# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_LBCu
_database_code_depnum_ccdc_archive 'CCDC 1977263'
loop_
_audit_author_name
_audit_author_address
'Hyosun Lee'
;Kyungpook National University
South Korea
;
_audit_update_record             
;
2020-04-11 deposited with the CCDC.	2020-04-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H48 Cl8 Cu4 N8 O4'
_chemical_formula_weight         1194.58

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0020 0.0010 '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'
Cl Cl 0.1230 0.1260 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3380 1.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0040 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0080 0.0050 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.8760(18)
_cell_length_b                   6.9330(14)
_cell_length_c                   18.664(4)
_cell_angle_alpha                90
_cell_angle_beta                 93.56(3)
_cell_angle_gamma                90
_cell_volume                     1146.3(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    19224
_cell_measurement_theta_min      0.361
_cell_measurement_theta_max      33.548

_exptl_crystal_description       cubic
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_F_000             604
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.103
_exptl_absorpt_coefficient_mu    1.677
_shelx_estimated_absorpt_T_min   0.779
_shelx_estimated_absorpt_T_max   0.846
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.864
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.630
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13176
_diffrn_reflns_av_unetI/netI     0.0806
_diffrn_reflns_av_R_equivalents  0.1146
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.779
_diffrn_reflns_theta_max         29.997
_diffrn_reflns_theta_full        22.210
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measured_fraction_theta_full 0.925
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_Laue_measured_fraction_full 0.925
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_point_group_measured_fraction_full 0.925
_reflns_number_total             4618
_reflns_number_gt                4392
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'PAL BL2D-SMDC Program (Shin et. al, 2016)'
_computing_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury 4.1.0'
_computing_publication_material  'enCIFer 1.7.1'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1121P)²+0.3926P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4618
_refine_ls_number_parameters     137
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0577
_refine_ls_wR_factor_ref         0.1742
_refine_ls_wR_factor_gt          0.1719
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_restrained_S_all      1.139
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.07264(2) 0.74558(2) 0.00987(2) 0.00801(11) Uani 1 1 d . . . . .
N01 N 0.23606(15) 0.84553(19) 0.08249(7) 0.0102(2) Uani 1 1 d . . . . .
N02 N 0.25986(12) 0.67292(18) -0.04153(6) 0.0079(2) Uani 1 1 d . . . . .
Cl1 Cl -0.08388(3) 0.61576(5) -0.07835(2) 0.00919(11) Uani 1 1 d . . . . .
Cl2 Cl -0.11881(4) 0.87874(5) 0.06740(2) 0.01134(11) Uani 1 1 d . . . . .
O1 O 0.31106(15) 0.6598(2) 0.22004(7) 0.0169(2) Uani 1 1 d . . . . .
C01 C 0.26699(15) 0.5773(2) -0.10322(8) 0.0102(2) Uani 1 1 d . . . . .
H01 H 0.176862 0.525725 -0.125723 0.012 Uiso 1 1 calc R U . . .
C02 C 0.40312(16) 0.5507(2) -0.13578(8) 0.0125(2) Uani 1 1 d . . . . .
H02 H 0.405200 0.482973 -0.179953 0.015 Uiso 1 1 calc R U . . .
C03 C 0.53491(16) 0.6243(2) -0.10281(9) 0.0129(3) Uani 1 1 d . . . . .
H03 H 0.628148 0.610213 -0.124653 0.015 Uiso 1 1 calc R U . . .
C04 C 0.52920(16) 0.7196(2) -0.03705(9) 0.0118(3) Uani 1 1 d . . . . .
H04 H 0.618160 0.768780 -0.012652 0.014 Uiso 1 1 calc R U . . .
C05 C 0.3898(2) 0.73997(17) -0.00864(10) 0.0091(3) Uani 1 1 d . . . . .
C06 C 0.36985(16) 0.8305(2) 0.06134(8) 0.0110(2) Uani 1 1 d . . . . .
H06 H 0.454239 0.876691 0.090135 0.013 Uiso 1 1 calc R U . . .
C07 C 0.21415(18) 0.9284(2) 0.15311(8) 0.0138(3) Uani 1 1 d . . . . .
H07A H 0.130232 1.022623 0.149251 0.017 Uiso 1 1 calc R U . . .
H07B H 0.306818 0.997434 0.170734 0.017 Uiso 1 1 calc R U . . .
C08 C 0.1785(2) 0.7713(3) 0.20577(10) 0.0151(3) Uani 1 1 d . . . . .
H08A H 0.145890 0.829103 0.250783 0.018 Uiso 1 1 calc R U . . .
H08B H 0.095801 0.688657 0.185124 0.018 Uiso 1 1 calc R U . . .
C09 C 0.2841(3) 0.5001(3) 0.26536(10) 0.0257(4) Uani 1 1 d . . . . .
H09A H 0.248938 0.546832 0.310974 0.039 Uiso 1 1 calc R U . . .
H09B H 0.377886 0.427005 0.274474 0.039 Uiso 1 1 calc R U . . .
H09C H 0.207033 0.416346 0.241861 0.039 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 N02 2.0330(13) . ?
Cu1 N01 2.0438(14) . ?
Cu1 Cl2 2.2627(6) . ?
Cu1 Cl1 2.2732(7) . ?
N01 C06 1.279(2) . ?
N01 C07 1.462(2) . ?
N02 C01 1.3336(19) . ?
N02 C05 1.355(2) . ?
O1 C08 1.419(2) . ?
O1 C09 1.423(2) . ?
C01 C02 1.3980(19) . ?
C01 H01 0.9500 . ?
C02 C03 1.385(2) . ?
C02 H02 0.9500 . ?
C03 C04 1.397(2) . ?
C03 H03 0.9500 . ?
C04 C05 1.383(2) . ?
C04 H04 0.9500 . ?
C05 C06 1.470(2) . ?
C06 H06 0.9500 . ?
C07 C08 1.514(2) . ?
C07 H07A 0.9900 . ?
C07 H07B 0.9900 . ?
C08 H08A 0.9900 . ?
C08 H08B 0.9900 . ?
C09 H09A 0.9800 . ?
C09 H09B 0.9800 . ?
C09 H09C 0.9800 . ?

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
N02 Cu1 N01 80.19(5) . . ?
N02 Cu1 Cl2 170.05(4) . . ?
N01 Cu1 Cl2 94.01(4) . . ?
N02 Cu1 Cl1 92.34(4) . . ?
N01 Cu1 Cl1 172.43(4) . . ?
Cl2 Cu1 Cl1 93.56(2) . . ?
C06 N01 C07 119.24(12) . . ?
C06 N01 Cu1 113.71(10) . . ?
C07 N01 Cu1 127.05(10) . . ?
C01 N02 C05 118.49(13) . . ?
C01 N02 Cu1 127.92(9) . . ?
C05 N02 Cu1 113.52(11) . . ?
C08 O1 C09 111.56(15) . . ?
N02 C01 C02 121.97(13) . . ?
N02 C01 H01 119.0 . . ?
C02 C01 H01 119.0 . . ?
C03 C02 C01 119.16(14) . . ?
C03 C02 H02 120.4 . . ?
C01 C02 H02 120.4 . . ?
C02 C03 C04 119.25(14) . . ?
C02 C03 H03 120.4 . . ?
C04 C03 H03 120.4 . . ?
C05 C04 C03 117.84(14) . . ?
C05 C04 H04 121.1 . . ?
C03 C04 H04 121.1 . . ?
N02 C05 C04 123.23(15) . . ?
N02 C05 C06 113.77(15) . . ?
C04 C05 C06 122.97(15) . . ?
N01 C06 C05 118.33(13) . . ?
N01 C06 H06 120.8 . . ?
C05 C06 H06 120.8 . . ?
N01 C07 C08 110.34(13) . . ?
N01 C07 H07A 109.6 . . ?
C08 C07 H07A 109.6 . . ?
N01 C07 H07B 109.6 . . ?
C08 C07 H07B 109.6 . . ?
H07A C07 H07B 108.1 . . ?
O1 C08 C07 108.01(15) . . ?
O1 C08 H08A 110.1 . . ?
C07 C08 H08A 110.1 . . ?
O1 C08 H08B 110.1 . . ?
C07 C08 H08B 110.1 . . ?
H08A C08 H08B 108.4 . . ?
O1 C09 H09A 109.5 . . ?
O1 C09 H09B 109.5 . . ?
H09A C09 H09B 109.5 . . ?
O1 C09 H09C 109.5 . . ?
H09A C09 H09C 109.5 . . ?
H09B C09 H09C 109.5 . . ?

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
C05 N02 C01 C02 -2.3(2) . . . . ?
Cu1 N02 C01 C02 174.56(11) . . . . ?
N02 C01 C02 C03 0.5(2) . . . . ?
C01 C02 C03 C04 1.4(2) . . . . ?
C02 C03 C04 C05 -1.5(2) . . . . ?
C01 N02 C05 C04 2.2(2) . . . . ?
Cu1 N02 C05 C04 -175.14(11) . . . . ?
C01 N02 C05 C06 -175.81(13) . . . . ?
Cu1 N02 C05 C06 6.90(15) . . . . ?
C03 C04 C05 N02 -0.2(2) . . . . ?
C03 C04 C05 C06 177.54(14) . . . . ?
C07 N01 C06 C05 177.68(13) . . . . ?
Cu1 N01 C06 C05 -2.23(17) . . . . ?
N02 C05 C06 N01 -3.17(19) . . . . ?
C04 C05 C06 N01 178.86(14) . . . . ?
C06 N01 C07 C08 -104.72(17) . . . . ?
Cu1 N01 C07 C08 75.19(16) . . . . ?
C09 O1 C08 C07 -175.87(14) . . . . ?
N01 C07 C08 O1 69.83(16) . . . . ?

_refine_diff_density_max         2.699
_refine_diff_density_min         -2.403
_refine_diff_density_rms         0.201

# start Validation Reply Form
_vrf_PLAT971_LBCu                
;
PROBLEM: Check Calcd Resid. Dens.  0.67A   From Cu1             2.85 eA-3  
RESPONSE: The alert was mainly due the large residual electron density
near Cu metal center. However, all the q peaks appreared has less than 1A
distance to the Cu, and therefore, such residual density is not likely 
from unaccounted atom types.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_SL6Cu-a
_database_code_depnum_ccdc_archive 'CCDC 1977264'
loop_
_audit_author_name
_audit_author_address
'Hyosun Lee'
;Kyungpook National University
South Korea
;
_audit_update_record             
;
2020-03-26 deposited with the CCDC.	2020-04-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C13 H19 Cl2 Cu N3'
_chemical_formula_weight         351.75

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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.3629(19)
_cell_length_b                   6.8532(11)
_cell_length_c                   19.328(3)
_cell_angle_alpha                90
_cell_angle_beta                 104.988(4)
_cell_angle_gamma                90
_cell_volume                     1453.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    2720
_cell_measurement_theta_min      3.17
_cell_measurement_theta_max      26.53

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_F_000             724
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.859
_shelx_estimated_absorpt_T_min   0.624
_shelx_estimated_absorpt_T_max   0.836
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6241
_exptl_absorpt_correction_T_max  0.8359
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10315
_diffrn_reflns_av_unetI/netI     0.0925
_diffrn_reflns_av_R_equivalents  0.0675
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.182
_diffrn_reflns_theta_max         28.354
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             3595
_reflns_number_gt                2084
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2017)'
_computing_molecular_graphics    'Mercury 4.1.0'
_computing_publication_material  'enCIFer 1.7.1'
_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0408P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3595
_refine_ls_number_parameters     172
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1051
_refine_ls_R_factor_gt           0.0431
_refine_ls_wR_factor_ref         0.1178
_refine_ls_wR_factor_gt          0.0830
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.54593(4) 0.72396(7) 0.19978(3) 0.02255(16) Uani 1 1 d . . . . .
Cl1 Cl 0.34983(9) 0.88562(16) 0.12289(6) 0.0307(3) Uani 1 1 d . . . . .
Cl2 Cl 0.66780(9) 0.98061(15) 0.23720(6) 0.0271(3) Uani 1 1 d . . . . .
N1 N 0.4839(3) 0.6897(5) 0.29184(17) 0.0198(7) Uani 1 1 d . . . . .
N2 N 0.5000(3) 0.4466(5) 0.18716(18) 0.0234(8) Uani 1 1 d . . . . .
C1 C 0.4303(4) 0.8721(6) 0.3117(2) 0.0273(10) Uani 1 1 d . . . . .
H1A H 0.358813 0.908150 0.272360 0.033 Uiso 1 1 calc R U . . .
H1AB H 0.491019 0.978262 0.316634 0.033 Uiso 1 1 calc R U . . .
C2 C 0.3907(4) 0.8570(7) 0.3810(2) 0.0320(11) Uani 1 1 d . . . . .
H2A H 0.324261 0.760128 0.375165 0.038 Uiso 1 1 calc R U . . .
H2AB H 0.359312 0.984842 0.392083 0.038 Uiso 1 1 calc R U . . .
C3 C 0.4978(4) 0.7956(7) 0.4426(2) 0.0350(11) Uani 1 1 d . . . . .
H3A H 0.469186 0.774094 0.486213 0.042 Uiso 1 1 calc R U . . .
H3AB H 0.559470 0.900946 0.452753 0.042 Uiso 1 1 calc R U . . .
C4 C 0.5552(4) 0.6087(6) 0.4236(2) 0.0325(11) Uani 1 1 d . . . . .
H4A H 0.497210 0.499150 0.420309 0.039 Uiso 1 1 calc R U . . .
H4AB H 0.629322 0.577899 0.461923 0.039 Uiso 1 1 calc R U . . .
C5 C 0.5890(4) 0.6303(6) 0.3520(2) 0.0254(9) Uani 1 1 d . . . . .
H5A H 0.654411 0.728868 0.357472 0.030 Uiso 1 1 calc R U . . .
H5AB H 0.621359 0.504379 0.339808 0.030 Uiso 1 1 calc R U . . .
C6 C 0.3890(4) 0.5331(6) 0.2712(2) 0.0278(10) Uani 1 1 d . . . . .
H6A H 0.316131 0.585761 0.236424 0.033 Uiso 1 1 calc R U . . .
H6AB H 0.364259 0.488823 0.314143 0.033 Uiso 1 1 calc R U . . .
C7 C 0.4393(4) 0.3629(6) 0.2383(2) 0.0295(10) Uani 1 1 d . . . . .
H7A H 0.498025 0.288090 0.275672 0.035 Uiso 1 1 calc R U . . .
H7AB H 0.372781 0.274471 0.213675 0.035 Uiso 1 1 calc R U . . .
C8 C 0.5315(4) 0.3504(6) 0.1390(2) 0.0258(10) Uani 1 1 d . . . . .
H8 H 0.514370 0.215226 0.131509 0.031 Uiso 1 1 calc R U . . .
C9 C 0.5964(4) 0.4621(6) 0.0952(2) 0.0234(9) Uani 1 1 d . . . . .
C10 C 0.6342(3) 0.3853(6) 0.0386(2) 0.0257(10) Uani 1 1 d . . . . .
H10 H 0.623744 0.250461 0.027259 0.031 Uiso 1 1 calc R U . . .
C11 C 0.6878(4) 0.5083(7) -0.0014(2) 0.0298(10) Uani 1 1 d . . . . .
H11 H 0.714533 0.458747 -0.040720 0.036 Uiso 1 1 calc R U . . .
C12 C 0.7019(4) 0.7027(7) 0.0164(2) 0.0321(11) Uani 1 1 d . . . . .
H12 H 0.737456 0.789839 -0.010702 0.039 Uiso 1 1 calc R U . . .
C13 C 0.6630(4) 0.7695(6) 0.0749(2) 0.0285(10) Uani 1 1 d . . . . .
H13 H 0.673125 0.903750 0.087207 0.034 Uiso 1 1 calc R U . . .
N3 N 0.6123(3) 0.6533(5) 0.11410(18) 0.0228(8) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 N2 1.970(3) . ?
Cu1 N3 2.048(3) . ?
Cu1 N1 2.089(3) . ?
Cu1 Cl2 2.2397(11) . ?
Cu1 Cl1 2.5862(12) . ?
N1 C1 1.483(5) . ?
N1 C5 1.491(5) . ?
N1 C6 1.501(5) . ?
N2 C8 1.266(5) . ?
N2 C7 1.461(5) . ?
C1 C2 1.523(6) . ?
C2 C3 1.524(6) . ?
C3 C4 1.525(6) . ?
C4 C5 1.536(5) . ?
C6 C7 1.510(6) . ?
C8 C9 1.472(6) . ?
C9 N3 1.360(5) . ?
C9 C10 1.379(5) . ?
C10 C11 1.388(6) . ?
C11 C12 1.375(6) . ?
C12 C13 1.393(6) . ?
C13 N3 1.329(5) . ?

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
N2 Cu1 N3 79.22(13) . . ?
N2 Cu1 N1 81.97(13) . . ?
N3 Cu1 N1 159.75(13) . . ?
N2 Cu1 Cl2 156.90(10) . . ?
N3 Cu1 Cl2 96.91(9) . . ?
N1 Cu1 Cl2 97.46(9) . . ?
N2 Cu1 Cl1 100.43(10) . . ?
N3 Cu1 Cl1 94.56(9) . . ?
N1 Cu1 Cl1 96.15(9) . . ?
Cl2 Cu1 Cl1 102.59(4) . . ?
C1 N1 C5 109.1(3) . . ?
C1 N1 C6 110.9(3) . . ?
C5 N1 C6 112.8(3) . . ?
C1 N1 Cu1 112.2(2) . . ?
C5 N1 Cu1 108.4(2) . . ?
C6 N1 Cu1 103.4(2) . . ?
C8 N2 C7 124.5(3) . . ?
C8 N2 Cu1 118.5(3) . . ?
C7 N2 Cu1 116.8(3) . . ?
N1 C1 C2 113.9(3) . . ?
C1 C2 C3 110.4(3) . . ?
C2 C3 C4 110.4(4) . . ?
C3 C4 C5 111.0(4) . . ?
N1 C5 C4 113.1(3) . . ?
N1 C6 C7 109.9(3) . . ?
N2 C7 C6 106.2(3) . . ?
N2 C8 C9 115.5(4) . . ?
N3 C9 C10 122.2(4) . . ?
N3 C9 C8 113.5(3) . . ?
C10 C9 C8 124.2(4) . . ?
C9 C10 C11 118.9(4) . . ?
C12 C11 C10 119.2(4) . . ?
C11 C12 C13 118.7(4) . . ?
N3 C13 C12 122.8(4) . . ?
C13 N3 C9 118.1(4) . . ?
C13 N3 Cu1 128.7(3) . . ?
C9 N3 Cu1 113.2(3) . . ?

_refine_diff_density_max         0.853
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.155

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_tt_a
_database_code_depnum_ccdc_archive 'CCDC 1977266'
loop_
_audit_author_name
_audit_author_address
'Hyosun Lee'
;Kyungpook National University
South Korea
;
_audit_update_record             
;
2020-04-11 deposited with the CCDC.	2020-04-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H14 Cl2 Cu N2 O'
_chemical_formula_weight         312.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0021 0.0012 '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 0.0044 0.0024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0078 0.0044 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1177 0.1185 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3370 0.9703 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   19.134(4)
_cell_length_b                   8.7200(17)
_cell_length_c                   7.4760(15)
_cell_angle_alpha                90
_cell_angle_beta                 93.41(3)
_cell_angle_gamma                90
_cell_volume                     1245.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    32498
_cell_measurement_theta_min      0.35
_cell_measurement_theta_max      33.68

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_F_000             636
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.035
_exptl_absorpt_coefficient_mu    1.415
_shelx_estimated_absorpt_T_min   0.907
_shelx_estimated_absorpt_T_max   0.952
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.931
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'HKL3000 Scalepack'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.610
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19721
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.204
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_full        21.469
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measured_fraction_theta_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_point_group_measured_fraction_full 0.968
_reflns_number_total             5437
_reflns_number_gt                4893
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'PAL BL2D-SMDC Program'
_computing_cell_refinement       HKL3000sm
_computing_data_reduction        HKL3000sm
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  WinGX
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0681P)²+0.4729P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5437
_refine_ls_number_parameters     146
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0418
_refine_ls_wR_factor_ref         0.1215
_refine_ls_wR_factor_gt          0.1191
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.101
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.20012(2) 0.68099(2) 0.55169(2) 0.02092(7) Uani 1 1 d . . . . .
Cl1 Cl 0.12598(2) 0.83741(4) 0.39101(5) 0.02711(9) Uani 1 1 d . . . . .
Cl2 Cl 0.26246(2) 0.87680(4) 0.67923(5) 0.02690(9) Uani 1 1 d . . . . .
N1 N 0.14386(7) 0.49040(12) 0.48025(15) 0.01911(19) Uani 1 1 d . . . . .
N2 N 0.26787(7) 0.51448(14) 0.64701(16) 0.0209(2) Uani 1 1 d . . . . .
O1 O 0.49631(7) 0.51743(17) 0.75347(19) 0.0342(3) Uani 1 1 d . . . . .
C1 C 0.08019(8) 0.48278(15) 0.3966(2) 0.0240(3) Uani 1 1 d . . . . .
H1 H 0.058107 0.574991 0.355886 0.029 Uiso 1 1 calc R U . . .
C2 C 0.04512(9) 0.34396(17) 0.3672(2) 0.0273(3) Uani 1 1 d . . . . .
H2 H -0.000605 0.342033 0.310285 0.033 Uiso 1 1 calc R U . . .
C3 C 0.07786(10) 0.20939(17) 0.4221(2) 0.0290(3) Uani 1 1 d . . . . .
H3 H 0.054890 0.113651 0.403303 0.035 Uiso 1 1 calc R U . . .
C4 C 0.14477(9) 0.21540(16) 0.5052(2) 0.0261(3) Uani 1 1 d . . . . .
H4 H 0.168806 0.124243 0.541597 0.031 Uiso 1 1 calc R U . . .
C5 C 0.17542(8) 0.35789(15) 0.53349(18) 0.0201(2) Uani 1 1 d . . . . .
C6 C 0.24456(8) 0.37852(16) 0.62459(19) 0.0230(2) Uani 1 1 d . . . . .
H6 H 0.271442 0.292637 0.666043 0.028 Uiso 1 1 calc R U . . .
C7 C 0.33793(8) 0.53668(18) 0.73384(19) 0.0240(2) Uani 1 1 d . . . . .
H7A H 0.354414 0.439737 0.790914 0.029 Uiso 1 1 calc R U . . .
H7B H 0.336091 0.615901 0.828293 0.029 Uiso 1 1 calc R U . . .
C8 C 0.38844(9) 0.5863(2) 0.5956(2) 0.0300(3) Uani 1 1 d . . . . .
H8A H 0.396996 0.498639 0.515663 0.036 Uiso 1 1 calc R U . . .
H8B H 0.366520 0.669265 0.521180 0.036 Uiso 1 1 calc R U . . .
C9 C 0.45764(10) 0.6425(2) 0.6782(3) 0.0316(3) Uani 1 1 d . . . . .
H9A H 0.484573 0.692670 0.585446 0.038 Uiso 1 1 calc R U . . .
H9B H 0.449418 0.718996 0.772488 0.038 Uiso 1 1 calc R U . . .
C10 C 0.56048(11) 0.5667(3) 0.8387(3) 0.0402(4) Uani 1 1 d . . . . .
H10A H 0.584613 0.634490 0.757946 0.060 Uiso 1 1 calc R U . . .
H10B H 0.589981 0.477388 0.868567 0.060 Uiso 1 1 calc R U . . .
H10C H 0.551240 0.622436 0.948710 0.060 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 2.0342(12) . ?
Cu1 N2 2.0461(13) . ?
Cu1 Cl2 2.2609(5) . ?
Cu1 Cl1 2.2613(6) . ?
N1 C1 1.337(2) . ?
N1 C5 1.3526(17) . ?
N2 C6 1.2742(18) . ?
N2 C7 1.467(2) . ?
O1 C9 1.416(2) . ?
O1 C10 1.416(3) . ?
C1 C2 1.395(2) . ?
C2 C3 1.381(2) . ?
C3 C4 1.390(2) . ?
C4 C5 1.385(2) . ?
C5 C6 1.463(2) . ?
C7 C8 1.520(2) . ?
C8 C9 1.509(3) . ?

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 N2 79.99(5) . . ?
N1 Cu1 Cl2 170.20(3) . . ?
N2 Cu1 Cl2 94.68(4) . . ?
N1 Cu1 Cl1 92.74(4) . . ?
N2 Cu1 Cl1 167.83(4) . . ?
Cl2 Cu1 Cl1 93.85(2) . . ?
C1 N1 C5 118.26(12) . . ?
C1 N1 Cu1 128.06(9) . . ?
C5 N1 Cu1 113.61(10) . . ?
C6 N2 C7 118.97(13) . . ?
C6 N2 Cu1 113.88(11) . . ?
C7 N2 Cu1 127.14(10) . . ?
C9 O1 C10 111.33(17) . . ?
N1 C1 C2 122.21(13) . . ?
C3 C2 C1 119.01(16) . . ?
C2 C3 C4 119.35(14) . . ?
C5 C4 C3 118.19(14) . . ?
N1 C5 C4 122.95(14) . . ?
N1 C5 C6 114.05(12) . . ?
C4 C5 C6 122.99(13) . . ?
N2 C6 C5 118.39(12) . . ?
N2 C7 C8 109.75(12) . . ?
C9 C8 C7 113.08(13) . . ?
O1 C9 C8 109.75(16) . . ?

_refine_diff_density_max         0.813
_refine_diff_density_min         -1.418
_refine_diff_density_rms         0.151

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_[LGCuCl2]
_database_code_depnum_ccdc_archive 'CCDC 1977265'
loop_
_audit_author_name
_audit_author_address
'Hyosun Lee'
;Kyungpook National University
South Korea
;
_audit_update_record             
;
2020-03-26 deposited with the CCDC.	2020-04-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C11 H17 Cl2 Cu N3'
_chemical_formula_weight         325.71

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0021 0.0012 '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 0.0044 0.0024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1177 0.1185 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3370 0.9703 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   7.2550(15)
_cell_length_b                   8.9600(18)
_cell_length_c                   11.553(2)
_cell_angle_alpha                96.81(3)
_cell_angle_beta                 102.83(3)
_cell_angle_gamma                113.02(3)
_cell_volume                     656.0(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    21761
_cell_measurement_theta_min      0.35
_cell_measurement_theta_max      33.68

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_F_000             334
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.035
_exptl_absorpt_coefficient_mu    1.344
_shelx_estimated_absorpt_T_min   0.948
_shelx_estimated_absorpt_T_max   0.954
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.945
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'HKL3000sm Scalepack'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.610
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11940
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.594
_diffrn_reflns_theta_max         33.566
_diffrn_reflns_theta_full        21.469
_diffrn_measured_fraction_theta_max 0.746
_diffrn_measured_fraction_theta_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.746
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.746
_diffrn_reflns_point_group_measured_fraction_full 0.954
_reflns_number_total             6098
_reflns_number_gt                4699
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'PAL BL2D-SMDC Program'
_computing_cell_refinement       HKL3000sm
_computing_data_reduction        HKL3000sm
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  WinGX
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0999P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.117(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6098
_refine_ls_number_parameters     223
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0519
_refine_ls_wR_factor_ref         0.1532
_refine_ls_wR_factor_gt          0.1399
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.23343(4) 0.39069(3) 0.26115(2) 0.01323(9) Uani 1 1 d . . . . .
Cl1 Cl -0.07228(8) 0.21919(7) 0.08304(4) 0.01780(11) Uani 1 1 d . . . . .
Cl2 Cl 0.15647(9) 0.59436(7) 0.34698(5) 0.01908(12) Uani 1 1 d . . . . .
N1 N 0.4258(3) 0.5602(3) 0.18382(16) 0.0159(3) Uani 1 1 d . . . . .
N2 N 0.4179(3) 0.2784(3) 0.22760(16) 0.0154(3) Uani 1 1 d . . . . .
N3 N 0.1338(3) 0.2440(3) 0.38519(16) 0.0167(3) Uani 1 1 d . . . . .
C1 C 0.4133(4) 0.6939(3) 0.1522(2) 0.0177(4) Uani 1 1 d . . . . .
H2 H 0.308(6) 0.722(5) 0.169(3) 0.020(8) Uiso 1 1 d . . . . .
C2 C 0.5604(4) 0.8019(3) 0.1042(2) 0.0185(4) Uani 1 1 d . . . . .
H3 H 0.549(6) 0.899(5) 0.082(3) 0.020(8) Uiso 1 1 d . . . . .
C3 C 0.7264(4) 0.7675(3) 0.08976(19) 0.0191(4) Uani 1 1 d . . . . .
H13 H 0.820(6) 0.839(5) 0.056(3) 0.025(9) Uiso 1 1 d . . . . .
C4 C 0.7394(3) 0.6269(3) 0.12132(19) 0.0182(4) Uani 1 1 d . . . . .
H12 H 0.853(5) 0.595(4) 0.115(3) 0.015(7) Uiso 1 1 d . . . . .
C5 C 0.5854(3) 0.5253(3) 0.16667(18) 0.0148(3) Uani 1 1 d . . . . .
C6 C 0.5710(3) 0.3656(3) 0.19019(18) 0.0162(4) Uani 1 1 d . . . . .
H15 H 0.661(6) 0.329(4) 0.173(3) 0.015(7) Uiso 1 1 d . . . . .
C7 C 0.3790(4) 0.1081(3) 0.2327(2) 0.0192(4) Uani 1 1 d . . . . .
H14 H 0.272(7) 0.044(5) 0.172(4) 0.031(10) Uiso 1 1 d . . . . .
H7 H 0.493(6) 0.083(5) 0.221(3) 0.020(8) Uiso 1 1 d . . . . .
C8 C 0.3306(4) 0.0687(3) 0.3501(2) 0.0212(4) Uani 1 1 d . . . . .
H6 H 0.314(6) -0.044(5) 0.353(4) 0.030(10) Uiso 1 1 d . . . . .
H8 H 0.438(6) 0.145(5) 0.419(3) 0.022(9) Uiso 1 1 d . . . . .
C9 C 0.1272(4) 0.0758(3) 0.3567(2) 0.0200(4) Uani 1 1 d . . . . .
H5 H 0.034(5) 0.032(4) 0.288(3) 0.009(7) Uiso 1 1 d . . . . .
H9 H 0.090(6) 0.022(4) 0.425(3) 0.020(8) Uiso 1 1 d . . . . .
C10 C 0.2681(4) 0.3323(3) 0.5118(2) 0.0209(4) Uani 1 1 d . . . . .
H17 H 0.222(8) 0.259(6) 0.562(5) 0.052(13) Uiso 1 1 d . . . . .
H1 H 0.256(6) 0.434(5) 0.531(4) 0.028(9) Uiso 1 1 d . . . . .
H10 H 0.412(5) 0.353(4) 0.523(3) 0.016(8) Uiso 1 1 d . . . . .
C11 C -0.0839(4) 0.2173(3) 0.3792(2) 0.0203(4) Uani 1 1 d . . . . .
H16 H -0.125(6) 0.144(5) 0.433(4) 0.028(9) Uiso 1 1 d . . . . .
H4 H -0.176(6) 0.160(5) 0.294(4) 0.025(9) Uiso 1 1 d . . . . .
H11 H -0.089(6) 0.325(5) 0.399(3) 0.019(8) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 N2 2.0361(19) . ?
Cu1 N1 2.067(2) . ?
Cu1 N3 2.114(2) . ?
Cu1 Cl2 2.2887(8) . ?
Cu1 Cl1 2.4641(15) . ?
N1 C1 1.323(3) . ?
N1 C5 1.359(3) . ?
N2 C6 1.283(3) . ?
N2 C7 1.451(3) . ?
N3 C9 1.484(3) . ?
N3 C10 1.485(3) . ?
N3 C11 1.486(3) . ?
C1 C2 1.401(3) . ?
C1 H2 0.95(3) . ?
C2 C3 1.393(3) . ?
C2 H3 0.97(4) . ?
C3 C4 1.384(4) . ?
C3 H13 0.93(4) . ?
C4 C5 1.389(3) . ?
C4 H12 0.99(3) . ?
C5 C6 1.456(3) . ?
C6 H15 0.89(3) . ?
C7 C8 1.521(3) . ?
C7 H14 0.86(4) . ?
C7 H7 0.97(3) . ?
C8 C9 1.521(3) . ?
C8 H6 0.97(4) . ?
C8 H8 0.94(4) . ?
C9 H5 0.85(3) . ?
C9 H9 1.01(3) . ?
C10 H17 0.94(5) . ?
C10 H1 0.96(4) . ?
C10 H10 0.96(3) . ?
C11 H16 0.96(4) . ?
C11 H4 1.00(4) . ?
C11 H11 0.98(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
N2 Cu1 N1 79.20(8) . . ?
N2 Cu1 N3 92.33(8) . . ?
N1 Cu1 N3 160.76(8) . . ?
N2 Cu1 Cl2 156.80(6) . . ?
N1 Cu1 Cl2 89.52(6) . . ?
N3 Cu1 Cl2 91.93(6) . . ?
N2 Cu1 Cl1 96.74(6) . . ?
N1 Cu1 Cl1 101.66(6) . . ?
N3 Cu1 Cl1 96.44(6) . . ?
Cl2 Cu1 Cl1 105.42(4) . . ?
C1 N1 C5 118.43(19) . . ?
C1 N1 Cu1 128.66(14) . . ?
C5 N1 Cu1 112.91(16) . . ?
C6 N2 C7 119.22(19) . . ?
C6 N2 Cu1 114.99(17) . . ?
C7 N2 Cu1 125.57(14) . . ?
C9 N3 C10 109.9(2) . . ?
C9 N3 C11 106.16(19) . . ?
C10 N3 C11 107.77(17) . . ?
C9 N3 Cu1 113.71(13) . . ?
C10 N3 Cu1 110.44(15) . . ?
C11 N3 Cu1 108.57(15) . . ?
N1 C1 C2 122.5(2) . . ?
N1 C1 H2 118(2) . . ?
C2 C1 H2 119(2) . . ?
C3 C2 C1 118.8(2) . . ?
C3 C2 H3 120(2) . . ?
C1 C2 H3 121(2) . . ?
C4 C3 C2 119.2(2) . . ?
C4 C3 H13 124(2) . . ?
C2 C3 H13 117(2) . . ?
C3 C4 C5 118.3(2) . . ?
C3 C4 H12 124(2) . . ?
C5 C4 H12 118(2) . . ?
N1 C5 C4 122.8(2) . . ?
N1 C5 C6 114.18(18) . . ?
C4 C5 C6 122.84(19) . . ?
N2 C6 C5 117.89(19) . . ?
N2 C6 H15 123(2) . . ?
C5 C6 H15 119(2) . . ?
N2 C7 C8 111.46(19) . . ?
N2 C7 H14 107(3) . . ?
C8 C7 H14 109(3) . . ?
N2 C7 H7 112(2) . . ?
C8 C7 H7 112(2) . . ?
H14 C7 H7 105(3) . . ?
C9 C8 C7 111.5(2) . . ?
C9 C8 H6 107(2) . . ?
C7 C8 H6 109(2) . . ?
C9 C8 H8 108(2) . . ?
C7 C8 H8 111(2) . . ?
H6 C8 H8 110(3) . . ?
N3 C9 C8 116.6(2) . . ?
N3 C9 H5 102(2) . . ?
C8 C9 H5 111(2) . . ?
N3 C9 H9 107(2) . . ?
C8 C9 H9 106(2) . . ?
H5 C9 H9 115(3) . . ?
N3 C10 H17 106(3) . . ?
N3 C10 H1 108(2) . . ?
H17 C10 H1 114(4) . . ?
N3 C10 H10 113(2) . . ?
H17 C10 H10 105(3) . . ?
H1 C10 H10 111(3) . . ?
N3 C11 H16 105(2) . . ?
N3 C11 H4 109(2) . . ?
H16 C11 H4 109(3) . . ?
N3 C11 H11 110(2) . . ?
H16 C11 H11 116(3) . . ?
H4 C11 H11 108(3) . . ?

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
C5 N1 C1 C2 -1.3(3) . . . . ?
Cu1 N1 C1 C2 177.65(16) . . . . ?
N1 C1 C2 C3 -0.3(3) . . . . ?
C1 C2 C3 C4 1.0(3) . . . . ?
C2 C3 C4 C5 -0.1(3) . . . . ?
C1 N1 C5 C4 2.2(3) . . . . ?
Cu1 N1 C5 C4 -176.88(16) . . . . ?
C1 N1 C5 C6 -172.87(19) . . . . ?
Cu1 N1 C5 C6 8.0(2) . . . . ?
C3 C4 C5 N1 -1.5(3) . . . . ?
C3 C4 C5 C6 173.2(2) . . . . ?
C7 N2 C6 C5 169.96(19) . . . . ?
Cu1 N2 C6 C5 -4.9(2) . . . . ?
N1 C5 C6 N2 -2.2(3) . . . . ?
C4 C5 C6 N2 -177.3(2) . . . . ?
C6 N2 C7 C8 136.7(2) . . . . ?
Cu1 N2 C7 C8 -48.9(3) . . . . ?
N2 C7 C8 C9 64.9(3) . . . . ?
C10 N3 C9 C8 -66.9(2) . . . . ?
C11 N3 C9 C8 176.77(19) . . . . ?
Cu1 N3 C9 C8 57.5(2) . . . . ?
C7 C8 C9 N3 -75.3(3) . . . . ?

_refine_diff_density_max         1.197
_refine_diff_density_min         -2.163
_refine_diff_density_rms         0.198

# start Validation Reply Form
_vrf_PLAT029_LGCuCl2             
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.954 Why?  
RESPONSE: To get the diffraction data for small crystal, we used
synchrotron radiation that has one rotation axis for diffraction data
collection. Due to the low symmetry of this crystal (Triclinic P-1),
the diffraction data collection using single rotational axis (omega scan)
from synchrotron radiation can gives 95.4% of data completeness.
;
_vrf_PLAT250_LGCuCl2             
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        4.6 Note  
RESPONSE:  This is a minor deviation.
No obvious source of error in the model was discovered.
;
# end Validation Reply Form
