# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_ral1106a
_database_code_depnum_ccdc_archive 'CCDC 1456584'
_audit_update_record             
;
2016-02-29 deposited with the CCDC.
2016-04-20 downloaded from the CCDC.
;
_audit_creation_date             11-11-04
_audit_creation_method           CRYSTALS_ver_14.11

_oxford_structure_analysis_title '11031626 ral1106'
_chemical_name_systematic        
;
1,5,5,9,13,13,20,20-octamethyl-3,7,11,15,18,
22-hexaazabicyclo[7.7.7]tricosanezinc(II) nitrate monohydrate
;
_chemical_melting_point          ?

_cell_length_a                   10.4071(2)
_cell_length_b                   17.2603(4)
_cell_length_c                   17.7437(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.3125(15)
_cell_angle_gamma                90.00
_cell_volume                     3074.15(12)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1 '
_symmetry_space_group_name_Hall  ?

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Zn 0.2839 1.4301 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097
1.3041 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C25 H54 N8 O6 Zn1 
# Dc =      1.36 Fooo =   1392.00 Mu =      8.50 M =    314.07
# Found Formula = C25 H56 N8 O7 Zn1 
# Dc =      1.40 FOOO =   1392.00 Mu =      8.54 M =    323.07

_chemical_formula_sum            'C25 H56 N8 O7 Zn'
_chemical_formula_moiety         'C25 H54 N6 Zn 2+, (N O3 -)2, H2 O '
_chemical_compound_source        ' from U of Wollongong'
_chemical_formula_weight         646.15


_cell_measurement_reflns_used    33931
_cell_measurement_theta_min      3
_cell_measurement_theta_max      27.5
_cell_measurement_temperature    200

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.080
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_max          0.220

_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1392
_exptl_absorpt_coefficient_mu    0.854

# Sheldrick geometric approximatio 0.90 0.93 
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.100
-1 0 0 0.120
0 1 0 0.030
0 -1 0 0.050
0 0 1 0.080
0 0 -1 0.040
-1 0 2 0.108
1 0 -2 0.057
0 1 -1 0.010
0 -1 1 0.070
0 1 1 0.060
0 -1 -1 0.060


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.868
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_process_details   
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
#_diffrn_reflns_av_R_equivalents   0.066

# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
#_diffrn_measurement_method       '\f & \w scans'
_diffrn_special_details          
;
CCD data collecting conditions-
phi and omega scans of width 1.8 deg at rate 270 sec/frame,
crystal-detector distance 28mm,
multiple scan sets so over 90 percent of data collected with 4-fold  
redundancy or more.
;

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;

_diffrn_standards_interval_time  ?
_diffrn_standards_interval_count ?
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      200
_diffrn_reflns_number            30806
_reflns_number_total             3523
_diffrn_reflns_av_R_equivalents  0.075
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 3523 
# Theoretical number of reflections is about 7074 


_diffrn_reflns_theta_min         2.643
_diffrn_reflns_theta_max         27.517
_diffrn_measured_fraction_theta_max 0.995

_diffrn_reflns_theta_full        27.517
_diffrn_measured_fraction_theta_full 0.995


_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_reflns_limit_h_min              -13
_reflns_limit_h_max              13
_reflns_limit_k_min              0
_reflns_limit_k_max              22
_reflns_limit_l_min              0
_reflns_limit_l_max              23

_oxford_diffrn_Wilson_B_factor   2.27
_oxford_diffrn_Wilson_scale      9.75

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -0.58
_refine_diff_density_max         0.32


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
#_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         3522
_refine_ls_number_restraints     0
_refine_ls_number_parameters     271
#_oxford_refine_ls_R_factor_ref   0.0362
_refine_ls_wR_factor_ref         0.0806
_refine_ls_goodness_of_fit_ref   1.0040
_refine_ls_shift/su_max          0.0072251
_refine_ls_shift/su_mean         0.0010439


# The values computed from all data 
#_oxford_reflns_number_all        3522
_refine_ls_R_factor_all          0.0362
_refine_ls_wR_factor_all         0.0806

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                3201
_refine_ls_R_factor_gt           0.0319
_refine_ls_wR_factor_gt          0.0786

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    refxyz # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.04P)² + 2.88P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_special_details          
;
The largest features in the
final difference electron density map are located 
midway along bonds.
;


# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Zn1 Zn 0.5000 0.578187(13) 0.7500 0.0233 1.0000 Uani S T . . . .
O21 O 0.1470(2) 0.44571(13) 0.84249(12) 0.0792 1.0000 Uani . . . . . .
O22 O 0.35116(17) 0.44910(9) 0.91227(9) 0.0547 1.0000 Uani . . . . . .
O23 O 0.23027(18) 0.34628(9) 0.91104(10) 0.0622 1.0000 Uani . . . . . .
O30 O 0.0000 0.31598(14) 0.7500 0.0692 1.0000 Uani S T . . . .
N4 N 0.30414(13) 0.58773(7) 0.78179(8) 0.0262 1.0000 Uani . . . . . .
N10 N 0.41963(13) 0.65716(8) 0.65212(8) 0.0261 1.0000 Uani . . . . . .
N13 N 0.40134(13) 0.48280(7) 0.66864(8) 0.0260 1.0000 Uani . . . . . .
N20 N 0.24233(19) 0.41379(10) 0.88925(10) 0.0459 1.0000 Uani . . . . . .
C1 C 0.06466(18) 0.58013(12) 0.57668(11) 0.0383 1.0000 Uani . . . . . .
C2 C 0.20496(15) 0.57831(9) 0.63313(9) 0.0279 1.0000 Uani . . . . . .
C3 C 0.18587(15) 0.56958(10) 0.71559(10) 0.0294 1.0000 Uani . . . . . .
C5 C 0.29545(16) 0.66671(9) 0.81361(10) 0.0303 1.0000 Uani . . . . . .
C6 C 0.37788(16) 0.67693(10) 0.89844(9) 0.0311 1.0000 Uani . . . . . .
C7 C 0.30816(19) 0.63759(13) 0.95476(11) 0.0398 1.0000 Uani . . . . . .
C8 C 0.3922(2) 0.76347(11) 0.91696(12) 0.0417 1.0000 Uani . . . . . .
C9 C 0.27137(15) 0.65546(9) 0.62207(10) 0.0289 1.0000 Uani . . . . . .
C11 C 0.48496(16) 0.63960(10) 0.58856(9) 0.0298 1.0000 Uani . . . . . .
C12 C 0.27680(15) 0.50799(9) 0.60963(9) 0.0289 1.0000 Uani . . . . . .
C14 C 0.37638(16) 0.41675(9) 0.71671(10) 0.0290 1.0000 Uani . . . . . .
C15 C 0.5000 0.36651(12) 0.7500 0.0298 1.0000 Uani S T . . . .
C16 C 0.5287(2) 0.31482(10) 0.68608(11) 0.0372 1.0000 Uani . . . . . .
H11 H 0.070(2) 0.5786(13) 0.5198(15) 0.0561 1.0000 Uiso . . . . . .
H12 H 0.020(2) 0.6285(14) 0.5853(14) 0.0557 1.0000 Uiso . . . . . .
H13 H 0.011(2) 0.5368(14) 0.5866(14) 0.0561 1.0000 Uiso . . . . . .
H31 H 0.115(2) 0.6044(12) 0.7191(11) 0.0342 1.0000 Uiso . . . . . .
H32 H 0.1582(19) 0.5152(12) 0.7224(11) 0.0346 1.0000 Uiso . . . . . .
H41 H 0.304(2) 0.5536(12) 0.8215(12) 0.0386 1.0000 Uiso . . . . . .
H51 H 0.199(2) 0.6811(12) 0.8097(12) 0.0361 1.0000 Uiso . . . . . .
H52 H 0.325(2) 0.7049(11) 0.7820(11) 0.0346 1.0000 Uiso . . . . . .
H71 H 0.366(2) 0.6409(14) 1.0088(15) 0.0582 1.0000 Uiso . . . . . .
H72 H 0.228(3) 0.6629(15) 0.9531(14) 0.0578 1.0000 Uiso . . . . . .
H73 H 0.288(3) 0.5800(14) 0.9406(15) 0.0581 1.0000 Uiso . . . . . .
H81 H 0.440(3) 0.7714(15) 0.9724(15) 0.0616 1.0000 Uiso . . . . . .
H82 H 0.302(3) 0.7911(14) 0.9098(14) 0.0610 1.0000 Uiso . . . . . .
H83 H 0.440(3) 0.7929(14) 0.8833(15) 0.0615 1.0000 Uiso . . . . . .
H91 H 0.2324(19) 0.6958(11) 0.6467(12) 0.0330 1.0000 Uiso . . . . . .
H92 H 0.2479(19) 0.6691(11) 0.5680(12) 0.0332 1.0000 Uiso . . . . . .
H101 H 0.438(2) 0.7048(12) 0.6691(12) 0.0381 1.0000 Uiso . . . . . .
H111 H 0.430(2) 0.6558(11) 0.5390(12) 0.0348 1.0000 Uiso . . . . . .
H112 H 0.493(2) 0.5830(11) 0.5845(12) 0.0338 1.0000 Uiso . . . . . .
H121 H 0.2983(19) 0.5197(11) 0.5609(11) 0.0338 1.0000 Uiso . . . . . .
H122 H 0.216(2) 0.4636(12) 0.5994(11) 0.0335 1.0000 Uiso . . . . . .
H131 H 0.461(2) 0.4666(12) 0.6407(12) 0.0376 1.0000 Uiso . . . . . .
H141 H 0.344(2) 0.4385(11) 0.7600(12) 0.0349 1.0000 Uiso . . . . . .
H142 H 0.307(2) 0.3832(12) 0.6871(12) 0.0354 1.0000 Uiso . . . . . .
H161 H 0.611(3) 0.2888(14) 0.7068(14) 0.0545 1.0000 Uiso . . . . . .
H162 H 0.534(2) 0.3438(14) 0.6395(14) 0.0530 1.0000 Uiso . . . . . .
H163 H 0.459(2) 0.2743(14) 0.6698(14) 0.0549 1.0000 Uiso . . . . . .
H301 H 0.047(4) 0.3450(19) 0.784(2) 0.1029 1.0000 Uiso . . . . . .


_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.3130(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zn1 . N4 . 2.2600(12) yes
Zn1 . N10 . 2.1924(13) yes
Zn1 . N13 . 2.2508(13) yes
O21 . N20 . 1.242(3) yes
O22 . N20 . 1.256(2) yes
O23 . N20 . 1.244(2) yes
O30 . H301 5_556 0.83(3) no
O30 . H301 . 0.83(3) no
N4 . C3 . 1.493(2) yes
N4 . C5 . 1.487(2) yes
N4 . H41 . 0.92(2) no
N10 . C9 . 1.494(2) yes
N10 . C11 . 1.4937(19) yes
N10 . H101 . 0.88(2) no
N13 . C12 . 1.4994(19) yes
N13 . C14 . 1.4874(19) yes
N13 . H131 . 0.93(2) no
C1 . C2 . 1.537(2) yes
C1 . H11 . 1.03(3) no
C1 . H12 . 0.99(3) no
C1 . H13 . 0.97(2) no
C2 . C3 . 1.535(2) yes
C2 . C9 . 1.537(2) yes
C2 . C12 . 1.540(2) yes
C3 . H31 . 0.97(2) no
C3 . H32 . 1.00(2) no
C5 . C6 . 1.533(2) yes
C5 . H51 . 1.02(2) no
C5 . H52 . 0.96(2) no
C6 . C11 5_656 1.527(2) yes
C6 . C7 . 1.539(2) yes
C6 . C8 . 1.528(2) yes
C7 . H71 . 0.99(3) no
C7 . H72 . 0.93(3) no
C7 . H73 . 1.03(2) no
C8 . H81 . 0.99(3) no
C8 . H82 . 1.03(3) no
C8 . H83 . 1.01(3) no
C9 . H91 . 0.97(2) no
C9 . H92 . 0.96(2) no
C11 . H111 . 0.96(2) no
C11 . H112 . 0.985(19) no
C12 . H121 . 0.97(2) no
C12 . H122 . 0.98(2) no
C14 . C15 . 1.534(2) yes
C14 . H141 . 0.99(2) no
C14 . H142 . 0.97(2) no
C15 . C16 5_656 1.533(2) yes
C15 . C16 . 1.533(2) yes
C16 . H161 . 0.95(3) no
C16 . H162 . 0.98(2) no
C16 . H163 . 0.99(2) no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag

N4 5_656 Zn1 . N4 . 171.64(7) yes
N13 5_656 Zn1 . N4 . 100.49(5) yes
N10 5_656 Zn1 . N4 . 86.42(5) yes
N13 5_656 Zn1 . N10 . 167.65(5) yes
N10 5_656 Zn1 . N10 . 103.12(7) yes
N4 . Zn1 . N10 . 88.39(5) yes
N13 5_656 Zn1 . N13 . 85.98(6) yes
N4 . Zn1 . N13 . 85.68(5) yes
N10 . Zn1 . N13 . 86.14(5) yes
H301 5_556 O30 . H301 . 106(5) no
Zn1 . N4 . C3 . 113.51(9) yes
Zn1 . N4 . C5 . 108.11(9) yes
C3 . N4 . C5 . 111.77(12) yes
Zn1 . N4 . H41 . 108.9(13) no
C3 . N4 . H41 . 107.8(13) no
C5 . N4 . H41 . 106.5(13) no
Zn1 . N10 . C9 . 114.36(9) yes
Zn1 . N10 . C11 . 108.51(10) yes
C9 . N10 . C11 . 111.09(12) yes
Zn1 . N10 . H101 . 107.8(13) no
C9 . N10 . H101 . 104.8(14) no
C11 . N10 . H101 . 110.1(13) no
Zn1 . N13 . C12 . 113.55(9) yes
Zn1 . N13 . C14 . 108.18(9) yes
C12 . N13 . C14 . 111.90(12) yes
Zn1 . N13 . H131 . 107.9(12) no
C12 . N13 . H131 . 106.7(13) no
C14 . N13 . H131 . 108.5(12) no
O22 . N20 . O23 . 120.65(19) yes
O22 . N20 . O21 . 119.67(19) yes
O23 . N20 . O21 . 119.6(2) yes
C2 . C1 . H11 . 110.8(14) no
C2 . C1 . H12 . 108.6(14) no
H11 . C1 . H12 . 108.8(19) no
C2 . C1 . H13 . 110.8(14) no
H11 . C1 . H13 . 109.6(18) no
H12 . C1 . H13 . 108(2) no
C1 . C2 . C3 . 106.45(13) yes
C1 . C2 . C9 . 106.32(13) yes
C3 . C2 . C9 . 112.49(13) yes
C1 . C2 . C12 . 106.58(13) yes
C3 . C2 . C12 . 112.02(13) yes
C9 . C2 . C12 . 112.44(13) yes
C2 . C3 . N4 . 116.23(13) yes
C2 . C3 . H31 . 107.1(11) no
N4 . C3 . H31 . 107.8(11) no
C2 . C3 . H32 . 108.8(11) no
N4 . C3 . H32 . 107.8(11) no
H31 . C3 . H32 . 109.0(16) no
N4 . C5 . C6 . 113.81(13) yes
N4 . C5 . H51 . 110.8(11) no
C6 . C5 . H51 . 108.9(11) no
N4 . C5 . H52 . 110.2(12) no
C6 . C5 . H52 . 108.2(12) no
H51 . C5 . H52 . 104.5(16) no
C5 . C6 . C11 5_656 110.98(13) yes
C5 . C6 . C7 . 110.44(14) yes
C11 5_656 C6 . C7 . 107.33(14) yes
C5 . C6 . C8 . 108.72(15) yes
C11 5_656 C6 . C8 . 110.23(15) yes
C7 . C6 . C8 . 109.11(14) yes
C6 . C7 . H71 . 109.7(14) no
C6 . C7 . H72 . 110.1(15) no
H71 . C7 . H72 . 108.0(20) no
C6 . C7 . H73 . 111.5(14) no
H71 . C7 . H73 . 109(2) no
H72 . C7 . H73 . 109(2) no
C6 . C8 . H81 . 110.2(15) no
C6 . C8 . H82 . 113.0(14) no
H81 . C8 . H82 . 105.0(20) no
C6 . C8 . H83 . 113.6(14) no
H81 . C8 . H83 . 109(2) no
H82 . C8 . H83 . 105.8(20) no
C2 . C9 . N10 . 115.37(13) yes
C2 . C9 . H91 . 108.1(11) no
N10 . C9 . H91 . 110.0(12) no
C2 . C9 . H92 . 109.7(12) no
N10 . C9 . H92 . 108.7(12) no
H91 . C9 . H92 . 104.5(16) no
C6 5_656 C11 . N10 . 113.21(13) yes
C6 5_656 C11 . H111 . 109.0(12) no
N10 . C11 . H111 . 110.6(12) no
C6 5_656 C11 . H112 . 109.6(12) no
N10 . C11 . H112 . 108.8(12) no
H111 . C11 . H112 . 105.4(16) no
C2 . C12 . N13 . 115.57(13) yes
C2 . C12 . H121 . 108.6(11) no
N13 . C12 . H121 . 108.8(11) no
C2 . C12 . H122 . 109.3(11) no
N13 . C12 . H122 . 107.4(11) no
H121 . C12 . H122 . 106.7(15) no
N13 . C14 . C15 . 113.47(12) yes
N13 . C14 . H141 . 107.6(12) no
C15 . C14 . H141 . 109.9(12) no
N13 . C14 . H142 . 111.5(12) no
C15 . C14 . H142 . 107.7(12) no
H141 . C14 . H142 . 106.5(16) no
C14 . C15 . C14 5_656 111.18(18) yes
C14 . C15 . C16 5_656 107.83(10) yes
C14 5_656 C15 . C16 5_656 110.58(10) yes
C14 . C15 . C16 . 110.58(10) yes
C14 5_656 C15 . C16 . 107.83(10) yes
C16 5_656 C15 . C16 . 108.83(19) yes
C15 . C16 . H161 . 108.7(15) no
C15 . C16 . H162 . 113.2(14) no
H161 . C16 . H162 . 108.7(20) no
C15 . C16 . H163 . 110.7(14) no
H161 . C16 . H163 . 107.0(19) no
H162 . C16 . H163 . 108.4(19) no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
N4 . H41 . O21 . 134.6(16) 0.92(2) 2.57(2) 3.283(2) yes
N4 . H41 . O22 . 164.6(18) 0.92(2) 2.38(2) 3.275(2) yes
N10 . H101 . O30 3_555 163.8(18) 0.88(2) 2.38(2) 3.235(2) yes
N13 . H131 . O22 5_656 165.6(17) 0.93(2) 2.41(2) 3.315(2) yes
O30 . H301 . O21 . 162(3) 0.83(3) 2.15(3) 2.953(2) yes
O30 . H301 . O23 . 144(3) 0.83(3) 2.54(3) 3.250(2) yes

#------------------------------------------------------------------------------
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
O21 O30 2.953(3) . . no
O21 C3 3.207(3) . . no
O21 N4 3.282(3) . . no
O22 N4 3.275(2) . . no
O22 N13 3.315(2) . 5_656 no
O22 C16 3.337(3) . 5_656 no
O22 C7 3.396(3) . . no
O22 C11 3.430(2) . 6_565 no
O22 C14 3.592(2) . . no
O23 O30 3.250(2) . . no
O23 C9 3.345(2) . 7_546 no
O23 C16 3.441(3) . 5_656 no
O23 C11 3.549(2) . 6_565 no
O30 N10 3.235(2) . 3_445 no
O30 N10 3.235(2) . 7_546 no
O30 N20 3.468(2) . . no
O30 N20 3.468(2) . 5_556 no
O30 C8 3.551(2) . 3_445 no
O30 C8 3.551(2) . 7_546 no
N20 C16 3.474(3) . 5_656 no
#------------------------------------------------------------------------------
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Zn1 N4 C3 C2 . . . . -22.6(2) no
Zn1 N4 C5 C6 . . . . -78.1(2) no
Zn1 N4 C3 C2 . 5_656 5_656 5_656 -22.6(2) no
Zn1 N4 C5 C6 . 5_656 5_656 5_656 -78.1(2) no
Zn1 N10 C9 C2 . . . . -28.1(2) no
Zn1 N10 C11 C6 . . . 5_656 -81.5(1) no
Zn1 N10 C9 C2 . 5_656 5_656 5_656 -28.1(2) no
Zn1 N10 C11 C6 . 5_656 5_656 . -81.5(1) no
Zn1 N13 C12 C2 . . . . -24.8(2) no
Zn1 N13 C14 C15 . . . . -80.0(1) no
Zn1 N13 C12 C2 . 5_656 5_656 5_656 -24.8(2) no
Zn1 N13 C14 C15 . 5_656 5_656 . -80.0(1) no
N4 Zn1 N10 C9 . . . . -26.8(1) no
N4 Zn1 N10 C11 . . . . -151.4(1) no
N4 Zn1 N10 C9 . . 5_656 5_656 159.7(1) no
N4 Zn1 N10 C11 . . 5_656 5_656 35.1(1) no
N4 Zn1 N13 C12 . . . . 57.8(1) no
N4 Zn1 N13 C14 . . . . -67.0(1) no
N4 Zn1 N13 C12 . . 5_656 5_656 -116.5(1) no
N4 Zn1 N13 C14 . . 5_656 5_656 118.6(1) no
N4 C3 C2 C1 . . . . -164.0(1) no
N4 C3 C2 C9 . . . . -47.9(2) no
N4 C3 C2 C12 . . . . 79.9(2) no
N4 C5 C6 C7 . . . . -75.6(2) no
N4 C5 C6 C8 . . . . 164.7(2) no
N4 C5 C6 C11 . . . 5_656 43.3(2) no
N10 Zn1 N4 C3 . . . . 53.6(1) no
N10 Zn1 N4 C5 . . . . -71.0(1) no
N10 Zn1 N4 C3 . . 5_656 5_656 156.8(1) no
N10 Zn1 N4 C5 . . 5_656 5_656 32.2(1) no
N10 Zn1 N10 C9 . . 5_656 5_656 -112.8(1) no
N10 Zn1 N10 C11 . . 5_656 5_656 122.6(1) no
N10 Zn1 N13 C12 . . . . -30.9(1) no
N10 Zn1 N13 C14 . . . . -155.7(1) no
N10 Zn1 N13 C12 . . 5_656 5_656 108.2(2) no
N10 Zn1 N13 C14 . . 5_656 5_656 -16.7(3) no
N10 C9 C2 C1 . . . . -162.2(1) no
N10 C9 C2 C3 . . . . 81.7(2) no
N10 C9 C2 C12 . . . . -45.9(2) no
N10 C11 C6 C5 . . 5_656 5_656 44.6(2) no
N10 C11 C6 C7 . . 5_656 5_656 165.4(1) no
N10 C11 C6 C8 . . 5_656 5_656 -75.9(2) no
N13 Zn1 N4 C3 . . . . -32.7(1) no
N13 Zn1 N4 C5 . . . . -157.3(1) no
N13 Zn1 N4 C3 . . 5_656 5_656 -117.8(1) no
N13 Zn1 N4 C5 . . 5_656 5_656 117.64(9) no
N13 Zn1 N10 C9 . . . . 58.9(1) no
N13 Zn1 N10 C11 . . . . -65.7(1) no
N13 Zn1 N10 C9 . . 5_656 5_656 109.4(2) no
N13 Zn1 N10 C11 . . 5_656 5_656 -15.2(3) no
N13 Zn1 N13 C12 . . 5_656 5_656 158.7(1) no
N13 Zn1 N13 C14 . . 5_656 5_656 33.80(8) no
N13 C12 C2 C1 . . . . -164.9(1) no
N13 C12 C2 C3 . . . . -48.9(2) no
N13 C12 C2 C9 . . . . 79.0(2) no
N13 C14 C15 C14 . . . 5_656 44.31(9) no
N13 C14 C15 C16 . . . . -75.4(2) no
N13 C14 C15 C16 . . . 5_656 165.7(1) no
C2 C3 N4 C5 . . . . 100.0(2) no
C2 C9 N10 C11 . . . . 95.2(2) no
C2 C12 N13 C14 . . . . 98.0(2) no
C3 N4 C5 C6 . . . . 156.3(1) no
C6 C11 N10 C9 . 5_656 5_656 5_656 151.9(1) no
C12 N13 C14 C15 . . . . 154.2(1) no
#------------------------------------------------------------------------------

_iucr_refine_instruction_details_constraints 
;
#
# Punched on 04/11/11 at 16:53:47
#
#LIST     12                                                                    
BLOCK 
CONT SCALE 
CONT ZN   (    1 ,X'S,U'S)  UNTIL C    (   16 ) 
CONT H    (   11 ,X'S)  UNTIL H    (  301 ) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 04/11/11 at 16:53:47
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;




#===END

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ral1104
_database_code_depnum_ccdc_archive 'CCDC 1456585'
_audit_update_record             
;
2016-02-29 deposited with the CCDC.
2016-04-20 downloaded from the CCDC.
;
_audit_creation_date             11-10-24
_audit_creation_method           CRYSTALS_ver_14.11

_oxford_structure_analysis_title 'transform axes for std setting of sp gp'
_chemical_name_systematic        
;
1,5,5,9,13,13,20,20-octamethyl-3,7,11,15,18,
22-hexaazabicyclo[7.7.7]tricosanecadmium(II) nitrate dihydrate
;
_chemical_melting_point          ?

_cell_length_a                   18.6325(4)
_cell_length_b                   16.3963(3)
_cell_length_c                   10.5649(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3227.62(11)

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P n m a '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,z+1/2
x+1/2,-y+1/2,-z+1/2
x,-y+1/2,z
-x,y+1/2,-z
-x+1/2,-y,z+1/2
x+1/2,y,-z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cd -0.8075 1.2024 19.2214 0.5946 17.6444 6.9089 4.4610 24.7008 1.6029 87.4825
5.0694 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C25 H56 Cd1 N8 O7 
# Dc =      1.43 Fooo =   1504.00 Mu =      7.30 M =    346.58
# Found Formula = C25 H58 Cd1 N8 O8 
# Dc =      1.46 FOOO =   1504.00 Mu =      7.34 M =    355.59

_chemical_formula_sum            'C25 H58 Cd N8 O8'
_chemical_formula_moiety         'C25 H54 Cd N6 2+, (N O3 -)2, 2(H2 O)'
_chemical_compound_source        ' from U of Wollongong'
_chemical_formula_weight         711.18


_cell_measurement_reflns_used    44397
_cell_measurement_theta_min      3
_cell_measurement_theta_max      30
_cell_measurement_temperature    200

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.070
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_max          0.330

_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1504
_exptl_absorpt_coefficient_mu    0.734

# Sheldrick geometric approximatio 0.86 0.95 
# Absorption correction 
#axes transformed to match new cell

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.100
0 0 -1 0.110
0 1 0 0.150
0 -1 0 0.180
-1 0 0 0.030
1 0 0 0.040
0 -1 -1 0.160
0 1 1 0.130
-4 0 -1 0.046


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.849
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_process_details   
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
#_diffrn_reflns_av_R_equivalents   0.035

# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
#_diffrn_measurement_method       '\f & \w scans'
_diffrn_special_details          
;
CCD data collecting conditions-
phi and omega scans of width 1.5 deg at rate 135 sec/frame,
crystal-detector distance 40mm,
multiple scan sets so over 90 percent of data collected with 4-fold  
redundancy or more.
;

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;

_diffrn_standards_interval_time  ?
_diffrn_standards_interval_count ?
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      200
_diffrn_reflns_number            45358
_reflns_number_total             4850
_diffrn_reflns_av_R_equivalents  0.045
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 4850 
# Theoretical number of reflections is about 9458 


_diffrn_reflns_theta_min         2.915
_diffrn_reflns_theta_max         30.051
_diffrn_measured_fraction_theta_max 0.995

_diffrn_reflns_theta_full        30.051
_diffrn_measured_fraction_theta_full 0.995


_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_reflns_limit_h_min              0
_reflns_limit_h_max              26
_reflns_limit_k_min              0
_reflns_limit_k_max              23
_reflns_limit_l_min              0
_reflns_limit_l_max              14

_oxford_diffrn_Wilson_B_factor   1.84
_oxford_diffrn_Wilson_scale      28.80

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -0.72
_refine_diff_density_max         2.03


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
#_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         4850
_refine_ls_number_restraints     41
_refine_ls_number_parameters     257
_oxford_refine_ls_R_factor_ref   0.0430
_refine_ls_wR_factor_ref         0.0826
_refine_ls_goodness_of_fit_ref   1.0251
_refine_ls_shift/su_max          0.0451128
_refine_ls_shift/su_mean         0.0042741


# The values computed from all data 
_oxford_reflns_number_all        4850
_refine_ls_R_factor_all          0.0430
_refine_ls_wR_factor_all         0.0826

# The values computed with a 2 sigma cutoff - a la SHELX 
#_reflns_threshold_expression     I>2.0\s(I)
_reflns_number_gt                4089
_refine_ls_R_factor_gt           0.0332
_refine_ls_wR_factor_gt          0.0792

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    mixed # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.03P)² + 4.47P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_special_details          
;
H atoms attached to C were included at calculated positions.
Subsequent difference electron density maps showed peaks attributable to the 
H atoms of the amine groups
and the water molecule.
The H atoms were initially refined with soft restraints on the 
bond lengths and angles to regularise their geometry 
(C---H in the range 0.93--0.98 Å, 
N---H = 0.86 Å and
O---H = 0.82 Å) and with
Uiso(H) in the range 1.2-1.5 times Ueq of the parent atom. 
In the final refinement
 the coordinates of H atoms attached to N and O were refined
(with restraints for the water molecule) 
but H atoms attached to C ride on the atom to which they are 
respectively bonded.

The largest feature in the final difference electron density map
is a large peak (2.03 e⁻⁻/Α³) at (0.571, 0.250, 0.780)
which is 2.08 Α from Cd1 and is at the centre of a square face of the 
trigonal bipyramidal coordination sphere.
It equates approximately to an O atom with occupancy 0.12.
We can attach no chemical explanation to its existence.
The next largest features in the
final difference map 
are all less than 0.47 e⁻⁻/Α³ and are located randomly
through the structure.
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Cd1 Cd 0.667085(11) 0.2500 0.681115(19) 0.0227 1.0000 Uani S T . . . .
O51 O 0.5965(3) 0.4949(4) 0.1419(4) 0.0719 0.533(7) Uani D U P . . .
O52 O 0.6343(3) 0.5517(3) 0.3117(5) 0.0653 0.533(7) Uani D U P . . .
O53 O 0.6088(4) 0.4266(6) 0.3115(9) 0.1057 0.533(7) Uani D U P . . .
O55 O 0.5433(3) 0.4499(4) 0.2019(5) 0.0859 0.467(7) Uani D U P . . .
O56 O 0.6137(5) 0.5504(5) 0.2267(10) 0.1392 0.467(7) Uani D U P . . .
O57 O 0.6352(4) 0.4347(6) 0.3167(8) 0.0738 0.467(7) Uani D U P . . .
O60 O 0.48237(13) 0.59374(15) 0.0587(2) 0.0645 1.0000 Uani D . . . . .
N4 N 0.75421(10) 0.34736(11) 0.60676(17) 0.0265 1.0000 Uani . . . . . .
N10 N 0.66319(10) 0.34686(11) 0.85102(16) 0.0251 1.0000 Uani . . . . . .
N16 N 0.58639(9) 0.34699(10) 0.58637(17) 0.0250 1.0000 Uani . . . . . .
N50 N 0.6128(4) 0.4916(5) 0.2558(6) 0.0455 0.533(7) Uani D U P . . .
N54 N 0.5977(4) 0.4791(5) 0.2509(7) 0.0463 0.467(7) Uani D U P . . .
C1 C 0.66668(15) 0.55162(14) 0.6792(2) 0.0401 1.0000 Uani . . . . . .
C2 C 0.66697(12) 0.45765(12) 0.6801(2) 0.0278 1.0000 Uani . . . . . .
C3 C 0.72473(12) 0.43067(13) 0.5858(2) 0.0305 1.0000 Uani . . . . . .
C5 C 0.80183(12) 0.32763(14) 0.4982(2) 0.0309 1.0000 Uani . . . . . .
C6 C 0.84646(16) 0.2500 0.5105(3) 0.0299 1.0000 Uani S T . . . .
C7 C 0.89890(19) 0.2500 0.3979(3) 0.0407 1.0000 Uani S T . . . .
C8 C 0.89038(19) 0.2500 0.6340(3) 0.0379 1.0000 Uani S T . . . .
C9 C 0.68462(13) 0.43150(13) 0.8165(2) 0.0304 1.0000 Uani . . . . . .
C11 C 0.69870(12) 0.32767(13) 0.97347(19) 0.0278 1.0000 Uani . . . . . .
C12 C 0.67383(16) 0.2500 1.0397(3) 0.0264 1.0000 Uani S T . . . .
C13 C 0.7108(2) 0.2500 1.1712(3) 0.0356 1.0000 Uani S T . . . .
C14 C 0.59288(17) 0.2500 1.0614(3) 0.0328 1.0000 Uani S T . . . .
C15 C 0.59159(12) 0.43120(13) 0.6396(2) 0.0295 1.0000 Uani . . . . . .
C17 C 0.50906(11) 0.32755(13) 0.5735(2) 0.0294 1.0000 Uani . . . . . .
C18 C 0.49082(16) 0.2500 0.5008(3) 0.0255 1.0000 Uani S T . . . .
C19 C 0.40872(17) 0.2500 0.4847(3) 0.0363 1.0000 Uani S T . . . .
C20 C 0.52529(19) 0.2500 0.3693(3) 0.0339 1.0000 Uani S T . . . .
H11 H 0.6314 0.5710 0.7368 0.0478 1.0000 Uiso R . . . . .
H12 H 0.7126 0.5712 0.7039 0.0478 1.0000 Uiso R . . . . .
H13 H 0.6559 0.5705 0.5964 0.0478 1.0000 Uiso R . . . . .
H31 H 0.7634 0.4684 0.5908 0.0367 1.0000 Uiso R . . . . .
H32 H 0.7044 0.4323 0.5034 0.0367 1.0000 Uiso R . . . . .
H41 H 0.7834(15) 0.3513(16) 0.672(2) 0.0324 1.0000 Uiso . . . . . .
H51 H 0.8340 0.3720 0.4871 0.0369 1.0000 Uiso R . . . . .
H52 H 0.7726 0.3222 0.4251 0.0369 1.0000 Uiso R . . . . .
H71 H 0.9284 0.2972 0.4016 0.0483 1.0000 Uiso R . . . . .
H72 H 0.8724 0.2500 0.3211 0.0483 1.0000 Uiso R . . . . .
H81 H 0.9218 0.2956 0.6347 0.0450 1.0000 Uiso R . . . . .
H82 H 0.8587 0.2500 0.7042 0.0450 1.0000 Uiso R . . . . .
H91 H 0.7350 0.4362 0.8278 0.0364 1.0000 Uiso R . . . . .
H92 H 0.6608 0.4679 0.8724 0.0364 1.0000 Uiso R . . . . .
H101 H 0.6196(15) 0.3485(16) 0.862(3) 0.0328 1.0000 Uiso . . . . . .
H111 H 0.7487 0.3226 0.9580 0.0337 1.0000 Uiso R . . . . .
H112 H 0.6904 0.3721 1.0292 0.0337 1.0000 Uiso R . . . . .
H131 H 0.6969 0.2972 1.2171 0.0422 1.0000 Uiso R . . . . .
H132 H 0.7614 0.2500 1.1600 0.0422 1.0000 Uiso R . . . . .
H141 H 0.5801 0.2954 1.1126 0.0391 1.0000 Uiso R . . . . .
H142 H 0.5689 0.2500 0.9823 0.0391 1.0000 Uiso R . . . . .
H151 H 0.5611 0.4343 0.7115 0.0353 1.0000 Uiso R . . . . .
H152 H 0.5753 0.4682 0.5767 0.0353 1.0000 Uiso R . . . . .
H161 H 0.6036(14) 0.3520(15) 0.511(2) 0.0303 1.0000 Uiso . . . . . .
H171 H 0.4896 0.3224 0.6563 0.0353 1.0000 Uiso R . . . . .
H172 H 0.4867 0.3720 0.5313 0.0353 1.0000 Uiso R . . . . .
H191 H 0.3945 0.2972 0.4389 0.0435 1.0000 Uiso R . . . . .
H192 H 0.3865 0.2500 0.5657 0.0435 1.0000 Uiso R . . . . .
H201 H 0.5085 0.2956 0.3224 0.0401 1.0000 Uiso R . . . . .
H202 H 0.5759 0.2500 0.3782 0.0401 1.0000 Uiso R . . . . .
H601 H 0.4681(19) 0.579(2) -0.019(2) 0.0770 1.0000 Uiso D . . . . .
H602 H 0.5125(17) 0.5560(17) 0.088(3) 0.0770 1.0000 Uiso D . . . . .


_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.28242(19)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cd1 . N4 . 2.4084(18) yes
Cd1 . N10 . 2.3978(17) yes
Cd1 . N16 . 2.4065(18) yes
O51 . N50 . 1.243(7) yes
O52 . N50 . 1.216(7) yes
O53 . N50 . 1.219(8) yes
O55 . N54 . 1.236(7) yes
O56 . N54 . 1.233(7) yes
O57 . N54 . 1.225(7) yes
O60 . H601 . 0.898(18) no
O60 . H602 . 0.890(18) no
N4 . C3 . 1.489(3) yes
N4 . C5 . 1.486(3) yes
N4 . H41 . 0.88(3) no
N10 . C9 . 1.490(3) yes
N10 . C11 . 1.487(3) yes
N10 . H101 . 0.82(3) no
N16 . C15 . 1.494(3) yes
N16 . C17 . 1.482(3) yes
N16 . H161 . 0.86(3) no
C1 . C2 . 1.541(3) yes
C1 . H11 . 0.950 no
C1 . H12 . 0.950 no
C1 . H13 . 0.950 no
C2 . C3 . 1.532(3) yes
C2 . C9 . 1.538(3) yes
C2 . C15 . 1.531(3) yes
C3 . H31 . 0.950 no
C3 . H32 . 0.950 no
C5 . C6 . 1.526(3) yes
C5 . H51 . 0.950 no
C5 . H52 . 0.950 no
C6 . C7 . 1.539(4) yes
C6 . C8 . 1.540(4) yes
C7 . H71 5_555 0.950 no
C7 . H71 . 0.950 no
C7 . H72 . 0.950 no
C8 . H81 5_555 0.950 no
C8 . H81 . 0.950 no
C8 . H82 . 0.949 no
C9 . H91 . 0.950 no
C9 . H92 . 0.950 no
C11 . C12 . 1.525(3) yes
C11 . H111 . 0.950 no
C11 . H112 . 0.950 no
C12 . C13 . 1.551(4) yes
C12 . C14 . 1.526(4) yes
C13 . H131 5_555 0.950 no
C13 . H131 . 0.950 no
C13 . H132 . 0.950 no
C14 . H141 5_555 0.950 no
C14 . H141 . 0.950 no
C14 . H142 . 0.948 no
C15 . H151 . 0.950 no
C15 . H152 . 0.950 no
C17 . C18 . 1.524(3) yes
C17 . H171 . 0.950 no
C17 . H172 . 0.950 no
C18 . C19 . 1.539(4) yes
C18 . C20 . 1.530(4) yes
C19 . H191 5_555 0.950 no
C19 . H191 . 0.950 no
C19 . H192 . 0.950 no
C20 . H201 5_555 0.950 no
C20 . H201 . 0.950 no
C20 . H202 . 0.948 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N4 5_555 Cd1 . N4 . 83.03(9) yes
N16 5_555 Cd1 . N4 . 136.34(6) yes
N10 5_555 Cd1 . N4 . 134.71(6) yes
N16 5_555 Cd1 . N10 . 136.90(6) yes
N10 5_555 Cd1 . N10 . 82.96(8) yes
N4 . Cd1 . N10 . 79.95(6) yes
N16 5_555 Cd1 . N16 . 82.72(8) yes
N4 . Cd1 . N16 . 81.22(6) yes
N10 . Cd1 . N16 . 81.65(6) yes
H601 . O60 . H602 . 108.3(17) no
Cd1 . N4 . C3 . 114.08(13) yes
Cd1 . N4 . C5 . 120.67(13) yes
C3 . N4 . C5 . 107.78(16) yes
Cd1 . N4 . H41 . 102.1(17) no
C3 . N4 . H41 . 106.1(17) no
C5 . N4 . H41 . 104.6(17) no
Cd1 . N10 . C9 . 115.19(12) yes
Cd1 . N10 . C11 . 119.85(13) yes
C9 . N10 . C11 . 106.92(16) yes
Cd1 . N10 . H101 . 99.1(19) no
C9 . N10 . H101 . 105.6(19) no
C11 . N10 . H101 . 108.8(19) no
Cd1 . N16 . C15 . 114.43(12) yes
Cd1 . N16 . C17 . 120.23(13) yes
C15 . N16 . C17 . 107.24(16) yes
Cd1 . N16 . H161 . 102.4(17) no
C15 . N16 . H161 . 103.6(17) no
C17 . N16 . H161 . 107.4(17) no
O51 . N50 . O53 . 119.3(7) yes
O51 . N50 . O52 . 121.0(7) yes
O53 . N50 . O52 . 119.6(7) yes
O55 . N54 . O56 . 118.6(8) yes
O55 . N54 . O57 . 118.4(8) yes
O56 . N54 . O57 . 123.0(9) yes
C2 . C1 . H11 . 109.5 no
C2 . C1 . H12 . 109.5 no
H11 . C1 . H12 . 109.5 no
C2 . C1 . H13 . 109.4 no
H11 . C1 . H13 . 109.5 no
H12 . C1 . H13 . 109.5 no
C1 . C2 . C3 . 106.69(18) yes
C1 . C2 . C9 . 106.57(18) yes
C3 . C2 . C9 . 112.23(18) yes
C1 . C2 . C15 . 106.16(19) yes
C3 . C2 . C15 . 112.38(18) yes
C9 . C2 . C15 . 112.27(18) yes
C2 . C3 . N4 . 115.30(17) yes
C2 . C3 . H31 . 108.0 no
N4 . C3 . H31 . 108.0 no
C2 . C3 . H32 . 108.0 no
N4 . C3 . H32 . 108.0 no
H31 . C3 . H32 . 109.5 no
N4 . C5 . C6 . 116.19(19) yes
N4 . C5 . H51 . 107.8 no
C6 . C5 . H51 . 107.8 no
N4 . C5 . H52 . 107.8 no
C6 . C5 . H52 . 107.7 no
H51 . C5 . H52 . 109.5 no
C5 . C6 . C5 5_555 113.1(3) yes
C5 . C6 . C7 . 106.27(16) yes
C5 5_555 C6 . C7 . 106.27(16) yes
C5 . C6 . C8 . 111.20(16) yes
C5 5_555 C6 . C8 . 111.20(16) yes
C7 . C6 . C8 . 108.5(3) yes
C6 . C7 . H71 5_555 109.6 no
C6 . C7 . H71 . 109.6 no
H71 5_555 C7 . H71 . 109.1 no
C6 . C7 . H72 . 109.3 no
H71 5_555 C7 . H72 . 109.6 no
H71 . C7 . H72 . 109.6 no
C6 . C8 . H81 5_555 109.6 no
C6 . C8 . H81 . 109.6 no
H81 5_555 C8 . H81 . 103.9 no
C6 . C8 . H82 . 109.3 no
H81 5_555 C8 . H82 . 112.2 no
H81 . C8 . H82 . 112.2 no
C2 . C9 . N10 . 115.58(17) yes
C2 . C9 . H91 . 107.9 no
N10 . C9 . H91 . 108.0 no
C2 . C9 . H92 . 107.9 no
N10 . C9 . H92 . 107.9 no
H91 . C9 . H92 . 109.5 no
N10 . C11 . C12 . 116.13(18) yes
N10 . C11 . H111 . 107.8 no
C12 . C11 . H111 . 107.7 no
N10 . C11 . H112 . 107.7 no
C12 . C11 . H112 . 107.9 no
H111 . C11 . H112 . 109.5 no
C11 . C12 . C11 5_555 113.3(2) yes
C11 . C12 . C13 . 106.00(16) yes
C11 5_555 C12 . C13 . 106.00(16) yes
C11 . C12 . C14 . 111.69(16) yes
C11 5_555 C12 . C14 . 111.69(16) yes
C13 . C12 . C14 . 107.7(3) yes
C12 . C13 . H131 5_555 109.6 no
C12 . C13 . H131 . 109.6 no
H131 5_555 C13 . H131 . 109.2 no
C12 . C13 . H132 . 109.2 no
H131 5_555 C13 . H132 . 109.6 no
H131 . C13 . H132 . 109.6 no
C12 . C14 . H141 5_555 109.5 no
C12 . C14 . H141 . 109.5 no
H141 5_555 C14 . H141 . 103.1 no
C12 . C14 . H142 . 109.5 no
H141 5_555 C14 . H142 . 112.6 no
H141 . C14 . H142 . 112.6 no
C2 . C15 . N16 . 115.25(17) yes
C2 . C15 . H151 . 108.1 no
N16 . C15 . H151 . 108.1 no
C2 . C15 . H152 . 108.0 no
N16 . C15 . H152 . 107.9 no
H151 . C15 . H152 . 109.5 no
N16 . C17 . C18 . 116.27(19) yes
N16 . C17 . H171 . 107.8 no
C18 . C17 . H171 . 107.7 no
N16 . C17 . H172 . 107.7 no
C18 . C17 . H172 . 107.8 no
H171 . C17 . H172 . 109.5 no
C17 5_555 C18 . C17 . 113.1(2) yes
C17 5_555 C18 . C19 . 106.11(16) yes
C17 . C18 . C19 . 106.11(16) yes
C17 5_555 C18 . C20 . 111.34(16) yes
C17 . C18 . C20 . 111.34(16) yes
C19 . C18 . C20 . 108.5(3) yes
C18 . C19 . H191 5_555 109.4 no
C18 . C19 . H191 . 109.4 no
H191 5_555 C19 . H191 . 109.1 no
C18 . C19 . H192 . 109.5 no
H191 5_555 C19 . H192 . 109.7 no
H191 . C19 . H192 . 109.7 no
C18 . C20 . H201 5_555 109.7 no
C18 . C20 . H201 . 109.7 no
H201 5_555 C20 . H201 . 103.8 no
C18 . C20 . H202 . 109.2 no
H201 5_555 C20 . H202 . 112.2 no
H201 . C20 . H202 . 112.2 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
N4 . H41 . O56 7_665 133(2) 0.88(3) 2.57(3) 3.236(3) yes
N10 . H101 . O60 2_666 153(3) 0.82(3) 2.28(3) 3.035(3) yes
N16 . H161 . O53 . 149(2) 0.86(3) 2.44(3) 3.211(3) yes
N16 . H161 . O57 . 153(2) 0.86(3) 2.53(3) 3.318(3) yes
O60 . H601 . O51 2_665 151(3) 0.898(18) 2.14(3) 2.960(3) yes
O60 . H601 . O55 2_665 169(4) 0.898(18) 2.00(2) 2.885(3) yes
O60 . H602 . O51 . 165(4) 0.890(18) 1.94(2) 2.815(3) yes
O60 . H602 . O55 . 155(3) 0.890(18) 2.19(2) 3.023(3) yes
O60 . H602 . O56 . 137(3) 0.890(18) 2.39(3) 3.105(3) yes


#------------------------------------------------------------------------------
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
O51 O60 2.815(6) . . no
O51 O60 2.960(6) . 2_665 no
O51 C3 3.597(6) . 7_664 no
O52 C9 3.386(6) . 7_664 no
O52 N4 3.427(6) . 7_664 no
O52 C17 3.539(6) . 2_666 no
O52 C3 3.561(6) . 7_664 no
O53 N16 3.21(1) . . no
O53 C20 3.343(9) . . no
O53 C15 3.48(1) . . no
O55 O60 2.885(6) . 2_665 no
O55 O60 3.023(7) . . no
O55 C15 3.595(6) . 2_666 no
O56 O60 3.11(1) . . no
O56 N4 3.236(9) . 7_664 no
O56 C3 3.37(1) . 7_664 no
O56 C8 3.417(9) . 7_664 no
O56 C5 3.51(1) . 7_664 no
O57 C3 3.297(9) . . no
O57 N16 3.319(9) . . no
O57 C15 3.507(9) . . no
O60 N10 3.036(3) . 2_666 no
O60 C14 3.184(3) . 6_656 no
O60 O60 3.379(5) . 2_665 no
O60 C9 3.405(3) . 2_666 no
O60 C15 3.497(3) . 2_666 no
O60 N54 3.503(8) . . no
O60 C8 3.580(3) . 7_664 no
C14 C20 3.488(4) . 1_556 no
#------------------------------------------------------------------------------
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Cd1 N4 C3 C2 . . . . 35.9(2) no
Cd1 N4 C5 C6 . . . . -55.4(2) no
Cd1 N4 C3 C2 . 5 5 5 -35.9(2) no
Cd1 N4 C5 C6 . 5 5 . 55.4(2) no
Cd1 N10 C9 C2 . . . . 31.8(2) no
Cd1 N10 C11 C12 . . . . -57.4(2) no
Cd1 N10 C9 C2 . 5 5 5 -31.8(2) no
Cd1 N10 C11 C12 . 5 5 . 57.4(2) no
Cd1 N16 C15 C2 . . . . 34.5(2) no
Cd1 N16 C17 C18 . . . . -56.7(2) no
Cd1 N16 C15 C2 . 5 5 5 -34.5(2) no
Cd1 N16 C17 C18 . 5 5 . 56.7(2) no
N4 Cd1 N4 C3 . . 5 5 -161.2(1) no
N4 Cd1 N4 C5 . . 5 5 -30.4(2) no
N4 Cd1 N10 C9 . . . . 25.5(1) no
N4 Cd1 N10 C11 . . . . -104.3(2) no
N4 Cd1 N10 C9 . . 5 5 -95.1(2) no
N4 Cd1 N10 C11 . . 5 5 34.7(2) no
N4 Cd1 N16 C15 . . . . -58.5(1) no
N4 Cd1 N16 C17 . . . . 171.6(2) no
N4 Cd1 N16 C15 . . 5 5 128.6(1) no
N4 Cd1 N16 C17 . . 5 5 -101.5(2) no
N4 C3 C2 C1 . . . . 157.0(2) no
N4 C3 C2 C9 . . . . 40.6(2) no
N4 C3 C2 C15 . . . . -87.1(2) no
N4 C5 C6 C5 . . . 5 72.3(3) no
N4 C5 C6 C7 . . . . -171.5(2) no
N4 C5 C6 C8 . . . . -53.6(3) no
N10 Cd1 N4 C3 . . . . -61.0(1) no
N10 Cd1 N4 C5 . . . . 168.2(2) no
N10 Cd1 N4 C3 . . 5 5 130.4(1) no
N10 Cd1 N4 C5 . . 5 5 -98.7(2) no
N10 Cd1 N10 C9 . . 5 5 -163.4(1) no
N10 Cd1 N10 C11 . . 5 5 -33.6(2) no
N10 Cd1 N16 C15 . . . . 22.6(1) no
N10 Cd1 N16 C17 . . . . -107.3(1) no
N10 Cd1 N16 C15 . . 5 5 -92.8(1) no
N10 Cd1 N16 C17 . . 5 5 37.1(2) no
N10 C9 C2 C1 . . . . 159.4(2) no
N10 C9 C2 C3 . . . . -84.2(2) no
N10 C9 C2 C15 . . . . 43.6(3) no
N10 C11 C12 C11 . . . 5 71.5(3) no
N10 C11 C12 C13 . . . . -172.6(2) no
N10 C11 C12 C14 . . . . -55.5(3) no
N16 Cd1 N4 C3 . . . . 22.0(1) no
N16 Cd1 N4 C5 . . . . -108.8(2) no
N16 Cd1 N4 C3 . . 5 5 -91.7(1) no
N16 Cd1 N4 C5 . . 5 5 39.1(2) no
N16 Cd1 N10 C9 . . . . -57.0(1) no
N16 Cd1 N10 C11 . . . . 173.2(2) no
N16 Cd1 N10 C9 . . 5 5 126.8(1) no
N16 Cd1 N10 C11 . . 5 5 -103.3(2) no
N16 Cd1 N16 C15 . . 5 5 -162.3(1) no
N16 Cd1 N16 C17 . . 5 5 -32.4(2) no
N16 C15 C2 C1 . . . . 157.5(2) no
N16 C15 C2 C3 . . . . 41.3(2) no
N16 C15 C2 C9 . . . . -86.4(2) no
N16 C17 C18 C17 . . . 5 71.8(3) no
N16 C17 C18 C19 . . . . -172.3(2) no
N16 C17 C18 C20 . . . . -54.4(3) no
C2 C3 N4 C5 . . . . 172.8(2) no
C2 C9 N10 C11 . . . . 167.7(2) no
C2 C15 N16 C17 . . . . 170.6(2) no
C3 N4 C5 C6 . . . . 171.1(2) no
C9 N10 C11 C12 . . . . 169.2(2) no
C15 N16 C17 C18 . . . . 170.3(2) no
#------------------------------------------------------------------------------



_iucr_refine_instruction_details_constraints 
;
#
# Punched on 24/10/11 at 11:57:18
#
#LIST     12                                                                    
BLOCK SCALE X'S, CD(1,U'S) 
CONT O(51,U'S,OCC) UNTIL O(57) 
CONT O(60,U'S) UNTIL N(16) 
CONT N(50,U'S) UNTIL N(54) 
CONT C(1,U'S) UNTIL  C(20) 
CONT H(41,X'S) H(101,X'S) H(161,X'S) 
CONT H(601,X'S) H(602,X'S) 
EQUIV O(51,OCC) UNTIL O(57) N(50,OCC) UNTIL N(54) 
WEIGHT -1 O(55,OCC) UNTIL O(57) N(54,OCC) 
RIDE C ( 1,X'S) H( 11,X'S) H( 12,X'S) H( 13,X'S) 
RIDE C ( 3,X'S) H( 31,X'S) H( 32,X'S) 
RIDE C ( 5,X'S) H( 51,X'S) H( 52,X'S) 
RIDE C ( 7,X,Z) H( 71,X,Z) H( 72,X,Z) 
RIDE C ( 8,X,Z) H( 81,X,Z) H( 82,X,Z) 
RIDE C ( 9,X'S) H( 91,X'S) H( 92,X'S) 
RIDE C ( 11,X'S) H( 111,X'S) H( 112,X'S) 
RIDE C ( 13,X,Z) H( 131,X,Z) H( 132,X,Z) 
RIDE C ( 14,X,Z) H( 141,X,Z) H( 142,X,Z) 
RIDE C ( 15,X'S) H( 151,X'S) H( 152,X'S) 
RIDE C ( 17,X'S) H( 171,X'S) H( 172,X'S) 
RIDE C ( 19,X,Z) H( 191,X,Z) H( 192,X,Z) 
RIDE C ( 20,X,Z) H( 201,X,Z) H( 202,X,Z) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 24/10/11 at 11:57:18
#
#LIST     16                                                                    
REM DIST 1.54, .02 = C(12) TO C(14) 
REM 
DIST 0.0, .01 = MEAN N(50) TO O(51), N(50) TO O(52), N(50) TO O(53) 
ANGLE 120. 2. = O(51) TO N(50) TO O(52), O(51) TO N(50) TO O(53) 
CONT            O(52) TO N(50) TO O(53) 
PLANAR N(50) O(51) UNTIL O(53) 
REM 
DIST 0.0, .01 = MEAN N(54) TO O(55), N(54) TO O(56), N(54) TO O(57) 
ANGLE 120. 2. = O(55) TO N(54) TO O(56), O(55) TO N(54) TO O(57) 
CONT            O(56) TO N(54) TO O(57) 
PLANAR N(54) O(55) UNTIL O(57) 
REM 
U(IJ) 0.0, .02 = N(50) TO N(54) 
VIBR 0.0, .01 = N(50) TO O(51), N(50) TO O(52), N(50) TO O(53) 
VIBR 0.0, .01 = N(54) TO O(55), N(54) TO O(56), N(54) TO O(57) 
VIBR 0.0, .01 = O(51) TO O(52), O(52) TO O(53), O(53) TO O(51) 
VIBR 0.0, .01 = O(55) TO O(56), O(56) TO O(57), O(57) TO O(55) 
REM 
DIST 0.85, .02 = O(60) TO H(601), O(60) TO H(602) 
ANGLE 110., 2. = H(601) TO O(60) TO H(602) 
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;




#===END

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ral1103a
_database_code_depnum_ccdc_archive 'CCDC 1456586'
_audit_update_record             
;
2016-02-29 deposited with the CCDC.
2016-04-20 downloaded from the CCDC.
;
_audit_creation_date             11-10-06
_audit_creation_method           CRYSTALS_ver_14.11

_oxford_structure_analysis_title 'transform axes for std setting of sp gp'
_chemical_name_systematic        
;
1,5,5,9,13,13,20,20-octamethyl-3,7,11,15,18,22-hexaazabicyclo[7.7.7]tricosanemercury(II) nitrate dihydrate
;
_chemical_melting_point          ?

_cell_length_a                   18.6126(3)
_cell_length_b                   16.4042(2)
_cell_length_c                   10.5731(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3228.23(9)

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n m a '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,z+1/2
x+1/2,-y+1/2,-z+1/2
x,-y+1/2,z
-x,y+1/2,-z
-x+1/2,-y,z+1/2
x+1/2,y,-z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Hg -2.3894 9.2266 20.6809 0.5450 19.0417 8.4484 21.6575 1.5729 5.9676 38.3246
12.6089 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C25 H54 Hg1 N8 O6 
# Dc =      1.57 Fooo =   1616.00 Mu =     48.17 M =    763.34 wrong
# Found Formula = C25 H54 Hg1 N8 O8 
# Dc =      1.64 FOOO =   1616.00 Mu =     48.25 M =    795.34
# Full Correct Formula = C25 H58 Hg1 N8 O8 
# Dc =      1.653 FOOO =   1632.00 Mu =     48.25? M =    799.38

_chemical_formula_sum            'C25 H58 Hg N8 O8'
_chemical_formula_moiety         'C25 H54 Hg N6 2+, (N O3 -)2, 2(H2 O)'
_chemical_compound_source        ' from U of Wollongong'
_chemical_formula_weight         799.38 #795.34


_cell_measurement_reflns_used    76950
_cell_measurement_theta_min      3
_cell_measurement_theta_max      30
_cell_measurement_temperature    200

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1632
_exptl_absorpt_coefficient_mu    4.825

# Sheldrick geometric approximatio 0.51 0.62 
# Absorption correction ; faces have been transformed to match solution

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 0 0.001
1 0 0 0.100
0 1 1 0.070
0 -1 -1 0.070
0 -1 1 0.050
0 1 -1 0.080
0 1 0 0.109
0 -1 0 0.093
3 -3 0 0.117
-3 -3 0 0.050
3 3 0 0.132
-3 3 0 0.065
1 0 1 0.095
-1 0 -1 0.060
1 0 -1 0.110
-1 0 1 0.043


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.517
_exptl_absorpt_correction_T_max  0.646
_exptl_absorpt_process_details   
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
#_diffrn_reflns_av_R_equivalents   0.032

# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
#_diffrn_measurement_method       '\f & \w scans'
_diffrn_special_details          
;
CCD data collecting conditions-
phi and omega scans of width 1.2 deg at rate 48 sec/frame,
crystal-detector distance 32mm,
multiple scan sets so over 90 percent of data collected with 4-fold  
redundancy or more.
;

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      200
_diffrn_reflns_number            52233
_reflns_number_total             4853
_diffrn_reflns_av_R_equivalents  0.047
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 4853 
# Theoretical number of reflections is about 9440 


_diffrn_reflns_theta_min         2.916
_diffrn_reflns_theta_max         30.028
_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        30.028
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_reflns_limit_h_min              0
_reflns_limit_h_max              26
_reflns_limit_k_min              0
_reflns_limit_k_max              23
_reflns_limit_l_min              0
_reflns_limit_l_max              14

_oxford_diffrn_Wilson_B_factor   1.82
_oxford_diffrn_Wilson_scale      34.29

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -1.26
_refine_diff_density_max         1.58


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         4853
_refine_ls_number_restraints     38
_refine_ls_number_parameters     251
_oxford_refine_ls_R_factor_ref   0.0387
_refine_ls_wR_factor_ref         0.0575
_refine_ls_goodness_of_fit_ref   0.9915
_refine_ls_shift/su_max          0.0061509
_refine_ls_shift/su_mean         0.0003737


# The values computed from all data 
_oxford_reflns_number_all        4853
_refine_ls_R_factor_all          0.0387
_refine_ls_wR_factor_all         0.0575

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                3984
_refine_ls_R_factor_gt           0.0263
_refine_ls_wR_factor_gt          0.0543

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    mixed # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.02P)² + 5.13P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_special_details          
;
The largest features in the
final difference electron density map are located 
on the y=0.25 plane.
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Hg1 Hg 0.666067(8) 0.2500 0.681619(12) 0.0229 1.0000 Uani S T . . . .
O51 O 0.5985(3) 0.4980(5) 0.1440(5) 0.0840 0.573(8) Uani D U P . . .
O52 O 0.6367(3) 0.5525(4) 0.3140(6) 0.0719 0.573(8) Uani D U P . . .
O53 O 0.6041(5) 0.4307(6) 0.3147(9) 0.1172 0.573(8) Uani D U P . . .
O55 O 0.5430(4) 0.4471(6) 0.2035(7) 0.0894 0.427(8) Uani D U P . . .
O56 O 0.6125(7) 0.5512(5) 0.2261(12) 0.1386 0.427(8) Uani D U P . . .
O57 O 0.6369(6) 0.4351(8) 0.3169(9) 0.0779 0.427(8) Uani D U P . . .
O60 O 0.48467(17) 0.5923(2) 0.0546(3) 0.0791 1.0000 Uani . . . . . .
N4 N 0.75438(13) 0.34895(14) 0.6075(2) 0.0263 1.0000 Uani . . . . . .
N10 N 0.66173(13) 0.34849(14) 0.8535(2) 0.0262 1.0000 Uani . . . . . .
N16 N 0.58464(12) 0.34861(13) 0.5852(2) 0.0248 1.0000 Uani . . . . . .
N50 N 0.6131(4) 0.4938(5) 0.2584(7) 0.0506 0.573(8) Uani D U P . . .
N54 N 0.5978(5) 0.4783(5) 0.2512(8) 0.0489 0.427(8) Uani D U P . . .
C1 C 0.6654(2) 0.55222(18) 0.6803(3) 0.0435 1.0000 Uani . . . . . .
C2 C 0.66575(16) 0.45828(16) 0.6810(2) 0.0284 1.0000 Uani . . . . . .
C3 C 0.72401(16) 0.43150(16) 0.5866(3) 0.0313 1.0000 Uani . . . . . .
C5 C 0.80089(16) 0.32793(19) 0.4986(2) 0.0311 1.0000 Uani . . . . . .
C6 C 0.8452(2) 0.2500 0.5111(4) 0.0296 1.0000 Uani S T . . . .
C7 C 0.8974(2) 0.2500 0.3982(4) 0.0419 1.0000 Uani S T . . . .
C8 C 0.8891(2) 0.2500 0.6335(4) 0.0383 1.0000 Uani S T . . . .
C9 C 0.68373(17) 0.43239(17) 0.8172(3) 0.0322 1.0000 Uani . . . . . .
C11 C 0.69748(15) 0.32786(17) 0.9747(2) 0.0286 1.0000 Uani . . . . . .
C12 C 0.6722(2) 0.2500 1.0400(4) 0.0267 1.0000 Uani S T . . . .
C13 C 0.7087(3) 0.2500 1.1713(4) 0.0356 1.0000 Uani S T . . . .
C14 C 0.5911(2) 0.2500 1.0605(4) 0.0355 1.0000 Uani S T . . . .
C15 C 0.59002(16) 0.43185(16) 0.6408(3) 0.0307 1.0000 Uani . . . . . .
C17 C 0.50747(15) 0.32802(17) 0.5745(3) 0.0297 1.0000 Uani . . . . . .
C18 C 0.4898(2) 0.2500 0.5006(3) 0.0262 1.0000 Uani S T . . . .
C19 C 0.4075(2) 0.2500 0.4847(4) 0.0371 1.0000 Uani S T . . . .
C20 C 0.5250(2) 0.2500 0.3708(4) 0.0311 1.0000 Uani S T . . . .
H11 H 0.6300 0.5715 0.7377 0.0523 1.0000 Uiso R . . . . .
H12 H 0.7113 0.5718 0.7054 0.0523 1.0000 Uiso R . . . . .
H13 H 0.6548 0.5712 0.5976 0.0523 1.0000 Uiso R . . . . .
H31 H 0.7623 0.4696 0.5913 0.0376 1.0000 Uiso R . . . . .
H32 H 0.7036 0.4327 0.5042 0.0376 1.0000 Uiso R . . . . .
H41 H 0.7835(18) 0.353(2) 0.673(3) 0.0324 1.0000 Uiso . . . . . .
H51 H 0.8333 0.3719 0.4858 0.0373 1.0000 Uiso R . . . . .
H52 H 0.7709 0.3222 0.4264 0.0373 1.0000 Uiso R . . . . .
H71 H 0.8708 0.2500 0.3215 0.0504 1.0000 Uiso R . . . . .
H72 H 0.9271 0.2971 0.4020 0.0504 1.0000 Uiso R . . . . .
H81 H 0.8576 0.2500 0.7040 0.0460 1.0000 Uiso R . . . . .
H82 H 0.9209 0.2953 0.6337 0.0460 1.0000 Uiso R . . . . .
H91 H 0.7343 0.4364 0.8278 0.0387 1.0000 Uiso R . . . . .
H92 H 0.6606 0.4694 0.8730 0.0387 1.0000 Uiso R . . . . .
H101 H 0.6181(18) 0.349(2) 0.862(3) 0.0328 1.0000 Uiso . . . . . .
H111 H 0.7475 0.3224 0.9585 0.0343 1.0000 Uiso R . . . . .
H112 H 0.6898 0.3719 1.0315 0.0343 1.0000 Uiso R . . . . .
H131 H 0.7594 0.2500 1.1610 0.0428 1.0000 Uiso R . . . . .
H132 H 0.6943 0.2971 1.2170 0.0428 1.0000 Uiso R . . . . .
H141 H 0.5674 0.2500 0.9811 0.0426 1.0000 Uiso R . . . . .
H142 H 0.5781 0.2951 1.1119 0.0426 1.0000 Uiso R . . . . .
H151 H 0.5600 0.4337 0.7133 0.0369 1.0000 Uiso R . . . . .
H152 H 0.5731 0.4697 0.5796 0.0369 1.0000 Uiso R . . . . .
H161 H 0.6012(17) 0.3519(19) 0.513(3) 0.0303 1.0000 Uiso . . . . . .
H171 H 0.4889 0.3220 0.6577 0.0356 1.0000 Uiso R . . . . .
H172 H 0.4840 0.3722 0.5337 0.0356 1.0000 Uiso R . . . . .
H191 H 0.3853 0.2500 0.5656 0.0446 1.0000 Uiso R . . . . .
H192 H 0.3932 0.2973 0.4394 0.0446 1.0000 Uiso R . . . . .
H201 H 0.5757 0.2500 0.3802 0.0373 1.0000 Uiso R . . . . .
H202 H 0.5083 0.2954 0.3235 0.0373 1.0000 Uiso R . . . . .


_refine_ls_extinction_method     ?
_oxford_refine_ls_scale          0.17886(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Hg1 . N16 5_555 2.440(2) yes
Hg1 . N4 5_555 2.439(2) yes
Hg1 . N10 5_555 2.433(2) yes
Hg1 . N4 . 2.439(2) yes
Hg1 . N10 . 2.433(2) yes
Hg1 . N16 . 2.440(2) yes
O51 . N50 . 1.242(7) yes
O52 . N50 . 1.210(7) yes
O52 . N54 . 1.564(12) yes
O53 . N50 . 1.207(8) yes
O55 . N54 . 1.248(8) yes
O56 . N54 . 1.254(8) yes
O57 . N54 . 1.230(8) yes
N4 . C3 . 1.484(3) yes
N4 . C5 . 1.482(3) yes
N4 . H41 . 0.88(3) no
N10 . C9 . 1.486(4) yes
N10 . C11 . 1.483(3) yes
N10 . H101 . 0.82(3) no
N16 . C15 . 1.490(3) yes
N16 . C17 . 1.480(3) yes
N16 . H161 . 0.82(3) no
C1 . C2 . 1.541(4) yes
C1 . H11 . 0.950 no
C1 . H12 . 0.950 no
C1 . H13 . 0.950 no
C2 . C3 . 1.538(4) yes
C2 . C9 . 1.539(4) yes
C2 . C15 . 1.535(4) yes
C3 . H31 . 0.950 no
C3 . H32 . 0.950 no
C5 . C6 . 1.528(4) yes
C5 . H51 . 0.950 no
C5 . H52 . 0.950 no
C6 . C7 . 1.539(5) yes
C6 . C8 . 1.530(5) yes
C7 . H72 5_555 0.950 no
C7 . H71 . 0.950 no
C7 . H72 . 0.950 no
C8 . H82 5_555 0.950 no
C8 . H81 . 0.948 no
C8 . H82 . 0.950 no
C9 . H91 . 0.950 no
C9 . H92 . 0.950 no
C11 . C12 . 1.526(3) yes
C11 . H111 . 0.950 no
C11 . H112 . 0.950 no
C12 . C13 . 1.546(5) yes
C12 . C14 . 1.526(5) yes
C13 . H132 5_555 0.950 no
C13 . H131 . 0.950 no
C13 . H132 . 0.950 no
C14 . H142 5_555 0.950 no
C14 . H141 . 0.948 no
C14 . H142 . 0.950 no
C15 . H151 . 0.950 no
C15 . H152 . 0.950 no
C17 . C18 . 1.535(3) yes
C17 . H171 . 0.950 no
C17 . H172 . 0.950 no
C18 . C19 . 1.542(5) yes
C18 . C20 . 1.521(5) yes
C19 . H192 5_555 0.950 no
C19 . H191 . 0.950 no
C19 . H192 . 0.950 no
C20 . H202 5_555 0.950 no
C20 . H201 . 0.948 no
C20 . H202 . 0.950 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N16 5_555 Hg1 . N4 5_555 80.97(8) yes
N16 5_555 Hg1 . N10 5_555 81.46(8) yes
N4 5_555 Hg1 . N10 5_555 79.66(8) yes
N16 5_555 Hg1 . N4 . 136.50(8) yes
N4 5_555 Hg1 . N4 . 83.43(11) yes
N10 5_555 Hg1 . N4 . 134.76(8) yes
N16 5_555 Hg1 . N10 . 137.04(8) yes
N4 5_555 Hg1 . N10 . 134.76(8) yes
N10 5_555 Hg1 . N10 . 83.21(11) yes
N4 . Hg1 . N10 . 79.66(8) yes
N16 5_555 Hg1 . N16 . 83.05(10) yes
N4 5_555 Hg1 . N16 . 136.50(8) yes
N10 5_555 Hg1 . N16 . 137.04(8) yes
N4 . Hg1 . N16 . 80.97(8) yes
N10 . Hg1 . N16 . 81.46(8) yes
Hg1 . N4 . C3 . 113.48(17) yes
Hg1 . N4 . C5 . 119.25(17) yes
C3 . N4 . C5 . 108.6(2) yes
Hg1 . N4 . H41 . 102(2) no
C3 . N4 . H41 . 106(2) no
C5 . N4 . H41 . 106(2) no
Hg1 . N10 . C9 . 114.38(16) yes
Hg1 . N10 . C11 . 118.62(17) yes
C9 . N10 . C11 . 108.1(2) yes
Hg1 . N10 . H101 . 97(2) no
C9 . N10 . H101 . 107(2) no
C11 . N10 . H101 . 111(2) no
Hg1 . N16 . C15 . 113.63(16) yes
Hg1 . N16 . C17 . 118.90(16) yes
C15 . N16 . C17 . 107.7(2) yes
Hg1 . N16 . H161 . 101(2) no
C15 . N16 . H161 . 106(2) no
C17 . N16 . H161 . 108(2) no
O51 . N50 . O52 . 120.6(8) yes
O51 . N50 . O53 . 119.9(8) yes
O52 . N50 . O53 . 119.6(8) yes
O56 . N54 . O55 . 119.0(9) yes
O56 . N54 . O57 . 122.6(10) yes
O55 . N54 . O57 . 118.4(9) yes
C2 . C1 . H11 . 109.5 no
C2 . C1 . H12 . 109.5 no
H11 . C1 . H12 . 109.5 no
C2 . C1 . H13 . 109.5 no
H11 . C1 . H13 . 109.5 no
H12 . C1 . H13 . 109.5 no
C1 . C2 . C3 . 106.6(2) yes
C1 . C2 . C9 . 106.3(2) yes
C3 . C2 . C9 . 112.0(2) yes
C1 . C2 . C15 . 106.1(2) yes
C3 . C2 . C15 . 112.8(2) yes
C9 . C2 . C15 . 112.4(2) yes
C2 . C3 . N4 . 115.6(2) yes
C2 . C3 . H31 . 107.9 no
N4 . C3 . H31 . 107.9 no
C2 . C3 . H32 . 107.9 no
N4 . C3 . H32 . 107.9 no
H31 . C3 . H32 . 109.5 no
N4 . C5 . C6 . 116.3(2) yes
N4 . C5 . H51 . 107.7 no
C6 . C5 . H51 . 107.7 no
N4 . C5 . H52 . 107.7 no
C6 . C5 . H52 . 107.7 no
H51 . C5 . H52 . 109.5 no
C5 . C6 . C5 5_555 113.6(3) yes
C5 . C6 . C7 . 105.9(2) yes
C5 5_555 C6 . C7 . 105.9(2) yes
C5 . C6 . C8 . 111.2(2) yes
C5 5_555 C6 . C8 . 111.2(2) yes
C7 . C6 . C8 . 108.6(3) yes
C6 . C7 . H72 5_555 109.5 no
C6 . C7 . H71 . 109.5 no
H72 5_555 C7 . H71 . 109.9 no
C6 . C7 . H72 . 109.5 no
H72 5_555 C7 . H72 . 108.7 no
H71 . C7 . H72 . 109.9 no
C6 . C8 . H82 5_555 109.5 no
C6 . C8 . H81 . 109.5 no
H82 5_555 C8 . H81 . 112.6 no
C6 . C8 . H82 . 109.5 no
H82 5_555 C8 . H82 . 103.1 no
H81 . C8 . H82 . 112.6 no
C2 . C9 . N10 . 115.9(2) yes
C2 . C9 . H91 . 107.8 no
N10 . C9 . H91 . 107.8 no
C2 . C9 . H92 . 107.8 no
N10 . C9 . H92 . 107.8 no
H91 . C9 . H92 . 109.5 no
N10 . C11 . C12 . 116.3(2) yes
N10 . C11 . H111 . 107.7 no
C12 . C11 . H111 . 107.8 no
N10 . C11 . H112 . 107.7 no
C12 . C11 . H112 . 107.7 no
H111 . C11 . H112 . 109.5 no
C11 . C12 . C11 5_555 113.7(3) yes
C11 . C12 . C13 . 105.7(2) yes
C11 5_555 C12 . C13 . 105.7(2) yes
C11 . C12 . C14 . 111.7(2) yes
C11 5_555 C12 . C14 . 111.7(2) yes
C13 . C12 . C14 . 107.9(3) yes
C12 . C13 . H132 5_555 109.5 no
C12 . C13 . H131 . 109.5 no
H132 5_555 C13 . H131 . 109.8 no
C12 . C13 . H132 . 109.5 no
H132 5_555 C13 . H132 . 108.8 no
H131 . C13 . H132 . 109.8 no
C12 . C14 . H142 5_555 109.5 no
C12 . C14 . H141 . 109.5 no
H142 5_555 C14 . H141 . 112.9 no
C12 . C14 . H142 . 109.5 no
H142 5_555 C14 . H142 . 102.4 no
H141 . C14 . H142 . 112.9 no
C2 . C15 . N16 . 115.5(2) yes
C2 . C15 . H151 . 108.0 no
N16 . C15 . H151 . 108.0 no
C2 . C15 . H152 . 108.0 no
N16 . C15 . H152 . 108.0 no
H151 . C15 . H152 . 109.5 no
N16 . C17 . C18 . 115.9(2) yes
N16 . C17 . H171 . 107.9 no
C18 . C17 . H171 . 107.9 no
N16 . C17 . H172 . 107.8 no
C18 . C17 . H172 . 107.8 no
H171 . C17 . H172 . 109.5 no
C17 5_555 C18 . C17 . 112.9(3) yes
C17 5_555 C18 . C19 . 105.5(2) yes
C17 . C18 . C19 . 105.5(2) yes
C17 5_555 C18 . C20 . 111.6(2) yes
C17 . C18 . C20 . 111.6(2) yes
C19 . C18 . C20 . 109.3(3) yes
C18 . C19 . H192 5_555 109.5 no
C18 . C19 . H191 . 109.5 no
H192 5_555 C19 . H191 . 109.4 no
C18 . C19 . H192 . 109.5 no
H192 5_555 C19 . H192 . 109.6 no
H191 . C19 . H192 . 109.4 no
C18 . C20 . H202 5_555 109.5 no
C18 . C20 . H201 . 109.5 no
H202 5_555 C20 . H201 . 112.4 no
C18 . C20 . H202 . 109.5 no
H202 5_555 C20 . H202 . 103.3 no
H201 . C20 . H202 . 112.4 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
N4 . H41 . O56 7_665 133(3) 0.88(3) 2.55(3) 3.224(4) yes
N10 . H101 . O60 2_666 151(3) 0.82(3) 2.31(3) 3.051(4) yes
N16 . H161 . O53 . 146(3) 0.82(3) 2.46(3) 3.181(4) yes
N16 . H161 . O57 . 151(3) 0.82(3) 2.57(3) 3.317(4) yes


#------------------------------------------------------------------------------
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
O51 O60 2.788(7) . . no
O51 O60 3.000(7) . 2_665 no
O51 C3 3.552(7) . 7_664 no
O52 C9 3.352(6) . 7_664 no
O52 N4 3.390(7) . 7_664 no
O52 C17 3.526(7) . 2_666 no
O52 C3 3.546(7) . 7_664 no
O53 N16 3.18(1) . . no
O53 C20 3.36(1) . . no
O53 C15 3.46(1) . . no
O55 O60 2.851(8) . 2_665 no
O55 O60 3.055(9) . . no
O55 C15 3.575(9) . 2_666 no
O56 O60 3.07(1) . . no
O56 N4 3.22(1) . 7_664 no
O56 C3 3.39(1) . 7_664 no
O56 C8 3.405(9) . 7_664 no
O56 C5 3.51(1) . 7_664 no
O57 C3 3.28(1) . . no
O57 N16 3.32(1) . . no
O57 C15 3.53(1) . . no
O60 N10 3.052(4) . 2_666 no
O60 C14 3.188(4) . 6_656 no
O60 O60 3.291(7) . 2_665 no
O60 C9 3.439(4) . 2_666 no
O60 N54 3.500(9) . . no
O60 C15 3.530(4) . 2_666 no
O60 C8 3.593(4) . 7_664 no
C14 C20 3.504(6) . 1_556 no
#------------------------------------------------------------------------------
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Hg1 N4 C3 C2 . . . . 36.4(3) no
Hg1 N4 C5 C6 . . . . -56.0(3) no
Hg1 N4 C3 C2 . 5 5 5 -36.4(3) no
Hg1 N4 C5 C6 . 5 5 . 56.0(3) no
Hg1 N10 C9 C2 . . . . 32.7(3) no
Hg1 N10 C11 C12 . . . . -57.7(3) no
Hg1 N10 C9 C2 . 5 5 5 -32.7(3) no
Hg1 N10 C11 C12 . 5 5 . 57.7(3) no
Hg1 N16 C15 C2 . . . . 35.7(3) no
Hg1 N16 C17 C18 . . . . -57.9(3) no
Hg1 N16 C15 C2 . 5 5 5 -35.7(3) no
Hg1 N16 C17 C18 . 5 5 . 57.9(3) no
N4 Hg1 N4 C3 . . 5 5 -161.0(1) no
N4 Hg1 N4 C5 . . 5 5 -31.1(2) no
N4 Hg1 N10 C9 . . . . 25.2(2) no
N4 Hg1 N10 C11 . . . . -104.3(2) no
N4 Hg1 N10 C9 . . 5 5 -95.0(2) no
N4 Hg1 N10 C11 . . 5 5 34.5(2) no
N4 Hg1 N16 C15 . . . . -59.0(2) no
N4 Hg1 N16 C17 . . . . 172.5(2) no
N4 Hg1 N16 C15 . . 5 5 129.4(2) no
N4 Hg1 N16 C17 . . 5 5 -102.1(2) no
N4 C3 C2 C1 . . . . 156.3(2) no
N4 C3 C2 C9 . . . . 40.4(3) no
N4 C3 C2 C15 . . . . -87.6(3) no
N4 C5 C6 C5 . . . 5 73.6(4) no
N4 C5 C6 C7 . . . . -170.5(2) no
N4 C5 C6 C8 . . . . -52.8(4) no
N10 Hg1 N4 C3 . . . . -61.1(2) no
N10 Hg1 N4 C5 . . . . 168.9(2) no
N10 Hg1 N4 C3 . . 5 5 130.6(2) no
N10 Hg1 N4 C5 . . 5 5 -99.4(2) no
N10 Hg1 N10 C9 . . 5 5 -163.2(2) no
N10 Hg1 N10 C11 . . 5 5 -33.7(2) no
N10 Hg1 N16 C15 . . . . 21.8(2) no
N10 Hg1 N16 C17 . . . . -106.7(2) no
N10 Hg1 N16 C15 . . 5 5 -92.1(2) no
N10 Hg1 N16 C17 . . 5 5 36.4(2) no
N10 C9 C2 C1 . . . . 158.5(3) no
N10 C9 C2 C3 . . . . -85.4(3) no
N10 C9 C2 C15 . . . . 42.8(3) no
N10 C11 C12 C11 . . . 57 73.1(4) no
N10 C11 C12 C13 . . . . -171.5(3) no
N10 C11 C12 C14 . . . . -54.4(4) no
N16 Hg1 N4 C3 . . . . 21.8(2) no
N16 Hg1 N4 C5 . . . . -108.2(2) no
N16 Hg1 N4 C3 . . 5 5 -91.6(2) no
N16 Hg1 N4 C5 . . 5 5 38.4(2) no
N16 Hg1 N10 C9 . . . . -57.1(2) no
N16 Hg1 N10 C11 . . . . 173.4(2) no
N16 Hg1 N10 C9 . . 5 5 127.2(2) no
N16 Hg1 N10 C11 . . 5 5 -103.3(2) no
N16 Hg1 N16 C15 . . 5 5 -161.6(1) no
N16 Hg1 N16 C17 . . 5 5 -33.1(2) no
N16 C15 C2 C1 . . . . 156.4(2) no
N16 C15 C2 C3 . . . . 40.1(3) no
N16 C15 C2 C9 . . . . -87.7(3) no
N16 C17 C18 C17 . . . 5 74.1(4) no
N16 C17 C18 C19 . . . . -171.0(2) no
N16 C17 C18 C20 . . . . -52.5(3) no
N50 O51 O55 N54 . . . . -3.7(7) no
N50 O51 O56 N54 . . . . -13.5(7) no
N50 O52 O56 N54 . . . . 8.5(6) no
N50 O53 O55 N54 . . . . 0.6(8) no
N50 O53 O57 N54 . . . . -9.3(7) no
N50 O55 O51 N54 . . . . 3.7(7) no
N50 O55 O53 N54 . . . . -0.6(8) no
N50 O56 O51 N54 . . . . 13.5(7) no
N50 O56 O52 N54 . . . . -8.5(6) no
N50 O57 O53 N54 . . . . 9.3(7) no
C2 C3 N4 C5 . . . . 171.5(2) no
C2 C9 N10 C11 . . . . 167.2(2) no
C2 C15 N16 C17 . . . . 169.7(2) no
C3 N4 C5 C6 . . . . 171.9(2) no
C9 N10 C11 C12 . . . . 169.9(2) no
C15 N16 C17 C18 . . . . 171.0(2) no
#------------------------------------------------------------------------------



_iucr_refine_instruction_details_constraints 
;
#
# Punched on 06/10/11 at 15:18:23
#
#LIST     12                                                                    
BLOCK SCALE X'S, HG(1,U'S) 
CONT O(51,U'S,OCC) UNTIL O(57) 
CONT O(60,U'S) UNTIL N(16) 
CONT N(50,U'S) UNTIL N(54) 
CONT C(1,U'S) UNTIL  C(20) 
CONT H(41,X'S) H(101,X'S) H(161,X'S) 
EQUIV O(51,OCC) UNTIL O(57) N(50,OCC) UNTIL N(54) 
WEIGHT -1 O(55,OCC) UNTIL O(57) N(54,OCC) 
RIDE C ( 1,X'S) H( 11,X'S) H( 12,X'S) H( 13,X'S) 
RIDE C ( 3,X'S) H( 31,X'S) H( 32,X'S) 
RIDE C ( 5,X'S) H( 51,X'S) H( 52,X'S) 
RIDE C ( 7,X,Z) H( 71,X,Z) H( 72,X,Z) 
RIDE C ( 8,X,Z) H( 81,X,Z) H( 82,X,Z) 
RIDE C ( 9,X'S) H( 91,X'S) H( 92,X'S) 
RIDE C ( 11,X'S) H( 111,X'S) H( 112,X'S) 
RIDE C ( 13,X,Z) H( 131,X,Z) H( 132,X,Z) 
RIDE C ( 14,X,Z) H( 141,X,Z) H( 142,X,Z) 
RIDE C ( 15,X'S) H( 151,X'S) H( 152,X'S) 
RIDE C ( 17,X'S) H( 171,X'S) H( 172,X'S) 
RIDE C ( 19,X,Z) H( 191,X,Z) H( 192,X,Z) 
RIDE C ( 20,X,Z) H( 201,X,Z) H( 202,X,Z) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 06/10/11 at 15:18:23
#
#LIST     16                                                                    
REM DIST 1.54, .02 = C(12) TO C(14) 
REM 
DIST 0.0, .01 = MEAN N(50) TO O(51), N(50) TO O(52), N(50) TO O(53) 
ANGLE 120. 2. = O(51) TO N(50) TO O(52), O(51) TO N(50) TO O(53) 
CONT            O(52) TO N(50) TO O(53) 
PLANAR N(50) O(51) UNTIL O(53) 
REM 
DIST 0.0, .01 = MEAN N(54) TO O(55), N(54) TO O(56), N(54) TO O(57) 
ANGLE 120. 2. = O(55) TO N(54) TO O(56), O(55) TO N(54) TO O(57) 
CONT            O(56) TO N(54) TO O(57) 
PLANAR N(54) O(55) UNTIL O(57) 
REM 
U(IJ) 0.0, .02 = N(50) TO N(54) 
VIBR 0.0, .01 = N(50) TO O(51), N(50) TO O(52), N(50) TO O(53) 
VIBR 0.0, .01 = N(54) TO O(55), N(54) TO O(56), N(54) TO O(57) 
VIBR 0.0, .01 = O(51) TO O(52), O(52) TO O(53), O(53) TO O(51) 
VIBR 0.0, .01 = O(55) TO O(56), O(56) TO O(57), O(57) TO O(55) 
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

# start Validation Reply Form 
_vrf_PLAT306_ral1103a            
; 
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O60      
RESPONSE: ... Yes, H atoms on water O60 have not been located, 
as mentioned in text at _refine_special_details.
Molecular weight, density, F(000) etc. are calculated 
with missing H's included.
;
# end Validation Reply Form



#===END

