# Electronic Supplementary Material (ESI) for Chemical Communications.
# 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_exp_4389
_database_code_depnum_ccdc_archive 'CCDC 2011181'
loop_
_audit_author_name
_audit_author_address
'Mingjun Xia'
;Technical Institute of Physics and Chemistry, CAS
China
;
_audit_update_record             
;
2020-06-22 deposited with the CCDC.	2020-09-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 Cl Cu3 K4 N6 O6'
_chemical_formula_weight         634.59

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'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   P-3m1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'

_cell_length_a                   11.1833(9)
_cell_length_b                   11.1833(9)
_cell_length_c                   3.6304(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     393.21(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.680
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             306
_exptl_absorpt_coefficient_mu    5.290
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3866
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_sigmaI/netI    0.0147
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_theta_min         3.64
_diffrn_reflns_theta_max         26.33
_reflns_number_total             317
_reflns_number_gt                274
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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     
'calc w=1/[σ²(Fo²)+(0.0513P)²+0.3824P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   none
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         317
_refine_ls_number_parameters     31
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0335
_refine_ls_wR_factor_ref         0.0934
_refine_ls_wR_factor_gt          0.0893
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.091
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.0000 0.5000 0.0000 0.0446(4) Uani 1 4 d S . .
K1 K 0.0000 0.76381(16) 0.5000 0.0806(8) Uani 0.67 2 d SP . .
Cl1 Cl 0.0000 1.0000 0.0000 0.0443(6) Uani 1 12 d S . .
C1 C 0.2637(2) 0.7363(2) -0.0002(11) 0.0458(11) Uani 1 2 d S . .
O1 O 0.19916(18) 0.80084(18) -0.0002(11) 0.0632(10) Uani 1 2 d S . .
N1 N -0.1921(4) 0.40394(18) -0.0001(10) 0.0420(8) Uani 1 2 d S . .


_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 1.861(3) 7_565 ?
Cu1 N1 1.861(3) . ?
Cu1 K1 3.4639(15) . ?
Cu1 K1 3.4639(15) 7_565 ?
Cu1 K1 3.4639(15) 1_554 ?
Cu1 K1 3.4639(15) 7_566 ?
K1 K1 2.6414(18) 9_666 ?
K1 K1 2.6414(18) 8_456 ?
K1 O1 2.739(3) 8_455 ?
K1 O1 2.739(3) 1_556 ?
K1 O1 2.740(3) . ?
K1 O1 2.740(3) 8_456 ?
K1 Cl1 3.2050(15) 1_556 ?
K1 Cl1 3.2050(15) . ?
K1 Cu1 3.4639(15) 1_556 ?
K1 K1 3.6304(4) 1_556 ?
K1 K1 3.6304(4) 1_554 ?
Cl1 K1 3.2050(15) 2_675 ?
Cl1 K1 3.2050(15) 8_455 ?
Cl1 K1 3.2050(15) 9_666 ?
Cl1 K1 3.2050(15) 7_576 ?
Cl1 K1 3.2050(15) 3_464 ?
Cl1 K1 3.2050(15) 2_674 ?
Cl1 K1 3.2050(15) 1_554 ?
Cl1 K1 3.2050(15) 9_665 ?
Cl1 K1 3.2050(15) 7_575 ?
Cl1 K1 3.2050(15) 3_465 ?
Cl1 K1 3.2050(15) 8_456 ?
C1 O1 1.251(6) . ?
C1 N1 1.358(3) 9_665 ?
C1 N1 1.358(3) 7_565 ?
O1 K1 2.739(3) 1_554 ?
O1 K1 2.739(3) 9_665 ?
O1 K1 2.740(3) 9_666 ?
N1 C1 1.358(3) 8_455 ?
N1 C1 1.358(3) 7_565 ?

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 N1 180.0(2) 7_565 . ?
N1 Cu1 K1 90.00(6) 7_565 . ?
N1 Cu1 K1 90.00(6) . . ?
N1 Cu1 K1 90.00(6) 7_565 7_565 ?
N1 Cu1 K1 90.00(6) . 7_565 ?
K1 Cu1 K1 180.00(3) . 7_565 ?
N1 Cu1 K1 90.00(6) 7_565 1_554 ?
N1 Cu1 K1 90.00(6) . 1_554 ?
K1 Cu1 K1 63.21(3) . 1_554 ?
K1 Cu1 K1 116.79(3) 7_565 1_554 ?
N1 Cu1 K1 90.00(6) 7_565 7_566 ?
N1 Cu1 K1 90.00(6) . 7_566 ?
K1 Cu1 K1 116.79(3) . 7_566 ?
K1 Cu1 K1 63.21(3) 7_565 7_566 ?
K1 Cu1 K1 180.00(3) 1_554 7_566 ?
K1 K1 K1 120.0 9_666 8_456 ?
K1 K1 O1 137.53(8) 9_666 8_455 ?
K1 K1 O1 61.17(5) 8_456 8_455 ?
K1 K1 O1 61.17(5) 9_666 1_556 ?
K1 K1 O1 137.53(8) 8_456 1_556 ?
O1 K1 O1 150.41(13) 8_455 1_556 ?
K1 K1 O1 61.18(5) 9_666 . ?
K1 K1 O1 137.50(8) 8_456 . ?
O1 K1 O1 89.51(3) 8_455 . ?
O1 K1 O1 83.00(8) 1_556 . ?
K1 K1 O1 137.50(8) 9_666 8_456 ?
K1 K1 O1 61.18(5) 8_456 8_456 ?
O1 K1 O1 83.00(8) 8_455 8_456 ?
O1 K1 O1 89.51(3) 1_556 8_456 ?
O1 K1 O1 150.42(13) . 8_456 ?
K1 K1 Cl1 65.665(6) 9_666 1_556 ?
K1 K1 Cl1 65.665(5) 8_456 1_556 ?
O1 K1 Cl1 125.85(5) 8_455 1_556 ?
O1 K1 Cl1 80.52(7) 1_556 1_556 ?
O1 K1 Cl1 125.86(5) . 1_556 ?
O1 K1 Cl1 80.50(7) 8_456 1_556 ?
K1 K1 Cl1 65.665(6) 9_666 . ?
K1 K1 Cl1 65.665(6) 8_456 . ?
O1 K1 Cl1 80.52(7) 8_455 . ?
O1 K1 Cl1 125.85(5) 1_556 . ?
O1 K1 Cl1 80.50(7) . . ?
O1 K1 Cl1 125.86(5) 8_456 . ?
Cl1 K1 Cl1 68.99(4) 1_556 . ?
K1 K1 Cu1 115.204(5) 9_666 . ?
K1 K1 Cu1 115.204(5) 8_456 . ?
O1 K1 Cu1 55.62(4) 8_455 . ?
O1 K1 Cu1 97.45(8) 1_556 . ?
O1 K1 Cu1 55.62(4) . . ?
O1 K1 Cu1 97.47(8) 8_456 . ?
Cl1 K1 Cu1 177.11(3) 1_556 . ?
Cl1 K1 Cu1 113.900(8) . . ?
K1 K1 Cu1 115.204(4) 9_666 1_556 ?
K1 K1 Cu1 115.204(5) 8_456 1_556 ?
O1 K1 Cu1 97.45(8) 8_455 1_556 ?
O1 K1 Cu1 55.62(5) 1_556 1_556 ?
O1 K1 Cu1 97.47(8) . 1_556 ?
O1 K1 Cu1 55.62(4) 8_456 1_556 ?
Cl1 K1 Cu1 113.900(8) 1_556 1_556 ?
Cl1 K1 Cu1 177.11(3) . 1_556 ?
Cu1 K1 Cu1 63.21(3) . 1_556 ?
K1 K1 K1 90.0 9_666 1_556 ?
K1 K1 K1 90.0 8_456 1_556 ?
O1 K1 K1 131.49(7) 8_455 1_556 ?
O1 K1 K1 48.51(7) 1_556 1_556 ?
O1 K1 K1 131.51(7) . 1_556 ?
O1 K1 K1 48.49(7) 8_456 1_556 ?
Cl1 K1 K1 55.503(18) 1_556 1_556 ?
Cl1 K1 K1 124.497(18) . 1_556 ?
Cu1 K1 K1 121.603(16) . 1_556 ?
Cu1 K1 K1 58.397(16) 1_556 1_556 ?
K1 K1 K1 90.0 9_666 1_554 ?
K1 K1 K1 90.0 8_456 1_554 ?
O1 K1 K1 48.51(7) 8_455 1_554 ?
O1 K1 K1 131.49(7) 1_556 1_554 ?
O1 K1 K1 48.49(7) . 1_554 ?
O1 K1 K1 131.51(7) 8_456 1_554 ?
Cl1 K1 K1 124.497(18) 1_556 1_554 ?
Cl1 K1 K1 55.503(18) . 1_554 ?
Cu1 K1 K1 58.397(16) . 1_554 ?
Cu1 K1 K1 121.603(16) 1_556 1_554 ?
K1 K1 K1 180.00(11) 1_556 1_554 ?
K1 Cl1 K1 180.0 2_675 8_455 ?
K1 Cl1 K1 48.671(11) 2_675 9_666 ?
K1 Cl1 K1 131.329(11) 8_455 9_666 ?
K1 Cl1 K1 48.671(11) 2_675 7_576 ?
K1 Cl1 K1 131.329(11) 8_455 7_576 ?
K1 Cl1 K1 91.08(3) 9_666 7_576 ?
K1 Cl1 K1 131.329(11) 2_675 3_464 ?
K1 Cl1 K1 48.671(11) 8_455 3_464 ?
K1 Cl1 K1 180.0 9_666 3_464 ?
K1 Cl1 K1 88.92(3) 7_576 3_464 ?
K1 Cl1 K1 68.99(4) 2_675 2_674 ?
K1 Cl1 K1 111.01(4) 8_455 2_674 ?
K1 Cl1 K1 88.92(3) 9_666 2_674 ?
K1 Cl1 K1 88.92(3) 7_576 2_674 ?
K1 Cl1 K1 91.08(3) 3_464 2_674 ?
K1 Cl1 K1 131.329(11) 2_675 1_554 ?
K1 Cl1 K1 48.671(11) 8_455 1_554 ?
K1 Cl1 K1 88.92(3) 9_666 1_554 ?
K1 Cl1 K1 180.0 7_576 1_554 ?
K1 Cl1 K1 91.08(3) 3_464 1_554 ?
K1 Cl1 K1 91.08(3) 2_674 1_554 ?
K1 Cl1 K1 88.92(3) 2_675 9_665 ?
K1 Cl1 K1 91.08(3) 8_455 9_665 ?
K1 Cl1 K1 68.99(4) 9_666 9_665 ?
K1 Cl1 K1 131.329(12) 7_576 9_665 ?
K1 Cl1 K1 111.01(4) 3_464 9_665 ?
K1 Cl1 K1 48.671(11) 2_674 9_665 ?
K1 Cl1 K1 48.671(11) 1_554 9_665 ?
K1 Cl1 K1 88.92(3) 2_675 7_575 ?
K1 Cl1 K1 91.08(3) 8_455 7_575 ?
K1 Cl1 K1 131.329(12) 9_666 7_575 ?
K1 Cl1 K1 68.99(4) 7_576 7_575 ?
K1 Cl1 K1 48.671(11) 3_464 7_575 ?
K1 Cl1 K1 48.671(11) 2_674 7_575 ?
K1 Cl1 K1 111.01(4) 1_554 7_575 ?
K1 Cl1 K1 91.08(3) 9_665 7_575 ?
K1 Cl1 K1 91.08(3) 2_675 3_465 ?
K1 Cl1 K1 88.92(3) 8_455 3_465 ?
K1 Cl1 K1 111.01(4) 9_666 3_465 ?
K1 Cl1 K1 48.671(11) 7_576 3_465 ?
K1 Cl1 K1 68.99(4) 3_464 3_465 ?
K1 Cl1 K1 131.329(11) 2_674 3_465 ?
K1 Cl1 K1 131.329(11) 1_554 3_465 ?
K1 Cl1 K1 180.0 9_665 3_465 ?
K1 Cl1 K1 88.92(3) 7_575 3_465 ?
K1 Cl1 K1 91.08(3) 2_675 . ?
K1 Cl1 K1 88.92(3) 8_455 . ?
K1 Cl1 K1 48.671(11) 9_666 . ?
K1 Cl1 K1 111.01(4) 7_576 . ?
K1 Cl1 K1 131.329(12) 3_464 . ?
K1 Cl1 K1 131.329(11) 2_674 . ?
K1 Cl1 K1 68.99(4) 1_554 . ?
K1 Cl1 K1 88.92(3) 9_665 . ?
K1 Cl1 K1 180.00(4) 7_575 . ?
K1 Cl1 K1 91.08(3) 3_465 . ?
K1 Cl1 K1 111.01(4) 2_675 8_456 ?
K1 Cl1 K1 68.99(4) 8_455 8_456 ?
K1 Cl1 K1 91.08(3) 9_666 8_456 ?
K1 Cl1 K1 91.08(3) 7_576 8_456 ?
K1 Cl1 K1 88.92(3) 3_464 8_456 ?
K1 Cl1 K1 180.0 2_674 8_456 ?
K1 Cl1 K1 88.92(3) 1_554 8_456 ?
K1 Cl1 K1 131.329(11) 9_665 8_456 ?
K1 Cl1 K1 131.329(11) 7_575 8_456 ?
K1 Cl1 K1 48.671(11) 3_465 8_456 ?
K1 Cl1 K1 48.671(11) . 8_456 ?
O1 C1 N1 119.3(2) . 9_665 ?
O1 C1 N1 119.3(2) . 7_565 ?
N1 C1 N1 121.4(4) 9_665 7_565 ?
C1 O1 K1 125.0(3) . 1_554 ?
C1 O1 K1 125.0(3) . 9_665 ?
K1 O1 K1 57.66(9) 1_554 9_665 ?
C1 O1 K1 125.0(3) . 9_666 ?
K1 O1 K1 110.06(13) 1_554 9_666 ?
K1 O1 K1 83.00(8) 9_665 9_666 ?
C1 O1 K1 125.0(3) . . ?
K1 O1 K1 83.00(8) 1_554 . ?
K1 O1 K1 110.06(13) 9_665 . ?
K1 O1 K1 57.63(9) 9_666 . ?
C1 N1 C1 118.6(4) 8_455 7_565 ?
C1 N1 Cu1 120.7(2) 8_455 . ?
C1 N1 Cu1 120.7(2) 7_565 . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.33
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.130
####################################################################### 
# 
# 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_exp_4529
_database_code_depnum_ccdc_archive 'CCDC 2011182'
loop_
_audit_author_name
_audit_author_address
'Mingjun Xia'
;Technical Institute of Physics and Chemistry, CAS
China
;
_audit_update_record             
;
2020-06-22 deposited with the CCDC.	2020-09-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 Br Cu3 K4 N6 O6'
_chemical_formula_weight         679.05

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'
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'
K K 0.2009 0.2494 '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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'

_cell_length_a                   11.2089(8)
_cell_length_b                   11.2089(8)
_cell_length_c                   3.7195(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     404.71(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.786
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             324
_exptl_absorpt_coefficient_mu    7.443
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4134
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0187
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_theta_min         4.20
_diffrn_reflns_theta_max         26.35
_reflns_number_total             319
_reflns_number_gt                246
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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     
'calc w=1/[σ²(Fo²)+(0.0927P)²+1.6722P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         319
_refine_ls_number_parameters     30
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0563
_refine_ls_wR_factor_ref         0.1733
_refine_ls_wR_factor_gt          0.1641
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_restrained_S_all      1.287
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.0000 0.5000 0.0000 0.0362(7) Uani 1 4 d S . .
K1 K 0.0000 0.7549(4) 0.5000 0.091(2) Uani 0.67 2 d SPU . .
Br1 Br 0.0000 1.0000 0.0000 0.0444(9) Uani 1 12 d S . .
C1 C 0.2635(6) 0.7365(6) 0.000(2) 0.043(3) Uani 1 2 d S . .
O1 O 0.1992(4) 0.8008(4) -0.002(3) 0.057(2) Uani 1 2 d S . .
N1 N -0.1936(8) 0.4032(4) 0.000(2) 0.0377(19) Uani 1 2 d S . .


_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 1.879(8) 7_565 ?
Cu1 N1 1.879(8) . ?
Cu1 K1 3.409(4) . ?
Cu1 K1 3.409(4) 7_565 ?
Cu1 K1 3.409(4) 1_554 ?
Cu1 K1 3.409(4) 7_566 ?
K1 O1 2.746(8) 8_455 ?
K1 O1 2.746(8) 1_556 ?
K1 K1 2.747(4) 9_666 ?
K1 K1 2.747(4) 8_456 ?
K1 O1 2.754(8) 8_456 ?
K1 O1 2.754(8) . ?
K1 Br1 3.318(4) 1_556 ?
K1 Br1 3.318(4) . ?
K1 Cu1 3.409(4) 1_556 ?
K1 K1 3.7195(4) 1_556 ?
K1 K1 3.7195(4) 1_554 ?
Br1 K1 3.318(4) 2_675 ?
Br1 K1 3.318(4) 8_455 ?
Br1 K1 3.318(4) 9_666 ?
Br1 K1 3.318(4) 7_576 ?
Br1 K1 3.318(4) 3_464 ?
Br1 K1 3.318(4) 1_554 ?
Br1 K1 3.318(4) 3_465 ?
Br1 K1 3.318(4) 2_674 ?
Br1 K1 3.318(4) 8_456 ?
Br1 K1 3.318(4) 7_575 ?
Br1 K1 3.318(4) 9_665 ?
C1 O1 1.247(12) . ?
C1 N1 1.357(7) 9_665 ?
C1 N1 1.357(7) 7_565 ?
O1 K1 2.746(8) 1_554 ?
O1 K1 2.746(8) 9_665 ?
O1 K1 2.754(8) 9_666 ?
N1 C1 1.357(7) 8_455 ?
N1 C1 1.357(7) 7_565 ?

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 N1 180.0(3) 7_565 . ?
N1 Cu1 K1 90.00(13) 7_565 . ?
N1 Cu1 K1 90.00(13) . . ?
N1 Cu1 K1 90.00(13) 7_565 7_565 ?
N1 Cu1 K1 90.00(13) . 7_565 ?
K1 Cu1 K1 180.0 . 7_565 ?
N1 Cu1 K1 90.00(13) 7_565 1_554 ?
N1 Cu1 K1 90.00(13) . 1_554 ?
K1 Cu1 K1 66.12(8) . 1_554 ?
K1 Cu1 K1 113.88(8) 7_565 1_554 ?
N1 Cu1 K1 90.00(13) 7_565 7_566 ?
N1 Cu1 K1 90.00(13) . 7_566 ?
K1 Cu1 K1 113.88(8) . 7_566 ?
K1 Cu1 K1 66.12(8) 7_565 7_566 ?
K1 Cu1 K1 180.0 1_554 7_566 ?
O1 K1 O1 154.6(3) 8_455 1_556 ?
O1 K1 K1 136.03(18) 8_455 9_666 ?
O1 K1 K1 59.99(11) 1_556 9_666 ?
O1 K1 K1 59.99(11) 8_455 8_456 ?
O1 K1 K1 136.03(18) 1_556 8_456 ?
K1 K1 K1 120.0 9_666 8_456 ?
O1 K1 O1 85.11(15) 8_455 8_456 ?
O1 K1 O1 89.39(6) 1_556 8_456 ?
K1 K1 O1 135.86(18) 9_666 8_456 ?
K1 K1 O1 60.08(11) 8_456 8_456 ?
O1 K1 O1 89.39(6) 8_455 . ?
O1 K1 O1 85.11(15) 1_556 . ?
K1 K1 O1 60.08(11) 9_666 . ?
K1 K1 O1 135.86(18) 8_456 . ?
O1 K1 O1 154.7(3) 8_456 . ?
O1 K1 Br1 124.07(13) 8_455 1_556 ?
O1 K1 Br1 78.65(16) 1_556 1_556 ?
K1 K1 Br1 65.540(13) 9_666 1_556 ?
K1 K1 Br1 65.541(13) 8_456 1_556 ?
O1 K1 Br1 78.55(16) 8_456 1_556 ?
O1 K1 Br1 124.12(13) . 1_556 ?
O1 K1 Br1 78.65(16) 8_455 . ?
O1 K1 Br1 124.07(13) 1_556 . ?
K1 K1 Br1 65.541(13) 9_666 . ?
K1 K1 Br1 65.541(13) 8_456 . ?
O1 K1 Br1 124.12(13) 8_456 . ?
O1 K1 Br1 78.55(16) . . ?
Br1 K1 Br1 68.19(8) 1_556 . ?
O1 K1 Cu1 56.48(10) 8_455 . ?
O1 K1 Cu1 100.62(19) 1_556 . ?
K1 K1 Cu1 114.775(12) 9_666 . ?
K1 K1 Cu1 114.775(13) 8_456 . ?
O1 K1 Cu1 100.73(19) 8_456 . ?
O1 K1 Cu1 56.43(10) . . ?
Br1 K1 Cu1 178.96(8) 1_556 . ?
Br1 K1 Cu1 112.844(7) . . ?
O1 K1 Cu1 100.62(19) 8_455 1_556 ?
O1 K1 Cu1 56.48(10) 1_556 1_556 ?
K1 K1 Cu1 114.775(12) 9_666 1_556 ?
K1 K1 Cu1 114.775(12) 8_456 1_556 ?
O1 K1 Cu1 56.43(10) 8_456 1_556 ?
O1 K1 Cu1 100.73(19) . 1_556 ?
Br1 K1 Cu1 112.844(7) 1_556 1_556 ?
Br1 K1 Cu1 178.96(8) . 1_556 ?
Cu1 K1 Cu1 66.12(8) . 1_556 ?
O1 K1 K1 132.47(17) 8_455 1_556 ?
O1 K1 K1 47.53(17) 1_556 1_556 ?
K1 K1 K1 90.0 9_666 1_556 ?
K1 K1 K1 90.0 8_456 1_556 ?
O1 K1 K1 47.36(17) 8_456 1_556 ?
O1 K1 K1 132.64(17) . 1_556 ?
Br1 K1 K1 55.90(4) 1_556 1_556 ?
Br1 K1 K1 124.10(4) . 1_556 ?
Cu1 K1 K1 123.06(4) . 1_556 ?
Cu1 K1 K1 56.94(4) 1_556 1_556 ?
O1 K1 K1 47.53(17) 8_455 1_554 ?
O1 K1 K1 132.47(17) 1_556 1_554 ?
K1 K1 K1 90.0 9_666 1_554 ?
K1 K1 K1 90.0 8_456 1_554 ?
O1 K1 K1 132.64(17) 8_456 1_554 ?
O1 K1 K1 47.36(17) . 1_554 ?
Br1 K1 K1 124.10(4) 1_556 1_554 ?
Br1 K1 K1 55.90(4) . 1_554 ?
Cu1 K1 K1 56.94(4) . 1_554 ?
Cu1 K1 K1 123.06(4) 1_556 1_554 ?
K1 K1 K1 180.0(3) 1_556 1_554 ?
K1 Br1 K1 180.0 2_675 8_455 ?
K1 Br1 K1 48.92(3) 2_675 9_666 ?
K1 Br1 K1 131.08(3) 8_455 9_666 ?
K1 Br1 K1 48.92(3) 2_675 7_576 ?
K1 Br1 K1 131.08(3) 8_455 7_576 ?
K1 Br1 K1 91.64(6) 9_666 7_576 ?
K1 Br1 K1 131.08(3) 2_675 3_464 ?
K1 Br1 K1 48.92(3) 8_455 3_464 ?
K1 Br1 K1 180.0 9_666 3_464 ?
K1 Br1 K1 88.36(6) 7_576 3_464 ?
K1 Br1 K1 131.08(3) 2_675 1_554 ?
K1 Br1 K1 48.92(3) 8_455 1_554 ?
K1 Br1 K1 88.36(6) 9_666 1_554 ?
K1 Br1 K1 180.0 7_576 1_554 ?
K1 Br1 K1 91.64(6) 3_464 1_554 ?
K1 Br1 K1 91.64(6) 2_675 3_465 ?
K1 Br1 K1 88.36(6) 8_455 3_465 ?
K1 Br1 K1 111.81(9) 9_666 3_465 ?
K1 Br1 K1 48.92(3) 7_576 3_465 ?
K1 Br1 K1 68.19(9) 3_464 3_465 ?
K1 Br1 K1 131.08(3) 1_554 3_465 ?
K1 Br1 K1 68.19(9) 2_675 2_674 ?
K1 Br1 K1 111.81(9) 8_455 2_674 ?
K1 Br1 K1 88.36(6) 9_666 2_674 ?
K1 Br1 K1 88.36(6) 7_576 2_674 ?
K1 Br1 K1 91.64(6) 3_464 2_674 ?
K1 Br1 K1 91.64(6) 1_554 2_674 ?
K1 Br1 K1 131.08(3) 3_465 2_674 ?
K1 Br1 K1 111.81(9) 2_675 8_456 ?
K1 Br1 K1 68.19(9) 8_455 8_456 ?
K1 Br1 K1 91.64(6) 9_666 8_456 ?
K1 Br1 K1 91.64(6) 7_576 8_456 ?
K1 Br1 K1 88.36(6) 3_464 8_456 ?
K1 Br1 K1 88.36(6) 1_554 8_456 ?
K1 Br1 K1 48.92(3) 3_465 8_456 ?
K1 Br1 K1 180.0 2_674 8_456 ?
K1 Br1 K1 88.36(6) 2_675 7_575 ?
K1 Br1 K1 91.64(6) 8_455 7_575 ?
K1 Br1 K1 131.08(3) 9_666 7_575 ?
K1 Br1 K1 68.19(8) 7_576 7_575 ?
K1 Br1 K1 48.92(3) 3_464 7_575 ?
K1 Br1 K1 111.81(8) 1_554 7_575 ?
K1 Br1 K1 88.36(6) 3_465 7_575 ?
K1 Br1 K1 48.92(3) 2_674 7_575 ?
K1 Br1 K1 131.08(3) 8_456 7_575 ?
K1 Br1 K1 88.36(6) 2_675 9_665 ?
K1 Br1 K1 91.64(6) 8_455 9_665 ?
K1 Br1 K1 68.19(9) 9_666 9_665 ?
K1 Br1 K1 131.08(3) 7_576 9_665 ?
K1 Br1 K1 111.81(9) 3_464 9_665 ?
K1 Br1 K1 48.92(3) 1_554 9_665 ?
K1 Br1 K1 180.0 3_465 9_665 ?
K1 Br1 K1 48.92(3) 2_674 9_665 ?
K1 Br1 K1 131.08(3) 8_456 9_665 ?
K1 Br1 K1 91.64(6) 7_575 9_665 ?
K1 Br1 K1 91.64(6) 2_675 . ?
K1 Br1 K1 88.36(6) 8_455 . ?
K1 Br1 K1 48.92(3) 9_666 . ?
K1 Br1 K1 111.81(8) 7_576 . ?
K1 Br1 K1 131.08(3) 3_464 . ?
K1 Br1 K1 68.19(8) 1_554 . ?
K1 Br1 K1 91.64(6) 3_465 . ?
K1 Br1 K1 131.08(3) 2_674 . ?
K1 Br1 K1 48.92(3) 8_456 . ?
K1 Br1 K1 180.00(8) 7_575 . ?
K1 Br1 K1 88.36(6) 9_665 . ?
O1 C1 N1 120.0(5) . 9_665 ?
O1 C1 N1 120.0(5) . 7_565 ?
N1 C1 N1 120.0(10) 9_665 7_565 ?
C1 O1 K1 123.1(6) . 1_554 ?
C1 O1 K1 123.1(6) . 9_665 ?
K1 O1 K1 60.0(2) 1_554 9_665 ?
C1 O1 K1 122.5(6) . 9_666 ?
K1 O1 K1 114.4(3) 1_554 9_666 ?
K1 O1 K1 85.11(15) 9_665 9_666 ?
C1 O1 K1 122.5(6) . . ?
K1 O1 K1 85.11(15) 1_554 . ?
K1 O1 K1 114.4(3) 9_665 . ?
K1 O1 K1 59.8(2) 9_666 . ?
C1 N1 C1 120.0(10) 8_455 7_565 ?
C1 N1 Cu1 120.0(5) 8_455 . ?
C1 N1 Cu1 120.0(5) 7_565 . ?

_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full        26.35
_diffrn_measured_fraction_theta_full 0.979
_refine_diff_density_max         1.052
_refine_diff_density_min         -1.033
_refine_diff_density_rms         0.222
