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#$Date: 2017-01-09 05:10:34 +0200 (Mon, 09 Jan 2017) $
#$Revision: 190094 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/69/7226941.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_7226941
loop_
_publ_author_name
'Świtlicka, A.'
'Czerwińska, K.'
'Machura, B.'
'Penkala, M.'
'Bieńko, A.'
'Bieńko, D.'
'Zierkiewicz, W.'
_publ_section_title
;
 Thiocyanate copper complexes with pyrazole-derived ligands -- synthesis,
 crystal structures, DFT calculations and magnetic properties
;
_journal_issue                   47
_journal_name_full               CrystEngComm
_journal_page_first              9042
_journal_paper_doi               10.1039/C6CE01739H
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C10 H14 Cu N6 O S2'
_chemical_formula_sum            'C10 H14 Cu N6 O S2'
_chemical_formula_weight         361.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2016-07-14 deposited with the CCDC.
2016-10-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 121.342(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.855(2)
_cell_length_b                   5.6220(4)
_cell_length_c                   16.886(2)
_cell_measurement_reflns_used    1245
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.2421
_cell_measurement_theta_min      3.4738
_cell_volume                     1528.8(4)
_computing_cell_refinement       'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_data_collection       'CrysAlis CCD v. 1.163 (UNIL IC & KUMA 2000)'
_computing_data_reduction        'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_molecular_graphics
'Mercury(Macrae, J.Appl.Cryst.41(2008)466-470'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Diffraction Gemini A Ultra'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3669
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.049
_diffrn_reflns_theta_min         3.839
_exptl_absorpt_coefficient_mu    1.705
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35357
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. A51 (1995) 33-38'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       plate
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       0.0078(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         1344
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0417P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0837
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1140
_reflns_number_total             1344
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6ce01739h2.cif
_cod_data_source_block           cu95
_cod_depositor_comments
'Adding full bibliography for 7226941--7226944.cif.'
_cod_database_code               7226941
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cu1 Cu 0.0000 0.5000 0.0000 0.0269(2) Uani 1 2 d S . P
N1 N 0.08667(14) 0.5436(4) 0.13521(16) 0.0301(6) Uani 1 1 d . . .
N2 N 0.09658(14) 0.3936(4) 0.20285(15) 0.0311(6) Uani 1 1 d . . .
H2A H 0.0659 0.2709 0.1933 0.037 Uiso 1 1 calc R U .
C1 C 0.14603(17) 0.7046(5) 0.1784(2) 0.0365(7) Uani 1 1 d . . .
H1 H 0.1550 0.8315 0.1494 0.044 Uiso 1 1 calc R U .
C2 C 0.19312(18) 0.6584(6) 0.2729(2) 0.0381(7) Uani 1 1 d . . .
H2 H 0.2380 0.7460 0.3177 0.046 Uiso 1 1 calc R U .
C3 C 0.16006(18) 0.4588(5) 0.2867(2) 0.0308(7) Uani 1 1 d . . .
C4 C 0.1835(2) 0.3203(6) 0.3720(2) 0.0458(8) Uani 1 1 d . . .
H4A H 0.2330 0.3867 0.4235 0.069 Uiso 1 1 calc R U .
H4B H 0.1935 0.1578 0.3633 0.069 Uiso 1 1 calc R U .
H4C H 0.1392 0.3272 0.3842 0.069 Uiso 1 1 calc R U .
C99 C -0.07261(17) 0.0394(5) 0.03069(19) 0.0238(6) Uani 1 1 d . . .
N99 N -0.04195(14) 0.2173(4) 0.03049(16) 0.0318(6) Uani 1 1 d . . .
S99 S -0.11602(5) -0.20931(13) 0.03227(5) 0.0370(3) Uani 1 1 d . . .
O1 O 0.0000 0.0184(6) 0.2500 0.0617(11) Uani 1 2 d S T P
H1O H -0.0303 -0.1190 0.2013 0.20(3) Uiso 1 1 d 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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N99 Cu1 N99 180.0 . 5_565
N99 Cu1 N1 89.92(9) . 5_565
N99 Cu1 N1 90.08(9) 5_565 5_565
N99 Cu1 N1 90.08(9) . .
N99 Cu1 N1 89.92(9) 5_565 .
N1 Cu1 N1 180.0 5_565 .
C1 N1 N2 104.8(2) . .
C1 N1 Cu1 131.5(2) . .
N2 N1 Cu1 123.73(17) . .
C3 N2 N1 112.1(2) . .
N1 C1 C2 110.9(3) . .
C3 C2 C1 105.9(3) . .
N2 C3 C2 106.3(2) . .
N2 C3 C4 122.0(3) . .
C2 C3 C4 131.7(3) . .
N99 C99 S99 179.1(3) . .
C99 N99 Cu1 166.7(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N99 1.960(2) .
Cu1 N99 1.960(2) 5_565
Cu1 N1 2.015(2) 5_565
Cu1 N1 2.015(2) .
N1 C1 1.324(4) .
N1 N2 1.352(3) .
N2 C3 1.345(4) .
C1 C2 1.389(4) .
C2 C3 1.361(4) .
C3 C4 1.488(4) .
C99 N99 1.156(3) .
C99 S99 1.628(3) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1 H1O S99 1.05 2.49 3.4022(17) 143.9
N2 H2A O1 0.86 2.39 3.148(3) 147.2
N2 H2A N99 0.86 2.44 2.893(3) 113.2
