# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_1L
_database_code_depnum_ccdc_archive 'CCDC 1041356'
_audit_update_record             
;
2015-04-10 deposited with the CCDC.
2015-04-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H27 N7 O3'
_chemical_formula_sum            'C30 H27 N7 O3'

_chemical_formula_weight         533.59

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'

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                   19.7331(5)
_cell_length_b                   14.8638(5)
_cell_length_c                   19.2351(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.017(2)
_cell_angle_gamma                90.00
_cell_volume                     5555.8(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1004
_cell_measurement_theta_min      2.54
_cell_measurement_theta_max      22.10

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2240.0
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.975
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_process_details   SADBAS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            37111
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.72
_diffrn_reflns_theta_max         28.21
_reflns_number_total             6812
_reflns_number_gt                3510
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0786P)²+0.4630P] 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         6812
_refine_ls_number_parameters     361
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1086
_refine_ls_R_factor_gt           0.0531
_refine_ls_wR_factor_ref         0.1557
_refine_ls_wR_factor_gt          0.1301
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001

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
C12 C 1.11995(10) 0.22918(11) 1.01553(9) 0.0659(5) Uani 1 1 d . . .
H12A H 1.1638 0.2470 1.0037 0.079 Uiso 1 1 calc R . .
H12B H 1.1221 0.1652 1.0257 0.079 Uiso 1 1 calc R . .
N1 N 1.04581(7) 0.25590(8) 1.10699(7) 0.0521(4) Uani 1 1 d . . .
C24 C 0.84778(8) 0.12164(10) 0.97754(9) 0.0551(4) Uani 1 1 d . . .
C3 C 0.91805(9) 0.48250(10) 1.05175(9) 0.0603(5) Uani 1 1 d . . .
C11 C 1.10865(9) 0.27978(11) 1.08101(9) 0.0615(5) Uani 1 1 d . . .
H11A H 1.1477 0.2688 1.1183 0.074 Uiso 1 1 calc R . .
H11B H 1.1076 0.3437 1.0708 0.074 Uiso 1 1 calc R . .
C14 C 0.97634(9) 0.21087(11) 0.85581(9) 0.0577(4) Uani 1 1 d . . .
C13 C 1.02961(9) 0.18146(11) 0.91767(9) 0.0612(5) Uani 1 1 d . . .
C22 C 0.98282(10) 0.12242(11) 1.14490(9) 0.0679(5) Uani 1 1 d . . .
H22A H 0.9917 0.0685 1.1734 0.081 Uiso 1 1 calc R . .
H22B H 0.9576 0.1640 1.1698 0.081 Uiso 1 1 calc R . .
C23 C 0.89247(9) 0.15443(10) 1.04420(9) 0.0578(4) Uani 1 1 d . . .
C4 C 0.85735(9) 0.47132(10) 0.99423(9) 0.0571(4) Uani 1 1 d . . .
C7 C 0.74623(10) 0.46124(12) 0.88410(9) 0.0679(5) Uani 1 1 d . . .
C25 C 0.85488(10) 0.03964(11) 0.94555(10) 0.0738(6) Uani 1 1 d . . .
H25 H 0.8911 0.0018 0.9640 0.089 Uiso 1 1 calc R . .
C2 C 1.01116(9) 0.41323(11) 1.13294(9) 0.0654(5) Uani 1 1 d . . .
H2A H 1.0026 0.4512 1.1715 0.079 Uiso 1 1 calc R . .
H2B H 1.0482 0.4400 1.1128 0.079 Uiso 1 1 calc R . .
C5 C 0.80431(9) 0.53363(11) 0.98793(9) 0.0664(5) Uani 1 1 d . . .
H5 H 0.8061 0.5795 1.0211 0.080 Uiso 1 1 calc R . .
C17 C 0.87704(10) 0.25725(14) 0.73923(10) 0.0719(5) Uani 1 1 d . . .
C21 C 1.05120(9) 0.16496(10) 1.13713(9) 0.0650(5) Uani 1 1 d . . .
H21A H 1.0803 0.1673 1.1833 0.078 Uiso 1 1 calc R . .
H21B H 1.0737 0.1265 1.1074 0.078 Uiso 1 1 calc R . .
C6 C 0.74895(10) 0.52871(12) 0.93324(10) 0.0699(5) Uani 1 1 d . . .
H6 H 0.7137 0.5709 0.9297 0.084 Uiso 1 1 calc R . .
C1 C 1.03244(9) 0.32028(11) 1.16087(9) 0.0621(5) Uani 1 1 d . . .
H1A H 1.0737 0.3258 1.1963 0.075 Uiso 1 1 calc R . .
H1B H 0.9964 0.2962 1.1840 0.075 Uiso 1 1 calc R . .
C27 C 0.75499(9) 0.06857(12) 0.85841(9) 0.0639(5) Uani 1 1 d . . .
C15 C 0.96417(11) 0.29823(13) 0.83567(12) 0.0881(7) Uani 1 1 d . . .
H15 H 0.9895 0.3435 0.8616 0.106 Uiso 1 1 calc R . .
C29 C 0.79394(10) 0.17622(11) 0.94766(11) 0.0762(6) Uani 1 1 d . . .
H29 H 0.7888 0.2322 0.9678 0.091 Uiso 1 1 calc R . .
C9 C 0.85376(12) 0.40376(12) 0.94480(10) 0.0808(6) Uani 1 1 d . . .
H9 H 0.8887 0.3612 0.9487 0.097 Uiso 1 1 calc R . .
C28 C 0.74776(10) 0.15054(12) 0.88922(11) 0.0769(6) Uani 1 1 d . . .
H28 H 0.7117 0.1885 0.8706 0.092 Uiso 1 1 calc R . .
C30 C 0.70567(11) 0.04214(13) 0.79784(12) 0.0833(6) Uani 1 1 d . . .
C26 C 0.80896(11) 0.01320(12) 0.88662(10) 0.0822(6) Uani 1 1 d . . .
H26 H 0.8144 -0.0422 0.8658 0.099 Uiso 1 1 calc R . .
C8 C 0.79909(13) 0.39840(13) 0.88967(10) 0.0873(7) Uani 1 1 d . . .
H8 H 0.7975 0.3529 0.8563 0.105 Uiso 1 1 calc R . .
C10 C 0.68985(12) 0.45586(13) 0.82539(11) 0.0796(6) Uani 1 1 d . . .
C20 C 0.82667(12) 0.28109(16) 0.67828(12) 0.0888(6) Uani 1 1 d . . .
C19 C 0.93697(13) 0.14691(13) 0.81598(12) 0.1013(8) Uani 1 1 d . . .
H19 H 0.9435 0.0865 0.8279 0.122 Uiso 1 1 calc R . .
C16 C 0.91538(12) 0.32148(14) 0.77800(13) 0.0987(8) Uani 1 1 d . . .
H16 H 0.9087 0.3817 0.7656 0.118 Uiso 1 1 calc R . .
C18 C 0.88785(13) 0.17052(16) 0.75840(12) 0.1047(8) Uani 1 1 d . . .
H18 H 0.8619 0.1258 0.7325 0.126 Uiso 1 1 calc R . .
N4 N 0.94031(7) 0.09907(8) 1.07815(7) 0.0620(4) Uani 1 1 d . . .
H4N H 0.9461 0.0476 1.0597 0.074 Uiso 1 1 calc R . .
N3 N 1.06602(8) 0.24554(8) 0.95507(7) 0.0626(4) Uani 1 1 d . . .
H3N H 1.0571 0.3005 0.9427 0.075 Uiso 1 1 calc R . .
N2 N 0.94982(7) 0.40871(8) 1.07968(7) 0.0613(4) Uani 1 1 d . . .
H2N H 0.9334 0.3569 1.0657 0.074 Uiso 1 1 calc R . .
O3 O 0.88228(6) 0.23014(7) 1.06697(7) 0.0740(4) Uani 1 1 d . . .
O1 O 0.93826(7) 0.55843(7) 1.07142(7) 0.0919(5) Uani 1 1 d . . .
O2 O 1.03844(8) 0.10087(8) 0.93150(8) 0.0950(5) Uani 1 1 d . . .
N6 N 0.78658(11) 0.29919(17) 0.62997(11) 0.1180(7) Uani 1 1 d . . .
N7 N 0.66494(11) 0.02420(13) 0.75000(12) 0.1187(8) Uani 1 1 d . . .
N5 N 0.64588(11) 0.45200(13) 0.77793(10) 0.1029(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
C12 N3 1.454(2) . ?
C12 C11 1.516(2) . ?
N1 C11 1.459(2) . ?
N1 C1 1.468(2) . ?
N1 C21 1.4673(19) . ?
C24 C29 1.380(2) . ?
C24 C25 1.383(2) . ?
C24 C23 1.505(2) . ?
C3 O1 1.2344(18) . ?
C3 N2 1.3294(19) . ?
C3 C4 1.492(2) . ?
C14 C15 1.364(2) . ?
C14 C19 1.374(2) . ?
C14 C13 1.509(2) . ?
C13 O2 1.2329(18) . ?
C13 N3 1.327(2) . ?
C22 N4 1.449(2) . ?
C22 C21 1.521(3) . ?
C23 O3 1.2366(18) . ?
C23 N4 1.334(2) . ?
C4 C9 1.376(2) . ?
C4 C5 1.387(2) . ?
C7 C6 1.373(2) . ?
C7 C8 1.390(3) . ?
C7 C10 1.443(3) . ?
C25 C26 1.380(2) . ?
C2 N2 1.445(2) . ?
C2 C1 1.515(2) . ?
C5 C6 1.381(2) . ?
C17 C18 1.348(3) . ?
C17 C16 1.358(3) . ?
C17 C20 1.443(3) . ?
C27 C28 1.373(2) . ?
C27 C26 1.380(2) . ?
C27 C30 1.437(3) . ?
C15 C16 1.380(3) . ?
C29 C28 1.372(2) . ?
C9 C8 1.377(3) . ?
C30 N7 1.143(2) . ?
C10 N5 1.146(2) . ?
C20 N6 1.143(3) . ?
C19 C18 1.384(3) . ?

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
N3 C12 C11 112.86(14) . . ?
C11 N1 C1 110.56(13) . . ?
C11 N1 C21 110.60(13) . . ?
C1 N1 C21 109.33(13) . . ?
C29 C24 C25 117.57(16) . . ?
C29 C24 C23 117.32(15) . . ?
C25 C24 C23 125.07(15) . . ?
O1 C3 N2 121.74(15) . . ?
O1 C3 C4 120.27(14) . . ?
N2 C3 C4 117.98(13) . . ?
N1 C11 C12 114.86(14) . . ?
C15 C14 C19 116.47(17) . . ?
C15 C14 C13 124.32(15) . . ?
C19 C14 C13 119.21(16) . . ?
O2 C13 N3 122.52(17) . . ?
O2 C13 C14 120.30(15) . . ?
N3 C13 C14 117.17(14) . . ?
N4 C22 C21 113.53(15) . . ?
O3 C23 N4 122.19(16) . . ?
O3 C23 C24 119.27(15) . . ?
N4 C23 C24 118.49(14) . . ?
C9 C4 C5 118.65(16) . . ?
C9 C4 C3 122.14(16) . . ?
C5 C4 C3 119.13(15) . . ?
C6 C7 C8 119.92(17) . . ?
C6 C7 C10 120.78(19) . . ?
C8 C7 C10 119.28(18) . . ?
C26 C25 C24 120.90(16) . . ?
N2 C2 C1 110.81(13) . . ?
C6 C5 C4 121.09(16) . . ?
C18 C17 C16 118.41(19) . . ?
C18 C17 C20 120.73(18) . . ?
C16 C17 C20 120.8(2) . . ?
N1 C21 C22 114.67(14) . . ?
C7 C6 C5 119.63(18) . . ?
N1 C1 C2 114.63(14) . . ?
C28 C27 C26 119.37(17) . . ?
C28 C27 C30 119.08(16) . . ?
C26 C27 C30 121.55(16) . . ?
C14 C15 C16 122.02(17) . . ?
C28 C29 C24 122.07(16) . . ?
C8 C9 C4 120.90(18) . . ?
C29 C28 C27 119.76(16) . . ?
N7 C30 C27 177.2(2) . . ?
C27 C26 C25 120.32(17) . . ?
C9 C8 C7 119.81(17) . . ?
N5 C10 C7 178.7(2) . . ?
N6 C20 C17 179.4(3) . . ?
C14 C19 C18 121.35(19) . . ?
C17 C16 C15 120.62(19) . . ?
C17 C18 C19 121.13(18) . . ?
C23 N4 C22 122.51(14) . . ?
C13 N3 C12 124.44(14) . . ?
C3 N2 C2 121.74(13) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        28.21
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.164
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.068
####################################################################### 
# 
# 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_1LH-Br
_database_code_depnum_ccdc_archive 'CCDC 1041357'
_audit_update_record             
;
2015-04-10 deposited with the CCDC.
2015-04-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H28 N7 O3, Br'
_chemical_formula_sum            'C30 H28 Br N7 O3'

_chemical_formula_weight         614.49

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'
Br Br -0.2901 2.4595 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.6711(5)
_cell_length_b                   11.9923(9)
_cell_length_c                   16.3251(11)
_cell_angle_alpha                71.874(5)
_cell_angle_beta                 85.255(5)
_cell_angle_gamma                87.127(5)
_cell_volume                     1421.92(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    6125
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      25.66

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             632.0
_exptl_absorpt_coefficient_mu    1.490
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.656
_exptl_absorpt_correction_T_max  0.742
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19711
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.79
_diffrn_reflns_theta_max         26.44
_reflns_number_total             5801
_reflns_number_gt                3629
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0292P)²+0.4722P] 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         5801
_refine_ls_number_parameters     386
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0421
_refine_ls_wR_factor_ref         0.0875
_refine_ls_wR_factor_gt          0.0766
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_restrained_S_all      0.990
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001

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
O1 O 0.2938(2) 0.26584(16) 0.34198(14) 0.0543(6) Uani 1 1 d . . .
O2 O 0.1654(3) 0.5724(2) 0.08206(15) 0.0705(7) Uani 1 1 d . . .
O3 O -0.2667(3) 0.39703(18) 0.20739(14) 0.0588(6) Uani 1 1 d . . .
N1 N 0.2321(3) 0.49844(19) 0.32880(14) 0.0321(5) Uani 1 1 d . . .
N2 N 0.4994(3) 0.2831(2) 0.42604(16) 0.0412(6) Uani 1 1 d . . .
N5 N 0.7458(4) -0.2869(3) 0.3178(2) 0.0885(10) Uani 1 1 d . . .
N3 N 0.3999(3) 0.5087(2) 0.15855(15) 0.0395(6) Uani 1 1 d . . .
N6 N 0.3755(4) 0.0640(3) -0.0896(2) 0.0807(9) Uani 1 1 d . . .
N4 N -0.0505(3) 0.3593(2) 0.29699(17) 0.0432(6) Uani 1 1 d . . .
N7 N 0.1128(5) -0.1477(3) 0.1133(2) 0.0964(12) Uani 1 1 d . . .
C1 C 0.3720(3) 0.4906(2) 0.39052(18) 0.0409(7) Uani 1 1 d . . .
H1A H 0.3428 0.5472 0.4213 0.049 Uiso 1 1 calc R . .
H1B H 0.4821 0.5133 0.3570 0.049 Uiso 1 1 calc R . .
C2 C 0.3982(4) 0.3709(2) 0.45640(18) 0.0442(7) Uani 1 1 d . . .
H2A H 0.4557 0.3817 0.5041 0.053 Uiso 1 1 calc R . .
H2B H 0.2839 0.3396 0.4791 0.053 Uiso 1 1 calc R . .
C3 C 0.4323(3) 0.2286(2) 0.37670(18) 0.0375(7) Uani 1 1 d . . .
C4 C 0.5199(3) 0.1202(2) 0.36454(18) 0.0362(6) Uani 1 1 d . . .
C5 C 0.4635(4) 0.0827(2) 0.29944(19) 0.0480(8) Uani 1 1 d . . .
H5 H 0.3812 0.1279 0.2636 0.058 Uiso 1 1 calc R . .
C6 C 0.5273(4) -0.0204(3) 0.2869(2) 0.0546(8) Uani 1 1 d . . .
H6 H 0.4885 -0.0443 0.2427 0.066 Uiso 1 1 calc R . .
C7 C 0.6494(4) -0.0885(2) 0.3402(2) 0.0468(8) Uani 1 1 d . . .
C8 C 0.7076(4) -0.1991(3) 0.3282(2) 0.0598(9) Uani 1 1 d . . .
C9 C 0.7089(4) -0.0514(2) 0.4053(2) 0.0477(8) Uani 1 1 d . . .
H9 H 0.7918 -0.0967 0.4408 0.057 Uiso 1 1 calc R . .
C10 C 0.6453(4) 0.0528(2) 0.41757(18) 0.0423(7) Uani 1 1 d . . .
H10 H 0.6859 0.0779 0.4609 0.051 Uiso 1 1 calc R . .
C11 C 0.2426(3) 0.6104(2) 0.25490(17) 0.0389(7) Uani 1 1 d . . .
H11A H 0.2536 0.6754 0.2774 0.047 Uiso 1 1 calc R . .
H11B H 0.1346 0.6226 0.2259 0.047 Uiso 1 1 calc R . .
C12 C 0.3953(4) 0.6104(2) 0.18958(18) 0.0430(7) Uani 1 1 d . . .
H12A H 0.3878 0.6812 0.1408 0.052 Uiso 1 1 calc R . .
H12B H 0.5036 0.6118 0.2159 0.052 Uiso 1 1 calc R . .
C13 C 0.2872(4) 0.5014(2) 0.10112(18) 0.0424(7) Uani 1 1 d . . .
C14 C 0.3140(3) 0.4022(2) 0.06261(17) 0.0373(7) Uani 1 1 d . . .
C15 C 0.4297(4) 0.3083(3) 0.0921(2) 0.0515(8) Uani 1 1 d . . .
H15 H 0.4971 0.3048 0.1376 0.062 Uiso 1 1 calc R . .
C16 C 0.4454(4) 0.2197(3) 0.0540(2) 0.0540(8) Uani 1 1 d . . .
H16 H 0.5237 0.1571 0.0737 0.065 Uiso 1 1 calc R . .
C17 C 0.2152(4) 0.4056(3) -0.00510(19) 0.0471(8) Uani 1 1 d . . .
H17 H 0.1378 0.4686 -0.0253 0.056 Uiso 1 1 calc R . .
C18 C 0.2286(4) 0.3181(3) -0.04327(19) 0.0479(8) Uani 1 1 d . . .
H18 H 0.1606 0.3216 -0.0887 0.057 Uiso 1 1 calc R . .
C19 C 0.3446(4) 0.2246(2) -0.01336(18) 0.0435(7) Uani 1 1 d . . .
C20 C 0.3615(4) 0.1342(3) -0.0554(2) 0.0555(8) Uani 1 1 d . . .
C21 C 0.0525(3) 0.4851(2) 0.37559(17) 0.0381(7) Uani 1 1 d . . .
H21A H 0.0214 0.5559 0.3909 0.046 Uiso 1 1 calc R . .
H21B H 0.0567 0.4204 0.4288 0.046 Uiso 1 1 calc R . .
C22 C -0.0882(3) 0.4631(2) 0.3235(2) 0.0447(7) Uani 1 1 d . . .
H22A H -0.1990 0.4541 0.3578 0.054 Uiso 1 1 calc R . .
H22B H -0.0996 0.5306 0.2726 0.054 Uiso 1 1 calc R . .
C23 C -0.1418(4) 0.3339(2) 0.23914(18) 0.0401(7) Uani 1 1 d . . .
C24 C -0.0849(3) 0.2273(2) 0.21384(18) 0.0371(7) Uani 1 1 d . . .
C25 C -0.0055(3) 0.1296(2) 0.27021(18) 0.0415(7) Uani 1 1 d . . .
H25 H 0.0148 0.1297 0.3256 0.050 Uiso 1 1 calc R . .
C26 C 0.0433(4) 0.0326(2) 0.2444(2) 0.0469(8) Uani 1 1 d . . .
H26 H 0.0955 -0.0326 0.2824 0.056 Uiso 1 1 calc R . .
C27 C 0.0144(4) 0.0328(3) 0.1618(2) 0.0462(7) Uani 1 1 d . . .
C28 C -0.0639(4) 0.1296(3) 0.10492(19) 0.0507(8) Uani 1 1 d . . .
H28 H -0.0824 0.1295 0.0494 0.061 Uiso 1 1 calc R . .
C29 C -0.1142(4) 0.2261(3) 0.13108(19) 0.0467(7) Uani 1 1 d . . .
H29 H -0.1680 0.2907 0.0932 0.056 Uiso 1 1 calc R . .
C30 C 0.0674(5) -0.0681(3) 0.1344(2) 0.0635(9) Uani 1 1 d . . .
Br1 Br 0.83971(4) 0.24118(3) 0.54856(2) 0.05635(13) Uani 1 1 d . . .
H2N H 0.594(4) 0.255(2) 0.4529(18) 0.057(10) Uiso 1 1 d . . .
H1N H 0.251(3) 0.436(2) 0.3059(16) 0.042(8) Uiso 1 1 d . . .
H3N H 0.489(3) 0.466(2) 0.1650(17) 0.041(9) Uiso 1 1 d . . .
H4N H 0.032(4) 0.314(2) 0.3154(17) 0.044(9) Uiso 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
O1 C3 1.242(3) . ?
O2 C13 1.224(3) . ?
O3 C23 1.235(3) . ?
N1 C11 1.500(3) . ?
N1 C21 1.510(3) . ?
N1 C1 1.512(3) . ?
N1 H1N 0.94(3) . ?
N2 C3 1.331(3) . ?
N2 C2 1.462(3) . ?
N2 H2N 0.88(3) . ?
N5 C8 1.137(4) . ?
N3 C13 1.352(3) . ?
N3 C12 1.456(3) . ?
N3 H3N 0.82(3) . ?
N6 C20 1.142(4) . ?
N4 C23 1.336(3) . ?
N4 C22 1.449(3) . ?
N4 H4N 0.82(3) . ?
N7 C30 1.142(4) . ?
C1 C2 1.518(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.494(4) . ?
C4 C5 1.382(4) . ?
C4 C10 1.397(4) . ?
C5 C6 1.374(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.385(4) . ?
C6 H6 0.9300 . ?
C7 C9 1.389(4) . ?
C7 C8 1.444(4) . ?
C9 C10 1.386(4) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.517(3) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.507(4) . ?
C14 C15 1.386(4) . ?
C14 C17 1.380(4) . ?
C15 C16 1.384(4) . ?
C15 H15 0.9300 . ?
C16 C19 1.381(4) . ?
C16 H16 0.9300 . ?
C17 C18 1.373(4) . ?
C17 H17 0.9300 . ?
C18 C19 1.385(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.448(4) . ?
C21 C22 1.509(4) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.496(4) . ?
C24 C29 1.392(4) . ?
C24 C25 1.393(4) . ?
C25 C26 1.380(4) . ?
C25 H25 0.9300 . ?
C26 C27 1.383(4) . ?
C26 H26 0.9300 . ?
C27 C28 1.387(4) . ?
C27 C30 1.445(5) . ?
C28 C29 1.381(4) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?

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
C11 N1 C21 111.2(2) . . ?
C11 N1 C1 111.4(2) . . ?
C21 N1 C1 110.9(2) . . ?
C11 N1 H1N 107.8(15) . . ?
C21 N1 H1N 107.4(15) . . ?
C1 N1 H1N 107.9(16) . . ?
C3 N2 C2 121.8(2) . . ?
C3 N2 H2N 120.6(19) . . ?
C2 N2 H2N 115.7(19) . . ?
C13 N3 C12 120.8(2) . . ?
C13 N3 H3N 119.1(19) . . ?
C12 N3 H3N 117.7(19) . . ?
C23 N4 C22 122.3(2) . . ?
C23 N4 H4N 116.2(19) . . ?
C22 N4 H4N 121.5(19) . . ?
N1 C1 C2 115.5(2) . . ?
N1 C1 H1A 108.4 . . ?
C2 C1 H1A 108.4 . . ?
N1 C1 H1B 108.4 . . ?
C2 C1 H1B 108.4 . . ?
H1A C1 H1B 107.5 . . ?
N2 C2 C1 116.7(2) . . ?
N2 C2 H2A 108.1 . . ?
C1 C2 H2A 108.1 . . ?
N2 C2 H2B 108.1 . . ?
C1 C2 H2B 108.1 . . ?
H2A C2 H2B 107.3 . . ?
O1 C3 N2 120.2(2) . . ?
O1 C3 C4 119.4(2) . . ?
N2 C3 C4 120.4(2) . . ?
C5 C4 C10 119.3(3) . . ?
C5 C4 C3 116.6(2) . . ?
C10 C4 C3 124.0(3) . . ?
C6 C5 C4 121.0(3) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C5 C6 C7 119.9(3) . . ?
C5 C6 H6 120.1 . . ?
C7 C6 H6 120.1 . . ?
C6 C7 C9 119.8(3) . . ?
C6 C7 C8 118.6(3) . . ?
C9 C7 C8 121.5(3) . . ?
N5 C8 C7 176.8(4) . . ?
C10 C9 C7 120.2(3) . . ?
C10 C9 H9 119.9 . . ?
C7 C9 H9 119.9 . . ?
C9 C10 C4 119.7(3) . . ?
C9 C10 H10 120.2 . . ?
C4 C10 H10 120.2 . . ?
N1 C11 C12 113.0(2) . . ?
N1 C11 H11A 109.0 . . ?
C12 C11 H11A 109.0 . . ?
N1 C11 H11B 109.0 . . ?
C12 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
N3 C12 C11 113.0(2) . . ?
N3 C12 H12A 109.0 . . ?
C11 C12 H12A 109.0 . . ?
N3 C12 H12B 109.0 . . ?
C11 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
O2 C13 N3 120.8(3) . . ?
O2 C13 C14 121.1(3) . . ?
N3 C13 C14 118.1(2) . . ?
C15 C14 C17 118.8(3) . . ?
C15 C14 C13 123.7(3) . . ?
C17 C14 C13 117.4(2) . . ?
C14 C15 C16 120.4(3) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C19 C16 C15 119.8(3) . . ?
C19 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
C18 C17 C14 121.5(3) . . ?
C18 C17 H17 119.2 . . ?
C14 C17 H17 119.2 . . ?
C17 C18 C19 119.2(3) . . ?
C17 C18 H18 120.4 . . ?
C19 C18 H18 120.4 . . ?
C16 C19 C18 120.3(3) . . ?
C16 C19 C20 120.8(3) . . ?
C18 C19 C20 118.9(3) . . ?
N6 C20 C19 179.1(4) . . ?
N1 C21 C22 113.7(2) . . ?
N1 C21 H21A 108.8 . . ?
C22 C21 H21A 108.8 . . ?
N1 C21 H21B 108.8 . . ?
C22 C21 H21B 108.8 . . ?
H21A C21 H21B 107.7 . . ?
N4 C22 C21 112.4(2) . . ?
N4 C22 H22A 109.1 . . ?
C21 C22 H22A 109.1 . . ?
N4 C22 H22B 109.1 . . ?
C21 C22 H22B 109.1 . . ?
H22A C22 H22B 107.9 . . ?
O3 C23 N4 121.0(3) . . ?
O3 C23 C24 121.7(3) . . ?
N4 C23 C24 117.3(2) . . ?
C29 C24 C25 119.3(3) . . ?
C29 C24 C23 118.4(2) . . ?
C25 C24 C23 122.4(3) . . ?
C26 C25 C24 120.4(3) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C25 C26 C27 119.8(3) . . ?
C25 C26 H26 120.1 . . ?
C27 C26 H26 120.1 . . ?
C26 C27 C28 120.5(3) . . ?
C26 C27 C30 119.8(3) . . ?
C28 C27 C30 119.7(3) . . ?
C29 C28 C27 119.7(3) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
C28 C29 C24 120.4(3) . . ?
C28 C29 H29 119.8 . . ?
C24 C29 H29 119.8 . . ?
N7 C30 C27 178.5(4) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        26.44
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.058
####################################################################### 
# 
# 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_1LH-I
_database_code_depnum_ccdc_archive 'CCDC 1041358'
_audit_update_record             
;
2015-04-10 deposited with the CCDC.
2015-04-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H28 N7 O3, I'
_chemical_formula_sum            'C30 H28 I N7 O3'

_chemical_formula_weight         661.49

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'
I I -0.4742 1.8119 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.7036(7)
_cell_length_b                   12.0659(11)
_cell_length_c                   16.4604(14)
_cell_angle_alpha                72.706(5)
_cell_angle_beta                 84.786(5)
_cell_angle_gamma                86.852(5)
_cell_volume                     1454.2(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    4165
_cell_measurement_theta_min      2.60
_cell_measurement_theta_max      20.62

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             668.0
_exptl_absorpt_coefficient_mu    1.145
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.678
_exptl_absorpt_correction_T_max  0.751
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13002
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_unetI/netI     0.1372
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.30
_diffrn_reflns_theta_max         27.79
_reflns_number_total             6798
_reflns_number_gt                3466
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0704P)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         6798
_refine_ls_number_parameters     374
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1314
_refine_ls_R_factor_gt           0.0583
_refine_ls_wR_factor_ref         0.1429
_refine_ls_wR_factor_gt          0.1199
_refine_ls_goodness_of_fit_ref   0.908
_refine_ls_restrained_S_all      0.908
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.008

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
O2 O 0.8339(8) -0.0731(5) 0.4211(3) 0.0713(19) Uani 1 1 d . . .
O3 O 1.2720(7) 0.0976(5) 0.2964(3) 0.0625(16) Uani 1 1 d . . .
O1 O 0.7098(6) 0.2270(4) 0.1704(3) 0.0527(14) Uani 1 1 d . . .
N6 N 0.6276(10) 0.4391(6) 0.5855(4) 0.085(3) Uani 1 1 d . . .
N7 N 0.8978(13) 0.6456(8) 0.3842(5) 0.104(3) Uani 1 1 d . . .
N1 N 0.7694(8) -0.0018(5) 0.1786(3) 0.0352(16) Uani 1 1 d . . .
N4 N 1.0529(7) 0.1350(5) 0.2097(3) 0.0457(16) Uani 1 1 d . . .
H4N H 0.9685 0.1813 0.1890 0.055 Uiso 1 1 calc R . .
N3 N 0.5993(7) -0.0123(5) 0.3471(3) 0.0439(16) Uani 1 1 d . . .
H3N H 0.5227 0.0425 0.3301 0.053 Uiso 1 1 calc R . .
N2 N 0.5117(8) 0.2164(5) 0.0831(3) 0.0418(16) Uani 1 1 d . . .
H2N H 0.4082 0.2357 0.0672 0.050 Uiso 1 1 calc R . .
C11 C 0.7557(10) -0.1128(6) 0.2513(4) 0.046(2) Uani 1 1 d . . .
H11B H 0.8629 -0.1258 0.2800 0.056 Uiso 1 1 calc R . .
H11A H 0.7449 -0.1769 0.2281 0.056 Uiso 1 1 calc R . .
C13 C 0.7147(11) -0.0031(7) 0.4021(4) 0.043(2) Uani 1 1 d . . .
C14 C 0.6886(10) 0.0962(7) 0.4394(4) 0.040(2) Uani 1 1 d . . .
C15 C 0.7895(9) 0.0951(6) 0.5050(4) 0.046(2) Uani 1 1 d . . .
H15 H 0.8677 0.0334 0.5249 0.056 Uiso 1 1 calc R . .
C16 C 0.7746(10) 0.1852(7) 0.5411(4) 0.050(2) Uani 1 1 d . . .
H16 H 0.8438 0.1839 0.5848 0.060 Uiso 1 1 calc R . .
C19 C 0.5710(11) 0.1900(7) 0.4106(4) 0.056(2) Uani 1 1 d . . .
H19 H 0.5026 0.1922 0.3664 0.067 Uiso 1 1 calc R . .
C18 C 0.5572(10) 0.2780(7) 0.4474(4) 0.054(2) Uani 1 1 d . . .
H18 H 0.4784 0.3394 0.4279 0.065 Uiso 1 1 calc R . .
C17 C 0.6575(10) 0.2781(7) 0.5130(4) 0.043(2) Uani 1 1 d . . .
C20 C 0.6384(11) 0.3687(7) 0.5532(5) 0.056(2) Uani 1 1 d . . .
C21 C 0.9465(9) 0.0094(6) 0.1327(4) 0.0419(19) Uani 1 1 d . . .
H21A H 0.9430 0.0731 0.0805 0.050 Uiso 1 1 calc R . .
H21B H 0.9759 -0.0611 0.1169 0.050 Uiso 1 1 calc R . .
C22 C 1.0909(9) 0.0304(6) 0.1840(4) 0.048(2) Uani 1 1 d . . .
H22A H 1.1018 -0.0356 0.2344 0.057 Uiso 1 1 calc R . .
H22B H 1.2012 0.0380 0.1496 0.057 Uiso 1 1 calc R . .
C30 C 1.0199(9) 0.3635(7) 0.2337(4) 0.044(2) Uani 1 1 d . . .
H30 H 1.0026 0.3617 0.1789 0.053 Uiso 1 1 calc R . .
C24 C 1.0923(9) 0.2680(7) 0.2904(4) 0.0358(18) Uani 1 1 d . . .
C25 C 1.1178(9) 0.2715(7) 0.3715(4) 0.046(2) Uani 1 1 d . . .
H25 H 1.1673 0.2071 0.4097 0.055 Uiso 1 1 calc R . .
C26 C 1.0718(10) 0.3674(8) 0.3966(5) 0.053(2) Uani 1 1 d . . .
H26 H 1.0901 0.3689 0.4514 0.064 Uiso 1 1 calc R . .
C27 C 0.9974(10) 0.4630(7) 0.3398(5) 0.049(2) Uani 1 1 d . . .
C29 C 0.9728(10) 0.4619(7) 0.2578(4) 0.047(2) Uani 1 1 d . . .
H29 H 0.9252 0.5268 0.2193 0.057 Uiso 1 1 calc R . .
C28 C 0.9445(13) 0.5662(10) 0.3652(5) 0.070(3) Uani 1 1 d . . .
C3 C 0.5759(11) 0.2699(7) 0.1335(4) 0.047(2) Uani 1 1 d . . .
C23 C 1.1496(11) 0.1593(7) 0.2659(4) 0.044(2) Uani 1 1 d . . .
I1 I 0.84845(7) 0.73302(4) 0.04654(3) 0.0557(3) Uani 1 1 d . . .
C1 C 0.6305(8) 0.0077(6) 0.1183(4) 0.040(2) Uani 1 1 d . . .
H1B H 0.5200 -0.0119 0.1515 0.048 Uiso 1 1 calc R . .
H1A H 0.6569 -0.0495 0.0878 0.048 Uiso 1 1 calc R . .
C12 C 0.6036(9) -0.1134(6) 0.3165(4) 0.0430(19) Uani 1 1 d . . .
H12B H 0.4957 -0.1155 0.2910 0.052 Uiso 1 1 calc R . .
H12A H 0.6121 -0.1830 0.3644 0.052 Uiso 1 1 calc R . .
C2 C 0.6095(9) 0.1261(6) 0.0534(4) 0.042(2) Uani 1 1 d . . .
H2B H 0.7250 0.1544 0.0313 0.050 Uiso 1 1 calc R . .
H2A H 0.5523 0.1158 0.0061 0.050 Uiso 1 1 calc R . .
C8 C 0.3166(10) 0.5502(7) 0.1002(4) 0.054(2) Uani 1 1 d . . .
H8 H 0.2371 0.5951 0.0637 0.064 Uiso 1 1 calc R . .
C7 C 0.3732(10) 0.5886(7) 0.1635(5) 0.048(2) Uani 1 1 d . . .
C6 C 0.4884(10) 0.5207(7) 0.2194(5) 0.052(2) Uani 1 1 d . . .
H6 H 0.5242 0.5456 0.2634 0.063 Uiso 1 1 calc R . .
C5 C 0.5487(10) 0.4166(7) 0.2090(4) 0.047(2) Uani 1 1 d . . .
H5 H 0.6269 0.3708 0.2458 0.057 Uiso 1 1 calc R . .
C9 C 0.3783(10) 0.4445(7) 0.0907(4) 0.046(2) Uani 1 1 d . . .
H9 H 0.3410 0.4180 0.0478 0.055 Uiso 1 1 calc R . .
C4 C 0.4947(9) 0.3794(6) 0.1450(4) 0.0351(19) Uani 1 1 d . . .
C10 C 0.3170(12) 0.7006(10) 0.1738(5) 0.064(3) Uani 1 1 d . . .
N5 N 0.2809(11) 0.7898(7) 0.1819(5) 0.094(3) Uani 1 1 d . . .
H1N H 0.749(10) 0.055(7) 0.208(4) 0.09(3) Uiso 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
O2 C13 1.211(8) . ?
O3 C23 1.217(8) . ?
O1 C3 1.253(8) . ?
N6 C20 1.125(8) . ?
N7 C28 1.125(10) . ?
N1 C21 1.491(8) . ?
N1 C1 1.502(7) . ?
N1 C11 1.509(8) . ?
N1 H1N 0.95(8) . ?
N4 C23 1.344(8) . ?
N4 C22 1.453(8) . ?
N4 H4N 0.8600 . ?
N3 C13 1.357(8) . ?
N3 C12 1.449(7) . ?
N3 H3N 0.8600 . ?
N2 C3 1.333(7) . ?
N2 C2 1.468(8) . ?
N2 H2N 0.8600 . ?
C11 C12 1.514(9) . ?
C11 H11B 0.9700 . ?
C11 H11A 0.9700 . ?
C13 C14 1.497(10) . ?
C14 C15 1.383(8) . ?
C14 C19 1.405(10) . ?
C15 C16 1.380(9) . ?
C15 H15 0.9300 . ?
C16 C17 1.393(9) . ?
C16 H16 0.9300 . ?
C19 C18 1.366(9) . ?
C19 H19 0.9300 . ?
C18 C17 1.384(9) . ?
C18 H18 0.9300 . ?
C17 C20 1.431(10) . ?
C21 C22 1.531(8) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C30 C29 1.381(9) . ?
C30 C24 1.376(9) . ?
C30 H30 0.9300 . ?
C24 C25 1.381(8) . ?
C24 C23 1.515(10) . ?
C25 C26 1.360(9) . ?
C25 H25 0.9300 . ?
C26 C27 1.385(10) . ?
C26 H26 0.9300 . ?
C27 C29 1.384(9) . ?
C27 C28 1.454(13) . ?
C29 H29 0.9300 . ?
C3 C4 1.487(10) . ?
C1 C2 1.518(8) . ?
C1 H1B 0.9700 . ?
C1 H1A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 H12A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 H2A 0.9700 . ?
C8 C7 1.373(9) . ?
C8 C9 1.384(9) . ?
C8 H8 0.9300 . ?
C7 C6 1.388(9) . ?
C7 C10 1.449(12) . ?
C6 C5 1.369(9) . ?
C6 H6 0.9300 . ?
C5 C4 1.366(8) . ?
C5 H5 0.9300 . ?
C9 C4 1.367(9) . ?
C9 H9 0.9300 . ?
C10 N5 1.139(10) . ?

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
C21 N1 C1 111.2(5) . . ?
C21 N1 C11 111.5(5) . . ?
C1 N1 C11 111.3(5) . . ?
C21 N1 H1N 111(5) . . ?
C1 N1 H1N 110(5) . . ?
C11 N1 H1N 102(4) . . ?
C23 N4 C22 120.1(6) . . ?
C23 N4 H4N 120.0 . . ?
C22 N4 H4N 120.0 . . ?
C13 N3 C12 120.7(6) . . ?
C13 N3 H3N 119.7 . . ?
C12 N3 H3N 119.7 . . ?
C3 N2 C2 123.0(6) . . ?
C3 N2 H2N 118.5 . . ?
C2 N2 H2N 118.5 . . ?
N1 C11 C12 114.2(6) . . ?
N1 C11 H11B 108.7 . . ?
C12 C11 H11B 108.7 . . ?
N1 C11 H11A 108.7 . . ?
C12 C11 H11A 108.7 . . ?
H11B C11 H11A 107.6 . . ?
O2 C13 N3 121.3(7) . . ?
O2 C13 C14 121.0(7) . . ?
N3 C13 C14 117.7(8) . . ?
C15 C14 C19 119.0(7) . . ?
C15 C14 C13 117.2(7) . . ?
C19 C14 C13 123.8(6) . . ?
C16 C15 C14 120.2(7) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C15 C16 C17 121.1(7) . . ?
C15 C16 H16 119.5 . . ?
C17 C16 H16 119.5 . . ?
C18 C19 C14 120.0(7) . . ?
C18 C19 H19 120.0 . . ?
C14 C19 H19 120.0 . . ?
C19 C18 C17 121.7(7) . . ?
C19 C18 H18 119.2 . . ?
C17 C18 H18 119.2 . . ?
C18 C17 C16 118.1(7) . . ?
C18 C17 C20 121.4(8) . . ?
C16 C17 C20 120.4(6) . . ?
N6 C20 C17 178.2(9) . . ?
N1 C21 C22 114.5(5) . . ?
N1 C21 H21A 108.6 . . ?
C22 C21 H21A 108.6 . . ?
N1 C21 H21B 108.6 . . ?
C22 C21 H21B 108.6 . . ?
H21A C21 H21B 107.6 . . ?
N4 C22 C21 110.9(6) . . ?
N4 C22 H22A 109.5 . . ?
C21 C22 H22A 109.5 . . ?
N4 C22 H22B 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 108.0 . . ?
C29 C30 C24 120.3(6) . . ?
C29 C30 H30 119.8 . . ?
C24 C30 H30 119.9 . . ?
C25 C24 C30 119.5(7) . . ?
C25 C24 C23 118.5(7) . . ?
C30 C24 C23 122.0(6) . . ?
C26 C25 C24 121.2(7) . . ?
C26 C25 H25 119.4 . . ?
C24 C25 H25 119.4 . . ?
C25 C26 C27 119.2(7) . . ?
C25 C26 H26 120.4 . . ?
C27 C26 H26 120.4 . . ?
C26 C27 C29 120.5(8) . . ?
C26 C27 C28 120.5(7) . . ?
C29 C27 C28 119.0(8) . . ?
C30 C29 C27 119.3(7) . . ?
C30 C29 H29 120.4 . . ?
C27 C29 H29 120.4 . . ?
N7 C28 C27 177.6(11) . . ?
O1 C3 N2 118.5(8) . . ?
O1 C3 C4 119.9(6) . . ?
N2 C3 C4 121.6(6) . . ?
O3 C23 N4 122.7(8) . . ?
O3 C23 C24 122.3(6) . . ?
N4 C23 C24 115.0(7) . . ?
N1 C1 C2 115.2(5) . . ?
N1 C1 H1B 108.5 . . ?
C2 C1 H1B 108.5 . . ?
N1 C1 H1A 108.5 . . ?
C2 C1 H1A 108.5 . . ?
H1B C1 H1A 107.5 . . ?
N3 C12 C11 112.0(5) . . ?
N3 C12 H12B 109.2 . . ?
C11 C12 H12B 109.2 . . ?
N3 C12 H12A 109.2 . . ?
C11 C12 H12A 109.2 . . ?
H12B C12 H12A 107.9 . . ?
N2 C2 C1 117.1(6) . . ?
N2 C2 H2B 108.0 . . ?
C1 C2 H2B 108.0 . . ?
N2 C2 H2A 108.0 . . ?
C1 C2 H2A 108.0 . . ?
H2B C2 H2A 107.3 . . ?
C7 C8 C9 119.8(7) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 H8 120.1 . . ?
C8 C7 C6 120.3(8) . . ?
C8 C7 C10 121.7(8) . . ?
C6 C7 C10 118.0(7) . . ?
C5 C6 C7 119.1(7) . . ?
C5 C6 H6 120.4 . . ?
C7 C6 H6 120.4 . . ?
C6 C5 C4 120.4(7) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C4 C9 C8 119.4(7) . . ?
C4 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
C9 C4 C5 120.9(7) . . ?
C9 C4 C3 121.6(6) . . ?
C5 C4 C3 117.3(7) . . ?
N5 C10 C7 176.8(10) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.79
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.149
_refine_diff_density_min         -1.186
_refine_diff_density_rms         0.124
####################################################################### 
# 
# 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_(1LH)2-2NO3-H2O
_database_code_depnum_ccdc_archive 'CCDC 1041359'
_audit_update_record             
;
2015-04-10 deposited with the CCDC.
2015-04-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C30 H28 N7 O3), 2(N O3), H2O'
_chemical_formula_sum            'C60 H58 N16 O13'

_chemical_formula_weight         1211.21

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'

_symmetry_cell_setting           TRICLINIC
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.7878(5)
_cell_length_b                   11.9857(8)
_cell_length_c                   16.6759(12)
_cell_angle_alpha                71.155(4)
_cell_angle_beta                 84.920(4)
_cell_angle_gamma                88.018(4)
_cell_volume                     1467.31(17)
_cell_formula_units_Z            1
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    4252
_cell_measurement_theta_min      2.15
_cell_measurement_theta_max      27.68

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLORLESS
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             632.0
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.969
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14891
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.80
_diffrn_reflns_theta_max         25.85
_reflns_number_total             5612
_reflns_number_gt                3199
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.1725P)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         5077
_refine_ls_number_parameters     422
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0650
_refine_ls_wR_factor_ref         0.2364
_refine_ls_wR_factor_gt          0.2003
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_restrained_S_all      0.946
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001

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
N2 N 0.3955(3) 0.5086(2) 0.15329(15) 0.0502(6) Uani 1 1 d . . .
N3 N -0.0624(3) 0.3582(2) 0.29071(17) 0.0537(7) Uani 1 1 d . . .
N1 N 0.2238(3) 0.49466(19) 0.32002(14) 0.0436(6) Uani 1 1 d . . .
N4 N 0.4758(3) 0.2716(2) 0.41478(17) 0.0534(7) Uani 1 1 d . . .
N8 N 0.8398(4) 0.2450(3) 0.5419(2) 0.0748(9) Uani 1 1 d . . .
N5 N 0.3775(5) 0.0628(3) -0.0851(2) 0.0938(11) Uani 1 1 d . . .
N6 N 0.0893(5) -0.1465(3) 0.1135(2) 0.1078(13) Uani 1 1 d . . .
N7 N 0.7029(5) -0.2959(3) 0.3108(3) 0.1043(12) Uani 1 1 d . . .
C3 C 0.2839(4) 0.4995(2) 0.09870(18) 0.0482(7) Uani 1 1 d . . .
C4 C 0.3106(4) 0.4009(2) 0.06131(17) 0.0464(7) Uani 1 1 d . . .
C2 C 0.3885(4) 0.6103(2) 0.18351(19) 0.0558(8) Uani 1 1 d . . .
H2C H 0.3809 0.6815 0.1352 0.067 Uiso 1 1 calc R . .
H2D H 0.4949 0.6136 0.2088 0.067 Uiso 1 1 calc R . .
C9 C 0.2127(4) 0.4022(3) -0.00426(19) 0.0554(8) Uani 1 1 d . . .
H9 H 0.1349 0.4636 -0.0237 0.066 Uiso 1 1 calc R . .
C1 C 0.2385(4) 0.6081(2) 0.24805(18) 0.0540(8) Uani 1 1 d . . .
H1A H 0.2512 0.6721 0.2708 0.065 Uiso 1 1 calc R . .
H1B H 0.1326 0.6217 0.2197 0.065 Uiso 1 1 calc R . .
C7 C 0.3427(4) 0.2231(2) -0.01260(18) 0.0521(7) Uani 1 1 d . . .
C5 C 0.4263(4) 0.3087(3) 0.0893(2) 0.0618(9) Uani 1 1 d . . .
H5 H 0.4944 0.3070 0.1327 0.074 Uiso 1 1 calc R . .
C8 C 0.2276(4) 0.3150(3) -0.0414(2) 0.0585(8) Uani 1 1 d . . .
H8 H 0.1609 0.3177 -0.0856 0.070 Uiso 1 1 calc R . .
C10 C 0.3625(4) 0.1325(3) -0.0526(2) 0.0637(9) Uani 1 1 d . . .
C6 C 0.4417(4) 0.2197(3) 0.0536(2) 0.0655(9) Uani 1 1 d . . .
H6 H 0.5180 0.1575 0.0736 0.079 Uiso 1 1 calc R . .
C13 C -0.1559(3) 0.3348(2) 0.23450(18) 0.0484(7) Uani 1 1 d . . .
C19 C -0.0336(4) 0.1278(2) 0.26688(19) 0.0545(8) Uani 1 1 d . . .
H19 H -0.0182 0.1261 0.3219 0.065 Uiso 1 1 calc R . .
C15 C -0.1274(4) 0.2285(3) 0.12844(19) 0.0585(8) Uani 1 1 d . . .
H15 H -0.1772 0.2940 0.0907 0.070 Uiso 1 1 calc R . .
C14 C -0.1036(3) 0.2282(2) 0.20973(18) 0.0465(7) Uani 1 1 d . . .
C18 C 0.0124(4) 0.0315(2) 0.2415(2) 0.0587(8) Uani 1 1 d . . .
H18 H 0.0580 -0.0355 0.2796 0.070 Uiso 1 1 calc R . .
C12 C -0.0937(4) 0.4619(3) 0.3167(2) 0.0589(8) Uani 1 1 d . . .
H12A H -0.2028 0.4532 0.3510 0.071 Uiso 1 1 calc R . .
H12B H -0.1028 0.5304 0.2666 0.071 Uiso 1 1 calc R . .
C16 C -0.0785(4) 0.1333(3) 0.1029(2) 0.0634(9) Uani 1 1 d . . .
H16 H -0.0921 0.1356 0.0476 0.076 Uiso 1 1 calc R . .
C11 C 0.0468(4) 0.4821(2) 0.36690(19) 0.0507(7) Uani 1 1 d . . .
H11A H 0.0487 0.4165 0.4194 0.061 Uiso 1 1 calc R . .
H11B H 0.0199 0.5529 0.3818 0.061 Uiso 1 1 calc R . .
C17 C -0.0091(4) 0.0343(3) 0.1590(2) 0.0584(8) Uani 1 1 d . . .
C20 C 0.0444(5) -0.0663(3) 0.1330(2) 0.0753(10) Uani 1 1 d . . .
C23 C 0.4087(4) 0.2219(2) 0.36435(18) 0.0479(7) Uani 1 1 d . . .
C22 C 0.3641(4) 0.4823(2) 0.3789(2) 0.0569(8) Uani 1 1 d . . .
H22A H 0.3430 0.5396 0.4086 0.068 Uiso 1 1 calc R . .
H22B H 0.4731 0.5021 0.3448 0.068 Uiso 1 1 calc R . .
C29 C 0.6087(4) 0.0438(2) 0.40360(19) 0.0530(7) Uani 1 1 d . . .
H29 H 0.6498 0.0680 0.4460 0.064 Uiso 1 1 calc R . .
C24 C 0.4874(4) 0.1127(2) 0.35230(17) 0.0468(7) Uani 1 1 d . . .
C28 C 0.6685(4) -0.0603(2) 0.3920(2) 0.0592(8) Uani 1 1 d . . .
H28 H 0.7501 -0.1057 0.4263 0.071 Uiso 1 1 calc R . .
C21 C 0.3819(4) 0.3615(3) 0.44443(19) 0.0581(8) Uani 1 1 d . . .
H21A H 0.4399 0.3707 0.4911 0.070 Uiso 1 1 calc R . .
H21B H 0.2672 0.3320 0.4670 0.070 Uiso 1 1 calc R . .
C27 C 0.6066(4) -0.0965(2) 0.3294(2) 0.0557(8) Uani 1 1 d . . .
C25 C 0.4282(4) 0.0761(3) 0.2893(2) 0.0630(9) Uani 1 1 d . . .
H25 H 0.3475 0.1217 0.2546 0.076 Uiso 1 1 calc R . .
C30 C 0.6635(5) -0.2075(3) 0.3187(2) 0.0730(10) Uani 1 1 d . . .
C26 C 0.4875(5) -0.0277(3) 0.2773(2) 0.0684(9) Uani 1 1 d . . .
H26 H 0.4478 -0.0514 0.2344 0.082 Uiso 1 1 calc R . .
O2 O -0.2764(3) 0.39879(19) 0.20422(15) 0.0698(7) Uani 1 1 d . . .
O3 O 0.2779(3) 0.26570(18) 0.32691(15) 0.0696(7) Uani 1 1 d . . .
O1 O 0.1635(3) 0.5694(2) 0.07953(16) 0.0811(8) Uani 1 1 d . . .
O6 O 0.9618(5) 0.2462(3) 0.5800(3) 0.1415(14) Uani 1 1 d . . .
O4 O 0.7320(5) 0.3146(5) 0.5354(4) 0.195(2) Uani 1 1 d . . .
O5 O 0.8142(8) 0.1832(5) 0.5035(4) 0.223(3) Uani 1 1 d . . .
O7 O 0.0741(10) 0.0489(8) 0.4676(5) 0.154(3) Uani 0.50 1 d P . .
H1N H 0.245(3) 0.432(2) 0.2945(16) 0.047(7) Uiso 1 1 d . . .
H4N H 0.558(5) 0.236(3) 0.445(2) 0.081(11) Uiso 1 1 d . . .
H2N H 0.484(5) 0.461(3) 0.164(2) 0.073(10) Uiso 1 1 d . . .
H3N H 0.015(4) 0.307(2) 0.3144(18) 0.055(8) Uiso 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
N2 C3 1.344(4) . ?
N2 C2 1.460(3) . ?
N3 C13 1.339(4) . ?
N3 C12 1.450(3) . ?
N1 C1 1.495(3) . ?
N1 C22 1.505(3) . ?
N1 C11 1.511(4) . ?
N4 C23 1.326(4) . ?
N4 C21 1.472(4) . ?
N8 O4 1.149(4) . ?
N8 O5 1.158(4) . ?
N8 O6 1.191(4) . ?
N5 C10 1.132(4) . ?
N6 C20 1.144(4) . ?
N7 C30 1.138(4) . ?
C3 O1 1.229(3) . ?
C3 C4 1.504(4) . ?
C4 C9 1.383(4) . ?
C4 C5 1.387(4) . ?
C2 C1 1.511(4) . ?
C9 C8 1.373(4) . ?
C7 C8 1.383(4) . ?
C7 C6 1.390(4) . ?
C7 C10 1.444(4) . ?
C5 C6 1.377(4) . ?
C13 O2 1.228(3) . ?
C13 C14 1.497(4) . ?
C19 C18 1.379(4) . ?
C19 C14 1.400(4) . ?
C15 C16 1.372(4) . ?
C15 C14 1.383(4) . ?
C18 C17 1.391(4) . ?
C12 C11 1.506(4) . ?
C16 C17 1.379(4) . ?
C17 C20 1.444(4) . ?
C23 O3 1.252(3) . ?
C23 C24 1.490(4) . ?
C22 C21 1.517(4) . ?
C29 C28 1.382(4) . ?
C29 C24 1.392(4) . ?
C24 C25 1.381(4) . ?
C28 C27 1.381(4) . ?
C27 C26 1.386(4) . ?
C27 C30 1.448(4) . ?
C25 C26 1.381(4) . ?
O7 O7 1.711(18) 2_556 ?

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
C3 N2 C2 120.3(2) . . ?
C13 N3 C12 122.0(2) . . ?
C1 N1 C22 111.4(2) . . ?
C1 N1 C11 111.0(2) . . ?
C22 N1 C11 111.8(2) . . ?
C23 N4 C21 122.1(3) . . ?
O4 N8 O5 110.3(4) . . ?
O4 N8 O6 121.5(4) . . ?
O5 N8 O6 128.1(4) . . ?
O1 C3 N2 121.3(3) . . ?
O1 C3 C4 120.6(2) . . ?
N2 C3 C4 118.1(2) . . ?
C9 C4 C5 118.3(3) . . ?
C9 C4 C3 117.9(2) . . ?
C5 C4 C3 123.8(2) . . ?
N2 C2 C1 113.7(2) . . ?
C8 C9 C4 121.7(3) . . ?
N1 C1 C2 113.4(2) . . ?
C8 C7 C6 119.8(3) . . ?
C8 C7 C10 119.9(3) . . ?
C6 C7 C10 120.2(3) . . ?
C6 C5 C4 120.9(3) . . ?
C9 C8 C7 119.5(3) . . ?
N5 C10 C7 178.9(4) . . ?
C5 C6 C7 119.8(3) . . ?
O2 C13 N3 121.4(3) . . ?
O2 C13 C14 122.1(2) . . ?
N3 C13 C14 116.5(2) . . ?
C18 C19 C14 120.0(3) . . ?
C16 C15 C14 120.7(3) . . ?
C15 C14 C19 119.1(3) . . ?
C15 C14 C13 119.0(2) . . ?
C19 C14 C13 121.8(2) . . ?
C19 C18 C17 120.1(3) . . ?
N3 C12 C11 112.5(2) . . ?
C15 C16 C17 120.3(3) . . ?
C12 C11 N1 113.7(2) . . ?
C16 C17 C18 119.7(3) . . ?
C16 C17 C20 121.0(3) . . ?
C18 C17 C20 119.2(3) . . ?
N6 C20 C17 178.7(4) . . ?
O3 C23 N4 120.4(3) . . ?
O3 C23 C24 119.4(2) . . ?
N4 C23 C24 120.3(2) . . ?
N1 C22 C21 115.7(2) . . ?
C28 C29 C24 120.5(3) . . ?
C25 C24 C29 119.1(3) . . ?
C25 C24 C23 117.1(2) . . ?
C29 C24 C23 123.7(3) . . ?
C29 C28 C27 119.7(3) . . ?
N4 C21 C22 116.5(3) . . ?
C28 C27 C26 120.2(3) . . ?
C28 C27 C30 120.2(3) . . ?
C26 C27 C30 119.6(3) . . ?
C26 C25 C24 120.6(3) . . ?
N7 C30 C27 177.8(4) . . ?
C25 C26 C27 119.8(3) . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        25.85
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.059

# start Validation Reply Form
_vrf_PLAT430_1LH2-2NO3-H2O       
;
PROBLEM: Short Inter D...A Contact  O7     ..  O7      ..       1.71 Ang.  
RESPONSE: These alert is generating due to modeling of 
the water oxygen O7 segment of the crystal.
These oxygen atoms O7 and O7A vibrated over two position.
;
####################################################################### 
# 
# 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_1LH-ClO4
_database_code_depnum_ccdc_archive 'CCDC 1041360'
_audit_update_record             
;
2015-04-10 deposited with the CCDC.
2015-04-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H28 N7 O3, Cl O4'
_chemical_formula_sum            'C30 H28 Cl N7 O7'

_chemical_formula_weight         634.04

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.7883(13)
_cell_length_b                   12.119(2)
_cell_length_c                   16.814(3)
_cell_angle_alpha                73.176(10)
_cell_angle_beta                 84.484(9)
_cell_angle_gamma                86.573(11)
_cell_volume                     1511.2(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    5000
_cell_measurement_theta_min      2.82
_cell_measurement_theta_max      22.29

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             660.0
_exptl_absorpt_coefficient_mu    0.186
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.944
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15221
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.27
_diffrn_reflns_theta_max         28.28
_reflns_number_total             7453
_reflns_number_gt                4410
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.1815P)²+0.0888P] 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         7453
_refine_ls_number_parameters     410
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1324
_refine_ls_R_factor_gt           0.0832
_refine_ls_wR_factor_ref         0.3068
_refine_ls_wR_factor_gt          0.2649
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_restrained_S_all      1.096
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.003

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
Cl1 Cl 0.63492(16) 0.27382(10) 0.45753(7) 0.0748(4) Uani 1 1 d . . .
N3 N 0.4401(4) 0.8732(2) 0.2828(2) 0.0554(9) Uani 1 1 d . . .
H3N H 0.5228 0.8269 0.3037 0.067 Uiso 1 1 calc R . .
N1 N 0.7255(4) 1.0090(2) 0.31104(19) 0.0443(8) Uani 1 1 d . . .
N2 N 0.8975(4) 1.0154(2) 0.14673(19) 0.0515(8) Uani 1 1 d . . .
H2N H 0.9740 0.9616 0.1635 0.062 Uiso 1 1 calc R . .
N4 N 0.9737(4) 0.7904(2) 0.40553(19) 0.0537(9) Uani 1 1 d . . .
H4N H 1.0741 0.7679 0.4226 0.064 Uiso 1 1 calc R . .
N5 N 0.8735(7) 0.5581(4) -0.0834(3) 0.1011(16) Uani 1 1 d . . .
N6 N 0.5902(7) 0.3575(4) 0.1154(3) 0.1089(17) Uani 1 1 d . . .
N7 N 1.1930(7) 0.2097(4) 0.3181(4) 0.122(2) Uani 1 1 d . . .
C13 C 0.3454(5) 0.8454(3) 0.2300(2) 0.0478(9) Uani 1 1 d . . .
C11 C 0.5486(5) 0.9993(3) 0.3567(2) 0.0512(10) Uani 1 1 d . . .
H11A H 0.5198 1.0696 0.3723 0.061 Uiso 1 1 calc R . .
H11B H 0.5512 0.9361 0.4076 0.061 Uiso 1 1 calc R . .
C4 C 0.8118(5) 0.9038(3) 0.0576(2) 0.0464(9) Uani 1 1 d . . .
C3 C 0.7852(5) 1.0044(3) 0.0935(2) 0.0508(9) Uani 1 1 d . . .
C23 C 0.9105(5) 0.7380(3) 0.3551(2) 0.0476(9) Uani 1 1 d . . .
C14 C 0.3986(5) 0.7369(3) 0.2067(2) 0.0470(9) Uani 1 1 d . . .
C19 C 0.3764(5) 0.7335(3) 0.1264(2) 0.0572(11) Uani 1 1 d . . .
H19 H 0.3289 0.7976 0.0889 0.069 Uiso 1 1 calc R . .
C22 C 0.8828(5) 0.8833(3) 0.4334(2) 0.0565(11) Uani 1 1 d . . .
H22A H 0.9419 0.8942 0.4786 0.068 Uiso 1 1 calc R . .
H22B H 0.7677 0.8581 0.4561 0.068 Uiso 1 1 calc R . .
C12 C 0.4079(5) 0.9790(3) 0.3061(3) 0.0582(11) Uani 1 1 d . . .
H12A H 0.2975 0.9755 0.3387 0.070 Uiso 1 1 calc R . .
H12B H 0.4015 1.0434 0.2562 0.070 Uiso 1 1 calc R . .
C15 C 0.4671(5) 0.6409(3) 0.2637(2) 0.0554(10) Uani 1 1 d . . .
H15 H 0.4817 0.6425 0.3176 0.066 Uiso 1 1 calc R . .
C16 C 0.5138(6) 0.5414(3) 0.2385(3) 0.0636(12) Uani 1 1 d . . .
H16 H 0.5592 0.4762 0.2758 0.076 Uiso 1 1 calc R . .
C21 C 0.8655(5) 0.9995(3) 0.3685(2) 0.0564(10) Uani 1 1 d . . .
H21A H 0.8437 1.0585 0.3971 0.068 Uiso 1 1 calc R . .
H21B H 0.9747 1.0153 0.3352 0.068 Uiso 1 1 calc R . .
C9 C 0.7121(5) 0.9017(3) -0.0052(2) 0.0559(10) Uani 1 1 d . . .
H9 H 0.6347 0.9630 -0.0246 0.067 Uiso 1 1 calc R . .
C17 C 0.4918(5) 0.5410(3) 0.1581(3) 0.0582(11) Uani 1 1 d . . .
C2 C 0.8901(5) 1.1172(3) 0.1759(3) 0.0564(10) Uani 1 1 d . . .
H2A H 0.8822 1.1853 0.1285 0.068 Uiso 1 1 calc R . .
H2B H 0.9962 1.1203 0.2009 0.068 Uiso 1 1 calc R . .
C1 C 0.7372(5) 1.1193(3) 0.2395(2) 0.0532(10) Uani 1 1 d . . .
H1A H 0.7473 1.1838 0.2618 0.064 Uiso 1 1 calc R . .
H1B H 0.6314 1.1314 0.2116 0.064 Uiso 1 1 calc R . .
C29 C 0.9397(6) 0.5888(3) 0.2830(3) 0.0612(11) Uani 1 1 d . . .
H29 H 0.8668 0.6352 0.2453 0.073 Uiso 1 1 calc R . .
C27 C 1.1058(6) 0.4138(3) 0.3312(3) 0.0615(11) Uani 1 1 d . . .
C18 C 0.4238(6) 0.6361(3) 0.1016(2) 0.0586(10) Uani 1 1 d . . .
H18 H 0.4101 0.6346 0.0475 0.070 Uiso 1 1 calc R . .
C7 C 0.8412(5) 0.7205(3) -0.0121(3) 0.0555(10) Uani 1 1 d . . .
C5 C 0.9297(6) 0.8125(3) 0.0848(3) 0.0618(11) Uani 1 1 d . . .
H5 H 1.0003 0.8133 0.1261 0.074 Uiso 1 1 calc R . .
C8 C 0.7239(5) 0.8111(3) -0.0401(3) 0.0589(11) Uani 1 1 d . . .
H8 H 0.6540 0.8108 -0.0819 0.071 Uiso 1 1 calc R . .
C25 C 1.1009(5) 0.5576(3) 0.4028(3) 0.0584(10) Uani 1 1 d . . .
H25 H 1.1367 0.5828 0.4456 0.070 Uiso 1 1 calc R . .
C26 C 1.1578(6) 0.4519(3) 0.3936(3) 0.0661(12) Uani 1 1 d . . .
H26 H 1.2326 0.4059 0.4303 0.079 Uiso 1 1 calc R . .
C24 C 0.9881(5) 0.6268(3) 0.3469(2) 0.0479(9) Uani 1 1 d . . .
C6 C 0.9431(6) 0.7209(3) 0.0510(3) 0.0636(12) Uani 1 1 d . . .
H6 H 1.0203 0.6595 0.0706 0.076 Uiso 1 1 calc R . .
C28 C 0.9972(6) 0.4838(4) 0.2740(3) 0.0695(12) Uani 1 1 d . . .
H28 H 0.9645 0.4592 0.2304 0.083 Uiso 1 1 calc R . .
C10 C 0.8599(6) 0.6284(4) -0.0514(3) 0.0690(12) Uani 1 1 d . . .
C30 C 1.1575(7) 0.3002(4) 0.3237(4) 0.0842(15) Uani 1 1 d . . .
C20 C 0.5464(7) 0.4381(4) 0.1332(3) 0.0747(13) Uani 1 1 d . . .
O2 O 0.2228(4) 0.9071(2) 0.20071(19) 0.0708(9) Uani 1 1 d . . .
O3 O 0.7829(3) 0.7826(2) 0.31629(17) 0.0610(8) Uani 1 1 d . . .
O1 O 0.6656(4) 1.0741(2) 0.0751(2) 0.0796(10) Uani 1 1 d . . .
O4 O 0.7331(7) 0.1801(7) 0.4964(3) 0.202(3) Uani 1 1 d . . .
O5 O 0.4799(7) 0.2653(6) 0.4966(7) 0.303(7) Uani 1 1 d . . .
O6 O 0.6063(13) 0.2722(4) 0.3821(4) 0.252(5) Uani 1 1 d . . .
O7 O 0.6897(11) 0.3840(7) 0.4494(5) 0.251(4) Uani 1 1 d . . .
H1N H 0.749(5) 0.952(3) 0.292(2) 0.053(11) Uiso 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
Cl1 O5 1.313(6) . ?
Cl1 O6 1.315(5) . ?
Cl1 O4 1.365(5) . ?
Cl1 O7 1.391(6) . ?
N3 C13 1.332(4) . ?
N3 C12 1.447(4) . ?
N1 C21 1.503(4) . ?
N1 C11 1.505(5) . ?
N1 C1 1.518(4) . ?
N2 C3 1.348(4) . ?
N2 C2 1.450(4) . ?
N4 C23 1.339(4) . ?
N4 C22 1.461(4) . ?
N5 C10 1.128(5) . ?
N6 C20 1.127(5) . ?
N7 C30 1.143(5) . ?
C13 O2 1.228(4) . ?
C13 C14 1.501(5) . ?
C11 C12 1.522(5) . ?
C4 C9 1.376(5) . ?
C4 C5 1.394(5) . ?
C4 C3 1.504(5) . ?
C3 O1 1.219(4) . ?
C23 O3 1.250(4) . ?
C23 C24 1.481(5) . ?
C14 C15 1.391(5) . ?
C14 C19 1.391(5) . ?
C19 C18 1.382(5) . ?
C22 C21 1.519(5) . ?
C15 C16 1.407(5) . ?
C16 C17 1.380(6) . ?
C9 C8 1.383(5) . ?
C17 C18 1.378(5) . ?
C17 C20 1.455(6) . ?
C2 C1 1.526(6) . ?
C29 C28 1.369(5) . ?
C29 C24 1.377(5) . ?
C27 C26 1.364(6) . ?
C27 C28 1.399(6) . ?
C27 C30 1.448(6) . ?
C7 C6 1.386(5) . ?
C7 C8 1.388(5) . ?
C7 C10 1.446(6) . ?
C5 C6 1.380(5) . ?
C25 C26 1.376(5) . ?
C25 C24 1.405(5) . ?

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 Cl1 O6 103.1(6) . . ?
O5 Cl1 O4 108.3(4) . . ?
O6 Cl1 O4 111.4(4) . . ?
O5 Cl1 O7 107.2(6) . . ?
O6 Cl1 O7 106.0(4) . . ?
O4 Cl1 O7 119.4(5) . . ?
C13 N3 C12 122.0(3) . . ?
C21 N1 C11 112.1(3) . . ?
C21 N1 C1 111.5(3) . . ?
C11 N1 C1 110.9(3) . . ?
C3 N2 C2 120.5(3) . . ?
C23 N4 C22 124.1(3) . . ?
O2 C13 N3 121.2(3) . . ?
O2 C13 C14 121.9(3) . . ?
N3 C13 C14 116.9(3) . . ?
N1 C11 C12 113.7(3) . . ?
C9 C4 C5 118.3(3) . . ?
C9 C4 C3 117.8(3) . . ?
C5 C4 C3 124.0(3) . . ?
O1 C3 N2 120.8(3) . . ?
O1 C3 C4 121.1(3) . . ?
N2 C3 C4 118.1(3) . . ?
O3 C23 N4 119.4(3) . . ?
O3 C23 C24 120.2(3) . . ?
N4 C23 C24 120.4(3) . . ?
C15 C14 C19 120.0(3) . . ?
C15 C14 C13 121.5(3) . . ?
C19 C14 C13 118.5(3) . . ?
C18 C19 C14 120.9(3) . . ?
N4 C22 C21 116.9(3) . . ?
N3 C12 C11 111.8(3) . . ?
C14 C15 C16 119.0(3) . . ?
C17 C16 C15 119.6(3) . . ?
N1 C21 C22 115.1(3) . . ?
C4 C9 C8 121.8(3) . . ?
C18 C17 C16 121.5(3) . . ?
C18 C17 C20 120.2(4) . . ?
C16 C17 C20 118.3(4) . . ?
N2 C2 C1 112.9(3) . . ?
N1 C1 C2 113.0(3) . . ?
C28 C29 C24 121.0(4) . . ?
C26 C27 C28 120.0(4) . . ?
C26 C27 C30 121.3(4) . . ?
C28 C27 C30 118.7(4) . . ?
C17 C18 C19 119.0(4) . . ?
C6 C7 C8 120.0(3) . . ?
C6 C7 C10 120.7(4) . . ?
C8 C7 C10 119.3(3) . . ?
C6 C5 C4 120.9(3) . . ?
C9 C8 C7 119.2(3) . . ?
C26 C25 C24 119.3(4) . . ?
C27 C26 C25 120.9(4) . . ?
C29 C24 C25 119.4(3) . . ?
C29 C24 C23 117.3(3) . . ?
C25 C24 C23 123.3(3) . . ?
C5 C6 C7 119.8(4) . . ?
C29 C28 C27 119.3(4) . . ?
N5 C10 C7 178.7(5) . . ?
N7 C30 C27 177.9(5) . . ?
N6 C20 C17 178.6(5) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.817
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.073
####################################################################### 
# 
# 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_4LH-4HF2-3H2O
_database_code_depnum_ccdc_archive 'CCDC 1041361'
_audit_update_record             
;
2015-04-23 deposited with the CCDC.
2015-04-23 downloaded from the CCDC.
;
_audit_creation_date             2015-04-17
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2015.02.26 svn.r3159 for OlexSys, GUI svn.r3563)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '4(C48 H40 N7 O6), 4(F2 H), 2(H2 O), H4 O '
_chemical_formula_sum            'C192 H172 F8 N28 O27'
_chemical_formula_weight         3455.58
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C  2/c '
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.7467(16)
_cell_length_b                   18.6826(16)
_cell_length_c                   16.7739(11)
_cell_angle_alpha                90
_cell_angle_beta                 111.627(4)
_cell_angle_gamma                90
_cell_volume                     8374.5(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12652
_cell_measurement_temperature    298(2)
_cell_measurement_theta_min      1.5852
_cell_measurement_theta_max      27.5367
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             3616
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   0.991
_exptl_transmission_factor_min   0.982
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            28319
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        24.370
_diffrn_reflns_theta_max         24.370
_diffrn_reflns_theta_min         1.52
_diffrn_ambient_temperature      298
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4867
_reflns_number_total             6757

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         8756
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0519
_refine_ls_restrained_S_all      1.161
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1233P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1470
_refine_ls_wR_factor_ref         0.1892
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 O7-H7B_$1
 0.85 with sigma of 0.02
 O7A-H7AA
 0.85 with sigma of 0.02
3. Others
 Fixed Sof: O7A(0.25)
4.a Riding coordinates:
 F2(H1C)
4.b Ternary CH refined with riding coordinates:
 N1(H1)
4.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1A,H1B), C17(H17A,H17B), C18(H18A,H18B), C34(H34A,H34B),
 C33(H33A,H33B)
4.d Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), C5(H5), C7(H7), C4(H4A), C8(H8), C14(H14), C11(H11), C15(H15),
  C16(H16), C24(H24), C23(H23), C20(H20), C21(H21), C26(H26), C29(H29),
 C30(H30), C32(H32), C37(H37), C39(H39), C36(H36), C40(H40), C41(H41), C46(H46),
  C42(H42), C44(H44), N7(H7A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N2 N 0.71851(13) 1.0795(2) 0.3899(2) 0.0704(11) Uani 1 1 d . . . . .
H2 H 0.6994 1.0989 0.4130 0.084 Uiso 1 1 calc R . . . .
N4 N 0.59211(15) 0.2277(2) 0.1768(2) 0.0809(12) Uani 1 1 d . . . . .
H4 H 0.5709 0.2059 0.1934 0.097 Uiso 1 1 calc R . . . .
N1 N 0.66494(15) 0.63660(16) 0.3433(3) 0.0739(11) Uani 1 1 d . . . . .
H1 H 0.6681 0.5858 0.3589 0.089 Uiso 1 1 calc R . . . .
N3 N 0.71682(16) 1.4885(2) 0.3724(3) 0.0996(14) Uani 1 1 d . . . . .
N6 N 0.4610(2) -0.0382(3) 0.6366(4) 0.140(2) Uani 1 1 d . . . . .
N5 N 0.61542(17) -0.1790(3) 0.1966(4) 0.131(2) Uani 1 1 d . . . . .
C5 C 0.69203(18) 0.9674(3) 0.4309(3) 0.0780(14) Uani 1 1 d . . . . .
H5 H 0.6751 0.9931 0.4592 0.094 Uiso 1 1 calc R . . . .
C10 C 0.7369(2) 1.2029(2) 0.3692(3) 0.0675(13) Uani 1 1 d . . . . .
C7 C 0.74286(17) 0.9631(3) 0.3481(3) 0.0784(14) Uani 1 1 d . . . . .
H7 H 0.7607 0.9859 0.3190 0.094 Uiso 1 1 calc R . . . .
C3 C 0.7154(2) 0.8544(3) 0.3910(3) 0.0694(14) Uani 1 1 d . . . . .
C4 C 0.69047(19) 0.8939(3) 0.4311(3) 0.0819(15) Uani 1 1 d . . . . .
H4A H 0.6722 0.8707 0.4590 0.098 Uiso 1 1 calc R . . . .
C12 C 0.7279(2) 1.3510(3) 0.3748(3) 0.0733(14) Uani 1 1 d . . . . .
C6 C 0.71865(18) 1.0040(3) 0.3889(3) 0.0640(12) Uani 1 1 d . . . . .
C2 C 0.72393(17) 0.7379(2) 0.3399(3) 0.0782(14) Uani 1 1 d . . . . .
H2A H 0.7582 0.7464 0.3450 0.094 Uiso 1 1 calc R . . . .
H2B H 0.7021 0.7501 0.2820 0.094 Uiso 1 1 calc R . . . .
C8 C 0.74146(18) 0.8895(3) 0.3490(3) 0.0813(14) Uani 1 1 d . . . . .
H8 H 0.7583 0.8633 0.3209 0.098 Uiso 1 1 calc R . . . .
C14 C 0.7716(2) 1.3207(3) 0.3743(3) 0.0851(15) Uani 1 1 d . . . . .
H14 H 0.7982 1.3498 0.3762 0.102 Uiso 1 1 calc R . . . .
C9 C 0.7440(2) 1.1252(3) 0.3596(3) 0.0726(14) Uani 1 1 d . . . . .
C11 C 0.69359(19) 1.2337(3) 0.3727(3) 0.0735(14) Uani 1 1 d . . . . .
H11 H 0.6675 1.2048 0.3737 0.088 Uiso 1 1 calc R . . . .
C1 C 0.71744(17) 0.6611(2) 0.3565(3) 0.0808(14) Uani 1 1 d . . . . .
H1A H 0.7388 0.6505 0.4153 0.097 Uiso 1 1 calc R . . . .
H1B H 0.7294 0.6327 0.3196 0.097 Uiso 1 1 calc R . . . .
C15 C 0.77578(19) 1.2483(3) 0.3710(3) 0.0817(14) Uani 1 1 d . . . . .
H15 H 0.8053 1.2286 0.3700 0.098 Uiso 1 1 calc R . . . .
C13 C 0.72204(18) 1.4276(3) 0.3738(3) 0.0813(15) Uani 1 1 d . . . . .
C16 C 0.68957(19) 1.3067(3) 0.3746(3) 0.0777(14) Uani 1 1 d . . . . .
H16 H 0.6603 1.3268 0.3759 0.093 Uiso 1 1 calc R . . . .
C31 C 0.61665(18) 0.1073(3) 0.1583(4) 0.0770(14) Uani 1 1 d . . . . .
C24 C 0.6216(2) 0.4201(3) 0.1683(3) 0.0827(15) Uani 1 1 d . . . . .
H24 H 0.6392 0.4494 0.1444 0.099 Uiso 1 1 calc R . . . .
C17 C 0.62978(18) 0.6389(2) 0.2513(3) 0.0815(14) Uani 1 1 d . . . . .
H17A H 0.5967 0.6524 0.2488 0.098 Uiso 1 1 calc R . . . .
H17B H 0.6410 0.6752 0.2211 0.098 Uiso 1 1 calc R . . . .
C23 C 0.61914(19) 0.3475(3) 0.1522(3) 0.0855(15) Uani 1 1 d . . . . .
H23 H 0.6354 0.3287 0.1181 0.103 Uiso 1 1 calc R . . . .
C22 C 0.5930(2) 0.3020(3) 0.1855(3) 0.0745(14) Uani 1 1 d . . . . .
C19 C 0.59864(19) 0.4501(3) 0.2189(3) 0.0707(13) Uani 1 1 d . . . . .
C20 C 0.57061(18) 0.4061(3) 0.2500(3) 0.0755(14) Uani 1 1 d . . . . .
H20 H 0.5534 0.4255 0.2823 0.091 Uiso 1 1 calc R . . . .
C27 C 0.61569(18) -0.0415(3) 0.1766(4) 0.0825(14) Uani 1 1 d . . . . .
C28 C 0.61563(18) -0.1189(4) 0.1870(4) 0.0959(17) Uani 1 1 d . . . . .
C21 C 0.56792(18) 0.3340(3) 0.2338(3) 0.0804(14) Uani 1 1 d . . . . .
H21 H 0.5489 0.3054 0.2555 0.097 Uiso 1 1 calc R . . . .
C26 C 0.6018(2) 0.0758(3) 0.2199(4) 0.0954(16) Uani 1 1 d . . . . .
H26 H 0.5922 0.1048 0.2562 0.114 Uiso 1 1 calc R . . . .
C29 C 0.6306(2) -0.0118(4) 0.1156(4) 0.1122(19) Uani 1 1 d . . . . .
H29 H 0.6401 -0.0407 0.0791 0.135 Uiso 1 1 calc R . . . .
C25 C 0.6194(2) 0.1849(3) 0.1462(4) 0.0849(15) Uani 1 1 d . . . . .
C18 C 0.62680(19) 0.5684(2) 0.2076(3) 0.0846(15) Uani 1 1 d . . . . .
H18A H 0.6087 0.5734 0.1463 0.102 Uiso 1 1 calc R . . . .
H18B H 0.6601 0.5506 0.2171 0.102 Uiso 1 1 calc R . . . .
C30 C 0.6316(2) 0.0615(4) 0.1089(4) 0.1077(18) Uani 1 1 d . . . . .
H30 H 0.6430 0.0809 0.0685 0.129 Uiso 1 1 calc R . . . .
C32 C 0.60101(19) 0.0026(3) 0.2286(4) 0.0981(16) Uani 1 1 d . . . . .
H32 H 0.5905 -0.0172 0.2699 0.118 Uiso 1 1 calc R . . . .
C38 C 0.5640(2) 0.3732(3) 0.4782(3) 0.0719(13) Uani 1 1 d . . . . .
C35 C 0.6083(2) 0.5002(3) 0.4614(3) 0.0731(13) Uani 1 1 d . . . . .
C37 C 0.53615(19) 0.4344(3) 0.4559(3) 0.0756(14) Uani 1 1 d . . . . .
H37 H 0.5022 0.4331 0.4463 0.091 Uiso 1 1 calc R . . . .
C39 C 0.6145(2) 0.3751(3) 0.4910(3) 0.0815(14) Uani 1 1 d . . . . .
H39 H 0.6335 0.3335 0.5047 0.098 Uiso 1 1 calc R . . . .
C34 C 0.6066(2) 0.6224(3) 0.4184(3) 0.0972(16) Uani 1 1 d . . . . .
H34A H 0.5919 0.6442 0.4561 0.117 Uiso 1 1 calc R . . . .
H34B H 0.5801 0.6107 0.3644 0.117 Uiso 1 1 calc R . . . .
C36 C 0.5581(2) 0.4978(3) 0.4476(3) 0.0796(14) Uani 1 1 d . . . . .
H36 H 0.5389 0.5393 0.4327 0.096 Uiso 1 1 calc R . . . .
C40 C 0.63595(19) 0.4389(3) 0.4832(3) 0.0783(14) Uani 1 1 d . . . . .
H40 H 0.6699 0.4405 0.4929 0.094 Uiso 1 1 calc R . . . .
C33 C 0.6441(2) 0.6720(2) 0.4044(3) 0.0940(16) Uani 1 1 d . . . . .
H33A H 0.6710 0.6820 0.4586 0.113 Uiso 1 1 calc R . . . .
H33B H 0.6281 0.7169 0.3804 0.113 Uiso 1 1 calc R . . . .
C43 C 0.4756(2) 0.0911(3) 0.5934(4) 0.0906(16) Uani 1 1 d . . . . .
C47 C 0.50054(19) 0.2262(3) 0.5539(4) 0.0822(15) Uani 1 1 d . . . . .
C41 C 0.4799(2) 0.2160(3) 0.6178(4) 0.1021(17) Uani 1 1 d . . . . .
H41 H 0.4747 0.2550 0.6479 0.122 Uiso 1 1 calc R . . . .
C46 C 0.50624(18) 0.1674(3) 0.5093(3) 0.0892(15) Uani 1 1 d . . . . .
H46 H 0.5188 0.1734 0.4659 0.107 Uiso 1 1 calc R . . . .
C42 C 0.4677(2) 0.1487(4) 0.6349(4) 0.1026(17) Uani 1 1 d . . . . .
H42 H 0.4536 0.1425 0.6762 0.123 Uiso 1 1 calc R . . . .
C44 C 0.4938(2) 0.0999(3) 0.5273(4) 0.1016(17) Uani 1 1 d . . . . .
H44 H 0.4975 0.0607 0.4960 0.122 Uiso 1 1 calc R . . . .
C45 C 0.4665(2) 0.0192(4) 0.6160(4) 0.1125(19) Uani 1 1 d . . . . .
N7 N 0.54316(16) 0.3066(2) 0.4891(3) 0.0823(12) Uani 1 1 d . . . . .
H7A H 0.5474 0.2700 0.4615 0.099 Uiso 1 1 calc R . . . .
O1 O 0.71251(12) 0.78152(17) 0.39898(19) 0.0843(10) Uani 1 1 d . . . . .
O3 O 0.60116(11) 0.52039(18) 0.24316(19) 0.0803(9) Uani 1 1 d . . . . .
O2 O 0.63434(12) 0.56036(18) 0.4567(2) 0.0893(10) Uani 1 1 d . . . . .
C48 C 0.5172(2) 0.2981(3) 0.5407(4) 0.0885(16) Uani 1 1 d . . . . .
O6 O 0.77308(14) 1.10459(16) 0.3249(2) 0.0949(12) Uani 1 1 d . . . . .
O4 O 0.50653(15) 0.3490(2) 0.5785(3) 0.1197(13) Uani 1 1 d . . . . .
O5 O 0.64559(16) 0.2092(2) 0.1085(3) 0.1230(15) Uani 1 1 d . . . . .
F1 F 0.64611(11) 0.11604(14) 0.4617(2) 0.1189(11) Uani 1 1 d . . . A 1
F2 F 0.58922(16) 0.20355(17) 0.4238(3) 0.198(2) Uani 1 1 d . . . B 2
H1C H 0.6203 0.1637 0.4502 0.21(4) Uiso 1 1 d R . . . .
O7 O 0.5000 0.1804(3) 0.2500 0.183(3) Uani 1 2 d DS T P . .
O7A O 0.5000 0.6279(8) 0.2500 0.148(4) Uani 0.5 2 d DS T P . .
H7B H 0.5350(7) 0.176(2) 0.275(3) 0.09(2) Uiso 1 1 d D . . . .
H7AA H 0.497(10) 0.655(7) 0.289(10) 0.61(11) 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
N2 H2 0.8600 . ?
N2 C6 1.410(5) . ?
N2 C9 1.342(6) . ?
N4 H4 0.8600 . ?
N4 C22 1.396(6) . ?
N4 C25 1.347(6) . ?
N1 H1 0.9800 . ?
N1 C1 1.513(5) . ?
N1 C17 1.502(5) . ?
N1 C33 1.517(5) . ?
N3 C13 1.147(5) . ?
N6 C45 1.156(7) . ?
N5 C28 1.135(6) . ?
C5 H5 0.9300 . ?
C5 C4 1.373(6) . ?
C5 C6 1.395(6) . ?
C10 C9 1.482(6) . ?
C10 C11 1.393(6) . ?
C10 C15 1.394(6) . ?
C7 H7 0.9300 . ?
C7 C6 1.374(6) . ?
C7 C8 1.377(6) . ?
C3 C4 1.366(6) . ?
C3 C8 1.369(6) . ?
C3 O1 1.374(5) . ?
C4 H4A 0.9300 . ?
C12 C14 1.380(6) . ?
C12 C13 1.440(7) . ?
C12 C16 1.378(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.487(5) . ?
C2 O1 1.412(5) . ?
C8 H8 0.9300 . ?
C14 H14 0.9300 . ?
C14 C15 1.361(6) . ?
C9 O6 1.242(5) . ?
C11 H11 0.9300 . ?
C11 C16 1.370(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C31 C26 1.386(6) . ?
C31 C25 1.471(7) . ?
C31 C30 1.366(6) . ?
C24 H24 0.9300 . ?
C24 C23 1.381(6) . ?
C24 C19 1.372(6) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.495(6) . ?
C23 H23 0.9300 . ?
C23 C22 1.382(6) . ?
C22 C21 1.401(6) . ?
C19 C20 1.381(6) . ?
C19 O3 1.370(5) . ?
C20 H20 0.9300 . ?
C20 C21 1.370(5) . ?
C27 C28 1.456(8) . ?
C27 C29 1.365(7) . ?
C27 C32 1.375(7) . ?
C21 H21 0.9300 . ?
C26 H26 0.9300 . ?
C26 C32 1.377(6) . ?
C29 H29 0.9300 . ?
C29 C30 1.374(7) . ?
C25 O5 1.233(6) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 O3 1.425(5) . ?
C30 H30 0.9300 . ?
C32 H32 0.9300 . ?
C38 C37 1.367(6) . ?
C38 C39 1.386(6) . ?
C38 N7 1.423(5) . ?
C35 C36 1.375(6) . ?
C35 C40 1.365(6) . ?
C35 O2 1.369(5) . ?
C37 H37 0.9300 . ?
C37 C36 1.373(6) . ?
C39 H39 0.9300 . ?
C39 C40 1.370(6) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 C33 1.504(6) . ?
C34 O2 1.420(5) . ?
C36 H36 0.9300 . ?
C40 H40 0.9300 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C43 C42 1.345(7) . ?
C43 C44 1.400(7) . ?
C43 C45 1.446(8) . ?
C47 C41 1.415(6) . ?
C47 C46 1.373(6) . ?
C47 C48 1.471(7) . ?
C41 H41 0.9300 . ?
C41 C42 1.364(7) . ?
C46 H46 0.9300 . ?
C46 C44 1.373(6) . ?
C42 H42 0.9300 . ?
C44 H44 0.9300 . ?
N7 H7A 0.8600 . ?
N7 C48 1.344(6) . ?
C48 O4 1.243(5) . ?
F1 H1C 1.1301 . ?
F2 H1C 1.1202 . ?
O7 H7B 0.939(19) . ?
O7A H7AA 0.85(2) . ?

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
C6 N2 H2 115.5 . . ?
C9 N2 H2 115.5 . . ?
C9 N2 C6 128.9(4) . . ?
C22 N4 H4 115.1 . . ?
C25 N4 H4 115.1 . . ?
C25 N4 C22 129.8(5) . . ?
C1 N1 H1 105.3 . . ?
C1 N1 C33 113.0(4) . . ?
C17 N1 H1 105.3 . . ?
C17 N1 C1 113.5(4) . . ?
C17 N1 C33 113.5(4) . . ?
C33 N1 H1 105.3 . . ?
C4 C5 H5 119.5 . . ?
C4 C5 C6 121.1(5) . . ?
C6 C5 H5 119.5 . . ?
C11 C10 C9 124.8(5) . . ?
C11 C10 C15 118.0(4) . . ?
C15 C10 C9 117.1(5) . . ?
C6 C7 H7 119.1 . . ?
C6 C7 C8 121.8(4) . . ?
C8 C7 H7 119.1 . . ?
C4 C3 C8 118.8(4) . . ?
C4 C3 O1 115.2(5) . . ?
C8 C3 O1 126.0(5) . . ?
C5 C4 H4A 119.5 . . ?
C3 C4 C5 121.0(5) . . ?
C3 C4 H4A 119.5 . . ?
C14 C12 C13 120.8(5) . . ?
C16 C12 C14 118.8(4) . . ?
C16 C12 C13 120.5(5) . . ?
C5 C6 N2 118.7(5) . . ?
C7 C6 N2 124.4(5) . . ?
C7 C6 C5 116.9(4) . . ?
H2A C2 H2B 108.1 . . ?
C1 C2 H2A 109.6 . . ?
C1 C2 H2B 109.6 . . ?
O1 C2 H2A 109.6 . . ?
O1 C2 H2B 109.6 . . ?
O1 C2 C1 110.4(4) . . ?
C7 C8 H8 119.8 . . ?
C3 C8 C7 120.5(4) . . ?
C3 C8 H8 119.8 . . ?
C12 C14 H14 119.9 . . ?
C15 C14 C12 120.3(4) . . ?
C15 C14 H14 119.9 . . ?
N2 C9 C10 117.8(6) . . ?
O6 C9 N2 122.3(4) . . ?
O6 C9 C10 119.9(5) . . ?
C10 C11 H11 120.1 . . ?
C16 C11 C10 119.8(4) . . ?
C16 C11 H11 120.1 . . ?
N1 C1 H1A 108.1 . . ?
N1 C1 H1B 108.1 . . ?
C2 C1 N1 116.8(3) . . ?
C2 C1 H1A 108.1 . . ?
C2 C1 H1B 108.1 . . ?
H1A C1 H1B 107.3 . . ?
C10 C15 H15 119.2 . . ?
C14 C15 C10 121.5(5) . . ?
C14 C15 H15 119.2 . . ?
N3 C13 C12 179.2(6) . . ?
C12 C16 H16 119.2 . . ?
C11 C16 C12 121.6(4) . . ?
C11 C16 H16 119.2 . . ?
C26 C31 C25 124.7(6) . . ?
C30 C31 C26 116.0(5) . . ?
C30 C31 C25 119.3(6) . . ?
C23 C24 H24 119.4 . . ?
C19 C24 H24 119.4 . . ?
C19 C24 C23 121.3(5) . . ?
N1 C17 H17A 109.2 . . ?
N1 C17 H17B 109.2 . . ?
H17A C17 H17B 107.9 . . ?
C18 C17 N1 111.9(3) . . ?
C18 C17 H17A 109.2 . . ?
C18 C17 H17B 109.2 . . ?
C24 C23 H23 119.3 . . ?
C24 C23 C22 121.5(5) . . ?
C22 C23 H23 119.3 . . ?
N4 C22 C21 119.4(5) . . ?
C23 C22 N4 124.1(6) . . ?
C23 C22 C21 116.4(5) . . ?
C24 C19 C20 118.2(5) . . ?
O3 C19 C24 126.2(5) . . ?
O3 C19 C20 115.6(5) . . ?
C19 C20 H20 119.8 . . ?
C21 C20 C19 120.5(5) . . ?
C21 C20 H20 119.8 . . ?
C29 C27 C28 120.6(6) . . ?
C29 C27 C32 119.1(5) . . ?
C32 C27 C28 120.3(6) . . ?
N5 C28 C27 178.7(7) . . ?
C22 C21 H21 119.0 . . ?
C20 C21 C22 122.0(5) . . ?
C20 C21 H21 119.0 . . ?
C31 C26 H26 119.3 . . ?
C32 C26 C31 121.5(5) . . ?
C32 C26 H26 119.3 . . ?
C27 C29 H29 120.4 . . ?
C27 C29 C30 119.2(6) . . ?
C30 C29 H29 120.4 . . ?
N4 C25 C31 117.6(6) . . ?
O5 C25 N4 121.9(5) . . ?
O5 C25 C31 120.5(6) . . ?
C17 C18 H18A 110.3 . . ?
C17 C18 H18B 110.3 . . ?
H18A C18 H18B 108.5 . . ?
O3 C18 C17 107.1(4) . . ?
O3 C18 H18A 110.3 . . ?
O3 C18 H18B 110.3 . . ?
C31 C30 C29 123.7(5) . . ?
C31 C30 H30 118.2 . . ?
C29 C30 H30 118.2 . . ?
C27 C32 C26 120.5(5) . . ?
C27 C32 H32 119.8 . . ?
C26 C32 H32 119.8 . . ?
C37 C38 C39 119.7(5) . . ?
C37 C38 N7 122.3(5) . . ?
C39 C38 N7 118.0(5) . . ?
C40 C35 C36 119.3(5) . . ?
C40 C35 O2 115.2(6) . . ?
O2 C35 C36 125.5(5) . . ?
C38 C37 H37 119.8 . . ?
C38 C37 C36 120.3(5) . . ?
C36 C37 H37 119.8 . . ?
C38 C39 H39 120.3 . . ?
C40 C39 C38 119.4(4) . . ?
C40 C39 H39 120.3 . . ?
H34A C34 H34B 108.8 . . ?
C33 C34 H34A 110.8 . . ?
C33 C34 H34B 110.8 . . ?
O2 C34 H34A 110.8 . . ?
O2 C34 H34B 110.8 . . ?
O2 C34 C33 105.0(4) . . ?
C35 C36 H36 119.9 . . ?
C37 C36 C35 120.2(4) . . ?
C37 C36 H36 119.9 . . ?
C35 C40 C39 121.1(5) . . ?
C35 C40 H40 119.5 . . ?
C39 C40 H40 119.5 . . ?
N1 C33 H33A 109.9 . . ?
N1 C33 H33B 109.9 . . ?
C34 C33 N1 108.7(4) . . ?
C34 C33 H33A 109.9 . . ?
C34 C33 H33B 109.9 . . ?
H33A C33 H33B 108.3 . . ?
C42 C43 C44 120.0(5) . . ?
C42 C43 C45 121.8(7) . . ?
C44 C43 C45 118.2(6) . . ?
C41 C47 C48 119.2(6) . . ?
C46 C47 C41 118.2(5) . . ?
C46 C47 C48 122.5(6) . . ?
C47 C41 H41 120.1 . . ?
C42 C41 C47 119.7(5) . . ?
C42 C41 H41 120.1 . . ?
C47 C46 H46 119.3 . . ?
C47 C46 C44 121.4(5) . . ?
C44 C46 H46 119.3 . . ?
C43 C42 C41 121.5(6) . . ?
C43 C42 H42 119.3 . . ?
C41 C42 H42 119.3 . . ?
C43 C44 H44 120.5 . . ?
C46 C44 C43 119.0(5) . . ?
C46 C44 H44 120.5 . . ?
N6 C45 C43 177.4(7) . . ?
C38 N7 H7A 118.4 . . ?
C48 N7 C38 123.1(4) . . ?
C48 N7 H7A 118.4 . . ?
C3 O1 C2 117.7(4) . . ?
C19 O3 C18 117.3(4) . . ?
C35 O2 C34 117.9(4) . . ?
N7 C48 C47 119.5(6) . . ?
O4 C48 C47 117.9(6) . . ?
O4 C48 N7 122.6(5) . . ?

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
N4 C22 C21 C20 175.0(4) . . . . ?
N1 C17 C18 O3 70.0(4) . . . . ?
C10 C11 C16 C12 -1.1(7) . . . . ?
C4 C5 C6 N2 179.3(4) . . . . ?
C4 C5 C6 C7 0.1(6) . . . . ?
C4 C3 C8 C7 0.6(6) . . . . ?
C4 C3 O1 C2 161.4(4) . . . . ?
C12 C14 C15 C10 -0.9(7) . . . . ?
C6 N2 C9 C10 -179.9(4) . . . . ?
C6 N2 C9 O6 -0.3(7) . . . . ?
C6 C5 C4 C3 0.7(6) . . . . ?
C6 C7 C8 C3 0.2(6) . . . . ?
C8 C7 C6 N2 -179.7(4) . . . . ?
C8 C7 C6 C5 -0.6(6) . . . . ?
C8 C3 C4 C5 -1.1(6) . . . . ?
C8 C3 O1 C2 -20.2(6) . . . . ?
C14 C12 C16 C11 -1.1(7) . . . . ?
C9 N2 C6 C5 174.7(4) . . . . ?
C9 N2 C6 C7 -6.3(6) . . . . ?
C9 C10 C11 C16 -174.7(4) . . . . ?
C9 C10 C15 C14 175.9(4) . . . . ?
C11 C10 C9 N2 -28.2(6) . . . . ?
C11 C10 C9 O6 152.1(4) . . . . ?
C11 C10 C15 C14 -1.3(7) . . . . ?
C1 N1 C17 C18 94.2(4) . . . . ?
C1 N1 C33 C34 -152.2(4) . . . . ?
C1 C2 O1 C3 -178.3(3) . . . . ?
C15 C10 C9 N2 154.8(4) . . . . ?
C15 C10 C9 O6 -24.9(6) . . . . ?
C15 C10 C11 C16 2.3(6) . . . . ?
C13 C12 C14 C15 -176.8(4) . . . . ?
C13 C12 C16 C11 177.8(4) . . . . ?
C16 C12 C14 C15 2.1(7) . . . . ?
C31 C26 C32 C27 0.9(8) . . . . ?
C24 C23 C22 N4 -175.1(4) . . . . ?
C24 C23 C22 C21 2.1(6) . . . . ?
C24 C19 C20 C21 2.9(6) . . . . ?
C24 C19 O3 C18 5.2(6) . . . . ?
C17 N1 C1 C2 67.2(5) . . . . ?
C17 N1 C33 C34 76.7(5) . . . . ?
C17 C18 O3 C19 -173.3(3) . . . . ?
C23 C24 C19 C20 -3.2(7) . . . . ?
C23 C24 C19 O3 175.8(4) . . . . ?
C23 C22 C21 C20 -2.4(6) . . . . ?
C22 N4 C25 C31 169.6(4) . . . . ?
C22 N4 C25 O5 -11.0(7) . . . . ?
C19 C24 C23 C22 0.7(7) . . . . ?
C19 C20 C21 C22 -0.1(6) . . . . ?
C20 C19 O3 C18 -175.8(4) . . . . ?
C27 C29 C30 C31 -2.3(8) . . . . ?
C28 C27 C29 C30 -178.2(5) . . . . ?
C28 C27 C32 C26 178.9(4) . . . . ?
C26 C31 C25 N4 -21.3(7) . . . . ?
C26 C31 C25 O5 159.3(5) . . . . ?
C26 C31 C30 C29 2.4(8) . . . . ?
C29 C27 C32 C26 -0.6(7) . . . . ?
C25 N4 C22 C23 9.1(7) . . . . ?
C25 N4 C22 C21 -168.0(4) . . . . ?
C25 C31 C26 C32 -178.8(5) . . . . ?
C25 C31 C30 C29 179.7(5) . . . . ?
C30 C31 C26 C32 -1.7(7) . . . . ?
C30 C31 C25 N4 161.6(4) . . . . ?
C30 C31 C25 O5 -17.7(7) . . . . ?
C32 C27 C29 C30 1.2(8) . . . . ?
C38 C37 C36 C35 0.2(7) . . . . ?
C38 C39 C40 C35 -1.3(7) . . . . ?
C38 N7 C48 C47 -174.9(4) . . . . ?
C38 N7 C48 O4 4.8(7) . . . . ?
C37 C38 C39 C40 1.7(7) . . . . ?
C37 C38 N7 C48 -52.9(6) . . . . ?
C39 C38 C37 C36 -1.1(7) . . . . ?
C39 C38 N7 C48 127.0(5) . . . . ?
C36 C35 C40 C39 0.4(7) . . . . ?
C36 C35 O2 C34 -13.2(6) . . . . ?
C40 C35 C36 C37 0.1(7) . . . . ?
C40 C35 O2 C34 167.9(4) . . . . ?
C33 N1 C1 C2 -63.8(5) . . . . ?
C33 N1 C17 C18 -135.0(4) . . . . ?
C33 C34 O2 C35 -167.4(4) . . . . ?
C47 C41 C42 C43 1.2(8) . . . . ?
C47 C46 C44 C43 -0.8(7) . . . . ?
C41 C47 C46 C44 -2.0(7) . . . . ?
C41 C47 C48 N7 170.6(5) . . . . ?
C41 C47 C48 O4 -9.1(7) . . . . ?
C46 C47 C41 C42 1.8(7) . . . . ?
C46 C47 C48 N7 -6.4(7) . . . . ?
C46 C47 C48 O4 173.9(5) . . . . ?
C42 C43 C44 C46 3.8(8) . . . . ?
C44 C43 C42 C41 -4.1(8) . . . . ?
C45 C43 C42 C41 174.9(5) . . . . ?
C45 C43 C44 C46 -175.2(4) . . . . ?
N7 C38 C37 C36 178.7(4) . . . . ?
N7 C38 C39 C40 -178.2(4) . . . . ?
O1 C3 C4 C5 177.4(4) . . . . ?
O1 C3 C8 C7 -177.7(4) . . . . ?
O1 C2 C1 N1 64.7(5) . . . . ?
O3 C19 C20 C21 -176.2(4) . . . . ?
O2 C35 C36 C37 -178.7(4) . . . . ?
O2 C35 C40 C39 179.4(4) . . . . ?
O2 C34 C33 N1 62.0(5) . . . . ?
C48 C47 C41 C42 -175.3(5) . . . . ?
C48 C47 C46 C44 175.0(5) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_2LH-Br
_database_code_depnum_ccdc_archive 'CCDC 1041362'
_audit_update_record             
;
2015-04-10 deposited with the CCDC.
2015-04-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H40 N7 O6, Br'
_chemical_formula_sum            'C48 H40 Br N7 O6'

_chemical_formula_weight         890.77

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.4588(5)
_cell_length_b                   13.6915(7)
_cell_length_c                   20.4866(10)
_cell_angle_alpha                91.493(3)
_cell_angle_beta                 94.733(2)
_cell_angle_gamma                103.295(2)
_cell_volume                     2570.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    12652
_cell_measurement_theta_min      1.91
_cell_measurement_theta_max      25.49

_exptl_crystal_description       'thin plate'
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             920.0
_exptl_absorpt_coefficient_mu    0.849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.816
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            39258
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.53
_diffrn_reflns_theta_max         28.65
_reflns_number_total             13138
_reflns_number_gt                7346
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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.
;
_PLAT606_ALERT_4_G               
;
Problem:VERY LARGE Solvent Accessible VOID(S) in Structure
Response: SQUEEZE has been performed to the disordered solvent molecule. 
This calculated amount of 554 electrons per unit cell or 98 electrons per 
molecule may be attributed to two water and two DMF molecules.
;

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 0.000 0.500 554 98 ' '

_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)+(0.1147P)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         13168
_refine_ls_number_parameters     569
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0573
_refine_ls_wR_factor_ref         0.1852
_refine_ls_wR_factor_gt          0.1704
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.005

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
Br2 Br 0.39985(12) 0.08945(7) 0.29494(5) 0.1124(3) Uani 0.50 1 d P . .
Br1 Br 0.0000 0.5000 0.0000 0.05548(15) Uani 1 2 d S . .
N1 N 0.18843(19) 0.75781(14) 0.16424(10) 0.0386(4) Uani 1 1 d . . .
N2 N -0.4497(2) 1.09892(14) 0.14566(10) 0.0444(5) Uani 1 1 d . . .
H2N H -0.4873 1.1061 0.1818 0.053 Uiso 1 1 calc R . .
N3 N 0.8158(2) 0.44058(14) 0.14007(10) 0.0438(5) Uani 1 1 d . . .
H3N H 0.8545 0.4371 0.1038 0.053 Uiso 1 1 calc R . .
N4 N 0.6657(2) 0.54381(19) 0.43941(11) 0.0607(6) Uani 1 1 d . . .
H4N H 0.6752 0.4874 0.4230 0.073 Uiso 1 1 calc R . .
C10 C -0.5522(2) 1.24010(16) 0.11665(11) 0.0374(5) Uani 1 1 d . . .
C4 C -0.2388(2) 0.91641(17) 0.09070(12) 0.0432(5) Uani 1 1 d . . .
H4 H -0.2124 0.8901 0.0525 0.052 Uiso 1 1 calc R . .
C21 C 0.6562(2) 0.53227(18) 0.08709(12) 0.0425(5) Uani 1 1 d . . .
H21 H 0.6674 0.5007 0.0477 0.051 Uiso 1 1 calc R . .
C9 C -0.4776(2) 1.15887(17) 0.09711(12) 0.0417(5) Uani 1 1 d . . .
C20 C 0.5667(2) 0.60082(17) 0.08768(12) 0.0418(5) Uani 1 1 d . . .
H20 H 0.5183 0.6147 0.0489 0.050 Uiso 1 1 calc R . .
C24 C 0.7277(2) 0.51143(16) 0.14437(12) 0.0393(5) Uani 1 1 d . . .
C12 C -0.7024(2) 1.35241(17) 0.08080(12) 0.0441(6) Uani 1 1 d . . .
H12 H -0.7583 1.3756 0.0479 0.053 Uiso 1 1 calc R . .
C26 C 0.9170(2) 0.29825(17) 0.16370(13) 0.0439(6) Uani 1 1 d . . .
C25 C 0.8453(2) 0.37864(18) 0.18613(12) 0.0438(5) Uani 1 1 d . . .
C6 C -0.3653(2) 1.02551(16) 0.14394(12) 0.0404(5) Uani 1 1 d . . .
C19 C 0.5509(2) 0.64731(16) 0.14591(11) 0.0385(5) Uani 1 1 d . . .
C3 C -0.1899(2) 0.88754(17) 0.15095(12) 0.0431(5) Uani 1 1 d . . .
C13 C -0.6856(2) 1.39400(16) 0.14435(12) 0.0398(5) Uani 1 1 d . . .
C17 C 0.2966(2) 0.80683(18) 0.11773(13) 0.0461(6) Uani 1 1 d . . .
H17A H 0.2450 0.8291 0.0802 0.055 Uiso 1 1 calc R . .
H17B H 0.3629 0.8653 0.1397 0.055 Uiso 1 1 calc R . .
C11 C -0.6344(2) 1.27585(17) 0.06749(12) 0.0408(5) Uani 1 1 d . . .
H11 H -0.6439 1.2479 0.0250 0.049 Uiso 1 1 calc R . .
C15 C -0.5360(3) 1.28316(17) 0.17935(12) 0.0453(6) Uani 1 1 d . . .
H16 H -0.4805 1.2599 0.2124 0.054 Uiso 1 1 calc R . .
C14 C -0.6017(3) 1.36051(18) 0.19311(13) 0.0471(6) Uani 1 1 d . . .
H15 H -0.5894 1.3900 0.2352 0.057 Uiso 1 1 calc R . .
C5 C -0.3276(2) 0.98480(17) 0.08701(12) 0.0440(5) Uani 1 1 d . . .
H5 H -0.3617 1.0032 0.0463 0.053 Uiso 1 1 calc R . .
C1 C 0.0399(2) 0.70978(17) 0.13074(13) 0.0465(6) Uani 1 1 d . . .
H1A H 0.0525 0.6674 0.0940 0.056 Uiso 1 1 calc R . .
H1B H -0.0145 0.6664 0.1613 0.056 Uiso 1 1 calc R . .
C22 C 0.6253(2) 0.62832(18) 0.20386(12) 0.0445(6) Uani 1 1 d . . .
H22 H 0.6162 0.6614 0.2430 0.053 Uiso 1 1 calc R . .
C23 C 0.7129(2) 0.56022(18) 0.20327(12) 0.0441(5) Uani 1 1 d . . .
H23 H 0.7618 0.5469 0.2421 0.053 Uiso 1 1 calc R . .
C27 C 0.8957(3) 0.25936(19) 0.09942(13) 0.0506(6) Uani 1 1 d . . .
H27 H 0.8391 0.2857 0.0684 0.061 Uiso 1 1 calc R . .
C7 C -0.3180(3) 0.9933(2) 0.20446(13) 0.0540(7) Uani 1 1 d . . .
H8 H -0.3445 1.0189 0.2429 0.065 Uiso 1 1 calc R . .
C18 C 0.3824(3) 0.73464(19) 0.09464(12) 0.0478(6) Uani 1 1 d . . .
H18A H 0.3178 0.6734 0.0753 0.057 Uiso 1 1 calc R . .
H18B H 0.4470 0.7647 0.0625 0.057 Uiso 1 1 calc R . .
C29 C 1.0448(3) 0.14529(18) 0.12699(15) 0.0523(7) Uani 1 1 d . . .
C2 C -0.0501(3) 0.78022(18) 0.10596(13) 0.0460(6) Uani 1 1 d . . .
H2A H 0.0082 0.8326 0.0820 0.055 Uiso 1 1 calc R . .
H2B H -0.1324 0.7441 0.0767 0.055 Uiso 1 1 calc R . .
C28 C 0.9576(3) 0.18212(19) 0.08099(15) 0.0555(7) Uani 1 1 d . . .
H28 H 0.9409 0.1552 0.0381 0.067 Uiso 1 1 calc R . .
C31 C 1.0008(3) 0.2587(2) 0.20982(15) 0.0582(7) Uani 1 1 d . . .
H31 H 1.0133 0.2829 0.2532 0.070 Uiso 1 1 calc R . .
C30 C 1.0666(3) 0.1822(2) 0.19093(16) 0.0621(8) Uani 1 1 d . . .
H30 H 1.1249 0.1563 0.2215 0.075 Uiso 1 1 calc R . .
C8 C -0.2336(3) 0.9248(2) 0.20776(13) 0.0563(7) Uani 1 1 d . . .
H9 H -0.2050 0.9030 0.2483 0.068 Uiso 1 1 calc R . .
C39 C 0.5724(3) 0.5935(2) 0.40164(13) 0.0556(7) Uani 1 1 d . . .
C33 C 0.1857(3) 0.82603(19) 0.22317(12) 0.0505(6) Uani 1 1 d . . .
H33A H 0.0932 0.8057 0.2420 0.061 Uiso 1 1 calc R . .
H33B H 0.1969 0.8948 0.2101 0.061 Uiso 1 1 calc R . .
C38 C 0.4551(3) 0.5348(2) 0.36464(13) 0.0540(6) Uani 1 1 d . . .
H38 H 0.4391 0.4652 0.3651 0.065 Uiso 1 1 calc R . .
C36 C 0.3827(3) 0.6795(2) 0.32601(12) 0.0505(6) Uani 1 1 d . . .
C37 C 0.3603(3) 0.5776(2) 0.32657(13) 0.0527(6) Uani 1 1 d . . .
H37 H 0.2813 0.5370 0.3014 0.063 Uiso 1 1 calc R . .
C42 C 0.8150(3) 0.5017(2) 0.53142(13) 0.0558(7) Uani 1 1 d . . .
C41 C 0.7407(3) 0.5749(2) 0.49774(15) 0.0614(7) Uani 1 1 d . . .
C34 C 0.3094(3) 0.8190(2) 0.27324(14) 0.0591(7) Uani 1 1 d . . .
H34A H 0.4029 0.8397 0.2553 0.071 Uiso 1 1 calc R . .
H34B H 0.3097 0.8606 0.3123 0.071 Uiso 1 1 calc R . .
C45 C 0.9550(3) 0.3750(3) 0.60071(15) 0.0645(8) Uani 1 1 d . . .
C40 C 0.5947(3) 0.6967(2) 0.40136(15) 0.0630(7) Uani 1 1 d . . .
H40 H 0.6733 0.7373 0.4269 0.076 Uiso 1 1 calc R . .
C35 C 0.5000(3) 0.7396(2) 0.36296(15) 0.0605(7) Uani 1 1 d . . .
H35 H 0.5157 0.8091 0.3622 0.073 Uiso 1 1 calc R . .
C44 C 0.8469(4) 0.3356(3) 0.55032(15) 0.0704(8) Uani 1 1 d . . .
H44 H 0.8213 0.2669 0.5399 0.085 Uiso 1 1 calc R . .
C43 C 0.7783(3) 0.4002(3) 0.51617(14) 0.0676(8) Uani 1 1 d . . .
H43 H 0.7064 0.3745 0.4824 0.081 Uiso 1 1 calc R . .
C47 C 0.9229(3) 0.5395(2) 0.58180(15) 0.0659(8) Uani 1 1 d . . .
H47 H 0.9488 0.6082 0.5922 0.079 Uiso 1 1 calc R . .
C46 C 0.9917(3) 0.4762(3) 0.61635(16) 0.0718(9) Uani 1 1 d . . .
H46 H 1.0631 0.5021 0.6503 0.086 Uiso 1 1 calc R . .
O2 O -0.4439(2) 1.15072(14) 0.04124(9) 0.0579(5) Uani 1 1 d . . .
O1 O -0.10045(19) 0.82324(13) 0.16093(9) 0.0542(5) Uani 1 1 d . . .
O4 O 0.8124(2) 0.38287(15) 0.24307(9) 0.0630(5) Uani 1 1 d . . .
O5 O 0.27967(19) 0.71499(14) 0.28748(9) 0.0556(5) Uani 1 1 d . . .
O6 O 0.7475(3) 0.6582(2) 0.52309(12) 0.0957(8) Uani 1 1 d . . .
O3 O 0.46404(16) 0.71437(12) 0.15238(8) 0.0454(4) Uani 1 1 d . . .
C48 C 1.0251(3) 0.3071(3) 0.63645(17) 0.0770(9) Uani 1 1 d . . .
N7 N 1.0779(3) 0.2517(3) 0.66495(16) 0.1010(11) Uani 1 1 d . . .
C32 C 1.1134(3) 0.0671(2) 0.10556(17) 0.0655(8) Uani 1 1 d . . .
N6 N 1.1688(3) 0.00725(18) 0.08697(18) 0.0891(10) Uani 1 1 d . . .
C16 C -0.7541(2) 1.47531(18) 0.15960(13) 0.0449(6) Uani 1 1 d . . .
N5 N -0.8080(2) 1.53811(16) 0.17174(12) 0.0570(6) Uani 1 1 d . . .
H1N H 0.218(2) 0.7087(16) 0.1788(10) 0.026(5) Uiso 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
N1 C1 1.506(3) . ?
N1 C17 1.511(3) . ?
N1 C33 1.513(3) . ?
N2 C9 1.354(3) . ?
N2 C6 1.421(2) . ?
N3 C25 1.340(3) . ?
N3 C24 1.422(2) . ?
N4 C41 1.344(4) . ?
N4 C39 1.426(3) . ?
C10 C15 1.381(3) . ?
C10 C11 1.390(3) . ?
C10 C9 1.509(3) . ?
C4 C3 1.382(3) . ?
C4 C5 1.394(3) . ?
C21 C24 1.375(3) . ?
C21 C20 1.402(3) . ?
C9 O2 1.222(3) . ?
C20 C19 1.373(3) . ?
C24 C23 1.397(3) . ?
C12 C11 1.382(3) . ?
C12 C13 1.389(3) . ?
C26 C31 1.384(3) . ?
C26 C27 1.389(4) . ?
C26 C25 1.500(3) . ?
C25 O4 1.235(3) . ?
C6 C5 1.387(3) . ?
C6 C7 1.400(3) . ?
C19 O3 1.376(2) . ?
C19 C22 1.391(3) . ?
C3 O1 1.363(2) . ?
C3 C8 1.390(3) . ?
C13 C14 1.378(3) . ?
C13 C16 1.450(3) . ?
C17 C18 1.506(3) . ?
C15 C14 1.380(3) . ?
C1 C2 1.498(3) . ?
C22 C23 1.382(3) . ?
C27 C28 1.380(3) . ?
C7 C8 1.364(3) . ?
C18 O3 1.427(3) . ?
C29 C30 1.373(4) . ?
C29 C28 1.382(4) . ?
C29 C32 1.449(3) . ?
C2 O1 1.423(3) . ?
C31 C30 1.397(4) . ?
C39 C38 1.368(4) . ?
C39 C40 1.379(4) . ?
C33 C34 1.513(3) . ?
C38 C37 1.381(3) . ?
C36 C37 1.363(4) . ?
C36 C35 1.374(4) . ?
C36 O5 1.386(3) . ?
C42 C43 1.375(4) . ?
C42 C47 1.389(4) . ?
C42 C41 1.502(4) . ?
C41 O6 1.226(4) . ?
C34 O5 1.430(3) . ?
C45 C46 1.371(5) . ?
C45 C44 1.395(4) . ?
C45 C48 1.443(4) . ?
C40 C35 1.385(4) . ?
C44 C43 1.383(4) . ?
C47 C46 1.375(4) . ?
C48 N7 1.146(4) . ?
C32 N6 1.143(3) . ?
C16 N5 1.128(3) . ?

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
C1 N1 C17 113.56(19) . . ?
C1 N1 C33 114.15(17) . . ?
C17 N1 C33 112.31(19) . . ?
C9 N2 C6 127.6(2) . . ?
C25 N3 C24 127.36(19) . . ?
C41 N4 C39 127.4(3) . . ?
C15 C10 C11 119.4(2) . . ?
C15 C10 C9 123.3(2) . . ?
C11 C10 C9 117.2(2) . . ?
C3 C4 C5 120.3(2) . . ?
C24 C21 C20 120.4(2) . . ?
O2 C9 N2 123.7(2) . . ?
O2 C9 C10 121.0(2) . . ?
N2 C9 C10 115.3(2) . . ?
C19 C20 C21 119.5(2) . . ?
C21 C24 C23 119.71(19) . . ?
C21 C24 N3 117.3(2) . . ?
C23 C24 N3 123.0(2) . . ?
C11 C12 C13 118.7(2) . . ?
C31 C26 C27 119.5(2) . . ?
C31 C26 C25 118.3(2) . . ?
C27 C26 C25 122.2(2) . . ?
O4 C25 N3 123.8(2) . . ?
O4 C25 C26 120.5(2) . . ?
N3 C25 C26 115.6(2) . . ?
C5 C6 C7 118.84(19) . . ?
C5 C6 N2 124.5(2) . . ?
C7 C6 N2 116.6(2) . . ?
C20 C19 O3 124.5(2) . . ?
C20 C19 C22 120.41(19) . . ?
O3 C19 C22 115.1(2) . . ?
O1 C3 C4 125.7(2) . . ?
O1 C3 C8 114.8(2) . . ?
C4 C3 C8 119.48(19) . . ?
C14 C13 C12 120.8(2) . . ?
C14 C13 C16 119.2(2) . . ?
C12 C13 C16 119.9(2) . . ?
C18 C17 N1 110.93(18) . . ?
C12 C11 C10 120.9(2) . . ?
C10 C15 C14 120.3(2) . . ?
C13 C14 C15 119.9(2) . . ?
C6 C5 C4 120.1(2) . . ?
C2 C1 N1 116.16(18) . . ?
C23 C22 C19 120.0(2) . . ?
C22 C23 C24 120.0(2) . . ?
C28 C27 C26 120.8(2) . . ?
C8 C7 C6 120.8(2) . . ?
O3 C18 C17 104.7(2) . . ?
C30 C29 C28 121.0(2) . . ?
C30 C29 C32 121.0(3) . . ?
C28 C29 C32 118.0(3) . . ?
O1 C2 C1 108.1(2) . . ?
C27 C28 C29 119.2(3) . . ?
C26 C31 C30 119.8(3) . . ?
C29 C30 C31 119.6(2) . . ?
C7 C8 C3 120.4(2) . . ?
C38 C39 C40 119.4(2) . . ?
C38 C39 N4 117.5(3) . . ?
C40 C39 N4 123.1(3) . . ?
N1 C33 C34 108.59(18) . . ?
C39 C38 C37 120.8(3) . . ?
C37 C36 C35 120.1(2) . . ?
C37 C36 O5 115.4(2) . . ?
C35 C36 O5 124.5(2) . . ?
C36 C37 C38 119.9(3) . . ?
C43 C42 C47 119.1(3) . . ?
C43 C42 C41 123.3(3) . . ?
C47 C42 C41 117.5(3) . . ?
O6 C41 N4 122.4(3) . . ?
O6 C41 C42 121.0(3) . . ?
N4 C41 C42 116.6(3) . . ?
O5 C34 C33 103.9(2) . . ?
C46 C45 C44 120.4(3) . . ?
C46 C45 C48 121.0(3) . . ?
C44 C45 C48 118.6(3) . . ?
C39 C40 C35 119.8(3) . . ?
C36 C35 C40 120.1(3) . . ?
C43 C44 C45 118.9(3) . . ?
C42 C43 C44 121.0(3) . . ?
C46 C47 C42 120.6(3) . . ?
C45 C46 C47 119.9(3) . . ?
C3 O1 C2 119.34(18) . . ?
C36 O5 C34 119.1(2) . . ?
C19 O3 C18 117.37(17) . . ?
N7 C48 C45 178.5(4) . . ?
N6 C32 C29 177.8(3) . . ?
N5 C16 C13 179.5(3) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        28.65
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.435
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.062

# start Validation Reply Form
_vrf_PLAT094_2LH-Br              
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       4.46 Report
RESPONSE: A consequence of the poor crystal quality.
;
####################################################################### 
# 
# 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_2LH-NO3-H20
_database_code_depnum_ccdc_archive 'CCDC 1041363'
_audit_update_record             
;
2015-04-10 deposited with the CCDC.
2015-04-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H40 N7 O6, N O3, H2O'
_chemical_formula_sum            'C48 H42 N8 O10'
_chemical_formula_weight         890.88

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'I 2/c'

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

_cell_length_a                   16.7671(5)
_cell_length_b                   18.6175(5)
_cell_length_c                   28.0023(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.197(3)
_cell_angle_gamma                90.00
_cell_volume                     8543.9(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    6315
_cell_measurement_theta_min      2.75
_cell_measurement_theta_max      30.45

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3712.0
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.986
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18465
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.95
_diffrn_reflns_theta_max         28.67
_reflns_number_total             10907
_reflns_number_gt                5935
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.2000P)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         9711
_refine_ls_number_parameters     596
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1103
_refine_ls_R_factor_gt           0.0711
_refine_ls_wR_factor_ref         0.3150
_refine_ls_wR_factor_gt          0.2733
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.002

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
O1 O 0.38771(13) 0.76726(11) 0.64871(8) 0.0620(6) Uani 1 1 d . . .
O8 O 0.56064(15) 0.36460(12) 0.60501(9) 0.0740(7) Uani 1 1 d . . .
O5 O 0.30172(15) 1.35172(13) 0.47276(9) 0.0762(7) Uani 1 1 d . . .
O2 O 0.43667(14) 1.02820(11) 0.53768(9) 0.0675(6) Uani 1 1 d . . .
O11 O 0.56820(15) 0.80703(12) 0.61660(9) 0.0710(6) Uani 1 1 d . . .
O7 O 0.66239(15) 0.42954(14) 0.63970(9) 0.0792(7) Uani 1 1 d . . .
O3 O 0.82045(17) 0.60196(14) 0.74863(12) 0.1008(10) Uani 1 1 d . . .
N8 N 0.58898(17) 0.41372(14) 0.63410(10) 0.0613(7) Uani 1 1 d . . .
N3 N 0.41820(15) 1.32735(13) 0.52831(9) 0.0551(6) Uani 1 1 d . . .
H3N H 0.4590 1.3475 0.5473 0.066 Uiso 1 1 calc R . .
N1 N 0.42595(15) 0.88406(13) 0.58613(10) 0.0592(7) Uani 1 1 d . . .
H1N H 0.4379 0.8367 0.5836 0.071 Uiso 1 1 calc R . .
O4 O 0.21544(18) 0.45111(16) 0.60299(12) 0.1009(10) Uani 1 1 d . . .
N4 N 0.70039(16) 0.55585(14) 0.70802(10) 0.0622(7) Uani 1 1 d . . .
H4N H 0.6717 0.5174 0.7019 0.075 Uiso 1 1 calc R . .
N2 N 0.33594(17) 0.47238(14) 0.65613(10) 0.0622(7) Uani 1 1 d . . .
H2N H 0.3741 0.4509 0.6765 0.075 Uiso 1 1 calc R . .
O6 O 0.54466(18) 0.44728(15) 0.65699(10) 0.0840(8) Uani 1 1 d . . .
O9 O 0.5000 0.5742(3) 0.2500 0.147(2) Uani 1 2 d S . .
C42 C 0.37798(17) 1.45095(16) 0.50985(10) 0.0514(7) Uani 1 1 d . . .
C38 C 0.41817(18) 1.25083(15) 0.52855(10) 0.0510(7) Uani 1 1 d . . .
N6 N 0.4047(2) 1.73694(17) 0.53405(13) 0.0821(9) Uani 1 1 d . . .
C6 C 0.66559(17) 0.62125(16) 0.68703(11) 0.0543(7) Uani 1 1 d . . .
C35 C 0.42581(19) 1.10128(16) 0.53365(12) 0.0563(7) Uani 1 1 d . . .
C10 C 0.8041(2) 0.47613(17) 0.75185(11) 0.0578(8) Uani 1 1 d . . .
C19 C 0.36709(19) 0.69586(16) 0.65101(11) 0.0549(7) Uani 1 1 d . . .
C45 C 0.39366(19) 1.59946(17) 0.52103(11) 0.0556(7) Uani 1 1 d . . .
C3 C 0.60019(19) 0.74704(17) 0.64275(13) 0.0594(8) Uani 1 1 d . . .
C41 C 0.36221(19) 1.37246(17) 0.50197(11) 0.0543(7) Uani 1 1 d . . .
C37 C 0.48753(19) 1.21656(17) 0.55369(12) 0.0592(8) Uani 1 1 d . . .
H37 H 0.5320 1.2439 0.5690 0.071 Uiso 1 1 calc R . .
C43 C 0.42092(19) 1.48053(17) 0.55346(11) 0.0571(7) Uani 1 1 d . . .
H43 H 0.4444 1.4504 0.5791 0.069 Uiso 1 1 calc R . .
C21 C 0.4137(2) 0.57945(17) 0.68121(11) 0.0592(8) Uani 1 1 d . . .
H21 H 0.4537 0.5506 0.7000 0.071 Uiso 1 1 calc R . .
C34 C 0.3650(2) 0.98467(17) 0.52797(13) 0.0631(8) Uani 1 1 d . . .
H34B H 0.3354 0.9924 0.4947 0.076 Uiso 1 1 calc R . .
H34A H 0.3297 0.9977 0.5499 0.076 Uiso 1 1 calc R . .
C20 C 0.42642(19) 0.65189(17) 0.67906(11) 0.0572(7) Uani 1 1 d . . .
H20 H 0.4748 0.6719 0.6964 0.069 Uiso 1 1 calc R . .
C5 C 0.6704(2) 0.68448(17) 0.71357(12) 0.0609(8) Uani 1 1 d . . .
H5 H 0.6951 0.6844 0.7466 0.073 Uiso 1 1 calc R . .
C7 C 0.62629(18) 0.62149(17) 0.63830(12) 0.0598(8) Uani 1 1 d . . .
H7 H 0.6218 0.5790 0.6204 0.072 Uiso 1 1 calc R . .
C26 C 0.29738(19) 0.34962(17) 0.63212(11) 0.0583(7) Uani 1 1 d . . .
C4 C 0.63889(19) 0.74743(17) 0.69150(13) 0.0631(8) Uani 1 1 d . . .
H4 H 0.6436 0.7900 0.7093 0.076 Uiso 1 1 calc R . .
C22 C 0.34114(19) 0.54813(17) 0.65542(11) 0.0566(7) Uani 1 1 d . . .
C9 C 0.7753(2) 0.55031(17) 0.73682(12) 0.0622(8) Uani 1 1 d . . .
C39 C 0.3519(2) 1.20958(18) 0.50628(12) 0.0659(9) Uani 1 1 d . . .
H39 H 0.3043 1.2317 0.4898 0.079 Uiso 1 1 calc R . .
C36 C 0.49220(19) 1.14290(17) 0.55653(12) 0.0601(8) Uani 1 1 d . . .
H36 H 0.5394 1.1209 0.5736 0.072 Uiso 1 1 calc R . .
N5 N 0.3573(3) 0.06657(18) 0.64046(14) 0.0923(11) Uani 1 1 d . . .
C24 C 0.29383(19) 0.66570(18) 0.62699(13) 0.0633(8) Uani 1 1 d . . .
H24 H 0.2531 0.6950 0.6093 0.076 Uiso 1 1 calc R . .
C40 C 0.3566(2) 1.13522(18) 0.50863(13) 0.0680(9) Uani 1 1 d . . .
H40 H 0.3123 1.1079 0.4930 0.082 Uiso 1 1 calc R . .
C17 C 0.3673(2) 0.88628(17) 0.62041(13) 0.0690(9) Uani 1 1 d . . .
H17A H 0.3967 0.9000 0.6528 0.083 Uiso 1 1 calc R . .
H17B H 0.3259 0.9224 0.6092 0.083 Uiso 1 1 calc R . .
C15 C 0.7517(2) 0.41772(19) 0.74895(11) 0.0619(8) Uani 1 1 d . . .
H15 H 0.6957 0.4244 0.7390 0.074 Uiso 1 1 calc R . .
C48 C 0.3999(2) 1.67605(18) 0.52794(13) 0.0638(8) Uani 1 1 d . . .
C29 C 0.3232(2) 0.20254(18) 0.63599(12) 0.0623(8) Uani 1 1 d . . .
C2 C 0.5583(2) 0.87011(19) 0.64377(15) 0.0779(11) Uani 1 1 d . . .
H2A H 0.6107 0.8919 0.6574 0.093 Uiso 1 1 calc R . .
H2B H 0.5310 0.8589 0.6701 0.093 Uiso 1 1 calc R . .
C47 C 0.3441(2) 1.49755(18) 0.47162(11) 0.0629(8) Uani 1 1 d . . .
H47 H 0.3158 1.4786 0.4422 0.076 Uiso 1 1 calc R . .
C44 C 0.4291(2) 1.55388(17) 0.55915(12) 0.0609(8) Uani 1 1 d . . .
H44 H 0.4582 1.5729 0.5884 0.073 Uiso 1 1 calc R . .
C8 C 0.59380(19) 0.68402(19) 0.61607(12) 0.0618(8) Uani 1 1 d . . .
H8 H 0.5677 0.6839 0.5833 0.074 Uiso 1 1 calc R . .
C33 C 0.3890(2) 0.90739(17) 0.53513(12) 0.0642(8) Uani 1 1 d . . .
H33A H 0.4276 0.8968 0.5147 0.077 Uiso 1 1 calc R . .
H33B H 0.3408 0.8783 0.5233 0.077 Uiso 1 1 calc R . .
C18 C 0.3267(2) 0.81480(18) 0.62327(13) 0.0637(8) Uani 1 1 d . . .
H18B H 0.2827 0.8195 0.6406 0.076 Uiso 1 1 calc R . .
H18A H 0.3043 0.7966 0.5907 0.076 Uiso 1 1 calc R . .
C23 C 0.28089(19) 0.59248(19) 0.62909(14) 0.0672(9) Uani 1 1 d . . .
H23 H 0.2316 0.5728 0.6128 0.081 Uiso 1 1 calc R . .
C46 C 0.3518(2) 1.57028(19) 0.47682(12) 0.0644(8) Uani 1 1 d . . .
H46 H 0.3293 1.6004 0.4510 0.077 Uiso 1 1 calc R . .
C27 C 0.3755(2) 0.32262(18) 0.64612(13) 0.0642(8) Uani 1 1 d . . .
H27 H 0.4195 0.3539 0.6543 0.077 Uiso 1 1 calc R . .
C13 C 0.8657(2) 0.3398(2) 0.77641(13) 0.0667(9) Uani 1 1 d . . .
C14 C 0.7824(2) 0.3504(2) 0.76070(12) 0.0675(9) Uani 1 1 d . . .
H14 H 0.7471 0.3114 0.7581 0.081 Uiso 1 1 calc R . .
C25 C 0.2786(2) 0.4290(2) 0.62888(13) 0.0678(9) Uani 1 1 d . . .
N7 N 0.9197(2) 0.2094(2) 0.78876(17) 0.1069(13) Uani 1 1 d . . .
C28 C 0.3886(2) 0.24966(19) 0.64802(13) 0.0673(9) Uani 1 1 d . . .
H28 H 0.4414 0.2318 0.6574 0.081 Uiso 1 1 calc R . .
C32 C 0.3400(2) 0.1257(2) 0.63809(13) 0.0694(9) Uani 1 1 d . . .
C11 C 0.8865(2) 0.4655(2) 0.76966(14) 0.0764(10) Uani 1 1 d . . .
H11 H 0.9219 0.5045 0.7733 0.092 Uiso 1 1 calc R . .
C1 C 0.5065(2) 0.91956(19) 0.60682(15) 0.0751(10) Uani 1 1 d . . .
H1B H 0.4975 0.9645 0.6224 0.090 Uiso 1 1 calc R . .
H1A H 0.5346 0.9301 0.5807 0.090 Uiso 1 1 calc R . .
C30 C 0.2451(2) 0.2290(2) 0.62198(14) 0.0730(9) Uani 1 1 d . . .
H30 H 0.2010 0.1978 0.6142 0.088 Uiso 1 1 calc R . .
C31 C 0.2329(2) 0.3019(2) 0.61949(15) 0.0755(10) Uani 1 1 d . . .
H31 H 0.1802 0.3197 0.6091 0.091 Uiso 1 1 calc R . .
C12 C 0.9172(2) 0.3976(2) 0.78221(14) 0.0771(10) Uani 1 1 d . . .
H12 H 0.9728 0.3912 0.7946 0.093 Uiso 1 1 calc R . .
C16 C 0.8962(2) 0.2675(2) 0.78458(15) 0.0812(11) Uani 1 1 d . . .
O9A O 0.5000 0.8719(11) 0.7500 0.370(9) Uani 1 2 d S . .


_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
O1 C19 1.378(4) . ?
O1 C18 1.425(4) . ?
O8 N8 1.250(3) . ?
O5 C41 1.223(4) . ?
O2 C35 1.374(4) . ?
O2 C34 1.427(4) . ?
O11 C3 1.380(4) . ?
O11 C2 1.428(4) . ?
O7 N8 1.243(4) . ?
O3 C9 1.225(4) . ?
N8 O6 1.247(4) . ?
N3 C41 1.356(4) . ?
N3 C38 1.425(4) . ?
N1 C33 1.496(4) . ?
N1 C1 1.506(4) . ?
N1 C17 1.513(4) . ?
O4 C25 1.221(4) . ?
N4 C9 1.346(4) . ?
N4 C6 1.423(4) . ?
N2 C25 1.360(4) . ?
N2 C22 1.413(4) . ?
C42 C43 1.393(4) . ?
C42 C47 1.402(4) . ?
C42 C41 1.493(4) . ?
C38 C37 1.382(4) . ?
C38 C39 1.386(4) . ?
N6 C48 1.147(4) . ?
C6 C7 1.384(4) . ?
C6 C5 1.385(4) . ?
C35 C40 1.376(5) . ?
C35 C36 1.396(4) . ?
C10 C11 1.381(5) . ?
C10 C15 1.390(5) . ?
C10 C9 1.494(5) . ?
C19 C24 1.388(5) . ?
C19 C20 1.395(4) . ?
C45 C44 1.395(4) . ?
C45 C46 1.397(5) . ?
C45 C48 1.440(4) . ?
C3 C8 1.383(5) . ?
C3 C4 1.382(5) . ?
C37 C36 1.375(4) . ?
C43 C44 1.378(4) . ?
C21 C20 1.369(4) . ?
C21 C22 1.404(4) . ?
C34 C33 1.496(5) . ?
C5 C4 1.377(4) . ?
C7 C8 1.377(4) . ?
C26 C27 1.380(5) . ?
C26 C31 1.387(5) . ?
C26 C25 1.510(5) . ?
C22 C23 1.390(4) . ?
C39 C40 1.387(5) . ?
N5 C32 1.137(5) . ?
C24 C23 1.384(5) . ?
C17 C18 1.504(5) . ?
C15 C14 1.369(5) . ?
C29 C30 1.375(5) . ?
C29 C28 1.389(5) . ?
C29 C32 1.457(5) . ?
C2 C1 1.514(5) . ?
C47 C46 1.365(5) . ?
C27 C28 1.375(5) . ?
C13 C12 1.368(5) . ?
C13 C14 1.386(5) . ?
C13 C16 1.441(5) . ?
N7 C16 1.149(5) . ?
C11 C12 1.382(5) . ?
C30 C31 1.372(5) . ?

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
C19 O1 C18 117.5(3) . . ?
C35 O2 C34 117.1(3) . . ?
C3 O11 C2 117.3(3) . . ?
O7 N8 O6 119.9(3) . . ?
O7 N8 O8 119.1(3) . . ?
O6 N8 O8 121.0(3) . . ?
C41 N3 C38 128.4(2) . . ?
C33 N1 C1 113.4(3) . . ?
C33 N1 C17 113.8(3) . . ?
C1 N1 C17 113.2(3) . . ?
C9 N4 C6 124.2(3) . . ?
C25 N2 C22 128.5(3) . . ?
C43 C42 C47 118.4(3) . . ?
C43 C42 C41 124.0(3) . . ?
C47 C42 C41 117.5(3) . . ?
C37 C38 C39 118.8(3) . . ?
C37 C38 N3 117.6(3) . . ?
C39 C38 N3 123.6(3) . . ?
C7 C6 C5 119.2(3) . . ?
C7 C6 N4 118.6(3) . . ?
C5 C6 N4 122.2(3) . . ?
O2 C35 C40 125.4(3) . . ?
O2 C35 C36 115.7(3) . . ?
C40 C35 C36 118.9(3) . . ?
C11 C10 C15 118.7(3) . . ?
C11 C10 C9 118.3(3) . . ?
C15 C10 C9 123.0(3) . . ?
O1 C19 C24 124.9(3) . . ?
O1 C19 C20 115.9(3) . . ?
C24 C19 C20 119.2(3) . . ?
C44 C45 C46 119.6(3) . . ?
C44 C45 C48 119.5(3) . . ?
C46 C45 C48 120.8(3) . . ?
O11 C3 C8 115.0(3) . . ?
O11 C3 C4 124.6(3) . . ?
C8 C3 C4 120.3(3) . . ?
O5 C41 N3 123.3(3) . . ?
O5 C41 C42 120.2(3) . . ?
N3 C41 C42 116.4(3) . . ?
C36 C37 C38 121.4(3) . . ?
C44 C43 C42 120.9(3) . . ?
C20 C21 C22 120.8(3) . . ?
O2 C34 C33 109.2(3) . . ?
C21 C20 C19 120.3(3) . . ?
C4 C5 C6 120.6(3) . . ?
C8 C7 C6 120.6(3) . . ?
C27 C26 C31 118.8(3) . . ?
C27 C26 C25 123.2(3) . . ?
C31 C26 C25 118.0(3) . . ?
C5 C4 C3 119.6(3) . . ?
C23 C22 C21 118.7(3) . . ?
C23 C22 N2 124.1(3) . . ?
C21 C22 N2 117.2(3) . . ?
O3 C9 N4 123.1(3) . . ?
O3 C9 C10 120.4(3) . . ?
N4 C9 C10 116.4(3) . . ?
C38 C39 C40 120.0(3) . . ?
C37 C36 C35 119.8(3) . . ?
C23 C24 C19 120.6(3) . . ?
C35 C40 C39 121.1(3) . . ?
C18 C17 N1 111.8(3) . . ?
C14 C15 C10 120.1(3) . . ?
N6 C48 C45 179.1(4) . . ?
C30 C29 C28 119.8(3) . . ?
C30 C29 C32 121.9(3) . . ?
C28 C29 C32 118.3(3) . . ?
O11 C2 C1 104.5(3) . . ?
C46 C47 C42 121.2(3) . . ?
C43 C44 C45 119.9(3) . . ?
C7 C8 C3 119.7(3) . . ?
C34 C33 N1 116.9(3) . . ?
O1 C18 C17 106.9(3) . . ?
C24 C23 C22 120.3(3) . . ?
C47 C46 C45 119.9(3) . . ?
C28 C27 C26 120.3(3) . . ?
C12 C13 C14 119.6(3) . . ?
C12 C13 C16 121.4(3) . . ?
C14 C13 C16 118.9(3) . . ?
C15 C14 C13 120.6(3) . . ?
O4 C25 N2 123.7(3) . . ?
O4 C25 C26 120.6(3) . . ?
N2 C25 C26 115.7(3) . . ?
C27 C28 C29 120.2(3) . . ?
N5 C32 C29 176.6(5) . . ?
C10 C11 C12 120.9(4) . . ?
N1 C1 C2 109.5(3) . . ?
C31 C30 C29 119.5(3) . . ?
C30 C31 C26 121.3(3) . . ?
C13 C12 C11 119.8(3) . . ?
N7 C16 C13 176.8(5) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        28.67
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.053

# start Validation Reply Form
_vrf_PLAT306_2LH-NO3-H20         
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O9 Check 
RESPONSE: We can not locate hydrogen after increasing 
the Q peak numbers in XShell.
;
####################################################################### 
# 
# 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_2LH-ClO4
_database_code_depnum_ccdc_archive 'CCDC 1041364'
_audit_update_record             
;
2015-04-10 deposited with the CCDC.
2015-04-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H40 N7 O6, Cl O4'
_chemical_formula_sum            'C48 H40 Cl N7 O10'

_chemical_formula_weight         910.32

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/a'

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

_cell_length_a                   15.9320(10)
_cell_length_b                   18.5172(6)
_cell_length_c                   36.597(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.905(6)
_cell_angle_gamma                90.00
_cell_volume                     10666.6(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    15281
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      23.85

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.134
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3792.0
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.976
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            55649
_diffrn_reflns_av_R_equivalents  0.0751
_diffrn_reflns_av_unetI/netI     0.2176
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_theta_min         3.11
_diffrn_reflns_theta_max         28.70
_reflns_number_total             27403
_reflns_number_gt                15793
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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.
;
_PLAT606_ALERT_4_G               
;
Problem: VERY LARGE Solvent Accessible VOID(S) in Structure        
Response: In this case there exists certain  amount  of  DMF-water  
solvent  trapped  in  the  crystal  lattice  in  a  disordered  
manner These electron densities were moved during refinement and 
the count of electron removed in total was 226 per two symmetry 
independent molecules which account for five DMF and three water molecules.
;

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material


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 0.026 0.750 0.243 1216 226 ' '
2 0.083 0.250 0.757 1216 225 ' '


_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0480P)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         27403
_refine_ls_number_parameters     1189
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2866
_refine_ls_R_factor_gt           0.0977
_refine_ls_wR_factor_ref         0.2438
_refine_ls_wR_factor_gt          0.2061
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_restrained_S_all      0.987
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001

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
Cl1 Cl 0.42762(13) 0.36845(9) 0.37775(5) 0.0900(6) Uani 1 1 d . . .
Cl2 Cl 0.93254(16) 0.56663(9) 0.85852(5) 0.0978(6) Uani 1 1 d . . .
O13 O 0.5481(2) 0.29208(15) 0.95295(10) 0.0720(11) Uani 1 1 d . . .
O1 O 0.5577(2) 1.00131(17) 0.46799(10) 0.0696(11) Uani 1 1 d . . .
O5 O 0.6424(2) 0.74940(17) 0.38400(9) 0.0726(11) Uani 1 1 d . . .
O14 O 0.6614(3) -0.03453(17) 1.00817(12) 0.0953(15) Uani 1 1 d . . .
O11 O 0.6730(2) 0.56885(17) 0.89618(9) 0.0758(12) Uani 1 1 d . . .
N9 N 0.5559(3) -0.00921(18) 0.96114(10) 0.0565(12) Uani 1 1 d . . .
H9N H 0.5179 -0.0288 0.9449 0.068 Uiso 1 1 calc R . .
O2 O 0.6775(3) 1.32656(17) 0.52456(11) 0.0962(15) Uani 1 1 d . . .
O10 O 0.4374(3) 0.3517(2) 0.41574(10) 0.1054(14) Uani 1 1 d . . .
O3 O 0.4394(3) 0.7824(2) 0.39555(11) 0.0970(13) Uani 1 1 d . . .
O15 O 0.4710(3) 0.50431(19) 0.87403(10) 0.0833(12) Uani 1 1 d . . .
N8 N 0.6012(3) 0.44027(19) 0.92292(12) 0.0650(13) Uani 1 1 d . . .
H8N H 0.5802 0.4860 0.9221 0.078 Uiso 1 1 calc R . .
N110 N 0.5800(3) 0.8605(2) 0.43091(12) 0.0627(12) Uani 1 1 d . . .
H3A H 0.5679 0.8125 0.4306 0.075 Uiso 1 1 calc R . .
O12 O 0.8181(3) 0.88656(18) 0.94907(11) 0.0957(14) Uani 1 1 d . . .
O16 O 0.3637(3) 0.71489(19) 0.73261(10) 0.1078(16) Uani 1 1 d . . .
O20 O 0.9200(3) 0.5458(2) 0.89479(13) 0.1244(17) Uani 1 1 d . . .
N12 N 0.5494(3) -0.4204(2) 0.96053(13) 0.0899(17) Uani 1 1 d . . .
N10 N 0.7141(3) 0.8673(2) 0.90152(12) 0.0746(14) Uani 1 1 d . . .
H10N H 0.6794 0.8891 0.8847 0.090 Uiso 1 1 calc R . .
N4 N 0.7055(3) 0.4548(2) 0.37801(12) 0.0730(14) Uani 1 1 d . . .
H4N H 0.6804 0.4338 0.3583 0.088 Uiso 1 1 calc R . .
N2 N 0.5789(3) 1.3014(2) 0.47502(11) 0.0647(13) Uani 1 1 d . . .
H2N H 0.5444 1.3212 0.4575 0.078 Uiso 1 1 calc R . .
C49 C 0.5989(4) 0.4131(2) 0.96162(13) 0.0685(17) Uani 1 1 d . . .
H49A H 0.6389 0.4411 0.9786 0.082 Uiso 1 1 calc R . .
H49B H 0.5427 0.4223 0.9677 0.082 Uiso 1 1 calc R . .
N11 N 0.3996(3) 0.7544(2) 0.78984(12) 0.0718(13) Uani 1 1 d . . .
H11N H 0.4048 0.7929 0.8031 0.086 Uiso 1 1 calc R . .
N3 N 0.3741(3) 0.5391(3) 0.30776(15) 0.1005(18) Uani 1 1 d . . .
H3N H 0.3802 0.4996 0.3203 0.121 Uiso 1 1 calc R . .
C10 C 0.6150(3) 1.4266(2) 0.49067(14) 0.0521(14) Uani 1 1 d . . .
C58 C 0.5870(3) -0.1342(2) 0.97693(13) 0.0507(14) Uani 1 1 d . . .
O6 O 0.7948(3) 0.4363(2) 0.43112(13) 0.1115(16) Uani 1 1 d . . .
C6 C 0.5792(4) 1.2243(2) 0.47595(13) 0.0501(14) Uani 1 1 d . . .
C51 C 0.5554(4) 0.2187(2) 0.95649(14) 0.0550(15) Uani 1 1 d . . .
C56 C 0.6201(4) 0.1846(2) 0.97922(14) 0.0695(17) Uani 1 1 d . . .
H56 H 0.6628 0.2114 0.9933 0.083 Uiso 1 1 calc R . .
O4 O 0.3427(4) 0.5800(3) 0.24871(13) 0.147(2) Uani 1 1 d . . .
C86 C 0.4131(4) 0.6873(3) 0.80970(16) 0.0702(17) Uani 1 1 d . . .
C2 C 0.6293(4) 0.9566(3) 0.47874(14) 0.0715(17) Uani 1 1 d . . .
H2A H 0.6492 0.9628 0.5050 0.086 Uiso 1 1 calc R . .
H2B H 0.6747 0.9709 0.4654 0.086 Uiso 1 1 calc R . .
C61 C 0.5676(4) -0.2834(2) 0.96858(14) 0.0628(16) Uani 1 1 d . . .
C1 C 0.6075(4) 0.8791(2) 0.47090(14) 0.0738(18) Uani 1 1 d . . .
H1A H 0.5623 0.8656 0.4846 0.089 Uiso 1 1 calc R . .
H1B H 0.6568 0.8499 0.4803 0.089 Uiso 1 1 calc R . .
C50 C 0.6188(4) 0.3343(2) 0.96841(13) 0.0688(17) Uani 1 1 d . . .
H50A H 0.6680 0.3211 0.9573 0.083 Uiso 1 1 calc R . .
H50B H 0.6319 0.3252 0.9948 0.083 Uiso 1 1 calc R . .
C3 C 0.5673(4) 1.0760(3) 0.47274(14) 0.0585(15) Uani 1 1 d . . .
C67 C 0.6894(4) 0.6423(2) 0.89884(15) 0.0618(16) Uani 1 1 d . . .
C90 C 0.3741(4) 0.8399(3) 0.74100(15) 0.0671(17) Uani 1 1 d . . .
C52 C 0.4937(4) 0.1789(2) 0.93504(16) 0.0793(19) Uani 1 1 d . . .
H52 H 0.4516 0.2018 0.9187 0.095 Uiso 1 1 calc R . .
C36 C 0.6121(3) 0.6366(3) 0.35999(14) 0.0626(15) Uani 1 1 d . . .
H36 H 0.5649 0.6566 0.3454 0.075 Uiso 1 1 calc R . .
C5 C 0.6380(4) 1.1836(2) 0.49705(14) 0.0673(17) Uani 1 1 d . . .
H5 H 0.6819 1.2056 0.5129 0.081 Uiso 1 1 calc R . .
C81 C 0.5449(4) 0.3990(2) 0.89388(14) 0.0766(18) Uani 1 1 d . . .
H81B H 0.4950 0.3823 0.9036 0.092 Uiso 1 1 calc R . .
H81A H 0.5749 0.3571 0.8866 0.092 Uiso 1 1 calc R . .
C38 C 0.6991(4) 0.5320(3) 0.37981(15) 0.0615(15) Uani 1 1 d . . .
C8 C 0.5052(3) 1.1173(3) 0.45157(15) 0.0675(16) Uani 1 1 d . . .
H8 H 0.4598 1.0954 0.4366 0.081 Uiso 1 1 calc R . .
C69 C 0.6421(4) 0.7595(3) 0.87885(14) 0.0662(16) Uani 1 1 d . . .
H69 H 0.6029 0.7889 0.8643 0.079 Uiso 1 1 calc R . .
C53 C 0.4949(4) 0.1038(3) 0.93801(16) 0.0780(18) Uani 1 1 d . . .
H53 H 0.4519 0.0771 0.9241 0.094 Uiso 1 1 calc R . .
C57 C 0.6057(4) -0.0549(2) 0.98343(16) 0.0587(15) Uani 1 1 d . . .
C7 C 0.5122(3) 1.1919(3) 0.45320(14) 0.0592(15) Uani 1 1 d . . .
H7 H 0.4717 1.2204 0.4389 0.071 Uiso 1 1 calc R . .
C31 C 0.4093(5) 0.4006(4) 0.27610(19) 0.106(2) Uani 1 1 d . . .
H31 H 0.4465 0.4120 0.2975 0.127 Uiso 1 1 calc R . .
C9 C 0.6258(4) 1.3460(3) 0.49809(15) 0.0584(15) Uani 1 1 d . . .
O9 O 0.4955(3) 0.4148(3) 0.36880(13) 0.149(2) Uani 1 1 d . . .
C54 C 0.5585(4) 0.0679(2) 0.96123(14) 0.0566(15) Uani 1 1 d . . .
C15 C 0.5912(3) 1.4545(3) 0.45482(15) 0.0662(16) Uani 1 1 d . . .
H15 H 0.5796 1.4240 0.4345 0.079 Uiso 1 1 calc R . .
C55 C 0.6211(3) 0.1087(2) 0.98098(14) 0.0625(15) Uani 1 1 d . . .
H55 H 0.6656 0.0857 0.9960 0.075 Uiso 1 1 calc R . .
C35 C 0.6675(4) 0.6792(3) 0.38290(15) 0.0586(15) Uani 1 1 d . . .
C73 C 0.7669(4) 0.9107(3) 0.92462(16) 0.0672(17) Uani 1 1 d . . .
C68 C 0.6320(4) 0.6853(2) 0.87722(13) 0.0633(16) Uani 1 1 d . . .
H68 H 0.5867 0.6648 0.8616 0.076 Uiso 1 1 calc R . .
C39 C 0.7551(4) 0.5769(3) 0.40030(15) 0.0731(17) Uani 1 1 d . . .
H39 H 0.8055 0.5583 0.4130 0.088 Uiso 1 1 calc R . .
C85 C 0.3976(3) 0.6839(3) 0.84675(14) 0.0699(17) Uani 1 1 d . . .
H85 H 0.3743 0.7235 0.8572 0.084 Uiso 1 1 calc R . .
C66 C 0.7234(4) 0.5220(2) 0.92142(17) 0.088(2) Uani 1 1 d . . .
H66A H 0.7201 0.5361 0.9467 0.106 Uiso 1 1 calc R . .
H66B H 0.7824 0.5242 0.9177 0.106 Uiso 1 1 calc R . .
C59 C 0.5240(4) -0.1617(3) 0.95265(14) 0.0760(18) Uani 1 1 d . . .
H59 H 0.4867 -0.1305 0.9383 0.091 Uiso 1 1 calc R . .
C33 C 0.6522(4) 0.8684(3) 0.40781(15) 0.0789(18) Uani 1 1 d . . .
H33B H 0.6918 0.9051 0.4187 0.095 Uiso 1 1 calc R . .
H33A H 0.6289 0.8838 0.3830 0.095 Uiso 1 1 calc R . .
C13 C 0.6003(4) 1.5735(3) 0.47971(17) 0.0649(16) Uani 1 1 d . . .
C37 C 0.6281(4) 0.5624(3) 0.35895(15) 0.0722(17) Uani 1 1 d . . .
H37 H 0.5901 0.5329 0.3439 0.087 Uiso 1 1 calc R . .
C4 C 0.6329(4) 1.1085(3) 0.49501(14) 0.0645(16) Uani 1 1 d . . .
H4 H 0.6745 1.0804 0.5089 0.077 Uiso 1 1 calc R . .
C42 C 0.7283(4) 0.3343(3) 0.40191(17) 0.0657(16) Uani 1 1 d . . .
N5 N 0.5863(4) 1.7127(2) 0.46820(16) 0.111(2) Uani 1 1 d . . .
C74 C 0.7596(4) 0.9904(3) 0.91872(16) 0.0695(17) Uani 1 1 d . . .
C83 C 0.4519(3) 0.5632(3) 0.85188(15) 0.0633(15) Uani 1 1 d . . .
C17 C 0.5032(4) 0.8950(3) 0.41262(17) 0.088(2) Uani 1 1 d . . .
H17B H 0.5169 0.9425 0.4040 0.105 Uiso 1 1 calc R . .
H17A H 0.4638 0.9011 0.4301 0.105 Uiso 1 1 calc R . .
C11 C 0.6309(3) 1.4729(3) 0.51949(14) 0.0684(16) Uani 1 1 d . . .
H11 H 0.6469 1.4547 0.5432 0.082 Uiso 1 1 calc R . .
C70 C 0.7086(4) 0.7901(3) 0.90147(14) 0.0595(15) Uani 1 1 d . . .
C12 C 0.6239(4) 1.5468(3) 0.51432(17) 0.0745(18) Uani 1 1 d . . .
H12 H 0.6353 1.5779 0.5344 0.089 Uiso 1 1 calc R . .
C87 C 0.4475(3) 0.6285(3) 0.79327(15) 0.0739(17) Uani 1 1 d . . .
H87 H 0.4588 0.6307 0.7691 0.089 Uiso 1 1 calc R . .
C14 C 0.5856(3) 1.5272(3) 0.45071(16) 0.0649(16) Uani 1 1 d . . .
H14 H 0.5711 1.5460 0.4270 0.078 Uiso 1 1 calc R . .
C95 C 0.3188(4) 0.8573(3) 0.70935(15) 0.0747(17) Uani 1 1 d . . .
H95 H 0.2834 0.8223 0.6970 0.090 Uiso 1 1 calc R . .
C34 C 0.6993(3) 0.7965(3) 0.40603(16) 0.0770(18) Uani 1 1 d . . .
H34A H 0.7503 0.8034 0.3950 0.092 Uiso 1 1 calc R . .
H34B H 0.7153 0.7766 0.4307 0.092 Uiso 1 1 calc R . .
N13 N 0.7531(4) 1.2772(3) 0.90480(17) 0.139(3) Uani 1 1 d . . .
C65 C 0.6892(4) 0.4462(2) 0.91416(17) 0.0844(19) Uani 1 1 d . . .
H65A H 0.6892 0.4340 0.8884 0.101 Uiso 1 1 calc R . .
H65B H 0.7258 0.4122 0.9292 0.101 Uiso 1 1 calc R . .
C46 C 0.7576(5) 0.2155(4) 0.42814(19) 0.099(2) Uani 1 1 d . . .
H46 H 0.7886 0.1862 0.4459 0.118 Uiso 1 1 calc R . .
C64 C 0.5555(4) -0.3616(3) 0.96399(15) 0.0699(17) Uani 1 1 d . . .
C44 C 0.6545(4) 0.2301(3) 0.37384(19) 0.104(2) Uani 1 1 d . . .
H44 H 0.6160 0.2102 0.3548 0.125 Uiso 1 1 calc R . .
C62 C 0.6316(4) -0.2556(3) 0.99273(18) 0.090(2) Uani 1 1 d . . .
H62 H 0.6700 -0.2868 1.0066 0.108 Uiso 1 1 calc R . .
C16 C 0.5925(4) 1.6507(3) 0.47371(17) 0.0806(19) Uani 1 1 d . . .
C94 C 0.3168(4) 0.9282(4) 0.69611(16) 0.086(2) Uani 1 1 d . . .
H94 H 0.2771 0.9409 0.6758 0.103 Uiso 1 1 calc R . .
C84 C 0.4169(3) 0.6226(3) 0.86719(15) 0.0725(17) Uani 1 1 d . . .
H84 H 0.4064 0.6207 0.8915 0.087 Uiso 1 1 calc R . .
C40 C 0.7382(4) 0.6496(3) 0.40248(15) 0.0688(17) Uani 1 1 d . . .
H40 H 0.7761 0.6789 0.4177 0.083 Uiso 1 1 calc R . .
N14 N 0.3653(5) 1.1077(3) 0.68596(17) 0.177(3) Uani 1 1 d . . .
C23 C 0.3975(4) 0.5976(3) 0.36713(18) 0.0824(19) Uani 1 1 d . . .
H23 H 0.3967 0.5525 0.3782 0.099 Uiso 1 1 calc R . .
C29 C 0.3494(5) 0.3144(4) 0.2298(2) 0.104(2) Uani 1 1 d . . .
C19 C 0.4168(4) 0.7250(3) 0.3706(2) 0.086(2) Uani 1 1 d . . .
C63 C 0.6419(4) -0.1818(3) 0.99749(18) 0.101(2) Uani 1 1 d . . .
H63 H 0.6863 -0.1641 1.0147 0.121 Uiso 1 1 calc R . .
C72 C 0.7572(4) 0.6734(3) 0.92131(16) 0.0764(18) Uani 1 1 d . . .
H72 H 0.7963 0.6444 0.9361 0.092 Uiso 1 1 calc R . .
C27 C 0.3050(4) 0.4372(4) 0.22238(18) 0.099(2) Uani 1 1 d . . .
H27 H 0.2738 0.4731 0.2086 0.119 Uiso 1 1 calc R . .
C75 C 0.6909(4) 1.0238(3) 0.89705(16) 0.086(2) Uani 1 1 d . . .
H75 H 0.6462 0.9958 0.8853 0.103 Uiso 1 1 calc R . .
C89 C 0.3799(4) 0.7642(3) 0.75366(15) 0.0672(17) Uani 1 1 d . . .
C88 C 0.4644(4) 0.5650(3) 0.81513(16) 0.0821(19) Uani 1 1 d . . .
H88 H 0.4843 0.5239 0.8046 0.099 Uiso 1 1 calc R . .
C41 C 0.7472(4) 0.4129(3) 0.40437(17) 0.0715(18) Uani 1 1 d . . .
C79 C 0.8265(4) 1.0309(3) 0.93537(18) 0.091(2) Uani 1 1 d . . .
H79 H 0.8721 1.0086 0.9500 0.110 Uiso 1 1 calc R . .
C60 C 0.5128(4) -0.2361(3) 0.94830(15) 0.0783(18) Uani 1 1 d . . .
H60 H 0.4678 -0.2538 0.9315 0.094 Uiso 1 1 calc R . .
C71 C 0.7672(4) 0.7473(3) 0.92200(16) 0.0806(19) Uani 1 1 d . . .
H71 H 0.8142 0.7679 0.9365 0.097 Uiso 1 1 calc R . .
C76 C 0.6884(5) 1.0978(3) 0.89287(18) 0.104(2) Uani 1 1 d . . .
H76 H 0.6417 1.1206 0.8792 0.125 Uiso 1 1 calc R . .
C93 C 0.3726(5) 0.9793(3) 0.71268(18) 0.094(2) Uani 1 1 d . . .
C80 C 0.7563(5) 1.2166(3) 0.9055(2) 0.111(3) Uani 1 1 d . . .
N7 N 0.6723(5) 0.0471(3) 0.39952(19) 0.155(3) Uani 1 1 d . . .
C45 C 0.6983(5) 0.1858(3) 0.4013(2) 0.086(2) Uani 1 1 d . . .
C82 C 0.5179(4) 0.4477(3) 0.86025(15) 0.092(2) Uani 1 1 d . . .
H82A H 0.5671 0.4668 0.8509 0.111 Uiso 1 1 calc R . .
H82B H 0.4828 0.4215 0.8406 0.111 Uiso 1 1 calc R . .
C43 C 0.6692(4) 0.3049(3) 0.37526(18) 0.0860(19) Uani 1 1 d . . .
H43 H 0.6380 0.3348 0.3577 0.103 Uiso 1 1 calc R . .
C77 C 0.7579(5) 1.1371(3) 0.9097(2) 0.086(2) Uani 1 1 d . . .
C24 C 0.4132(4) 0.6578(3) 0.38836(18) 0.0838(19) Uani 1 1 d . . .
H24 H 0.4214 0.6547 0.4140 0.101 Uiso 1 1 calc R . .
C28 C 0.3008(4) 0.3671(4) 0.21000(18) 0.101(2) Uani 1 1 d . . .
H28 H 0.2653 0.3551 0.1882 0.122 Uiso 1 1 calc R . .
C91 C 0.4303(4) 0.8909(3) 0.75802(15) 0.089(2) Uani 1 1 d . . .
H91 H 0.4685 0.8793 0.7791 0.107 Uiso 1 1 calc R . .
C22 C 0.3830(4) 0.6036(3) 0.3296(2) 0.091(2) Uani 1 1 d . . .
C30 C 0.4040(4) 0.3318(4) 0.26319(18) 0.104(2) Uani 1 1 d . . .
H30 H 0.4363 0.2957 0.2763 0.125 Uiso 1 1 calc R . .
C18 C 0.4605(4) 0.8491(3) 0.37918(16) 0.089(2) Uani 1 1 d . . .
H18A H 0.4100 0.8729 0.3665 0.106 Uiso 1 1 calc R . .
H18B H 0.4995 0.8410 0.3617 0.106 Uiso 1 1 calc R . .
C25 C 0.3578(5) 0.5297(4) 0.2706(2) 0.110(3) Uani 1 1 d . . .
C78 C 0.8263(5) 1.1050(3) 0.93039(19) 0.097(2) Uani 1 1 d . . .
H78 H 0.8724 1.1327 0.9410 0.117 Uiso 1 1 calc R . .
C20 C 0.4013(5) 0.7325(4) 0.3342(2) 0.110(3) Uani 1 1 d . . .
H20 H 0.4028 0.7779 0.3234 0.132 Uiso 1 1 calc R . .
N6 N 0.3393(6) 0.1783(4) 0.20692(19) 0.160(3) Uani 1 1 d . . .
C48 C 0.6833(5) 0.1066(4) 0.40142(19) 0.114(3) Uani 1 1 d . . .
C92 C 0.4286(4) 0.9613(3) 0.74273(18) 0.105(2) Uani 1 1 d . . .
H92 H 0.4669 0.9958 0.7537 0.126 Uiso 1 1 calc R . .
C21 C 0.3833(4) 0.6722(4) 0.31285(18) 0.109(2) Uani 1 1 d . . .
H21 H 0.3711 0.6765 0.2873 0.131 Uiso 1 1 calc R . .
C47 C 0.7715(4) 0.2903(4) 0.42875(19) 0.095(2) Uani 1 1 d . . .
H47 H 0.8105 0.3104 0.4475 0.114 Uiso 1 1 calc R . .
O18 O 0.9072(4) 0.6356(3) 0.85102(15) 0.201(3) Uani 1 1 d . . .
C26 C 0.3582(4) 0.4549(4) 0.25682(18) 0.0847(19) Uani 1 1 d . . .
C96 C 0.3685(6) 1.0523(4) 0.69754(18) 0.127(3) Uani 1 1 d . . .
O7 O 0.4229(6) 0.3049(3) 0.35810(17) 0.269(4) Uani 1 1 d . . .
C32 C 0.3464(6) 0.2412(5) 0.2170(2) 0.124(3) Uani 1 1 d . . .
O8 O 0.3526(4) 0.4045(4) 0.36698(19) 0.231(4) Uani 1 1 d . . .
O17 O 1.0154(5) 0.5664(5) 0.8565(2) 0.288(5) Uani 1 1 d . . .
O19 O 0.8819(7) 0.5273(4) 0.83454(18) 0.330(6) 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
Cl1 O8 1.372(5) . ?
Cl1 O7 1.376(5) . ?
Cl1 O10 1.409(4) . ?
Cl1 O9 1.457(5) . ?
Cl2 O19 1.315(6) . ?
Cl2 O17 1.333(7) . ?
Cl2 O18 1.354(5) . ?
Cl2 O20 1.426(4) . ?
O13 C51 1.369(5) . ?
O13 C50 1.415(5) . ?
O1 C3 1.399(5) . ?
O1 C2 1.414(5) . ?
O5 C35 1.363(5) . ?
O5 C34 1.416(5) . ?
O14 C57 1.226(6) . ?
O11 C67 1.385(5) . ?
O11 C66 1.422(5) . ?
N9 C57 1.345(6) . ?
N9 C54 1.428(5) . ?
O2 C9 1.225(5) . ?
O3 C19 1.411(6) . ?
O3 C18 1.437(6) . ?
O15 C83 1.364(5) . ?
O15 C82 1.424(6) . ?
N8 C65 1.490(6) . ?
N8 C81 1.491(5) . ?
N8 C49 1.509(5) . ?
N110 C17 1.449(6) . ?
N110 C1 1.501(5) . ?
N110 C33 1.536(6) . ?
O12 C73 1.200(6) . ?
O16 C89 1.197(5) . ?
N12 C64 1.098(5) . ?
N10 C73 1.360(6) . ?
N10 C70 1.433(5) . ?
N4 C41 1.332(6) . ?
N4 C38 1.436(6) . ?
N2 C9 1.326(5) . ?
N2 C6 1.430(5) . ?
C49 C50 1.506(5) . ?
N11 C89 1.325(6) . ?
N11 C86 1.438(6) . ?
N3 C25 1.355(7) . ?
N3 C22 1.433(7) . ?
C10 C11 1.352(6) . ?
C10 C15 1.407(6) . ?
C10 C9 1.521(6) . ?
C58 C59 1.334(6) . ?
C58 C63 1.380(6) . ?
C58 C57 1.510(6) . ?
O6 C41 1.221(6) . ?
C6 C5 1.349(6) . ?
C6 C7 1.384(6) . ?
C51 C52 1.372(6) . ?
C51 C56 1.374(6) . ?
C56 C55 1.406(5) . ?
O4 C25 1.229(7) . ?
C86 C87 1.396(6) . ?
C86 C85 1.417(7) . ?
C2 C1 1.495(6) . ?
C61 C62 1.345(6) . ?
C61 C60 1.370(6) . ?
C61 C64 1.467(6) . ?
C3 C4 1.361(6) . ?
C3 C8 1.389(6) . ?
C67 C68 1.368(6) . ?
C67 C72 1.378(6) . ?
C90 C95 1.380(6) . ?
C90 C91 1.382(7) . ?
C90 C89 1.475(6) . ?
C52 C53 1.395(6) . ?
C36 C35 1.369(6) . ?
C36 C37 1.399(6) . ?
C5 C4 1.395(6) . ?
C81 C82 1.534(6) . ?
C38 C39 1.358(6) . ?
C38 C37 1.383(6) . ?
C8 C7 1.385(6) . ?
C69 C70 1.363(6) . ?
C69 C68 1.384(6) . ?
C53 C54 1.388(6) . ?
C31 C30 1.358(8) . ?
C31 C26 1.412(8) . ?
C54 C55 1.366(6) . ?
C15 C14 1.355(6) . ?
C35 C40 1.354(6) . ?
C73 C74 1.493(6) . ?
C39 C40 1.378(6) . ?
C85 C84 1.368(6) . ?
C66 C65 1.514(6) . ?
C59 C60 1.396(6) . ?
C33 C34 1.535(6) . ?
C13 C14 1.356(6) . ?
C13 C12 1.358(7) . ?
C13 C16 1.450(7) . ?
C42 C43 1.360(7) . ?
C42 C47 1.376(7) . ?
C42 C41 1.487(7) . ?
N5 C16 1.167(6) . ?
C74 C79 1.367(7) . ?
C74 C75 1.392(7) . ?
C83 C84 1.391(6) . ?
C83 C88 1.390(7) . ?
C17 C18 1.557(7) . ?
C11 C12 1.383(6) . ?
C70 C71 1.360(6) . ?
C87 C88 1.425(6) . ?
C95 C94 1.398(6) . ?
N13 C80 1.124(6) . ?
C46 C45 1.368(8) . ?
C46 C47 1.401(7) . ?
C44 C45 1.398(8) . ?
C44 C43 1.404(7) . ?
C62 C63 1.385(6) . ?
C94 C93 1.374(8) . ?
N14 C96 1.109(7) . ?
C23 C22 1.360(7) . ?
C23 C24 1.358(7) . ?
C29 C28 1.379(8) . ?
C29 C30 1.423(8) . ?
C29 C32 1.433(9) . ?
C19 C20 1.323(7) . ?
C19 C24 1.410(7) . ?
C72 C71 1.376(6) . ?
C27 C28 1.374(7) . ?
C27 C26 1.443(7) . ?
C75 C76 1.379(6) . ?
C79 C78 1.385(7) . ?
C76 C77 1.387(8) . ?
C93 C92 1.347(8) . ?
C93 C96 1.457(8) . ?
C80 C77 1.480(7) . ?
N7 C48 1.117(7) . ?
C45 C48 1.485(8) . ?
C77 C78 1.364(8) . ?
C91 C92 1.418(7) . ?
C22 C21 1.412(7) . ?
C25 C26 1.475(8) . ?
C20 C21 1.368(7) . ?
N6 C32 1.222(9) . ?

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
O8 Cl1 O7 106.9(5) . . ?
O8 Cl1 O10 110.4(4) . . ?
O7 Cl1 O10 108.4(3) . . ?
O8 Cl1 O9 107.0(3) . . ?
O7 Cl1 O9 111.6(4) . . ?
O10 Cl1 O9 112.3(3) . . ?
O19 Cl2 O17 118.1(6) . . ?
O19 Cl2 O18 104.7(5) . . ?
O17 Cl2 O18 105.0(5) . . ?
O19 Cl2 O20 108.2(4) . . ?
O17 Cl2 O20 109.5(4) . . ?
O18 Cl2 O20 111.3(3) . . ?
C51 O13 C50 117.4(4) . . ?
C3 O1 C2 118.4(4) . . ?
C35 O5 C34 116.0(4) . . ?
C67 O11 C66 118.1(4) . . ?
C57 N9 C54 127.8(4) . . ?
C19 O3 C18 115.5(5) . . ?
C83 O15 C82 117.3(4) . . ?
C65 N8 C81 111.5(4) . . ?
C65 N8 C49 112.8(4) . . ?
C81 N8 C49 113.4(4) . . ?
C17 N110 C1 116.6(4) . . ?
C17 N110 C33 110.8(4) . . ?
C1 N110 C33 112.6(4) . . ?
C73 N10 C70 128.5(5) . . ?
C41 N4 C38 125.3(5) . . ?
C9 N2 C6 127.5(5) . . ?
C50 C49 N8 116.3(4) . . ?
C89 N11 C86 128.1(5) . . ?
C25 N3 C22 130.9(6) . . ?
C11 C10 C15 119.0(5) . . ?
C11 C10 C9 118.7(5) . . ?
C15 C10 C9 122.3(4) . . ?
C59 C58 C63 117.9(5) . . ?
C59 C58 C57 125.9(5) . . ?
C63 C58 C57 116.2(5) . . ?
C5 C6 C7 120.4(4) . . ?
C5 C6 N2 124.8(5) . . ?
C7 C6 N2 114.8(5) . . ?
O13 C51 C52 115.9(5) . . ?
O13 C51 C56 123.9(5) . . ?
C52 C51 C56 120.2(4) . . ?
C51 C56 C55 119.2(5) . . ?
C87 C86 C85 121.0(5) . . ?
C87 C86 N11 119.6(5) . . ?
C85 C86 N11 119.2(5) . . ?
O1 C2 C1 110.9(4) . . ?
C62 C61 C60 117.8(5) . . ?
C62 C61 C64 121.7(5) . . ?
C60 C61 C64 120.5(5) . . ?
C2 C1 N110 115.5(4) . . ?
O13 C50 C49 109.5(4) . . ?
C4 C3 C8 120.3(5) . . ?
C4 C3 O1 124.8(5) . . ?
C8 C3 O1 114.9(5) . . ?
C68 C67 C72 119.5(4) . . ?
C68 C67 O11 115.4(5) . . ?
C72 C67 O11 125.1(5) . . ?
C95 C90 C91 120.3(5) . . ?
C95 C90 C89 119.1(5) . . ?
C91 C90 C89 120.2(5) . . ?
C51 C52 C53 119.4(5) . . ?
C35 C36 C37 118.7(5) . . ?
C6 C5 C4 119.7(5) . . ?
N8 C81 C82 109.4(4) . . ?
C39 C38 C37 117.9(5) . . ?
C39 C38 N4 126.1(5) . . ?
C37 C38 N4 116.0(5) . . ?
C7 C8 C3 118.7(5) . . ?
C70 C69 C68 120.8(5) . . ?
C54 C53 C52 121.7(5) . . ?
O14 C57 N9 123.1(4) . . ?
O14 C57 C58 121.2(5) . . ?
N9 C57 C58 115.7(5) . . ?
C6 C7 C8 120.5(5) . . ?
C30 C31 C26 119.6(7) . . ?
O2 C9 N2 124.3(5) . . ?
O2 C9 C10 118.3(5) . . ?
N2 C9 C10 117.4(5) . . ?
C55 C54 C53 117.6(4) . . ?
C55 C54 N9 125.0(5) . . ?
C53 C54 N9 117.4(5) . . ?
C14 C15 C10 118.2(5) . . ?
C54 C55 C56 121.8(5) . . ?
C40 C35 O5 126.5(5) . . ?
C40 C35 C36 119.7(5) . . ?
O5 C35 C36 113.8(5) . . ?
O12 C73 N10 121.8(5) . . ?
O12 C73 C74 120.3(6) . . ?
N10 C73 C74 117.8(5) . . ?
C67 C68 C69 119.4(5) . . ?
C38 C39 C40 120.8(5) . . ?
C84 C85 C86 120.2(5) . . ?
O11 C66 C65 107.4(4) . . ?
C58 C59 C60 121.5(5) . . ?
N110 C33 C34 110.7(4) . . ?
C14 C13 C12 119.3(5) . . ?
C14 C13 C16 120.3(5) . . ?
C12 C13 C16 120.4(5) . . ?
C38 C37 C36 121.5(5) . . ?
C3 C4 C5 120.4(5) . . ?
C43 C42 C47 119.3(6) . . ?
C43 C42 C41 123.1(6) . . ?
C47 C42 C41 117.5(6) . . ?
C79 C74 C75 120.0(5) . . ?
C79 C74 C73 116.0(6) . . ?
C75 C74 C73 123.9(6) . . ?
O15 C83 C84 117.3(5) . . ?
O15 C83 C88 122.8(5) . . ?
C84 C83 C88 119.8(5) . . ?
N110 C17 C18 110.9(4) . . ?
C10 C11 C12 121.2(5) . . ?
C71 C70 C69 119.8(5) . . ?
C71 C70 N10 123.0(5) . . ?
C69 C70 N10 117.2(5) . . ?
C13 C12 C11 119.5(5) . . ?
C86 C87 C88 117.1(5) . . ?
C15 C14 C13 122.7(5) . . ?
C90 C95 C94 119.1(5) . . ?
O5 C34 C33 106.5(4) . . ?
N8 C65 C66 110.9(4) . . ?
C45 C46 C47 119.9(7) . . ?
N12 C64 C61 177.5(7) . . ?
C45 C44 C43 119.4(6) . . ?
C61 C62 C63 121.6(5) . . ?
N5 C16 C13 178.8(7) . . ?
C93 C94 C95 121.1(6) . . ?
C85 C84 C83 120.4(5) . . ?
C35 C40 C39 121.3(5) . . ?
C22 C23 C24 119.9(6) . . ?
C28 C29 C30 120.7(7) . . ?
C28 C29 C32 120.6(8) . . ?
C30 C29 C32 118.7(8) . . ?
C20 C19 C24 122.8(6) . . ?
C20 C19 O3 124.2(6) . . ?
C24 C19 O3 113.0(6) . . ?
C58 C63 C62 120.6(5) . . ?
C71 C72 C67 120.3(5) . . ?
C28 C27 C26 119.6(6) . . ?
C76 C75 C74 120.7(6) . . ?
O16 C89 N11 122.2(5) . . ?
O16 C89 C90 121.7(5) . . ?
N11 C89 C90 116.0(5) . . ?
C83 C88 C87 121.3(5) . . ?
O6 C41 N4 123.6(5) . . ?
O6 C41 C42 119.4(6) . . ?
N4 C41 C42 116.9(5) . . ?
C74 C79 C78 119.9(6) . . ?
C61 C60 C59 120.7(5) . . ?
C70 C71 C72 120.1(5) . . ?
C75 C76 C77 117.7(6) . . ?
C92 C93 C94 119.4(6) . . ?
C92 C93 C96 121.6(7) . . ?
C94 C93 C96 118.9(7) . . ?
N13 C80 C77 175.0(8) . . ?
C46 C45 C44 119.5(6) . . ?
C46 C45 C48 119.3(7) . . ?
C44 C45 C48 121.2(7) . . ?
O15 C82 C81 104.3(4) . . ?
C42 C43 C44 120.9(6) . . ?
C78 C77 C76 122.2(6) . . ?
C78 C77 C80 119.3(7) . . ?
C76 C77 C80 118.4(7) . . ?
C23 C24 C19 118.5(6) . . ?
C27 C28 C29 120.0(7) . . ?
C90 C91 C92 118.6(5) . . ?
C23 C22 C21 120.0(6) . . ?
C23 C22 N3 118.8(6) . . ?
C21 C22 N3 121.0(7) . . ?
C31 C30 C29 120.6(7) . . ?
O3 C18 C17 104.1(5) . . ?
O4 C25 N3 123.1(7) . . ?
O4 C25 C26 119.9(7) . . ?
N3 C25 C26 117.0(7) . . ?
C77 C78 C79 119.3(6) . . ?
C19 C20 C21 118.7(6) . . ?
N7 C48 C45 176.2(8) . . ?
C93 C92 C91 121.3(6) . . ?
C20 C21 C22 120.0(6) . . ?
C42 C47 C46 120.9(7) . . ?
C31 C26 C27 119.4(6) . . ?
C31 C26 C25 122.0(6) . . ?
C27 C26 C25 118.6(7) . . ?
N14 C96 C93 179.9(12) . . ?
N6 C32 C29 176.0(10) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        28.70
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.060

# start Validation Reply Form
_vrf_PLAT230_2LH-ClO4            
;
PROBLEM: Hirshfeld Test Diff for O3 -- C19 .. 7.2 su
RESPONSE: The chemical composition and geometry of the ring is correct. 
These carbons can not be split further.
;
_vrf_PLAT230_B_2LH-ClO4          
;
PROBLEM: Hirshfeld Test Diff for C30 -- C31 .. 7.2 su.
RESPONSE: SEE _PLAT230_ALERT_2_B_
;
_vrf_PLAT230                     
;
PROBLEM: Hirshfeld Test Diff for C85 -- C86 .. 7.3 su 
RESPONSE: SEE _PLAT230_ALERT_2_B_
;
####################################################################### 
# 
# 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_(2LH)2-SIF6-4H20-2DMF
_database_code_depnum_ccdc_archive 'CCDC 1041365'
_audit_update_record             
;
2015-04-10 deposited with the CCDC.
2015-04-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C48H40N7O6), F6 Si, 2(C3H7NO), 4(H2O)'
_chemical_formula_sum            'C102 H102 F6 N16 O18 Si'

_chemical_formula_weight         1982.09

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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.0320(8)
_cell_length_b                   13.7659(9)
_cell_length_c                   15.5660(11)
_cell_angle_alpha                99.496(5)
_cell_angle_beta                 108.367(5)
_cell_angle_gamma                101.296(5)
_cell_volume                     2520.6(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2467
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      24.19

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             880
_exptl_absorpt_coefficient_mu    0.109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.973
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25806
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_unetI/netI     0.0935
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.42
_diffrn_reflns_theta_max         27.04
_reflns_number_total             10949
_reflns_number_gt                6677
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.1271P)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         10049
_refine_ls_number_parameters     668
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1958
_refine_ls_R_factor_gt           0.0732
_refine_ls_wR_factor_ref         0.2639
_refine_ls_wR_factor_gt          0.1985
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_restrained_S_all      0.984
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001

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
Si1 Si 0.0000 0.5000 0.0000 0.0612(5) Uani 1 2 d S . .
N6 N 0.2254(3) 0.5591(3) 0.5439(3) 0.0744(11) Uani 1 1 d . . .
H6 H 0.1837 0.5751 0.5741 0.089 Uiso 1 1 calc R . .
N4 N 0.0952(3) 0.5774(3) 0.7919(3) 0.0761(12) Uani 1 1 d . . .
H4N H 0.0658 0.5804 0.8342 0.091 Uiso 1 1 calc R . .
N1 N 0.6321(4) 0.3458(3) 0.8311(3) 0.0769(13) Uani 1 1 d . . .
N2 N 0.1563(4) 0.1519(4) 1.0176(3) 0.1026(15) Uani 1 1 d . . .
H2N H 0.1025 0.1753 0.9880 0.123 Uiso 1 1 calc R . .
N7 N -0.0934(6) 0.9390(5) 0.3714(4) 0.132(2) Uani 1 1 d . . .
N5 N -0.4419(6) 0.7508(6) 0.6629(7) 0.216(5) Uani 1 1 d . . .
N3 N -0.3241(8) 0.1209(6) 1.1959(6) 0.184(3) Uani 1 1 d . . .
N8 N 0.6509(6) 0.0172(5) 0.4555(7) 0.152(3) Uani 1 1 d . . .
C3 C 0.4179(5) 0.1814(4) 0.9158(4) 0.0857(16) Uani 1 1 d . . .
C1 C 0.6774(4) 0.2644(4) 0.8732(4) 0.0919(16) Uani 1 1 d . . .
H1A H 0.7564 0.2920 0.9108 0.110 Uiso 1 1 calc R . .
H1B H 0.6699 0.2074 0.8237 0.110 Uiso 1 1 calc R . .
C8 C 0.3110(5) 0.1733(4) 0.8589(4) 0.0816(15) Uani 1 1 d . . .
H8 H 0.2955 0.1749 0.7966 0.098 Uiso 1 1 calc R . .
C6 C 0.2486(5) 0.1600(4) 0.9860(4) 0.0924(17) Uani 1 1 d . . .
C7 C 0.2272(5) 0.1627(4) 0.8944(4) 0.0846(15) Uani 1 1 d . . .
H7 H 0.1543 0.1571 0.8558 0.102 Uiso 1 1 calc R . .
C10 C 0.0387(5) 0.1142(5) 1.1101(4) 0.1045(19) Uani 1 1 d . . .
C2 C 0.6142(5) 0.2275(5) 0.9330(4) 0.110(2) Uani 1 1 d . . .
H2A H 0.6384 0.1712 0.9556 0.132 Uiso 1 1 calc R . .
H2B H 0.6265 0.2822 0.9862 0.132 Uiso 1 1 calc R . .
C11 C 0.0253(6) 0.0761(4) 1.1816(5) 0.105(2) Uani 1 1 d . . .
H11 H 0.0798 0.0482 1.2152 0.127 Uiso 1 1 calc R . .
C4 C 0.4405(5) 0.1757(6) 1.0063(4) 0.125(2) Uani 1 1 d . . .
H4 H 0.5131 0.1795 1.0442 0.151 Uiso 1 1 calc R . .
C13 C -0.1471(6) 0.1157(5) 1.1563(5) 0.1005(19) Uani 1 1 d . . .
C9 C 0.1434(6) 0.1121(6) 1.0882(5) 0.111(2) Uani 1 1 d . . .
C5 C 0.3549(6) 0.1643(6) 1.0414(4) 0.130(3) Uani 1 1 d . . .
H5 H 0.3698 0.1596 1.1029 0.156 Uiso 1 1 calc R . .
C15 C -0.0443(7) 0.1566(10) 1.0628(6) 0.220(6) Uani 1 1 d . . .
H15 H -0.0360 0.1861 1.0150 0.265 Uiso 1 1 calc R . .
C12 C -0.0672(7) 0.0775(5) 1.2059(5) 0.111(2) Uani 1 1 d . . .
H12 H -0.0743 0.0522 1.2562 0.133 Uiso 1 1 calc R . .
C16 C -0.2444(9) 0.1185(6) 1.1791(6) 0.135(3) Uani 1 1 d . . .
C19 C 0.3964(4) 0.4912(4) 0.8579(3) 0.0672(12) Uani 1 1 d . . .
C25 C 0.0416(4) 0.6010(4) 0.7130(4) 0.0693(13) Uani 1 1 d . . .
C22 C 0.1978(4) 0.5475(4) 0.8117(3) 0.0637(12) Uani 1 1 d . . .
C21 C 0.2057(4) 0.4626(4) 0.8474(3) 0.0702(13) Uani 1 1 d . . .
H21 H 0.1441 0.4244 0.8561 0.084 Uiso 1 1 calc R . .
C26 C -0.0647(4) 0.6336(4) 0.7067(3) 0.0685(12) Uani 1 1 d . . .
C24 C 0.3911(4) 0.5765(4) 0.8238(3) 0.0729(13) Uani 1 1 d . . .
H24 H 0.4535 0.6147 0.8162 0.087 Uiso 1 1 calc R . .
C18 C 0.5900(4) 0.5103(4) 0.8744(4) 0.0847(15) Uani 1 1 d . . .
H18A H 0.6177 0.5770 0.9177 0.102 Uiso 1 1 calc R . .
H18B H 0.5764 0.5193 0.8116 0.102 Uiso 1 1 calc R . .
C23 C 0.2911(4) 0.6051(4) 0.8008(3) 0.0711(13) Uani 1 1 d . . .
H23 H 0.2866 0.6630 0.7779 0.085 Uiso 1 1 calc R . .
C27 C -0.1200(5) 0.6219(5) 0.7687(4) 0.1001(19) Uani 1 1 d . . .
H27 H -0.0921 0.5924 0.8177 0.120 Uiso 1 1 calc R . .
C31 C -0.1086(4) 0.6757(4) 0.6341(3) 0.0835(15) Uani 1 1 d . . .
H31 H -0.0727 0.6836 0.5917 0.100 Uiso 1 1 calc R . .
C29 C -0.2589(5) 0.6953(5) 0.6843(5) 0.0931(17) Uani 1 1 d . . .
C17 C 0.6730(4) 0.4477(4) 0.8986(4) 0.0891(16) Uani 1 1 d . . .
H17B H 0.7444 0.4837 0.8978 0.107 Uiso 1 1 calc R . .
H17A H 0.6845 0.4385 0.9611 0.107 Uiso 1 1 calc R . .
C28 C -0.2160(5) 0.6538(5) 0.7579(5) 0.105(2) Uani 1 1 d . . .
H28 H -0.2520 0.6472 0.8005 0.126 Uiso 1 1 calc R . .
C30 C -0.2048(5) 0.7064(5) 0.6234(4) 0.1027(19) Uani 1 1 d . . .
H30 H -0.2334 0.7351 0.5739 0.123 Uiso 1 1 calc R . .
C32 C -0.3608(6) 0.7272(6) 0.6743(6) 0.137(3) Uani 1 1 d . . .
C40 C 0.2869(4) 0.4882(4) 0.5730(3) 0.0685(13) Uani 1 1 d . . .
C37 C 0.2391(4) 0.4102(4) 0.6076(3) 0.0715(13) Uani 1 1 d . . .
H37 H 0.1678 0.4051 0.6097 0.086 Uiso 1 1 calc R . .
C36 C 0.2962(4) 0.3418(4) 0.6381(3) 0.0747(14) Uani 1 1 d . . .
H36 H 0.2648 0.2915 0.6625 0.090 Uiso 1 1 calc R . .
C43 C 0.1418(5) 0.7422(4) 0.5246(4) 0.0840(15) Uani 1 1 d . . .
H43 H 0.1775 0.7421 0.5866 0.101 Uiso 1 1 calc R . .
C41 C 0.2270(4) 0.6036(4) 0.4725(3) 0.0739(14) Uani 1 1 d . . .
C38 C 0.4495(4) 0.4239(4) 0.5981(3) 0.0795(14) Uani 1 1 d . . .
H38 H 0.5203 0.4279 0.5950 0.095 Uiso 1 1 calc R . .
C42 C 0.1539(4) 0.6736(4) 0.4541(3) 0.0709(13) Uani 1 1 d . . .
C35 C 0.4012(4) 0.3477(4) 0.6326(3) 0.0717(13) Uani 1 1 d . . .
C39 C 0.3927(4) 0.4935(4) 0.5684(3) 0.0752(14) Uani 1 1 d . . .
H39 H 0.4251 0.5443 0.5450 0.090 Uiso 1 1 calc R . .
C47 C 0.1007(5) 0.6769(5) 0.3622(4) 0.0869(16) Uani 1 1 d . . .
H47 H 0.1087 0.6328 0.3140 0.104 Uiso 1 1 calc R . .
C46 C 0.0359(5) 0.7448(5) 0.3412(4) 0.0913(16) Uani 1 1 d . . .
H46 H -0.0004 0.7453 0.2794 0.110 Uiso 1 1 calc R . .
C45 C 0.0260(4) 0.8113(4) 0.4126(4) 0.0802(14) Uani 1 1 d . . .
C48 C -0.0413(6) 0.8836(6) 0.3904(4) 0.1025(19) Uani 1 1 d . . .
C34 C 0.5595(5) 0.2708(5) 0.6606(4) 0.0923(17) Uani 1 1 d . . .
H34A H 0.5631 0.2832 0.6019 0.111 Uiso 1 1 calc R . .
H34B H 0.5710 0.2038 0.6640 0.111 Uiso 1 1 calc R . .
C33 C 0.6503(4) 0.3508(5) 0.7406(4) 0.0888(16) Uani 1 1 d . . .
H33A H 0.6497 0.4179 0.7294 0.107 Uiso 1 1 calc R . .
H33B H 0.7228 0.3398 0.7449 0.107 Uiso 1 1 calc R . .
C44 C 0.0779(5) 0.8104(4) 0.5042(4) 0.0864(16) Uani 1 1 d . . .
H44 H 0.0700 0.8551 0.5520 0.104 Uiso 1 1 calc R . .
C50 C 0.7208(9) -0.0440(8) 0.5220(11) 0.244(7) Uani 1 1 d . . .
H50C H 0.7683 0.0022 0.5808 0.366 Uiso 1 1 calc R . .
H50A H 0.7659 -0.0734 0.4926 0.366 Uiso 1 1 calc R . .
H50B H 0.6696 -0.0973 0.5322 0.366 Uiso 1 1 calc R . .
C51 C 0.6190(19) 0.0828(15) 0.4875(19) 0.49(2) Uani 1 1 d . . .
H51 H 0.5770 0.1209 0.4544 0.591 Uiso 1 1 calc R . .
C49 C 0.6257(10) -0.0049(9) 0.3579(8) 0.216(5) Uani 1 1 d . . .
H49C H 0.5749 0.0329 0.3303 0.324 Uiso 1 1 calc R . .
H49B H 0.5915 -0.0767 0.3317 0.324 Uiso 1 1 calc R . .
H49A H 0.6935 0.0141 0.3454 0.324 Uiso 1 1 calc R . .
O4 O 0.4898(3) 0.4538(3) 0.8813(2) 0.0825(10) Uani 1 1 d . . .
O1 O 0.4986(3) 0.1951(3) 0.8738(2) 0.0985(12) Uani 1 1 d . . .
O5 O 0.4506(3) 0.2734(3) 0.6643(2) 0.0829(10) Uani 1 1 d . . .
O6 O 0.2823(3) 0.5868(3) 0.4242(2) 0.0936(12) Uani 1 1 d . . .
O3 O 0.0747(3) 0.5984(3) 0.6470(2) 0.0947(12) Uani 1 1 d . . .
O2 O 0.2151(4) 0.0790(5) 1.1360(4) 0.1367(18) Uani 1 1 d . . .
O7 O 0.6565(7) 0.0947(6) 0.5889(8) 0.246(4) Uani 1 1 d . . .
C20 C 0.3058(4) 0.4344(4) 0.8703(3) 0.0702(13) Uani 1 1 d . . .
H20 H 0.3112 0.3771 0.8940 0.084 Uiso 1 1 calc R . .
F1 F 0.0842(2) 0.4214(2) 0.00923(19) 0.0780(8) Uani 1 1 d . . .
F3 F -0.08959(19) 0.4163(2) 0.02811(17) 0.0744(7) Uani 1 1 d . . .
F2 F 0.0679(2) 0.5595(2) 0.11368(16) 0.0792(8) Uani 1 1 d . . .
C14 C -0.1357(7) 0.1557(10) 1.0848(6) 0.205(5) Uani 1 1 d . . .
H14 H -0.1913 0.1824 1.0510 0.246 Uiso 1 1 calc R . .
O8 O 0.9897(6) 0.2240(6) 0.8784(4) 0.1121(18) Uani 1 1 d . . .
O9 O 0.7799(6) 0.0914(5) 0.7728(5) 0.162(2) Uani 1 1 d D . .
H1N H 0.561(4) 0.329(3) 0.815(3) 0.080(15) Uiso 1 1 d . . .
H9OB H 0.748(9) 0.058(8) 0.833(10) 0.83(8) Uiso 1 1 d D . .
H9OA H 0.755(3) 0.128(3) 0.735(2) 0.055(13) Uiso 1 1 d D . .
H8OA H 0.999(8) 0.287(8) 0.895(6) 0.18(5) Uiso 1 1 d . . .
H8OB H 0.960(10) 0.186(8) 0.883(8) 0.34(7) Uiso 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
Si1 F1 1.677(2) 2_565 ?
Si1 F1 1.677(2) . ?
Si1 F3 1.687(2) . ?
Si1 F3 1.687(2) 2_565 ?
Si1 F2 1.684(2) 2_565 ?
Si1 F2 1.684(2) . ?
N6 C41 1.358(6) . ?
N6 C40 1.421(6) . ?
N4 C25 1.334(6) . ?
N4 C22 1.432(6) . ?
N1 C17 1.491(6) . ?
N1 C33 1.511(6) . ?
N1 C1 1.514(7) . ?
N2 C9 1.348(8) . ?
N2 C6 1.428(7) . ?
N7 C48 1.132(8) . ?
N5 C32 1.136(8) . ?
N3 C16 1.153(9) . ?
N8 C51 1.169(19) . ?
N8 C49 1.415(11) . ?
N8 C50 1.614(13) . ?
C3 C8 1.367(7) . ?
C3 C4 1.365(8) . ?
C3 O1 1.401(6) . ?
C1 C2 1.510(7) . ?
C8 C7 1.365(7) . ?
C6 C7 1.372(7) . ?
C6 C5 1.366(8) . ?
C10 C11 1.351(8) . ?
C10 C15 1.392(10) . ?
C10 C9 1.511(9) . ?
C2 O1 1.430(6) . ?
C11 C12 1.374(8) . ?
C4 C5 1.382(8) . ?
C13 C14 1.357(9) . ?
C13 C12 1.341(9) . ?
C13 C16 1.426(10) . ?
C9 O2 1.215(8) . ?
C15 C14 1.337(10) . ?
C19 C20 1.369(6) . ?
C19 C24 1.371(7) . ?
C19 O4 1.381(5) . ?
C25 O3 1.232(5) . ?
C25 C26 1.517(6) . ?
C22 C21 1.382(6) . ?
C22 C23 1.390(6) . ?
C21 C20 1.389(6) . ?
C26 C31 1.371(6) . ?
C26 C27 1.385(7) . ?
C24 C23 1.391(6) . ?
C18 O4 1.428(6) . ?
C18 C17 1.507(7) . ?
C27 C28 1.376(8) . ?
C31 C30 1.371(7) . ?
C29 C30 1.359(8) . ?
C29 C28 1.374(8) . ?
C29 C32 1.450(9) . ?
C40 C39 1.392(6) . ?
C40 C37 1.404(6) . ?
C37 C36 1.366(7) . ?
C36 C35 1.385(6) . ?
C43 C44 1.384(7) . ?
C43 C42 1.395(6) . ?
C41 O6 1.220(5) . ?
C41 C42 1.483(7) . ?
C38 C39 1.374(7) . ?
C38 C35 1.388(7) . ?
C42 C47 1.392(7) . ?
C35 O5 1.388(6) . ?
C47 C46 1.389(7) . ?
C46 C45 1.376(7) . ?
C45 C44 1.375(7) . ?
C45 C48 1.464(9) . ?
C34 O5 1.446(6) . ?
C34 C33 1.506(7) . ?
C51 O7 1.47(3) . ?

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
F1 Si1 F1 180.000(1) 2_565 . ?
F1 Si1 F3 90.73(12) 2_565 . ?
F1 Si1 F3 89.27(12) . . ?
F1 Si1 F3 89.27(12) 2_565 2_565 ?
F1 Si1 F3 90.73(12) . 2_565 ?
F3 Si1 F3 180.00(18) . 2_565 ?
F1 Si1 F2 90.10(13) 2_565 2_565 ?
F1 Si1 F2 89.90(13) . 2_565 ?
F3 Si1 F2 89.81(12) . 2_565 ?
F3 Si1 F2 90.19(12) 2_565 2_565 ?
F1 Si1 F2 89.90(13) 2_565 . ?
F1 Si1 F2 90.10(13) . . ?
F3 Si1 F2 90.19(12) . . ?
F3 Si1 F2 89.81(12) 2_565 . ?
F2 Si1 F2 180.0(2) 2_565 . ?
C41 N6 C40 125.6(4) . . ?
C25 N4 C22 125.3(4) . . ?
C17 N1 C33 112.4(4) . . ?
C17 N1 C1 112.9(4) . . ?
C33 N1 C1 112.4(4) . . ?
C9 N2 C6 127.7(6) . . ?
C51 N8 C49 117.3(19) . . ?
C51 N8 C50 120.1(18) . . ?
C49 N8 C50 122.6(8) . . ?
C8 C3 C4 120.6(5) . . ?
C8 C3 O1 115.1(5) . . ?
C4 C3 O1 124.4(5) . . ?
N1 C1 C2 110.4(4) . . ?
C3 C8 C7 119.2(5) . . ?
C7 C6 C5 119.2(5) . . ?
C7 C6 N2 117.1(5) . . ?
C5 C6 N2 123.7(6) . . ?
C6 C7 C8 121.2(5) . . ?
C11 C10 C15 117.2(7) . . ?
C11 C10 C9 118.8(7) . . ?
C15 C10 C9 124.0(7) . . ?
O1 C2 C1 105.6(5) . . ?
C10 C11 C12 121.5(7) . . ?
C3 C4 C5 119.7(6) . . ?
C14 C13 C12 120.7(7) . . ?
C14 C13 C16 118.2(8) . . ?
C12 C13 C16 121.1(7) . . ?
O2 C9 N2 121.8(7) . . ?
O2 C9 C10 120.1(7) . . ?
N2 C9 C10 118.0(7) . . ?
C6 C5 C4 120.1(6) . . ?
C14 C15 C10 121.3(8) . . ?
C13 C12 C11 119.3(7) . . ?
N3 C16 C13 178.7(10) . . ?
C20 C19 C24 121.4(4) . . ?
C20 C19 O4 114.1(5) . . ?
C24 C19 O4 124.5(4) . . ?
O3 C25 N4 123.4(5) . . ?
O3 C25 C26 119.4(5) . . ?
N4 C25 C26 117.1(4) . . ?
C21 C22 C23 119.5(4) . . ?
C21 C22 N4 118.9(4) . . ?
C23 C22 N4 121.5(5) . . ?
C22 C21 C20 119.9(4) . . ?
C31 C26 C27 118.7(5) . . ?
C31 C26 C25 117.3(4) . . ?
C27 C26 C25 124.0(5) . . ?
C19 C24 C23 119.0(4) . . ?
O4 C18 C17 105.5(4) . . ?
C22 C23 C24 120.4(5) . . ?
C28 C27 C26 120.3(6) . . ?
C26 C31 C30 120.7(5) . . ?
C30 C29 C28 119.7(5) . . ?
C30 C29 C32 121.5(7) . . ?
C28 C29 C32 118.8(7) . . ?
N1 C17 C18 111.0(4) . . ?
C29 C28 C27 120.0(6) . . ?
C29 C30 C31 120.6(6) . . ?
N5 C32 C29 177.4(9) . . ?
C39 C40 C37 118.9(5) . . ?
C39 C40 N6 122.3(4) . . ?
C37 C40 N6 118.8(4) . . ?
C36 C37 C40 120.7(5) . . ?
C37 C36 C35 119.7(5) . . ?
C44 C43 C42 121.3(5) . . ?
O6 C41 N6 123.5(5) . . ?
O6 C41 C42 120.7(5) . . ?
N6 C41 C42 115.7(4) . . ?
C39 C38 C35 119.9(5) . . ?
C47 C42 C43 117.8(5) . . ?
C47 C42 C41 118.7(5) . . ?
C43 C42 C41 123.3(5) . . ?
C38 C35 C36 120.4(5) . . ?
C38 C35 O5 125.0(5) . . ?
C36 C35 O5 114.7(5) . . ?
C38 C39 C40 120.4(5) . . ?
C42 C47 C46 121.2(5) . . ?
C45 C46 C47 119.3(5) . . ?
C46 C45 C44 120.9(6) . . ?
C46 C45 C48 119.3(6) . . ?
C44 C45 C48 119.8(5) . . ?
N7 C48 C45 178.6(7) . . ?
O5 C34 C33 110.2(4) . . ?
C34 C33 N1 110.4(4) . . ?
C45 C44 C43 119.4(5) . . ?
N8 C51 O7 108(3) . . ?
C19 O4 C18 118.2(4) . . ?
C3 O1 C2 118.1(4) . . ?
C35 O5 C34 119.7(4) . . ?
C19 C20 C21 119.8(5) . . ?
C13 C14 C15 119.9(8) . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        27.04
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.922
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.052

# start Validation Reply Form
_vrf_PLAT223_2LH2-SIF6-4H20-2DMF 
;
PROBLEM: Large Solvent/Anion H    Ueq(max)/Ueq(min) .....       10.0 Ratio 
RESPONSE: It is originating due hydrogen assignment of the water molecule.
;
_vrf_PLAT245_2LH2-SIF6-4H20-2DMF 
;
PROBLEM: U(iso) H9OA    Smaller than U(eq) O9      by ...      0.107 AngSq 
RESPONSE: Due to the disorder in the H atom assinged to the water.
;
_vrf_PLAT355_2LH2-SIF6-4H20-2DMF 
;
PROBLEM: Long    O-H (X0.82,N0.98A) O9     -   H9OB   ...       1.26 Ang.  
RESPONSE: Due to the disorder in the H atom assinged to the water.
;
_vrf_PLAT241_2LH2-SIF6-4H20-2DMF 
;
PROBLEM: High      Ueq as Compared to Neighbors for .....        C15 Check 
RESPONSE: ...
;
_vrf_PLAT415_2LH2-SIF6-4H20-2DMF 
;
PROBLEM: Short Inter D-H..H-X       H8OB   ..  H15     ..       2.04 Ang.  
RESPONSE: Due to the disorder in the H atom assinged to the water.
;
# end Validation Reply Form
