# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_hp_0_60gpa
_database_code_depnum_ccdc_archive 'CCDC 1845702'
_audit_update_record             
;
2018-05-28 deposited with the CCDC.
2018-07-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_hp_0_60gpa          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.738 Why?
RESPONSE: The data come from studies of high-pressure studies and are limited by the DAC opening angle
;
_vrf_PLAT305_hp_0_60gpa          
;
PROBLEM: Isolated Hydrogen Atom   (Outside Bond Range ??)        H1A Check
RESPONSE: Dma H-atoms were located also by using difference Fourier map therfore they can differ from the ideal positions.
;
_vrf_PLAT413_hp_0_60gpa          
;
PROBLEM: Short Inter XH3 .. XHn     H2       ..H2               1.35 Ang.
RESPONSE: Dma amine in framework is strongly disordered so exact location of H-atoms was difficult
;
_vrf_PLAT415_hp_0_60gpa          
;
PROBLEM: Short Inter D-H..H-X       H1A      ..H2               1.55 Ang.
RESPONSE: The guest is disordered in the three positions which results in short contacts between other H atoms
;
_vrf_PLAT417_hp_0_60gpa          
;
PROBLEM: Short Inter D-H..H-D       H1A      ..H1A              1.21 Ang.
RESPONSE: The guest is disordered in the three positions which results in short contacts between other H atoms
;

_audit_creation_date             2018-05-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;

# CHEMICAL DATA 

_chemical_name_common            DmaNiFor3
_chemical_name_systematic        
;
 catena-(dimethylammonium tris(μ₂-formato)-nickel(ii))
;
_chemical_formula_moiety         '(C3 H3 Ni1 O6 1-)n,n(C2 H8 N1 1+))'
_chemical_formula_sum            'C5 H15 N Ni O6'
_chemical_formula_weight         243.88
_chemical_melting_point          ?
_chemical_oxdiff_formula         C15H9N9Ni3O18
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'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-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'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+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-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+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-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+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'

_cell_length_a                   8.0794(7)
_cell_length_b                   8.0794(7)
_cell_length_c                   21.859(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1235.7(2)
_cell_formula_units_Z            6.00012
_cell_measurement_reflns_used    1337
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.7130
_cell_measurement_theta_min      5.0200
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.356
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.966
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_preparation       DMF
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.209
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 Data were collected at room temperature and pressure of 0.60(2) GPa
 (600000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique.
 Pressure was determined by monitoring the shift of the ruby
 R1-fluorescence line.
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?

# APARATURE DETAILS

_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 0.738
_diffrn_reflns_Laue_measured_fraction_max 0.637
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            1981
_diffrn_reflns_point_group_measured_fraction_full 0.738
_diffrn_reflns_point_group_measured_fraction_max 0.637
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.523
_diffrn_reflns_theta_min         5.047
_diffrn_ambient_temperature      293(2)
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         600000
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0593
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.738
_diffrn_measured_fraction_theta_max 0.637
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   35.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   35.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   35.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   35.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0636837000
_diffrn_orient_matrix_UB_12      -0.0699278000
_diffrn_orient_matrix_UB_13      -0.0210198000
_diffrn_orient_matrix_UB_21      -0.0782982000
_diffrn_orient_matrix_UB_22      -0.0001605000
_diffrn_orient_matrix_UB_23      0.0146917000
_diffrn_orient_matrix_UB_31      0.0092844000
_diffrn_orient_matrix_UB_32      0.0734047000
_diffrn_orient_matrix_UB_33      -0.0199212000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                206
_reflns_number_total             225
_reflns_odcompleteness_completeness 62.15
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.46
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       0.007(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.861
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     35
_refine_ls_number_reflns         225
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0263
_refine_ls_restrained_S_all      0.857
_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)+(0.0905P)²+1.2323P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0892
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N1_$1-C2
 1.402 with sigma of 0.005
 N1-H1A \\sim C2-H2
 with sigma of 0.02
3. Others
 Fixed Sof: N1(0.16667)
;

#ATOMS POSITIONS

_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_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
Ni1 Ni 0.0000 0.0000 0.0000 0.0160(5) Uani 1 6 d S T P . .
C1 C 0.1274(5) -0.2060(5) 0.0833 0.0219(8) Uani 1 2 d S T P . .
H1 H 0.262(5) -0.071(5) 0.0833 0.026 Uiso 1 2 d RS T P . .
O1 O -0.0083(2) -0.2153(2) 0.05333(9) 0.0250(6) Uani 1 1 d . . . . .
N1 N 0.3333 -0.4191(14) -0.0833 0.034(3) Uani 0.3333 2 d DS T P . .
C2 C 0.3333 -0.3333 -0.0277(3) 0.051(2) Uani 1 3 d DS T P . .
H2 H 0.229(6) -0.351(9) -0.016(3) 0.074(16) Uiso 1 1 d D . . . .
H1A H 0.419(9) -0.445(11) -0.080(8) 0.17(6) Uiso 1 1 d 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
Ni1 0.0161(6) 0.0161(6) 0.0157(8) 0.000 0.000 0.0081(3)
C1 0.0216(14) 0.0216(14) 0.024(2) 0.0006(6) -0.0006(6) 0.0117(14)
O1 0.0239(10) 0.0238(11) 0.0265(16) 0.0049(6) -0.0033(6) 0.0113(7)
N1 0.018(5) 0.021(4) 0.062(10) 0.003(3) 0.006(6) 0.009(2)
C2 0.056(4) 0.056(4) 0.040(6) 0.000 0.000 0.0279(18)

_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
Ni1 O1 2.0671(16) 20 ?
Ni1 O1 2.0671(16) 3 ?
Ni1 O1 2.0671(16) 21 ?
Ni1 O1 2.0672(16) . ?
Ni1 O1 2.0671(16) 19 ?
Ni1 O1 2.0671(16) 2 ?
C1 O1 1.247(2) . ?
C1 O1 1.247(2) 18_544 ?
N1 N1 1.20(2) 12_544 ?
N1 N1 1.20(2) 2_545 ?
N1 C2 1.399(5) . ?
N1 C2 1.399(5) 10_444 ?
C2 N1 1.399(5) 2_545 ?
C2 N1 1.399(5) 12_544 ?

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 Ni1 O1 180.00(12) 20 2 ?
O1 Ni1 O1 88.68(7) 3 19 ?
O1 Ni1 O1 91.32(7) 20 19 ?
O1 Ni1 O1 91.32(7) 21 19 ?
O1 Ni1 O1 91.31(7) 2 . ?
O1 Ni1 O1 91.31(7) 3 . ?
O1 Ni1 O1 88.68(7) 20 3 ?
O1 Ni1 O1 91.32(7) 20 21 ?
O1 Ni1 O1 91.32(7) 2 3 ?
O1 Ni1 O1 88.69(7) 20 . ?
O1 Ni1 O1 180.00(10) 21 3 ?
O1 Ni1 O1 88.68(7) 2 21 ?
O1 Ni1 O1 88.69(7) 21 . ?
O1 Ni1 O1 88.68(7) 2 19 ?
O1 Ni1 O1 180.0 19 . ?
O1 C1 O1 123.9(3) . 18_544 ?
C1 O1 Ni1 126.02(19) . . ?
N1 N1 N1 60.0 12_544 2_545 ?
N1 N1 C2 64.6(4) 12_544 . ?
N1 N1 C2 64.6(4) 12_544 10_444 ?
N1 N1 C2 64.6(4) 2_545 10_444 ?
N1 N1 C2 64.6(4) 2_545 . ?
C2 N1 C2 120.7(10) . 10_444 ?
N1 C2 N1 50.8(9) . 12_544 ?
N1 C2 N1 50.8(9) 2_545 . ?
N1 C2 N1 50.8(9) 2_545 12_544 ?

_iucr_refine_instructions_details 
;
TITL a in R-3c #167
REM reset to R-3c #167
CELL 0.71073 8.079354 8.079354 21.858761 90 90 120
ZERR 6.00012 0.000666 0.000666 0.002539 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -Y+X,-Y,0.5-Z
SYMM -X,-X+Y,0.5-Z
SYMM +Y,+X,0.5-Z
SFAC C H N Ni O
UNIT 30 90 6 6 36
EQIV $1 0.667+Y,-0.667+X,-0.167-Z
DFIX 1.402 0.005 N1_$1 C2
SADI N1 H1a C2 H2
 
L.S. 44
PLAN  10
BOND
fmap 2
acta
OMIT 7 2 8
OMIT 7 1 6
OMIT 7 0 4
OMIT 1 1 3
OMIT 4 2 -22
OMIT -7 9 8
REM <olex2.extras>
REM <HklSrc "%.\\hp_0_60GPa.hkl">
REM </olex2.extras>
 
WGHT    0.090500    1.232300
EXTI    0.007497
FVAR       5.29970
NI1   4    0.000000    0.000000    0.000000    10.16667    0.01613    0.01613 =
         0.01569    0.00000    0.00000    0.00806
C1    1    0.127374   -0.205959    0.083333    10.50000    0.02162    0.02162 =
         0.02363    0.00058   -0.00058    0.01171
H1    2    0.262366   -0.070967    0.083333    10.50000   -1.20000
O1    5   -0.008284   -0.215309    0.053334    11.00000    0.02388    0.02382 =
         0.02651    0.00489   -0.00331    0.01130
N1    3    0.333333   -0.419067   -0.083333    10.16667    0.01806    0.02109 =
         0.06228    0.00296    0.00592    0.00903
C2    1    0.333333   -0.333333   -0.027713    10.33333    0.05584    0.05584 =
         0.04041    0.00000    0.00000    0.02792
H2    2    0.228949   -0.351353   -0.015925    11.00000    0.07381
H1A   2    0.418982   -0.445208   -0.080034    11.00000    0.16833
HKLF 4
 
REM  a in R-3c #167
REM R1 =  0.0263 for     206 Fo > 4sig(Fo)  and  0.0284 for all     225 data
REM     35 parameters refined using      2 restraints
 
END  
     
WGHT      0.0509      0.0100 

REM Highest difference peak  0.352,  deepest hole -0.316,  1-sigma level  0.083
Q1    1   0.0399  0.0887  0.0387  11.00000  0.05    0.35
Q2    1  -0.0721 -0.3083  0.0386  11.00000  0.05    0.29
Q3    1  -0.0841 -0.1826  0.0204  11.00000  0.05    0.28
Q4    1   0.0000  0.0000  0.0676  10.33333  0.05    0.25
Q5    1   0.3333 -0.3333  0.0524  10.33333  0.05    0.25
Q6    1   0.0352 -0.1828  0.0163  11.00000  0.05    0.24
Q7    1   0.0148 -0.1194  0.0853  11.00000  0.05    0.24
Q8    1  -0.0682 -0.2389  0.1175  11.00000  0.05    0.23
Q9    1   0.3333 -0.3333 -0.0833  10.16667  0.05    0.22
Q10   1   0.1150 -0.2830  0.0857  11.00000  0.05    0.21

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0263 for 206 Fo > 4sig(Fo) and 0.0284 for all 2234 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.35, deepest hole -0.32
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0284
  REM R1_gt = 0.0263
  REM wR_ref = 0.0892
  REM GOOF = 0.861
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 2234
  REM Reflections_gt = 206
  REM Parameters = n/a
  REM Hole = -0.32
  REM Peak = 0.35
  REM Flack = n/a

  
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.764
_oxdiff_exptl_absorpt_empirical_full_min 0.737
####################################################################### 
# 
# 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_hp_3_34gpa
_database_code_depnum_ccdc_archive 'CCDC 1845708'
_audit_update_record             
;
2018-05-28 deposited with the CCDC.
2018-07-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_hp_3_34gpa          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.624 Why?
RESPONSE: The data comes from high-pressure measurments and it is a consequence of the used apparatus
;
_vrf_PLAT305_hp_3_34gpa          
;
PROBLEM: Isolated Hydrogen Atom   (Outside Bond Range ??)        H1A Check
RESPONSE: Dma H-atoms were located also by using difference Fourier map therfore they can differ from the ideal positions.
;
_vrf_PLAT413_hp_3_34gpa          
;
PROBLEM: Short Inter XH3 .. XHn     H2       ..H2               1.48 Ang.
RESPONSE: Dma amine in framework is strongly disordered so exact location of H-atoms was difficult
;
_vrf_PLAT414_hp_3_34gpa          
;
PROBLEM: Short Intra D-H..H-X       H1A      ..H2               1.50 Ang.
RESPONSE: The guest is disordered in the three positions which results in short contacts between other H atoms
;
_vrf_PLAT415_hp_3_34gpa          
;
PROBLEM: Short Inter D-H..H-X       H1A      ..H2               1.73 Ang.
RESPONSE: Dma amine in framework is strongly disordered so exact location of H-atoms was difficult
;
_vrf_PLAT417_hp_3_34gpa          
;
PROBLEM: Short Inter D-H..H-D       H1A      ..H1A              1.22 Ang.
RESPONSE: The guest is disordered in the three positions which results in short contacts between other H atoms
;
_vrf_PLAT031_hp_3_34gpa          
;
PROBLEM: Refined Extinction Parameter Within Range ......      1.375 Sigma
RESPONSE: Crystal used for hp studies was extremely small.
;
_vrf_PLAT415_hp_3_34gpa_2        
;
PROBLEM: Short Inter D-H..H-X       H1A      ..H2               2.09 Ang.
RESPONSE: The guest is disordered in the three positions which results in short contacts between other H atoms
;

_audit_creation_date             2018-05-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_shelxl_version_number           2013-2



# CHEMICAL DATA 

_chemical_name_common            DmaNiFor3
_chemical_name_systematic        
;
 catena-(dimethylammonium tris(μ₂-formato)-nickel(ii))
;
_chemical_formula_moiety         '(C3 H3 Ni1 O6 1-)n,n(C2 H8 N1 1+))'
_chemical_formula_sum            'C5 H15 N Ni O6'
_chemical_formula_weight         243.88
_chemical_melting_point          ?
_chemical_oxdiff_formula         C15H9N9Ni3O18
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'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-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'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+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-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+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-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+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'

_cell_length_a                   7.9580(6)
_cell_length_b                   7.9580(6)
_cell_length_c                   21.1236(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1158.52(19)
_cell_formula_units_Z            6.00012
_cell_measurement_reflns_used    1448
_cell_measurement_temperature    293(2)
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         3340000
_cell_measurement_theta_max      27.8740
_cell_measurement_theta_min      5.8220
_shelx_estimated_absorpt_T_max   0.635
_shelx_estimated_absorpt_T_min   0.582
_exptl_absorpt_coefficient_mu    2.513
_exptl_absorpt_correction_T_max  0.761
_exptl_absorpt_correction_T_min  0.749
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.097
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_preparation       DMF
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.196
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.195
_exptl_special_details           
;
 Data were collected at room temperature and pressure of 3.34(2) GPa
 (33400000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique.
 Pressure was determined by monitoring the shift of the ruby
 R1-fluorescence line.
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?

# APARATURE DETAILS

_diffrn_reflns_av_R_equivalents  0.0861
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.624
_diffrn_reflns_Laue_measured_fraction_max 0.531
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            2143
_diffrn_reflns_point_group_measured_fraction_full 0.624
_diffrn_reflns_point_group_measured_fraction_max 0.531
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.556
_diffrn_reflns_theta_min         5.888
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0593
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.624
_diffrn_measured_fraction_theta_max 0.531
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 phi    -35.00   19.75   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
   0.0000  -30.0000    0.0000     -     73

#__ type_ start__ end____ width___ exp.time_
  2 phi    140.00  200.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
   0.0000  -30.0000    0.0000     -     80

#__ type_ start__ end____ width___ exp.time_
  3 phi    160.00  217.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
   0.0000   30.0000    0.0000     -     76

#__ type_ start__ end____ width___ exp.time_
  4 phi    -20.00   34.75   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
   0.0000   30.0000    0.0000     -     73

#__ type_ start__ end____ width___ exp.time_
  5 omega  -24.00   24.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   39.4600  -12.9000 64

#__ type_ start__ end____ width___ exp.time_
  6 omega  -24.00   24.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   39.4600  167.1000 64

#__ type_ start__ end____ width___ exp.time_
  7 omega  -50.00   10.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   39.4600  167.1000 80

#__ type_ start__ end____ width___ exp.time_
  8 omega  -50.00   10.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   39.4600  -12.9000 80

#__ type_ start__ end____ width___ exp.time_
  9 omega  -64.00   -8.50   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   81.4000  -28.9000 74

#__ type_ start__ end____ width___ exp.time_
 10 omega  -64.00   -8.50   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   81.4000  151.1000 74

#__ type_ start__ end____ width___ exp.time_
 11 omega  -19.00    8.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   81.4000  151.1000 36

#__ type_ start__ end____ width___ exp.time_
 12 omega  -19.00    8.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   81.4000  -28.9000 36

#__ type_ start__ end____ width___ exp.time_
 13 omega  -43.00  -21.25   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  134.6000  -56.9000 29

#__ type_ start__ end____ width___ exp.time_
 14 omega  -43.00  -21.25   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  134.6000  123.1000 29

#__ type_ start__ end____ width___ exp.time_
 15 omega  -90.00  -36.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000  134.6000  123.1000 72

#__ type_ start__ end____ width___ exp.time_
 16 omega  -90.00  -36.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000  134.6000  -56.9000 72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω and π scans'
_diffrn_orient_matrix_UB_11      0.0420014333
_diffrn_orient_matrix_UB_12      0.0859899667
_diffrn_orient_matrix_UB_13      0.0184431667
_diffrn_orient_matrix_UB_21      0.0933361667
_diffrn_orient_matrix_UB_22      0.0238194333
_diffrn_orient_matrix_UB_23      -0.0111887667
_diffrn_orient_matrix_UB_31      -0.0105371333
_diffrn_orient_matrix_UB_32      0.0512802333
_diffrn_orient_matrix_UB_33      -0.0257466667
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                164
_reflns_number_total             178
_reflns_odcompleteness_completeness 57.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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         0.225
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       0.0022(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     36
_refine_ls_number_reflns         178
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0280
_refine_ls_restrained_S_all      1.183
_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)+(0.0162P)²+7.5651P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0643
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Restrained distances
 C2-N1
 1.378 with sigma of 0.005
 N1-H1A \\sim C2-H2
 with sigma of 0.02
2. Others
 Fixed Sof: N1(0.16667)
;

#ATOMS POSITIONS

_atom_sites_solution_hydrogens   difmap
_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
Ni1 Ni 0.0000 0.0000 0.0000 0.0123(5) Uani 1 6 d S T P . .
C1 C 0.1196(7) -0.2138(7) 0.0833 0.0175(11) Uani 1 2 d S T P . .
O1 O -0.0194(3) -0.2214(3) 0.05381(11) 0.0198(7) Uani 1 1 d . . . . .
N1 N 0.2541(14) -0.3333 -0.0833 0.028(4) Uani 0.3333 2 d DS T P . .
C2 C 0.3333 -0.3333 -0.0253(3) 0.045(2) Uani 1 3 d DS T P . .
H1 H 0.224(6) -0.109(6) 0.0833 0.002(11) Uiso 1 2 d S T P . .
H2 H 0.221(10) -0.345(15) -0.016(5) 0.12(3) Uiso 1 1 d D . . . .
H1A H 0.141(10) -0.438(8) -0.079(5) 0.13(4) Uiso 1 1 d 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
Ni1 0.0117(6) 0.0117(6) 0.0136(7) 0.000 0.000 0.0058(3)
C1 0.015(2) 0.015(2) 0.022(3) -0.0015(10) 0.0015(10) 0.008(2)
O1 0.0172(13) 0.0176(14) 0.0250(15) 0.0031(10) -0.0030(10) 0.0090(11)
N1 0.016(5) 0.012(7) 0.054(13) 0.006(8) 0.003(4) 0.006(4)
C2 0.054(4) 0.054(4) 0.027(5) 0.000 0.000 0.0268(19)

_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
Ni1 O1 2.036(2) . ?
Ni1 O1 2.036(2) 19 ?
Ni1 O1 2.036(2) 2 ?
Ni1 O1 2.036(2) 3 ?
Ni1 O1 2.036(2) 21 ?
Ni1 O1 2.036(2) 20 ?
C1 O1 1.244(3) . ?
C1 O1 1.244(3) 18_544 ?
N1 N1 1.09(2) 2_545 ?
N1 N1 1.09(2) 3_655 ?
N1 C2 1.379(5) . ?
N1 C2 1.379(5) 10_444 ?
C2 N1 1.379(5) 3_655 ?
C2 N1 1.379(5) 2_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
O1 Ni1 O1 88.12(9) . 20 ?
O1 Ni1 O1 91.88(9) 19 21 ?
O1 Ni1 O1 88.12(9) . 21 ?
O1 Ni1 O1 88.12(9) 2 21 ?
O1 Ni1 O1 88.12(9) 20 3 ?
O1 Ni1 O1 88.12(9) 19 3 ?
O1 Ni1 O1 180.0 . 19 ?
O1 Ni1 O1 91.88(9) . 2 ?
O1 Ni1 O1 91.88(9) 20 19 ?
O1 Ni1 O1 91.88(9) . 3 ?
O1 Ni1 O1 88.12(9) 2 19 ?
O1 Ni1 O1 180.00(17) 20 2 ?
O1 Ni1 O1 91.88(9) 2 3 ?
O1 Ni1 O1 91.88(9) 20 21 ?
O1 Ni1 O1 180.00(13) 21 3 ?
O1 C1 O1 124.1(4) . 18_544 ?
C1 O1 Ni1 123.8(2) . . ?
N1 N1 N1 60.001(1) 2_545 3_655 ?
N1 N1 C2 66.7(4) 2_545 . ?
N1 N1 C2 66.7(4) 2_545 10_444 ?
N1 N1 C2 66.7(4) 3_655 10_444 ?
N1 N1 C2 66.7(4) 3_655 . ?
C2 N1 C2 125.6(10) . 10_444 ?
N1 C2 N1 46.7(8) . 2_545 ?
N1 C2 N1 46.7(8) 3_655 . ?
N1 C2 N1 46.7(8) 3_655 2_545 ?

_iucr_refine_instructions_details 
;
TITL b in R-3c #167
REM reset to R-3c #167
CELL 0.71073 7.957983 7.957983 21.123627 90 90 120
ZERR 6.00012 0.000553 0.000553 0.001704 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -Y+X,-Y,0.5-Z
SYMM -X,-X+Y,0.5-Z
SYMM +Y,+X,0.5-Z
SFAC C H N Ni O
UNIT 30 90 6 6 36
EQIV $1 -0.333-Y+X,-0.667-Y,-0.167-Z
DFIX 1.378 0.005 C2 N1
SADI N1 H1a C2 H2
 
L.S. 44
PLAN  1
FREE N1 H2_$1
FREE N1 H2
BOND
fmap 2
acta
OMIT -3 9 12
OMIT -1 2 6
OMIT -3 4 23
OMIT -2 6 22
REM <olex2.extras>
REM <HklSrc "%.\\hp_3_34GPa.hkl">
REM </olex2.extras>
 
WGHT    0.016200    7.565100
EXTI    0.002178
FVAR       4.90630
NI1   4    0.000000    0.000000    0.000000    10.16667    0.01170    0.01170 =
         0.01361    0.00000    0.00000    0.00585
C1    1    0.119559   -0.213775    0.083333    10.50000    0.01509    0.01509 =
         0.02231   -0.00150    0.00150    0.00762
O1    5   -0.019408   -0.221377    0.053808    11.00000    0.01719    0.01763 =
         0.02498    0.00313   -0.00302    0.00900
N1    3    0.254088   -0.333333   -0.083333    10.16667    0.01594    0.01162 =
         0.05359    0.00605    0.00302    0.00581
C2    1    0.333333   -0.333333   -0.025269    10.33333    0.05362    0.05362 =
         0.02684    0.00000    0.00000    0.02681
H1    2    0.224345   -0.108989    0.083333    10.50000    0.00235
H2    2    0.221129   -0.345181   -0.015771    11.00000    0.11671
H1A   2    0.141366   -0.437648   -0.078984    11.00000    0.12888
HKLF 4
 
REM  b in R-3c #167
REM R1 =  0.0280 for     164 Fo > 4sig(Fo)  and  0.0310 for all     178 data
REM     36 parameters refined using      2 restraints
 
END  
     
WGHT      0.0167      7.5491 

REM Highest difference peak  0.225,  deepest hole -0.281,  1-sigma level  0.065
Q1    1   0.0358 -0.1187  0.0364  11.00000  0.05    0.22

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0280 for 164 Fo > 4sig(Fo) and 0.0310 for all 2457 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.22, deepest hole -0.28
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0310
  REM R1_gt = 0.0280
  REM wR_ref = 0.0643
  REM GOOF = 1.191
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 2457
  REM Reflections_gt = 164
  REM Parameters = n/a
  REM Hole = -0.28
  REM Peak = 0.22
  REM Flack = n/a

  
;
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-7 0 44 0.1000 -6.9985 0.0153 44.0114 0.5191 -1.1453 -1.0586
-4 11 27 0.1000 -3.9947 11.0409 26.8813 1.2774 -0.4106 -0.0838
-4 11 -21 0.1000 -4.0072 11.0193 -21.0576 0.3909 0.1241 1.1495
-7 0 -37 0.1000 -7.0197 -0.0211 -36.8855 -0.9769 -0.2430 1.0226
-9 -7 4 0.1000 -9.0144 -7.0239 4.1598 -0.9059 -1.0552 -0.3723
7 0 37 0.1000 7.0197 0.0211 36.8855 0.9769 0.2430 -1.0226
9 7 -4 0.1000 9.0144 7.0239 -4.1598 0.9059 1.0552 0.3723
7 0 -44 0.1000 6.9985 -0.0153 -44.0114 -0.5191 1.1453 1.0586
4 -11 -27 0.1000 3.9947 -11.0409 -26.8813 -1.2774 0.4106 0.0838
4 -11 21 0.1000 4.0072 -11.0193 21.0576 -0.3909 -0.1241 -1.1495
-14 7 9 0.1000 -14.0152 7.0150 9.0452 0.1814 -1.2422 0.2745
14 -7 -9 0.1000 14.0152 -7.0150 -9.0452 -0.1814 1.2422 -0.2745

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_co_hp_0_15gpa
_database_code_depnum_ccdc_archive 'CCDC 1845709'
_audit_update_record             
;
2018-05-28 deposited with the CCDC.
2018-07-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_co_hp_0_15gpa       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.670 Why?
RESPONSE: The data comes from high-pressure measurments and it is a consequence of the used apparatus
;
_vrf_PLAT413_co_hp_0_15gpa       
;
PROBLEM: Short Inter XH3 .. XHn     H2       ..H2               1.10 Ang.
RESPONSE: Dma H-atoms were located also by using difference Fourier map therfore they can differ from the ideal positions.
;

_audit_creation_date             2018-05-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;

# CHEMICAL DATA 

_chemical_name_common            DmaCoFor3
_chemical_name_systematic        
;
  catena-(dimethylammonium tris(μ₂-formato)-cobalt(ii))
;
_chemical_formula_moiety         'C3 H3 Co1 O6 1-)n,n(C2 H8 N1 1+))'
_chemical_formula_sum            'C5 H12 Co N O6'
_chemical_formula_weight         241.08
_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 0.0033 0.0016 '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 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'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-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'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+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-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+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-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+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'

_cell_length_a                   8.1727(8)
_cell_length_b                   8.1727(8)
_cell_length_c                   22.176(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1282.8(3)
_cell_formula_units_Z            6.00012
_cell_measurement_reflns_used    1295
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.277
_cell_measurement_theta_min      4.784
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.006
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.7793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.873
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_preparation       DMF
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 Data were collected at room temperature and pressure of 0.15(2) GPa
 (150000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique.
 Pressure was determined by monitoring the shift of the ruby
 R1-fluorescence line.
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?

# APARATURE DETAILS

_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.670
_diffrn_reflns_Laue_measured_fraction_max 0.662
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            1817
_diffrn_reflns_point_group_measured_fraction_full 0.670
_diffrn_reflns_point_group_measured_fraction_max 0.662
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.277
_diffrn_reflns_theta_min         4.989
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 15.9452
_diffrn_measured_fraction_theta_full 0.670
_diffrn_measured_fraction_theta_max 0.662
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                147
_reflns_number_total             194
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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         0.359
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.000
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     35
_refine_ls_number_reflns         194
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0376
_refine_ls_restrained_S_all      5.777
_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)+(0.0263P)²+4.5943P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0788
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Restrained distances
 C2-H2
 0.98 with sigma of 0.02
 H1A-C2
 1.8 with sigma of 0.02
 H1A-N1
 1 with sigma of 0.02
 C2_$1-C2
 2.312 with sigma of 0.003
 N1-C2
 1.449 with sigma of 0.001
2. Others
 Fixed Sof: N1(0.16665) H1A(0.5)
 Fixed U13: Co1(0) C2(0)
 Fixed U23: Co1(0) C2(0)
 Fixed X: Co1(0) N1(0.749499) C2(0.6666)
 Fixed Y: Co1(0) C2(0.333301)
 Fixed Z: Co1(0) C1(0.083301) N1(0.083301)
;


#ATOMS POSITIONS

_atom_sites_solution_hydrogens   difmap
_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 0.0000 0.0000 0.0000 0.0218(7) Uani 1 6 d S T P . .
C1 C 0.1230(11) -0.2103(11) 0.0833 0.0304(19) Uani 1 2 d S T P . .
O1 O -0.0086(5) -0.2164(4) 0.05350(16) 0.0320(10) Uani 1 1 d . . . . .
N1 N 0.7495 0.3333 0.0833 0.055(7) Uani 0.3333 2 d DS T P . .
C2 C 0.6666 0.3333 0.02762(5) 0.057(3) Uani 1 3 d DS T P . .
H2 H 0.66(4) 0.41(3) -0.004(5) 0.30(9) Uiso 1 1 d D . . . .
H1A H 0.72(12) 0.20(5) 0.080(19) 2(6) Uiso 0.5 1 d D . . . .
H1 H 0.229(9) -0.104(9) 0.0833 0.03(2) Uiso 1 2 d S T 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 0.0222(8) 0.0222(8) 0.0209(10) 0.000 0.000 0.0111(4)
C1 0.037(4) 0.037(4) 0.025(5) 0.0010(15) -0.0010(15) 0.024(5)
O1 0.031(2) 0.031(2) 0.035(2) 0.0066(15) -0.0050(15) 0.0155(19)
N1 0.042(10) 0.069(15) 0.064(18) -0.008(12) -0.004(6) 0.035(7)
C2 0.072(5) 0.072(5) 0.029(7) 0.000 0.000 0.036(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 O1 2.101(3) . ?
Co1 O1 2.101(3) 21 ?
Co1 O1 2.101(3) 2 ?
Co1 O1 2.101(3) 3 ?
Co1 O1 2.101(3) 19 ?
Co1 O1 2.101(3) 20 ?
C1 O1 1.242(5) . ?
C1 O1 1.243(5) 18_544 ?
C1 H1 0.87(7) . ?
N1 N1 1.17252(12) 2_655 ?
N1 N1 1.17253(11) 3_665 ?
N1 C2 1.4085(9) . ?
N1 C2 1.4093(9) 17_654 ?
N1 H1A 1.00(2) . ?
C2 N1 1.4080(9) 3_665 ?
C2 N1 1.4082(9) 2_655 ?
C2 H2 0.98(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
O1 Co1 O1 88.75(14) . 20 ?
O1 Co1 O1 91.25(14) 20 21 ?
O1 Co1 O1 180.0 . 19 ?
O1 Co1 O1 91.25(14) 21 19 ?
O1 Co1 O1 88.75(14) 2 21 ?
O1 Co1 O1 180.00(16) 21 3 ?
O1 Co1 O1 88.75(14) . 21 ?
O1 Co1 O1 91.25(14) . 2 ?
O1 Co1 O1 91.25(14) 2 3 ?
O1 Co1 O1 88.75(14) 20 3 ?
O1 Co1 O1 88.75(14) 19 3 ?
O1 Co1 O1 180.00(16) 20 2 ?
O1 Co1 O1 88.75(14) 2 19 ?
O1 Co1 O1 91.25(14) 20 19 ?
O1 Co1 O1 91.25(14) . 3 ?
O1 C1 O1 126.2(7) . 18_544 ?
O1 C1 H1 116.9(4) . . ?
O1 C1 H1 117.0(4) 18_544 . ?
C1 O1 Co1 127.1(4) . . ?
N1 N1 N1 59.999(1) 2_655 3_665 ?
N1 N1 C2 65.378(17) 3_665 . ?
N1 N1 C2 65.388(17) 2_655 . ?
N1 N1 C2 65.442(17) 3_665 17_654 ?
N1 N1 C2 65.432(17) 2_655 17_654 ?
N1 N1 H1A 139(10) 2_655 . ?
N1 N1 H1A 80(10) 3_665 . ?
C2 N1 C2 122.56(4) . 17_654 ?
C2 N1 H1A 95.2(19) . . ?
C2 N1 H1A 103(10) 17_654 . ?
N1 C2 N1 49.20(3) 2_655 . ?
N1 C2 N1 49.20(3) 3_665 . ?
N1 C2 N1 49.21(3) 3_665 2_655 ?
N1 C2 H2 140(10) 3_665 . ?
N1 C2 H2 107(10) 2_655 . ?
N1 C2 H2 145(10) . . ?

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
O1 C1 O1 Co1 -177.5(3) 18_544 . . . ?
N1 N1 C2 N1 -66.731(10) 2_655 . . 3_665 ?
N1 N1 C2 N1 66.731(10) 3_665 . . 2_655 ?
C2 N1 C2 N1 33.364(5) 17_654 . . 2_655 ?
C2 N1 C2 N1 -33.367(5) 17_654 . . 3_665 ?

_iucr_refine_instructions_details 
;
TITL a in R-3c #167
REM reset to R-3c #167
CELL 0.71073 8.1727 8.1727 22.1759 90 90 120
ZERR 6.00012 0.0008 0.0008 0.0035 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -Y+X,-Y,0.5-Z
SYMM -X,-X+Y,0.5-Z
SYMM +Y,+X,0.5-Z
SFAC C H Co N O
UNIT 30 72 6 6 36
EQIV $1 1.333-X,0.667-X+Y,0.167-Z
 
L.S. 44
PLAN  1
BOND
MORE -1
BOND $H
CONF
fmap 2
ACTA
OMIT -5 10 0
OMIT -3 7 5
OMIT 6 4 -1
OMIT 5 2 15
OMIT 5 1 13
OMIT 5 3 -1
REM <olex2.extras>
REM <HklSrc "%.\\Co_hp_0_15GPa.hkl">
REM </olex2.extras>
 
WGHT    0.017000    6.647200
EXTI    0.00000
FVAR       0.16950
CO1   3   10.000000   10.000000   10.000000    10.16667    0.02223    0.02223 =
         0.02094   10.00000  -10.00000    0.01111
C1    1    0.123002   -0.210331   10.083301    10.50000    0.03678    0.03678 =
         0.02505    0.00102   -0.00102    0.02392
O1    5   -0.008638   -0.216360    0.053495    11.00000    0.03066    0.03091 =
         0.03461    0.00655   -0.00499    0.01545
N1    4   10.749499    0.333333   10.083301    10.16665    0.04211    0.06937 =
         0.06358   -0.00836   -0.00418    0.03469
C2    1   10.666600   10.333301    0.027615    10.33333    0.07158    0.07158 =
         0.02908   10.00000  -10.00000    0.03579
H2    2    0.658669    0.413373   -0.003839    11.00000    0.30363
H1A   2    0.723843    0.200523    0.079742    10.50000    2.00000
H1    2    0.229209   -0.104124    0.083333    10.50000    0.03352
HKLF 4
 
REM  a in R-3c #167
REM R1 =  0.0375 for     147 Fo > 4sig(Fo)  and  0.0633 for all     194 data
REM     35 parameters refined using      5 restraints
 
END  
     
WGHT      0.0132      7.2173 

REM Highest difference peak  0.368,  deepest hole -0.293,  1-sigma level  0.080
Q1    1   0.2309  0.0118  0.0511  11.00000  0.05    0.37

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0375 for 147 Fo > 4sig(Fo) and 0.0633 for all 2041 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.37, deepest hole -0.29
  REM Mean Shift 0.0000, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0633
  REM R1_gt = 0.0375
  REM wR_ref = 0.0722
  REM GOOF = 1.185
  REM Shift_max = 0.000
  REM Shift_mean = 0.000
  REM Reflections_all = 2041
  REM Reflections_gt = 147
  REM Parameters = n/a
  REM Hole = -0.29
  REM Peak = 0.37
  REM Flack = n/a

  
;
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_co_hp_0_52gpa
_database_code_depnum_ccdc_archive 'CCDC 1845711'
_audit_update_record             
;
2018-05-28 deposited with the CCDC.
2018-07-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_co_hp_0_52gpa       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.808 Why?
RESPONSE: The data come from studies of high-pressure studies and are limited by the DAC opening angle
;
_vrf_PLAT305_co_hp_0_52gpa       
;
PROBLEM: Isolated Hydrogen Atom   (Outside Bond Range ??)        H1A Check
RESPONSE: Dma H-atoms were located also by using difference Fourier map therfore they can differ from the ideal positions.
;
_vrf_PLAT413_co_hp_0_52gpa       
;
PROBLEM: Short Inter XH3 .. XHn     H2       ..H2               1.60 Ang.
RESPONSE: Dma amine in framework is strongly disordered so exact location of H-atoms was difficult
;
_vrf_PLAT415_co_hp_0_52gpa       
;
PROBLEM: Short Inter D-H..H-X       H1A      ..H2               1.20 Ang.
RESPONSE: The guest is disordered in the three positions which results in short contacts between other H atoms
;
_vrf_PLAT417_co_hp_0_52gpa       
;
PROBLEM: Short Inter D-H..H-D       H1A      ..H1A              1.47 Ang.
RESPONSE: Dma amine in framework is strongly disordered so exact location of H-atoms was difficult
;
_vrf_PLAT414_co_hp_0_52gpa       
;
PROBLEM: Short Intra D-H..H-X       H1A      ..H2               1.80 Ang.
RESPONSE: The dma H-atoms were located also by using difference Fourier map therfore they can differ from the ideal positions.
;

_audit_creation_date             2018-05-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;

# CHEMICAL DATA 

_chemical_name_common            DmaCoFor3
_chemical_name_systematic        
;
  catena-(dimethylammonium tris(μ₂-formato)-cobalt(ii))
;
_chemical_formula_moiety         'C3 H3 Co1 O6 1-)n,n(C2 H8 N1 1+))'
_chemical_formula_sum            'C5 H15 Co N O6'
_chemical_formula_weight         244.10
_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 0.0033 0.0016 '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 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'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-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'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+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-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+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-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+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'

_cell_length_a                   8.161(5)
_cell_length_b                   8.161(5)
_cell_length_c                   22.00(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1269(2)
_cell_formula_units_Z            6.00012
_cell_measurement_reflns_used    1079
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.135
_cell_measurement_theta_min      4.649
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.029
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.7793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.916
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_preparation       DMF
_exptl_crystal_F_000             762
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 Data were collected at room temperature and pressure of 0.52(2) GPa
 (520000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique.
 Pressure was determined by monitoring the shift of the ruby
 R1-fluorescence line.
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?

# APARATURE DETAILS

_diffrn_reflns_av_R_equivalents  0.1206
_diffrn_reflns_av_unetI/netI     0.1001
_diffrn_reflns_Laue_measured_fraction_full 0.808
_diffrn_reflns_Laue_measured_fraction_max 0.779
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            1179
_diffrn_reflns_point_group_measured_fraction_full 0.808
_diffrn_reflns_point_group_measured_fraction_max 0.779
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.135
_diffrn_reflns_theta_min         4.996
_diffrn_ambient_temperature      293(2)
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         520000
_diffrn_detector_area_resol_mean 16.1682
_diffrn_measured_fraction_theta_full 0.808
_diffrn_measured_fraction_theta_max 0.779
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                128
_reflns_number_total             222
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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         0.556
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       0.0000
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     33
_refine_ls_number_reflns         222
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.1407
_refine_ls_R_factor_gt           0.0777
_refine_ls_restrained_S_all      6.868
_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)+(0.0498P)²+21.4796P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1502
_refine_ls_wR_factor_ref         0.1887
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 H1A-N1
 0.95 with sigma of 0.02
 C2-H1A
 1.6 with sigma of 0.02
 C2-H2
 0.95 with sigma of 0.02
 C2_$1-C2
 2.481 with sigma of 0.001
 N1_$2-N1
 1.1 with sigma of 0.001
 C2_$3-N1_$2
 1.35 with sigma of 0.001
3. Rigid body (RIGU) restrains
 C1, O1, Co1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: N1(0.16665)
 Fixed U13: Co1(0) C2(0)
 Fixed U23: Co1(0) C2(0)
 Fixed X: Co1(0) N1(0.749499) C2(0.6666)
 Fixed Y: Co1(0) C2(0.333301)
 Fixed Z: Co1(0) C1(0.083301) N1(0.083301)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1)
;

#ATOMS POSITIONS

_atom_sites_solution_hydrogens   mixed
_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 0.0000 0.0000 0.0000 0.0536(19) Uani 1 6 d S TU P . .
C1 C 0.119(2) -0.214(2) 0.0833 0.061(4) Uani 1 2 d S TU P . .
H1 H 0.2335 -0.0999 0.0833 0.073 Uiso 1 2 calc RS T P . .
O1 O -0.0105(11) -0.2185(11) 0.0535(3) 0.066(3) Uani 1 1 d . U . . .
N1 N 0.7495 0.3333 0.0833 0.069(11) Uani 0.3333 2 d DS TU P . .
C2 C 0.6666 0.3333 0.02748(2) 0.076(6) Uani 1 3 d DS TU P . .
H1A H 0.859(6) 0.437(12) 0.066(3) 0.13(6) Uiso 1 1 d D . . . .
H2 H 0.68(3) 0.454(13) 0.028(9) 0.17(7) Uiso 1 1 d 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 0.052(2) 0.052(2) 0.057(2) 0.000 0.000 0.0260(11)
C1 0.076(8) 0.076(8) 0.053(7) -0.004(3) 0.004(3) 0.056(9)
O1 0.063(5) 0.067(6) 0.069(4) 0.006(4) -0.006(3) 0.033(4)
N1 0.078(16) 0.06(3) 0.061(12) 0.003(9) 0.002(5) 0.030(14)
C2 0.082(10) 0.082(10) 0.064(10) 0.000 0.000 0.041(5)

_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 2.102(7) 20 ?
Co1 O1 2.102(7) . ?
Co1 O1 2.102(7) 19 ?
Co1 O1 2.102(7) 2 ?
Co1 O1 2.102(7) 21 ?
Co1 O1 2.102(7) 3 ?
C1 O1 1.232(10) . ?
C1 O1 1.233(10) 18_544 ?
N1 N1 1.1709(7) 3_665 ?
N1 N1 1.1709(7) 2_655 ?
N1 C2 1.4021(12) . ?
N1 C2 1.4034(12) 16_554 ?
N1 C2 1.4032(12) 18_544 ?
C2 N1 1.4017(12) 3_665 ?
C2 N1 1.4019(12) 2_655 ?

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 180.0(3) 20 2 ?
O1 Co1 O1 91.7(3) 21 19 ?
O1 Co1 O1 88.3(3) 21 . ?
O1 Co1 O1 91.7(3) 20 21 ?
O1 Co1 O1 88.3(3) 20 . ?
O1 Co1 O1 88.3(3) 2 21 ?
O1 Co1 O1 88.3(3) 2 19 ?
O1 Co1 O1 88.3(3) 20 3 ?
O1 Co1 O1 88.3(3) 3 19 ?
O1 Co1 O1 91.7(3) 2 3 ?
O1 Co1 O1 91.7(3) 2 . ?
O1 Co1 O1 180.0(4) 21 3 ?
O1 Co1 O1 91.7(3) 3 . ?
O1 Co1 O1 91.7(3) 20 19 ?
O1 Co1 O1 180.0 19 . ?
O1 C1 O1 127.1(16) . 18_544 ?
C1 O1 Co1 127.1(9) . . ?
N1 N1 N1 60.0 3_665 2_655 ?
N1 N1 C2 65.34(2) 3_665 16_554 ?
N1 N1 C2 65.35(2) 2_655 18_544 ?
N1 N1 C2 65.31(2) 2_655 . ?
N1 N1 C2 65.32(2) 2_655 16_554 ?
N1 N1 C2 65.30(3) 3_665 . ?
N1 N1 C2 65.33(2) 3_665 18_544 ?
C2 N1 C2 122.34(6) . 16_554 ?
C2 N1 C2 0.0 18_544 16_554 ?
C2 N1 C2 122.35(6) . 18_544 ?
N1 C2 N1 49.37(5) 3_665 2_655 ?
N1 C2 N1 49.36(5) 2_655 . ?
N1 C2 N1 49.37(5) 3_665 . ?

_iucr_refine_instructions_details 
;
TITL Co_hp_0_52GPa in R-3c #167
REM reset to R-3c #167
CELL 0.71073 8.1612 8.1612 22.0028 90 90 120
ZERR 6.00012 0.0051 0.0051 0.0215 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -Y+X,-Y,0.5-Z
SYMM -X,-X+Y,0.5-Z
SYMM +Y,+X,0.5-Z
SFAC C H Co N O
UNIT 30 90 6 6 36
EQIV $1 0.333+Y,-0.333+X,0.167-Z
EQIV $2 1-Y,+X-Y,+Z
EQIV $3 0.333-Y+X,0.667-Y,0.167-Z
RIGU C1 O1 Co1
RIGU N1 C2
 
L.S. 44
PLAN  1
BOND
fmap 2
acta
OMIT 6 2 10
OMIT 5 3 14
OMIT 2 1 -26
OMIT 7 1 -12
OMIT 2 2 21
OMIT 7 1 -12
OMIT 8 0 8
OMIT 7 1 -3
OMIT 4 2 -1
OMIT 2 1 -23
OMIT 7 1 -12
OMIT -5 7 12
OMIT 8 0 8
REM <olex2.extras>
REM <HklSrc "%.\\Co_hp_0_52GPa.hkl">
REM </olex2.extras>
 
WGHT    0.049800   21.479601
EXTI    0.00000
FVAR       0.21331
CO1   3   10.000000   10.000000   10.000000    10.16667    0.05206    0.05206 =
         0.05681   10.00000  -10.00000    0.02603
C1    1    0.119484   -0.213850   10.083301    10.50000    0.07628    0.07628 =
         0.05316   -0.00443    0.00443    0.05567
AFIX  43
H1    2    0.233469   -0.099928    0.083261    10.50000   -1.20000
AFIX   0
O1    5   -0.010521   -0.218460    0.053485    11.00000    0.06322    0.06694 =
         0.06899    0.00635   -0.00551    0.03265
 
N1    4   10.749499    0.333333   10.083301    10.16665    0.07829    0.06089 =
         0.06110    0.00311    0.00155    0.03044
C2    1   10.666600   10.333301    0.027482    10.33333    0.08203    0.08203 =
         0.06443   10.00000   10.00000    0.04102
H1A   2    0.858561    0.437467    0.066336    11.00000    0.12709
H2    2    0.676176    0.454130    0.028387    11.00000    0.16620
HKLF 4
 
REM  Co_hp_0_52GPa in R-3c #167
REM R1 =  0.0777 for     128 Fo > 4sig(Fo)  and  0.1407 for all     222 data
REM     33 parameters refined using     18 restraints
 
END  
     
WGHT      0.0520     19.3423 

REM Highest difference peak  0.556,  deepest hole -0.661,  1-sigma level  0.124
Q1    1   0.0559 -0.0453  0.0238  11.00000  0.05    0.56

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0777 for 128 Fo > 4sig(Fo) and 0.1407 for all 1389 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.56, deepest hole -0.66
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.1407
  REM R1_gt = 0.0777
  REM wR_ref = 0.1887
  REM GOOF = 1.155
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 1389
  REM Reflections_gt = 128
  REM Parameters = n/a
  REM Hole = -0.66
  REM Peak = 0.56
  REM Flack = n/a

  
;
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_hp_2_73gpa
_database_code_depnum_ccdc_archive 'CCDC 1845706'
_audit_update_record             
;
2018-05-28 deposited with the CCDC.
2018-07-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_hp_2_73gpa          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.777 Why?
RESPONSE: The data come from studies of high-pressure studies and are limited by the DAC opening angle
;
_vrf_PLAT305_hp_2_73gpa          
;
PROBLEM: Isolated Hydrogen Atom   (Outside Bond Range ??)         H1 Check
RESPONSE: Dma H-atoms were located also by using difference Fourier map therfore they can differ from the ideal positions.
;
_vrf_PLAT413_hp_2_73gpa          
;
PROBLEM: Short Inter XH3 .. XHn     H1A      ..H1A              1.47 Ang.
RESPONSE: Dma amine in framework is strongly disordered so exact location of H-atoms was difficult
;
_vrf_PLAT415_hp_2_73gpa          
;
PROBLEM: Short Inter D-H..H-X       H1       ..H1A              1.30 Ang.
RESPONSE: The guest is disordered in the three positions which results in short contacts between other H atoms
;
_vrf_PLAT417_hp_2_73gpa          
;
PROBLEM: Short Inter D-H..H-D       H1       ..H1               1.70 Ang.
RESPONSE: Dma amine in framework is strongly disordered so exact location of H-atoms was difficult
;

_audit_creation_date             2018-05-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_shelxl_version_number           2013-2



# CHEMICAL DATA 

_chemical_name_common            DmaNiFor3
_chemical_name_systematic        
;
 catena-(dimethylammonium tris(μ₂-formato)-nickel(ii))
;
_chemical_formula_moiety         '(C3 H3 Ni1 O6 1-)n,n(C2 H8 N1 1+))'
_chemical_formula_sum            'C5 H15 N Ni O6'
_chemical_formula_weight         243.88
_chemical_melting_point          ?
_chemical_oxdiff_formula         C15H9N9Ni3O18
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'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-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'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+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-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+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-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+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'

_cell_length_a                   8.0039(15)
_cell_length_b                   8.0039(15)
_cell_length_c                   21.172(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1174.6(5)
_cell_formula_units_Z            6.00012
_cell_measurement_reflns_used    1399
_cell_measurement_temperature    293(2)
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         2730000
_cell_measurement_theta_max      27.8040
_cell_measurement_theta_min      3.0010
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.478
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82841
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.069
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_preparation       DMF
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.195
_exptl_special_details           
;
 Data were collected at room temperature and pressure of 2.73(2) GPa
 (27300000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique.
 Pressure was determined by monitoring the shift of the ruby
 R1-fluorescence line.
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1359
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.777
_diffrn_reflns_Laue_measured_fraction_max 0.708
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            2117
_diffrn_reflns_point_group_measured_fraction_full 0.777
_diffrn_reflns_point_group_measured_fraction_max 0.708
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.201
_diffrn_reflns_theta_min         5.859
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0593
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.777
_diffrn_measured_fraction_theta_max 0.708
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 phi    -35.00   19.75   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
   0.0000  -30.0000    0.0000     -     73

#__ type_ start__ end____ width___ exp.time_
  2 phi    140.00  200.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
   0.0000  -30.0000    0.0000     -     80

#__ type_ start__ end____ width___ exp.time_
  3 phi    160.00  217.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
   0.0000   30.0000    0.0000     -     76

#__ type_ start__ end____ width___ exp.time_
  4 phi    -20.00   34.75   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
   0.0000   30.0000    0.0000     -     73

#__ type_ start__ end____ width___ exp.time_
  5 omega  -24.00   24.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   39.4600  -12.9000 64

#__ type_ start__ end____ width___ exp.time_
  6 omega  -24.00   24.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   39.4600  167.1000 64

#__ type_ start__ end____ width___ exp.time_
  7 omega  -50.00   10.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   39.4600  167.1000 80

#__ type_ start__ end____ width___ exp.time_
  8 omega  -50.00   10.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   39.4600  -12.9000 80

#__ type_ start__ end____ width___ exp.time_
  9 omega  -64.00   -8.50   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   81.4000  -28.9000 74

#__ type_ start__ end____ width___ exp.time_
 10 omega  -64.00   -8.50   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   81.4000  151.1000 74

#__ type_ start__ end____ width___ exp.time_
 11 omega  -19.00    8.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   81.4000  151.1000 36

#__ type_ start__ end____ width___ exp.time_
 12 omega  -19.00    8.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   81.4000  -28.9000 36

#__ type_ start__ end____ width___ exp.time_
 13 omega  -43.00  -21.25   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  134.6000  -56.9000 29

#__ type_ start__ end____ width___ exp.time_
 14 omega  -43.00  -21.25   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  134.6000  123.1000 29

#__ type_ start__ end____ width___ exp.time_
 15 omega  -90.00  -36.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000  134.6000  123.1000 72

#__ type_ start__ end____ width___ exp.time_
 16 omega  -90.00  -36.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000  134.6000  -56.9000 72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω and π scans'
_diffrn_orient_matrix_UB_11      -0.0580809000
_diffrn_orient_matrix_UB_12      -0.0845328000
_diffrn_orient_matrix_UB_13      -0.0178853000
_diffrn_orient_matrix_UB_21      -0.0838759667
_diffrn_orient_matrix_UB_22      -0.0109643333
_diffrn_orient_matrix_UB_23      0.0152471667
_diffrn_orient_matrix_UB_31      -0.0102251667
_diffrn_orient_matrix_UB_32      0.0565806667
_diffrn_orient_matrix_UB_33      -0.0238026333
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                208
_reflns_number_total             230
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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         0.787
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       0.007(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.206
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     36
_refine_ls_number_reflns         230
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0469
_refine_ls_restrained_S_all      1.203
_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)+(0.0666P)²+1.8327P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1139
_refine_ls_wR_factor_ref         0.1204
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Restrained distances
 C1-N1
 1.383 with sigma of 0.005
2. Others
 Fixed Sof: N1(0.16667)
;

#ATOMS POSITIONS

_atom_sites_solution_hydrogens   difmap
_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
Ni1 Ni -0.3333 -0.6667 0.3333 0.0181(6) Uani 1 6 d S T P . .
O1 O -0.3153(3) -0.8692(3) 0.27939(10) 0.0255(8) Uani 1 1 d . . . . .
C2 C -0.4523(6) -1.0000 0.2500 0.0217(10) Uani 1 2 d S T P . .
H2 H -0.566(8) -1.0000 0.2500 0.026 Uiso 1 2 d RS T P . .
N1 N -0.3333 -0.7467(18) 0.0833 0.032(4) Uani 0.3333 2 d DS T P . .
C1 C -0.3333 -0.6667 0.1412(4) 0.049(3) Uani 1 3 d DS T P . .
H1A H -0.252(10) -0.547(14) 0.159(5) 0.08(3) Uiso 1 1 d . . . . .
H1 H -0.417(13) -0.858(18) 0.066(8) 0.13(5) Uiso 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
Ni1 0.0160(6) 0.0160(6) 0.0222(10) 0.000 0.000 0.0080(3)
O1 0.0203(13) 0.0225(13) 0.0337(19) -0.0085(9) -0.0026(9) 0.0107(10)
C2 0.0158(17) 0.023(2) 0.028(3) 0.003(2) 0.0013(10) 0.0117(12)
N1 0.017(6) 0.023(4) 0.053(12) -0.001(4) -0.002(9) 0.008(3)
C1 0.060(5) 0.060(5) 0.026(7) 0.000 0.000 0.030(2)

_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
Ni1 O1 2.046(2) 2_445 ?
Ni1 O1 2.046(2) 32_545 ?
Ni1 O1 2.046(2) 33_445 ?
Ni1 O1 2.046(2) . ?
Ni1 O1 2.046(2) 31_435 ?
Ni1 O1 2.046(2) 3_545 ?
O1 C2 1.240(3) . ?
C2 O1 1.240(3) 4_435 ?
N1 N1 1.11(2) 2_445 ?
N1 N1 1.11(2) 3_545 ?
N1 C1 1.382(5) . ?
N1 C1 1.382(5) 16_434 ?
C1 N1 1.382(5) 2_445 ?
C1 N1 1.382(5) 3_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
O1 Ni1 O1 91.87(9) 2_445 . ?
O1 Ni1 O1 88.13(9) 3_545 32_545 ?
O1 Ni1 O1 91.87(9) 33_445 31_435 ?
O1 Ni1 O1 91.87(9) 2_445 3_545 ?
O1 Ni1 O1 88.13(9) 2_445 31_435 ?
O1 Ni1 O1 91.87(9) . 3_545 ?
O1 Ni1 O1 88.13(9) . 32_545 ?
O1 Ni1 O1 88.13(9) 2_445 33_445 ?
O1 Ni1 O1 91.87(9) 33_445 32_545 ?
O1 Ni1 O1 88.13(9) . 33_445 ?
O1 Ni1 O1 180.0 . 31_435 ?
O1 Ni1 O1 180.0 3_545 33_445 ?
O1 Ni1 O1 91.87(9) 32_545 31_435 ?
O1 Ni1 O1 180.0 2_445 32_545 ?
O1 Ni1 O1 88.13(9) 3_545 31_435 ?
C2 O1 Ni1 124.5(2) . . ?
O1 C2 O1 125.0(4) . 4_435 ?
N1 N1 N1 60.000(1) 3_545 2_445 ?
N1 N1 C1 66.3(5) 3_545 16_434 ?
N1 N1 C1 66.3(5) 2_445 . ?
N1 N1 C1 66.3(5) 2_445 16_434 ?
N1 N1 C1 66.3(5) 3_545 . ?
C1 N1 C1 124.7(13) 16_434 . ?
N1 C1 N1 47.4(11) . 3_545 ?
N1 C1 N1 47.4(11) 2_445 3_545 ?
N1 C1 N1 47.4(11) . 2_445 ?

_iucr_refine_instructions_details 
;
TITL 34 in R-3c #167
REM reset to R-3c #167
CELL 0.71073 8.003856 8.003856 21.17212 90 90 120
ZERR 6.00012 0.001524 0.001524 0.004593 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -Y+X,-Y,0.5-Z
SYMM -X,-X+Y,0.5-Z
SYMM +Y,+X,0.5-Z
SFAC C H N Ni O
UNIT 30 90 6 6 36
EQIV $1 -0.667-Y+X,-1.333-Y,0.167-Z
DFIX 1.383 0.005 C1 N1
 
L.S. 44
PLAN  1
FREE N1 H1a
FREE N1 H1a_$1
BOND
fmap 2
ACTA
OMIT 0 58
OMIT 0 2 16
OMIT 0 5 22
OMIT -1 3 20
OMIT -5 5 2
OMIT 4 0 -20
OMIT 4 1 6
OMIT 3 0 -18
OMIT 6 4 8
OMIT -4 5 24
REM <olex2.extras>
REM <HklSrc "%.\\hp_2_73GPa.hkl">
REM </olex2.extras>
 
WGHT    0.065700    1.554700
FVAR       4.97089
NI1   4   -0.333333   -0.666667    0.333333    10.16667    0.01597    0.01597 =
         0.02224    0.00000    0.00000    0.00798
O1    5   -0.315346   -0.869195    0.279392    11.00000    0.02030    0.02248 =
         0.03366   -0.00851   -0.00259    0.01067
C2    1   -0.452259   -1.000000    0.250000    10.50000    0.01582    0.02348 =
         0.02848    0.00258    0.00129    0.01174
H2    2   -0.566345   -1.000000    0.250000    10.50000   -1.20000
N1    3   -0.333333   -0.746734    0.083333    10.16667    0.01680    0.02285 =
         0.05310   -0.00088   -0.00176    0.00840
C1    1   -0.333333   -0.666667    0.141167    10.33333    0.06005    0.06005 =
         0.02552    0.00000    0.00000    0.03003
H1A   2   -0.251768   -0.546590    0.158752    11.00000    0.08115
H1    2   -0.416820   -0.858204    0.065930    11.00000    0.12816
HKLF 4
 
REM  34 in R-3c #167
REM R1 =  0.0477 for     208 Fo > 4sig(Fo)  and  0.0531 for all     230 data
REM     34 parameters refined using      1 restraints
 
END  
     
WGHT      0.0681      1.5904 

REM Highest difference peak  0.826,  deepest hole -0.498,  1-sigma level  0.129
Q1    1  -0.3931 -0.7933  0.2927  11.00000  0.05    0.83

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0477 for 208 Fo > 4sig(Fo) and 0.0531 for all 2422 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.83, deepest hole -0.50
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0531
  REM R1_gt = 0.0477
  REM wR_ref = 0.1226
  REM GOOF = 1.243
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 2422
  REM Reflections_gt = 208
  REM Parameters = n/a
  REM Hole = -0.50
  REM Peak = 0.83
  REM Flack = n/a

  
;
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_hp_1_40gpa
_database_code_depnum_ccdc_archive 'CCDC 1845703'
_audit_update_record             
;
2018-05-28 deposited with the CCDC.
2018-07-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_hp_1_40gpa          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.741 Why?
RESPONSE: The data comes from high-pressure measurments and it is a consequence of the used apparatus
;
_vrf_PLAT305_hp_1_40gpa          
;
PROBLEM: Isolated Hydrogen Atom   (Outside Bond Range ??)        H1A Check
RESPONSE: Dma H-atoms were located also by using difference Fourier map therfore they can differ from the ideal positions.
;
_vrf_PLAT413_hp_1_40gpa          
;
PROBLEM: Short Inter XH3 .. XHn     H2       ..H2               1.39 Ang.
RESPONSE: The dma H-atoms were located also by using difference Fourier map therfore they can differ from the ideal positions.
;
_vrf_PLAT415_hp_1_40gpa          
;
PROBLEM: Short Inter D-H..H-X       H1A      ..H2               1.39 Ang.
RESPONSE: The dma amine in framework is strongly disordered so exact location of H-atoms was difficult
;
_vrf_PLAT417_hp_1_40gpa          
;
PROBLEM: Short Inter D-H..H-D       H1A      ..H1A              1.38 Ang.
RESPONSE: The guest is disordered in the three positions which results in short contacts between other H atoms
;

_audit_creation_date             2018-05-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_shelxl_version_number           2013-2



# CHEMICAL DATA 

_chemical_name_common            DmaNiFor3
_chemical_name_systematic        
;
 catena-(dimethylammonium tris(μ₂-formato)-nickel(ii))
;
_chemical_formula_moiety         '(C3 H3 Ni1 O6 1-)n,n(C2 H8 N1 1+))'
_chemical_formula_sum            'C5 H15 N Ni O6'
_chemical_formula_weight         243.88
_chemical_melting_point          ?
_chemical_oxdiff_formula         C15H9N9Ni3O18
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'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-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'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+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-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+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-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+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'

_cell_length_a                   8.0395(4)
_cell_length_b                   8.0395(4)
_cell_length_c                   21.5732(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1207.55(14)
_cell_formula_units_Z            6.00012
_cell_measurement_reflns_used    1370
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.9170
_cell_measurement_theta_min      5.7780
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.411
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82841
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.012
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_preparation       DMF
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1963
_exptl_special_details           
;
 Data were collected at room temperature and pressure of 1.40(2) GPa
 (1400000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique.
 Pressure was determined by monitoring the shift of the ruby
 R1-fluorescence line.
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?

# APARATURE DETAILS

_diffrn_reflns_av_R_equivalents  0.0972
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 0.741
_diffrn_reflns_Laue_measured_fraction_max 0.659
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            1956
_diffrn_reflns_point_group_measured_fraction_full 0.741
_diffrn_reflns_point_group_measured_fraction_max 0.659
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.011
_diffrn_reflns_theta_min         5.813
_diffrn_ambient_temperature      293(2)
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         1400000
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0338
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.741
_diffrn_measured_fraction_theta_max 0.659
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 phi    -35.00   19.75   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
   0.0000  -30.0000    0.0000     -     73

#__ type_ start__ end____ width___ exp.time_
  2 phi    140.00  200.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
   0.0000  -30.0000    0.0000     -     80

#__ type_ start__ end____ width___ exp.time_
  3 phi    160.00  217.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
   0.0000   30.0000    0.0000     -     76

#__ type_ start__ end____ width___ exp.time_
  4 phi    -20.00   34.75   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
   0.0000   30.0000    0.0000     -     73

#__ type_ start__ end____ width___ exp.time_
  5 omega  -24.00   24.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   39.4600  -12.9000 64

#__ type_ start__ end____ width___ exp.time_
  6 omega  -24.00   24.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   39.4600  167.1000 64

#__ type_ start__ end____ width___ exp.time_
  7 omega  -50.00   10.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   39.4600  167.1000 80

#__ type_ start__ end____ width___ exp.time_
  8 omega  -50.00   10.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   39.4600  -12.9000 80

#__ type_ start__ end____ width___ exp.time_
  9 omega  -64.00   -8.50   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   81.4000  -28.9000 74

#__ type_ start__ end____ width___ exp.time_
 10 omega  -64.00   -8.50   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   81.4000  151.1000 74

#__ type_ start__ end____ width___ exp.time_
 11 omega  -19.00    8.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   81.4000  151.1000 36

#__ type_ start__ end____ width___ exp.time_
 12 omega  -19.00    8.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   81.4000  -28.9000 36

#__ type_ start__ end____ width___ exp.time_
 13 omega  -43.00  -21.25   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  134.6000  -56.9000 29

#__ type_ start__ end____ width___ exp.time_
 14 omega  -43.00  -21.25   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  134.6000  123.1000 29

#__ type_ start__ end____ width___ exp.time_
 15 omega  -90.00  -36.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000  134.6000  123.1000 72

#__ type_ start__ end____ width___ exp.time_
 16 omega  -90.00  -36.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000  134.6000  -56.9000 72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω and π scans'
_diffrn_orient_matrix_UB_11      -0.0022315000
_diffrn_orient_matrix_UB_12      -0.0708462000
_diffrn_orient_matrix_UB_13      0.0201386000
_diffrn_orient_matrix_UB_21      -0.0801620333
_diffrn_orient_matrix_UB_22      -0.0721880667
_diffrn_orient_matrix_UB_23      -0.0163970667
_diffrn_orient_matrix_UB_31      0.0628113333
_diffrn_orient_matrix_UB_32      -0.0120802333
_diffrn_orient_matrix_UB_33      -0.0201723333
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                200
_reflns_number_total             216
_reflns_odcompleteness_completeness 46.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.95
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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         0.312
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       0.007(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     36
_refine_ls_number_reflns         216
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0269
_refine_ls_restrained_S_all      1.128
_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)+(0.0466P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0696
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Restrained distances
 C2_$1-N1_$2
 1.396 with sigma of 0.01
2. Others
 Fixed Sof: N1(0.16667)
;


#ATOMS POSITIONS

_atom_sites_solution_hydrogens   difmap
_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
Ni1 Ni 0.0000 0.0000 0.0000 0.0164(4) Uani 1 6 d S T P . .
C1 C 0.1236(4) -0.2097(4) 0.0833 0.0207(7) Uani 1 2 d S T P . .
O1 O -0.01273(18) -0.21768(17) 0.05353(6) 0.0253(6) Uani 1 1 d . . . . .
N1 N 0.5829(12) 0.2496(12) 0.0833 0.0287(19) Uani 0.3333 2 d DS T P . .
C2 C 0.6667 0.3333 0.0267(3) 0.0506(18) Uani 1 3 d DS T P . .
H1 H 0.243(5) -0.090(5) 0.0833 0.036(10) Uiso 1 2 d S T P . .
H2 H 0.643(9) 0.419(7) 0.024(3) 0.091(18) Uiso 1 1 d . . . . .
H1A H 0.570(9) 0.138(13) 0.081(6) 0.17(5) Uiso 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
Ni1 0.0156(5) 0.0156(5) 0.0180(6) 0.000 0.000 0.0078(2)
C1 0.0210(12) 0.0210(12) 0.0199(18) -0.0012(6) 0.0012(6) 0.0103(14)
O1 0.0233(9) 0.0227(9) 0.0301(12) 0.0048(4) -0.0033(5) 0.0116(6)
N1 0.024(3) 0.024(3) 0.039(7) 0.002(2) -0.002(2) 0.014(4)
C2 0.054(3) 0.054(3) 0.043(5) 0.000 0.000 0.0272(15)

_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
Ni1 O1 2.0561(12) 20 ?
Ni1 O1 2.0561(12) 2 ?
Ni1 O1 2.0561(12) 3 ?
Ni1 O1 2.0561(12) 21 ?
Ni1 O1 2.0561(12) 19 ?
Ni1 O1 2.0561(12) . ?
C1 O1 1.245(2) 18_544 ?
C1 O1 1.245(2) . ?
N1 N1 1.166(17) 2_655 ?
N1 N1 1.166(17) 3_665 ?
N1 C2 1.394(7) 16_554 ?
N1 C2 1.394(7) . ?
C2 N1 1.394(7) 2_655 ?
C2 N1 1.394(7) 3_665 ?

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 Ni1 O1 180.00(9) 20 2 ?
O1 Ni1 O1 88.46(5) 2 21 ?
O1 Ni1 O1 91.54(5) 2 3 ?
O1 Ni1 O1 180.00(7) 21 3 ?
O1 Ni1 O1 91.54(5) 19 21 ?
O1 Ni1 O1 88.46(5) 20 3 ?
O1 Ni1 O1 91.54(5) 20 19 ?
O1 Ni1 O1 88.46(5) 19 3 ?
O1 Ni1 O1 88.46(5) 20 . ?
O1 Ni1 O1 91.54(5) 2 . ?
O1 Ni1 O1 88.46(5) 2 19 ?
O1 Ni1 O1 88.46(5) 21 . ?
O1 Ni1 O1 91.54(5) 3 . ?
O1 Ni1 O1 91.54(5) 20 21 ?
O1 Ni1 O1 180.0 19 . ?
O1 C1 O1 124.4(3) . 18_544 ?
C1 O1 Ni1 125.35(17) . . ?
N1 N1 N1 59.999(1) 2_655 3_665 ?
N1 N1 C2 65.3(3) 2_655 . ?
N1 N1 C2 65.3(3) 3_665 . ?
N1 N1 C2 65.3(3) 2_655 16_554 ?
N1 N1 C2 65.3(3) 3_665 16_554 ?
C2 N1 C2 122.3(8) . 16_554 ?
N1 C2 N1 49.4(7) 2_655 3_665 ?
N1 C2 N1 49.4(7) 2_655 . ?
N1 C2 N1 49.4(7) 3_665 . ?

_iucr_refine_instructions_details 
;
TITL 32 in R-3c #167
REM reset to R-3c #167
CELL 0.71073 8.039503 8.039503 21.573233 90 90 120
ZERR 6.00012 0.000386 0.000386 0.001374 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -Y+X,-Y,0.5-Z
SYMM -X,-X+Y,0.5-Z
SYMM +Y,+X,0.5-Z
SFAC C H N Ni O
UNIT 30 90 6 6 36
EQIV $1 0.667-Y,0.333-X,-0.167+Z
EQIV $2 -Y+X,-1+X,-Z
DFIX 1.396 0.01 C2_$1 N1_$2
 
L.S. 44 0 0
PLAN  1
BOND
fmap 2 53
acta
OMIT 4 0 -20
OMIT 7 2 -10
OMIT 2 0 -4
REM <olex2.extras>
REM <HklSrc "%.\\hp_1_40GPa.hkl">
REM </olex2.extras>
 
WGHT    0.046600
EXTI    0.006831
FVAR       5.18265
NI1   4    0.000000    0.000000    0.000000    10.16667    0.01565    0.01565 =
         0.01799    0.00000    0.00000    0.00782
C1    1    0.123635   -0.209698    0.083333    10.50000    0.02103    0.02103 =
         0.01987   -0.00125    0.00125    0.01030
O1    5   -0.012733   -0.217682    0.053529    11.00000    0.02332    0.02271 =
         0.03008    0.00477   -0.00332    0.01162
N1    3    0.582930    0.249596    0.083333    10.16667    0.02437    0.02437 =
         0.03927    0.00156   -0.00156    0.01357
C2    1    0.666667    0.333333    0.026733    10.33333    0.05437    0.05437 =
         0.04305    0.00000    0.00000    0.02718
H1    2    0.243405   -0.089928    0.083333    10.50000    0.03609
H2    2    0.643221    0.419421    0.024086    11.00000    0.09058
H1A   2    0.570423    0.137964    0.081217    11.00000    0.17284
HKLF 4
 
REM  32 in R-3c #167
REM R1 =  0.0269 for     200 Fo > 4sig(Fo)  and  0.0286 for all     216 data
REM     36 parameters refined using      1 restraints
 
END  
     
WGHT      0.0466      0.0000 

REM Highest difference peak  0.312,  deepest hole -0.354,  1-sigma level  0.084
Q1    1   0.0169 -0.2379  0.0263  11.00000  0.05    0.31

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0269 for 200 Fo > 4sig(Fo) and 0.0286 for all 2215 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.31, deepest hole -0.35
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0286
  REM R1_gt = 0.0269
  REM wR_ref = 0.0696
  REM GOOF = 1.131
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 2215
  REM Reflections_gt = 200
  REM Parameters = n/a
  REM Hole = -0.35
  REM Peak = 0.31
  REM Flack = n/a

  
;
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_co_hp_1_52gpa
_database_code_depnum_ccdc_archive 'CCDC 1845713'
_audit_update_record             
;
2018-05-28 deposited with the CCDC.
2018-07-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT305_co_hp_1_52gpa       
;
PROBLEM: Isolated Hydrogen Atom   (Outside Bond Range ??)        H1A Check
RESPONSE: The data comes from high-pressure measurments and it is a consequence of the used apparatus
;
_vrf_PLAT413_co_hp_1_52gpa       
;
PROBLEM: Short Inter XH3 .. XHn     H2       ..H2               0.90 Ang.
RESPONSE: Dma H-atoms were located also by using difference Fourier map therfore they can differ from the ideal positions.
;
_vrf_PLAT417_co_hp_1_52gpa       
;
PROBLEM: Short Inter D-H..H-D       H1A      ..H1A              1.66 Ang.
RESPONSE: The guest is disordered in the three positions which results in short contacts between other H atoms
;
_vrf_PLAT415_co_hp_1_52gpa       
;
PROBLEM: Short Inter D-H..H-X       H1A      ..H2               1.90 Ang.
RESPONSE: The dma H-atoms were located also by using difference Fourier map therfore they can differ from the ideal positions.
;
_audit_creation_date             2018-05-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;

# CHEMICAL DATA 

_chemical_name_common            DmaCoFor3
_chemical_name_systematic        
;
  catena-(dimethylammonium tris(μ₂-formato)-cobalt(ii))
;
_chemical_formula_moiety         'C3 H3 Co1 O6 1-)n,n(C2 H8 N1 1+))'
_chemical_formula_sum            'C5 H15 Co N O6'
_chemical_formula_weight         244.10
_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 0.0033 0.0016 '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 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'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-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'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+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-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+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-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+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'

_cell_length_a                   8.1000(12)
_cell_length_b                   8.1000(12)
_cell_length_c                   21.699(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1232.9(5)
_cell_formula_units_Z            6.00012
_cell_measurement_reflns_used    1674
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.000
_cell_measurement_theta_min      5.034
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.088
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.734
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.973
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_preparation       DMF
_exptl_crystal_F_000             762
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 Data were collected at room temperature and pressure of 1.52(2) GPa
 (1520000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique.
 Pressure was determined by monitoring the shift of the ruby
 R1-fluorescence line.
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?

# APARATURE DETAILS

_diffrn_reflns_av_R_equivalents  0.1383
_diffrn_reflns_av_unetI/netI     0.0835
_diffrn_reflns_Laue_measured_fraction_full 0.675
_diffrn_reflns_Laue_measured_fraction_max 0.681
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            1942
_diffrn_reflns_point_group_measured_fraction_full 0.675
_diffrn_reflns_point_group_measured_fraction_max 0.681
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.972
_diffrn_reflns_theta_min         5.034
_diffrn_ambient_temperature      293(2)
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         1520000
_diffrn_detector_area_resol_mean 16.0456
_diffrn_measured_fraction_theta_full 0.675
_diffrn_measured_fraction_theta_max 0.681
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                131
_reflns_number_total             188
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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         0.417
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       0.0000
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     34
_refine_ls_number_reflns         188
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1024
_refine_ls_R_factor_gt           0.0462
_refine_ls_restrained_S_all      2.743
_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)+13.6181P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0718
_refine_ls_wR_factor_ref         0.0901
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Restrained distances
 N1-H1A
 0.94 with sigma of 0.02
 C2-C2_$1
 2.481 with sigma of 0.002
 N1-C2
 1.345 with sigma of 0.002
2. Others
 Fixed Sof: N1(0.16665)
 Fixed U13: Co1(0) C2(0)
 Fixed U23: Co1(0) C2(0)
 Fixed Uiso: H1(0.026)
 Fixed X: Co1(0) N1(0.749499) C2(0.66667)
 Fixed Y: Co1(0) C2(0.33333)
 Fixed Z: Co1(0) C1(0.08333) H1(0.08333) N1(0.08333)
;


#ATOMS POSITIONS

_atom_sites_solution_hydrogens   difmap
_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 0.0000 0.0000 0.0000 0.0245(10) Uani 1 6 d S T P . .
C1 C 0.1184(13) -0.2149(13) 0.0833 0.028(3) Uani 1 2 d S T P . .
H1 H 0.233(11) -0.100(11) 0.0833 0.026 Uiso 1 2 d S T P . .
O1 O -0.0159(6) -0.2212(6) 0.0537(2) 0.0325(15) Uani 1 1 d . . . . .
N1 N 0.7495 0.3333 0.0833 0.040(8) Uani 0.3333 2 d DS T P . .
C2 C 0.6667 0.3333 0.02672(5) 0.056(4) Uani 1 3 d DS T P . .
H2 H 0.60(6) 0.27(7) -0.001(11) 0.31(14) Uiso 1 1 d . . . . .
H1A H 0.875(11) 0.428(15) 0.073(12) 0.30(13) Uiso 1 1 d 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 0.0248(12) 0.0248(12) 0.0239(15) 0.000 0.000 0.0124(6)
C1 0.028(5) 0.028(5) 0.022(6) 0.001(2) -0.001(2) 0.009(5)
O1 0.024(3) 0.031(3) 0.040(3) 0.006(2) -0.003(2) 0.012(3)
N1 0.022(11) 0.033(16) 0.07(2) -0.018(16) -0.009(8) 0.017(8)
C2 0.061(7) 0.061(7) 0.046(12) 0.000 0.000 0.030(4)

_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 2.087(4) 21 ?
Co1 O1 2.087(4) 19 ?
Co1 O1 2.087(4) 20 ?
Co1 O1 2.087(4) 3 ?
Co1 O1 2.087(4) . ?
Co1 O1 2.087(4) 2 ?
C1 O1 1.242(6) 18_544 ?
C1 O1 1.242(6) . ?
N1 N1 1.16209(17) 2_655 ?
N1 N1 1.16210(17) 3_665 ?
N1 C2 1.3998(9) 16_554 ?
N1 C2 1.3997(9) . ?
C2 N1 1.3997(9) 3_665 ?
C2 N1 1.3997(9) 2_655 ?

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 180.0(3) 21 3 ?
O1 Co1 O1 88.18(19) . 20 ?
O1 Co1 O1 88.18(19) 2 19 ?
O1 Co1 O1 88.18(19) 21 . ?
O1 Co1 O1 91.82(19) 21 19 ?
O1 Co1 O1 91.82(19) 3 . ?
O1 Co1 O1 88.18(19) 3 20 ?
O1 Co1 O1 88.18(19) 21 2 ?
O1 Co1 O1 180.0(3) 2 20 ?
O1 Co1 O1 91.82(19) 3 2 ?
O1 Co1 O1 88.18(19) 3 19 ?
O1 Co1 O1 91.82(19) . 2 ?
O1 Co1 O1 91.82(19) 20 19 ?
O1 Co1 O1 91.82(19) 21 20 ?
O1 Co1 O1 180.0 . 19 ?
O1 C1 O1 125.4(9) . 18_544 ?
C1 O1 Co1 125.2(5) . . ?
N1 N1 N1 60.0 2_655 3_665 ?
N1 N1 C2 65.472(18) 2_655 . ?
N1 N1 C2 65.478(18) 3_665 16_554 ?
N1 N1 C2 65.471(18) 3_665 . ?
N1 N1 C2 65.477(18) 2_655 16_554 ?
C2 N1 C2 122.72(4) . 16_554 ?
N1 C2 N1 49.06(4) 3_665 . ?
N1 C2 N1 49.05(4) 2_655 . ?
N1 C2 N1 49.06(4) 3_665 2_655 ?

_iucr_refine_instructions_details 
;
TITL Co_hp_1_52GPa in R-3c #167
REM reset to R-3c #167
CELL 0.71073 8.1 8.1 21.699 90 90 120
ZERR 6.00012 0.0012 0.0012 0.0057 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -Y+X,-Y,0.5-Z
SYMM -X,-X+Y,0.5-Z
SYMM +Y,+X,0.5-Z
SFAC C H Co N O
UNIT 30 90 6 6 36
EQIV $1 0.333-Y+X,0.667-Y,0.167-Z

 
L.S. 44
PLAN  2
BOND
fmap 2
acta 52
OMIT -1 2 9
REM <olex2.extras>
REM <HklSrc "%.\\Co_hp_1_52GPa.hkl">
REM </olex2.extras>
 
WGHT    0.000000   13.618101
EXTI    0.000000
FVAR       0.32843
CO1   3   10.000000   10.000000   10.000000    10.16667    0.02476    0.02476 =
         0.02387  -10.00000  -10.00000    0.01238
C1    1    0.118405   -0.214928   10.083330    10.50000    0.02785    0.02785 =
         0.02183    0.00068   -0.00068    0.00942
H1    2    0.233011   -0.100323   10.083330    10.50000   10.02600
O1    5   -0.015902   -0.221197    0.053733    11.00000    0.02402    0.03130 =
         0.03957    0.00597   -0.00288    0.01180
N1    4   10.749499    0.333333   10.083330    10.16665    0.02188    0.03312 =
         0.06961   -0.01822   -0.00911    0.01656
C2    1   10.666670   10.333330    0.026719    10.33333    0.06082    0.06082 =
         0.04591  -10.00000  -10.00000    0.03041
H2    2    0.601302    0.272234   -0.001315    11.00000    0.31458
H1A   2    0.874557    0.428208    0.073106    11.00000    0.30231
HKLF 4
 
REM  Co_hp_1_52GPa in R-3c #167
REM R1 =  0.0462 for     131 Fo > 4sig(Fo)  and  0.1024 for all     188 data
REM     34 parameters refined using      3 restraints
 
END  
     
WGHT      0.0000     12.3926 

REM Highest difference peak  0.417,  deepest hole -0.480,  1-sigma level  0.099
Q1    1   0.0000  0.0000  0.0520  10.33333  0.05    0.42
Q2    1   0.3395 -0.1224  0.1150  11.00000  0.05    0.37

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0462 for 131 Fo > 4sig(Fo) and 0.1024 for all 2192 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.42, deepest hole -0.48
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.1024
  REM R1_gt = 0.0462
  REM wR_ref = 0.0901
  REM GOOF = 1.156
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 2192
  REM Reflections_gt = 131
  REM Parameters = n/a
  REM Hole = -0.48
  REM Peak = 0.42
  REM Flack = n/a

  
;
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_co_hp_2_45gpa
_database_code_depnum_ccdc_archive 'CCDC 1845714'
_audit_update_record             
;
2018-05-28 deposited with the CCDC.
2018-07-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_co_hp_2_45gpa       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.676 Why?
RESPONSE: The data comes from high-pressure measurments and it is a consequence of the used apparatus
;
_vrf_PLAT411_co_hp_2_45gpa       
;
PROBLEM: Short Inter H...H Contact  H1A      ..H1A              0.70 Ang.
RESPONSE: Dma H-atoms were located also by using difference Fourier map therfore they can differ from the ideal positions.
;
_vrf_PLAT415_co_hp_2_45gpa       
;
PROBLEM: Short Inter D-H..H-X       H1A      ..H1B              1.80 Ang.
RESPONSE: The guest is disordered in the three positions which results in short contacts between other H atoms
;
_vrf_PLAT417_co_hp_2_45gpa       
;
PROBLEM: Short Inter D-H..H-D       H1B      ..H1B              1.66 Ang.
RESPONSE: The dma H-atoms were located also by using difference Fourier map therfore they can differ from the ideal positions.
;
_vrf_PLAT417_co_hp_2_45gpa_2     
;
PROBLEM: Short Inter D-H..H-D       H1B      ..H1B              1.87 Ang.
RESPONSE: Dma amine in framework is strongly disordered so exact location of H-atoms was difficult
;
_audit_creation_date             2018-05-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;

# CHEMICAL DATA 

_chemical_name_common            DmaCoFor3
_chemical_name_systematic        
;
  catena-(dimethylammonium tris(μ₂-formato)-cobalt(ii))
;
_chemical_formula_moiety         'C3 H3 Co1 O6 1-)n,n(C2 H8 N1 1+))'
_chemical_formula_sum            'C5 H15 Co N O6'
_chemical_formula_weight         244.10
_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 0.0033 0.0016 '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 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'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-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'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+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-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+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-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+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'

_cell_length_a                   8.0621(10)
_cell_length_b                   8.0621(10)
_cell_length_c                   21.424(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1206.0(4)
_cell_formula_units_Z            6.00012
_cell_measurement_reflns_used    1684
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.218
_cell_measurement_theta_min      5.058
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.135
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.017
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_preparation       DMF
_exptl_crystal_F_000             762
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 Data were collected at room temperature and pressure of 2.45(2) GPa
 (2450000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique.
 Pressure was determined by monitoring the shift of the ruby
 R1-fluorescence line.
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?

# APARATURE DETAILS

_diffrn_reflns_av_R_equivalents  0.1371
_diffrn_reflns_av_unetI/netI     0.0892
_diffrn_reflns_Laue_measured_fraction_full 0.676
_diffrn_reflns_Laue_measured_fraction_max 0.675
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            1917
_diffrn_reflns_point_group_measured_fraction_full 0.676
_diffrn_reflns_point_group_measured_fraction_max 0.675
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.218
_diffrn_reflns_theta_min         5.058
_diffrn_ambient_temperature      293(2)
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         2450000
_diffrn_detector_area_resol_mean 16.0548
_diffrn_measured_fraction_theta_full 0.676
_diffrn_measured_fraction_theta_max 0.675
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                133
_reflns_number_total             187
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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         0.382
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     33
_refine_ls_number_reflns         187
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0491
_refine_ls_restrained_S_all      1.128
_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)+(0.0206P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0611
_refine_ls_wR_factor_ref         0.0714
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 H1B-N2
 0.98 with sigma of 0.02
 H1A-C1
 0.98 with sigma of 0.02
 C1_$1-C1
 2.51 with sigma of 0.02
 N2_$2-C1
 1.389 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: N2(0.16667)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2)
;

#ATOMS POSITIONS

_atom_sites_solution_hydrogens   mixed
_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 0.0000 0.0000 0.0000 0.0226(6) Uani 1 6 d S T P . .
O1 O -0.0193(5) -0.2230(5) 0.05434(18) 0.0293(10) Uani 1 1 d . . . . .
C2 C 0.1159(9) -0.2174(9) 0.0833 0.0221(15) Uani 1 2 d S TU P . .
H2 H 0.2313 -0.1021 0.0833 0.027 Uiso 1 2 calc RS T P . .
C1 C 0.6667 0.3333 0.0255(4) 0.055(3) Uani 1 3 d DS T P . .
N2 N 0.586(2) 0.253(2) 0.0833 0.042(7) Uani 0.3333 2 d DS T P . .
H1A H 0.63(9) 0.35(7) -0.019(5) 0.40(11) Uiso 1 1 d D . . . .
H1B H 0.555(15) 0.209(14) 0.040(2) 0.18(6) Uiso 1 1 d 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 0.0226(7) 0.0226(7) 0.0225(12) 0.000 0.000 0.0113(4)
O1 0.022(2) 0.028(2) 0.037(3) 0.0073(18) -0.0035(17) 0.0113(19)
C2 0.0223(15) 0.0223(15) 0.0220(18) -0.0004(7) 0.0004(7) 0.0112(11)
C1 0.069(6) 0.069(6) 0.027(9) 0.000 0.000 0.035(3)
N2 0.028(11) 0.028(11) 0.06(2) -0.002(7) 0.002(7) 0.005(10)

_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 2.081(3) 20 ?
Co1 O1 2.081(3) 21 ?
Co1 O1 2.081(3) 19 ?
Co1 O1 2.081(3) . ?
Co1 O1 2.081(3) 3 ?
Co1 O1 2.081(3) 2 ?
O1 C2 1.236(4) . ?
C2 O1 1.236(4) 18_544 ?
C2 H2 0.9300 . ?
C1 N2 1.398(10) 2_655 ?
C1 N2 1.398(10) 3_665 ?
C1 N2 1.398(10) . ?
C1 H1A 1.04(8) . ?
C1 H1B 1.00(10) . ?
N2 C1 1.398(10) 18_544 ?
N2 N2 1.12(3) 3_665 ?
N2 N2 1.12(3) 2_655 ?
N2 H1B 0.98(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
O1 Co1 O1 180.0(2) 20 2 ?
O1 Co1 O1 180.0(2) 21 3 ?
O1 Co1 O1 88.24(15) 20 3 ?
O1 Co1 O1 88.24(15) 19 3 ?
O1 Co1 O1 91.76(15) 19 21 ?
O1 Co1 O1 88.24(15) 21 . ?
O1 Co1 O1 91.76(15) 20 21 ?
O1 Co1 O1 91.76(15) 20 19 ?
O1 Co1 O1 88.24(15) 2 21 ?
O1 Co1 O1 91.76(15) 2 . ?
O1 Co1 O1 91.76(15) 3 . ?
O1 Co1 O1 88.24(15) 2 19 ?
O1 Co1 O1 88.24(15) 20 . ?
O1 Co1 O1 91.76(15) 2 3 ?
O1 Co1 O1 180.00(18) 19 . ?
C2 O1 Co1 124.5(3) . . ?
O1 C2 O1 125.3(6) . 18_544 ?
O1 C2 H2 117.3 . . ?
O1 C2 H2 117.3 18_544 . ?
N2 C1 N2 47.4(11) 3_665 . ?
N2 C1 N2 47.4(11) 2_655 3_665 ?
N2 C1 N2 47.4(11) 2_655 . ?
N2 C1 H1A 169(10) 2_655 . ?
N2 C1 H1A 133(10) 3_665 . ?
N2 C1 H1A 143(10) . . ?
N2 C1 H1B 85(3) 2_655 . ?
N2 C1 H1B 89(3) 3_665 . ?
N2 C1 H1B 44.7(13) . . ?
H1A C1 H1B 106(10) . . ?
C1 N2 C1 124.7(14) . 18_544 ?
C1 N2 H1B 46(6) . . ?
C1 N2 H1B 169(7) 18_544 . ?
N2 N2 C1 66.3(6) 3_665 18_544 ?
N2 N2 C1 66.3(6) 2_655 18_544 ?
N2 N2 C1 66.3(6) 3_665 . ?
N2 N2 C1 66.3(6) 2_655 . ?
N2 N2 N2 60.000(2) 2_655 3_665 ?
N2 N2 H1B 108(6) 3_665 . ?
N2 N2 H1B 103(7) 2_655 . ?

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 C2 O1 -174.8(3) . . . 18_544 ?
N2 C1 N2 C1 -33.10(16) 3_665 . . 18_544 ?
N2 C1 N2 C1 33.10(16) 2_655 . . 18_544 ?
N2 C1 N2 N2 -66.2(3) 3_665 . . 2_655 ?
N2 C1 N2 N2 66.2(3) 2_655 . . 3_665 ?

_iucr_refine_instructions_details 
;
TITL r-3c in R-3c #167
REM reset to R-3c #167
CELL 0.71073 8.0621 8.0621 21.4242 90 90 120
ZERR 6.00012 0.001 0.001 0.0051 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -Y+X,-Y,0.5-Z
SYMM -X,-X+Y,0.5-Z
SYMM +Y,+X,0.5-Z
SFAC C H Co N O
UNIT 30 90 6 6 36
EQIV $1 0.333+Y,-0.333+X,0.167-Z
EQIV $2 1-Y,+X-Y,+Z
ISOR 0.001 0.002 C2
 
L.S. 44
PLAN  5
BOND
MORE -1
BOND $H
CONF
fmap 2
acta 52
OMIT -1 2 9
REM <olex2.extras>
REM <HklSrc "%.\\Co_hp_2_45GPa.hkl">
REM </olex2.extras>
 
WGHT    0.020600
FVAR       0.29985
CO1   3    0.000000    0.000000    0.000000    10.16667    0.02264    0.02264 =
         0.02247    0.00000    0.00000    0.01132
O1    5   -0.019318   -0.223000    0.054338    11.00000    0.02158    0.02767 =
         0.03731    0.00729   -0.00350    0.01128
C2    1    0.115925   -0.217408    0.083333    10.50000    0.02225    0.02225 =
         0.02196   -0.00038    0.00038    0.01121
AFIX  43
H2    2    0.231279   -0.102053    0.083334    10.50000   -1.20000
AFIX   0
 
C1    1    0.666667    0.333333    0.025530    10.33333    0.06932    0.06932 =
         0.02659    0.00000    0.00000    0.03466
N2    4    0.586140    0.252806    0.083333    10.16667    0.02845    0.02845 =
         0.05795   -0.00201    0.00201    0.00531
H1A   2    0.632568    0.354120   -0.019362    11.00000    0.39887
H1B   2    0.555277    0.208759    0.039854    11.00000    0.17754
HKLF 4
 
REM  r-3c in R-3c #167
REM R1 =  0.0491 for     133 Fo > 4sig(Fo)  and  0.0965 for all     187 data
REM     33 parameters refined using     10 restraints
 
END  
     
WGHT      0.0207      0.0000 

REM Highest difference peak  0.382,  deepest hole -0.321,  1-sigma level  0.087
Q1    1  -0.0582 -0.3319  0.1090  11.00000  0.05    0.33
Q2    1   0.1014 -0.3004  0.0897  11.00000  0.05    0.27
Q3    1   0.4683  0.1144  0.0580  11.00000  0.05    0.27
Q4    1   0.0332 -0.2526  0.0255  11.00000  0.05    0.26
Q5    1   0.2458  0.0453  0.0503  11.00000  0.05    0.25

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0491 for 133 Fo > 4sig(Fo) and 0.0965 for all 2164 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.38, deepest hole -0.32
  REM Mean Shift 0.000, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0965
  REM R1_gt = 0.0491
  REM wR_ref = 0.0714
  REM GOOF = 1.130
  REM Shift_max = 0.000
  REM Shift_mean = 0.000
  REM Reflections_all = 2164
  REM Reflections_gt = 133
  REM Parameters = n/a
  REM Hole = -0.32
  REM Peak = 0.38
  REM Flack = n/a

  
;
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_co_hp_0_34gpa
_database_code_depnum_ccdc_archive 'CCDC 1845710'
_audit_update_record             
;
2018-05-28 deposited with the CCDC.
2018-07-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_co_hp_0_34gpa       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.844 Why?
RESPONSE: The data comes from high-pressure measurments and it is a consequence of the used apparatus
;
_vrf_PLAT413_co_hp_0_34gpa       
;
PROBLEM: Short Inter XH3 .. XHn     H2       ..H2               1.40 Ang.
RESPONSE: Dma H-atoms were located also by using difference Fourier map therfore they can differ from the ideal positions.
;
_vrf_PLAT414_co_hp_0_34gpa       
;
PROBLEM: Short Intra D-H..H-X       H1A      ..H2               1.61 Ang.
RESPONSE: The guest is disordered in the three positions which results in short contacts between other H atoms
;
_vrf_PLAT415_co_hp_0_34gpa       
;
PROBLEM: Short Inter D-H..H-X       H1A      ..H2               1.89 Ang.
RESPONSE: The dma amine in framework is strongly disordered so exact location of H-atoms was difficult
;
_vrf_PLAT417_co_hp_0_34gpa       
;
PROBLEM: Short Inter D-H..H-D       H1A      ..H1A              1.16 Ang.
RESPONSE: The guest is disordered in the three positions which results in short contacts between other H atoms
;
_vrf_PLAT771_co_hp_0_34gpa       
;
PROBLEM: Suspect N-H Bond in CIF: N1       --H2        ..       1.50 Ang.
RESPONSE: The dma amine in framework is strongly disordered so exact location of H-atoms was difficult
;

_audit_creation_date             2018-05-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;

# CHEMICAL DATA 

_chemical_name_common            DmaCoFor3
_chemical_name_systematic        
;
  catena-(dimethylammonium tris(μ₂-formato)-cobalt(ii))
;
_chemical_formula_moiety         'C3 H3 Co1 O6 1-)n,n(C2 H8 N1 1+))'
_chemical_formula_sum            'C5 H15 Co N O6'
_chemical_formula_weight         244.10
_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 0.0033 0.0016 '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 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'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-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'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+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-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+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-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+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'

_cell_length_a                   8.1686(14)
_cell_length_b                   8.1686(14)
_cell_length_c                   22.105(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1277.4(5)
_cell_formula_units_Z            6.00012
_cell_measurement_reflns_used    1492
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.446
_cell_measurement_theta_min      4.765
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.016
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.7793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.904
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_preparation       DMF
_exptl_crystal_F_000             762
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 Data were collected at room temperature and pressure of 0.34(2) GPa
 (340000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique.
 Pressure was determined by monitoring the shift of the ruby
 R1-fluorescence line.
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?

# APARATURE DETAILS

_diffrn_reflns_av_R_equivalents  0.0852
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 0.844
_diffrn_reflns_Laue_measured_fraction_max 0.789
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            1858
_diffrn_reflns_point_group_measured_fraction_full 0.844
_diffrn_reflns_point_group_measured_fraction_max 0.789
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.446
_diffrn_reflns_theta_min         4.991
_diffrn_ambient_temperature      293(2)
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         340000
_diffrn_detector_area_resol_mean 16.0519
_diffrn_measured_fraction_theta_full 0.844
_diffrn_measured_fraction_theta_max 0.789
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                176
_reflns_number_total             236
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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         0.584
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       0.0000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     33
_refine_ls_number_reflns         236
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0504
_refine_ls_restrained_S_all      1.086
_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)+(0.0776P)²+2.1990P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1364
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C2-N1
 1.41 with sigma of 0.005
 N1-H2
 1.5 with sigma of 0.02
3. Others
 Fixed Sof: N1(0.16667)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1)
;

#ATOMS POSITIONS

_atom_sites_solution_hydrogens   mixed
_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 0.0000 0.0000 0.0000 0.0333(8) Uani 1 6 d S T P . .
O1 O -0.0083(5) -0.2171(6) 0.05373(18) 0.0446(12) Uani 1 1 d . . . . .
C1 C 0.1219(11) -0.2115(11) 0.0833 0.0395(19) Uani 1 2 d S T P . .
H1 H 0.2357 -0.0976 0.0833 0.047 Uiso 1 2 calc RS T P . .
C2 C 0.0000 0.0000 0.1945(5) 0.065(4) Uani 1 3 d DS T P . .
N1 N 0.0000 -0.084(2) 0.2500 0.050(7) Uani 0.3333 2 d DS T P . .
H2 H -0.032(18) -0.107(15) 0.1831(13) 0.13(4) Uiso 1 1 d D . . . .
H1A H -0.091(10) -0.173(11) 0.252(5) 0.08(4) Uiso 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 0.0359(10) 0.0359(10) 0.0282(10) 0.000 0.000 0.0179(5)
O1 0.039(3) 0.048(3) 0.046(2) 0.0052(18) -0.0053(17) 0.022(2)
C1 0.043(4) 0.043(4) 0.034(4) -0.0008(18) 0.0008(18) 0.023(4)
C2 0.072(7) 0.072(7) 0.051(7) 0.000 0.000 0.036(3)
N1 0.036(16) 0.055(12) 0.052(15) 0.002(6) 0.004(13) 0.018(8)

_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 2.107(4) . ?
Co1 O1 2.107(4) 2 ?
Co1 O1 2.107(4) 3 ?
Co1 O1 2.107(4) 19 ?
Co1 O1 2.107(4) 20 ?
Co1 O1 2.107(4) 21 ?
O1 C1 1.230(5) . ?
C1 O1 1.229(5) 18_544 ?
C1 H1 0.9300 . ?
C2 N1 1.406(5) . ?
C2 N1 1.406(5) 3 ?
C2 N1 1.406(5) 2 ?
C2 H2 0.82(9) . ?
N1 C2 1.406(5) 4 ?
N1 N1 1.19(3) 3 ?
N1 N1 1.19(3) 2 ?
N1 H2 1.50(2) . ?
N1 H1A 0.74(8) . ?

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 88.66(16) . 21 ?
O1 Co1 O1 180.0(3) 2 20 ?
O1 Co1 O1 88.66(16) . 20 ?
O1 Co1 O1 88.66(16) 3 20 ?
O1 Co1 O1 91.34(16) 3 2 ?
O1 Co1 O1 88.66(16) 2 19 ?
O1 Co1 O1 91.34(16) . 2 ?
O1 Co1 O1 91.34(16) . 3 ?
O1 Co1 O1 88.66(16) 21 2 ?
O1 Co1 O1 91.34(16) 21 19 ?
O1 Co1 O1 91.34(16) 20 19 ?
O1 Co1 O1 180.0(2) 21 3 ?
O1 Co1 O1 180.0 . 19 ?
O1 Co1 O1 91.34(16) 21 20 ?
O1 Co1 O1 88.66(16) 3 19 ?
C1 O1 Co1 127.2(5) . . ?
O1 C1 O1 126.4(8) 18_544 . ?
O1 C1 H1 116.8 18_544 . ?
O1 C1 H1 116.8 . . ?
N1 C2 N1 49.9(14) 2 3 ?
N1 C2 N1 49.9(14) . 2 ?
N1 C2 N1 49.9(14) . 3 ?
N1 C2 H2 80(3) . . ?
N1 C2 H2 112(7) 3 . ?
N1 C2 H2 127(4) 2 . ?
C2 N1 C2 121.7(17) 4 . ?
C2 N1 H2 33(4) . . ?
C2 N1 H2 152(4) 4 . ?
C2 N1 H1A 100(8) 4 . ?
C2 N1 H1A 108(8) . . ?
N1 N1 C2 65.1(7) 3 4 ?
N1 N1 C2 65.1(7) 3 . ?
N1 N1 C2 65.1(7) 2 . ?
N1 N1 C2 65.1(7) 2 4 ?
N1 N1 N1 60.001(1) 2 3 ?
N1 N1 H2 96(4) 2 . ?
N1 N1 H2 88(4) 3 . ?
N1 N1 H1A 89(6) 3 . ?
N1 N1 H1A 149(6) 2 . ?
H2 N1 H1A 85(10) . . ?

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 O1 -177.5(4) . . . 18_544 ?
N1 C2 N1 C2 -33.5(2) 3 . . 4 ?
N1 C2 N1 C2 33.5(2) 2 . . 4 ?
N1 C2 N1 N1 -66.9(4) 3 . . 2 ?
N1 C2 N1 N1 66.9(4) 2 . . 3 ?

_iucr_refine_instructions_details 
;
TITL r-3c_2 in R-3c #167
REM reset to R-3c #167
CELL 0.71073 8.1686 8.1686 22.1047 90 90 120
ZERR 6.00012 0.0014 0.0014 0.0046 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -Y+X,-Y,0.5-Z
SYMM -X,-X+Y,0.5-Z
SYMM +Y,+X,0.5-Z
SFAC C H Co N O
UNIT 30 90 6 6 36
EQIV $1 -X,-X+Y,0.5-Z

 
L.S. 44
PLAN  1
FREE N1 H2_$1
FREE N1 H2
BOND
MORE -1
BOND $H
CONF
fmap 2
acta
OMIT 0 0 6
OMIT 1 0 16
OMIT 1 1 3
OMIT 8 1 -5
OMIT 6 2 13
OMIT 1 1 21
OMIT 6 2 13
OMIT 1 1 21
OMIT 4 0 10
OMIT 5 3 -13
OMIT 5 2 3
OMIT 4 1 -21
OMIT 4 2 17
OMIT 7 1 -9
OMIT 0 0 12
OMIT 2 1 -5
OMIT 1 1 6
OMIT 3 2 -11
OMIT -1 1 16
OMIT 5 3 14
OMIT 2 1 25
OMIT 1 1 0
REM <olex2.extras>
REM <HklSrc "%.\\r-3c_2.hkl">
REM </olex2.extras>
 
WGHT    0.077600    2.199000
FVAR       0.18695
CO1   3    0.000000    0.000000    0.000000    10.16667    0.03586    0.03586 =
         0.02817    0.00000    0.00000    0.01793
O1    5   -0.008299   -0.217124    0.053734    11.00000    0.03943    0.04848 =
         0.04594    0.00523   -0.00528    0.02192
C1    1    0.121875   -0.211458    0.083333    10.50000    0.04320    0.04320 =
         0.03372   -0.00081    0.00081    0.02279
AFIX  43
H1    2    0.235723   -0.097605    0.083337    10.50000   -1.20000
AFIX   0
 
C2    1    0.000000    0.000000    0.194451    10.33333    0.07246    0.07246 =
         0.05068    0.00000    0.00000    0.03623
N1    4    0.000000   -0.083798    0.250000    10.16667    0.03635    0.05465 =
         0.05198    0.00219    0.00438    0.01817
H2    2   -0.032297   -0.107178    0.183087    11.00000    0.12674
H1A   2   -0.091182   -0.173425    0.252484    11.00000    0.08458
HKLF 4
 
REM  r-3c_2 in R-3c #167
REM R1 =  0.0504 for     176 Fo > 4sig(Fo)  and  0.0767 for all     236 data
REM     33 parameters refined using      2 restraints
 
END  
     
WGHT      0.0720      4.1552 

REM Highest difference peak  0.584,  deepest hole -0.519,  1-sigma level  0.111
Q1    1  -0.0538  0.0355  0.0333  11.00000  0.05    0.58

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0504 for 176 Fo > 4sig(Fo) and 0.0767 for all 2197 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.58, deepest hole -0.52
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0767
  REM R1_gt = 0.0504
  REM wR_ref = 0.1364
  REM GOOF = 1.089
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 2197
  REM Reflections_gt = 176
  REM Parameters = n/a
  REM Hole = -0.52
  REM Peak = 0.58
  REM Flack = n/a

  
;
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_hp_2_25gpa
_database_code_depnum_ccdc_archive 'CCDC 1845705'
_audit_update_record             
;
2018-05-28 deposited with the CCDC.
2018-07-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_hp_2_25gpa          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.737 Why?
RESPONSE: The data come from studies of high-pressure studies and are limited by the DAC opening angle
;
_vrf_PLAT305_hp_2_25gpa          
;
PROBLEM: Isolated Hydrogen Atom   (Outside Bond Range ??)        H1A Check
RESPONSE: Dma H-atoms were located also by using difference Fourier map therfore they can differ from the ideal positions.
;
_vrf_PLAT413_hp_2_25gpa          
;
PROBLEM: Short Inter XH3 .. XHn     H2       ..H2               1.45 Ang.
RESPONSE: Dma amine in framework is strongly disordered so exact location of H-atoms was difficult
;
_vrf_PLAT415_hp_2_25gpa          
;
PROBLEM: Short Inter D-H..H-X       H1A      ..H2               1.60 Ang.
RESPONSE: The guest is disordered in the three positions which results in short contacts between other H atoms
;
_vrf_PLAT417_hp_2_25gpa          
;
PROBLEM: Short Inter D-H..H-D       H1A      ..H1A              1.33 Ang.
RESPONSE: Dma amine in framework is strongly disordered so exact location of H-atoms was difficult
;
_vrf_PLAT415_hp_2_25gpa_2        
;
PROBLEM: Short Inter D-H..H-X       H1A      ..H2               2.00 Ang.
RESPONSE: Dma amine in framework is strongly disordered so exact location of H-atoms was difficult
;

_audit_creation_date             2018-05-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;

# CHEMICAL DATA 

_chemical_name_common            DmaNiFor3
_chemical_name_systematic        
;
 catena-(dimethylammonium tris(μ₂-formato)-nickel(ii))
;
_chemical_formula_moiety         '(C3 H3 Ni1 O6 1-)n,n(C2 H8 N1 1+))'
_chemical_formula_sum            'C5 H15 N Ni O6'
_chemical_formula_weight         243.88
_chemical_melting_point          ?
_chemical_oxdiff_formula         C15H9N9Ni3O18
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'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-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'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+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-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+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-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+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'

_cell_length_a                   7.981(4)
_cell_length_b                   7.981(4)
_cell_length_c                   21.55(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1189.0(19)
_cell_formula_units_Z            6.00012
_cell_measurement_reflns_used    344
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.0470
_cell_measurement_theta_min      4.9880
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.448
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56379
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.044
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_preparation       DMF
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.202
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.195
_exptl_special_details           
;
 Data were collected at room temperature and pressure of 2.25(2) GPa
 (2250000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique.
 Pressure was determined by monitoring the shift of the ruby
 R1-fluorescence line.
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?

# APARATURE DETAILS

_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0130
_diffrn_reflns_Laue_measured_fraction_full 0.737
_diffrn_reflns_Laue_measured_fraction_max 0.634
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            1892
_diffrn_reflns_point_group_measured_fraction_full 0.737
_diffrn_reflns_point_group_measured_fraction_max 0.634
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.241
_diffrn_reflns_theta_min         4.797
_diffrn_ambient_temperature      293(2)
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         2250000
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0593
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.737
_diffrn_measured_fraction_theta_max 0.634
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 phi    -35.00   19.75   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
   0.0000  -30.0000    0.0000     -     73

#__ type_ start__ end____ width___ exp.time_
  2 phi    140.00  200.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
   0.0000  -30.0000    0.0000     -     80

#__ type_ start__ end____ width___ exp.time_
  3 phi    160.00  217.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
   0.0000   30.0000    0.0000     -     76

#__ type_ start__ end____ width___ exp.time_
  4 phi    -20.00   34.75   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
   0.0000   30.0000    0.0000     -     73

#__ type_ start__ end____ width___ exp.time_
  5 omega  -24.00   24.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   39.4600  -12.9000 64

#__ type_ start__ end____ width___ exp.time_
  6 omega  -24.00   24.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   39.4600  167.1000 64

#__ type_ start__ end____ width___ exp.time_
  7 omega  -50.00   10.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   39.4600  167.1000 80

#__ type_ start__ end____ width___ exp.time_
  8 omega  -50.00   10.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   39.4600  -12.9000 80

#__ type_ start__ end____ width___ exp.time_
  9 omega  -64.00   -8.50   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   81.4000  -28.9000 74

#__ type_ start__ end____ width___ exp.time_
 10 omega  -64.00   -8.50   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   81.4000  151.1000 74

#__ type_ start__ end____ width___ exp.time_
 11 omega  -19.00    8.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   81.4000  151.1000 36

#__ type_ start__ end____ width___ exp.time_
 12 omega  -19.00    8.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   81.4000  -28.9000 36

#__ type_ start__ end____ width___ exp.time_
 13 omega  -43.00  -21.25   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  134.6000  -56.9000 29

#__ type_ start__ end____ width___ exp.time_
 14 omega  -43.00  -21.25   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  134.6000  123.1000 29

#__ type_ start__ end____ width___ exp.time_
 15 omega  -90.00  -36.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000  134.6000  123.1000 72

#__ type_ start__ end____ width___ exp.time_
 16 omega  -90.00  -36.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000  134.6000  -56.9000 72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω and π scans'
_diffrn_orient_matrix_UB_11      -0.0130529000
_diffrn_orient_matrix_UB_12      -0.0769807000
_diffrn_orient_matrix_UB_13      -0.0197368000
_diffrn_orient_matrix_UB_21      0.0764297000
_diffrn_orient_matrix_UB_22      -0.0035517000
_diffrn_orient_matrix_UB_23      0.0156216000
_diffrn_orient_matrix_UB_31      -0.0668908000
_diffrn_orient_matrix_UB_32      -0.0674920000
_diffrn_orient_matrix_UB_33      0.0216785000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                199
_reflns_number_total             211
_reflns_odcompleteness_completeness 68.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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         0.297
_refine_diff_density_min         -0.175
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.0027(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     36
_refine_ls_number_reflns         211
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0196
_refine_ls_restrained_S_all      1.110
_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)+(0.0264P)²+1.9920P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0471
_refine_ls_wR_factor_ref         0.0477
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Others
 Fixed Sof: N1(0.16667)
;

#ATOMS POSITIONS

_atom_sites_solution_hydrogens   difmap
_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
Ni1 Ni 0.0000 0.0000 0.0000 0.0133(3) Uani 1 6 d S T P . .
C1 C 0.1221(4) -0.2113(4) 0.0833 0.0179(6) Uani 1 2 d S T P . .
O1 O -0.01631(19) -0.21968(19) 0.05369(7) 0.0219(4) Uani 1 1 d . . . . .
N1 N -0.3333 -0.5853(11) 0.0833 0.027(2) Uani 0.3333 2 d S T P . .
C2 C -0.3333 -0.6667 0.0266(3) 0.0464(13) Uani 1 3 d S T P . .
H1 H 0.250(5) -0.083(5) 0.0833 0.030(9) Uiso 1 2 d S T P . .
H2 H -0.428(7) -0.779(7) 0.020(3) 0.116(18) Uiso 1 1 d . . . . .
H1A H -0.237(6) -0.474(8) 0.083(4) 0.15(3) Uiso 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
Ni1 0.0126(3) 0.0126(3) 0.0146(5) 0.000 0.000 0.00628(17)
C1 0.0188(11) 0.0188(11) 0.0186(18) -0.0002(5) 0.0002(5) 0.0111(12)
O1 0.0191(8) 0.0204(8) 0.0260(10) 0.0048(5) -0.0027(5) 0.0097(6)
N1 0.015(4) 0.019(3) 0.045(7) 0.0003(19) 0.001(4) 0.0074(19)
C2 0.051(2) 0.051(2) 0.037(4) 0.000 0.000 0.0254(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
Ni1 O1 2.0499(17) . ?
Ni1 O1 2.0499(17) 3 ?
Ni1 O1 2.0499(17) 21 ?
Ni1 O1 2.0499(17) 19 ?
Ni1 O1 2.0499(17) 20 ?
Ni1 O1 2.0499(17) 2 ?
C1 O1 1.248(2) 18_544 ?
C1 O1 1.248(2) . ?
N1 N1 1.125(15) 2_445 ?
N1 N1 1.125(15) 3_545 ?
N1 C2 1.384(7) 16_434 ?
N1 C2 1.384(7) . ?
C2 N1 1.384(7) 3_545 ?
C2 N1 1.384(7) 2_445 ?

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 Ni1 O1 180.0 . 19 ?
O1 Ni1 O1 91.26(8) 20 21 ?
O1 Ni1 O1 91.26(8) 2 3 ?
O1 Ni1 O1 88.74(8) . 20 ?
O1 Ni1 O1 91.26(8) . 3 ?
O1 Ni1 O1 91.26(8) 19 20 ?
O1 Ni1 O1 91.26(8) 19 21 ?
O1 Ni1 O1 91.26(8) . 2 ?
O1 Ni1 O1 88.74(8) 2 21 ?
O1 Ni1 O1 88.74(8) 19 2 ?
O1 Ni1 O1 88.74(8) 19 3 ?
O1 Ni1 O1 180.00(10) 20 2 ?
O1 Ni1 O1 180.00(8) 21 3 ?
O1 Ni1 O1 88.74(8) . 21 ?
O1 Ni1 O1 88.74(8) 20 3 ?
O1 C1 O1 124.0(3) . 18_544 ?
C1 O1 Ni1 124.53(15) . . ?
N1 N1 N1 60.000(1) 2_445 3_545 ?
N1 N1 C2 66.0(3) 2_445 . ?
N1 N1 C2 66.0(3) 3_545 16_434 ?
N1 N1 C2 66.0(3) 3_545 . ?
N1 N1 C2 66.0(3) 2_445 16_434 ?
C2 N1 C2 124.0(7) . 16_434 ?
N1 C2 N1 48.0(6) 3_545 . ?
N1 C2 N1 48.0(6) 2_445 . ?
N1 C2 N1 48.0(6) 3_545 2_445 ?

_iucr_refine_instructions_details 
;
TITL 32a in R-3c #167
REM reset to R-3c #167
CELL 0.71073 7.981219 7.981219 21.553216 90 90 120
ZERR 6.00012 0.004273 0.004273 0.026031 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -Y+X,-Y,0.5-Z
SYMM -X,-X+Y,0.5-Z
SYMM +Y,+X,0.5-Z
SFAC C H N Ni O
UNIT 30 90 6 6 36
 
L.S. 44 0 0
PLAN  4
BOND
fmap 2 53
acta
OMIT -1 2 3
OMIT 1 0 4
REM <olex2.extras>
REM <HklSrc "%.\\hp_2_25GPa.hkl">
REM </olex2.extras>
 
WGHT    0.026394    1.991985
EXTI    0.002708
FVAR       4.98434
NI1   4    0.000000    0.000000    0.000000    10.16667    0.01257    0.01257 =
         0.01463    0.00000    0.00000    0.00628
C1    1    0.122064   -0.211269    0.083333    10.50000    0.01877    0.01877 =
         0.01855   -0.00022    0.00022    0.01113
O1    5   -0.016315   -0.219683    0.053690    11.00000    0.01907    0.02038 =
         0.02600    0.00475   -0.00269    0.00970
N1    3   -0.333333   -0.585291    0.083333    10.16667    0.01477    0.01884 =
         0.04506    0.00033    0.00067    0.00739
C2    1   -0.333333   -0.666667    0.026625    10.33333    0.05082    0.05082 =
         0.03747    0.00000    0.00000    0.02541
H1    2    0.250408   -0.082925    0.083333    10.50000    0.02997
H2    2   -0.427606   -0.779015    0.020203    11.00000    0.11643
H1A   2   -0.236586   -0.473599    0.082879    11.00000    0.14833
HKLF 4
 
REM  32a in R-3c #167
REM R1 =  0.0196 for     199 Fo > 4sig(Fo)  and  0.0211 for all     211 data
REM     36 parameters refined using      0 restraints
 
END  
     
WGHT      0.0282      1.9246 

REM Highest difference peak  0.297,  deepest hole -0.175,  1-sigma level  0.051
Q1    1   0.0000  0.0000  0.0471  10.33333  0.05    0.30
Q2    1  -0.3333 -0.6667 -0.0255  10.33333  0.05    0.26
Q3    1  -0.0155 -0.1675  0.0173  11.00000  0.05    0.18
Q4    1  -0.3696 -0.7445  0.0010  11.00000  0.05    0.17

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0196 for 199 Fo > 4sig(Fo) and 0.0211 for all 2154 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.30, deepest hole -0.17
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0211
  REM R1_gt = 0.0196
  REM wR_ref = 0.0477
  REM GOOF = 1.110
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 2154
  REM Reflections_gt = 199
  REM Parameters = n/a
  REM Hole = -0.17
  REM Peak = 0.30
  REM Flack = n/a

  
;
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_hp_1_90gpa
_database_code_depnum_ccdc_archive 'CCDC 1845704'
_audit_update_record             
;
2018-05-28 deposited with the CCDC.
2018-07-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_hp_1_90gpa          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.802 Why?
RESPONSE: The data comes from high-pressure measurments and it is a consequence of the used apparatus
;
_vrf_PLAT305_hp_1_90gpa          
;
PROBLEM: Isolated Hydrogen Atom   (Outside Bond Range ??)        H1A Check
RESPONSE: Dma H-atoms were located also by using difference Fourier map therfore they can differ from the ideal positions.
;
_vrf_PLAT413_hp_1_90gpa          
;
PROBLEM: Short Inter XH3 .. XHn     H2       ..H2               1.51 Ang.
RESPONSE: Dma amine in framework is strongly disordered so exact location of H-atoms was difficult
;
_vrf_PLAT415_hp_1_90gpa          
;
PROBLEM: Short Inter D-H..H-X       H1A      ..H2               1.80 Ang.
RESPONSE: The guest is disordered in the three positions which results in short contacts between other H atoms
;
_vrf_PLAT417_hp_1_90gpa          
;
PROBLEM: Short Inter D-H..H-D       H1A      ..H1A              1.20 Ang.
RESPONSE: Dma amine in framework is strongly disordered so exact location of H-atoms was difficult
;

_audit_creation_date             2018-05-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;

# CHEMICAL DATA 

_chemical_name_common            DmaNiFor3
_chemical_name_systematic        
;
 catena-(dimethylammonium tris(μ₂-formato)-nickel(ii))
;
_chemical_formula_moiety         '(C3 H3 Ni1 O6 1-)n,n(C2 H8 N1 1+))'
_chemical_formula_sum            'C5 H15 N Ni O6'
_chemical_formula_weight         243.88
_chemical_melting_point          ?
_chemical_oxdiff_formula         C15H9N9Ni3O18
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'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-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'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+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-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+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-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+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'

_cell_length_a                   8.0016(16)
_cell_length_b                   8.0016(16)
_cell_length_c                   21.563(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1195.6(6)
_cell_formula_units_Z            6.00012
_cell_measurement_reflns_used    1190
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.7240
_cell_measurement_theta_min      3.1150
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.435
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41675
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.032
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_preparation       DMF
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.202
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1966
_exptl_special_details           
;
 Data were collected at room temperature and pressure of 1.90(2) GPa
 (1900000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique.
 Pressure was determined by monitoring the shift of the ruby
 R1-fluorescence line.
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?

# APARATURE DETAILS

_diffrn_reflns_av_R_equivalents  0.0983
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.802
_diffrn_reflns_Laue_measured_fraction_max 0.702
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            2305
_diffrn_reflns_point_group_measured_fraction_full 0.802
_diffrn_reflns_point_group_measured_fraction_max 0.702
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.574
_diffrn_reflns_theta_min         5.096
_diffrn_ambient_temperature      293(2)
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         1900000
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0593
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.802
_diffrn_measured_fraction_theta_max 0.702
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 phi    -35.00   19.75   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
   0.0000  -30.0000    0.0000     -     73

#__ type_ start__ end____ width___ exp.time_
  2 phi    140.00  200.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
   0.0000  -30.0000    0.0000     -     80

#__ type_ start__ end____ width___ exp.time_
  3 phi    160.00  217.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
   0.0000   30.0000    0.0000     -     76

#__ type_ start__ end____ width___ exp.time_
  4 phi    -20.00   34.75   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
   0.0000   30.0000    0.0000     -     73

#__ type_ start__ end____ width___ exp.time_
  5 omega  -24.00   24.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   39.4600  -12.9000 64

#__ type_ start__ end____ width___ exp.time_
  6 omega  -24.00   24.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   39.4600  167.1000 64

#__ type_ start__ end____ width___ exp.time_
  7 omega  -50.00   10.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   39.4600  167.1000 80

#__ type_ start__ end____ width___ exp.time_
  8 omega  -50.00   10.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   39.4600  -12.9000 80

#__ type_ start__ end____ width___ exp.time_
  9 omega  -64.00   -8.50   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   81.4000  -28.9000 74

#__ type_ start__ end____ width___ exp.time_
 10 omega  -64.00   -8.50   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   81.4000  151.1000 74

#__ type_ start__ end____ width___ exp.time_
 11 omega  -19.00    8.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   81.4000  151.1000 36

#__ type_ start__ end____ width___ exp.time_
 12 omega  -19.00    8.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   81.4000  -28.9000 36

#__ type_ start__ end____ width___ exp.time_
 13 omega  -43.00  -21.25   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  134.6000  -56.9000 29

#__ type_ start__ end____ width___ exp.time_
 14 omega  -43.00  -21.25   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  134.6000  123.1000 29

#__ type_ start__ end____ width___ exp.time_
 15 omega  -90.00  -36.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000  134.6000  123.1000 72

#__ type_ start__ end____ width___ exp.time_
 16 omega  -90.00  -36.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000  134.6000  -56.9000 72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω and π scans'
_diffrn_orient_matrix_UB_11      0.0696796333
_diffrn_orient_matrix_UB_12      0.0676979667
_diffrn_orient_matrix_UB_13      -0.0207620333
_diffrn_orient_matrix_UB_21      -0.0013497667
_diffrn_orient_matrix_UB_22      0.0760476667
_diffrn_orient_matrix_UB_23      0.0164285667
_diffrn_orient_matrix_UB_31      0.0748426000
_diffrn_orient_matrix_UB_32      0.0082084000
_diffrn_orient_matrix_UB_33      0.0196549000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                221
_reflns_number_total             243
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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         0.464
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       0.0053(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     36
_refine_ls_number_reflns         243
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0391
_refine_ls_restrained_S_all      1.158
_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)+(0.0462P)²+5.0118P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.0926
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Restrained distances
 C2-N1
 1.39 with sigma of 0.001
 H1A-N1
 0.98 with sigma of 0.02
2. Others
 Fixed Sof: N1(0.16667)
;

#ATOMS POSITIONS

_atom_sites_solution_hydrogens   difmap
_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
Ni1 Ni 0.0000 0.0000 0.0000 0.0139(6) Uani 1 6 d S T P . .
C1 C 0.1229(6) -0.2104(6) 0.0833 0.0207(11) Uani 1 2 d S T P . .
O1 O -0.0142(3) -0.2187(3) 0.05384(11) 0.0225(8) Uani 1 1 d . . . . .
N1 N 0.2502(14) -0.3333 -0.0833 0.029(4) Uani 0.3333 2 d DS T P . .
C2 C 0.3333 -0.3333 -0.0267(3) 0.046(2) Uani 1 3 d DS T P . .
H1 H 0.243(10) -0.090(10) 0.0833 0.05(2) Uiso 1 2 d S T P . .
H2 H 0.351(16) -0.432(14) -0.019(7) 0.12(3) Uiso 1 1 d . . . . .
H1A H 0.26(7) -0.21(4) -0.07(3) 0.6(4) Uiso 1 1 d 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
Ni1 0.0127(6) 0.0127(6) 0.0163(10) 0.000 0.000 0.0064(3)
C1 0.0185(17) 0.0185(17) 0.026(3) 0.0003(9) -0.0003(9) 0.0099(18)
O1 0.0171(12) 0.0184(12) 0.031(2) 0.0048(8) -0.0036(9) 0.0080(9)
N1 0.018(4) 0.023(6) 0.048(14) -0.009(6) -0.005(3) 0.012(3)
C2 0.054(4) 0.054(4) 0.031(8) 0.000 0.000 0.0268(19)

_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
Ni1 O1 2.055(2) 20 ?
Ni1 O1 2.055(2) 3 ?
Ni1 O1 2.055(2) 21 ?
Ni1 O1 2.055(2) 2 ?
Ni1 O1 2.055(2) . ?
Ni1 O1 2.055(2) 19 ?
C1 O1 1.241(3) 18_544 ?
C1 O1 1.241(3) . ?
N1 N1 1.153(19) 2_545 ?
N1 N1 1.153(19) 3_655 ?
N1 C2 1.3901(11) 10_444 ?
N1 C2 1.3902(11) . ?
C2 N1 1.3901(11) 3_655 ?
C2 N1 1.3901(11) 2_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
O1 Ni1 O1 180.0(2) 20 2 ?
O1 Ni1 O1 88.77(9) . 21 ?
O1 Ni1 O1 88.77(9) 19 3 ?
O1 Ni1 O1 88.77(9) 20 . ?
O1 Ni1 O1 88.77(9) 20 3 ?
O1 Ni1 O1 91.23(9) 2 . ?
O1 Ni1 O1 88.77(9) 2 21 ?
O1 Ni1 O1 91.23(9) 20 19 ?
O1 Ni1 O1 91.23(9) 19 21 ?
O1 Ni1 O1 88.77(9) 2 19 ?
O1 Ni1 O1 91.23(9) 2 3 ?
O1 Ni1 O1 180.0 . 19 ?
O1 Ni1 O1 180.00(13) 21 3 ?
O1 Ni1 O1 91.23(9) 20 21 ?
O1 Ni1 O1 91.23(9) . 3 ?
O1 C1 O1 124.1(4) . 18_544 ?
C1 O1 Ni1 125.0(2) . . ?
N1 N1 N1 60.0 2_545 3_655 ?
N1 N1 C2 65.5(4) 2_545 . ?
N1 N1 C2 65.5(4) 3_655 10_444 ?
N1 N1 C2 65.5(4) 3_655 . ?
N1 N1 C2 65.5(4) 2_545 10_444 ?
C2 N1 C2 122.8(11) . 10_444 ?
N1 C2 N1 49.0(9) 3_655 2_545 ?
N1 C2 N1 49.0(9) . 2_545 ?
N1 C2 N1 49.0(9) 3_655 . ?

_iucr_refine_instructions_details 
;
TITL 35 in R-3c #167
REM reset to R-3c #167
CELL 0.71073 8.001602 8.001602 21.562615 90 90 120
ZERR 6.00012 0.001558 0.001558 0.00629 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -Y+X,-Y,0.5-Z
SYMM -X,-X+Y,0.5-Z
SYMM +Y,+X,0.5-Z
SFAC C H N Ni O
UNIT 30 90 6 6 36
EQIV $1 -Y,-1+X-Y,+Z
EQIV $2 1+Y-X,-X,+Z
EQIV $3 0.667-X,0.333-X+Y,-0.167-Z
EQIV $4 0.667+Y,-0.667+X,-0.167-Z
EQIV $5 -0.333-Y+X,-0.667-Y,-0.167-Z
DFIX 1.39 0.001 C2 N1
DFIX 0.98 H1a N1
 
L.S. 44
PLAN  25
FREE N1 H2_$2
FREE C2 H1a_$4
FREE C2 H1a_$2
FREE C2 H1a_$5
FREE C2 H1a_$1
FREE C2 H1a_$3
FREE C2 H1a
BOND
fmap 2
acta
OMIT 0 4 20
OMIT -1 1 10
OMIT -3 4 20
OMIT 0 5 22
OMIT 0 3 18
OMIT -3 3 18
OMIT 1 0 -2
OMIT 7 0 -8
OMIT 4 3 16
OMIT 4 2 20
OMIT 3 2 22
OMIT 1 1 15
OMIT 2 2 21
OMIT 1 1 15
OMIT 5 0 8
OMIT 8 1 7
OMIT 4 3 -2
OMIT 5 3 11
OMIT 7 2 -7
OMIT 4 2 14
OMIT 5 3 -16
OMIT 2 0 14
OMIT 6 3 12
OMIT 6 3 12
OMIT 5 1 10
OMIT -3 5 22
OMIT -1 2 15
OMIT 0 1 2
OMIT -2 4 21
OMIT -3 7 2
OMIT 2 2 15
OMIT -2 2 14
OMIT 2 2 0
OMIT 2 1 -14
OMIT 6 1 -10
OMIT 5 2 12
REM <olex2.extras>
REM <HklSrc "%.\\hp_1_90GPa.hkl">
REM </olex2.extras>
 
WGHT    0.046200    5.011800
EXTI    0.005260
FVAR       4.87867
NI1   4    0.000000    0.000000    0.000000    10.16667    0.01270    0.01270 =
         0.01632    0.00000    0.00000    0.00635
C1    1    0.122909   -0.210424    0.083333    10.50000    0.01847    0.01847 =
         0.02606    0.00028   -0.00028    0.00991
O1    5   -0.014196   -0.218724    0.053837    11.00000    0.01709    0.01841 =
         0.03082    0.00478   -0.00359    0.00805
N1    3    0.250152   -0.333333   -0.083333    10.16667    0.01780    0.02322 =
         0.04825   -0.00909   -0.00455    0.01161
C2    1    0.333333   -0.333333   -0.026732    10.33333    0.05362    0.05362 =
         0.03120    0.00000    0.00000    0.02681
H1    2    0.243407   -0.089926    0.083333    10.50000    0.05469
H2    2    0.350766   -0.432448   -0.018531    11.00000    0.11767
H1A   2    0.262844   -0.208556   -0.072328    11.00000    0.59868
HKLF 4
 
REM  35 in R-3c #167
REM R1 =  0.0391 for     221 Fo > 4sig(Fo)  and  0.0436 for all     243 data
REM     36 parameters refined using      2 restraints
 
END  
     
WGHT      0.0453      5.0693 

REM Highest difference peak  0.464,  deepest hole -0.695,  1-sigma level  0.127
Q1    1  -0.0763 -0.1882  0.0864  11.00000  0.05    0.46
Q2    1  -0.0687 -0.2230  0.0210  11.00000  0.05    0.46
Q3    1   0.3750 -0.0442 -0.0476  11.00000  0.05    0.44
Q4    1   0.3333 -0.3333  0.0001  10.33333  0.05    0.43
Q5    1   0.1046 -0.0079  0.0044  11.00000  0.05    0.39
Q6    1   0.2420 -0.2611 -0.0545  11.00000  0.05    0.36
Q7    1   0.3022 -0.5223  0.0312  11.00000  0.05    0.34
Q8    1   0.0559 -0.2665  0.0374  11.00000  0.05    0.33
Q9    1   0.1748 -0.0035  0.0598  11.00000  0.05    0.32
Q10   1  -0.0510 -0.3242  0.0677  11.00000  0.05    0.32
Q11   1   0.3022 -0.1738  0.0414  11.00000  0.05    0.31
Q12   1   0.2377 -0.2485  0.0582  11.00000  0.05    0.31
Q13   1   0.3728 -0.5628 -0.0439  11.00000  0.05    0.31
Q14   1   0.3009 -0.5933 -0.0302  11.00000  0.05    0.30
Q15   1   0.0166 -0.1531  0.0505  11.00000  0.05    0.30
Q16   1   0.3677 -0.0392  0.0098  11.00000  0.05    0.29
Q17   1   0.0000  0.0000  0.0327  10.33333  0.05    0.28
Q18   1   0.0777 -0.0841  0.0275  11.00000  0.05    0.28
Q19   1   0.4189 -0.3423 -0.0226  11.00000  0.05    0.28
Q20   1   0.1526 -0.1564  0.0132  11.00000  0.05    0.27
Q21   1   0.2702 -0.0528  0.0371  11.00000  0.05    0.27
Q22   1   0.0414 -0.0475  0.0927  11.00000  0.05    0.26
Q23   1   0.4925 -0.3523 -0.0103  11.00000  0.05    0.25
Q24   1   0.1923 -0.5818 -0.0122  11.00000  0.05    0.24
Q25   1   0.3229 -0.0817  0.0723  11.00000  0.05    0.24

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0391 for 221 Fo > 4sig(Fo) and 0.0436 for all 2636 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.46, deepest hole -0.70
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0436
  REM R1_gt = 0.0391
  REM wR_ref = 0.0926
  REM GOOF = 1.163
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 2636
  REM Reflections_gt = 221
  REM Parameters = n/a
  REM Hole = -0.70
  REM Peak = 0.46
  REM Flack = n/a

  
;
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_co_hp_0_82gpa
_database_code_depnum_ccdc_archive 'CCDC 1845712'
_audit_update_record             
;
2018-05-28 deposited with the CCDC.
2018-07-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_co_hp_0_82gpa       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.703 Why?
RESPONSE: The data comes from high-pressure measurments and it is a consequence of the used apparatus
;
_vrf_PLAT305_co_hp_0_82gpa       
;
PROBLEM: Isolated Hydrogen Atom   (Outside Bond Range ??)        H1A Check
RESPONSE: Dma H-atoms were located also by using difference Fourier map therfore they can differ from the ideal positions.
;
_vrf_PLAT413_co_hp_0_82gpa       
;
PROBLEM: Short Inter XH3 .. XHn     H2       ..H2               1.37 Ang.
RESPONSE: The dma H-atoms were located also by using difference Fourier map therfore they can differ from the ideal positions.
;
_vrf_PLAT415_co_hp_0_82gpa       
;
PROBLEM: Short Inter D-H..H-X       H1       ..H1A              1.86 Ang.
RESPONSE: The guest is disordered in the three positions which results in short contacts between other H atoms
;
_vrf_PLAT415_co_hp_0_82gpa_2     
;
PROBLEM: Short Inter D-H..H-X       H1A      ..H2               2.01 Ang.
RESPONSE: Dma amine in framework is strongly disordered so exact location of H-atoms was difficult
;
_audit_creation_date             2018-05-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;

# CHEMICAL DATA 

_chemical_name_common            DmaCoFor3
_chemical_name_systematic        
;
  catena-(dimethylammonium tris(μ₂-formato)-cobalt(ii))
;
_chemical_formula_moiety         'C3 H3 Co1 O6 1-)n,n(C2 H8 N1 1+))'
_chemical_formula_sum            'C5 H12 Co N O6'
_chemical_formula_weight         241.08
_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 0.0033 0.0016 '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 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'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-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'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+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-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+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-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+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'

_cell_length_a                   8.142(3)
_cell_length_b                   8.142(3)
_cell_length_c                   21.986(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1262.1(12)
_cell_formula_units_Z            6.00012
_cell_measurement_reflns_used    1289
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.457
_cell_measurement_theta_min      4.608
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.039
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.903
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_preparation       DMF
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 Data were collected at room temperature and pressure of 0.82(2) GPa
 (820000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique.
 Pressure was determined by monitoring the shift of the ruby
 R1-fluorescence line.
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?

# APARATURE DETAILS

_diffrn_reflns_av_R_equivalents  0.1182
_diffrn_reflns_av_unetI/netI     0.0794
_diffrn_reflns_Laue_measured_fraction_full 0.703
_diffrn_reflns_Laue_measured_fraction_max 0.667
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            1980
_diffrn_reflns_point_group_measured_fraction_full 0.703
_diffrn_reflns_point_group_measured_fraction_max 0.667
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.457
_diffrn_reflns_theta_min         5.008
_diffrn_ambient_temperature      293(2)
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         820000
_diffrn_detector_area_resol_mean 16.6462
_diffrn_measured_fraction_theta_full 0.703
_diffrn_measured_fraction_theta_max 0.667
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                131
_reflns_number_total             196
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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         0.380
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     31
_refine_ls_number_reflns         196
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0407
_refine_ls_restrained_S_all      280.081
_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)+(0.0392P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0907
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 H1A-N1
 0.98 with sigma of 0.005
 N1_$1-N1_$2
 1.17 with sigma of 0.002
 N1-N1_$4
 1.16 with sigma of 0.002
 N1-C2
 1.389 with sigma of 0.005
 C2-C2_$3
 2.457 with sigma of 0.002
 N1-H1A \\sim C2-H2
 with sigma of 0.02
3. Others
 Fixed Sof: N1(0.16667)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1)
;

#ATOMS POSITIONS

_atom_sites_solution_hydrogens   mixed
_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 0.0000 0.0000 0.0000 0.0238(6) Uani 1 6 d S T P . .
O1 O -0.0119(5) -0.2187(5) 0.05385(18) 0.0325(11) Uani 1 1 d . . . . .
C1 C 0.1207(9) -0.2126(9) 0.0833 0.026(2) Uani 1 2 d S T P . .
H1 H 0.2349 -0.0984 0.0833 0.031 Uiso 1 2 calc RS T P . .
C2 C 0.0000 0.0000 0.19414(5) 0.054(3) Uani 1 3 d DS T P . .
N1 N 0.08226(15) 0.08226(15) 0.2500 0.054(8) Uani 0.3333 2 d DS T P . .
H2 H 0.083(14) 0.107(10) 0.168(4) 0.17(5) Uiso 1 1 d D . . . .
H1A H 0.2027(7) 0.2027(7) 0.2500 2(6) Uiso 1 2 d DS T 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 0.0224(8) 0.0224(8) 0.0266(12) 0.000 0.000 0.0112(4)
O1 0.024(2) 0.031(2) 0.042(3) 0.0045(18) -0.0059(18) 0.013(2)
C1 0.021(4) 0.021(4) 0.032(5) -0.0007(19) 0.0007(19) 0.007(4)
C2 0.057(6) 0.057(6) 0.048(10) 0.000 0.000 0.029(3)
N1 0.026(10) 0.026(10) 0.10(2) 0.004(7) -0.004(7) 0.008(10)

_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 2.100(3) . ?
Co1 O1 2.100(3) 3 ?
Co1 O1 2.100(3) 21 ?
Co1 O1 2.100(3) 19 ?
Co1 O1 2.100(3) 20 ?
Co1 O1 2.100(3) 2 ?
O1 C1 1.239(4) . ?
C1 O1 1.239(4) 18_544 ?
C1 H1 0.9300 . ?
C2 N1 1.3989(13) . ?
C2 N1 1.3989(13) 3 ?
C2 N1 1.3989(13) 2 ?
C2 H2 0.98(2) . ?
N1 C2 1.3989(13) 6 ?
N1 N1 1.160(2) 2 ?
N1 N1 1.160(2) 3 ?
N1 H1A 0.980(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
O1 Co1 O1 180.0 . 19 ?
O1 Co1 O1 88.68(15) 2 21 ?
O1 Co1 O1 91.32(15) 2 3 ?
O1 Co1 O1 88.67(15) . 20 ?
O1 Co1 O1 88.68(15) 19 3 ?
O1 Co1 O1 91.32(15) 19 20 ?
O1 Co1 O1 91.32(15) 19 21 ?
O1 Co1 O1 91.33(15) . 2 ?
O1 Co1 O1 91.33(15) . 3 ?
O1 Co1 O1 88.68(15) 19 2 ?
O1 Co1 O1 88.68(15) 20 3 ?
O1 Co1 O1 180.0(4) 20 2 ?
O1 Co1 O1 180.0(2) 21 3 ?
O1 Co1 O1 88.67(15) . 21 ?
O1 Co1 O1 91.32(15) 20 21 ?
C1 O1 Co1 126.2(3) . . ?
O1 C1 O1 125.8(7) 18_544 . ?
O1 C1 H1 117.1 . . ?
O1 C1 H1 117.1 18_544 . ?
N1 C2 N1 48.99(9) . 2 ?
N1 C2 N1 48.99(9) . 3 ?
N1 C2 N1 48.99(9) 2 3 ?
N1 C2 H2 98(6) . . ?
N1 C2 H2 130(7) 2 . ?
N1 C2 H2 141(7) 3 . ?
C2 N1 C2 122.79(11) . 6 ?
C2 N1 H1A 118.61(5) 6 . ?
C2 N1 H1A 118.61(5) . . ?
N1 N1 C2 65.50(4) 3 6 ?
N1 N1 C2 65.50(4) 3 . ?
N1 N1 C2 65.50(4) 2 6 ?
N1 N1 C2 65.50(4) 2 . ?
N1 N1 N1 60.0 2 3 ?
N1 N1 H1A 150.000(1) 2 . ?
N1 N1 H1A 150.000(1) 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 O1 C1 O1 -176.6(4) . . . 18_544 ?
N1 C2 N1 C2 -33.330(13) 3 . . 6 ?
N1 C2 N1 C2 33.330(14) 2 . . 6 ?
N1 C2 N1 N1 -66.66(3) 3 . . 2 ?
N1 C2 N1 N1 66.66(3) 2 . . 3 ?

_iucr_refine_instructions_details 
;
TITL a in R-3c #167
REM reset to R-3c #167
CELL 0.71073 8.1415 8.1415 21.9862 90 90 120
ZERR 6.00012 0.003 0.003 0.014 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -Y+X,-Y,0.5-Z
SYMM -X,-X+Y,0.5-Z
SYMM +Y,+X,0.5-Z
SFAC C H Co N O
UNIT 30 72 6 6 36
EQIV $1 1-Y,1+X-Y,+Z
EQIV $2 0.667-X,0.333-X+Y,0.833-Z
EQIV $3 +Y,+X,0.5-Z
EQIV $4 +Y-X,-X,+Z
DFIX 0.98 0.005 H1a N1
DFIX 1.17 0.002 N1_$1 N1_$2
DFIX 1.16 0.002 N1 N1_$4
DFIX 1.389 0.005 N1 C2
DFIX 2.457 0.002 C2 C2_$3
SADI N1 H1a C2 H2
 
L.S. 44
PLAN  1
TEMP 293
BOND
MORE -1
BOND $H
CONF
fmap 2
acta
OMIT 6 3 -12
OMIT 5 3 -1
OMIT 7 2 -4
OMIT 5 4 -11
OMIT 5 3 -1
OMIT 7 1 -6
OMIT 2 2 21
OMIT 1 1 0
OMIT 5 1 -20
OMIT 7 1 -3
OMIT 7 1 -3
OMIT 4 1 -9
REM <olex2.extras>
REM <HklSrc "%.\\Co_hp_0_82GPa.hkl">
REM </olex2.extras>
 
WGHT    0.037700
FVAR       0.32055
CO1   3    0.000000    0.000000    0.000000    10.16667    0.02244    0.02244 =
         0.02664    0.00000    0.00000    0.01122
O1    5   -0.011935   -0.218721    0.053848    11.00000    0.02436    0.03070 =
         0.04153    0.00448   -0.00588    0.01318
C1    1    0.120712   -0.212621    0.083333    10.50000    0.02056    0.02056 =
         0.03205   -0.00071    0.00071    0.00716
AFIX  43
H1    2    0.234937   -0.098387    0.083338    10.50000   -1.20000
AFIX   0
 
C2    1    0.000000    0.000000    0.194140    10.33333    0.05744    0.05744 =
         0.04809    0.00000    0.00000    0.02872
N1    4    0.082263    0.082263    0.250000    10.16667    0.02573    0.02573 =
         0.10470    0.00436   -0.00436    0.00787
H2    2    0.083373    0.107119    0.167720    11.00000    0.17110
H1A   2    0.202658    0.202658    0.250000    10.50000    2.00000
HKLF 4
 
REM  a in R-3c #167
REM R1 =  0.0407 for     131 Fo > 4sig(Fo)  and  0.0797 for all     196 data
REM     31 parameters refined using      6 restraints
 
END  
     
WGHT      0.0391      0.0000 

REM Highest difference peak  0.379,  deepest hole -0.397,  1-sigma level  0.082
Q1    1   0.0000  0.0000  0.1267  10.33333  0.05    0.38

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0407 for 131 Fo > 4sig(Fo) and 0.0797 for all 2215 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.38, deepest hole -0.40
  REM Mean Shift 0.000, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0797
  REM R1_gt = 0.0407
  REM wR_ref = 0.0895
  REM GOOF = 1.067
  REM Shift_max = 0.000
  REM Shift_mean = 0.000
  REM Reflections_all = 2215
  REM Reflections_gt = 131
  REM Parameters = n/a
  REM Hole = -0.40
  REM Peak = 0.38
  REM Flack = n/a

  
;
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_hp_3_14gpa
_database_code_depnum_ccdc_archive 'CCDC 1845707'
_audit_update_record             
;
2018-05-28 deposited with the CCDC.
2018-07-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_hp_3_14gpa          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.561 Why?
RESPONSE: The data come from studies of high-pressure studies and are limited by the DAC opening angle
;
_vrf_PLAT031_hp_3_14gpa          
;
PROBLEM: Refined Extinction Parameter Within Range ......      2.182 Sigma
RESPONSE: Crystal used for x-ray measurement was extremely small
;

_audit_creation_date             2018-05-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_shelxl_version_number           2013-2



# CHEMICAL DATA 

_chemical_name_common            DmaNiFor3
_chemical_name_systematic        
;
 catena-(dimethylammonium tris(μ₂-formato)-nickel(ii))
;
_chemical_formula_moiety         '(C3 H3 Ni1 O6 1-)n,n(C2 H8 N1 1+))'
_chemical_formula_sum            'C5 H15 N Ni O6'
_chemical_formula_weight         243.88
_chemical_melting_point          ?
_chemical_oxdiff_formula         C15H9N9Ni3O18

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'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-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'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+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-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+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-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+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'

_cell_length_a                   7.9659(6)
_cell_length_b                   7.9659(6)
_cell_length_c                   21.172(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1163.5(2)
_cell_formula_units_Z            6.00012
_cell_measurement_reflns_used    1278
_cell_measurement_temperature    293(2)
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         3140000
_cell_measurement_theta_max      27.8500
_cell_measurement_theta_min      5.8410
_shelx_estimated_absorpt_T_max   0.635
_shelx_estimated_absorpt_T_min   0.582
_exptl_absorpt_coefficient_mu    2.502
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.088
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_preparation       DMF
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.197
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.195
_exptl_special_details           
;
 Data were collected at room temperature and pressure of 3.14(2) GPa
 (31400000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique.
 Pressure was determined by monitoring the shift of the ruby
 R1-fluorescence line.
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?

# APARATURE DETAILS

_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0134
_diffrn_reflns_Laue_measured_fraction_full 0.561
_diffrn_reflns_Laue_measured_fraction_max 0.505
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            1825
_diffrn_reflns_point_group_measured_fraction_full 0.561
_diffrn_reflns_point_group_measured_fraction_max 0.505
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.833
_diffrn_reflns_theta_min         5.119
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0338
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.561
_diffrn_measured_fraction_theta_max 0.505
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 phi    -35.00   19.75   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
   0.0000  -30.0000    0.0000     -     73

#__ type_ start__ end____ width___ exp.time_
  2 phi    140.00  200.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
   0.0000  -30.0000    0.0000     -     80

#__ type_ start__ end____ width___ exp.time_
  3 phi    160.00  217.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
   0.0000   30.0000    0.0000     -     76

#__ type_ start__ end____ width___ exp.time_
  4 phi    -20.00   34.75   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
   0.0000   30.0000    0.0000     -     73

#__ type_ start__ end____ width___ exp.time_
  5 omega  -24.00   24.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   39.4600  -12.9000 64

#__ type_ start__ end____ width___ exp.time_
  6 omega  -24.00   24.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   39.4600  167.1000 64

#__ type_ start__ end____ width___ exp.time_
  7 omega  -50.00   10.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   39.4600  167.1000 80

#__ type_ start__ end____ width___ exp.time_
  8 omega  -50.00   10.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   39.4600  -12.9000 80

#__ type_ start__ end____ width___ exp.time_
  9 omega  -64.00   -8.50   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   81.4000  -28.9000 74

#__ type_ start__ end____ width___ exp.time_
 10 omega  -64.00   -8.50   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   81.4000  151.1000 74

#__ type_ start__ end____ width___ exp.time_
 11 omega  -19.00    8.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   81.4000  151.1000 36

#__ type_ start__ end____ width___ exp.time_
 12 omega  -19.00    8.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   81.4000  -28.9000 36

#__ type_ start__ end____ width___ exp.time_
 13 omega  -43.00  -21.25   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  134.6000  -56.9000 29

#__ type_ start__ end____ width___ exp.time_
 14 omega  -43.00  -21.25   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  134.6000  123.1000 29

#__ type_ start__ end____ width___ exp.time_
 15 omega  -90.00  -36.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000  134.6000  123.1000 72

#__ type_ start__ end____ width___ exp.time_
 16 omega  -90.00  -36.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000  134.6000  -56.9000 72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω and π scans'
_diffrn_orient_matrix_UB_11      0.0887158000
_diffrn_orient_matrix_UB_12      0.0465660000
_diffrn_orient_matrix_UB_13      -0.0169121000
_diffrn_orient_matrix_UB_21      0.0208570000
_diffrn_orient_matrix_UB_22      0.0903408000
_diffrn_orient_matrix_UB_23      0.0131407000
_diffrn_orient_matrix_UB_31      0.0475267000
_diffrn_orient_matrix_UB_32      -0.0154609000
_diffrn_orient_matrix_UB_33      0.0258293000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                151
_reflns_number_total             158
_reflns_odcompleteness_completeness 52.09
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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         0.339
_refine_diff_density_min         -0.128
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       0.0024(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     36
_refine_ls_number_reflns         158
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0195
_refine_ls_R_factor_gt           0.0181
_refine_ls_restrained_S_all      1.130
_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)+(0.0304P)²+0.6507P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0450
_refine_ls_wR_factor_ref         0.0453
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Restrained distances
 N1-C2
 1.384 with sigma of 0.002
 N1_$3-N1_$6
 1.11 with sigma of 0.001
2. Others
 Fixed Sof: N1(0.16667)
;

#ATOMS POSITIONS

_atom_sites_solution_hydrogens   difmap
_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
Ni1 Ni 0.0000 0.0000 0.0000 0.0129(3) Uani 1 6 d S T P . .
C1 C 0.3333 0.1210(4) -0.0833 0.0181(7) Uani 1 2 d S T P . .
O1 O 0.20211(19) -0.01868(18) -0.05377(6) 0.0208(4) Uani 1 1 d . . . . .
N1 N 0.58621(8) 0.25288(8) 0.0833 0.025(2) Uani 0.3333 2 d DS T P . .
C2 C 0.6667 0.3333 0.02551(11) 0.0437(14) Uani 1 3 d DS T P . .
H1 H 0.3333 0.247(5) -0.0833 0.036(10) Uiso 1 2 d S T P . .
H2 H 0.571(6) 0.222(7) 0.021(3) 0.090(14) Uiso 1 1 d . . . . .
H1A H 0.497(8) 0.248(6) 0.086(4) 0.12(3) Uiso 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
Ni1 0.0128(4) 0.0128(4) 0.0129(5) 0.000 0.000 0.00641(19)
C1 0.0178(17) 0.0177(13) 0.0187(15) -0.0002(6) -0.0004(12) 0.0089(8)
O1 0.0192(8) 0.0182(8) 0.0246(8) 0.0027(7) 0.0068(6) 0.0089(6)
N1 0.021(3) 0.021(3) 0.034(7) 0.001(3) -0.001(3) 0.011(5)
C2 0.052(2) 0.052(2) 0.028(3) 0.000 0.000 0.0259(12)

_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
Ni1 O1 2.0371(12) . ?
Ni1 O1 2.0371(12) 2 ?
Ni1 O1 2.0371(12) 20 ?
Ni1 O1 2.0371(12) 21 ?
Ni1 O1 2.0371(12) 3 ?
Ni1 O1 2.0371(12) 19 ?
C1 O1 1.2486(18) 11_554 ?
C1 O1 1.2487(18) . ?
N1 N1 1.1101(11) 17_654 ?
N1 C2 1.382(2) . ?
N1 C2 1.382(2) 16_554 ?
C2 N1 1.382(2) 2_655 ?
C2 N1 1.382(2) 17_654 ?
C2 N1 1.382(2) 3_665 ?

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 Ni1 O1 88.20(5) . 21 ?
O1 Ni1 O1 88.20(5) 3 20 ?
O1 Ni1 O1 88.20(5) 19 2 ?
O1 Ni1 O1 91.80(5) . 3 ?
O1 Ni1 O1 91.80(5) . 2 ?
O1 Ni1 O1 180.00(9) 21 3 ?
O1 Ni1 O1 91.80(5) 21 20 ?
O1 Ni1 O1 180.0 . 19 ?
O1 Ni1 O1 91.80(5) 19 20 ?
O1 Ni1 O1 91.80(5) 21 19 ?
O1 Ni1 O1 88.20(5) 21 2 ?
O1 Ni1 O1 88.20(5) 3 19 ?
O1 Ni1 O1 180.00(9) 20 2 ?
O1 Ni1 O1 88.20(5) . 20 ?
O1 Ni1 O1 91.80(5) 3 2 ?
O1 C1 O1 123.6(3) . 11_554 ?
C1 O1 Ni1 123.72(13) . . ?
N1 N1 C2 66.32(5) 17_654 . ?
N1 N1 C2 66.32(5) 17_654 16_554 ?
C2 N1 C2 124.73(11) . 16_554 ?
N1 C2 N1 47.37(9) 3_665 17_654 ?
N1 C2 N1 47.37(9) . 17_654 ?
N1 C2 N1 0.000(1) 2_655 17_654 ?
N1 C2 N1 47.37(9) 2_655 3_665 ?
N1 C2 N1 47.37(9) . 3_665 ?
N1 C2 N1 47.37(9) 2_655 . ?

_iucr_refine_instructions_details 
;
TITL 32b in R-3c #167
REM reset to R-3c #167
CELL 0.71073 7.9659 7.9659 21.172387 90 90 120
ZERR 6.00012 0.0006 0.0006 0.0026 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -Y+X,-Y,0.5-Z
SYMM -X,-X+Y,0.5-Z
SYMM +Y,+X,0.5-Z
SFAC C H N Ni O
UNIT 30 90 6 6 36
EQIV $1 1-Y,+X-Y,+Z
EQIV $2 0.333-Y+X,0.667-Y,1.167-Z
EQIV $3 1+Y-X,1-X,+Z
EQIV $4 1.333-X,0.667-X+Y,1.167-Z
EQIV $5 0.333+Y,-0.333+X,0.167-Z
EQIV $6 1.333-X,0.667-X+Y,0.167-Z
DFIX 1.384 0.002 N1 C2
DFIX 1.11 0.001 N1_$3 N1_$6
 
L.S. 44
PLAN  1
SIZE 0.2 0.2168 0.2428
FREE C2 H1a_$3
FREE C2 H1a_$1
FREE C2 H1a
FREE N1 N1_$4
FREE N1 N1_$2
FREE N1 N1_$3
FREE N1 N1_$1
FREE N1 H2_$5
FREE N1 H2
BOND
fmap 2
acta
OMIT 1 1 3
OMIT -1 2 3
OMIT 7 2 -7
OMIT 1 1 0
REM <olex2.extras>
REM <HklSrc "%.\\hp_3_14GPa.hkl">
REM </olex2.extras>
 
WGHT    0.030400    0.650700
EXTI    0.002427
FVAR       0.16411
NI1   4    0.000000    0.000000    0.000000    10.16667    0.01281    0.01281 =
         0.01295    0.00000    0.00000    0.00641
C1    1    0.333333    0.121002   -0.083333    10.50000    0.01782    0.01772 =
         0.01868   -0.00020   -0.00040    0.00891
O1    5    0.202106   -0.018677   -0.053774    11.00000    0.01915    0.01821 =
         0.02458    0.00272    0.00681    0.00893
N1    3    0.586209    0.252876    0.083333    10.16667    0.02074    0.02074 =
         0.03367    0.00093   -0.00093    0.01107
C2    1    0.666667    0.333333    0.025512    10.33333    0.05177    0.05177 =
         0.02770    0.00000    0.00000    0.02588
H1    2    0.333333    0.246620   -0.083333    10.50000    0.03587
H2    2    0.571276    0.222331    0.021221    11.00000    0.08995
H1A   2    0.496530    0.248116    0.085914    11.00000    0.11925
HKLF 4
 
REM  32b in R-3c #167
REM R1 =  0.0181 for     151 Fo > 4sig(Fo)  and  0.0195 for all     158 data
REM     36 parameters refined using      2 restraints
 
END  
     
WGHT      0.0302      0.6680 

REM Highest difference peak  0.339,  deepest hole -0.128,  1-sigma level  0.047
Q1    1   0.6667  0.3333 -0.0220  10.33333  0.05    0.34

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0181 for 151 Fo > 4sig(Fo) and 0.0195 for all 6462 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.34, deepest hole -0.13
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0195
  REM R1_gt = 0.0181
  REM wR_ref = 0.0453
  REM GOOF = 1.135
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 6462
  REM Reflections_gt = 151
  REM Parameters = n/a
  REM Hole = -0.13
  REM Peak = 0.34
  REM Flack = n/a

  
;
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-7 0 -37 0.1000 -7.0134 0.0062 -37.0078 0.0040 -0.6320 -1.2893
4 -11 -21 0.1000 4.0083 -11.0111 -21.0298 0.1985 -1.1875 -0.1824
-7 0 44 0.1000 -7.0153 0.0058 43.8643 -1.3639 0.4306 0.7995
4 -11 27 0.1000 4.0072 -11.0113 26.8944 -0.6121 -0.5578 1.0554
7 0 -44 0.1000 7.0153 -0.0058 -43.8643 1.3639 -0.4306 -0.7995
14 -7 -3 0.1000 14.0283 -7.0169 -2.9270 0.9673 -0.3798 0.6996
-4 11 21 0.1000 -4.0083 11.0111 21.0298 -0.1985 1.1875 0.1824
-14 7 3 0.1000 -14.0283 7.0169 2.9270 -0.9673 0.3798 -0.6996
-4 11 -27 0.1000 -4.0072 11.0113 -26.8944 0.6121 0.5578 -1.0554
-9 -7 7 0.1000 -9.0187 -6.9972 6.8397 -1.2416 -0.7304 -0.1438
7 0 37 0.1000 7.0134 -0.0062 37.0078 -0.0040 0.6320 1.2893
9 7 -7 0.1000 9.0187 6.9972 -6.8397 1.2416 0.7304 0.1438

_olex2_submission_special_instructions 'No special instructions were received'
