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

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

data_ch1ppx451v_0m
_database_code_depnum_ccdc_archive 'CCDC 1968822'
loop_
_audit_author_name
_audit_author_address
'Craig Robertson'
;University of Sheffield
United Kingdom
;
_audit_update_record             
;
2019-11-28 deposited with the CCDC.	2020-10-14 downloaded from the CCDC.
;
_audit_creation_date             2019-11-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        'Sodium nitrotetrazolate tetrahydrate'
_chemical_formula_moiety         '0.5(C2 H8 N10 Na2 O8), 2(H2 O)'
_chemical_formula_sum            'C H8 N5 Na O6'
_chemical_formula_weight         209.11
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   17.7189(10)
_cell_length_b                   3.5053(2)
_cell_length_c                   13.3457(8)
_cell_angle_alpha                90
_cell_angle_beta                 100.282(2)
_cell_angle_gamma                90
_cell_volume                     815.59(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6147
_cell_measurement_temperature    100
_cell_measurement_theta_max      66.75
_cell_measurement_theta_min      3.37
_shelx_estimated_absorpt_T_max   0.761
_shelx_estimated_absorpt_T_min   0.556
_exptl_absorpt_coefficient_mu    1.925
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5275
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1391 before and 0.0946 after correction. The Ratio of minimum to maximum transmission is 0.7007. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.345
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9009
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        66.741
_diffrn_reflns_theta_max         66.741
_diffrn_reflns_theta_min         5.073
_diffrn_ambient_temperature      99.97
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                673
_reflns_number_total             710
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2017)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         710
_refine_ls_number_restraints     73
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0390
_refine_ls_restrained_S_all      1.125
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0517P)²+1.1521P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1004
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O3-H3B = O3-H3A
 0.87 with sigma of 0.02
 O4-H4B = O4-H4A
 0.87 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: O1(0.5) O2(0.5) N1(0.5) N2(0.5) N3(0.5) N4(0.5) N5(0.5)
5.a Free rotating group:
 O4(H4A)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Na1 Na 0.7500 0.2500 0.5000 0.0116(3) Uani 1 2 d S TU P . .
O1 O 0.8852(5) 0.232(3) 0.5126(7) 0.0168(18) Uani 0.5 1 d . U . A -1
O2 O 0.4564(4) -0.050(2) 0.6510(4) 0.0192(14) Uani 0.5 1 d . U . B -1
O3 O 0.74998(7) 0.7476(3) 0.62075(10) 0.0128(4) Uani 1 1 d D U . . .
H3A H 0.7859(12) 0.800(7) 0.6687(16) 0.024(6) Uiso 1 1 d D . . . .
H3B H 0.7124(16) 0.709(11) 0.652(3) 0.066(11) Uiso 1 1 d D . . . .
N1 N 0.6025(7) 0.217(4) 0.4648(8) 0.0101(15) Uani 0.5 1 d . U . A -1
N2 N 0.56574(16) 0.1652(9) 0.5438(2) 0.0098(6) Uani 0.5 1 d . U . A -1
N3 N 0.49383(16) -0.0633(9) 0.4012(2) 0.0101(6) Uani 0.5 1 d . U . A -1
N4 N 0.5593(4) 0.079(3) 0.3793(7) 0.0123(13) Uani 0.5 1 d . U . A -1
N5 N 0.4426(3) -0.1139(10) 0.5588(4) 0.0106(7) Uani 0.5 1 d . U . B -1
C1 C 0.5000 0.0000 0.5000 0.0085(5) Uani 1 2 d S TU P . .
O4 O 0.63351(7) 0.5186(4) 0.72616(9) 0.0143(4) Uani 1 1 d D U . . .
H4A H 0.6009 0.3750 0.6866 0.021 Uiso 1 1 d DG . . . .
H4B H 0.6055(14) 0.677(7) 0.749(2) 0.034(7) 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
Na1 Na1 3.50530(19) 1_565 ?
Na1 Na1 3.5053(2) 1_545 ?
Na1 O1 2.372(10) . ?
Na1 O3 2.3747(13) . ?
Na1 O3 2.3872(13) 1_545 ?
Na1 O3 2.3747(13) 7_656 ?
Na1 O3 2.3872(13) 7_666 ?
Na1 N1 2.573(12) . ?
O2 N5 1.231(7) . ?
O3 Na1 2.3872(12) 1_565 ?
N1 N2 1.347(13) . ?
N1 N4 1.346(11) . ?
N2 C1 1.338(3) . ?
N3 N4 1.342(9) . ?
N3 C1 1.322(3) . ?
N5 C1 1.447(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
Na1 Na1 Na1 180.0 1_545 1_565 ?
O1 Na1 Na1 88.5(3) . 1_545 ?
O1 Na1 Na1 91.5(3) . 1_565 ?
O1 Na1 O3 93.1(3) . 1_545 ?
O1 Na1 O3 86.9(3) . 7_666 ?
O1 Na1 O3 95.4(2) . . ?
O1 Na1 O3 84.6(2) . 7_656 ?
O1 Na1 N1 172.4(4) . . ?
O3 Na1 Na1 42.74(3) . 1_565 ?
O3 Na1 Na1 137.26(3) . 1_545 ?
O3 Na1 Na1 137.26(3) 7_656 1_565 ?
O3 Na1 Na1 137.54(3) 7_666 1_545 ?
O3 Na1 Na1 137.54(3) 1_545 1_565 ?
O3 Na1 Na1 42.46(3) 7_666 1_565 ?
O3 Na1 Na1 42.74(3) 7_656 1_545 ?
O3 Na1 Na1 42.46(3) 1_545 1_545 ?
O3 Na1 O3 180.0 . 7_656 ?
O3 Na1 O3 94.80(5) . 1_545 ?
O3 Na1 O3 180.0 7_666 1_545 ?
O3 Na1 O3 85.20(5) . 7_666 ?
O3 Na1 O3 85.20(5) 7_656 1_545 ?
O3 Na1 O3 94.80(5) 7_656 7_666 ?
O3 Na1 N1 88.1(3) 7_656 . ?
O3 Na1 N1 91.9(2) . . ?
O3 Na1 N1 91.9(3) 7_666 . ?
O3 Na1 N1 88.1(3) 1_545 . ?
N1 Na1 Na1 92.6(3) . 1_565 ?
N1 Na1 Na1 87.4(3) . 1_545 ?
Na1 O3 Na1 94.80(5) . 1_565 ?
N2 N1 Na1 118.8(6) . . ?
N4 N1 Na1 125.2(9) . . ?
N4 N1 N2 109.4(10) . . ?
C1 N2 N1 102.9(5) . . ?
C1 N3 N4 103.5(4) . . ?
N3 N4 N1 109.4(9) . . ?
O2 N5 C1 117.3(5) . . ?
N2 C1 N5 121.6(3) . . ?
N3 C1 N2 114.73(18) . . ?
N3 C1 N5 123.6(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
O3 H3A O4 0.839(18) 1.969(18) 2.7988(18) 170(3) 4_656
O3 H3B O4 0.858(19) 1.97(2) 2.8139(18) 169(4) .
O4 H4A N2 0.87 2.03 2.803(3) 146.8 .

_olex2_exptl_crystal_mounting_method 'Mitigen microloop in fombin oil'
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: H2O'
####################################################################### 
# 
# 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_dbxx_2
_database_code_depnum_ccdc_archive 'CCDC 1983373'
loop_
_audit_author_name
_audit_author_address
'Peter Peter Portius'
;The University of Sheffield
United Kingdom
;
_audit_update_record             
;
2020-02-11 deposited with the CCDC.	2020-10-14 downloaded from the CCDC.
;
_audit_creation_date             2019-04-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C2 Cl Cu3 N10 O4'
_chemical_formula_sum            'C2 Cl Cu3 N10 O4'
_chemical_formula_weight         454.19
_chemical_melting_point          ?
_chemical_oxdiff_formula         CuClNOC
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.8980(10)
_cell_length_b                   9.2377(9)
_cell_length_c                   10.3680(10)
_cell_angle_alpha                90
_cell_angle_beta                 100.493(10)
_cell_angle_gamma                90
_cell_volume                     1026.32(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    618
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      71.4880
_cell_measurement_theta_min      4.0900
_shelx_estimated_absorpt_T_max   0.906
_shelx_estimated_absorpt_T_min   0.906
_exptl_absorpt_coefficient_mu    10.046
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86129
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.42a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.939
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0827
_diffrn_reflns_av_unetI/netI     0.1114
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4254
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.144
_diffrn_reflns_theta_min         4.126
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -44.00 134.00   1.00    5.00    --   44.80  20.00  30.00  178
  2  ω     19.00  90.00   1.00   15.00    --  108.20  40.00 120.00   71
  3  ω     93.00 157.00   1.00   15.00    --  108.20  40.00 120.00   64
  4  ω    132.00 198.00   1.00   15.00    --  108.20  40.00-150.00   66
  5  ω     48.00  74.00   1.00   15.00    --  108.20  30.00 150.00   26
  6  ω     77.00 182.00   1.00   15.00    --  108.20  30.00 150.00  105
  7  ω     57.00 147.00   1.00   15.00    --  108.20  40.00  90.00   90
  8  ω     19.00  68.00   1.00   15.00    --  108.20  40.00-150.00   49
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0891865000
_diffrn_orient_matrix_UB_12      -0.1307947000
_diffrn_orient_matrix_UB_13      0.0165457000
_diffrn_orient_matrix_UB_21      0.0200321000
_diffrn_orient_matrix_UB_22      0.0191627000
_diffrn_orient_matrix_UB_23      -0.1423291000
_diffrn_orient_matrix_UB_31      0.1109370000
_diffrn_orient_matrix_UB_32      0.1016278000
_diffrn_orient_matrix_UB_33      0.0482226000
_diffrn_oxdiff_digest_frames     
;
019433775da7a37f881268d92bdf33a75b00026926c
;
_diffrn_oxdiff_digest_hkl        
;
0158a90190ab289e24496d010b54773d750926
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1314
_reflns_number_total             2060
_reflns_odcompleteness_completeness 98.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.012
_refine_diff_density_min         -0.927
_refine_diff_density_rms         0.215
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2060
_refine_ls_number_restraints     84
_refine_ls_R_factor_all          0.1046
_refine_ls_R_factor_gt           0.0569
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0169P)²+8.5252P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1200
_refine_ls_wR_factor_ref         0.1429
_refine_special_details          ?
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
O4 \\sim N10 \\sim O3: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004
2. Rigid body (RIGU) restrains
 O2, O1, N8, N7, N6, N5
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O3, O4, N10, N4, N3, N2, N1, C2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Cu3 Cu 0.62154(12) 1.07839(15) 0.41458(12) 0.0154(3) Uani 1 1 d . . . . .
Cu2 Cu 0.16417(12) 0.73847(15) 0.33569(14) 0.0178(3) Uani 1 1 d . . . . .
Cu1 Cu 0.06699(14) 0.10137(15) 0.41557(14) 0.0221(4) Uani 1 1 d . . . . .
Cl1 Cl 0.15790(18) -0.0897(2) 0.5283(2) 0.0160(4) Uani 1 1 d . . . . .
O3 O 0.2800(7) 0.5311(7) 0.5723(7) 0.0267(14) Uani 1 1 d . U . . .
O4 O 0.2298(7) 0.3114(7) 0.6104(7) 0.0220(13) Uani 1 1 d . U . . .
O2 O 0.6112(7) 0.7225(9) 0.1006(8) 0.0341(18) Uani 1 1 d . U . . .
O1 O 0.6792(7) 0.9223(9) 0.1977(7) 0.0320(17) Uani 1 1 d . U . . .
N10 N 0.2173(7) 0.4239(8) 0.5468(8) 0.0198(12) Uani 1 1 d . U . . .
N4 N 0.0847(7) 0.5448(8) 0.3621(7) 0.0151(14) Uani 1 1 d . U . . .
N3 N -0.0088(7) 0.5004(8) 0.2668(7) 0.0144(14) Uani 1 1 d . U . . .
N2 N -0.0277(7) 0.3582(8) 0.2824(7) 0.0159(14) Uani 1 1 d . U . . .
N1 N 0.0537(7) 0.3120(8) 0.3879(7) 0.0129(13) Uani 1 1 d . U . . .
N7 N 0.5097(6) 0.9065(9) 0.3556(6) 0.0139(14) Uani 1 1 d . U . . .
N6 N 0.4041(7) 0.8740(9) 0.3976(7) 0.0153(14) Uani 1 1 d . U . . .
N5 N 0.3420(7) 0.7717(8) 0.3206(7) 0.0132(14) Uani 1 1 d . U . . .
N9 N 0.4089(7) 0.7337(8) 0.2274(7) 0.0148(15) Uani 1 1 d . . . . .
N8 N 0.6060(8) 0.8218(9) 0.1776(8) 0.0175(15) Uani 1 1 d . U . . .
C2 C 0.1182(8) 0.4243(10) 0.4316(8) 0.0135(14) Uani 1 1 d . U . . .
C1 C 0.5081(9) 0.8199(10) 0.2532(9) 0.0148(18) 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
Cu3 Cl1 2.371(2) 3_666 ?
Cu3 N7 2.027(8) . ?
Cu3 N6 2.065(7) 3_676 ?
Cu3 N9 2.039(7) 2_655 ?
Cu2 Cl1 2.561(3) 1_565 ?
Cu2 N4 2.028(7) . ?
Cu2 N2 2.067(7) 2 ?
Cu2 N5 1.996(7) . ?
Cu1 Cl1 2.245(2) . ?
Cu1 Cl1 2.622(3) 3_556 ?
Cu1 N3 2.100(7) 2_545 ?
Cu1 N1 1.968(7) . ?
Cl1 Cu3 2.371(2) 3_666 ?
Cl1 Cu2 2.561(3) 1_545 ?
Cl1 Cu1 2.622(3) 3_556 ?
O3 N10 1.205(10) . ?
O4 N10 1.225(10) . ?
O2 N8 1.224(10) . ?
O1 N8 1.217(11) . ?
N10 C2 1.457(11) . ?
N4 N3 1.347(10) . ?
N4 C2 1.340(12) . ?
N3 Cu1 2.101(7) 2 ?
N3 N2 1.344(10) . ?
N2 Cu2 2.067(7) 2_545 ?
N2 N1 1.346(11) . ?
N1 C2 1.289(11) . ?
N7 N6 1.337(10) . ?
N7 C1 1.327(12) . ?
N6 Cu3 2.065(7) 3_676 ?
N6 N5 1.339(10) . ?
N5 N9 1.358(10) . ?
N9 Cu3 2.039(7) 2_645 ?
N9 C1 1.330(12) . ?
N8 C1 1.434(12) . ?

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
N7 Cu3 Cl1 129.5(2) . 3_666 ?
N7 Cu3 N6 105.9(3) . 3_676 ?
N7 Cu3 N9 108.9(3) . 2_655 ?
N6 Cu3 Cl1 93.4(2) 3_676 3_666 ?
N9 Cu3 Cl1 100.0(2) 2_655 3_666 ?
N9 Cu3 N6 119.9(3) 2_655 3_676 ?
N4 Cu2 Cl1 111.6(2) . 1_565 ?
N4 Cu2 N2 105.9(3) . 2 ?
N2 Cu2 Cl1 90.7(2) 2 1_565 ?
N5 Cu2 Cl1 97.5(2) . 1_565 ?
N5 Cu2 N4 126.2(3) . . ?
N5 Cu2 N2 118.4(3) . 2 ?
Cl1 Cu1 Cl1 101.18(8) . 3_556 ?
N3 Cu1 Cl1 92.3(2) 2_545 3_556 ?
N3 Cu1 Cl1 98.7(2) 2_545 . ?
N1 Cu1 Cl1 91.5(2) . 3_556 ?
N1 Cu1 Cl1 150.1(2) . . ?
N1 Cu1 N3 107.8(3) . 2_545 ?
Cu3 Cl1 Cu2 93.00(8) 3_666 1_545 ?
Cu3 Cl1 Cu1 153.17(10) 3_666 3_556 ?
Cu2 Cl1 Cu1 107.83(8) 1_545 3_556 ?
Cu1 Cl1 Cu3 115.26(10) . 3_666 ?
Cu1 Cl1 Cu2 98.82(9) . 1_545 ?
Cu1 Cl1 Cu1 78.82(8) . 3_556 ?
O3 N10 O4 125.2(7) . . ?
O3 N10 C2 118.9(8) . . ?
O4 N10 C2 115.9(7) . . ?
N3 N4 Cu2 117.0(6) . . ?
C2 N4 Cu2 136.4(6) . . ?
C2 N4 N3 103.7(7) . . ?
N4 N3 Cu1 126.1(6) . 2 ?
N2 N3 Cu1 121.0(6) . 2 ?
N2 N3 N4 108.7(7) . . ?
N3 N2 Cu2 124.2(6) . 2_545 ?
N3 N2 N1 108.4(7) . . ?
N1 N2 Cu2 127.5(6) . 2_545 ?
N2 N1 Cu1 116.9(5) . . ?
C2 N1 Cu1 136.4(6) . . ?
C2 N1 N2 105.5(7) . . ?
N6 N7 Cu3 125.7(6) . . ?
C1 N7 Cu3 129.3(6) . . ?
C1 N7 N6 103.8(7) . . ?
N7 N6 Cu3 122.1(6) . 3_676 ?
N7 N6 N5 109.7(7) . . ?
N5 N6 Cu3 124.9(5) . 3_676 ?
N6 N5 Cu2 117.0(5) . . ?
N6 N5 N9 109.1(7) . . ?
N9 N5 Cu2 132.1(6) . . ?
N5 N9 Cu3 131.1(6) . 2_645 ?
C1 N9 Cu3 125.8(6) . 2_645 ?
C1 N9 N5 103.0(7) . . ?
O2 N8 C1 118.3(8) . . ?
O1 N8 O2 125.2(8) . . ?
O1 N8 C1 116.5(7) . . ?
N4 C2 N10 122.1(8) . . ?
N1 C2 N10 124.2(8) . . ?
N1 C2 N4 113.7(7) . . ?
N7 C1 N9 114.4(8) . . ?
N7 C1 N8 121.8(8) . . ?
N9 C1 N8 123.8(8) . . ?

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
Cu3 N7 N6 Cu3 -31.7(10) . . . 3_676 ?
Cu3 N7 N6 N5 167.9(5) . . . . ?
Cu3 N7 C1 N9 -168.2(6) . . . . ?
Cu3 N7 C1 N8 11.4(13) . . . . ?
Cu3 N6 N5 Cu2 34.5(9) 3_676 . . . ?
Cu3 N6 N5 N9 -158.5(6) 3_676 . . . ?
Cu3 N9 C1 N7 -176.2(6) 2_645 . . . ?
Cu3 N9 C1 N8 4.1(13) 2_645 . . . ?
Cu2 N4 N3 Cu1 7.2(9) . . . 2 ?
Cu2 N4 N3 N2 164.1(6) . . . . ?
Cu2 N4 C2 N10 21.7(13) . . . . ?
Cu2 N4 C2 N1 -159.4(7) . . . . ?
Cu2 N2 N1 Cu1 12.2(10) 2_545 . . . ?
Cu2 N2 N1 C2 -178.5(6) 2_545 . . . ?
Cu2 N5 N9 Cu3 -20.0(11) . . . 2_645 ?
Cu2 N5 N9 C1 162.9(7) . . . . ?
Cu1 N3 N2 Cu2 -23.3(10) 2 . . 2_545 ?
Cu1 N3 N2 N1 158.3(6) 2 . . . ?
Cu1 N1 C2 N10 -14.5(15) . . . . ?
Cu1 N1 C2 N4 166.5(6) . . . . ?
O3 N10 C2 N4 -8.2(13) . . . . ?
O3 N10 C2 N1 172.9(9) . . . . ?
O4 N10 C2 N4 172.1(8) . . . . ?
O4 N10 C2 N1 -6.8(13) . . . . ?
O2 N8 C1 N7 166.8(10) . . . . ?
O2 N8 C1 N9 -13.6(14) . . . . ?
O1 N8 C1 N7 -12.0(13) . . . . ?
O1 N8 C1 N9 167.6(9) . . . . ?
N4 N3 N2 Cu2 178.4(6) . . . 2_545 ?
N4 N3 N2 N1 0.0(10) . . . . ?
N3 N4 C2 N10 -179.3(8) . . . . ?
N3 N4 C2 N1 -0.3(10) . . . . ?
N3 N2 N1 Cu1 -169.6(6) . . . . ?
N3 N2 N1 C2 -0.2(10) . . . . ?
N2 N1 C2 N10 179.3(8) . . . . ?
N2 N1 C2 N4 0.3(10) . . . . ?
N7 N6 N5 Cu2 -165.7(5) . . . . ?
N7 N6 N5 N9 1.2(9) . . . . ?
N6 N7 C1 N9 -0.3(11) . . . . ?
N6 N7 C1 N8 179.3(8) . . . . ?
N6 N5 N9 Cu3 175.7(6) . . . 2_645 ?
N6 N5 N9 C1 -1.4(9) . . . . ?
N5 N9 C1 N7 1.1(11) . . . . ?
N5 N9 C1 N8 -178.6(8) . . . . ?
C2 N4 N3 Cu1 -156.7(6) . . . 2 ?
C2 N4 N3 N2 0.1(9) . . . . ?
C1 N7 N6 Cu3 159.8(6) . . . 3_676 ?
C1 N7 N6 N5 -0.6(9) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.156
_oxdiff_exptl_absorpt_empirical_full_min 0.814
