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

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

data_SP3153_ambient
_database_code_depnum_ccdc_archive 'CCDC 1447804'
_audit_update_record             
;
2016-05-13 deposited with the CCDC.
2016-05-13 downloaded from the CCDC.
;
_audit_creation_date             14-01-13
_audit_creation_method           CRYSTALS_ver_14.40
_oxford_structure_analysis_title 'SP3153 in I-42d'
_chemical_name_systematic        'potassium cobalt (II) citrate, UTSA-16'

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
;
#-------------------------------------------------------------------------------# 
# CheckCIF responses  
PLAT430_ALERT_2_A Short Inter D...A Contact  O5     ..  O10     ..       2.45 Ang.  
PLAT430_ALERT_2_A Short Inter D...A Contact  O10    ..  O10     ..       2.37 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact  O5     ..  O10     ..       2.74 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact  O2     ..  O11     ..       2.77 Ang.    
PLAT430_ALERT_2_B Short Inter D...A Contact  O11    ..  O80     ..       2.54 Ang.
PLAT430_ALERT_2_C Short Inter D...A Contact  O5     ..  O9      ..       2.88 Ang.  
PLAT430_ALERT_2_C Short Inter D...A Contact  O7     ..  O10     ..       2.85 Ang.
 - Atoms form a hydrogen bonded network of water molecules in the pore of the 
framework.
PLAT601_ALERT_2_A Structure Contains Solvent Accessible VOIDS of .        543 Ang3  
 - The structure is a porous metal-organic framework containing mobile disordered
solvent.
PLAT242_ALERT_2_B Low    'MainMol' Ueq as Compared to Neighbors of         K1 Check
 - O8 is a water molecule bound to the heavier K1 leading to a significant
discrepancy in Ueqs. 
PLAT306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?) .......        O11 Check 
PLAT090_ALERT_3_C Poor Data / Parameter Ratio (Zmax > 18) ........       8.09 Note  
PLAT004_ALERT_5_G Polymeric Structure Found with Maximum Dimension          3 Info  
 - Correct.
PLAT005_ALERT_5_G No Embedded Refinement Details found  in the CIF     Please Do ! 
 - Not correct see end of data block.
PLAT003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...         13 Report
PLAT300_ALERT_4_G Atom Site Occupancy of >O80    is Constrained at     0.5194 Check 
PLAT300_ALERT_4_G Atom Site Occupancy of <O81    is Constrained at     0.4806 Check 
PLAT300_ALERT_4_G Atom Site Occupancy of >O9     is Constrained at      0.591 Check 
PLAT300_ALERT_4_G Atom Site Occupancy of <O10    is Constrained at      0.409 Check 
PLAT311_ALERT_2_G Isolated Disordered Oxygen Atom (No H's ?) .....         O9 Check 
PLAT311_ALERT_2_G Isolated Disordered Oxygen Atom (No H's ?) .....        O10 Check 
 - O9 and O10 are restrained and model a weakly bound disordered water position.
Occupancies and Uiso's refined for O9-O81.
PLAT301_ALERT_3_G Main Residue  Disorder ............ Percentage =          6 Note  
PLAT302_ALERT_4_G Anion/Solvent Disorder ............ Percentage =         50 Note
PLAT202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent .........          1 Check 
PLAT201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) .......          1 Report 
PLAT220_ALERT_2_B Non-Solvent Resd 1   O   Ueq(max)/Ueq(min) Range        7.3 Ratio 
 - The main framework is not disordered, this alert arises from the definition of 
the framework connectivity.
PLAT792_ALERT_1_G The Model has Chirality at C3      (Polar  SPGR)          S Verify
PLAT794_ALERT_5_G Tentative Bond Valency for Co2     (III)   .....       1.58 Note  
PLAT808_ALERT_5_G No Parseable SHELXL Style Weighting Scheme Found     Please Check
 - Non-SHELXL weighting scheme used.
PLAT860_ALERT_3_G Number of Least-Squares Restraints .............        101 Note  
 - Not correct, see refinement details at end of data block.
#-------------------------------------------------------------------------------#
;


_cell_length_a                   13.0691(4)
_cell_length_b                   13.0691(4)
_cell_length_c                   30.1570(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5150.9(3)


_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I -4 2 d '
_symmetry_space_group_name_Hall  'I -4 2bw'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,y+1/2,z+1/2
y,-x,-z
y+1/2,-x+1/2,-z+1/2
-x,-y,z
-x+1/2,-y+1/2,z+1/2
-y,x,-z
-y+1/2,x+1/2,-z+1/2
-x+1/2,y,-z+3/4
-x+1,y+1/2,-z+5/4
-y+1/2,-x,z+3/4
-y+1,-x+1/2,z+5/4
x+1/2,-y,-z+3/4
x+1,-y+1/2,-z+5/4
y+1/2,x,z+3/4
y+1,x+1/2,z+5/4

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'
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'
K 0.2009 0.2494 8.2186 12.7949 7.4398 0.7748 1.0519 213.1870 0.8659 41.6841
1.4228 '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            8

# Given Formula = C12 H12 Co3 K2 O16 
# Dc =      1.72 Fooo =   2720.00 Mu =     22.98 M =    333.61
# Found Formula = C12 H8 Co3 K1 O20 
# Dc =      1.77 FOOO =   2720.00 Mu =     21.55 M =    344.04

_chemical_formula_sum            'C12 H8 Co3 K1 O20'
_chemical_formula_moiety         'C12 H8 Co3 K1 O14, O6'
_chemical_compound_source        ?
_chemical_formula_weight         688.08


_cell_measurement_reflns_used    9907
_cell_measurement_theta_min      3
_cell_measurement_theta_max      25
_cell_measurement_temperature    300

_exptl_crystal_description       octahedron
_exptl_crystal_colour            purple
_exptl_crystal_size_min          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.500

_exptl_crystal_density_diffrn    1.774
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2720
_exptl_absorpt_coefficient_mu    2.155

# Sheldrick geometric approximatio 0.72 0.72 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_T_max  0.72
_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    'SIR92 (Altomare et al., 1994)'
_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      300
_diffrn_reflns_number            24384
_reflns_number_total             2365
_diffrn_reflns_av_R_equivalents  0.046
# Number of reflections without Friedels Law is 2365 
# Number of reflections with Friedels Law is 1319 
# Theoretical number of reflections is about 1178 


_diffrn_reflns_theta_min         1.698
_diffrn_reflns_theta_max         25.339
_diffrn_measured_fraction_theta_max 1.000

_diffrn_reflns_theta_full        25.339
_diffrn_measured_fraction_theta_full 1.000


_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_reflns_limit_h_min              -11
_reflns_limit_h_max              11
_reflns_limit_k_min              0
_reflns_limit_k_max              15
_reflns_limit_l_min              0
_reflns_limit_l_max              36

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

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

_refine_diff_density_min         -0.51
_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>2.0\s(I)
_refine_ls_number_reflns         2187
_refine_ls_number_restraints     101
_refine_ls_number_parameters     163
_oxford_refine_ls_R_factor_ref   0.0352
_refine_ls_wR_factor_ref         0.0893
_refine_ls_goodness_of_fit_ref   0.9014
_refine_ls_shift/su_max          0.0008587
_refine_ls_shift/su_mean         0.0000365


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        2353
_refine_ls_R_factor_all          0.0389
_refine_ls_wR_factor_all         0.0961

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                2187
_refine_ls_R_factor_gt           0.0352
_refine_ls_wR_factor_gt          0.0893

_refine_ls_abs_structure_Flack   0.04(2)
_refine_ls_abs_structure_details 'Flack (1983), 1046 Friedel-pairs'
# 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 ad


_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, 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: 
 8.59 13.2 6.79 1.91 
;

# 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 0.89563(4) 0.95191(4) 0.459630(15) 0.0190 1.0000 Uani . . . . . .
Co2 Co 1.0000 1.0000 0.30727(2) 0.0264 1.0000 Uani S T . . . .
K1 K 0.7500 0.83937(13) 0.3750 0.0407 1.0000 Uani S T . . . .
C1 C 1.1070(3) 0.9172(3) 0.37798(13) 0.0221 1.0000 Uani . U . . . .
C2 C 1.1479(3) 0.8342(3) 0.40768(13) 0.0245 1.0000 Uani . U . . . .
C3 C 1.0780(3) 0.8100(3) 0.44758(12) 0.0201 1.0000 Uani . U . . . .
C4 C 1.1396(3) 0.7334(3) 0.47656(13) 0.0248 1.0000 Uani . U . . . .
C5 C 1.0774(3) 0.6840(3) 0.51328(12) 0.0225 1.0000 Uani . U . . . .
C6 C 0.9777(3) 0.7580(3) 0.43128(13) 0.0271 1.0000 Uani . U . . . .
H21 H 1.2149 0.8576 0.4187 0.0284 1.0000 Uiso R . . . . .
H22 H 1.1558 0.7716 0.3911 0.0278 1.0000 Uiso R . . . . .
H41 H 1.1942 0.7725 0.4897 0.0280 1.0000 Uiso R . . . . .
H42 H 1.1693 0.6809 0.4585 0.0281 1.0000 Uiso R . . . . .
O1 O 1.1091(2) 1.0083(2) 0.39036(8) 0.0246 1.0000 Uani . U . . . .
O2 O 1.0691(2) 0.8898(2) 0.34074(9) 0.0282 1.0000 Uani . U . . . .
O3 O 1.0530(2) 0.9008(2) 0.47106(8) 0.0191 1.0000 Uani . U . . . .
O4 O 0.8943(3) 0.8034(2) 0.43758(10) 0.0285 1.0000 Uani . U . . . .
O5 O 0.9865(3) 0.6728(3) 0.41289(15) 0.0531 1.0000 Uani . U . . . .
O6 O 1.0358(2) 0.7382(2) 0.54179(9) 0.0294 1.0000 Uani . U . . . .
O7 O 1.0742(3) 0.5870(2) 0.51393(11) 0.0390 1.0000 Uani . U . . . .
O9 O 1.1741(11) 0.4531(12) 0.4486(5) 0.117(4) 0.5910 Uiso . . . . . .
O10 O 1.0906(10) 0.4945(11) 0.4286(4) 0.067(3) 0.4090 Uiso . . . . . .
O11 O 0.4347(13) 0.7089(12) 0.4573(6) 0.2392 1.0000 Uani . . . . . .
O80 O 0.6121(19) 0.7168(18) 0.4231(7) 0.140(7) 0.5194 Uiso . . . . . .
O81 O 0.6472(18) 0.6781(18) 0.4162(7) 0.124(7) 0.4806 Uiso . . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0184(3) 0.0218(3) 0.0167(2) -0.0008(2) -0.0008(2) -0.0018(2)
Co2 0.0222(4) 0.0369(5) 0.0201(4) 0.0000 0.0000 -0.0044(4)
K1 0.0403(8) 0.0406(8) 0.0411(7) 0.0000 -0.0175(7) 0.0000
C1 0.0198(17) 0.0288(15) 0.0178(14) 0.0007(12) 0.0042(14) -0.0004(15)
C2 0.028(2) 0.0257(19) 0.0195(15) 0.0001(14) 0.0053(14) 0.0055(16)
C3 0.0237(17) 0.0180(15) 0.0187(16) 0.0003(11) 0.0026(13) 0.0010(13)
C4 0.027(2) 0.0219(18) 0.0255(17) 0.0025(14) 0.0043(14) 0.0047(15)
C5 0.028(2) 0.0199(14) 0.0198(16) 0.0026(12) -0.0021(13) 0.0029(14)
C6 0.0301(16) 0.0291(18) 0.0221(18) -0.0051(14) -0.0015(14) -0.0026(13)
O1 0.0266(13) 0.0267(12) 0.0205(11) 0.0022(11) 0.0013(11) -0.0019(13)
O2 0.0352(16) 0.0301(15) 0.0193(11) 0.0002(11) -0.0015(11) 0.0001(13)
O3 0.0223(13) 0.0161(12) 0.0189(11) -0.0010(10) 0.0013(10) -0.0004(12)
O4 0.0284(14) 0.0270(15) 0.0303(14) -0.0043(12) -0.0054(13) -0.0040(11)
O5 0.040(2) 0.0378(19) 0.082(3) -0.0290(19) -0.007(2) -0.0009(16)
O6 0.0396(17) 0.0229(13) 0.0257(13) 0.0024(11) 0.0084(13) 0.0004(12)
O7 0.063(2) 0.0198(12) 0.0346(16) -0.0002(12) 0.0193(15) -0.0026(14)
O11 0.242(16) 0.185(13) 0.290(18) 0.146(13) -0.049(14) -0.032(11)

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.059752(18)
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 . O1 5_775 2.153(3) yes
Co1 . O3 3_576 2.092(2) yes
Co1 . O3 5_775 2.068(3) yes
Co1 . O6 3_576 2.065(3) yes
Co1 . Co1 5_775 3.0037(10) yes
Co1 . Co1 3_576 3.2311(8) yes
Co1 . Co1 7_756 3.2311(8) yes
Co1 . O3 . 2.190(3) yes
Co1 . O4 . 2.052(3) yes
Co2 . O7 11_674 1.985(3) yes
Co2 . O7 15_554 1.985(3) yes
Co2 . O2 5_775 1.977(3) yes
Co2 . O2 . 1.977(3) yes
C1 . C2 . 1.505(6) yes
C1 . O1 . 1.248(5) yes
C1 . O2 . 1.278(5) yes
C2 . C3 . 1.543(5) yes
C2 . H21 . 0.984 no
C2 . H22 . 0.964 no
C3 . C4 . 1.553(6) yes
C3 . C6 . 1.556(6) yes
C3 . O3 . 1.420(5) yes
C4 . C5 . 1.518(6) yes
C4 . H41 . 0.963 no
C4 . H42 . 0.958 no
C5 . O6 . 1.239(5) yes
C5 . O7 . 1.269(5) yes
C6 . O4 . 1.256(6) yes
C6 . O5 . 1.249(6) yes
O9 . O10 . 1.359(18) 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
O1 5_775 Co1 . O3 3_576 167.80(11) yes
O1 5_775 Co1 . O3 5_775 86.93(10) yes
O3 3_576 Co1 . O3 5_775 81.46(10) yes
O1 5_775 Co1 . O6 3_576 86.12(12) yes
O3 3_576 Co1 . O6 3_576 93.17(10) yes
O3 5_775 Co1 . O6 3_576 104.76(12) yes
O1 5_775 Co1 . Co1 5_775 85.72(9) yes
O3 3_576 Co1 . Co1 5_775 89.05(7) yes
O3 5_775 Co1 . Co1 5_775 46.80(8) yes
O6 3_576 Co1 . Co1 5_775 150.78(9) yes
O1 5_775 Co1 . Co1 3_576 126.07(8) yes
O3 3_576 Co1 . Co1 3_576 42.16(7) yes
O3 5_775 Co1 . Co1 3_576 39.32(7) yes
O6 3_576 Co1 . Co1 3_576 101.22(9) yes
Co1 5_775 Co1 . Co1 3_576 62.302(9) yes
O1 5_775 Co1 . Co1 7_756 143.49(9) yes
O3 3_576 Co1 . Co1 7_756 38.77(7) yes
O3 5_775 Co1 . Co1 7_756 83.46(7) yes
O6 3_576 Co1 . Co1 7_756 130.39(8) yes
Co1 5_775 Co1 . Co1 7_756 62.302(9) yes
O1 5_775 Co1 . O3 . 104.68(11) yes
O3 3_576 Co1 . O3 . 78.65(10) yes
O3 5_775 Co1 . O3 . 87.29(11) yes
O6 3_576 Co1 . O3 . 164.40(11) yes
Co1 5_775 Co1 . O3 . 43.50(7) yes
O1 5_775 Co1 . O4 . 85.04(12) yes
O3 3_576 Co1 . O4 . 107.16(11) yes
O3 5_775 Co1 . O4 . 159.64(12) yes
O6 3_576 Co1 . O4 . 93.34(13) yes
Co1 5_775 Co1 . O4 . 113.81(10) yes
Co1 3_576 Co1 . Co1 7_756 55.397(18) yes
Co1 3_576 Co1 . O3 . 81.70(7) yes
Co1 7_756 Co1 . O3 . 39.89(6) yes
Co1 3_576 Co1 . O4 . 146.05(9) yes
Co1 7_756 Co1 . O4 . 91.96(9) yes
O3 . Co1 . O4 . 76.73(12) yes
O7 11_674 Co2 . O7 15_554 97.7(2) yes
O7 11_674 Co2 . O2 5_775 115.50(13) yes
O7 15_554 Co2 . O2 5_775 104.00(14) yes
O7 11_674 Co2 . O2 . 104.00(14) yes
O7 15_554 Co2 . O2 . 115.50(13) yes
O2 5_775 Co2 . O2 . 118.59(17) yes
C2 . C1 . O1 . 120.1(4) yes
C2 . C1 . O2 . 117.3(4) yes
O1 . C1 . O2 . 122.6(4) yes
C1 . C2 . C3 . 113.7(3) yes
C1 . C2 . H21 . 107.0 no
C3 . C2 . H21 . 109.1 no
C1 . C2 . H22 . 110.0 no
C3 . C2 . H22 . 107.0 no
H21 . C2 . H22 . 110.0 no
C2 . C3 . C4 . 105.4(3) yes
C2 . C3 . C6 . 110.0(3) yes
C4 . C3 . C6 . 109.4(3) yes
C2 . C3 . O3 . 110.7(3) yes
C4 . C3 . O3 . 112.2(3) yes
C6 . C3 . O3 . 109.2(3) yes
C3 . C4 . C5 . 114.1(3) yes
C3 . C4 . H41 . 105.9 no
C5 . C4 . H41 . 108.8 no
C3 . C4 . H42 . 110.5 no
C5 . C4 . H42 . 109.1 no
H41 . C4 . H42 . 108.3 no
C4 . C5 . O6 . 119.8(4) yes
C4 . C5 . O7 . 117.0(3) yes
O6 . C5 . O7 . 123.1(4) yes
C3 . C6 . O4 . 118.5(4) yes
C3 . C6 . O5 . 116.9(4) yes
O4 . C6 . O5 . 124.6(4) yes
Co1 5_775 O1 . C1 . 121.3(2) yes
Co2 . O2 . C1 . 114.9(3) yes
Co1 . O3 . Co1 7_756 97.95(10) yes
Co1 . O3 . C3 . 113.1(2) yes
Co1 7_756 O3 . C3 . 118.6(2) yes
Co1 . O3 . Co1 5_775 89.70(10) yes
Co1 7_756 O3 . Co1 5_775 101.92(11) yes
C3 . O3 . Co1 5_775 128.3(2) yes
Co1 . O4 . C6 . 119.2(3) yes
Co1 7_756 O6 . C5 . 121.4(3) yes
Co2 12_664 O7 . C5 . 126.7(3) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 27/04/16 at 15:14:06
#
#LIST     12                                                                    
BLOCK 
CONT SCALE 
CONT CO   (    1 ,X'S,U'S)  UNTIL C    (    6 ) 
CONT O    (    1 ,X'S,U'S)  UNTIL O    (    7 ) 
CONT O    (    9 ,X'S,U[ISO])  UNTIL O    (   10 ) 
CONT O    (   11 ,X'S,U'S) 
CONT O    (   80 ,X'S,U[ISO])  UNTIL O    (   81 ) 
CONT ENANTIO 
RIDE C   (   2,X'S) H   (  21,X'S) H   (  22,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) H   (  42,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 27/04/16 at 15:14:06
#
#LIST     16                                                                    
NO 
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 C(2) 
VIBR .0, 0.00200 = C(1) TO O(1) 
VIBR .0, 0.00200 = C(1) TO O(2) 
VIBR .0, 0.00500 = O(1) TO C(2) 
VIBR .0, 0.00500 = O(2) TO C(2) 
VIBR .0, 0.00500 = O(2) TO O(1) 
VIBR .0, 0.00200 = C(2) TO C(3) 
VIBR .0, 0.00500 = C(3) TO C(1) 
VIBR .0, 0.00200 = C(3) TO C(4) 
VIBR .0, 0.00200 = C(3) TO C(6) 
VIBR .0, 0.00200 = C(3) TO O(3) 
VIBR .0, 0.00500 = C(4) TO C(2) 
VIBR .0, 0.00500 = C(6) TO C(2) 
VIBR .0, 0.00500 = C(6) TO C(4) 
VIBR .0, 0.00500 = O(3) TO C(2) 
VIBR .0, 0.00500 = O(3) TO C(4) 
VIBR .0, 0.00500 = O(3) TO C(6) 
VIBR .0, 0.00200 = C(4) TO C(5) 
VIBR .0, 0.00500 = C(5) TO C(3) 
VIBR .0, 0.00200 = C(5) TO O(6) 
VIBR .0, 0.00200 = C(5) TO O(7) 
VIBR .0, 0.00500 = O(6) TO C(4) 
VIBR .0, 0.00500 = O(7) TO C(4) 
VIBR .0, 0.00500 = O(7) TO O(6) 
VIBR .0, 0.00200 = C(6) TO O(4) 
VIBR .0, 0.00200 = C(6) TO O(5) 
VIBR .0, 0.00500 = O(4) TO C(3) 
VIBR .0, 0.00500 = O(5) TO C(3) 
VIBR .0, 0.00500 = O(5) TO O(4) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = C(1) TO C(2) 
U(IJ) .0, 0.08000 = C(1) TO O(1) 
U(IJ) .0, 0.08000 = C(1) TO O(2) 
U(IJ) .0, 0.04000 = C(2) TO C(3) 
U(IJ) .0, 0.04000 = C(3) TO C(4) 
U(IJ) .0, 0.04000 = C(3) TO C(6) 
U(IJ) .0, 0.08000 = C(3) TO O(3) 
U(IJ) .0, 0.04000 = C(4) TO C(5) 
U(IJ) .0, 0.08000 = C(5) TO O(6) 
U(IJ) .0, 0.08000 = C(5) TO O(7) 
U(IJ) .0, 0.08000 = C(6) TO O(4) 
U(IJ) .0, 0.08000 = C(6) TO O(5) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
_exptl_crystal_recrystallization_method 'hydrothermal synthesis'
####################################################################### 
# 
# 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_SP3064_3kbar
_database_code_depnum_ccdc_archive 'CCDC 1447805'
_audit_update_record             
;
2016-05-13 deposited with the CCDC.
2016-05-13 downloaded from the CCDC.
;

_audit_creation_date             14-07-21
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 'UTSA16 in I-42d'
_chemical_name_systematic        'potassium cobalt (II) citrate, UTSA-16'

_exptl_special_details           
; 
Sample was placed in a Merrill-Basset DAC with Fluorinert FC70 at a pressure
of 0.3(1) GPa.
;
_refine_special_details          
; 
Main residue atoms could be anisotropically refined, however pore water atoms
were isotropically refined.  
;


#    CheckCIF Responses
#   Alert level A
#   PLAT027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............      18.08 Degree
#   PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low .......      0.784 Note 
#   PLAT341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............     0.0144 Ang. 
#   PLAT090_ALERT_3_C Poor Data / Parameter Ratio (Zmax > 18) ........       7.66 Note
#   REFNR01_ALERT_3_C  Ratio of reflections to parameters is < 10 for a
#               non-centrosymmetric structure, where ZMAX > 18
#               sine(theta)/lambda                0.5747
#               Proportion of unique data used    0.8686
#               Ratio reflections to parameters   8.6040 
#   PLAT003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...         13 Why ?  
#    - The high pressure cell causes shading of a significant proportion of the
#   sphere of reflections. This means that the completeness is reduced and as
#   such the quality of the model is lower. 
#   
#   PLAT940_ALERT_3_B F**2 Refinement with I < n * Sigma(I) only .....     Please Check
#    - The lower data quality forced the usage of an I/sig(I) cut off of 2.0 to
#   be used.
#   
#   PLAT601_ALERT_2_A Structure Contains Solvent Accessible VOIDS of .       1048 Ang3  
#   PLAT004_ALERT_5_G Polymeric Structure Found with Dimension .......          3 Info  
#    - The structure is a porous metal-organic framework containing mobile disordered
#   solvent. 
#   Alert level B
#   THETM01_ALERT_3_B  The value of sine(theta_max)/wavelength is less than 0.575
#               Calculated sin(theta_max)/wavelength =    0.5747
#   PLAT780_ALERT_1_A Coordinates do not Form a Properly Connected Set     Please Do ! 
#    - No action taken
#   
#   PLAT201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) .......          1 Why ? 
#   PLAT220_ALERT_2_B Large Non-Solvent  O     Ueq(max)/Ueq(min) Range        7.3 Ratio
#   PLAT202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent .........          1 
#   PLAT302_ALERT_4_G Anion/Solvent Disorder ............ Percentage =        100 Note  
#   PLAT311_ALERT_2_G Isolated Disordered Oxygen Atom (No H's ?) .....         O9 Check 
#   PLAT311_ALERT_2_G Isolated Disordered Oxygen Atom (No H's ?) .....        O10 Check 
#    - The 'main' and 'solvent' residues as termed by CheckCIF do not follow
#   our analysis. The large 'non-solvent' oxygen atom is a solvent water 
#   molecule which is isotropically refined. Oxygen atoms O9 and O10 are pore 
#   water molecules
#   
#   Alert level C
#   PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       2.19 Why ? 
#    - We believe the pore contents to contain further highly disorder water and
#   potassium species and so some residual density is to be expected.      
#   
#   Alert level G
#   PLAT199_ALERT_1_G Reported _cell_measurement_temperature ..... (K)        293 Check 
#   PLAT200_ALERT_1_G Reported   _diffrn_ambient_temperature ..... (K)        293 Check 
#    - Correct
#   
#   PLAT794_ALERT_5_G Tentative Bond Valency for Co2     (III)   .....       1.61 Note 
#    - Correct 
#   PLAT808_ALERT_5_G No Parseable SHELXL Style Weighting Scheme Found     Please Check
#    - Weighting scheme given below
#   PLAT860_ALERT_3_G Number of Least-Squares Restraints .............        101 Note  
#    - Low data quality due to the high-pressure cell requires numerous restraints
#   on the citrate moiety to give stable refinements.




_cell_length_a                   13.0005(5)
_cell_length_b                   13.0005(5)
_cell_length_c                   30.2002(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5104.2(3)

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I -4 2 d '
_symmetry_space_group_name_Hall  'I -4 2bw'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,y+1/2,z+1/2
y,-x,-z
y+1/2,-x+1/2,-z+1/2
-x,-y,z
-x+1/2,-y+1/2,z+1/2
-y,x,-z
-y+1/2,x+1/2,-z+1/2
-x+1/2,y,-z+3/4
-x+1,y+1/2,-z+5/4
-y+1/2,-x,z+3/4
-y+1,-x+1/2,z+5/4
x+1/2,-y,-z+3/4
x+1,-y+1/2,-z+5/4
y+1/2,x,z+3/4
y+1,x+1/2,z+5/4

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'
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'
K 0.2009 0.2494 8.2186 12.7949 7.4398 0.7748 1.0519 213.1870 0.8659 41.6841
1.4228 '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            8

# Given Formula = C12 H12 Co3 K2 O16 
# Dc =      1.74 Fooo =   2592.00 Mu =     23.19 M =    333.61
# Found Formula = C12 H8 Co3 K1 O18 
# Dc =      1.71 FOOO =   2592.00 Mu =     21.64 M =    328.04

_chemical_formula_sum            'C12 H8 Co3 K1 O18'
_chemical_formula_moiety         'C12 H8 Co3 K1 O14,O4'
_chemical_compound_source        ?
_chemical_formula_weight         656.08


_cell_measurement_reflns_used    4122
_cell_measurement_theta_min      4
_cell_measurement_theta_max      25
_cell_measurement_temperature    293

_exptl_crystal_description       octahedron
_exptl_crystal_colour            purple
_exptl_crystal_size_min          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.450

_exptl_crystal_density_diffrn    1.707
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2592
_exptl_absorpt_coefficient_mu    2.164

# Sheldrick geometric approximatio 0.72 0.72 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.43
_exptl_absorpt_correction_T_max  0.72
_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            7155
_reflns_number_total             1476
_diffrn_reflns_av_R_equivalents  0.048
# Number of reflections without Friedels Law is 1476 
# Number of reflections with Friedels Law is 843 
# Theoretical number of reflections is about 1014 


_diffrn_reflns_theta_min         3.720
_diffrn_reflns_theta_max         24.107
_diffrn_measured_fraction_theta_max 0.739

_diffrn_reflns_theta_full        18.080
_diffrn_measured_fraction_theta_full 0.784


_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_reflns_limit_h_min              -8
_reflns_limit_h_max              8
_reflns_limit_k_min              0
_reflns_limit_k_max              13
_reflns_limit_l_min              0
_reflns_limit_l_max              34

_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         -0.52
_refine_diff_density_max         1.14


# 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         1282
_refine_ls_number_restraints     101
_refine_ls_number_parameters     149
_oxford_refine_ls_R_factor_ref   0.0576
_refine_ls_wR_factor_ref         0.1485
_refine_ls_goodness_of_fit_ref   0.9537
_refine_ls_shift/su_max          0.0015751
_refine_ls_shift/su_mean         0.0000722


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        1473
_refine_ls_R_factor_all          0.0866
_refine_ls_wR_factor_all         0.3531

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                1282
_refine_ls_R_factor_gt           0.0576
_refine_ls_wR_factor_gt          0.1485

_refine_ls_abs_structure_Flack   0.07(5)
_refine_ls_abs_structure_details 'Flack (1983), 633 Friedel-pairs'
# 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 ad


_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, 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: 
 18.6 29.7 17.5 6.83 1.60 
;

# 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 0.89540(11) 0.95131(11) 0.45964(3) 0.0203 1.0000 Uani . . . . . .
Co2 Co 1.0000 1.0000 0.30781(5) 0.0275 1.0000 Uani S T . . . .
K1 K 0.7500 0.8369(3) 0.3750 0.0436 1.0000 Uani S T . . . .
C1 C 1.1065(8) 0.9159(8) 0.3783(3) 0.0205 1.0000 Uani . U . . . .
C2 C 1.1502(9) 0.8328(9) 0.4082(3) 0.0284 1.0000 Uani . U . . . .
C3 C 1.0771(8) 0.8090(8) 0.4483(3) 0.0244 1.0000 Uani . U . . . .
C4 C 1.1400(9) 0.7335(9) 0.4767(3) 0.0269 1.0000 Uani . U . . . .
C5 C 1.0801(8) 0.6841(9) 0.5135(2) 0.0205 1.0000 Uani . U . . . .
C6 C 0.9785(9) 0.7557(9) 0.4314(3) 0.0280 1.0000 Uani . U . . . .
O1 O 1.1096(6) 1.0093(6) 0.39071(16) 0.0255 1.0000 Uani . U . . . .
O2 O 1.0697(6) 0.8893(6) 0.34092(18) 0.0303 1.0000 Uani . U . . . .
O3 O 1.0543(6) 0.9011(5) 0.47128(16) 0.0242 1.0000 Uani . U . . . .
O4 O 0.8952(6) 0.8011(6) 0.43768(19) 0.0240 1.0000 Uani . U . . . .
O5 O 0.9907(8) 0.6714(7) 0.4144(3) 0.0550 1.0000 Uani . U . . . .
O6 O 1.0373(6) 0.7368(6) 0.54193(18) 0.0327 1.0000 Uani . U . . . .
O7 O 1.0753(7) 0.5848(6) 0.5143(2) 0.0417 1.0000 Uani . U . . . .
O8 O 1.3097(19) 0.623(2) 0.5825(8) 0.176(9) 1.0000 Uiso . . . . . .
O9 O 1.178(2) 0.453(3) 0.4493(9) 0.1128 0.54(2) Uiso . . P . . .
O10 O 1.097(3) 0.490(3) 0.4298(10) 0.1180 0.46(2) Uiso . . P . . .
H21 H 1.2171 0.8561 0.4192 0.0284 1.0000 Uiso R . . . . .
H22 H 1.1581 0.7701 0.3916 0.0278 1.0000 Uiso R . . . . .
H41 H 1.1946 0.7726 0.4899 0.0280 1.0000 Uiso R . . . . .
H42 H 1.1697 0.6810 0.4586 0.0281 1.0000 Uiso R . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0210(8) 0.0228(8) 0.0172(5) 0.0002(5) -0.0003(4) -0.0007(8)
Co2 0.0229(13) 0.0402(14) 0.0194(8) 0.0000 0.0000 -0.0018(12)
K1 0.046(3) 0.044(3) 0.0414(17) 0.0000 -0.0193(15) 0.0000
C1 0.006(5) 0.028(3) 0.028(3) 0.002(2) 0.000(3) -0.003(5)
C2 0.031(5) 0.035(5) 0.020(3) 0.003(3) 0.003(3) 0.005(5)
C3 0.025(4) 0.026(4) 0.022(4) 0.001(2) 0.002(2) 0.005(3)
C4 0.034(6) 0.026(5) 0.021(3) 0.003(3) 0.002(3) 0.005(4)
C5 0.017(6) 0.022(3) 0.023(4) 0.002(2) -0.004(3) 0.003(4)
C6 0.030(3) 0.034(5) 0.020(4) -0.007(3) 0.001(3) 0.003(3)
O1 0.026(4) 0.028(3) 0.022(3) 0.004(2) 0.002(2) -0.010(4)
O2 0.037(5) 0.031(4) 0.023(2) -0.004(2) -0.001(2) 0.008(4)
O3 0.033(4) 0.024(3) 0.016(2) 0.002(2) 0.001(2) -0.002(4)
O4 0.026(3) 0.019(4) 0.027(3) -0.006(2) -0.004(3) -0.003(4)
O5 0.036(6) 0.047(5) 0.082(5) -0.034(4) -0.011(5) 0.013(5)
O6 0.047(5) 0.025(4) 0.026(3) -0.001(2) 0.008(3) 0.001(4)
O7 0.071(6) 0.022(3) 0.032(3) 0.002(3) 0.017(3) 0.003(4)

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.06335(4)
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 . O1 5_775 2.145(5) yes
Co1 . O3 3_576 2.089(5) yes
Co1 . O6 3_576 2.068(8) yes
Co1 . O3 5_775 2.058(7) yes
Co1 . Co1 5_775 3.000(3) yes
Co1 . Co1 3_576 3.2316(19) yes
Co1 . Co1 7_756 3.2316(19) yes
Co1 . O3 . 2.195(7) yes
Co1 . O4 . 2.062(7) yes
Co2 . O7 15_554 1.976(7) yes
Co2 . O7 11_674 1.976(7) yes
Co2 . O2 5_775 1.972(7) yes
Co2 . O2 . 1.972(7) yes
C1 . C2 . 1.517(14) yes
C1 . O1 . 1.272(13) yes
C1 . O2 . 1.274(11) yes
C2 . C3 . 1.571(13) yes
C2 . H21 . 0.980 no
C2 . H22 . 0.961 no
C3 . C4 . 1.540(14) yes
C3 . C6 . 1.544(15) yes
C3 . O3 . 1.415(12) yes
C4 . C5 . 1.500(14) yes
C4 . H41 . 0.959 no
C4 . H42 . 0.955 no
C5 . O6 . 1.232(12) yes
C5 . O7 . 1.293(15) yes
C6 . O4 . 1.248(13) yes
C6 . O5 . 1.221(14) 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
O1 5_775 Co1 . O3 3_576 168.2(3) yes
O1 5_775 Co1 . O6 3_576 86.0(3) yes
O3 3_576 Co1 . O6 3_576 93.5(2) yes
O1 5_775 Co1 . O3 5_775 87.3(2) yes
O3 3_576 Co1 . O3 5_775 81.4(2) yes
O6 3_576 Co1 . O3 5_775 104.7(3) yes
O1 5_775 Co1 . Co1 5_775 85.8(2) yes
O3 3_576 Co1 . Co1 5_775 89.0(2) yes
O6 3_576 Co1 . Co1 5_775 150.9(2) yes
O3 5_775 Co1 . Co1 5_775 47.0(2) yes
O1 5_775 Co1 . Co1 3_576 126.3(2) yes
O3 3_576 Co1 . Co1 3_576 42.3(2) yes
O6 3_576 Co1 . Co1 3_576 101.4(2) yes
O3 5_775 Co1 . Co1 3_576 39.15(14) yes
Co1 5_775 Co1 . Co1 3_576 62.34(2) yes
O1 5_775 Co1 . Co1 7_756 143.6(2) yes
O3 3_576 Co1 . Co1 7_756 38.45(19) yes
O6 3_576 Co1 . Co1 7_756 130.42(17) yes
O3 5_775 Co1 . Co1 7_756 83.39(17) yes
Co1 5_775 Co1 . Co1 7_756 62.34(2) yes
O1 5_775 Co1 . O3 . 104.8(2) yes
O3 3_576 Co1 . O3 . 78.2(2) yes
O6 3_576 Co1 . O3 . 164.5(3) yes
O3 5_775 Co1 . O3 . 87.2(3) yes
Co1 5_775 Co1 . O3 . 43.31(18) yes
O1 5_775 Co1 . O4 . 85.1(3) yes
O3 3_576 Co1 . O4 . 106.7(3) yes
O6 3_576 Co1 . O4 . 93.4(3) yes
O3 5_775 Co1 . O4 . 159.8(3) yes
Co1 5_775 Co1 . O4 . 113.6(2) yes
Co1 3_576 Co1 . Co1 7_756 55.31(4) yes
Co1 3_576 Co1 . O3 . 81.43(16) yes
Co1 7_756 Co1 . O3 . 39.81(13) yes
Co1 3_576 Co1 . O4 . 145.78(18) yes
Co1 7_756 Co1 . O4 . 91.7(2) yes
O3 . Co1 . O4 . 76.8(3) yes
O7 15_554 Co2 . O7 11_674 96.6(5) yes
O7 15_554 Co2 . O2 5_775 103.4(3) yes
O7 11_674 Co2 . O2 5_775 116.3(3) yes
O7 15_554 Co2 . O2 . 116.3(3) yes
O7 11_674 Co2 . O2 . 103.4(3) yes
O2 5_775 Co2 . O2 . 119.1(4) yes
C2 . C1 . O1 . 119.6(8) yes
C2 . C1 . O2 . 118.3(9) yes
O1 . C1 . O2 . 122.1(9) yes
C1 . C2 . C3 . 111.8(9) yes
C1 . C2 . H21 . 108.2 no
C3 . C2 . H21 . 109.7 no
C1 . C2 . H22 . 109.6 no
C3 . C2 . H22 . 107.4 no
H21 . C2 . H22 . 110.1 no
C2 . C3 . C4 . 103.5(8) yes
C2 . C3 . C6 . 109.6(7) yes
C4 . C3 . C6 . 109.8(9) yes
C2 . C3 . O3 . 109.8(8) yes
C4 . C3 . O3 . 112.2(7) yes
C6 . C3 . O3 . 111.6(9) yes
C3 . C4 . C5 . 114.1(9) yes
C3 . C4 . H41 . 106.6 no
C5 . C4 . H41 . 107.7 no
C3 . C4 . H42 . 110.6 no
C5 . C4 . H42 . 109.1 no
H41 . C4 . H42 . 108.5 no
C4 . C5 . O6 . 120.9(11) yes
C4 . C5 . O7 . 117.8(9) yes
O6 . C5 . O7 . 121.3(8) yes
C3 . C6 . O4 . 117.3(9) yes
C3 . C6 . O5 . 115.7(10) yes
O4 . C6 . O5 . 127.0(11) yes
Co1 5_775 O1 . C1 . 120.8(5) yes
Co2 . O2 . C1 . 115.1(7) yes
Co1 . O3 . Co1 7_756 97.9(3) yes
Co1 . O3 . C3 . 111.7(6) yes
Co1 7_756 O3 . C3 . 117.8(5) yes
Co1 . O3 . Co1 5_775 89.7(3) yes
Co1 7_756 O3 . Co1 5_775 102.4(3) yes
C3 . O3 . Co1 5_775 129.7(5) yes
Co1 . O4 . C6 . 119.7(7) yes
Co1 7_756 O6 . C5 . 120.4(7) yes
Co2 12_664 O7 . C5 . 126.4(6) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 21/07/14 at 12:05:48
#
#LIST     12                                                                    
BLOCK 
CONT SCALE 
CONT CO   (    1 ,X'S,U'S)  UNTIL O    (    7 ) 
CONT O    (    8 ,X'S,U[ISO]) 
CONT O    (    9 ,X'S,OCC)  UNTIL O    (   10 ) 
EQUIV O(9,OCC) O(10,OCC) 
WEIGHT -1 O(10,OCC) 
CONT ENANTIO 
RIDE C   (   2,X'S) H   (  21,X'S) H   (  22,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) H   (  42,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 21/07/14 at 12:05:48
#
#LIST     16                                                                    
NO 
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 C(2) 
VIBR .0, 0.00200 = C(1) TO O(1) 
VIBR .0, 0.00200 = C(1) TO O(2) 
VIBR .0, 0.00500 = O(1) TO C(2) 
VIBR .0, 0.00500 = O(2) TO C(2) 
VIBR .0, 0.00500 = O(2) TO O(1) 
VIBR .0, 0.00200 = C(2) TO C(3) 
VIBR .0, 0.00500 = C(3) TO C(1) 
VIBR .0, 0.00200 = C(3) TO C(4) 
VIBR .0, 0.00200 = C(3) TO C(6) 
VIBR .0, 0.00200 = C(3) TO O(3) 
VIBR .0, 0.00500 = C(4) TO C(2) 
VIBR .0, 0.00500 = C(6) TO C(2) 
VIBR .0, 0.00500 = C(6) TO C(4) 
VIBR .0, 0.00500 = O(3) TO C(2) 
VIBR .0, 0.00500 = O(3) TO C(4) 
VIBR .0, 0.00500 = O(3) TO C(6) 
VIBR .0, 0.00200 = C(4) TO C(5) 
VIBR .0, 0.00500 = C(5) TO C(3) 
VIBR .0, 0.00200 = C(5) TO O(6) 
VIBR .0, 0.00200 = C(5) TO O(7) 
VIBR .0, 0.00500 = O(6) TO C(4) 
VIBR .0, 0.00500 = O(7) TO C(4) 
VIBR .0, 0.00500 = O(7) TO O(6) 
VIBR .0, 0.00200 = C(6) TO O(4) 
VIBR .0, 0.00200 = C(6) TO O(5) 
VIBR .0, 0.00500 = O(4) TO C(3) 
VIBR .0, 0.00500 = O(5) TO C(3) 
VIBR .0, 0.00500 = O(5) TO O(4) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = C(1) TO C(2) 
U(IJ) .0, 0.08000 = C(1) TO O(1) 
U(IJ) .0, 0.08000 = C(1) TO O(2) 
U(IJ) .0, 0.04000 = C(2) TO C(3) 
U(IJ) .0, 0.04000 = C(3) TO C(4) 
U(IJ) .0, 0.04000 = C(3) TO C(6) 
U(IJ) .0, 0.08000 = C(3) TO O(3) 
U(IJ) .0, 0.04000 = C(4) TO C(5) 
U(IJ) .0, 0.08000 = C(5) TO O(6) 
U(IJ) .0, 0.08000 = C(5) TO O(7) 
U(IJ) .0, 0.08000 = C(6) TO O(4) 
U(IJ) .0, 0.08000 = C(6) TO O(5) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_sp3067_5kbar
_database_code_depnum_ccdc_archive 'CCDC 1447806'
_audit_update_record             
;
2016-05-13 deposited with the CCDC.
2016-05-13 downloaded from the CCDC.
;


_audit_creation_date             14-07-21
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 'UTSA16 in I-42d at 0.3 GPa'
_chemical_name_systematic        'potassium cobalt (II) citrate, UTSA-16'

_exptl_special_details           
; 
Sample was placed in a Merrill-Basset DAC with Fluorinert FC70 at a pressure
of 0.5(1) GPa 
;
_refine_special_details          
; 
Main residue atoms could be anisotropically refined, however pore water atoms
were isotropically refined.
;


#CheckCIF responses

#   PLAT027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............      18.53 Degree
#   PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low .......      0.772 Note 
#   PLAT341_ALERT_3_B Low Bond Precision on  C-C Bonds ...............     0.0172 Ang.
#   PLAT090_ALERT_3_C Poor Data / Parameter Ratio (Zmax > 18) ........       7.75 Note 
#   REFNR01_ALERT_3_C  Ratio of reflections to parameters is < 10 for a
#               non-centrosymmetric structure, where ZMAX > 18
#               sine(theta)/lambda                0.5881
#               Proportion of unique data used    0.8825
#               Ratio reflections to parameters   8.6818 
#    - The high pressure cell causes shading of a significant proportion of the
#   sphere of reflections. This means that the completeness is reduced and as
#   such the quality of the model is lower.  
#   
#   PLAT601_ALERT_2_A Structure Contains Solvent Accessible VOIDS of .        916 Ang3  
#   PLAT004_ALERT_5_G Polymeric Structure Found with Dimension .......          3 Info 
#    - The structure is a porous metal-organic framework containing mobile disordered
#   solvent. 
#     
#   PLAT940_ALERT_3_B F**2 Refinement with I < n * Sigma(I) only .....     Please Check
#    - The lower data quality forced the usage of an I/sig(I) cut off of 3.0 to
#   be used.
#   
#   PLAT202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent .........          1       
#   PLAT220_ALERT_2_C Large Non-Solvent  O     Ueq(max)/Ueq(min) Range        5.9 Ratio 
#   PLAT301_ALERT_3_G Main Residue  Disorder ............ Percentage =          6 Note  
#   PLAT302_ALERT_4_G Anion/Solvent Disorder ............ Percentage =        100 Note  
#   PLAT311_ALERT_2_G Isolated Disordered Oxygen Atom (No H's ?) .....        O91 Check 
#   PLAT311_ALERT_2_G Isolated Disordered Oxygen Atom (No H's ?) .....        O90 Check
#    - The 'main' and 'solvent' residues as termed by CheckCIF do not follow
#   our analysis. The large 'non-solvent' oxygen atom is a solvent water 
#   molecule which is isotropically refined. Oxygen atoms O90 and O91 are pore 
#   water molecules
#   
#   PLAT199_ALERT_1_G Reported _cell_measurement_temperature ..... (K)        293 Check 
#   PLAT200_ALERT_1_G Reported   _diffrn_ambient_temperature ..... (K)        293 Check 
#    - Correct
#
#   PLAT860_ALERT_3_G Number of Least-Squares Restraints .............        101 Note  
#   - Low data quality due to the high-pressure cell requires numerous restraints
#   on the citrate moiety to give stable refinements.
#   PLAT780_ALERT_1_G Coordinates do not Form a Properly Connected Set     Please Do ! 
#    - No action taken
#   PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd.  #          2 Note  
#                 O                                                                 
#   PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd.  #          3 Note  
#                 O      
#    - No action taken, not part of the main residue      
#                                                    
#   PLAT792_ALERT_1_G The Model has Chirality at C3      .............          S Verify
#    - Correct
#   PLAT794_ALERT_5_G Tentative Bond Valency for Co2     (III)   .....       1.59 Note  
#    - Correct
#   PLAT808_ALERT_5_G No Parseable SHELXL Style Weighting Scheme Found     Please Check
#    - CheckCIF bug, weighting scheme is given under _refine_ls_weighting_details 



_cell_length_a                   12.8201(5)
_cell_length_b                   12.8201(5)
_cell_length_c                   30.2685(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4974.8(3)

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I -4 2 d '
_symmetry_space_group_name_Hall  'I -4 2bw'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,y+1/2,z+1/2
y,-x,-z
y+1/2,-x+1/2,-z+1/2
-x,-y,z
-x+1/2,-y+1/2,z+1/2
-y,x,-z
-y+1/2,x+1/2,-z+1/2
-x+1/2,y,-z+3/4
-x+1,y+1/2,-z+5/4
-y+1/2,-x,z+3/4
-y+1,-x+1/2,z+5/4
x+1/2,-y,-z+3/4
x+1,-y+1/2,-z+5/4
y+1/2,x,z+3/4
y+1,x+1/2,z+5/4

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'
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'
K 0.2009 0.2494 8.2186 12.7949 7.4398 0.7748 1.0519 213.1870 0.8659 41.6841
1.4228 '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            8

# Given Formula = C12 H12 Co3 K2 O16 
# Dc =      1.78 Fooo =   2592.00 Mu =     23.79 M =    333.61
# Found Formula = C12 H8 Co3 K1 O18 
# Dc =      1.75 FOOO =   2592.00 Mu =     22.20 M =    328.04

_chemical_formula_sum            'C12 H8 Co3 K1 O18'
_chemical_formula_moiety         'C12 H8 Co3 K1 O14,O4'
_chemical_compound_source        ?
_chemical_formula_weight         656.08


_cell_measurement_reflns_used    4072
_cell_measurement_theta_min      4
_cell_measurement_theta_max      25
_cell_measurement_temperature    293

_exptl_crystal_description       octahedron
_exptl_crystal_colour            purple
_exptl_crystal_size_min          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.450

_exptl_crystal_density_diffrn    1.752
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2592.000
_exptl_absorpt_coefficient_mu    2.220

# Sheldrick geometric approximatio 0.72 0.72 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.46
_exptl_absorpt_correction_T_max  0.72
_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_ambient_pressure         0.5 #GPa
_diffrn_reflns_number            7130
_reflns_number_total             1515
_diffrn_reflns_av_R_equivalents  0.050
# Number of reflections without Friedels Law is 1515 
# Number of reflections with Friedels Law is 863 
# Theoretical number of reflections is about 1060 


_diffrn_reflns_theta_min         3.722
_diffrn_reflns_theta_max         24.707
_diffrn_measured_fraction_theta_max 0.722

_diffrn_reflns_theta_full        18.530
_diffrn_measured_fraction_theta_full 0.772


_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_reflns_limit_h_min              -7
_reflns_limit_h_max              7
_reflns_limit_k_min              0
_reflns_limit_k_max              13
_reflns_limit_l_min              0
_reflns_limit_l_max              34

_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         -0.77
_refine_diff_density_max         1.39


# 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>3.0\s(I)
_refine_ls_number_reflns         1260
_refine_ls_number_restraints     101
_refine_ls_number_parameters     154
_oxford_refine_ls_R_factor_ref   0.0643
_refine_ls_wR_factor_ref         0.1690
_refine_ls_goodness_of_fit_ref   1.0214
_refine_ls_shift/su_max          0.0007885
_refine_ls_shift/su_mean         0.0000526


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        1514
_refine_ls_R_factor_all          0.0910
_refine_ls_wR_factor_all         0.2657

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                1337
_refine_ls_R_factor_gt           0.0672
_refine_ls_wR_factor_gt          0.1806

_refine_ls_abs_structure_Flack   0.08(5)
_refine_ls_abs_structure_details 'Flack (1983), 652 Friedel-pairs'
# 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 ad


_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, 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: 
 9.73 13.0 5.40 
;

# 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 0.89500(12) 0.94950(12) 0.45963(4) 0.0200 1.0000 Uani . . . . . .
Co2 Co 1.0000 1.0000 0.30855(5) 0.0285 1.0000 Uani S T . . . .
K1 K 0.7500 0.8314(4) 0.3750 0.0419 1.0000 Uani S T . . . .
C1 C 1.1071(8) 0.9156(10) 0.3782(3) 0.0204 1.0000 Uani . U . . . .
C2 C 1.1503(11) 0.8340(10) 0.4087(3) 0.0272 1.0000 Uani . U . . . .
C3 C 1.0813(10) 0.8072(9) 0.4490(3) 0.0259 1.0000 Uani . U . . . .
C4 C 1.1463(10) 0.7320(9) 0.4765(3) 0.0254 1.0000 Uani . U . . . .
C5 C 1.0853(9) 0.6805(9) 0.5135(3) 0.0194 1.0000 Uani . U . . . .
C6 C 0.9807(11) 0.7511(10) 0.4330(3) 0.0297 1.0000 Uani . U . . . .
O1 O 1.1110(6) 1.0101(6) 0.39072(18) 0.0221 1.0000 Uani . U . . . .
O2 O 1.0711(7) 0.8886(7) 0.3417(2) 0.0323 1.0000 Uani . U . . . .
O3 O 1.0558(6) 0.9002(6) 0.47109(18) 0.0224 1.0000 Uani . U . . . .
O4 O 0.8948(7) 0.7971(7) 0.4382(2) 0.0260 1.0000 Uani . U . . . .
O5 O 0.9919(9) 0.6659(8) 0.4155(3) 0.0489 1.0000 Uani . U . . . .
O6 O 1.0396(7) 0.7345(6) 0.5421(2) 0.0327 1.0000 Uani . U . . . .
O7 O 1.0821(8) 0.5813(6) 0.5148(2) 0.0364 1.0000 Uani . U . . . .
O90 O 1.156(3) 0.475(3) 0.4390(10) 0.067(9) 0.3639 Uiso . . . . . .
O91 O 1.184(2) 0.439(3) 0.4602(10) 0.125(10) 0.6361 Uiso . . . . . .
H21 H 1.2158 0.8580 0.4193 0.0364 1.0000 Uiso R . . . . .
H22 H 1.1602 0.7720 0.3920 0.0364 1.0000 Uiso R . . . . .
H41 H 1.2020 0.7705 0.4893 0.0339 1.0000 Uiso R . . . . .
H42 H 1.1738 0.6793 0.4578 0.0339 1.0000 Uiso R . . . . .
O80 O 1.292(3) 0.603(4) 0.5762(12) 0.109(12) 0.5000 Uiso . . . . . .
O81 O 1.338(4) 0.648(4) 0.5840(13) 0.138(16) 0.5000 Uiso . . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0210(9) 0.0228(9) 0.0162(6) -0.0003(5) 0.0001(5) 0.0002(9)
Co2 0.0256(14) 0.0426(15) 0.0174(10) 0.0000 0.0000 -0.0037(14)
K1 0.044(3) 0.043(3) 0.0383(18) 0.0000 -0.0194(17) 0.0000
C1 0.008(6) 0.027(4) 0.027(3) 0.003(3) 0.001(3) -0.005(5)
C2 0.033(6) 0.024(5) 0.024(4) 0.002(3) 0.001(3) -0.001(5)
C3 0.026(5) 0.023(5) 0.029(4) 0.001(2) 0.001(3) -0.001(4)
C4 0.036(6) 0.020(5) 0.020(4) 0.001(3) 0.000(3) -0.004(4)
C5 0.016(7) 0.013(3) 0.029(4) 0.003(3) -0.001(3) 0.002(5)
C6 0.031(4) 0.024(5) 0.034(5) -0.003(4) -0.003(3) -0.002(3)
O1 0.020(4) 0.026(3) 0.020(3) 0.006(2) 0.004(3) -0.002(5)
O2 0.048(6) 0.029(5) 0.020(3) -0.002(3) 0.000(3) 0.004(5)
O3 0.034(5) 0.023(4) 0.010(3) 0.004(2) -0.001(3) -0.004(4)
O4 0.027(4) 0.028(5) 0.023(3) -0.004(3) -0.005(3) -0.005(4)
O5 0.036(6) 0.032(5) 0.080(6) -0.021(4) 0.001(5) -0.001(5)
O6 0.049(6) 0.022(4) 0.027(3) -0.003(3) 0.007(3) 0.002(5)
O7 0.056(6) 0.013(3) 0.040(4) 0.001(3) 0.013(4) -0.003(4)

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.06067(4)
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 . O1 5_775 2.150(6) yes
Co1 . O3 3_576 2.099(5) yes
Co1 . O6 3_576 2.063(8) yes
Co1 . O3 5_775 2.057(7) yes
Co1 . Co1 5_775 2.987(3) yes
Co1 . Co1 7_756 3.230(2) yes
Co1 . Co1 3_576 3.230(2) yes
Co1 . O3 . 2.184(8) yes
Co1 . O4 . 2.058(9) yes
Co2 . O7 11_674 1.988(8) yes
Co2 . O7 15_554 1.988(8) yes
Co2 . O2 5_775 1.970(8) yes
Co2 . O2 . 1.970(8) yes
C1 . C2 . 1.501(15) yes
C1 . O1 . 1.271(15) yes
C1 . O2 . 1.244(13) yes
C2 . C3 . 1.547(14) yes
C2 . H21 . 0.950 no
C2 . H22 . 0.950 no
C3 . C4 . 1.521(16) yes
C3 . C6 . 1.554(17) yes
C3 . O3 . 1.406(13) yes
C4 . C5 . 1.517(15) yes
C4 . H41 . 0.950 no
C4 . H42 . 0.950 no
C5 . O6 . 1.253(13) yes
C5 . O7 . 1.273(15) yes
C6 . O4 . 1.260(16) yes
C6 . O5 . 1.223(16) 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
O1 5_775 Co1 . O3 3_576 167.9(3) yes
O1 5_775 Co1 . O6 3_576 85.6(3) yes
O3 3_576 Co1 . O6 3_576 93.4(3) yes
O1 5_775 Co1 . O3 5_775 87.1(3) yes
O3 3_576 Co1 . O3 5_775 81.5(3) yes
O6 3_576 Co1 . O3 5_775 104.3(4) yes
O1 5_775 Co1 . Co1 5_775 85.9(2) yes
O3 3_576 Co1 . Co1 5_775 89.2(2) yes
O6 3_576 Co1 . Co1 5_775 150.4(3) yes
O3 5_775 Co1 . Co1 5_775 47.0(2) yes
O1 5_775 Co1 . Co1 7_756 143.9(2) yes
O3 3_576 Co1 . Co1 7_756 38.5(2) yes
O6 3_576 Co1 . Co1 7_756 130.47(19) yes
O3 5_775 Co1 . Co1 7_756 83.43(19) yes
Co1 5_775 Co1 . Co1 7_756 62.46(2) yes
O1 5_775 Co1 . Co1 3_576 126.4(2) yes
O3 3_576 Co1 . Co1 3_576 42.0(2) yes
O6 3_576 Co1 . Co1 3_576 101.1(2) yes
O3 5_775 Co1 . Co1 3_576 39.46(16) yes
Co1 5_775 Co1 . Co1 3_576 62.46(2) yes
O1 5_775 Co1 . O3 . 104.9(3) yes
O3 3_576 Co1 . O3 . 78.6(3) yes
O6 3_576 Co1 . O3 . 164.8(3) yes
O3 5_775 Co1 . O3 . 87.4(3) yes
Co1 5_775 Co1 . O3 . 43.51(19) yes
O1 5_775 Co1 . O4 . 85.6(3) yes
O3 3_576 Co1 . O4 . 106.5(3) yes
O6 3_576 Co1 . O4 . 93.1(4) yes
O3 5_775 Co1 . O4 . 160.5(4) yes
Co1 5_775 Co1 . O4 . 114.4(3) yes
Co1 7_756 Co1 . Co1 3_576 55.08(5) yes
Co1 7_756 Co1 . O3 . 40.06(14) yes
Co1 3_576 Co1 . O3 . 81.61(18) yes
Co1 7_756 Co1 . O4 . 91.9(2) yes
Co1 3_576 Co1 . O4 . 145.5(2) yes
O3 . Co1 . O4 . 77.1(3) yes
O7 11_674 Co2 . O7 15_554 96.3(5) yes
O7 11_674 Co2 . O2 5_775 118.8(4) yes
O7 15_554 Co2 . O2 5_775 101.5(4) yes
O7 11_674 Co2 . O2 . 101.5(4) yes
O7 15_554 Co2 . O2 . 118.8(4) yes
O2 5_775 Co2 . O2 . 118.7(4) yes
C2 . C1 . O1 . 117.7(9) yes
C2 . C1 . O2 . 119.2(11) yes
O1 . C1 . O2 . 123.0(10) yes
C1 . C2 . C3 . 115.5(10) yes
C1 . C2 . H21 . 108.0 no
C3 . C2 . H21 . 108.0 no
C1 . C2 . H22 . 107.8 no
C3 . C2 . H22 . 108.0 no
H21 . C2 . H22 . 109.5 no
C2 . C3 . C4 . 105.0(9) yes
C2 . C3 . C6 . 109.3(8) yes
C4 . C3 . C6 . 109.4(10) yes
C2 . C3 . O3 . 108.6(9) yes
C4 . C3 . O3 . 113.9(8) yes
C6 . C3 . O3 . 110.3(10) yes
C3 . C4 . C5 . 113.4(10) yes
C3 . C4 . H41 . 107.8 no
C5 . C4 . H41 . 108.3 no
C3 . C4 . H42 . 109.1 no
C5 . C4 . H42 . 108.8 no
H41 . C4 . H42 . 109.5 no
C4 . C5 . O6 . 120.6(11) yes
C4 . C5 . O7 . 118.3(10) yes
O6 . C5 . O7 . 121.1(9) yes
C3 . C6 . O4 . 118.1(11) yes
C3 . C6 . O5 . 116.8(12) yes
O4 . C6 . O5 . 125.1(13) yes
Co1 5_775 O1 . C1 . 121.2(6) yes
Co2 . O2 . C1 . 114.9(8) yes
Co1 . O3 . Co1 7_756 97.9(3) yes
Co1 . O3 . Co1 5_775 89.5(3) yes
Co1 7_756 O3 . Co1 5_775 102.0(3) yes
Co1 . O3 . C3 . 113.0(7) yes
Co1 7_756 O3 . C3 . 117.1(5) yes
Co1 5_775 O3 . C3 . 130.0(6) yes
Co1 . O4 . C6 . 118.8(8) yes
Co1 7_756 O6 . C5 . 120.2(7) yes
Co2 12_664 O7 . C5 . 124.1(7) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 21/07/14 at 13:00:46
#
#LIST     12                                                                    
BLOCK 
CONT SCALE 
CONT CO   (    1 ,X'S,U'S)  UNTIL O    (    7 ) 
CONT O    (   90 ,X'S,U[ISO])  UNTIL O    (   91 ) 
CONT O    (   80 ,X'S,U[ISO])  UNTIL O    (   81 ) 
CONT ENANTIO 
RIDE C   (   2,X'S) H   (  21,X'S) H   (  22,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) H   (  42,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 21/07/14 at 13:00:46
#
#LIST     16                                                                    
NO 
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 C(2) 
VIBR .0, 0.00200 = C(1) TO O(1) 
VIBR .0, 0.00200 = C(1) TO O(2) 
VIBR .0, 0.00500 = O(1) TO C(2) 
VIBR .0, 0.00500 = O(2) TO C(2) 
VIBR .0, 0.00500 = O(2) TO O(1) 
VIBR .0, 0.00200 = C(2) TO C(3) 
VIBR .0, 0.00500 = C(3) TO C(1) 
VIBR .0, 0.00200 = C(3) TO C(4) 
VIBR .0, 0.00200 = C(3) TO C(6) 
VIBR .0, 0.00200 = C(3) TO O(3) 
VIBR .0, 0.00500 = C(4) TO C(2) 
VIBR .0, 0.00500 = C(6) TO C(2) 
VIBR .0, 0.00500 = C(6) TO C(4) 
VIBR .0, 0.00500 = O(3) TO C(2) 
VIBR .0, 0.00500 = O(3) TO C(4) 
VIBR .0, 0.00500 = O(3) TO C(6) 
VIBR .0, 0.00200 = C(4) TO C(5) 
VIBR .0, 0.00500 = C(5) TO C(3) 
VIBR .0, 0.00200 = C(5) TO O(6) 
VIBR .0, 0.00200 = C(5) TO O(7) 
VIBR .0, 0.00500 = O(6) TO C(4) 
VIBR .0, 0.00500 = O(7) TO C(4) 
VIBR .0, 0.00500 = O(7) TO O(6) 
VIBR .0, 0.00200 = C(6) TO O(4) 
VIBR .0, 0.00200 = C(6) TO O(5) 
VIBR .0, 0.00500 = O(4) TO C(3) 
VIBR .0, 0.00500 = O(5) TO C(3) 
VIBR .0, 0.00500 = O(5) TO O(4) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = C(1) TO C(2) 
U(IJ) .0, 0.08000 = C(1) TO O(1) 
U(IJ) .0, 0.08000 = C(1) TO O(2) 
U(IJ) .0, 0.04000 = C(2) TO C(3) 
U(IJ) .0, 0.04000 = C(3) TO C(4) 
U(IJ) .0, 0.04000 = C(3) TO C(6) 
U(IJ) .0, 0.08000 = C(3) TO O(3) 
U(IJ) .0, 0.04000 = C(4) TO C(5) 
U(IJ) .0, 0.08000 = C(5) TO O(6) 
U(IJ) .0, 0.08000 = C(5) TO O(7) 
U(IJ) .0, 0.08000 = C(6) TO O(4) 
U(IJ) .0, 0.08000 = C(6) TO O(5) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_SP3070_10kbar
_database_code_depnum_ccdc_archive 'CCDC 1447807'
_audit_update_record             
;
2016-05-13 deposited with the CCDC.
2016-05-13 downloaded from the CCDC.
;

_audit_creation_date             14-07-21
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 'UTSA16 in I-42d at 1.0 GPa'
_chemical_name_systematic        'potassium cobalt (II) citrate, UTSA-16'

_exptl_special_details           
; 
Sample was placed in a Merrill-Basset DAC with Fluorinert FC70 at a pressure
of 1.0(1) GPa  
;
_refine_special_details          
; 
Main residue atoms could be anisotropically refined, however pore water atoms
were isotropically refined.
;

#CheckCIF Responses

# PLAT027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............      18.27 Degree
# PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low .......      0.772 Note 
# REFNR01_ALERT_3_B  Ratio of reflections to parameters is < 8 for a
#             non-centrosymmetric structure, where ZMAX > 18
#             sine(theta)/lambda                0.5805
#             Proportion of unique data used    0.8268
#             Ratio reflections to parameters   7.5000
# PLAT341_ALERT_3_B Low Bond Precision on  C-C Bonds ...............     0.0196 Ang.
# PLAT090_ALERT_3_C Poor Data / Parameter Ratio (Zmax > 18) ........       7.25 Note    
#   - The high pressure cell causes shading of a significant proportion of the
#  sphere of reflections. This means that the completeness is reduced and as
#  such the quality of the model is lower. 
# 
# 
#  
# PLAT601_ALERT_2_A Structure Contains Solvent Accessible VOIDS of .        862 Ang3 
# PLAT004_ALERT_5_G Polymeric Structure Found with Dimension .......          3 Info  
#  - The structure is a porous metal-organic framework containing mobile disordered
# solvent.
#  
# DIFMX01_ALERT_2_C  The maximum difference density is > 0.1*ZMAX*0.75
#             _refine_diff_density_max given =      2.240
#             Test value =      2.025
# DIFMX02_ALERT_1_C  The maximum difference density is > 0.1*ZMAX*0.75
#             The relevant atom site should be identified.
# PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       3.11 Why ? 
# PLAT097_ALERT_2_C Large Reported Max.  (Positive) Residual Density       2.24 eA-3  
#  - We believe the pore contents to contain further highly disorder water and
# potassium species and so some residual density is to be expected. 
# 
# PLAT199_ALERT_1_G Reported _cell_measurement_temperature ..... (K)        293 Check 
# PLAT200_ALERT_1_G Reported   _diffrn_ambient_temperature ..... (K)        293 Check 
#  - Correct
# 
# PLAT202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent .........          1       
# PLAT213_ALERT_2_C Atom O4              has ADP max/min Ratio .....        3.8 prolat
# PLAT220_ALERT_2_C Large Non-Solvent  O     Ueq(max)/Ueq(min) Range        5.7 Ratio 
# PLAT003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...         13 Why ?
# PLAT301_ALERT_3_G Main Residue  Disorder ............ Percentage =          6 Note  
# PLAT302_ALERT_4_G Anion/Solvent Disorder ............ Percentage =        100 Note  
# PLAT311_ALERT_2_G Isolated Disordered Oxygen Atom (No H's ?) .....        O10 Check 
# PLAT311_ALERT_2_G Isolated Disordered Oxygen Atom (No H's ?) .....         O9 Check
#  - The 'main' and 'solvent' residues as termed by CheckCIF do not follow
# our analysis. The large 'non-solvent' oxygen atom is a solvent water 
# molecule which is isotropically refined. Oxygen atoms O9 and O10 are pore 
# water molecules
# 
# 
# PLAT780_ALERT_1_G Coordinates do not Form a Properly Connected Set     Please Do ! 
# PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd.  #          2 Note  
#               O                                                                 
# PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd.  #          3 Note  
#               O  
#  - No action taken, atoms are not part of the main residue 
#                                                               
# PLAT792_ALERT_1_G The Model has Chirality at C3      .............          S Verify
#  - Correct
# 
# PLAT794_ALERT_5_G Tentative Bond Valency for Co2     (III)   .....       1.61 Note
#  - Correct  
# 
# PLAT808_ALERT_5_G No Parseable SHELXL Style Weighting Scheme Found     Please Check
# - CheckCIF bug, weighting scheme is given under _refine_ls_weighting_details 
# 
# PLAT860_ALERT_3_G Number of Least-Squares Restraints .............        101 Note  
# - Low data quality due to the high-pressure cell requires numerous restraints
# on the citrate moiety to give stable refinements.


_cell_length_a                   12.6111(5)
_cell_length_b                   12.6111(5)
_cell_length_c                   30.2999(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4818.9(3)

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I -4 2 d '
_symmetry_space_group_name_Hall  'I -4 2bw'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,y+1/2,z+1/2
y,-x,-z
y+1/2,-x+1/2,-z+1/2
-x,-y,z
-x+1/2,-y+1/2,z+1/2
-y,x,-z
-y+1/2,x+1/2,-z+1/2
-x+1/2,y,-z+3/4
-x+1,y+1/2,-z+5/4
-y+1/2,-x,z+3/4
-y+1,-x+1/2,z+5/4
x+1/2,-y,-z+3/4
x+1,-y+1/2,-z+5/4
y+1/2,x,z+3/4
y+1,x+1/2,z+5/4

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'
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'
K 0.2009 0.2494 8.2186 12.7949 7.4398 0.7748 1.0519 213.1870 0.8659 41.6841
1.4228 '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            8

# Given Formula = C12 H12 Co3 K2 O16 
# Dc =      1.84 Fooo =   2592.00 Mu =     24.56 M =    333.61
# Found Formula = C12 H8 Co3 K1 O18 
# Dc =      1.81 FOOO =   2592.00 Mu =     22.92 M =    328.04

_chemical_formula_sum            'C12 H8 Co3 K1 O18'
_chemical_formula_moiety         'C12 H8 Co3 K1 O14,O4'
_chemical_formula_weight         656.08


_cell_measurement_reflns_used    3611
_cell_measurement_theta_min      4
_cell_measurement_theta_max      24
_cell_measurement_temperature    293

_exptl_crystal_description       octahedron
_exptl_crystal_colour            purple
_exptl_crystal_size_min          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.450

_exptl_crystal_density_diffrn    1.809
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2592
_exptl_absorpt_coefficient_mu    2.292

# Sheldrick geometric approximatio 0.71 0.71 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.43
_exptl_absorpt_correction_T_max  0.71
_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_ambient_pressure         1.0 #GPa
_diffrn_reflns_number            6416
_reflns_number_total             1397
_diffrn_reflns_av_R_equivalents  0.052
# Number of reflections without Friedels Law is 1397 
# Number of reflections with Friedels Law is 806 
# Theoretical number of reflections is about 984 


_diffrn_reflns_theta_min         3.675
_diffrn_reflns_theta_max         24.365
_diffrn_measured_fraction_theta_max 0.720

_diffrn_reflns_theta_full        18.274
_diffrn_measured_fraction_theta_full 0.772


_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_reflns_limit_h_min              -7
_reflns_limit_h_max              7
_reflns_limit_k_min              0
_reflns_limit_k_max              13
_reflns_limit_l_min              0
_reflns_limit_l_max              34

_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         -0.72
_refine_diff_density_max         2.25


# 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>3.0\s(I)
_refine_ls_number_reflns         1155
_refine_ls_number_restraints     107
_refine_ls_number_parameters     154
_oxford_refine_ls_R_factor_ref   0.0732
_refine_ls_wR_factor_ref         0.1949
_refine_ls_goodness_of_fit_ref   1.0185
_refine_ls_shift/su_max          0.0002910
_refine_ls_shift/su_mean         0.0000276


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        1394
_refine_ls_R_factor_all          0.1068
_refine_ls_wR_factor_all         0.2688

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                1217
_refine_ls_R_factor_gt           0.0774
_refine_ls_wR_factor_gt          0.2027

_refine_ls_abs_structure_Flack   0.13(7)
_refine_ls_abs_structure_details 'Flack (1983), 591 Friedel-pairs'
# 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 ad


_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, 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: 
 23.3 36.9 22.6 8.96 2.58 
;

# 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 0.89434(16) 0.94719(16) 0.45954(5) 0.0204 1.0000 Uani . . . . . .
Co2 Co 1.0000 1.0000 0.30964(7) 0.0280 1.0000 Uani S T . . . .
K1 K 0.7500 0.8275(5) 0.3750 0.0393 1.0000 Uani S T . . . .
C1 C 1.1095(13) 0.9143(12) 0.3788(4) 0.0227 1.0000 Uani . U . . . .
C2 C 1.1575(13) 0.8344(14) 0.4097(4) 0.0277 1.0000 Uani . U . . . .
C3 C 1.0839(12) 0.8048(12) 0.4493(4) 0.0184 1.0000 Uani . U . . . .
C4 C 1.1491(14) 0.7300(13) 0.4775(4) 0.0275 1.0000 Uani . U . . . .
C5 C 1.0915(13) 0.6763(13) 0.5134(4) 0.0210 1.0000 Uani . U . . . .
C6 C 0.9821(14) 0.7477(14) 0.4322(4) 0.0279 1.0000 Uani . U . . . .
O1 O 1.1108(9) 1.0099(9) 0.3911(2) 0.0249 1.0000 Uani . U . . . .
O2 O 1.0722(9) 0.8876(9) 0.3427(3) 0.0265 1.0000 Uani . U . . . .
O3 O 1.0598(9) 0.8979(8) 0.4715(2) 0.0244 1.0000 Uani . U . . . .
O4 O 0.8937(9) 0.7924(9) 0.4383(3) 0.0240 1.0000 Uani . U . . . .
O5 O 0.9944(11) 0.6604(10) 0.4169(4) 0.0494 1.0000 Uani . U . . . .
O6 O 1.0440(10) 0.7341(9) 0.5423(3) 0.0357 1.0000 Uani . U . . . .
O7 O 1.0877(11) 0.5759(9) 0.5153(3) 0.0426 1.0000 Uani . U . . . .
O9 O 1.166(4) 0.461(4) 0.4404(14) 0.074(12) 0.4179 Uiso . . . . . .
O10 O 1.184(3) 0.438(3) 0.4607(11) 0.083(9) 0.5821 Uiso . . . . . .
H21 H 1.2244 0.8578 0.4207 0.0284 1.0000 Uiso R . . . . .
H22 H 1.1654 0.7718 0.3932 0.0278 1.0000 Uiso R . . . . .
H41 H 1.2037 0.7691 0.4906 0.0280 1.0000 Uiso R . . . . .
H42 H 1.1788 0.6775 0.4594 0.0281 1.0000 Uiso R . . . . .
O80 O 1.297(4) 0.605(4) 0.5795(14) 0.103(14) 0.5000 Uiso . . . . . .
O81 O 1.344(5) 0.650(5) 0.5819(16) 0.123(19) 0.5000 Uiso . . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0224(12) 0.0228(12) 0.0159(8) 0.0000(7) 0.0009(7) -0.0010(12)
Co2 0.0230(18) 0.040(2) 0.0207(12) 0.0000 0.0000 -0.0024(19)
K1 0.039(4) 0.038(4) 0.041(2) 0.0000 -0.024(2) 0.0000
C1 0.017(8) 0.031(5) 0.020(4) 0.001(3) 0.009(4) 0.004(7)
C2 0.024(7) 0.037(7) 0.022(4) 0.007(4) 0.008(4) 0.002(6)
C3 0.013(5) 0.022(6) 0.020(5) -0.001(3) 0.003(3) 0.001(4)
C4 0.039(8) 0.022(6) 0.021(5) 0.003(4) -0.007(4) 0.000(5)
C5 0.028(9) 0.014(4) 0.021(5) -0.005(3) -0.007(4) -0.005(6)
C6 0.025(4) 0.035(6) 0.023(5) -0.004(4) -0.003(4) -0.008(4)
O1 0.021(6) 0.029(5) 0.025(4) 0.005(3) -0.001(4) -0.008(7)
O2 0.035(7) 0.026(5) 0.019(4) -0.001(3) 0.007(3) 0.010(6)
O3 0.041(7) 0.021(5) 0.010(3) -0.001(3) -0.001(3) 0.001(5)
O4 0.016(4) 0.036(6) 0.020(4) -0.006(3) -0.004(4) -0.016(5)
O5 0.039(8) 0.044(7) 0.065(7) -0.025(6) -0.019(6) -0.003(6)
O6 0.064(9) 0.024(5) 0.019(4) 0.003(3) -0.001(4) 0.018(7)
O7 0.077(11) 0.013(4) 0.038(5) 0.002(4) 0.010(5) 0.002(7)

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.05963(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Co1 . O1 5_775 2.145(8) yes
Co1 . O3 3_576 2.093(7) yes
Co1 . O3 5_775 2.069(10) yes
Co1 . Co1 5_775 2.979(4) yes
Co1 . O6 3_576 2.025(11) yes
Co1 . Co1 7_756 3.233(3) yes
Co1 . Co1 3_576 3.233(3) yes
Co1 . O3 . 2.207(11) yes
Co1 . O4 . 2.056(11) yes
Co2 . O7 15_554 1.985(11) yes
Co2 . O7 11_674 1.985(11) yes
Co2 . O2 5_775 1.960(10) yes
Co2 . O2 . 1.960(10) yes
C1 . C2 . 1.50(2) yes
C1 . O1 . 1.262(18) yes
C1 . O2 . 1.237(17) yes
C2 . C3 . 1.560(17) yes
C2 . H21 . 0.955 no
C2 . H22 . 0.941 no
C3 . C4 . 1.52(2) yes
C3 . C6 . 1.56(2) yes
C3 . O3 . 1.387(16) yes
C4 . C5 . 1.47(2) yes
C4 . H41 . 0.936 no
C4 . H42 . 0.937 no
C5 . O6 . 1.287(18) yes
C5 . O7 . 1.27(2) yes
C6 . O4 . 1.26(2) yes
C6 . O5 . 1.21(2) 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
O1 5_775 Co1 . O3 3_576 167.8(4) yes
O1 5_775 Co1 . O3 5_775 86.5(4) yes
O3 3_576 Co1 . O3 5_775 81.9(4) yes
O1 5_775 Co1 . Co1 5_775 85.1(3) yes
O3 3_576 Co1 . Co1 5_775 90.0(3) yes
O3 5_775 Co1 . Co1 5_775 47.8(3) yes
O1 5_775 Co1 . O6 3_576 86.0(4) yes
O3 3_576 Co1 . O6 3_576 92.9(4) yes
O3 5_775 Co1 . O6 3_576 103.4(5) yes
Co1 5_775 Co1 . O6 3_576 150.2(4) yes
O1 5_775 Co1 . Co1 7_756 143.5(3) yes
O3 3_576 Co1 . Co1 7_756 38.8(3) yes
O3 5_775 Co1 . Co1 7_756 83.6(2) yes
Co1 5_775 Co1 . Co1 7_756 62.56(3) yes
O6 3_576 Co1 . Co1 7_756 130.5(3) yes
O1 5_775 Co1 . Co1 3_576 125.7(3) yes
O3 3_576 Co1 . Co1 3_576 42.6(3) yes
O3 5_775 Co1 . Co1 3_576 39.3(2) yes
Co1 5_775 Co1 . Co1 3_576 62.56(3) yes
O6 3_576 Co1 . Co1 3_576 101.1(3) yes
O1 5_775 Co1 . O3 . 104.9(3) yes
O3 3_576 Co1 . O3 . 78.7(3) yes
O3 5_775 Co1 . O3 . 88.4(4) yes
Co1 5_775 Co1 . O3 . 44.0(3) yes
O6 3_576 Co1 . O3 . 164.5(4) yes
O1 5_775 Co1 . O4 . 86.3(4) yes
O3 3_576 Co1 . O4 . 105.8(4) yes
O3 5_775 Co1 . O4 . 162.2(4) yes
Co1 5_775 Co1 . O4 . 115.3(3) yes
O6 3_576 Co1 . O4 . 92.3(5) yes
Co1 7_756 Co1 . Co1 3_576 54.88(6) yes
Co1 7_756 Co1 . O3 . 39.93(18) yes
Co1 3_576 Co1 . O3 . 81.7(2) yes
Co1 7_756 Co1 . O4 . 92.5(3) yes
Co1 3_576 Co1 . O4 . 145.6(3) yes
O3 . Co1 . O4 . 77.7(4) yes
O7 15_554 Co2 . O7 11_674 94.9(7) yes
O7 15_554 Co2 . O2 5_775 99.5(5) yes
O7 11_674 Co2 . O2 5_775 121.6(5) yes
O7 15_554 Co2 . O2 . 121.6(5) yes
O7 11_674 Co2 . O2 . 99.5(5) yes
O2 5_775 Co2 . O2 . 118.6(5) yes
C2 . C1 . O1 . 116.7(13) yes
C2 . C1 . O2 . 121.5(14) yes
O1 . C1 . O2 . 121.8(13) yes
C1 . C2 . C3 . 113.6(13) yes
C1 . C2 . H21 . 111.5 no
C3 . C2 . H21 . 109.4 no
C1 . C2 . H22 . 105.8 no
C3 . C2 . H22 . 105.7 no
H21 . C2 . H22 . 110.5 no
C2 . C3 . C4 . 105.0(12) yes
C2 . C3 . C6 . 110.2(10) yes
C4 . C3 . C6 . 110.3(12) yes
C2 . C3 . O3 . 107.5(12) yes
C4 . C3 . O3 . 111.9(10) yes
C6 . C3 . O3 . 111.8(12) yes
C3 . C4 . C5 . 115.8(14) yes
C3 . C4 . H41 . 108.1 no
C5 . C4 . H41 . 106.8 no
C3 . C4 . H42 . 109.1 no
C5 . C4 . H42 . 107.7 no
H41 . C4 . H42 . 109.1 no
C4 . C5 . O6 . 118.1(15) yes
C4 . C5 . O7 . 120.7(13) yes
O6 . C5 . O7 . 121.1(13) yes
C3 . C6 . O4 . 118.2(13) yes
C3 . C6 . O5 . 116.3(16) yes
O4 . C6 . O5 . 125.2(16) yes
Co1 5_775 O1 . C1 . 121.8(8) yes
Co2 . O2 . C1 . 115.5(10) yes
Co1 . O3 . Co1 7_756 97.5(4) yes
Co1 . O3 . Co1 5_775 88.3(4) yes
Co1 7_756 O3 . Co1 5_775 101.9(4) yes
Co1 . O3 . C3 . 111.5(8) yes
Co1 7_756 O3 . C3 . 118.4(7) yes
Co1 5_775 O3 . C3 . 130.8(8) yes
Co1 . O4 . C6 . 117.8(10) yes
Co1 7_756 O6 . C5 . 121.4(10) yes
Co2 12_664 O7 . C5 . 122.2(10) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 21/07/14 at 13:30:22
#
#LIST     12                                                                    
BLOCK 
CONT SCALE 
CONT CO   (    1 ,X'S,U'S)  UNTIL O    (    7 ) 
CONT O    (    9 ,X'S,U[ISO])  UNTIL O    (   10 ) 
CONT O    (   80 ,X'S,U[ISO])  UNTIL O    (   81 ) 
CONT ENANTIO 
RIDE C   (   2,X'S) H   (  21,X'S) H   (  22,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) H   (  42,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 21/07/14 at 13:30:22
#
#LIST     16                                                                    
NO 
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 C(2) 
VIBR .0, 0.00200 = C(1) TO O(1) 
VIBR .0, 0.00200 = C(1) TO O(2) 
VIBR .0, 0.00500 = O(1) TO C(2) 
VIBR .0, 0.00500 = O(2) TO C(2) 
VIBR .0, 0.00500 = O(2) TO O(1) 
VIBR .0, 0.00200 = C(2) TO C(3) 
VIBR .0, 0.00500 = C(3) TO C(1) 
VIBR .0, 0.00200 = C(3) TO C(4) 
VIBR .0, 0.00200 = C(3) TO C(6) 
VIBR .0, 0.00200 = C(3) TO O(3) 
VIBR .0, 0.00500 = C(4) TO C(2) 
VIBR .0, 0.00500 = C(6) TO C(2) 
VIBR .0, 0.00500 = C(6) TO C(4) 
VIBR .0, 0.00500 = O(3) TO C(2) 
VIBR .0, 0.00500 = O(3) TO C(4) 
VIBR .0, 0.00500 = O(3) TO C(6) 
VIBR .0, 0.00200 = C(4) TO C(5) 
VIBR .0, 0.00500 = C(5) TO C(3) 
VIBR .0, 0.00200 = C(5) TO O(6) 
VIBR .0, 0.00200 = C(5) TO O(7) 
VIBR .0, 0.00500 = O(6) TO C(4) 
VIBR .0, 0.00500 = O(7) TO C(4) 
VIBR .0, 0.00500 = O(7) TO O(6) 
VIBR .0, 0.00200 = C(6) TO O(4) 
VIBR .0, 0.00200 = C(6) TO O(5) 
VIBR .0, 0.00500 = O(4) TO C(3) 
VIBR .0, 0.00500 = O(5) TO C(3) 
VIBR .0, 0.00500 = O(5) TO O(4) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = C(1) TO C(2) 
U(IJ) .0, 0.08000 = C(1) TO O(1) 
U(IJ) .0, 0.08000 = C(1) TO O(2) 
U(IJ) .0, 0.04000 = C(2) TO C(3) 
U(IJ) .0, 0.04000 = C(3) TO C(4) 
U(IJ) .0, 0.04000 = C(3) TO C(6) 
U(IJ) .0, 0.08000 = C(3) TO O(3) 
U(IJ) .0, 0.04000 = C(4) TO C(5) 
U(IJ) .0, 0.08000 = C(5) TO O(6) 
U(IJ) .0, 0.08000 = C(5) TO O(7) 
U(IJ) .0, 0.08000 = C(6) TO O(4) 
U(IJ) .0, 0.08000 = C(6) TO O(5) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
U(IJ)'S  0.0, 0.010000 = C(6) TO O(4) 
END                                                                             
;
