# 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 1008931'
_audit_update_record             
;
2014-06-18 deposited with the CCDC.
2015-06-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H50 Cl2 Cu4 N4 O30'
_chemical_formula_sum            'C32 H50 Cl2 Cu4 N4 O30'
_chemical_formula_weight         1295.82

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   8.697(6)
_cell_length_b                   25.050(17)
_cell_length_c                   11.638(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.010(10)
_cell_angle_gamma                90.00
_cell_volume                     2460(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6992
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      28.24

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1320
_exptl_absorpt_coefficient_mu    1.913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7009
_exptl_absorpt_correction_T_max  0.7246
_exptl_absorpt_process_details   'sadabs(Bruker, 1997)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       'ω and φ scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16373
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.63
_diffrn_reflns_theta_max         27.50
_reflns_number_total             5654
_reflns_number_gt                4759
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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     
'calc w=1/[σ²(Fo²)+(0.0678P)²+1.8143P] where P=(Fo²+2Fc²)/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         5654
_refine_ls_number_parameters     325
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0378
_refine_ls_wR_factor_ref         0.1118
_refine_ls_wR_factor_gt          0.1074
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_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
Cu1 Cu 0.58793(4) 0.033192(12) 0.60365(2) 0.02581(10) Uani 1 1 d . . .
Cu2 Cu 0.27507(4) 0.084852(12) 0.40521(3) 0.02484(10) Uani 1 1 d . . .
Cl1 Cl 0.75889(11) 0.10140(4) 0.60414(8) 0.0498(2) Uani 1 1 d . . .
O1 O 0.3567(2) 0.05262(9) 0.66777(17) 0.0354(5) Uani 1 1 d . . .
O2 O 0.1848(2) 0.03370(8) 0.49698(15) 0.0311(4) Uani 1 1 d . . .
O3 O 0.3407(3) -0.02152(9) 1.22751(16) 0.0385(5) Uani 1 1 d . . .
O4 O 0.1808(3) 0.04856(10) 1.22133(17) 0.0438(6) Uani 1 1 d . . .
O5 O 0.5755(2) 0.37437(9) -0.12476(18) 0.0363(5) Uani 1 1 d . . .
O6 O 0.6664(3) 0.33427(11) 0.0491(2) 0.0526(6) Uani 1 1 d . . .
O7 O 0.3624(3) 0.14424(9) 0.3320(2) 0.0457(6) Uani 1 1 d . . .
O8 O 0.5650(3) 0.10552(10) 0.2763(2) 0.0486(6) Uani 1 1 d . . .
O9 O 0.4742(2) 0.04340(7) 0.43822(14) 0.0237(4) Uani 1 1 d . . .
H99A H 0.5455 0.0567 0.3912 0.028 Uiso 1 1 calc R . .
N1 N 0.1588(3) 0.01098(10) 0.79894(19) 0.0310(5) Uani 1 1 d . . .
N2 N 0.4283(3) 0.26219(9) 0.0093(2) 0.0333(5) Uani 1 1 d . . .
C1 C 0.0971(4) 0.05014(14) 0.8518(3) 0.0393(7) Uani 1 1 d . . .
H1A H 0.0321 0.0756 0.8059 0.047 Uiso 1 1 calc R . .
C2 C 0.1290(4) 0.05315(13) 0.9736(2) 0.0366(6) Uani 1 1 d . . .
H2A H 0.0864 0.0807 1.0098 0.044 Uiso 1 1 calc R . .
C3 C 0.2247(3) 0.01499(11) 1.0416(2) 0.0266(5) Uani 1 1 d . . .
C4 C 0.2909(4) -0.02409(13) 0.9846(3) 0.0391(7) Uani 1 1 d . . .
H4A H 0.3589 -0.0494 1.0283 0.047 Uiso 1 1 calc R . .
C5 C 0.2558(4) -0.02532(14) 0.8626(3) 0.0416(7) Uani 1 1 d . . .
H5A H 0.3000 -0.0517 0.8243 0.050 Uiso 1 1 calc R . .
C6 C 0.1143(4) 0.00653(15) 0.6678(2) 0.0383(7) Uani 1 1 d . . .
H6A H 0.0101 0.0221 0.6380 0.046 Uiso 1 1 calc R . .
H6B H 0.1076 -0.0309 0.6460 0.046 Uiso 1 1 calc R . .
C7 C 0.2315(3) 0.03409(11) 0.6090(2) 0.0248(5) Uani 1 1 d . . .
C8 C 0.2506(3) 0.01485(12) 1.1761(2) 0.0279(5) Uani 1 1 d . . .
C9 C 0.3242(4) 0.26132(14) 0.0775(4) 0.0484(9) Uani 1 1 d . . .
H9A H 0.2444 0.2869 0.0668 0.058 Uiso 1 1 calc R . .
C10 C 0.3348(4) 0.22277(13) 0.1633(4) 0.0494(9) Uani 1 1 d . . .
H10A H 0.2633 0.2226 0.2112 0.059 Uiso 1 1 calc R . .
C11 C 0.4520(3) 0.18431(11) 0.1782(3) 0.0316(6) Uani 1 1 d . . .
C12 C 0.5575(4) 0.18577(13) 0.1059(3) 0.0394(7) Uani 1 1 d . . .
H12A H 0.6371 0.1603 0.1140 0.047 Uiso 1 1 calc R . .
C13 C 0.5426(4) 0.22544(13) 0.0221(3) 0.0416(7) Uani 1 1 d . . .
H13A H 0.6133 0.2267 -0.0263 0.050 Uiso 1 1 calc R . .
C14 C 0.4214(4) 0.30504(12) -0.0787(3) 0.0377(7) Uani 1 1 d . . .
H14A H 0.3274 0.3266 -0.0832 0.045 Uiso 1 1 calc R . .
H14B H 0.4141 0.2894 -0.1561 0.045 Uiso 1 1 calc R . .
C15 C 0.5688(3) 0.34056(11) -0.0451(3) 0.0319(6) Uani 1 1 d . . .
C16 C 0.4632(4) 0.14025(11) 0.2700(3) 0.0337(6) Uani 1 1 d . . .
O1W O 0.5505(5) -0.11575(16) 1.1305(3) 0.0932(12) Uani 1 1 d . . .
O2W O 0.6973(5) 0.31288(19) 0.3020(3) 0.1062(14) Uani 1 1 d . . .
O3W O 0.9356(5) 0.1510(2) 0.1255(4) 0.1203(17) Uani 1 1 d . . .
O4W O 0.6762(10) 0.1700(3) -0.1952(7) 0.191(3) Uani 1 1 d . . .
O5W O 0.4594(7) 0.2265(3) -0.3675(9) 0.216(4) Uani 1 1 d . . .
O6W O -0.0518(11) 0.1870(6) 0.9100(8) 0.293(7) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O3 1.934(2) 3_657 ?
Cu1 O9 1.957(2) . ?
Cu1 O9 2.021(2) 3_656 ?
Cu1 Cl1 2.2640(14) . ?
Cu1 O1 2.359(2) . ?
Cu1 Cu1 3.0229(14) 3_656 ?
Cu2 O2 1.951(2) . ?
Cu2 O7 1.957(2) . ?
Cu2 O5 1.971(2) 4_566 ?
Cu2 O9 1.975(2) . ?
Cu2 O4 2.287(2) 1_554 ?
O1 C7 1.228(3) . ?
O2 C7 1.268(3) . ?
O3 C8 1.255(3) . ?
O3 Cu1 1.934(2) 3_657 ?
O4 C8 1.230(4) . ?
O4 Cu2 2.287(2) 1_556 ?
O5 C15 1.268(3) . ?
O5 Cu2 1.971(2) 4_665 ?
O6 C15 1.223(4) . ?
O7 C16 1.267(4) . ?
O8 C16 1.231(4) . ?
O9 Cu1 2.021(2) 3_656 ?
O9 H99A 0.9800 . ?
N1 C5 1.336(4) . ?
N1 C1 1.337(4) . ?
N1 C6 1.486(3) . ?
N2 C13 1.337(4) . ?
N2 C9 1.341(4) . ?
N2 C14 1.475(4) . ?
C1 C2 1.379(4) . ?
C1 H1A 0.9300 . ?
C2 C3 1.384(4) . ?
C2 H2A 0.9300 . ?
C3 C4 1.384(4) . ?
C3 C8 1.526(3) . ?
C4 C5 1.378(4) . ?
C4 H4A 0.9300 . ?
C5 H5A 0.9300 . ?
C6 C7 1.523(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C9 C10 1.376(5) . ?
C9 H9A 0.9300 . ?
C10 C11 1.383(4) . ?
C10 H10A 0.9300 . ?
C11 C12 1.387(4) . ?
C11 C16 1.523(4) . ?
C12 C13 1.376(4) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 C15 1.532(4) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Cu1 O9 168.77(9) 3_657 . ?
O3 Cu1 O9 95.90(8) 3_657 3_656 ?
O9 Cu1 O9 81.08(8) . 3_656 ?
O3 Cu1 Cl1 93.57(8) 3_657 . ?
O9 Cu1 Cl1 94.54(6) . . ?
O9 Cu1 Cl1 148.68(6) 3_656 . ?
O3 Cu1 O1 78.38(9) 3_657 . ?
O9 Cu1 O1 91.01(8) . . ?
O9 Cu1 O1 94.21(8) 3_656 . ?
Cl1 Cu1 O1 116.95(7) . . ?
O3 Cu1 Cu1 134.72(8) 3_657 3_656 ?
O9 Cu1 Cu1 41.33(6) . 3_656 ?
O9 Cu1 Cu1 39.75(5) 3_656 3_656 ?
Cl1 Cu1 Cu1 128.48(4) . 3_656 ?
O1 Cu1 Cu1 93.47(6) . 3_656 ?
O2 Cu2 O7 171.08(9) . . ?
O2 Cu2 O5 89.04(10) . 4_566 ?
O7 Cu2 O5 86.95(10) . 4_566 ?
O2 Cu2 O9 89.91(9) . . ?
O7 Cu2 O9 94.01(9) . . ?
O5 Cu2 O9 178.84(8) 4_566 . ?
O2 Cu2 O4 98.66(10) . 1_554 ?
O7 Cu2 O4 89.06(11) . 1_554 ?
O5 Cu2 O4 86.54(8) 4_566 1_554 ?
O9 Cu2 O4 94.11(8) . 1_554 ?
C7 O1 Cu1 117.04(17) . . ?
C7 O2 Cu2 119.11(18) . . ?
C8 O3 Cu1 127.15(18) . 3_657 ?
C8 O4 Cu2 124.82(18) . 1_556 ?
C15 O5 Cu2 114.29(19) . 4_665 ?
C16 O7 Cu2 125.66(19) . . ?
Cu1 O9 Cu2 118.07(9) . . ?
Cu1 O9 Cu1 98.92(8) . 3_656 ?
Cu2 O9 Cu1 106.35(9) . 3_656 ?
Cu1 O9 H99A 110.9 . . ?
Cu2 O9 H99A 110.9 . . ?
Cu1 O9 H99A 110.9 3_656 . ?
C5 N1 C1 120.9(2) . . ?
C5 N1 C6 119.4(3) . . ?
C1 N1 C6 119.6(3) . . ?
C13 N2 C9 120.9(3) . . ?
C13 N2 C14 118.9(3) . . ?
C9 N2 C14 120.2(3) . . ?
N1 C1 C2 120.6(3) . . ?
N1 C1 H1A 119.7 . . ?
C2 C1 H1A 119.7 . . ?
C1 C2 C3 119.6(3) . . ?
C1 C2 H2A 120.2 . . ?
C3 C2 H2A 120.2 . . ?
C2 C3 C4 118.5(2) . . ?
C2 C3 C8 120.5(2) . . ?
C4 C3 C8 121.0(2) . . ?
C5 C4 C3 119.7(3) . . ?
C5 C4 H4A 120.1 . . ?
C3 C4 H4A 120.1 . . ?
N1 C5 C4 120.6(3) . . ?
N1 C5 H5A 119.7 . . ?
C4 C5 H5A 119.7 . . ?
N1 C6 C7 113.0(2) . . ?
N1 C6 H6A 109.0 . . ?
C7 C6 H6A 109.0 . . ?
N1 C6 H6B 109.0 . . ?
C7 C6 H6B 109.0 . . ?
H6A C6 H6B 107.8 . . ?
O1 C7 O2 126.6(2) . . ?
O1 C7 C6 121.4(2) . . ?
O2 C7 C6 112.0(2) . . ?
O4 C8 O3 127.6(2) . . ?
O4 C8 C3 118.1(2) . . ?
O3 C8 C3 114.3(2) . . ?
N2 C9 C10 120.3(3) . . ?
N2 C9 H9A 119.8 . . ?
C10 C9 H9A 119.8 . . ?
C9 C10 C11 119.8(3) . . ?
C9 C10 H10A 120.1 . . ?
C11 C10 H10A 120.1 . . ?
C10 C11 C12 118.8(3) . . ?
C10 C11 C16 120.8(3) . . ?
C12 C11 C16 120.4(3) . . ?
C13 C12 C11 119.1(3) . . ?
C13 C12 H12A 120.4 . . ?
C11 C12 H12A 120.4 . . ?
N2 C13 C12 121.0(3) . . ?
N2 C13 H13A 119.5 . . ?
C12 C13 H13A 119.5 . . ?
N2 C14 C15 110.8(2) . . ?
N2 C14 H14A 109.5 . . ?
C15 C14 H14A 109.5 . . ?
N2 C14 H14B 109.5 . . ?
C15 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
O6 C15 O5 126.6(3) . . ?
O6 C15 C14 120.7(3) . . ?
O5 C15 C14 112.7(3) . . ?
O8 C16 O7 127.5(3) . . ?
O8 C16 C11 118.5(3) . . ?
O7 C16 C11 114.0(2) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.087
#=========================================================================END  
####################################################################### 
# 
# 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 1008932'
_audit_update_record             
;
2014-06-18 deposited with the CCDC.
2015-06-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 [Ag2(L)(NO3)]-(H2O) 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H6 Ag2 N2 O7, H2 O'
_chemical_formula_sum            'C8 H8 Ag2 N2 O8'
_chemical_formula_weight         475.90

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   12.0276(11)
_cell_length_b                   5.2148(4)
_cell_length_c                   17.8366(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.7730(10)
_cell_angle_gamma                90.00
_cell_volume                     1118.20(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5185
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      27.95

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.827
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             912
_exptl_absorpt_coefficient_mu    3.547
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6556
_exptl_absorpt_correction_T_max  0.6755
_exptl_absorpt_process_details   sadabs(Bruker,1997)

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       'ω and φ scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5539
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0404
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.39
_diffrn_reflns_theta_max         25.49
_reflns_number_total             2044
_reflns_number_gt                1933
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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     
'calc w=1/[σ²(Fo²)+(0.0524P)²+3.4541P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0345(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2044
_refine_ls_number_parameters     188
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0388
_refine_ls_wR_factor_ref         0.1005
_refine_ls_wR_factor_gt          0.0990
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.063
_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
Ag1 Ag 0.90386(4) 0.84476(8) 0.40662(2) 0.0411(2) Uani 1 1 d . . .
Ag2 Ag 0.82105(3) 0.38594(7) 0.46957(2) 0.0372(2) Uani 1 1 d . . .
O1 O 0.3134(3) 0.2245(7) 0.84219(17) 0.0325(7) Uani 1 1 d . . .
O2 O 0.4098(3) -0.1083(6) 0.80021(19) 0.0337(8) Uani 1 1 d . . .
O3 O 0.7650(3) -0.0427(7) 0.49500(19) 0.0317(7) Uani 1 1 d . . .
O4 O 0.6551(3) -0.3819(7) 0.4854(2) 0.0388(9) Uani 1 1 d . . .
O5 O 1.0181(4) 1.2297(12) 0.4540(2) 0.0660(14) Uani 1 1 d . . .
O6 O 1.0721(4) 1.1385(10) 0.3466(3) 0.0680(15) Uani 1 1 d . . .
O7 O 1.1320(5) 1.4753(11) 0.4018(3) 0.088(2) Uani 1 1 d . . .
N1 N 0.4644(3) 0.1440(7) 0.6715(2) 0.0231(8) Uani 1 1 d . . .
N2 N 1.0769(3) 1.2822(9) 0.3994(2) 0.0326(9) Uani 1 1 d . . .
C1 C 0.5641(4) 0.2537(9) 0.6617(2) 0.0253(9) Uani 1 1 d . . .
H1A H 0.5849 0.3973 0.6897 0.030 Uiso 1 1 calc R . .
C2 C 0.6352(4) 0.1544(9) 0.6106(2) 0.0255(9) Uani 1 1 d . . .
H2A H 0.7034 0.2330 0.6033 0.031 Uiso 1 1 calc R . .
C3 C 0.6060(3) -0.0609(8) 0.5702(2) 0.0211(8) Uani 1 1 d . . .
C4 C 0.5046(4) -0.1745(8) 0.5834(2) 0.0235(9) Uani 1 1 d . . .
H4A H 0.4838 -0.3232 0.5578 0.028 Uiso 1 1 calc R . .
C5 C 0.4347(4) -0.0685(9) 0.6341(2) 0.0247(9) Uani 1 1 d . . .
H5A H 0.3663 -0.1447 0.6426 0.030 Uiso 1 1 calc R . .
C6 C 0.3853(4) 0.2608(10) 0.7230(2) 0.0287(10) Uani 1 1 d . . .
H6A H 0.3137 0.2782 0.6970 0.034 Uiso 1 1 calc R . .
H6B H 0.4112 0.4317 0.7361 0.034 Uiso 1 1 calc R . .
C7 C 0.3699(4) 0.1081(9) 0.7952(2) 0.0244(9) Uani 1 1 d . . .
C8 C 0.6817(4) -0.1715(9) 0.5117(2) 0.0242(9) Uani 1 1 d . . .
O1W O 0.6821(4) 0.7378(10) 0.7490(3) 0.0588(11) Uani 1 1 d D . .
H1WA H 0.651(6) 0.785(16) 0.787(3) 0.071 Uiso 1 1 d D . .
H1WB H 0.719(6) 0.846(12) 0.728(4) 0.071 Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 O2 2.266(3) 4_665 ?
Ag1 O3 2.405(3) 1_565 ?
Ag1 O5 2.561(6) . ?
Ag1 Ag2 2.8367(6) . ?
Ag1 Ag2 3.2073(6) 1_565 ?
Ag2 O1 2.343(3) 4_665 ?
Ag2 O4 2.359(4) 1_565 ?
Ag2 O3 2.382(3) . ?
Ag2 O7 2.455(5) 3_776 ?
Ag2 O5 2.529(4) 1_545 ?
Ag2 Ag1 3.2073(6) 1_545 ?
O1 C7 1.252(6) . ?
O1 Ag2 2.343(3) 4_566 ?
O2 C7 1.228(6) . ?
O2 Ag1 2.266(3) 4_566 ?
O3 C8 1.250(6) . ?
O3 Ag1 2.405(3) 1_545 ?
O4 C8 1.232(6) . ?
O4 Ag2 2.359(4) 1_545 ?
O5 N2 1.253(6) . ?
O5 Ag2 2.529(4) 1_565 ?
O6 N2 1.203(6) . ?
O7 N2 1.205(6) . ?
O7 Ag2 2.455(5) 3_776 ?
N1 C5 1.336(6) . ?
N1 C1 1.345(6) . ?
N1 C6 1.474(6) . ?
C1 C2 1.370(6) . ?
C1 H1A 0.9300 . ?
C2 C3 1.374(6) . ?
C2 H2A 0.9300 . ?
C3 C4 1.382(6) . ?
C3 C8 1.519(6) . ?
C4 C5 1.371(6) . ?
C4 H4A 0.9300 . ?
C5 H5A 0.9300 . ?
C6 C7 1.530(6) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
O1W H1WA 0.818(10) . ?
O1W H1WB 0.819(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ag1 O3 136.23(13) 4_665 1_565 ?
O2 Ag1 O5 132.26(13) 4_665 . ?
O3 Ag1 O5 88.21(12) 1_565 . ?
O2 Ag1 Ag2 83.86(9) 4_665 . ?
O3 Ag1 Ag2 71.75(8) 1_565 . ?
O5 Ag1 Ag2 136.21(10) . . ?
O2 Ag1 Ag2 142.20(9) 4_665 1_565 ?
O3 Ag1 Ag2 47.64(8) 1_565 1_565 ?
O5 Ag1 Ag2 50.50(10) . 1_565 ?
Ag2 Ag1 Ag2 119.142(19) . 1_565 ?
O1 Ag2 O4 103.54(13) 4_665 1_565 ?
O1 Ag2 O3 87.20(12) 4_665 . ?
O4 Ag2 O3 102.30(12) 1_565 . ?
O1 Ag2 O7 168.47(15) 4_665 3_776 ?
O4 Ag2 O7 84.71(19) 1_565 3_776 ?
O3 Ag2 O7 99.02(14) . 3_776 ?
O1 Ag2 O5 79.82(14) 4_665 1_545 ?
O4 Ag2 O5 167.85(17) 1_565 1_545 ?
O3 Ag2 O5 89.46(16) . 1_545 ?
O7 Ag2 O5 90.48(19) 3_776 1_545 ?
O1 Ag2 Ag1 80.05(9) 4_665 . ?
O4 Ag2 Ag1 85.60(9) 1_565 . ?
O3 Ag2 Ag1 166.33(8) . . ?
O7 Ag2 Ag1 92.75(11) 3_776 . ?
O5 Ag2 Ag1 83.49(14) 1_545 . ?
O1 Ag2 Ag1 56.46(9) 4_665 1_545 ?
O4 Ag2 Ag1 140.04(9) 1_565 1_545 ?
O3 Ag2 Ag1 48.23(7) . 1_545 ?
O7 Ag2 Ag1 121.44(16) 3_776 1_545 ?
O5 Ag2 Ag1 51.39(14) 1_545 1_545 ?
Ag1 Ag2 Ag1 119.142(19) . 1_545 ?
C7 O1 Ag2 121.6(3) . 4_566 ?
C7 O2 Ag1 122.6(3) . 4_566 ?
C8 O3 Ag2 141.6(3) . . ?
C8 O3 Ag1 127.1(3) . 1_545 ?
Ag2 O3 Ag1 84.13(10) . 1_545 ?
C8 O4 Ag2 107.0(3) . 1_545 ?
N2 O5 Ag2 124.7(3) . 1_565 ?
N2 O5 Ag1 103.0(4) . . ?
Ag2 O5 Ag1 78.11(14) 1_565 . ?
N2 O7 Ag2 112.9(4) . 3_776 ?
C5 N1 C1 120.9(4) . . ?
C5 N1 C6 119.1(4) . . ?
C1 N1 C6 120.0(4) . . ?
O6 N2 O7 124.2(6) . . ?
O6 N2 O5 117.2(5) . . ?
O7 N2 O5 118.6(5) . . ?
N1 C1 C2 120.2(4) . . ?
N1 C1 H1A 119.9 . . ?
C2 C1 H1A 119.9 . . ?
C1 C2 C3 120.2(4) . . ?
C1 C2 H2A 119.9 . . ?
C3 C2 H2A 119.9 . . ?
C2 C3 C4 118.2(4) . . ?
C2 C3 C8 121.4(4) . . ?
C4 C3 C8 120.3(4) . . ?
C5 C4 C3 120.1(4) . . ?
C5 C4 H4A 119.9 . . ?
C3 C4 H4A 119.9 . . ?
N1 C5 C4 120.3(4) . . ?
N1 C5 H5A 119.9 . . ?
C4 C5 H5A 119.9 . . ?
N1 C6 C7 114.0(4) . . ?
N1 C6 H6A 108.8 . . ?
C7 C6 H6A 108.8 . . ?
N1 C6 H6B 108.8 . . ?
C7 C6 H6B 108.8 . . ?
H6A C6 H6B 107.7 . . ?
O2 C7 O1 128.0(4) . . ?
O2 C7 C6 118.8(4) . . ?
O1 C7 C6 113.2(4) . . ?
O4 C8 O3 126.1(4) . . ?
O4 C8 C3 116.4(4) . . ?
O3 C8 C3 117.5(4) . . ?
H1WA O1W H1WB 116(9) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WA O7 0.818(10) 2.42(4) 3.183(7) 156(8) 4_586
O1W H1WB O1W 0.819(11) 2.39(5) 3.076(6) 142(8) 2_656

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        25.49
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         1.050
_refine_diff_density_min         -1.310
_refine_diff_density_rms         0.175
####################################################################### 
# 
# 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 1008934'
_audit_update_record             
;
2014-06-18 deposited with the CCDC.
2015-06-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H6 N2 O7 Pb'
_chemical_formula_sum            'C8 H6 N2 O7 Pb'
_chemical_formula_weight         449.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'

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

_cell_length_a                   4.5139(3)
_cell_length_b                   11.3181(7)
_cell_length_c                   20.4554(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1045.04(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2784
_cell_measurement_theta_min      2.663
_cell_measurement_theta_max      28.353

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.856
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             824
_exptl_absorpt_coefficient_mu    16.176
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2276
_exptl_absorpt_correction_T_max  0.3577
_exptl_absorpt_process_details   'sadabs (1997)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex CCD diffractometer'
_diffrn_measurement_method       'w and φ scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5882
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_av_sigmaI/netI    0.0747
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.99
_diffrn_reflns_theta_max         28.39
_reflns_number_total             2596
_reflns_number_gt                2395
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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     
'calc w=1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/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   0.051(17)
_refine_ls_number_reflns         2596
_refine_ls_number_parameters     163
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0327
_refine_ls_wR_factor_ref         0.0762
_refine_ls_wR_factor_gt          0.0739
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_restrained_S_all      0.953
_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
Pb1 Pb 0.36688(7) 0.58168(2) 0.946279(12) 0.02496(9) Uani 1 1 d . . .
O1 O 0.2510(13) 0.9175(5) 0.5163(3) 0.0341(13) Uani 1 1 d . . .
O2 O -0.1415(14) 0.8928(5) 0.5820(3) 0.0349(13) Uani 1 1 d . . .
O3 O -0.4395(14) 0.5344(5) 0.8313(3) 0.0374(15) Uani 1 1 d . . .
O4 O -0.0925(17) 0.6412(5) 0.8803(3) 0.0350(14) Uani 1 1 d . . .
O5 O -0.0394(17) 0.6748(6) 1.0350(4) 0.0470(18) Uani 1 1 d . . .
O6 O 0.2380(19) 0.5367(6) 1.0724(4) 0.058(2) Uani 1 1 d . . .
O7 O -0.006(2) 0.6421(8) 1.1382(4) 0.086(3) Uani 1 1 d . . .
N1 N 0.1091(18) 0.7090(5) 0.6455(3) 0.0256(13) Uani 1 1 d . . .
N2 N 0.059(2) 0.6188(6) 1.0832(4) 0.041(2) Uani 1 1 d . . .
C1 C 0.200(2) 0.7658(7) 0.7000(4) 0.033(2) Uani 1 1 d . . .
H1A H 0.3342 0.8278 0.6968 0.040 Uiso 1 1 calc R . .
C2 C 0.095(2) 0.7325(7) 0.7598(4) 0.0359(19) Uani 1 1 d . . .
H2A H 0.1575 0.7714 0.7974 0.043 Uiso 1 1 calc R . .
C3 C -0.106(2) 0.6397(6) 0.7641(4) 0.0279(16) Uani 1 1 d . . .
C4 C -0.2014(18) 0.5863(7) 0.7074(3) 0.0288(16) Uani 1 1 d . . .
H4A H -0.3405 0.5257 0.7091 0.035 Uiso 1 1 calc R . .
C5 C -0.089(2) 0.6232(6) 0.6481(4) 0.0267(16) Uani 1 1 d . . .
H5A H -0.1525 0.5874 0.6097 0.032 Uiso 1 1 calc R . .
C6 C 0.2344(18) 0.7481(7) 0.5815(4) 0.0278(16) Uani 1 1 d . . .
H6A H 0.1951 0.6881 0.5488 0.033 Uiso 1 1 calc R . .
H6B H 0.4476 0.7561 0.5856 0.033 Uiso 1 1 calc R . .
C7 C 0.1060(19) 0.8637(6) 0.5590(3) 0.0241(15) Uani 1 1 d . . .
C8 C -0.218(2) 0.6010(7) 0.8304(4) 0.0321(19) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O2 2.437(5) 3_546 ?
Pb1 O3 2.566(6) 1_655 ?
Pb1 O4 2.564(7) . ?
Pb1 O1 2.649(6) 3_646 ?
Pb1 O6 2.692(8) . ?
O1 C7 1.249(9) . ?
O1 Pb1 2.649(6) 3_656 ?
O2 C7 1.256(10) . ?
O2 Pb1 2.437(5) 3_556 ?
O3 C8 1.253(11) . ?
O3 Pb1 2.566(6) 1_455 ?
O4 C8 1.253(10) . ?
O5 N2 1.254(10) . ?
O6 N2 1.251(10) . ?
O7 N2 1.192(10) . ?
N1 C5 1.320(11) . ?
N1 C1 1.351(10) . ?
N1 C6 1.493(9) . ?
C1 C2 1.365(11) . ?
C1 H1A 0.9300 . ?
C2 C3 1.391(12) . ?
C2 H2A 0.9300 . ?
C3 C4 1.375(11) . ?
C3 C8 1.512(10) . ?
C4 C5 1.380(10) . ?
C4 H4A 0.9300 . ?
C5 H5A 0.9300 . ?
C6 C7 1.504(10) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Pb1 O3 75.0(2) 3_546 1_655 ?
O2 Pb1 O4 76.6(2) 3_546 . ?
O3 Pb1 O4 81.2(2) 1_655 . ?
O2 Pb1 O1 74.04(19) 3_546 3_646 ?
O3 Pb1 O1 84.08(19) 1_655 3_646 ?
O4 Pb1 O1 149.68(19) . 3_646 ?
O2 Pb1 O6 88.4(2) 3_546 . ?
O3 Pb1 O6 155.8(2) 1_655 . ?
O4 Pb1 O6 112.3(2) . . ?
O1 Pb1 O6 74.41(19) 3_646 . ?
C7 O1 Pb1 118.7(5) . 3_656 ?
C7 O2 Pb1 120.8(5) . 3_556 ?
C8 O3 Pb1 99.2(5) . 1_455 ?
C8 O4 Pb1 134.3(6) . . ?
N2 O6 Pb1 99.7(5) . . ?
C5 N1 C1 121.4(7) . . ?
C5 N1 C6 120.7(7) . . ?
C1 N1 C6 117.9(7) . . ?
O7 N2 O5 123.0(9) . . ?
O7 N2 O6 119.3(9) . . ?
O5 N2 O6 117.7(7) . . ?
N1 C1 C2 120.2(8) . . ?
N1 C1 H1A 119.9 . . ?
C2 C1 H1A 119.9 . . ?
C1 C2 C3 119.4(8) . . ?
C1 C2 H2A 120.3 . . ?
C3 C2 H2A 120.3 . . ?
C4 C3 C2 118.9(8) . . ?
C4 C3 C8 121.7(8) . . ?
C2 C3 C8 119.4(8) . . ?
C5 C4 C3 119.5(8) . . ?
C5 C4 H4A 120.3 . . ?
C3 C4 H4A 120.3 . . ?
N1 C5 C4 120.5(7) . . ?
N1 C5 H5A 119.7 . . ?
C4 C5 H5A 119.7 . . ?
N1 C6 C7 112.4(6) . . ?
N1 C6 H6A 109.1 . . ?
C7 C6 H6A 109.1 . . ?
N1 C6 H6B 109.1 . . ?
C7 C6 H6B 109.1 . . ?
H6A C6 H6B 107.9 . . ?
O2 C7 O1 126.9(7) . . ?
O2 C7 C6 117.1(6) . . ?
O1 C7 C6 115.9(7) . . ?
O3 C8 O4 124.6(7) . . ?
O3 C8 C3 116.9(8) . . ?
O4 C8 C3 118.4(8) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.39
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.649
_refine_diff_density_min         -1.872
_refine_diff_density_rms         0.240
####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1008935'
_audit_update_record             
;
2014-06-18 deposited with the CCDC.
2015-06-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H28 Br2 N4 O18 Pb3'
_chemical_formula_sum            'C32 H28 Br2 N4 O18 Pb3'
_chemical_formula_weight         1537.97

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

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

_cell_length_a                   24.044(3)
_cell_length_b                   10.7102(14)
_cell_length_c                   16.138(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.264(2)
_cell_angle_gamma                90.00
_cell_volume                     3898.4(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5903
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      27.42

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.620
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2832
_exptl_absorpt_coefficient_mu    15.057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3144
_exptl_absorpt_correction_T_max  0.3443
_exptl_absorpt_process_details   'sadabs (1997, Bruker)'
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apec CCD'
_diffrn_measurement_method       'ω and φ'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9544
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_sigmaI/netI    0.0594
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.81
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3389
_reflns_number_gt                2845
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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     
'calc w=1/[σ²(Fo²)+(0.1727P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3389
_refine_ls_number_parameters     273
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0658
_refine_ls_wR_factor_ref         0.2161
_refine_ls_wR_factor_gt          0.2075
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_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
Pb1 Pb 0.0000 1.30940(6) 0.2500 0.0244(3) Uani 1 2 d S . .
Pb2 Pb 0.15838(2) 1.31055(4) 0.43373(3) 0.0243(3) Uani 1 1 d . . .
O1 O 0.1641(4) 0.5475(9) 0.5067(7) 0.038(2) Uani 1 1 d . . .
O1W O 0.2026(5) 1.2123(10) 0.3158(8) 0.042(3) Uani 1 1 d D . .
H1WA H 0.184(6) 1.153(10) 0.287(10) 0.050 Uiso 1 1 d D . .
H1WB H 0.237(2) 1.189(13) 0.332(12) 0.050 Uiso 1 1 d D . .
O2 O 0.1855(4) 0.3776(8) 0.5922(7) 0.038(2) Uani 1 1 d . . .
O3 O 0.1334(4) 1.1241(8) 0.5219(7) 0.037(2) Uani 1 1 d . . .
O4 O 0.2257(4) 1.1262(8) 0.5221(7) 0.035(2) Uani 1 1 d . . .
O5 O -0.0221(4) 1.2398(9) 0.4151(6) 0.032(2) Uani 1 1 d . . .
O6 O 0.0489(4) 1.3737(9) 0.4174(6) 0.032(2) Uani 1 1 d . . .
O7 O -0.1431(5) 1.0247(10) 0.6889(10) 0.059(4) Uani 1 1 d . . .
O8 O -0.0831(4) 0.8713(10) 0.6809(7) 0.040(2) Uani 1 1 d . . .
N1 N 0.2081(4) 0.7065(9) 0.6414(7) 0.022(2) Uani 1 1 d . . .
N2 N 0.0043(5) 1.2464(9) 0.5919(7) 0.025(2) Uani 1 1 d . . .
C1 C 0.1563(6) 0.7649(12) 0.6254(10) 0.028(3) Uani 1 1 d . . .
H1A H 0.1256 0.7238 0.6367 0.034 Uiso 1 1 calc R . .
C2 C 0.1475(6) 0.8837(12) 0.5929(10) 0.033(3) Uani 1 1 d . . .
H2A H 0.1108 0.9219 0.5804 0.040 Uiso 1 1 calc R . .
C3 C 0.1932(6) 0.9464(11) 0.5787(9) 0.026(3) Uani 1 1 d . . .
C4 C 0.2470(6) 0.8861(12) 0.5962(11) 0.037(4) Uani 1 1 d . . .
H4A H 0.2781 0.9255 0.5851 0.045 Uiso 1 1 calc R . .
C5 C 0.2536(6) 0.7666(13) 0.6303(11) 0.037(4) Uani 1 1 d . . .
H5A H 0.2904 0.7275 0.6458 0.044 Uiso 1 1 calc R . .
C6 C 0.2131(6) 0.5736(11) 0.6654(9) 0.029(3) Uani 1 1 d . . .
H6A H 0.1928 0.5568 0.7067 0.034 Uiso 1 1 calc R . .
H6B H 0.2545 0.5507 0.6931 0.034 Uiso 1 1 calc R . .
C7 C 0.1844(5) 0.4968(12) 0.5789(10) 0.029(3) Uani 1 1 d . . .
C8 C 0.1841(5) 1.0751(11) 0.5387(8) 0.025(3) Uani 1 1 d . . .
C9 C 0.0195(6) 1.1240(13) 0.5988(10) 0.035(3) Uani 1 1 d . . .
H9A H 0.0520 1.0977 0.5847 0.042 Uiso 1 1 calc R . .
C10 C -0.0126(6) 1.0398(12) 0.6262(10) 0.030(3) Uani 1 1 d . . .
H10A H -0.0018 0.9560 0.6312 0.036 Uiso 1 1 calc R . .
C11 C -0.0616(5) 1.0783(12) 0.6470(8) 0.025(3) Uani 1 1 d . . .
C12 C -0.0738(7) 1.2057(13) 0.6422(12) 0.039(4) Uani 1 1 d . . .
H12A H -0.1048 1.2355 0.6586 0.047 Uiso 1 1 calc R . .
C13 C -0.0409(6) 1.2867(12) 0.6141(11) 0.033(3) Uani 1 1 d . . .
H13A H -0.0500 1.3714 0.6103 0.040 Uiso 1 1 calc R . .
C14 C 0.0375(6) 1.3322(12) 0.5536(10) 0.031(3) Uani 1 1 d . . .
H14A H 0.0797 1.3171 0.5809 0.037 Uiso 1 1 calc R . .
H14B H 0.0297 1.4181 0.5652 0.037 Uiso 1 1 calc R . .
C15 C 0.0180(5) 1.3102(10) 0.4523(9) 0.024(3) Uani 1 1 d . . .
C16 C -0.0995(6) 0.9841(12) 0.6756(10) 0.032(3) Uani 1 1 d . . .
Br1 Br -0.09222(6) 1.48902(12) 0.24552(9) 0.0350(4) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O6 2.637(10) . ?
Pb1 O6 2.637(10) 2 ?
Pb1 O8 2.727(9) 5_576 ?
Pb1 O8 2.727(9) 6_575 ?
Pb1 Br1 2.9175(13) 2 ?
Pb1 Br1 2.9175(13) . ?
Pb2 O2 2.515(11) 1_565 ?
Pb2 O4 2.636(9) . ?
Pb2 O3 2.639(9) . ?
Pb2 O6 2.640(8) . ?
Pb2 O1W 2.693(11) . ?
Pb2 O4 2.713(9) 7_576 ?
O1 C7 1.223(16) . ?
O1W H1WA 0.821(10) . ?
O1W H1WB 0.820(11) . ?
O2 C7 1.293(16) . ?
O2 Pb2 2.515(11) 1_545 ?
O3 C8 1.267(15) . ?
O4 C8 1.248(14) . ?
O4 Pb2 2.713(9) 7_576 ?
O5 C15 1.207(15) . ?
O6 C15 1.275(14) . ?
O7 C16 1.221(16) . ?
O8 C16 1.265(17) . ?
O8 Pb1 2.727(9) 5_576 ?
N1 C5 1.335(16) . ?
N1 C1 1.335(15) . ?
N1 C6 1.470(15) . ?
N2 C13 1.328(17) . ?
N2 C9 1.355(19) . ?
N2 C14 1.485(16) . ?
C1 C2 1.364(19) . ?
C1 H1A 0.9300 . ?
C2 C3 1.373(17) . ?
C2 H2A 0.9300 . ?
C3 C4 1.384(18) . ?
C3 C8 1.505(17) . ?
C4 C5 1.381(19) . ?
C4 H4A 0.9300 . ?
C5 H5A 0.9300 . ?
C6 C7 1.560(19) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C9 C10 1.36(2) . ?
C9 H9A 0.9300 . ?
C10 C11 1.396(18) . ?
C10 H10A 0.9300 . ?
C11 C12 1.392(18) . ?
C11 C16 1.533(18) . ?
C12 C13 1.35(2) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 C15 1.56(2) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Pb1 O6 149.7(4) . 2 ?
O6 Pb1 O8 76.3(3) . 5_576 ?
O6 Pb1 O8 127.5(3) 2 5_576 ?
O6 Pb1 O8 127.5(3) . 6_575 ?
O6 Pb1 O8 76.3(3) 2 6_575 ?
O8 Pb1 O8 89.6(4) 5_576 6_575 ?
O6 Pb1 Br1 74.73(18) . 2 ?
O6 Pb1 Br1 85.3(2) 2 2 ?
O8 Pb1 Br1 90.9(2) 5_576 2 ?
O8 Pb1 Br1 157.1(2) 6_575 2 ?
O6 Pb1 Br1 85.3(2) . . ?
O6 Pb1 Br1 74.73(18) 2 . ?
O8 Pb1 Br1 157.1(2) 5_576 . ?
O8 Pb1 Br1 90.9(2) 6_575 . ?
Br1 Pb1 Br1 97.49(5) 2 . ?
O2 Pb2 O4 76.7(3) 1_565 . ?
O2 Pb2 O3 72.3(3) 1_565 . ?
O4 Pb2 O3 49.7(3) . . ?
O2 Pb2 O6 85.8(3) 1_565 . ?
O4 Pb2 O6 130.5(3) . . ?
O3 Pb2 O6 81.0(3) . . ?
O2 Pb2 O1W 143.4(3) 1_565 . ?
O4 Pb2 O1W 76.8(3) . . ?
O3 Pb2 O1W 107.7(3) . . ?
O6 Pb2 O1W 130.8(3) . . ?
O2 Pb2 O4 77.4(3) 1_565 7_576 ?
O4 Pb2 O4 70.3(3) . 7_576 ?
O3 Pb2 O4 116.9(3) . 7_576 ?
O6 Pb2 O4 149.3(3) . 7_576 ?
O1W Pb2 O4 70.3(3) . 7_576 ?
Pb2 O1W H1WA 115(10) . . ?
Pb2 O1W H1WB 120(10) . . ?
H1WA O1W H1WB 104(10) . . ?
C7 O2 Pb2 97.5(9) . 1_545 ?
C8 O3 Pb2 92.7(7) . . ?
C8 O4 Pb2 93.3(7) . . ?
C8 O4 Pb2 151.6(9) . 7_576 ?
Pb2 O4 Pb2 109.7(3) . 7_576 ?
C15 O6 Pb1 101.0(8) . . ?
C15 O6 Pb2 122.2(8) . . ?
Pb1 O6 Pb2 96.4(3) . . ?
C16 O8 Pb1 150.8(9) . 5_576 ?
C5 N1 C1 120.1(11) . . ?
C5 N1 C6 120.3(10) . . ?
C1 N1 C6 119.5(10) . . ?
C13 N2 C9 121.0(11) . . ?
C13 N2 C14 121.2(11) . . ?
C9 N2 C14 117.6(10) . . ?
N1 C1 C2 121.4(11) . . ?
N1 C1 H1A 119.3 . . ?
C2 C1 H1A 119.3 . . ?
C1 C2 C3 119.6(11) . . ?
C1 C2 H2A 120.2 . . ?
C3 C2 H2A 120.2 . . ?
C2 C3 C4 118.9(11) . . ?
C2 C3 C8 120.9(11) . . ?
C4 C3 C8 120.1(11) . . ?
C5 C4 C3 119.0(11) . . ?
C5 C4 H4A 120.5 . . ?
C3 C4 H4A 120.5 . . ?
N1 C5 C4 120.8(11) . . ?
N1 C5 H5A 119.6 . . ?
C4 C5 H5A 119.6 . . ?
N1 C6 C7 107.7(11) . . ?
N1 C6 H6A 110.2 . . ?
C7 C6 H6A 110.2 . . ?
N1 C6 H6B 110.2 . . ?
C7 C6 H6B 110.2 . . ?
H6A C6 H6B 108.5 . . ?
O1 C7 O2 125.0(13) . . ?
O1 C7 C6 121.7(12) . . ?
O2 C7 C6 113.3(12) . . ?
O4 C8 O3 123.7(11) . . ?
O4 C8 C3 119.0(11) . . ?
O3 C8 C3 117.3(10) . . ?
N2 C9 C10 120.2(12) . . ?
N2 C9 H9A 119.9 . . ?
C10 C9 H9A 119.9 . . ?
C9 C10 C11 120.3(12) . . ?
C9 C10 H10A 119.8 . . ?
C11 C10 H10A 119.8 . . ?
C12 C11 C10 117.1(12) . . ?
C12 C11 C16 121.7(12) . . ?
C10 C11 C16 121.2(11) . . ?
C13 C12 C11 120.7(13) . . ?
C13 C12 H12A 119.6 . . ?
C11 C12 H12A 119.6 . . ?
N2 C13 C12 120.6(12) . . ?
N2 C13 H13A 119.7 . . ?
C12 C13 H13A 119.7 . . ?
N2 C14 C15 109.5(11) . . ?
N2 C14 H14A 109.8 . . ?
C15 C14 H14A 109.8 . . ?
N2 C14 H14B 109.8 . . ?
C15 C14 H14B 109.8 . . ?
H14A C14 H14B 108.2 . . ?
O5 C15 O6 127.1(13) . . ?
O5 C15 C14 121.0(11) . . ?
O6 C15 C14 111.9(10) . . ?
O7 C16 O8 126.5(12) . . ?
O7 C16 C11 117.0(12) . . ?
O8 C16 C11 116.4(11) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WA O7 0.821(10) 2.23(12) 2.901(15) 139(16) 5_576
O1W H1WB O2 0.820(11) 1.98(7) 2.759(15) 160(18) 7_566

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         3.738
_refine_diff_density_min         -3.940
_refine_diff_density_rms         0.544
####################################################################### 
# 
# 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_6
_database_code_depnum_ccdc_archive 'CCDC 1008936'
_audit_update_record             
;
2014-06-18 deposited with the CCDC.
2015-06-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H16 N3 O13 Pr'
_chemical_formula_sum            'C16 H16 N3 O13 Pr'
_chemical_formula_weight         599.23

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/4, y+1/4, z+1/4'
'x+1/4, -y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/4, y+3/4, z+3/4'
'x+1/4, -y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+3/4, y+1/4, z+3/4'
'x+3/4, -y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+3/4, y+3/4, z+1/4'
'x+3/4, -y+3/4, z+1/4'

_cell_length_a                   10.5744(5)
_cell_length_b                   39.183(3)
_cell_length_c                   9.2768(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3843.7(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    108(2)
_cell_measurement_reflns_used    2842
_cell_measurement_theta_min      2.9609
_cell_measurement_theta_max      28.4790

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.071
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2368
_exptl_absorpt_coefficient_mu    2.617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6646
_exptl_absorpt_correction_T_max  0.7272
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      108(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.2563
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6597
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.97
_diffrn_reflns_theta_max         27.50
_reflns_number_total             2140
_reflns_number_gt                2082
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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     
'calc w=1/[σ²(Fo²)+(0.0392P)²+5.0171P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_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   0.018(18)
_refine_ls_number_reflns         2140
_refine_ls_number_parameters     159
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0249
_refine_ls_wR_factor_ref         0.0626
_refine_ls_wR_factor_gt          0.0617
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.094
_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
Pr1 Pr 0.2500 0.2500 0.40098(6) 0.00711(8) Uani 1 2 d S . .
O1W O 0.4697(3) 0.23157(8) 0.3736(3) 0.0127(5) Uani 1 1 d D . .
O3 O 0.2113(3) 0.19335(8) 0.4934(3) 0.0216(6) Uani 1 1 d . . .
O4 O 0.3252(3) 0.15520(8) 0.3670(4) 0.0296(7) Uani 1 1 d . . .
O2 O -0.1222(2) 0.06311(7) 0.7507(3) 0.0127(5) Uani 1 1 d . . .
O1 O -0.0876(2) 0.02958(7) 0.9414(3) 0.0130(6) Uani 1 1 d . . .
O5 O 0.1478(3) 0.25363(7) 0.6600(3) 0.0133(6) Uani 1 1 d . . .
O6 O 0.2500 0.2500 0.8638(4) 0.0187(11) Uani 1 2 d S . .
N1 N 0.1251(3) 0.08330(8) 0.7360(3) 0.0095(6) Uani 1 1 d . . .
N2 N 0.2500 0.2500 0.7313(5) 0.0091(10) Uani 1 2 d S . .
C1 C 0.1794(3) 0.07589(10) 0.6086(4) 0.0124(7) Uani 1 1 d . . .
H1A H 0.1913 0.0528 0.5809 0.015 Uiso 1 1 calc R . .
C2 C 0.2176(4) 0.10177(10) 0.5186(4) 0.0133(7) Uani 1 1 d . . .
H2A H 0.2558 0.0966 0.4285 0.016 Uiso 1 1 calc R . .
C3 C 0.2003(4) 0.13541(10) 0.5594(4) 0.0135(8) Uani 1 1 d . . .
C4 C 0.1394(3) 0.14235(10) 0.6894(4) 0.0120(8) Uani 1 1 d . . .
H4A H 0.1229 0.1653 0.7171 0.014 Uiso 1 1 calc R . .
C5 C 0.1034(3) 0.11587(9) 0.7770(4) 0.0116(7) Uani 1 1 d . . .
H5A H 0.0633 0.1204 0.8665 0.014 Uiso 1 1 calc R . .
C8 C 0.2511(3) 0.16352(12) 0.4623(5) 0.0156(9) Uani 1 1 d . . .
C6 C 0.0893(3) 0.05528(10) 0.8355(4) 0.0113(7) Uani 1 1 d . . .
H6A H 0.1200 0.0608 0.9336 0.014 Uiso 1 1 calc R . .
H6B H 0.1317 0.0340 0.8042 0.014 Uiso 1 1 calc R . .
C7 C -0.0535(3) 0.04920(9) 0.8411(4) 0.0098(7) Uani 1 1 d . . .
H1WA H 0.493(4) 0.2134(9) 0.408(7) 0.03(2) Uiso 1 1 d D . .
H1WB H 0.512(5) 0.237(2) 0.304(5) 0.041(19) Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pr1 O3 2.414(3) . ?
Pr1 O3 2.414(3) 14 ?
Pr1 O1 2.446(3) 4_554 ?
Pr1 O1 2.446(3) 3_554 ?
Pr1 O1W 2.446(3) 14 ?
Pr1 O1W 2.446(3) . ?
Pr1 O5 2.639(3) 14 ?
Pr1 O5 2.639(3) . ?
O1W H1WA 0.82(2) . ?
O1W H1WB 0.82(2) . ?
O3 C8 1.275(6) . ?
O4 C8 1.226(6) . ?
O2 C7 1.236(5) . ?
O1 C7 1.260(4) . ?
O1 Pr1 2.446(3) 7_545 ?
O5 N2 1.275(4) . ?
O6 N2 1.230(6) . ?
N1 C1 1.346(5) . ?
N1 C5 1.351(5) . ?
N1 C6 1.483(5) . ?
N2 O5 1.275(4) 14 ?
C1 C2 1.374(5) . ?
C1 H1A 0.9500 . ?
C2 C3 1.384(6) . ?
C2 H2A 0.9500 . ?
C3 C4 1.393(5) . ?
C3 C8 1.521(6) . ?
C4 C5 1.372(5) . ?
C4 H4A 0.9500 . ?
C5 H5A 0.9500 . ?
C6 C7 1.529(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?

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
O3 Pr1 O3 138.42(15) . 14 ?
O3 Pr1 O1 77.42(10) . 4_554 ?
O3 Pr1 O1 141.45(10) 14 4_554 ?
O3 Pr1 O1 141.46(10) . 3_554 ?
O3 Pr1 O1 77.42(10) 14 3_554 ?
O1 Pr1 O1 74.70(13) 4_554 3_554 ?
O3 Pr1 O1W 98.46(11) . 14 ?
O3 Pr1 O1W 85.79(11) 14 14 ?
O1 Pr1 O1W 72.40(9) 4_554 14 ?
O1 Pr1 O1W 97.89(9) 3_554 14 ?
O3 Pr1 O1W 85.79(11) . . ?
O3 Pr1 O1W 98.46(11) 14 . ?
O1 Pr1 O1W 97.89(9) 4_554 . ?
O1 Pr1 O1W 72.40(9) 3_554 . ?
O1W Pr1 O1W 168.08(14) 14 . ?
O3 Pr1 O5 72.34(9) . 14 ?
O3 Pr1 O5 69.93(9) 14 14 ?
O1 Pr1 O5 148.60(8) 4_554 14 ?
O1 Pr1 O5 126.46(9) 3_554 14 ?
O1W Pr1 O5 119.97(10) 14 14 ?
O1W Pr1 O5 71.91(10) . 14 ?
O3 Pr1 O5 69.93(9) . . ?
O3 Pr1 O5 72.34(9) 14 . ?
O1 Pr1 O5 126.46(9) 4_554 . ?
O1 Pr1 O5 148.60(8) 3_554 . ?
O1W Pr1 O5 71.91(10) 14 . ?
O1W Pr1 O5 119.97(10) . . ?
O5 Pr1 O5 48.81(13) 14 . ?
Pr1 O1W H1WA 120(3) . . ?
Pr1 O1W H1WB 122(4) . . ?
H1WA O1W H1WB 112(6) . . ?
C8 O3 Pr1 135.0(3) . . ?
C7 O1 Pr1 140.1(2) . 7_545 ?
N2 O5 Pr1 96.8(2) . . ?
C1 N1 C5 121.6(3) . . ?
C1 N1 C6 119.7(3) . . ?
C5 N1 C6 118.7(3) . . ?
O6 N2 O5 121.2(2) . 14 ?
O6 N2 O5 121.2(2) . . ?
O5 N2 O5 117.6(5) 14 . ?
N1 C1 C2 120.0(4) . . ?
N1 C1 H1A 120.0 . . ?
C2 C1 H1A 120.0 . . ?
C1 C2 C3 119.8(4) . . ?
C1 C2 H2A 120.1 . . ?
C3 C2 H2A 120.1 . . ?
C2 C3 C4 119.0(4) . . ?
C2 C3 C8 118.8(4) . . ?
C4 C3 C8 122.3(4) . . ?
C5 C4 C3 119.5(4) . . ?
C5 C4 H4A 120.2 . . ?
C3 C4 H4A 120.2 . . ?
N1 C5 C4 120.0(3) . . ?
N1 C5 H5A 120.0 . . ?
C4 C5 H5A 120.0 . . ?
O4 C8 O3 128.1(4) . . ?
O4 C8 C3 117.4(4) . . ?
O3 C8 C3 114.4(4) . . ?
N1 C6 C7 112.9(3) . . ?
N1 C6 H6A 109.0 . . ?
C7 C6 H6A 109.0 . . ?
N1 C6 H6B 109.0 . . ?
C7 C6 H6B 109.0 . . ?
H6A C6 H6B 107.8 . . ?
O2 C7 O1 126.9(3) . . ?
O2 C7 C6 119.3(3) . . ?
O1 C7 C6 113.8(3) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.095
#=========================================================================END  
