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#$Date: 2019-11-17 08:35:03 +0200 (Sun, 17 Nov 2019) $
#$Revision: 228885 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/08/7230870.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_7230870
loop_
_publ_author_name
'Wu, Xiang-Wen'
'Pan, Feng'
'Yin, Shi'
'Ge, Jing-Yuan'
'Jin, Guo-Xia'
'Wang, Peng'
'Ma, Jian-Ping'
_publ_section_title
;
 Solvent-induced structural transformation and magnetic modulation in 1D
 copper(ii) polymers based on a semi-rigid ligand containing
 4-amino-1,2,4-triazole
;
_journal_issue                   28
_journal_name_full               CrystEngComm
_journal_page_first              3955
_journal_paper_doi               10.1039/C8CE00820E
_journal_volume                  20
_journal_year                    2018
_chemical_formula_sum            'C18.5 H16.25 Br2 Cu N6.75 S'
_chemical_formula_weight         588.55
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-11-17 deposited with the CCDC.
2018-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.4816(6)
_cell_length_b                   15.3597(17)
_cell_length_c                   19.7243(15)
_cell_measurement_reflns_used    1333
_cell_measurement_temperature    112(19)
_cell_measurement_theta_max      65.8680
_cell_measurement_theta_min      4.4870
_cell_volume                     2569.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      112(19)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0793
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0527
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            5568
_diffrn_reflns_theta_full        67.07
_diffrn_reflns_theta_max         67.07
_diffrn_reflns_theta_min         3.65
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 1.00
_diffrn_standards_interval_time  2.92
_diffrn_standards_number         6212
_exptl_absorpt_coefficient_mu    5.741
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1158
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.904
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.45(7)
_refine_ls_extinction_coef       0.0015(3)
_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    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         3490
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0843
_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)+(0.1439P)²+4.1063P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2284
_refine_ls_wR_factor_ref         0.2420
_reflns_number_gt                2868
_reflns_number_total             3490
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8ce00820e2.cif
_cod_data_source_block           exp_1692
_cod_depositor_comments
'Adding full bibliography for 7230867--7230871.cif.'
_cod_original_formula_sum        'C18.50 H16.25 Br2 Cu N6.75 S'
_cod_database_code               7230870
_oxdiff_exptl_absorpt_empirical_full_min 0.641
_oxdiff_exptl_absorpt_empirical_full_max 1.524
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, 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
N6 N 0.1882(11) 0.6267(8) 0.8634(6) 0.066(3) Uani 1 1 d . . .
Br2 Br 1.03079(16) 0.51211(8) 0.29051(8) 0.0660(5) Uani 1 1 d . A .
Cu1 Cu 0.8336(2) 0.49923(13) 0.38022(13) 0.0654(6) Uani 1 1 d . . .
S1 S 0.8158(6) 0.8851(3) 0.5307(2) 0.0955(16) Uani 1 1 d . A .
N4 N 0.6271(14) 0.8156(7) 0.6261(7) 0.071(3) Uani 1 1 d . . .
C8 C 0.5957(16) 0.7367(9) 0.6543(8) 0.065(4) Uani 1 1 d . . .
C17 C 0.1209(16) 0.6854(10) 0.9038(8) 0.069(4) Uani 1 1 d . . .
H17 H 0.0573 0.6646 0.9386 0.083 Uiso 1 1 calc R . .
C12 C 0.2823(14) 0.6564(9) 0.8121(7) 0.056(3) Uani 1 1 d . . .
N3 N 0.6888(12) 0.6777(8) 0.6263(7) 0.070(3) Uani 1 1 d . . .
C15 C 0.2355(17) 0.8059(10) 0.8457(8) 0.070(4) Uani 1 1 d . . .
H15 H 0.2519 0.8653 0.8401 0.084 Uiso 1 1 calc R . .
C13 C 0.3537(14) 0.5947(8) 0.7691(7) 0.063(3) Uani 1 1 d . . .
H13 H 0.3337 0.5356 0.7745 0.075 Uiso 1 1 calc R . .
N1 N 0.8120(12) 0.6287(7) 0.3783(6) 0.061(3) Uani 1 1 d . A .
C14 C 0.4528(14) 0.6234(9) 0.7194(8) 0.064(3) Uani 1 1 d . . .
H14 H 0.5026 0.5826 0.6919 0.077 Uiso 1 1 calc R . .
C11 C 0.3076(12) 0.7477(7) 0.8022(6) 0.052(3) Uani 1 1 d . . .
C5 C 0.8737(15) 0.6772(10) 0.4259(7) 0.064(3) Uani 1 1 d . . .
H5 H 0.9269 0.6509 0.4617 0.076 Uiso 1 1 calc R A .
N2 N 0.7791(14) 0.7199(9) 0.5757(7) 0.078(4) Uani 1 1 d . . .
C16 C 0.1382(15) 0.7764(10) 0.8982(8) 0.066(3) Uani 1 1 d . . .
H16 H 0.0879 0.8146 0.9277 0.079 Uiso 1 1 calc R . .
N5 N 0.5537(16) 0.8961(8) 0.6347(8) 0.090(4) Uani 1 1 d . . .
H5A H 0.4522 0.8877 0.6441 0.134 Uiso 1 1 d R . .
H5B H 0.5625 0.9264 0.5964 0.134 Uiso 1 1 d R . .
C7 C 0.7419(17) 0.8006(10) 0.5798(9) 0.076(4) Uani 1 1 d . . .
C6 C 0.9508(16) 0.8189(12) 0.4790(9) 0.087(6) Uani 1 1 d . . .
H6A H 1.0267 0.8567 0.4571 0.104 Uiso 1 1 calc R A .
H6B H 1.0083 0.7794 0.5083 0.104 Uiso 1 1 calc R . .
C9 C 0.4828(15) 0.7142(9) 0.7081(8) 0.063(3) Uani 1 1 d . . .
C10 C 0.4097(14) 0.7745(9) 0.7508(7) 0.060(3) Uani 1 1 d . . .
H10 H 0.4295 0.8336 0.7449 0.071 Uiso 1 1 calc R . .
C3 C 0.7821(17) 0.8071(10) 0.3734(8) 0.073(4) Uani 1 1 d . . .
H3 H 0.7765 0.8675 0.3714 0.088 Uiso 1 1 calc R A .
C4 C 0.8614(14) 0.7650(10) 0.4238(7) 0.062(3) Uani 1 1 d . A .
C1 C 0.7265(17) 0.6646(10) 0.3278(9) 0.077(4) Uani 1 1 d . . .
H1 H 0.6792 0.6294 0.2953 0.092 Uiso 1 1 calc R A .
C2 C 0.7096(18) 0.7542(10) 0.3247(10) 0.078(4) Uani 1 1 d . A .
H2 H 0.6501 0.7792 0.2902 0.093 Uiso 1 1 calc R . .
Br1 Br 0.5716(5) 0.4780(2) 0.4402(3) 0.1103(18) Uani 0.50 1 d P A 1
N7 N 0.989(4) 0.474(2) 0.4776(18) 0.099(9) Uani 0.50 1 d PDU A 1
C18 C 1.098(4) 0.456(3) 0.5064(19) 0.107(12) Uani 0.50 1 d PDU A 1
C19 C 1.201(5) 0.414(3) 0.562(2) 0.135(16) Uani 0.50 1 d PDU A 1
H19A H 1.2674 0.4577 0.5814 0.202 Uiso 0.50 1 calc PR A 1
H19B H 1.2643 0.3690 0.5421 0.202 Uiso 0.50 1 calc PR A 1
H19C H 1.1340 0.3896 0.5961 0.202 Uiso 0.50 1 calc PR A 1
N8 N 0.499(6) 0.367(5) 0.680(3) 0.099(12) Uani 0.25 1 d PDU B 1
C21 C 0.601(6) 0.397(5) 0.653(3) 0.099(12) Uani 0.25 1 d PDU B 1
C20 C 0.731(7) 0.453(5) 0.623(4) 0.098(12) Uani 0.25 1 d PDU B 1
H20A H 0.7542 0.4336 0.5780 0.147 Uiso 0.25 1 calc PR B 1
H20B H 0.8239 0.4489 0.6506 0.147 Uiso 0.25 1 calc PR B 1
H20C H 0.6969 0.5129 0.6215 0.147 Uiso 0.25 1 calc PR B 1
Br1' Br 0.7344(6) 0.4960(2) 0.4873(2) 0.0956(14) Uani 0.50 1 d P A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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
C17 N6 C12 117.8(12) . .
C17 N6 Cu1 121.6(10) . 2_665
C12 N6 Cu1 120.4(9) . 2_665
N6 Cu1 N1 164.9(5) 2_664 .
N6 Cu1 Br1' 95.8(4) 2_664 .
N1 Cu1 Br1' 90.3(3) . .
N6 Cu1 N7 91.7(9) 2_664 .
N1 Cu1 N7 103.2(9) . .
Br1' Cu1 N7 56.4(9) . .
N6 Cu1 Br2 91.2(3) 2_664 .
N1 Cu1 Br2 88.2(3) . .
Br1' Cu1 Br2 158.09(18) . .
N7 Cu1 Br2 102.7(9) . .
N6 Cu1 Br1 82.5(3) 2_664 .
N1 Cu1 Br1 93.2(3) . .
Br1' Cu1 Br1 40.6(2) . .
N7 Cu1 Br1 95.1(9) . .
Br2 Cu1 Br1 161.32(19) . .
C7 S1 C6 96.9(8) . .
C7 N4 C8 105.3(12) . .
C7 N4 N5 123.7(13) . .
C8 N4 N5 130.8(11) . .
N3 C8 N4 108.8(12) . .
N3 C8 C9 122.0(14) . .
N4 C8 C9 129.2(12) . .
N6 C17 C16 125.5(14) . .
N6 C17 H17 117.3 . .
C16 C17 H17 117.3 . .
N6 C12 C13 118.2(12) . .
N6 C12 C11 121.0(12) . .
C13 C12 C11 120.8(12) . .
C8 N3 N2 107.8(12) . .
C11 C15 C16 120.8(14) . .
C11 C15 H15 119.6 . .
C16 C15 H15 119.6 . .
C14 C13 C12 118.7(12) . .
C14 C13 H13 120.6 . .
C12 C13 H13 120.6 . .
C5 N1 C1 120.8(13) . .
C5 N1 Cu1 121.1(10) . .
C1 N1 Cu1 118.0(9) . .
C13 C14 C9 122.3(12) . .
C13 C14 H14 118.8 . .
C9 C14 H14 118.8 . .
C15 C11 C10 122.3(12) . .
C15 C11 C12 118.9(12) . .
C10 C11 C12 118.7(11) . .
N1 C5 C4 121.0(14) . .
N1 C5 H5 119.5 . .
C4 C5 H5 119.5 . .
C7 N2 N3 105.4(11) . .
C15 C16 C17 116.1(14) . .
C15 C16 H16 122.0 . .
C17 C16 H16 122.0 . .
N4 N5 H5A 109.1 . .
N4 N5 H5B 108.8 . .
H5A N5 H5B 109.5 . .
N2 C7 N4 112.6(13) . .
N2 C7 S1 126.8(12) . .
N4 C7 S1 120.5(12) . .
C4 C6 S1 112.1(9) . .
C4 C6 H6A 109.2 . .
S1 C6 H6A 109.2 . .
C4 C6 H6B 109.2 . .
S1 C6 H6B 109.2 . .
H6A C6 H6B 107.9 . .
C10 C9 C14 118.1(14) . .
C10 C9 C8 124.7(13) . .
C14 C9 C8 117.1(12) . .
C11 C10 C9 121.2(13) . .
C11 C10 H10 119.4 . .
C9 C10 H10 119.4 . .
C4 C3 C2 116.2(14) . .
C4 C3 H3 121.9 . .
C2 C3 H3 121.9 . .
C5 C4 C3 122.1(13) . .
C5 C4 C6 118.0(14) . .
C3 C4 C6 119.8(14) . .
N1 C1 C2 119.7(15) . .
N1 C1 H1 120.2 . .
C2 C1 H1 120.2 . .
C1 C2 C3 120.0(17) . .
C1 C2 H2 120.0 . .
C3 C2 H2 120.0 . .
C18 N7 Cu1 156(3) . .
N7 C18 C19 159(4) . .
N8 C21 C20 170(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N6 C17 1.331(19) .
N6 C12 1.369(17) .
N6 Cu1 1.970(12) 2_665
Br2 Cu1 2.443(3) .
Cu1 N6 1.970(12) 2_664
Cu1 N1 1.997(11) .
Cu1 Br1' 2.275(4) .
Cu1 N7 2.36(3) .
Cu1 Br1 2.538(4) .
S1 C7 1.737(16) .
S1 C6 1.840(14) .
N4 C7 1.355(18) .
N4 C8 1.361(19) .
N4 N5 1.395(16) .
C8 N3 1.322(16) .
C8 C9 1.47(2) .
C17 C16 1.41(2) .
C17 H17 0.9300 .
C12 C13 1.408(18) .
C12 C11 1.432(18) .
N3 N2 1.415(17) .
C15 C11 1.382(18) .
C15 C16 1.40(2) .
C15 H15 0.9300 .
C13 C14 1.364(19) .
C13 H13 0.9300 .
N1 C5 1.307(16) .
N1 C1 1.35(2) .
C14 C9 1.435(19) .
C14 H14 0.9300 .
C11 C10 1.395(18) .
C5 C4 1.35(2) .
C5 H5 0.9300 .
N2 C7 1.28(2) .
C16 H16 0.9300 .
N5 H5A 0.8900 .
N5 H5B 0.8900 .
C6 C4 1.563(19) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C9 C10 1.398(19) .
C10 H10 0.9300 .
C3 C4 1.36(2) .
C3 C2 1.40(2) .
C3 H3 0.9300 .
C1 C2 1.38(2) .
C1 H1 0.9300 .
C2 H2 0.9300 .
N7 C18 1.125(10) .
C18 C19 1.533(10) .
C19 H19A 0.9600 .
C19 H19B 0.9600 .
C19 H19C 0.9600 .
N8 C21 1.118(10) .
C21 C20 1.519(10) .
C20 H20A 0.9600 .
C20 H20B 0.9600 .
C20 H20C 0.9600 .
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
C7 N4 C8 N3 0.5(17) .
N5 N4 C8 N3 174.7(14) .
C7 N4 C8 C9 179.1(14) .
N5 N4 C8 C9 -7(3) .
C12 N6 C17 C16 0(2) .
Cu1 N6 C17 C16 175.8(10) 2_665
C17 N6 C12 C13 -179.9(12) .
Cu1 N6 C12 C13 4.3(16) 2_665
C17 N6 C12 C11 0.1(17) .
Cu1 N6 C12 C11 -175.7(8) 2_665
N4 C8 N3 N2 -2.7(15) .
C9 C8 N3 N2 178.5(12) .
N6 C12 C13 C14 -177.4(12) .
C11 C12 C13 C14 2.6(19) .
N6 Cu1 N1 C5 167.3(16) 2_664
Br1' Cu1 N1 C5 53.5(10) .
N7 Cu1 N1 C5 -2.0(13) .
Br2 Cu1 N1 C5 -104.6(10) .
Br1 Cu1 N1 C5 94.0(10) .
N6 Cu1 N1 C1 -10(3) 2_664
Br1' Cu1 N1 C1 -124.0(10) .
N7 Cu1 N1 C1 -179.4(13) .
Br2 Cu1 N1 C1 77.9(10) .
Br1 Cu1 N1 C1 -83.4(10) .
C12 C13 C14 C9 -2(2) .
C16 C15 C11 C10 -177.7(12) .
C16 C15 C11 C12 -0.6(19) .
N6 C12 C11 C15 0.2(18) .
C13 C12 C11 C15 -179.8(12) .
N6 C12 C11 C10 177.4(11) .
C13 C12 C11 C10 -2.6(17) .
C1 N1 C5 C4 -3.8(19) .
Cu1 N1 C5 C4 178.8(9) .
C8 N3 N2 C7 4.0(16) .
C11 C15 C16 C17 0.7(19) .
N6 C17 C16 C15 0(2) .
N3 N2 C7 N4 -3.8(19) .
N3 N2 C7 S1 179.5(11) .
C8 N4 C7 N2 2(2) .
N5 N4 C7 N2 -172.5(13) .
C8 N4 C7 S1 179.1(11) .
N5 N4 C7 S1 4(2) .
C6 S1 C7 N2 -0.5(17) .
C6 S1 C7 N4 -176.9(14) .
C7 S1 C6 C4 75.7(14) .
C13 C14 C9 C10 1(2) .
C13 C14 C9 C8 178.2(12) .
N3 C8 C9 C10 163.6(13) .
N4 C8 C9 C10 -15(2) .
N3 C8 C9 C14 -13(2) .
N4 C8 C9 C14 168.7(14) .
C15 C11 C10 C9 179.1(12) .
C12 C11 C10 C9 2.0(18) .
C14 C9 C10 C11 -1.4(19) .
C8 C9 C10 C11 -177.9(12) .
N1 C5 C4 C3 1(2) .
N1 C5 C4 C6 -174.7(11) .
C2 C3 C4 C5 2(2) .
C2 C3 C4 C6 177.9(11) .
S1 C6 C4 C5 -119.7(13) .
S1 C6 C4 C3 64.1(17) .
C5 N1 C1 C2 3(2) .
Cu1 N1 C1 C2 -179.7(11) .
N1 C1 C2 C3 1(2) .
C4 C3 C2 C1 -3(2) .
N6 Cu1 N7 C18 73(8) 2_664
N1 Cu1 N7 C18 -109(8) .
Br1' Cu1 N7 C18 169(9) .
Br2 Cu1 N7 C18 -18(8) .
Br1 Cu1 N7 C18 156(8) .
Cu1 N7 C18 C19 -139(10) .
