# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_Co2dobdc-CO
_database_code_depnum_ccdc_archive 'CCDC 1530122'
_audit_update_record             
;
2017-01-28 deposited with the CCDC.
2017-04-19 downloaded from the CCDC.
;
_audit_creation_date             2016-04-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            Co2(dobdc)(CO)0.58
_chemical_name_systematic        ?
_chemical_formula_moiety         '(Co2 C8 H2 O6) 0.58(C O)'
_chemical_formula_sum            'C8.58 H2 Co2 O6.58'
_chemical_formula_weight         328.20
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3550 1.1300 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0140 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   25.8262(16)
_cell_length_b                   25.8262(16)
_cell_length_c                   6.8315(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3946.1(5)
_cell_formula_units_Z            9
_cell_measurement_reflns_used    9939
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      34.756
_cell_measurement_theta_min      3.400
_shelx_estimated_absorpt_T_max   0.869
_shelx_estimated_absorpt_T_min   0.671
_exptl_absorpt_coefficient_mu    2.410
_exptl_absorpt_correction_T_max  0.869
_exptl_absorpt_correction_T_min  0.674
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1697 before and 0.0589 after correction.
 The Ratio of minimum to maximum transmission not present.
 The λ/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1664 before and 0.0572 after correction.
 The Ratio of minimum to maximum transmission is 0.78.
 The λ/2 correction factor is Not present

Final HKLF 4 output contains 24400 reflections, Rint = 0.0528
 (18579 with I > 3sig(I), Rint = 0.0504)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1441
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_exptl_special_details           
;
Data was collected at Beamline 11.3.1 at the Advanced
 Light Source, Lawrence Berkeley National Laboratory using synchrotron
 radiation (lamda = 0.7749 angstroms) and a Bruker APEX-II CCD detector.

The crystal was mounted on a MiTeGen loop using a minimal amount
 of epoxy to ensure that the crystal pores remained accessible.
 The sample was then placed in a custom-made gas cell equipped
 with a borosilicate glass cap, O-ring seal, and gas loading
 valve.  The cell was evacuated under reduced pressure at
 453 K for 4 hours to remove solvent molecules filling
 the pores and bound onto the exposed Co sites within the crystal.
 After obtaining the structure of the desolvated crystal to
 confirm the absence of solvent bound onto the Co sites, the
 crystal was cooled to 298 K then dosed with 1060 mbar CO.
 The crystal was then cooled to a final temperature of 90 K followed by data collection.  
The crystal was found to be an obverse/reverse twin based on the diffraction
 pattern.  CELL_NOW was used to determine the orientation matrices
 and the domains were related by a 180 deg rotation around the
 reciprocal axis 0 1 1. The integration was preformed with both
 matrices. TWINABS was used to produce a merged HKLF4 file, for
 structure solution and initial refinement, and HKLF5 file for
 final structure refinement. The HKLF5 file contained the merged
 reflections from the second component and those that overlapped with the
 first component were split into two reflections. TWINABS indicated
 the twin faction to be 51:49. The structure was solved using the
 HKLF4 file, but the best refinement was given by the HKLF5 file.  
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            24400
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         34.756
_diffrn_reflns_theta_min         3.400
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω/θ scans'
_diffrn_radiation_monochromator  'channel-cut Si(111) crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2604
_reflns_number_total             2857
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.578
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         2857
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0274
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0328P)²+3.0666P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0718
_refine_special_details          
;Thermal parameters were refined anisotropically for all non-hydrogen atoms. 
Hydrogen atoms were placed in ideal positions and refined using the riding 
model. The chemcial occupancy of CO coordinated to the Co sites was allowed 
to refine freely then was fixed in the final refinement, resulting in a 
chemical occupancy of 29%., Twin
;
_vrf_PLAT602_Co2dobdc-CO         
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info 
RESPONSE: The structure is of a metal-organic framework that exhibits 
one-dimensional hexagonal pores. Solvent molecules within the pores and 
coordinated onto exposed Co sites in the framework were removed by 
heating the crystal under vacuum. The crystal was then dosed with CO to 
characterize the interaction of CO with the exposed Co site. Considering 
that the CO coordinated to Co was found to only have 29% occupancy, it is 
likely that the pores are largely empty or filled with CO in the gas phase.   
;
_vrf_PLAT220_Co2dobdc-CO         
;
PROBLEM: Non-Solvent Resd 1   O   Ueq(max)/Ueq(min) Range        8.8 Ratio 
RESPONSE: This refers to the oxygen atom of CO bound to Co sites in the 
framework. The CO molecule exhibits relatively large displacement 
parameters parallel to the direction of the CO-Co bond because it is weakly 
bound to Co and does not possess any nearby atoms to stabilize the molecule 
into a single orientation.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.510(1) 0.490(1)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Others
 Fixed Sof: O4(0.29) C5(0.29)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.64738(2) 0.02996(2) 0.14363(3) 0.01541(7) Uani 1 1 d . . . . .
O1 O 0.72568(5) 0.08107(5) 0.00555(14) 0.0170(2) Uani 1 1 d . . . . .
O2 O 0.66000(5) -0.03724(5) 0.02813(15) 0.0192(2) Uani 1 1 d . . . . .
O3 O 0.59458(5) 0.03194(5) -0.06839(15) 0.0198(2) Uani 1 1 d . . . . .
O4 O 0.6491(8) 0.1501(6) 0.317(2) 0.149(6) Uani 0.29 1 d . . P . .
C1 C 0.54502(6) -0.01060(7) -0.5775(2) 0.0167(3) Uani 1 1 d . . . . .
C2 C 0.54670(6) 0.00630(7) -0.3787(2) 0.0166(2) Uani 1 1 d . . . . .
C3 C 0.50191(7) 0.01632(7) -0.3072(2) 0.0181(3) Uani 1 1 d . . . . .
H3 H 0.5035 0.0275 -0.1740 0.022 Uiso 1 1 calc R . . . .
C4 C 0.59511(6) 0.01553(7) -0.2413(2) 0.0163(2) Uani 1 1 d . . . . .
C5 C 0.6487(4) 0.1104(3) 0.2632(10) 0.0342(14) Uani 0.29 1 d . . P . .

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 0.01586(10) 0.02058(10) 0.01007(9) 0.00116(6) -0.00003(6) 0.00932(8)
O1 0.0165(5) 0.0176(5) 0.0110(4) -0.0018(3) -0.0013(3) 0.0042(4)
O2 0.0291(5) 0.0180(5) 0.0131(4) 0.0017(4) 0.0046(4) 0.0136(4)
O3 0.0222(5) 0.0315(6) 0.0107(4) -0.0028(4) -0.0026(4) 0.0173(5)
O4 0.189(14) 0.087(8) 0.175(12) -0.011(8) 0.043(11) 0.072(9)
C1 0.0166(6) 0.0218(6) 0.0125(6) 0.0000(5) 0.0006(4) 0.0102(5)
C2 0.0166(6) 0.0228(7) 0.0113(5) -0.0011(5) -0.0006(4) 0.0105(5)
C3 0.0200(6) 0.0260(7) 0.0102(6) -0.0015(5) -0.0006(4) 0.0130(6)
C4 0.0172(6) 0.0202(6) 0.0122(6) 0.0001(5) -0.0009(4) 0.0099(5)
C5 0.051(4) 0.027(3) 0.030(3) -0.008(2) 0.002(3) 0.024(3)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 Co1 2.9803(2) 5_545 ?
Co1 Co1 2.9804(2) 9_654 ?
Co1 O1 2.0129(10) . ?
Co1 O1 1.9967(10) 5_545 ?
Co1 O2 2.0752(11) . ?
Co1 O2 2.0790(11) 5_545 ?
Co1 O3 2.0076(10) . ?
Co1 C5 2.215(6) . ?
O1 Co1 1.9968(10) 9_654 ?
O1 C1 1.3500(17) 9_655 ?
O2 Co1 2.0792(11) 9_654 ?
O2 C4 1.2669(17) 5_545 ?
O3 C4 1.2576(16) . ?
O4 C5 1.084(13) . ?
C1 O1 1.3499(17) 5_544 ?
C1 C2 1.4204(19) . ?
C1 C3 1.3898(19) 10_654 ?
C2 C3 1.394(2) . ?
C2 C4 1.484(2) . ?
C3 C1 1.3898(19) 10_654 ?
C3 H3 0.9500 . ?
C4 O2 1.2671(17) 9_654 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Co1 Co1 Co1 112.067(9) 5_545 9_654 ?
O1 Co1 Co1 42.20(3) 5_545 5_545 ?
O1 Co1 Co1 121.74(3) . 5_545 ?
O1 Co1 Co1 139.46(3) 5_545 9_654 ?
O1 Co1 Co1 41.78(3) . 9_654 ?
O1 Co1 O1 163.16(5) 5_545 . ?
O1 Co1 O2 81.30(4) 5_545 5_545 ?
O1 Co1 O2 81.91(4) . 5_545 ?
O1 Co1 O2 95.63(4) 5_545 . ?
O1 Co1 O2 81.02(4) . . ?
O1 Co1 O3 100.05(4) 5_545 . ?
O1 Co1 C5 90.98(19) 5_545 . ?
O1 Co1 C5 91.0(2) . . ?
O2 Co1 Co1 95.76(3) 5_545 9_654 ?
O2 Co1 Co1 73.49(3) . 5_545 ?
O2 Co1 Co1 44.21(3) . 9_654 ?
O2 Co1 Co1 44.11(3) 5_545 5_545 ?
O2 Co1 O2 82.836(13) . 5_545 ?
O2 Co1 C5 171.3(2) . . ?
O2 Co1 C5 92.7(2) 5_545 . ?
O3 Co1 Co1 137.55(4) . 5_545 ?
O3 Co1 Co1 83.89(3) . 9_654 ?
O3 Co1 O1 96.76(4) . . ?
O3 Co1 O2 98.03(5) . . ?
O3 Co1 O2 178.29(5) . 5_545 ?
O3 Co1 C5 86.3(2) . . ?
C5 Co1 Co1 129.55(19) . 9_654 ?
C5 Co1 Co1 108.31(18) . 5_545 ?
Co1 O1 Co1 96.03(4) 9_654 . ?
C1 O1 Co1 125.58(9) 9_655 9_654 ?
C1 O1 Co1 126.48(9) 9_655 . ?
Co1 O2 Co1 91.69(4) . 9_654 ?
C4 O2 Co1 131.99(10) 5_545 9_654 ?
C4 O2 Co1 134.00(9) 5_545 . ?
C4 O3 Co1 123.17(10) . . ?
O1 C1 C2 124.33(12) 5_544 . ?
O1 C1 C3 117.92(12) 5_544 10_654 ?
C3 C1 C2 117.75(12) 10_654 . ?
C1 C2 C4 123.23(13) . . ?
C3 C2 C1 119.42(13) . . ?
C3 C2 C4 117.34(12) . . ?
C1 C3 C2 122.84(12) 10_654 . ?
C1 C3 H3 118.6 10_654 . ?
C2 C3 H3 118.6 . . ?
O2 C4 C2 117.77(12) 9_654 . ?
O3 C4 O2 122.37(13) . 9_654 ?
O3 C4 C2 119.86(13) . . ?
O4 C5 Co1 178.0(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co1 O3 C4 O2 -13.1(2) . . . 9_654 ?
Co1 O3 C4 C2 167.31(10) . . . . ?
O1 C1 C2 C3 -179.19(14) 5_544 . . . ?
O1 C1 C2 C4 2.4(2) 5_544 . . . ?
C1 C2 C3 C1 -0.1(3) . . . 10_654 ?
C1 C2 C4 O2 -1.4(2) . . . 9_654 ?
C1 C2 C4 O3 178.21(15) . . . . ?
C3 C1 C2 C3 0.1(2) 10_654 . . . ?
C3 C1 C2 C4 -178.34(14) 10_654 . . . ?
C3 C2 C4 O2 -179.82(14) . . . 9_654 ?
C3 C2 C4 O3 -0.2(2) . . . . ?
C4 C2 C3 C1 178.43(14) . . . 10_654 ?

_shelx_res_file                  
;
    twin4.res created by SHELXL-2014/7

TITL twin4 in R-3 #148
REM reset to R-3 #148
CELL 0.7749 25.8262 25.8262 6.8315 90 90 120
ZERR 9 0.0016 0.0016 0.0004 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SFAC C H Co O
DISP C 0.004 0.002 13.872
DISP Co 0.355 1.13 5089.307
DISP H -0 0 0.627
DISP O 0.014 0.007 40.889
UNIT 77.22 18 18 59.22

L.S. 4 0 0
PLAN  20
SIZE 0.06 0.06 0.18
TEMP -183(2)
BOND
fmap 2
MORE -1
BOND $H
CONF
ACTA
REM <olex2.extras>
REM <HklSrc "%./twin5.hkl">
REM </olex2.extras>

WGHT    0.032800    3.066600
BASF   0.49000
FVAR       0.44397
CO1   3    0.647383    0.029965    0.143630    11.00000    0.01586    0.02058 =
         0.01007    0.00116   -0.00003    0.00932
O1    4    0.725679    0.081072    0.005549    11.00000    0.01653    0.01761 =
         0.01103   -0.00184   -0.00133    0.00420
O2    4    0.660000   -0.037236    0.028131    11.00000    0.02912    0.01801 =
         0.01305    0.00174    0.00458    0.01363
O3    4    0.594576    0.031944   -0.068394    11.00000    0.02215    0.03155 =
         0.01071   -0.00284   -0.00260    0.01727
O4    4    0.649098    0.150068    0.316580    10.29000    0.18903    0.08737 =
         0.17456   -0.01071    0.04328    0.07201
C1    1    0.545017   -0.010596   -0.577504    11.00000    0.01657    0.02179 =
         0.01250   -0.00002    0.00055    0.01015
C2    1    0.546702    0.006296   -0.378708    11.00000    0.01663    0.02275 =
         0.01132   -0.00106   -0.00058    0.01051
C3    1    0.501911    0.016320   -0.307224    11.00000    0.02004    0.02595 =
         0.01021   -0.00149   -0.00063    0.01298
AFIX  43
H3    2    0.503532    0.027549   -0.173964    11.00000   -1.20000
AFIX   0
C4    1    0.595109    0.015528   -0.241334    11.00000    0.01725    0.02022 =
         0.01224    0.00005   -0.00092    0.00988
C5    1    0.648748    0.110357    0.263232    10.29000    0.05135    0.02691 =
         0.03039   -0.00781    0.00239    0.02408
HKLF 5

REM  twin4 in R-3 #148
REM R1 =  0.0274 for    2604 Fo > 4sig(Fo)  and  0.0317 for all    2857 data
REM     92 parameters refined using      0 restraints

END

WGHT      0.0328      3.0665

REM Highest difference peak  0.578,  deepest hole -0.391,  1-sigma level  0.073
Q1    1   0.6648  0.0670  0.1243  11.00000  0.05    0.58
Q2    1   0.6405 -0.0005  0.1797  11.00000  0.05    0.45
Q3    1   0.6254  0.0375  0.1753  11.00000  0.05    0.44
Q4    1   0.5242  0.0119 -0.3465  11.00000  0.05    0.44
Q5    1   0.6752  0.0532  0.1873  11.00000  0.05    0.43
Q6    1   0.6522 -0.0624  0.0670  11.00000  0.05    0.36
Q7    1   0.5168 -0.0243 -0.6302  11.00000  0.05    0.36
Q8    1   0.6693  0.0132  0.1111  11.00000  0.05    0.35
Q9    1   0.5668  0.0048 -0.3074  11.00000  0.05    0.33
Q10   1   0.6473 -0.0258  0.0919  11.00000  0.05    0.31
Q11   1   0.7459  0.1159  0.0267  11.00000  0.05    0.31
Q12   1   0.6115  0.0100  0.1110  11.00000  0.05    0.29
Q13   1   0.6972 -0.0278  0.0641  11.00000  0.05    0.28
Q14   1   0.4568 -0.0388 -0.3488  11.00000  0.05    0.28
Q15   1   0.5450  0.0011 -0.4657  11.00000  0.05    0.27
Q16   1   0.6519  0.0348  0.3368  11.00000  0.05    0.26
Q17   1   0.7006  0.0842  0.0395  11.00000  0.05    0.26
Q18   1   0.6160  0.0806  0.2598  11.00000  0.05    0.25
Q19   1   0.6030  0.1223  0.0282  11.00000  0.05    0.25
Q20   1   0.6502  0.0913  0.2256  11.00000  0.05    0.24
;
_shelx_res_checksum              69455
_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.510(1)
2 0.490(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_Co2dobdc-N2
_database_code_depnum_ccdc_archive 'CCDC 1530121'
_audit_update_record             
;
2017-01-28 deposited with the CCDC.
2017-04-19 downloaded from the CCDC.
;
_audit_creation_date             2016-04-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            Co2(dobdc)(N2)3.78
_chemical_name_systematic        ?
_chemical_formula_moiety         '(C8 H2 Co2 O6), 3.78(N2)'
_chemical_formula_sum            'C8 H2 Co2 N7.55 O6'
_chemical_formula_weight         417.72
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0020 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3360 0.7510 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0040 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0080 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   25.810(8)
_cell_length_b                   25.810(8)
_cell_length_c                   6.901(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3981(3)
_cell_formula_units_Z            9
_cell_measurement_reflns_used    2635
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.492
_cell_measurement_theta_min      8.550
_shelx_estimated_absorpt_T_max   0.937
_shelx_estimated_absorpt_T_min   0.880
_exptl_absorpt_coefficient_mu    1.312
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.638
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1960 before and 0.0724 after correction.
 The Ratio of minimum to maximum transmission not present.
 The λ/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1936 before and 0.0735 after correction.
 The Ratio of minimum to maximum transmission is 0.68.
 The λ/2 correction factor is Not present

Final HKLF 4 output contains 18343 reflections, Rint = 0.5196
 (8596 with I > 3sig(I), Rint = 0.5097)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1844
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
Data was collected at Beamline 11.3.1 at the Advanced
 Light Source, Lawrence Berkeley National Laboratory using synchrotron
 radiation (lamda = 0.6199 angstroms) and a Bruker APEX-II CCD detector.

The crystal was mounted on a borosilicate glass fiber using a minimal amount
 of epoxy to ensure that the crystal pores remained accessible.
 The sample was then placed in a 1.0 mm borosilicate glass capillary, which was connected to a Micromeretics ASAP 2020 instrument via a custom-built adapter with an o-ring seal and gas loading
 valve.  The capillary was evacuated under reduced pressure at
 453 K for 24 hours to remove solvent molecules filling
 the pores and bound onto the exposed Co sites within the crystal.
 The capillary was then dosed with 800 mbar N2, then flame sealed.
 The capillary was cooled to 100 K using an Oxford Cryosystems cryostream for data collection.

The crystal was found to be an obverse/reverse twin based on the diffraction
 pattern.  CELL_NOW was used to determine the orientation matrices
 and the domains were related by a 180 deg rotation around the
 real axis 1 0 0. The integration was preformed with both
 matrices. TWINABS was used to produce a merged HKLF4 file, for
 structure solution and initial refinement, and HKLF5 file for
 final structure refinement. The HKLF5 file contained the merged
 reflections from the second component and those that overlapped with the
 first component were split into two reflections. TWINABS indicated
 the twin faction to be 47:53. The structure was solved using the
 HKLF4 file, but the best refinement was given by the HKLF5 file.  
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1089
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            18343
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        21.835
_diffrn_reflns_theta_max         23.733
_diffrn_reflns_theta_min         2.384
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω/θ scans'
_diffrn_radiation_monochromator  'channel-cut Si(111) crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6199
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1753
_reflns_number_total             2040
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.155
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         2040
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0632
_refine_ls_restrained_S_all      1.191
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+50.4354P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1328
_refine_special_details          
;Thermal parameters were refined anisotropically for all non-hydrogen atoms. 
Hydrogen atoms were placed in ideal positions and refined using the riding model.
The chemcial occupancy of N2 in a secondary binding site (N3 and N5) was initially allowed to refine freely, resulting in a chemical occupancy 89%.
Disorder of the N2 molecule in the secondary binding site required displacement parameter restraints. The N-N distances for N2 in the secondary binding sites were also restrained to be 1.098 angstroms., Twin
;
_vrf_PLAT601_Co2dobdc-N2         
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        241 Ang3  
RESPONSE: The structure is of a metal-organic framework that exhibits 
one-dimensional hexagonal pores. Solvent molecules within the pores and 
coordinated onto exposed Co sites in the framework were removed by 
heating the crystal under vacuum. The crystal was then dosed with N2 to 
characterize its interaction with the exposed Co site. It is likely that
the pores are largely empty or filled with N2 in the gas phase.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.467(2) 0.533(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 N3-N4
 1.098 with sigma of 0.02
4. Rigid bond restraints
 N3, N4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
N3 \\sim N4: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
6. Others
 Fixed Sof: N3(0.89) N4(0.89)
7.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.68593(3) 0.05053(3) 0.02140(10) 0.01127(19) Uani 1 1 d . . . . .
O1 O 0.60782(15) 0.02285(16) 0.1627(5) 0.0139(7) Uani 1 1 d . . . . .
O2 O 0.62955(16) -0.00762(16) -0.1921(4) 0.0136(7) Uani 1 1 d . . . . .
O3 O 0.74005(16) 0.10311(15) 0.2381(5) 0.0144(7) Uani 1 1 d . . . . .
N1 N 0.6889(3) 0.1339(3) -0.0842(8) 0.0392(14) Uani 1 1 d . . . . .
N2 N 0.6949(7) 0.1775(5) -0.1134(18) 0.111(4) Uani 1 1 d . . . . .
C1 C 0.5558(2) 0.0108(2) 0.0776(7) 0.0153(10) Uani 1 1 d . . . . .
C2 C 0.5413(2) -0.0048(2) -0.1200(7) 0.0162(10) Uani 1 1 d . . . . .
C3 C 0.4867(2) -0.0148(2) -0.1916(7) 0.0151(10) Uani 1 1 d . . . . .
H3 H 0.4779 -0.0248 -0.3246 0.018 Uiso 1 1 calc R . . . .
C4 C 0.5804(2) -0.0142(2) -0.2563(7) 0.0133(10) Uani 1 1 d . . . . .
N3 N 0.3715(13) -0.1332(9) -0.488(3) 0.157(9) Uani 0.89 1 d D U P . .
N4 N 0.3627(13) -0.1572(8) -0.361(3) 0.160(8) Uani 0.89 1 d D U P . .

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 0.0123(3) 0.0138(4) 0.0063(3) -0.0004(2) 0.0000(2) 0.0054(3)
O1 0.0113(17) 0.0221(19) 0.0080(15) 0.0013(14) -0.0017(13) 0.0081(15)
O2 0.0162(18) 0.0192(17) 0.0054(15) -0.0035(12) -0.0016(13) 0.0087(15)
O3 0.0162(17) 0.0123(17) 0.0083(16) 0.0009(13) -0.0017(13) 0.0023(14)
N1 0.057(4) 0.041(4) 0.032(3) 0.011(3) 0.005(3) 0.035(3)
N2 0.165(12) 0.083(8) 0.104(8) 0.019(6) -0.006(8) 0.076(9)
C1 0.017(2) 0.019(2) 0.012(2) 0.0000(19) -0.0004(19) 0.010(2)
C2 0.018(2) 0.021(3) 0.011(2) -0.003(2) -0.003(2) 0.010(2)
C3 0.021(3) 0.015(2) 0.009(2) -0.0018(18) -0.0024(19) 0.008(2)
C4 0.015(2) 0.015(2) 0.009(2) 0.0003(18) 0.0019(18) 0.007(2)
N3 0.23(2) 0.110(15) 0.115(14) -0.056(11) -0.078(17) 0.079(16)
N4 0.22(2) 0.093(13) 0.143(17) -0.034(12) -0.024(19) 0.057(14)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 2.013(3) 9_654 ?
Co1 O1 2.021(3) . ?
Co1 O2 2.103(4) 5_545 ?
Co1 O2 2.087(3) . ?
Co1 O3 2.033(3) . ?
Co1 N1 2.236(6) . ?
O1 Co1 2.013(3) 5_545 ?
O1 C1 1.352(6) . ?
O2 Co1 2.103(4) 9_654 ?
O2 C4 1.272(6) . ?
O3 C4 1.261(6) 9_655 ?
N1 N2 1.077(11) . ?
C1 C2 1.418(7) . ?
C1 C3 1.394(7) 10_655 ?
C2 C3 1.391(7) . ?
C2 C4 1.486(7) . ?
C3 C1 1.394(7) 10_655 ?
C3 H3 0.9500 . ?
C4 O3 1.261(6) 5_544 ?
N3 N4 1.033(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Co1 O1 163.54(15) 9_654 . ?
O1 Co1 O2 94.42(14) 9_654 5_545 ?
O1 Co1 O2 80.54(14) . 5_545 ?
O1 Co1 O2 82.70(14) . . ?
O1 Co1 O2 81.09(14) 9_654 . ?
O1 Co1 O3 99.59(14) 9_654 . ?
O1 Co1 O3 96.43(15) . . ?
O1 Co1 N1 92.43(19) 9_654 . ?
O1 Co1 N1 92.6(2) . . ?
O2 Co1 O2 82.26(4) . 5_545 ?
O2 Co1 N1 97.93(19) . . ?
O2 Co1 N1 173.09(19) 5_545 . ?
O3 Co1 O2 94.56(14) . 5_545 ?
O3 Co1 O2 176.80(14) . . ?
O3 Co1 N1 85.2(2) . . ?
Co1 O1 Co1 97.44(15) 5_545 . ?
C1 O1 Co1 124.9(3) . . ?
C1 O1 Co1 124.4(3) . 5_545 ?
Co1 O2 Co1 92.70(14) . 9_654 ?
C4 O2 Co1 134.1(3) . 9_654 ?
C4 O2 Co1 129.2(3) . . ?
C4 O3 Co1 124.9(3) 9_655 . ?
N2 N1 Co1 170.2(9) . . ?
O1 C1 C2 125.0(5) . . ?
O1 C1 C3 117.7(4) . 10_655 ?
C3 C1 C2 117.3(5) 10_655 . ?
C1 C2 C4 123.4(5) . . ?
C3 C2 C1 119.5(5) . . ?
C3 C2 C4 117.0(4) . . ?
C1 C3 H3 118.4 10_655 . ?
C2 C3 C1 123.2(5) . 10_655 ?
C2 C3 H3 118.4 . . ?
O2 C4 C2 118.1(4) . . ?
O3 C4 O2 122.3(5) 5_544 . ?
O3 C4 C2 119.6(4) 5_544 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co1 O1 C1 C2 -108.6(5) 5_545 . . . ?
Co1 O1 C1 C2 23.3(7) . . . . ?
Co1 O1 C1 C3 72.3(6) 5_545 . . 10_655 ?
Co1 O1 C1 C3 -155.8(4) . . . 10_655 ?
Co1 O2 C4 O3 -2.0(8) 9_654 . . 5_544 ?
Co1 O2 C4 O3 149.1(4) . . . 5_544 ?
Co1 O2 C4 C2 176.3(3) 9_654 . . . ?
Co1 O2 C4 C2 -32.6(6) . . . . ?
O1 C1 C2 C3 -178.4(5) . . . . ?
O1 C1 C2 C4 4.5(8) . . . . ?
C1 C2 C3 C1 -0.7(9) . . . 10_655 ?
C1 C2 C4 O2 -0.3(8) . . . . ?
C1 C2 C4 O3 178.0(5) . . . 5_544 ?
C3 C1 C2 C3 0.7(8) 10_655 . . . ?
C3 C1 C2 C4 -176.3(5) 10_655 . . . ?
C3 C2 C4 O2 -177.4(5) . . . . ?
C3 C2 C4 O3 0.9(7) . . . 5_544 ?
C4 C2 C3 C1 176.5(5) . . . 10_655 ?

_shelx_res_file                  
;
    twin4.res created by SHELXL-2014/7

TITL twin4 in R-3 #148
REM reset to R-3 #148
CELL 0.6199 25.8105 25.8105 6.9011 90 90 120
ZERR 9 0.0077 0.0077 0.0021 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SFAC C H Co N O
DISP C 0.002 0.001 8.816
DISP Co 0.336 0.751 2743.04
DISP H -0 0 0.618
DISP N 0.004 0.002 14.369
DISP O 0.008 0.004 22.984
UNIT 72 18 18 67.94 54
DFIX 1.098 N3 N4
DELU N3 N4
SIMU N3 N4

L.S. 4
PLAN  20
SIZE 0.05 0.05 0.1
TEMP -173(2)
BOND
fmap 2
MORE -1
BOND $H
CONF
ACTA
REM <olex2.extras>
REM <HklSrc "%./twin5.hkl">
REM </olex2.extras>

WGHT    0.000000   50.435421
BASF   0.53346
FVAR       0.20911
CO1   3    0.685927    0.050533    0.021401    11.00000    0.01227    0.01378 =
         0.00632   -0.00035   -0.00002    0.00543
O1    5    0.607823    0.022855    0.162744    11.00000    0.01134    0.02207 =
         0.00803    0.00128   -0.00174    0.00810
O2    5    0.629546   -0.007621   -0.192096    11.00000    0.01624    0.01915 =
         0.00538   -0.00355   -0.00163    0.00874
O3    5    0.740051    0.103110    0.238061    11.00000    0.01622    0.01226 =
         0.00834    0.00088   -0.00174    0.00234
N1    4    0.688903    0.133890   -0.084198    11.00000    0.05713    0.04131 =
         0.03249    0.01068    0.00517    0.03473
N2    4    0.694923    0.177543   -0.113362    11.00000    0.16495    0.08257 =
         0.10387    0.01938   -0.00575    0.07646
C1    1    0.555791    0.010809    0.077561    11.00000    0.01653    0.01876 =
         0.01169   -0.00001   -0.00035    0.00964
C2    1    0.541291   -0.004837   -0.119987    11.00000    0.01767    0.02086 =
         0.01081   -0.00265   -0.00308    0.01022
C3    1    0.486661   -0.014783   -0.191588    11.00000    0.02056    0.01486 =
         0.00910   -0.00177   -0.00242    0.00830
AFIX  43
H3    2    0.477873   -0.024765   -0.324641    11.00000   -1.20000
AFIX   0
C4    1    0.580415   -0.014217   -0.256259    11.00000    0.01468    0.01519 =
         0.00890    0.00033    0.00189    0.00658

N3    4    0.371530   -0.133203   -0.488350    10.89000    0.23495    0.11040 =
         0.11528   -0.05632   -0.07812    0.07873
N4    4    0.362658   -0.157192   -0.361000    10.89000    0.21644    0.09320 =
         0.14309   -0.03371   -0.02401    0.05732
HKLF 5

REM  twin4 in R-3 #148
REM R1 =  0.0632 for    1753 Fo > 4sig(Fo)  and  0.0805 for all    2040 data
REM    110 parameters refined using      8 restraints

END

WGHT      0.0000     50.4353

REM Highest difference peak  0.688,  deepest hole -0.753,  1-sigma level  0.155
Q1    1   0.3567 -0.2873 -0.5708  11.00000  0.05    0.69
Q2    1   0.3400 -0.3138 -0.1524  11.00000  0.05    0.65
Q3    1   0.6883  0.0271  0.0748  11.00000  0.05    0.62
Q4    1   0.6313  0.0336 -0.2465  11.00000  0.05    0.62
Q5    1   0.6639  0.2847 -0.2463  11.00000  0.05    0.60
Q6    1   0.5433 -0.0078 -0.0205  11.00000  0.05    0.57
Q7    1   0.4720 -0.0403 -0.3863  11.00000  0.05    0.55
Q8    1   0.6746  0.2775 -0.3418  11.00000  0.05    0.53
Q9    1   0.6605  0.0407 -0.1407  11.00000  0.05    0.53
Q10   1   0.5988  0.0366  0.3792  11.00000  0.05    0.52
Q11   1   0.3604 -0.1694 -0.1567  11.00000  0.05    0.50
Q12   1   0.6388  0.2783  0.0437  11.00000  0.05    0.50
Q13   1   0.6933  0.0807  0.1907  11.00000  0.05    0.50
Q14   1   0.6826  0.3228  0.0194  11.00000  0.05    0.49
Q15   1   0.6604  0.0311 -0.3315  11.00000  0.05    0.49
Q16   1   0.7126  0.0754  0.0941  11.00000  0.05    0.49
Q17   1   0.6967  0.2741 -0.1935  11.00000  0.05    0.49
Q18   1   0.3695 -0.2692 -0.1568  11.00000  0.05    0.48
Q19   1   0.3903 -0.1204 -0.1750  11.00000  0.05    0.47
Q20   1   0.5798  0.0194  0.1148  11.00000  0.05    0.47
;
_shelx_res_checksum              1069
_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.467(2)
2 0.533(2)







####################################################################### 
# 
# 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_Co2dobdc
_database_code_depnum_ccdc_archive 'CCDC 1530119'
_audit_update_record             
;
2017-01-28 deposited with the CCDC.
2017-04-19 downloaded from the CCDC.
;
_audit_creation_date             2016-04-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            Co2(dobdc)
_chemical_name_systematic        ?
_chemical_formula_moiety         'Co2 (C8 H2 O6)'
_chemical_formula_sum            'C8 H2 Co2 O6'
_chemical_formula_weight         311.96
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3550 1.1300 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0140 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   25.892(4)
_cell_length_b                   25.892(4)
_cell_length_c                   6.8482(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3975.9(12)
_cell_formula_units_Z            9
_cell_measurement_reflns_used    8401
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      31.779
_cell_measurement_theta_min      3.801
_shelx_estimated_absorpt_T_max   0.890
_shelx_estimated_absorpt_T_min   0.731
_exptl_absorpt_coefficient_mu    2.385
_exptl_absorpt_correction_T_max  0.890
_exptl_absorpt_correction_T_min  0.613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1823 before and 0.0828 after correction.
 The Ratio of minimum to maximum transmission not present.
 The λ/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1791 before and 0.0843 after correction.
 The Ratio of minimum to maximum transmission is 0.69.
 The λ/2 correction factor is Not present

Final HKLF 4 output contains 20587 reflections, Rint = 0.5108
 (11056 with I > 3sig(I), Rint = 0.5120)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
Data was collected at Beamline 11.3.1 at the Advanced
 Light Source, Lawrence Berkeley National Laboratory using synchrotron
 radiation (lamda = 0.7749 angstroms) and a Bruker APEX-II CCD detector.

The crystal was mounted on a MiTeGen loop using a minimal amount
 of epoxy to ensure that the crystal pores remained accessible.
 The sample was then placed in a custom-made gas cell equipped
 with a borosilicate glass cap, O-ring seal, and gas loading
 valve.  The cell was evacuated under reduced pressure at
 473 K for 6 hours to remove solvent molecules filling
 the pores and bound onto the exposed Co sites within the crystal.
 The crystal was then cooled to a final temperature of 296.15 K followed by data collection.
The crystal was found to be an obverse/reverse twin based on the diffraction
 pattern.  CELL_NOW was used to determine the orientation matrices
 and the domains were related by a 60 deg rotation around the
 real axis 1 0 0. The integration was preformed with both
 matrices. TWINABS was used to produce a merged HKLF4 file, for
 structure solution and initial refinement, and HKLF5 file for
 final structure refinement. The HKLF5 file contained the merged
 reflections from the second component and those that overlapped with the
 first component were split into two reflections. TWINABS indicated
 the twin faction to be 54:46. The structure was solved using the
 HKLF4 file, but the best refinement was given by the HKLF5 file.  
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0896
_diffrn_reflns_av_unetI/netI     0.0616
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            20587
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         32.088
_diffrn_reflns_theta_min         3.391
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω/θ scans'
_diffrn_radiation_monochromator  'channel-cut Si(111) crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2103
_reflns_number_total             2374
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.990
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         2374
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0485
_refine_ls_restrained_S_all      1.116
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0596P)²+12.8961P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1370
_refine_ls_wR_factor_ref         0.1453
_refine_special_details          
;Thermal parameters were refined anisotropically for all non-hydrogen atoms. 
Hydrogen atoms on the organic linker were placed in ideal positions and refined using the riding model.
The structure contains unassigned residual electron density (1.0 electron/cubic angstrom) 2.28 angstroms from Co. The distance of the q peak was too far to be conistent with water or methanol, even when modeled as an oxygen atom with freely refinened occupancy.
The density may be due to defects in the structure where a very small fraction of the Co sites remain inaccessible., Twin
;
_vrf_PLAT602_Co2dobdc            
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info 
RESPONSE: The structure is of a metal-organic framework that exhibits 
one-dimensional hexagonal pores. Solvent molecules within the pores and 
coordinated onto exposed Co sites in the framework were removed by 
heating the crystal under vacuum. It is likely that the pores are 
largely empty. 
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.539(2) 0.461(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.36219(2) 0.04843(2) 0.02411(6) 0.02096(17) Uani 1 1 d . . . . .
O1 O 0.41418(11) 0.02221(12) 0.1604(3) 0.0250(5) Uani 1 1 d . . . . .
O2 O 0.36573(12) -0.00446(14) -0.1989(4) 0.0289(6) Uani 1 1 d . . . . .
O3 O 0.36477(13) 0.10388(12) 0.2338(3) 0.0291(6) Uani 1 1 d . . . . .
C1 C 0.32296(17) 0.11094(16) 0.7436(5) 0.0252(7) Uani 1 1 d . . . . .
C2 C 0.33925(17) 0.12628(16) 0.5454(5) 0.0254(7) Uani 1 1 d . . . . .
C3 C 0.34948(18) 0.18138(17) 0.4736(5) 0.0276(7) Uani 1 1 d . . . . .
H3 H 0.3605 0.1909 0.3435 0.033 Uiso 1 1 calc R . . . .
C4 C 0.34769(17) 0.08704(16) 0.4052(5) 0.0233(7) Uani 1 1 d . . . . .

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 0.0271(3) 0.0238(3) 0.0137(2) -0.00099(15) -0.00023(15) 0.0140(2)
O1 0.0244(12) 0.0398(14) 0.0151(10) 0.0001(9) 0.0014(9) 0.0192(11)
O2 0.0288(13) 0.0461(16) 0.0185(11) -0.0089(11) -0.0058(9) 0.0236(12)
O3 0.0508(17) 0.0265(13) 0.0139(10) 0.0000(9) 0.0056(10) 0.0222(13)
C1 0.0373(19) 0.0255(16) 0.0184(15) 0.0009(12) 0.0019(13) 0.0199(15)
C2 0.0346(19) 0.0281(17) 0.0165(14) -0.0011(12) 0.0004(12) 0.0179(15)
C3 0.042(2) 0.0279(17) 0.0165(15) 0.0018(12) 0.0036(13) 0.0204(16)
C4 0.0328(17) 0.0249(16) 0.0148(13) -0.0030(11) -0.0014(12) 0.0165(14)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 Co1 2.9652(6) 8_544 ?
Co1 Co1 2.9651(6) 6 ?
Co1 O1 2.015(2) . ?
Co1 O1 1.997(2) 8_544 ?
Co1 O2 2.084(3) . ?
Co1 O2 2.070(3) 6 ?
Co1 O3 2.008(2) . ?
O1 Co1 1.997(2) 6 ?
O1 C1 1.356(4) 6_554 ?
O2 Co1 2.070(3) 8_544 ?
O2 C4 1.266(4) 6_554 ?
O3 C4 1.253(4) . ?
C1 O1 1.356(4) 8_545 ?
C1 C2 1.418(4) . ?
C1 C3 1.393(5) 13_556 ?
C2 C3 1.404(5) . ?
C2 C4 1.492(5) . ?
C3 C1 1.393(5) 13_556 ?
C3 H3 0.9300 . ?
C4 O2 1.267(4) 8_545 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Co1 Co1 Co1 112.89(2) 6 8_544 ?
O1 Co1 Co1 121.53(8) . 8_544 ?
O1 Co1 Co1 42.11(7) . 6 ?
O1 Co1 Co1 42.57(7) 8_544 8_544 ?
O1 Co1 Co1 140.70(8) 8_544 6 ?
O1 Co1 O1 162.92(11) 8_544 . ?
O1 Co1 O2 80.80(11) . 6 ?
O1 Co1 O2 96.69(10) 8_544 6 ?
O1 Co1 O2 82.06(10) . . ?
O1 Co1 O2 80.87(10) 8_544 . ?
O1 Co1 O3 100.15(11) 8_544 . ?
O2 Co1 Co1 44.64(7) 6 6 ?
O2 Co1 Co1 97.82(8) . 6 ?
O2 Co1 Co1 73.20(7) 6 8_544 ?
O2 Co1 Co1 44.26(7) . 8_544 ?
O2 Co1 O2 83.52(3) 6 . ?
O3 Co1 Co1 138.29(9) . 8_544 ?
O3 Co1 Co1 83.94(7) . 6 ?
O3 Co1 O1 96.92(11) . . ?
O3 Co1 O2 175.88(12) . . ?
O3 Co1 O2 100.28(11) . 6 ?
Co1 O1 Co1 95.32(10) 6 . ?
C1 O1 Co1 127.1(2) 6_554 . ?
C1 O1 Co1 125.7(2) 6_554 6 ?
Co1 O2 Co1 91.10(10) 8_544 . ?
C4 O2 Co1 133.8(2) 6_554 . ?
C4 O2 Co1 134.0(2) 6_554 8_544 ?
C4 O3 Co1 122.8(2) . . ?
O1 C1 C2 124.8(3) 8_545 . ?
O1 C1 C3 117.6(3) 8_545 13_556 ?
C3 C1 C2 117.6(3) 13_556 . ?
C1 C2 C4 123.4(3) . . ?
C3 C2 C1 119.9(3) . . ?
C3 C2 C4 116.7(3) . . ?
C1 C3 C2 122.5(3) 13_556 . ?
C1 C3 H3 118.8 13_556 . ?
C2 C3 H3 118.8 . . ?
O2 C4 C2 117.2(3) 8_545 . ?
O3 C4 O2 121.9(3) . 8_545 ?
O3 C4 C2 120.8(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co1 O3 C4 O2 13.1(5) . . . 8_545 ?
Co1 O3 C4 C2 -168.0(3) . . . . ?
O1 C1 C2 C3 178.9(4) 8_545 . . . ?
O1 C1 C2 C4 -2.5(6) 8_545 . . . ?
C1 C2 C3 C1 -0.6(7) . . . 13_556 ?
C1 C2 C4 O2 2.2(6) . . . 8_545 ?
C1 C2 C4 O3 -176.7(4) . . . . ?
C3 C1 C2 C3 0.6(6) 13_556 . . . ?
C3 C1 C2 C4 179.3(4) 13_556 . . . ?
C3 C2 C4 O2 -179.1(4) . . . 8_545 ?
C3 C2 C4 O3 2.0(5) . . . . ?
C4 C2 C3 C1 -179.4(4) . . . 13_556 ?

_shelx_res_file                  
;
    twin4.res created by SHELXL-2014/7

TITL twin4 in R-3 #148
REM reset to R-3 #148
CELL 0.7749 25.892 25.892 6.8482 90 90 120
ZERR 9 0.0036 0.0036 0.0009 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SFAC C H Co O
DISP C 0.004 0.002 13.872
DISP Co 0.355 1.13 5089.307
DISP H -0 0 0.627
DISP O 0.014 0.007 40.889
UNIT 72 18 18 54

L.S. 4
PLAN  20
SIZE 0.05 0.05 0.14
TEMP 23
BOND
MORE -1
BOND $H
CONF
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%./twin5.hkl">
REM </olex2.extras>

WGHT    0.059600   12.896100
BASF   0.46115
FVAR       0.27943
CO1   3    0.362190    0.048429    0.024105    11.00000    0.02710    0.02382 =
         0.01365   -0.00099   -0.00023    0.01401
O1    4    0.414181    0.022207    0.160438    11.00000    0.02442    0.03975 =
         0.01509    0.00007    0.00144    0.01921
O2    4    0.365731   -0.004462   -0.198928    11.00000    0.02875    0.04608 =
         0.01851   -0.00889   -0.00581    0.02365
O3    4    0.364771    0.103879    0.233824    11.00000    0.05077    0.02647 =
         0.01392   -0.00002    0.00560    0.02224
C1    1    0.322956    0.110937    0.743630    11.00000    0.03735    0.02554 =
         0.01838    0.00091    0.00186    0.01990
C2    1    0.339252    0.126278    0.545428    11.00000    0.03462    0.02809 =
         0.01652   -0.00113    0.00042    0.01794
C3    1    0.349477    0.181378    0.473558    11.00000    0.04213    0.02789 =
         0.01655    0.00176    0.00358    0.02035
AFIX  43
H3    2    0.360518    0.190867    0.343519    11.00000   -1.20000
AFIX   0
C4    1    0.347692    0.087035    0.405165    11.00000    0.03278    0.02491 =
         0.01483   -0.00301   -0.00137    0.01646
HKLF 5

REM  twin4 in R-3 #148
REM R1 =  0.0485 for    2103 Fo > 4sig(Fo)  and  0.0564 for all    2374 data
REM     74 parameters refined using      0 restraints

END

WGHT      0.0597     12.7718

REM Highest difference peak  0.990,  deepest hole -0.519,  1-sigma level  0.122
Q1    1   0.4439  0.1298 -0.1017  11.00000  0.05    0.99
Q2    1   0.4638  0.0777  0.2265  11.00000  0.05    0.49
Q3    1   0.3449 -0.0337 -0.2222  11.00000  0.05    0.48
Q4    1   0.1993  0.0388  0.5140  11.00000  0.05    0.47
Q5    1   0.1566  0.0850  0.4376  11.00000  0.05    0.47
Q6    1   0.4346  0.0405  0.2513  11.00000  0.05    0.47
Q7    1   0.5910  0.3030  0.1738  11.00000  0.05    0.46
Q8    1   0.6667  0.3333  0.8333  10.16667  0.05    0.45
Q9    1   0.4809  0.1488  0.0411  11.00000  0.05    0.43
Q10   1   0.3804  0.1207  0.1347  11.00000  0.05    0.43
Q11   1   0.3500  0.0199  0.0876  11.00000  0.05    0.40
Q12   1   0.4681  0.0530  0.1846  11.00000  0.05    0.40
Q13   1   0.6189  0.3134 -0.0536  11.00000  0.05    0.39
Q14   1   0.2725  0.0966  0.6756  11.00000  0.05    0.38
Q15   1   0.5218  0.2521  0.4383  11.00000  0.05    0.38
Q16   1   0.3227  0.0204  0.1085  11.00000  0.05    0.37
Q17   1   0.3609  0.1621  0.5262  11.00000  0.05    0.37
Q18   1   0.3038 -0.0813 -0.2097  11.00000  0.05    0.37
Q19   1   0.3973  0.0052  0.2340  11.00000  0.05    0.37
Q20   1   0.3923  0.0841  0.0632  11.00000  0.05    0.36
;
_shelx_res_checksum              12951
_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.539(2)
2 0.461(2)







####################################################################### 
# 
# 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_Co2dobdc-P4
_database_code_depnum_ccdc_archive 'CCDC 1530126'
_audit_update_record             
;
2017-01-28 deposited with the CCDC.
2017-04-19 downloaded from the CCDC.
;
_audit_creation_date             2017-01-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.11.30 svn.r3368 for OlexSys, GUI svn.r5269)
;
_chemical_name_common            Co2(dobdc)(P4)1.32
_chemical_name_systematic        ?
_chemical_formula_moiety         '(C8 H2 Co2 O4), 1.32(P4)'
_chemical_formula_sum            'C8 H2 Co2 O6 P5.28'
_chemical_formula_weight         475.58
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'
H H 0.0000 0.0000
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'
Co Co 0.3480 1.1400
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'
O O 0.0130 0.0070
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'
P P 0.1180 0.1130
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   25.7348(8)
_cell_length_b                   25.7348(8)
_cell_length_c                   6.8385(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3922.2(3)
_cell_formula_units_Z            9
_cell_measurement_reflns_used    9311
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      37.233
_cell_measurement_theta_min      3.397
_shelx_estimated_absorpt_T_max   0.816
_shelx_estimated_absorpt_T_min   0.611
_exptl_absorpt_coefficient_mu    3.034
_exptl_absorpt_correction_T_max  0.816
_exptl_absorpt_correction_T_min  0.694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0760 before and 0.0473 after correction.
 The Ratio of minimum to maximum transmission not present.
 The λ/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0758 before and 0.0462 after correction.
 The Ratio of minimum to maximum transmission is 0.85.
 The λ/2 correction factor is Not present

Final HKLF 4 output contains 43953 reflections, Rint = 0.0392
 (30737 with I > 3sig(I), Rint = 0.0342)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_colour_modifier   ?
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2081
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_exptl_special_details           
;
X-ray diffraction analyses were performed on single crystals coated with
 Paratone-N oil and mounted on MiTeGen loops. Crystals were frozen at a
 temperature of 100 K by an Oxford Cryosystems Cyrostream using N₂ during
 the experiments. Data was collected at Beamline 11.3.1 at the Advanced
 Light Source, Lawrence Berkeley National Laboratory using synchrotron
 radiation (lamda = 0.7749 angstrom) on a Bruker D8 diffractometer
equipped with a Bruker PHOTON100 CMOS detector.

The crystal was found to be a two-component non-merohedral twin based on 
the diffraction pattern. CELL_NOW was used to determine the orientation 
matrices and the domains were related by a 179.8 deg rotation around the
reciprocal axis 0 1 -0.5. The integration was preformed with both matrices. 
TWINABS was used to produce a merged HKLF4 file, for structure solution 
and initial refinement, and a HKLF5 file for final structure refinement. 
The HKLF5 file contained all reflections that involved domain 2. TWINABS 
indicated the twin faction to be 49:51. The structure was solved using the
HKLF4 file, but the best refinement was given by the HKLF5 file. 
;

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            43953
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         37.238
_diffrn_reflns_theta_min         3.398
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 with PHOTON100 CMOS detector'
_diffrn_measurement_method       'φ and ω shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3064
_reflns_number_total             3479
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         2.388
_refine_diff_density_min         -1.557
_refine_diff_density_rms         0.269
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         3479
_refine_ls_number_restraints     216
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0822
_refine_ls_restrained_S_all      1.228
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1256P)²+39.0610P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2465
_refine_ls_wR_factor_ref         0.2530
_refine_special_details          
;Thermal parameters were refined anisotropically for all non-hydrogen atoms. 
Hydrogen atoms were placed in ideal positions and refined using the riding model.
The structure shows P4 coordinated to the Co centers of the metal-organic framework,
Co2(dobdc). Initial refinement of the structure resulted in unusually long P-P bond
distances (2.5-2.6 angstroms) between the phosphorus atom coordinated to Co (P1) 
and the other phosphorus atoms in the P4 molecule. While this may result from
activation of the P4 molecule by the Co center, the long Co-P distance
(2.6 angstroms) indicated that the P4 molecule was only weakly bound and unactivated.
In addition, the atomic displacement parameters of the phosphorus atoms were large 
and severely prolate. These observations sugested that the long P-P bond distances
were artefacts that stem from disorder of the P4 molecule. Thus, the P4 molecule was
modeled to be disordered over two positions with all P-P distances restrained to be
similar (SADI). Refinement of the site occupancy of each position for the P4 moiety
resulted in chemical occupancies of 45.5(1.0)% and 20.6(1.0)%, which gives an overall
P4 occupancy of 66.1%. In the position with 45.5% occupancy, P4 coordinates to Co
vertex-on, with a Co-P distance of 2.625(10) angstroms. In the second position, the
P4 molecule was found 3.88(3) angstroms away from Co, which is too far for it to be
considered coordinated to the Co center. Further inspection of the structure reveals
that coordination of P4 at each Co site cannot occur because this would result in
P-P contacts that are much shorter (2.5 angstroms) than the sum of their van der 
Waals radii (3.9 angstroms), which likely results in the occupancy of coordinated
P4 to be close to 50%. The second P4 position likely arises from P4 molecules
filling sites where the first position remains unoccupied. Steric repulsion with
neighboring coordinated P4 prevents closer approach of P4 at the secondry sites,
leading to long Co-P distances for P4 at these sites., Twin
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.479(4) 0.521(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 P1A-P2A \\sim P1A-P3A \\sim P1A-P4A \\sim P1B-P2B \\sim P1B-P3B \\sim P1B-P4B
\\sim P2A-P3A \\sim P2A-P4A
 \\sim P3A-P4A \\sim P2B-P3B \\sim P2B-P4B \\sim P3B-P4B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
P1A \\sim P3A \\sim P4A \\sim P2A \\sim P1B \\sim P3B \\sim P4B \\sim P2B:
within 2.3A with sigma of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 P1A, P3A, P4A, P2A, P1B, P3B, P4B, P2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(P1A)=Sof(P2A)=Sof(P3A)=Sof(P4A)=FVAR(1)
 Sof(P1B)=Sof(P2B)=Sof(P3B)=Sof(P4B)=FVAR(2)
7.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.31433(3) -0.05038(3) 0.48019(8) 0.01840(19) Uani 1 1 d . . . . .
O1 O 0.39206(16) -0.02320(17) 0.3379(4) 0.0214(6) Uani 1 1 d . . . . .
O2 O 0.37117(17) 0.00876(18) 0.6930(5) 0.0212(6) Uani 1 1 d . . . . .
O3 O 0.43759(16) 0.03149(18) 0.9315(5) 0.0227(7) Uani 1 1 d . . . . .
C1 C 0.4437(2) -0.0113(2) 0.4217(6) 0.0204(8) Uani 1 1 d . . . . .
C2 C 0.4591(2) 0.0059(2) 0.6208(6) 0.0203(8) Uani 1 1 d . . . . .
C3 C 0.5141(2) 0.0161(2) 0.6928(6) 0.0210(8) Uani 1 1 d . . . . .
H3 H 0.523280 0.026829 0.826517 0.025 Uiso 1 1 calc R . . . .
C4 C 0.4203(2) 0.0156(2) 0.7582(6) 0.0194(7) Uani 1 1 d . . . . .
P1A P 0.3200(3) -0.1403(3) 0.6386(12) 0.084(3) Uani 0.455(10) 1 d D U P A -1
P2A P 0.3645(7) -0.1960(6) 0.706(2) 0.157(5) Uani 0.455(10) 1 d D U P A -1
P3A P 0.3674(7) -0.1324(6) 0.933(2) 0.145(5) Uani 0.455(10) 1 d D U P A -1
P4A P 0.2805(7) -0.2151(6) 0.862(2) 0.167(6) Uani 0.455(10) 1 d D U P A -1
P1B P 0.3295(17) -0.1668(14) 0.799(4) 0.172(9) Uani 0.206(10) 1 d D U P B -2
P2B P 0.3589(12) -0.2297(11) 0.926(5) 0.140(8) Uani 0.206(10) 1 d D U P B -2
P3B P 0.3464(14) -0.1668(12) 1.118(4) 0.139(8) Uani 0.206(10) 1 d D U P B -2
P4B P 0.2666(10) -0.2461(14) 0.987(5) 0.163(9) Uani 0.206(10) 1 d D U P B -2

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 0.0229(3) 0.0228(3) 0.0067(2) -0.00047(18) -0.00016(18) 0.0093(2)
O1 0.0228(15) 0.0324(17) 0.0094(12) -0.0007(11) -0.0032(10) 0.0141(14)
O2 0.0250(15) 0.0324(17) 0.0093(11) -0.0036(11) -0.0003(11) 0.0167(14)
O3 0.0238(15) 0.0386(19) 0.0084(12) -0.0034(12) -0.0013(10) 0.0176(15)
C1 0.026(2) 0.031(2) 0.0085(14) -0.0009(14) -0.0005(13) 0.0174(18)
C2 0.0247(19) 0.033(2) 0.0085(15) -0.0001(14) 0.0001(13) 0.0180(18)
C3 0.0233(19) 0.035(2) 0.0086(14) 0.0011(14) 0.0007(13) 0.0175(18)
C4 0.0228(19) 0.027(2) 0.0098(15) -0.0001(14) 0.0013(13) 0.0135(16)
P1A 0.057(3) 0.078(4) 0.096(5) -0.031(4) 0.023(3) 0.018(3)
P2A 0.165(10) 0.154(10) 0.205(12) -0.054(9) -0.029(9) 0.119(8)
P3A 0.195(12) 0.105(8) 0.143(10) -0.032(7) -0.044(9) 0.080(8)
P4A 0.185(11) 0.100(8) 0.194(12) 0.038(8) 0.048(10) 0.056(7)
P1B 0.168(15) 0.145(14) 0.195(15) -0.022(12) 0.003(13) 0.072(12)
P2B 0.146(14) 0.108(12) 0.188(17) -0.046(11) 0.024(13) 0.081(11)
P3B 0.166(15) 0.125(13) 0.180(15) -0.043(12) -0.002(14) 0.114(12)
P4B 0.150(15) 0.162(16) 0.20(2) 0.017(14) -0.007(15) 0.094(13)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 2.007(3) 6 ?
Co1 O1 2.009(4) . ?
Co1 O2 2.085(3) . ?
Co1 O2 2.095(3) 8_544 ?
Co1 O3 2.022(3) 6_554 ?
Co1 P1A 2.625(10) . ?
O1 C1 1.336(6) . ?
O2 C4 1.268(6) . ?
O3 C4 1.259(5) . ?
C1 C2 1.425(6) . ?
C1 C3 1.392(6) 10_656 ?
C2 C3 1.395(6) . ?
C2 C4 1.480(6) . ?
P1A P2A 2.285(13) . ?
P1A P3A 2.309(14) . ?
P1A P4A 2.262(14) . ?
P2A P3A 2.226(14) . ?
P2A P4A 2.234(16) . ?
P3A P4A 2.236(15) . ?
P1B P2B 2.278(18) . ?
P1B P3B 2.227(18) . ?
P1B P4B 2.268(18) . ?
P2B P3B 2.230(16) . ?
P2B P4B 2.236(17) . ?
P3B P4B 2.235(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Co1 O1 164.15(16) 6 . ?
O1 Co1 O2 81.82(14) 6 . ?
O1 Co1 O2 93.52(14) 6 8_544 ?
O1 Co1 O2 82.59(13) . . ?
O1 Co1 O2 81.50(15) . 8_544 ?
O1 Co1 O3 99.31(15) 6 6_554 ?
O1 Co1 O3 96.13(14) . 6_554 ?
O1 Co1 P1A 91.99(17) 6 . ?
O1 Co1 P1A 91.28(18) . . ?
O2 Co1 O2 82.08(4) . 8_544 ?
O2 Co1 P1A 170.92(19) 8_544 . ?
O2 Co1 P1A 91.59(19) . . ?
O3 Co1 O2 95.26(14) 6_554 8_544 ?
O3 Co1 O2 177.18(14) 6_554 . ?
O3 Co1 P1A 90.9(2) 6_554 . ?
Co1 O1 Co1 97.05(15) 8_544 . ?
C1 O1 Co1 125.2(3) . . ?
C1 O1 Co1 124.2(3) . 8_544 ?
Co1 O2 Co1 92.07(14) . 6 ?
C4 O2 Co1 129.4(3) . . ?
C4 O2 Co1 134.1(3) . 6 ?
C4 O3 Co1 123.7(3) . 8_545 ?
O1 C1 C2 124.8(4) . . ?
O1 C1 C3 118.0(4) . 10_656 ?
C3 C1 C2 117.2(4) 10_656 . ?
C1 C2 C4 123.6(4) . . ?
C3 C2 C1 119.6(4) . . ?
C3 C2 C4 116.8(4) . . ?
C1 C3 C2 123.2(4) 10_656 . ?
O2 C4 C2 117.6(4) . . ?
O3 C4 O2 122.8(4) . . ?
O3 C4 C2 119.6(4) . . ?
P2A P1A Co1 154.5(5) . . ?
P2A P1A P3A 58.0(4) . . ?
P3A P1A Co1 122.8(4) . . ?
P4A P1A Co1 146.0(5) . . ?
P4A P1A P2A 58.8(4) . . ?
P4A P1A P3A 58.5(4) . . ?
P3A P2A P1A 61.6(4) . . ?
P3A P2A P4A 60.2(4) . . ?
P4A P2A P1A 60.1(4) . . ?
P2A P3A P1A 60.5(4) . . ?
P2A P3A P4A 60.1(4) . . ?
P4A P3A P1A 59.7(4) . . ?
P2A P4A P1A 61.1(4) . . ?
P2A P4A P3A 59.7(4) . . ?
P3A P4A P1A 61.8(4) . . ?
P3B P1B P2B 59.3(5) . . ?
P3B P1B P4B 59.6(5) . . ?
P4B P1B P2B 58.9(5) . . ?
P3B P2B P1B 59.2(5) . . ?
P3B P2B P4B 60.1(5) . . ?
P4B P2B P1B 60.3(5) . . ?
P1B P3B P2B 61.5(5) . . ?
P1B P3B P4B 61.1(5) . . ?
P2B P3B P4B 60.1(5) . . ?
P2B P4B P1B 60.8(5) . . ?
P2B P4B P3B 59.8(5) . . ?
P3B P4B P1B 59.3(5) . . ?

_shelx_res_file                  
;
TITL twin4 in R-3 #148
    twin4.res
    created by SHELXL-2016/6 at 01:07:25 on 06-Jan-2017
REM reset to R-3 #148
CELL 0.7749 25.7348 25.7348 6.8385 90 90 120
ZERR 9 0.0008 0.0008 0.0002 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SFAC C H Co O P
DISP C 0.004 0.002 13.6
DISP Co 0.348 1.14 5063.1
DISP H -0 0 0.7
DISP O 0.013 0.007 40.2
DISP P 0.118 0.113 519.8
UNIT 72 18 18 54 47.55
SADI P1A P2A P1A P3A P1A P4A P1B P2B P1B P3B P1B P4B P2A P3A P2A P4A P3A P4A =
 P2B P3B P2B P4B P3B P4B
SIMU 0.04 0.08 2.3 P1A P3A P4A P2A P1B P3B P4B P2B
RIGU P1A P3A P4A P2A P1B P3B P4B P2B

L.S. 20
PLAN  20
SIZE 0.18 0.07 0.07
TEMP -173(2)
MORE -1
BOND
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%./twin5.hkl">
REM </olex2.extras>

WGHT    0.125600   39.061001
BASF   0.52099
FVAR       0.24074   0.45480   0.20633
CO1   3    0.314332   -0.050384    0.480185    11.00000    0.02288    0.02284 =
         0.00666   -0.00047   -0.00016    0.00931
O1    4    0.392055   -0.023205    0.337892    11.00000    0.02285    0.03241 =
         0.00939   -0.00067   -0.00317    0.01410
O2    4    0.371167    0.008759    0.693001    11.00000    0.02502    0.03244 =
         0.00927   -0.00364   -0.00034    0.01672
O3    4    0.437593    0.031491    0.931498    11.00000    0.02380    0.03857 =
         0.00845   -0.00341   -0.00134    0.01765
C1    1    0.443743   -0.011311    0.421652    11.00000    0.02627    0.03053 =
         0.00855   -0.00093   -0.00055    0.01737
C2    1    0.459079    0.005892    0.620779    11.00000    0.02469    0.03259 =
         0.00854   -0.00010    0.00015    0.01796
C3    1    0.514114    0.016094    0.692837    11.00000    0.02329    0.03495 =
         0.00864    0.00113    0.00065    0.01749
AFIX  43
H3    2    0.523280    0.026829    0.826517    11.00000   -1.20000
AFIX   0
C4    1    0.420333    0.015645    0.758240    11.00000    0.02282    0.02693 =
         0.00982   -0.00006    0.00133    0.01348
PART -1
P1A   5    0.319989   -0.140334    0.638569    21.00000    0.05706    0.07752 =
         0.09644   -0.03053    0.02311    0.01828
P2A   5    0.364515   -0.195976    0.706383    21.00000    0.16524    0.15373 =
         0.20476   -0.05399   -0.02887    0.11946
P3A   5    0.367397   -0.132450    0.932816    21.00000    0.19549    0.10491 =
         0.14269   -0.03189   -0.04449    0.08020
P4A   5    0.280516   -0.215061    0.862302    21.00000    0.18530    0.09980 =
         0.19411    0.03798    0.04800    0.05574

PART 0
PART -2
P1B   5    0.329488   -0.166751    0.798843    31.00000    0.16847    0.14458 =
         0.19499   -0.02183    0.00301    0.07234
P2B   5    0.358916   -0.229737    0.926411    31.00000    0.14616    0.10836 =
         0.18783   -0.04589    0.02366    0.08063
P3B   5    0.346403   -0.166759    1.118181    31.00000    0.16615    0.12463 =
         0.17970   -0.04328   -0.00162    0.11350
P4B   5    0.266573   -0.246073    0.987165    31.00000    0.15003    0.16224 =
         0.19894    0.01714   -0.00708    0.09394
HKLF 5




REM  twin4 in R-3 #148
REM R1 =  0.0822 for    3064 Fo > 4sig(Fo)  and  0.0902 for all    3479 data
REM    148 parameters refined using    216 restraints

END

WGHT      0.1294     39.6721

REM Highest difference peak  2.388,  deepest hole -1.557,  1-sigma level  0.269
Q1    1   0.3093 -0.1255  0.5977  11.00000  0.05    2.39
Q2    1   0.3112 -0.0257  0.4735  11.00000  0.05    1.92
Q3    1   0.2837 -0.0671  0.4794  11.00000  0.05    1.77
Q4    1   0.3205 -0.0744  0.4742  11.00000  0.05    1.33
Q5    1   0.3234 -0.2519  1.2136  11.00000  0.05    1.27
Q6    1   0.3426 -0.0445  0.4850  11.00000  0.05    1.25
Q7    1   0.2709 -0.2349  1.2035  11.00000  0.05    1.23
Q8    1   0.2962 -0.2054  1.0595  11.00000  0.05    1.22
Q9    1   0.3936 -0.1463  0.9650  11.00000  0.05    1.18
Q10   1   0.3386 -0.2529  1.1067  11.00000  0.05    1.13
Q11   1   0.3117 -0.2029  1.1272  11.00000  0.05    1.11
Q12   1   0.4195 -0.1319  0.8995  11.00000  0.05    1.10
Q13   1   0.3547 -0.2368  1.0153  11.00000  0.05    1.07
Q14   1   0.3676 -0.1551  1.0483  11.00000  0.05    1.06
Q15   1   0.4513  0.0158  0.4777  11.00000  0.05    0.80
Q16   1   0.4029 -0.1322  0.8445  11.00000  0.05    0.75
Q17   1   0.3837 -0.0647  0.8100  11.00000  0.05    0.74
Q18   1   0.3191 -0.2328  0.7120  11.00000  0.05    0.68
Q19   1   0.4493  0.0157  0.7121  11.00000  0.05    0.67
Q20   1   0.4002  0.0286  0.7443  11.00000  0.05    0.66
;
_shelx_res_checksum              66035
_shelx_SHELXL_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.479(4)
2 0.521(4)



####################################################################### 
# 
# 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_Co2-dobdc-Ar
_database_code_depnum_ccdc_archive 'CCDC 1530123'
_audit_update_record             
;
2017-01-28 deposited with the CCDC.
2017-04-19 downloaded from the CCDC.
;
_audit_creation_date             2016-04-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            Co2(dobdc)Ar2
_chemical_name_systematic        ?
_chemical_formula_moiety         'Co2 (C8 H2 O6) Ar2'
_chemical_formula_sum            'C8 H2 Ar2 Co2 O6'
_chemical_formula_weight         391.86
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ar Ar 0.1610 0.1770 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3460 0.8250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0090 0.0050 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   25.860(4)
_cell_length_b                   25.860(4)
_cell_length_c                   6.8678(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3977.5(12)
_cell_formula_units_Z            9
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.468
_cell_measurement_theta_min      2.848
_shelx_estimated_absorpt_T_max   0.900
_shelx_estimated_absorpt_T_min   0.717
_exptl_absorpt_coefficient_mu    1.785
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_correction_T_min  0.738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1600 before and 0.0899 after correction.
 The Ratio of minimum to maximum transmission not present.
 The λ/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1630 before and 0.0886 after correction.
 The Ratio of minimum to maximum transmission is 0.83.
 The λ/2 correction factor is Not present

Final HKLF 4 output contains 35948 reflections, Rint = 0.0936
 (18422 with I > 3sig(I), Rint = 0.0772)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1692
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_exptl_special_details           
;
Data was collected at Beamline 11.3.1 at the Advanced
 Light Source, Lawrence Berkeley National Laboratory using synchrotron
 radiation (lamda = 0.6525 angstroms) and a Bruker APEX-II CCD detector.

The crystal was mounted on a MiTeGen loop using a minimal amount
 of epoxy to ensure that the crystal pores remained accessible.
 The sample was then placed in a custom-made gas cell equipped
 with a borosilicate glass cap, O-ring seal, and gas loading
 valve.  The cell was evacuated under reduced pressure at
 500 K for 5 hours to remove solvent molecules filling
 the pores and bound onto the exposed Co sites within the crystal.
 After obtaining the structure of the desolvated crystal to
 confirm the absence of solvent bound onto the Co sites, the
 crystal was cooled to 298 deg C then dosed with 1.14 bar Ar.
 The crystal was then cooled to a final temperature of 90 K at ramp rate of 6 deg C per minute followed by data collection.
The crystal was found to be an obverse/reverse twin based on the diffraction
 pattern.  CELL_NOW was used to determine the orientation matrices
 and the domains were related by a 180 deg rotation around the
 reciprocal axis 0 1 -0.5 The integration was preformed with both
 matrices. TWINABS was used to produce a merged HKLF4 file, for
 structure solution and initial refinement, and HKLF5 file for
 final structure refinement. The HKLF5 file contained the merged
 reflections from the second component and those that overlapped with the
 first component were split into two reflections. TWINABS indicated
 the twin faction to be 52:48. The structure was solved using the
 HKLF4 file, but the best refinement was given by the HKLF5 file.  
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0936
_diffrn_reflns_av_unetI/netI     0.0605
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            35948
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        23.048
_diffrn_reflns_theta_max         31.785
_diffrn_reflns_theta_min         2.848
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω/θ scans'
_diffrn_radiation_monochromator  'channel-cut Si(111) crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6525
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3302
_reflns_number_total             3887
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.740
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         3887
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0513
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0512P)²+14.0654P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1272
_refine_ls_wR_factor_ref         0.1358
_refine_special_details          
;Thermal parameters were refined anisotropically for all non-hydrogen atoms. 
Hydrogen atoms were placed in ideal positions and refined using the riding model.
The chemcial occupancies of Ar interacting with the Co sites (Ar1) and Ar in a secondary binding site (Ar2) were initially allowed to refine freely, resulting in a chemical occupancy of roughly 60% for Ar1 40% for Ar2. The two sites were found to be too close to each other for both sites to be populated at the same time. 
Thus, the chemical occupancies of the Ar1 and Ar2 were refined against each other, resulting in a chemical occupancy of 61% for Ar1 and 39% for Ar2.
The interaction of both Ar atoms with the framework is so weak that it unlikely to form an ordered orientation at 100 K, which explains the relatively large thermal displacement parameters for Ar1 and Ar2. The displacement parameters for Ar1 and Ar2 were restrained to be similar, 
because the proximity of the two sites was causing the thermal ellipsoids of Ar2 to extend toward the site of Ar1., Twin
;
_vrf_PLAT601_Co2-dobdc-Ar        
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        255 Ang3  
RESPONSE: The structure is of a metal-organic framework that exhibits 
one-dimensional hexagonal pores. Solvent molecules within the pores and 
coordinated onto exposed Co sites in the framework were removed by 
heating the crystal under vacuum. The crystal was then dosed with Ar 
to characterize its interaction with the exposed Co site. It is likely 
that the pores are largely empty or filled with Ar in the gas phase.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.5551(17) 0.4449(17)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Uiso/Uaniso restraints and constraints
Ar2 \\sim Ar1: within 3A with sigma of 0.04 and sigma for terminal atoms of 0.08
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.36295(2) 0.04900(2) 0.52338(5) 0.01338(9) Uani 1 1 d . . . . .
O1 O 0.31120(8) 0.05898(8) 0.3278(2) 0.0158(3) Uani 1 1 d . . . . .
O2 O 0.29608(8) -0.03088(8) 0.6374(3) 0.0174(3) Uani 1 1 d . . . . .
O3 O 0.36499(9) 0.10394(8) 0.7350(3) 0.0181(3) Uani 1 1 d . . . . .
C1 C 0.32274(11) 0.11099(11) 1.2437(3) 0.0153(4) Uani 1 1 d . . . . .
C2 C 0.33927(11) 0.12607(11) 1.0461(3) 0.0158(4) Uani 1 1 d . . . . .
C3 C 0.34948(12) 0.18115(11) 0.9739(3) 0.0166(4) Uani 1 1 d . . . . .
H3 H 0.3606 0.1907 0.8412 0.020 Uiso 1 1 calc R . . . .
C4 C 0.34829(11) 0.08681(10) 0.9071(3) 0.0148(4) Uani 1 1 d . . . . .
Ar1 Ar 0.4698(4) 0.1516(4) 0.3607(16) 0.238(6) Uani 0.606(13) 1 d . U . A 1
Ar2 Ar 0.5079(9) 0.1441(8) -0.001(5) 0.417(19) Uani 0.393(16) 1 d . U . B 2

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 0.01699(15) 0.01500(14) 0.00979(13) -0.00062(9) -0.00031(10) 0.00924(12)
O1 0.0223(8) 0.0140(7) 0.0122(7) 0.0022(5) 0.0001(6) 0.0100(6)
O2 0.0168(7) 0.0176(7) 0.0116(7) 0.0023(6) -0.0021(6) 0.0039(6)
O3 0.0287(9) 0.0169(7) 0.0111(7) 0.0004(6) 0.0030(6) 0.0133(7)
C1 0.0192(9) 0.0158(9) 0.0128(9) 0.0004(7) 0.0010(7) 0.0102(8)
C2 0.0212(10) 0.0166(9) 0.0131(9) 0.0005(7) 0.0006(7) 0.0120(8)
C3 0.0248(10) 0.0168(9) 0.0110(8) 0.0011(7) 0.0017(7) 0.0125(8)
C4 0.0194(9) 0.0155(9) 0.0107(8) -0.0016(7) -0.0004(7) 0.0097(8)
Ar1 0.205(8) 0.212(9) 0.313(12) 0.021(8) -0.075(7) 0.117(7)
Ar2 0.272(19) 0.211(16) 0.76(4) -0.22(2) -0.25(2) 0.110(13)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 Co1 2.9843(5) 6 ?
Co1 Co1 2.9844(5) 8_544 ?
Co1 O1 2.0191(17) 6 ?
Co1 O1 2.0017(18) . ?
Co1 O2 2.0733(18) . ?
Co1 O2 2.0899(18) 8_544 ?
Co1 O3 2.0147(18) . ?
Co1 Ar1 2.932(9) . ?
O1 Co1 2.0192(17) 8_544 ?
O1 C1 1.353(3) 1_554 ?
O2 Co1 2.0898(18) 6 ?
O2 C4 1.264(3) 8_544 ?
O3 C4 1.260(3) . ?
C1 O1 1.353(3) 1_556 ?
C1 C2 1.418(3) . ?
C1 C3 1.393(3) 13_557 ?
C2 C3 1.403(3) . ?
C2 C4 1.494(3) . ?
C3 C1 1.393(3) 13_557 ?
C3 H3 0.9500 . ?
C4 O2 1.264(3) 6 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Co1 Co1 Co1 112.498(16) 6 8_544 ?
O1 Co1 Co1 139.94(5) . 6 ?
O1 Co1 Co1 41.86(5) 6 6 ?
O1 Co1 Co1 42.30(5) . 8_544 ?
O1 Co1 Co1 121.77(5) 6 8_544 ?
O1 Co1 O1 163.18(8) . 6 ?
O1 Co1 O2 81.09(7) . 8_544 ?
O1 Co1 O2 82.12(7) 6 8_544 ?
O1 Co1 O2 95.95(7) . . ?
O1 Co1 O2 81.09(7) 6 . ?
O1 Co1 O3 100.18(7) . . ?
O1 Co1 Ar1 90.90(16) . . ?
O1 Co1 Ar1 90.27(16) 6 . ?
O2 Co1 Co1 43.98(5) 8_544 8_544 ?
O2 Co1 Co1 44.43(5) . 6 ?
O2 Co1 Co1 73.59(5) . 8_544 ?
O2 Co1 Co1 96.46(6) 8_544 6 ?
O2 Co1 O2 83.13(2) . 8_544 ?
O2 Co1 Ar1 170.06(19) . . ?
O2 Co1 Ar1 90.9(2) 8_544 . ?
O3 Co1 Co1 83.64(5) . 6 ?
O3 Co1 Co1 137.84(6) . 8_544 ?
O3 Co1 O1 96.63(7) . 6 ?
O3 Co1 O2 98.34(8) . . ?
O3 Co1 O2 177.92(8) . 8_544 ?
O3 Co1 Ar1 87.5(2) . . ?
Ar1 Co1 Co1 107.4(2) . 8_544 ?
Ar1 Co1 Co1 129.16(15) . 6 ?
Co1 O1 Co1 95.84(7) . 8_544 ?
C1 O1 Co1 126.32(14) 1_554 8_544 ?
C1 O1 Co1 125.81(15) 1_554 . ?
Co1 O2 Co1 91.59(7) . 6 ?
C4 O2 Co1 134.08(15) 8_544 . ?
C4 O2 Co1 132.15(16) 8_544 6 ?
C4 O3 Co1 123.03(16) . . ?
O1 C1 C2 124.6(2) 1_556 . ?
O1 C1 C3 117.5(2) 1_556 13_557 ?
C3 C1 C2 117.9(2) 13_557 . ?
C1 C2 C4 123.5(2) . . ?
C3 C2 C1 119.7(2) . . ?
C3 C2 C4 116.7(2) . . ?
C1 C3 C2 122.4(2) 13_557 . ?
C1 C3 H3 118.8 13_557 . ?
C2 C3 H3 118.8 . . ?
O2 C4 C2 117.4(2) 6 . ?
O3 C4 O2 122.4(2) . 6 ?
O3 C4 C2 120.2(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co1 O3 C4 O2 13.8(3) . . . 6 ?
Co1 O3 C4 C2 -167.64(17) . . . . ?
O1 C1 C2 C3 179.2(2) 1_556 . . . ?
O1 C1 C2 C4 -2.5(4) 1_556 . . . ?
C1 C2 C3 C1 -0.1(4) . . . 13_557 ?
C1 C2 C4 O2 1.1(4) . . . 6 ?
C1 C2 C4 O3 -177.5(2) . . . . ?
C3 C1 C2 C3 0.1(4) 13_557 . . . ?
C3 C1 C2 C4 178.4(2) 13_557 . . . ?
C3 C2 C4 O2 179.5(2) . . . 6 ?
C3 C2 C4 O3 0.8(3) . . . . ?
C4 C2 C3 C1 -178.6(2) . . . 13_557 ?

_shelx_res_file                  
;
    twin284.res created by SHELXL-2014/7

TITL twin284 in R-3 #148
REM reset to R-3 #148
CELL 0.6525 25.8602 25.8602 6.8678 90 90 120
ZERR 9 0.0036 0.0036 0.001 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SFAC C H Ar Co O
DISP Ar 0.161 0.177 663.804
DISP C 0.003 0.001 9.695
DISP Co 0.346 0.825 3161.971
DISP H -0 0 0.621
DISP O 0.009 0.005 26.098
UNIT 72 18 18 18 54
SIMU 0.04 0.08 3 Ar2 Ar1

L.S. 4 0 0
PLAN  20
SIZE 0.06 0.06 0.2
TEMP -183(2)
BOND
MORE -1
BOND $H
CONF
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%./twin285.hkl">
REM </olex2.extras>

WGHT    0.051200   14.065400
BASF   0.44487
FVAR       0.26149
CO1   4    0.362945    0.049001    0.523380    11.00000    0.01699    0.01500 =
         0.00979   -0.00062   -0.00031    0.00924
O1    5    0.311204    0.058982    0.327780    11.00000    0.02231    0.01399 =
         0.01224    0.00222    0.00010    0.00997
O2    5    0.296082   -0.030883    0.637383    11.00000    0.01679    0.01756 =
         0.01157    0.00227   -0.00212    0.00390
O3    5    0.364989    0.103944    0.735016    11.00000    0.02874    0.01686 =
         0.01113    0.00042    0.00300    0.01334
C1    1    0.322744    0.110986    1.243744    11.00000    0.01924    0.01580 =
         0.01283    0.00040    0.00098    0.01020
C2    1    0.339265    0.126068    1.046108    11.00000    0.02120    0.01665 =
         0.01306    0.00047    0.00064    0.01204
C3    1    0.349481    0.181146    0.973889    11.00000    0.02481    0.01678 =
         0.01096    0.00108    0.00167    0.01253
AFIX  43
H3    2    0.360595    0.190692    0.841242    11.00000   -1.20000
AFIX   0
C4    1    0.348294    0.086810    0.907133    11.00000    0.01938    0.01548 =
         0.01072   -0.00157   -0.00037    0.00965
PART 1
AR1   3    0.469822    0.151647    0.360664     0.60607    0.20459    0.21198 =
         0.31325    0.02094   -0.07504    0.11655
PART 0
PART 2
AR2   3    0.507888    0.144131   -0.000784     0.39309    0.27160    0.21069 =
         0.75613   -0.22497   -0.24584    0.11040
HKLF 5

REM  twin284 in R-3 #148
REM R1 =  0.0513 for    3302 Fo > 4sig(Fo)  and  0.0637 for all    3887 data
REM     94 parameters refined using      6 restraints

END

WGHT      0.0512     14.0528

REM Highest difference peak  1.740,  deepest hole -0.956,  1-sigma level  0.156
Q1    1   0.4437  0.1270  0.4065  11.00000  0.05    1.74
Q2    1   0.3344  0.0284  0.4843  11.00000  0.05    0.80
Q3    1   0.4781  0.1408  0.2496  11.00000  0.05    0.70
Q4    1   0.3695  0.0756  0.4750  11.00000  0.05    0.70
Q5    1   0.3320  0.1038  1.1341  11.00000  0.05    0.62
Q6    1   0.4626  0.1962  0.4433  11.00000  0.05    0.61
Q7    1   0.4901  0.1262  0.0580  11.00000  0.05    0.59
Q8    1   0.3599  0.0731  0.6946  11.00000  0.05    0.57
Q9    1   0.5013  0.1649  0.6664  11.00000  0.05    0.57
Q10   1   0.3925  0.0641  0.5611  11.00000  0.05    0.56
Q11   1   0.3558  0.0236  0.5895  11.00000  0.05    0.56
Q12   1   0.3825  0.0435  0.4805  11.00000  0.05    0.55
Q13   1   0.2886  0.0356  0.2727  11.00000  0.05    0.55
Q14   1   0.3443  0.0590  0.5764  11.00000  0.05    0.54
Q15   1   0.5569  0.2844  0.3182  11.00000  0.05    0.53
Q16   1   0.4722  0.1771  0.3905  11.00000  0.05    0.52
Q17   1   0.3383  0.1538  1.0278  11.00000  0.05    0.51
Q18   1   0.3787  0.0628  0.7803  11.00000  0.05    0.50
Q19   1   0.4268  0.1763  0.9549  11.00000  0.05    0.50
Q20   1   0.2776 -0.0561  0.6373  11.00000  0.05    0.48
;
_shelx_res_checksum              57462
_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.5551(17)
2 0.4449(17)









####################################################################### 
# 
# 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_Co2dobdc-O2
_database_code_depnum_ccdc_archive 'CCDC 1530120'
_audit_update_record             
;
2017-01-28 deposited with the CCDC.
2017-04-19 downloaded from the CCDC.
;
_audit_creation_date             2016-04-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            Co2(dobdc)(O2)5.94
_chemical_name_systematic        ?
_chemical_formula_moiety         'Co2 (C8 H2 O6) 5.94(O2)'
_chemical_formula_sum            'C8 H2 Co2 O17.92'
_chemical_formula_weight         502.68
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3550 1.1300 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0140 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   25.7599(9)
_cell_length_b                   25.7599(9)
_cell_length_c                   6.8766(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3951.8(3)
_cell_formula_units_Z            9
_cell_measurement_reflns_used    4033
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.145
_cell_measurement_theta_min      2.986
_shelx_estimated_absorpt_T_max   0.906
_shelx_estimated_absorpt_T_min   0.787
_exptl_absorpt_coefficient_mu    2.511
_exptl_absorpt_correction_T_max  0.906
_exptl_absorpt_correction_T_min  0.521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1370 before and 0.0605 after correction.
 The Ratio of minimum to maximum transmission not present.
 The λ/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1333 before and 0.0597 after correction.
 The Ratio of minimum to maximum transmission is 0.58.
 The λ/2 correction factor is Not present

Final HKLF 4 output contains 13575 reflections, Rint = 0.0893
 (6594 with I > 3sig(I), Rint = 0.0619)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.901
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2226
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_exptl_special_details           
;
Data was collected at Beamline 11.3.1 at the Advanced
 Light Source, Lawrence Berkeley National Laboratory using synchrotron
 radiation (lamda = 0.7749 angstroms) and a Bruker PHOTON100 CMOS detector.

The crystal was mounted on a borosilicate glass fiber using a minimal amount
 of epoxy to ensure that the crystal pores remained accessible.
 The sample was then placed in a 1.0 mm borosilicate glass capillary, which was connected to a Micromeretics ASAP 2020 instrument via a custom-built adapter with an o-ring seal and gas loading
 valve.  The capillary was evacuated under reduced pressure at
 453 K for 24 hours to remove solvent molecules filling
 the pores and bound onto the exposed Co sites within the crystal.
 The capillary was then dosed with 500 mbar O2, then flame sealed.
 The capillary was cooled to 100 K using an Oxford Cryosystems cryostream for data collection.

The crystal was found to be an obverse/reverse twin based on the diffraction
 pattern.  CELL_NOW was used to determine the orientation matrices
 and the domains were related by a 180 deg rotation around the
 reciprocal axis 0 1 -0.5 The integration was preformed with both
 matrices. TWINABS was used to produce a merged HKLF4 file, for
 structure solution and initial refinement, and HKLF5 file for
 final structure refinement. The HKLF5 file contained the merged
 reflections from the second component and those that overlapped with the
 first component were split into two reflections. TWINABS indicated
 the twin faction to be 53:47. The structure was solved using the
 HKLF4 file, but the best refinement was given by the HKLF5 file.  
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0893
_diffrn_reflns_av_unetI/netI     0.0764
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13575
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        27.452
_diffrn_reflns_theta_max         27.452
_diffrn_reflns_theta_min         2.987
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker PHOTON100 CMOS diffractometer'
_diffrn_measurement_method       'ω/θ scans'
_diffrn_radiation_monochromator  'channel-cut Si(111) crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1093
_reflns_number_total             1536
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.145
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         1536
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0481
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0573P)²+17.6031P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1045
_refine_ls_wR_factor_ref         0.1203
_refine_special_details          
;Thermal parameters were refined anisotropically for all non-hydrogen atoms. 
Hydrogen atoms were placed in ideal positions and refined using the riding model.
The chemcial occupancies of O2 interacting with the Co sites (O4, O5a, and O5b) and O2 in a secondary (O6 and O7) and tertiary binding sites (O8 and O9) were initially allowed to refine freely, resulting in a chemical occupancy 100% for O2 in the first and second binding sites and 97% for O2 in the third binding site.
The terminal oxygen on O2 bound to Co was found to be disordered over two positions (O5a and O5b), so the occupancies of these two positions were refined against each other, resulting in a site occupancy of 73% for O5a and 27% for O5b. 
Disorder of all the O2 molecules interacting with the framework required displacement parameter restraints. The O-O distances for O2 in the secondary and tertiary binding sites were also restrained to be 1.21 angstroms., Twin
;
_vrf_PLAT220_Co2dobdc-O2         
;
PROBLEM: Non-Solvent Resd 1   O   Ueq(max)/Ueq(min) Range       10.0 Ratio 
RESPONSE: The interaction of the O2 molecules with the framework is so 
weak that the thermal displacement parameters of these molecules are still 
very large at 100 K.
;
_vrf_PLAT242_Co2dobdc-O2         
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         O4 Check 
RESPONSE: This corresponds to the O2 oxygen atom directly interacting with 
the Co center. The interaction of Co with this oxygen atom stabilizes it 
relative to the terminal oxygen atom, which is disordered over two 
positions. This results in much lower displacement parameters for O4 
compared to O5a and O5b.
;
_vrf_PLAT430_Co2dobdc-O2         
;
PROBLEM: Short Inter D...A Contact  O5A    ..  O8      ..       2.84 Ang.  
RESPONSE: This contact is between one position for the disordered 
terminal oxygen atom on O2 bound to Co and O2 in a tertiary binding site, 
which has very large displacement parameters. This reflects only an 
average distance between multiple relative orientations for both 
molecules. It is unlikely that these two molecules actually exist in 
relative orienations that are this close to each other.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.522(3) 0.478(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 O7-O6
 1.21 with sigma of 0.02
 O8-O9
 1.21 with sigma of 0.02
4. Rigid bond restraints
 O7, O6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O8, O9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
O7 \\sim O6: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
O9 \\sim O8: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
O4 \\sim O5A \\sim O5B: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
6. Others
 Sof(O5B)=1-FVAR(1)
 Sof(O5A)=FVAR(1)
 Fixed Sof: O9(0.97) O8(0.97)
7.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.31428(4) 0.36412(4) 0.47743(11) 0.0169(3) Uani 1 1 d . . . . .
O2 O 0.02929(17) 0.32539(17) 0.6415(5) 0.0184(9) Uani 1 1 d . . . . .
O1 O 0.25231(17) 0.31108(17) 0.6705(5) 0.0191(9) Uani 1 1 d . . . . .
O3 O 0.07257(18) 0.30239(18) 0.4047(5) 0.0201(9) Uani 1 1 d . . . . .
O4 O 0.3156(4) 0.4454(3) 0.5892(8) 0.0476(14) Uani 1 1 d . U . . .
C4 C 0.0716(3) 0.3183(3) 0.5754(8) 0.0188(13) Uani 1 1 d . . . . .
C2 C 0.1197(3) 0.3270(3) 0.7134(8) 0.0198(14) Uani 1 1 d . . . . .
C3 C 0.1649(3) 0.3181(3) 0.6431(8) 0.0222(14) Uani 1 1 d . . . . .
H3 H 0.1636 0.3079 0.5097 0.027 Uiso 1 1 calc R . . . .
C1 C 0.2115(3) 0.3229(3) 0.7540(8) 0.0234(15) Uani 1 1 d . . . . .
O5A O 0.2784(9) 0.4548(7) 0.590(3) 0.148(8) Uani 0.73(3) 1 d . U P A 1
O7 O 0.1689(9) 0.4822(9) 0.253(3) 0.241(9) Uani 1 1 d D U . . .
O6 O 0.1807(9) 0.4591(7) 0.367(2) 0.203(7) Uani 1 1 d D U . . .
O9 O 0.269(3) 0.567(4) 0.970(8) 0.64(3) Uani 0.97 1 d D U P . .
O8 O 0.263(2) 0.536(3) 0.829(8) 0.55(2) Uani 0.97 1 d D U P . .
O5B O 0.341(3) 0.491(2) 0.535(8) 0.20(2) Uani 0.27(3) 1 d . U P A 2

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 0.0181(5) 0.0219(5) 0.0108(4) 0.0002(3) -0.0008(3) 0.0100(4)
O2 0.021(2) 0.023(2) 0.0118(19) -0.0036(16) -0.0024(17) 0.012(2)
O1 0.022(2) 0.028(2) 0.0125(19) 0.0035(18) 0.0053(18) 0.017(2)
O3 0.024(2) 0.030(3) 0.014(2) -0.0054(18) -0.0038(18) 0.018(2)
O4 0.063(4) 0.044(4) 0.048(3) 0.002(3) 0.006(3) 0.035(4)
C4 0.019(3) 0.020(3) 0.017(3) -0.001(3) 0.000(3) 0.010(3)
C2 0.021(3) 0.025(4) 0.014(3) 0.000(3) 0.003(3) 0.013(3)
C3 0.021(3) 0.025(3) 0.016(3) 0.000(3) 0.002(3) 0.008(3)
C1 0.027(4) 0.020(3) 0.017(3) -0.001(3) 0.002(3) 0.007(3)
O5A 0.125(15) 0.120(13) 0.231(18) -0.013(11) 0.015(12) 0.085(12)
O7 0.261(16) 0.199(17) 0.211(17) -0.057(12) -0.105(14) 0.076(13)
O6 0.349(19) 0.145(11) 0.128(11) -0.012(9) 0.059(12) 0.133(11)
O9 0.41(3) 1.05(8) 0.47(7) -0.10(4) 0.02(4) 0.37(4)
O8 0.33(3) 1.03(8) 0.43(7) -0.08(4) -0.05(4) 0.45(4)
O5B 0.21(4) 0.11(3) 0.24(4) 0.04(3) 0.06(4) 0.06(3)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O2 2.081(4) 15_556 ?
Co1 O2 2.079(4) 11_556 ?
Co1 O1 2.007(4) 9_554 ?
Co1 O1 1.999(4) . ?
Co1 O3 2.025(4) 16 ?
Co1 O4 2.216(5) . ?
O2 Co1 2.079(4) 12_556 ?
O2 Co1 2.081(4) 14_456 ?
O2 C4 1.276(7) . ?
O1 Co1 2.007(4) 5 ?
O1 C1 1.360(7) . ?
O3 Co1 2.025(4) 16 ?
O3 C4 1.248(7) . ?
O4 O5A 1.099(15) . ?
O4 O5B 1.08(5) . ?
C4 C2 1.485(8) . ?
C2 C3 1.382(8) . ?
C2 C1 1.429(8) 16_556 ?
C3 H3 0.9500 . ?
C3 C1 1.375(9) . ?
C1 C2 1.429(8) 16_556 ?
O7 O6 1.117(14) . ?
O9 O8 1.20(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Co1 O2 82.67(4) 11_556 15_556 ?
O2 Co1 O4 95.18(19) 15_556 . ?
O2 Co1 O4 171.8(2) 11_556 . ?
O1 Co1 O2 80.81(15) 9_554 11_556 ?
O1 Co1 O2 82.64(15) 9_554 15_556 ?
O1 Co1 O2 80.94(15) . 15_556 ?
O1 Co1 O2 94.87(15) . 11_556 ?
O1 Co1 O1 163.43(17) . 9_554 ?
O1 Co1 O3 100.11(16) . 16 ?
O1 Co1 O3 96.24(16) 9_554 16 ?
O1 Co1 O4 91.1(2) 9_554 . ?
O1 Co1 O4 92.6(2) . . ?
O3 Co1 O2 177.91(15) 16 15_556 ?
O3 Co1 O2 95.42(15) 16 11_556 ?
O3 Co1 O4 86.59(19) 16 . ?
Co1 O2 Co1 92.49(15) 12_556 14_456 ?
C4 O2 Co1 130.0(4) . 14_456 ?
C4 O2 Co1 133.6(3) . 12_556 ?
Co1 O1 Co1 97.19(16) . 5 ?
C1 O1 Co1 125.8(3) . 5 ?
C1 O1 Co1 124.7(3) . . ?
C4 O3 Co1 124.2(4) . 16 ?
O5A O4 Co1 127.3(10) . . ?
O5B O4 Co1 128(3) . . ?
O2 C4 C2 117.3(5) . . ?
O3 C4 O2 122.7(5) . . ?
O3 C4 C2 119.9(5) . . ?
C3 C2 C4 117.3(5) . . ?
C3 C2 C1 118.5(6) . 16_556 ?
C1 C2 C4 124.2(5) 16_556 . ?
C2 C3 H3 117.9 . . ?
C1 C3 C2 124.1(5) . . ?
C1 C3 H3 117.9 . . ?
O1 C1 C2 123.7(6) . 16_556 ?
O1 C1 C3 118.9(5) . . ?
C3 C1 C2 117.4(6) . 16_556 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co1 O2 C4 O3 1.3(9) 12_556 . . . ?
Co1 O2 C4 O3 -149.9(4) 14_456 . . . ?
Co1 O2 C4 C2 33.0(7) 14_456 . . . ?
Co1 O2 C4 C2 -175.7(4) 12_556 . . . ?
Co1 O1 C1 C2 -108.6(6) . . . 16_556 ?
Co1 O1 C1 C2 24.8(8) 5 . . 16_556 ?
Co1 O1 C1 C3 72.3(7) . . . . ?
Co1 O1 C1 C3 -154.3(4) 5 . . . ?
Co1 O3 C4 O2 14.0(8) 16 . . . ?
Co1 O3 C4 C2 -169.0(4) 16 . . . ?
O2 C4 C2 C3 178.6(5) . . . . ?
O2 C4 C2 C1 -1.2(9) . . . 16_556 ?
O3 C4 C2 C3 1.5(8) . . . . ?
O3 C4 C2 C1 -178.4(6) . . . 16_556 ?
C4 C2 C3 C1 -178.3(6) . . . . ?
C2 C3 C1 O1 177.7(6) . . . . ?
C2 C3 C1 C2 -1.5(10) . . . 16_556 ?
C1 C2 C3 C1 1.5(10) 16_556 . . . ?

_shelx_res_file                  
;
    twin4.res created by SHELXL-2014/7

TITL twin4 in R-3
CELL 0.7749 25.7599 25.7599 6.8766 90 90 120
ZERR 9 0.0009 0.0009 0.0003 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SFAC C H Co O
DISP C 0.004 0.002 13.872
DISP Co 0.355 1.13 5089.307
DISP H -0 0 0.627
DISP O 0.014 0.007 40.889
UNIT 72 18 18 161.28
DFIX 1.21 O7 O6
DFIX 1.21 O8 O9
DELU O7 O6
DELU O8 O9
SIMU 0.02 0.04 1.7 O7 O6
SIMU 0.02 0.04 1.7 O9 O8
SIMU 0.04 0.08 1.7 O4 O5A O5B

L.S. 10
PLAN  20
SIZE 0.04 0.04 0.1
TEMP -273.15
BOND $H
LIST 6
MORE -1
CONF
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%./twin5.hkl">
REM </olex2.extras>

WGHT    0.057300   17.603100
BASF   0.47753
FVAR       0.22666   0.72622
CO1   3    0.314285    0.364119    0.477427    11.00000    0.01806    0.02195 =
         0.01076    0.00023   -0.00078    0.01005
O2    4    0.029289    0.325394    0.641538    11.00000    0.02065    0.02342 =
         0.01183   -0.00361   -0.00241    0.01166
O1    4    0.252306    0.311080    0.670535    11.00000    0.02245    0.02791 =
         0.01252    0.00348    0.00528    0.01673
O3    4    0.072565    0.302386    0.404718    11.00000    0.02359    0.02957 =
         0.01376   -0.00535   -0.00383    0.01835
O4    4    0.315603    0.445443    0.589201    11.00000    0.06279    0.04369 =
         0.04766    0.00221    0.00554    0.03511
C4    1    0.071632    0.318346    0.575395    11.00000    0.01943    0.02025 =
         0.01663   -0.00062   -0.00017    0.00995
C2    1    0.119657    0.327017    0.713434    11.00000    0.02138    0.02546 =
         0.01444   -0.00037    0.00271    0.01319
C3    1    0.164852    0.318081    0.643071    11.00000    0.02093    0.02489 =
         0.01595   -0.00038    0.00193    0.00784
AFIX  43
H3    2    0.163608    0.307938    0.509666    11.00000   -1.20000
AFIX   0
C1    1    0.211511    0.322949    0.754001    11.00000    0.02652    0.01998 =
         0.01734   -0.00067    0.00220    0.00676
PART 1
O5A   4    0.278362    0.454761    0.589950    21.00000    0.12502    0.12021 =
         0.23115   -0.01253    0.01508    0.08456

PART 0
O7    4    0.168887    0.482239    0.252766    11.00000    0.26125    0.19875 =
         0.21142   -0.05748   -0.10467    0.07560
O6    4    0.180721    0.459073    0.366932    11.00000    0.34884    0.14465 =
         0.12839   -0.01165    0.05895    0.13252

O9    4    0.269308    0.566548    0.969836    10.97000    0.40585    1.05302 =
         0.46958   -0.10460    0.02256    0.37432
O8    4    0.262811    0.536080    0.829040    10.97000    0.32904    1.02637 =
         0.42816   -0.07837   -0.05074    0.44944
PART 2
O5B   4    0.340716    0.490666    0.534711   -21.00000    0.21304    0.10940 =
         0.23880    0.03748    0.05636    0.05855
HKLF 5

REM  twin4 in R-3
REM R1 =  0.0481 for    1093 Fo > 4sig(Fo)  and  0.0860 for all    1536 data
REM    138 parameters refined using     34 restraints

END

WGHT      0.0574     17.6942

REM Highest difference peak  0.826,  deepest hole -0.587,  1-sigma level  0.145
Q1    1   0.1541  0.4586  0.3129  11.00000  0.05    0.83
Q2    1   0.2117  0.4853  0.2531  11.00000  0.05    0.61
Q3    1   0.2725  0.5930  0.6296  11.00000  0.05    0.55
Q4    1   0.1904  0.3438  0.7868  11.00000  0.05    0.53
Q5    1   0.2517  0.2984  0.5776  11.00000  0.05    0.52
Q6    1   0.3573  0.6080  0.8649  11.00000  0.05    0.51
Q7    1   0.2951  0.5703  0.7893  11.00000  0.05    0.51
Q8    1   0.3319  0.6409  1.1198  11.00000  0.05    0.49
Q9    1   0.2468  0.3232  0.4498  11.00000  0.05    0.49
Q10   1   0.2697  0.3027  0.4158  11.00000  0.05    0.47
Q11   1   0.2425  0.5539  0.7267  11.00000  0.05    0.46
Q12   1   0.1443  0.2862  0.7698  11.00000  0.05    0.45
Q13   1   0.3112  0.6173  0.7827  11.00000  0.05    0.45
Q14   1   0.3207  0.5593  0.9132  11.00000  0.05    0.45
Q15   1   0.2729  0.3924  0.4719  11.00000  0.05    0.44
Q16   1   0.2716  0.3178  0.8300  11.00000  0.05    0.44
Q17   1   0.2999  0.3349  0.5244  11.00000  0.05    0.44
Q18   1   0.3372  0.6236  1.0022  11.00000  0.05    0.43
Q19   1   0.1054  0.3327  0.6305  11.00000  0.05    0.42
Q20   1   0.2866  0.3332  0.6881  11.00000  0.05    0.42
;
_shelx_res_checksum              50055
_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.522(3)
2 0.478(3)






####################################################################### 
# 
# 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_Co2dobdc-CH4
_database_code_depnum_ccdc_archive 'CCDC 1530124'
_audit_update_record             
;
2017-01-28 deposited with the CCDC.
2017-04-19 downloaded from the CCDC.
;
_audit_creation_date             2016-04-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            Co2(dobdc)(CH4)2
_chemical_name_systematic        ?
_chemical_formula_moiety         'Co2 (C8 H2 O6) 2(CH4)'
_chemical_formula_sum            'C10 H10 Co2 O6'
_chemical_formula_weight         344.05
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3550 1.1300 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0140 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   25.866(5)
_cell_length_b                   25.866(5)
_cell_length_c                   6.8457(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3966.4(15)
_cell_formula_units_Z            9
_cell_measurement_reflns_used    6642
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.287
_cell_measurement_theta_min      2.974
_shelx_estimated_absorpt_T_max   0.890
_shelx_estimated_absorpt_T_min   0.730
_exptl_absorpt_coefficient_mu    2.397
_exptl_absorpt_correction_T_max  0.890
_exptl_absorpt_correction_T_min  0.679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1690 before and 0.0851 after correction.
 The Ratio of minimum to maximum transmission not present.
 The λ/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1772 before and 0.0865 after correction.
 The Ratio of minimum to maximum transmission is 0.77.
 The λ/2 correction factor is Not present

Final HKLF 4 output contains 21978 reflections, Rint = 0.1021
 (10699 with I > 3sig(I), Rint = 0.0855)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1476
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
Data was collected at Beamline 11.3.1 at the Advanced
 Light Source, Lawrence Berkeley National Laboratory using synchrotron
 radiation (lamda = 0.7749 angstroms) and a Bruker APEX-II CCD detector.

The crystal was mounted on a MiTeGen loop using a minimal amount
 of epoxy to ensure that the crystal pores remained accessible.
 The sample was then placed in a custom-made gas cell equipped
 with a borosilicate glass cap, O-ring seal, and gas loading
 valve.  The cell was evacuated under reduced pressure at
 473 K for 6 hours to remove solvent molecules filling
 the pores and bound onto the exposed Co sites within the crystal.
 After obtaining the structure of the desolvated crystal to
 confirm the absence of solvent bound onto the Co sites, the
 crystal was cooled to 298 deg C then dosed with 1 bar CH4.
 The crystal was then cooled to a final temperature of 100 K followed by data collection.
The crystal was found to be an obverse/reverse twin based on the diffraction
 pattern.  CELL_NOW was used to determine the orientation matrices
 and the domains were related by a 180 deg rotation around the
 reciprocal axis 0 1 -0.5 The integration was preformed with both
 matrices. TWINABS was used to produce a merged HKLF4 file, for
 structure solution and initial refinement, and HKLF5 file for
 final structure refinement. The HKLF5 file contained the merged
 reflections from the second component and those that overlapped with the
 first component were split into two reflections. TWINABS indicated
 the twin faction to be 52:48. The structure was solved using the
 HKLF4 file, but the best refinement was given by the HKLF5 file.  
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1021
_diffrn_reflns_av_unetI/netI     0.0714
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            21978
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         32.562
_diffrn_reflns_theta_min         3.393
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω/θ scans'
_diffrn_radiation_monochromator  'channel-cut Si(111) crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2163
_reflns_number_total             2442
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.777
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         2442
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0477
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0324P)²+13.8674P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1205
_refine_ls_wR_factor_ref         0.1271
_refine_special_details          
;Thermal parameters were refined anisotropically for all non-hydrogen atoms. 
Hydrogen atoms on the organic linker were placed in ideal positions and refined using the riding model.
The chemcial occupancy of the carbon atom of CH4 interacting with the Co sites was initially allowed to refine freely, resulting in a chemical occupancy of 110%. Thus, the chemical occupancy of the CH4 carbon atom was fixed at 100% in the final refinement.
The interaction of CH4 with Co is so weak that it unlikely to form an ordered orientation at 100 K, which explains the relatively large thermal displacement parameters on the CH4 carbon and the inability to locate electron density corresponding to the 
CH4 hydrogen atoms in the electron difference map. The CH4 hydrogen atoms were omitted from the refinement but not the formula., Twin
;
_vrf_PLAT602_Co2dobdc-CH4        
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info 
RESPONSE: The structure is of a metal-organic framework that exhibits 
one-dimensional hexagonal pores. Solvent molecules within the pores 
and coordinated onto exposed Co sites in the framework were removed 
by heating the crystal under vacuum. The crystal was then dosed with 
CH4 to characterize its interaction with the exposed Co site. 
It is likely that the pores are largely empty or filled with CH4 
in the gas phase. 
;
_vrf_PLAT043_Co2dobdc-CH4        
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       4.04 Check 
RESPONSE: Due to the weak interaction of CH4 with the Co site, CH4 does 
not order at a specific orientation even at 100 K. This prevents the 
hydrogen atoms on CH4 from being located in the electron difference map.
Consequently, the hydrogen atoms of CH4 were omitted from the refinement, 
but not the formula.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.471(2) 0.529(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.97041(2) 0.61787(2) 0.14301(6) 0.01681(14) Uani 1 1 d . . . . .
O1 O 0.91909(10) 0.64466(10) 0.0051(3) 0.0198(4) Uani 1 1 d . . . . .
O2 O 0.96898(10) 0.67286(11) 0.3628(3) 0.0218(5) Uani 1 1 d . . . . .
O3 O 0.96838(11) 0.56260(10) -0.0678(3) 0.0229(5) Uani 1 1 d . . . . .
C1 C 1.01033(15) 0.55561(14) -0.5772(4) 0.0209(6) Uani 1 1 d . . . . .
C2 C 0.99415(15) 0.54070(14) -0.3785(4) 0.0206(6) Uani 1 1 d . . . . .
C3 C 0.98405(16) 0.48547(15) -0.3073(4) 0.0222(6) Uani 1 1 d . . . . .
H3 H 0.9729 0.4758 -0.1744 0.027 Uiso 1 1 calc R . . . .
C4 C 0.98494(14) 0.57941(13) -0.2397(4) 0.0182(6) Uani 1 1 d . . . . .
C5 C 0.8628(8) 0.5158(8) 0.308(2) 0.207(7) Uani 1 1 d . . . . .

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 0.0219(2) 0.0192(2) 0.0108(2) -0.00094(13) -0.00027(14) 0.01139(17)
O1 0.0212(10) 0.0294(12) 0.0141(9) 0.0014(8) 0.0015(8) 0.0166(10)
O2 0.0222(11) 0.0316(12) 0.0142(10) -0.0064(9) -0.0043(8) 0.0154(10)
O3 0.0371(13) 0.0219(11) 0.0117(9) -0.0003(8) 0.0024(9) 0.0163(10)
C1 0.0281(16) 0.0198(14) 0.0176(13) 0.0017(11) 0.0014(12) 0.0141(13)
C2 0.0267(16) 0.0215(14) 0.0152(13) 0.0002(11) 0.0003(11) 0.0134(13)
C3 0.0321(17) 0.0236(15) 0.0135(13) -0.0004(11) 0.0023(11) 0.0159(14)
C4 0.0241(14) 0.0171(13) 0.0142(12) -0.0028(10) 0.0007(11) 0.0110(12)
C5 0.26(2) 0.224(18) 0.210(14) 0.005(14) -0.053(15) 0.179(17)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 Co1 2.9742(6) 5_655 ?
Co1 Co1 2.9740(6) 9_664 ?
Co1 O1 2.013(2) . ?
Co1 O1 1.997(2) 5_655 ?
Co1 O2 2.083(2) . ?
Co1 O2 2.070(2) 9_664 ?
Co1 O3 2.014(2) . ?
O1 Co1 1.997(2) 9_664 ?
O1 C1 1.355(4) 9_665 ?
O2 Co1 2.070(2) 5_655 ?
O2 C4 1.275(4) 9_665 ?
O3 C4 1.253(4) . ?
C1 O1 1.355(4) 5_654 ?
C1 C2 1.419(4) . ?
C1 C3 1.389(4) 10_764 ?
C2 C3 1.405(4) . ?
C2 C4 1.483(4) . ?
C3 C1 1.389(4) 10_764 ?
C3 H3 0.9500 . ?
C4 O2 1.275(4) 5_654 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Co1 Co1 Co1 112.52(2) 9_664 5_655 ?
O1 Co1 Co1 121.87(7) . 5_655 ?
O1 Co1 Co1 41.93(6) . 9_664 ?
O1 Co1 Co1 42.34(6) 5_655 5_655 ?
O1 Co1 Co1 139.89(7) 5_655 9_664 ?
O1 Co1 O1 163.32(10) 5_655 . ?
O1 Co1 O2 95.91(9) 5_655 9_664 ?
O1 Co1 O2 82.16(9) . . ?
O1 Co1 O2 81.18(9) 5_655 . ?
O1 Co1 O2 81.14(9) . 9_664 ?
O1 Co1 O3 99.75(9) 5_655 . ?
O1 Co1 O3 96.93(9) . . ?
O2 Co1 Co1 44.09(6) . 5_655 ?
O2 Co1 Co1 73.50(6) 9_664 5_655 ?
O2 Co1 Co1 96.60(7) . 9_664 ?
O2 Co1 Co1 44.45(6) 9_664 9_664 ?
O2 Co1 O2 83.18(3) 9_664 . ?
O3 Co1 Co1 137.56(7) . 5_655 ?
O3 Co1 Co1 83.99(6) . 9_664 ?
O3 Co1 O2 98.70(9) . 9_664 ?
O3 Co1 O2 177.78(10) . . ?
Co1 O1 Co1 95.73(9) 9_664 . ?
C1 O1 Co1 125.8(2) 9_665 9_664 ?
C1 O1 Co1 126.35(18) 9_665 . ?
Co1 O2 Co1 91.46(9) 5_655 . ?
C4 O2 Co1 132.3(2) 9_665 . ?
C4 O2 Co1 134.15(19) 9_665 5_655 ?
C4 O3 Co1 122.9(2) . . ?
O1 C1 C2 124.6(3) 5_654 . ?
O1 C1 C3 117.5(3) 5_654 10_764 ?
C3 C1 C2 117.9(3) 10_764 . ?
C1 C2 C4 123.8(3) . . ?
C3 C2 C1 119.2(3) . . ?
C3 C2 C4 117.0(3) . . ?
C1 C3 C2 122.9(3) 10_764 . ?
C1 C3 H3 118.6 10_764 . ?
C2 C3 H3 118.6 . . ?
O2 C4 C2 117.2(3) 5_654 . ?
O3 C4 O2 122.2(3) . 5_654 ?
O3 C4 C2 120.6(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co1 O3 C4 O2 -13.4(4) . . . 5_654 ?
Co1 O3 C4 C2 167.6(2) . . . . ?
O1 C1 C2 C3 -179.0(3) 5_654 . . . ?
O1 C1 C2 C4 3.3(5) 5_654 . . . ?
C1 C2 C3 C1 0.6(6) . . . 10_764 ?
C1 C2 C4 O2 -1.9(5) . . . 5_654 ?
C1 C2 C4 O3 177.2(3) . . . . ?
C3 C1 C2 C3 -0.5(5) 10_764 . . . ?
C3 C1 C2 C4 -178.3(3) 10_764 . . . ?
C3 C2 C4 O2 -179.7(3) . . . 5_654 ?
C3 C2 C4 O3 -0.6(5) . . . . ?
C4 C2 C3 C1 178.5(3) . . . 10_764 ?

_shelx_res_file                  
;
    twin234.res created by SHELXL-2014/7

TITL twin234 in R-3 #148
REM reset to R-3 #148
CELL 0.7749 25.8657 25.8657 6.8457 90 90 120
ZERR 9 0.0045 0.0045 0.0012 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SFAC C H Co O
DISP C 0.004 0.002 13.872
DISP Co 0.355 1.13 5089.307
DISP H -0 0 0.627
DISP O 0.014 0.007 40.889
UNIT 90 18 18 54

L.S. 4 0 0
PLAN  20
SIZE 0.05 0.05 0.14
TEMP -173(2)
BOND
MORE -1
BOND $H
CONF
fmap 2
ACTA
OMIT -2 4 0
REM <olex2.extras>
REM <HklSrc "%./twin235.hkl">
REM </olex2.extras>

WGHT    0.032400   13.867400
BASF   0.52947
FVAR       0.28224
CO1   3    0.970413    0.617869    0.143014    11.00000    0.02193    0.01921 =
         0.01077   -0.00094   -0.00027    0.01139
O1    4    0.919087    0.644660    0.005135    11.00000    0.02117    0.02936 =
         0.01413    0.00141    0.00150    0.01659
O2    4    0.968983    0.672863    0.362780    11.00000    0.02222    0.03159 =
         0.01425   -0.00636   -0.00426    0.01536
O3    4    0.968377    0.562599   -0.067826    11.00000    0.03711    0.02188 =
         0.01172   -0.00026    0.00239    0.01634
C1    1    1.010330    0.555609   -0.577186    11.00000    0.02815    0.01976 =
         0.01756    0.00174    0.00143    0.01406
C2    1    0.994155    0.540703   -0.378490    11.00000    0.02673    0.02154 =
         0.01519    0.00015    0.00027    0.01340
C3    1    0.984051    0.485470   -0.307325    11.00000    0.03207    0.02364 =
         0.01351   -0.00045    0.00227    0.01594
AFIX  43
H3    2    0.972882    0.475783   -0.174351    11.00000   -1.20000
AFIX   0
C4    1    0.984939    0.579407   -0.239708    11.00000    0.02410    0.01715 =
         0.01423   -0.00277    0.00074    0.01099

C5    1    0.862838    0.515771    0.308387    11.00000    0.26206    0.22378 =
         0.21034    0.00514   -0.05329    0.17870
HKLF 5

REM  twin234 in R-3 #148
REM R1 =  0.0477 for    2163 Fo > 4sig(Fo)  and  0.0558 for all    2442 data
REM     83 parameters refined using      0 restraints

END

WGHT      0.0324     13.8121

REM Highest difference peak  0.777,  deepest hole -0.482,  1-sigma level  0.118
Q1    1   0.8954  0.5405  0.2526  11.00000  0.05    0.78
Q2    1   1.0041  0.6378  0.0721  11.00000  0.05    0.51
Q3    1   0.8477  0.3714 -0.0672  11.00000  0.05    0.48
Q4    1   0.8968  0.4552  0.1680  11.00000  0.05    0.48
Q5    1   0.6667  0.3333  0.0079  10.33333  0.05    0.47
Q6    1   1.0047  0.6255  0.2323  11.00000  0.05    0.45
Q7    1   0.8634  0.4857  0.2985  11.00000  0.05    0.44
Q8    1   0.8402  0.5346  0.4319  11.00000  0.05    0.44
Q9    1   0.8834  0.5610  0.5030  11.00000  0.05    0.44
Q10   1   0.9502  0.6490  0.0701  11.00000  0.05    0.44
Q11   1   0.8426  0.4985  0.2118  11.00000  0.05    0.43
Q12   1   1.0466  0.5111 -0.1358  11.00000  0.05    0.43
Q13   1   1.0039  0.5663 -0.2824  11.00000  0.05    0.42
Q14   1   0.8998  0.4920  0.2852  11.00000  0.05    0.41
Q15   1   0.8226  0.5142  0.5658  11.00000  0.05    0.40
Q16   1   0.8370  0.5375  0.6507  11.00000  0.05    0.40
Q17   1   0.8335  0.5155  0.1053  11.00000  0.05    0.39
Q18   1   0.9462  0.5433 -0.0265  11.00000  0.05    0.38
Q19   1   1.0254  0.5551 -0.4791  11.00000  0.05    0.38
Q20   1   0.9696  0.6487  0.4026  11.00000  0.05    0.36
;
_shelx_res_checksum              79153
_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.471(2)
2 0.529(2)






####################################################################### 
# 
# 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_Co2dobdc-COB
_database_code_depnum_ccdc_archive 'CCDC 1530125'
_audit_update_record             
;
2017-01-28 deposited with the CCDC.
2017-04-19 downloaded from the CCDC.
;
_audit_creation_date             2016-06-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            Co2(dobdc)(CO)1.19
_chemical_name_systematic        ?
_chemical_formula_moiety         '(Co2 C8 H2 O6) 1.19(C O)'
_chemical_formula_sum            'C9.19 H2 Co2 O7.19'
_chemical_formula_weight         345.19
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3550 1.1300 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0140 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   25.853(3)
_cell_length_b                   25.853(3)
_cell_length_c                   6.8494(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3964.6(9)
_cell_formula_units_Z            9
_cell_measurement_reflns_used    8223
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.355
_cell_measurement_theta_min      3.392
_shelx_estimated_absorpt_T_max   0.910
_shelx_estimated_absorpt_T_min   0.699
_exptl_absorpt_coefficient_mu    2.407
_exptl_absorpt_correction_T_max  0.910
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1437 before and 0.0868 after correction.
 The Ratio of minimum to maximum transmission not present.
 The λ/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1405 before and 0.0840 after correction.
 The Ratio of minimum to maximum transmission is 0.74.
 The λ/2 correction factor is Not present

Final HKLF 4 output contains 24665 reflections, Rint = 0.0844
 (12621 with I > 3sig(I), Rint = 0.0747)
;
_exptl_special_details           
;
Data was collected at Beamline 11.3.1 at the Advanced
 Light Source, Lawrence Berkeley National Laboratory using synchrotron
 radiation (lamda = 0.7749 angstroms) and a Bruker APEX-II CCD detector.

The crystal was mounted on a MiTeGen loop using a minimal amount
 of epoxy to ensure that the crystal pores remained accessible.
 The sample was then placed in a custom-made gas cell equipped
 with a borosilicate glass cap, O-ring seal, and gas loading
 valve.  The cell was evacuated under reduced pressure at
 453 K for 4 hours to remove solvent molecules filling
 the pores and bound onto the exposed Co sites within the crystal.
 After obtaining the structure of the desolvated crystal to
 confirm the absence of solvent bound onto the Co sites, the
 crystal was cooled to 298 deg C then dosed with around 1 bar CO.
 The crystal was then cooled to a final temperature of 100 K followed by data collection.  
The crystal was found to be an obverse/reverse twin based on the diffraction
 pattern.  CELL_NOW was used to determine the orientation matrices
 and the domains were related by a 180 deg rotation around the
 reciprocal axis 0 1 1. The integration was preformed with both
 matrices. TWINABS was used to produce a merged HKLF4 file, for
 structure solution and initial refinement, and HKLF5 file for
 final structure refinement. The HKLF5 file contained the merged
 reflections from the second component and those that overlapped with the
 first component were split into two reflections. TWINABS indicated
 the twin faction to be 51:49. The structure was solved using the
 HKLF4 file, but the best refinement was given by the HKLF5 file.  
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1518
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0844
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            24665
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         34.715
_diffrn_reflns_theta_min         3.391
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω/θ scans'
_diffrn_radiation_monochromator  'channel-cut Si(111) crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2437
_reflns_number_total             2885
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         2885
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0389
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0302P)²+2.6904P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1032
_refine_special_details          
;Thermal parameters were refined anisotropically for all non-hydrogen atoms. 
Hydrogen atoms were placed in ideal positions and refined using the riding model.
The chemcial occupancy of CO coordinated to the Co sites was allowed to refine freely then was fixed in the final refinement, resulting in a chemical occupancy of 59%., Twin
;
_vrf_PLAT602_Co2dobdc-COB        
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info 
RESPONSE: The structure is of a metal-organic framework that exhibits 
one-dimensional hexagonal pores. Solvent molecules within the pores and 
coordinated onto exposed Co sites in the framework were removed by 
heating the crystal under vacuum. The crystal was then dosed with CO to 
characterize the interaction of CO with the exposed Co site. Considering
that the CO coordinated to Co was found to only have 29% occupancy, it is 
likely that the pores are largely empty or filled with CO in the gas phase. 
;
_vrf_PLAT220_Co2dobdc-COB        
;
PROBLEM: Non-Solvent Resd 1   O   Ueq(max)/Ueq(min) Range       10.0 Ratio 
RESPONSE: This refers to the oxygen atom of CO bound to Co sites in the 
framework. The CO molecule exhibits relatively large displacement 
parameters parallel to the direction of the CO-Co bond because it is weakly 
bound to Co and does not possess any nearby atoms to stabilize the molecule 
into a single orientation.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.5681(16) 0.4319(16)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Uiso/Uaniso restraints and constraints
C5 \\sim O4: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 O4, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C5(0.59) O4(0.59)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.96921(2) 0.35229(2) 0.14382(4) 0.02214(10) Uani 1 1 d . . . . .
O2 O 1.03778(7) 0.34128(8) 0.0262(2) 0.0275(3) Uani 1 1 d . . . . .
O1 O 1.02161(8) 0.41429(7) 0.3379(2) 0.0252(3) Uani 1 1 d . . . . .
O3 O 0.96802(9) 0.40525(8) -0.0704(2) 0.0308(4) Uani 1 1 d . . . . .
C2 C 1.12612(10) 0.33960(11) -0.0463(3) 0.0245(4) Uani 1 1 d . . . . .
C3 C 1.18100(10) 0.34957(11) 0.0249(3) 0.0276(4) Uani 1 1 d . . . . .
H3 H 1.1907 0.3609 0.1578 0.033 Uiso 1 1 calc R . . . .
C1 C 1.11145(10) 0.32291(10) -0.2439(3) 0.0234(4) Uani 1 1 d . . . . .
C4 C 1.08722(9) 0.34921(10) 0.0915(3) 0.0234(4) Uani 1 1 d . . . . .
C5 C 0.8887(3) 0.3510(3) 0.2608(10) 0.0624(17) Uani 0.59 1 d . U P . .
O4 O 0.8501(6) 0.3513(9) 0.306(2) 0.294(8) Uani 0.59 1 d . U P . .

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 0.02903(16) 0.02382(15) 0.01413(14) 0.00052(9) -0.00082(10) 0.01363(12)
O2 0.0267(7) 0.0436(9) 0.0179(7) -0.0077(6) -0.0028(6) 0.0217(7)
O1 0.0407(9) 0.0264(7) 0.0149(6) -0.0019(5) 0.0000(6) 0.0217(7)
O3 0.0520(11) 0.0346(8) 0.0150(7) 0.0036(6) 0.0046(7) 0.0286(8)
C2 0.0262(10) 0.0377(12) 0.0144(9) -0.0012(8) -0.0005(7) 0.0196(9)
C3 0.0293(11) 0.0439(13) 0.0138(9) -0.0021(8) -0.0002(7) 0.0215(10)
C1 0.0256(10) 0.0337(11) 0.0156(9) -0.0005(7) 0.0001(7) 0.0183(9)
C4 0.0231(9) 0.0323(10) 0.0157(9) -0.0014(7) 0.0010(7) 0.0145(8)
C5 0.049(3) 0.089(5) 0.059(4) -0.002(3) 0.012(3) 0.042(3)
O4 0.159(9) 0.390(19) 0.371(16) -0.063(15) 0.058(9) 0.166(11)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O2 2.0922(16) . ?
Co1 O2 2.0908(16) 6_665 ?
Co1 O1 2.0161(15) 8_644 ?
Co1 O1 2.0001(15) . ?
Co1 O3 2.0178(16) . ?
Co1 C5 2.215(6) . ?
O2 Co1 2.0909(16) 8_644 ?
O2 C4 1.270(2) . ?
O1 Co1 2.0160(15) 6_665 ?
O1 C1 1.358(2) 8_645 ?
O3 C4 1.248(2) 8_644 ?
C2 C3 1.397(3) . ?
C2 C1 1.414(3) . ?
C2 C4 1.488(3) . ?
C3 H3 0.9500 . ?
C3 C1 1.383(3) 16_754 ?
C1 O1 1.359(2) 6_664 ?
C1 C3 1.383(3) 16_754 ?
C4 O3 1.248(2) 6_665 ?
C5 O4 1.046(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Co1 O2 82.453(19) 6_665 . ?
O2 Co1 C5 172.3(2) . . ?
O2 Co1 C5 94.25(19) 6_665 . ?
O1 Co1 O2 81.78(6) 8_644 6_665 ?
O1 Co1 O2 81.06(7) 8_644 . ?
O1 Co1 O2 94.85(6) . . ?
O1 Co1 O2 81.47(6) . 6_665 ?
O1 Co1 O1 163.14(7) . 8_644 ?
O1 Co1 O3 100.00(7) . . ?
O1 Co1 O3 96.72(7) 8_644 . ?
O1 Co1 C5 91.6(2) 8_644 . ?
O1 Co1 C5 91.53(19) . . ?
O3 Co1 O2 96.54(7) . . ?
O3 Co1 O2 178.30(7) . 6_665 ?
O3 Co1 C5 86.59(19) . . ?
Co1 O2 Co1 91.68(6) 8_644 . ?
C4 O2 Co1 134.04(14) . . ?
C4 O2 Co1 130.87(14) . 8_644 ?
Co1 O1 Co1 96.69(6) . 6_665 ?
C1 O1 Co1 125.76(12) 8_645 6_665 ?
C1 O1 Co1 125.85(14) 8_645 . ?
C4 O3 Co1 123.89(14) 8_644 . ?
C3 C2 C1 118.91(19) . . ?
C3 C2 C4 117.17(18) . . ?
C1 C2 C4 123.89(19) . . ?
C2 C3 H3 118.5 . . ?
C1 C3 C2 122.91(19) 16_754 . ?
C1 C3 H3 118.5 16_754 . ?
O1 C1 C2 124.09(18) 6_664 . ?
O1 C1 C3 117.72(18) 6_664 16_754 ?
C3 C1 C2 118.18(19) 16_754 . ?
O2 C4 C2 117.35(18) . . ?
O3 C4 O2 122.47(19) 6_665 . ?
O3 C4 C2 120.17(19) 6_665 . ?
O4 C5 Co1 175.7(12) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co1 O2 C4 O3 2.8(4) . . . 6_665 ?
Co1 O2 C4 O3 -150.18(18) 8_644 . . 6_665 ?
Co1 O2 C4 C2 -176.15(15) . . . . ?
Co1 O2 C4 C2 30.9(3) 8_644 . . . ?
C3 C2 C1 O1 179.6(2) . . . 6_664 ?
C3 C2 C1 C3 0.1(4) . . . 16_754 ?
C3 C2 C4 O2 178.7(2) . . . . ?
C3 C2 C4 O3 -0.2(3) . . . 6_665 ?
C1 C2 C3 C1 -0.1(4) . . . 16_754 ?
C1 C2 C4 O2 0.7(3) . . . . ?
C1 C2 C4 O3 -178.3(2) . . . 6_665 ?
C4 C2 C3 C1 -178.3(2) . . . 16_754 ?
C4 C2 C1 O1 -2.4(4) . . . 6_664 ?
C4 C2 C1 C3 178.1(2) . . . 16_754 ?

_shelx_res_file                  
;
    twin4.res created by SHELXL-2014/7

TITL twin4 in R-3 #148
REM reset to R-3 #148
CELL 0.7749 25.8529 25.8529 6.8494 90 90 120
ZERR 9 0.0028 0.0028 0.0007 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SFAC C H Co O
DISP C 0.004 0.002 13.872
DISP Co 0.355 1.13 5089.307
DISP H -0 0 0.627
DISP O 0.014 0.007 40.889
UNIT 82.68 18 18 64.68
SIMU C5 O4
RIGU O4 C5

L.S. 5 0 0
PLAN  20
SIZE 0.16 0.04 0.04
TEMP -173(2)
BOND
MORE -1
BOND $H
CONF
fmap 2
ACTA
REM <olex2.extras>
REM <HklSrc "%./twin5.hkl">
REM </olex2.extras>

WGHT    0.030200    2.690400
BASF   0.43194
FVAR       0.27892
CO1   3    0.969212    0.352293    0.143817    11.00000    0.02903    0.02382 =
         0.01413    0.00052   -0.00082    0.01363
O2    4    1.037782    0.341277    0.026214    11.00000    0.02669    0.04355 =
         0.01795   -0.00766   -0.00277    0.02173
O1    4    1.021607    0.414293    0.337928    11.00000    0.04072    0.02639 =
         0.01493   -0.00190    0.00001    0.02169
O3    4    0.968016    0.405252   -0.070440    11.00000    0.05201    0.03458 =
         0.01502    0.00363    0.00461    0.02858
C2    1    1.126119    0.339599   -0.046302    11.00000    0.02623    0.03766 =
         0.01443   -0.00122   -0.00050    0.01957
C3    1    1.180997    0.349570    0.024912    11.00000    0.02930    0.04393 =
         0.01377   -0.00212   -0.00015    0.02149
AFIX  43
H3    2    1.190655    0.360851    0.157756    11.00000   -1.20000
AFIX   0
C1    1    1.111450    0.322915   -0.243932    11.00000    0.02564    0.03373 =
         0.01555   -0.00049    0.00008    0.01829
C4    1    1.087216    0.349210    0.091475    11.00000    0.02308    0.03225 =
         0.01572   -0.00145    0.00103    0.01446
C5    1    0.888671    0.350957    0.260792    10.59000    0.04879    0.08903 =
         0.05898   -0.00201    0.01172    0.04174
O4    4    0.850144    0.351279    0.305671    10.59000    0.15904    0.39024 =
         0.37056   -0.06328    0.05801    0.16642
HKLF 5

REM  twin4 in R-3 #148
REM R1 =  0.0389 for    2437 Fo > 4sig(Fo)  and  0.0491 for all    2885 data
REM     92 parameters refined using      9 restraints

END

WGHT      0.0302      2.6895

REM Highest difference peak  0.454,  deepest hole -0.432,  1-sigma level  0.092
Q1    1   0.6667  0.3333  0.1790  10.33333  0.05    0.45
Q2    1   0.9651  0.3788  0.0301  11.00000  0.05    0.45
Q3    1   0.9970  0.3593  0.0452  11.00000  0.05    0.41
Q4    1   0.9573  0.3835 -0.1190  11.00000  0.05    0.39
Q5    1   1.0005  0.3868  0.2687  11.00000  0.05    0.38
Q6    1   1.1113  0.3509  0.0155  11.00000  0.05    0.37
Q7    1   1.0130  0.3131 -0.0789  11.00000  0.05    0.36
Q8    1   1.1534  0.3372 -0.0137  11.00000  0.05    0.36
Q9    1   0.9006  0.3872  0.2290  11.00000  0.05    0.34
Q10   1   1.0229  0.4018  0.4058  11.00000  0.05    0.34
Q11   1   1.0316  0.4269  0.2341  11.00000  0.05    0.34
Q12   1   1.0219  0.4346  0.3881  11.00000  0.05    0.31
Q13   1   0.8035  0.3709  0.0199  11.00000  0.05    0.31
Q14   1   0.9383  0.3459  0.2651  11.00000  0.05    0.31
Q15   1   0.7709  0.3474 -0.1574  11.00000  0.05    0.31
Q16   1   0.8777  0.3784 -0.2451  11.00000  0.05    0.30
Q17   1   1.0278  0.4316  0.0973  11.00000  0.05    0.30
Q18   1   0.8713  0.3451  0.2105  11.00000  0.05    0.29
Q19   1   0.7172  0.3340  0.3661  11.00000  0.05    0.28
Q20   1   1.1098  0.2884 -0.0478  11.00000  0.05    0.28
;
_shelx_res_checksum              24079
_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.5681(16)
2 0.4319(16)





