# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1404576'
_audit_update_record             
;
2015-07-14 deposited with the CCDC.
2015-07-23 downloaded from the CCDC.
;

_audit_creation_date             2015-07-08T20:05:51-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C10 H34 Cu N4 O11 V2'
_chemical_formula_sum            'C10 H34 Cu N4 O11 V2'
_chemical_formula_weight         551.83
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   16.4455(3)
_cell_length_b                   15.0098(5)
_cell_length_c                   27.8995(7)
_cell_angle_alpha                79.513(2)
_cell_angle_beta                 98.024(2)
_cell_angle_gamma                105.156(2)
_cell_volume                     6505.5(3)
_cell_formula_units_Z            12
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    13498
_cell_measurement_theta_min      1.887
_cell_measurement_theta_max      27.992

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#
_exptl_crystal_description       prism
_exptl_crystal_colour            purple
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.69
_exptl_crystal_F_000             3420

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.95956
_exptl_absorpt_correction_T_max  1

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_detector_area_resol_mean 16.2439
_diffrn_orient_matrix_ub_11      0.024691
_diffrn_orient_matrix_ub_12      -0.0043702
_diffrn_orient_matrix_ub_13      -0.0240898
_diffrn_orient_matrix_ub_21      -0.040847
_diffrn_orient_matrix_ub_22      -0.0038886
_diffrn_orient_matrix_ub_23      -0.0079479
_diffrn_orient_matrix_ub_31      -0.0132561
_diffrn_orient_matrix_ub_32      0.0445132
_diffrn_orient_matrix_ub_33      -0.0055991
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.072
_diffrn_reflns_number            46122
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.672
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        24.998
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 1
_reflns_number_total             22908
_reflns_number_gt                17910
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
        (compiled May 22 2014,16:03:01)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
        (compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
        (compiled May 22 2014,16:03:01)
;
_computing_structure_solution    'OLEX2 (Dolomanov, 2009)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom


#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0397P)²+13.3392P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         22908
_refine_ls_number_parameters     1558
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0458
_refine_ls_wR_factor_ref         0.1106
_refine_ls_wR_factor_gt          0.1012
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.997
_refine_diff_density_min         -1.075
_refine_diff_density_rms         0.107

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'

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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.07832(4) 0.62407(5) 0.17775(3) 0.00903(16) Uani 1 d . .
V2 V 0.20012(4) 0.60708(5) 0.09577(3) 0.00944(16) Uani 1 d . .
V3 V 0.36314(4) 0.53036(5) 0.15735(3) 0.00839(16) Uani 1 d . .
V4 V 0.57072(4) 0.56631(5) 0.19901(3) 0.00905(16) Uani 1 d . .
V5 V 0.71353(4) 0.51696(5) 0.14403(3) 0.00884(16) Uani 1 d . .
V6 V 0.88841(4) 0.45755(5) 0.20637(3) 0.00832(16) Uani 1 d . .
V7 V 0.43956(4) -0.00647(5) 0.29241(3) 0.00918(16) Uani 1 d . .
V8 V 0.29767(4) 0.02552(5) 0.35368(3) 0.00946(16) Uani 1 d . .
V9 V 0.12724(4) 0.10011(5) 0.29692(3) 0.00961(16) Uani 1 d . .
V10 V -0.07197(4) -0.06358(5) 0.31040(3) 0.00879(16) Uani 1 d . .
V11 V -0.20134(4) -0.07867(5) 0.39832(3) 0.01079(16) Uani 1 d . .
V12 V -0.35856(4) 0.01593(5) 0.34375(3) 0.00986(16) Uani 1 d . .
Cu1A Cu 0.76192(3) 0.45493(4) 0.02571(2) 0.01112(12) Uani 1 d . .
Cu1B Cu 0.75023(3) 0.79266(4) 0.22149(2) 0.01423(13) Uani 1 d . .
Cu1C Cu 0.77419(3) 0.24102(4) 0.28258(2) 0.01082(12) Uani 1 d . .
Cu1D Cu 0.24537(3) 0.06182(4) 0.47527(2) 0.01250(13) Uani 1 d . .
Cu1E Cu 0.24978(3) 0.77829(4) 0.25168(2) 0.01186(12) Uani 1 d . .
Cu1F Cu 0.23923(3) 0.31435(4) 0.22424(2) 0.01075(12) Uani 1 d . .
O1 O 0.07027(18) 0.7290(2) 0.15078(11) 0.0148(7) Uani 1 d . .
O2 O 0.20171(19) 0.7110(2) 0.06407(11) 0.0158(7) Uani 1 d . .
O3 O 0.35371(18) 0.4564(2) 0.11847(11) 0.0132(7) Uani 1 d . .
O4 O 0.55565(19) 0.5106(2) 0.25424(11) 0.0172(7) Uani 1 d . .
O5 O 0.74624(18) 0.6264(2) 0.11777(11) 0.0132(7) Uani 1 d . .
O6 O 0.97631(18) 0.5551(2) 0.19583(11) 0.0154(7) Uani 1 d . .
O7 O 0.46507(19) 0.0566(2) 0.23989(11) 0.0164(7) Uani 1 d . .
O8 O 0.2688(2) -0.0866(2) 0.37598(11) 0.0190(7) Uani 1 d . .
O9 O 0.13882(18) 0.1727(2) 0.33647(10) 0.0134(7) Uani 1 d . .
O10 O -0.06031(18) -0.1700(2) 0.32919(11) 0.0142(7) Uani 1 d . .
O11 O -0.20083(19) -0.1882(2) 0.42103(12) 0.0192(7) Uani 1 d . .
O12 O 0.11798(18) 0.5680(2) 0.13688(11) 0.0140(7) Uani 1 d . .
O1M O 0.14807(18) 0.6379(2) 0.22557(11) 0.0153(7) Uani 1 d . .
O2M O 0.18711(18) 0.5330(2) 0.05700(10) 0.0120(7) Uani 1 d . .
O3M O 0.32696(18) 0.4695(2) 0.20803(11) 0.0147(7) Uani 1 d . .
O4M O 0.64138(17) 0.6652(2) 0.20269(11) 0.0140(7) Uani 1 d . .
O5M O 0.70642(18) 0.4492(2) 0.10282(10) 0.0121(7) Uani 1 d . .
O6M O 0.89357(18) 0.4026(2) 0.26307(11) 0.0145(7) Uani 1 d . .
O7M O 0.36691(18) -0.1006(2) 0.28194(11) 0.0161(7) Uani 1 d . .
O8M O 0.30398(18) 0.0855(2) 0.39812(10) 0.0128(7) Uani 1 d . .
O9M O 0.12570(18) 0.1594(2) 0.24126(11) 0.0156(7) Uani 1 d . .
O10M O -0.12716(18) -0.0624(2) 0.25633(11) 0.0150(7) Uani 1 d . .
O11M O -0.17842(19) -0.0175(2) 0.44327(11) 0.0185(7) Uani 1 d . .
O12M O -0.31151(19) 0.0796(2) 0.29680(11) 0.0186(7) Uani 1 d . .
O23 O 0.30122(18) 0.6133(2) 0.13285(11) 0.0143(7) Uani 1 d . .
O34 O 0.47260(17) 0.5916(2) 0.16780(10) 0.0115(7) Uani 1 d . .
O45 O 0.61072(17) 0.4954(2) 0.16554(11) 0.0128(7) Uani 1 d . .
O56 O 0.78723(17) 0.4893(2) 0.19500(10) 0.0120(7) Uani 1 d . .
O61 O 0.88493(18) 0.3827(2) 0.16919(11) 0.0132(7) Uani 1 d . .
O78 O 0.39791(18) 0.0592(2) 0.32806(11) 0.0130(7) Uani 1 d . .
O89 O 0.21825(18) 0.0519(2) 0.30582(11) 0.0180(7) Uani 1 d . .
O101 O -0.12746(19) -0.0294(2) 0.35259(11) 0.0162(7) Uani 1 d . .
O112 O -0.30558(18) -0.0750(2) 0.36978(12) 0.0192(7) Uani 1 d . .
O127 O -0.35110(19) 0.0861(2) 0.38437(11) 0.0186(7) Uani 1 d . .
O712 O 0.53248(17) -0.0390(2) 0.32724(11) 0.0128(7) Uani 1 d . .
O910 O 0.03041(18) 0.0135(2) 0.30408(11) 0.0162(7) Uani 1 d . .
N4A N 0.8737(2) 0.4450(3) 0.06303(13) 0.0131(8) Uani 1 d . .
H4A H 0.8681 0.445 0.0976 0.016 Uiso 1 calc . .
N11F N 0.1384(2) 0.3704(3) 0.20075(13) 0.0114(8) Uani 1 d . .
H11F H 0.1607 0.4347 0.1853 0.014 Uiso 1 calc . .
N11B N 0.8269(2) 0.7178(3) 0.26117(15) 0.0232(10) Uani 1 d . .
H11B H 0.8668 0.7592 0.2818 0.028 Uiso 1 calc . .
N4B N 0.6794(3) 0.8766(3) 0.18203(15) 0.0246(10) Uani 1 d . .
H4B H 0.6335 0.8363 0.1639 0.03 Uiso 1 calc . .
N8F N 0.2320(2) 0.3465(3) 0.29044(13) 0.0136(8) Uani 1 d . .
H8F H 0.2029 0.2888 0.31 0.016 Uiso 1 calc . .
N4F N 0.3349(2) 0.2507(3) 0.24953(13) 0.0138(8) Uani 1 d . .
H4F H 0.3091 0.1885 0.2664 0.017 Uiso 1 calc . .
N8B N 0.8166(2) 0.7979(3) 0.16446(15) 0.0241(10) Uani 1 d . .
H8B H 0.7851 0.7456 0.1475 0.029 Uiso 1 calc . .
N8A N 0.7866(2) 0.5950(3) 0.02303(13) 0.0128(8) Uani 1 d . .
H8A H 0.7735 0.6049 0.0546 0.015 Uiso 1 calc . .
N1A N 0.7383(2) 0.3149(3) 0.02903(13) 0.0132(8) Uani 1 d . .
H1A H 0.7509 0.3041 -0.0024 0.016 Uiso 1 calc . .
N1F N 0.2452(2) 0.2771(3) 0.15934(13) 0.0142(8) Uani 1 d . .
H1F H 0.2778 0.3324 0.1396 0.017 Uiso 1 calc . .
N11A N 0.6510(2) 0.4650(3) -0.01247(13) 0.0134(8) Uani 1 d . .
H11A H 0.6585 0.4684 -0.047 0.016 Uiso 1 calc . .
N1B N 0.6892(3) 0.7955(3) 0.27865(15) 0.0249(10) Uani 1 d . .
H1B H 0.726 0.8422 0.2976 0.03 Uiso 1 calc . .
C13A C 0.5885(3) 0.2941(3) -0.00484(17) 0.0198(11) Uani 1 d . .
H13A H 0.609 0.2967 -0.0361 0.024 Uiso 1 calc . .
H13B H 0.5342 0.2488 -0.0038 0.024 Uiso 1 calc . .
C6F C 0.3671(3) 0.3106(3) 0.32934(17) 0.0206(11) Uani 1 d . .
H6FA H 0.414 0.3305 0.3534 0.025 Uiso 1 calc . .
H6FB H 0.333 0.2512 0.3437 0.025 Uiso 1 calc . .
C7F C 0.3136(3) 0.3817(3) 0.31907(17) 0.0182(11) Uani 1 d . .
H7FA H 0.3026 0.3956 0.3498 0.022 Uiso 1 calc . .
H7FB H 0.3445 0.4392 0.301 0.022 Uiso 1 calc . .
C9A C 0.7225(3) 0.6268(3) -0.01410(16) 0.0168(10) Uani 1 d . .
H9AA H 0.738 0.6303 -0.0468 0.02 Uiso 1 calc . .
H9AB H 0.7184 0.6882 -0.01 0.02 Uiso 1 calc . .
C10A C 0.6389(3) 0.5566(3) -0.00689(17) 0.0167(10) Uani 1 d . .
H10A H 0.6224 0.5543 0.0255 0.02 Uiso 1 calc . .
H10B H 0.595 0.5736 -0.0311 0.02 Uiso 1 calc . .
C5A C 0.9474(3) 0.5217(3) 0.04918(17) 0.0197(11) Uani 1 d . .
H5AA H 0.9558 0.5225 0.0154 0.024 Uiso 1 calc . .
H5AB H 0.9976 0.5102 0.0695 0.024 Uiso 1 calc . .
C7B C 0.8304(3) 0.8807(4) 0.12615(18) 0.0258(12) Uani 1 d . .
H7BA H 0.8508 0.8649 0.0986 0.031 Uiso 1 calc . .
H7BB H 0.8745 0.9299 0.1389 0.031 Uiso 1 calc . .
C10F C 0.1031(3) 0.3758(3) 0.24603(16) 0.0144(10) Uani 1 d . .
H10C H 0.071 0.3145 0.2594 0.017 Uiso 1 calc . .
H10D H 0.0655 0.4177 0.2387 0.017 Uiso 1 calc . .
C13F C 0.1096(3) 0.3144(3) 0.12025(16) 0.0163(10) Uani 1 d . .
H13C H 0.1429 0.3749 0.1067 0.02 Uiso 1 calc . .
H13D H 0.0633 0.2949 0.0958 0.02 Uiso 1 calc . .
C2F C 0.2961(3) 0.2066(3) 0.16870(18) 0.0187(11) Uani 1 d . .
H2FA H 0.3168 0.202 0.1386 0.022 Uiso 1 calc . .
H2FB H 0.2615 0.1459 0.181 0.022 Uiso 1 calc . .
C3A C 0.8849(3) 0.3519(3) 0.05927(18) 0.0184(11) Uani 1 d . .
H3AA H 0.9281 0.3354 0.0842 0.022 Uiso 1 calc . .
H3AB H 0.9022 0.3522 0.0274 0.022 Uiso 1 calc . .
C7A C 0.8738(3) 0.6521(3) 0.01657(17) 0.0201(11) Uani 1 d . .
H7AA H 0.8768 0.7165 0.0192 0.024 Uiso 1 calc . .
H7AB H 0.888 0.6506 -0.0158 0.024 Uiso 1 calc . .
C14A C 0.6502(3) 0.2606(3) 0.03584(17) 0.0201(11) Uani 1 d . .
H14A H 0.6354 0.2673 0.0672 0.024 Uiso 1 calc . .
H14B H 0.6462 0.1949 0.0359 0.024 Uiso 1 calc . .
C3F C 0.3689(3) 0.2363(3) 0.20575(17) 0.0186(11) Uani 1 d . .
H3FA H 0.4006 0.1886 0.2148 0.022 Uiso 1 calc . .
H3FB H 0.4066 0.2938 0.1921 0.022 Uiso 1 calc . .
C14F C 0.1649(3) 0.2447(3) 0.12958(16) 0.0144(10) Uani 1 d . .
H14C H 0.1339 0.1857 0.1463 0.017 Uiso 1 calc . .
H14D H 0.1772 0.2339 0.0984 0.017 Uiso 1 calc . .
C13B C 0.7422(3) 0.6627(4) 0.33154(19) 0.0305(13) Uani 1 d . .
H13E H 0.7839 0.7067 0.3494 0.037 Uiso 1 calc . .
H13F H 0.7232 0.6069 0.3548 0.037 Uiso 1 calc . .
C6A C 0.9367(3) 0.6157(4) 0.05486(17) 0.0220(12) Uani 1 d . .
H6AA H 0.9912 0.6603 0.0534 0.026 Uiso 1 calc . .
H6AB H 0.9185 0.6114 0.087 0.026 Uiso 1 calc . .
C14B C 0.6677(3) 0.7044(4) 0.3133(2) 0.0329(14) Uani 1 d . .
H14E H 0.6442 0.715 0.3412 0.039 Uiso 1 calc . .
H14F H 0.6244 0.6599 0.2967 0.039 Uiso 1 calc . .
C5B C 0.7183(3) 0.9532(4) 0.14581(19) 0.0293(13) Uani 1 d . .
H5BA H 0.7634 0.9965 0.1621 0.035 Uiso 1 calc . .
H5BB H 0.6764 0.9866 0.1297 0.035 Uiso 1 calc . .
C12A C 0.5754(3) 0.3886(3) -0.00178(18) 0.0192(11) Uani 1 d . .
H12A H 0.528 0.3999 -0.0249 0.023 Uiso 1 calc . .
H12B H 0.5612 0.3886 0.0308 0.023 Uiso 1 calc . .
C9F C 0.1755(3) 0.4113(3) 0.28251(17) 0.0173(10) Uani 1 d . .
H9FA H 0.2059 0.474 0.2699 0.021 Uiso 1 calc . .
H9FB H 0.1545 0.4129 0.3131 0.021 Uiso 1 calc . .
C12F C 0.0729(3) 0.3252(3) 0.16523(16) 0.0148(10) Uani 1 d . .
H12C H 0.0313 0.3622 0.1552 0.018 Uiso 1 calc . .
H12D H 0.0441 0.2641 0.1809 0.018 Uiso 1 calc . .
C9B C 0.8961(3) 0.7749(4) 0.1854(2) 0.0295(13) Uani 1 d . .
H9BA H 0.9349 0.8287 0.1974 0.035 Uiso 1 calc . .
H9BB H 0.922 0.7569 0.1607 0.035 Uiso 1 calc . .
C2A C 0.8019(3) 0.2834(3) 0.06636(17) 0.0199(11) Uani 1 d . .
H2AA H 0.8056 0.2216 0.0626 0.024 Uiso 1 calc . .
H2AB H 0.7861 0.2807 0.0989 0.024 Uiso 1 calc . .
C10B C 0.8771(3) 0.6950(3) 0.22709(19) 0.0224(11) Uani 1 d . .
H10E H 0.8458 0.6386 0.2142 0.027 Uiso 1 calc . .
H10F H 0.9297 0.6837 0.2445 0.027 Uiso 1 calc . .
C3B C 0.6389(3) 0.9082(4) 0.2182(2) 0.0304(13) Uani 1 d . .
H3BA H 0.678 0.9605 0.2314 0.036 Uiso 1 calc . .
H3BB H 0.589 0.9283 0.2024 0.036 Uiso 1 calc . .
C2B C 0.6151(3) 0.8298(4) 0.2581(2) 0.0305(13) Uani 1 d . .
H2BA H 0.5927 0.8506 0.2833 0.037 Uiso 1 calc . .
H2BB H 0.5715 0.78 0.2454 0.037 Uiso 1 calc . .
C6B C 0.7536(3) 0.9176(4) 0.1082(2) 0.0345(14) Uani 1 d . .
H6BA H 0.7097 0.8682 0.0954 0.041 Uiso 1 calc . .
H6BB H 0.7676 0.9679 0.0812 0.041 Uiso 1 calc . .
C12B C 0.7857(3) 0.6369(4) 0.29404(19) 0.0312(13) Uani 1 d . .
H12E H 0.8277 0.604 0.3107 0.037 Uiso 1 calc . .
H12F H 0.7444 0.5948 0.275 0.037 Uiso 1 calc . .
C5F C 0.4022(3) 0.2959(3) 0.28481(17) 0.0189(11) Uani 1 d . .
H5FA H 0.4324 0.3559 0.2686 0.023 Uiso 1 calc . .
H5FB H 0.4424 0.2574 0.2953 0.023 Uiso 1 calc . .
N8D N 0.2897(2) 0.1977(3) 0.48218(14) 0.0180(9) Uani 1 d . .
H8D H 0.2794 0.2043 0.515 0.022 Uiso 1 calc . .
N11D N 0.1427(2) 0.1005(3) 0.43888(14) 0.0165(9) Uani 1 d . .
H11D H 0.1495 0.1073 0.404 0.02 Uiso 1 calc . .
N4D N 0.3472(2) 0.0234(3) 0.51378(14) 0.0175(9) Uani 1 d . .
H4D H 0.3379 0.0151 0.5484 0.021 Uiso 1 calc . .
N1D N 0.2003(2) -0.0740(3) 0.46823(13) 0.0174(9) Uani 1 d . .
H1D H 0.2115 -0.0802 0.4356 0.021 Uiso 1 calc . .
C2D C 0.2533(3) -0.1256(3) 0.50362(17) 0.0218(11) Uani 1 d . .
H2DA H 0.2476 -0.1867 0.4948 0.026 Uiso 1 calc . .
H2DB H 0.2355 -0.134 0.5362 0.026 Uiso 1 calc . .
C6D C 0.4338(3) 0.1847(4) 0.51678(19) 0.0272(13) Uani 1 d . .
H6DA H 0.4136 0.1809 0.5483 0.033 Uiso 1 calc . .
H6DB H 0.4921 0.2208 0.5182 0.033 Uiso 1 calc . .
C7D C 0.3816(3) 0.2361(4) 0.47781(19) 0.0254(12) Uani 1 d . .
H7DA H 0.3967 0.3019 0.481 0.03 Uiso 1 calc . .
H7DB H 0.3943 0.2308 0.4457 0.03 Uiso 1 calc . .
C10D C 0.1471(3) 0.1953(4) 0.44903(18) 0.0222(11) Uani 1 d . .
H10G H 0.1293 0.1917 0.4812 0.027 Uiso 1 calc . .
H10H H 0.1104 0.2252 0.4248 0.027 Uiso 1 calc . .
C14D C 0.1082(3) -0.1148(4) 0.47181(19) 0.0260(12) Uani 1 d . .
H14G H 0.0954 -0.1159 0.5048 0.031 Uiso 1 calc . .
H14H H 0.094 -0.1788 0.4654 0.031 Uiso 1 calc . .
C12D C 0.0598(3) 0.0365(4) 0.44630(19) 0.0256(12) Uani 1 d . .
H12G H 0.0166 0.0617 0.4251 0.031 Uiso 1 calc . .
H12H H 0.0482 0.0322 0.4799 0.031 Uiso 1 calc . .
C3D C 0.3439(3) -0.0703(4) 0.50287(18) 0.0244(12) Uani 1 d . .
H3DA H 0.3801 -0.1007 0.5273 0.029 Uiso 1 calc . .
H3DB H 0.3632 -0.0653 0.4709 0.029 Uiso 1 calc . .
C9D C 0.2372(3) 0.2495(3) 0.44685(18) 0.0222(11) Uani 1 d . .
H9DA H 0.2539 0.2564 0.4141 0.027 Uiso 1 calc . .
H9DB H 0.2441 0.3113 0.4551 0.027 Uiso 1 calc . .
C5D C 0.4313(3) 0.0870(4) 0.50856(18) 0.0231(12) Uani 1 d . .
H5DA H 0.4469 0.0896 0.476 0.028 Uiso 1 calc . .
H5DB H 0.4726 0.0625 0.532 0.028 Uiso 1 calc . .
C13D C 0.0548(3) -0.0598(4) 0.43591(18) 0.0259(12) Uani 1 d . .
H13G H 0.072 -0.0542 0.4034 0.031 Uiso 1 calc . .
H13H H -0.0038 -0.095 0.4356 0.031 Uiso 1 calc . .
N1E N 0.1672(2) 0.8073(3) 0.29037(14) 0.0156(9) Uani 1 d . .
H1E H 0.1998 0.8532 0.3111 0.019 Uiso 1 calc . .
N4E N 0.2081(2) 0.8652(3) 0.19558(13) 0.0142(8) Uani 1 d . .
H4E H 0.166 0.8259 0.1748 0.017 Uiso 1 calc . .
N11E N 0.2927(2) 0.6944(3) 0.30899(14) 0.0183(9) Uani 1 d . .
H11E H 0.3323 0.7355 0.33 0.022 Uiso 1 calc . .
N8E N 0.3326(2) 0.7487(3) 0.21331(14) 0.0176(9) Uani 1 d . .
H8E H 0.3008 0.6987 0.1949 0.021 Uiso 1 calc . .
C3E C 0.1622(3) 0.9190(3) 0.21654(18) 0.0217(11) Uani 1 d . .
H3EA H 0.1256 0.9464 0.191 0.026 Uiso 1 calc . .
H3EB H 0.2021 0.969 0.2312 0.026 Uiso 1 calc . .
C6E C 0.3170(3) 0.8693(4) 0.14171(19) 0.0291(13) Uani 1 d . .
H6EA H 0.2752 0.8204 0.1273 0.035 Uiso 1 calc . .
H6EB H 0.3482 0.9096 0.1156 0.035 Uiso 1 calc . .
C7E C 0.3770(3) 0.8257(4) 0.17777(19) 0.0272(13) Uani 1 d . .
H7EA H 0.4116 0.8017 0.1603 0.033 Uiso 1 calc . .
H7EB H 0.4143 0.8731 0.1954 0.033 Uiso 1 calc . .
C5E C 0.2712(3) 0.9264(3) 0.16342(18) 0.0232(12) Uani 1 d . .
H5EA H 0.3121 0.9695 0.1821 0.028 Uiso 1 calc . .
H5EB H 0.243 0.9627 0.1372 0.028 Uiso 1 calc . .
C12E C 0.2299(3) 0.6314(3) 0.34053(18) 0.0262(12) Uani 1 d . .
H12K H 0.2591 0.5974 0.3674 0.031 Uiso 1 calc . .
H12L H 0.1923 0.5861 0.3216 0.031 Uiso 1 calc . .
C14E C 0.1196(3) 0.7269(3) 0.32305(18) 0.0237(12) Uani 1 d . .
H14K H 0.0856 0.6808 0.3034 0.028 Uiso 1 calc . .
H14L H 0.0815 0.748 0.3395 0.028 Uiso 1 calc . .
C2E C 0.1104(3) 0.8534(3) 0.25478(18) 0.0217(11) Uani 1 d . .
H2EA H 0.0832 0.8878 0.2712 0.026 Uiso 1 calc . .
H2EB H 0.0668 0.8071 0.2395 0.026 Uiso 1 calc . .
C13E C 0.1778(3) 0.6816(4) 0.36116(18) 0.0295(13) Uani 1 d . .
H13K H 0.2158 0.7295 0.3783 0.035 Uiso 1 calc . .
H13L H 0.1439 0.6375 0.385 0.035 Uiso 1 calc . .
C10E C 0.3434(3) 0.6446(3) 0.2891(2) 0.0268(13) Uani 1 d . .
H10K H 0.3065 0.5915 0.2755 0.032 Uiso 1 calc . .
H10L H 0.3819 0.6215 0.3151 0.032 Uiso 1 calc . .
C9E C 0.3925(3) 0.7093(4) 0.2503(2) 0.0254(12) Uani 1 d . .
H9EA H 0.4337 0.7591 0.2644 0.03 Uiso 1 calc . .
H9EB H 0.4225 0.6758 0.2351 0.03 Uiso 1 calc . .
N1C N 0.7746(2) 0.2137(2) 0.21433(12) 0.0106(8) Uani 1 d . .
H1C H 0.801 0.2728 0.1948 0.013 Uiso 1 calc . .
N8C N 0.7716(2) 0.2700(3) 0.35003(13) 0.0125(8) Uani 1 d . .
H8C H 0.7335 0.2156 0.3672 0.015 Uiso 1 calc . .
N4C N 0.8722(2) 0.1800(3) 0.30138(13) 0.0118(8) Uani 1 d . .
H4C H 0.8486 0.1141 0.3138 0.014 Uiso 1 calc . .
N11C N 0.6831(2) 0.3117(3) 0.26114(13) 0.0122(8) Uani 1 d . .
H11C H 0.7103 0.3728 0.2437 0.015 Uiso 1 calc . .
C7C C 0.8511(3) 0.2885(3) 0.38235(17) 0.0178(11) Uani 1 d . .
H7CA H 0.838 0.291 0.4149 0.021 Uiso 1 calc . .
H7CB H 0.8858 0.3493 0.3702 0.021 Uiso 1 calc . .
C14C C 0.6899(3) 0.1798(3) 0.18881(17) 0.0163(10) Uani 1 d . .
H14I H 0.6603 0.1228 0.2079 0.02 Uiso 1 calc . .
H14J H 0.6963 0.1655 0.1572 0.02 Uiso 1 calc . .
C2C C 0.8316(3) 0.1515(3) 0.21808(16) 0.0136(10) Uani 1 d . .
H2CA H 0.8508 0.1545 0.1864 0.016 Uiso 1 calc . .
H2CB H 0.8024 0.0875 0.2291 0.016 Uiso 1 calc . .
C10C C 0.6540(3) 0.3291(4) 0.30597(17) 0.0196(11) Uani 1 d . .
H10I H 0.6117 0.275 0.3189 0.024 Uiso 1 calc . .
H10J H 0.6288 0.3823 0.2982 0.024 Uiso 1 calc . .
C9C C 0.7293(3) 0.3482(3) 0.34319(17) 0.0192(11) Uani 1 d . .
H9CA H 0.7684 0.4065 0.3319 0.023 Uiso 1 calc . .
H9CB H 0.7113 0.3532 0.374 0.023 Uiso 1 calc . .
C3C C 0.9059(3) 0.1833(3) 0.25428(16) 0.0146(10) Uani 1 d . .
H3CA H 0.9442 0.1425 0.2585 0.018 Uiso 1 calc . .
H3CB H 0.9366 0.2463 0.2426 0.018 Uiso 1 calc . .
C6C C 0.9016(3) 0.2160(3) 0.38606(16) 0.0150(10) Uani 1 d . .
H6CA H 0.8652 0.1546 0.3951 0.018 Uiso 1 calc . .
H6CB H 0.9473 0.2263 0.412 0.018 Uiso 1 calc . .
C13C C 0.6384(3) 0.2515(3) 0.18150(17) 0.0184(11) Uani 1 d . .
H13I H 0.5882 0.2315 0.1596 0.022 Uiso 1 calc . .
H13J H 0.6713 0.31 0.1654 0.022 Uiso 1 calc . .
C5C C 0.9387(3) 0.2173(3) 0.33888(16) 0.0144(10) Uani 1 d . .
H5CA H 0.9672 0.2808 0.3265 0.017 Uiso 1 calc . .
H5CB H 0.9803 0.18 0.3456 0.017 Uiso 1 calc . .
C12C C 0.6110(3) 0.2692(3) 0.22750(17) 0.0183(11) Uani 1 d . .
H12I H 0.5729 0.3105 0.2186 0.022 Uiso 1 calc . .
H12J H 0.58 0.2106 0.2445 0.022 Uiso 1 calc . .
O1W O 0.5028(2) 0.0516(2) 0.14439(12) 0.0211(8) Uani 1 d . .
O2W O 0.4568(2) 0.2023(2) 0.08947(12) 0.0263(8) Uani 1 d . .
O3W O 0.9891(2) 0.0522(2) 0.18482(11) 0.0238(8) Uani 1 d . .
O4W O 1.0294(2) 1.0312(2) 0.09259(12) 0.0253(8) Uani 1 d . .
O5W O 1.0408(3) 0.8456(3) -0.02451(16) 0.0257(11) Uani 0.75 d . .
O6W O 1.0790(10) 0.9329(13) -0.0111(5) 0.046(5) Uani 0.25 d . .
O7W O 1.0085(2) 0.8496(3) 0.07230(14) 0.0372(10) Uani 1 d . .
O8W O 1.0100(2) 0.4964(3) 0.33767(14) 0.0381(10) Uani 1 d . .
O9W O 0.9029(3) 0.5362(3) 0.39541(16) 0.0511(12) Uani 1 d . .
O10W O 0.8797(3) 0.4276(3) 0.48976(17) 0.0522(12) Uani 1 d . .
O11W O 0.9232(2) 0.7197(2) 0.41864(12) 0.0249(8) Uani 1 d . .
O12W O 0.9698(5) 0.6164(6) 0.5072(3) 0.027(2) Uani 0.5 d . .
O13W O 0.9975(6) 0.6690(7) 0.5129(3) 0.038(2) Uani 0.5 d . .
O14W O 0.6897(3) 0.6414(3) 0.45092(14) 0.0445(11) Uani 1 d . .
O15W O 0.53408(19) 0.7745(2) 0.11662(11) 0.0158(7) Uani 1 d . .
O16W O 0.50681(19) 0.9467(2) 0.07501(11) 0.0192(7) Uani 1 d . .
O17W O 0.6249(2) 0.7144(2) 0.06075(11) 0.0192(7) Uani 1 d . .
O18W O 0.6697(2) 0.8557(2) -0.01638(12) 0.0210(8) Uani 1 d . .
O19W O 0.7099(3) 0.3473(3) 0.50054(14) 0.0398(10) Uani 1 d . .
O20W O 0.5452(3) 0.4803(3) 0.35582(14) 0.0532(13) Uani 1 d . .
O21W O 0.5320(3) 0.6230(3) 0.40352(17) 0.0503(12) Uani 1 d . .
O22W O 0.5505(5) 0.4378(6) 0.5061(3) 0.040(2) Uani 0.5 d . .
O23W O 0.4149(7) 0.4865(8) 0.4396(4) 0.082(3) Uani 0.5 d . .
O24W O 0.5781(2) 0.3396(3) 0.42756(14) 0.0349(9) Uani 1 d . .
O25W O 0.4638(2) 0.7710(2) 0.36556(12) 0.0260(8) Uani 1 d . .
O26W O 0.2686(3) 0.4846(3) 0.46861(16) 0.0502(12) Uani 1 d . .
O27W O 0.1096(7) 0.4542(9) 0.4282(4) 0.045(3) Uani 0.4 d . .
O28W O 0.1162(5) 0.4170(5) 0.4090(3) 0.0355(19) Uani 0.6 d . .
O29W O 0.3604(2) 0.7915(3) 0.42889(13) 0.0311(9) Uani 1 d . .
O30W O 0.48622(19) 0.3788(2) 0.11182(12) 0.0192(7) Uani 1 d . .
O31W O 0.2153(2) 0.8880(3) 0.01125(15) 0.0394(11) Uani 1 d . .
O32W O 0.61552(19) 1.0097(2) -0.00002(12) 0.0198(7) Uani 1 d . .
O33W O 0.8443(10) 0.8988(13) -0.0289(6) 0.023(4) Uani 0.2 d . .
O34W O 0.8177(3) 0.9545(4) -0.0502(2) 0.0442(14) Uani 0.8 d . .
O35W O 0.5199(2) 0.1677(2) 0.39370(12) 0.0237(8) Uani 1 d . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
V1 O1M 1.640(3) . ?
V1 O1 1.648(3) . ?
V1 O12 1.810(3) . ?
V1 O6 1.811(3) 1_455 ?
V2 O2 1.643(3) . ?
V2 O2M 1.643(3) . ?
V2 O12 1.805(3) . ?
V2 O23 1.821(3) . ?
V3 O3M 1.633(3) . ?
V3 O3 1.654(3) . ?
V3 O23 1.793(3) . ?
V3 O34 1.805(3) . ?
V4 O4 1.632(3) . ?
V4 O4M 1.639(3) . ?
V4 O34 1.821(3) . ?
V4 O45 1.827(3) . ?
V5 O5M 1.641(3) . ?
V5 O5 1.653(3) . ?
V5 O56 1.797(3) . ?
V5 O45 1.803(3) . ?
V6 O6M 1.647(3) . ?
V6 O61 1.648(3) . ?
V6 O6 1.782(3) . ?
V6 O56 1.819(3) . ?
V7 O7 1.636(3) . ?
V7 O7M 1.637(3) . ?
V7 O712 1.822(3) . ?
V7 O78 1.825(3) . ?
V8 O8M 1.637(3) . ?
V8 O8 1.652(3) . ?
V8 O89 1.799(3) . ?
V8 O78 1.801(3) . ?
V9 O9M 1.644(3) . ?
V9 O9 1.647(3) . ?
V9 O910 1.782(3) . ?
V9 O89 1.795(3) . ?
V10 O10 1.640(3) . ?
V10 O10M 1.648(3) . ?
V10 O910 1.787(3) . ?
V10 O101 1.802(3) . ?
V11 O11M 1.632(3) . ?
V11 O11 1.653(3) . ?
V11 O112 1.797(3) . ?
V11 O101 1.808(3) . ?
V12 O12M 1.633(3) . ?
V12 O127 1.654(3) . ?
V12 O112 1.798(3) . ?
V12 O712 1.799(3) 1_455 ?
Cu1A N11A 2.007(4) . ?
Cu1A N4A 2.009(3) . ?
Cu1A N1A 2.022(4) . ?
Cu1A N8A 2.024(4) . ?
Cu1A O5M 2.431(3) . ?
Cu1B N11B 1.994(4) . ?
Cu1B N1B 2.012(4) . ?
Cu1B N4B 2.016(4) . ?
Cu1B N8B 2.030(4) . ?
Cu1B O4M 2.335(3) . ?
Cu1C N8C 2.016(4) . ?
Cu1C N4C 2.019(4) . ?
Cu1C N11C 2.019(4) . ?
Cu1C N1C 2.021(3) . ?
Cu1D N11D 2.010(4) . ?
Cu1D N8D 2.014(4) . ?
Cu1D N1D 2.015(4) . ?
Cu1D N4D 2.016(4) . ?
Cu1D O8M 2.410(3) . ?
Cu1E N4E 2.011(4) . ?
Cu1E N11E 2.014(4) . ?
Cu1E N1E 2.022(4) . ?
Cu1E N8E 2.023(4) . ?
Cu1F N1F 2.012(4) . ?
Cu1F N8F 2.018(4) . ?
Cu1F N11F 2.027(4) . ?
Cu1F N4F 2.029(4) . ?
Cu1F O3M 2.399(3) . ?
O6 V1 1.811(3) 1_655 ?
O712 V12 1.799(3) 1_655 ?
N4A C5A 1.478(6) . ?
N4A C3A 1.481(6) . ?
N11F C12F 1.473(5) . ?
N11F C10F 1.486(5) . ?
N11B C12B 1.452(6) . ?
N11B C10B 1.480(6) . ?
N4B C5B 1.457(6) . ?
N4B C3B 1.488(6) . ?
N8F C9F 1.483(6) . ?
N8F C7F 1.483(5) . ?
N4F C3F 1.484(6) . ?
N4F C5F 1.484(6) . ?
N8B C9B 1.455(6) . ?
N8B C7B 1.475(6) . ?
N8A C9A 1.481(6) . ?
N8A C7A 1.482(5) . ?
N1A C2A 1.475(6) . ?
N1A C14A 1.484(5) . ?
N1F C14F 1.475(5) . ?
N1F C2F 1.480(6) . ?
N11A C12A 1.477(6) . ?
N11A C10A 1.478(6) . ?
N1B C2B 1.450(7) . ?
N1B C14B 1.513(7) . ?
C13A C12A 1.508(7) . ?
C13A C14A 1.520(7) . ?
C6F C5F 1.514(7) . ?
C6F C7F 1.519(7) . ?
C9A C10A 1.511(6) . ?
C5A C6A 1.504(7) . ?
C7B C6B 1.498(8) . ?
C10F C9F 1.505(6) . ?
C13F C12F 1.517(6) . ?
C13F C14F 1.524(6) . ?
C2F C3F 1.498(6) . ?
C3A C2A 1.492(6) . ?
C7A C6A 1.512(7) . ?
C13B C12B 1.502(8) . ?
C13B C14B 1.505(8) . ?
C5B C6B 1.505(8) . ?
C9B C10B 1.513(7) . ?
C3B C2B 1.476(8) . ?
N8D C9D 1.468(6) . ?
N8D C7D 1.484(6) . ?
N11D C12D 1.464(6) . ?
N11D C10D 1.482(6) . ?
N4D C5D 1.470(6) . ?
N4D C3D 1.478(6) . ?
N1D C2D 1.472(6) . ?
N1D C14D 1.487(6) . ?
C2D C3D 1.506(7) . ?
C6D C7D 1.515(7) . ?
C6D C5D 1.515(7) . ?
C10D C9D 1.496(7) . ?
C14D C13D 1.514(7) . ?
C12D C13D 1.504(7) . ?
N1E C2E 1.471(6) . ?
N1E C14E 1.485(6) . ?
N4E C3E 1.475(6) . ?
N4E C5E 1.479(6) . ?
N11E C10E 1.472(6) . ?
N11E C12E 1.476(6) . ?
N8E C9E 1.477(6) . ?
N8E C7E 1.482(6) . ?
C3E C2E 1.506(7) . ?
C6E C7E 1.494(8) . ?
C6E C5E 1.524(7) . ?
C12E C13E 1.505(7) . ?
C14E C13E 1.517(7) . ?
C10E C9E 1.490(7) . ?
N1C C2C 1.469(6) . ?
N1C C14C 1.479(5) . ?
N8C C7C 1.474(6) . ?
N8C C9C 1.484(6) . ?
N4C C5C 1.475(5) . ?
N4C C3C 1.484(5) . ?
N11C C12C 1.485(5) . ?
N11C C10C 1.488(6) . ?
C7C C6C 1.515(6) . ?
C14C C13C 1.505(6) . ?
C2C C3C 1.505(6) . ?
C10C C9C 1.503(6) . ?
C6C C5C 1.521(6) . ?
C13C C12C 1.506(7) . ?
O5W O6W 1.390(19) . ?
O12W O13W 0.834(9) . ?
O27W O28W 0.876(13) . ?
O33W O34W 1.087(18) . ?

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
O1M V1 O1 107.11(16) . . ?
O1M V1 O12 108.00(15) . . ?
O1 V1 O12 109.91(15) . . ?
O1M V1 O6 111.03(15) . 1_455 ?
O1 V1 O6 109.87(15) . 1_455 ?
O12 V1 O6 110.85(14) . 1_455 ?
O2 V2 O2M 108.10(15) . . ?
O2 V2 O12 113.03(15) . . ?
O2M V2 O12 109.95(14) . . ?
O2 V2 O23 107.98(14) . . ?
O2M V2 O23 110.27(14) . . ?
O12 V2 O23 107.49(14) . . ?
O3M V3 O3 107.28(15) . . ?
O3M V3 O23 109.32(15) . . ?
O3 V3 O23 109.82(15) . . ?
O3M V3 O34 111.26(14) . . ?
O3 V3 O34 109.95(14) . . ?
O23 V3 O34 109.18(14) . . ?
O4 V4 O4M 108.91(16) . . ?
O4 V4 O34 110.31(14) . . ?
O4M V4 O34 108.63(14) . . ?
O4 V4 O45 108.94(15) . . ?
O4M V4 O45 108.98(14) . . ?
O34 V4 O45 111.04(13) . . ?
O5M V5 O5 107.81(15) . . ?
O5M V5 O56 109.88(15) . . ?
O5 V5 O56 110.41(14) . . ?
O5M V5 O45 108.27(14) . . ?
O5 V5 O45 111.76(15) . . ?
O56 V5 O45 108.67(13) . . ?
O6M V6 O61 108.25(16) . . ?
O6M V6 O6 112.44(15) . . ?
O61 V6 O6 109.61(14) . . ?
O6M V6 O56 106.46(14) . . ?
O61 V6 O56 106.69(14) . . ?
O6 V6 O56 113.11(14) . . ?
O7 V7 O7M 108.72(16) . . ?
O7 V7 O712 109.92(14) . . ?
O7M V7 O712 109.76(15) . . ?
O7 V7 O78 110.40(15) . . ?
O7M V7 O78 109.15(14) . . ?
O712 V7 O78 108.87(14) . . ?
O8M V8 O8 108.08(15) . . ?
O8M V8 O89 110.33(15) . . ?
O8 V8 O89 108.08(16) . . ?
O8M V8 O78 108.58(14) . . ?
O8 V8 O78 113.90(15) . . ?
O89 V8 O78 107.86(14) . . ?
O9M V9 O9 108.74(15) . . ?
O9M V9 O910 110.16(15) . . ?
O9 V9 O910 109.13(15) . . ?
O9M V9 O89 106.77(15) . . ?
O9 V9 O89 108.81(15) . . ?
O910 V9 O89 113.12(15) . . ?
O10 V10 O10M 107.77(15) . . ?
O10 V10 O910 108.48(15) . . ?
O10M V10 O910 109.05(15) . . ?
O10 V10 O101 110.66(15) . . ?
O10M V10 O101 109.53(15) . . ?
O910 V10 O101 111.26(14) . . ?
O11M V11 O11 108.49(16) . . ?
O11M V11 O112 109.26(16) . . ?
O11 V11 O112 108.64(15) . . ?
O11M V11 O101 110.17(15) . . ?
O11 V11 O101 112.27(15) . . ?
O112 V11 O101 107.97(15) . . ?
O12M V12 O127 106.80(16) . . ?
O12M V12 O112 109.70(16) . . ?
O127 V12 O112 109.56(16) . . ?
O12M V12 O712 112.36(15) . 1_455 ?
O127 V12 O712 110.80(15) . 1_455 ?
O112 V12 O712 107.61(14) . 1_455 ?
N11A Cu1A N4A 179.19(15) . . ?
N11A Cu1A N1A 94.51(15) . . ?
N4A Cu1A N1A 85.44(15) . . ?
N11A Cu1A N8A 86.14(15) . . ?
N4A Cu1A N8A 93.91(15) . . ?
N1A Cu1A N8A 179.32(15) . . ?
N11A Cu1A O5M 91.83(12) . . ?
N4A Cu1A O5M 88.97(12) . . ?
N1A Cu1A O5M 95.52(12) . . ?
N8A Cu1A O5M 84.25(12) . . ?
N11B Cu1B N1B 94.31(18) . . ?
N11B Cu1B N4B 175.90(16) . . ?
N1B Cu1B N4B 86.11(18) . . ?
N11B Cu1B N8B 86.14(17) . . ?
N1B Cu1B N8B 176.35(17) . . ?
N4B Cu1B N8B 93.19(17) . . ?
N11B Cu1B O4M 96.05(14) . . ?
N1B Cu1B O4M 88.03(14) . . ?
N4B Cu1B O4M 88.04(14) . . ?
N8B Cu1B O4M 95.53(14) . . ?
N8C Cu1C N4C 95.17(14) . . ?
N8C Cu1C N11C 85.93(15) . . ?
N4C Cu1C N11C 175.13(15) . . ?
N8C Cu1C N1C 178.58(15) . . ?
N4C Cu1C N1C 86.24(14) . . ?
N11C Cu1C N1C 92.65(15) . . ?
N11D Cu1D N8D 85.19(16) . . ?
N11D Cu1D N1D 94.45(16) . . ?
N8D Cu1D N1D 179.63(17) . . ?
N11D Cu1D N4D 178.18(15) . . ?
N8D Cu1D N4D 94.33(16) . . ?
N1D Cu1D N4D 86.03(16) . . ?
N11D Cu1D O8M 88.70(13) . . ?
N8D Cu1D O8M 91.93(13) . . ?
N1D Cu1D O8M 88.16(13) . . ?
N4D Cu1D O8M 93.07(13) . . ?
N4E Cu1E N11E 178.32(16) . . ?
N4E Cu1E N1E 85.90(15) . . ?
N11E Cu1E N1E 93.29(16) . . ?
N4E Cu1E N8E 94.43(16) . . ?
N11E Cu1E N8E 86.37(16) . . ?
N1E Cu1E N8E 179.66(17) . . ?
N1F Cu1F N8F 177.83(15) . . ?
N1F Cu1F N11F 94.65(15) . . ?
N8F Cu1F N11F 86.23(14) . . ?
N1F Cu1F N4F 85.84(15) . . ?
N8F Cu1F N4F 93.16(15) . . ?
N11F Cu1F N4F 176.34(14) . . ?
N1F Cu1F O3M 96.42(13) . . ?
N8F Cu1F O3M 85.59(13) . . ?
N11F Cu1F O3M 87.22(12) . . ?
N4F Cu1F O3M 96.35(13) . . ?
V6 O6 V1 160.2(2) . 1_655 ?
V2 O12 V1 133.92(17) . . ?
V3 O3M Cu1F 130.91(16) . . ?
V4 O4M Cu1B 169.74(18) . . ?
V5 O5M Cu1A 139.11(16) . . ?
V8 O8M Cu1D 137.19(16) . . ?
V3 O23 V2 134.07(18) . . ?
V3 O34 V4 137.98(17) . . ?
V5 O45 V4 129.17(17) . . ?
V5 O56 V6 138.96(17) . . ?
V8 O78 V7 127.67(17) . . ?
V9 O89 V8 139.52(18) . . ?
V10 O101 V11 141.22(19) . . ?
V11 O112 V12 135.27(18) . . ?
V12 O712 V7 138.25(18) 1_655 . ?
V9 O910 V10 174.1(2) . . ?
C5A N4A C3A 113.0(3) . . ?
C5A N4A Cu1A 116.0(3) . . ?
C3A N4A Cu1A 106.7(3) . . ?
C12F N11F C10F 112.0(3) . . ?
C12F N11F Cu1F 118.2(3) . . ?
C10F N11F Cu1F 105.2(3) . . ?
C12B N11B C10B 113.5(4) . . ?
C12B N11B Cu1B 115.3(3) . . ?
C10B N11B Cu1B 107.6(3) . . ?
C5B N4B C3B 112.8(4) . . ?
C5B N4B Cu1B 119.1(3) . . ?
C3B N4B Cu1B 105.9(3) . . ?
C9F N8F C7F 112.9(4) . . ?
C9F N8F Cu1F 106.7(3) . . ?
C7F N8F Cu1F 116.5(3) . . ?
C3F N4F C5F 112.5(3) . . ?
C3F N4F Cu1F 106.4(3) . . ?
C5F N4F Cu1F 117.2(3) . . ?
C9B N8B C7B 111.4(4) . . ?
C9B N8B Cu1B 106.8(3) . . ?
C7B N8B Cu1B 120.6(3) . . ?
C9A N8A C7A 113.0(3) . . ?
C9A N8A Cu1A 106.0(3) . . ?
C7A N8A Cu1A 119.2(3) . . ?
C2A N1A C14A 113.6(4) . . ?
C2A N1A Cu1A 106.5(3) . . ?
C14A N1A Cu1A 116.9(3) . . ?
C14F N1F C2F 111.0(4) . . ?
C14F N1F Cu1F 117.9(3) . . ?
C2F N1F Cu1F 107.2(3) . . ?
C12A N11A C10A 112.0(3) . . ?
C12A N11A Cu1A 118.2(3) . . ?
C10A N11A Cu1A 106.0(3) . . ?
C2B N1B C14B 112.7(4) . . ?
C2B N1B Cu1B 106.2(3) . . ?
C14B N1B Cu1B 115.4(3) . . ?
C12A C13A C14A 114.0(4) . . ?
C5F C6F C7F 114.6(4) . . ?
N8F C7F C6F 111.3(4) . . ?
N8A C9A C10A 107.4(4) . . ?
N11A C10A C9A 106.9(4) . . ?
N4A C5A C6A 112.6(4) . . ?
N8B C7B C6B 114.6(4) . . ?
N11F C10F C9F 108.3(3) . . ?
C12F C13F C14F 114.6(4) . . ?
N1F C2F C3F 108.2(4) . . ?
N4A C3A C2A 107.3(4) . . ?
N8A C7A C6A 110.7(4) . . ?
N1A C14A C13A 110.9(4) . . ?
N4F C3F C2F 108.4(4) . . ?
N1F C14F C13F 112.6(4) . . ?
C12B C13B C14B 117.3(5) . . ?
C5A C6A C7A 114.1(4) . . ?
C13B C14B N1B 113.9(4) . . ?
N4B C5B C6B 111.0(4) . . ?
N11A C12A C13A 112.5(4) . . ?
N8F C9F C10F 107.2(4) . . ?
N11F C12F C13F 112.2(3) . . ?
N8B C9B C10B 108.0(4) . . ?
N1A C2A C3A 107.6(4) . . ?
N11B C10B C9B 109.9(4) . . ?
C2B C3B N4B 108.8(4) . . ?
N1B C2B C3B 109.2(4) . . ?
C7B C6B C5B 115.4(5) . . ?
N11B C12B C13B 112.7(5) . . ?
N4F C5F C6F 112.3(4) . . ?
C9D N8D C7D 112.7(4) . . ?
C9D N8D Cu1D 107.0(3) . . ?
C7D N8D Cu1D 115.5(3) . . ?
C12D N11D C10D 112.4(4) . . ?
C12D N11D Cu1D 117.8(3) . . ?
C10D N11D Cu1D 107.1(3) . . ?
C5D N4D C3D 111.8(4) . . ?
C5D N4D Cu1D 118.8(3) . . ?
C3D N4D Cu1D 106.3(3) . . ?
C2D N1D C14D 112.6(4) . . ?
C2D N1D Cu1D 106.4(3) . . ?
C14D N1D Cu1D 117.5(3) . . ?
N1D C2D C3D 108.4(4) . . ?
C7D C6D C5D 114.3(4) . . ?
N8D C7D C6D 111.2(4) . . ?
N11D C10D C9D 107.1(4) . . ?
N1D C14D C13D 111.8(4) . . ?
N11D C12D C13D 112.7(4) . . ?
N4D C3D C2D 107.2(4) . . ?
N8D C9D C10D 107.5(4) . . ?
N4D C5D C6D 112.1(4) . . ?
C12D C13D C14D 115.3(4) . . ?
C2E N1E C14E 112.0(4) . . ?
C2E N1E Cu1E 106.8(3) . . ?
C14E N1E Cu1E 115.8(3) . . ?
C3E N4E C5E 112.0(4) . . ?
C3E N4E Cu1E 106.8(3) . . ?
C5E N4E Cu1E 117.4(3) . . ?
C10E N11E C12E 112.9(4) . . ?
C10E N11E Cu1E 106.3(3) . . ?
C12E N11E Cu1E 117.4(3) . . ?
C9E N8E C7E 111.9(4) . . ?
C9E N8E Cu1E 105.7(3) . . ?
C7E N8E Cu1E 117.1(3) . . ?
N4E C3E C2E 108.1(4) . . ?
C7E C6E C5E 114.3(4) . . ?
N8E C7E C6E 112.4(4) . . ?
N4E C5E C6E 111.1(4) . . ?
N11E C12E C13E 113.3(4) . . ?
N1E C14E C13E 112.2(4) . . ?
N1E C2E C3E 108.3(4) . . ?
C12E C13E C14E 114.2(4) . . ?
N11E C10E C9E 109.5(4) . . ?
N8E C9E C10E 108.2(4) . . ?
C2C N1C C14C 114.4(3) . . ?
C2C N1C Cu1C 106.8(3) . . ?
C14C N1C Cu1C 115.1(3) . . ?
C7C N8C C9C 111.4(4) . . ?
C7C N8C Cu1C 119.1(3) . . ?
C9C N8C Cu1C 106.3(3) . . ?
C5C N4C C3C 112.6(3) . . ?
C5C N4C Cu1C 117.8(3) . . ?
C3C N4C Cu1C 104.5(3) . . ?
C12C N11C C10C 111.7(3) . . ?
C12C N11C Cu1C 116.4(3) . . ?
C10C N11C Cu1C 107.8(3) . . ?
N8C C7C C6C 113.5(4) . . ?
N1C C14C C13C 111.4(4) . . ?
N1C C2C C3C 107.8(4) . . ?
N11C C10C C9C 108.2(4) . . ?
N8C C9C C10C 108.5(4) . . ?
N4C C3C C2C 107.5(3) . . ?
C7C C6C C5C 113.6(4) . . ?
C14C C13C C12C 115.4(4) . . ?
N4C C5C C6C 111.2(3) . . ?
N11C C12C C13C 113.0(4) . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
_chemical_properties_physical    Heat-sensitive
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1404577'
_audit_update_record             
;
2015-07-14 deposited with the CCDC.
2015-07-23 downloaded from the CCDC.
;
#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C10 H30 Cu N4 O9 V2'
_chemical_formula_sum            'C10 H30 Cu N4 O9 V2'
_chemical_formula_weight         515.8
_chemical_compound_source        'synthesis as described'


#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.0199(2)
_cell_length_b                   13.9524(6)
_cell_length_c                   14.2588(5)
_cell_angle_alpha                102.032(3)
_cell_angle_beta                 101.742(3)
_cell_angle_gamma                97.560(3)
_cell_volume                     1502.39(10)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5724
_cell_measurement_theta_min      2.372
_cell_measurement_theta_max      28.087

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.1213
_exptl_crystal_size_mid          0.1012
_exptl_crystal_size_min          0.0602
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.71
_exptl_crystal_F_000             795
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3 -17 13 0.043
-2 -15 16 0.0435
5 12 -16 0.046
0 -4 -17 0.0293
-2 -12 -11 0.0279
-11 8 4 0.0439
11 -8 -4 0.0568
1 11 12 0.0299


#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    2.014
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
        (compiled May 22 2014,16:03:01)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (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_correction_T_min  0.958
_exptl_absorpt_correction_T_max  0.975

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_detector_area_resol_mean 16.2439
_diffrn_orient_matrix_ub_11      0.0897824
_diffrn_orient_matrix_ub_12      0.0108259
_diffrn_orient_matrix_ub_13      0.0229175
_diffrn_orient_matrix_ub_21      -0.0134114
_diffrn_orient_matrix_ub_22      0.040479
_diffrn_orient_matrix_ub_23      0.0352752
_diffrn_orient_matrix_ub_31      -0.0140622
_diffrn_orient_matrix_ub_32      -0.0322228
_diffrn_orient_matrix_ub_33      0.0311928
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_number            9271
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.86
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_reflns_number_total             5290
_reflns_number_gt                4751
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
        (compiled May 22 2014,16:03:01)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
        (compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
        (compiled May 22 2014,16:03:01)
;
_computing_structure_solution    'OLEX2 (Dolomanov, 2009)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0366P)²+1.8005P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5290
_refine_ls_number_parameters     406
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0292
_refine_ls_wR_factor_ref         0.0776
_refine_ls_wR_factor_gt          0.0743
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.001
_refine_diff_density_max         0.837
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.077

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'

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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.85344(5) 0.72421(3) 0.14391(3) 0.01114(11) Uani 1 d . .
V2 V 0.25620(5) 0.84299(3) 0.13405(3) 0.00902(11) Uani 1 d . .
V3 V 0.61300(6) 0.82388(3) 0.28768(3) 0.01096(11) Uani 1 d . .
Cu1A Cu 0.5 1 0.5 0.01304(11) Uani 1 d . .
Cu1B Cu 0.5 0.5 0 0.01923(13) Uani 1 d . .
Cu1C Cu 0.5 1 0 0.01098(11) Uani 1 d . .
O1 O 0.9037(2) 0.64355(14) 0.21019(15) 0.0196(4) Uani 1 d . .
O12 O 1.0385(2) 0.77404(14) 0.10424(14) 0.0155(4) Uani 1 d . .
O13 O 0.7731(2) 0.82430(14) 0.21506(14) 0.0155(4) Uani 1 d . .
O2 O 0.2657(2) 0.95636(13) 0.19976(13) 0.0144(4) Uani 1 d . .
O23 O 0.4015(2) 0.78064(14) 0.20437(13) 0.0154(4) Uani 1 d . .
O3 O 0.6394(3) 0.74897(15) 0.36307(14) 0.0186(4) Uani 1 d . .
O1M O 0.6978(2) 0.66479(14) 0.04725(14) 0.0184(4) Uani 1 d . .
O2M O 0.3220(2) 0.85389(14) 0.03435(13) 0.0170(4) Uani 1 d . .
O3M O 0.6224(2) 0.93682(14) 0.35407(13) 0.0157(4) Uani 1 d . .
N4A N 0.2719(3) 0.9865(2) 0.40576(18) 0.0272(6) Uani 1 d . .
H4A H 0.2861 0.9554 0.3403 0.033 Uiso 1 calc . .
N1A N 0.4589(4) 0.85758(19) 0.51289(18) 0.0302(7) Uani 1 d . .
H1A H 0.4866 0.8168 0.4553 0.036 Uiso 1 calc . .
C5A C 0.1225(4) 0.9234(4) 0.4217(3) 0.0563(14) Uani 1 d . .
H5AA H 0.0212 0.9204 0.3699 0.068 Uiso 1 calc . .
H5AB H 0.0992 0.954 0.4842 0.068 Uiso 1 calc . .
C2A C 0.5908(7) 0.8526(3) 0.5998(3) 0.0506(12) Uani 1 d . .
H2AA H 0.6027 0.7839 0.5977 0.061 Uiso 1 calc . .
H2AB H 0.5571 0.8798 0.66 0.061 Uiso 1 calc . .
C6A C 0.1507(6) 0.8204(4) 0.4224(3) 0.0636(16) Uani 1 d . .
H6AA H 0.1899 0.7934 0.3641 0.076 Uiso 1 calc . .
H6AB H 0.041 0.7793 0.4188 0.076 Uiso 1 calc . .
C3A C 0.2434(6) 1.0885(3) 0.4028(3) 0.0509(12) Uani 1 d . .
H3AA H 0.2057 1.1185 0.4608 0.061 Uiso 1 calc . .
H3AB H 0.1547 1.0866 0.3447 0.061 Uiso 1 calc . .
C7A C 0.2821(6) 0.8140(3) 0.5135(3) 0.0599(14) Uani 1 d . .
H7AA H 0.2521 0.8489 0.5723 0.072 Uiso 1 calc . .
H7AB H 0.2776 0.7447 0.5157 0.072 Uiso 1 calc . .
N4B N 0.3326(3) 0.56868(18) 0.06561(19) 0.0218(6) Uani 1 d . .
H4B H 0.3927 0.6368 0.0992 0.026 Uiso 1 calc . .
N1B N 0.3765(3) 0.53140(18) -0.12491(19) 0.0211(5) Uani 1 d . .
H1B H 0.2949 0.4706 -0.1629 0.025 Uiso 1 calc . .
C2B C 0.2707(4) 0.6059(2) -0.0948(2) 0.0255(7) Uani 1 d . .
H2BA H 0.1805 0.6077 -0.1509 0.031 Uiso 1 calc . .
H2BB H 0.3425 0.6716 -0.0697 0.031 Uiso 1 calc . .
C3B C 0.1915(4) 0.5762(2) -0.0157(2) 0.0242(7) Uani 1 d . .
H3BA H 0.1259 0.6256 0.0085 0.029 Uiso 1 calc . .
H3BB H 0.1134 0.5125 -0.0423 0.029 Uiso 1 calc . .
C5B C 0.2664(4) 0.5248(2) 0.1404(2) 0.0274(7) Uani 1 d . .
H5BA H 0.1981 0.459 0.1085 0.033 Uiso 1 calc . .
H5BB H 0.1911 0.5659 0.1678 0.033 Uiso 1 calc . .
C6B C 0.4109(4) 0.5165(2) 0.2231(2) 0.0292(7) Uani 1 d . .
H6BA H 0.3613 0.4998 0.2756 0.035 Uiso 1 calc . .
H6BB H 0.4866 0.581 0.2497 0.035 Uiso 1 calc . .
C7B C 0.4815(4) 0.5609(2) -0.1920(3) 0.0281(7) Uani 1 d . .
H7BA H 0.5579 0.624 -0.1591 0.034 Uiso 1 calc . .
H7BB H 0.4052 0.5701 -0.2503 0.034 Uiso 1 calc . .
N4C N 0.7211(3) 0.96138(17) 0.06585(16) 0.0131(5) Uani 1 d . .
H4C H 0.6883 0.91 0.0996 0.016 Uiso 1 calc . .
N1C N 0.5163(3) 0.90645(16) -0.12493(16) 0.0123(5) Uani 1 d . .
H1C H 0.5646 0.9476 -0.1644 0.015 Uiso 1 calc . .
C5C C 0.8527(3) 1.0412(2) 0.1395(2) 0.0171(6) Uani 1 d . .
H5CA H 0.8967 1.0897 0.1065 0.021 Uiso 1 calc . .
H5CB H 0.949 1.0123 0.1675 0.021 Uiso 1 calc . .
C2C C 0.6466(3) 0.8460(2) -0.0948(2) 0.0155(6) Uani 1 d . .
H2CA H 0.6888 0.8161 -0.151 0.019 Uiso 1 calc . .
H2CB H 0.5952 0.7931 -0.0693 0.019 Uiso 1 calc . .
C3C C 0.7937(3) 0.9136(2) -0.0160(2) 0.0156(6) Uani 1 d . .
H3CA H 0.8788 0.8754 0.0078 0.019 Uiso 1 calc . .
H3CB H 0.8501 0.964 -0.0427 0.019 Uiso 1 calc . .
C6C C 0.7798(4) 1.0935(2) 0.2218(2) 0.0172(6) Uani 1 d . .
H6CA H 0.8745 1.1363 0.2731 0.021 Uiso 1 calc . .
H6CB H 0.7258 1.0438 0.2502 0.021 Uiso 1 calc . .
C7C C 0.6475(4) 1.1559(2) 0.1889(2) 0.0159(6) Uani 1 d . .
H7CA H 0.623 1.1967 0.2467 0.019 Uiso 1 calc . .
H7CB H 0.696 1.2002 0.1532 0.019 Uiso 1 calc . .
O1W O 0.8133(8) 0.6317(4) 0.4665(4) 0.0663(14) Uani 0.7 d . .
O2W O 0.657(3) 0.6190(8) 0.4828(9) 0.103(6) Uani 0.3 d . .
O3W O 0.3864(14) 0.6296(8) 0.4346(8) 0.045(3) Uani 0.25 d . .
O4W O 0.382(4) 0.555(2) 0.503(3) 0.181(15) Uani 0.25 d . .
O5W O 0.2499(13) 0.5541(6) 0.5134(7) 0.096(3) Uani 0.5 d . .
O6W O 1.0454(9) 0.6415(5) 0.6353(6) 0.121(2) Uani 0.75 d . .
O7W O 0.877(4) 0.6804(11) 0.6909(12) 0.179(15) Uani 0.25 d . .
O8W O 0.926(3) 0.7206(13) 0.861(2) 0.109(8) Uani 0.2 d . .
O9W O 0.565(4) 0.558(2) 0.5598(14) 0.197(12) Uani 0.3 d . .
O10W O 1.0191(6) 0.5478(3) 0.3532(3) 0.1016(15) Uani 1 d . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
V1 O1M 1.6422(19) . ?
V1 O1 1.6522(19) . ?
V1 O12 1.7998(18) . ?
V1 O13 1.8185(19) . ?
V2 O2M 1.6424(18) . ?
V2 O2 1.6452(18) . ?
V2 O12 1.8003(18) 1_455 ?
V2 O23 1.8096(18) . ?
V3 O3M 1.6440(19) . ?
V3 O3 1.6512(19) . ?
V3 O13 1.8061(19) . ?
V3 O23 1.8067(18) . ?
Cu1A N4A 1.998(2) . ?
Cu1A N4A 1.998(2) 2_676 ?
Cu1A N1A 2.024(3) . ?
Cu1A N1A 2.024(3) 2_676 ?
Cu1B N1B 2.017(3) 2_665 ?
Cu1B N1B 2.017(3) . ?
Cu1B N4B 2.018(2) . ?
Cu1B N4B 2.018(2) 2_665 ?
Cu1C N1C 2.016(2) . ?
Cu1C N1C 2.016(2) 2_675 ?
Cu1C N4C 2.025(2) . ?
Cu1C N4C 2.025(2) 2_675 ?
O12 V2 1.8003(18) 1_655 ?
N4A C5A 1.476(5) . ?
N4A C3A 1.479(5) . ?
N1A C7A 1.470(5) . ?
N1A C2A 1.476(5) . ?
C5A C6A 1.486(7) . ?
C2A C3A 1.480(6) 2_676 ?
C6A C7A 1.523(7) . ?
C3A C2A 1.480(6) 2_676 ?
N4B C3B 1.478(4) . ?
N4B C5B 1.488(4) . ?
N1B C2B 1.477(4) . ?
N1B C7B 1.481(4) . ?
C2B C3B 1.505(4) . ?
C5B C6B 1.511(5) . ?
C6B C7B 1.520(5) 2_665 ?
C7B C6B 1.520(5) 2_665 ?
N4C C3C 1.484(3) . ?
N4C C5C 1.486(3) . ?
N1C C2C 1.479(3) . ?
N1C C7C 1.482(3) 2_675 ?
C5C C6C 1.512(4) . ?
C2C C3C 1.506(4) . ?
C6C C7C 1.522(4) . ?
C7C N1C 1.482(3) 2_675 ?
O1W O2W 1.32(2) . ?
O2W O9W 1.74(3) . ?
O3W O4W 1.57(3) . ?
O4W O5W 1.10(3) . ?
O4W O9W 1.51(3) . ?
O4W O9W 1.79(4) 2_666 ?
O6W O7W 1.79(3) . ?
O9W O4W 1.79(4) 2_666 ?

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
O1M V1 O1 107.60(10) . . ?
O1M V1 O12 109.75(9) . . ?
O1 V1 O12 110.58(9) . . ?
O1M V1 O13 108.32(9) . . ?
O1 V1 O13 110.21(9) . . ?
O12 V1 O13 110.31(9) . . ?
O2M V2 O2 107.26(9) . . ?
O2M V2 O12 111.70(9) . 1_455 ?
O2 V2 O12 110.00(9) . 1_455 ?
O2M V2 O23 108.95(9) . . ?
O2 V2 O23 109.21(9) . . ?
O12 V2 O23 109.66(8) 1_455 . ?
O3M V3 O3 108.27(10) . . ?
O3M V3 O13 110.36(9) . . ?
O3 V3 O13 112.36(9) . . ?
O3M V3 O23 109.50(9) . . ?
O3 V3 O23 108.02(9) . . ?
O13 V3 O23 108.28(9) . . ?
N4A Cu1A N4A 180 . 2_676 ?
N4A Cu1A N1A 94.64(12) . . ?
N4A Cu1A N1A 85.36(12) 2_676 . ?
N4A Cu1A N1A 85.36(12) . 2_676 ?
N4A Cu1A N1A 94.64(12) 2_676 2_676 ?
N1A Cu1A N1A 180 . 2_676 ?
N1B Cu1B N1B 180 2_665 . ?
N1B Cu1B N4B 93.63(10) 2_665 . ?
N1B Cu1B N4B 86.37(10) . . ?
N1B Cu1B N4B 86.37(10) 2_665 2_665 ?
N1B Cu1B N4B 93.63(10) . 2_665 ?
N4B Cu1B N4B 180 . 2_665 ?
N1C Cu1C N1C 180 . 2_675 ?
N1C Cu1C N4C 86.49(9) . . ?
N1C Cu1C N4C 93.51(9) 2_675 . ?
N1C Cu1C N4C 93.50(9) . 2_675 ?
N1C Cu1C N4C 86.50(9) 2_675 2_675 ?
N4C Cu1C N4C 180 . 2_675 ?
V1 O12 V2 149.66(12) . 1_655 ?
V3 O13 V1 132.19(11) . . ?
V3 O23 V2 132.44(11) . . ?
C5A N4A C3A 113.3(3) . . ?
C5A N4A Cu1A 116.8(2) . . ?
C3A N4A Cu1A 106.9(2) . . ?
C7A N1A C2A 113.4(3) . . ?
C7A N1A Cu1A 117.2(3) . . ?
C2A N1A Cu1A 106.5(2) . . ?
N4A C5A C6A 113.0(3) . . ?
N1A C2A C3A 107.6(3) . 2_676 ?
C5A C6A C7A 113.7(3) . . ?
N4A C3A C2A 107.9(3) . 2_676 ?
N1A C7A C6A 111.6(3) . . ?
C3B N4B C5B 112.3(2) . . ?
C3B N4B Cu1B 105.69(18) . . ?
C5B N4B Cu1B 117.42(19) . . ?
C2B N1B C7B 112.4(2) . . ?
C2B N1B Cu1B 106.43(19) . . ?
C7B N1B Cu1B 118.12(19) . . ?
N1B C2B C3B 107.7(2) . . ?
N4B C3B C2B 108.4(2) . . ?
N4B C5B C6B 112.2(2) . . ?
C5B C6B C7B 113.9(3) . 2_665 ?
N1B C7B C6B 112.1(3) . 2_665 ?
C3C N4C C5C 111.4(2) . . ?
C3C N4C Cu1C 105.48(16) . . ?
C5C N4C Cu1C 117.55(17) . . ?
C2C N1C C7C 112.3(2) . 2_675 ?
C2C N1C Cu1C 106.28(16) . . ?
C7C N1C Cu1C 116.98(17) 2_675 . ?
N4C C5C C6C 112.3(2) . . ?
N1C C2C C3C 108.1(2) . . ?
N4C C3C C2C 107.9(2) . . ?
C5C C6C C7C 113.9(2) . . ?
N1C C7C C6C 112.2(2) 2_675 . ?
O1W O2W O9W 133.3(12) . . ?
O5W O4W O9W 141(3) . . ?
O5W O4W O3W 99.7(18) . . ?
O9W O4W O3W 109.0(19) . . ?
O5W O4W O9W 119(2) . 2_666 ?
O9W O4W O9W 77(2) . 2_666 ?
O3W O4W O9W 107(2) . 2_666 ?
O4W O9W O2W 93.0(15) . . ?
O4W O9W O4W 103(2) . 2_666 ?
O2W O9W O4W 88.3(15) . 2_666 ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1404578'
_audit_update_record             
;
2015-07-14 deposited with the CCDC.
2015-07-23 downloaded from the CCDC.
;
#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C10 H26.67 Cu N4 O7.33 V2'
_chemical_formula_sum            'C10 H26.67 Cu N4 O7.33 V2'
_chemical_formula_weight         485.77
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.6253(10)
_cell_length_b                   12.890(2)
_cell_length_c                   13.368(2)
_cell_angle_alpha                103.208(14)
_cell_angle_beta                 106.557(12)
_cell_angle_gamma                95.595(11)
_cell_volume                     1365.7(4)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1438
_cell_measurement_theta_min      2.479
_cell_measurement_theta_max      24.88

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#
_exptl_crystal_description       prism
_exptl_crystal_colour            pink
_exptl_crystal_density_method    'not measured'
_exptl_crystal_size_max          0.2659
_exptl_crystal_size_mid          0.0649
_exptl_crystal_size_min          0.0371
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_F_000             745
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-12 6 2 0.1202
0 -7 -14 0.0127
12 0 -2 0.1326
-12 1 3 0.1175
0 12 9 0.0421
0 -12 16 0.0129
0 14 -15 0.0235


#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    2.203
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
        (compiled May 22 2014,16:03:01)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (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_correction_T_min  0.711
_exptl_absorpt_correction_T_max  0.933

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_detector_area_resol_mean 16.2439
_diffrn_orient_matrix_ub_11      0.0429004
_diffrn_orient_matrix_ub_12      -0.0004858
_diffrn_orient_matrix_ub_13      0.0536807
_diffrn_orient_matrix_ub_21      -0.0481645
_diffrn_orient_matrix_ub_22      -0.0508663
_diffrn_orient_matrix_ub_23      -0.0080755
_diffrn_orient_matrix_ub_31      0.0585697
_diffrn_orient_matrix_ub_32      -0.0265949
_diffrn_orient_matrix_ub_33      -0.0188539
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_unetI/netI     0.1383
_diffrn_reflns_number            8860
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.65
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_reflns_number_total             4794
_reflns_number_gt                3280
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
        (compiled May 22 2014,16:03:01)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
        (compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
        (compiled May 22 2014,16:03:01)
;
_computing_structure_solution    'OLEX2 (Dolomanov, 2009)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0366P)²+9.9777P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4794
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1338
_refine_ls_R_factor_gt           0.0886
_refine_ls_wR_factor_ref         0.1828
_refine_ls_wR_factor_gt          0.1621
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_restrained_S_all      1.132
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.334
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.15

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'

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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.03494(19) 0.27302(13) 0.65599(13) 0.0217(4) Uani 1 d . .
V2 V 0.44851(19) 0.34661(13) 0.70848(14) 0.0213(4) Uani 1 d . .
V3 V 0.76858(19) 0.19969(13) 0.79161(14) 0.0234(4) Uani 1 d . .
Cu1A Cu 0.5 0.5 1 0.0275(5) Uani 1 d . .
Cu1B Cu 0 0 0.5 0.0230(4) Uani 1 d . .
Cu1C Cu 0.5 0.5 0.5 0.0277(5) Uani 1 d . .
O1 O -0.0008(8) 0.3955(5) 0.6651(6) 0.0338(18) Uani 1 d . .
O2 O 0.4990(8) 0.4655(6) 0.7972(6) 0.0360(19) Uani 1 d . .
O3 O 0.8467(8) 0.2510(6) 0.9221(6) 0.0376(19) Uani 1 d . .
O12 O 0.2569(7) 0.2765(5) 0.7117(5) 0.0229(15) Uani 1 d . .
O23 O 0.6010(8) 0.2664(6) 0.7409(7) 0.046(2) Uani 1 d . .
O13 O -0.0692(8) 0.2081(6) 0.7311(6) 0.0358(19) Uani 1 d . .
O1M O -0.0316(8) 0.2013(6) 0.5299(5) 0.0331(18) Uani 1 d . .
O2M O 0.4317(8) 0.3639(6) 0.5888(5) 0.0304(17) Uani 1 d . .
O3M O 0.6978(8) 0.0710(5) 0.7662(5) 0.0302(17) Uani 1 d . .
N1C N 0.2597(10) 0.5056(7) 0.4444(7) 0.028(2) Uani 1 d . .
H1C H 0.2497 0.5546 0.3974 0.034 Uiso 1 calc . .
N1B N 0.2297(9) 0.0371(6) 0.6073(6) 0.0234(19) Uani 1 d . .
H1B H 0.2446 0.1132 0.6471 0.028 Uiso 1 calc . .
N4C N 0.4984(9) 0.3907(7) 0.3627(7) 0.029(2) Uani 1 d . .
H4C H 0.5068 0.432 0.3107 0.035 Uiso 1 calc . .
N4B N 0.1058(9) 0.0238(6) 0.3899(6) 0.0211(18) Uani 1 d . .
H4B H 0.1158 -0.0478 0.3499 0.025 Uiso 1 calc . .
C3B C 0.2777(11) 0.0830(8) 0.4533(8) 0.025(2) Uani 1 d . .
H3BA H 0.3465 0.0772 0.4068 0.03 Uiso 1 calc . .
H3BB H 0.2769 0.159 0.4825 0.03 Uiso 1 calc . .
C2B C 0.3422(11) 0.0320(8) 0.5430(8) 0.022(2) Uani 1 d . .
H2BA H 0.3496 -0.0427 0.5135 0.026 Uiso 1 calc . .
H2BB H 0.451 0.0703 0.5883 0.026 Uiso 1 calc . .
C6C C 0.1967(13) 0.3533(9) 0.2829(8) 0.032(3) Uani 1 d . .
H6CA H 0.2106 0.4076 0.2451 0.038 Uiso 1 calc . .
H6CB H 0.1074 0.2964 0.2341 0.038 Uiso 1 calc . .
C5B C 0.0203(11) 0.0772(7) 0.3083(8) 0.021(2) Uani 1 d . .
H5BA H 0.082 0.0806 0.2584 0.025 Uiso 1 calc . .
H5BB H 0.016 0.1507 0.3444 0.025 Uiso 1 calc . .
C7B C 0.2706(12) -0.0239(8) 0.6896(8) 0.028(2) Uani 1 d . .
H7BA H 0.3812 0.0053 0.7384 0.034 Uiso 1 calc . .
H7BB H 0.2674 -0.0991 0.6541 0.034 Uiso 1 calc . .
C7C C 0.1492(11) 0.4031(8) 0.3783(9) 0.031(3) Uani 1 d . .
H7CA H 0.0378 0.4166 0.3542 0.037 Uiso 1 calc . .
H7CB H 0.1513 0.3529 0.4227 0.037 Uiso 1 calc . .
C5C C 0.3518(11) 0.3059(9) 0.3080(9) 0.031(3) Uani 1 d . .
H5CA H 0.3451 0.2585 0.3541 0.037 Uiso 1 calc . .
H5CB H 0.3618 0.2628 0.2412 0.037 Uiso 1 calc . .
C6B C -0.1512(11) 0.0176(8) 0.2459(8) 0.028(2) Uani 1 d . .
H6BA H -0.1464 -0.0579 0.2176 0.034 Uiso 1 calc . .
H6BB H -0.1938 0.0465 0.1845 0.034 Uiso 1 calc . .
C3C C 0.6521(12) 0.3475(8) 0.3915(9) 0.032(3) Uani 1 d . .
H3CA H 0.6764 0.3133 0.3264 0.038 Uiso 1 calc . .
H3CB H 0.6415 0.2937 0.4305 0.038 Uiso 1 calc . .
C2C C 0.2125(12) 0.5601(9) 0.5388(9) 0.031(3) Uani 1 d . .
H2CA H 0.1958 0.5094 0.5799 0.038 Uiso 1 calc . .
H2CB H 0.1108 0.5868 0.5144 0.038 Uiso 1 calc . .
N4A N 0.2922(9) 0.3907(7) 0.9446(7) 0.030(2) Uani 1 d . .
H4A H 0.276 0.3581 0.8678 0.036 Uiso 1 calc . .
N1A N 0.3538(9) 0.6102(7) 0.9766(7) 0.027(2) Uani 1 d . .
H1A H 0.3433 0.6445 1.0473 0.032 Uiso 1 calc . .
C5A C 0.2843(12) 0.3007(9) 0.9943(9) 0.036(3) Uani 1 d . .
H5AA H 0.1799 0.2524 0.9565 0.043 Uiso 1 calc . .
H5AB H 0.2887 0.3292 1.069 0.043 Uiso 1 calc . .
C3A C 0.1560(11) 0.4530(8) 0.9486(9) 0.031(3) Uani 1 d . .
H3AA H 0.1532 0.4762 1.0223 0.037 Uiso 1 calc . .
H3AB H 0.0512 0.4084 0.9034 0.037 Uiso 1 calc . .
C7A C 0.4100(12) 0.6984(9) 0.9346(8) 0.035(3) Uani 1 d . .
H7AA H 0.3297 0.7462 0.9275 0.042 Uiso 1 calc . .
H7AB H 0.4175 0.6678 0.8631 0.042 Uiso 1 calc . .
C2A C 0.1893(12) 0.5504(8) 0.9071(9) 0.034(3) Uani 1 d . .
H2AA H 0.1867 0.5273 0.8322 0.041 Uiso 1 calc . .
H2AB H 0.107 0.596 0.9114 0.041 Uiso 1 calc . .
C6A C 0.4234(12) 0.2363(8) 0.9917(9) 0.032(3) Uani 1 d . .
H6AA H 0.4016 0.1714 1.0141 0.038 Uiso 1 calc . .
H6AB H 0.4265 0.2142 0.918 0.038 Uiso 1 calc . .
O1W O -0.0534(10) 0.1364(6) 0.0703(6) 0.045(2) Uani 1 d . .
O2W O 0.2423(10) 0.0532(6) 0.0853(7) 0.048(2) Uani 1 d . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
V1 O1 1.622(7) . ?
V1 O1M 1.630(7) . ?
V1 O13 1.807(7) . ?
V1 O12 1.838(6) . ?
V2 O2M 1.634(7) . ?
V2 O2 1.640(7) . ?
V2 O23 1.770(7) . ?
V2 O12 1.821(6) . ?
V3 O3 1.628(7) . ?
V3 O3M 1.633(7) . ?
V3 O23 1.799(7) . ?
V3 O13 1.811(7) 1_655 ?
Cu1A N4A 2.005(8) . ?
Cu1A N4A 2.005(8) 2_667 ?
Cu1A N1A 2.009(8) . ?
Cu1A N1A 2.009(8) 2_667 ?
Cu1B N4B 2.003(8) . ?
Cu1B N4B 2.003(8) 2_556 ?
Cu1B N1B 2.023(8) 2_556 ?
Cu1B N1B 2.023(8) . ?
Cu1C N1C 2.007(8) . ?
Cu1C N1C 2.007(8) 2_666 ?
Cu1C N4C 2.038(8) 2_666 ?
Cu1C N4C 2.038(8) . ?
O13 V3 1.812(7) 1_455 ?
N1C C7C 1.476(12) . ?
N1C C2C 1.482(12) . ?
N1B C2B 1.464(11) . ?
N1B C7B 1.477(12) . ?
N4C C5C 1.472(12) . ?
N4C C3C 1.473(12) . ?
N4B C5B 1.480(11) . ?
N4B C3B 1.506(11) . ?
C3B C2B 1.494(13) . ?
C6C C7C 1.477(14) . ?
C6C C5C 1.507(13) . ?
C5B C6B 1.502(12) . ?
C7B C6B 1.518(13) 2_556 ?
C6B C7B 1.518(13) 2_556 ?
C3C C2C 1.501(14) 2_666 ?
C2C C3C 1.501(14) 2_666 ?
N4A C5A 1.467(14) . ?
N4A C3A 1.493(12) . ?
N1A C2A 1.476(12) . ?
N1A C7A 1.478(13) . ?
C5A C6A 1.528(14) . ?
C3A C2A 1.519(15) . ?
C7A C6A 1.524(13) 2_667 ?
C6A C7A 1.524(13) 2_667 ?

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 V1 O1M 110.4(4) . . ?
O1 V1 O13 110.6(4) . . ?
O1M V1 O13 107.9(4) . . ?
O1 V1 O12 109.4(3) . . ?
O1M V1 O12 109.6(3) . . ?
O13 V1 O12 108.9(3) . . ?
O2M V2 O2 108.7(4) . . ?
O2M V2 O23 109.0(4) . . ?
O2 V2 O23 110.6(4) . . ?
O2M V2 O12 111.5(3) . . ?
O2 V2 O12 109.3(3) . . ?
O23 V2 O12 107.8(3) . . ?
O3 V3 O3M 109.1(4) . . ?
O3 V3 O23 108.8(4) . . ?
O3M V3 O23 108.7(3) . . ?
O3 V3 O13 108.9(3) . 1_655 ?
O3M V3 O13 106.3(3) . 1_655 ?
O23 V3 O13 114.9(4) . 1_655 ?
N4A Cu1A N4A 180 . 2_667 ?
N4A Cu1A N1A 86.0(3) . . ?
N4A Cu1A N1A 94.0(3) 2_667 . ?
N4A Cu1A N1A 94.0(3) . 2_667 ?
N4A Cu1A N1A 86.0(3) 2_667 2_667 ?
N1A Cu1A N1A 180 . 2_667 ?
N4B Cu1B N4B 180 . 2_556 ?
N4B Cu1B N1B 93.7(3) . 2_556 ?
N4B Cu1B N1B 86.3(3) 2_556 2_556 ?
N4B Cu1B N1B 86.3(3) . . ?
N4B Cu1B N1B 93.7(3) 2_556 . ?
N1B Cu1B N1B 180 2_556 . ?
N1C Cu1C N1C 180 . 2_666 ?
N1C Cu1C N4C 85.9(3) . 2_666 ?
N1C Cu1C N4C 94.1(3) 2_666 2_666 ?
N1C Cu1C N4C 94.1(3) . . ?
N1C Cu1C N4C 85.9(3) 2_666 . ?
N4C Cu1C N4C 180 2_666 . ?
V2 O12 V1 138.7(4) . . ?
V2 O23 V3 171.9(6) . . ?
V1 O13 V3 149.6(5) . 1_455 ?
C7C N1C C2C 113.7(8) . . ?
C7C N1C Cu1C 116.9(6) . . ?
C2C N1C Cu1C 106.8(6) . . ?
C2B N1B C7B 112.6(7) . . ?
C2B N1B Cu1B 106.3(6) . . ?
C7B N1B Cu1B 118.1(6) . . ?
C5C N4C C3C 113.3(8) . . ?
C5C N4C Cu1C 117.1(6) . . ?
C3C N4C Cu1C 106.0(6) . . ?
C5B N4B C3B 112.2(7) . . ?
C5B N4B Cu1B 117.9(6) . . ?
C3B N4B Cu1B 105.9(6) . . ?
C2B C3B N4B 107.3(8) . . ?
N1B C2B C3B 108.4(8) . . ?
C7C C6C C5C 114.9(9) . . ?
N4B C5B C6B 111.7(8) . . ?
N1B C7B C6B 111.2(8) . 2_556 ?
N1C C7C C6C 112.1(8) . . ?
N4C C5C C6C 111.7(9) . . ?
C5B C6B C7B 115.0(8) . 2_556 ?
N4C C3C C2C 108.1(8) . 2_666 ?
N1C C2C C3C 108.3(8) . 2_666 ?
C5A N4A C3A 112.2(8) . . ?
C5A N4A Cu1A 118.3(6) . . ?
C3A N4A Cu1A 106.4(6) . . ?
C2A N1A C7A 111.7(8) . . ?
C2A N1A Cu1A 107.1(6) . . ?
C7A N1A Cu1A 117.2(6) . . ?
N4A C5A C6A 113.0(9) . . ?
N4A C3A C2A 106.9(8) . . ?
N1A C7A C6A 112.1(9) . 2_667 ?
N1A C2A C3A 106.7(8) . . ?
C7A C6A C5A 112.2(8) 2_667 . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1404579'
_audit_update_record             
;
2015-07-14 deposited with the CCDC.
2015-07-23 downloaded from the CCDC.
;
#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C10 H24 Cu N4 O6 V2'
_chemical_formula_sum            'C10 H24 Cu N4 O6 V2'
_chemical_formula_weight         461.75
_chemical_compound_source        'synthesis as described'
#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.751(2)
_cell_length_b                   13.094(3)
_cell_length_c                   13.363(3)
_cell_angle_alpha                102.449(18)
_cell_angle_beta                 101.653(19)
_cell_angle_gamma                101.148(19)
_cell_volume                     1418.7(6)
_cell_formula_units_Z            3
_cell_measurement_temperature    393(2)
_cell_measurement_reflns_used    690
_cell_measurement_theta_min      2.447
_cell_measurement_theta_max      17.408

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.1255
_exptl_crystal_size_mid          0.0853
_exptl_crystal_size_min          0.0304
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             705
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-4 -16 8 0.0426
5 -15 -7 0.0276
-11 8 -1 0.0566
-1 3 17 0.0108
1 -3 -17 0.0197
-12 -1 4 0.0658
0 18 -7 0.0385
12 -1 -3 0.0574



#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    2.111
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
        (compiled May 22 2014,16:03:01)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (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_correction_T_min  0.895
_exptl_absorpt_correction_T_max  0.964

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      393(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_detector_area_resol_mean 16.2439
_diffrn_orient_matrix_ub_11      -0.0817958
_diffrn_orient_matrix_ub_12      -0.029399
_diffrn_orient_matrix_ub_13      -0.0193224
_diffrn_orient_matrix_ub_21      0.0103739
_diffrn_orient_matrix_ub_22      -0.0128493
_diffrn_orient_matrix_ub_23      -0.0521486
_diffrn_orient_matrix_ub_31      0.0223456
_diffrn_orient_matrix_ub_32      -0.0474276
_diffrn_orient_matrix_ub_33      0.008125
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0969
_diffrn_reflns_av_unetI/netI     0.354
_diffrn_reflns_number            8399
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.975
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_reflns_number_total             4991
_reflns_number_gt                2116
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
        (compiled May 22 2014,16:03:01)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
        (compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
        (compiled May 22 2014,16:03:01)
;
_computing_structure_solution    'OLEX2 (Dolomanov, 2009)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'


#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0545P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4991
_refine_ls_number_parameters     316
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2426
_refine_ls_R_factor_gt           0.1078
_refine_ls_wR_factor_ref         0.2511
_refine_ls_wR_factor_gt          0.1866
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_diff_density_max         0.841
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.123

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'

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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1A Cu 0.5 0.5 0.5 0.0558(8) Uani 1 d . .
Cu1B Cu 1 1 1 0.0525(8) Uani 1 d . .
Cu1C Cu 1 0.5 1 0.0586(8) Uani 1 d . .
V1 V 0.9538(3) 0.71468(19) 0.85150(19) 0.0416(7) Uani 1 d . .
V2 V 0.5651(3) 0.6472(2) 0.7896(2) 0.0472(8) Uani 1 d . .
V3 V 0.2672(3) 0.7796(2) 0.7300(2) 0.0557(9) Uani 1 d . .
O1 O 1.0010(11) 0.7946(8) 0.9715(7) 0.061(3) Uani 1 d . .
O1M O 0.9525(11) 0.5925(7) 0.8626(8) 0.060(3) Uani 1 d . .
O2 O 0.5995(11) 0.6135(10) 0.8988(8) 0.086(4) Uani 1 d . .
O2M O 0.4944(11) 0.5434(9) 0.6901(8) 0.081(4) Uani 1 d . .
O3 O 0.2113(14) 0.7244(11) 0.6068(10) 0.113(5) Uani 1 d . .
O3M O 0.3334(12) 0.9089(9) 0.7495(9) 0.079(4) Uani 1 d . .
O12 O 0.7575(10) 0.7200(7) 0.7774(7) 0.052(3) Uani 1 d . .
O23 O 0.4328(13) 0.7316(10) 0.7952(11) 0.111(5) Uani 1 d . .
O31 O 0.1015(11) 0.7609(9) 0.7863(9) 0.079(4) Uani 1 d . .
N1B N 0.8787(14) 0.9843(9) 1.1096(11) 0.055(4) Uani 1 d . .
H1B H 0.8706 1.0575 1.1404 0.066 Uiso 1 calc . .
N4B N 0.7842(12) 0.9543(9) 0.8967(10) 0.050(3) Uani 1 d . .
H4B H 0.7665 0.8769 0.8641 0.06 Uiso 1 calc . .
C3B C 0.6629(18) 0.9641(14) 0.9557(14) 0.074(6) Uani 1 d . .
H3BA H 0.5579 0.9206 0.9129 0.089 Uiso 1 calc . .
H3BB H 0.6572 1.0387 0.9765 0.089 Uiso 1 calc . .
N1C N 0.7746(14) 0.4859(10) 1.0158(10) 0.058(4) Uani 1 d . .
H1C H 0.7247 0.5256 0.9696 0.07 Uiso 1 calc . .
C3A C 0.7884(19) 0.4566(15) 0.5861(13) 0.077(6) Uani 1 d . .
H3AA H 0.8651 0.4122 0.5844 0.092 Uiso 1 calc . .
H3AB H 0.7863 0.4835 0.6592 0.092 Uiso 1 calc . .
C2B C 0.7139(17) 0.9249(12) 1.0515(13) 0.062(5) Uani 1 d . .
H2BA H 0.6417 0.9354 1.097 0.074 Uiso 1 calc . .
H2BB H 0.7084 0.8483 1.03 0.074 Uiso 1 calc . .
N1A N 0.7107(14) 0.6108(12) 0.5417(11) 0.071(4) Uani 1 d . .
H1A H 0.7257 0.6478 0.6163 0.085 Uiso 1 calc . .
N4C N 0.9060(14) 0.3535(10) 0.8967(9) 0.058(4) Uani 1 d . .
H4C H 0.9327 0.3006 0.9348 0.07 Uiso 1 calc . .
C7B C 1.055(2) 1.0521(14) 0.8020(14) 0.077(5) Uani 1 d . .
H7BA H 1.1203 1.0439 0.7517 0.093 Uiso 1 calc . .
H7BB H 1.0607 1.1285 0.8263 0.093 Uiso 1 calc . .
C2A C 0.8385(19) 0.5507(16) 0.5399(14) 0.081(6) Uani 1 d . .
H2AA H 0.9421 0.5969 0.5823 0.097 Uiso 1 calc . .
H2AB H 0.8464 0.5246 0.4679 0.097 Uiso 1 calc . .
C2C C 0.6857(18) 0.3753(13) 0.9738(15) 0.076(6) Uani 1 d . .
H2CA H 0.571 0.3698 0.9616 0.091 Uiso 1 calc . .
H2CB H 0.7156 0.3333 1.0228 0.091 Uiso 1 calc . .
C5C C 0.970(2) 0.3340(13) 0.8010(14) 0.085(6) Uani 1 d . .
H5CA H 0.9392 0.3818 0.7586 0.101 Uiso 1 calc . .
H5CB H 0.9213 0.2603 0.7587 0.101 Uiso 1 calc . .
C6A C 0.397(2) 0.2420(13) 0.5040(16) 0.093(6) Uani 1 d . .
H6AA H 0.3677 0.178 0.5283 0.111 Uiso 1 calc . .
H6AB H 0.3991 0.2185 0.4304 0.111 Uiso 1 calc . .
C3C C 0.7278(19) 0.3346(14) 0.8705(14) 0.082(6) Uani 1 d . .
H3CA H 0.677 0.2582 0.8403 0.099 Uiso 1 calc . .
H3CB H 0.692 0.3735 0.8199 0.099 Uiso 1 calc . .
C7C C 1.241(2) 0.4672(14) 0.8788(16) 0.090(6) Uani 1 d . .
H7CA H 1.3545 0.4719 0.8831 0.108 Uiso 1 calc . .
H7CB H 1.2065 0.511 0.8329 0.108 Uiso 1 calc . .
C6B C 0.880(2) 0.9929(13) 0.7446(14) 0.071(5) Uani 1 d . .
H6BA H 0.8486 1.019 0.6828 0.085 Uiso 1 calc . .
H6BB H 0.8747 0.9167 0.7197 0.085 Uiso 1 calc . .
N4A N 0.6281(15) 0.3924(11) 0.5233(11) 0.068(4) Uani 1 d . .
H4A H 0.6405 0.3572 0.4539 0.081 Uiso 1 calc . .
C5A C 0.564(3) 0.3060(17) 0.5685(17) 0.114(8) Uani 1 d . .
H5AA H 0.5597 0.3372 0.6403 0.137 Uiso 1 calc . .
H5AB H 0.6353 0.258 0.5714 0.137 Uiso 1 calc . .
C6C C 1.1493(19) 0.3521(14) 0.8275(13) 0.071(5) Uani 1 d . .
H6CA H 1.181 0.3269 0.7629 0.086 Uiso 1 calc . .
H6CB H 1.1799 0.3085 0.8747 0.086 Uiso 1 calc . .
C7A C 0.269(2) 0.3062(16) 0.5115(16) 0.097(7) Uani 1 d . .
H7AA H 0.1631 0.2578 0.4804 0.116 Uiso 1 calc . .
H7AB H 0.2767 0.3382 0.5855 0.116 Uiso 1 calc . .
C5B C 0.7603(19) 1.0048(15) 0.8096(13) 0.072(5) Uani 1 d . .
H5BA H 0.7689 1.0809 0.8381 0.086 Uiso 1 calc . .
H5BB H 0.6525 0.9726 0.7642 0.086 Uiso 1 calc . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
Cu1A N4A 2.000(12) . ?
Cu1A N4A 2.000(12) 2_666 ?
Cu1A N1A 2.005(12) . ?
Cu1A N1A 2.005(12) 2_666 ?
Cu1B N4B 1.996(11) . ?
Cu1B N4B 1.996(11) 2_777 ?
Cu1B N1B 1.996(12) . ?
Cu1B N1B 1.996(12) 2_777 ?
Cu1C N1C 2.003(11) 2_767 ?
Cu1C N1C 2.003(11) . ?
Cu1C N4C 2.013(12) . ?
Cu1C N4C 2.013(12) 2_767 ?
Cu1C O1M 2.420(10) 2_767 ?
Cu1C O1M 2.420(10) . ?
V1 O1M 1.636(9) . ?
V1 O1 1.637(9) . ?
V1 O31 1.781(10) 1_655 ?
V1 O12 1.823(9) . ?
V2 O2M 1.601(10) . ?
V2 O2 1.602(11) . ?
V2 O23 1.750(10) . ?
V2 O12 1.825(9) . ?
V3 O3 1.580(12) . ?
V3 O3M 1.625(11) . ?
V3 O31 1.764(9) . ?
V3 O23 1.825(11) . ?
O31 V1 1.781(10) 1_455 ?
N1B C7B 1.428(18) 2_777 ?
N1B C2B 1.463(16) . ?
N4B C3B 1.453(17) . ?
N4B C5B 1.456(18) . ?
C3B C2B 1.50(2) . ?
N1C C2C 1.434(17) . ?
N1C C7C 1.456(19) 2_767 ?
C3A N4A 1.463(18) . ?
C3A C2A 1.52(2) . ?
N1A C7A 1.42(2) 2_666 ?
N1A C2A 1.49(2) . ?
N4C C3C 1.486(17) . ?
N4C C5C 1.489(18) . ?
C7B N1B 1.428(18) 2_777 ?
C7B C6B 1.53(2) . ?
C2C C3C 1.51(2) . ?
C5C C6C 1.50(2) . ?
C6A C5A 1.51(2) . ?
C6A C7A 1.53(2) . ?
C7C N1C 1.456(19) 2_767 ?
C7C C6C 1.50(2) . ?
C6B C5B 1.50(2) . ?
N4A C5A 1.46(2) . ?
C7A N1A 1.42(2) 2_666 ?

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
N4A Cu1A N4A 180 . 2_666 ?
N4A Cu1A N1A 86.9(6) . . ?
N4A Cu1A N1A 93.1(6) 2_666 . ?
N4A Cu1A N1A 93.1(6) . 2_666 ?
N4A Cu1A N1A 86.9(6) 2_666 2_666 ?
N1A Cu1A N1A 180 . 2_666 ?
N4B Cu1B N4B 180 . 2_777 ?
N4B Cu1B N1B 85.7(5) . . ?
N4B Cu1B N1B 94.3(5) 2_777 . ?
N4B Cu1B N1B 94.3(5) . 2_777 ?
N4B Cu1B N1B 85.7(5) 2_777 2_777 ?
N1B Cu1B N1B 180 . 2_777 ?
N1C Cu1C N1C 180 2_767 . ?
N1C Cu1C N4C 96.3(5) 2_767 . ?
N1C Cu1C N4C 83.7(5) . . ?
N1C Cu1C N4C 83.7(5) 2_767 2_767 ?
N1C Cu1C N4C 96.3(5) . 2_767 ?
N4C Cu1C N4C 180 . 2_767 ?
N1C Cu1C O1M 92.2(4) 2_767 2_767 ?
N1C Cu1C O1M 87.8(4) . 2_767 ?
N4C Cu1C O1M 87.3(4) . 2_767 ?
N4C Cu1C O1M 92.7(4) 2_767 2_767 ?
N1C Cu1C O1M 87.8(4) 2_767 . ?
N1C Cu1C O1M 92.2(4) . . ?
N4C Cu1C O1M 92.7(4) . . ?
N4C Cu1C O1M 87.3(4) 2_767 . ?
O1M Cu1C O1M 180 2_767 . ?
O1M V1 O1 107.3(5) . . ?
O1M V1 O31 111.6(5) . 1_655 ?
O1 V1 O31 107.9(5) . 1_655 ?
O1M V1 O12 110.9(4) . . ?
O1 V1 O12 110.5(4) . . ?
O31 V1 O12 108.5(5) 1_655 . ?
O2M V2 O2 111.4(7) . . ?
O2M V2 O23 111.4(6) . . ?
O2 V2 O23 108.6(6) . . ?
O2M V2 O12 108.1(5) . . ?
O2 V2 O12 107.2(5) . . ?
O23 V2 O12 110.1(5) . . ?
O3 V3 O3M 109.0(7) . . ?
O3 V3 O31 110.1(6) . . ?
O3M V3 O31 106.8(5) . . ?
O3 V3 O23 111.7(6) . . ?
O3M V3 O23 106.9(6) . . ?
O31 V3 O23 112.2(6) . . ?
V1 O1M Cu1C 139.2(5) . . ?
V1 O12 V2 124.5(5) . . ?
V2 O23 V3 150.2(8) . . ?
V3 O31 V1 165.5(7) . 1_455 ?
C7B N1B C2B 114.8(13) 2_777 . ?
C7B N1B Cu1B 119.9(10) 2_777 . ?
C2B N1B Cu1B 106.1(10) . . ?
C3B N4B C5B 111.2(13) . . ?
C3B N4B Cu1B 108.2(10) . . ?
C5B N4B Cu1B 118.1(9) . . ?
N4B C3B C2B 106.2(13) . . ?
C2C N1C C7C 112.5(13) . 2_767 ?
C2C N1C Cu1C 109.5(10) . . ?
C7C N1C Cu1C 116.1(10) 2_767 . ?
N4A C3A C2A 108.8(14) . . ?
N1B C2B C3B 109.8(13) . . ?
C7A N1A C2A 112.3(14) 2_666 . ?
C7A N1A Cu1A 119.5(12) 2_666 . ?
C2A N1A Cu1A 106.7(11) . . ?
C3C N4C C5C 113.0(13) . . ?
C3C N4C Cu1C 107.7(9) . . ?
C5C N4C Cu1C 115.7(10) . . ?
N1B C7B C6B 114.5(13) 2_777 . ?
N1A C2A C3A 105.9(13) . . ?
N1C C2C C3C 106.4(14) . . ?
N4C C5C C6C 112.9(15) . . ?
C5A C6A C7A 113.0(15) . . ?
N4C C3C C2C 106.2(13) . . ?
N1C C7C C6C 116.2(14) 2_767 . ?
C5B C6B C7B 115.3(15) . . ?
C3A N4A C5A 112.4(16) . . ?
C3A N4A Cu1A 105.2(9) . . ?
C5A N4A Cu1A 118.5(12) . . ?
N4A C5A C6A 111.7(18) . . ?
C5C C6C C7C 114.8(14) . . ?
N1A C7A C6A 111.3(16) 2_666 . ?
N4B C5B C6B 112.6(14) . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
