#------------------------------------------------------------------------------
#$Date: 2019-10-03 17:15:21 +0300 (Thu, 03 Oct 2019) $
#$Revision: 219077 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/34/7013414.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_7013414
loop_
_publ_author_name
'Blower, Philip J.'
'Castle, Thomas C.'
'Cowley, Andrew R.'
'Dilworth, Jonathan R.'
'Donnelly, Paul S.'
'Labisbal, Elena'
'Sowrey, Frank E.'
'Teat, Simon J.'
'Went, Michael J.'
_publ_section_title
;
 Structural trends in copper(II) bis(thiosemicarbazone) radiopharmaceuticals
;
_journal_coden_ASTM              DTARAF
_journal_issue                   23
_journal_name_full               'Dalton Transactions'
_journal_page_first              4416
_journal_page_last               4425
_journal_paper_doi               10.1039/b307499d
_journal_year                    2003
_chemical_formula_sum            'C5 H7 Cu N6 S2'
_chemical_formula_weight         278.83
_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                 102.193(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.5081(4)
_cell_length_b                   15.4057(10)
_cell_length_c                   11.6504(8)
_cell_measurement_reflns_used    5258
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      58.26
_cell_measurement_theta_min      5.14
_cell_volume                     966.31(12)
_computing_cell_refinement       'Bruker AXS SAINT v6.02a'
_computing_data_collection       'Bruker AXS SMART'
_computing_data_reduction        'Bruker AXS SAINT'
_computing_molecular_graphics    'Bruker AXS SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Bruker AXS SHELXTL'
_computing_structure_solution    'Bruker AXS SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  'Bruker AXS SMART CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'Daresbury SRS Station 9.8'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6904
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6518
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.22
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        10
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.659
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.917
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2587
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0388
_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)+(0.0512P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0941
_reflns_number_gt                2165
_reflns_number_total             2587
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b307499d.txt
_cod_data_source_block           kent2
_cod_depositor_comments
;
 Updated bibliographic information.

 Antanas Vaitkus,
 2019-10-04
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7013414
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_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
Cu Cu 0.28036(6) 0.60065(2) 0.72461(3) 0.02289(12) Uani 1 1 d . . .
S1 S 0.03218(14) 0.67719(5) 0.58420(7) 0.03105(18) Uani 1 1 d . . .
S2 S 0.59613(14) 0.68448(4) 0.81518(7) 0.03163(18) Uani 1 1 d . . .
C1 C -0.0750(12) 0.3590(4) 0.7223(5) 0.0253(14) Uani 0.459(6) 1 d P . .
H1A H -0.2290 0.3754 0.7463 0.038 Uiso 0.459(6) 1 calc PR . .
H1B H 0.0056 0.3116 0.7723 0.038 Uiso 0.459(6) 1 calc PR . .
H1C H -0.1135 0.3400 0.6402 0.038 Uiso 0.459(6) 1 calc PR . .
C2 C 0.4491(11) 0.3529(3) 0.8737(5) 0.0310(14) Uani 0.541(6) 1 d P . .
H2A H 0.6037 0.3397 0.8484 0.047 Uiso 0.541(6) 1 calc PR . .
H2B H 0.3321 0.3047 0.8525 0.047 Uiso 0.541(6) 1 calc PR . .
H2C H 0.4845 0.3612 0.9590 0.047 Uiso 0.541(6) 1 calc PR . .
N11 N 0.0327(4) 0.50779(14) 0.68093(19) 0.0211(4) Uani 1 1 d . . .
C11 C 0.0935(5) 0.43470(17) 0.7347(2) 0.0233(5) Uani 1 1 d . . .
C12 C -0.2004(5) 0.59771(17) 0.5546(2) 0.0235(5) Uani 1 1 d . . .
N12 N -0.1878(4) 0.51868(14) 0.60279(19) 0.0226(4) Uani 1 1 d . . .
N13 N -0.4079(5) 0.61763(15) 0.4758(2) 0.0285(5) Uani 1 1 d . . .
H13A H -0.5284 0.5793 0.4579 0.034 Uiso 1 1 calc R . .
H13B H -0.4235 0.6690 0.4421 0.034 Uiso 1 1 calc R . .
C21 C 0.3384(5) 0.43356(17) 0.8148(2) 0.0236(5) Uani 1 1 d . . .
N21 N 0.4574(4) 0.50686(14) 0.82186(19) 0.0216(4) Uani 1 1 d . . .
N22 N 0.6888(4) 0.51643(14) 0.8922(2) 0.0239(5) Uani 1 1 d . . .
C22 C 0.7669(5) 0.59797(17) 0.8905(3) 0.0264(6) Uani 1 1 d . . .
N23 N 0.9981(5) 0.61607(16) 0.9509(3) 0.0355(6) Uani 1 1 d . . .
H23A H 1.0910 0.5746 0.9895 0.043 Uiso 1 1 calc R . .
H23B H 1.0562 0.6693 0.9518 0.043 Uiso 1 1 calc R . .
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
N21 Cu N11 81.20(9) . . ?
N21 Cu S1 164.46(7) . . ?
N11 Cu S1 84.88(7) . . ?
N21 Cu S2 84.89(7) . . ?
N11 Cu S2 165.11(7) . . ?
S1 Cu S2 109.53(3) . . ?
C12 S1 Cu 94.83(9) . . ?
C22 S2 Cu 94.49(10) . . ?
C11 C1 H1A 109.5 . . ?
C11 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C11 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C21 C2 H2A 109.5 . . ?
C21 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C21 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C11 N11 N12 122.1(2) . . ?
C11 N11 Cu 114.31(18) . . ?
N12 N11 Cu 123.60(16) . . ?
N11 C11 C21 115.2(2) . . ?
N11 C11 C1 123.0(3) . . ?
C21 C11 C1 121.7(3) . . ?
N12 C12 N13 117.2(2) . . ?
N12 C12 S1 125.6(2) . . ?
N13 C12 S1 117.2(2) . . ?
C12 N12 N11 110.6(2) . . ?
C12 N13 H13A 120.0 . . ?
C12 N13 H13B 120.0 . . ?
H13A N13 H13B 120.0 . . ?
N21 C21 C11 114.4(2) . . ?
N21 C21 C2 123.0(3) . . ?
C11 C21 C2 122.4(3) . . ?
C21 N21 N22 121.6(2) . . ?
C21 N21 Cu 114.89(18) . . ?
N22 N21 Cu 123.49(17) . . ?
C22 N22 N21 110.8(2) . . ?
N22 C22 N23 117.4(3) . . ?
N22 C22 S2 125.7(2) . . ?
N23 C22 S2 116.8(2) . . ?
C22 N23 H23A 120.0 . . ?
C22 N23 H23B 120.0 . . ?
H23A N23 H23B 120.0 . . ?
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
Cu N21 1.963(2) . ?
Cu N11 1.968(2) . ?
Cu S1 2.2340(8) . ?
Cu S2 2.2431(8) . ?
S1 C12 1.753(3) . ?
S2 C22 1.756(3) . ?
C1 C11 1.478(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C21 1.486(6) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
N11 C11 1.298(3) . ?
N11 N12 1.365(3) . ?
C11 C21 1.470(4) . ?
C12 N12 1.336(3) . ?
C12 N13 1.341(4) . ?
N13 H13A 0.8800 . ?
N13 H13B 0.8800 . ?
C21 N21 1.299(3) . ?
N21 N22 1.370(3) . ?
N22 C22 1.329(3) . ?
C22 N23 1.348(4) . ?
N23 H23A 0.8800 . ?
N23 H23B 0.8800 . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N21 Cu S1 C12 31.2(3) . . . . ?
N11 Cu S1 C12 4.80(11) . . . . ?
S2 Cu S1 C12 -171.37(9) . . . . ?
N21 Cu S2 C22 5.53(11) . . . . ?
N11 Cu S2 C22 26.5(3) . . . . ?
S1 Cu S2 C22 -168.54(10) . . . . ?
N21 Cu N11 C11 1.7(2) . . . . ?
S1 Cu N11 C11 174.8(2) . . . . ?
S2 Cu N11 C11 -19.4(4) . . . . ?
N21 Cu N11 N12 -179.6(2) . . . . ?
S1 Cu N11 N12 -6.56(18) . . . . ?
S2 Cu N11 N12 159.26(18) . . . . ?
N12 N11 C11 C21 179.3(2) . . . . ?
Cu N11 C11 C21 -2.0(3) . . . . ?
N12 N11 C11 C1 -4.0(5) . . . . ?
Cu N11 C11 C1 174.6(3) . . . . ?
Cu S1 C12 N12 -4.7(2) . . . . ?
Cu S1 C12 N13 176.0(2) . . . . ?
N13 C12 N12 N11 -179.9(2) . . . . ?
S1 C12 N12 N11 0.8(3) . . . . ?
C11 N11 N12 C12 -176.5(2) . . . . ?
Cu N11 N12 C12 5.0(3) . . . . ?
N11 C11 C21 N21 1.2(4) . . . . ?
C1 C11 C21 N21 -175.5(4) . . . . ?
N11 C11 C21 C2 -173.3(3) . . . . ?
C1 C11 C21 C2 10.0(5) . . . . ?
C11 C21 N21 N22 -179.6(2) . . . . ?
C2 C21 N21 N22 -5.1(5) . . . . ?
C11 C21 N21 Cu 0.3(3) . . . . ?
C2 C21 N21 Cu 174.7(3) . . . . ?
N11 Cu N21 C21 -1.0(2) . . . . ?
S1 Cu N21 C21 -27.6(4) . . . . ?
S2 Cu N21 C21 173.6(2) . . . . ?
N11 Cu N21 N22 178.8(2) . . . . ?
S1 Cu N21 N22 152.22(19) . . . . ?
S2 Cu N21 N22 -6.50(19) . . . . ?
C21 N21 N22 C22 -176.3(2) . . . . ?
Cu N21 N22 C22 3.8(3) . . . . ?
N21 N22 C22 N23 -176.5(2) . . . . ?
N21 N22 C22 S2 2.9(3) . . . . ?
Cu S2 C22 N22 -6.5(3) . . . . ?
Cu S2 C22 N23 172.9(2) . . . . ?
