# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_K2120
_database_code_depnum_ccdc_archive 'CCDC 844291'
_audit_update_record             
;
2016-05-03 deposited with the CCDC.
2016-05-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C4 Cu K2 O8'
_chemical_formula_weight         317.78

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'
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'

_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                   4.8886(11)
_cell_length_b                   6.6448(15)
_cell_length_c                   13.171(3)
_cell_angle_alpha                90
_cell_angle_beta                 96.305(5)
_cell_angle_gamma                90
_cell_volume                     425.25(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1498
_cell_measurement_theta_min      1.5556
_cell_measurement_theta_max      27.4687

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.482
_exptl_crystal_F_000             310
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.071
_exptl_absorpt_coefficient_mu    3.568
_shelx_estimated_absorpt_T_min   0.674
_shelx_estimated_absorpt_T_max   0.786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7782
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_detector       CCD
_diffrn_measurement_device       
;
Saturn724+ (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_method       dtprofit.ref
_diffrn_reflns_number            3644
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.112
_diffrn_reflns_theta_max         27.468
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             977
_reflns_number_gt                916
_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       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-98 (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0315P)²+0.4296P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         977
_refine_ls_number_parameters     70
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0332
_refine_ls_wR_factor_ref         0.0768
_refine_ls_wR_factor_gt          0.0753
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_restrained_S_all      1.174
_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 0.0000 0.5000 0.5000 0.01498(16) Uani 1 2 d S . P . .
K1 K 0.86918(13) 0.92287(9) 0.34879(5) 0.01975(18) Uani 1 1 d . . . . .
O1 O 0.6204(4) 0.5598(3) 0.34211(15) 0.0206(4) Uani 1 1 d . . . . .
O2 O 0.2702(4) 0.6380(3) 0.42940(14) 0.0166(4) Uani 1 1 d . . . . .
O3 O 0.1258(4) 0.2570(3) 0.43945(15) 0.0182(4) Uani 1 1 d . . . . .
O4 O 0.4123(4) 0.1704(3) 0.32543(16) 0.0237(5) Uani 1 1 d . . . . .
C1 C 0.3133(5) 0.2929(4) 0.3803(2) 0.0175(6) Uani 1 1 d . . . . .
C2 C 0.4137(6) 0.5152(4) 0.3820(2) 0.0161(6) 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 O2 1.9288(19) 3_566 ?
Cu1 O2 1.9288(19) . ?
Cu1 O3 1.931(2) 3_566 ?
Cu1 O3 1.931(2) . ?
Cu1 K1 3.4628(9) 3_666 ?
Cu1 K1 3.4628(8) 1_455 ?
K1 O1 2.680(2) 2_655 ?
K1 O1 2.699(2) . ?
K1 O3 2.757(2) 1_665 ?
K1 O4 2.764(2) 1_565 ?
K1 O2 2.845(2) 1_655 ?
K1 O3 3.032(2) 3_666 ?
K1 O4 3.124(2) 2_655 ?
K1 O4 3.167(2) 1_665 ?
K1 C1 3.276(3) 1_665 ?
K1 C2 3.384(3) 2_655 ?
K1 Cu1 3.4628(8) 1_655 ?
K1 K1 4.1751(15) 3_776 ?
O1 C2 1.225(3) . ?
O1 K1 2.680(2) 2_645 ?
O2 C2 1.282(3) . ?
O2 K1 2.845(2) 1_455 ?
O3 C1 1.289(3) . ?
O3 K1 2.757(2) 1_445 ?
O3 K1 3.032(2) 3_666 ?
O4 C1 1.223(3) . ?
O4 K1 2.764(2) 1_545 ?
O4 K1 3.124(2) 2_645 ?
O4 K1 3.167(2) 1_445 ?
C1 C2 1.556(4) . ?
C1 K1 3.276(3) 1_445 ?
C2 K1 3.384(3) 2_645 ?

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
O2 Cu1 O2 180 3_566 . ?
O2 Cu1 O3 86.13(8) 3_566 3_566 ?
O2 Cu1 O3 93.87(8) . 3_566 ?
O2 Cu1 O3 93.87(8) 3_566 . ?
O2 Cu1 O3 86.13(8) . . ?
O3 Cu1 O3 180 3_566 . ?
O2 Cu1 K1 55.25(6) 3_566 3_666 ?
O2 Cu1 K1 124.75(6) . 3_666 ?
O3 Cu1 K1 119.21(6) 3_566 3_666 ?
O3 Cu1 K1 60.79(6) . 3_666 ?
O2 Cu1 K1 124.75(6) 3_566 1_455 ?
O2 Cu1 K1 55.25(6) . 1_455 ?
O3 Cu1 K1 60.79(6) 3_566 1_455 ?
O3 Cu1 K1 119.21(6) . 1_455 ?
K1 Cu1 K1 180 3_666 1_455 ?
O1 K1 O1 109.14(5) 2_655 . ?
O1 K1 O3 94.49(7) 2_655 1_665 ?
O1 K1 O3 156.36(6) . 1_665 ?
O1 K1 O4 77.99(6) 2_655 1_565 ?
O1 K1 O4 99.94(7) . 1_565 ?
O3 K1 O4 83.84(6) 1_665 1_565 ?
O1 K1 O2 119.52(6) 2_655 1_655 ?
O1 K1 O2 72.96(6) . 1_655 ?
O3 K1 O2 96.43(6) 1_665 1_655 ?
O4 K1 O2 162.31(6) 1_565 1_655 ?
O1 K1 O3 176.30(6) 2_655 3_666 ?
O1 K1 O3 68.64(6) . 3_666 ?
O3 K1 O3 87.80(6) 1_665 3_666 ?
O4 K1 O3 105.18(6) 1_565 3_666 ?
O2 K1 O3 57.24(5) 1_655 3_666 ?
O1 K1 O4 56.62(6) 2_655 2_655 ?
O1 K1 O4 71.65(6) . 2_655 ?
O3 K1 O4 125.07(6) 1_665 2_655 ?
O4 K1 O4 125.11(4) 1_565 2_655 ?
O2 K1 O4 68.88(6) 1_655 2_655 ?
O3 K1 O4 119.68(6) 3_666 2_655 ?
O1 K1 O4 68.28(6) 2_655 1_665 ?
O1 K1 O4 147.22(6) . 1_665 ?
O3 K1 O4 43.72(5) 1_665 1_665 ?
O4 K1 O4 110.86(8) 1_565 1_665 ?
O2 K1 O4 80.28(6) 1_655 1_665 ?
O3 K1 O4 111.84(6) 3_666 1_665 ?
O4 K1 O4 81.35(4) 2_655 1_665 ?
O1 K1 C1 77.50(7) 2_655 1_665 ?
O1 K1 C1 164.79(7) . 1_665 ?
O3 K1 C1 22.63(6) 1_665 1_665 ?
O4 K1 C1 94.80(7) 1_565 1_665 ?
O2 K1 C1 91.84(7) 1_655 1_665 ?
O3 K1 C1 103.94(6) 3_666 1_665 ?
O4 K1 C1 102.75(7) 2_655 1_665 ?
O4 K1 C1 21.80(6) 1_665 1_665 ?
O1 K1 C2 19.17(6) 2_655 2_655 ?
O1 K1 C2 108.51(7) . 2_655 ?
O3 K1 C2 94.03(7) 1_665 2_655 ?
O4 K1 C2 96.98(7) 1_565 2_655 ?
O2 K1 C2 100.63(6) 1_655 2_655 ?
O3 K1 C2 157.84(6) 3_666 2_655 ?
O4 K1 C2 43.22(6) 2_655 2_655 ?
O4 K1 C2 57.96(6) 1_665 2_655 ?
C1 K1 C2 73.07(7) 1_665 2_655 ?
O1 K1 Cu1 142.54(5) 2_655 1_655 ?
O1 K1 Cu1 49.27(5) . 1_655 ?
O3 K1 Cu1 110.97(5) 1_665 1_655 ?
O4 K1 Cu1 130.01(5) 1_565 1_655 ?
O2 K1 Cu1 33.84(4) 1_655 1_655 ?
O3 K1 Cu1 33.78(4) 3_666 1_655 ?
O4 K1 Cu1 86.00(4) 2_655 1_655 ?
O4 K1 Cu1 111.93(4) 1_665 1_655 ?
C1 K1 Cu1 117.27(5) 1_665 1_655 ?
C2 K1 Cu1 127.40(5) 2_655 1_655 ?
O1 K1 K1 140.93(6) 2_655 3_776 ?
O1 K1 K1 109.89(5) . 3_776 ?
O3 K1 K1 46.52(4) 1_665 3_776 ?
O4 K1 K1 96.85(5) 1_565 3_776 ?
O2 K1 K1 71.40(4) 1_655 3_776 ?
O3 K1 K1 41.28(4) 3_666 3_776 ?
O4 K1 K1 137.64(5) 2_655 3_776 ?
O4 K1 K1 78.05(4) 1_665 3_776 ?
C1 K1 K1 64.25(5) 1_665 3_776 ?
C2 K1 K1 135.96(5) 2_655 3_776 ?
Cu1 K1 K1 68.45(2) 1_655 3_776 ?
C2 O1 K1 114.94(18) . 2_645 ?
C2 O1 K1 126.29(19) . . ?
K1 O1 K1 106.21(7) 2_645 . ?
C2 O2 Cu1 111.88(18) . . ?
C2 O2 K1 129.26(16) . 1_455 ?
Cu1 O2 K1 90.91(7) . 1_455 ?
C1 O3 Cu1 112.00(18) . . ?
C1 O3 K1 101.98(16) . 1_445 ?
Cu1 O3 K1 134.58(9) . 1_445 ?
C1 O3 K1 133.99(16) . 3_666 ?
Cu1 O3 K1 85.44(7) . 3_666 ?
K1 O3 K1 92.20(6) 1_445 3_666 ?
C1 O4 K1 134.23(19) . 1_545 ?
C1 O4 K1 105.43(18) . 2_645 ?
K1 O4 K1 93.67(6) 1_545 2_645 ?
C1 O4 K1 84.15(17) . 1_445 ?
K1 O4 K1 110.86(8) 1_545 1_445 ?
K1 O4 K1 135.10(7) 2_645 1_445 ?
O4 C1 O3 126.0(3) . . ?
O4 C1 C2 119.7(2) . . ?
O3 C1 C2 114.3(2) . . ?
O4 C1 K1 74.05(17) . 1_445 ?
O3 C1 K1 55.39(14) . 1_445 ?
C2 C1 K1 156.61(17) . 1_445 ?
O1 C2 O2 125.2(3) . . ?
O1 C2 C1 119.8(2) . . ?
O2 C2 C1 115.0(2) . . ?
O1 C2 K1 45.89(14) . 2_645 ?
O2 C2 K1 142.69(18) . 2_645 ?
C1 C2 K1 86.83(15) . 2_645 ?

_refine_diff_density_max         0.433
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.109

####################################################################### 
# 
# 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_K2122
_database_code_depnum_ccdc_archive 'CCDC 844292'
_audit_update_record             
;
2016-05-03 deposited with the CCDC.
2016-05-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C4 H4 Cu K2 O10'
_chemical_formula_weight         353.81

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'
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'

_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                   6.904(2)
_cell_length_b                   8.660(3)
_cell_length_c                   8.929(3)
_cell_angle_alpha                107.950(4)
_cell_angle_beta                 99.637(4)
_cell_angle_gamma                97.637(4)
_cell_volume                     490.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1917
_cell_measurement_theta_min      2.4539
_cell_measurement_theta_max      27.4793

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.394
_exptl_crystal_F_000             350
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.293
_exptl_crystal_size_mid          0.252
_exptl_crystal_size_min          0.198
_exptl_absorpt_coefficient_mu    3.118
_shelx_estimated_absorpt_T_min   0.462
_shelx_estimated_absorpt_T_max   0.577
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4632
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_diffrn_source_current           24.0000
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_detector       CCD
_diffrn_measurement_device       
;
Saturn724+ (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_method       merged.ref
_diffrn_reflns_number            4162
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.557
_diffrn_reflns_theta_max         27.541
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measured_fraction_theta_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_point_group_measured_fraction_full 0.978
_reflns_number_total             2211
_reflns_number_gt                2158
_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       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0475P)²+0.2130P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2211
_refine_ls_number_parameters     173
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0283
_refine_ls_wR_factor_ref         0.0781
_refine_ls_wR_factor_gt          0.0774
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.075
_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 0.0000 0.0000 0.0000 0.01361(11) Uani 1 2 d S . P . .
Cu2 Cu 0.5000 0.0000 0.5000 0.01372(11) Uani 1 2 d S . P . .
K1 K 0.13059(6) 0.33461(5) 0.36231(5) 0.02060(12) Uani 1 1 d . . . . .
K2 K 0.75877(6) 0.62533(5) 0.03717(6) 0.02195(12) Uani 1 1 d . . . . .
O5 O -0.0728(3) -0.0169(2) 0.2514(2) 0.0257(3) Uani 1 1 d . . . . .
H1 H -0.198(6) -0.020(4) 0.264(4) 0.054(10) Uiso 1 1 d . . . . .
H2 H 0.007(5) -0.036(4) 0.322(4) 0.045(9) Uiso 1 1 d . . . . .
O1 O 0.2689(2) 0.10815(16) 0.12535(17) 0.0160(3) Uani 1 1 d . . . . .
O2 O 0.0996(2) -0.20473(16) -0.03626(17) 0.0161(3) Uani 1 1 d . . . . .
O3 O 0.5434(2) 0.03606(18) 0.23018(19) 0.0203(3) Uani 1 1 d . . . . .
O4 O 0.3854(2) -0.28731(17) 0.02972(17) 0.0194(3) Uani 1 1 d . . . . .
C1 C 0.3774(3) 0.0028(2) 0.1389(2) 0.0133(3) Uani 1 1 d . . . . .
C2 C 0.2841(3) -0.1808(2) 0.0342(2) 0.0136(3) Uani 1 1 d . . . . .
O6 O 0.7656(2) 0.13021(17) 0.60321(17) 0.0172(3) Uani 1 1 d . . . . .
O7 O 0.4094(2) 0.20986(17) 0.56581(18) 0.0187(3) Uani 1 1 d . . . . .
O8 O 0.9097(2) 0.39077(18) 0.75212(19) 0.0240(3) Uani 1 1 d . . . . .
O9 O 0.5369(2) 0.47157(18) 0.7205(2) 0.0270(3) Uani 1 1 d . . . . .
C3 C 0.7637(3) 0.2839(2) 0.6733(2) 0.0159(4) Uani 1 1 d . . . . .
C4 C 0.5533(3) 0.3285(2) 0.6529(2) 0.0175(4) Uani 1 1 d . . . . .
O10 O 0.7453(2) 0.3675(2) 0.38115(19) 0.0211(3) Uani 1 1 d . . . . .
H3 H 0.685(5) 0.421(4) 0.336(4) 0.042(9) Uiso 1 1 d . . . . .
H4 H 0.687(5) 0.276(4) 0.345(4) 0.037(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 O2 1.9406(14) 2 ?
Cu1 O2 1.9406(14) . ?
Cu1 O1 1.9423(14) 2 ?
Cu1 O1 1.9423(14) . ?
Cu1 O5 2.4238(18) . ?
Cu1 O5 2.4238(18) 2 ?
Cu1 K1 3.4965(10) 2 ?
Cu1 K1 3.4965(10) . ?
Cu1 K2 3.5811(11) 1_445 ?
Cu1 K2 3.5811(11) 2_665 ?
Cu2 O6 1.9305(15) 2_656 ?
Cu2 O6 1.9305(15) . ?
Cu2 O7 1.9512(15) 2_656 ?
Cu2 O7 1.9512(15) . ?
K1 O10 2.7396(18) 1_455 ?
K1 O10 2.7840(18) 2_666 ?
K1 O1 2.8019(16) . ?
K1 O2 2.8675(17) 2 ?
K1 O8 2.8907(17) 2_666 ?
K1 O5 2.960(2) . ?
K1 O7 2.9605(16) . ?
K1 O9 2.9910(19) 2_666 ?
K1 C3 3.411(2) 2_666 ?
K1 C4 3.456(2) 2_666 ?
K1 K2 3.8768(13) 2_665 ?
K2 O8 2.7570(16) 2_766 ?
K2 O4 2.7773(16) 1_565 ?
K2 O9 2.7928(18) 1_554 ?
K2 O4 2.8045(17) 2_655 ?
K2 O2 2.8850(16) 1_665 ?
K2 O5 3.042(2) 1_665 ?
K2 O1 3.0916(16) 2_665 ?
K2 O8 3.1551(18) 1_554 ?
K2 O9 3.419(2) 2_666 ?
K2 C4 3.515(2) 1_554 ?
K2 Cu1 3.5811(11) 1_665 ?
K2 K2 3.7651(13) 2_665 ?
O5 K2 3.042(2) 1_445 ?
O5 H1 0.89(4) . ?
O5 H2 0.83(4) . ?
O1 C1 1.275(2) . ?
O1 K2 3.0916(16) 2_665 ?
O2 C2 1.281(2) . ?
O2 K1 2.8675(17) 2 ?
O2 K2 2.8850(16) 1_445 ?
O3 C1 1.231(2) . ?
O4 C2 1.225(2) . ?
O4 K2 2.7773(16) 1_545 ?
O4 K2 2.8046(17) 2_655 ?
C1 C2 1.558(2) . ?
O6 C3 1.287(2) . ?
O7 C4 1.275(2) . ?
O8 C3 1.218(2) . ?
O8 K2 2.7570(16) 2_766 ?
O8 K1 2.8907(17) 2_666 ?
O8 K2 3.1551(18) 1_556 ?
O9 C4 1.229(2) . ?
O9 K2 2.7928(18) 1_556 ?
O9 K1 2.9910(19) 2_666 ?
O9 K2 3.419(2) 2_666 ?
C3 C4 1.548(3) . ?
C3 K1 3.411(2) 2_666 ?
C4 K1 3.456(2) 2_666 ?
C4 K2 3.515(2) 1_556 ?
O10 K1 2.7396(18) 1_655 ?
O10 K1 2.7840(18) 2_666 ?
O10 H3 0.81(4) . ?
O10 H4 0.78(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
O2 Cu1 O2 180 2 . ?
O2 Cu1 O1 85.71(6) 2 2 ?
O2 Cu1 O1 94.29(6) . 2 ?
O2 Cu1 O1 94.29(6) 2 . ?
O2 Cu1 O1 85.71(6) . . ?
O1 Cu1 O1 180 2 . ?
O2 Cu1 O5 90.10(6) 2 . ?
O2 Cu1 O5 89.90(6) . . ?
O1 Cu1 O5 94.14(6) 2 . ?
O1 Cu1 O5 85.86(6) . . ?
O2 Cu1 O5 89.90(6) 2 2 ?
O2 Cu1 O5 90.10(6) . 2 ?
O1 Cu1 O5 85.86(6) 2 2 ?
O1 Cu1 O5 94.14(6) . 2 ?
O5 Cu1 O5 180 . 2 ?
O2 Cu1 K1 124.92(4) 2 2 ?
O2 Cu1 K1 55.08(4) . 2 ?
O1 Cu1 K1 53.14(4) 2 2 ?
O1 Cu1 K1 126.86(4) . 2 ?
O5 Cu1 K1 123.44(5) . 2 ?
O5 Cu1 K1 56.56(5) 2 2 ?
O2 Cu1 K1 55.08(4) 2 . ?
O2 Cu1 K1 124.92(4) . . ?
O1 Cu1 K1 126.86(4) 2 . ?
O1 Cu1 K1 53.14(4) . . ?
O5 Cu1 K1 56.56(5) . . ?
O5 Cu1 K1 123.44(5) 2 . ?
K1 Cu1 K1 180 2 . ?
O2 Cu1 K2 126.50(5) 2 1_445 ?
O2 Cu1 K2 53.50(5) . 1_445 ?
O1 Cu1 K2 59.60(4) 2 1_445 ?
O1 Cu1 K2 120.40(4) . 1_445 ?
O5 Cu1 K2 57.05(5) . 1_445 ?
O5 Cu1 K2 122.95(5) 2 1_445 ?
K1 Cu1 K2 66.42(2) 2 1_445 ?
K1 Cu1 K2 113.58(2) . 1_445 ?
O2 Cu1 K2 53.50(5) 2 2_665 ?
O2 Cu1 K2 126.50(5) . 2_665 ?
O1 Cu1 K2 120.40(4) 2 2_665 ?
O1 Cu1 K2 59.60(4) . 2_665 ?
O5 Cu1 K2 122.95(5) . 2_665 ?
O5 Cu1 K2 57.05(5) 2 2_665 ?
K1 Cu1 K2 113.58(2) 2 2_665 ?
K1 Cu1 K2 66.42(2) . 2_665 ?
K2 Cu1 K2 180 1_445 2_665 ?
O6 Cu2 O6 180 2_656 . ?
O6 Cu2 O7 85.58(6) 2_656 2_656 ?
O6 Cu2 O7 94.42(6) . 2_656 ?
O6 Cu2 O7 94.42(6) 2_656 . ?
O6 Cu2 O7 85.58(6) . . ?
O7 Cu2 O7 180 2_656 . ?
O10 K1 O10 87.13(5) 1_455 2_666 ?
O10 K1 O1 129.33(5) 1_455 . ?
O10 K1 O1 142.49(5) 2_666 . ?
O10 K1 O2 74.18(5) 1_455 2 ?
O10 K1 O2 140.08(5) 2_666 2 ?
O1 K1 O2 60.26(4) . 2 ?
O10 K1 O8 78.23(5) 1_455 2_666 ?
O10 K1 O8 69.87(5) 2_666 2_666 ?
O1 K1 O8 105.36(5) . 2_666 ?
O2 K1 O8 71.91(4) 2 2_666 ?
O10 K1 O5 79.18(5) 1_455 . ?
O10 K1 O5 146.62(5) 2_666 . ?
O1 K1 O5 62.56(5) . . ?
O2 K1 O5 64.44(4) 2 . ?
O8 K1 O5 134.77(5) 2_666 . ?
O10 K1 O7 127.38(5) 1_455 . ?
O10 K1 O7 84.39(5) 2_666 . ?
O1 K1 O7 79.33(5) . . ?
O2 K1 O7 134.89(5) 2 . ?
O8 K1 O7 143.37(4) 2_666 . ?
O5 K1 O7 80.24(5) . . ?
O10 K1 O9 133.72(5) 1_455 2_666 ?
O10 K1 O9 74.29(5) 2_666 2_666 ?
O1 K1 O9 73.15(5) . 2_666 ?
O2 K1 O9 93.43(5) 2 2_666 ?
O8 K1 O9 55.69(4) 2_666 2_666 ?
O5 K1 O9 135.69(5) . 2_666 ?
O7 K1 O9 93.14(5) . 2_666 ?
O10 K1 C3 91.35(5) 1_455 2_666 ?
O10 K1 C3 54.74(5) 2_666 2_666 ?
O1 K1 C3 108.72(5) . 2_666 ?
O2 K1 C3 90.11(4) 2 2_666 ?
O8 K1 C3 20.19(4) 2_666 2_666 ?
O5 K1 C3 154.36(5) . 2_666 ?
O7 K1 C3 123.39(4) . 2_666 ?
O9 K1 C3 43.37(4) 2_666 2_666 ?
O10 K1 C4 117.08(5) 1_455 2_666 ?
O10 K1 C4 57.02(5) 2_666 2_666 ?
O1 K1 C4 93.17(5) . 2_666 ?
O2 K1 C4 100.55(5) 2 2_666 ?
O8 K1 C4 43.29(4) 2_666 2_666 ?
O5 K1 C4 155.28(5) . 2_666 ?
O7 K1 C4 100.87(5) . 2_666 ?
O9 K1 C4 20.39(4) 2_666 2_666 ?
C3 K1 C4 26.05(4) 2_666 2_666 ?
O10 K1 Cu1 95.64(4) 1_455 . ?
O10 K1 Cu1 170.20(4) 2_666 . ?
O1 K1 Cu1 33.69(3) . . ?
O2 K1 Cu1 33.70(3) 2 . ?
O8 K1 Cu1 101.44(4) 2_666 . ?
O5 K1 Cu1 43.11(3) . . ?
O7 K1 Cu1 101.19(4) . . ?
O9 K1 Cu1 97.20(4) 2_666 . ?
C3 K1 Cu1 115.69(4) 2_666 . ?
C4 K1 Cu1 113.63(4) 2_666 . ?
O10 K1 K2 110.70(4) 1_455 2_665 ?
O10 K1 K2 112.39(4) 2_666 2_665 ?
O1 K1 K2 52.18(3) . 2_665 ?
O2 K1 K2 47.82(4) 2 2_665 ?
O8 K1 K2 53.18(3) 2_666 2_665 ?
O5 K1 K2 100.93(4) . 2_665 ?
O7 K1 K2 120.52(4) . 2_665 ?
O9 K1 K2 45.77(3) 2_666 2_665 ?
C3 K1 K2 60.01(3) 2_666 2_665 ?
C4 K1 K2 56.94(3) 2_666 2_665 ?
Cu1 K1 K2 57.84(2) . 2_665 ?
O8 K2 O4 141.73(5) 2_766 1_565 ?
O8 K2 O9 141.74(5) 2_766 1_554 ?
O4 K2 O9 73.35(5) 1_565 1_554 ?
O8 K2 O4 89.31(4) 2_766 2_655 ?
O4 K2 O4 95.17(4) 1_565 2_655 ?
O9 K2 O4 68.12(5) 1_554 2_655 ?
O8 K2 O2 74.16(5) 2_766 1_665 ?
O4 K2 O2 126.04(5) 1_565 1_665 ?
O9 K2 O2 97.39(5) 1_554 1_665 ?
O4 K2 O2 131.33(4) 2_655 1_665 ?
O8 K2 O5 75.54(5) 2_766 1_665 ?
O4 K2 O5 85.80(5) 1_565 1_665 ?
O9 K2 O5 134.48(5) 1_554 1_665 ?
O4 K2 O5 155.70(5) 2_655 1_665 ?
O2 K2 O5 63.05(4) 1_665 1_665 ?
O8 K2 O1 125.74(4) 2_766 2_665 ?
O4 K2 O1 70.24(4) 1_565 2_665 ?
O9 K2 O1 71.71(5) 1_554 2_665 ?
O4 K2 O1 139.71(5) 2_655 2_665 ?
O2 K2 O1 56.76(4) 1_665 2_665 ?
O5 K2 O1 63.18(5) 1_665 2_665 ?
O8 K2 O8 88.47(5) 2_766 1_554 ?
O4 K2 O8 127.96(4) 1_565 1_554 ?
O9 K2 O8 54.63(5) 1_554 1_554 ?
O4 K2 O8 66.16(4) 2_655 1_554 ?
O2 K2 O8 67.90(4) 1_665 1_554 ?
O5 K2 O8 130.83(5) 1_665 1_554 ?
O1 K2 O8 92.89(5) 2_665 1_554 ?
O8 K2 O9 89.23(5) 2_766 2_666 ?
O4 K2 O9 59.71(4) 1_565 2_666 ?
O9 K2 O9 106.16(5) 1_554 2_666 ?
O4 K2 O9 63.73(4) 2_655 2_666 ?
O2 K2 O9 156.13(4) 1_665 2_666 ?
O5 K2 O9 96.64(5) 1_665 2_666 ?
O1 K2 O9 127.41(4) 2_665 2_666 ?
O8 K2 O9 129.86(4) 1_554 2_666 ?
O8 K2 C4 124.46(5) 2_766 1_554 ?
O4 K2 C4 87.33(5) 1_565 1_554 ?
O9 K2 C4 18.27(4) 1_554 1_554 ?
O4 K2 C4 53.88(4) 2_655 1_554 ?
O2 K2 C4 98.84(5) 1_665 1_554 ?
O5 K2 C4 150.22(5) 1_665 1_554 ?
O1 K2 C4 87.24(5) 2_665 1_554 ?
O8 K2 C4 41.72(4) 1_554 1_554 ?
O9 K2 C4 104.73(5) 2_666 1_554 ?
O8 K2 Cu1 92.99(4) 2_766 1_665 ?
O4 K2 Cu1 94.92(4) 1_565 1_665 ?
O9 K2 Cu1 99.12(4) 1_554 1_665 ?
O4 K2 Cu1 160.57(3) 2_655 1_665 ?
O2 K2 Cu1 32.73(3) 1_665 1_665 ?
O5 K2 Cu1 41.95(4) 1_665 1_665 ?
O1 K2 Cu1 32.81(3) 2_665 1_665 ?
O8 K2 Cu1 94.60(3) 1_554 1_665 ?
O9 K2 Cu1 135.54(3) 2_666 1_665 ?
C4 K2 Cu1 110.16(4) 1_554 1_665 ?
O8 K2 K2 124.77(4) 2_766 2_665 ?
O4 K2 K2 47.89(4) 1_565 2_665 ?
O9 K2 K2 60.72(4) 1_554 2_665 ?
O4 K2 K2 47.28(3) 2_655 2_665 ?
O2 K2 K2 157.81(4) 1_665 2_665 ?
O5 K2 K2 128.67(4) 1_665 2_665 ?
O1 K2 K2 108.59(3) 2_665 2_665 ?
O8 K2 K2 98.78(3) 1_554 2_665 ?
O9 K2 K2 45.44(3) 2_666 2_665 ?
C4 K2 K2 61.74(4) 1_554 2_665 ?
Cu1 K2 K2 139.97(2) 1_665 2_665 ?
Cu1 O5 K1 80.34(5) . . ?
Cu1 O5 K2 81.00(5) . 1_445 ?
K1 O5 K2 161.27(6) . 1_445 ?
Cu1 O5 H1 119(2) . . ?
K1 O5 H1 108(2) . . ?
K2 O5 H1 82(2) 1_445 . ?
Cu1 O5 H2 124(2) . . ?
K1 O5 H2 92(2) . . ?
K2 O5 H2 98(2) 1_445 . ?
H1 O5 H2 116(3) . . ?
C1 O1 Cu1 111.43(12) . . ?
C1 O1 K1 129.70(12) . . ?
Cu1 O1 K1 93.17(6) . . ?
C1 O1 K2 139.21(12) . 2_665 ?
Cu1 O1 K2 87.58(5) . 2_665 ?
K1 O1 K2 82.11(4) . 2_665 ?
C2 O2 Cu1 112.38(12) . . ?
C2 O2 K1 136.43(12) . 2 ?
Cu1 O2 K1 91.22(5) . 2 ?
C2 O2 K2 126.98(11) . 1_445 ?
Cu1 O2 K2 93.77(6) . 1_445 ?
K1 O2 K2 84.74(4) 2 1_445 ?
C2 O4 K2 148.62(13) . 1_545 ?
C2 O4 K2 126.34(12) . 2_655 ?
K2 O4 K2 84.83(4) 1_545 2_655 ?
O3 C1 O1 124.87(17) . . ?
O3 C1 C2 119.39(17) . . ?
O1 C1 C2 115.71(16) . . ?
O4 C2 O2 126.24(17) . . ?
O4 C2 C1 119.59(17) . . ?
O2 C2 C1 114.12(16) . . ?
C3 O6 Cu2 112.36(12) . . ?
C4 O7 Cu2 111.48(13) . . ?
C4 O7 K1 108.94(11) . . ?
Cu2 O7 K1 126.99(7) . . ?
C3 O8 K2 129.75(12) . 2_766 ?
C3 O8 K1 104.79(12) . 2_666 ?
K2 O8 K1 124.93(5) 2_766 2_666 ?
C3 O8 K2 105.14(13) . 1_556 ?
K2 O8 K2 91.54(5) 2_766 1_556 ?
K1 O8 K2 79.64(4) 2_666 1_556 ?
C4 O9 K2 116.34(13) . 1_556 ?
C4 O9 K1 101.67(13) . 2_666 ?
K2 O9 K1 84.11(5) 1_556 2_666 ?
C4 O9 K2 95.45(13) . 2_666 ?
K2 O9 K2 73.84(5) 1_556 2_666 ?
K1 O9 K2 156.49(5) 2_666 2_666 ?
O8 C3 O6 125.55(18) . . ?
O8 C3 C4 119.85(17) . . ?
O6 C3 C4 114.60(16) . . ?
O8 C3 K1 55.02(10) . 2_666 ?
O6 C3 K1 142.46(13) . 2_666 ?
C4 C3 K1 78.60(10) . 2_666 ?
O9 C4 O7 125.42(18) . . ?
O9 C4 C3 118.90(17) . . ?
O7 C4 C3 115.68(16) . . ?
O9 C4 K1 57.95(11) . 2_666 ?
O7 C4 K1 141.75(13) . 2_666 ?
C3 C4 K1 75.36(10) . 2_666 ?
O9 C4 K2 45.40(10) . 1_556 ?
O7 C4 K2 146.29(14) . 1_556 ?
C3 C4 K2 83.09(10) . 1_556 ?
K1 C4 K2 67.57(4) 2_666 1_556 ?
K1 O10 K1 92.87(5) 1_655 2_666 ?
K1 O10 H3 122(2) 1_655 . ?
K1 O10 H3 85(2) 2_666 . ?
K1 O10 H4 103(2) 1_655 . ?
K1 O10 H4 150(2) 2_666 . ?
H3 O10 H4 107(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H1 O3 0.89(4) 1.92(5) 2.734(2) 153(3) 1_455
O5 H2 O6 0.83(4) 1.98(4) 2.750(2) 154(3) 2_656
O5 H1 O3 0.89(4) 1.92(5) 2.734(2) 153(3) 1_455
O5 H2 O6 0.83(4) 1.98(4) 2.750(2) 154(3) 2_656
O10 H3 O9 0.81(4) 1.97(4) 2.734(2) 156(3) 2_666
O10 H4 O3 0.78(3) 2.04(3) 2.814(2) 174(3) .

_refine_diff_density_max         0.525
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.106

####################################################################### 
# 
# 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. 
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#######################################################################

data_K2124
_audit_block_doi                 10.5517/ccxkrv1
_database_code_depnum_ccdc_archive 'CCDC 851224'
_audit_update_record             
;
2016-05-03 deposited with the CCDC.
2016-05-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C4 H8 Cu K2 O12'
_chemical_formula_weight         389.84

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'
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'

_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                   3.7345(7)
_cell_length_b                   14.764(3)
_cell_length_c                   10.742(2)
_cell_angle_alpha                90
_cell_angle_beta                 93.23(3)
_cell_angle_gamma                90
_cell_volume                     591.3(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1849
_cell_measurement_theta_min      1.8989
_cell_measurement_theta_max      27.4578

_exptl_crystal_description       needle
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.190
_exptl_crystal_F_000             390
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.094
_exptl_absorpt_coefficient_mu    2.611
_shelx_estimated_absorpt_T_min   0.528
_shelx_estimated_absorpt_T_max   0.791
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.6079
_exptl_absorpt_correction_T_max  0.8047
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(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  CCD
_diffrn_measurement_device       
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4206
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.350
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             1341
_reflns_number_gt                1268
_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       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0177P)²+0.5322P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1341
_refine_ls_number_parameters     104
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0304
_refine_ls_wR_factor_ref         0.0640
_refine_ls_wR_factor_gt          0.0623
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_restrained_S_all      1.132
_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 0.0000 0.0000 0.0000 0.01557(13) Uani 1 2 d S . P . .
K1 K 0.28023(14) 0.13353(3) 0.51304(5) 0.01793(14) Uani 1 1 d . . . . .
O1 O -0.0039(5) 0.03080(11) 0.17506(14) 0.0181(4) Uani 1 1 d . . . . .
O2 O 0.2139(5) -0.02100(11) 0.35980(15) 0.0183(4) Uani 1 1 d . . . . .
O3 O 0.3468(5) -0.09099(11) 0.05427(14) 0.0201(4) Uani 1 1 d . . . . .
O4 O 0.5696(5) -0.15378(11) 0.23093(16) 0.0217(4) Uani 1 1 d . . . . .
C1 C 0.1854(6) -0.02360(15) 0.2457(2) 0.0154(5) Uani 1 1 d . . . . .
C2 C 0.3861(6) -0.09726(15) 0.1735(2) 0.0162(5) Uani 1 1 d . . . . .
O5 O 0.6822(5) 0.17062(14) 0.31562(18) 0.0251(4) Uani 1 1 d . . . . .
O6 O -0.2055(5) 0.26708(13) 0.5732(2) 0.0244(4) Uani 1 1 d . . . . .
H1 H 0.785(9) 0.137(2) 0.272(3) 0.039(10) Uiso 1 1 d . . . . .
H2 H 0.772(10) 0.220(3) 0.300(3) 0.046(10) Uiso 1 1 d . . . . .
H3 H -0.110(9) 0.309(2) 0.530(3) 0.044(10) Uiso 1 1 d . . . . .
H4 H -0.172(10) 0.275(2) 0.634(3) 0.038(12) 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 O3 1.9330(16) 3 ?
Cu1 O3 1.9330(16) . ?
Cu1 O1 1.9356(16) . ?
Cu1 O1 1.9356(16) 3 ?
K1 O5 2.722(2) . ?
K1 O6 2.780(2) . ?
K1 O4 2.7918(18) 3_656 ?
K1 O6 2.803(2) 1_655 ?
K1 O2 2.8113(18) 3_656 ?
K1 O2 2.8160(17) . ?
K1 O2 2.8835(19) 3_556 ?
K1 O5 3.042(2) 1_455 ?
K1 K1 3.7345(7) 1_655 ?
K1 K1 3.7345(7) 1_455 ?
K1 K1 4.2860(13) 3_656 ?
K1 K1 4.4653(13) 3_556 ?
K1 H3 2.98(3) . ?
K1 H4 3.02(4) . ?
O1 C1 1.289(3) . ?
O2 C1 1.225(3) . ?
O2 K1 2.8114(18) 3_656 ?
O2 K1 2.8836(18) 3_556 ?
O3 C2 1.284(3) . ?
O4 C2 1.224(3) . ?
O4 K1 2.7918(18) 3_656 ?
C1 C2 1.553(3) . ?
O5 K1 3.042(2) 1_655 ?
O5 H1 0.79(4) . ?
O5 H2 0.82(4) . ?
O6 K1 2.803(2) 1_455 ?
O6 H3 0.86(4) . ?
O6 H4 0.66(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
O3 Cu1 O3 180 3 . ?
O3 Cu1 O1 95.05(7) 3 . ?
O3 Cu1 O1 84.95(7) . . ?
O3 Cu1 O1 84.95(7) 3 3 ?
O3 Cu1 O1 95.05(7) . 3 ?
O1 Cu1 O1 180 . 3 ?
O5 K1 O6 115.72(7) . . ?
O5 K1 O4 131.07(6) . 3_656 ?
O6 K1 O4 78.03(6) . 3_656 ?
O5 K1 O6 68.72(7) . 1_655 ?
O6 K1 O6 83.98(6) . 1_655 ?
O4 K1 O6 66.46(6) 3_656 1_655 ?
O5 K1 O2 96.46(6) . 3_656 ?
O6 K1 O2 137.36(6) . 3_656 ?
O4 K1 O2 59.50(5) 3_656 3_656 ?
O6 K1 O2 82.57(6) 1_655 3_656 ?
O5 K1 O2 75.04(6) . . ?
O6 K1 O2 132.33(6) . . ?
O4 K1 O2 131.97(5) 3_656 . ?
O6 K1 O2 137.84(6) 1_655 . ?
O2 K1 O2 80.78(5) 3_656 . ?
O5 K1 O2 151.73(6) . 3_556 ?
O6 K1 O2 81.68(6) . 3_556 ?
O4 K1 O2 72.15(5) 3_656 3_556 ?
O6 K1 O2 138.14(6) 1_655 3_556 ?
O2 K1 O2 81.94(5) 3_656 3_556 ?
O2 K1 O2 76.85(6) . 3_556 ?
O5 K1 O5 80.57(5) . 1_455 ?
O6 K1 O5 64.61(6) . 1_455 ?
O4 K1 O5 140.03(6) 3_656 1_455 ?
O6 K1 O5 120.05(6) 1_655 1_455 ?
O2 K1 O5 153.13(6) 3_656 1_455 ?
O2 K1 O5 72.63(5) . 1_455 ?
O2 K1 O5 88.26(5) 3_556 1_455 ?
O5 K1 K1 53.46(5) . 1_655 ?
O6 K1 K1 131.73(4) . 1_655 ?
O4 K1 K1 81.64(5) 3_656 1_655 ?
O6 K1 K1 47.75(4) 1_655 1_655 ?
O2 K1 K1 49.86(4) 3_656 1_655 ?
O2 K1 K1 93.15(4) . 1_655 ?
O2 K1 K1 131.81(4) 3_556 1_655 ?
O5 K1 K1 134.03(4) 1_455 1_655 ?
O5 K1 K1 126.54(5) . 1_455 ?
O6 K1 K1 48.27(4) . 1_455 ?
O4 K1 K1 98.36(5) 3_656 1_455 ?
O6 K1 K1 132.25(4) 1_655 1_455 ?
O2 K1 K1 130.14(4) 3_656 1_455 ?
O2 K1 K1 86.85(4) . 1_455 ?
O2 K1 K1 48.19(4) 3_556 1_455 ?
O5 K1 K1 45.97(4) 1_455 1_455 ?
K1 K1 K1 180.0 1_655 1_455 ?
O5 K1 K1 84.50(5) . 3_656 ?
O6 K1 K1 157.67(5) . 3_656 ?
O4 K1 K1 96.11(4) 3_656 3_656 ?
O6 K1 K1 113.72(5) 1_655 3_656 ?
O2 K1 K1 40.43(3) 3_656 3_656 ?
O2 K1 K1 40.35(4) . 3_656 ?
O2 K1 K1 76.03(4) 3_556 3_656 ?
O5 K1 K1 112.89(4) 1_455 3_656 ?
K1 K1 K1 67.253(15) 1_655 3_656 ?
K1 K1 K1 112.748(15) 1_455 3_656 ?
O5 K1 K1 113.95(5) . 3_556 ?
O6 K1 K1 109.34(5) . 3_556 ?
O4 K1 K1 102.93(4) 3_656 3_556 ?
O6 K1 K1 161.52(5) 1_655 3_556 ?
O2 K1 K1 78.96(4) 3_656 3_556 ?
O2 K1 K1 38.97(4) . 3_556 ?
O2 K1 K1 37.89(3) 3_556 3_556 ?
O5 K1 K1 78.00(4) 1_455 3_556 ?
K1 K1 K1 117.724(15) 1_655 3_556 ?
K1 K1 K1 62.277(15) 1_455 3_556 ?
K1 K1 K1 50.470(17) 3_656 3_556 ?
O5 K1 H3 99.5(8) . . ?
O6 K1 H3 16.7(7) . . ?
O4 K1 H3 85.3(7) 3_656 . ?
O6 K1 H3 72.9(7) 1_655 . ?
O2 K1 H3 143.2(7) 3_656 . ?
O2 K1 H3 135.4(7) . . ?
O2 K1 H3 98.3(8) 3_556 . ?
O5 K1 H3 62.9(6) 1_455 . ?
K1 K1 H3 119.4(7) 1_655 . ?
K1 K1 H3 60.6(7) 1_455 . ?
K1 K1 H3 173.3(7) 3_656 . ?
K1 K1 H3 122.8(7) 3_556 . ?
O5 K1 H4 122.8(7) . . ?
O6 K1 H4 12.3(7) . . ?
O4 K1 H4 65.8(7) 3_656 . ?
O6 K1 H4 79.0(7) 1_655 . ?
O2 K1 H4 125.2(7) 3_656 . ?
O2 K1 H4 141.0(7) . . ?
O2 K1 H4 78.8(7) 3_556 . ?
O5 K1 H4 76.6(7) 1_455 . ?
K1 K1 H4 125.7(7) 1_655 . ?
K1 K1 H4 54.3(7) 1_455 . ?
K1 K1 H4 152.7(7) 3_656 . ?
K1 K1 H4 111.4(7) 3_556 . ?
H3 K1 H4 24.1(9) . . ?
C1 O1 Cu1 113.07(15) . . ?
C1 O2 K1 119.07(15) . 3_656 ?
C1 O2 K1 127.60(15) . . ?
K1 O2 K1 99.22(5) 3_656 . ?
C1 O2 K1 115.72(15) . 3_556 ?
K1 O2 K1 81.94(5) 3_656 3_556 ?
K1 O2 K1 103.15(6) . 3_556 ?
C2 O3 Cu1 112.82(15) . . ?
C2 O4 K1 119.94(15) . 3_656 ?
O2 C1 O1 125.7(2) . . ?
O2 C1 C2 120.3(2) . . ?
O1 C1 C2 114.0(2) . . ?
O4 C2 O3 125.5(2) . . ?
O4 C2 C1 119.9(2) . . ?
O3 C2 C1 114.6(2) . . ?
K1 O5 K1 80.57(5) . 1_655 ?
K1 O5 H1 130(2) . . ?
K1 O5 H1 86(2) 1_655 . ?
K1 O5 H2 126(2) . . ?
K1 O5 H2 90(2) 1_655 . ?
H1 O5 H2 102(3) . . ?
K1 O6 K1 83.98(6) . 1_455 ?
K1 O6 H3 95(2) . . ?
K1 O6 H3 133(2) 1_455 . ?
K1 O6 H4 105(3) . . ?
K1 O6 H4 116(3) 1_455 . ?
H3 O6 H4 110(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H1 O1 0.79(4) 2.07(4) 2.849(3) 169(3) 1_655
O5 H2 O4 0.82(4) 1.99(4) 2.808(3) 172(4) 2_655
O6 H3 O3 0.86(4) 2.02(4) 2.875(3) 174(3) 2
O6 H4 O5 0.66(4) 2.44(4) 3.049(3) 155(4) 4_566

_refine_diff_density_max         0.421
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.080

