#------------------------------------------------------------------------------
#$Date: 2023-11-05 01:56:22 +0200 (Sun, 05 Nov 2023) $
#$Revision: 287262 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/76/7247668.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_7247668
loop_
_publ_author_name
'Lu, Kuang-Lieh'
'Sie, Shu-Ling'
'Kamal, Surabhi'
'Zong-Zhan, Lu'
'Wei, Ling-Fang'
'Luo, Tzuoo-Tsair'
'Liu, Yen-Hsiang'
'Chang, Chao-Wan'
'Chi, Kai-Ming'
_publ_section_title
;
 Fine-tuning synthesis of a novel CuI/CuII mixed-valence coordination
 polymer
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D3CE01001E
_journal_year                    2023
_chemical_formula_moiety         'C6 H4 Cl Cu2 N5'
_chemical_formula_sum            'C6 H4 Cl Cu2 N5'
_chemical_formula_weight         308.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difma;
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-10-21 deposited with the CCDC.	2023-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.953(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.689(5)
_cell_length_b                   3.6236(9)
_cell_length_c                   11.631(3)
_cell_measurement_reflns_used    2199
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.59
_cell_measurement_theta_min      2.05
_cell_volume                     808.7(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 19)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX2'
_diffrn_measurement_method       'phi & omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            1437
_diffrn_reflns_point_group_measured_fraction_full 0.838
_diffrn_reflns_point_group_measured_fraction_max 0.838
_diffrn_reflns_theta_full        25.069
_diffrn_reflns_theta_max         25.069
_diffrn_reflns_theta_min         2.123
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.543
_exptl_absorpt_correction_T_max  0.8087
_exptl_absorpt_correction_T_min  0.3752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.535
_exptl_crystal_description       prism
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.894
_refine_diff_density_rms         0.312
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.38(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1200
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0240
_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)+(0.0805P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.1018
_reflns_Friedel_coverage         0.712
_reflns_Friedel_fraction_full    0.699
_reflns_Friedel_fraction_max     0.698
_reflns_number_gt                1156
_reflns_number_total             1200
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3ce01001e2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        808.7(3)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7247668
_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.
;
_shelx_estimated_absorpt_t_min   0.375
_shelx_estimated_absorpt_t_max   0.809
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'
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 -0.14358(8) -0.1553(4) 0.64765(14) 0.0215(4) Uani 1 1 d . . . . .
Cu2 Cu -0.05000(6) -0.9890(3) 0.46608(9) 0.0192(4) Uani 1 1 d . . . . .
Cl1 Cl -0.13477(13) -0.4986(6) 0.4667(2) 0.0164(6) Uani 1 1 d . . . . .
C1 C 0.0567(5) 0.141(3) 0.7142(8) 0.013(2) Uani 1 1 d . . . . .
C2 C 0.1244(5) 0.222(3) 0.6871(9) 0.0120(18) Uani 1 1 d . . . . .
C3 C 0.1753(5) 0.385(3) 0.7735(9) 0.0126(19) Uani 1 1 d . . . . .
H3 H 0.164467 0.463987 0.845212 0.015 Uiso 1 1 calc R U . . .
C4 C 0.2411(5) 0.434(3) 0.7563(10) 0.017(2) Uani 1 1 d . . . . .
H4 H 0.275057 0.550338 0.816363 0.020 Uiso 1 1 calc R U . . .
C5 C 0.2094(5) 0.173(2) 0.5715(9) 0.0137(19) Uani 1 1 d . . . . .
H5 H 0.221407 0.099052 0.500210 0.016 Uiso 1 1 calc R U . . .
C6 C 0.1418(5) 0.121(3) 0.5818(9) 0.0136(19) Uani 1 1 d . . . . .
H6 H 0.107895 0.019203 0.518676 0.016 Uiso 1 1 calc R U . . .
N1 N -0.0476(5) -0.030(2) 0.7096(10) 0.0150(17) Uani 1 1 d . . . . .
N2 N -0.0027(4) 0.032(2) 0.6403(8) 0.0127(17) Uani 1 1 d . . . . .
N3 N 0.0495(4) 0.149(2) 0.8269(7) 0.0150(17) Uani 1 1 d . . . . .
N4 N -0.0159(4) 0.040(2) 0.8208(8) 0.0150(19) Uani 1 1 d . . . . .
N5 N 0.2594(4) 0.323(2) 0.6566(8) 0.0151(17) 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
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'
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'
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 N5 152.7(4) . 3_445 ?
N1 Cu1 Cl1 100.7(3) . . ?
N5 Cu1 Cl1 106.4(3) 3_445 . ?
N4 Cu2 N2 133.9(3) 2_544 1_545 ?
N4 Cu2 Cl1 116.0(3) 2_544 . ?
N2 Cu2 Cl1 97.5(2) 1_545 . ?
N4 Cu2 Cl1 106.9(3) 2_544 1_545 ?
N2 Cu2 Cl1 100.5(2) 1_545 1_545 ?
Cl1 Cu2 Cl1 94.63(9) . 1_545 ?
Cu2 Cl1 Cu1 123.05(11) . . ?
Cu2 Cl1 Cu2 94.63(9) . 1_565 ?
Cu1 Cl1 Cu2 78.78(8) . 1_565 ?
N2 C1 N3 111.2(9) . . ?
N2 C1 C2 128.5(9) . . ?
N3 C1 C2 120.2(8) . . ?
C3 C2 C6 118.0(9) . . ?
C3 C2 C1 118.4(8) . . ?
C6 C2 C1 123.5(9) . . ?
C4 C3 C2 120.4(9) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
N5 C4 C3 122.1(9) . . ?
N5 C4 H4 118.9 . . ?
C3 C4 H4 118.9 . . ?
N5 C5 C6 123.6(9) . . ?
N5 C5 H5 118.2 . . ?
C6 C5 H5 118.2 . . ?
C5 C6 C2 118.4(9) . . ?
C5 C6 H6 120.8 . . ?
C2 C6 H6 120.8 . . ?
N4 N1 N2 108.9(8) . . ?
N4 N1 Cu1 128.2(8) . . ?
N2 N1 Cu1 122.6(8) . . ?
N1 N2 C1 105.1(9) . . ?
N1 N2 Cu2 112.2(6) . 1_565 ?
C1 N2 Cu2 141.7(7) . 1_565 ?
N4 N3 C1 104.6(8) . . ?
N1 N4 N3 110.2(9) . . ?
N1 N4 Cu2 130.1(7) . 2_545 ?
N3 N4 Cu2 119.6(6) . 2_545 ?
C5 N5 C4 117.4(9) . . ?
C5 N5 Cu1 123.0(7) . 3 ?
C4 N5 Cu1 119.4(7) . 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 N1 1.920(10) . ?
Cu1 N5 1.938(8) 3_445 ?
Cu1 Cl1 2.484(3) . ?
Cu2 N4 1.962(9) 2_544 ?
Cu2 N2 2.033(9) 1_545 ?
Cu2 Cl1 2.439(2) . ?
Cu2 Cl1 2.490(2) 1_545 ?
C1 N2 1.347(13) . ?
C1 N3 1.350(13) . ?
C1 C2 1.467(13) . ?
C2 C3 1.384(14) . ?
C2 C6 1.392(14) . ?
C3 C4 1.366(15) . ?
C3 H3 0.9500 . ?
C4 N5 1.350(15) . ?
C4 H4 0.9500 . ?
C5 N5 1.345(13) . ?
C5 C6 1.375(15) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
N1 N4 1.328(14) . ?
N1 N2 1.341(14) . ?
N3 N4 1.334(12) . ?
