# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_compound-1
_database_code_depnum_ccdc_archive 'CCDC 1901745'
loop_
_audit_author_name
_audit_author_address
'Wei-Wei Xiong'
;Nanjing Tech University (NanjingTech)
China
;
_audit_update_record             
;
2019-04-28 deposited with the CCDC.	2019-06-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H9 N2 O6 Zn-, (H4 N)+, H2O'
_chemical_formula_sum            'C9 H11 N3 O7 Zn'
_chemical_formula_weight         338.58

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_H-M_alt        'C m c m'
_space_group_name_Hall           '-C 2c 2'

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

_cell_length_a                   10.1186(5)
_cell_length_b                   19.0860(10)
_cell_length_c                   6.9839(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1348.76(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2157
_cell_measurement_theta_min      3.6020
_cell_measurement_theta_max      28.0380

_exptl_crystal_description       plate-like
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_F_000             688
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    1.856
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.03794
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5264
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.615
_diffrn_reflns_theta_max         29.121
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             970
_reflns_number_gt                888
_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       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND. Version 3.0. Crystal Impact'
_computing_publication_material  'Windows Word 2010'
_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)+(0.0472P)²+2.5034P] 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         970
_refine_ls_number_parameters     83
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0395
_refine_ls_wR_factor_ref         0.0965
_refine_ls_wR_factor_gt          0.0927
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001

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
Zn1 Zn 0.000000 -0.05467(3) 0.750000 0.0260(2) Uani 1 4 d S T P . .
C1 C -0.500000 0.2129(3) 0.750000 0.0351(12) Uani 1 4 d S T P . .
C2 C -0.500000 -0.0121(2) 0.750000 0.0231(9) Uani 1 4 d S T P . .
C3 C -0.3810(3) 0.02335(16) 0.750000 0.0244(6) Uani 1 2 d S T P . .
C4 C -0.3816(3) 0.09649(17) 0.750000 0.0285(7) Uani 1 2 d S T P . .
C5 C -0.500000 0.1334(2) 0.750000 0.0287(10) Uani 1 4 d S T P . .
C6 C -0.2541(3) -0.01716(17) 0.750000 0.0273(7) Uani 1 2 d S T P . .
O1 O -0.1463(2) 0.01699(12) 0.750000 0.0306(5) Uani 1 2 d S T P . .
O2 O -0.2571(3) -0.08206(13) 0.750000 0.0493(8) Uani 1 2 d S T P . .
O3 O -0.4058(4) 0.24299(17) 0.6677(6) 0.0483(11) Uani 0.5 1 d . . P . .
N1 N 0.000000 -0.1154(2) 0.5169(5) 0.0380(8) Uani 1 2 d S T P . .
N2 N -0.3584(4) 0.2153(2) 0.250000 0.100(2) Uani 0.5 2 d S T P . .
O4 O -0.3584(4) 0.2153(2) 0.250000 0.100(2) Uani 0.5 2 d DS T P . .
H2 H -0.500000 -0.061(4) 0.750000 0.07(2) Uiso 1 4 d S . P . .
H4 H -0.306(4) 0.124(2) 0.750000 0.035(10) Uiso 1 2 d S . P . .
H4A H -0.275(3) 0.234(3) 0.250000 0.11(2) Uiso 1 2 d DS . P . .
H1A H 0.000000 -0.152(3) 0.548(8) 0.054(16) Uiso 1 2 d S . P . .
H1B H -0.056(4) -0.106(2) 0.436(6) 0.102(17) 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
Zn1 N1 1.999(3) . ?
Zn1 N1 1.999(3) 10_557 ?
Zn1 O1 2.016(2) 3_556 ?
Zn1 O1 2.016(2) . ?
C1 O3 1.253(4) . ?
C1 O3 1.253(4) 10_557 ?
C1 O3 1.253(4) 12_455 ?
C1 O3 1.253(4) 3_456 ?
C1 C5 1.516(6) . ?
C2 C3 1.381(4) . ?
C2 C3 1.381(4) 3_456 ?
C3 C4 1.396(4) . ?
C3 C6 1.499(4) . ?
C4 C5 1.391(4) . ?
C6 O2 1.239(4) . ?
C6 O1 1.270(4) . ?
O3 O3 1.150(9) 10_557 ?

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 Zn1 N1 109.1(2) . 10_557 ?
N1 Zn1 O1 113.18(8) . 3_556 ?
N1 Zn1 O1 113.18(8) 10_557 3_556 ?
N1 Zn1 O1 113.18(8) . . ?
N1 Zn1 O1 113.18(8) 10_557 . ?
O1 Zn1 O1 94.55(13) 3_556 . ?
O3 C1 O3 54.7(4) . 10_557 ?
O3 C1 O3 99.1(4) . 12_455 ?
O3 C1 O3 125.4(5) 10_557 12_455 ?
O3 C1 O3 125.4(5) . 3_456 ?
O3 C1 O3 99.1(4) 10_557 3_456 ?
O3 C1 O3 54.7(4) 12_455 3_456 ?
O3 C1 C5 117.3(3) . . ?
O3 C1 C5 117.3(3) 10_557 . ?
O3 C1 C5 117.3(3) 12_455 . ?
O3 C1 C5 117.3(3) 3_456 . ?
C3 C2 C3 121.3(4) . 3_456 ?
C2 C3 C4 119.2(3) . . ?
C2 C3 C6 119.6(3) . . ?
C4 C3 C6 121.3(3) . . ?
C5 C4 C3 120.7(3) . . ?
C4 C5 C4 119.1(4) 3_456 . ?
C4 C5 C1 120.5(2) 3_456 . ?
C4 C5 C1 120.5(2) . . ?
O2 C6 O1 122.3(3) . . ?
O2 C6 C3 119.6(3) . . ?
O1 C6 C3 118.1(3) . . ?
C6 O1 Zn1 106.40(19) . . ?
O3 O3 C1 62.7(2) 10_557 . ?

_refine_diff_density_max         0.587
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.083

####################################################################### 
# 
# 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_compound-7
_database_code_depnum_ccdc_archive 'CCDC 1901751'
loop_
_audit_author_name
_audit_author_address
'Wei-Wei Xiong'
;Nanjing Tech University (NanjingTech)
China
;
_audit_update_record             
;
2019-04-28 deposited with the CCDC.	2019-06-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C9 H3 O6) 2(C H4 N2 O) Co3, 2(H2O)'
_chemical_formula_sum            'C20 H18 Co3 N4 O16'
_chemical_formula_weight         747.17

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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                   8.076(2)
_cell_length_b                   9.409(2)
_cell_length_c                   9.653(2)
_cell_angle_alpha                63.445(7)
_cell_angle_beta                 87.358(8)
_cell_angle_gamma                68.411(7)
_cell_volume                     603.9(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    299(2)
_cell_measurement_reflns_used    5615
_cell_measurement_theta_min      2.952
_cell_measurement_theta_max      27.423

_exptl_crystal_description       prism
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.055
_exptl_crystal_F_000             375
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    2.131
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6761
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      299(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8695
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.969
_diffrn_reflns_theta_max         27.736
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2807
_reflns_number_gt                2066
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND. Version 3.0. Crystal Impact'
_computing_publication_material  'Windows Word 2010'
_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)+(0.0238P)²+0.4920P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2807
_refine_ls_number_parameters     211
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0356
_refine_ls_wR_factor_ref         0.0701
_refine_ls_wR_factor_gt          0.0632
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_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
Co1 Co 0.000000 1.000000 1.000000 0.01203(14) Uani 1 2 d S . P . .
Co2 Co -0.26820(5) 1.26555(5) 0.68346(4) 0.01322(12) Uani 1 1 d . . . . .
O1 O -0.2371(3) 1.3758(2) 0.4558(2) 0.0203(5) Uani 1 1 d . . . . .
O2 O 0.0202(2) 1.1273(2) 0.7583(2) 0.0146(4) Uani 1 1 d . . . . .
O3 O 0.2616(2) 0.9502(2) 1.0943(2) 0.0133(4) Uani 1 1 d . . . . .
O4 O 0.1085(3) 0.7758(2) 0.9927(2) 0.0180(5) Uani 1 1 d . . . . .
O5 O -0.2682(3) 1.0190(2) 0.6943(2) 0.0185(5) Uani 1 1 d . . . . .
O6 O -0.2677(3) 1.4277(2) 0.7727(2) 0.0191(5) Uani 1 1 d . . . . .
O7 O -0.5455(3) 1.3640(2) 0.6223(2) 0.0174(5) Uani 1 1 d . . . . .
C1 C 0.2579(4) 1.5442(4) 0.8726(3) 0.0152(6) Uani 1 1 d . . . . .
C2 C 0.2669(4) 1.0404(3) 1.1619(3) 0.0125(6) Uani 1 1 d . . . . .
C3 C 0.2343(4) 1.4939(3) 1.0295(3) 0.0133(6) Uani 1 1 d . . . . .
C4 C -0.3341(4) 1.5253(4) 0.3515(3) 0.0136(6) Uani 1 1 d . . . . .
C5 C 0.2706(4) 1.2143(3) 1.0630(3) 0.0125(6) Uani 1 1 d . . . . .
C6 C 0.3040(4) 1.2626(4) 0.9095(3) 0.0138(6) Uani 1 1 d . . . . .
C7 C 0.2387(4) 1.3300(4) 1.1237(3) 0.0133(6) Uani 1 1 d . . . . .
C8 C 0.2007(4) 0.6229(3) 1.0899(3) 0.0135(6) Uani 1 1 d . . . . .
N1 N 0.3095(3) 0.9660(3) 0.7617(3) 0.0266(7) Uani 1 1 d . . . . .
H2B H 0.334571 0.935549 0.858991 0.032 Uiso 1 1 calc R U . . .
H2C H 0.391842 0.928577 0.712473 0.032 Uiso 1 1 calc R U . . .
C9 C 0.2978(4) 1.4274(3) 0.8137(3) 0.0123(6) Uani 1 1 d . . . . .
C10 C 0.1441(4) 1.0705(4) 0.6876(3) 0.0193(7) Uani 1 1 d . . . . .
N2 N 0.1103(4) 1.1140(4) 0.5385(3) 0.0464(9) Uani 1 1 d . . . . .
H1A H 0.003854 1.181328 0.488089 0.056 Uiso 1 1 calc R U . . .
H1B H 0.194792 1.074985 0.491670 0.056 Uiso 1 1 calc R U . . .
O8 O 0.4785(4) 0.1979(4) 0.4161(3) 0.0410(8) Uani 1 1 d . . . . .
H5 H 0.326(5) 1.186(5) 0.873(4) 0.049 Uiso 1 1 d . U . . .
H4 H 0.214(5) 1.299(5) 1.224(4) 0.049 Uiso 1 1 d . U . . .
H10 H 0.253(5) 1.658(5) 0.805(4) 0.049 Uiso 1 1 d . U . . .
H1C H 0.527(6) 0.162(5) 0.495(5) 0.049 Uiso 1 1 d . U . . .
H1D H 0.429(6) 0.298(5) 0.377(5) 0.049 Uiso 1 1 d . 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
Co1 O4 1.9973(19) 2_577 ?
Co1 O4 1.9973(19) . ?
Co1 O2 2.1247(19) . ?
Co1 O2 2.1247(19) 2_577 ?
Co1 O3 2.140(2) . ?
Co1 O3 2.140(2) 2_577 ?
Co2 O1 2.0177(19) . ?
Co2 O6 2.0620(19) . ?
Co2 O7 2.081(2) . ?
Co2 O2 2.174(2) . ?
Co2 O3 2.1822(19) 2_577 ?
Co2 O5 2.275(2) . ?
O1 C4 1.266(3) . ?
O2 C10 1.274(3) . ?
O3 C2 1.293(3) . ?
O4 C8 1.254(3) . ?
O5 C2 1.242(3) 2_577 ?
O6 C8 1.261(3) 2_577 ?
O7 C4 1.249(3) 2_486 ?
C1 C9 1.384(4) . ?
C1 C3 1.397(4) . ?
C2 C5 1.492(4) . ?
C3 C7 1.384(4) . ?
C3 C8 1.505(4) 1_565 ?
C4 C9 1.498(4) 2_586 ?
C5 C6 1.388(4) . ?
C5 C7 1.394(4) . ?
C6 C9 1.388(4) . ?
N1 C10 1.325(4) . ?
C10 N2 1.319(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
O4 Co1 O4 180.0 2_577 . ?
O4 Co1 O2 91.45(7) 2_577 . ?
O4 Co1 O2 88.55(7) . . ?
O4 Co1 O2 88.55(7) 2_577 2_577 ?
O4 Co1 O2 91.45(7) . 2_577 ?
O2 Co1 O2 180.0 . 2_577 ?
O4 Co1 O3 92.29(8) 2_577 . ?
O4 Co1 O3 87.71(8) . . ?
O2 Co1 O3 98.62(7) . . ?
O2 Co1 O3 81.38(7) 2_577 . ?
O4 Co1 O3 87.71(8) 2_577 2_577 ?
O4 Co1 O3 92.29(8) . 2_577 ?
O2 Co1 O3 81.38(7) . 2_577 ?
O2 Co1 O3 98.62(7) 2_577 2_577 ?
O3 Co1 O3 180.0 . 2_577 ?
O1 Co2 O6 107.60(8) . . ?
O1 Co2 O7 90.51(8) . . ?
O6 Co2 O7 96.62(8) . . ?
O1 Co2 O2 92.59(8) . . ?
O6 Co2 O2 89.51(8) . . ?
O7 Co2 O2 171.96(7) . . ?
O1 Co2 O3 154.22(8) . 2_577 ?
O6 Co2 O3 96.87(8) . 2_577 ?
O7 Co2 O3 94.71(7) . 2_577 ?
O2 Co2 O3 79.35(7) . 2_577 ?
O1 Co2 O5 96.51(8) . . ?
O6 Co2 O5 155.71(7) . . ?
O7 Co2 O5 85.82(8) . . ?
O2 Co2 O5 86.46(7) . . ?
O3 Co2 O5 58.85(7) 2_577 . ?
C4 O1 Co2 126.66(18) . . ?
C10 O2 Co1 126.33(17) . . ?
C10 O2 Co2 129.99(18) . . ?
Co1 O2 Co2 95.17(7) . . ?
C2 O3 Co1 115.99(17) . . ?
C2 O3 Co2 92.22(16) . 2_577 ?
Co1 O3 Co2 94.47(7) . 2_577 ?
C8 O4 Co1 135.11(19) . . ?
C2 O5 Co2 89.31(16) 2_577 . ?
C8 O6 Co2 124.25(18) 2_577 . ?
C4 O7 Co2 128.93(18) 2_486 . ?
C9 C1 C3 120.4(3) . . ?
O5 C2 O3 119.6(2) 2_577 . ?
O5 C2 C5 122.0(2) 2_577 . ?
O3 C2 C5 118.4(2) . . ?
C7 C3 C1 119.8(3) . . ?
C7 C3 C8 121.9(2) . 1_565 ?
C1 C3 C8 118.3(2) . 1_565 ?
O7 C4 O1 124.5(3) 2_486 . ?
O7 C4 C9 118.3(2) 2_486 2_586 ?
O1 C4 C9 117.2(2) . 2_586 ?
C6 C5 C7 119.6(3) . . ?
C6 C5 C2 120.2(2) . . ?
C7 C5 C2 120.2(2) . . ?
C9 C6 C5 120.7(3) . . ?
C3 C7 C5 120.0(3) . . ?
O4 C8 O6 126.1(3) . 2_577 ?
O4 C8 C3 114.5(2) . 1_545 ?
O6 C8 C3 119.4(2) 2_577 1_545 ?
C1 C9 C6 119.3(3) . . ?
C1 C9 C4 121.5(2) . 2_586 ?
C6 C9 C4 119.1(2) . 2_586 ?
O2 C10 N2 120.6(3) . . ?
O2 C10 N1 121.0(3) . . ?
N2 C10 N1 118.4(3) . . ?

_refine_diff_density_max         0.449
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.100

####################################################################### 
# 
# 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_compound-5
_database_code_depnum_ccdc_archive 'CCDC 1901749'
loop_
_audit_author_name
_audit_author_address
'Wei-Wei Xiong'
;Nanjing Tech University (NanjingTech)
China
;
_audit_update_record             
;
2019-04-28 deposited with the CCDC.	2019-06-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C9 H3 O6 Mn)-, H4 N+, H2O'
_chemical_formula_sum            'C9 H9 Mn N O7'
_chemical_formula_weight         298.11

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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                   7.0734(5)
_cell_length_b                   9.6325(7)
_cell_length_c                   15.3798(11)
_cell_angle_alpha                90
_cell_angle_beta                 94.408(2)
_cell_angle_gamma                90
_cell_volume                     1044.80(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2566
_cell_measurement_theta_min      3.085
_cell_measurement_theta_max      27.555

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.895
_exptl_crystal_F_000             604
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    1.293
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6660
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14227
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.085
_diffrn_reflns_theta_max         27.591
_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             2418
_reflns_number_gt                2119
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND. Version 3.0. Crystal Impact'
_computing_publication_material  'Windows Word 2010'
_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)+(0.0419P)²+0.3764P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2418
_refine_ls_number_parameters     199
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0251
_refine_ls_wR_factor_ref         0.0680
_refine_ls_wR_factor_gt          0.0641
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_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
Mn1 Mn 0.08638(3) 0.59359(2) 0.36072(2) 0.01635(9) Uani 1 1 d . . . . .
N1 N -0.0641(2) 0.87267(17) 0.16837(10) 0.0249(3) Uani 1 1 d . . . . .
O2 O 0.15897(18) 0.77397(11) 0.43112(8) 0.0247(3) Uani 1 1 d . . . . .
O3 O 0.3149(2) 0.64470(15) 0.27686(9) 0.0315(3) Uani 1 1 d . . . . .
O4 O -0.10481(19) 0.61286(12) 0.23666(7) 0.0264(3) Uani 1 1 d . . . . .
O5 O -0.15814(15) 0.53661(11) 0.43275(7) 0.0187(2) Uani 1 1 d . . . . .
O6 O 0.11163(19) -0.05829(13) 0.33264(8) 0.0295(3) Uani 1 1 d . . . . .
O7 O 0.25551(16) 0.44191(11) 0.43347(7) 0.0207(2) Uani 1 1 d . . . . .
O8 O 0.00688(19) 0.40390(12) 0.26425(8) 0.0260(3) Uani 1 1 d . . . . .
C1 C 0.1622(2) -0.10128(15) 0.40763(10) 0.0169(3) Uani 1 1 d . . . . .
C2 C 0.2923(2) -0.03951(16) 0.55926(10) 0.0174(3) Uani 1 1 d . . . . .
C3 C 0.3258(2) 0.19807(16) 0.60651(10) 0.0165(3) Uani 1 1 d . . . . .
C4 C 0.2229(2) 0.39334(15) 0.50699(10) 0.0145(3) Uani 1 1 d . . . . .
C5 C 0.2147(2) 0.14585(16) 0.45813(10) 0.0169(3) Uani 1 1 d . . . . .
C6 C -0.1536(2) 0.44284(16) 0.12428(10) 0.0162(3) Uani 1 1 d . . . . .
C7 C 0.2604(2) 0.24225(15) 0.52351(10) 0.0155(3) Uani 1 1 d . . . . .
C8 C -0.0796(2) 0.48833(16) 0.21350(10) 0.0181(3) Uani 1 1 d . . . . .
C9 C 0.2271(2) 0.00389(15) 0.47629(10) 0.0162(3) Uani 1 1 d . . . . .
H3 H 0.350(3) 0.2626(19) 0.6499(12) 0.018(4) Uiso 1 1 d . . . . .
H5 H 0.166(3) 0.176(2) 0.4015(12) 0.021(5) Uiso 1 1 d . . . . .
H2 H 0.289(3) -0.137(2) 0.5719(12) 0.026(5) Uiso 1 1 d . . . . .
H1A H -0.091(3) 0.780(3) 0.1781(15) 0.040(6) Uiso 1 1 d . . . . .
H1B H -0.025(4) 0.909(3) 0.2230(18) 0.054(7) Uiso 1 1 d . . . . .
H3A H 0.336(3) 0.589(3) 0.2316(17) 0.046(7) Uiso 1 1 d . . . . .
H3B H 0.356(4) 0.726(3) 0.2670(17) 0.058(8) Uiso 1 1 d . . . . .
H1C H 0.030(4) 0.880(2) 0.1344(16) 0.040(6) Uiso 1 1 d . . . . .
H1D H -0.171(4) 0.919(3) 0.1378(18) 0.055(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
Mn1 O2 2.0903(11) . ?
Mn1 O7 2.1475(11) . ?
Mn1 O5 2.1942(11) . ?
Mn1 O3 2.1999(13) . ?
Mn1 O4 2.2599(12) . ?
Mn1 O8 2.3932(12) . ?
O2 C1 1.2556(19) 1_565 ?
O4 C8 1.2677(19) . ?
O5 C4 1.2607(19) 3_566 ?
O6 C1 1.2513(19) . ?
O7 C4 1.2612(18) . ?
O8 C8 1.2537(19) . ?
C1 C9 1.509(2) . ?
C2 C9 1.388(2) . ?
C2 C6 1.398(2) 4_666 ?
C3 C6 1.390(2) 4_666 ?
C3 C7 1.391(2) . ?
C4 C7 1.498(2) . ?
C5 C7 1.388(2) . ?
C5 C9 1.397(2) . ?
C6 C8 1.496(2) . ?

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 Mn1 O7 101.00(5) . . ?
O2 Mn1 O5 96.78(4) . . ?
O7 Mn1 O5 89.77(4) . . ?
O2 Mn1 O3 87.44(5) . . ?
O7 Mn1 O3 93.02(5) . . ?
O5 Mn1 O3 174.41(5) . . ?
O2 Mn1 O4 118.44(4) . . ?
O7 Mn1 O4 140.27(4) . . ?
O5 Mn1 O4 90.17(4) . . ?
O3 Mn1 O4 84.59(5) . . ?
O2 Mn1 O8 172.92(4) . . ?
O7 Mn1 O8 84.18(4) . . ?
O5 Mn1 O8 88.01(4) . . ?
O3 Mn1 O8 87.46(5) . . ?
O4 Mn1 O8 56.11(4) . . ?
C1 O2 Mn1 130.97(10) 1_565 . ?
C8 O4 Mn1 94.11(9) . . ?
C4 O5 Mn1 125.61(10) 3_566 . ?
C4 O7 Mn1 125.91(10) . . ?
C8 O8 Mn1 88.33(9) . . ?
O6 C1 O2 124.87(14) . 1_545 ?
O6 C1 C9 118.21(14) . . ?
O2 C1 C9 116.89(13) 1_545 . ?
C9 C2 C6 120.70(14) . 4_666 ?
C6 C3 C7 120.11(14) 4_666 . ?
O5 C4 O7 124.22(13) 3_566 . ?
O5 C4 C7 117.71(13) 3_566 . ?
O7 C4 C7 118.06(13) . . ?
C7 C5 C9 120.16(14) . . ?
C3 C6 C2 119.40(14) 4_565 4_565 ?
C3 C6 C8 119.36(14) 4_565 . ?
C2 C6 C8 121.21(14) 4_565 . ?
C5 C7 C3 120.17(14) . . ?
C5 C7 C4 119.92(13) . . ?
C3 C7 C4 119.69(13) . . ?
O8 C8 O4 120.75(14) . . ?
O8 C8 C6 120.04(14) . . ?
O4 C8 C6 119.21(14) . . ?
C2 C9 C5 119.34(14) . . ?
C2 C9 C1 120.20(13) . . ?
C5 C9 C1 120.41(13) . . ?

_refine_diff_density_max         0.337
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.065

####################################################################### 
# 
# 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_compound-6
_database_code_depnum_ccdc_archive 'CCDC 1901750'
loop_
_audit_author_name
_audit_author_address
'Wei-Wei Xiong'
;Nanjing Tech University (NanjingTech)
China
;
_audit_update_record             
;
2019-04-28 deposited with the CCDC.	2019-06-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '[3(C9 H3 O6) Mn3]-, (C H4 N)+, H2O'
_chemical_formula_sum            'C28 H11 Cl0 Mn3 N O20'
_chemical_formula_weight         846.20

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/c'
_space_group_name_Hall           '-P 2yc'

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

_cell_length_a                   9.7273(11)
_cell_length_b                   12.8613(14)
_cell_length_c                   14.2241(17)
_cell_angle_alpha                90
_cell_angle_beta                 109.652(13)
_cell_angle_gamma                90
_cell_volume                     1675.9(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1614
_cell_measurement_theta_min      3.1010
_cell_measurement_theta_max      23.4290

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_F_000             842
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_absorpt_coefficient_mu    1.200
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.73214
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11652
_diffrn_reflns_av_unetI/netI     0.1316
_diffrn_reflns_av_R_equivalents  0.0991
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.730
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3695
_reflns_number_gt                2466
_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       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND. Version 3.0. Crystal Impact'
_computing_publication_material  'Windows Word 2010'
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0923P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3695
_refine_ls_number_parameters     243
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_gt           0.0830
_refine_ls_wR_factor_ref         0.2109
_refine_ls_wR_factor_gt          0.1881
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.210
_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
Mn1 Mn 1.000000 0.500000 0.500000 0.0183(4) Uani 1 2 d S . P . .
Mn2 Mn 1.05840(12) 0.72882(9) 0.64903(7) 0.0205(3) Uani 1 1 d . . . . .
C1 C 0.5291(9) 0.4057(7) 0.6214(6) 0.035(2) Uani 1 1 d . . . . .
C2 C 1.0098(8) 0.1024(6) 0.6670(5) 0.0286(18) Uani 1 1 d . . . . .
H4A H 1.015217 0.066290 0.611713 0.034 Uiso 1 1 calc R U . . .
C3 C 0.4118(8) 0.4652(7) 0.6236(5) 0.0292(18) Uani 1 1 d . . . . .
H5A H 0.325262 0.432540 0.620947 0.035 Uiso 1 1 calc R U . . .
C4 C 1.0165(9) 0.2713(6) 0.5782(5) 0.0284(17) Uani 1 1 d . . . . .
C5 C 0.6576(8) 0.4535(7) 0.6255(6) 0.0321(19) Uani 1 1 d . . . . .
H9A H 0.735616 0.413734 0.621923 0.038 Uiso 1 1 calc R U . . .
C6 C 1.0114(9) 0.2104(6) 0.6680(5) 0.0267(18) Uani 1 1 d . . . . .
C7 C 0.6713(8) 0.5608(7) 0.6349(5) 0.0259(18) Uani 1 1 d . . . . .
C8 C 0.4207(7) 0.5707(6) 0.6297(5) 0.0227(16) Uani 1 1 d . . . . .
C9 C 1.000000 0.0482(9) 0.750000 0.028(2) Uani 1 2 d S T P . .
C10 C 0.2915(8) 0.6335(7) 0.6316(5) 0.0250(17) Uani 1 1 d . . . . .
C11 C 0.5506(8) 0.6199(6) 0.6375(5) 0.0263(17) Uani 1 1 d . . . . .
H19A H 0.558161 0.691755 0.644276 0.032 Uiso 1 1 calc R U . . .
C12 C 1.000000 0.2642(8) 0.750000 0.021(2) Uani 1 2 d S T P . .
H21A H 1.000001 0.336517 0.750001 0.026 Uiso 1 2 calc R U P . .
C13 C 1.000000 -0.0693(8) 0.750000 0.028(2) Uani 1 2 d S TU P . .
C14 C 0.8103(8) 0.6116(7) 0.6364(5) 0.0281(18) Uani 1 1 d . . . . .
C15 C 0.5148(12) 0.2931(9) 0.6094(10) 0.067(3) Uani 1 1 d . . . . .
O1 O 0.8783(6) 0.5714(5) 0.5862(5) 0.0448(17) Uani 1 1 d . . . . .
O2 O 0.1712(6) 0.5863(5) 0.6175(4) 0.0319(13) Uani 1 1 d . . . . .
O3 O 0.8526(6) 0.6943(5) 0.6851(4) 0.0362(14) Uani 1 1 d . . . . .
O4 O 1.0264(7) 0.3677(4) 0.5892(4) 0.0422(15) Uani 1 1 d . U . . .
O5 O 1.0119(6) 0.2206(4) 0.5020(3) 0.0303(12) Uani 1 1 d . . . . .
O6 O 0.9545(6) -0.1134(4) 0.8123(4) 0.0369(14) Uani 1 1 d . . . . .
O7 O 0.3026(6) 0.7289(5) 0.6512(4) 0.0363(13) Uani 1 1 d . . . . .
O8 O 0.2544(15) 0.0839(14) 0.5122(13) 0.217(8) Uani 1 1 d D . . . .
H8 H 0.288781 0.027992 0.553775 0.325 Uiso 1 1 d DR U . . .
O9 O 0.3898(12) 0.2552(8) 0.5970(12) 0.145(5) Uani 1 1 d . . . . .
O10 O 0.6176(11) 0.2397(7) 0.6070(10) 0.122(4) Uani 1 1 d . . . . .
N1A N 0.328(3) 0.095(2) 0.0411(19) 0.121(11) Uani 0.25 1 d D . P A 1
N1B N 0.328(3) 0.095(2) 0.0411(19) 0.121(11) Uani 0.25 1 d D . P B 2
C16A C 0.417(7) 0.045(5) 0.138(3) 0.27(3) Uiso 0.25 1 d D U P A 1
C16B C 0.417(7) 0.045(5) 0.138(3) 0.27(3) Uiso 0.25 1 d D U P B 2


_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
Mn1 O4 2.085(5) . ?
Mn1 O4 2.085(5) 3_766 ?
Mn1 O1 2.173(5) . ?
Mn1 O1 2.173(5) 3_766 ?
Mn1 O2 2.219(5) 1_655 ?
Mn1 O2 2.219(5) 3_666 ?
Mn2 O6 2.117(5) 2_766 ?
Mn2 O5 2.125(5) 3_766 ?
Mn2 O2 2.258(6) 1_655 ?
Mn2 O3 2.267(5) 2_756 ?
Mn2 O3 2.271(5) . ?
Mn2 O7 2.365(5) 1_655 ?
C1 C5 1.377(11) . ?
C1 C3 1.384(11) . ?
C1 C15 1.459(13) . ?
C2 C6 1.390(11) . ?
C2 C9 1.401(9) . ?
C2 H4A 0.9300 . ?
C3 C8 1.360(11) . ?
C3 H5A 0.9300 . ?
C4 O4 1.249(9) . ?
C4 O5 1.253(9) . ?
C4 C6 1.513(10) . ?
C5 C7 1.389(12) . ?
C5 H9A 0.9300 . ?
C6 C12 1.392(9) . ?
C7 C11 1.409(10) . ?
C7 C14 1.496(10) . ?
C8 C11 1.384(10) . ?
C8 C10 1.502(10) . ?
C9 C13 1.511(15) . ?
C10 O7 1.254(10) . ?
C10 O2 1.273(9) . ?
C11 H19A 0.9300 . ?
C12 H21A 0.9300 . ?
C13 O6 1.251(7) 2_756 ?
C13 O6 1.251(7) . ?
C14 O1 1.238(9) . ?
C14 O3 1.261(9) . ?
C15 O10 1.223(13) . ?
C15 O9 1.266(14) . ?
O8 H8 0.9200 . ?
N1A C16A 1.507(7) . ?
N1B C16B 1.507(7) . ?

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
O4 Mn1 O4 180.0 . 3_766 ?
O4 Mn1 O1 88.9(2) . . ?
O4 Mn1 O1 91.1(2) 3_766 . ?
O4 Mn1 O1 91.1(2) . 3_766 ?
O4 Mn1 O1 88.9(2) 3_766 3_766 ?
O1 Mn1 O1 180.0 . 3_766 ?
O4 Mn1 O2 92.4(2) . 1_655 ?
O4 Mn1 O2 87.6(2) 3_766 1_655 ?
O1 Mn1 O2 77.1(2) . 1_655 ?
O1 Mn1 O2 102.9(2) 3_766 1_655 ?
O4 Mn1 O2 87.6(2) . 3_666 ?
O4 Mn1 O2 92.4(2) 3_766 3_666 ?
O1 Mn1 O2 102.9(2) . 3_666 ?
O1 Mn1 O2 77.1(2) 3_766 3_666 ?
O2 Mn1 O2 180.0 1_655 3_666 ?
O6 Mn2 O5 86.7(2) 2_766 3_766 ?
O6 Mn2 O2 154.8(2) 2_766 1_655 ?
O5 Mn2 O2 93.5(2) 3_766 1_655 ?
O6 Mn2 O3 87.2(2) 2_766 2_756 ?
O5 Mn2 O3 172.9(2) 3_766 2_756 ?
O2 Mn2 O3 90.4(2) 1_655 2_756 ?
O6 Mn2 O3 89.7(2) 2_766 . ?
O5 Mn2 O3 106.2(2) 3_766 . ?
O2 Mn2 O3 114.2(2) 1_655 . ?
O3 Mn2 O3 77.5(2) 2_756 . ?
O6 Mn2 O7 98.3(2) 2_766 1_655 ?
O5 Mn2 O7 89.7(2) 3_766 1_655 ?
O2 Mn2 O7 56.6(2) 1_655 1_655 ?
O3 Mn2 O7 87.5(2) 2_756 1_655 ?
O3 Mn2 O7 162.7(2) . 1_655 ?
C5 C1 C3 119.7(8) . . ?
C5 C1 C15 119.8(8) . . ?
C3 C1 C15 120.3(8) . . ?
C6 C2 C9 119.5(7) . . ?
C6 C2 H4A 120.2 . . ?
C9 C2 H4A 120.2 . . ?
C8 C3 C1 121.2(7) . . ?
C8 C3 H5A 119.4 . . ?
C1 C3 H5A 119.4 . . ?
O4 C4 O5 127.1(7) . . ?
O4 C4 C6 115.5(6) . . ?
O5 C4 C6 117.3(7) . . ?
C1 C5 C7 120.2(7) . . ?
C1 C5 H9A 119.9 . . ?
C7 C5 H9A 119.9 . . ?
C2 C6 C12 120.1(7) . . ?
C2 C6 C4 120.8(7) . . ?
C12 C6 C4 119.0(7) . . ?
C5 C7 C11 119.0(7) . . ?
C5 C7 C14 119.5(7) . . ?
C11 C7 C14 121.4(8) . . ?
C3 C8 C11 119.9(7) . . ?
C3 C8 C10 120.2(7) . . ?
C11 C8 C10 119.9(7) . . ?
C2 C9 C2 120.3(10) 2_756 . ?
C2 C9 C13 119.8(5) 2_756 . ?
C2 C9 C13 119.8(5) . . ?
O7 C10 O2 120.5(7) . . ?
O7 C10 C8 121.4(7) . . ?
O2 C10 C8 118.0(7) . . ?
C8 C11 C7 119.9(8) . . ?
C8 C11 H19A 120.1 . . ?
C7 C11 H19A 120.1 . . ?
C6 C12 C6 120.4(10) 2_756 . ?
C6 C12 H21A 119.8 2_756 . ?
C6 C12 H21A 119.8 . . ?
O6 C13 O6 126.1(10) 2_756 . ?
O6 C13 C9 117.0(5) 2_756 . ?
O6 C13 C9 117.0(5) . . ?
O1 C14 O3 122.0(7) . . ?
O1 C14 C7 117.7(8) . . ?
O3 C14 C7 120.2(7) . . ?
O10 C15 O9 122.4(12) . . ?
O10 C15 C1 120.9(10) . . ?
O9 C15 C1 116.6(10) . . ?
C14 O1 Mn1 179.1(6) . . ?
C10 O2 Mn1 140.8(5) . 1_455 ?
C10 O2 Mn2 93.6(5) . 1_455 ?
Mn1 O2 Mn2 105.3(2) 1_455 1_455 ?
C14 O3 Mn2 132.6(5) . 2_756 ?
C14 O3 Mn2 101.0(5) . . ?
Mn2 O3 Mn2 98.0(2) 2_756 . ?
C4 O4 Mn1 138.2(5) . . ?
C4 O5 Mn2 128.4(5) . 3_766 ?
C13 O6 Mn2 133.2(6) . 2_746 ?
C10 O7 Mn2 89.2(4) . 1_455 ?

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 C1 C3 C8 0.1(12) . . . . ?
C15 C1 C3 C8 -176.7(9) . . . . ?
C3 C1 C5 C7 1.9(12) . . . . ?
C15 C1 C5 C7 178.8(9) . . . . ?
C9 C2 C6 C12 -1.4(11) . . . . ?
C9 C2 C6 C4 -177.8(6) . . . . ?
O4 C4 C6 C2 -175.8(8) . . . . ?
O5 C4 C6 C2 3.4(11) . . . . ?
O4 C4 C6 C12 7.7(10) . . . . ?
O5 C4 C6 C12 -173.0(6) . . . . ?
C1 C5 C7 C11 -1.7(11) . . . . ?
C1 C5 C7 C14 -178.3(7) . . . . ?
C1 C3 C8 C11 -2.4(11) . . . . ?
C1 C3 C8 C10 179.7(7) . . . . ?
C6 C2 C9 C2 0.7(5) . . . 2_756 ?
C6 C2 C9 C13 -179.3(5) . . . . ?
C3 C8 C10 O7 169.8(7) . . . . ?
C11 C8 C10 O7 -8.2(10) . . . . ?
C3 C8 C10 O2 -6.7(10) . . . . ?
C11 C8 C10 O2 175.3(6) . . . . ?
C3 C8 C11 C7 2.5(10) . . . . ?
C10 C8 C11 C7 -179.5(6) . . . . ?
C5 C7 C11 C8 -0.5(10) . . . . ?
C14 C7 C11 C8 176.0(6) . . . . ?
C2 C6 C12 C6 0.7(5) . . . 2_756 ?
C4 C6 C12 C6 177.2(8) . . . 2_756 ?
C2 C9 C13 O6 -162.3(5) 2_756 . . 2_756 ?
C2 C9 C13 O6 17.7(5) . . . 2_756 ?
C2 C9 C13 O6 17.7(5) 2_756 . . . ?
C2 C9 C13 O6 -162.3(5) . . . . ?
C5 C7 C14 O1 32.8(10) . . . . ?
C11 C7 C14 O1 -143.7(7) . . . . ?
C5 C7 C14 O3 -149.4(7) . . . . ?
C11 C7 C14 O3 34.2(10) . . . . ?
C5 C1 C15 O10 2.9(19) . . . . ?
C3 C1 C15 O10 179.8(12) . . . . ?
C5 C1 C15 O9 -173.7(12) . . . . ?
C3 C1 C15 O9 3.1(18) . . . . ?
O7 C10 O2 Mn1 117.3(8) . . . 1_455 ?
C8 C10 O2 Mn1 -66.1(10) . . . 1_455 ?
O7 C10 O2 Mn2 -2.4(7) . . . 1_455 ?
C8 C10 O2 Mn2 174.2(5) . . . 1_455 ?
O1 C14 O3 Mn2 -111.9(7) . . . 2_756 ?
C7 C14 O3 Mn2 70.4(9) . . . 2_756 ?
O1 C14 O3 Mn2 0.0(8) . . . . ?
C7 C14 O3 Mn2 -177.8(6) . . . . ?
O5 C4 O4 Mn1 15.6(14) . . . . ?
C6 C4 O4 Mn1 -165.2(6) . . . . ?
O4 C4 O5 Mn2 -25.0(12) . . . 3_766 ?
C6 C4 O5 Mn2 155.9(5) . . . 3_766 ?
O6 C13 O6 Mn2 4.2(3) 2_756 . . 2_746 ?
C9 C13 O6 Mn2 -175.8(3) . . . 2_746 ?
O2 C10 O7 Mn2 2.3(7) . . . 1_455 ?
C8 C10 O7 Mn2 -174.2(6) . . . 1_455 ?

_refine_diff_density_max         0.895
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.138


# start Validation Reply Form
_vrf_PLAT315_compound-6          
;
PROBLEM: Singly Bonded Carbon Detected (H-atoms Missing).       C16A Check 
RESPONSE: This alert is due to the non-assignment of the H-atoms 
bonded to protonated methylamine cations
;
_vrf_PLAT430_compound-6          
;
PROBLEM: Short Inter D...A Contact  O7       ..N1A      .       2.81 Ang.  
RESPONSE: This alert is due to the non-assignment of the H-atoms 
bonded to protonated methylamine cations
;
# 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_compound-2
_database_code_depnum_ccdc_archive 'CCDC 1901746'
loop_
_audit_author_name
_audit_author_address
'Wei-Wei Xiong'
;Nanjing Tech University (NanjingTech)
China
;
_audit_update_record             
;
2019-04-28 deposited with the CCDC.	2019-06-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H6 N2 O4 Cu'
_chemical_formula_sum            'C7 H6 Cu N2 O4'
_chemical_formula_weight         245.68

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'
Cu Cu 0.3201 1.2651 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

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

_cell_length_a                   7.7542(6)
_cell_length_b                   10.5032(6)
_cell_length_c                   9.6297(10)
_cell_angle_alpha                90
_cell_angle_beta                 92.624(7)
_cell_angle_gamma                90
_cell_volume                     783.46(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    716
_cell_measurement_theta_min      5.0670
_cell_measurement_theta_max      27.8360

_exptl_crystal_description       rod-like
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.083
_exptl_crystal_F_000             492
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    2.774
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.45471
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1806
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.880
_diffrn_reflns_theta_max         29.282
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.833
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.833
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.833
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             896
_reflns_number_gt                750
_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       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND. Version 3.0. Crystal Impact'
_computing_publication_material  'Windows Word 2010'
_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)+(0.0391P)²+0.2967P] 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         896
_refine_ls_number_parameters     66
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0335
_refine_ls_wR_factor_ref         0.0792
_refine_ls_wR_factor_gt          0.0731
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_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 0.250000 0.16506(4) 0.500000 0.02540(19) Uani 1 2 d S T P . .
O1 O 0.0080(3) 0.3520(2) 0.1859(2) 0.0372(6) Uani 1 1 d . . . . .
O2 O 0.0860(3) 0.1965(2) 0.3349(2) 0.0300(5) Uani 1 1 d . . . . .
N2 N 0.250000 -0.0206(3) 0.500000 0.0362(9) Uani 1 2 d S T P . .
H2B H 0.180858 -0.048868 0.430372 0.054 Uiso 0.5 1 calc R U P . .
H2C H 0.356789 -0.048868 0.489310 0.054 Uiso 0.5 1 calc R U P . .
H2D H 0.212353 -0.048868 0.580317 0.054 Uiso 0.5 1 calc R U P . .
N1 N 0.250000 0.3454(3) 0.500000 0.0196(7) Uani 1 2 d S T P . .
C1 C 0.250000 0.6030(4) 0.500000 0.0282(10) Uani 1 2 d S T P . .
H1 H 0.250000 0.691531 0.499999 0.034 Uiso 1 2 calc R U P . .
C2 C 0.1624(4) 0.5379(3) 0.3929(3) 0.0258(7) Uani 1 1 d . . . . .
H2 H 0.104221 0.581388 0.320896 0.031 Uiso 1 1 calc R U . . .
C3 C 0.1645(4) 0.4066(3) 0.3967(3) 0.0221(6) Uani 1 1 d . . . . .
C4 C 0.0769(4) 0.3132(3) 0.2954(3) 0.0253(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 N1 1.894(3) . ?
Cu1 N2 1.950(4) . ?
Cu1 O2 2.017(2) 2_556 ?
Cu1 O2 2.017(2) . ?
O1 C4 1.230(4) . ?
O2 C4 1.284(4) . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
N2 H2B 0.8900 2_556 ?
N2 H2C 0.8900 2_556 ?
N2 H2D 0.8900 2_556 ?
N1 C3 1.335(3) 2_556 ?
N1 C3 1.335(3) . ?
C1 C2 1.389(4) 2_556 ?
C1 C2 1.389(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.380(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.522(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 N2 180.0 . . ?
N1 Cu1 O2 80.59(6) . 2_556 ?
N2 Cu1 O2 99.41(6) . 2_556 ?
N1 Cu1 O2 80.59(6) . . ?
N2 Cu1 O2 99.41(6) . . ?
O2 Cu1 O2 161.17(12) 2_556 . ?
C4 O2 Cu1 114.43(19) . . ?
Cu1 N2 H2B 109.5 . . ?
Cu1 N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
Cu1 N2 H2D 109.5 . . ?
H2B N2 H2D 109.5 . . ?
H2C N2 H2D 109.5 . . ?
Cu1 N2 H2B 109.470(2) . 2_556 ?
H2B N2 H2B 141.1 . 2_556 ?
H2C N2 H2B 56.2 . 2_556 ?
H2D N2 H2B 56.3 . 2_556 ?
Cu1 N2 H2C 109.470(2) . 2_556 ?
H2B N2 H2C 56.3 . 2_556 ?
H2C N2 H2C 141.1 . 2_556 ?
H2D N2 H2C 56.3 . 2_556 ?
H2B N2 H2C 109.5 2_556 2_556 ?
Cu1 N2 H2D 109.471(2) . 2_556 ?
H2B N2 H2D 56.3 . 2_556 ?
H2C N2 H2D 56.3 . 2_556 ?
H2D N2 H2D 141.1 . 2_556 ?
H2B N2 H2D 109.5 2_556 2_556 ?
H2C N2 H2D 109.5 2_556 2_556 ?
C3 N1 C3 122.4(3) 2_556 . ?
C3 N1 Cu1 118.79(17) 2_556 . ?
C3 N1 Cu1 118.79(17) . . ?
C2 C1 C2 121.0(4) 2_556 . ?
C2 C1 H1 119.5 2_556 . ?
C2 C1 H1 119.5 . . ?
C3 C2 C1 117.9(3) . . ?
C3 C2 H2 121.1 . . ?
C1 C2 H2 121.1 . . ?
N1 C3 C2 120.4(3) . . ?
N1 C3 C4 111.1(3) . . ?
C2 C3 C4 128.5(3) . . ?
O1 C4 O2 125.9(3) . . ?
O1 C4 C3 120.0(3) . . ?
O2 C4 C3 114.1(2) . . ?

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
O2 Cu1 N1 C3 -5.19(14) 2_556 . . 2_556 ?
O2 Cu1 N1 C3 174.81(14) . . . 2_556 ?
O2 Cu1 N1 C3 174.81(14) 2_556 . . . ?
O2 Cu1 N1 C3 -5.19(14) . . . . ?
C2 C1 C2 C3 0.31(18) 2_556 . . . ?
C3 N1 C3 C2 0.33(19) 2_556 . . . ?
Cu1 N1 C3 C2 -179.67(19) . . . . ?
C3 N1 C3 C4 -179.0(2) 2_556 . . . ?
Cu1 N1 C3 C4 1.0(2) . . . . ?
C1 C2 C3 N1 -0.6(4) . . . . ?
C1 C2 C3 C4 178.5(2) . . . . ?
Cu1 O2 C4 O1 167.9(3) . . . . ?
Cu1 O2 C4 C3 -10.9(3) . . . . ?
N1 C3 C4 O1 -172.1(2) . . . . ?
C2 C3 C4 O1 8.7(5) . . . . ?
N1 C3 C4 O2 6.8(3) . . . . ?
C2 C3 C4 O2 -172.4(3) . . . . ?

_refine_diff_density_max         0.436
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.090

####################################################################### 
# 
# 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_compound-3
_database_code_depnum_ccdc_archive 'CCDC 1901747'
loop_
_audit_author_name
_audit_author_address
'Wei-Wei Xiong'
;Nanjing Tech University (NanjingTech)
China
;
_audit_update_record             
;
2019-04-28 deposited with the CCDC.	2019-06-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C9 H5 O6) 2(C3H6O) Co, C3H6O, 0.25(H2 O)'
_chemical_formula_sum            'C27 H27 Co N6 O15.25'
_chemical_formula_weight         738.47

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'
Co Co 0.3494 0.9721 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'I 2/m'
_space_group_name_Hall           '-I 2y'

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

_cell_length_a                   9.3019(17)
_cell_length_b                   28.739(5)
_cell_length_c                   11.788(2)
_cell_angle_alpha                90
_cell_angle_beta                 103.534(14)
_cell_angle_gamma                90
_cell_volume                     3063.7(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4576
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      26.44

_exptl_crystal_description       block-like
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_F_000             1520
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    0.646
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5673
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13182
_diffrn_reflns_av_unetI/netI     0.1180
_diffrn_reflns_av_R_equivalents  0.1178
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.361
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             3065
_reflns_number_gt                2167
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND. Version 3.0. Crystal Impact'
_computing_publication_material  'Windows Word 2010'
_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)+(0.0505P)²+46.3491P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_extinction_coef       0.0046(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3065
_refine_ls_number_parameters     245
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.1117
_refine_ls_R_factor_gt           0.0794
_refine_ls_wR_factor_ref         0.2125
_refine_ls_wR_factor_gt          0.1963
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_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
Co1 Co 1.000000 0.17635(4) 0.000000 0.0166(4) Uani 1 2 d S T P . .
C1 C 1.0764(8) 0.0266(2) 0.2074(6) 0.0378(17) Uani 1 1 d . . . . .
H1A H 1.082121 0.039065 0.286674 0.045 Uiso 1 1 calc R U . . .
H1B H 1.160115 0.039064 0.178030 0.045 Uiso 1 1 calc R U . . .
C2 C 0.7893(9) 0.0667(2) 0.4456(7) 0.0373(18) Uani 1 1 d . . . . .
C3 C 0.4894(8) 0.0926(2) -0.1762(7) 0.0409(18) Uani 1 1 d . . . . .
H3A H 0.402217 0.080402 -0.151034 0.049 Uiso 1 1 calc R U . . .
H3B H 0.494562 0.077725 -0.250984 0.049 Uiso 1 1 calc R U . . .
C4 C 0.8613(11) 0.000000 0.0815(9) 0.032(2) Uani 1 2 d S T P . .
C5 C 0.7139(7) 0.1218(2) -0.0796(6) 0.0273(14) Uani 1 1 d . . . . .
C6 C 0.4843(9) 0.1461(3) -0.1868(8) 0.054(2) Uani 1 1 d . . . . .
H6A H 0.448310 0.156279 -0.268784 0.065 Uiso 1 1 calc R U . . .
H6B H 0.422178 0.160136 -0.138222 0.065 Uiso 1 1 calc R U . . .
C7 C 0.6703(6) 0.23006(18) 0.5469(5) 0.0182(12) Uani 1 1 d . . . . .
C8 C 0.7995(7) 0.11740(18) 0.4343(5) 0.0229(13) Uani 1 1 d . . . . .
C9 C 0.8239(6) 0.21318(18) 0.4037(5) 0.0173(11) Uani 1 1 d . . . . .
H9A H 0.831616 0.245763 0.392837 0.021 Uiso 1 1 calc R U . . .
C10 C 0.9704(6) 0.20001(19) 0.2524(5) 0.0175(12) Uani 1 1 d . . . . .
C11 C 0.8903(6) 0.18241(19) 0.3401(5) 0.0171(11) Uani 1 1 d . . . . .
C12 C 0.7456(6) 0.19634(18) 0.4837(5) 0.0163(11) Uani 1 1 d . . . . .
C13 C 0.8758(6) 0.13498(19) 0.3541(5) 0.0201(12) Uani 1 1 d . . . . .
H13A H 0.918223 0.114023 0.308778 0.024 Uiso 1 1 calc R U . . .
C14 C 0.7344(6) 0.14869(18) 0.4998(5) 0.0188(12) Uani 1 1 d . . . . .
H14A H 0.683091 0.137209 0.554765 0.023 Uiso 1 1 calc R U . . .
N1 N 0.9361(7) 0.0380(2) 0.1292(6) 0.0474(17) Uani 1 1 d . . . . .
H1C H 0.903378 0.066644 0.114444 0.057 Uiso 1 1 calc R U . . .
N3 N 0.6410(7) 0.1568(2) -0.1419(7) 0.060(2) Uani 1 1 d . . . . .
H3C H 0.682303 0.183305 -0.154440 0.072 Uiso 1 1 calc R U . . .
N4 N 0.6228(6) 0.08523(18) -0.0886(5) 0.0355(14) Uani 1 1 d . . . . .
H4A H 0.642483 0.059868 -0.045957 0.043 Uiso 1 1 calc R U . . .
O3 O 1.0006(5) 0.24409(13) 0.2599(4) 0.0249(10) Uani 1 1 d . . . . .
O4 O 0.7415(8) 0.000000 0.0085(7) 0.0401(18) Uani 1 2 d S T P . .
O5 O 0.6163(5) 0.21309(13) 0.6272(4) 0.0240(10) Uani 1 1 d . . . . .
O6 O 1.0032(4) 0.17296(13) 0.1802(3) 0.0221(9) Uani 1 1 d . . . . .
O7 O 0.8440(4) 0.12319(13) -0.0197(4) 0.0238(9) Uani 1 1 d . . . . .
O8 O 0.6635(4) 0.27214(12) 0.5162(3) 0.0184(9) Uani 1 1 d . . . . .
H3 H 1.062(10) 0.257(3) 0.193(8) 0.07(3) Uiso 1 1 d . . . . .
O1 O 0.7119(6) 0.04856(15) 0.5081(5) 0.0356(12) Uani 1 1 d D . . . .
O2A O 0.835(6) 0.0424(4) 0.369(4) 0.072(12) Uani 0.65(8) 1 d . . P A 1
O2B O 0.902(3) 0.0425(7) 0.426(5) 0.028(9) Uani 0.35(8) 1 d . U P A 2
O9 O 0.500000 0.000000 0.500000 0.081(8) Uiso 0.5 4 d S . P . .
H1D H 0.623(14) 0.050(7) 0.449(15) 0.32(13) Uiso 1 1 d 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
Co1 O7 2.082(4) . ?
Co1 O7 2.082(4) 2_755 ?
Co1 O8 2.099(4) 8_554 ?
Co1 O8 2.099(4) 7_655 ?
Co1 O6 2.120(4) 2_755 ?
Co1 O6 2.120(4) . ?
C1 N1 1.448(9) . ?
C1 C1 1.531(13) 6 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 O1 1.258(8) . ?
C2 O2A 1.291(16) . ?
C2 O2B 1.322(19) . ?
C2 C8 1.469(8) . ?
C3 N4 1.433(9) . ?
C3 C6 1.543(10) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 O4 1.238(12) . ?
C4 N1 1.346(9) 6 ?
C4 N1 1.346(9) . ?
C5 O7 1.252(8) . ?
C5 N3 1.335(8) . ?
C5 N4 1.338(8) . ?
C6 N3 1.463(10) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 O8 1.260(6) . ?
C7 O5 1.268(6) . ?
C7 C12 1.493(7) . ?
C8 C13 1.403(8) . ?
C8 C14 1.410(7) . ?
C9 C11 1.393(7) . ?
C9 C12 1.406(7) . ?
C9 H9A 0.9500 . ?
C10 O6 1.242(6) . ?
C10 O3 1.296(7) . ?
C10 C11 1.497(7) . ?
C11 C13 1.383(7) . ?
C12 C14 1.390(7) . ?
C13 H13A 0.9500 . ?
C14 H14A 0.9500 . ?
N1 H1C 0.8800 . ?
N3 H3C 0.8800 . ?
N4 H4A 0.8800 . ?
O3 H3 1.13(9) . ?
O1 H1D 0.950(10) . ?

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
O7 Co1 O7 85.6(2) . 2_755 ?
O7 Co1 O8 177.28(15) . 8_554 ?
O7 Co1 O8 92.09(15) 2_755 8_554 ?
O7 Co1 O8 92.09(15) . 7_655 ?
O7 Co1 O8 177.28(15) 2_755 7_655 ?
O8 Co1 O8 90.3(2) 8_554 7_655 ?
O7 Co1 O6 90.51(16) . 2_755 ?
O7 Co1 O6 85.63(16) 2_755 2_755 ?
O8 Co1 O6 87.89(15) 8_554 2_755 ?
O8 Co1 O6 95.82(15) 7_655 2_755 ?
O7 Co1 O6 85.63(16) . . ?
O7 Co1 O6 90.51(16) 2_755 . ?
O8 Co1 O6 95.82(15) 8_554 . ?
O8 Co1 O6 87.89(15) 7_655 . ?
O6 Co1 O6 174.7(2) 2_755 . ?
N1 C1 C1 103.1(4) . 6 ?
N1 C1 H1A 111.2 . . ?
C1 C1 H1A 111.2 6 . ?
N1 C1 H1B 111.2 . . ?
C1 C1 H1B 111.2 6 . ?
H1A C1 H1B 109.1 . . ?
O1 C2 O2A 121.0(11) . . ?
O1 C2 O2B 118.1(16) . . ?
O1 C2 C8 121.4(6) . . ?
O2A C2 C8 115.7(7) . . ?
O2B C2 C8 115.8(10) . . ?
N4 C3 C6 102.1(6) . . ?
N4 C3 H3A 111.3 . . ?
C6 C3 H3A 111.3 . . ?
N4 C3 H3B 111.3 . . ?
C6 C3 H3B 111.3 . . ?
H3A C3 H3B 109.2 . . ?
O4 C4 N1 125.7(5) . 6 ?
O4 C4 N1 125.7(5) . . ?
N1 C4 N1 108.6(9) 6 . ?
O7 C5 N3 125.9(6) . . ?
O7 C5 N4 125.5(5) . . ?
N3 C5 N4 108.6(6) . . ?
N3 C6 C3 99.9(6) . . ?
N3 C6 H6A 111.8 . . ?
C3 C6 H6A 111.8 . . ?
N3 C6 H6B 111.8 . . ?
C3 C6 H6B 111.8 . . ?
H6A C6 H6B 109.5 . . ?
O8 C7 O5 125.6(5) . . ?
O8 C7 C12 118.5(5) . . ?
O5 C7 C12 115.9(5) . . ?
C13 C8 C14 119.3(5) . . ?
C13 C8 C2 118.2(5) . . ?
C14 C8 C2 122.6(5) . . ?
C11 C9 C12 120.5(5) . . ?
C11 C9 H9A 119.8 . . ?
C12 C9 H9A 119.8 . . ?
O6 C10 O3 125.1(5) . . ?
O6 C10 C11 120.2(5) . . ?
O3 C10 C11 114.7(5) . . ?
C13 C11 C9 119.6(5) . . ?
C13 C11 C10 119.6(5) . . ?
C9 C11 C10 120.8(5) . . ?
C14 C12 C9 119.8(5) . . ?
C14 C12 C7 120.9(5) . . ?
C9 C12 C7 119.3(5) . . ?
C11 C13 C8 120.9(5) . . ?
C11 C13 H13A 119.5 . . ?
C8 C13 H13A 119.5 . . ?
C12 C14 C8 119.9(5) . . ?
C12 C14 H14A 120.0 . . ?
C8 C14 H14A 120.0 . . ?
C4 N1 C1 112.5(6) . . ?
C4 N1 H1C 123.7 . . ?
C1 N1 H1C 123.7 . . ?
C5 N3 C6 112.0(6) . . ?
C5 N3 H3C 124.0 . . ?
C6 N3 H3C 124.0 . . ?
C5 N4 C3 111.6(5) . . ?
C5 N4 H4A 124.2 . . ?
C3 N4 H4A 124.2 . . ?
C10 O3 H3 114(4) . . ?
C10 O6 Co1 135.2(4) . . ?
C5 O7 Co1 130.0(4) . . ?
C7 O8 Co1 133.6(3) . 7_655 ?
C2 O1 H1D 94(10) . . ?

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
N4 C3 C6 N3 22.8(8) . . . . ?
O1 C2 C8 C13 -173.7(7) . . . . ?
O2A C2 C8 C13 -9(3) . . . . ?
O2B C2 C8 C13 31(3) . . . . ?
O1 C2 C8 C14 5.6(12) . . . . ?
O2A C2 C8 C14 170(3) . . . . ?
O2B C2 C8 C14 -150(3) . . . . ?
C12 C9 C11 C13 1.5(9) . . . . ?
C12 C9 C11 C10 178.3(5) . . . . ?
O6 C10 C11 C13 11.3(9) . . . . ?
O3 C10 C11 C13 -168.4(5) . . . . ?
O6 C10 C11 C9 -165.6(5) . . . . ?
O3 C10 C11 C9 14.7(8) . . . . ?
C11 C9 C12 C14 0.1(9) . . . . ?
C11 C9 C12 C7 -177.4(5) . . . . ?
O8 C7 C12 C14 -168.8(6) . . . . ?
O5 C7 C12 C14 10.3(8) . . . . ?
O8 C7 C12 C9 8.7(8) . . . . ?
O5 C7 C12 C9 -172.2(5) . . . . ?
C9 C11 C13 C8 -2.1(9) . . . . ?
C10 C11 C13 C8 -179.0(6) . . . . ?
C14 C8 C13 C11 1.2(10) . . . . ?
C2 C8 C13 C11 -179.5(6) . . . . ?
C9 C12 C14 C8 -1.1(9) . . . . ?
C7 C12 C14 C8 176.4(5) . . . . ?
C13 C8 C14 C12 0.5(9) . . . . ?
C2 C8 C14 C12 -178.8(7) . . . . ?
O4 C4 N1 C1 -177.1(9) . . . . ?
N1 C4 N1 C1 4.9(12) 6 . . . ?
C1 C1 N1 C4 -2.9(7) 6 . . . ?
O7 C5 N3 C6 -171.0(7) . . . . ?
N4 C5 N3 C6 6.8(10) . . . . ?
C3 C6 N3 C5 -19.0(10) . . . . ?
O7 C5 N4 C3 -171.9(7) . . . . ?
N3 C5 N4 C3 10.3(9) . . . . ?
C6 C3 N4 C5 -21.5(8) . . . . ?
O3 C10 O6 Co1 -41.5(9) . . . . ?
C11 C10 O6 Co1 138.8(4) . . . . ?
N3 C5 O7 Co1 -4.2(10) . . . . ?
N4 C5 O7 Co1 178.3(5) . . . . ?
O5 C7 O8 Co1 -37.5(9) . . . 7_655 ?
C12 C7 O8 Co1 141.5(4) . . . 7_655 ?

_refine_diff_density_max         0.730
_refine_diff_density_min         -0.964
_refine_diff_density_rms         0.129

####################################################################### 
# 
# 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_compound-4
_database_code_depnum_ccdc_archive 'CCDC 1901748'
loop_
_audit_author_name
_audit_author_address
'Wei-Wei Xiong'
;Nanjing Tech University
China
;
_audit_update_record             
;
2019-05-22 deposited with the CCDC.	2019-06-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C5 H N2 O4 Mn), K0.63, N0.37 H1.48'
_chemical_formula_sum            'C5 H K0.63 Mn N2.37 O4'
_chemical_formula_weight         237.91

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'
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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           135
_space_group_name_H-M_alt        'P 42/m b c'
_space_group_name_Hall           '-P 4c 2ab'

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

_cell_length_a                   8.2634(2)
_cell_length_b                   8.2634(2)
_cell_length_c                   20.2666(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1383.88(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1203
_cell_measurement_theta_min      4.0070
_cell_measurement_theta_max      28.6520

_exptl_crystal_description       flake
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.283
_exptl_crystal_F_000             933
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    2.265
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.76995
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4777
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.487
_diffrn_reflns_theta_max         29.231
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             906
_reflns_number_gt                682
_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       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND. Version 3.0. Crystal Impact'
_computing_publication_material  'Windows Word 2010'
_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)+(0.0286P)²+1.5361P] 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         906
_refine_ls_number_parameters     66
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0372
_refine_ls_wR_factor_ref         0.0829
_refine_ls_wR_factor_gt          0.0734
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_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
Mn1 Mn 0.000000 0.000000 0.11033(3) 0.01548(19) Uani 1 2 d S T P A .
O1 O 0.2457(2) 0.0630(2) 0.14629(10) 0.0220(5) Uani 1 1 d . . . . .
O2 O 0.0772(2) -0.2373(2) 0.16336(9) 0.0195(4) Uani 1 1 d . . . . .
N1 N 0.0457(2) -0.1814(2) 0.03314(10) 0.0149(5) Uani 1 1 d . . . . .
C1 C 0.3742(3) 0.1850(3) 0.05382(14) 0.0143(6) Uani 1 1 d . . . . .
C2 C 0.3235(5) 0.0950(5) 0.000000 0.0167(8) Uani 1 2 d S T P . .
C3 C 0.3457(3) 0.1668(3) 0.12541(13) 0.0156(6) Uani 1 1 d . . . . .
K1 K 0.33078(11) -0.16922(11) 0.250000 0.0240(5) Uani 0.633(6) 2 d S T P A 1
N2 N 0.33078(11) -0.16922(11) 0.250000 0.0240(5) Uani 0.367(6) 2 d S T P A 2
H2 H 0.261(5) -0.001(5) 0.000000 0.016(10) Uiso 1 2 d S . P . .


_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
Mn1 N1 2.199(2) . ?
Mn1 N1 2.199(2) 2 ?
Mn1 O1 2.219(2) . ?
Mn1 O1 2.219(2) 2 ?
Mn1 O2 2.3251(19) 2 ?
Mn1 O2 2.3251(19) . ?
O1 C3 1.264(3) . ?
O1 K1 2.9314(19) . ?
O1 K1 3.117(2) 12_556 ?
O2 C3 1.275(3) 14_655 ?
O2 K1 2.791(2) . ?
O2 K1 2.7974(19) 11_556 ?
N1 N1 1.343(4) 10 ?
N1 C1 1.354(3) 14_655 ?
C1 C2 1.385(4) . ?
C1 C3 1.477(4) . ?
C3 K1 3.216(3) 12_556 ?
K1 K1 3.955(3) 2_655 ?
K1 K1 4.3420(6) 12_546 ?

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 Mn1 N1 89.30(11) . 2 ?
N1 Mn1 O1 103.66(8) . . ?
N1 Mn1 O1 103.36(7) 2 . ?
N1 Mn1 O1 103.36(7) . 2 ?
N1 Mn1 O1 103.66(8) 2 2 ?
O1 Mn1 O1 141.66(10) . 2 ?
N1 Mn1 O2 161.92(7) . 2 ?
N1 Mn1 O2 72.96(7) 2 2 ?
O1 Mn1 O2 84.34(7) . 2 ?
O1 Mn1 O2 78.17(7) 2 2 ?
N1 Mn1 O2 72.96(7) . . ?
N1 Mn1 O2 161.92(7) 2 . ?
O1 Mn1 O2 78.17(7) . . ?
O1 Mn1 O2 84.34(7) 2 . ?
O2 Mn1 O2 124.94(10) 2 . ?
C3 O1 Mn1 130.35(17) . . ?
C3 O1 K1 121.83(16) . . ?
Mn1 O1 K1 107.54(7) . . ?
C3 O1 K1 82.91(15) . 12_556 ?
Mn1 O1 K1 101.68(7) . 12_556 ?
K1 O1 K1 91.71(5) . 12_556 ?
C3 O2 Mn1 112.50(16) 14_655 . ?
C3 O2 K1 97.44(15) 14_655 . ?
Mn1 O2 K1 109.07(7) . . ?
C3 O2 K1 124.78(16) 14_655 11_556 ?
Mn1 O2 K1 108.87(7) . 11_556 ?
K1 O2 K1 101.96(6) . 11_556 ?
N1 N1 C1 108.03(15) 10 14_655 ?
N1 N1 Mn1 135.35(6) 10 . ?
C1 N1 Mn1 114.81(17) 14_655 . ?
N1 C1 C2 110.0(2) 14_665 . ?
N1 C1 C3 117.7(2) 14_665 . ?
C2 C1 C3 132.1(2) . . ?
C1 C2 C1 103.9(3) 10 . ?
O1 C3 O2 123.1(2) . 14_665 ?
O1 C3 C1 120.1(2) . . ?
O2 C3 C1 116.7(2) 14_665 . ?
O1 C3 K1 74.13(15) . 12_556 ?
O2 C3 K1 59.40(13) 14_665 12_556 ?
C1 C3 K1 143.16(17) . 12_556 ?
O2 K1 O2 95.35(9) . 7_545 ?
O2 K1 O2 109.52(7) . 12_556 ?
O2 K1 O2 95.51(6) 7_545 12_556 ?
O2 K1 O2 95.51(6) . 13_655 ?
O2 K1 O2 109.52(7) 7_545 13_655 ?
O2 K1 O2 142.76(9) 12_556 13_655 ?
O2 K1 O1 60.05(6) . . ?
O2 K1 O1 153.40(7) 7_545 . ?
O2 K1 O1 84.69(6) 12_556 . ?
O2 K1 O1 84.56(6) 13_655 . ?
O2 K1 O1 153.40(7) . 7_545 ?
O2 K1 O1 60.05(6) 7_545 7_545 ?
O2 K1 O1 84.56(6) 12_556 7_545 ?
O2 K1 O1 84.69(6) 13_655 7_545 ?
O1 K1 O1 145.90(9) . 7_545 ?
O2 K1 O1 43.99(5) . 14_655 ?
O2 K1 O1 81.39(6) 7_545 14_655 ?
O2 K1 O1 152.13(6) 12_556 14_655 ?
O2 K1 O1 61.85(5) 13_655 14_655 ?
O1 K1 O1 86.13(5) . 14_655 ?
O1 K1 O1 116.49(7) 7_545 14_655 ?
O2 K1 O1 81.39(6) . 11_556 ?
O2 K1 O1 43.99(5) 7_545 11_556 ?
O2 K1 O1 61.85(5) 12_556 11_556 ?
O2 K1 O1 152.13(6) 13_655 11_556 ?
O1 K1 O1 116.49(7) . 11_556 ?
O1 K1 O1 86.13(5) 7_545 11_556 ?
O1 K1 O1 99.60(8) 14_655 11_556 ?
O2 K1 C3 23.16(6) . 14_655 ?
O2 K1 C3 94.94(7) 7_545 14_655 ?
O2 K1 C3 132.40(7) 12_556 14_655 ?
O2 K1 C3 73.79(6) 13_655 14_655 ?
O1 K1 C3 66.68(6) . 14_655 ?
O1 K1 C3 139.36(7) 7_545 14_655 ?
O1 K1 C3 22.96(6) 14_655 14_655 ?
O1 K1 C3 97.01(7) 11_556 14_655 ?
O2 K1 C3 94.94(7) . 11_556 ?
O2 K1 C3 23.16(6) 7_545 11_556 ?
O2 K1 C3 73.79(6) 12_556 11_556 ?
O2 K1 C3 132.40(7) 13_655 11_556 ?
O1 K1 C3 139.36(7) . 11_556 ?
O1 K1 C3 66.68(6) 7_545 11_556 ?
O1 K1 C3 97.01(7) 14_655 11_556 ?
O1 K1 C3 22.96(6) 11_556 11_556 ?
C3 K1 C3 103.55(10) 14_655 11_556 ?
O2 K1 K1 132.33(4) . 2_655 ?
O2 K1 K1 132.33(4) 7_545 2_655 ?
O2 K1 K1 71.38(5) 12_556 2_655 ?
O2 K1 K1 71.38(5) 13_655 2_655 ?
O1 K1 K1 72.95(4) . 2_655 ?
O1 K1 K1 72.95(4) 7_545 2_655 ?
O1 K1 K1 130.20(4) 14_655 2_655 ?
O1 K1 K1 130.20(4) 11_556 2_655 ?
C3 K1 K1 128.23(5) 14_655 2_655 ?
C3 K1 K1 128.23(5) 11_556 2_655 ?
O2 K1 K1 65.00(5) . 12_546 ?
O2 K1 K1 39.07(4) 7_545 12_546 ?
O2 K1 K1 127.42(5) 12_556 12_546 ?
O2 K1 K1 87.76(4) 13_655 12_546 ?
O1 K1 K1 123.30(5) . 12_546 ?
O1 K1 K1 88.46(4) 7_545 12_546 ?
O1 K1 K1 42.44(4) 14_655 12_546 ?
O1 K1 K1 65.72(5) 11_556 12_546 ?
C3 K1 K1 57.28(5) 14_655 12_546 ?
C3 K1 K1 55.86(5) 11_556 12_546 ?
K1 K1 K1 152.91(2) 2_655 12_546 ?

_refine_diff_density_max         0.377
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.084

