# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

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

data_ZIF-7-IV/0.4GPa
_database_code_depnum_ccdc_archive 'CCDC 1036075'
_audit_update_record             
;
2014-11-25 deposited with the CCDC.
2015-01-23 downloaded from the CCDC.
;
_chemical_name_mineral           ZIF-7-IV(0.4GPa)
_cell_length_a                   14.29698
_cell_length_b                   14.17061
_cell_length_c                   14.32013
_cell_angle_alpha                107.4945
_cell_angle_beta                 108.1296
_cell_angle_gamma                106.599
_cell_volume                     2388.448
_symmetry_space_group_name_H-M   P-1
loop_
_symmetry_equiv_pos_as_xyz
'-x, -y, -z'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
Cd1A C 0 1.47675 0.81904 1.15655 1 1
N1A N 0 1.38985 0.7623635 1.096712 1 1
C1A C 0 1.478678 0.8490975 1.12524 1 1
H1A H 0 1.481582 0.8882995 1.08372 1 1
N3A N 0 1.563983 0.8766389 1.217715 1 1
C2A C 0 1.419612 0.7259439 1.177282 1 1
C3A C 0 1.361412 0.6401588 1.191698 1 1
H3A H 0 1.290203 0.59289 1.142278 1 1
C4A C 0 1.413301 0.6271768 1.28192 1 1
H4A H 0 1.376407 0.569471 1.293492 1 1
C5A C 0 1.521698 0.6996137 1.358475 1 1
H5A H 0 1.554318 0.6880733 1.418726 1 1
C6A C 0 1.527247 0.7978965 1.253165 1 1
C7A C 0 1.579079 0.7858751 1.345233 1 1
H7A H 0 1.649731 0.8343943 1.395847 1 1
Cd1B C 0 0.79866 1.16352 1.4999 1 1
N1B N 0 0.7360599 1.10992 1.413012 1 1
C1B C 0 0.8040511 1.117335 1.505743 1 1
H1B H 0 0.8106962 1.056524 1.513797 1 1
N3B N 0 0.8625627 1.218049 1.587098 1 1
C2B C 0 0.7481171 1.216943 1.43538 1 1
C3B C 0 0.6996942 1.260008 1.370667 1 1
H3B H 0 0.6476102 1.216132 1.299439 1 1
C4B C 0 0.7312932 1.370455 1.416093 1 1
H4B H 0 0.6994565 1.4019 1.374703 1 1
C5B C 0 0.8115975 1.438312 1.524468 1 1
H5B H 0 0.8308415 1.513009 1.552585 1 1
C6B C 0 0.8278064 1.284177 1.543003 1 1
C7B C 0 0.8610375 1.395944 1.588317 1 1
H7B H 0 0.9146769 1.440206 1.658994 1 1
Cd1C C 0 1.14354 1.51512 0.80672 1 1
N1C N 0 1.095435 1.425635 0.7498532 1 1
C1C C 0 1.096102 1.523881 0.7893259 1 1
H1C H 0 1.033882 1.535682 0.7659685 1 1
N3C N 0 1.192161 1.605065 0.8650143 1 1
C2C C 0 1.203382 1.443229 0.8026898 1 1
C3C C 0 1.251949 1.372037 0.7958423 1 1
H3C H 0 1.212862 1.29855 0.7486172 1 1
C4C C 0 1.360679 1.414416 0.8613849 1 1
H4C H 0 1.395998 1.36854 0.858026 1 1
C5C C 0 1.420866 1.526346 0.9346061 1 1
H5C H 0 1.494673 1.552201 0.9777376 1 1
C6C C 0 1.26302 1.554381 0.8752872 1 1
C7C C 0 1.372454 1.596857 0.9427966 1 1
H7C H 0 1.411242 1.670063 0.9916041 1 1
Cd2A C 0 1.25474 0.88704 0.87326 1 1
N2A N 0 1.261307 0.8454131 0.9295314 1 1
C8A C 0 1.245525 0.8391481 0.8307616 1 1
H8A H 0 1.234127 0.7764166 0.7749466 1 1
N4A N 0 1.247055 0.9289854 0.8165247 1 1
C9A C 0 1.267697 1.00329 0.9182413 1 1
C10A C 0 1.276169 1.108967 0.9521004 1 1
H10A H 0 1.26789 1.142051 0.9047548 1 1
C11A C 0 1.278106 0.9520217 0.9889424 1 1
C12A C 0 1.297431 1.005417 1.095249 1 1
H12A H 0 1.303679 0.9717627 1.142012 1 1
C13A C 0 1.297075 1.162409 1.058165 1 1
H13A H 0 1.304668 1.234085 1.084285 1 1
C14A C 0 1.307599 1.110659 1.129288 1 1
H14A H 0 1.32151 1.149191 1.200904 1 1
Cd2B C 0 0.87101 0.87694 1.27124 1 1
N2B N 0 0.8267012 0.930428 1.284916 1 1
C8B C 0 0.8208909 0.8309688 1.237999 1 1
H8B H 0 0.754988 0.7702635 1.194831 1 1
N4B N 0 0.9160482 0.82353 1.256771 1 1
C9B C 0 0.9932468 0.9303582 1.325159 1 1
C10B C 0 1.105232 0.9729503 1.369566 1 1
H10B H 0 1.141441 0.9291084 1.355822 1 1
C11B C 0 0.9378926 0.9966044 1.343971 1 1
C12B C 0 0.9933598 1.107012 1.407838 1 1
H12B H 0 0.9572551 1.151165 1.419944 1 1
C13B C 0 1.160157 1.082327 1.434359 1 1
H13B H 0 1.235591 1.113715 1.466777 1 1
C14B C 0 1.104265 1.148926 1.453273 1 1
H14B H 0 1.144053 1.223115 1.497516 1 1
Cd2C C 0 0.90114 1.24981 0.88794 1 1
N2C N 0 0.9541627 1.265792 0.8451273 1 1
C8C C 0 0.8550777 1.219583 0.8372032 1 1
H8C H 0 0.794273 1.180403 0.7705255 1 1
N4C N 0 0.8481695 1.232956 0.9314123 1 1
C9C C 0 0.9550116 1.296591 1.01039 1 1
C10C C 0 0.9979838 1.334406 1.122297 1 1
H10C H 0 0.9544491 1.318685 1.157116 1 1
C11C C 0 1.020737 1.318361 0.9570233 1 1
C12C C 0 1.130998 1.378661 1.014455 1 1
H12C H 0 1.17479 1.392669 0.9796282 1 1
C13C C 0 1.10726 1.395724 1.179269 1 1
H13C H 0 1.13893 1.423737 1.254791 1 1
C14C C 0 1.173335 1.417626 1.125381 1 1
H14C H 0 1.247461 1.459356 1.166517 1 1
Zn1 Zn 0 1.23844 0.73234 0.98644 1 1
Zn2 Zn 0 0.70761 0.98928 1.27112 1 1
Zn3 Zn 0 0.99736 1.27892 0.72652 1 1
Zn1a Zn 0 1.23844 1.73234 0.98644 0 1
Zn2a Zn 0 1.70761 0.98928 1.27112 0 1
Zn3a Zn 0 0.99736 1.27892 1.72652 0 1
Zn1b Zn 0 0.76156 1.26766 1.01356 0 1
Zn2b Zn 0 1.29239 1.01072 0.72888 0 1
Zn3b Zn 0 1.00264 0.72108 1.27348 0 1
Cd1Aa C 0 0.47675 0.81904 1.15655 0 1
Cd1Ba C 0 0.79866 1.16352 0.4999 0 1
Cd1Ca C 0 1.14354 0.51512 0.80672 0 1
Cd2Aa C 0 0.74526 1.11296 1.12674 0 1
Cd2Ba C 0 1.12899 1.12306 0.72876 0 1
Cd2Ca C 0 1.09886 0.75019 1.11206 0 1
s1N1 N 0 -0.4940738 -0.1409072 -1.211444 1 1
s1C1 C 0 -0.4585273 -0.1618266 -1.286755 1 1
s1C2 C 0 -0.4236234 -0.1035703 -1.096671 1 1
s1C3 C 0 -0.6058143 -0.1546595 -1.238485 1 1
s1O1 O 0 -0.3639532 -0.1504682 -1.268637 1 1
s1H1 H 0 -0.5086786 -0.1873486 -1.360086 1 1
s1H2 H 0 -0.4605285 -0.1471865 -1.066604 1 1
s1H3 H 0 -0.4067166 -0.02674364 -1.056716 1 1
s1H4 H 0 -0.3562855 -0.1117631 -1.089684 1 1
s1H5 H 0 -0.6062482 -0.085497 -1.198177 1 1
s1H6 H 0 -0.6415913 -0.2104771 -1.218686 1 1
s1H7 H 0 -0.6445698 -0.1773577 -1.316672 1 1
####################################################################### 
# 
# 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_ZIF-9/9kbar
_database_code_depnum_ccdc_archive 'CCDC 1036076'
_audit_update_record             
;
2014-11-25 deposited with the CCDC.
2015-01-23 downloaded from the CCDC.
;
_audit_creation_date             2014-08-19
_audit_creation_method           CRYSTALS_ver_14.43

_oxford_structure_analysis_title 'cobe01 in R-3'
_chemical_name_systematic        ?
_chemical_melting_point          ?

#end of refcif 
_cell_length_a                   22.4424(18)
_cell_length_b                   22.4424(18)
_cell_length_c                   15.8063(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6894.4(11)

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 '
_symmetry_space_group_name_Hall  '-R 3'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/3,y+2/3,z+2/3
-x+1/3,-y+2/3,-z+2/3
x+2/3,y+1/3,z+1/3
-x+2/3,-y+1/3,-z+1/3
-y,x-y,z
y,-x+y,-z
-y+1/3,x-y+2/3,z+2/3
y+1/3,-x+y+2/3,-z+2/3
-y+2/3,x-y+1/3,z+1/3
y+2/3,-x+y+1/3,-z+1/3
-x+y,-x,z
x-y,x,-z
-x+y+1/3,-x+2/3,z+2/3
x-y+1/3,x+2/3,-z+2/3
-x+y+2/3,-x+1/3,z+1/3
x-y+2/3,x+1/3,-z+1/3

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'
Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692
1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            18

# Given Formula = C13.50 H6 Co0.50 N4 O1.50 
# Dc =      1.20 Fooo =   2682.00 Mu =      5.98 M =    277.69
# Found Formula = C14 H10 Co1 N4 
# Dc =      1.27 FOOO =   2682.00 Mu =     11.11 M =    293.19

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 0.000 0.000 0.000 120 39 ' '
2 0.000 0.500 0.000 120 43 ' '
3 0.333 0.667 0.167 90 29 ' '
4 0.500 0.500 0.000 120 44 ' '
5 0.500 0.000 0.000 120 43 ' '
6 0.667 0.333 -0.167 90 29 ' '
7 0.667 0.333 0.333 119 38 ' '
8 0.167 0.333 0.333 120 43 ' '
9 0.167 0.833 0.333 120 43 ' '
10 0.667 0.833 0.333 120 43 ' '
11 0.000 0.000 0.500 89 29 ' '
12 0.333 0.667 0.667 119 38 ' '
13 0.333 0.167 0.667 120 43 ' '
14 0.833 0.667 0.667 120 43 ' '
15 0.833 0.167 0.667 120 43 ' '
_platon_squeeze_details          
;
;

_chemical_formula_sum            'C14 H10 Co1 N4'
_chemical_formula_moiety         'C14 H10 Co1 N4'
_chemical_compound_source        ?
_chemical_formula_weight         293.19


_cell_measurement_reflns_used    1859
_cell_measurement_theta_min      2
_cell_measurement_theta_max      12
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2682
_exptl_absorpt_coefficient_mu    1.111

# Sheldrick geometric approximatio 0.80 0.89 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_T_max  0.89
_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    'USER DEFINED STRUCTURE SOLUTION'
_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_reflns_number            8734
_reflns_number_total             762
_diffrn_reflns_av_R_equivalents  0.103
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 762 
# Theoretical number of reflections is about 1866 


_diffrn_reflns_theta_min         1.661
_diffrn_reflns_theta_max         17.255
_diffrn_measured_fraction_theta_max 0.815

_diffrn_reflns_theta_full        12.941
_diffrn_measured_fraction_theta_full 0.892


_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       12
_reflns_limit_h_min              -18
_reflns_limit_h_max              9
_reflns_limit_k_min              0
_reflns_limit_k_max              18
_reflns_limit_l_min              0
_reflns_limit_l_max              12

_oxford_diffrn_Wilson_B_factor   4.63
_oxford_diffrn_Wilson_scale      282.11

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

_refine_diff_density_min         -0.21
_refine_diff_density_max         0.29


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


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_refine_ls_number_reflns         477
_refine_ls_number_restraints     230
_refine_ls_number_parameters     172
_oxford_refine_ls_R_factor_ref   0.0474
_refine_ls_wR_factor_ref         0.0576
_refine_ls_goodness_of_fit_ref   1.3552
_refine_ls_shift/su_max          0.0001435
_refine_ls_shift/su_mean         0.0000177


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        749
_refine_ls_R_factor_all          0.0850
_refine_ls_wR_factor_all         0.0764

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                477
_refine_ls_R_factor_gt           0.0474
_refine_ls_wR_factor_gt          0.0576

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


_refine_ls_structure_factor_coef F
_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, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.504 0.233 0.254 
;

# 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
Co1 Co 0.40124(9) 0.06123(9) 0.32262(10) 0.0689 1.0000 Uani . . . . . .
C1 C 0.3392(4) 0.0284(4) 0.1542(5) 0.0704 1.0000 Uani D U . . . .
C2 C 0.3622(3) -0.0493(4) 0.1831(4) 0.0630 1.0000 Uani D U . . . .
C3 C 0.3816(4) -0.0927(4) 0.2187(5) 0.0776 1.0000 Uani D U . . . .
C4 C 0.3700(4) -0.1474(4) 0.1721(6) 0.0916 1.0000 Uani D U . . . .
C5 C 0.3896(4) 0.1891(4) 0.3352(4) 0.0634 1.0000 Uani D U . . . .
C6 C 0.4525(4) 0.1966(4) 0.2310(4) 0.0720 1.0000 Uani D U . . . .
C7 C 0.4897(4) 0.1869(5) 0.1694(5) 0.0854 1.0000 Uani D U . . . .
C8 C 0.5263(4) 0.2421(5) 0.1140(5) 0.1050 1.0000 Uani D U . . . .
C9 C 0.4515(3) 0.2571(4) 0.2379(4) 0.0694 1.0000 Uani D U . . . .
C10 C 0.4883(4) 0.3105(4) 0.1830(5) 0.0894 1.0000 Uani D U . . . .
C11 C 0.5255(4) 0.3014(5) 0.1211(5) 0.1030 1.0000 Uani D U . . . .
C12 C 0.3318(3) -0.0618(3) 0.1039(4) 0.0668 1.0000 Uani D U . . . .
C13 C 0.3203(4) -0.1179(4) 0.0562(5) 0.0788 1.0000 Uani D U . . . .
C14 C 0.3406(4) -0.1602(4) 0.0921(6) 0.0943 1.0000 Uani D U . . . .
N1 N 0.3666(3) 0.0093(4) 0.2154(4) 0.0673 1.0000 Uani D U . . . .
N2 N 0.4115(4) 0.1535(3) 0.2952(5) 0.0711 1.0000 Uani D U . . . .
N3 N 0.4100(3) 0.2513(4) 0.3060(4) 0.0642 1.0000 Uani D U . . . .
N4 N 0.3177(3) -0.0106(4) 0.0861(5) 0.0707 1.0000 Uani D U . . . .
H11 H 0.3353 0.0676 0.1592 0.0843 1.0000 Uiso R . . . . .
H31 H 0.4015 -0.0847 0.2721 0.0931 1.0000 Uiso R . . . . .
H41 H 0.3823 -0.1782 0.1943 0.1104 1.0000 Uiso R . . . . .
H51 H 0.3609 0.1717 0.3821 0.0761 1.0000 Uiso R . . . . .
H71 H 0.4906 0.1460 0.1646 0.1023 1.0000 Uiso R . . . . .
H81 H 0.5520 0.2376 0.0709 0.1260 1.0000 Uiso R . . . . .
H101 H 0.4879 0.3516 0.1877 0.1072 1.0000 Uiso R . . . . .
H111 H 0.5508 0.3369 0.0832 0.1235 1.0000 Uiso R . . . . .
H131 H 0.3000 -0.1264 0.0030 0.0946 1.0000 Uiso R . . . . .
H141 H 0.3346 -0.1985 0.0622 0.1136 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.0527(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
Co1 . N4 17_555 1.985(7) yes
Co1 . N3 16_545 1.982(7) yes
Co1 . N1 . 1.982(7) yes
Co1 . N2 . 2.013(7) yes
C1 . N1 . 1.328(7) yes
C1 . N4 . 1.317(7) yes
C1 . H11 . 0.930 no
C2 . C3 . 1.370(7) yes
C2 . C12 . 1.385(6) yes
C2 . N1 . 1.367(6) yes
C3 . C4 . 1.342(7) yes
C3 . H31 . 0.930 no
C4 . C14 . 1.388(7) yes
C4 . H41 . 0.930 no
C5 . N2 . 1.294(6) yes
C5 . N3 . 1.316(6) yes
C5 . H51 . 0.930 no
C6 . C7 . 1.370(7) yes
C6 . C9 . 1.373(6) yes
C6 . N2 . 1.385(6) yes
C7 . C8 . 1.399(7) yes
C7 . H71 . 0.930 no
C8 . C11 . 1.344(7) yes
C8 . H81 . 0.930 no
C9 . C10 . 1.372(7) yes
C9 . N3 . 1.386(6) yes
C10 . C11 . 1.366(7) yes
C10 . H101 . 0.930 no
C11 . H111 . 0.930 no
C12 . C13 . 1.375(7) yes
C12 . N4 . 1.365(6) yes
C13 . C14 . 1.366(7) yes
C13 . H131 . 0.930 no
C14 . H141 . 0.930 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N4 17_555 Co1 . N3 16_545 105.1(3) yes
N4 17_555 Co1 . N1 . 112.8(3) yes
N3 16_545 Co1 . N1 . 115.4(3) yes
N4 17_555 Co1 . N2 . 112.5(3) yes
N3 16_545 Co1 . N2 . 107.9(3) yes
N1 . Co1 . N2 . 103.3(3) yes
N1 . C1 . N4 . 117.1(5) yes
N1 . C1 . H11 . 121.4 no
N4 . C1 . H11 . 121.5 no
C3 . C2 . C12 . 121.7(4) yes
C3 . C2 . N1 . 129.3(5) yes
C12 . C2 . N1 . 109.0(4) yes
C2 . C3 . C4 . 116.2(5) yes
C2 . C3 . H31 . 121.9 no
C4 . C3 . H31 . 121.9 no
C3 . C4 . C14 . 122.8(5) yes
C3 . C4 . H41 . 118.6 no
C14 . C4 . H41 . 118.6 no
N2 . C5 . N3 . 116.5(5) yes
N2 . C5 . H51 . 121.7 no
N3 . C5 . H51 . 121.8 no
C7 . C6 . C9 . 121.8(4) yes
C7 . C6 . N2 . 130.8(5) yes
C9 . C6 . N2 . 107.4(4) yes
C6 . C7 . C8 . 116.0(5) yes
C6 . C7 . H71 . 122.0 no
C8 . C7 . H71 . 122.0 no
C7 . C8 . C11 . 122.1(5) yes
C7 . C8 . H81 . 119.0 no
C11 . C8 . H81 . 118.9 no
C6 . C9 . C10 . 120.9(4) yes
C6 . C9 . N3 . 108.1(4) yes
C10 . C9 . N3 . 131.0(5) yes
C9 . C10 . C11 . 117.9(5) yes
C9 . C10 . H101 . 121.0 no
C11 . C10 . H101 . 121.1 no
C10 . C11 . C8 . 121.3(5) yes
C10 . C11 . H111 . 119.3 no
C8 . C11 . H111 . 119.4 no
C2 . C12 . C13 . 122.0(4) yes
C2 . C12 . N4 . 108.2(4) yes
C13 . C12 . N4 . 129.8(5) yes
C12 . C13 . C14 . 115.6(5) yes
C12 . C13 . H131 . 122.2 no
C14 . C13 . H131 . 122.2 no
C4 . C14 . C13 . 121.7(5) yes
C4 . C14 . H141 . 119.2 no
C13 . C14 . H141 . 119.2 no
C2 . N1 . Co1 . 134.8(5) yes
C2 . N1 . C1 . 102.4(5) yes
Co1 . N1 . C1 . 122.8(5) yes
C6 . N2 . Co1 . 124.8(5) yes
C6 . N2 . C5 . 104.5(5) yes
Co1 . N2 . C5 . 130.3(5) yes
C9 . N3 . Co1 10_555 123.5(5) yes
C9 . N3 . C5 . 103.5(5) yes
Co1 10_555 N3 . C5 . 133.0(5) yes
C12 . N4 . Co1 9_544 133.0(5) yes
C12 . N4 . C1 . 103.3(5) yes
Co1 9_544 N4 . C1 . 123.6(5) yes


_iucr_refine_instructions_details_constraints 
;
#
# Punched on 19/08/14 at 14:19:12
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (   1,X'S) H   (  11,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
END                                                                             
;


_iucr_refine_instructions_details_restraints 
;
#
# Punched on 19/08/14 at 14:19:12
#
#LIST     16                                                                    
DIST   1.331,.01= C(1) TO N(1) 
DIST   1.311,.01= C(1) TO N(4) 
DIST   1.360,.01= C(2) TO C(3) 
DIST   1.385,.01= C(2) TO C(12) 
DIST   1.353,.01= C(2) TO N(1) 
DIST   1.328,.01= C(3) TO C(4) 
DIST   1.382,.01= C(4) TO C(14) 
DIST   1.294,.01= C(5) TO N(2) 
DIST   1.306,.01= C(5) TO N(3) 
DIST   1.368,.01= C(6) TO C(7) 
DIST   1.367,.01= C(6) TO C(9) 
DIST   1.382,.01= C(6) TO N(2) 
DIST   1.391,.01= C(7) TO C(8) 
DIST   1.335,.01= C(8) TO C(11) 
DIST   1.374,.01= C(9) TO C(10) 
DIST   1.383,.01= C(9) TO N(3) 
DIST   1.362,.01= C(10) TO C(11) 
DIST   1.373,.01= C(12) TO C(13) 
DIST   1.355,.01= C(12) TO N(4) 
DIST   1.360,.01= C(13) TO C(14) 
ANGL 117,1= N(4) TO C(1) TO N(1) 
ANGL 122,1= C(12) TO C(2) TO C(3) 
ANGL 129,1= N(1) TO C(2) TO C(3) 
ANGL 109,1= N(1) TO C(2) TO C(12) 
ANGL 116,1= C(4) TO C(3) TO C(2) 
ANGL 123,1= C(14) TO C(4) TO C(3) 
ANGL 116,1= N(3) TO C(5) TO N(2) 
ANGL 122,1= C(9) TO C(6) TO C(7) 
ANGL 131,1= N(2) TO C(6) TO C(7) 
ANGL 107,1= N(2) TO C(6) TO C(9) 
ANGL 116,1= C(8) TO C(7) TO C(6) 
ANGL 122,1= C(11) TO C(8) TO C(7) 
ANGL 121,1= C(10) TO C(9) TO C(6) 
ANGL 108,1= N(3) TO C(9) TO C(6) 
ANGL 131,1= N(3) TO C(9) TO C(10) 
ANGL 118,1= C(11) TO C(10) TO C(9) 
ANGL 121,1= C(10) TO C(11) TO C(8) 
ANGL 122,1= C(13) TO C(12) TO C(2) 
ANGL 108,1= N(4) TO C(12) TO C(2) 
ANGL 129,1= N(4) TO C(12) TO C(13) 
ANGL 115,1= C(14) TO C(13) TO C(12) 
ANGL 122,1= C(13) TO C(14) TO C(4) 
ANGL 102,1= C(2) TO N(1) TO C(1) 
ANGL 105,1= C(6) TO N(2) TO C(5) 
ANGL 104,1= C(9) TO N(3) TO C(5) 
ANGL 103,1= C(12) TO N(4) TO C(1) 
PLANAR 0.010000  C(1) C(2) C(3) C(4) C(12) C(13) C(14) N(1) N(4) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = C(1) TO N(1) 
VIBR .0, 0.00200 = C(1) TO N(4) 
VIBR .0, 0.00500 = N(4) TO N(1) 
VIBR .0, 0.00200 = C(2) TO C(3) 
VIBR .0, 0.00200 = C(2) TO C(12) 
VIBR .0, 0.00200 = C(2) TO N(1) 
VIBR .0, 0.00500 = C(12) TO C(3) 
VIBR .0, 0.00500 = N(1) TO C(3) 
VIBR .0, 0.00500 = N(1) TO C(12) 
VIBR .0, 0.00200 = C(3) TO C(4) 
VIBR .0, 0.00500 = C(4) TO C(2) 
VIBR .0, 0.00200 = C(4) TO C(14) 
VIBR .0, 0.00500 = C(14) TO C(3) 
VIBR .0, 0.00200 = C(5) TO N(2) 
VIBR .0, 0.00200 = C(5) TO N(3) 
VIBR .0, 0.00500 = N(3) TO N(2) 
VIBR .0, 0.00200 = C(6) TO C(7) 
VIBR .0, 0.00200 = C(6) TO C(9) 
VIBR .0, 0.00200 = C(6) TO N(2) 
VIBR .0, 0.00500 = C(9) TO C(7) 
VIBR .0, 0.00500 = N(2) TO C(7) 
VIBR .0, 0.00500 = N(2) TO C(9) 
VIBR .0, 0.00200 = C(7) TO C(8) 
VIBR .0, 0.00500 = C(8) TO C(6) 
VIBR .0, 0.00200 = C(8) TO C(11) 
VIBR .0, 0.00500 = C(11) TO C(7) 
VIBR .0, 0.00200 = C(9) TO C(10) 
VIBR .0, 0.00200 = C(9) TO N(3) 
VIBR .0, 0.00500 = C(10) TO C(6) 
VIBR .0, 0.00500 = N(3) TO C(6) 
VIBR .0, 0.00500 = N(3) TO C(10) 
VIBR .0, 0.00200 = C(10) TO C(11) 
VIBR .0, 0.00500 = C(11) TO C(9) 
VIBR .0, 0.00500 = C(8) TO C(10) 
VIBR .0, 0.00200 = C(12) TO C(13) 
VIBR .0, 0.00200 = C(12) TO N(4) 
VIBR .0, 0.00500 = C(13) TO C(2) 
VIBR .0, 0.00500 = N(4) TO C(2) 
VIBR .0, 0.00500 = N(4) TO C(13) 
VIBR .0, 0.00200 = C(13) TO C(14) 
VIBR .0, 0.00500 = C(14) TO C(12) 
VIBR .0, 0.00500 = C(13) TO C(4) 
VIBR .0, 0.00500 = C(1) TO C(2) 
VIBR .0, 0.00500 = C(5) TO C(6) 
VIBR .0, 0.00500 = C(5) TO C(9) 
VIBR .0, 0.00500 = C(1) TO C(12) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = C(1) TO N(1) 
U(IJ) .0, 0.04000 = C(1) TO N(4) 
U(IJ) .0, 0.04000 = C(2) TO C(3) 
U(IJ) .0, 0.04000 = C(2) TO C(12) 
U(IJ) .0, 0.04000 = C(2) TO N(1) 
U(IJ) .0, 0.04000 = C(3) TO C(4) 
U(IJ) .0, 0.04000 = C(4) TO C(14) 
U(IJ) .0, 0.04000 = C(5) TO N(2) 
U(IJ) .0, 0.04000 = C(5) TO N(3) 
U(IJ) .0, 0.04000 = C(6) TO C(7) 
U(IJ) .0, 0.04000 = C(6) TO C(9) 
U(IJ) .0, 0.04000 = C(6) TO N(2) 
U(IJ) .0, 0.04000 = C(7) TO C(8) 
U(IJ) .0, 0.04000 = C(8) TO C(11) 
U(IJ) .0, 0.04000 = C(9) TO C(10) 
U(IJ) .0, 0.04000 = C(9) TO N(3) 
U(IJ) .0, 0.04000 = C(10) TO C(11) 
U(IJ) .0, 0.04000 = C(12) TO C(13) 
U(IJ) .0, 0.04000 = C(12) TO N(4) 
U(IJ) .0, 0.04000 = C(13) TO C(14) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
PLANAR 0.010000  C(5) C(6) C(7) C(8) C(9) C(10) C(11) N(2) N(3) 
END                                                                             
;

# 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
-11 11 2 x .
-11 11 5 x .
-2 2 2 x .
0 2 1 x .
-2 4 0 x .
####################################################################### 
# 
# 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_ZIF-9/18kbar
_database_code_depnum_ccdc_archive 'CCDC 1036077'
_audit_update_record             
;
2014-11-25 deposited with the CCDC.
2015-01-23 downloaded from the CCDC.
;
_audit_creation_date             2014-08-19
_audit_creation_method           CRYSTALS_ver_14.43

_oxford_structure_analysis_title 'cobe02 in R-3'
_chemical_name_systematic        ?
_chemical_melting_point          ?

#end of refcif 
_cell_length_a                   21.926(3)
_cell_length_b                   21.926(3)
_cell_length_c                   15.704(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6538(2)

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 '
_symmetry_space_group_name_Hall  '-R 3'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/3,y+2/3,z+2/3
-x+1/3,-y+2/3,-z+2/3
x+2/3,y+1/3,z+1/3
-x+2/3,-y+1/3,-z+1/3
-y,x-y,z
y,-x+y,-z
-y+1/3,x-y+2/3,z+2/3
y+1/3,-x+y+2/3,-z+2/3
-y+2/3,x-y+1/3,z+1/3
y+2/3,-x+y+1/3,-z+1/3
-x+y,-x,z
x-y,x,-z
-x+y+1/3,-x+2/3,z+2/3
x-y+1/3,x+2/3,-z+2/3
-x+y+2/3,-x+1/3,z+1/3
x-y+2/3,x+1/3,-z+1/3

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'
Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692
1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            18

# Given Formula = C13.33 H26.67 Co0.67 N5.33 O2 
# Dc =      1.52 Fooo =   2682.00 Mu =      8.29 M =    333.02
# Found Formula = C14 H10 Co1 N4 
# Dc =      1.34 FOOO =   2682.00 Mu =     11.72 M =    293.19

_chemical_formula_sum            'C14 H10 Co1 N4'
_chemical_formula_moiety         'C14 H10 Co1 N4'
_chemical_compound_source        ?
_chemical_formula_weight         293.19


_cell_measurement_reflns_used    1082
_cell_measurement_theta_min      2
_cell_measurement_theta_max      12
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2682
_exptl_absorpt_coefficient_mu    1.172

# Sheldrick geometric approximatio 0.79 0.89 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_T_max  0.89
_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    'USER DEFINED STRUCTURE SOLUTION'
_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_reflns_number            7412
_reflns_number_total             705
_diffrn_reflns_av_R_equivalents  0.176
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 705 
# Theoretical number of reflections is about 1755 


_diffrn_reflns_theta_min         1.683
_diffrn_reflns_theta_max         17.232
_diffrn_measured_fraction_theta_max 0.782

_diffrn_reflns_theta_full        12.924
_diffrn_measured_fraction_theta_full 0.879


_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       12
_reflns_limit_h_min              -18
_reflns_limit_h_max              8
_reflns_limit_k_min              0
_reflns_limit_k_max              18
_reflns_limit_l_min              0
_reflns_limit_l_max              12

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

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

_refine_diff_density_min         -0.32
_refine_diff_density_max         0.42


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


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_refine_ls_number_reflns         303
_refine_ls_number_restraints     230
_refine_ls_number_parameters     172
_oxford_refine_ls_R_factor_ref   0.0765
_refine_ls_wR_factor_ref         0.0760
_refine_ls_goodness_of_fit_ref   1.6578
_refine_ls_shift/su_max          0.0006168
_refine_ls_shift/su_mean         0.0001038


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        679
_refine_ls_R_factor_all          0.1497
_refine_ls_wR_factor_all         0.0952

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                303
_refine_ls_R_factor_gt           0.0765
_refine_ls_wR_factor_gt          0.0760

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


_refine_ls_structure_factor_coef F
_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, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 1.60 0.312 1.32 
;

# 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
Co1 Co 0.39962(17) 0.05811(16) 0.3218(2) 0.1034 1.0000 Uani . . . . . .
C1 C 0.3408(5) 0.0274(5) 0.1521(9) 0.1129 1.0000 Uani D U . . . .
C2 C 0.3639(4) -0.0524(5) 0.1790(6) 0.1134 1.0000 Uani D U . . . .
C3 C 0.3845(4) -0.0964(7) 0.2126(8) 0.1220 1.0000 Uani D U . . . .
C4 C 0.3724(5) -0.1514(6) 0.1647(10) 0.1344 1.0000 Uani D U . . . .
C5 C 0.3838(4) 0.1840(7) 0.3357(6) 0.1026 1.0000 Uani D U . . . .
C6 C 0.4491(4) 0.1918(5) 0.2314(6) 0.1175 1.0000 Uani D U . . . .
C7 C 0.4870(5) 0.1818(7) 0.1693(7) 0.1346 1.0000 Uani D U . . . .
C8 C 0.5250(5) 0.2383(9) 0.1145(6) 0.1385 1.0000 Uani D U . . . .
C9 C 0.4487(4) 0.2537(5) 0.2390(6) 0.1085 1.0000 Uani D U . . . .
C10 C 0.4869(5) 0.3084(5) 0.1841(7) 0.1246 1.0000 Uani D U . . . .
C11 C 0.5247(5) 0.2990(8) 0.1217(7) 0.1328 1.0000 Uani D U . . . .
C12 C 0.3325(4) -0.0642(5) 0.0998(6) 0.1223 1.0000 Uani D U . . . .
C13 C 0.3201(4) -0.1209(6) 0.0505(7) 0.1218 1.0000 Uani D U . . . .
C14 C 0.3410(5) -0.1643(5) 0.0854(10) 0.1290 1.0000 Uani D U . . . .
N1 N 0.3694(4) 0.0072(5) 0.2125(7) 0.1089 1.0000 Uani D U . . . .
N2 N 0.4065(5) 0.1478(5) 0.2953(7) 0.1115 1.0000 Uani D U . . . .
N3 N 0.4060(5) 0.2478(7) 0.3073(7) 0.1078 1.0000 Uani D U . . . .
N4 N 0.3178(4) -0.0120(6) 0.0838(7) 0.1203 1.0000 Uani D U . . . .
H11 H 0.3358 0.0660 0.1558 0.1095 1.0000 Uiso R . . . . .
H31 H 0.4035 -0.0897 0.2663 0.1096 1.0000 Uiso R . . . . .
H41 H 0.3853 -0.1835 0.1864 0.1098 1.0000 Uiso R . . . . .
H51 H 0.3562 0.1670 0.3846 0.1279 1.0000 Uiso R . . . . .
H71 H 0.4886 0.1421 0.1636 0.1282 1.0000 Uiso R . . . . .
H81 H 0.5512 0.2364 0.0707 0.1282 1.0000 Uiso R . . . . .
H101 H 0.4866 0.3522 0.1913 0.1282 1.0000 Uiso R . . . . .
H111 H 0.5498 0.3375 0.0842 0.1283 1.0000 Uiso R . . . . .
H131 H 0.3013 -0.1299 -0.0052 0.1096 1.0000 Uiso R . . . . .
H141 H 0.3358 -0.2042 0.0545 0.1097 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.0624(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
Co1 . N3 16_545 1.968(11) yes
Co1 . N4 17_555 1.928(11) yes
Co1 . N1 . 1.973(10) yes
Co1 . N2 . 1.940(11) yes
C1 . N1 . 1.330(6) yes
C1 . N4 . 1.310(6) yes
C1 . H11 . 0.908 no
C2 . C3 . 1.361(6) yes
C2 . C12 . 1.382(6) yes
C2 . N1 . 1.355(6) yes
C3 . C4 . 1.331(6) yes
C3 . H31 . 0.919 no
C4 . C14 . 1.383(6) yes
C4 . H41 . 0.943 no
C5 . N2 . 1.294(6) yes
C5 . N3 . 1.309(6) yes
C5 . H51 . 0.933 no
C6 . C7 . 1.368(6) yes
C6 . C9 . 1.367(6) yes
C6 . N2 . 1.382(6) yes
C7 . C8 . 1.392(6) yes
C7 . H71 . 0.894 no
C8 . C11 . 1.338(6) yes
C8 . H81 . 0.911 no
C9 . C10 . 1.370(6) yes
C9 . N3 . 1.386(6) yes
C10 . C11 . 1.366(6) yes
C10 . H101 . 0.968 no
C11 . H111 . 0.948 no
C12 . C13 . 1.373(6) yes
C12 . N4 . 1.358(6) yes
C13 . C14 . 1.360(6) yes
C13 . H131 . 0.945 no
C14 . H141 . 0.956 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
N3 16_545 Co1 . N4 17_555 105.7(5) yes
N3 16_545 Co1 . N1 . 112.3(5) yes
N4 17_555 Co1 . N1 . 116.4(4) yes
N3 16_545 Co1 . N2 . 110.2(4) yes
N4 17_555 Co1 . N2 . 109.4(5) yes
N1 . Co1 . N2 . 102.8(5) yes
N1 . C1 . N4 . 117.0(4) yes
N1 . C1 . H11 . 124.2 no
N4 . C1 . H11 . 118.8 no
C3 . C2 . C12 . 121.8(4) yes
C3 . C2 . N1 . 129.1(4) yes
C12 . C2 . N1 . 109.1(4) yes
C2 . C3 . C4 . 116.0(4) yes
C2 . C3 . H31 . 121.8 no
C4 . C3 . H31 . 122.2 no
C3 . C4 . C14 . 123.1(5) yes
C3 . C4 . H41 . 118.3 no
C14 . C4 . H41 . 118.6 no
N2 . C5 . N3 . 115.9(4) yes
N2 . C5 . H51 . 122.1 no
N3 . C5 . H51 . 121.9 no
C7 . C6 . C9 . 121.8(4) yes
C7 . C6 . N2 . 131.1(4) yes
C9 . C6 . N2 . 107.1(4) yes
C6 . C7 . C8 . 116.1(4) yes
C6 . C7 . H71 . 123.4 no
C8 . C7 . H71 . 120.5 no
C7 . C8 . C11 . 122.3(5) yes
C7 . C8 . H81 . 122.4 no
C11 . C8 . H81 . 115.3 no
C6 . C9 . C10 . 120.7(4) yes
C6 . C9 . N3 . 108.2(4) yes
C10 . C9 . N3 . 131.1(4) yes
C9 . C10 . C11 . 118.0(4) yes
C9 . C10 . H101 . 119.4 no
C11 . C10 . H101 . 122.6 no
C10 . C11 . C8 . 121.2(5) yes
C10 . C11 . H111 . 115.9 no
C8 . C11 . H111 . 123.0 no
C2 . C12 . C13 . 122.1(4) yes
C2 . C12 . N4 . 108.4(4) yes
C13 . C12 . N4 . 129.5(4) yes
C12 . C13 . C14 . 115.1(4) yes
C12 . C13 . H131 . 125.3 no
C14 . C13 . H131 . 119.5 no
C4 . C14 . C13 . 121.9(5) yes
C4 . C14 . H141 . 117.5 no
C13 . C14 . H141 . 120.5 no
C2 . N1 . C1 . 102.3(4) yes
C2 . N1 . Co1 . 136.6(8) yes
C1 . N1 . Co1 . 120.8(8) yes
C6 . N2 . C5 . 105.1(4) yes
C6 . N2 . Co1 . 123.2(7) yes
C5 . N2 . Co1 . 131.1(8) yes
C9 . N3 . Co1 10_555 122.9(7) yes
C9 . N3 . C5 . 103.8(4) yes
Co1 10_555 N3 . C5 . 133.3(8) yes
C12 . N4 . C1 . 103.2(4) yes
C12 . N4 . Co1 9_544 133.1(8) yes
C1 . N4 . Co1 9_544 123.7(8) yes


_iucr_refine_instructions_details_constraints 
;
#
# Punched on 19/08/14 at 14:50:03
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (   1,X'S) H   (  11,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
END                                                                             
;


_iucr_refine_instructions_details_restraints 
;
#
# Punched on 19/08/14 at 14:50:03
#
#LIST     16                                                                    
DIST   1.331,.01= C(1) TO N(1) 
DIST   1.311,.01= C(1) TO N(4) 
DIST   1.360,.01= C(2) TO C(3) 
DIST   1.385,.01= C(2) TO C(12) 
DIST   1.353,.01= C(2) TO N(1) 
DIST   1.328,.01= C(3) TO C(4) 
DIST   1.382,.01= C(4) TO C(14) 
DIST   1.294,.01= C(5) TO N(2) 
DIST   1.306,.01= C(5) TO N(3) 
DIST   1.368,.01= C(6) TO C(7) 
DIST   1.367,.01= C(6) TO C(9) 
DIST   1.382,.01= C(6) TO N(2) 
DIST   1.391,.01= C(7) TO C(8) 
DIST   1.335,.01= C(8) TO C(11) 
DIST   1.374,.01= C(9) TO C(10) 
DIST   1.383,.01= C(9) TO N(3) 
DIST   1.362,.01= C(10) TO C(11) 
DIST   1.373,.01= C(12) TO C(13) 
DIST   1.355,.01= C(12) TO N(4) 
DIST   1.360,.01= C(13) TO C(14) 
ANGL 117,1= N(4) TO C(1) TO N(1) 
ANGL 122,1= C(12) TO C(2) TO C(3) 
ANGL 129,1= N(1) TO C(2) TO C(3) 
ANGL 109,1= N(1) TO C(2) TO C(12) 
ANGL 116,1= C(4) TO C(3) TO C(2) 
ANGL 123,1= C(14) TO C(4) TO C(3) 
ANGL 116,1= N(3) TO C(5) TO N(2) 
ANGL 122,1= C(9) TO C(6) TO C(7) 
ANGL 131,1= N(2) TO C(6) TO C(7) 
ANGL 107,1= N(2) TO C(6) TO C(9) 
ANGL 116,1= C(8) TO C(7) TO C(6) 
ANGL 122,1= C(11) TO C(8) TO C(7) 
ANGL 121,1= C(10) TO C(9) TO C(6) 
ANGL 108,1= N(3) TO C(9) TO C(6) 
ANGL 131,1= N(3) TO C(9) TO C(10) 
ANGL 118,1= C(11) TO C(10) TO C(9) 
ANGL 121,1= C(10) TO C(11) TO C(8) 
ANGL 122,1= C(13) TO C(12) TO C(2) 
ANGL 108,1= N(4) TO C(12) TO C(2) 
ANGL 129,1= N(4) TO C(12) TO C(13) 
ANGL 115,1= C(14) TO C(13) TO C(12) 
ANGL 122,1= C(13) TO C(14) TO C(4) 
ANGL 102,1= C(2) TO N(1) TO C(1) 
ANGL 105,1= C(6) TO N(2) TO C(5) 
ANGL 104,1= C(9) TO N(3) TO C(5) 
ANGL 103,1= C(12) TO N(4) TO C(1) 
PLANAR 0.010000  C(1) C(2) C(3) C(4) C(12) C(13) C(14) N(1) N(4) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = C(1) TO N(1) 
VIBR .0, 0.00200 = C(1) TO N(4) 
VIBR .0, 0.00500 = N(4) TO N(1) 
VIBR .0, 0.00200 = C(2) TO C(3) 
VIBR .0, 0.00200 = C(2) TO C(12) 
VIBR .0, 0.00200 = C(2) TO N(1) 
VIBR .0, 0.00500 = C(12) TO C(3) 
VIBR .0, 0.00500 = N(1) TO C(3) 
VIBR .0, 0.00500 = N(1) TO C(12) 
VIBR .0, 0.00200 = C(3) TO C(4) 
VIBR .0, 0.00500 = C(4) TO C(2) 
VIBR .0, 0.00200 = C(4) TO C(14) 
VIBR .0, 0.00500 = C(14) TO C(3) 
VIBR .0, 0.00200 = C(5) TO N(2) 
VIBR .0, 0.00200 = C(5) TO N(3) 
VIBR .0, 0.00500 = N(3) TO N(2) 
VIBR .0, 0.00200 = C(6) TO C(7) 
VIBR .0, 0.00200 = C(6) TO C(9) 
VIBR .0, 0.00200 = C(6) TO N(2) 
VIBR .0, 0.00500 = C(9) TO C(7) 
VIBR .0, 0.00500 = N(2) TO C(7) 
VIBR .0, 0.00500 = N(2) TO C(9) 
VIBR .0, 0.00200 = C(7) TO C(8) 
VIBR .0, 0.00500 = C(8) TO C(6) 
VIBR .0, 0.00200 = C(8) TO C(11) 
VIBR .0, 0.00500 = C(11) TO C(7) 
VIBR .0, 0.00200 = C(9) TO C(10) 
VIBR .0, 0.00200 = C(9) TO N(3) 
VIBR .0, 0.00500 = C(10) TO C(6) 
VIBR .0, 0.00500 = N(3) TO C(6) 
VIBR .0, 0.00500 = N(3) TO C(10) 
VIBR .0, 0.00200 = C(10) TO C(11) 
VIBR .0, 0.00500 = C(11) TO C(9) 
VIBR .0, 0.00500 = C(8) TO C(10) 
VIBR .0, 0.00200 = C(12) TO C(13) 
VIBR .0, 0.00200 = C(12) TO N(4) 
VIBR .0, 0.00500 = C(13) TO C(2) 
VIBR .0, 0.00500 = N(4) TO C(2) 
VIBR .0, 0.00500 = N(4) TO C(13) 
VIBR .0, 0.00200 = C(13) TO C(14) 
VIBR .0, 0.00500 = C(14) TO C(12) 
VIBR .0, 0.00500 = C(13) TO C(4) 
VIBR .0, 0.00500 = C(1) TO C(2) 
VIBR .0, 0.00500 = C(5) TO C(6) 
VIBR .0, 0.00500 = C(5) TO C(9) 
VIBR .0, 0.00500 = C(1) TO C(12) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = C(1) TO N(1) 
U(IJ) .0, 0.04000 = C(1) TO N(4) 
U(IJ) .0, 0.04000 = C(2) TO C(3) 
U(IJ) .0, 0.04000 = C(2) TO C(12) 
U(IJ) .0, 0.04000 = C(2) TO N(1) 
U(IJ) .0, 0.04000 = C(3) TO C(4) 
U(IJ) .0, 0.04000 = C(4) TO C(14) 
U(IJ) .0, 0.04000 = C(5) TO N(2) 
U(IJ) .0, 0.04000 = C(5) TO N(3) 
U(IJ) .0, 0.04000 = C(6) TO C(7) 
U(IJ) .0, 0.04000 = C(6) TO C(9) 
U(IJ) .0, 0.04000 = C(6) TO N(2) 
U(IJ) .0, 0.04000 = C(7) TO C(8) 
U(IJ) .0, 0.04000 = C(8) TO C(11) 
U(IJ) .0, 0.04000 = C(9) TO C(10) 
U(IJ) .0, 0.04000 = C(9) TO N(3) 
U(IJ) .0, 0.04000 = C(10) TO C(11) 
U(IJ) .0, 0.04000 = C(12) TO C(13) 
U(IJ) .0, 0.04000 = C(12) TO N(4) 
U(IJ) .0, 0.04000 = C(13) TO C(14) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
PLANAR 0.010000  C(5) C(6) C(7) C(8) C(9) C(10) C(11) N(2) N(3) 
END                                                                             
;

# 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
-2 2 2 x .
0 2 1 x .
-2 4 0 x .
-1 2 0 x .
-1 5 0 x .
####################################################################### 
# 
# 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_ZIF-9/27kbar
_database_code_depnum_ccdc_archive 'CCDC 1036078'
_audit_update_record             
;
2014-11-25 deposited with the CCDC.
2015-01-23 downloaded from the CCDC.
;
_audit_creation_date             2014-08-19
_audit_creation_method           CRYSTALS_ver_14.43

_oxford_structure_analysis_title 'cobe03 in R-3'
_chemical_name_systematic        ?
_chemical_melting_point          ?

#end of refcif 
_cell_length_a                   21.607(3)
_cell_length_b                   21.607(3)
_cell_length_c                   15.608(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6310(2)

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/3,y+2/3,z+2/3
-x+1/3,-y+2/3,-z+2/3
x+2/3,y+1/3,z+1/3
-x+2/3,-y+1/3,-z+1/3
-y,x-y,z
y,-x+y,-z
-y+1/3,x-y+2/3,z+2/3
y+1/3,-x+y+2/3,-z+2/3
-y+2/3,x-y+1/3,z+1/3
y+2/3,-x+y+1/3,-z+1/3
-x+y,-x,z
x-y,x,-z
-x+y+1/3,-x+2/3,z+2/3
x-y+1/3,x+2/3,-z+2/3
-x+y+2/3,-x+1/3,z+1/3
x-y+2/3,x+1/3,-z+1/3

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'
Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692
1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            18

# Given Formula = C10 H20 Co0.50 N4 O1.50 
# Dc =      1.18 Fooo =   2682.00 Mu =      6.45 M =    249.76
# Found Formula = C14 H10 Co1 N4 
# Dc =      1.39 FOOO =   2682.00 Mu =     12.14 M =    293.19

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 0.000 0.000 0.000 111 42 ' '
2 0.000 0.500 0.000 98 41 ' '
3 0.333 0.667 0.167 58 30 ' '
4 0.500 0.500 0.000 98 41 ' '
5 0.500 0.000 0.000 98 41 ' '
6 0.667 0.333 -0.167 58 30 ' '
7 0.667 0.333 0.333 112 42 ' '
8 0.167 0.333 0.333 98 41 ' '
9 0.167 0.833 0.333 98 41 ' '
10 0.667 0.833 0.333 98 41 ' '
11 0.000 0.000 0.500 60 30 ' '
12 0.333 0.667 0.667 111 42 ' '
13 0.333 0.167 0.667 98 41 ' '
14 0.833 0.667 0.667 98 41 ' '
15 0.833 0.167 0.667 98 41 ' '
_platon_squeeze_details          
;
;

_chemical_formula_sum            'C14 H10 Co1 N4'
_chemical_formula_moiety         'C14 H10 Co1 N4'
_chemical_compound_source        ?
_chemical_formula_weight         293.19


_cell_measurement_reflns_used    892
_cell_measurement_theta_min      2
_cell_measurement_theta_max      12
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2682
_exptl_absorpt_coefficient_mu    1.214

# Sheldrick geometric approximatio 0.78 0.89 
_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  0.89
_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    'USER DEFINED STRUCTURE SOLUTION'
_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_reflns_number            7100
_reflns_number_total             700
_diffrn_reflns_av_R_equivalents  0.209
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 700 
# Theoretical number of reflections is about 1315 


_diffrn_reflns_theta_min         1.699
_diffrn_reflns_theta_max         15.776
_diffrn_measured_fraction_theta_max 0.863

_diffrn_reflns_theta_full        14.040
_diffrn_measured_fraction_theta_full 0.885


_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       11
_reflns_limit_h_min              -16
_reflns_limit_h_max              7
_reflns_limit_k_min              0
_reflns_limit_k_max              16
_reflns_limit_l_min              0
_reflns_limit_l_max              11

_oxford_diffrn_Wilson_B_factor   9.43
_oxford_diffrn_Wilson_scale      178.89

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

_refine_diff_density_min         -0.23
_refine_diff_density_max         0.25


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


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_refine_ls_number_reflns         239
_refine_ls_number_restraints     230
_refine_ls_number_parameters     172
_oxford_refine_ls_R_factor_ref   0.0824
_refine_ls_wR_factor_ref         0.0835
_refine_ls_goodness_of_fit_ref   1.9654
_refine_ls_shift/su_max          0.0072763
_refine_ls_shift/su_mean         0.0009054


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        575
_refine_ls_R_factor_all          0.1611
_refine_ls_wR_factor_all         0.1117

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                239
_refine_ls_R_factor_gt           0.0824
_refine_ls_wR_factor_gt          0.0835

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


_refine_ls_structure_factor_coef F
_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, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 1.38 0.248 1.02 
;

# 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
Co1 Co 0.3988(2) 0.0573(2) 0.3249(3) 0.1415 1.0000 Uani . . . . . .
C1 C 0.3385(5) 0.0231(5) 0.1572(11) 0.1342 1.0000 Uani D U . . . .
C2 C 0.3664(3) -0.0550(5) 0.1810(6) 0.1341 1.0000 Uani D U . . . .
C3 C 0.3899(4) -0.0982(7) 0.2129(9) 0.1383 1.0000 Uani D U . . . .
C4 C 0.3804(5) -0.1520(6) 0.1627(13) 0.1513 1.0000 Uani D U . . . .
C5 C 0.3837(5) 0.1869(8) 0.3331(7) 0.1358 1.0000 Uani D U . . . .
C6 C 0.4481(5) 0.1899(6) 0.2287(7) 0.1534 1.0000 Uani D U . . . .
C7 C 0.4848(6) 0.1765(8) 0.1669(8) 0.1622 1.0000 Uani D U . . . .
C8 C 0.5249(5) 0.2323(11) 0.1104(7) 0.1631 1.0000 Uani D U . . . .
C9 C 0.4510(5) 0.2544(5) 0.2344(7) 0.1497 1.0000 Uani D U . . . .
C10 C 0.4912(5) 0.3084(6) 0.1776(8) 0.1626 1.0000 Uani D U . . . .
C11 C 0.5279(5) 0.2955(9) 0.1158(7) 0.1644 1.0000 Uani D U . . . .
C12 C 0.3347(4) -0.0665(6) 0.1012(6) 0.1418 1.0000 Uani D U . . . .
C13 C 0.3249(5) -0.1220(7) 0.0495(8) 0.1507 1.0000 Uani D U . . . .
C14 C 0.3488(6) -0.1645(5) 0.0827(12) 0.1576 1.0000 Uani D U . . . .
N1 N 0.3689(4) 0.0031(6) 0.2171(8) 0.1316 1.0000 Uani D U . . . .
N2 N 0.4040(5) 0.1474(6) 0.2939(8) 0.1437 1.0000 Uani D U . . . .
N3 N 0.4087(5) 0.2514(7) 0.3026(7) 0.1375 1.0000 Uani D U . . . .
N4 N 0.3170(4) -0.0154(7) 0.0872(9) 0.1450 1.0000 Uani D U . . . .
H11 H 0.3330 0.0627 0.1649 0.1606 1.0000 Uiso R . . . . .
H31 H 0.4113 -0.0906 0.2665 0.1657 1.0000 Uiso R . . . . .
H41 H 0.3957 -0.1829 0.1823 0.1814 1.0000 Uiso R . . . . .
H51 H 0.3533 0.1705 0.3802 0.1624 1.0000 Uiso R . . . . .
H71 H 0.4830 0.1327 0.1630 0.1944 1.0000 Uiso R . . . . .
H81 H 0.5505 0.2253 0.0673 0.1958 1.0000 Uiso R . . . . .
H101 H 0.4932 0.3523 0.1812 0.1948 1.0000 Uiso R . . . . .
H111 H 0.5555 0.3312 0.0767 0.1973 1.0000 Uiso R . . . . .
H131 H 0.3034 -0.1300 -0.0041 0.1799 1.0000 Uiso R . . . . .
H141 H 0.3436 -0.2031 0.0506 0.1886 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.0676(8)
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
Co1 . N4 17_555 1.928(12) yes
Co1 . N3 16_545 1.919(11) yes
Co1 . N1 . 1.965(12) yes
Co1 . N2 . 1.955(11) yes
C1 . N1 . 1.331(5) yes
C1 . N4 . 1.311(5) yes
C1 . H11 . 0.930 no
C2 . C3 . 1.360(5) yes
C2 . C12 . 1.383(4) yes
C2 . N1 . 1.353(5) yes
C3 . C4 . 1.330(5) yes
C3 . H31 . 0.930 no
C4 . C14 . 1.384(5) yes
C4 . H41 . 0.930 no
C5 . N2 . 1.292(5) yes
C5 . N3 . 1.308(5) yes
C5 . H51 . 0.930 no
C6 . C7 . 1.368(5) yes
C6 . C9 . 1.366(4) yes
C6 . N2 . 1.382(5) yes
C7 . C8 . 1.392(5) yes
C7 . H71 . 0.930 no
C8 . C11 . 1.338(5) yes
C8 . H81 . 0.930 no
C9 . C10 . 1.373(5) yes
C9 . N3 . 1.384(5) yes
C10 . C11 . 1.364(5) yes
C10 . H101 . 0.930 no
C11 . H111 . 0.930 no
C12 . C13 . 1.372(5) yes
C12 . N4 . 1.355(5) yes
C13 . C14 . 1.360(5) yes
C13 . H131 . 0.930 no
C14 . H141 . 0.930 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N4 17_555 Co1 . N3 16_545 106.4(6) yes
N4 17_555 Co1 . N1 . 116.3(4) yes
N3 16_545 Co1 . N1 . 113.1(6) yes
N4 17_555 Co1 . N2 . 108.5(6) yes
N3 16_545 Co1 . N2 . 109.7(4) yes
N1 . Co1 . N2 . 102.6(6) yes
N1 . C1 . N4 . 117.1(4) yes
N1 . C1 . H11 . 121.3 no
N4 . C1 . H11 . 121.5 no
C3 . C2 . C12 . 121.9(3) yes
C3 . C2 . N1 . 129.0(3) yes
C12 . C2 . N1 . 109.1(3) yes
C2 . C3 . C4 . 115.9(3) yes
C2 . C3 . H31 . 122.1 no
C4 . C3 . H31 . 121.9 no
C3 . C4 . C14 . 123.1(4) yes
C3 . C4 . H41 . 118.6 no
C14 . C4 . H41 . 118.4 no
N2 . C5 . N3 . 115.9(4) yes
N2 . C5 . H51 . 122.1 no
N3 . C5 . H51 . 122.1 no
C7 . C6 . C9 . 121.8(3) yes
C7 . C6 . N2 . 131.1(3) yes
C9 . C6 . N2 . 107.1(3) yes
C6 . C7 . C8 . 116.0(3) yes
C6 . C7 . H71 . 122.0 no
C8 . C7 . H71 . 122.0 no
C7 . C8 . C11 . 122.4(4) yes
C7 . C8 . H81 . 118.8 no
C11 . C8 . H81 . 118.8 no
C6 . C9 . C10 . 120.7(3) yes
C6 . C9 . N3 . 108.1(3) yes
C10 . C9 . N3 . 131.1(3) yes
C9 . C10 . C11 . 117.9(3) yes
C9 . C10 . H101 . 121.0 no
C11 . C10 . H101 . 121.0 no
C10 . C11 . C8 . 121.1(4) yes
C10 . C11 . H111 . 119.4 no
C8 . C11 . H111 . 119.4 no
C2 . C12 . C13 . 122.1(3) yes
C2 . C12 . N4 . 108.4(3) yes
C13 . C12 . N4 . 129.4(3) yes
C12 . C13 . C14 . 114.9(3) yes
C12 . C13 . H131 . 122.4 no
C14 . C13 . H131 . 122.6 no
C4 . C14 . C13 . 122.0(4) yes
C4 . C14 . H141 . 119.1 no
C13 . C14 . H141 . 118.9 no
C2 . N1 . C1 . 102.2(3) yes
C2 . N1 . Co1 . 139.3(9) yes
C1 . N1 . Co1 . 118.4(9) yes
C6 . N2 . Co1 . 121.4(8) yes
C6 . N2 . C5 . 105.0(3) yes
Co1 . N2 . C5 . 132.2(8) yes
C9 . N3 . C5 . 103.9(3) yes
C9 . N3 . Co1 10_555 127.7(8) yes
C5 . N3 . Co1 10_555 128.5(8) yes
C12 . N4 . C1 . 103.1(3) yes
C12 . N4 . Co1 9_544 133.9(10) yes
C1 . N4 . Co1 9_544 122.8(10) yes


_iucr_refine_instructions_details_constraints 
;
#
# Punched on 19/08/14 at 15:26:02
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (   1,X'S) H   (  11,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
END                                                                             
;


_iucr_refine_instructions_details_restraints 
;
#
# Punched on 19/08/14 at 15:26:02
#
#LIST     16                                                                    
DIST   1.331,.01= C(1) TO N(1) 
DIST   1.311,.01= C(1) TO N(4) 
DIST   1.360,.01= C(2) TO C(3) 
DIST   1.385,.01= C(2) TO C(12) 
DIST   1.353,.01= C(2) TO N(1) 
DIST   1.328,.01= C(3) TO C(4) 
DIST   1.382,.01= C(4) TO C(14) 
DIST   1.294,.01= C(5) TO N(2) 
DIST   1.306,.01= C(5) TO N(3) 
DIST   1.368,.01= C(6) TO C(7) 
DIST   1.367,.01= C(6) TO C(9) 
DIST   1.382,.01= C(6) TO N(2) 
DIST   1.391,.01= C(7) TO C(8) 
DIST   1.335,.01= C(8) TO C(11) 
DIST   1.374,.01= C(9) TO C(10) 
DIST   1.383,.01= C(9) TO N(3) 
DIST   1.362,.01= C(10) TO C(11) 
DIST   1.373,.01= C(12) TO C(13) 
DIST   1.355,.01= C(12) TO N(4) 
DIST   1.360,.01= C(13) TO C(14) 
ANGL 117,1= N(4) TO C(1) TO N(1) 
ANGL 122,1= C(12) TO C(2) TO C(3) 
ANGL 129,1= N(1) TO C(2) TO C(3) 
ANGL 109,1= N(1) TO C(2) TO C(12) 
ANGL 116,1= C(4) TO C(3) TO C(2) 
ANGL 123,1= C(14) TO C(4) TO C(3) 
ANGL 116,1= N(3) TO C(5) TO N(2) 
ANGL 122,1= C(9) TO C(6) TO C(7) 
ANGL 131,1= N(2) TO C(6) TO C(7) 
ANGL 107,1= N(2) TO C(6) TO C(9) 
ANGL 116,1= C(8) TO C(7) TO C(6) 
ANGL 122,1= C(11) TO C(8) TO C(7) 
ANGL 121,1= C(10) TO C(9) TO C(6) 
ANGL 108,1= N(3) TO C(9) TO C(6) 
ANGL 131,1= N(3) TO C(9) TO C(10) 
ANGL 118,1= C(11) TO C(10) TO C(9) 
ANGL 121,1= C(10) TO C(11) TO C(8) 
ANGL 122,1= C(13) TO C(12) TO C(2) 
ANGL 108,1= N(4) TO C(12) TO C(2) 
ANGL 129,1= N(4) TO C(12) TO C(13) 
ANGL 115,1= C(14) TO C(13) TO C(12) 
ANGL 122,1= C(13) TO C(14) TO C(4) 
ANGL 102,1= C(2) TO N(1) TO C(1) 
ANGL 105,1= C(6) TO N(2) TO C(5) 
ANGL 104,1= C(9) TO N(3) TO C(5) 
ANGL 103,1= C(12) TO N(4) TO C(1) 
PLANAR 0.010000  C(1) C(2) C(3) C(4) C(12) C(13) C(14) N(1) N(4) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = C(1) TO N(1) 
VIBR .0, 0.00200 = C(1) TO N(4) 
VIBR .0, 0.00500 = N(4) TO N(1) 
VIBR .0, 0.00200 = C(2) TO C(3) 
VIBR .0, 0.00200 = C(2) TO C(12) 
VIBR .0, 0.00200 = C(2) TO N(1) 
VIBR .0, 0.00500 = C(12) TO C(3) 
VIBR .0, 0.00500 = N(1) TO C(3) 
VIBR .0, 0.00500 = N(1) TO C(12) 
VIBR .0, 0.00200 = C(3) TO C(4) 
VIBR .0, 0.00500 = C(4) TO C(2) 
VIBR .0, 0.00200 = C(4) TO C(14) 
VIBR .0, 0.00500 = C(14) TO C(3) 
VIBR .0, 0.00200 = C(5) TO N(2) 
VIBR .0, 0.00200 = C(5) TO N(3) 
VIBR .0, 0.00500 = N(3) TO N(2) 
VIBR .0, 0.00200 = C(6) TO C(7) 
VIBR .0, 0.00200 = C(6) TO C(9) 
VIBR .0, 0.00200 = C(6) TO N(2) 
VIBR .0, 0.00500 = C(9) TO C(7) 
VIBR .0, 0.00500 = N(2) TO C(7) 
VIBR .0, 0.00500 = N(2) TO C(9) 
VIBR .0, 0.00200 = C(7) TO C(8) 
VIBR .0, 0.00500 = C(8) TO C(6) 
VIBR .0, 0.00200 = C(8) TO C(11) 
VIBR .0, 0.00500 = C(11) TO C(7) 
VIBR .0, 0.00200 = C(9) TO C(10) 
VIBR .0, 0.00200 = C(9) TO N(3) 
VIBR .0, 0.00500 = C(10) TO C(6) 
VIBR .0, 0.00500 = N(3) TO C(6) 
VIBR .0, 0.00500 = N(3) TO C(10) 
VIBR .0, 0.00200 = C(10) TO C(11) 
VIBR .0, 0.00500 = C(11) TO C(9) 
VIBR .0, 0.00500 = C(8) TO C(10) 
VIBR .0, 0.00200 = C(12) TO C(13) 
VIBR .0, 0.00200 = C(12) TO N(4) 
VIBR .0, 0.00500 = C(13) TO C(2) 
VIBR .0, 0.00500 = N(4) TO C(2) 
VIBR .0, 0.00500 = N(4) TO C(13) 
VIBR .0, 0.00200 = C(13) TO C(14) 
VIBR .0, 0.00500 = C(14) TO C(12) 
VIBR .0, 0.00500 = C(13) TO C(4) 
VIBR .0, 0.00500 = C(1) TO C(2) 
VIBR .0, 0.00500 = C(5) TO C(6) 
VIBR .0, 0.00500 = C(5) TO C(9) 
VIBR .0, 0.00500 = C(1) TO C(12) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = C(1) TO N(1) 
U(IJ) .0, 0.04000 = C(1) TO N(4) 
U(IJ) .0, 0.04000 = C(2) TO C(3) 
U(IJ) .0, 0.04000 = C(2) TO C(12) 
U(IJ) .0, 0.04000 = C(2) TO N(1) 
U(IJ) .0, 0.04000 = C(3) TO C(4) 
U(IJ) .0, 0.04000 = C(4) TO C(14) 
U(IJ) .0, 0.04000 = C(5) TO N(2) 
U(IJ) .0, 0.04000 = C(5) TO N(3) 
U(IJ) .0, 0.04000 = C(6) TO C(7) 
U(IJ) .0, 0.04000 = C(6) TO C(9) 
U(IJ) .0, 0.04000 = C(6) TO N(2) 
U(IJ) .0, 0.04000 = C(7) TO C(8) 
U(IJ) .0, 0.04000 = C(8) TO C(11) 
U(IJ) .0, 0.04000 = C(9) TO C(10) 
U(IJ) .0, 0.04000 = C(9) TO N(3) 
U(IJ) .0, 0.04000 = C(10) TO C(11) 
U(IJ) .0, 0.04000 = C(12) TO C(13) 
U(IJ) .0, 0.04000 = C(12) TO N(4) 
U(IJ) .0, 0.04000 = C(13) TO C(14) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
PLANAR 0.010000  C(5) C(6) C(7) C(8) C(9) C(10) C(11) N(2) N(3) 
END                                                                             
;

# 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 .
-2 2 2 x .
0 0 3 x .
-2 4 0 x .
-1 2 0 x .
####################################################################### 
# 
# 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_ZIF-9/ambient
_database_code_depnum_ccdc_archive 'CCDC 1036079'
_audit_update_record             
;
2014-11-25 deposited with the CCDC.
2015-01-23 downloaded from the CCDC.
;
_audit_creation_date             10-05-05
_audit_creation_method           CRYSTALS_ver_14.06

_oxford_structure_analysis_title 'zif9 in R-3'
_chemical_name_systematic        ?
_chemical_melting_point          ?

#end of refcif 
_cell_length_a                   23.0110(8)
_cell_length_b                   23.0110(8)
_cell_length_c                   15.7647(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     7229.2(5)

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   'R -3 '
_symmetry_space_group_name_Hall  '-R 3'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/3,y+2/3,z+2/3
-x+1/3,-y+2/3,-z+2/3
x+2/3,y+1/3,z+1/3
-x+2/3,-y+1/3,-z+1/3
-y,x-y,z
y,-x+y,-z
-y+1/3,x-y+2/3,z+2/3
y+1/3,-x+y+2/3,-z+2/3
-y+2/3,x-y+1/3,z+1/3
y+2/3,-x+y+1/3,-z+1/3
-x+y,-x,z
x-y,x,-z
-x+y+1/3,-x+2/3,z+2/3
x-y+1/3,x+2/3,-z+2/3
-x+y+2/3,-x+1/3,z+1/3
x-y+2/3,x+1/3,-z+1/3

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'
Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692
1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            18

# Given Formula = C3 H5 Co3 N2 O1 
# Dc =      1.08 Fooo =   2682.00 Mu =     30.23 M =    261.88
# Found Formula = C14 H10 Co1 N4 
# Dc =      1.21 FOOO =   2682.00 Mu =     10.60 M =    293.19

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 0.000 0.000 -0.011 248 62 ' '
2 0.000 0.500 0.000 135 43 ' '
3 0.333 0.667 -0.095 246 62 ' '
4 0.500 0.500 0.000 135 43 ' '
5 0.500 0.000 0.000 135 43 ' '
6 0.667 0.333 0.091 246 62 ' '
7 0.167 0.333 0.333 134 43 ' '
8 0.167 0.833 0.333 134 43 ' '
9 0.667 0.833 0.333 134 43 ' '
10 0.333 0.167 0.667 134 43 ' '
11 0.833 0.667 0.667 134 43 ' '
12 0.833 0.167 0.667 134 43 ' '
_platon_squeeze_details          
;
;

_chemical_formula_sum            'C14 H10 Co1 N4'
_chemical_formula_moiety         'C14 H10 Co1 N4'
_chemical_compound_source        ?
_chemical_formula_weight         293.19


_cell_measurement_reflns_used    5739
_cell_measurement_theta_min      2
_cell_measurement_theta_max      20
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2682
_exptl_absorpt_coefficient_mu    1.060

# Sheldrick geometric approximatio 0.81 0.90 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_T_max  0.90
_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    'USER DEFINED STRUCTURE SOLUTION'
_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_reflns_number            3290
_reflns_number_total             3290
_diffrn_reflns_av_R_equivalents  0.102
# Number of reflections without Friedels Law is 3290 
# Number of reflections with Friedels Law is 0 
# Theoretical number of reflections is about 3286 


_diffrn_reflns_theta_min         1.647
_diffrn_reflns_theta_max         26.374
_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        26.374
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       19
_reflns_limit_h_min              -28
_reflns_limit_h_max              14
_reflns_limit_k_min              0
_reflns_limit_k_max              28
_reflns_limit_l_min              0
_reflns_limit_l_max              19

_oxford_diffrn_Wilson_B_factor   3.19
_oxford_diffrn_Wilson_scale      905.06

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

_refine_diff_density_min         -0.85
_refine_diff_density_max         0.72


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


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         3276
_refine_ls_number_restraints     0
_refine_ls_number_parameters     172
_oxford_refine_ls_R_factor_ref   0.0892
_refine_ls_wR_factor_ref         0.0916
_refine_ls_goodness_of_fit_ref   0.8669
_refine_ls_shift/su_max          0.0005496
_refine_ls_shift/su_mean         0.0000193


# The values computed from all data 
_oxford_reflns_number_all        3276
_refine_ls_R_factor_all          0.0892
_refine_ls_wR_factor_all         0.0916

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                1895
_refine_ls_R_factor_gt           0.0392
_refine_ls_wR_factor_gt          0.0823

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


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    none # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.04P)² + 5.56P] 
 ,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 atomsattached to an atom.

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
Co1 Co 0.40361(2) 0.065623(19) 0.32560(2) 0.0427 1.0000 Uani . . . . . . .
C1 C 0.33781(15) 0.03327(15) 0.15800(19) 0.0480 1.0000 Uani . . . . . . .
C2 C 0.36156(15) -0.04313(15) 0.18766(19) 0.0464 1.0000 Uani . . . . . . .
C3 C 0.38137(16) -0.08591(17) 0.2236(2) 0.0619 1.0000 Uani . . . . . . .
C4 C 0.36852(19) -0.14204(19) 0.1785(3) 0.0757 1.0000 Uani . . . . . . .
C5 C 0.39309(15) 0.19221(15) 0.33969(17) 0.0467 1.0000 Uani . . . . . . .
C6 C 0.45281(15) 0.19628(15) 0.23332(19) 0.0501 1.0000 Uani . . . . . . .
C7 C 0.48890(19) 0.18533(18) 0.1707(2) 0.0730 1.0000 Uani . . . . . . .
C8 C 0.5233(2) 0.2365(2) 0.1136(2) 0.0890 1.0000 Uani . . . . . . .
C9 C 0.45173(15) 0.25596(15) 0.23785(19) 0.0490 1.0000 Uani . . . . . . .
C10 C 0.48772(18) 0.30791(18) 0.1802(2) 0.0672 1.0000 Uani . . . . . . .
C11 C 0.5232(2) 0.2964(2) 0.1183(2) 0.0848 1.0000 Uani . . . . . . .
C12 C 0.32895(14) -0.05759(14) 0.10899(19) 0.0456 1.0000 Uani . . . . . . .
C13 C 0.31701(16) -0.11424(17) 0.0628(2) 0.0593 1.0000 Uani . . . . . . .
C14 C 0.3376(2) -0.15532(18) 0.1000(3) 0.0755 1.0000 Uani . . . . . . .
N1 N 0.36676(12) 0.01551(12) 0.21802(14) 0.0467 1.0000 Uani . . . . . . .
N2 N 0.41394(12) 0.15530(12) 0.30014(14) 0.0473 1.0000 Uani . . . . . . .
N3 N 0.41264(12) 0.25292(12) 0.30727(14) 0.0477 1.0000 Uani . . . . . . .
N4 N 0.31388(12) -0.00784(12) 0.09108(14) 0.0458 1.0000 Uani . . . . . . .
H11 H 0.3335 0.0719 0.1614 0.0585 1.0000 Uiso . . . . . . .
H31 H 0.4024 -0.0758 0.2776 0.0752 1.0000 Uiso . . . . . . .
H41 H 0.3821 -0.1708 0.2015 0.0911 1.0000 Uiso . . . . . . .
H51 H 0.3664 0.1766 0.3891 0.0575 1.0000 Uiso . . . . . . .
H71 H 0.4884 0.1441 0.1674 0.0888 1.0000 Uiso . . . . . . .
H81 H 0.5473 0.2308 0.0682 0.1106 1.0000 Uiso . . . . . . .
H101 H 0.4884 0.3497 0.1842 0.0834 1.0000 Uiso . . . . . . .
H111 H 0.5482 0.3311 0.0780 0.0986 1.0000 Uiso . . . . . . .
H131 H 0.2943 -0.1240 0.0104 0.0724 1.0000 Uiso . . . . . . .
H141 H 0.3309 -0.1940 0.0692 0.0927 1.0000 Uiso . . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.051495(8)
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
Co1 . N3 16_545 1.993(2) yes
Co1 . N4 17_555 1.986(2) yes
Co1 . N1 . 1.987(2) yes
Co1 . N2 . 1.996(2) yes
C1 . N1 . 1.334(3) yes
C1 . N4 . 1.338(3) yes
C1 . H11 . 0.945 no
C2 . C3 . 1.395(4) yes
C2 . C12 . 1.401(4) yes
C2 . N1 . 1.379(3) yes
C3 . C4 . 1.371(5) yes
C3 . H31 . 0.949 no
C4 . C14 . 1.383(5) yes
C4 . H41 . 0.935 no
C5 . N2 . 1.322(3) yes
C5 . N3 . 1.337(3) yes
C5 . H51 . 0.945 no
C6 . C7 . 1.392(4) yes
C6 . C9 . 1.388(4) yes
C6 . N2 . 1.398(3) yes
C7 . C8 . 1.376(5) yes
C7 . H71 . 0.945 no
C8 . C11 . 1.380(5) yes
C8 . H81 . 0.951 no
C9 . C10 . 1.397(4) yes
C9 . N3 . 1.396(3) yes
C10 . C11 . 1.381(5) yes
C10 . H101 . 0.957 no
C11 . H111 . 0.956 no
C12 . C13 . 1.395(4) yes
C12 . N4 . 1.381(3) yes
C13 . C14 . 1.382(5) yes
C13 . H131 . 0.944 no
C14 . H141 . 0.955 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
N3 16_545 Co1 . N4 17_555 104.30(9) yes
N3 16_545 Co1 . N1 . 115.30(10) yes
N4 17_555 Co1 . N1 . 112.36(9) yes
N3 16_545 Co1 . N2 . 108.10(10) yes
N4 17_555 Co1 . N2 . 114.10(9) yes
N1 . Co1 . N2 . 102.95(10) yes
N1 . C1 . N4 . 115.8(3) yes
N1 . C1 . H11 . 123.5 no
N4 . C1 . H11 . 120.7 no
C3 . C2 . C12 . 121.1(3) yes
C3 . C2 . N1 . 130.5(3) yes
C12 . C2 . N1 . 108.3(2) yes
C2 . C3 . C4 . 117.5(3) yes
C2 . C3 . H31 . 119.9 no
C4 . C3 . H31 . 122.6 no
C3 . C4 . C14 . 121.2(3) yes
C3 . C4 . H41 . 118.2 no
C14 . C4 . H41 . 120.6 no
N2 . C5 . N3 . 116.8(3) yes
N2 . C5 . H51 . 121.4 no
N3 . C5 . H51 . 121.8 no
C7 . C6 . C9 . 121.5(3) yes
C7 . C6 . N2 . 130.6(3) yes
C9 . C6 . N2 . 107.9(3) yes
C6 . C7 . C8 . 116.7(3) yes
C6 . C7 . H71 . 120.8 no
C8 . C7 . H71 . 122.5 no
C7 . C8 . C11 . 122.1(3) yes
C7 . C8 . H81 . 119.9 no
C11 . C8 . H81 . 118.0 no
C6 . C9 . C10 . 121.1(3) yes
C6 . C9 . N3 . 108.7(3) yes
C10 . C9 . N3 . 130.1(3) yes
C9 . C10 . C11 . 116.7(3) yes
C9 . C10 . H101 . 121.5 no
C11 . C10 . H101 . 121.8 no
C10 . C11 . C8 . 121.8(3) yes
C10 . C11 . H111 . 118.4 no
C8 . C11 . H111 . 119.8 no
C2 . C12 . C13 . 121.0(3) yes
C2 . C12 . N4 . 108.1(3) yes
C13 . C12 . N4 . 130.9(3) yes
C12 . C13 . C14 . 116.4(3) yes
C12 . C13 . H131 . 120.4 no
C14 . C13 . H131 . 123.2 no
C4 . C14 . C13 . 122.8(3) yes
C4 . C14 . H141 . 119.0 no
C13 . C14 . H141 . 118.1 no
C2 . N1 . Co1 . 131.8(2) yes
C2 . N1 . C1 . 104.0(2) yes
Co1 . N1 . C1 . 124.2(2) yes
C6 . N2 . Co1 . 123.63(19) yes
C6 . N2 . C5 . 103.7(2) yes
Co1 . N2 . C5 . 132.5(2) yes
C9 . N3 . Co1 10_555 123.1(2) yes
C9 . N3 . C5 . 102.9(2) yes
Co1 10_555 N3 . C5 . 134.0(2) yes
C12 . N4 . C1 . 103.9(2) yes
C12 . N4 . Co1 9_544 130.9(2) yes
C1 . N4 . Co1 9_544 125.2(2) yes
