# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2021

####################################################################### 
# 
# 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_glyfencuv_cu
_audit_block_doi                 10.5517/ccdc.csd.cc250hqf
_database_code_depnum_ccdc_archive 'CCDC 1996484'
loop_
_citation_id
_citation_doi
_citation_year
1 10.3390/cryst10060492 2020
loop_
_audit_author_name
_audit_author_address
'Angel Mendoza'
;BUAP
Mexico
;
_audit_update_record             
;
2020-04-12 deposited with the CCDC.	2021-02-09 downloaded from the CCDC.
;
_audit_creation_date             2020-04-12
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.01.31 svn.r88ba2a32 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C14 H14 Cu N3 O3, C14 H12 Cu N3 O8 V2, 4(H2 O), H2 O0.786, 0.214(O)'
_chemical_formula_sum            'C28 H36 Cu2 N6 O16 V2'
_chemical_formula_weight         941.59
_chemical_melting_point          ?
_chemical_oxdiff_formula         C28H36N6Cu2V2O16
_chemical_oxdiff_usercomment     'Eduardo Sanchez Lara'
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'
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'
V V 0.0687 2.1097 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.9249(4)
_cell_length_b                   13.2626(4)
_cell_length_c                   13.5191(4)
_cell_angle_alpha                109.108(3)
_cell_angle_beta                 95.685(3)
_cell_angle_gamma                113.173(3)
_cell_volume                     1792.27(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12971
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      77.1460
_cell_measurement_theta_min      3.5460
_shelx_estimated_absorpt_T_max   0.736
_shelx_estimated_absorpt_T_min   0.252
_exptl_absorpt_coefficient_mu    6.292
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.572
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             956
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
7 -7 2 0.0640
-6 2 -4 0.0837
1 0 8 0.0197
6 -7 -1 0.0625
-2 -7 3 0.1585
0 3 -9 0.0551
2 -2 -8 0.0180
-7 1 4 0.1240
1 7 -2 0.1138
1 -2 8 0.0348
-7 6 2 0.0723
-1 1 -8 0.0246
7 -6 -1 0.0639

_exptl_crystal_size_max          0.303
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.052
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
6.9975 -6.9961 2.0038 0.5537 -0.8793 0.0426
-5.9838 1.9837 -4.0002 -0.8396 0.3332 0.4137
0.9971 0.0027 7.9963 0.9794 0.3556 -0.1026
5.9988 -6.9972 -0.9949 0.1405 -0.9713 0.1479
-1.9997 -6.9977 3.0012 0.0059 -0.2311 1.0052
0.0027 2.9964 -8.9969 -0.9391 -0.2510 -0.3434
2.0101 -2.0084 -7.9874 -0.8113 -0.7038 0.0074
-6.9990 0.9995 3.9959 -0.0344 0.7485 0.6376
0.9997 6.9978 -2.0019 0.0339 0.3500 -0.8978
0.9972 -1.9968 7.9972 0.9260 0.2066 0.1231
-6.9987 5.9976 1.9947 -0.1274 1.0156 0.0724
-0.9971 0.9970 -7.9967 -0.9527 -0.2811 -0.0103
6.9984 -5.9973 -0.9952 0.2407 -0.9629 -0.0718

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            38143
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.355
_diffrn_reflns_theta_min         3.586
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5564
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9862
_diffrn_measured_fraction_theta_max 0.9972
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

 # Type Start End Width tₑₓₚ ω θ κ φ Frames
#--------------------------------------------------------------------------
 1 ω -95.00 3.00 1.00 1.91 -- -41.16 125.00 -30.00 98
 2 ω -117.00 -15.00 1.00 1.91 -- -41.16 -38.00 120.00 102
 3 ω -117.00 -15.00 1.00 1.91 -- -41.16 -38.00 30.00 102
 4 ω -95.00 3.00 1.00 1.91 -- -41.16 125.00-180.00 98
 5 ω -115.00 -67.00 1.00 1.91 -- -41.16-134.00 171.00 48
 6 ω 24.00 103.00 1.00 1.91 -- 41.16-134.00 171.00 79
 7 ω 18.00 98.00 1.00 1.91 -- 41.16-125.00 0.00 80
 8 ω 100.00 178.00 1.00 7.63 -- 115.00 111.00 -90.00 78
 9 ω 57.00 178.00 1.00 7.63 -- 115.00 16.00 39.56 121
 10 ω 40.00 147.00 1.00 7.63 -- 115.00 -68.00 -36.01 107
 11 ω 84.00 178.00 1.00 7.63 -- 115.00 30.00 120.00 94
 12 ω 37.00 116.00 1.00 7.63 -- 115.00-111.00 90.00 79
 13 ω 31.00 109.00 1.00 7.63 -- 115.00 -95.00 90.00 78
 14 ω 37.00 116.00 1.00 7.63 -- 115.00-111.00 150.00 79
 15 ω 57.00 150.00 1.00 7.63 -- 115.00 178.00 -90.00 93
 16 ω 85.00 178.00 1.00 7.63 -- 115.00 61.00-180.00 93
 17 ω 37.00 116.00 1.00 7.63 -- 115.00-111.00-150.00 79
 18 ω 37.00 116.00 1.00 7.63 -- 115.00-111.00 -60.00 79
 19 ω 37.00 116.00 1.00 7.63 -- 115.00-111.00 -30.00 79
 20 ω 31.00 109.00 1.00 7.63 -- 115.00 -95.00-180.00 78
 21 ω 100.00 178.00 1.00 7.63 -- 115.00 111.00 150.00 78
 22 ω 37.00 116.00 1.00 7.63 -- 115.00-111.00 -90.00 79
 23 ω 81.00 178.00 1.00 7.63 -- 115.00 77.00 -60.00 97
 24 ω 85.00 178.00 1.00 7.63 -- 115.00 61.00-120.00 93
 25 ω 36.00 149.00 1.00 7.63 -- 115.00 -77.00-120.00 113
 26 ω 31.00 109.00 1.00 7.63 -- 115.00 -95.00-150.00 78
 27 ω 40.00 143.00 1.00 7.63 -- 115.00 -45.00 0.00 103
 28 ω 31.00 109.00 1.00 7.63 -- 115.00 -95.00 -30.00 78
 29 ω 84.00 178.00 1.00 7.63 -- 115.00 30.00-120.00 94
 30 ω 57.00 150.00 1.00 7.63 -- 115.00 178.00-120.00 93
 31 ω 31.00 109.00 1.00 7.63 -- 115.00 -95.00 120.00 78
 32 ω 37.00 146.00 1.00 7.63 -- 115.00 -30.00-120.00 109
 33 ω 31.00 109.00 1.00 7.63 -- 115.00 -95.00 30.00 78
 34 ω 37.00 116.00 1.00 7.63 -- 115.00-111.00 30.00 79
 35 ω 37.00 146.00 1.00 7.63 -- 115.00 -30.00-180.00 109
 36 ω 32.00 176.00 1.00 7.63 -- 115.00 -15.00 120.00 144
 37 ω 99.00 149.00 1.00 7.63 -- 115.00 -82.00-154.37 50
 38 ω 31.00 67.00 1.00 7.63 -- 115.00 -95.00 -60.00 36
 39 ω 72.00 98.00 1.00 7.63 -- 115.00 -95.00 -60.00 26
 40 ω 119.00 145.00 1.00 7.63 -- 115.00 45.00 60.00 26
 41 ω 86.00 116.00 1.00 7.63 -- 115.00 61.00 60.00 30
 42 ω 72.00 98.00 1.00 7.63 -- 115.00 -77.00-180.00 26
 43 ω 34.00 81.00 1.00 7.63 -- 115.00 -82.00-154.37 47
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0734398000
_diffrn_orient_matrix_UB_12      0.0267657000
_diffrn_orient_matrix_UB_13      0.1133180000
_diffrn_orient_matrix_UB_21      -0.0662099000
_diffrn_orient_matrix_UB_22      0.0745528000
_diffrn_orient_matrix_UB_23      0.0527051000
_diffrn_orient_matrix_UB_31      -0.1069102000
_diffrn_orient_matrix_UB_32      -0.1128682000
_diffrn_orient_matrix_UB_33      0.0005437000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6525
_reflns_number_total             7587
_reflns_odcompleteness_completeness 98.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     78.17
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXD (Sheldrick, 2008)'
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       0.00035(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         7587
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0372
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0495P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0913
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Sof(O13A)=1-FVAR(1)
 Sof(O13)=FVAR(1)
 Sof(O10B)=1-FVAR(2)
 Sof(O10A)=FVAR(2)
 Sof(O8B)=1-FVAR(3)
 Sof(O8A)=FVAR(3)
3.a Free rotating group:
 O12(H12A,H12B), O11(H11A,H11B), O14(H14A,H14B), O10B(H10A,H10B), O13(H13A,H13B)
3.b Rotating group:
 O9(H9A,H9B)
3.c Secondary CH2 refined with riding coordinates:
 N6(H6A,H6B), N3(H3A,H3B), C26(H26A,H26B), C28(H28A,H28B)
3.d Aromatic/amide H refined with riding coordinates:
 C14(H14), C22(H22), C18(H18), C13(H13), C1(H1), C21(H21), C17(H17), C9(H9),
 C10(H10), C3(H3), C8(H8), C6(H6), C15(H15), C20(H20), C5(H5), C2(H2)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
Cu2 Cu 0.19892(3) -0.04258(3) 0.84001(3) 0.03431(9) Uani 1 1 d . . . . .
Cu1 Cu 0.92577(3) 0.16576(3) 0.67621(3) 0.03308(9) Uani 1 1 d . . . . .
V1 V 0.97277(3) 0.35119(3) 0.53146(3) 0.02772(9) Uani 1 1 d . . . . .
V2 V 1.17744(3) 0.48691(3) 0.42003(3) 0.02987(9) Uani 1 1 d . . . . .
O4 O 1.04724(15) 0.35750(14) 0.42210(14) 0.0374(3) Uani 1 1 d . . . . .
O15 O 1.07510(16) 0.13987(16) 0.67296(17) 0.0442(4) Uani 1 1 d . . . . .
N5 N 0.30241(17) -0.13300(17) 0.80957(15) 0.0332(3) Uani 1 1 d . . . . .
O2 O 0.83819(15) 0.37934(14) 0.51135(15) 0.0389(3) Uani 1 1 d . . . . .
N2 N 0.80656(18) -0.01013(16) 0.60010(16) 0.0352(4) Uani 1 1 d . . . . .
O1 O 0.92658(16) 0.21601(14) 0.53352(14) 0.0375(3) Uani 1 1 d . . . . .
N1 N 0.76301(18) 0.17680(18) 0.68903(17) 0.0363(4) Uani 1 1 d . . . . .
O5 O 1.1682(2) 0.46209(19) 0.29214(17) 0.0544(5) Uani 1 1 d . . . . .
N4 N 0.36962(17) 0.09869(17) 0.90686(15) 0.0341(4) Uani 1 1 d . . . . .
O7 O 0.11537(17) 0.05540(18) 0.8915(2) 0.0564(5) Uani 1 1 d . . . . .
C23 C 0.46423(19) 0.0673(2) 0.89997(17) 0.0324(4) Uani 1 1 d . . . . .
N6 N 0.03091(18) -0.18064(18) 0.80639(19) 0.0425(4) Uani 1 1 d . . . . .
H6A H 0.012928 -0.235597 0.740068 0.051 Uiso 1 1 calc R U . . .
H6B H 0.031355 -0.214074 0.853673 0.051 Uiso 1 1 calc R U . . .
O3 O 1.07162(18) 0.45266(16) 0.64680(16) 0.0473(4) Uani 1 1 d . . . . .
C12 C 0.6855(2) -0.0332(2) 0.60030(18) 0.0352(4) Uani 1 1 d . . . . .
C24 C 0.4281(2) -0.0577(2) 0.84820(16) 0.0324(4) Uani 1 1 d . . . . .
N3 N 1.0439(2) 0.32377(19) 0.79421(19) 0.0454(5) Uani 1 1 d . . . . .
H3A H 1.035329 0.381875 0.780337 0.054 Uiso 1 1 calc R U . . .
H3B H 1.025466 0.326575 0.856973 0.054 Uiso 1 1 calc R U . . .
C11 C 0.6614(2) 0.0672(2) 0.64662(18) 0.0351(4) Uani 1 1 d . . . . .
C27 C 1.1791(2) 0.2287(2) 0.7333(2) 0.0396(5) Uani 1 1 d . . . . .
C7 C 0.5373(2) 0.0503(3) 0.6452(2) 0.0417(5) Uani 1 1 d . . . . .
C16 C 0.5203(2) -0.0984(2) 0.83719(18) 0.0379(4) Uani 1 1 d . . . . .
C14 C 0.3513(3) -0.2971(2) 0.7434(2) 0.0457(5) Uani 1 1 d . . . . .
H14 H 0.322355 -0.379034 0.706697 0.055 Uiso 1 1 calc R U . . .
O6 O 1.31463(17) 0.50229(18) 0.4777(2) 0.0538(5) Uani 1 1 d . . . . .
C19 C 0.5924(2) 0.1509(2) 0.93977(19) 0.0386(5) Uani 1 1 d . . . . .
O12 O 0.5150(2) 0.5476(2) 0.6438(2) 0.0618(5) Uani 1 1 d G . . . .
H12A H 0.574810 0.538358 0.619501 0.093 Uiso 1 1 d G U . . .
H12B H 0.455390 0.530078 0.591511 0.093 Uiso 1 1 d G U . . .
O16 O 1.28238(19) 0.2275(2) 0.7374(2) 0.0555(5) Uani 1 1 d . . . . .
O9 O 0.1778(2) -0.03555(18) 0.67407(17) 0.0559(5) Uani 1 1 d . . . . .
H9A H 0.193899 0.035417 0.680885 0.084 Uiso 1 1 d R U . . .
H9B H 0.145479 -0.091843 0.612625 0.084 Uiso 1 1 d R U . . .
C22 C 0.3977(2) 0.2136(2) 0.9539(2) 0.0427(5) Uani 1 1 d . . . . .
H22 H 0.332651 0.235382 0.959704 0.051 Uiso 1 1 calc R U . . .
C18 C 0.6854(2) 0.1074(3) 0.9272(2) 0.0464(6) Uani 1 1 d . . . . .
H18 H 0.770719 0.161724 0.953000 0.056 Uiso 1 1 calc R U . . .
C13 C 0.2657(2) -0.2492(2) 0.7581(2) 0.0399(5) Uani 1 1 d . . . . .
H13 H 0.179678 -0.300894 0.730824 0.048 Uiso 1 1 calc R U . . .
C26 C -0.0647(2) -0.1354(3) 0.8132(3) 0.0553(7) Uani 1 1 d . . . . .
H26A H -0.119256 -0.167473 0.855247 0.066 Uiso 1 1 calc R U . . .
H26B H -0.116628 -0.163235 0.740844 0.066 Uiso 1 1 calc R U . . .
C4 C 0.5855(2) -0.1502(2) 0.5567(2) 0.0434(5) Uani 1 1 d . . . . .
C1 C 0.8327(3) -0.1010(2) 0.5574(2) 0.0460(5) Uani 1 1 d . . . . .
H1 H 0.915601 -0.085193 0.556179 0.055 Uiso 1 1 calc R U . . .
C21 C 0.5240(3) 0.3031(2) 0.9953(2) 0.0506(6) Uani 1 1 d . . . . .
H21 H 0.541660 0.383219 1.026974 0.061 Uiso 1 1 calc R U . . .
C17 C 0.6511(2) -0.0114(3) 0.8783(2) 0.0456(5) Uani 1 1 d . . . . .
H17 H 0.713328 -0.036881 0.871300 0.055 Uiso 1 1 calc R U . . .
O11 O 0.4805(2) 0.4601(3) 0.8074(2) 0.0709(7) Uani 1 1 d G . . . .
H11A H 0.470137 0.475776 0.742889 0.106 Uiso 1 1 d G U . . .
H11B H 0.422916 0.380815 0.792217 0.106 Uiso 1 1 d G U . . .
C9 C 0.6223(3) 0.2630(3) 0.7282(3) 0.0525(6) Uani 1 1 d . . . . .
H9 H 0.611716 0.331878 0.755313 0.063 Uiso 1 1 calc R U . . .
C28 C 1.1732(3) 0.3416(3) 0.8021(3) 0.0539(6) Uani 1 1 d . . . . .
H28A H 1.215520 0.366818 0.877202 0.065 Uiso 1 1 calc R U . . .
H28B H 1.217843 0.404844 0.778797 0.065 Uiso 1 1 calc R U . . .
C10 C 0.7435(3) 0.2719(2) 0.7279(2) 0.0463(5) Uani 1 1 d . . . . .
H10 H 0.812422 0.347497 0.756049 0.056 Uiso 1 1 calc R U . . .
O14 O 1.0233(3) 0.2764(3) 0.9998(3) 0.0763(7) Uani 1 1 d G . . . .
H14A H 1.103549 0.308009 1.015297 0.114 Uiso 1 1 d G U . . .
H14B H 0.992842 0.208836 0.946534 0.114 Uiso 1 1 d G U . . .
C3 C 0.6163(3) -0.2441(2) 0.5136(2) 0.0547(7) Uani 1 1 d . . . . .
H3 H 0.553389 -0.322883 0.484585 0.066 Uiso 1 1 calc R U . . .
C8 C 0.5206(3) 0.1534(3) 0.6887(2) 0.0507(6) Uani 1 1 d . . . . .
H8 H 0.440263 0.146775 0.690410 0.061 Uiso 1 1 calc R U . . .
C6 C 0.4364(2) -0.0703(3) 0.5988(2) 0.0509(6) Uani 1 1 d . . . . .
H6 H 0.353723 -0.082853 0.596940 0.061 Uiso 1 1 calc R U . . .
C15 C 0.4784(3) -0.2220(3) 0.7835(2) 0.0460(5) Uani 1 1 d . . . . .
H15 H 0.536417 -0.252801 0.775213 0.055 Uiso 1 1 calc R U . . .
O10B O 0.751(3) 0.552(2) 0.8898(19) 0.064(8) Uani 0.14(3) 1 d G . P A 2
H10A H 0.748980 0.579680 0.824854 0.096 Uiso 1 1 d G U . . .
H10B H 0.646297 0.556358 0.869411 0.096 Uiso 1 1 d G U . . .
C20 C 0.6207(2) 0.2724(2) 0.9889(2) 0.0472(6) Uani 1 1 d . . . . .
H20 H 0.704267 0.331168 1.016697 0.057 Uiso 1 1 calc R U . . .
C25 C -0.0041(3) -0.0004(3) 0.8652(3) 0.0612(8) Uani 1 1 d . . . . .
O8B O -0.0746(16) 0.0520(17) 0.853(3) 0.056(5) Uani 0.34(11) 1 d . . P B 2
O13 O 0.9411(4) 0.4270(4) 1.1286(3) 0.0825(13) Uani 0.786(9) 1 d G . P C 1
H13A H 0.982031 0.440364 1.190357 0.124 Uiso 1 1 d G U . C 1
H13B H 0.974372 0.394375 1.083958 0.124 Uiso 1 1 d G U . C 1
C5 C 0.4594(3) -0.1650(3) 0.5581(2) 0.0516(7) Uani 1 1 d . . . . .
H5 H 0.392530 -0.241723 0.530188 0.062 Uiso 1 1 calc R U . . .
C2 C 0.7389(3) -0.2201(3) 0.5140(3) 0.0562(7) Uani 1 1 d . . . . .
H2 H 0.759820 -0.282336 0.485772 0.067 Uiso 1 1 calc R U . . .
O13A O 0.944(3) 0.4621(19) 1.031(2) 0.138(11) Uani 0.214(9) 1 d . . P C 2
O10A O 0.7346(4) 0.6032(14) 0.8834(5) 0.119(5) Uani 0.86(3) 1 d . . P A 1
O8A O -0.0719(10) 0.0453(10) 0.894(5) 0.088(10) Uani 0.66(11) 1 d . . P B 1


_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
Cu2 N5 2.0181(19) . ?
Cu2 N4 1.9991(18) . ?
Cu2 O7 1.9313(19) . ?
Cu2 N6 1.9901(19) . ?
Cu2 O9 2.269(2) . ?
Cu1 O15 1.9437(18) . ?
Cu1 N2 2.0125(19) . ?
Cu1 O1 2.2373(16) . ?
Cu1 N1 2.023(2) . ?
Cu1 N3 1.991(2) . ?
V1 O4 1.8067(16) . ?
V1 O2 1.8000(16) . ?
V1 O1 1.6664(15) . ?
V1 O3 1.6265(18) . ?
V2 O4 1.8166(15) . ?
V2 O2 1.8054(17) 2_766 ?
V2 O5 1.634(2) . ?
V2 O6 1.6449(19) . ?
O15 C27 1.270(3) . ?
N5 C24 1.358(3) . ?
N5 C13 1.326(3) . ?
N2 C12 1.354(3) . ?
N2 C1 1.325(3) . ?
N1 C11 1.357(3) . ?
N1 C10 1.321(3) . ?
N4 C23 1.349(3) . ?
N4 C22 1.327(3) . ?
O7 C25 1.265(4) . ?
C23 C24 1.429(3) . ?
C23 C19 1.403(3) . ?
N6 H6A 0.8900 . ?
N6 H6B 0.8900 . ?
N6 C26 1.480(4) . ?
C12 C11 1.426(4) . ?
C12 C4 1.409(3) . ?
C24 C16 1.403(3) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 C28 1.453(3) . ?
C11 C7 1.405(3) . ?
C27 O16 1.234(3) . ?
C27 C28 1.514(4) . ?
C7 C8 1.403(4) . ?
C7 C6 1.442(4) . ?
C16 C17 1.436(4) . ?
C16 C15 1.403(4) . ?
C14 H14 0.9300 . ?
C14 C13 1.397(4) . ?
C14 C15 1.370(4) . ?
C19 C18 1.437(4) . ?
C19 C20 1.407(4) . ?
O12 H12A 0.8490 . ?
O12 H12B 0.8495 . ?
O9 H9A 0.8536 . ?
O9 H9B 0.8367 . ?
C22 H22 0.9300 . ?
C22 C21 1.408(4) . ?
C18 H18 0.9300 . ?
C18 C17 1.358(4) . ?
C13 H13 0.9300 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 C25 1.510(4) . ?
C4 C3 1.397(5) . ?
C4 C5 1.440(4) . ?
C1 H1 0.9300 . ?
C1 C2 1.401(4) . ?
C21 H21 0.9300 . ?
C21 C20 1.368(5) . ?
C17 H17 0.9300 . ?
O11 H11A 0.9671 . ?
O11 H11B 0.9394 . ?
C9 H9 0.9300 . ?
C9 C10 1.403(4) . ?
C9 C8 1.359(5) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C10 H10 0.9300 . ?
O14 H14A 0.8499 . ?
O14 H14B 0.8502 . ?
C3 H3 0.9300 . ?
C3 C2 1.367(5) . ?
C8 H8 0.9300 . ?
C6 H6 0.9300 . ?
C6 C5 1.342(5) . ?
C15 H15 0.9300 . ?
O10B H10A 1.0571 . ?
O10B H10B 1.2794 . ?
C20 H20 0.9300 . ?
C25 O8B 1.314(18) . ?
C25 O8A 1.212(9) . ?
O13 H13A 0.8495 . ?
O13 H13B 0.8493 . ?
C5 H5 0.9300 . ?
C2 H2 0.9300 . ?
O13A O13A 1.80(4) 2_767 ?
O10A H10A 0.8123 . ?
O10A H10B 0.9484 . ?

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
N5 Cu2 O9 93.36(8) . . ?
N4 Cu2 N5 82.54(8) . . ?
N4 Cu2 O9 95.46(8) . . ?
O7 Cu2 N5 171.33(9) . . ?
O7 Cu2 N4 91.98(8) . . ?
O7 Cu2 N6 85.36(9) . . ?
O7 Cu2 O9 93.85(10) . . ?
N6 Cu2 N5 98.55(9) . . ?
N6 Cu2 N4 167.52(9) . . ?
N6 Cu2 O9 96.88(9) . . ?
O15 Cu1 N2 93.17(8) . . ?
O15 Cu1 O1 96.07(7) . . ?
O15 Cu1 N1 172.30(8) . . ?
O15 Cu1 N3 84.45(9) . . ?
N2 Cu1 O1 99.22(7) . . ?
N2 Cu1 N1 82.27(8) . . ?
N1 Cu1 O1 90.81(7) . . ?
N3 Cu1 N2 160.41(9) . . ?
N3 Cu1 O1 100.37(9) . . ?
N3 Cu1 N1 97.76(9) . . ?
O2 V1 O4 109.63(8) . . ?
O1 V1 O4 109.14(8) . . ?
O1 V1 O2 109.83(8) . . ?
O3 V1 O4 110.12(9) . . ?
O3 V1 O2 108.48(10) . . ?
O3 V1 O1 109.63(9) . . ?
O2 V2 O4 110.03(7) 2_766 . ?
O5 V2 O4 106.07(9) . . ?
O5 V2 O2 110.49(10) . 2_766 ?
O5 V2 O6 109.22(12) . . ?
O6 V2 O4 111.35(10) . . ?
O6 V2 O2 109.64(10) . 2_766 ?
V1 O4 V2 126.98(9) . . ?
C27 O15 Cu1 115.95(16) . . ?
C24 N5 Cu2 111.36(15) . . ?
C13 N5 Cu2 130.10(16) . . ?
C13 N5 C24 118.5(2) . . ?
V1 O2 V2 128.97(10) . 2_766 ?
C12 N2 Cu1 111.95(15) . . ?
C1 N2 Cu1 128.97(18) . . ?
C1 N2 C12 119.0(2) . . ?
V1 O1 Cu1 128.99(9) . . ?
C11 N1 Cu1 111.79(16) . . ?
C10 N1 Cu1 129.90(17) . . ?
C10 N1 C11 118.3(2) . . ?
C23 N4 Cu2 112.49(15) . . ?
C22 N4 Cu2 128.32(17) . . ?
C22 N4 C23 119.2(2) . . ?
C25 O7 Cu2 115.0(2) . . ?
N4 C23 C24 116.63(19) . . ?
N4 C23 C19 123.0(2) . . ?
C19 C23 C24 120.3(2) . . ?
Cu2 N6 H6A 110.1 . . ?
Cu2 N6 H6B 110.1 . . ?
H6A N6 H6B 108.4 . . ?
C26 N6 Cu2 107.93(16) . . ?
C26 N6 H6A 110.1 . . ?
C26 N6 H6B 110.1 . . ?
N2 C12 C11 117.17(19) . . ?
N2 C12 C4 122.6(2) . . ?
C4 C12 C11 120.2(2) . . ?
N5 C24 C23 116.98(19) . . ?
N5 C24 C16 122.5(2) . . ?
C16 C24 C23 120.5(2) . . ?
Cu1 N3 H3A 109.7 . . ?
Cu1 N3 H3B 109.7 . . ?
H3A N3 H3B 108.2 . . ?
C28 N3 Cu1 109.79(17) . . ?
C28 N3 H3A 109.7 . . ?
C28 N3 H3B 109.7 . . ?
N1 C11 C12 116.7(2) . . ?
N1 C11 C7 123.0(2) . . ?
C7 C11 C12 120.3(2) . . ?
O15 C27 C28 116.9(2) . . ?
O16 C27 O15 123.6(3) . . ?
O16 C27 C28 119.5(2) . . ?
C11 C7 C6 118.4(3) . . ?
C8 C7 C11 117.0(2) . . ?
C8 C7 C6 124.6(3) . . ?
C24 C16 C17 118.3(2) . . ?
C15 C16 C24 117.5(2) . . ?
C15 C16 C17 124.1(2) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
C15 C14 C13 119.4(2) . . ?
C23 C19 C18 118.3(2) . . ?
C23 C19 C20 117.1(2) . . ?
C20 C19 C18 124.6(2) . . ?
H12A O12 H12B 109.6 . . ?
Cu2 O9 H9A 109.7 . . ?
Cu2 O9 H9B 129.3 . . ?
H9A O9 H9B 119.9 . . ?
N4 C22 H22 119.4 . . ?
N4 C22 C21 121.3(2) . . ?
C21 C22 H22 119.4 . . ?
C19 C18 H18 119.3 . . ?
C17 C18 C19 121.3(2) . . ?
C17 C18 H18 119.3 . . ?
N5 C13 C14 122.6(2) . . ?
N5 C13 H13 118.7 . . ?
C14 C13 H13 118.7 . . ?
N6 C26 H26A 109.3 . . ?
N6 C26 H26B 109.3 . . ?
N6 C26 C25 111.8(2) . . ?
H26A C26 H26B 107.9 . . ?
C25 C26 H26A 109.3 . . ?
C25 C26 H26B 109.3 . . ?
C12 C4 C5 118.3(3) . . ?
C3 C4 C12 117.1(3) . . ?
C3 C4 C5 124.7(2) . . ?
N2 C1 H1 119.1 . . ?
N2 C1 C2 121.9(3) . . ?
C2 C1 H1 119.1 . . ?
C22 C21 H21 120.0 . . ?
C20 C21 C22 120.1(3) . . ?
C20 C21 H21 120.0 . . ?
C16 C17 H17 119.4 . . ?
C18 C17 C16 121.2(2) . . ?
C18 C17 H17 119.4 . . ?
H11A O11 H11B 109.2 . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C8 C9 C10 119.7(3) . . ?
N3 C28 C27 112.0(2) . . ?
N3 C28 H28A 109.2 . . ?
N3 C28 H28B 109.2 . . ?
C27 C28 H28A 109.2 . . ?
C27 C28 H28B 109.2 . . ?
H28A C28 H28B 107.9 . . ?
N1 C10 C9 122.3(3) . . ?
N1 C10 H10 118.8 . . ?
C9 C10 H10 118.8 . . ?
H14A O14 H14B 109.5 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 C4 120.0(2) . . ?
C2 C3 H3 120.0 . . ?
C7 C8 H8 120.2 . . ?
C9 C8 C7 119.6(2) . . ?
C9 C8 H8 120.2 . . ?
C7 C6 H6 119.3 . . ?
C5 C6 C7 121.4(2) . . ?
C5 C6 H6 119.3 . . ?
C16 C15 H15 120.3 . . ?
C14 C15 C16 119.5(2) . . ?
C14 C15 H15 120.3 . . ?
H10A O10B H10B 72.2 . . ?
C19 C20 H20 120.3 . . ?
C21 C20 C19 119.3(2) . . ?
C21 C20 H20 120.3 . . ?
O7 C25 C26 117.7(3) . . ?
O7 C25 O8B 121.7(10) . . ?
O8B C25 C26 117.7(8) . . ?
O8A C25 O7 124.2(6) . . ?
O8A C25 C26 117.1(6) . . ?
H13A O13 H13B 104.5 . . ?
C4 C5 H5 119.3 . . ?
C6 C5 C4 121.4(2) . . ?
C6 C5 H5 119.3 . . ?
C1 C2 H2 120.3 . . ?
C3 C2 C1 119.5(3) . . ?
C3 C2 H2 120.3 . . ?
H10A O10A H10B 103.8 . . ?

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
Cu2 N5 C24 C23 -0.9(2) . . . . ?
Cu2 N5 C24 C16 -179.89(16) . . . . ?
Cu2 N5 C13 C14 179.43(19) . . . . ?
Cu2 N4 C23 C24 -0.3(2) . . . . ?
Cu2 N4 C23 C19 179.08(17) . . . . ?
Cu2 N4 C22 C21 -178.6(2) . . . . ?
Cu2 O7 C25 C26 8.9(5) . . . . ?
Cu2 O7 C25 O8B -151.3(17) . . . . ?
Cu2 O7 C25 O8A 177(4) . . . . ?
Cu2 N6 C26 C25 -12.0(3) . . . . ?
Cu1 O15 C27 O16 -177.5(2) . . . . ?
Cu1 O15 C27 C28 1.7(3) . . . . ?
Cu1 N2 C12 C11 3.5(2) . . . . ?
Cu1 N2 C12 C4 -176.78(17) . . . . ?
Cu1 N2 C1 C2 175.1(2) . . . . ?
Cu1 N1 C11 C12 -1.0(2) . . . . ?
Cu1 N1 C11 C7 -179.87(17) . . . . ?
Cu1 N1 C10 C9 178.4(2) . . . . ?
Cu1 N3 C28 C27 -9.8(3) . . . . ?
O4 V1 O2 V2 -104.28(13) . . . 2_766 ?
O4 V1 O1 Cu1 143.82(11) . . . . ?
O15 C27 C28 N3 5.7(4) . . . . ?
N5 C24 C16 C17 178.4(2) . . . . ?
N5 C24 C16 C15 0.2(3) . . . . ?
O2 V1 O4 V2 93.11(13) . . . . ?
O2 V1 O1 Cu1 -95.97(12) . . . . ?
O2 V2 O4 V1 -37.20(15) 2_766 . . . ?
N2 C12 C11 N1 -1.7(3) . . . . ?
N2 C12 C11 C7 177.2(2) . . . . ?
N2 C12 C4 C3 0.9(3) . . . . ?
N2 C12 C4 C5 -178.2(2) . . . . ?
N2 C1 C2 C3 1.2(5) . . . . ?
O1 V1 O4 V2 -146.56(12) . . . . ?
O1 V1 O2 V2 135.81(12) . . . 2_766 ?
N1 C11 C7 C8 1.1(3) . . . . ?
N1 C11 C7 C6 -179.6(2) . . . . ?
O5 V2 O4 V1 -156.71(13) . . . . ?
N4 C23 C24 N5 0.8(3) . . . . ?
N4 C23 C24 C16 179.8(2) . . . . ?
N4 C23 C19 C18 -179.4(2) . . . . ?
N4 C23 C19 C20 0.1(3) . . . . ?
N4 C22 C21 C20 -1.0(4) . . . . ?
C23 N4 C22 C21 0.9(4) . . . . ?
C23 C24 C16 C17 -0.5(3) . . . . ?
C23 C24 C16 C15 -178.7(2) . . . . ?
C23 C19 C18 C17 -0.1(4) . . . . ?
C23 C19 C20 C21 -0.2(4) . . . . ?
N6 C26 C25 O7 2.7(5) . . . . ?
N6 C26 C25 O8B 163.7(18) . . . . ?
N6 C26 C25 O8A -166(4) . . . . ?
O3 V1 O4 V2 -26.17(16) . . . . ?
O3 V1 O2 V2 16.01(15) . . . 2_766 ?
O3 V1 O1 Cu1 23.13(15) . . . . ?
C12 N2 C1 C2 -1.0(4) . . . . ?
C12 C11 C7 C8 -177.7(2) . . . . ?
C12 C11 C7 C6 1.6(3) . . . . ?
C12 C4 C3 C2 -0.6(4) . . . . ?
C12 C4 C5 C6 0.6(4) . . . . ?
C24 N5 C13 C14 0.8(4) . . . . ?
C24 C23 C19 C18 -0.1(3) . . . . ?
C24 C23 C19 C20 179.5(2) . . . . ?
C24 C16 C17 C18 0.3(4) . . . . ?
C24 C16 C15 C14 0.7(4) . . . . ?
C11 N1 C10 C9 1.0(4) . . . . ?
C11 C12 C4 C3 -179.5(2) . . . . ?
C11 C12 C4 C5 1.4(3) . . . . ?
C11 C7 C8 C9 0.8(4) . . . . ?
C11 C7 C6 C5 0.4(4) . . . . ?
C7 C6 C5 C4 -1.5(4) . . . . ?
O6 V2 O4 V1 84.57(15) . . . . ?
C19 C23 C24 N5 -178.53(19) . . . . ?
C19 C23 C24 C16 0.4(3) . . . . ?
C19 C18 C17 C16 0.0(4) . . . . ?
O16 C27 C28 N3 -175.0(3) . . . . ?
C22 N4 C23 C24 -179.9(2) . . . . ?
C22 N4 C23 C19 -0.5(3) . . . . ?
C22 C21 C20 C19 0.6(4) . . . . ?
C18 C19 C20 C21 179.3(3) . . . . ?
C13 N5 C24 C23 178.0(2) . . . . ?
C13 N5 C24 C16 -1.0(3) . . . . ?
C13 C14 C15 C16 -1.0(4) . . . . ?
C4 C12 C11 N1 178.6(2) . . . . ?
C4 C12 C11 C7 -2.5(3) . . . . ?
C4 C3 C2 C1 -0.4(5) . . . . ?
C1 N2 C12 C11 -179.7(2) . . . . ?
C1 N2 C12 C4 -0.1(3) . . . . ?
C17 C16 C15 C14 -177.3(2) . . . . ?
C10 N1 C11 C12 176.8(2) . . . . ?
C10 N1 C11 C7 -2.0(3) . . . . ?
C10 C9 C8 C7 -1.7(4) . . . . ?
C3 C4 C5 C6 -178.5(3) . . . . ?
C8 C7 C6 C5 179.6(3) . . . . ?
C8 C9 C10 N1 0.8(5) . . . . ?
C6 C7 C8 C9 -178.5(3) . . . . ?
C15 C16 C17 C18 178.3(2) . . . . ?
C15 C14 C13 N5 0.2(4) . . . . ?
C20 C19 C18 C17 -179.6(3) . . . . ?
C5 C4 C3 C2 178.4(3) . . . . ?

_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 1.567
_oxdiff_exptl_absorpt_empirical_full_min 0.853
####################################################################### 
# 
# 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_lolacuv_1_mo
_database_code_depnum_ccdc_archive 'CCDC 2044082'
loop_
_audit_author_name
_audit_author_address
'Eduardo Sanchez'
;Benemerita Universidad Autonoma de Puebla
Mexico
;
_audit_update_record             
;
2020-11-12 deposited with the CCDC.	2021-02-09 downloaded from the CCDC.
;
_audit_creation_date             2017-11-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C34 H40 Cu2 N8 O16 V4, 6(H2 O)'
_chemical_formula_sum            'C34 H52 Cu2 N8 O22 V4'
_chemical_formula_weight         1255.67
_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 0.0033 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'
V V 0.3005 0.5294 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.9373(3)
_cell_length_b                   11.4902(4)
_cell_length_c                   12.9580(4)
_cell_angle_alpha                70.470(3)
_cell_angle_beta                 73.209(3)
_cell_angle_gamma                80.836(3)
_cell_volume                     1197.75(7)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    7258
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5160
_cell_measurement_theta_min      3.2910
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.708
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87097
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             638
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            26431
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.917
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3994
_reflns_number_total             4904
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_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 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         4904
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0586
_refine_ls_restrained_S_all      1.105
_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)+(0.0538P)²+3.7280P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1502
_refine_ls_wR_factor_ref         0.1582
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H,H)
  groups
 At 1.5 times of:
  All N(H,H,H,H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O9-H9A = O9-H9B
 0.85 with sigma of 0.02
 H9A-H9B
 1.34 with sigma of 0.04
 O10-H10A = O10-H10B
 0.85 with sigma of 0.02
 H10A-H10B
 1.34 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 O5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C2B)=Sof(H2B)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=Sof(C5B)=Sof(H5BA)=Sof(H5BB)=
 Sof(H4BC)=Sof(H4BD)=Sof(H1BC)=Sof(H1BD)=Sof(H4BF)=Sof(H4BG)=Sof(H4BH)=1-FVAR(1)
 Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=
 Sof(H4AA)=Sof(H4AB)=Sof(H1AA)=Sof(H1AB)=Sof(H4AC)=Sof(H4AD)=Sof(H4AE)=FVAR(1)
6.a Riding coordinates:
 O11(H11A,H11B)
6.b Ternary CH refined with riding coordinates:
 C2A(H2A), C2B(H2B)
6.c Secondary CH2 refined with riding coordinates:
 C3A(H3AA,H3AB), C5A(H5AA,H5AB), C3B(H3BA,H3BB), C5B(H5BA,H5BB), C4(H4AA,H4AB),
  C4(H4BC,H4BD), N1(H1AA,H1AB), N1(H1BC,H1BD)
6.d Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15)
6.e Idealised Me refined as rotating group:
 N4(H4AC,H4AD,H4AE), N4(H4BF,H4BG,H4BH)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
C1 C 0.8683(8) 0.3782(5) 0.6127(5) 0.0601(15) Uani 1 1 d . . . . .
C2A C 0.848(2) 0.3981(14) 0.7319(13) 0.038(4) Uani 0.401(16) 1 d . . P A 1
H2A H 0.754259 0.361963 0.787484 0.045 Uiso 0.401(16) 1 calc R . P A 1
C3A C 0.999(2) 0.3489(17) 0.7771(15) 0.053(4) Uani 0.401(16) 1 d . . P A 1
H3AA H 1.037984 0.269284 0.765474 0.064 Uiso 0.401(16) 1 calc R . P A 1
H3AB H 1.080199 0.406327 0.736830 0.064 Uiso 0.401(16) 1 calc R . P A 1
C5A C 1.062(2) 0.291(3) 0.957(2) 0.104(9) Uani 0.401(16) 1 d . . P A 1
H5AA H 1.133243 0.353662 0.939843 0.124 Uiso 0.401(16) 1 calc R . P A 1
H5AB H 1.120965 0.222534 0.931257 0.124 Uiso 0.401(16) 1 calc R . P A 1
C2B C 0.919(2) 0.4149(11) 0.6969(13) 0.059(3) Uani 0.599(16) 1 d . . P A 2
H2B H 1.030395 0.429178 0.664346 0.070 Uiso 0.599(16) 1 calc R . P A 2
C3B C 0.910(2) 0.3118(12) 0.8048(13) 0.082(4) Uani 0.599(16) 1 d . . P A 2
H3BA H 0.977883 0.242548 0.787199 0.099 Uiso 0.599(16) 1 calc R . P A 2
H3BB H 0.803747 0.285897 0.832450 0.099 Uiso 0.599(16) 1 calc R . P A 2
C5B C 0.9538(17) 0.2172(10) 0.9932(10) 0.071(4) Uani 0.599(16) 1 d . . P A 2
H5BA H 1.035111 0.159612 0.966483 0.085 Uiso 0.599(16) 1 calc R . P A 2
H5BB H 0.853592 0.181814 1.014640 0.085 Uiso 0.599(16) 1 calc R . P A 2
C4 C 0.9538(11) 0.3359(7) 0.9037(6) 0.088(2) Uani 1 1 d . . . . .
H4AA H 0.917690 0.417181 0.912287 0.106 Uiso 0.401(16) 1 calc R . P A 1
H4AB H 0.866115 0.284009 0.940363 0.106 Uiso 0.401(16) 1 calc R . P A 1
H4BC H 1.056573 0.368301 0.877655 0.106 Uiso 0.599(16) 1 calc R . P A 2
H4BD H 0.877993 0.395701 0.931870 0.106 Uiso 0.599(16) 1 calc R . P A 2
C6 C 0.6039(7) 0.6513(6) 0.3825(5) 0.0560(14) Uani 1 1 d . . . . .
H6 H 0.602284 0.565674 0.404198 0.067 Uiso 1 1 calc R . . . .
C7 C 0.5497(8) 0.7227(7) 0.2885(5) 0.0667(17) Uani 1 1 d . . . . .
H7 H 0.511608 0.684657 0.249083 0.080 Uiso 1 1 calc R . . . .
C8 C 0.5523(8) 0.8478(7) 0.2542(5) 0.0691(18) Uani 1 1 d . . . . .
H8 H 0.517136 0.895660 0.190952 0.083 Uiso 1 1 calc R . . . .
C9 C 0.6090(7) 0.9049(5) 0.3157(4) 0.0562(14) Uani 1 1 d . . . . .
C10 C 0.6141(9) 1.0359(6) 0.2896(6) 0.0723(19) Uani 1 1 d . . . . .
H10 H 0.583205 1.088873 0.226173 0.087 Uiso 1 1 calc R . . . .
C11 C 0.6629(9) 1.0839(6) 0.3553(5) 0.0699(18) Uani 1 1 d . . . . .
H11 H 0.663299 1.169336 0.337220 0.084 Uiso 1 1 calc R . . . .
C12 C 0.7137(7) 1.0057(5) 0.4516(5) 0.0570(14) Uani 1 1 d . . . . .
C13 C 0.7661(8) 1.0486(6) 0.5257(6) 0.0672(17) Uani 1 1 d . . . . .
H13 H 0.772666 1.132854 0.511203 0.081 Uiso 1 1 calc R . . . .
C14 C 0.8061(9) 0.9659(6) 0.6170(6) 0.0693(18) Uani 1 1 d . . . . .
H14 H 0.838711 0.993206 0.666439 0.083 Uiso 1 1 calc R . . . .
C15 C 0.7989(8) 0.8400(6) 0.6378(5) 0.0609(15) Uani 1 1 d . . . . .
H15 H 0.827050 0.784911 0.701470 0.073 Uiso 1 1 calc R . . . .
C16 C 0.7113(7) 0.8781(5) 0.4785(4) 0.0479(12) Uani 1 1 d . . . . .
C17 C 0.6574(6) 0.8267(5) 0.4103(4) 0.0454(12) Uani 1 1 d . . . . .
Cu1 Cu 0.74059(9) 0.61862(6) 0.57923(5) 0.0513(2) Uani 1 1 d . . . . .
N1 N 0.8401(7) 0.5350(4) 0.7076(4) 0.0611(13) Uani 1 1 d . . . . .
H1AA H 0.936104 0.559954 0.689767 0.073 Uiso 0.401(16) 1 calc R . P A 1
H1AB H 0.784181 0.555281 0.768827 0.073 Uiso 0.401(16) 1 calc R . P A 1
H1BC H 0.909596 0.582801 0.707028 0.073 Uiso 0.599(16) 1 calc R . P A 2
H1BD H 0.767298 0.522904 0.772952 0.073 Uiso 0.599(16) 1 calc R . P A 2
N2 N 0.7538(6) 0.7955(4) 0.5709(3) 0.0484(10) Uani 1 1 d . . . . .
N3 N 0.6579(5) 0.7016(4) 0.4423(3) 0.0472(10) Uani 1 1 d . . . . .
N4 N 0.9837(8) 0.2406(8) 1.0957(6) 0.106(3) Uani 1 1 d . . . . .
H4AC H 0.983474 0.158414 1.118418 0.159 Uiso 0.401(16) 1 calc GR . P A 1
H4AD H 0.885823 0.273319 1.111651 0.159 Uiso 0.401(16) 1 calc GR . P A 1
H4AE H 1.040045 0.263182 1.131443 0.159 Uiso 0.401(16) 1 calc GR . P A 1
H4BF H 0.926305 0.307866 1.107561 0.159 Uiso 0.599(16) 1 calc GR . P A 2
H4BG H 1.084731 0.251664 1.082016 0.159 Uiso 0.599(16) 1 calc GR . P A 2
H4BH H 0.957324 0.175641 1.156826 0.159 Uiso 0.599(16) 1 calc GR . P A 2
O1 O 0.7940(5) 0.4611(4) 0.5480(3) 0.0616(11) Uani 1 1 d . . . . .
O2 O 0.9215(7) 0.2773(4) 0.5975(5) 0.0928(17) Uani 1 1 d . . . . .
O3 O 0.4909(5) 0.5939(4) 0.6907(3) 0.0643(11) Uani 1 1 d . . . . .
O4 O 0.2257(6) 0.5641(5) 0.8458(5) 0.0931(17) Uani 1 1 d . . . . .
O5 O 0.4456(9) 0.6774(4) 0.8796(4) 0.106(2) Uani 1 1 d . U . . .
O6 O 0.7427(7) 0.6625(6) 0.9039(5) 0.111(2) Uani 1 1 d . . . . .
O7 O 0.5296(8) 0.8315(4) 0.9715(5) 0.1004(19) Uani 1 1 d . . . . .
O8 O 0.5061(5) 0.5849(3) 1.1022(3) 0.0519(9) Uani 1 1 d . . . . .
O9 O 0.1311(8) 0.6607(5) 0.6388(5) 0.104(2) Uani 1 1 d D . . . .
H9A H 0.139(12) 0.638(10) 0.582(6) 0.156 Uiso 1 1 d DR . . . .
H9B H 0.213(8) 0.631(10) 0.661(8) 0.156 Uiso 1 1 d DR . . . .
O10 O 0.7198(9) 1.0129(7) 0.9525(7) 0.122(2) Uani 1 1 d D . . . .
H10A H 0.666(13) 0.951(8) 0.973(9) 0.182 Uiso 1 1 d DR . . . .
H10B H 0.774(14) 1.016(12) 0.887(5) 0.182 Uiso 1 1 d DR . . . .
O11 O 0.9805(9) 1.0249(7) 0.7899(7) 0.144(3) Uani 1 1 d . . . . .
H11A H 0.947320 1.088791 0.743860 0.216 Uiso 1 1 d R . . . .
H11B H 1.057610 1.028491 0.814440 0.216 Uiso 1 1 d R . . . .
V1 V 0.41359(10) 0.56302(7) 0.82614(7) 0.0395(2) Uani 1 1 d . . . . .
V2 V 0.55925(12) 0.69418(8) 0.96389(7) 0.0460(2) 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
C1 C2A 1.592(17) . ?
C1 C2B 1.492(15) . ?
C1 O1 1.280(7) . ?
C1 O2 1.237(7) . ?
C2A H2A 0.9800 . ?
C2A C3A 1.57(3) . ?
C2A N1 1.491(16) . ?
C3A H3AA 0.9700 . ?
C3A H3AB 0.9700 . ?
C3A C4 1.533(19) . ?
C5A H5AA 0.9700 . ?
C5A H5AB 0.9700 . ?
C5A C4 1.29(2) . ?
C5A N4 1.67(2) . ?
C2B H2B 0.9800 . ?
C2B C3B 1.49(2) . ?
C2B N1 1.477(13) . ?
C3B H3BA 0.9700 . ?
C3B H3BB 0.9700 . ?
C3B C4 1.561(17) . ?
C5B H5BA 0.9700 . ?
C5B H5BB 0.9700 . ?
C5B C4 1.466(13) . ?
C5B N4 1.541(12) . ?
C4 H4AA 0.9700 . ?
C4 H4AB 0.9700 . ?
C4 H4BC 0.9700 . ?
C4 H4BD 0.9700 . ?
C6 H6 0.9300 . ?
C6 C7 1.392(8) . ?
C6 N3 1.331(7) . ?
C7 H7 0.9300 . ?
C7 C8 1.357(9) . ?
C8 H8 0.9300 . ?
C8 C9 1.418(9) . ?
C9 C10 1.434(9) . ?
C9 C17 1.394(7) . ?
C10 H10 0.9300 . ?
C10 C11 1.351(10) . ?
C11 H11 0.9300 . ?
C11 C12 1.420(9) . ?
C12 C13 1.428(9) . ?
C12 C16 1.391(7) . ?
C13 H13 0.9300 . ?
C13 C14 1.347(9) . ?
C14 H14 0.9300 . ?
C14 C15 1.388(9) . ?
C15 H15 0.9300 . ?
C15 N2 1.319(7) . ?
C16 C17 1.430(8) . ?
C16 N2 1.367(6) . ?
C17 N3 1.356(6) . ?
Cu1 N1 1.998(5) . ?
Cu1 N2 2.019(4) . ?
Cu1 N3 2.002(4) . ?
Cu1 O1 1.941(4) . ?
Cu1 O3 2.283(4) . ?
N1 H1AA 0.8900 . ?
N1 H1AB 0.8900 . ?
N1 H1BC 0.8900 . ?
N1 H1BD 0.8900 . ?
N4 H4AC 0.8900 . ?
N4 H4AD 0.8900 . ?
N4 H4AE 0.8900 . ?
N4 H4BF 0.8900 . ?
N4 H4BG 0.8900 . ?
N4 H4BH 0.8900 . ?
O3 V1 1.626(4) . ?
O4 V1 1.623(5) . ?
O5 V1 1.770(4) . ?
O5 V2 1.762(5) . ?
O6 V2 1.639(6) . ?
O7 V2 1.590(4) . ?
O8 V1 1.791(4) 2_667 ?
O8 V2 1.791(4) . ?
O9 H9A 0.84(2) . ?
O9 H9B 0.84(2) . ?
O10 H10A 0.85(2) . ?
O10 H10B 0.84(2) . ?
O11 H11A 0.8500 . ?
O11 H11B 0.8500 . ?

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
O1 C1 C2A 114.2(7) . . ?
O1 C1 C2B 117.4(6) . . ?
O2 C1 C2A 120.3(8) . . ?
O2 C1 C2B 118.0(7) . . ?
O2 C1 O1 123.6(6) . . ?
C1 C2A H2A 111.7 . . ?
C3A C2A C1 111.7(12) . . ?
C3A C2A H2A 111.7 . . ?
N1 C2A C1 104.9(9) . . ?
N1 C2A H2A 111.7 . . ?
N1 C2A C3A 104.8(14) . . ?
C2A C3A H3AA 110.1 . . ?
C2A C3A H3AB 110.1 . . ?
H3AA C3A H3AB 108.4 . . ?
C4 C3A C2A 107.9(14) . . ?
C4 C3A H3AA 110.1 . . ?
C4 C3A H3AB 110.1 . . ?
H5AA C5A H5AB 108.1 . . ?
C4 C5A H5AA 109.5 . . ?
C4 C5A H5AB 109.5 . . ?
C4 C5A N4 110.5(16) . . ?
N4 C5A H5AA 109.5 . . ?
N4 C5A H5AB 109.5 . . ?
C1 C2B H2B 105.8 . . ?
C3B C2B C1 111.7(12) . . ?
C3B C2B H2B 105.8 . . ?
N1 C2B C1 110.9(9) . . ?
N1 C2B H2B 105.8 . . ?
N1 C2B C3B 116.0(13) . . ?
C2B C3B H3BA 107.7 . . ?
C2B C3B H3BB 107.7 . . ?
C2B C3B C4 118.4(13) . . ?
H3BA C3B H3BB 107.1 . . ?
C4 C3B H3BA 107.7 . . ?
C4 C3B H3BB 107.7 . . ?
H5BA C5B H5BB 108.4 . . ?
C4 C5B H5BA 110.1 . . ?
C4 C5B H5BB 110.1 . . ?
C4 C5B N4 108.2(8) . . ?
N4 C5B H5BA 110.1 . . ?
N4 C5B H5BB 110.1 . . ?
C3A C4 H4AA 108.1 . . ?
C3A C4 H4AB 108.1 . . ?
C5A C4 C3A 116.7(15) . . ?
C5A C4 H4AA 108.1 . . ?
C5A C4 H4AB 108.1 . . ?
C3B C4 H4BC 110.3 . . ?
C3B C4 H4BD 110.3 . . ?
C5B C4 C3B 107.2(9) . . ?
C5B C4 H4BC 110.3 . . ?
C5B C4 H4BD 110.3 . . ?
H4AA C4 H4AB 107.3 . . ?
H4BC C4 H4BD 108.5 . . ?
C7 C6 H6 118.9 . . ?
N3 C6 H6 118.9 . . ?
N3 C6 C7 122.1(6) . . ?
C6 C7 H7 119.9 . . ?
C8 C7 C6 120.1(6) . . ?
C8 C7 H7 119.9 . . ?
C7 C8 H8 120.3 . . ?
C7 C8 C9 119.4(6) . . ?
C9 C8 H8 120.3 . . ?
C8 C9 C10 124.6(6) . . ?
C17 C9 C8 116.7(5) . . ?
C17 C9 C10 118.6(6) . . ?
C9 C10 H10 119.4 . . ?
C11 C10 C9 121.3(6) . . ?
C11 C10 H10 119.4 . . ?
C10 C11 H11 119.6 . . ?
C10 C11 C12 120.9(6) . . ?
C12 C11 H11 119.6 . . ?
C11 C12 C13 124.5(6) . . ?
C16 C12 C11 119.1(6) . . ?
C16 C12 C13 116.3(5) . . ?
C12 C13 H13 120.3 . . ?
C14 C13 C12 119.3(6) . . ?
C14 C13 H13 120.3 . . ?
C13 C14 H14 119.8 . . ?
C13 C14 C15 120.4(6) . . ?
C15 C14 H14 119.8 . . ?
C14 C15 H15 118.7 . . ?
N2 C15 C14 122.7(6) . . ?
N2 C15 H15 118.7 . . ?
C12 C16 C17 120.3(5) . . ?
N2 C16 C12 123.5(5) . . ?
N2 C16 C17 116.2(5) . . ?
C9 C17 C16 119.8(5) . . ?
N3 C17 C9 123.4(5) . . ?
N3 C17 C16 116.8(4) . . ?
N1 Cu1 N2 98.04(19) . . ?
N1 Cu1 N3 175.4(2) . . ?
N1 Cu1 O3 94.2(2) . . ?
N2 Cu1 O3 97.63(17) . . ?
N3 Cu1 N2 82.29(18) . . ?
N3 Cu1 O3 90.32(16) . . ?
O1 Cu1 N1 83.91(18) . . ?
O1 Cu1 N2 160.51(19) . . ?
O1 Cu1 N3 94.27(17) . . ?
O1 Cu1 O3 101.58(17) . . ?
C2A N1 Cu1 109.8(7) . . ?
C2A N1 H1AA 109.7 . . ?
C2A N1 H1AB 109.7 . . ?
C2B N1 Cu1 109.8(6) . . ?
C2B N1 H1BC 109.7 . . ?
C2B N1 H1BD 109.7 . . ?
Cu1 N1 H1AA 109.7 . . ?
Cu1 N1 H1AB 109.7 . . ?
Cu1 N1 H1BC 109.7 . . ?
Cu1 N1 H1BD 109.7 . . ?
H1AA N1 H1AB 108.2 . . ?
H1BC N1 H1BD 108.2 . . ?
C15 N2 C16 117.7(5) . . ?
C15 N2 Cu1 130.3(4) . . ?
C16 N2 Cu1 111.9(4) . . ?
C6 N3 C17 118.1(5) . . ?
C6 N3 Cu1 129.2(4) . . ?
C17 N3 Cu1 112.6(4) . . ?
C5A N4 H4AC 109.5 . . ?
C5A N4 H4AD 109.5 . . ?
C5A N4 H4AE 109.5 . . ?
C5B N4 H4BF 109.5 . . ?
C5B N4 H4BG 109.5 . . ?
C5B N4 H4BH 109.5 . . ?
H4AC N4 H4AD 109.5 . . ?
H4AC N4 H4AE 109.5 . . ?
H4AD N4 H4AE 109.5 . . ?
H4BF N4 H4BG 109.5 . . ?
H4BF N4 H4BH 109.5 . . ?
H4BG N4 H4BH 109.5 . . ?
C1 O1 Cu1 116.3(4) . . ?
V1 O3 Cu1 134.0(3) . . ?
V2 O5 V1 138.6(3) . . ?
V2 O8 V1 135.2(2) . 2_667 ?
H9A O9 H9B 106(5) . . ?
H10A O10 H10B 105(5) . . ?
H11A O11 H11B 120.0 . . ?
O3 V1 O5 112.2(3) . . ?
O3 V1 O8 109.13(19) . 2_667 ?
O4 V1 O3 107.0(3) . . ?
O4 V1 O5 107.0(3) . . ?
O4 V1 O8 111.6(2) . 2_667 ?
O5 V1 O8 109.9(2) . 2_667 ?
O5 V2 O8 109.4(2) . . ?
O6 V2 O5 107.0(3) . . ?
O6 V2 O8 108.9(2) . . ?
O7 V2 O5 109.1(3) . . ?
O7 V2 O6 111.9(4) . . ?
O7 V2 O8 110.4(2) . . ?

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
N1 H1AA O9 0.89 2.07 2.940(9) 165.9 1_655
N1 H1AB O6 0.89 2.38 3.192(8) 152.6 .
N4 H4AC O11 0.89 2.07 2.923(12) 160.3 2_767
N4 H4BF O4 0.89 1.96 2.845(9) 170.0 2_667
N4 H4BG O6 0.89 2.04 2.845(11) 150.4 2_767
O9 H9A O1 0.84(2) 2.23(3) 3.050(7) 165(9) 2_666
O9 H9A O2 0.84(2) 2.39(7) 3.062(8) 137(9) 2_666
O9 H9B O3 0.84(2) 2.57(4) 3.391(8) 165(11) .
O9 H9B O4 0.84(2) 2.29(8) 2.857(8) 125(9) .
O10 H10A O7 0.85(2) 1.98(5) 2.799(8) 161(12) .
O10 H10B O11 0.84(2) 1.90(8) 2.638(10) 145(13) .
O11 H11A O2 0.85 2.39 3.216(10) 165.8 1_565

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
C1 C2A C3A C4 -163.5(10) . . . . ?
C1 C2A N1 Cu1 31.4(11) . . . . ?
C1 C2B C3B C4 -178.1(11) . . . . ?
C1 C2B N1 Cu1 -14.1(13) . . . . ?
C2A C1 O1 Cu1 21.9(9) . . . . ?
C2A C3A C4 C5A 176.8(17) . . . . ?
C3A C2A N1 Cu1 149.2(10) . . . . ?
C2B C1 O1 Cu1 -5.7(11) . . . . ?
C2B C3B C4 C5B -173.3(15) . . . . ?
C3B C2B N1 Cu1 -142.8(13) . . . . ?
C6 C7 C8 C9 -0.7(10) . . . . ?
C7 C6 N3 C17 0.8(8) . . . . ?
C7 C6 N3 Cu1 179.9(4) . . . . ?
C7 C8 C9 C10 -178.4(6) . . . . ?
C7 C8 C9 C17 -0.9(9) . . . . ?
C8 C9 C10 C11 176.8(7) . . . . ?
C8 C9 C17 C16 -178.0(5) . . . . ?
C8 C9 C17 N3 2.5(8) . . . . ?
C9 C10 C11 C12 1.2(11) . . . . ?
C9 C17 N3 C6 -2.5(8) . . . . ?
C9 C17 N3 Cu1 178.3(4) . . . . ?
C10 C9 C17 C16 -0.3(8) . . . . ?
C10 C9 C17 N3 -179.8(5) . . . . ?
C10 C11 C12 C13 -179.6(7) . . . . ?
C10 C11 C12 C16 -0.6(10) . . . . ?
C11 C12 C13 C14 177.6(7) . . . . ?
C11 C12 C16 C17 -0.4(9) . . . . ?
C11 C12 C16 N2 -178.2(6) . . . . ?
C12 C13 C14 C15 1.1(11) . . . . ?
C12 C16 C17 C9 0.8(8) . . . . ?
C12 C16 C17 N3 -179.7(5) . . . . ?
C12 C16 N2 C15 0.2(8) . . . . ?
C12 C16 N2 Cu1 -178.4(5) . . . . ?
C13 C12 C16 C17 178.7(5) . . . . ?
C13 C12 C16 N2 0.9(9) . . . . ?
C13 C14 C15 N2 0.1(11) . . . . ?
C14 C15 N2 C16 -0.7(9) . . . . ?
C14 C15 N2 Cu1 177.6(5) . . . . ?
C16 C12 C13 C14 -1.5(10) . . . . ?
C16 C17 N3 C6 178.0(5) . . . . ?
C16 C17 N3 Cu1 -1.2(6) . . . . ?
C17 C9 C10 C11 -0.7(10) . . . . ?
C17 C16 N2 C15 -177.7(5) . . . . ?
C17 C16 N2 Cu1 3.7(6) . . . . ?
Cu1 O3 V1 O4 178.0(3) . . . . ?
Cu1 O3 V1 O5 61.0(4) . . . . ?
Cu1 O3 V1 O8 -61.1(4) . . . 2_667 ?
N1 C2A C3A C4 83.5(16) . . . . ?
N1 C2B C3B C4 -50(2) . . . . ?
N2 C16 C17 C9 178.8(5) . . . . ?
N2 C16 C17 N3 -1.7(7) . . . . ?
N3 C6 C7 C8 0.7(10) . . . . ?
N4 C5A C4 C3A -161.7(13) . . . . ?
N4 C5B C4 C3B -175.5(10) . . . . ?
O1 C1 C2A C3A -148.3(12) . . . . ?
O1 C1 C2A N1 -35.3(13) . . . . ?
O1 C1 C2B C3B 144.5(12) . . . . ?
O1 C1 C2B N1 13.4(15) . . . . ?
O2 C1 C2A C3A 46.8(17) . . . . ?
O2 C1 C2A N1 159.8(8) . . . . ?
O2 C1 C2B C3B -46.7(18) . . . . ?
O2 C1 C2B N1 -177.8(8) . . . . ?
O2 C1 O1 Cu1 -173.8(6) . . . . ?
V1 O5 V2 O6 56.2(6) . . . . ?
V1 O5 V2 O7 177.5(6) . . . . ?
V1 O5 V2 O8 -61.6(7) . . . . ?
V1 O8 V2 O5 99.8(4) 2_667 . . . ?
V1 O8 V2 O6 -16.8(5) 2_667 . . . ?
V1 O8 V2 O7 -140.1(4) 2_667 . . . ?
V2 O5 V1 O3 -107.8(6) . . . . ?
V2 O5 V1 O4 135.2(6) . . . . ?
V2 O5 V1 O8 13.8(7) . . . 2_667 ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
####################################################################### 
# 
# 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_ov_aml-403_mo
_database_code_depnum_ccdc_archive 'CCDC 2044083'
loop_
_audit_author_name
_audit_author_address
'Eduardo Sanchez'
;Benemerita Universidad Autonoma de Puebla
Mexico
;
_audit_update_record             
;
2020-11-12 deposited with the CCDC.	2021-02-09 downloaded from the CCDC.
;
_audit_creation_date             2019-06-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C16 H22 Cu N4 O8 V2), 7(H2 O)'
_chemical_formula_sum            'C32 H58 Cu2 N8 O23 V4'
_chemical_formula_weight         1253.70
_chemical_melting_point          ?
_chemical_oxdiff_formula         C32H58Cu2N8O23V4
_chemical_oxdiff_usercomment     .
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'
V V 0.3005 0.5294 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_symmetry_space_group_name_H-M_alt 'P -1'
_cell_length_a                   11.9013(3)
_cell_length_b                   12.1828(2)
_cell_length_c                   18.2260(3)
_cell_angle_alpha                98.0718(16)
_cell_angle_beta                 108.6313(19)
_cell_angle_gamma                92.8695(18)
_cell_volume                     2466.59(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    26797
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.5380
_cell_measurement_theta_min      3.1940
_cell_oxdiff_angle_alpha         98.0718(16)
_cell_oxdiff_angle_beta          108.6313(19)
_cell_oxdiff_angle_gamma         92.8695(18)
_cell_oxdiff_length_a            11.9013(3)
_cell_oxdiff_length_b            12.1828(2)
_cell_oxdiff_length_c            18.2260(3)
_cell_oxdiff_measurement_reflns_used 26797
_cell_oxdiff_volume              2466.59(9)
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.660
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55073
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0982
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            83873
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.883
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5564
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -115.00 -57.00   1.00   10.02    --  -24.73-178.00-150.00   58
  2  ω   -115.00 -57.00   1.00   10.02    --  -24.73-178.00 -30.00   58
  3  ω   -115.00 -57.00   1.00   10.02    --  -24.73-178.00  90.00   58
  4  ω      0.00 103.00   1.00   10.02    --   26.76  38.00  60.00  103
  5  ω     -7.00 105.00   1.00   10.02    --   26.76  77.00  60.00  112
  6  ω     35.00 117.00   1.00   10.02    --   26.76 178.00 -90.00   82
  7  ω    -47.00  56.00   1.00   10.02    --   26.76 -57.00 -90.00  103
  8  ω    -25.00  69.00   1.00   10.02    --   26.76 -99.00 150.00   94
  9  ω     32.00 115.00   1.00   10.02    --   26.76-178.00-120.00   83
 10  ω     -7.00 105.00   1.00   10.02    --   26.76  77.00 -90.00  112
 11  ω   -113.00 -53.00   1.00   10.02    --  -24.73 178.00 150.00   60
 12  ω    -99.00   5.00   1.00   10.02    --  -24.73 -57.00 -90.00  104
 13  ω     -7.00 105.00   1.00   10.02    --   26.76  77.00-120.00  112
 14  ω     -3.00 101.00   1.00   10.02    --   26.76  57.00-180.00  104
 15  ω    -25.00  69.00   1.00   10.02    --   26.76 -99.00   0.00   94
 16  ω    -25.00  69.00   1.00   10.02    --   26.76 -99.00  60.00   94
 17  ω     35.00 117.00   1.00   10.02    --   26.76 178.00 150.00   82
 18  ω    -25.00  69.00   1.00   10.02    --   26.76 -99.00-120.00   94
 19  ω    -19.00 108.00   1.00   10.02    --   26.76  19.00-150.00  127
 20  ω      0.00 103.00   1.00   10.02    --   26.76  38.00  90.00  103
 21  ω      0.00 103.00   1.00   10.02    --   26.76  38.00-150.00  103
 22  ω    -63.00 116.00   1.00   10.02    --   26.76   0.00-150.00  179
 23  ω    -63.00   5.00   1.00   10.02    --   26.76   0.00-120.00   68
 24  ω    -63.00 116.00   1.00   10.02    --   26.76   0.00-180.00  179
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0569803000
_diffrn_orient_matrix_UB_12      -0.0200668000
_diffrn_orient_matrix_UB_13      0.0105846000
_diffrn_orient_matrix_UB_21      -0.0254429000
_diffrn_orient_matrix_UB_22      -0.0523709000
_diffrn_orient_matrix_UB_23      -0.0234826000
_diffrn_orient_matrix_UB_31      0.0101268000
_diffrn_orient_matrix_UB_32      0.0186627000
_diffrn_orient_matrix_UB_33      -0.0327196000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7676
_reflns_number_total             8700
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.07
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.777
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     713
_refine_ls_number_reflns         8700
_refine_ls_number_restraints     109
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0609
_refine_ls_restrained_S_all      1.129
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0415P)²+9.0430P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1440
_refine_ls_wR_factor_ref         0.1488
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H)
  groups, All N(H,H,H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups, All N(H,H,H,H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C30A-C31A \\sim C30B-C31B
 with sigma of 0.02
 C32B-C31B \\sim C32A-C31A
 with sigma of 0.02
 C33-C32A \\sim C32B-C33
 with sigma of 0.02
 C30B-C29 \\sim C29-C30A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N17) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C32B) = Uanis(C32A)
Uanis(C31B) = Uanis(C31A)
Uanis(C30B) = Uanis(C30A)
Uanis(C15A) = Uanis(C15B)
4. Rigid body (RIGU) restrains
 C29, C30B, C31B, C32B, C33, N34
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C11, C12B, C13B, C16A, C14B, C15A, O8B, O7B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C11, C12A, N17, C13A, C14A, C16B, C15B, O7A, O8A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(H3BC)=Sof(H3BD)=Sof(C12B)=Sof(H12B)=Sof(C13B)=Sof(H13A)=Sof(H13B)=
 Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C16B)=Sof(H16C)=Sof(H16D)=Sof(C14B)=
 Sof(H14C)=Sof(H14D)=Sof(C15B)=Sof(H15C)=Sof(H15D)=Sof(O8B)=Sof(O7B)=1-FVAR(1)
 Sof(H3AA)=Sof(H3AB)=Sof(C12A)=Sof(H12A)=Sof(H17A)=Sof(H17B)=Sof(H17C)=
 Sof(C16A)=Sof(H16A)=Sof(H16B)=Sof(C13A)=Sof(H13C)=Sof(H13D)=Sof(C14A)=
 Sof(H14A)=Sof(H14B)=Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(O7A)=Sof(O8A)=FVAR(1)
 Sof(H29A)=Sof(C30B)=Sof(H30A)=Sof(H30B)=Sof(H33C)=Sof(H33D)=Sof(C31B)=
 Sof(H31C)=Sof(H31D)=Sof(C32B)=Sof(H32C)=Sof(H32D)=1-FVAR(2)
 Sof(H29)=Sof(C30A)=Sof(H30C)=Sof(H30D)=Sof(H33A)=Sof(H33B)=Sof(C31A)=
 Sof(H31A)=Sof(H31B)=Sof(C32A)=Sof(H32A)=Sof(H32B)=FVAR(2)
6.a Free rotating group:
 O17(H17G,H17H), O22(H22A,H22B), O23(H23A,H23B), O19(H19A,H19B), O18(H18A,
 H18B), O20(H20A,H20B), O21(H21A,H21B)
6.b Ternary CH refined with riding coordinates:
 C12B(H12B), C12A(H12A), C29(H29A), C29(H29)
6.c Secondary CH2 refined with riding coordinates:
 N3(H3BC,H3BD), N3(H3AA,H3AB), N6(H6A,H6B), C13B(H13A,H13B), C16A(H16A,H16B),
 C13A(H13C,H13D), C14A(H14A,H14B), C16B(H16C,H16D), C14B(H14C,H14D), C15A(H15A,
 H15B), C15B(H15C,H15D), C30B(H30A,H30B), C30A(H30C,H30D), C33(H33A,H33B),
 C33(H33C,H33D), C31A(H31A,H31B), C31B(H31C,H31D), C32A(H32A,H32B), C32B(H32C,
 H32D)
6.d Aromatic/amide H refined with riding coordinates:
 C10(H10), C1(H1), C7(H7), C8(H8), C2(H2), C9(H9), C4(H4), C24(H24), C27(H27),
 C26(H26), C18(H18), C3(H3), C21(H21), C20(H20), C19(H19), C25(H25)
6.e Idealised Me refined as rotating group:
 N17(H17A,H17B,H17C), N17(H17D,H17E,H17F), N34(H34A,H34B,H34C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
Cu1 Cu 0.30851(6) 0.93932(5) 0.69571(3) 0.03638(17) Uani 1 1 d . . . . .
Cu2 Cu 0.19798(6) 0.60758(5) 0.81932(4) 0.03886(17) Uani 1 1 d . . . . .
V2 V 0.55799(8) 0.81534(7) 0.51870(5) 0.0358(2) Uani 1 1 d . . . . .
V3 V -0.04857(7) 0.46475(7) 0.85660(5) 0.0344(2) Uani 1 1 d . . . . .
V4 V 0.05883(8) 0.32622(7) 1.00607(5) 0.0381(2) Uani 1 1 d . . . . .
V1 V 0.54829(8) 1.06151(7) 0.64057(5) 0.0367(2) Uani 1 1 d . . . . .
O9 O 0.0175(3) 0.5055(3) 0.7963(2) 0.0452(9) Uani 1 1 d . . . . .
O15 O 0.1673(4) 0.6795(3) 0.7276(2) 0.0501(10) Uani 1 1 d . . . . .
O1 O 0.4907(3) 1.0483(3) 0.7104(2) 0.0452(9) Uani 1 1 d . . . . .
O3 O 0.6759(4) 1.1370(4) 0.6795(2) 0.0580(11) Uani 1 1 d . . . . .
N1 N 0.2239(4) 1.0658(3) 0.7249(2) 0.0359(9) Uani 1 1 d . . . . .
N2 N 0.2296(4) 0.9731(3) 0.5876(2) 0.0349(9) Uani 1 1 d . . . . .
N4 N 0.2670(4) 0.4840(3) 0.7702(3) 0.0381(10) Uani 1 1 d . . . . .
O12 O 0.0559(4) 0.4024(4) 0.9282(2) 0.0549(10) Uani 1 1 d . . . . .
O10 O -0.0994(4) 0.5829(4) 0.9015(2) 0.0659(12) Uani 1 1 d . . . . .
O2 O 0.4504(4) 1.1320(4) 0.5694(2) 0.0556(10) Uani 1 1 d . . . . .
O5 O 0.4357(4) 0.7333(4) 0.5032(3) 0.0623(12) Uani 1 1 d . . . . .
O11 O -0.1625(4) 0.3745(4) 0.8071(2) 0.0597(11) Uani 1 1 d . . . . .
N5 N 0.2833(4) 0.5463(4) 0.9162(3) 0.0401(10) Uani 1 1 d . . . . .
O4 O 0.5647(4) 0.9261(3) 0.5960(2) 0.0605(11) Uani 1 1 d . . . . .
O14 O 0.1516(4) 0.2328(4) 1.0081(3) 0.0692(13) Uani 1 1 d . . . . .
N3 N 0.3849(4) 0.8029(4) 0.6717(2) 0.0394(10) Uani 1 1 d . . . . .
H3BC H 0.330625 0.744023 0.653390 0.047 Uiso 0.54(2) 1 calc R . P A 2
H3BD H 0.418966 0.811352 0.635654 0.047 Uiso 0.54(2) 1 calc R . P A 2
H3AA H 0.330198 0.753444 0.635883 0.047 Uiso 0.46(2) 1 calc R . P A 1
H3AB H 0.440574 0.820706 0.651227 0.047 Uiso 0.46(2) 1 calc R . P A 1
O16 O 0.0919(4) 0.8248(4) 0.6761(3) 0.0671(12) Uani 1 1 d . . . . .
O17 O 0.3482(5) 0.8888(4) 0.9759(3) 0.0718(13) Uani 1 1 d . . . . .
H17G H 0.397898 0.870547 0.952800 0.108 Uiso 1 1 d G . . . .
H17H H 0.337236 0.955560 0.969076 0.108 Uiso 1 1 d G . . . .
O6 O 0.6729(4) 0.7461(4) 0.5429(3) 0.0645(12) Uani 1 1 d . . . . .
O13 O -0.0749(4) 0.2652(4) 0.9883(3) 0.0692(13) Uani 1 1 d . . . . .
N6 N 0.1368(4) 0.7423(4) 0.8628(3) 0.0492(12) Uani 1 1 d . . . . .
H6A H 0.091164 0.723166 0.890276 0.059 Uiso 1 1 calc R . . . .
H6B H 0.197248 0.790341 0.894548 0.059 Uiso 1 1 calc R . . . .
O22 O 0.2696(5) 0.6048(5) 0.5438(3) 0.0736(13) Uani 1 1 d . . . . .
H22A H 0.317827 0.560591 0.565689 0.110 Uiso 1 1 d G . . . .
H22B H 0.286753 0.612665 0.502879 0.110 Uiso 1 1 d G . . . .
O23 O 0.1581(5) 0.3994(4) 0.4607(4) 0.0769(14) Uani 1 1 d . . . . .
H23A H 0.097821 0.357154 0.458759 0.115 Uiso 1 1 d G . . . .
H23B H 0.209821 0.355211 0.457062 0.115 Uiso 1 1 d G . . . .
C23 C 0.3343(4) 0.4524(4) 0.9023(3) 0.0403(12) Uani 1 1 d . . . . .
C10 C 0.2406(5) 0.9226(5) 0.5205(3) 0.0433(12) Uani 1 1 d . . . . .
H10 H 0.283463 0.860785 0.521224 0.052 Uiso 1 1 calc R . . . .
C22 C 0.3319(4) 0.4224(4) 0.8198(3) 0.0388(11) Uani 1 1 d . . . . .
C5 C 0.1557(4) 1.1094(4) 0.6629(3) 0.0378(11) Uani 1 1 d . . . . .
O19 O 0.6702(5) 0.8892(5) 1.0071(3) 0.0896(17) Uani 1 1 d . . . . .
H19A H 0.619002 0.881136 0.961343 0.134 Uiso 1 1 d G . . . .
H19B H 0.727026 0.853570 1.000964 0.134 Uiso 1 1 d G . . . .
O18 O 0.5532(6) 1.1538(5) 0.8756(3) 0.0920(18) Uani 1 1 d . . . . .
H18A H 0.576211 1.119631 0.914585 0.138 Uiso 1 1 d G . . . .
H18B H 0.514222 1.107635 0.834746 0.138 Uiso 1 1 d G . . . .
C6 C 0.1654(4) 1.0616(4) 0.5866(3) 0.0358(11) Uani 1 1 d . . . . .
O20 O 0.0485(6) 0.6981(5) 0.5284(4) 0.0904(17) Uani 1 1 d . . . . .
H20A H 0.074378 0.634951 0.521698 0.136 Uiso 1 1 d G . . . .
H20B H 0.054037 0.709615 0.576554 0.136 Uiso 1 1 d G . . . .
C1 C 0.2195(5) 1.1030(4) 0.7962(3) 0.0424(12) Uani 1 1 d . . . . .
H1 H 0.265890 1.072724 0.838588 0.051 Uiso 1 1 calc R . . . .
C7 C 0.1138(5) 1.1025(5) 0.5174(3) 0.0498(14) Uani 1 1 d . . . . .
H7 H 0.070710 1.164104 0.517279 0.060 Uiso 1 1 calc R . . . .
C8 C 0.1272(5) 1.0502(5) 0.4483(3) 0.0511(14) Uani 1 1 d . . . . .
H8 H 0.093620 1.076685 0.401418 0.061 Uiso 1 1 calc R . . . .
C2 C 0.1487(5) 1.1846(5) 0.8095(4) 0.0508(14) Uani 1 1 d . . . . .
H2 H 0.147984 1.209621 0.859951 0.061 Uiso 1 1 calc R . . . .
C9 C 0.1899(5) 0.9600(5) 0.4500(3) 0.0497(14) Uani 1 1 d . . . . .
H9 H 0.198835 0.923505 0.404177 0.060 Uiso 1 1 calc R . . . .
C4 C 0.0818(5) 1.1921(5) 0.6722(4) 0.0499(14) Uani 1 1 d . . . . .
H4 H 0.035930 1.221735 0.629303 0.060 Uiso 1 1 calc R . . . .
C24 C 0.3834(5) 0.3893(5) 0.9604(4) 0.0542(15) Uani 1 1 d . . . . .
H24 H 0.416874 0.324360 0.949195 0.065 Uiso 1 1 calc R . . . .
C28 C 0.1116(5) 0.7652(5) 0.7280(4) 0.0509(14) Uani 1 1 d . . . . .
C11 C 0.4305(5) 0.8294(5) 0.8141(3) 0.0483(13) Uani 1 1 d . U . . .
C27 C 0.2822(5) 0.5806(6) 0.9886(3) 0.0514(14) Uani 1 1 d . . . . .
H27 H 0.247577 0.645401 0.998445 0.062 Uiso 1 1 calc R . . . .
O21 O 0.0650(7) 0.5623(6) 0.3647(4) 0.0991(19) Uani 1 1 d . . . . .
H21A H 0.030310 0.542160 0.315656 0.149 Uiso 1 1 d G . . . .
H21B H 0.096940 0.505201 0.380236 0.149 Uiso 1 1 d G . . . .
C26 C 0.3312(5) 0.5225(6) 1.0500(4) 0.0577(16) Uani 1 1 d . . . . .
H26 H 0.330253 0.548673 1.100217 0.069 Uiso 1 1 calc R . . . .
C18 C 0.2563(5) 0.4619(5) 0.6939(3) 0.0469(13) Uani 1 1 d . . . . .
H18 H 0.211393 0.505765 0.659931 0.056 Uiso 1 1 calc R . . . .
C3 C 0.0786(6) 1.2285(5) 0.7461(4) 0.0586(16) Uani 1 1 d . . . . .
H3 H 0.029351 1.282712 0.753717 0.070 Uiso 1 1 calc R . . . .
C21 C 0.3891(5) 0.3357(5) 0.7932(4) 0.0515(14) Uani 1 1 d . . . . .
H21 H 0.434860 0.293609 0.828267 0.062 Uiso 1 1 calc R . . . .
C20 C 0.3776(6) 0.3131(5) 0.7154(4) 0.0603(17) Uani 1 1 d . . . . .
H20 H 0.415380 0.255501 0.697274 0.072 Uiso 1 1 calc R . . . .
C19 C 0.3098(6) 0.3759(5) 0.6638(4) 0.0576(16) Uani 1 1 d . . . . .
H19 H 0.300055 0.361169 0.610558 0.069 Uiso 1 1 calc R . . . .
C25 C 0.3812(5) 0.4253(6) 1.0353(4) 0.0631(18) Uani 1 1 d . . . . .
H25 H 0.413007 0.384558 1.075264 0.076 Uiso 1 1 calc R . . . .
C12B C 0.4750(14) 0.7872(14) 0.7453(8) 0.041(3) Uani 0.54(2) 1 d . U P A 2
H12B H 0.544181 0.839281 0.751609 0.050 Uiso 0.54(2) 1 calc R . P A 2
C13B C 0.5210(16) 0.6766(13) 0.7503(7) 0.055(4) Uani 0.54(2) 1 d . U P A 2
H13A H 0.587235 0.683710 0.799001 0.066 Uiso 0.54(2) 1 calc R . P A 2
H13B H 0.458790 0.625671 0.754439 0.066 Uiso 0.54(2) 1 calc R . P A 2
C12A C 0.4406(18) 0.7506(14) 0.7427(10) 0.039(3) Uani 0.46(2) 1 d . U P A 1
H12A H 0.397584 0.677661 0.737351 0.046 Uiso 0.46(2) 1 calc R . P A 1
N17 N 0.7150(6) 0.3741(5) 0.6492(3) 0.0761(17) Uani 1 1 d . U . . .
H17A H 0.722996 0.344006 0.692109 0.114 Uiso 0.46(2) 1 calc GR . P A 1
H17B H 0.783994 0.410553 0.653367 0.114 Uiso 0.46(2) 1 calc GR . P A 1
H17C H 0.693553 0.320508 0.607327 0.114 Uiso 0.46(2) 1 calc GR . P A 1
H17D H 0.768885 0.361356 0.625421 0.114 Uiso 0.54(2) 1 calc GR . P A 2
H17E H 0.649294 0.327822 0.624206 0.114 Uiso 0.54(2) 1 calc GR . P A 2
H17F H 0.744283 0.363032 0.698691 0.114 Uiso 0.54(2) 1 calc GR . P A 2
C16A C 0.6229(18) 0.4521(19) 0.6404(12) 0.074(5) Uani 0.46(2) 1 d . U P A 1
H16A H 0.552041 0.414487 0.644712 0.089 Uiso 0.46(2) 1 calc R . P A 1
H16B H 0.602196 0.471261 0.588161 0.089 Uiso 0.46(2) 1 calc R . P A 1
C13A C 0.5696(15) 0.737(2) 0.7519(9) 0.064(5) Uani 0.46(2) 1 d . U P A 1
H13C H 0.606277 0.810852 0.753045 0.076 Uiso 0.46(2) 1 calc R . P A 1
H13D H 0.605389 0.718570 0.803720 0.076 Uiso 0.46(2) 1 calc R . P A 1
C14A C 0.608(2) 0.662(3) 0.6990(17) 0.100(10) Uani 0.46(2) 1 d . U P A 1
H14A H 0.538202 0.645579 0.652375 0.120 Uiso 0.46(2) 1 calc R . P A 1
H14B H 0.663739 0.709017 0.685340 0.120 Uiso 0.46(2) 1 calc R . P A 1
C16B C 0.686(2) 0.4900(15) 0.6478(11) 0.081(5) Uani 0.54(2) 1 d . U P A 2
H16C H 0.638182 0.497618 0.594944 0.097 Uiso 0.54(2) 1 calc R . P A 2
H16D H 0.758898 0.539221 0.662654 0.097 Uiso 0.54(2) 1 calc R . P A 2
C14B C 0.5609(15) 0.6244(14) 0.6873(11) 0.052(4) Uani 0.54(2) 1 d . U P A 2
H14C H 0.615741 0.678023 0.678032 0.063 Uiso 0.54(2) 1 calc R . P A 2
H14D H 0.492537 0.606215 0.639735 0.063 Uiso 0.54(2) 1 calc R . P A 2
C15A C 0.659(3) 0.560(2) 0.7003(15) 0.071(4) Uani 0.46(2) 1 d . U P A 1
H15A H 0.658226 0.537545 0.749259 0.086 Uiso 0.46(2) 1 calc R . P A 1
H15B H 0.741891 0.579425 0.707048 0.086 Uiso 0.46(2) 1 calc R . P A 1
C15B C 0.619(2) 0.5235(18) 0.7021(13) 0.071(4) Uani 0.54(2) 1 d . U P A 2
H15C H 0.559805 0.463148 0.697217 0.086 Uiso 0.54(2) 1 calc R . P A 2
H15D H 0.674208 0.535605 0.755639 0.086 Uiso 0.54(2) 1 calc R . P A 2
O8B O 0.471(3) 0.784(3) 0.8776(15) 0.074(6) Uani 0.54(2) 1 d . U P A 2
O7B O 0.381(2) 0.913(3) 0.8089(14) 0.043(4) Uani 0.54(2) 1 d . U P A 2
O7A O 0.353(3) 0.905(3) 0.7958(18) 0.042(5) Uani 0.46(2) 1 d . U P A 1
O8A O 0.464(4) 0.808(3) 0.8775(18) 0.069(6) Uani 0.46(2) 1 d . U P A 1
C29 C 0.0669(6) 0.7933(6) 0.7966(4) 0.0688(18) Uani 1 1 d D U . . .
H29A H 0.090989 0.873274 0.814119 0.083 Uiso 0.524(8) 1 calc R . P B 2
H29 H -0.007543 0.743898 0.778400 0.083 Uiso 0.476(8) 1 calc R . P B 1
C30B C -0.0598(11) 0.7851(11) 0.7724(9) 0.073(2) Uani 0.524(8) 1 d D U P B 2
H30A H -0.089182 0.707034 0.763699 0.087 Uiso 0.524(8) 1 calc R . P B 2
H30B H -0.088768 0.811040 0.722352 0.087 Uiso 0.524(8) 1 calc R . P B 2
C30A C 0.0247(13) 0.8963(11) 0.8144(10) 0.073(2) Uani 0.476(8) 1 d D . P B 1
H30C H 0.002905 0.929043 0.766881 0.087 Uiso 0.476(8) 1 calc R . P B 1
H30D H 0.091835 0.944098 0.852245 0.087 Uiso 0.476(8) 1 calc R . P B 1
C33 C -0.2089(10) 1.0339(8) 0.8539(6) 0.103(3) Uani 1 1 d D U . . .
H33A H -0.199513 1.020124 0.906549 0.124 Uiso 0.476(8) 1 calc R . P B 1
H33B H -0.270250 0.980349 0.815872 0.124 Uiso 0.476(8) 1 calc R . P B 1
H33C H -0.172978 1.032936 0.909604 0.124 Uiso 0.524(8) 1 calc R . P B 2
H33D H -0.285685 0.990023 0.836946 0.124 Uiso 0.524(8) 1 calc R . P B 2
N34 N -0.2322(6) 1.1513(5) 0.8447(4) 0.0792(17) Uani 1 1 d . U . . .
H34A H -0.174614 1.197677 0.880840 0.119 Uiso 1 1 calc GR . . . .
H34B H -0.302039 1.163971 0.850676 0.119 Uiso 1 1 calc GR . . . .
H34C H -0.233983 1.162111 0.797072 0.119 Uiso 1 1 calc GR . . . .
C31A C -0.0779(17) 0.9043(15) 0.8459(15) 0.089(4) Uani 0.476(8) 1 d D . P B 1
H31A H -0.055086 0.891677 0.899828 0.107 Uiso 0.476(8) 1 calc R . P B 1
H31B H -0.145978 0.852275 0.813899 0.107 Uiso 0.476(8) 1 calc R . P B 1
C31B C -0.1143(16) 0.8501(13) 0.8293(13) 0.089(4) Uani 0.524(8) 1 d D U P B 2
H31C H -0.061805 0.852065 0.882684 0.107 Uiso 0.524(8) 1 calc R . P B 2
H31D H -0.189943 0.810469 0.824054 0.107 Uiso 0.524(8) 1 calc R . P B 2
C32A C -0.1051(15) 1.0350(15) 0.8388(14) 0.089(4) Uani 0.476(8) 1 d D . P B 1
H32A H -0.043524 1.087471 0.877631 0.107 Uiso 0.476(8) 1 calc R . P B 1
H32B H -0.114379 1.051306 0.786765 0.107 Uiso 0.476(8) 1 calc R . P B 1
C32B C -0.1356(16) 0.9757(13) 0.8147(12) 0.089(4) Uani 0.524(8) 1 d D U P B 2
H32C H -0.058386 1.018779 0.831040 0.107 Uiso 0.524(8) 1 calc R . P B 2
H32D H -0.171686 0.974233 0.758686 0.107 Uiso 0.524(8) 1 calc R . 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
Cu1 O1 2.404(4) . ?
Cu1 N1 1.985(4) . ?
Cu1 N2 2.004(4) . ?
Cu1 N3 1.995(4) . ?
Cu1 O7B 2.04(2) . ?
Cu1 O7A 1.85(3) . ?
Cu2 O9 2.312(4) . ?
Cu2 O15 1.936(4) . ?
Cu2 N4 1.989(4) . ?
Cu2 N5 2.002(4) . ?
Cu2 N6 1.994(4) . ?
V2 O2 1.787(4) 2_676 ?
V2 O5 1.645(4) . ?
V2 O4 1.787(4) . ?
V2 O6 1.615(4) . ?
V3 O9 1.656(3) . ?
V3 O12 1.779(4) . ?
V3 O10 1.783(4) . ?
V3 O11 1.629(4) . ?
V4 O12 1.793(4) . ?
V4 O10 1.789(4) 2_567 ?
V4 O14 1.620(4) . ?
V4 O13 1.635(4) . ?
V1 O1 1.650(4) . ?
V1 O3 1.626(4) . ?
V1 O2 1.796(4) . ?
V1 O4 1.783(4) . ?
O15 C28 1.264(7) . ?
N1 C5 1.357(7) . ?
N1 C1 1.333(6) . ?
N2 C10 1.338(7) . ?
N2 C6 1.352(6) . ?
N4 C22 1.334(6) . ?
N4 C18 1.342(7) . ?
N5 C23 1.352(7) . ?
N5 C27 1.330(7) . ?
N3 H3BC 0.8900 . ?
N3 H3BD 0.8900 . ?
N3 H3AA 0.8900 . ?
N3 H3AB 0.8900 . ?
N3 C12B 1.469(15) . ?
N3 C12A 1.499(17) . ?
O16 C28 1.244(7) . ?
O17 H17G 0.8493 . ?
O17 H17H 0.8501 . ?
N6 H6A 0.8900 . ?
N6 H6B 0.8900 . ?
N6 C29 1.469(8) . ?
O22 H22A 0.8499 . ?
O22 H22B 0.8504 . ?
O23 H23A 0.8501 . ?
O23 H23B 0.8497 . ?
C23 C22 1.486(8) . ?
C23 C24 1.391(8) . ?
C10 H10 0.9300 . ?
C10 C9 1.385(8) . ?
C22 C21 1.398(8) . ?
C5 C6 1.473(7) . ?
C5 C4 1.398(7) . ?
O19 H19A 0.8496 . ?
O19 H19B 0.8503 . ?
O18 H18A 0.8504 . ?
O18 H18B 0.8499 . ?
C6 C7 1.389(7) . ?
O20 H20A 0.8501 . ?
O20 H20B 0.8498 . ?
C1 H1 0.9300 . ?
C1 C2 1.380(8) . ?
C7 H7 0.9300 . ?
C7 C8 1.390(9) . ?
C8 H8 0.9300 . ?
C8 C9 1.358(9) . ?
C2 H2 0.9300 . ?
C2 C3 1.385(9) . ?
C9 H9 0.9300 . ?
C4 H4 0.9300 . ?
C4 C3 1.371(9) . ?
C24 H24 0.9300 . ?
C24 C25 1.382(9) . ?
C28 C29 1.511(9) . ?
C11 C12B 1.545(14) . ?
C11 C12A 1.546(16) . ?
C11 O8B 1.312(19) . ?
C11 O7B 1.21(2) . ?
C11 O7A 1.33(2) . ?
C11 O8A 1.17(2) . ?
C27 H27 0.9300 . ?
C27 C26 1.394(8) . ?
O21 H21A 0.8493 . ?
O21 H21B 0.8501 . ?
C26 H26 0.9300 . ?
C26 C25 1.383(10) . ?
C18 H18 0.9300 . ?
C18 C19 1.391(8) . ?
C3 H3 0.9300 . ?
C21 H21 0.9300 . ?
C21 C20 1.367(9) . ?
C20 H20 0.9300 . ?
C20 C19 1.378(9) . ?
C19 H19 0.9300 . ?
C25 H25 0.9300 . ?
C12B H12B 0.9800 . ?
C12B C13B 1.48(2) . ?
C13B H13A 0.9700 . ?
C13B H13B 0.9700 . ?
C13B C14B 1.457(18) . ?
C12A H12A 0.9800 . ?
C12A C13A 1.51(3) . ?
N17 H17A 0.8900 . ?
N17 H17B 0.8900 . ?
N17 H17C 0.8900 . ?
N17 H17D 0.8900 . ?
N17 H17E 0.8900 . ?
N17 H17F 0.8900 . ?
N17 C16A 1.471(19) . ?
N17 C16B 1.473(17) . ?
C16A H16A 0.9700 . ?
C16A H16B 0.9700 . ?
C16A C15A 1.53(4) . ?
C13A H13C 0.9700 . ?
C13A H13D 0.9700 . ?
C13A C14A 1.44(3) . ?
C14A H14A 0.9700 . ?
C14A H14B 0.9700 . ?
C14A C15A 1.40(4) . ?
C16B H16C 0.9700 . ?
C16B H16D 0.9700 . ?
C16B C15B 1.48(3) . ?
C14B H14C 0.9700 . ?
C14B H14D 0.9700 . ?
C14B C15B 1.46(3) . ?
C15A H15A 0.9700 . ?
C15A H15B 0.9700 . ?
C15B H15C 0.9700 . ?
C15B H15D 0.9700 . ?
C29 H29A 0.9800 . ?
C29 H29 0.9800 . ?
C29 C30B 1.424(13) . ?
C29 C30A 1.410(13) . ?
C30B H30A 0.9700 . ?
C30B H30B 0.9700 . ?
C30B C31B 1.541(16) . ?
C30A H30C 0.9700 . ?
C30A H30D 0.9700 . ?
C30A C31A 1.508(16) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 H33C 0.9700 . ?
C33 H33D 0.9700 . ?
C33 N34 1.492(10) . ?
C33 C32A 1.348(16) . ?
C33 C32B 1.446(15) . ?
N34 H34A 0.8900 . ?
N34 H34B 0.8900 . ?
N34 H34C 0.8900 . ?
C31A H31A 0.9700 . ?
C31A H31B 0.9700 . ?
C31A C32A 1.655(18) . ?
C31B H31C 0.9700 . ?
C31B H31D 0.9700 . ?
C31B C32B 1.609(17) . ?
C32A H32A 0.9700 . ?
C32A H32B 0.9700 . ?
C32B H32C 0.9700 . ?
C32B H32D 0.9700 . ?

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 O1 96.44(15) . . ?
N1 Cu1 N2 82.12(17) . . ?
N1 Cu1 N3 174.17(17) . . ?
N1 Cu1 O7B 93.5(7) . . ?
N2 Cu1 O1 92.42(15) . . ?
N2 Cu1 O7B 175.5(6) . . ?
N3 Cu1 O1 88.37(16) . . ?
N3 Cu1 N2 101.03(17) . . ?
N3 Cu1 O7B 83.3(7) . . ?
O7B Cu1 O1 88.8(10) . . ?
O7A Cu1 O1 97.0(12) . . ?
O7A Cu1 N1 92.2(8) . . ?
O7A Cu1 N2 169.5(10) . . ?
O7A Cu1 N3 83.9(9) . . ?
O15 Cu2 O9 102.49(15) . . ?
O15 Cu2 N4 91.45(17) . . ?
O15 Cu2 N5 161.68(18) . . ?
O15 Cu2 N6 83.58(17) . . ?
N4 Cu2 O9 94.68(16) . . ?
N4 Cu2 N5 81.46(18) . . ?
N4 Cu2 N6 173.84(18) . . ?
N5 Cu2 O9 94.94(15) . . ?
N6 Cu2 O9 89.96(18) . . ?
N6 Cu2 N5 102.20(19) . . ?
O2 V2 O4 110.8(2) 2_676 . ?
O5 V2 O2 109.0(2) . 2_676 ?
O5 V2 O4 106.7(2) . . ?
O6 V2 O2 109.2(2) . 2_676 ?
O6 V2 O5 110.0(2) . . ?
O6 V2 O4 111.1(2) . . ?
O9 V3 O12 108.51(19) . . ?
O9 V3 O10 108.9(2) . . ?
O12 V3 O10 111.1(2) . . ?
O11 V3 O9 109.5(2) . . ?
O11 V3 O12 109.8(2) . . ?
O11 V3 O10 109.0(2) . . ?
O10 V4 O12 111.2(2) 2_567 . ?
O14 V4 O12 108.7(2) . . ?
O14 V4 O10 110.9(2) . 2_567 ?
O14 V4 O13 109.6(3) . . ?
O13 V4 O12 108.5(2) . . ?
O13 V4 O10 107.9(2) . 2_567 ?
O1 V1 O2 109.01(19) . . ?
O1 V1 O4 108.6(2) . . ?
O3 V1 O1 108.5(2) . . ?
O3 V1 O2 108.7(2) . . ?
O3 V1 O4 111.5(2) . . ?
O4 V1 O2 110.5(2) . . ?
V3 O9 Cu2 131.8(2) . . ?
C28 O15 Cu2 116.3(4) . . ?
V1 O1 Cu1 126.34(19) . . ?
C5 N1 Cu1 114.2(3) . . ?
C1 N1 Cu1 126.7(4) . . ?
C1 N1 C5 118.8(4) . . ?
C10 N2 Cu1 127.1(4) . . ?
C10 N2 C6 119.3(4) . . ?
C6 N2 Cu1 113.4(3) . . ?
C22 N4 Cu2 115.1(4) . . ?
C22 N4 C18 119.5(5) . . ?
C18 N4 Cu2 125.4(4) . . ?
V3 O12 V4 138.9(2) . . ?
V3 O10 V4 139.1(3) . 2_567 ?
V2 O2 V1 140.1(2) 2_676 . ?
C23 N5 Cu2 113.9(4) . . ?
C27 N5 Cu2 126.8(4) . . ?
C27 N5 C23 118.8(5) . . ?
V1 O4 V2 157.7(3) . . ?
Cu1 N3 H3BC 110.3 . . ?
Cu1 N3 H3BD 110.3 . . ?
Cu1 N3 H3AA 109.0 . . ?
Cu1 N3 H3AB 109.0 . . ?
H3BC N3 H3BD 108.5 . . ?
H3AA N3 H3AB 107.8 . . ?
C12B N3 Cu1 107.2(6) . . ?
C12B N3 H3BC 110.3 . . ?
C12B N3 H3BD 110.3 . . ?
C12A N3 Cu1 112.8(6) . . ?
C12A N3 H3AA 109.0 . . ?
C12A N3 H3AB 109.0 . . ?
H17G O17 H17H 104.6 . . ?
Cu2 N6 H6A 110.1 . . ?
Cu2 N6 H6B 110.1 . . ?
H6A N6 H6B 108.5 . . ?
C29 N6 Cu2 107.8(4) . . ?
C29 N6 H6A 110.1 . . ?
C29 N6 H6B 110.1 . . ?
H22A O22 H22B 104.5 . . ?
H23A O23 H23B 104.5 . . ?
N5 C23 C22 114.3(4) . . ?
N5 C23 C24 122.3(5) . . ?
C24 C23 C22 123.3(5) . . ?
N2 C10 H10 119.1 . . ?
N2 C10 C9 121.8(5) . . ?
C9 C10 H10 119.1 . . ?
N4 C22 C23 114.6(4) . . ?
N4 C22 C21 120.7(5) . . ?
C21 C22 C23 124.7(5) . . ?
N1 C5 C6 114.7(4) . . ?
N1 C5 C4 121.7(5) . . ?
C4 C5 C6 123.6(5) . . ?
H19A O19 H19B 104.4 . . ?
H18A O18 H18B 109.4 . . ?
N2 C6 C5 115.2(4) . . ?
N2 C6 C7 120.8(5) . . ?
C7 C6 C5 123.9(5) . . ?
H20A O20 H20B 104.5 . . ?
N1 C1 H1 118.8 . . ?
N1 C1 C2 122.5(5) . . ?
C2 C1 H1 118.8 . . ?
C6 C7 H7 120.4 . . ?
C6 C7 C8 119.3(6) . . ?
C8 C7 H7 120.4 . . ?
C7 C8 H8 120.4 . . ?
C9 C8 C7 119.1(5) . . ?
C9 C8 H8 120.4 . . ?
C1 C2 H2 120.7 . . ?
C1 C2 C3 118.6(5) . . ?
C3 C2 H2 120.7 . . ?
C10 C9 H9 120.2 . . ?
C8 C9 C10 119.7(5) . . ?
C8 C9 H9 120.2 . . ?
C5 C4 H4 120.9 . . ?
C3 C4 C5 118.2(6) . . ?
C3 C4 H4 120.9 . . ?
C23 C24 H24 120.8 . . ?
C25 C24 C23 118.5(6) . . ?
C25 C24 H24 120.8 . . ?
O15 C28 C29 116.1(5) . . ?
O16 C28 O15 124.1(6) . . ?
O16 C28 C29 119.8(6) . . ?
O8B C11 C12B 116.3(12) . . ?
O7B C11 C12B 115.7(15) . . ?
O7B C11 O8B 126.4(17) . . ?
O7A C11 C12A 114.6(15) . . ?
O8A C11 C12A 121.9(16) . . ?
O8A C11 O7A 121(2) . . ?
N5 C27 H27 119.0 . . ?
N5 C27 C26 122.1(6) . . ?
C26 C27 H27 119.0 . . ?
H21A O21 H21B 104.5 . . ?
C27 C26 H26 120.4 . . ?
C25 C26 C27 119.1(6) . . ?
C25 C26 H26 120.4 . . ?
N4 C18 H18 118.8 . . ?
N4 C18 C19 122.4(5) . . ?
C19 C18 H18 118.8 . . ?
C2 C3 H3 119.9 . . ?
C4 C3 C2 120.2(5) . . ?
C4 C3 H3 119.9 . . ?
C22 C21 H21 120.2 . . ?
C20 C21 C22 119.7(6) . . ?
C20 C21 H21 120.2 . . ?
C21 C20 H20 120.1 . . ?
C21 C20 C19 119.8(6) . . ?
C19 C20 H20 120.1 . . ?
C18 C19 H19 121.1 . . ?
C20 C19 C18 117.9(6) . . ?
C20 C19 H19 121.1 . . ?
C24 C25 C26 119.2(6) . . ?
C24 C25 H25 120.4 . . ?
C26 C25 H25 120.4 . . ?
N3 C12B C11 108.5(8) . . ?
N3 C12B H12B 105.4 . . ?
N3 C12B C13B 118.4(13) . . ?
C11 C12B H12B 105.4 . . ?
C13B C12B C11 112.8(13) . . ?
C13B C12B H12B 105.4 . . ?
C12B C13B H13A 107.6 . . ?
C12B C13B H13B 107.6 . . ?
H13A C13B H13B 107.1 . . ?
C14B C13B C12B 118.8(14) . . ?
C14B C13B H13A 107.6 . . ?
C14B C13B H13B 107.6 . . ?
N3 C12A C11 106.9(9) . . ?
N3 C12A H12A 109.8 . . ?
N3 C12A C13A 109.8(14) . . ?
C11 C12A H12A 109.8 . . ?
C13A C12A C11 110.6(16) . . ?
C13A C12A H12A 109.8 . . ?
H17A N17 H17B 109.5 . . ?
H17A N17 H17C 109.5 . . ?
H17B N17 H17C 109.5 . . ?
H17D N17 H17E 109.5 . . ?
H17D N17 H17F 109.5 . . ?
H17E N17 H17F 109.5 . . ?
C16A N17 H17A 109.5 . . ?
C16A N17 H17B 109.5 . . ?
C16A N17 H17C 109.5 . . ?
C16B N17 H17D 109.5 . . ?
C16B N17 H17E 109.5 . . ?
C16B N17 H17F 109.5 . . ?
N17 C16A H16A 108.6 . . ?
N17 C16A H16B 108.6 . . ?
N17 C16A C15A 114.8(17) . . ?
H16A C16A H16B 107.5 . . ?
C15A C16A H16A 108.6 . . ?
C15A C16A H16B 108.6 . . ?
C12A C13A H13C 106.3 . . ?
C12A C13A H13D 106.3 . . ?
H13C C13A H13D 106.4 . . ?
C14A C13A C12A 124.1(18) . . ?
C14A C13A H13C 106.3 . . ?
C14A C13A H13D 106.3 . . ?
C13A C14A H14A 102.9 . . ?
C13A C14A H14B 102.9 . . ?
H14A C14A H14B 105.1 . . ?
C15A C14A C13A 137(3) . . ?
C15A C14A H14A 102.9 . . ?
C15A C14A H14B 102.9 . . ?
N17 C16B H16C 109.3 . . ?
N17 C16B H16D 109.3 . . ?
N17 C16B C15B 111.5(16) . . ?
H16C C16B H16D 108.0 . . ?
C15B C16B H16C 109.3 . . ?
C15B C16B H16D 109.3 . . ?
C13B C14B H14C 108.5 . . ?
C13B C14B H14D 108.5 . . ?
C13B C14B C15B 114.9(17) . . ?
H14C C14B H14D 107.5 . . ?
C15B C14B H14C 108.5 . . ?
C15B C14B H14D 108.5 . . ?
C16A C15A H15A 104.7 . . ?
C16A C15A H15B 104.7 . . ?
C14A C15A C16A 130(2) . . ?
C14A C15A H15A 104.7 . . ?
C14A C15A H15B 104.7 . . ?
H15A C15A H15B 105.7 . . ?
C16B C15B H15C 109.0 . . ?
C16B C15B H15D 109.0 . . ?
C14B C15B C16B 113.0(16) . . ?
C14B C15B H15C 109.0 . . ?
C14B C15B H15D 109.0 . . ?
H15C C15B H15D 107.8 . . ?
C11 O7B Cu1 113.1(18) . . ?
C11 O7A Cu1 119(2) . . ?
N6 C29 C28 109.7(5) . . ?
N6 C29 H29A 103.9 . . ?
N6 C29 H29 100.5 . . ?
C28 C29 H29A 103.9 . . ?
C28 C29 H29 100.5 . . ?
C30B C29 N6 121.4(8) . . ?
C30B C29 C28 112.0(8) . . ?
C30B C29 H29A 103.9 . . ?
C30A C29 N6 117.3(9) . . ?
C30A C29 C28 123.2(8) . . ?
C30A C29 H29 100.5 . . ?
C29 C30B H30A 108.2 . . ?
C29 C30B H30B 108.2 . . ?
C29 C30B C31B 116.3(13) . . ?
H30A C30B H30B 107.4 . . ?
C31B C30B H30A 108.2 . . ?
C31B C30B H30B 108.2 . . ?
C29 C30A H30C 106.9 . . ?
C29 C30A H30D 106.9 . . ?
C29 C30A C31A 121.6(12) . . ?
H30C C30A H30D 106.7 . . ?
C31A C30A H30C 106.9 . . ?
C31A C30A H30D 106.9 . . ?
H33A C33 H33B 109.8 . . ?
H33C C33 H33D 106.8 . . ?
N34 C33 H33A 112.2 . . ?
N34 C33 H33B 112.2 . . ?
N34 C33 H33C 107.2 . . ?
N34 C33 H33D 107.2 . . ?
C32A C33 H33A 112.2 . . ?
C32A C33 H33B 112.2 . . ?
C32A C33 N34 97.7(10) . . ?
C32B C33 H33C 107.2 . . ?
C32B C33 H33D 107.2 . . ?
C32B C33 N34 120.6(10) . . ?
C33 N34 H34A 109.5 . . ?
C33 N34 H34B 109.5 . . ?
C33 N34 H34C 109.5 . . ?
H34A N34 H34B 109.5 . . ?
H34A N34 H34C 109.5 . . ?
H34B N34 H34C 109.5 . . ?
C30A C31A H31A 111.7 . . ?
C30A C31A H31B 111.7 . . ?
C30A C31A C32A 100.6(11) . . ?
H31A C31A H31B 109.4 . . ?
C32A C31A H31A 111.7 . . ?
C32A C31A H31B 111.7 . . ?
C30B C31B H31C 108.8 . . ?
C30B C31B H31D 108.8 . . ?
C30B C31B C32B 113.7(13) . . ?
H31C C31B H31D 107.7 . . ?
C32B C31B H31C 108.8 . . ?
C32B C31B H31D 108.8 . . ?
C33 C32A C31A 99.3(11) . . ?
C33 C32A H32A 111.9 . . ?
C33 C32A H32B 111.9 . . ?
C31A C32A H32A 111.9 . . ?
C31A C32A H32B 111.9 . . ?
H32A C32A H32B 109.6 . . ?
C33 C32B C31B 116.8(12) . . ?
C33 C32B H32C 108.1 . . ?
C33 C32B H32D 108.1 . . ?
C31B C32B H32C 108.1 . . ?
C31B C32B H32D 108.1 . . ?
H32C C32B H32D 107.3 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3AA O22 0.89 2.20 3.031(7) 154.4 . yes
O17 H17G O8B 0.85 2.05 2.86(3) 160.3 . yes
O17 H17G O8A 0.85 1.88 2.70(3) 162.1 . yes
O17 H17H O19 0.85 1.89 2.706(8) 159.8 2_677 yes
N6 H6A O13 0.89 2.27 3.042(6) 145.2 2_567 yes
N6 H6B O17 0.89 2.11 2.995(8) 173.5 . yes
O22 H22B O5 0.85 2.24 2.804(7) 123.4 . yes
O23 H23A O20 0.85 1.93 2.753(8) 162.6 2_566 yes
O23 H23B O6 0.85 1.91 2.757(6) 175.5 2_666 yes
O19 H19A O8B 0.85 2.09 2.84(4) 146.9 . yes
O19 H19A O8A 0.85 2.04 2.82(4) 152.1 . yes
O19 H19B O14 0.85 1.87 2.714(7) 175.5 2_667 yes
O18 H18A O17 0.85 1.93 2.720(8) 154.0 2_677 yes
O18 H18B O1 0.85 2.20 2.942(7) 145.5 . yes
O20 H20A O22 0.85 2.29 2.866(8) 125.7 . yes
O20 H20B O16 0.85 2.04 2.786(9) 146.1 . yes
O21 H21A O9 0.85 1.93 2.765(7) 168.9 2_566 yes
O21 H21B O23 0.85 2.07 2.861(8) 154.7 . yes
N17 H17B O21 0.89 1.95 2.792(11) 157.7 2_666 yes
N17 H17C O5 0.89 2.10 2.864(7) 143.6 2_666 yes
N17 H17F O11 0.89 1.91 2.779(7) 163.9 1_655 yes
N34 H34A O13 0.89 1.97 2.805(8) 155.6 1_565 yes
N34 H34B O18 0.89 1.92 2.786(10) 164.0 1_455 yes
N34 H34C O3 0.89 2.04 2.833(7) 148.1 1_455 yes

_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 6.608
_oxdiff_exptl_absorpt_empirical_full_min 0.626
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
