#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:44:41 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179732 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/28/7002864.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_7002864
loop_
_publ_author_name
'Wriedt, Mario'
'Näther, Christian'
_publ_section_title
;
 In situ solid state formation of copper(I) coordination polymers by
 thermal reduction of copper(II) precursor compounds: structure and
 reactivity of [Cu(NCS)2(pyrimidine)2]n
;
_journal_issue                   46
_journal_name_full               'Dalton Transactions'
_journal_page_first              10192
_journal_page_last               10198
_journal_paper_doi               10.1039/b909838k
_journal_year                    2009
_chemical_formula_moiety         'C10 H8 Cu N6 S2'
_chemical_formula_sum            'C10 H8 Cu N6 S2'
_chemical_formula_weight         339.88
_chemical_name_systematic
;
catena[bis(mu2-thiocyanato-N,S)
-bis(pyrimidine-N)-copper(II)]
;
_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                97.879(9)
_cell_angle_beta                 97.745(9)
_cell_angle_gamma                115.761(8)
_cell_formula_units_Z            4
_cell_length_a                   9.3335(7)
_cell_length_b                   9.3730(7)
_cell_length_c                   17.1942(13)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      7.5
_cell_volume                     1309.7(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'STOE IPDS-1'
_diffrn_measurement_method       'Phi scans'
_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  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10205
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.45
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.980
_exptl_absorpt_correction_T_max  0.849
_exptl_absorpt_correction_T_min  0.798
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Platon
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.0027(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         4967
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0310
_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)+(0.0492P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0781
_reflns_number_gt                4258
_reflns_number_total             4967
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b909838k.txt
_cod_data_source_block           ss109
_cod_original_cell_volume        1309.69(17)
_cod_database_code               7002864
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.05079(5) 0.45896(5) 0.25199(3) 0.01213(10) Uani 1 1 d . . .
Cu2 Cu 0.5000 1.0000 0.5000 0.01318(15) Uani 1 2 d S . .
N1 N -0.0814(4) 0.5838(3) 0.25830(18) 0.0134(5) Uani 1 1 d . . .
N2 N -0.2775(4) 0.6318(4) 0.31804(19) 0.0229(7) Uani 1 1 d . . .
C1 C -0.1776(4) 0.5660(4) 0.3115(2) 0.0159(7) Uani 1 1 d . . .
H1 H -0.1741 0.4997 0.3481 0.019 Uiso 1 1 calc R . .
C2 C -0.2771(4) 0.7265(5) 0.2669(3) 0.0267(9) Uani 1 1 d . . .
H2 H -0.3450 0.7779 0.2697 0.032 Uiso 1 1 calc R . .
C3 C -0.1830(4) 0.7535(4) 0.2100(2) 0.0216(8) Uani 1 1 d . . .
H3 H -0.1854 0.8215 0.1742 0.026 Uiso 1 1 calc R . .
C4 C -0.0855(4) 0.6783(4) 0.2071(2) 0.0177(7) Uani 1 1 d . . .
H4 H -0.0200 0.6935 0.1682 0.021 Uiso 1 1 calc R . .
N11 N 0.1651(4) 0.3148(4) 0.24537(19) 0.0139(5) Uani 1 1 d . . .
N12 N 0.1482(4) 0.0631(4) 0.1832(2) 0.0277(7) Uani 1 1 d . . .
C11 C 0.0887(5) 0.1672(4) 0.1960(2) 0.0197(8) Uani 1 1 d . . .
H11 H -0.0189 0.1341 0.1672 0.024 Uiso 1 1 calc R . .
C12 C 0.2991(5) 0.1110(4) 0.2262(3) 0.0292(9) Uani 1 1 d . . .
H12 H 0.3471 0.0404 0.2191 0.035 Uiso 1 1 calc R . .
C13 C 0.3879(5) 0.2602(5) 0.2806(3) 0.0298(10) Uani 1 1 d . . .
H13 H 0.4932 0.2910 0.3114 0.036 Uiso 1 1 calc R . .
C14 C 0.3160(4) 0.3609(4) 0.2876(2) 0.0208(8) Uani 1 1 d . . .
H14 H 0.3741 0.4648 0.3230 0.025 Uiso 1 1 calc R . .
N51 N 0.1280(4) 0.5236(3) 0.36899(17) 0.0150(6) Uani 1 1 d . . .
C51 C 0.1786(4) 0.5942(4) 0.43560(19) 0.0113(7) Uani 1 1 d . . .
S51 S 0.25074(12) 0.69525(10) 0.52933(5) 0.0184(2) Uani 1 1 d . . .
N61 N -0.0358(4) 0.3883(3) 0.13580(17) 0.0155(6) Uani 1 1 d . . .
C61 C -0.1026(4) 0.3389(4) 0.06841(19) 0.0105(7) Uani 1 1 d . . .
S61 S -0.19753(11) 0.26541(11) -0.02644(5) 0.01605(19) Uani 1 1 d . . .
N22 N 0.9376(4) 0.9910(5) 0.6050(2) 0.0350(9) Uani 1 1 d . . .
N21 N 0.6774(4) 0.9292(3) 0.52845(17) 0.0156(6) Uani 1 1 d . . .
C21 C 0.8171(5) 1.0263(5) 0.5824(2) 0.0241(9) Uani 1 1 d . . .
H21 H 0.8312 1.1301 0.6068 0.029 Uiso 1 1 calc R . .
C22 C 0.9151(5) 0.8444(6) 0.5702(3) 0.0327(10) Uani 1 1 d . . .
H22 H 0.9981 0.8140 0.5847 0.039 Uiso 1 1 calc R . .
C23 C 0.7764(6) 0.7356(5) 0.5142(2) 0.0315(10) Uani 1 1 d . . .
H23 H 0.7621 0.6314 0.4904 0.038 Uiso 1 1 calc R . .
C24 C 0.6591(5) 0.7839(5) 0.4940(2) 0.0242(9) Uani 1 1 d . . .
H24 H 0.5629 0.7122 0.4546 0.029 Uiso 1 1 calc R . .
N41 N 0.4551(4) 0.8928(3) 0.38766(18) 0.0161(6) Uani 1 1 d . . .
C41 C 0.4006(4) 0.8227(4) 0.3212(2) 0.0110(7) Uani 1 1 d . . .
S41 S 0.32315(11) 0.72358(10) 0.22751(5) 0.01407(18) Uani 1 1 d . . .
Cu3 Cu -0.5000 0.0000 0.0000 0.01472(15) Uani 1 2 d S . .
N31 N -0.5876(4) 0.1637(3) 0.02763(17) 0.0156(6) Uani 1 1 d . . .
N32 N -0.5383(5) 0.4262(4) 0.0930(2) 0.0366(9) Uani 1 1 d . . .
C31 C -0.4946(5) 0.3100(5) 0.0762(2) 0.0245(9) Uani 1 1 d . . .
H31 H -0.3873 0.3331 0.1009 0.029 Uiso 1 1 calc R . .
C32 C -0.6913(6) 0.3894(5) 0.0581(3) 0.0339(10) Uani 1 1 d . . .
H32 H -0.7279 0.4688 0.0684 0.041 Uiso 1 1 calc R . .
C33 C -0.7963(5) 0.2430(5) 0.0085(3) 0.0282(9) Uani 1 1 d . . .
H33 H -0.9041 0.2196 -0.0154 0.034 Uiso 1 1 calc R . .
C34 C -0.7405(4) 0.1305(5) -0.0056(2) 0.0202(8) Uani 1 1 d . . .
H34 H -0.8114 0.0270 -0.0395 0.024 Uiso 1 1 calc R . .
N71 N -0.3983(4) 0.0427(4) 0.11185(18) 0.0178(7) Uani 1 1 d . . .
S71 S -0.24872(12) 0.15777(11) 0.27539(5) 0.0186(2) Uani 1 1 d . . .
C71 C -0.3366(4) 0.0912(4) 0.18034(19) 0.0110(7) Uani 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'
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'
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
_geom_angle_publ_flag
N61 Cu1 N51 177.48(14) . . ?
N61 Cu1 N1 88.98(13) . . ?
N51 Cu1 N1 90.16(13) . . ?
N61 Cu1 N11 90.18(13) . . ?
N51 Cu1 N11 90.47(13) . . ?
N1 Cu1 N11 174.86(12) . . ?
N61 Cu1 S41 89.73(9) . . ?
N51 Cu1 S41 92.68(9) . . ?
N1 Cu1 S41 93.19(9) . . ?
N11 Cu1 S41 91.87(9) . . ?
N41 Cu2 N41 180.000(1) . 2_676 ?
N41 Cu2 N21 89.71(12) . 2_676 ?
N41 Cu2 N21 90.29(12) 2_676 2_676 ?
N41 Cu2 N21 90.29(12) . . ?
N41 Cu2 N21 89.71(12) 2_676 . ?
N21 Cu2 N21 180.00(16) 2_676 . ?
C4 N1 C1 116.8(3) . . ?
C4 N1 Cu1 122.4(3) . . ?
C1 N1 Cu1 120.7(2) . . ?
C1 N2 C2 115.2(3) . . ?
N2 C1 N1 126.5(3) . . ?
N2 C2 C3 123.1(3) . . ?
C4 C3 C2 117.5(3) . . ?
N1 C4 C3 121.0(3) . . ?
C11 N11 C14 117.0(3) . . ?
C11 N11 Cu1 119.6(2) . . ?
C14 N11 Cu1 123.4(2) . . ?
C11 N12 C12 115.6(3) . . ?
N12 C11 N11 126.6(3) . . ?
N12 C12 C13 122.6(3) . . ?
C14 C13 C12 117.0(3) . . ?
N11 C14 C13 121.2(3) . . ?
C51 N51 Cu1 165.3(3) . . ?
N51 C51 S51 179.5(3) . . ?
C61 N61 Cu1 173.2(3) . . ?
N61 C61 S61 178.8(3) . . ?
C21 N22 C22 115.9(4) . . ?
C24 N21 C21 116.5(3) . . ?
C24 N21 Cu2 121.6(2) . . ?
C21 N21 Cu2 121.9(2) . . ?
N22 C21 N21 126.2(4) . . ?
N22 C22 C23 122.5(4) . . ?
C22 C23 C24 117.3(4) . . ?
N21 C24 C23 121.5(4) . . ?
C41 N41 Cu2 168.1(3) . . ?
N41 C41 S41 179.8(4) . . ?
C41 S41 Cu1 98.17(12) . . ?
N71 Cu3 N71 180.0(2) 2_455 . ?
N71 Cu3 N31 90.28(12) 2_455 2_455 ?
N71 Cu3 N31 89.72(12) . 2_455 ?
N71 Cu3 N31 89.72(12) 2_455 . ?
N71 Cu3 N31 90.28(12) . . ?
N31 Cu3 N31 180.00(12) 2_455 . ?
C31 N31 C34 116.6(3) . . ?
C31 N31 Cu3 122.3(3) . . ?
C34 N31 Cu3 121.0(2) . . ?
C31 N32 C32 115.7(4) . . ?
N32 C31 N31 126.1(4) . . ?
N32 C32 C33 122.7(4) . . ?
C32 C33 C34 117.5(4) . . ?
N31 C34 C33 121.3(4) . . ?
C71 N71 Cu3 169.6(3) . . ?
N71 C71 S71 179.1(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N61 1.954(3) . ?
Cu1 N51 1.957(3) . ?
Cu1 N1 2.040(2) . ?
Cu1 N11 2.054(2) . ?
Cu1 S41 2.8081(10) . ?
Cu2 N41 1.949(3) . ?
Cu2 N41 1.949(3) 2_676 ?
Cu2 N21 2.060(3) 2_676 ?
Cu2 N21 2.060(3) . ?
N1 C4 1.339(4) . ?
N1 C1 1.343(5) . ?
N2 C1 1.331(5) . ?
N2 C2 1.332(5) . ?
C2 C3 1.378(6) . ?
C3 C4 1.374(5) . ?
N11 C11 1.342(4) . ?
N11 C14 1.344(5) . ?
N12 C11 1.325(5) . ?
N12 C12 1.345(5) . ?
C12 C13 1.393(5) . ?
C13 C14 1.377(5) . ?
N51 C51 1.161(4) . ?
C51 S51 1.638(3) . ?
N61 C61 1.163(4) . ?
C61 S61 1.641(3) . ?
N22 C21 1.329(5) . ?
N22 C22 1.335(6) . ?
N21 C24 1.336(5) . ?
N21 C21 1.342(5) . ?
C22 C23 1.374(6) . ?
C23 C24 1.377(6) . ?
N41 C41 1.159(4) . ?
C41 S41 1.635(3) . ?
Cu3 N71 1.930(3) 2_455 ?
Cu3 N71 1.930(3) . ?
Cu3 N31 2.061(3) 2_455 ?
Cu3 N31 2.061(3) . ?
N31 C31 1.337(5) . ?
N31 C34 1.343(5) . ?
N32 C31 1.329(5) . ?
N32 C32 1.342(6) . ?
C32 C33 1.362(6) . ?
C33 C34 1.372(6) . ?
N71 C71 1.170(4) . ?
S71 C71 1.627(3) . ?
