# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2021

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

data_1_EtOH_210GPa
_database_code_depnum_ccdc_archive 'CCDC 2087891'
loop_
_audit_author_name
_audit_author_address
'Stephen Moggach'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2021-06-03 deposited with the CCDC.	2021-09-29 downloaded from the CCDC.
;
_audit_creation_date             2021-05-26
_audit_creation_method           CRYSTALS_ver_14.61_build_6999

_refine_special_details          
; 
23_ALERT_3_A Resolution (too) Low [sin(theta)/Lambda < 0.6]..       0.50 Ang-1
027_ALERT_3_A _diffrn_reflns_theta_full value (too) Low ......      15.63 Degree
029_ALERT_3_A _diffrn_measured_fraction_theta_full value Low .      0.697 Why?
910_ALERT_3_C Missing # of FCF Reflection(s) Below Theta(Min).          5 Note
911_ALERT_3_B Missing FCF Refl Between Thmin & STh/L=    0.501        403 Report
341_ALERT_3_B Low Bond Precision on  C-C Bonds ...............     0.0185 Ang.

These are caused by shading from the pressure cell.

084_ALERT_3_A High wR2 Value (i.e. > 0.25) ...................       0.49 Report
020_ALERT_3_B The Value of Rint is Greater Than 0.12 .........      0.183 Report
082_ALERT_2_B High R1 Value ..................................       0.18 Report

The sample has undergone a phase transition, which has caused twinning 
and breakup of the crystal.

922_ALERT_1_A wR2 in the CIF and FCF Differ by ...............     0.1161 Check
921_ALERT_1_B R1  in the CIF and FCF Differ by ...............     0.0258 Check

Reflections that overlap with W-gasket, or have poor correlations within 
2 degrees of the half-opening angle of the cell have been removed, 
causing the above alert. These were removed after data processing, 
as a number of strong reflections were measures well close to W-rings
that we wanted to include in the refinement.

430_ALERT_2_A Short Inter D...A Contact  N1       ..N1       .       2.51 Ang.
                                                   1-x,y,-z  =      5_655 Check

This is correct, and corresponds to the DABCO N...N distance.

201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) .......          7 Report
              O1        O2        N1        C1        C2                  etc.
076_ALERT_1_C Occupancy      0.500 Less Than 1.0 for Sp.pos  .           C5
076_ALERT_1_C Occupancy      0.500 Less Than 1.0 for Sp.pos  .           C8
906_ALERT_3_C Large K Value in the Analysis of Variance ......      4.670 Check
906_ALERT_3_C Large K Value in the Analysis of Variance ......      2.001 Check

These are all caused by disorder on the DABCO ligand.

992_ALERT_5_B Repd & Actual _reflns_number_gt Values Differ by         40 Check

This has been checked.  Reported numbers came from the twinabs output.

002_ALERT_2_G Number of Distance or Angle Restraints on AtSite         11 Note
003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...         11 Report
004_ALERT_5_G Polymeric Structure Found with Maximum Dimension          2 Info
042_ALERT_1_G Calc. and Reported Moiety Formula Strings Differ     Please Check
045_ALERT_1_G Calculated and Reported Z Differ by a Factor ...       2.00 Check
072_ALERT_2_G SHELXL First  Parameter in WGHT  Unusually Large       0.20 Report
093_ALERT_1_G No s.u.'s on H-positions, Refinement Reported as      mixed Check
199_ALERT_1_G Reported _cell_measurement_temperature ..... (K)        293 Check
200_ALERT_1_G Reported   _diffrn_ambient_temperature ..... (K)        293 Check
300_ALERT_4_G Atom Site Occupancy of C5         Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of C6         Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of C7         Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of C8         Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of H51        Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of H52        Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of H61        Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of H62        Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of H71        Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of H72        Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of H81        Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of H82        Constrained at        0.5 Check
301_ALERT_3_G Main Residue  Disorder ..............(Resd  1  )        22% Note
432_ALERT_2_G Short Inter X...Y Contact  N1       ..C8               2.44 Ang.
                                                   1-x,y,-z  =      5_655 Check
432_ALERT_2_G Short Inter X...Y Contact  N1       ..C6               2.44 Ang.
                                                   1-x,y,-z  =      5_655 Check
432_ALERT_2_G Short Inter X...Y Contact  N1       ..C6               2.44 Ang.
                                                  1-x,-y,-z  =      2_655 Check
432_ALERT_2_G Short Inter X...Y Contact  N1       ..C7               2.45 Ang.
                                                  1-x,-y,-z  =      2_655 Check
432_ALERT_2_G Short Inter X...Y Contact  N1       ..C7               2.45 Ang.
                                                   1-x,y,-z  =      5_655 Check
432_ALERT_2_G Short Inter X...Y Contact  N1       ..C5               2.46 Ang.
                                                   1-x,y,-z  =      5_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C5       ..C8               1.53 Ang.
                                                   1-x,y,-z  =      5_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C5       ..C7               2.10 Ang.
                                                  1-x,-y,-z  =      2_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C5       ..C7               2.10 Ang.
                                                   1-x,y,-z  =      5_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C5       ..C6               2.78 Ang.
                                                   1-x,y,-z  =      5_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C5       ..C6               2.78 Ang.
                                                  1-x,-y,-z  =      2_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C5       ..C5               3.19 Ang.
                                                   1-x,y,-z  =      5_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C6       ..C7               1.52 Ang.
                                                   1-x,y,-z  =      5_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C6       ..C6               1.87 Ang.
                                                   1-x,y,-z  =      5_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C6       ..C8               2.14 Ang.
                                                   1-x,y,-z  =      5_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C6       ..C7               2.92 Ang.
                                                  1-x,-y,-z  =      2_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C6       ..C6               3.15 Ang.
                                                  1-x,-y,-z  =      2_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C7       ..C7               2.00 Ang.
                                                   1-x,y,-z  =      5_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C7       ..C8               2.81 Ang.
                                                   1-x,y,-z  =      5_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C7       ..C7               3.16 Ang.
                                                  1-x,-y,-z  =      2_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C8       ..C8               3.14 Ang.
                                                   1-x,y,-z  =      5_655 Check
606_ALERT_4_G Solvent Accessible VOID(S) in Structure ........          ! Info
760_ALERT_1_G CIF Contains no Torsion Angles .................          ? Info
769_ALERT_4_G CIF Embedded explicitly supplied scattering data     Please Note
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      40.70 Deg.
              H82  -C7   -C8      6_555   1_555   1_555 ......     #   82 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      19.00 Deg.
              H82  -C7   -H71     6_555   1_555   1_555 ......     #   89 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       0.30 Deg.
              H82  -C7   -H81     6_555   1_555   1_555 ......     #  104 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      40.90 Deg.
              C8   -C7   -H81     1_555   1_555   1_555 ......     #  105 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      13.30 Deg.
              H72  -C7   -H61     1_555   1_555   1_555 ......     #  109 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      18.80 Deg.
              H71  -C7   -H81     1_555   1_555   1_555 ......     #  110 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.40 Deg.
              C7   -C8   -H71     6_555   1_555   6_555 ......     #  131 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      21.00 Deg.
              H81  -C8   -H71     6_555   1_555   6_555 ......     #  132 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.40 Deg.
              C7   -C8   -H71     1_555   1_555   1_555 ......     #  135 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       0.20 Deg.
              H81  -C8   -H82     6_555   1_555   1_555 ......     #  147 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      21.00 Deg.
              H82  -C8   -H71     6_555   1_555   1_555 ......     #  149 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       0.20 Deg.
              H82  -C8   -H81     6_555   1_555   1_555 ......     #  151 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      21.00 Deg.
              H71  -C8   -H81     1_555   1_555   1_555 ......     #  153 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      21.00 Deg.
              H71  -C8   -H82     6_555   1_555   1_555 ......     #  155 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       9.10 Deg.
              H72  -C6   -H61     1_555   1_555   1_555 ......     #  172 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      43.40 Deg.
              H82  -H71  -C8      6_555   1_555   1_555 ......     #  181 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       0.60 Deg.
              H82  -H71  -H81     6_555   1_555   1_555 ......     #  183 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      43.90 Deg.
              C8   -H71  -H81     1_555   1_555   1_555 ......     #  184 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      38.50 Deg.
              H71  -H81  -C7      1_555   1_555   1_555 ......     #  193 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      38.90 Deg.
              H71  -H82  -C7      6_555   1_555   6_555 ......     #  196 Check
795_ALERT_4_G C-Atom in CIF Coordinate List Out-of-Sequence ..         C2 Note
796_ALERT_4_G O-Atom in CIF Coordinate List Out-of-Sequence ..         O1 Note
860_ALERT_3_G Number of Least-Squares Restraints .............         86 Note
869_ALERT_4_G ALERTS Related to the Use of SQUEEZE Suppressed           ! Info
909_ALERT_3_G Percentage of I>2sig(I) Data at Theta(Max) Still        59% Note
913_ALERT_3_G Missing # of Very Strong Reflections in FCF ....          3 Note
956_ALERT_1_G Calculated (ThMax) and Actual (FCF) Hmax Differ           2 Units
957_ALERT_1_G Calculated (ThMax) and Actual (FCF) Kmax Differ           3 Units
961_ALERT_5_G Dataset Contains no Negative Intensities .......     Please Check
#===============================================================================
No action taken.
;

_cell_length_a                   14.176(3)
_cell_length_b                   16.361(3)
_cell_length_c                   9.6086(11)
_cell_angle_alpha                90
_cell_angle_beta                 92.168(10)
_cell_angle_gamma                90
_cell_volume                     2227.1(6)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/m 1 '
_symmetry_space_group_name_Hall  '-C 2y'
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
x,-y,z
-x+1/2,y+1/2,-z
x+1/2,-y+1/2,z

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            2

# Given Formula = C36 H18 N6 O12 Zn6 
# Dc =      1.67 Fooo =   1104.00 Mu =     32.41 M =   1118.85
# Found Formula = C22 H24 N2 O8 Zn2 
# Dc =      0.86 FOOO =    588.00 Mu =     11.03 M =    575.20

_chemical_formula_sum            'C45.8 H97.4 O19.9 N2 Zn2'
_chemical_formula_moiety         '(C22 H26 N2 O8 Zn2)n 11.9 (C2 O H6)'
_chemical_compound_source        .
_chemical_formula_weight         1125.44

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 -0.002 0.351 -0.116 1330 617 '11.9 (C2 O H6) '
_platon_squeeze_details          
;
see text for details
;

_cell_measurement_reflns_used    926
_cell_measurement_theta_min      3
_cell_measurement_theta_max      21
_cell_measurement_temperature    293

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.050
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.150

_exptl_crystal_density_diffrn    1.678
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1210.8
_exptl_absorpt_coefficient_mu    1.17

# Sheldrick geometric approximatio 0.85 0.95 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_T_max  0.95
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      293
_diffrn_ambient_pressure         2100000
_diffrn_reflns_number            2069
_diffrn_reflns_av_unetI/netI     0.239
_reflns_number_total             769
_diffrn_reflns_av_R_equivalents  0.183
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 769 
# Theoretical number of reflections is about 2341 


_diffrn_reflns_theta_min         2.889
_diffrn_reflns_theta_max         20.842
_diffrn_measured_fraction_theta_max 0.646

_diffrn_reflns_theta_full        15.631
_diffrn_measured_fraction_theta_full 0.697


_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       9
_reflns_limit_h_min              -12
_reflns_limit_h_max              11
_reflns_limit_k_min              0
_reflns_limit_k_max              13
_reflns_limit_l_min              0
_reflns_limit_l_max              9

_oxford_diffrn_Wilson_B_factor   0.27
_oxford_diffrn_Wilson_scale      35.56

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

_refine_diff_density_min         -1.83
_refine_diff_density_max         1.46


# 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_refine_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_restraints     86
_refine_ls_number_parameters     50
_refine_ls_number_reflns         747
_oxford_refine_ls_R_factor_ref   0.1922
_refine_ls_wR_factor_ref         0.3770
_refine_ls_goodness_of_fit_ref   1.2985
_refine_ls_shift/su_max          0.0033672
_refine_ls_shift/su_mean         0.0004517


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        796
_refine_ls_R_factor_all          0.2172
_refine_ls_wR_factor_all         0.4931

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                511
_refine_ls_R_factor_gt           0.1765
_refine_ls_wR_factor_gt          0.4515


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    mixed #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.20P)² + 0.00P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

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

# Replace last . with number of unfound hydrogen atoms attached 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 0.4950(3) 0.0000 0.3468(3) 0.0215 1.0000 Uani S T . . . .
O2 O 0.6016(7) 0.0846(8) 0.6262(12) 0.039(3) 1.0000 Uiso D U . . . .
O1 O 0.5996(7) 0.0871(8) 0.3895(12) 0.039(3) 1.0000 Uiso D U . . . .
N1 N 0.4939(7) 0.0000 0.1301(18) 0.016(4) 1.0000 Uiso DS U . . . .
C4 C 0.7228(8) 0.2180(9) 0.6283(17) 0.040(3) 1.0000 Uiso D U . . . .
C2 C 0.6891(7) 0.1834(7) 0.5043(16) 0.040(3) 1.0000 Uiso D U . . . .
C1 C 0.6235(7) 0.1111(7) 0.5087(12) 0.039(3) 1.0000 Uiso D U . . . .
C3 C 0.7164(8) 0.2159(9) 0.3807(18) 0.040(3) 1.0000 Uiso D U . . . .
C5 C 0.3983(13) 0.0000 0.065(3) 0.016(4) 0.5000 Uiso DS U . . . .
C7 C 0.5420(7) 0.0748(8) 0.086(2) 0.016(4) 0.5000 Uiso D U . . . .
C8 C 0.5936(12) -0.0000 0.093(3) 0.016(4) 0.5000 Uiso DS U . . . .
C6 C 0.4577(8) 0.0774(8) 0.072(2) 0.016(4) 0.5000 Uiso D U . . . .
H41 H 0.7060 0.1981 0.7158 0.0479 1.0000 Uiso R . . . . .
H31 H 0.6920 0.1912 0.2975 0.0479 1.0000 Uiso R . . . . .
H71 H 0.6056 0.0736 0.1244 0.0183 0.5000 Uiso R . . . . .
H72 H 0.5101 0.1220 0.1207 0.0183 0.5000 Uiso R . . . . .
H51 H 0.3651 0.0479 0.0934 0.0182 0.5000 Uiso R . . . . .
H52 H 0.3651 -0.0479 0.0934 0.0182 0.5000 Uiso R . . . . .
H61 H 0.4965 0.1218 0.1053 0.0189 0.5000 Uiso R . . . . .
H62 H 0.3943 0.0859 0.1009 0.0189 0.5000 Uiso R . . . . .
H81 H 0.6237 0.0479 0.1310 0.0188 0.5000 Uiso . . . . . .
H82 H 0.6235 -0.0476 0.1310 0.0188 0.5000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.313(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 . Zn1 2_656 2.941(5) yes
Zn1 . O1 6_555 2.086(16) yes
Zn1 . O2 2_656 1.972(16) yes
Zn1 . O2 5_656 1.972(16) yes
Zn1 . O1 . 2.086(16) yes
Zn1 . N1 . 2.082(18) yes
O2 . C1 . 1.260(9) yes
O1 . C1 . 1.245(9) yes
N1 . C7 6_555 1.470(9) yes
N1 . C6 6_555 1.469(9) yes
N1 . C5 . 1.471(9) yes
N1 . C7 . 1.470(9) yes
N1 . C8 . 1.471(9) yes
N1 . C6 . 1.469(9) yes
C4 . C3 4_656 1.387(7) yes
C4 . C2 . 1.388(9) yes
C4 . H41 . 0.940 no
C2 . C1 . 1.506(9) yes
C2 . C3 . 1.371(9) yes
C3 . H31 . 0.950 no
C5 . C8 2_655 1.5230(7) yes
C5 . C6 6_555 1.521(15) yes
C5 . H52 6_555 0.960 no
C5 . H51 6_555 0.960 no
C5 . C6 . 1.521(15) yes
C5 . H51 . 0.960 no
C5 . H52 . 0.960 no
C7 . C6 5_655 1.5230(7) yes
C7 . H82 6_555 1.296 no
C7 . C8 . 1.426(15) yes
C7 . C6 . 1.198(15) yes
C7 . H71 . 0.960 no
C7 . H72 . 0.960 no
C7 . H61 . 1.024 no
C7 . H81 . 1.297 no
C8 . H81 6_555 0.959 no
C8 . H82 6_555 0.954 no
C8 . H71 6_555 1.252 no
C8 . H71 . 1.252 no
C8 . H81 . 0.959 no
C8 . H82 . 0.954 no
C6 . H72 . 1.130 no
C6 . H61 . 0.959 no
C6 . H62 . 0.960 no
H71 . H82 6_555 0.498 no
H71 . H81 . 0.496 no
H51 . H62 . 0.749 no
H52 . H62 6_555 0.749 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
Zn1 2_656 Zn1 . O1 6_555 78.3(3) yes
Zn1 2_656 Zn1 . O2 2_656 82.9(4) yes
O1 6_555 Zn1 . O2 2_656 89.22(9) yes
Zn1 2_656 Zn1 . O2 5_656 82.9(4) yes
O1 6_555 Zn1 . O2 5_656 161.1(5) yes
O2 2_656 Zn1 . O2 5_656 89.2(2) yes
Zn1 2_656 Zn1 . O1 . 78.3(3) yes
O1 6_555 Zn1 . O1 . 86.2(2) yes
O2 2_656 Zn1 . O1 . 161.1(5) yes
O2 5_656 Zn1 . O1 . 89.22(9) yes
Zn1 2_656 Zn1 . N1 . 177.7(4) yes
O1 6_555 Zn1 . N1 . 100.1(4) yes
O2 2_656 Zn1 . N1 . 98.7(4) yes
O2 5_656 Zn1 . N1 . 98.7(4) yes
O1 . Zn1 . N1 . 100.1(4) yes
Zn1 2_656 O2 . C1 . 123.8(12) yes
Zn1 . O1 . C1 . 124.3(12) yes
C7 6_555 N1 . C6 6_555 48.1(6) yes
C7 6_555 N1 . Zn1 . 107.4(11) yes
C6 6_555 N1 . Zn1 . 111.7(11) yes
C7 6_555 N1 . C5 . 107.9(11) yes
C6 6_555 N1 . C5 . 62.3(6) yes
Zn1 . N1 . C5 . 113.5(14) yes
C7 6_555 N1 . C7 . 112.7(14) yes
C6 6_555 N1 . C7 . 140.2(15) yes
Zn1 . N1 . C7 . 107.4(11) yes
C5 . N1 . C7 . 107.9(11) yes
C7 6_555 N1 . C8 . 58.0(6) yes
C6 6_555 N1 . C8 . 103.4(10) yes
Zn1 . N1 . C8 . 105.8(14) yes
C5 . N1 . C8 . 140.7(15) yes
C7 . N1 . C8 . 58.0(6) yes
C7 6_555 N1 . C6 . 140.2(15) yes
C6 6_555 N1 . C6 . 119.2(15) yes
Zn1 . N1 . C6 . 111.7(11) yes
C5 . N1 . C6 . 62.3(6) yes
C7 . N1 . C6 . 48.1(6) yes
C8 . N1 . C6 . 103.4(10) yes
C3 4_656 C4 . C2 . 117.3(17) yes
C3 4_656 C4 . H41 . 120.3 no
C2 . C4 . H41 . 122.4 no
C4 . C2 . C1 . 119.3(15) yes
C4 . C2 . C3 . 119.1(14) yes
C1 . C2 . C3 . 121.6(15) yes
C2 . C1 . O2 . 117.9(13) yes
C2 . C1 . O1 . 111.7(13) yes
O2 . C1 . O1 . 130.4(16) yes
C4 4_656 C3 . C2 . 123.6(18) yes
C4 4_656 C3 . H31 . 119.1 no
C2 . C3 . H31 . 117.3 no
C8 2_655 C5 . C6 6_555 89.0(18) yes
C8 2_655 C5 . N1 . 109(2) yes
C6 6_555 C5 . N1 . 58.8(5) yes
C8 2_655 C5 . H52 6_555 109.9 no
C6 6_555 C5 . H52 6_555 160.7 no
N1 . C5 . H52 6_555 109.4 no
C8 2_655 C5 . H51 6_555 109.9 no
C6 6_555 C5 . H51 6_555 65.4 no
N1 . C5 . H51 6_555 109.4 no
H52 6_555 C5 . H51 6_555 109.5 no
C8 2_655 C5 . C6 . 89.0(18) yes
C6 6_555 C5 . C6 . 112.8(13) yes
N1 . C5 . C6 . 58.8(5) yes
H52 6_555 C5 . C6 . 65.4 no
H51 6_555 C5 . C6 . 160.7 no
C8 2_655 C5 . H51 . 109.9 no
C6 6_555 C5 . H51 . 160.7 no
N1 . C5 . H51 . 109.4 no
H51 6_555 C5 . H51 . 109.5 no
C8 2_655 C5 . H52 . 109.9 no
C6 6_555 C5 . H52 . 65.4 no
N1 . C5 . H52 . 109.4 no
H52 6_555 C5 . H52 . 109.5 no
C6 . C5 . H51 . 65.4 no
C6 . C5 . H52 . 160.7 no
H51 . C5 . H52 . 109.5 no
C6 5_655 C7 . N1 . 109.1(17) yes
C6 5_655 C7 . H82 6_555 107.7 no
N1 . C7 . H82 6_555 92.2 no
C6 5_655 C7 . C8 . 92.7(17) yes
N1 . C7 . C8 . 61.0(6) yes
H82 6_555 C7 . C8 . 40.7 no
C6 5_655 C7 . C6 . 86(2) yes
N1 . C7 . C6 . 65.9(6) yes
H82 6_555 C7 . C6 . 157.4 no
C8 . C7 . C6 . 122.9(14) yes
C6 5_655 C7 . H71 . 110.0 no
N1 . C7 . H71 . 108.3 no
H82 6_555 C7 . H71 . 19.0 no
C8 . C7 . H71 . 59.6 no
C6 . C7 . H71 . 164.3 no
C6 5_655 C7 . H72 . 109.9 no
N1 . C7 . H72 . 110.0 no
H82 6_555 C7 . H72 . 126.0 no
C8 . C7 . H72 . 157.4 no
C6 . C7 . H72 . 62.0 no
C6 5_655 C7 . H61 . 100.5 no
N1 . C7 . H61 . 105.8 no
H82 6_555 C7 . H61 . 139.3 no
C8 . C7 . H61 . 164.2 no
C6 . C7 . H61 . 50.4 no
C6 5_655 C7 . H81 . 107.6 no
N1 . C7 . H81 . 92.4 no
H82 6_555 C7 . H81 . 0.3 no
C8 . C7 . H81 . 40.9 no
C6 . C7 . H81 . 157.6 no
H71 . C7 . H72 . 109.5 no
H71 . C7 . H61 . 122.4 no
H72 . C7 . H61 . 13.3 no
H71 . C7 . H81 . 18.8 no
H72 . C7 . H81 . 125.9 no
H61 . C7 . H81 . 139.1 no
C5 2_655 C8 . N1 . 111(2) yes
C5 2_655 C8 . C7 . 90.8(18) yes
N1 . C8 . C7 . 61.0(6) yes
C5 2_655 C8 . C7 6_555 90.8(18) yes
N1 . C8 . C7 6_555 61.0(6) yes
C7 . C8 . C7 6_555 118.2(14) yes
C5 2_655 C8 . H81 6_555 109.3 no
N1 . C8 . H81 6_555 109.0 no
C7 . C8 . H81 6_555 159.8 no
C7 6_555 C8 . H81 6_555 62.3 no
C5 2_655 C8 . H82 6_555 109.5 no
N1 . C8 . H82 6_555 108.9 no
C7 . C8 . H82 6_555 62.3 no
C7 6_555 C8 . H82 6_555 159.7 no
H81 6_555 C8 . H82 6_555 109.6 no
C5 2_655 C8 . H71 6_555 103.1 no
N1 . C8 . H71 6_555 93.7 no
C7 . C8 . H71 6_555 154.3 no
C7 6_555 C8 . H71 6_555 41.4 no
H81 6_555 C8 . H71 6_555 21.0 no
C5 2_655 C8 . H71 . 103.1 no
N1 . C8 . H71 . 93.7 no
C7 . C8 . H71 . 41.4 no
C7 6_555 C8 . H71 . 154.3 no
H81 6_555 C8 . H71 . 129.8 no
C5 2_655 C8 . H81 . 109.3 no
N1 . C8 . H81 . 109.0 no
C7 . C8 . H81 . 62.3 no
C7 6_555 C8 . H81 . 159.8 no
H81 6_555 C8 . H81 . 109.7 no
C5 2_655 C8 . H82 . 109.5 no
N1 . C8 . H82 . 108.9 no
C7 . C8 . H82 . 159.7 no
C7 6_555 C8 . H82 . 62.3 no
H81 6_555 C8 . H82 . 0.2 no
H82 6_555 C8 . H71 6_555 129.7 no
H82 6_555 C8 . H71 . 21.0 no
H71 6_555 C8 . H71 . 148.3 no
H82 6_555 C8 . H81 . 0.2 no
H71 6_555 C8 . H81 . 129.8 no
H71 . C8 . H81 . 21.0 no
H82 6_555 C8 . H82 . 109.6 no
H71 6_555 C8 . H82 . 21.0 no
H71 . C8 . H82 . 129.7 no
H81 . C8 . H82 . 109.6 no
C7 5_655 C6 . C5 . 87.3(16) yes
C7 5_655 C6 . N1 . 109.9(16) yes
C5 . C6 . N1 . 58.9(5) yes
C7 5_655 C6 . C7 . 94(2) yes
C5 . C6 . C7 . 121.5(12) yes
N1 . C6 . C7 . 66.0(6) yes
C7 5_655 C6 . H72 . 113.9 no
C5 . C6 . H72 . 155.6 no
N1 . C6 . H72 . 100.7 no
C7 . C6 . H72 . 48.6 no
C7 5_655 C6 . H61 . 109.4 no
C5 . C6 . H61 . 162.9 no
N1 . C6 . H61 . 109.8 no
C7 . C6 . H61 . 55.3 no
H72 . C6 . H61 . 9.1 no
C7 5_655 C6 . H62 . 109.3 no
C5 . C6 . H62 . 67.1 no
N1 . C6 . H62 . 109.4 no
C7 . C6 . H62 . 155.7 no
H72 . C6 . H62 . 113.3 no
H61 . C6 . H62 . 109.0 no
C7 . H71 . H82 6_555 122.1 no
C7 . H71 . C8 . 79.0 no
H82 6_555 H71 . C8 . 43.4 no
C7 . H71 . H81 . 122.7 no
H82 6_555 H71 . H81 . 0.6 no
C8 . H71 . H81 . 43.9 no
C6 . H72 . C7 . 69.4 no
C5 . H51 . H62 . 115.4 no
H62 6_555 H52 . C5 . 115.4 no
C7 . H61 . C6 . 74.3 no
H51 . H62 . C6 . 111.9 no
H52 6_555 H62 . C6 . 111.9 no
C8 . H81 . H71 . 115.1 no
C8 . H81 . C7 . 76.8 no
H71 . H81 . C7 . 38.5 no
C8 . H82 . H71 6_555 115.6 no
C8 . H82 . C7 6_555 77.0 no
H71 6_555 H82 . C7 6_555 38.9 no



# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
0 2 1 x .
1 5 1 x .
-3 1 1 x .
-4 2 1 x .
-2 2 2 x .
5 5 2 x .
-3 3 2 x .
-7 5 6 x .
4 2 0 x .
-2 6 1 x .
-2 8 2 x .
6 6 2 x .
-4 4 7 x .
-4 4 2 x .
6 10 3 x .
-7 5 1 x .
3 3 0 x .
2 0 2 x .
2 2 3 x .
1 3 0 x .
3 7 0 x .
-1 3 3 x .
-2 0 3 x .
1 1 3 x .
-2 0 1 x .
4 0 2 x .
8 0 6 x .
0 6 3 x .
-8 10 3 x .
1 5 3 x .
1 7 3 x .
7 3 0 x .
-6 6 1 x .
0 0 5 x .
9 5 1 x .
-8 4 1 x .
11 3 5 x .
7 5 0 x .
5 3 0 x .
-2 0 2 x .
5 1 1 x .
3 9 7 x .
2 8 3 x .
-7 7 1 x .
4 0 3 x .
-6 2 1 x .
0 0 6 x .
7 1 6 x .
3 1 4 x .
# looking for ARCHIVE-HKL.CIF 

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

data_1_EtOH_031GPa
_database_code_depnum_ccdc_archive 'CCDC 2087892'
loop_
_audit_author_name
_audit_author_address
'Stephen Moggach'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2021-06-03 deposited with the CCDC.	2021-09-29 downloaded from the CCDC.
;
_audit_creation_date             2021-05-26
_audit_creation_method           CRYSTALS_ver_14.61_build_6999

_refine_special_details          
; 
029_ALERT_3_A _diffrn_measured_fraction_theta_full value Low .      0.581 Why?
911_ALERT_3_B Missing FCF Refl Between Thmin & STh/L=    0.595        255 Report
341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............       0.01 Ang.

These are caused by shading from the pressure cell.

430_ALERT_2_B Short Inter D...A Contact  N1       ..N1       .       2.62 Ang.
                                                     y,x,-z  =     16_555 Check

This is correct, and corresponds to the DABCO N...N distance.

921_ALERT_1_C R1  in the CIF and FCF Differ by ...............     0.0036 Check
922_ALERT_1_B wR2 in the CIF and FCF Differ by ...............     0.0129 Check

Reflections that overlap with W-gasket, or have poor correlations within 
2 degrees of the half-opening angle of the cell have been removed, 
causing the above alert. These were removed after data processing, 
as a number of strong reflections were measures well close to W-rings
that we wanted to include in the refinement.

#===============================================================================
002_ALERT_2_G Number of Distance or Angle Restraints on AtSite          7 Note
003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...          7 Report
004_ALERT_5_G Polymeric Structure Found with Maximum Dimension          3 Info
042_ALERT_1_G Calc. and Reported Moiety Formula Strings Differ     Please Check
045_ALERT_1_G Calculated and Reported Z Differ by a Factor ...       2.00 Check
083_ALERT_2_G SHELXL Second Parameter in WGHT  Unusually Large      23.55 Why ?
300_ALERT_4_G Atom Site Occupancy of C4         Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of C5         Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H13        Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H51        Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H52        Constrained at      0.375 Check
301_ALERT_3_G Main Residue  Disorder ..............(Resd  1  )        22% Note
432_ALERT_2_G Short Inter X...Y Contact  N1       ..C5               2.47 Ang.
                                                   x,1-y,-z  =     10_565 Check
432_ALERT_2_G Short Inter X...Y Contact  N1       ..C5               2.47 Ang.
                                                 1-y,1-x,-z  =     12_665 Check
432_ALERT_2_G Short Inter X...Y Contact  N1       ..C4               2.50 Ang.
                                                   y,1-x,-z  =      4_565 Check
432_ALERT_2_G Short Inter X...Y Contact  N1       ..C4               2.50 Ang.
                                                 1-y,1-x,-z  =     12_665 Check
432_ALERT_2_G Short Inter X...Y Contact  C2       ..C3               2.41 Ang.
                                                   -x,y,1-z  =     14_556 Check
432_ALERT_2_G Short Inter X...Y Contact  C3       ..C3               2.76 Ang.
                                                   -x,y,1-z  =     14_556 Check
432_ALERT_2_G Short Inter X...Y Contact  C4       ..C4               2.49 Ang.
                                                   y,1-x,-z  =      4_565 Check
432_ALERT_2_G Short Inter X...Y Contact  C4       ..C5               2.95 Ang.
                                                   x,1-y,-z  =     10_565 Check
432_ALERT_2_G Short Inter X...Y Contact  C4       ..C5               2.95 Ang.
                                                 1-y,1-x,-z  =     12_665 Check
432_ALERT_2_G Short Inter X...Y Contact  C4       ..C4               3.16 Ang.
                                                 1-y,1-x,-z  =     12_665 Check
432_ALERT_2_G Short Inter X...Y Contact  C5       ..C5               2.44 Ang.
                                                 1-y,1-x,-z  =     12_665 Check
432_ALERT_2_G Short Inter X...Y Contact  C5       ..C5               3.09 Ang.
                                                   x,1-y,-z  =     10_565 Check
605_ALERT_4_G Largest Solvent Accessible VOID in the Structure        722 A**3
760_ALERT_1_G CIF Contains no Torsion Angles .................          ? Info
769_ALERT_4_G CIF Embedded explicitly supplied scattering data     Please Note
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       0.20 Deg.
              H52  -C4   -H51    11_555   1_555   7_565 ......     #   25 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       9.30 Deg.
              H13  -C4   -H51    11_555   1_555   9_655 ......     #   27 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       9.20 Deg.
              H52  -C4   -H13    11_555   1_555   1_555 ......     #   37 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       9.30 Deg.
              H51  -C4   -H13     7_565   1_555   1_555 ......     #   38 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       9.20 Deg.
              H13  -C4   -H52    11_555   1_555   1_555 ......     #   41 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       0.20 Deg.
              H51  -C4   -H52     9_655   1_555   1_555 ......     #   44 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       0.10 Deg.
              H52  -C5   -H51     9_655   1_555   1_555 ......     #   56 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       0.10 Deg.
              H51  -C5   -H52     9_655   1_555   1_555 ......     #   59 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.66 Deg.
              C4   -N1   -C5      7_565   1_555  11_555 ......     #   70 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.66 Deg.
              C4   -N1   -C5      1_555   1_555  11_555 ......     #   72 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.66 Deg.
              C4   -N1   -C5      3_655   1_555   1_555 ......     #   75 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.66 Deg.
              C4   -N1   -C5      1_555   1_555   1_555 ......     #   76 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.66 Deg.
              C4   -N1   -C5      5_665   1_555   3_655 ......     #   78 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.66 Deg.
              C4   -N1   -C5      3_655   1_555   3_655 ......     #   80 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.66 Deg.
              C4   -N1   -C5      5_665   1_555   5_665 ......     #   83 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.66 Deg.
              C4   -N1   -C5      7_565   1_555   5_665 ......     #   84 Check
860_ALERT_3_G Number of Least-Squares Restraints .............         78 Note
869_ALERT_4_G ALERTS Related to the Use of SQUEEZE Suppressed           ! Info
909_ALERT_3_G Percentage of I>2sig(I) Data at Theta(Max) Still       100% Note
910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min).          3 Note
913_ALERT_3_G Missing # of Very Strong Reflections in FCF ....          2 Note
960_ALERT_3_G Number of Intensities with I  <   - 2*sig(I) ...          4 Check
992_ALERT_5_G Repd & Actual _reflns_number_gt Values Differ by          4 Check
#=============================================================================== 

No action taken.
;

_cell_length_a                   10.9805(16)
_cell_length_b                   10.9805(16)
_cell_length_c                   9.7220(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1172.2(4)

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P 4/m m m '
_symmetry_space_group_name_Hall  '-P 4 2'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-y,x,z
y,-x,-z
-x,-y,z
x,y,-z
y,-x,z
-y,x,-z
-x,y,z
x,-y,-z
y,x,z
-y,-x,-z
x,-y,z
-x,y,-z
-y,-x,z
y,x,-z

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            1

# Given Formula = C22 H20 N2 O8 Zn2 
# Dc =      0.81 Fooo =    290.00 Mu =     10.48 M =    571.17
# Found Formula = C22 H26 N2 O8 Zn2 
# Dc =      0.82 FOOO =    296.00 Mu =     10.48 M =    577.22

_chemical_formula_sum            'C37.6 H72.8 O15.8 N2 Zn2'
_chemical_formula_moiety         '(C22 H26 N2 O8 Zn2)n 7.8 (C2 O H6)'
_chemical_compound_source        .
_chemical_formula_weight         936.56

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 -0.002 -0.002 -0.020 719 202 '7.8 (C2 O H6)'
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
see text for details
;

_cell_measurement_reflns_used    3660
_cell_measurement_theta_min      3
_cell_measurement_theta_max      25
_cell_measurement_temperature    298

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.050
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.150

_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             498.8
_exptl_absorpt_coefficient_mu    1.09

# Sheldrick geometric approximatio 0.85 0.95 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_T_max  0.95
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      298
_diffrn_ambient_pressure         310000
_diffrn_reflns_number            4042
_diffrn_reflns_av_unetI/netI     0.064
_reflns_number_total             386
_diffrn_reflns_av_R_equivalents  0.048
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 386 
# Theoretical number of reflections is about 1036 


_diffrn_reflns_theta_min         2.798
_diffrn_reflns_theta_max         25.031
_diffrn_measured_fraction_theta_max 0.581

_diffrn_reflns_theta_full        25.031
_diffrn_measured_fraction_theta_full 0.581


_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_reflns_limit_h_min              0
_reflns_limit_h_max              5
_reflns_limit_k_min              0
_reflns_limit_k_max              11
_reflns_limit_l_min              0
_reflns_limit_l_max              11

_oxford_diffrn_Wilson_B_factor   0.24
_oxford_diffrn_Wilson_scale      37.55

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

_refine_diff_density_min         -1.17
_refine_diff_density_max         1.89


# 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_refine_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_restraints     78
_refine_ls_number_parameters     31
_refine_ls_number_reflns         379
_oxford_refine_ls_R_factor_ref   0.0938
_refine_ls_wR_factor_ref         0.1895
_refine_ls_goodness_of_fit_ref   1.0161
_refine_ls_shift/su_max          0.0091720
_refine_ls_shift/su_mean         0.0003097


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        386
_refine_ls_R_factor_all          0.0976
_refine_ls_wR_factor_all         0.2024

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                333
_refine_ls_R_factor_gt           0.0762
_refine_ls_wR_factor_gt          0.1709


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.00P)² +23.55P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

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

# Replace last . with number of unfound hydrogen atoms attached 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 0.5000 0.3469(2) 0.0247 1.0000 Uani S T . . . .
C1 C 0.2638(10) 0.5000 0.5000 0.0305 1.0000 Uani DS TU . . . .
C2 C 0.1273(10) 0.5000 0.5000 0.0300 1.0000 Uani DS TU . . . .
C3 C 0.0633(4) 0.5000 0.3777(8) 0.0513 1.0000 Uani DS TU . . . .
C4 C 0.4115(6) 0.4115(6) 0.0800(5) 0.0246 0.3750 Uani DS U . . . .
C5 C 0.5000 0.3778(9) 0.0787(5) 0.0244 0.3750 Uani DS U . . . .
N1 N 0.5000 0.5000 0.1350 0.0236 1.0000 Uani D U . . . .
O1 O 0.3177(7) 0.5000 0.3853(6) 0.0383 1.0000 Uani DS TU . . . .
H13 H 0.3304 0.4392 0.1006 0.0468 0.3750 Uiso R . . . . .
H32 H 0.1059 0.5000 0.2926 0.0597 1.0000 Uiso RS . . . . .
H51 H 0.5715 0.3359 0.1104 0.0293 0.3750 Uiso R . . . . .
H52 H 0.4288 0.3359 0.1104 0.0293 0.3750 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.2422(9)
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 . Zn1 2_666 2.977(4) yes
Zn1 . O1 3_655 2.036(8) yes
Zn1 . O1 5_665 2.036(8) yes
Zn1 . O1 7_565 2.036(8) yes
Zn1 . O1 . 2.036(8) yes
C1 . O1 6_556 1.262(6) yes
C1 . C2 . 1.499(8) yes
C1 . O1 . 1.262(6) yes
C2 . C3 6_556 1.381(7) yes
C2 . C3 . 1.381(7) yes
C3 . C3 5_565 1.390(9) yes
C3 . H32 . 0.950 no
C4 . C4 6_555 1.556(9) yes
C4 . H13 11_555 0.962 no
C4 . H52 11_555 0.901 no
C4 . H51 7_565 0.901 no
C4 . H51 9_655 0.901 no
C4 . N1 . 1.475(9) yes
C4 . H13 . 0.962 no
C4 . H52 . 0.901 no
C5 . C5 6_555 1.529(9) yes
C5 . H51 9_655 0.961 no
C5 . H52 9_655 0.959 no
C5 . N1 . 1.449(9) yes
C5 . H51 . 0.961 no
C5 . H52 . 0.959 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
Zn1 2_666 Zn1 . O1 3_655 79.44(18) yes
Zn1 2_666 Zn1 . O1 5_665 79.44(18) yes
O1 3_655 Zn1 . O1 5_665 88.07(7) yes
Zn1 2_666 Zn1 . O1 7_565 79.44(18) yes
O1 3_655 Zn1 . O1 7_565 158.9(4) yes
O1 5_665 Zn1 . O1 7_565 88.07(7) yes
Zn1 2_666 Zn1 . O1 . 79.44(18) yes
O1 3_655 Zn1 . O1 . 88.07(7) yes
O1 5_665 Zn1 . O1 . 158.9(4) yes
O1 7_565 Zn1 . O1 . 88.07(7) yes
O1 6_556 C1 . C2 . 118.0(6) yes
O1 6_556 C1 . O1 . 124.1(11) yes
C2 . C1 . O1 . 118.0(6) yes
C1 . C2 . C3 6_556 120.6(5) yes
C1 . C2 . C3 . 120.6(5) yes
C3 6_556 C2 . C3 . 118.8(10) yes
C3 5_565 C3 . C2 . 120.6(5) yes
C3 5_565 C3 . H32 . 119.5 no
C2 . C3 . H32 . 119.9 no
C4 6_555 C4 . H13 11_555 102.0 no
C4 6_555 C4 . H52 11_555 109.1 no
H13 11_555 C4 . H52 11_555 114.7 no
C4 6_555 C4 . H51 7_565 109.1 no
H13 11_555 C4 . H51 7_565 114.5 no
H52 11_555 C4 . H51 7_565 0.2 no
C4 6_555 C4 . H51 9_655 109.1 no
H13 11_555 C4 . H51 9_655 9.3 no
H52 11_555 C4 . H51 9_655 106.1 no
H51 7_565 C4 . H51 9_655 105.9 no
C4 6_555 C4 . N1 . 111.2(2) yes
H13 11_555 C4 . N1 . 109.0 no
H52 11_555 C4 . N1 . 110.5 no
H51 7_565 C4 . N1 . 110.6 no
H51 9_655 C4 . N1 . 110.6 no
C4 6_555 C4 . H13 . 102.0 no
H13 11_555 C4 . H13 . 122.9 no
H52 11_555 C4 . H13 . 9.2 no
H51 7_565 C4 . H13 . 9.3 no
H51 9_655 C4 . H13 . 114.5 no
C4 6_555 C4 . H52 . 109.1 no
H13 11_555 C4 . H52 . 9.2 no
H52 11_555 C4 . H52 . 106.3 no
H51 7_565 C4 . H52 . 106.1 no
H51 9_655 C4 . H52 . 0.2 no
N1 . C4 . H13 . 109.0 no
N1 . C4 . H52 . 110.5 no
H13 . C4 . H52 . 114.7 no
C5 6_555 C5 . H51 9_655 108.7 no
C5 6_555 C5 . H52 9_655 108.8 no
H51 9_655 C5 . H52 9_655 109.5 no
C5 6_555 C5 . N1 . 112.2(2) yes
H51 9_655 C5 . N1 . 108.8 no
H52 9_655 C5 . N1 . 108.8 no
C5 6_555 C5 . H51 . 108.7 no
H51 9_655 C5 . H51 . 109.6 no
H52 9_655 C5 . H51 . 0.1 no
N1 . C5 . H51 . 108.8 no
C5 6_555 C5 . H52 . 108.8 no
H51 9_655 C5 . H52 . 0.1 no
H52 9_655 C5 . H52 . 109.3 no
N1 . C5 . H52 . 108.8 no
H51 . C5 . H52 . 109.5 no
C4 5_665 N1 . C4 7_565 82.45(15) yes
C4 5_665 N1 . C4 3_655 82.45(15) yes
C4 7_565 N1 . C4 3_655 137.5(5) yes
C4 5_665 N1 . C4 . 137.5(5) yes
C4 7_565 N1 . C4 . 82.45(15) yes
C4 3_655 N1 . C4 . 82.45(15) yes
C4 5_665 N1 . C5 11_555 118.2(2) yes
C4 7_565 N1 . C5 11_555 41.66(5) yes
C4 3_655 N1 . C5 11_555 118.2(2) yes
C4 . N1 . C5 11_555 41.66(5) yes
C4 5_665 N1 . C5 . 118.2(2) yes
C4 7_565 N1 . C5 . 118.2(2) yes
C4 3_655 N1 . C5 . 41.66(5) yes
C4 . N1 . C5 . 41.66(5) yes
C5 11_555 N1 . C5 . 81.78(17) yes
C4 5_665 N1 . C5 3_655 41.66(5) yes
C4 7_565 N1 . C5 3_655 118.2(2) yes
C4 3_655 N1 . C5 3_655 41.66(5) yes
C4 . N1 . C5 3_655 118.2(2) yes
C5 11_555 N1 . C5 3_655 135.6(5) yes
C4 5_665 N1 . C5 5_665 41.66(5) yes
C4 7_565 N1 . C5 5_665 41.66(5) yes
C4 3_655 N1 . C5 5_665 118.2(2) yes
C4 . N1 . C5 5_665 118.2(2) yes
C5 11_555 N1 . C5 5_665 81.78(17) yes
C5 . N1 . C5 3_655 81.78(17) yes
C5 . N1 . C5 5_665 135.6(5) yes
C5 3_655 N1 . C5 5_665 81.78(17) yes
Zn1 . O1 . C1 . 128.5(7) yes
C5 . H51 . C4 3_655 67.8 no
C5 . H52 . C4 . 67.9 no



# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
0 4 0 x .
3 11 5 x .
4 7 9 x .
4 6 5 x .
0 3 2 x .
0 4 11 x .
0 0 2 x .
# looking for ARCHIVE-HKL.CIF 

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

data_2_FC70_010GPa
_database_code_depnum_ccdc_archive 'CCDC 2087894'
loop_
_audit_author_name
_audit_author_address
'Stephen Moggach'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2021-06-03 deposited with the CCDC.	2021-09-29 downloaded from the CCDC.
;
_audit_creation_date             2021-05-26
_audit_creation_method           CRYSTALS_ver_14.61_build_6999

_refine_special_details          
; 
027_ALERT_3_A _diffrn_reflns_theta_full value (too) Low ......      15.17 Degree
029_ALERT_3_A _diffrn_measured_fraction_theta_full value Low .      0.413 Why?
913_ALERT_3_C Missing # of Very Strong Reflections in FCF ....         18 Note
088_ALERT_3_B Poor Data / Parameter Ratio ....................       6.11 Note
910_ALERT_3_B Missing # of FCF Reflection(s) Below Theta(Min).         12 Note
911_ALERT_3_B Missing FCF Refl Between Thmin & STh/L=    0.600        231 Report
341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............    0.00975 Ang.

These are caused by shading from the pressure cell.


921_ALERT_1_A R1  in the CIF and FCF Differ by ...............     0.1072 Check
922_ALERT_1_A wR2 in the CIF and FCF Differ by ...............     0.3313 Check

Reflections that overlap with W-gasket, or have poor correlations within 
2 degrees of the half-opening angle of the cell have been removed, 
causing the above alert. These were removed after data processing, 
as a number of strong reflections were measures well close to W-rings
that we wanted to include in the refinement.


992_ALERT_5_B Repd & Actual _reflns_number_gt Values Differ by         45 Check

This has been checked.


084_ALERT_3_A High wR2 Value (i.e. > 0.25) ...................       0.56 Report
082_ALERT_2_B High R1 Value ..................................       0.18 Report
148_ALERT_3_C s.u. on the      a    - Axis is (Too) Large ....      0.018 Ang.
148_ALERT_3_C s.u. on the      c    - Axis is (Too) Large ....      0.040 Ang.
202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent .........          3 Check
              N10     C10     C11
241_ALERT_2_C High   'MainMol' Ueq as Compared to Neighbors of         O1 Check
242_ALERT_2_C Low    'MainMol' Ueq as Compared to Neighbors of         N1 Check
329_ALERT_4_C Carbon Atom Hybridisation Unclear for ..........        C10 Check
905_ALERT_3_C Negative K value in the Analysis of Variance ...     -4.448 Report

These are all caused by disorder on the DABCO ligand and DMF solvent.


601_ALERT_2_C Unit Cell Contains Solvent Accessible VOIDS of .         45 Ang**3

This is correct.



#===============================================================================
002_ALERT_2_G Number of Distance or Angle Restraints on AtSite         12 Note
003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...         11 Report
042_ALERT_1_G Calc. and Reported Moiety Formula Strings Differ     Please Check
072_ALERT_2_G SHELXL First  Parameter in WGHT  Unusually Large       0.15 Report
083_ALERT_2_G SHELXL Second Parameter in WGHT  Unusually Large      28.44 Why ?
092_ALERT_4_G Check: Wavelength Given is not Cu,Ga,Mo,Ag,In Ka    0.48590 Ang.
300_ALERT_4_G Atom Site Occupancy of C4         Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of C5         Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H41        Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H42        Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H51        Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H52        Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of O10        Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of H101       Constrained at        0.5 Check
301_ALERT_3_G Main Residue  Disorder ..............(Resd  1  )        14% Note
302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd  2  )        20% Note
760_ALERT_1_G CIF Contains no Torsion Angles .................          ? Info
769_ALERT_4_G CIF Embedded explicitly supplied scattering data     Please Note
773_ALERT_2_G Check long C-C Bond in CIF: C4       --C5              1.85 Ang.
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      35.00 Deg.
              C4   -C4   -C5     18_566   1_555  30_556 ......     #   26 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       0.70 Deg.
              H52  -C4   -H42    13_565   1_555   1_555 ......     #   46 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       4.50 Deg.
              H41  -C4   -H51     1_555   1_555   1_555 ......     #   59 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      33.80 Deg.
              C5   -C5   -C4     30_556   1_555  30_556 ......     #   62 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       1.40 Deg.
              H42  -C5   -H52     5_655   1_555   1_555 ......     #   87 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       4.80 Deg.
              H41  -C5   -H51     1_555   1_555   1_555 ......     #   93 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      16.20 Deg.
              H101 -C10  -O10    31_664   1_555   1_555 ......     #  100 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      16.20 Deg.
              O10  -C10  -H101   31_664   1_555   1_555 ......     #  104 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      42.60 Deg.
              C4   -N1   -C5      9_665   1_555   5_655 ......     #  119 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.30 Deg.
              C4   -N1   -C5      5_655   1_555   5_655 ......     #  121 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.30 Deg.
              C4   -N1   -C5     13_565   1_555  13_565 ......     #  124 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      42.60 Deg.
              C4   -N1   -C5      1_555   1_555  13_565 ......     #  126 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.30 Deg.
              C4   -N1   -C5      9_665   1_555   9_665 ......     #  128 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      42.60 Deg.
              C4   -N1   -C5     13_565   1_555   9_665 ......     #  129 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      42.60 Deg.
              C4   -N1   -C5      5_655   1_555   1_555 ......     #  135 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.30 Deg.
              C4   -N1   -C5      1_555   1_555   1_555 ......     #  136 Check
804_ALERT_5_G Number of ARU-Code Packing Problem(s) in PLATON           1 Info
860_ALERT_3_G Number of Least-Squares Restraints .............        165 Note
912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600          1 Note
958_ALERT_1_G Calculated (ThMax) and Actual (FCF) Lmax Differ          14 Units
960_ALERT_3_G Number of Intensities with I  <   - 2*sig(I) ...         10 Check
#===============================================================================

No action taken. 
;

_cell_length_a                   15.130(18)
_cell_length_b                   15.130(18)
_cell_length_c                   19.32(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4423(14)

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I 4/m c m '
_symmetry_space_group_name_Hall  '-I 4 2c'
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
-y,x,z
y,-x,-z
-y+1/2,x+1/2,z+1/2
y+1/2,-x+1/2,-z+1/2
-x,-y,z
x,y,-z
-x+1/2,-y+1/2,z+1/2
x+1/2,y+1/2,-z+1/2
y,-x,z
-y,x,-z
y+1/2,-x+1/2,z+1/2
-y+1/2,x+1/2,-z+1/2
-x,y,z+1/2
x,-y,-z+1/2
-x+1/2,y+1/2,z+1
x+1/2,-y+1/2,-z+1
y,x,z+1/2
-y,-x,-z+1/2
y+1/2,x+1/2,z+1
-y+1/2,-x+1/2,-z+1
x,-y,z+1/2
-x,y,-z+1/2
x+1/2,-y+1/2,z+1
-x+1/2,y+1/2,-z+1
-y,-x,z+1/2
y,x,-z+1/2
-y+1/2,-x+1/2,z+1
y+1/2,x+1/2,-z+1

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 0.0006 0.0007 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 0.0016 0.0014 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 0.0036 0.0026 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 0.3043 0.7253 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 = C37.50 H7.50 N7.50 O7.50 Zn7.50 
# Dc =      1.76 Fooo =   2280.00 Mu =     40.50 M =   1173.37
# Found Formula = C34 H48 N6 O12 Zn2 
# Dc =      1.30 FOOO =   1800.00 Mu =     11.44 M =    863.55

_chemical_formula_sum            'C34 H48 N6 O12 Zn2'
_chemical_formula_moiety         '(C22 H20 N2 O8 Zn2)n. 4(C3H7NO)'
_chemical_compound_source        .
_chemical_formula_weight         863.55


_cell_measurement_reflns_used    942
_cell_measurement_theta_min      3
_cell_measurement_theta_max      17
_cell_measurement_temperature    298

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.050
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.150

_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1800
_exptl_absorpt_coefficient_mu    1.144

# Sheldrick geometric approximatio 0.84 0.94 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_T_max  0.94
_diffrn_measurement_device_type  Synchrotron
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.48590
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count 942
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      298
_diffrn_ambient_pressure         100000
_diffrn_reflns_number            9425
_diffrn_reflns_av_unetI/netI     0.108
_reflns_number_total             476
_diffrn_reflns_av_R_equivalents  0.083
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 476 
# Theoretical number of reflections is about 2100 


_diffrn_reflns_theta_min         2.180
_diffrn_reflns_theta_max         17.235
_diffrn_measured_fraction_theta_max 0.410

_diffrn_reflns_theta_full        15.166
_diffrn_measured_fraction_theta_full 0.413


_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_reflns_limit_h_min              0
_reflns_limit_h_max              13
_reflns_limit_k_min              2
_reflns_limit_k_max              18
_reflns_limit_l_min              0
_reflns_limit_l_max              9

_oxford_diffrn_Wilson_B_factor   1.77
_oxford_diffrn_Wilson_scale      855.88

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

_refine_diff_density_min         -0.37
_refine_diff_density_max         0.46


# 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_refine_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_restraints     165
_refine_ls_number_parameters     70
_refine_ls_number_reflns         428
_oxford_refine_ls_R_factor_ref   0.0864
_refine_ls_wR_factor_ref         0.2287
_refine_ls_goodness_of_fit_ref   1.0796
_refine_ls_shift/su_max          0.0262173
_refine_ls_shift/su_mean         0.0007864


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        476
_refine_ls_R_factor_all          0.1881
_refine_ls_wR_factor_all         0.5600

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                386
_refine_ls_R_factor_gt           0.1787
_refine_ls_wR_factor_gt          0.5520


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.15P)² +28.44P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

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

# Replace last . with number of unfound hydrogen atoms attached 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 0.5000 0.5772(3) 0.0414 1.0000 Uani DS T . . . .
C1 C 0.6504(5) 0.5802(6) 0.5000 0.0576 1.0000 Uani DS TU . . . .
C2 C 0.7272(5) 0.6427(6) 0.5000 0.0522 1.0000 Uani DS TU . . . .
C3 C 0.7616(5) 0.6731(5) 0.5615(3) 0.0604 1.0000 Uani D U . . . .
C4 C 0.5906(9) 0.5010(3) 0.7102(2) 0.0594 0.3750 Uani D U . . . .
C5 C 0.5638(7) 0.5637(7) 0.7102(2) 0.0590 0.3750 Uani D U . . . .
C10 C 0.684(2) 0.816(2) 0.723(3) 0.300(17) 1.0000 Uiso DS U . . . .
C11 C 0.563(2) 0.825(2) 0.628(2) 0.300(17) 1.0000 Uiso D U . . . .
N1 N 0.5000 0.5000 0.6832(16) 0.0372 1.0000 Uani DS TU . . . .
N10 N 0.6353(16) 0.8647(16) 0.665(2) 0.300(17) 1.0000 Uiso DS U . . . .
O1 O 0.6203(4) 0.5576(4) 0.5574(3) 0.0712 1.0000 Uani D U . . . .
O10 O 0.752(2) 0.858(2) 0.740(3) 0.300(17) 0.5000 Uiso D U . . . .
H32 H 0.7365 0.6546 0.6042 0.0722 1.0000 Uiso R . . . . .
H111 H 0.5483 0.8587 0.5866 0.3980 1.0000 Uiso R . . . . .
H112 H 0.5097 0.8162 0.6561 0.3980 1.0000 Uiso R . . . . .
H113 H 0.5865 0.7667 0.6145 0.3980 1.0000 Uiso R . . . . .
H101 H 0.6597 0.7676 0.7480 0.3003 0.5000 Uiso R . . . . .
H41 H 0.6198 0.5537 0.6946 0.0688 0.3750 Uiso R . . . . .
H42 H 0.6216 0.4502 0.6930 0.0688 0.3750 Uiso R . . . . .
H51 H 0.6215 0.5481 0.6940 0.0685 0.3750 Uiso R . . . . .
H52 H 0.5485 0.6217 0.6937 0.0685 0.3750 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.444(6)
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 . Zn1 2_666 2.984(12) yes
Zn1 . O1 5_655 2.054(5) yes
Zn1 . O1 13_565 2.054(5) yes
Zn1 . O1 9_665 2.054(5) yes
Zn1 . N1 . 2.05(3) yes
Zn1 . O1 . 2.054(5) yes
C1 . O1 10_556 1.246(6) yes
C1 . C2 . 1.498(6) yes
C1 . O1 . 1.246(6) yes
C2 . C3 10_556 1.377(6) yes
C2 . C3 . 1.377(6) yes
C3 . C3 31_664 1.396(7) yes
C3 . H32 . 0.950 no
C4 . C4 18_566 1.538(9) yes
C4 . H52 13_565 0.940 no
C4 . C5 30_556 1.854(9) yes
C4 . C5 13_565 1.062(11) yes
C4 . C5 . 1.031(11) yes
C4 . N1 . 1.467(8) yes
C4 . H41 . 0.960 no
C4 . H42 . 0.960 no
C4 . H51 . 0.907 no
C5 . C5 30_556 1.538(9) yes
C5 . H42 5_655 0.961 no
C5 . N1 . 1.460(8) yes
C5 . H41 . 0.910 no
C5 . H51 . 0.956 no
C5 . H52 . 0.962 no
C10 . H101 31_664 0.952 no
C10 . O10 31_664 1.248(6) yes
C10 . N10 . 1.523(9) yes
C10 . O10 . 1.248(6) yes
C10 . H101 . 0.952 no
C11 . N10 . 1.443(8) yes
C11 . H111 . 0.980 no
C11 . H112 . 0.980 no
C11 . H113 . 0.980 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
Zn1 2_666 Zn1 . O1 5_655 79.2(2) yes
Zn1 2_666 Zn1 . O1 13_565 79.2(2) yes
O1 5_655 Zn1 . O1 13_565 158.5(4) yes
Zn1 2_666 Zn1 . O1 9_665 79.2(2) yes
O1 5_655 Zn1 . O1 9_665 88.00(15) yes
O1 13_565 Zn1 . O1 9_665 88.00(8) yes
Zn1 2_666 Zn1 . N1 . 179.99 yes
O1 5_655 Zn1 . N1 . 100.8(2) yes
O1 13_565 Zn1 . N1 . 100.8(2) yes
O1 9_665 Zn1 . N1 . 100.8(2) yes
Zn1 2_666 Zn1 . O1 . 79.2(2) yes
O1 5_655 Zn1 . O1 . 88.00(8) yes
O1 13_565 Zn1 . O1 . 88.00(15) yes
O1 9_665 Zn1 . O1 . 158.5(4) yes
N1 . Zn1 . O1 . 100.8(2) yes
O1 10_556 C1 . C2 . 117.2(3) yes
O1 10_556 C1 . O1 . 125.5(6) yes
C2 . C1 . O1 . 117.2(3) yes
C1 . C2 . C3 10_556 120.3(3) yes
C1 . C2 . C3 . 120.3(3) yes
C3 10_556 C2 . C3 . 119.4(5) yes
C3 31_664 C3 . C2 . 120.2(3) yes
C3 31_664 C3 . H32 . 119.4 no
C2 . C3 . H32 . 119.9 no
C4 18_566 C4 . H52 13_565 108.9 no
C4 18_566 C4 . C5 30_556 35.0(4) yes
H52 13_565 C4 . C5 30_556 143.2 no
C4 18_566 C4 . C5 13_565 89.0(5) yes
H52 13_565 C4 . C5 13_565 57.0 no
C5 30_556 C4 . C5 13_565 112.9(7) yes
C4 18_566 C4 . C5 . 91.1(5) yes
H52 13_565 C4 . C5 . 158.3 no
C5 30_556 C4 . C5 . 56.1(5) yes
C5 13_565 C4 . C5 . 134.3(12) yes
C4 18_566 C4 . N1 . 110.8(13) yes
H52 13_565 C4 . N1 . 109.7 no
C5 30_556 C4 . N1 . 95.4(13) yes
C5 13_565 C4 . N1 . 68.4(6) yes
C5 . C4 . N1 . 69.0(6) yes
C4 18_566 C4 . H41 . 109.3 no
H52 13_565 C4 . H41 . 109.1 no
C5 30_556 C4 . H41 . 86.3 no
C5 13_565 C4 . H41 . 160.7 no
C5 . C4 . H41 . 54.3 no
C4 18_566 C4 . H42 . 109.3 no
H52 13_565 C4 . H42 . 0.7 no
C5 30_556 C4 . H42 . 143.6 no
C5 13_565 C4 . H42 . 56.5 no
C5 . C4 . H42 . 158.2 no
C4 18_566 C4 . H51 . 111.1 no
H52 13_565 C4 . H51 . 104.6 no
C5 30_556 C4 . H51 . 89.8 no
C5 13_565 C4 . H51 . 157.3 no
C5 . C4 . H51 . 58.7 no
N1 . C4 . H41 . 109.0 no
N1 . C4 . H42 . 109.0 no
H41 . C4 . H42 . 109.5 no
N1 . C4 . H51 . 111.5 no
H41 . C4 . H51 . 4.5 no
H42 . C4 . H51 . 105.0 no
C5 30_556 C5 . H42 5_655 110.1 no
C5 30_556 C5 . C4 30_556 33.8(4) yes
H42 5_655 C5 . C4 30_556 88.4 no
C5 30_556 C5 . C4 5_655 89.9(5) yes
H42 5_655 C5 . C4 5_655 56.4 no
C4 30_556 C5 . C4 5_655 56.0(5) yes
C5 30_556 C5 . C4 . 90.1(5) yes
H42 5_655 C5 . C4 . 157.8 no
C4 30_556 C5 . C4 . 113.8(7) yes
C4 5_655 C5 . C4 . 135.7(12) yes
C5 30_556 C5 . N1 . 110.9(13) yes
H42 5_655 C5 . N1 . 109.5 no
C4 30_556 C5 . N1 . 95.9(13) yes
C4 5_655 C5 . N1 . 69.1(6) yes
C4 . C5 . N1 . 69.7(6) yes
C5 30_556 C5 . H41 . 109.4 no
H42 5_655 C5 . H41 . 104.0 no
C4 30_556 C5 . H41 . 141.9 no
C4 5_655 C5 . H41 . 157.1 no
C4 . C5 . H41 . 58.9 no
C5 30_556 C5 . H51 . 109.2 no
H42 5_655 C5 . H51 . 108.3 no
C4 30_556 C5 . H51 . 142.5 no
C4 5_655 C5 . H51 . 159.6 no
C4 . C5 . H51 . 54.2 no
C5 30_556 C5 . H52 . 109.3 no
H42 5_655 C5 . H52 . 1.4 no
C4 30_556 C5 . H52 . 87.2 no
C4 5_655 C5 . H52 . 55.1 no
C4 . C5 . H52 . 159.0 no
N1 . C5 . H41 . 112.8 no
N1 . C5 . H51 . 108.9 no
H41 . C5 . H51 . 4.8 no
N1 . C5 . H52 . 108.9 no
H41 . C5 . H52 . 105.3 no
H51 . C5 . H52 . 109.6 no
H101 31_664 C10 . O10 31_664 125.2 no
H101 31_664 C10 . N10 . 124.0 no
O10 31_664 C10 . N10 . 110.0(4) yes
H101 31_664 C10 . O10 . 16.2 no
O10 31_664 C10 . O10 . 140.0(7) yes
N10 . C10 . O10 . 110.0(4) yes
H101 31_664 C10 . H101 . 109.7 no
O10 31_664 C10 . H101 . 16.2 no
N10 . C10 . H101 . 124.0 no
O10 . C10 . H101 . 125.2 no
N10 . C11 . H111 . 111.0 no
N10 . C11 . H112 . 113.7 no
H111 . C11 . H112 . 109.5 no
N10 . C11 . H113 . 103.5 no
H111 . C11 . H113 . 109.5 no
H112 . C11 . H113 . 109.5 no
C4 9_665 N1 . C4 13_565 82.7(9) yes
C4 9_665 N1 . C4 5_655 82.7(9) yes
C4 13_565 N1 . C4 5_655 138(3) yes
C4 9_665 N1 . C4 . 138(3) yes
C4 13_565 N1 . C4 . 82.7(9) yes
C4 5_655 N1 . C4 . 82.7(9) yes
C4 9_665 N1 . C5 5_655 42.6(5) yes
C4 13_565 N1 . C5 5_655 119.9(17) yes
C4 5_655 N1 . C5 5_655 41.3(5) yes
C4 . N1 . C5 5_655 118.9(17) yes
C4 9_665 N1 . C5 13_565 118.9(17) yes
C4 13_565 N1 . C5 13_565 41.3(5) yes
C4 5_655 N1 . C5 13_565 119.9(17) yes
C4 . N1 . C5 13_565 42.6(5) yes
C5 5_655 N1 . C5 13_565 138(3) yes
C4 9_665 N1 . C5 9_665 41.3(5) yes
C4 13_565 N1 . C5 9_665 42.6(5) yes
C4 5_655 N1 . C5 9_665 118.9(17) yes
C4 . N1 . C5 9_665 119.9(17) yes
C5 5_655 N1 . C5 9_665 82.7(9) yes
C4 9_665 N1 . C5 . 119.9(17) yes
C4 13_565 N1 . C5 . 118.9(17) yes
C4 5_655 N1 . C5 . 42.6(5) yes
C4 . N1 . C5 . 41.3(5) yes
C5 5_655 N1 . C5 . 82.7(9) yes
C4 9_665 N1 . Zn1 . 110.8(13) yes
C4 13_565 N1 . Zn1 . 110.8(13) yes
C4 5_655 N1 . Zn1 . 110.8(13) yes
C4 . N1 . Zn1 . 110.8(13) yes
C5 5_655 N1 . Zn1 . 110.9(13) yes
C5 13_565 N1 . C5 9_665 82.7(9) yes
C5 13_565 N1 . C5 . 82.7(9) yes
C5 9_665 N1 . C5 . 138(3) yes
C5 13_565 N1 . Zn1 . 110.9(13) yes
C5 9_665 N1 . Zn1 . 110.9(13) yes
C5 . N1 . Zn1 . 110.9(13) yes
C10 . N10 . C11 31_664 121.9(6) yes
C10 . N10 . C11 . 121.9(6) yes
C11 31_664 N10 . C11 . 113.0(8) yes
Zn1 . O1 . C1 . 127.4(5) yes
C4 . H41 . C5 . 66.9 no
C5 13_565 H42 . C4 . 67.1 no
C5 . H51 . C4 . 67.1 no
C5 . H52 . C4 5_655 67.9 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
C4 . H42 . O10 19_644 133 0.96 2.54 3.27(2) yes
C4 5_655 H52 . O10 31_664 135 0.94 2.54 3.27(2) yes



# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
1 2 1 x .
6 12 0 x .
1 15 0 x .
9 12 1 x .
3 10 7 x .
4 10 6 x .
3 6 1 x .
6 12 2 x .
2 15 1 x .
6 9 5 x .
8 8 4 x .
10 13 9 x .
10 14 6 x .
0 12 0 x .
1 15 2 x .
3 17 6 x .
0 4 0 x .
6 6 0 x .
3 4 3 x .
1 9 0 x .
0 10 6 x .
2 7 3 x .
1 11 0 x .
5 14 3 x .
6 11 7 x .
8 15 7 x .
4 17 5 x .
0 10 0 x .
2 6 4 x .
5 8 1 x .
9 10 1 x .
10 11 3 x .
3 13 2 x .
3 11 4 x .
4 13 1 x .
5 6 3 x .
6 16 6 x .
6 7 3 x .
7 9 4 x .
5 10 5 x .
3 12 5 x .
11 13 6 x .
1 6 3 x .
5 6 1 x .
9 15 4 x .
3 10 5 x .
6 10 8 x .
11 14 1 x .
# looking for ARCHIVE-HKL.CIF 

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

data_3_Ben_015GPa
_database_code_depnum_ccdc_archive 'CCDC 2087896'
loop_
_audit_author_name
_audit_author_address
'Stephen Moggach'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2021-06-03 deposited with the CCDC.	2021-09-29 downloaded from the CCDC.
;
_audit_creation_date             2021-05-26
_audit_creation_method           CRYSTALS_ver_14.61_build_6999

_refine_special_details          
; 
027_ALERT_3_A _diffrn_reflns_theta_full value (too) Low ......      17.46 Degree
029_ALERT_3_A _diffrn_measured_fraction_theta_full value Low .      0.784 Why?
910_ALERT_3_C Missing # of FCF Reflection(s) Below Theta(Min).          5 Note
023_ALERT_3_B Resolution (too) Low [sin(theta)/Lambda < 0.6]..       0.56 Ang-1
088_ALERT_3_B Poor Data / Parameter Ratio ....................       7.33 Note
341_ALERT_3_B Low Bond Precision on  C-C Bonds ...............    0.02329 Ang.
911_ALERT_3_B Missing FCF Refl Between Thmin & STh/L=    0.556        230 Report

These are caused by shading from the pressure cell.

922_ALERT_1_A wR2 in the CIF and FCF Differ by ...............     0.1436 Check
921_ALERT_1_B R1  in the CIF and FCF Differ by ...............     0.0155 Check

Reflections that overlap with W-gasket, or have poor correlations within 
2 degrees of the half-opening angle of the cell have been removed, 
causing the above alert. These were removed after data processing, 
as a number of strong reflections measured well close to W-rings
that we wanted to include in the refinement.

601_ALERT_2_B Unit Cell Contains Solvent Accessible VOIDS of .        191 Ang**3

These are correct.

076_ALERT_1_C Occupancy      0.500 Less Than 1.0 for Sp.pos  .           C9
076_ALERT_1_C Occupancy      0.500 Less Than 1.0 for Sp.pos  .          H91
084_ALERT_3_C High wR2 Value (i.e. > 0.25) ...................       0.35 Report
241_ALERT_2_C High   'MainMol' Ueq as Compared to Neighbors of         O1 Check
242_ALERT_2_C Low    'MainMol' Ueq as Compared to Neighbors of        Zn1 Check
250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....        3.0 Note
260_ALERT_2_C Large Average Ueq of Residue Including        C7      0.195 Check
260_ALERT_2_C Large Average Ueq of Residue Including        C9      0.245 Check

These are all caused by disorder in the DABCO and partial occupancy of included 
benzene solvent molecules.

#===============================================================================
002_ALERT_2_G Number of Distance or Angle Restraints on AtSite         12 Note
003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...         12 Report
004_ALERT_5_G Polymeric Structure Found with Maximum Dimension          3 Info
042_ALERT_1_G Calc. and Reported Moiety Formula Strings Differ     Please Check
045_ALERT_1_G Calculated and Reported Z Differ by a Factor ...       2.00 Check
072_ALERT_2_G SHELXL First  Parameter in WGHT  Unusually Large       0.12 Report
083_ALERT_2_G SHELXL Second Parameter in WGHT  Unusually Large      43.74 Why ?
093_ALERT_1_G No s.u.'s on H-positions, Refinement Reported as      mixed Check
300_ALERT_4_G Atom Site Occupancy of C4         Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of C5         Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of C6         Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H41        Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H42        Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H51        Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H52        Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H61        Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H62        Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of C9         Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of C10        Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of H91        Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of H101       Constrained at        0.5 Check
301_ALERT_3_G Main Residue  Disorder ..............(Resd  1  )        20% Note
302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd  3  )       100% Note
432_ALERT_2_G Short Inter X...Y Contact  C9       ..C10              1.35 Ang.
                                                    1-x,y,z  =      5_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C9       ..C10              2.38 Ang.
                                                    x,y,1-z  =     14_556 Check
432_ALERT_2_G Short Inter X...Y Contact  C9       ..C10              2.38 Ang.
                                                  1-x,y,1-z  =     10_656 Check
432_ALERT_2_G Short Inter X...Y Contact  C9       ..C9               2.75 Ang.
                                                  1-x,y,1-z  =     10_656 Check
432_ALERT_2_G Short Inter X...Y Contact  C10      ..C10              1.40 Ang.
                                                    x,y,1-z  =     14_556 Check
432_ALERT_2_G Short Inter X...Y Contact  C10      ..C10              2.35 Ang.
                                                    1-x,y,z  =      5_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C10      ..C10              2.73 Ang.
                                                  1-x,y,1-z  =     10_656 Check
760_ALERT_1_G CIF Contains no Torsion Angles .................          ? Info
769_ALERT_4_G CIF Embedded explicitly supplied scattering data     Please Note
773_ALERT_2_G Check long C-C Bond in CIF: C5       --C5              1.84 Ang.
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      40.00 Deg.
              C4   -N1   -C5      5_555   1_555   5_555 ......     #   26 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      40.00 Deg.
              C4   -N1   -C5      5_555   1_555  13_555 ......     #   27 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      44.80 Deg.
              C5   -N1   -C6     13_555   1_555   9_555 ......     #   34 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      44.80 Deg.
              C5   -N1   -C6      9_555   1_555   9_555 ......     #   35 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      40.00 Deg.
              C5   -N1   -C4      9_555   1_555   1_555 ......     #   49 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      44.80 Deg.
              C5   -N1   -C6      5_555   1_555   1_555 ......     #   52 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      40.00 Deg.
              C5   -N1   -C4      1_555   1_555   1_555 ......     #   58 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      44.80 Deg.
              C5   -N1   -C6      1_555   1_555   1_555 ......     #   60 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      11.10 Deg.
              H62  -C5   -H61     5_555   1_555   1_555 ......     #   74 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       6.60 Deg.
              H62  -C5   -H51     5_555   1_555   1_555 ......     #   79 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       6.50 Deg.
              H42  -C5   -H52     9_555   1_555   1_555 ......     #   85 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       2.10 Deg.
              H42  -C5   -H41     9_555   1_555   1_555 ......     #   90 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       5.40 Deg.
              H61  -C5   -H51     1_555   1_555   1_555 ......     #   92 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       8.50 Deg.
              H52  -C5   -H41     1_555   1_555   1_555 ......     #   97 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      10.00 Deg.
              H41  -C4   -H52     9_555   1_555   9_555 ......     #  106 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      11.30 Deg.
              H42  -C4   -H52     9_555   1_555   1_555 ......     #  111 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       1.30 Deg.
              H42  -C4   -H41     9_555   1_555   1_555 ......     #  116 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       1.30 Deg.
              H41  -C4   -H42     9_555   1_555   1_555 ......     #  120 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      11.30 Deg.
              H52  -C4   -H42     9_555   1_555   1_555 ......     #  122 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      10.00 Deg.
              H52  -C4   -H41     1_555   1_555   1_555 ......     #  123 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       3.60 Deg.
              H61  -C6   -H51     5_555   1_555   5_555 ......     #  142 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       6.70 Deg.
              H62  -C6   -H61     5_555   1_555   1_555 ......     #  152 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       6.70 Deg.
              H61  -C6   -H62     5_555   1_555   1_555 ......     #  154 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       4.40 Deg.
              H51  -C6   -H62     5_555   1_555   1_555 ......     #  156 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       4.40 Deg.
              H62  -C6   -H51     5_555   1_555   1_555 ......     #  162 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       3.60 Deg.
              H61  -C6   -H51     1_555   1_555   1_555 ......     #  164 Check
860_ALERT_3_G Number of Least-Squares Restraints .............        185 Note
909_ALERT_3_G Percentage of I>2sig(I) Data at Theta(Max) Still        81% Note
956_ALERT_1_G Calculated (ThMax) and Actual (FCF) Hmax Differ           2 Units
957_ALERT_1_G Calculated (ThMax) and Actual (FCF) Kmax Differ           2 Units
992_ALERT_5_G Repd & Actual _reflns_number_gt Values Differ by          8 Check
#===============================================================================

No action taken.
;

_cell_length_a                   13.6785(13)
_cell_length_b                   16.9282(15)
_cell_length_c                   9.6888(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2243.5(3)

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'C m m m '
_symmetry_space_group_name_Hall  '-C 2 2 '
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
x,-y,-z
-x+1/2,y+1/2,z
x+1/2,-y+1/2,-z
x,-y,z
-x,y,-z
x+1/2,-y+1/2,z
-x+1/2,y+1/2,-z
-x,-y,z
x,y,-z
-x+1/2,-y+1/2,z
x+1/2,y+1/2,-z

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            2

# Given Formula = C32 H16 N4 O4 Zn8 
# Dc =      1.54 Fooo =   1016.00 Mu =     42.32 M =   1043.54
# Found Formula = C34 H38 N2 O8 Zn2 
# Dc =      1.09 FOOO =    760.00 Mu =     11.08 M =    733.44

_chemical_formula_sum            'C34 H38 N2 O8 Zn2'
_chemical_formula_moiety         '(C22 H20 N2 O8 Zn2)n . 2 (C6 H6)'
_chemical_compound_source        .
_chemical_formula_weight         733.44


_cell_measurement_reflns_used    2140
_cell_measurement_theta_min      3
_cell_measurement_theta_max      23
_cell_measurement_temperature    298

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.050
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.150

_exptl_crystal_density_diffrn    1.086
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             760
_exptl_absorpt_coefficient_mu    1.108

# Sheldrick geometric approximatio 0.85 0.95 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_T_max  0.95
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      298
_diffrn_ambient_pressure         150000
_diffrn_reflns_number            3438
_diffrn_reflns_av_unetI/netI     0.097
_reflns_number_total             682
_diffrn_reflns_av_R_equivalents  0.068
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 682 
# Theoretical number of reflections is about 516 


_diffrn_reflns_theta_min         3.196
_diffrn_reflns_theta_max         23.275
_diffrn_measured_fraction_theta_max 0.722

_diffrn_reflns_theta_full        17.457
_diffrn_measured_fraction_theta_full 0.784


_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_reflns_limit_h_min              0
_reflns_limit_h_max              14
_reflns_limit_k_min              0
_reflns_limit_k_max              17
_reflns_limit_l_min              0
_reflns_limit_l_max              10

_oxford_diffrn_Wilson_B_factor   0.72
_oxford_diffrn_Wilson_scale      323.38

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

_refine_diff_density_min         -1.02
_refine_diff_density_max         0.68


# 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_refine_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_restraints     185
_refine_ls_number_parameters     91
_refine_ls_number_reflns         667
_oxford_refine_ls_R_factor_ref   0.0824
_refine_ls_wR_factor_ref         0.2097
_refine_ls_goodness_of_fit_ref   1.0115
_refine_ls_shift/su_max          0.0075935
_refine_ls_shift/su_mean         0.0001723


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        682
_refine_ls_R_factor_all          0.1048
_refine_ls_wR_factor_all         0.3533

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                572
_refine_ls_R_factor_gt           0.0840
_refine_ls_wR_factor_gt          0.3163


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    mixed #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.12P)² +43.74P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

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

# Replace last . with number of unfound hydrogen atoms attached 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 0.0000 0.0000 0.15262(16) 0.0206 1.0000 Uani S T . . . .
O1 O 0.1017(5) 0.0841(3) 0.1155(6) 0.0525 1.0000 Uani D U . . . .
C1 C 0.1263(9) 0.1116(6) 0.0000 0.0346 1.0000 Uani DS TU . . . .
C2 C 0.1909(9) 0.1824(6) 0.0000 0.0350 1.0000 Uani DS TU . . . .
C3 C 0.2189(8) 0.2171(6) 0.1225(9) 0.0657 1.0000 Uani D U . . . .
N1 N 0.0000 0.0000 0.3700(11) 0.0241 1.0000 Uani DS TU . . . .
C5 C 0.0739(14) 0.0544(12) 0.420(2) 0.0364 0.3750 Uani D U . . . .
C4 C 0.101(2) -0.0000 0.418(3) 0.0365 0.3750 Uani DS TU . . . .
C7 C 0.400(4) 0.0000 -0.0000 0.1947 1.0000 Uani DS TU . . . .
C8 C 0.4499(13) 0.0696(15) 0.0000 0.1968 1.0000 Uani DS TU . . . .
C9 C 0.5000 0.1979(5) 0.358(2) 0.2458 0.5000 Uani DS TU . . . .
C10 C 0.5857(18) 0.1977(3) 0.428(2) 0.2480 0.5000 Uani D U . . . .
C6 C -0.0000 0.0798(15) 0.421(3) 0.0370 0.3750 Uani DS TU . . . .
H61 H 0.0644 0.1073 0.3893 0.0497 0.3750 Uiso R . . . . .
H62 H -0.0502 0.1073 0.3893 0.0497 0.3750 Uiso R . . . . .
H51 H 0.0583 0.1064 0.3858 0.0481 0.3750 Uiso R . . . . .
H52 H 0.1395 0.0374 0.3839 0.0481 0.3750 Uiso . . . . . .
H41 H 0.1329 0.0463 0.3821 0.0328 0.3750 Uiso . . . . . .
H42 H 0.1301 -0.0448 0.3840 0.0328 0.3750 Uiso R . . . . .
H31 H 0.1943 0.1971 0.2073 0.0745 1.0000 Uiso R . . . . .
H71 H 0.3301 -0.0000 0.0000 0.2328 1.0000 Uiso RS . . . . .
H81 H 0.4159 0.1185 -0.0000 0.2360 1.0000 Uiso RS . . . . .
H91 H 0.5000 0.1982 0.2602 0.2852 0.5000 Uiso RS . . . . .
H101 H 0.6458 0.1976 0.3793 0.2894 0.5000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.1262(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 . Zn1 2_555 2.957(3) yes
Zn1 . O1 5_555 2.022(5) yes
Zn1 . O1 9_555 2.022(5) yes
Zn1 . O1 13_555 2.022(5) yes
Zn1 . O1 . 2.022(5) yes
Zn1 . N1 . 2.107(11) yes
O1 . C1 . 1.258(7) yes
C1 . C2 . 1.488(14) yes
C2 . C3 14_555 1.379(9) yes
C2 . C3 . 1.379(9) yes
C3 . C3 15_555 1.401(15) yes
C3 . H31 . 0.950 no
N1 . C4 5_555 1.46(3) yes
N1 . C5 5_555 1.449(8) yes
N1 . C5 13_555 1.449(8) yes
N1 . C5 9_555 1.449(8) yes
N1 . C6 9_555 1.44(3) yes
N1 . C5 . 1.449(8) yes
N1 . C4 . 1.46(3) yes
N1 . C6 . 1.44(3) yes
C5 . C5 14_556 1.56(4) yes
C5 . H62 5_555 0.997 no
C5 . H42 9_555 0.858 no
C5 . C5 9_555 1.84(4) yes
C5 . H61 . 0.952 no
C5 . H51 . 0.964 no
C5 . H52 . 1.003 no
C5 . H41 . 0.895 no
C4 . C4 6_556 1.60(6) yes
C4 . H41 9_555 0.959 no
C4 . H42 9_555 0.915 no
C4 . H52 9_555 0.883 no
C4 . H52 . 0.883 no
C4 . H41 . 0.959 no
C4 . H42 . 0.915 no
C7 . C8 6_555 1.36(2) yes
C7 . C8 . 1.36(2) yes
C7 . H71 . 0.950 no
C8 . C8 5_655 1.37(4) yes
C8 . H81 . 0.950 no
C9 . C10 5_655 1.35(3) yes
C9 . C10 . 1.35(3) yes
C9 . H91 . 0.950 no
C10 . C10 14_556 1.39(4) yes
C10 . H101 . 0.950 no
C6 . C6 10_556 1.54(6) yes
C6 . H61 5_555 1.042 no
C6 . H51 5_555 0.977 no
C6 . H62 5_555 0.885 no
C6 . H61 . 1.042 no
C6 . H62 . 0.885 no
C6 . H51 . 0.977 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
Zn1 2_555 Zn1 . O1 5_555 79.74(16) yes
Zn1 2_555 Zn1 . O1 9_555 79.74(16) yes
O1 5_555 Zn1 . O1 9_555 159.5(3) yes
Zn1 2_555 Zn1 . O1 13_555 79.74(16) yes
O1 5_555 Zn1 . O1 13_555 89.5(4) yes
O1 9_555 Zn1 . O1 13_555 86.9(4) yes
Zn1 2_555 Zn1 . O1 . 79.74(16) yes
O1 5_555 Zn1 . O1 . 86.9(4) yes
O1 9_555 Zn1 . O1 . 89.5(4) yes
O1 13_555 Zn1 . O1 . 159.5(3) yes
Zn1 2_555 Zn1 . N1 . 179.99 yes
O1 5_555 Zn1 . N1 . 100.26(16) yes
O1 9_555 Zn1 . N1 . 100.26(16) yes
O1 13_555 Zn1 . N1 . 100.26(16) yes
O1 . Zn1 . N1 . 100.26(16) yes
Zn1 . O1 . C1 . 127.1(6) yes
O1 . C1 . O1 14_555 125.5(9) yes
O1 . C1 . C2 . 117.2(5) yes
O1 14_555 C1 . C2 . 117.2(5) yes
C1 . C2 . C3 14_555 120.5(5) yes
C1 . C2 . C3 . 120.5(5) yes
C3 14_555 C2 . C3 . 118.8(9) yes
C3 15_555 C3 . C2 . 120.5(5) yes
C3 15_555 C3 . H31 . 119.9 no
C2 . C3 . H31 . 119.6 no
C4 5_555 N1 . C5 5_555 40.0(10) yes
C4 5_555 N1 . C5 13_555 40.0(10) yes
C5 5_555 N1 . C5 13_555 79(2) yes
C4 5_555 N1 . C5 9_555 123.9(14) yes
C5 5_555 N1 . C5 9_555 141.3(19) yes
C5 13_555 N1 . C5 9_555 88.5(20) yes
C4 5_555 N1 . C6 9_555 83.8(6) yes
C5 5_555 N1 . C6 9_555 118.9(13) yes
C5 13_555 N1 . C6 9_555 44.8(10) yes
C5 9_555 N1 . C6 9_555 44.8(10) yes
C4 5_555 N1 . Zn1 . 108.4(13) yes
C5 5_555 N1 . Zn1 . 109.3(9) yes
C5 13_555 N1 . Zn1 . 109.3(9) yes
C5 9_555 N1 . Zn1 . 109.3(9) yes
C6 9_555 N1 . Zn1 . 110.0(13) yes
C4 5_555 N1 . C5 . 123.9(14) yes
C5 5_555 N1 . C5 . 88.5(20) yes
C5 13_555 N1 . C5 . 141.3(19) yes
C5 9_555 N1 . C5 . 79(2) yes
C6 9_555 N1 . C5 . 118.9(13) yes
C4 5_555 N1 . C4 . 143(3) yes
C5 5_555 N1 . C4 . 123.9(14) yes
C5 13_555 N1 . C4 . 123.9(14) yes
C5 9_555 N1 . C4 . 40.0(10) yes
C6 9_555 N1 . C4 . 83.8(6) yes
C4 5_555 N1 . C6 . 83.8(6) yes
C5 5_555 N1 . C6 . 44.8(10) yes
C5 13_555 N1 . C6 . 118.9(13) yes
C5 9_555 N1 . C6 . 118.9(13) yes
C6 9_555 N1 . C6 . 140(3) yes
Zn1 . N1 . C5 . 109.3(9) yes
Zn1 . N1 . C4 . 108.4(13) yes
C5 . N1 . C4 . 40.0(10) yes
Zn1 . N1 . C6 . 110.0(13) yes
C5 . N1 . C6 . 44.8(10) yes
C4 . N1 . C6 . 83.8(6) yes
C5 14_556 C5 . N1 . 109.3(9) yes
C5 14_556 C5 . H62 5_555 107.1 no
N1 . C5 . H62 5_555 104.3 no
C5 14_556 C5 . H42 9_555 113.7 no
N1 . C5 . H42 9_555 111.8 no
H62 5_555 C5 . H42 9_555 110.0 no
C5 14_556 C5 . C5 9_555 90.000(7) yes
N1 . C5 . C5 9_555 50.6(10) yes
H62 5_555 C5 . C5 9_555 154.0 no
H42 9_555 C5 . C5 9_555 79.1 no
C5 14_556 C5 . H61 . 108.0 no
N1 . C5 . H61 . 113.6 no
H62 5_555 C5 . H61 . 11.1 no
H42 9_555 C5 . H61 . 100.2 no
C5 9_555 C5 . H61 . 160.3 no
C5 14_556 C5 . H51 . 109.9 no
N1 . C5 . H51 . 108.3 no
H62 5_555 C5 . H51 . 6.6 no
H42 9_555 C5 . H51 . 103.5 no
C5 9_555 C5 . H51 . 156.1 no
C5 14_556 C5 . H52 . 110.2 no
N1 . C5 . H52 . 109.1 no
H62 5_555 C5 . H52 . 116.5 no
H42 9_555 C5 . H52 . 6.5 no
C5 9_555 C5 . H52 . 73.3 no
C5 14_556 C5 . H41 . 113.9 no
N1 . C5 . H41 . 113.4 no
H62 5_555 C5 . H41 . 108.1 no
H42 9_555 C5 . H41 . 2.1 no
C5 9_555 C5 . H41 . 81.2 no
H61 . C5 . H51 . 5.4 no
H61 . C5 . H52 . 106.7 no
H51 . C5 . H52 . 110.1 no
H61 . C5 . H41 . 98.2 no
H51 . C5 . H41 . 101.6 no
H52 . C5 . H41 . 8.5 no
C4 6_556 C4 . N1 . 108.4(13) yes
C4 6_556 C4 . H41 9_555 111.0 no
N1 . C4 . H41 9_555 108.3 no
C4 6_556 C4 . H42 9_555 110.8 no
N1 . C4 . H42 9_555 107.3 no
H41 9_555 C4 . H42 9_555 110.8 no
C4 6_556 C4 . H52 9_555 111.7 no
N1 . C4 . H52 9_555 116.5 no
H41 9_555 C4 . H52 9_555 10.0 no
H42 9_555 C4 . H52 9_555 101.9 no
C4 6_556 C4 . H52 . 111.7 no
N1 . C4 . H52 . 116.5 no
H41 9_555 C4 . H52 . 100.7 no
H42 9_555 C4 . H52 . 11.3 no
H52 9_555 C4 . H52 . 91.5 no
C4 6_556 C4 . H41 . 111.0 no
N1 . C4 . H41 . 108.3 no
H41 9_555 C4 . H41 . 109.7 no
H42 9_555 C4 . H41 . 1.3 no
H52 9_555 C4 . H41 . 100.7 no
C4 6_556 C4 . H42 . 110.8 no
N1 . C4 . H42 . 107.3 no
H41 9_555 C4 . H42 . 1.3 no
H42 9_555 C4 . H42 . 112.0 no
H52 9_555 C4 . H42 . 11.3 no
H52 . C4 . H41 . 10.0 no
H52 . C4 . H42 . 101.9 no
H41 . C4 . H42 . 110.8 no
C8 6_555 C7 . C8 . 119(5) yes
C8 6_555 C7 . H71 . 120.3 no
C8 . C7 . H71 . 120.3 no
C8 5_655 C8 . C7 . 120(2) yes
C8 5_655 C8 . H81 . 119.3 no
C7 . C8 . H81 . 120.4 no
C10 5_655 C9 . C10 . 119.9(8) yes
C10 5_655 C9 . H91 . 120.1 no
C10 . C9 . H91 . 120.1 no
C10 14_556 C10 . C9 . 120.1(4) yes
C10 14_556 C10 . H101 . 120.0 no
C9 . C10 . H101 . 120.0 no
C6 10_556 C6 . H61 5_555 107.0 no
C6 10_556 C6 . N1 . 110.0(13) yes
H61 5_555 C6 . N1 . 108.7 no
C6 10_556 C6 . H51 5_555 110.3 no
H61 5_555 C6 . H51 5_555 3.6 no
N1 . C6 . H51 5_555 108.4 no
C6 10_556 C6 . H62 5_555 110.2 no
H61 5_555 C6 . H62 5_555 108.6 no
N1 . C6 . H62 5_555 112.2 no
H51 5_555 C6 . H62 5_555 105.8 no
C6 10_556 C6 . H61 . 107.0 no
H61 5_555 C6 . H61 . 115.4 no
N1 . C6 . H61 . 108.7 no
H51 5_555 C6 . H61 . 112.5 no
H62 5_555 C6 . H61 . 6.7 no
C6 10_556 C6 . H62 . 110.2 no
H61 5_555 C6 . H62 . 6.7 no
N1 . C6 . H62 . 112.2 no
H51 5_555 C6 . H62 . 4.4 no
H62 5_555 C6 . H62 . 101.9 no
C6 10_556 C6 . H51 . 110.3 no
H61 5_555 C6 . H51 . 112.5 no
N1 . C6 . H51 . 108.4 no
H51 5_555 C6 . H51 . 109.5 no
H62 5_555 C6 . H51 . 4.4 no
H61 . C6 . H62 . 108.6 no
H61 . C6 . H51 . 3.6 no
H62 . C6 . H51 . 105.8 no
C6 . H61 . C5 . 66.7 no
C5 5_555 H62 . C6 . 71.2 no
C6 . H51 . C5 . 69.0 no
C5 . H52 . C4 . 63.2 no
C4 . H41 . C5 . 64.7 no
C4 . H42 . C5 9_555 68.1 no



# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
0 0 2 x .
3 1 0 x .
3 1 1 x .
8 10 7 x .
14 6 2 x .
14 6 1 x .
1 17 4 x .
13 5 2 x .
5 7 8 x .
2 0 7 x .
3 1 9 x .
4 2 10 x .
4 0 9 x .
12 6 0 x .
3 3 10 x .
11 5 0 x .
# looking for ARCHIVE-HKL.CIF 

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

data_2_DMF_033GPa
_database_code_depnum_ccdc_archive 'CCDC 2087895'
loop_
_audit_author_name
_audit_author_address
'Stephen Moggach'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2021-06-03 deposited with the CCDC.	2021-09-29 downloaded from the CCDC.
;
_audit_creation_date             2021-05-26
_audit_creation_method           CRYSTALS_ver_14.61_build_6999

_refine_special_details          
; 
029_ALERT_3_A _diffrn_measured_fraction_theta_full value Low .      0.837 Why?
911_ALERT_3_B Missing FCF Refl Between Thmin & STh/L=    0.600        143 Report
913_ALERT_3_C Missing # of Very Strong Reflections in FCF ....          9 Note

These are caused by shading from the pressure cell.

430_ALERT_2_A Short Inter D...A Contact  O1       ..O1       .       2.25 Ang.
                                                    x,y,1-z  =      6_556 Check
430_ALERT_2_B Short Inter D...A Contact  O1       ..O1       .       2.60 Ang.
                                                   x,-y,1-z  =     10_556 Check
430_ALERT_2_C Short Inter D...A Contact  O1       ..O1       .       2.87 Ang.
                                                    y,x,1-z  =     16_556 Check
													
This is cauded by disordered DMF.
													
601_ALERT_2_A Unit Cell Contains Solvent Accessible VOIDS of .        513 Ang**3
049_ALERT_1_B Calculated Density Less Than 1.0 gcm-3 .........     0.8602 Check

These are correct.

922_ALERT_1_A wR2 in the CIF and FCF Differ by ...............     0.2457 Check
921_ALERT_1_B R1  in the CIF and FCF Differ by ...............     0.0481 Check

Reflections that overlap with W-gasket, or have poor correlations within 
2 degrees of the half-opening angle of the cell have been removed, 
causing the above alert. These were removed after data processing, 
as a number of strong reflections were measures well close to W-rings
that we wanted to include in the refinement.

084_ALERT_3_B High wR2 Value (i.e. > 0.25) ...................       0.45 Report
076_ALERT_1_C Occupancy      0.500 Less Than 1.0 for Sp.pos  .           C1
076_ALERT_1_C Occupancy      0.500 Less Than 1.0 for Sp.pos  .           C2
082_ALERT_2_C High R1 Value ..................................       0.12 Report
094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       2.20 Report
242_ALERT_2_C Low    'MainMol' Ueq as Compared to Neighbors of         N1 Check

These are all caused by disorder on the DABCO ligand.

992_ALERT_5_B Repd & Actual _reflns_number_gt Values Differ by         37 Check

This has been checked.

#===============================================================================
002_ALERT_2_G Number of Distance or Angle Restraints on AtSite          7 Note
003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...          7 Report
072_ALERT_2_G SHELXL First  Parameter in WGHT  Unusually Large       0.17 Report
092_ALERT_4_G Check: Wavelength Given is not Cu,Ga,Mo,Ag,In Ka    0.48590 Ang.
300_ALERT_4_G Atom Site Occupancy of O1         Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of C1         Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of C2         Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of C3         Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of C4         Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of C5         Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H32        Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of H41        Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H51        Constrained at      0.375 Check
301_ALERT_3_G Main Residue  Disorder ..............(Resd  1  )        92% Note
432_ALERT_2_G Short Inter X...Y Contact  C1       ..C3               2.49 Ang.
                                                    x,y,1-z  =      6_556 Check
432_ALERT_2_G Short Inter X...Y Contact  C1       ..C3               3.00 Ang.
                                                   x,-y,1-z  =     10_556 Check
432_ALERT_2_G Short Inter X...Y Contact  C2       ..C3               1.38 Ang.
                                                    x,y,1-z  =      6_556 Check
432_ALERT_2_G Short Inter X...Y Contact  C2       ..C3               2.31 Ang.
                                                   x,-y,1-z  =     10_556 Check
432_ALERT_2_G Short Inter X...Y Contact  C2       ..C3               2.41 Ang.
                                                  1-x,y,1-z  =     14_656 Check
432_ALERT_2_G Short Inter X...Y Contact  C2       ..C3               2.41 Ang.
                                                    1-x,y,z  =      9_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C2       ..C2               2.79 Ang.
                                                    1-x,y,z  =      9_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C2       ..C3               3.04 Ang.
                                                 1-x,-y,1-z  =      2_656 Check
432_ALERT_2_G Short Inter X...Y Contact  C2       ..C3               3.04 Ang.
                                                   1-x,-y,z  =      5_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C3       ..C3               1.40 Ang.
                                                    1-x,y,z  =      9_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C3       ..C3               2.34 Ang.
                                                   1-x,-y,z  =      5_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C3       ..C3               2.38 Ang.
                                                    x,y,1-z  =      6_556 Check
432_ALERT_2_G Short Inter X...Y Contact  C3       ..C3               2.77 Ang.
                                                  1-x,y,1-z  =     14_656 Check
432_ALERT_2_G Short Inter X...Y Contact  C3       ..C3               3.03 Ang.
                                                   x,-y,1-z  =     10_556 Check
760_ALERT_1_G CIF Contains no Torsion Angles .................          ? Info
769_ALERT_4_G CIF Embedded explicitly supplied scattering data     Please Note
773_ALERT_2_G Check long C-C Bond in CIF: C2       --C2              1.82 Ang.
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      42.09 Deg.
              C5   -N1   -C4      5_555   1_555   7_555 ......     #   26 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      42.09 Deg.
              C5   -N1   -C4      7_555   1_555   7_555 ......     #   27 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      42.09 Deg.
              C5   -N1   -C4     15_555   1_555   3_555 ......     #   28 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      42.09 Deg.
              C5   -N1   -C4     15_555   1_555   5_555 ......     #   32 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      42.09 Deg.
              C5   -N1   -C4      5_555   1_555   5_555 ......     #   33 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      42.09 Deg.
              C5   -N1   -C4      7_555   1_555   1_555 ......     #   39 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      42.09 Deg.
              C4   -N1   -C5      3_555   1_555   1_555 ......     #   46 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      42.09 Deg.
              C4   -N1   -C5      1_555   1_555   1_555 ......     #   54 Check
811_ALERT_5_G No ADDSYM Analysis: Too Many Excluded Atoms ....          ! Info
860_ALERT_3_G Number of Least-Squares Restraints .............        167 Note
910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min).          4 Note
912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600         13 Note
#===============================================================================

No action taken.
;

_cell_length_a                   10.6890(6)
_cell_length_b                   10.6890(6)
_cell_length_c                   9.6506(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1102.63(14)

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P 4/m m m '
_symmetry_space_group_name_Hall  '-P 4 2'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-y,x,z
y,-x,-z
-x,-y,z
x,y,-z
y,-x,z
-y,x,-z
-x,y,z
x,-y,-z
y,x,z
-y,-x,-z
x,-y,z
-x,y,-z
-y,-x,z
y,x,-z

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 0.0006 0.0007 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 0.0016 0.0014 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 0.0036 0.0026 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 0.3043 0.7253 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            1

# Given Formula = C40 H30 N10 O20 Zn8 
# Dc =      2.25 Fooo =    740.00 Mu =     43.72 M =   1493.77
# Found Formula = C22 H20 N2 O8 Zn2 
# Dc =      0.86 FOOO =    290.00 Mu =     11.14 M =    571.17

_chemical_formula_sum            'C34 H48 N6 O12 Zn2'
_chemical_formula_moiety         '(C22 H20 N2 O8 Zn2)n. 4(C3H7NO)'
_chemical_compound_source        .
_chemical_formula_weight         863.55

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 -0.024 0.478 -0.013 502 158 '4(C3H7NO) '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
see text for details
;

_cell_measurement_reflns_used    4883
_cell_measurement_theta_min      2
_cell_measurement_theta_max      17
_cell_measurement_temperature    298

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.050
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.150

_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1800
_exptl_absorpt_coefficient_mu    1.114

# Sheldrick geometric approximatio 0.85 0.95 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_T_max  0.95
_diffrn_measurement_device_type  Synchrotron
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.48590
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      298
_diffrn_ambient_pressure         330000
_diffrn_reflns_number            5314
_diffrn_reflns_av_unetI/netI     0.130
_reflns_number_total             600
_diffrn_reflns_av_R_equivalents  0.093
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 600 
# Theoretical number of reflections is about 1129 


_diffrn_reflns_theta_min         2.340
_diffrn_reflns_theta_max         17.687
_diffrn_measured_fraction_theta_max 0.837

_diffrn_reflns_theta_full        17.687
_diffrn_measured_fraction_theta_full 0.837


_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_reflns_limit_h_min              0
_reflns_limit_h_max              8
_reflns_limit_k_min              0
_reflns_limit_k_max              13
_reflns_limit_l_min              0
_reflns_limit_l_max              12

_oxford_diffrn_Wilson_B_factor   1.77
_oxford_diffrn_Wilson_scale      17.49

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

_refine_diff_density_min         -0.79
_refine_diff_density_max         1.74


# 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_refine_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_restraints     167
_refine_ls_number_parameters     51
_refine_ls_number_reflns         557
_oxford_refine_ls_R_factor_ref   0.0800
_refine_ls_wR_factor_ref         0.2030
_refine_ls_goodness_of_fit_ref   1.0063
_refine_ls_shift/su_max          0.0001492
_refine_ls_shift/su_mean         0.0000141


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        600
_refine_ls_R_factor_all          0.1292
_refine_ls_wR_factor_all         0.4487

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                506
_refine_ls_R_factor_gt           0.1169
_refine_ls_wR_factor_gt          0.4331


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.17P)² + 0.75P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

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

# Replace last . with number of unfound hydrogen atoms attached 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 0.0000 0.0000 0.65366(12) 0.0271 1.0000 Uani S T . . . .
N1 N 0.0000 0.0000 0.8674(9) 0.0286 1.0000 Uani DS TU . . . .
O1 O 0.1779(6) 0.0608(6) 0.6167(6) 0.0461 0.5000 Uani D U . . . .
C1 C 0.2304(8) 0.0702(7) 0.5000 0.0447 0.5000 Uani DS TU . . . .
C2 C 0.3695(6) 0.0853(7) 0.5000 0.0406 0.5000 Uani DS TU . . . .
C3 C 0.4345(4) 0.0876(7) 0.6235(6) 0.0424 0.5000 Uani D U . . . .
C4 C -0.0913(4) -0.0913(4) 0.9202(5) 0.0564 0.3750 Uani DS TU . . . .
C5 C 0.0000 -0.1291(8) 0.9200(4) 0.0550 0.3750 Uani DS TU . . . .
H32 H 0.3909 0.0804 0.7089 0.0498 0.5000 Uiso R . . . . .
H41 H -0.1740 -0.0693 0.8869 0.0680 0.3750 Uiso R . . . . .
H51 H 0.0741 -0.1722 0.8869 0.0651 0.3750 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.546(6)
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 . Zn1 2_556 2.966(2) yes
Zn1 . O1 3_555 2.041(6) yes
Zn1 . O1 11_555 2.041(6) yes
Zn1 . O1 13_555 2.041(6) yes
Zn1 . O1 9_555 2.041(6) yes
Zn1 . O1 . 2.041(6) yes
Zn1 . N1 . 2.063(9) yes
N1 . C5 15_555 1.471(8) yes
N1 . C5 5_555 1.471(8) yes
N1 . C5 7_555 1.471(8) yes
N1 . C4 7_555 1.471(4) yes
N1 . C4 3_555 1.471(4) yes
N1 . C4 5_555 1.471(4) yes
N1 . C4 . 1.471(4) yes
N1 . C5 . 1.471(8) yes
O1 . O1 11_555 1.771(13) yes
O1 . O1 13_555 1.300(12) yes
O1 . C1 . 1.262(6) yes
C1 . C1 13_555 1.501(16) yes
C1 . C2 . 1.496(8) yes
C2 . C3 6_556 1.380(5) yes
C2 . C2 10_556 1.823(15) yes
C2 . C3 . 1.380(5) yes
C3 . C3 9_655 1.400(8) yes
C3 . H32 . 0.950 no
C4 . C4 6_557 1.541(9) yes
C4 . H41 11_555 0.970 no
C4 . H41 . 0.970 no
C5 . C5 6_557 1.544(9) yes
C5 . H51 9_555 0.970 no
C5 . H51 . 0.970 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
Zn1 2_556 Zn1 . O1 3_555 79.93(16) yes
Zn1 2_556 Zn1 . O1 11_555 79.93(16) yes
O1 3_555 Zn1 . O1 11_555 37.1(3) yes
Zn1 2_556 Zn1 . O1 13_555 79.93(16) yes
O1 3_555 Zn1 . O1 13_555 124.2(3) yes
O1 11_555 Zn1 . O1 13_555 88.25(6) yes
Zn1 2_556 Zn1 . O1 9_555 79.93(16) yes
O1 3_555 Zn1 . O1 9_555 51.4(3) yes
O1 11_555 Zn1 . O1 9_555 88.25(5) yes
O1 13_555 Zn1 . O1 9_555 159.9(3) yes
Zn1 2_556 Zn1 . O1 . 79.93(16) yes
O1 3_555 Zn1 . O1 . 88.25(5) yes
O1 11_555 Zn1 . O1 . 51.4(3) yes
O1 13_555 Zn1 . O1 . 37.1(3) yes
O1 9_555 Zn1 . O1 . 137.4(3) yes
Zn1 2_556 Zn1 . N1 . 179.99 yes
O1 3_555 Zn1 . N1 . 100.07(16) yes
O1 11_555 Zn1 . N1 . 100.07(16) yes
O1 13_555 Zn1 . N1 . 100.07(16) yes
O1 9_555 Zn1 . N1 . 100.07(16) yes
O1 . Zn1 . N1 . 100.07(16) yes
C5 15_555 N1 . C5 5_555 83.2(3) yes
C5 15_555 N1 . C5 7_555 139.6(8) yes
C5 5_555 N1 . C5 7_555 83.2(3) yes
C5 15_555 N1 . C4 7_555 120.2(5) yes
C5 5_555 N1 . C4 7_555 42.09(11) yes
C5 7_555 N1 . C4 7_555 42.09(11) yes
C5 15_555 N1 . C4 3_555 42.09(11) yes
C5 5_555 N1 . C4 3_555 120.2(5) yes
C5 7_555 N1 . C4 3_555 120.2(5) yes
C4 7_555 N1 . C4 3_555 139.5(8) yes
C5 15_555 N1 . C4 5_555 42.09(11) yes
C5 5_555 N1 . C4 5_555 42.09(11) yes
C5 7_555 N1 . C4 5_555 120.2(5) yes
C4 7_555 N1 . C4 5_555 83.1(3) yes
C4 3_555 N1 . C4 5_555 83.1(3) yes
C5 15_555 N1 . C4 . 120.2(5) yes
C5 5_555 N1 . C4 . 120.2(5) yes
C5 7_555 N1 . C4 . 42.09(11) yes
C4 7_555 N1 . C4 . 83.1(3) yes
C4 3_555 N1 . C4 . 83.1(3) yes
C5 15_555 N1 . C5 . 83.2(3) yes
C5 5_555 N1 . C5 . 139.6(8) yes
C5 7_555 N1 . C5 . 83.2(3) yes
C4 7_555 N1 . C5 . 120.2(5) yes
C4 3_555 N1 . C5 . 42.09(11) yes
C5 15_555 N1 . Zn1 . 110.2(4) yes
C5 5_555 N1 . Zn1 . 110.2(4) yes
C5 7_555 N1 . Zn1 . 110.2(4) yes
C4 7_555 N1 . Zn1 . 110.3(4) yes
C4 3_555 N1 . Zn1 . 110.3(4) yes
C4 5_555 N1 . C4 . 139.5(8) yes
C4 5_555 N1 . C5 . 120.2(5) yes
C4 . N1 . C5 . 42.09(11) yes
C4 5_555 N1 . Zn1 . 110.3(4) yes
C4 . N1 . Zn1 . 110.3(4) yes
C5 . N1 . Zn1 . 110.2(4) yes
O1 11_555 O1 . O1 13_555 135.000(3) yes
O1 11_555 O1 . Zn1 . 64.30(17) yes
O1 13_555 O1 . Zn1 . 71.44(17) yes
O1 11_555 O1 . C1 . 104.9(4) yes
O1 13_555 O1 . C1 . 94.6(4) yes
Zn1 . O1 . C1 . 126.5(5) yes
C1 13_555 C1 . O1 6_556 85.4(4) yes
C1 13_555 C1 . O1 . 85.4(4) yes
O1 6_556 C1 . O1 . 126.4(8) yes
C1 13_555 C1 . C2 . 96.2(4) yes
O1 6_556 C1 . C2 . 116.8(4) yes
O1 . C1 . C2 . 116.8(4) yes
C1 . C2 . C3 6_556 120.2(3) yes
C1 . C2 . C2 10_556 83.8(4) yes
C3 6_556 C2 . C2 10_556 91.0(4) yes
C1 . C2 . C3 . 120.2(3) yes
C3 6_556 C2 . C3 . 119.5(6) yes
C2 10_556 C2 . C3 . 91.0(4) yes
C3 9_655 C3 . C2 . 120.2(3) yes
C3 9_655 C3 . H32 . 119.4 no
C2 . C3 . H32 . 120.1 no
C4 6_557 C4 . N1 . 110.3(4) yes
C4 6_557 C4 . H41 11_555 109.3 no
N1 . C4 . H41 11_555 109.2 no
C4 6_557 C4 . H41 . 109.3 no
N1 . C4 . H41 . 109.2 no
H41 11_555 C4 . H41 . 109.5 no
C5 6_557 C5 . N1 . 110.2(4) yes
C5 6_557 C5 . H51 9_555 109.2 no
N1 . C5 . H51 9_555 109.3 no
C5 6_557 C5 . H51 . 109.2 no
N1 . C5 . H51 . 109.3 no
H51 9_555 C5 . H51 . 109.5 no



# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
1 2 1 x .
1 2 8 x .
1 2 3 x .
0 2 2 x .
1 1 4 x .
7 8 4 x .
7 7 5 x .
7 7 6 x .
1 1 8 x .
1 6 5 x .
1 3 8 x .
0 3 8 x .
2 6 5 x .
1 4 2 x .
2 2 1 x .
0 6 5 x .
3 6 5 x .
2 4 1 x .
0 3 1 x .
0 3 2 x .
0 1 6 x .
2 6 2 x .
0 8 0 x .
8 8 6 x .
5 6 6 x .
7 9 6 x .
2 4 2 x .
1 4 8 x .
0 1 9 x .
7 10 4 x .
6 8 2 x .
5 8 1 x .
7 7 8 x .
1 1 6 x .
4 6 8 x .
6 7 8 x .
0 4 1 x .
2 6 6 x .
1 1 2 x .
0 3 0 x .
6 7 4 x .
1 3 2 x .
4 4 6 x .
# looking for ARCHIVE-HKL.CIF 

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

data_3_Ben_020GPa
_database_code_depnum_ccdc_archive 'CCDC 2087897'
loop_
_audit_author_name
_audit_author_address
'Stephen Moggach'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2021-06-03 deposited with the CCDC.	2021-09-29 downloaded from the CCDC.
;
_audit_creation_date             2021-05-26
_audit_creation_method           CRYSTALS_ver_14.61_build_6999

_refine_special_details          
; 
023_ALERT_3_A Resolution (too) Low [sin(theta)/Lambda < 0.6]..       0.53 Ang-1
027_ALERT_3_A _diffrn_reflns_theta_full value (too) Low ......      17.15 Degree
029_ALERT_3_A _diffrn_measured_fraction_theta_full value Low .      0.636 Why?
341_ALERT_3_B Low Bond Precision on  C-C Bonds ...............    0.02404 Ang.
911_ALERT_3_B Missing FCF Refl Between Thmin & STh/L=    0.527        258 Report
088_ALERT_3_C Poor Data / Parameter Ratio ....................       8.98 Note
910_ALERT_3_C Missing # of FCF Reflection(s) Below Theta(Min).          5 Note

These are caused by shading from the pressure cell.

601_ALERT_2_A Unit Cell Contains Solvent Accessible VOIDS of .        204 Ang**3

This is correct.

082_ALERT_2_C High R1 Value ..................................       0.11 Report
084_ALERT_3_B High wR2 Value (i.e. > 0.25) ...................       0.36 Report
076_ALERT_1_C Occupancy      0.500 Less Than 1.0 for Sp.pos  .           C9
076_ALERT_1_C Occupancy      0.500 Less Than 1.0 for Sp.pos  .          H91
260_ALERT_2_C Large Average Ueq of Residue Including        C7      0.173 Check
701_ALERT_1_C Bond    Calc   1.4880(3), Rep   1.4876(2), Dev..       1.33 Sigma
              C1       -C2              1_555   1_555 ........     #    8 Check

These are all caused by disorder in the DABCO and partial occupancy of included 
benzene solvent molecules.



#===============================================================================
002_ALERT_2_G Number of Distance or Angle Restraints on AtSite         12 Note
003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...         12 Report
004_ALERT_5_G Polymeric Structure Found with Maximum Dimension          3 Info
042_ALERT_1_G Calc. and Reported Moiety Formula Strings Differ     Please Check
045_ALERT_1_G Calculated and Reported Z Differ by a Factor ...       2.00 Check
072_ALERT_2_G SHELXL First  Parameter in WGHT  Unusually Large       0.12 Report
093_ALERT_1_G No s.u.'s on H-positions, Refinement Reported as      mixed Check
300_ALERT_4_G Atom Site Occupancy of C4         Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of C5         Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of C6         Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H41        Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H42        Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H51        Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H52        Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H61        Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H62        Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of C9         Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of C10        Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of H91        Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of H101       Constrained at        0.5 Check
301_ALERT_3_G Main Residue  Disorder ..............(Resd  1  )        20% Note
302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd  3  )       100% Note
432_ALERT_2_G Short Inter X...Y Contact  C9       ..C10              1.35 Ang.
                                                    1-x,y,z  =      5_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C9       ..C10              2.38 Ang.
                                                    x,y,1-z  =     14_556 Check
432_ALERT_2_G Short Inter X...Y Contact  C9       ..C10              2.38 Ang.
                                                  1-x,y,1-z  =     10_656 Check
432_ALERT_2_G Short Inter X...Y Contact  C9       ..C9               2.75 Ang.
                                                  1-x,y,1-z  =     10_656 Check
432_ALERT_2_G Short Inter X...Y Contact  C10      ..C10              1.39 Ang.
                                                    x,y,1-z  =     14_556 Check
432_ALERT_2_G Short Inter X...Y Contact  C10      ..C10              2.34 Ang.
                                                    1-x,y,z  =      5_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C10      ..C10              2.73 Ang.
                                                  1-x,y,1-z  =     10_656 Check
760_ALERT_1_G CIF Contains no Torsion Angles .................          ? Info
769_ALERT_4_G CIF Embedded explicitly supplied scattering data     Please Note
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.20 Deg.
              C4   -N1   -C5      5_555   1_555   5_555 ......     #   26 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.20 Deg.
              C4   -N1   -C5      5_555   1_555  13_555 ......     #   29 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      42.30 Deg.
              C5   -N1   -C6      9_555   1_555   9_555 ......     #   34 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      42.30 Deg.
              C5   -N1   -C6     13_555   1_555   9_555 ......     #   35 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.20 Deg.
              C5   -N1   -C4      9_555   1_555   1_555 ......     #   48 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      42.30 Deg.
              C5   -N1   -C6      5_555   1_555   1_555 ......     #   52 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.20 Deg.
              C5   -N1   -C4      1_555   1_555   1_555 ......     #   58 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      42.30 Deg.
              C5   -N1   -C6      1_555   1_555   1_555 ......     #   60 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       2.20 Deg.
              H61  -C5   -H62     5_555   1_555   1_555 ......     #   71 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       5.30 Deg.
              H42  -C5   -H51     9_555   1_555   1_555 ......     #   74 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       3.00 Deg.
              H61  -C5   -H52     5_555   1_555   1_555 ......     #   80 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       5.00 Deg.
              H62  -C5   -H52     1_555   1_555   1_555 ......     #   81 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       1.50 Deg.
              H42  -C5   -H41     9_555   1_555   1_555 ......     #   84 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       3.80 Deg.
              H51  -C5   -H41     1_555   1_555   1_555 ......     #   88 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       4.50 Deg.
              H41  -C4   -H51     9_555   1_555   9_555 ......     #   99 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       4.30 Deg.
              H42  -C4   -H51     9_555   1_555   1_555 ......     #  102 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       0.60 Deg.
              H42  -C4   -H41     9_555   1_555   1_555 ......     #  107 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       0.60 Deg.
              H41  -C4   -H42     9_555   1_555   1_555 ......     #  113 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       4.30 Deg.
              H51  -C4   -H42     9_555   1_555   1_555 ......     #  114 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       4.50 Deg.
              H51  -C4   -H41     1_555   1_555   1_555 ......     #  115 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       7.00 Deg.
              H62  -C6   -H52     5_555   1_555   5_555 ......     #  138 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       1.20 Deg.
              H62  -C6   -H61     5_555   1_555   1_555 ......     #  142 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       5.90 Deg.
              H52  -C6   -H61     5_555   1_555   1_555 ......     #  144 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       1.20 Deg.
              H61  -C6   -H62     5_555   1_555   1_555 ......     #  148 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       5.90 Deg.
              H61  -C6   -H52     5_555   1_555   1_555 ......     #  153 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       7.00 Deg.
              H62  -C6   -H52     1_555   1_555   1_555 ......     #  157 Check
809_ALERT_1_G Can not Parse the SHELXL Weighting Scheme String     Please Check
860_ALERT_3_G Number of Least-Squares Restraints .............        144 Note
909_ALERT_3_G Percentage of I>2sig(I) Data at Theta(Max) Still        52% Note
929_ALERT_5_G No Weight Pars,Obs and Calc R1,wR2,S not Checked          ! Info
956_ALERT_1_G Calculated (ThMax) and Actual (FCF) Hmax Differ           3 Units
960_ALERT_3_G Number of Intensities with I  <   - 2*sig(I) ...          1 Check
992_ALERT_5_G Repd & Actual _reflns_number_gt Values Differ by          3 Check
#===============================================================================

No action taken.
;

_cell_length_a                   13.575(3)
_cell_length_b                   16.993(3)
_cell_length_c                   9.6680(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2230.3(7)

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'C m m m '
_symmetry_space_group_name_Hall  '-C 2 2 '
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
x,-y,-z
-x+1/2,y+1/2,z
x+1/2,-y+1/2,-z
x,-y,z
-x,y,-z
x+1/2,-y+1/2,z
-x+1/2,y+1/2,-z
-x,-y,z
x,y,-z
-x+1/2,-y+1/2,z
x+1/2,y+1/2,-z

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            2

# Given Formula = C40 H30 N10 O3 Zn10 
# Dc =      2.01 Fooo =   1328.00 Mu =     53.24 M =   1352.54
# Found Formula = C34 H38 N2 O8 Zn2 
# Dc =      1.09 FOOO =    760.00 Mu =     11.15 M =    733.44

_chemical_formula_sum            'C34 H38 N2 O8 Zn2'
_chemical_formula_moiety         '(C22 H20 N2 O8 Zn2)n . 2 (C6 H6)'
_chemical_compound_source        .
_chemical_formula_weight         733.44


_cell_measurement_reflns_used    1166
_cell_measurement_theta_min      3
_cell_measurement_theta_max      22
_cell_measurement_temperature    298

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.050
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.150

_exptl_crystal_density_diffrn    1.092
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             760
_exptl_absorpt_coefficient_mu    1.115

# Sheldrick geometric approximatio 0.85 0.95 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_T_max  0.95
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      298
_diffrn_ambient_pressure         200000
_diffrn_reflns_number            2039
_diffrn_reflns_av_unetI/netI     0.118
_reflns_number_total             490
_diffrn_reflns_av_R_equivalents  0.082
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 490 
# Theoretical number of reflections is about 1365 


_diffrn_reflns_theta_min         3.192
_diffrn_reflns_theta_max         21.984
_diffrn_measured_fraction_theta_max 0.606

_diffrn_reflns_theta_full        17.148
_diffrn_measured_fraction_theta_full 0.636


_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_reflns_limit_h_min              0
_reflns_limit_h_max              11
_reflns_limit_k_min              0
_reflns_limit_k_max              16
_reflns_limit_l_min              0
_reflns_limit_l_max              9

_oxford_diffrn_Wilson_B_factor   1.81
_oxford_diffrn_Wilson_scale      401.04

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

_refine_diff_density_min         -0.97
_refine_diff_density_max         1.16


# 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_refine_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_restraints     144
_refine_ls_number_parameters     54
_refine_ls_number_reflns         485
_oxford_refine_ls_R_factor_ref   0.1417
_refine_ls_wR_factor_ref         0.2867
_refine_ls_goodness_of_fit_ref   1.0149
_refine_ls_shift/su_max          0.0194589
_refine_ls_shift/su_mean         0.0006051


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        490
_refine_ls_R_factor_all          0.1522
_refine_ls_wR_factor_all         0.3634

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                351
_refine_ls_R_factor_gt           0.1134
_refine_ls_wR_factor_gt          0.3289


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    mixed #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.12P)² +*****P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

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

# Replace last . with number of unfound hydrogen atoms attached 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 0.0000 0.0000 0.1523(3) 0.0367 1.0000 Uani S T . . . .
O1 O 0.0987(9) 0.0857(6) 0.1211(9) 0.0520 1.0000 Uani D U . . . .
C1 C 0.1244 0.1127 0.0000 0.0514 1.0000 Uani D U . . . .
C2 C 0.1933 0.1808 0.0000 0.0491 1.0000 Uani D U . . . .
C3 C 0.2172(15) 0.2186(10) 0.1227(12) 0.0650 1.0000 Uani D U . . . .
N1 N 0.0000 0.0000 0.3668(19) 0.0314 1.0000 Uani DS TU . . . .
C5 C 0.071(2) 0.0552(18) 0.4212(4) 0.0350 0.3750 Uani D U . . . .
C4 C 0.102(3) 0.0000 0.4213(5) 0.0350 0.3750 Uani DS U . . . .
C7 C 0.410(5) -0.0000 0.0000 0.1701 1.0000 Uani DS U . . . .
C8 C 0.4490(14) 0.074(2) -0.0000 0.1751 1.0000 Uani DS TU . . . .
C9 C 0.5000 0.2003(5) 0.358(3) 0.30(4) 0.5000 Uiso DS U . . . .
C10 C 0.5863(19) 0.2002(3) 0.428(2) 0.30(4) 0.5000 Uiso D U . . . .
C6 C -0.0000 0.0775(19) 0.4212(5) 0.0333 0.3750 Uani DS U . . . .
H31 H 0.1925 0.1986 0.2075 0.0745 1.0000 Uiso R . . . . .
H71 H 0.3407 -0.0000 0.0000 0.2328 1.0000 Uiso RS . . . . .
H81 H 0.4150 0.1231 -0.0000 0.2360 1.0000 Uiso RS . . . . .
H61 H -0.0565 0.1035 0.3890 0.0403 0.3750 Uiso R . . . . .
H62 H 0.0590 0.1035 0.3890 0.0403 0.3750 Uiso R . . . . .
H51 H 0.1356 0.0420 0.3889 0.0396 0.3750 Uiso R . . . . .
H52 H 0.0520 0.1079 0.3889 0.0396 0.3750 Uiso . . . . . .
H41 H 0.1326 0.0461 0.3889 0.0404 0.3750 Uiso . . . . . .
H42 H 0.1339 -0.0474 0.3889 0.0404 0.3750 Uiso R . . . . .
H91 H 0.5000 0.2004 0.2601 0.4088 0.5000 Uiso RS . . . . .
H101 H 0.6470 0.2002 0.3793 0.4089 0.5000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.388(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 . Zn1 2_555 2.945(6) yes
Zn1 . O1 5_555 2.002(10) yes
Zn1 . O1 13_555 2.002(10) yes
Zn1 . O1 9_555 2.002(10) yes
Zn1 . O1 . 2.002(10) yes
Zn1 . N1 . 2.073(19) yes
O1 . C1 . 1.305(9) yes
C1 . C2 . 1.4876(2) yes
C2 . C3 14_555 1.388(11) yes
C2 . C3 . 1.388(11) yes
C3 . C3 15_555 1.39(2) yes
C3 . H31 . 0.948 no
N1 . C4 5_555 1.48(3) yes
N1 . C5 5_555 1.442(8) yes
N1 . C5 9_555 1.442(8) yes
N1 . C5 13_555 1.442(8) yes
N1 . C6 9_555 1.42(3) yes
N1 . C5 . 1.442(8) yes
N1 . C4 . 1.48(3) yes
N1 . C6 . 1.42(3) yes
C5 . C5 14_556 1.523(9) yes
C5 . H42 9_555 0.922 no
C5 . H61 5_555 0.899 no
C5 . H62 . 0.892 no
C5 . H51 . 0.961 no
C5 . H52 . 0.983 no
C5 . H41 . 0.909 no
C4 . C4 14_556 1.523(9) yes
C4 . H42 9_555 0.967 no
C4 . H41 9_555 0.942 no
C4 . H51 9_555 0.904 no
C4 . H51 . 0.904 no
C4 . H41 . 0.942 no
C4 . H42 . 0.967 no
C7 . C8 6_555 1.37(3) yes
C7 . C8 . 1.37(3) yes
C7 . H71 . 0.943 no
C8 . C8 5_655 1.39(4) yes
C8 . H81 . 0.951 no
C9 . C10 5_655 1.35(3) yes
C9 . C10 . 1.35(3) yes
C9 . H91 . 0.950 no
C10 . C10 14_556 1.38(4) yes
C10 . H101 . 0.950 no
C6 . C6 14_556 1.524(9) yes
C6 . H62 5_555 0.966 no
C6 . H61 5_555 0.937 no
C6 . H52 5_555 0.928 no
C6 . H61 . 0.937 no
C6 . H62 . 0.966 no
C6 . H52 . 0.928 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
Zn1 2_555 Zn1 . O1 5_555 81.3(3) yes
Zn1 2_555 Zn1 . O1 13_555 81.3(3) yes
O1 5_555 Zn1 . O1 13_555 93.4(7) yes
Zn1 2_555 Zn1 . O1 9_555 81.3(3) yes
O1 5_555 Zn1 . O1 9_555 162.6(5) yes
O1 13_555 Zn1 . O1 9_555 84.0(7) yes
Zn1 2_555 Zn1 . O1 . 81.3(3) yes
O1 5_555 Zn1 . O1 . 84.0(7) yes
O1 13_555 Zn1 . O1 . 162.6(5) yes
O1 9_555 Zn1 . O1 . 93.4(7) yes
Zn1 2_555 Zn1 . N1 . 179.99 yes
O1 5_555 Zn1 . N1 . 98.7(3) yes
O1 13_555 Zn1 . N1 . 98.7(3) yes
O1 9_555 Zn1 . N1 . 98.7(3) yes
O1 . Zn1 . N1 . 98.7(3) yes
Zn1 . O1 . C1 . 124.8(6) yes
O1 . C1 . O1 14_555 127.6(9) yes
O1 . C1 . C2 . 116.2(4) yes
O1 14_555 C1 . C2 . 116.2(4) yes
C1 . C2 . C3 14_555 120.4(5) yes
C1 . C2 . C3 . 120.4(5) yes
C3 14_555 C2 . C3 . 117.5(10) yes
C3 15_555 C3 . C2 . 120.3(7) yes
C3 15_555 C3 . H31 . 120.1 no
C2 . C3 . H31 . 119.4 no
C4 5_555 N1 . C5 5_555 41.2(16) yes
C4 5_555 N1 . C5 9_555 119.5(17) yes
C5 5_555 N1 . C5 9_555 137.2(17) yes
C4 5_555 N1 . C5 13_555 41.2(16) yes
C5 5_555 N1 . C5 13_555 81(3) yes
C5 9_555 N1 . C5 13_555 84(3) yes
C4 5_555 N1 . C6 9_555 82.4(6) yes
C5 5_555 N1 . C6 9_555 117.9(17) yes
C5 9_555 N1 . C6 9_555 42.3(16) yes
C5 13_555 N1 . C6 9_555 42.3(16) yes
C4 5_555 N1 . Zn1 . 110.9(9) yes
C5 5_555 N1 . Zn1 . 111.4(8) yes
C5 9_555 N1 . Zn1 . 111.4(8) yes
C5 13_555 N1 . Zn1 . 111.4(8) yes
C6 9_555 N1 . Zn1 . 111.8(9) yes
C4 5_555 N1 . C5 . 119.5(17) yes
C5 5_555 N1 . C5 . 84(3) yes
C5 9_555 N1 . C5 . 81(3) yes
C5 13_555 N1 . C5 . 137.2(17) yes
C6 9_555 N1 . C5 . 117.9(17) yes
C4 5_555 N1 . C4 . 138.3(18) yes
C5 5_555 N1 . C4 . 119.5(17) yes
C5 9_555 N1 . C4 . 41.2(16) yes
C5 13_555 N1 . C4 . 119.5(17) yes
C6 9_555 N1 . C4 . 82.4(6) yes
C4 5_555 N1 . C6 . 82.4(6) yes
C5 5_555 N1 . C6 . 42.3(16) yes
C5 9_555 N1 . C6 . 117.9(17) yes
C5 13_555 N1 . C6 . 117.9(17) yes
C6 9_555 N1 . C6 . 136.5(18) yes
Zn1 . N1 . C5 . 111.4(8) yes
Zn1 . N1 . C4 . 110.9(9) yes
C5 . N1 . C4 . 41.2(16) yes
Zn1 . N1 . C6 . 111.8(9) yes
C5 . N1 . C6 . 42.3(16) yes
C4 . N1 . C6 . 82.4(6) yes
C5 14_556 C5 . N1 . 111.4(8) yes
C5 14_556 C5 . H42 9_555 109.8 no
N1 . C5 . H42 9_555 113.7 no
C5 14_556 C5 . H61 5_555 110.3 no
N1 . C5 . H61 5_555 108.9 no
H42 9_555 C5 . H61 5_555 102.3 no
C5 14_556 C5 . H62 . 110.4 no
N1 . C5 . H62 . 110.6 no
H42 9_555 C5 . H62 . 100.3 no
H61 5_555 C5 . H62 . 2.2 no
C5 14_556 C5 . H51 . 109.0 no
N1 . C5 . H51 . 109.9 no
H42 9_555 C5 . H51 . 5.3 no
H61 5_555 C5 . H51 . 107.3 no
H62 . C5 . H51 . 105.3 no
C5 14_556 C5 . H52 . 108.5 no
N1 . C5 . H52 . 107.7 no
H42 9_555 C5 . H52 . 105.3 no
H61 5_555 C5 . H52 . 3.0 no
H62 . C5 . H52 . 5.0 no
C5 14_556 C5 . H41 . 110.1 no
N1 . C5 . H41 . 112.3 no
H42 9_555 C5 . H41 . 1.5 no
H61 5_555 C5 . H41 . 103.6 no
H62 . C5 . H41 . 101.6 no
H51 . C5 . H52 . 110.3 no
H51 . C5 . H41 . 3.8 no
H52 . C5 . H41 . 106.5 no
C4 14_556 C4 . N1 . 110.9(9) yes
C4 14_556 C4 . H42 9_555 108.9 no
N1 . C4 . H42 9_555 107.8 no
C4 14_556 C4 . H41 9_555 109.4 no
N1 . C4 . H41 9_555 107.2 no
H42 9_555 C4 . H41 9_555 112.7 no
C4 14_556 C4 . H51 9_555 110.3 no
N1 . C4 . H51 9_555 110.5 no
H42 9_555 C4 . H51 9_555 108.5 no
H41 9_555 C4 . H51 9_555 4.5 no
C4 14_556 C4 . H51 . 110.3 no
N1 . C4 . H51 . 110.5 no
H42 9_555 C4 . H51 . 4.3 no
H41 9_555 C4 . H51 . 108.5 no
H51 9_555 C4 . H51 . 104.2 no
C4 14_556 C4 . H41 . 109.4 no
N1 . C4 . H41 . 107.2 no
H42 9_555 C4 . H41 . 0.6 no
H41 9_555 C4 . H41 . 112.7 no
H51 9_555 C4 . H41 . 108.5 no
C4 14_556 C4 . H42 . 108.9 no
N1 . C4 . H42 . 107.8 no
H42 9_555 C4 . H42 . 112.7 no
H41 9_555 C4 . H42 . 0.6 no
H51 9_555 C4 . H42 . 4.3 no
H51 . C4 . H41 . 4.5 no
H51 . C4 . H42 . 108.5 no
H41 . C4 . H42 . 112.7 no
C8 6_555 C7 . C8 . 135(7) yes
C8 6_555 C7 . H71 . 112.7 no
C8 . C7 . H71 . 112.7 no
C8 5_655 C8 . C7 . 113(3) yes
C8 5_655 C8 . H81 . 119.0 no
C7 . C8 . H81 . 128.3 no
C10 5_655 C9 . C10 . 120.0(8) yes
C10 5_655 C9 . H91 . 120.0 no
C10 . C9 . H91 . 120.0 no
C10 14_556 C10 . C9 . 120.0(4) yes
C10 14_556 C10 . H101 . 120.0 no
C9 . C10 . H101 . 120.0 no
C6 14_556 C6 . N1 . 111.8(9) yes
C6 14_556 C6 . H62 5_555 108.8 no
N1 . C6 . H62 5_555 107.7 no
C6 14_556 C6 . H61 5_555 109.4 no
N1 . C6 . H61 5_555 108.3 no
H62 5_555 C6 . H61 5_555 110.9 no
C6 14_556 C6 . H52 5_555 109.6 no
N1 . C6 . H52 5_555 113.1 no
H62 5_555 C6 . H52 5_555 7.0 no
H61 5_555 C6 . H52 5_555 104.4 no
C6 14_556 C6 . H61 . 109.4 no
N1 . C6 . H61 . 108.3 no
H62 5_555 C6 . H61 . 1.2 no
H61 5_555 C6 . H61 . 109.7 no
H52 5_555 C6 . H61 . 5.9 no
C6 14_556 C6 . H62 . 108.8 no
N1 . C6 . H62 . 107.7 no
H62 5_555 C6 . H62 . 112.1 no
H61 5_555 C6 . H62 . 1.2 no
H52 5_555 C6 . H62 . 105.6 no
C6 14_556 C6 . H52 . 109.6 no
N1 . C6 . H52 . 113.1 no
H62 5_555 C6 . H52 . 105.6 no
H61 5_555 C6 . H52 . 5.9 no
H52 5_555 C6 . H52 . 99.0 no
H61 . C6 . H62 . 110.9 no
H61 . C6 . H52 . 104.4 no
H62 . C6 . H52 . 7.0 no
C6 . H61 . C5 5_555 68.4 no
C6 . H62 . C5 . 67.4 no
C5 . H51 . C4 . 66.8 no
C5 . H52 . C6 . 65.3 no
C4 . H41 . C5 . 67.5 no
C4 . H42 . C5 9_555 65.9 no



# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
6 12 0 x .
3 1 1 x .
2 0 2 x .
6 2 2 x .
2 10 2 x .
# looking for ARCHIVE-HKL.CIF 

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

data_1_EtOH_069GPa
_database_code_depnum_ccdc_archive 'CCDC 2087900'
loop_
_audit_author_name
_audit_author_address
'Stephen Moggach'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2021-06-03 deposited with the CCDC.	2021-09-29 downloaded from the CCDC.
;
_audit_creation_date             2021-05-26
_audit_creation_method           CRYSTALS_ver_14.61_build_6999

_refine_special_details          
; 
027_ALERT_3_A _diffrn_reflns_theta_full value (too) Low ......      18.32 Degree
029_ALERT_3_A _diffrn_measured_fraction_theta_full value Low .      0.681 Why?
911_ALERT_3_B Missing FCF Refl Between Thmin & STh/L=    0.582        202 Report
023_ALERT_3_C Resolution (too) Low [sin(theta)/Lambda < 0.6]..       0.58 Ang-1
341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............    0.01075 Ang.

These are caused by shading from the pressure cell.

430_ALERT_2_B Short Inter D...A Contact  N1       ..N1       .       2.64 Ang.
                                                     y,x,-z  =     16_555 Check

This is correct, and corresponds to the DABCO N...N distance.


002_ALERT_2_G Number of Distance or Angle Restraints on AtSite          7 Note
003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...          7 Report
004_ALERT_5_G Polymeric Structure Found with Maximum Dimension          3 Info
042_ALERT_1_G Calc. and Reported Moiety Formula Strings Differ     Please Check
045_ALERT_1_G Calculated and Reported Z Differ by a Factor ...       2.00 Check
083_ALERT_2_G SHELXL Second Parameter in WGHT  Unusually Large      24.92 Why ?
300_ALERT_4_G Atom Site Occupancy of C4         Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of C5         Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H13        Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H51        Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H53        Constrained at      0.375 Check
301_ALERT_3_G Main Residue  Disorder ..............(Resd  1  )        22% Note
432_ALERT_2_G Short Inter X...Y Contact  N1       ..C5               2.47 Ang.
                                                   x,1-y,-z  =     10_565 Check
432_ALERT_2_G Short Inter X...Y Contact  N1       ..C5               2.47 Ang.
                                                 1-y,1-x,-z  =     12_665 Check
432_ALERT_2_G Short Inter X...Y Contact  N1       ..C4               2.51 Ang.
                                                   y,1-x,-z  =      4_565 Check
432_ALERT_2_G Short Inter X...Y Contact  N1       ..C4               2.51 Ang.
                                                 1-y,1-x,-z  =     12_665 Check
432_ALERT_2_G Short Inter X...Y Contact  C2       ..C3               2.40 Ang.
                                                   -x,y,1-z  =     14_556 Check
432_ALERT_2_G Short Inter X...Y Contact  C3       ..C3               2.77 Ang.
                                                   -x,y,1-z  =     14_556 Check
432_ALERT_2_G Short Inter X...Y Contact  C4       ..C4               2.49 Ang.
                                                   y,1-x,-z  =      4_565 Check
432_ALERT_2_G Short Inter X...Y Contact  C4       ..C5               2.93 Ang.
                                                   x,1-y,-z  =     10_565 Check
432_ALERT_2_G Short Inter X...Y Contact  C4       ..C5               2.93 Ang.
                                                 1-y,1-x,-z  =     12_665 Check
432_ALERT_2_G Short Inter X...Y Contact  C4       ..C4               3.15 Ang.
                                                 1-y,1-x,-z  =     12_665 Check
432_ALERT_2_G Short Inter X...Y Contact  C5       ..C5               2.42 Ang.
                                                 1-y,1-x,-z  =     12_665 Check
432_ALERT_2_G Short Inter X...Y Contact  C5       ..C5               3.07 Ang.
                                                   x,1-y,-z  =     10_565 Check
605_ALERT_4_G Largest Solvent Accessible VOID in the Structure        723 A**3
760_ALERT_1_G CIF Contains no Torsion Angles .................          ? Info
769_ALERT_4_G CIF Embedded explicitly supplied scattering data     Please Note
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       9.40 Deg.
              H13  -C4   -H51    11_555   1_555   9_655 ......     #   29 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       0.10 Deg.
              H53  -C4   -H51    11_555   1_555   7_565 ......     #   33 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       9.40 Deg.
              H53  -C4   -H13    11_555   1_555   1_555 ......     #   42 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       9.40 Deg.
              H51  -C4   -H13     7_565   1_555   1_555 ......     #   44 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       9.40 Deg.
              H13  -C4   -H53    11_555   1_555   1_555 ......     #   46 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       0.10 Deg.
              H51  -C4   -H53     9_655   1_555   1_555 ......     #   48 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       0.00 Deg.
              H53  -C5   -H51     9_655   1_555   1_555 ......     #   58 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       0.00 Deg.
              H51  -C5   -H53     9_655   1_555   1_555 ......     #   60 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.54 Deg.
              C4   -N1   -C5      5_665   1_555   3_655 ......     #   74 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.54 Deg.
              C4   -N1   -C5      3_655   1_555   3_655 ......     #   76 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.54 Deg.
              C4   -N1   -C5      5_665   1_555   5_665 ......     #   78 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.54 Deg.
              C4   -N1   -C5     13_565   1_555   5_665 ......     #   81 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.54 Deg.
              C4   -N1   -C5      1_555   1_555  11_555 ......     #   84 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.54 Deg.
              C4   -N1   -C5     13_565   1_555  11_555 ......     #   86 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.54 Deg.
              C4   -N1   -C5      1_555   1_555   1_555 ......     #   94 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.54 Deg.
              C4   -N1   -C5      3_655   1_555   1_555 ......     #   95 Check
860_ALERT_3_G Number of Least-Squares Restraints .............         69 Note
869_ALERT_4_G ALERTS Related to the Use of SQUEEZE Suppressed           ! Info
909_ALERT_3_G Percentage of I>2sig(I) Data at Theta(Max) Still        57% Note
910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min).          3 Note
913_ALERT_3_G Missing # of Very Strong Reflections in FCF ....          1 Note
960_ALERT_3_G Number of Intensities with I  <   - 2*sig(I) ...          3 Check
992_ALERT_5_G Repd & Actual _reflns_number_gt Values Differ by          2 Check
#===============================================================================

No action taken.
;

_cell_length_a                   10.9830(16)
_cell_length_b                   10.9830(16)
_cell_length_c                   9.727(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1173.3(4)

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P 4/m m m '
_symmetry_space_group_name_Hall  '-P 4 2 '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-y,x,z
y,-x,-z
-x,-y,z
x,y,-z
y,-x,z
-y,x,-z
-x,y,z
x,-y,-z
y,x,z
-y,-x,-z
x,-y,z
-x,y,-z
-y,-x,z
y,x,-z

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            1

# Given Formula = C22 H20 N2 O8 Zn2 
# Dc =      0.81 Fooo =    290.00 Mu =     10.47 M =    571.17
# Found Formula = C22 H26 N2 O8 Zn2 
# Dc =      0.82 FOOO =    296.00 Mu =     10.47 M =    577.22

_chemical_formula_sum            'C38.2 H74.6 O16.1 N2 Zn2'
_chemical_formula_moiety         '(C22 H26 N2 O8 Zn2)n 8.1 (C2 O H6)'
_chemical_compound_source        .
_chemical_formula_weight         950.39

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 -0.002 -0.002 -0.020 720 211 '8.1 (C2 O H6)'
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
see text for details
;

_cell_measurement_reflns_used    3661
_cell_measurement_theta_min      3
_cell_measurement_theta_max      25
_cell_measurement_temperature    298

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.050
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.150

_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             506.6
_exptl_absorpt_coefficient_mu    1.09

# Sheldrick geometric approximatio 0.85 0.95 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_T_max  0.95
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      298
_diffrn_ambient_pressure         690000
_diffrn_reflns_number            4233
_diffrn_reflns_av_unetI/netI     0.058
_reflns_number_total             399
_diffrn_reflns_av_R_equivalents  0.044
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 399 
# Theoretical number of reflections is about 967 


_diffrn_reflns_theta_min         2.797
_diffrn_reflns_theta_max         24.420
_diffrn_measured_fraction_theta_max 0.642

_diffrn_reflns_theta_full        18.315
_diffrn_measured_fraction_theta_full 0.681


_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_reflns_limit_h_min              0
_reflns_limit_h_max              5
_reflns_limit_k_min              0
_reflns_limit_k_max              11
_reflns_limit_l_min              0
_reflns_limit_l_max              11

_oxford_diffrn_Wilson_B_factor   0.24
_oxford_diffrn_Wilson_scale      53.57

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

_refine_diff_density_min         -1.03
_refine_diff_density_max         1.26


# 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_refine_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_restraints     69
_refine_ls_number_parameters     31
_refine_ls_number_reflns         399
_oxford_refine_ls_R_factor_ref   0.0916
_refine_ls_wR_factor_ref         0.2126
_refine_ls_goodness_of_fit_ref   1.0403
_refine_ls_shift/su_max          0.0180922
_refine_ls_shift/su_mean         0.0005979


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        399
_refine_ls_R_factor_all          0.0916
_refine_ls_wR_factor_all         0.2126

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                346
_refine_ls_R_factor_gt           0.0761
_refine_ls_wR_factor_gt          0.1909


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #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 +24.92P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

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

# Replace last . with number of unfound hydrogen atoms attached 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 0.5000 0.3463(2) 0.0243 1.0000 Uani S T . . . .
C1 C 0.2633(11) 0.5000 0.5000 0.0395 1.0000 Uani DS TU . . . .
C2 C 0.1267(11) 0.5000 0.5000 0.0318 1.0000 Uani DS TU . . . .
C3 C 0.0630(4) 0.5000 0.3768(9) 0.0506 1.0000 Uani DS TU . . . .
C4 C 0.4118(6) 0.4118(6) 0.0801(5) 0.0363 0.3750 Uani DS U . . . .
C5 C 0.5000 0.3790(9) 0.0788(5) 0.0336 0.3750 Uani DS U . . . .
N1 N 0.5000 0.5000 0.1359 0.0202 1.0000 Uani D U . . . .
O1 O 0.3160(8) 0.5000 0.3847(7) 0.0427 1.0000 Uani DS TU . . . .
H13 H 0.3308 0.4395 0.1007 0.0468 0.3750 Uiso R . . . . .
H51 H 0.5714 0.3370 0.1104 0.0403 0.3750 Uiso R . . . . .
H53 H 0.4287 0.3370 0.1104 0.0403 0.3750 Uiso R . . . . .
H32 H 0.1059 0.5000 0.2920 0.0598 1.0000 Uiso RS . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.2005(7)
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 . Zn1 2_666 2.991(4) yes
Zn1 . O1 3_655 2.056(8) yes
Zn1 . O1 5_665 2.056(8) yes
Zn1 . O1 7_565 2.056(8) yes
Zn1 . O1 . 2.056(8) yes
Zn1 . N1 . 2.047(2) yes
C1 . O1 6_556 1.262(7) yes
C1 . C2 . 1.501(9) yes
C1 . O1 . 1.262(7) yes
C2 . C3 6_556 1.388(7) yes
C2 . C3 . 1.388(7) yes
C3 . C3 5_565 1.384(9) yes
C3 . H32 . 0.950 no
C4 . C4 6_555 1.559(9) yes
C4 . H13 11_555 0.962 no
C4 . H53 11_555 0.893 no
C4 . H51 9_655 0.892 no
C4 . H51 7_565 0.892 no
C4 . N1 . 1.473(9) yes
C4 . H13 . 0.962 no
C4 . H53 . 0.893 no
C5 . C5 6_555 1.533(9) yes
C5 . H51 9_655 0.961 no
C5 . H53 9_655 0.960 no
C5 . H51 . 0.961 no
C5 . H53 . 0.960 no
C5 . N1 . 1.440(9) yes
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
Zn1 2_666 Zn1 . O1 3_655 79.52(19) yes
Zn1 2_666 Zn1 . O1 5_665 79.52(19) yes
O1 3_655 Zn1 . O1 5_665 88.10(7) yes
Zn1 2_666 Zn1 . O1 7_565 79.52(19) yes
O1 3_655 Zn1 . O1 7_565 159.0(4) yes
O1 5_665 Zn1 . O1 7_565 88.10(7) yes
Zn1 2_666 Zn1 . O1 . 79.52(19) yes
O1 3_655 Zn1 . O1 . 88.10(7) yes
O1 5_665 Zn1 . O1 . 159.0(4) yes
O1 7_565 Zn1 . O1 . 88.10(7) yes
Zn1 2_666 Zn1 . N1 . 179.99 yes
O1 3_655 Zn1 . N1 . 100.48(19) yes
O1 5_665 Zn1 . N1 . 100.48(19) yes
O1 7_565 Zn1 . N1 . 100.48(19) yes
O1 . Zn1 . N1 . 100.48(19) yes
O1 6_556 C1 . C2 . 117.3(6) yes
O1 6_556 C1 . O1 . 125.5(12) yes
C2 . C1 . O1 . 117.3(6) yes
C1 . C2 . C3 6_556 120.3(5) yes
C1 . C2 . C3 . 120.3(5) yes
C3 6_556 C2 . C3 . 119.5(11) yes
C2 . C3 . C3 5_565 120.3(5) yes
C2 . C3 . H32 . 120.0 no
C3 5_565 C3 . H32 . 119.7 no
C4 6_555 C4 . H13 11_555 102.0 no
C4 6_555 C4 . H53 11_555 109.2 no
H13 11_555 C4 . H53 11_555 114.5 no
C4 6_555 C4 . H51 9_655 109.3 no
H13 11_555 C4 . H51 9_655 9.4 no
H53 11_555 C4 . H51 9_655 105.8 no
C4 6_555 C4 . H51 7_565 109.3 no
H13 11_555 C4 . H51 7_565 114.4 no
H53 11_555 C4 . H51 7_565 0.1 no
H51 9_655 C4 . H51 7_565 105.7 no
C4 6_555 C4 . N1 . 111.6(2) yes
H13 11_555 C4 . N1 . 108.9 no
H53 11_555 C4 . N1 . 110.4 no
H51 9_655 C4 . N1 . 110.4 no
H51 7_565 C4 . N1 . 110.4 no
C4 6_555 C4 . H13 . 102.0 no
H13 11_555 C4 . H13 . 122.8 no
H53 11_555 C4 . H13 . 9.4 no
H51 9_655 C4 . H13 . 114.4 no
H51 7_565 C4 . H13 . 9.4 no
C4 6_555 C4 . H53 . 109.2 no
H13 11_555 C4 . H53 . 9.4 no
H53 11_555 C4 . H53 . 105.9 no
H51 9_655 C4 . H53 . 0.1 no
H51 7_565 C4 . H53 . 105.8 no
N1 . C4 . H13 . 108.9 no
N1 . C4 . H53 . 110.4 no
H13 . C4 . H53 . 114.5 no
C5 6_555 C5 . H51 9_655 108.6 no
C5 6_555 C5 . H53 9_655 108.7 no
H51 9_655 C5 . H53 9_655 109.4 no
C5 6_555 C5 . H51 . 108.6 no
H51 9_655 C5 . H51 . 109.5 no
H53 9_655 C5 . H51 . 0.0 no
C5 6_555 C5 . H53 . 108.7 no
H51 9_655 C5 . H53 . 0.0 no
H53 9_655 C5 . H53 . 109.4 no
H51 . C5 . H53 . 109.4 no
C5 6_555 C5 . N1 . 112.7(2) yes
H51 9_655 C5 . N1 . 108.7 no
H53 9_655 C5 . N1 . 108.7 no
H51 . C5 . N1 . 108.7 no
H53 . C5 . N1 . 108.7 no
C4 5_665 N1 . C4 . 136.8(5) yes
C4 5_665 N1 . C4 3_655 82.21(16) yes
C4 . N1 . C4 3_655 82.21(16) yes
C4 5_665 N1 . C4 13_565 82.21(16) yes
C4 . N1 . C4 13_565 82.21(16) yes
C4 3_655 N1 . C4 13_565 136.8(5) yes
C4 5_665 N1 . C5 3_655 41.54(5) yes
C4 . N1 . C5 3_655 117.7(2) yes
C4 3_655 N1 . C5 3_655 41.54(5) yes
C4 13_565 N1 . C5 3_655 117.7(2) yes
C4 5_665 N1 . C5 5_665 41.54(5) yes
C4 . N1 . C5 5_665 117.7(2) yes
C4 3_655 N1 . C5 5_665 117.7(2) yes
C4 13_565 N1 . C5 5_665 41.54(5) yes
C5 3_655 N1 . C5 5_665 81.46(17) yes
C4 5_665 N1 . C5 11_555 117.7(2) yes
C4 . N1 . C5 11_555 41.54(5) yes
C4 3_655 N1 . C5 11_555 117.7(2) yes
C4 13_565 N1 . C5 11_555 41.54(5) yes
C5 3_655 N1 . C5 11_555 134.7(5) yes
C4 5_665 N1 . Zn1 . 111.6(2) yes
C4 . N1 . Zn1 . 111.6(2) yes
C4 3_655 N1 . Zn1 . 111.6(2) yes
C4 13_565 N1 . Zn1 . 111.6(2) yes
C5 3_655 N1 . Zn1 . 112.7(2) yes
C4 5_665 N1 . C5 . 117.7(2) yes
C4 . N1 . C5 . 41.54(5) yes
C4 3_655 N1 . C5 . 41.54(5) yes
C4 13_565 N1 . C5 . 117.7(2) yes
C5 3_655 N1 . C5 . 81.46(17) yes
C5 5_665 N1 . C5 11_555 81.46(17) yes
C5 5_665 N1 . Zn1 . 112.7(2) yes
C5 11_555 N1 . Zn1 . 112.7(2) yes
C5 5_665 N1 . C5 . 134.7(5) yes
C5 11_555 N1 . C5 . 81.46(17) yes
Zn1 . N1 . C5 . 112.7(2) yes
Zn1 . O1 . C1 . 127.7(7) yes
C5 . H51 . C4 9_655 67.7 no
C5 . H53 . C4 . 67.7 no


# looking for ARCHIVE-HKL.CIF 

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

data_1_EtOH_119GPa
_database_code_depnum_ccdc_archive 'CCDC 2087893'
loop_
_audit_author_name
_audit_author_address
'Stephen Moggach'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2021-06-03 deposited with the CCDC.	2021-09-29 downloaded from the CCDC.
;
_audit_creation_date             2021-05-26
_audit_creation_method           CRYSTALS_ver_14.61_build_6999

_refine_special_details          
; 
027_ALERT_3_A _diffrn_reflns_theta_full value (too) Low ......      17.45 Degree
029_ALERT_3_A _diffrn_measured_fraction_theta_full value Low .      0.673 Why?
023_ALERT_3_B Resolution (too) Low [sin(theta)/Lambda < 0.6]..       0.56 Ang-1
341_ALERT_3_B Low Bond Precision on  C-C Bonds ...............     0.0155 Ang.
911_ALERT_3_B Missing FCF Refl Between Thmin & STh/L=    0.556        558 Report

These are caused by shading from the pressure cell.


430_ALERT_2_A Short Inter D...A Contact  N1       ..N1       .       2.53 Ang.
                                                   1-x,y,-z  =      6_655 Check

This is correct, and corresponds to the DABCO N...N distance.


770_ALERT_2_A Suspect C-H Bond in CIF:  C7       --H81       .       1.31 Ang.
770_ALERT_2_A Suspect C-H Bond in CIF:  C7       --H82       .       1.31 Ang.
201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) .......          7 Report
              O1        O2        N1        C1        C2                  etc.
076_ALERT_1_C Occupancy      0.500 Less Than 1.0 for Sp.pos  .           C5
076_ALERT_1_C Occupancy      0.500 Less Than 1.0 for Sp.pos  .           C8
701_ALERT_1_C Bond    Calc   2.9748(2), Rep 2.97517(12), Dev..       1.85 Sigma
              ZN1      -ZN1             1_555   2_656 ........     #    1 Check
906_ALERT_3_C Large K Value in the Analysis of Variance ......      3.299 Check

These are all caused by disorder on the DABCO ligand.

082_ALERT_2_C High R1 Value ..................................       0.13 Report
084_ALERT_3_C High wR2 Value (i.e. > 0.25) ...................       0.31 Report

The sample has undergone a phase transition, which has caused twinning 
and breakup of the crystal.

921_ALERT_1_B R1  in the CIF and FCF Differ by ...............     0.0082 Check
922_ALERT_1_B wR2 in the CIF and FCF Differ by ...............     0.0338 Check


Reflections that overlap with W-gasket, or have poor correlations within 
2 degrees of the half-opening angle of the cell have been removed, 
causing the above alert. These were removed after data processing, 
as a number of strong reflections were measures well close to W-rings
that we wanted to include in the refinement.


992_ALERT_5_B Repd & Actual _reflns_number_gt Values Differ by         36 Check

This has been checked.  Reported numbers came from the twinabs output.

#===============================================================================
002_ALERT_2_G Number of Distance or Angle Restraints on AtSite         11 Note
003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...         11 Report
004_ALERT_5_G Polymeric Structure Found with Maximum Dimension          2 Info
042_ALERT_1_G Calc. and Reported Moiety Formula Strings Differ     Please Check
045_ALERT_1_G Calculated and Reported Z Differ by a Factor ...       2.00 Check
083_ALERT_2_G SHELXL Second Parameter in WGHT  Unusually Large      85.30 Why ?
199_ALERT_1_G Reported _cell_measurement_temperature ..... (K)        293 Check
200_ALERT_1_G Reported   _diffrn_ambient_temperature ..... (K)        293 Check
300_ALERT_4_G Atom Site Occupancy of C5         Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of C6         Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of C7         Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of C8         Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of H51        Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of H52        Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of H61        Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of H62        Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of H71        Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of H72        Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of H81        Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of H82        Constrained at        0.5 Check
301_ALERT_3_G Main Residue  Disorder ..............(Resd  1  )        22% Note
432_ALERT_2_G Short Inter X...Y Contact  N1       ..C5               2.37 Ang.
                                                   1-x,y,-z  =      6_655 Check
432_ALERT_2_G Short Inter X...Y Contact  N1       ..C6               2.40 Ang.
                                                  1-x,-y,-z  =      2_655 Check
432_ALERT_2_G Short Inter X...Y Contact  N1       ..C6               2.40 Ang.
                                                   1-x,y,-z  =      6_655 Check
432_ALERT_2_G Short Inter X...Y Contact  N1       ..C7               2.49 Ang.
                                                  1-x,-y,-z  =      2_655 Check
432_ALERT_2_G Short Inter X...Y Contact  N1       ..C7               2.49 Ang.
                                                   1-x,y,-z  =      6_655 Check
432_ALERT_2_G Short Inter X...Y Contact  N1       ..C8               2.54 Ang.
                                                   1-x,y,-z  =      6_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C5       ..C8               1.52 Ang.
                                                   1-x,y,-z  =      6_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C5       ..C7               2.04 Ang.
                                                  1-x,-y,-z  =      2_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C5       ..C7               2.04 Ang.
                                                   1-x,y,-z  =      6_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C5       ..C6               2.76 Ang.
                                                  1-x,-y,-z  =      2_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C5       ..C6               2.76 Ang.
                                                   1-x,y,-z  =      6_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C5       ..C5               3.03 Ang.
                                                   1-x,y,-z  =      6_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C6       ..C7               1.52 Ang.
                                                   1-x,y,-z  =      6_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C6       ..C6               2.05 Ang.
                                                   1-x,y,-z  =      6_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C6       ..C8               2.05 Ang.
                                                   1-x,y,-z  =      6_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C6       ..C7               2.82 Ang.
                                                  1-x,-y,-z  =      2_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C6       ..C6               3.08 Ang.
                                                  1-x,-y,-z  =      2_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C7       ..C7               2.10 Ang.
                                                   1-x,y,-z  =      6_655 Check
432_ALERT_2_G Short Inter X...Y Contact  C7       ..C8               2.92 Ang.
                                                   1-x,y,-z  =      6_655 Check
606_ALERT_4_G Solvent Accessible VOID(S) in Structure ........          ! Info
760_ALERT_1_G CIF Contains no Torsion Angles .................          ? Info
769_ALERT_4_G CIF Embedded explicitly supplied scattering data     Please Note
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      18.40 Deg.
              H51  -C5   -H62     5_555   1_555   5_555 ......     #   59 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.80 Deg.
              H62  -C5   -C6      5_555   1_555   5_555 ......     #   65 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      18.40 Deg.
              H62  -C5   -H52     5_555   1_555   1_555 ......     #   78 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      18.40 Deg.
              H52  -C5   -H62     5_555   1_555   1_555 ......     #   82 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.80 Deg.
              C6   -C5   -H62     1_555   1_555   1_555 ......     #   91 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      18.40 Deg.
              H51  -C5   -H62     1_555   1_555   1_555 ......     #   92 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      40.80 Deg.
              H81  -C7   -C8      5_555   1_555   1_555 ......     #   99 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      40.80 Deg.
              C8   -C7   -H82     1_555   1_555   1_555 ......     #  106 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      25.50 Deg.
              H81  -C7   -H71     5_555   1_555   1_555 ......     #  110 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      25.50 Deg.
              H82  -C7   -H71     1_555   1_555   1_555 ......     #  123 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      12.60 Deg.
              H72  -C7   -H61     1_555   1_555   1_555 ......     #  128 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.90 Deg.
              C7   -C6   -H72     1_555   1_555   1_555 ......     #  168 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      20.70 Deg.
              H52  -C6   -H62     5_555   1_555   1_555 ......     #  181 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      12.10 Deg.
              H72  -C6   -H61     1_555   1_555   1_555 ......     #  185 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      20.70 Deg.
              H51  -C6   -H62     1_555   1_555   1_555 ......     #  188 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      42.80 Deg.
              H71  -H81  -C7      5_555   1_555   5_555 ......     #  191 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      42.80 Deg.
              C7   -H82  -H71     1_555   1_555   1_555 ......     #  195 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.60 Deg.
              C5   -H62  -H52     1_555   1_555   5_555 ......     #  207 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.60 Deg.
              C5   -H62  -H51     1_555   1_555   1_555 ......     #  209 Check
795_ALERT_4_G C-Atom in CIF Coordinate List Out-of-Sequence ..         C2 Note
796_ALERT_4_G O-Atom in CIF Coordinate List Out-of-Sequence ..         O1 Note
860_ALERT_3_G Number of Least-Squares Restraints .............        121 Note
869_ALERT_4_G ALERTS Related to the Use of SQUEEZE Suppressed           ! Info
909_ALERT_3_G Percentage of I>2sig(I) Data at Theta(Max) Still        75% Note
910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min).          3 Note
913_ALERT_3_G Missing # of Very Strong Reflections in FCF ....          1 Note
956_ALERT_1_G Calculated (ThMax) and Actual (FCF) Hmax Differ           2 Units
957_ALERT_1_G Calculated (ThMax) and Actual (FCF) Kmax Differ           4 Units
961_ALERT_5_G Dataset Contains no Negative Intensities .......     Please Check
#===============================================================================

No action taken.
;

_cell_length_a                   14.4123(12)
_cell_length_b                   16.3757(13)
_cell_length_c                   9.7030(4)
_cell_angle_alpha                90
_cell_angle_beta                 92.158(4)
_cell_angle_gamma                90
_cell_volume                     2288.4(3)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/m '
_symmetry_space_group_name_Hall  '-C 2y'
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
-x,y,-z
x+1/2,-y+1/2,z
-x+1/2,y+1/2,-z

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            2

# Given Formula = C24 H24 N8 O16 Zn8 
# Dc =      1.75 Fooo =   1184.00 Mu =     41.82 M =   1203.54
# Found Formula = C22 H24 N2 O8 Zn2 
# Dc =      0.83 FOOO =    588.00 Mu =     10.74 M =    575.20

_chemical_formula_sum            'C45.8 H97.4 O19.9 N2 Zn2'
_chemical_formula_moiety         '(C22 H26 N2 O8 Zn2)n 11.9(C2 O H6)'
_chemical_compound_source        .
_chemical_formula_weight         1125.44

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 -0.013 -0.007 -0.011 1431 620 '11.9(C2 O H6) '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
see text for details
;

_cell_measurement_reflns_used    2067
_cell_measurement_theta_min      3
_cell_measurement_theta_max      23
_cell_measurement_temperature    293

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.050
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.150

_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1210.8
_exptl_absorpt_coefficient_mu    1.14

# Sheldrick geometric approximatio 0.85 0.95 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_T_max  0.95
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      293
_diffrn_ambient_pressure         1190000
_diffrn_reflns_number            8127
_diffrn_reflns_av_unetI/netI     0.087
_reflns_number_total             1089
_diffrn_reflns_av_R_equivalents  0.088
# Number of reflections without Friedels Law is 1089 
# Number of reflections with Friedels Law is 1089 
# Theoretical number of reflections is about 1645 


_diffrn_reflns_theta_min         2.781
_diffrn_reflns_theta_max         23.262
_diffrn_measured_fraction_theta_max 0.636

_diffrn_reflns_theta_full        17.446
_diffrn_measured_fraction_theta_full 0.673


_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_reflns_limit_h_min              -14
_reflns_limit_h_max              13
_reflns_limit_k_min              0
_reflns_limit_k_max              14
_reflns_limit_l_min              0
_reflns_limit_l_max              10

_oxford_diffrn_Wilson_B_factor   1.06
_oxford_diffrn_Wilson_scale      386.49

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

_refine_diff_density_min         -1.38
_refine_diff_density_max         1.34


# 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_refine_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_restraints     121
_refine_ls_number_parameters     44
_refine_ls_number_reflns         1038
_oxford_refine_ls_R_factor_ref   0.1541
_refine_ls_wR_factor_ref         0.2762
_refine_ls_goodness_of_fit_ref   1.5129
_refine_ls_shift/su_max          0.0038954
_refine_ls_shift/su_mean         0.0005072


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        1089
_refine_ls_R_factor_all          0.1699
_refine_ls_wR_factor_all         0.3100

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                824
_refine_ls_R_factor_gt           0.1332
_refine_ls_wR_factor_gt          0.2881


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.00P)² +85.30P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

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

# Replace last . with number of unfound hydrogen atoms attached 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 0.4966 0.0000 0.3466 0.0236 1.0000 Uani . . . . . .
O2 O 0.6008(5) 0.0842(6) 0.6255(10) 0.0484(18) 1.0000 Uiso D U . . . .
O1 O 0.5990(6) 0.0867(6) 0.3914(9) 0.0480(18) 1.0000 Uiso D U . . . .
N1 N 0.5023(6) 0.0000 0.1303(14) 0.026(3) 1.0000 Uiso DS U . . . .
C4 C 0.7219(6) 0.2168(7) 0.6246(14) 0.0489(18) 1.0000 Uiso D U . . . .
C2 C 0.6893(5) 0.1834(6) 0.5006(13) 0.0485(18) 1.0000 Uiso D U . . . .
C1 C 0.6239(5) 0.1117(6) 0.5107(10) 0.0487(18) 1.0000 Uiso D U . . . .
C3 C 0.7178(7) 0.2169(7) 0.3806(14) 0.0492(18) 1.0000 Uiso D U . . . .
C5 C 0.4070(11) 0.0000 0.068(2) 0.027(3) 0.5000 Uiso DS U . . . .
C7 C 0.5479(7) 0.0745(7) 0.0841(17) 0.027(3) 0.5000 Uiso D U . . . .
C8 C 0.5991(10) -0.0000 0.089(2) 0.027(3) 0.5000 Uiso DS U . . . .
C6 C 0.4504(7) 0.0703(8) 0.0726(17) 0.027(3) 0.5000 Uiso D U . . . .
H41 H 0.7011 0.1966 0.7099 0.0598 1.0000 Uiso R . . . . .
H31 H 0.6923 0.1959 0.2962 0.0607 1.0000 Uiso R . . . . .
H81 H 0.6308 -0.0479 0.1229 0.0588 0.5000 Uiso R . . . . .
H82 H 0.6308 0.0479 0.1229 0.0588 0.5000 Uiso R . . . . .
H71 H 0.6097 0.0800 0.1236 0.0550 0.5000 Uiso R . . . . .
H72 H 0.5111 0.1203 0.1109 0.0550 0.5000 Uiso R . . . . .
H51 H 0.3757 0.0479 0.0999 0.0513 0.5000 Uiso R . . . . .
H52 H 0.3757 -0.0479 0.0999 0.0513 0.5000 Uiso R . . . . .
H61 H 0.4904 0.1193 0.1154 0.0443 0.5000 Uiso R . . . . .
H62 H 0.3910 0.0722 0.1028 0.0443 0.5000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.10530(10)
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 . Zn1 2_656 2.97517(12) yes
Zn1 . O1 5_555 2.082(12) yes
Zn1 . O2 6_656 1.994(12) yes
Zn1 . O2 2_656 1.994(12) yes
Zn1 . O1 . 2.082(12) yes
Zn1 . N1 . 2.103(14) yes
O2 . C1 . 1.257(8) yes
O1 . C1 . 1.266(8) yes
N1 . C6 5_555 1.472(9) yes
N1 . C7 5_555 1.465(9) yes
N1 . C5 . 1.477(9) yes
N1 . C7 . 1.465(9) yes
N1 . C8 . 1.468(9) yes
N1 . C6 . 1.472(9) yes
C4 . C3 4_656 1.392(6) yes
C4 . C2 . 1.388(9) yes
C4 . H41 . 0.950 no
C2 . C1 . 1.510(9) yes
C2 . C3 . 1.366(8) yes
C3 . H31 . 0.950 no
C5 . C8 2_655 1.5230(7) yes
C5 . H51 5_555 0.960 no
C5 . H52 5_555 0.960 no
C5 . H62 5_555 1.252 no
C5 . C6 5_555 1.309(14) yes
C5 . C6 . 1.309(14) yes
C5 . H51 . 0.960 no
C5 . H52 . 0.960 no
C5 . H62 . 1.252 no
C7 . C6 6_655 1.5230(7) yes
C7 . H81 5_555 1.313 no
C7 . C8 . 1.426(14) yes
C7 . C6 . 1.408(13) yes
C7 . H82 . 1.313 no
C7 . H71 . 0.960 no
C7 . H72 . 0.960 no
C7 . H61 . 1.156 no
C8 . H82 5_555 0.960 no
C8 . H81 5_555 0.960 no
C8 . H81 . 0.960 no
C8 . H82 . 0.960 no
C6 . H52 5_555 1.177 no
C6 . H72 . 1.244 no
C6 . H51 . 1.177 no
C6 . H61 . 1.064 no
C6 . H62 . 0.915 no
H81 . H71 5_555 0.608 no
H82 . H71 . 0.608 no
H51 . H62 . 0.455 no
H52 . H62 5_555 0.455 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
Zn1 2_656 Zn1 . O1 5_555 78.1(3) yes
Zn1 2_656 Zn1 . O2 6_656 82.0(3) yes
O1 5_555 Zn1 . O2 6_656 160.1(4) yes
Zn1 2_656 Zn1 . O2 2_656 82.0(3) yes
O1 5_555 Zn1 . O2 2_656 89.86(8) yes
O2 6_656 Zn1 . O2 2_656 87.50(14) yes
Zn1 2_656 Zn1 . O1 . 78.1(3) yes
O1 5_555 Zn1 . O1 . 85.96(16) yes
O2 6_656 Zn1 . O1 . 89.86(8) yes
O2 2_656 Zn1 . O1 . 160.1(4) yes
Zn1 2_656 Zn1 . N1 . 175.9(2) yes
O1 5_555 Zn1 . N1 . 98.9(3) yes
O2 6_656 Zn1 . N1 . 100.9(3) yes
O2 2_656 Zn1 . N1 . 100.9(3) yes
O1 . Zn1 . N1 . 98.9(3) yes
Zn1 2_656 O2 . C1 . 125.4(9) yes
Zn1 . O1 . C1 . 125.9(9) yes
C6 5_555 N1 . C7 5_555 57.3(5) yes
C6 5_555 N1 . Zn1 . 110.0(9) yes
C7 5_555 N1 . Zn1 . 109.9(9) yes
C6 5_555 N1 . C5 . 52.7(6) yes
C7 5_555 N1 . C5 . 107.3(9) yes
Zn1 . N1 . C5 . 109.6(11) yes
C6 5_555 N1 . C7 . 139.7(12) yes
C7 5_555 N1 . C7 . 112.8(13) yes
Zn1 . N1 . C7 . 109.9(9) yes
C5 . N1 . C7 . 107.3(9) yes
C6 5_555 N1 . C8 . 111.7(9) yes
C7 5_555 N1 . C8 . 58.2(6) yes
Zn1 . N1 . C8 . 110.3(11) yes
C5 . N1 . C8 . 140.1(12) yes
C7 . N1 . C8 . 58.2(6) yes
C6 5_555 N1 . C6 . 102.9(12) yes
C7 5_555 N1 . C6 . 139.7(12) yes
Zn1 . N1 . C6 . 110.0(9) yes
C5 . N1 . C6 . 52.7(6) yes
C7 . N1 . C6 . 57.3(5) yes
C8 . N1 . C6 . 111.7(9) yes
C3 4_656 C4 . C2 . 117.9(14) yes
C3 4_656 C4 . H41 . 121.4 no
C2 . C4 . H41 . 120.6 no
C4 . C2 . C1 . 116.3(12) yes
C4 . C2 . C3 . 118.5(11) yes
C1 . C2 . C3 . 125.2(12) yes
C2 . C1 . O1 . 110.4(10) yes
C2 . C1 . O2 . 121.4(11) yes
O1 . C1 . O2 . 128.2(12) yes
C4 4_656 C3 . C2 . 123.6(14) yes
C4 4_656 C3 . H31 . 118.3 no
C2 . C3 . H31 . 118.0 no
C8 2_655 C5 . N1 . 115.2(18) yes
C8 2_655 C5 . H51 5_555 107.9 no
N1 . C5 . H51 5_555 108.1 no
C8 2_655 C5 . H52 5_555 107.9 no
N1 . C5 . H52 5_555 108.1 no
H51 5_555 C5 . H52 5_555 109.5 no
C8 2_655 C5 . H62 5_555 105.2 no
N1 . C5 . H62 5_555 94.0 no
H51 5_555 C5 . H62 5_555 18.4 no
H52 5_555 C5 . H62 5_555 126.3 no
C8 2_655 C5 . C6 5_555 92.3(15) yes
N1 . C5 . C6 5_555 63.4(6) yes
H51 5_555 C5 . C6 5_555 60.1 no
H52 5_555 C5 . C6 5_555 159.6 no
H62 5_555 C5 . C6 5_555 41.8 no
C8 2_655 C5 . C6 . 92.3(15) yes
N1 . C5 . C6 . 63.4(6) yes
H51 5_555 C5 . C6 . 159.6 no
H52 5_555 C5 . C6 . 60.1 no
H62 5_555 C5 . C6 . 156.1 no
C8 2_655 C5 . H51 . 107.9 no
N1 . C5 . H51 . 108.1 no
H51 5_555 C5 . H51 . 109.5 no
H62 5_555 C5 . H51 . 126.3 no
C8 2_655 C5 . H52 . 107.9 no
N1 . C5 . H52 . 108.1 no
H52 5_555 C5 . H52 . 109.5 no
H62 5_555 C5 . H52 . 18.4 no
C8 2_655 C5 . H62 . 105.2 no
N1 . C5 . H62 . 94.0 no
H51 5_555 C5 . H62 . 126.3 no
H52 5_555 C5 . H62 . 18.4 no
H62 5_555 C5 . H62 . 141.5 no
C6 5_555 C5 . C6 . 123.0(14) yes
C6 5_555 C5 . H51 . 159.6 no
C6 . C5 . H51 . 60.1 no
C6 5_555 C5 . H52 . 60.1 no
C6 . C5 . H52 . 159.6 no
H51 . C5 . H52 . 109.5 no
C6 5_555 C5 . H62 . 156.1 no
C6 . C5 . H62 . 41.8 no
H51 . C5 . H62 . 18.4 no
H52 . C5 . H62 . 126.3 no
C6 6_655 C7 . N1 . 106.9(14) yes
C6 6_655 C7 . H81 5_555 102.9 no
N1 . C7 . H81 5_555 92.9 no
C6 6_655 C7 . C8 . 87.9(14) yes
N1 . C7 . C8 . 61.0(5) yes
H81 5_555 C7 . C8 . 40.8 no
C6 6_655 C7 . C6 . 88.4(16) yes
N1 . C7 . C6 . 61.6(5) yes
H81 5_555 C7 . C6 . 154.3 no
C8 . C7 . C6 . 118.3(11) yes
C6 6_655 C7 . H82 . 102.9 no
N1 . C7 . H82 . 92.9 no
C8 . C7 . H82 . 40.8 no
C6 . C7 . H82 . 154.3 no
C6 6_655 C7 . H71 . 110.7 no
N1 . C7 . H71 . 112.1 no
H81 5_555 C7 . H71 . 25.5 no
C8 . C7 . H71 . 66.2 no
C6 . C7 . H71 . 160.8 no
C6 6_655 C7 . H72 . 109.6 no
N1 . C7 . H72 . 107.9 no
H81 5_555 C7 . H72 . 133.5 no
C8 . C7 . H72 . 161.9 no
C6 . C7 . H72 . 59.9 no
C6 6_655 C7 . H61 . 109.3 no
N1 . C7 . H61 . 96.5 no
H81 5_555 C7 . H61 . 142.1 no
C8 . C7 . H61 . 155.5 no
C6 . C7 . H61 . 47.8 no
H82 . C7 . H71 . 25.5 no
H82 . C7 . H72 . 133.5 no
H71 . C7 . H72 . 109.5 no
H82 . C7 . H61 . 142.1 no
H71 . C7 . H61 . 119.9 no
H72 . C7 . H61 . 12.6 no
C5 2_655 C8 . N1 . 104.8(18) yes
C5 2_655 C8 . C7 . 87.6(14) yes
N1 . C8 . C7 . 60.8(5) yes
C5 2_655 C8 . C7 5_555 87.6(14) yes
N1 . C8 . C7 5_555 60.8(5) yes
C7 . C8 . C7 5_555 117.7(12) yes
C5 2_655 C8 . H82 5_555 110.8 no
N1 . C8 . H82 5_555 110.4 no
C7 . C8 . H82 5_555 161.4 no
C7 5_555 C8 . H82 5_555 63.3 no
C5 2_655 C8 . H81 5_555 110.8 no
N1 . C8 . H81 5_555 110.4 no
C7 . C8 . H81 5_555 63.3 no
C7 5_555 C8 . H81 5_555 161.4 no
H82 5_555 C8 . H81 5_555 109.5 no
C5 2_655 C8 . H81 . 110.8 no
N1 . C8 . H81 . 110.4 no
C7 . C8 . H81 . 161.4 no
C7 5_555 C8 . H81 . 63.3 no
C5 2_655 C8 . H82 . 110.8 no
N1 . C8 . H82 . 110.4 no
C7 . C8 . H82 . 63.3 no
C7 5_555 C8 . H82 . 161.4 no
H82 5_555 C8 . H82 . 109.5 no
H81 5_555 C8 . H81 . 109.5 no
H81 . C8 . H82 . 109.5 no
C7 6_655 C6 . N1 . 112.9(14) yes
C7 6_655 C6 . H52 5_555 106.7 no
N1 . C6 . H52 5_555 97.2 no
C7 6_655 C6 . C7 . 91.4(16) yes
N1 . C6 . C7 . 61.1(5) yes
H52 5_555 C6 . C7 . 156.4 no
C7 6_655 C6 . C5 . 92.0(15) yes
N1 . C6 . C5 . 63.9(6) yes
H52 5_555 C6 . C5 . 45.0 no
C7 . C6 . C5 . 121.3(11) yes
C7 6_655 C6 . H72 . 103.4 no
N1 . C6 . H72 . 93.4 no
H52 5_555 C6 . H72 . 140.9 no
C7 . C6 . H72 . 41.9 no
C5 . C6 . H72 . 156.4 no
C7 6_655 C6 . H51 . 106.7 no
N1 . C6 . H51 . 97.2 no
C7 . C6 . H51 . 156.4 no
C5 . C6 . H51 . 45.0 no
C7 6_655 C6 . H61 . 109.1 no
N1 . C6 . H61 . 100.4 no
H52 5_555 C6 . H61 . 129.4 no
C7 . C6 . H61 . 53.6 no
C5 . C6 . H61 . 157.8 no
C7 6_655 C6 . H62 . 111.6 no
N1 . C6 . H62 . 111.8 no
H52 5_555 C6 . H62 . 20.7 no
C7 . C6 . H62 . 156.3 no
C5 . C6 . H62 . 65.7 no
H72 . C6 . H51 . 140.9 no
H72 . C6 . H61 . 12.1 no
H51 . C6 . H61 . 129.4 no
H72 . C6 . H62 . 122.4 no
H51 . C6 . H62 . 20.7 no
H61 . C6 . H62 . 110.4 no
H71 5_555 H81 . C8 . 118.7 no
H71 5_555 H81 . C7 5_555 42.8 no
C8 . H81 . C7 5_555 75.9 no
C8 . H82 . C7 . 75.9 no
C8 . H82 . H71 . 118.7 no
C7 . H82 . H71 . 42.8 no
H81 5_555 H71 . C7 . 111.8 no
H82 . H71 . C7 . 111.8 no
C7 . H72 . C6 . 78.2 no
C6 . H51 . C5 . 74.8 no
C6 . H51 . H62 . 45.3 no
C5 . H51 . H62 . 120.0 no
C6 5_555 H52 . C5 . 74.8 no
C6 5_555 H52 . H62 5_555 45.3 no
C5 . H52 . H62 5_555 120.0 no
C6 . H61 . C7 . 78.6 no
C5 . H62 . C6 . 72.5 no
C5 . H62 . H52 5_555 41.6 no
C6 . H62 . H52 5_555 114.0 no
C5 . H62 . H51 . 41.6 no
C6 . H62 . H51 . 114.0 no



# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
4 0 2 x .
-9 1 4 x .
-4 2 1 x .
1 1 2 x .
-2 0 2 x .
-2 2 2 x .
2 0 2 x .
6 14 5 x .
-1 5 1 x .
-11 3 4 x .
-2 4 3 x .
10 2 4 x .
-2 10 4 x .
-6 14 5 x .
-13 5 5 x .
0 0 5 x .
-1 3 2 x .
-3 3 2 x .
-9 1 9 x .
3 11 4 x .
2 0 1 x .
1 3 0 x .
4 2 0 x .
-1 1 5 x .
-2 0 1 x .
1 1 5 x .
4 2 3 x .
-1 3 1 x .
-1 1 2 x .
5 13 5 x .
5 3 1 x .
1 1 1 x .
0 2 1 x .
9 1 7 x .
-5 3 1 x .
-1 5 6 x .
2 4 4 x .
-3 11 4 x .
-7 5 1 x .
8 0 6 x .
-1 9 6 x .
9 1 6 x .
-4 12 4 x .
8 0 7 x .
-8 4 1 x .
2 6 9 x .
5 3 0 x .
-6 0 5 x .
-5 1 6 x .
0 8 6 x .
-2 4 2 x .
# looking for ARCHIVE-HKL.CIF 

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

data_2_DMF_010GPa
_database_code_depnum_ccdc_archive 'CCDC 2087899'
loop_
_audit_author_name
_audit_author_address
'Stephen Moggach'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2021-06-03 deposited with the CCDC.	2021-09-29 downloaded from the CCDC.
;
_audit_creation_date             2021-05-26
_audit_creation_method           CRYSTALS_ver_14.61_build_6999

_refine_special_details          
; 
029_ALERT_3_A _diffrn_measured_fraction_theta_full value Low .      0.759 Why?
911_ALERT_3_B Missing FCF Refl Between Thmin & STh/L=    0.600        299 Report
913_ALERT_3_C Missing # of Very Strong Reflections in FCF ....          9 Note

These are caused by shading from the pressure cell.

601_ALERT_2_A Unit Cell Contains Solvent Accessible VOIDS of .        218 Ang**3

This is correct.

922_ALERT_1_A wR2 in the CIF and FCF Differ by ...............     0.1918 Check
921_ALERT_1_B R1  in the CIF and FCF Differ by ...............     0.0403 Check

Reflections that overlap with W-gasket, or have poor correlations within 
2 degrees of the half-opening angle of the cell have been removed, 
causing the above alert. These were removed after data processing, 
as a number of strong reflections were measures well close to W-rings
that we wanted to include in the refinement.


202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent .........          3 Check
              N10     C10     C11

This is correct, and corresponds to the DABCO N...N distance.

084_ALERT_3_B High wR2 Value (i.e. > 0.25) ...................       0.39 Report
241_ALERT_2_C High   'MainMol' Ueq as Compared to Neighbors of         O1 Check
242_ALERT_2_C Low    'MainMol' Ueq as Compared to Neighbors of         N1 Check
250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....        2.2 Note
329_ALERT_4_C Carbon Atom Hybridisation Unclear for ..........        C10 Check
341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............     0.0095 Ang.
905_ALERT_3_C Negative K value in the Analysis of Variance ...     -8.890 Report
905_ALERT_3_C Negative K value in the Analysis of Variance ...     -1.005 Report

These are all caused by disorder on the DABCO ligand.


992_ALERT_5_C Repd & Actual _reflns_number_gt Values Differ by         23 Check

This has been checked. 

#===============================================================================
002_ALERT_2_G Number of Distance or Angle Restraints on AtSite         12 Note
003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...         11 Report
042_ALERT_1_G Calc. and Reported Moiety Formula Strings Differ     Please Check
083_ALERT_2_G SHELXL Second Parameter in WGHT  Unusually Large      59.13 Why ?
092_ALERT_4_G Check: Wavelength Given is not Cu,Ga,Mo,Ag,In Ka    0.48590 Ang.
300_ALERT_4_G Atom Site Occupancy of C4         Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of C5         Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H41        Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H42        Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H51        Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H52        Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of O10        Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of H101       Constrained at        0.5 Check
301_ALERT_3_G Main Residue  Disorder ..............(Resd  1  )        14% Note
302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd  2  )        20% Note
760_ALERT_1_G CIF Contains no Torsion Angles .................          ? Info
769_ALERT_4_G CIF Embedded explicitly supplied scattering data     Please Note
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      16.00 Deg.
              H101 -C10  -O10    31_664   1_555   1_555 ......     #   40 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      16.00 Deg.
              O10  -C10  -H101   31_664   1_555   1_555 ......     #   44 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      42.70 Deg.
              C5   -N1   -C4      5_655   1_555   9_665 ......     #   59 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.00 Deg.
              C5   -N1   -C4      9_665   1_555   9_665 ......     #   60 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.00 Deg.
              C5   -N1   -C4      1_555   1_555   1_555 ......     #   65 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      42.70 Deg.
              C5   -N1   -C4     13_565   1_555   1_555 ......     #   66 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      42.70 Deg.
              C5   -N1   -C4      9_665   1_555  13_565 ......     #   69 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.00 Deg.
              C5   -N1   -C4     13_565   1_555  13_565 ......     #   71 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.00 Deg.
              C5   -N1   -C4      5_655   1_555   5_655 ......     #   73 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      42.70 Deg.
              C5   -N1   -C4      1_555   1_555   5_655 ......     #   75 Check
804_ALERT_5_G Number of ARU-Code Packing Problem(s) in PLATON           1 Info
860_ALERT_3_G Number of Least-Squares Restraints .............        165 Note
910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min).          4 Note
912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600         24 Note
960_ALERT_3_G Number of Intensities with I  <   - 2*sig(I) ...          9 Check
#===============================================================================

No action taken.
;
_cell_length_a                   15.1100(10)
_cell_length_b                   15.1100(10)
_cell_length_c                   19.2672(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4398.9(6)

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I 4/m c m '
_symmetry_space_group_name_Hall  '-I 4 2c '
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
-y,x,z
y,-x,-z
-y+1/2,x+1/2,z+1/2
y+1/2,-x+1/2,-z+1/2
-x,-y,z
x,y,-z
-x+1/2,-y+1/2,z+1/2
x+1/2,y+1/2,-z+1/2
y,-x,z
-y,x,-z
y+1/2,-x+1/2,z+1/2
-y+1/2,x+1/2,-z+1/2
-x,y,z+1/2
x,-y,-z+1/2
-x+1/2,y+1/2,z+1
x+1/2,-y+1/2,-z+1
y,x,z+1/2
-y,-x,-z+1/2
y+1/2,x+1/2,z+1
-y+1/2,-x+1/2,-z+1
x,-y,z+1/2
-x,y,-z+1/2
x+1/2,-y+1/2,z+1
-x+1/2,y+1/2,-z+1
-y,-x,z+1/2
y,x,-z+1/2
-y+1/2,-x+1/2,z+1
y+1/2,x+1/2,-z+1

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 0.0006 0.0007 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 0.0016 0.0014 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 0.0036 0.0026 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 0.3043 0.7253 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 = C40 H30 N10 O20 Zn8 
# Dc =      2.26 Fooo =   2960.00 Mu =     43.83 M =   1493.77
# Found Formula = C34 H48 N6 O12 Zn2 
# Dc =      1.30 FOOO =   1800.00 Mu =     11.50 M =    863.55

_chemical_formula_sum            'C34 H48 N6 O12 Zn2'
_chemical_formula_moiety         '(C22 H20 N2 O8 Zn2)n. 4(C3H7NO)'
_chemical_compound_source        .
_chemical_formula_weight         863.55


_cell_measurement_reflns_used    4952
_cell_measurement_theta_min      3
_cell_measurement_theta_max      18
_cell_measurement_temperature    298

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.050
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.150

_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1800
_exptl_absorpt_coefficient_mu    1.150

# Sheldrick geometric approximatio 0.84 0.94 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_T_max  0.94
_diffrn_measurement_device_type  Synchrotron
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.48590
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      298
_diffrn_ambient_pressure         100000
_diffrn_reflns_number            10160
_diffrn_reflns_av_unetI/netI     0.145
_reflns_number_total             935
_diffrn_reflns_av_R_equivalents  0.112
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 935 
# Theoretical number of reflections is about 2245 


_diffrn_reflns_theta_min         2.184
_diffrn_reflns_theta_max         17.667
_diffrn_measured_fraction_theta_max 0.759

_diffrn_reflns_theta_full        17.667
_diffrn_measured_fraction_theta_full 0.759


_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_reflns_limit_h_min              0
_reflns_limit_h_max              13
_reflns_limit_k_min              0
_reflns_limit_k_max              18
_reflns_limit_l_min              0
_reflns_limit_l_max              24

_oxford_diffrn_Wilson_B_factor   1.77
_oxford_diffrn_Wilson_scale      855.88

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

_refine_diff_density_min         -1.28
_refine_diff_density_max         1.79


# 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_refine_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_restraints     165
_refine_ls_number_parameters     70
_refine_ls_number_reflns         904
_oxford_refine_ls_R_factor_ref   0.1087
_refine_ls_wR_factor_ref         0.1969
_refine_ls_goodness_of_fit_ref   0.9768
_refine_ls_shift/su_max          0.0015416
_refine_ls_shift/su_mean         0.0000748


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        935
_refine_ls_R_factor_all          0.1452
_refine_ls_wR_factor_all         0.3887

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                575
_refine_ls_R_factor_gt           0.1009
_refine_ls_wR_factor_gt          0.3645


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.09P)² +59.13P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

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

# Replace last . with number of unfound hydrogen atoms attached 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 0.5000 0.57665(6) 0.0270 1.0000 Uani DS T . . . .
C1 C 0.6505(6) 0.5804(6) 0.5000 0.0388 1.0000 Uani DS TU . . . .
C2 C 0.7275(6) 0.6423(6) 0.5000 0.0369 1.0000 Uani DS TU . . . .
C3 C 0.7626(5) 0.6722(5) 0.5619(2) 0.0468 1.0000 Uani D U . . . .
C4 C 0.5898(6) 0.5010(4) 0.7102(2) 0.0553 0.3750 Uani D U . . . .
C5 C 0.5640(5) 0.5634(5) 0.7101(2) 0.0544 0.3750 Uani D U . . . .
C10 C 0.6706(16) 0.8294(16) 0.7189(13) 0.250(9) 1.0000 Uiso DS U . . . .
C11 C 0.5718(13) 0.8154(13) 0.6105(11) 0.249(9) 1.0000 Uiso D U . . . .
N1 N 0.5000 0.5000 0.6831(4) 0.0286 1.0000 Uani DS TU . . . .
N10 N 0.6354(12) 0.8646(12) 0.6509(11) 0.249(9) 1.0000 Uiso DS U . . . .
O1 O 0.6197(4) 0.5583(4) 0.5577(2) 0.0506 1.0000 Uani D U . . . .
O10 O 0.7387(14) 0.8714(15) 0.7357(16) 0.250(9) 0.5000 Uiso D U . . . .
H32 H 0.7374 0.6537 0.6046 0.0722 1.0000 Uiso R . . . . .
H111 H 0.5571 0.8496 0.5690 0.3980 1.0000 Uiso R . . . . .
H112 H 0.5185 0.8072 0.6385 0.3980 1.0000 Uiso R . . . . .
H113 H 0.5954 0.7577 0.5969 0.3980 1.0000 Uiso R . . . . .
H41 H 0.6195 0.5541 0.6942 0.0665 0.3750 Uiso R . . . . .
H42 H 0.6208 0.4493 0.6931 0.0665 0.3750 Uiso R . . . . .
H51 H 0.6226 0.5474 0.6938 0.0662 0.3750 Uiso R . . . . .
H52 H 0.5489 0.6220 0.6933 0.0662 0.3750 Uiso R . . . . .
H101 H 0.6467 0.7806 0.7437 0.3003 0.5000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.424(2)
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 . Zn1 2_666 2.954(2) yes
Zn1 . O1 5_655 2.045(5) yes
Zn1 . O1 13_565 2.045(5) yes
Zn1 . O1 9_665 2.045(5) yes
Zn1 . N1 . 2.051(8) yes
Zn1 . O1 . 2.045(5) yes
C1 . O1 10_556 1.251(4) yes
C1 . C2 . 1.493(7) yes
C1 . O1 . 1.251(4) yes
C2 . C3 10_556 1.382(5) yes
C2 . C3 . 1.382(5) yes
C3 . C3 31_664 1.393(7) yes
C3 . H32 . 0.948 no
C4 . C4 18_566 1.533(9) yes
C4 . N1 . 1.454(8) yes
C4 . H41 . 0.970 no
C4 . H42 . 0.970 no
C5 . C5 30_556 1.538(9) yes
C5 . N1 . 1.458(8) yes
C5 . H51 . 0.970 no
C5 . H52 . 0.970 no
C10 . H101 31_664 0.950 no
C10 . O10 31_664 1.251(6) yes
C10 . N10 . 1.511(9) yes
C10 . O10 . 1.251(6) yes
C10 . H101 . 0.950 no
C11 . N10 . 1.442(9) yes
C11 . H111 . 0.978 no
C11 . H112 . 0.978 no
C11 . H113 . 0.979 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
Zn1 2_666 Zn1 . O1 5_655 79.73(12) yes
Zn1 2_666 Zn1 . O1 13_565 79.73(12) yes
O1 5_655 Zn1 . O1 13_565 159.5(2) yes
Zn1 2_666 Zn1 . O1 9_665 79.73(12) yes
O1 5_655 Zn1 . O1 9_665 88.18(4) yes
O1 13_565 Zn1 . O1 9_665 88.18(4) yes
Zn1 2_666 Zn1 . N1 . 179.99 yes
O1 5_655 Zn1 . N1 . 100.27(12) yes
O1 13_565 Zn1 . N1 . 100.27(12) yes
O1 9_665 Zn1 . N1 . 100.27(12) yes
Zn1 2_666 Zn1 . O1 . 79.73(12) yes
O1 5_655 Zn1 . O1 . 88.18(4) yes
O1 13_565 Zn1 . O1 . 88.18(4) yes
O1 9_665 Zn1 . O1 . 159.5(2) yes
N1 . Zn1 . O1 . 100.27(12) yes
O1 10_556 C1 . C2 . 117.2(3) yes
O1 10_556 C1 . O1 . 125.6(5) yes
C2 . C1 . O1 . 117.2(3) yes
C1 . C2 . C3 10_556 120.3(2) yes
C1 . C2 . C3 . 120.3(2) yes
C3 10_556 C2 . C3 . 119.4(5) yes
C3 31_664 C3 . C2 . 120.2(2) yes
C3 31_664 C3 . H32 . 119.5 no
C2 . C3 . H32 . 119.9 no
C4 18_566 C4 . N1 . 111.1(4) yes
C4 18_566 C4 . H41 . 109.6 no
N1 . C4 . H41 . 109.1 no
C4 18_566 C4 . H42 . 108.9 no
N1 . C4 . H42 . 108.7 no
H41 . C4 . H42 . 109.5 no
C5 30_556 C5 . N1 . 110.9(4) yes
C5 30_556 C5 . H51 . 109.3 no
N1 . C5 . H51 . 109.0 no
C5 30_556 C5 . H52 . 109.2 no
N1 . C5 . H52 . 109.0 no
H51 . C5 . H52 . 109.5 no
H101 31_664 C10 . O10 31_664 125.2 no
H101 31_664 C10 . N10 . 125.1 no
O10 31_664 C10 . N10 . 109.6(5) yes
H101 31_664 C10 . O10 . 16.0 no
O10 31_664 C10 . O10 . 140.1(9) yes
N10 . C10 . O10 . 109.6(5) yes
H101 31_664 C10 . H101 . 109.8 no
O10 31_664 C10 . H101 . 16.0 no
N10 . C10 . H101 . 125.1 no
O10 . C10 . H101 . 125.2 no
N10 . C11 . H111 . 108.7 no
N10 . C11 . H112 . 108.4 no
H111 . C11 . H112 . 109.4 no
N10 . C11 . H113 . 111.2 no
H111 . C11 . H113 . 109.5 no
H112 . C11 . H113 . 109.5 no
C5 5_655 N1 . C5 9_665 82.7(3) yes
C5 5_655 N1 . C5 . 82.7(3) yes
C5 9_665 N1 . C5 . 138.2(8) yes
C5 5_655 N1 . C5 13_565 138.2(8) yes
C5 9_665 N1 . C5 13_565 82.7(3) yes
C5 . N1 . C5 13_565 82.7(3) yes
C5 5_655 N1 . C4 9_665 42.7(3) yes
C5 9_665 N1 . C4 9_665 41.0(3) yes
C5 . N1 . C4 9_665 119.8(5) yes
C5 13_565 N1 . C4 9_665 118.6(5) yes
C5 5_655 N1 . C4 . 118.6(5) yes
C5 9_665 N1 . C4 . 119.8(5) yes
C5 . N1 . C4 . 41.0(3) yes
C5 13_565 N1 . C4 . 42.7(3) yes
C4 9_665 N1 . C4 . 137.8(8) yes
C5 5_655 N1 . C4 13_565 119.8(5) yes
C5 9_665 N1 . C4 13_565 42.7(3) yes
C5 . N1 . C4 13_565 118.6(5) yes
C5 13_565 N1 . C4 13_565 41.0(3) yes
C4 9_665 N1 . C4 13_565 82.6(3) yes
C5 5_655 N1 . C4 5_655 41.0(3) yes
C5 9_665 N1 . C4 5_655 118.6(5) yes
C5 . N1 . C4 5_655 42.7(3) yes
C5 13_565 N1 . C4 5_655 119.8(5) yes
C4 9_665 N1 . C4 5_655 82.6(3) yes
C5 5_655 N1 . Zn1 . 110.9(4) yes
C5 9_665 N1 . Zn1 . 110.9(4) yes
C5 . N1 . Zn1 . 110.9(4) yes
C5 13_565 N1 . Zn1 . 110.9(4) yes
C4 9_665 N1 . Zn1 . 111.1(4) yes
C4 . N1 . C4 13_565 82.6(3) yes
C4 . N1 . C4 5_655 82.6(3) yes
C4 13_565 N1 . C4 5_655 137.8(8) yes
C4 . N1 . Zn1 . 111.1(4) yes
C4 13_565 N1 . Zn1 . 111.1(4) yes
C4 5_655 N1 . Zn1 . 111.1(4) yes
C10 . N10 . C11 . 121.4(6) yes
C10 . N10 . C11 31_664 121.4(6) yes
C11 . N10 . C11 31_664 113.3(9) yes
Zn1 . O1 . C1 . 127.0(4) yes
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
C4 . H42 . O10 19_644 131 0.97 2.56 3.286(15) yes
C5 13_565 H42 . O10 19_644 123 0.95 2.56 3.184(15) yes
C4 5_655 H52 . O10 31_664 133 0.96 2.56 3.286(15) yes
C5 . H52 . O10 31_664 122 0.97 2.56 3.184(15) yes



# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
1 2 3 x .
0 12 12 x .
1 1 4 x .
3 5 4 x .
2 5 5 x .
6 7 3 x .
4 5 7 x .
1 1 12 x .
1 2 19 x .
2 9 9 x .
9 12 1 x .
0 8 4 x .
3 17 8 x .
2 14 2 x .
2 16 12 x .
1 13 8 x .
1 13 10 x .
1 9 2 x .
1 5 0 x .
2 14 4 x .
7 11 14 x .
2 2 2 x .
4 5 3 x .
5 14 3 x .
1 2 15 x .
5 8 1 x .
4 8 4 x .
2 5 1 x .
1 1 16 x .
1 4 3 x .
10 11 3 x .
# looking for ARCHIVE-HKL.CIF 

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

data_2_FC70_032GPa
_database_code_depnum_ccdc_archive 'CCDC 2087898'
loop_
_audit_author_name
_audit_author_address
'Stephen Moggach'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2021-06-03 deposited with the CCDC.	2021-09-29 downloaded from the CCDC.
;
_audit_creation_date             2021-05-26
_audit_creation_method           CRYSTALS_ver_14.61_build_6999

_refine_special_details          
; 
023_ALERT_3_A Resolution (too) Low [sin(theta)/Lambda < 0.6]..       0.50 Ang-1
027_ALERT_3_A _diffrn_reflns_theta_full value (too) Low ......      10.54 Degree
029_ALERT_3_A _diffrn_measured_fraction_theta_full value Low .      0.482 Why?
911_ALERT_3_B Missing FCF Refl Between Thmin & STh/L=    0.500        138 Report
088_ALERT_3_A Poor Data / Parameter Ratio ....................       5.44 Note
913_ALERT_3_C Missing # of Very Strong Reflections in FCF ....          4 Note

These are caused by shading from the pressure cell.

084_ALERT_3_A High wR2 Value (i.e. > 0.25) ...................       0.59 Report
082_ALERT_2_B High R1 Value ..................................       0.19 Report
201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) .......          4 Report
              N1        C1        C2        C3
202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent .........          3 Check
              N10     C10     C11
341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............    0.01375 Ang.

These are all caused by disorder on the DABCO ligand and DMF solvent.

601_ALERT_2_B Unit Cell Contains Solvent Accessible VOIDS of .        200 Ang**3
329_ALERT_4_C Carbon Atom Hybridisation Unclear for ..........        C10 Check

These are correct.

992_ALERT_5_B Repd & Actual _reflns_number_gt Values Differ by         34 Check

This has been checked.


#===============================================================================
002_ALERT_2_G Number of Distance or Angle Restraints on AtSite         12 Note
003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...         11 Report
042_ALERT_1_G Calc. and Reported Moiety Formula Strings Differ     Please Check
092_ALERT_4_G Check: Wavelength Given is not Cu,Ga,Mo,Ag,In Ka    0.48590 Ang.
300_ALERT_4_G Atom Site Occupancy of C4         Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of C5         Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H41        Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H42        Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H51        Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H52        Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of O10        Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of H101       Constrained at        0.5 Check
301_ALERT_3_G Main Residue  Disorder ..............(Resd  1  )        14% Note
302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd  2  )        20% Note
760_ALERT_1_G CIF Contains no Torsion Angles .................          ? Info
769_ALERT_4_G CIF Embedded explicitly supplied scattering data     Please Note
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      16.70 Deg.
              H101 -C10  -O10    31_664   1_555   1_555 ......     #   35 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      16.70 Deg.
              O10  -C10  -H101   31_664   1_555   1_555 ......     #   39 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      42.70 Deg.
              C4   -N1   -C5      9_665   1_555   5_655 ......     #   54 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      42.70 Deg.
              C4   -N1   -C5      5_655   1_555   5_655 ......     #   56 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      42.70 Deg.
              C4   -N1   -C5      1_555   1_555   1_555 ......     #   59 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      42.70 Deg.
              C4   -N1   -C5      5_655   1_555   1_555 ......     #   60 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      42.70 Deg.
              C4   -N1   -C5      9_665   1_555   9_665 ......     #   63 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      42.70 Deg.
              C4   -N1   -C5     13_565   1_555   9_665 ......     #   66 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      42.70 Deg.
              C4   -N1   -C5      1_555   1_555  13_565 ......     #   69 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      42.70 Deg.
              C4   -N1   -C5     13_565   1_555  13_565 ......     #   71 Check
804_ALERT_5_G Number of ARU-Code Packing Problem(s) in PLATON           1 Info
809_ALERT_1_G Can not Parse the SHELXL Weighting Scheme String     Please Check
860_ALERT_3_G Number of Least-Squares Restraints .............         79 Note
909_ALERT_3_G Percentage of I>2sig(I) Data at Theta(Max) Still        68% Note
910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min).          4 Note
929_ALERT_5_G No Weight Pars,Obs and Calc R1,wR2,S not Checked          ! Info
958_ALERT_1_G Calculated (ThMax) and Actual (FCF) Lmax Differ          11 Units
960_ALERT_3_G Number of Intensities with I  <   - 2*sig(I) ...          3 Check
#=============================================================================== 
;

_cell_length_a                   14.9647(9)
_cell_length_b                   14.9647(9)
_cell_length_c                   19.266(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4314.4(11)

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I 4/m c m '
_symmetry_space_group_name_Hall  '-I 4 2c'
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
-y,x,z
y,-x,-z
-y+1/2,x+1/2,z+1/2
y+1/2,-x+1/2,-z+1/2
-x,-y,z
x,y,-z
-x+1/2,-y+1/2,z+1/2
x+1/2,y+1/2,-z+1/2
y,-x,z
-y,x,-z
y+1/2,-x+1/2,z+1/2
-y+1/2,x+1/2,-z+1/2
-x,y,z+1/2
x,-y,-z+1/2
-x+1/2,y+1/2,z+1
x+1/2,-y+1/2,-z+1
y,x,z+1/2
-y,-x,-z+1/2
y+1/2,x+1/2,z+1
-y+1/2,-x+1/2,-z+1
x,-y,z+1/2
-x,y,-z+1/2
x+1/2,-y+1/2,z+1
-x+1/2,y+1/2,-z+1
-y,-x,z+1/2
y,x,-z+1/2
-y+1/2,-x+1/2,z+1
y+1/2,x+1/2,-z+1

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 0.0006 0.0007 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 0.0016 0.0014 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 0.0036 0.0026 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 0.3043 0.7255 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 = C40 H30 N10 O20 Zn8 
# Dc =      2.30 Fooo =   2960.00 Mu =     44.69 M =   1493.77
# Found Formula = C34 H48 N6 O12 Zn2 
# Dc =      1.33 FOOO =   1800.00 Mu =     11.73 M =    863.55

_chemical_formula_sum            'C34 H48 N6 O12 Zn2'
_chemical_formula_moiety         '(C22 H20 N2 O8 Zn2)n. 4(C3H7NO)'
_chemical_compound_source        .
_chemical_formula_weight         863.55


_cell_measurement_reflns_used    4199
_cell_measurement_theta_min      2
_cell_measurement_theta_max      14
_cell_measurement_temperature    298

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.050
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.150

_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1800
_exptl_absorpt_coefficient_mu    1.173

# Sheldrick geometric approximatio 0.84 0.94 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_T_max  0.94
_diffrn_measurement_device_type  Synchrotron
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.48590
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_reduction        
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      298
_diffrn_ambient_pressure         320000
_diffrn_reflns_number            5869
_diffrn_reflns_av_unetI/netI     0.089
_reflns_number_total             301
_diffrn_reflns_av_R_equivalents  0.068
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 301 
# Theoretical number of reflections is about 1128 


_diffrn_reflns_theta_min         2.202
_diffrn_reflns_theta_max         14.054
_diffrn_measured_fraction_theta_max 0.472

_diffrn_reflns_theta_full        10.540
_diffrn_measured_fraction_theta_full 0.482


_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       8
_reflns_limit_h_min              0
_reflns_limit_h_max              10
_reflns_limit_k_min              2
_reflns_limit_k_max              14
_reflns_limit_l_min              0
_reflns_limit_l_max              8

_oxford_diffrn_Wilson_B_factor   1.61
_oxford_diffrn_Wilson_scale      871.13

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

_refine_diff_density_min         -0.60
_refine_diff_density_max         0.65


# 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_refine_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_restraints     79
_refine_ls_number_parameters     48
_refine_ls_number_reflns         261
_oxford_refine_ls_R_factor_ref   0.1045
_refine_ls_wR_factor_ref         0.2208
_refine_ls_goodness_of_fit_ref   1.0291
_refine_ls_shift/su_max          0.0084893
_refine_ls_shift/su_mean         0.0002752


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        301
_refine_ls_R_factor_all          0.2081
_refine_ls_wR_factor_all         0.5903

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                244
_refine_ls_R_factor_gt           0.1925
_refine_ls_wR_factor_gt          0.5828


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.08P)² +*****P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

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

# Replace last . with number of unfound hydrogen atoms attached 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 0.5000 0.5787(4) 0.0678 1.0000 Uani DS T . . . .
C1 C 0.6497(10) 0.5800(12) 0.5000 0.062(4) 1.0000 Uiso DS U . . . .
C2 C 0.7310(9) 0.6382(11) 0.5000 0.062(3) 1.0000 Uiso DS U . . . .
C3 C 0.7654(7) 0.6687(7) 0.5616(3) 0.063(3) 1.0000 Uiso D U . . . .
C4 C 0.5938(9) 0.5003(3) 0.7100(2) 0.073(6) 0.3750 Uiso D U . . . .
C5 C 0.5656(7) 0.5660(7) 0.7100(2) 0.073(6) 0.3750 Uiso D U . . . .
C10 C 0.667(2) 0.833(2) 0.722(3) 0.314(17) 1.0000 Uiso DS U . . . .
C11 C 0.5722(18) 0.8139(17) 0.610(3) 0.313(17) 1.0000 Uiso D U . . . .
N1 N 0.5000 0.5000 0.6868(17) 0.073(6) 1.0000 Uiso DS U . . . .
N10 N 0.6364(17) 0.8636(17) 0.651(3) 0.313(17) 1.0000 Uiso DS U . . . .
O1 O 0.6229(7) 0.5523(6) 0.5576(3) 0.0797 1.0000 Uani D U . . . .
O10 O 0.727(2) 0.884(2) 0.744(3) 0.314(17) 0.5000 Uiso D U . . . .
H32 H 0.7403 0.6502 0.6042 0.0722 1.0000 Uiso R . . . . .
H111 H 0.5575 0.8481 0.5688 0.3980 1.0000 Uiso R . . . . .
H112 H 0.5188 0.8056 0.6384 0.3980 1.0000 Uiso R . . . . .
H113 H 0.5957 0.7561 0.5967 0.3980 1.0000 Uiso R . . . . .
H41 H 0.6236 0.5533 0.6940 0.0665 0.3750 Uiso R . . . . .
H42 H 0.6249 0.4485 0.6929 0.0665 0.3750 Uiso R . . . . .
H51 H 0.6242 0.5500 0.6937 0.0662 0.3750 Uiso R . . . . .
H52 H 0.5505 0.6246 0.6932 0.0662 0.3750 Uiso R . . . . .
H101 H 0.6432 0.7841 0.7469 0.3768 0.5000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.2587(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
Zn1 . O1 5_655 2.039(9) yes
Zn1 . O1 9_665 2.039(9) yes
Zn1 . O1 13_565 2.039(9) yes
Zn1 . N1 . 2.08(3) yes
Zn1 . O1 . 2.039(9) yes
C1 . O1 10_556 1.251(6) yes
C1 . C2 . 1.495(7) yes
C1 . O1 . 1.251(6) yes
C2 . C3 10_556 1.372(6) yes
C2 . C3 . 1.372(6) yes
C3 . C3 31_664 1.393(8) yes
C3 . H32 . 0.945 no
C4 . C4 18_566 1.540(9) yes
C4 . N1 . 1.474(8) yes
C4 . H41 . 0.962 no
C4 . H42 . 0.962 no
C5 . C5 30_556 1.540(9) yes
C5 . N1 . 1.463(8) yes
C5 . H51 . 0.962 no
C5 . H52 . 0.962 no
C10 . H101 31_664 0.943 no
C10 . O10 31_664 1.250(6) yes
C10 . N10 . 1.523(9) yes
C10 . O10 . 1.250(6) yes
C10 . H101 . 0.943 no
C11 . N10 . 1.443(8) yes
C11 . H111 . 0.975 no
C11 . H112 . 0.972 no
C11 . H113 . 0.970 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
O1 5_655 Zn1 . O1 9_665 87.73(11) yes
O1 5_655 Zn1 . O1 13_565 157.1(6) yes
O1 9_665 Zn1 . O1 13_565 87.73(11) yes
O1 5_655 Zn1 . N1 . 101.5(3) yes
O1 9_665 Zn1 . N1 . 101.5(3) yes
O1 13_565 Zn1 . N1 . 101.5(3) yes
O1 5_655 Zn1 . O1 . 87.73(11) yes
O1 9_665 Zn1 . O1 . 157.1(6) yes
O1 13_565 Zn1 . O1 . 87.73(11) yes
N1 . Zn1 . O1 . 101.5(3) yes
O1 10_556 C1 . C2 . 117.0(4) yes
O1 10_556 C1 . O1 . 125.1(7) yes
C2 . C1 . O1 . 117.0(4) yes
C1 . C2 . C3 10_556 120.0(3) yes
C1 . C2 . C3 . 120.0(3) yes
C3 10_556 C2 . C3 . 119.7(6) yes
C3 31_664 C3 . C2 . 120.1(3) yes
C3 31_664 C3 . H32 . 119.2 no
C2 . C3 . H32 . 120.3 no
C4 18_566 C4 . N1 . 107.7(13) yes
C4 18_566 C4 . H41 . 109.0 no
N1 . C4 . H41 . 110.2 no
C4 18_566 C4 . H42 . 109.8 no
N1 . C4 . H42 . 110.7 no
H41 . C4 . H42 . 109.3 no
C5 30_556 C5 . N1 . 107.8(14) yes
C5 30_556 C5 . H51 . 108.8 no
N1 . C5 . H51 . 110.1 no
C5 30_556 C5 . H52 . 110.0 no
N1 . C5 . H52 . 110.8 no
H51 . C5 . H52 . 109.3 no
H101 31_664 C10 . O10 31_664 125.1 no
H101 31_664 C10 . N10 . 125.2 no
O10 31_664 C10 . N10 . 109.6(6) yes
H101 31_664 C10 . O10 . 16.7 no
O10 31_664 C10 . O10 . 139.8(8) yes
N10 . C10 . O10 . 109.6(6) yes
H101 31_664 C10 . H101 . 109.4 no
O10 31_664 C10 . H101 . 16.7 no
N10 . C10 . H101 . 125.2 no
O10 . C10 . H101 . 125.1 no
N10 . C11 . H111 . 108.8 no
N10 . C11 . H112 . 108.2 no
H111 . C11 . H112 . 109.8 no
N10 . C11 . H113 . 111.3 no
H111 . C11 . H113 . 109.1 no
H112 . C11 . H113 . 109.6 no
C4 9_665 N1 . C4 . 145(3) yes
C4 9_665 N1 . C4 5_655 84.7(8) yes
C4 . N1 . C4 5_655 84.7(8) yes
C4 9_665 N1 . C4 13_565 84.7(8) yes
C4 . N1 . C4 13_565 84.7(8) yes
C4 5_655 N1 . C4 13_565 145(3) yes
C4 9_665 N1 . C5 5_655 42.7(4) yes
C4 . N1 . C5 5_655 123.2(16) yes
C4 5_655 N1 . C5 5_655 42.7(4) yes
C4 13_565 N1 . C5 5_655 123.2(16) yes
C4 9_665 N1 . C5 . 123.2(16) yes
C4 . N1 . C5 . 42.7(4) yes
C4 5_655 N1 . C5 . 42.7(4) yes
C4 13_565 N1 . C5 . 123.2(16) yes
C5 5_655 N1 . C5 . 84.6(8) yes
C4 9_665 N1 . C5 9_665 42.7(4) yes
C4 . N1 . C5 9_665 123.2(16) yes
C4 5_655 N1 . C5 9_665 123.2(16) yes
C4 13_565 N1 . C5 9_665 42.7(4) yes
C5 5_655 N1 . C5 9_665 84.6(8) yes
C4 9_665 N1 . C5 13_565 123.2(16) yes
C4 . N1 . C5 13_565 42.7(4) yes
C4 5_655 N1 . C5 13_565 123.2(16) yes
C4 13_565 N1 . C5 13_565 42.7(4) yes
C5 5_655 N1 . C5 13_565 144(3) yes
C4 9_665 N1 . Zn1 . 107.7(13) yes
C4 . N1 . Zn1 . 107.7(13) yes
C4 5_655 N1 . Zn1 . 107.7(13) yes
C4 13_565 N1 . Zn1 . 107.7(13) yes
C5 5_655 N1 . Zn1 . 107.9(14) yes
C5 . N1 . C5 9_665 144(3) yes
C5 . N1 . C5 13_565 84.6(8) yes
C5 9_665 N1 . C5 13_565 84.6(8) yes
C5 . N1 . Zn1 . 107.9(14) yes
C5 9_665 N1 . Zn1 . 107.9(14) yes
C5 13_565 N1 . Zn1 . 107.9(14) yes
C10 . N10 . C11 . 122.2(6) yes
C10 . N10 . C11 31_664 122.2(6) yes
C11 . N10 . C11 31_664 113.3(8) yes
Zn1 . O1 . C1 . 126.4(7) yes



# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
3 6 1 x .
6 12 0 x .
2 14 6 x .
5 8 1 x .
6 9 5 x .
10 11 1 x .
3 14 5 x .
7 12 7 x .
9 10 1 x .
3 13 2 x .
6 12 2 x .
1 11 4 x .
1 11 8 x .
4 6 6 x .
3 11 8 x .
4 14 4 x .
6 7 3 x .
6 9 1 x .
2 13 3 x .
5 14 1 x .
6 6 2 x .
2 9 3 x .
9 9 2 x .
3 13 0 x .
1 5 2 x .
2 4 2 x .
8 9 3 x .
6 7 1 x .
0 4 0 x .
1 8 3 x .
5 8 3 x .
3 3 2 x .
7 9 8 x .
10 10 2 x .
8 8 0 x .
7 8 1 x .
8 8 2 x .
1 4 3 x .
4 11 1 x .
2 11 1 x .
0 12 8 x .
# looking for ARCHIVE-HKL.CIF 

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

data_1_EtOH_0GPa
_database_code_depnum_ccdc_archive 'CCDC 2087901'
loop_
_audit_author_name
_audit_author_address
'Stephen Moggach'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2021-06-03 deposited with the CCDC.	2021-09-29 downloaded from the CCDC.
;
_audit_creation_date             2021-05-26
_audit_creation_method           CRYSTALS_ver_14.61_build_6999

_refine_special_details          
; 
430_ALERT_2_A Short Inter D...A Contact  N1       ..N1       .       2.59 Ang.
                                                     y,x,-z  =     13_555 Check

This is correct, and corresponds to the DABCO N...N distance.

241_ALERT_2_C High   'MainMol' Ueq as Compared to Neighbors of         O1 Check
242_ALERT_2_C Low    'MainMol' Ueq as Compared to Neighbors of        Zn1 Check
242_ALERT_2_C Low    'MainMol' Ueq as Compared to Neighbors of         N1 Check
245_ALERT_2_C U(iso) H13       Smaller than U(eq) C4        by      0.015 Ang**2
250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....        3.0 Note

These are caused by disorder of the DABCO ligand.


#===============================================================================
003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...          7 Report
004_ALERT_5_G Polymeric Structure Found with Maximum Dimension          3 Info
042_ALERT_1_G Calc. and Reported Moiety Formula Strings Differ     Please Check
045_ALERT_1_G Calculated and Reported Z Differ by a Factor ...       2.00 Check
143_ALERT_4_G s.u. on c - Axis Small or Missing ..............    0.00004 Ang.
180_ALERT_4_G Check Cell Rounding: # of Values Ending with 0 =          3 Note
300_ALERT_4_G Atom Site Occupancy of C4         Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of C5         Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H13        Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H51        Constrained at      0.375 Check
300_ALERT_4_G Atom Site Occupancy of H53        Constrained at      0.375 Check
301_ALERT_3_G Main Residue  Disorder ..............(Resd  1  )        22% Note
432_ALERT_2_G Short Inter X...Y Contact  N1       ..C5               2.45 Ang.
                                                   x,1-y,-z  =      9_565 Check
432_ALERT_2_G Short Inter X...Y Contact  N1       ..C5               2.45 Ang.
                                                 1-y,1-x,-z  =      4_665 Check
432_ALERT_2_G Short Inter X...Y Contact  N1       ..C4               2.47 Ang.
                                                   y,1-x,-z  =     12_565 Check
432_ALERT_2_G Short Inter X...Y Contact  N1       ..C4               2.47 Ang.
                                                 1-y,1-x,-z  =      4_665 Check
432_ALERT_2_G Short Inter X...Y Contact  C2       ..C3               2.39 Ang.
                                                   -x,y,1-z  =      5_556 Check
432_ALERT_2_G Short Inter X...Y Contact  C3       ..C3               2.73 Ang.
                                                   -x,y,1-z  =      5_556 Check
432_ALERT_2_G Short Inter X...Y Contact  C4       ..C4               2.47 Ang.
                                                   y,1-x,-z  =     12_565 Check
432_ALERT_2_G Short Inter X...Y Contact  C4       ..C5               2.93 Ang.
                                                   x,1-y,-z  =      9_565 Check
432_ALERT_2_G Short Inter X...Y Contact  C4       ..C5               2.93 Ang.
                                                 1-y,1-x,-z  =      4_665 Check
432_ALERT_2_G Short Inter X...Y Contact  C4       ..C4               3.13 Ang.
                                                 1-y,1-x,-z  =      4_665 Check
432_ALERT_2_G Short Inter X...Y Contact  C5       ..C5               2.43 Ang.
                                                 1-y,1-x,-z  =      4_665 Check
432_ALERT_2_G Short Inter X...Y Contact  C5       ..C5               3.08 Ang.
                                                   x,1-y,-z  =      9_565 Check
605_ALERT_4_G Largest Solvent Accessible VOID in the Structure        702 A**3
760_ALERT_1_G CIF Contains no Torsion Angles .................          ? Info
769_ALERT_4_G CIF Embedded explicitly supplied scattering data     Please Note
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       1.40 Deg.
              H51  -C4   -H53     3_555   1_555   8_565 ......     #   30 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      10.30 Deg.
              H13  -C4   -H53     3_555   1_555  10_655 ......     #   32 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       9.40 Deg.
              H51  -C4   -H13     3_555   1_555   1_555 ......     #   42 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      10.30 Deg.
              H53  -C4   -H13     8_565   1_555   1_555 ......     #   43 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       9.40 Deg.
              H13  -C4   -H51     3_555   1_555   1_555 ......     #   46 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       1.40 Deg.
              H53  -C4   -H51    10_655   1_555   1_555 ......     #   49 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       0.70 Deg.
              H53  -C5   -H51    10_655   1_555   1_555 ......     #   57 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...       0.70 Deg.
              H51  -C5   -H53    10_655   1_555   1_555 ......     #   61 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.80 Deg.
              C4   -N1   -C5     14_665   1_555  11_655 ......     #   76 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.80 Deg.
              C4   -N1   -C5     10_655   1_555  11_655 ......     #   77 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.80 Deg.
              C4   -N1   -C5      8_565   1_555  15_665 ......     #   78 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.80 Deg.
              C4   -N1   -C5     14_665   1_555  15_665 ......     #   80 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.80 Deg.
              C4   -N1   -C5      8_565   1_555   3_555 ......     #   83 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.80 Deg.
              C4   -N1   -C5      1_555   1_555   3_555 ......     #   84 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.80 Deg.
              C4   -N1   -C5      1_555   1_555   1_555 ......     #   94 Check
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF ...      41.80 Deg.
              C4   -N1   -C5     10_655   1_555   1_555 ......     #   96 Check
860_ALERT_3_G Number of Least-Squares Restraints .............         73 Note
869_ALERT_4_G ALERTS Related to the Use of SQUEEZE Suppressed           ! Info
910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min).          1 Note
912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600          2 Note
913_ALERT_3_G Missing # of Very Strong Reflections in FCF ....          1 Note
#===============================================================================

No action taken.
;

_cell_length_a                   10.91350(4)
_cell_length_b                   10.91350(4)
_cell_length_c                   9.62600(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1146.500(10)

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P 4/m m m '
_symmetry_space_group_name_Hall  '-P 4 2'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
y,x,z
-y,-x,-z
-x,y,-z
x,-y,z
-y,x,-z
y,-x,z
x,-y,-z
-x,y,z
-y,x,z
y,-x,-z
y,x,-z
-y,-x,z
-x,-y,z
x,y,-z

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            1

# Given Formula = C22 H20 N2 O8 Zn2 
# Dc =      0.83 Fooo =    290.00 Mu =     10.71 M =    571.17
# Found Formula = C22 H26 N2 O8 Zn2 
# Dc =      0.84 FOOO =    296.00 Mu =     10.72 M =    577.22

_chemical_formula_sum            'C29.8 H49.4 O11.9 N2 Zn2'
_chemical_formula_moiety         '(C22 H26 N2 O8 Zn2)n 3.9 (C2 O H6)'
_chemical_compound_source        .
_chemical_formula_weight         756.9

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 -0.002 -0.002 -0.021 695 102 '3.9 (C2 O H6) '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
see text for details
;

_cell_measurement_reflns_used    24471
_cell_measurement_theta_min      2
_cell_measurement_theta_max      26
_cell_measurement_temperature    298

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.050
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.150

_exptl_crystal_density_diffrn    1.097
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             397.4
_exptl_absorpt_coefficient_mu    1.09

# Sheldrick geometric approximatio 0.85 0.95 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_T_max  0.95
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      298
_diffrn_ambient_pressure         101
_diffrn_reflns_number            24471
_diffrn_reflns_av_unetI/netI     0.055
_reflns_number_total             745
_diffrn_reflns_av_R_equivalents  0.043
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 745 
# Theoretical number of reflections is about 1177 


_diffrn_reflns_theta_min         2.116
_diffrn_reflns_theta_max         26.406
_diffrn_measured_fraction_theta_max 0.996

_diffrn_reflns_theta_full        26.406
_diffrn_measured_fraction_theta_full 0.996


_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_reflns_limit_h_min              0
_reflns_limit_h_max              9
_reflns_limit_k_min              0
_reflns_limit_k_max              13
_reflns_limit_l_min              0
_reflns_limit_l_max              12

_oxford_diffrn_Wilson_B_factor   1.53
_oxford_diffrn_Wilson_scale      29.42

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

_refine_diff_density_min         -0.37
_refine_diff_density_max         0.36


# 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_refine_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_restraints     73
_refine_ls_number_parameters     31
_refine_ls_number_reflns         745
_oxford_refine_ls_R_factor_ref   0.0246
_refine_ls_wR_factor_ref         0.0668
_refine_ls_goodness_of_fit_ref   1.0364
_refine_ls_shift/su_max          0.0087092
_refine_ls_shift/su_mean         0.0003984


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        745
_refine_ls_R_factor_all          0.0246
_refine_ls_wR_factor_all         0.0668

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                718
_refine_ls_R_factor_gt           0.0241
_refine_ls_wR_factor_gt          0.0665


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #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 + 0.47P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

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

# Replace last . with number of unfound hydrogen atoms attached 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 0.5000 0.34860(4) 0.0256 1.0000 Uani S T . . . .
C1 C 0.2651(2) 0.5000 0.5000 0.0432 1.0000 Uani S TU . . . .
C2 C 0.1276(3) 0.5000 0.5000 0.0495 1.0000 Uani S TU . . . .
C3 C 0.0635(2) 0.5000 0.3779(2) 0.0858 1.0000 Uani S TU . . . .
C4 C 0.4116(3) 0.4116(3) 0.0802(5) 0.0615 0.3750 Uani S U . . . .
C5 C 0.5000 0.3773(5) 0.0791(5) 0.0605 0.3750 Uani S U . . . .
N1 N 0.5000 0.5000 0.1343 0.0301 1.0000 Uani . U . . . .
O1 O 0.31747(14) 0.5000 0.38492(16) 0.0607 1.0000 Uani S TU . . . .
H13 H 0.3305 0.4393 0.1007 0.0468 0.3750 Uiso R . . . . .
H51 H 0.4292 0.3360 0.1113 0.0743 0.3750 Uiso R . . . . .
H53 H 0.5728 0.3360 0.1113 0.0743 0.3750 Uiso R . . . . .
H32 H 0.1060 0.5000 0.2918 0.1028 1.0000 Uiso RS . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.744(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 . Zn1 2_666 2.9147(7) yes
Zn1 . O1 3_555 2.0225(15) yes
Zn1 . O1 8_565 2.0225(15) yes
Zn1 . O1 10_655 2.0225(15) yes
Zn1 . O1 . 2.0225(15) yes
Zn1 . N1 . 2.0633(3) yes
C1 . O1 9_566 1.2463(19) yes
C1 . C2 . 1.500(4) yes
C1 . O1 . 1.2463(19) yes
C2 . C3 9_566 1.368(3) yes
C2 . C3 . 1.368(3) yes
C3 . C3 10_555 1.385(5) yes
C3 . H32 . 0.950 no
C4 . C4 13_555 1.543(9) yes
C4 . H13 3_555 0.956 no
C4 . H51 3_555 0.898 no
C4 . H53 8_565 0.894 no
C4 . H53 10_655 0.894 no
C4 . N1 . 1.461(5) yes
C4 . H13 . 0.956 no
C4 . H51 . 0.898 no
C5 . C5 5_655 1.524(10) yes
C5 . H53 10_655 0.965 no
C5 . H51 10_655 0.947 no
C5 . H51 . 0.947 no
C5 . H53 . 0.965 no
C5 . N1 . 1.440(5) yes
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
Zn1 2_666 Zn1 . O1 3_555 80.04(4) yes
Zn1 2_666 Zn1 . O1 8_565 80.04(4) yes
O1 3_555 Zn1 . O1 8_565 160.09(9) yes
Zn1 2_666 Zn1 . O1 10_655 80.04(4) yes
O1 3_555 Zn1 . O1 10_655 88.287(15) yes
O1 8_565 Zn1 . O1 10_655 88.287(15) yes
Zn1 2_666 Zn1 . O1 . 80.04(4) yes
O1 3_555 Zn1 . O1 . 88.287(15) yes
O1 8_565 Zn1 . O1 . 88.287(15) yes
O1 10_655 Zn1 . O1 . 160.09(9) yes
Zn1 2_666 Zn1 . N1 . 179.99 yes
O1 3_555 Zn1 . N1 . 99.96(4) yes
O1 8_565 Zn1 . N1 . 99.95(4) yes
O1 10_655 Zn1 . N1 . 99.95(4) yes
O1 . Zn1 . N1 . 99.96(4) yes
O1 9_566 C1 . C2 . 117.27(13) yes
O1 9_566 C1 . O1 . 125.5(3) yes
C2 . C1 . O1 . 117.27(13) yes
C1 . C2 . C3 9_566 120.79(14) yes
C1 . C2 . C3 . 120.79(14) yes
C3 9_566 C2 . C3 . 118.4(3) yes
C3 10_555 C3 . C2 . 120.79(14) yes
C3 10_555 C3 . H32 . 119.2 no
C2 . C3 . H32 . 120.0 no
C4 13_555 C4 . H13 3_555 101.9 no
C4 13_555 C4 . H51 3_555 109.5 no
H13 3_555 C4 . H51 3_555 114.8 no
C4 13_555 C4 . H53 8_565 109.6 no
H13 3_555 C4 . H53 8_565 113.5 no
H51 3_555 C4 . H53 8_565 1.4 no
C4 13_555 C4 . H53 10_655 109.6 no
H13 3_555 C4 . H53 10_655 10.3 no
H51 3_555 C4 . H53 10_655 105.1 no
H53 8_565 C4 . H53 10_655 103.8 no
C4 13_555 C4 . N1 . 110.89(19) yes
H13 3_555 C4 . N1 . 109.2 no
H51 3_555 C4 . N1 . 110.3 no
H53 8_565 C4 . N1 . 111.3 no
H53 10_655 C4 . N1 . 111.3 no
C4 13_555 C4 . H13 . 101.9 no
H13 3_555 C4 . H13 . 122.9 no
H51 3_555 C4 . H13 . 9.4 no
H53 8_565 C4 . H13 . 10.3 no
H53 10_655 C4 . H13 . 113.5 no
C4 13_555 C4 . H51 . 109.5 no
H13 3_555 C4 . H51 . 9.4 no
H51 3_555 C4 . H51 . 106.3 no
H53 8_565 C4 . H51 . 105.1 no
H53 10_655 C4 . H51 . 1.4 no
N1 . C4 . H13 . 109.2 no
N1 . C4 . H51 . 110.3 no
H13 . C4 . H51 . 114.8 no
C5 5_655 C5 . H53 10_655 108.7 no
C5 5_655 C5 . H51 10_655 109.1 no
H53 10_655 C5 . H51 10_655 110.2 no
C5 5_655 C5 . H51 . 109.1 no
H53 10_655 C5 . H51 . 0.7 no
H51 10_655 C5 . H51 . 109.5 no
C5 5_655 C5 . H53 . 108.7 no
H53 10_655 C5 . H53 . 110.9 no
H51 10_655 C5 . H53 . 0.7 no
H51 . C5 . H53 . 110.2 no
C5 5_655 C5 . N1 . 111.6(2) yes
H53 10_655 C5 . N1 . 108.4 no
H51 10_655 C5 . N1 . 108.8 no
H51 . C5 . N1 . 108.8 no
H53 . C5 . N1 . 108.4 no
C4 8_565 N1 . C4 . 82.70(13) yes
C4 8_565 N1 . C4 14_665 82.70(13) yes
C4 . N1 . C4 14_665 138.2(4) yes
C4 8_565 N1 . C4 10_655 138.2(4) yes
C4 . N1 . C4 10_655 82.70(13) yes
C4 14_665 N1 . C4 10_655 82.70(13) yes
C4 8_565 N1 . C5 11_655 118.88(15) yes
C4 . N1 . C5 11_655 118.88(15) yes
C4 14_665 N1 . C5 11_655 41.80(3) yes
C4 10_655 N1 . C5 11_655 41.80(3) yes
C4 8_565 N1 . C5 15_665 41.80(3) yes
C4 . N1 . C5 15_665 118.88(15) yes
C4 14_665 N1 . C5 15_665 41.80(3) yes
C4 10_655 N1 . C5 15_665 118.88(15) yes
C5 11_655 N1 . C5 15_665 82.20(14) yes
C4 8_565 N1 . C5 3_555 41.80(3) yes
C4 . N1 . C5 3_555 41.80(3) yes
C4 14_665 N1 . C5 3_555 118.88(15) yes
C4 10_655 N1 . C5 3_555 118.88(15) yes
C5 11_655 N1 . C5 3_555 136.8(4) yes
C4 8_565 N1 . Zn1 . 110.89(19) yes
C4 . N1 . Zn1 . 110.89(19) yes
C4 14_665 N1 . Zn1 . 110.89(19) yes
C4 10_655 N1 . Zn1 . 110.89(19) yes
C5 11_655 N1 . Zn1 . 111.6(2) yes
C4 8_565 N1 . C5 . 118.88(15) yes
C4 . N1 . C5 . 41.80(3) yes
C4 14_665 N1 . C5 . 118.88(15) yes
C4 10_655 N1 . C5 . 41.80(3) yes
C5 11_655 N1 . C5 . 82.20(14) yes
C5 15_665 N1 . C5 3_555 82.20(14) yes
C5 15_665 N1 . Zn1 . 111.6(2) yes
C5 3_555 N1 . Zn1 . 111.6(2) yes
C5 15_665 N1 . C5 . 136.8(4) yes
C5 3_555 N1 . C5 . 82.20(14) yes
Zn1 . N1 . C5 . 111.6(2) yes
Zn1 . O1 . C1 . 127.23(15) yes
C5 . H51 . C4 . 68.2 no
C5 . H53 . C4 11_655 67.6 no


# looking for ARCHIVE-HKL.CIF 

