H -0.3564(18) 1.2823(19) 0.1355(12) 0.008(4) Uiso 1 1 d .
H12 H -0.2674(19) 1.1620(16) 0.2100(13) 0.011(4) Uiso 1 1 d .
C2 C -0.5000 1.4079(2) 0.2500 0.0137(4) Uani 1 2 d S
H2 H -0.5007(17) 1.4690(17) 0.1967(11) 0.005(4) Uiso 1 1 d .
C3 C -0.35813(16) 1.22540(16) 0.36481(10) 0.0119(3) Uani 1 1 d .
H31 H -0.2688(19) 1.1671(15) 0.3817(12) 0.009(4) Uiso 1 1 d .
H32 H -0.3569(19) 1.2828(18) 0.4193(12) 0.008(4) Uiso 1 1 d .
C4 C -0.5000 1.0404(2) 0.2500 0.0112(3) Uani 1 2 d S
H4 H -0.598(2) 0.9834(19) 0.2318(13) 0.018(5) Uiso 1 1 d .
N3 N -0.25519(14) 0.63871(14) 0.15228(10) 0.0175(3) Uani 1 1 d .
N4 N -0.23584(14) 0.97654(14) 0.06778(9) 0.0153(2) Uani 1 1 d .
C6 C -0.38199(16) 0.68677(15) 0.12292(10) 0.0131(3) Uani 1 1 d .
C5 C -0.10787(16) 0.93337(15) 0.09539(10) 0.0124(3) Uani 1 1 d .
C7 C -0.0299(2) 0.3741(2) 0.09386(14) 0.0299(4) Uani 1 1 d .
H71 H -0.1350 0.4128 0.0706 0.032(5) Uiso 1 1 calc R
H72 H -0.0301 0.2868 0.1319 0.044(6) Uiso 1 1 calc R
H73 H 0.0065 0.3529 0.0361 0.045(7) Uiso 1 1 calc R
O1 O 0.07210(13) 0.47744(13) 0.15749(9) 0.0213(2) Uani 1 1 d .
H1 H 0.153(3) 0.447(2) 0.1759(15) 0.033(6) Uiso 1 1 d .
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'
S S 0.1246 0.1234 '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'
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
_geom_angle_site_symmetry_3
N3 Cd2 N3 169.25(7) . 2
N3 Cd2 O1 89.87(4) . .
N3 Cd2 O1 82.25(4) 2 .
N3 Cd2 O1 82.25(4) . 2
N3 Cd2 O1 89.87(4) 2 2
O1 Cd2 O1 85.83(7) . 2
N3 Cd2 S2 92.30(4) . 2
N3 Cd2 S2 95.35(3) 2 2
O1 Cd2 S2 177.08(3) . 2
O1 Cd2 S2 92.52(3) 2 2
N3 Cd2 S2 95.35(3) . .
N3 Cd2 S2 92.30(4) 2 .
O1 Cd2 S2 92.52(3) . .
O1 Cd2 S2 177.08(3) 2 .
S2 Cd2 S2 89.227(17) 2 .
N4 Cd1 N4 180.0 . 3_475
N4 Cd1 N1 87.44(4) . .
N4 Cd1 N1 92.56(4) 3_475 .
N4 Cd1 N1 92.56(4) . 3_475
N4 Cd1 N1 87.44(4) 3_475 3_475
N1 Cd1 N1 180.00(5) . 3_475
N4 Cd1 S1 86.12(3) . 3_475
N4 Cd1 S1 93.88(3) 3_475 3_475
N1 Cd1 S1 89.87(3) . 3_475
N1 Cd1 S1 90.13(3) 3_475 3_475
N4 Cd1 S1 93.88(3) . .
N4 Cd1 S1 86.12(3) 3_475 .
N1 Cd1 S1 90.13(3) . .
N1 Cd1 S1 89.87(3) 3_475 .
S1 Cd1 S1 180.0 3_475 .
C6 S1 Cd1 97.80(5) . .
C5 S2 Cd2 93.31(5) . .
C3 N2 C1 108.70(11) . .
C3 N2 C2 108.56(10) . .
C1 N2 C2 108.42(9) . .
C3 N1 C4 108.16(10) 2_455 .
C3 N1 C1 108.41(11) 2_455 .
C4 N1 C1 107.94(9) . .
C3 N1 Cd1 107.37(7) 2_455 .
C4 N1 Cd1 116.95(9) . .
C1 N1 Cd1 107.75(8) . .
N2 C1 N1 111.63(11) . .
N2 C1 H11 109.5(10) . .
N1 C1 H11 108.5(10) . .
N2 C1 H12 108.9(10) . .
N1 C1 H12 106.9(9) . .
H11 C1 H12 111.4(14) . .
N2 C2 N2 111.76(16) . 2_455
N2 C2 H2 110.6(9) . .
N2 C2 H2 109.6(9) 2_455 .
N2 C3 N1 111.63(10) . 2_455
N2 C3 H31 108.8(10) . .
N1 C3 H31 108.7(9) 2_455 .
N2 C3 H32 108.9(10) . .
N1 C3 H32 109.5(10) 2_455 .
H31 C3 H32 109.3(14) . .
N1 C4 N1 111.52(16) 2_455 .
N1 C4 H4 106.9(11) 2_455 .
N1 C4 H4 108.1(10) . .
C6 N3 Cd2 149.25(12) . .
C5 N4 Cd1 164.89(12) . .
N3 C6 S1 177.67(14) . .
N4 C5 S2 179.17(14) . .
O1 C7 H71 109.5 . .
O1 C7 H72 109.5 . .
H71 C7 H72 109.5 . .
O1 C7 H73 109.5 . .
H71 C7 H73 109.5 . .
H72 C7 H73 109.5 . .
C7 O1 Cd2 126.72(10) . .
C7 O1 H1 109.3(17) . .
Cd2 O1 H1 119.1(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd2 N3 2.2712(12) .
Cd2 N3 2.2712(12) 2
Cd2 O1 2.3211(12) .
Cd2 O1 2.3211(12) 2
Cd2 S2 2.6913(4) 2
Cd2 S2 2.6913(4) .
Cd1 N4 2.2594(12) .
Cd1 N4 2.2594(12) 3_475
Cd1 N1 2.5079(11) .
Cd1 N1 2.5079(11) 3_475
Cd1 S1 2.7049(4) 3_475
Cd1 S1 2.7050(4) .
S1 C6 1.6438(14) .
S2 C5 1.6474(14) .
N2 C3 1.4670(18) .
N2 C1 1.4710(17) .
N2 C2 1.4765(16) .
N1 C3 1.4859(17) 2_455
N1 C4 1.4851(16) .
N1 C1 1.4863(17) .
C1 H11 0.924(16) .
C1 H12 0.958(16) .
C2 N2 1.4766(16) 2_455
C2 H2 0.921(15) .
C3 N1 1.4859(17) 2_455
C3 H31 0.928(15) .
C3 H32 0.912(16) .
C4 N1 1.4850(16) 2_455
C4 H4 0.983(17) .
N3 C6 1.1636(18) .
N4 C5 1.1553(18) .
C7 O1 1.4204(19) .
C7 H71 0.9600 .
C7 H72 0.9600 .
C7 H73 0.9600 .
O1 H1 0.74(2) .
