# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2013

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#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
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#  fide research purposes only. It may contain copyright material
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data_tp-PMBB-6-stp-1_0m

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C126 H161 Cl14 Cr9 Cu6 N18 O65.50'
_chemical_formula_weight         4321.27

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0002 0.0005 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0004 0.0009 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0015 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.1580 0.2154 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.0535 0.0512 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.2418 0.4566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   P63/mcm

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, x, z+1/2'
'y, -x+y, z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'-y, -x, -z'
'x, x-y, -z'
'-x+y, y, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, -x, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'y, x, z'
'-x, -x+y, z'
'x-y, -y, z'

_cell_length_a                   29.72(2)
_cell_length_b                   29.72(2)
_cell_length_c                   26.388(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     20192(24)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.711
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4390
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9873
_exptl_absorpt_correction_T_max  0.9974
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2003)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.40663
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         synchrotron
_diffrn_radiation_monochromator  ?
_diffrn_measurement_device_type  'BRUKER SMART APEXII CCD'
_diffrn_measurement_method       'phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7178
_diffrn_reflns_av_R_equivalents  0.1506
_diffrn_reflns_av_sigmaI/netI    0.1086
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         0.91
_diffrn_reflns_theta_max         8.06
_reflns_number_total             1228
_reflns_number_gt                731
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_cell_refinement       'APEX2 (Bruker, 2010); SAINT (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009);XPREP(Sheldrick,2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  'APEX2 (Bruker, 2010)'

_refine_special_details          
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
The following restraints have been needed because of disorder and lower 
resolution of the data:
flat c11 c7 c8 c9 c5 n1 c6 c10
flat c11 o2 o5
dfix 2.38 0.01 c8 c10 c9 c6
dfix 1.5 c7 c11
isor 0.01 o5
dfix 1.25 0.01 c11 o5 c11 o2
dfix 1.39 c7 c8 c8 c9 c9 c5 c5 c6 c6 c10 c10 c7
dfix 2.51 c10 c11 c8 c11
rem isor 0.01 c1 c8 c9 c6 c10 c7 c11 o7 o2
flat 0.01 o2 o5 c11 c7
simu 0.02 n1 c5 c9 c8 c7 c11 c6 c10
delu 0.02 n1 c5 c9 c8 c7 c11
simu o2 c11 Cr2
delu o2 C11 Cr2
rem isor 0.01 C1 O7
simu 0.02 c1 c2 o7
delu 0.02 c1 c2 o7
sadi o4 Cr3 o4 Cr2isor 0.02 o4
simu c11 o5 o2
delu c11 o5 o2eqiv $14 x, y, 0.5-z
dfix 2.38 c12 c12_$14 c13 c13_$14
dfix 1.39 c2 c13 c13 c12 c12 c14
dfix 1.5 c14 n15
flat 0.01 c2 c12 c13 c14 n15 c1 c13_$14 c12_$14
flat 0.05 c1 o7 o7_$14 C2
dfix 2.5 o31 o32 o31 o33 o32 o33
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1340P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1228
_refine_ls_number_parameters     177
_refine_ls_number_restraints     136
_refine_ls_R_factor_all          0.1336
_refine_ls_R_factor_gt           0.0931
_refine_ls_wR_factor_ref         0.2452
_refine_ls_wR_factor_gt          0.2290
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.23654(16) 0.61827(8) 0.5000 0.119(2) Uani 1 2 d S . .
Cr2 Cr 0.0000 0.5837(3) 0.2500 0.106(3) Uani 1 4 d SDU . .
Cr3 Cr 0.0000 0.6781(2) 0.3120(2) 0.119(3) Uani 1 2 d SD . .
Cl1 Cl 0.2136(2) 0.6689(2) 0.5462(2) 0.128(3) Uani 1 1 d . . .
Cl2 Cl 0.3333 0.6667 0.5000 0.105(5) Uani 1 6 d S . .
C1 C 0.069(2) 0.7607(18) 0.2500 0.136(11) Uani 1 2 d SDU . .
C2 C 0.1224(13) 0.8073(12) 0.2500 0.186(13) Uani 1 2 d SDU . .
O1 O 0.0000 0.5097(10) 0.2500 0.153(13) Uani 1 4 d S . .
O2 O 0.0521(7) 0.6038(6) 0.2971(7) 0.160(7) Uani 1 1 d DU . .
O3 O 0.0000 0.7124(7) 0.3836(8) 0.171(10) Uani 1 2 d S . .
O4 O 0.0000 0.6459(5) 0.2500 0.115(11) Uani 1 4 d SDU . .
O5 O 0.0538(6) 0.6681(6) 0.3416(6) 0.119(6) Uani 1 1 d DU . .
O6 O 0.3333 0.6667 0.3598(7) 0.096(8) Uani 1 3 d S . .
O7 O 0.0522(7) 0.7445(6) 0.2954(7) 0.148(7) Uani 1 1 d DU . .
N1 N 0.2481(7) 0.6646(7) 0.4370(6) 0.133(7) Uani 1 1 d DU . .
H1A H 0.2661 0.6988 0.4469 0.159 Uiso 1 1 calc R . .
H1B H 0.2686 0.6595 0.4143 0.159 Uiso 1 1 calc R . .
C5 C 0.2004(10) 0.6551(10) 0.4107(9) 0.129(7) Uani 1 1 d DU . .
C6 C 0.1782(9) 0.6191(8) 0.3729(9) 0.155(9) Uani 1 1 d DU . .
H6 H 0.1946 0.6001 0.3627 0.185 Uiso 1 1 calc R . .
C7 C 0.1158(7) 0.6437(6) 0.3587(6) 0.130(8) Uani 1 1 d DU . .
C8 C 0.1387(8) 0.6798(7) 0.3965(7) 0.133(7) Uani 1 1 d DU . .
H8 H 0.1244 0.7012 0.4046 0.160 Uiso 1 1 calc R . .
C9 C 0.1812(9) 0.6866(8) 0.4233(8) 0.139(7) Uani 1 1 d DU . .
H9 H 0.1964 0.7120 0.4492 0.167 Uiso 1 1 calc R . .
C10 C 0.1334(9) 0.6095(8) 0.3491(8) 0.148(9) Uani 1 1 d DU . .
H10 H 0.1152 0.5807 0.3271 0.178 Uiso 1 1 calc R . .
C11 C 0.0701(6) 0.6383(5) 0.3303(5) 0.123(7) Uani 1 1 d DU . .
C12 C 0.1976(14) 0.8734(13) 0.2952(4) 0.45(3) Uiso 1 1 d D . .
H12 H 0.2147 0.8884 0.3263 0.546 Uiso 1 1 calc R . .
C13 C 0.1482(13) 0.8300(12) 0.2950(4) 0.354 Uiso 1 1 d D . .
H13 H 0.1316 0.8154 0.3264 0.425 Uiso 1 1 calc R . .
C14 C 0.2215(19) 0.8944(17) 0.2500 0.46(5) Uiso 1 2 d SD . .
N15 N 0.275(2) 0.9410(18) 0.2500 0.65(7) Uiso 1 2 d SD . .
H15A H 0.2904 0.9548 0.2211 0.777 Uiso 0.50 1 calc PR . .
H15B H 0.2904 0.9548 0.2789 0.777 Uiso 0.50 1 calc PR . .
O31 O 0.314(2) 1.0000 0.359(3) 0.57(4) Uiso 1 2 d SD . .
O32 O 0.287(3) 1.0000 0.448(3) 0.53(8) Uiso 0.50 2 d SPD . .
O33 O 0.232(2) 1.0000 0.376(3) 0.49(5) Uiso 0.75 2 d SPD . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.149(5) 0.138(3) 0.074(4) 0.005(3) 0.000 0.075(2)
Cr2 0.112(8) 0.150(7) 0.044(6) 0.000 0.000 0.056(4)
Cr3 0.159(7) 0.136(5) 0.068(5) -0.013(4) 0.000 0.079(3)
Cl1 0.130(6) 0.148(7) 0.115(6) 0.020(5) 0.015(4) 0.076(5)
Cl2 0.131(9) 0.131(9) 0.052(11) 0.000 0.000 0.066(4)
C1 0.21(2) 0.083(19) 0.10(2) 0.000 0.000 0.062(17)
C2 0.24(3) 0.13(2) 0.13(2) 0.000 0.000 0.04(2)
O1 0.23(4) 0.16(2) 0.09(3) 0.000 0.000 0.116(19)
O2 0.199(16) 0.114(14) 0.180(17) -0.068(10) -0.087(11) 0.089(12)
O3 0.30(3) 0.160(15) 0.10(2) 0.004(13) 0.000 0.150(16)
O4 0.125(17) 0.114(16) 0.110(19) 0.000 0.000 0.063(8)
O5 0.128(9) 0.126(9) 0.101(9) -0.019(7) 0.012(7) 0.061(7)
O6 0.116(13) 0.116(13) 0.057(18) 0.000 0.000 0.058(6)
O7 0.217(17) 0.091(14) 0.080(19) -0.028(9) 0.004(10) 0.035(13)
N1 0.176(18) 0.150(15) 0.081(15) 0.024(12) 0.002(12) 0.088(14)
C5 0.175(16) 0.135(15) 0.080(15) -0.012(12) -0.016(12) 0.080(13)
C6 0.184(18) 0.156(16) 0.103(17) -0.020(13) -0.029(14) 0.070(15)
C7 0.175(15) 0.130(15) 0.083(14) -0.019(11) -0.032(11) 0.076(13)
C8 0.176(17) 0.139(15) 0.082(15) -0.014(11) -0.031(11) 0.077(13)
C9 0.169(17) 0.146(16) 0.099(15) -0.016(13) -0.023(11) 0.077(13)
C10 0.183(17) 0.150(16) 0.101(15) -0.013(13) -0.057(13) 0.075(15)
C11 0.162(16) 0.116(16) 0.091(15) -0.028(10) -0.031(11) 0.070(12)

_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 2.074(15) 11_566 ?
Cu1 N1 2.074(15) . ?
Cu1 Cl1 2.289(6) 11_566 ?
Cu1 Cl1 2.289(6) . ?
Cu1 Cl2 2.492(5) . ?
Cr2 O2 1.837(17) . ?
Cr2 O2 1.837(17) 8 ?
Cr2 O2 1.837(17) 23 ?
Cr2 O2 1.837(17) 14_556 ?
Cr2 O4 1.848(13) . ?
Cr2 O1 2.20(3) . ?
Cr3 O7 1.853(16) . ?
Cr3 O7 1.853(15) 23 ?
Cr3 O4 1.896(8) . ?
Cr3 O5 1.932(17) 23 ?
Cr3 O5 1.932(17) . ?
Cr3 O3 2.15(2) . ?
Cl2 Cu1 2.492(5) 4_565 ?
Cl2 Cu1 2.492(5) 3_665 ?
C1 O7 1.30(2) 14_556 ?
C1 O7 1.30(2) . ?
C1 C2 1.49(5) . ?
C2 C13 1.392(18) . ?
C2 C13 1.392(18) 14_556 ?
O2 C11 1.247(10) . ?
O4 Cr3 1.896(8) 14_556 ?
O5 C11 1.242(10) . ?
N1 C5 1.47(2) . ?
N1 H1A 0.9200 . ?
N1 H1B 0.9200 . ?
C5 C9 1.358(17) . ?
C5 C6 1.369(17) . ?
C6 C10 1.367(17) . ?
C6 H6 0.9500 . ?
C7 C8 1.370(15) . ?
C7 C10 1.379(15) . ?
C7 C11 1.486(16) . ?
C8 C9 1.371(17) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C12 C14 1.37(2) . ?
C12 C13 1.389(19) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C12 1.37(2) 14_556 ?
C14 N15 1.49(2) . ?
N15 H15A 0.8800 . ?
N15 H15B 0.8800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 N1 163.5(11) 11_566 . ?
N1 Cu1 Cl1 89.7(6) 11_566 11_566 ?
N1 Cu1 Cl1 94.5(6) . 11_566 ?
N1 Cu1 Cl1 94.5(6) 11_566 . ?
N1 Cu1 Cl1 89.7(6) . . ?
Cl1 Cu1 Cl1 150.1(4) 11_566 . ?
N1 Cu1 Cl2 81.7(5) 11_566 . ?
N1 Cu1 Cl2 81.7(5) . . ?
Cl1 Cu1 Cl2 104.96(19) 11_566 . ?
Cl1 Cu1 Cl2 104.96(19) . . ?
O2 Cr2 O2 169.0(11) . 8 ?
O2 Cr2 O2 93.7(11) . 23 ?
O2 Cr2 O2 85.3(11) 8 23 ?
O2 Cr2 O2 85.3(11) . 14_556 ?
O2 Cr2 O2 93.7(11) 8 14_556 ?
O2 Cr2 O2 169.0(11) 23 14_556 ?
O2 Cr2 O4 95.5(5) . . ?
O2 Cr2 O4 95.5(5) 8 . ?
O2 Cr2 O4 95.5(5) 23 . ?
O2 Cr2 O4 95.5(5) 14_556 . ?
O2 Cr2 O1 84.5(5) . . ?
O2 Cr2 O1 84.5(5) 8 . ?
O2 Cr2 O1 84.5(5) 23 . ?
O2 Cr2 O1 84.5(5) 14_556 . ?
O4 Cr2 O1 180.000(6) . . ?
O7 Cr3 O7 92.9(10) . 23 ?
O7 Cr3 O4 97.0(6) . . ?
O7 Cr3 O4 97.0(6) 23 . ?
O7 Cr3 O5 169.4(7) . 23 ?
O7 Cr3 O5 86.7(7) 23 23 ?
O4 Cr3 O5 93.5(5) . 23 ?
O7 Cr3 O5 86.7(7) . . ?
O7 Cr3 O5 169.4(7) 23 . ?
O4 Cr3 O5 93.5(5) . . ?
O5 Cr3 O5 91.7(10) 23 . ?
O7 Cr3 O3 84.3(7) . . ?
O7 Cr3 O3 84.3(7) 23 . ?
O4 Cr3 O3 178.0(8) . . ?
O5 Cr3 O3 85.1(6) 23 . ?
O5 Cr3 O3 85.1(6) . . ?
Cu1 Cl2 Cu1 120.000(1) 4_565 . ?
Cu1 Cl2 Cu1 120.000(1) 4_565 3_665 ?
Cu1 Cl2 Cu1 120.000(1) . 3_665 ?
O7 C1 O7 135(5) 14_556 . ?
O7 C1 C2 113(3) 14_556 . ?
O7 C1 C2 113(3) . . ?
C13 C2 C13 117(3) . 14_556 ?
C13 C2 C1 121.4(13) . . ?
C13 C2 C1 121.4(13) 14_556 . ?
C11 O2 Cr2 133.6(15) . . ?
Cr2 O4 Cr3 120.3(4) . . ?
Cr2 O4 Cr3 120.3(4) . 14_556 ?
Cr3 O4 Cr3 119.3(9) . 14_556 ?
C11 O5 Cr3 131.5(15) . . ?
C1 O7 Cr3 125(3) . . ?
C5 N1 Cu1 115.2(14) . . ?
C5 N1 H1A 108.5 . . ?
Cu1 N1 H1A 108.5 . . ?
C5 N1 H1B 108.5 . . ?
Cu1 N1 H1B 108.5 . . ?
H1A N1 H1B 107.5 . . ?
C9 C5 C6 120.8(18) . . ?
C9 C5 N1 117(2) . . ?
C6 C5 N1 122(2) . . ?
C10 C6 C5 122(2) . . ?
C10 C6 H6 118.8 . . ?
C5 C6 H6 118.8 . . ?
C8 C7 C10 119.2(14) . . ?
C8 C7 C11 121.4(15) . . ?
C10 C7 C11 119.3(15) . . ?
C7 C8 C9 123.3(18) . . ?
C7 C8 H8 118.3 . . ?
C9 C8 H8 118.3 . . ?
C5 C9 C8 117(2) . . ?
C5 C9 H9 121.7 . . ?
C8 C9 H9 121.7 . . ?
C6 C10 C7 116.8(19) . . ?
C6 C10 H10 121.6 . . ?
C7 C10 H10 121.6 . . ?
O5 C11 O2 126.4(19) . . ?
O5 C11 C7 117.6(17) . . ?
O2 C11 C7 116.0(16) . . ?
C14 C12 C13 119(2) . . ?
C14 C12 H12 120.4 . . ?
C13 C12 H12 120.4 . . ?
C12 C13 C2 121.5(17) . . ?
C12 C13 H13 119.2 . . ?
C2 C13 H13 119.2 . . ?
C12 C14 C12 121(3) 14_556 . ?
C12 C14 N15 119.4(17) 14_556 . ?
C12 C14 N15 119.4(17) . . ?
C14 N15 H15A 120.0 . . ?
C14 N15 H15B 120.0 . . ?
H15A N15 H15B 120.0 . . ?

_diffrn_measured_fraction_theta_max 0.956
_diffrn_reflns_theta_full        8.06
_diffrn_measured_fraction_theta_full 0.956
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.061

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.006 -0.004 -0.008 13353 2633 ' '
_platon_squeeze_details          
;
Mixture of MeOH and CH2Cl2 solvents have been used. 
Water can be present as well.Possible formula would therefore be 
[(Cr3O)3(H2O)3 (C7H6NO2)18(Cu3ClCl6)2].23.5H2O.(xCH2Cl2,yMeOH,zH2O)
with total number of electrons from x,y,z solcents not exceeding 
1332 per formula unit. 
;
_vrf_THETM01_I                   
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The lack of high angle diffraction data (despite of using 
synchrotron source and trying several crystals) can be attributed to 
the presence of the ligand / solvent disorder.
;
_vrf_PLAT023_I                   
;
PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6]..       8.06 Deg. 
RESPONSE: The lack of high angle diffraction data (despite of using 
synchrotron source and trying several crystals) can be attributed to 
the presence of the ligand / solvent disorder.
;
_vrf_PLAT306_I                   
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O6     
RESPONSE: Atoms O6, O31, O32, O33 are involved in hydrogen bonding. 
Hydrogen atoms could not be localized.
;
_vrf_PLAT430_I                   
;
PROBLEM: Short Inter D...A Contact  O31    ..  O32     ..       2.48 Ang. 
RESPONSE: Atoms O31, O32, O33 are involved in hydrogen bonding.
Hydrogen atoms could not be localized.
;
# end Validation Reply Form
_database_code_depnum_ccdc_archive 'CCDC 943023'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_tp-PMBB-6_0m

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C54 H42 N6 O16 Cr3 7+,(N O3 -)7,(C H Cl3)3,(C H4 O)8.25,(H2 O)10.16'
_chemical_formula_sum            'C53.25 H98.33 Cl9 Cr3 N13 O52.40'
_chemical_formula_weight         2234.23

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   R3m

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'

_cell_length_a                   15.2032(6)
_cell_length_b                   15.2032(6)
_cell_length_c                   46.090(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     9225.8(7)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3459
_exptl_absorpt_coefficient_mu    4.653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3320
_exptl_absorpt_correction_T_max  0.3833
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2003)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'INCOATEC Imus micro-focus source'
_diffrn_radiation_monochromator  mirrors
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14040
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1091
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_theta_min         3.87
_diffrn_reflns_theta_max         65.88
_reflns_number_total             14040
_reflns_number_gt                10805
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_cell_refinement       'APEX2 (Bruker, 2010); SAINT (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009);XPREP(Sheldrick,2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008), OLEX2 (2009)'
_computing_molecular_graphics    ?
_computing_publication_material  'OLEX2 (Dolomanov,2009)'

_refine_special_details          
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
The following restraints have been needed during the refinement 
due to the disorder
EQIV $1 1-Y,1-X,+Z
DFIX 1.75 Cl2 C13 Cl3 C13
DFIX 1.4 O15 C17 O4 C29 O4 C15 O1G C28 O1M C1K
DFIX 1.24 O12 N5 O10 N18 N18 O31
DFIX 1.75 Cl15 C19
FLAT O31 N18 O10 O10_$1
DELU O4 C11
DELU C1 C2
SIMU 0.01 0.02 1.7 C13 Cl2 Cl3
EADP C13 C19 Cl15
EADP N18 O31
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1704P)^2^+44.8317P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.073(12)
_refine_ls_number_reflns         14040
_refine_ls_number_parameters     258
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.1374
_refine_ls_R_factor_gt           0.1109
_refine_ls_wR_factor_ref         0.3143
_refine_ls_wR_factor_gt          0.2833
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.92791(4) 0.07209(4) 0.33046(3) 0.0460(3) Uani 1 2 d S . .
O5 O 1.0000 0.0000 0.33007(16) 0.0441(17) Uani 1 6 d S . .
O1 O 0.8335(3) -0.0110(3) 0.29967(9) 0.0754(12) Uani 1 1 d . . .
C1 C 0.8101(6) -0.0950(3) 0.28909(16) 0.0560(19) Uani 1 2 d SU . .
C2 C 0.7519(6) -0.1241(3) 0.2624(2) 0.068(2) Uani 1 2 d SU . .
C3 C 0.7265(7) -0.2139(6) 0.24840(17) 0.098(2) Uani 1 1 d . . .
H3 H 0.7466 -0.2579 0.2569 0.118 Uiso 1 1 calc R . .
C4 C 0.6731(6) -0.2431(6) 0.22251(18) 0.100(3) Uani 1 1 d . . .
H4 H 0.6540 -0.3067 0.2137 0.120 Uiso 1 1 calc R . .
C5 C 0.6495(9) -0.1753(4) 0.2104(2) 0.096(3) Uani 1 2 d S . .
N1 N 0.5926(8) -0.2037(4) 0.18221(19) 0.098(3) Uani 1 2 d S . .
H1A H 0.5294 -0.2581 0.1850 0.147 Uiso 0.50 1 calc PR . .
H1B H 0.6266 -0.2200 0.1690 0.147 Uiso 0.50 1 calc PR . .
H1C H 0.5871 -0.1504 0.1755 0.147 Uiso 0.50 1 calc PR . .
O3 O 0.8321(3) -0.0116(3) 0.36085(8) 0.0570(9) Uani 1 1 d . . .
C6 C 0.8063(5) -0.0968(3) 0.37045(15) 0.0480(17) Uani 1 2 d S . .
C7 C 0.7350(5) -0.1325(3) 0.39647(16) 0.0535(18) Uani 1 2 d S . .
C8 C 0.7064(6) -0.2224(6) 0.40850(19) 0.094(2) Uani 1 1 d . . .
H8 H 0.7285 -0.2658 0.4006 0.112 Uiso 1 1 calc R . .
C9 C 0.6445(7) -0.2517(6) 0.4324(2) 0.107(3) Uani 1 1 d . . .
H9 H 0.6261 -0.3153 0.4411 0.128 Uiso 1 1 calc R . .
C10 C 0.6087(7) -0.1956(3) 0.44405(18) 0.065(2) Uani 1 2 d S . .
N2 N 0.5391(6) -0.2305(3) 0.46765(18) 0.087(2) Uani 1 2 d S . .
H2A H 0.4823 -0.2893 0.4626 0.130 Uiso 0.50 1 calc PR . .
H2B H 0.5219 -0.1827 0.4721 0.130 Uiso 0.50 1 calc PR . .
H2C H 0.5684 -0.2417 0.4833 0.130 Uiso 0.50 1 calc PR . .
Cl1 Cl 0.93815(10) 0.06185(10) 0.45220(7) 0.1383(15) Uani 1 2 d S . .
C16 C 1.0000 0.0000 0.4628(5) 0.089(5) Uani 1 6 d S . .
H16 H 1.0000 0.0000 0.4845 0.107 Uiso 1 6 calc SR . .
Cl4 Cl 0.4556(5) -0.2722(3) 0.2582(2) 0.276(4) Uani 1 2 d S . .
C12 C 0.3333 -0.3333 0.2431(6) 0.135(9) Uani 1 6 d S . .
H12 H 0.3333 -0.3333 0.2214 0.162 Uiso 1 6 calc SR . .
Cl2 Cl 1.0000 0.0000 0.2371(2) 0.139(3) Uani 0.75 6 d SPD . .
Cl3 Cl 0.9396(3) 0.0604(3) 0.1892(3) 0.254(5) Uani 0.67 2 d SPDU . .
C13 C 1.0000 0.0000 0.1996(5) 0.301(9) Uiso 0.75 6 d SPDU . .
C19 C 1.0000 0.0000 0.1851(19) 0.301(9) Uiso 0.25 6 d SPD . .
Cl15 Cl 1.0000 0.0000 0.1470(19) 0.301(9) Uiso 0.25 6 d SPD . .
O4 O 0.84996(18) 0.15004(18) 0.33029(13) 0.0667(14) Uani 1 2 d SDU . .
C11 C 0.8176(10) 0.1824(10) 0.3535(6) 0.121(8) Uani 0.50 2 d SPU . .
C15 C 0.7412(14) 0.095(2) 0.3288(10) 0.071(10) Uiso 0.15 1 d PD . .
C29 C 0.8192(16) 0.1808(16) 0.3059(8) 0.087(13) Uiso 0.20 2 d SPD . .
O10 O 0.7354(10) 0.1301(11) 0.4711(3) 0.127(4) Uani 0.50 1 d PD . .
N18 N 0.7872(14) 0.2128(14) 0.4611(9) 0.21(2) Uiso 0.25 2 d SPD . .
O31 O 0.757(2) 0.243(2) 0.4411(12) 0.21(2) Uiso 0.25 2 d SPD . .
C28 C 0.5314(17) 0.063(3) 0.4136(10) 0.093(12) Uiso 0.25 2 d SPD . .
O1G O 0.5223(17) 0.045(3) 0.3835(10) 0.159(15) Uiso 0.25 2 d SPD . .
C1K C 0.529(2) 0.059(4) 0.2428(12) 0.108(18) Uiso 0.25 2 d SPD . .
O1M O 0.5682(15) 0.136(3) 0.2225(9) 0.133(12) Uiso 0.25 2 d SPD . .
N3 N 0.3333 -0.3333 0.4261(8) 0.090(9) Uani 0.50 6 d SP . .
O7 O 0.3787(8) -0.2426(16) 0.4255(5) 0.134(6) Uiso 0.50 2 d SP . .
N4 N 0.4580(4) -0.0840(8) 0.1765(2) 0.091(2) Uiso 1 2 d S . .
O8 O 0.5494(5) -0.0370(5) 0.17148(12) 0.1132(17) Uani 1 1 d . . .
O9 O 0.4148(3) -0.1704(6) 0.18499(15) 0.092(2) Uani 1 2 d S . .
N5 N 0.6667 0.3333 0.1911(14) 0.088(18) Uiso 0.25 6 d SPD . .
O12 O 0.6179(6) 0.2358(13) 0.1923(6) 0.086(7) Uiso 0.25 2 d SPD . .
O6 O 0.4514(3) -0.0972(7) 0.4765(2) 0.129(3) Uiso 1 2 d S . .
C14 C 0.4750(7) -0.0499(15) 0.5056(5) 0.171(6) Uiso 1 2 d S . .
C17 C 0.6967(12) 0.3033(12) 0.1880(6) 0.062(8) Uiso 0.25 2 d SPD . .
O15 O 0.6667 0.3333 0.1654(4) 0.102(4) Uiso 0.75 6 d SPD . .
O13 O 0.5331(9) 0.0662(18) 0.4372(6) 0.156(7) Uiso 0.50 2 d SP . .
O19 O 0.6087(18) -0.031(2) 0.3246(6) 0.126(7) Uiso 0.25 1 d P . .
O1E O 0.595(2) -0.101(2) 0.3283(7) 0.125(8) Uiso 0.25 1 d P . .
O1F O 0.5083(9) 0.0166(18) 0.2496(5) 0.134(7) Uiso 0.50 2 d SP . .
O1H O 0.7844(17) 0.2156(17) 0.2611(13) 0.151(14) Uiso 0.25 2 d SP . .
O1I O 0.7941(19) 0.2059(19) 0.2364(13) 0.159(15) Uiso 0.25 2 d SP . .
O27 O 0.491(5) -0.255(3) 0.3756(18) 0.23(3) Uiso 0.25 2 d SP . .
O11 O 0.6667 0.3333 0.385(3) 0.18(4) Uiso 0.25 6 d SP . .
O16 O 0.6667 0.3333 0.4032(19) 0.077(18) Uiso 0.17 6 d SP . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cr1 0.0530(4) 0.0530(4) 0.0324(5) 0.0012(3) -0.0012(3) 0.0268(5)
O5 0.056(3) 0.056(3) 0.020(4) 0.000 0.000 0.0281(13)
O1 0.090(3) 0.100(3) 0.057(3) -0.031(2) -0.040(2) 0.064(3)
C1 0.061(4) 0.075(4) 0.027(4) -0.0057(17) -0.011(3) 0.030(2)
C2 0.047(4) 0.074(4) 0.074(6) -0.0070(19) -0.014(4) 0.023(2)
C3 0.135(6) 0.095(5) 0.070(5) -0.020(4) -0.055(5) 0.062(5)
C4 0.116(6) 0.114(5) 0.079(5) -0.041(5) -0.067(5) 0.065(5)
C5 0.107(7) 0.121(7) 0.055(6) -0.019(3) -0.039(5) 0.053(4)
N1 0.129(7) 0.106(4) 0.066(5) -0.029(3) -0.059(5) 0.065(3)
O3 0.063(2) 0.063(2) 0.050(2) 0.0202(18) 0.0226(18) 0.0353(18)
C6 0.045(4) 0.060(4) 0.034(4) -0.0027(15) -0.005(3) 0.0225(18)
C7 0.044(4) 0.069(4) 0.039(4) 0.0029(16) 0.006(3) 0.0219(19)
C8 0.104(5) 0.090(5) 0.098(6) 0.034(4) 0.059(5) 0.057(4)
C9 0.123(6) 0.094(5) 0.114(7) 0.055(5) 0.060(6) 0.062(5)
C10 0.084(5) 0.072(4) 0.043(5) 0.010(2) 0.020(4) 0.042(3)
N2 0.092(5) 0.101(4) 0.065(5) 0.009(2) 0.019(4) 0.046(3)
Cl1 0.226(4) 0.226(4) 0.0687(19) 0.0051(6) -0.0051(6) 0.193(4)
C16 0.086(7) 0.086(7) 0.097(15) 0.000 0.000 0.043(3)
Cl4 0.178(5) 0.356(10) 0.234(9) 0.025(3) 0.049(5) 0.089(3)
C12 0.166(14) 0.166(14) 0.074(14) 0.000 0.000 0.083(7)
Cl2 0.146(4) 0.146(4) 0.123(7) 0.000 0.000 0.073(2)
Cl3 0.277(7) 0.277(7) 0.305(10) 0.027(3) -0.027(3) 0.212(8)
O4 0.075(3) 0.075(3) 0.064(4) -0.0007(13) 0.0007(13) 0.048(3)
C11 0.148(16) 0.148(16) 0.098(18) -0.013(6) 0.013(6) 0.096(18)
O10 0.120(8) 0.169(11) 0.135(11) -0.067(9) -0.039(7) 0.105(8)
N3 0.050(8) 0.050(8) 0.17(3) 0.000 0.000 0.025(4)
O8 0.115(4) 0.152(4) 0.060(3) -0.009(3) -0.035(3) 0.057(3)
O9 0.110(4) 0.110(5) 0.057(4) 0.001(4) 0.0005(18) 0.055(3)

_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
Cr1 O5 1.8985(10) . ?
Cr1 O3 1.962(3) 4_665 ?
Cr1 O3 1.962(3) . ?
Cr1 O1 1.964(4) 4_665 ?
Cr1 O1 1.964(4) . ?
Cr1 O4 2.052(5) . ?
O5 Cr1 1.8985(10) 3_765 ?
O5 Cr1 1.8985(10) 2_645 ?
O1 C1 1.241(5) . ?
C1 O1 1.241(5) 6_545 ?
C1 C2 1.450(12) . ?
C2 C3 1.379(9) 6_545 ?
C2 C3 1.379(9) . ?
C3 C4 1.385(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.371(8) . ?
C4 H4 0.9500 . ?
C5 C4 1.371(8) 6_545 ?
C5 N1 1.498(12) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
O3 C6 1.233(5) . ?
C6 O3 1.233(5) 6_545 ?
C6 C7 1.523(11) . ?
C7 C8 1.331(8) . ?
C7 C8 1.331(8) 6_545 ?
C8 C9 1.372(10) . ?
C8 H8 0.9500 . ?
C9 C10 1.331(9) . ?
C9 H9 0.9500 . ?
C10 C9 1.331(9) 6_545 ?
C10 N2 1.423(11) . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 H2C 0.9100 . ?
Cl1 C16 1.700(7) . ?
C16 Cl1 1.700(7) 2_645 ?
C16 Cl1 1.700(7) 3_765 ?
C16 H16 1.0000 . ?
Cl4 C12 1.755(13) . ?
C12 Cl4 1.755(13) 2_545 ?
C12 Cl4 1.755(13) 3_655 ?
C12 H12 1.0000 . ?
Cl2 C13 1.730(19) . ?
Cl3 C19 1.601(14) . ?
Cl3 C13 1.660(9) . ?
C13 C19 0.67(9) . ?
C13 Cl3 1.660(9) 2_645 ?
C13 Cl3 1.660(9) 3_765 ?
C19 Cl3 1.601(14) 3_765 ?
C19 Cl3 1.601(14) 2_645 ?
C19 Cl15 1.76(2) . ?
O4 C11 1.37(2) . ?
O4 C29 1.384(19) . ?
O4 C15 1.434(18) . ?
O4 C15 1.434(18) 4_665 ?
C11 C15 1.69(4) . ?
C11 C15 1.69(4) 4_665 ?
C15 C29 1.63(4) . ?
C29 C15 1.63(4) 4_665 ?
O10 N18 1.194(18) . ?
N18 O10 1.194(18) 4_665 ?
N18 O31 1.22(2) . ?
C28 O13 1.09(4) . ?
C28 O1G 1.407(19) . ?
C1K O1F 0.64(4) . ?
C1K O1M 1.39(2) . ?
N3 O7 1.19(2) 2_545 ?
N3 O7 1.19(2) . ?
N3 O7 1.19(2) 3_655 ?
N4 O9 1.204(11) . ?
N4 O8 1.225(7) 5_655 ?
N4 O8 1.225(7) . ?
N5 C17 0.80(4) . ?
N5 C17 0.80(4) 3_665 ?
N5 C17 0.80(4) 2_655 ?
N5 O15 1.19(6) . ?
N5 O12 1.285(17) 3_665 ?
N5 O12 1.285(17) . ?
N5 O12 1.285(17) 2_655 ?
O12 C17 1.140(15) . ?
O12 C17 1.140(15) 3_665 ?
O12 O15 1.79(3) . ?
O6 C14 1.48(2) . ?
C17 O12 1.140(15) 2_655 ?
C17 O15 1.308(18) . ?
C17 C17 1.37(5) 2_655 ?
C17 C17 1.37(5) 3_665 ?
O15 C17 1.308(18) 2_655 ?
O15 C17 1.308(18) 3_665 ?
O15 O12 1.79(3) 3_665 ?
O15 O12 1.79(3) 2_655 ?
O19 O1E 0.98(3) . ?
O1H O1I 1.17(6) . ?
O11 O16 0.82(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Cr1 O3 95.04(19) . 4_665 ?
O5 Cr1 O3 95.04(19) . . ?
O3 Cr1 O3 88.1(2) 4_665 . ?
O5 Cr1 O1 94.0(2) . 4_665 ?
O3 Cr1 O1 91.82(17) 4_665 4_665 ?
O3 Cr1 O1 170.96(16) . 4_665 ?
O5 Cr1 O1 94.0(2) . . ?
O3 Cr1 O1 170.96(16) 4_665 . ?
O3 Cr1 O1 91.83(17) . . ?
O1 Cr1 O1 86.8(3) 4_665 . ?
O5 Cr1 O4 179.2(3) . . ?
O3 Cr1 O4 85.51(16) 4_665 . ?
O3 Cr1 O4 85.51(16) . . ?
O1 Cr1 O4 85.48(17) 4_665 . ?
O1 Cr1 O4 85.48(17) . . ?
Cr1 O5 Cr1 119.993(10) . 3_765 ?
Cr1 O5 Cr1 119.993(10) . 2_645 ?
Cr1 O5 Cr1 119.988(10) 3_765 2_645 ?
C1 O1 Cr1 133.4(4) . . ?
O1 C1 O1 124.6(7) . 6_545 ?
O1 C1 C2 117.7(3) . . ?
O1 C1 C2 117.7(3) 6_545 . ?
C3 C2 C3 116.5(8) 6_545 . ?
C3 C2 C1 121.7(4) 6_545 . ?
C3 C2 C1 121.7(4) . . ?
C2 C3 C4 123.3(7) . . ?
C2 C3 H3 118.3 . . ?
C4 C3 H3 118.3 . . ?
C5 C4 C3 116.2(7) . . ?
C5 C4 H4 121.9 . . ?
C3 C4 H4 121.9 . . ?
C4 C5 C4 124.3(9) . 6_545 ?
C4 C5 N1 117.9(4) . . ?
C4 C5 N1 117.9(4) 6_545 . ?
C5 N1 H1A 109.5 . . ?
C5 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C5 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C6 O3 Cr1 132.9(4) . . ?
O3 C6 O3 126.2(7) . 6_545 ?
O3 C6 C7 116.9(3) . . ?
O3 C6 C7 116.9(3) 6_545 . ?
C8 C7 C8 119.5(8) . 6_545 ?
C8 C7 C6 120.2(4) . . ?
C8 C7 C6 120.2(4) 6_545 . ?
C7 C8 C9 119.2(7) . . ?
C7 C8 H8 120.4 . . ?
C9 C8 H8 120.4 . . ?
C10 C9 C8 123.3(7) . . ?
C10 C9 H9 118.4 . . ?
C8 C9 H9 118.4 . . ?
C9 C10 C9 115.3(9) 6_545 . ?
C9 C10 N2 122.4(4) 6_545 . ?
C9 C10 N2 122.4(4) . . ?
C10 N2 H2A 109.5 . . ?
C10 N2 H2B 109.5 . . ?
H2A N2 H2B 109.5 . . ?
C10 N2 H2C 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
Cl1 C16 Cl1 112.1(6) 2_645 3_765 ?
Cl1 C16 Cl1 112.1(6) 2_645 . ?
Cl1 C16 Cl1 112.1(6) 3_765 . ?
Cl1 C16 H16 106.7 2_645 . ?
Cl1 C16 H16 106.7 3_765 . ?
Cl1 C16 H16 106.7 . . ?
Cl4 C12 Cl4 105.2(10) 2_545 3_655 ?
Cl4 C12 Cl4 105.2(10) 2_545 . ?
Cl4 C12 Cl4 105.2(10) 3_655 . ?
Cl4 C12 H12 113.5 2_545 . ?
Cl4 C12 H12 113.5 3_655 . ?
Cl4 C12 H12 113.5 . . ?
C19 Cl3 C13 23(3) . . ?
C19 C13 Cl3 73.3(9) . . ?
C19 C13 Cl3 73.3(9) . 2_645 ?
Cl3 C13 Cl3 112.1(8) . 2_645 ?
C19 C13 Cl3 73.3(9) . 3_765 ?
Cl3 C13 Cl3 112.1(8) . 3_765 ?
Cl3 C13 Cl3 112.1(8) 2_645 3_765 ?
C19 C13 Cl2 180.000(10) . . ?
Cl3 C13 Cl2 106.7(9) . . ?
Cl3 C13 Cl2 106.7(9) 2_645 . ?
Cl3 C13 Cl2 106.7(9) 3_765 . ?
C13 C19 Cl3 83(3) . 3_765 ?
C13 C19 Cl3 83(3) . 2_645 ?
Cl3 C19 Cl3 118.6(13) 3_765 2_645 ?
C13 C19 Cl3 83(3) . . ?
Cl3 C19 Cl3 118.6(13) 3_765 . ?
Cl3 C19 Cl3 118.6(13) 2_645 . ?
C13 C19 Cl15 180.000(13) . . ?
Cl3 C19 Cl15 97(3) 3_765 . ?
Cl3 C19 Cl15 97(3) 2_645 . ?
Cl3 C19 Cl15 97(3) . . ?
C11 O4 C29 106(2) . . ?
C11 O4 C15 74.2(19) . . ?
C29 O4 C15 71(2) . . ?
C11 O4 C15 74.2(19) . 4_665 ?
C29 O4 C15 71(2) . 4_665 ?
C15 O4 C15 120(3) . 4_665 ?
C11 O4 Cr1 128.4(12) . . ?
C29 O4 Cr1 126(2) . . ?
C15 O4 Cr1 119.8(15) . . ?
C15 O4 Cr1 119.8(15) 4_665 . ?
O4 C11 C15 54.7(13) . . ?
O4 C11 C15 54.7(13) . 4_665 ?
C15 C11 C15 95(3) . 4_665 ?
O4 C15 C29 53.2(12) . . ?
O4 C15 C11 51.1(12) . . ?
C29 C15 C11 82.6(17) . . ?
O4 C29 C15 56.0(13) . 4_665 ?
O4 C29 C15 56.0(13) . . ?
C15 C29 C15 99(3) 4_665 . ?
O10 N18 O10 118(4) 4_665 . ?
O10 N18 O31 121(2) 4_665 . ?
O10 N18 O31 121(2) . . ?
O13 C28 O1G 172(5) . . ?
O1F C1K O1M 167(10) . . ?
O7 N3 O7 119.95(19) 2_545 . ?
O7 N3 O7 119.95(19) 2_545 3_655 ?
O7 N3 O7 119.95(19) . 3_655 ?
O9 N4 O8 122.6(5) . 5_655 ?
O9 N4 O8 122.6(5) . . ?
O8 N4 O8 114.9(11) 5_655 . ?
C17 N5 C17 117(3) . 3_665 ?
C17 N5 C17 117(3) . 2_655 ?
C17 N5 C17 117(3) 3_665 2_655 ?
C17 N5 O15 80(5) . . ?
C17 N5 O15 80(5) 3_665 . ?
C17 N5 O15 80(5) 2_655 . ?
C17 N5 O12 172(8) . 3_665 ?
C17 N5 O12 61.1(4) 3_665 3_665 ?
C17 N5 O12 61.1(4) 2_655 3_665 ?
O15 N5 O12 92(3) . 3_665 ?
C17 N5 O12 61.1(4) . . ?
C17 N5 O12 61.1(4) 3_665 . ?
C17 N5 O12 172(8) 2_655 . ?
O15 N5 O12 92(3) . . ?
O12 N5 O12 119.8(5) 3_665 . ?
C17 N5 O12 61.1(4) . 2_655 ?
C17 N5 O12 172(8) 3_665 2_655 ?
C17 N5 O12 61.1(4) 2_655 2_655 ?
O15 N5 O12 92(3) . 2_655 ?
O12 N5 O12 119.8(5) 3_665 2_655 ?
O12 N5 O12 119.8(5) . 2_655 ?
C17 O12 C17 74(3) . 3_665 ?
C17 O12 N5 38.1(19) . . ?
C17 O12 N5 38.1(19) 3_665 . ?
C17 O12 O15 47.0(13) . . ?
C17 O12 O15 47.0(13) 3_665 . ?
N5 O12 O15 42(3) . . ?
N5 C17 O12 81(2) . 2_655 ?
N5 C17 O12 81(2) . . ?
O12 C17 O12 155(4) 2_655 . ?
N5 C17 O15 63(5) . . ?
O12 C17 O15 93.5(17) 2_655 . ?
O12 C17 O15 93.5(17) . . ?
N5 C17 C17 31.6(15) . 2_655 ?
O12 C17 C17 53.1(17) 2_655 2_655 ?
O12 C17 C17 112.0(18) . 2_655 ?
O15 C17 C17 58.4(13) . 2_655 ?
N5 C17 C17 31.6(15) . 3_665 ?
O12 C17 C17 112.0(18) 2_655 3_665 ?
O12 C17 C17 53.1(17) . 3_665 ?
O15 C17 C17 58.4(13) . 3_665 ?
C17 C17 C17 59.997(13) 2_655 3_665 ?
N5 O15 C17 37.2(17) . . ?
N5 O15 C17 37.2(17) . 2_655 ?
C17 O15 C17 63(3) . 2_655 ?
N5 O15 C17 37.2(17) . 3_665 ?
C17 O15 C17 63(3) . 3_665 ?
C17 O15 C17 63(3) 2_655 3_665 ?
N5 O15 O12 46.0(9) . 3_665 ?
C17 O15 O12 83(2) . 3_665 ?
C17 O15 O12 39.5(7) 2_655 3_665 ?
C17 O15 O12 39.5(7) 3_665 3_665 ?
N5 O15 O12 46.0(9) . 2_655 ?
C17 O15 O12 39.5(7) . 2_655 ?
C17 O15 O12 39.5(7) 2_655 2_655 ?
C17 O15 O12 83(2) 3_665 2_655 ?
O12 O15 O12 77.0(14) 3_665 2_655 ?
N5 O15 O12 45.9(9) . . ?
C17 O15 O12 39.5(7) . . ?
C17 O15 O12 83(2) 2_655 . ?
C17 O15 O12 39.5(7) 3_665 . ?
O12 O15 O12 77.0(14) 3_665 . ?
O12 O15 O12 77.0(14) 2_655 . ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        65.88
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         0.992
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.141

_vrf_PLAT043_I                   
;

PROBLEM: Check Reported Molecular Weight ................    2234.23      
RESPONSE: Due to the disorder it was not possible to locate some of NO3- anions 
and H atoms of water, methanol and one of ChCl3  molecules  - those atoms have 
been inluded in _chemical_formula_sum in order to obtain correct molecular weight 
and density.
;
_vrf_PLAT044_I                   
;
PROBLEM: Calculated and Reported Dx Differ ..............          ? Check
RESPONSE: Due to the disorder it was not possible to locate some of NO3- anions 
and H atoms of water, methanol and one of ChCl3  molecules  - those atoms have 
been inluded in _chemical_formula_sum in order to obtain correct molecular weight 
and density.
;
_database_code_depnum_ccdc_archive 'CCDC 943024'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_tp-PMBB-5-acs-1_0m

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H36 Cl7 Cr3 Cu3 N6 O16'
_chemical_formula_weight         1475.54

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   P-6c2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, -z'
'x, x-y, -z'
'-x+y, y, -z'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'-y, -x, z+1/2'
'x, y, -z+1/2'
'-x+y, -x, -z+1/2'
'-y, x-y, -z+1/2'

_cell_length_a                   13.469(12)
_cell_length_b                   13.469(12)
_cell_length_c                   27.51(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     4323(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    228(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.134
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1472
_exptl_absorpt_coefficient_mu    6.185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5767
_exptl_absorpt_correction_T_max  0.6713
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2003)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      228(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BRUKER SMART APEXII CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            2324
_diffrn_reflns_av_R_equivalents  0.0759
_diffrn_reflns_av_sigmaI/netI    0.0989
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.79
_diffrn_reflns_theta_max         38.97
_reflns_number_total             794
_reflns_number_gt                618
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_cell_refinement       'APEX2 (Bruker, 2010); SAINT (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009);XPREP(Sheldrick,2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  'APEX2 (Bruker, 2010)'

_refine_special_details          
;
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F^2^, conventional R-factors R are based
 on F, with F set to zero for negative F^2^. The threshold expression of
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F^2^ are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
The follwoing restraints have been used during the refinement:
SIMU 0.02 C1 C2 C7 C6 C5 C4 C3 O2 O1 N1
sadi c1 o1 c1 o2
dfix 1.44 c4 n1
dfix 1.5 c1 c2


;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.10(2)
_refine_ls_number_reflns         794
_refine_ls_number_parameters     109
_refine_ls_number_restraints     63
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0449
_refine_ls_wR_factor_ref         0.0936
_refine_ls_wR_factor_gt          0.0887
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_restrained_S_all      0.928
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.2222(3) 0.11110(13) 0.0000 0.0745(11) Uani 1 2 d S . .
Cr1 Cr 0.5145(3) 0.3047(3) 0.2500 0.0469(11) Uani 1 2 d S . .
Cl2 Cl 0.0000 0.0000 0.0000 0.059(3) Uani 1 6 d S . .
Cl1 Cl 0.2600(4) 0.0014(5) -0.05315(14) 0.1217(19) Uani 1 1 d . . .
O3 O 0.3439(9) 0.2723(8) 0.2500 0.045(4) Uani 1 2 d S . .
O1 O 0.4660(7) 0.1915(9) 0.1969(3) 0.066(4) Uani 1 1 d DU . .
N1 N 0.2008(9) 0.0005(10) 0.0550(4) 0.088(4) Uani 1 1 d DU . .
H1A H 0.1629 0.0132 0.0794 0.105 Uiso 1 1 calc R . .
H1B H 0.1534 -0.0717 0.0438 0.105 Uiso 1 1 calc R . .
O4 O 0.6667 0.3333 0.2500 0.025(5) Uani 1 6 d S . .
O2 O 0.5829(8) 0.1256(8) 0.1964(3) 0.065(3) Uani 1 1 d DU . .
C6 C 0.4304(11) -0.0729(9) 0.0747(4) 0.106(6) Uani 1 1 d GU . .
H6 H 0.4548 -0.1205 0.0605 0.127 Uiso 1 1 calc R . .
C5 C 0.3370(10) -0.0688(8) 0.0555(3) 0.096(5) Uani 1 1 d GU . .
H5 H 0.2984 -0.1136 0.0283 0.115 Uiso 1 1 calc R . .
C4 C 0.3009(8) 0.0015(11) 0.0766(4) 0.089(4) Uani 1 1 d GDU . .
C3 C 0.3581(10) 0.0677(8) 0.1169(4) 0.083(5) Uani 1 1 d GU . .
H3 H 0.3337 0.1153 0.1312 0.100 Uiso 1 1 calc R . .
C2 C 0.4514(9) 0.0637(8) 0.1361(3) 0.074(5) Uani 1 1 d GDU . .
C7 C 0.4876(7) -0.0067(10) 0.1150(4) 0.105(5) Uani 1 1 d GU . .
H7 H 0.5507 -0.0094 0.1280 0.126 Uiso 1 1 calc R . .
C1 C 0.5043(13) 0.1331(14) 0.1808(6) 0.061(5) Uani 1 1 d DU . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.066(3) 0.087(2) 0.063(2) -0.0157(18) 0.000 0.0330(13)
Cr1 0.070(3) 0.055(3) 0.025(2) 0.000 0.000 0.038(3)
Cl2 0.055(4) 0.055(4) 0.068(6) 0.000 0.000 0.027(2)
Cl1 0.103(4) 0.154(4) 0.113(3) -0.041(3) 0.003(3) 0.068(4)
O3 0.048(9) 0.038(8) 0.032(7) 0.000 0.000 0.009(7)
O1 0.063(8) 0.072(8) 0.043(7) -0.016(5) 0.002(5) 0.019(6)
N1 0.059(10) 0.124(10) 0.072(8) -0.019(8) -0.008(7) 0.040(9)
O4 0.026(9) 0.026(9) 0.022(11) 0.000 0.000 0.013(4)
O2 0.055(9) 0.071(7) 0.061(7) -0.007(6) -0.023(6) 0.025(6)
C6 0.107(12) 0.145(13) 0.106(11) -0.072(10) -0.016(9) 0.093(10)
C5 0.099(12) 0.134(12) 0.100(10) -0.058(9) -0.018(9) 0.092(10)
C4 0.066(10) 0.129(10) 0.086(10) -0.028(9) -0.013(9) 0.060(9)
C3 0.074(11) 0.115(11) 0.063(10) -0.028(9) -0.010(8) 0.049(9)
C2 0.071(10) 0.101(11) 0.065(9) -0.020(8) -0.014(8) 0.054(8)
C7 0.090(11) 0.134(13) 0.102(12) -0.054(10) -0.009(9) 0.065(10)
C1 0.061(11) 0.068(10) 0.057(10) -0.005(8) -0.012(9) 0.035(9)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 2.039(11) 5 ?
Cu1 N1 2.039(11) . ?
Cu1 Cl1 2.310(4) 5 ?
Cu1 Cl1 2.310(4) . ?
Cu1 Cl2 2.592(4) . ?
Cr1 O4 1.887(4) . ?
Cr1 O1 1.972(9) . ?
Cr1 O1 1.972(9) 10 ?
Cr1 O2 2.009(9) 11_665 ?
Cr1 O2 2.009(9) 3_665 ?
Cr1 O3 2.113(11) . ?
Cl2 Cu1 2.592(4) 3 ?
Cl2 Cu1 2.592(4) 2 ?
O1 C1 1.218(11) . ?
N1 C4 1.468(10) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
O4 Cr1 1.887(4) 2_655 ?
O4 Cr1 1.887(4) 3_665 ?
O2 C1 1.193(11) . ?
O2 Cr1 2.009(9) 2_655 ?
C6 C5 1.3900 . ?
C6 C7 1.3900 . ?
C6 H6 0.9400 . ?
C5 C4 1.3900 . ?
C5 H5 0.9400 . ?
C4 C3 1.3900 . ?
C3 C2 1.3900 . ?
C3 H3 0.9400 . ?
C2 C7 1.3900 . ?
C2 C1 1.493(15) . ?
C7 H7 0.9400 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 N1 166.0(6) 5 . ?
N1 Cu1 Cl1 89.9(3) 5 5 ?
N1 Cu1 Cl1 92.8(3) . 5 ?
N1 Cu1 Cl1 92.8(3) 5 . ?
N1 Cu1 Cl1 89.9(3) . . ?
Cl1 Cu1 Cl1 158.0(3) 5 . ?
N1 Cu1 Cl2 83.0(3) 5 . ?
N1 Cu1 Cl2 83.0(3) . . ?
Cl1 Cu1 Cl2 101.01(13) 5 . ?
Cl1 Cu1 Cl2 101.01(13) . . ?
O4 Cr1 O1 93.7(3) . . ?
O4 Cr1 O1 93.7(3) . 10 ?
O1 Cr1 O1 95.7(6) . 10 ?
O4 Cr1 O2 94.0(3) . 11_665 ?
O1 Cr1 O2 172.3(4) . 11_665 ?
O1 Cr1 O2 84.4(4) 10 11_665 ?
O4 Cr1 O2 94.0(3) . 3_665 ?
O1 Cr1 O2 84.4(4) . 3_665 ?
O1 Cr1 O2 172.3(4) 10 3_665 ?
O2 Cr1 O2 94.4(6) 11_665 3_665 ?
O4 Cr1 O3 179.9(3) . . ?
O1 Cr1 O3 86.3(3) . . ?
O1 Cr1 O3 86.3(3) 10 . ?
O2 Cr1 O3 86.1(4) 11_665 . ?
O2 Cr1 O3 86.1(4) 3_665 . ?
Cu1 Cl2 Cu1 120.0 3 . ?
Cu1 Cl2 Cu1 120.0 3 2 ?
Cu1 Cl2 Cu1 120.0 . 2 ?
C1 O1 Cr1 133.1(11) . . ?
C4 N1 Cu1 120.1(8) . . ?
C4 N1 H1A 107.3 . . ?
Cu1 N1 H1A 107.3 . . ?
C4 N1 H1B 107.3 . . ?
Cu1 N1 H1B 107.3 . . ?
H1A N1 H1B 106.9 . . ?
Cr1 O4 Cr1 120.000(1) 2_655 3_665 ?
Cr1 O4 Cr1 120.0 2_655 . ?
Cr1 O4 Cr1 120.0 3_665 . ?
C1 O2 Cr1 131.8(12) . 2_655 ?
C5 C6 C7 120.0 . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C3 C4 C5 120.0 . . ?
C3 C4 N1 122.8(11) . . ?
C5 C4 N1 117.2(11) . . ?
C2 C3 C4 120.0 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C7 C2 C3 120.0 . . ?
C7 C2 C1 123.5(11) . . ?
C3 C2 C1 116.5(11) . . ?
C2 C7 C6 120.0 . . ?
C2 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
O2 C1 O1 127.2(17) . . ?
O2 C1 C2 114.1(13) . . ?
O1 C1 C2 118.7(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Cu1 Cl2 Cu1 131.7(3) 5 . . 3 ?
N1 Cu1 Cl2 Cu1 -48.3(3) . . . 3 ?
Cl1 Cu1 Cl2 Cu1 -139.83(12) 5 . . 3 ?
Cl1 Cu1 Cl2 Cu1 40.17(12) . . . 3 ?
N1 Cu1 Cl2 Cu1 -48.3(3) 5 . . 2 ?
N1 Cu1 Cl2 Cu1 131.7(3) . . . 2 ?
Cl1 Cu1 Cl2 Cu1 40.17(12) 5 . . 2 ?
Cl1 Cu1 Cl2 Cu1 -139.83(12) . . . 2 ?
O4 Cr1 O1 C1 21.3(16) . . . . ?
O1 Cr1 O1 C1 -72.8(17) 10 . . . ?
O2 Cr1 O1 C1 -163(3) 11_665 . . . ?
O2 Cr1 O1 C1 114.9(17) 3_665 . . . ?
O3 Cr1 O1 C1 -158.7(16) . . . . ?
N1 Cu1 N1 C4 175.6(10) 5 . . . ?
Cl1 Cu1 N1 C4 -83.7(10) 5 . . . ?
Cl1 Cu1 N1 C4 74.5(9) . . . . ?
Cl2 Cu1 N1 C4 175.6(10) . . . . ?
O1 Cr1 O4 Cr1 -48.0(3) . . . 2_655 ?
O1 Cr1 O4 Cr1 48.0(3) 10 . . 2_655 ?
O2 Cr1 O4 Cr1 132.6(3) 11_665 . . 2_655 ?
O2 Cr1 O4 Cr1 -132.6(3) 3_665 . . 2_655 ?
O3 Cr1 O4 Cr1 0(100) . . . 2_655 ?
O1 Cr1 O4 Cr1 132.0(3) . . . 3_665 ?
O1 Cr1 O4 Cr1 -132.0(3) 10 . . 3_665 ?
O2 Cr1 O4 Cr1 -47.4(3) 11_665 . . 3_665 ?
O2 Cr1 O4 Cr1 47.4(3) 3_665 . . 3_665 ?
O3 Cr1 O4 Cr1 180(100) . . . 3_665 ?
C7 C6 C5 C4 0.0 . . . . ?
C6 C5 C4 C3 0.0 . . . . ?
C6 C5 C4 N1 -179.1(10) . . . . ?
Cu1 N1 C4 C3 91.7(9) . . . . ?
Cu1 N1 C4 C5 -89.2(9) . . . . ?
C5 C4 C3 C2 0.0 . . . . ?
N1 C4 C3 C2 179.1(10) . . . . ?
C4 C3 C2 C7 0.0 . . . . ?
C4 C3 C2 C1 -177.1(9) . . . . ?
C3 C2 C7 C6 0.0 . . . . ?
C1 C2 C7 C6 176.9(10) . . . . ?
C5 C6 C7 C2 0.0 . . . . ?
Cr1 O2 C1 O1 -6(3) 2_655 . . . ?
Cr1 O2 C1 C2 172.7(6) 2_655 . . . ?
Cr1 O1 C1 O2 5(3) . . . . ?
Cr1 O1 C1 C2 -173.9(6) . . . . ?
C7 C2 C1 O2 1.9(19) . . . . ?
C3 C2 C1 O2 178.9(11) . . . . ?
C7 C2 C1 O1 -179.4(12) . . . . ?
C3 C2 C1 O1 -2.4(19) . . . . ?

_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full        38.97
_diffrn_measured_fraction_theta_full 0.979
_refine_diff_density_max         0.168
_refine_diff_density_min         -0.196
_refine_diff_density_rms         0.042

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.359 -0.181 0.118 1538 411 ' '
2 0.667 0.333 0.000 225 42 ' '
3 0.667 0.333 0.500 225 42 ' '
_platon_squeeze_details          
;
Mixture of DMF and MeCN solvents have been used. 
Water can be present as well.Possible formula would therefore be 
[Cr3O(H2O)3(C7H6NO2)6Cu3Cl7]. xDMF,yMECN,zH2O 
with total number of electrons from x,y,z solvents not exceeding 248 
per formula unit.
;
_vrf_THETM01_I                   
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The lack of high angle diffraction data can be attributed to 
the presence of disordered solvent in structural cavities.  
;
_vrf_PLAT023_I                   
;
PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6]..      38.97 Deg. 
RESPONSE: The lack of high angle diffraction data can be attributed to 
the presence of disordered solvent in structural cavities.
;
_database_code_depnum_ccdc_archive 'CCDC 943025'