#------------------------------------------------------------------------------
#$Date: 2023-03-04 10:48:54 +0200 (Sat, 04 Mar 2023) $
#$Revision: 281297 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/25/7712510.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_7712510
loop_
_publ_author_name
'Hsieh, Chang-Chih'
'Liao, Po-Kuang'
'Chen, Chia-Wei'
'Chiang, Ming-Hsi'
'Horng, Yih-Chern'
_publ_section_title
;
 The effect of anions in the synthesis and structure of pyrazolylamidino
 copper(II) complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00103B
_journal_year                    2023
_chemical_formula_sum            'C10 H14 Cl4 Cu2 N6'
_chemical_formula_weight         487.17
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-11-28 deposited with the CCDC.	2023-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                94.69(2)
_cell_angle_beta                 104.15(2)
_cell_angle_gamma                106.77(3)
_cell_formula_units_Z            2
_cell_length_a                   8.279(3)
_cell_length_b                   9.550(3)
_cell_length_c                   11.678(4)
_cell_measurement_reflns_used    1491
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.05
_cell_measurement_theta_min      2.66
_cell_volume                     845.6(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0896
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8038
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.280
_diffrn_reflns_theta_min         2.258
_exptl_absorpt_coefficient_mu    3.149
_exptl_absorpt_correction_T_max  0.810
_exptl_absorpt_correction_T_min  0.754
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.913
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.896
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.797
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         4066
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.797
_refine_ls_R_factor_all          0.1123
_refine_ls_R_factor_gt           0.0546
_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)+(0.1000P)²+1.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.1790
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1824
_reflns_number_total             4066
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt00103b2.cif
_cod_data_source_block           Cpd3
_cod_database_code               7712510
_shelx_shelxl_version_number     2018/3
_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.
;
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.04798(10) 0.78230(8) 0.80325(6) 0.0414(2) Uani 1 1 d . . . . .
Cu2 Cu 0.44134(10) 0.76225(9) 0.75606(7) 0.0469(3) Uani 1 1 d . . . . .
Cl2 Cl 0.1375(2) 0.58111(17) 0.77784(14) 0.0494(4) Uani 1 1 d . . . . .
Cl4 Cl 0.3553(2) 0.96770(18) 0.77233(15) 0.0523(4) Uani 1 1 d . . . . .
Cl1 Cl 0.1292(2) 0.8164(2) 1.00368(13) 0.0591(5) Uani 1 1 d . . . . .
N6 N 0.5536(7) 0.7971(6) 0.9343(5) 0.0527(15) Uani 1 1 d . . . . .
H9 H 0.544828 0.868334 0.981407 0.063 Uiso 1 1 calc R U . . .
N1 N -0.0633(7) 0.7608(6) 0.6273(4) 0.0441(13) Uani 1 1 d . . . . .
N4 N 0.5649(7) 0.6093(6) 0.7721(5) 0.0481(13) Uani 1 1 d . . . . .
N3 N -0.0773(7) 0.9344(6) 0.7978(4) 0.0488(14) Uani 1 1 d . . . . .
H4 H -0.082466 0.981830 0.862953 0.059 Uiso 1 1 calc R U . . .
N2 N -0.1421(6) 0.8664(6) 0.6012(4) 0.0429(13) Uani 1 1 d . . . . .
C4 C -0.1484(8) 0.9580(7) 0.6956(5) 0.0409(14) Uani 1 1 d . . . . .
C9 C 0.6365(8) 0.7122(7) 0.9749(5) 0.0459(16) Uani 1 1 d . . . . .
C5 C -0.2388(10) 1.0719(8) 0.6691(6) 0.0596(19) Uani 1 1 d . . . . .
H5A H -0.226597 1.132691 0.743406 0.089 Uiso 1 1 calc R U . . .
H5B H -0.362522 1.022526 0.629034 0.089 Uiso 1 1 calc R U . . .
H5C H -0.185892 1.134074 0.617762 0.089 Uiso 1 1 calc R U . . .
C3 C -0.2049(9) 0.8550(9) 0.4802(6) 0.0587(19) Uani 1 1 d . . . . .
H3 H -0.264082 0.914524 0.439121 0.070 Uiso 1 1 calc R U . . .
C1 C -0.0787(10) 0.6856(8) 0.5264(6) 0.062(2) Uani 1 1 d . . . . .
H1 H -0.037506 0.604369 0.518288 0.074 Uiso 1 1 calc R U . . .
C2 C -0.1643(10) 0.7401(9) 0.4309(6) 0.068(2) Uani 1 1 d . . . . .
H2 H -0.189047 0.704679 0.348952 0.081 Uiso 1 1 calc R U . . .
Cl3 Cl 0.3856(3) 0.7258(2) 0.55729(15) 0.0646(5) Uani 1 1 d . . . . .
C10 C 0.7235(9) 0.7122(7) 1.1017(6) 0.0581(19) Uani 1 1 d . . . . .
H10A H 0.714512 0.794202 1.151804 0.087 Uiso 1 1 calc R U . . .
H10B H 0.846380 0.722771 1.111391 0.087 Uiso 1 1 calc R U . . .
H10C H 0.666565 0.619549 1.125069 0.087 Uiso 1 1 calc R U . . .
C6 C 0.5931(9) 0.5045(7) 0.7120(7) 0.0551(18) Uani 1 1 d . . . . .
H6 H 0.554232 0.480718 0.628005 0.066 Uiso 1 1 calc R U . . .
C8 C 0.7215(10) 0.4968(8) 0.8979(7) 0.063(2) Uani 1 1 d . . . . .
H8 H 0.785684 0.473939 0.967980 0.075 Uiso 1 1 calc R U . . .
C7 C 0.6887(10) 0.4294(9) 0.7856(7) 0.069(2) Uani 1 1 d . . . . .
H7 H 0.722538 0.348632 0.761150 0.082 Uiso 1 1 calc R U . . .
N5 N 0.6432(6) 0.6061(5) 0.8908(4) 0.0403(12) 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'
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 '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
N1 Cu1 N3 78.2(2) . . ?
N1 Cu1 Cl1 169.56(16) . . ?
N3 Cu1 Cl1 92.93(15) . . ?
N1 Cu1 Cl2 92.12(15) . . ?
N3 Cu1 Cl2 167.72(15) . . ?
Cl1 Cu1 Cl2 95.85(7) . . ?
N4 Cu2 N6 78.2(2) . . ?
N4 Cu2 Cl3 92.06(17) . . ?
N6 Cu2 Cl3 165.43(18) . . ?
N4 Cu2 Cl4 166.94(15) . . ?
N6 Cu2 Cl4 91.13(16) . . ?
Cl3 Cu2 Cl4 96.90(7) . . ?
N4 Cu2 Cl2 94.67(17) . . ?
N6 Cu2 Cl2 91.77(18) . . ?
Cl3 Cu2 Cl2 99.87(7) . . ?
Cl4 Cu2 Cl2 93.14(7) . . ?
Cu1 Cl2 Cu2 88.79(6) . . ?
C9 N6 Cu2 117.6(5) . . ?
C1 N1 N2 106.5(5) . . ?
C1 N1 Cu1 141.5(5) . . ?
N2 N1 Cu1 111.8(4) . . ?
C6 N4 N5 104.9(5) . . ?
C6 N4 Cu2 143.0(5) . . ?
N5 N4 Cu2 111.9(4) . . ?
C4 N3 Cu1 117.1(5) . . ?
C3 N2 N1 110.1(6) . . ?
C3 N2 C4 132.4(6) . . ?
N1 N2 C4 117.5(4) . . ?
N3 C4 N2 114.8(5) . . ?
N3 C4 C5 126.8(6) . . ?
N2 C4 C5 118.4(5) . . ?
N6 C9 N5 115.4(5) . . ?
N6 C9 C10 127.5(7) . . ?
N5 C9 C10 117.1(5) . . ?
C2 C3 N2 106.1(6) . . ?
N1 C1 C2 111.2(7) . . ?
C3 C2 C1 106.1(6) . . ?
N4 C6 C7 112.5(6) . . ?
C7 C8 N5 106.7(6) . . ?
C8 C7 C6 105.8(6) . . ?
C9 N5 C8 133.2(5) . . ?
C9 N5 N4 116.7(5) . . ?
C8 N5 N4 110.0(5) . . ?
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 N1 2.003(5) . ?
Cu1 N3 2.010(5) . ?
Cu1 Cl1 2.2397(18) . ?
Cu1 Cl2 2.2724(18) . ?
Cu2 N4 2.007(5) . ?
Cu2 N6 2.018(5) . ?
Cu2 Cl3 2.2301(19) . ?
Cu2 Cl4 2.2814(19) . ?
Cu2 Cl2 2.695(2) . ?
N6 C9 1.256(8) . ?
N1 C1 1.286(8) . ?
N1 N2 1.366(7) . ?
N4 C6 1.284(8) . ?
N4 N5 1.386(7) . ?
N3 C4 1.265(7) . ?
N2 C3 1.365(8) . ?
N2 C4 1.371(8) . ?
C4 C5 1.500(8) . ?
C9 N5 1.375(8) . ?
C9 C10 1.480(8) . ?
C3 C2 1.361(11) . ?
C1 C2 1.392(10) . ?
C6 C7 1.405(10) . ?
C8 C7 1.339(10) . ?
C8 N5 1.376(8) . ?
